# Supplementary Material (ESI) for Chemical Communications

# This journal is © The Royal Society of Chemistry 2002



data_global

_journal_name_full               Chem.Commun.



_journal_coden_Cambridge         0182



loop_

_publ_author_name

'Wing-Por Leung'

'Thomas C. W. Mak'

'Cheuk-Wai So'

'Jin-Zhi Wang'



_publ_contact_author_name        'Prof Wing-Por Leung'

_publ_contact_author_address     

;

Department of Chemistry

The Chinese University of Hong Kong

Science Centre

Shatin

HONG KONG

;



_publ_contact_author_email       KEVINLEUNG@CUHK.EDU.HK



_publ_section_title              

;

A novel synthesis of metallogermacyclopropane and

molybdenum bis(iminophosphorano)carbene complexes from

bisgermavinylidene

;



data_scw1

_database_code_CSD               188276



_audit_creation_method           SHELXL-97

_chemical_name_systematic        

; 

? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C39 H38 Ge N2 O8 P2 Si2 W2'

_chemical_formula_weight         1221.12



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Orthorhombic

_symmetry_space_group_name_H-M   P2(1)2(1)2(1)



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-x+1/2, -y, z+1/2'

'-x, y+1/2, -z+1/2'

'x+1/2, -y+1/2, -z'



_cell_length_a                   10.9208(15)

_cell_length_b                   19.945(3)

_cell_length_c                   20.951(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     4563.3(11)

_cell_formula_units_Z            4

_cell_measurement_temperature    294(2)

_cell_measurement_reflns_used    21414

_cell_measurement_theta_min      1

_cell_measurement_theta_max      27.5



_exptl_crystal_description       block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.28

_exptl_crystal_size_mid          0.22

_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.777

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2352

_exptl_absorpt_coefficient_mu    5.855

_exptl_absorpt_correction_type   empirical

_exptl_absorpt_correction_T_min  0.2910

_exptl_absorpt_correction_T_max  0.3872

_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'



_exptl_special_details           

; 

? 

;



_diffrn_ambient_temperature      294(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker CCD Area Detector'

_diffrn_measurement_method       'phi and omega scan'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            31134

_diffrn_reflns_av_R_equivalents  0.0390

_diffrn_reflns_av_sigmaI/netI    0.0397

_diffrn_reflns_limit_h_min       -11

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -25

_diffrn_reflns_limit_k_max       25

_diffrn_reflns_limit_l_min       -19

_diffrn_reflns_limit_l_max       27

_diffrn_reflns_theta_min         1.41

_diffrn_reflns_theta_max         27.54

_reflns_number_total             10521

_reflns_number_gt                9264

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SHELXTL NT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL NT'

_computing_publication_material  'Bruker SHELXTL NT'



_refine_special_details          

; 

Refinement of F² against ALL reflections.  The weighted R-factor wR and 

goodness of fit S are based on F², conventional R-factors R are based 

on F, with F set to zero for negative F². The threshold expression of 

F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 

not relevant to the choice of reflections for refinement.  R-factors based 

on F² are statistically about twice as large as those based on F, and R- 

factors based on ALL data will be even larger. 

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     

'calc w=1/[σ²(Fo²)+(0.0442P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -0.011(8)

_refine_ls_number_reflns         10521

_refine_ls_number_parameters     505

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0370

_refine_ls_R_factor_gt           0.0277

_refine_ls_wR_factor_ref         0.0836

_refine_ls_wR_factor_gt          0.0628

_refine_ls_goodness_of_fit_ref   1.090

_refine_ls_restrained_S_all      1.090

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

W1 W 0.043231(16) 0.410896(9) 0.733114(10) 0.04301(4) Uani 1 1 d . . .

W2 W 0.130613(15) 0.517364(8) 0.931946(9) 0.03732(4) Uani 1 1 d . . .

Ge1 Ge 0.16264(4) 0.43234(2) 0.83852(2) 0.03675(11) Uani 1 1 d . . .

Si1 Si 0.29182(16) 0.28679(6) 0.89285(9) 0.0623(4) Uani 1 1 d . . .

Si2 Si 0.20496(12) 0.68916(6) 0.95086(7) 0.0474(4) Uani 1 1 d . . .

P1 P 0.39601(9) 0.43055(5) 0.87429(6) 0.0369(3) Uani 1 1 d . . .

P2 P 0.31502(9) 0.58398(5) 0.86008(5) 0.0348(2) Uani 1 1 d . . .

O1 O 0.2625(4) 0.4565(3) 0.6429(2) 0.0919(15) Uani 1 1 d . . .

O2 O 0.1357(5) 0.2620(2) 0.7175(3) 0.1117(18) Uani 1 1 d . . .

O3 O -0.1070(4) 0.3926(2) 0.6072(2) 0.0894(14) Uani 1 1 d . . .

O4 O -0.1763(4) 0.3547(2) 0.8184(3) 0.0962(17) Uani 1 1 d . . .

O5 O -0.0492(4) 0.56218(19) 0.7347(2) 0.0828(14) Uani 1 1 d . . .

O6 O 0.1063(5) 0.3842(2) 1.0083(2) 0.0919(15) Uani 1 1 d . . .

O7 O -0.1270(3) 0.5010(2) 0.8734(2) 0.0772(13) Uani 1 1 d . . .

O8 O -0.0506(4) 0.5637(3) 1.0392(2) 0.0971(15) Uani 1 1 d . . .

N1 N 0.2944(3) 0.37101(17) 0.87169(19) 0.0417(9) Uani 1 1 d . . .

N2 N 0.2226(3) 0.61068(16) 0.91382(18) 0.0382(9) Uani 1 1 d . . .

C1 C 0.1877(5) 0.4408(3) 0.6771(3) 0.0629(16) Uani 1 1 d . . .

C2 C 0.1012(5) 0.3158(3) 0.7245(3) 0.0648(16) Uani 1 1 d . . .

C3 C -0.0542(5) 0.3988(3) 0.6543(3) 0.0600(15) Uani 1 1 d . . .

C4 C -0.0996(5) 0.3762(3) 0.7885(3) 0.0595(16) Uani 1 1 d . . .

C5 C -0.0151(4) 0.5080(2) 0.7370(3) 0.0526(13) Uani 1 1 d . . .

C6 C 0.1152(5) 0.4310(3) 0.9781(2) 0.0551(14) Uani 1 1 d . . .

C7 C -0.0315(4) 0.5050(2) 0.8952(3) 0.0524(13) Uani 1 1 d . . .

C8 C 0.0187(5) 0.5482(3) 1.0007(3) 0.0572(14) Uani 1 1 d . . .

C9 C 0.2944(4) 0.49839(17) 0.8679(2) 0.0323(10) Uani 1 1 d . . .

C10 C 0.1292(7) 0.2607(3) 0.8927(4) 0.089(2) Uani 1 1 d . . .

H10A H 0.0955 0.2670 0.8508 0.133 Uiso 1 1 calc R . .

H10B H 0.0843 0.2874 0.9229 0.133 Uiso 1 1 calc R . .

H10C H 0.1235 0.2143 0.9044 0.133 Uiso 1 1 calc R . .

C11 C 0.3831(8) 0.2357(3) 0.8426(4) 0.123(3) Uani 1 1 d . . .

H11A H 0.3550 0.2398 0.7993 0.184 Uiso 1 1 calc R . .

H11B H 0.3767 0.1898 0.8560 0.184 Uiso 1 1 calc R . .

H11C H 0.4669 0.2499 0.8452 0.184 Uiso 1 1 calc R . .

C12 C 0.3542(8) 0.2732(3) 0.9753(3) 0.106(3) Uani 1 1 d . . .

H12A H 0.3080 0.2994 1.0053 0.159 Uiso 1 1 calc R . .

H12B H 0.4386 0.2868 0.9765 0.159 Uiso 1 1 calc R . .

H12C H 0.3481 0.2266 0.9862 0.159 Uiso 1 1 calc R . .

C13 C 0.0435(5) 0.7185(3) 0.9416(4) 0.078(2) Uani 1 1 d . . .

H13A H -0.0111 0.6863 0.9603 0.117 Uiso 1 1 calc R . .

H13B H 0.0248 0.7235 0.8971 0.117 Uiso 1 1 calc R . .

H13C H 0.0337 0.7609 0.9627 0.117 Uiso 1 1 calc R . .

C14 C 0.2392(6) 0.6777(3) 1.0370(3) 0.0704(18) Uani 1 1 d . . .

H14A H 0.3218 0.6622 1.0419 0.106 Uiso 1 1 calc R . .

H14B H 0.1838 0.6454 1.0548 0.106 Uiso 1 1 calc R . .

H14C H 0.2297 0.7198 1.0588 0.106 Uiso 1 1 calc R . .

C15 C 0.3116(5) 0.7528(2) 0.9143(3) 0.0681(19) Uani 1 1 d . . .

H15A H 0.3947 0.7380 0.9193 0.102 Uiso 1 1 calc R . .

H15B H 0.3012 0.7952 0.9353 0.102 Uiso 1 1 calc R . .

H15C H 0.2933 0.7576 0.8697 0.102 Uiso 1 1 calc R . .

C16 C 0.4711(4) 0.6092(2) 0.8751(2) 0.0419(11) Uani 1 1 d . . .

C17 C 0.5443(5) 0.6388(3) 0.8288(3) 0.0628(15) Uani 1 1 d . . .

H17A H 0.5114 0.6498 0.7892 0.075 Uiso 1 1 calc R . .

C18 C 0.6678(5) 0.6521(3) 0.8418(4) 0.081(2) Uani 1 1 d . . .

H18A H 0.7183 0.6702 0.8105 0.097 Uiso 1 1 calc R . .

C19 C 0.7134(5) 0.6381(3) 0.9017(4) 0.076(2) Uani 1 1 d . . .

H19A H 0.7947 0.6480 0.9108 0.092 Uiso 1 1 calc R . .

C20 C 0.6421(4) 0.6102(3) 0.9475(3) 0.0613(16) Uani 1 1 d . . .

H20A H 0.6753 0.6006 0.9874 0.074 Uiso 1 1 calc R . .

C21 C 0.5206(4) 0.5961(2) 0.9354(3) 0.0456(11) Uani 1 1 d . . .

H21A H 0.4716 0.5779 0.9673 0.055 Uiso 1 1 calc R . .

C22 C 0.2770(4) 0.6130(2) 0.7810(2) 0.0474(12) Uani 1 1 d . . .

C23 C 0.3361(6) 0.5861(3) 0.7275(3) 0.0677(16) Uani 1 1 d . . .

H23A H 0.3932 0.5519 0.7324 0.081 Uiso 1 1 calc R . .

C24 C 0.3090(7) 0.6108(4) 0.6665(3) 0.093(2) Uani 1 1 d . . .

H24A H 0.3510 0.5938 0.6315 0.112 Uiso 1 1 calc R . .

C25 C 0.2207(9) 0.6603(4) 0.6570(4) 0.113(3) Uani 1 1 d . . .

H25A H 0.2028 0.6760 0.6163 0.136 Uiso 1 1 calc R . .

C26 C 0.1651(8) 0.6833(3) 0.7062(4) 0.111(3) Uani 1 1 d . . .

H26A H 0.1061 0.7162 0.6996 0.133 Uiso 1 1 calc R . .

C27 C 0.1872(5) 0.6623(2) 0.7704(3) 0.0643(16) Uani 1 1 d . . .

H27A H 0.1433 0.6806 0.8042 0.077 Uiso 1 1 calc R . .

C28 C 0.4916(4) 0.4264(2) 0.9448(2) 0.0427(12) Uani 1 1 d . . .

C29 C 0.6145(4) 0.4088(3) 0.9422(3) 0.0611(15) Uani 1 1 d . . .

H29A H 0.6482 0.3971 0.9030 0.073 Uiso 1 1 calc R . .

C30 C 0.6882(6) 0.4080(3) 0.9955(3) 0.0774(19) Uani 1 1 d . . .

H30A H 0.7707 0.3967 0.9926 0.093 Uiso 1 1 calc R . .

C31 C 0.6370(6) 0.4241(3) 1.0521(3) 0.085(2) Uani 1 1 d . . .

H31A H 0.6855 0.4247 1.0886 0.102 Uiso 1 1 calc R . .

C32 C 0.5135(6) 0.4399(3) 1.0569(3) 0.0704(18) Uani 1 1 d . . .

H32A H 0.4789 0.4489 1.0966 0.085 Uiso 1 1 calc R . .

C33 C 0.4435(5) 0.4421(2) 1.0031(2) 0.0545(14) Uani 1 1 d . . .

H33A H 0.3616 0.4544 1.0061 0.065 Uiso 1 1 calc R . .

C34 C 0.4963(4) 0.4298(2) 0.8062(2) 0.0481(13) Uani 1 1 d . . .

C35 C 0.4655(5) 0.3905(3) 0.7532(3) 0.0711(18) Uani 1 1 d . . .

H35A H 0.4005 0.3604 0.7552 0.085 Uiso 1 1 calc R . .

C36 C 0.5328(6) 0.3970(4) 0.6983(3) 0.095(2) Uani 1 1 d . . .

H36A H 0.5149 0.3690 0.6641 0.114 Uiso 1 1 calc R . .

C37 C 0.6241(6) 0.4423(5) 0.6917(3) 0.106(3) Uani 1 1 d . . .

H37A H 0.6637 0.4475 0.6528 0.127 Uiso 1 1 calc R . .

C38 C 0.6576(5) 0.4807(4) 0.7436(3) 0.088(2) Uani 1 1 d . . .

H38A H 0.7225 0.5107 0.7405 0.106 Uiso 1 1 calc R . .

C39 C 0.5934(4) 0.4741(3) 0.8006(3) 0.0608(15) Uani 1 1 d . . .

H39A H 0.6162 0.4999 0.8356 0.073 Uiso 1 1 calc R . .






_geom_special_details            

; 

All esds (except the esd in the dihedral angle between two l.s. planes) 

are estimated using the full covariance matrix.  The cell esds are taken 

into account individually in the estimation of esds in distances, angles 

and torsion angles; correlations between esds in cell parameters are only 

used when they are defined by crystal symmetry.  An approximate (isotropic) 

treatment of cell esds is used for estimating esds involving l.s. planes. 

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

W1 C3 1.979(5) . ?

W1 C2 2.008(5) . ?

W1 C5 2.040(5) . ?

W1 C1 2.054(6) . ?

W1 C4 2.064(6) . ?

W1 Ge1 2.6001(6) . ?

W2 C7 1.946(5) . ?

W2 C6 1.982(5) . ?

W2 C8 1.987(5) . ?

W2 N2 2.149(3) . ?

W2 C9 2.267(4) . ?

W2 Ge1 2.6133(5) . ?

W2 P2 2.8440(11) . ?

Ge1 N1 2.013(4) . ?

Ge1 C9 2.046(4) . ?

Ge1 P1 2.6567(12) . ?

Si1 N1 1.737(4) . ?

Si1 C11 1.772(8) . ?

Si1 C10 1.850(7) . ?

Si1 C12 1.876(7) . ?

Si2 N2 1.758(3) . ?

Si2 C14 1.857(6) . ?

Si2 C13 1.868(6) . ?

Si2 C15 1.885(5) . ?

P1 N1 1.626(4) . ?

P1 C9 1.755(4) . ?

P1 C34 1.798(5) . ?

P1 C28 1.811(5) . ?

P2 N2 1.603(4) . ?

P2 C9 1.730(4) . ?

P2 C22 1.803(5) . ?

P2 C16 1.805(4) . ?

O1 C1 1.131(7) . ?

O2 C2 1.146(7) . ?

O3 C3 1.149(7) . ?

O4 C4 1.129(7) . ?

O5 C5 1.145(6) . ?

O6 C6 1.133(6) . ?

O7 C7 1.142(6) . ?

O8 C8 1.149(7) . ?

C10 H10A 0.9600 . ?

C10 H10B 0.9600 . ?

C10 H10C 0.9600 . ?

C11 H11A 0.9600 . ?

C11 H11B 0.9600 . ?

C11 H11C 0.9600 . ?

C12 H12A 0.9600 . ?

C12 H12B 0.9600 . ?

C12 H12C 0.9600 . ?

C13 H13A 0.9600 . ?

C13 H13B 0.9600 . ?

C13 H13C 0.9600 . ?

C14 H14A 0.9600 . ?

C14 H14B 0.9600 . ?

C14 H14C 0.9600 . ?

C15 H15A 0.9600 . ?

C15 H15B 0.9600 . ?

C15 H15C 0.9600 . ?

C16 C17 1.388(7) . ?

C16 C21 1.399(7) . ?

C17 C18 1.401(8) . ?

C17 H17A 0.9300 . ?

C18 C19 1.379(9) . ?

C18 H18A 0.9300 . ?

C19 C20 1.355(9) . ?

C19 H19A 0.9300 . ?

C20 C21 1.381(6) . ?

C20 H20A 0.9300 . ?

C21 H21A 0.9300 . ?

C22 C23 1.401(8) . ?

C22 C27 1.406(7) . ?

C23 C24 1.401(9) . ?

C23 H23A 0.9300 . ?

C24 C25 1.393(9) . ?

C24 H24A 0.9300 . ?

C25 C26 1.281(9) . ?

C25 H25A 0.9300 . ?

C26 C27 1.431(9) . ?

C26 H26A 0.9300 . ?

C27 H27A 0.9300 . ?

C28 C33 1.365(7) . ?

C28 C29 1.389(7) . ?

C29 C30 1.377(8) . ?

C29 H29A 0.9300 . ?

C30 C31 1.350(9) . ?

C30 H30A 0.9300 . ?

C31 C32 1.388(9) . ?

C31 H31A 0.9300 . ?

C32 C33 1.364(8) . ?

C32 H32A 0.9300 . ?

C33 H33A 0.9300 . ?

C34 C39 1.385(7) . ?

C34 C35 1.401(8) . ?

C35 C36 1.370(9) . ?

C35 H35A 0.9300 . ?

C36 C37 1.353(9) . ?

C36 H36A 0.9300 . ?

C37 C38 1.378(9) . ?

C37 H37A 0.9300 . ?

C38 C39 1.391(8) . ?

C38 H38A 0.9300 . ?

C39 H39A 0.9300 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag

C3 W1 C2 88.8(2) . . ?

C3 W1 C5 88.9(2) . . ?

C2 W1 C5 177.1(2) . . ?

C3 W1 C1 88.4(2) . . ?

C2 W1 C1 88.9(2) . . ?

C5 W1 C1 89.3(2) . . ?

C3 W1 C4 91.3(2) . . ?

C2 W1 C4 88.4(2) . . ?

C5 W1 C4 93.4(2) . . ?

C1 W1 C4 177.3(2) . . ?

C3 W1 Ge1 176.66(15) . . ?

C2 W1 Ge1 94.24(17) . . ?

C5 W1 Ge1 88.09(16) . . ?

C1 W1 Ge1 92.97(16) . . ?

C4 W1 Ge1 87.52(16) . . ?

C7 W2 C6 90.3(2) . . ?

C7 W2 C8 76.5(2) . . ?

C6 W2 C8 82.1(2) . . ?

C7 W2 N2 117.70(18) . . ?

C6 W2 N2 151.47(18) . . ?

C8 W2 N2 98.49(18) . . ?

C7 W2 C9 117.53(19) . . ?

C6 W2 C9 102.16(18) . . ?

C8 W2 C9 164.96(18) . . ?

N2 W2 C9 70.82(13) . . ?

C7 W2 Ge1 75.11(14) . . ?

C6 W2 Ge1 79.22(15) . . ?

C8 W2 Ge1 145.73(15) . . ?

N2 W2 Ge1 111.54(10) . . ?

C9 W2 Ge1 48.93(10) . . ?

C7 W2 P2 119.58(16) . . ?

C6 W2 P2 136.42(16) . . ?

C8 W2 P2 132.45(16) . . ?

N2 W2 P2 33.98(10) . . ?

C9 W2 P2 37.46(9) . . ?

Ge1 W2 P2 79.16(3) . . ?

N1 Ge1 C9 77.55(15) . . ?

N1 Ge1 W1 123.50(11) . . ?

C9 Ge1 W1 135.60(12) . . ?

N1 Ge1 W2 103.39(11) . . ?

C9 Ge1 W2 56.67(11) . . ?

W1 Ge1 W2 132.513(19) . . ?

N1 Ge1 P1 37.67(10) . . ?

C9 Ge1 P1 41.33(11) . . ?

W1 Ge1 P1 135.93(3) . . ?

W2 Ge1 P1 85.75(3) . . ?

N1 Si1 C11 113.2(3) . . ?

N1 Si1 C10 106.7(2) . . ?

C11 Si1 C10 112.2(4) . . ?

N1 Si1 C12 111.6(2) . . ?

C11 Si1 C12 105.1(4) . . ?

C10 Si1 C12 108.0(4) . . ?

N2 Si2 C14 107.3(2) . . ?

N2 Si2 C13 109.7(2) . . ?

C14 Si2 C13 109.2(3) . . ?

N2 Si2 C15 110.6(2) . . ?

C14 Si2 C15 110.7(3) . . ?

C13 Si2 C15 109.3(3) . . ?

N1 P1 C9 97.42(18) . . ?

N1 P1 C34 112.5(2) . . ?

C9 P1 C34 109.4(2) . . ?

N1 P1 C28 112.8(2) . . ?

C9 P1 C28 117.5(2) . . ?

C34 P1 C28 107.2(2) . . ?

N1 P1 Ge1 49.15(13) . . ?

C9 P1 Ge1 50.33(13) . . ?

C34 P1 Ge1 111.13(16) . . ?

C28 P1 Ge1 141.58(16) . . ?

N2 P2 C9 100.30(19) . . ?

N2 P2 C22 113.2(2) . . ?

C9 P2 C22 112.0(2) . . ?

N2 P2 C16 112.3(2) . . ?

C9 P2 C16 112.43(19) . . ?

C22 P2 C16 106.7(2) . . ?

N2 P2 W2 48.50(12) . . ?

C9 P2 W2 52.86(14) . . ?

C22 P2 W2 118.25(15) . . ?

C16 P2 W2 134.98(17) . . ?

P1 N1 Si1 135.1(2) . . ?

P1 N1 Ge1 93.19(17) . . ?

Si1 N1 Ge1 131.6(2) . . ?

P2 N2 Si2 132.4(2) . . ?

P2 N2 W2 97.51(15) . . ?

Si2 N2 W2 130.0(2) . . ?

O1 C1 W1 175.5(5) . . ?

O2 C2 W1 177.7(6) . . ?

O3 C3 W1 177.4(5) . . ?

O4 C4 W1 177.3(5) . . ?

O5 C5 W1 175.3(5) . . ?

O6 C6 W2 175.2(5) . . ?

O7 C7 W2 176.8(4) . . ?

O8 C8 W2 176.3(5) . . ?

P2 C9 P1 133.3(2) . . ?

P2 C9 Ge1 134.3(2) . . ?

P1 C9 Ge1 88.34(15) . . ?

P2 C9 W2 89.68(16) . . ?

P1 C9 W2 125.6(2) . . ?

Ge1 C9 W2 74.39(13) . . ?

Si1 C10 H10A 109.5 . . ?

Si1 C10 H10B 109.5 . . ?

H10A C10 H10B 109.5 . . ?

Si1 C10 H10C 109.5 . . ?

H10A C10 H10C 109.5 . . ?

H10B C10 H10C 109.5 . . ?

Si1 C11 H11A 109.5 . . ?

Si1 C11 H11B 109.5 . . ?

H11A C11 H11B 109.5 . . ?

Si1 C11 H11C 109.5 . . ?

H11A C11 H11C 109.5 . . ?

H11B C11 H11C 109.5 . . ?

Si1 C12 H12A 109.5 . . ?

Si1 C12 H12B 109.5 . . ?

H12A C12 H12B 109.5 . . ?

Si1 C12 H12C 109.5 . . ?

H12A C12 H12C 109.5 . . ?

H12B C12 H12C 109.5 . . ?

Si2 C13 H13A 109.5 . . ?

Si2 C13 H13B 109.5 . . ?

H13A C13 H13B 109.5 . . ?

Si2 C13 H13C 109.5 . . ?

H13A C13 H13C 109.5 . . ?

H13B C13 H13C 109.5 . . ?

Si2 C14 H14A 109.5 . . ?

Si2 C14 H14B 109.5 . . ?

H14A C14 H14B 109.5 . . ?

Si2 C14 H14C 109.5 . . ?

H14A C14 H14C 109.5 . . ?

H14B C14 H14C 109.5 . . ?

Si2 C15 H15A 109.5 . . ?

Si2 C15 H15B 109.5 . . ?

H15A C15 H15B 109.5 . . ?

Si2 C15 H15C 109.5 . . ?

H15A C15 H15C 109.5 . . ?

H15B C15 H15C 109.5 . . ?

C17 C16 C21 119.2(4) . . ?

C17 C16 P2 122.7(4) . . ?

C21 C16 P2 118.0(3) . . ?

C16 C17 C18 119.9(6) . . ?

C16 C17 H17A 120.0 . . ?

C18 C17 H17A 120.0 . . ?

C19 C18 C17 119.1(6) . . ?

C19 C18 H18A 120.5 . . ?

C17 C18 H18A 120.5 . . ?

C20 C19 C18 121.4(5) . . ?

C20 C19 H19A 119.3 . . ?

C18 C19 H19A 119.3 . . ?

C19 C20 C21 120.4(6) . . ?

C19 C20 H20A 119.8 . . ?

C21 C20 H20A 119.8 . . ?

C20 C21 C16 120.0(5) . . ?

C20 C21 H21A 120.0 . . ?

C16 C21 H21A 120.0 . . ?

C23 C22 C27 117.6(5) . . ?

C23 C22 P2 120.4(4) . . ?

C27 C22 P2 122.0(4) . . ?

C24 C23 C22 119.9(6) . . ?

C24 C23 H23A 120.1 . . ?

C22 C23 H23A 120.1 . . ?

C25 C24 C23 121.7(7) . . ?

C25 C24 H24A 119.2 . . ?

C23 C24 H24A 119.2 . . ?

C26 C25 C24 117.9(7) . . ?

C26 C25 H25A 121.1 . . ?

C24 C25 H25A 121.1 . . ?

C25 C26 C27 124.8(7) . . ?

C25 C26 H26A 117.6 . . ?

C27 C26 H26A 117.6 . . ?

C22 C27 C26 118.1(6) . . ?

C22 C27 H27A 121.0 . . ?

C26 C27 H27A 121.0 . . ?

C33 C28 C29 117.8(5) . . ?

C33 C28 P1 119.8(4) . . ?

C29 C28 P1 122.4(4) . . ?

C30 C29 C28 122.4(5) . . ?

C30 C29 H29A 118.8 . . ?

C28 C29 H29A 118.8 . . ?

C31 C30 C29 117.9(6) . . ?

C31 C30 H30A 121.1 . . ?

C29 C30 H30A 121.1 . . ?

C30 C31 C32 121.3(6) . . ?

C30 C31 H31A 119.3 . . ?

C32 C31 H31A 119.3 . . ?

C33 C32 C31 119.5(6) . . ?

C33 C32 H32A 120.3 . . ?

C31 C32 H32A 120.3 . . ?

C32 C33 C28 121.1(5) . . ?

C32 C33 H33A 119.5 . . ?

C28 C33 H33A 119.5 . . ?

C39 C34 C35 118.2(5) . . ?

C39 C34 P1 121.9(4) . . ?

C35 C34 P1 119.2(4) . . ?

C36 C35 C34 118.9(6) . . ?

C36 C35 H35A 120.5 . . ?

C34 C35 H35A 120.5 . . ?

C37 C36 C35 122.9(7) . . ?

C37 C36 H36A 118.5 . . ?

C35 C36 H36A 118.5 . . ?

C36 C37 C38 119.1(6) . . ?

C36 C37 H37A 120.4 . . ?

C38 C37 H37A 120.4 . . ?

C37 C38 C39 119.3(6) . . ?

C37 C38 H38A 120.3 . . ?

C39 C38 H38A 120.3 . . ?

C34 C39 C38 121.3(6) . . ?

C34 C39 H39A 119.4 . . ?

C38 C39 H39A 119.4 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

C3 W1 Ge1 N1 170(3) . . . . ?

C2 W1 Ge1 N1 13.3(2) . . . . ?

C5 W1 Ge1 N1 -164.95(19) . . . . ?

C1 W1 Ge1 N1 -75.8(2) . . . . ?

C4 W1 Ge1 N1 101.52(19) . . . . ?

C3 W1 Ge1 C9 -82(3) . . . . ?

C2 W1 Ge1 C9 121.2(2) . . . . ?

C5 W1 Ge1 C9 -57.1(2) . . . . ?

C1 W1 Ge1 C9 32.1(2) . . . . ?

C4 W1 Ge1 C9 -150.6(2) . . . . ?

C3 W1 Ge1 W2 0(3) . . . . ?

C2 W1 Ge1 W2 -156.26(17) . . . . ?

C5 W1 Ge1 W2 25.48(14) . . . . ?

C1 W1 Ge1 W2 114.64(17) . . . . ?

C4 W1 Ge1 W2 -68.05(14) . . . . ?

C3 W1 Ge1 P1 -143(3) . . . . ?

C2 W1 Ge1 P1 60.38(17) . . . . ?

C5 W1 Ge1 P1 -117.88(15) . . . . ?

C1 W1 Ge1 P1 -28.71(17) . . . . ?

C4 W1 Ge1 P1 148.59(15) . . . . ?

C7 W2 Ge1 N1 -144.95(19) . . . . ?

C6 W2 Ge1 N1 -51.7(2) . . . . ?

C8 W2 Ge1 N1 -109.8(3) . . . . ?

N2 W2 Ge1 N1 100.72(15) . . . . ?

C9 W2 Ge1 N1 65.06(17) . . . . ?

P2 W2 Ge1 N1 90.23(11) . . . . ?

C7 W2 Ge1 C9 150.0(2) . . . . ?

C6 W2 Ge1 C9 -116.8(2) . . . . ?

C8 W2 Ge1 C9 -174.9(3) . . . . ?

N2 W2 Ge1 C9 35.66(16) . . . . ?

P2 W2 Ge1 C9 25.17(13) . . . . ?

C7 W2 Ge1 W1 26.13(16) . . . . ?

C6 W2 Ge1 W1 119.37(16) . . . . ?

C8 W2 Ge1 W1 61.2(3) . . . . ?

N2 W2 Ge1 W1 -88.21(10) . . . . ?

C9 W2 Ge1 W1 -123.87(13) . . . . ?

P2 W2 Ge1 W1 -98.70(3) . . . . ?

C7 W2 Ge1 P1 -178.47(16) . . . . ?

C6 W2 Ge1 P1 -85.23(16) . . . . ?

C8 W2 Ge1 P1 -143.4(3) . . . . ?

N2 W2 Ge1 P1 67.19(10) . . . . ?

C9 W2 Ge1 P1 31.54(13) . . . . ?

P2 W2 Ge1 P1 56.71(3) . . . . ?

C9 Ge1 P1 N1 159.9(3) . . . . ?

W1 Ge1 P1 N1 -87.73(19) . . . . ?

W2 Ge1 P1 N1 118.45(18) . . . . ?

N1 Ge1 P1 C9 -159.9(3) . . . . ?

W1 Ge1 P1 C9 112.39(19) . . . . ?

W2 Ge1 P1 C9 -41.44(18) . . . . ?

N1 Ge1 P1 C34 102.0(3) . . . . ?

C9 Ge1 P1 C34 -98.1(3) . . . . ?

W1 Ge1 P1 C34 14.28(18) . . . . ?

W2 Ge1 P1 C34 -139.54(17) . . . . ?

N1 Ge1 P1 C28 -74.5(3) . . . . ?

C9 Ge1 P1 C28 85.4(3) . . . . ?

W1 Ge1 P1 C28 -162.2(2) . . . . ?

W2 Ge1 P1 C28 43.9(2) . . . . ?

C7 W2 P2 N2 96.6(2) . . . . ?

C6 W2 P2 N2 -136.1(3) . . . . ?

C8 W2 P2 N2 -2.4(3) . . . . ?

C9 W2 P2 N2 -165.8(3) . . . . ?

Ge1 W2 P2 N2 162.37(18) . . . . ?

C7 W2 P2 C9 -97.6(2) . . . . ?

C6 W2 P2 C9 29.7(3) . . . . ?

C8 W2 P2 C9 163.4(3) . . . . ?

N2 W2 P2 C9 165.8(3) . . . . ?

Ge1 W2 P2 C9 -31.82(18) . . . . ?

C7 W2 P2 C22 -0.4(2) . . . . ?

C6 W2 P2 C22 126.9(3) . . . . ?

C8 W2 P2 C22 -99.4(3) . . . . ?

N2 W2 P2 C22 -96.9(2) . . . . ?

C9 W2 P2 C22 97.2(3) . . . . ?

Ge1 W2 P2 C22 65.43(18) . . . . ?

C7 W2 P2 C16 177.0(3) . . . . ?

C6 W2 P2 C16 -55.7(3) . . . . ?

C8 W2 P2 C16 78.0(3) . . . . ?

N2 W2 P2 C16 80.4(3) . . . . ?

C9 W2 P2 C16 -85.4(3) . . . . ?

Ge1 W2 P2 C16 -117.2(2) . . . . ?

C9 P1 N1 Si1 -161.3(3) . . . . ?

C34 P1 N1 Si1 84.1(4) . . . . ?

C28 P1 N1 Si1 -37.3(4) . . . . ?

Ge1 P1 N1 Si1 -176.8(4) . . . . ?

C9 P1 N1 Ge1 15.5(2) . . . . ?

C34 P1 N1 Ge1 -99.1(2) . . . . ?

C28 P1 N1 Ge1 139.50(18) . . . . ?

C11 Si1 N1 P1 -69.8(5) . . . . ?

C10 Si1 N1 P1 166.3(4) . . . . ?

C12 Si1 N1 P1 48.5(5) . . . . ?

C11 Si1 N1 Ge1 114.4(4) . . . . ?

C10 Si1 N1 Ge1 -9.4(4) . . . . ?

C12 Si1 N1 Ge1 -127.2(4) . . . . ?

C9 Ge1 N1 P1 -13.45(17) . . . . ?

W1 Ge1 N1 P1 123.55(12) . . . . ?

W2 Ge1 N1 P1 -64.34(16) . . . . ?

C9 Ge1 N1 Si1 163.5(3) . . . . ?

W1 Ge1 N1 Si1 -59.5(3) . . . . ?

W2 Ge1 N1 Si1 112.7(3) . . . . ?

P1 Ge1 N1 Si1 177.0(4) . . . . ?

C9 P2 N2 Si2 165.1(3) . . . . ?

C22 P2 N2 Si2 -75.4(3) . . . . ?

C16 P2 N2 Si2 45.5(4) . . . . ?

W2 P2 N2 Si2 176.6(4) . . . . ?

C9 P2 N2 W2 -11.5(2) . . . . ?

C22 P2 N2 W2 108.0(2) . . . . ?

C16 P2 N2 W2 -131.05(18) . . . . ?

C14 Si2 N2 P2 -116.5(3) . . . . ?

C13 Si2 N2 P2 125.0(4) . . . . ?

C15 Si2 N2 P2 4.4(4) . . . . ?

C14 Si2 N2 W2 59.1(3) . . . . ?

C13 Si2 N2 W2 -59.4(4) . . . . ?

C15 Si2 N2 W2 180.0(3) . . . . ?

C7 W2 N2 P2 -102.6(2) . . . . ?

C6 W2 N2 P2 89.1(4) . . . . ?

C8 W2 N2 P2 178.2(2) . . . . ?

C9 W2 N2 P2 9.09(16) . . . . ?

Ge1 W2 N2 P2 -18.65(18) . . . . ?

C7 W2 N2 Si2 80.6(3) . . . . ?

C6 W2 N2 Si2 -87.6(4) . . . . ?

C8 W2 N2 Si2 1.5(3) . . . . ?

C9 W2 N2 Si2 -167.6(3) . . . . ?

Ge1 W2 N2 Si2 164.6(2) . . . . ?

P2 W2 N2 Si2 -176.7(4) . . . . ?

C3 W1 C1 O1 -1(7) . . . . ?

C2 W1 C1 O1 88(7) . . . . ?

C5 W1 C1 O1 -90(7) . . . . ?

C4 W1 C1 O1 82(9) . . . . ?

Ge1 W1 C1 O1 -178(100) . . . . ?

C3 W1 C2 O2 56(13) . . . . ?

C5 W1 C2 O2 17(16) . . . . ?

C1 W1 C2 O2 -33(13) . . . . ?

C4 W1 C2 O2 147(13) . . . . ?

Ge1 W1 C2 O2 -126(13) . . . . ?

C2 W1 C3 O3 -88(11) . . . . ?

C5 W1 C3 O3 90(11) . . . . ?

C1 W1 C3 O3 0(11) . . . . ?

C4 W1 C3 O3 -177(100) . . . . ?

Ge1 W1 C3 O3 115(10) . . . . ?

C3 W1 C4 O4 85(12) . . . . ?

C2 W1 C4 O4 -4(12) . . . . ?

C5 W1 C4 O4 174(100) . . . . ?

C1 W1 C4 O4 2(15) . . . . ?

Ge1 W1 C4 O4 -98(12) . . . . ?

C3 W1 C5 O5 -23(5) . . . . ?

C2 W1 C5 O5 15(8) . . . . ?

C1 W1 C5 O5 65(5) . . . . ?

C4 W1 C5 O5 -115(5) . . . . ?

Ge1 W1 C5 O5 158(5) . . . . ?

C7 W2 C6 O6 -113(6) . . . . ?

C8 W2 C6 O6 -37(6) . . . . ?

N2 W2 C6 O6 56(6) . . . . ?

C9 W2 C6 O6 128(6) . . . . ?

Ge1 W2 C6 O6 172(6) . . . . ?

P2 W2 C6 O6 110(6) . . . . ?

C6 W2 C7 O7 154(8) . . . . ?

C8 W2 C7 O7 72(8) . . . . ?

N2 W2 C7 O7 -21(8) . . . . ?

C9 W2 C7 O7 -102(8) . . . . ?

Ge1 W2 C7 O7 -128(8) . . . . ?

P2 W2 C7 O7 -60(8) . . . . ?

C7 W2 C8 O8 28(9) . . . . ?

C6 W2 C8 O8 -64(9) . . . . ?

N2 W2 C8 O8 145(9) . . . . ?

C9 W2 C8 O8 -172(8) . . . . ?

Ge1 W2 C8 O8 -7(9) . . . . ?

P2 W2 C8 O8 146(8) . . . . ?

N2 P2 C9 P1 -131.9(3) . . . . ?

C22 P2 C9 P1 107.8(4) . . . . ?

C16 P2 C9 P1 -12.4(4) . . . . ?

W2 P2 C9 P1 -142.7(4) . . . . ?

N2 P2 C9 Ge1 78.3(3) . . . . ?

C22 P2 C9 Ge1 -42.0(4) . . . . ?

C16 P2 C9 Ge1 -162.1(3) . . . . ?

W2 P2 C9 Ge1 67.6(3) . . . . ?

N2 P2 C9 W2 10.76(19) . . . . ?

C22 P2 C9 W2 -109.5(2) . . . . ?

C16 P2 C9 W2 130.3(2) . . . . ?

N1 P1 C9 P2 -174.1(4) . . . . ?

C34 P1 C9 P2 -57.0(4) . . . . ?

C28 P1 C9 P2 65.4(4) . . . . ?

Ge1 P1 C9 P2 -158.9(4) . . . . ?

N1 P1 C9 Ge1 -15.2(2) . . . . ?

C34 P1 C9 Ge1 101.8(2) . . . . ?

C28 P1 C9 Ge1 -135.72(19) . . . . ?

N1 P1 C9 W2 54.2(3) . . . . ?

C34 P1 C9 W2 171.2(2) . . . . ?

C28 P1 C9 W2 -66.3(3) . . . . ?

Ge1 P1 C9 W2 69.4(2) . . . . ?

N1 Ge1 C9 P2 170.9(4) . . . . ?

W1 Ge1 C9 P2 45.3(4) . . . . ?

W2 Ge1 C9 P2 -73.7(3) . . . . ?

P1 Ge1 C9 P2 158.5(4) . . . . ?

N1 Ge1 C9 P1 12.43(16) . . . . ?

W1 Ge1 C9 P1 -113.19(14) . . . . ?

W2 Ge1 C9 P1 127.8(2) . . . . ?

N1 Ge1 C9 W2 -115.40(15) . . . . ?

W1 Ge1 C9 W2 118.98(11) . . . . ?

P1 Ge1 C9 W2 -127.8(2) . . . . ?

C7 W2 C9 P2 103.6(2) . . . . ?

C6 W2 C9 P2 -159.6(2) . . . . ?

C8 W2 C9 P2 -54.5(8) . . . . ?

N2 W2 C9 P2 -8.34(15) . . . . ?

Ge1 W2 C9 P2 136.6(2) . . . . ?

C7 W2 C9 P1 -109.3(3) . . . . ?

C6 W2 C9 P1 -12.5(3) . . . . ?

C8 W2 C9 P1 92.6(7) . . . . ?

N2 W2 C9 P1 138.8(3) . . . . ?

Ge1 W2 C9 P1 -76.3(2) . . . . ?

P2 W2 C9 P1 147.1(4) . . . . ?

C7 W2 C9 Ge1 -33.0(2) . . . . ?

C6 W2 C9 Ge1 63.80(19) . . . . ?

C8 W2 C9 Ge1 168.9(7) . . . . ?

N2 W2 C9 Ge1 -144.97(16) . . . . ?

P2 W2 C9 Ge1 -136.6(2) . . . . ?

N2 P2 C16 C17 -130.6(4) . . . . ?

C9 P2 C16 C17 117.2(4) . . . . ?

C22 P2 C16 C17 -6.0(5) . . . . ?

W2 P2 C16 C17 176.4(3) . . . . ?

N2 P2 C16 C21 51.6(4) . . . . ?

C9 P2 C16 C21 -60.7(4) . . . . ?

C22 P2 C16 C21 176.1(3) . . . . ?

W2 P2 C16 C21 -1.4(5) . . . . ?

C21 C16 C17 C18 3.2(8) . . . . ?

P2 C16 C17 C18 -174.7(4) . . . . ?

C16 C17 C18 C19 -2.8(9) . . . . ?

C17 C18 C19 C20 1.7(10) . . . . ?

C18 C19 C20 C21 -1.0(9) . . . . ?

C19 C20 C21 C16 1.4(8) . . . . ?

C17 C16 C21 C20 -2.5(7) . . . . ?

P2 C16 C21 C20 175.5(4) . . . . ?

N2 P2 C22 C23 -169.8(4) . . . . ?

C9 P2 C22 C23 -57.3(5) . . . . ?

C16 P2 C22 C23 66.1(5) . . . . ?

W2 P2 C22 C23 -115.9(4) . . . . ?

N2 P2 C22 C27 9.4(5) . . . . ?

C9 P2 C22 C27 121.9(4) . . . . ?

C16 P2 C22 C27 -114.7(4) . . . . ?

W2 P2 C22 C27 63.3(4) . . . . ?

C27 C22 C23 C24 3.1(8) . . . . ?

P2 C22 C23 C24 -177.7(5) . . . . ?

C22 C23 C24 C25 -2.4(11) . . . . ?

C23 C24 C25 C26 0.7(13) . . . . ?

C24 C25 C26 C27 0.2(13) . . . . ?

C23 C22 C27 C26 -2.2(8) . . . . ?

P2 C22 C27 C26 178.5(5) . . . . ?

C25 C26 C27 C22 0.6(11) . . . . ?

N1 P1 C28 C33 -71.2(4) . . . . ?

C9 P1 C28 C33 40.9(4) . . . . ?

C34 P1 C28 C33 164.4(4) . . . . ?

Ge1 P1 C28 C33 -19.0(5) . . . . ?

N1 P1 C28 C29 110.0(4) . . . . ?

C9 P1 C28 C29 -137.9(4) . . . . ?

C34 P1 C28 C29 -14.4(5) . . . . ?

Ge1 P1 C28 C29 162.2(3) . . . . ?

C33 C28 C29 C30 -1.3(8) . . . . ?

P1 C28 C29 C30 177.6(5) . . . . ?

C28 C29 C30 C31 1.0(9) . . . . ?

C29 C30 C31 C32 1.1(10) . . . . ?

C30 C31 C32 C33 -3.0(10) . . . . ?

C31 C32 C33 C28 2.6(8) . . . . ?

C29 C28 C33 C32 -0.6(7) . . . . ?

P1 C28 C33 C32 -179.4(4) . . . . ?

N1 P1 C34 C39 -176.6(4) . . . . ?

C9 P1 C34 C39 76.4(4) . . . . ?

C28 P1 C34 C39 -52.0(5) . . . . ?

Ge1 P1 C34 C39 130.2(4) . . . . ?

N1 P1 C34 C35 13.0(5) . . . . ?

C9 P1 C34 C35 -94.1(5) . . . . ?

C28 P1 C34 C35 137.5(4) . . . . ?

Ge1 P1 C34 C35 -40.2(5) . . . . ?

C39 C34 C35 C36 0.4(8) . . . . ?

P1 C34 C35 C36 171.2(5) . . . . ?

C34 C35 C36 C37 -3.5(11) . . . . ?

C35 C36 C37 C38 4.7(12) . . . . ?

C36 C37 C38 C39 -2.8(11) . . . . ?

C35 C34 C39 C38 1.4(8) . . . . ?

P1 C34 C39 C38 -169.2(5) . . . . ?

C37 C38 C39 C34 -0.2(10) . . . . ?



_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.54

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         1.149

_refine_diff_density_min         -1.099

_refine_diff_density_rms         0.315



data_scw178

_database_code_CSD               188277



_audit_creation_method           SHELXL-97

_chemical_name_systematic        

; 

? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C42 H59 Mo N2 O5 P2 Si2'

_chemical_formula_weight         885.97



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Triclinic

_symmetry_space_group_name_H-M   p-1



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-x, -y, -z'



_cell_length_a                   11.1278(11)

_cell_length_b                   14.2454(13)

_cell_length_c                   16.2005(15)

_cell_angle_alpha                98.922(2)

_cell_angle_beta                 95.369(2)

_cell_angle_gamma                110.193(2)

_cell_volume                     2350.9(4)

_cell_formula_units_Z            2

_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       needle

_exptl_crystal_colour            ?

_exptl_crystal_size_max          1.50

_exptl_crystal_size_mid          0.72

_exptl_crystal_size_min          0.65

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.252

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             930

_exptl_absorpt_coefficient_mu    0.439

_exptl_absorpt_correction_type   SADABS

_exptl_absorpt_correction_T_min  0.5588

_exptl_absorpt_correction_T_max  0.7634

_exptl_absorpt_process_details   ?



_exptl_special_details           

; 

? 

;



_diffrn_ambient_temperature      293(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  ?

_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            15832

_diffrn_reflns_av_R_equivalents  0.0158

_diffrn_reflns_av_sigmaI/netI    0.0292

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -12

_diffrn_reflns_limit_k_max       18

_diffrn_reflns_limit_l_min       -21

_diffrn_reflns_limit_l_max       20

_diffrn_reflns_theta_min         1.55

_diffrn_reflns_theta_max         28.03

_reflns_number_total             11098

_reflns_number_gt                9410

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_refine_special_details          

; 

Refinement of F² against ALL reflections.  The weighted R-factor wR and 

goodness of fit S are based on F², conventional R-factors R are based 

on F, with F set to zero for negative F². The threshold expression of 

F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 

not relevant to the choice of reflections for refinement.  R-factors based 

on F² are statistically about twice as large as those based on F, and R- 

factors based on ALL data will be even larger. 

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     

'calc w=1/[σ²(Fo²)+(0.0772P)²+1.3708P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         11098

_refine_ls_number_parameters     487

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0499

_refine_ls_R_factor_gt           0.0429

_refine_ls_wR_factor_ref         0.1282

_refine_ls_wR_factor_gt          0.1219

_refine_ls_goodness_of_fit_ref   1.037

_refine_ls_restrained_S_all      1.037

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

Mo1 Mo 0.241860(18) 0.312975(14) 0.282715(12) 0.03131(7) Uani 1 1 d . . .

Si1 Si 0.12002(8) 0.03739(6) 0.22077(6) 0.04780(19) Uani 1 1 d . . .

Si2 Si 0.24154(8) 0.37143(6) 0.07373(5) 0.04578(17) Uani 1 1 d . . .

P1 P -0.02871(6) 0.17684(4) 0.26861(4) 0.03172(13) Uani 1 1 d . . .

P2 P 0.04410(6) 0.36743(4) 0.19379(4) 0.03373(13) Uani 1 1 d . . .

N1 N 0.0843(2) 0.14538(15) 0.23636(13) 0.0350(4) Uani 1 1 d . . .

N2 N 0.1538(2) 0.33851(16) 0.15334(13) 0.0367(4) Uani 1 1 d . . .

O1 O 0.3465(2) 0.30689(18) 0.46473(13) 0.0571(5) Uani 1 1 d . . .

O2 O 0.4987(2) 0.2930(2) 0.23970(18) 0.0763(8) Uani 1 1 d . . .

O3 O 0.4254(2) 0.53083(16) 0.36836(15) 0.0614(6) Uani 1 1 d . . .

O4 O 0.3712(3) 0.6733(2) 0.51137(17) 0.0696(6) Uani 1 1 d . . .

O5 O 0.5793(2) 0.74328(19) 0.35927(17) 0.0679(6) Uani 1 1 d . . .

C1 C 0.3010(2) 0.30242(19) 0.39392(17) 0.0389(5) Uani 1 1 d . . .

C2 C 0.4009(3) 0.2975(2) 0.25348(18) 0.0451(6) Uani 1 1 d . . .

C3 C 0.3513(3) 0.4501(2) 0.33097(17) 0.0405(5) Uani 1 1 d . . .

C4 C 0.0230(2) 0.30970(17) 0.28185(15) 0.0328(4) Uani 1 1 d . . .

H4A H 0.0047 0.3469 0.3322 0.039 Uiso 1 1 calc R . .

C5 C 0.1647(7) 0.0164(4) 0.1151(4) 0.124(3) Uani 1 1 d . . .

H5A H 0.2338 0.0764 0.1087 0.186 Uiso 1 1 calc R . .

H5B H 0.0908 0.0024 0.0729 0.186 Uiso 1 1 calc R . .

H5C H 0.1927 -0.0406 0.1085 0.186 Uiso 1 1 calc R . .

C6 C 0.2609(4) 0.0501(3) 0.2995(4) 0.0911(15) Uani 1 1 d . . .

H6A H 0.3332 0.1101 0.2972 0.137 Uiso 1 1 calc R . .

H6B H 0.2840 -0.0089 0.2867 0.137 Uiso 1 1 calc R . .

H6C H 0.2379 0.0556 0.3553 0.137 Uiso 1 1 calc R . .

C7 C -0.0151(4) -0.0821(2) 0.2305(3) 0.0750(11) Uani 1 1 d . . .

H7A H -0.0904 -0.0927 0.1908 0.113 Uiso 1 1 calc R . .

H7B H -0.0353 -0.0750 0.2869 0.113 Uiso 1 1 calc R . .

H7C H 0.0117 -0.1394 0.2187 0.113 Uiso 1 1 calc R . .

C8 C 0.1502(5) 0.3987(4) -0.0172(3) 0.0889(14) Uani 1 1 d . . .

H8A H 0.1236 0.4544 0.0028 0.133 Uiso 1 1 calc R . .

H8B H 0.0751 0.3391 -0.0419 0.133 Uiso 1 1 calc R . .

H8C H 0.2053 0.4166 -0.0590 0.133 Uiso 1 1 calc R . .

C9 C 0.2887(5) 0.2633(3) 0.0290(3) 0.0810(12) Uani 1 1 d . . .

H9A H 0.3360 0.2464 0.0733 0.121 Uiso 1 1 calc R . .

H9B H 0.3422 0.2825 -0.0133 0.121 Uiso 1 1 calc R . .

H9C H 0.2121 0.2051 0.0039 0.121 Uiso 1 1 calc R . .

C10 C 0.3914(4) 0.4856(3) 0.1139(3) 0.0859(13) Uani 1 1 d . . .

H10A H 0.4402 0.4739 0.1607 0.129 Uiso 1 1 calc R . .

H10B H 0.3687 0.5438 0.1321 0.129 Uiso 1 1 calc R . .

H10C H 0.4429 0.4980 0.0695 0.129 Uiso 1 1 calc R . .

C11 C 0.3252(5) 0.5819(5) 0.5501(4) 0.1017(16) Uani 1 1 d . . .

H11A H 0.3338 0.5247 0.5133 0.122 Uiso 1 1 calc R . .

H11B H 0.3811 0.5947 0.6035 0.122 Uiso 1 1 calc R . .

C12 C 0.1941(7) 0.5537(7) 0.5649(5) 0.162(3) Uani 1 1 d . . .

H12A H 0.1718 0.4944 0.5900 0.243 Uiso 1 1 calc R . .

H12B H 0.1375 0.5388 0.5122 0.243 Uiso 1 1 calc R . .

H12C H 0.1849 0.6090 0.6025 0.243 Uiso 1 1 calc R . .

C13 C 0.3823(6) 0.7667(4) 0.5630(3) 0.0991(16) Uani 1 1 d . . .

H13A H 0.4337 0.7761 0.6175 0.119 Uiso 1 1 calc R . .

H13B H 0.2969 0.7652 0.5724 0.119 Uiso 1 1 calc R . .

C14 C 0.4441(7) 0.8516(4) 0.5219(4) 0.1122(18) Uani 1 1 d . . .

H14A H 0.4510 0.9146 0.5570 0.168 Uiso 1 1 calc R . .

H14B H 0.3926 0.8424 0.4682 0.168 Uiso 1 1 calc R . .

H14C H 0.5291 0.8535 0.5134 0.168 Uiso 1 1 calc R . .

C15 C 0.7033(5) 0.7501(4) 0.3381(4) 0.0981(15) Uani 1 1 d . . .

H15A H 0.7289 0.8011 0.3033 0.118 Uiso 1 1 calc R . .

H15B H 0.7655 0.7748 0.3900 0.118 Uiso 1 1 calc R . .

C16 C 0.7126(7) 0.6590(6) 0.2951(6) 0.172(4) Uani 1 1 d . . .

H16A H 0.8000 0.6722 0.2850 0.258 Uiso 1 1 calc R . .

H16B H 0.6549 0.6353 0.2420 0.258 Uiso 1 1 calc R . .

H16C H 0.6892 0.6079 0.3290 0.258 Uiso 1 1 calc R . .

C17 C 0.4850(5) 0.7389(4) 0.2907(3) 0.0953(15) Uani 1 1 d . . .

H17A H 0.3994 0.7124 0.3064 0.114 Uiso 1 1 calc R . .

H17B H 0.4878 0.6913 0.2418 0.114 Uiso 1 1 calc R . .

C18 C 0.5034(8) 0.8365(6) 0.2668(6) 0.177(4) Uani 1 1 d . . .

H18A H 0.4369 0.8276 0.2208 0.265 Uiso 1 1 calc R . .

H18B H 0.5868 0.8626 0.2495 0.265 Uiso 1 1 calc R . .

H18C H 0.4986 0.8839 0.3143 0.265 Uiso 1 1 calc R . .

C21 C -0.0655(3) 0.1476(2) 0.37125(17) 0.0426(5) Uani 1 1 d . . .

C22 C 0.0029(3) 0.2156(3) 0.44591(19) 0.0553(7) Uani 1 1 d . . .

H22A H 0.0638 0.2790 0.4441 0.066 Uiso 1 1 calc R . .

C23 C -0.0202(4) 0.1882(4) 0.5233(2) 0.0797(12) Uani 1 1 d . . .

H23A H 0.0246 0.2342 0.5731 0.096 Uiso 1 1 calc R . .

C24 C -0.1076(5) 0.0949(4) 0.5274(3) 0.0883(14) Uani 1 1 d . . .

H24A H -0.1201 0.0768 0.5796 0.106 Uiso 1 1 calc R . .

C25 C -0.1772(5) 0.0278(3) 0.4537(3) 0.0880(14) Uani 1 1 d . . .

H25A H -0.2380 -0.0354 0.4561 0.106 Uiso 1 1 calc R . .

C26 C -0.1568(4) 0.0543(3) 0.3762(2) 0.0671(9) Uani 1 1 d . . .

H26A H -0.2049 0.0090 0.3268 0.081 Uiso 1 1 calc R . .

C31 C -0.1856(2) 0.11030(18) 0.20152(16) 0.0373(5) Uani 1 1 d . . .

C32 C -0.2057(3) 0.0355(2) 0.13138(17) 0.0453(6) Uani 1 1 d . . .

H32A H -0.1364 0.0185 0.1154 0.054 Uiso 1 1 calc R . .

C33 C -0.3289(3) -0.0151(2) 0.0841(2) 0.0560(7) Uani 1 1 d . . .

H33A H -0.3421 -0.0665 0.0374 0.067 Uiso 1 1 calc R . .

C34 C -0.4309(3) 0.0107(3) 0.1062(2) 0.0582(8) Uani 1 1 d . . .

H34A H -0.5136 -0.0244 0.0754 0.070 Uiso 1 1 calc R . .

C35 C -0.4109(3) 0.0885(3) 0.1739(2) 0.0643(9) Uani 1 1 d . . .

H35A H -0.4794 0.1078 0.1877 0.077 Uiso 1 1 calc R . .

C36 C -0.2895(3) 0.1378(3) 0.2212(2) 0.0553(7) Uani 1 1 d . . .

H36A H -0.2766 0.1903 0.2670 0.066 Uiso 1 1 calc R . .

C41 C -0.1052(3) 0.3318(2) 0.11940(17) 0.0408(5) Uani 1 1 d . . .

C42 C -0.1316(3) 0.2578(2) 0.04781(19) 0.0505(6) Uani 1 1 d . . .

H42A H -0.0710 0.2283 0.0356 0.061 Uiso 1 1 calc R . .

C43 C -0.2490(3) 0.2266(3) -0.0067(2) 0.0638(9) Uani 1 1 d . . .

H43A H -0.2655 0.1775 -0.0557 0.077 Uiso 1 1 calc R . .

C44 C -0.3398(3) 0.2679(3) 0.0117(2) 0.0680(9) Uani 1 1 d . . .

H44A H -0.4181 0.2467 -0.0246 0.082 Uiso 1 1 calc R . .

C45 C -0.3151(3) 0.3406(3) 0.0838(3) 0.0708(10) Uani 1 1 d . . .

H45A H -0.3774 0.3680 0.0965 0.085 Uiso 1 1 calc R . .

C46 C -0.1980(3) 0.3734(3) 0.1379(2) 0.0595(8) Uani 1 1 d . . .

H46A H -0.1815 0.4232 0.1865 0.071 Uiso 1 1 calc R . .

C51 C 0.0817(3) 0.50320(19) 0.23285(17) 0.0419(5) Uani 1 1 d . . .

C52 C 0.0849(4) 0.5662(2) 0.1750(2) 0.0647(9) Uani 1 1 d . . .

H52A H 0.0672 0.5384 0.1173 0.078 Uiso 1 1 calc R . .

C53 C 0.1141(5) 0.6699(3) 0.2020(3) 0.0770(11) Uani 1 1 d . . .

H53A H 0.1170 0.7113 0.1626 0.092 Uiso 1 1 calc R . .

C54 C 0.1387(4) 0.7113(2) 0.2865(3) 0.0704(10) Uani 1 1 d . . .

H54A H 0.1552 0.7804 0.3045 0.084 Uiso 1 1 calc R . .

C55 C 0.1392(4) 0.6509(3) 0.3448(2) 0.0694(10) Uani 1 1 d . . .

H55A H 0.1576 0.6792 0.4024 0.083 Uiso 1 1 calc R . .

C56 C 0.1123(4) 0.5478(2) 0.3176(2) 0.0566(8) Uani 1 1 d . . .

H56A H 0.1148 0.5077 0.3574 0.068 Uiso 1 1 calc R . .






_geom_special_details            

; 

All esds (except the esd in the dihedral angle between two l.s. planes) 

are estimated using the full covariance matrix.  The cell esds are taken 

into account individually in the estimation of esds in distances, angles 

and torsion angles; correlations between esds in cell parameters are only 

used when they are defined by crystal symmetry.  An approximate (isotropic) 

treatment of cell esds is used for estimating esds involving l.s. planes. 

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

Mo1 C3 1.901(3) . ?

Mo1 C1 1.906(3) . ?

Mo1 C2 1.950(3) . ?

Mo1 N2 2.363(2) . ?

Mo1 N1 2.376(2) . ?

Mo1 C4 2.419(2) . ?

Mo1 P2 2.9072(6) . ?

Mo1 P1 2.9294(7) . ?

Si1 N1 1.706(2) . ?

Si1 C5 1.836(4) . ?

Si1 C6 1.864(4) . ?

Si1 C7 1.882(4) . ?

Si2 N2 1.716(2) . ?

Si2 C10 1.856(4) . ?

Si2 C9 1.859(4) . ?

Si2 C8 1.877(4) . ?

P1 N1 1.579(2) . ?

P1 C4 1.749(2) . ?

P1 C31 1.819(3) . ?

P1 C21 1.825(3) . ?

P2 N2 1.581(2) . ?

P2 C4 1.749(2) . ?

P2 C41 1.823(3) . ?

P2 C51 1.824(3) . ?

O1 C1 1.193(3) . ?

O2 C2 1.151(4) . ?

O3 C3 1.186(3) . ?

O4 C13 1.418(5) . ?

O4 C11 1.484(6) . ?

O5 C15 1.428(6) . ?

O5 C17 1.434(5) . ?

C11 C12 1.428(8) . ?

C13 C14 1.463(8) . ?

C15 C16 1.417(8) . ?

C17 C18 1.453(8) . ?

C21 C26 1.386(4) . ?

C21 C22 1.391(4) . ?

C22 C23 1.390(5) . ?

C23 C24 1.365(7) . ?

C24 C25 1.379(7) . ?

C25 C26 1.383(5) . ?

C31 C32 1.375(4) . ?

C31 C36 1.391(4) . ?

C32 C33 1.392(4) . ?

C33 C34 1.369(5) . ?

C34 C35 1.374(5) . ?

C35 C36 1.374(4) . ?

C41 C42 1.374(4) . ?

C41 C46 1.390(4) . ?

C42 C43 1.394(4) . ?

C43 C44 1.367(5) . ?

C44 C45 1.371(6) . ?

C45 C46 1.388(5) . ?

C51 C56 1.378(4) . ?

C51 C52 1.390(4) . ?

C52 C53 1.386(5) . ?

C53 C54 1.365(6) . ?

C54 C55 1.374(5) . ?

C55 C56 1.382(4) . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag

C3 Mo1 C1 77.98(11) . . ?

C3 Mo1 C2 84.62(12) . . ?

C1 Mo1 C2 85.86(11) . . ?

C3 Mo1 N2 99.12(9) . . ?

C1 Mo1 N2 172.54(9) . . ?

C2 Mo1 N2 100.78(10) . . ?

C3 Mo1 N1 171.56(9) . . ?

C1 Mo1 N1 98.96(9) . . ?

C2 Mo1 N1 103.11(10) . . ?

N2 Mo1 N1 82.94(7) . . ?

C3 Mo1 C4 105.34(10) . . ?

C1 Mo1 C4 106.54(9) . . ?

C2 Mo1 C4 165.32(10) . . ?

N2 Mo1 C4 67.40(8) . . ?

N1 Mo1 C4 67.78(7) . . ?

C3 Mo1 P2 94.83(8) . . ?

C1 Mo1 P2 139.95(8) . . ?

C2 Mo1 P2 133.17(8) . . ?

N2 Mo1 P2 32.91(5) . . ?

N1 Mo1 P2 82.42(5) . . ?

C4 Mo1 P2 36.93(6) . . ?

C3 Mo1 P1 139.53(8) . . ?

C1 Mo1 P1 97.81(8) . . ?

C2 Mo1 P1 135.64(9) . . ?

N2 Mo1 P1 79.87(5) . . ?

N1 Mo1 P1 32.55(5) . . ?

C4 Mo1 P1 36.63(5) . . ?

P2 Mo1 P1 62.557(18) . . ?

N1 Si1 C5 109.60(18) . . ?

N1 Si1 C6 110.85(17) . . ?

C5 Si1 C6 107.5(3) . . ?

N1 Si1 C7 114.77(15) . . ?

C5 Si1 C7 107.9(3) . . ?

C6 Si1 C7 105.88(18) . . ?

N2 Si2 C10 111.26(16) . . ?

N2 Si2 C9 108.89(16) . . ?

C10 Si2 C9 108.4(2) . . ?

N2 Si2 C8 114.19(16) . . ?

C10 Si2 C8 107.5(2) . . ?

C9 Si2 C8 106.3(2) . . ?

N1 P1 C4 106.80(11) . . ?

N1 P1 C31 114.05(11) . . ?

C4 P1 C31 113.30(11) . . ?

N1 P1 C21 114.92(12) . . ?

C4 P1 C21 105.84(12) . . ?

C31 P1 C21 101.79(12) . . ?

N1 P1 Mo1 54.07(7) . . ?

C4 P1 Mo1 55.59(8) . . ?

C31 P1 Mo1 147.30(8) . . ?

C21 P1 Mo1 110.80(9) . . ?

N2 P2 C4 105.51(11) . . ?

N2 P2 C41 113.38(12) . . ?

C4 P2 C41 113.48(12) . . ?

N2 P2 C51 116.01(12) . . ?

C4 P2 C51 106.37(12) . . ?

C41 P2 C51 102.15(12) . . ?

N2 P2 Mo1 54.28(8) . . ?

C4 P2 Mo1 56.17(8) . . ?

C41 P2 Mo1 150.61(9) . . ?

C51 P2 Mo1 107.19(9) . . ?

P1 N1 Si1 136.62(13) . . ?

P1 N1 Mo1 93.38(9) . . ?

Si1 N1 Mo1 124.14(11) . . ?

P2 N2 Si2 136.17(14) . . ?

P2 N2 Mo1 92.81(9) . . ?

Si2 N2 Mo1 123.71(11) . . ?

C13 O4 C11 115.6(4) . . ?

C15 O5 C17 115.6(4) . . ?

O1 C1 Mo1 172.8(2) . . ?

O2 C2 Mo1 176.2(3) . . ?

O3 C3 Mo1 172.1(2) . . ?

P1 C4 P2 120.05(13) . . ?

P1 C4 Mo1 87.78(9) . . ?

P2 C4 Mo1 86.90(9) . . ?

C12 C11 O4 114.5(6) . . ?

O4 C13 C14 109.9(4) . . ?

C16 C15 O5 116.6(5) . . ?

O5 C17 C18 114.3(5) . . ?

C26 C21 C22 118.7(3) . . ?

C26 C21 P1 120.4(2) . . ?

C22 C21 P1 120.8(2) . . ?

C23 C22 C21 119.6(3) . . ?

C24 C23 C22 121.2(4) . . ?

C23 C24 C25 119.5(4) . . ?

C24 C25 C26 120.1(4) . . ?

C25 C26 C21 120.8(4) . . ?

C32 C31 C36 118.5(2) . . ?

C32 C31 P1 123.1(2) . . ?

C36 C31 P1 118.5(2) . . ?

C31 C32 C33 120.4(3) . . ?

C34 C33 C32 120.2(3) . . ?

C33 C34 C35 119.9(3) . . ?

C34 C35 C36 119.9(3) . . ?

C35 C36 C31 121.0(3) . . ?

C42 C41 C46 119.3(3) . . ?

C42 C41 P2 120.3(2) . . ?

C46 C41 P2 120.2(2) . . ?

C41 C42 C43 120.3(3) . . ?

C44 C43 C42 120.2(3) . . ?

C43 C44 C45 119.9(3) . . ?

C44 C45 C46 120.5(3) . . ?

C45 C46 C41 119.8(3) . . ?

C56 C51 C52 117.7(3) . . ?

C56 C51 P2 123.1(2) . . ?

C52 C51 P2 119.1(2) . . ?

C53 C52 C51 120.9(3) . . ?

C54 C53 C52 120.0(3) . . ?

C53 C54 C55 120.1(3) . . ?

C54 C55 C56 119.7(3) . . ?

C51 C56 C55 121.5(3) . . ?



_diffrn_measured_fraction_theta_max 0.974

_diffrn_reflns_theta_full        28.03

_diffrn_measured_fraction_theta_full 0.974

_refine_diff_density_max         3.783

_refine_diff_density_min         -0.340

_refine_diff_density_rms         0.073





