Syntheses and crystal structures of two heterometallic iodoplumbates containing mixed-valence copper(I/II).
Fan, Le Qing; Zhu, Xiao Tong; Acta crystallographica. Section C, Structural chemistry 73 (2017) 1098–1103; doi:10.1107/S2053229617015807

data_2311956
_publ_section_title
;
 Syntheses and crystal structures of two heterometallic iodoplumbates
 containing mixed-valence copper(I/II).
;
_journal_coeditor_code           OV3096
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              1098
_journal_page_last               1103
_journal_paper_doi               10.1107/S2053229617015807
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C16 H36 N)2 [Cu5 Pb6 (C3 H6 N1 S2)2 I18]'
_chemical_formula_moiety         'C38 H84 Cu5 I18 N4 Pb6 S4'
_chemical_formula_sum            'C38 H84 Cu5 I18 N4 Pb6 S4'
_chemical_formula_weight         4570.37
_chemical_name_systematic
;Poly[tetra-<i>n</i>-butylammonium
[bis(\m~2~-dimethyldithiocarbamato)dodeca-\m~3~-iodido-hexa-\m~2~-iodido-tetracopper(I)copper(II)hexalead(II)]]
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                94.449(3)
_cell_angle_beta                 92.316(3)
_cell_angle_gamma                119.009(4)
_cell_formula_units_Z            1
_cell_length_a                   13.5451(18)
_cell_length_b                   13.8890(19)
_cell_length_c                   14.4514(12)
_cell_measurement_reflns_used    4164
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0088
_cell_volume                     2361.0(5)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2007)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2007)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2007)
;
_computing_molecular_graphics
;
XP (Sheldrick, 1998)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15026
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.753
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2007)
;
_exptl_crystal_colour            Gray
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1995
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.251
_refine_diff_density_min         -2.973
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.0230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                5419
_reflns_number_total             8225
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           I
_cod_database_code               2311956