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_4085682
_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         'C35 H37 N2 O3 P Pd S'
_chemical_formula_sum            'C35 H37 N2 O3 P Pd S'
_chemical_formula_weight         703.10
_chemical_name_common
; 
K^2^(2-triphenylphosphinimine-5-methylbenzenesulfonate)
 palladium(methyl)(4-tbutylpyridine)
;
_chemical_name_systematic
; 
 K^2^(2-triphenylphosphinimine-5-methylbenzenesulfonate)
 palladium(methyl)(4-tbutylpyridine) 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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
;
May_17_2012 text and data added by Mark S. Mashuta
Sept_2_2012 text and data added by Mark S. Mashuta
Dec_9_2014 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.86211(17)
_cell_length_b                   17.52994(15)
_cell_length_c                   21.0147(2)
_cell_measurement_reflns_used    36170
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      30.6634
_cell_measurement_theta_min      3.2048
_cell_volume                     6580.16(10)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_reduction        '<i>CrysAlis PRO</i> (Agilent, 2010)'
_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      100.0
_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  -13.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953   57.0000    0.0000 105

  2 omega   -7.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953   77.0000 -150.0000 108

  3 omega  -28.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953  -57.0000   90.0000 26

  4 omega   23.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953  -57.0000   90.0000 26

  5 omega   -8.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953   77.0000   90.0000 109

  6 omega  -66.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953  -77.0000   30.0000 120

  7 omega  -60.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953  -57.0000  120.0000 110

  8 omega  -18.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953   77.0000  120.0000 120

  9 omega  -15.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953   57.0000  -90.0000 77

 10 omega  -60.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8953  -57.0000 -120.0000 110

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8871
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.109
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         8871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+1.6771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                6867
_reflns_number_total             8871
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om501262r_si_001.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085682--4085683.cif.
;
_cod_original_cell_volume        6580.15(11)
_cod_database_code               4085682