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_4032961
_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            'C75 H110 O10'
_chemical_formula_weight         1171.62
_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   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                95.191(7)
_cell_angle_beta                 117.822(8)
_cell_angle_gamma                114.325(8)
_cell_formula_units_Z            2
_cell_length_a                   16.620(3)
_cell_length_b                   16.686(3)
_cell_length_c                   16.858(3)
_cell_measurement_reflns_used    5039
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.23
_cell_volume                     3528.1(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.2254
_diffrn_reflns_av_unetI/netI     0.3924
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27263
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         12261
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.4213
_refine_ls_R_factor_gt           0.1323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.4465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2150
_reflns_number_total             12261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01837_si_002.cif
_cod_data_source_block           Pillar_1bOH
_cod_depositor_comments
'Adding full bibliography for 4032958--4032966.cif.'
_cod_original_cell_volume        3528.0(12)
_cod_database_code               4032961
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              68346
_shelx_hkl_checksum              1774
_shelx_fab_checksum              98403