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_7717134
_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, C H4 O, N O3'
_chemical_formula_sum            'C41 H28 Br2 Fe N5 O6'
_chemical_formula_weight         902.35
_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             2024-07-03
_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                110.74(3)
_cell_angle_beta                 95.023(17)
_cell_angle_gamma                103.366(19)
_cell_formula_units_Z            2
_cell_length_a                   11.649(7)
_cell_length_b                   12.268(8)
_cell_length_c                   13.964(8)
_cell_measurement_reflns_used    1474
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      2.99
_cell_volume                     1784.0(19)
_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      300.00
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.956
_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     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.956
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6298
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.192
_diffrn_reflns_theta_min         2.996
_exptl_absorpt_coefficient_mu    4.394
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.2009
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1361 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.6670.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.851
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6298
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0843
_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^)+(0.0700P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             6298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01954g2.cif
_cod_data_source_block           NO3@300K
_cod_depositor_comments
'Adding full bibliography for 7717133--7717140.cif.'
_cod_original_cell_volume        1784.0(18)
_cod_database_code               7717134
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.599
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.716(6)
 0.284(6)
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
 N5-O3 \\sim N5A-O3A
 with sigma of 0.02
 O3-N5 \\sim O3A-N5A
 with sigma of 0.01
 O3-O5 \\sim O3A-O5A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 N5-O5 \\sim N5A-O5A
 with sigma of 0.01
 N5-O4 \\sim N5A-O4A
 with sigma of 0.01
 O5-O4 \\sim O5A-O4A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O3 \\sim N5 \\sim O5 \\sim O4 \\sim N5A \\sim O3A \\sim O5A \\sim O4A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(N5A)=Sof(O3A)=Sof(O5A)=Sof(O4A)=1-FVAR(1)
 Sof(N5)=Sof(O3)=Sof(O5)=Sof(O4)=FVAR(1)
 Fixed X: N5A(0.18482)
6.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C17(H17), C13(H13), C14(H14), C7(H7), C2(H2), C3(H3),
 C8(H8), C9(H9), C10(H10), C11(H11), C40(H40), C39(H39), C38(H38), C33(H33),
 C34(H34), C31(H31), C27(H27), C28(H28), C29(H29), C30(H30), C23(H23), C22(H22)
6.b Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
6.c Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              20040
_shelx_hkl_checksum              85444
_olex2_submission_special_instructions 'No special instructions were received'