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_4115926
_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     '[enPd(2,2'-bpz)enPt]3(PF6)5(NO3)7 * 9.75H2O'
_chemical_formula_sum            'C36 H85.5 F30 N31 O30.75 P5 Pd3 Pt3'
_chemical_formula_weight         3074.17
_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                 95.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.920(3)
_cell_length_b                   24.099(5)
_cell_length_c                   22.146(4)
_cell_measurement_reflns_used    20196
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      2.56
_cell_volume                     8993(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      143(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 30s 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  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20196
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    5.477
_exptl_absorpt_correction_T_max  0.1250
_exptl_absorpt_correction_T_min  0.1049
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_description       block
_exptl_crystal_F_000             5926
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.69
_exptl_crystal_size_min          0.65
_refine_diff_density_max         2.595
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.229
_refine_ls_extinction_coef       0.00059(8)
_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   1.112
_refine_ls_goodness_of_fit_obs   1.209
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         11364
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.199
_refine_ls_restrained_S_obs      1.210
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_obs          0.0937
_refine_ls_shift/esd_max         2.249
_refine_ls_shift/esd_mean        0.184
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+318.0578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2583
_refine_ls_wR_factor_obs         0.2266
_reflns_number_observed          8762
_reflns_number_total             11388
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9931325_6.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+318.0578P] 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^)+(0.0785P)^2^+318.0578P] 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        8993.3(29)
_cod_original_formula_sum        'C36 H85.50 F30 N31 O30.75 P5 Pd3 Pt3'
_cod_database_code               4115926