Synthesis, Complexation, and Supramolecular Assembly of 21,30-Dithia-17,25-dimethyl-1,4,7,10,13- pentaoxa[13.3.3](1,2,6)cyclophane†
Xu, Jianwei; Lai, Yee-Hing; Organic Letters 4 (2002) 3211–; doi:10.1021/ol026374+

data_1517199
_publ_section_title
;
 Synthesis, Complexation, and Supramolecular Assembly of
 21,30-Dithia-17,25-dimethyl-1,4,7,10,13-
 pentaoxa[13.3.3](1,2,6)cyclophane&#x2020;
;
_journal_issue                   19
_journal_name_full               'Organic Letters'
_journal_page_first              3211
_journal_paper_doi               10.1021/ol026374+
_journal_volume                  4
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_sum            'C26 H34 O5 S2'
_chemical_formula_weight         490.65
_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
_cell_angle_alpha                89.227(1)
_cell_angle_beta                 85.947(1)
_cell_angle_gamma                83.901(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1151(1)
_cell_length_b                   10.0902(3)
_cell_length_c                   13.9221(4)
_cell_measurement_reflns_used    2957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.03
_cell_volume                     1270.00(5)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames \w 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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.4233
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal plates'
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0048(26)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.154
_refine_ls_hydrogen_treatment
;
riding models
;
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.154
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_obs          0.0715
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1889
_refine_ls_wR_factor_obs         0.1698
_reflns_number_observed          2626
_reflns_number_total             4196
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ol026374%2B_s1.cif
_cod_data_source_block           lai9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1270.01(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517199