Cucurbit[n]uril Formation Proceeds by Step-Growth Cyclo-oligomerization
Wei-Hao Huang; Peter Y. Zavalij; Lyle Isaacs; Journal of the American Chemical Society 130 (2008) 8446–8454; doi:10.1021/ja8013693

data_4107957
_publ_section_title
;
 Cucurbit[n]uril Formation Proceeds by Step-Growth Cyclo-oligomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8446
_journal_page_last               8454
_journal_paper_doi               10.1021/ja8013693
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C44 H48 N32 Na O17, 4(C2 F3 O2)'
_chemical_formula_sum            'C58 H56 F21 N32 Na O31'
_chemical_formula_weight         2119.34
_chemical_name_common            Na*2CB4*H2O*7TFA
_chemical_name_systematic
;
Na*2CB4*H2O*7TFA
;
_space_group_IT_number           84
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c'
_symmetry_space_group_name_H-M   'P 42/m'
_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            2
_cell_length_a                   18.6306(8)
_cell_length_b                   18.6306(8)
_cell_length_c                   15.2173(12)
_cell_measurement_reflns_used    4859
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      2.4
_cell_volume                     5281.9(5)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      366,366,366,726
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'catus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0508870
_diffrn_orient_matrix_UB_12      0.0002146
_diffrn_orient_matrix_UB_13      -0.0209239
_diffrn_orient_matrix_UB_21      -0.0066772
_diffrn_orient_matrix_UB_22      -0.0496397
_diffrn_orient_matrix_UB_23      0.0236003
_diffrn_orient_matrix_UB_31      -0.0157268
_diffrn_orient_matrix_UB_32      0.0204250
_diffrn_orient_matrix_UB_33      0.0576565
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25719
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.09
_diffrn_source_current           40
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152
_exptl_crystal_id                'Isaacs tetramer CB4 none-cyclic'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         2590
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0779
_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^)+(0.02P)^2^+29.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                2044
_reflns_number_total             2590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8013693-file004.cif
_cod_data_source_block           1407
_cod_database_code               4107957
_diffrn_measurement_total_frames-ccd 1824
_diffrn_measurement_frame_width-ccd 0.5
_diffrn_detector_distance-ccd    4.939
_diffrn_measurement_frame_time-ccd 38
_diffrn_measurement_total_time-ccd 22.88
_diffrn_measurement_frame_size-ccd 512