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_4032958
_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            'C81 H82 O10'
_chemical_formula_weight         1215.47
_chemical_name_common            'Benzoxymethoxy Pillerene'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                72.623(5)
_cell_angle_beta                 76.291(5)
_cell_angle_gamma                77.888(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0438(11)
_cell_length_b                   14.5042(14)
_cell_length_c                   22.049(3)
_cell_measurement_reflns_used    5202
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     3530.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1093
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27683
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.294
_refine_ls_extinction_coef       0.0070(19)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         12358
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.2028
_refine_ls_R_factor_gt           0.1038
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2834
_refine_ls_wR_factor_ref         0.3483
_reflns_number_gt                5331
_reflns_number_total             12358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b01837_si_002.cif
_cod_data_source_block           Pillar_1a
_cod_depositor_comments
'Adding full bibliography for 4032958--4032966.cif.'
_cod_database_code               4032958