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_7105807
_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
'2(C44 H44 Cl N2 P2 Pd 1+),2(B F4 1-),5(C H2 Cl2)'
_chemical_formula_sum            'C93 H98 B2 Cl12 F8 N4 P4 Pd2'
_chemical_formula_weight         2207.45
_chemical_name_systematic
;
N-methyl-3-(dimethylamino-methylidenyl)-4,5-dihydropyrrolyliden-2-yl-
bis-(triphenylphosphine)-chloro-palladium(ii) tetrafluoroborate
tris-dichloromethane solute
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                AVM-AB-407-01
_audit_creation_date             2010-07-06
_cell_angle_alpha                90.00
_cell_angle_beta                 125.390(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.7088(4)
_cell_length_b                   16.8288(2)
_cell_length_c                   23.4760(3)
_cell_measurement_reflns_used    278975
_cell_measurement_temperature    160
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.91
_cell_volume                     10534.7(3)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            115104
_diffrn_reflns_theta_full        33.19
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         6.81
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.87787
_exptl_absorpt_correction_T_min  0.76729
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             4488
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.272
_refine_diff_density_min         -1.906
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         19883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1208P)^2^+48.4188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                16131
_reflns_number_total             19883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03128C.TXT
_cod_data_source_block           4
_cod_original_cell_volume        10534.7(2)
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_database_code               7105807