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_7708192
_publ_section_title
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 An azido-bridged [FeII4] grid-like molecule showing spin crossover
 behaviour
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01908B
_journal_year                    2021
_chemical_formula_moiety
'C56 H64 Fe4 N36, C H Cl3, 4(C24 H20 B), C H4 O, 4(C2 H3 N), [+ solvents]2[CHCl3], 1[CH3OH]'
_chemical_formula_sum            'C162 H161 B4 Cl3 Fe4 N40 O'
_chemical_formula_weight         3057.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
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2021-09-02 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                89.217(2)
_cell_angle_beta                 72.662(2)
_cell_angle_gamma                62.820(2)
_cell_formula_units_Z            2
_cell_length_a                   18.0455(8)
_cell_length_b                   19.1164(8)
_cell_length_c                   28.9018(12)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.24
_cell_volume                     8377.7(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            200308
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.314
_exptl_absorpt_coefficient_mu    0.449
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1960
_refine_ls_number_reflns         37755
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0492P)^2^+8.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27166
_reflns_number_total             37755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01908b2.cif
_cod_data_source_block           fe4
_cod_original_cell_volume        8377.7(6)
_cod_database_code               7708192
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.877
_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, All O(H) groups
2. Restrained distances
 C168-C160 = C2-C1
 1.52 with sigma of 0.02
 N38-C168 = C2-N38A
 2.72 with sigma of 0.02
 N38-C160 = N38A-C1
 1.2 with sigma of 0.02
 N32-N31
 1.2 with sigma of 0.001
 N25-N26
 1.2 with sigma of 0.001
 N35-N34
 1.2 with sigma of 0.001
3. Rigid bond restraints
 N31, N32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N25, N26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N35, N34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C2 \\sim N38A \\sim C1 \\sim C168 \\sim N38 \\sim C160: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N38) = Uanis(N38A)
Uanis(C160) = Uanis(C1)
Uanis(C168) = Uanis(C2)
5. Others
 Sof(N38A)=Sof(C1)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(H2c)=1-FVAR(1)
 Sof(N38)=Sof(C160)=Sof(C168)=Sof(H16g)=Sof(H16h)=Sof(H16i)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C150(H150)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C23(H23), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31),
 C37(H37), C39(H39), C41(H41), C42(H42), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C52(H52), C53(H53), C54(H54), C56(H56), C59(H59), C62(H62),
 C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C97(H97), C99(H99), C100(H100), C103(H103), C105(H105), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C121(H121), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C129(H129), C130(H130), C131(H131),
 C132(H132), C133(H133), C135(H135), C137(H137), C139(H139), C140(H140),
 C141(H141), C144(H144), C145(H145), C146(H146), C147(H147), C148(H148),
 C149(H149), C151(H151), C153(H153), C154(H154), C155(H155), C156(H156),
 C158(H158), C159(H159)
6.c Idealised Me refined as rotating group:
 C51(H51a,H51b,H51c), C73(H73a,H73b,H73c), C76(H76a,H76b,H76c), C77(H77a,H77b,
 H77c), C95(H95a,H95b,H95c), C96(H96a,H96b,H96c), C98(H98a,H98b,H98c),
 C101(H10a,H10b,H10c), C102(H10d,H10e,H10f), C104(H10g,H10h,H10i), C120(H12a,
 H12b,H12c), C134(H13a,H13b,H13c), C136(H13d,H13e,H13f), C142(H14a,H14b,H14c),
 C143(H14d,H14e,H14f), C152(H15a,H15b,H15c), C157(H15d,H15e,H15f), C161(H16a,
 H16b,H16c), C164(H16j,H16k,H16l), C165(H16d,H16e,H16f), C168(H16g,H16h,H16i),
 C2(H2a,H2b,H2c)
6.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 273 electrons were 
found in a volume of 1035\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
4[CHCl3], 2[CH3OH] per Unit Cell 
which account for 268 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11985
_shelx_hkl_checksum              30556
_shelx_fab_checksum              52557
_olex2_submission_special_instructions 'No special instructions were received'