Synthesis of Functional Polyolefins Using Cationic Bisphosphine Monoxide-Palladium Complexes
Brad P. Carrow; Kyoko Nozaki; Journal of the American Chemical Society 134 (2012) 8802–8805; doi:10.1021/ja303507t

data_4117995
_publ_section_title
;
 Synthesis of Functional Polyolefins Using Cationic Bisphosphine
 Monoxide-Palladium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8802
_journal_page_last               8805
_journal_paper_doi               10.1021/ja303507t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C28 H44 F6 N O2 P2 Pd Sb'
_chemical_formula_weight         830.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.728(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.515(4)
_cell_length_b                   19.977(7)
_cell_length_c                   15.190(5)
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.8805
_cell_measurement_theta_min      1.7259
_cell_volume                     3363(2)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'RIGAKU/MSC Mercury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21808
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.8652
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.621
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0667P)^2^+9.5837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                5098
_reflns_number_total             5916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303507t_si_002.cif
_cod_data_source_block           iii-105
_cod_database_code               4117995