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_7002064
_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 H56 N4 O4, 2(Br), H2O'
_chemical_formula_sum            'C40 H58 Br2 N4 O5'
_chemical_formula_weight         834.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-07-13T21:14:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.091(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.686(3)
_cell_length_b                   15.0391(6)
_cell_length_c                   18.3270(10)
_cell_measurement_reflns_used    20053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5174
_cell_measurement_theta_min      3.3223
_cell_volume                     8270.1(10)
_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      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0157201239
_diffrn_orient_matrix_UB_12      0.0402738592
_diffrn_orient_matrix_UB_13      -0.0095899001
_diffrn_orient_matrix_UB_21      0.0065974948
_diffrn_orient_matrix_UB_22      0.0198701846
_diffrn_orient_matrix_UB_23      0.0213877995
_diffrn_orient_matrix_UB_31      0.0356932954
_diffrn_orient_matrix_UB_32      0.0141045752
_diffrn_orient_matrix_UB_33      -0.0027169468
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.07
_diffrn_reflns_av_unetI/netI     0.1638
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            99530
_diffrn_reflns_theta_full        31
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.77368
_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    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.909
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         28124
_refine_ls_number_restraints     1429
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1185P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.2354
_reflns_number_gt                12625
_reflns_number_total             28124
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908613g.txt
_cod_data_source_block           ps88b
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               7002064