Crystal Structure of 25-(2-tert-Butoxyethoxy)-27-hydroxycalix[4]arene-crown-6 in the Cone Conformation
Guillon, Jean; Leger, Jean-Michel; Sonnet, Pascal; Jarry, Christian; Analytical Sciences: X-ray Structure Analysis Online 19 (2003) x9–x10; doi:10.2116/analscix.19.x9

data_1100653
_publ_section_title
;
 Crystal Structure of 25-(2-tert-Butoxyethoxy)-27-hydroxycalix[4]arene-crown-6
 in the Cone Conformation
;
_journal_name_full
;
 Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first              x9
_journal_page_last               x10
_journal_paper_doi               10.2116/analscix.19.x9
_journal_volume                  19
_journal_year                    2003
_chemical_formula_sum            'C44 H54 O9'
_chemical_formula_weight         726.87
_space_group_IT_number           2
_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
_cell_angle_alpha                84.74(2)
_cell_angle_beta                 87.840(10)
_cell_angle_gamma                75.77(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2140(10)
_cell_length_b                   12.734(5)
_cell_length_c                   16.062(2)
_cell_measurement_temperature    296(2)
_cell_volume                     2016.2(9)
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6795
_diffrn_reflns_theta_full        64.88
_diffrn_reflns_theta_max         64.88
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.9242
_exptl_absorpt_correction_T_min  0.6345
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.178
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1622P)^2^+0.8043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2599
_refine_ls_wR_factor_ref         0.2807
_reflns_number_gt                5105
_reflns_number_total             6795
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1100653