Synthesis and Reactivity of Neutral Palladium(II) Alkyl Complexes that Contain Phosphinimine-Arenesulfonate Ligands
Burns, Christopher T.; Shang, Suisheng; Mashuta, Mark S.; Organometallics 34 (2015) 1844–; doi:10.1021/om501262r

data_4085683
_publ_section_title
;
 Synthesis and Reactivity of Neutral Palladium(II) Alkyl Complexes that
 Contain Phosphinimine-Arenesulfonate Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1844
_journal_paper_doi               10.1021/om501262r
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
;
C34 H20 N2 O3 P Pd S, C6, 0.5(C6 H6) 
;
_chemical_formula_sum            'C43 H23 N2 O3 P Pd S'
_chemical_formula_weight         785.06
_chemical_name_common
; 
 K^3^(2-triphenylphosphinimine-5-methylbenzenesulfonate)
 palladium(4-tbutylpyridine) 
;
_chemical_name_systematic
; 
 K^3^(2-triphenylphosphinimine-5-methylbenzenesulfonate)
 palladium(4-tbutylpyridine) 
;
_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
;
 <i>CrysAlis PRO</i> (Agilent, 2013) 
;
_audit_update_record
;
Nov_8_2013 text and data added by Mark S. Mashuta
Dec_9_2014 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                87.010(6)
_cell_angle_beta                 87.005(6)
_cell_angle_gamma                69.223(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3572(6)
_cell_length_b                   11.8341(8)
_cell_length_c                   18.5228(14)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      27.5006
_cell_measurement_theta_min      3.2582
_cell_volume                     1913.9(2)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_data_reduction        '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae<i>et al.</i>, 2006)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -10.00   16.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418   57.0000    0.0000 26

  2 omega  -12.00   88.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418   77.0000 -150.0000 100

  3 omega  -55.00   43.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418  -57.0000  -30.0000 98

  4 omega  -43.00   46.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418  -77.0000   90.0000 89

  5 omega  -43.00   45.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4293   57.0000  -60.0000 88

  6 omega  -20.00   92.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418   77.0000   30.0000 112

  7 omega  -60.00   43.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7418  -57.0000 -150.0000 103

;
_diffrn_measurement_device_type  'Xcalibur Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0201116000
_diffrn_orient_matrix_UB_12      -0.0219740000
_diffrn_orient_matrix_UB_13      -0.0313936000
_diffrn_orient_matrix_UB_21      0.0354241000
_diffrn_orient_matrix_UB_22      0.0340947000
_diffrn_orient_matrix_UB_23      -0.0220559000
_diffrn_orient_matrix_UB_31      0.0701593000
_diffrn_orient_matrix_UB_32      -0.0496948000
_diffrn_orient_matrix_UB_33      0.0005339000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30705
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8824
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0314P)^2^+3.4847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                6946
_reflns_number_total             8824
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om501262r_si_001.cif
_cod_data_source_block           6a
_cod_depositor_comments
'Adding full bibliography for 4085682--4085683.cif.'
_cod_database_code               4085683