Spin-crossover cobalt(II) complexes exhibiting temperature- and concentration-dependent optical changes in solution.
Izumiyama, Naoki; Fujii, Shun; Kato, Kiichi; Tokunaga, Ryuya; Hayami, Shinya; Nakaya, Manabu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9547–9553; doi:10.1039/d4dt00433g

data_7716004
_publ_section_title
;
 Spin-crossover cobalt(II) complexes exhibiting temperature- and
 concentration-dependent optical changes in solution.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9547
_journal_page_last               9553
_journal_paper_doi               10.1039/d4dt00433g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H40 Co N8, 2(C24 H20 B)'
_chemical_formula_sum            'C94 H80 B2 Co N8'
_chemical_formula_weight         1402.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.4872(17)
_cell_length_b                   11.4740(4)
_cell_length_c                   16.3188(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.41
_cell_volume                     7393.7(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            105492
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.253
_diffrn_reflns_theta_min         2.230
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1262 before and 0.0824 after correction.
The Ratio of minimum to maximum transmission is 0.8079.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.612
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 5355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         15934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0471P)^2^+0.4501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                14240
_reflns_number_total             15934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00433g2.cif
_cod_data_source_block           2_bph4
_cod_depositor_comments
'Adding full bibliography for 7716001--7716004.cif.'
_cod_database_code               7716004
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.844
_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:
 C48(H48), C49(H49), C35(H35), C59(H59), C3(H3), C69(H69), C38(H38), C57(H57),
 C36(H36), C13(H13), C9(H9), C60(H60), C29(H29), C22(H22), C54(H54), C7(H7),
 C42(H42), C19(H19), C33(H33), C88(H88), C4(H4), C62(H62), C65(H65), C93(H93),
 C16(H16), C66(H66), C68(H68), C1(H1), C53(H53), C63(H63), C24(H24), C86(H86),
 C50(H50), C30(H30), C80(H80), C32(H32), C12(H12), C14(H14), C89(H89), C56(H56),
  C39(H39), C2(H2), C51(H51), C55(H55), C85(H85), C79(H79), C15(H15), C28(H28),
 C71(H71), C27(H27), C41(H41), C61(H61), C83(H83), C92(H92), C67(H67), C91(H91),
  C84(H84), C94(H94), C90(H90), C78(H78), C17(H17), C81(H81), C18(H18),
 C72(H72), C77(H77), C73(H73), C75(H75), C74(H74)
2.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C45(H45A,H45B,
 H45C)
;
_shelx_res_checksum              8125
_olex2_submission_special_instructions 'No special instructions were received'