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_7700136
_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
'0.5(C64 H64 Cl4 Co4 N8 O16), C36 H36 N24 O12, 1.6(H2 O), 2.4(O)'
_chemical_formula_sum            'C68 H76 Cl2 Co2 N28 O24'
_chemical_formula_weight         1858.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-09
_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                 110.087(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.256(5)
_cell_length_b                   19.149(5)
_cell_length_c                   14.830(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.313
_cell_measurement_theta_min      3.043
_cell_volume                     3802(2)
_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 0.983
_diffrn_measured_fraction_theta_max 0.982
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38328
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         3.043
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_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    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0524P)^2^+3.3327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7844
_reflns_number_total             9304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01544b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7700136--7700138.cif.'
_cod_database_code               7700136
_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
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4W) \\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: O1W(0.8) H1WA(0.8) H1WB(0.8) O2W(0.4) O3W(0.4) O4W(0.4)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27), C23(H23), C22(H22)
4.c Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), C7(H7A,H7B), C20(H20A,H20B), C8(H8A,H8B), C32(H32A,H32B),
 C30(H30A,H30B), C6(H6A,H6B), C34(H34A,H34B), C28(H28A,H28B), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C11(H11), C1(H1), C2(H2), C14(H14), C5(H5), C12(H12)
;
_shelx_res_checksum              76030
_olex2_submission_special_instructions 'No special instructions were received'