Molecular Architecture Based on Metal Triangles Derived from 2,2'-Bipyrazine (Bpz) and EnMII (M = Pt, Pd)
Ralf-Dieter Schnebeck; Eva Freisinger; Frank Glahé; Bernhard Lippert; Journal of the American Chemical Society 122 (2000) 1381–1390; doi:10.1021/ja9931325

data_4115922
_publ_contact_author_address
; 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        'Prof. Bernhard Lippert'
_publ_contact_author_phone       '231 755-3840'
_publ_section_title
;
 Molecular Architecture Based on Metal Triangles Derived from
 2,2'-Bipyrazine (Bpz) and EnMII (M = Pt, Pd)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1381
_journal_page_last               1390
_journal_paper_doi               10.1021/ja9931325
_journal_volume                  122
_journal_year                    2000
_chemical_formula_structural     '[enPt(bpz)]3(PF6)4(NO3)2 * 5.25H2O'
_chemical_formula_sum            'C60 H105 F48 N40 O22.5 P8 Pt6'
_chemical_formula_weight         4077.14
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.95(3)
_cell_angle_beta                 75.24(3)
_cell_angle_gamma                86.00(3)
_cell_formula_units_Z            2
_cell_length_a                   15.363(3)
_cell_length_b                   18.948(4)
_cell_length_c                   21.679(4)
_cell_measurement_reflns_used    15245
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      1.37
_cell_volume                     6087(2)
_computing_cell_refinement       'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_collection
'Collect, datacollection software, Nonius, 1998'
_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      123(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
359 frames via \w-rotation (\D\w\=1\%) and two times 40s 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  0.070
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15245
_diffrn_reflns_theta_max         24.38
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    7.125
_exptl_absorpt_correction_T_max  0.1727
_exptl_absorpt_correction_T_min  0.1249
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_description       block
_exptl_crystal_F_000             3890
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.489
_refine_diff_density_min         -1.759
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.00020(6)
_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   1.019
_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1338
_refine_ls_number_reflns         15233
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_obs          0.0731
_refine_ls_shift/esd_max         -0.951
_refine_ls_shift/esd_mean        0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+39.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2223
_refine_ls_wR_factor_obs         0.1872
_reflns_number_observed          9421
_reflns_number_total             15245
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9931325_2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+39.6515P] 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^)+(0.1254P)^2^+39.6515P] 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        6086.7(21)
_cod_original_formula_sum        'C60 H105 F48 N40 O22.50 P8 Pt6'
_cod_database_code               4115922