Synthesis and structural characterization of Sb(iii) and Bi(iii) complexes with an N2O2-type tetradentate dipyrrin ligand
Agou, Tomohiro; Kuroiwa, Shunsuke; Moriyama, Ryo; Kuroda, Takuma; Kubo, Kazuya; Fukumoto, Hiroki; Morita, Masato; Inoue, Ryo; Nabeshima, Tatsuya; Chemical Communications 61 (2025) 7141–7144; doi:10.1039/D5CC01037C

data_7134798
_publ_section_title
;
 Synthesis and structural characterization of Sb(iii) and Bi(iii)
 complexes with an N2O2-type tetradentate dipyrrin ligand
;
_journal_issue                   39
_journal_name_full               'Chemical Communications'
_journal_page_first              7141
_journal_page_last               7144
_journal_paper_doi               10.1039/D5CC01037C
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C46 H55 Bi N2 O2, C H2 Cl2'
_chemical_formula_sum            'C47 H57 Bi Cl2 N2 O2'
_chemical_formula_weight         961.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2025-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-08 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                62.515(7)
_cell_angle_beta                 80.924(6)
_cell_angle_gamma                62.258(7)
_cell_formula_units_Z            2
_cell_length_a                   13.8968(10)
_cell_length_b                   14.1548(10)
_cell_length_c                   14.2678(10)
_cell_measurement_reflns_used    8198
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.8070
_cell_measurement_theta_min      2.2200
_cell_volume                     2197.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -100.00  80.00   0.50   16.00    --  -10.00  45.00   0.00  360
  2  \w   -100.00  80.00   0.50   16.00    --  -10.00  45.00  90.00  360
  3  \w   -100.00 -39.50   0.50   16.00    --  -10.00  45.00 180.00  121
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469255000
_diffrn_orient_matrix_UB_12      -0.0352837000
_diffrn_orient_matrix_UB_13      -0.0180103000
_diffrn_orient_matrix_UB_21      -0.0306163000
_diffrn_orient_matrix_UB_22      0.0216847000
_diffrn_orient_matrix_UB_23      -0.0469844000
_diffrn_orient_matrix_UB_31      0.0142851000
_diffrn_orient_matrix_UB_32      0.0477263000
_diffrn_orient_matrix_UB_33      -0.0250014000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8844
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         1.660
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_preparation       CH2Cl2/hexane
_exptl_crystal_recrystallization_method CH2Cl2/hexane
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.314
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8844
_refine_ls_number_restraints     472
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+90.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6195
_reflns_number_total             8844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01037c2.cif
_cod_data_source_block           20240905-kuro2
_cod_database_code               7134798
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C47H57BiCl2N2O2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.987(2)
 0.013(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C47) = Uanis(C48)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C48(0.75) H48A(0.75) H48B(0.75) C47(0.25) H47A(0.25) H47B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C40(H40), C3(H3), C6(H6), C42(H42), C8(H8), C21(H21), C22(H22),
 C27(H27), C25(H25)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C45(H45A,H45B,H45C), C13(H13A,H13B,H13C), C35(H35A,H35B,
 H35C), C44(H44A,H44B,H44C), C36(H36A,H36B,H36C), C16(H16A,H16B,H16C), C31(H31A,
 H31B,H31C), C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C),
 C46(H46A,H46B,H46C), C37(H37A,H37B,H37C), C14(H14A,H14B,H14C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              92501
_shelx_hkl_checksum              71372
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.602
_oxdiff_exptl_absorpt_empirical_full_min 0.659