#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:10:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179716 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/18/7001830.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_7001830
loop_
_publ_author_name
'Lee, Kyung-Eun'
'Jeon, Hyeong-Tak'
'Han, Sam-Yong'
'Ham, Jungyeob'
'Kim, Yong-Joo'
'Lee, Soon W.'
_publ_section_title
;
 Cyclopalladated azido complexes containing C,N-donor (HC∼ N =
 2-(2′-thienyl)pyridine, azobenzene, 3,3′-dimethyl
 azobenzene, N,N′-dimethylbenzylamine, 2-phenylpyridine)
 ligands: reactivity towards organic unsaturated compounds and
 catalytic properties
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              6578
_journal_page_last               6592
_journal_paper_doi               10.1039/b907324h
_journal_year                    2009
_chemical_formula_sum            'C12 H15 N4 P Pd S'
_chemical_formula_weight         384.71
_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                 112.4870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4930(3)
_cell_length_b                   11.9648(3)
_cell_length_c                   12.7272(3)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.43
_cell_volume                     1476.37(7)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23540
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4669
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0132(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0186
_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/[σ²(Fo²)+(0.0223P)²+0.6778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                3360
_reflns_number_total             3606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907324h.txt
_cod_data_source_block           cxh257
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7001830
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.716380(12) 0.340596(10) 0.095183(10) 0.03381(6) Uani 1 1 d . . .
S1 S 0.26570(5) 0.27851(5) -0.05585(5) 0.05448(13) Uani 1 1 d . . .
P1 P 0.83396(5) 0.21334(4) 0.04004(4) 0.03898(10) Uani 1 1 d . . .
N1 N 0.59295(15) 0.44422(11) 0.15279(12) 0.0384(3) Uani 1 1 d . . .
N2 N 0.89117(18) 0.43000(16) 0.19789(15) 0.0569(4) Uani 1 1 d . . .
N3 N 0.97398(16) 0.47337(14) 0.17031(14) 0.0499(4) Uani 1 1 d . . .
N4 N 1.0586(2) 0.5175(2) 0.1502(2) 0.0881(7) Uani 1 1 d . . .
C1 C 0.6368(2) 0.52501(15) 0.23117(16) 0.0480(4) Uani 1 1 d . . .
H1 H 0.7298 0.5440 0.2607 0.058 Uiso 1 1 calc R . .
C2 C 0.5478(3) 0.58103(17) 0.26957(18) 0.0574(5) Uani 1 1 d . . .
H2 H 0.5805 0.6360 0.3252 0.069 Uiso 1 1 calc R . .
C3 C 0.4099(3) 0.55412(18) 0.2242(2) 0.0589(5) Uani 1 1 d . . .
H3 H 0.3486 0.5904 0.2495 0.071 Uiso 1 1 calc R . .
C4 C 0.3628(2) 0.47343(17) 0.14112(18) 0.0524(5) Uani 1 1 d . . .
H4 H 0.2693 0.4565 0.1078 0.063 Uiso 1 1 calc R . .
C5 C 0.45772(18) 0.41752(14) 0.10778(15) 0.0396(3) Uani 1 1 d . . .
C6 C 0.42874(17) 0.32785(14) 0.02612(15) 0.0394(4) Uani 1 1 d . . .
C7 C 0.53163(17) 0.27478(13) 0.00363(14) 0.0372(3) Uani 1 1 d . . .
C8 C 0.4735(2) 0.19314(16) -0.08337(17) 0.0474(4) Uani 1 1 d . . .
H8 H 0.5265 0.1488 -0.1111 0.057 Uiso 1 1 calc R . .
C9 C 0.3344(2) 0.18600(18) -0.12198(19) 0.0553(5) Uani 1 1 d . . .
H9 H 0.2822 0.1363 -0.1782 0.066 Uiso 1 1 calc R . .
C10 C 1.0183(2) 0.2177(2) 0.1204(3) 0.0765(7) Uani 1 1 d . . .
H10A H 1.0366 0.2130 0.2002 0.115 Uiso 1 1 calc R . .
H10B H 1.0549 0.2866 0.1050 0.115 Uiso 1 1 calc R . .
H10C H 1.0613 0.1559 0.0987 0.115 Uiso 1 1 calc R . .
C11 C 0.8202(3) 0.2228(2) -0.10499(18) 0.0609(5) Uani 1 1 d . . .
H11A H 0.8403 0.2978 -0.1206 0.091 Uiso 1 1 calc R . .
H11B H 0.7282 0.2034 -0.1552 0.091 Uiso 1 1 calc R . .
H11C H 0.8846 0.1723 -0.1166 0.091 Uiso 1 1 calc R . .
C12 C 0.7938(3) 0.06901(18) 0.0577(2) 0.0627(5) Uani 1 1 d . . .
H12A H 0.7995 0.0576 0.1340 0.094 Uiso 1 1 calc R . .
H12B H 0.8584 0.0208 0.0432 0.094 Uiso 1 1 calc R . .
H12C H 0.7021 0.0521 0.0051 0.094 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pd1 N2 170.55(7) . . ?
C7 Pd1 N1 81.22(6) . . ?
N2 Pd1 N1 89.45(6) . . ?
C7 Pd1 P1 94.43(5) . . ?
N2 Pd1 P1 95.00(5) . . ?
N1 Pd1 P1 172.92(4) . . ?
C9 S1 C6 90.67(9) . . ?
C11 P1 C10 103.13(13) . . ?
C11 P1 C12 104.83(11) . . ?
C10 P1 C12 101.93(13) . . ?
C11 P1 Pd1 116.22(8) . . ?
C10 P1 Pd1 113.69(9) . . ?
C12 P1 Pd1 115.32(8) . . ?
C1 N1 C5 119.54(16) . . ?
C1 N1 Pd1 126.89(13) . . ?
C5 N1 Pd1 113.43(11) . . ?
N3 N2 Pd1 127.62(14) . . ?
N4 N3 N2 175.8(2) . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.88(19) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.8(2) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 120.98(18) . . ?
N1 C5 C6 112.30(14) . . ?
C4 C5 C6 126.72(18) . . ?
C7 C6 C5 121.86(15) . . ?
C7 C6 S1 113.02(13) . . ?
C5 C6 S1 125.09(14) . . ?
C6 C7 C8 109.96(15) . . ?
C6 C7 Pd1 111.11(12) . . ?
C8 C7 Pd1 138.80(14) . . ?
C9 C8 C7 114.01(19) . . ?
C9 C8 H8 123.0 . . ?
C7 C8 H8 123.0 . . ?
C8 C9 S1 112.34(16) . . ?
C8 C9 H9 123.8 . . ?
S1 C9 H9 123.8 . . ?
P1 C10 H10A 109.5 . . ?
P1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 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
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C7 2.0020(16) . ?
Pd1 N2 2.0935(16) . ?
Pd1 N1 2.1163(14) . ?
Pd1 P1 2.2350(4) . ?
S1 C9 1.708(3) . ?
S1 C6 1.7316(17) . ?
P1 C11 1.799(2) . ?
P1 C10 1.811(2) . ?
P1 C12 1.812(2) . ?
N1 C1 1.338(2) . ?
N1 C5 1.350(2) . ?
N2 N3 1.175(2) . ?
N3 N4 1.143(2) . ?
C1 C2 1.382(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.443(3) . ?
C6 C7 1.374(2) . ?
C7 C8 1.427(2) . ?
C8 C9 1.353(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
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 . ?
