Synthesis and reactivity of alkyl-palladium N-heterocyclic carbene complexes.
Esposito, Oriana; Lewis, Alexandra K de K; Hitchcock, Peter B; Caddick, Stephen; Cloke, F Geoffrey N; Chemical communications (Cambridge, England)  (2007) 1157–1159; doi:10.1039/b700671c

data_7101796
_publ_section_title
;
 Synthesis and reactivity of alkyl-palladium N-heterocyclic carbene
 complexes.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1157
_journal_page_last               1159
_journal_paper_doi               10.1039/b700671c
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C64 H94 Cl2 N4 Pd2, 2(C4 H10 O)'
_chemical_formula_sum            'C72 H114 Cl2 N4 O2 Pd2'
_chemical_formula_weight         1351.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-03-03T15:28:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.288(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4708(6)
_cell_length_b                   17.9840(7)
_cell_length_c                   19.0590(5)
_cell_measurement_reflns_used    15174
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     7392.9(4)
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.335063E-1
_diffrn_orient_matrix_UB_12      -0.199758E-1
_diffrn_orient_matrix_UB_13      0.420605E-1
_diffrn_orient_matrix_UB_21      0.306006E-1
_diffrn_orient_matrix_UB_22      0.340447E-1
_diffrn_orient_matrix_UB_23      -0.127222E-1
_diffrn_orient_matrix_UB_31      -0.95106E-2
_diffrn_orient_matrix_UB_32      0.391642E-1
_diffrn_orient_matrix_UB_33      0.325123E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24839
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.9244
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.774
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.043
_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^)+(0.0783P)^2^+50.0248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                5451
_reflns_number_total             7207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700671c.txt
_cod_data_source_block           mar606
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7101796