#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:55:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179943 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/38/7023855.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_7023855
loop_
_publ_author_name
'Liu, Baolin'
'Liu, Qingxia'
'Xiao, Hongping'
'Zhang, Wu'
'Tao, Ruojie'
_publ_section_title
;
 Family of dumbbell Ni4Ln2 (Ln = Pr, Sm, Eu, Gd, Tb, Ho, Er) complexes:
 syntheses, structures, luminescent and magnetic properties.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5047
_journal_page_last               5055
_journal_paper_doi               10.1039/c3dt32935f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C60 H58 N8 Ni4 O24 Tb2, 8(H2 O)'
_chemical_formula_sum            'C60 H74 N8 Ni4 O32 Tb2'
_chemical_formula_weight         1971.95
_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                 96.424(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6435(13)
_cell_length_b                   18.3018(19)
_cell_length_c                   15.4157(16)
_cell_measurement_reflns_used    5068
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.47
_cell_volume                     3544.8(6)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2(Bruker, 2009)'
_computing_data_reduction        'SAINT(Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL(Bruker, 2009)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'φ and 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18031
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.104
_exptl_absorpt_correction_T_max  0.7071
_exptl_absorpt_correction_T_min  0.4561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6232
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0378
_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)+(0.0588P)²+2.3046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                4985
_reflns_number_total             6232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32935f.txt
_cod_data_source_block           1813
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7023855
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 0.57899(2) 1.051608(15) 0.099155(18) 0.02477(11) Uani 1 1 d . . .
N1 N 0.7851(4) 0.8264(3) 0.2562(4) 0.0407(13) Uani 1 1 d . . .
N2 N 0.6370(4) 0.8147(3) 0.1028(4) 0.0443(14) Uani 1 1 d . . .
H2A H 0.5895 0.7794 0.1109 0.053 Uiso 1 1 calc R . .
H2B H 0.6168 0.8372 0.0517 0.053 Uiso 1 1 calc R . .
N3 N 0.5797(4) 0.8368(3) 0.2949(4) 0.0440(14) Uani 1 1 d . . .
N4 N 0.8175(5) 0.9782(3) 0.3182(4) 0.0438(14) Uani 1 1 d . . .
Ni2 Ni 0.80369(6) 1.04185(4) 0.20976(5) 0.02955(19) Uani 1 1 d . . .
Ni3 Ni 0.64703(6) 0.88780(4) 0.20319(5) 0.0307(2) Uani 1 1 d . . .
O1 O 0.5142(3) 0.9499(2) 0.1749(3) 0.0305(9) Uani 1 1 d . . .
O2 O 0.4088(3) 1.0166(2) 0.0325(2) 0.0283(9) Uani 1 1 d . . .
O3 O 0.2449(3) 1.0542(2) 0.0462(3) 0.0386(11) Uani 1 1 d . . .
O4 O 0.6594(3) 1.0721(2) 0.2391(3) 0.0353(10) Uani 1 1 d . . .
O5 O 0.4691(3) 1.1240(3) 0.1708(3) 0.0458(12) Uani 1 1 d . . .
O6 O 0.3884(5) 1.1883(5) 0.2613(5) 0.108(2) Uani 1 1 d U . .
O7 O 0.9425(3) 1.0231(2) 0.1569(3) 0.0394(11) Uani 1 1 d . . .
O8 O 0.7530(3) 1.1029(2) 0.1027(3) 0.0298(9) Uani 1 1 d . . .
O9 O 0.5739(3) 1.1528(2) 0.0082(3) 0.0410(11) Uani 1 1 d . . .
O10 O 0.6024(4) 1.2447(3) -0.0783(3) 0.0554(14) Uani 1 1 d . . .
O11 O 0.7174(3) 0.9635(2) 0.1379(2) 0.0277(9) Uani 1 1 d . . .
H11 H 0.7515 0.9447 0.0884 0.033 Uiso 1 1 calc R . .
O1W O 0.8856(4) 1.1234(3) 0.2848(3) 0.0509(12) Uani 1 1 d . . .
H1WA H 0.9419 1.1421 0.2689 0.061 Uiso 1 1 d R . .
H1WB H 0.8947 1.1252 0.3402 0.061 Uiso 1 1 d R . .
C1 C 0.7876(6) 0.7635(4) 0.1962(5) 0.0500(18) Uani 1 1 d . . .
H1A H 0.7453 0.7240 0.2162 0.060 Uiso 1 1 calc R . .
H1B H 0.8603 0.7463 0.1972 0.060 Uiso 1 1 calc R . .
C2 C 0.7449(5) 0.7834(4) 0.1033(5) 0.0498(18) Uani 1 1 d . . .
H2C H 0.7916 0.8188 0.0802 0.060 Uiso 1 1 calc R . .
H2D H 0.7422 0.7402 0.0666 0.060 Uiso 1 1 calc R . .
C3 C 0.7617(6) 0.7994(4) 0.3436(5) 0.056(2) Uani 1 1 d . . .
H3A H 0.7798 0.8370 0.3871 0.067 Uiso 1 1 calc R . .
H3B H 0.8049 0.7567 0.3597 0.067 Uiso 1 1 calc R . .
C4 C 0.6455(6) 0.7800(5) 0.3419(5) 0.059(2) Uani 1 1 d . . .
H4A H 0.6320 0.7332 0.3131 0.071 Uiso 1 1 calc R . .
H4B H 0.6271 0.7758 0.4011 0.071 Uiso 1 1 calc R . .
C5 C 0.4823(6) 0.8433(4) 0.3103(5) 0.0521(19) Uani 1 1 d . . .
H5 H 0.4611 0.8135 0.3541 0.062 Uiso 1 1 calc R . .
C6 C 0.4030(5) 0.8906(4) 0.2687(4) 0.0422(16) Uani 1 1 d . . .
C7 C 0.3036(6) 0.8862(5) 0.2993(5) 0.061(2) Uani 1 1 d . . .
H7 H 0.2944 0.8540 0.3445 0.073 Uiso 1 1 calc R . .
C8 C 0.2183(6) 0.9283(5) 0.2647(5) 0.062(2) Uani 1 1 d . . .
H8 H 0.1538 0.9268 0.2884 0.074 Uiso 1 1 calc R . .
C9 C 0.2312(5) 0.9726(4) 0.1940(5) 0.0465(18) Uani 1 1 d . . .
H9 H 0.1735 0.9997 0.1688 0.056 Uiso 1 1 calc R . .
C10 C 0.3281(4) 0.9780(3) 0.1595(4) 0.0291(13) Uani 1 1 d . . .
C11 C 0.3250(4) 1.0201(3) 0.0751(4) 0.0296(13) Uani 1 1 d . . .
C12 C 0.4177(5) 0.9396(3) 0.1997(4) 0.0288(13) Uani 1 1 d . . .
C13 C 0.8903(5) 0.8654(4) 0.2624(5) 0.0433(16) Uani 1 1 d . . .
H13A H 0.9465 0.8296 0.2753 0.052 Uiso 1 1 calc R . .
H13B H 0.8987 0.8863 0.2058 0.052 Uiso 1 1 calc R . .
C14 C 0.9052(6) 0.9248(4) 0.3295(5) 0.0528(19) Uani 1 1 d . . .
H14A H 0.9087 0.9035 0.3874 0.063 Uiso 1 1 calc R . .
H14B H 0.9721 0.9497 0.3248 0.063 Uiso 1 1 calc R . .
C15 C 0.7647(7) 0.9911(5) 0.3839(5) 0.062(2) Uani 1 1 d . . .
H15 H 0.7878 0.9665 0.4354 0.074 Uiso 1 1 calc R . .
C16 C 0.6742(9) 1.0391(5) 0.3871(5) 0.072(3) Uani 1 1 d U . .
C17 C 0.6300(10) 1.0452(6) 0.4676(7) 0.101(3) Uani 1 1 d U . .
H17 H 0.6642 1.0218 0.5165 0.121 Uiso 1 1 calc R . .
C18 C 0.5403(10) 1.0836(6) 0.4763(7) 0.104(3) Uani 1 1 d U . .
H18 H 0.5155 1.0878 0.5306 0.125 Uiso 1 1 calc R . .
C19 C 0.4866(9) 1.1160(6) 0.4051(6) 0.092(3) Uani 1 1 d U . .
H19 H 0.4248 1.1422 0.4109 0.110 Uiso 1 1 calc R . .
C20 C 0.5242(6) 1.1101(4) 0.3222(5) 0.0498(19) Uani 1 1 d . . .
C21 C 0.4577(5) 1.1431(4) 0.2466(5) 0.053(2) Uani 1 1 d . . .
C22 C 0.6189(6) 1.0738(4) 0.3138(4) 0.0400(16) Uani 1 1 d . . .
C23 C 0.9707(5) 1.0571(4) 0.0934(5) 0.0394(16) Uani 1 1 d . . .
H23 H 1.0402 1.0480 0.0819 0.047 Uiso 1 1 calc R . .
C24 C 0.9135(5) 1.1079(3) 0.0351(4) 0.0359(15) Uani 1 1 d . . .
C25 C 0.9680(5) 1.1374(4) -0.0309(5) 0.0518(19) Uani 1 1 d . . .
H25 H 1.0391 1.1254 -0.0331 0.062 Uiso 1 1 calc R . .
C26 C 0.9179(6) 1.1838(5) -0.0922(5) 0.059(2) Uani 1 1 d . . .
H26 H 0.9554 1.2045 -0.1346 0.071 Uiso 1 1 calc R . .
C27 C 0.8115(5) 1.1994(4) -0.0906(4) 0.0448(17) Uani 1 1 d . . .
H27 H 0.7784 1.2301 -0.1334 0.054 Uiso 1 1 calc R . .
C28 C 0.7510(5) 1.1716(3) -0.0281(4) 0.0307(13) Uani 1 1 d . . .
C29 C 0.6364(5) 1.1913(3) -0.0333(4) 0.0341(14) Uani 1 1 d . . .
C30 C 0.8035(5) 1.1258(3) 0.0390(4) 0.0283(13) Uani 1 1 d . . .
O2W O 0.4362(6) 0.2745(3) 0.0811(4) 0.101(2) Uani 1 1 d . . .
H2WA H 0.3728 0.2591 0.0699 0.121 Uiso 1 1 d R . .
H2WB H 0.4574 0.2568 0.1310 0.121 Uiso 1 1 d R . .
O3W O 0.2140(5) 0.1877(4) 0.1436(4) 0.093(2) Uani 1 1 d . . .
H3WA H 0.2710 0.1858 0.1785 0.111 Uiso 1 1 d R . .
H3WB H 0.2095 0.1459 0.1195 0.111 Uiso 1 1 d R . .
O4W O 0.0775(7) 0.1759(6) 0.2649(6) 0.060(3) Uani 0.50 1 d PU . .
H4WA H 0.1065 0.2023 0.3063 0.073 Uiso 0.50 1 d PR . .
H4WB H 0.1291 0.1536 0.2457 0.073 Uiso 0.50 1 d PR . .
O5W O 0.9240(9) 0.1121(6) 0.4679(6) 0.078(4) Uani 0.50 1 d P . .
H5WA H 0.8971 0.1226 0.5145 0.093 Uiso 0.50 1 d PR . .
H5WB H 0.9823 0.0909 0.4854 0.093 Uiso 0.50 1 d PR . .
O6W O 0.9031(10) 0.9706(7) 0.5731(8) 0.101(4) Uani 0.60 1 d P A 1
H6WA H 0.9573 0.9477 0.5594 0.122 Uiso 0.60 1 d PR A 1
H6WB H 0.8606 0.9372 0.5857 0.122 Uiso 0.60 1 d PR A 1
O7W O 0.7783(17) 0.8768(10) 0.5820(12) 0.115(7) Uani 0.40 1 d P B 2
H7WA H 0.8355 0.8834 0.5588 0.138 Uiso 0.40 1 d PR B 2
H7WB H 0.7290 0.8845 0.5409 0.138 Uiso 0.40 1 d PR B 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'
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'
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
O5 Tb1 O4 71.53(16) . .
O5 Tb1 O9 81.50(16) . .
O4 Tb1 O9 114.50(16) . .
O5 Tb1 O2 78.16(15) . .
O4 Tb1 O2 137.11(13) . .
O9 Tb1 O2 89.50(14) . .
O5 Tb1 O8 111.61(15) . .
O4 Tb1 O8 66.84(14) . .
O9 Tb1 O8 70.31(13) . .
O2 Tb1 O8 155.15(13) . .
O5 Tb1 O1 87.43(15) . .
O4 Tb1 O1 78.98(15) . .
O9 Tb1 O1 158.31(14) . .
O2 Tb1 O1 69.91(14) . .
O8 Tb1 O1 131.34(13) . .
O5 Tb1 O2 143.87(15) . 3_675
O4 Tb1 O2 144.09(13) . 3_675
O9 Tb1 O2 84.52(14) . 3_675
O2 Tb1 O2 68.54(14) . 3_675
O8 Tb1 O2 94.46(13) . 3_675
O1 Tb1 O2 93.80(13) . 3_675
O5 Tb1 O11 137.02(15) . .
O4 Tb1 O11 69.20(14) . .
O9 Tb1 O11 130.98(14) . .
O2 Tb1 O11 121.82(13) . .
O8 Tb1 O11 67.36(13) . .
O1 Tb1 O11 68.67(13) . .
O2 Tb1 O11 75.37(13) 3_675 .
O5 Tb1 Tb1 111.66(12) . 3_675
O4 Tb1 Tb1 159.02(11) . 3_675
O9 Tb1 Tb1 86.36(11) . 3_675
O2 Tb1 Tb1 34.56(9) . 3_675
O8 Tb1 Tb1 126.32(10) . 3_675
O1 Tb1 Tb1 80.45(10) . 3_675
O2 Tb1 Tb1 33.98(9) 3_675 3_675
O11 Tb1 Tb1 99.36(9) . 3_675
C1 N1 C3 109.1(6) . .
C1 N1 C13 109.1(5) . .
C3 N1 C13 111.3(5) . .
C1 N1 Ni3 103.9(4) . .
C3 N1 Ni3 106.3(4) . .
C13 N1 Ni3 116.7(4) . .
C2 N2 Ni3 105.8(4) . .
C2 N2 H2A 110.6 . .
Ni3 N2 H2A 110.6 . .
C2 N2 H2B 110.6 . .
Ni3 N2 H2B 110.6 . .
H2A N2 H2B 108.7 . .
C5 N3 C4 118.4(6) . .
C5 N3 Ni3 126.1(5) . .
C4 N3 Ni3 115.1(4) . .
C15 N4 C14 118.3(6) . .
C15 N4 Ni2 122.4(5) . .
C14 N4 Ni2 118.2(5) . .
O4 Ni2 N4 88.2(2) . .
O4 Ni2 O8 79.60(16) . .
N4 Ni2 O8 166.7(2) . .
O4 Ni2 O7 168.21(18) . .
N4 Ni2 O7 103.5(2) . .
O8 Ni2 O7 88.61(16) . .
O4 Ni2 O11 82.67(16) . .
N4 Ni2 O11 92.0(2) . .
O8 Ni2 O11 81.15(16) . .
O7 Ni2 O11 95.48(17) . .
O4 Ni2 O1W 94.87(18) . .
N4 Ni2 O1W 87.8(2) . .
O8 Ni2 O1W 98.49(18) . .
O7 Ni2 O1W 86.94(19) . .
O11 Ni2 O1W 177.54(17) . .
N3 Ni3 O11 162.3(2) . .
N3 Ni3 O1 90.36(19) . .
O11 Ni3 O1 84.70(16) . .
N3 Ni3 N2 103.8(2) . .
O11 Ni3 N2 93.8(2) . .
O1 Ni3 N2 102.97(19) . .
N3 Ni3 N1 82.9(2) . .
O11 Ni3 N1 99.55(18) . .
O1 Ni3 N1 170.15(19) . .
N2 Ni3 N1 85.7(2) . .
C12 O1 Ni3 128.3(4) . .
C12 O1 Tb1 128.7(3) . .
Ni3 O1 Tb1 102.71(16) . .
C11 O2 Tb1 121.1(4) . .
C11 O2 Tb1 125.6(4) . 3_675
Tb1 O2 Tb1 111.46(14) . 3_675
C22 O4 Ni2 131.2(4) . .
C22 O4 Tb1 130.5(4) . .
Ni2 O4 Tb1 93.49(15) . .
C21 O5 Tb1 139.1(5) . .
C23 O7 Ni2 124.3(4) . .
C30 O8 Ni2 130.8(4) . .
C30 O8 Tb1 129.7(4) . .
Ni2 O8 Tb1 90.49(14) . .
C29 O9 Tb1 139.8(4) . .
Ni3 O11 Ni2 117.18(19) . .
Ni3 O11 Tb1 103.83(16) . .
Ni2 O11 Tb1 89.61(14) . .
Ni3 O11 H11 114.4 . .
Ni2 O11 H11 114.4 . .
Tb1 O11 H11 114.4 . .
Ni2 O1W H1WA 120.4 . .
Ni2 O1W H1WB 125.9 . .
H1WA O1W H1WB 104.5 . .
N1 C1 C2 111.9(6) . .
N1 C1 H1A 109.2 . .
C2 C1 H1A 109.2 . .
N1 C1 H1B 109.2 . .
C2 C1 H1B 109.2 . .
H1A C1 H1B 107.9 . .
N2 C2 C1 109.1(5) . .
N2 C2 H2C 109.9 . .
C1 C2 H2C 109.9 . .
N2 C2 H2D 109.9 . .
C1 C2 H2D 109.9 . .
H2C C2 H2D 108.3 . .
N1 C3 C4 110.7(6) . .
N1 C3 H3A 109.5 . .
C4 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 108.1 . .
N3 C4 C3 109.7(6) . .
N3 C4 H4A 109.7 . .
C3 C4 H4A 109.7 . .
N3 C4 H4B 109.7 . .
C3 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
N3 C5 C6 127.9(6) . .
N3 C5 H5 116.0 . .
C6 C5 H5 116.0 . .
C7 C6 C12 119.3(6) . .
C7 C6 C5 115.4(6) . .
C12 C6 C5 125.3(6) . .
C8 C7 C6 122.2(7) . .
C8 C7 H7 118.9 . .
C6 C7 H7 118.9 . .
C7 C8 C9 118.3(7) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
C8 C9 C10 121.9(7) . .
C8 C9 H9 119.0 . .
C10 C9 H9 119.0 . .
C9 C10 C12 119.6(6) . .
C9 C10 C11 115.2(5) . .
C12 C10 C11 125.0(5) . .
O3 C11 O2 121.5(6) . .
O3 C11 C10 120.9(5) . .
O2 C11 C10 117.5(5) . .
O1 C12 C10 121.2(5) . .
O1 C12 C6 120.4(5) . .
C10 C12 C6 118.4(5) . .
C14 C13 N1 115.5(6) . .
C14 C13 H13A 108.4 . .
N1 C13 H13A 108.4 . .
C14 C13 H13B 108.4 . .
N1 C13 H13B 108.4 . .
H13A C13 H13B 107.5 . .
N4 C14 C13 111.4(6) . .
N4 C14 H14A 109.4 . .
C13 C14 H14A 109.4 . .
N4 C14 H14B 109.4 . .
C13 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
N4 C15 C16 128.0(7) . .
N4 C15 H15 116.0 . .
C16 C15 H15 116.0 . .
C22 C16 C17 117.1(8) . .
C22 C16 C15 124.6(7) . .
C17 C16 C15 117.9(8) . .
C18 C17 C16 122.9(10) . .
C18 C17 H17 118.6 . .
C16 C17 H17 118.6 . .
C17 C18 C19 119.7(9) . .
C17 C18 H18 120.2 . .
C19 C18 H18 120.2 . .
C18 C19 C20 120.5(9) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
C22 C20 C19 120.1(8) . .
C22 C20 C21 122.6(6) . .
C19 C20 C21 117.3(7) . .
O5 C21 O6 121.1(8) . .
O5 C21 C20 120.6(6) . .
O6 C21 C20 118.3(7) . .
O4 C22 C20 121.3(6) . .
O4 C22 C16 119.0(6) . .
C20 C22 C16 119.7(6) . .
O7 C23 C24 130.5(6) . .
O7 C23 H23 114.8 . .
C24 C23 H23 114.8 . .
C25 C24 C23 116.9(6) . .
C25 C24 C30 120.0(6) . .
C23 C24 C30 123.0(6) . .
C26 C25 C24 120.9(6) . .
C26 C25 H25 119.6 . .
C24 C25 H25 119.6 . .
C25 C26 C27 119.5(6) . .
C25 C26 H26 120.3 . .
C27 C26 H26 120.3 . .
C26 C27 C28 123.4(6) . .
C26 C27 H27 118.3 . .
C28 C27 H27 118.3 . .
C27 C28 C30 117.8(5) . .
C27 C28 C29 118.8(5) . .
C30 C28 C29 123.3(5) . .
O10 C29 O9 121.0(6) . .
O10 C29 C28 119.5(5) . .
O9 C29 C28 119.5(5) . .
O8 C30 C28 120.5(5) . .
O8 C30 C24 121.2(5) . .
C28 C30 C24 118.3(5) . .
H2WA O2W H2WB 104.5 . .
H3WA O3W H3WB 104.5 . .
H4WA O4W H4WB 104.5 . .
H5WA O5W H5WB 104.5 . .
H6WA O6W H6WB 104.5 . .
H7WA O7W H7WB 104.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O5 2.292(4) .
Tb1 O4 2.310(4) .
Tb1 O9 2.320(4) .
Tb1 O2 2.367(4) .
Tb1 O8 2.387(4) .
Tb1 O1 2.390(4) .
Tb1 O2 2.403(4) 3_675
Tb1 O11 2.406(4) .
N1 C1 1.480(9) .
N1 C3 1.495(8) .
N1 C13 1.502(8) .
N1 Ni3 2.158(5) .
N2 C2 1.479(8) .
N2 Ni3 2.038(6) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 C5 1.287(8) .
N3 C4 1.470(8) .
N3 Ni3 1.966(5) .
N4 C15 1.295(9) .
N4 C14 1.474(9) .
N4 Ni2 2.029(6) .
Ni2 O4 2.006(4) .
Ni2 O8 2.036(4) .
Ni2 O7 2.045(4) .
Ni2 O11 2.050(4) .
Ni2 O1W 2.091(5) .
Ni3 O11 1.981(4) .
Ni3 O1 2.035(4) .
O1 C12 1.332(7) .
O2 C11 1.309(7) .
O2 Tb1 2.403(4) 3_675
O3 C11 1.230(7) .
O4 C22 1.312(7) .
O5 C21 1.242(8) .
O6 C21 1.245(8) .
O7 C23 1.245(8) .
O8 C30 1.300(7) .
O9 C29 1.282(7) .
O10 C29 1.247(7) .
O11 H11 0.9800 .
O1W H1WA 0.8500 .
O1W H1WB 0.8500 .
C1 C2 1.517(10) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2C 0.9700 .
C2 H2D 0.9700 .
C3 C4 1.509(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.422(9) .
C5 H5 0.9300 .
C6 C7 1.393(9) .
C6 C12 1.419(8) .
C7 C8 1.383(11) .
C7 H7 0.9300 .
C8 C9 1.384(10) .
C8 H8 0.9300 .
C9 C10 1.392(8) .
C9 H9 0.9300 .
C10 C12 1.415(8) .
C10 C11 1.510(8) .
C13 C14 1.499(10) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.448(12) .
C15 H15 0.9300 .
C16 C22 1.412(11) .
C16 C17 1.421(12) .
C17 C18 1.354(14) .
C17 H17 0.9300 .
C18 C19 1.359(15) .
C18 H18 0.9300 .
C19 C20 1.416(10) .
C19 H19 0.9300 .
C20 C22 1.387(9) .
C20 C21 1.487(11) .
C23 C24 1.432(9) .
C23 H23 0.9300 .
C24 C25 1.398(9) .
C24 C30 1.438(8) .
C25 C26 1.372(10) .
C25 H25 0.9300 .
C26 C27 1.378(9) .
C26 H26 0.9300 .
C27 C28 1.391(8) .
C27 H27 0.9300 .
C28 C30 1.435(8) .
C28 C29 1.487(8) .
O2W H2WA 0.8500 .
O2W H2WB 0.8500 .
O3W H3WA 0.8500 .
O3W H3WB 0.8500 .
O4W H4WA 0.8500 .
O4W H4WB 0.8500 .
O5W H5WA 0.8500 .
O5W H5WB 0.8500 .
O6W H6WA 0.8500 .
O6W H6WB 0.8500 .
O7W H7WA 0.8500 .
O7W H7WB 0.8500 .
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
N2 H2A O10 0.90 2.46 3.198(7) 139.3 3_675
N2 H2B O9 0.90 2.49 3.061(7) 121.7 3_675
O11 H11 O3 0.98 2.08 2.947(6) 146.5 3_675
O1W H1WA O4W 0.85 1.83 2.659(9) 164.5 1_665
O1W H1WB O5W 0.85 1.98 2.818(10) 170.5 1_565
O2W H2WB O5 0.85 2.51 3.090(8) 126.6 1_545
O2W H2WB O6 0.85 2.60 3.309(11) 141.7 1_545
O3W H3WA O6 0.85 1.85 2.695(9) 174.2 1_545
O3W H3WB O3 0.85 2.10 2.917(8) 161.2 1_545
O4W H4WA O10 0.85 2.03 2.808(9) 151.3 4_576
O4W H4WA O7W 0.85 2.57 2.98(2) 110.3 3_666
O4W H4WB O3W 0.85 2.10 2.692(10) 126.5 .
O5W H5WA O2W 0.85 2.17 2.703(11) 120.2 4_666
O5W H5WB O6W 0.85 2.11 2.790(15) 136.0 3_766
O6W H6WA O5W 0.85 1.94 2.790(15) 175.1 3_766
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C15 N4 Ni2 O4 -24.0(6) . .
C14 N4 Ni2 O4 168.1(5) . .
C15 N4 Ni2 O8 -47.8(12) . .
C14 N4 Ni2 O8 144.3(8) . .
C15 N4 Ni2 O7 157.3(6) . .
C14 N4 Ni2 O7 -10.6(5) . .
C15 N4 Ni2 O11 -106.6(6) . .
C14 N4 Ni2 O11 85.5(5) . .
C15 N4 Ni2 O1W 70.9(6) . .
C14 N4 Ni2 O1W -96.9(5) . .
C5 N3 Ni3 O11 81.0(10) . .
C4 N3 Ni3 O11 -106.8(7) . .
C5 N3 Ni3 O1 7.5(7) . .
C4 N3 Ni3 O1 179.8(5) . .
C5 N3 Ni3 N2 -95.9(7) . .
C4 N3 Ni3 N2 76.3(6) . .
C5 N3 Ni3 N1 -179.7(7) . .
C4 N3 Ni3 N1 -7.5(5) . .
C2 N2 Ni3 N3 -103.7(4) . .
C2 N2 Ni3 O11 77.2(4) . .
C2 N2 Ni3 O1 162.7(4) . .
C2 N2 Ni3 N1 -22.1(4) . .
C1 N1 Ni3 N3 99.0(4) . .
C3 N1 Ni3 N3 -16.0(5) . .
C13 N1 Ni3 N3 -140.7(5) . .
C1 N1 Ni3 O11 -98.6(4) . .
C3 N1 Ni3 O11 146.3(4) . .
C13 N1 Ni3 O11 21.6(5) . .
C1 N1 Ni3 N2 -5.5(4) . .
C3 N1 Ni3 N2 -120.5(5) . .
C13 N1 Ni3 N2 114.7(5) . .
N3 Ni3 O1 C12 -14.0(5) . .
O11 Ni3 O1 C12 -177.0(5) . .
N2 Ni3 O1 C12 90.3(5) . .
N3 Ni3 O1 Tb1 160.5(2) . .
O11 Ni3 O1 Tb1 -2.51(16) . .
N2 Ni3 O1 Tb1 -95.2(2) . .
O5 Tb1 O1 C12 33.2(5) . .
O4 Tb1 O1 C12 104.9(5) . .
O9 Tb1 O1 C12 -25.9(7) . .
O2 Tb1 O1 C12 -45.2(4) . .
O8 Tb1 O1 C12 150.0(4) . .
O2 Tb1 O1 C12 -110.7(5) 3_675 .
O11 Tb1 O1 C12 176.7(5) . .
Tb1 Tb1 O1 C12 -79.3(5) 3_675 .
O5 Tb1 O1 Ni3 -141.27(19) . .
O4 Tb1 O1 Ni3 -69.59(17) . .
O9 Tb1 O1 Ni3 159.6(3) . .
O2 Tb1 O1 Ni3 140.4(2) . .
O8 Tb1 O1 Ni3 -24.4(3) . .
O2 Tb1 O1 Ni3 74.90(17) 3_675 .
O11 Tb1 O1 Ni3 2.21(14) . .
Tb1 Tb1 O1 Ni3 106.26(15) 3_675 .
O5 Tb1 O2 C11 -29.0(4) . .
O4 Tb1 O2 C11 16.4(5) . .
O9 Tb1 O2 C11 -110.4(4) . .
O8 Tb1 O2 C11 -145.3(4) . .
O1 Tb1 O2 C11 62.6(4) . .
O2 Tb1 O2 C11 165.3(5) 3_675 .
O11 Tb1 O2 C11 109.5(4) . .
Tb1 Tb1 O2 C11 165.3(5) 3_675 .
O5 Tb1 O2 Tb1 165.7(2) . 3_675
O4 Tb1 O2 Tb1 -148.82(18) . 3_675
O9 Tb1 O2 Tb1 84.31(17) . 3_675
O8 Tb1 O2 Tb1 49.5(4) . 3_675
O1 Tb1 O2 Tb1 -102.68(18) . 3_675
O2 Tb1 O2 Tb1 0.0 3_675 3_675
O11 Tb1 O2 Tb1 -55.7(2) . 3_675
N4 Ni2 O4 C22 24.8(6) . .
O8 Ni2 O4 C22 -160.7(6) . .
O7 Ni2 O4 C22 -161.3(8) . .
O11 Ni2 O4 C22 117.0(6) . .
O1W Ni2 O4 C22 -62.9(6) . .
N4 Ni2 O4 Tb1 -132.0(2) . .
O8 Ni2 O4 Tb1 42.62(15) . .
O7 Ni2 O4 Tb1 42.0(10) . .
O11 Ni2 O4 Tb1 -39.68(15) . .
O1W Ni2 O4 Tb1 140.38(18) . .
O5 Tb1 O4 C22 40.4(5) . .
O9 Tb1 O4 C22 111.6(5) . .
O2 Tb1 O4 C22 -6.9(6) . .
O8 Tb1 O4 C22 164.9(6) . .
O1 Tb1 O4 C22 -50.5(5) . .
O2 Tb1 O4 C22 -131.7(5) 3_675 .
O11 Tb1 O4 C22 -121.7(5) . .
Tb1 Tb1 O4 C22 -62.0(6) 3_675 .
O5 Tb1 O4 Ni2 -162.6(2) . .
O9 Tb1 O4 Ni2 -91.46(18) . .
O2 Tb1 O4 Ni2 150.08(15) . .
O8 Tb1 O4 Ni2 -38.16(14) . .
O1 Tb1 O4 Ni2 106.45(17) . .
O2 Tb1 O4 Ni2 25.3(3) 3_675 .
O11 Tb1 O4 Ni2 35.26(14) . .
Tb1 Tb1 O4 Ni2 95.0(3) 3_675 .
O4 Tb1 O5 C21 -15.4(7) . .
O9 Tb1 O5 C21 -134.9(7) . .
O2 Tb1 O5 C21 133.8(7) . .
O8 Tb1 O5 C21 -70.1(7) . .
O1 Tb1 O5 C21 63.8(7) . .
O2 Tb1 O5 C21 156.7(6) 3_675 .
O11 Tb1 O5 C21 9.4(8) . .
Tb1 Tb1 O5 C21 142.5(7) 3_675 .
O4 Ni2 O7 C23 13.3(12) . .
N4 Ni2 O7 C23 -172.9(5) . .
O8 Ni2 O7 C23 12.7(5) . .
O11 Ni2 O7 C23 93.7(5) . .
O1W Ni2 O7 C23 -85.9(5) . .
O4 Ni2 O8 C30 170.9(5) . .
N4 Ni2 O8 C30 -164.9(8) . .
O7 Ni2 O8 C30 -9.3(5) . .
O11 Ni2 O8 C30 -105.0(5) . .
O1W Ni2 O8 C30 77.4(5) . .
O4 Ni2 O8 Tb1 -40.85(15) . .
N4 Ni2 O8 Tb1 -16.6(9) . .
O7 Ni2 O8 Tb1 139.02(17) . .
O11 Ni2 O8 Tb1 43.25(14) . .
O1W Ni2 O8 Tb1 -134.29(16) . .
O5 Tb1 O8 C30 -116.4(5) . .
O4 Tb1 O8 C30 -173.7(5) . .
O9 Tb1 O8 C30 -44.5(4) . .
O2 Tb1 O8 C30 -7.2(6) . .
O1 Tb1 O8 C30 137.1(4) . .
O2 Tb1 O8 C30 38.0(5) 3_675 .
O11 Tb1 O8 C30 110.1(5) . .
Tb1 Tb1 O8 C30 25.2(5) 3_675 .
O5 Tb1 O8 Ni2 94.73(18) . .
O4 Tb1 O8 Ni2 37.42(14) . .
O9 Tb1 O8 Ni2 166.63(19) . .
O2 Tb1 O8 Ni2 -156.0(3) . .
O1 Tb1 O8 Ni2 -11.8(2) . .
O2 Tb1 O8 Ni2 -110.82(15) 3_675 .
O11 Tb1 O8 Ni2 -38.69(13) . .
Tb1 Tb1 O8 Ni2 -123.65(10) 3_675 .
O5 Tb1 O9 C29 138.3(7) . .
O4 Tb1 O9 C29 73.2(7) . .
O2 Tb1 O9 C29 -143.6(6) . .
O8 Tb1 O9 C29 21.7(6) . .
O1 Tb1 O9 C29 -161.6(5) . .
O2 Tb1 O9 C29 -75.1(6) 3_675 .
O11 Tb1 O9 C29 -9.9(7) . .
Tb1 Tb1 O9 C29 -109.1(6) 3_675 .
N3 Ni3 O11 Ni2 25.0(7) . .
O1 Ni3 O11 Ni2 99.3(2) . .
N2 Ni3 O11 Ni2 -158.0(2) . .
N1 Ni3 O11 Ni2 -71.7(2) . .
N3 Ni3 O11 Tb1 -71.8(7) . .
O1 Ni3 O11 Tb1 2.51(16) . .
N2 Ni3 O11 Tb1 105.19(19) . .
N1 Ni3 O11 Tb1 -168.53(19) . .
O4 Ni2 O11 Ni3 -67.6(2) . .
N4 Ni2 O11 Ni3 20.3(2) . .
O8 Ni2 O11 Ni3 -148.2(2) . .
O7 Ni2 O11 Ni3 124.1(2) . .
O4 Ni2 O11 Tb1 37.73(15) . .
N4 Ni2 O11 Tb1 125.67(19) . .
O8 Ni2 O11 Tb1 -42.82(13) . .
O7 Ni2 O11 Tb1 -130.55(15) . .
O5 Tb1 O11 Ni3 58.4(3) . .
O4 Tb1 O11 Ni3 83.63(18) . .
O9 Tb1 O11 Ni3 -171.44(16) . .
O2 Tb1 O11 Ni3 -49.7(2) . .
O8 Tb1 O11 Ni3 156.3(2) . .
O1 Tb1 O11 Ni3 -2.28(15) . .
O2 Tb1 O11 Ni3 -102.38(17) 3_675 .
Tb1 Tb1 O11 Ni3 -78.11(14) 3_675 .
O5 Tb1 O11 Ni2 -59.5(2) . .
O4 Tb1 O11 Ni2 -34.32(14) . .
O9 Tb1 O11 Ni2 70.6(2) . .
O2 Tb1 O11 Ni2 -167.69(12) . .
O8 Tb1 O11 Ni2 38.37(13) . .
O1 Tb1 O11 Ni2 -120.23(17) . .
O2 Tb1 O11 Ni2 139.67(16) 3_675 .
Tb1 Tb1 O11 Ni2 163.94(10) 3_675 .
C3 N1 C1 C2 145.5(6) . .
C13 N1 C1 C2 -92.8(6) . .
Ni3 N1 C1 C2 32.5(6) . .
Ni3 N2 C2 C1 45.9(6) . .
N1 C1 C2 N2 -54.8(8) . .
C1 N1 C3 C4 -75.5(7) . .
C13 N1 C3 C4 164.0(6) . .
Ni3 N1 C3 C4 36.0(7) . .
C5 N3 C4 C3 -157.5(7) . .
Ni3 N3 C4 C3 29.6(8) . .
N1 C3 C4 N3 -43.6(9) . .
C4 N3 C5 C6 -175.4(8) . .
Ni3 N3 C5 C6 -3.3(12) . .
N3 C5 C6 C7 -179.7(8) . .
N3 C5 C6 C12 1.0(13) . .
C12 C6 C7 C8 -0.1(13) . .
C5 C6 C7 C8 -179.4(8) . .
C6 C7 C8 C9 3.9(14) . .
C7 C8 C9 C10 -2.5(13) . .
C8 C9 C10 C12 -2.8(11) . .
C8 C9 C10 C11 171.7(7) . .
Tb1 O2 C11 O3 125.4(5) . .
Tb1 O2 C11 O3 -71.6(7) 3_675 .
Tb1 O2 C11 C10 -57.4(6) . .
Tb1 O2 C11 C10 105.7(5) 3_675 .
C9 C10 C11 O3 8.4(9) . .
C12 C10 C11 O3 -177.4(6) . .
C9 C10 C11 O2 -168.9(6) . .
C12 C10 C11 O2 5.3(9) . .
Ni3 O1 C12 C10 -165.9(4) . .
Tb1 O1 C12 C10 21.0(8) . .
Ni3 O1 C12 C6 15.4(8) . .
Tb1 O1 C12 C6 -157.7(5) . .
C9 C10 C12 O1 -172.1(6) . .
C11 C10 C12 O1 13.9(9) . .
C9 C10 C12 C6 6.6(9) . .
C11 C10 C12 C6 -167.4(6) . .
C7 C6 C12 O1 173.5(7) . .
C5 C6 C12 O1 -7.2(11) . .
C7 C6 C12 C10 -5.2(10) . .
C5 C6 C12 C10 174.1(7) . .
C1 N1 C13 C14 -172.6(6) . .
C3 N1 C13 C14 -52.2(7) . .
Ni3 N1 C13 C14 70.0(7) . .
C15 N4 C14 C13 124.3(8) . .
Ni2 N4 C14 C13 -67.3(7) . .
N1 C13 C14 N4 -53.6(8) . .
C14 N4 C15 C16 -177.8(9) . .
Ni2 N4 C15 C16 14.3(13) . .
N4 C15 C16 C22 8.5(16) . .
N4 C15 C16 C17 -179.1(10) . .
C22 C16 C17 C18 -1.5(18) . .
C15 C16 C17 C18 -174.5(11) . .
C16 C17 C18 C19 2(2) . .
C17 C18 C19 C20 -0.3(19) . .
C18 C19 C20 C22 -2.9(15) . .
C18 C19 C20 C21 176.3(10) . .
Tb1 O5 C21 O6 176.3(6) . .
Tb1 O5 C21 C20 -5.9(12) . .
C22 C20 C21 O5 18.5(11) . .
C19 C20 C21 O5 -160.7(8) . .
C22 C20 C21 O6 -163.7(8) . .
C19 C20 C21 O6 17.1(11) . .
Ni2 O4 C22 C20 167.1(5) . .
Tb1 O4 C22 C20 -44.1(9) . .
Ni2 O4 C22 C16 -11.7(10) . .
Tb1 O4 C22 C16 137.0(6) . .
C19 C20 C22 O4 -175.0(8) . .
C21 C20 C22 O4 5.9(11) . .
C19 C20 C22 C16 3.8(12) . .
C21 C20 C22 C16 -175.3(7) . .
C17 C16 C22 O4 177.2(8) . .
C15 C16 C22 O4 -10.4(13) . .
C17 C16 C22 C20 -1.7(13) . .
C15 C16 C22 C20 170.8(8) . .
Ni2 O7 C23 C24 -9.3(10) . .
O7 C23 C24 C25 179.9(7) . .
O7 C23 C24 C30 -3.7(11) . .
C23 C24 C25 C26 176.8(7) . .
C30 C24 C25 C26 0.3(11) . .
C24 C25 C26 C27 -2.3(13) . .
C25 C26 C27 C28 1.4(12) . .
C26 C27 C28 C30 1.5(10) . .
C26 C27 C28 C29 -179.1(7) . .
Tb1 O9 C29 O10 179.7(5) . .
Tb1 O9 C29 C28 0.0(10) . .
C27 C28 C29 O10 -17.4(9) . .
C30 C28 C29 O10 161.9(6) . .
C27 C28 C29 O9 162.3(6) . .
C30 C28 C29 O9 -18.4(9) . .
Ni2 O8 C30 C28 -177.1(4) . .
Tb1 O8 C30 C28 46.0(7) . .
Ni2 O8 C30 C24 1.0(8) . .
Tb1 O8 C30 C24 -135.9(5) . .
C27 C28 C30 O8 174.8(6) . .
C29 C28 C30 O8 -4.6(9) . .
C27 C28 C30 C24 -3.4(8) . .
C29 C28 C30 C24 177.2(6) . .
C25 C24 C30 O8 -175.6(6) . .
C23 C24 C30 O8 8.2(9) . .
C25 C24 C30 C28 2.6(9) . .
C23 C24 C30 C28 -173.6(6) . .
