C‒H Bond Activation by a Palladium(II) Thioether Complex: Formation of the Bis(nitromethanate) Complex [Pd(9S3)(CH2NO2)2]
Lee, John P.; Keller, C. Luke; Werlein, Ashley A.; Janzen, Daron E.; VanDerveer, Donald G.; Grant, Gregory J.; Organometallics 31 (2012) 6505–; doi:10.1021/om3006382

data_4079274
_publ_section_title
;
 C--H Bond Activation by a Palladium(II) Thioether Complex: Formation of
 the Bis(nitromethanate) Complex [Pd(9S3)(CH2NO2)2]
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              6505
_journal_paper_doi               10.1021/om3006382
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C8 H16 N2 O4 Pd S3'
_chemical_formula_sum            'C8 H16 N2 O4 Pd S3'
_chemical_formula_weight         406.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8595(16)
_cell_length_b                   9.904(2)
_cell_length_c                   18.205(4)
_cell_measurement_reflns_used    8849
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.0212
_cell_measurement_theta_min      2.6045
_cell_volume                     1409.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0273
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11480
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0222P)^2^+4.5443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2266
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3006382_si_002.cif
_cod_data_source_block           pd9s3ch2no22
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079274