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_4103423
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C107 H203.25 Cr7 F8 N3 Ni O37.25'
_chemical_formula_sum            'C107 H203.25 Cr7 F8 N3 Ni O37.25'
_chemical_formula_weight         2702.69
_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      2.3
_audit_creation_date             2009-09-14T17:47:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.122(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4959(8)
_cell_length_b                   31.4557(15)
_cell_length_c                   28.2556(13)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     14623.6(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            95939
_diffrn_reflns_theta_full        21
_diffrn_reflns_theta_max         21
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_correction_T_min  0.7665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (2008),
 Bruker AXS area detector scaling and absorption corection program
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5729
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1512
_refine_ls_number_reflns         12047
_refine_ls_number_restraints     2854
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+124.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                11475
_reflns_number_total             12047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1074773_si_008.cif
_cod_data_source_block           robin
_cod_database_code               4103423