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_7705824
_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(C24 H20 B)'
_chemical_formula_sum            'C130 H122 B2 Fe N10'
_chemical_formula_weight         1901.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                113.376(3)
_cell_angle_beta                 102.769(3)
_cell_angle_gamma                106.168(3)
_cell_formula_units_Z            2
_cell_length_a                   17.4723(6)
_cell_length_b                   18.4311(7)
_cell_length_c                   20.0010(7)
_cell_measurement_reflns_used    47715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.58
_cell_measurement_theta_min      2.60
_cell_volume                     5261.8(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.968
_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  0.2000
_diffrn_reflns_av_unetI/netI     0.1549
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            192446
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.789
_diffrn_reflns_theta_min         2.597
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.859
_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-orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       rod
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1490
_refine_ls_number_reflns         19961
_refine_ls_number_restraints     883
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1142P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6918
_reflns_number_total             20618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb128
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705824
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.585
_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
 C81, C81A, C80, C79A, C82, C80A, C39, C39A, C41, C41A, C40, C40A, C10Z, C9Z,
 C10Y, C11Z, C11Y, C8Z, C12Z, C9Y, C7Z, C12Y, C24Y, C23Y, C5Z, C6Z, C19Y, C20Y,
 C2Z, C3Z, C21Y, C4Z, C22Y, C24Z, C6Y, C19Z, C1Y, C2Y, C20Z, C3Y, C21Z, C4Y,
 C22Z, C5Y, C23Z, C7Y, C14Z, C8Y, C15Z, C16Z, C17Z, C13Z, C18Z, C13Y, B1Z, B1Y,
 C14Y, C15Y, C16Y, C17Y, C18Y
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C81 \\sim C81A \\sim C80 \\sim C79A \\sim C82 \\sim C80A \\sim C39 \\sim C39A
\\sim C41 \\sim C41A \\sim C40 \\sim C40A \\sim C10Z \\sim C9Z \\sim C10Y \\sim
C11Z \\sim C11Y \\sim C8Z \\sim C12Z \\sim C9Y \\sim C7Z \\sim C12Y \\sim C24Y
\\sim C23Y \\sim C5Z \\sim C6Z \\sim C19Y \\sim C20Y \\sim C2Z \\sim C3Z \\sim
C21Y \\sim C4Z \\sim C22Y \\sim C24Z \\sim C6Y \\sim C19Z \\sim C1Y \\sim C2Y
\\sim C20Z \\sim C3Y \\sim C21Z \\sim C4Y \\sim C22Z \\sim C5Y \\sim C23Z \\sim
C7Y \\sim C14Z \\sim C8Y \\sim C15Z \\sim C16Z \\sim C17Z \\sim C13Z \\sim C18Z
\\sim C13Y \\sim B1Z \\sim B1Y \\sim C14Y \\sim C15Y \\sim C16Y \\sim C17Y
\\sim C18Y: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C80(0.5) H80A(0.5)
 H80B(0.5) H80C(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) H82C(0.5) C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5) C40A(0.5)
 H40D(0.5) H40E(0.5) H40F(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
 C79A(0.5) H79A(0.5) H79B(0.5) H79C(0.5) C80A(0.5) H80D(0.5) H80E(0.5)
 H80F(0.5) C81A(0.5) H81D(0.5) H81E(0.5) H81F(0.5) C1Z(0.5) C2Z(0.5) H2Z(0.5)
 C3Z(0.5) H3Z(0.5) C4Z(0.5) H4Z(0.5) C5Z(0.5) H5Z(0.5) C6Z(0.5) H6Z(0.5)
 C7Z(0.5) C8Z(0.5) H8Z(0.5) C9Z(0.5) H9Z(0.5) C10Z(0.5) H10Z(0.5) C11Z(0.5)
 H11Z(0.5) C12Z(0.5) H12Z(0.5) C13Z(0.5) C14Z(0.5) H14Z(0.5) C15Z(0.5)
 H15Z(0.5) C16Z(0.5) H16Z(0.5) C17Z(0.5) H17Z(0.5) C18Z(0.5) H18Z(0.5)
 C19Z(0.5) C20Z(0.5) H20Z(0.5) C21Z(0.5) H21Z(0.5) C22Z(0.5) H22Z(0.5)
 C23Z(0.5) H23Z(0.5) C24Z(0.5) H24Z(0.5) B1Z(0.5) C1Y(0.5) C2Y(0.5) H2Y(0.5)
 C3Y(0.5) H3Y(0.5) C4Y(0.5) H4Y(0.5) C5Y(0.5) H5Y(0.5) C6Y(0.5) H6Y(0.5)
 C7Y(0.5) C8Y(0.5) H8Y(0.5) C9Y(0.5) H9Y(0.5) C10Y(0.5) H10Y(0.5) C11Y(0.5)
 H11Y(0.5) C12Y(0.5) H12Y(0.5) C13Y(0.5) C14Y(0.5) H14Y(0.5) C15Y(0.5)
 H15Y(0.5) C16Y(0.5) H16Y(0.5) C17Y(0.5) H17Y(0.5) C18Y(0.5) H18Y(0.5)
 C19Y(0.5) C20Y(0.5) H20Y(0.5) C21Y(0.5) H21Y(0.5) C22Y(0.5) H22Y(0.5)
 C23Y(0.5) H23Y(0.5) C24Y(0.5) H24Y(0.5) B1Y(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C31(H31A,H31B), C49(H49A,H49B), C72(H72A,H72B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29), C33(H33),
  C34(H34), C36(H36), C37(H37), C44(H44), C45(H45), C46(H46), C47(H47),
 C51(H51), C52(H52), C54(H54), C55(H55), C61(H61), C62(H62), C63(H63), C67(H67),
  C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C77(H77), C78(H78),
 C2Z(H2Z), C3Z(H3Z), C4Z(H4Z), C5Z(H5Z), C6Z(H6Z), C8Z(H8Z), C9Z(H9Z),
 C10Z(H10Z), C11Z(H11Z), C12Z(H12Z), C14Z(H14Z), C15Z(H15Z), C16Z(H16Z),
 C17Z(H17Z), C18Z(H18Z), C20Z(H20Z), C21Z(H21Z), C22Z(H22Z), C23Z(H23Z),
 C24Z(H24Z), C2X(H2X), C3X(H3X), C4X(H4X), C5X(H5X), C6X(H6X), C8X(H8X),
 C9X(H9X), C10X(H10X), C11X(H11X), C12X(H12X), C14X(H14X), C15X(H15X),
 C16X(H16X), C17X(H17X), C18X(H18X), C20X(H20X), C21X(H21X), C22X(H22X),
 C23X(H23X), C24X(H24X), C2Y(H2Y), C3Y(H3Y), C4Y(H4Y), C5Y(H5Y), C6Y(H6Y),
 C8Y(H8Y), C9Y(H9Y), C10Y(H10Y), C11Y(H11Y), C12Y(H12Y), C14Y(H14Y), C15Y(H15Y),
  C16Y(H16Y), C17Y(H17Y), C18Y(H18Y), C20Y(H20Y), C21Y(H21Y), C22Y(H22Y),
 C23Y(H23Y), C24Y(H24Y)
5.c Fitted hexagon refined as free rotating group:
 C1Z(C2Z,C3Z,C4Z,C5Z,C6Z), C7Z(C8Z,C9Z,C10Z,C11Z,C12Z), C13Z(C14Z,C15Z,C16Z,
 C17Z,C18Z), C19Z(C20Z,C21Z,C22Z,C23Z,C24Z), C1Y(C2Y,C3Y,C4Y,C5Y,C6Y), C7Y(C8Y,
 C9Y,C10Y,C11Y,C12Y), C13Y(C14Y,C15Y,C16Y,C17Y,C18Y), C19Y(C20Y,C21Y,C22Y,C23Y,
 C24Y)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C79A(H79A,H79B,H79C), C80A(H80D,H80E,H80F), C81A(H81D,H81E,H81F)
;
_shelx_res_checksum              41705
_olex2_submission_special_instructions 'No special instructions were received'