#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/74/4307444.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_4307444
loop_
_publ_author_name
'Takuya Shiga'
'Nobuhiro Ito'
'Akiko Hidaka'
'Hisashi Ōkawa'
'Susumu Kitagawa'
'Masaaki Ohba'
_publ_contact_author_address
;Department of Synthetic Chemistry and Biological Chemistry,
Graduate School of Engineering,
Kyoto University,
Katsura, Nishikyo-ku, Kyoto 615-8510, Japan
;
_publ_contact_author_email       ohba@sbchem.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-383-2732
_publ_contact_author_name        'Masaaki Ohba'
_publ_contact_author_phone       +81-75-383-2807
_publ_section_title
;
Series of Trinuclear NiIILnIIINiII Complexes Derived from
2,6-Di(acetoacetyl)pyridine: Synthesis, Structure, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3492
_journal_page_last               3501
_journal_paper_doi               10.1021/ic0619153
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C34 H50 N5 Ni2 O23 Tm'
_chemical_formula_weight         1183.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                109.1785(7)
_cell_angle_beta                 100.1183(7)
_cell_angle_gamma                110.2845(8)
_cell_formula_units_Z            2
_cell_length_a                   10.8582(1)
_cell_length_b                   14.8577
_cell_length_c                   16.5084(2)
_cell_measurement_reflns_used    13798
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     2229.86(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 8.00
_diffrn_measured_fraction_theta_full 0.9836
_diffrn_measured_fraction_theta_max 0.9836
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21040
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    2.893
_exptl_absorpt_correction_T_max  0.445
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10071
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.0070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.09500(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                9170
_reflns_number_total             3350
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic0619153si20061007_020931_17.cif
_cod_data_source_block
12_Ni2Tm_D_[Ni2Tm(L)2(NO3)2(H2O)(MeOH)3]NO3.Et2O.MeOH
_cod_original_cell_volume        2229.85(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C34 H50 N5 O23 Ni2 Tm '
_cod_database_code               4307444
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm Tm 0.18263(1) 0.44181(1) 0.243507(8) 0.01537(5) Uani 1.00 d . . .
Ni(1) Ni -0.08566(4) 0.18559(3) 0.18973(3) 0.0193(1) Uani 1.00 d . . .
Ni(2) Ni 0.45029(4) 0.69516(3) 0.29837(3) 0.0192(1) Uani 1.00 d . . .
O(1) O -0.2189(2) 0.1360(2) 0.2522(2) 0.0292(6) Uani 1.00 d . . .
O(2) O 0.0164(2) 0.3315(2) 0.2908(1) 0.0185(5) Uani 1.00 d . . .
O(3) O 0.4051(2) 0.5812(2) 0.3445(1) 0.0201(5) Uani 1.00 d . . .
O(4) O 0.6428(2) 0.7791(2) 0.3900(2) 0.0288(6) Uani 1.00 d . . .
O(5) O 0.4571(3) 0.8039(2) 0.2498(2) 0.0269(6) Uani 1.00 d . . .
O(6) O 0.2636(2) 0.5882(2) 0.2048(1) 0.0190(5) Uani 1.00 d . . .
O(7) O 0.0396(2) 0.2600(2) 0.1325(1) 0.0192(5) Uani 1.00 d . . .
O(8) O -0.1659(3) 0.0457(2) 0.0847(2) 0.0290(6) Uani 1.00 d . . .
O(9) O 0.3454(2) 0.3949(2) 0.1790(2) 0.0244(6) Uani 1.00 d . . .
O(10) O 0.2993(2) 0.3406(2) 0.2811(2) 0.0219(6) Uani 1.00 d . . .
O(11) O 0.4480(3) 0.3055(2) 0.2175(2) 0.0324(7) Uani 1.00 d . . .
O(12) O 0.0832(3) 0.5583(2) 0.3230(2) 0.0259(6) Uani 1.00 d . . .
O(13) O -0.0402(2) 0.4412(2) 0.1865(2) 0.0238(6) Uani 1.00 d . . .
O(14) O -0.1302(3) 0.5325(3) 0.2666(2) 0.0390(9) Uani 1.00 d . . .
O(15) O 0.3254(3) 0.1209(2) 0.3003(2) 0.0486(9) Uani 1.00 d . . .
O(16) O 0.1270(3) -0.0153(2) 0.2460(2) 0.0383(7) Uani 1.00 d . . .
O(17) O 0.3083(4) -0.0154(3) 0.3246(3) 0.059(1) Uani 1.00 d . . .
O(18) O 0.0655(2) 0.1534(2) 0.2540(2) 0.0271(6) Uani 1.00 d . . .
O(19) O -0.2296(2) 0.2285(2) 0.1244(2) 0.0314(7) Uani 1.00 d . . .
O(20) O 0.5422(3) 0.6350(2) 0.2078(2) 0.0302(7) Uani 1.00 d . . .
O(21) O 0.3641(2) 0.7649(2) 0.3891(2) 0.0254(6) Uani 1.00 d . . .
O(22) O 0.1438(3) 0.7930(2) 0.3177(2) 0.0424(8) Uani 1.00 d . . .
O(23) O 0.3247(6) 0.2305(5) -0.1384(4) 0.106(3) Uani 1.00 d . . .
N(1) N 0.2394(3) 0.4842(2) 0.4141(2) 0.0176(6) Uani 1.00 d . . .
N(2) N 0.1203(3) 0.4023(2) 0.0732(2) 0.0184(6) Uani 1.00 d . . .
N(3) N 0.3661(3) 0.3449(2) 0.2246(2) 0.0212(6) Uani 1.00 d . . .
N(4) N -0.0308(3) 0.5128(2) 0.2603(2) 0.0245(7) Uani 1.00 d . . .
N(5) N 0.2545(3) 0.0309(3) 0.2907(2) 0.0310(8) Uani 1.00 d . . .
C(1) C -0.3212(5) 0.1430(4) 0.3671(3) 0.051(1) Uani 1.00 d . . .
C(2) C -0.2076(4) 0.1880(3) 0.3324(2) 0.0302(9) Uani 1.00 d . . .
C(3) C -0.0909(3) 0.2861(3) 0.3938(2) 0.0267(8) Uani 1.00 d . . .
C(4) C 0.0150(3) 0.3465(2) 0.3729(2) 0.0191(7) Uani 1.00 d . . .
C(5) C 0.1423(3) 0.4360(3) 0.4453(2) 0.0202(7) Uani 1.00 d . . .
C(6) C 0.1639(4) 0.4654(3) 0.5381(2) 0.0280(9) Uani 1.00 d . . .
C(7) C 0.2904(4) 0.5462(3) 0.5991(2) 0.0328(9) Uani 1.00 d . . .
C(8) C 0.3906(4) 0.5946(3) 0.5668(2) 0.0283(8) Uani 1.00 d . . .
C(9) C 0.3623(3) 0.5611(3) 0.4735(2) 0.0209(7) Uani 1.00 d . . .
C(10) C 0.4581(3) 0.6132(3) 0.4312(2) 0.0205(7) Uani 1.00 d . . .
C(11) C 0.5904(3) 0.6910(3) 0.4847(2) 0.0251(8) Uani 1.00 d . . .
C(12) C 0.6789(3) 0.7646(3) 0.4591(2) 0.0266(8) Uani 1.00 d . . .
C(13) C 0.8272(4) 0.8331(3) 0.5201(3) 0.0372(10) Uani 1.00 d . . .
C(14) C 0.4027(5) 0.8715(3) 0.1444(3) 0.039(1) Uani 1.00 d . . .
C(15) C 0.3838(3) 0.7825(3) 0.1729(2) 0.0246(8) Uani 1.00 d . . .
C(16) C 0.2850(4) 0.6777(3) 0.1080(2) 0.0250(8) Uani 1.00 d . . .
C(17) C 0.2405(3) 0.5889(3) 0.1247(2) 0.0190(7) Uani 1.00 d . . .
C(18) C 0.1607(3) 0.4824(3) 0.0473(2) 0.0198(7) Uani 1.00 d . . .
C(19) C 0.1367(4) 0.4643(3) -0.0432(2) 0.0265(8) Uani 1.00 d . . .
C(20) C 0.0705(4) 0.3618(3) -0.1091(2) 0.0322(9) Uani 1.00 d . . .
C(21) C 0.0278(4) 0.2788(3) -0.0830(2) 0.0281(8) Uani 1.00 d . . .
C(22) C 0.0538(3) 0.3027(2) 0.0087(2) 0.0193(7) Uani 1.00 d . . .
C(23) C 0.0045(3) 0.2218(2) 0.0451(2) 0.0191(7) Uani 1.00 d . . .
C(24) C -0.0777(3) 0.1170(3) -0.0149(2) 0.0239(8) Uani 1.00 d . . .
C(25) C -0.1543(3) 0.0338(3) 0.0074(2) 0.0244(8) Uani 1.00 d . . .
C(26) C -0.2308(4) -0.0753(3) -0.0676(3) 0.0350(9) Uani 1.00 d . . .
C(27) C -0.3705(5) 0.1949(6) 0.1220(4) 0.071(2) Uani 1.00 d . . .
C(28) C 0.6431(4) 0.5987(3) 0.2336(3) 0.034(1) Uani 1.00 d . . .
C(29) C 0.4475(4) 0.8745(3) 0.4486(3) 0.0345(9) Uani 1.00 d . . .
C(30) C 0.0720(6) 0.8103(4) 0.3809(4) 0.062(2) Uani 1.00 d . . .
C(31) C 0.1848(6) 0.0761(5) -0.2836(6) 0.080(2) Uani 1.00 d . . .
C(32) C 0.2195(6) 0.1086(5) -0.1867(6) 0.073(2) Uani 1.00 d . . .
C(33) C 0.3619(8) 0.2609(9) -0.0472(6) 0.099(3) Uani 1.00 d . . .
C(34) C 0.4461(8) 0.3706(7) -0.0006(5) 0.088(2) Uani 1.00 d . . .
H(1) H -0.4086 0.1340 0.3302 0.0641 Uiso 1.00 calc . . .
H(2) H -0.3321 0.0755 0.3638 0.0641 Uiso 1.00 calc . . .
H(3) H -0.3038 0.1888 0.4278 0.0641 Uiso 1.00 calc . . .
H(4) H -0.0868 0.3112 0.4562 0.0330 Uiso 1.00 calc . . .
H(5) H 0.0930 0.4309 0.5591 0.0346 Uiso 1.00 calc . . .
H(6) H 0.3072 0.5681 0.6631 0.0403 Uiso 1.00 calc . . .
H(7) H 0.4790 0.6497 0.6081 0.0343 Uiso 1.00 calc . . .
H(8) H 0.6253 0.6963 0.5444 0.0319 Uiso 1.00 calc . . .
H(9) H 0.8448 0.8160 0.5703 0.0470 Uiso 1.00 calc . . .
H(10) H 0.8451 0.9061 0.5424 0.0470 Uiso 1.00 calc . . .
H(11) H 0.8898 0.8232 0.4877 0.0470 Uiso 1.00 calc . . .
H(12) H 0.4967 0.9040 0.1452 0.0494 Uiso 1.00 calc . . .
H(13) H 0.3851 0.9240 0.1856 0.0494 Uiso 1.00 calc . . .
H(14) H 0.3417 0.8460 0.0850 0.0494 Uiso 1.00 calc . . .
H(15) H 0.2482 0.6690 0.0475 0.0310 Uiso 1.00 calc . . .
H(16) H 0.1659 0.5223 -0.0601 0.0338 Uiso 1.00 calc . . .
H(17) H 0.0539 0.3469 -0.1720 0.0396 Uiso 1.00 calc . . .
H(18) H -0.0192 0.2067 -0.1282 0.0346 Uiso 1.00 calc . . .
H(19) H -0.0829 0.0984 -0.0767 0.0307 Uiso 1.00 calc . . .
H(20) H -0.2148 -0.0746 -0.1223 0.0439 Uiso 1.00 calc . . .
H(21) H -0.3287 -0.1002 -0.0773 0.0439 Uiso 1.00 calc . . .
H(22) H -0.2012 -0.1226 -0.0526 0.0439 Uiso 1.00 calc . . .
H(23) H 0.0752 0.0901 0.2341 0.0291 Uiso 1.00 calc . . .
H(24) H 0.1567 0.1985 0.2648 0.0291 Uiso 1.00 calc . . .
H(25) H -0.1880 0.3029 0.1444 0.0291 Uiso 1.00 calc . . .
H(26) H -0.3759 0.2139 0.1815 0.0834 Uiso 1.00 calc . . .
H(27) H -0.4137 0.2281 0.0928 0.0834 Uiso 1.00 calc . . .
H(28) H -0.4207 0.1203 0.0881 0.0834 Uiso 1.00 calc . . .
H(29) H 0.5577 0.6584 0.1661 0.0291 Uiso 1.00 calc . . .
H(30) H 0.7286 0.6563 0.2740 0.0422 Uiso 1.00 calc . . .
H(31) H 0.6591 0.5590 0.1805 0.0422 Uiso 1.00 calc . . .
H(32) H 0.6092 0.5529 0.2619 0.0422 Uiso 1.00 calc . . .
H(33) H 0.2808 0.7620 0.3593 0.0291 Uiso 1.00 calc . . .
H(34) H 0.5138 0.8814 0.4994 0.0442 Uiso 1.00 calc . . .
H(35) H 0.4961 0.9111 0.4177 0.0442 Uiso 1.00 calc . . .
H(36) H 0.3910 0.9074 0.4706 0.0442 Uiso 1.00 calc . . .
H(37) H 0.1808 0.8373 0.3065 0.0291 Uiso 1.00 calc . . .
H(38) H 0.1287 0.8750 0.4340 0.0722 Uiso 1.00 calc . . .
H(39) H -0.0108 0.8157 0.3547 0.0722 Uiso 1.00 calc . . .
H(40) H 0.0441 0.7536 0.3988 0.0722 Uiso 1.00 calc . . .
H(41) H 0.2663 0.0884 -0.3009 0.0945 Uiso 1.00 calc . . .
H(42) H 0.1213 0.0040 -0.3157 0.0945 Uiso 1.00 calc . . .
H(43) H 0.1425 0.1178 -0.3006 0.0945 Uiso 1.00 calc . . .
H(44) H 0.1386 0.0974 -0.1698 0.0862 Uiso 1.00 calc . . .
H(45) H 0.2626 0.0681 -0.1701 0.0862 Uiso 1.00 calc . . .
H(46) H 0.4194 0.2305 -0.0292 0.1198 Uiso 1.00 calc . . .
H(47) H 0.2872 0.2482 -0.0270 0.1198 Uiso 1.00 calc . . .
H(48) H 0.5277 0.3894 -0.0174 0.1040 Uiso 1.00 calc . . .
H(49) H 0.4730 0.3898 0.0633 0.1040 Uiso 1.00 calc . . .
H(50) H 0.3956 0.4071 -0.0144 0.1040 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Tm Tm -0.314 5.248
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ni Ni 0.339 1.112
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(2) Tm O(3) 123.79(7) . . . yes
O(2) Tm O(6) 150.40(7) . . . yes
O(2) Tm O(7) 64.09(7) . . . yes
O(2) Tm O(9) 124.48(8) . . . yes
O(2) Tm O(10) 78.39(7) . . . yes
O(2) Tm O(12) 76.19(8) . . . yes
O(2) Tm O(13) 72.20(7) . . . yes
O(2) Tm N(1) 61.66(8) . . . yes
O(2) Tm N(2) 117.91(8) . . . yes
O(3) Tm O(6) 65.54(8) . . . yes
O(3) Tm O(7) 150.35(7) . . . yes
O(3) Tm O(9) 75.89(8) . . . yes
O(3) Tm O(10) 79.17(8) . . . yes
O(3) Tm O(12) 86.08(8) . . . yes
O(3) Tm O(13) 132.41(8) . . . yes
O(3) Tm N(1) 62.27(8) . . . yes
O(3) Tm N(2) 118.25(8) . . . yes
O(6) Tm O(7) 123.79(7) . . . yes
O(6) Tm O(9) 84.24(7) . . . yes
O(6) Tm O(10) 130.43(7) . . . yes
O(6) Tm O(12) 76.70(7) . . . yes
O(6) Tm O(13) 81.83(7) . . . yes
O(6) Tm N(1) 116.93(8) . . . yes
O(6) Tm N(2) 62.41(8) . . . yes
O(7) Tm O(9) 77.28(8) . . . yes
O(7) Tm O(10) 74.70(7) . . . yes
O(7) Tm O(12) 122.71(8) . . . yes
O(7) Tm O(13) 76.70(8) . . . yes
O(7) Tm N(1) 119.17(8) . . . yes
O(7) Tm N(2) 61.41(8) . . . yes
O(9) Tm O(10) 53.00(7) . . . yes
O(9) Tm O(12) 157.95(9) . . . yes
O(9) Tm O(13) 136.27(8) . . . yes
O(9) Tm N(1) 113.58(8) . . . yes
O(9) Tm N(2) 68.25(8) . . . yes
O(10) Tm O(12) 136.15(8) . . . yes
O(10) Tm O(13) 145.64(8) . . . yes
O(10) Tm N(1) 69.53(8) . . . yes
O(10) Tm N(2) 112.30(8) . . . yes
O(12) Tm O(13) 51.97(8) . . . yes
O(12) Tm N(1) 67.04(8) . . . yes
O(12) Tm N(2) 111.09(8) . . . yes
O(13) Tm N(1) 109.70(8) . . . yes
O(13) Tm N(2) 68.54(8) . . . yes
N(1) Tm N(2) 178.10(7) . . . yes
O(1) Ni(1) O(2) 93.11(10) . . . yes
O(1) Ni(1) O(7) 168.8(1) . . . yes
O(1) Ni(1) O(8) 93.8(1) . . . yes
O(1) Ni(1) O(18) 94.9(1) . . . yes
O(1) Ni(1) O(19) 88.2(1) . . . yes
O(2) Ni(1) O(7) 79.55(9) . . . yes
O(2) Ni(1) O(8) 172.81(9) . . . yes
O(2) Ni(1) O(18) 85.60(10) . . . yes
O(2) Ni(1) O(19) 91.75(10) . . . yes
O(7) Ni(1) O(8) 93.96(10) . . . yes
O(7) Ni(1) O(18) 92.99(9) . . . yes
O(7) Ni(1) O(19) 83.54(9) . . . yes
O(8) Ni(1) O(18) 91.7(1) . . . yes
O(8) Ni(1) O(19) 90.6(1) . . . yes
O(18) Ni(1) O(19) 176.0(1) . . . yes
O(3) Ni(2) O(4) 92.36(10) . . . yes
O(3) Ni(2) O(5) 168.94(10) . . . yes
O(3) Ni(2) O(6) 79.76(9) . . . yes
O(3) Ni(2) O(20) 97.55(10) . . . yes
O(3) Ni(2) O(21) 85.92(9) . . . yes
O(4) Ni(2) O(5) 96.3(1) . . . yes
O(4) Ni(2) O(6) 169.74(10) . . . yes
O(4) Ni(2) O(20) 86.3(1) . . . yes
O(4) Ni(2) O(21) 92.4(1) . . . yes
O(5) Ni(2) O(6) 92.35(10) . . . yes
O(5) Ni(2) O(20) 89.9(1) . . . yes
O(5) Ni(2) O(21) 86.86(10) . . . yes
O(6) Ni(2) O(20) 88.20(10) . . . yes
O(6) Ni(2) O(21) 93.58(9) . . . yes
O(20) Ni(2) O(21) 176.3(1) . . . yes
Ni(1) O(1) C(2) 124.4(2) . . . yes
Tm O(2) Ni(1) 108.62(9) . . . yes
Tm O(2) C(4) 128.4(2) . . . yes
Ni(1) O(2) C(4) 120.0(2) . . . yes
Tm O(3) Ni(2) 107.08(9) . . . yes
Tm O(3) C(10) 128.6(2) . . . yes
Ni(2) O(3) C(10) 115.9(2) . . . yes
Ni(2) O(4) C(12) 123.2(2) . . . yes
Ni(2) O(5) C(15) 123.8(2) . . . yes
Tm O(6) Ni(2) 107.61(9) . . . yes
Tm O(6) C(17) 128.8(2) . . . yes
Ni(2) O(6) C(17) 116.6(2) . . . yes
Tm O(7) Ni(1) 107.71(9) . . . yes
Tm O(7) C(23) 128.8(2) . . . yes
Ni(1) O(7) C(23) 119.0(2) . . . yes
Ni(1) O(8) C(25) 123.4(2) . . . yes
Tm O(9) N(3) 96.5(2) . . . yes
Tm O(10) N(3) 94.6(2) . . . yes
Tm O(12) N(4) 94.9(2) . . . yes
Tm O(13) N(4) 96.5(2) . . . yes
Ni(1) O(19) C(27) 124.3(3) . . . yes
Ni(2) O(20) C(28) 121.1(2) . . . yes
Ni(2) O(21) C(29) 115.8(2) . . . yes
C(32) O(23) C(33) 108.3(6) . . . yes
Tm N(1) C(5) 120.5(2) . . . yes
Tm N(1) C(9) 120.2(2) . . . yes
C(5) N(1) C(9) 119.0(3) . . . yes
Tm N(2) C(18) 120.2(2) . . . yes
Tm N(2) C(22) 121.3(2) . . . yes
C(18) N(2) C(22) 118.4(3) . . . yes
O(9) N(3) O(10) 115.9(2) . . . yes
O(9) N(3) O(11) 122.2(3) . . . yes
O(10) N(3) O(11) 121.8(3) . . . yes
O(12) N(4) O(13) 116.1(3) . . . yes
O(12) N(4) O(14) 123.7(3) . . . yes
O(13) N(4) O(14) 120.2(3) . . . yes
O(15) N(5) O(16) 120.2(3) . . . yes
O(15) N(5) O(17) 120.3(3) . . . yes
O(16) N(5) O(17) 119.5(3) . . . yes
O(1) C(2) C(1) 117.8(3) . . . yes
O(1) C(2) C(3) 124.3(3) . . . yes
C(1) C(2) C(3) 117.9(3) . . . yes
C(2) C(3) C(4) 127.0(3) . . . yes
O(2) C(4) C(3) 124.8(3) . . . yes
O(2) C(4) C(5) 114.1(3) . . . yes
C(3) C(4) C(5) 121.1(3) . . . yes
N(1) C(5) C(4) 114.0(3) . . . yes
N(1) C(5) C(6) 122.1(3) . . . yes
C(4) C(5) C(6) 123.8(3) . . . yes
C(5) C(6) C(7) 118.5(3) . . . yes
C(6) C(7) C(8) 119.3(3) . . . yes
C(7) C(8) C(9) 119.2(3) . . . yes
N(1) C(9) C(8) 121.8(3) . . . yes
N(1) C(9) C(10) 114.1(3) . . . yes
C(8) C(9) C(10) 123.8(3) . . . yes
O(3) C(10) C(9) 114.7(3) . . . yes
O(3) C(10) C(11) 125.5(3) . . . yes
C(9) C(10) C(11) 119.8(3) . . . yes
C(10) C(11) C(12) 125.6(3) . . . yes
O(4) C(12) C(11) 125.1(3) . . . yes
O(4) C(12) C(13) 116.5(3) . . . yes
C(11) C(12) C(13) 118.4(3) . . . yes
O(5) C(15) C(14) 118.1(3) . . . yes
O(5) C(15) C(16) 124.4(3) . . . yes
C(14) C(15) C(16) 117.5(3) . . . yes
C(15) C(16) C(17) 126.1(3) . . . yes
O(6) C(17) C(16) 125.5(3) . . . yes
O(6) C(17) C(18) 114.8(3) . . . yes
C(16) C(17) C(18) 119.7(3) . . . yes
N(2) C(18) C(17) 113.6(3) . . . yes
N(2) C(18) C(19) 122.1(3) . . . yes
C(17) C(18) C(19) 124.2(3) . . . yes
C(18) C(19) C(20) 119.3(3) . . . yes
C(19) C(20) C(21) 119.1(3) . . . yes
C(20) C(21) C(22) 118.6(3) . . . yes
N(2) C(22) C(21) 122.6(3) . . . yes
N(2) C(22) C(23) 113.5(3) . . . yes
C(21) C(22) C(23) 123.9(3) . . . yes
O(7) C(23) C(22) 114.4(3) . . . yes
O(7) C(23) C(24) 126.2(3) . . . yes
C(22) C(23) C(24) 119.3(3) . . . yes
C(23) C(24) C(25) 126.2(3) . . . yes
O(8) C(25) C(24) 125.2(3) . . . yes
O(8) C(25) C(26) 117.4(3) . . . yes
C(24) C(25) C(26) 117.3(3) . . . yes
O(23) C(32) C(31) 107.8(5) . . . yes
O(23) C(33) C(34) 110.8(6) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm O(2) 2.416(2) . . yes
Tm O(3) 2.398(2) . . yes
Tm O(6) 2.387(2) . . yes
Tm O(7) 2.431(2) . . yes
Tm O(9) 2.403(2) . . yes
Tm O(10) 2.431(2) . . yes
Tm O(12) 2.487(2) . . yes
Tm O(13) 2.432(2) . . yes
Tm N(1) 2.581(3) . . yes
Tm N(2) 2.584(3) . . yes
Ni(1) O(1) 1.996(2) . . yes
Ni(1) O(2) 2.005(2) . . yes
Ni(1) O(7) 2.015(2) . . yes
Ni(1) O(8) 1.982(3) . . yes
Ni(1) O(18) 2.078(2) . . yes
Ni(1) O(19) 2.137(3) . . yes
Ni(2) O(3) 2.022(2) . . yes
Ni(2) O(4) 2.014(2) . . yes
Ni(2) O(5) 2.011(2) . . yes
Ni(2) O(6) 2.018(2) . . yes
Ni(2) O(20) 2.072(3) . . yes
Ni(2) O(21) 2.084(2) . . yes
O(1) C(2) 1.253(4) . . yes
O(2) C(4) 1.304(4) . . yes
O(3) C(10) 1.296(4) . . yes
O(4) C(12) 1.251(4) . . yes
O(5) C(15) 1.246(4) . . yes
O(6) C(17) 1.306(4) . . yes
O(7) C(23) 1.291(4) . . yes
O(8) C(25) 1.265(4) . . yes
O(9) N(3) 1.262(4) . . yes
O(10) N(3) 1.282(3) . . yes
O(11) N(3) 1.225(4) . . yes
O(12) N(4) 1.253(4) . . yes
O(13) N(4) 1.287(4) . . yes
O(14) N(4) 1.225(4) . . yes
O(15) N(5) 1.229(4) . . yes
O(16) N(5) 1.258(4) . . yes
O(17) N(5) 1.244(4) . . yes
O(19) C(27) 1.424(5) . . yes
O(20) C(28) 1.439(4) . . yes
O(21) C(29) 1.431(4) . . yes
O(22) C(30) 1.418(6) . . yes
O(23) C(32) 1.586(9) . . yes
O(23) C(33) 1.357(9) . . yes
N(1) C(5) 1.342(4) . . yes
N(1) C(9) 1.340(4) . . yes
N(2) C(18) 1.352(4) . . yes
N(2) C(22) 1.342(4) . . yes
C(1) C(2) 1.491(5) . . yes
C(2) C(3) 1.433(5) . . yes
C(3) C(4) 1.369(4) . . yes
C(4) C(5) 1.486(4) . . yes
C(5) C(6) 1.397(4) . . yes
C(6) C(7) 1.385(5) . . yes
C(7) C(8) 1.378(5) . . yes
C(8) C(9) 1.393(4) . . yes
C(9) C(10) 1.490(4) . . yes
C(10) C(11) 1.383(4) . . yes
C(11) C(12) 1.419(5) . . yes
C(12) C(13) 1.504(5) . . yes
C(14) C(15) 1.506(5) . . yes
C(15) C(16) 1.437(5) . . yes
C(16) C(17) 1.376(4) . . yes
C(17) C(18) 1.490(4) . . yes
C(18) C(19) 1.387(4) . . yes
C(19) C(20) 1.377(5) . . yes
C(20) C(21) 1.395(5) . . yes
C(21) C(22) 1.388(4) . . yes
C(22) C(23) 1.494(4) . . yes
C(23) C(24) 1.383(4) . . yes
C(24) C(25) 1.432(5) . . yes
C(25) C(26) 1.495(5) . . yes
C(31) C(32) 1.45(1) . . yes
C(33) C(34) 1.41(1) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Tm N(1) 2.581(3) . . ?
Tm N(2) 2.584(3) . . ?
O(1) C(32) 3.432(7) . 2_555 ?
O(1) C(31) 3.487(7) . 2_555 ?
O(4) C(31) 3.473(8) . 2_665 ?
O(5) O(23) 3.319(5) . 2_665 ?
O(5) C(31) 3.520(7) . 2_665 ?
O(5) O(17) 3.587(4) . 1_565 ?
O(8) C(32) 3.222(7) . 2_555 ?
O(9) C(34) 3.290(7) . . ?
O(10) C(8) 3.429(4) . 2_666 ?
O(10) O(15) 3.481(4) . . ?
O(11) C(26) 3.191(5) . 2_555 ?
O(11) C(7) 3.217(5) . 2_666 ?
O(11) C(8) 3.238(4) . 2_666 ?
O(11) C(27) 3.271(6) . 1_655 ?
O(11) O(15) 3.425(4) . . ?
O(12) O(22) 3.352(4) . . ?
O(12) C(30) 3.599(6) . . ?
O(13) C(19) 3.316(4) . 2_565 ?
O(14) C(28) 2.980(4) . 1_455 ?
O(14) C(6) 3.300(4) . 2_566 ?
O(14) C(7) 3.310(4) . 2_566 ?
O(14) C(20) 3.495(4) . 2_565 ?
O(14) C(30) 3.544(7) . . ?
O(15) O(18) 3.034(4) . . ?
O(15) C(11) 3.437(5) . 2_666 ?
O(15) C(26) 3.563(5) . 2_555 ?
O(16) O(18) 2.777(4) . . ?
O(16) C(32) 3.351(7) . 2_555 ?
O(16) C(31) 3.412(7) . 2_555 ?
O(16) O(22) 3.470(4) . 1_545 ?
O(16) C(24) 3.473(4) . 2_555 ?
O(16) C(21) 3.510(4) . 2_555 ?
O(17) O(22) 2.737(5) . 1_545 ?
O(17) C(14) 3.422(6) . 1_545 ?
O(17) C(30) 3.459(7) . 1_545 ?
O(17) C(29) 3.459(5) . 1_545 ?
O(17) C(29) 3.598(5) . 2_666 ?
O(18) N(5) 3.281(4) . . ?
O(20) O(23) 2.736(5) . 2_665 ?
O(20) C(34) 3.421(7) . 2_665 ?
O(21) O(22) 2.704(4) . . ?
O(21) C(30) 3.452(6) . . ?
O(22) C(29) 3.165(5) . . ?
O(22) C(20) 3.291(5) . 2_565 ?
O(22) N(5) 3.523(4) . 1_565 ?
O(23) C(28) 3.352(6) . 2_665 ?
O(23) C(15) 3.372(6) . 2_665 ?
N(3) C(26) 3.561(5) . 2_555 ?
N(3) C(8) 3.573(4) . 2_666 ?
N(5) C(13) 3.563(5) . 2_666 ?
C(1) C(29) 3.598(6) . 2_566 ?
C(18) C(19) 3.576(5) . 2_565 ?
C(29) C(29) 3.210(7) . 2_676 ?
