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_7700137
_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
'0.25(C136 H120 Co8 N16 O48), C36 H36 N24 O12, 2(H O), 5(H2 O)'
_chemical_formula_sum            'C70 H80 Co2 N28 O31'
_chemical_formula_weight         1927.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.034(5)
_cell_length_b                   14.409(5)
_cell_length_c                   27.801(5)
_cell_measurement_reflns_used    6877
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.064
_cell_measurement_theta_min      2.954
_cell_volume                     7625(4)
_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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16951
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.064
_diffrn_reflns_theta_max         25.064
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.877
_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    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.014
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.1019
_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^)+(0.0250P)^2^+77.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4603
_reflns_number_total             6476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01544b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7700136--7700138.cif.'
_cod_database_code               7700137
_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) groups, All O(H,H) groups
2. Restrained distances
 N1-C1 \\sim C2-C3 \\sim C4-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O1W(0.85) H1WA(0.85) H1WB(0.85) O3W(0.65) H3WA(0.65) H3WB(0.65)
5.a Riding coordinates:
 O4W(H4W), O2W(H2WA,H2WB), O1W(H1WA,H1WB), O3W(H3WA,H3WB)
5.b Ternary CH refined with riding coordinates:
 C26(H26), C28(H28), C27(H27), C30(H30), C25(H25), C29(H29)
5.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C24(H24A,H24B), C8(H8A,H8B), C18(H18A,H18B), C6(H6A,H6B),
 C34(H34A,H34B), C7(H7A,H7B), C32(H32A,H32B), C22(H22A,H22B), C20(H20A,H20B)
5.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C5(H5), C13(H13), C2(H2), C11(H11), C1(H1)
;
_shelx_res_checksum              74128
_olex2_submission_special_instructions 'No special instructions were received'