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_7058697
_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         'C18 H17 Br2 Cl Fe N3 O2, C H4 O'
_chemical_formula_sum            'C19 H21 Br2 Cl Fe N3 O3'
_chemical_formula_weight         590.51
_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     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                94.651(2)
_cell_angle_beta                 101.474(3)
_cell_angle_gamma                106.584(3)
_cell_formula_units_Z            4
_cell_length_a                   11.5360(4)
_cell_length_b                   12.6730(4)
_cell_length_c                   16.2456(5)
_cell_measurement_reflns_used    7562
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      4.086
_cell_volume                     2206.59(13)
_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      150.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur 2 Single Crystal X-ray Diffractometer with Sapphire CCD Detector.'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.191
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlis RED, Rigaku Oxford Diffraction Ltd.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       needle
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.231
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         9005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6507
_reflns_number_total             9005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03087e4.cif
_cod_data_source_block           4_150K
_cod_depositor_comments
'Adding full bibliography for 7058691--7058703.cif.'
_cod_database_code               7058697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.238
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N5(H5A)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C17(H17),
 C20(H20), C21(H21), C23(H23), C25(H25), C30(H30), C32(H32), C34(H34), C35(H35)
2.d Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
2.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S)
;
_shelx_res_checksum              97103
_olex2_submission_special_instructions 'No special instructions were received'