A [2]rota[2]catenane, constructed from a pillar[5]arene-crown ether fused double-cavity macrocycle: synthesis and structural characterization
Wei-Bo Hu; Wen-Jing Hu; Xiao-Li Zhao; Yahu A. Liu; Jiu-Sheng Li; Biao Jiang; Ke Wen; Chem.Commun. 51 (2015) 13882–; doi:10.1039/C5cc05623C

data_7117719
_publ_section_title
;
 A [2]rota[2]catenane, constructed from a pillar[5]arene-crown ether fused
 double-cavity macrocycle: synthesis and structural characterization
;
_journal_name_full               Chem.Commun.
_journal_page_first              13882
_journal_paper_doi               10.1039/C5cc05623C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C105 H113 F27 N4 O18 P4.5'
_chemical_formula_weight         2371.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-05 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                71.1160(10)
_cell_angle_beta                 78.710(2)
_cell_angle_gamma                76.663(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1777(6)
_cell_length_b                   20.5414(9)
_cell_length_c                   24.6430(10)
_cell_measurement_temperature    173(2)
_cell_volume                     6549.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1041
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            76514
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.9366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2451
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1429
_refine_ls_number_reflns         22945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1707
_refine_ls_R_factor_gt           0.1070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1905P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2908
_refine_ls_wR_factor_ref         0.3280
_reflns_number_gt                10204
_reflns_number_total             22945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc05623c2.cif
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C105 H113 F27 N4 O18 P4.50'
_cod_database_code               7117719