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_4115925
_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     '[{(en)Pd(bpz)Pd(en)}3](NO3)4(PF6)8 * 5H2O'
_chemical_formula_sum            'C36 H76 F48 N28 O17 P8 Pd6'
_chemical_formula_weight         2971.41
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.977(3)
_cell_length_b                   22.705(5)
_cell_length_c                   22.734(5)
_cell_measurement_reflns_used    12757
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      2.57
_cell_volume                     8744(3)
_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      133(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 60s 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  0.095
_diffrn_reflns_av_sigmaI/netI    0.1170
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12757
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.7196
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_description       cube
_exptl_crystal_F_000             5808
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00006(3)
_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   0.898
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         12744
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.976
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         -0.023
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1341
_refine_ls_wR_factor_obs         0.1115
_reflns_number_observed          6968
_reflns_number_total             12757
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9931325_5.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0643P)^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^)+(0.0643P)^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        8744.4(31)
_cod_database_code               4115925