Reactions of Monodithiolene Tungsten(VI) Sulfido Complexes with Copper(I) in Relation to the Structure of the Active Site of Carbon Monoxide Dehydrogenase
Stanislav Groysman; Amit Majumdar; Shao-Liang Zheng; R. H. Holm; Inorganic Chemistry 49 (2010) 1082–1089; doi:10.1021/ic902066m

data_4314694
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Cambridge
Massachusetts 02138
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_name        'Prof. R. H. Holm'
_publ_section_title
;
 Reactions of Monodithiolene Tungsten(VI) Sulfido Complexes with Copper(I)
 in Relation to the Structure of the Active Site of Carbon Monoxide
 Dehydrogenase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1082
_journal_page_last               1089
_journal_paper_doi               10.1021/ic902066m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H30 Cu S2 Si2, C8 H20 N'
_chemical_formula_sum            'C44 H50 Cu N S2 Si2'
_chemical_formula_weight         776.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.349(4)
_cell_angle_beta                 96.600(5)
_cell_angle_gamma                117.022(4)
_cell_formula_units_Z            1
_cell_length_a                   9.448(3)
_cell_length_b                   9.582(3)
_cell_length_c                   12.742(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.41
_cell_volume                     1010.1(6)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6792
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.5042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                3978
_reflns_number_total             4720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902066m_si_001_06.cif
_cod_data_source_block           '[Et4N][Cu(SSiPh3)2]'
_cod_original_cell_volume        1010.0(5)
_cod_database_code               4314694