#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:48:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180449 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/18/7211808.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_7211808
loop_
_publ_author_name
'Qiu, Yongcai'
'Liu, Zhihui'
'Mou, Jixia'
'Deng, Hong'
'Zeller, Matthias'
_publ_section_title
;
 Rationally designed and controlled syntheses of different series of
 4d--4f heterometallic coordination frameworks based on lanthanide
 carboxylate and Ag(IN)2 substructures
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              277
_journal_paper_doi               10.1039/b915025k
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C38 H30 Ag4 Cl2 N6 O27 Tb2'
_chemical_formula_weight         1822.90
_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                90.699(2)
_cell_angle_beta                 103.392(2)
_cell_angle_gamma                110.548(2)
_cell_formula_units_Z            1
_cell_length_a                   8.3112(4)
_cell_length_b                   9.9605(4)
_cell_length_c                   16.4964(7)
_cell_measurement_reflns_used    4010
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.36
_cell_volume                     1237.41(10)
_computing_cell_refinement       'Apex2 v2.1-4'
_computing_data_collection       'Apex2 v2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Apex2 v2.1-4'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_structure_solution    'SHELXTL 6.14 (Bruker, 2000-2003)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10485
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.578
_exptl_absorpt_correction_T_max  0.6374
_exptl_absorpt_correction_T_min  0.3640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.1-4 (Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+19.3016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1889
_reflns_number_gt                4054
_reflns_number_total             4284
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b915025k.txt
_cod_data_source_block           2c
_cod_original_cell_volume        1237.41(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7211808
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
Tb1 Tb 0.60621(5) 0.29148(4) 0.48415(2) 0.02184(9) Uani 1 1 d .
Ag1 Ag 1.1147(2) -0.0200(2) 0.46423(11) 0.0624(5) Uani 0.50 1 d P
Ag2 Ag 0.5000 0.0000 0.0000 0.0531(3) Uani 1 2 d S
Ag3 Ag 0.83460(12) 0.33881(10) 0.00156(4) 0.0524(3) Uani 1 1 d .
C1 C 0.6242(10) 0.5416(8) 0.6372(5) 0.024(2) Uani 1 1 d .
C2 C 0.6780(11) 0.4965(9) 0.7236(5) 0.029(2) Uani 1 1 d .
C3 C 0.8002(10) 0.4286(9) 0.7398(5) 0.029(2) Uani 1 1 d .
H3 H 0.8509 0.4109 0.6981 0.035 Uiso 1 1 calc R
C4 C 0.8449(11) 0.3878(10) 0.8187(6) 0.036(2) Uani 1 1 d .
H4 H 0.9290 0.3443 0.8296 0.043 Uiso 1 1 calc R
C5 C 0.6550(13) 0.4730(12) 0.8638(6) 0.046(3) Uani 1 1 d .
H5 H 0.6047 0.4884 0.9062 0.055 Uiso 1 1 calc R
C6 C 0.6059(12) 0.5176(10) 0.7871(6) 0.041(2) Uani 1 1 d .
H6 H 0.5231 0.5624 0.7780 0.049 Uiso 1 1 calc R
C7 C 0.3941(9) -0.0399(9) 0.3750(5) 0.024(2) Uani 1 1 d .
C8 C 0.4167(10) -0.0306(8) 0.2870(5) 0.026(2) Uani 1 1 d .
C9 C 0.5111(11) -0.1008(9) 0.2578(5) 0.034(2) Uani 1 1 d .
H9 H 0.5623 -0.1555 0.2926 0.040 Uiso 1 1 calc R
C10 C 0.5297(12) -0.0904(10) 0.1774(6) 0.040(2) Uani 1 1 d .
H10 H 0.5973 -0.1364 0.1598 0.048 Uiso 1 1 calc R
C11 C 0.3598(14) 0.0495(12) 0.1519(6) 0.051(3) Uani 1 1 d .
H11 H 0.3036 0.0988 0.1151 0.062 Uiso 1 1 calc R
C12 C 0.3426(11) 0.0478(11) 0.2320(5) 0.039(2) Uani 1 1 d .
H12 H 0.2808 0.0994 0.2497 0.047 Uiso 1 1 calc R
C13 C 0.8521(12) 0.1672(10) 0.3774(6) 0.037(2) Uani 1 1 d .
C14 C 0.8599(10) 0.2146(9) 0.2898(5) 0.028(2) Uani 1 1 d .
C15 C 0.9429(12) 0.1608(11) 0.2419(6) 0.044(3) Uani 1 1 d .
H15 H 1.0036 0.1016 0.2640 0.052 Uiso 1 1 calc R
C16 C 0.9351(12) 0.1958(11) 0.1605(5) 0.040(3) Uani 1 1 d .
H16 H 0.9906 0.1582 0.1284 0.048 Uiso 1 1 calc R
C17 C 0.7693(13) 0.3319(11) 0.1733(6) 0.045(3) Uani 1 1 d .
H17 H 0.7094 0.3910 0.1501 0.054 Uiso 1 1 calc R
C18 C 0.7705(12) 0.2996(11) 0.2547(5) 0.039(2) Uani 1 1 d .
H18 H 0.7109 0.3356 0.2852 0.047 Uiso 1 1 calc R
C19 C 0.9689(11) 0.5378(9) 0.4621(5) 0.031(2) Uani 1 1 d .
Cl1 Cl 0.7891(3) 0.7482(3) 0.05318(17) 0.0555(7) Uani 1 1 d .
N1 N 0.7746(10) 0.4072(9) 0.8798(5) 0.040(2) Uani 1 1 d .
N2 N 0.4561(10) -0.0180(9) 0.1236(4) 0.040(2) Uani 1 1 d .
N3 N 0.8518(10) 0.2806(9) 0.1266(5) 0.039(2) Uani 1 1 d .
O1 O 0.6264(12) 0.7584(12) 0.0085(6) 0.103(3) Uani 1 1 d .
O2 O 0.9077(14) 0.7779(17) 0.0009(7) 0.135(5) Uani 1 1 d .
O3 O 0.7558(18) 0.6022(11) 0.0661(9) 0.127(5) Uani 1 1 d .
O4 O 0.8651(16) 0.8256(16) 0.1323(8) 0.138(5) Uani 1 1 d .
O5 O 0.5549(7) 0.6367(6) 0.6327(4) 0.0348(16) Uani 1 1 d .
O6 O 0.6525(9) 0.4894(6) 0.5770(4) 0.0448(19) Uani 1 1 d .
O7 O 0.3837(8) 0.0677(6) 0.4112(4) 0.0349(16) Uani 1 1 d .
O8 O 0.3918(8) -0.1534(6) 0.4053(4) 0.0355(17) Uani 1 1 d .
O9 O 0.8032(8) 0.4994(7) 0.4347(4) 0.0400(18) Uani 1 1 d .
O10 O 1.0813(7) 0.6347(6) 0.4390(3) 0.0303(16) Uani 1 1 d .
O11 O 0.7408(7) 0.1898(7) 0.4075(4) 0.0352(16) Uani 1 1 d .
O12 O 0.9597(10) 0.1148(10) 0.4124(5) 0.087(2) Uani 1 1 d .
O1W O 0.3222(7) 0.2530(8) 0.5191(4) 0.0431(18) Uani 1 1 d .
H1W H 0.3457 0.3421 0.5210 0.065 Uiso 1 1 d R
H2W H 0.2251 0.2178 0.4837 0.065 Uiso 1 1 d R
O2W O 0.904(3) -0.1952(17) 0.3454(13) 0.116(8) Uani 0.50 1 d PD
H3W H 0.9541 -0.1996 0.3088 0.174 Uiso 0.50 1 d PRD
H4W H 0.8029 -0.2586 0.3301 0.174 Uiso 0.50 1 d PRD
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'
Cl Cl 0.1484 0.1585 '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'
Tb Tb -0.1723 4.1537 '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
O8 Tb1 O11 98.9(2) 2_656 .
O8 Tb1 O6 89.2(2) 2_656 .
O11 Tb1 O6 144.2(2) . .
O8 Tb1 O5 149.3(2) 2_656 2_666
O11 Tb1 O5 94.7(2) . 2_666
O6 Tb1 O5 95.7(2) . 2_666
O8 Tb1 O7 82.0(2) 2_656 .
O11 Tb1 O7 72.8(2) . .
O6 Tb1 O7 143.1(2) . .
O5 Tb1 O7 76.0(2) 2_666 .
O8 Tb1 O9 140.0(2) 2_656 .
O11 Tb1 O9 77.1(2) . .
O6 Tb1 O9 74.5(2) . .
O5 Tb1 O9 70.0(2) 2_666 .
O7 Tb1 O9 131.9(2) . .
O8 Tb1 O10 74.6(2) 2_656 2_766
O11 Tb1 O10 73.0(2) . 2_766
O6 Tb1 O10 75.7(2) . 2_766
O5 Tb1 O10 136.0(2) 2_666 2_766
O7 Tb1 O10 134.4(2) . 2_766
O9 Tb1 O10 66.1(2) . 2_766
O8 Tb1 O1W 75.5(2) 2_656 .
O11 Tb1 O1W 142.8(2) . .
O6 Tb1 O1W 73.0(2) . .
O5 Tb1 O1W 77.0(2) 2_666 .
O7 Tb1 O1W 70.0(2) . .
O9 Tb1 O1W 130.4(2) . .
O10 Tb1 O1W 136.5(2) 2_766 .
O12 Ag1 O12 111.2(3) . 2_756
O12 Ag1 O7 105.0(3) . 1_655
O12 Ag1 O7 136.8(3) 2_756 1_655
O12 Ag1 O2W 82.5(5) . .
O12 Ag1 O2W 106.3(6) 2_756 .
O7 Ag1 O2W 101.0(6) 1_655 .
O12 Ag1 Ag1 58.4(2) . 2_756
O12 Ag1 Ag1 52.8(2) 2_756 2_756
O7 Ag1 Ag1 152.43(19) 1_655 2_756
O2W Ag1 Ag1 98.4(6) . 2_756
N2 Ag2 N2 180.0(7) 2_655 .
N1 Ag3 N3 168.8(4) 1_554 .
O6 C1 O5 123.6(8) . .
O6 C1 C2 120.1(8) . .
O5 C1 C2 116.3(8) . .
C6 C2 C3 117.9(8) . .
C6 C2 C1 121.9(8) . .
C3 C2 C1 120.2(8) . .
C4 C3 C2 118.7(9) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
N1 C4 C3 123.4(9) . .
N1 C4 H4 118.3 . .
C3 C4 H4 118.3 . .
N1 C5 C6 121.9(10) . .
N1 C5 H5 119.1 . .
C6 C5 H5 119.1 . .
C5 C6 C2 120.3(10) . .
C5 C6 H6 119.9 . .
C2 C6 H6 119.9 . .
O8 C7 O7 126.3(8) . .
O8 C7 C8 115.7(8) . .
O7 C7 C8 117.9(7) . .
C9 C8 C12 117.2(8) . .
C9 C8 C7 121.2(8) . .
C12 C8 C7 121.6(8) . .
C10 C9 C8 120.0(9) . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
N2 C10 C9 123.3(10) . .
N2 C10 H10 118.3 . .
C9 C10 H10 118.3 . .
C12 C11 N2 122.6(10) . .
C12 C11 H11 118.7 . .
N2 C11 H11 118.7 . .
C11 C12 C8 120.1(10) . .
C11 C12 H12 120.0 . .
C8 C12 H12 120.0 . .
O12 C13 O11 125.5(9) . .
O12 C13 C14 118.0(9) . .
O11 C13 C14 116.5(9) . .
C18 C14 C15 118.4(8) . .
C18 C14 C13 120.8(9) . .
C15 C14 C13 120.5(9) . .
C14 C15 C16 119.3(10) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
N3 C16 C15 122.6(10) . .
N3 C16 H16 118.7 . .
C15 C16 H16 118.7 . .
N3 C17 C18 122.2(10) . .
N3 C17 H17 118.9 . .
C18 C17 H17 118.9 . .
C14 C18 C17 119.5(10) . .
C14 C18 H18 120.3 . .
C17 C18 H18 120.3 . .
O10 C19 O9 126.4(8) . .
O10 C19 C19 118.1(9) . 2_766
O9 C19 C19 115.2(9) . 2_766
O4 Cl1 O3 106.1(9) . .
O4 Cl1 O2 113.1(7) . .
O3 Cl1 O2 103.7(10) . .
O4 Cl1 O1 116.1(8) . .
O3 Cl1 O1 107.6(7) . .
O2 Cl1 O1 109.2(7) . .
C4 N1 C5 117.8(8) . .
C4 N1 Ag3 124.3(7) . 1_556
C5 N1 Ag3 117.9(7) . 1_556
C10 N2 C11 116.7(8) . .
C10 N2 Ag2 121.0(7) . .
C11 N2 Ag2 122.2(7) . .
C16 N3 C17 118.0(8) . .
C16 N3 Ag3 124.5(7) . .
C17 N3 Ag3 117.5(7) . .
C1 O5 Tb1 130.3(5) . 2_666
C1 O6 Tb1 151.1(6) . .
C7 O7 Tb1 132.5(5) . .
C7 O7 Ag1 107.1(5) . 1_455
Tb1 O7 Ag1 114.6(3) . 1_455
C7 O8 Tb1 151.7(6) . 2_656
C19 O9 Tb1 120.2(5) . .
C19 O10 Tb1 119.6(5) . 2_766
C13 O11 Tb1 162.6(5) . .
C13 O12 Ag1 169.0(7) . .
C13 O12 Ag1 109.7(7) . 2_756
Ag1 O12 Ag1 68.8(3) . 2_756
Tb1 O1W H1W 89.0 . .
Tb1 O1W H2W 122.2 . .
H1W O1W H2W 104.3 . .
Ag1 O2W H3W 109.7 . .
Ag1 O2W H4W 143.7 . .
H3W O2W H4W 106.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O8 2.298(6) 2_656
Tb1 O11 2.301(7) .
Tb1 O6 2.345(6) .
Tb1 O5 2.352(6) 2_666
Tb1 O7 2.418(5) .
Tb1 O9 2.432(6) .
Tb1 O10 2.450(5) 2_766
Tb1 O1W 2.460(6) .
Ag1 O12 2.219(10) .
Ag1 O12 2.374(9) 2_756
Ag1 O7 2.466(6) 1_655
Ag1 O2W 2.478(18) .
Ag1 Ag1 2.598(4) 2_756
Ag2 N2 2.151(7) 2_655
Ag2 N2 2.151(7) .
Ag3 N1 2.134(8) 1_554
Ag3 N3 2.136(8) .
C1 O6 1.223(11) .
C1 O5 1.265(11) .
C1 C2 1.514(11) .
C2 C6 1.369(14) .
C2 C3 1.386(13) .
C3 C4 1.376(12) .
C3 H3 0.9300 .
C4 N1 1.320(13) .
C4 H4 0.9300 .
C5 N1 1.352(15) .
C5 C6 1.366(14) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O8 1.237(10) .
C7 O7 1.260(11) .
C7 C8 1.507(11) .
C8 C9 1.374(14) .
C8 C12 1.381(13) .
C9 C10 1.371(13) .
C9 H9 0.9300 .
C10 N2 1.325(13) .
C10 H10 0.9300 .
C11 C12 1.361(14) .
C11 N2 1.362(15) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 O12 1.226(13) .
C13 O11 1.229(12) .
C13 C14 1.534(12) .
C14 C18 1.363(14) .
C14 C15 1.373(14) .
C15 C16 1.385(13) .
C15 H15 0.9300 .
C16 N3 1.322(14) .
C16 H16 0.9300 .
C17 N3 1.343(15) .
C17 C18 1.384(14) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 O10 1.221(10) .
C19 O9 1.259(10) .
C19 C19 1.549(16) 2_766
Cl1 O4 1.396(12) .
Cl1 O3 1.410(11) .
Cl1 O2 1.413(12) .
Cl1 O1 1.420(10) .
N1 Ag3 2.134(8) 1_556
O5 Tb1 2.352(6) 2_666
O7 Ag1 2.466(6) 1_455
O8 Tb1 2.298(6) 2_656
O10 Tb1 2.450(5) 2_766
O12 Ag1 2.374(9) 2_756
O1W H1W 0.8381 .
O1W H2W 0.8326 .
O2W H3W 0.8200 .
O2W H4W 0.8304 .
