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_7706566
_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(Cl O4)'
_chemical_formula_sum            'C46 H38 Cl2 Fe N6 O12'
_chemical_formula_weight         993.57
_chemical_name_common            1(ClO4)-296K
_chemical_name_systematic        1(ClO4)-296K
_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                 118.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.453(5)
_cell_length_b                   11.2220(12)
_cell_length_c                   21.261(2)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.027
_cell_measurement_theta_min      2.179
_cell_volume                     8907.8(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'kappa X8 APEX II Bruker ICMMO'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.9025.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             4096
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile and ether'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         8752
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+29.7906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6749
_reflns_number_total             8752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03978k2.cif
_cod_data_source_block           2045167
_cod_depositor_comments
'Adding full bibliography for 7706562--7706567.cif.'
_cod_original_cell_volume        8907.7(17)
_cod_database_code               7706566
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   'SADABS; Bruker, 2000'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8
 with sigma of 0.01
 Cl1-O5 \\sim Cl1A-O5A
 with sigma of 0.02
 O11-O9 \\sim O11A-O9A
 with sigma of 0.04
 Cl1-O6 \\sim Cl1A-O6A
 with sigma of 0.02
 O10-O11 \\sim O10A-O11A
 with sigma of 0.04
 Cl1-O7 \\sim Cl1A-O7A
 with sigma of 0.02
 Cl1-O8 \\sim Cl1A-O8A
 with sigma of 0.02
 Cl2-O10 \\sim Cl2A-O10A
 with sigma of 0.02
 Cl2-O11 \\sim Cl2A-O11A
 with sigma of 0.02
 O10-O12 \\sim O10A-O12A
 with sigma of 0.04
 Cl2-O9 \\sim Cl2A-O9A
 with sigma of 0.02
 Cl2-O12 \\sim Cl2A-O12A
 with sigma of 0.02
 O10-O9 \\sim O10A-O9A
 with sigma of 0.04
 O11-O12 \\sim O11A-O12A
 with sigma of 0.04
 O9-O12 \\sim O9A-O12A
 with sigma of 0.04
 O6-O7 \\sim O6A-O7A
 with sigma of 0.04
 O5-O8 \\sim O5A-O8A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O5-O7 \\sim O5A-O7A
 with sigma of 0.04
 O6-O8 \\sim O6A-O8A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.02 within 2A
4. Rigid body (RIGU) restrains
 O5A, Cl1A, O6A, O7A, O8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, Cl1, O6, O7, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9A, Cl2A, O10A, O11A, O12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O10, Cl2, O11, O9, O12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl2A)=Sof(O10A)=Sof(O11A)=Sof(O9A)=Sof(O12A)=1-FVAR(1)
 Sof(Cl2)=Sof(O10)=Sof(O11)=Sof(O9)=Sof(O12)=FVAR(1)
 Sof(Cl1A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(2)
 Sof(Cl1)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C17(H17), C24(H24), 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:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              53920
_olex2_submission_special_instructions 'No special instructions were received'