Calixarene Metalloreceptors. Synthesis and Molecular Recognition Properties of Upper-Rim Functionalized Calix[4]arenes Containing an Organopalladium Binding Site
Beth R. Cameron; Stephen J. Loeb; Glenn P. A. Yap; Inorganic Chemistry 36 (1997) 5498–5504; doi:10.1021/ic9705913

data_4323693
_publ_section_title
;
 Calixarene Metalloreceptors. Synthesis and Molecular Recognition
 Properties of Upper-Rim Functionalized Calix[4]arenes Containing an
 Organopalladium Binding Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5498
_journal_page_last               5504
_journal_paper_doi               10.1021/ic9705913
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C56 H66 N4 O6 S2'
_chemical_formula_weight         955.25
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.526(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5095(1)
_cell_length_b                   9.9090(1)
_cell_length_c                   23.3586(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.47
_cell_volume                     5439.59(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18310
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.28396
_exptl_absorpt_correction_T_min  0.21122
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.208
_refine_ls_goodness_of_fit_obs   1.378
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_restrained_S_obs      1.378
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_obs          0.1013
_refine_ls_shift/esd_max         0.200
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+3.4097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2406
_refine_ls_wR_factor_obs         0.2192
_reflns_number_observed          3861
_reflns_number_total             5802
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9705913.cif
_cod_data_source_block           sl009
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+3.4097P] 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^)+(0.0867P)^2^+3.4097P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323693