#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332139.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332139
loop_
_publ_author_name
'Yoon, Il'
'Seo, Joobeom'
'Lee, Ji-Eun'
'Park, Ki-Min'
'Kim, Jae Sang'
'Lah, Myoung Soo'
'Lee, Shim Sung'
_publ_section_title
;
 Assembly of a Heterobinuclear 2-D Network:  A Rare Example of
 Endo- and Exocyclic Coordination of PdII/AgIin a Single Macrocycle
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3487
_journal_page_last               3489
_journal_paper_doi               10.1021/ic060005i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C19 H22 Cl2 O2 Pd S3'
_chemical_formula_weight         555.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                83.109(2)
_cell_angle_beta                 69.472(2)
_cell_angle_gamma                67.026(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6041(12)
_cell_length_b                   10.6566(12)
_cell_length_c                   10.9529(12)
_cell_measurement_reflns_used    3304
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.99
_cell_volume                     1067.0(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6880
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.589
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0421
_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)+(0.0763P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                3304
_reflns_number_total             4870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060005isup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd Pd 0.86402(4) 0.67472(4) 0.50607(3) 0.03426(14) Uani 1 1 d .
Cl1 Cl 0.69959(16) 0.71196(14) 0.71670(12) 0.0476(3) Uani 1 1 d .
Cl2 Cl 0.99959(14) 0.77807(14) 0.54927(13) 0.0461(3) Uani 1 1 d .
S1 S 0.33105(16) 0.91901(15) 0.49240(13) 0.0484(4) Uani 1 1 d .
S2 S 0.74391(14) 0.56444(12) 0.45451(12) 0.0394(3) Uani 1 1 d .
S3 S 1.02228(14) 0.64107(13) 0.29833(11) 0.0379(3) Uani 1 1 d .
O1 O 0.5527(4) 0.9130(4) 0.1152(4) 0.0515(10) Uani 1 1 d .
O2 O 0.7932(4) 0.8313(5) 0.0746(4) 0.0605(12) Uani 1 1 d .
C1 C 0.6829(6) 0.9054(6) 0.0205(6) 0.0554(16) Uani 1 1 d .
H1A H 0.6833 0.9960 -0.0027 0.067 Uiso 1 1 calc R
H1B H 0.6976 0.8591 -0.0573 0.067 Uiso 1 1 calc R
C2 C 0.5203(5) 0.7971(5) 0.1407(5) 0.0350(11) Uani 1 1 d .
C3 C 0.5993(6) 0.6788(6) 0.0640(5) 0.0451(13) Uani 1 1 d .
H3A H 0.6795 0.6744 -0.0089 0.054 Uiso 1 1 calc R
C4 C 0.5590(7) 0.5697(6) 0.0960(6) 0.0576(16) Uani 1 1 d .
H4A H 0.6133 0.4902 0.0454 0.069 Uiso 1 1 calc R
C5 C 0.4397(7) 0.5747(6) 0.2017(6) 0.0566(16) Uani 1 1 d .
H5A H 0.4126 0.4995 0.2221 0.068 Uiso 1 1 calc R
C6 C 0.3605(6) 0.6920(6) 0.2772(5) 0.0477(13) Uani 1 1 d .
H6A H 0.2794 0.6958 0.3489 0.057 Uiso 1 1 calc R
C7 C 0.4001(5) 0.8052(5) 0.2475(5) 0.0375(11) Uani 1 1 d .
C8 C 0.3132(6) 0.9312(5) 0.3325(5) 0.0493(14) Uani 1 1 d .
H8A H 0.2115 0.9557 0.3436 0.059 Uiso 1 1 calc R
H8B H 0.3414 1.0050 0.2870 0.059 Uiso 1 1 calc R
C9 C 0.5244(6) 0.8237(5) 0.4593(5) 0.0454(13) Uani 1 1 d .
H9A H 0.5769 0.8327 0.3683 0.054 Uiso 1 1 calc R
H9B H 0.5589 0.8605 0.5123 0.054 Uiso 1 1 calc R
C10 C 0.5531(6) 0.6748(5) 0.4893(5) 0.0444(12) Uani 1 1 d .
H10A H 0.5127 0.6412 0.4394 0.053 Uiso 1 1 calc R
H10B H 0.5016 0.6677 0.5809 0.053 Uiso 1 1 calc R
C11 C 0.8068(6) 0.5678(6) 0.2761(5) 0.0474(13) Uani 1 1 d .
H11A H 0.7856 0.5011 0.2420 0.057 Uiso 1 1 calc R
H11B H 0.7559 0.6571 0.2475 0.057 Uiso 1 1 calc R
C12 C 0.9678(6) 0.5361(5) 0.2244(5) 0.0428(12) Uani 1 1 d .
H12A H 0.9972 0.5490 0.1309 0.051 Uiso 1 1 calc R
H12B H 1.0184 0.4410 0.2398 0.051 Uiso 1 1 calc R
C13 C 0.9562(6) 0.8110(5) 0.2294(5) 0.0406(12) Uani 1 1 d .
H13A H 0.8511 0.8447 0.2556 0.049 Uiso 1 1 calc R
H13B H 0.9817 0.8732 0.2651 0.049 Uiso 1 1 calc R
C14 C 1.0183(6) 0.8103(5) 0.0825(5) 0.0361(11) Uani 1 1 d .
C15 C 1.1615(6) 0.7987(5) 0.0199(6) 0.0475(13) Uani 1 1 d .
H15A H 1.2205 0.7892 0.0691 0.057 Uiso 1 1 calc R
C16 C 1.2173(7) 0.8012(6) -0.1151(6) 0.0584(16) Uani 1 1 d .
H16A H 1.3130 0.7937 -0.1567 0.070 Uiso 1 1 calc R
C17 C 1.1295(8) 0.8148(6) -0.1855(6) 0.0618(18) Uani 1 1 d .
H17A H 1.1666 0.8169 -0.2759 0.074 Uiso 1 1 calc R
C18 C 0.9885(7) 0.8256(6) -0.1274(5) 0.0529(15) Uani 1 1 d .
H18A H 0.9309 0.8343 -0.1778 0.064 Uiso 1 1 calc R
C19 C 0.9323(6) 0.8235(5) 0.0076(5) 0.0428(12) 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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S2 Pd S3 89.93(5)
S2 Pd Cl2 176.40(5)
S3 Pd Cl2 87.04(5)
S2 Pd Cl1 89.82(5)
S3 Pd Cl1 179.01(5)
Cl2 Pd Cl1 93.25(5)
C8 S1 C9 102.9(2)
C10 S2 C11 99.8(3)
C10 S2 Pd 110.04(19)
C11 S2 Pd 102.56(19)
C12 S3 C13 104.5(2)
C12 S3 Pd 103.27(18)
C13 S3 Pd 101.42(16)
C2 O1 C1 118.4(4)
C19 O2 C1 118.8(4)
O1 C1 O2 106.5(4)
C7 C2 O1 115.8(4)
C7 C2 C3 120.4(5)
O1 C2 C3 123.8(5)
C4 C3 C2 119.8(5)
C3 C4 C5 121.1(5)
C4 C5 C6 119.3(6)
C5 C6 C7 120.9(5)
C2 C7 C6 118.5(5)
C2 C7 C8 121.7(5)
C6 C7 C8 119.9(5)
C7 C8 S1 116.0(4)
C10 C9 S1 110.3(4)
C9 C10 S2 115.4(4)
C12 C11 S2 110.0(4)
C11 C12 S3 113.3(4)
C14 C13 S3 112.8(3)
C19 C14 C15 118.8(5)
C19 C14 C13 120.3(5)
C15 C14 C13 120.8(5)
C16 C15 C14 120.7(6)
C17 C16 C15 118.8(6)
C16 C17 C18 122.1(5)
C17 C18 C19 119.1(6)
O2 C19 C14 116.2(4)
O2 C19 C18 123.4(5)
C14 C19 C18 120.4(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd S2 2.2703(14)
Pd S3 2.2738(13)
Pd Cl2 2.3112(14)
Pd Cl1 2.3191(13)
S1 C8 1.811(5)
S1 C9 1.819(5)
S2 C10 1.826(5)
S2 C11 1.831(5)
S3 C12 1.814(5)
S3 C13 1.842(5)
O1 C2 1.379(6)
O1 C1 1.384(7)
O2 C19 1.372(6)
O2 C1 1.413(6)
C2 C7 1.377(7)
C2 C3 1.391(7)
C3 C4 1.357(8)
C4 C5 1.370(9)
C5 C6 1.376(8)
C6 C7 1.394(8)
C7 C8 1.500(7)
C9 C10 1.512(7)
C11 C12 1.506(8)
C13 C14 1.509(6)
C14 C19 1.386(7)
C14 C15 1.392(8)
C15 C16 1.388(8)
C16 C17 1.362(9)
C17 C18 1.368(9)
C18 C19 1.389(7)
