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_7711307
_publ_section_title
;
 Boron complexes of \p-extended nitroxide ligands exhibiting three-state
 redox processes and near-infrared-II (NIR-II) absorption properties.
;
_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         'C35 H26 B F10 N3 O3, Cl6 Sb'
_chemical_formula_sum            'C35 H26 B Cl6 F10 N3 O3 Sb'
_chemical_formula_weight         1071.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-08-24 deposited with the CCDC.	2022-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.647(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0480(11)
_cell_length_b                   10.6917(7)
_cell_length_c                   21.8391(12)
_cell_measurement_reflns_used    6284
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      3.246
_cell_volume                     4111.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a'
_computing_data_collection       'CrysAlisPro 1.171.41.117a'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Pilatus P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34211
_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         27.481
_diffrn_reflns_theta_min         2.767
_diffrn_source                   'Rigaku VariMax DW'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.51931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0284P)^2^+3.8790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6193
_reflns_number_total             9429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02545k2.cif
_cod_data_source_block           20220302_1_auto
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711307
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              41148
_shelx_hkl_checksum              22046