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_7223021
_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_compound_source        SYNTHESISED
_chemical_formula_moiety         'C96 H80 Cu2 P4 Pb S4, C6 H6 S'
_chemical_formula_sum            'C102 H86 Cu2 P4 Pb S5'
_chemical_formula_weight         296.95
_chemical_name_common            'COPPERR-LEAD THIOLATE'
_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                100.487(4)
_cell_angle_beta                 90.174(4)
_cell_angle_gamma                118.261(5)
_cell_formula_units_Z            13
_cell_length_a                   12.8133(7)
_cell_length_b                   13.2814(7)
_cell_length_c                   30.5065(15)
_cell_measurement_reflns_used    2930
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1354
_cell_measurement_theta_min      3.0369
_cell_volume                     4472.4(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'XCalibur Eos, Oxford'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19385
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis Pro, Agilent Technologies Ltd'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.867
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         15624
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.2923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                9986
_reflns_number_total             15624
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra15195c2.cif
_cod_data_source_block           pbtp-cuy
_cod_original_cell_volume        4472.4(4)
_cod_database_code               7223021