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_7058696
_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         'C22 H25 Br2 Cl Fe N3 O4, H2 O'
_chemical_formula_sum            'C22 H27 Br2 Cl Fe N3 O5'
_chemical_formula_weight         664.58
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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
_cell_angle_beta                 112.820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0070(10)
_cell_length_b                   16.9410(10)
_cell_length_c                   13.6630(10)
_cell_measurement_reflns_used    8694
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      4.089
_cell_volume                     2561.7(4)
_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      293
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.1635
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9415
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.850
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.488
_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    1.723
_exptl_crystal_description       needle
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00048(18)
_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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5134
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.2067
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2457
_reflns_number_total             5134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03087e4.cif
_cod_data_source_block           8_293K
_cod_depositor_comments
'Adding full bibliography for 7058691--7058703.cif.'
_cod_database_code               7058696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-H5A = O5-H5B
 0.82 with sigma of 0.001
 H5A-H5B
 1.365 with sigma of 0.02
 H5A-O2_$1 = H5B-O4_$1
 2.1 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Riding coordinates:
 O5(H5A,H5B)
4.b Ternary CH refined with riding coordinates:
 N2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B)
4.d Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
4.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C14(H14), C17(H17), C18(H18)
;
_shelx_res_checksum              65467
_olex2_submission_special_instructions 'No special instructions were received'