# 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

'David McGuinness'

'John T. Dixon'

'Ulli Englert'

'Cronje Grove'

'Chinhua Hu'

'Peter Wassercheid'



_publ_contact_author_name        'Dr David McGuinness'

_publ_contact_author_address     

;

Chemistry 

Imperial College London 

Exhibition Rd 

South Kensington 

London 

SW7 2AY 

UNITED KINGDOM

;



_publ_contact_author_email       D.MCGUINNESS@IC.AC.UK



_publ_section_title              

;

Novel Cr-PNP complexes as catalylst for the

trimerisation of ethylene 

;



#

_publ_section_exptl_refinement   

;

All H atoms were introduced in idealized positions and included as 

riding with Uiso(H) = 1.3Ueq(non-H).

The sulfur atom of DMSO solvate is disordered in two positons with the 

occupacy of 0.90:0.10.

;



_publ_section_references         

;

Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, Wisconson, 

USA.



Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, Wisconson, 

USA.



Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany.



Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, 

Wisconson, USA.



Spek, A. L. (1990). Acta Cryst. A46, C-34.

;



data_dm1d

_database_code_CSD               179726



_audit_creation_date             15-02-02

_audit_creation_method           SHELXTL

_audit_update_record             

; 

?

;



_chemical_name_systematic        

;  ?

;

_chemical_name_common            'Compound 1'

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C30 H35 Cl3 Cr N O P2 S'

_chemical_formula_weight         677.95



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'

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

Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

S S 0.1246 0.1234 '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'



_symmetry_cell_setting           monoclinic

_symmetry_space_group_name_H-M   C2/c



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

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

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

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

'-x, -y, -z'

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

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

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



_cell_length_a                   27.667(7)

_cell_length_b                   14.751(4)

_cell_length_c                   16.512(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 100.923(7)

_cell_angle_gamma                90.00

_cell_volume                     6617(3)

_cell_formula_units_Z            8

_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    28626

_cell_measurement_theta_min      2.10

_cell_measurement_theta_max      26.06



_exptl_crystal_description       plate

_exptl_crystal_colour            blue-purple

_exptl_crystal_size_max          0.64

_exptl_crystal_size_mid          0.39

_exptl_crystal_size_min          0.08

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.361

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2808.0

_exptl_absorpt_coefficient_mu    0.772

_exptl_absorpt_correction_type   empirical

_exptl_absorpt_correction_T_min  0.817901

_exptl_absorpt_correction_T_max  1.000000

_exptl_absorpt_process_details   'SADABS (1996)'



_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  'Bruker SMART APEX CCD diffractometer'

_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        0

_diffrn_reflns_number            28626

_diffrn_reflns_av_R_equivalents  0.0662

_diffrn_reflns_av_sigmaI/netI    0.0652

_diffrn_reflns_limit_h_min       -33

_diffrn_reflns_limit_h_max       34

_diffrn_reflns_limit_k_min       -18

_diffrn_reflns_limit_k_max       18

_diffrn_reflns_limit_l_min       -20

_diffrn_reflns_limit_l_max       20

_diffrn_reflns_theta_min         2.10

_diffrn_reflns_theta_max         26.06

_reflns_number_total             6532

_reflns_number_gt                4607

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'SMART (Bruker, 2001)'

_computing_cell_refinement       'SMART (Bruker, 2001)'

_computing_data_reduction        'SAINT+ (Bruker, 1999)'

_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'

_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'

_computing_molecular_graphics    'PLATON (Spek, 1990)'

_computing_publication_material  'SHELXTL (Sheldrick, 1998)'



_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)+(0.0687P)²+6.1765P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         6532

_refine_ls_number_parameters     355

_refine_ls_number_restraints     7

_refine_ls_R_factor_all          0.0778

_refine_ls_R_factor_gt           0.0521

_refine_ls_wR_factor_ref         0.1512

_refine_ls_wR_factor_gt          0.1361

_refine_ls_goodness_of_fit_ref   1.044

_refine_ls_restrained_S_all      1.047

_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

Cr Cr 0.29628(2) 0.34364(3) 0.85131(3) 0.03519(17) Uani 1 1 d . . .

Cl1 Cl 0.30768(4) 0.49429(6) 0.82619(6) 0.0536(3) Uani 1 1 d . . .

Cl2 Cl 0.33413(4) 0.29318(6) 0.74659(5) 0.0486(2) Uani 1 1 d . . .

Cl3 Cl 0.25322(4) 0.37490(6) 0.95773(5) 0.0464(2) Uani 1 1 d . . .

P1 P 0.37402(4) 0.32213(6) 0.95066(6) 0.0402(2) Uani 1 1 d . . .

P2 P 0.21437(4) 0.31915(6) 0.76449(6) 0.0398(2) Uani 1 1 d . . .

N N 0.28729(10) 0.20457(17) 0.88200(17) 0.0368(6) Uani 1 1 d . . .

H1 H 0.2731 0.2066 0.9300 0.048 Uiso 1 1 calc R . .

C1 C 0.36724(14) 0.2022(2) 0.9778(2) 0.0445(9) Uani 1 1 d . . .

H1A H 0.3996 0.1730 0.9889 0.058 Uiso 1 1 calc R . .

H1B H 0.3532 0.1984 1.0279 0.058 Uiso 1 1 calc R . .

C2 C 0.33385(14) 0.1532(2) 0.9076(2) 0.0444(9) Uani 1 1 d . . .

H2A H 0.3506 0.1472 0.8606 0.058 Uiso 1 1 calc R . .

H2B H 0.3265 0.0923 0.9255 0.058 Uiso 1 1 calc R . .

C3 C 0.20295(14) 0.2058(2) 0.8021(2) 0.0463(9) Uani 1 1 d . . .

H3A H 0.1888 0.2107 0.8520 0.060 Uiso 1 1 calc R . .

H3B H 0.1795 0.1734 0.7601 0.060 Uiso 1 1 calc R . .

C4 C 0.25114(14) 0.1543(2) 0.8209(2) 0.0447(9) Uani 1 1 d . . .

H4A H 0.2456 0.0942 0.8426 0.058 Uiso 1 1 calc R . .

H4B H 0.2641 0.1462 0.7701 0.058 Uiso 1 1 calc R . .

C5 C 0.38613(14) 0.3817(3) 1.0495(2) 0.0480(9) Uani 1 1 d . . .

C6 C 0.42043(16) 0.3467(3) 1.1151(2) 0.0583(11) Uani 1 1 d . . .

H6 H 0.4392 0.2919 1.1078 0.076 Uiso 1 1 calc R . .

C7 C 0.42759(19) 0.3913(4) 1.1918(3) 0.0773(15) Uani 1 1 d . . .

H7 H 0.4514 0.3674 1.2385 0.100 Uiso 1 1 calc R . .

C8 C 0.4012(2) 0.4683(4) 1.2014(3) 0.0822(17) Uani 1 1 d . . .

H8 H 0.4059 0.4985 1.2551 0.107 Uiso 1 1 calc R . .

C9 C 0.36815(19) 0.5031(4) 1.1357(3) 0.0757(14) Uani 1 1 d . . .

H9 H 0.3499 0.5585 1.1426 0.098 Uiso 1 1 calc R . .

C10 C 0.36077(16) 0.4603(3) 1.0605(3) 0.0589(11) Uani 1 1 d . . .

H10 H 0.3373 0.4856 1.0141 0.077 Uiso 1 1 calc R . .

C11 C 0.43217(15) 0.3316(3) 0.9144(2) 0.0503(9) Uani 1 1 d . . .

C12 C 0.45599(18) 0.4151(3) 0.9193(3) 0.0680(13) Uani 1 1 d . . .

H12 H 0.4420 0.4674 0.9433 0.088 Uiso 1 1 calc R . .

C13 C 0.4998(2) 0.4242(4) 0.8899(3) 0.0868(17) Uani 1 1 d . . .

H13 H 0.5163 0.4833 0.8924 0.113 Uiso 1 1 calc R . .

C14 C 0.5198(2) 0.3516(5) 0.8579(3) 0.0923(18) Uani 1 1 d . . .

H14 H 0.5512 0.3581 0.8393 0.120 Uiso 1 1 calc R . .

C15 C 0.4966(2) 0.2696(5) 0.8513(3) 0.0881(17) Uani 1 1 d . . .

H15 H 0.5112 0.2179 0.8273 0.115 Uiso 1 1 calc R . .

C16 C 0.45191(17) 0.2590(3) 0.8789(3) 0.0671(12) Uani 1 1 d . . .

H16 H 0.4348 0.2005 0.8729 0.087 Uiso 1 1 calc R . .

C17 C 0.16327(14) 0.3899(3) 0.7809(2) 0.0453(9) Uani 1 1 d . . .

C18 C 0.16916(17) 0.4832(3) 0.7864(3) 0.0632(11) Uani 1 1 d . . .

H18 H 0.2008 0.5100 0.7812 0.082 Uiso 1 1 calc R . .

C19 C 0.1312(2) 0.5389(4) 0.7992(3) 0.0829(15) Uani 1 1 d . . .

H19 H 0.1357 0.6049 0.8015 0.108 Uiso 1 1 calc R . .

C20 C 0.0876(2) 0.5017(4) 0.8087(4) 0.0930(18) Uani 1 1 d . . .

H20 H 0.0610 0.5412 0.8193 0.121 Uiso 1 1 calc R . .

C21 C 0.0803(2) 0.4099(5) 0.8036(4) 0.0943(18) Uani 1 1 d . . .

H21 H 0.0485 0.3842 0.8100 0.123 Uiso 1 1 calc R . .

C22 C 0.11819(17) 0.3530(3) 0.7893(3) 0.0687(13) Uani 1 1 d . . .

H22 H 0.1130 0.2873 0.7851 0.089 Uiso 1 1 calc R . .

C23 C 0.20750(14) 0.3121(2) 0.6521(2) 0.0433(8) Uani 1 1 d . . .

C24 C 0.22202(18) 0.3869(3) 0.6116(3) 0.0644(12) Uani 1 1 d . . .

H24 H 0.2367 0.4395 0.6433 0.084 Uiso 1 1 calc R . .

C25 C 0.2157(2) 0.3872(3) 0.5256(3) 0.0780(15) Uani 1 1 d . . .

H25 H 0.2256 0.4406 0.4973 0.101 Uiso 1 1 calc R . .

C26 C 0.1961(2) 0.3140(4) 0.4808(3) 0.0786(15) Uani 1 1 d . . .

H26 H 0.1917 0.3147 0.4205 0.102 Uiso 1 1 calc R . .

C27 C 0.1825(2) 0.2393(4) 0.5208(3) 0.0779(14) Uani 1 1 d . . .

H27 H 0.1685 0.1865 0.4887 0.101 Uiso 1 1 calc R . .

C28 C 0.18833(17) 0.2376(3) 0.6066(3) 0.0608(11) Uani 1 1 d . . .

H28 H 0.1788 0.1835 0.6344 0.079 Uiso 1 1 calc R . .

O O 0.48556(18) 0.1106(5) 1.0503(4) 0.167(2) Uani 1 1 d D . .

C29 C 0.5524(3) 0.2297(7) 1.0728(6) 0.198(5) Uani 1 1 d D . .

H29A H 0.5306 0.2760 1.0501 0.257 Uiso 0.90 1 d PR A -1

H29B H 0.5858 0.2382 1.0651 0.257 Uiso 0.90 1 d PR A -1

H29C H 0.5519 0.2196 1.1319 0.257 Uiso 0.90 1 d PR A -1

H29D H 0.5302 0.2603 1.0288 0.257 Uiso 0.10 1 d PR A -2

H29E H 0.5843 0.2193 1.0573 0.257 Uiso 0.10 1 d PR A -2

H29F H 0.5562 0.2632 1.1240 0.257 Uiso 0.10 1 d PR A -2

C30 C 0.5772(3) 0.0519(6) 1.0690(5) 0.167(4) Uani 1 1 d D . .

H30A H 0.5753 0.0504 1.1275 0.217 Uiso 0.90 1 d PR B -1

H30B H 0.6087 0.0766 1.0618 0.217 Uiso 0.90 1 d PR B -1

H30C H 0.5715 -0.0072 1.0444 0.217 Uiso 0.90 1 d PR B -1

H30D H 0.5614 -0.0009 1.0408 0.217 Uiso 0.10 1 d PR B -2

H30E H 0.5960 0.0357 1.1231 0.217 Uiso 0.10 1 d PR B -2

H30F H 0.5971 0.0836 1.0365 0.217 Uiso 0.10 1 d PR B -2

S1A S 0.53101(7) 0.12520(18) 1.01880(13) 0.1217(7) Uani 0.90 1 d PD C -1

S1B S 0.5315(5) 0.1226(10) 1.0993(11) 0.1217(7) Uani 0.10 1 d PD C -2






_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

Cr N 2.139(3) . ?

Cr Cl1 2.2934(11) . ?

Cr Cl2 2.3081(11) . ?

Cr Cl3 2.3480(11) . ?

Cr P1 2.4660(12) . ?

Cr P2 2.4678(12) . ?

P1 C11 1.825(4) . ?

P1 C5 1.827(4) . ?

P1 C1 1.843(4) . ?

P2 C17 1.818(4) . ?

P2 C3 1.831(4) . ?

P2 C23 1.832(4) . ?

N C4 1.478(4) . ?

N C2 1.485(4) . ?

N H1 0.9500 . ?

C1 C2 1.521(5) . ?

C1 H1A 0.9800 . ?

C1 H1B 0.9800 . ?

C2 H2A 0.9800 . ?

C2 H2B 0.9800 . ?

C3 C4 1.515(5) . ?

C3 H3A 0.9800 . ?

C3 H3B 0.9800 . ?

C4 H4A 0.9800 . ?

C4 H4B 0.9800 . ?

C5 C10 1.385(6) . ?

C5 C6 1.397(6) . ?

C6 C7 1.408(6) . ?

C6 H6 0.9800 . ?

C7 C8 1.376(8) . ?

C7 H7 0.9800 . ?

C8 C9 1.379(8) . ?

C8 H8 0.9800 . ?

C9 C10 1.373(6) . ?

C9 H9 0.9800 . ?

C10 H10 0.9800 . ?

C11 C16 1.382(6) . ?

C11 C12 1.392(6) . ?

C12 C13 1.395(7) . ?

C12 H12 0.9800 . ?

C13 C14 1.358(8) . ?

C13 H13 0.9800 . ?

C14 C15 1.363(8) . ?

C14 H14 0.9800 . ?

C15 C16 1.405(7) . ?

C15 H15 0.9800 . ?

C16 H16 0.9800 . ?

C17 C18 1.386(6) . ?

C17 C22 1.392(6) . ?

C18 C19 1.381(6) . ?

C18 H18 0.9800 . ?

C19 C20 1.363(8) . ?

C19 H19 0.9800 . ?

C20 C21 1.369(8) . ?

C20 H20 0.9800 . ?

C21 C22 1.398(7) . ?

C21 H21 0.9800 . ?

C22 H22 0.9800 . ?

C23 C28 1.381(5) . ?

C23 C24 1.388(5) . ?

C24 C25 1.397(6) . ?

C24 H24 0.9800 . ?

C25 C26 1.362(7) . ?

C25 H25 0.9800 . ?

C26 C27 1.373(7) . ?

C26 H26 0.9800 . ?

C27 C28 1.394(6) . ?

C27 H27 0.9800 . ?

C28 H28 0.9800 . ?

O S1B 1.384(14) . ?

O S1A 1.465(5) . ?

C29 S1B 1.765(14) . ?

C29 S1A 1.822(8) . ?

C29 H29A 0.9408 . ?

C29 H29B 0.9656 . ?

C29 H29C 0.9886 . ?

C29 H29D 0.9689 . ?

C29 H29E 0.9781 . ?

C29 H29F 0.9676 . ?

C30 S1A 1.757(7) . ?

C30 S1B 1.781(14) . ?

C30 H30A 0.9779 . ?

C30 H30B 0.9733 . ?

C30 H30C 0.9619 . ?

C30 H30D 0.9672 . ?

C30 H30E 0.9752 . ?

C30 H30F 0.9607 . ?

S1B H29C 1.5940 . ?

S1B H30A 1.6123 . ?



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

N Cr Cl1 176.74(8) . . ?

N Cr Cl2 87.59(8) . . ?

Cl1 Cr Cl2 94.56(4) . . ?

N Cr Cl3 85.00(8) . . ?

Cl1 Cr Cl3 92.96(4) . . ?

Cl2 Cr Cl3 172.15(4) . . ?

N Cr P1 81.08(8) . . ?

Cl1 Cr P1 96.45(4) . . ?

Cl2 Cr P1 89.68(4) . . ?

Cl3 Cr P1 91.70(4) . . ?

N Cr P2 82.07(8) . . ?

Cl1 Cr P2 100.34(4) . . ?

Cl2 Cr P2 90.85(4) . . ?

Cl3 Cr P2 85.59(4) . . ?

P1 Cr P2 163.10(4) . . ?

C11 P1 C5 103.42(18) . . ?

C11 P1 C1 106.83(18) . . ?

C5 P1 C1 104.73(17) . . ?

C11 P1 Cr 118.95(13) . . ?

C5 P1 Cr 121.44(14) . . ?

C1 P1 Cr 99.73(12) . . ?

C17 P2 C3 106.56(18) . . ?

C17 P2 C23 104.40(17) . . ?

C3 P2 C23 107.48(17) . . ?

C17 P2 Cr 118.93(13) . . ?

C3 P2 Cr 97.76(12) . . ?

C23 P2 Cr 120.28(13) . . ?

C4 N C2 112.1(3) . . ?

C4 N Cr 114.4(2) . . ?

C2 N Cr 115.0(2) . . ?

C4 N H1 104.6 . . ?

C2 N H1 104.6 . . ?

Cr N H1 104.6 . . ?

C2 C1 P1 110.2(2) . . ?

C2 C1 H1A 109.6 . . ?

P1 C1 H1A 109.6 . . ?

C2 C1 H1B 109.6 . . ?

P1 C1 H1B 109.6 . . ?

H1A C1 H1B 108.1 . . ?

N C2 C1 110.1(3) . . ?

N C2 H2A 109.6 . . ?

C1 C2 H2A 109.6 . . ?

N C2 H2B 109.6 . . ?

C1 C2 H2B 109.6 . . ?

H2A C2 H2B 108.2 . . ?

C4 C3 P2 109.0(3) . . ?

C4 C3 H3A 109.9 . . ?

P2 C3 H3A 109.9 . . ?

C4 C3 H3B 109.9 . . ?

P2 C3 H3B 109.9 . . ?

H3A C3 H3B 108.3 . . ?

N C4 C3 110.1(3) . . ?

N C4 H4A 109.6 . . ?

C3 C4 H4A 109.6 . . ?

N C4 H4B 109.6 . . ?

C3 C4 H4B 109.6 . . ?

H4A C4 H4B 108.2 . . ?

C10 C5 C6 119.6(4) . . ?

C10 C5 P1 120.5(3) . . ?

C6 C5 P1 119.9(3) . . ?

C5 C6 C7 119.0(5) . . ?

C5 C6 H6 120.5 . . ?

C7 C6 H6 120.5 . . ?

C8 C7 C6 120.1(5) . . ?

C8 C7 H7 119.9 . . ?

C6 C7 H7 119.9 . . ?

C7 C8 C9 120.3(4) . . ?

C7 C8 H8 119.9 . . ?

C9 C8 H8 119.9 . . ?

C10 C9 C8 120.2(5) . . ?

C10 C9 H9 119.9 . . ?

C8 C9 H9 119.9 . . ?

C9 C10 C5 120.8(5) . . ?

C9 C10 H10 119.6 . . ?

C5 C10 H10 119.6 . . ?

C16 C11 C12 119.3(4) . . ?

C16 C11 P1 121.6(3) . . ?

C12 C11 P1 119.1(3) . . ?

C11 C12 C13 119.9(5) . . ?

C11 C12 H12 120.0 . . ?

C13 C12 H12 120.0 . . ?

C14 C13 C12 120.2(5) . . ?

C14 C13 H13 119.9 . . ?

C12 C13 H13 119.9 . . ?

C13 C14 C15 120.8(5) . . ?

C13 C14 H14 119.6 . . ?

C15 C14 H14 119.6 . . ?

C14 C15 C16 120.1(5) . . ?

C14 C15 H15 119.9 . . ?

C16 C15 H15 119.9 . . ?

C11 C16 C15 119.6(5) . . ?

C11 C16 H16 120.2 . . ?

C15 C16 H16 120.2 . . ?

C18 C17 C22 118.6(4) . . ?

C18 C17 P2 119.7(3) . . ?

C22 C17 P2 121.8(3) . . ?

C19 C18 C17 121.2(5) . . ?

C19 C18 H18 119.4 . . ?

C17 C18 H18 119.4 . . ?

C20 C19 C18 119.5(5) . . ?

C20 C19 H19 120.2 . . ?

C18 C19 H19 120.2 . . ?

C19 C20 C21 121.0(5) . . ?

C19 C20 H20 119.5 . . ?

C21 C20 H20 119.5 . . ?

C20 C21 C22 119.8(5) . . ?

C20 C21 H21 120.1 . . ?

C22 C21 H21 120.1 . . ?

C17 C22 C21 119.8(5) . . ?

C17 C22 H22 120.1 . . ?

C21 C22 H22 120.1 . . ?

C28 C23 C24 119.1(4) . . ?

C28 C23 P2 123.5(3) . . ?

C24 C23 P2 117.4(3) . . ?

C23 C24 C25 120.1(4) . . ?

C23 C24 H24 120.0 . . ?

C25 C24 H24 120.0 . . ?

C26 C25 C24 120.6(5) . . ?

C26 C25 H25 119.7 . . ?

C24 C25 H25 119.7 . . ?

C25 C26 C27 119.4(4) . . ?

C25 C26 H26 120.3 . . ?

C27 C26 H26 120.3 . . ?

C26 C27 C28 121.0(5) . . ?

C26 C27 H27 119.5 . . ?

C28 C27 H27 119.5 . . ?

C23 C28 C27 119.8(4) . . ?

C23 C28 H28 120.1 . . ?

C27 C28 H28 120.1 . . ?

S1B O S1A 55.4(7) . . ?

S1B C29 S1A 43.4(6) . . ?

S1B C29 H29A 122.3 . . ?

S1A C29 H29A 107.1 . . ?

S1B C29 H29B 121.1 . . ?

S1A C29 H29B 106.0 . . ?

H29A C29 H29B 114.2 . . ?

S1B C29 H29C 63.6 . . ?

S1A C29 H29C 107.0 . . ?

H29A C29 H29C 112.1 . . ?

H29B C29 H29C 110.0 . . ?

S1B C29 H29D 114.4 . . ?

S1A C29 H29D 85.8 . . ?

H29A C29 H29D 25.3 . . ?

H29B C29 H29D 109.0 . . ?

H29C C29 H29D 133.2 . . ?

S1B C29 H29E 106.2 . . ?

S1A C29 H29E 88.0 . . ?

H29A C29 H29E 123.5 . . ?

H29B C29 H29E 18.1 . . ?

H29C C29 H29E 114.6 . . ?

H29D C29 H29E 110.6 . . ?

S1B C29 H29F 103.2 . . ?

S1A C29 H29F 146.3 . . ?

H29A C29 H29F 86.2 . . ?

H29B C29 H29F 95.7 . . ?

H29C C29 H29F 40.1 . . ?

H29D C29 H29F 111.5 . . ?

H29E C29 H29F 110.7 . . ?

S1A C30 S1B 44.1(6) . . ?

S1A C30 H30A 108.0 . . ?

S1B C30 H30A 63.9 . . ?

S1A C30 H30B 107.5 . . ?

S1B C30 H30B 120.9 . . ?

H30A C30 H30B 110.2 . . ?

S1A C30 H30C 108.2 . . ?

S1B C30 H30C 125.5 . . ?

H30A C30 H30C 111.2 . . ?

H30B C30 H30C 111.6 . . ?

S1A C30 H30D 92.7 . . ?

S1B C30 H30D 109.1 . . ?

H30A C30 H30D 110.7 . . ?

H30B C30 H30D 125.2 . . ?

H30C C30 H30D 17.2 . . ?

S1A C30 H30E 142.9 . . ?

S1B C30 H30E 99.8 . . ?

H30A C30 H30E 37.7 . . ?

H30B C30 H30E 82.3 . . ?

H30C C30 H30E 100.4 . . ?

H30D C30 H30E 111.0 . . ?

S1A C30 H30F 83.1 . . ?

S1B C30 H30F 112.6 . . ?

H30A C30 H30F 135.0 . . ?

H30B C30 H30F 29.2 . . ?

H30C C30 H30F 105.8 . . ?

H30D C30 H30F 112.2 . . ?

H30E C30 H30F 111.5 . . ?

O S1A C30 109.8(4) . . ?

O S1A C29 99.9(5) . . ?

C30 S1A C29 98.7(4) . . ?

O S1B C29 106.1(10) . . ?

O S1B C30 112.5(10) . . ?

C29 S1B C30 99.9(8) . . ?

O S1B H29C 122.7 . . ?

C29 S1B H29C 33.8 . . ?

C30 S1B H29C 113.3 . . ?

O S1B H30A 129.9 . . ?

C29 S1B H30A 113.6 . . ?

C30 S1B H30A 33.0 . . ?

H29C S1B H30A 107.3 . . ?



loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_distance_DA

_geom_hbond_angle_DHA

_geom_hbond_site_symmetry_A

N H1 Cl3 0.95 2.43 3.280(3) 148.3 7_557



_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        26.06

_diffrn_measured_fraction_theta_full 0.996

_refine_diff_density_max         0.492

_refine_diff_density_min         -0.725

_refine_diff_density_rms         0.077



data_dm2a

_database_code_CSD               179727



_audit_creation_date             15-02-02

_audit_creation_method           'from SDP and SHELXTL'



_chemical_name_systematic        

; 

? 

;

_chemical_name_common            'Compound 2'

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C31 H59 Cl3 Cr N O P2'

_chemical_formula_weight         682.08



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'

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

Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Cr Cr 0.3209 0.6236 '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'



_symmetry_cell_setting           monoclinic

_symmetry_space_group_name_H-M   P2(1)/n



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

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

'-x, -y, -z'

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



_cell_length_a                   10.340(3)

_cell_length_b                   16.2779(11)

_cell_length_c                   21.3434(18)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.757(13)

_cell_angle_gamma                90.00

_cell_volume                     3592.1(11)

_cell_formula_units_Z            4

_cell_measurement_temperature    223(2)

_cell_measurement_reflns_used    25

_cell_measurement_theta_min      13

_cell_measurement_theta_max      15



_exptl_crystal_description       prism

_exptl_crystal_colour            blue-purple

_exptl_crystal_size_max          0.48

_exptl_crystal_size_mid          0.28

_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.261

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1460

_exptl_absorpt_coefficient_mu    0.655

_exptl_absorpt_correction_type   empirical

_exptl_absorpt_correction_T_min  0.827

_exptl_absorpt_correction_T_max  0.999

_exptl_absorpt_process_details   ?



_exptl_special_details           

; 

? 

;



_diffrn_ambient_temperature      223(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  'Enraf-Nonius CAD4'

_diffrn_measurement_method       ω/2θ

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         3

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  120

_diffrn_standards_decay_%        -2.43

_diffrn_reflns_number            10559

_diffrn_reflns_av_R_equivalents  0.0494

_diffrn_reflns_av_sigmaI/netI    0.0799

_diffrn_reflns_limit_h_min       -12

_diffrn_reflns_limit_h_max       4

_diffrn_reflns_limit_k_min       0

_diffrn_reflns_limit_k_max       20

_diffrn_reflns_limit_l_min       -26

_diffrn_reflns_limit_l_max       26

_diffrn_reflns_theta_min         2.18

_diffrn_reflns_theta_max         25.98

_reflns_number_total             7031

_reflns_number_gt                4774

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'

_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'

_computing_data_reduction        'PROCESS MolEN (Fair, 1990)'

_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'

_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'

_computing_molecular_graphics    'PLATON (Spek, 1990)'

_computing_publication_material  'SHELXTL (Sheldrick, 1998)'



_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)+(0.0838P)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    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         7031

_refine_ls_number_parameters     352

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0917

_refine_ls_R_factor_gt           0.0520

_refine_ls_wR_factor_ref         0.1399

_refine_ls_wR_factor_gt          0.1279

_refine_ls_goodness_of_fit_ref   0.978

_refine_ls_restrained_S_all      0.978

_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

Cr Cr 0.82426(5) 0.88859(3) 0.10108(2) 0.02189(14) Uani 1 1 d . . .

Cl1 Cl 0.86622(9) 0.83569(6) 0.19866(4) 0.0362(2) Uani 1 1 d . . .

Cl2 Cl 0.62260(8) 0.82840(5) 0.09244(4) 0.0326(2) Uani 1 1 d . . .

Cl3 Cl 1.02386(8) 0.95851(5) 0.09528(4) 0.0306(2) Uani 1 1 d . . .

P1 P 0.92159(9) 0.77549(5) 0.04097(4) 0.0257(2) Uani 1 1 d . . .

P2 P 0.71961(8) 1.01846(5) 0.13286(4) 0.0256(2) Uani 1 1 d . . .

N N 0.7887(3) 0.93764(16) 0.00961(12) 0.0249(6) Uani 1 1 d . . .

H1 H 0.8612 0.9715 0.0012 0.032 Uiso 1 1 calc R . .

C1 C 0.9081(4) 0.8221(2) -0.03706(16) 0.0319(8) Uani 1 1 d . . .

H1A H 0.9845 0.8559 -0.0451 0.042 Uiso 1 1 calc R . .

H1B H 0.9035 0.7789 -0.0690 0.042 Uiso 1 1 calc R . .

C2 C 0.7870(4) 0.8751(2) -0.04072(16) 0.0333(8) Uani 1 1 d . . .

H2A H 0.7822 0.9024 -0.0816 0.043 Uiso 1 1 calc R . .

H2B H 0.7102 0.8403 -0.0366 0.043 Uiso 1 1 calc R . .

C3 C 0.6845(4) 1.0604(2) 0.05420(16) 0.0324(8) Uani 1 1 d . . .

H3A H 0.6028 1.0909 0.0550 0.042 Uiso 1 1 calc R . .

H3B H 0.7531 1.0989 0.0427 0.042 Uiso 1 1 calc R . .

C4 C 0.6751(3) 0.9928(2) 0.00536(16) 0.0317(8) Uani 1 1 d . . .

H4A H 0.5960 0.9609 0.0118 0.041 Uiso 1 1 calc R . .

H4B H 0.6702 1.0173 -0.0365 0.041 Uiso 1 1 calc R . .

C5 C 0.8303(4) 0.6782(2) 0.03406(17) 0.0326(8) Uani 1 1 d . . .

H5 H 0.7460 0.6936 0.0162 0.042 Uiso 1 1 calc R . .

C6 C 0.8866(4) 0.6152(2) -0.01181(19) 0.0454(10) Uani 1 1 d . . .

H6A H 0.9013 0.6414 -0.0525 0.059 Uiso 1 1 calc R . .

H6B H 0.9697 0.5949 0.0044 0.059 Uiso 1 1 calc R . .

C7 C 0.7926(5) 0.5439(3) -0.0198(2) 0.0568(12) Uani 1 1 d . . .

H7A H 0.7129 0.5638 -0.0401 0.074 Uiso 1 1 calc R . .

H7B H 0.8309 0.5026 -0.0474 0.074 Uiso 1 1 calc R . .

C8 C 0.7597(5) 0.5042(3) 0.0417(2) 0.0565(12) Uani 1 1 d . . .

H8A H 0.8373 0.4783 0.0596 0.073 Uiso 1 1 calc R . .

H8B H 0.6949 0.4612 0.0345 0.073 Uiso 1 1 calc R . .

C9 C 0.7075(5) 0.5664(2) 0.0878(2) 0.0540(12) Uani 1 1 d . . .

H9A H 0.6935 0.5395 0.1282 0.070 Uiso 1 1 calc R . .

H9B H 0.6240 0.5871 0.0724 0.070 Uiso 1 1 calc R . .

C10 C 0.8008(4) 0.6380(2) 0.09662(18) 0.0413(9) Uani 1 1 d . . .

H10A H 0.7627 0.6787 0.1247 0.054 Uiso 1 1 calc R . .

H10B H 0.8813 0.6182 0.1160 0.054 Uiso 1 1 calc R . .

C11 C 1.0950(3) 0.7588(2) 0.05510(17) 0.0317(8) Uani 1 1 d . . .

H11 H 1.1309 0.8138 0.0618 0.041 Uiso 1 1 calc R . .

C12 C 1.1767(4) 0.7215(2) 0.00260(19) 0.0415(9) Uani 1 1 d . . .

H12A H 1.1509 0.6643 -0.0045 0.054 Uiso 1 1 calc R . .

H12B H 1.1616 0.7521 -0.0364 0.054 Uiso 1 1 calc R . .

C13 C 1.3191(4) 0.7251(3) 0.0204(2) 0.0483(11) Uani 1 1 d . . .

H13A H 1.3697 0.6991 -0.0127 0.063 Uiso 1 1 calc R . .

H13B H 1.3461 0.7827 0.0235 0.063 Uiso 1 1 calc R . .

C14 C 1.3474(4) 0.6826(3) 0.0818(2) 0.0496(11) Uani 1 1 d . . .

H14A H 1.3307 0.6236 0.0772 0.064 Uiso 1 1 calc R . .

H14B H 1.4389 0.6897 0.0929 0.064 Uiso 1 1 calc R . .

C15 C 1.2653(4) 0.7164(3) 0.1335(2) 0.0581(12) Uani 1 1 d . . .

H15A H 1.2903 0.7735 0.1417 0.076 Uiso 1 1 calc R . .

H15B H 1.2813 0.6847 0.1718 0.076 Uiso 1 1 calc R . .

C16 C 1.1214(4) 0.7130(3) 0.11674(19) 0.0481(11) Uani 1 1 d . . .

H16A H 1.0714 0.7382 0.1504 0.062 Uiso 1 1 calc R . .

H16B H 1.0940 0.6556 0.1125 0.062 Uiso 1 1 calc R . .

C17 C 0.5643(4) 1.0088(2) 0.1736(2) 0.0418(9) Uani 1 1 d . . .

H17 H 0.5171 0.9674 0.1490 0.054 Uiso 1 1 calc R . .

C18 C 0.4747(5) 1.0803(3) 0.1741(3) 0.0706(15) Uani 1 1 d . . .

H18A H 0.4600 1.0997 0.1311 0.092 Uiso 1 1 calc R . .

H18B H 0.5137 1.1252 0.1983 0.092 Uiso 1 1 calc R . .

C19 C 0.3446(4) 1.0556(3) 0.2033(2) 0.0658(14) Uani 1 1 d . . .

H19A H 0.2888 1.1041 0.2058 0.086 Uiso 1 1 calc R . .

H19B H 0.3013 1.0152 0.1761 0.086 Uiso 1 1 calc R . .

C20 C 0.3628(5) 1.0196(4) 0.2677(3) 0.0756(16) Uani 1 1 d . . .

H20A H 0.3957 1.0621 0.2962 0.098 Uiso 1 1 calc R . .

H20B H 0.2790 1.0010 0.2833 0.098 Uiso 1 1 calc R . .

C21 C 0.4528(6) 0.9507(4) 0.2672(3) 0.106(3) Uani 1 1 d . . .

H21A H 0.4118 0.9048 0.2449 0.138 Uiso 1 1 calc R . .

H21B H 0.4687 0.9330 0.3105 0.138 Uiso 1 1 calc R . .

C22 C 0.5821(4) 0.9689(3) 0.2370(2) 0.0586(13) Uani 1 1 d . . .

H22A H 0.6327 1.0054 0.2644 0.076 Uiso 1 1 calc R . .

H22B H 0.6306 0.9175 0.2323 0.076 Uiso 1 1 calc R . .

C23 C 0.8236(3) 1.0979(2) 0.16789(16) 0.0308(8) Uani 1 1 d . . .

H23 H 0.8966 1.1028 0.1393 0.040 Uiso 1 1 calc R . .

C24 C 0.8844(4) 1.0713(2) 0.2306(2) 0.0467(10) Uani 1 1 d . . .

H24A H 0.9195 1.0156 0.2270 0.061 Uiso 1 1 calc R . .

H24B H 0.8185 1.0710 0.2632 0.061 Uiso 1 1 calc R . .

C25 C 0.9931(4) 1.1315(3) 0.2486(2) 0.0563(12) Uani 1 1 d . . .

H25A H 1.0304 1.1157 0.2893 0.073 Uiso 1 1 calc R . .

H25B H 1.0617 1.1285 0.2174 0.073 Uiso 1 1 calc R . .

C26 C 0.9426(4) 1.2194(2) 0.2522(2) 0.0490(11) Uani 1 1 d . . .

H26A H 0.8810 1.2237 0.2866 0.064 Uiso 1 1 calc R . .

H26B H 1.0148 1.2567 0.2613 0.064 Uiso 1 1 calc R . .

C27 C 0.8770(4) 1.2448(2) 0.1915(2) 0.0447(10) Uani 1 1 d . . .

H27A H 0.9410 1.2466 0.1580 0.058 Uiso 1 1 calc R . .

H27B H 0.8408 1.3001 0.1961 0.058 Uiso 1 1 calc R . .

C28 C 0.7691(4) 1.1852(2) 0.17320(18) 0.0388(9) Uani 1 1 d . . .

H28A H 0.7304 1.2018 0.1330 0.050 Uiso 1 1 calc R . .

H28B H 0.7014 1.1865 0.2049 0.050 Uiso 1 1 calc R . .

C29 C 0.4000(7) 0.3194(3) 0.1466(3) 0.086(2) Uani 1 1 d . . .

C30 C 0.4971(7) 0.3837(4) 0.1449(3) 0.101(2) Uani 1 1 d . A .

H30A H 0.5324 0.3873 0.1026 0.132 Uiso 1 1 calc R . .

H30B H 0.5669 0.3708 0.1748 0.132 Uiso 1 1 calc R . .

H30C H 0.4576 0.4363 0.1561 0.132 Uiso 1 1 calc R . .

C31 C 0.3358(7) 0.3029(5) 0.2058(4) 0.113(3) Uani 1 1 d . A .

H31A H 0.2736 0.2580 0.2000 0.147 Uiso 1 1 calc R . .

H31B H 0.2902 0.3524 0.2195 0.147 Uiso 1 1 calc R . .

H31C H 0.4005 0.2872 0.2376 0.147 Uiso 1 1 calc R . .

O O 0.3784(9) 0.2793(4) 0.1016(3) 0.219(4) Uani 1 1 d . A -1






_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

Cr N 2.137(3) . ?

Cr Cl1 2.2898(10) . ?

Cr Cl2 2.3090(11) . ?

Cr Cl3 2.3616(11) . ?

Cr P1 2.4662(10) . ?

Cr P2 2.4736(10) . ?

P1 C1 1.834(3) . ?

P1 C11 1.835(4) . ?

P1 C5 1.848(3) . ?

P2 C23 1.834(3) . ?

P2 C17 1.843(4) . ?

P2 C3 1.844(3) . ?

N C2 1.480(4) . ?

N C4 1.480(4) . ?

N H1 0.9500 . ?

C1 C2 1.521(5) . ?

C1 H1A 0.9800 . ?

C1 H1B 0.9800 . ?

C2 H2A 0.9800 . ?

C2 H2B 0.9800 . ?

C3 C4 1.518(5) . ?

C3 H3A 0.9800 . ?

C3 H3B 0.9800 . ?

C4 H4A 0.9800 . ?

C4 H4B 0.9800 . ?

C5 C10 1.522(5) . ?

C5 C6 1.537(5) . ?

C5 H5 0.9800 . ?

C6 C7 1.523(5) . ?

C6 H6A 0.9800 . ?

C6 H6B 0.9800 . ?

C7 C8 1.507(6) . ?

C7 H7A 0.9800 . ?

C7 H7B 0.9800 . ?

C8 C9 1.515(6) . ?

C8 H8A 0.9800 . ?

C8 H8B 0.9800 . ?

C9 C10 1.523(5) . ?

C9 H9A 0.9800 . ?

C9 H9B 0.9800 . ?

C10 H10A 0.9800 . ?

C10 H10B 0.9800 . ?

C11 C16 1.533(5) . ?

C11 C12 1.537(5) . ?

C11 H11 0.9800 . ?

C12 C13 1.517(5) . ?

C12 H12A 0.9800 . ?

C12 H12B 0.9800 . ?

C13 C14 1.508(6) . ?

C13 H13A 0.9800 . ?

C13 H13B 0.9800 . ?

C14 C15 1.504(6) . ?

C14 H14A 0.9800 . ?

C14 H14B 0.9800 . ?

C15 C16 1.527(5) . ?

C15 H15A 0.9800 . ?

C15 H15B 0.9800 . ?

C16 H16A 0.9800 . ?

C16 H16B 0.9800 . ?

C17 C18 1.486(6) . ?

C17 C22 1.511(6) . ?

C17 H17 0.9800 . ?

C18 C19 1.544(6) . ?

C18 H18A 0.9800 . ?

C18 H18B 0.9800 . ?

C19 C20 1.504(7) . ?

C19 H19A 0.9800 . ?

C19 H19B 0.9800 . ?

C20 C21 1.458(7) . ?

C20 H20A 0.9800 . ?

C20 H20B 0.9800 . ?

C21 C22 1.521(6) . ?

C21 H21A 0.9800 . ?

C21 H21B 0.9800 . ?

C22 H22A 0.9800 . ?

C22 H22B 0.9800 . ?

C23 C24 1.534(5) . ?

C23 C28 1.534(5) . ?

C23 H23 0.9800 . ?

C24 C25 1.535(5) . ?

C24 H24A 0.9800 . ?

C24 H24B 0.9800 . ?

C25 C26 1.526(6) . ?

C25 H25A 0.9800 . ?

C25 H25B 0.9800 . ?

C26 C27 1.514(6) . ?

C26 H26A 0.9800 . ?

C26 H26B 0.9800 . ?

C27 C28 1.525(5) . ?

C27 H27A 0.9800 . ?

C27 H27B 0.9800 . ?

C28 H28A 0.9800 . ?

C28 H28B 0.9800 . ?

C29 O 1.179(7) . ?

C29 C30 1.450(8) . ?

C29 C31 1.460(9) . ?

C30 H30A 0.9800 . ?

C30 H30B 0.9800 . ?

C30 H30C 0.9800 . ?

C31 H31A 0.9800 . ?

C31 H31B 0.9800 . ?

C31 H31C 0.9800 . ?



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

N Cr Cl1 178.96(8) . . ?

N Cr Cl2 86.63(8) . . ?

Cl1 Cr Cl2 94.19(4) . . ?

N Cr Cl3 84.95(8) . . ?

Cl1 Cr Cl3 94.23(4) . . ?

Cl2 Cr Cl3 171.58(4) . . ?

N Cr P1 82.54(7) . . ?

Cl1 Cr P1 96.81(4) . . ?

Cl2 Cr P1 90.92(4) . . ?

Cl3 Cr P1 88.25(4) . . ?

N Cr P2 81.99(7) . . ?

Cl1 Cr P2 98.65(4) . . ?

Cl2 Cr P2 89.24(4) . . ?

Cl3 Cr P2 89.33(4) . . ?

P1 Cr P2 164.49(4) . . ?

C1 P1 C11 105.87(17) . . ?

C1 P1 C5 104.43(16) . . ?

C11 P1 C5 112.51(16) . . ?

C1 P1 Cr 97.86(11) . . ?

C11 P1 Cr 115.47(12) . . ?

C5 P1 Cr 118.01(12) . . ?

C23 P2 C17 112.19(18) . . ?

C23 P2 C3 102.55(16) . . ?

C17 P2 C3 107.38(18) . . ?

C23 P2 Cr 117.24(12) . . ?

C17 P2 Cr 116.33(13) . . ?

C3 P2 Cr 98.53(11) . . ?

C2 N C4 111.8(2) . . ?

C2 N Cr 114.0(2) . . ?

C4 N Cr 114.2(2) . . ?

C2 N H1 105.3 . . ?

C4 N H1 105.3 . . ?

Cr N H1 105.3 . . ?

C2 C1 P1 109.5(2) . . ?

C2 C1 H1A 109.8 . . ?

P1 C1 H1A 109.8 . . ?

C2 C1 H1B 109.8 . . ?

P1 C1 H1B 109.8 . . ?

H1A C1 H1B 108.2 . . ?

N C2 C1 110.5(3) . . ?

N C2 H2A 109.5 . . ?

C1 C2 H2A 109.5 . . ?

N C2 H2B 109.5 . . ?

C1 C2 H2B 109.5 . . ?

H2A C2 H2B 108.1 . . ?

C4 C3 P2 111.5(2) . . ?

C4 C3 H3A 109.3 . . ?

P2 C3 H3A 109.3 . . ?

C4 C3 H3B 109.3 . . ?

P2 C3 H3B 109.3 . . ?

H3A C3 H3B 108.0 . . ?

N C4 C3 110.7(3) . . ?

N C4 H4A 109.5 . . ?

C3 C4 H4A 109.5 . . ?

N C4 H4B 109.5 . . ?

C3 C4 H4B 109.5 . . ?

H4A C4 H4B 108.1 . . ?

C10 C5 C6 110.7(3) . . ?

C10 C5 P1 114.0(2) . . ?

C6 C5 P1 115.2(3) . . ?

C10 C5 H5 105.3 . . ?

C6 C5 H5 105.3 . . ?

P1 C5 H5 105.3 . . ?

C7 C6 C5 109.5(3) . . ?

C7 C6 H6A 109.8 . . ?

C5 C6 H6A 109.8 . . ?

C7 C6 H6B 109.8 . . ?

C5 C6 H6B 109.8 . . ?

H6A C6 H6B 108.2 . . ?

C8 C7 C6 112.3(4) . . ?

C8 C7 H7A 109.1 . . ?

C6 C7 H7A 109.1 . . ?

C8 C7 H7B 109.1 . . ?

C6 C7 H7B 109.1 . . ?

H7A C7 H7B 107.9 . . ?

C7 C8 C9 111.5(4) . . ?

C7 C8 H8A 109.3 . . ?

C9 C8 H8A 109.3 . . ?

C7 C8 H8B 109.3 . . ?

C9 C8 H8B 109.3 . . ?

H8A C8 H8B 108.0 . . ?

C8 C9 C10 111.2(4) . . ?

C8 C9 H9A 109.4 . . ?

C10 C9 H9A 109.4 . . ?

C8 C9 H9B 109.4 . . ?

C10 C9 H9B 109.4 . . ?

H9A C9 H9B 108.0 . . ?

C5 C10 C9 110.8(3) . . ?

C5 C10 H10A 109.5 . . ?

C9 C10 H10A 109.5 . . ?

C5 C10 H10B 109.5 . . ?

C9 C10 H10B 109.5 . . ?

H10A C10 H10B 108.1 . . ?

C16 C11 C12 109.9(3) . . ?

C16 C11 P1 112.1(3) . . ?

C12 C11 P1 119.0(3) . . ?

C16 C11 H11 104.8 . . ?

C12 C11 H11 104.8 . . ?

P1 C11 H11 104.8 . . ?

C13 C12 C11 110.1(3) . . ?

C13 C12 H12A 109.6 . . ?

C11 C12 H12A 109.6 . . ?

C13 C12 H12B 109.6 . . ?

C11 C12 H12B 109.6 . . ?

H12A C12 H12B 108.2 . . ?

C14 C13 C12 112.1(3) . . ?

C14 C13 H13A 109.2 . . ?

C12 C13 H13A 109.2 . . ?

C14 C13 H13B 109.2 . . ?

C12 C13 H13B 109.2 . . ?

H13A C13 H13B 107.9 . . ?

C15 C14 C13 111.4(3) . . ?

C15 C14 H14A 109.4 . . ?

C13 C14 H14A 109.4 . . ?

C15 C14 H14B 109.4 . . ?

C13 C14 H14B 109.4 . . ?

H14A C14 H14B 108.0 . . ?

C14 C15 C16 111.9(4) . . ?

C14 C15 H15A 109.2 . . ?

C16 C15 H15A 109.2 . . ?

C14 C15 H15B 109.2 . . ?

C16 C15 H15B 109.2 . . ?

H15A C15 H15B 107.9 . . ?

C15 C16 C11 110.2(4) . . ?

C15 C16 H16A 109.6 . . ?

C11 C16 H16A 109.6 . . ?

C15 C16 H16B 109.6 . . ?

C11 C16 H16B 109.6 . . ?

H16A C16 H16B 108.1 . . ?

C18 C17 C22 113.5(4) . . ?

C18 C17 P2 118.9(3) . . ?

C22 C17 P2 111.2(3) . . ?

C18 C17 H17 103.7 . . ?

C22 C17 H17 103.7 . . ?

P2 C17 H17 103.7 . . ?

C17 C18 C19 110.2(4) . . ?

C17 C18 H18A 109.6 . . ?

C19 C18 H18A 109.6 . . ?

C17 C18 H18B 109.6 . . ?

C19 C18 H18B 109.6 . . ?

H18A C18 H18B 108.1 . . ?

C20 C19 C18 111.8(4) . . ?

C20 C19 H19A 109.3 . . ?

C18 C19 H19A 109.3 . . ?

C20 C19 H19B 109.3 . . ?

C18 C19 H19B 109.3 . . ?

H19A C19 H19B 107.9 . . ?

C21 C20 C19 111.4(5) . . ?

C21 C20 H20A 109.3 . . ?

C19 C20 H20A 109.3 . . ?

C21 C20 H20B 109.3 . . ?

C19 C20 H20B 109.3 . . ?

H20A C20 H20B 108.0 . . ?

C20 C21 C22 114.7(5) . . ?

C20 C21 H21A 108.6 . . ?

C22 C21 H21A 108.6 . . ?

C20 C21 H21B 108.6 . . ?

C22 C21 H21B 108.6 . . ?

H21A C21 H21B 107.6 . . ?

C17 C22 C21 111.4(4) . . ?

C17 C22 H22A 109.3 . . ?

C21 C22 H22A 109.3 . . ?

C17 C22 H22B 109.3 . . ?

C21 C22 H22B 109.3 . . ?

H22A C22 H22B 108.0 . . ?

C24 C23 C28 110.1(3) . . ?

C24 C23 P2 112.9(2) . . ?

C28 C23 P2 118.0(2) . . ?

C24 C23 H23 104.9 . . ?

C28 C23 H23 104.9 . . ?

P2 C23 H23 104.9 . . ?

C23 C24 C25 109.2(3) . . ?

C23 C24 H24A 109.8 . . ?

C25 C24 H24A 109.8 . . ?

C23 C24 H24B 109.8 . . ?

C25 C24 H24B 109.8 . . ?

H24A C24 H24B 108.3 . . ?

C26 C25 C24 111.2(4) . . ?

C26 C25 H25A 109.4 . . ?

C24 C25 H25A 109.4 . . ?

C26 C25 H25B 109.4 . . ?

C24 C25 H25B 109.4 . . ?

H25A C25 H25B 108.0 . . ?

C27 C26 C25 111.3(3) . . ?

C27 C26 H26A 109.4 . . ?

C25 C26 H26A 109.4 . . ?

C27 C26 H26B 109.4 . . ?

C25 C26 H26B 109.4 . . ?

H26A C26 H26B 108.0 . . ?

C26 C27 C28 111.3(3) . . ?

C26 C27 H27A 109.4 . . ?

C28 C27 H27A 109.4 . . ?

C26 C27 H27B 109.4 . . ?

C28 C27 H27B 109.4 . . ?

H27A C27 H27B 108.0 . . ?

C27 C28 C23 109.9(3) . . ?

C27 C28 H28A 109.7 . . ?

C23 C28 H28A 109.7 . . ?

C27 C28 H28B 109.7 . . ?

C23 C28 H28B 109.7 . . ?

H28A C28 H28B 108.2 . . ?

O C29 C30 120.2(7) . . ?

O C29 C31 121.2(7) . . ?

C30 C29 C31 118.5(5) . . ?

C29 C30 H30A 109.5 . . ?

C29 C30 H30B 109.5 . . ?

H30A C30 H30B 109.5 . . ?

C29 C30 H30C 109.5 . . ?

H30A C30 H30C 109.5 . . ?

H30B C30 H30C 109.5 . . ?

C29 C31 H31A 109.5 . . ?

C29 C31 H31B 109.5 . . ?

H31A C31 H31B 109.5 . . ?

C29 C31 H31C 109.5 . . ?

H31A C31 H31C 109.5 . . ?

H31B C31 H31C 109.5 . . ?



loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_distance_DA

_geom_hbond_angle_DHA

_geom_hbond_site_symmetry_A

N H1 Cl3 0.95 2.65 3.426(3) 139.5 3_775



_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        25.98

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.775

_refine_diff_density_min         -0.632

_refine_diff_density_rms         0.089

#==============================================================================







