#------------------------------------------------------------------------------
#$Date: 2015-06-07 01:14:53 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138551 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/03/7220362.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_7220362
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 Ag2 N4 O10 Pd'
_chemical_formula_sum            'C12 H12 Ag2 N4 O10 Pd'
_chemical_formula_weight         694.40
_chemical_name_common            7
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.265(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.6283(8)
_cell_length_b                   25.815(4)
_cell_length_c                   7.8121(13)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.82
_cell_volume                     900.5(3)
_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      100(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  0.0323
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10789
_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         26.613
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_description       rod
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0180
_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)+(0.0215P)²+0.3205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1768
_reflns_number_total             1878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00043b3.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7220357--7220365.cif.'
_cod_original_cell_volume        900.4(3)
_cod_database_code               7220362
_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   0.719
_shelx_estimated_absorpt_t_max   0.883
_shelxl_version_number           2013-4
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'
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
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 . . .
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'
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 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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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
