#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:21:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180134 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/32/7103205.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_7103205
loop_
_publ_author_name
'Bai, Shi-Qiang'
'Hor, T S Andy'
_publ_section_title
;
 Isolation of an [SNS]Pd(II) pincer with a water ladder and its Suzuki
 coupling activity in water.
;
_journal_issue                   27
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3172
_journal_page_last               3174
_journal_paper_doi               10.1039/b802043d
_journal_year                    2008
_chemical_formula_sum            'C18 H23 Cl2 N Pd S2'
_chemical_formula_weight         494.79
_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                 99.3760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3815(6)
_cell_length_b                   5.6441(3)
_cell_length_c                   28.7929(15)
_cell_measurement_reflns_used    5492
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.87
_cell_volume                     1985.24(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            13376
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.8715
_exptl_absorpt_correction_T_min  0.4376
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0249
_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)+(0.0281P)²+0.8159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                4076
_reflns_number_total             4540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802043d.txt
_cod_data_source_block           2
_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               7103205
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 0.617448(11) 0.20442(3) 0.132441(5) 0.02214(6) Uani 1 1 d . . .
Cl1 Cl 0.71794(5) -0.07170(11) 0.18041(2) 0.04043(14) Uani 1 1 d . . .
Cl2 Cl 0.36054(4) 0.07727(9) 0.038524(19) 0.03346(12) Uani 1 1 d . . .
S1 S 0.48487(4) 0.22022(9) 0.179396(18) 0.02587(11) Uani 1 1 d . . .
S2 S 0.74400(4) 0.22918(10) 0.082698(19) 0.02758(12) Uani 1 1 d . . .
N1 N 0.52691(13) 0.4438(3) 0.09013(6) 0.0227(3) Uani 1 1 d . . .
C1 C 0.45795(17) 0.5904(4) 0.11663(7) 0.0285(4) Uani 1 1 d . . .
H1A H 0.4077 0.6882 0.0948 0.034 Uiso 1 1 calc R . .
H1B H 0.5043 0.6956 0.1385 0.034 Uiso 1 1 calc R . .
C2 C 0.39388(16) 0.4264(4) 0.14356(7) 0.0294(5) Uani 1 1 d . . .
H2A H 0.3403 0.3377 0.1214 0.035 Uiso 1 1 calc R . .
H2B H 0.3538 0.5201 0.1638 0.035 Uiso 1 1 calc R . .
C3 C 0.54675(17) 0.4045(4) 0.22908(7) 0.0320(5) Uani 1 1 d . . .
H3A H 0.6128 0.3274 0.2457 0.038 Uiso 1 1 calc R . .
H3B H 0.5677 0.5585 0.2176 0.038 Uiso 1 1 calc R . .
C4 C 0.46613(17) 0.4393(4) 0.26200(7) 0.0272(4) Uani 1 1 d . . .
C5 C 0.39947(19) 0.6391(4) 0.25933(8) 0.0331(5) Uani 1 1 d . . .
H5 H 0.4086 0.7604 0.2379 0.040 Uiso 1 1 calc R . .
C6 C 0.3202(2) 0.6619(4) 0.28765(8) 0.0365(5) Uani 1 1 d . . .
H6 H 0.2749 0.7965 0.2850 0.044 Uiso 1 1 calc R . .
C7 C 0.30729(18) 0.4859(4) 0.31999(8) 0.0340(5) Uani 1 1 d . . .
H7 H 0.2533 0.5009 0.3393 0.041 Uiso 1 1 calc R . .
C8 C 0.37411(18) 0.2889(4) 0.32364(8) 0.0316(5) Uani 1 1 d . . .
H8 H 0.3662 0.1705 0.3458 0.038 Uiso 1 1 calc R . .
C9 C 0.45272(18) 0.2646(4) 0.29490(8) 0.0305(5) Uani 1 1 d . . .
H9 H 0.4975 0.1293 0.2976 0.037 Uiso 1 1 calc R . .
C10 C 0.59495(16) 0.5913(4) 0.06333(7) 0.0269(4) Uani 1 1 d . . .
H10A H 0.6392 0.7023 0.0847 0.032 Uiso 1 1 calc R . .
H10B H 0.5476 0.6833 0.0393 0.032 Uiso 1 1 calc R . .
C11 C 0.66896(17) 0.4324(4) 0.04015(7) 0.0293(4) Uani 1 1 d . . .
H11A H 0.7208 0.5297 0.0262 0.035 Uiso 1 1 calc R . .
H11B H 0.6249 0.3418 0.0148 0.035 Uiso 1 1 calc R . .
C12 C 0.84558(17) 0.4202(4) 0.11765(8) 0.0354(5) Uani 1 1 d . . .
H12A H 0.8104 0.5681 0.1249 0.043 Uiso 1 1 calc R . .
H12B H 0.8739 0.3413 0.1475 0.043 Uiso 1 1 calc R . .
C13 C 0.93917(16) 0.4763(4) 0.09212(7) 0.0268(4) Uani 1 1 d . . .
C14 C 0.9452(2) 0.6894(4) 0.06872(9) 0.0377(5) Uani 1 1 d . . .
H14 H 0.8877 0.7994 0.0670 0.045 Uiso 1 1 calc R . .
C15 C 1.0353(3) 0.7403(5) 0.04792(9) 0.0496(7) Uani 1 1 d . . .
H15 H 1.0396 0.8864 0.0327 0.059 Uiso 1 1 calc R . .
C16 C 1.1187(2) 0.5786(5) 0.04944(9) 0.0501(7) Uani 1 1 d . . .
H16 H 1.1805 0.6155 0.0358 0.060 Uiso 1 1 calc R . .
C17 C 1.11180(18) 0.3642(5) 0.07080(9) 0.0440(6) Uani 1 1 d . . .
H17 H 1.1675 0.2510 0.0707 0.053 Uiso 1 1 calc R . .
C18 C 1.02318(17) 0.3143(4) 0.09239(8) 0.0321(5) Uani 1 1 d . . .
H18 H 1.0196 0.1678 0.1076 0.039 Uiso 1 1 calc R . .
H1N H 0.4839(19) 0.349(4) 0.0716(9) 0.032(6) Uiso 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'
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'
S S 0.1246 0.1234 '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
N1 Pd1 S1 87.11(5) . . ?
N1 Pd1 S2 87.21(5) . . ?
S1 Pd1 S2 173.75(2) . . ?
N1 Pd1 Cl1 179.07(5) . . ?
S1 Pd1 Cl1 92.37(2) . . ?
S2 Pd1 Cl1 93.34(2) . . ?
C2 S1 C3 102.78(11) . . ?
C2 S1 Pd1 97.31(7) . . ?
C3 S1 Pd1 103.54(7) . . ?
C11 S2 C12 103.24(11) . . ?
C11 S2 Pd1 97.65(7) . . ?
C12 S2 Pd1 99.84(7) . . ?
C1 N1 C10 112.10(16) . . ?
C1 N1 Pd1 111.71(12) . . ?
C10 N1 Pd1 112.33(12) . . ?
N1 C1 C2 108.40(17) . . ?
C1 C2 S1 110.74(14) . . ?
C4 C3 S1 109.36(14) . . ?
C5 C4 C9 118.3(2) . . ?
C5 C4 C3 121.4(2) . . ?
C9 C4 C3 120.16(19) . . ?
C6 C5 C4 121.0(2) . . ?
C5 C6 C7 120.0(2) . . ?
C8 C7 C6 119.6(2) . . ?
C7 C8 C9 120.4(2) . . ?
C8 C9 C4 120.6(2) . . ?
N1 C10 C11 109.40(17) . . ?
C10 C11 S2 110.87(14) . . ?
C13 C12 S2 111.76(15) . . ?
C18 C13 C14 118.4(2) . . ?
C18 C13 C12 119.8(2) . . ?
C14 C13 C12 121.8(2) . . ?
C15 C14 C13 120.2(2) . . ?
C16 C15 C14 120.3(2) . . ?
C17 C16 C15 120.1(2) . . ?
C16 C17 C18 119.8(2) . . ?
C17 C18 C13 121.1(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 N1 2.0300(16) . ?
Pd1 S1 2.2920(5) . ?
Pd1 S2 2.2929(5) . ?
Pd1 Cl1 2.3075(6) . ?
S1 C2 1.819(2) . ?
S1 C3 1.833(2) . ?
S2 C11 1.819(2) . ?
S2 C12 1.829(2) . ?
N1 C1 1.486(2) . ?
N1 C10 1.487(2) . ?
C1 C2 1.513(3) . ?
C3 C4 1.497(3) . ?
C4 C5 1.392(3) . ?
C4 C9 1.396(3) . ?
C5 C6 1.380(3) . ?
C6 C7 1.388(3) . ?
C7 C8 1.380(3) . ?
C8 C9 1.383(3) . ?
C10 C11 1.513(3) . ?
C12 C13 1.504(3) . ?
C13 C18 1.384(3) . ?
C13 C14 1.387(3) . ?
C14 C15 1.380(4) . ?
C15 C16 1.374(4) . ?
C16 C17 1.367(4) . ?
C17 C18 1.376(3) . ?
