Templated Synthesis of Cyclic [4]Rotaxanes Consisting of Two Stiff Rods Threaded through Two Bis-macrocycles with a Large and Rigid Central Plate as Spacer
Jean-Paul Collin; Fabien Durola; Julien Frey; Valérie Heitz; Felipe Reviriego; Jean-Pierre Sauvage; Yann Trolez; Kari Rissanen; Journal of the American Chemical Society 132 (2010) 6840–6850; doi:10.1021/ja101759w

data_4102402
_publ_section_title
;
 Templated Synthesis of Cyclic [4]Rotaxanes Consisting of Two Stiff Rods
 Threaded through Two Bis-macrocycles with a Large and Rigid Central Plate
 as Spacer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6840
_journal_page_last               6850
_journal_paper_doi               10.1021/ja101759w
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C524 H534 Cu4 F24 N52 O30 P4 Zn2'
_chemical_formula_sum            'C524 H534 Cu4 F24 N52 O30 P4 Zn2'
_chemical_formula_weight         9004.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2010-01-14T09:50:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.843(5)
_cell_angle_beta                 79.695(6)
_cell_angle_gamma                73.704(6)
_cell_formula_units_Z            1
_cell_length_a                   15.9812(19)
_cell_length_b                   27.908(4)
_cell_length_c                   34.355(4)
_cell_measurement_reflns_used    77366
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      50.436
_cell_measurement_theta_min      0.883
_cell_measurement_wavelength     0.71073
_cell_volume                     13829(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.752
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.487331E-1
_diffrn_orient_matrix_UB_12      -0.172169E-1
_diffrn_orient_matrix_UB_13      0.28715E-2
_diffrn_orient_matrix_UB_21      -0.33125E-1
_diffrn_orient_matrix_UB_22      0.324845E-1
_diffrn_orient_matrix_UB_23      -0.191427E-1
_diffrn_orient_matrix_UB_31      0.284383E-1
_diffrn_orient_matrix_UB_32      -0.131013E-1
_diffrn_orient_matrix_UB_33      -0.241439E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.2611
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36398
_diffrn_reflns_theta_full        50
_diffrn_reflns_theta_max         50
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4734
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2695
_refine_ls_number_reflns         21362
_refine_ls_number_restraints     4153
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.2505
_refine_ls_R_factor_gt           0.122
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3031
_refine_ls_wR_factor_ref         0.357
_reflns_number_gt                5573
_reflns_number_total             21362
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja101759w_si_001.cif
_cod_data_source_block           comp2
_cod_database_code               4102402