Constitutional Isomers of Pentahydroxy-Functionalized Pillar[5]arenes: Synthesis, Characterization, and Crystal Structures.
Al-Azemi, Talal F; Vinodh, Mickey; Alipour, Fatemeh H.; Mohamod, Abdirahman A.; The Journal of organic chemistry 82 (2017) 10945–10952; doi:10.1021/acs.joc.7b01837

data_4032960
_publ_section_title
;
 Constitutional Isomers of Pentahydroxy-Functionalized Pillar[5]arenes:
 Synthesis, Characterization, and Crystal Structures.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10945
_journal_page_last               10952
_journal_paper_doi               10.1021/acs.joc.7b01837
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C110 H140 O10'
_chemical_formula_weight         1622.22
_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'
_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                 104.773(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.045(10)
_cell_length_b                   21.347(5)
_cell_length_c                   23.043(5)
_cell_measurement_reflns_used    3102
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      3.00
_cell_volume                     20474(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71278
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             7040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00052(15)
_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   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         17960
_refine_ls_number_restraints     435
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.2489
_refine_ls_R_factor_gt           0.1480
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3802
_refine_ls_wR_factor_ref         0.4289
_reflns_number_gt                5695
_reflns_number_total             17960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b01837_si_002.cif
_cod_data_source_block           Pillar_1b
_cod_depositor_comments
'Adding full bibliography for 4032958--4032966.cif.'
_cod_database_code               4032960