[3]Rotaxanes and [3]pseudorotaxanes with a rigid two-bidentate chelate axle threaded through two coordinating rings
Collin, Jean-Paul; Sauvage, Jean-Pierre; Trolez, Yann; Rissanen, Kari; New Journal of Chemistry 33 (2009) 2148–; doi:10.1039/b9nj00278b

data_7054131
_publ_section_title
;
 [3]Rotaxanes and [3]pseudorotaxanes with a rigid two-bidentate chelate
 axle threaded through two coordinating rings
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2148
_journal_paper_doi               10.1039/b9nj00278b
_journal_volume                  33
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C116 H130 Cu2 F12 N6 O14 P2 Si2'
_chemical_formula_sum            'C123.5 H142 Cu2 F12 N8 O17 P2 Si2'
_chemical_formula_weight         2483.65
_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             2009-04-22T10:13:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.490(2)
_cell_angle_beta                 88.660(2)
_cell_angle_gamma                74.205(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3567(7)
_cell_length_b                   20.1482(7)
_cell_length_c                   26.9262(10)
_cell_measurement_reflns_used    13156
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     6509.7(5)
_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      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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      -0.661786E-1
_diffrn_orient_matrix_UB_12      -0.88871E-2
_diffrn_orient_matrix_UB_13      -0.90749E-2
_diffrn_orient_matrix_UB_21      -0.216226E-1
_diffrn_orient_matrix_UB_22      0.506929E-1
_diffrn_orient_matrix_UB_23      -0.277676E-1
_diffrn_orient_matrix_UB_31      0.352958E-1
_diffrn_orient_matrix_UB_32      -0.200477E-1
_diffrn_orient_matrix_UB_33      -0.270002E-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  0.0532
_diffrn_reflns_av_unetI/netI     0.1202
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25576
_diffrn_reflns_theta_full        22.5
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.13
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.45
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2598
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1509
_refine_ls_number_reflns         16719
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.218
_refine_ls_R_factor_gt           0.1327
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_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          0.3318
_refine_ls_wR_factor_ref         0.379
_reflns_number_gt                7862
_reflns_number_total             16719
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b9nj00278b.txt
_cod_data_source_block           jps005
_cod_original_cell_volume        6509.8(5)
_cod_original_formula_sum        'C123.50 H142 Cu2 F12 N8 O17 P2 Si2'
_cod_database_code               7054131