Rich Synthetic and Structural Chemistry of Polynuclear Pb(II)-Cu(I)/Ag(I) Heterobimetallic Thiolate Clusters, their Decomposition and Generation of a Cu(II) Hydrosulfide Variant.
Gupta, Geetika; Bhattacharya, Subrato; RSC Adv.  (2015) –; doi:10.1039/C5RA15195C

data_7223020
_publ_section_title
;
 Rich Synthetic and Structural Chemistry of Polynuclear Pb(II)-Cu(I)/Ag(I)
 Heterobimetallic Thiolate Clusters, their Decomposition and Generation of
 a Cu(II) Hydrosulfide Variant.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA15195C
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_compound_source        Synthesized
_chemical_formula_moiety         (PPh3)3Cu(SPh)7Pb
_chemical_formula_sum            'C97 H81 Cl3 Cu5 O6 P3 Pb S7'
_chemical_formula_weight         2291.19
_chemical_name_common            'Copper-lead thiolate cluster'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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           SHELXL-97
_audit_update_record
;
2015-06-30 deposited with the CCDC.
2015-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                74.232(9)
_cell_angle_beta                 75.087(8)
_cell_angle_gamma                60.183(10)
_cell_formula_units_Z            2
_cell_length_a                   15.6761(15)
_cell_length_b                   15.7459(16)
_cell_length_c                   24.799(2)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5614
_cell_measurement_theta_min      3.0505
_cell_volume                     5056.0(10)
_computing_cell_refinement       'CrysAlis Pro, Agilent Technologies Ltd.'
_computing_data_collection       'CrysAlis Pro, Agilent Technologies Ltd.'
_computing_data_reduction        'CrysAlis Pro, Agilent Technologies Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_sigmaI/netI    0.2519
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27344
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.44
_diffrn_reflns_theta_min         3.09
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.5841
_exptl_absorpt_correction_T_min  0.4553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis Pro, Agilent Technologies Ltd.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         21606
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.2045
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                17840
_reflns_number_total             21606
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra15195c2.cif
_cod_data_source_block           pbtp-cu
_cod_original_cell_volume        5055.9(9)
_cod_database_code               7223020