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_7203297
_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. 4.5(C6 H7 N). 0.5(H2O)'
_chemical_formula_sum            'C103 H120.5 N4.5 O16.5 S4'
_chemical_formula_weight         1813.78
_chemical_melting_point          209.9
_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. 4.5(3-picoline). 0.5(H2O) clathrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.2390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   44.8472(3)
_cell_length_b                   20.7901(2)
_cell_length_c                   23.3348(2)
_cell_measurement_reflns_used    71620
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.02
_cell_volume                     19344.1(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69690
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'clear blocks'
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         22846
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.898
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1162P)^2^+55.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2447
_reflns_number_gt                14370
_reflns_number_total             22846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601560c.txt
_cod_data_source_block           H.4.5(3PIC).0.5(H2O)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C103 H120.50 N4.50 O16.50 S4'
_cod_database_code               7203297