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_4319653
_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         '[Ph4P]2[Pd29(CO)28(PPh3)7]_3(MeCN)'
_chemical_formula_sum            'C208 H154 N3 Ni0 O28 P9 Pd29'
_chemical_formula_weight         6507.67
_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
_cell_angle_alpha                82.367(1)
_cell_angle_beta                 79.800(1)
_cell_angle_gamma                67.029(1)
_cell_formula_units_Z            2
_cell_length_a                   20.5934(1)
_cell_length_b                   21.0563(3)
_cell_length_c                   28.3899(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.0
_cell_volume                     11127.5(2)
_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      188(2)
_diffrn_measurement_device       'Siemens P4-CCD'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39477
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         0.73
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             6232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.803
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.186
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           'blocked cycle'
_refine_ls_number_parameters     2087
_refine_ls_number_reflns         25512
_refine_ls_number_restraints     1320
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_obs          0.1136
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+896.5696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2792
_refine_ls_wR_factor_obs         0.2404
_reflns_number_observed          19616
_reflns_number_total             25523
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000979p_4.cif
_cod_data_source_block           dahl24f(Pd29)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0333P)^2^+896.5696P] 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^)+(0.0333P)^2^+896.5696P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319653