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_4083151
_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 Cl N P2 Pd, C F3 O3 S'
_chemical_formula_sum            'C24 H43 Cl F3 N O3 P2 Pd S'
_chemical_formula_weight         686.44
_chemical_name_common            wdb_1_125
_chemical_name_systematic
;
 wdb_1_125
;
_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             2013-05-03T12:57:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.643(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0998(12)
_cell_length_b                   9.8492(10)
_cell_length_c                   24.725(3)
_cell_measurement_reflns_used    315
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2946.4(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 1
_diffrn_measured_fraction_theta_max 0.996
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            121179
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.9632
_exptl_absorpt_correction_T_min  0.8334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       icicle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+3.3838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.057
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                6256
_reflns_number_total             7391
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500054f_si_002.cif
_cod_data_source_block           '[(PNP)PdCl]OTf_compound_8'
_cod_depositor_comments
'Adding full bibliography for 4083148--4083151.cif.'
_cod_original_cell_volume        2946.3(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083151