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_4083148
_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 N P2 Pd'
_chemical_formula_sum            'C23 H43 N P2 Pd'
_chemical_formula_weight         501.92
_chemical_name_common            wdb_1_113
_chemical_name_systematic
;
 wdb_1_113
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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      2.4
_audit_creation_date             2013-01-24T14:07:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.021(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3997(13)
_cell_length_b                   11.3514(15)
_cell_length_c                   23.623(3)
_cell_measurement_reflns_used    270
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2520.6(6)
_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 0.977
_diffrn_measured_fraction_theta_max 0.973
_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  0.1434
_diffrn_reflns_av_unetI/netI     0.1536
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26610
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.9336
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.712
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1824
_reflns_number_gt                2841
_reflns_number_total             4530
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500054f_si_002.cif
_cod_data_source_block           (PNP*)PdH_compound_1
_cod_depositor_comments
'Adding full bibliography for 4083148--4083151.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083148