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_7705827
_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(Cl O4), H2 O, C2 H6 O'
_chemical_formula_sum            'C100 H122 Cl2 Fe N10 O10'
_chemical_formula_weight         1750.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 113.4950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4211(4)
_cell_length_b                   28.6434(4)
_cell_length_c                   18.6619(4)
_cell_measurement_reflns_used    352184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.76
_cell_measurement_theta_min      2.92
_cell_volume                     9520.7(3)
_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 0.980
_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  0.1084
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            319586
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.504
_diffrn_reflns_theta_min         2.922
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.462
_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            violet
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         17540
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0747
_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^)+(0.1637P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12394
_reflns_number_total             17894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb191
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705827
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.588
_shelx_estimated_absorpt_t_min   0.383
_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, All O(H,H) groups
2. Restrained distances
 C1E-O9
 1.43 with sigma of 0.003
 C94-C91
 1.54 with sigma of 0.003
3. Rigid bond restraints
 C49, C48, C47, C91, C94, C93, C92, C2E, C1E, O5, O7, O6, Cl2, O8, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C49 \\sim C48 \\sim C47 \\sim C91 \\sim C94 \\sim C93 \\sim C92 \\sim C2E \\sim
C1E \\sim O5 \\sim O7 \\sim O6 \\sim Cl2 \\sim O8 \\sim O9: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Free rotating group:
 O10(H10A,H10B)
5.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C84(H84A,H84B), C35(H35A,H35B), C8(H8A,H8B), C1E(H1EA,H1EB)
5.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C14(H14), C10(H10), C6(H6), C52(H52), C30(H30), C75(H75), C3(H3),
 C55(H55), C12(H12), C73(H73), C33(H33), C90(H90), C53(H53), C5(H5), C59(H59),
 C39(H39), C79(H79), C37(H37), C24(H24), C82(H82), C31(H31), C74(H74), C54(H54),
  C32(H32), C81(H81), C4(H4), C26(H26), C80(H80), C41(H41), C86(H86), C25(H25),
 C61(H61), C88(H88)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C70(H70A,H70B,H70C), C18(H18A,H18B,H18C), C44(H44A,H44B,
 H44C), C98(H98A,H98B,H98C), C97(H97A,H97B,H97C), C66(H66A,H66B,H66C), C96(H96A,
 H96B,H96C), C45(H45A,H45B,H45C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C),
 C43(H43A,H43B,H43C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C71(H71A,H71B,
 H71C), C67(H67A,H67B,H67C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C47(H47A,
 H47B,H47C), C49(H49A,H49B,H49C), C92(H92A,H92B,H92C), C48(H48A,H48B,H48C),
 C93(H93A,H93B,H93C), C2E(H2EA,H2EB,H2EC), C94(H94A,H94B,H94C)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              40987
_shelx_fab_checksum              88417
_olex2_submission_special_instructions 'No special instructions were received'