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_7717137
_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, Cl O4, C H4 O'
_chemical_formula_sum            'C41 H28 Br2 Cl Fe N4 O7'
_chemical_formula_weight         939.79
_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   mixed
_audit_creation_date             2024-07-03
_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                106.646(8)
_cell_angle_beta                 93.560(8)
_cell_angle_gamma                101.853(8)
_cell_formula_units_Z            2
_cell_length_a                   11.811(2)
_cell_length_b                   12.312(2)
_cell_length_c                   13.297(2)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    90.00
_cell_measurement_theta_max      53.80
_cell_measurement_theta_min      3.35
_cell_volume                     1797.9(5)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.00
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6100
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        52.975
_diffrn_reflns_theta_max         52.975
_diffrn_reflns_theta_min         3.352
_exptl_absorpt_coefficient_mu    4.833
_exptl_absorpt_correction_T_max  0.0508
_exptl_absorpt_correction_T_min  0.0041
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1449 before and 0.0929 after correction.
The Ratio of minimum to maximum transmission is 0.0807.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.782
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         6100
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.1050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2356
_refine_ls_wR_factor_ref         0.2632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2604
_reflns_number_total             6100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01954g2.cif
_cod_data_source_block           ClO4@90K
_cod_depositor_comments
'Adding full bibliography for 7717133--7717140.cif.'
_cod_database_code               7717137
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.572
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.607(4)
 0.393(4)
2. 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
3. Restrained distances
 O7-C41
 1.43 with sigma of 0.01
 C41-O7 \\sim C41A-O7A
 with sigma of 0.01
4. Restrained planarity
 N1, C1, C2, C3, C4, C5
 with sigma of 0.001
 C1, C2, C3, C4, C5, N1, C6, C7, C8, C9
 with sigma of 0.001
5. Rigid bond restraints
 C3, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Uiso/Uaniso restraints and constraints
O7A \\sim C41A \\sim C41 \\sim O7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C3) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O7A) \\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
7. Others
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(O7A)=Sof(H7AA)=1-FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
8.a Riding coordinates:
 O7A(H7AA)
8.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39)
8.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C41A(H41D,H41E,H41F)
8.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_shelx_res_checksum              13251
_shelx_hkl_checksum              84779
_olex2_submission_special_instructions 'No special instructions were received'