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_4107959
_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         'C34 H36 N24 O12'
_chemical_formula_sum            'C34 H60 Cl2 N24 O23'
_chemical_formula_weight         1243.96
_chemical_name_common            'CB6 hydrate'
_chemical_name_systematic
;
CB6 hydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   24.119(2)
_cell_length_b                   12.8676(13)
_cell_length_c                   31.795(3)
_cell_measurement_reflns_used    6864
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      20.3
_cell_measurement_theta_min      2.1
_cell_volume                     9867.7(16)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      306,606,209,260
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0084257
_diffrn_orient_matrix_UB_12      -0.0040966
_diffrn_orient_matrix_UB_13      -0.0307582
_diffrn_orient_matrix_UB_21      0.0146805
_diffrn_orient_matrix_UB_22      0.0727245
_diffrn_orient_matrix_UB_23      0.0007482
_diffrn_orient_matrix_UB_31      0.0378659
_diffrn_orient_matrix_UB_32      -0.0272032
_diffrn_orient_matrix_UB_33      0.0065989
_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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51174
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.56
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       ball
_exptl_crystal_F_000             5200
_exptl_crystal_id                'Isaacs/WHHuang CB6 not-cycle in H2O, MeOH'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.047
_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     631
_refine_ls_number_reflns         6402
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0565
_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^+13.15P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                3874
_reflns_number_total             6402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8013693-file006.cif
_cod_data_source_block           1513
_cod_original_cell_volume        9867.6(17)
_cod_database_code               4107959
_diffrn_measurement_total_frames-ccd 1381
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.950
_diffrn_measurement_frame_time-ccd 38
_diffrn_measurement_total_time-ccd 17.3
_diffrn_measurement_frame_size-ccd 512