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_7002066
_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, 0.84(C H Cl3)'
_chemical_formula_sum            'C40.84 H54.84 Br2 Cl2.53 N4 O4 Pd'
_chemical_formula_weight         1021.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-07-14T12:20:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.190(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4781(5)
_cell_length_b                   9.9160(2)
_cell_length_c                   25.6217(7)
_cell_measurement_reflns_used    10784
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.9929
_cell_measurement_theta_min      2.6153
_cell_volume                     4782.4(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0197690825
_diffrn_orient_matrix_UB_12      0.0304385822
_diffrn_orient_matrix_UB_13      0.0265427466
_diffrn_orient_matrix_UB_21      0.012921515
_diffrn_orient_matrix_UB_22      -0.0641396033
_diffrn_orient_matrix_UB_23      0.0116976383
_diffrn_orient_matrix_UB_31      0.0292345035
_diffrn_orient_matrix_UB_32      0.0076625078
_diffrn_orient_matrix_UB_33      -0.0079220113
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44053
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    2.241
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.12
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10634
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.134
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+21.2762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2248
_reflns_number_gt                5718
_reflns_number_total             10634
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908613g.txt
_cod_data_source_block           ps93f4
_cod_original_sg_symbol_Hall     -p_2yc
_cod_database_code               7002066