Synthesis and Characterization of Anionic, Neutral, and Cationic PNP Pincer PdIIand PtIIHydrides
Bailey, Wilson D.; Kaminsky, Werner; Kemp, Richard A.; Goldberg, Karen I.; Organometallics 33 (2014) 2503–; doi:10.1021/om500054f

data_4083149
_publ_section_title
;
 Synthesis and Characterization of Anionic, Neutral, and Cationic PNP
 Pincer PdIIand PtIIHydrides
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2503
_journal_paper_doi               10.1021/om500054f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C23 H43.92 Cl0.09 N P2 Pd, C F3 O3 S'
_chemical_formula_sum            'C24 H43.915 Cl0.085 F3 N O3 P2 Pd S'
_chemical_formula_weight         654.93
_chemical_name_common            wdb_1_163
_chemical_name_systematic
;
 wdb_1_163
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-01-17T12:16:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                83.144(4)
_cell_angle_beta                 81.714(5)
_cell_angle_gamma                83.180(4)
_cell_formula_units_Z            8
_cell_length_a                   15.0598(15)
_cell_length_b                   15.4771(14)
_cell_length_c                   25.655(3)
_cell_measurement_reflns_used    552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5843.5(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            272155
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.8955
_exptl_absorpt_correction_T_min  0.8664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2715
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.226
_refine_diff_density_min         -1.16
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         29404
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+8.4745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.076
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                24901
_reflns_number_total             29404
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500054f_si_002.cif
_cod_data_source_block           '[(PNP)PdH]OTf_compound_2'
_cod_depositor_comments
'Adding full bibliography for 4083148--4083151.cif.'
_cod_original_cell_volume        5843.6(10)
_cod_database_code               4083149