Synthesis and Self-Assembly Processes of Monofunctionalized Cucurbit[7]uril
Brittany Vinciguerra; Liping Cao; Joe R. Cannon; Peter Y. Zavalij; Catherine Fenselau; Lyle Isaacs; Journal of the American Chemical Society 134 (2012) 13133–13140; doi:10.1021/ja3058502

data_4118492
_publ_section_title
;
 Synthesis and Self-Assembly Processes of Monofunctionalized
 Cucurbit[7]uril
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13133
_journal_page_last               13140
_journal_paper_doi               10.1021/ja3058502
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'(C44 H46 N28 O14), (C8 H14 N2), I2, 11(H2 O)'
_chemical_formula_sum            'C52 H80 I2 N30 O25'
_chemical_formula_weight         1779.26
_chemical_name_common            Me2CB7*DAA*I2.nH2O
_chemical_name_systematic
;
Me2CB7*DAA*I2.nH2O
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.750(4)
_cell_length_b                   49.017(8)
_cell_length_c                   13.018(2)
_cell_measurement_reflns_used    41211
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.2
_cell_volume                     15155(4)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      0.0160241
_diffrn_orient_matrix_UB_12      -0.0159230
_diffrn_orient_matrix_UB_13      -0.0183979
_diffrn_orient_matrix_UB_21      -0.0056014
_diffrn_orient_matrix_UB_22      0.0384731
_diffrn_orient_matrix_UB_23      -0.0081643
_diffrn_orient_matrix_UB_31      0.0749216
_diffrn_orient_matrix_UB_32      0.0062628
_diffrn_orient_matrix_UB_33      0.0033284
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            104851
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       prism
_exptl_crystal_F_000             7264
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_platon_squeeze_details
; 1457 electrons per unit cell corresponds to 12 I- ions and about 82 water
molecules.
;
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         13325
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0762
_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^)+(0.05P)^2^+49.67P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                10588
_reflns_number_total             13325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3058502_si_002.cif
_cod_data_source_block           2261
_cod_original_cell_volume        15154(4)
_cod_database_code               4118492