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_4115286
_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(C50 H28 N2 O10 S2) . Pd C18 H12 N2 O2 . 4(CH2Cl2)'
_chemical_formula_sum            'C122 H76 Cl8 N6 O22 Pd S4'
_chemical_formula_weight         2496.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.651(3)
_cell_length_b                   16.699(2)
_cell_length_c                   30.468(2)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      7.98
_cell_volume                     11016(2)
_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      293(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1856
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7457
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         4.08
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.493
_exptl_absorpt_correction_T_max  .994
_exptl_absorpt_correction_T_min  .635
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Lamina 0 0 1'
_exptl_crystal_colour            Olive/grey
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       'Rhombic plates'
_exptl_crystal_F_000             5088
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.347
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         5866
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.156
_refine_ls_restrained_S_obs      1.347
_refine_ls_R_factor_all          0.2447
_refine_ls_R_factor_obs          0.0998
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+3.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2830
_refine_ls_wR_factor_obs         0.1953
_reflns_number_observed          2959
_reflns_number_total             7457
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027851m-2_s2_4.cif
_cod_data_source_block           hmc0204_Compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+3.0459P] 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^)+(0.0757P)^2^+3.0459P] 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        11016.0(18)
_cod_database_code               4115286