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_4087509
_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         'C14 H32 Cl2 P2 Pd'
_chemical_formula_sum            'C14 H32 Cl2 P2 Pd'
_chemical_formula_weight         439.63
_chemical_name_common            jonlm11
_chemical_name_systematic
; 
 (dippe)PdCl2
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_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                   14.308(5)
_cell_length_b                   14.308(5)
_cell_length_c                   18.642(7)
_cell_measurement_reflns_used    3906
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.41
_cell_measurement_theta_min      2.97
_cell_volume                     3816(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.982
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37616
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.706
_diffrn_reflns_theta_min         2.013
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
; 
 Flack x determined using 2281 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+0.7619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0389
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                5088
_reflns_number_total             5317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00194_si_002.cif
_cod_data_source_block           dippePdCl2
_cod_original_cell_volume        3816(3)
_cod_database_code               4087509
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.766