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_7125449
_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             2019-11-13
_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                 106.85(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.45(2)
_cell_length_b                   16.983(9)
_cell_length_c                   18.105(14)
_cell_measurement_reflns_used    1378
_cell_measurement_temperature    240
_cell_measurement_theta_max      47.40
_cell_measurement_theta_min      20.91
_cell_volume                     9549(11)
_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      240.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25289
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        59.328
_diffrn_reflns_theta_max         59.328
_diffrn_reflns_theta_min         2.846
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1102 before and 0.0852 after correction. The Ratio of minimum to maximum transmission is 0.8514. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.896
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2098 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(7)
_refine_ls_extinction_coef       0.00039(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   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         12584
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0839P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.820
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                6911
_reflns_number_total             12584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09063k2.cif
_cod_data_source_block           1CH3OH_240K
_cod_depositor_comments
'Adding full bibliography for 7125447--7125452.cif.'
_cod_original_cell_volume        9550(11)
_cod_database_code               7125449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.830
_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
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 O5-C75
 1.45 with sigma of 0.02
 C75-O6
 1.45 with sigma of 0.02
 O4-C74
 1.45 with sigma of 0.02
 O6-C76
 1.45 with sigma of 0.02
 C75-C76
 2.3 with sigma of 0.04
 C76-C75
 2.3 with sigma of 0.04
3. Rigid bond restraints
 O8, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C75
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq,
Uanis(C76) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B)
5.b Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C74(H74A,H74B,H74C)
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:
 C72(H72A,H72B,H72C), C78(H78A,H78B,H78C), B1(H1A,H1B,H1C), B2(H2A,H2B,H2C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 774.6 electrons were found in a volume of 3486.9\%A^3 in 1-CH^3^OH-240K void. This is consistent with the presence of about 10.5[CH3OH ] per formula unit which account for 756.0 electrons.
;
_shelx_res_checksum              68587
_shelx_fab_checksum              95683
_olex2_submission_special_instructions 'No special instructions were received'