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_7705831
_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(B F4)'
_chemical_formula_sum            'C69 H69 B2 F8 Fe N9'
_chemical_formula_weight         1253.81
_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
_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                 104.172(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1330(6)
_cell_length_b                   15.2696(3)
_cell_length_c                   39.7635(11)
_cell_measurement_reflns_used    214778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.53
_cell_measurement_theta_min      2.44
_cell_volume                     14206.9(6)
_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_measured_fraction_theta_full 0.995
_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  0.2218
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            651623
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.727
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.682
_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            dark_violet
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         27363
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.1224
_refine_ls_shift/su_max          3.660
_refine_ls_shift/su_mean         0.034
_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          0.3698
_refine_ls_wR_factor_ref         0.4296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8990
_reflns_number_total             28276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb137
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705831
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.534
_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
 C23-C21
 2.42 with sigma of 0.003
 C23-C22
 2.42 with sigma of 0.003
 C22-C21
 2.42 with sigma of 0.003
 C20-C23
 1.54 with sigma of 0.003
 C20-C21
 1.54 with sigma of 0.003
 C20-C22
 1.54 with sigma of 0.003
3. Rigid bond restraints
 C23, C22, C21, C69, C67, C68, C138, C137, C136, F13, B4, F16, F15, F14, F4,
 F3, B1, F1, F2, C114, C90, C92, C91, C113, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C23 \\sim C22 \\sim C21 \\sim C69 \\sim C67 \\sim C68 \\sim C138 \\sim C137
\\sim C136 \\sim F13 \\sim B4 \\sim F16 \\sim F15 \\sim F14 \\sim F4 \\sim F3
\\sim B1 \\sim F1 \\sim F2 \\sim C114 \\sim C90 \\sim C92 \\sim C91 \\sim C113
\\sim C115: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C105(H10A,H10B), C36(H36A,H36B), C82(H82A,H82B), C13(H13J,H13K), C128(H12A,
 H12B), C59(H59A,H59B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C50(H50), C51(H51), C120(H120), C29(H29), C74(H74), C98(H98),
 C125(H125), C5(H5), C9(H9), C121(H121), C101(H101), C124(H124), C127(H127),
 C26(H26), C104(H104), C11(H11), C33(H33), C102(H102), C52(H52), C97(H97),
 C15(H15), C119(H119), C34(H34), C80(H80), C75(H75), C111(H111), C81(H81),
 C10(H10), C103(H103), C118(H118), C27(H27), C35(H35), C39(H39), C12(H12),
 C58(H58), C56(H56), C73(H73), C38(H38), C42(H42), C28(H28), C41(H41),
 C107(H107), C110(H110), C32(H32), C3(H3), C78(H78), C126(H126), C79(H79),
 C55(H55), C134(H134), C57(H57), C19(H19), C72(H72), C4(H4), C95(H95),
 C133(H133), C84(H84), C130(H130), C96(H96), C108(H108), C49(H49), C18(H18),
 C131(H131), C61(H61), C16(H16), C88(H88), C85(H85), C65(H65), C87(H87),
 C62(H62), C64(H64)
5.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C115(H11A,H11B,
 H11C), C92(H92A,H92B,H92C), C113(H11D,H11E,H11F), C136(H13A,H13B,H13C),
 C91(H91A,H91B,H91C), C21(H21A,H21B,H21C), C114(H11G,H11H,H11I), C69(H69A,H69B,
 H69C), C137(H13D,H13E,H13F), C22(H22A,H22B,H22C), C138(H13G,H13H,H13I),
 C68(H68A,H68B,H68C), C67(H67A,H67B,H67C), C23(H23A,H23B,H23C), C90(H90A,H90B,
 H90C)
;
_shelx_res_checksum              25960
_shelx_fab_checksum              96565
_olex2_submission_special_instructions 'No special instructions were received'