Syntheses of a pillar[4]arene[1]quinone and a difunctionalized pillar[5]arene by partial oxidation
Chengyou Han; Zibin Zhang; Guocan Yu; Feihe Huang; Chem.Commun. 48 (2012) 9876–; doi:10.1039/c2cc35498e

data_7108401
_publ_section_title
;
 Syntheses of a pillar[4]arene[1]quinone and a difunctionalized
 pillar[5]arene by partial oxidation
;
_journal_name_full               Chem.Commun.
_journal_page_first              9876
_journal_paper_doi               10.1039/c2cc35498e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         '2(C43 H44 O10), 3(C H2 Cl2)'
_chemical_formula_sum            'C44.5 H47 Cl3 O10'
_chemical_formula_weight         848.17
_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                 92.9319(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   36.5565(4)
_cell_length_b                   20.67542(18)
_cell_length_c                   22.5397(2)
_cell_measurement_reflns_used    31801
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      67.4362
_cell_measurement_theta_min      2.8995
_cell_volume                     17013.7(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102790
_diffrn_reflns_theta_full        67.56
_diffrn_reflns_theta_max         67.56
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.6175
_exptl_absorpt_correction_T_min  0.5108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7120
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2103
_refine_ls_number_reflns         30386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0840P)^2^+18.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1838
_reflns_number_gt                24099
_reflns_number_total             30386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35498e.txt
_cod_data_source_block           120621_hcy_po_cu
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7108401