A dimer-to-dimer metal–metal linear aggregate from a nitrate-bridged <i>cis</i>-(2,2':6',2''-terpyridyl-κ^3^<i>N</i>)palladium(II) cofacial dimer
Mei, Guang-Quan; Huang, Ke-Long; Huang, Hai-Ping; Acta Crystallographica Section E 63 (2007) m2510–m2511; doi:10.1107/S1600536807042766

data_2215455
_publ_section_title
;
 A dimer-to-dimer metal--metal linear aggregate from a nitrate-bridged
 <i>cis</i>-(2,2':6',2''-terpyridyl-\k^3^<i>N</i>)palladium(II)
 cofacial dimer
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2510
_journal_page_last               m2511
_journal_paper_doi               10.1107/S1600536807042766
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pd2 (C15 H11 N3)2 N O3] (P F6)3, C2 H3 N'
_chemical_formula_moiety         'C30 H22 N7 O3 Pd2 3+, 3(F6 P)-, 0.5(C2 H3 N)'
_chemical_formula_sum            'C31 H23.5 F18 N7.5 O3 P3 Pd2'
_chemical_formula_weight         1196.78
_chemical_name_systematic
;
\m-nitrato-bis[(2,2':6',2''-terpyridyl-\k3N)palladium(II)]
 hexakis(hexafluorophosphate) acetonitrile solvate
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.681(4)
_cell_angle_beta                 90.4500(10)
_cell_angle_gamma                102.226(3)
_cell_formula_units_Z            4
_cell_length_a                   14.0633(3)
_cell_length_b                   14.7277(4)
_cell_length_c                   20.7043(7)
_cell_measurement_reflns_used    683
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.02
_cell_volume                     4045.6(2)
_computing_cell_refinement       'Rapid-Auto (Rigaku, 1999)'
_computing_data_collection       'Rapid-Auto (Rigaku, 1999)'
_computing_data_reduction        'Rapid-Auto (Rigaku, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997) and PLATON (Spek, 2003)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27513
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.609
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         17102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+15.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                13353
_reflns_number_total             17102
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3057.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C30 H22 N7 O3 Pd2) 3+, 6(F6 P)-, C2 H3 N'
_cod_original_formula_iupac      '[Pd2 (C15 H11 N3)2 N O3] P F6, C2 H3 N'
_cod_original_formula_sum        'C62 H47 F36 N15 O6 P6 Pd4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2393.57
_cod_database_code               2215455
_cod_database_fobs_code          2215455