Syntheses and characterization of aryl-substituted pyrogallol[4]arenes and resorcin[4]arenes
Pfeiffer, Constance R.; Feaster, Kyle A.; Dalgarno, Scott J.; Atwood, Jerry L.; CrystEngComm 18 (2016) 222–; doi:10.1039/C5CE01792K

data_7223655
_publ_section_title
;
 Syntheses and characterization of aryl-substituted pyrogallol[4]arenes
 and resorcin[4]arenes
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              222
_journal_paper_doi               10.1039/C5CE01792K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C68 H72 O16, 12(C2 H6 O S)'
_chemical_formula_sum            'C92 H144 O28 S12'
_chemical_formula_weight         2082.79
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-05 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                110.429(4)
_cell_angle_beta                 109.634(4)
_cell_angle_gamma                92.886(5)
_cell_formula_units_Z            1
_cell_length_a                   13.5643(10)
_cell_length_b                   14.1911(11)
_cell_length_c                   15.9372(12)
_cell_measurement_reflns_used    8369
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.2
_cell_volume                     2658.4(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36332
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         10615
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0647P)^2^+8.6547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1928
_reflns_number_gt                6821
_reflns_number_total             10615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01792k2.cif
_cod_data_source_block           Cocrystal5
_cod_original_cell_volume        2658.4(3)
_cod_database_code               7223655