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_4107958
_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         'C28 H30 N20 O10, C1.70 F2.55 O1.70'
_chemical_formula_sum            'C38.9 H38 F16.35 N20 O24.9'
_chemical_formula_weight         1494.74
_chemical_name_common            '[CB5<0.85TFA]*4.6TFA*4H2O'
_chemical_name_systematic
;
Semi-circle CB5 trifluoroacetic acid hydrate, CB5*5.45TFA*4H2O
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   11.662(4)
_cell_length_b                   33.042(11)
_cell_length_c                   14.952(5)
_cell_measurement_reflns_used    9031
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      2.2
_cell_volume                     5762(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      606,606,606
_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      -0.0261928
_diffrn_orient_matrix_UB_12      -0.0283561
_diffrn_orient_matrix_UB_13      0.0109349
_diffrn_orient_matrix_UB_21      -0.0457782
_diffrn_orient_matrix_UB_22      0.0003996
_diffrn_orient_matrix_UB_23      -0.0565067
_diffrn_orient_matrix_UB_31      0.0675586
_diffrn_orient_matrix_UB_32      -0.0105950
_diffrn_orient_matrix_UB_33      -0.0340458
_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  0.1058
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28204
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.72
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    not-measur
_exptl_crystal_description       prism
_exptl_crystal_F_000             3031
_exptl_crystal_id                'Isaacs/Huang Ser from T/H in T xtal-2 - b'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.062
_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     326
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0854
_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^)+(0.002P)^2^+18.7P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                2830
_reflns_number_total             3824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8013693-file005.cif
_cod_data_source_block           1426b
_cod_original_formula_sum        'C38.90 H38 F16.35 N20 O24.90'
_cod_database_code               4107958
_diffrn_measurement_total_frames-ccd 1818
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.939
_diffrn_measurement_frame_time-ccd 38
_diffrn_measurement_total_time-ccd 22.80
_diffrn_measurement_frame_size-ccd 512