Spin crossover Fe<sup>III</sup> complexes with a substituted Hqnal ligand: effects of anions and solvents.
Chen, Feng-Li; Liu, Xin-Li; Zhao, Yue; Li, Gang; Gao, Bo-Hong; Wang, Xin-Yi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17233–17243; doi:10.1039/d4dt01954g

data_7717135
_publ_section_title
;
 Spin crossover Fe<sup>III</sup> complexes with a substituted Hqnal
 ligand: effects of anions and solvents.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17233
_journal_page_last               17243
_journal_paper_doi               10.1039/d4dt01954g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H24 Br2 Fe N4 O2, C2 F6 N O4 S2, C H2 Cl2'
_chemical_formula_sum            'C43 H26 Br2 Cl2 F6 Fe N5 O6 S2'
_chemical_formula_weight         1173.38
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                104.455(3)
_cell_angle_beta                 99.916(4)
_cell_angle_gamma                111.885(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2508(12)
_cell_length_b                   13.8357(13)
_cell_length_c                   14.0684(14)
_cell_measurement_reflns_used    6894
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      51.11
_cell_measurement_theta_min      2.95
_cell_volume                     2214.3(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.00
_diffrn_measured_fraction_theta_full 0.998
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.014
_diffrn_reflns_theta_min         2.954
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.070
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.7603.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       block
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0685P)^2^+2.2794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5052
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01954g2.cif
_cod_data_source_block           NTf@300K
_cod_depositor_comments
'Adding full bibliography for 7717133--7717140.cif.'
_cod_database_code               7717135
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.605
_shelx_estimated_absorpt_t_min   0.559
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C27(H27), C13(H13), C3(H3), C2(H2), C10(H10), C33(H33), C34(H34),
 C14(H14), C18(H18), C19(H19), C20(H20), C28(H28), C22(H22), C40(H40), C38(H38),
  C23(H23), C8(H8), C7(H7), C39(H39), C31(H31), C9(H9), C30(H30), C29(H29)
;
_shelx_res_checksum              83123
_shelx_hkl_checksum              68208
_olex2_submission_special_instructions 'No special instructions were received'