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_7125447
_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     dual
_audit_creation_date             2019-11-08
_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                 104.814(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.9544(10)
_cell_length_b                   16.4618(5)
_cell_length_c                   17.8159(5)
_cell_measurement_reflns_used    3992
_cell_measurement_temperature    100
_cell_measurement_theta_max      49.95
_cell_measurement_theta_min      2.86
_cell_volume                     9060.1(5)
_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      99.71
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.1163
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21892
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        50.626
_diffrn_reflns_theta_max         50.626
_diffrn_reflns_theta_min         2.861
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.8577.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.945
_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         0.249
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1402 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.091(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1064P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1967
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                5183
_reflns_number_total             8855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09063k2.cif
_cod_data_source_block           1CH3CN_100K
_cod_depositor_comments
'Adding full bibliography for 7125447--7125452.cif.'
_cod_database_code               7125447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.835
_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
 O8B-C77
 1.45 with sigma of 0.02
 O8A-C77
 1.45 with sigma of 0.02
 O6B-C76
 1.5 with sigma of 0.02
 O6A-C76
 1.5 with sigma of 0.02
 O8A-C78A
 1.45 with sigma of 0.02
 O8B-C78B
 1.45 with sigma of 0.02
 C78A-C77
 2.3 with sigma of 0.02
 C78B-C77
 2.3 with sigma of 0.04
3. Rigid bond restraints
 C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C75, O6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C76, O6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(O8B)=Sof(C78B)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(1)
 Sof(O8A)=Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(H78C)=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(0.35) O6B(0.65)
 Fixed Uiso: C78A(0.26017) C78B(0.26947)
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)
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), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), B1(H1A,H1B,H1C),
 C78A(H78A,H78B,H78C), C78B(H78D,H78E,H78F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 668.0 electrons were found in a volume of 2944.9\%A^3 in 1-CH^3^CN-100K void. This is consistent with the presence of 7.5[CH3CN ] per formula unit which account for 660.0 electrons.
;
_shelx_res_checksum              26371
_shelx_fab_checksum              79643
_olex2_submission_special_instructions 'No special instructions were received'