#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/03/7220365.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_7220365
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, 0.5B F4, 0.5Cl O4, C H3 O H'
_chemical_formula_sum            'C13 H16 Ag B0.5 Cl0.5 F2 N2 O7 Pd'
_chemical_formula_weight         587.68
_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   mixed
_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                 98.158(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6840(11)
_cell_length_b                   17.2956(16)
_cell_length_c                   9.1223(9)
_cell_measurement_reflns_used    4075
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.36
_cell_volume                     1824.8(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 0.998
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19702
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.264
_diffrn_reflns_theta_min         1.761
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_description       rod
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.170
_refine_diff_density_max         2.432
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0412
_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)+(0.0397P)²+13.3733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2614
_reflns_number_total             3294
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00043b3.cif
_cod_data_source_block           4alpha
_cod_depositor_comments
'Adding full bibliography for 7220357--7220365.cif.'
_cod_original_formula_sum        'C13 H16 Ag B0.50 Cl0.50 F2 N2 O7 Pd'
_cod_database_code               7220365
#BEGIN Tags that were not found in dictionaries:
_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   0.569
_shelx_estimated_absorpt_t_max   0.707
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
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 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
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
