Room-Temperature Carbon‒Sulfur Bond Activation by a Reactive (dippe)Pd Fragment
Munjanja, Lloyd; Brennessel, William W.; Jones, William D.; Organometallics 34 (2015) 1716–; doi:10.1021/acs.organomet.5b00194

data_4087505
_publ_section_title
;
 Room-Temperature Carbon--Sulfur Bond Activation by a Reactive (dippe)Pd
 Fragment
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1716
_journal_paper_doi               10.1021/acs.organomet.5b00194
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H40 P2 Pd S2, 0.25(C6 H6)'
_chemical_formula_sum            'C27.5 H41.5 P2 Pd S2'
_chemical_formula_weight         604.56
_chemical_name_common            jonlm05
_chemical_name_systematic
; 
 (dippe)Pd(thianthrene)
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                103.038(2)
_cell_angle_beta                 103.999(2)
_cell_angle_gamma                101.001(2)
_cell_formula_units_Z            4
_cell_length_a                   10.8988(9)
_cell_length_b                   15.1108(13)
_cell_length_c                   19.0889(16)
_cell_measurement_reflns_used    3959
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      33.66
_cell_measurement_theta_min      2.33
_cell_volume                     2869.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            71889
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        36.320
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         27346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0350P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17474
_reflns_number_total             27346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00194_si_002.cif
_cod_data_source_block           9
_cod_database_code               4087505
_shelx_estimated_absorpt_t_min   0.770
_shelx_estimated_absorpt_t_max   0.810