Isolation and reactivity of palladium hydrido complexes: intermediates in the hydrodefluorination of pentafluoropyridine.
Breyer, David; Braun, Thomas; Penner, Anna; Dalton transactions (Cambridge, England : 2003) 39 (2010) 7513–7520; doi:10.1039/c0dt00086h

data_7025974
_publ_section_title
;
 Isolation and reactivity of palladium hydrido complexes: intermediates in
 the hydrodefluorination of pentafluoropyridine.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7513
_journal_page_last               7520
_journal_paper_doi               10.1039/c0dt00086h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C25 H45 F4 N2 P2 Pd, B F4'
_chemical_formula_sum            'C25 H45 B F8 N2 P2 Pd'
_chemical_formula_weight         704.78
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.560(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3812(4)
_cell_length_b                   8.1047(2)
_cell_length_c                   37.4697(16)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      1.94
_cell_volume                     3125.2(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,220 exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15491
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.9209
_exptl_absorpt_correction_T_min  0.7503
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After
that a numerical absorption correction basing on a Gaussian algorithsm
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.801
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                6522
_reflns_number_total             8573
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c0dt00086h.txt
_cod_data_source_block           complex6b_\anna\david16
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7025974