Tuning the Stability of Pd(IV) Intermediates Using a Redox Non-innocent Ligand Combined with an Organolanthanide Fragment.
Goudy, Violaine; Jaoul, Arnaud; Cordier, Marie; Clavaguéra, Carine; Nocton, Grégory; Journal of the American Chemical Society 139 (2017) 10633–10636; doi:10.1021/jacs.7b05634

data_4131466
_publ_section_title
;
 Tuning the Stability of Pd(IV) Intermediates Using a Redox Non-innocent
 Ligand Combined with an Organolanthanide Fragment.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10633
_journal_page_last               10636
_journal_paper_doi               10.1021/jacs.7b05634
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C31 H45 I N4 Pd Yb, 3(C7 H8)'
_chemical_formula_sum            'C52 H69 I N4 Pd Yb'
_chemical_formula_weight         1156.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1623(9)
_cell_length_b                   12.2012(5)
_cell_length_c                   15.2011(5)
_cell_measurement_reflns_used    5090
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.0540
_cell_measurement_theta_min      2.2679
_cell_volume                     5037.8(3)
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_computing_structure_solution    SHELXT(Sheldrick,2014)
_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       32
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_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_point_group_measured_fraction_full 0.909
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_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         3.000
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
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_exptl_transmission_factor_min   0.5726
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+3.8393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3397
_reflns_number_total             4383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05634_si_002.cif
_cod_data_source_block           8
_cod_database_code               4131466
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.502
_shelx_estimated_absorpt_t_max   0.804
_shelx_res_checksum              77945
_shelx_hkl_checksum              28069
_shelx_fab_checksum              21041