Above room temperature spin crossover in mononuclear iron(II) complexes featuring pyridyl-benzimidazole bidentate ligands adorned with aliphatic chains.
Šagátová, Alexandra; Kotrle, Kamil; Brachňaková, Barbora; Havlíček, Lubomír; Nemec, Ivan; Herchel, Radovan; Hofbauerova, Monika; Halahovets, Yuriy; Šiffalovič, Peter; Čižmár, Erik; Fellner, Ondřej F; Šalitroš, Ivan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14037–14045; doi:10.1039/d4dt01338g

data_7716769
_publ_section_title
;
 Above room temperature spin crossover in mononuclear iron(II) complexes
 featuring pyridyl-benzimidazole bidentate ligands adorned with aliphatic
 chains.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14037
_journal_page_last               14045
_journal_paper_doi               10.1039/d4dt01338g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C57 H69 Fe N9, 2(Cl O4)'
_chemical_formula_sum            'C57 H69 Cl2 Fe N9 O8'
_chemical_formula_weight         1134.96
_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             2024-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9658(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.58967(13)
_cell_length_b                   15.02560(17)
_cell_length_c                   25.1896(3)
_cell_measurement_reflns_used    18373
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      71.2170
_cell_measurement_theta_min      3.3350
_cell_volume                     5481.27(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'XtaLAB Synergy'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.622
_diffrn_reflns_theta_min         3.336
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         10589
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0424P)^2^+3.9367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9682
_reflns_number_total             10589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01338g2.cif
_cod_data_source_block           04
_cod_depositor_comments
'Adding full bibliography for 7716767--7716771.cif.'
_cod_original_cell_volume        5481.28(10)
_cod_database_code               7716769
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C40 \\sim C39-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A \\sim C41-C42 \\sim C41-C42A
 with sigma of 0.02
 C44-C43 \\sim C44-C43A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 C41-C43 \\sim C41-C43A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C41A) = Uanis(C41)
Uanis(C40A) = Uanis(C40)
4. Others
 Sof(H39C)=Sof(H39D)=Sof(H44C)=Sof(H44D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C40A)=
 Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H44A)=Sof(H44B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C39(H39C,H39D),
  C40(H40A,H40B), C44(H44A,H44B), C44(H44C,H44D), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C41A(H41C,H41D), C42A(H42C,H42D), C43A(H43C,H43D),
 C40A(H40C,H40D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31),
  C46(H46), C47(H47), C48(H48), C49(H49), C53(H53), C54(H54), C55(H55), C56(H56)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              71392
_olex2_submission_special_instructions 'No special instructions were received'