Macrocyclic aromatic polysulfones and sulfide-sulfones: synthesis and structural characterisation of molecular pentagons and rectangles
Ben-Haida, Abderrazak; Colquhoun, Howard M.; Hodge, Philip; Raftery, James; White, Andrew J. P.; Williams, David J.; Organic & Biomolecular Chemistry 7 (2009) 5229–5235; doi:10.1039/b912193e

data_7150758
_publ_section_title
;
 Macrocyclic aromatic polysulfones and sulfide-sulfones: synthesis and
 structural characterisation of molecular pentagons and rectangles
;
_journal_issue                   24
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              5229
_journal_page_last               5235
_journal_paper_doi               10.1039/b912193e
_journal_volume                  7
_journal_year                    2009
_chemical_formula_moiety         'C39 H28 O4 S4, C H2 Cl2'
_chemical_formula_sum            'C40 H30 Cl2 O4 S4'
_chemical_formula_weight         773.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.428(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0673(10)
_cell_length_b                   17.1131(16)
_cell_length_c                   21.5403(16)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      4.14
_cell_volume                     3687.7(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6688
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.31
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.034
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4897
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Bruker XPREP, version 5.1/NT
Lamina [0 0 1] absorption correction using psi-scans
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'platy prisms'
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
SQUEEZE suggests 151e/cell. Before SQUEEZE, solvent looked like dcm
and was full occupancy in the middle of the macrocycle.
dcm = CH2Cl2 = 42e. 151e/cell = 37.8e/cell. This is close enough for
the solvent to be considered as 1 dcm per macrocycle.

asu thus C H2 Cl2 low, so UNIT C4 H8 Cl8 low, i.e. C156 H112 O16 S16 Cl0
;
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                3419
_reflns_number_total             5229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912193e.txt
_cod_data_source_block           Compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7150758