Pendant orientation and its influence on the formation of hydrogen-bonded thiacalixarene nanotubes
Li, Yan; Yang, Weiping; Chen, Yuanyin; Gong, Shuling; CrystEngComm 13 (2011) 259–; doi:10.1039/c0ce00129e

data_7205159
_publ_section_title
;
 Pendant orientation and its influence on the formation of
 hydrogen-bonded thiacalixarene nanotubes
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              259
_journal_paper_doi               10.1039/c0ce00129e
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
'C51 H62 N6 O12 S4, 1.17 (CH3OH), 0.67 (CH2Cl2)'
_chemical_formula_sum            'C52.84 H68.02 Cl1.34 N6 O13.17 S4'
_chemical_formula_weight         1173.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   20.3779(12)
_cell_length_b                   20.3779(12)
_cell_length_c                   76.563(9)
_cell_measurement_reflns_used    3518
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.84
_cell_measurement_theta_min      2.19
_cell_volume                     27534(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1200
_diffrn_reflns_av_sigmaI/netI    0.1373
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            46006
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             11131
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
During the refinement, the potential methanol and
dichloromethane molecules are seriously disordered.
During the final refinement, the contribution of the solvent
molecules to the crystal structure is treated by using the
Platon/SQUEEZE procedure. Check using platon shows
that there are 4446.0 \%A^3^ volumes in the unit
cell (approximately 871 electrons, i.e. ca. 21 methanol
and 12 CH~2~Cl~2~ molecules based on the solvents
we have used and each host molecule was distributed 1.17
methanol and 0.67 CH~2~Cl~2~ molecules). So the suitable
formula should be
C~51~ H~62~ N~6~ O~12~ S~4.(MeOH)~1.17~.(CH~2~Cl~2~)~0.67~.
Some related items (i.e. D(calc), F000 & Mol.Wght ) have
been added in the cif file.
;
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         10797
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                4278
_reflns_number_total             10797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00129E.TXT
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C52.84 H68.02 N6 O13.17 S4 Cl1.34'
_cod_database_code               7205159