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_7705825
_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         'C82 H82 Fe N10, 2(C F3 O3 S)'
_chemical_formula_sum            'C84 H82 F6 Fe N10 O6 S2'
_chemical_formula_weight         1561.56
_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             2019-08-12
_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                 104.386(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4248(4)
_cell_length_b                   19.6746(4)
_cell_length_c                   28.0978(7)
_cell_measurement_reflns_used    100813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.69
_cell_measurement_theta_min      2.77
_cell_volume                     7724.2(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.951
_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  0.1718
_diffrn_reflns_av_unetI/netI     0.1354
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            157716
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.756
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.772
_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            orange-brown
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         14390
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      2.209
_refine_ls_R_factor_all          0.2914
_refine_ls_R_factor_gt           0.2418
_refine_ls_shift/su_max          0.357
_refine_ls_shift/su_mean         0.013
_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          0.6194
_refine_ls_wR_factor_ref         0.6262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7111
_reflns_number_total             15125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03497e3.cif
_cod_data_source_block           bb195_bb13
_cod_depositor_comments
'Adding full bibliography for 7705824--7705831.cif.'
_cod_database_code               7705825
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.479
_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
 C53-C54 \\sim C55-C50 \\sim C51-C52
 with sigma of 0.02
 C70-C69 \\sim C68-C67 \\sim C66-C71
 with sigma of 0.02
 C48-C47 \\sim C46-C45 \\sim C44-C43
 with sigma of 0.02
 C58-C57 \\sim C57-C59
 with sigma of 0.02
3. Rigid bond restraints
 C32, C33, C34, C35, C36, C37, C38, C39, C40, C41, C50, C51, C52, C53, C54,
 C55, C56, C57, C58, C59, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56 \\sim C57 \\sim C58 \\sim C59 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C31(H31A,H31B), C49(H49A,H49B), C72(H72A,H72B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29), C33(H33),
  C34(H34), C36(H36), C37(H37), C44(H44), C45(H45), C46(H46), C47(H47),
 C51(H51), C52(H52), C54(H54), C55(H55), C61(H61), C62(H62), C63(H63), C67(H67),
  C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C77(H77), C78(H78)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C)
;
_shelx_res_checksum              8093
_olex2_submission_special_instructions 'No special instructions were received'