Low-spin and spin-crossover iron(II) complexes with pyridyl-benzimidazole ligands: synthesis, and structural, magnetic and solution study.
Brachňaková, Barbora; Adamko KoŽíšková, Júlia; KoŽíšek, Jozef; Melníková, Eva; Gál, Miroslav; Herchel, Radovan; Dubaj, Tibor; Šalitroš, Ivan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17786–17795; doi:10.1039/d0dt03497e

data_7705829
_publ_section_title
;
 Low-spin and spin-crossover iron(II) complexes with pyridyl-benzimidazole
 ligands: synthesis, and structural, magnetic and solution study.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17786
_journal_page_last               17795
_journal_paper_doi               10.1039/d0dt03497e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C82 H82 Fe N10, 2(Cl O4), C3 H6 O'
_chemical_formula_sum            'C85 H88 Cl2 Fe N10 O9'
_chemical_formula_weight         1520.41
_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     dual
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-06-19 deposited with the CCDC.	2020-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.7600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5941(2)
_cell_length_b                   16.9152(2)
_cell_length_c                   22.1820(2)
_cell_measurement_reflns_used    232563
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.70
_cell_measurement_theta_min      2.50
_cell_volume                     7716.25(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            409872
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        58.933
_diffrn_reflns_theta_max         58.933
_diffrn_reflns_theta_min         2.500
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7901
_reflns_number_total             11085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb196
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705829
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.611
_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
2. Rigid bond restraints
 C3E, C1E, O1E, C2E, C58, C59, C57, C17, C18, C16, C15, C12, C11, C13, C39,
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C3E \\sim C1E \\sim O1E \\sim C2E \\sim C58 \\sim C59 \\sim C57 \\sim C17 \\sim
C18 \\sim C16 \\sim C15 \\sim C12 \\sim C11 \\sim C13 \\sim C39 \\sim C40 \\sim
C41: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C72(H72A,H72B), C8(H8A,H8B), C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C26(H26), C22(H22), C20(H20), C28(H28), C70(H70), C61(H61),
 C27(H27), C63(H63), C5(H5), C21(H21), C6(H6), C33(H33), C47(H47), C74(H74),
 C62(H62), C67(H67), C3(H3), C69(H69), C77(H77), C75(H75), C4(H4), C78(H78),
 C68(H68), C55(H55), C44(H44), C52(H52), C51(H51), C10(H10), C54(H54), C36(H36),
  C34(H34), C37(H37), C45(H45), C14(H14), C46(H46), C11(H11), C13(H13)
4.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C41(H41A,H41B,
 H41C), C40(H40A,H40B,H40C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C39(H39A,
 H39B,H39C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C57(H57A,H57B,H57C),
 C18(H18A,H18B,H18C), C2E(H2EA,H2EB,H2EC), C3E(H3EA,H3EB,H3EC)
;
_shelx_res_checksum              48734
_olex2_submission_special_instructions 'No special instructions were received'