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_7711977
_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         'C12 H20 Cl2 Fe N4 O, C F3 O3 S'
_chemical_formula_sum            'C13 H20 Cl2 F3 Fe N4 O4 S'
_chemical_formula_weight         512.140
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-29
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.07.25 svn.r36e0af09 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.035(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0308(5)
_cell_length_b                   13.8067(9)
_cell_length_c                   20.6288(14)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      3.60
_cell_volume                     1987.4(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9789
_diffrn_measured_fraction_theta_max 0.9801
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.9789
_diffrn_reflns_Laue_measured_fraction_max 0.9801
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            164665
_diffrn_reflns_point_group_measured_fraction_full 0.9789
_diffrn_reflns_point_group_measured_fraction_max 0.9801
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.92
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0764 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.9099.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       prism
_exptl_crystal_F_000             1047.866
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.9963
_refine_diff_density_min         -0.6814
_refine_diff_density_rms         0.1424
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.9779
_refine_ls_extinction_coef       0.0092
_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   1.0046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0046
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+21.6446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                3791
_reflns_number_total             3832
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt03485a2.cif
_cod_data_source_block           MM_III_111820_OMePyN3_0m
_cod_depositor_comments
'Adding full bibliography for 7711977--7711979.cif.'
_cod_database_code               7711977
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C2(H2a,H2b), C4(H4a,H4b), C3(H3a,H3b), C7(H7a,H7b), C5(H5a,H5b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9)
2.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c)
;
_olex2_submission_special_instructions 'No special instructions were received'