Antimony <i>vs.</i> bismuth: structural differences in Cat{[MCl<sub>5</sub>](I<sub>2</sub>)} halogen bond-linked supramolecular complexes.
Korobeynikov, Nikita A.; Usoltsev, Andrey N.; Sokolov, Maxim N.; Novikov, Alexander S.; Adonin, Sergey A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10294–10303; doi:10.1039/d5dt00697j

data_7718800
_publ_section_title
;
 Antimony <i>vs.</i> bismuth: structural differences in
 Cat{[MCl<sub>5</sub>](I<sub>2</sub>)} halogen bond-linked supramolecular
 complexes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10294
_journal_page_last               10303
_journal_paper_doi               10.1039/d5dt00697j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Bi Cl5, I2, C12 H14 N2'
_chemical_formula_sum            'C12 H14 Bi Cl5 I2 N2'
_chemical_formula_weight         826.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-22 deposited with the CCDC.	2025-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4735(2)
_cell_length_b                   14.2835(4)
_cell_length_c                   19.7322(6)
_cell_measurement_reflns_used    8671
_cell_measurement_temperature    220.00
_cell_measurement_theta_max      31.47
_cell_measurement_theta_min      2.85
_cell_volume                     2106.37(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      220.00
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27777
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.508
_diffrn_reflns_theta_min         2.064
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.933
_exptl_absorpt_correction_T_max  0.3728
_exptl_absorpt_correction_T_min  0.1658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1396 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.4447.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00195(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.6520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3007
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00697j2.cif
_cod_data_source_block           2_nk1198
_cod_depositor_comments
'Adding full bibliography for 7718795--7718800.cif.'
_cod_database_code               7718800
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.154
_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. Restrained distances
 Bi1-Cl1A \\sim Bi1-Cl1B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C6, C3, C4, C2, C5, C1, C7, N1, C8, C9, C12, C10, C11, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1B)=0.5*(1-FVAR(2))
 Sof(Cl1A)=0.5*FVAR(2)
 Fixed Sof: C3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) N1(0.5) H1(0.5) C1(0.5)
 H1A(0.5) C2(0.5) H2(0.5) C8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) N2(0.5)
 H2A(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5)
 H7A(0.5) H7B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), N1(H1), C1(H1A), C2(H2), C9(H9), C10(H10), N2(H2A), C11(H11),
 C12(H12)
5.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,N2,C11,C12)
;
_shelx_res_checksum              41757
_shelx_hkl_checksum              73582
_olex2_submission_special_instructions 'No special instructions were received'