Chiral 2,6-lutidinyl-biscarbene complexes of palladium
Tulloch, Arran A. D.; Danopoulos, Andreas A.; Tizzard, Graham J.; Coles, Simon J.; Hursthouse, Michael B.; Hay-Motherwell, Robyn S.; Motherwell, William B.; Chemical Communications  (2001) 1270–; doi:10.1039/b103330c

data_7115006
_publ_section_title
;
 Chiral 2,6-lutidinyl-biscarbene complexes of palladium
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1270
_journal_paper_doi               10.1039/b103330c
_journal_year                    2001
_chemical_formula_moiety         'C36 H41 Cl4.50 N5 Pd1'
_chemical_formula_sum            'C36 H41 Cl4.5 N5 Pd'
_chemical_formula_weight         809.66
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.077(3)
_cell_angle_beta                 83.364(3)
_cell_angle_gamma                71.322(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4782(4)
_cell_length_b                   11.8790(6)
_cell_length_c                   20.8146(11)
_cell_measurement_reflns_used    14147
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.86
_cell_volume                     1917.65(17)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo a. Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '9.091 pixels/mm'
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14147
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.9597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SORTAV (Blessing, 1995-1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             829
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.730
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          14.249
_refine_ls_shift/su_mean         0.325
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1574P)^2^+7.8887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2213
_refine_ls_wR_factor_ref         0.2562
_reflns_number_gt                4241
_reflns_number_total             6524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103330c.txt
_cod_data_source_block           00skl044
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C36 H41 Cl4.50 N5 Pd'
_cod_database_code               7115006