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_7205158
_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         '2(C52 H64 N8 O12 S4), H2 O, 2(C4 H8 0)'
_chemical_formula_sum            'C112 H146 N16 O27 S8'
_chemical_formula_weight         2404.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.281(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.9385(5)
_cell_length_b                   25.0431(8)
_cell_length_c                   15.9995(5)
_cell_measurement_reflns_used    6785
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      2.46
_cell_volume                     5984.0(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37926
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
During the refinement, except for the symmetry-disordered
water O13 molecule being assigned, the other potential
THF molecules are disordered and the refinement gave
very unstable thermal factors. 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 640.2 \%A^3^ volumes in the unit
cell (approximately 152 electrons, i.e. ca. 4 THF
molecules based on the solvents we have used and each host molecule was
distributed one THF . So the suitable formula should be
C~52~H~64~N~8~O~12~S~4~. 0.5(H~2~O).(C~4~ H~8~O).
Some related items (i.e. D(calc), F000 & Mol.Wght ) have
been added in the cif file.
;
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         10509
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1494
_reflns_number_gt                7690
_reflns_number_total             10509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00129E.TXT
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7205158