Synthesis and optical properties of antimony(V) complexes of a trianionic N<sub>2</sub>O<sub>2</sub>-type tetradentate dipyrrin ligand.
Agou, Tomohiro; Kuroiwa, Shunsuke; Fukumoto, Hiroki; Nabeshima, Tatsuya; Chemical communications (Cambridge, England) 60 (2024) 4557–4560; doi:10.1039/d4cc00630e

data_7132896
_publ_section_title
;
 Synthesis and optical properties of antimony(V) complexes of a trianionic
 N<sub>2</sub>O<sub>2</sub>-type tetradentate dipyrrin ligand.
;
_journal_issue                   34
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4557
_journal_page_last               4560
_journal_paper_doi               10.1039/d4cc00630e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C46 H55 Cl2 N2 O2 Sb'
_chemical_formula_sum            'C46 H55 Cl2 N2 O2 Sb'
_chemical_formula_weight         860.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.815(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0826(9)
_cell_length_b                   14.1346(5)
_cell_length_c                   15.2463(7)
_cell_measurement_reflns_used    15535
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.4200
_cell_measurement_theta_min      3.0840
_cell_volume                     4250.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -105.00  75.00   0.50   20.00    --  -15.00  45.00   0.00  360
  2  \w   -105.00  69.00   0.50   20.00    --  -15.00  45.00 270.00  348
  3  \w   -105.00  60.00   0.50   20.00    --  -15.00  45.00  45.00  330
  4  \w   -105.00  51.00   0.50   20.00    --  -15.00  45.00 180.00  312
;
_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      0.0092870000
_diffrn_orient_matrix_UB_12      0.0465750000
_diffrn_orient_matrix_UB_13      -0.0102270000
_diffrn_orient_matrix_UB_21      -0.0343501000
_diffrn_orient_matrix_UB_22      0.0143118000
_diffrn_orient_matrix_UB_23      -0.0053010000
_diffrn_orient_matrix_UB_31      0.0050739000
_diffrn_orient_matrix_UB_32      0.0119810000
_diffrn_orient_matrix_UB_33      0.0459680000
_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  0.1105
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30936
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.720
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 2834 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8642
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                7311
_reflns_number_total             8642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00630e2.cif
_cod_data_source_block           v230921a_autored
_cod_depositor_comments
'Adding full bibliography for 7132896--7132898.cif.'
_cod_database_code               7132896
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C39(H39), C37(H37), C18(H18), C23(H23), C25(H25), C33(H33),
 C1(H1), C32(H32)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C29(H29A,H29B,
 H29C), C28(H28A,H28B,H28C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C44(H44A,
 H44B,H44C), C43(H43A,H43B,H43C), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C), C8(H8A,
 H8B,H8C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              94837
_shelx_hkl_checksum              59778
_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 2.632
_oxdiff_exptl_absorpt_empirical_full_min 0.648