Facial Tridentate Ligands for Stabilizing Palladium(IV) Complexes
Maleckis, Ansis; Sanford, Melanie S.; Organometallics 30 (2011) 6617–; doi:10.1021/om200779j

data_4065412
_publ_section_title
;
 Facial Tridentate Ligands for Stabilizing Palladium(IV) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6617
_journal_paper_doi               10.1021/om200779j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C29 H29 Cl F3 N3 O2 Pd S, 2(C2 H3 N)'
_chemical_formula_sum            'C33 H35 Cl F3 N5 O2 Pd S'
_chemical_formula_weight         764.57
_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                67.070(5)
_cell_angle_beta                 78.111(5)
_cell_angle_gamma                73.844(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9337(2)
_cell_length_b                   13.4448(3)
_cell_length_c                   14.1447(10)
_cell_measurement_reflns_used    18798
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      3.40
_cell_volume                     1660.93(15)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotting anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34052
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    6.306
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         5929
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+2.0101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                5842
_reflns_number_total             5929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200779j_si_001.cif
_cod_data_source_block           complex_12
_cod_original_cell_volume        1660.93(13)
_cod_database_code               4065412