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_4083150
_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 H43.90 Cl0.11 N P2 Pt, C F3 O3 S'
_chemical_formula_sum            'C24 H43.9 Cl0.11 F3 N O3 P2 Pt S'
_chemical_formula_weight         744.39
_chemical_name_common            wdb_2_56
_chemical_name_systematic
;
 wdb_2_56
;
_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             2013-09-17T12:25:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                106.715(7)
_cell_angle_beta                 92.145(7)
_cell_angle_gamma                96.467(7)
_cell_formula_units_Z            6
_cell_length_a                   15.062(2)
_cell_length_b                   15.441(2)
_cell_length_c                   19.890(3)
_cell_measurement_reflns_used    581
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     4390.4(11)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0956
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21855
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.029
_exptl_absorpt_correction_T_max  0.6891
_exptl_absorpt_correction_T_min  0.4328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chard
_exptl_crystal_F_000             2231
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.462
_refine_diff_density_min         -2.199
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         21855
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                19566
_reflns_number_total             21855
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500054f_si_002.cif
_cod_data_source_block           '[(PNP)PtH]OTf_compound_5'
_cod_depositor_comments
;
Adding full bibliography for 4083148--4083151.cif.

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         2233.48
_cod_original_formula_moiety      '3(C23 H43.90 Cl0.11 N P2 Pt), 3(C F3 O3 S)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4390.5(12)
_cod_original_formula_sum        'C72 H131.70 Cl0.33 F9 N3 O9 P6 Pt3 S3'
_cod_database_code               4083150