Self-sorting of crown ether/secondary ammonium ion hetero-[c2]daisy chain pseudorotaxanes
Zheng, Bo; Klautzsch, Fabian; Xue, Min; Huang, Feihe; Schalley, Christoph A.; Org. Chem. Front. 1 (2014) 532–; doi:10.1039/C4QO00064A

data_1552984
_publ_section_title
;
 Self-sorting of crown ether/secondary ammonium ion hetero-[c2]daisy chain
 pseudorotaxanes
;
_journal_issue                   5
_journal_name_full               'Org. Chem. Front.'
_journal_page_first              532
_journal_paper_doi               10.1039/C4QO00064A
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C39 H46 N O10, F6 P' 
_chemical_formula_sum            'C39 H46 F6 N O10 P'
_chemical_formula_weight         833.73
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 113.902(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.4663(3)
_cell_length_b                   42.4866(16)
_cell_length_c                   25.4339(9)
_cell_measurement_reflns_used    9106
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      67.4873
_cell_measurement_theta_min      2.8151
_cell_volume                     10339.9(7)
_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      140(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_sigmaI/netI    0.1127
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36086
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.7937
_exptl_absorpt_correction_T_min  0.7292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.348
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         13857
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.1859
_refine_ls_R_factor_gt           0.1501
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3841
_refine_ls_wR_factor_ref         0.4125
_reflns_number_gt                8431
_reflns_number_total             13857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qo00064a2.cif
_cod_data_source_block           130301_zb_188
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H90 F12 N2 O20 P2'
_cod_original_formula_weight         1665.46
_cod_original_formula_moiety
;
C39 H46 N O10, C39 H44 N O10, 2(F6 P) 
;
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10339.9(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1552984