Dative Pd(0)-Mo(II) Bonds in a Linearly Aligned Tetrametal System: Preparation, Characterization, and Reaction of a Tetranuclear Pd(0)-Mo(II)-Mo(II)-Pd(0) Supported by Four 6-Diphenylphosphino-2-pyridonate Ligands
Kazushi Mashima; Atsushi Fukumoto; Hiroshi Nakano; Yutaka Kaneda; Kazuhide Tani; Akira Nakamura; Journal of the American Chemical Society 120 (1998) 12151–12152; doi:10.1021/ja9817702

data_4116893
_publ_section_title
;
 Dative Pd(0)-Mo(II) Bonds in a Linearly Aligned Tetrametal System:
 Preparation, Characterization, and Reaction of a Tetranuclear
 Pd(0)-Mo(II)-Mo(II)-Pd(0) Supported by Four
 6-Diphenylphosphino-2-pyridonate Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12151
_journal_page_last               12152
_journal_paper_doi               10.1021/ja9817702
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C92 H76 Mo2 N12 O7 P4 Pd2'
_chemical_formula_weight         1990.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Thu Feb 26 19:32:35 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90.24(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.844(7)
_cell_length_b                   21.276(7)
_cell_length_c                   30.941(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      14.2
_cell_volume                     9772(6)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00891
_diffrn_orient_matrix_UB_12      -0.01964
_diffrn_orient_matrix_UB_13      0.02903
_diffrn_orient_matrix_UB_21      0.00664
_diffrn_orient_matrix_UB_22      0.04215
_diffrn_orient_matrix_UB_23      0.01396
_diffrn_orient_matrix_UB_31      -0.06645
_diffrn_orient_matrix_UB_32      0.00684
_diffrn_orient_matrix_UB_33      -0.00263
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            23312
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -1.04
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4016.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.970
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     529
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         3.0590
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0500
_reflns_number_observed          4249
_reflns_number_total             8483
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ja9817702_1.cif
_cod_data_source_block           Mo2Pd2(pyphos)4(tcne)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' 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) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9771(4)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C92 H76 N12 Mo2 O7 P4 Pd2 '
_cod_database_code               4116893