# 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



_publ_section_title              

;

A New Reactivity Pattern of Low-Valent Transition-Metal 

Hydroxo Complexes: Straightforward Synthesis of Hydrosulfido 

Complexes Via Reaction with Carbon Disulfide.

;



_publ_contact_author_name        'Dr Julio Perez'

_publ_contact_author_address     

;

Departamento de Quimica Organica e Inorganica - IUQOEM

Universidad de Oviedo

Facultad de Quimica -CSIC

Oviedo

33071

SPAIN

;



_publ_contact_author_phone       +34-85-102985

_publ_contact_author_fax         +34-85-103446

_publ_contact_author_email       japm@sauron.quimica.uniovi.es





loop_

_publ_author_name

_publ_author_address



'Dario C. Gerbino'

;

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'Eva Hevia'

;

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'Dolores Morales'

;

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'M. Elena Navarro-Clemente'

;

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'Julio Perez'

;

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;



'V.Riera'



;    

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'Daniel Miguel'

;    

Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química

Universidad de Oviedo

C/ Julian Claveria s/n

33006 Oviedo  (ASTURIAS)

SPAIN

;

'L.Riera'

;

Departamento de Quimica Inorganica

Facultad de Ciencias

Universidad de Valladolid

47071 Valladolid

SPAIN

;



data_Compound_3_(lr39bm)

_database_code_CSD                  193532



_audit_creation_method           SHELXL-97

_chemical_name_systematic        

; 

? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C18 H16 Mo N2 O2 S'

_chemical_formula_weight         420.33



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'

S S 0.1246 0.1234 '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           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                   8.6005(10)

_cell_length_b                   15.0923(17)

_cell_length_c                   13.5883(15)

_cell_angle_alpha                90.00

_cell_angle_beta                 101.228(2)

_cell_angle_gamma                90.00

_cell_volume                     1730.0(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    299(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       PRISM

_exptl_crystal_colour            RED_BLACK

_exptl_crystal_size_max          0.14

_exptl_crystal_size_mid          0.16

_exptl_crystal_size_min          0.21

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.614

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             848

_exptl_absorpt_coefficient_mu    0.891

_exptl_absorpt_correction_type   SADABS

_exptl_absorpt_correction_T_min  0.859004

_exptl_absorpt_correction_T_max  1.000000

_exptl_absorpt_process_details   ?



_exptl_special_details           

; 

? 

;



_diffrn_ambient_temperature      299(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            7677

_diffrn_reflns_av_R_equivalents  0.0236

_diffrn_reflns_av_sigmaI/netI    0.0241

_diffrn_reflns_limit_h_min       -9

_diffrn_reflns_limit_h_max       9

_diffrn_reflns_limit_k_min       -16

_diffrn_reflns_limit_k_max       16

_diffrn_reflns_limit_l_min       -14

_diffrn_reflns_limit_l_max       15

_diffrn_reflns_theta_min         2.04

_diffrn_reflns_theta_max         23.28

_reflns_number_total             2498

_reflns_number_gt                2135

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SHELXTL'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_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)+(0.0584P)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_number_reflns         2498

_refine_ls_number_parameters     221

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0370

_refine_ls_R_factor_gt           0.0296

_refine_ls_wR_factor_ref         0.0829

_refine_ls_wR_factor_gt          0.0787

_refine_ls_goodness_of_fit_ref   1.000

_refine_ls_restrained_S_all      1.000

_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 0.16413(3) 0.291779(19) 0.77404(2) 0.04072(14) Uani 1 1 d . . .

S1 S -0.01309(13) 0.24354(7) 0.89017(7) 0.0566(3) Uani 1 1 d G . .

H1 H -0.0048 0.1786 0.8853 0.085 Uiso 1 1 d G . .

N1 N 0.1864(3) 0.41376(17) 0.87190(19) 0.0394(6) Uani 1 1 d . . .

N2 N -0.0443(3) 0.37921(18) 0.7121(2) 0.0435(7) Uani 1 1 d . . .

C1 C 0.3257(5) 0.2135(2) 0.8503(3) 0.0525(9) Uani 1 1 d . . .

O1 O 0.4181(4) 0.1644(2) 0.8941(2) 0.0795(9) Uani 1 1 d . . .

C2 C 0.1020(4) 0.1806(3) 0.7017(3) 0.0522(9) Uani 1 1 d . . .

O2 O 0.0638(3) 0.1145(2) 0.6628(2) 0.0741(8) Uani 1 1 d . . .

C3 C 0.4119(5) 0.3374(3) 0.7501(3) 0.0613(10) Uani 1 1 d . . .

H3A H 0.4650 0.3823 0.7957 0.074 Uiso 1 1 calc R . .

H3B H 0.4824 0.2915 0.7345 0.074 Uiso 1 1 calc R . .

C4 C 0.2931(5) 0.3671(3) 0.6703(3) 0.0558(10) Uani 1 1 d . . .

C5 C 0.2119(5) 0.2986(3) 0.6115(3) 0.0610(11) Uani 1 1 d . . .

H5A H 0.2763 0.2516 0.5916 0.073 Uiso 1 1 calc R . .

H5B H 0.1235 0.3159 0.5593 0.073 Uiso 1 1 calc R . .

C6 C 0.2572(6) 0.4637(3) 0.6477(4) 0.0770(13) Uani 1 1 d . . .

H6A H 0.3293 0.4866 0.6082 0.116 Uiso 1 1 calc R . .

H6B H 0.2691 0.4962 0.7094 0.116 Uiso 1 1 calc R . .

H6C H 0.1504 0.4697 0.6110 0.116 Uiso 1 1 calc R . .

C11 C 0.2938(4) 0.4270(2) 0.9547(2) 0.0429(8) Uani 1 1 d . . .

H11 H 0.3713 0.3841 0.9740 0.052 Uiso 1 1 calc R . .

C12 C 0.2961(4) 0.5031(2) 1.0147(2) 0.0456(8) Uani 1 1 d . . .

H12 H 0.3725 0.5096 1.0730 0.055 Uiso 1 1 calc R . .

C13 C 0.1855(4) 0.5668(2) 0.9866(2) 0.0450(8) Uani 1 1 d . . .

H13 H 0.1869 0.6180 1.0249 0.054 Uiso 1 1 calc R . .

C14 C 0.0690(4) 0.5558(2) 0.8998(2) 0.0399(8) Uani 1 1 d . . .

C15 C -0.0530(4) 0.6196(2) 0.8651(3) 0.0475(8) Uani 1 1 d . . .

H15 H -0.0541 0.6726 0.8998 0.057 Uiso 1 1 calc R . .

C16 C -0.1662(4) 0.6041(2) 0.7832(3) 0.0531(9) Uani 1 1 d . . .

H16 H -0.2424 0.6472 0.7614 0.064 Uiso 1 1 calc R . .

C17 C -0.1705(4) 0.5217(3) 0.7292(2) 0.0490(9) Uani 1 1 d . . .

C18 C -0.2899(5) 0.4993(3) 0.6471(3) 0.0624(11) Uani 1 1 d . . .

H18 H -0.3708 0.5392 0.6233 0.075 Uiso 1 1 calc R . .

C19 C -0.2866(5) 0.4194(3) 0.6030(3) 0.0650(11) Uani 1 1 d . . .

H19 H -0.3680 0.4032 0.5505 0.078 Uiso 1 1 calc R . .

C20 C -0.1624(4) 0.3614(3) 0.6357(3) 0.0545(9) Uani 1 1 d . . .

H20 H -0.1615 0.3075 0.6026 0.065 Uiso 1 1 calc R . .

C21 C 0.0718(4) 0.4767(2) 0.8457(2) 0.0364(7) Uani 1 1 d . . .

C22 C -0.0504(4) 0.4585(2) 0.7596(2) 0.0405(8) Uani 1 1 d . . .



loop_

_atom_site_aniso_label

_atom_site_aniso_U_11

_atom_site_aniso_U_22

_atom_site_aniso_U_33

_atom_site_aniso_U_23

_atom_site_aniso_U_13

_atom_site_aniso_U_12

Mo1 0.0435(2) 0.0416(2) 0.0350(2) -0.00621(12) 0.00270(13) 0.00159(13)

S1 0.0668(6) 0.0550(6) 0.0496(6) -0.0057(5) 0.0158(5) -0.0130(5)

N1 0.0422(16) 0.0403(15) 0.0348(15) -0.0008(12) 0.0054(12) -0.0031(13)

N2 0.0446(16) 0.0465(17) 0.0374(15) -0.0021(13) 0.0032(13) -0.0003(13)

C1 0.057(2) 0.051(2) 0.045(2) -0.0100(18) 0.0007(19) -0.0014(19)

O1 0.081(2) 0.075(2) 0.072(2) 0.0036(17) -0.0122(16) 0.0244(18)

C2 0.047(2) 0.059(2) 0.050(2) -0.011(2) 0.0071(17) 0.0027(18)

O2 0.078(2) 0.0625(18) 0.078(2) -0.0371(16) 0.0076(16) -0.0109(15)

C3 0.052(2) 0.075(3) 0.059(3) -0.015(2) 0.0175(19) -0.006(2)

C4 0.058(2) 0.066(3) 0.048(2) 0.0005(19) 0.0234(19) 0.002(2)

C5 0.060(3) 0.078(3) 0.044(2) -0.0090(19) 0.0089(19) 0.008(2)

C6 0.091(3) 0.069(3) 0.081(3) 0.016(2) 0.042(3) 0.001(2)

C11 0.0415(18) 0.0443(19) 0.0414(19) 0.0009(15) 0.0042(15) -0.0020(15)

C12 0.052(2) 0.044(2) 0.0399(19) -0.0040(16) 0.0068(16) -0.0094(17)

C13 0.057(2) 0.0380(19) 0.044(2) -0.0082(15) 0.0195(17) -0.0104(17)

C14 0.0427(18) 0.0381(18) 0.0426(19) 0.0028(15) 0.0171(15) -0.0065(15)

C15 0.055(2) 0.0411(19) 0.050(2) -0.0017(16) 0.0196(18) 0.0003(17)

C16 0.051(2) 0.048(2) 0.063(3) 0.0068(19) 0.0166(19) 0.0106(17)

C17 0.044(2) 0.055(2) 0.049(2) 0.0095(17) 0.0101(16) 0.0025(17)

C18 0.049(2) 0.073(3) 0.061(3) 0.004(2) -0.0013(19) 0.010(2)

C19 0.051(2) 0.083(3) 0.053(2) -0.001(2) -0.0105(18) 0.000(2)

C20 0.057(2) 0.060(2) 0.043(2) -0.0057(17) -0.0005(17) -0.0022(19)

C21 0.0388(17) 0.0361(17) 0.0360(18) 0.0016(14) 0.0114(14) -0.0029(14)

C22 0.0405(18) 0.0441(19) 0.0382(18) 0.0059(15) 0.0109(14) 0.0012(15)



_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 C1 1.960(4) . ?

Mo1 C2 1.965(4) . ?

Mo1 N2 2.253(3) . ?

Mo1 N1 2.257(3) . ?

Mo1 C4 2.263(4) . ?

Mo1 C3 2.322(4) . ?

Mo1 C5 2.326(4) . ?

Mo1 S1 2.5059(10) . ?

N1 C11 1.324(4) . ?

N1 C21 1.365(4) . ?

N2 C20 1.331(4) . ?

N2 C22 1.366(4) . ?

C1 O1 1.162(5) . ?

C2 O2 1.148(4) . ?

C3 C4 1.411(6) . ?

C4 C5 1.406(5) . ?

C4 C6 1.509(6) . ?

C11 C12 1.407(5) . ?

C12 C13 1.354(5) . ?

C13 C14 1.400(5) . ?

C14 C21 1.405(4) . ?

C14 C15 1.435(5) . ?

C15 C16 1.348(5) . ?

C16 C17 1.442(5) . ?

C17 C18 1.402(5) . ?

C17 C22 1.407(5) . ?

C18 C19 1.349(6) . ?

C19 C20 1.386(6) . ?

C21 C22 1.438(5) . ?



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

C1 Mo1 C2 81.10(15) . . ?

C1 Mo1 N2 168.95(13) . . ?

C2 Mo1 N2 101.19(13) . . ?

C1 Mo1 N1 102.15(12) . . ?

C2 Mo1 N1 167.05(13) . . ?

N2 Mo1 N1 73.28(10) . . ?

C1 Mo1 C4 104.43(16) . . ?

C2 Mo1 C4 103.65(15) . . ?

N2 Mo1 C4 85.63(12) . . ?

N1 Mo1 C4 87.80(12) . . ?

C1 Mo1 C3 71.14(16) . . ?

C2 Mo1 C3 110.52(15) . . ?

N2 Mo1 C3 117.36(14) . . ?

N1 Mo1 C3 82.30(12) . . ?

C4 Mo1 C3 35.83(14) . . ?

C1 Mo1 C5 106.88(15) . . ?

C2 Mo1 C5 69.14(15) . . ?

N2 Mo1 C5 83.93(12) . . ?

N1 Mo1 C5 120.86(12) . . ?

C4 Mo1 C5 35.67(14) . . ?

C3 Mo1 C5 61.14(14) . . ?

C1 Mo1 S1 87.00(12) . . ?

C2 Mo1 S1 85.84(11) . . ?

N2 Mo1 S1 82.42(8) . . ?

N1 Mo1 S1 81.85(7) . . ?

C4 Mo1 S1 166.02(10) . . ?

C3 Mo1 S1 149.50(11) . . ?

C5 Mo1 S1 148.46(11) . . ?

C11 N1 C21 117.7(3) . . ?

C11 N1 Mo1 126.1(2) . . ?

C21 N1 Mo1 116.09(19) . . ?

C20 N2 C22 116.9(3) . . ?

C20 N2 Mo1 127.1(2) . . ?

C22 N2 Mo1 116.0(2) . . ?

O1 C1 Mo1 177.5(3) . . ?

O2 C2 Mo1 177.3(4) . . ?

C4 C3 Mo1 69.8(2) . . ?

C5 C4 C3 114.0(4) . . ?

C5 C4 C6 122.4(4) . . ?

C3 C4 C6 123.6(4) . . ?

C5 C4 Mo1 74.6(2) . . ?

C3 C4 Mo1 74.4(2) . . ?

C6 C4 Mo1 120.5(3) . . ?

C4 C5 Mo1 69.7(2) . . ?

N1 C11 C12 123.0(3) . . ?

C13 C12 C11 119.1(3) . . ?

C12 C13 C14 120.1(3) . . ?

C13 C14 C21 117.4(3) . . ?

C13 C14 C15 123.7(3) . . ?

C21 C14 C15 119.0(3) . . ?

C16 C15 C14 121.3(3) . . ?

C15 C16 C17 120.8(3) . . ?

C18 C17 C22 116.9(3) . . ?

C18 C17 C16 123.7(3) . . ?

C22 C17 C16 119.4(3) . . ?

C19 C18 C17 119.6(4) . . ?

C18 C19 C20 120.3(4) . . ?

N2 C20 C19 123.0(4) . . ?

N1 C21 C14 122.7(3) . . ?

N1 C21 C22 117.1(3) . . ?

C14 C21 C22 120.2(3) . . ?

N2 C22 C17 123.2(3) . . ?

N2 C22 C21 117.5(3) . . ?

C17 C22 C21 119.2(3) . . ?



_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        23.28

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.800

_refine_diff_density_min         -0.261

_refine_diff_density_rms         0.072







#===END



data_Compound_4_(d3am)

_database_code_CSD                  193533



_audit_creation_method           SHELXL-97

_chemical_name_systematic        

; 

? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C13 H9 N2 O3 Re S'

_chemical_formula_weight         459.48



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'

S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Re Re -1.0185 7.2310 '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                   8.174(5)

_cell_length_b                   8.372(5)

_cell_length_c                   10.931(7)

_cell_angle_alpha                100.773(9)

_cell_angle_beta                 103.413(9)

_cell_angle_gamma                93.959(9)

_cell_volume                     709.8(8)

_cell_formula_units_Z            2

_cell_measurement_temperature    299(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       PLATE

_exptl_crystal_colour            ORANGE

_exptl_crystal_size_max          0.05

_exptl_crystal_size_mid          0.11

_exptl_crystal_size_min          0.17

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    2.150

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             432

_exptl_absorpt_coefficient_mu    8.713

_exptl_absorpt_correction_type   SADABS

_exptl_absorpt_correction_T_min  0.589750

_exptl_absorpt_correction_T_max  1.000000

_exptl_absorpt_process_details   ?



_exptl_special_details           

; 

? 

;



_diffrn_ambient_temperature      299(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            3249

_diffrn_reflns_av_R_equivalents  0.0251

_diffrn_reflns_av_sigmaI/netI    0.0352

_diffrn_reflns_limit_h_min       -9

_diffrn_reflns_limit_h_max       6

_diffrn_reflns_limit_k_min       -9

_diffrn_reflns_limit_k_max       9

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       12

_diffrn_reflns_theta_min         1.96

_diffrn_reflns_theta_max         23.62

_reflns_number_total             2051

_reflns_number_gt                1861

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SHELXTL'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_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)+(0.0433P)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     SHELXL

_refine_ls_extinction_coef       0.0006(4)

_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

_refine_ls_number_reflns         2051

_refine_ls_number_parameters     185

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0316

_refine_ls_R_factor_gt           0.0279

_refine_ls_wR_factor_ref         0.0675

_refine_ls_wR_factor_gt          0.0662

_refine_ls_goodness_of_fit_ref   1.018

_refine_ls_restrained_S_all      1.018

_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

Re1 Re 0.23778(3) 0.30170(3) 0.30622(3) 0.03108(15) Uani 1 1 d . . .

S1 S 0.2550(3) 0.1378(3) 0.0930(2) 0.0476(5) Uani 1 1 d G . .

H1 H 0.1147 0.0904 0.0270 0.071 Uiso 1 1 d R . .

N1 N 0.0710(7) 0.0905(7) 0.3124(6) 0.0333(13) Uani 1 1 d . . .

N2 N -0.0146(7) 0.3366(6) 0.2018(5) 0.0307(13) Uani 1 1 d . . .

C1 C 0.2161(8) 0.4292(8) 0.4686(9) 0.0381(18) Uani 1 1 d . . .

O1 O 0.2021(8) 0.5049(7) 0.5625(6) 0.0556(15) Uani 1 1 d . . .

C2 C 0.3629(9) 0.4884(10) 0.2800(8) 0.0440(19) Uani 1 1 d . . .

O2 O 0.4377(8) 0.6029(8) 0.2632(6) 0.0681(18) Uani 1 1 d . . .

C3 C 0.4476(9) 0.2354(9) 0.3945(8) 0.0421(18) Uani 1 1 d . . .

O3 O 0.5671(7) 0.1873(8) 0.4434(7) 0.0723(19) Uani 1 1 d . . .

C11 C 0.1232(10) -0.0346(8) 0.3684(7) 0.0412(18) Uani 1 1 d . . .

H11 H 0.2381 -0.0321 0.4059 0.049 Uiso 1 1 calc R . .

C12 C 0.0154(10) -0.1640(9) 0.3724(8) 0.049(2) Uani 1 1 d . . .

H12 H 0.0568 -0.2471 0.4122 0.058 Uiso 1 1 calc R . .

C13 C -0.1558(12) -0.1712(9) 0.3170(8) 0.052(2) Uani 1 1 d . . .

H13 H -0.2313 -0.2586 0.3188 0.062 Uiso 1 1 calc R . .

C14 C -0.2125(9) -0.0437(9) 0.2582(8) 0.0428(18) Uani 1 1 d . . .

H14 H -0.3270 -0.0447 0.2202 0.051 Uiso 1 1 calc R . .

C15 C -0.0952(9) 0.0854(8) 0.2572(7) 0.0332(16) Uani 1 1 d . . .

C16 C -0.1435(8) 0.2213(8) 0.1910(6) 0.0307(15) Uani 1 1 d . . .

C17 C -0.3055(9) 0.2327(9) 0.1233(8) 0.046(2) Uani 1 1 d . . .

H17 H -0.3930 0.1532 0.1193 0.056 Uiso 1 1 calc R . .

C18 C -0.3390(9) 0.3590(10) 0.0623(8) 0.049(2) Uani 1 1 d . . .

H18 H -0.4475 0.3641 0.0137 0.059 Uiso 1 1 calc R . .

C19 C -0.2093(10) 0.4786(10) 0.0741(8) 0.050(2) Uani 1 1 d . . .

H19 H -0.2291 0.5676 0.0352 0.060 Uiso 1 1 calc R . .

C20 C -0.0507(9) 0.4652(9) 0.1436(7) 0.0388(17) Uani 1 1 d . . .

H20 H 0.0363 0.5472 0.1517 0.047 Uiso 1 1 calc R . .



loop_

_atom_site_aniso_label

_atom_site_aniso_U_11

_atom_site_aniso_U_22

_atom_site_aniso_U_33

_atom_site_aniso_U_23

_atom_site_aniso_U_13

_atom_site_aniso_U_12

Re1 0.02534(19) 0.0337(2) 0.0328(2) 0.00818(13) 0.00375(12) 0.00253(11)

S1 0.0400(10) 0.0591(12) 0.0389(12) -0.0021(10) 0.0115(9) 0.0000(9)

N1 0.035(3) 0.033(3) 0.032(4) 0.008(3) 0.006(3) 0.009(3)

N2 0.031(3) 0.031(3) 0.027(3) 0.002(3) 0.005(2) 0.005(2)

C1 0.027(4) 0.026(4) 0.060(6) 0.020(4) 0.001(4) -0.001(3)

O1 0.071(4) 0.048(3) 0.047(4) 0.004(3) 0.018(3) 0.005(3)

C2 0.032(4) 0.061(5) 0.038(5) 0.013(4) 0.004(3) 0.008(4)

O2 0.061(4) 0.068(4) 0.075(5) 0.030(4) 0.012(3) -0.018(3)

C3 0.033(4) 0.045(4) 0.042(5) 0.010(4) -0.002(3) 0.001(3)

O3 0.040(3) 0.075(4) 0.094(5) 0.031(4) -0.013(3) 0.019(3)

C11 0.044(4) 0.038(4) 0.045(5) 0.015(4) 0.010(4) 0.010(3)

C12 0.054(5) 0.039(4) 0.055(6) 0.016(4) 0.013(4) 0.006(4)

C13 0.075(6) 0.034(4) 0.047(5) 0.010(4) 0.019(5) -0.005(4)

C14 0.037(4) 0.041(4) 0.044(5) 0.005(4) 0.006(4) -0.009(3)

C15 0.039(4) 0.031(4) 0.032(4) 0.006(3) 0.012(3) 0.006(3)

C16 0.028(4) 0.035(4) 0.027(4) 0.003(3) 0.006(3) 0.006(3)

C17 0.030(4) 0.050(5) 0.061(6) 0.015(4) 0.011(4) 0.010(3)

C18 0.032(4) 0.056(5) 0.054(6) 0.011(4) -0.001(4) 0.015(4)

C19 0.051(5) 0.053(5) 0.056(6) 0.024(4) 0.017(4) 0.027(4)

C20 0.038(4) 0.045(4) 0.035(4) 0.013(4) 0.008(3) 0.009(3)



_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

Re1 C2 1.911(8) . ?

Re1 C3 1.935(7) . ?

Re1 C1 1.946(9) . ?

Re1 N1 2.178(6) . ?

Re1 N2 2.182(5) . ?

Re1 S1 2.514(2) . ?

N1 C15 1.346(9) . ?

N1 C11 1.355(8) . ?

N2 C16 1.347(8) . ?

N2 C20 1.365(9) . ?

C1 O1 1.135(9) . ?

C2 O2 1.168(9) . ?

C3 O3 1.138(8) . ?

C11 C12 1.362(10) . ?

C12 C13 1.382(12) . ?

C13 C14 1.398(10) . ?

C14 C15 1.398(9) . ?

C15 C16 1.487(9) . ?

C16 C17 1.378(10) . ?

C17 C18 1.363(11) . ?

C18 C19 1.374(11) . ?

C19 C20 1.366(10) . ?



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

C2 Re1 C3 89.4(3) . . ?

C2 Re1 C1 89.6(3) . . ?

C3 Re1 C1 89.9(3) . . ?

C2 Re1 N1 172.4(3) . . ?

C3 Re1 N1 97.2(3) . . ?

C1 Re1 N1 94.2(2) . . ?

C2 Re1 N2 98.9(3) . . ?

C3 Re1 N2 171.1(2) . . ?

C1 Re1 N2 93.5(2) . . ?

N1 Re1 N2 74.3(2) . . ?

C2 Re1 S1 91.0(2) . . ?

C3 Re1 S1 92.1(2) . . ?

C1 Re1 S1 177.97(19) . . ?

N1 Re1 S1 85.04(16) . . ?

N2 Re1 S1 84.48(15) . . ?

C15 N1 C11 118.2(6) . . ?

C15 N1 Re1 117.4(4) . . ?

C11 N1 Re1 124.4(5) . . ?

C16 N2 C20 117.5(6) . . ?

C16 N2 Re1 117.9(4) . . ?

C20 N2 Re1 124.6(5) . . ?

O1 C1 Re1 179.1(6) . . ?

O2 C2 Re1 179.2(7) . . ?

O3 C3 Re1 176.1(7) . . ?

N1 C11 C12 123.1(7) . . ?

C11 C12 C13 119.7(7) . . ?

C12 C13 C14 118.3(7) . . ?

C15 C14 C13 119.2(7) . . ?

N1 C15 C14 121.6(6) . . ?

N1 C15 C16 115.7(6) . . ?

C14 C15 C16 122.7(6) . . ?

N2 C16 C17 121.2(6) . . ?

N2 C16 C15 114.6(6) . . ?

C17 C16 C15 124.2(6) . . ?

C18 C17 C16 120.8(7) . . ?

C17 C18 C19 118.6(7) . . ?

C20 C19 C18 119.2(7) . . ?

N2 C20 C19 122.7(7) . . ?



_diffrn_measured_fraction_theta_max 0.956

_diffrn_reflns_theta_full        23.62

_diffrn_measured_fraction_theta_full 0.956

_refine_diff_density_max         1.420

_refine_diff_density_min         -0.979

_refine_diff_density_rms         0.150





#===END

