A high-yield synthesis and acid-base response of phosphate-templated [3]rotaxanes.
Qiao, Bo; Liu, Yun; Lee, Semin; Pink, Maren; Flood, Amar H.; Chemical communications (Cambridge, England) 52 (2016) 13675–13678; doi:10.1039/c6cc08113d

data_7125273
_publ_section_title
;
 A high-yield synthesis and acid-base response of phosphate-templated
 [3]rotaxanes.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13675
_journal_page_last               13678
_journal_paper_doi               10.1039/c6cc08113d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'2(C65 H65 N5), [(C14 H14 N3 O4)]2 O4 P, C16 H36 N, 6(C H Cl3)'
_chemical_formula_sum            'C180 H200 Cl18 N17 O12 P'
_chemical_formula_weight         3462.63
_chemical_name_systematic        TBA-C4-[3]Rotaxane
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-07 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.7191(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.3787(16)
_cell_length_b                   19.6365(10)
_cell_length_c                   32.742(3)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.54
_cell_volume                     18386(2)
_computing_cell_refinement       'APEX II v2014.11-0 (Bruker, 2014)'
_computing_data_collection       'APEX II v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'APEX II v2014.11-0 (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX (Bruker, 2014)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
'0.50 degree frames measured for 60 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            61341
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.258
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2016'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             7264
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.230
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1304
_refine_ls_number_reflns         20734
_refine_ls_number_restraints     3206
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.1781
_refine_ls_R_factor_gt           0.1234
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2500P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3704
_refine_ls_wR_factor_ref         0.4377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12081
_reflns_number_total             20734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08113d2.cif
_cod_data_source_block           16070
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7125273
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              2546
_shelx_hkl_checksum              16651