Three Protocols for the Formation of a [3]Pseudorotaxane via Orthogonal Cryptand-Based Host-Guest Recognition and Coordination-Driven Self-Assembly.
Li, Jinying; Wei, Peifa; Wu, Xiujuan; Xue, Min; Yan, Xuzhou; Organic letters 15 (2013) 4984–4987; doi:10.1021/ol402294q

data_1512361
_publ_section_title
;
 Three Protocols for the Formation of a [3]Pseudorotaxane via Orthogonal
 Cryptand-Based Host-Guest Recognition and Coordination-Driven
 Self-Assembly.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              4984
_journal_page_last               4987
_journal_paper_doi               10.1021/ol402294q
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C37 H45 N O14, C14 H12 N2, 2(F6 P)'
_chemical_formula_sum            'C51 H57 F12 N3 O14 P2'
_chemical_formula_weight         1225.94
_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                 90.764(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3728(11)
_cell_length_b                   10.8964(6)
_cell_length_c                   25.8063(16)
_cell_measurement_reflns_used    4463
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.5172
_cell_measurement_theta_min      2.9706
_cell_volume                     6009.4(6)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25170
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.9269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
;
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+4.4242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2672
_refine_ls_wR_factor_ref         0.2939
_reflns_number_gt                6904
_reflns_number_total             10978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402294q_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512361