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_7061770
_publ_section_title
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 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         'C20 H21 Cl4 Fe N4 O3'
_chemical_formula_sum            'C20 H21 Cl4 Fe N4 O3'
_chemical_formula_weight         563.070
_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_Int_Tables_number      14
_audit_creation_date             2021-06-16
_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                 99.143(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2923(8)
_cell_length_b                   10.0590(7)
_cell_length_c                   16.1597(11)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.73
_cell_volume                     2293.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46929
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9984
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.77
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.6466
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0563 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.9109.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             1152.206
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4024
_refine_diff_density_min         -0.3621
_refine_diff_density_rms         0.0913
_refine_ls_d_res_high            0.8189
_refine_ls_d_res_low             11.5169
_refine_ls_goodness_of_fit_ref   1.0480
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0480
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+1.7383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -17
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -11
_reflns_number_gt                3635
_reflns_number_total             4382
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj02294j2.cif
_cod_data_source_block           Rajnak_CRRM75B
_cod_depositor_comments
'Adding full bibliography for 7061770--7061774.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7061770
_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), C17(H17), C19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'