Reductive Elimination of Alkanes and Arenes from [Pd2R2(μ-H)(μ-dppm)2]PF6 Complexes
Robert A. Stockland; Gordon K. Anderson; Nigam P. Rath; Journal of the American Chemical Society 121 (1999) 7945–7946; doi:10.1021/ja990815b

data_4116503
_publ_section_title
;
 Reductive Elimination of Alkanes and Arenes from
 [Pd2R2(\m-H)(\m-dppm)2]PF6 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7945
_journal_page_last               7946
_journal_paper_doi               10.1021/ja990815b
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C32.5 H31 B0.5 N0.5 P2 Pd'
_chemical_formula_weight         602.32
_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                106.587(1)
_cell_angle_beta                 93.100(1)
_cell_angle_gamma                116.809(1)
_cell_formula_units_Z            2
_cell_length_a                   11.5028(1)
_cell_length_b                   12.4083(1)
_cell_length_c                   12.4609(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.0
_cell_volume                     1486.17(4)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            44293
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_number         'CCD data, see expt'
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   'empirical, sadabs'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plates
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_obs          0.0436
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1445
_refine_ls_wR_factor_obs         0.1181
_reflns_number_observed          5173
_reflns_number_total             7148
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990815b.cif
_cod_data_source_block           a11897s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^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^)+(0.0800P)^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        1486.16(3)
_cod_original_formula_sum        'C32.50 H31 B0.50 N0.50 P2 Pd'
_cod_database_code               4116503