Reversible Redox Chemistry and Catalytic C(sp(3))-H Amination Reactivity of a Paramagnetic Pd Complex Bearing a Redox-Active o-Aminophenol-Derived NNO Pincer Ligand.
Broere, Daniël L J; van Leest, Nicolaas P.; de Bruin, Bas; Siegler, Maxime A.; van der Vlugt, Jarl Ivar; Inorganic chemistry 55 (2016) 8603–8611; doi:10.1021/acs.inorgchem.6b01192

data_4348475
_publ_section_title
;
 Reversible Redox Chemistry and Catalytic C(sp(3))-H Amination Reactivity
 of a Paramagnetic Pd Complex Bearing a Redox-Active o-Aminophenol-Derived
 NNO Pincer Ligand.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8603
_journal_page_last               8611
_journal_paper_doi               10.1021/acs.inorgchem.6b01192
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C22 H30 B Cl F4 N2 O Pd'
_chemical_formula_weight         567.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.531(3)
_cell_angle_beta                 89.979(4)
_cell_angle_gamma                107.760(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3768(4)
_cell_length_b                   12.0798(7)
_cell_length_c                   15.1667(9)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.9845
_cell_measurement_theta_min      6.7018
_cell_volume                     1284.41(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31066
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.200
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         2.900
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.137
_exptl_transmission_factor_max   0.7465
_exptl_transmission_factor_min   0.6374
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4607
_refine_ls_number_restraints     866
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.9031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3779
_reflns_number_total             4607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01192_si_002.cif
_cod_data_source_block           refin
_cod_database_code               4348475
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              44796
_shelx_hkl_checksum              7559
_shelx_fab_checksum              91532