Three-dimensional bis(m-phenylene)-32-crown-10-based cryptand/paraquat catenanes
Liu, Ming; Li, Shijun; Zhang, Mingming; Zhou, Qizhong; Wang, Feng; Hu, Menglong; Fronczek, Frank R.; Li, Ning; Huang, Feihe; Organic & Biomolecular Chemistry 7 (2009) 1288–1291; doi:10.1039/B815929G

data_7150560
_publ_section_title
;
 Three-dimensional bis(m-phenylene)-32-crown-10-based cryptand/paraquat
 catenanes
;
_journal_issue                   7
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1288
_journal_page_last               1291
_journal_paper_doi               10.1039/B815929G
_journal_volume                  7
_journal_year                    2009
_chemical_formula_moiety
'C36 H53.925 I0.075 O15, C36 H32 N4, 4(F6 P), 5(C2 H3 N), H2 O'
_chemical_formula_sum            'C82 H102.925 F24 I0.075 N9 O16 P4'
_chemical_formula_weight         2060.06
_chemical_melting_point          525(2)
_chemical_name_common
;Bis(m-phenylene)-32-crown-10-Based Cryptand/Paraquat
(2)Catenane
;
_chemical_name_systematic
;
Bis(m-phenylene)-32-crown-10-Based Cryptand/Paraquat [2]Catenane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.665(4)
_cell_angle_beta                 81.887(4)
_cell_angle_gamma                74.949(5)
_cell_formula_units_Z            2
_cell_length_a                   13.9005(15)
_cell_length_b                   14.0323(11)
_cell_length_c                   26.137(2)
_cell_measurement_reflns_used    37989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.6
_cell_volume                     4753.9(7)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       '\w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30619
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2132.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.135
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         17056
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1437P)^2^+15.6290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2500
_refine_ls_wR_factor_ref         0.2700
_reflns_number_gt                12674
_reflns_number_total             17056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B815929G.txt
_cod_data_source_block           4
_cod_database_code               7150560