Crystal structure of tris(3-iodopyridin-1-ium) catena-poly[(hexachlorido-κ1 Cl)-(μ2-trichlorido-κ2 Cl:Cl)diantimony(III)], C15H15Cl9I3N3Sb2
Ma, Yuxin; Hao, Munan; Sun, Ruijin; Jin, Shifeng; Zhao, Changchun; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 937–939; doi:10.1515/ncrs-2021-0156

data_8104629
_publ_section_title
;
 Crystal structure of tris(3-iodopyridin-1-ium)
 catena-poly[(hexachlorido-\k1 Cl)-(\m2-trichlorido-\k2
 Cl:Cl)diantimony(III)], C15H15Cl9I3N3Sb2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              937
_journal_page_last               939
_journal_paper_doi               10.1515/ncrs-2021-0156
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'Cl9 Sb2, 3(C5 H5 I N)'
_chemical_formula_sum            'C15 H15 Cl9 I3 N3 Sb2'
_chemical_formula_weight         1180.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.5840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2633(7)
_cell_length_b                   12.4964(3)
_cell_length_c                   9.1542(3)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.73
_cell_volume                     3188.04(15)
_computing_cell_refinement       'Bruker Smart [1]'
_computing_data_collection       'Bruker Smart [1]'
_computing_data_reduction        'Bruker Smart [1]'
_computing_molecular_graphics
'Olex2 1.5-alpha (Dolomanov et al., 2009) [4]'
_computing_publication_material
'Olex2 1.5-alpha (Dolomanov et al., 2009) [4]'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015) [3]'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008) [2]'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24356
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.681
_diffrn_reflns_theta_min         2.732
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.367
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   adsabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_density_meas      .
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+5.1353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3595
_reflns_number_total             4107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0156_suppl.cif
_cod_data_source_block           new
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8104629
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{C9, N2}
3. Restrained distances
 C10-H10
 0.93 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(N2)
5. Others
 Sof(I2)=1-FVAR(1)
 Sof(I1)=FVAR(1)
 Fixed Sof: H8B(0.5) H8A(0.5) C9(0.5) H9(0.5) I3(0.5) N2(0.5) H2(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C3(H3), C4(H4), C5(H5), C8(H8B), C8(H8A), C9(H9), N2(H2)
;