#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/32/1513203.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1513203
loop_
_publ_author_name
'Yong-Joo Kim'
'Hyun-Kyung Kim'
'Jung-Hyun Lee'
'Zhen Nu Zheng'
'Soon W. Lee'
_publ_section_title
;
 Synthesis and structures of n1-allenyl and/or -propargyl Pd(II) complexes
 and their reactivity toward trimethylsilyl pseudohalides, organic thiols,
 and N-heterocyclic carbene ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              54
_journal_page_last               63
_journal_paper_doi               10.1016/j.ica.2012.12.011
_journal_volume                  398
_journal_year                    2013
_chemical_formula_moiety         'C12 H23 Cl P2 Pd S'
_chemical_formula_sum            'C12 H23 Cl P2 Pd S'
_chemical_formula_weight         403.16
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.039(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0682(6)
_cell_length_b                   11.0519(4)
_cell_length_c                   11.8852(5)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.38
_cell_volume                     1766.80(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29877
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.8660
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0324P)²+0.8606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                3614
_reflns_number_total             4381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-398-54-63-4.cif
_cod_data_source_block           ljh2-58
_cod_original_sg_symbol_H-M      'P 21/c  '
_cod_database_code               1513203
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.737224(13) 0.231239(16) 0.186043(16) 0.04122(7) Uani 1 1 d .
Cl1 Cl 0.82139(6) 0.41338(6) 0.24936(7) 0.06743(19) Uani 1 1 d .
P1 P 0.88380(5) 0.15661(6) 0.16136(6) 0.04753(15) Uani 1 1 d .
P2 P 0.59186(5) 0.31038(8) 0.20831(8) 0.0634(2) Uani 1 1 d .
S1 S 0.65508(5) 0.05087(7) 0.13162(6) 0.06186(19) Uani 1 1 d .
C1 C 0.71268(17) -0.0497(2) 0.2465(2) 0.0494(6) Uani 1 1 d .
C2 C 0.7474(2) -0.0140(3) 0.3631(3) 0.0605(7) Uani 1 1 d .
H2 H 0.7428 0.0671 0.3817 0.073 Uiso 1 1 calc R
C3 C 0.7886(2) -0.0947(3) 0.4522(3) 0.0766(9) Uani 1 1 d .
H3 H 0.8110 -0.0675 0.5295 0.092 Uiso 1 1 calc R
C4 C 0.7968(3) -0.2130(3) 0.4285(4) 0.0872(12) Uani 1 1 d .
H4 H 0.8243 -0.2672 0.4892 0.105 Uiso 1 1 calc R
C5 C 0.7642(2) -0.2530(3) 0.3135(4) 0.0826(13) Uani 1 1 d .
H5 H 0.7706 -0.3342 0.2966 0.099 Uiso 1 1 calc R
C6 C 0.7214(2) -0.1718(3) 0.2218(3) 0.0667(8) Uani 1 1 d .
H6 H 0.6988 -0.1995 0.1447 0.080 Uiso 1 1 calc R
C7 C 0.9275(3) 0.2527(3) 0.0632(4) 0.0874(11) Uani 1 1 d .
H7A H 0.8765 0.2600 -0.0106 0.131 Uiso 1 1 calc R
H7B H 0.9859 0.2177 0.0503 0.131 Uiso 1 1 calc R
H7C H 0.9433 0.3314 0.0979 0.131 Uiso 1 1 calc R
C8 C 0.8872(3) 0.0083(3) 0.0975(3) 0.0847(10) Uani 1 1 d .
H8A H 0.8355 0.0026 0.0241 0.127 Uiso 1 1 calc R
H8B H 0.8773 -0.0527 0.1505 0.127 Uiso 1 1 calc R
H8C H 0.9506 -0.0036 0.0840 0.127 Uiso 1 1 calc R
C9 C 0.9853(2) 0.1533(4) 0.2946(3) 0.0947(13) Uani 1 1 d .
H9A H 0.9686 0.1014 0.3508 0.142 Uiso 1 1 calc R
H9B H 0.9977 0.2336 0.3263 0.142 Uiso 1 1 calc R
H9C H 1.0437 0.1231 0.2780 0.142 Uiso 1 1 calc R
C10 C 0.4778(3) 0.2690(5) 0.1032(4) 0.1114(17) Uani 1 1 d .
H10A H 0.4807 0.2885 0.0256 0.167 Uiso 1 1 calc R
H10B H 0.4241 0.3126 0.1190 0.167 Uiso 1 1 calc R
H10C H 0.4671 0.1837 0.1084 0.167 Uiso 1 1 calc R
C11 C 0.5711(3) 0.2645(6) 0.3445(4) 0.133(2) Uani 1 1 d .
H11A H 0.6286 0.2837 0.4088 0.199 Uiso 1 1 calc R
H11B H 0.5593 0.1789 0.3430 0.199 Uiso 1 1 calc R
H11C H 0.5143 0.3065 0.3543 0.199 Uiso 1 1 calc R
C12 C 0.5859(4) 0.4713(5) 0.2152(10) 0.284(6) Uani 1 1 d .
H12A H 0.6458 0.5014 0.2698 0.426 Uiso 1 1 calc R
H12B H 0.5298 0.4943 0.2409 0.426 Uiso 1 1 calc R
H12C H 0.5788 0.5047 0.1387 0.426 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S1 Pd1 P2 88.38(3)
S1 Pd1 P1 92.77(3)
P2 Pd1 P1 178.47(3)
S1 Pd1 Cl1 177.72(3)
P2 Pd1 Cl1 91.09(3)
P1 Pd1 Cl1 87.81(3)
C9 P1 C8 103.83(19)
C9 P1 C7 104.4(2)
C8 P1 C7 101.82(18)
C9 P1 Pd1 113.73(11)
C8 P1 Pd1 120.56(12)
C7 P1 Pd1 110.78(13)
C10 P2 C12 104.1(3)
C10 P2 C11 102.0(2)
C12 P2 C11 102.5(4)
C10 P2 Pd1 117.94(14)
C12 P2 Pd1 116.00(18)
C11 P2 Pd1 112.26(16)
C1 S1 Pd1 104.46(8)
C2 C1 C6 117.4(3)
C2 C1 S1 122.8(2)
C6 C1 S1 119.8(2)
C3 C2 C1 122.0(3)
C3 C2 H2 119.0
C1 C2 H2 119.0
C4 C3 C2 120.7(4)
C4 C3 H3 119.6
C2 C3 H3 119.6
C3 C4 C5 119.5(3)
C3 C4 H4 120.3
C5 C4 H4 120.3
C4 C5 C6 120.4(3)
C4 C5 H5 119.8
C6 C5 H5 119.8
C1 C6 C5 120.0(3)
C1 C6 H6 120.0
C5 C6 H6 120.0
P1 C7 H7A 109.5
P1 C7 H7B 109.5
H7A C7 H7B 109.5
P1 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
P1 C8 H8A 109.5
P1 C8 H8B 109.5
H8A C8 H8B 109.5
P1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
P1 C9 H9A 109.5
P1 C9 H9B 109.5
H9A C9 H9B 109.5
P1 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
P2 C10 H10A 109.5
P2 C10 H10B 109.5
H10A C10 H10B 109.5
P2 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
P2 C11 H11A 109.5
P2 C11 H11B 109.5
H11A C11 H11B 109.5
P2 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
P2 C12 H12A 109.5
P2 C12 H12B 109.5
H12A C12 H12B 109.5
P2 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 S1 2.2999(7)
Pd1 P2 2.3096(7)
Pd1 P1 2.3180(6)
Pd1 Cl1 2.3449(7)
P1 C9 1.795(3)
P1 C8 1.813(3)
P1 C7 1.813(3)
P2 C10 1.780(4)
P2 C12 1.783(5)
P2 C11 1.800(5)
S1 C1 1.763(3)
C1 C2 1.385(4)
C1 C6 1.394(4)
C2 C3 1.376(4)
C2 H2 0.9300
C3 C4 1.349(5)
C3 H3 0.9300
C4 C5 1.381(5)
C4 H4 0.9300
C5 C6 1.403(5)
C5 H5 0.9300
C6 H6 0.9300
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C9 H9A 0.9600
C9 H9B 0.9600
C9 H9C 0.9600
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
C11 H11A 0.9600
C11 H11B 0.9600
C11 H11C 0.9600
C12 H12A 0.9600
C12 H12B 0.9600
C12 H12C 0.9600
