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_4107956
_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_absolute_configuration ad
_chemical_formula_moiety         'C10 H12 N8 O4, 5(C2 H F3 O2)'
_chemical_formula_sum            'C20 H17 F15 N8 O14'
_chemical_formula_weight         878.42
_chemical_name_common            CB2.5CF3COOH
_chemical_name_systematic
;
CB2.5CF3COOH
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.8769(3)
_cell_length_b                   12.8191(4)
_cell_length_c                   29.5359(9)
_cell_measurement_reflns_used    5901
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.1
_cell_volume                     3361.00(19)
_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      223(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      586,443,458
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
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_diffrn_orient_matrix_UB_12      0.0178742
_diffrn_orient_matrix_UB_13      0.0327317
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_diffrn_orient_matrix_UB_22      0.0155476
_diffrn_orient_matrix_UB_23      0.0022823
_diffrn_orient_matrix_UB_31      -0.0199720
_diffrn_orient_matrix_UB_32      0.0743252
_diffrn_orient_matrix_UB_33      -0.0083508
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
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_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.68
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_id                'Isaacs/Huang - dimmer  CB2'
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_coef       0.0035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         7659
_refine_ls_number_restraints     1012
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_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^+1.53P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.772
_reflns_number_gt                6778
_reflns_number_total             7659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8013693-file003.cif
_cod_data_source_block           1306
_cod_database_code               4107956
_diffrn_measurement_total_frames-ccd 1487
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.958
_diffrn_measurement_frame_time-ccd 13
_diffrn_measurement_total_time-ccd 8.32
_diffrn_measurement_frame_size-ccd 512