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_7062131
_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 H24 Fe N10, 2(B F4), 3(H2 O), C2 H6 O'
_chemical_formula_sum            'C38 H36 B2 F8 Fe N10 O4'
_chemical_formula_weight         926.24
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-10 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.579(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3214(6)
_cell_length_b                   15.2951(8)
_cell_length_c                   21.4537(11)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    110
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     4016.5(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81395
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.763
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0796P)^2^+7.8212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             7081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04774h2.cif
_cod_data_source_block           bb261
_cod_depositor_comments
'Adding full bibliography for 7062127--7062133.cif.'
_cod_database_code               7062131
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C27(H27), C16(H16), C3(H3), C17(H17), C24(H24), C6(H6), C5(H5),
 C29(H29), C18(H18), C32(H32), C34(H34), C14(H14), C11(H11), C28(H28), C21(H21),
  C23(H23), C33(H33), C22(H22), C35(H35), C4(H4), C10(H10), C36(H36), C9(H9)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              59860
_olex2_submission_special_instructions 'No special instructions were received'