Redox noninnocence of Nitrosoarene Ligands in Transition Metal Complexes
Neil C. Tomson; Liezel A. Labios; Thomas Weyhermüller; Joshua S. Figueroa; Karl Wieghardt; Inorganic Chemistry 50 (2011) 5763–5776; doi:10.1021/ic2005979

data_4325439
_publ_contact_author_address
;Max-Planck-Institut fuer Bioanorganische Chemie
Stiftstrasse 34-36
45470 Muelheim an der Ruhr
Germany
;
_publ_contact_author_email       wieghardt@mpi-muelheim.mpg.de
_publ_contact_author_fax         +49-(0)208-306-3952
_publ_contact_author_name        'Prof. Karl Wieghardt'
_publ_contact_author_phone       +49-(0)208-306-3609
_publ_section_title
;
 Redox noninnocence of Nitrosoarene Ligands in Transition Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5763
_journal_page_last               5776
_journal_paper_doi               10.1021/ic2005979
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C72 H85.5 O1.75 Pd n3'
_chemical_formula_weight         1108.80
_chemical_name_common            (eta-2-o-tolNO)Pd(CNArDipp2)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.733(2)
_cell_angle_beta                 87.768(2)
_cell_angle_gamma                85.113(2)
_cell_formula_units_Z            4
_cell_length_a                   12.734(2)
_cell_length_b                   21.459(3)
_cell_length_c                   23.750(4)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.32
_cell_volume                     6424.8(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            74974
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_correction_T_min  0.9908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       Block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.022
_platon_squeeze_details
; 
Three voids were found, one of which contained a 
disordered diethyl ether molecule. Its formula was 
added to the formula for the unit cell and its 
electron density removed. 
;
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1412
_refine_ls_number_reflns         23628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+4.6157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                17771
_reflns_number_total             23628
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic2005979_si_002_2.cif
_cod_data_source_block           5
_cod_original_cell_volume        6424.7(17)
_cod_original_formula_sum        'C72 H85.5 n3 O1.75 Pd'
_cod_database_code               4325439