Metal complexes with carbene ligands stabilized by lateral enamines
Manuel Alcarazo; Karin Radkowski; Richard Goddard; Alois Furstner; Chem.Commun. 47 (2011) 776–; doi:10.1039/c0cc03128c

data_7105810
_publ_section_title
;
 Metal complexes with carbene ligands stabilized by lateral enamines
;
_journal_name_full               Chem.Commun.
_journal_page_first              776
_journal_paper_doi               10.1039/c0cc03128c
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        dichloromethane/diethylether
_chemical_formula_moiety         'C47 H48 Cl N2 P2 Pd 1+, C H2 Cl2, B F4 1-'
_chemical_formula_sum            'C48 H50 B Cl3 F4 N2 P2 Pd'
_chemical_formula_weight         1016.40
_chemical_name_systematic
;
2,5-di-(dimethyl-aminomethylidenyl)-cylcopentan-1-ylidene-chloro-
bis(triphenylphosphine)palladium(ii) tetrafluoroborate
dichloromethane solute
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                RKI-RE-150-01
_audit_creation_date             2010-07-29
_cell_angle_alpha                90.00
_cell_angle_beta                 134.308(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1142(25)
_cell_length_b                   19.5329(32)
_cell_length_c                   21.5750(26)
_cell_measurement_reflns_used    251834
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.45
_cell_volume                     4558.0(13)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            251840
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         36.72
_diffrn_reflns_theta_min         6.80
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'TWINABS (Bruker AXS, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.772
_refine_diff_density_min         -2.330
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         23291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0760P)^2^+1.2421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                18801
_reflns_number_total             23291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03128C.TXT
_cod_data_source_block           7
_cod_original_cell_volume        4557.9(13)
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7105810