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_7711979
_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
'C11 H17 Cl2 Fe I N4, 0.667(C F3 O3 S), 0.333(C F3.044 O3.118 S)'
_chemical_formula_sum            'C12 H17 Cl2 F3.01 Fe I N4 O3.04 S'
_chemical_formula_weight         608.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.259(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   25.1399(17)
_cell_length_b                   8.2657(5)
_cell_length_c                   31.080(2)
_cell_measurement_reflns_used    9534
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      3.02
_cell_volume                     6018.9(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            386474
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.627
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    2.705
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.8402.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       prism
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.000055(16)
_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   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         16935
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+22.0427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15770
_reflns_number_total             16935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03485a2.cif
_cod_data_source_block           mm_ii_new
_cod_depositor_comments
'Adding full bibliography for 7711977--7711979.cif.'
_cod_database_code               7711979
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.351
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 S00F-O01F \\sim S00G-O01G
 with sigma of 0.02
 O023-O10 \\sim O0-O10A
 with sigma of 0.04
 S00F-O023 \\sim S00G-O0
 with sigma of 0.02
 S00F-C029 \\sim S00G-C0
 with sigma of 0.02
 S00F-O10 \\sim S00G-O10A
 with sigma of 0.02
 F00R-C029 \\sim F00S-C0
 with sigma of 0.02
 O01F-C029 \\sim O01G-C0
 with sigma of 0.04
 F021-C029 \\sim F1-C0
 with sigma of 0.02
 F027-C029 \\sim F0-C0
 with sigma of 0.02
 O01F-O023 \\sim O01G-O0
 with sigma of 0.04
 O01F-O10 \\sim O01G-O10A
 with sigma of 0.04
 F021-F027 \\sim F1-F0
 with sigma of 0.04
 O023-C029 \\sim O0-C0
 with sigma of 0.04
 S00F-F00R \\sim S00G-F00S
 with sigma of 0.04
 S00F-F021 \\sim S00G-F1
 with sigma of 0.04
 S00F-F027 \\sim S00G-F0
 with sigma of 0.04
 C029-O10 \\sim C0-O10A
 with sigma of 0.04
 F00R-F021 \\sim F00S-F1
 with sigma of 0.04
 F00R-F027 \\sim F00S-F0
 with sigma of 0.04
3. Others
 Sof(O10A)=Sof(O01G)=Sof(S00G)=Sof(O0)=Sof(C0)=Sof(F0)=Sof(F1)=Sof(F00S)=1-
 FVAR(1)
 Sof(S00F)=Sof(F00R)=Sof(O01F)=Sof(F021)=Sof(O023)=Sof(F027)=Sof(C029)=
 Sof(O10)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N00P(H00P), N00Q(H00Q), N00S(H00S), N00V(H00V), N00Y(H00Y), N00Z(H00Z),
 N010(H010), N011(H011), N01C(H01)
4.b Secondary CH2 refined with riding coordinates:
 C01I(H01N,H01O), C01J(H2,H), C01O(H01P,H01Q), C01P(H3,HA), C01Q(H01R,H01S),
 C01R(H01T,H01U), C01S(H01A,H01B), C01T(H01C,H01D), C01U(H01E,H01F), C01V(H01V,
 H01W), C01W(H01G,H01I), C01X(H01J,H01K), C01Z(H01X,H01Y), C020(H02A,H02B),
 C022(H02C,H02D), C024(H02E,H02F), C025(H02G,H02H), C028(H02I,H02J)
4.c Aromatic/amide H refined with riding coordinates:
 C019(H019), C01A(H01Z), C01D(H01M), C01G(H1), C01H(H01H), C01L(H01L)
;
_shelx_res_checksum              42988
_olex2_submission_special_instructions 'No special instructions were received'