1,3-Alternate and partial cone conformers of tetramethyl (5,11,17,23-tetra-<i>tert</i>-butyl-2,8,14,20-tetrathiacalix[4]arene-25,26,27,28-tetrayltetraoxy)tetraacetate and tetramethyl (5,11,17,23-tetrabromo-2,8,14,20-tetrathiacalix[4]arene-25,26,27,28-tetrayltetraoxy)tetraacetate
Xu, Wei-Na; Yuan, Jiu-Mao; Liu, Yang; Ma, Jian-Ping; Guo, Dian-Shun; Acta Crystallographica Section C 64 (2008) o349–o352; doi:10.1107/S0108270108013838

data_2016641
_publ_section_title
;1,3-Alternate and partial cone conformers of tetramethyl
 (5,11,17,23-tetra-<i>tert</i>-butyl-2,8,14,20-tetrathiacalix[4]arene-25,26,27,28-tetrayltetraoxy)tetraacetate
 and tetramethyl
 (5,11,17,23-tetrabromo-2,8,14,20-tetrathiacalix[4]arene-25,26,27,28-tetrayltetraoxy)tetraacetate
;
_journal_coeditor_code           GG3153
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o349
_journal_page_last               o352
_journal_paper_doi               10.1107/S0108270108013838
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C52 H64 O12 S4'
_chemical_formula_moiety         'C52 H64 O12 S4'
_chemical_formula_sum            'C52 H64 O12 S4'
_chemical_formula_weight         1009.27
_chemical_melting_point          583
_chemical_name_systematic
;
tetramethyl
(5,11,17,23-tetra-<i>tert</i>-butyl-2,8,14,20-tetrathiacalix[4]arene-
25,26,27,28-tetrayltetraoxy)tetraacetate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 122.890(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.060(4)
_cell_length_b                   13.547(2)
_cell_length_c                   20.083(4)
_cell_measurement_reflns_used    3304
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.137
_cell_measurement_theta_min      2.491
_cell_volume                     5268.2(16)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13453
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+12.3991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                3834
_reflns_number_total             4893
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3153.cif
_cod_data_source_block           I
_cod_original_cell_volume        5268.3(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016641
_cod_database_fobs_code          2016641