Synthetic and computational studies of the palladium(IV) system Pd(alkyl)(aryl)(alkynyl)(bidentate)(triflate) exhibiting selectivity in C-C reductive elimination.
Sharma, Manab; Ariafard, Alireza; Canty, Allan J.; Yates, Brian F.; Gardiner, Michael G.; Jones, Roderick C.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11820–11828; doi:10.1039/c2dt31086d

data_7030119
_publ_section_title
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 Synthetic and computational studies of the palladium(IV) system
 Pd(alkyl)(aryl)(alkynyl)(bidentate)(triflate) exhibiting selectivity in
 C-C reductive elimination.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11820
_journal_page_last               11828
_journal_paper_doi               10.1039/c2dt31086d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C14 H16 N2 O Pd'
_chemical_formula_sum            'C14 H16 N2 O Pd'
_chemical_formula_weight         334.69
_chemical_name_systematic
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?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97
_cell_angle_alpha                84.0070(10)
_cell_angle_beta                 80.678(5)
_cell_angle_gamma                79.390(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6740(7)
_cell_length_b                   9.1480(7)
_cell_length_c                   9.4860(6)
_cell_measurement_reflns_used    6461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.98
_cell_volume                     643.99(9)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)'
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'synchrotron BM'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.77487
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6554
_diffrn_reflns_theta_full        26.23
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.082(8)
_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   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0497P)^2^+1.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1694
_reflns_number_total             1750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31086d.txt
_cod_data_source_block           c:\Complex_11
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7030119
_plat029_alert_3_a
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PROBLEM: diffrn measured fraction theta full Low ....... 0.88

RESPONSE: This is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection
with a fixed detector and affects some high angle data
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