Designed Synthesis of Metal Cluster-Centered Pseudo-Rotaxane Supramolecular Architectures
Cai-Yan Gao; Liang Zhao; Mei-Xiang Wang; Journal of the American Chemical Society 133 (2011) 8448–8451; doi:10.1021/ja202294v

data_4106203
_publ_section_title
;
 Designed Synthesis of Metal Cluster-Centered Pseudo-Rotaxane
 Supramolecular Architectures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8448
_journal_page_last               8451
_journal_paper_doi               10.1021/ja202294v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C128 H108 Ag8 F18 N32 O18 S6'
_chemical_formula_weight         3779.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                99.56(3)
_cell_angle_beta                 107.48(3)
_cell_angle_gamma                91.06(3)
_cell_formula_units_Z            2
_cell_length_a                   17.278(4)
_cell_length_b                   18.822(4)
_cell_length_c                   27.281(6)
_cell_measurement_reflns_used    21079
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3483
_cell_measurement_theta_min      1.5911
_cell_volume                     8323(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            67241
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6124
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Block
_exptl_crystal_F_000             3756
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0.00111(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1852
_refine_ls_number_reflns         30133
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0946
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2633
_refine_ls_wR_factor_ref         0.2912
_reflns_number_gt                19062
_reflns_number_total             30133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202294v_si_002_2.cif
_cod_data_source_block           Py8CCPhCCPhCCPhCC
_cod_original_cell_volume        8323(3)
_cod_database_code               4106203