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_7716002
_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 H47 Co N8, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C70 H53 Co F12 N10 P2'
_chemical_formula_weight         1383.09
_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
_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                 91.231(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5636(4)
_cell_length_b                   16.2032(6)
_cell_length_c                   35.9590(17)
_cell_measurement_reflns_used    9779
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.26
_cell_volume                     6153.5(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            80874
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.114
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1079 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.8536.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0010(2)
_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   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         10837
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0802P)^2^+11.8141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8161
_reflns_number_total             10837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00433g2.cif
_cod_data_source_block           1_pf6_100k
_cod_depositor_comments
'Adding full bibliography for 7716001--7716004.cif.'
_cod_database_code               7716002
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.873
_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. Rigid bond restraints
 Co1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
P2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(P2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C22(H22), C16(H16), C46(H46), C27(H27), C53(H53), C54(H54), C7(H7),
 C44(H44), C9(H9), C43(H43), C17(H17), C30(H30), C18(H18), C12(H12), C28(H28),
 C19(H19), C15(H15), C47(H47), C2(H2), C24(H24), C51(H51), C3(H3), C1(H1),
 C13(H13), C35(H35), C66(H66), C41(H41), C29(H29), C14(H14), C56(H56), C37(H37),
  C39(H39), C62(H62), C40(H40), C57(H57), C38(H38), C63(H63), C33(H33),
 C34(H34), C64(H64), C65(H65), C60(H60), C31(H31), C32(H32), C58(H58), C59(H59)
4.b Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              22254
_olex2_submission_special_instructions 'No special instructions were received'