High-Nuclearity Close-Packed Palladium-Nickel Carbonyl Phosphine Clusters: Heteropalladium [Pd16Ni4(CO)22(PPh3)4]2- and [Pd33Ni9(CO)41(PPh3)6]4- Containing Pseudo-Tdccp Pd16Ni4 and Pseudo-D3 hhcp Pd33Ni9 Cores
Masaki Kawano; Jeffrey W. Bacon; Charles F. Campana; Brian E. Winger; James D. Dudek; Scott A. Sirchio; Sabrina L. Scruggs; Urs Geiser; Lawrence F. Dahl; Inorganic Chemistry 40 (2001) 2554–2569; doi:10.1021/ic000979p

data_4319652
_publ_section_title
;
 High-Nuclearity Close-Packed Palladium-Nickel Carbonyl Phosphine
 Clusters: Heteropalladium [Pd16Ni4(CO)22(PPh3)4]2- and
 [Pd33Ni9(CO)41(PPh3)6]4- Containing Pseudo-Tdccp Pd16Ni4 and Pseudo-D3
 hhcp Pd33Ni9 Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2554
_journal_page_last               2569
_journal_paper_doi               10.1021/ic000979p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[Pd12(CO)12(PPh3)6]_2(Me2CO)'
_chemical_formula_sum            'C126 H102 O14 P6 Pd12'
_chemical_formula_weight         3302.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.863(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.1712(1)
_cell_length_b                   23.8035(2)
_cell_length_c                   18.8776(1)
_cell_measurement_reflns_used    8118
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.0
_cell_volume                     5989.03(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT & SADABS '
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measurement_device       'Siemens P4-CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39088
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.085
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.936
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         10652
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      0.915
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1046
_refine_ls_wR_factor_obs         0.0948
_reflns_number_observed          7017
_reflns_number_total             10654
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000979p_3.cif
_cod_data_source_block           dahl48s(Pd12)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0343P)^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^)+(0.0343P)^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        5989.03(7)
_cod_database_code               4319652