Synthesis of a D3 Symmetric Trefoil Knotted Cyclophane
Karla I. Arias; Eli Zysman-Colman; Jon C. Loren; Anthony Linden; Jay S. Siegel; Chem.Commun. 47 (2011) 9588–; doi:10.1039/c1cc11209k

data_7106778
_publ_section_title
;
 Synthesis of a D3 Symmetric Trefoil Knotted Cyclophane
;
_journal_name_full               Chem.Commun.
_journal_page_first              9588
_journal_paper_doi               10.1039/c1cc11209k
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C168 H132 Cu3 F18 N12 O6 P3'
_chemical_formula_sum            'C168 H132 Cu3 F18 N12 O6 P3'
_chemical_formula_weight         3040.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           218
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      218
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             06-03-10
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.7312(6)
_cell_length_b                   33.7312(6)
_cell_length_c                   33.7312(6)
_cell_measurement_reflns_used    308743
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.0
_cell_volume                     38379.2(12)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 '65 mm CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4511
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            162826
_diffrn_reflns_theta_full        21.95
_diffrn_reflns_theta_max         21.95
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             12528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), ? Friedel pairs'
_refine_ls_abs_structure_Flack   0.48(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7819
_refine_ls_number_restraints     498
_refine_ls_restrained_S_all      2.152
_refine_ls_R_factor_all          0.3009
_refine_ls_R_factor_gt           0.2080
_refine_ls_shift/su_max          0.202
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4008
_refine_ls_wR_factor_ref         0.4291
_reflns_number_gt                4112
_reflns_number_total             7819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c1cc11209k.txt
_cod_data_source_block           SG0613
_cod_original_cell_volume        38379.1(12)
_cod_original_sg_symbol_H-M      'P -4 3 n '
_cod_database_code               7106778