Pyridine modifications regulate the electronics and reactivity of Fe-pyridinophane complexes.
Mekhail, Magy A.; Pota, Kristof; Kharel, Sugam; Freire, David M.; Green, Kayla N.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 892–901; doi:10.1039/d2dt03485a

data_7711978
_publ_section_title
;
 Pyridine modifications regulate the electronics and reactivity of
 Fe-pyridinophane complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              892
_journal_page_last               901
_journal_paper_doi               10.1039/d2dt03485a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C13 H23 Cl2 Fe N5, C F3 O3 S'
_chemical_formula_sum            'C14 H23 Cl2 F3 Fe N5 O3 S'
_chemical_formula_weight         525.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-01-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-01-25 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8637(4)
_cell_length_b                   8.6169(5)
_cell_length_c                   36.4304(19)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.90
_cell_volume                     2154.6(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            54536
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.429
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0728 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8905.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.241
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         3778
_refine_ls_number_restraints     476
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.1186
_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^)+73.3927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2586
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3761
_reflns_number_total             3778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03485a2.cif
_cod_data_source_block           mm_iii_102821_monoclinic
_cod_depositor_comments
'Adding full bibliography for 7711977--7711979.cif.'
_cod_database_code               7711978
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(13)
 0.50(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C14-F3 = C14-F4 = C14-F5
 1.33 with sigma of 0.02
 C14-S6
 1.82 with sigma of 0.02
 S6-O7 = S6-O8 = S6-O9
 1.44 with sigma of 0.02
 C14-O7
 2.58 with sigma of 0.04
 C14-O9
 2.57 with sigma of 0.04
 C14-O8
 2.56 with sigma of 0.04
 C14-F3 \\sim C14-F4 \\sim C14-F5
 with sigma of 0.02
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.04
 S6-F3 \\sim S6-F4 \\sim S6-F5
 with sigma of 0.04
 S6-O7 \\sim S6-O8 \\sim S6-O9
 with sigma of 0.02
 O7-O8 \\sim O8-O9 \\sim O7-O9
 with sigma of 0.04
 C14-O7 \\sim C14-O8 \\sim C14-O9
 with sigma of 0.04
 O7-O9 \\sim O7A-O9A
 with sigma of 0.04
 C14-F4 \\sim C2A-F4A
 with sigma of 0.02
 C14-F5 \\sim C2A-F5A
 with sigma of 0.02
 C14-S6 \\sim C2A-S6A
 with sigma of 0.02
 C14-F3 \\sim C2A-F3A
 with sigma of 0.02
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 S6-O7 \\sim S6A-O7A
 with sigma of 0.02
 S6-O8 \\sim S6A-O8A
 with sigma of 0.02
 S6-O9 \\sim S6A-O9A
 with sigma of 0.02
 F3-S6 \\sim F3A-S6A
 with sigma of 0.04
 F4-S6 \\sim F4A-S6A
 with sigma of 0.04
 F5-S6 \\sim F5A-S6A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 C14-O7 \\sim C2A-O7A
 with sigma of 0.04
 C14-O8 \\sim C2A-O8A
 with sigma of 0.04
 C14-O9 \\sim C2A-O9A
 with sigma of 0.04
 O8-O9 \\sim O8A-O9A
 with sigma of 0.04
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
4. Restrained planarity
 C1, N4, C8, C9, C10, C11
 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
C14 \\sim F3 \\sim F4 \\sim F5 \\sim S6 \\sim O7 \\sim O8 \\sim O9: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C14, F3, F4, F5, S6, O7, O8, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: C14(0.6) F3(0.6) F4(0.6) F5(0.6) S6(0.6) O7(0.6) O8(0.6) O9(0.6)
 S6A(0.4) C2A(0.4) F3A(0.4) F4A(0.4) F5A(0.4) O7A(0.4) O8A(0.4) O9A(0.4)
8.a Ternary CH refined with riding coordinates:
 N3(H3), N1(H1), N2(H2)
8.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B)
8.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11)
8.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 20 electrons were 
found in a volume of 128\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 0.5[H2O] per Formula Unit 
which account for 20 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   0.9
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6586
_shelx_fab_checksum              52272
_olex2_submission_special_instructions 'No special instructions were received'