Dynamic behaviour of monohaptoallylpalladium species: internal coordination as a driving force in allylic alkylation chemistry
Xie, Lan-Gui; Bagutski, Viktor; Audisio, Davide; Wolf, Larry M.; Schmidts, Volker; Hofmann, Kathrin; Wirtz, Cornelia; Thiel, Walter; Thiele, Christina M.; Maulide, Nuno; Chem. Sci. 6 (2015) 5734–; doi:10.1039/C5SC01867F

data_1520960
_publ_section_title
;
 Dynamic behaviour of monohaptoallylpalladium species: internal
 coordination as a driving force in allylic alkylation chemistry
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5734
_journal_paper_doi               10.1039/C5SC01867F
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C34 H30 Br N2 O5 P Pd'
_chemical_formula_weight         763.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-03-11 deposited with the CCDC.
2015-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.566(2)
_cell_length_b                   10.649(2)
_cell_length_c                   17.115(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.99
_cell_measurement_theta_min      2.14
_cell_volume                     1736.4(6)
_computing_cell_refinement       'Stoe X-Area (Stoe & Cie. GmbH, Darmstadt)'
_computing_data_collection       'Stoe X-Area (Stoe & Cie. GmbH, Darmstadt)'
_computing_data_reduction        'Stoe X-Area (Stoe & Cie. GmbH, Darmstadt)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Stoe IPDS II Single Crystal X-ray Diffractometer
;
_diffrn_measurement_method
; 
Imaging-plate diffractometer with two-circle goniometer
;
_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  0.1429
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15415
_diffrn_reflns_theta_full        21.86
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.0
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.2205
_exptl_crystal_size_mid          0.1648
_exptl_crystal_size_min          0.0342
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         4118
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                2755
_reflns_number_total             4118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01867f2.cif
_cod_data_source_block           vb4b
_cod_depositor_comments          'Adding full bibliography for 1520960.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1520960