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_7716246
_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
'C23 H19 Fe N7 O S2, 1.333(C2 H3 N), C1.167 H1 N0.667'
_chemical_formula_sum            'C28 H26.5 Fe N9.5 O S2'
_chemical_formula_weight         632.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.110(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.6059(10)
_cell_length_b                   11.7584(5)
_cell_length_c                   17.6574(6)
_cell_measurement_reflns_used    37934
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.88
_cell_measurement_theta_min      1.86
_cell_volume                     6134.8(4)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173
_diffrn_detector                 Pilatus100K
_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 0.919
_diffrn_measurement_details
;
 3079 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_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.969
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.2527
_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    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0848
_reflns_d_resolution_high        0.691
_reflns_d_resolution_low         10.925
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              43
_reflns_limit_h_min              -38
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                6971
_reflns_number_total             8963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01141d2.cif
_cod_data_source_block           je-259-4
_cod_depositor_comments
'Adding full bibliography for 7716239--7716246.cif.'
_cod_original_formula_sum        'C28 H26.50 Fe N9.50 O S2'
_cod_database_code               7716246
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.815
_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
Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: N9(0.5) C26(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) N10(0.5)
 C28(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) N11(0.5) C30(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5)
4.a Riding coordinates:
 C29(H29A,H29B,H29C)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21)
4.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              76531
_shelx_hkl_checksum              47749
_olex2_submission_special_instructions 'No special instructions were received'