Mono- and Dihydroxylated Symmetrical Octamethylcucurbiturils and Allylated Derivatives.
Shen, Fang-Fang; Chen, Kai; Zhang, Yun-Qian; Zhu, Qian-Jiang; Tao, Zhu; Cong, Hang; Organic letters 18 (2016) 5544–5547; doi:10.1021/acs.orglett.6b02789

data_1555874
_publ_section_title
;
 Mono- and Dihydroxylated Symmetrical Octamethylcucurbiturils and
 Allylated Derivatives.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5544
_journal_page_last               5547
_journal_paper_doi               10.1021/acs.orglett.6b02789
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C66 H138 N36 O51'
_chemical_formula_weight         2252.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                83.660(3)
_cell_angle_beta                 83.950(3)
_cell_angle_gamma                82.860(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4005(17)
_cell_length_b                   12.7258(18)
_cell_length_c                   34.039(5)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.31
_cell_volume                     5274.4(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            35427
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_platon_squeeze_details
'                                                '
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         18609
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0979
_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^)+(0.1758P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2804
_refine_ls_wR_factor_ref         0.3018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10551
_reflns_number_total             18609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02789_si_003.cif
_cod_data_source_block           B
_cod_original_cell_volume        5274.3(13)
_cod_database_code               1555874
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              16035
_shelx_hkl_checksum              98385