7,11,15,28-Tetrakis[(2-formylphenoxy)methyl]-1,21,23,25-tetramethylresorcin[4]arene cavitand ethyl acetate clathrate at 173 K
Mc Kay, Michael G.; Friedrich, Holger B.; Howie, R. Alan; Maguire, Glenn E. M.; Acta Crystallographica Section E 65 (2009) o692–o693; doi:10.1107/S1600536809007582

data_2221347
_publ_section_title
;7,11,15,28-Tetrakis[(2-formylphenoxy)methyl]-1,21,23,25-tetramethylresorcin[4]arene
 cavitand ethyl acetate clathrate at 173 K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o692
_journal_page_last               o693
_journal_paper_doi               10.1107/S1600536809007582
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C68 H56 O16'
_chemical_formula_moiety         'C68 H56 O16'
_chemical_formula_sum            'C68 H56 O16'
_chemical_formula_weight         1183.17
_chemical_melting_point          400
_chemical_name_common
;
7,11,15,28-Tetrakis[(2-formylphenoxy)methyl]-1,21,23,25-
tetramethylresorcin[4]arene cavitand
;
_chemical_name_systematic
;
7,11,15,28-Tetrakis[(2-formylphenoxy)methylene]-1,21,23,25-tetramethylpentyl-
2,20:3,19-dimetheno-1<i>H</i>,21<i>H</i>,23<i>H</i>,25<i>H</i>-
bis[1,3]dioxocino[5,4-i:5',4'-i']benzo[1,2-d:5,4-d']bis[1,3]benzodioxocin
stereoisomer
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 117.005(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9228(7)
_cell_length_b                   23.2806(15)
_cell_length_c                   12.2320(7)
_cell_measurement_temperature    173(2)
_cell_volume                     3025.0(3)
_computing_cell_refinement       'SAINT-NT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-NT (Bruker, 2005)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24858
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.9668
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SAINT-NT; Bruker, 2005)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1238
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5470
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+0.9365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2302
_reflns_number_gt                3556
_reflns_number_total             5470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fl2233.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2221347
_cod_database_fobs_code          2221347