Ion-Pairing Crystal Polymorphs of Interlocked [2 + 1]-Type Receptor-Anion Complexes.
Yamakado, Ryohei; Sato, Ryuma; Shigeta, Yasuteru; Maeda, Hiromitsu; The Journal of organic chemistry 81 (2016) 8530–8536; doi:10.1021/acs.joc.6b01688

data_4037195
_publ_section_title
;
 Ion-Pairing Crystal Polymorphs of Interlocked [2 + 1]-Type Receptor-Anion
 Complexes.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8530
_journal_page_last               8536
_journal_paper_doi               10.1021/acs.joc.6b01688
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         '2(C35 H31 B F4 N2 O2), C16 H36 N, Cl'
_chemical_formula_sum            'C86 H98 B2 Cl F8 N5 O4'
_chemical_formula_weight         1474.76
_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                108.335(12)
_cell_angle_beta                 101.007(4)
_cell_angle_gamma                90.798(4)
_cell_formula_units_Z            2
_cell_length_a                   13.613(2)
_cell_length_b                   17.506(5)
_cell_length_c                   17.927(5)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      25.36
_cell_volume                     3968.1(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            102998
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.344
_diffrn_reflns_theta_min         6.567
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         14279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.7506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12676
_reflns_number_total             14279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01688_si_002.cif
_cod_data_source_block           60217m4
_cod_database_code               4037195
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              80421
_shelx_hkl_checksum              21131