Zerovalent N-Heterocyclic Carbene Complexes of Palladium and Nickel Dimethyl Fumarate: Synthesis, Structure, and Dynamic Behavior
Clement, Nicolas D.; Cavell, Kingsley J.; Ooi, Li-ling; Organometallics 25 (2006) 4155–; doi:10.1021/om0602759

data_4075433
_publ_section_title
;
 Zerovalent N-Heterocyclic Carbene Complexes of Palladium and Nickel
 Dimethyl Fumarate:&#x00A0; Synthesis, Structure, and Dynamic Behavior
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4155
_journal_paper_doi               10.1021/om0602759
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C66 H72 N4 Ni O4'
_chemical_formula_weight         1043.99
_chemical_name_common            kjc0407
_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_method           SHELXL-97
_cell_angle_alpha                116.8790(10)
_cell_angle_beta                 91.5910(10)
_cell_angle_gamma                97.8850(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2286(2)
_cell_length_b                   17.0906(2)
_cell_length_c                   18.8608(3)
_cell_measurement_reflns_used    49606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2898.02(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Dirdif 99 (Beurskens, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60692
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.9698
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         13032
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+2.6723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                9303
_reflns_number_total             13032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0602759si20060618_090404.cif
_cod_data_source_block           kjc0407
_cod_original_cell_volume        2898.01(8)
_cod_database_code               4075433