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_7203298
_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. 6.5(C6H7N). 2(H2O)'
_chemical_formula_sum            'C112 H130 N6 O16 S4'
_chemical_formula_weight         1944.46
_chemical_melting_point          211.4
_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. 6.5(4-picoline). 2(H2O) 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                104.4950(10)
_cell_angle_beta                 96.6710(10)
_cell_angle_gamma                105.44
_cell_formula_units_Z            2
_cell_length_a                   16.93660(10)
_cell_length_b                   17.9477(2)
_cell_length_c                   19.4997(2)
_cell_measurement_reflns_used    89710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.02
_cell_volume                     5424.44(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46049
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'clear plates'
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1238
_refine_ls_number_reflns         25436
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+5.6155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                16716
_reflns_number_total             25436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601560c.txt
_cod_data_source_block           H.6.5(4PIC).2(H2O)
_cod_original_cell_volume        5424.27(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203298