#------------------------------------------------------------------------------
#$Date: 2015-06-07 01:14:53 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138551 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/03/7220364.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7220364
loop_
_publ_author_name
'Guo, Qianqian'
'Merkens, Carina'
'Si, Runze'
'Englert, Ulli'
_publ_section_title
;
 Crosslinking of the Pd(acacCN)2building unit with Ag(i) salts: dynamic 1D
 polymers and an extended 3D network
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4383
_journal_paper_doi               10.1039/C5CE00043B
_journal_volume                  17
_journal_year                    2015
_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
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-01 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.440(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9150(17)
_cell_length_b                   17.722(3)
_cell_length_c                   9.1692(13)
_cell_measurement_reflns_used    4345
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.30
_cell_volume                     1923.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      320(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10680
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.298
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       rod
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.659
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1618
_reflns_number_total             1794
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00043b3.cif
_cod_data_source_block           3beta
_cod_depositor_comments
'Adding full bibliography for 7220357--7220365.cif.'
_cod_original_cell_volume        1924.0(5)
_cod_database_code               7220364
_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.
;
_shelx_estimated_absorpt_t_min   0.360
_shelx_estimated_absorpt_t_max   0.754
_shelxl_version_number           2013-4
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'
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 . . . . .
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'
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
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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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
