Combining the Reactivity Properties of PCy3and PtBu3into a Single Ligand, P(iPr)(tBu)2. Reaction via Mono- or Bisphosphine Palladium(0) Centers and Palladium(I) Dimer Formation
Proutiere, Fabien; Lyngvi, Eirik; Aufiero, Marialuisa; Sanhueza, Italo A.; Schoenebeck, Franziska; Organometallics 33 (2014) 6879–; doi:10.1021/om5009605

data_4084911
_publ_section_title
;
 Combining the Reactivity Properties of PCy3and PtBu3into a Single Ligand,
 P(iPr)(tBu)2. Reaction via Mono- or Bisphosphine Palladium(0) Centers and
 Palladium(I) Dimer Formation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6879
_journal_paper_doi               10.1021/om5009605
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C22 H50 I2 P2 Pd2'
_chemical_formula_sum            'C22 H50 I2 P2 Pd2'
_chemical_formula_weight         843.16
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2014-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                84.7690(10)
_cell_angle_beta                 86.613(2)
_cell_angle_gamma                87.770(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4969(10)
_cell_length_b                   11.1685(11)
_cell_length_c                   12.5738(12)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.47
_cell_volume                     1464.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  ETH_LOC_ApexIID8_Mo
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8811
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.467
_diffrn_reflns_theta_min         2.341
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.453
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0586 before and 0.0290 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0666 before and 0.0289 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 26028 reflections, Rint = 0.0244
 (16760 with I > 3sig(I), Rint = 0.0219)
;
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       irregular
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         8807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7142
_reflns_number_total             8807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5009605_si_003.cif
_cod_data_source_block           sb030914twinn
_cod_depositor_comments
'Adding full bibliography for 4084910--4084911.cif.'
_cod_database_code               4084911
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C12(H12)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              28103
_shelx_hkl_checksum              14790
_olex2_submission_original_sample_id sb030914
_olex2_submission_special_instructions 'No special instructions were received'