Selective enclathration of picoline isomers by a resorcinarene host
Caira, Mino R.; le Roex, Tanya; Nassimbeni, Luigi R.; CrystEngComm 8 (2006) 275–; doi:10.1039/b601560c

data_7203296
_publ_section_title
;
 Selective enclathration of picoline isomers by a resorcinarene host
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              275
_journal_paper_doi               10.1039/b601560c
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C76 H88 O16 S4. 5(C6 H7 N)'
_chemical_formula_sum            'C106 H123 N5 O16 S4'
_chemical_formula_weight         1851.33
_chemical_melting_point          213.1
_chemical_name_common            none
_chemical_name_systematic
;
1^4^,1^6^,5^4^,5^6^-tetrahydroxy-2,4,6,8-tetrapentyl-3^4^,3^6^,7^4^,7^6^-
tetra(p-toluenesulfonyl-oxy)
-1,3,5,7(1,3)-tetrabenzenacyclooctaphane.5(2-picoline) clathrate
;
_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
_cell_angle_alpha                77.8920(10)
_cell_angle_beta                 86.0920(10)
_cell_angle_gamma                83.9360(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6878(2)
_cell_length_b                   16.3438(3)
_cell_length_c                   22.3279(5)
_cell_measurement_reflns_used    73118
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.02
_cell_volume                     4851.11(16)
_computing_cell_refinement       'Collect (Nonius, 2000)'
_computing_data_collection       'Collect (Nonius, 2000)'
_computing_data_reduction        'Collect (Nonius, 2000)'
_computing_molecular_graphics
'XSEED, a graphical interface to SHELX (1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'combination of phi and omega'
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            72434
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9517
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'clear plates'
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         21799
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+4.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                14737
_reflns_number_total             21799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601560c.txt
_cod_data_source_block           H.5(2PIC)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203296