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_7002067
_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, 2.5(C6 H6)'
_chemical_formula_sum            'C55 H69 Br2 N4 O4 Pd'
_chemical_formula_weight         1116.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_date             2009-07-14T09:05:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.149(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.2399(9)
_cell_length_b                   20.8844(4)
_cell_length_c                   20.5822(4)
_cell_measurement_reflns_used    5884
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.0692
_cell_measurement_theta_min      2.6537
_cell_volume                     11708.9(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0312483853
_diffrn_orient_matrix_UB_12      -0.0299497138
_diffrn_orient_matrix_UB_13      0.0544742582
_diffrn_orient_matrix_UB_21      -0.044582388
_diffrn_orient_matrix_UB_22      0.04039439
_diffrn_orient_matrix_UB_23      -0.0216581
_diffrn_orient_matrix_UB_31      -0.0161952573
_diffrn_orient_matrix_UB_32      -0.0540486765
_diffrn_orient_matrix_UB_33      -0.0464855023
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67877
_diffrn_reflns_theta_full        67.74
_diffrn_reflns_theta_max         67.74
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    4.489
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         2.451
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10449
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.073
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                3743
_reflns_number_total             10449
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908613g.txt
_cod_data_source_block           ps97
_cod_database_code               7002067