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_7717139
_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, H2 O, 2(C H4 O)'
_chemical_formula_sum            'C43 H34 Br2 F3 Fe N4 O8 S'
_chemical_formula_weight         1039.47
_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                71.329(5)
_cell_angle_beta                 73.875(5)
_cell_angle_gamma                83.853(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0896(18)
_cell_length_b                   13.4142(19)
_cell_length_c                   13.4157(18)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      54.21
_cell_measurement_theta_min      3.03
_cell_volume                     1979.7(5)
_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      100.00
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22950
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.257
_diffrn_reflns_theta_min         3.026
_exptl_absorpt_coefficient_mu    4.441
_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    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         7137
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1058P)^2^+0.9848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5038
_reflns_number_total             7137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01954g2.cif
_cod_data_source_block           otf@100k
_cod_depositor_comments
'Adding full bibliography for 7717133--7717140.cif.'
_cod_database_code               7717139
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.596
_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, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 O8-C42 = O8A-C42A
 1.43 with sigma of 0.01
 O7A-C41
 1.43 with sigma of 0.01
 O8A-C42A \\sim O8-C42
 with sigma of 0.01
 O7A-C41 \\sim O7-C41
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O8 \\sim O8A \\sim C42 \\sim C42A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O6 \\sim O6A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O7 \\sim O7A \\sim C41: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(O8)=Sof(H8)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(1)
 Sof(O8A)=Sof(H8A)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(2)
 Sof(O7A)=Sof(H7AA)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(2)
 Sof(O6)=Sof(H6A)=Sof(H6B)=1-FVAR(3)
 Sof(O6A)=Sof(H6AA)=Sof(H6AB)=FVAR(3)
5.a Riding coordinates:
 O6(H6A,H6B), O6A(H6AA,H6AB)
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)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C41(H41D,H41E,H41F), C41(H41A,H41B,H41C), C42A(H42D,H42E,
 H42F)
5.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O7A(H7AA), O8(H8), O8A(H8A)
;
_shelx_res_checksum              68781
_shelx_hkl_checksum              23754
_olex2_submission_special_instructions 'No special instructions were received'