#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302432.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_4302432
loop_
_publ_author_name
'Jean-Pascal Sutter'
'Sébastien Dhers'
'Jean-Pierre Costes'
'Carine Duhayon'
'Laure Vendier'
'Raghunathan Rajamani'
'S. Ramasesha'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       jean-pascal.sutter@lcc-toulouse.fr
_publ_contact_author_name        'J.-P. Sutter'
_publ_section_title
;
Hetero-Metallic {3d-4f-5d} Complexes: Preparation and Magnetic Behavior of
Trinuclear [(LMe2Ni-Ln){W(CN)8}] Compounds (Ln = Gd, Tb, Dy, Ho, Er, Y;
LMe2= Schiff base) and Variable SMM Characteristics for the Tb Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5820
_journal_page_last               5828
_journal_paper_doi               10.1021/ic900003m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C36.5H46.5N12.5Ni1O9Tb1W1,0.5(C3 H7 N O), H2 O'
_chemical_formula_sum            'C38 H52 N13 Ni O10.5 Tb W'
_chemical_formula_weight         1260.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-09-26
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 94.115(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9579(11)
_cell_length_b                   15.0637(9)
_cell_length_c                   25.2840(42)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     5302.4(10)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52783
_diffrn_reflns_theta_full        25.512
_diffrn_reflns_theta_max         26.033
_diffrn_reflns_theta_min         2.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.89
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_description       plate
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.70
_refine_diff_density_min         -1.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.006912
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 3.90 -0.627 3.34 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0522
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0489
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                7293
_reflns_number_total             10360
_reflns_threshold_expression     I>3.0σ(I)
_cod_data_source_file            ic900003m_si_004.cif
_cod_data_source_block           Cmp_3b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5302.5(10)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C38 H52 N13 Ni1 O10.50 Tb1 W1'
_cod_database_code               4302432
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.741897(16) 0.397658(15) 0.332514(9) 0.0266 1.0000 Uani . . . . . .
Ni1 Ni 0.75107(5) 0.69302(5) 0.44897(3) 0.0263 1.0000 Uani . . . . . .
Tb1 Tb 0.70200(2) 0.822283(19) 0.337445(12) 0.0319 1.0000 Uani . . . . . .
C1 C 0.7564(4) 0.5229(4) 0.3745(2) 0.0316 1.0000 Uani . . . . . .
C2 C 0.6599(5) 0.4984(4) 0.2882(3) 0.0398 1.0000 Uani . . . . . .
C3 C 0.8914(4) 0.4369(5) 0.3297(3) 0.0452 1.0000 Uani . . . . . .
C4 C 0.7761(5) 0.3844(6) 0.2507(3) 0.0464 1.0000 Uani . . . . . .
C5 C 0.8008(5) 0.2646(4) 0.3297(3) 0.0415 1.0000 Uani . . . . . .
C6 C 0.6263(5) 0.3206(4) 0.2927(3) 0.0414 1.0000 Uani . . . . . .
C7 C 0.7970(5) 0.3640(5) 0.4121(3) 0.0431 1.0000 Uani . . . . . .
C8 C 0.6199(5) 0.3972(6) 0.3810(3) 0.0524 1.0000 Uani . . . . . .
C9 C 0.8914(7) 0.9735(7) 0.3054(5) 0.0817 1.0000 Uani . . . . . .
C10 C 0.9401(4) 0.8674(4) 0.3723(3) 0.0383 1.0000 Uani . . . . . .
C11 C 1.0343(5) 0.8923(5) 0.3733(3) 0.0478 1.0000 Uani . . . . . .
C12 C 1.1010(5) 0.8536(6) 0.4089(3) 0.0519 1.0000 Uani . . . . . .
C13 C 1.0733(5) 0.7898(6) 0.4427(3) 0.0511 1.0000 Uani . . . . . .
C14 C 0.9774(4) 0.7617(5) 0.4422(3) 0.0407 1.0000 Uani . . . . . .
C15 C 0.9096(4) 0.8018(4) 0.4066(3) 0.0373 1.0000 Uani . . . . . .
C16 C 0.9576(4) 0.6901(5) 0.4787(3) 0.0404 1.0000 Uani . . . . . .
C17 C 0.8813(4) 0.5722(5) 0.5182(3) 0.0387 1.0000 Uani . . . . . .
C18 C 0.7991(5) 0.5584(5) 0.5543(2) 0.0375 1.0000 Uani . . . . . .
C19 C 0.7033(5) 0.5416(4) 0.5220(3) 0.0377 1.0000 Uani . . . . . .
C20 C 0.5713(4) 0.6247(4) 0.4872(3) 0.0336 1.0000 Uani . . . . . .
C21 C 0.5131(4) 0.6857(4) 0.4546(3) 0.0324 1.0000 Uani . . . . . .
C22 C 0.4129(4) 0.6849(4) 0.4618(3) 0.0391 1.0000 Uani . . . . . .
C23 C 0.3500(4) 0.7364(5) 0.4306(3) 0.0420 1.0000 Uani . . . . . .
C24 C 0.3838(4) 0.7930(4) 0.3930(3) 0.0367 1.0000 Uani . . . . . .
C25 C 0.4816(4) 0.7965(4) 0.3866(2) 0.0313 1.0000 Uani . . . . . .
C26 C 0.5470(4) 0.7424(4) 0.4158(2) 0.0282 1.0000 Uani . . . . . .
C27 C 0.4675(5) 0.9289(5) 0.3337(3) 0.0483 1.0000 Uani . . . . . .
C28 C 0.8231(6) 0.4721(6) 0.5843(3) 0.0552 1.0000 Uani . . . . . .
C29 C 0.7926(7) 0.6329(7) 0.5930(3) 0.0606 1.0000 Uani . . . . . .
C30 C 0.6301(5) 0.9454(5) 0.2264(3) 0.0408 1.0000 Uani . . . . . .
C31 C 0.5764(6) 1.0524(7) 0.1605(4) 0.0654 1.0000 Uani . . . . . .
C33 C 0.6639(10) 0.9764(7) 0.4275(4) 0.0459 0.5000 Uani D . . . . .
C34 C 0.628(2) 1.0518(19) 0.4894(10) 0.0967 0.5000 Uani D . . . . .
C36 C 0.8794(5) 0.6957(5) 0.2998(3) 0.0467 1.0000 Uani . . . . . .
C37 C 0.9609(8) 0.7768(8) 0.2342(5) 0.0893 1.0000 Uani . . . . . .
C38 C 1.0484(6) 0.6659(6) 0.2931(5) 0.0675 1.0000 Uani . . . . . .
C39 C 0.9500(15) 0.9583(15) 0.5059(9) 0.0749 0.5000 Uani . . . . . .
C40 C 0.9838(16) 0.8444(15) 0.5744(9) 0.0749 0.5000 Uani . . . . . .
C41 C 1.1085(16) 0.9429(15) 0.5453(9) 0.0749 0.5000 Uani . . . . . .
C321 C 0.6850(11) 1.0981(9) 0.2320(6) 0.0530 0.6000 Uani . . . . . .
C322 C 0.647(2) 1.0903(19) 0.2553(12) 0.0807 0.4000 Uani . . . . . .
C351 C 0.728(3) 1.126(3) 0.429(2) 0.0967 0.2500 Uani D . . . . .
C352 C 0.637(4) 1.1572(16) 0.420(2) 0.0967 0.2500 Uani D . . . . .
N1 N 0.7602(4) 0.5888(3) 0.3963(2) 0.0341 1.0000 Uani . . . . . .
N2 N 0.6180(5) 0.5511(4) 0.2644(3) 0.0560 1.0000 Uani . . . . . .
N3 N 0.9687(5) 0.4572(5) 0.3276(4) 0.0729 1.0000 Uani . . . . . .
N4 N 0.7912(5) 0.3786(7) 0.2071(3) 0.0731 1.0000 Uani . . . . . .
N5 N 0.8299(5) 0.1949(4) 0.3279(3) 0.0590 1.0000 Uani . . . . . .
N6 N 0.5641(5) 0.2843(5) 0.2724(3) 0.0650 1.0000 Uani . . . . . .
N7 N 0.8227(6) 0.3470(5) 0.4547(3) 0.0599 1.0000 Uani . . . . . .
N8 N 0.5573(6) 0.3981(8) 0.4063(3) 0.0867 1.0000 Uani . . . . . .
N9 N 0.8773(4) 0.6530(4) 0.4862(2) 0.0345 1.0000 Uani . . . . . .
N10 N 0.6638(4) 0.6181(3) 0.4908(2) 0.0310 1.0000 Uani . . . . . .
N11 N 0.6278(4) 1.0262(4) 0.2094(2) 0.0385 1.0000 Uani . . . . . .
N12 N 0.6547(9) 1.0637(7) 0.4373(5) 0.0459 0.5000 Uani D . . . . .
N13 N 0.9571(4) 0.7092(4) 0.2749(3) 0.0529 1.0000 Uani . . . . . .
N14 N 1.0119(13) 0.9146(12) 0.5403(7) 0.0749 0.5000 Uani . . . . . .
O1 O 0.8672(3) 0.9002(3) 0.3372(2) 0.0460 1.0000 Uani . . . . . .
O2 O 0.8169(3) 0.7795(3) 0.40220(19) 0.0381 1.0000 Uani . . . . . .
O3 O 0.6385(3) 0.7474(3) 0.40502(17) 0.0323 1.0000 Uani . . . . . .
O4 O 0.5239(3) 0.8530(3) 0.35146(19) 0.0355 1.0000 Uani . . . . . .
O5 O 0.6719(4) 0.9197(4) 0.2681(2) 0.0631 1.0000 Uani . . . . . .
O6 O 0.6899(4) 0.9518(3) 0.38673(19) 0.0459 1.0000 Uani D . . . . .
O7 O 0.8009(4) 0.7337(3) 0.2889(2) 0.0502 1.0000 Uani . . . . . .
O8 O 0.6014(4) 0.7318(4) 0.2830(2) 0.0575 1.0000 Uani . . . . . .
O9 O 0.7391(5) 0.8044(4) 0.5012(3) 0.0618 1.0000 Uani . . . . . .
O10 O 0.8623(10) 0.9417(10) 0.4992(6) 0.0749 0.5000 Uani . . . . . .
O20 O 0.682(2) 0.865(2) 0.6217(11) 0.149(7) 0.5000 Uiso . . . . . .
O21 O 0.596(3) 0.872(3) 0.5513(16) 0.191(7) 0.5000 Uiso . . . . . .
H91 H 0.8371 0.9892 0.2819 0.1170 1.0000 Uiso R . . . . .
H92 H 0.9094 1.0234 0.3275 0.1170 1.0000 Uiso R . . . . .
H93 H 0.9440 0.9571 0.2849 0.1169 1.0000 Uiso R . . . . .
H111 H 1.0529 0.9343 0.3495 0.0561 1.0000 Uiso R . . . . .
H121 H 1.1648 0.8720 0.4101 0.0611 1.0000 Uiso R . . . . .
H131 H 1.1187 0.7634 0.4665 0.0590 1.0000 Uiso R . . . . .
H161 H 1.0111 0.6667 0.4983 0.0491 1.0000 Uiso R . . . . .
H171 H 0.9405 0.5732 0.5405 0.0449 1.0000 Uiso R . . . . .
H172 H 0.8807 0.5225 0.4942 0.0451 1.0000 Uiso R . . . . .
H191 H 0.6567 0.5245 0.5469 0.0450 1.0000 Uiso R . . . . .
H192 H 0.7129 0.4930 0.4975 0.0450 1.0000 Uiso R . . . . .
H201 H 0.5387 0.5864 0.5083 0.0400 1.0000 Uiso R . . . . .
H221 H 0.3896 0.6490 0.4880 0.0469 1.0000 Uiso R . . . . .
H231 H 0.2846 0.7329 0.4349 0.0511 1.0000 Uiso R . . . . .
H241 H 0.3415 0.8286 0.3723 0.0439 1.0000 Uiso R . . . . .
H271 H 0.5061 0.9682 0.3146 0.0729 1.0000 Uiso R . . . . .
H272 H 0.4446 0.9582 0.3641 0.0728 1.0000 Uiso R . . . . .
H273 H 0.4141 0.9090 0.3108 0.0729 1.0000 Uiso R . . . . .
H281 H 0.8857 0.4764 0.6026 0.0810 1.0000 Uiso R . . . . .
H282 H 0.7760 0.4617 0.6097 0.0810 1.0000 Uiso R . . . . .
H283 H 0.8225 0.4232 0.5596 0.0811 1.0000 Uiso R . . . . .
H291 H 0.8536 0.6421 0.6120 0.0899 1.0000 Uiso R . . . . .
H292 H 0.7459 0.6187 0.6174 0.0899 1.0000 Uiso R . . . . .
H293 H 0.7735 0.6856 0.5743 0.0899 1.0000 Uiso R . . . . .
H301 H 0.5987 0.9026 0.2047 0.0482 1.0000 Uiso R . . . . .
H311 H 0.6182 1.0864 0.1397 0.0929 1.0000 Uiso R . . . . .
H312 H 0.5559 1.0007 0.1411 0.0931 1.0000 Uiso R . . . . .
H313 H 0.5217 1.0875 0.1682 0.0929 1.0000 Uiso R . . . . .
H331 H 0.6516 0.9350 0.4534 0.0490 0.5000 Uiso R . . . . .
H341 H 0.5754 1.0897 0.4954 0.1200 0.5000 Uiso R . . . . .
H342 H 0.6809 1.0666 0.5137 0.1199 0.5000 Uiso R . . . . .
H343 H 0.6099 0.9916 0.4947 0.1200 0.5000 Uiso R . . . . .
H361 H 0.8828 0.6543 0.3275 0.0570 1.0000 Uiso R . . . . .
H371 H 0.9921 0.7534 0.2045 0.1340 1.0000 Uiso R . . . . .
H372 H 0.9970 0.8263 0.2489 0.1341 1.0000 Uiso R . . . . .
H373 H 0.8970 0.7961 0.2229 0.1340 1.0000 Uiso R . . . . .
H381 H 1.0774 0.6420 0.2627 0.0980 1.0000 Uiso R . . . . .
H382 H 1.0911 0.7077 0.3111 0.0981 1.0000 Uiso R . . . . .
H383 H 1.0344 0.6184 0.3169 0.0980 1.0000 Uiso R . . . . .
H391 H 0.9757 1.0056 0.4859 0.0963 0.5000 Uiso R . . . . .
H401 H 1.0262 0.8435 0.6059 0.1200 0.5000 Uiso R . . . . .
H402 H 0.9193 0.8560 0.5837 0.1198 0.5000 Uiso R . . . . .
H403 H 0.9861 0.7882 0.5567 0.1201 0.5000 Uiso R . . . . .
H411 H 1.1335 0.9402 0.5816 0.1200 0.5000 Uiso R . . . . .
H412 H 1.1113 1.0028 0.5325 0.1200 0.5000 Uiso R . . . . .
H413 H 1.1450 0.9045 0.5238 0.1200 0.5000 Uiso R . . . . .
H3211 H 0.7183 1.0789 0.2645 0.0608 0.6000 Uiso R . . . . .
H3212 H 0.6439 1.1472 0.2390 0.0608 0.6000 Uiso R . . . . .
H3213 H 0.7309 1.1163 0.2076 0.0608 0.6000 Uiso R . . . . .
H3221 H 0.6436 1.1499 0.2418 0.0940 0.4000 Uiso R . . . . .
H3222 H 0.7095 1.0791 0.2718 0.0940 0.4000 Uiso R . . . . .
H3223 H 0.5997 1.0828 0.2809 0.0940 0.4000 Uiso R . . . . .
H3511 H 0.7346 1.1205 0.3916 0.0959 0.2500 Uiso R . . . . .
H3512 H 0.7034 1.1839 0.4365 0.0959 0.2500 Uiso R . . . . .
H3513 H 0.7888 1.1175 0.4481 0.0959 0.2500 Uiso R . . . . .
H3521 H 0.6563 1.1608 0.3842 0.0959 0.2500 Uiso R . . . . .
H3522 H 0.6757 1.1972 0.4421 0.0959 0.2500 Uiso R . . . . .
H3523 H 0.5708 1.1734 0.4205 0.0959 0.2500 Uiso R . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620
3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 . W1 . C2 . 70.7(2) yes
C1 . W1 . C3 . 74.0(2) yes
C2 . W1 . C3 . 105.4(3) yes
C1 . W1 . C4 . 121.9(3) yes
C2 . W1 . C4 . 73.4(3) yes
C3 . W1 . C4 . 73.5(3) yes
C1 . W1 . C5 . 143.0(2) yes
C2 . W1 . C5 . 144.9(3) yes
C3 . W1 . C5 . 83.3(3) yes
C4 . W1 . C5 . 76.9(3) yes
C1 . W1 . C6 . 137.0(2) yes
C2 . W1 . C6 . 77.7(3) yes
C3 . W1 . C6 . 144.2(3) yes
C4 . W1 . C6 . 73.5(3) yes
C5 . W1 . C6 . 76.2(2) yes
C1 . W1 . C7 . 74.6(2) yes
C2 . W1 . C7 . 141.8(3) yes
C3 . W1 . C7 . 79.4(3) yes
C4 . W1 . C7 . 141.2(3) yes
C5 . W1 . C7 . 72.8(3) yes
C1 . W1 . C8 . 77.0(3) yes
C2 . W1 . C8 . 83.6(3) yes
C3 . W1 . C8 . 144.5(3) yes
C4 . W1 . C8 . 140.9(3) yes
C5 . W1 . C8 . 109.3(3) yes
C6 . W1 . C7 . 120.5(3) yes
C6 . W1 . C8 . 70.9(3) yes
C7 . W1 . C8 . 73.4(3) yes
N1 . Ni1 . N9 . 88.9(2) yes
N1 . Ni1 . N10 . 88.9(2) yes
N9 . Ni1 . N10 . 97.3(2) yes
N1 . Ni1 . O2 . 93.5(2) yes
N9 . Ni1 . O2 . 92.69(19) yes
N10 . Ni1 . O2 . 169.74(18) yes
N1 . Ni1 . O3 . 92.03(19) yes
N9 . Ni1 . O3 . 170.34(19) yes
N10 . Ni1 . O3 . 92.30(18) yes
O2 . Ni1 . O3 . 77.65(16) yes
N1 . Ni1 . O9 . 177.8(2) yes
N9 . Ni1 . O9 . 92.9(2) yes
N10 . Ni1 . O9 . 92.2(2) yes
O2 . Ni1 . O9 . 85.1(2) yes
O3 . Ni1 . O9 . 86.0(2) yes
O1 . Tb1 . O2 . 63.43(15) yes
O1 . Tb1 . O3 . 128.35(15) yes
O2 . Tb1 . O3 . 67.45(15) yes
O1 . Tb1 . O4 . 141.90(15) yes
O2 . Tb1 . O4 . 125.62(16) yes
O3 . Tb1 . O4 . 63.60(14) yes
O1 . Tb1 . O5 . 79.80(19) yes
O2 . Tb1 . O5 . 143.17(19) yes
O3 . Tb1 . O5 . 145.81(17) yes
O4 . Tb1 . O5 . 82.26(17) yes
O1 . Tb1 . O6 . 73.74(18) yes
O2 . Tb1 . O6 . 85.83(18) yes
O3 . Tb1 . O6 . 88.08(16) yes
O4 . Tb1 . O6 . 70.61(16) yes
O5 . Tb1 . O6 . 81.8(2) yes
O1 . Tb1 . O7 . 72.37(18) yes
O2 . Tb1 . O7 . 78.82(19) yes
O3 . Tb1 . O7 . 112.86(17) yes
O4 . Tb1 . O7 . 142.02(17) yes
O5 . Tb1 . O7 . 92.6(2) yes
O1 . Tb1 . O8 . 139.6(2) yes
O2 . Tb1 . O8 . 128.01(18) yes
O3 . Tb1 . O8 . 84.5(2) yes
O4 . Tb1 . O8 . 68.96(17) yes
O5 . Tb1 . O8 . 81.6(2) yes
O6 . Tb1 . O7 . 146.10(18) yes
O6 . Tb1 . O8 . 137.87(17) yes
O7 . Tb1 . O8 . 73.07(19) yes
W1 . C1 . N1 . 177.4(5) yes
W1 . C2 . N2 . 179.0(7) yes
W1 . C3 . N3 . 179.2(8) yes
W1 . C4 . N4 . 177.7(6) yes
W1 . C5 . N5 . 178.8(6) yes
W1 . C6 . N6 . 176.8(7) yes
W1 . C7 . N7 . 177.4(7) yes
W1 . C8 . N8 . 179.0(10) yes
O1 . C9 . H91 . 109.5 no
O1 . C9 . H92 . 109.9 no
H91 . C9 . H92 . 109.3 no
O1 . C9 . H93 . 109.1 no
H91 . C9 . H93 . 109.3 no
H92 . C9 . H93 . 109.7 no
C11 . C10 . C15 . 121.1(6) yes
C11 . C10 . O1 . 124.9(6) yes
C15 . C10 . O1 . 113.9(5) yes
C10 . C11 . C12 . 120.0(6) yes
C10 . C11 . H111 . 119.4 no
C12 . C11 . H111 . 120.6 no
C11 . C12 . C13 . 120.0(6) yes
C11 . C12 . H121 . 119.7 no
C13 . C12 . H121 . 120.3 no
C12 . C13 . C14 . 121.4(7) yes
C12 . C13 . H131 . 119.8 no
C14 . C13 . H131 . 118.8 no
C13 . C14 . C15 . 118.5(6) yes
C13 . C14 . C16 . 116.2(6) yes
C15 . C14 . C16 . 125.3(6) yes
C10 . C15 . C14 . 118.9(6) yes
C10 . C15 . O2 . 117.5(6) yes
C14 . C15 . O2 . 123.6(6) yes
C14 . C16 . N9 . 128.6(6) yes
C14 . C16 . H161 . 115.7 no
N9 . C16 . H161 . 115.7 no
C18 . C17 . N9 . 116.3(5) yes
C18 . C17 . H171 . 107.4 no
N9 . C17 . H171 . 107.9 no
C18 . C17 . H172 . 107.4 no
N9 . C17 . H172 . 107.4 no
H171 . C17 . H172 . 110.4 no
C17 . C18 . C19 . 111.4(5) yes
C17 . C18 . C28 . 105.3(6) yes
C19 . C18 . C28 . 105.9(5) yes
C17 . C18 . C29 . 111.8(6) yes
C19 . C18 . C29 . 112.3(6) yes
C28 . C18 . C29 . 109.6(6) yes
C18 . C19 . N10 . 115.6(5) yes
C18 . C19 . H191 . 107.2 no
N10 . C19 . H191 . 108.0 no
C18 . C19 . H192 . 107.9 no
N10 . C19 . H192 . 108.0 no
H191 . C19 . H192 . 110.0 no
C21 . C20 . N10 . 127.4(6) yes
C21 . C20 . H201 . 116.4 no
N10 . C20 . H201 . 116.3 no
C20 . C21 . C22 . 116.1(6) yes
C20 . C21 . C26 . 125.5(5) yes
C22 . C21 . C26 . 118.4(6) yes
C21 . C22 . C23 . 121.0(6) yes
C21 . C22 . H221 . 119.4 no
C23 . C22 . H221 . 119.5 no
C22 . C23 . C24 . 120.4(6) yes
C22 . C23 . H231 . 119.6 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 119.3(6) yes
C23 . C24 . H241 . 120.6 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 121.9(6) yes
C24 . C25 . O4 . 124.3(6) yes
C26 . C25 . O4 . 113.8(5) yes
C21 . C26 . C25 . 118.9(5) yes
C21 . C26 . O3 . 123.6(5) yes
C25 . C26 . O3 . 117.4(5) yes
O4 . C27 . H271 . 109.4 no
O4 . C27 . H272 . 108.7 no
H271 . C27 . H272 . 110.6 no
O4 . C27 . H273 . 108.9 no
H271 . C27 . H273 . 109.5 no
H272 . C27 . H273 . 109.8 no
C18 . C28 . H281 . 109.9 no
C18 . C28 . H282 . 109.4 no
H281 . C28 . H282 . 109.3 no
C18 . C28 . H283 . 109.6 no
H281 . C28 . H283 . 109.2 no
H282 . C28 . H283 . 109.5 no
C18 . C29 . H291 . 110.1 no
C18 . C29 . H292 . 109.4 no
H291 . C29 . H292 . 109.3 no
C18 . C29 . H293 . 109.4 no
H291 . C29 . H293 . 109.6 no
H292 . C29 . H293 . 109.1 no
N11 . C30 . O5 . 125.5(7) yes
N11 . C30 . H301 . 117.1 no
O5 . C30 . H301 . 117.4 no
N11 . C31 . H311 . 109.4 no
N11 . C31 . H312 . 109.3 no
H311 . C31 . H312 . 109.1 no
N11 . C31 . H313 . 109.4 no
H311 . C31 . H313 . 109.8 no
H312 . C31 . H313 . 109.9 no
N12 . C33 . O6 . 120.6(11) yes
N12 . C33 . H331 . 119.9 no
O6 . C33 . H331 . 119.4 no
N12 . C34 . H341 . 109.3 no
N12 . C34 . H342 . 109.4 no
H341 . C34 . H342 . 109.2 no
N12 . C34 . H343 . 110.1 no
H341 . C34 . H343 . 109.4 no
H342 . C34 . H343 . 109.4 no
N13 . C36 . O7 . 124.6(7) yes
N13 . C36 . H361 . 117.6 no
O7 . C36 . H361 . 117.8 no
N13 . C37 . H371 . 109.8 no
N13 . C37 . H372 . 108.4 no
H371 . C37 . H372 . 109.4 no
N13 . C37 . H373 . 110.2 no
H371 . C37 . H373 . 109.8 no
H372 . C37 . H373 . 109.2 no
N13 . C38 . H381 . 108.7 no
N13 . C38 . H382 . 110.6 no
H381 . C38 . H382 . 109.9 no
N13 . C38 . H383 . 108.3 no
H381 . C38 . H383 . 109.7 no
H382 . C38 . H383 . 109.7 no
N14 . C39 . O10 . 125(2) yes
N14 . C39 . H391 . 117.1 no
O10 . C39 . H391 . 118.4 no
N14 . C40 . H401 . 109.3 no
N14 . C40 . H402 . 108.3 no
H401 . C40 . H402 . 109.5 no
N14 . C40 . H403 . 110.4 no
H401 . C40 . H403 . 109.7 no
H402 . C40 . H403 . 109.7 no
N14 . C41 . H411 . 110.7 no
N14 . C41 . H412 . 108.4 no
H411 . C41 . H412 . 110.0 no
N14 . C41 . H413 . 108.0 no
H411 . C41 . H413 . 110.0 no
H412 . C41 . H413 . 109.8 no
N11 . C321 . H3211 . 109.5 no
N11 . C321 . H3212 . 109.3 no
H3211 . C321 . H3212 . 109.5 no
N11 . C321 . H3213 . 109.7 no
H3211 . C321 . H3213 . 109.5 no
H3212 . C321 . H3213 . 109.5 no
N11 . C321 . H3221 . 111.5 no
H3211 . C321 . H3221 . 105.7 no
H3213 . C321 . H3221 . 110.9 no
N11 . C322 . H3221 . 108.9 no
N11 . C322 . H3222 . 108.9 no
H3221 . C322 . H3222 . 109.5 no
N11 . C322 . H3223 . 110.7 no
H3221 . C322 . H3223 . 109.5 no
H3222 . C322 . H3223 . 109.5 no
N12 . C351 . H3511 . 102.5 no
N12 . C351 . H3512 . 107.9 no
H3511 . C351 . H3512 . 109.5 no
N12 . C351 . H3513 . 117.6 no
H3511 . C351 . H3513 . 109.5 no
H3512 . C351 . H3513 . 109.5 no
N12 . C352 . H3521 . 106.2 no
N12 . C352 . H3522 . 110.3 no
H3521 . C352 . H3522 . 109.5 no
N12 . C352 . H3523 . 111.8 no
H3521 . C352 . H3523 . 109.5 no
H3522 . C352 . H3523 . 109.5 no
Ni1 . N1 . C1 . 166.9(5) yes
C17 . N9 . C16 . 116.6(5) yes
C17 . N9 . Ni1 . 120.1(4) yes
C16 . N9 . Ni1 . 122.9(4) yes
C19 . N10 . C20 . 115.5(5) yes
C19 . N10 . Ni1 . 119.9(4) yes
C20 . N10 . Ni1 . 124.0(4) yes
C322 . N11 . C31 . 122.1(13) yes
C321 . N11 . C31 . 111.2(8) yes
C322 . N11 . C30 . 110.3(13) yes
C321 . N11 . C30 . 125.3(8) yes
C31 . N11 . C30 . 122.9(7) yes
C352 . N12 . C351 . 55(3) yes
C352 . N12 . C34 . 110(3) yes
C351 . N12 . C34 . 118(3) yes
C352 . N12 . C33 . 152(2) yes
C351 . N12 . C33 . 123(2) yes
C34 . N12 . C33 . 94.8(14) yes
C38 . N13 . C37 . 117.2(7) yes
C38 . N13 . C36 . 120.6(7) yes
C37 . N13 . C36 . 121.5(7) yes
C40 . N14 . C41 . 118.0(18) yes
C40 . N14 . C39 . 123.6(18) yes
C41 . N14 . C39 . 118.3(19) yes
Tb1 . O1 . C9 . 127.0(5) yes
Tb1 . O1 . C10 . 116.6(4) yes
C9 . O1 . C10 . 116.5(6) yes
C15 . O2 . Tb1 . 127.7(4) yes
C15 . O2 . Ni1 . 126.3(4) yes
Tb1 . O2 . Ni1 . 105.87(17) yes
C26 . O3 . Ni1 . 125.6(4) yes
C26 . O3 . Tb1 . 127.9(4) yes
Ni1 . O3 . Tb1 . 106.44(17) yes
Tb1 . O4 . C27 . 127.6(4) yes
Tb1 . O4 . C25 . 115.8(3) yes
C27 . O4 . C25 . 115.9(5) yes
C30 . O5 . Tb1 . 154.5(6) yes
Tb1 . O6 . C33 . 140.5(7) yes
Tb1 . O7 . C36 . 133.5(5) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . C1 . 2.167(6) yes
W1 . C2 . 2.164(7) yes
W1 . C3 . 2.175(6) yes
W1 . C4 . 2.165(7) yes
W1 . C5 . 2.169(6) yes
W1 . C6 . 2.175(6) yes
W1 . C7 . 2.163(7) yes
W1 . C8 . 2.168(7) yes
Ni1 . N1 . 2.069(5) yes
Ni1 . N9 . 2.029(5) yes
Ni1 . N10 . 2.016(5) yes
Ni1 . O2 . 2.024(4) yes
Ni1 . O3 . 2.031(4) yes
Ni1 . O9 . 2.150(6) yes
Tb1 . O1 . 2.588(5) yes
Tb1 . O2 . 2.300(4) yes
Tb1 . O3 . 2.279(4) yes
Tb1 . O4 . 2.578(4) yes
Tb1 . O5 . 2.303(5) yes
Tb1 . O6 . 2.328(5) yes
Tb1 . O7 . 2.332(5) yes
Tb1 . O8 . 2.333(5) yes
C1 . N1 . 1.135(8) yes
C2 . N2 . 1.134(9) yes
C3 . N3 . 1.127(10) yes
C4 . N4 . 1.141(10) yes
C5 . N5 . 1.128(9) yes
C6 . N6 . 1.120(9) yes
C7 . N7 . 1.137(10) yes
C8 . N8 . 1.118(11) yes
C9 . O1 . 1.421(9) yes
C9 . H91 . 0.958 no
C9 . H92 . 0.961 no
C9 . H93 . 0.961 no
C10 . C11 . 1.367(9) yes
C10 . C15 . 1.400(9) yes
C10 . O1 . 1.392(8) yes
C11 . C12 . 1.376(10) yes
C11 . H111 . 0.924 no
C12 . C13 . 1.359(11) yes
C12 . H121 . 0.931 no
C13 . C14 . 1.403(9) yes
C13 . H131 . 0.931 no
C14 . C15 . 1.395(9) yes
C14 . C16 . 1.461(9) yes
C15 . O2 . 1.334(7) yes
C16 . N9 . 1.278(8) yes
C16 . H161 . 0.934 no
C17 . C18 . 1.531(9) yes
C17 . N9 . 1.460(8) yes
C17 . H171 . 0.967 no
C17 . H172 . 0.964 no
C18 . C19 . 1.538(9) yes
C18 . C28 . 1.531(10) yes
C18 . C29 . 1.494(12) yes
C19 . N10 . 1.480(8) yes
C19 . H191 . 0.972 no
C19 . H192 . 0.975 no
C20 . C21 . 1.446(9) yes
C20 . N10 . 1.291(8) yes
C20 . H201 . 0.926 no
C21 . C22 . 1.423(9) yes
C21 . C26 . 1.408(9) yes
C22 . C23 . 1.376(10) yes
C22 . H221 . 0.931 no
C23 . C24 . 1.385(10) yes
C23 . H231 . 0.929 no
C24 . C25 . 1.388(8) yes
C24 . H241 . 0.931 no
C25 . C26 . 1.395(8) yes
C25 . O4 . 1.392(8) yes
C26 . O3 . 1.328(7) yes
C27 . O4 . 1.442(8) yes
C27 . H271 . 0.954 no
C27 . H272 . 0.960 no
C27 . H273 . 0.957 no
C28 . H281 . 0.961 no
C28 . H282 . 0.963 no
C28 . H283 . 0.967 no
C29 . H291 . 0.957 no
C29 . H292 . 0.955 no
C29 . H293 . 0.951 no
C30 . N11 . 1.291(8) yes
C30 . O5 . 1.230(9) yes
C30 . H301 . 0.935 no
C31 . N11 . 1.439(9) yes
C31 . H311 . 0.961 no
C31 . H312 . 0.953 no
C31 . H313 . 0.960 no
C33 . N12 . 1.347(9) yes
C33 . O6 . 1.176(8) yes
C33 . H331 . 0.928 no
C34 . N12 . 1.40(2) yes
C34 . H341 . 0.951 no
C34 . H342 . 0.953 no
C34 . H343 . 0.953 no
C36 . N13 . 1.308(9) yes
C36 . O7 . 1.250(9) yes
C36 . H361 . 0.937 no
C37 . N13 . 1.451(11) yes
C37 . H371 . 0.962 no
C37 . H372 . 0.960 no
C37 . H373 . 0.963 no
C38 . N13 . 1.474(10) yes
C38 . H381 . 0.964 no
C38 . H382 . 0.960 no
C38 . H383 . 0.964 no
C39 . H391 2_776 1.176 no
C39 . N14 . 1.35(3) yes
C39 . O10 . 1.25(2) yes
C39 . H391 . 0.960 no
C40 . N14 . 1.44(3) yes
C40 . H401 . 0.958 no
C40 . H402 . 0.962 no
C40 . H403 . 0.959 no
C41 . N14 . 1.41(3) yes
C41 . H411 . 0.960 no
C41 . H412 . 0.961 no
C41 . H413 . 0.963 no
C321 . N11 . 1.439(15) yes
C321 . H3211 . 0.960 no
C321 . H3212 . 0.960 no
C321 . H3213 . 0.960 no
C321 . H3221 . 1.013 no
C322 . N11 . 1.52(3) yes
C322 . H3221 . 0.960 no
C322 . H3222 . 0.960 no
C322 . H3223 . 0.960 no
C351 . N12 . 1.41(4) yes
C351 . H3511 . 0.960 no
C351 . H3512 . 0.960 no
C351 . H3513 . 0.960 no
C352 . N12 . 1.491(10) yes
C352 . H3521 . 0.960 no
C352 . H3522 . 0.960 no
C352 . H3523 . 0.960 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N14 2_776 H391 . N14 . 154 1.39 1.98 3.283(2) yes
N14 2_776 H391 . O10 . 131 1.39 1.90 3.001(2) yes
O10 2_776 H412 . N14 . 141 1.23 1.94 3.001(2) yes
