Synthesis of a Triptycene-Derived Bisparaphenylene-34-crown-10 and Its Complexation with Both Paraquat and Cyclobis(paraquat-p-phenylene)
Yi Jiang; Jing Cao; Jian-Min Zhao; Jun-Feng Xiang; Chuan-Feng Chen; Journal of Organic Chemistry 75 (2010) 1767–1770; doi:10.1021/jo902571n

data_4025270
_publ_section_title
;
 Synthesis of a Triptycene-Derived Bisparaphenylene-34-crown-10 and Its
 Complexation with Both Paraquat and Cyclobis(paraquat-p-phenylene)
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1767
_journal_page_last               1770
_journal_paper_doi               10.1021/jo902571n
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C70 H72 Cl6 F12 N2 O10 P2'
_chemical_formula_weight         1603.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.497(2)
_cell_length_b                   18.213(4)
_cell_length_c                   21.191(6)
_cell_measurement_reflns_used    10687
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.0
_cell_volume                     3864.5(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear(Rigaku/MSC Inc., 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30812
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0199(19)
_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   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6810
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.1358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+35.1555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3211
_refine_ls_wR_factor_ref         0.3261
_reflns_number_gt                5854
_reflns_number_total             6810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902571n_si_002.cif
_cod_data_source_block           r90409g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3864.5(16)
_cod_database_code               4025270