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_7150755
_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         'C36 H24 O8 S4, C Cl2 O, 2(C H Cl3)'
_chemical_formula_sum            'C39 H26 Cl8 O9 S4'
_chemical_formula_weight         1050.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.555(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8261(19)
_cell_length_b                   10.809(2)
_cell_length_c                   20.350(4)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      4.01
_cell_volume                     2157.2(7)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4/RA'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3616
_diffrn_reflns_theta_full        61.99
_diffrn_reflns_theta_max         61.99
_diffrn_reflns_theta_min         4.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.052
_exptl_absorpt_correction_T_max  0.2821
_exptl_absorpt_correction_T_min  0.0833
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Bruker XPREP, version 5.1/NT
Ellipsoidal absorption correction using psi-scans
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.77
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
SQUEEZE suggests 308e/cell. Before SQUEEZE, solvent looked like COCl2
inside the macrocycle and 2CHCl3 outside (per macrocycle).
COCl2 = 48e, CHCl3 = 58e. 308e/cell = 154e/macrocycle. This is close
to COCl2.2CHCl3 (48+58+58=164e) so this was considered to be the
solvent present.

asu thus C1.5 H O0.5 Cl4 low, so UNIT C6 H4 O2 Cl16 low,
i.e. C72 H48 O16 S8 Cl0
;
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0540
_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^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                2739
_reflns_number_total             3397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912193e.txt
_cod_data_source_block           Compound_3
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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)/n
_cod_database_code               7150755