data_1100957
_chemical_formula_sum    'C20 H22 N5 Ni O13 Tb'
_chemical_formula_weight          758.06
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'
 'Ni'  'Ni'   0.3393   1.1124
 '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'
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
_cell_length_a                    8.607(3)
_cell_length_b                    21.240(4)
_cell_length_c                    13.742(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2512.1(11)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
_exptl_crystal_description        ?
_exptl_crystal_colour             Red
_exptl_crystal_size_max           55
_exptl_crystal_size_mid           30
_exptl_crystal_size_min           15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.004
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1496
_exptl_absorpt_coefficient_mu     3.620
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             2526
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0347
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        1
_diffrn_reflns_limit_k_min        -25
_diffrn_reflns_limit_k_max        1
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        1
_diffrn_reflns_theta_min          1.92
_diffrn_reflns_theta_max          24.99
_reflns_number_total              2526
_reflns_number_gt                 2280
_reflns_threshold_expression      >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.7501P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00167(14)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    -0.03(2)
_refine_ls_number_reflns          2526
_refine_ls_number_parameters      362
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0316
_refine_ls_R_factor_gt            0.0265
_refine_ls_wR_factor_ref          0.0698
_refine_ls_wR_factor_gt           0.0659
_refine_ls_goodness_of_fit_ref    1.059
_refine_ls_restrained_S_all       1.059
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
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
Tb Tb 0.49643(3) 0.151345(12) 0.249626(19) 0.02728(12) Uani 1 1 d . . .
Ni Ni 0.81595(9) 0.06452(4) 0.30981(5) 0.02873(19) Uani 1 1 d . . .
O10 O 0.4742(6) 0.2659(2) 0.2439(4) 0.0483(12) Uani 1 1 d . . .
N1 N 0.9495(6) 0.0128(3) 0.2433(4) 0.0346(12) Uani 1 1 d . . .
O1 O 0.7152(5) 0.0946(2) 0.1991(3) 0.0319(10) Uani 1 1 d . . .
O4 O 0.4356(5) 0.1794(2) 0.4304(3) 0.0347(10) Uani 1 1 d . . .
N4 N 0.6172(8) 0.2788(3) 0.2593(4) 0.0422(14) Uani 1 1 d . . .
O12 O 0.4301(6) 0.0398(2) 0.2924(4) 0.0487(14) Uani 1 1 d . . .
C7 C 0.9736(8) 0.0119(3) 0.1501(5) 0.0335(15) Uani 1 1 d . . .
H7A H 1.0422 -0.0180 0.1257 0.040 Uiso 1 1 calc R . .
O8 O 0.6678(9) 0.3327(3) 0.2542(4) 0.0705(17) Uani 1 1 d . . .
C6 C 0.9002(7) 0.0548(3) 0.0810(4) 0.0313(15) Uani 1 1 d . . .
N2 N 0.9223(6) 0.0403(3) 0.4197(4) 0.0310(12) Uani 1 1 d . . .
N5 N 0.3936(7) 0.0237(3) 0.2061(5) 0.0413(15) Uani 1 1 d . . .
O13 O 0.4000(6) 0.0665(3) 0.1413(3) 0.0450(12) Uani 1 1 d . . .
C11 C 0.7689(8) 0.0995(3) 0.5364(5) 0.0336(15) Uani 1 1 d . . .
O9 O 0.7013(7) 0.2325(2) 0.2781(4) 0.0550(14) Uani 1 1 d . . .
C15 C 0.5359(8) 0.1603(3) 0.5032(4) 0.0320(15) Uani 1 1 d . . .
C10 C 0.8939(7) 0.0584(3) 0.5082(4) 0.0347(15) Uani 1 1 d . . .
H10A H 0.9592 0.0436 0.5571 0.042 Uiso 1 1 calc R . .
O2 O 0.6685(6) 0.1129(2) 0.3738(3) 0.0340(10) Uani 1 1 d . . .
C16 C 0.6605(7) 0.1231(3) 0.4710(4) 0.0275(13) Uani 1 1 d . . .
C14 C 0.5224(9) 0.1753(3) 0.6015(4) 0.0404(17) Uani 1 1 d . . .
H14A H 0.4387 0.1991 0.6232 0.048 Uiso 1 1 calc R . .
C12 C 0.7556(10) 0.1165(4) 0.6366(5) 0.0455(19) Uani 1 1 d . . .
H12A H 0.8285 0.1021 0.6813 0.055 Uiso 1 1 calc R . .
C13 C 0.6340(9) 0.1545(3) 0.6672(4) 0.0466(19) Uani 1 1 d . . .
H13A H 0.6271 0.1662 0.7323 0.056 Uiso 1 1 calc R . .
O6 O 0.2181(5) 0.1398(2) 0.2830(3) 0.0448(12) Uani 1 1 d . . .
O3 O 0.5950(6) 0.1735(2) 0.0774(3) 0.0340(10) Uani 1 1 d . . .
N3 N 0.1650(7) 0.1712(3) 0.2109(5) 0.0425(14) Uani 1 1 d . . .
C19 C 0.2985(8) 0.2150(3) 0.4607(5) 0.0391(16) Uani 1 1 d . . .
H19A H 0.2569 0.2377 0.4052 0.047 Uiso 1 1 calc R . .
H19B H 0.3284 0.2457 0.5095 0.047 Uiso 1 1 calc R . .
C2 C 0.7151(7) 0.1358(3) 0.0418(4) 0.0297(14) Uani 1 1 d . . .
O11 O 0.3549(7) -0.0300(2) 0.1852(5) 0.0705(18) Uani 1 1 d . . .
C20 C 0.1757(10) 0.1731(4) 0.5014(6) 0.056(2) Uani 1 1 d . . .
H20A H 0.0876 0.1980 0.5205 0.084 Uiso 1 1 calc R . .
H20B H 0.2159 0.1512 0.5571 0.084 Uiso 1 1 calc R . .
H20C H 0.1445 0.1431 0.4529 0.084 Uiso 1 1 calc R . .
C3 C 0.7755(8) 0.1391(4) -0.0530(4) 0.0410(17) Uani 1 1 d . . .
H3A H 0.7361 0.1682 -0.0971 0.049 Uiso 1 1 calc R . .
C8 C 1.0254(8) -0.0342(3) 0.3075(5) 0.0429(16) Uani 1 1 d . . .
H8A H 1.1205 -0.0498 0.2782 0.051 Uiso 1 1 calc R . .
H8B H 0.9566 -0.0695 0.3197 0.051 Uiso 1 1 calc R . .
C5 C 0.9561(8) 0.0575(4) -0.0156(5) 0.0436(18) Uani 1 1 d . . .
H5A H 1.0361 0.0309 -0.0352 0.052 Uiso 1 1 calc R . .
C17 C 0.5263(8) 0.2210(3) 0.0124(5) 0.0363(15) Uani 1 1 d . . .
H17A H 0.6088 0.2423 -0.0225 0.044 Uiso 1 1 calc R . .
H17B H 0.4720 0.2521 0.0512 0.044 Uiso 1 1 calc R . .
C9 C 1.0594(9) 0.0004(3) 0.3998(5) 0.0449(18) Uani 1 1 d . . .
H9A H 1.0763 -0.0290 0.4528 0.054 Uiso 1 1 calc R . .
H9B H 1.1517 0.0262 0.3924 0.054 Uiso 1 1 calc R . .
C1 C 0.7762(8) 0.0934(3) 0.1091(4) 0.0297(14) Uani 1 1 d . . .
C4 C 0.8927(9) 0.0992(4) -0.0803(5) 0.0455(19) Uani 1 1 d . . .
H4A H 0.9298 0.1004 -0.1438 0.055 Uiso 1 1 calc R . .
O5 O 0.0265(6) 0.1795(3) 0.1996(6) 0.079(2) Uani 1 1 d . . .
O7 O 0.2651(6) 0.1937(3) 0.1535(4) 0.0567(15) Uani 1 1 d . . .
C18 C 0.4143(9) 0.1927(4) -0.0602(5) 0.051(2) Uani 1 1 d . . .
H18A H 0.3727 0.2254 -0.1007 0.076 Uiso 1 1 calc R . .
H18B H 0.3311 0.1723 -0.0260 0.076 Uiso 1 1 calc R . .
H18C H 0.4679 0.1625 -0.0998 0.076 Uiso 1 1 calc R . .
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Tb 0.02835(17) 0.03133(18) 0.02217(17) 0.00257(12) -0.00056(17) 0.00289(11)
Ni 0.0277(4) 0.0355(4) 0.0230(3) 0.0052(4) -0.0002(3) 0.0051(4)
O10 0.053(3) 0.043(3) 0.048(3) 0.003(2) -0.007(3) 0.008(2)
N1 0.032(3) 0.038(3) 0.034(3) 0.009(3) -0.001(3) 0.002(2)
O1 0.034(2) 0.039(2) 0.022(2) 0.0049(19) 0.001(2) 0.003(2)
O4 0.036(2) 0.043(3) 0.025(2) 0.000(2) 0.003(2) 0.009(2)
N4 0.062(4) 0.031(3) 0.033(3) 0.000(3) -0.005(3) -0.002(3)
O12 0.051(3) 0.046(3) 0.049(3) 0.011(3) 0.008(3) 0.003(3)
C7 0.029(3) 0.037(3) 0.034(3) 0.002(3) 0.006(3) 0.004(3)
O8 0.107(5) 0.042(3) 0.062(3) -0.005(3) -0.012(4) -0.024(3)
C6 0.028(3) 0.036(4) 0.030(3) 0.002(3) 0.007(3) 0.002(3)
N2 0.027(3) 0.035(3) 0.030(3) 0.011(2) -0.002(2) 0.002(2)
N5 0.037(3) 0.038(3) 0.049(4) -0.005(3) 0.014(3) 0.006(3)
O13 0.051(3) 0.050(3) 0.033(2) -0.001(3) 0.002(2) 0.001(3)
C11 0.039(4) 0.033(3) 0.028(3) 0.005(3) 0.001(3) -0.003(3)
O9 0.052(3) 0.050(3) 0.064(3) 0.002(3) -0.003(3) 0.003(3)
C15 0.040(4) 0.033(3) 0.024(3) -0.002(3) 0.001(3) -0.003(3)
C10 0.029(3) 0.048(4) 0.027(3) 0.013(3) -0.008(3) -0.003(3)
O2 0.037(3) 0.047(3) 0.0183(19) 0.0012(19) 0.002(2) 0.010(2)
C16 0.031(3) 0.029(3) 0.022(3) 0.004(2) 0.002(3) -0.005(3)
C14 0.052(5) 0.046(4) 0.023(3) -0.006(3) 0.006(3) 0.003(4)
C12 0.059(5) 0.054(4) 0.024(3) 0.003(3) -0.008(3) -0.007(4)
C13 0.065(5) 0.057(5) 0.018(3) -0.001(3) -0.001(3) -0.010(4)
O6 0.036(3) 0.060(3) 0.039(3) 0.007(2) -0.004(2) 0.005(3)
O3 0.045(3) 0.035(2) 0.021(2) 0.005(2) -0.001(2) 0.007(2)
N3 0.034(3) 0.044(3) 0.050(3) 0.001(3) -0.013(3) 0.001(3)
C19 0.036(4) 0.042(4) 0.039(3) -0.007(3) 0.001(3) 0.009(3)
C2 0.029(3) 0.036(3) 0.024(3) -0.002(3) -0.001(3) -0.003(3)
O11 0.073(4) 0.039(3) 0.099(5) -0.020(3) 0.035(4) -0.015(3)
C20 0.051(5) 0.062(5) 0.055(5) -0.005(4) 0.010(4) -0.002(5)
C3 0.043(4) 0.059(4) 0.021(3) 0.013(3) -0.002(3) -0.001(4)
C8 0.041(4) 0.043(4) 0.046(4) 0.018(3) 0.008(4) 0.012(3)
C5 0.037(4) 0.059(5) 0.036(3) -0.008(4) 0.006(3) 0.003(4)
C17 0.047(4) 0.033(3) 0.029(3) 0.010(3) -0.001(3) 0.005(3)
C9 0.037(4) 0.045(4) 0.052(4) 0.012(4) 0.004(3) 0.015(3)
C1 0.036(4) 0.034(3) 0.020(3) 0.001(3) 0.002(3) -0.012(3)
C4 0.041(4) 0.069(5) 0.027(3) 0.004(3) 0.011(3) 0.001(4)
O5 0.035(3) 0.090(5) 0.113(5) 0.019(5) -0.016(4) 0.005(3)
O7 0.044(3) 0.066(4) 0.060(3) 0.029(3) -0.007(3) -0.001(3)
C18 0.048(4) 0.071(5) 0.033(4) 0.000(4) -0.011(4) 0.010(4)