The Cone Conformer of a Tetrakis(methylthio)tetrapropoxycalix[4]arene
Schultz, Thomas M.; Hazell, Rita G.; Larsen, Mogens; Acta Crystallographica Section C 53 (1997) 1495–1497; doi:10.1107/S0108270197007725

data_2006547
_publ_section_title
;
 The Cone Conformer of a Tetrakis(methylthio)tetrapropoxycalix[4]arene
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1495
_journal_page_last               1497
_journal_paper_doi               10.1107/S0108270197007725
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C44 H56 O4 S4'
_chemical_formula_weight         777.20
_chemical_melting_point          451.6(5)
_chemical_name_systematic
;
5,11,17,23-tetra(methylthio)-25,26,27,28-tetrapropoxy-calix[4]arene
;
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90.00
_cell_angle_beta                 97.400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.479(3)
_cell_length_b                   27.145(8)
_cell_length_c                   12.591(4)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    120
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     4230(2)
_computing_cell_refinement       MAD
_computing_data_collection       'MAD (Allibon, 1995)'
_computing_data_reduction        'KRYSTAL (Hazell, 1995)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996), KRYSTAL'
_computing_publication_material  KRYSTAL
_computing_structure_refinement
'modified ORFLS (Busing, Martin & Levy, 1962)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994), KRYSTAL'
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Huber four-circle diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6324
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.67(6)
_refine_diff_density_min         -0.39(6)
_refine_ls_extinction_coef       4E1(4)
_refine_ls_extinction_method
;type 1, Lorentzian isotropic (Becker & Coppens, 1975); mean path length put
 to 1
;
_refine_ls_goodness_of_fit_obs   1.466
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     508
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .057
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
   w = 1/{[\s(F^2^)+1.03F^2^]^1/2^-|F|}^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .067
_reflns_number_observed          4431
_reflns_number_total             5999
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ab1468.cif
_cod_data_source_block           calix
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '178-179\%C' was changed to
'451.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_atom_site_thermal_displace_type' tag value 'Uij' was
replaced with 'Uani' value 56 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '178-179\%C' was changed to
'451.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006547