31-Benzyloxy-5,11,17,23,29-penta-<i>tert</i>-butylcalix[5]arene-32,33,34,35-tetraol
Gargiulli, Claudia; Gattuso, Giuseppe; Notti, Anna; Nicoló, Francesco; Pappalardo, Andrea; Acta Crystallographica Section E 68 (2012) o3423–; doi:10.1107/S1600536812047435

data_2236925
_publ_section_title
;
 31-Benzyloxy-5,11,17,23,29-penta-<i>tert</i>-butylcalix[5]arene-32,33,34,35-tetraol
;
_journal_coeditor_code           IS5208
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3423
_journal_paper_doi               10.1107/S1600536812047435
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C62 H76 O5'
_chemical_formula_moiety         'C62 H76 O5'
_chemical_formula_sum            'C62 H76 O5'
_chemical_formula_weight         901.23
_chemical_name_systematic
;
31-Benzyloxy-5,11,17,23,29-penta-<i>tert</i>-butylcalix[5]arene-
32,33,34,35-tetraol
;
_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                70.653(3)
_cell_angle_beta                 78.776(3)
_cell_angle_gamma                71.573(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1467(8)
_cell_length_b                   14.3235(9)
_cell_length_c                   15.2179(9)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.11
_cell_measurement_theta_min      2.83
_cell_volume                     2746.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker 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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75089
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.160
_refine_ls_extinction_coef       0.0062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         10532
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                5343
_reflns_number_total             10532
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5208.cif
_cod_data_source_block           I
_cod_database_code               2236925
_cod_database_fobs_code          2236925