# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1005519'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            1
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 N2 O4 Pd'
_chemical_formula_sum            'C12 H12 N2 O4 Pd'
_chemical_formula_weight         354.64

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.8536(11)
_cell_length_b                   7.8906(17)
_cell_length_c                   8.8251(19)
_cell_angle_alpha                78.1348(27)
_cell_angle_beta                 86.3966(28)
_cell_angle_gamma                75.1220(28)
_cell_volume                     319.65(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2245
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.66

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_F_000             176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    1.462
_shelx_estimated_absorpt_T_min   0.629
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microsource
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4614
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.358
_diffrn_reflns_theta_max         30.181
_diffrn_reflns_theta_full        28.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1768
_reflns_number_gt                1755
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0335P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1768
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.5000 0.0000 0.01322(9) Uani 1 2 d S . P . .
O1 O 0.4094(4) 0.2646(2) 0.05899(19) 0.0163(3) Uani 1 1 d . . . . .
O2 O 0.2080(4) 0.6143(2) 0.13873(19) 0.0169(3) Uani 1 1 d . . . . .
N1 N -0.3210(5) 0.2311(3) 0.4301(3) 0.0247(5) Uani 1 1 d . . . . .
C1 C 0.1814(6) 0.0426(3) 0.1823(3) 0.0213(5) Uani 1 1 d . . . . .
H1A H 0.3083 -0.0236 0.1118 0.032 Uiso 1 1 calc R U . . .
H1B H -0.0168 0.0469 0.1623 0.032 Uiso 1 1 calc R U . . .
H1C H 0.2284 -0.0174 0.2896 0.032 Uiso 1 1 calc R U . . .
C2 C 0.2186(5) 0.2299(3) 0.1567(3) 0.0160(4) Uani 1 1 d . . . . .
C3 C 0.0386(5) 0.3542(3) 0.2394(3) 0.0156(4) Uani 1 1 d . . . . .
C4 C 0.0410(5) 0.5353(3) 0.2264(3) 0.0157(4) Uani 1 1 d . . . . .
C5 C -0.1720(5) 0.6522(3) 0.3167(3) 0.0204(5) Uani 1 1 d . . . . .
H5A H -0.0986 0.7530 0.3295 0.031 Uiso 1 1 calc R U . . .
H5B H -0.2038 0.5823 0.4187 0.031 Uiso 1 1 calc R U . . .
H5C H -0.3524 0.6975 0.2606 0.031 Uiso 1 1 calc R U . . .
C6 C -0.1630(5) 0.2872(3) 0.3455(3) 0.0180(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.9750(16) 2_665 ?
Pd1 O2 1.9750(16) . ?
Pd1 O1 1.9770(17) . ?
Pd1 O1 1.9770(17) 2_665 ?
O1 C2 1.268(3) . ?
O2 C4 1.276(3) . ?
N1 C6 1.144(3) . ?
C1 C2 1.504(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.425(3) . ?
C3 C4 1.413(3) . ?
C3 C6 1.435(3) . ?
C4 C5 1.505(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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
O2 Pd1 O2 180.0 2_665 . ?
O2 Pd1 O1 85.70(7) 2_665 . ?
O2 Pd1 O1 94.30(7) . . ?
O2 Pd1 O1 94.30(7) 2_665 2_665 ?
O2 Pd1 O1 85.70(7) . 2_665 ?
O1 Pd1 O1 180.00(10) . 2_665 ?
C2 O1 Pd1 124.59(15) . . ?
C4 O2 Pd1 124.53(15) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.2(2) . . ?
O1 C2 C1 115.9(2) . . ?
C3 C2 C1 118.9(2) . . ?
C4 C3 C2 126.1(2) . . ?
C4 C3 C6 117.6(2) . . ?
C2 C3 C6 116.3(2) . . ?
O2 C4 C3 125.3(2) . . ?
O2 C4 C5 114.8(2) . . ?
C3 C4 C5 119.9(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C3 178.9(3) . . ?

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.132

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2alpha
_database_code_depnum_ccdc_archive 'CCDC 1005520'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Ag N2 O4 Pd, B F4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag B F4 N2 O5 Pd'
_chemical_formula_weight         581.36

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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.6947(9)
_cell_length_b                   17.3278(14)
_cell_length_c                   9.1324(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.1670(10)
_cell_angle_gamma                90
_cell_volume                     1831.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7530
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.59

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    2.117
_shelx_estimated_absorpt_T_min   0.609
_shelx_estimated_absorpt_T_max   0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21198
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.759
_diffrn_reflns_theta_max         26.592
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3820
_reflns_number_gt                3107
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²+4.5803P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3820
_refine_ls_number_parameters     253
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1242
_refine_ls_wR_factor_gt          0.1204
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.25885(3) 0.26193(2) 0.79211(4) 0.01552(13) Uani 1 1 d . . . . .
O1 O 0.3368(2) 0.17595(16) 0.7048(3) 0.0193(6) Uani 1 1 d . . . . .
O2 O 0.3419(2) 0.34231(17) 0.6951(3) 0.0209(6) Uani 1 1 d . . . . .
C1 C 0.4657(4) 0.1089(3) 0.5751(5) 0.0260(10) Uani 1 1 d . . . . .
H1A H 0.5449 0.1035 0.6259 0.039 Uiso 1 1 calc R U . . .
H1B H 0.4663 0.1097 0.4679 0.039 Uiso 1 1 calc R U . . .
H1C H 0.4190 0.0653 0.6009 0.039 Uiso 1 1 calc R U . . .
C2 C 0.4146(3) 0.1832(2) 0.6223(5) 0.0183(8) Uani 1 1 d . . . . .
C3 C 0.4549(4) 0.2557(3) 0.5722(6) 0.0198(9) Uani 1 1 d . . . . .
C4 C 0.4140(3) 0.3299(2) 0.6070(5) 0.0189(9) Uani 1 1 d . . . . .
C5 C 0.4536(4) 0.4010(3) 0.5356(5) 0.0247(10) Uani 1 1 d . . . . .
H5A H 0.3913 0.4202 0.4614 0.037 Uiso 1 1 calc R U . . .
H5B H 0.5212 0.3887 0.4877 0.037 Uiso 1 1 calc R U . . .
H5C H 0.4743 0.4408 0.6111 0.037 Uiso 1 1 calc R U . . .
C6 C 0.5431(4) 0.2516(3) 0.4822(5) 0.0186(9) Uani 1 1 d . . . . .
N1 N 0.6153(3) 0.2472(2) 0.4103(5) 0.0258(9) Uani 1 1 d . . . . .
O3 O 0.1716(2) 0.18133(16) 0.8833(3) 0.0189(6) Uani 1 1 d . . . . .
O4 O 0.1865(2) 0.34804(16) 0.8877(3) 0.0183(6) Uani 1 1 d . . . . .
C7 C 0.0333(4) 0.1243(3) 1.0099(5) 0.0257(10) Uani 1 1 d . . . . .
H7A H 0.0661 0.0779 0.9709 0.039 Uiso 1 1 calc R U . . .
H7B H -0.0493 0.1273 0.9720 0.039 Uiso 1 1 calc R U . . .
H7C H 0.0436 0.1219 1.1182 0.039 Uiso 1 1 calc R U . . .
C8 C 0.0932(3) 0.1941(2) 0.9621(5) 0.0185(8) Uani 1 1 d . . . . .
C9 C 0.0622(4) 0.2686(2) 1.0082(5) 0.0162(9) Uani 1 1 d . . . . .
C10 C 0.1128(3) 0.3405(2) 0.9752(5) 0.0173(8) Uani 1 1 d . . . . .
C11 C 0.0804(4) 0.4130(2) 1.0483(5) 0.0245(9) Uani 1 1 d . . . . .
H11A H 0.1151 0.4574 1.0049 0.037 Uiso 1 1 calc R U . . .
H11B H 0.1087 0.4105 1.1545 0.037 Uiso 1 1 calc R U . . .
H11C H -0.0039 0.4185 1.0334 0.037 Uiso 1 1 calc R U . . .
C12 C -0.0268(4) 0.2722(2) 1.0985(6) 0.0219(10) Uani 1 1 d . . . . .
N2 N -0.0990(3) 0.2742(2) 1.1715(5) 0.0268(9) Uani 1 1 d . . . . .
Ag1 Ag 0.75732(3) 0.26524(2) 0.29098(5) 0.02442(14) Uani 1 1 d . . . . .
O5 O 0.7264(3) 0.4113(2) 0.3177(4) 0.0356(8) Uani 1 1 d D . . . .
H5O H 0.731(4) 0.430(3) 0.403(3) 0.034(15) Uiso 1 1 d D . . . .
C13 C 0.7746(5) 0.4676(3) 0.2297(7) 0.0419(13) Uani 1 1 d . . . . .
H13A H 0.8579 0.4719 0.2626 0.063 Uiso 1 1 calc R U . . .
H13B H 0.7378 0.5177 0.2406 0.063 Uiso 1 1 calc R U . . .
H13C H 0.7613 0.4519 0.1256 0.063 Uiso 1 1 calc R U . . .
B1 B 0.7709(5) 0.0697(3) 0.2188(7) 0.0285(12) Uani 1 1 d . . . . .
F1 F 0.6933(3) 0.0350(2) 0.2949(4) 0.0626(11) Uani 1 1 d . . . . .
F2 F 0.8034(4) 0.0187(2) 0.1185(5) 0.0823(14) Uani 1 1 d . . . . .
F3 F 0.8622(4) 0.0976(2) 0.3135(5) 0.0833(15) Uani 1 1 d . . . . .
F4 F 0.7202(3) 0.13205(18) 0.1347(4) 0.0497(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 1.973(3) . ?
Pd1 O2 1.978(3) . ?
Pd1 O4 1.979(3) . ?
Pd1 O3 1.982(3) . ?
O1 C2 1.267(5) . ?
O2 C4 1.265(5) . ?
C1 C2 1.508(6) . ?
C2 C3 1.438(6) . ?
C3 C6 1.409(7) . ?
C3 C4 1.424(6) . ?
C4 C5 1.498(6) . ?
C6 N1 1.143(6) . ?
N1 Ag1 2.135(4) . ?
O3 C8 1.263(5) . ?
O4 C10 1.262(5) . ?
C7 C8 1.494(6) . ?
C8 C9 1.421(6) . ?
C9 C12 1.419(7) . ?
C9 C10 1.429(6) . ?
C10 C11 1.496(6) . ?
C12 N2 1.149(6) . ?
N2 Ag1 2.134(4) 1_456 ?
Ag1 N2 2.134(4) 1_654 ?
Ag1 O5 2.573(4) . ?
O5 C13 1.431(6) . ?
B1 F1 1.359(6) . ?
B1 F3 1.363(7) . ?
B1 F2 1.365(7) . ?
B1 F4 1.407(6) . ?

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
O1 Pd1 O2 93.80(12) . . ?
O1 Pd1 O4 177.32(12) . . ?
O2 Pd1 O4 86.25(12) . . ?
O1 Pd1 O3 86.15(12) . . ?
O2 Pd1 O3 178.04(12) . . ?
O4 Pd1 O3 93.90(12) . . ?
C2 O1 Pd1 125.2(3) . . ?
C4 O2 Pd1 125.4(3) . . ?
O1 C2 C3 124.9(4) . . ?
O1 C2 C1 115.6(4) . . ?
C3 C2 C1 119.6(4) . . ?
C6 C3 C4 118.2(4) . . ?
C6 C3 C2 116.3(4) . . ?
C4 C3 C2 125.6(4) . . ?
O2 C4 C3 124.8(4) . . ?
O2 C4 C5 114.4(4) . . ?
C3 C4 C5 120.8(4) . . ?
N1 C6 C3 178.8(5) . . ?
C6 N1 Ag1 167.1(4) . . ?
C8 O3 Pd1 125.1(3) . . ?
C10 O4 Pd1 125.1(3) . . ?
O3 C8 C9 124.4(4) . . ?
O3 C8 C7 115.7(4) . . ?
C9 C8 C7 119.9(4) . . ?
C12 C9 C8 116.8(4) . . ?
C12 C9 C10 116.4(4) . . ?
C8 C9 C10 126.8(4) . . ?
O4 C10 C9 124.3(4) . . ?
O4 C10 C11 115.7(4) . . ?
C9 C10 C11 119.9(4) . . ?
N2 C12 C9 179.2(5) . . ?
C12 N2 Ag1 172.5(4) . 1_456 ?
N2 Ag1 N1 175.75(15) 1_654 . ?
N2 Ag1 O5 96.22(13) 1_654 . ?
N1 Ag1 O5 88.02(13) . . ?
C13 O5 Ag1 123.1(3) . . ?
F1 B1 F3 110.6(5) . . ?
F1 B1 F2 109.0(5) . . ?
F3 B1 F2 112.8(5) . . ?
F1 B1 F4 111.0(4) . . ?
F3 B1 F4 107.8(4) . . ?
F2 B1 F4 105.5(5) . . ?

_refine_diff_density_max         1.171
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.176

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3alpha
_database_code_depnum_ccdc_archive 'CCDC 1005521'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Ag N2 O4 Pd, Cl O4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag Cl N2 O9 Pd'
_chemical_formula_weight         594.00

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'
O O 0.0106 0.0060 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.7013(18)
_cell_length_b                   17.518(3)
_cell_length_c                   9.1703(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.006(2)
_cell_angle_gamma                90
_cell_volume                     1861.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6372
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.47

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.211
_shelx_estimated_absorpt_T_min   0.679
_shelx_estimated_absorpt_T_max   0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22129
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.526
_diffrn_reflns_theta_max         26.522
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3852
_reflns_number_gt                3229
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+1.4059P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3852
_refine_ls_number_parameters     272
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.25546(2) 0.26273(2) 0.77536(2) 0.01479(7) Uani 1 1 d . . . . .
O1 O 0.33402(14) 0.17804(9) 0.68737(19) 0.0188(4) Uani 1 1 d . U . . .
O2 O 0.33665(14) 0.34277(9) 0.67802(19) 0.0195(4) Uani 1 1 d . U . . .
C1 C 0.4639(2) 0.11292(14) 0.5601(3) 0.0260(6) Uani 1 1 d . . . . .
H1A H 0.5450 0.1104 0.6043 0.039 Uiso 1 1 calc R U . . .
H1B H 0.4589 0.1113 0.4526 0.039 Uiso 1 1 calc R U . . .
H1C H 0.4219 0.0694 0.5939 0.039 Uiso 1 1 calc R U . . .
C2 C 0.41173(19) 0.18564(14) 0.6053(3) 0.0178(5) Uani 1 1 d . . . . .
C3 C 0.4496(2) 0.25733(14) 0.5557(3) 0.0174(5) Uani 1 1 d . . . . .
C4 C 0.40840(19) 0.33084(14) 0.5892(3) 0.0178(5) Uani 1 1 d . . . . .
C5 C 0.4467(2) 0.40104(14) 0.5170(3) 0.0233(6) Uani 1 1 d . . . . .
H5A H 0.3843 0.4190 0.4424 0.035 Uiso 1 1 calc R U . . .
H5B H 0.5148 0.3892 0.4699 0.035 Uiso 1 1 calc R U . . .
H5C H 0.4661 0.4409 0.5912 0.035 Uiso 1 1 calc R U . . .
C6 C 0.5381(2) 0.25422(14) 0.4639(3) 0.0184(5) Uani 1 1 d . . . . .
N1 N 0.60989(19) 0.25076(12) 0.3908(3) 0.0256(5) Uani 1 1 d . . . . .
O3 O 0.16881(14) 0.18300(9) 0.86636(19) 0.0189(4) Uani 1 1 d . U . . .
O4 O 0.18332(14) 0.34772(9) 0.87108(19) 0.0192(4) Uani 1 1 d . U . . .
C7 C 0.0315(2) 0.12615(14) 0.9954(3) 0.0234(6) Uani 1 1 d . . . . .
H7A H 0.0623 0.0804 0.9534 0.035 Uiso 1 1 calc R U . . .
H7B H -0.0515 0.1299 0.9617 0.035 Uiso 1 1 calc R U . . .
H7C H 0.0448 0.1229 1.1031 0.035 Uiso 1 1 calc R U . . .
C8 C 0.09119(19) 0.19551(14) 0.9464(3) 0.0177(5) Uani 1 1 d . . . . .
C9 C 0.0601(2) 0.26938(13) 0.9933(3) 0.0172(5) Uani 1 1 d . . . . .
C10 C 0.10973(19) 0.34028(14) 0.9597(3) 0.0177(5) Uani 1 1 d . . . . .
C11 C 0.0789(2) 0.41199(14) 1.0329(3) 0.0235(6) Uani 1 1 d . . . . .
H11A H 0.1079 0.4560 0.9834 0.035 Uiso 1 1 calc R U . . .
H11B H 0.1137 0.4114 1.1365 0.035 Uiso 1 1 calc R U . . .
H11C H -0.0052 0.4156 1.0269 0.035 Uiso 1 1 calc R U . . .
C12 C -0.0290(2) 0.27219(13) 1.0838(3) 0.0190(5) Uani 1 1 d . . . . .
N2 N -0.10104(19) 0.27397(12) 1.1566(3) 0.0255(5) Uani 1 1 d . . . . .
Ag1 Ag 0.75328(2) 0.26284(2) 0.27139(3) 0.02259(8) Uani 1 1 d . . . . .
O5 O 0.72035(19) 0.40785(12) 0.3077(2) 0.0355(5) Uani 1 1 d D . . . .
H5O H 0.732(4) 0.415(3) 0.397(2) 0.085(16) Uiso 1 1 d D . . . .
C13 C 0.7700(3) 0.46805(18) 0.2354(4) 0.0394(7) Uani 1 1 d . . . . .
H13A H 0.8530 0.4706 0.2705 0.059 Uiso 1 1 calc R U . . .
H13B H 0.7336 0.5164 0.2565 0.059 Uiso 1 1 calc R U . . .
H13C H 0.7580 0.4588 0.1289 0.059 Uiso 1 1 calc R U . . .
Cl1 Cl 0.76758(6) 0.07082(4) 0.22564(8) 0.02954(16) Uani 1 1 d D . . . .
O6 O 0.72000(19) 0.12694(12) 0.1187(2) 0.0446(6) Uani 1 1 d D U . . .
O7 O 0.6795(2) 0.03189(18) 0.2849(3) 0.0707(8) Uani 1 1 d D U . . .
O8A O 0.8732(9) 0.0291(5) 0.1960(11) 0.048(2) Uani 0.379(12) 1 d D U P A 1
O9A O 0.8619(8) 0.1019(6) 0.3148(12) 0.044(2) Uani 0.379(12) 1 d D U P A 1
O8B O 0.8091(7) 0.0149(2) 0.1330(8) 0.0592(18) Uani 0.621(12) 1 d D U P A 2
O9B O 0.8205(7) 0.1128(4) 0.3539(7) 0.0515(17) Uani 0.621(12) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.9753(16) . ?
Pd1 O1 1.9758(16) . ?
Pd1 O4 1.9764(16) . ?
Pd1 O3 1.9776(16) . ?
O1 C2 1.266(3) . ?
O2 C4 1.266(3) . ?
C1 C2 1.496(3) . ?
C2 C3 1.427(3) . ?
C3 C4 1.424(3) . ?
C3 C6 1.424(4) . ?
C4 C5 1.495(3) . ?
C6 N1 1.147(3) . ?
N1 Ag1 2.138(2) . ?
O3 C8 1.264(3) . ?
O4 C10 1.270(3) . ?
C7 C8 1.501(3) . ?
C8 C9 1.427(3) . ?
C9 C12 1.421(4) . ?
C9 C10 1.423(3) . ?
C10 C11 1.492(3) . ?
C12 N2 1.146(3) . ?
N2 Ag1 2.133(2) 1_456 ?
Ag1 N2 2.133(2) 1_654 ?
Ag1 O5 2.598(2) . ?
O5 C13 1.413(4) . ?
Cl1 O9A 1.390(8) . ?
Cl1 O7 1.406(2) . ?
Cl1 O8B 1.426(4) . ?
Cl1 O6 1.444(2) . ?
Cl1 O9B 1.451(5) . ?
Cl1 O8A 1.492(7) . ?
O8A O9A 1.694(18) . ?

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
O2 Pd1 O1 93.91(7) . . ?
O2 Pd1 O4 85.87(7) . . ?
O1 Pd1 O4 177.22(7) . . ?
O2 Pd1 O3 177.67(7) . . ?
O1 Pd1 O3 86.39(7) . . ?
O4 Pd1 O3 93.94(7) . . ?
C2 O1 Pd1 125.28(15) . . ?
C4 O2 Pd1 125.27(15) . . ?
O1 C2 C3 124.2(2) . . ?
O1 C2 C1 115.5(2) . . ?
C3 C2 C1 120.3(2) . . ?
C4 C3 C6 117.3(2) . . ?
C4 C3 C2 126.7(2) . . ?
C6 C3 C2 116.0(2) . . ?
O2 C4 C3 124.3(2) . . ?
O2 C4 C5 114.6(2) . . ?
C3 C4 C5 121.1(2) . . ?
N1 C6 C3 179.1(3) . . ?
C6 N1 Ag1 170.1(2) . . ?
C8 O3 Pd1 125.09(16) . . ?
C10 O4 Pd1 125.20(15) . . ?
O3 C8 C9 124.5(2) . . ?
O3 C8 C7 115.8(2) . . ?
C9 C8 C7 119.7(2) . . ?
C12 C9 C10 116.8(2) . . ?
C12 C9 C8 116.5(2) . . ?
C10 C9 C8 126.7(2) . . ?
O4 C10 C9 124.2(2) . . ?
O4 C10 C11 115.4(2) . . ?
C9 C10 C11 120.4(2) . . ?
N2 C12 C9 179.5(3) . . ?
C12 N2 Ag1 171.1(2) . 1_456 ?
N2 Ag1 N1 178.68(9) 1_654 . ?
N2 Ag1 O5 96.71(7) 1_654 . ?
N1 Ag1 O5 83.69(8) . . ?
C13 O5 Ag1 126.26(18) . . ?
O9A Cl1 O7 121.8(5) . . ?
O7 Cl1 O8B 103.0(3) . . ?
O9A Cl1 O6 109.4(5) . . ?
O7 Cl1 O6 111.00(15) . . ?
O8B Cl1 O6 101.2(3) . . ?
O7 Cl1 O9B 100.7(4) . . ?
O8B Cl1 O9B 133.6(6) . . ?
O6 Cl1 O9B 106.6(3) . . ?
O9A Cl1 O8A 71.9(9) . . ?
O7 Cl1 O8A 120.2(4) . . ?
O6 Cl1 O8A 117.4(3) . . ?
Cl1 O8A O9A 51.2(4) . . ?
Cl1 O9A O8A 56.9(6) . . ?

_refine_diff_density_max         0.759
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.110

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1005522'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            2c
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H16 Ag N2 O5 Pd, F6 P'
_chemical_formula_sum            'C13 H16 Ag F6 N2 O5 P Pd'
_chemical_formula_weight         639.52

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.358(4)
_cell_length_b                   10.882(5)
_cell_length_c                   10.968(4)
_cell_angle_alpha                116.299(6)
_cell_angle_beta                 96.468(6)
_cell_angle_gamma                91.599(6)
_cell_volume                     991.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4160
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.48

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_F_000             620
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.058
_shelx_estimated_absorpt_T_min   0.587
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3903
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.092
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3903
_reflns_number_gt                3387
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1168P)²+1.2889P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3903
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1765
_refine_ls_wR_factor_gt          0.1688
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.74576(5) 0.49162(5) 0.51702(5) 0.0143(2) Uani 1 1 d . . . . .
O1 O 0.6607(5) 0.4902(5) 0.6747(5) 0.0187(11) Uani 1 1 d . . . . .
O2 O 0.6477(5) 0.6522(5) 0.5241(5) 0.0199(11) Uani 1 1 d . . . . .
C1 C 0.5135(9) 0.5441(8) 0.8437(8) 0.0248(17) Uani 1 1 d . . . . .
H1A H 0.4164 0.4971 0.8053 0.037 Uiso 1 1 calc R U . . .
H1B H 0.5079 0.6304 0.9258 0.037 Uiso 1 1 calc R U . . .
H1C H 0.5751 0.4849 0.8682 0.037 Uiso 1 1 calc R U . . .
C2 C 0.5753(8) 0.5741(8) 0.7404(8) 0.0190(15) Uani 1 1 d . . . . .
C3 C 0.5329(8) 0.6877(8) 0.7174(8) 0.0187(15) Uani 1 1 d . . . . .
C4 C 0.5690(7) 0.7224(8) 0.6142(8) 0.0183(15) Uani 1 1 d . . . . .
C5 C 0.5143(9) 0.8448(9) 0.6030(9) 0.0283(18) Uani 1 1 d . . . . .
H5A H 0.5518 0.8531 0.5269 0.043 Uiso 1 1 calc R U . . .
H5B H 0.5465 0.9278 0.6888 0.043 Uiso 1 1 calc R U . . .
H5C H 0.4085 0.8339 0.5860 0.043 Uiso 1 1 calc R U . . .
C6 C 0.4431(9) 0.7755(8) 0.8092(9) 0.0229(17) Uani 1 1 d . . . . .
N1 N 0.3692(7) 0.8448(7) 0.8856(7) 0.0231(14) Uani 1 1 d . . . . .
O3 O 0.8503(5) 0.3348(5) 0.5152(5) 0.0191(11) Uani 1 1 d . . . . .
O4 O 0.8252(5) 0.4889(5) 0.3572(5) 0.0182(11) Uani 1 1 d . . . . .
C7 C 1.0172(8) 0.1697(8) 0.4621(8) 0.0221(16) Uani 1 1 d . . . . .
H7A H 1.1074 0.2145 0.5233 0.033 Uiso 1 1 calc R U . . .
H7B H 1.0390 0.0958 0.3759 0.033 Uiso 1 1 calc R U . . .
H7C H 0.9570 0.1310 0.5064 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9390(7) 0.2720(7) 0.4328(7) 0.0144(14) Uani 1 1 d . . . . .
C9 C 0.9645(7) 0.2982(8) 0.3202(8) 0.0145(14) Uani 1 1 d . . . . .
C10 C 0.9093(7) 0.4038(8) 0.2892(7) 0.0169(15) Uani 1 1 d . . . . .
C11 C 0.9498(9) 0.4178(9) 0.1671(8) 0.0251(18) Uani 1 1 d . . . . .
H11A H 0.9153 0.3336 0.0832 0.038 Uiso 1 1 calc R U . . .
H11B H 1.0550 0.4327 0.1764 0.038 Uiso 1 1 calc R U . . .
H11C H 0.9055 0.4963 0.1621 0.038 Uiso 1 1 calc R U . . .
C12 C 1.0568(8) 0.2090(8) 0.2307(8) 0.0184(15) Uani 1 1 d . . . . .
N2 N 1.1299(7) 0.1353(7) 0.1599(7) 0.0231(14) Uani 1 1 d . . . . .
Ag1 Ag 0.24827(6) 0.97906(6) 1.03177(6) 0.0223(2) Uani 1 1 d . . . . .
O5 O 0.1931(7) 0.8538(8) 1.1724(7) 0.0423(16) Uani 1 1 d . . . . .
H5O H 0.1000 0.8677 1.2003 0.051 Uiso 1 1 calc R U . . .
C13 C 0.2685(14) 0.7695(16) 1.2176(17) 0.075(4) Uani 1 1 d . . . . .
H13A H 0.2205 0.6760 1.1714 0.113 Uiso 1 1 calc R U . . .
H13B H 0.2705 0.8056 1.3171 0.113 Uiso 1 1 calc R U . . .
H13C H 0.3675 0.7676 1.1962 0.113 Uiso 1 1 calc R U . . .
P1 P 0.2353(2) 1.1748(2) 0.8176(2) 0.0290(5) Uani 1 1 d . . . . .
F1 F 0.2130(6) 1.2634(8) 0.9751(6) 0.0584(18) Uani 1 1 d . . . . .
F2 F 0.3091(7) 1.3058(7) 0.8178(7) 0.0592(18) Uani 1 1 d . . . . .
F3 F 0.2513(7) 1.0859(7) 0.6615(6) 0.0608(18) Uani 1 1 d . . . . .
F4 F 0.0797(6) 1.2118(8) 0.7699(7) 0.0605(18) Uani 1 1 d . . . . .
F5 F 0.3851(6) 1.1372(6) 0.8678(7) 0.0603(19) Uani 1 1 d . . . . .
F6A F 0.1907(19) 1.0202(17) 0.7957(16) 0.037(5) Uiso 0.40(3) 1 d . . P A 1
F6B F 0.1339(12) 1.0608(11) 0.8341(10) 0.035(3) Uiso 0.60(3) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O4 1.969(5) . ?
Pd1 O2 1.972(5) . ?
Pd1 O3 1.984(5) . ?
Pd1 O1 1.989(5) . ?
O1 C2 1.257(9) . ?
O2 C4 1.276(9) . ?
C1 C2 1.479(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.426(11) . ?
C3 C4 1.412(11) . ?
C3 C6 1.419(12) . ?
C4 C5 1.489(11) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N1 1.162(10) . ?
N1 Ag1 2.100(6) . ?
O3 C8 1.275(9) . ?
O4 C10 1.263(9) . ?
C7 C8 1.479(11) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.429(10) . ?
C9 C10 1.429(11) . ?
C9 C12 1.430(11) . ?
C10 C11 1.500(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.145(10) . ?
N2 Ag1 2.105(6) 1_644 ?
Ag1 N2 2.105(6) 1_466 ?
Ag1 O5 2.551(6) . ?
O5 C13 1.396(13) . ?
O5 H5O 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
P1 F2 1.565(6) . ?
P1 F3 1.577(7) . ?
P1 F5 1.579(6) . ?
P1 F1 1.604(6) . ?
P1 F4 1.614(6) . ?
P1 F6A 1.625(14) . ?
P1 F6B 1.626(9) . ?

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
O4 Pd1 O2 86.1(2) . . ?
O4 Pd1 O3 94.1(2) . . ?
O2 Pd1 O3 177.8(2) . . ?
O4 Pd1 O1 178.3(2) . . ?
O2 Pd1 O1 94.0(2) . . ?
O3 Pd1 O1 85.8(2) . . ?
C2 O1 Pd1 124.5(5) . . ?
C4 O2 Pd1 125.5(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.6(7) . . ?
O1 C2 C1 114.9(7) . . ?
C3 C2 C1 120.4(7) . . ?
C4 C3 C6 116.6(8) . . ?
C4 C3 C2 127.7(7) . . ?
C6 C3 C2 115.6(7) . . ?
O2 C4 C3 123.4(7) . . ?
O2 C4 C5 115.4(7) . . ?
C3 C4 C5 121.2(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C3 178.2(9) . . ?
C6 N1 Ag1 176.0(7) . . ?
C8 O3 Pd1 125.5(5) . . ?
C10 O4 Pd1 125.1(5) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 123.2(7) . . ?
O3 C8 C7 115.6(6) . . ?
C9 C8 C7 121.2(6) . . ?
C10 C9 C8 127.1(6) . . ?
C10 C9 C12 117.4(7) . . ?
C8 C9 C12 115.5(7) . . ?
O4 C10 C9 124.8(6) . . ?
O4 C10 C11 115.4(7) . . ?
C9 C10 C11 119.8(6) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 178.5(8) . . ?
C12 N2 Ag1 172.4(6) . 1_644 ?
N1 Ag1 N2 169.8(2) . 1_466 ?
N1 Ag1 O5 104.1(2) . . ?
N2 Ag1 O5 86.1(2) 1_466 . ?
C13 O5 Ag1 134.6(7) . . ?
C13 O5 H5O 112.7 . . ?
Ag1 O5 H5O 112.7 . . ?
O5 C13 H13A 109.5 . . ?
O5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
F2 P1 F3 91.2(4) . . ?
F2 P1 F5 91.2(4) . . ?
F3 P1 F5 92.6(4) . . ?
F2 P1 F1 90.0(4) . . ?
F3 P1 F1 177.9(4) . . ?
F5 P1 F1 89.1(4) . . ?
F2 P1 F4 90.2(4) . . ?
F3 P1 F4 88.7(4) . . ?
F5 P1 F4 178.0(4) . . ?
F1 P1 F4 89.6(4) . . ?
F2 P1 F6A 165.7(8) . . ?
F3 P1 F6A 78.4(7) . . ?
F5 P1 F6A 79.6(7) . . ?
F1 P1 F6A 100.7(7) . . ?
F4 P1 F6A 99.2(7) . . ?
F2 P1 F6B 167.8(6) . . ?
F3 P1 F6B 97.2(5) . . ?
F5 P1 F6B 97.2(5) . . ?
F1 P1 F6B 81.3(5) . . ?
F4 P1 F6B 81.2(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C2 C3 -3.8(10) . . . . ?
Pd1 O1 C2 C1 173.6(5) . . . . ?
O1 C2 C3 C4 4.5(12) . . . . ?
C1 C2 C3 C4 -172.8(7) . . . . ?
O1 C2 C3 C6 -175.8(7) . . . . ?
C1 C2 C3 C6 6.9(11) . . . . ?
Pd1 O2 C4 C3 -4.7(10) . . . . ?
Pd1 O2 C4 C5 176.2(5) . . . . ?
C6 C3 C4 O2 -179.4(7) . . . . ?
C2 C3 C4 O2 0.3(12) . . . . ?
C6 C3 C4 C5 -0.3(10) . . . . ?
C2 C3 C4 C5 179.4(8) . . . . ?
Pd1 O3 C8 C9 -6.4(9) . . . . ?
Pd1 O3 C8 C7 172.7(5) . . . . ?
O3 C8 C9 C10 6.5(11) . . . . ?
C7 C8 C9 C10 -172.5(7) . . . . ?
O3 C8 C9 C12 -174.1(6) . . . . ?
C7 C8 C9 C12 6.8(10) . . . . ?
Pd1 O4 C10 C9 -2.3(10) . . . . ?
Pd1 O4 C10 C11 177.1(5) . . . . ?
C8 C9 C10 O4 -1.8(12) . . . . ?
C12 C9 C10 O4 178.9(6) . . . . ?
C8 C9 C10 C11 178.9(7) . . . . ?
C12 C9 C10 C11 -0.4(10) . . . . ?

_refine_diff_density_max         2.544
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.254

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1005523'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            6
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H12 Ag F3 N2 O7 Pd S, C H2 Cl2'
_chemical_formula_sum            'C14 H14 Ag Cl2 F3 N2 O7 Pd S'
_chemical_formula_weight         696.50

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'
Ag Ag -0.8971 1.1015 '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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9183(13)
_cell_length_b                   10.7825(14)
_cell_length_c                   11.6604(15)
_cell_angle_alpha                65.896(2)
_cell_angle_beta                 71.7491(19)
_cell_angle_gamma                88.957(2)
_cell_volume                     1072.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1831
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      25.46

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15506
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         30.03
_reflns_number_total             5733
_reflns_number_gt                3811
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0264P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5733
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0720
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_iucr_refine_instruction_details 
;
TITL c12_17 in P-1                
CELL  0.71073     9.9183   10.7825   11.6604   65.8965   71.7491   88.9573
ZERR  2          0.0013    0.0014    0.0015    0.0020    0.0019    0.0021 
LATT   1
SFAC  C   H   AG  CL  F   N   O   PD  S
UNIT   28    28   2   4   6   4  14   2   2
L.S. 6
SIZE 0.14 0.10 0.04
FMAP 2
TEMP -173
PLAN -20
ACTA 56
BOND $H
CONF
WGHT    0.026400
FVAR       0.25803
AG1   3    0.252409    1.006627   -0.001166    11.00000    0.01359    0.02497 =
         0.01974   -0.01093    0.00250    0.00354
PD1   8   -0.500000    1.000000    0.500000    10.50000    0.00947    0.01734 =
         0.01474   -0.00895   -0.00078    0.00148
PD2   8    1.000000    1.000000   -0.500000    10.50000    0.00951    0.01838 =
         0.01210   -0.00584   -0.00055    0.00247
O1    7    0.842996    0.859196   -0.356344    11.00000    0.01374    0.02127 =
         0.01419   -0.00479   -0.00014    0.00307
O2    7    0.894496    1.154562   -0.490125    11.00000    0.01200    0.02196 =
         0.01574   -0.00948    0.00036    0.00411
O3    7   -0.388226    0.858648    0.463734    11.00000    0.01388    0.01703 =
         0.01723   -0.00791    0.00145    0.00113
O4    7   -0.350437    1.153265    0.365493    11.00000    0.01192    0.02001 =
         0.01790   -0.00948   -0.00191    0.00186
N1    6    0.442365    1.031151   -0.158730    11.00000    0.01446    0.02471 =
         0.01886   -0.00793    0.00095    0.00313
N2    6    0.066475    1.021378    0.141109    11.00000    0.01833    0.01986 =
         0.02337   -0.01026   -0.00119    0.00397
C1    1    0.621287    0.759629   -0.189036    11.00000    0.01809    0.02477 =
         0.02166   -0.00551    0.00000    0.00400
AFIX 137
H1A   2    0.552204    0.742402   -0.226922    11.00000   -1.50000
H1B   2    0.570523    0.775644   -0.110434    11.00000   -1.50000
H1C   2    0.672945    0.679985   -0.163080    11.00000   -1.50000
AFIX   0
C2    1    0.725410    0.883094   -0.290841    11.00000    0.01454    0.02722 =
         0.01284   -0.00704   -0.00466    0.00271
C3    1    0.687816    1.017076   -0.311834    11.00000    0.01005    0.02200 =
         0.01459   -0.00791   -0.00243    0.00279
C4    1    0.769223    1.142751   -0.410845    11.00000    0.01816    0.02166 =
         0.01338   -0.00932   -0.00776    0.00487
C5    1    0.704948    1.273303   -0.428908    11.00000    0.01654    0.02355 =
         0.02052   -0.01265   -0.00646    0.00620
AFIX 137
H5A   2    0.776014    1.351073   -0.497518    11.00000   -1.50000
H5B   2    0.675275    1.282336   -0.344511    11.00000   -1.50000
H5C   2    0.621481    1.271952   -0.456519    11.00000   -1.50000
AFIX   0
C6    1    0.551023    1.025343   -0.226779    11.00000    0.01848    0.02086 =
         0.01734   -0.00908   -0.00840    0.00334
C7    1   -0.198782    0.759289    0.370539    11.00000    0.01793    0.02070 =
         0.03339   -0.01491    0.00071    0.00456
AFIX 137
H7A   2   -0.123638    0.742015    0.411287    11.00000   -1.50000
H7B   2   -0.157192    0.775316    0.276812    11.00000   -1.50000
H7C   2   -0.272605    0.679669    0.418049    11.00000   -1.50000
AFIX   0
C8    1   -0.264367    0.882886    0.378898    11.00000    0.01383    0.02374 =
         0.01929   -0.01276   -0.00552    0.00339
C9    1   -0.185084    1.014270    0.297487    11.00000    0.01020    0.02280 =
         0.01357   -0.00991   -0.00121    0.00089
C10   1   -0.228155    1.141884    0.295367    11.00000    0.01251    0.02356 =
         0.01421   -0.00860   -0.00520    0.00216
C11   1   -0.127396    1.270792    0.208741    11.00000    0.01513    0.01928 =
         0.01713   -0.00811   -0.00182    0.00120
AFIX 137
H11A  2   -0.171467    1.347169    0.224182    11.00000   -1.50000
H11B  2   -0.105816    1.288846    0.114966    11.00000   -1.50000
H11C  2   -0.038668    1.261099    0.230130    11.00000   -1.50000
AFIX   0
C12   1   -0.045065    1.019841    0.209518    11.00000    0.01958    0.01878 =
         0.02059   -0.00997   -0.00793    0.00335
MOLE 2
S1    9    0.237569    0.679550    0.098852    11.00000    0.02174    0.02100 =
         0.01960   -0.00994   -0.00636    0.00187
O5    7    0.131066    0.763302    0.054683    11.00000    0.03203    0.02393 =
         0.02942   -0.01013   -0.01781    0.00823
O6    7    0.338873    0.750916    0.124842    11.00000    0.02427    0.02236 =
         0.02597   -0.00821   -0.00927   -0.00392
O7    7    0.298223    0.599624    0.027499    11.00000    0.03632    0.03578 =
         0.03110   -0.02343   -0.00747    0.01073
C13   1    0.133142    0.551223    0.263793    11.00000    0.02286    0.02625 =
         0.03200   -0.01529   -0.00865    0.00144
F1    5    0.070683    0.608989    0.345841    11.00000    0.02290    0.04136 =
         0.02497   -0.01355    0.00073    0.00615
F3    5    0.215145    0.465580    0.319671    11.00000    0.04028    0.02764 =
         0.03376   -0.00372   -0.01176    0.01328
F2    5    0.030085    0.480129    0.258005    11.00000    0.04461    0.04099 =
         0.04647   -0.01021   -0.01597   -0.02246
MOLE 3
CL1   4    0.548139    0.496977    0.335002    11.00000    0.03215    0.04222 =
         0.02670   -0.00131   -0.00536    0.00530
CL2   4    0.779669    0.659073    0.090224    11.00000    0.03040    0.03327 =
         0.03979   -0.01433    0.00178   -0.00457
C14   1    0.608301    0.566421    0.160484    11.00000    0.02752    0.03734 =
         0.02570   -0.01375   -0.00642    0.00173
AFIX  23
H14A  2    0.540364    0.627695    0.127099    11.00000   -1.20000
H14B  2    0.610376    0.491459    0.131891    11.00000   -1.20000
HKLF 4
;

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
Ag1 Ag 0.25241(3) 1.00663(3) -0.00117(3) 0.02102(8) Uani 1 1 d . . .
Pd1 Pd -0.5000 1.0000 0.5000 0.01394(9) Uani 1 2 d S . .
Pd2 Pd 1.0000 1.0000 -0.5000 0.01435(9) Uani 1 2 d S . .
O1 O 0.8430(3) 0.8592(2) -0.3563(2) 0.0185(6) Uani 1 1 d . . .
O2 O 0.8945(2) 1.1546(2) -0.4901(2) 0.0174(5) Uani 1 1 d . . .
O3 O -0.3882(3) 0.8586(2) 0.4637(2) 0.0175(5) Uani 1 1 d . . .
O4 O -0.3504(2) 1.1533(2) 0.3655(2) 0.0169(5) Uani 1 1 d . . .
N1 N 0.4424(3) 1.0312(3) -0.1587(3) 0.0215(7) Uani 1 1 d . . .
N2 N 0.0665(3) 1.0214(3) 0.1411(3) 0.0216(7) Uani 1 1 d . . .
C1 C 0.6213(4) 0.7596(4) -0.1890(4) 0.0248(9) Uani 1 1 d . . .
H1A H 0.5522 0.7424 -0.2269 0.037 Uiso 1 1 calc R . .
H1B H 0.5705 0.7756 -0.1104 0.037 Uiso 1 1 calc R . .
H1C H 0.6729 0.6800 -0.1631 0.037 Uiso 1 1 calc R . .
C2 C 0.7254(4) 0.8831(4) -0.2908(3) 0.0187(8) Uani 1 1 d . . .
C3 C 0.6878(4) 1.0171(4) -0.3118(3) 0.0160(7) Uani 1 1 d . . .
C4 C 0.7692(4) 1.1428(4) -0.4108(3) 0.0165(8) Uani 1 1 d . . .
C5 C 0.7049(4) 1.2733(4) -0.4289(3) 0.0190(8) Uani 1 1 d . . .
H5A H 0.7760 1.3511 -0.4975 0.029 Uiso 1 1 calc R . .
H5B H 0.6753 1.2823 -0.3445 0.029 Uiso 1 1 calc R . .
H5C H 0.6215 1.2720 -0.4565 0.029 Uiso 1 1 calc R . .
C6 C 0.5510(4) 1.0253(4) -0.2268(4) 0.0179(8) Uani 1 1 d . . .
C7 C -0.1988(4) 0.7593(4) 0.3705(4) 0.0252(9) Uani 1 1 d . . .
H7A H -0.1236 0.7420 0.4113 0.038 Uiso 1 1 calc R . .
H7B H -0.1572 0.7753 0.2768 0.038 Uiso 1 1 calc R . .
H7C H -0.2726 0.6797 0.4180 0.038 Uiso 1 1 calc R . .
C8 C -0.2644(4) 0.8829(4) 0.3789(4) 0.0177(8) Uani 1 1 d . . .
C9 C -0.1851(4) 1.0143(4) 0.2975(3) 0.0155(7) Uani 1 1 d . . .
C10 C -0.2282(4) 1.1419(4) 0.2954(3) 0.0164(8) Uani 1 1 d . . .
C11 C -0.1274(4) 1.2708(3) 0.2087(3) 0.0180(8) Uani 1 1 d . . .
H11A H -0.1715 1.3472 0.2242 0.027 Uiso 1 1 calc R . .
H11B H -0.1058 1.2889 0.1150 0.027 Uiso 1 1 calc R . .
H11C H -0.0387 1.2611 0.2301 0.027 Uiso 1 1 calc R . .
C12 C -0.0451(4) 1.0198(4) 0.2095(4) 0.0188(8) Uani 1 1 d . . .
S1 S 0.23757(10) 0.67955(10) 0.09885(9) 0.0204(2) Uani 1 1 d . . .
O5 O 0.1311(3) 0.7633(3) 0.0547(3) 0.0270(6) Uani 1 1 d . . .
O6 O 0.3389(3) 0.7509(3) 0.1248(2) 0.0246(6) Uani 1 1 d . . .
O7 O 0.2982(3) 0.5996(3) 0.0275(3) 0.0322(7) Uani 1 1 d . . .
C13 C 0.1331(4) 0.5512(4) 0.2638(4) 0.0261(9) Uani 1 1 d . . .
F1 F 0.0707(2) 0.6090(2) 0.3458(2) 0.0322(6) Uani 1 1 d . . .
F3 F 0.2151(3) 0.4656(2) 0.3197(2) 0.0374(6) Uani 1 1 d . . .
F2 F 0.0301(3) 0.4801(3) 0.2580(3) 0.0464(7) Uani 1 1 d . . .
Cl1 Cl 0.54814(12) 0.49698(12) 0.33500(10) 0.0395(3) Uani 1 1 d . . .
Cl2 Cl 0.77967(12) 0.65907(11) 0.09022(11) 0.0383(3) Uani 1 1 d . . .
C14 C 0.6083(4) 0.5664(4) 0.1605(4) 0.0307(10) Uani 1 1 d . . .
H14A H 0.5404 0.6277 0.1271 0.037 Uiso 1 1 calc R . .
H14B H 0.6104 0.4915 0.1319 0.037 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Ag1 N1 2.109(3) . ?
Ag1 N2 2.114(3) . ?
Pd1 O3 1.975(2) 2_476 ?
Pd1 O3 1.975(2) . ?
Pd1 O4 1.976(2) . ?
Pd1 O4 1.976(2) 2_476 ?
Pd2 O2 1.976(2) 2_774 ?
Pd2 O2 1.976(2) . ?
Pd2 O1 1.978(2) . ?
Pd2 O1 1.978(2) 2_774 ?
O1 C2 1.266(4) . ?
O2 C4 1.267(4) . ?
O3 C8 1.263(4) . ?
O4 C10 1.269(4) . ?
N1 C6 1.139(4) . ?
N2 C12 1.139(4) . ?
C1 C2 1.496(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.426(5) . ?
C3 C4 1.414(5) . ?
C3 C6 1.434(5) . ?
C4 C5 1.497(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C8 1.498(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.415(5) . ?
C9 C10 1.426(5) . ?
C9 C12 1.430(5) . ?
C10 C11 1.491(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
S1 O7 1.432(3) . ?
S1 O6 1.450(3) . ?
S1 O5 1.457(3) . ?
S1 C13 1.821(4) . ?
C13 F2 1.323(4) . ?
C13 F3 1.324(4) . ?
C13 F1 1.337(4) . ?
Cl1 C14 1.752(4) . ?
Cl2 C14 1.755(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?

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 Ag1 N2 169.57(12) . . ?
O3 Pd1 O3 180.0 2_476 . ?
O3 Pd1 O4 86.05(10) 2_476 . ?
O3 Pd1 O4 93.95(10) . . ?
O3 Pd1 O4 93.95(10) 2_476 2_476 ?
O3 Pd1 O4 86.05(10) . 2_476 ?
O4 Pd1 O4 180.0 . 2_476 ?
O2 Pd2 O2 179.998(2) 2_774 . ?
O2 Pd2 O1 86.15(10) 2_774 . ?
O2 Pd2 O1 93.85(10) . . ?
O2 Pd2 O1 93.85(10) 2_774 2_774 ?
O2 Pd2 O1 86.15(10) . 2_774 ?
O1 Pd2 O1 180.0 . 2_774 ?
C2 O1 Pd2 125.3(2) . . ?
C4 O2 Pd2 125.0(2) . . ?
C8 O3 Pd1 124.6(2) . . ?
C10 O4 Pd1 125.7(2) . . ?
C6 N1 Ag1 167.8(3) . . ?
C12 N2 Ag1 169.0(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.1(3) . . ?
O1 C2 C1 115.7(3) . . ?
C3 C2 C1 120.2(3) . . ?
C4 C3 C2 126.8(3) . . ?
C4 C3 C6 116.5(3) . . ?
C2 C3 C6 116.7(3) . . ?
O2 C4 C3 124.7(3) . . ?
O2 C4 C5 115.9(3) . . ?
C3 C4 C5 119.4(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C3 179.6(5) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 125.1(3) . . ?
O3 C8 C7 115.3(3) . . ?
C9 C8 C7 119.5(3) . . ?
C8 C9 C10 127.2(3) . . ?
C8 C9 C12 116.6(3) . . ?
C10 C9 C12 116.2(3) . . ?
O4 C10 C9 123.3(3) . . ?
O4 C10 C11 116.5(3) . . ?
C9 C10 C11 120.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 178.5(4) . . ?
O7 S1 O6 115.41(17) . . ?
O7 S1 O5 115.75(16) . . ?
O6 S1 O5 113.23(16) . . ?
O7 S1 C13 103.40(18) . . ?
O6 S1 C13 103.63(17) . . ?
O5 S1 C13 103.19(17) . . ?
F2 C13 F3 108.8(3) . . ?
F2 C13 F1 107.1(3) . . ?
F3 C13 F1 106.9(3) . . ?
F2 C13 S1 111.2(3) . . ?
F3 C13 S1 111.2(3) . . ?
F1 C13 S1 111.4(3) . . ?
Cl1 C14 Cl2 111.9(2) . . ?
Cl1 C14 H14A 109.2 . . ?
Cl2 C14 H14A 109.2 . . ?
Cl1 C14 H14B 109.2 . . ?
Cl2 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Pd2 O1 C2 178.3(3) 2_774 . . . ?
O2 Pd2 O1 C2 -1.7(3) . . . . ?
O1 Pd2 O2 C4 -0.2(3) . . . . ?
O1 Pd2 O2 C4 179.8(3) 2_774 . . . ?
O4 Pd1 O3 C8 0.4(3) . . . . ?
O4 Pd1 O3 C8 -179.6(3) 2_476 . . . ?
O3 Pd1 O4 C10 176.8(3) 2_476 . . . ?
O3 Pd1 O4 C10 -3.2(3) . . . . ?
N2 Ag1 N1 C6 139.7(13) . . . . ?
N1 Ag1 N2 C12 114.9(16) . . . . ?
Pd2 O1 C2 C3 0.4(5) . . . . ?
Pd2 O1 C2 C1 178.5(2) . . . . ?
O1 C2 C3 C4 3.5(6) . . . . ?
C1 C2 C3 C4 -174.5(3) . . . . ?
O1 C2 C3 C6 -178.9(3) . . . . ?
C1 C2 C3 C6 3.1(5) . . . . ?
Pd2 O2 C4 C3 3.6(5) . . . . ?
Pd2 O2 C4 C5 -174.7(2) . . . . ?
C2 C3 C4 O2 -5.7(6) . . . . ?
C6 C3 C4 O2 176.6(3) . . . . ?
C2 C3 C4 C5 172.5(3) . . . . ?
C6 C3 C4 C5 -5.1(5) . . . . ?
Pd1 O3 C8 C9 0.8(5) . . . . ?
Pd1 O3 C8 C7 178.7(2) . . . . ?
O3 C8 C9 C10 0.1(6) . . . . ?
C7 C8 C9 C10 -177.7(3) . . . . ?
O3 C8 C9 C12 178.7(3) . . . . ?
C7 C8 C9 C12 0.8(5) . . . . ?
Pd1 O4 C10 C9 4.8(5) . . . . ?
Pd1 O4 C10 C11 -174.7(2) . . . . ?
C8 C9 C10 O4 -3.2(6) . . . . ?
C12 C9 C10 O4 178.3(3) . . . . ?
C8 C9 C10 C11 176.3(3) . . . . ?
C12 C9 C10 C11 -2.3(5) . . . . ?
O7 S1 C13 F2 -62.0(3) . . . . ?
O6 S1 C13 F2 177.2(3) . . . . ?
O5 S1 C13 F2 58.9(3) . . . . ?
O7 S1 C13 F3 59.4(3) . . . . ?
O6 S1 C13 F3 -61.3(3) . . . . ?
O5 S1 C13 F3 -179.6(3) . . . . ?
O7 S1 C13 F1 178.5(3) . . . . ?
O6 S1 C13 F1 57.8(3) . . . . ?
O5 S1 C13 F1 -60.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.133



_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1005524'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            7
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Ag2 N4 O10 Pd'
_chemical_formula_sum            'C12 H12 Ag2 N4 O10 Pd'
_chemical_formula_weight         694.40

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.6283(8)
_cell_length_b                   25.815(4)
_cell_length_c                   7.8121(13)
_cell_angle_alpha                90
_cell_angle_beta                 105.265(2)
_cell_angle_gamma                90
_cell_volume                     900.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4815
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      26.57

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_F_000             664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.205
_shelx_estimated_absorpt_T_min   0.719
_shelx_estimated_absorpt_T_max   0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10789
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.816
_diffrn_reflns_theta_max         26.613
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1878
_reflns_number_gt                1768
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0215P)²+0.3205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1878
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0440
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.5000 0.0000 0.5000 0.01282(7) Uani 1 2 d S . P . .
O1 O 1.3748(3) 0.05489(6) 0.6435(2) 0.0166(3) Uani 1 1 d . . . . .
O2 O 1.1858(3) 0.01711(6) 0.2805(2) 0.0163(3) Uani 1 1 d . . . . .
C1 C 1.0983(6) 0.12375(9) 0.7166(3) 0.0221(5) Uani 1 1 d . . . . .
H1A H 1.2448 0.1187 0.8313 0.033 Uiso 1 1 calc R U . . .
H1B H 0.8956 0.1192 0.7307 0.033 Uiso 1 1 calc R U . . .
H1C H 1.1190 0.1588 0.6731 0.033 Uiso 1 1 calc R U . . .
C2 C 1.1524(5) 0.08490(9) 0.5861(3) 0.0161(5) Uani 1 1 d . . . . .
C3 C 0.9592(5) 0.08379(8) 0.4118(3) 0.0141(4) Uani 1 1 d . . . . .
C4 C 0.9866(5) 0.05162(8) 0.2703(3) 0.0150(4) Uani 1 1 d . . . . .
C5 C 0.7665(5) 0.05733(9) 0.0912(3) 0.0194(5) Uani 1 1 d . . . . .
H5A H 0.8277 0.0352 0.0051 0.029 Uiso 1 1 calc R U . . .
H5B H 0.7617 0.0935 0.0528 0.029 Uiso 1 1 calc R U . . .
H5C H 0.5667 0.0470 0.0992 0.029 Uiso 1 1 calc R U . . .
C6 C 0.7171(5) 0.12021(8) 0.3727(3) 0.0162(5) Uani 1 1 d . . . . .
N1 N 0.5205(5) 0.14839(8) 0.3393(3) 0.0202(4) Uani 1 1 d . . . . .
Ag1 Ag 0.19086(4) 0.20978(2) 0.23924(2) 0.02277(7) Uani 1 1 d . . . . .
N2 N -0.2192(5) 0.21589(7) -0.1113(3) 0.0193(4) Uani 1 1 d . . . . .
O3 O 0.0185(4) 0.24306(7) -0.0536(2) 0.0249(4) Uani 1 1 d . . . . .
O4 O -0.3815(4) 0.22340(7) -0.2630(2) 0.0251(4) Uani 1 1 d . . . . .
O5 O -0.2756(4) 0.18217(6) -0.0104(2) 0.0256(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.9840(15) 3_856 ?
Pd1 O2 1.9840(15) . ?
Pd1 O1 1.9856(15) . ?
Pd1 O1 1.9856(15) 3_856 ?
O1 C2 1.272(3) . ?
O2 C4 1.269(3) . ?
C1 C2 1.497(3) . ?
C2 C3 1.419(3) . ?
C3 C4 1.415(3) . ?
C3 C6 1.432(3) . ?
C4 C5 1.505(3) . ?
C6 N1 1.140(3) . ?
N1 Ag1 2.196(2) . ?
Ag1 O3 2.3273(17) 4_566 ?
Ag1 O3 2.3767(18) . ?
Ag1 O5 2.5994(18) . ?
N2 O4 1.240(3) . ?
N2 O5 1.247(3) . ?
N2 O3 1.282(3) . ?
O3 Ag1 2.3272(17) 4_565 ?

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
O2 Pd1 O2 180.0 3_856 . ?
O2 Pd1 O1 85.85(6) 3_856 . ?
O2 Pd1 O1 94.15(6) . . ?
O2 Pd1 O1 94.15(6) 3_856 3_856 ?
O2 Pd1 O1 85.85(6) . 3_856 ?
O1 Pd1 O1 180.0 . 3_856 ?
C2 O1 Pd1 124.42(14) . . ?
C4 O2 Pd1 124.46(14) . . ?
O1 C2 C3 125.0(2) . . ?
O1 C2 C1 115.7(2) . . ?
C3 C2 C1 119.4(2) . . ?
C4 C3 C2 126.7(2) . . ?
C4 C3 C6 116.4(2) . . ?
C2 C3 C6 116.8(2) . . ?
O2 C4 C3 125.2(2) . . ?
O2 C4 C5 115.47(19) . . ?
C3 C4 C5 119.37(19) . . ?
N1 C6 C3 178.5(3) . . ?
C6 N1 Ag1 168.42(19) . . ?
N1 Ag1 O3 117.60(7) . 4_566 ?
N1 Ag1 O3 128.99(7) . . ?
O3 Ag1 O3 112.99(4) 4_566 . ?
N1 Ag1 O5 115.54(7) . . ?
O3 Ag1 O5 107.22(6) 4_566 . ?
O3 Ag1 O5 51.29(5) . . ?
O4 N2 O5 122.5(2) . . ?
O4 N2 O3 119.9(2) . . ?
O5 N2 O3 117.6(2) . . ?
N2 O3 Ag1 117.47(14) . 4_565 ?
N2 O3 Ag1 100.37(13) . . ?
Ag1 O3 Ag1 140.24(8) 4_565 . ?
N2 O5 Ag1 90.68(13) . . ?

_refine_diff_density_max         0.445
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.089

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2beta
_database_code_depnum_ccdc_archive 'CCDC 1042065'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Ag N2 O4 Pd, B F4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag B F4 N2 O5 Pd'
_chemical_formula_weight         581.36

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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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'

_cell_length_a                   11.9640(16)
_cell_length_b                   17.688(2)
_cell_length_c                   9.1080(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.437(3)
_cell_angle_gamma                90
_cell_volume                     1915.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    2002
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      25.22

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.025
_shelx_estimated_absorpt_T_min   0.331
_shelx_estimated_absorpt_T_max   0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5071
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.909
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1747
_reflns_number_gt                1520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1747
_refine_ls_number_parameters     137
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.1291
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.51102(3) 0.7500 0.0422(2) Uani 1 2 d S T P . .
Ag1 Ag 1.0000 0.51364(4) 0.2500 0.0681(3) Uani 1 2 d S TU P . .
O1 O 0.58206(19) 0.42968(14) 0.6596(3) 0.0523(6) Uani 1 1 d . . . . .
O2 O 0.57851(19) 0.59258(14) 0.6539(3) 0.0533(6) Uani 1 1 d . . . . .
C1 C 0.7110(4) 0.3685(3) 0.5260(5) 0.0739(12) Uani 1 1 d . . . . .
H1A H 0.7914 0.3717 0.5452 0.111 Uiso 1 1 calc R U . . .
H1B H 0.6900 0.3622 0.4218 0.111 Uiso 1 1 calc R U . . .
H1C H 0.6847 0.3261 0.5780 0.111 Uiso 1 1 calc R U . . .
C2 C 0.6597(3) 0.4393(2) 0.5769(4) 0.0488(8) Uani 1 1 d . . . . .
C3 C 0.6964(4) 0.5116(3) 0.5323(5) 0.0480(11) Uani 1 1 d . . . . .
C4 C 0.6531(3) 0.5832(2) 0.5673(4) 0.0481(8) Uani 1 1 d . . . . .
C5 C 0.6920(3) 0.6533(2) 0.4999(5) 0.0668(11) Uani 1 1 d . . . . .
H5A H 0.6676 0.6964 0.5518 0.100 Uiso 1 1 calc R U . . .
H5B H 0.6610 0.6557 0.3981 0.100 Uiso 1 1 calc R U . . .
H5C H 0.7726 0.6531 0.5061 0.100 Uiso 1 1 calc R U . . .
C6 C 0.7860(5) 0.5111(3) 0.4411(6) 0.0545(12) Uani 1 1 d . . . . .
N1 N 0.8580(3) 0.5104(2) 0.3704(5) 0.0747(11) Uani 1 1 d . . . . .
C7 C 0.978(4) 0.7171(9) 0.255(6) 0.120(10) Uani 0.5 1 d . U P A -1
H7A H 0.9957 0.7070 0.3582 0.180 Uiso 0.5 1 calc R U P A -1
H7B H 0.8993 0.7274 0.2334 0.180 Uiso 0.5 1 calc R U P A -1
H7C H 1.0204 0.7602 0.2279 0.180 Uiso 0.5 1 calc R U P A -1
O5 O 1.0058(11) 0.6551(5) 0.1746(10) 0.133(3) Uani 0.5 1 d . U P A -1
H5 H 1.0393 0.6690 0.1056 0.200 Uiso 0.5 1 calc R U P A -1
B1 B 1.0000 0.3172(6) 0.2500 0.095(3) Uani 1 2 d S T P . .
F1 F 0.9536(5) 0.3634(3) 0.1454(6) 0.209(3) Uani 1 1 d . . . . .
F2 F 1.0710(9) 0.2753(6) 0.1978(12) 0.287(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 1.973(2) . ?
Pd1 O1 1.973(2) 2_656 ?
Pd1 O2 1.978(2) . ?
Pd1 O2 1.978(2) 2_656 ?
Ag1 N1 2.124(3) 2_755 ?
Ag1 N1 2.124(3) . ?
Ag1 O5 2.598(9) . ?
O1 C2 1.271(4) . ?
O2 C4 1.266(4) . ?
C1 C2 1.491(6) . ?
C2 C3 1.426(6) . ?
C3 C4 1.419(6) . ?
C3 C6 1.428(10) . ?
C4 C5 1.481(5) . ?
C6 N1 1.131(6) . ?
C7 O5 1.38(3) . ?
B1 F2 1.260(8) . ?
B1 F2 1.260(8) 2_755 ?
B1 F1 1.328(7) 2_755 ?
B1 F1 1.328(7) . ?

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
O1 Pd1 O1 86.35(14) . 2_656 ?
O1 Pd1 O2 93.67(10) . . ?
O1 Pd1 O2 178.16(9) 2_656 . ?
O1 Pd1 O2 178.16(9) . 2_656 ?
O1 Pd1 O2 93.68(10) 2_656 2_656 ?
O2 Pd1 O2 86.36(13) . 2_656 ?
N1 Ag1 N1 176.9(2) 2_755 . ?
N1 Ag1 O5 80.9(2) 2_755 . ?
N1 Ag1 O5 102.1(2) . . ?
C2 O1 Pd1 125.5(2) . . ?
C4 O2 Pd1 125.6(2) . . ?
O1 C2 C3 123.9(4) . . ?
O1 C2 C1 115.2(4) . . ?
C3 C2 C1 120.9(4) . . ?
C4 C3 C6 117.0(3) . . ?
C4 C3 C2 127.2(4) . . ?
C6 C3 C2 115.9(3) . . ?
O2 C4 C3 123.9(4) . . ?
O2 C4 C5 115.2(3) . . ?
C3 C4 C5 120.9(3) . . ?
N1 C6 C3 179.1(6) . . ?
C6 N1 Ag1 175.8(4) . . ?
C7 O5 Ag1 127.7(17) . . ?
F2 B1 F2 107.9(12) . 2_755 ?
F2 B1 F1 112.8(6) . 2_755 ?
F2 B1 F1 109.7(6) 2_755 2_755 ?
F2 B1 F1 109.7(6) . . ?
F2 B1 F1 112.8(6) 2_755 . ?
F1 B1 F1 104.2(8) 2_755 . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.128

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3beta
_database_code_depnum_ccdc_archive 'CCDC 1042066'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Ag N2 O4 Pd, Cl O4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag Cl N2 O9 Pd'
_chemical_formula_weight         594.00

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'
O O 0.0106 0.0060 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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'

_cell_length_a                   11.9150(17)
_cell_length_b                   17.722(3)
_cell_length_c                   9.1692(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.440(2)
_cell_angle_gamma                90
_cell_volume                     1924.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    4345
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      26.53

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.139
_shelx_estimated_absorpt_T_min   0.360
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4554
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10680
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.298
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1794
_reflns_number_gt                1618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1794
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.51231(2) 0.7500 0.0328(2) Uani 1 2 d S T P . .
Ag1 Ag 1.0000 0.51309(2) 0.2500 0.0544(2) Uani 1 2 d S T P . .
O1 O 0.58194(16) 0.43126(11) 0.6584(2) 0.0416(5) Uani 1 1 d . . . . .
O2 O 0.57706(14) 0.59382(10) 0.6532(2) 0.0414(5) Uani 1 1 d . . . . .
C1 C 0.7120(3) 0.37089(19) 0.5273(4) 0.0586(9) Uani 1 1 d . . . . .
H1A H 0.7923 0.3731 0.5529 0.088 Uiso 1 1 calc R U . . .
H1B H 0.6955 0.3663 0.4228 0.088 Uiso 1 1 calc R U . . .
H1C H 0.6820 0.3280 0.5740 0.088 Uiso 1 1 calc R U . . .
C2 C 0.6593(2) 0.44121(16) 0.5774(3) 0.0374(6) Uani 1 1 d . . . . .
C3 C 0.6949(4) 0.51297(18) 0.5295(5) 0.0372(9) Uani 1 1 d . . . . .
C4 C 0.6506(2) 0.58420(15) 0.5655(3) 0.0362(6) Uani 1 1 d . . . . .
C5 C 0.6879(3) 0.65476(17) 0.4960(4) 0.0520(8) Uani 1 1 d . . . . .
H5A H 0.6818 0.6966 0.5612 0.078 Uiso 1 1 calc R U . . .
H5B H 0.6408 0.6637 0.4056 0.078 Uiso 1 1 calc R U . . .
H5C H 0.7649 0.6494 0.4764 0.078 Uiso 1 1 calc R U . . .
C6 C 0.7829(4) 0.51333(19) 0.4386(5) 0.0432(10) Uani 1 1 d . . . . .
N1 N 0.8547(2) 0.51306(15) 0.3653(4) 0.0590(8) Uani 1 1 d . . . . .
C7 C 1.005(4) 0.7172(6) 0.269(6) 0.111(10) Uani 0.5 1 d . . P A -1
H7A H 1.0624 0.7121 0.3506 0.167 Uiso 0.5 1 calc R U P A -1
H7B H 0.9321 0.7203 0.3053 0.167 Uiso 0.5 1 calc R U P A -1
H7C H 1.0177 0.7622 0.2155 0.167 Uiso 0.5 1 calc R U P A -1
O5 O 1.0070(8) 0.6556(3) 0.1788(8) 0.108(2) Uani 0.5 1 d . . P A -1
H5 H 1.0071 0.6698 0.0937 0.162 Uiso 0.5 1 calc R U P A -1
Cl1 Cl 1.0000 0.32016(7) 0.2500 0.0724(4) Uani 1 2 d S T P . .
O3 O 0.9548(4) 0.3673(2) 0.1341(4) 0.1286(14) Uani 1 1 d . . . . .
O4 O 1.0828(6) 0.2762(5) 0.2007(7) 0.196(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.9748(18) . ?
Pd1 O2 1.9749(17) 2_656 ?
Pd1 O1 1.9763(18) . ?
Pd1 O1 1.9763(18) 2_656 ?
Ag1 N1 2.128(3) 2_755 ?
Ag1 N1 2.128(3) . ?
O1 C2 1.259(3) . ?
O2 C4 1.265(3) . ?
C1 C2 1.491(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.426(5) . ?
C3 C6 1.411(9) . ?
C3 C4 1.421(4) . ?
C4 C5 1.494(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N1 1.145(5) . ?
C7 O5 1.37(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
O5 H5 0.8200 . ?
Cl1 O4 1.372(5) . ?
Cl1 O4 1.372(5) 2_755 ?
Cl1 O3 1.411(4) . ?
Cl1 O3 1.411(4) 2_755 ?

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
O2 Pd1 O2 85.99(10) . 2_656 ?
O2 Pd1 O1 93.66(8) . . ?
O2 Pd1 O1 177.93(8) 2_656 . ?
O2 Pd1 O1 177.93(8) . 2_656 ?
O2 Pd1 O1 93.66(8) 2_656 2_656 ?
O1 Pd1 O1 86.76(11) . 2_656 ?
N1 Ag1 N1 179.97(15) 2_755 . ?
C2 O1 Pd1 125.31(18) . . ?
C4 O2 Pd1 125.24(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.7(3) . . ?
O1 C2 C1 115.2(3) . . ?
C3 C2 C1 120.0(3) . . ?
C6 C3 C4 117.0(3) . . ?
C6 C3 C2 116.9(3) . . ?
C4 C3 C2 126.1(4) . . ?
O2 C4 C3 124.7(3) . . ?
O2 C4 C5 114.7(2) . . ?
C3 C4 C5 120.6(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C3 179.4(4) . . ?
C6 N1 Ag1 173.9(3) . . ?
O5 C7 H7A 109.5 . . ?
O5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C7 O5 H5 109.5 . . ?
O4 Cl1 O4 110.8(8) . 2_755 ?
O4 Cl1 O3 108.4(3) . . ?
O4 Cl1 O3 110.9(4) 2_755 . ?
O4 Cl1 O3 110.9(4) . 2_755 ?
O4 Cl1 O3 108.4(3) 2_755 2_755 ?
O3 Cl1 O3 107.3(4) . 2_755 ?

_refine_diff_density_max         0.659
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.269

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4alpha
_database_code_depnum_ccdc_archive 'CCDC 1042067'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C12 H12 Ag N2 O4 Pd, 0.5B F4, 0.5Cl O4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag B0.50 Cl0.50 F2 N2 O7 Pd'
_chemical_formula_weight         587.68

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'
O O 0.0106 0.0060 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.6840(11)
_cell_length_b                   17.2956(16)
_cell_length_c                   9.1223(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.158(2)
_cell_angle_gamma                90
_cell_volume                     1824.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4075
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25.22

_exptl_crystal_description       rod
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    2.190
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5415
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19702
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.761
_diffrn_reflns_theta_max         25.264
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3294
_reflns_number_gt                2614
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+13.3733P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3294
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.25876(3) 0.26241(2) 0.79549(5) 0.01335(14) Uani 1 1 d . . . . .
O1 O 0.3366(3) 0.1762(2) 0.7076(4) 0.0164(8) Uani 1 1 d . . . . .
O2 O 0.3413(3) 0.3430(2) 0.6982(4) 0.0163(8) Uani 1 1 d . . . . .
C1 C 0.4654(5) 0.1094(3) 0.5788(7) 0.0212(13) Uani 1 1 d . . . . .
H1A H 0.5451 0.1046 0.6284 0.032 Uiso 1 1 calc R U . . .
H1B H 0.4649 0.1097 0.4713 0.032 Uiso 1 1 calc R U . . .
H1C H 0.4197 0.0655 0.6061 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4141(4) 0.1832(3) 0.6255(6) 0.0165(11) Uani 1 1 d . . . . .
C3 C 0.4540(5) 0.2555(3) 0.5753(6) 0.0163(11) Uani 1 1 d . . . . .
C4 C 0.4134(5) 0.3306(3) 0.6093(6) 0.0160(11) Uani 1 1 d . . . . .
C5 C 0.4532(5) 0.4014(3) 0.5374(7) 0.0206(12) Uani 1 1 d . . . . .
H5A H 0.3909 0.4204 0.4627 0.031 Uiso 1 1 calc R U . . .
H5B H 0.5210 0.3887 0.4899 0.031 Uiso 1 1 calc R U . . .
H5C H 0.4738 0.4414 0.6125 0.031 Uiso 1 1 calc R U . . .
C6 C 0.5424(5) 0.2513(3) 0.4830(7) 0.0178(12) Uani 1 1 d . . . . .
N1 N 0.6143(4) 0.2473(3) 0.4108(6) 0.0215(11) Uani 1 1 d . . . . .
O3 O 0.1712(3) 0.1820(2) 0.8857(4) 0.0160(8) Uani 1 1 d . . . . .
O4 O 0.1870(3) 0.3489(2) 0.8913(4) 0.0180(8) Uani 1 1 d . . . . .
C7 C 0.0321(5) 0.1251(3) 1.0129(7) 0.0200(12) Uani 1 1 d . . . . .
H7A H 0.0640 0.0786 0.9726 0.030 Uiso 1 1 calc R U . . .
H7B H -0.0506 0.1290 0.9753 0.030 Uiso 1 1 calc R U . . .
H7C H 0.0426 0.1220 1.1213 0.030 Uiso 1 1 calc R U . . .
C8 C 0.0934(5) 0.1951(3) 0.9664(6) 0.0158(11) Uani 1 1 d . . . . .
C9 C 0.0630(5) 0.2695(3) 1.0125(6) 0.0156(12) Uani 1 1 d . . . . .
C10 C 0.1132(4) 0.3414(3) 0.9797(6) 0.0156(11) Uani 1 1 d . . . . .
C11 C 0.0823(5) 0.4136(3) 1.0534(7) 0.0208(12) Uani 1 1 d . . . . .
H11A H 0.1135 0.4582 1.0061 0.031 Uiso 1 1 calc R U . . .
H11B H 0.1151 0.4121 1.1583 0.031 Uiso 1 1 calc R U . . .
H11C H -0.0020 0.4180 1.0443 0.031 Uiso 1 1 calc R U . . .
C12 C -0.0265(5) 0.2730(3) 1.1028(6) 0.0161(12) Uani 1 1 d . . . . .
N2 N -0.0987(4) 0.2753(3) 1.1760(6) 0.0222(11) Uani 1 1 d . . . . .
Ag1 Ag 0.75684(4) 0.26613(3) 0.29403(5) 0.02066(15) Uani 1 1 d . . . . .
O5 O 0.7265(4) 0.4123(3) 0.3181(5) 0.0301(10) Uani 1 1 d . . . . .
H5O H 0.7313 0.4302 0.4029 0.07(3) Uiso 1 1 d R . . . .
C13 C 0.7746(6) 0.4679(4) 0.2299(8) 0.0338(16) Uani 1 1 d . . . . .
H13A H 0.8586 0.4697 0.2585 0.051 Uiso 1 1 calc R U . . .
H13B H 0.7415 0.5189 0.2452 0.051 Uiso 1 1 calc R U . . .
H13C H 0.7568 0.4535 0.1253 0.051 Uiso 1 1 calc R U . . .
Cl1 Cl 0.7688(3) 0.0720(2) 0.2206(4) 0.0487(8) Uani 0.5 1 d . . P . .
B1 B 0.7688(3) 0.0720(2) 0.2206(4) 0.0487(8) Uani 0.5 1 d . . P . .
O6 O 0.7194(4) 0.1338(2) 0.1353(4) 0.0322(10) Uani 0.5 1 d . . P . .
F6 F 0.7194(4) 0.1338(2) 0.1353(4) 0.0322(10) Uani 0.5 1 d . . P . .
O7 O 0.6908(4) 0.0380(3) 0.2987(5) 0.0425(12) Uani 0.5 1 d . . P . .
F7 F 0.6908(4) 0.0380(3) 0.2987(5) 0.0425(12) Uani 0.5 1 d . . P . .
O8 O 0.8024(4) 0.0176(3) 0.1171(5) 0.0467(12) Uani 0.5 1 d . . P . .
F8 F 0.8024(4) 0.0176(3) 0.1171(5) 0.0467(12) Uani 0.5 1 d . . P . .
O9 O 0.8655(4) 0.0975(3) 0.3137(5) 0.0495(14) Uani 0.5 1 d . . P . .
F9 F 0.8655(4) 0.0975(3) 0.3137(5) 0.0495(14) Uani 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O3 1.973(4) . ?
Pd1 O1 1.975(4) . ?
Pd1 O2 1.976(4) . ?
Pd1 O4 1.978(4) . ?
O1 C2 1.261(6) . ?
O2 C4 1.268(6) . ?
C1 C2 1.498(8) . ?
C2 C3 1.432(8) . ?
C3 C6 1.424(8) . ?
C3 C4 1.431(8) . ?
C4 C5 1.493(8) . ?
C6 N1 1.141(8) . ?
N1 Ag1 2.125(5) . ?
O3 C8 1.268(6) . ?
O4 C10 1.268(6) . ?
C7 C8 1.498(8) . ?
C8 C9 1.415(8) . ?
C9 C12 1.422(8) . ?
C9 C10 1.425(8) . ?
C10 C11 1.486(8) . ?
C12 N2 1.149(7) . ?
N2 Ag1 2.133(5) 1_456 ?
Ag1 N2 2.133(5) 1_654 ?
Ag1 O5 2.566(5) . ?
O5 C13 1.420(8) . ?
Cl1 O7 1.366(5) . ?
Cl1 O9 1.385(5) . ?
Cl1 O6 1.398(5) . ?
Cl1 O8 1.427(5) . ?

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
O3 Pd1 O1 86.15(15) . . ?
O3 Pd1 O2 177.65(16) . . ?
O1 Pd1 O2 93.92(15) . . ?
O3 Pd1 O4 94.08(15) . . ?
O1 Pd1 O4 177.29(16) . . ?
O2 Pd1 O4 85.97(15) . . ?
C2 O1 Pd1 125.4(4) . . ?
C4 O2 Pd1 125.4(4) . . ?
O1 C2 C3 124.6(5) . . ?
O1 C2 C1 115.9(5) . . ?
C3 C2 C1 119.5(5) . . ?
C6 C3 C4 117.7(5) . . ?
C6 C3 C2 116.1(5) . . ?
C4 C3 C2 126.2(5) . . ?
O2 C4 C3 124.3(5) . . ?
O2 C4 C5 114.7(5) . . ?
C3 C4 C5 121.0(5) . . ?
N1 C6 C3 178.9(7) . . ?
C6 N1 Ag1 166.8(5) . . ?
C8 O3 Pd1 125.0(4) . . ?
C10 O4 Pd1 125.0(4) . . ?
O3 C8 C9 124.4(5) . . ?
O3 C8 C7 115.6(5) . . ?
C9 C8 C7 120.0(5) . . ?
C8 C9 C12 116.6(5) . . ?
C8 C9 C10 127.1(5) . . ?
C12 C9 C10 116.3(5) . . ?
O4 C10 C9 124.0(5) . . ?
O4 C10 C11 115.7(5) . . ?
C9 C10 C11 120.3(5) . . ?
N2 C12 C9 179.6(6) . . ?
C12 N2 Ag1 171.9(5) . 1_456 ?
N1 Ag1 N2 175.47(19) . 1_654 ?
N1 Ag1 O5 88.88(16) . . ?
N2 Ag1 O5 95.65(16) 1_654 . ?
C13 O5 Ag1 123.3(4) . . ?
O7 Cl1 O9 111.3(4) . . ?
O7 Cl1 O6 111.5(4) . . ?
O9 Cl1 O6 109.5(3) . . ?
O7 Cl1 O8 109.1(4) . . ?
O9 Cl1 O8 109.8(4) . . ?
O6 Cl1 O8 105.4(3) . . ?

_refine_diff_density_max         2.432
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.148

_shelxl_version_number           2013-4

