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_4347132
_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
'C132 H130 B4 Cl Cu12 N24 P6 S24 W4, F6 P, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C133.5 H133 B4 Cl4 Cu12 F6 N24 O0 P7 S24 W4'
_chemical_formula_weight         4856.78
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-27 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.4883(3)
_cell_length_b                   18.4883(3)
_cell_length_c                   46.7635(15)
_cell_measurement_reflns_used    18748
_cell_measurement_temperature    285(2)
_cell_measurement_theta_max      29.9360
_cell_measurement_theta_min      3.4650
_cell_volume                     13843.0(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      285(2)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            34425
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.084
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.277
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             7131
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.529
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6293
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+162.0904P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4973
_reflns_number_total             6293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02765_si_002.cif
_cod_data_source_block           Compound7
_cod_original_cell_volume        13843.0(6)
_cod_original_formula_sum
'C133.50 H133 B4 Cl4 Cu12 F6 N24 O0 P7 S24 W4'
_cod_database_code               4347132
_publcif_datablock.id            {1ca2fa55-b5ad-4ef6-b52e-b224027af6a3}
_shelx_estimated_absorpt_t_min   0.360
_shelx_estimated_absorpt_t_max   0.628
_shelxl_version_number           2013-2
_shelx_res_checksum              92410
_shelx_hkl_checksum              64667