Acyclic Cucurbit[n]uril Congeners Are High Affinity Hosts
Da Ma; Peter Y. Zavalij; Lyle Isaacs; Journal of Organic Chemistry 75 (2010) 4786–4795; doi:10.1021/jo100760g

data_4025537
_publ_section_title
;
 Acyclic Cucurbit[n]uril Congeners Are High Affinity Hosts
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4786
_journal_page_last               4795
_journal_paper_doi               10.1021/jo100760g
_journal_volume                  75
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C50 H52 N16 O20, C10 H30 N4, 4(C2 F3 O2), 7(C2 H F3 O2), 2(H2 O)'
_chemical_formula_sum            'C82 H93 F33 N20 O44'
_chemical_formula_weight         2689.76
_chemical_name_common            Ph2CB4@tetra-ammonium
_chemical_name_systematic
;
Ph2CB4@tetra-ammonium
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 121.6142(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.448(3)
_cell_length_b                   23.608(3)
_cell_length_c                   19.660(2)
_cell_measurement_reflns_used    32335
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.3
_cell_volume                     10849(2)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      366,366,366,720
_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      0.0076273
_diffrn_orient_matrix_UB_12      0.0373846
_diffrn_orient_matrix_UB_13      -0.0165339
_diffrn_orient_matrix_UB_21      -0.0411776
_diffrn_orient_matrix_UB_22      0.0027275
_diffrn_orient_matrix_UB_23      -0.0435205
_diffrn_orient_matrix_UB_31      -0.0087324
_diffrn_orient_matrix_UB_32      0.0197208
_diffrn_orient_matrix_UB_33      0.0374115
_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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66440
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.02
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       prism
_exptl_crystal_F_000             5496
_exptl_crystal_id                'Isaacs/Ma Me-Host spermine CB4@C2Ph(OR)2'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1988
_refine_ls_number_reflns         24400
_refine_ls_number_restraints     1089
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0412
_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^)+(0.01P)^2^+13.945P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.959
_reflns_number_gt                21942
_reflns_number_total             24400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo100760g_si_004.cif
_cod_data_source_block           1817
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        10850(2)
_cod_database_code               4025537
_diffrn_measurement_frame_width-ccd -0.5
_diffrn_measurement_total_frames-ccd 1818
_diffrn_measurement_frame_time-ccd 20
_diffrn_measurement_total_time-ccd 13.1
_diffrn_detector_distance-ccd    5.800
_diffrn_measurement_frame_size-ccd 512