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_7117720
_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            'C166 H205 F30 N8 O26 P5'
_chemical_formula_weight         3453.22
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-05 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                65.6220(10)
_cell_angle_beta                 74.3130(10)
_cell_angle_gamma                66.014(2)
_cell_formula_units_Z            2
_cell_length_a                   20.5486(17)
_cell_length_b                   21.3959(19)
_cell_length_c                   24.984(2)
_cell_measurement_reflns_used    9467
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.19
_cell_volume                     9071.3(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63342
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.838
_diffrn_reflns_theta_min         0.902
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             3620
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_platon_squeeze_details          ' '
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2071
_refine_ls_number_reflns         38333
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.1115
_refine_ls_shift/su_max          0.004
_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          0.3021
_refine_ls_wR_factor_ref         0.3579
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                15936
_reflns_number_total             38333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05623c2.cif
_cod_data_source_block           mo_40930a
_cod_original_cell_volume        9071.2(13)
_cod_database_code               7117720
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-2
_shelx_res_checksum              78104