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_7705830
_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(B F4)'
_chemical_formula_sum            'C98 H114 B2 F8 Fe N10'
_chemical_formula_weight         1661.47
_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             2020-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-19 deposited with the CCDC.	2020-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                67.5660(10)
_cell_angle_beta                 83.7780(10)
_cell_angle_gamma                72.0360(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8365(2)
_cell_length_b                   18.3000(2)
_cell_length_c                   19.4293(3)
_cell_measurement_reflns_used    118791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.28
_cell_measurement_theta_min      2.73
_cell_volume                     4638.02(12)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.966
_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  0.0774
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            182316
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.776
_diffrn_reflns_theta_min         2.730
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.820
_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    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1760
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.893
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.789
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         17845
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.791
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.1318
_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          0.3832
_refine_ls_wR_factor_ref         0.3986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14915
_reflns_number_total             18479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb252
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705830
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.627
_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
 C91-C93
 1.54 with sigma of 0.003
 C92-C91
 1.54 with sigma of 0.003
 C94-C91
 1.54 with sigma of 0.003
 C95-C98
 1.54 with sigma of 0.003
 C95-C97
 1.54 with sigma of 0.003
 C95-C96
 1.54 with sigma of 0.003
 C15-C18
 1.54 with sigma of 0.003
 C15-C16
 1.54 with sigma of 0.003
 C15-C17
 1.54 with sigma of 0.003
 C19-C22
 1.54 with sigma of 0.003
 C19-C20
 1.54 with sigma of 0.003
 C19-C21
 1.54 with sigma of 0.003
 C46-C47
 1.54 with sigma of 0.003
 C46-C49
 1.54 with sigma of 0.003
 C46-C48
 1.54 with sigma of 0.003
 C42-C44
 1.54 with sigma of 0.003
 C42-C45
 1.54 with sigma of 0.003
 C42-C43
 1.54 with sigma of 0.003
 C64-C65
 1.54 with sigma of 0.003
 C64-C67
 1.54 with sigma of 0.003
 C64-C66
 1.54 with sigma of 0.003
 C68-C69
 1.54 with sigma of 0.003
 C68-C71
 1.54 with sigma of 0.003
 C68-C70
 1.54 with sigma of 0.003
 F5-F7 \\sim F6-F7
 with sigma of 0.04
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C46 \\sim C49 \\sim C47 \\sim C48: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C92 \\sim C91 \\sim C94 \\sim C93: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C94 \\sim C92 \\sim C93: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C91 \\sim C94 \\sim C92 \\sim C93: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C47 \\sim C46 \\sim C49 \\sim C48: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 N2, C27, C23, Fe1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87, C91, C94, C92, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C35(H35A,H35B), C57(H57A,H57B), C84(H84A,H84B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C14(H14), C24(H24),
 C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C39(H39),
  C41(H41), C52(H52), C53(H53), C54(H54), C55(H55), C59(H59), C61(H61),
 C63(H63), C73(H73), C74(H74), C75(H75), C79(H79), C80(H80), C81(H81), C82(H82),
  C86(H86), C88(H88), C90(H90)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C),
 C97(H97A,H97B,H97C), C98(H98A,H98B,H98C)
;
_shelx_res_checksum              8856
_shelx_fab_checksum              40958
_olex2_submission_special_instructions 'No special instructions were received'