A cyclic dipalladium compound formed by concomitant N‒C coupling and [2+3]-cycloaddition: bis{μ-1-[4-(carbodiimido)phenyl]tetrazolato-κ^2^<i>N</i>:<i>C</i>^5^}bis[bis(trimethylphosphine-κ<i>P</i>)palladium(II)]
Han, Won Seok; Lee, Hee Keun; Kim, Yong-Joo; Lee, Soon W.; Acta Crystallographica Section E 60 (2004) m1813–m1814; doi:10.1107/S1600536804028260

data_2204796
_publ_section_title
;A cyclic dipalladium compound formed by concomitant N--C coupling and
 [2+3]-cycloaddition:
 bis{\m-1-[4-(carbodiimido)phenyl]tetrazolato-\k^2^<i>N</i>:<i>C</i>^5^}bis[bis(trimethylphosphine-\k<i>P</i>)palladium(II)]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1813
_journal_page_last               m1814
_journal_paper_doi               10.1107/S1600536804028260
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Pd2 (C8 H4 N6)2 (C3 H9 P)4]'
_chemical_formula_moiety         'C28 H44 N12 P4 Pd2'
_chemical_formula_sum            'C28 H44 N12 P4 Pd2'
_chemical_formula_weight         885.43
_chemical_name_systematic
;
bis{\m-1-[4-(carbodiimido)phenyl]tetrazolato-\k^2^N:C^5^}
bis[bis(trimethylphosphine-\kP)palladium(II)]
;
_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
_cell_angle_alpha                99.095(19)
_cell_angle_beta                 103.42(2)
_cell_angle_gamma                90.85(2)
_cell_formula_units_Z            1
_cell_length_a                   8.842(3)
_cell_length_b                   9.519(3)
_cell_length_c                   11.996(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      5.12
_cell_volume                     968.4(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1995)'
_computing_data_reduction        'SHELXTL (Siemens, 1997) '
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3615
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0632P)^2^+0.2618P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3039
_reflns_number_total             3374
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6022.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        968.5(5)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               2204796
_cod_database_fobs_code          2204796