#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:54:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003156.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_7003156
loop_
_publ_author_name
'Yen, Swee Kuan'
'Koh, Lip Lin'
'Huynh, Han Vinh'
'Hor, T. S. Andy'
_publ_section_title
;
 Pd(ii) complexes with mixed benzothiazolin-2-ylidene and phosphine
 ligands and their catalytic activities toward C--C coupling reactions
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              699
_journal_page_last               706
_journal_paper_doi               10.1039/b713152f
_journal_year                    2008
_chemical_formula_sum            'C28 H26 Br2 Cl3 N2 P Pd S'
_chemical_formula_weight         826.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.276(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4169(9)
_cell_length_b                   18.4151(14)
_cell_length_c                   16.1271(12)
_cell_measurement_reflns_used    4438
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.18
_cell_volume                     3219.6(4)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22528
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.443
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.3397
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                5646
_reflns_number_total             7378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713152f.txt
_cod_data_source_block           5425
_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)/n
_cod_database_code               7003156
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.23374(2) 0.205552(12) 0.785174(15) 0.02357(7) Uani 1 1 d . . .
Br1 Br 0.16481(3) 0.297612(17) 0.66763(2) 0.03778(10) Uani 1 1 d . . .
Br2 Br 0.41048(3) 0.17392(2) 0.73547(3) 0.04453(11) Uani 1 1 d . . .
P1 P 0.06634(8) 0.23020(4) 0.82741(6) 0.02903(19) Uani 1 1 d . . .
S1 S 0.37423(8) 0.16299(4) 0.98337(5) 0.03008(18) Uani 1 1 d . . .
N1 N 0.2799(2) 0.06266(13) 0.87701(16) 0.0260(6) Uani 1 1 d . . .
C1 C 0.2940(3) 0.13417(16) 0.8801(2) 0.0252(7) Uani 1 1 d . . .
C2 C 0.3257(3) 0.02747(16) 0.9583(2) 0.0263(7) Uani 1 1 d . . .
C3 C 0.3180(3) -0.04632(17) 0.9746(2) 0.0343(8) Uani 1 1 d . . .
H3 H 0.2800 -0.0791 0.9295 0.041 Uiso 1 1 calc R . .
C4 C 0.3684(3) -0.06921(17) 1.0596(2) 0.0384(8) Uani 1 1 d . . .
H4 H 0.3640 -0.1187 1.0725 0.046 Uiso 1 1 calc R . .
C5 C 0.4254(3) -0.02191(19) 1.1263(2) 0.0400(9) Uani 1 1 d . . .
H5 H 0.4594 -0.0399 1.1833 0.048 Uiso 1 1 calc R . .
C6 C 0.4333(3) 0.05155(18) 1.1107(2) 0.0342(8) Uani 1 1 d . . .
H6 H 0.4721 0.0839 1.1561 0.041 Uiso 1 1 calc R . .
C7 C 0.3817(3) 0.07565(16) 1.0252(2) 0.0280(7) Uani 1 1 d . . .
C8 C 0.2190(3) 0.02219(17) 0.7968(2) 0.0353(8) Uani 1 1 d . . .
H8A H 0.2663 -0.0220 0.7959 0.042 Uiso 1 1 calc R . .
H8B H 0.2193 0.0518 0.7464 0.042 Uiso 1 1 calc R . .
C9 C 0.0882(4) 0.0016(2) 0.7880(3) 0.0469(9) Uani 1 1 d . . .
H9A H 0.0378 0.0456 0.7814 0.056 Uiso 1 1 calc R . .
H9B H 0.0859 -0.0236 0.8410 0.056 Uiso 1 1 calc R . .
C10 C 0.0346(5) -0.0476(2) 0.7092(3) 0.0719(14) Uani 1 1 d . . .
H10A H 0.0399 -0.0234 0.6570 0.108 Uiso 1 1 calc R . .
H10B H -0.0510 -0.0580 0.7028 0.108 Uiso 1 1 calc R . .
H10C H 0.0810 -0.0926 0.7176 0.108 Uiso 1 1 calc R . .
C1A C 0.0633(3) 0.19778(17) 0.9343(2) 0.0336(8) Uani 1 1 d . . .
C2A C 0.0498(4) 0.2432(2) 0.9983(3) 0.0581(12) Uani 1 1 d . . .
H1A H 0.0426 0.2936 0.9891 0.070 Uiso 1 1 calc R . .
C3A C 0.0470(6) 0.2135(3) 1.0765(3) 0.0774(16) Uani 1 1 d . . .
H2A H 0.0348 0.2433 1.1204 0.093 Uiso 1 1 calc R . .
C4A C 0.0623(5) 0.1403(2) 1.0888(3) 0.0674(14) Uani 1 1 d . . .
H3A H 0.0633 0.1189 1.1419 0.081 Uiso 1 1 calc R . .
C5A C 0.0761(4) 0.0987(2) 1.0218(3) 0.0511(10) Uani 1 1 d . . .
H4A H 0.0854 0.0483 1.0303 0.061 Uiso 1 1 calc R . .
N2 N 0.0773(3) 0.12579(15) 0.9454(2) 0.0407(7) Uani 1 1 d . . .
C1B C 0.0427(4) 0.32761(17) 0.8340(2) 0.0368(8) Uani 1 1 d . . .
C2B C -0.0731(4) 0.3589(2) 0.8116(3) 0.0474(10) Uani 1 1 d . . .
H2B H -0.1441 0.3304 0.7886 0.057 Uiso 1 1 calc R . .
C3B C -0.0831(5) 0.4330(2) 0.8235(3) 0.0591(12) Uani 1 1 d . . .
H3B H -0.1615 0.4547 0.8090 0.071 Uiso 1 1 calc R . .
C4B C 0.0209(5) 0.4748(2) 0.8565(3) 0.0601(12) Uani 1 1 d . . .
H4B H 0.0131 0.5250 0.8641 0.072 Uiso 1 1 calc R . .
C5B C 0.1351(4) 0.4442(2) 0.8782(3) 0.0564(11) Uani 1 1 d . . .
H5B H 0.2058 0.4731 0.9009 0.068 Uiso 1 1 calc R . .
C6B C 0.1468(4) 0.37007(19) 0.8666(3) 0.0461(9) Uani 1 1 d . . .
H6B H 0.2255 0.3488 0.8810 0.055 Uiso 1 1 calc R . .
C1C C -0.0734(3) 0.18992(18) 0.7539(2) 0.0353(8) Uani 1 1 d . . .
C2C C -0.1718(4) 0.1709(2) 0.7816(3) 0.0574(11) Uani 1 1 d . . .
H2C H -0.1703 0.1818 0.8388 0.069 Uiso 1 1 calc R . .
C3C C -0.2735(4) 0.1356(3) 0.7250(4) 0.0721(15) Uani 1 1 d . . .
H3C H -0.3402 0.1228 0.7444 0.087 Uiso 1 1 calc R . .
C4C C -0.2770(4) 0.1196(3) 0.6424(3) 0.0702(14) Uani 1 1 d . . .
H4C H -0.3461 0.0956 0.6048 0.084 Uiso 1 1 calc R . .
C5C C -0.1815(4) 0.1380(3) 0.6135(3) 0.0694(14) Uani 1 1 d . . .
H5C H -0.1845 0.1271 0.5559 0.083 Uiso 1 1 calc R . .
C6C C -0.0788(4) 0.1731(2) 0.6694(3) 0.0507(10) Uani 1 1 d . . .
H6C H -0.0125 0.1855 0.6494 0.061 Uiso 1 1 calc R . .
C1S C 0.1804(4) 0.1604(2) 0.5073(3) 0.0560(11) Uani 1 1 d . . .
H1S H 0.2170 0.1919 0.5587 0.067 Uiso 1 1 calc R . .
Cl1A Cl 0.08724(14) 0.09473(8) 0.53435(9) 0.0813(4) Uani 1 1 d . . .
Cl1B Cl 0.29948(14) 0.11535(7) 0.48081(10) 0.0822(4) Uani 1 1 d . . .
Cl1C Cl 0.09568(16) 0.21383(6) 0.42066(9) 0.0890(5) Uani 1 1 d . . .
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'
Br Br -0.2901 2.4595 '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'
Cl Cl 0.1484 0.1585 '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
C1 Pd1 P1 91.27(9) . . ?
C1 Pd1 Br2 88.45(8) . . ?
P1 Pd1 Br2 177.35(3) . . ?
C1 Pd1 Br1 178.02(9) . . ?
P1 Pd1 Br1 89.85(2) . . ?
Br2 Pd1 Br1 90.507(14) . . ?
C1C P1 C1B 108.88(17) . . ?
C1C P1 C1A 102.04(16) . . ?
C1B P1 C1A 102.64(15) . . ?
C1C P1 Pd1 111.82(12) . . ?
C1B P1 Pd1 111.65(11) . . ?
C1A P1 Pd1 118.90(11) . . ?
C1 S1 C7 92.10(15) . . ?
C1 N1 C2 114.6(3) . . ?
C1 N1 C8 123.8(3) . . ?
C2 N1 C8 121.5(2) . . ?
N1 C1 S1 111.4(2) . . ?
N1 C1 Pd1 128.7(2) . . ?
S1 C1 Pd1 119.89(16) . . ?
C7 C2 C3 121.2(3) . . ?
C7 C2 N1 112.0(3) . . ?
C3 C2 N1 126.7(3) . . ?
C4 C3 C2 117.1(3) . . ?
C3 C4 C5 122.1(3) . . ?
C4 C5 C6 121.2(3) . . ?
C5 C6 C7 117.4(3) . . ?
C2 C7 C6 121.0(3) . . ?
C2 C7 S1 109.6(2) . . ?
C6 C7 S1 129.4(3) . . ?
N1 C8 C9 113.2(3) . . ?
C8 C9 C10 110.8(3) . . ?
N2 C1A C2A 122.6(3) . . ?
N2 C1A P1 114.2(2) . . ?
C2A C1A P1 123.2(3) . . ?
C1A C2A C3A 119.0(4) . . ?
C4A C3A C2A 118.9(4) . . ?
C3A C4A C5A 118.5(4) . . ?
N2 C5A C4A 123.8(4) . . ?
C5A N2 C1A 117.3(3) . . ?
C6B C1B C2B 120.1(3) . . ?
C6B C1B P1 117.0(3) . . ?
C2B C1B P1 122.9(3) . . ?
C1B C2B C3B 119.2(4) . . ?
C4B C3B C2B 120.4(4) . . ?
C5B C4B C3B 120.6(4) . . ?
C4B C5B C6B 119.8(4) . . ?
C1B C6B C5B 120.0(4) . . ?
C2C C1C C6C 118.3(4) . . ?
C2C C1C P1 122.0(3) . . ?
C6C C1C P1 119.6(3) . . ?
C1C C2C C3C 120.2(4) . . ?
C4C C3C C2C 120.6(4) . . ?
C3C C4C C5C 120.3(4) . . ?
C4C C5C C6C 119.8(5) . . ?
C1C C6C C5C 120.8(4) . . ?
Cl1C C1S Cl1A 111.3(3) . . ?
Cl1C C1S Cl1B 110.5(2) . . ?
Cl1A C1S Cl1B 108.1(2) . . ?
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 C1 1.971(3) . ?
Pd1 P1 2.2670(8) . ?
Pd1 Br2 2.4633(4) . ?
Pd1 Br1 2.4802(4) . ?
P1 C1C 1.821(4) . ?
P1 C1B 1.822(3) . ?
P1 C1A 1.835(3) . ?
S1 C1 1.714(3) . ?
S1 C7 1.736(3) . ?
N1 C1 1.326(4) . ?
N1 C2 1.408(4) . ?
N1 C8 1.465(4) . ?
C2 C7 1.388(4) . ?
C2 C3 1.392(4) . ?
C3 C4 1.375(5) . ?
C4 C5 1.378(5) . ?
C5 C6 1.384(5) . ?
C6 C7 1.391(4) . ?
C8 C9 1.503(5) . ?
C9 C10 1.523(5) . ?
C1A N2 1.341(4) . ?
C1A C2A 1.373(5) . ?
C2A C3A 1.384(6) . ?
C3A C4A 1.366(6) . ?
C4A C5A 1.373(6) . ?
C5A N2 1.333(4) . ?
C1B C6B 1.382(5) . ?
C1B C2B 1.382(5) . ?
C2B C3B 1.388(5) . ?
C3B C4B 1.375(6) . ?
C4B C5B 1.362(6) . ?
C5B C6B 1.390(5) . ?
C1C C2C 1.378(5) . ?
C1C C6C 1.379(5) . ?
C2C C3C 1.392(6) . ?
C3C C4C 1.352(7) . ?
C4C C5C 1.358(6) . ?
C5C C6C 1.394(6) . ?
C1S Cl1C 1.734(5) . ?
C1S Cl1A 1.754(4) . ?
C1S Cl1B 1.756(4) . ?
