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_7705826
_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         'C98 H114 Fe N10, 2(C F3 O3 S), 3(C2 H6 O)'
_chemical_formula_sum            'C106 H132 F6 Fe N10 O9 S2'
_chemical_formula_weight         1924.19
_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
_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                85.3170(10)
_cell_angle_beta                 89.5340(10)
_cell_angle_gamma                64.2240(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2071(2)
_cell_length_b                   15.9757(2)
_cell_length_c                   25.0471(3)
_cell_measurement_reflns_used    392882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.61
_cell_measurement_theta_min      3.08
_cell_volume                     5099.79(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.969
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            288727
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.166
_diffrn_reflns_theta_min         3.083
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.712
_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    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.125
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.0021(5)
_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   2.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1235
_refine_ls_number_reflns         19465
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      2.035
_refine_ls_R_factor_all          0.1430
_refine_ls_R_factor_gt           0.1378
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4312
_refine_ls_wR_factor_ref         0.4349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16804
_reflns_number_total             20099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb193
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_original_cell_volume        5099.80(12)
_cod_database_code               7705826
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.672
_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. Rigid bond restraints
 O1E, C1E, C2E, F3, C1T, F2, F1, O3, S1, O2, O1, C4E, C3E, O2E, F4, C2T, F5,
 F6, O4, S2, O6, O5, C5E, C6E, O3E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O1E \\sim C1E \\sim C2E \\sim F3 \\sim C1T \\sim F2 \\sim F1 \\sim O3 \\sim S1
\\sim O2 \\sim O1 \\sim C4E \\sim C3E \\sim O2E \\sim F4 \\sim C2T \\sim F5
\\sim F6 \\sim O4 \\sim S2 \\sim O6 \\sim O5 \\sim C5E \\sim C6E \\sim O3E:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C57(H57A,H57B), C35(H35A,H35B), C84(H84A,H84B), C3E(H3EA,H3EB),
 C1E(H1EA,H1EB), C5E(H5EA,H5EB)
4.b Aromatic/amide H refined with riding coordinates:
 C63(H63), C12(H12), C33(H33), C55(H55), C82(H82), C10(H10), C41(H41),
 C86(H86), C5(H5), C39(H39), C3(H3), C90(H90), C6(H6), C73(H73), C14(H14),
 C37(H37), C81(H81), C75(H75), C88(H88), C4(H4), C25(H25), C52(H52), C24(H24),
 C61(H61), C74(H74), C53(H53), C59(H59), C31(H31), C30(H30), C32(H32), C26(H26),
  C80(H80), C54(H54), C79(H79)
4.c Tetrahedral OH refined with riding coordinates:
 O2E(H2E), O1E(H1E), O3E(H3E)
4.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C96(H96A,H96B,H96C), C17(H17A,H17B,H17C), C69(H69A,H69B,
 H69C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C98(H98A,H98B,H98C), C22(H22A,
 H22B,H22C), C18(H18A,H18B,H18C), C97(H97A,H97B,H97C), C48(H48A,H48B,H48C),
 C21(H21A,H21B,H21C), C66(H66A,H66B,H66C), C71(H71A,H71B,H71C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C65(H65A,H65B,H65C), C45(H45A,H45B,H45C), C70(H70A,
 H70B,H70C), C67(H67A,H67B,H67C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C),
 C49(H49A,H49B,H49C), C93(H93A,H93B,H93C), C4E(H4EA,H4EB,H4EC), C2E(H2EA,H2EB,
 H2EC), C6E(H6EA,H6EB,H6EC)
;
_shelx_res_checksum              52853
_shelx_fab_checksum              71441
_olex2_submission_special_instructions 'No special instructions were received'