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_7150561
_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 H54 O15, 0.5(C48 H40 N4), 2(F6 P), 5(C2 H3 N), 5(H2 O)'
_chemical_formula_sum            'C70 H99 F12 N7 O20 P2'
_chemical_formula_weight         1648.50
_chemical_melting_point          537(2)
_chemical_name_common
;Bis(m-phenylene)-32-crown-10-Based Cryptand/Paraquat
(3)Catenane
;
_chemical_name_systematic
;
Bis(m-phenylene)-32-crown-10-Based Cryptand/Paraquat [3]Catenane
;
_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                 92.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.196(4)
_cell_length_b                   14.757(3)
_cell_length_c                   28.726(6)
_cell_measurement_reflns_used    77143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     8552(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62628
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
The PLATON/SQUEEZE was used to remove the contributions of disordered
water molecules, leaving two large voids at the coordinates of
(1.000, -0.069, 0.250) and (1.000, -0.026, 0.750) with the same
volumes of 617 \%A^3^. 80 electrons were effectively removed in each
void, which corresponds with 16 water molecules in the unit cell, or
4 per asymmetric unit. After L.S.-convergence, a proper final FCF file
was produced by running PLATON/CALC FCF.
;
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         15437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0832P)^2^+3.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1528
_reflns_number_gt                11651
_reflns_number_total             15437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B815929G.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7150561