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_7132898
_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 H57 N2 O4 Sb'
_chemical_formula_sum            'C46 H57 N2 O4 Sb'
_chemical_formula_weight         823.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   28.4574(5)
_cell_length_b                   27.9101(4)
_cell_length_c                   32.3437(6)
_cell_measurement_reflns_used    64851
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.4320
_cell_measurement_theta_min      1.6230
_cell_volume                     25688.9(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -120.00  60.00   0.50   30.00    --  -30.00  45.00 270.00  360
  2  \w   -120.00  60.00   0.50   30.00    --  -30.00  45.00  90.00  360
  3  \w   -120.00  60.00   0.50   30.00    --  -30.00  45.00   0.00  360
  4  \w   -120.00  60.00   0.50   30.00    --  -30.00  45.00 180.00  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      0.0019049000
_diffrn_orient_matrix_UB_12      0.0059292000
_diffrn_orient_matrix_UB_13      -0.0212583000
_diffrn_orient_matrix_UB_21      -0.0125673000
_diffrn_orient_matrix_UB_22      0.0215497000
_diffrn_orient_matrix_UB_23      0.0035996000
_diffrn_orient_matrix_UB_31      0.0214345000
_diffrn_orient_matrix_UB_32      0.0121080000
_diffrn_orient_matrix_UB_33      0.0039991000
_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  0.1196
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            281142
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.589
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70396
_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    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             10320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1493
_refine_ls_number_reflns         26265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+14.6108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18165
_reflns_number_total             26265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00630e2.cif
_cod_data_source_block           v231215a_autored
_cod_depositor_comments
'Adding full bibliography for 7132896--7132898.cif.'
_cod_database_code               7132898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1.a Free rotating group:
 O55(H55), O107(H107), O3(H3), O2(H2), O108(H108)
1.b Aromatic/amide H refined with riding coordinates:
 C59(H59), C142(H142), C88(H88), C143(H143), C160(H160), C21(H21), C9(H9),
 C150(H150), C61(H61), C89(H89), C7(H7), C42(H42), C22(H22), C114(H114),
 C37(H37), C74(H74), C36(H36), C112(H112), C96(H96), C128(H128), C94(H94),
 C148(H148), C79(H79), C73(H73), C133(H133), C27(H27), C127(H127), C29(H29),
 C135(H135), C81(H81)
1.c Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C105(H10D,H10E,H10F), C139(H13D,H13E,H13F), C64(H64A,
 H64B,H64C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C65(H65A,H65B,H65C),
 C119(H11A,H11B,H11C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C46(H46A,H46B,
 H46C), C66(H66A,H66B,H66C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C12(H12A,
 H12B,H12C), C50(H50A,H50B,H50C), C84(H84A,H84B,H84C), C120(H12D,H12E,H12F),
 C99(H99A,H99B,H99C), C13(H13A,H13B,H13C), C70(H70A,H70B,H70C), C52(H52A,H52B,
 H52C), C118(H11D,H11E,H11F), C100(H10G,H10H,H10I), C104(H10J,H10K,H10L),
 C137(H13G,H13H,H13I), C51(H51A,H51B,H51C), C18(H18A,H18B,H18C), C153(H15A,H15B,
 H15C), C83(H83A,H83B,H83C), C32(H32A,H32B,H32C), C124(H12G,H12H,H12I),
 C159(H15D,H15E,H15F), C138(H13J,H13K,H13L), C17(H17A,H17B,H17C), C68(H68A,H68B,
 H68C), C123(H12J,H12K,H12L), C157(H15G,H15H,H15I), C155(H15J,H15K,H15L),
 C103(H10M,H10N,H10O), C122(H12M,H12N,H12O), C69(H69A,H69B,H69C), C158(H15M,
 H15N,H15O), C154(H15P,H15Q,H15R), C85(H85A,H85B,H85C)
1.d Idealised tetrahedral OH refined as rotating group:
 O54(H54)
;
_shelx_res_checksum              66515
_shelx_hkl_checksum              10142
_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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.642