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_7030117
_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 H26 P2 Pd'
_chemical_formula_sum            'C14 H26 P2 Pd'
_chemical_formula_weight         362.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 107.991(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.782(2)
_cell_length_b                   18.624(3)
_cell_length_c                   10.664(2)
_cell_measurement_reflns_used    12390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.49
_cell_volume                     1658.9(6)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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     0.77488
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17001
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         26.22
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+2.3621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                2152
_reflns_number_total             2520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31086d.txt
_cod_data_source_block           c:\Complex_1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7030117
_thetm01_alert_3_b
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PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5702

RESPONSE: The resolution limitation is due to the size of the detector at the Australian synchrotron
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