Acyclic CB[n]-type molecular containers: effect of solubilizing group on their function as solubilizing excipients.
Zhang, Ben; Zavalij, Peter Y.; Isaacs, Lyle; Organic & biomolecular chemistry 12 (2014) 2413–2422; doi:10.1039/c3ob42603c

data_7153674
_publ_section_title
;
 Acyclic CB[n]-type molecular containers: effect of solubilizing group on
 their function as solubilizing excipients.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2413
_journal_page_last               2422
_journal_paper_doi               10.1039/c3ob42603c
_journal_volume                  12
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C50 H68 N20 O12,  4(Cl),  13.14(H2 O)'
_chemical_formula_sum            'C50 H94.28 Cl4 N20 O25.14'
_chemical_formula_weight         1519.77
_chemical_name_common            '[CB4(Ph(OC2H4NH3)2)2]Cl4.nH2O'
_chemical_name_systematic
;
[CB4(Ph(OC2H4NH3)2)2]Cl4.nH2O
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 92.5526(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7177(10)
_cell_length_b                   27.048(2)
_cell_length_c                   18.9817(14)
_cell_measurement_reflns_used    48774
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.3
_cell_volume                     7035.9(9)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-2012
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0720287
_diffrn_orient_matrix_UB_12      0.0005402
_diffrn_orient_matrix_UB_13      -0.0060845
_diffrn_orient_matrix_UB_21      -0.0013918
_diffrn_orient_matrix_UB_22      0.0369520
_diffrn_orient_matrix_UB_23      -0.0013993
_diffrn_orient_matrix_UB_31      0.0116052
_diffrn_orient_matrix_UB_32      0.0010648
_diffrn_orient_matrix_UB_33      0.0523641
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            118279
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.276
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3214
_exptl_crystal_id                'Isaacs-BenZhang AH-BZ 150K'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1686
_refine_ls_number_reflns         39291
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0100P)^2^+9.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                34631
_reflns_number_total             39291
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'See _shelx_res_file'
_cod_data_source_file            c3ob42603c3.cif
_cod_data_source_block           2349
_cod_database_code               7153674
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.955
_diffrn_reflns_sigmai/neti       0.0463