A Shape-Persistent Cryptand for Capturing Polycyclic Aromatic Hydrocarbons.
Zhang, Rui-Feng; Hu, Wen-Jing; Liu, Yahu A.; Zhao, Xiao-Li; Li, Jiu-Sheng; Jiang, Biao; Wen, Ke; The Journal of organic chemistry 81 (2016) 5649–5654; doi:10.1021/acs.joc.6b01115

data_4036980
_publ_section_title
;
 A Shape-Persistent Cryptand for Capturing Polycyclic Aromatic
 Hydrocarbons.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5649
_journal_page_last               5654
_journal_paper_doi               10.1021/acs.joc.6b01115
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C73 H60 Cl6 N10 O10'
_chemical_formula_weight         1450.01
_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-2013
_cell_angle_alpha                65.263(3)
_cell_angle_beta                 87.570(3)
_cell_angle_gamma                73.367(3)
_cell_formula_units_Z            2
_cell_length_a                   14.259(3)
_cell_length_b                   18.033(3)
_cell_length_c                   20.014(4)
_cell_measurement_reflns_used    3452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.21
_cell_measurement_theta_min      2.36
_cell_volume                     4460.7(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31844
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.125
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_platon_squeeze_details          ' '
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.0026(9)
_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   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         19268
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.2215
_refine_ls_R_factor_gt           0.1377
_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^)+(0.2000P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3548
_refine_ls_wR_factor_ref         0.4050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7738
_reflns_number_total             19268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01115_si_001.cif
_cod_data_source_block           mo_50330b
_cod_original_cell_volume        4460.8(14)
_cod_database_code               4036980
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-2
_shelx_res_checksum              89448
_shelx_hkl_checksum              31824