# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- cif_cmpd1.cif' _audit_creation_date 12-06-25 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'jps241111 in P-1' _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # 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_contact_author_name 'Jean-Pascal Sutter' _publ_contact_author_address ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; _publ_contact_author_phone '(33) 5 61 33 31 57' _publ_contact_author_fax '(33) 5 61 55 30 03' _publ_contact_author_email sutter@lcc-toulouse.fr _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_section_title # Title of paper - generally just the systematic or trivial name ; [{Mo(NCS)6}2{MLN4}3] (M = CoII, NiII): First Ferrimagnets Based on Thiocyanato-Bridges ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote # Author 1 # Author 2 # Author 2 # Author 2 # Author 2 'Maliheh Mousavi' ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; ; ? # Footnote for author 1 ; V.Bereau ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; 'Carine Duhayon' ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; 'Philippe Guionneau' ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; 'Jean-Pascal Sutter' ; CNRS, LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, BP 44099, F-31077 Toulouse Cedex 4, France ; ; ? # Footnote 2 ; _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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: ; Refinement is done with no allowance at all for the H atoms at disordered carbon sites. Other H atoms were refined with riding constraints Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # data_1 _database_code_depnum_ccdc_archive 'CCDC 881664' #TrackingRef '- cif_cmpd1.cif' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; We used different types of restraints for the two disordered macrocyclic ligands bonded to Ni1 and Ni2 : -Geometrical restraints, using the command SAME. This commands permits to have equivalent geometries for the two disordered parts of the two ligands -Restraints on anisotropic displacement parameters, using the commands SIMU and DELU. They take into account that atoms, which are bound to one another, move similarly, both in direction and amount -U(IJ) used to ensure that the vibration parameters of adjacent atoms are similar ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 12.5105(10) _cell_length_b 16.4003(13) _cell_length_c 19.0260(15) _cell_angle_alpha 90.419(4) _cell_angle_beta 94.755(4) _cell_angle_gamma 108.682(4) _cell_volume 3682.9(5) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 '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' 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' _cell_formula_units_Z 2 _chemical_formula_sum 'C57 H66 Mo2 N24 Ni3 S12' _chemical_formula_moiety 'C57 H66 Mo2 N24 Ni3 S12' _chemical_compound_source ? _chemical_formula_weight 1840.12 _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.480 # Sheldrick geometric approximatio 0.86 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _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 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 100 _diffrn_reflns_number 56578 _reflns_number_total 17765 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17765 # Theoretical number of reflections is about 36949 _diffrn_reflns_theta_min 1.075 _diffrn_reflns_theta_max 28.402 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.278 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.86 _refine_diff_density_max 1.70 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 10632 _refine_ls_number_restraints 1039 _refine_ls_number_parameters 1244 _oxford_refine_ls_R_factor_ref 0.0666 _refine_ls_wR_factor_ref 0.0669 _refine_ls_goodness_of_fit_ref 1.1302 _refine_ls_shift/su_max 0.0035301 _refine_ls_shift/su_mean 0.0001490 # The values computed from all data _oxford_reflns_number_all 17718 _refine_ls_R_factor_all 0.1254 _refine_ls_wR_factor_all 0.1120 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10632 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_gt 0.0669 # 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: 0.627 0.613 0.370 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 Mo1 Mo 0.26256(6) 0.23940(4) 0.50597(4) 0.0154 1.0000 Uani . . . . . . Mo2 Mo 0.74175(6) 0.25431(5) 1.01302(4) 0.0212 1.0000 Uani . . . . . . Ni1 Ni -0.24198(8) 0.22961(7) 0.50131(6) 0.0240 1.0000 Uani . . . . . . Ni2 Ni 0.34702(10) 0.34480(7) 0.82878(6) 0.0268 1.0000 Uani . . . . . . Ni3 Ni 1.16857(10) 0.17113(8) 1.17058(7) 0.0275 1.0000 Uani . . . . . . C1 C 0.0206(7) 0.2607(5) 0.4463(5) 0.0218 1.0000 Uani . . . . . . C2 C 0.2873(7) 0.3533(6) 0.6504(5) 0.0244 1.0000 Uani . . . . . . C3 C 0.2498(7) 0.1289(5) 0.3610(4) 0.0233 1.0000 Uani . . . . . . C4 C 0.5054(7) 0.2166(5) 0.5603(5) 0.0252 1.0000 Uani . . . . . . C5 C 0.3729(8) 0.4205(6) 0.4312(5) 0.0298 1.0000 Uani . . . . . . C6 C 0.1341(6) 0.0533(5) 0.5731(4) 0.0182 1.0000 Uani . . . . . . C7 C 0.4905(8) 0.2705(6) 0.9710(5) 0.0287 1.0000 Uani . . . . . . C8 C 1.0011(8) 0.2453(6) 1.0389(5) 0.0237 1.0000 Uani . . . . . . C9 C 0.8468(8) 0.4426(5) 0.9480(5) 0.0236 1.0000 Uani . . . . . . C10 C 0.7204(8) 0.1712(6) 0.8558(5) 0.0260 1.0000 Uani . . . . . . C11 C 0.6206(8) 0.0676(6) 1.0771(5) 0.0302 1.0000 Uani . . . . . . C12 C 0.7679(8) 0.3375(6) 1.1718(5) 0.0277 1.0000 Uani . . . . . . C43 C 0.9491(8) 0.0635(6) 1.1489(4) 0.0298 1.0000 Uani . . . . . . C44 C 0.9436(7) 0.1359(6) 1.1925(4) 0.0289 1.0000 Uani . . . . . . C45 C 1.0468(11) 0.2712(9) 1.2480(8) 0.0670 1.0000 Uani . . . . . . C46 C 1.1593(11) 0.3311(9) 1.2702(9) 0.0775 1.0000 Uani . . . . . . C47 C 1.2623(14) 0.3378(9) 1.2457(11) 0.0955 1.0000 Uani . . . . . . C50 C 1.3866(7) 0.1513(6) 1.1219(5) 0.0429 1.0000 Uani D . . . . . C51 C 1.2091(8) 0.0457(5) 1.0930(4) 0.0301 1.0000 Uani . . . . . . C52 C 1.0851(7) 0.0170(5) 1.0987(4) 0.0252 1.0000 Uani . . . . . . C53 C 1.0019(9) -0.0557(6) 1.0700(5) 0.0384 1.0000 Uani . . . . . . C54 C 0.8910(8) -0.0670(6) 1.0797(5) 0.0364 1.0000 Uani . . . . . . C55 C 0.8614(8) -0.0070(6) 1.1195(5) 0.0367 1.0000 Uani . . . . . . C56 C 0.8349(8) 0.1406(7) 1.2162(6) 0.0398 1.0000 Uani . . . . . . C57 C 1.2650(9) -0.0041(7) 1.0506(5) 0.0378 1.0000 Uani . . . . . . N1 N 0.1032(6) 0.2536(4) 0.4733(4) 0.0195 1.0000 Uani . . . . . . N2 N 0.2735(6) 0.3078(5) 0.6011(4) 0.0238 1.0000 Uani . . . . . . N3 N 0.2552(6) 0.1713(5) 0.4120(4) 0.0236 1.0000 Uani . . . . . . N4 N 0.4210(6) 0.2261(4) 0.5374(4) 0.0199 1.0000 Uani . . . . . . N5 N 0.3380(6) 0.3541(4) 0.4585(4) 0.0228 1.0000 Uani . . . . . . N6 N 0.1843(5) 0.1230(4) 0.5533(3) 0.0185 1.0000 Uani . . . . . . N7 N 0.5783(7) 0.2649(5) 0.9873(4) 0.0286 1.0000 Uani . . . . . . N8 N 0.9039(7) 0.2416(5) 1.0348(4) 0.0274 1.0000 Uani . . . . . . N9 N 0.8109(7) 0.3756(5) 0.9728(4) 0.0269 1.0000 Uani . . . . . . N10 N 0.7314(7) 0.2017(5) 0.9127(4) 0.0268 1.0000 Uani . . . . . . N11 N 0.6646(6) 0.1331(5) 1.0538(4) 0.0247 1.0000 Uani . . . . . . N12 N 0.7535(7) 0.3087(5) 1.1143(4) 0.0255 1.0000 Uani . . . . . . N21 N 1.0570(6) 0.0732(4) 1.1365(4) 0.0262 1.0000 Uani . . . . . . N22 N 1.0415(6) 0.1956(5) 1.2081(4) 0.0319 1.0000 Uani . . . . . . N23 N 1.2883(6) 0.2731(5) 1.2084(5) 0.0443 1.0000 Uani D . . . . . N24 N 1.2633(6) 0.1177(5) 1.1252(4) 0.0273 1.0000 Uani D . . . . . S1 S -0.09568(18) 0.27272(15) 0.40808(12) 0.0283 1.0000 Uani . . . . . . S2 S 0.3020(2) 0.42051(14) 0.71753(12) 0.0300 1.0000 Uani . . . . . . S3 S 0.2499(2) 0.07111(15) 0.29288(12) 0.0359 1.0000 Uani . . . . . . S4 S 0.6193(2) 0.19718(18) 0.59502(14) 0.0383 1.0000 Uani . . . . . . S5 S 0.4252(3) 0.51061(19) 0.39273(19) 0.0662 1.0000 Uani . . . . . . S6 S 0.06768(19) -0.03951(13) 0.60181(12) 0.0278 1.0000 Uani . . . . . . S7 S 0.3633(2) 0.27630(17) 0.94984(14) 0.0368 1.0000 Uani . . . . . . S8 S 1.1337(2) 0.25170(17) 1.04014(14) 0.0349 1.0000 Uani . . . . . . S9 S 0.9010(3) 0.53473(19) 0.91310(19) 0.0568 1.0000 Uani . . . . . . S10 S 0.7064(2) 0.1241(2) 0.77834(14) 0.0405 1.0000 Uani . . . . . . S11 S 0.5556(2) -0.02547(19) 1.10919(18) 0.0483 1.0000 Uani . . . . . . S12 S 0.7846(3) 0.3767(3) 1.25098(16) 0.0603 1.0000 Uani . . . . . . C32 C 0.4688(9) 0.5041(12) 0.9067(7) 0.0478 0.5000 Uani D U . . . . C320 C 0.5121(9) 0.5037(11) 0.8976(8) 0.0478 0.5000 Uani D U . . . . C31 C 0.3732(11) 0.5295(7) 0.8960(9) 0.0451 0.5000 Uani D U . . . . C310 C 0.4211(10) 0.5335(7) 0.8924(9) 0.0450 0.5000 Uani D U . . . . C30 C 0.2455(8) 0.4692(8) 0.9075(9) 0.0375 0.5000 Uani D U . . . . C300 C 0.2988(9) 0.4823(9) 0.9162(8) 0.0373 0.5000 Uani D U . . . . N18 N 0.2129(7) 0.3791(8) 0.8676(11) 0.0316 0.5000 Uani D U . . . . N180 N 0.2441(7) 0.3949(8) 0.8747(10) 0.0316 0.5000 Uani D U . . . . C29 C 0.1153(6) 0.3237(7) 0.8544(8) 0.0299 0.5000 Uani D U . . . . C290 C 0.1419(7) 0.3502(7) 0.8662(9) 0.0298 0.5000 Uani D U . . . . C41 C 0.0019(9) 0.3358(8) 0.8719(9) 0.0329 0.5000 Uani D U . . . . C410 C 0.0425(9) 0.3750(8) 0.8940(9) 0.0328 0.5000 Uani D U . . . . C28 C 0.1092(6) 0.2441(7) 0.8155(10) 0.0261 0.5000 Uani D U . . . . C280 C 0.1143(6) 0.2681(7) 0.8266(10) 0.0262 0.5000 Uani D U . . . . C400 C 0.0108(7) 0.2049(7) 0.8058(8) 0.0282 0.5000 Uani D U . . . . C40 C 0.0175(7) 0.1717(7) 0.7922(8) 0.0282 0.5000 Uani D U . . . . C390 C 0.0100(7) 0.1327(7) 0.7663(8) 0.0296 0.5000 Uani D U . . . . C39 C 0.0366(7) 0.1064(7) 0.7526(7) 0.0298 0.5000 Uani D U . . . . C380 C 0.1066(8) 0.1247(7) 0.7468(8) 0.0288 0.5000 Uani D U . . . . C38 C 0.1413(8) 0.1091(6) 0.7422(8) 0.0289 0.5000 Uani D U . . . . C370 C 0.2114(6) 0.1882(8) 0.7684(9) 0.0273 0.5000 Uani D U . . . . C37 C 0.2344(7) 0.1820(7) 0.7657(10) 0.0273 0.5000 Uani D U . . . . N170 N 0.2104(6) 0.2546(11) 0.8073(14) 0.0257 0.5000 Uani D U . . . . N17 N 0.2140(7) 0.2451(10) 0.8002(14) 0.0257 0.5000 Uani D U . . . . C360 C 0.3270(7) 0.1894(7) 0.7556(10) 0.0298 0.5000 Uani D U . . . . C36 C 0.3547(8) 0.2002(7) 0.7548(11) 0.0297 0.5000 Uani D U . . . . C420 C 0.3428(9) 0.1131(8) 0.7173(10) 0.0308 0.5000 Uani D U . . . . C42 C 0.3916(9) 0.1334(8) 0.7163(10) 0.0308 0.5000 Uani D U . . . . N200 N 0.4067(8) 0.2586(8) 0.7763(14) 0.0324 0.5000 Uani D U . . . . N20 N 0.4212(8) 0.2732(10) 0.7802(13) 0.0324 0.5000 Uani D U . . . . C350 C 0.5295(9) 0.2692(7) 0.7736(9) 0.0377 0.5000 Uani D U . . . . C35 C 0.5428(10) 0.3092(8) 0.7649(8) 0.0378 0.5000 Uani D U . . . . C34 C 0.6082(8) 0.3848(9) 0.8138(8) 0.0440 0.5000 Uani D U . . . . C340 C 0.6031(9) 0.3627(8) 0.7824(8) 0.0440 0.5000 Uani D U . . . . C33 C 0.5705(13) 0.4574(7) 0.8254(8) 0.0461 0.5000 Uani D U . . . . C330 C 0.6014(10) 0.4177(10) 0.8422(9) 0.0461 0.5000 Uani D U . . . . N19 N 0.4671(8) 0.4436(8) 0.8591(10) 0.0458 0.5000 Uani D U . . . . N190 N 0.5038(9) 0.4467(10) 0.8458(8) 0.0457 0.5000 Uani D U . . . . N15 N -0.2620(12) 0.1050(8) 0.4820(8) 0.0297 0.5000 Uani D U . . . . N150 N -0.2419(13) 0.1062(9) 0.4981(8) 0.0297 0.5000 Uani D U . . . . C17 C -0.2298(11) 0.0635(7) 0.5468(6) 0.0308 0.5000 Uani D U . . . . C170 C -0.1979(12) 0.0796(7) 0.5668(6) 0.0309 0.5000 Uani D U . . . . C16 C -0.1112(10) 0.1092(7) 0.5787(7) 0.0311 0.5000 Uani D U . . . . C160 C -0.0823(10) 0.1383(7) 0.5935(7) 0.0310 0.5000 Uani D U . . . . C150 C -0.0718(14) 0.2255(6) 0.6266(6) 0.0310 0.5000 Uani D U . . . . C15 C -0.0882(14) 0.1934(6) 0.6206(6) 0.0312 0.5000 Uani D U . . . . N14 N -0.1216(17) 0.2590(6) 0.5833(9) 0.0316 0.5000 Uani D U . . . . N140 N -0.1174(17) 0.2799(6) 0.5819(9) 0.0316 0.5000 Uani D U . . . . C140 C -0.0928(14) 0.3636(5) 0.5940(7) 0.0370 0.5000 Uani D U . . . . C14 C -0.0865(12) 0.3406(6) 0.6042(6) 0.0370 0.5000 Uani D U . . . . C26 C -0.0072(15) 0.3761(7) 0.6692(8) 0.0424 0.5000 Uani D U . . . . C260 C -0.0127(15) 0.4132(7) 0.6540(8) 0.0422 0.5000 Uani D U . . . . C130 C -0.1517(11) 0.4057(5) 0.5425(6) 0.0365 0.5000 Uani D U . . . . C13 C -0.1392(12) 0.3958(5) 0.5603(7) 0.0365 0.5000 Uani D U . . . . C250 C -0.1257(13) 0.4948(6) 0.5303(8) 0.0399 0.5000 Uani D U . . . . C25 C -0.1101(13) 0.4867(6) 0.5630(8) 0.0401 0.5000 Uani D U . . . . C24 C -0.1715(13) 0.5250(5) 0.5164(8) 0.0414 0.5000 Uani D U . . . . C240 C -0.1903(14) 0.5201(5) 0.4764(9) 0.0413 0.5000 Uani D U . . . . N130 N -0.2321(17) 0.3490(5) 0.5010(10) 0.0342 0.5000 Uani D U . . . . N13 N -0.2191(17) 0.3500(5) 0.5125(10) 0.0343 0.5000 Uani D U . . . . C220 C -0.2997(11) 0.3694(5) 0.4481(6) 0.0345 0.5000 Uani D U . . . . C22 C -0.2801(11) 0.3836(5) 0.4641(6) 0.0345 0.5000 Uani D U . . . . C230 C -0.2780(12) 0.4589(6) 0.4354(8) 0.0377 0.5000 Uani D U . . . . C23 C -0.2596(11) 0.4745(6) 0.4693(7) 0.0378 0.5000 Uani D U . . . . C210 C -0.3774(13) 0.2958(5) 0.4078(8) 0.0318 0.5000 Uani D U . . . . C21 C -0.3646(12) 0.3199(5) 0.4180(7) 0.0318 0.5000 Uani D U . . . . C270 C -0.4639(13) 0.3050(7) 0.3508(8) 0.0335 0.5000 Uani D U . . . . C27 C -0.4465(13) 0.3439(7) 0.3655(8) 0.0336 0.5000 Uani D U . . . . N160 N -0.3631(16) 0.2229(6) 0.4239(10) 0.0302 0.5000 Uani D U . . . . N16 N -0.3591(16) 0.2422(6) 0.4235(10) 0.0302 0.5000 Uani D U . . . . C200 C -0.4406(10) 0.1409(6) 0.3905(8) 0.0321 0.5000 Uani D U . . . . C20 C -0.4392(10) 0.1698(6) 0.3795(8) 0.0321 0.5000 Uani D U . . . . C19 C -0.3966(11) 0.0949(7) 0.3756(6) 0.0331 0.5000 Uani D U . . . . C190 C -0.3881(11) 0.0704(7) 0.3951(6) 0.0330 0.5000 Uani D U . . . . C18 C -0.3723(10) 0.0552(7) 0.4444(7) 0.0336 0.5000 Uani D U . . . . C180 C -0.3523(10) 0.0461(7) 0.4682(7) 0.0336 0.5000 Uani D U . . . . H452 H 1.0081 0.2527 1.2902 0.0841 1.0000 Uiso R . . . . . H451 H 1.0061 0.3027 1.2192 0.0842 1.0000 Uiso R . . . . . H531 H 1.0206 -0.0970 1.0440 0.0461 1.0000 Uiso R . . . . . H541 H 0.8340 -0.1152 1.0592 0.0441 1.0000 Uiso R . . . . . H551 H 0.7858 -0.0141 1.1265 0.0450 1.0000 Uiso R . . . . . H562 H 0.8497 0.1790 1.2571 0.0653 1.0000 Uiso R . . . . . H561 H 0.7896 0.0840 1.2286 0.0651 1.0000 Uiso R . . . . . H563 H 0.7939 0.1612 1.1792 0.0652 1.0000 Uiso R . . . . . H572 H 1.3239 -0.0164 1.0802 0.0570 1.0000 Uiso R . . . . . H573 H 1.2081 -0.0570 1.0328 0.0570 1.0000 Uiso R . . . . . H571 H 1.2964 0.0308 1.0122 0.0570 1.0000 Uiso R . . . . . H461 H 1.1690 0.3225 1.3183 0.0992 1.0000 Uiso R . . . . . H462 H 1.1522 0.3853 1.2636 0.0992 1.0000 Uiso R . . . . . H471 H 1.3134 0.3501 1.2858 0.1133 1.0000 Uiso R . . . . . H472 H 1.2789 0.3850 1.2169 0.1133 1.0000 Uiso R . . . . . C49 C 1.4429(7) 0.2410(8) 1.1428(11) 0.0442 0.5000 Uani D U . . . . C490 C 1.4467(9) 0.2169(10) 1.1749(8) 0.0439 0.5000 Uani D U . . . . C480 C 1.4058(7) 0.2814(7) 1.2023(10) 0.0443 0.5000 Uani D U . . . . C48 C 1.3903(12) 0.2981(5) 1.1710(10) 0.0444 0.5000 Uani D U . . . . 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 Mo1 0.0124(3) 0.0104(3) 0.0224(3) 0.0024(3) 0.0034(2) 0.0019(2) Mo2 0.0217(4) 0.0195(4) 0.0239(4) 0.0015(3) 0.0059(3) 0.0078(3) Ni1 0.0182(5) 0.0231(5) 0.0329(6) 0.0073(4) 0.0065(4) 0.0085(4) Ni2 0.0299(6) 0.0217(6) 0.0288(6) -0.0010(5) 0.0071(5) 0.0074(5) Ni3 0.0268(6) 0.0259(5) 0.0307(6) 0.0001(4) 0.0109(5) 0.0075(5) C1 0.021(4) 0.019(4) 0.025(4) 0.004(3) 0.003(3) 0.005(3) C2 0.019(4) 0.029(5) 0.031(5) 0.007(4) 0.010(3) 0.014(4) C3 0.018(4) 0.025(4) 0.021(4) -0.003(3) 0.007(3) -0.002(3) C4 0.022(4) 0.021(4) 0.031(5) 0.002(3) 0.014(4) 0.002(3) C5 0.025(4) 0.023(4) 0.028(5) 0.006(4) 0.001(4) -0.009(3) C6 0.008(3) 0.015(3) 0.030(4) -0.001(3) 0.006(3) 0.001(3) C7 0.030(5) 0.023(4) 0.025(4) 0.004(3) -0.001(4) -0.003(4) C8 0.025(5) 0.024(4) 0.025(4) 0.008(3) 0.017(3) 0.010(4) C9 0.026(4) 0.019(4) 0.025(4) -0.004(3) 0.004(3) 0.006(3) C10 0.022(4) 0.028(5) 0.030(5) 0.002(4) 0.015(4) 0.007(4) C11 0.032(5) 0.029(5) 0.032(5) 0.001(4) -0.002(4) 0.015(4) C12 0.024(4) 0.040(5) 0.025(5) -0.004(4) 0.005(3) 0.017(4) C43 0.036(5) 0.034(5) 0.018(4) 0.006(3) -0.002(3) 0.012(4) C44 0.029(4) 0.032(4) 0.026(4) 0.021(4) 0.016(3) 0.007(4) C45 0.060(7) 0.071(8) 0.078(9) -0.027(7) 0.029(7) 0.028(6) C46 0.053(7) 0.074(9) 0.099(11) -0.059(8) 0.020(7) 0.009(7) C47 0.083(11) 0.051(8) 0.145(16) -0.049(9) 0.037(10) 0.005(8) C50 0.023(3) 0.051(4) 0.054(5) 0.000(4) 0.012(3) 0.009(3) C51 0.048(5) 0.026(4) 0.024(4) 0.011(3) 0.006(4) 0.022(4) C52 0.039(5) 0.028(4) 0.015(4) 0.003(3) -0.002(3) 0.022(4) C53 0.048(6) 0.031(5) 0.033(5) -0.001(4) -0.007(4) 0.011(4) C54 0.030(5) 0.023(4) 0.047(6) 0.001(4) -0.017(4) -0.001(4) C55 0.028(4) 0.047(6) 0.032(5) 0.012(4) -0.003(4) 0.010(4) C56 0.026(5) 0.049(6) 0.047(6) 0.008(5) 0.013(4) 0.014(4) C57 0.045(5) 0.057(6) 0.025(4) 0.009(4) 0.004(4) 0.034(5) N1 0.013(3) 0.014(3) 0.028(4) 0.002(3) 0.006(3) -0.001(3) N2 0.021(4) 0.025(4) 0.029(4) -0.001(3) 0.006(3) 0.011(3) N3 0.014(3) 0.023(4) 0.032(4) 0.011(3) 0.002(3) 0.004(3) N4 0.015(3) 0.026(4) 0.022(4) -0.003(3) 0.007(3) 0.009(3) N5 0.018(3) 0.019(3) 0.029(4) 0.001(3) 0.002(3) 0.002(3) N6 0.014(3) 0.025(3) 0.020(3) -0.004(3) 0.006(3) 0.009(3) N7 0.032(4) 0.022(4) 0.032(4) 0.012(3) 0.006(3) 0.008(3) N8 0.029(4) 0.024(4) 0.034(4) 0.006(3) 0.013(3) 0.012(3) N9 0.028(4) 0.031(4) 0.022(4) 0.004(3) 0.004(3) 0.011(3) N10 0.030(4) 0.023(4) 0.027(4) 0.003(3) 0.004(3) 0.007(3) N11 0.026(4) 0.024(4) 0.026(4) 0.002(3) 0.003(3) 0.011(3) N12 0.028(4) 0.019(4) 0.030(4) 0.000(3) -0.002(3) 0.011(3) N21 0.026(3) 0.025(3) 0.029(4) 0.007(3) 0.004(3) 0.009(3) N22 0.032(4) 0.040(4) 0.028(4) 0.000(3) 0.011(3) 0.015(3) N23 0.024(3) 0.053(4) 0.051(4) -0.009(3) 0.007(3) 0.006(3) N24 0.035(4) 0.036(4) 0.017(3) 0.003(3) 0.003(3) 0.021(3) S1 0.0196(10) 0.0320(11) 0.0346(12) 0.0086(9) 0.0033(8) 0.0099(9) S2 0.0352(12) 0.0220(10) 0.0327(11) -0.0034(9) 0.0094(9) 0.0076(9) S3 0.0351(12) 0.0358(12) 0.0284(11) -0.0088(9) 0.0081(9) -0.0015(10) S4 0.0269(11) 0.0569(15) 0.0402(13) 0.0187(11) 0.0081(10) 0.0243(11) S5 0.072(2) 0.0350(15) 0.064(2) 0.0295(15) -0.0047(16) -0.0182(14) S6 0.0272(10) 0.0140(9) 0.0388(12) 0.0017(8) 0.0115(9) -0.0002(8) S7 0.0257(11) 0.0468(14) 0.0399(13) 0.0057(11) 0.0033(10) 0.0141(10) S8 0.0241(11) 0.0402(13) 0.0467(14) 0.0085(11) 0.0101(10) 0.0174(11) S9 0.064(2) 0.0322(14) 0.067(2) 0.0226(14) 0.0026(16) 0.0050(13) S10 0.0247(11) 0.0606(17) 0.0321(12) -0.0149(12) 0.0054(9) 0.0076(11) S11 0.0277(13) 0.0435(15) 0.0678(19) 0.0311(14) 0.0060(12) 0.0021(11) S12 0.071(2) 0.090(3) 0.0325(15) -0.0176(15) 0.0013(14) 0.045(2) C32 0.039(4) 0.048(3) 0.058(4) -0.001(3) 0.013(4) 0.015(4) C320 0.039(4) 0.048(3) 0.058(4) -0.001(3) 0.013(4) 0.015(4) C31 0.040(4) 0.044(3) 0.053(4) 0.002(3) 0.012(4) 0.015(4) C310 0.040(4) 0.044(3) 0.053(4) 0.003(3) 0.011(4) 0.015(4) C30 0.040(4) 0.037(3) 0.044(3) 0.004(3) 0.017(4) 0.021(3) C300 0.040(4) 0.037(3) 0.044(3) 0.004(3) 0.017(4) 0.021(3) N18 0.037(3) 0.035(3) 0.033(3) 0.006(3) 0.016(3) 0.022(3) N180 0.037(3) 0.035(3) 0.033(3) 0.007(3) 0.016(3) 0.022(3) C29 0.035(3) 0.034(3) 0.029(3) 0.010(3) 0.014(3) 0.021(3) C290 0.035(3) 0.034(3) 0.029(3) 0.010(3) 0.014(3) 0.021(3) C41 0.036(4) 0.038(4) 0.034(4) 0.009(3) 0.015(3) 0.021(3) C410 0.036(4) 0.038(4) 0.033(4) 0.009(3) 0.015(3) 0.021(3) C28 0.031(2) 0.031(3) 0.026(3) 0.012(2) 0.011(2) 0.019(2) C280 0.031(2) 0.031(3) 0.026(3) 0.012(2) 0.011(2) 0.019(2) C400 0.033(3) 0.032(4) 0.027(3) 0.010(3) 0.010(3) 0.017(3) C40 0.033(3) 0.032(4) 0.027(3) 0.010(3) 0.010(3) 0.017(3) C390 0.034(3) 0.032(4) 0.028(3) 0.008(3) 0.010(3) 0.016(3) C39 0.034(3) 0.032(4) 0.028(3) 0.008(3) 0.010(3) 0.015(3) C380 0.033(3) 0.031(3) 0.027(3) 0.007(3) 0.009(3) 0.016(3) C38 0.033(3) 0.031(3) 0.027(3) 0.007(3) 0.009(3) 0.016(3) C370 0.032(3) 0.028(3) 0.027(3) 0.008(2) 0.011(3) 0.017(2) C37 0.033(3) 0.028(3) 0.027(3) 0.007(2) 0.011(3) 0.017(2) N170 0.031(2) 0.028(3) 0.025(3) 0.009(2) 0.012(2) 0.017(2) N17 0.031(2) 0.028(3) 0.025(3) 0.009(2) 0.012(2) 0.017(2) C360 0.033(3) 0.030(3) 0.033(3) 0.006(2) 0.011(3) 0.017(2) C36 0.032(3) 0.030(3) 0.033(3) 0.006(2) 0.011(3) 0.017(2) C420 0.033(4) 0.029(4) 0.035(3) 0.004(3) 0.011(4) 0.016(3) C42 0.033(4) 0.029(4) 0.036(3) 0.004(3) 0.011(4) 0.016(3) N200 0.033(3) 0.033(3) 0.038(3) 0.005(3) 0.013(3) 0.018(3) N20 0.033(3) 0.033(3) 0.038(3) 0.005(3) 0.013(3) 0.018(3) C350 0.034(3) 0.039(4) 0.046(3) 0.001(3) 0.015(3) 0.018(3) C35 0.034(3) 0.039(4) 0.046(3) 0.001(3) 0.015(3) 0.018(3) C34 0.036(3) 0.045(4) 0.054(4) -0.001(3) 0.011(3) 0.014(3) C340 0.036(3) 0.045(4) 0.054(4) -0.001(3) 0.011(3) 0.014(3) C33 0.036(4) 0.047(4) 0.058(4) -0.002(3) 0.011(3) 0.014(3) C330 0.036(4) 0.047(4) 0.058(4) -0.002(3) 0.011(3) 0.014(3) N19 0.036(4) 0.047(3) 0.058(4) -0.002(3) 0.011(3) 0.015(3) N190 0.035(4) 0.047(3) 0.057(4) -0.002(3) 0.011(4) 0.015(3) N15 0.027(3) 0.028(3) 0.035(4) 0.008(3) 0.012(3) 0.008(3) N150 0.027(3) 0.028(3) 0.035(4) 0.008(3) 0.012(3) 0.008(3) C17 0.026(4) 0.031(3) 0.036(4) 0.008(3) 0.010(3) 0.008(3) C170 0.027(4) 0.031(3) 0.036(4) 0.008(3) 0.009(3) 0.008(3) C16 0.026(3) 0.033(4) 0.036(4) 0.008(3) 0.006(3) 0.011(3) C160 0.026(3) 0.033(4) 0.036(4) 0.008(3) 0.006(3) 0.011(3) C150 0.025(3) 0.034(4) 0.038(3) 0.006(3) 0.003(3) 0.014(3) C15 0.025(3) 0.034(4) 0.038(3) 0.006(3) 0.003(3) 0.014(3) N14 0.025(3) 0.035(3) 0.040(3) 0.005(3) 0.005(2) 0.016(3) N140 0.025(3) 0.035(3) 0.040(3) 0.005(3) 0.005(2) 0.016(3) C140 0.033(3) 0.036(3) 0.043(3) 0.000(3) 0.004(3) 0.013(3) C14 0.033(3) 0.036(3) 0.043(3) 0.000(3) 0.004(3) 0.013(3) C26 0.039(4) 0.040(4) 0.046(4) -0.001(4) 0.001(3) 0.010(4) C260 0.039(4) 0.039(4) 0.046(4) -0.001(4) 0.001(3) 0.011(4) C130 0.033(3) 0.034(3) 0.044(3) 0.000(3) 0.006(3) 0.013(2) C13 0.033(3) 0.034(3) 0.044(3) 0.000(3) 0.006(3) 0.012(2) C250 0.037(3) 0.035(3) 0.049(4) 0.001(3) 0.005(3) 0.011(3) C25 0.037(3) 0.035(3) 0.049(4) 0.001(3) 0.005(3) 0.011(3) C24 0.038(3) 0.036(3) 0.050(4) 0.003(3) 0.006(3) 0.012(3) C240 0.038(3) 0.036(3) 0.050(4) 0.003(3) 0.006(3) 0.012(3) N130 0.030(3) 0.034(3) 0.042(3) 0.004(2) 0.008(2) 0.013(2) N13 0.030(3) 0.034(3) 0.042(3) 0.004(2) 0.008(2) 0.013(2) C220 0.030(3) 0.035(3) 0.042(3) 0.008(2) 0.010(2) 0.014(2) C22 0.030(3) 0.035(3) 0.042(3) 0.008(2) 0.010(2) 0.014(2) C230 0.034(3) 0.036(3) 0.046(4) 0.007(3) 0.007(3) 0.013(3) C23 0.034(3) 0.036(3) 0.046(4) 0.007(3) 0.007(3) 0.013(3) C210 0.027(3) 0.034(3) 0.039(3) 0.009(3) 0.010(2) 0.015(3) C21 0.027(3) 0.034(3) 0.039(3) 0.009(3) 0.010(2) 0.015(3) C270 0.029(3) 0.036(4) 0.040(4) 0.010(4) 0.008(3) 0.015(4) C27 0.029(3) 0.036(4) 0.040(4) 0.011(4) 0.008(3) 0.015(4) N160 0.025(3) 0.033(3) 0.037(3) 0.008(3) 0.010(2) 0.014(3) N16 0.025(3) 0.033(3) 0.037(3) 0.008(3) 0.010(2) 0.014(3) C200 0.029(3) 0.034(4) 0.036(3) 0.008(3) 0.009(3) 0.011(3) C20 0.029(3) 0.034(4) 0.036(3) 0.008(3) 0.010(3) 0.011(3) C19 0.031(3) 0.032(3) 0.036(4) 0.007(3) 0.011(3) 0.009(3) C190 0.031(3) 0.032(3) 0.036(4) 0.007(3) 0.010(3) 0.009(3) C18 0.031(3) 0.032(3) 0.036(4) 0.008(3) 0.010(3) 0.006(3) C180 0.031(3) 0.032(3) 0.036(4) 0.008(3) 0.010(3) 0.006(3) C49 0.022(3) 0.054(4) 0.055(5) -0.003(4) 0.008(3) 0.008(3) C490 0.022(3) 0.053(4) 0.055(5) -0.002(4) 0.008(3) 0.009(3) C480 0.024(3) 0.052(4) 0.054(4) -0.005(4) 0.006(3) 0.008(3) C48 0.024(3) 0.052(4) 0.054(4) -0.005(4) 0.006(3) 0.008(3) _refine_ls_extinction_method None loop_ _oxford_twin_element_scale_factors 0.5172(12) 0.4828(12) 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 Mo1 . N1 . 2.124(7) yes Mo1 . N2 . 2.093(8) yes Mo1 . N3 . 2.081(8) yes Mo1 . N4 . 2.101(7) yes Mo1 . N5 . 2.068(7) yes Mo1 . N6 . 2.094(7) yes Mo2 . N7 . 2.125(8) yes Mo2 . N8 . 2.113(8) yes Mo2 . N9 . 2.078(7) yes Mo2 . N10 . 2.066(8) yes Mo2 . N11 . 2.098(7) yes Mo2 . N12 . 2.093(8) yes Ni1 . S4 1_455 2.531(3) yes Ni1 . S1 . 2.593(2) yes Ni1 . N15 . 2.005(17) yes Ni1 . N150 . 2.024(17) yes Ni1 . N14 . 2.017(8) yes Ni1 . N140 . 2.055(8) yes Ni1 . N130 . 1.923(9) yes Ni1 . N13 . 1.910(8) yes Ni1 . N160 . 2.000(8) yes Ni1 . N16 . 2.054(8) yes Ni2 . S2 . 2.574(3) yes Ni2 . S7 . 2.591(3) yes Ni2 . N18 . 2.117(7) yes Ni2 . N180 . 1.988(7) yes Ni2 . N170 . 1.880(8) yes Ni2 . N17 . 1.957(7) yes Ni2 . N200 . 2.081(8) yes Ni2 . N20 . 1.980(8) yes Ni2 . N19 . 1.870(10) yes Ni2 . N190 . 2.129(13) yes Ni3 . S3 1_656 3.142(3) yes Ni3 . N21 . 1.829(7) yes Ni3 . N22 . 1.947(7) yes Ni3 . N23 . 1.938(8) yes Ni3 . N24 . 1.934(7) yes Ni3 . S8 . 2.887(3) yes C1 . N1 . 1.155(11) yes C1 . S1 . 1.642(9) yes C2 . N2 . 1.162(12) yes C2 . S2 . 1.640(10) yes C3 . N3 . 1.174(11) yes C3 . S3 . 1.600(8) yes C4 . N4 . 1.166(11) yes C4 . S4 . 1.646(9) yes C5 . N5 . 1.177(10) yes C5 . S5 . 1.621(8) yes C6 . N6 . 1.195(10) yes C6 . S6 . 1.607(7) yes C7 . N7 . 1.148(12) yes C7 . S7 . 1.642(10) yes C8 . N8 . 1.194(12) yes C8 . S8 . 1.627(9) yes C9 . N9 . 1.166(11) yes C9 . S9 . 1.618(9) yes C10 . N10 . 1.168(12) yes C10 . S10 . 1.629(10) yes C11 . N11 . 1.150(11) yes C11 . S11 . 1.632(10) yes C12 . N12 . 1.163(12) yes C12 . S12 . 1.605(10) yes C43 . C44 . 1.467(13) yes C43 . C55 . 1.389(13) yes C43 . N21 . 1.349(11) yes C44 . C56 . 1.492(12) yes C44 . N22 . 1.309(11) yes C45 . C46 . 1.461(18) yes C45 . N22 . 1.429(13) yes C45 . H452 . 0.972 no C45 . H451 . 0.974 no C46 . C47 . 1.378(19) yes C46 . H461 . 0.930 no C46 . H462 . 0.930 no C47 . N23 . 1.409(14) yes C47 . H471 . 0.930 no C47 . H472 . 0.930 no C50 . N24 . 1.469(9) yes C50 . C49 . 1.449(8) yes C50 . C490 . 1.442(8) yes C51 . C52 . 1.484(13) yes C51 . C57 . 1.503(12) yes C51 . N24 . 1.280(11) yes C52 . C53 . 1.381(12) yes C52 . N21 . 1.315(10) yes C53 . C54 . 1.368(14) yes C53 . H531 . 0.935 no C54 . C55 . 1.397(14) yes C54 . H541 . 0.934 no C55 . H551 . 0.936 no C56 . H562 . 0.964 no C56 . H561 . 0.962 no C56 . H563 . 0.964 no C57 . H572 . 0.963 no C57 . H573 . 0.967 no C57 . H571 . 0.963 no N23 . C480 . 1.446(8) yes N23 . C48 . 1.456(8) yes C32 . C31 . 1.388(8) yes C32 . N19 . 1.332(9) yes C320 . C310 . 1.373(9) yes C320 . N190 . 1.327(9) yes C31 . C30 . 1.621(9) yes C310 . C300 . 1.596(9) yes C30 . N18 . 1.573(8) yes C300 . N180 . 1.553(8) yes N18 . C29 . 1.270(8) yes N180 . C290 . 1.249(8) yes C29 . C41 . 1.556(9) yes C29 . C28 . 1.474(8) yes C290 . C410 . 1.556(9) yes C290 . C280 . 1.465(8) yes C28 . C40 . 1.399(7) yes C28 . N17 . 1.361(7) yes C280 . C400 . 1.398(7) yes C280 . N170 . 1.367(7) yes C400 . C390 . 1.395(7) yes C40 . C39 . 1.398(7) yes C390 . C380 . 1.339(7) yes C39 . C38 . 1.328(7) yes C380 . C370 . 1.415(7) yes C38 . C37 . 1.415(7) yes C370 . N170 . 1.317(7) yes C370 . C360 . 1.480(7) yes C37 . N17 . 1.325(7) yes C37 . C36 . 1.471(8) yes C360 . C420 . 1.518(9) yes C360 . N200 . 1.281(8) yes C360 . N20 . 1.536(13) yes C36 . C42 . 1.523(9) yes C36 . N20 . 1.282(8) yes N200 . C350 . 1.495(8) yes N20 . C35 . 1.499(8) yes C350 . C340 . 1.516(9) yes C35 . C34 . 1.509(9) yes C34 . C33 . 1.437(9) yes C340 . C330 . 1.451(9) yes C33 . N19 . 1.445(9) yes C330 . N190 . 1.452(9) yes N15 . C17 . 1.502(8) yes N15 . C18 . 1.480(8) yes N150 . C170 . 1.500(8) yes N150 . C180 . 1.481(8) yes C17 . C16 . 1.504(8) yes C170 . C160 . 1.501(8) yes C16 . C15 . 1.521(8) yes C160 . C150 . 1.520(8) yes C150 . N140 . 1.450(8) yes C15 . N14 . 1.446(8) yes N14 . C14 . 1.315(8) yes N140 . C140 . 1.321(8) yes C140 . C260 . 1.497(9) yes C140 . C130 . 1.483(8) yes C14 . C26 . 1.506(9) yes C14 . C13 . 1.501(8) yes C130 . C250 . 1.416(7) yes C130 . N130 . 1.325(7) yes C13 . C25 . 1.416(7) yes C13 . N13 . 1.322(7) yes C250 . C240 . 1.401(7) yes C25 . C24 . 1.406(7) yes C24 . C23 . 1.395(7) yes C240 . C230 . 1.401(7) yes N130 . C220 . 1.374(7) yes N13 . C22 . 1.376(7) yes C220 . C230 . 1.431(7) yes C220 . C210 . 1.449(8) yes C22 . C23 . 1.430(7) yes C22 . C21 . 1.451(8) yes C210 . C270 . 1.511(9) yes C210 . N160 . 1.299(8) yes C21 . C27 . 1.516(9) yes C21 . N16 . 1.302(8) yes N160 . C200 . 1.485(8) yes N16 . C20 . 1.483(8) yes C200 . C190 . 1.500(8) yes C20 . C19 . 1.490(8) yes C19 . C18 . 1.518(8) yes C190 . C18 . 0.992(16) yes C190 . C180 . 1.521(8) yes C49 . C48 . 1.429(7) yes C490 . C480 . 1.426(7) yes 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 . Mo1 . N2 . 91.6(2) yes N1 . Mo1 . N3 . 89.6(3) yes N2 . Mo1 . N3 . 178.8(3) yes N1 . Mo1 . N4 . 179.4(3) yes N2 . Mo1 . N4 . 88.7(3) yes N3 . Mo1 . N4 . 90.1(3) yes N1 . Mo1 . N5 . 87.9(3) yes N2 . Mo1 . N5 . 89.5(3) yes N3 . Mo1 . N5 . 90.4(3) yes N4 . Mo1 . N5 . 91.6(3) yes N1 . Mo1 . N6 . 91.4(2) yes N2 . Mo1 . N6 . 90.7(3) yes N3 . Mo1 . N6 . 89.4(3) yes N4 . Mo1 . N6 . 89.1(3) yes N5 . Mo1 . N6 . 179.3(3) yes N7 . Mo2 . N8 . 177.9(3) yes N7 . Mo2 . N9 . 88.5(3) yes N8 . Mo2 . N9 . 91.5(3) yes N7 . Mo2 . N10 . 87.9(3) yes N8 . Mo2 . N10 . 90.0(3) yes N9 . Mo2 . N10 . 88.6(3) yes N7 . Mo2 . N11 . 88.9(3) yes N8 . Mo2 . N11 . 91.1(3) yes N9 . Mo2 . N11 . 177.3(3) yes N10 . Mo2 . N11 . 92.0(3) yes N7 . Mo2 . N12 . 92.3(3) yes N8 . Mo2 . N12 . 89.8(3) yes N9 . Mo2 . N12 . 90.8(3) yes N10 . Mo2 . N12 . 179.4(3) yes N11 . Mo2 . N12 . 88.5(3) yes S4 1_455 Ni1 . S1 . 176.46(10) yes S4 1_455 Ni1 . N15 . 93.4(6) yes S1 . Ni1 . N15 . 90.0(6) yes S4 1_455 Ni1 . N150 . 91.6(5) yes S1 . Ni1 . N150 . 91.6(5) yes N15 . Ni1 . N150 . 10.7(4) yes S4 1_455 Ni1 . N14 . 85.1(8) yes S1 . Ni1 . N14 . 93.4(7) yes N15 . Ni1 . N14 . 101.6(4) yes N150 . Ni1 . N14 . 90.9(4) yes S4 1_455 Ni1 . N140 . 86.7(7) yes S1 . Ni1 . N140 . 91.3(7) yes N15 . Ni1 . N140 . 110.6(4) yes N150 . Ni1 . N140 . 100.0(4) yes N14 . Ni1 . N140 . 9.3(4) yes S4 1_455 Ni1 . N130 . 92.4(8) yes S1 . Ni1 . N130 . 84.4(8) yes N15 . Ni1 . N130 . 169.0(5) yes N150 . Ni1 . N130 . 175.8(9) yes N14 . Ni1 . N130 . 88.2(4) yes S4 1_455 Ni1 . N13 . 90.7(8) yes S1 . Ni1 . N13 . 85.9(8) yes N15 . Ni1 . N13 . 175.5(9) yes N150 . Ni1 . N13 . 170.9(5) yes N14 . Ni1 . N13 . 80.6(3) yes S4 1_455 Ni1 . N160 . 92.8(8) yes S1 . Ni1 . N160 . 88.1(8) yes N15 . Ni1 . N160 . 89.3(4) yes N150 . Ni1 . N160 . 100.0(4) yes N14 . Ni1 . N160 . 169.0(4) yes S4 1_455 Ni1 . N16 . 93.8(7) yes S1 . Ni1 . N16 . 86.5(7) yes N15 . Ni1 . N16 . 97.7(4) yes N150 . Ni1 . N16 . 108.3(4) yes N14 . Ni1 . N16 . 160.8(4) yes N140 . Ni1 . N130 . 79.0(3) yes N140 . Ni1 . N13 . 71.4(4) yes N130 . Ni1 . N13 . 7.7(4) yes N140 . Ni1 . N160 . 160.1(4) yes N130 . Ni1 . N160 . 81.1(3) yes N13 . Ni1 . N160 . 88.7(4) yes N140 . Ni1 . N16 . 151.7(3) yes N130 . Ni1 . N16 . 72.7(4) yes N13 . Ni1 . N16 . 80.3(3) yes N160 . Ni1 . N16 . 8.5(4) yes S2 . Ni2 . S7 . 169.68(9) yes S2 . Ni2 . N18 . 83.8(6) yes S7 . Ni2 . N18 . 85.9(6) yes S2 . Ni2 . N180 . 85.8(6) yes S7 . Ni2 . N180 . 84.0(6) yes N18 . Ni2 . N180 . 10.7(4) yes S2 . Ni2 . N170 . 89.2(9) yes S7 . Ni2 . N170 . 87.5(9) yes N18 . Ni2 . N170 . 70.8(4) yes N180 . Ni2 . N170 . 81.4(3) yes S2 . Ni2 . N17 . 89.0(9) yes S7 . Ni2 . N17 . 88.8(9) yes N18 . Ni2 . N17 . 77.0(3) yes N180 . Ni2 . N17 . 87.6(3) yes N170 . Ni2 . N17 . 6.2(4) yes S2 . Ni2 . N200 . 95.8(8) yes S7 . Ni2 . N200 . 93.3(8) yes N18 . Ni2 . N200 . 151.0(3) yes N180 . Ni2 . N200 . 161.4(4) yes N170 . Ni2 . N200 . 80.1(3) yes S2 . Ni2 . N20 . 95.6(9) yes S7 . Ni2 . N20 . 94.0(9) yes N18 . Ni2 . N20 . 157.6(4) yes N180 . Ni2 . N20 . 168.0(4) yes N170 . Ni2 . N20 . 86.7(4) yes S2 . Ni2 . N19 . 90.6(6) yes S7 . Ni2 . N19 . 90.8(6) yes N18 . Ni2 . N19 . 98.8(4) yes N180 . Ni2 . N19 . 88.3(4) yes N170 . Ni2 . N19 . 169.6(4) yes S2 . Ni2 . N190 . 88.0(5) yes S7 . Ni2 . N190 . 95.6(5) yes N18 . Ni2 . N190 . 111.5(3) yes N180 . Ni2 . N190 . 101.1(4) yes N170 . Ni2 . N190 . 176.1(9) yes N17 . Ni2 . N200 . 74.0(3) yes N17 . Ni2 . N20 . 80.6(3) yes N200 . Ni2 . N20 . 6.6(4) yes N17 . Ni2 . N19 . 175.8(4) yes N200 . Ni2 . N19 . 110.2(4) yes N20 . Ni2 . N19 . 103.6(4) yes N17 . Ni2 . N190 . 170.6(5) yes N200 . Ni2 . N190 . 97.5(4) yes N20 . Ni2 . N190 . 90.8(4) yes N19 . Ni2 . N190 . 13.4(5) yes S3 1_656 Ni3 . N21 . 91.6(2) yes S3 1_656 Ni3 . N22 . 102.6(2) yes N21 . Ni3 . N22 . 82.2(3) yes S3 1_656 Ni3 . N23 . 86.9(3) yes N21 . Ni3 . N23 . 178.5(4) yes N22 . Ni3 . N23 . 98.3(3) yes S3 1_656 Ni3 . N24 . 76.8(2) yes N21 . Ni3 . N24 . 82.2(3) yes N22 . Ni3 . N24 . 164.4(3) yes N23 . Ni3 . N24 . 97.2(3) yes S3 1_656 Ni3 . S8 . 166.10(8) yes N21 . Ni3 . S8 . 88.6(2) yes N22 . Ni3 . S8 . 91.2(2) yes N23 . Ni3 . S8 . 92.8(3) yes N24 . Ni3 . S8 . 89.5(2) yes N1 . C1 . S1 . 178.9(8) yes N2 . C2 . S2 . 176.6(8) yes N3 . C3 . S3 . 176.6(8) yes N4 . C4 . S4 . 176.1(8) yes N5 . C5 . S5 . 177.6(10) yes N6 . C6 . S6 . 178.4(8) yes N7 . C7 . S7 . 178.0(8) yes N8 . C8 . S8 . 177.1(8) yes N9 . C9 . S9 . 177.8(9) yes N10 . C10 . S10 . 176.8(9) yes N11 . C11 . S11 . 178.8(9) yes N12 . C12 . S12 . 178.6(9) yes C44 . C43 . C55 . 129.1(8) yes C44 . C43 . N21 . 110.8(8) yes C55 . C43 . N21 . 120.1(8) yes C43 . C44 . C56 . 122.3(8) yes C43 . C44 . N22 . 114.3(7) yes C56 . C44 . N22 . 123.4(8) yes C46 . C45 . N22 . 117.1(10) yes C46 . C45 . H452 . 107.7 no N22 . C45 . H452 . 107.5 no C46 . C45 . H451 . 107.6 no N22 . C45 . H451 . 107.5 no H452 . C45 . H451 . 109.2 no C45 . C46 . C47 . 129.6(11) yes C45 . C46 . H461 . 104.0 no C47 . C46 . H461 . 104.7 no C45 . C46 . H462 . 104.4 no C47 . C46 . H462 . 103.9 no H461 . C46 . H462 . 109.5 no C46 . C47 . N23 . 126.1(12) yes C46 . C47 . H471 . 104.8 no N23 . C47 . H471 . 104.5 no C46 . C47 . H472 . 105.9 no N23 . C47 . H472 . 105.5 no H471 . C47 . H472 . 109.5 no N24 . C50 . C49 . 117.1(6) yes N24 . C50 . C490 . 115.0(8) yes C52 . C51 . C57 . 122.6(8) yes C52 . C51 . N24 . 114.2(7) yes C57 . C51 . N24 . 123.1(9) yes C51 . C52 . C53 . 129.6(8) yes C51 . C52 . N21 . 110.7(7) yes C53 . C52 . N21 . 119.7(8) yes C52 . C53 . C54 . 119.3(9) yes C52 . C53 . H531 . 120.7 no C54 . C53 . H531 . 119.9 no C53 . C54 . C55 . 120.8(8) yes C53 . C54 . H541 . 119.9 no C55 . C54 . H541 . 119.2 no C54 . C55 . C43 . 117.1(8) yes C54 . C55 . H551 . 121.6 no C43 . C55 . H551 . 121.3 no C44 . C56 . H562 . 110.1 no C44 . C56 . H561 . 109.0 no H562 . C56 . H561 . 108.9 no C44 . C56 . H563 . 110.5 no H562 . C56 . H563 . 109.0 no H561 . C56 . H563 . 109.4 no C51 . C57 . H572 . 109.5 no C51 . C57 . H573 . 108.3 no H572 . C57 . H573 . 110.4 no C51 . C57 . H571 . 107.6 no H572 . C57 . H571 . 110.5 no H573 . C57 . H571 . 110.4 no Mo1 . N1 . C1 . 170.7(7) yes Mo1 . N2 . C2 . 172.6(7) yes Mo1 . N3 . C3 . 176.3(6) yes Mo1 . N4 . C4 . 174.3(7) yes Mo1 . N5 . C5 . 174.8(7) yes Mo1 . N6 . C6 . 172.7(6) yes Mo2 . N7 . C7 . 177.6(8) yes Mo2 . N8 . C8 . 168.6(7) yes Mo2 . N9 . C9 . 177.4(7) yes Mo2 . N10 . C10 . 177.0(7) yes Mo2 . N11 . C11 . 178.2(8) yes Mo2 . N12 . C12 . 174.6(7) yes C43 . N21 . C52 . 122.9(8) yes C43 . N21 . Ni3 . 118.6(6) yes C52 . N21 . Ni3 . 118.5(6) yes C45 . N22 . C44 . 119.6(8) yes C45 . N22 . Ni3 . 126.2(7) yes C44 . N22 . Ni3 . 114.1(6) yes C47 . N23 . Ni3 . 120.3(8) yes C47 . N23 . C480 . 119.1(9) yes Ni3 . N23 . C480 . 120.4(5) yes C47 . N23 . C48 . 118.1(9) yes Ni3 . N23 . C48 . 115.7(7) yes C50 . N24 . C51 . 117.8(7) yes C50 . N24 . Ni3 . 127.8(5) yes C51 . N24 . Ni3 . 114.3(6) yes Ni1 . S1 . C1 . 105.2(3) yes Ni2 . S2 . C2 . 106.7(3) yes C3 . S3 . Ni3 1_454 101.9(3) yes Ni1 1_655 S4 . C4 . 106.3(3) yes Ni2 . S7 . C7 . 112.5(3) yes Ni3 . S8 . C8 . 102.2(3) yes C31 . C32 . N19 . 111.21(10) yes C310 . C320 . N190 . 111.21(10) yes C32 . C31 . C30 . 124.75(10) yes C320 . C310 . C300 . 124.71(10) yes C31 . C30 . N18 . 112.21(10) yes C310 . C300 . N180 . 112.11(10) yes C30 . N18 . Ni2 . 116.7(3) yes C30 . N18 . C29 . 128.42(9) yes Ni2 . N18 . C29 . 114.8(3) yes C300 . N180 . Ni2 . 117.3(3) yes C300 . N180 . C290 . 128.49(9) yes Ni2 . N180 . C290 . 114.2(3) yes N18 . C29 . C41 . 125.20(9) yes N18 . C29 . C28 . 116.96(9) yes C41 . C29 . C28 . 117.73(9) yes N180 . C290 . C410 . 125.26(8) yes N180 . C290 . C280 . 116.91(8) yes C410 . C290 . C280 . 117.83(8) yes C29 . C28 . C40 . 131.74(8) yes C29 . C28 . N17 . 110.94(8) yes C40 . C28 . N17 . 117.31(7) yes C290 . C280 . C400 . 131.79(8) yes C290 . C280 . N170 . 110.85(8) yes C400 . C280 . N170 . 117.36(7) yes C280 . C400 . C390 . 119.22(9) yes C28 . C40 . C39 . 119.24(9) yes C400 . C390 . C380 . 120.61(9) yes C40 . C39 . C38 . 120.63(9) yes C390 . C380 . C370 . 120.14(9) yes C39 . C38 . C37 . 120.14(9) yes C380 . C370 . N170 . 118.16(8) yes C380 . C370 . C360 . 128.53(8) yes N170 . C370 . C360 . 113.27(8) yes C38 . C37 . N17 . 118.12(8) yes C38 . C37 . C36 . 128.49(8) yes N17 . C37 . C36 . 113.35(8) yes C280 . N170 . C370 . 124.44(9) yes C280 . N170 . Ni2 . 116.5(3) yes C370 . N170 . Ni2 . 118.6(4) yes C28 . N17 . C37 . 124.30(9) yes C28 . N17 . Ni2 . 120.2(3) yes C37 . N17 . Ni2 . 115.5(3) yes C370 . C360 . C420 . 119.52(9) yes C370 . C360 . N200 . 115.32(8) yes C420 . C360 . N200 . 125.10(9) yes C370 . C360 . N20 . 114.5(5) yes C420 . C360 . N20 . 125.9(5) yes C37 . C36 . C42 . 119.50(8) yes C37 . C36 . N20 . 115.38(8) yes C42 . C36 . N20 . 125.12(8) yes C360 . N200 . Ni2 . 112.1(3) yes C360 . N200 . C350 . 123.20(9) yes Ni2 . N200 . C350 . 124.0(6) yes C360 . N20 . Ni2 . 106.2(6) yes C36 . N20 . Ni2 . 115.3(3) yes C360 . N20 . C35 . 132.2(6) yes C36 . N20 . C35 . 123.17(9) yes Ni2 . N20 . C35 . 120.9(6) yes N200 . C350 . C340 . 112.01(10) yes N20 . C35 . C34 . 112.04(10) yes C35 . C34 . C33 . 123.03(10) yes C350 . C340 . C330 . 123.01(10) yes C34 . C33 . N19 . 118.31(10) yes C340 . C330 . N190 . 118.33(10) yes C33 . N19 . C32 . 115.60(10) yes C33 . N19 . Ni2 . 116.0(7) yes C32 . N19 . Ni2 . 128.4(7) yes C330 . N190 . C320 . 115.57(10) yes C330 . N190 . Ni2 . 112.9(9) yes C320 . N190 . Ni2 . 116.6(10) yes Ni1 . N15 . C17 . 111.4(10) yes Ni1 . N15 . C18 . 114.7(11) yes C17 . N15 . C18 . 114.16(10) yes Ni1 . N150 . C170 . 113.0(10) yes Ni1 . N150 . C180 . 111.9(11) yes C170 . N150 . C180 . 114.17(10) yes N15 . C17 . C16 . 113.11(10) yes N150 . C170 . C160 . 113.10(10) yes C17 . C16 . C15 . 118.67(10) yes C170 . C160 . C150 . 118.66(10) yes C160 . C150 . N140 . 115.03(10) yes C16 . C15 . N14 . 115.02(10) yes C15 . N14 . Ni1 . 121.9(4) yes C15 . N14 . C14 . 123.41(9) yes Ni1 . N14 . C14 . 114.3(3) yes C150 . N140 . Ni1 . 121.9(4) yes C150 . N140 . C140 . 123.43(9) yes Ni1 . N140 . C140 . 114.2(4) yes N140 . C140 . C260 . 124.04(8) yes N140 . C140 . C130 . 114.03(8) yes C260 . C140 . C130 . 121.93(8) yes N14 . C14 . C26 . 123.98(9) yes N14 . C14 . C13 . 113.98(9) yes C26 . C14 . C13 . 121.90(9) yes C140 . C130 . C250 . 127.98(9) yes C140 . C130 . N130 . 112.23(8) yes C250 . C130 . N130 . 119.58(9) yes C14 . C13 . C25 . 128.07(8) yes C14 . C13 . N13 . 112.31(8) yes C25 . C13 . N13 . 119.57(8) yes C130 . C250 . C240 . 118.29(9) yes C13 . C25 . C24 . 118.24(9) yes C25 . C24 . C23 . 120.74(9) yes C250 . C240 . C230 . 120.79(9) yes C130 . N130 . Ni1 . 119.5(4) yes C130 . N130 . C220 . 125.11(8) yes Ni1 . N130 . C220 . 114.5(4) yes C13 . N13 . Ni1 . 118.5(4) yes C13 . N13 . C22 . 125.04(9) yes Ni1 . N13 . C22 . 116.0(3) yes N130 . C220 . C230 . 116.87(9) yes N130 . C220 . C210 . 114.56(9) yes C230 . C220 . C210 . 128.28(9) yes N13 . C22 . C23 . 116.85(9) yes N13 . C22 . C21 . 114.58(9) yes C23 . C22 . C21 . 128.33(9) yes C220 . C230 . C240 . 119.24(9) yes C22 . C23 . C24 . 119.16(9) yes C220 . C210 . C270 . 122.16(8) yes C220 . C210 . N160 . 113.90(8) yes C270 . C210 . N160 . 123.91(8) yes C22 . C21 . C27 . 122.15(9) yes C22 . C21 . N16 . 113.87(9) yes C27 . C21 . N16 . 123.89(9) yes C210 . N160 . Ni1 . 115.5(3) yes C210 . N160 . C200 . 120.44(9) yes Ni1 . N160 . C200 . 123.8(4) yes C21 . N16 . Ni1 . 114.6(3) yes C21 . N16 . C20 . 120.45(9) yes Ni1 . N16 . C20 . 124.7(4) yes N160 . C200 . C190 . 111.70(10) yes N16 . C20 . C19 . 111.69(10) yes C20 . C19 . C18 . 117.70(10) yes C200 . C190 . C18 . 113.1(15) yes C200 . C190 . C180 . 117.70(10) yes C19 . C18 . N15 . 112.51(10) yes N15 . C18 . C190 . 117.4(12) yes C190 . C180 . N150 . 112.50(10) yes C50 . C49 . C48 . 125.70(10) yes C50 . C490 . C480 . 125.68(10) yes N23 . C480 . C490 . 126.00(10) yes N23 . C48 . C49 . 126.05(10) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/06/12 at 16:35:58 # #LIST 12 BLOCK SCALE X'S, U'S SUMFIX ELEMENT SCALES RIDE C ( 45,X'S) H ( 452,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 562,X'S) H ( 561,X'S) H ( 563,X'S) RIDE C ( 57,X'S) H ( 572,X'S) H ( 573,X'S) H ( 571,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/06/12 at 16:35:58 # #LIST 16 SAME C(28) C(29) C(30) C(31) C(32) C(33) CONT C(34) C(35) C(36) C(37) C(38) C(39) CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20) CONT AND CONT C(280) C(290) C(300) C(310) C(320) C(330) CONT C(340) C(350) C(360) C(370) C(380) C(390) CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200) REM DELU 0.005 C(28) C(29) C(30) C(31) C(32) C(33) CONT C(34) C(35) C(36) C(37) C(38) C(39) CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20) CONT AND CONT C(280) C(290) C(300) C(310) C(320) C(330) CONT C(340) C(350) C(360) C(370) C(380) C(390) CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200) REM SIMU 0.005 C(28) C(29) C(30) C(31) C(32) C(33) CONT C(34) C(35) C(36) C(37) C(38) C(39) CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20) CONT AND CONT C(280) C(290) C(300) C(310) C(320) C(330) CONT C(340) C(350) C(360) C(370) C(380) C(390) CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200) REM U(IJ) 0,.001 =C(28) TO C(280) C(29) TO C(290) CONT C(30) TO C(300) C(31) TO C(310) CONT C(32) TO C(320) C(33) TO C(330) CONT C(34) TO C(340) C(35) TO C(350) CONT C(36) TO C(360) C(37) TO C(370) CONT C(38) TO C(380) C(39) TO C(390) CONT C(40) TO C(400) C(41) TO C(410) CONT C(42) TO C(420) CONT N(17) TO N(170) N(18) TO N(180) CONT N(19) TO N(190) N(20) TO N(200) REM REM SAME C(13) C(14) C(15) C(16) C(17) C(18) CONT C(19) C(20) C(21) C(22) C(23) C(24) CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16) CONT AND CONT C(130) C(140) C(150) C(160) C(170) C(180) CONT C(190) C(200) C(210) C(220) C(230) C(240) CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160) REM DELU 0.005 C(13) C(14) C(15) C(16) C(17) C(18) CONT C(19) C(20) C(21) C(22) C(23) C(24) CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16) CONT AND CONT C(130) C(140) C(150) C(160) C(170) C(180) CONT C(190) C(200) C(210) C(220) C(230) C(240) CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160) REM SIMU 0.005 C(13) C(14) C(15) C(16) C(17) C(18) CONT C(19) C(20) C(21) C(22) C(23) C(24) CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16) CONT AND CONT C(130) C(140) C(150) C(160) C(170) C(180) CONT C(190) C(200) C(210) C(220) C(230) C(240) CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160) REM U(IJ) 0,.001 =C(13) TO C(130) C(14) TO C(140) CONT C(15) TO C(150) C(16) TO C(160) CONT C(17) TO C(170) C(18) TO C(180) CONT C(19) TO C(190) C(20) TO C(200) CONT C(21) TO C(210) C(22) TO C(220) CONT C(23) TO C(230) C(24) TO C(240) CONT C(25) TO C(250) C(26) TO C(260) CONT C(27) TO C(270) CONT N(13) TO N(130) N(14) TO N(140) CONT N(15) TO N(150) N(16) TO N(160) DIST 1.45,0.02=N(23) TO C(48), C(48) TO C(49) CONT C(49) TO C(50), C(50) TO N(24) CONT N(23) TO C(480), C(480) TO C(490) CONT C(490) TO C(50) SAME N(23) C(48) C(49) C(50) CONT AND N(23) C(480) C(490) C(50) REM DELU 0.005 N(23) C(48) C(49) C(50) CONT AND N(23) C(480) C(490) C(50) REM SIMU 0.005 N(23) C(48) C(49) C(50) CONT AND N(23) C(480) C(490) C(50) REM U(IJ) 0,.001 =C(48) TO C(480) C(49) TO C(490) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 3 -1 1 x . -1 -3 1 x . -2 0 4 x . 2 -2 3 x . -1 1 5 x . 0 3 1 x .