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_7716003
_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         '2(C46 H40 Co N8), 4(F6 P)'
_chemical_formula_sum            'C92 H80 Co2 F24 N16 P4'
_chemical_formula_weight         2107.46
_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             2024-04-28
_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                75.417(5)
_cell_angle_beta                 89.684(5)
_cell_angle_gamma                88.213(6)
_cell_formula_units_Z            2
_cell_length_a                   15.346(2)
_cell_length_b                   16.020(2)
_cell_length_c                   18.525(3)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.59
_cell_volume                     4405.4(11)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39765
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.897
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5779
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1227 before and 0.0871 after correction.
The Ratio of minimum to maximum transmission is 0.7753.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.656
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         16645
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1787
_refine_ls_R_factor_gt           0.1285
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+110.1766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2858
_refine_ls_wR_factor_ref         0.3185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11557
_reflns_number_total             16645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00433g2.cif
_cod_data_source_block           2_pf6_100k
_cod_depositor_comments
'Adding full bibliography for 7716001--7716004.cif.'
_cod_original_cell_volume        4405.6(11)
_cod_database_code               7716003
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.764(4)
 0.236(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(N17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C97) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C98) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C99) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C65) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C68) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C62(0.4) N15(0.6) C64(0.6) H64(0.6) C63(0.6) H63(0.6) C65(0.6)
 C67(0.6) H67(0.6) C66(0.6) H66(0.6) C69(0.6) H69A(0.6) H69B(0.6) H69C(0.6)
 C68(0.6) H68A(0.6) H68B(0.6) H68C(0.6) C93(0.4) H93(0.4) C94(0.6) N17(0.4)
 C95(0.4) C96(0.4) H96A(0.4) H96B(0.4) H96C(0.4) C97(0.4) H97A(0.4) H97B(0.4)
 H97C(0.4) C98(0.4) H98(0.4) C99(0.4) H99(0.4) C100(0.4) H100(0.4)
5.a Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C96(H96A,H96B,H96C), C97(H97A,H97B,
 H97C)
5.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C78(H78), C71(H71), C4(H4), C9(H9), C40(H40), C61(H61), C1(H1),
 C37(H37), C72(H72), C35(H35), C70(H70), C30(H30), C7(H7), C32(H32), C44(H44),
 C76(H76), C73(H73), C43(H43), C41(H41), C2(H2), C86(H86), C15(H15), C36(H36),
 C87(H87), C55(H55), C60(H60), C17(H17), C27(H27), C53(H53), C90(H90), C20(H20),
  C84(H84), C14(H14), C21(H21), C58(H58), C3(H3), C24(H24), C18(H18), C12(H12),
 C47(H47), C50(H50), C13(H13), C89(H89), C59(H59), C81(H81), C82(H82), C26(H26),
  C83(H83), C25(H25), C48(H48), C49(H49), C64(H64), C63(H63), C67(H67),
 C66(H66), C93(H93), C98(H98), C99(H99), C100(H100)
5.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C91(H91A,H91B,H91C), C23(H23A,H23B,H23C), C92(H92A,H92B,
 H92C), C46(H46A,H46B,H46C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              5715
_olex2_submission_special_instructions 'No special instructions were received'