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_7709725
_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 H74 B4 Fe4 N26 O2 P2, 2[C4H11O2N]'
_chemical_formula_sum            'C68 H74 B4 Fe4 N26 O2 P2'
_chemical_formula_weight         1616.11
_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                   28.913(5)
_cell_length_b                   47.393(8)
_cell_length_c                   13.020(2)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.66
_cell_volume                     17841(5)
_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 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_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            121562
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.146
_diffrn_reflns_theta_max         25.146
_diffrn_reflns_theta_min         2.664
_diffrn_source_current           1.2
_diffrn_source_power             0.0576
_diffrn_source_voltage           48.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Darkred
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       Block
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.025(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7898
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+24.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                7577
_reflns_number_total             7898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00058j2.cif
_cod_data_source_block           100k
_cod_database_code               7709725
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97544
 0.02456
2. Restrained distances
 B2-H2B = B2-H2A
 0.98 with sigma of 0.02
 B2-H2A = B2-H2B
 0.98 with sigma of 0.02
 B2-H2C
 0.98 with sigma of 0.02
 B2-H2B = B2-H2A = B2-H2C
 1.15 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
H2C \\sim H2B \\sim H2A \\sim B2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(Fe2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 B1(H1)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C27(H27), C29(H29), C32(H32), C36(H36), C37(H37), C21(H21),
 C13(H13), C24(H24), C26(H26), C9(H9), C30(H30), C17(H17), C22(H22), C33(H33)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C5(H5A,H5B,
 H5C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3366
_shelx_hkl_checksum              71223
_shelx_fab_checksum              23538
_olex2_submission_special_instructions 'No special instructions were received'