Unraveling the Structure-Affinity Relationship between Cucurbit[n]urils (n = 7, 8) and Cationic Diamondoids.
Sigwalt, David; Šekutor, Marina; Cao, Liping; Zavalij, Peter Y.; Hostaš, Jiří; Ajani, Haresh; Hobza, Pavel; Mlinarić-Majerski, Kata; Glaser, Robert; Isaacs, Lyle; Journal of the American Chemical Society 139 (2017) 3249–3258; doi:10.1021/jacs.7b00056

data_4125666
_publ_section_title
;
 Unraveling the Structure-Affinity Relationship between Cucurbit[n]urils
 (n = 7, 8) and Cationic Diamondoids.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3249
_journal_page_last               3258
_journal_paper_doi               10.1021/jacs.7b00056
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'(C48 H48 N32 O16), (C14 H24 N2), (Cl0.5 I1.5), 9.5(H2 O)'
_chemical_formula_sum            'C62 H111 Cl0.5 I1.5 N34 O35.5'
_chemical_formula_weight         2108.92
_chemical_name_common            'CB8 Diadamantane 2,6-diammonium'
_chemical_name_systematic
;
CB8 Diadamantane 2,6-diammonium iodide chloride hydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.455(3)
_cell_length_b                   25.742(3)
_cell_length_c                   13.1609(15)
_cell_measurement_reflns_used    26053
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.2
_cell_volume                     8962.6(18)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-2012
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0343157
_diffrn_orient_matrix_UB_12      0.0034226
_diffrn_orient_matrix_UB_13      0.0311645
_diffrn_orient_matrix_UB_21      -0.0130433
_diffrn_orient_matrix_UB_22      0.0154942
_diffrn_orient_matrix_UB_23      -0.0645398
_diffrn_orient_matrix_UB_31      -0.0090136
_diffrn_orient_matrix_UB_32      -0.0354608
_diffrn_orient_matrix_UB_33      -0.0252423
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            71375
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.208
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4372
_exptl_crystal_id                'Isaacs-Xu CB8 150K'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Removed electron density corresponds to 56 water 
molecules per unit cell
;
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0100P)^2^+49.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6855
_reflns_number_total             7845
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'See _shelx_res_file'
_cod_data_source_file            ja7b00056_si_002.cif
_cod_data_source_block           2348
_cod_original_cell_volume        8962.5(18)
_cod_original_formula_sum        'C62 H111 Cl0.50 I1.50 N34 O35.5'
_cod_database_code               4125666
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.915
_diffrn_reflns_sigmai/neti       0.0304