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_7716001
_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
'C66 H48 Co N8, 2(C24 H20 B), 2.75(C2 H3 N), 0.8(C H4 O), 0.25(O)'
_chemical_formula_sum            'C120.3 H99.45 B2 Co N10.75 O1.05'
_chemical_formula_weight         1793.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                98.6460(10)
_cell_angle_beta                 112.5360(10)
_cell_angle_gamma                105.9460(10)
_cell_formula_units_Z            2
_cell_length_a                   15.9874(6)
_cell_length_b                   18.4762(8)
_cell_length_c                   19.2522(8)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.31
_cell_volume                     4836.7(3)
_computing_cell_refinement       'Bruker APEX4'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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      100.00
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35099
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.920
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.8756.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0061(6)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1268
_refine_ls_number_reflns         16748
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0448P)^2^+4.8413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14797
_reflns_number_total             16748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00433g2.cif
_cod_data_source_block           1_bph4_100k
_cod_depositor_comments
'Adding full bibliography for 7716001--7716004.cif.'
_cod_original_formula_sum        'C120.30 H99.45 B2 Co N10.75 O1.05'
_cod_database_code               7716001
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.883
_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
 O1-C123
 1.4 with sigma of 0.002
3. Rigid bond restraints
 Co1, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Co1, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(N11) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N12) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C123) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: N11(0.5) O1(0.8) H1A(0.8) C119(0.5) C120(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5) C123(0.8) H12D(0.8) H12E(0.8) H12F(0.8) O2(0.25) C122(0.25)
 H12G(0.25) H12H(0.25) H12I(0.25) C121(0.25) N12(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C80(H80), C7(H7), C108(H108), C90(H90), C27(H27), C54(H54),
 C2(H2), C69(H69), C50(H50), C107(H107), C68(H68), C81(H81), C72(H72), C19(H19),
  C9(H9), C22(H22), C24(H24), C104(H104), C53(H53), C56(H56), C15(H15), C1(H1),
 C98(H98), C51(H51), C89(H89), C86(H86), C102(H102), C66(H66), C63(H63),
 C62(H62), C12(H12), C70(H70), C38(H38), C84(H84), C92(H92), C40(H40), C32(H32),
  C99(H99), C18(H18), C71(H71), C57(H57), C42(H42), C96(H96), C14(H14),
 C39(H39), C95(H95), C28(H28), C106(H106), C82(H82), C48(H48), C87(H87),
 C93(H93), C65(H65), C88(H88), C30(H30), C44(H44), C105(H105), C16(H16),
 C110(H110), C17(H17), C74(H74), C33(H33), C78(H78), C36(H36), C64(H64),
 C94(H94), C58(H58), C59(H59), C75(H75), C13(H13), C60(H60), C83(H83),
 C101(H101), C29(H29), C114(H114), C35(H35), C77(H77), C113(H113), C100(H100),
 C76(H76), C47(H47), C111(H111), C41(H41), C112(H112), C45(H45), C46(H46)
6.b Idealised Me refined as rotating group:
 C118(H11D,H11E,H11F), C116(H11A,H11B,H11C), C120(H12A,H12B,H12C), C123(H12D,
 H12E,H12F), C122(H12G,H12H,H12I)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              13597
_olex2_submission_special_instructions 'No special instructions were received'