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_2311957
_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          '[Cu2 Pb I5 (C12 H8 N2)2], 0.5I2'
_chemical_formula_moiety         'C24 H16 Cu2 I5 N4 Pb, 0.5(I2)'
_chemical_formula_sum            'C24 H16 Cu2 I6 N4 Pb'
_chemical_formula_weight         1456.08
_chemical_name_systematic
'Poly[[\m~3~-iodido-tri-\m~2~-iodido-iodido[bis(1,10-phenanthroline)copper(I)]copper(I)copper(II)lead(II)] hemiiodine]'
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 128.789(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5853(9)
_cell_length_b                   18.1041(8)
_cell_length_c                   13.0705(6)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1480
_cell_measurement_theta_min      3.3280
_cell_volume                     3243.5(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.842
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7250
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2007)
;
_exptl_crystal_colour            Gray
_exptl_crystal_density_diffrn    2.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.771
_refine_diff_density_min         -1.797
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0331P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                2846
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ov3096sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2311957