Synthesis of Water-Soluble Deep-Cavity Cavitands.
Hillyer, Matthew B.; Gibb, Corinne L. D.; Sokkalingam, Punidha; Jordan, Jacobs H.; Ioup, Sarah E.; Mague, Joel T.; Gibb, Bruce C.; Organic letters 18 (2016) 4048–4051; doi:10.1021/acs.orglett.6b01903

data_1555664
_publ_section_title
;
 Synthesis of Water-Soluble Deep-Cavity Cavitands.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4048
_journal_page_last               4051
_journal_paper_doi               10.1021/acs.orglett.6b01903
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C100 H72.78 Br8 Cl10.5 O15.5'
_chemical_formula_weight         2533.86
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.481(4)
_cell_angle_beta                 100.258(3)
_cell_angle_gamma                92.601(4)
_cell_formula_units_Z            4
_cell_length_a                   19.082(5)
_cell_length_b                   19.769(5)
_cell_length_c                   29.220(8)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.109
_cell_measurement_theta_min      2.17
_cell_volume                     10834(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents
;
Value not automatically inserted upon CIF generation
due to twinned crystal used.
;
_diffrn_reflns_av_unetI/netI     0.1697
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_number            30838
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        23.357
_diffrn_reflns_theta_max         23.357
_diffrn_reflns_theta_min         0.708
_exptl_absorpt_coefficient_mu    3.279
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             5021
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.120
_refine_diff_density_max         6.710
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2473
_refine_ls_number_reflns         30838
_refine_ls_number_restraints     1753
_refine_ls_restrained_S_all      1.784
_refine_ls_R_factor_all          0.2500
_refine_ls_R_factor_gt           0.1494
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3563
_refine_ls_wR_factor_ref         0.3799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14356
_reflns_number_total             30838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01903_si_002.cif
_cod_data_source_block           bcg008_0m_4_sq
_cod_original_formula_sum        'C100 H72.78 Br8 Cl10.50 O15.50'
_cod_database_code               1555664
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.385
_shelx_estimated_absorpt_t_max   0.694
_shelx_res_checksum              60557
_shelx_hkl_checksum              98663
_shelx_fab_checksum              48138