Macrocyclic Aromatic Ether-Imide-Sulfones: Versatile Supramolecular Receptors with Extreme Thermochemical and Oxidative Stability
Howard M. Colquhoun; David J. Williams; Zhixue Zhu; Journal of the American Chemical Society 124 (2002) 13346–13347; doi:10.1021/ja027851m

data_4115285
_publ_section_title
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 Macrocyclic Aromatic Ether-Imide-Sulfones: Versatile Supramolecular
 Receptors with Extreme Thermochemical and Oxidative Stability
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13346
_journal_page_last               13347
_journal_paper_doi               10.1021/ja027851m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C50 H28 N2 O10 S2 . C20 H12 . 2(C3 H7 N O)'
_chemical_formula_sum            'C76 H54 N4 O12 S2'
_chemical_formula_weight         1279.35
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 106.171(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8199(6)
_cell_length_b                   36.2332(12)
_cell_length_c                   17.4128(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      9.81
_cell_volume                     5950.5(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9938
_diffrn_reflns_theta_max         61.99
_diffrn_reflns_theta_min         2.44
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  0.8901
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red-brown
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       laths
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          .57
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00040(4)
_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_all   1.042
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         8769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_obs          0.0423
_refine_ls_shift/esd_max         -0.089
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+1.2240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1147
_refine_ls_wR_factor_obs         0.1014
_reflns_number_observed          7375
_reflns_number_total             9334
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027851m-2_s2_3.cif
_cod_data_source_block           hmc0120_Compound6
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+1.2240P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+1.2240P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4115285