5,11,17,23-Tetrakis(1,1-dimethylethyl)-26,28-dihydroxycalix[4]arene-25,27-monothiacrown-3
Xie, De-Xun; An, De-Lie; Acta Crystallographica Section E 69 (2013) o690–; doi:10.1107/S1600536813008684

data_2238082
_publ_section_title
;
 5,11,17,23-Tetrakis(1,1-dimethylethyl)-26,28-dihydroxycalix[4]arene-25,27-monothiacrown-3
;
_journal_coeditor_code           XU5679
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o690
_journal_paper_doi               10.1107/S1600536813008684
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C52 H70 O4 S'
_chemical_formula_moiety         'C52 H70 O4 S'
_chemical_formula_sum            'C52 H70 O4 S'
_chemical_formula_weight         791.14
_chemical_name_systematic
3,9,15,34-Tetra-<i>tert</i>-butyl-19,29-dioxa-24-thiahexacyclo[15.13.7.1^7,11^.1^32,36^.0^5,30^.0^13,18^]nonatriaconta-1(30),2,4,7,9,11(39),13,15,17,32,34,36(38)-dodecaene-38,39-diol
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6222(8)
_cell_length_b                   18.4690(14)
_cell_length_c                   24.5375(18)
_cell_measurement_reflns_used    4874
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      2.2
_cell_volume                     4813.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25550
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.306
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.329
_refine_ls_abs_structure_details 'Flack (1983), 3232 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.09(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         8942
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                5384
_reflns_number_total             8942
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5679.cif
_cod_data_source_block           I
_cod_database_code               2238082
_cod_database_fobs_code          2238082