#------------------------------------------------------------------------------
#$Date: 2015-06-07 01:14:53 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138551 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/03/7220360.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_7220360
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         'C13 H16 Ag N2 O5 Pd, F6 P'
_chemical_formula_sum            'C13 H16 Ag F6 N2 O5 P Pd'
_chemical_formula_weight         639.52
_chemical_name_common            2c
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                116.299(6)
_cell_angle_beta                 96.468(6)
_cell_angle_gamma                91.599(6)
_cell_formula_units_Z            2
_cell_length_a                   9.358(4)
_cell_length_b                   10.882(5)
_cell_length_c                   10.968(4)
_cell_measurement_reflns_used    4160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.20
_cell_volume                     991.1(7)
_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_unetI/netI     0.0595
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3903
_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         25.994
_diffrn_reflns_theta_min         2.092
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       rod
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.544
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1168P)²+1.2889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3387
_reflns_number_total             3903
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00043b3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7220357--7220365.cif.'
_cod_original_cell_volume        991.2(7)
_cod_database_code               7220360
_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   0.587
_shelx_estimated_absorpt_t_max   0.821
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
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)
