An azido-bridged [FeII4] grid-like molecule showing spin crossover behaviour
Guo, Zhilin; You, Maolin; Deng, Yi-Fei; Liu, Qiang; Meng, Yin-Shan; Pikramenou, Zoe; Zhang, Yuan-Zhu; Dalton Transactions  (2021) –; doi:10.1039/D1DT01908B

data_7708189
_publ_section_title
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 An azido-bridged [FeII4] grid-like molecule showing spin crossover
 behaviour
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01908B
_journal_year                    2021
_chemical_formula_moiety         'C56 H40 Fe4 N28, 4(C24 H20 B), C4 H6 N2'
_chemical_formula_sum            'C156 H126 B4 Fe4 N30'
_chemical_formula_weight         2687.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-18 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4466(3)
_cell_length_b                   17.4466(3)
_cell_length_c                   43.6969(13)
_cell_measurement_reflns_used    5393
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      62.53
_cell_measurement_theta_min      3.95
_cell_volume                     13300.6(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            26215
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        65.150
_diffrn_reflns_theta_max         65.150
_diffrn_reflns_theta_min         3.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.954
_exptl_absorpt_correction_T_max  0.1621
_exptl_absorpt_correction_T_min  0.0471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1266 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.2906. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5667
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0742P)^2^+2.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3785
_reflns_number_total             5667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01908b2.cif
_cod_data_source_block           300k
_cod_original_cell_volume        13300.6(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7708189
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.438
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N5, N6
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.08
3. Uiso/Uaniso restraints and constraints
N5 \\sim N6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) = Uanis(N6)
4. Others
 Fixed Sof: H39A(0.5) H39B(0.5) H39C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C19(H19), C34(H34), C20(H20), C16(H16), C38(H38), C14(H14),
 C32(H32), C22(H22), C17(H17), C4(H4), C35(H35), C36(H36), C1(H1), C18(H18),
 C26(H26), C28(H28), C29(H29), C11(H11), C31(H31), C3(H3), C24(H24), C37(H37),
 C25(H25), C30(H30), C12(H12), C13(H13), C23(H23), C2(H2)
5.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              6104
_shelx_hkl_checksum              53281
_olex2_submission_special_instructions 'No special instructions were received'