Synthesis and characterization of a cyclic vinylpalladium(ii) complex: vinylpalladium species as the possible intermediate in the catalytic direct olefination reaction of enamide
Xu, Yun-He; Chok, Yew Keong; Loh, Teck-Peng; Chemical Science 2 (2011) 1822–; doi:10.1039/c1sc00262g

data_1515619
_publ_section_title
;
 Synthesis and characterization of a cyclic vinylpalladium(ii) complex:
 vinylpalladium species as the possible intermediate in the catalytic
 direct olefination reaction of enamide
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              1822
_journal_paper_doi               10.1039/c1sc00262g
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C16 H18 Cl N O2 Pd S'
_chemical_formula_sum            'C16 H18 Cl N O2 Pd S'
_chemical_formula_weight         430.22
_chemical_name_common            LTP196
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 117.218(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4450(7)
_cell_length_b                   9.4054(5)
_cell_length_c                   14.8518(7)
_cell_measurement_reflns_used    8128
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.06
_cell_measurement_theta_min      2.66
_cell_volume                     1670.14(16)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22627
_diffrn_reflns_theta_full        31.08
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.8726
_exptl_absorpt_correction_T_min  0.8069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+1.2069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                4588
_reflns_number_total             5333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00262g.txt
_cod_data_source_block           ltp196s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1670.14(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1515619