Observation of face-to-face host-guest associated states prior to threading of dialkylammonium ions into the DB24C8-like openings of a molecular cage
Chun-Ju Chuang; Ming-Liang Yen; Chien-Chen Lai; Yi-Hung Liu; Shie-Ming Penga; Sheng-Hsien Chiu; Chem.Commun. 49 (2013) 4199–; doi:10.1039/c2cc34669a

data_7109180
_publ_section_title
;
 Observation of face-to-face host-guest associated states prior to
 threading of dialkylammonium ions into the DB24C8-like openings of a
 molecular cage
;
_journal_name_full               Chem.Commun.
_journal_page_first              4199
_journal_paper_doi               10.1039/c2cc34669a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C84 H111 F12 N3 O18 P2'
_chemical_formula_weight         1740.70
_chemical_name_systematic
;
?
;
_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                 115.059(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.0161(3)
_cell_length_b                   15.12550(10)
_cell_length_c                   24.3838(3)
_cell_measurement_reflns_used    21649
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.9595
_cell_measurement_theta_min      3.2105
_cell_volume                     9026.1(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49844
_diffrn_reflns_theta_full        67.99
_diffrn_reflns_theta_max         67.99
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.461
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1176
_refine_ls_number_reflns         16439
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1745
_refine_ls_R_factor_gt           0.1497
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+48.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3483
_refine_ls_wR_factor_ref         0.3669
_reflns_number_gt                12992
_reflns_number_total             16439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34669a.txt
_cod_data_source_block           ic14788
_cod_original_cell_volume        9026.11(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7109180