Metallosupramolecular poly[2]pseudorotaxane constructed by metal coordination and crown-ether-based molecular recognition.
Wei, Peifa; Li, Jinying; Yan, Xuzhou; Zhou, Qizhong; Organic letters 16 (2014) 126–129; doi:10.1021/ol403111e

data_1513558
_publ_section_title
;
 Metallosupramolecular poly[2]pseudorotaxane constructed by metal
 coordination and crown-ether-based molecular recognition.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              126
_journal_page_last               129
_journal_paper_doi               10.1021/ol403111e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
;
C42 H50 N2 O14, C24 H16 N4, F6 P, CH3 CN, C6 H14 O
;
_chemical_formula_sum            'C74 H83 F6 N7 O15 P'
_chemical_formula_weight         1455.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2525(15)
_cell_length_b                   26.897(2)
_cell_length_c                   16.0354(11)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.7138
_cell_measurement_theta_min      2.8900
_cell_volume                     8303.7(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21689
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.9627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1199P)^2^+0.3535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                5146
_reflns_number_total             7589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol403111e_si_002.cif
_cod_data_source_block           121108_yxz_h4g13
_cod_original_cell_volume        8303.8(12)
_cod_original_sg_symbol_Hall     '-P 2n 2ab '
_cod_database_code               1513558