5,11,17,23-Tetra-<i>tert</i>-butyl-25,26,27,28-tetramethoxycalix[4]arene dichloromethane hemisolvate
Fischer, Conrad; Gruber, Tobias; Seichter, Wilhelm; Schindler, Diana; Weber, Edwin; Acta Crystallographica Section E 64 (2008) o673–; doi:10.1107/S1600536808002304

data_2218002
_publ_section_title
;
 5,11,17,23-Tetra-<i>tert</i>-butyl-25,26,27,28-tetramethoxycalix[4]arene
 dichloromethane hemisolvate
;
_journal_coeditor_code           SI2068
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o673
_journal_paper_doi               10.1107/S1600536808002304
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C48 H64 O4, 0.5C H2 Cl2'
_chemical_formula_moiety         'C48 H64 O4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C48.5 H65 Cl O4'
_chemical_formula_weight         747.46
_chemical_name_systematic
;
5,11,17,23-Tetra-<i>tert</i>-butyl-25,26,27,28-tetramethoxycalix[4]arene
dichloromethane hemisolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.097(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7012(6)
_cell_length_b                   19.7113(8)
_cell_length_c                   28.2577(11)
_cell_measurement_temperature    133(2)
_cell_volume                     9060.5(6)
_computing_cell_refinement       'SAINT-NT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-NT (Bruker, 2004)'
_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      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            186561
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.9292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         20781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1495P)^2^+1.8277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2718
_reflns_number_gt                12758
_reflns_number_total             20781
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2068.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C48.5 H65 Cl1 O4'
_cod_database_code               2218002
_cod_database_fobs_code          2218002