Zerovalent [Pd(NHC)(Alkene)1,2] Complexes Bearing Expanded-Ring N-Heterocyclic Carbene Ligands in Transfer Hydrogenation of Alkynes
Hauwert, Peter; Dunsford, Jay J.; Tromp, Dorette S.; Weigand, Jan J.; Lutz, Martin; Cavell, Kingsley J.; Elsevier, Cornelis J.; Organometallics 32 (2013) 131–; doi:10.1021/om300930w

data_4079825
_publ_section_title
;
 Zerovalent [Pd(NHC)(Alkene)1,2] Complexes Bearing Expanded-Ring
 N-Heterocyclic Carbene Ligands in Transfer Hydrogenation of Alkynes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              131
_journal_paper_doi               10.1021/om300930w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C26 H24 N2 O6 Pd, 0.5(C7 H8)'
_chemical_formula_sum            'C29.5 H28 N2 O6 Pd'
_chemical_formula_weight         612.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.4640(8)
_cell_angle_beta                 89.7292(8)
_cell_angle_gamma                79.8575(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4199(3)
_cell_length_b                   10.7383(4)
_cell_length_c                   15.3555(5)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.31
_cell_volume                     1366.19(8)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, Sadabs-2008/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27302
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6207
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.8779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                5919
_reflns_number_total             6207
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300930w_si_002.cif
_cod_data_source_block           l0154a
_cod_original_formula_sum        'C29.50 H28 N2 O6 Pd'
_cod_database_code               4079825