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_2016640
_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          'C36 H28 Br4 O12 S4'
_chemical_formula_moiety         'C36 H28 Br4 O12 S4'
_chemical_formula_sum            'C36 H28 Br4 O12 S4'
_chemical_formula_weight         1100.46
_chemical_name_systematic
;
tetramethyl
(5,11,17,23-tetrabromo-2,8,14,20-tetrathiacalix[4]arene-25,26,27,28-
tetrayltetraoxy)tetraacetate
;
_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-97
_cell_angle_alpha                82.296(2)
_cell_angle_beta                 84.921(2)
_cell_angle_gamma                74.872(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4298(15)
_cell_length_b                   13.960(2)
_cell_length_c                   14.701(2)
_cell_measurement_reflns_used    3300
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     2044.4(5)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10757
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    4.202
_exptl_absorpt_correction_T_max  0.4724
_exptl_absorpt_correction_T_min  0.1943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.667
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                5974
_reflns_number_total             7443
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3153.cif
_cod_data_source_block           II
_cod_original_cell_volume        2044.5(5)
_cod_database_code               2016640
_cod_database_fobs_code          2016640