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_7716242
_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 H25 B2 Fe N7 O, C2 H3 N'
_chemical_formula_sum            'C25 H28 B2 Fe N8 O'
_chemical_formula_weight         534.02
_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   geom
_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                 91.611(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.819(2)
_cell_length_b                   11.1057(7)
_cell_length_c                   20.7090(17)
_cell_measurement_reflns_used    30218
_cell_measurement_temperature    240
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      1.70
_cell_volume                     5475.9(7)
_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      240
_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 0.927
_diffrn_measurement_details
;
 3067 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  0.0391
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.718
_diffrn_reflns_theta_min         1.968
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.1064
_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    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1186
_reflns_d_resolution_high        0.696
_reflns_d_resolution_low         10.448
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              34
_reflns_limit_h_min              -33
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              28
_reflns_limit_l_min              -29
_reflns_number_gt                5570
_reflns_number_total             7890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01141d2.cif
_cod_data_source_block           xl-023-3b_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7716239--7716246.cif.'
_cod_original_cell_volume        5476.0(7)
_cod_database_code               7716242
_shelx_shelxl_version_number     2018/3
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N8-C24 \\sim N8A-C24A
 with sigma of 0.02
 N8-C25 \\sim N8A-C25A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N8A \\sim N8 \\sim C24A \\sim C24 \\sim C25A \\sim C25: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C25A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(N8A)=Sof(C24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(N8)=Sof(C24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
5.b 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)
5.c Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              99940
_shelx_hkl_checksum              18285
_olex2_submission_special_instructions 'No special instructions were received'