Iterative Synthesis of Oligo[n]rotaxanes in Excellent Yield.
Lewis, James E. M.; Winn, Joby; Cera, Luca; Goldup, Stephen M.; Journal of the American Chemical Society 138 (2016) 16329–16336; doi:10.1021/jacs.6b08958

data_4131055
_publ_section_title
;
 Iterative Synthesis of Oligo[n]rotaxanes in Excellent Yield.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16329
_journal_page_last               16336
_journal_paper_doi               10.1021/jacs.6b08958
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C60 H69 N5 O2'
_chemical_formula_weight         892.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.617(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3026(18)
_cell_length_b                   12.7660(9)
_cell_length_c                   19.7821(10)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0430
_cell_measurement_theta_min      2.6860
_cell_volume                     5205.6(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23808
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         2.143
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.68326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       Block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.779
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         8854
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.784
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.1243
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3919
_refine_ls_wR_factor_ref         0.4787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5518
_reflns_number_total             8854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08958_si_003.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4131055
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              7821
_shelx_hkl_checksum              2786