Synthesis and X-ray Crystal Structure of Difunctionalized Pillar[5]arene at A1/B2 Positions by in-situ Cyclization and Deprotection
Tomoki Ogoshi; Keisuke Kitajima; Shuhei Fujinami; Tada-aki Yamagishi; Chem.Commun. 47 (2011) 10106–; doi:10.1039/c1cc13546e

data_7106832
_publ_section_title
;
 Synthesis and X-ray Crystal Structure of Difunctionalized Pillar[5]arene
 at A1/B2 Positions by in-situ Cyclization and Deprotection
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              10106
_journal_paper_doi               10.1039/c1cc13546e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C44 H46 O11'
_chemical_formula_weight         750.84
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 99.209(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.069(3)
_cell_length_b                   14.029(2)
_cell_length_c                   13.773(2)
_cell_measurement_reflns_used    7235
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     3827.8(10)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123.2
_diffrn_detector_area_resol_mean 14.46
_diffrn_measured_fraction_theta_full 0.9868
_diffrn_measured_fraction_theta_max 0.9868
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4511
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1608.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2513
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00144|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                2513
_reflns_number_total             4341
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            c1cc13546e.txt
_cod_data_source_block           global
_cod_original_cell_volume        3827.7(9)
_cod_original_formula_sum        'C44 H46 O11 '
_cod_database_code               7106832