Reactions of thiacalix[4]arene 1,3-bistriflate: formation of thiacalix[2]phenoxathiins—structural and complexation studies
Habashneh, Almeqdad; Jablonski, Chester R.; Collins, Julie; Georghiou, Paris E.; New Journal of Chemistry 32 (2008) 1590–; doi:10.1039/b801483c

data_7051954
_publ_section_title
;
 Reactions of thiacalix[4]arene 1,3-bistriflate: formation of
 thiacalix[2]phenoxathiins---structural and complexation studies
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1590
_journal_paper_doi               10.1039/b801483c
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C41 H47 F3 O5 S5'
_chemical_formula_weight         837.09
_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                61.816(9)
_cell_angle_beta                 75.573(13)
_cell_angle_gamma                81.851(13)
_cell_formula_units_Z            2
_cell_length_a                   10.9907(13)
_cell_length_b                   14.3416(11)
_cell_length_c                   15.5658(8)
_cell_measurement_reflns_used    8694
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      2.2
_cell_volume                     2093.6(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure 3.7.0'
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20163
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.9325
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1077P)^2^+2.5511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2403
_reflns_number_gt                7249
_reflns_number_total             8573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801483c.txt
_cod_data_source_block           shelxl2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2093.6(3)
_cod_database_code               7051954