# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Jean-Pascal Sutter' ; Laboratoire de Chimie de Coordination du CNRS, Universit\'e Paul Sabatier, 205 route de Narbonne, 31077 Toulouse (France). ; ; ? # Footnote for author 1 ; 'Jean-Pierre Costes' ; Laboratoire de Chimie de Coordination du CNRS, Universit\'e Paul Sabatier, 205 route de Narbonne, 31077 Toulouse (France). ; ; ? # Footnote 2 ; 'Sebastien Dhers' ; Laboratoire de Chimie de Coordination du CNRS, Universit\'e Paul Sabatier, 205 route de Narbonne, 31077 Toulouse (France). ; ; ? # Footnote 2 ; 'Carine Duhayon' '' '' 'S. Ramasesha' '' '' _publ_contact_author_name 'Jean-Pascal Sutter' _publ_contact_author_email SUTTER@LCC-TOULOUSE.FR _publ_section_title ; 1-D hydrogen-bonded organization of hexanuclear {3d-4f-5d} complexes: Evidence for slow relaxation of the magnetization of [{LMe2Ni(H2O)Ln(H2O)4.5}2{W(CN)8}2] with Ln = Tb and Dy ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_address ; Laboratoire de Chimie de Coordination du CNRS, Universit\'e Paul Sabatier, 205 route de Narbonne, 31077 Toulouse (France). ; _publ_contact_author_fax '(33) 561 55 30 03' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD # Attachment 'Cmpd2_CCDC655372.cif' data_Cmpd_2 _database_code_depnum_ccdc_archive 'CCDC 655372' _audit_creation_date 07-06-07 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 18.2699(4) _cell_length_b 26.9303(8) _cell_length_c 18.3479(5) _cell_angle_alpha 90 _cell_angle_beta 90.658(2) _cell_angle_gamma 90 _cell_volume 9026.8(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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 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' 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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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' _cell_formula_units_Z 4 _chemical_formula_sum 'C58 H100 N20 Ni2 O34 Tb2 W2' _chemical_formula_moiety 'C58 H70 N20 Ni2 O19 Tb2 W2, 15(H2 O) ' _chemical_compound_source ? _chemical_formula_weight 2424.52 _cell_measurement_reflns_used 8387 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 180 _exptl_crystal_description planar _exptl_crystal_colour greenish-yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.78 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 4.58 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.80 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 84557 _reflns_number_total 24353 _diffrn_reflns_av_R_equivalents 0.083 # Number of reflections with Friedels Law is 24353 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 24162 _diffrn_reflns_theta_min 2.608 _diffrn_reflns_theta_max 29.077 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.495 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -24 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 36 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.54 _refine_diff_density_max 2.17 _refine_ls_number_reflns 10064 _refine_ls_number_restraints 0 _refine_ls_number_parameters 968 #_refine_ls_R_factor_ref 0.0319 _refine_ls_wR_factor_ref 0.0370 _refine_ls_goodness_of_fit_ref 1.1194 #_reflns_number_all 24014 _refine_ls_R_factor_all 0.0903 _refine_ls_wR_factor_all 0.0675 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.8\s(I) _reflns_number_gt 10064 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_gt 0.0370 _refine_ls_shift/su_max 0.001985 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.889 0.199 0.618 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; The H atoms were located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Hydrogen atoms could not be located on water molecules ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Ni1 Ni 0.42948(5) 0.71559(3) 0.37158(5) 0.0154 1.0000 Uani . . . . . . Ni2 Ni 0.99292(5) 0.73004(3) 0.38397(5) 0.0161 1.0000 Uani . . . . . . Tb1 Tb 0.454098(19) 0.843603(13) 0.35952(2) 0.0159 1.0000 Uani . . . . . . Tb2 Tb 0.962619(18) 0.857798(13) 0.35588(2) 0.0157 1.0000 Uani . . . . . . W1 W 0.713271(15) 0.668128(11) 0.358120(17) 0.0142 1.0000 Uani . . . . . . W2 W 0.301725(16) 1.032360(11) 0.355197(18) 0.0174 1.0000 Uani . . . . . . C1 C 0.6001(4) 0.6901(3) 0.3593(4) 0.0202 1.0000 Uani . . . . . . C2 C 0.8237(4) 0.6959(3) 0.3667(4) 0.0182 1.0000 Uani . . . . . . C3 C 0.7048(4) 0.7292(3) 0.2809(4) 0.0236 1.0000 Uani . . . . . . C4 C 0.7087(4) 0.7356(3) 0.4231(4) 0.0235 1.0000 Uani . . . . . . C5 C 0.7450(5) 0.6408(4) 0.2540(6) 0.0390 1.0000 Uani . . . . . . C6 C 0.7843(5) 0.6049(3) 0.3777(6) 0.0327 1.0000 Uani . . . . . . C7 C 0.6946(6) 0.6447(4) 0.4676(5) 0.0376 1.0000 Uani . . . . . . C8 C 0.6464(4) 0.6026(3) 0.3386(5) 0.0268 1.0000 Uani . . . . . . C9 C 0.3453(4) 0.9587(3) 0.3562(4) 0.0237 1.0000 Uani . . . . . . C10 C 0.2840(5) 1.0023(4) 0.4605(6) 0.0382 1.0000 Uani . . . . . . C11 C 0.2042(5) 0.9888(4) 0.3399(6) 0.0382 1.0000 Uani . . . . . . C12 C 0.2123(5) 1.0758(4) 0.3962(6) 0.0382 1.0000 Uani . . . . . . C13 C 0.3023(5) 1.1017(4) 0.2971(6) 0.0382 1.0000 Uani . . . . . . C14 C 0.3549(5) 1.0816(4) 0.4308(6) 0.0382 1.0000 Uani . . . . . . C15 C 0.4155(5) 1.0350(4) 0.3245(6) 0.0382 1.0000 Uani . . . . . . C16 C 0.2974(4) 1.0136(3) 0.2410(5) 0.0262 1.0000 Uani . . . . . . C21 C 0.4076(5) 0.9013(3) 0.1922(5) 0.0339 1.0000 Uani . . . . . . C22 C 0.3814(4) 0.8143(3) 0.1954(4) 0.0186 1.0000 Uani . . . . . . C23 C 0.3457(5) 0.8156(3) 0.1289(5) 0.0276 1.0000 Uani . . . . . . C24 C 0.3218(6) 0.7718(4) 0.0974(5) 0.0394 1.0000 Uani . . . . . . C25 C 0.3340(5) 0.7276(3) 0.1324(5) 0.0305 1.0000 Uani . . . . . . C26 C 0.3691(4) 0.7252(3) 0.2013(4) 0.0189 1.0000 Uani . . . . . . C27 C 0.3921(4) 0.7696(3) 0.2335(4) 0.0173 1.0000 Uani . . . . . . C28 C 0.3808(4) 0.6758(3) 0.2307(4) 0.0219 1.0000 Uani . . . . . . C29 C 0.4200(5) 0.6121(3) 0.3099(5) 0.0251 1.0000 Uani . . . . . . C30 C 0.3964(4) 0.5926(3) 0.3831(5) 0.0263 1.0000 Uani . . . . . . C31 C 0.4407(5) 0.6158(3) 0.4460(5) 0.0267 1.0000 Uani . . . . . . C32 C 0.4145(4) 0.6840(3) 0.5220(5) 0.0251 1.0000 Uani . . . . . . C33 C 0.4051(4) 0.7354(3) 0.5467(5) 0.0220 1.0000 Uani . . . . . . C34 C 0.3820(5) 0.7416(4) 0.6191(5) 0.0294 1.0000 Uani . . . . . . C35 C 0.3755(4) 0.7880(4) 0.6492(5) 0.0318 1.0000 Uani . . . . . . C36 C 0.3928(5) 0.8295(3) 0.6079(5) 0.0300 1.0000 Uani . . . . . . C37 C 0.4151(4) 0.8242(3) 0.5379(4) 0.0201 1.0000 Uani . . . . . . C38 C 0.4223(4) 0.7775(3) 0.5048(4) 0.0169 1.0000 Uani . . . . . . C39 C 0.4358(5) 0.9120(3) 0.5252(5) 0.0324 1.0000 Uani . . . . . . C40 C 0.3147(4) 0.6006(3) 0.3951(6) 0.0323 1.0000 Uani . . . . . . C41 C 0.4140(5) 0.5367(3) 0.3835(6) 0.0397 1.0000 Uani . . . . . . C51 C 1.0171(5) 0.9055(3) 0.1832(5) 0.0301 1.0000 Uani . . . . . . C52 C 1.0362(4) 0.8172(3) 0.1960(4) 0.0200 1.0000 Uani . . . . . . C53 C 1.0706(5) 0.8149(3) 0.1298(4) 0.0289 1.0000 Uani . . . . . . C54 C 1.0933(5) 0.7693(4) 0.1040(5) 0.0354 1.0000 Uani . . . . . . C55 C 1.0801(5) 0.7272(4) 0.1423(5) 0.0318 1.0000 Uani . . . . . . C56 C 1.0466(4) 0.7293(3) 0.2119(4) 0.0204 1.0000 Uani . . . . . . C57 C 1.0244(4) 0.7754(3) 0.2392(4) 0.0184 1.0000 Uani . . . . . . C58 C 1.0347(4) 0.6816(3) 0.2475(5) 0.0238 1.0000 Uani . . . . . . C59 C 1.0038(5) 0.6226(3) 0.3359(5) 0.0291 1.0000 Uani . . . . . . C60 C 1.0333(4) 0.6087(3) 0.4107(5) 0.0275 1.0000 Uani . . . . . . C61 C 0.9901(4) 0.6345(3) 0.4709(5) 0.0283 1.0000 Uani . . . . . . C62 C 1.0102(4) 0.7068(3) 0.5381(5) 0.0257 1.0000 Uani . . . . . . C63 C 1.0177(4) 0.7588(3) 0.5581(4) 0.0194 1.0000 Uani . . . . . . C64 C 1.0410(5) 0.7681(4) 0.6297(5) 0.0314 1.0000 Uani . . . . . . C65 C 1.0497(5) 0.8154(4) 0.6554(5) 0.0311 1.0000 Uani . . . . . . C66 C 1.0383(5) 0.8559(4) 0.6089(5) 0.0302 1.0000 Uani . . . . . . C67 C 1.0160(4) 0.8468(3) 0.5384(4) 0.0236 1.0000 Uani . . . . . . C68 C 1.0033(4) 0.7985(3) 0.5105(4) 0.0198 1.0000 Uani . . . . . . C69 C 1.0065(6) 0.9340(3) 0.5162(5) 0.0385 1.0000 Uani . . . . . . C70 C 1.0216(6) 0.5529(3) 0.4209(6) 0.0418 1.0000 Uani . . . . . . C71 C 1.1147(4) 0.6206(4) 0.4178(6) 0.0368 1.0000 Uani . . . . . . N1 N 0.5405(3) 0.7035(2) 0.3608(4) 0.0229 1.0000 Uani . . . . . . N2 N 0.8818(3) 0.7118(2) 0.3707(4) 0.0213 1.0000 Uani . . . . . . N3 N 0.7009(4) 0.7615(3) 0.2412(5) 0.0397 1.0000 Uani . . . . . . N4 N 0.7041(4) 0.7717(2) 0.4548(4) 0.0262 1.0000 Uani . . . . . . N5 N 0.7584(6) 0.6233(4) 0.1988(5) 0.0603 1.0000 Uani . . . . . . N6 N 0.8224(5) 0.5717(3) 0.3876(7) 0.0568 1.0000 Uani . . . . . . N7 N 0.6867(7) 0.6287(4) 0.5243(5) 0.0630 1.0000 Uani . . . . . . N8 N 0.6117(4) 0.5684(3) 0.3273(5) 0.0405 1.0000 Uani . . . . . . N9 N 0.3754(4) 0.9205(3) 0.3586(4) 0.0245 1.0000 Uani . . . . . . N10 N 0.2787(5) 0.9883(4) 0.5211(6) 0.0519 1.0000 Uani . . . . . . N11 N 0.1521(5) 0.9659(4) 0.3346(5) 0.0519 1.0000 Uani . . . . . . N12 N 0.1647(5) 1.0981(4) 0.4209(5) 0.0519 1.0000 Uani . . . . . . N13 N 0.3019(5) 1.1389(4) 0.2691(5) 0.0519 1.0000 Uani . . . . . . N14 N 0.3832(5) 1.1074(4) 0.4721(5) 0.0519 1.0000 Uani . . . . . . N15 N 0.4755(5) 1.0323(4) 0.3095(5) 0.0519 1.0000 Uani . . . . . . N16 N 0.2957(5) 1.0032(4) 0.1803(6) 0.0519 1.0000 Uani . . . . . . N17 N 0.4055(3) 0.6649(2) 0.2951(3) 0.0193 1.0000 Uani . . . . . . N18 N 0.4274(3) 0.6694(2) 0.4572(4) 0.0211 1.0000 Uani . . . . . . N19 N 1.0153(3) 0.6745(3) 0.3145(4) 0.0238 1.0000 Uani . . . . . . N20 N 0.9991(3) 0.6888(2) 0.4750(4) 0.0203 1.0000 Uani . . . . . . O1 O 0.4057(3) 0.8559(2) 0.2328(3) 0.0246 1.0000 Uani . . . . . . O2 O 0.4250(3) 0.77155(19) 0.2985(3) 0.0179 1.0000 Uani . . . . . . O3 O 0.4456(3) 0.7751(2) 0.4374(3) 0.0206 1.0000 Uani . . . . . . O4 O 0.4330(3) 0.8631(2) 0.4921(3) 0.0232 1.0000 Uani . . . . . . O5 O 0.3227(3) 0.8294(2) 0.3765(3) 0.0218 1.0000 Uani . . . . . . O6 O 0.5207(3) 0.9224(2) 0.3562(4) 0.0351 1.0000 Uani . . . . . . O7 O 0.5718(3) 0.8322(2) 0.4200(3) 0.0255 1.0000 Uani . . . . . . O8 O 0.5535(3) 0.8338(2) 0.2706(3) 0.0308 1.0000 Uani . . . . . . O9 O 0.3119(3) 0.73090(19) 0.3885(3) 0.0194 1.0000 Uani . . . . . . O10 O 1.0111(3) 0.8615(2) 0.2277(3) 0.0238 1.0000 Uani . . . . . . O11 O 0.9928(3) 0.78130(19) 0.3035(3) 0.0176 1.0000 Uani . . . . . . O12 O 0.9795(3) 0.79426(19) 0.4424(3) 0.0172 1.0000 Uani . . . . . . O13 O 1.0042(3) 0.8847(2) 0.4879(3) 0.0261 1.0000 Uani . . . . . . O14 O 1.0986(3) 0.8518(2) 0.3674(3) 0.0249 1.0000 Uani . . . . . . O15 O 1.0096(3) 0.9400(2) 0.3490(3) 0.0254 1.0000 Uani . . . . . . O16 O 0.8779(3) 0.9090(2) 0.2851(3) 0.0281 1.0000 Uani . . . . . . O17 O 0.8537(3) 0.8149(2) 0.3130(4) 0.0312 1.0000 Uani . . . . . . O18 O 0.8666(3) 0.8867(3) 0.4316(3) 0.0390 1.0000 Uani . . . . . . O19 O 1.1090(3) 0.7492(2) 0.3953(3) 0.0221 1.0000 Uani . . . . . . O20 O 0.2940(3) 0.2335(2) 0.2121(3) 0.0238 1.0000 Uani . . . . . . O21 O 0.2952(3) 0.3379(2) 0.2311(3) 0.0305 1.0000 Uani . . . . . . O22 O 0.2861(4) 0.3760(3) 0.0365(4) 0.0408 1.0000 Uani . . . . . . O23 O 0.5865(5) 0.5109(3) 0.1968(4) 0.0558 1.0000 Uani . . . . . . O24 O 0.7651(4) 0.3628(3) 0.1314(5) 0.0485 1.0000 Uani . . . . . . O25 O 0.8384(4) 0.4486(3) 0.1655(7) 0.0783 1.0000 Uani . . . . . . O26 O 0.7090(4) 0.6904(3) 0.0769(4) 0.0475 1.0000 Uani . . . . . . O27 O 0.7154(4) 0.7780(3) 0.0025(4) 0.0424 1.0000 Uani . . . . . . O28 O 0.7063(4) 0.8357(3) 0.1282(4) 0.0439 1.0000 Uani . . . . . . O29 O 0.5851(4) 0.8933(3) 0.1576(5) 0.0573 1.0000 Uani . . . . . . O30 O 0.8377(7) 0.9800(4) 0.0748(6) 0.0935 1.0000 Uani . . . . . . O31 O 0.8327(5) 0.8926(3) 0.1498(4) 0.0578 1.0000 Uani . . . . . . O32 O 0.2060(4) 0.9085(3) 0.1642(4) 0.0451 1.0000 Uani . . . . . . O33 O 0.2812(7) 0.9983(4) 0.0156(5) 0.0861 1.0000 Uani . . . . . . O34 O 0.6064(7) 0.9982(5) 0.2160(7) 0.0370 0.5000 Uani . . . . . . O35 O 0.6791(7) 0.5556(5) 0.1073(8) 0.0404 0.5000 Uani . . . . . . H211 H 0.4327 0.9261 0.2204 0.0510 1.0000 Uiso R . . . . . H212 H 0.4331 0.8962 0.1472 0.0510 1.0000 Uiso R . . . . . H213 H 0.3584 0.9120 0.1818 0.0509 1.0000 Uiso R . . . . . H231 H 0.3383 0.8459 0.1054 0.0332 1.0000 Uiso R . . . . . H241 H 0.2978 0.7723 0.0523 0.0481 1.0000 Uiso R . . . . . H251 H 0.3188 0.6983 0.1105 0.0360 1.0000 Uiso R . . . . . H281 H 0.3695 0.6491 0.2000 0.0270 1.0000 Uiso R . . . . . H291 H 0.4726 0.6076 0.3073 0.0321 1.0000 Uiso R . . . . . H292 H 0.3960 0.5927 0.2721 0.0320 1.0000 Uiso R . . . . . H311 H 0.4928 0.6109 0.4373 0.0330 1.0000 Uiso R . . . . . H312 H 0.4272 0.5986 0.4905 0.0331 1.0000 Uiso R . . . . . H321 H 0.4108 0.6594 0.5575 0.0311 1.0000 Uiso R . . . . . H341 H 0.3709 0.7138 0.6467 0.0352 1.0000 Uiso R . . . . . H351 H 0.3599 0.7916 0.6969 0.0369 1.0000 Uiso R . . . . . H361 H 0.3888 0.8610 0.6281 0.0380 1.0000 Uiso R . . . . . H391 H 0.4501 0.9361 0.4895 0.0491 1.0000 Uiso R . . . . . H392 H 0.4709 0.9120 0.5646 0.0490 1.0000 Uiso R . . . . . H393 H 0.3887 0.9204 0.5437 0.0489 1.0000 Uiso R . . . . . H401 H 0.2996 0.5858 0.4401 0.0500 1.0000 Uiso R . . . . . H402 H 0.3041 0.6354 0.3955 0.0500 1.0000 Uiso R . . . . . H403 H 0.2881 0.5854 0.3556 0.0499 1.0000 Uiso R . . . . . H411 H 0.4018 0.5235 0.4303 0.0590 1.0000 Uiso R . . . . . H412 H 0.4652 0.5325 0.3749 0.0589 1.0000 Uiso R . . . . . H413 H 0.3860 0.5204 0.3461 0.0591 1.0000 Uiso R . . . . . H511 H 0.9964 0.9330 0.2087 0.0441 1.0000 Uiso R . . . . . H512 H 1.0674 0.9120 0.1737 0.0440 1.0000 Uiso R . . . . . H513 H 0.9913 0.9008 0.1379 0.0441 1.0000 Uiso R . . . . . H531 H 1.0784 0.8440 0.1031 0.0338 1.0000 Uiso R . . . . . H541 H 1.1178 0.7673 0.0603 0.0430 1.0000 Uiso R . . . . . H551 H 1.0926 0.6964 0.1229 0.0391 1.0000 Uiso R . . . . . H581 H 1.0419 0.6531 0.2192 0.0281 1.0000 Uiso R . . . . . H591 H 1.0265 0.6012 0.3002 0.0350 1.0000 Uiso R . . . . . H592 H 0.9515 0.6162 0.3363 0.0349 1.0000 Uiso R . . . . . H611 H 1.0046 0.6202 0.5175 0.0340 1.0000 Uiso R . . . . . H612 H 0.9388 0.6278 0.4616 0.0340 1.0000 Uiso R . . . . . H621 H 1.0139 0.6839 0.5761 0.0310 1.0000 Uiso R . . . . . H641 H 1.0506 0.7413 0.6604 0.0361 1.0000 Uiso R . . . . . H651 H 1.0628 0.8210 0.7042 0.0391 1.0000 Uiso R . . . . . H661 H 1.0462 0.8884 0.6254 0.0379 1.0000 Uiso R . . . . . H691 H 0.9958 0.9568 0.4777 0.0590 1.0000 Uiso R . . . . . H692 H 1.0544 0.9405 0.5356 0.0590 1.0000 Uiso R . . . . . H693 H 0.9706 0.9373 0.5539 0.0590 1.0000 Uiso R . . . . . H701 H 1.0365 0.5434 0.4695 0.0641 1.0000 Uiso R . . . . . H702 H 1.0503 0.5351 0.3860 0.0640 1.0000 Uiso R . . . . . H703 H 0.9707 0.5453 0.4135 0.0640 1.0000 Uiso R . . . . . H711 H 1.1317 0.6115 0.4656 0.0570 1.0000 Uiso R . . . . . H712 H 1.1226 0.6553 0.4097 0.0570 1.0000 Uiso R . . . . . H713 H 1.1406 0.6017 0.3818 0.0569 1.0000 Uiso 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 Ni1 0.0133(4) 0.0142(4) 0.0186(5) -0.0008(4) -0.0019(3) 0.0004(3) Ni2 0.0122(4) 0.0163(5) 0.0200(5) -0.0012(4) 0.0010(4) 0.0011(3) Tb1 0.01569(16) 0.01452(16) 0.01750(18) -0.00175(14) -0.00210(13) 0.00096(13) Tb2 0.01396(16) 0.01614(17) 0.01695(18) -0.00021(14) 0.00034(13) 0.00069(13) W1 0.01095(12) 0.01534(14) 0.01631(14) 0.00068(12) 0.00054(10) -0.00001(11) W2 0.01767(14) 0.01189(14) 0.02274(16) 0.00217(12) 0.00214(11) 0.00142(11) C1 0.018(4) 0.015(3) 0.028(4) -0.002(3) 0.000(3) -0.008(3) C2 0.019(4) 0.017(4) 0.018(4) 0.003(3) 0.002(3) 0.004(3) C3 0.023(4) 0.028(4) 0.020(4) 0.003(3) 0.001(3) 0.000(3) C4 0.018(4) 0.035(5) 0.018(4) 0.010(3) 0.003(3) 0.000(3) C5 0.043(5) 0.038(5) 0.037(5) -0.004(4) 0.018(4) -0.017(4) C6 0.026(4) 0.021(4) 0.052(6) 0.001(4) 0.018(4) -0.007(3) C7 0.051(6) 0.037(5) 0.025(5) 0.002(4) 0.005(4) -0.001(4) C8 0.022(4) 0.029(4) 0.030(5) 0.001(4) 0.006(3) 0.005(3) C9 0.0237(8) 0.0237(8) 0.0237(8) -0.0003(8) 0.0000(8) -0.0003(8) C10 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C11 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C12 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C13 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C14 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C15 0.0382(6) 0.0382(6) 0.0382(6) -0.0010(6) -0.0005(6) -0.0010(6) C16 0.0262(6) 0.0262(6) 0.0262(6) -0.0010(6) -0.0007(6) -0.0010(6) C21 0.036(5) 0.034(5) 0.032(5) 0.002(4) -0.003(4) 0.010(4) C22 0.020(3) 0.016(3) 0.020(4) -0.006(3) -0.004(3) 0.005(3) C23 0.030(4) 0.031(5) 0.022(4) 0.003(3) -0.009(3) 0.009(3) C24 0.047(6) 0.049(6) 0.022(5) 0.000(4) -0.014(4) -0.001(5) C25 0.035(5) 0.024(4) 0.033(5) -0.015(4) -0.003(4) -0.005(4) C26 0.017(3) 0.025(4) 0.015(4) -0.001(3) -0.004(3) -0.005(3) C27 0.015(3) 0.028(4) 0.009(3) -0.004(3) 0.001(3) 0.004(3) C28 0.018(3) 0.021(4) 0.027(4) -0.011(3) 0.003(3) -0.006(3) C29 0.030(4) 0.013(4) 0.033(5) -0.011(3) -0.002(3) 0.002(3) C30 0.021(4) 0.016(4) 0.041(5) 0.001(4) 0.002(3) 0.001(3) C31 0.027(4) 0.018(4) 0.034(5) 0.008(3) -0.004(3) -0.002(3) C32 0.020(4) 0.030(4) 0.025(4) 0.008(3) -0.005(3) 0.002(3) C33 0.014(3) 0.025(4) 0.027(4) 0.003(3) -0.006(3) -0.006(3) C34 0.027(4) 0.041(5) 0.020(4) 0.008(4) 0.001(3) -0.001(4) C35 0.023(4) 0.050(6) 0.023(4) 0.003(4) 0.004(3) 0.000(4) C36 0.028(4) 0.033(5) 0.029(5) -0.015(4) 0.001(3) 0.010(4) C37 0.019(3) 0.027(4) 0.014(4) -0.002(3) -0.007(3) 0.004(3) C38 0.012(3) 0.019(4) 0.020(4) -0.001(3) -0.009(3) 0.000(3) C39 0.045(5) 0.025(4) 0.027(5) -0.011(4) 0.003(4) 0.004(4) C40 0.022(4) 0.022(4) 0.053(6) 0.003(4) -0.002(4) -0.009(3) C41 0.039(5) 0.022(4) 0.058(7) 0.006(4) 0.002(5) 0.002(4) C51 0.031(4) 0.031(5) 0.028(5) 0.000(4) 0.002(4) -0.009(4) C52 0.016(3) 0.027(4) 0.017(4) -0.005(3) 0.001(3) -0.003(3) C53 0.037(5) 0.037(5) 0.012(4) 0.001(3) 0.003(3) -0.003(4) C54 0.030(4) 0.049(6) 0.028(5) -0.014(4) 0.009(4) -0.002(4) C55 0.033(4) 0.041(5) 0.021(4) -0.012(4) 0.002(4) 0.007(4) C56 0.013(3) 0.031(4) 0.017(4) -0.005(3) -0.006(3) 0.001(3) C57 0.013(3) 0.028(4) 0.015(4) -0.003(3) -0.003(3) 0.003(3) C58 0.008(3) 0.026(4) 0.038(5) -0.010(3) -0.002(3) 0.005(3) C59 0.025(4) 0.013(4) 0.049(6) -0.007(4) 0.006(4) 0.004(3) C60 0.022(4) 0.020(4) 0.040(5) 0.002(4) -0.003(4) 0.002(3) C61 0.020(4) 0.020(4) 0.044(5) 0.009(4) 0.000(4) 0.000(3) C62 0.020(4) 0.026(4) 0.031(5) 0.007(4) 0.005(3) 0.003(3) C63 0.015(3) 0.031(4) 0.012(4) 0.001(3) -0.002(3) 0.003(3) C64 0.023(4) 0.044(5) 0.027(5) 0.010(4) 0.000(3) -0.001(4) C65 0.031(4) 0.043(5) 0.018(4) 0.000(4) 0.001(3) 0.008(4) C66 0.031(4) 0.036(5) 0.024(4) -0.012(4) -0.002(3) 0.001(4) C67 0.018(3) 0.030(4) 0.023(4) 0.004(3) 0.004(3) 0.003(3) C68 0.015(3) 0.021(4) 0.023(4) 0.006(3) 0.001(3) 0.002(3) C69 0.067(7) 0.021(4) 0.027(5) -0.011(4) -0.010(5) 0.004(4) C70 0.040(5) 0.021(4) 0.064(7) 0.002(5) 0.005(5) 0.002(4) C71 0.018(4) 0.038(5) 0.054(6) 0.012(5) 0.003(4) 0.007(4) N1 0.014(3) 0.021(3) 0.033(4) -0.001(3) -0.001(3) -0.001(2) N2 0.023(3) 0.018(3) 0.023(4) -0.005(3) 0.004(3) 0.007(3) N3 0.038(4) 0.043(5) 0.038(5) 0.007(4) -0.001(4) -0.005(4) N4 0.039(4) 0.018(3) 0.022(4) -0.006(3) -0.005(3) 0.004(3) N5 0.093(8) 0.045(6) 0.044(6) -0.015(4) 0.033(5) -0.020(5) N6 0.029(4) 0.025(4) 0.116(9) 0.009(5) -0.007(5) 0.013(4) N7 0.115(9) 0.044(6) 0.029(5) 0.016(4) 0.025(5) 0.029(6) N8 0.037(4) 0.019(4) 0.065(6) -0.009(4) 0.004(4) -0.008(3) N9 0.0245(8) 0.0245(8) 0.0245(8) -0.0003(8) 0.0000(8) -0.0003(8) N10 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N11 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N12 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N13 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N14 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N15 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N16 0.0519(7) 0.0519(7) 0.0519(7) 0.0004(7) 0.0010(7) 0.0004(7) N17 0.015(3) 0.021(3) 0.023(3) 0.002(3) 0.003(2) 0.000(2) N18 0.016(3) 0.019(3) 0.028(4) 0.000(3) -0.003(2) -0.003(2) N19 0.014(3) 0.025(4) 0.032(4) -0.003(3) 0.003(3) 0.005(3) N20 0.012(3) 0.018(3) 0.031(4) 0.003(3) 0.005(3) 0.001(2) O1 0.032(3) 0.016(3) 0.026(3) 0.001(2) -0.006(2) 0.003(2) O2 0.022(3) 0.016(3) 0.016(3) -0.002(2) -0.003(2) 0.001(2) O3 0.020(3) 0.025(3) 0.017(3) -0.003(2) -0.001(2) 0.003(2) O4 0.029(3) 0.020(3) 0.021(3) -0.008(2) -0.001(2) 0.005(2) O5 0.018(2) 0.021(3) 0.026(3) 0.001(2) -0.003(2) -0.003(2) O6 0.029(3) 0.020(3) 0.056(4) -0.001(3) -0.003(3) -0.003(2) O7 0.017(2) 0.033(3) 0.027(3) 0.003(3) -0.005(2) 0.002(2) O8 0.029(3) 0.036(3) 0.028(3) 0.004(3) 0.002(2) -0.003(3) O9 0.014(2) 0.018(3) 0.027(3) -0.002(2) -0.001(2) 0.000(2) O10 0.032(3) 0.021(3) 0.018(3) 0.002(2) 0.004(2) 0.001(2) O11 0.018(2) 0.016(3) 0.019(3) -0.001(2) 0.004(2) -0.003(2) O12 0.020(2) 0.021(3) 0.011(3) -0.001(2) -0.0002(19) 0.002(2) O13 0.035(3) 0.020(3) 0.024(3) -0.007(2) -0.001(2) 0.002(2) O14 0.014(2) 0.025(3) 0.036(3) -0.003(2) 0.000(2) -0.005(2) O15 0.024(3) 0.017(3) 0.035(3) 0.000(2) -0.003(2) -0.003(2) O16 0.025(3) 0.026(3) 0.032(3) 0.009(3) -0.004(2) -0.002(2) O17 0.020(3) 0.024(3) 0.049(4) -0.001(3) -0.003(3) 0.001(2) O18 0.024(3) 0.070(5) 0.023(3) -0.007(3) 0.004(2) 0.016(3) O19 0.014(2) 0.026(3) 0.026(3) -0.001(2) -0.004(2) -0.001(2) O20 0.018(3) 0.024(3) 0.029(3) 0.009(2) -0.005(2) 0.001(2) O21 0.025(3) 0.038(4) 0.029(3) 0.001(3) 0.000(2) -0.003(3) O22 0.037(4) 0.041(4) 0.043(4) 0.012(3) -0.003(3) -0.001(3) O23 0.071(5) 0.043(4) 0.054(5) -0.015(4) -0.003(4) -0.015(4) O24 0.027(3) 0.037(4) 0.081(6) -0.010(4) 0.015(3) -0.005(3) O25 0.029(4) 0.052(5) 0.154(10) -0.025(6) -0.018(5) 0.002(4) O26 0.041(4) 0.064(5) 0.038(4) 0.004(4) 0.001(3) 0.005(4) O27 0.031(3) 0.063(5) 0.034(4) -0.004(3) -0.001(3) -0.006(3) O28 0.048(4) 0.052(5) 0.031(4) 0.007(3) 0.001(3) -0.006(3) O29 0.048(4) 0.066(6) 0.058(5) 0.018(4) 0.004(4) -0.002(4) O30 0.149(11) 0.045(6) 0.085(8) -0.002(5) -0.041(7) -0.002(6) O31 0.063(5) 0.061(5) 0.049(5) 0.004(4) -0.021(4) -0.010(4) O32 0.056(5) 0.043(4) 0.036(4) 0.002(3) -0.006(3) -0.007(3) O33 0.122(9) 0.075(7) 0.061(6) -0.025(5) -0.024(6) 0.034(6) O34 0.0370(17) 0.0370(17) 0.0370(17) 0.0011(17) 0.0015(17) 0.0011(17) O35 0.0404(17) 0.0404(17) 0.0404(17) 0.0011(17) 0.0016(17) 0.0011(17) _refine_ls_extinction_method None 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 Ni1 . N1 . 2.066(6) yes Ni1 . N17 . 2.003(7) yes Ni1 . N18 . 2.005(7) yes Ni1 . O2 . 2.018(5) yes Ni1 . O3 . 2.026(5) yes Ni1 . O9 . 2.213(5) yes Ni2 . N2 . 2.101(7) yes Ni2 . N19 . 2.011(7) yes Ni2 . N20 . 2.009(7) yes Ni2 . O11 . 2.021(5) yes Ni2 . O12 . 2.051(5) yes Ni2 . O19 . 2.191(5) yes Tb1 . N9 . 2.521(7) yes Tb1 . O1 . 2.500(6) yes Tb1 . O2 . 2.300(5) yes Tb1 . O3 . 2.340(5) yes Tb1 . O4 . 2.523(5) yes Tb1 . O5 . 2.454(5) yes Tb1 . O6 . 2.447(6) yes Tb1 . O7 . 2.428(5) yes Tb1 . O8 . 2.469(6) yes Tb2 . O10 . 2.524(5) yes Tb2 . O11 . 2.342(5) yes Tb2 . O12 . 2.352(5) yes Tb2 . O13 . 2.631(6) yes Tb2 . O14 . 2.497(5) yes Tb2 . O15 . 2.378(5) yes Tb2 . O16 . 2.437(6) yes Tb2 . O17 . 2.424(6) yes Tb2 . O18 . 2.382(6) yes W1 . C1 . 2.152(8) yes W1 . C2 . 2.156(8) yes W1 . C3 . 2.176(8) yes W1 . C4 . 2.176(9) yes W1 . C5 . 2.133(10) yes W1 . C6 . 2.169(9) yes W1 . C7 . 2.137(9) yes W1 . C8 . 2.172(9) yes W2 . C9 . 2.139(8) yes W2 . C10 . 2.122(10) yes W2 . C11 . 2.149(10) yes W2 . C12 . 2.152(10) yes W2 . C13 . 2.151(10) yes W2 . C14 . 2.144(10) yes W2 . C15 . 2.161(10) yes W2 . C16 . 2.157(9) yes C1 . N1 . 1.147(10) yes C2 . N2 . 1.145(10) yes C3 . N3 . 1.136(11) yes C4 . N4 . 1.135(11) yes C5 . N5 . 1.147(13) yes C6 . N6 . 1.147(12) yes C7 . N7 . 1.136(12) yes C8 . N8 . 1.139(11) yes C9 . N9 . 1.166(10) yes C10 . N10 . 1.180(13) yes C11 . N11 . 1.138(13) yes C12 . N12 . 1.155(13) yes C13 . N13 . 1.124(13) yes C14 . N14 . 1.146(13) yes C15 . N15 . 1.136(13) yes C16 . N16 . 1.148(12) yes C21 . O1 . 1.431(10) yes C21 . H211 . 0.959 no C21 . H212 . 0.963 no C21 . H213 . 0.960 no C22 . C23 . 1.378(11) yes C22 . C27 . 1.404(11) yes C22 . O1 . 1.386(9) yes C23 . C24 . 1.381(13) yes C23 . H231 . 0.932 no C24 . C25 . 1.368(13) yes C24 . H241 . 0.933 no C25 . C26 . 1.413(12) yes C25 . H251 . 0.925 no C26 . C27 . 1.396(10) yes C26 . C28 . 1.451(11) yes C27 . O2 . 1.330(8) yes C28 . N17 . 1.294(10) yes C28 . H281 . 0.935 no C29 . C30 . 1.508(12) yes C29 . N17 . 1.470(10) yes C29 . H291 . 0.972 no C29 . H292 . 0.970 no C30 . C31 . 1.536(12) yes C30 . C40 . 1.526(11) yes C30 . C41 . 1.539(12) yes C31 . N18 . 1.479(10) yes C31 . H311 . 0.975 no C31 . H312 . 0.974 no C32 . C33 . 1.466(12) yes C32 . N18 . 1.276(11) yes C32 . H321 . 0.934 no C33 . C34 . 1.409(12) yes C33 . C38 . 1.409(11) yes C34 . C35 . 1.372(13) yes C34 . H341 . 0.928 no C35 . C36 . 1.388(13) yes C35 . H351 . 0.931 no C36 . C37 . 1.359(11) yes C36 . H361 . 0.927 no C37 . C38 . 1.404(10) yes C37 . O4 . 1.384(10) yes C38 . O3 . 1.314(9) yes C39 . O4 . 1.450(10) yes C39 . H391 . 0.960 no C39 . H392 . 0.961 no C39 . H393 . 0.956 no C40 . H401 . 0.961 no C40 . H402 . 0.959 no C40 . H403 . 0.960 no C41 . H411 . 0.958 no C41 . H412 . 0.958 no C41 . H413 . 0.957 no C51 . O10 . 1.442(10) yes C51 . H511 . 0.956 no C51 . H512 . 0.955 no C51 . H513 . 0.959 no C52 . C53 . 1.377(11) yes C52 . C57 . 1.395(11) yes C52 . O10 . 1.406(9) yes C53 . C54 . 1.382(13) yes C53 . H531 . 0.936 no C54 . C55 . 1.357(14) yes C54 . H541 . 0.925 no C55 . C56 . 1.423(11) yes C55 . H551 . 0.932 no C56 . C57 . 1.400(11) yes C56 . C58 . 1.459(12) yes C57 . O11 . 1.329(9) yes C58 . N19 . 1.298(11) yes C58 . H581 . 0.936 no C59 . C60 . 1.515(13) yes C59 . N19 . 1.468(10) yes C59 . H591 . 0.967 no C59 . H592 . 0.972 no C60 . C61 . 1.533(12) yes C60 . C70 . 1.528(12) yes C60 . C71 . 1.526(11) yes C61 . N20 . 1.472(10) yes C61 . H611 . 0.973 no C61 . H612 . 0.968 no C62 . C63 . 1.453(12) yes C62 . N20 . 1.269(11) yes C62 . H621 . 0.933 no C63 . C64 . 1.399(12) yes C63 . C68 . 1.403(11) yes C64 . C65 . 1.368(13) yes C64 . H641 . 0.931 no C65 . C66 . 1.398(13) yes C65 . H651 . 0.935 no C66 . C67 . 1.374(12) yes C66 . H661 . 0.935 no C67 . C68 . 1.417(11) yes C67 . O13 . 1.394(10) yes C68 . O12 . 1.323(9) yes C69 . O13 . 1.426(10) yes C69 . H691 . 0.955 no C69 . H692 . 0.957 no C69 . H693 . 0.961 no C70 . H701 . 0.964 no C70 . H702 . 0.961 no C70 . H703 . 0.961 no C71 . H711 . 0.958 no C71 . H712 . 0.957 no C71 . H713 . 0.961 no 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 N1 . Ni1 . N17 . 91.8(3) yes N1 . Ni1 . N18 . 90.3(3) yes N17 . Ni1 . N18 . 96.9(3) yes N1 . Ni1 . O2 . 94.9(2) yes N17 . Ni1 . O2 . 92.1(2) yes N18 . Ni1 . O2 . 169.4(2) yes N1 . Ni1 . O3 . 92.6(2) yes N17 . Ni1 . O3 . 170.4(2) yes N18 . Ni1 . O3 . 91.6(2) yes O2 . Ni1 . O3 . 79.0(2) yes N1 . Ni1 . O9 . 176.9(2) yes N17 . Ni1 . O9 . 91.2(2) yes N18 . Ni1 . O9 . 88.8(2) yes O2 . Ni1 . O9 . 85.5(2) yes O3 . Ni1 . O9 . 84.5(2) yes N2 . Ni2 . N19 . 87.5(2) yes N2 . Ni2 . N20 . 90.7(3) yes N19 . Ni2 . N20 . 96.1(3) yes N2 . Ni2 . O11 . 94.7(2) yes N19 . Ni2 . O11 . 92.5(2) yes N20 . Ni2 . O11 . 170.0(2) yes N2 . Ni2 . O12 . 97.8(2) yes N19 . Ni2 . O12 . 170.2(2) yes N20 . Ni2 . O12 . 92.1(2) yes O11 . Ni2 . O12 . 78.9(2) yes N2 . Ni2 . O19 . 178.8(2) yes N19 . Ni2 . O19 . 91.8(2) yes N20 . Ni2 . O19 . 90.3(2) yes O11 . Ni2 . O19 . 84.3(2) yes O12 . Ni2 . O19 . 82.7(2) yes N9 . Tb1 . O1 . 71.9(2) yes N9 . Tb1 . O2 . 124.1(2) yes O1 . Tb1 . O2 . 65.30(18) yes N9 . Tb1 . O3 . 127.6(2) yes O1 . Tb1 . O3 . 130.36(18) yes O2 . Tb1 . O3 . 67.40(18) yes N9 . Tb1 . O4 . 75.0(2) yes O1 . Tb1 . O4 . 144.35(18) yes O2 . Tb1 . O4 . 127.49(18) yes O3 . Tb1 . O4 . 64.12(18) yes N9 . Tb1 . O5 . 64.5(2) yes O1 . Tb1 . O5 . 78.63(19) yes O2 . Tb1 . O5 . 73.14(18) yes O3 . Tb1 . O5 . 74.21(18) yes O4 . Tb1 . O5 . 75.49(18) yes N9 . Tb1 . O6 . 64.7(2) yes O1 . Tb1 . O6 . 91.9(2) yes O2 . Tb1 . O6 . 146.3(2) yes O3 . Tb1 . O6 . 137.3(2) yes O4 . Tb1 . O6 . 85.7(2) yes N9 . Tb1 . O7 . 127.5(2) yes O1 . Tb1 . O7 . 138.03(19) yes O2 . Tb1 . O7 . 108.32(19) yes O3 . Tb1 . O7 . 71.71(19) yes O4 . Tb1 . O7 . 74.36(18) yes N9 . Tb1 . O8 . 120.5(2) yes O1 . Tb1 . O8 . 69.80(19) yes O2 . Tb1 . O8 . 75.83(19) yes O3 . Tb1 . O8 . 111.93(19) yes O4 . Tb1 . O8 . 141.37(19) yes O5 . Tb1 . O6 . 128.73(19) yes O5 . Tb1 . O7 . 141.73(19) yes O6 . Tb1 . O7 . 71.5(2) yes O5 . Tb1 . O8 . 142.66(19) yes O6 . Tb1 . O8 . 72.9(2) yes O7 . Tb1 . O8 . 68.52(19) yes O10 . Tb2 . O11 . 64.29(18) yes O10 . Tb2 . O12 . 127.83(17) yes O11 . Tb2 . O12 . 66.87(17) yes O10 . Tb2 . O13 . 138.23(18) yes O11 . Tb2 . O13 . 123.55(18) yes O12 . Tb2 . O13 . 62.92(17) yes O10 . Tb2 . O14 . 73.88(19) yes O11 . Tb2 . O14 . 74.85(18) yes O12 . Tb2 . O14 . 76.88(18) yes O13 . Tb2 . O14 . 70.32(18) yes O10 . Tb2 . O15 . 77.46(19) yes O11 . Tb2 . O15 . 135.26(18) yes O12 . Tb2 . O15 . 131.94(19) yes O13 . Tb2 . O15 . 72.07(19) yes O14 . Tb2 . O15 . 72.87(18) yes O10 . Tb2 . O16 . 73.04(19) yes O11 . Tb2 . O16 . 115.49(19) yes O12 . Tb2 . O16 . 148.09(18) yes O13 . Tb2 . O16 . 120.65(19) yes O14 . Tb2 . O16 . 135.03(19) yes O10 . Tb2 . O17 . 90.7(2) yes O11 . Tb2 . O17 . 69.13(18) yes O12 . Tb2 . O17 . 88.43(19) yes O13 . Tb2 . O17 . 131.1(2) yes O14 . Tb2 . O17 . 143.98(19) yes O10 . Tb2 . O18 . 143.0(2) yes O11 . Tb2 . O18 . 134.9(2) yes O12 . Tb2 . O18 . 86.3(2) yes O13 . Tb2 . O18 . 65.1(2) yes O14 . Tb2 . O18 . 135.3(2) yes O15 . Tb2 . O16 . 70.88(19) yes O15 . Tb2 . O17 . 136.2(2) yes O16 . Tb2 . O17 . 65.4(2) yes O15 . Tb2 . O18 . 89.7(2) yes O16 . Tb2 . O18 . 70.0(2) yes O17 . Tb2 . O18 . 74.8(2) yes C1 . W1 . C2 . 143.4(3) yes C1 . W1 . C3 . 74.8(3) yes C2 . W1 . C3 . 81.1(3) yes C1 . W1 . C4 . 73.8(3) yes C2 . W1 . C4 . 73.3(3) yes C3 . W1 . C4 . 73.9(3) yes C1 . W1 . C5 . 112.0(4) yes C2 . W1 . C5 . 85.5(3) yes C3 . W1 . C5 . 72.3(4) yes C4 . W1 . C5 . 142.3(3) yes C1 . W1 . C6 . 142.0(3) yes C2 . W1 . C6 . 72.7(3) yes C3 . W1 . C6 . 137.7(3) yes C4 . W1 . C6 . 126.3(3) yes C5 . W1 . C6 . 73.1(4) yes C1 . W1 . C7 . 84.7(4) yes C2 . W1 . C7 . 101.1(3) yes C3 . W1 . C7 . 145.6(3) yes C4 . W1 . C7 . 74.0(3) yes C5 . W1 . C7 . 142.0(4) yes C1 . W1 . C8 . 71.7(3) yes C2 . W1 . C8 . 144.8(3) yes C3 . W1 . C8 . 118.1(3) yes C4 . W1 . C8 . 138.0(3) yes C5 . W1 . C8 . 74.4(3) yes C6 . W1 . C7 . 73.4(4) yes C6 . W1 . C8 . 73.9(3) yes C7 . W1 . C8 . 79.6(4) yes C9 . W2 . C10 . 72.5(3) yes C9 . W2 . C11 . 78.7(3) yes C10 . W2 . C11 . 77.0(4) yes C9 . W2 . C12 . 141.8(3) yes C10 . W2 . C12 . 76.4(4) yes C11 . W2 . C12 . 73.1(4) yes C9 . W2 . C13 . 143.7(3) yes C10 . W2 . C13 . 141.6(4) yes C11 . W2 . C13 . 114.7(4) yes C12 . W2 . C13 . 73.1(4) yes C9 . W2 . C14 . 113.8(3) yes C10 . W2 . C14 . 73.8(4) yes C11 . W2 . C14 . 142.3(4) yes C12 . W2 . C14 . 77.1(4) yes C13 . W2 . C14 . 77.2(4) yes C9 . W2 . C15 . 71.0(3) yes C10 . W2 . C15 . 114.0(4) yes C11 . W2 . C15 . 141.6(4) yes C12 . W2 . C15 . 144.0(4) yes C13 . W2 . C15 . 80.3(4) yes C9 . W2 . C16 . 78.5(3) yes C10 . W2 . C16 . 142.2(4) yes C11 . W2 . C16 . 74.0(3) yes C12 . W2 . C16 . 116.6(4) yes C13 . W2 . C16 . 73.9(4) yes C14 . W2 . C15 . 73.6(4) yes C14 . W2 . C16 . 141.7(4) yes C15 . W2 . C16 . 77.2(3) yes W1 . C1 . N1 . 177.6(6) yes W1 . C2 . N2 . 178.2(6) yes W1 . C3 . N3 . 179.1(8) yes W1 . C4 . N4 . 176.9(7) yes W1 . C5 . N5 . 175.0(8) yes W1 . C6 . N6 . 179.2(8) yes W1 . C7 . N7 . 174.6(9) yes W1 . C8 . N8 . 179.0(8) yes W2 . C9 . N9 . 173.6(7) yes W2 . C10 . N10 . 174.3(9) yes W2 . C11 . N11 . 177.4(9) yes W2 . C12 . N12 . 177.3(9) yes W2 . C13 . N13 . 177.3(10) yes W2 . C14 . N14 . 178.8(9) yes W2 . C15 . N15 . 174.3(9) yes W2 . C16 . N16 . 179.3(8) yes O1 . C21 . H211 . 109.2 no O1 . C21 . H212 . 109.8 no H211 . C21 . H212 . 109.1 no O1 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.8 no H212 . C21 . H213 . 109.4 no C23 . C22 . C27 . 121.7(7) yes C23 . C22 . O1 . 124.4(7) yes C27 . C22 . O1 . 113.9(6) yes C22 . C23 . C24 . 119.5(8) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 120.8 no C23 . C24 . C25 . 119.9(8) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 120.0 no C24 . C25 . C26 . 121.8(8) yes C24 . C25 . H251 . 119.5 no C26 . C25 . H251 . 118.7 no C25 . C26 . C27 . 118.2(7) yes C25 . C26 . C28 . 115.9(7) yes C27 . C26 . C28 . 125.8(7) yes C22 . C27 . C26 . 118.9(7) yes C22 . C27 . O2 . 118.2(7) yes C26 . C27 . O2 . 122.9(7) yes C26 . C28 . N17 . 126.7(7) yes C26 . C28 . H281 . 116.8 no N17 . C28 . H281 . 116.6 no C30 . C29 . N17 . 116.7(6) yes C30 . C29 . H291 . 107.0 no N17 . C29 . H291 . 106.7 no C30 . C29 . H292 . 108.5 no N17 . C29 . H292 . 108.1 no H291 . C29 . H292 . 109.6 no C29 . C30 . C31 . 112.0(7) yes C29 . C30 . C40 . 111.6(7) yes C31 . C30 . C40 . 110.0(7) yes C29 . C30 . C41 . 106.5(7) yes C31 . C30 . C41 . 106.6(7) yes C40 . C30 . C41 . 110.0(7) yes C30 . C31 . N18 . 114.6(6) yes C30 . C31 . H311 . 109.2 no N18 . C31 . H311 . 108.4 no C30 . C31 . H312 . 107.5 no N18 . C31 . H312 . 107.7 no H311 . C31 . H312 . 109.3 no C33 . C32 . N18 . 127.1(8) yes C33 . C32 . H321 . 116.5 no N18 . C32 . H321 . 116.5 no C32 . C33 . C34 . 116.2(7) yes C32 . C33 . C38 . 124.3(7) yes C34 . C33 . C38 . 119.3(8) yes C33 . C34 . C35 . 121.0(8) yes C33 . C34 . H341 . 119.2 no C35 . C34 . H341 . 119.8 no C34 . C35 . C36 . 119.6(8) yes C34 . C35 . H351 . 120.1 no C36 . C35 . H351 . 120.3 no C35 . C36 . C37 . 120.2(8) yes C35 . C36 . H361 . 119.8 no C37 . C36 . H361 . 120.0 no C36 . C37 . C38 . 122.2(8) yes C36 . C37 . O4 . 124.7(7) yes C38 . C37 . O4 . 113.1(7) yes C33 . C38 . C37 . 117.6(7) yes C33 . C38 . O3 . 123.4(7) yes C37 . C38 . O3 . 119.0(7) yes O4 . C39 . H391 . 109.7 no O4 . C39 . H392 . 109.5 no H391 . C39 . H392 . 109.3 no O4 . C39 . H393 . 109.6 no H391 . C39 . H393 . 109.6 no H392 . C39 . H393 . 109.2 no C30 . C40 . H401 . 110.9 no C30 . C40 . H402 . 109.7 no H401 . C40 . H402 . 109.8 no C30 . C40 . H403 . 108.6 no H401 . C40 . H403 . 108.9 no H402 . C40 . H403 . 108.9 no C30 . C41 . H411 . 108.5 no C30 . C41 . H412 . 108.6 no H411 . C41 . H412 . 110.0 no C30 . C41 . H413 . 109.6 no H411 . C41 . H413 . 110.1 no H412 . C41 . H413 . 110.0 no O10 . C51 . H511 . 109.0 no O10 . C51 . H512 . 109.5 no H511 . C51 . H512 . 109.5 no O10 . C51 . H513 . 110.0 no H511 . C51 . H513 . 109.5 no H512 . C51 . H513 . 109.3 no C53 . C52 . C57 . 122.7(8) yes C53 . C52 . O10 . 123.9(7) yes C57 . C52 . O10 . 113.4(6) yes C52 . C53 . C54 . 118.9(8) yes C52 . C53 . H531 . 119.9 no C54 . C53 . H531 . 121.2 no C53 . C54 . C55 . 120.8(8) yes C53 . C54 . H541 . 120.0 no C55 . C54 . H541 . 119.3 no C54 . C55 . C56 . 120.7(8) yes C54 . C55 . H551 . 120.0 no C56 . C55 . H551 . 119.3 no C55 . C56 . C57 . 119.2(8) yes C55 . C56 . C58 . 115.6(7) yes C57 . C56 . C58 . 125.1(7) yes C56 . C57 . C52 . 117.7(7) yes C56 . C57 . O11 . 123.7(7) yes C52 . C57 . O11 . 118.6(7) yes C56 . C58 . N19 . 126.7(7) yes C56 . C58 . H581 . 116.8 no N19 . C58 . H581 . 116.4 no C60 . C59 . N19 . 115.3(7) yes C60 . C59 . H591 . 108.4 no N19 . C59 . H591 . 108.7 no C60 . C59 . H592 . 106.8 no N19 . C59 . H592 . 108.2 no H591 . C59 . H592 . 109.3 no C59 . C60 . C61 . 111.1(7) yes C59 . C60 . C70 . 107.8(8) yes C61 . C60 . C70 . 106.5(7) yes C59 . C60 . C71 . 111.2(7) yes C61 . C60 . C71 . 110.6(7) yes C70 . C60 . C71 . 109.4(7) yes C60 . C61 . N20 . 115.5(7) yes C60 . C61 . H611 . 108.4 no N20 . C61 . H611 . 108.6 no C60 . C61 . H612 . 107.2 no N20 . C61 . H612 . 107.6 no H611 . C61 . H612 . 109.5 no C63 . C62 . N20 . 127.8(8) yes C63 . C62 . H621 . 116.3 no N20 . C62 . H621 . 115.9 no C62 . C63 . C64 . 115.9(7) yes C62 . C63 . C68 . 124.1(7) yes C64 . C63 . C68 . 120.0(8) yes C63 . C64 . C65 . 121.6(8) yes C63 . C64 . H641 . 118.9 no C65 . C64 . H641 . 119.5 no C64 . C65 . C66 . 120.0(8) yes C64 . C65 . H651 . 120.5 no C66 . C65 . H651 . 119.5 no C65 . C66 . C67 . 118.4(8) yes C65 . C66 . H661 . 120.7 no C67 . C66 . H661 . 120.9 no C66 . C67 . C68 . 123.3(8) yes C66 . C67 . O13 . 122.6(8) yes C68 . C67 . O13 . 114.1(7) yes C67 . C68 . C63 . 116.5(7) yes C67 . C68 . O12 . 118.1(7) yes C63 . C68 . O12 . 125.4(7) yes O13 . C69 . H691 . 108.9 no O13 . C69 . H692 . 109.1 no H691 . C69 . H692 . 109.6 no O13 . C69 . H693 . 109.3 no H691 . C69 . H693 . 109.7 no H692 . C69 . H693 . 110.2 no C60 . C70 . H701 . 109.8 no C60 . C70 . H702 . 109.3 no H701 . C70 . H702 . 109.6 no C60 . C70 . H703 . 109.1 no H701 . C70 . H703 . 109.7 no H702 . C70 . H703 . 109.5 no C60 . C71 . H711 . 109.3 no C60 . C71 . H712 . 109.9 no H711 . C71 . H712 . 110.1 no C60 . C71 . H713 . 108.5 no H711 . C71 . H713 . 109.7 no H712 . C71 . H713 . 109.5 no Ni1 . N1 . C1 . 169.9(6) yes Ni2 . N2 . C2 . 171.0(6) yes Tb1 . N9 . C9 . 173.0(6) yes C29 . N17 . C28 . 116.7(7) yes C29 . N17 . Ni1 . 119.5(5) yes C28 . N17 . Ni1 . 123.7(5) yes C31 . N18 . C32 . 117.6(7) yes C31 . N18 . Ni1 . 119.4(5) yes C32 . N18 . Ni1 . 123.0(6) yes C59 . N19 . C58 . 115.8(7) yes C59 . N19 . Ni2 . 120.5(5) yes C58 . N19 . Ni2 . 123.4(6) yes C61 . N20 . C62 . 116.4(7) yes C61 . N20 . Ni2 . 120.0(6) yes C62 . N20 . Ni2 . 123.6(6) yes C21 . O1 . Tb1 . 125.9(5) yes C21 . O1 . C22 . 116.3(6) yes Tb1 . O1 . C22 . 117.4(4) yes C27 . O2 . Tb1 . 124.7(5) yes C27 . O2 . Ni1 . 125.5(5) yes Tb1 . O2 . Ni1 . 107.4(2) yes C38 . O3 . Tb1 . 124.1(5) yes C38 . O3 . Ni1 . 123.6(5) yes Tb1 . O3 . Ni1 . 105.6(2) yes C39 . O4 . Tb1 . 126.0(5) yes C39 . O4 . C37 . 116.2(6) yes Tb1 . O4 . C37 . 117.8(4) yes Tb2 . O10 . C51 . 126.1(5) yes Tb2 . O10 . C52 . 118.1(4) yes C51 . O10 . C52 . 115.8(6) yes C57 . O11 . Tb2 . 125.2(5) yes C57 . O11 . Ni2 . 124.8(5) yes Tb2 . O11 . Ni2 . 107.4(2) yes C68 . O12 . Tb2 . 127.9(5) yes C68 . O12 . Ni2 . 121.8(5) yes Tb2 . O12 . Ni2 . 106.0(2) yes Tb2 . O13 . C69 . 126.8(5) yes Tb2 . O13 . C67 . 116.9(5) yes C69 . O13 . C67 . 115.8(7) yes