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_4087508
_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         'C26.88 H40.88 O0.88 P2 Pd S1.12'
_chemical_formula_sum            'C26.88 H40.88 O0.88 P2 Pd S1.12'
_chemical_formula_weight         582.35
_chemical_name_common            jonlm10
_chemical_name_systematic
; 
 (dippe)Pd(SPh)2 / (dippe)Pd(SPh)(C(=O)Ph) 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.625(2)
_cell_length_b                   16.806(2)
_cell_length_c                   20.814(3)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.34
_cell_measurement_theta_min      2.42
_cell_volume                     5465.6(12)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            112219
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.621
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             2425
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         15125
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0379P)^2^+2.5047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10315
_reflns_number_total             15125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00194_si_002.cif
_cod_data_source_block           14-15
_cod_original_cell_volume        5465.8(12)
_cod_database_code               4087508
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.916