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_7223023
_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        ' Pb/Cu bimetallic thiolate'
_chemical_formula_sum            'C30 H34 Cu N4 O4 S2'
_chemical_formula_weight         642.30
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-01 deposited with the CCDC.
2015-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.1840(15)
_cell_length_b                   10.4657(4)
_cell_length_c                   10.5136(4)
_cell_measurement_reflns_used    59
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0970
_cell_measurement_theta_min      3.1338
_cell_volume                     3101.1(2)
_computing_cell_refinement       'crysalisPro, Agilent Technologies Ltd'
_computing_data_collection       'crysalisPro, Agilent Technologies Ltd'
_computing_data_reduction        'crysalisPro, Agilent Technologies Ltd'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.0938
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'XCalibur Eos, Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              "'Enhance (Mo) X-ray Source'"
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.8437
_exptl_absorpt_correction_T_min  0.7908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'crysalisPro, Agilent Technologies Ltd'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.230(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                3737
_reflns_number_total             4796
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra15195c2.cif
_cod_data_source_block           pbcus1
_cod_database_code               7223023