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_7132897
_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 H56 Cl N2 O3 Sb, C3 H6 O'
_chemical_formula_sum            'C49 H62 Cl N2 O4 Sb'
_chemical_formula_weight         900.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-27
_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                 100.297(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3993(6)
_cell_length_b                   16.8320(4)
_cell_length_c                   11.6630(3)
_cell_measurement_reflns_used    45334
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.3380
_cell_measurement_theta_min      2.0110
_cell_volume                     4712.7(2)
_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_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   -105.00  75.00   0.50   10.00    --  -15.00  45.00   0.00  360
  2  \w   -105.00  75.00   0.50   10.00    --  -15.00  45.00 270.00  360
  3  \w   -105.00  75.00   0.50   10.00    --  -15.00  45.00  90.00  360
  4  \w   -105.00  75.00   0.50   10.00    --  -15.00  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_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            76821
_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         1.697
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79595
_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    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9643
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0377P)^2^+2.6904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8679
_reflns_number_total             9643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00630e2.cif
_cod_data_source_block           v231004a_autored
_cod_depositor_comments
'Adding full bibliography for 7132896--7132898.cif.'
_cod_database_code               7132897
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 C42-C43 \\sim C42-C46
 with sigma of 0.02
 C42-C44 \\sim C42-C47
 with sigma of 0.02
 C42-C45 \\sim C42-C48
 with sigma of 0.02
 Sb1-Cl3 \\sim Sb1-Cl2
 with sigma of 0.001
 Sb1-O2 \\sim Sb1-O3
 with sigma of 0.001
 O57-C58 \\sim O57A-C58A
 with sigma of 0.02
 C58-C60 \\sim C58A-C60A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.02
 O57-C60 \\sim O57A-C60A
 with sigma of 0.04
 O57-C59 \\sim O57A-C59A
 with sigma of 0.04
 C60-C59 \\sim C60A-C59A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C46 \\sim C43 \\sim C48 \\sim C44 \\sim C47 \\sim C45: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
O57A \\sim C58A \\sim C60A \\sim C59A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Cl2 \\sim O2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(Cl2) = Uanis(Cl3)
Uanis(O2) = Uanis(O3)
4. Rigid body (RIGU) restrains
 C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C43, C42, C44, C47, C45, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 O57, C58, C60, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O57A, C58A, C60A, C59A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
 Sof(O57A)=Sof(C58A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C59A)=
 Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(2)
 Sof(O57)=Sof(C58)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C59)=Sof(H59A)=
 Sof(H59B)=Sof(H59C)=FVAR(2)
 Sof(O2)=Sof(H2)=Sof(Cl3)=1-FVAR(3)
 Sof(Cl2)=Sof(O3)=Sof(H3)=FVAR(3)
6.a Free rotating group:
 O3(H3)
6.b Me refined with riding coordinates:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C60(H60A,H60B,H60C), C59(H59A,H59B,
 H59C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C48(H48A,
 H48B,H48C), C60A(H60D,H60E,H60F), C59A(H59D,H59E,H59F)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C13(H13), C12(H12), C25(H25), C19(H19), C7(H7), C27(H27), C31(H31),
 C9(H9), C33(H33)
6.d Tetrahedral OH refined with riding coordinates:
 O2(H2)
6.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C41(H41A,H41B,H41C), C54(H54A,H54B,H54C), C51(H51A,
 H51B,H51C), C37(H37A,H37B,H37C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              20597
_shelx_hkl_checksum              70052
_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
;