Cyclic [2]Pseudorotaxane Tetramers Consisting of Two Rigid Rods Threaded through Two Bis-Macrocycles: Copper(I)-Templated Synthesis and X-ray Structure Studies
Julien Frey; Christian Tock; Jean-Paul Collin; Valérie Heitz; Jean-Pierre Sauvage; Kari Rissanen; Journal of the American Chemical Society 130 (2008) 11013–11022; doi:10.1021/ja801924y

data_4108194
_publ_contact_author_address
;Nanoscience Center
Department of Chemistry
University of Jyv\"askyl\"a
P.O. Box 35
FIN-40014 University of Jyv\"askyl\"a
Finland
;
_publ_contact_author_email       kari.rissanen@jyu.fi
_publ_contact_author_fax         358(14)2602651
_publ_contact_author_name        'Kari Rissanen'
_publ_contact_author_phone       358(14)2602672
_publ_section_title
;
 Cyclic [2]Pseudorotaxane Tetramers Consisting of Two Rigid Rods Threaded
 through Two Bis-Macrocycles: Copper(I)-Templated Synthesis and X-ray
 Structure Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11013
_journal_page_last               11022
_journal_paper_doi               10.1021/ja801924y
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C245 H218 Cl8 Cu4 F24 N20 O32 P4'
_chemical_formula_sum            'C245 H218 Cl8 Cu4 F24 N20 O32 P4'
_chemical_formula_weight         5072.09
_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             2008-02-20T16:44:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.311(1)
_cell_angle_beta                 66.573(1)
_cell_angle_gamma                64.109(1)
_cell_formula_units_Z            1
_cell_length_a                   18.4923(2)
_cell_length_b                   19.6458(4)
_cell_length_c                   20.4339(4)
_cell_measurement_reflns_used    163648
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     6074.0(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.325486E-1
_diffrn_orient_matrix_UB_12      0.569941E-1
_diffrn_orient_matrix_UB_13      0.70355E-2
_diffrn_orient_matrix_UB_21      -0.390416E-1
_diffrn_orient_matrix_UB_22      -0.9459E-3
_diffrn_orient_matrix_UB_23      0.503925E-1
_diffrn_orient_matrix_UB_31      0.42029E-1
_diffrn_orient_matrix_UB_32      0.30432E-2
_diffrn_orient_matrix_UB_33      0.175059E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35500
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.55
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       prism
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1579
_refine_ls_number_reflns         21336
_refine_ls_number_restraints     1779
_refine_ls_restrained_S_all      11.585
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.1149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1706P)^2^+22.4624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3003
_refine_ls_wR_factor_ref         0.3531
_reflns_number_gt                13695
_reflns_number_total             21336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801924y-file002.cif
_cod_data_source_block           Cu_Rotanaxe
_cod_database_code               4108194