Crystal structure of bis(μ2-azido-κ2 N:N)-tetrakis(azido-κ1 N)-tetrakis(1,10-phenanthroline-κ2 N,N′)dibismuth(III), C48H32N26Bi2
Zhong, Zhi-Guo; Li, Jing; Feng, Yu-Quan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 983–985; doi:10.1515/ncrs-2023-0312

data_8107618
_publ_section_title
;
 Crystal structure of bis(\m2-azido-\k2 N:N)-tetrakis(azido-\k1
 N)-tetrakis(1,10-phenanthroline-\k2 N,N&#x2032;)dibismuth(III),
 C48H32N26Bi2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              983
_journal_page_last               985
_journal_paper_doi               10.1515/ncrs-2023-0312
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C48 H32 Bi2 N26'
_chemical_formula_sum            'C48 H32 Bi2 N26'
_chemical_formula_weight         1390.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_cell_angle_alpha                83.816(10)
_cell_angle_beta                 74.471(10)
_cell_angle_gamma                66.120(8)
_cell_formula_units_Z            1
_cell_length_a                   9.781(5)
_cell_length_b                   11.667(6)
_cell_length_c                   11.973(7)
_cell_measurement_reflns_used    2079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.60
_cell_volume                     1203.7(11)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9939
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7846
_diffrn_reflns_theta_full        25.0998
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    7.366
_exptl_absorpt_correction_T_max  0.3506
_exptl_absorpt_correction_T_min  0.2503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.9186
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660.4433
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.5409
_refine_diff_density_min         -1.3415
_refine_diff_density_rms         0.2177
_refine_ls_d_res_high            0.8377
_refine_ls_d_res_low             10.6682
_refine_ls_goodness_of_fit_ref   1.0194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.0112
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3351
_reflns_number_total             4254
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2023-0312_suppl_001.cif
_cod_data_source_block           A
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_database_code               8107618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N8, N9, N9, N10, C19, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N7) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C12(H12), C24(H24), C8(H8), C1(H1), C9(H9), C2(H2),
 C21(H21), C3(H3), C20(H20), C13(H13), C22(H22), C23(H23), C15(H15), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'