#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:57:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179137 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/99/4309946.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_4309946
loop_
_publ_author_name
'Feng He'
'Ming-Liang Tong'
'Xiao-Ming Chen'
_publ_section_title
;
Synthesis, Structures, and Magnetic Properties of Heteronuclear
Cu(II)-Ln(III) (Ln = La, Gd, or Tb) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8285
_journal_page_last               8292
_journal_paper_doi               10.1021/ic0507159
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H16 Cu N5 O13 Tb'
_chemical_formula_weight         660.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.4380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6049(5)
_cell_length_b                   19.5974(13)
_cell_length_c                   13.6724(9)
_cell_measurement_temperature    298(2)
_cell_volume                     1973.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11877
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    4.713
_exptl_absorpt_correction_T_max  0.6929
_exptl_absorpt_correction_T_min  0.2909
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0349P)²+1.1526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                4033
_reflns_number_total             4573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0507159si20050507_083030_2.cif
_cod_data_source_block           compoud_1.Tb
_cod_database_code               4309946
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.45663(2) 0.770564(8) 0.653067(12) 0.02904(7) Uani 1 1 d . . .
Cu1 Cu 0.46244(6) 0.93810(2) 0.66735(3) 0.03189(11) Uani 1 1 d . . .
O1 O 0.3606(3) 0.87219(12) 0.56883(18) 0.0384(6) Uani 1 1 d . . .
O2 O 0.6137(3) 0.86484(12) 0.72805(18) 0.0370(6) Uani 1 1 d . . .
O3 O 0.7343(3) 0.72256(12) 0.77877(19) 0.0355(6) Uani 1 1 d . . .
O4 O 0.7834(4) 0.74992(14) 0.6360(2) 0.0403(6) Uani 1 1 d . . .
O5 O 0.9948(4) 0.70062(15) 0.7492(2) 0.0514(7) Uani 1 1 d . . .
O6 O 0.4495(5) 0.77515(15) 0.8575(2) 0.0569(8) Uani 1 1 d . . .
O7 O 0.2381(4) 0.81982(15) 0.74255(19) 0.0448(6) Uani 1 1 d . . .
O8 O 0.2210(4) 0.82203(16) 0.8982(2) 0.0606(9) Uani 1 1 d . . .
O9 O 0.5000(4) 0.64948(12) 0.6130(2) 0.0442(7) Uani 1 1 d . . .
O10 O 0.3691(4) 0.66242(15) 0.7334(2) 0.0481(7) Uani 1 1 d . . .
O11 O 0.4341(5) 0.56051(15) 0.6911(2) 0.0632(9) Uani 1 1 d . . .
O12 O 0.4690(5) 0.75613(17) 0.4787(2) 0.0432(7) Uani 1 1 d . . .
O13 O 0.1458(4) 0.74067(17) 0.5652(3) 0.0458(7) Uani 1 1 d . . .
N1 N 0.3251(4) 1.00421(14) 0.5686(2) 0.0320(6) Uani 1 1 d . . .
N2 N 0.5590(4) 0.98508(14) 0.7971(2) 0.0341(7) Uani 1 1 d . . .
N3 N 0.8423(4) 0.72399(13) 0.7215(2) 0.0330(7) Uani 1 1 d . . .
N4 N 0.3007(4) 0.80586(16) 0.8348(2) 0.0376(7) Uani 1 1 d . . .
N5 N 0.4348(4) 0.62231(16) 0.6804(3) 0.0402(8) Uani 1 1 d . . .
C1 C 0.2352(5) 0.97373(18) 0.4825(3) 0.0336(8) Uani 1 1 d . . .
C2 C 0.1295(5) 1.0115(2) 0.4028(3) 0.0427(9) Uani 1 1 d . . .
H2 H 0.0675 0.9898 0.3438 0.051 Uiso 1 1 calc R . .
C3 C 0.1176(6) 1.0810(2) 0.4122(3) 0.0475(10) Uani 1 1 d . . .
H3 H 0.0470 1.1069 0.3598 0.057 Uiso 1 1 calc R . .
C4 C 0.2114(5) 1.1119(2) 0.5000(3) 0.0472(10) Uani 1 1 d . . .
H4 H 0.2057 1.1589 0.5078 0.057 Uiso 1 1 calc R . .
C5 C 0.3128(5) 1.07249(18) 0.5756(3) 0.0407(9) Uani 1 1 d . . .
H5 H 0.3764 1.0938 0.6347 0.049 Uiso 1 1 calc R . .
C6 C 0.2565(5) 0.89778(18) 0.4776(3) 0.0362(8) Uani 1 1 d . . .
H6A H 0.1377 0.8764 0.4620 0.043 Uiso 1 1 calc R . .
H6B H 0.3144 0.8866 0.4239 0.043 Uiso 1 1 calc R . .
C7 C 0.6933(5) 0.94903(17) 0.8592(3) 0.0326(7) Uani 1 1 d . . .
C8 C 0.7782(6) 0.97192(19) 0.9536(3) 0.0431(9) Uani 1 1 d . . .
H8 H 0.8691 0.9460 0.9953 0.052 Uiso 1 1 calc R . .
C9 C 0.7287(6) 1.0332(2) 0.9864(3) 0.0513(11) Uani 1 1 d . . .
H9 H 0.7879 1.0500 1.0497 0.062 Uiso 1 1 calc R . .
C10 C 0.5904(6) 1.0698(2) 0.9248(3) 0.0517(11) Uani 1 1 d . . .
H10 H 0.5530 1.1111 0.9463 0.062 Uiso 1 1 calc R . .
C11 C 0.5090(6) 1.0446(2) 0.8315(3) 0.0440(10) Uani 1 1 d . . .
H11 H 0.4153 1.0694 0.7900 0.053 Uiso 1 1 calc R . .
C12 C 0.7391(5) 0.88188(18) 0.8187(3) 0.0392(9) Uani 1 1 d . . .
H12A H 0.8597 0.8844 0.8073 0.047 Uiso 1 1 calc R . .
H12B H 0.7397 0.8464 0.8683 0.047 Uiso 1 1 calc R . .
H12A H 0.402(6) 0.769(2) 0.432(4) 0.045(14) Uiso 1 1 d . . .
H12B H 0.542(7) 0.728(2) 0.472(4) 0.049(14) Uiso 1 1 d . . .
H13A H 0.091(6) 0.735(2) 0.505(4) 0.050(14) Uiso 1 1 d . . .
H13B H 0.065(8) 0.742(3) 0.593(4) 0.071(18) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
O2 Tb1 O1 66.20(8) . . ?
O2 Tb1 O12 112.89(10) . . ?
O1 Tb1 O12 72.39(10) . . ?
O2 Tb1 O13 138.10(10) . . ?
O1 Tb1 O13 79.39(10) . . ?
O12 Tb1 O13 76.04(12) . . ?
O2 Tb1 O9 141.83(9) . . ?
O1 Tb1 O9 138.95(9) . . ?
O12 Tb1 O9 68.35(10) . . ?
O13 Tb1 O9 80.05(10) . . ?
O2 Tb1 O7 78.78(9) . . ?
O1 Tb1 O7 75.27(9) . . ?
O12 Tb1 O7 136.23(10) . . ?
O13 Tb1 O7 69.62(10) . . ?
O9 Tb1 O7 128.46(10) . . ?
O2 Tb1 O3 75.21(8) . . ?
O1 Tb1 O3 139.09(8) . . ?
O12 Tb1 O3 113.03(10) . . ?
O13 Tb1 O3 141.40(10) . . ?
O9 Tb1 O3 70.21(8) . . ?
O7 Tb1 O3 110.74(8) . . ?
O2 Tb1 O10 129.67(9) . . ?
O1 Tb1 O10 147.29(9) . . ?
O12 Tb1 O10 113.87(10) . . ?
O13 Tb1 O10 71.80(10) . . ?
O9 Tb1 O10 50.38(9) . . ?
O7 Tb1 O10 80.37(9) . . ?
O3 Tb1 O10 70.37(8) . . ?
O2 Tb1 O4 76.21(9) . . ?
O1 Tb1 O4 106.24(9) . . ?
O12 Tb1 O4 67.63(10) . . ?
O13 Tb1 O4 138.85(10) . . ?
O9 Tb1 O4 69.27(9) . . ?
O7 Tb1 O4 151.53(8) . . ?
O3 Tb1 O4 49.39(8) . . ?
O10 Tb1 O4 105.59(9) . . ?
O2 Tb1 O6 70.57(9) . . ?
O1 Tb1 O6 112.56(9) . . ?
O12 Tb1 O6 175.01(10) . . ?
O13 Tb1 O6 103.91(11) . . ?
O9 Tb1 O6 106.69(9) . . ?
O7 Tb1 O6 47.03(9) . . ?
O3 Tb1 O6 63.84(9) . . ?
O10 Tb1 O6 61.73(9) . . ?
O4 Tb1 O6 110.61(9) . . ?
O2 Tb1 N5 141.04(8) . . ?
O1 Tb1 N5 152.73(8) . . ?
O12 Tb1 N5 91.54(11) . . ?
O13 Tb1 N5 75.33(10) . . ?
O9 Tb1 N5 25.24(10) . . ?
O7 Tb1 N5 104.77(10) . . ?
O3 Tb1 N5 67.22(8) . . ?
O10 Tb1 N5 25.17(9) . . ?
O4 Tb1 N5 86.71(9) . . ?
O6 Tb1 N5 83.66(9) . . ?
O2 Tb1 Cu1 34.21(6) . . ?
O1 Tb1 Cu1 34.13(6) . . ?
O12 Tb1 Cu1 99.88(8) . . ?
O13 Tb1 Cu1 105.42(8) . . ?
O9 Tb1 Cu1 165.80(7) . . ?
O7 Tb1 Cu1 65.46(7) . . ?
O3 Tb1 Cu1 109.39(5) . . ?
O10 Tb1 Cu1 143.61(7) . . ?
O4 Tb1 Cu1 99.36(6) . . ?
O6 Tb1 Cu1 84.97(6) . . ?
N5 Tb1 Cu1 168.42(8) . . ?
O1 Cu1 O2 83.71(10) . . ?
O1 Cu1 N2 163.04(12) . . ?
O2 Cu1 N2 84.87(11) . . ?
O1 Cu1 N1 84.72(11) . . ?
O2 Cu1 N1 163.10(12) . . ?
N2 Cu1 N1 108.92(12) . . ?
O1 Cu1 Tb1 43.73(7) . . ?
O2 Cu1 Tb1 42.94(7) . . ?
N2 Cu1 Tb1 121.08(8) . . ?
N1 Cu1 Tb1 128.19(8) . . ?
C6 O1 Cu1 115.7(2) . . ?
C6 O1 Tb1 142.2(2) . . ?
Cu1 O1 Tb1 102.14(10) . . ?
C12 O2 Cu1 114.3(2) . . ?
C12 O2 Tb1 138.5(2) . . ?
Cu1 O2 Tb1 102.85(10) . . ?
N3 O3 Tb1 97.5(2) . . ?
N3 O4 Tb1 96.2(2) . . ?
N4 O6 Tb1 90.5(2) . . ?
N4 O7 Tb1 106.0(2) . . ?
N5 O9 Tb1 98.3(2) . . ?
N5 O10 Tb1 95.0(2) . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Cu1 112.0(2) . . ?
C5 N1 Cu1 129.7(2) . . ?
C11 N2 C7 117.9(3) . . ?
C11 N2 Cu1 130.1(2) . . ?
C7 N2 Cu1 112.0(2) . . ?
O5 N3 O4 122.4(3) . . ?
O5 N3 O3 120.9(3) . . ?
O4 N3 O3 116.7(3) . . ?
O8 N4 O6 121.9(4) . . ?
O8 N4 O7 121.6(3) . . ?
O6 N4 O7 116.4(3) . . ?
O11 N5 O10 122.6(4) . . ?
O11 N5 O9 121.2(4) . . ?
O10 N5 O9 116.2(3) . . ?
O11 N5 Tb1 176.9(3) . . ?
O10 N5 Tb1 59.83(18) . . ?
O9 N5 Tb1 56.46(17) . . ?
N1 C1 C2 121.1(3) . . ?
N1 C1 C6 116.2(3) . . ?
C2 C1 C6 122.6(3) . . ?
C3 C2 C1 119.5(4) . . ?
C2 C3 C4 119.1(4) . . ?
C5 C4 C3 119.0(4) . . ?
N1 C5 C4 123.0(4) . . ?
O1 C6 C1 111.2(3) . . ?
N2 C7 C8 121.7(3) . . ?
N2 C7 C12 115.8(3) . . ?
C8 C7 C12 122.5(3) . . ?
C7 C8 C9 119.6(4) . . ?
C8 C9 C10 119.2(4) . . ?
C11 C10 C9 118.9(4) . . ?
N2 C11 C10 122.6(4) . . ?
O2 C12 C7 111.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.298(2) . ?
Tb1 O1 2.325(2) . ?
Tb1 O12 2.426(3) . ?
Tb1 O13 2.441(3) . ?
Tb1 O9 2.476(2) . ?
Tb1 O7 2.491(3) . ?
Tb1 O3 2.547(2) . ?
Tb1 O10 2.551(3) . ?
Tb1 O4 2.585(3) . ?
Tb1 O6 2.810(3) . ?
Tb1 N5 2.939(3) . ?
Tb1 Cu1 3.2887(5) . ?
Cu1 O1 1.887(2) . ?
Cu1 O2 1.896(2) . ?
Cu1 N2 1.971(3) . ?
Cu1 N1 1.972(3) . ?
O1 C6 1.393(4) . ?
O2 C12 1.403(4) . ?
O3 N3 1.268(4) . ?
O4 N3 1.251(4) . ?
O5 N3 1.216(4) . ?
O6 N4 1.250(4) . ?
O7 N4 1.262(4) . ?
O8 N4 1.217(4) . ?
O9 N5 1.267(4) . ?
O10 N5 1.255(4) . ?
O11 N5 1.220(4) . ?
N1 C1 1.345(4) . ?
N1 C5 1.347(5) . ?
N2 C11 1.346(5) . ?
N2 C7 1.353(4) . ?
C1 C2 1.394(5) . ?
C1 C6 1.500(5) . ?
C2 C3 1.374(6) . ?
C3 C4 1.375(6) . ?
C4 C5 1.365(5) . ?
C7 C8 1.367(5) . ?
C7 C12 1.502(5) . ?
C8 C9 1.368(5) . ?
C9 C10 1.374(6) . ?
C10 C11 1.364(5) . ?
