25-Decyloxy-26,27,28-trihydroxy-5,11,17-tris(4-nitrophenyldiazenyl)-2,8,14,20-thiacalix[4]arene toluene hemisolvate
Kasyan, Oleg; Kalchenko, Vitaly; Böhmer, Volker; Bolte, Michael; Acta Crystallographica Section E 63 (2007) o2346–o2348; doi:10.1107/S1600536807015012

data_2213330
_publ_section_title
;25-Decyloxy-26,27,28-trihydroxy-5,11,17-tris(4-nitrophenyldiazenyl)-2,8,14,20-thiacalix[4]arene
 toluene hemisolvate
;
_journal_coeditor_code           HB2337
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2346
_journal_page_last               o2348
_journal_paper_doi               10.1107/S1600536807015012
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C52 H45 N9 O10 S4 , 0.5C7 H8'
_chemical_formula_moiety         'C52 H45 N9 O10 S4 , 0.5C7 H8'
_chemical_formula_sum            'C55.5 H49 N9 O10 S4'
_chemical_formula_weight         1130.28
_chemical_name_systematic
;25-Decyloxy-26,27,28-trihydroxy-5,11,17-tris(4-nitrophenyldiazenyl)-2,8,14,20-
thiacalix[4]arene
 toluene hemisolvate
;
_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           SHELXL97
_cell_angle_alpha                69.893(6)
_cell_angle_beta                 65.769(5)
_cell_angle_gamma                76.226(6)
_cell_formula_units_Z            2
_cell_length_a                   14.0437(10)
_cell_length_b                   14.6038(11)
_cell_length_c                   16.0762(12)
_cell_measurement_reflns_used    20364
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.5
_cell_volume                     2805.2(4)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDSII two-circle'
_diffrn_measurement_method       \w
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46855
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.9314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.649
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         10524
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0769
_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^)+(0.116P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                6244
_reflns_number_total             10524
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2337.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C55.50 H49 N9 O10 S4'
_cod_database_code               2213330
_cod_database_fobs_code          2213330