Self-Assembly of Palladium(II) and Platinum(II) Complexes of 2-Hydroxypyrimidine to Novel Metallacalix[4]arenes. Receptor Properties through Multiple H-Bonding Interactions
Jorge A. R. Navarro; Eva Freisinger; Bernhard Lippert; Inorganic Chemistry 39 (2000) 2301–2305; doi:10.1021/ic991411n

data_4320999
_publ_contact_author_address
; Department of Inorganic Chemistry
  Universidad de Granada
  E-18071 Granada
  Spain

  Fachbereich Chemie
  Universit\"at Dortmund
  Otto-Hahn-Str. 6
  D-44221 Dortmund
  Germany
;
_publ_contact_author_email       lippert@pop.uni-dortmund.de
_publ_contact_author_fax         'Int. code + (231) 755-3797'
_publ_contact_author_name
'Dr. Jorge A. R. Navarro, Prof. Bernhard Lippert'
_publ_contact_author_phone       '231 755-3840'
_publ_section_title
;
 Self-Assembly of Palladium(II) and Platinum(II) Complexes of
 2-Hydroxypyrimidine to Novel Metallacalix[4]arenes. Receptor Properties
 through Multiple H-Bonding Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2301
_journal_page_last               2305
_journal_paper_doi               10.1021/ic991411n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 H59 Cl5 Cu0.5 N16 O31.5 Pt4'
_chemical_formula_weight         2065.25
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.693(3)
_cell_length_b                   15.203(3)
_cell_length_c                   23.483(5)
_cell_measurement_reflns_used    30581
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.95
_cell_volume                     5878(2)
_computing_cell_refinement       'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius BV, Netherlands)'
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via \w-rotation (\D\w\=1\%) and two times 200s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1273
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30581
_diffrn_reflns_theta_max         23.15
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    9.992
_exptl_absorpt_correction_T_max  0.6907
_exptl_absorpt_correction_T_min  0.1597
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_description       stick
_exptl_crystal_F_000             3914
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.867
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.879
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         -0.019
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1114
_refine_ls_wR_factor_obs         0.0972
_reflns_number_observed          4470
_reflns_number_total             8267
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991411n_3.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] 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^)+(0.0396P)^2^+0.0000P] 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        5877.9(20)
_cod_original_formula_sum        'C24 H59 Cl5 Cu0.50 N16 O31.50 Pt4'
_cod_database_code               4320999