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_7716771
_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         'C51 H57 Fe N9, 2(B F4), C4 H10 O'
_chemical_formula_sum            'C55 H67 B2 F8 Fe N9 O'
_chemical_formula_weight         1099.64
_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                 101.2251(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5535(3)
_cell_length_b                   16.3130(2)
_cell_length_c                   18.8082(3)
_cell_measurement_reflns_used    8225
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      68.366
_cell_measurement_theta_min      3.156
_cell_volume                     5282.70(14)
_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      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30191
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.401
_diffrn_reflns_theta_min         3.152
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.8322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         9568
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0611P)^2^+7.7322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8640
_reflns_number_total             9568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01338g2.cif
_cod_data_source_block           02
_cod_depositor_comments
'Adding full bibliography for 7716767--7716771.cif.'
_cod_original_cell_volume        5282.70(16)
_cod_database_code               7716771
_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
 B1-F1 \\sim B1-F1A \\sim B1-F3 \\sim B1-F3A \\sim B1-F4 \\sim B1-F4A
 with sigma of 0.02
 C36-C37 \\sim C36A-C37A \\sim C37-C38 \\sim C37A-C38A \\sim C38-C39 \\sim
C38A-C39
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 F4-B1 \\sim F4-B1A
 with sigma of 0.02
 F1-F4 \\sim F4-F3 \\sim F3-F1
 with sigma of 0.02
 F1A-F4A \\sim F4A-F3A \\sim F3A-F1A
 with sigma of 0.02
 F3-B1 \\sim F3A-B1A \\sim F1-B1 \\sim F1A-B1A \\sim F4-B1 \\sim F4A-B1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F3 \\sim F3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F4A \\sim F4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(C36) = Uanis(C36A) = Uanis(C35) = Uanis(C35A)
Uanis(C37) = Uanis(C38) = Uanis(C37A) = Uanis(C38A)
Uanis(F1) = Uanis(F1A)
Uanis(B1A) = Uanis(B1)
Uanis(F6A) = Uanis(F6)
Uanis(F5A) = Uanis(F5)
4. Others
 Sof(F4A)=Sof(F3A)=Sof(F1A)=Sof(B1A)=1-FVAR(1)
 Sof(F4)=Sof(F3)=Sof(F1)=Sof(B1)=FVAR(1)
 Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F5)=Sof(F6)=FVAR(2)
 Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=
 Sof(H38D)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36C)=
 Sof(H36D)=1-FVAR(3)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(H39A)=Sof(H39B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C30(H30A,H30B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,
 H33B), C31(H31A,H31B), C4(H4A,H4B), C38(H38A,H38B), C3(H3A,H3B), C37(H37A,
 H37B), C5(H5A,H5B), C2(H2A,H2B), C36(H36A,H36B), C53(H53A,H53B), C54(H54A,
 H54B), C37A(H37C,H37D), C38A(H38C,H38D), C36A(H36C,H36D)
5.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C9(H9), C7(H7), C43(H43), C27(H27), C10(H10), C28(H28), C21(H21),
 C49(H49), C16(H16), C14(H14), C19(H19), C17(H17), C50(H50), C42(H42), C51(H51),
  C44(H44), C18(H18), C8(H8), C48(H48), C25(H25), C15(H15), C20(H20), C26(H26)
5.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C1(H1A,H1B,H1C), C52(H52A,H52B,
 H52C), C55(H55A,H55B,H55C), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              75921
_olex2_submission_special_instructions 'No special instructions were received'