25-Allyloxy-5,11,17,23-tetra-<i>tert</i>-butyl-26,27,28-trihydroxycalix[4]arene chloroform disolvate
Gruber, Tobias; Eissmann, Frank; Seichter, Wilhelm; Weber, Edwin; Acta Crystallographica Section C 66 (2010) o334–o336; doi:10.1107/S0108270110020858

data_2017713
_publ_section_title
;
 25-Allyloxy-5,11,17,23-tetra-<i>tert</i>-butyl-26,27,28-trihydroxycalix[4]arene
 chloroform disolvate
;
_journal_coeditor_code           GD3348
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o334
_journal_page_last               o336
_journal_paper_doi               10.1107/S0108270110020858
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C47 H60 O4 , 2C H Cl3'
_chemical_formula_moiety         'C47 H60 O4 , 2C H Cl3'
_chemical_formula_sum            'C49 H62 Cl6 O4'
_chemical_formula_weight         927.69
_chemical_name_systematic
;
25-Allyloxy-5,11,17,23-tetra-<i>tert</i>-butyl-26,27,28-trihydroxycalix[4]arene
chloroform disolvate
;
_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                 120.068(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.8774(7)
_cell_length_b                   16.8275(7)
_cell_length_c                   23.3186(8)
_cell_measurement_reflns_used    8476
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      2.02
_cell_volume                     9806.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            102072
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.8751
_exptl_absorpt_correction_T_min  0.7910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.966
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8635
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0912P)^2^+22.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                7171
_reflns_number_total             8635
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3348.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017713
_cod_database_fobs_code          2017713