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_7125274
_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_sum            'C130 H130 N10'
_chemical_formula_weight         1832.43
_chemical_name_systematic        PC3-pseudorotaxane-SQUEEZE
_space_group_crystal_system      cubic
_space_group_IT_number           212
_space_group_name_Hall           'P 4acd 2ab 3'
_space_group_name_H-M_alt        'P 43 3 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   36.9585(19)
_cell_length_b                   36.9585(19)
_cell_length_c                   36.9585(19)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      2.27
_cell_volume                     50483(4)
_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      230(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.2119
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            326554
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         25.056
_diffrn_reflns_theta_min         1.232
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.042
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2016'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.723
_exptl_crystal_description       block
_exptl_crystal_F_000             11760
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
 PLATON/Squeeze was carried out for poorly defined ion pair and
 possibly solvent. Solvent accessible area per unit cell is 
 21236 Angstr^3 with (42% per unit cell) with electron count of 
 6563 which is consistent with the presence of TBA+ [PO4(C3H3)2]- 
 ion pair.
;
_refine_ls_abs_structure_Flack   0.8(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.587
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         14940
_refine_ls_number_restraints     2235
_refine_ls_restrained_S_all      1.536
_refine_ls_R_factor_all          0.1646
_refine_ls_R_factor_gt           0.1118
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2719
_refine_ls_wR_factor_ref         0.2950
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8451
_reflns_number_total             14940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08113d2.cif
_cod_data_source_block           16062_sq
_cod_original_cell_volume        50483(8)
_cod_database_code               7125274
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              28169
_shelx_hkl_checksum              79729
_shelx_fab_checksum              15420