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_7705828
_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         'C69 H69 Fe N9, 2(Cl O4)'
_chemical_formula_sum            'C69 H69 Cl2 Fe N9 O8'
_chemical_formula_weight         1279.09
_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   geom
_audit_creation_date             2019-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-05 deposited with the CCDC.	2020-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8200(4)
_cell_length_b                   15.3369(2)
_cell_length_c                   24.2864(4)
_cell_measurement_reflns_used    146917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.51
_cell_measurement_theta_min      3.44
_cell_volume                     7161.0(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.1038
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            298049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.619
_diffrn_reflns_theta_min         3.439
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.631
_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            bown-red
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         13841
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1314P)^2^+4.6330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8342
_reflns_number_total             13979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           BBPz_2_CE2
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705828
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.484
_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. Restrained distances
 C43-C44
 1.54 with sigma of 0.003
 C43-C45
 1.54 with sigma of 0.003
 C43-C46
 1.54 with sigma of 0.003
 C66-C67
 1.54 with sigma of 0.003
 C66-C68
 1.54 with sigma of 0.003
 C66-C69
 1.54 with sigma of 0.003
 C68-C67 \\sim C67-C69
 with sigma of 0.02
3. Rigid bond restraints
 C20, C21, C22, C23, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C60,
 C61, C62, C63, C64, C65, C66, C67, C68, C69, Cl2A, O5A, O6A, O7A, O8A, Cl2B,
 O5B, O6B, O7B, O8B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C60 \\sim C61 \\sim
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim
Cl2A \\sim O5A \\sim O6A \\sim O7A \\sim O8A \\sim Cl2B \\sim O5B \\sim O6B
\\sim O7B \\sim O8B: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
5. Others
 Fixed Sof: Cl2A(0.75) O5A(0.75) O6A(0.75) O7A(0.75) O8A(0.75) Cl2B(0.25)
 O5B(0.25) O6B(0.25) O7B(0.25) O8B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C36(H36A,H36B), C59(H59A,H59B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C18(H18), C19(H19), C26(H26), C27(H27), C28(H28), C29(H29),
  C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C41(H41),
 C42(H42), C49(H49), C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57),
  C58(H58), C61(H61), C62(H62), C64(H64), C65(H65)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              42291
_shelx_fab_checksum              21863
_olex2_submission_special_instructions 'No special instructions were received'