#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/19/7211924.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_7211924
loop_
_publ_author_name
'Bai, Shi-Qiang'
'Quek, Gabriel Y. H.'
'Koh, Lip Lin'
'Andy Hor, T. S.'
_publ_section_title
;
 Crystallographic analysis of different water--halide cluster blends in
 cationic [(SNS)PdII] pincer complexes
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              226
_journal_paper_doi               10.1039/b917189b
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C12 H30 Cl2 N O1.5 Pd S2'
_chemical_formula_weight         453.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.9110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.9875(16)
_cell_length_b                   8.9087(4)
_cell_length_c                   14.1037(7)
_cell_measurement_reflns_used    5295
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.37
_cell_volume                     3980.8(3)
_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      296(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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13800
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.8957
_exptl_absorpt_correction_T_min  0.7660
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sababs, (Sheldrick 2001)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0305
_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)+(0.0400P)²+0.6586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4015
_reflns_number_total             4567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917189b.txt
_cod_data_source_block           8303
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C12 H30 Cl2 N O1.50 Pd S2'
_cod_database_code               7211924
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Pd1 Pd 0.369329(5) 0.805281(18) 0.629584(11) 0.03723(7) Uani 1 1 d .
Cl1 Cl 0.31029(2) 0.94906(7) 0.63667(5) 0.05936(18) Uani 1 1 d .
Cl2 Cl 0.42664(3) 0.48932(9) 0.44902(5) 0.0754(2) Uani 1 1 d .
S1 S 0.34455(2) 0.60180(7) 0.70721(4) 0.05009(16) Uani 1 1 d .
S2 S 0.403975(19) 0.99771(7) 0.56151(4) 0.04378(14) Uani 1 1 d .
H1N H 0.4216(8) 0.644(3) 0.5810(18) 0.038(7) Uiso 1 1 d .
N1 N 0.42355(7) 0.6855(2) 0.63015(14) 0.0429(5) Uani 1 1 d .
C1 C 0.42801(8) 0.5669(3) 0.70486(17) 0.0520(6) Uani 1 1 d .
H1A H 0.4329 0.6124 0.7679 0.062 Uiso 1 1 calc R
H1B H 0.4519 0.5030 0.6975 0.062 Uiso 1 1 calc R
C2 C 0.38849(9) 0.4759(3) 0.6947(2) 0.0564(7) Uani 1 1 d .
H2A H 0.3905 0.3988 0.7437 0.068 Uiso 1 1 calc R
H2B H 0.3841 0.4275 0.6326 0.068 Uiso 1 1 calc R
C3 C 0.29825(10) 0.5134(3) 0.6332(3) 0.0674(8) Uani 1 1 d .
C4 C 0.29703(14) 0.3487(4) 0.6640(3) 0.1036(14) Uani 1 1 d .
H4A H 0.2979 0.3434 0.7322 0.155 Uiso 1 1 calc R
H4B H 0.3209 0.2967 0.6456 0.155 Uiso 1 1 calc R
H4C H 0.2715 0.3029 0.6334 0.155 Uiso 1 1 calc R
C5 C 0.26022(11) 0.5976(4) 0.6600(4) 0.1086(14) Uani 1 1 d .
H5A H 0.2350 0.5602 0.6228 0.163 Uiso 1 1 calc R
H5B H 0.2632 0.7027 0.6475 0.163 Uiso 1 1 calc R
H5C H 0.2585 0.5831 0.7268 0.163 Uiso 1 1 calc R
C6 C 0.30155(12) 0.5286(4) 0.5277(3) 0.0879(11) Uani 1 1 d .
H6A H 0.2784 0.4770 0.4911 0.132 Uiso 1 1 calc R
H6B H 0.3277 0.4856 0.5147 0.132 Uiso 1 1 calc R
H6C H 0.3007 0.6329 0.5104 0.132 Uiso 1 1 calc R
C7 C 0.46057(8) 0.7869(3) 0.63685(18) 0.0528(6) Uani 1 1 d .
H7A H 0.4859 0.7290 0.6324 0.063 Uiso 1 1 calc R
H7B H 0.4641 0.8384 0.6980 0.063 Uiso 1 1 calc R
C8 C 0.45388(8) 0.8994(3) 0.55685(19) 0.0548(6) Uani 1 1 d .
H8A H 0.4531 0.8487 0.4958 0.066 Uiso 1 1 calc R
H8B H 0.4770 0.9708 0.5633 0.066 Uiso 1 1 calc R
C9 C 0.38185(8) 1.0177(3) 0.43214(17) 0.0476(6) Uani 1 1 d .
C10 C 0.36523(10) 0.8686(3) 0.39121(19) 0.0633(8) Uani 1 1 d .
H10A H 0.3546 0.8807 0.3246 0.095 Uiso 1 1 calc R
H10B H 0.3430 0.8345 0.4251 0.095 Uiso 1 1 calc R
H10C H 0.3877 0.7961 0.3980 0.095 Uiso 1 1 calc R
C11 C 0.34669(10) 1.1325(3) 0.4317(2) 0.0651(8) Uani 1 1 d .
H11A H 0.3322 1.1435 0.3677 0.098 Uiso 1 1 calc R
H11B H 0.3585 1.2273 0.4539 0.098 Uiso 1 1 calc R
H11C H 0.3271 1.0991 0.4731 0.098 Uiso 1 1 calc R
C12 C 0.41640(10) 1.0789(4) 0.37888(19) 0.0642(7) Uani 1 1 d .
H12A H 0.4380 1.0042 0.3776 0.096 Uiso 1 1 calc R
H12B H 0.4284 1.1671 0.4109 0.096 Uiso 1 1 calc R
H12C H 0.4046 1.1040 0.3145 0.096 Uiso 1 1 calc R
O1W O 0.5000 0.1120(4) 0.7500 0.1104(14) Uani 1 2 d SD
H1W H 0.494(2) 0.177(8) 0.705(4) 0.080 Uiso 0.50 1 d PD
H2W H 0.495(3) 0.155(8) 0.802(3) 0.080 Uiso 0.50 1 d PD
O2W O 0.49480(11) 0.3069(4) 0.5906(2) 0.1030(10) Uani 1 1 d D
H3W H 0.5141(9) 0.370(4) 0.599(3) 0.080 Uiso 1 1 d D
H4W H 0.4776(10) 0.340(4) 0.547(2) 0.080 Uiso 1 1 d 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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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
N1 Pd1 Cl1 176.44(6)
N1 Pd1 S1 86.25(6)
Cl1 Pd1 S1 94.54(2)
N1 Pd1 S2 86.20(6)
Cl1 Pd1 S2 92.77(2)
S1 Pd1 S2 171.58(2)
C2 S1 C3 104.44(14)
C2 S1 Pd1 96.73(9)
C3 S1 Pd1 111.31(10)
C8 S2 C9 103.01(12)
C8 S2 Pd1 97.47(9)
C9 S2 Pd1 109.61(8)
C7 N1 C1 112.98(19)
C7 N1 Pd1 110.71(16)
C1 N1 Pd1 111.98(16)
N1 C1 C2 108.7(2)
C1 C2 S1 108.09(18)
C6 C3 C5 111.6(3)
C6 C3 C4 111.9(3)
C5 C3 C4 110.5(3)
C6 C3 S1 110.8(2)
C5 C3 S1 104.7(2)
C4 C3 S1 107.2(2)
N1 C7 C8 109.2(2)
C7 C8 S2 109.09(18)
C10 C9 C11 111.6(2)
C10 C9 C12 111.5(2)
C11 C9 C12 110.2(2)
C10 C9 S2 110.70(16)
C11 C9 S2 104.40(18)
C12 C9 S2 108.22(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N1 2.035(2)
Pd1 Cl1 2.2954(7)
Pd1 S1 2.3135(6)
Pd1 S2 2.3199(6)
S1 C2 1.826(3)
S1 C3 1.865(3)
S2 C8 1.830(3)
S2 C9 1.872(2)
N1 C7 1.482(3)
N1 C1 1.485(3)
C1 C2 1.492(4)
C3 C6 1.512(5)
C3 C5 1.521(5)
C3 C4 1.532(4)
C7 C8 1.502(4)
C9 C10 1.515(3)
C9 C11 1.520(4)
C9 C12 1.520(4)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N Cl2 0.78(2) 2.34(3) 3.108(2) 169(2) .
O1W H1W O2W 0.863(19) 1.99(2) 2.827(4) 163(7) .
O1W H2W O2W 0.86(2) 2.02(4) 2.827(4) 155(7) 2_656
O2W H3W Cl2 0.830(18) 2.45(2) 3.211(4) 154(4) 5_666
O2W H4W Cl2 0.824(17) 2.39(2) 3.191(3) 165(4) .
