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_7002063
_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
;
C46 H56 Br2 N4 O4 Pd, 5/2(C6 H6), C2 H3 N
;
_chemical_formula_sum            'C63 H74 Br2 N5 O4 Pd'
_chemical_formula_weight         1231.49
_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             2009-07-15T14:07:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.53(2)
_cell_angle_beta                 80.84(2)
_cell_angle_gamma                73.94(2)
_cell_formula_units_Z            4
_cell_length_a                   17.652(5)
_cell_length_b                   18.280(5)
_cell_length_c                   18.705(5)
_cell_measurement_reflns_used    35551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9903
_cell_measurement_theta_min      2.5844
_cell_volume                     5703(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET)
(compiled Mar 6 2006,22:55:04)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET)
(compiled Mar 6 2006,22:55:04)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET)
(compiled Mar 6 2006,22:55:04)
;
_computing_molecular_graphics    OrtepII
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0287441416
_diffrn_orient_matrix_UB_12      0.0252561588
_diffrn_orient_matrix_UB_13      0.0224998473
_diffrn_orient_matrix_UB_21      0.006096327
_diffrn_orient_matrix_UB_22      -0.0278806461
_diffrn_orient_matrix_UB_23      0.0298057507
_diffrn_orient_matrix_UB_31      0.0301650098
_diffrn_orient_matrix_UB_32      0.014951982
_diffrn_orient_matrix_UB_33      0.0085735015
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_unetI/netI     0.2138
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            152638
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         32
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET)
(compiled Mar 6 2006,22:55:04)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          .43
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .07
_refine_diff_density_max         7.177
_refine_diff_density_min         -2.925
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         35791
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.2099
_refine_ls_R_factor_gt           0.123
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1955P)^2^+62.2856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.348
_refine_ls_wR_factor_ref         0.3772
_reflns_number_gt                16905
_reflns_number_total             35791
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908613g.txt
_cod_data_source_block           dhb238
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               7002063