Modular Chelated Palladium Diaminocarbene Complexes: Synthesis, Characterization, and Optimization of Catalytic Suzuki−Miyaura Cross-Coupling Activity by Ligand Modification
Moncada, Adriana I.; Manne, Sudhakar; Tanski, Joseph M.; Slaughter, LeGrande M.; Organometallics 25 (2006) 491–; doi:10.1021/om050786f

data_4074675
_publ_section_title
;
 Modular Chelated Palladium Diaminocarbene Complexes:&#x00A0; Synthesis,
 Characterization, and Optimization of Catalytic Suzuki&#x2212;Miyaura
 Cross-Coupling Activity by Ligand Modification
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              491
_journal_paper_doi               10.1021/om050786f
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C8 H18 Br2 N4 Pd, 2(C2 H6 O S)'
_chemical_formula_sum            'C12 H30 Br2 N4 O2 Pd S2'
_chemical_formula_weight         592.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                74.7190(10)
_cell_angle_beta                 62.9710(10)
_cell_angle_gamma                62.2700(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8099(8)
_cell_length_b                   11.3178(9)
_cell_length_c                   11.3765(9)
_cell_measurement_reflns_used    5628
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      3.2
_cell_volume                     1095.03(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13623
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_T_max  0.6509
_exptl_absorpt_correction_T_min  0.3148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker(2001)SADABS,BrukerAXSInc.,Madison,WI
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method
'Slow diff of ether into DMSO soln of cmpd'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0042(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.6424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                5016
_reflns_number_total             5148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050786fsi20050911_103409.cif
_cod_data_source_block           lms_3b
_cod_original_cell_volume        1095.04(15)
_cod_database_code               4074675