A combined theoretical and experimental approach to determine the right choice of co-ligand to impart spin crossover in Fe(II) complexes based on 1,3,4-oxadiazole ligands.
Sundaresan, Sriram; Eppelsheimer, Julian; Gera, Esha; Wiener, Lukas; Carrella, Luca M.; Vignesh, Kuduva R.; Rentschler, Eva; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10303–10317; doi:10.1039/d4dt01141d

data_7716239
_publ_section_title
;
 A combined theoretical and experimental approach to determine the right
 choice of co-ligand to impart spin crossover in Fe(II) complexes based on
 1,3,4-oxadiazole ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10303
_journal_page_last               10317
_journal_paper_doi               10.1039/d4dt01141d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H36 Fe2 N12 O2, 4(Cl O4), 2(C H3 N O2)'
_chemical_formula_sum            'C42 H42 Cl4 Fe2 N14 O22'
_chemical_formula_weight         1348.39
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.600(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5361(4)
_cell_length_b                   16.0432(6)
_cell_length_c                   13.6085(5)
_cell_measurement_reflns_used    38385
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.79
_cell_measurement_theta_min      1.97
_cell_volume                     2723.87(17)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_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      150(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details
;
 2182 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31060
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.803
_diffrn_reflns_theta_min         1.968
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.6837
_exptl_absorpt_correction_T_min  0.5083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7639
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.4056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5795
_reflns_number_total             7639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01141d2.cif
_cod_data_source_block           je-215-1
_cod_depositor_comments
'Adding full bibliography for 7716239--7716246.cif.'
_cod_database_code               7716239
_shelx_shelxl_version_number     2016/6
_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. Uiso/Uaniso restraints and constraints
O4 \\sim O4A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O2A \\sim O2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O3 \\sim O3A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Sof(O9A)=Sof(O6A)=Sof(O8A)=1-FVAR(1)
 Sof(O8)=Sof(O6)=Sof(O9)=FVAR(1)
 Sof(O2A)=Sof(O5A)=Sof(O3A)=Sof(O4A)=1-FVAR(2)
 Sof(O2)=Sof(O4)=Sof(O5)=Sof(O3)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C20(H20), C5(H5), C13(H13), C7(H7), C11(H11), C6(H6),
 C12(H12), C19(H19), C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              21663
_shelx_hkl_checksum              31514
_olex2_submission_special_instructions 'No special instructions were received'