1,2,4,5-Tetrakis(phenylsulfonyl)benzene: a novel quadruped host with D2 symmetry having ordered sulfolane and cycloheptanone guests
Louis J. Farrugia; James H. Gall; David D. MacNicol; Chem.Commun. 48 (2012) 10600–; doi:10.1039/c2cc35647c

data_7108500
_publ_section_title
;
 1,2,4,5-Tetrakis(phenylsulfonyl)benzene: a novel quadruped host with D2
 symmetry having ordered sulfolane and cycloheptanone guests
;
_journal_name_full               Chem.Commun.
_journal_page_first              10600
_journal_paper_doi               10.1039/c2cc35647c
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H22 O8 S4, 2(C4 H8 O2 S)'
_chemical_formula_sum            'C38 H38 O12 S6'
_chemical_formula_weight         879.04
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-06-07T14:18:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.916(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3523(13)
_cell_length_b                   11.5228(8)
_cell_length_c                   18.6286(14)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8173
_cell_measurement_theta_min      2.2197
_cell_measurement_wavelength     0.71073
_cell_volume                     3938.9(5)
_computing_cell_refinement       'SAINT V7.68A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      -0.468577E-1
_diffrn_orient_matrix_UB_12      -0.248359E-1
_diffrn_orient_matrix_UB_13      -0.676418E-1
_diffrn_orient_matrix_UB_21      0.142704E-1
_diffrn_orient_matrix_UB_22      -0.831481E-1
_diffrn_orient_matrix_UB_23      0.198537E-1
_diffrn_orient_matrix_UB_31      -0.21978E-1
_diffrn_orient_matrix_UB_32      -0.103759E-2
_diffrn_orient_matrix_UB_33      0.280888E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60930
_diffrn_reflns_reduction_process
;
Scaled and merged with Sortav
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
After data reduction, the structure was transformed from the input space
group of C2/c (having a beta angle of ~134 deg) to the non-standard I2/a
cell with a beta angle closer to 90 deg. This was done to remove many high
correlations in the refinement.
The data given for _diffrn_reflns_limit_h_min etc are for the original C2/c
cell
;
_diffrn_reflns_theta_full        34.89
_diffrn_reflns_theta_max         34.89
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         8583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+1.8791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7301
_reflns_number_total             8583
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc35647c.txt
_cod_data_source_block           compound_1a
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7108500