#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:54:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003154.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_7003154
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 H44 Br2 N P Pd S'
_chemical_formula_weight         723.89
_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                 109.398(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.244(3)
_cell_length_b                   14.302(3)
_cell_length_c                   16.013(3)
_cell_measurement_reflns_used    2206
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20.69
_cell_measurement_theta_min      2.19
_cell_volume                     3077.0(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21001
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.7761
_exptl_absorpt_correction_T_min  0.4148
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.710
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0627
_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)+(0.0799P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                4070
_reflns_number_total             7058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713152f.txt
_cod_data_source_block           5445a
_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_cell_volume        3077.1(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003154
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 0.72749(4) 0.06330(3) 0.07794(3) 0.04398(17) Uani 1 1 d . . .
Br1 Br 0.86438(8) -0.03664(6) 0.06791(6) 0.0822(3) Uani 1 1 d . . .
Br2 Br 0.69748(6) -0.04609(5) 0.18691(5) 0.0633(2) Uani 1 1 d . . .
P1 P 0.74638(13) 0.16301(11) -0.02720(10) 0.0437(4) Uani 1 1 d . . .
S1 S 0.49602(12) 0.12006(11) 0.03466(10) 0.0463(4) Uani 1 1 d . . .
N1 N 0.6272(3) 0.1980(3) 0.1619(3) 0.0361(11) Uani 1 1 d . . .
C1 C 0.6186(5) 0.1362(4) 0.0964(3) 0.0397(14) Uani 1 1 d . . .
C2 C 0.5367(4) 0.2350(4) 0.1640(4) 0.0381(13) Uani 1 1 d . . .
C3 C 0.5260(5) 0.3049(4) 0.2224(4) 0.0443(15) Uani 1 1 d . . .
H3 H 0.5815 0.3328 0.2644 0.053 Uiso 1 1 calc R . .
C4 C 0.4309(5) 0.3300(5) 0.2149(4) 0.0503(16) Uani 1 1 d . . .
H4 H 0.4208 0.3764 0.2526 0.060 Uiso 1 1 calc R . .
C5 C 0.3485(5) 0.2886(5) 0.1528(5) 0.0599(19) Uani 1 1 d . . .
H5 H 0.2843 0.3063 0.1512 0.072 Uiso 1 1 calc R . .
C6 C 0.3584(5) 0.2223(5) 0.0932(4) 0.0536(17) Uani 1 1 d . . .
H6 H 0.3027 0.1954 0.0505 0.064 Uiso 1 1 calc R . .
C7 C 0.4557(5) 0.1973(4) 0.1002(4) 0.0428(14) Uani 1 1 d . . .
C8 C 0.7214(5) 0.2176(4) 0.2321(4) 0.0458(15) Uani 1 1 d . . .
H8A H 0.7304 0.2854 0.2390 0.055 Uiso 1 1 calc R . .
H8B H 0.7764 0.1925 0.2149 0.055 Uiso 1 1 calc R . .
C9 C 0.7255(5) 0.1748(5) 0.3209(4) 0.0592(18) Uani 1 1 d . . .
H9A H 0.6787 0.2079 0.3436 0.071 Uiso 1 1 calc R . .
H9B H 0.7050 0.1092 0.3120 0.071 Uiso 1 1 calc R . .
C10 C 0.8252(7) 0.1805(7) 0.3860(6) 0.101(3) Uani 1 1 d . . .
H10A H 0.8659 0.1303 0.3758 0.152 Uiso 1 1 calc R . .
H10B H 0.8212 0.1748 0.4451 0.152 Uiso 1 1 calc R . .
H10C H 0.8548 0.2402 0.3804 0.152 Uiso 1 1 calc R . .
C11 C 0.6762(5) 0.2744(4) -0.0379(4) 0.0445(15) Uani 1 1 d . . .
H11 H 0.6111 0.2569 -0.0326 0.053 Uiso 1 1 calc R . .
C12 C 0.7228(5) 0.3418(4) 0.0380(4) 0.0518(16) Uani 1 1 d . . .
H12A H 0.7849 0.3664 0.0329 0.062 Uiso 1 1 calc R . .
H12B H 0.7392 0.3080 0.0942 0.062 Uiso 1 1 calc R . .
C13 C 0.6533(6) 0.4235(5) 0.0383(5) 0.070(2) Uani 1 1 d . . .
H13A H 0.5925 0.3997 0.0467 0.084 Uiso 1 1 calc R . .
H13B H 0.6861 0.4659 0.0874 0.084 Uiso 1 1 calc R . .
C14 C 0.6269(6) 0.4760(5) -0.0490(5) 0.073(2) Uani 1 1 d . . .
H14A H 0.5790 0.5256 -0.0502 0.088 Uiso 1 1 calc R . .
H14B H 0.6869 0.5054 -0.0542 0.088 Uiso 1 1 calc R . .
C15 C 0.5829(6) 0.4108(5) -0.1263(5) 0.070(2) Uani 1 1 d . . .
H15A H 0.5703 0.4457 -0.1816 0.085 Uiso 1 1 calc R . .
H15B H 0.5189 0.3873 -0.1246 0.085 Uiso 1 1 calc R . .
C16 C 0.6513(5) 0.3278(5) -0.1254(4) 0.0548(17) Uani 1 1 d . . .
H16A H 0.6183 0.2858 -0.1748 0.066 Uiso 1 1 calc R . .
H16B H 0.7128 0.3505 -0.1331 0.066 Uiso 1 1 calc R . .
C17 C 0.6957(5) 0.1112(4) -0.1392(4) 0.0477(16) Uani 1 1 d . . .
H17 H 0.6991 0.1608 -0.1812 0.057 Uiso 1 1 calc R . .
C18 C 0.5868(6) 0.0870(6) -0.1617(4) 0.0633(19) Uani 1 1 d . . .
H18A H 0.5502 0.1422 -0.1531 0.076 Uiso 1 1 calc R . .
H18B H 0.5793 0.0377 -0.1219 0.076 Uiso 1 1 calc R . .
C19 C 0.5439(7) 0.0542(6) -0.2568(5) 0.076(2) Uani 1 1 d . . .
H19A H 0.4748 0.0345 -0.2685 0.091 Uiso 1 1 calc R . .
H19B H 0.5435 0.1066 -0.2963 0.091 Uiso 1 1 calc R . .
C20 C 0.6017(8) -0.0258(6) -0.2771(5) 0.091(3) Uani 1 1 d . . .
H20A H 0.5932 -0.0814 -0.2447 0.109 Uiso 1 1 calc R . .
H20B H 0.5748 -0.0400 -0.3405 0.109 Uiso 1 1 calc R . .
C21 C 0.7108(7) -0.0040(6) -0.2525(5) 0.082(3) Uani 1 1 d . . .
H21A H 0.7204 0.0448 -0.2919 0.099 Uiso 1 1 calc R . .
H21B H 0.7465 -0.0600 -0.2606 0.099 Uiso 1 1 calc R . .
C22 C 0.7539(6) 0.0290(5) -0.1564(5) 0.066(2) Uani 1 1 d . . .
H22A H 0.7521 -0.0226 -0.1167 0.080 Uiso 1 1 calc R . .
H22B H 0.8236 0.0473 -0.1436 0.080 Uiso 1 1 calc R . .
C23 C 0.8779(5) 0.1894(4) -0.0109(4) 0.0460(15) Uani 1 1 d . . .
H23 H 0.9058 0.1303 -0.0246 0.055 Uiso 1 1 calc R . .
C24 C 0.8961(4) 0.2607(4) -0.0739(4) 0.0445(14) Uani 1 1 d . . .
H24A H 0.8731 0.3222 -0.0621 0.053 Uiso 1 1 calc R . .
H24B H 0.8579 0.2433 -0.1350 0.053 Uiso 1 1 calc R . .
C25 C 1.0068(5) 0.2658(5) -0.0633(4) 0.0565(18) Uani 1 1 d . . .
H25A H 1.0282 0.2057 -0.0803 0.068 Uiso 1 1 calc R . .
H25B H 1.0170 0.3139 -0.1030 0.068 Uiso 1 1 calc R . .
C26 C 1.0686(5) 0.2883(6) 0.0299(5) 0.072(2) Uani 1 1 d . . .
H26A H 1.0516 0.3510 0.0452 0.087 Uiso 1 1 calc R . .
H26B H 1.1392 0.2882 0.0354 0.087 Uiso 1 1 calc R . .
C27 C 1.0508(5) 0.2176(6) 0.0933(5) 0.074(2) Uani 1 1 d . . .
H27A H 1.0899 0.2350 0.1541 0.088 Uiso 1 1 calc R . .
H27B H 1.0735 0.1560 0.0813 0.088 Uiso 1 1 calc R . .
C28 C 0.9407(5) 0.2119(5) 0.0848(4) 0.0567(18) Uani 1 1 d . . .
H28A H 0.9192 0.2717 0.1024 0.068 Uiso 1 1 calc R . .
H28B H 0.9313 0.1632 0.1243 0.068 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'
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'
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 94.10(15) . . ?
C1 Pd1 Br1 174.39(15) . . ?
P1 Pd1 Br1 91.40(5) . . ?
C1 Pd1 Br2 84.27(15) . . ?
P1 Pd1 Br2 176.90(5) . . ?
Br1 Pd1 Br2 90.28(3) . . ?
C23 P1 C17 105.7(3) . . ?
C23 P1 C11 109.2(3) . . ?
C17 P1 C11 103.3(3) . . ?
C23 P1 Pd1 112.70(19) . . ?
C17 P1 Pd1 111.1(2) . . ?
C11 P1 Pd1 114.22(19) . . ?
C1 S1 C7 92.5(3) . . ?
C1 N1 C2 114.9(5) . . ?
C1 N1 C8 123.2(5) . . ?
C2 N1 C8 121.6(4) . . ?
N1 C1 S1 110.4(4) . . ?
N1 C1 Pd1 126.3(4) . . ?
S1 C1 Pd1 123.0(3) . . ?
C7 C2 N1 112.6(5) . . ?
C7 C2 C3 121.6(5) . . ?
N1 C2 C3 125.8(5) . . ?
C4 C3 C2 116.7(6) . . ?
C3 C4 C5 121.8(6) . . ?
C6 C5 C4 121.8(6) . . ?
C5 C6 C7 116.4(6) . . ?
C2 C7 C6 121.6(6) . . ?
C2 C7 S1 109.5(4) . . ?
C6 C7 S1 128.9(5) . . ?
N1 C8 C9 112.3(5) . . ?
C10 C9 C8 111.7(7) . . ?
C12 C11 C16 108.8(5) . . ?
C12 C11 P1 113.0(4) . . ?
C16 C11 P1 117.8(4) . . ?
C11 C12 C13 112.0(6) . . ?
C14 C13 C12 109.6(6) . . ?
C15 C14 C13 110.9(6) . . ?
C14 C15 C16 112.4(6) . . ?
C11 C16 C15 110.4(5) . . ?
C18 C17 C22 111.1(6) . . ?
C18 C17 P1 111.2(4) . . ?
C22 C17 P1 115.2(5) . . ?
C17 C18 C19 110.4(6) . . ?
C20 C19 C18 112.7(7) . . ?
C21 C20 C19 112.2(7) . . ?
C20 C21 C22 111.2(7) . . ?
C17 C22 C21 111.1(7) . . ?
C24 C23 C28 110.7(5) . . ?
C24 C23 P1 115.7(4) . . ?
C28 C23 P1 114.4(4) . . ?
C23 C24 C25 110.9(5) . . ?
C26 C25 C24 111.3(5) . . ?
C25 C26 C27 110.6(7) . . ?
C26 C27 C28 111.8(6) . . ?
C27 C28 C23 109.9(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 C1 1.971(6) . ?
Pd1 P1 2.2895(15) . ?
Pd1 Br1 2.4656(9) . ?
Pd1 Br2 2.4841(8) . ?
P1 C23 1.843(7) . ?
P1 C17 1.852(6) . ?
P1 C11 1.858(6) . ?
S1 C1 1.713(6) . ?
S1 C7 1.747(6) . ?
N1 C1 1.345(7) . ?
N1 C2 1.405(7) . ?
N1 C8 1.464(7) . ?
C2 C7 1.372(8) . ?
C2 C3 1.410(8) . ?
C3 C4 1.368(8) . ?
C4 C5 1.394(9) . ?
C5 C6 1.385(10) . ?
C6 C7 1.400(9) . ?
C8 C9 1.531(8) . ?
C9 C10 1.457(10) . ?
C11 C12 1.520(8) . ?
C11 C16 1.531(8) . ?
C12 C13 1.533(9) . ?
C13 C14 1.521(10) . ?
C14 C15 1.509(11) . ?
C15 C16 1.533(9) . ?
C17 C18 1.511(9) . ?
C17 C22 1.515(9) . ?
C18 C19 1.515(9) . ?
C19 C20 1.507(12) . ?
C20 C21 1.503(12) . ?
C21 C22 1.531(10) . ?
C23 C24 1.515(8) . ?
C23 C28 1.531(8) . ?
C24 C25 1.531(8) . ?
C25 C26 1.495(9) . ?
C26 C27 1.513(11) . ?
C27 C28 1.530(10) . ?
