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_7223652
_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         'C56 H48 O16, 14(C2 H6 O S)'
_chemical_formula_sum            'C84 H132 O30 S14'
_chemical_formula_weight         2070.73
_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_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-05 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                105.3400(10)
_cell_angle_beta                 102.6120(10)
_cell_angle_gamma                106.3690(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3120(3)
_cell_length_b                   17.0039(4)
_cell_length_c                   22.7649(5)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.2
_cell_measurement_theta_min      2.9
_cell_volume                     4522.76(19)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_laue_measured_fraction_full 0.962
_diffrn_reflns_laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53435
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        65.499
_diffrn_reflns_theta_max         65.499
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'Incoatec micro-focus Cu tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    3.818
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.71
_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            Violet
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.490
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         14967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.490
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.1669
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5569
_refine_ls_wR_factor_ref         0.5766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10713
_reflns_number_total             14967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01792k2.cif
_cod_data_source_block           Cocrystal2
_cod_original_cell_volume        4522.76(18)
_cod_database_code               7223652
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.832
_shelx_res_checksum              90976
_shelx_fab_checksum              21443