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_4117996
_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            'C23 H41 Cl7 O P2 Pd'
_chemical_formula_weight         750.05
_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                 92.988(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.277(3)
_cell_length_b                   18.368(6)
_cell_length_c                   17.318(5)
_cell_measurement_reflns_used    11241
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.8261
_cell_measurement_theta_min      1.9844
_cell_volume                     3264.6(17)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury 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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21143
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  0.7045
_exptl_absorpt_correction_T_min  0.5725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       Block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+3.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                5226
_reflns_number_total             5692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303507t_si_003.cif
_cod_data_source_block           ii-152-2
_cod_original_cell_volume        3264.5(17)
_cod_database_code               4117996