Synthesis, characterization, dynamics and reactivity toward amination of η3-allyl palladium complexes bearing mixed ancillary ligands. Evaluation of the electronic characteristics of the ligands from kinetic data.
Canovese, Luciano; Visentin, Fabiano; Levi, Carlo; Dolmella, Alessandro; Dalton transactions (Cambridge, England : 2003) 40 (2011) 966–981; doi:10.1039/c0dt00811g

data_7014426
_publ_section_title
;
 Synthesis, characterization, dynamics and reactivity toward amination
 of \h3-allyl palladium complexes bearing mixed ancillary ligands.
 Evaluation of the electronic characteristics of the ligands from
 kinetic data.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              966
_journal_page_last               981
_journal_paper_doi               10.1039/c0dt00811g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C33 H39 Cl N3 O4 Pd'
_chemical_formula_weight         682.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'heavy-atom methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.063(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8436(1)
_cell_length_b                   13.2013(1)
_cell_length_c                   19.8990(2)
_cell_measurement_reflns_used    30639
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      3.27
_cell_volume                     3225.41(5)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
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_computing_structure_solution    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 16.1274
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_diffrn_measurement_details
;
1 omega -97.00 -55.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- -21.3113 157.0000 -27.0000 42

2 omega 44.00 90.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 179.0000 30.0000 46

3 omega -52.00 47.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 -38.0000 120.0000 99

4 omega -47.00 15.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 -77.0000 60.0000 62

5 omega -5.00 80.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 66.0000 117.0000 85

6 omega 2.00 82.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 77.0000 0.0000 80

7 omega -43.00 51.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 -77.0000 -30.0000 94

8 omega 2.00 93.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 77.0000 -90.0000 91

9 omega -47.00 42.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 -38.0000 -150.0000 89

10 omega -6.00 88.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 77.0000 -180.0000 94

11 omega 42.00 85.00 1.0000 11.4300
omega____ theta____ kappa____ phi______ frames
- 21.3895 -132.0000 -119.0000 43

;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
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_diffrn_orient_matrix_UB_12      -0.0374271123
_diffrn_orient_matrix_UB_13      -0.0178257397
_diffrn_orient_matrix_UB_21      0.0318099455
_diffrn_orient_matrix_UB_22      -0.0379273995
_diffrn_orient_matrix_UB_23      0.0219019870
_diffrn_orient_matrix_UB_31      -0.0301793108
_diffrn_orient_matrix_UB_32      0.0066913581
_diffrn_orient_matrix_UB_33      0.0243618730
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48218
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 50
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_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     'riding model'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0457P)^2^+0.7242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                6669
_reflns_number_total             7959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00811G.TXT
_cod_data_source_block           exp_50
_cod_original_cell_volume        3225.4(1)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 (No.14)'
_cod_original_formula_sum        'C33 H39 N3 O4 Cl1 Pd1'
_cod_database_code               7014426