Ligand-Induced Reductive Elimination of Ethane from Azopyridine Palladium Dimethyl Complexes.
Rudenko, Andrey E.; Clayman, Naomi E.; Walker, Katherine L.; Maclaren, Jana K.; Zimmerman, Paul M.; Waymouth, Robert M.; Journal of the American Chemical Society 140 (2018) 11408–11415; doi:10.1021/jacs.8b06398

data_4132779
_publ_section_title
;
 Ligand-Induced Reductive Elimination of Ethane from Azopyridine Palladium
 Dimethyl Complexes.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11408
_journal_page_last               11415
_journal_paper_doi               10.1021/jacs.8b06398
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C15 H16 F3 N3 Pd'
_chemical_formula_sum            'C15 H16 F3 N3 Pd'
_chemical_formula_weight         401.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                113.946(2)
_cell_angle_beta                 91.188(2)
_cell_angle_gamma                96.721(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1493(5)
_cell_length_b                   10.1574(7)
_cell_length_c                   10.6196(8)
_cell_measurement_reflns_used    7209
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.154
_cell_measurement_theta_min      2.345
_cell_volume                     795.61(10)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon100'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17582
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.887
_diffrn_reflns_theta_max         25.887
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0492 before and 0.0392 after correction. 
The Ratio of minimum to maximum transmission is 0.9333. 
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2685
_reflns_number_total             3070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06398_si_004.cif
_cod_data_source_block           arda_a
_cod_original_cell_volume        795.60(10)
_cod_database_code               4132779
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.874
_shelx_res_checksum              59366
_shelx_hkl_checksum              63085