Assembly of Three WS3Cu2 Cluster Units by μ3-S Bridges: Synthesis of [PPh4][{(C5Me5)WS3Cu2}3S2]
Jian-Ping Lang; Kazuyuki Tatsumi; Inorganic Chemistry 37 (1998) 160–162; doi:10.1021/ic970894x

data_4322594
_publ_section_title
;
 Assembly of Three WS3Cu2 Cluster Units by \m3-S Bridges: Synthesis of
 [PPh4][{(C5Me5)WS3Cu2}3S2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              160
_journal_page_last               162
_journal_paper_doi               10.1021/ic970894x
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C60 H74 Cu6 N3 P S11 W3'
_chemical_formula_weight         2153.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Mon Oct 20 21:49:00 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 91.35(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.477(4)
_cell_length_b                   21.652(5)
_cell_length_c                   21.623(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      11.3
_cell_volume                     7244(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00627
_diffrn_orient_matrix_UB_12      0.01737
_diffrn_orient_matrix_UB_13      -0.04251
_diffrn_orient_matrix_UB_21      0.01419
_diffrn_orient_matrix_UB_22      0.04133
_diffrn_orient_matrix_UB_23      0.01821
_diffrn_orient_matrix_UB_31      0.06274
_diffrn_orient_matrix_UB_32      -0.01108
_diffrn_orient_matrix_UB_33      0.00125
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_sigmaI/netI    0.095
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10197
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        3.86
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4168.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.37
_refine_diff_density_min         -1.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.630
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     484
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         0.1360
_refine_ls_shift/esd_mean        0.0080
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00026|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0552
_reflns_number_observed          5563
_reflns_number_total             9753
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic970894x.cif
_cod_data_source_block           '[PPh4][(Cp*WS3)3Cu6S2].3CH'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00026|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00026|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7244(2)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C60 H74 Cu6 N3 P S11 W3 '
_cod_database_code               4322594