Effects of mono- or di-fluoro-substitution on spin crossover behavior in a pair of Schiff base-like Fe<sup>II</sup>-coordination polymers.
Luo, Yu; Zhou, Ren-He; Shao, Zhen; Liu, Dan; Lu, Han-Han; Shang, Meng-Jia; Zhao, Liang; Liu, Tao; Meng, Yin-Shan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14692–14700; doi:10.1039/d4dt01103a

data_7717164
_publ_section_title
;
 Effects of mono- or di-fluoro-substitution on spin crossover behavior in
 a pair of Schiff base-like Fe<sup>II</sup>-coordination polymers.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14692
_journal_page_last               14700
_journal_paper_doi               10.1039/d4dt01103a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C36 H31 F3 Fe N4 O6, C36 H29.207 F3 Fe N4 O6, 0.25(C H4 O), 0.5[], 0.5[]'
_chemical_formula_sum            'C72.25 H61.21 F6 Fe2 N8 O12.25'
_chemical_formula_weight         1463.19
_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             2024-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.356(15)
_cell_angle_beta                 93.002(12)
_cell_angle_gamma                107.035(17)
_cell_formula_units_Z            2
_cell_length_a                   12.217(5)
_cell_length_b                   13.650(8)
_cell_length_c                   23.294(9)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.20
_cell_volume                     3667(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83716
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.711
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1127 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.9327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             1509
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL 1                P -1         R = 0.09
CELL   12.2170   13.6500   23.2940     97.36     93.00    107.04
SPGR P-1
Q101 0.734 0.903 0.418 !       1.84 eA-3
Q102 0.818 1.008 0.408 !       1.72 eA-3
Q103 0.045 0.980 0.260 !       1.66 eA-3
C104 0.202 0.986 0.368 !       1.61 eA-3
Q105 0.354 0.984 0.440 !       1.59 eA-3
C106 0.194 0.909 0.366 !       1.58 eA-3
C107 0.890 0.781 0.238 !       1.56 eA-3
C108 0.251 0.101 0.378 !       1.52 eA-3
Q109 0.739 0.856 0.462 !       1.52 eA-3
Q110 0.941 0.749 0.061 !       1.46 eA-3
Q111 0.746 0.050 0.268 !       1.24 eA-3
Q112 0.559 0.065 0.479 !       1.22 eA-3
Q113 0.017 0.767 0.336 !       1.14 eA-3
C114 0.096 1.003 0.314 !       1.13 eA-3
C115 0.171 0.067 0.365 !       1.08 eA-3
Q116 0.961 0.879 0.270 !       1.06 eA-3
Q117 0.945 0.828 0.332 !       1.04 eA-3
Q118 0.990 0.719 0.102 !       1.04 eA-3
C119 0.286 0.891 0.413 !       1.04 eA-3
C120 0.174 0.093 0.344 !       1.04 eA-3
Q121 0.722 0.026 0.328 !       0.99 eA-3
C122 0.307 0.079 0.422 !       0.98 eA-3
Q123 0.639 0.952 0.316 !       0.94 eA-3
Q124 0.444 1.000 0.477 !       0.91 eA-3
C125 0.091 0.928 0.318 !       0.89 eA-3
Q126 0.906 0.691 0.336 !       0.89 eA-3
C127 0.147 0.960 0.343 !       0.89 eA-3
Q128 0.485 0.065 0.440 !       0.87 eA-3
C129 0.131 1.000 0.344 !       0.85 eA-3
Q130 1.007 0.765 0.425 !       0.84 eA-3
Q131 0.341 0.919 0.476 !       0.84 eA-3
Q132 0.564 0.302 0.331 !       0.81 eA-3
Q133 0.030 0.123 0.207 !       0.80 eA-3
C134 0.300 0.036 0.362 !       0.80 eA-3
Q135 0.260 0.436 0.382 !       0.79 eA-3
Q136 0.244 0.860 0.472 !       0.76 eA-3
Q137 0.714 0.560 0.353 !       0.72 eA-3
C138 0.028 0.871 0.260 !       0.69 eA-3
Q139 0.618 0.218 0.328 !       0.68 eA-3
Q140 0.948 0.668 0.153 !       0.67 eA-3
Q141 0.140 0.846 0.321 !       0.67 eA-3
C142 0.091 0.958 0.284 !       0.67 eA-3
Q143 0.894 0.030 0.445 !       0.66 eA-3
Q144 0.016 0.736 0.155 !       0.66 eA-3
Q145 0.081 0.965 0.369 !       0.62 eA-3
C146 0.213 0.107 0.429 !       0.61 eA-3
Q147 0.364 0.058 0.387 !       0.60 eA-3
Q148 0.650 0.126 0.468 !       0.60 eA-3
Q149 0.159 0.185 0.296 !       0.60 eA-3
Q150 0.109 0.941 0.243 !       0.60 eA-3
Q151 0.564 0.313 0.437 !       0.59 eA-3
Q152 0.167 0.473 0.319 !       0.59 eA-3
Q153 0.902 0.730 0.104 !       0.57 eA-3
Q154 0.044 0.105 0.363 !       0.56 eA-3
Q155 0.242 0.969 0.336 !       0.55 eA-3
Q156 0.310 0.125 0.359 !       0.55 eA-3
Q157 0.156 0.999 0.269 !       0.55 eA-3
Q158 0.516 0.234 0.447 !       0.53 eA-3
Q159 0.671 0.750 0.429 !       0.53 eA-3
Q160 0.606 0.577 0.097 !       0.52 eA-3
Q161 0.668 0.108 0.213 !       0.52 eA-3
Q162 0.937 0.755 0.180 !       0.52 eA-3
Q163 0.077 0.329 0.397 !       0.52 eA-3
Q164 0.292 0.060 0.313 !       0.52 eA-3
Q165 0.330 0.860 0.453 !       0.51 eA-3
Q166 0.128 0.964 0.403 !       0.51 eA-3
Q167 0.119 0.770 0.393 !       0.50 eA-3
Q168 0.982 0.015 0.046 !       0.50 eA-3
;
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         13871
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0715
_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^)+(0.0807P)^2^+9.0647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9006
_reflns_number_total             13871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01103a2.cif
_cod_data_source_block           2-120k
_cod_database_code               7717164
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O13-C73
 1.4 with sigma of 0.02
 C79-C78
 1.54 with sigma of 0.02
 O7-C78
 1.45 with sigma of 0.02
 O7-C79
 2.45 with sigma of 0.04
3. Restrained planarity
 C46, C75, C76, C51, C74, C71, F11, F10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C78 \\sim C79: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C78 \\sim C79 \\sim O7 \\sim O14 \\sim C3: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
F10 \\sim C71: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
H65 \\sim F8 \\sim C46 \\sim C75 \\sim C76 \\sim C51 \\sim C74 \\sim C71:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O15 \\sim C3: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H63)=Sof(F5)=1-FVAR(1)
 Sof(H65)=Sof(F8)=FVAR(1)
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(C74)=Sof(H74)=Sof(C71)=1-FVAR(2)
 Sof(C48)=Sof(C50)=Sof(H50)=Sof(C47)=Sof(C49)=FVAR(2)
 Sof(O7)=Sof(O14)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=Sof(H79A)=Sof(H79B)=
 Sof(H79C)=1-FVAR(3)
 Sof(O8)=Sof(O15)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=
 FVAR(3)
 Fixed Sof: O13(0.25) H13(0.25) C73(0.25) H73A(0.25) H73B(0.25) H73C(0.25)
 F9(0.25) F7(0.25) F6(0.25) F11(0.125) F10(0.125)
6.a Riding coordinates:
 O13(H13), C79(H79A,H79B,H79C)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C39(H39A,H39B), C19(H19A,H19B), C1(H1A,H1B), C78(H78A,H78B)
6.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C27(H27), C56(H56), C55(H55), C57(H57), C53(H53), C58(H58),
 C59(H59), C54(H54), C70(H70), C7(H7), C42(H42), C66(H66), C65(H65), C34(H34),
 C29(H29), C32(H32), C44(H44), C72(H72), C9(H9), C60(H60), C69(H69), C43(H43),
 C63(H63), C12(H12), C14(H14), C41(H41), C75(H75), C74(H74), C50(H50), C77(H77)
6.d Fitted hexagon refined as free rotating group:
 C46(C75,C76,C51,C74,C71)
6.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C37(H37A,H37B,H37C), C4(H4A,H4B,
 H4C), C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C20(H20A,H20B,H20C), C73(H73A,
 H73B,H73C), C2(H2A,H2B,H2C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'