A New Synthetic Method for Non-symmetric Pillar[5]arenes with Simple Isolation and Improved Yield
Ding, Jiaming; Chen, Jiafu; Mao, Weipeng; Huang, Junrou; Ma, Da; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB02013A

data_7155864
_publ_section_title
;
 A New Synthetic Method for Non-symmetric Pillar[5]arenes with Simple
 Isolation and Improved Yield
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB02013A
_journal_year                    2017
_chemical_formula_sum            'C70 H75 Br5 O10'
_chemical_formula_weight         1475.85
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-18 deposited with the CCDC.
2017-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                75.920(5)
_cell_angle_beta                 73.481(5)
_cell_angle_gamma                86.123(6)
_cell_formula_units_Z            2
_cell_length_a                   12.160(4)
_cell_length_b                   16.526(5)
_cell_length_c                   19.764(6)
_cell_measurement_reflns_used    4669
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      2.16
_cell_volume                     3693(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.1353
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23878
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.476
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         3.504
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         14331
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.2148
_refine_ls_R_factor_gt           0.1380
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3774
_refine_ls_wR_factor_ref         0.4184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7000
_reflns_number_total             14331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob02013a2.cif
_cod_data_source_block           mo_70601a_sq
_cod_original_cell_volume        3693.4(19)
_cod_database_code               7155864
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.168
_shelx_estimated_absorpt_t_max   0.544
_shelx_res_checksum              1368
_shelx_fab_checksum              2921