A Calix[4]arene with Diethylthiocarbamoylmethyloxy Substituents in the 1,3 Positions
Drew, M. G. B.; Beer, P. D.; Ogden, M. I.; Acta Crystallographica Section C 53 (1997) 472–474; doi:10.1107/S0108270196015521

data_2006045
_publ_contact_author
;
Dr M. G. B. Drew
Department of Chemistry
University of Reading
Whiteknights
Reading RG6 2AD
;
_publ_section_title
;
 A Calix[4]arene with Diethylthiocarbamoylmethyloxy Substituents in the
 1,3 Positions
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              472
_journal_page_last               474
_journal_paper_doi               10.1107/S0108270196015521
_journal_volume                  53
_journal_year                    1997
_chemical_formula_structural     'C56 H78 N2 O4 S2'
_chemical_formula_sum            'C56 H78 N2 O4 S2'
_chemical_formula_weight         907.32
_chemical_name_systematic
;
5,11,17,23-Tetra-tert-butyl-25,27-bis((diethylthiocarbamoyl)-
methoxy)-26,28-dihydroxycalix[4]arene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                82.648(10)
_cell_angle_beta                 77.869(10)
_cell_angle_gamma                67.661(10)
_cell_formula_units_Z            2
_cell_length_a                   12.815(9)
_cell_length_b                   14.798(12)
_cell_length_c                   15.584(14)
_cell_measurement_reflns_used    1250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      3.34
_cell_volume                     2669(4)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1988)'
_computing_data_reduction        XDS
_computing_molecular_graphics    'PLATON (Spek, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2\% intervals, counting time 2 min'
_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  0.052
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16265
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         3.34
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.446
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.615
_refine_ls_goodness_of_fit_obs   0.602
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9432
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.621
_refine_ls_restrained_S_obs      0.610
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_obs          0.0831
_refine_ls_shift/esd_max         0.438
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2778P)^2^+11.3102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2928
_refine_ls_wR_factor_obs         0.2440
_reflns_number_observed          6739
_reflns_number_total             9432
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cf1144.cif
_cod_data_source_block           global
_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^)+(0.2778P)^2^+11.3102P] 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^)+(0.2778P)^2^+11.3102P] 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        2669.(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C56 H78 N2 O4 S2  '
_cod_database_code               2006045