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_4115283
_publ_section_title
;
 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
;
2(C46 H26 N2 O10 S2) .1.5(CHCl3) .1.25(CH2Cl2) .1.5(C2 H O2 F3) 
.0.5(CH3 OH) .1.5(H2 O)
;
_chemical_formula_sum            'C98.25 H62.5 Cl7 F4.5 N4 O25 S4'
_chemical_formula_weight         2160.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                79.492(12)
_cell_angle_beta                 86.200(12)
_cell_angle_gamma                69.796(9)
_cell_formula_units_Z            2
_cell_length_a                   12.7216(19)
_cell_length_b                   15.1679(19)
_cell_length_c                   25.883(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      20.98
_cell_measurement_theta_min      4.28
_cell_volume                     4608.4(12)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14325
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         1.74
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.7339
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Pale_yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2207
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00002(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   1.139
_refine_ls_goodness_of_fit_obs   1.268
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1413
_refine_ls_number_reflns         13619
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.282
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_obs          0.0863
_refine_ls_shift/esd_max         0.440
_refine_ls_shift/esd_mean        0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+2.3588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2174
_refine_ls_wR_factor_obs         0.1930
_reflns_number_observed          8273
_reflns_number_total             13619
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027851m-2_s2_1.cif
_cod_data_source_block           hmc0106_compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+2.3588P] 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^)+(0.0781P)^2^+2.3588P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4608.4(11)
_cod_original_formula_sum        'C98.25 H62.50 Cl7 F4.50 N4 O25 S4'
_cod_database_code               4115283