μ~3~-Iodo-tri-μ~3~-sulfido-sulfidotris[tris(4-methoxyphenyl)phosphine-κ<i>P</i>]tricopper(I)tungsten(VI) <i>N</i>,<i>N</i>-dimethylformide solvate
Tang, Guodong; Zhang, Jinfang; Zhang, Chi; Acta Crystallographica Section E 64 (2008) m72–m73; doi:10.1107/S1600536807055997

data_2216927
_publ_section_title
;\m~3~-Iodo-tri-\m~3~-sulfido-sulfidotris[tris(4-methoxyphenyl)phosphine-\k<i>P</i>]tricopper(I)tungsten(VI)
 <i>N</i>,<i>N</i>-dimethylformide solvate
;
_journal_coeditor_code           BR2058
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m72
_journal_page_last               m73
_journal_paper_doi               10.1107/S1600536807055997
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu3 W I S4 (C21 H21 O3 P)3], C3 H7 N O'
_chemical_formula_moiety         'C63 H63 Cu3 I O9 P3 S4 W, C3 H7 N O'
_chemical_formula_sum            'C66 H70 Cu3 I N O10 P3 S4 W'
_chemical_formula_weight         1759.75
_chemical_name_systematic
;
\m~3~-Iodo-tri-\m~3~-sulfido-sulfidotris[tris(4-methoxyphenyl)phosphine-
\kP]tricopper(I)tungsten(VI) N,N-dimethylformide solvate
;
_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           'SHELXTL (Sheldrick, 2000)'
_cell_angle_alpha                68.869(5)
_cell_angle_beta                 84.706(6)
_cell_angle_gamma                80.605(6)
_cell_formula_units_Z            2
_cell_length_a                   10.5383(11)
_cell_length_b                   18.5135(16)
_cell_length_c                   19.3412(19)
_cell_measurement_reflns_used    13164
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     3470.2(6)
_computing_cell_refinement       'CrystalClear (Rigaku, 2000)'
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalClear (Rigaku, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL  (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34152
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         12730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0341P)^2^+1.0220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                11088
_reflns_number_total             12730
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2058.cif
_cod_data_source_block           I
_cod_database_code               2216927
_cod_database_fobs_code          2216927