Manipulating the spin crossover behaviour in a series of cyanide-bridged {FeIII2FeII2} molecular squares through NCE- co-ligands
You, Maolin; Nguyen, Giang Truong; Shao, Dong; Wang, Te; Chang, Xiaoyong; Ungur, Liviu; Zhang, Yuan-Zhu; Dalton Transactions  (2022) –; doi:10.1039/D2DT00058J

data_7709728
_publ_section_title
;
 Manipulating the spin crossover behaviour in a series of cyanide-bridged
 {FeIII2FeII2} molecular squares through NCE- co-ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00058J
_journal_year                    2022
_chemical_formula_moiety         'C68 H68 B2 Fe4 N26 O2 P2 S2, 1.091(C H4 O)'
_chemical_formula_sum            'C69.09 H72.37 B2 Fe4 N26 O3.09 P2 S2'
_chemical_formula_weight         1687.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.674(5)
_cell_length_b                   47.644(9)
_cell_length_c                   13.108(3)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    300.01
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.61
_cell_volume                     18532(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Apex3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.01
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51316
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         2.615
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.05759999999999999
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           48.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.7704.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Darkred
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       Block
_exptl_crystal_F_000             6957
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0762P)^2^+13.9787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                7462
_reflns_number_total             8048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00058j2.cif
_cod_data_source_block           300K_CCDC2
_cod_database_code               7709728
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97568
 0.02432
2. Restrained distances
 O2-C35
 1.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
H17C \\sim H17B \\sim H17A \\sim C17: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Others
 Sof(O2)=Sof(H2)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
5.a Riding coordinates:
 O2(H2), C35(H35A,H35B,H35C)
5.b Ternary CH refined with riding coordinates:
 B1(H1)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C20(H20), C22(H22), C32(H32), C34(H34), C9(H9), C19(H19),
 C23(H23), C25(H25), C27(H27), C29(H29), C15(H15), C30(H30), C33(H33)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C17(H17A,H17B,
 H17C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              94355
_shelx_hkl_checksum              53797
_olex2_submission_special_instructions 'No special instructions were received'