Impact of the Schiff base ligand substituents on the solid state and solution properties of eleven iron(iii) complexes
Pogány, Lukáš; Brachňaková, Barbora; Masárová, Petra; Moncol, Ján; Pavlik, Ján; Gál, Miroslav; Mazúr, Milan; Herchel, Radovan; Nemec, Ivan; Šalitroš, Ivan; New Journal of Chemistry 43 (2019) 13916–; doi:10.1039/C9NJ03087E

data_7058693
_publ_section_title
;
 Impact of the Schiff base ligand substituents on the solid state and
 solution properties of eleven iron(iii) complexes
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13916
_journal_paper_doi               10.1039/C9NJ03087E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C23 H29 Cl Fe N3 O4'
_chemical_formula_sum            'C23 H29 Cl Fe N3 O4'
_chemical_formula_weight         502.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.162(5)
_cell_angle_beta                 91.327(5)
_cell_angle_gamma                107.242(5)
_cell_formula_units_Z            4
_cell_length_a                   9.8897(6)
_cell_length_b                   10.8138(6)
_cell_length_c                   22.2761(13)
_cell_measurement_reflns_used    7225
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      4.14
_cell_volume                     2274.5(2)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       '(CrysAlisPro; Agilent, 2012)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23677
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlis Pro, Rigaku Oxford Diffraction Ltd.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9274
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+2.7086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6642
_reflns_number_total             9274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03087e4.cif
_cod_data_source_block           5_150K
_cod_depositor_comments
'Adding full bibliography for 7058691--7058703.cif.'
_cod_database_code               7058693
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.786
_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. Restrained distances
 C30A-N4A \\sim C30B-N4B \\sim C36-N6
 with sigma of 0.001
 N4A-C31A \\sim N4B-C31B \\sim N6-C35A \\sim N6-C35B
 with sigma of 0.001
 C31A-C32A \\sim C31B-C32B \\sim C33A-C34A \\sim C34A-C35A \\sim C33B-C34B
\\sim C34B-C35B
 with sigma of 0.001
 N5A-C32A \\sim N5A-C33A \\sim N5B-C32B \\sim N5B-C33B
 with sigma of 0.001
 C29A-N4A \\sim C29B-N4B
 with sigma of 0.02
 C30A-C31A \\sim C30B-C31B \\sim C36-C35A \\sim C36-C35B
 with sigma of 0.02
 N4A-C32A \\sim N4B-C32B
 with sigma of 0.02
 C31A-N5A \\sim C31B-N5B
 with sigma of 0.02
 C32A-C33A \\sim C32B-C33B
 with sigma of 0.02
 N5A-C34A \\sim N5B-C34B
 with sigma of 0.02
 C33A-C35A \\sim C33B-C35B
 with sigma of 0.02
 N6-C34A \\sim N6-C34B
 with sigma of 0.02
 C2A-O3A \\sim C2B-O3B
 with sigma of 0.02
 O7-C45 \\sim O8A-C47A \\sim O8B-C47B \\sim O3A-C22A \\sim O3B-C22B
 with sigma of 0.001
 C45-C46 \\sim C47A-C48A \\sim C47B-C48B \\sim C22A-C23A \\sim C22B-C23B
 with sigma of 0.001
 C41-C45 \\sim C25A-C47A \\sim C25B-C47B \\sim C2A-C22A \\sim C2B-C22B
 with sigma of 0.02
 O7-C46 \\sim O8A-C48A \\sim O8B-C48B \\sim O3A-C23A \\sim O3B-C23B
 with sigma of 0.02
 C6A-C7 \\sim C6B-C7
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O5A) = Uanis(O5B) = Uanis(O6)
Uanis(O8A) = Uanis(O8B)
Uanis(C47A) = Uanis(C47B)
Uanis(C48A) = Uanis(C48B)
Uanis(C30A) = Uanis(C30B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C25B)
Uanis(C26A) = Uanis(C26B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
Uanis(C29A) = Uanis(C29B)
Uanis(C1A) = Uanis(C1B) = Uanis(C6A) = Uanis(C6B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C34A) = Uanis(C34B)
4. Rigid body (RIGU) restrains
 C6A, C1A, C2A, C3A, C4A, C5A, O3A, C22A, C23A, C6B, C1B, C2B, C3B, C4B, C5B,
 O3B, C22B, C23B, O5A, C24A, C25A, C26A, C27A, C28A, C29A, O8A, C30A, N4A, N5A,
 C31A, C32A, C33A, C34A, C35A, C47A, C48A, O5B, C24B, C25B, C26B, C27B, C28B,
 C29B, O8B, C30B, N4B, N5B, C31B, C32B, C33B, C34B, C35B, C47B, C48B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(C6B)=Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5BA)=Sof(O3B)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H7A)=Sof(C6A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5AA)=Sof(O3A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(O5B)=Sof(C24B)=Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=
 Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(O8B)=Sof(C30B)=Sof(H30B)=Sof(N4B)=Sof(N5B)=
 Sof(H5B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=
 Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(C35B)=Sof(H35C)=
 Sof(H35D)=Sof(C47B)=Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48D)=Sof(H48E)=
 Sof(H48F)=1-FVAR(2)
 Sof(O5A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(O8A)=Sof(C30A)=Sof(H30A)=Sof(N4A)=Sof(N5A)=
 Sof(H5A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(C35A)=Sof(H35A)=
 Sof(H35B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(2)
6.a Free rotating group:
 O5A(C24A,C25A,C26A,C27A,C28A,C29A,O8A,C30A,N4A,N5A,C31A,C32A,C33A,C34A,C35A,
 C47A,C48A), O5B(C24B,C25B,C26B,C27B,C28B,C29B,O8B,C30B,N4B,N5B,C31B,C32B,C33B,
 C34B,C35B,C47B,C48B)
6.b Ternary CH refined with riding coordinates:
 N2(H2), N5A(H5A), N5B(H5B)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C20(H20A,H20B), C45(H45A,H45B), C22A(H22A,H22B), C22B(H22C,H22D), C31A(H31A,
 H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C35A(H35A,H35B),
 C47A(H47A,H47B), C31B(H31C,H31D), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,
 H34D), C35B(H35C,H35D), C47B(H47C,H47D)
6.d Me refined with riding coordinates:
 C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F), C48A(H48A,H48B,H48C), C48B(H48D,
 H48E,H48F)
6.e Aromatic/amide H refined with riding coordinates:
 C7(H7A), C7(H7B), C13(H13), C15(H15), C16(H16), C17(H17), C36(H36), C38(H38),
 C39(H39), C40(H40), C3A(H3A), C4A(H4A), C5A(H5AA), C3B(H3B), C4B(H4B),
 C5B(H5BA), C26A(H26A), C27A(H27A), C28A(H28A), C30A(H30A), C26B(H26B),
 C27B(H27B), C28B(H28B), C30B(H30B)
6.f Fitted hexagon refined as free rotating group:
 C6A(C1A,C2A,C3A,C4A,C5A), C6B(C1B,C2B,C3B,C4B,C5B)
6.g Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              45460
_olex2_submission_special_instructions 'No special instructions were received'