High-nuclearity [Pd13Ni13(CO)34]4− containing a 26-atom Pd13Ni13 core with an unprecedented five-layer close-packed triangular stacking geometry: possible substitutional Pd/Ni crystal disorder at specific intralayer nickel sites †
Tran, Nguyet T.; Kawano, Masaki; Powell, Douglas R.; Dahl, Lawrence F.; Journal of the Chemical Society, Dalton Transactions  (2000) 4138–; doi:10.1039/b004595k

data_7009948
_publ_section_title
;
 High-nuclearity [Pd13Ni13(CO)34]4&#x2212; containing a 26-atom
 Pd13Ni13 core with an unprecedented five-layer close-packed triangular
 stacking geometry: possible substitutional Pd/Ni crystal disorder at
 specific intralayer nickel sites&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4138
_journal_paper_doi               10.1039/b004595k
_journal_year                    2000
_chemical_formula_moiety
'4(Ph4P)+ [Pd13.45 Ni12.55 (CO)34]4- 0.5(CH3CN)'
_chemical_formula_sum            'C131 H81.5 N0.5 Ni12.55 O34 P4 Pd13.45'
_chemical_formula_weight         4498.48
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.43
_cell_angle_beta                 87.58
_cell_angle_gamma                70.60
_cell_formula_units_Z            2
_cell_length_a                   17.226
_cell_length_b                   17.937
_cell_length_c                   22.82800(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     6594.99(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'Siemens P4/ccd'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41393
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.04
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    3.648
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4346
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.359
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1761
_refine_ls_number_reflns         22169
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0316P)^2^+45.3564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                18263
_reflns_number_total             22169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004595k.txt
_cod_data_source_block           dahl33f
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        6595.00(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C131 H81.50 N0.50 Ni12.55 O34 P4 Pd13.45'
_cod_database_code               7009948