Crystal structure of the lead-containing organic‒inorganic hybrid: (C~18~H~26~N~2~)~3~[Pb~4~I~14~(DMSO)~2~]·2DMSO
Li, Li; Zhao, Dan; Liu, Zhi; Zhang, Dingchao; Hu, Zhenhao; Li, Kunlun; Yang, Jing; Acta Crystallographica Section E 74 (2018) 1878–1880; doi:10.1107/S2056989018016584

data_2242761
_publ_section_title
;
 Crystal structure of the lead-containing organic--inorganic hybrid:
 (C~18~H~26~N~2~)~3~[Pb~4~I~14~(DMSO)~2~]&#x00B7;2DMSO
;
_journal_coeditor_code           EX2016
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1878
_journal_page_last               1880
_journal_paper_doi               10.1107/S2056989018016584
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'(C18 H26 N2)3 [Pb4 I14 (C2 H6 O S)2], 2C2 H6 O S'
_chemical_formula_moiety
'3(C18 H26 N2 2+), C4 H12 I14 O2 Pb4 S2 6-, 2(C2 H6 OS)'
_chemical_formula_sum            'C62 H102 I14 N6 O4 Pb4 S4'
_chemical_formula_weight         3729.08
_chemical_name_systematic
;
Tris(1,1'-dibutyl-4,4'-bipyridine-1,1'-diium) bis(dimethyl
sulfoxide)di-\m~3~-iodido-tetra-\m~2~-iodido-octaiodidotetralead(II)
dimethyl sulfoxide disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           APEX3
_cell_angle_alpha                80.3050(10)
_cell_angle_beta                 78.4490(10)
_cell_angle_gamma                81.7530(10)
_cell_formula_units_Z            1
_cell_length_a                   11.5011(10)
_cell_length_b                   14.2262(13)
_cell_length_c                   16.2969(14)
_cell_measurement_reflns_used    29882
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.8
_cell_volume                     2558.5(4)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX3 CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24466
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    10.904
_exptl_absorpt_correction_T_max  0.4403
_exptl_absorpt_correction_T_min  0.0654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2017)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1682
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.472
_refine_diff_density_min         -1.716
_refine_ls_extinction_coef       0.00081(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXTL (Bruker, 2017)
;
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+3.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                8219
_reflns_number_total             8975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ex2016sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C31 H51 I7 N3 O2 Pb2 S2'
_cod_original_formula_weight         1864.54
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2242761
_cod_database_fobs_code 2242761