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_7134797
_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 N2 O2 Sb'
_chemical_formula_sum            'C46 H55 N2 O2 Sb'
_chemical_formula_weight         789.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4576(6)
_cell_length_b                   16.2320(6)
_cell_length_c                   27.3781(10)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      2.2050
_cell_volume                     8202.6(5)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      213
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.836
_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    2.00    --  -10.00  45.00   0.00  360
;
_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      0.0109162000
_diffrn_orient_matrix_UB_12      0.0142705000
_diffrn_orient_matrix_UB_13      0.0233375000
_diffrn_orient_matrix_UB_21      -0.0047548000
_diffrn_orient_matrix_UB_22      -0.0402030000
_diffrn_orient_matrix_UB_23      0.0096547000
_diffrn_orient_matrix_UB_31      0.0365470000
_diffrn_orient_matrix_UB_32      -0.0094830000
_diffrn_orient_matrix_UB_33      -0.0057357000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34983
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.387
_diffrn_reflns_theta_min         1.488
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48818
_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 green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             3296
_exptl_crystal_preparation       acetone
_exptl_crystal_recrystallization_method acetone
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8597
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0352P)^2^+7.8212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5603
_reflns_number_total             8597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01037c2.cif
_cod_data_source_block           20241005-kurol1sb
_cod_database_code               7134797
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.932
_diffrn_oxdiff_ac3_digest_hkl    413ada541224193579487607fecf4f89891f88
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1-O2 \\sim Sb2-O2
 with sigma of 0.02
 Sb1-O1 \\sim Sb2-O1
 with sigma of 0.02
 Sb1-N2 \\sim Sb2-N2
 with sigma of 0.02
 Sb1-N1 \\sim Sb2-N1
 with sigma of 0.02
3. Others
 Sof(Sb2)=1-FVAR(1)
 Sof(Sb1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C21(H21), C22(H22), C8(H8), C27(H27), C6(H6), C2(H2), C40(H40),
 C42(H42), C3(H3)
4.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C17(H17A,H17B,H17C), C45(H45A,H45B,H45C), C35(H35A,H35B,
 H35C), C44(H44A,H44B,H44C), C37(H37A,H37B,H37C), C16(H16A,H16B,H16C), C14(H14A,
 H14B,H14C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C46(H46A,H46B,H46C),
 C18(H18A,H18B,H18C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              48656
_shelx_hkl_checksum              56914
_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 1.760
_oxdiff_exptl_absorpt_empirical_full_min 0.549