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_7058702
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
_cell_angle_beta                 107.526(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9944(2)
_cell_length_b                   22.3122(5)
_cell_length_c                   10.9698(2)
_cell_measurement_reflns_used    21053
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.53
_cell_measurement_theta_min      3.96
_cell_volume                     2332.68(9)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.136.0 (STOE, 2017)
;
_computing_data_reduction
'X-Area Integrate 1.71.2.0 (STOE, 2017) X-Area LANA 1.71.6.0 (STOE, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Pilatus3R 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS3R 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari with Xenocs Genix3D Cu HF'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            27726
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.417
_diffrn_reflns_theta_min         3.963
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.527
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'STOE LANA, J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.'
_exptl_crystal_colour            'blackish red'
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     524
_refine_ls_restrained_S_all      0.801
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2940
_reflns_number_total             4496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03087e4.cif
_cod_data_source_block           5_293K
_cod_depositor_comments
'Adding full bibliography for 7058691--7058703.cif.'
_cod_database_code               7058702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.139
_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. Shared sites
{N1, N1A}
3. Restrained distances
 Fe1-N2 \\sim Fe1-N2A
 with sigma of 0.002
 Fe1-N3 \\sim Fe1-N3A
 with sigma of 0.002
 Fe1-O2 \\sim Fe1-O2A
 with sigma of 0.002
 O3-C20 \\sim O4-C22 \\sim O4A-C22A
 with sigma of 0.004
 C20-C21 \\sim C22-C23 \\sim C22A-C23A
 with sigma of 0.004
 O3-C21 \\sim O4-C23 \\sim O4A-C23A
 with sigma of 0.3
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N1A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(N2) = Uanis(N2A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(N3) = Uanis(N3A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C15) = Uanis(C15A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(O2) = Uanis(O2A)
Uanis(O4) = Uanis(O4A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N1A, C8A, C9A, C10A, N2A, C11A, C12A, N3A, C13A, C14A, C15A, C16A, C17A, C18A,
C19A, O2A, O4A, C22A, C23A} sigma for 1-2: 0.01, 1-3: 0.04
as
{N1, C8, C9, C10, N2, C11, C12, N3, C13, C14, C15, C16, C17, C18, C19, O2, O4,
C22, C23}
7. Others
 Sof(H7B)=Sof(N1A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(N2A)=Sof(H2A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(N3A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(C15A)=
 Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(O2A)=
 Sof(O4A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 1-FVAR(1)
 Sof(H7A)=Sof(N1)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(N2)=Sof(H2)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(N3)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(C19)=Sof(O2)=Sof(O4)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
8.a Riding coordinates:
 C7(H7A,H7B)
8.b Ternary CH refined with riding coordinates:
 N2(H2), N2A(H2A)
8.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C22(H22A,H22B), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10C,
 H10D), C11A(H11C,H11D), C12A(H12C,H12D), C22A(H22C,H22D)
8.d Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F)
8.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C17(H17), C13A(H13A),
 C15A(H15A), C16A(H16A), C17A(H17A)
8.f Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              3828
_olex2_submission_special_instructions 'No special instructions were received'