Synthesis, Structure, and Dynamic Properties of Hybrid Organic-Inorganic Rotaxanes
Beatriz Ballesteros; Thomas B. Faust; Chin-Fa Lee; David A. Leigh; Christopher A. Muryn; Robin G. Pritchard; David Schultz; Simon J. Teat; Grigore A. Timco; Richard E. P. Winpenny; Journal of the American Chemical Society 132 (2010) 15435–15444; doi:10.1021/ja1074773

data_4103426
_publ_section_title
;
 Synthesis, Structure, and Dynamic Properties of Hybrid Organic-Inorganic
 Rotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15435
_journal_page_last               15444
_journal_paper_doi               10.1021/ja1074773
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C106.50 H200.50 Cr7 Cu F8 N3 O36.50'
_chemical_formula_sum            'C106.5 H200.5 Cr7 Cu F8 N3 O36.5'
_chemical_formula_weight         2686.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-06-16T07:54:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.2490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8601(2)
_cell_length_b                   32.0521(4)
_cell_length_c                   28.4030(5)
_cell_measurement_reflns_used    21269
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     15306.8(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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 Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.557157E-1
_diffrn_orient_matrix_UB_12      0.10912E-1
_diffrn_orient_matrix_UB_13      0.27979E-2
_diffrn_orient_matrix_UB_21      0.190526E-1
_diffrn_orient_matrix_UB_22      -0.271025E-1
_diffrn_orient_matrix_UB_23      0.141402E-1
_diffrn_orient_matrix_UB_31      0.83692E-2
_diffrn_orient_matrix_UB_32      -0.109442E-1
_diffrn_orient_matrix_UB_33      -0.322276E-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  0.0745
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24595
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        20
_diffrn_reflns_theta_max         20
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5686
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1450
_refine_ls_number_reflns         13942
_refine_ls_number_restraints     2487
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.15
_refine_ls_R_factor_gt           0.091
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+85.8786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2423
_reflns_number_gt                8496
_reflns_number_total             13942
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1074773_si_011.cif
_cod_data_source_block           rob
_cod_original_cell_volume        15306.7(4)
_cod_original_formula_sum        'C106.50 H200.50 Cr7 Cu F8 N3 O36.50'
_cod_database_code               4103426