Hexacoordinate high-spin Fe(iii) complexes composed of a pentadentate amino-type ligand and pseudohalido coligands
Mičová, Romana; Bielková, Zuzana; Rajnák, Cyril; Titiš, Ján; Gembický, Milan; Renz, Franz; Malina, Ondřej; Samoľová, Erika; Nováčiková, Jana; Boča, Roman; New Journal of Chemistry 46 (2022) 18083–18089; doi:10.1039/D2NJ02294J

data_7061772
_publ_section_title
;
 Hexacoordinate high-spin Fe(iii) complexes composed of a pentadentate
 amino-type ligand and pseudohalido coligands
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18083
_journal_page_last               18089
_journal_paper_doi               10.1039/D2NJ02294J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C19 H21 Cl5 Fe N3 O2'
_chemical_formula_sum            'C19 H21 Cl5 Fe N3 O2'
_chemical_formula_weight         556.49
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.368(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9994(16)
_cell_length_b                   8.9714(14)
_cell_length_c                   22.698(3)
_cell_measurement_reflns_used    9257
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.43
_cell_volume                     2221.3(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27413
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         1.809
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  0.4910
_exptl_absorpt_correction_T_min  0.3957
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1023 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.8059.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0365P)^2^+5.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3656
_reflns_number_total             4552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02294j2.cif
_cod_data_source_block           crrm71
_cod_depositor_comments
'Adding full bibliography for 7061770--7061774.cif.'
_cod_original_cell_volume        2221.4(6)
_cod_database_code               7061772
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C15(H15), C17(H17)
;
_shelx_res_checksum              78953
_olex2_submission_special_instructions 'No special instructions were received'