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_4347130
_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
'C58 H72 B2 Cl2 Cu4 N12 P2 S8 W2, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C62 H82 B2 Cl2 Cu4 N14 O2 P2 S8 W2'
_chemical_formula_weight         2088.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.091(5)
_cell_angle_beta                 71.087(5)
_cell_angle_gamma                71.093(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3572(4)
_cell_length_b                   14.0594(5)
_cell_length_c                   15.5995(12)
_cell_measurement_reflns_used    7535
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.1310
_cell_measurement_theta_min      3.4380
_cell_volume                     2015.1(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24580
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.391
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.567
_refine_diff_density_min         -3.850
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         24580
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+23.1339P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19692
_reflns_number_total             24580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02765_si_002.cif
_cod_data_source_block           compound5
_cod_database_code               4347130
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.728
_shelxl_version_number           2013-2
_shelx_res_checksum              54735
_shelx_hkl_checksum              44228