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_7223656
_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         'C68H48O12, 14(C2H6OS)'
_chemical_formula_sum            'C95.8 H131.4 O26 S14'
_chemical_formula_weight         2147.85
_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                97.687(2)
_cell_angle_beta                 112.271(2)
_cell_angle_gamma                98.894(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9732(18)
_cell_length_b                   14.665(2)
_cell_length_c                   15.949(2)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.19
_cell_volume                     2712.1(6)
_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, 2008)'
_computing_structure_refinement  'SHELXL-2008 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30957
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.41
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.85
_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    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12058
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0996
_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^)+(0.0874P)^2^+18.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2633
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                9507
_reflns_number_total             12058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01792k2.cif
_cod_data_source_block           Cocrystal6
_cod_original_cell_volume        2712.0(7)
_cod_original_formula_sum        'C95.80 H131.40 O26 S14'
_cod_database_code               7223656