A homochiral 3D framework of mechanically interlocked 1D loops with solvent-dependent spin-state switching behaviors.
Sun, Xiao-Peng; Tang, Zheng; Yao, Zi-Shuo; Tao, Jun; Chemical communications (Cambridge, England) 56 (2020) 133–136; doi:10.1039/c9cc09063k

data_7125448
_publ_section_title
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 A homochiral 3D framework of mechanically interlocked 1D loops with
 solvent-dependent spin-state switching behaviors.
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_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              133
_journal_page_last               136
_journal_paper_doi               10.1039/c9cc09063k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C78 H62 B2 Fe N6 O8'
_chemical_formula_sum            'C78 H62 B2 Fe N6 O8'
_chemical_formula_weight         1288.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-15 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.009(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.761(8)
_cell_length_b                   16.907(4)
_cell_length_c                   18.032(4)
_cell_measurement_reflns_used    1222
_cell_measurement_temperature    240
_cell_measurement_theta_max      46.98
_cell_measurement_theta_min      2.81
_cell_volume                     9600(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      239.99
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22811
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        51.248
_diffrn_reflns_theta_max         51.248
_diffrn_reflns_theta_min         2.549
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1197 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.8155.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.892
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 1146 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.100(10)
_refine_ls_extinction_coef       0.00013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         9053
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2429
_reflns_Friedel_coverage         0.711
_reflns_Friedel_fraction_full    0.755
_reflns_Friedel_fraction_max     0.755
_reflns_number_gt                4305
_reflns_number_total             9053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09063k2.cif
_cod_data_source_block           1CH3CN_240K
_cod_depositor_comments
'Adding full bibliography for 7125447--7125452.cif.'
_cod_database_code               7125448
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.843
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O5-C49
 1.45 with sigma of 0.01
 B2-C2
 1.6 with sigma of 0.02
 C1-B1
 1.6 with sigma of 0.02
 O8A-C77
 1.45 with sigma of 0.02
 O8A-C78A
 1.45 with sigma of 0.02
 C75-O5
 1.45 with sigma of 0.02
 O1-C71
 1.45 with sigma of 0.02
 C71-O2
 1.45 with sigma of 0.02
 O2-C72
 1.45 with sigma of 0.02
 C74-O4
 1.45 with sigma of 0.02
 O6B-C76
 1.45 with sigma of 0.02
 O6A-C76
 1.45 with sigma of 0.02
 O6A-C75
 1.45 with sigma of 0.02
 O6B-C75
 1.45 with sigma of 0.02
 O8B-C77
 1.45 with sigma of 0.02
 O8B-C78B
 1.45 with sigma of 0.02
 C72-C71
 2.3 with sigma of 0.04
 C76-C75
 2.3 with sigma of 0.04
 O5-O6B
 2.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C76 \\sim O6A \\sim O6B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C76) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(O2) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(O6B) \\sim Ueq, Uanis(B1)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C78B)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(O8B)=1-FVAR(1)
 Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(O8A)=FVAR(1)
 Fixed Sof: H75A(0.35) H75B(0.35) H75C(0.65) H75D(0.65) H76A(0.35) H76B(0.35)
 H76C(0.35) H76D(0.65) H76E(0.65) H76F(0.65) H77A(0.7) H77B(0.7) H77C(0.3)
 H77D(0.3) O6A(0.5) O6B(0.5)
 Fixed Uiso: C78A(0.26017) C78B(0.26947) C72(0.3612)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C73(H73A,H73B), C75(H75A,H75B), C75(H75C,H75D), C77(H77A,
 H77B), C77(H77C,H77D)
5.b Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C76(H76D,H76E,H76F), C72(H72A,H72B,H72C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C18(H18),
 C19(H19), C22(H22), C23(H23), C25(H25), C27(H27), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C45(H45),
 C47(H47), C48(H48), C52(H52), C53(H53), C56(H56), C57(H57), C59(H59), C61(H61),
  C62(H62), C67(H67), C68(H68), C69(H69), C70(H70)
5.d Idealised Me refined as rotating group:
 B2(H2A,H2B,H2C), C74(H74A,H74B,H74C), C78A(H78A,H78B,H78C), C78B(H78D,H78E,
 H78F), B1(H1A,H1B,H1C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 728.0 electrons were found in a volume of 3412.3 \%A^3 in 1-CH^3^CN-240K void. This is consistent with the presence of 8[CH3CN ] per formula unit which account for 704.0 electrons.
;
_shelx_res_checksum              97
_shelx_fab_checksum              5612
_olex2_submission_special_instructions 'No special instructions were received'