Ligand symmetry significantly affects spin crossover behaviour in isomeric [Fe(pybox)<sub>2</sub>]<sup>2+</sup> complexes.
Wang, Run-Guo; Meng, Yin-Shan; Gao, Fang-Fang; Gao, Wan-Qing; Liu, Chun-Hua; Li, Anyang; Liu, Tao; Zhu, Yuan-Yuan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3369–3378; doi:10.1039/d0dt03978k

data_7706564
_publ_section_title
;
 Ligand symmetry significantly affects spin crossover behaviour in
 isomeric [Fe(pybox)<sub>2</sub>]<sup>2+</sup> complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3369
_journal_page_last               3378
_journal_paper_doi               10.1039/d0dt03978k
_journal_volume                  50
_journal_year                    2021
_chemical_compound_source        no
_chemical_formula_moiety         'C46 H38 Fe N6 O4, 2(F6 P)'
_chemical_formula_sum            'C56 H53 F12 Fe N11 O4 P2'
_chemical_formula_weight         1289.88
_chemical_name_common            1(PF6)-MeCN-163K
_chemical_name_systematic        1(PF6)-MeCN-163K
_chemical_properties_physical    Air-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.525(8)
_cell_length_b                   12.034(2)
_cell_length_c                   23.788(5)
_cell_measurement_reflns_used    16025
_cell_measurement_temperature    163.15
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      1.1487
_cell_volume                     10149(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      163.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34044
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             5296
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile and ether'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
A solvent mask was calculated and 882 electrons were 
found in a volume of 1524\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 5[C2 H3 N] per Formula Unit,
which account for 880 electrons per unit cell.
;
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11585
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0805
_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^)+(0.0898P)^2^+28.3440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10170
_reflns_number_total             11585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03978k2.cif
_cod_data_source_block           2045169
_cod_depositor_comments
'Adding full bibliography for 7706562--7706567.cif.'
_cod_database_code               7706564
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.02
 F7-F9 \\sim F8-F10 \\sim F12-F11
 with sigma of 0.05
 F7-F8 \\sim F7-F10 \\sim F7-F11 \\sim F7-F12 \\sim F9-F8 \\sim F9-F10 \\sim
F9-F11 \\sim F9-F12 \\sim F10-F7
 \\sim F10-F9 \\sim F8-F9 \\sim F8-F7
 with sigma of 0.04
 F13-F14 \\sim F13-F16 \\sim F13-F17 \\sim F13-F18 \\sim F15-F14 \\sim F15-F16
\\sim F15-F17 \\sim F15-F18
 \\sim F16-F13 \\sim F16-F15 \\sim F14-F15 \\sim F14-F13
 with sigma of 0.04
 P3-F13 \\sim P3-F14 \\sim P3-F15 \\sim P3-F16 \\sim P3-F17 \\sim P3-F18
 with sigma of 0.02
 F13-F15 \\sim F14-F16 \\sim F18-F17
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
P2 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P3 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 P2, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P3, F13, F14, F15, F16, F17, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P3)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(1)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C30(H30), C40(H40)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C31(H31A,H31B), C39(H39A,H39B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75199
_shelx_fab_checksum              77412
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'