Synergetic Spin Singlet-Quintet Switching and Luminescence in mononuclear Fe(II) 1,3,4-Oxadiazole Tetradentate Chelates with NCBH3 Co-ligand
Sundaresan, Sriram; Becker, Jens-Georg; Eppelsheimer, Julian; Sedykh, Alexander E.; Carrella, Luca; Müller-Buschbaum, Klaus; Rentschler, Eva; Dalton Transactions  (2023) –; doi:10.1039/D3DT02420B

data_7713752
_publ_section_title
;
 Synergetic Spin Singlet-Quintet Switching and Luminescence in mononuclear
 Fe(II) 1,3,4-Oxadiazole Tetradentate Chelates with NCBH3 Co-ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02420B
_journal_year                    2023
_chemical_formula_moiety         'C27 H27 B2 Fe N7 O, 1.5(C H4 O)'
_chemical_formula_sum            'C28.5 H33 B2 Fe N7 O2.5'
_chemical_formula_weight         591.09
_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             2023-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.182(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.0632(7)
_cell_length_b                   10.5691(2)
_cell_length_c                   21.3067(6)
_cell_measurement_reflns_used    63217
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      1.92
_cell_volume                     5835.1(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_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 0.929
_diffrn_measurement_details
;
 1595 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  0.0308
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51641
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.771
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.2842
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8470
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0892P)^2^+0.2519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6496
_reflns_number_total             8470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02420b2.cif
_cod_data_source_block           je-266-1bnew
_cod_original_formula_sum        'C28.50 H33 B2 Fe N7 O2.50'
_cod_database_code               7713752
_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, All O(H) groups
2. Restrained distances
 O3-C29 \\sim O4-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30 \\sim C29: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 1.7A
Uanis(O2) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O2(0.5) H2(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) O4(0.5)
 H4A(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) O3(0.5) H3A(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5)
5.a Riding coordinates:
 O3(H3A), C30(H30A,H30B,H30C)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C14(H14A,H14B), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C25(H25), C1(H1), C9(H9), C19(H19), C24(H24), C22(H22), C18(H18),
 C17(H17), C8(H8), C3(H3), C23(H23), C4(H4), C6(H6), C5(H5)
5.d Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4A)
;
_shelx_res_checksum              2881
_olex2_submission_special_instructions 'No special instructions were received'