#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:44:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179672 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/25/4512599.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_4512599
loop_
_publ_author_name
'Zhang, Fengming'
'Zou, Xiaoyan'
'Yan, Pengfei'
'Sun, Jingwen'
'Hou, Guangfeng'
'Li, Guangming'
_publ_section_title
;
 Pyrazine-2,3-Carboxylate Based Ag+Homometallic and
 Ln3+--Ag+Heterometallic Coordination Frameworks: Synthesis, Structures,
 and Magnetic Properties
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1249
_journal_paper_doi               10.1021/cg501644z
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C12 H8 Ag N4 O10 Tb, 2(H2 O)'
_chemical_formula_sum            'C12 H12 Ag N4 O12 Tb'
_chemical_formula_weight         671.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.695(5)
_cell_angle_beta                 101.871(5)
_cell_angle_gamma                105.780(5)
_cell_formula_units_Z            2
_cell_length_a                   6.6739(4)
_cell_length_b                   10.0822(6)
_cell_length_c                   14.9383(8)
_cell_measurement_reflns_used    3554
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6702
_cell_measurement_theta_min      3.1484
_cell_volume                     919.34(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6161
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    4.954
_exptl_absorpt_correction_T_max  0.5236
_exptl_absorpt_correction_T_min  0.3827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.243
_refine_diff_density_min         -2.346
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3614
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0829P)²+0.7443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                3414
_reflns_number_total             3614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501644z_si_002.cif
_cod_data_source_block           Tb-Ag
_cod_depositor_comments
'Adding full bibliography for 4512597--4512602.cif.'
_cod_original_cell_volume        919.34(9)
_cod_database_code               4512599
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ag1 Ag 0.41385(10) 0.17716(6) 0.19920(4) 0.03278(18) Uani 1 1 d .
C1 C -0.2701(15) -0.1403(9) 0.1151(6) 0.040(2) Uani 1 1 d .
H1 H -0.2824 -0.2058 0.1523 0.048 Uiso 1 1 calc R
C2 C -0.3346(13) -0.1875(8) 0.0202(6) 0.0347(17) Uani 1 1 d .
H2 H -0.3950 -0.2847 -0.0058 0.042 Uiso 1 1 calc R
C3 C -0.2311(10) 0.0403(7) 0.0019(4) 0.0218(13) Uani 1 1 d D
C4 C -0.1688(11) 0.0870(8) 0.0999(5) 0.0241(14) Uani 1 1 d .
C5 C -0.0742(10) 0.2413(7) 0.1517(4) 0.0221(14) Uani 1 1 d .
C6 C -0.2066(11) 0.1386(7) -0.0628(5) 0.0256(15) Uani 1 1 d D
C7 C 0.5949(12) 0.1804(8) 0.4091(5) 0.0291(16) Uani 1 1 d .
H7 H 0.5466 0.0837 0.3816 0.035 Uiso 1 1 calc R
C8 C 0.6862(11) 0.2258(7) 0.5060(5) 0.0251(14) Uani 1 1 d .
H8 H 0.7005 0.1600 0.5416 0.030 Uiso 1 1 calc R
C9 C 0.7368(9) 0.4556(7) 0.4939(4) 0.0162(12) Uani 1 1 d .
C10 C 0.6501(9) 0.4097(7) 0.3961(4) 0.0163(12) Uani 1 1 d .
C11 C 0.6415(10) 0.5093(7) 0.3313(4) 0.0198(13) Uani 1 1 d .
C12 C 0.8144(9) 0.6110(7) 0.5438(4) 0.0191(13) Uani 1 1 d .
Tb1 Tb 0.10784(4) 0.51512(3) 0.271217(18) 0.01688(14) Uani 1 1 d .
N1 N -0.1887(11) -0.0008(7) 0.1567(5) 0.0362(15) Uani 1 1 d .
N2 N -0.3150(9) -0.1004(6) -0.0373(4) 0.0266(13) Uani 1 1 d .
N3 N 0.5739(9) 0.2694(6) 0.3545(4) 0.0216(12) Uani 1 1 d .
N4 N 0.7535(9) 0.3647(6) 0.5478(4) 0.0203(11) Uani 1 1 d .
O1 O 0.1259(8) 0.2998(5) 0.1737(3) 0.0296(11) Uani 1 1 d .
O2 O -0.1981(7) 0.3040(5) 0.1780(3) 0.0274(11) Uani 1 1 d .
O3 O -0.1396(10) 0.2708(5) -0.0239(4) 0.0379(13) Uani 1 1 d .
O4 O -0.2514(10) 0.0853(6) -0.1482(4) 0.0399(13) Uani 1 1 d .
O5 O 0.4678(7) 0.5321(5) 0.3035(3) 0.0243(10) Uani 1 1 d .
O6 O 0.8083(7) 0.5589(5) 0.3063(3) 0.0229(10) Uani 1 1 d .
O7 O 0.7808(9) 0.6979(5) 0.4997(3) 0.0303(11) Uani 1 1 d .
O8 O 0.9092(8) 0.6391(5) 0.6303(3) 0.0265(10) Uani 1 1 d .
O9 O -0.0051(11) 0.5434(7) 0.1174(4) 0.0586(18) Uani 1 1 d U
H91 H 0.0243 0.6100 0.0890 0.088 Uiso 1 1 d R
H92 H -0.0885 0.4672 0.0784 0.088 Uiso 1 1 d R
O10 O 0.2782(8) 0.7548(5) 0.2768(3) 0.0305(11) Uani 1 1 d .
H101 H 0.4142 0.7737 0.2957 0.046 Uiso 1 1 d R
H102 H 0.2546 0.8216 0.2524 0.046 Uiso 1 1 d R
O11 O 0.0596(11) 0.0337(7) 0.3544(5) 0.0566(18) Uani 1 1 d .
H111 H 0.0957 0.1043 0.4012 0.085 Uiso 1 1 d R
H112 H -0.0108 0.0505 0.3058 0.085 Uiso 1 1 d R
O12 O 0.6831(9) 0.8735(7) 0.3844(5) 0.0546(18) Uani 1 1 d .
H121 H 0.7947 0.9351 0.3799 0.082 Uiso 1 1 d R
H122 H 0.7154 0.8382 0.4311 0.082 Uiso 1 1 d R
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'
Tb Tb -0.1723 4.1537 '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'
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
N3 Ag1 N2 169.2(2) . 2
N3 Ag1 O4 116.5(2) . 2
N2 Ag1 O4 68.7(2) 2 2
N3 Ag1 O1 100.81(17) . .
N2 Ag1 O1 85.16(18) 2 .
O4 Ag1 O1 111.37(18) 2 .
N1 C1 C2 121.5(7) . .
N1 C1 H1 119.3 . .
C2 C1 H1 119.3 . .
N2 C2 C1 122.5(7) . .
N2 C2 H2 118.8 . .
C1 C2 H2 118.8 . .
N2 C3 C4 119.0(6) . .
N2 C3 C6 117.8(6) . .
C4 C3 C6 123.3(6) . .
N1 C4 C3 122.9(6) . .
N1 C4 C5 113.3(6) . .
C3 C4 C5 123.8(6) . .
O1 C5 O2 121.8(6) . .
O1 C5 C4 119.5(6) . .
O2 C5 C4 118.5(6) . .
O1 C5 Tb1 60.4(3) . .
O2 C5 Tb1 61.4(3) . .
C4 C5 Tb1 172.1(5) . .
O4 C6 O3 126.0(6) . .
O4 C6 C3 117.8(6) . .
O3 C6 C3 116.2(6) . .
N3 C7 C8 122.8(6) . .
N3 C7 H7 118.6 . .
C8 C7 H7 118.6 . .
N4 C8 C7 119.8(6) . .
N4 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
N4 C9 C10 121.8(6) . .
N4 C9 C12 116.5(5) . .
C10 C9 C12 121.7(6) . .
N3 C10 C9 120.0(6) . .
N3 C10 C11 116.4(5) . .
C9 C10 C11 123.6(6) . .
O5 C11 O6 124.4(6) . .
O5 C11 C10 118.3(6) . .
O6 C11 C10 117.3(5) . .
O7 C12 O8 125.4(6) . .
O7 C12 C9 119.4(6) . .
O8 C12 C9 115.3(6) . .
O6 Tb1 O5 154.39(17) 1_455 .
O6 Tb1 O8 88.65(17) 1_455 2_666
O5 Tb1 O8 83.95(17) . 2_666
O6 Tb1 O10 93.11(17) 1_455 .
O5 Tb1 O10 77.22(17) . .
O8 Tb1 O10 139.41(16) 2_666 .
O6 Tb1 O9 90.5(2) 1_455 .
O5 Tb1 O9 109.0(2) . .
O8 Tb1 O9 146.59(19) 2_666 .
O10 Tb1 O9 73.99(19) . .
O6 Tb1 O1 127.96(16) 1_455 .
O5 Tb1 O1 74.01(16) . .
O8 Tb1 O1 76.82(17) 2_666 .
O10 Tb1 O1 129.64(18) . .
O9 Tb1 O1 77.6(2) . .
O6 Tb1 O2 75.34(15) 1_455 .
O5 Tb1 O2 126.06(15) . .
O8 Tb1 O2 76.71(16) 2_666 .
O10 Tb1 O2 142.66(17) . .
O9 Tb1 O2 70.78(19) . .
O1 Tb1 O2 52.79(15) . .
O6 Tb1 N4 77.07(16) 1_455 2_666
O5 Tb1 N4 77.61(16) . 2_666
O8 Tb1 N4 64.55(16) 2_666 2_666
O10 Tb1 N4 76.37(17) . 2_666
O9 Tb1 N4 147.1(2) . 2_666
O1 Tb1 N4 133.84(17) . 2_666
O2 Tb1 N4 132.37(16) . 2_666
O6 Tb1 C5 101.64(18) 1_455 .
O5 Tb1 C5 99.90(18) . .
O8 Tb1 C5 74.37(18) 2_666 .
O10 Tb1 C5 143.89(19) . .
O9 Tb1 C5 73.1(2) . .
O1 Tb1 C5 26.37(17) . .
O2 Tb1 C5 26.45(17) . .
N4 Tb1 C5 138.90(19) 2_666 .
C4 N1 C1 116.5(7) . .
C2 N2 C3 117.7(6) . .
C2 N2 Ag1 123.5(5) . 2
C3 N2 Ag1 118.8(5) . 2
C7 N3 C10 117.4(6) . .
C7 N3 Ag1 118.1(4) . .
C10 N3 Ag1 124.5(4) . .
C9 N4 C8 118.2(6) . .
C9 N4 Tb1 113.7(4) . 2_666
C8 N4 Tb1 127.9(4) . 2_666
C5 O1 Tb1 93.2(4) . .
C5 O1 Ag1 126.5(4) . .
Tb1 O1 Ag1 129.04(19) . .
C5 O2 Tb1 92.1(4) . .
C6 O4 Ag1 116.6(5) . 2
C11 O5 Tb1 162.2(5) . .
C11 O6 Tb1 144.9(4) . 1_655
C12 O8 Tb1 127.4(4) . 2_666
Tb1 O9 H91 136.1 . .
Tb1 O9 H92 113.6 . .
H91 O9 H92 110.1 . .
Tb1 O10 H101 109.3 . .
Tb1 O10 H102 140.1 . .
H101 O10 H102 107.5 . .
H111 O11 H112 110.2 . .
H121 O12 H122 110.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N3 2.259(5) .
Ag1 N2 2.306(6) 2
Ag1 O4 2.485(6) 2
Ag1 O1 2.553(5) .
C1 N1 1.345(10) .
C1 C2 1.353(11) .
C1 H1 0.9300 .
C2 N2 1.328(10) .
C2 H2 0.9300 .
C3 N2 1.350(8) .
C3 C4 1.396(9) .
C3 C6 1.498(7) .
C4 N1 1.325(10) .
C4 C5 1.509(9) .
C5 O1 1.251(8) .
C5 O2 1.253(8) .
C5 Tb1 2.812(6) .
C6 O4 1.238(9) .
C6 O3 1.273(9) .
C7 N3 1.326(10) .
C7 C8 1.392(10) .
C7 H7 0.9300 .
C8 N4 1.343(9) .
C8 H8 0.9300 .
C9 N4 1.329(9) .
C9 C10 1.401(8) .
C9 C12 1.511(9) .
C10 N3 1.352(8) .
C10 C11 1.511(9) .
C11 O5 1.244(7) .
C11 O6 1.249(8) .
C12 O7 1.222(9) .
C12 O8 1.263(8) .
Tb1 O6 2.302(4) 1_455
Tb1 O5 2.303(4) .
Tb1 O8 2.310(5) 2_666
Tb1 O10 2.353(5) .
Tb1 O9 2.356(6) .
Tb1 O1 2.449(4) .
Tb1 O2 2.472(5) .
Tb1 N4 2.625(5) 2_666
N2 Ag1 2.306(6) 2
N4 Tb1 2.625(5) 2_666
O4 Ag1 2.485(5) 2
O6 Tb1 2.302(4) 1_655
O8 Tb1 2.310(5) 2_666
O9 H91 0.8536 .
O9 H92 0.8502 .
O10 H101 0.8503 .
O10 H102 0.8531 .
O11 H111 0.8502 .
O11 H112 0.8499 .
O12 H121 0.8528 .
O12 H122 0.8513 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H91 O3 0.85 1.78 2.617(8) 164.7 2_565
O9 H92 O3 0.85 2.18 2.956(8) 150.9 .
O10 H101 O12 0.85 1.89 2.669(7) 151.4 .
O10 H102 O4 0.85 1.95 2.717(8) 149.3 2_565
O11 H111 O7 0.85 2.11 2.950(8) 168.4 2_666
O11 H112 N1 0.85 2.20 2.986(9) 154.5 .
O12 H121 O11 0.85 1.93 2.761(9) 165.9 1_665
O12 H122 O7 0.85 1.97 2.779(7) 158.3 .
