Syntheses and magnetic properties of high-dimensional cucurbit[6]uril-based metal-organic rotaxane frameworks.
Wu, Xue-Song; Bao, Hong-Fei; Zhu, Fu-Long; Sun, Jing; Wang, Xin-Long; Su, Zhong-Min; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9939–9943; doi:10.1039/c9dt01544b

data_7700138
_publ_section_title
;
 Syntheses and magnetic properties of high-dimensional
 cucurbit[6]uril-based metal-organic rotaxane frameworks.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9939
_journal_page_last               9943
_journal_paper_doi               10.1039/c9dt01544b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C23 H19 Co N2 O6, C18 H18 N12 O6'
_chemical_formula_sum            'C41 H57 Co N14 O22'
_chemical_formula_weight         1156.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.949(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.868(5)
_cell_length_b                   14.824(5)
_cell_length_c                   25.364(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.086
_cell_measurement_theta_min      2.528
_cell_volume                     5207(3)
_computing_cell_refinement       'APEX2(Bruker, 2005)'
_computing_data_collection       'APEX2(Bruker, 2005)'
_computing_data_reduction        'SAINT(Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'Shelxl2014 (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41404
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.086
_diffrn_reflns_theta_max         25.086
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0521
_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^)+(0.1046P)^2^+3.8460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7560
_reflns_number_total             9162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01544b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7700136--7700138.cif.'
_cod_database_code               7700138
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Rigid bond restraints
 O3, Co1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C41(H41), C38(H38), C39(H39), C40(H40), C43(H43), C42(H42)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C23(H23A,H23B), C22(H22A,H22B), C34(H34A,H34B), C32(H32A,H32B),
 C26(H26A,H26B), C24(H24A,H24B), C36(H36A,H36B), C30(H30A,H30B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C13(H13), C9(H9), C7(H7), C4(H4), C21(H21), C3(H3),
 C17(H17), C19(H19), C18(H18)
;
_shelx_res_checksum              34825
_shelx_fab_checksum              30440
_olex2_submission_special_instructions 'No special instructions were received'