Boron complexes of π-extended nitroxide ligands exhibiting three-state redox processes and near-infrared-II (NIR-II) absorption properties.
Nakamura, Marika; Hyakutake, Risa; Morisako, Shogo; Sasamori, Takahiro; Mizuhata, Yoshiyuki; Tokitoh, Norihiro; Nakashima, Kouichi; Fukumoto, Hiroki; Agou, Tomohiro; Dalton transactions (Cambridge, England : 2003) 51 (2022) 13675–13680; doi:10.1039/d2dt02545k

data_7711305
_publ_section_title
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 Boron complexes of \p-extended nitroxide ligands exhibiting three-state
 redox processes and near-infrared-II (NIR-II) absorption properties.
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_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13675
_journal_page_last               13680
_journal_paper_doi               10.1039/d2dt02545k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'Cl6 Sb, C41 H38 B F10 N3 O, C H2 Cl2'
_chemical_formula_sum            'C42 H40 B Cl8 F10 N3 O Sb'
_chemical_formula_weight         1208.93
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.431(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0513(7)
_cell_length_b                   11.8757(3)
_cell_length_c                   23.2991(7)
_cell_measurement_reflns_used    17014
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      29.415
_cell_measurement_theta_min      2.96
_cell_volume                     5526.0(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 CCD
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44316
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.850
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.91904
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+8.5845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9694
_reflns_number_total             12659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02545k2.cif
_cod_data_source_block           20220202_5_auto_2
_cod_database_code               7711305
_shelx_shelxl_version_number     2014/7
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.725
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C15(H15),
 C19(H19), C21(H21), C23(H23)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C41(H41A,H41B,H41C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 198 electrons were 
found in a volume of 860\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15425
_shelx_hkl_checksum              65969
_shelx_fab_checksum              25912
_olex2_submission_special_instructions 'No special instructions were received'