Pyridyl-benzimidazole derivatives decorated with phenylazo substituents and their low-spin iron(ii) complexes: a study of the synthesis, structure and photoisomerization
Orvoš, Jakub; Fischer, Róbert; Brachňaková, Barbora; Pavlik, Ján; Moncoľ, Ján; Šagátová, Alexandra; Fronc, Marek; Kožíšek, Jozef; Routaboul, Lucie; Bousseksou, Azzedine; Šalitroš, Ivan; New Journal of Chemistry 47 (2023) 1488–1497; doi:10.1039/D2NJ04774H

data_7062133
_publ_section_title
;
 Pyridyl-benzimidazole derivatives decorated with phenylazo substituents
 and their low-spin iron(ii) complexes: a study of the synthesis,
 structure and photoisomerization
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1488
_journal_page_last               1497
_journal_paper_doi               10.1039/D2NJ04774H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C36 H26 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C36 H26 Cl2 Fe N10 O8'
_chemical_formula_weight         853.42
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.23290(10)
_cell_length_b                   16.50510(10)
_cell_length_c                   17.50870(10)
_cell_measurement_reflns_used    341828
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.55
_cell_measurement_theta_min      2.53
_cell_volume                     3819.77(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_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 0.994
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            204691
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.000
_diffrn_reflns_theta_min         4.895
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.016
_exptl_absorpt_correction_T_max  0.0061
_exptl_absorpt_correction_T_min  0.0014
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0776P)^2^+2.7864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7267
_reflns_number_total             7464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04774h2.cif
_cod_data_source_block           bb413
_cod_depositor_comments
'Adding full bibliography for 7062127--7062133.cif.'
_cod_database_code               7062133
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), C36(H36), C9(H9), C35(H35), C16(H16), C6(H6), C34(H34),
 C23(H23), C5(H5), C3(H3), C24(H24), C10(H10), C28(H28), C29(H29), C18(H18),
 C32(H32), C21(H21), C11(H11), C22(H22), C33(H33), C14(H14), C4(H4), C27(H27),
 C15(H15), C17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54187
_shelx_fab_checksum              95592
_olex2_submission_special_instructions 'No special instructions were received'