Diverse Tp*-Capped W-Cu-S Clusters from One-Pot Assembly Involving in Situ Thiolation of Phosphines.
Zhao, Xin; Zhou, Feng; Liu, Quan; Chen, Qiu-Fang; Yang, Jun-Yi; Zhang, Wen-Hua; Song, Ying-Lin; Lang, Jian-Ping; Inorganic chemistry 55 (2016) 1861–1871; doi:10.1021/acs.inorgchem.5b02765

data_4347127
_publ_section_title
;
 Diverse Tp*-Capped W-Cu-S Clusters from One-Pot Assembly Involving in
 Situ Thiolation of Phosphines.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1861
_journal_page_last               1871
_journal_paper_doi               10.1021/acs.inorgchem.5b02765
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C56 H68 B2 Cl2 Cu4 N12 P2 S6 W2'
_chemical_formula_sum            'C56 H68 B2 Cl2 Cu4 N12 P2 S6 W2'
_chemical_formula_weight         1877.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-05-15 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.371(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0020(6)
_cell_length_b                   15.1694(8)
_cell_length_c                   19.7883(11)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.32
_cell_volume                     3237.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_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  0.0991
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50834
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  0.8189
_exptl_absorpt_correction_T_min  0.1463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.573
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8035
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+21.8059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                5610
_reflns_number_total             8035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02765_si_002.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4347127
_publcif_datablock.id            {95282c62-bbe8-4b4c-a079-73e708be5fd2}