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_7717136
_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 F3 O3 S, 0.605(H2 O)'
_chemical_formula_sum            'C41 H25.19 Br2 F3 Fe N4 O5.6 S'
_chemical_formula_weight         968.17
_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                107.475(5)
_cell_angle_beta                 90.727(6)
_cell_angle_gamma                102.509(6)
_cell_formula_units_Z            2
_cell_length_a                   12.0862(18)
_cell_length_b                   12.2200(17)
_cell_length_c                   13.5092(19)
_cell_measurement_reflns_used    9383
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      54.19
_cell_measurement_theta_min      2.99
_cell_volume                     1851.5(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_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       -15
_diffrn_reflns_number            33272
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.595
_diffrn_reflns_theta_min         2.994
_exptl_absorpt_coefficient_mu    4.673
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4994
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1148 before and 0.0691 after correction.
The Ratio of minimum to maximum transmission is 0.6653.
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    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         6800
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0656P)^2^+1.8692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5756
_reflns_number_total             6800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01954g2.cif
_cod_data_source_block           OTfdesol@150K
_cod_depositor_comments
'Adding full bibliography for 7717133--7717140.cif.'
_cod_original_formula_sum        'C41 H25.19 Br2 F3 Fe N4 O5.60 S'
_cod_database_code               7717136
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.627
_shelx_estimated_absorpt_t_min   0.582
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 S1-O3 \\sim S1A-O3A
 with sigma of 0.02
 S1-O4 \\sim S1A-O4A
 with sigma of 0.02
 S1-O5 \\sim S1A-O5A
 with sigma of 0.02
 F1-C41 \\sim F1A-C41A
 with sigma of 0.02
 F2-C41 \\sim F2A-C41A
 with sigma of 0.02
 F3-C41 \\sim F3A-C41A
 with sigma of 0.02
 S1-F1 \\sim S1A-F1A
 with sigma of 0.04
 S1-F2 \\sim S1A-F2A
 with sigma of 0.04
 S1-F3 \\sim S1A-F3A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F2-F3 \\sim F2A-F3A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-O5 \\sim O3A-O5A
 with sigma of 0.04
 O3-C41 \\sim O3A-C41A
 with sigma of 0.04
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 O4-C41 \\sim O4A-C41A
 with sigma of 0.04
 O5-C41 \\sim O5A-C41A
 with sigma of 0.04
 S1-C41 \\sim S1A-C41A
 with sigma of 0.01
 S1-O4 \\sim S1-O3 \\sim S1-O5 \\sim S1A-O4A \\sim S1A-O5A \\sim S1A-O3A
 with sigma of 0.01
 F2-C41 \\sim F3-C41 \\sim F1-C41 \\sim F1A-C41A \\sim F2A-C41A \\sim F3A-C41A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim S1 \\sim O3 \\sim O4 \\sim O5 \\sim C41 \\sim F2 \\sim F3 \\sim C41A
\\sim F1A \\sim F2A \\sim S1A \\sim F3A \\sim O4A \\sim O5A \\sim O3A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(O4A)=Sof(S1A)=Sof(C41A)=Sof(O5A)=Sof(O3A)=Sof(F2A)=Sof(F3A)=Sof(F1A)=1-
 FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(C41)=FVAR(1)
 Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(2)
5.a Riding coordinates:
 O6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), 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)
;
_shelx_res_checksum              55958
_shelx_hkl_checksum              2203
_olex2_submission_special_instructions 'No special instructions were received'