Construction of Hetero[n]rotaxanes by Use of Polyfunctional Rotaxane Frameworks
Ziyong Li; Guoxing Liu; Wen Xue; Di Wu; Ying-Wei Yang; Jishan Wu; Sheng Hua Liu; Juyoung Yoon; Jun Yin; Journal of Organic Chemistry 78 (2013) 11560–11570; doi:10.1021/jo402166y

data_4028768
_publ_section_title
;
 Construction of Hetero[n]rotaxanes by Use of Polyfunctional Rotaxane
 Frameworks
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11560
_journal_page_last               11570
_journal_paper_doi               10.1021/jo402166y
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C44 H68 F12 N2 O16 P2'
_chemical_formula_weight         1170.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.062(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.013(5)
_cell_length_b                   27.362(16)
_cell_length_c                   25.684(14)
_cell_measurement_reflns_used    3965
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.22
_cell_volume                     5411(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1126
_diffrn_reflns_av_sigmaI/netI    0.1142
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32763
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9814
_exptl_absorpt_correction_T_min  0.9633
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.253
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.439
_refine_ls_extinction_coef       0.40(4)
_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   2.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.209
_refine_ls_R_factor_all          0.2784
_refine_ls_R_factor_gt           0.2424
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.014
_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          0.5717
_refine_ls_wR_factor_ref         0.5830
_reflns_number_gt                6026
_reflns_number_total             9500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402166y_si_001.cif
_cod_data_source_block           e:\120411g\work\mo_120411g_0m
_cod_original_cell_volume        5411(5)
_cod_original_sg_symbol_H-M      'P 1 21/n 1'
_cod_database_code               4028768