Direct observation of a carbonylation reaction relevant to CO/alkene copolymerization in a methylpalladium carbonyl complex containing a bis(N-heterocyclic carbene) ligand
Subramanium, Sri S.; Slaughter, LeGrande M.; Dalton Transactions  (2009) 6930–; doi:10.1039/b908689g

data_7002094
_publ_section_title
;
 Direct observation of a carbonylation reaction relevant to CO/alkene
 copolymerization in a methylpalladium carbonyl complex containing a
 bis(N-heterocyclic carbene) ligand
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              6930
_journal_paper_doi               10.1039/b908689g
_journal_year                    2009
_chemical_formula_moiety         'C27 H31 N4 O Pd, C H2 Cl2, B F4'
_chemical_formula_sum            'C28 H33 B Cl2 F4 N4 O Pd'
_chemical_formula_weight         705.69
_chemical_name_common            (Pd(DIMesMe)(CO)(CH3))(BF4)
_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                101.273(4)
_cell_angle_beta                 101.577(4)
_cell_angle_gamma                96.190(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3442(5)
_cell_length_b                   14.0019(9)
_cell_length_c                   15.7474(10)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.71
_cell_volume                     1537.46(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (XP)'
_computing_publication_material  'Bruker SHELXTL (XCIF)'
_computing_structure_refinement  'Bruker SHELXTL (XL)'
_computing_structure_solution    'Bruker SHELXTL (XS)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21988
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.35
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        N/A
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.8069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_recrystallization_method
'slow diff of hexane into diethyl ether/dichloromethane soln'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.374
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0586P)^2^+2.8491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                5179
_reflns_number_total             5799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908689g.txt
_cod_data_source_block           cmplx6_form1_lms195
_cod_original_cell_volume        1537.46(17)
_cod_database_code               7002094