Palladium complexes of o-xylyl-linked alkoxybenzimidazolin-2-ylidenes: interesting structural conformations and application as pre-catalysts
Baker, Murray V.; Brown, David H.; Simpson, Peter V.; Skelton, Brian W.; White, Allan H.; Dalton Transactions  (2009) 7294–; doi:10.1039/b908613g

data_7002068
_publ_section_title
;
 Palladium complexes of o-xylyl-linked alkoxybenzimidazolin-2-ylidenes:
 interesting structural conformations and application as pre-catalysts
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7294
_journal_paper_doi               10.1039/b908613g
_journal_year                    2009
_chemical_formula_moiety         'C40 H54 Br2 N4 O4 Pd,2(C2 H6 O S), C H Cl3'
_chemical_formula_sum            'C45 H67 Br2 Cl3 N4 O6 Pd S2'
_chemical_formula_weight         1196.72
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-07-14T11:19:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.016(4)
_cell_angle_beta                 86.629(5)
_cell_angle_gamma                72.488(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1456(7)
_cell_length_b                   14.5636(6)
_cell_length_c                   16.8254(10)
_cell_measurement_reflns_used    9271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.9245
_cell_measurement_theta_min      2.8355
_cell_volume                     2627.0(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    ORTEP2
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0347610204
_diffrn_orient_matrix_UB_12      -0.1177943373
_diffrn_orient_matrix_UB_13      0.0526028659
_diffrn_orient_matrix_UB_21      0.0247013914
_diffrn_orient_matrix_UB_22      -0.0208355232
_diffrn_orient_matrix_UB_23      -0.0833653923
_diffrn_orient_matrix_UB_31      0.126322923
_diffrn_orient_matrix_UB_32      -0.0012851917
_diffrn_orient_matrix_UB_33      0.0084520724
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32223
_diffrn_reflns_theta_full        67.23
_diffrn_reflns_theta_max         67.23
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    7.162
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.2621
_exptl_crystal_size_mid          0.0469
_exptl_crystal_size_min          0.0205
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         9288
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.063
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1245P)^2^+0.3208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                6622
_reflns_number_total             9288
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908613g.txt
_cod_data_source_block           ps97x
_cod_original_cell_volume        2627.0(2)
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               7002068