# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global-cpd2 _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- Compd_2new.cif' _audit_creation_date 11-05-26 _audit_creation_method CRYSTALS_ver_14.09 _oxford_structure_analysis_title 'monoc in C2/m' _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, F-31077 Toulouse, France ; _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 ; Oligomeric and polymeric organizations of potassium salts with compartmental Schiff-base complexes as ligands ; # 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 'Maliheh Mousavi' ; CNRS ; LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, F-31077 Toulouse, France ; ; ? # Footnote for author 1 ; V.Bereaua ; CNRS ; LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, F-31077 Toulouse, France ; ; ? # Footnote 2 ; 'Carine Duhayon' ; CNRS ; LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, F-31077 Toulouse, France ; ; ? # Footnote 2 ; 'Jean-Pascal Sutter' ; CNRS ; LCC (Laboratoire de Chimie de Coordination), 205 route de Narbonne, F-31077 Toulouse, 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: ; The H atoms 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 ; ? ; # 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 809267' #TrackingRef '- 1_new_ccdc809267.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 ; ? ; #--------------------------------------------------------------- # _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 14.1659(4) _cell_length_b 15.1150(4) _cell_length_c 15.5887(4) _cell_angle_alpha 73.0800(10) _cell_angle_beta 64.4580(10) _cell_angle_gamma 88.402(2) _cell_volume 2862.77(14) _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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 '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' 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' 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' 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' 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' _cell_formula_units_Z 1 _chemical_formula_sum 'C102 H114 K3 Mo N20 Ni4 O16 S6 ' _chemical_formula_moiety 'C88 H102 K3 N10 Ni4 O16, C6 Mo N6 S6, 4(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 2516.62 _cell_measurement_reflns_used 9382 _cell_measurement_theta_min 3 _cell_measurement_theta_max 34 _cell_measurement_temperature 180 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1301 _exptl_absorpt_coefficient_mu 1.040 # Sheldrick geometric approximatio 0.81 0.81 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.81 _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 'SHELXS 86 (Sheldrick, 1986)' _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 81299 _reflns_number_total 22734 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections without Friedels Law is 22734 # Number of reflections with Friedels Law is 22734 # Theoretical number of reflections is about 25763 _diffrn_reflns_theta_min 1.417 _diffrn_reflns_theta_max 35.291 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 28.586 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -20 _reflns_limit_h_max 22 _reflns_limit_k_min -23 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.35 _refine_diff_density_max 1.06 # 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>3.0\s(I) _refine_ls_number_reflns 15993 _refine_ls_number_restraints 0 _refine_ls_number_parameters 667 _oxford_refine_ls_R_factor_ref 0.0366 _refine_ls_wR_factor_ref 0.0386 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0005648 _refine_ls_shift/su_mean 0.0000260 # The values computed from all data _oxford_reflns_number_all 22698 _refine_ls_R_factor_all 0.0597 _refine_ls_wR_factor_all 0.0809 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 16964 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_gt 0.0403 # 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 # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. 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. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. 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 Mo1 Mo 0.5000 -0.5000 1.0000 0.0210 1.0000 Uani S . . . . . Ni1 Ni 0.17494(2) 0.165797(17) 0.762411(19) 0.0197 1.0000 Uani . . . . . . Ni2 Ni 0.360336(19) 0.038952(17) 0.557184(18) 0.0182 1.0000 Uani . . . . . . C1 C 0.57853(16) -0.70547(14) 1.00953(16) 0.0260 1.0000 Uani . . . . . . C2 C 0.2575(2) -0.58493(19) 1.1566(2) 0.0394 1.0000 Uani . . . . . . C3 C 0.46463(17) -0.48286(14) 0.80240(17) 0.0261 1.0000 Uani . . . . . . C4 C 0.20504(19) -0.05759(16) 1.12433(17) 0.0298 1.0000 Uani . . . . . . C5 C 0.24928(16) 0.09018(15) 0.99953(16) 0.0241 1.0000 Uani . . . . . . C6 C 0.29331(18) 0.12775(17) 1.04646(18) 0.0312 1.0000 Uani . . . . . . C7 C 0.3449(2) 0.21865(18) 1.0013(2) 0.0381 1.0000 Uani . . . . . . C8 C 0.3536(2) 0.26921(18) 0.9099(2) 0.0378 1.0000 Uani . . . . . . C9 C 0.30666(17) 0.23334(15) 0.86130(18) 0.0284 1.0000 Uani . . . . . . C10 C 0.25243(15) 0.14293(14) 0.90644(15) 0.0224 1.0000 Uani . . . . . . C11 C 0.32272(18) 0.28670(15) 0.76271(18) 0.0304 1.0000 Uani . . . . . . C12 C 0.30953(17) 0.32376(15) 0.60933(17) 0.0305 1.0000 Uani . . . . . . C13 C 0.11601(17) 0.33046(14) 0.66502(17) 0.0289 1.0000 Uani . . . . . . C14 C 0.06210(16) 0.19183(15) 0.64726(15) 0.0255 1.0000 Uani . . . . . . C15 C 0.04018(15) 0.09360(15) 0.66846(15) 0.0233 1.0000 Uani . . . . . . C16 C -0.00808(17) 0.06213(17) 0.61857(16) 0.0300 1.0000 Uani . . . . . . C17 C -0.04094(18) -0.03022(18) 0.64593(18) 0.0332 1.0000 Uani . . . . . . C18 C -0.03101(17) -0.09446(16) 0.72657(17) 0.0288 1.0000 Uani . . . . . . C19 C 0.01431(16) -0.06505(14) 0.77730(15) 0.0232 1.0000 Uani . . . . . . C20 C 0.05481(15) 0.03001(14) 0.74710(14) 0.0208 1.0000 Uani . . . . . . C21 C -0.02592(19) -0.21345(15) 0.89979(19) 0.0317 1.0000 Uani . . . . . . C22 C 0.2317(3) 0.47497(18) 0.6143(3) 0.0529 1.0000 Uani . . . . . . C23 C 0.2439(2) 0.4015(2) 0.48497(19) 0.0470 1.0000 Uani . . . . . . C24 C 0.2494(2) -0.32215(16) 0.85941(19) 0.0394 1.0000 Uani . . . . . . C25 C 0.22543(16) -0.22918(14) 0.71944(16) 0.0249 1.0000 Uani . . . . . . C26 C 0.17601(18) -0.30341(15) 0.71404(18) 0.0316 1.0000 Uani . . . . . . C27 C 0.14312(19) -0.29181(16) 0.6392(2) 0.0346 1.0000 Uani . . . . . . C29 C 0.21295(16) -0.12968(14) 0.57258(16) 0.0241 1.0000 Uani . . . . . . C30 C 0.24629(15) -0.13955(13) 0.64762(15) 0.0217 1.0000 Uani . . . . . . C31 C 0.22120(16) -0.03911(14) 0.50550(16) 0.0245 1.0000 Uani . . . . . . C32 C 0.26469(15) 0.12492(14) 0.43344(14) 0.0220 1.0000 Uani . . . . . . C33 C 0.36297(16) 0.16284(14) 0.33342(14) 0.0231 1.0000 Uani . . . . . . C34 C 0.46102(16) 0.13495(15) 0.34812(14) 0.0235 1.0000 Uani . . . . . . C35 C 0.51121(15) 0.19702(13) 0.44739(14) 0.0216 1.0000 Uani . . . . . . C36 C 0.52238(15) 0.20072(13) 0.53343(15) 0.0216 1.0000 Uani . . . . . . C37 C 0.58607(18) 0.27704(16) 0.52239(18) 0.0307 1.0000 Uani . . . . . . C38 C 0.6077(2) 0.27979(18) 0.5989(2) 0.0380 1.0000 Uani . . . . . . C39 C 0.56843(19) 0.20537(17) 0.68822(18) 0.0328 1.0000 Uani . . . . . . C40 C 0.50623(16) 0.12977(14) 0.70046(15) 0.0236 1.0000 Uani . . . . . . C41 C 0.47917(15) 0.12602(13) 0.62355(14) 0.0203 1.0000 Uani . . . . . . C42 C 0.5027(2) 0.05011(17) 0.85808(18) 0.0338 1.0000 Uani . . . . . . C43 C 0.3677(2) 0.26882(16) 0.29715(18) 0.0347 1.0000 Uani . . . . . . C44 C 0.3572(2) 0.1211(2) 0.25714(18) 0.0383 1.0000 Uani . . . . . . C45 C -0.1251(2) 0.3529(2) 0.8686(2) 0.0448 1.0000 Uani . . . . . . C46 C -0.1012(2) 0.2624(2) 0.9155(2) 0.0403 1.0000 Uani . . . . . . C49 C 0.1795(3) -0.5629(2) 0.9830(3) 0.0610 1.0000 Uani . . . . . . C50 C 0.1182(3) -0.5591(2) 0.9297(3) 0.0593 1.0000 Uani . . . . . . C67 C 0.22551(19) 0.38298(15) 0.59325(17) 0.0312 1.0000 Uani . . . . . . N1 N 0.54606(15) -0.63427(12) 1.00916(14) 0.0270 1.0000 Uani . . . . . . N2 N 0.34264(15) -0.55452(13) 1.09734(15) 0.0293 1.0000 Uani . . . . . . N3 N 0.47484(15) -0.49343(12) 0.87478(14) 0.0273 1.0000 Uani . . . . . . N4 N 0.27522(14) 0.26792(12) 0.71449(14) 0.0257 1.0000 Uani . . . . . . N5 N 0.11397(13) 0.22953(12) 0.68077(13) 0.0236 1.0000 Uani . . . . . . N6 N 0.27551(13) 0.03403(11) 0.49416(12) 0.0206 1.0000 Uani . . . . . . N7 N 0.45086(12) 0.13578(11) 0.44602(12) 0.0201 1.0000 Uani . . . . . . N8 N -0.0823(2) 0.1917(2) 0.9515(2) 0.0532 1.0000 Uani . . . . . . N10 N 0.0718(4) -0.5564(3) 0.8866(4) 0.1269 1.0000 Uani . . . . . . O1 O 0.19990(13) 0.00125(11) 1.03642(12) 0.0285 1.0000 Uani . . . . . . O2 O 0.20662(11) 0.10377(9) 0.86668(11) 0.0223 1.0000 Uani . . . . . . O3 O 0.09835(11) 0.05324(10) 0.79778(10) 0.0223 1.0000 Uani . . . . . . O4 O 0.02476(13) -0.12009(10) 0.85883(12) 0.0286 1.0000 Uani . . . . . . O5 O 0.25921(13) -0.23255(10) 0.79059(12) 0.0303 1.0000 Uani . . . . . . O6 O 0.29288(12) -0.07173(10) 0.65735(11) 0.0233 1.0000 Uani . . . . . . O7 O 0.41844(12) 0.05317(10) 0.63950(11) 0.0232 1.0000 Uani . . . . . . O8 O 0.46584(13) 0.05366(11) 0.78507(11) 0.0284 1.0000 Uani . . . . . . K1 K 0.0000 0.0000 1.0000 0.0299 1.0000 Uani S . . . . . K2 K 0.27207(5) -0.05943(3) 0.83071(4) 0.0341 1.0000 Uani . . . . . . S1 S 0.62598(6) -0.80400(4) 1.00585(6) 0.0453 1.0000 Uani . . . . . . S2 S 0.13808(7) -0.62739(9) 1.23927(8) 0.0866 1.0000 Uani . . . . . . S3 S 0.44856(6) -0.46947(5) 0.70248(5) 0.0383 1.0000 Uani . . . . . . C28 C 0.16122(18) -0.20616(15) 0.56946(19) 0.0312 1.0000 Uani . . . . . . C47 C 0.6910(3) 0.3956(3) 0.7439(3) 0.0588(8) 1.0000 Uiso . . . . . . C48 C 0.7712(4) 0.3453(3) 0.6918(3) 0.0676(11) 0.5000 Uiso . . . . . . C480 C 0.7847(4) 0.3628(3) 0.6873(3) 0.0676(11) 0.5000 Uiso . . . . . . N9 N 0.8313(5) 0.2997(5) 0.6523(4) 0.0976(18) 0.5000 Uiso . . . . . . N90 N 0.8616(5) 0.3397(5) 0.6405(4) 0.0976(18) 0.5000 Uiso . . . . . . H41 H 0.1702 -0.1176 1.1403 0.0483 1.0000 Uiso R . . . . . H43 H 0.2786 -0.0627 1.1096 0.0469 1.0000 Uiso R . . . . . H42 H 0.1715 -0.0317 1.1786 0.0467 1.0000 Uiso R . . . . . H61 H 0.2898 0.0926 1.1086 0.0426 1.0000 Uiso R . . . . . H71 H 0.3748 0.2442 1.0336 0.0508 1.0000 Uiso R . . . . . H81 H 0.3920 0.3287 0.8770 0.0492 1.0000 Uiso R . . . . . H111 H 0.3745 0.3385 0.7288 0.0367 1.0000 Uiso R . . . . . H121 H 0.3248 0.2803 0.5701 0.0317 1.0000 Uiso R . . . . . H122 H 0.3746 0.3635 0.5857 0.0323 1.0000 Uiso R . . . . . H132 H 0.0673 0.3530 0.6386 0.0319 1.0000 Uiso R . . . . . H131 H 0.0949 0.3397 0.7298 0.0324 1.0000 Uiso R . . . . . H141 H 0.0332 0.2315 0.6084 0.0291 1.0000 Uiso R . . . . . H161 H -0.0188 0.1061 0.5672 0.0379 1.0000 Uiso R . . . . . H171 H -0.0724 -0.0506 0.6113 0.0430 1.0000 Uiso R . . . . . H181 H -0.0550 -0.1576 0.7453 0.0379 1.0000 Uiso R . . . . . H211 H 0.0078 -0.2473 0.8525 0.0475 1.0000 Uiso R . . . . . H213 H -0.0190 -0.2412 0.9595 0.0482 1.0000 Uiso R . . . . . H212 H -0.1006 -0.2117 0.9156 0.0476 1.0000 Uiso R . . . . . H221 H 0.2959 0.5120 0.5666 0.0775 1.0000 Uiso R . . . . . H223 H 0.1754 0.5072 0.6090 0.0774 1.0000 Uiso R . . . . . H222 H 0.2239 0.4634 0.6819 0.0775 1.0000 Uiso R . . . . . H231 H 0.1972 0.4444 0.4733 0.0606 1.0000 Uiso R . . . . . H232 H 0.3177 0.4280 0.4401 0.0610 1.0000 Uiso R . . . . . H233 H 0.2310 0.3429 0.4745 0.0612 1.0000 Uiso R . . . . . H242 H 0.2828 -0.3157 0.9003 0.0552 1.0000 Uiso R . . . . . H241 H 0.2856 -0.3655 0.8231 0.0549 1.0000 Uiso R . . . . . H243 H 0.1743 -0.3455 0.9021 0.0545 1.0000 Uiso R . . . . . H261 H 0.1644 -0.3618 0.7617 0.0353 1.0000 Uiso R . . . . . H271 H 0.1086 -0.3427 0.6375 0.0425 1.0000 Uiso R . . . . . H281 H 0.1380 -0.1978 0.5183 0.0400 1.0000 Uiso R . . . . . H311 H 0.1807 -0.0319 0.4690 0.0304 1.0000 Uiso R . . . . . H321 H 0.2545 0.1685 0.4722 0.0257 1.0000 Uiso R . . . . . H322 H 0.2038 0.1199 0.4211 0.0250 1.0000 Uiso R . . . . . H341 H 0.5226 0.1776 0.2946 0.0276 1.0000 Uiso R . . . . . H342 H 0.4732 0.0720 0.3448 0.0277 1.0000 Uiso R . . . . . H351 H 0.5539 0.2422 0.3856 0.0253 1.0000 Uiso R . . . . . H371 H 0.6155 0.3256 0.4599 0.0368 1.0000 Uiso R . . . . . H381 H 0.6509 0.3313 0.5919 0.0452 1.0000 Uiso R . . . . . H391 H 0.5848 0.2074 0.7405 0.0416 1.0000 Uiso R . . . . . H422 H 0.4787 0.1005 0.8868 0.0544 1.0000 Uiso R . . . . . H421 H 0.4725 -0.0090 0.9104 0.0546 1.0000 Uiso R . . . . . H423 H 0.5800 0.0527 0.8267 0.0543 1.0000 Uiso R . . . . . H432 H 0.4227 0.2927 0.2306 0.0479 1.0000 Uiso R . . . . . H431 H 0.3002 0.2854 0.3000 0.0477 1.0000 Uiso R . . . . . H433 H 0.3814 0.2944 0.3415 0.0476 1.0000 Uiso R . . . . . H442 H 0.4217 0.1381 0.1972 0.0603 1.0000 Uiso R . . . . . H441 H 0.2989 0.1427 0.2434 0.0604 1.0000 Uiso R . . . . . H443 H 0.3474 0.0540 0.2829 0.0602 1.0000 Uiso R . . . . . H451 H -0.1961 0.3587 0.9079 0.0638 1.0000 Uiso R . . . . . H452 H -0.1146 0.3560 0.8032 0.0643 1.0000 Uiso R . . . . . H453 H -0.0797 0.4002 0.8663 0.0646 1.0000 Uiso R . . . . . H491 H 0.2475 -0.5270 0.9386 0.0984 1.0000 Uiso R . . . . . H493 H 0.1420 -0.5371 1.0372 0.0990 1.0000 Uiso R . . . . . H492 H 0.1920 -0.6264 1.0081 0.0981 1.0000 Uiso R . . . . . H474 H 0.7149 0.4579 0.7219 0.0703 0.5000 Uiso . . . . . . H473 H 0.6315 0.3884 0.7335 0.0703 0.5000 Uiso . . . . . . H475 H 0.6713 0.3713 0.8125 0.0703 0.5000 Uiso . . . . . . H472 H 0.6330 0.3525 0.7640 0.0703 0.5000 Uiso . . . . . . H471 H 0.6825 0.4524 0.7063 0.0703 0.5000 Uiso . . . . . . H476 H 0.6929 0.4016 0.8008 0.0703 0.5000 Uiso . . . . . . 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 0.02245(11) 0.01638(10) 0.02554(11) -0.00412(8) -0.01335(9) 0.00096(8) Ni1 0.01968(11) 0.01619(10) 0.02175(11) -0.00403(8) -0.00890(9) -0.00039(8) Ni2 0.01869(11) 0.01650(10) 0.01890(10) -0.00291(8) -0.00924(9) -0.00018(8) C1 0.0225(9) 0.0225(9) 0.0281(9) -0.0042(7) -0.0089(7) 0.0003(7) C2 0.0280(11) 0.0424(14) 0.0419(13) -0.0007(11) -0.0180(10) 0.0024(10) C3 0.0272(9) 0.0183(8) 0.0330(10) -0.0048(7) -0.0154(8) -0.0006(7) C4 0.0338(11) 0.0332(11) 0.0281(10) -0.0102(8) -0.0185(9) 0.0069(9) C5 0.0232(9) 0.0265(9) 0.0296(9) -0.0135(8) -0.0148(8) 0.0038(7) C6 0.0305(10) 0.0378(12) 0.0361(11) -0.0183(10) -0.0199(9) 0.0038(9) C7 0.0384(13) 0.0389(13) 0.0529(15) -0.0257(12) -0.0269(12) 0.0005(10) C8 0.0366(12) 0.0306(11) 0.0540(15) -0.0176(11) -0.0237(11) -0.0054(9) C9 0.0275(10) 0.0239(9) 0.0378(11) -0.0123(8) -0.0159(9) -0.0018(7) C10 0.0210(8) 0.0216(8) 0.0290(9) -0.0117(7) -0.0124(7) 0.0016(7) C11 0.0272(10) 0.0207(9) 0.0408(12) -0.0085(8) -0.0132(9) -0.0043(7) C12 0.0256(10) 0.0229(9) 0.0305(10) -0.0015(8) -0.0053(8) -0.0026(7) C13 0.0274(10) 0.0215(9) 0.0305(10) -0.0050(8) -0.0083(8) 0.0067(7) C14 0.0210(8) 0.0284(10) 0.0229(9) -0.0024(7) -0.0095(7) 0.0035(7) C15 0.0204(8) 0.0279(9) 0.0208(8) -0.0053(7) -0.0097(7) 0.0015(7) C16 0.0260(10) 0.0419(12) 0.0252(9) -0.0084(9) -0.0154(8) 0.0033(9) C17 0.0291(10) 0.0475(14) 0.0338(11) -0.0182(10) -0.0199(9) 0.0030(9) C18 0.0270(10) 0.0316(10) 0.0356(11) -0.0162(9) -0.0170(9) 0.0019(8) C19 0.0219(8) 0.0247(9) 0.0263(9) -0.0096(7) -0.0124(7) 0.0027(7) C20 0.0188(8) 0.0238(8) 0.0198(8) -0.0067(7) -0.0085(6) 0.0007(6) C21 0.0324(11) 0.0201(9) 0.0419(12) -0.0070(8) -0.0173(10) -0.0014(8) C22 0.0548(18) 0.0234(11) 0.074(2) -0.0137(13) -0.0231(16) 0.0026(11) C23 0.0443(15) 0.0453(15) 0.0310(12) 0.0053(11) -0.0092(11) 0.0043(12) C24 0.0504(15) 0.0236(10) 0.0343(12) 0.0025(9) -0.0170(11) 0.0028(10) C25 0.0230(9) 0.0184(8) 0.0272(9) -0.0048(7) -0.0070(7) 0.0005(7) C26 0.0296(10) 0.0183(9) 0.0390(12) -0.0061(8) -0.0096(9) -0.0016(7) C27 0.0324(11) 0.0228(10) 0.0495(14) -0.0143(9) -0.0167(10) -0.0011(8) C29 0.0221(9) 0.0209(8) 0.0312(10) -0.0092(7) -0.0128(8) 0.0020(7) C30 0.0187(8) 0.0186(8) 0.0250(9) -0.0058(7) -0.0079(7) 0.0007(6) C31 0.0229(9) 0.0249(9) 0.0292(10) -0.0095(7) -0.0140(8) 0.0031(7) C32 0.0217(8) 0.0226(8) 0.0222(8) -0.0051(7) -0.0115(7) 0.0043(7) C33 0.0260(9) 0.0244(9) 0.0186(8) -0.0046(7) -0.0110(7) 0.0022(7) C34 0.0216(8) 0.0279(9) 0.0191(8) -0.0069(7) -0.0074(7) 0.0032(7) C35 0.0170(8) 0.0208(8) 0.0222(8) -0.0020(6) -0.0073(6) 0.0020(6) C36 0.0188(8) 0.0201(8) 0.0252(9) -0.0047(7) -0.0106(7) 0.0008(6) C37 0.0312(11) 0.0255(10) 0.0324(11) -0.0020(8) -0.0153(9) -0.0070(8) C38 0.0418(13) 0.0326(11) 0.0399(13) -0.0047(10) -0.0214(11) -0.0133(10) C39 0.0359(12) 0.0335(11) 0.0334(11) -0.0079(9) -0.0204(10) -0.0059(9) C40 0.0234(9) 0.0235(9) 0.0260(9) -0.0071(7) -0.0130(7) 0.0019(7) C41 0.0188(8) 0.0192(8) 0.0242(8) -0.0067(6) -0.0107(7) 0.0028(6) C42 0.0429(13) 0.0355(12) 0.0290(11) -0.0078(9) -0.0226(10) 0.0013(10) C43 0.0357(12) 0.0277(11) 0.0312(11) 0.0024(8) -0.0135(9) 0.0020(9) C44 0.0383(13) 0.0546(16) 0.0263(11) -0.0178(11) -0.0146(10) 0.0023(11) C45 0.0357(13) 0.0542(17) 0.0387(14) -0.0077(12) -0.0154(11) 0.0058(12) C46 0.0360(13) 0.0531(16) 0.0406(13) -0.0216(12) -0.0203(11) 0.0055(11) C49 0.066(2) 0.0361(15) 0.088(3) -0.0052(16) -0.050(2) 0.0005(14) C50 0.067(2) 0.0437(17) 0.063(2) 0.0016(15) -0.0350(18) -0.0155(15) C67 0.0326(11) 0.0189(9) 0.0310(10) -0.0016(8) -0.0080(9) 0.0016(8) N1 0.0294(9) 0.0218(8) 0.0303(9) -0.0062(7) -0.0148(7) 0.0029(6) N2 0.0261(8) 0.0276(9) 0.0333(9) -0.0040(7) -0.0156(7) 0.0004(7) N3 0.0300(9) 0.0222(8) 0.0329(9) -0.0066(7) -0.0178(8) 0.0010(7) N4 0.0224(8) 0.0190(7) 0.0304(9) -0.0045(6) -0.0088(7) -0.0011(6) N5 0.0217(7) 0.0204(7) 0.0227(7) -0.0027(6) -0.0069(6) 0.0027(6) N6 0.0191(7) 0.0208(7) 0.0211(7) -0.0050(6) -0.0093(6) 0.0017(6) N7 0.0180(7) 0.0210(7) 0.0191(7) -0.0040(6) -0.0077(6) 0.0024(5) N8 0.0606(17) 0.0510(15) 0.0705(18) -0.0271(14) -0.0441(15) 0.0123(13) N10 0.153(4) 0.112(4) 0.135(4) 0.018(3) -0.112(4) -0.049(3) O1 0.0355(8) 0.0260(7) 0.0297(7) -0.0063(6) -0.0207(7) -0.0010(6) O2 0.0261(7) 0.0181(6) 0.0271(7) -0.0073(5) -0.0151(6) -0.0017(5) O3 0.0274(7) 0.0197(6) 0.0221(6) -0.0041(5) -0.0142(6) -0.0030(5) O4 0.0370(8) 0.0192(6) 0.0341(8) -0.0037(6) -0.0222(7) -0.0032(6) O5 0.0374(8) 0.0205(7) 0.0276(7) -0.0003(6) -0.0139(7) -0.0009(6) O6 0.0274(7) 0.0181(6) 0.0228(6) -0.0022(5) -0.0118(6) -0.0039(5) O7 0.0276(7) 0.0184(6) 0.0242(7) -0.0018(5) -0.0147(6) -0.0030(5) O8 0.0348(8) 0.0270(7) 0.0260(7) -0.0032(6) -0.0188(6) -0.0022(6) K1 0.0259(3) 0.0364(3) 0.0227(3) -0.0072(2) -0.0074(2) -0.0016(2) K2 0.0432(3) 0.0257(2) 0.0307(2) -0.00794(18) -0.0145(2) 0.00483(19) S1 0.0363(3) 0.0237(3) 0.0632(4) -0.0110(3) -0.0125(3) 0.0106(2) S2 0.0254(3) 0.1166(9) 0.0716(6) 0.0159(6) -0.0078(4) -0.0087(5) S3 0.0514(4) 0.0359(3) 0.0346(3) -0.0055(2) -0.0280(3) -0.0041(3) C28 0.0313 0.0246 0.0451 -0.0149 -0.0208 0.0020 _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 Mo1 . N3 2_647 2.1053(19) yes Mo1 . N2 2_647 2.0996(19) yes Mo1 . N1 2_647 2.0982(18) yes Mo1 . N1 . 2.0982(18) yes Mo1 . N2 . 2.0996(19) yes Mo1 . N3 . 2.1053(19) yes Ni1 . N4 . 1.8694(17) yes Ni1 . N5 . 1.8658(17) yes Ni1 . O2 . 1.8550(14) yes Ni1 . O3 . 1.8484(14) yes Ni2 . N6 . 1.8655(16) yes Ni2 . N7 . 1.8712(16) yes Ni2 . O6 . 1.8526(14) yes Ni2 . O7 . 1.8578(14) yes C1 . N1 . 1.158(3) yes C1 . S1 . 1.623(2) yes C2 . N2 . 1.158(3) yes C2 . S2 . 1.623(3) yes C3 . N3 . 1.164(3) yes C3 . S3 . 1.624(2) yes C4 . O1 . 1.431(3) yes C4 . H41 . 0.957 no C4 . H43 . 0.972 no C4 . H42 . 0.965 no C5 . C6 . 1.379(3) yes C5 . C10 . 1.420(3) yes C5 . O1 . 1.372(3) yes C6 . C7 . 1.403(3) yes C6 . H61 . 0.941 no C7 . C8 . 1.360(4) yes C7 . H71 . 0.943 no C8 . C9 . 1.415(3) yes C8 . H81 . 0.941 no C9 . C10 . 1.409(3) yes C9 . C11 . 1.432(3) yes C10 . O2 . 1.318(2) yes C11 . N4 . 1.292(3) yes C11 . H111 . 0.942 no C12 . C67 . 1.532(3) yes C12 . N4 . 1.472(3) yes C12 . H121 . 0.981 no C12 . H122 . 0.977 no C13 . C67 . 1.531(3) yes C13 . N5 . 1.472(3) yes C13 . H132 . 0.954 no C13 . H131 . 0.974 no C14 . C15 . 1.436(3) yes C14 . N5 . 1.290(3) yes C14 . H141 . 0.940 no C15 . C16 . 1.411(3) yes C15 . C20 . 1.411(3) yes C16 . C17 . 1.366(3) yes C16 . H161 . 0.946 no C17 . C18 . 1.406(3) yes C17 . H171 . 0.948 no C18 . C19 . 1.376(3) yes C18 . H181 . 0.939 no C19 . C20 . 1.426(3) yes C19 . O4 . 1.367(2) yes C20 . O3 . 1.312(2) yes C21 . O4 . 1.432(2) yes C21 . H211 . 0.968 no C21 . H213 . 0.949 no C21 . H212 . 0.979 no C22 . C67 . 1.531(4) yes C22 . H221 . 0.947 no C22 . H223 . 0.945 no C22 . H222 . 0.973 no C23 . C67 . 1.532(4) yes C23 . H231 . 0.950 no C23 . H232 . 0.986 no C23 . H233 . 0.982 no C24 . O5 . 1.428(3) yes C24 . H242 . 0.968 no C24 . H241 . 0.980 no C24 . H243 . 0.986 no C25 . C26 . 1.380(3) yes C25 . C30 . 1.425(3) yes C25 . O5 . 1.373(3) yes C26 . C27 . 1.398(4) yes C26 . H261 . 0.937 no C27 . C28 . 1.372(3) yes C27 . H271 . 0.937 no C29 . C30 . 1.409(3) yes C29 . C31 . 1.432(3) yes C29 . C28 . 1.409(3) yes C30 . O6 . 1.313(2) yes C31 . N6 . 1.289(3) yes C31 . H311 . 0.952 no C32 . C33 . 1.533(3) yes C32 . N6 . 1.471(2) yes C32 . H321 . 0.985 no C32 . H322 . 0.971 no C33 . C34 . 1.531(3) yes C33 . C43 . 1.528(3) yes C33 . C44 . 1.531(3) yes C34 . N7 . 1.474(3) yes C34 . H341 . 0.981 no C34 . H342 . 0.974 no C35 . C36 . 1.433(3) yes C35 . N7 . 1.288(2) yes C35 . H351 . 0.948 no C36 . C37 . 1.408(3) yes C36 . C41 . 1.413(3) yes C37 . C38 . 1.365(3) yes C37 . H371 . 0.954 no C38 . C39 . 1.403(3) yes C38 . H381 . 0.954 no C39 . C40 . 1.379(3) yes C39 . H391 . 0.946 no C40 . C41 . 1.423(3) yes C40 . O8 . 1.376(2) yes C41 . O7 . 1.313(2) yes C42 . O8 . 1.431(3) yes C42 . H422 . 0.974 no C42 . H421 . 0.971 no C42 . H423 . 0.984 no C43 . H432 . 0.956 no C43 . H431 . 0.968 no C43 . H433 . 0.971 no C44 . H442 . 0.954 no C44 . H441 . 0.965 no C44 . H443 . 0.965 no C45 . C46 . 1.458(4) yes C45 . H451 . 0.944 no C45 . H452 . 0.951 no C45 . H453 . 0.958 no C46 . N8 . 1.137(4) yes C49 . C50 . 1.428(5) yes C49 . H491 . 0.968 no C49 . H493 . 0.970 no C49 . H492 . 0.968 no C50 . N10 . 1.118(5) yes C28 . H281 . 0.962 no C47 . C48 . 1.430(6) yes C47 . C480 . 1.413(6) yes C47 . H474 . 0.921 no C47 . H473 . 0.939 no C47 . H475 . 0.935 no C47 . H472 . 0.942 no C47 . H471 . 0.926 no C47 . H476 . 0.929 no C48 . N9 . 1.158(6) yes C480 . N90 . 1.132(6) 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 N3 2_647 Mo1 . N2 2_647 91.20(7) yes N3 2_647 Mo1 . N1 2_647 91.36(7) yes N2 2_647 Mo1 . N1 2_647 91.24(7) yes N3 2_647 Mo1 . N1 . 88.64(7) yes N2 2_647 Mo1 . N1 . 88.76(7) yes N1 2_647 Mo1 . N1 . 179.995 yes N3 2_647 Mo1 . N2 . 88.80(7) yes N2 2_647 Mo1 . N2 . 179.995 yes N1 2_647 Mo1 . N2 . 88.76(7) yes N1 . Mo1 . N2 . 91.24(7) yes N3 2_647 Mo1 . N3 . 179.995 yes N2 2_647 Mo1 . N3 . 88.80(7) yes N1 2_647 Mo1 . N3 . 88.64(7) yes N1 . Mo1 . N3 . 91.36(7) yes N2 . Mo1 . N3 . 91.20(7) yes N4 . Ni1 . N5 . 91.17(8) yes N4 . Ni1 . O2 . 94.24(7) yes N5 . Ni1 . O2 . 167.07(7) yes N4 . Ni1 . O3 . 168.71(7) yes N5 . Ni1 . O3 . 93.61(7) yes O2 . Ni1 . O3 . 83.26(6) yes N6 . Ni2 . N7 . 90.41(7) yes N6 . Ni2 . O6 . 92.70(7) yes N7 . Ni2 . O6 . 168.12(7) yes N6 . Ni2 . O7 . 167.03(7) yes N7 . Ni2 . O7 . 94.62(7) yes O6 . Ni2 . O7 . 84.80(6) yes N1 . C1 . S1 . 178.0(2) yes N2 . C2 . S2 . 179.7(2) yes N3 . C3 . S3 . 179.0(2) yes O1 . C4 . H41 . 107.6 no O1 . C4 . H43 . 108.5 no H41 . C4 . H43 . 109.5 no O1 . C4 . H42 . 110.0 no H41 . C4 . H42 . 110.9 no H43 . C4 . H42 . 110.4 no C6 . C5 . C10 . 121.1(2) yes C6 . C5 . O1 . 124.5(2) yes C10 . C5 . O1 . 114.41(17) yes C5 . C6 . C7 . 120.2(2) yes C5 . C6 . H61 . 120.5 no C7 . C6 . H61 . 119.2 no C6 . C7 . C8 . 119.9(2) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 121.0(2) yes C7 . C8 . H81 . 120.6 no C9 . C8 . H81 . 118.4 no C8 . C9 . C10 . 119.9(2) yes C8 . C9 . C11 . 119.2(2) yes C10 . C9 . C11 . 120.68(19) yes C5 . C10 . C9 . 117.68(18) yes C5 . C10 . O2 . 118.17(17) yes C9 . C10 . O2 . 124.14(19) yes C9 . C11 . N4 . 125.66(19) yes C9 . C11 . H111 . 117.3 no N4 . C11 . H111 . 117.0 no C67 . C12 . N4 . 112.75(18) yes C67 . C12 . H121 . 108.9 no N4 . C12 . H121 . 107.3 no C67 . C12 . H122 . 110.1 no N4 . C12 . H122 . 109.6 no H121 . C12 . H122 . 108.1 no C67 . C13 . N5 . 112.59(17) yes C67 . C13 . H132 . 109.5 no N5 . C13 . H132 . 107.9 no C67 . C13 . H131 . 108.6 no N5 . C13 . H131 . 107.3 no H132 . C13 . H131 . 111.0 no C15 . C14 . N5 . 125.38(19) yes C15 . C14 . H141 . 116.9 no N5 . C14 . H141 . 117.7 no C14 . C15 . C16 . 119.28(19) yes C14 . C15 . C20 . 119.93(18) yes C16 . C15 . C20 . 120.33(19) yes C15 . C16 . C17 . 120.2(2) yes C15 . C16 . H161 . 119.0 no C17 . C16 . H161 . 120.7 no C16 . C17 . C18 . 120.5(2) yes C16 . C17 . H171 . 119.5 no C18 . C17 . H171 . 120.0 no C17 . C18 . C19 . 120.2(2) yes C17 . C18 . H181 . 119.6 no C19 . C18 . H181 . 120.2 no C18 . C19 . C20 . 120.73(19) yes C18 . C19 . O4 . 125.50(19) yes C20 . C19 . O4 . 113.77(17) yes C19 . C20 . C15 . 117.86(17) yes C19 . C20 . O3 . 117.68(17) yes C15 . C20 . O3 . 124.37(18) yes O4 . C21 . H211 . 109.7 no O4 . C21 . H213 . 107.1 no H211 . C21 . H213 . 110.4 no O4 . C21 . H212 . 109.0 no H211 . C21 . H212 . 111.1 no H213 . C21 . H212 . 109.5 no C67 . C22 . H221 . 110.4 no C67 . C22 . H223 . 108.0 no H221 . C22 . H223 . 108.8 no C67 . C22 . H222 . 110.5 no H221 . C22 . H222 . 110.9 no H223 . C22 . H222 . 108.1 no C67 . C23 . H231 . 107.7 no C67 . C23 . H232 . 108.7 no H231 . C23 . H232 . 110.5 no C67 . C23 . H233 . 109.8 no H231 . C23 . H233 . 111.0 no H232 . C23 . H233 . 109.1 no O5 . C24 . H242 . 108.0 no O5 . C24 . H241 . 110.1 no H242 . C24 . H241 . 108.5 no O5 . C24 . H243 . 109.8 no H242 . C24 . H243 . 109.9 no H241 . C24 . H243 . 110.5 no C26 . C25 . C30 . 120.8(2) yes C26 . C25 . O5 . 125.42(19) yes C30 . C25 . O5 . 113.74(17) yes C25 . C26 . C27 . 120.7(2) yes C25 . C26 . H261 . 118.9 no C27 . C26 . H261 . 120.4 no C26 . C27 . C28 . 119.8(2) yes C26 . C27 . H271 . 119.4 no C28 . C27 . H271 . 120.7 no C30 . C29 . C31 . 119.63(18) yes C30 . C29 . C28 . 120.70(19) yes C31 . C29 . C28 . 119.3(2) yes C25 . C30 . C29 . 117.44(18) yes C25 . C30 . O6 . 117.84(18) yes C29 . C30 . O6 . 124.70(18) yes C29 . C31 . N6 . 124.98(19) yes C29 . C31 . H311 . 117.3 no N6 . C31 . H311 . 117.6 no C33 . C32 . N6 . 112.27(16) yes C33 . C32 . H321 . 108.5 no N6 . C32 . H321 . 107.1 no C33 . C32 . H322 . 109.4 no N6 . C32 . H322 . 109.9 no H321 . C32 . H322 . 109.5 no C32 . C33 . C34 . 109.25(15) yes C32 . C33 . C43 . 108.68(17) yes C34 . C33 . C43 . 110.16(18) yes C32 . C33 . C44 . 109.46(18) yes C34 . C33 . C44 . 108.90(18) yes C43 . C33 . C44 . 110.37(19) yes C33 . C34 . N7 . 112.40(16) yes C33 . C34 . H341 . 109.3 no N7 . C34 . H341 . 109.6 no C33 . C34 . H342 . 110.3 no N7 . C34 . H342 . 106.9 no H341 . C34 . H342 . 108.3 no C36 . C35 . N7 . 125.74(17) yes C36 . C35 . H351 . 117.1 no N7 . C35 . H351 . 117.1 no C35 . C36 . C37 . 117.77(18) yes C35 . C36 . C41 . 120.98(17) yes C37 . C36 . C41 . 120.99(19) yes C36 . C37 . C38 . 120.3(2) yes C36 . C37 . H371 . 118.8 no C38 . C37 . H371 . 120.9 no C37 . C38 . C39 . 120.0(2) yes C37 . C38 . H381 . 120.7 no C39 . C38 . H381 . 119.3 no C38 . C39 . C40 . 120.7(2) yes C38 . C39 . H391 . 119.4 no C40 . C39 . H391 . 119.9 no C39 . C40 . C41 . 120.86(19) yes C39 . C40 . O8 . 124.18(19) yes C41 . C40 . O8 . 114.96(17) yes C40 . C41 . C36 . 117.15(17) yes C40 . C41 . O7 . 118.49(17) yes C36 . C41 . O7 . 124.34(18) yes O8 . C42 . H422 . 110.2 no O8 . C42 . H421 . 106.9 no H422 . C42 . H421 . 108.9 no O8 . C42 . H423 . 109.1 no H422 . C42 . H423 . 112.0 no H421 . C42 . H423 . 109.5 no C33 . C43 . H432 . 109.6 no C33 . C43 . H431 . 109.1 no H432 . C43 . H431 . 111.2 no C33 . C43 . H433 . 109.0 no H432 . C43 . H433 . 109.8 no H431 . C43 . H433 . 108.1 no C33 . C44 . H442 . 110.2 no C33 . C44 . H441 . 109.2 no H442 . C44 . H441 . 110.6 no C33 . C44 . H443 . 110.3 no H442 . C44 . H443 . 107.1 no H441 . C44 . H443 . 109.4 no C46 . C45 . H451 . 108.1 no C46 . C45 . H452 . 109.0 no H451 . C45 . H452 . 110.0 no C46 . C45 . H453 . 108.4 no H451 . C45 . H453 . 110.2 no H452 . C45 . H453 . 111.1 no C45 . C46 . N8 . 179.6(3) yes C50 . C49 . H491 . 109.9 no C50 . C49 . H493 . 108.2 no H491 . C49 . H493 . 109.9 no C50 . C49 . H492 . 110.3 no H491 . C49 . H492 . 107.3 no H493 . C49 . H492 . 111.1 no C49 . C50 . N10 . 178.7(6) yes C12 . C67 . C23 . 108.3(2) yes C12 . C67 . C22 . 110.5(2) yes C23 . C67 . C22 . 110.3(2) yes C12 . C67 . C13 . 109.57(17) yes C23 . C67 . C13 . 109.9(2) yes C22 . C67 . C13 . 108.3(2) yes Mo1 . N1 . C1 . 175.22(18) yes Mo1 . N2 . C2 . 175.1(2) yes Mo1 . N3 . C3 . 174.78(17) yes C12 . N4 . C11 . 118.75(18) yes C12 . N4 . Ni1 . 115.66(15) yes C11 . N4 . Ni1 . 125.21(15) yes C13 . N5 . C14 . 118.76(18) yes C13 . N5 . Ni1 . 115.04(15) yes C14 . N5 . Ni1 . 125.76(15) yes C32 . N6 . C31 . 118.87(17) yes C32 . N6 . Ni2 . 114.76(12) yes C31 . N6 . Ni2 . 126.14(14) yes C34 . N7 . C35 . 117.96(16) yes C34 . N7 . Ni2 . 116.29(13) yes C35 . N7 . Ni2 . 125.42(14) yes C4 . O1 . C5 . 116.21(16) yes C10 . O2 . Ni1 . 125.50(13) yes C20 . O3 . Ni1 . 126.09(12) yes C21 . O4 . C19 . 116.08(17) yes C24 . O5 . C25 . 116.52(18) yes C30 . O6 . Ni2 . 124.93(13) yes C41 . O7 . Ni2 . 126.17(12) yes C42 . O8 . C40 . 115.99(17) yes C29 . C28 . C27 . 120.5(2) yes C29 . C28 . H281 . 119.5 no C27 . C28 . H281 . 120.0 no C48 . C47 . H474 . 110.5 no C480 . C47 . H474 . 98.9 no C48 . C47 . H473 . 109.6 no C480 . C47 . H473 . 118.5 no H474 . C47 . H473 . 109.5 no C48 . C47 . H475 . 109.2 no C480 . C47 . H475 . 111.4 no H474 . C47 . H475 . 109.8 no H473 . C47 . H475 . 108.2 no C48 . C47 . H472 . 97.2 no C480 . C47 . H472 . 109.4 no H474 . C47 . H472 . 144.8 no H475 . C47 . H472 . 79.3 no C48 . C47 . H471 . 117.0 no C480 . C47 . H471 . 110.6 no H473 . C47 . H471 . 71.0 no H475 . C47 . H471 . 131.2 no C48 . C47 . H476 . 114.4 no C480 . C47 . H476 . 109.7 no H474 . C47 . H476 . 79.9 no H473 . C47 . H476 . 127.9 no H472 . C47 . H471 . 108.8 no H472 . C47 . H476 . 108.5 no H471 . C47 . H476 . 109.9 no C47 . C48 . N9 . 175.6(6) yes C47 . C480 . N90 . 177.5(6) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C34 . H342 . O7 2_656 145 0.97 2.43 3.276(4) yes C45 . H453 . N10 1_565 149 0.96 2.43 3.294(4) yes # 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 809268' #TrackingRef '- Compd_2new.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 ; ? ; #--------------------------------------------------------------- # _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 23.3664(8) _cell_length_b 37.452(2) _cell_length_c 12.1573(8) _cell_angle_alpha 90 _cell_angle_beta 105.626(6) _cell_angle_gamma 90 _cell_volume 10246.0(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1 ' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z x,-y,z -x+1/2,y+1/2,-z x+1/2,-y+1/2,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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 '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' 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' 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 4 # Given Formula = C85 H108 K2 Mo1 N17 Ni3 O14 S6 # Dc = 1.38 Fooo = 4420.00 Mu = 9.31 M = 1067.28 # Found Formula = C85 H104 K2 Mo1 N17 Ni3 O14 S6 # Dc = 1.38 FOOO = 4420.00 Mu = 9.30 M = 1065.26 _chemical_formula_sum 'C85 H108 K2 Mo1 N17 Ni3 O14 S6' _chemical_formula_moiety ; 3(C21 H24 N2 Ni1 O4),K2,(C8 H20 N),(C6 Mo N6 S6),4(C2 H3 N), 2(H2 O) ; _chemical_compound_source ? _chemical_formula_weight 2134.56 _cell_measurement_reflns_used 9586 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 180 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4420 _exptl_absorpt_coefficient_mu 0.931 # Sheldrick geometric approximatio 0.87 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.87 _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 '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 48950 _reflns_number_total 14120 _diffrn_reflns_av_R_equivalents 0.075 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 14120 # Theoretical number of reflections is about 27965 _diffrn_reflns_theta_min 2.829 _diffrn_reflns_theta_max 29.301 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.715 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -32 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 51 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.84 _refine_diff_density_max 1.80 # 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>1.8\s(I) _refine_ls_number_reflns 5855 _refine_ls_number_restraints 12 _refine_ls_number_parameters 582 _oxford_refine_ls_R_factor_ref 0.0639 _refine_ls_wR_factor_ref 0.0653 _refine_ls_goodness_of_fit_ref 1.0872 _refine_ls_shift/su_max 0.0099963 _refine_ls_shift/su_mean 0.0000640 # The values computed from all data _oxford_reflns_number_all 14088 _refine_ls_R_factor_all 0.1509 _refine_ls_wR_factor_all 0.1563 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5635 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_gt 0.0641 # 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: 0.436 0.460 0.192 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. 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. 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 Mo1 Mo 0.75302(5) 0.5000 0.28524(9) 0.0627 1.0000 Uani S T . . . . Ni1 Ni 0.68658(3) 0.754434(19) 0.07457(6) 0.0296 1.0000 Uani . . . . . . Ni2 Ni 0.5000 0.77089(3) 0.0000 0.0302 1.0000 Uani S T . . . . K1 K 0.57411(5) 0.68621(3) -0.03747(10) 0.0368 1.0000 Uani . . . . . . C1 C 0.8144(3) 0.55884(18) 0.1609(6) 0.0554 1.0000 Uani . . . . . . C2 C 0.8726(10) 0.5000 0.4787(18) 0.1062 1.0000 Uani S T . . . . C3 C 0.6931(4) 0.55773(19) 0.4153(7) 0.0670 1.0000 Uani . . . . . . C4 C 0.6454(6) 0.5000 0.0547(14) 0.0724 1.0000 Uani S T . . . . C5 C 0.6682(4) 0.60089(18) 0.0782(7) 0.0645 1.0000 Uani . . . . . . C6 C 0.7055(3) 0.65193(17) 0.1876(5) 0.0382 1.0000 Uani . . . . . . C7 C 0.7363(3) 0.63233(19) 0.2776(6) 0.0485 1.0000 Uani . . . . . . C8 C 0.7677(3) 0.6485(2) 0.3792(6) 0.0540 1.0000 Uani . . . . . . C9 C 0.7679(3) 0.6844(2) 0.3865(5) 0.0461 1.0000 Uani . . . . . . C10 C 0.7380(2) 0.70544(17) 0.2946(4) 0.0351 1.0000 Uani . . . . . . C11 C 0.7064(2) 0.68965(16) 0.1917(4) 0.0327 1.0000 Uani . . . . . . C12 C 0.7343(2) 0.74293(17) 0.3075(5) 0.0348 1.0000 Uani . . . . . . C13 C 0.7063(3) 0.80191(16) 0.2586(5) 0.0380 1.0000 Uani . . . . . . C14 C 0.7487(2) 0.82755(16) 0.2237(5) 0.0371 1.0000 Uani . . . . . . C15 C 0.7601(2) 0.81543(16) 0.1132(5) 0.0365 1.0000 Uani . . . . . . C16 C 0.6863(2) 0.81419(15) -0.0619(5) 0.0355 1.0000 Uani . . . . . . C17 C 0.6421(2) 0.80014(16) -0.1558(4) 0.0330 1.0000 Uani . . . . . . C18 C 0.6203(3) 0.82128(18) -0.2512(5) 0.0429 1.0000 Uani . . . . . . C19 C 0.5816(3) 0.80792(19) -0.3462(5) 0.0493 1.0000 Uani . . . . . . C20 C 0.5651(3) 0.7728(2) -0.3486(5) 0.0458 1.0000 Uani . . . . . . C21 C 0.5865(2) 0.75095(17) -0.2568(4) 0.0339 1.0000 Uani . . . . . . C22 C 0.6252(2) 0.76423(15) -0.1554(4) 0.0283 1.0000 Uani . . . . . . C23 C 0.5426(3) 0.6997(2) -0.3562(5) 0.0488 1.0000 Uani . . . . . . C24 C 0.8075(3) 0.82740(19) 0.3149(6) 0.0508 1.0000 Uani . . . . . . C25 C 0.7216(3) 0.86442(18) 0.2122(6) 0.0526 1.0000 Uani . . . . . . C26 C 0.4194(3) 0.6444(2) -0.2711(6) 0.0641 1.0000 Uani . . . . . . C27 C 0.4210(2) 0.70743(19) -0.2680(5) 0.0401 1.0000 Uani . . . . . . C28 C 0.3863(3) 0.7097(2) -0.3780(5) 0.0463 1.0000 Uani . . . . . . C29 C 0.3773(3) 0.7426(2) -0.4339(5) 0.0515 1.0000 Uani . . . . . . C30 C 0.4025(3) 0.7721(2) -0.3798(5) 0.0455 1.0000 Uani . . . . . . C31 C 0.4365(2) 0.77021(17) -0.2664(5) 0.0356 1.0000 Uani . . . . . . C32 C 0.4456(2) 0.73835(16) -0.2077(4) 0.0320 1.0000 Uani . . . . . . C33 C 0.4659(2) 0.80165(18) -0.2159(5) 0.0403 1.0000 Uani . . . . . . C34 C 0.5268(3) 0.83826(16) -0.0741(5) 0.0396 1.0000 Uani . . . . . . C35 C 0.5000 0.8618(2) 0.0000 0.0405 1.0000 Uani S T . . . . C36 C 0.5486(3) 0.8844(2) 0.0752(7) 0.0655 1.0000 Uani . . . . . . C37 C 0.9104(7) 0.5883(4) 0.4282(12) 0.1526 1.0000 Uani . . . . . . C38 C 0.9181(6) 0.6101(3) 0.5255(10) 0.1070 1.0000 Uani . . . . . . C39 C 0.5564(8) 0.5703(4) -0.3226(13) 0.1758 1.0000 Uani . . . . . . C40 C 0.5709(5) 0.6006(3) -0.2500(9) 0.0863 1.0000 Uani . . . . . . N1 N 0.7915(3) 0.53881(14) 0.2070(5) 0.0585 1.0000 Uani . . . . . . N2 N 0.8264(6) 0.5000 0.4178(12) 0.0824 1.0000 Uani S T . . . . N3 N 0.7149(3) 0.53854(16) 0.3657(6) 0.0737 1.0000 Uani . . . . . . N4 N 0.6795(5) 0.5000 0.1408(11) 0.0717 1.0000 Uani S T . . . . N5 N 0.71487(19) 0.76519(12) 0.2280(4) 0.0317 1.0000 Uani . . . . . . N6 N 0.70806(19) 0.79910(13) 0.0340(4) 0.0329 1.0000 Uani . . . . . . N7 N 0.4931(2) 0.80573(12) -0.1104(4) 0.0336 1.0000 Uani . . . . . . N8 N 0.9265(7) 0.6283(3) 0.5965(9) 0.1590 1.0000 Uani . . . . . . N9 N 0.5798(4) 0.6233(2) -0.1936(7) 0.0895 1.0000 Uani . . . . . . O1 O 0.67129(18) 0.63855(11) 0.0881(3) 0.0423 1.0000 Uani . . . . . . O2 O 0.67633(16) 0.70714(10) 0.1033(3) 0.0337 1.0000 Uani . . . . . . O3 O 0.64390(16) 0.74276(10) -0.0699(3) 0.0327 1.0000 Uani . . . . . . O4 O 0.57360(17) 0.71566(11) -0.2519(3) 0.0388 1.0000 Uani . . . . . . O5 O 0.43545(19) 0.67648(12) -0.2081(3) 0.0460 1.0000 Uani . . . . . . O6 O 0.47730(16) 0.73424(10) -0.1026(3) 0.0338 1.0000 Uani . . . . . . S1 S 0.84615(13) 0.58691(6) 0.0977(2) 0.0872 1.0000 Uani . . . . . . S2 S 0.9393(3) 0.5000 0.5680(6) 0.1808 1.0000 Uani S T . . . . S3 S 0.66442(15) 0.58476(6) 0.4888(2) 0.1040 1.0000 Uani . . . . . . S4 S 0.5952(2) 0.5000 -0.0669(5) 0.1218 1.0000 Uani S T . . . . C41 C 0.8378(13) 0.520594(10) 0.827(3) 0.158(11) 0.5000 Uiso D . . . . . C42 C 0.8488(15) 0.5464(9) 0.752(3) 0.162(13) 0.5000 Uiso D . . . . . C43 C 0.7834(11) 0.479726(10) 0.683(2) 0.125(8) 0.5000 Uiso D . . . . . C44 C 0.8275(11) 0.4495(6) 0.682(2) 0.110(8) 0.5000 Uiso D . . . . . C45 C 0.7257(14) 0.518242(10) 0.725(3) 0.182(14) 0.5000 Uiso D . . . . . C46 C 0.7063(18) 0.5458(10) 0.809(3) 0.188(16) 0.5000 Uiso D . . . . . C47 C 0.7746(12) 0.484614(10) 0.890(2) 0.155(11) 0.5000 Uiso D . . . . . C48 C 0.7305(9) 0.4562(6) 0.871(2) 0.089(6) 0.5000 Uiso D . . . . . N10 N 0.7827(4) 0.5000 0.7832(8) 0.069(2) 1.0000 Uiso DS . . . . . O7 O 0.5000 0.6235(3) 0.0000 0.108(3) 1.0000 Uiso S . . . . . O8 O 1.0590(13) 0.5000 0.813(2) 0.162(10) 0.5000 Uiso S . . . . . O9 O 0.4317(15) 0.5000 0.667(3) 0.182(12) 0.5000 Uiso S . . . . . H51 H 0.6448 0.5947 0.0026 0.0988 1.0000 Uiso R . . . . . H53 H 0.7078 0.5915 0.0910 0.0989 1.0000 Uiso R . . . . . H52 H 0.6505 0.5915 0.1347 0.0991 1.0000 Uiso R . . . . . H71 H 0.7360 0.6076 0.2716 0.0601 1.0000 Uiso R . . . . . H81 H 0.7885 0.6346 0.4402 0.0651 1.0000 Uiso R . . . . . H91 H 0.7885 0.6956 0.4546 0.0581 1.0000 Uiso R . . . . . H121 H 0.7477 0.7519 0.3818 0.0402 1.0000 Uiso R . . . . . H131 H 0.7114 0.8035 0.3409 0.0469 1.0000 Uiso R . . . . . H132 H 0.6660 0.8088 0.2183 0.0470 1.0000 Uiso R . . . . . H151 H 0.7722 0.8360 0.0768 0.0450 1.0000 Uiso R . . . . . H152 H 0.7922 0.7981 0.1304 0.0451 1.0000 Uiso R . . . . . H161 H 0.7007 0.8371 -0.0714 0.0413 1.0000 Uiso R . . . . . H181 H 0.6329 0.8450 -0.2492 0.0542 1.0000 Uiso R . . . . . H191 H 0.5659 0.8226 -0.4091 0.0591 1.0000 Uiso R . . . . . H201 H 0.5392 0.7631 -0.4142 0.0561 1.0000 Uiso R . . . . . H231 H 0.5366 0.6748 -0.3422 0.0721 1.0000 Uiso R . . . . . H232 H 0.5649 0.7022 -0.4122 0.0719 1.0000 Uiso R . . . . . H233 H 0.5045 0.7114 -0.3845 0.0719 1.0000 Uiso R . . . . . H242 H 0.8357 0.8416 0.2891 0.0760 1.0000 Uiso R . . . . . H243 H 0.8021 0.8370 0.3847 0.0760 1.0000 Uiso R . . . . . H241 H 0.8217 0.8033 0.3275 0.0760 1.0000 Uiso R . . . . . H251 H 0.7506 0.8818 0.2039 0.0821 1.0000 Uiso R . . . . . H252 H 0.7088 0.8699 0.2801 0.0820 1.0000 Uiso R . . . . . H253 H 0.6878 0.8649 0.1458 0.0821 1.0000 Uiso R . . . . . H262 H 0.4358 0.6247 -0.2235 0.0959 1.0000 Uiso R . . . . . H263 H 0.3765 0.6424 -0.2963 0.0960 1.0000 Uiso R . . . . . H261 H 0.4351 0.6451 -0.3368 0.0960 1.0000 Uiso R . . . . . H281 H 0.3686 0.6891 -0.4155 0.0571 1.0000 Uiso R . . . . . H291 H 0.3544 0.7440 -0.5090 0.0610 1.0000 Uiso R . . . . . H301 H 0.3969 0.7941 -0.4183 0.0553 1.0000 Uiso R . . . . . H331 H 0.4656 0.8210 -0.2639 0.0483 1.0000 Uiso R . . . . . H341 H 0.5285 0.8518 -0.1416 0.0501 1.0000 Uiso R . . . . . H342 H 0.5670 0.8317 -0.0305 0.0500 1.0000 Uiso R . . . . . H361 H 0.5718 0.8950 0.0297 0.0969 1.0000 Uiso R . . . . . H363 H 0.5308 0.9022 0.1114 0.0969 1.0000 Uiso R . . . . . H362 H 0.5736 0.8690 0.1311 0.0971 1.0000 Uiso R . . . . . H372 H 0.9319 0.5984 0.3784 0.2171 1.0000 Uiso R . . . . . H371 H 0.9256 0.5647 0.4487 0.2170 1.0000 Uiso R . . . . . H373 H 0.8695 0.5863 0.3863 0.2170 1.0000 Uiso R . . . . . H411 H 0.8376 0.5314 0.8948 0.1733 0.5000 Uiso R . . . . . H412 H 0.8704 0.5000 0.8423 0.1733 1.0000 Uiso RS . . . . . H421 H 0.8827 0.5578 0.7825 0.1920 0.5000 Uiso R . . . . . H422 H 0.8158 0.5620 0.7366 0.1920 0.5000 Uiso R . . . . . H423 H 0.8486 0.5346 0.6841 0.1920 0.5000 Uiso R . . . . . H451 H 0.6950 0.5000 0.7019 0.2274 1.0000 Uiso RS . . . . . H452 H 0.7300 0.5317 0.6661 0.2274 0.5000 Uiso R . . . . . H461 H 0.6692 0.5578 0.7799 0.2310 0.5000 Uiso R . . . . . H462 H 0.6999 0.5324 0.8748 0.2310 0.5000 Uiso R . . . . . H463 H 0.7348 0.5623 0.8390 0.2310 0.5000 Uiso R . . . . . H471 H 0.7583 0.5000 0.9231 0.1918 1.0000 Uiso RS . . . . . H472 H 0.8108 0.4773 0.9399 0.1918 0.5000 Uiso R . . . . . H481 H 0.7254 0.4488 0.9401 0.1066 0.5000 Uiso R . . . . . H482 H 0.6951 0.4631 0.8219 0.1066 0.5000 Uiso R . . . . . H483 H 0.7476 0.4379 0.8386 0.1066 0.5000 Uiso R . . . . . H432 H 0.7870 0.5000 0.6270 0.1517 1.0000 Uiso RS . . . . . H441 H 0.8209 0.4391 0.6108 0.1355 0.5000 Uiso R . . . . . H442 H 0.8226 0.4329 0.7351 0.1355 0.5000 Uiso R . . . . . H443 H 0.8646 0.4596 0.7044 0.1355 0.5000 Uiso R . . . . . H391 H 0.5862 0.5663 -0.3587 0.2066 1.0000 Uiso R . . . . . H392 H 0.5206 0.5744 -0.3772 0.2066 1.0000 Uiso R . . . . . H393 H 0.5526 0.5503 -0.2795 0.2066 1.0000 Uiso R . . . . . H431 H 0.7468 0.4704 0.6560 0.1496 0.5000 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 Mo1 0.0807(7) 0.0345(5) 0.0933(7) 0.0000 0.0586(6) 0.0000 Ni1 0.0289(3) 0.0373(4) 0.0234(3) 0.0008(3) 0.0084(3) -0.0034(3) Ni2 0.0325(5) 0.0362(6) 0.0224(5) 0.0000 0.0085(4) 0.0000 K1 0.0323(7) 0.0423(7) 0.0359(6) -0.0004(6) 0.0092(5) -0.0023(5) C1 0.064(5) 0.038(4) 0.076(5) -0.008(3) 0.040(4) 0.000(3) C2 0.121(15) 0.083(11) 0.138(16) 0.0000 0.077(13) 0.0000 C3 0.098(6) 0.037(4) 0.083(6) 0.012(4) 0.053(5) 0.006(4) C4 0.067(8) 0.052(7) 0.113(11) 0.0000 0.048(8) 0.0000 C5 0.076(5) 0.037(4) 0.078(5) -0.006(4) 0.017(4) 0.003(4) C6 0.037(3) 0.046(4) 0.036(3) 0.007(3) 0.017(3) -0.002(3) C7 0.049(4) 0.048(4) 0.053(4) 0.013(3) 0.021(3) 0.007(3) C8 0.041(4) 0.076(5) 0.045(4) 0.027(4) 0.012(3) 0.016(3) C9 0.034(3) 0.069(5) 0.036(3) 0.004(3) 0.010(3) 0.003(3) C10 0.025(3) 0.055(4) 0.026(3) 0.008(3) 0.008(2) 0.002(3) C11 0.023(3) 0.047(3) 0.030(3) 0.006(3) 0.011(2) -0.003(2) C12 0.023(3) 0.056(4) 0.026(3) -0.004(3) 0.007(2) -0.006(3) C13 0.035(3) 0.049(4) 0.034(3) -0.010(3) 0.015(2) -0.007(3) C14 0.031(3) 0.041(3) 0.043(3) -0.004(3) 0.014(2) -0.005(3) C15 0.030(3) 0.038(3) 0.045(3) 0.004(3) 0.015(2) -0.003(2) C16 0.038(3) 0.034(3) 0.041(3) 0.005(3) 0.023(3) 0.005(3) C17 0.033(3) 0.043(3) 0.026(3) 0.003(3) 0.015(2) 0.004(3) C18 0.047(4) 0.047(4) 0.040(3) 0.011(3) 0.022(3) 0.013(3) C19 0.054(4) 0.060(5) 0.038(4) 0.017(3) 0.018(3) 0.019(3) C20 0.038(3) 0.074(5) 0.025(3) 0.004(3) 0.009(3) 0.013(3) C21 0.024(3) 0.054(4) 0.025(3) 0.002(3) 0.010(2) 0.003(3) C22 0.019(2) 0.043(3) 0.023(3) -0.002(2) 0.008(2) 0.004(2) C23 0.039(3) 0.079(5) 0.028(3) -0.008(3) 0.008(3) -0.012(3) C24 0.041(4) 0.061(4) 0.049(4) -0.008(3) 0.010(3) -0.012(3) C25 0.064(4) 0.044(4) 0.054(4) -0.006(3) 0.022(3) -0.001(3) C26 0.070(5) 0.067(5) 0.060(5) -0.025(4) 0.026(4) -0.019(4) C27 0.026(3) 0.065(4) 0.030(3) -0.006(3) 0.008(2) 0.003(3) C28 0.028(3) 0.081(5) 0.033(3) -0.021(3) 0.013(3) -0.010(3) C29 0.026(3) 0.101(6) 0.027(3) 0.000(4) 0.006(2) 0.010(4) C30 0.030(3) 0.077(5) 0.029(3) 0.009(3) 0.007(2) 0.011(3) C31 0.024(3) 0.057(4) 0.027(3) 0.003(3) 0.010(2) 0.007(3) C32 0.021(3) 0.051(4) 0.027(3) -0.002(3) 0.010(2) 0.003(2) C33 0.032(3) 0.058(4) 0.037(3) 0.016(3) 0.019(3) 0.013(3) C34 0.040(3) 0.043(3) 0.043(3) 0.004(3) 0.023(3) 0.002(3) C35 0.047(5) 0.041(5) 0.043(5) 0.0000 0.028(4) 0.0000 C36 0.074(5) 0.055(4) 0.084(6) -0.020(4) 0.050(4) -0.022(4) C37 0.204(16) 0.105(10) 0.116(10) -0.022(8) -0.012(10) -0.016(10) C38 0.154(10) 0.057(6) 0.082(7) -0.001(5) -0.015(7) -0.022(6) C39 0.229(19) 0.170(15) 0.153(13) -0.052(12) 0.094(13) -0.048(13) C40 0.111(8) 0.084(7) 0.079(7) -0.013(6) 0.052(6) -0.010(6) N1 0.070(4) 0.033(3) 0.083(4) -0.001(3) 0.038(3) 0.000(3) N2 0.094(9) 0.060(6) 0.118(10) 0.0000 0.071(8) 0.0000 N3 0.099(5) 0.040(3) 0.107(6) 0.001(3) 0.071(5) 0.001(3) N4 0.087(8) 0.037(5) 0.113(9) 0.0000 0.064(7) 0.0000 N5 0.029(2) 0.040(3) 0.028(2) -0.003(2) 0.0130(19) -0.010(2) N6 0.031(2) 0.039(3) 0.031(2) -0.002(2) 0.013(2) -0.005(2) N7 0.034(3) 0.040(3) 0.029(2) 0.006(2) 0.013(2) 0.005(2) N8 0.283(16) 0.078(7) 0.083(7) -0.016(5) -0.007(8) -0.047(8) N9 0.097(6) 0.092(6) 0.085(6) -0.003(5) 0.033(5) 0.002(5) O1 0.048(2) 0.036(2) 0.042(2) 0.0004(19) 0.0116(19) 0.0004(19) O2 0.038(2) 0.036(2) 0.0250(19) 0.0047(17) 0.0055(16) -0.0050(17) O3 0.035(2) 0.039(2) 0.0212(18) 0.0003(17) 0.0023(15) -0.0024(17) O4 0.037(2) 0.050(3) 0.029(2) -0.0057(18) 0.0067(17) -0.0066(18) O5 0.048(3) 0.051(3) 0.039(2) -0.015(2) 0.0110(19) -0.007(2) O6 0.035(2) 0.043(2) 0.0196(18) -0.0022(16) 0.0006(15) 0.0028(17) S1 0.128(2) 0.0556(12) 0.1056(18) 0.0030(12) 0.0792(17) -0.0166(13) S2 0.149(5) 0.210(7) 0.166(6) 0.0000 0.013(5) 0.0000 S3 0.177(3) 0.0580(13) 0.112(2) 0.0137(14) 0.098(2) 0.0389(16) S4 0.096(3) 0.122(4) 0.149(4) 0.0000 0.035(3) 0.0000 _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 Mo1 . N3 6_565 2.074(6) yes Mo1 . N1 6_565 2.071(6) yes Mo1 . N1 . 2.071(6) yes Mo1 . N2 . 2.012(15) yes Mo1 . N3 . 2.074(6) yes Mo1 . N4 . 2.099(14) yes Ni1 . N5 . 1.848(4) yes Ni1 . N6 . 1.851(5) yes Ni1 . O2 . 1.833(4) yes Ni1 . O3 . 1.824(3) yes Ni2 . N7 5_655 1.848(4) yes Ni2 . O6 5_655 1.835(4) yes Ni2 . N7 . 1.848(4) yes Ni2 . O6 . 1.835(4) yes C1 . N1 . 1.151(8) yes C1 . S1 . 1.598(7) yes C2 . N2 . 1.13(2) yes C2 . S2 . 1.64(2) yes C3 . N3 . 1.143(9) yes C3 . S3 . 1.610(8) yes C4 . N4 . 1.132(16) yes C4 . S4 . 1.621(17) yes C5 . O1 . 1.416(8) yes C5 . H51 . 0.963 no C5 . H53 . 0.961 no C5 . H52 . 0.959 no C6 . C7 . 1.353(8) yes C6 . C11 . 1.413(8) yes C6 . O1 . 1.354(7) yes C7 . C8 . 1.394(10) yes C7 . H71 . 0.930 no C8 . C9 . 1.348(10) yes C8 . H81 . 0.929 no C9 . C10 . 1.391(8) yes C9 . H91 . 0.937 no C10 . C11 . 1.400(8) yes C10 . C12 . 1.418(9) yes C11 . O2 . 1.293(6) yes C12 . N5 . 1.264(7) yes C12 . H121 . 0.936 no C13 . C14 . 1.519(8) yes C13 . N5 . 1.452(7) yes C13 . H131 . 0.977 no C13 . H132 . 0.972 no C14 . C15 . 1.508(8) yes C14 . C24 . 1.516(8) yes C14 . C25 . 1.510(9) yes C15 . N6 . 1.466(7) yes C15 . H151 . 0.967 no C15 . H152 . 0.973 no C16 . C17 . 1.418(8) yes C16 . N6 . 1.272(7) yes C16 . H161 . 0.940 no C17 . C18 . 1.383(8) yes C17 . C22 . 1.403(8) yes C18 . C19 . 1.356(9) yes C18 . H181 . 0.936 no C19 . C20 . 1.370(10) yes C19 . H191 . 0.934 no C20 . C21 . 1.365(8) yes C20 . H201 . 0.935 no C21 . C22 . 1.408(7) yes C21 . O4 . 1.361(7) yes C22 . O3 . 1.294(6) yes C23 . O4 . 1.413(7) yes C23 . H231 . 0.965 no C23 . H232 . 0.967 no C23 . H233 . 0.968 no C24 . H242 . 0.963 no C24 . H243 . 0.961 no C24 . H241 . 0.960 no C25 . H251 . 0.965 no C25 . H252 . 0.972 no C25 . H253 . 0.964 no C26 . O5 . 1.418(8) yes C26 . H262 . 0.954 no C26 . H263 . 0.969 no C26 . H261 . 0.965 no C27 . C28 . 1.367(8) yes C27 . C32 . 1.408(8) yes C27 . O5 . 1.362(8) yes C28 . C29 . 1.393(10) yes C28 . H281 . 0.936 no C29 . C30 . 1.338(10) yes C29 . H291 . 0.928 no C30 . C31 . 1.395(8) yes C30 . H301 . 0.941 no C31 . C32 . 1.377(8) yes C31 . C33 . 1.418(9) yes C32 . O6 . 1.302(6) yes C33 . N7 . 1.278(7) yes C33 . H331 . 0.928 no C34 . C35 . 1.513(7) yes C34 . N7 . 1.453(7) yes C34 . H341 . 0.975 no C34 . H342 . 0.978 no C35 . C36 5_655 1.509(9) yes C35 . C36 . 1.509(9) yes C36 . H361 . 0.959 no C36 . H363 . 0.955 no C36 . H362 . 0.958 no C37 . C38 . 1.411(16) yes C37 . H372 . 0.962 no C37 . H371 . 0.959 no C37 . H373 . 0.957 no C38 . N8 . 1.075(13) yes C39 . C40 . 1.422(17) yes C39 . H391 . 0.930 no C39 . H392 . 0.930 no C39 . H393 . 0.930 no C40 . N9 . 1.076(11) yes C41 . C42 . 1.40(3) yes C41 . N10 . 1.47(2) yes C41 . H411 . 0.921 no C41 . H412 . 1.065 no C42 . H421 . 0.889 no C42 . H422 . 0.943 no C42 . H423 . 0.931 no C43 . C43 6_565 1.5186(8) yes C43 . C45 6_565 1.57(4) yes C43 . H452 6_565 1.282 no C43 . C44 . 1.53(2) yes C43 . N10 . 1.44(2) yes C43 . H432 . 1.037 no C43 . H431 . 0.900 no C44 . H441 . 0.929 no C44 . H442 . 0.925 no C44 . H443 . 0.918 no C45 . H431 6_565 1.164 no C45 . C45 6_565 1.3664(8) yes C45 . C46 . 1.60(3) yes C45 . N10 . 1.49(3) yes C45 . H451 . 0.975 no C45 . H452 . 0.905 no C46 . H483 6_565 1.117 no C46 . C48 6_565 0.81(4) yes C46 . H461 . 0.957 no C46 . H462 . 0.993 no C46 . H463 . 0.911 no C47 . C47 6_565 1.1525(8) yes C47 . C48 . 1.45(2) yes C47 . N10 . 1.48(2) yes C47 . H471 . 0.850 no C47 . H472 . 0.939 no C48 . H481 . 0.927 no C48 . H482 . 0.915 no C48 . H483 . 0.932 no H452 . H431 6_565 0.448 no H462 . H482 6_565 0.645 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 N3 6_565 Mo1 . N1 6_565 91.3(2) yes N3 6_565 Mo1 . N1 . 179.2(3) yes N1 6_565 Mo1 . N1 . 89.2(3) yes N3 6_565 Mo1 . N2 . 90.2(3) yes N1 6_565 Mo1 . N2 . 89.2(3) yes N1 . Mo1 . N2 . 89.2(3) yes N3 6_565 Mo1 . N3 . 88.2(3) yes N1 6_565 Mo1 . N3 . 179.2(3) yes N1 . Mo1 . N3 . 91.3(2) yes N2 . Mo1 . N3 . 90.2(3) yes N3 6_565 Mo1 . N4 . 92.1(3) yes N1 6_565 Mo1 . N4 . 88.5(3) yes N1 . Mo1 . N4 . 88.5(3) yes N2 . Mo1 . N4 . 176.8(4) yes N3 . Mo1 . N4 . 92.1(3) yes N5 . Ni1 . N6 . 91.31(19) yes N5 . Ni1 . O2 . 92.75(18) yes N6 . Ni1 . O2 . 169.24(18) yes N5 . Ni1 . O3 . 168.09(17) yes N6 . Ni1 . O3 . 94.44(18) yes O2 . Ni1 . O3 . 83.46(16) yes N7 5_655 Ni2 . O6 5_655 94.68(18) yes N7 5_655 Ni2 . N7 . 90.1(3) yes O6 5_655 Ni2 . N7 . 167.21(18) yes N7 5_655 Ni2 . O6 . 167.21(18) yes O6 5_655 Ni2 . O6 . 83.1(2) yes N7 . Ni2 . O6 . 94.68(18) yes N1 . C1 . S1 . 179.5(6) yes N2 . C2 . S2 . 179.5(17) yes N3 . C3 . S3 . 178.0(9) yes N4 . C4 . S4 . 178.5(12) yes O1 . C5 . H51 . 108.9 no O1 . C5 . H53 . 108.9 no H51 . C5 . H53 . 109.9 no O1 . C5 . H52 . 109.2 no H51 . C5 . H52 . 110.5 no H53 . C5 . H52 . 109.4 no C7 . C6 . C11 . 120.9(6) yes C7 . C6 . O1 . 125.4(6) yes C11 . C6 . O1 . 113.7(5) yes C6 . C7 . C8 . 121.3(7) yes C6 . C7 . H71 . 119.1 no C8 . C7 . H71 . 119.6 no C7 . C8 . C9 . 118.9(6) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 121.1 no C8 . C9 . C10 . 121.3(6) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 119.0 no C9 . C10 . C11 . 120.6(6) yes C9 . C10 . C12 . 120.2(5) yes C11 . C10 . C12 . 119.0(5) yes C6 . C11 . C10 . 116.9(5) yes C6 . C11 . O2 . 118.5(5) yes C10 . C11 . O2 . 124.5(5) yes C10 . C12 . N5 . 126.1(5) yes C10 . C12 . H121 . 116.7 no N5 . C12 . H121 . 117.3 no C14 . C13 . N5 . 112.5(4) yes C14 . C13 . H131 . 109.8 no N5 . C13 . H131 . 109.4 no C14 . C13 . H132 . 107.8 no N5 . C13 . H132 . 107.7 no H131 . C13 . H132 . 109.5 no C13 . C14 . C15 . 110.1(5) yes C13 . C14 . C24 . 108.9(5) yes C15 . C14 . C24 . 107.9(5) yes C13 . C14 . C25 . 108.4(5) yes C15 . C14 . C25 . 111.3(5) yes C24 . C14 . C25 . 110.3(5) yes C14 . C15 . N6 . 113.3(4) yes C14 . C15 . H151 . 108.1 no N6 . C15 . H151 . 108.9 no C14 . C15 . H152 . 108.8 no N6 . C15 . H152 . 108.5 no H151 . C15 . H152 . 109.1 no C17 . C16 . N6 . 126.7(5) yes C17 . C16 . H161 . 116.5 no N6 . C16 . H161 . 116.7 no C16 . C17 . C18 . 119.2(6) yes C16 . C17 . C22 . 119.9(5) yes C18 . C17 . C22 . 120.7(5) yes C17 . C18 . C19 . 120.9(6) yes C17 . C18 . H181 . 118.7 no C19 . C18 . H181 . 120.4 no C18 . C19 . C20 . 119.5(6) yes C18 . C19 . H191 . 120.3 no C20 . C19 . H191 . 120.2 no C19 . C20 . C21 . 121.2(6) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 118.5 no C20 . C21 . C22 . 120.8(6) yes C20 . C21 . O4 . 125.5(5) yes C22 . C21 . O4 . 113.7(5) yes C21 . C22 . C17 . 116.8(5) yes C21 . C22 . O3 . 118.8(5) yes C17 . C22 . O3 . 124.3(5) yes O4 . C23 . H231 . 108.3 no O4 . C23 . H232 . 110.3 no H231 . C23 . H232 . 110.3 no O4 . C23 . H233 . 109.1 no H231 . C23 . H233 . 109.6 no H232 . C23 . H233 . 109.1 no C14 . C24 . H242 . 109.0 no C14 . C24 . H243 . 109.6 no H242 . C24 . H243 . 110.2 no C14 . C24 . H241 . 109.0 no H242 . C24 . H241 . 109.6 no H243 . C24 . H241 . 109.4 no C14 . C25 . H251 . 109.7 no C14 . C25 . H252 . 109.3 no H251 . C25 . H252 . 109.3 no C14 . C25 . H253 . 108.9 no H251 . C25 . H253 . 109.8 no H252 . C25 . H253 . 109.8 no O5 . C26 . H262 . 108.9 no O5 . C26 . H263 . 109.7 no H262 . C26 . H263 . 110.1 no O5 . C26 . H261 . 108.7 no H262 . C26 . H261 . 110.0 no H263 . C26 . H261 . 109.3 no C28 . C27 . C32 . 120.6(6) yes C28 . C27 . O5 . 125.0(6) yes C32 . C27 . O5 . 114.4(5) yes C27 . C28 . C29 . 120.3(6) yes C27 . C28 . H281 . 119.5 no C29 . C28 . H281 . 120.2 no C28 . C29 . C30 . 120.1(6) yes C28 . C29 . H291 . 120.1 no C30 . C29 . H291 . 119.8 no C29 . C30 . C31 . 120.1(6) yes C29 . C30 . H301 . 119.8 no C31 . C30 . H301 . 120.1 no C30 . C31 . C32 . 121.5(6) yes C30 . C31 . C33 . 117.8(6) yes C32 . C31 . C33 . 120.4(5) yes C27 . C32 . C31 . 117.3(5) yes C27 . C32 . O6 . 117.3(5) yes C31 . C32 . O6 . 125.4(5) yes C31 . C33 . N7 . 125.9(5) yes C31 . C33 . H331 . 117.0 no N7 . C33 . H331 . 117.1 no C35 . C34 . N7 . 113.1(4) yes C35 . C34 . H341 . 108.4 no N7 . C34 . H341 . 108.8 no C35 . C34 . H342 . 108.3 no N7 . C34 . H342 . 108.5 no H341 . C34 . H342 . 109.7 no C34 . C35 . C34 5_655 108.5(7) yes C34 . C35 . C36 5_655 109.3(4) yes C34 5_655 C35 . C36 5_655 108.8(4) yes C34 . C35 . C36 . 108.8(4) yes C34 5_655 C35 . C36 . 109.3(4) yes C36 5_655 C35 . C36 . 112.1(9) yes C35 . C36 . H361 . 109.5 no C35 . C36 . H363 . 108.6 no H361 . C36 . H363 . 111.1 no C35 . C36 . H362 . 108.0 no H361 . C36 . H362 . 109.1 no H363 . C36 . H362 . 110.5 no C38 . C37 . H372 . 109.3 no C38 . C37 . H371 . 111.2 no H372 . C37 . H371 . 107.9 no C38 . C37 . H373 . 111.9 no H372 . C37 . H373 . 108.1 no H371 . C37 . H373 . 108.2 no C37 . C38 . N8 . 174.7(15) yes C40 . C39 . H391 . 109.7 no C40 . C39 . H392 . 109.1 no H391 . C39 . H392 . 109.5 no C40 . C39 . H393 . 109.5 no H391 . C39 . H393 . 109.5 no H392 . C39 . H393 . 109.5 no C39 . C40 . N9 . 177.1(12) yes Mo1 . N1 . C1 . 176.1(5) yes Mo1 . N2 . C2 . 168.6(13) yes Mo1 . N3 . C3 . 174.7(6) yes Mo1 . N4 . C4 . 170.7(10) yes C13 . N5 . C12 . 118.4(5) yes C13 . N5 . Ni1 . 115.4(4) yes C12 . N5 . Ni1 . 125.8(4) yes C15 . N6 . C16 . 118.2(5) yes C15 . N6 . Ni1 . 116.0(4) yes C16 . N6 . Ni1 . 125.1(4) yes C34 . N7 . C33 . 119.1(5) yes C34 . N7 . Ni2 . 115.9(4) yes C33 . N7 . Ni2 . 124.6(4) yes C5 . O1 . C6 . 116.7(5) yes C11 . O2 . Ni1 . 125.3(4) yes C22 . O3 . Ni1 . 127.1(3) yes C23 . O4 . C21 . 115.9(5) yes C26 . O5 . C27 . 116.1(5) yes C32 . O6 . Ni2 . 124.2(4) yes C42 . C41 . N10 . 115(2) yes C42 . C41 . H411 . 109.1 no N10 . C41 . H411 . 110.0 no C42 . C41 . H412 . 111.5 no N10 . C41 . H412 . 101.5 no H411 . C41 . H412 . 109.6 no C41 . C42 . H421 . 110.7 no C41 . C42 . H422 . 105.5 no H421 . C42 . H422 . 111.9 no C41 . C42 . H423 . 106.8 no H421 . C42 . H423 . 113.1 no H422 . C42 . H423 . 108.3 no C43 6_565 C43 . C45 6_565 87.22(7) yes C43 6_565 C43 . H452 6_565 109.5 no C43 6_565 C43 . C44 . 137.6(12) yes C45 6_565 C43 . C44 . 132.5(13) yes H452 6_565 C43 . C44 . 112.4 no C43 6_565 C43 . N10 . 58.2(5) yes C45 6_565 C43 . N10 . 59.4(12) yes H452 6_565 C43 . N10 . 94.5 no C44 . C43 . N10 . 123.6(19) yes C45 6_565 C43 . H432 . 114.2 no H452 6_565 C43 . H432 . 112.9 no C44 . C43 . H432 . 111.3 no N10 . C43 . H432 . 100.9 no C43 6_565 C43 . H431 . 112.9 no C44 . C43 . H431 . 106.6 no N10 . C43 . H431 . 106.6 no H432 . C43 . H431 . 106.7 no C43 . C44 . H441 . 111.9 no C43 . C44 . H442 . 106.7 no H441 . C44 . H442 . 110.1 no C43 . C44 . H443 . 106.3 no H441 . C44 . H443 . 110.7 no H442 . C44 . H443 . 111.1 no C43 6_565 C45 . C45 6_565 92.78(7) yes H431 6_565 C45 . C45 6_565 111.5 no C43 6_565 C45 . C46 . 126(2) yes H431 6_565 C45 . C46 . 118.0 no C45 6_565 C45 . C46 . 130.3(16) yes C43 6_565 C45 . N10 . 56.0(13) yes H431 6_565 C45 . N10 . 90.6 no C45 6_565 C45 . N10 . 62.8(5) yes C46 . C45 . N10 . 111(2) yes C43 6_565 C45 . H451 . 124.6 no H431 6_565 C45 . H451 . 117.9 no C46 . C45 . H451 . 109.0 no N10 . C45 . H451 . 108.0 no C43 6_565 C45 . H452 . 54.8 no C45 6_565 C45 . H452 . 123.9 no C46 . C45 . H452 . 104.8 no N10 . C45 . H452 . 110.7 no H451 . C45 . H452 . 113.0 no H483 6_565 C46 . C45 . 101.1 no H483 6_565 C46 . C48 6_565 55.0 no C45 . C46 . C48 6_565 106(4) yes H483 6_565 C46 . H461 . 118.8 no C45 . C46 . H461 . 117.1 no C48 6_565 C46 . H461 . 135.9 no H483 6_565 C46 . H462 . 108.7 no C45 . C46 . H462 . 108.5 no C48 6_565 C46 . H462 . 54.8 no H461 . C46 . H462 . 102.3 no C45 . C46 . H463 . 113.3 no C48 6_565 C46 . H463 . 56.0 no H461 . C46 . H463 . 108.8 no H462 . C46 . H463 . 105.8 no C47 6_565 C47 . C48 . 137.0(12) yes C47 6_565 C47 . N10 . 67.1(4) yes C48 . C47 . N10 . 113.3(19) yes C47 6_565 C47 . H471 . 47.3 no C48 . C47 . H471 . 100.6 no N10 . C47 . H471 . 109.4 no C47 6_565 C47 . H472 . 106.9 no C48 . C47 . H472 . 111.5 no N10 . C47 . H472 . 111.9 no H471 . C47 . H472 . 109.4 no C47 . C48 . C46 6_565 120(4) yes C47 . C48 . H481 . 109.4 no C46 6_565 C48 . H481 . 125.9 no C47 . C48 . H482 . 112.0 no H481 . C48 . H482 . 111.0 no C47 . C48 . H483 . 103.9 no C46 6_565 C48 . H483 . 79.3 no H481 . C48 . H483 . 109.6 no H482 . C48 . H483 . 110.7 no C45 . N10 . C45 6_565 54.4(10) yes C45 . N10 . C47 . 106.4(17) yes C45 6_565 N10 . C47 . 85.8(16) yes C45 . N10 . C47 6_565 85.8(16) yes C45 6_565 N10 . C47 6_565 106.4(17) yes C45 . N10 . C41 6_565 172.8(16) yes C45 6_565 N10 . C41 6_565 120.8(8) yes C47 . N10 . C41 6_565 77.6(15) yes C47 6_565 N10 . C41 6_565 101.2(16) yes C45 . N10 . C41 . 120.8(8) yes C45 6_565 N10 . C41 . 172.8(16) yes C47 . N10 . C41 . 101.2(16) yes C47 6_565 N10 . C41 . 77.6(15) yes C41 6_565 N10 . C41 . 63.2(11) yes C45 . N10 . C43 . 93.0(14) yes C45 6_565 N10 . C43 . 64.6(14) yes C47 . N10 . C43 . 124.8(6) yes C47 6_565 N10 . C43 . 169.1(11) yes C41 6_565 N10 . C43 . 79.8(14) yes C45 . N10 . C43 6_565 64.6(14) yes C45 6_565 N10 . C43 6_565 93.0(14) yes C47 . N10 . C43 6_565 169.1(11) yes C47 6_565 N10 . C43 6_565 124.8(6) yes C41 6_565 N10 . C43 6_565 112.0(16) yes C41 . N10 . C43 . 112.0(16) yes C41 . N10 . C43 6_565 79.8(14) yes C43 . N10 . C43 6_565 63.6(10) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C15 . H152 . O3 4_665 151 0.97 2.39 3.270(7) yes C33 . H331 . N8 8_464 160 0.93 2.55 3.434(15) yes C47 6_565 H471 . C48 . 128 0.85 1.81 2.428(15) yes C47 . H471 . C48 6_565 128 0.85 1.81 2.428(15) yes C43 . H432 . C44 6_565 123 1.04 2.14 2.843(15) yes C43 6_565 H432 . C44 . 123 1.04 2.14 2.843(15) yes C45 6_565 H431 . C44 . 127 1.16 1.99 2.838(15) yes # Attachment '3908_web_deposit_cif_file_2_Jean-PascalSutter_1295611074.cif' data_cpd3 _database_code_depnum_ccdc_archive 'CCDC 809269' #TrackingRef '3908_web_deposit_cif_file_2_Jean-PascalSutter_1295611074.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 ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 23.4893(11) _cell_length_b 33.2913(15) _cell_length_c 15.1039(6) _cell_angle_alpha 90 _cell_angle_beta 116.265(2) _cell_angle_gamma 90 _cell_volume 10591.7(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 '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' 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' 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' 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' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 '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 4 # Given Formula = C98 H116 Mo1 N15 Na2 Ni4 O16 S6 # Dc = 1.46 Fooo = 4836.00 Mu = 10.09 M = 1164.62 # Found Formula = C98 H116 Mo1 N15 Na2 Ni4 O16 S6 # Dc = 1.46 FOOO = 4836.00 Mu = 10.09 M = 1164.62 _chemical_formula_sum 'C98 H116 Mo1 N15 Na2 Ni4 O16 S6' _chemical_formula_moiety '2(C42 H48 N4 Na Ni2 O8),C8 H20 N,C6 Mo N6 S6 ' _chemical_compound_source ? _chemical_formula_weight 2329.25 _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2 _cell_measurement_theta_max 32 _cell_measurement_temperature 180 _exptl_crystal_description planar _exptl_crystal_colour orange _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4836 _exptl_absorpt_coefficient_mu 1.009 # Sheldrick geometric approximatio 0.74 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _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 '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 142585 _reflns_number_total 18759 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections without Friedels Law is 18759 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 18817 _diffrn_reflns_theta_min 1.144 _diffrn_reflns_theta_max 32.285 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 32.285 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -35 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 50 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.62 _refine_diff_density_max 1.04 # 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>3.0\s(I) _refine_ls_number_reflns 11492 _refine_ls_number_restraints 4 _refine_ls_number_parameters 635 _oxford_refine_ls_R_factor_ref 0.0364 _refine_ls_wR_factor_ref 0.0392 _refine_ls_goodness_of_fit_ref 1.0906 _refine_ls_shift/su_max 0.0003213 _refine_ls_shift/su_mean 0.0000961 # The values computed from all data _oxford_reflns_number_all 18716 _refine_ls_R_factor_all 0.0766 _refine_ls_wR_factor_all 0.0830 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12525 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_gt 0.0414 # 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: 0.492 0.255 0.221 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mo1 Mo 0.7500 0.7500 0.5000 0.0324 1.0000 Uani S . . . . . . Ni1 Ni 0.683380(12) 0.540286(7) 0.373737(18) 0.0222 1.0000 Uani . . . . . . . Ni2 Ni 0.796094(13) 0.361384(8) 0.58931(2) 0.0274 1.0000 Uani . . . . . . . C1 C 0.81201(11) 0.72400(7) 0.73201(19) 0.0343 1.0000 Uani . . . . . . . C2 C 0.80771(10) 0.66666(7) 0.45752(17) 0.0330 1.0000 Uani . . . . . . . C3 C 0.62631(11) 0.70847(7) 0.50227(17) 0.0323 1.0000 Uani . . . . . . . C4 C 0.70820(16) 0.36772(7) 0.3270(2) 0.0472 1.0000 Uani . . . . . . . C5 C 0.66268(11) 0.42914(6) 0.24703(16) 0.0304 1.0000 Uani . . . . . . . C6 C 0.62417(12) 0.40984(7) 0.15999(18) 0.0379 1.0000 Uani . . . . . . . C7 C 0.58646(12) 0.43196(8) 0.07586(18) 0.0412 1.0000 Uani . . . . . . . C8 C 0.58834(12) 0.47292(8) 0.07820(17) 0.0382 1.0000 Uani . . . . . . . C9 C 0.62611(10) 0.49335(6) 0.16705(15) 0.0293 1.0000 Uani . . . . . . . C10 C 0.66234(10) 0.47176(6) 0.25394(15) 0.0265 1.0000 Uani . . . . . . . C11 C 0.63202(10) 0.53625(7) 0.16687(15) 0.0297 1.0000 Uani . . . . . . . C12 C 0.66402(10) 0.60167(6) 0.23284(15) 0.0278 1.0000 Uani . . . . . . . C13 C 0.61586(10) 0.62698(6) 0.25106(15) 0.0266 1.0000 Uani . . . . . . . C14 C 0.61129(10) 0.61215(6) 0.34394(16) 0.0298 1.0000 Uani . . . . . . . C15 C 0.69983(10) 0.60533(6) 0.50147(15) 0.0278 1.0000 Uani . . . . . . . C16 C 0.74573(10) 0.58361(6) 0.58416(15) 0.0275 1.0000 Uani . . . . . . . C17 C 0.78301(12) 0.60388(7) 0.67349(17) 0.0359 1.0000 Uani . . . . . . . C18 C 0.81814(13) 0.58270(8) 0.75781(18) 0.0435 1.0000 Uani . . . . . . . C19 C 0.81592(12) 0.54059(8) 0.75698(16) 0.0379 1.0000 Uani . . . . . . . C20 C 0.78000(10) 0.52017(6) 0.67096(15) 0.0294 1.0000 Uani . . . . . . . C21 C 0.74549(9) 0.54146(6) 0.58111(14) 0.0255 1.0000 Uani . . . . . . . C22 C 0.80499(14) 0.45577(8) 0.74726(18) 0.0450 1.0000 Uani . . . . . . . C23 C 0.63759(13) 0.67069(7) 0.2642(2) 0.0405 1.0000 Uani . . . . . . . C24 C 0.55036(12) 0.62350(9) 0.16313(18) 0.0426 1.0000 Uani . . . . . . . C25 C 0.86582(14) 0.52295(7) 0.5235(2) 0.0449 1.0000 Uani . . . . . . . C26 C 0.89998(11) 0.45501(8) 0.5561(2) 0.0424 1.0000 Uani . . . . . . . C27 C 0.95973(14) 0.46372(10) 0.5662(3) 0.0689 1.0000 Uani . . . . . . . C28 C 1.00603(16) 0.43337(13) 0.5886(4) 0.0988 1.0000 Uani . . . . . . . C29 C 0.99217(16) 0.39497(12) 0.6021(4) 0.0907 1.0000 Uani . . . . . . . C30 C 0.93128(13) 0.38517(9) 0.5941(3) 0.0553 1.0000 Uani . . . . . . . C31 C 0.88426(11) 0.41498(7) 0.57096(19) 0.0373 1.0000 Uani . . . . . . . C32 C 0.91799(13) 0.34429(8) 0.6062(3) 0.0525 1.0000 Uani . . . . . . . C33 C 0.86185(13) 0.28699(7) 0.61219(19) 0.0387 1.0000 Uani . . . . . . . C34 C 0.85735(12) 0.27278(6) 0.70542(18) 0.0348 1.0000 Uani . . . . . . . C35 C 0.80867(14) 0.29806(7) 0.72290(18) 0.0420 1.0000 Uani . . . . . . . C36 C 0.70440(13) 0.30898(6) 0.59468(19) 0.0375 1.0000 Uani . . . . . . . C37 C 0.65409(12) 0.33155(7) 0.51942(19) 0.0356 1.0000 Uani . . . . . . . C38 C 0.59263(13) 0.31479(8) 0.4695(2) 0.0441 1.0000 Uani . . . . . . . C39 C 0.54346(13) 0.33682(9) 0.4043(2) 0.0465 1.0000 Uani . . . . . . . C40 C 0.55206(11) 0.37764(8) 0.39076(18) 0.0393 1.0000 Uani . . . . . . . C41 C 0.61099(11) 0.39538(7) 0.44182(16) 0.0313 1.0000 Uani . . . . . . . C42 C 0.66462(10) 0.37221(6) 0.50433(16) 0.0290 1.0000 Uani . . . . . . . C43 C 0.57251(11) 0.45972(8) 0.37149(19) 0.0397 1.0000 Uani . . . . . . . C44 C 0.83702(15) 0.22890(7) 0.6899(2) 0.0469 1.0000 Uani . . . . . . . C45 C 0.92182(16) 0.27618(10) 0.7957(2) 0.0584 1.0000 Uani . . . . . . . N1 N 0.79287(10) 0.73562(6) 0.65128(16) 0.0378 1.0000 Uani . . . . . . . N2 N 0.78575(10) 0.69563(6) 0.47314(16) 0.0391 1.0000 Uani . . . . . . . N3 N 0.66805(10) 0.72195(6) 0.49125(16) 0.0393 1.0000 Uani . . . . . . . N4 N 0.65574(8) 0.55851(5) 0.24477(12) 0.0260 1.0000 Uani . . . . . . . N5 N 0.66804(8) 0.59042(5) 0.41426(12) 0.0249 1.0000 Uani . . . . . . . N6 N 0.86729(10) 0.33086(6) 0.60816(16) 0.0365 1.0000 Uani . . . . . . . N7 N 0.76358(10) 0.31902(5) 0.63352(14) 0.0334 1.0000 Uani . . . . . . . O1 O 0.70322(9) 0.41040(4) 0.33235(12) 0.0371 1.0000 Uani . . . . . . . O2 O 0.69639(7) 0.48874(4) 0.34024(10) 0.0280 1.0000 Uani . . . . . . . O3 O 0.71449(7) 0.52017(4) 0.50033(10) 0.0280 1.0000 Uani . . . . . . . O4 O 0.77285(8) 0.47940(5) 0.66079(11) 0.0354 1.0000 Uani . . . . . . . O5 O 0.85128(8) 0.48188(5) 0.53042(14) 0.0394 1.0000 Uani . . . . . . . O6 O 0.82665(7) 0.40786(4) 0.55900(12) 0.0317 1.0000 Uani . . . . . . . O7 O 0.72028(7) 0.38994(4) 0.54794(11) 0.0286 1.0000 Uani . . . . . . . O8 O 0.62344(7) 0.43533(5) 0.43820(12) 0.0335 1.0000 Uani . . . . . . . S1 S 0.83889(4) 0.70740(2) 0.84483(5) 0.0469 1.0000 Uani . . . . . . . S2 S 0.83742(3) 0.62633(2) 0.43405(5) 0.0445 1.0000 Uani . . . . . . . S3 S 0.56771(3) 0.68904(2) 0.51616(6) 0.0483 1.0000 Uani . . . . . . . Na1 Na 0.74006(4) 0.45250(2) 0.48974(6) 0.0282 1.0000 Uani . . . . . . . N8 N 1.0000 0.32318(12) 0.2500 0.0574(9) 1.0000 Uiso S . . . . . . C46 C 1.0491(4) 0.3560(3) 0.2597(7) 0.075(2) 0.5000 Uiso . . . . . . . C47 C 1.018324(10) 0.3968(3) 0.215162(10) 0.117(4) 0.5000 Uiso . . . . . . . C48 C 0.9537(3) 0.31823(19) 0.1427(4) 0.0506(13) 0.5000 Uiso . . . . . . . C49 C 0.9841(3) 0.3075(2) 0.0747(5) 0.0580(15) 0.5000 Uiso . . . . . . . C50 C 1.0361(4) 0.2854(3) 0.2894(7) 0.086(2) 0.5000 Uiso . . . . . . . C51 C 1.000000(10) 0.2464(4) 0.250000(10) 0.217(6) 1.0000 Uiso S . . . . . . C52 C 0.9587(5) 0.3356(3) 0.2985(7) 0.088(3) 0.5000 Uiso . . . . . . . C53 C 0.9923(9) 0.3450(6) 0.4072(13) 0.188(7) 0.5000 Uiso . . . . . . . H43 H 0.7425 0.3585 0.3886 0.0738 1.0000 Uiso R . . . . . . H42 H 0.7184 0.3614 0.2734 0.0733 1.0000 Uiso R . . . . . . H41 H 0.6678 0.3553 0.3144 0.0743 1.0000 Uiso R . . . . . . H61 H 0.6236 0.3815 0.1566 0.0467 1.0000 Uiso R . . . . . . H71 H 0.5602 0.4183 0.0177 0.0508 1.0000 Uiso R . . . . . . H81 H 0.5649 0.4879 0.0203 0.0476 1.0000 Uiso R . . . . . . H111 H 0.6185 0.5492 0.1048 0.0359 1.0000 Uiso R . . . . . . H122 H 0.7066 0.6095 0.2805 0.0336 1.0000 Uiso R . . . . . . H121 H 0.6590 0.6066 0.1658 0.0341 1.0000 Uiso R . . . . . . H141 H 0.6036 0.6351 0.3773 0.0373 1.0000 Uiso R . . . . . . H142 H 0.5754 0.5934 0.3240 0.0368 1.0000 Uiso R . . . . . . H151 H 0.6908 0.6326 0.5121 0.0340 1.0000 Uiso R . . . . . . H171 H 0.7828 0.6322 0.6731 0.0442 1.0000 Uiso R . . . . . . H181 H 0.8436 0.5961 0.8177 0.0523 1.0000 Uiso R . . . . . . H191 H 0.8388 0.5261 0.8162 0.0465 1.0000 Uiso R . . . . . . H222 H 0.7943 0.4281 0.7292 0.0697 1.0000 Uiso R . . . . . . H221 H 0.8502 0.4595 0.7711 0.0694 1.0000 Uiso R . . . . . . H223 H 0.7923 0.4636 0.7977 0.0695 1.0000 Uiso R . . . . . . H232 H 0.6074 0.6869 0.2744 0.0627 1.0000 Uiso R . . . . . . H231 H 0.6784 0.6732 0.3199 0.0628 1.0000 Uiso R . . . . . . H233 H 0.6401 0.6798 0.2060 0.0630 1.0000 Uiso R . . . . . . H243 H 0.5214 0.6397 0.1771 0.0643 1.0000 Uiso R . . . . . . H242 H 0.5527 0.6330 0.1047 0.0651 1.0000 Uiso R . . . . . . H241 H 0.5369 0.5958 0.1561 0.0648 1.0000 Uiso R . . . . . . H253 H 0.8266 0.5381 0.5003 0.0704 1.0000 Uiso R . . . . . . H252 H 0.8957 0.5322 0.5873 0.0708 1.0000 Uiso R . . . . . . H251 H 0.8833 0.5254 0.4760 0.0702 1.0000 Uiso R . . . . . . H271 H 0.9701 0.4906 0.5589 0.0852 1.0000 Uiso R . . . . . . H281 H 1.0472 0.4398 0.5943 0.1164 1.0000 Uiso R . . . . . . H291 H 1.0232 0.3743 0.6172 0.1084 1.0000 Uiso R . . . . . . H321 H 0.9503 0.3253 0.6132 0.0622 1.0000 Uiso R . . . . . . H332 H 0.8992 0.2741 0.6114 0.0479 1.0000 Uiso R . . . . . . H331 H 0.8230 0.2785 0.5525 0.0480 1.0000 Uiso R . . . . . . H351 H 0.8317 0.3186 0.7721 0.0511 1.0000 Uiso R . . . . . . H352 H 0.7853 0.2812 0.7469 0.0512 1.0000 Uiso R . . . . . . H361 H 0.6932 0.2849 0.6179 0.0453 1.0000 Uiso R . . . . . . H381 H 0.5866 0.2880 0.4834 0.0538 1.0000 Uiso R . . . . . . H391 H 0.5025 0.3252 0.3691 0.0558 1.0000 Uiso R . . . . . . H401 H 0.5168 0.3932 0.3468 0.0492 1.0000 Uiso R . . . . . . H432 H 0.5883 0.4869 0.3769 0.0595 1.0000 Uiso R . . . . . . H431 H 0.5593 0.4501 0.3050 0.0595 1.0000 Uiso R . . . . . . H433 H 0.5369 0.4585 0.3886 0.0593 1.0000 Uiso R . . . . . . H443 H 0.8377 0.2187 0.7504 0.0719 1.0000 Uiso R . . . . . . H442 H 0.8666 0.2140 0.6738 0.0718 1.0000 Uiso R . . . . . . H441 H 0.7947 0.2269 0.6368 0.0718 1.0000 Uiso R . . . . . . H453 H 0.9174 0.2679 0.8531 0.0886 1.0000 Uiso R . . . . . . H452 H 0.9360 0.3036 0.8027 0.0887 1.0000 Uiso R . . . . . . H451 H 0.9516 0.2593 0.7856 0.0888 1.0000 Uiso R . . . . . . H461 H 1.0728 0.3475 0.2275 0.0908 0.5000 Uiso R . . . . . . H462 H 1.0758 0.3598 0.3263 0.0908 0.5000 Uiso R . . . . . . H471 H 1.0494 0.4156 0.2230 0.1425 0.5000 Uiso R . . . . . . H472 H 0.9917 0.3934 0.1483 0.1425 0.5000 Uiso R . . . . . . H473 H 1.0000 0.4057 0.2500 0.1425 1.0000 Uiso RS . . . . . . H481 H 0.9304 0.3418 0.1201 0.0619 0.5000 Uiso R . . . . . . H482 H 0.9264 0.2973 0.1385 0.0619 0.5000 Uiso R . . . . . . H491 H 0.9532 0.3044 0.0100 0.0670 0.5000 Uiso R . . . . . . H492 H 1.0112 0.3284 0.0776 0.0670 0.5000 Uiso R . . . . . . H493 H 1.0073 0.2839 0.0961 0.0670 0.5000 Uiso R . . . . . . H501 H 1.0709 0.2851 0.2754 0.1119 0.5000 Uiso R . . . . . . H502 H 1.0501 0.2851 0.3574 0.1119 0.5000 Uiso R . . . . . . H511 H 1.0259 0.2244 0.2787 0.2680 0.5000 Uiso R . . . . . . H512 H 0.9860 0.2457 0.1820 0.2680 0.5000 Uiso R . . . . . . H513 H 0.9652 0.2457 0.2640 0.2680 0.5000 Uiso R . . . . . . H521 H 0.9445 0.3614 0.2760 0.1103 0.5000 Uiso R . . . . . . H522 H 0.9240 0.3184 0.2796 0.1103 0.5000 Uiso R . . . . . . H531 H 0.9660 0.3539 0.4346 0.1795 0.5000 Uiso R . . . . . . H532 H 1.0269 0.3622 0.4259 0.1795 0.5000 Uiso R . . . . . . H533 H 1.0065 0.3192 0.4295 0.1795 0.5000 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 Mo1 0.02952(12) 0.03196(13) 0.03967(14) -0.00584(11) 0.01896(11) -0.00711(10) Ni1 0.02700(12) 0.02085(10) 0.01911(10) 0.00045(8) 0.01049(9) 0.00175(9) Ni2 0.03141(13) 0.02237(11) 0.03299(13) 0.00462(10) 0.01845(11) 0.00070(10) C1 0.0331(11) 0.0286(10) 0.0471(13) -0.0089(9) 0.0232(10) -0.0018(8) C2 0.0287(10) 0.0357(11) 0.0325(11) 0.0011(9) 0.0116(9) -0.0043(8) C3 0.0336(11) 0.0296(10) 0.0350(11) -0.0093(8) 0.0164(9) -0.0065(8) C4 0.086(2) 0.0222(10) 0.0475(14) -0.0012(9) 0.0425(15) 0.0033(11) C5 0.0415(11) 0.0252(9) 0.0335(10) -0.0036(8) 0.0247(9) -0.0024(8) C6 0.0475(13) 0.0324(11) 0.0432(13) -0.0146(9) 0.0287(11) -0.0108(10) C7 0.0398(12) 0.0478(13) 0.0347(12) -0.0183(10) 0.0153(10) -0.0102(10) C8 0.0389(12) 0.0458(13) 0.0259(10) -0.0084(9) 0.0109(9) -0.0009(10) C9 0.0316(10) 0.0323(10) 0.0245(9) -0.0037(7) 0.0130(8) 0.0002(8) C10 0.0318(10) 0.0253(8) 0.0265(9) -0.0040(7) 0.0165(8) -0.0008(7) C11 0.0331(10) 0.0331(10) 0.0216(9) 0.0042(7) 0.0108(8) 0.0046(8) C12 0.0320(10) 0.0277(9) 0.0253(9) 0.0044(7) 0.0142(8) 0.0002(8) C13 0.0271(9) 0.0241(8) 0.0269(9) 0.0044(7) 0.0104(8) 0.0026(7) C14 0.0286(10) 0.0313(10) 0.0311(10) 0.0054(8) 0.0147(8) 0.0070(8) C15 0.0361(10) 0.0231(8) 0.0289(9) -0.0004(7) 0.0187(8) 0.0016(7) C16 0.0320(10) 0.0280(9) 0.0243(9) -0.0029(7) 0.0140(8) -0.0005(8) C17 0.0417(12) 0.0338(11) 0.0306(11) -0.0080(8) 0.0147(10) -0.0063(9) C18 0.0459(14) 0.0503(14) 0.0267(11) -0.0094(10) 0.0092(10) -0.0083(11) C19 0.0389(12) 0.0450(12) 0.0239(9) 0.0015(9) 0.0086(9) -0.0004(10) C20 0.0314(10) 0.0317(10) 0.0244(9) 0.0012(7) 0.0117(8) 0.0016(8) C21 0.0271(9) 0.0283(9) 0.0219(8) -0.0010(7) 0.0115(7) 0.0007(7) C22 0.0508(15) 0.0438(13) 0.0311(11) 0.0139(10) 0.0097(11) 0.0070(11) C23 0.0515(14) 0.0271(10) 0.0470(13) 0.0017(9) 0.0256(12) -0.0012(10) C24 0.0338(12) 0.0507(14) 0.0337(12) 0.0044(10) 0.0063(10) 0.0051(10) C25 0.0544(15) 0.0304(11) 0.0570(16) 0.0028(10) 0.0310(13) -0.0102(10) C26 0.0306(11) 0.0377(12) 0.0546(15) 0.0178(11) 0.0151(11) -0.0023(9) C27 0.0370(14) 0.0556(18) 0.105(3) 0.0360(18) 0.0233(17) -0.0054(13) C28 0.0371(16) 0.079(3) 0.178(5) 0.064(3) 0.046(2) 0.0101(16) C29 0.0408(17) 0.069(2) 0.168(4) 0.062(3) 0.052(2) 0.0197(15) C30 0.0342(13) 0.0459(14) 0.090(2) 0.0319(15) 0.0308(14) 0.0093(11) C31 0.0276(10) 0.0355(11) 0.0471(13) 0.0154(10) 0.0149(10) -0.0009(8) C32 0.0419(14) 0.0426(14) 0.082(2) 0.0309(14) 0.0357(15) 0.0174(11) C33 0.0493(14) 0.0280(10) 0.0448(13) 0.0059(9) 0.0264(12) 0.0101(9) C34 0.0433(12) 0.0216(9) 0.0375(11) 0.0047(8) 0.0161(10) -0.0010(8) C35 0.0685(17) 0.0285(10) 0.0370(12) 0.0068(9) 0.0308(12) 0.0033(11) C36 0.0552(14) 0.0230(9) 0.0532(14) -0.0022(9) 0.0413(12) -0.0052(9) C37 0.0437(12) 0.0307(10) 0.0463(13) -0.0060(9) 0.0325(11) -0.0075(9) C38 0.0515(15) 0.0370(12) 0.0616(16) -0.0153(11) 0.0412(14) -0.0178(11) C39 0.0377(13) 0.0577(16) 0.0540(15) -0.0198(12) 0.0295(12) -0.0219(12) C40 0.0312(11) 0.0553(14) 0.0364(12) -0.0087(10) 0.0194(10) -0.0103(10) C41 0.0320(10) 0.0376(11) 0.0301(10) -0.0066(8) 0.0192(9) -0.0064(8) C42 0.0328(10) 0.0305(9) 0.0330(10) -0.0053(8) 0.0231(9) -0.0076(8) C43 0.0270(10) 0.0501(14) 0.0399(12) 0.0050(10) 0.0129(9) 0.0043(10) C44 0.0621(17) 0.0271(11) 0.0613(17) -0.0022(10) 0.0360(15) -0.0043(11) C45 0.0583(18) 0.0532(17) 0.0494(16) 0.0104(13) 0.0108(14) -0.0099(14) N1 0.0373(10) 0.0354(10) 0.0445(11) -0.0070(8) 0.0214(9) -0.0055(8) N2 0.0375(10) 0.0381(10) 0.0435(11) -0.0043(9) 0.0195(9) -0.0046(8) N3 0.0369(10) 0.0388(10) 0.0470(12) -0.0076(9) 0.0228(9) -0.0098(8) N4 0.0309(8) 0.0258(8) 0.0236(8) 0.0019(6) 0.0143(7) 0.0021(6) N5 0.0278(8) 0.0240(7) 0.0247(8) 0.0021(6) 0.0132(7) 0.0030(6) N6 0.0405(10) 0.0296(9) 0.0445(11) 0.0134(8) 0.0233(9) 0.0079(8) N7 0.0487(11) 0.0239(8) 0.0389(10) 0.0038(7) 0.0295(9) 0.0019(7) O1 0.0617(11) 0.0213(7) 0.0352(8) -0.0014(6) 0.0278(8) 0.0028(7) O2 0.0373(8) 0.0232(6) 0.0220(6) -0.0011(5) 0.0118(6) 0.0016(6) O3 0.0382(8) 0.0229(6) 0.0208(6) -0.0001(5) 0.0112(6) 0.0005(6) O4 0.0453(9) 0.0319(8) 0.0246(7) 0.0066(6) 0.0116(7) 0.0045(7) O5 0.0367(9) 0.0282(8) 0.0569(11) 0.0091(7) 0.0241(8) -0.0033(6) O6 0.0263(7) 0.0267(7) 0.0428(9) 0.0081(6) 0.0161(7) 0.0011(5) O7 0.0302(7) 0.0245(7) 0.0346(8) 0.0006(6) 0.0175(6) -0.0023(5) O8 0.0276(7) 0.0364(8) 0.0351(8) 0.0013(6) 0.0127(6) -0.0014(6) S1 0.0553(4) 0.0429(3) 0.0448(3) 0.0017(3) 0.0243(3) 0.0081(3) S2 0.0439(3) 0.0344(3) 0.0523(4) -0.0018(3) 0.0186(3) 0.0041(2) S3 0.0475(4) 0.0472(4) 0.0636(4) -0.0143(3) 0.0369(3) -0.0208(3) Na1 0.0304(4) 0.0230(4) 0.0314(4) 0.0030(3) 0.0138(3) 0.0008(3) _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 Mo1 . N2 4_666 2.109(2) yes Mo1 . N1 4_666 2.104(2) yes Mo1 . N3 4_666 2.0905(19) yes Mo1 . N1 . 2.104(2) yes Mo1 . N2 . 2.109(2) yes Mo1 . N3 . 2.0905(19) yes Ni1 . N4 . 1.8614(17) yes Ni1 . N5 . 1.8667(16) yes Ni1 . O2 . 1.8522(14) yes Ni1 . O3 . 1.8443(14) yes Ni2 . N6 . 1.868(2) yes Ni2 . N7 . 1.8626(18) yes Ni2 . O6 . 1.8467(14) yes Ni2 . O7 . 1.8655(15) yes C1 . N1 . 1.163(3) yes C1 . S1 . 1.630(3) yes C2 . N2 . 1.166(3) yes C2 . S2 . 1.623(2) yes C3 . N3 . 1.155(3) yes C3 . S3 . 1.616(2) yes C4 . O1 . 1.431(3) yes C4 . H43 . 0.972 no C4 . H42 . 0.964 no C4 . H41 . 0.975 no C5 . C6 . 1.381(3) yes C5 . C10 . 1.423(3) yes C5 . O1 . 1.368(3) yes C6 . C7 . 1.395(4) yes C6 . H61 . 0.944 no C7 . C8 . 1.364(4) yes C7 . H71 . 0.937 no C8 . C9 . 1.413(3) yes C8 . H81 . 0.943 no C9 . C10 . 1.405(3) yes C9 . C11 . 1.435(3) yes C10 . O2 . 1.317(2) yes C11 . N4 . 1.290(3) yes C11 . H111 . 0.949 no C12 . C13 . 1.530(3) yes C12 . N4 . 1.472(3) yes C12 . H122 . 0.974 no C12 . H121 . 0.979 no C13 . C14 . 1.535(3) yes C13 . C23 . 1.526(3) yes C13 . C24 . 1.528(3) yes C14 . N5 . 1.475(3) yes C14 . H141 . 0.975 no C14 . H142 . 0.984 no C15 . C16 . 1.433(3) yes C15 . N5 . 1.292(3) yes C15 . H151 . 0.961 no C16 . C17 . 1.413(3) yes C16 . C21 . 1.404(3) yes C17 . C18 . 1.367(4) yes C17 . H171 . 0.943 no C18 . C19 . 1.403(4) yes C18 . H181 . 0.946 no C19 . C20 . 1.376(3) yes C19 . H191 . 0.947 no C20 . C21 . 1.424(3) yes C20 . O4 . 1.368(3) yes C21 . O3 . 1.317(2) yes C22 . O4 . 1.422(3) yes C22 . H222 . 0.963 no C22 . H221 . 0.966 no C22 . H223 . 0.968 no C23 . H232 . 0.957 no C23 . H231 . 0.960 no C23 . H233 . 0.956 no C24 . H243 . 0.962 no C24 . H242 . 0.962 no C24 . H241 . 0.964 no C25 . O5 . 1.425(3) yes C25 . H253 . 0.970 no C25 . H252 . 0.958 no C25 . H251 . 0.976 no C26 . C27 . 1.374(4) yes C26 . C31 . 1.427(3) yes C26 . O5 . 1.366(3) yes C27 . C28 . 1.412(5) yes C27 . H271 . 0.948 no C28 . C29 . 1.357(5) yes C28 . H281 . 0.956 no C29 . C30 . 1.419(4) yes C29 . H291 . 0.955 no C30 . C31 . 1.409(4) yes C30 . C32 . 1.426(4) yes C31 . O6 . 1.305(3) yes C32 . N6 . 1.284(3) yes C32 . H321 . 0.956 no C33 . C34 . 1.533(3) yes C33 . N6 . 1.470(3) yes C33 . H332 . 0.981 no C33 . H331 . 0.998 no C34 . C35 . 1.534(4) yes C34 . C44 . 1.523(3) yes C34 . C45 . 1.529(4) yes C35 . N7 . 1.472(3) yes C35 . H351 . 0.979 no C35 . H352 . 0.963 no C36 . C37 . 1.437(4) yes C36 . N7 . 1.291(3) yes C36 . H361 . 0.957 no C37 . C38 . 1.414(3) yes C37 . C42 . 1.413(3) yes C38 . C39 . 1.355(4) yes C38 . H381 . 0.942 no C39 . C40 . 1.402(4) yes C39 . H391 . 0.951 no C40 . C41 . 1.384(3) yes C40 . H401 . 0.953 no C41 . C42 . 1.421(3) yes C41 . O8 . 1.368(3) yes C42 . O7 . 1.315(2) yes C43 . O8 . 1.428(3) yes C43 . H432 . 0.967 no C43 . H431 . 0.965 no C43 . H433 . 0.979 no C44 . H443 . 0.969 no C44 . H442 . 0.968 no C44 . H441 . 0.964 no C45 . H453 . 0.959 no C45 . H452 . 0.961 no C45 . H451 . 0.962 no O1 . Na1 . 2.5581(18) yes O2 . Na1 . 2.3573(16) yes O3 . Na1 . 2.3551(16) yes O4 . Na1 . 2.5116(18) yes O5 . Na1 . 2.5958(18) yes O6 . Na1 . 2.3573(17) yes O7 . Na1 . 2.3851(16) yes O8 . Na1 . 2.5593(17) yes N8 . C46 5_755 1.547(9) yes N8 . C52 5_755 1.510(9) yes N8 . C48 5_755 1.509(6) yes N8 . C50 5_755 1.486(9) yes N8 . C46 . 1.547(9) yes N8 . C48 . 1.509(6) yes N8 . C50 . 1.486(9) yes N8 . C52 . 1.510(9) yes C46 . C47 . 1.546(12) yes C46 . H461 . 0.930 no C46 . H462 . 0.930 no C47 . H471 . 0.930 no C47 . H472 . 0.930 no C47 . H473 . 0.866 no C48 . C49 . 1.530(9) yes C48 . H481 . 0.930 no C48 . H482 . 0.930 no C49 . H491 . 0.930 no C49 . H492 . 0.930 no C49 . H493 . 0.930 no C50 . C50 5_755 1.582(19) yes C50 . C51 . 1.519(13) yes C50 . H501 . 0.930 no C50 . H502 . 0.930 no C51 . H511 5_755 0.930 no C51 . H512 5_755 0.930 no C51 . H513 5_755 0.930 no C51 . H511 . 0.930 no C51 . H512 . 0.930 no C51 . H513 . 0.930 no C52 . C53 . 1.507(19) yes C52 . H521 . 0.930 no C52 . H522 . 0.930 no C53 . H492 5_755 0.619 no C53 . H531 . 0.930 no C53 . H532 . 0.930 no C53 . H533 . 0.930 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 N2 4_666 Mo1 . N1 4_666 88.49(8) yes N2 4_666 Mo1 . N3 4_666 92.20(8) yes N1 4_666 Mo1 . N3 4_666 87.24(8) yes N2 4_666 Mo1 . N1 . 91.51(8) yes N1 4_666 Mo1 . N1 . 179.995 yes N3 4_666 Mo1 . N1 . 92.76(8) yes N2 4_666 Mo1 . N2 . 179.995 yes N1 4_666 Mo1 . N2 . 91.51(8) yes N3 4_666 Mo1 . N2 . 87.80(8) yes N1 . Mo1 . N2 . 88.49(8) yes N2 4_666 Mo1 . N3 . 87.80(8) yes N1 4_666 Mo1 . N3 . 92.76(8) yes N3 4_666 Mo1 . N3 . 179.995 yes N1 . Mo1 . N3 . 87.24(8) yes N2 . Mo1 . N3 . 92.20(8) yes N4 . Ni1 . N5 . 91.33(7) yes N4 . Ni1 . O2 . 92.26(7) yes N5 . Ni1 . O2 . 175.49(7) yes N4 . Ni1 . O3 . 176.32(7) yes N5 . Ni1 . O3 . 91.72(7) yes O2 . Ni1 . O3 . 84.80(6) yes N6 . Ni2 . N7 . 90.86(8) yes N6 . Ni2 . O6 . 94.22(8) yes N7 . Ni2 . O6 . 171.63(8) yes N6 . Ni2 . O7 . 170.32(8) yes N7 . Ni2 . O7 . 91.37(8) yes O6 . Ni2 . O7 . 84.73(6) yes N1 . C1 . S1 . 179.6(2) yes N2 . C2 . S2 . 179.1(2) yes N3 . C3 . S3 . 179.0(2) yes O1 . C4 . H43 . 108.3 no O1 . C4 . H42 . 108.7 no H43 . C4 . H42 . 109.0 no O1 . C4 . H41 . 109.6 no H43 . C4 . H41 . 112.1 no H42 . C4 . H41 . 109.0 no C6 . C5 . C10 . 120.7(2) yes C6 . C5 . O1 . 125.1(2) yes C10 . C5 . O1 . 114.19(19) yes C5 . C6 . C7 . 120.4(2) yes C5 . C6 . H61 . 120.2 no C7 . C6 . H61 . 119.4 no C6 . C7 . C8 . 120.3(2) yes C6 . C7 . H71 . 119.2 no C8 . C7 . H71 . 120.6 no C7 . C8 . C9 . 120.3(2) yes C7 . C8 . H81 . 120.3 no C9 . C8 . H81 . 119.3 no C8 . C9 . C10 . 120.5(2) yes C8 . C9 . C11 . 119.9(2) yes C10 . C9 . C11 . 119.45(19) yes C5 . C10 . C9 . 117.53(19) yes C5 . C10 . O2 . 118.67(19) yes C9 . C10 . O2 . 123.79(18) yes C9 . C11 . N4 . 124.97(19) yes C9 . C11 . H111 . 117.6 no N4 . C11 . H111 . 117.4 no C13 . C12 . N4 . 111.55(16) yes C13 . C12 . H122 . 108.7 no N4 . C12 . H122 . 108.5 no C13 . C12 . H121 . 109.4 no N4 . C12 . H121 . 109.2 no H122 . C12 . H121 . 109.5 no C12 . C13 . C14 . 110.09(16) yes C12 . C13 . C23 . 108.48(18) yes C14 . C13 . C23 . 110.05(18) yes C12 . C13 . C24 . 110.00(18) yes C14 . C13 . C24 . 108.62(18) yes C23 . C13 . C24 . 109.59(19) yes C13 . C14 . N5 . 114.17(16) yes C13 . C14 . H141 . 108.9 no N5 . C14 . H141 . 109.1 no C13 . C14 . H142 . 108.8 no N5 . C14 . H142 . 106.7 no H141 . C14 . H142 . 109.0 no C16 . C15 . N5 . 124.57(18) yes C16 . C15 . H151 . 117.8 no N5 . C15 . H151 . 117.5 no C15 . C16 . C17 . 120.05(19) yes C15 . C16 . C21 . 119.02(18) yes C17 . C16 . C21 . 120.0(2) yes C16 . C17 . C18 . 120.4(2) yes C16 . C17 . H171 . 118.2 no C18 . C17 . H171 . 121.3 no C17 . C18 . C19 . 120.1(2) yes C17 . C18 . H181 . 120.9 no C19 . C18 . H181 . 118.9 no C18 . C19 . C20 . 120.5(2) yes C18 . C19 . H191 . 119.8 no C20 . C19 . H191 . 119.7 no C19 . C20 . C21 . 120.4(2) yes C19 . C20 . O4 . 126.2(2) yes C21 . C20 . O4 . 113.40(18) yes C20 . C21 . C16 . 118.29(18) yes C20 . C21 . O3 . 117.60(18) yes C16 . C21 . O3 . 124.10(18) yes O4 . C22 . H222 . 107.6 no O4 . C22 . H221 . 108.7 no H222 . C22 . H221 . 109.6 no O4 . C22 . H223 . 110.5 no H222 . C22 . H223 . 110.4 no H221 . C22 . H223 . 109.9 no C13 . C23 . H232 . 109.3 no C13 . C23 . H231 . 110.2 no H232 . C23 . H231 . 109.4 no C13 . C23 . H233 . 109.7 no H232 . C23 . H233 . 108.7 no H231 . C23 . H233 . 109.5 no C13 . C24 . H243 . 107.7 no C13 . C24 . H242 . 109.1 no H243 . C24 . H242 . 110.5 no C13 . C24 . H241 . 108.8 no H243 . C24 . H241 . 109.4 no H242 . C24 . H241 . 111.2 no O5 . C25 . H253 . 107.7 no O5 . C25 . H252 . 109.1 no H253 . C25 . H252 . 110.6 no O5 . C25 . H251 . 109.1 no H253 . C25 . H251 . 109.6 no H252 . C25 . H251 . 110.8 no C27 . C26 . C31 . 120.2(2) yes C27 . C26 . O5 . 125.4(2) yes C31 . C26 . O5 . 114.4(2) yes C26 . C27 . C28 . 121.1(3) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 119.6 no C27 . C28 . C29 . 120.0(3) yes C27 . C28 . H281 . 120.1 no C29 . C28 . H281 . 119.9 no C28 . C29 . C30 . 120.2(3) yes C28 . C29 . H291 . 120.5 no C30 . C29 . H291 . 119.3 no C29 . C30 . C31 . 120.6(3) yes C29 . C30 . C32 . 118.6(3) yes C31 . C30 . C32 . 120.8(2) yes C26 . C31 . C30 . 117.9(2) yes C26 . C31 . O6 . 118.2(2) yes C30 . C31 . O6 . 123.9(2) yes C30 . C32 . N6 . 126.4(2) yes C30 . C32 . H321 . 115.9 no N6 . C32 . H321 . 117.8 no C34 . C33 . N6 . 112.79(19) yes C34 . C33 . H332 . 107.6 no N6 . C33 . H332 . 109.8 no C34 . C33 . H331 . 109.6 no N6 . C33 . H331 . 107.8 no H332 . C33 . H331 . 109.2 no C33 . C34 . C35 . 110.40(18) yes C33 . C34 . C44 . 107.4(2) yes C35 . C34 . C44 . 110.2(2) yes C33 . C34 . C45 . 110.6(2) yes C35 . C34 . C45 . 109.0(2) yes C44 . C34 . C45 . 109.1(2) yes C34 . C35 . N7 . 113.02(18) yes C34 . C35 . H351 . 108.1 no N7 . C35 . H351 . 107.2 no C34 . C35 . H352 . 109.8 no N7 . C35 . H352 . 108.9 no H351 . C35 . H352 . 109.8 no C37 . C36 . N7 . 124.6(2) yes C37 . C36 . H361 . 117.7 no N7 . C36 . H361 . 117.7 no C36 . C37 . C38 . 120.2(2) yes C36 . C37 . C42 . 119.2(2) yes C38 . C37 . C42 . 120.2(2) yes C37 . C38 . C39 . 121.0(2) yes C37 . C38 . H381 . 118.3 no C39 . C38 . H381 . 120.7 no C38 . C39 . C40 . 119.9(2) yes C38 . C39 . H391 . 120.8 no C40 . C39 . H391 . 119.2 no C39 . C40 . C41 . 120.4(3) yes C39 . C40 . H401 . 119.4 no C41 . C40 . H401 . 120.3 no C40 . C41 . C42 . 120.8(2) yes C40 . C41 . O8 . 124.8(2) yes C42 . C41 . O8 . 114.32(18) yes C41 . C42 . C37 . 117.4(2) yes C41 . C42 . O7 . 118.79(19) yes C37 . C42 . O7 . 123.8(2) yes O8 . C43 . H432 . 107.6 no O8 . C43 . H431 . 109.2 no H432 . C43 . H431 . 109.4 no O8 . C43 . H433 . 109.6 no H432 . C43 . H433 . 111.1 no H431 . C43 . H433 . 110.0 no C34 . C44 . H443 . 108.6 no C34 . C44 . H442 . 108.7 no H443 . C44 . H442 . 109.9 no C34 . C44 . H441 . 109.3 no H443 . C44 . H441 . 110.0 no H442 . C44 . H441 . 110.2 no C34 . C45 . H453 . 108.9 no C34 . C45 . H452 . 109.1 no H453 . C45 . H452 . 110.2 no C34 . C45 . H451 . 108.6 no H453 . C45 . H451 . 110.7 no H452 . C45 . H451 . 109.4 no Mo1 . N1 . C1 . 172.33(19) yes Mo1 . N2 . C2 . 176.66(19) yes Mo1 . N3 . C3 . 168.8(2) yes C12 . N4 . C11 . 118.45(17) yes C12 . N4 . Ni1 . 116.27(13) yes C11 . N4 . Ni1 . 125.25(15) yes C14 . N5 . C15 . 118.44(17) yes C14 . N5 . Ni1 . 116.52(13) yes C15 . N5 . Ni1 . 124.72(14) yes C33 . N6 . C32 . 116.4(2) yes C33 . N6 . Ni2 . 117.29(16) yes C32 . N6 . Ni2 . 125.72(17) yes C35 . N7 . C36 . 119.2(2) yes C35 . N7 . Ni2 . 116.43(16) yes C36 . N7 . Ni2 . 124.27(17) yes C4 . O1 . C5 . 116.10(19) yes C4 . O1 . Na1 . 126.44(15) yes C5 . O1 . Na1 . 115.72(12) yes C10 . O2 . Ni1 . 124.51(13) yes C10 . O2 . Na1 . 122.99(12) yes Ni1 . O2 . Na1 . 105.48(6) yes C21 . O3 . Ni1 . 124.62(13) yes C21 . O3 . Na1 . 121.63(12) yes Ni1 . O3 . Na1 . 105.83(6) yes C22 . O4 . C20 . 117.19(19) yes C22 . O4 . Na1 . 122.96(15) yes C20 . O4 . Na1 . 115.83(12) yes C25 . O5 . C26 . 116.84(19) yes C25 . O5 . Na1 . 126.38(15) yes C26 . O5 . Na1 . 116.69(13) yes C31 . O6 . Ni2 . 127.64(14) yes C31 . O6 . Na1 . 125.81(13) yes Ni2 . O6 . Na1 . 106.53(7) yes C42 . O7 . Ni2 . 121.95(13) yes C42 . O7 . Na1 . 121.33(13) yes Ni2 . O7 . Na1 . 104.82(6) yes C43 . O8 . C41 . 117.00(18) yes C43 . O8 . Na1 . 122.51(14) yes C41 . O8 . Na1 . 115.08(13) yes O3 . Na1 . O2 . 63.87(5) yes O3 . Na1 . O6 . 140.25(7) yes O2 . Na1 . O6 . 132.22(6) yes O3 . Na1 . O7 . 135.50(6) yes O2 . Na1 . O7 . 136.62(6) yes O6 . Na1 . O7 . 63.67(5) yes O3 . Na1 . O4 . 63.93(5) yes O2 . Na1 . O4 . 127.47(6) yes O6 . Na1 . O4 . 87.52(6) yes O7 . Na1 . O4 . 87.32(6) yes O3 . Na1 . O1 . 126.56(6) yes O2 . Na1 . O1 . 64.24(5) yes O6 . Na1 . O1 . 86.42(6) yes O7 . Na1 . O1 . 79.80(6) yes O4 . Na1 . O1 . 167.12(6) yes O3 . Na1 . O8 . 87.91(6) yes O2 . Na1 . O8 . 82.50(6) yes O6 . Na1 . O8 . 126.26(6) yes O7 . Na1 . O8 . 63.91(5) yes O4 . Na1 . O8 . 101.08(6) yes O3 . Na1 . O5 . 83.33(6) yes O2 . Na1 . O5 . 89.98(6) yes O6 . Na1 . O5 . 63.39(5) yes O7 . Na1 . O5 . 125.56(6) yes O4 . Na1 . O5 . 78.69(6) yes O1 . Na1 . O8 . 73.65(6) yes O1 . Na1 . O5 . 108.51(7) yes O8 . Na1 . O5 . 170.34(6) yes C46 5_755 N8 . C52 5_755 112.0(6) yes C46 5_755 N8 . C48 5_755 109.4(4) yes C52 5_755 N8 . C48 5_755 103.8(4) yes C46 5_755 N8 . C50 5_755 106.9(5) yes C52 5_755 N8 . C50 5_755 114.4(6) yes C48 5_755 N8 . C50 5_755 110.5(5) yes C46 5_755 N8 . C46 . 90.3(7) yes C48 5_755 N8 . C46 . 79.8(4) yes C50 5_755 N8 . C46 . 154.7(5) yes C46 5_755 N8 . C48 . 79.8(4) yes C52 5_755 N8 . C48 . 79.7(4) yes C48 5_755 N8 . C48 . 167.5(6) yes C50 5_755 N8 . C48 . 57.7(4) yes C46 . N8 . C48 . 109.4(4) yes C46 5_755 N8 . C50 . 154.7(5) yes C52 5_755 N8 . C50 . 92.9(5) yes C48 5_755 N8 . C50 . 57.7(4) yes C50 5_755 N8 . C50 . 64.3(8) yes C46 . N8 . C50 . 106.9(5) yes C52 5_755 N8 . C52 . 148.2(8) yes C48 5_755 N8 . C52 . 79.7(4) yes C50 5_755 N8 . C52 . 92.9(5) yes C46 . N8 . C52 . 112.0(6) yes C48 . N8 . C50 . 110.5(5) yes C48 . N8 . C52 . 103.8(4) yes C50 . N8 . C52 . 114.4(6) yes N8 . C46 . C47 . 113.2(6) yes N8 . C46 . H461 . 109.3 no C47 . C46 . H461 . 108.2 no N8 . C46 . H462 . 108.5 no C47 . C46 . H462 . 108.1 no H461 . C46 . H462 . 109.5 no C46 . C47 . H471 . 110.4 no C46 . C47 . H472 . 109.0 no H471 . C47 . H472 . 109.5 no C46 . C47 . H473 . 107.4 no H471 . C47 . H473 . 105.3 no H472 . C47 . H473 . 115.2 no N8 . C48 . C49 . 114.6(5) yes N8 . C48 . H481 . 109.2 no C49 . C48 . H481 . 108.9 no N8 . C48 . H482 . 107.6 no C49 . C48 . H482 . 106.9 no H481 . C48 . H482 . 109.5 no C48 . C49 . H491 . 110.6 no C48 . C49 . H492 . 107.9 no H491 . C49 . H492 . 109.5 no C48 . C49 . H493 . 109.9 no H491 . C49 . H493 . 109.5 no H492 . C49 . H493 . 109.5 no C50 5_755 C50 . N8 . 57.8(4) yes C50 5_755 C50 . C51 . 58.6(5) yes N8 . C50 . C51 . 116.5(7) yes C50 5_755 C50 . H501 . 125.9 no N8 . C50 . H501 . 108.8 no C51 . C50 . H501 . 107.1 no C50 5_755 C50 . H502 . 124.7 no N8 . C50 . H502 . 108.2 no C51 . C50 . H502 . 106.6 no H501 . C50 . H502 . 109.5 no C50 5_755 C51 . C50 . 62.8(9) yes C50 5_755 C51 . H511 5_755 110.8 no C50 . C51 . H511 5_755 173.6 no C50 5_755 C51 . H512 5_755 108.5 no C50 . C51 . H512 5_755 74.1 no H511 5_755 C51 . H512 5_755 109.5 no C50 5_755 C51 . H513 5_755 109.0 no C50 . C51 . H513 5_755 73.5 no H511 5_755 C51 . H513 5_755 109.5 no H512 5_755 C51 . H513 5_755 109.5 no C50 5_755 C51 . H511 . 173.6 no C50 . C51 . H511 . 110.8 no H511 5_755 C51 . H511 . 75.6 no H512 5_755 C51 . H511 . 68.1 no H513 5_755 C51 . H511 . 68.1 no C50 5_755 C51 . H512 . 74.1 no C50 . C51 . H512 . 108.5 no H511 5_755 C51 . H512 . 68.1 no H512 5_755 C51 . H512 . 177.1 no H513 5_755 C51 . H512 . 70.4 no C50 5_755 C51 . H513 . 73.5 no C50 . C51 . H513 . 109.0 no H511 5_755 C51 . H513 . 68.1 no H512 5_755 C51 . H513 . 70.4 no H513 5_755 C51 . H513 . 177.1 no H511 . C51 . H512 . 109.5 no H511 . C51 . H513 . 109.5 no H512 . C51 . H513 . 109.5 no N8 . C52 . C53 . 116.5(10) yes N8 . C52 . H521 . 106.2 no C53 . C52 . H521 . 97.8 no N8 . C52 . H522 . 110.2 no C53 . C52 . H522 . 115.4 no H521 . C52 . H522 . 109.5 no C52 . C53 . H492 5_755 97.2 no C52 . C53 . H531 . 114.8 no H492 5_755 C53 . H531 . 84.0 no C52 . C53 . H532 . 115.2 no H492 5_755 C53 . H532 . 132.8 no H531 . C53 . H532 . 109.5 no C52 . C53 . H533 . 97.6 no H531 . C53 . H533 . 109.5 no H532 . C53 . H533 . 109.5 no C47 5_755 H473 . C47 . 139.9 no C49 . H492 . C53 5_755 119.1 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C12 . H121 . C42 6_564 169 0.98 2.60 3.565(5) yes C47 . H473 . C47 5_755 140 0.87 0.87 1.628(5) yes C50 . H502 . C49 5_755 128 0.93 1.73 2.417(5) yes C48 5_755 H502 . C51 . 129 1.11 1.99 2.822(5) yes C52 . H521 . C47 5_755 128 0.93 1.44 2.141(5) yes # Attachment '- 4_new_ccdc809270.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 809270' #TrackingRef '- 4_new_ccdc809270.cif' _audit_creation_date 11-04-19 _audit_creation_method CRYSTALS_ver_14.09 _oxford_structure_analysis_title 'JPS0941_111209_0m in Pnma' _chemical_name_systematic ? _chemical_melting_point ? _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 ; ? ; #--------------------------------------------------------------- # _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 7.4030(5) _cell_length_b 16.4860(10) _cell_length_c 18.0343(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2201.0(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_space_group_name_Hall '-P 2ac 2n' 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 x,-y+1/2,z -x,y+1/2,-z -x+1/2,-y,z+1/2 x+1/2,y,-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' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 '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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 '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' _cell_formula_units_Z 4 _chemical_formula_sum 'C22 H24 Cu1 K1 N3 O4 S1' _chemical_formula_moiety 'C22 H24 Cu1 K1 N3 O4 S1' _chemical_compound_source ? _chemical_formula_weight 529.16 _cell_measurement_reflns_used 7116 _cell_measurement_theta_min 3 _cell_measurement_theta_max 35 _cell_measurement_temperature 180 _exptl_crystal_description stick _exptl_crystal_colour green _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 1.312 # Sheldrick geometric approximatio 0.82 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.88 _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 '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 19159 _reflns_number_total 4812 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4812 # Theoretical number of reflections is about 9933 _diffrn_reflns_theta_min 2.259 _diffrn_reflns_theta_max 35.331 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 33.565 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.55 _refine_diff_density_max 0.60 # 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>3.0\s(I) _refine_ls_number_reflns 3623 _refine_ls_number_restraints 4 _refine_ls_number_parameters 159 _oxford_refine_ls_R_factor_ref 0.0292 _refine_ls_wR_factor_ref 0.0373 _refine_ls_goodness_of_fit_ref 1.0364 _refine_ls_shift/su_max 0.0292972 _refine_ls_shift/su_mean 0.0002757 # The values computed from all data _oxford_reflns_number_all 4803 _refine_ls_R_factor_all 0.0450 _refine_ls_wR_factor_all 0.0459 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3857 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_gt 0.0385 # 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: 0.921 0.653 0.627 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. 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. 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 O1 O 0.66986(17) 0.59615(6) 0.22567(5) 0.0294 1.0000 Uani . . . . . . O2 O 0.74489(14) 0.67332(5) 0.34704(5) 0.0184 1.0000 Uani . . . . . . C1 C 0.6593(2) 0.55218(10) 0.15763(8) 0.0330 1.0000 Uani . . . . . . C2 C 0.66027(18) 0.55156(8) 0.28956(7) 0.0212 1.0000 Uani . . . . . . C3 C 0.6156(2) 0.47041(8) 0.29361(9) 0.0277 1.0000 Uani . . . . . . C4 C 0.6123(2) 0.43036(8) 0.36248(9) 0.0294 1.0000 Uani . . . . . . C5 C 0.65819(19) 0.47138(8) 0.42580(8) 0.0238 1.0000 Uani . . . . . . C6 C 0.70744(16) 0.55449(7) 0.42278(6) 0.0177 1.0000 Uani . . . . . . C7 C 0.70442(16) 0.59696(7) 0.35475(6) 0.0161 1.0000 Uani . . . . . . C8 C 0.78835(16) 0.58880(7) 0.48816(6) 0.0180 1.0000 Uani . . . . . . C9 C 0.96469(18) 0.67388(8) 0.56281(6) 0.0200 1.0000 Uani . . . . . . C10 C 0.9249(2) 0.7500 0.60811(8) 0.0192 1.0000 Uani S T . . . . C11 C 0.7320(3) 0.750000(7) 0.63810(11) 0.0296 1.0000 Uani S T . . . . C12 C 1.0583(3) 0.750000(7) 0.67310(11) 0.0307 1.0000 Uani S T . . . . C13 C 1.2622(3) 0.7500 0.42162(10) 0.0226 1.0000 Uani S T . . . . Cu1 Cu 0.80138(3) 0.7500 0.424988(10) 0.0149 1.0000 Uani S T . . . . K1 K 0.46198(5) 0.7500 0.259990(19) 0.0211 1.0000 Uani S T . . . . S1 S 1.42240(7) 0.7500 0.48409(3) 0.0385 1.0000 Uani S T . . . . N1 N 0.85042(14) 0.66147(6) 0.49709(5) 0.0158 1.0000 Uani . . . . . . N2 N 1.1469(3) 0.7500 0.37773(11) 0.0352 1.0000 Uani S T . . . . H11 H 0.5436 0.5257 0.1540 0.0526 1.0000 Uiso R . . . . . H12 H 0.7528 0.5120 0.1560 0.0525 1.0000 Uiso R . . . . . H13 H 0.6729 0.5919 0.1179 0.0525 1.0000 Uiso R . . . . . H31 H 0.5896 0.4401 0.2504 0.0353 1.0000 Uiso R . . . . . H41 H 0.5803 0.3731 0.3644 0.0372 1.0000 Uiso R . . . . . H51 H 0.6599 0.4448 0.4719 0.0312 1.0000 Uiso R . . . . . H81 H 0.8031 0.5518 0.5273 0.0243 1.0000 Uiso R . . . . . H91 H 1.0909 0.6730 0.5469 0.0262 1.0000 Uiso R . . . . . H92 H 0.9462 0.6294 0.5971 0.0261 1.0000 Uiso R . . . . . H111 H 0.7041 0.7040 0.6687 0.0500 1.0000 Uiso R . . . . . H112 H 0.6549 0.7500 0.5969 0.0500 1.0000 Uiso RS . . . . . H121 H 1.1775 0.7500 0.6551 0.0396 1.0000 Uiso RS . . . . . H122 H 1.0396 0.7034 0.7022 0.0396 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 O1 0.0481(6) 0.0238(4) 0.0163(4) -0.0066(3) -0.0085(4) 0.0051(4) O2 0.0282(4) 0.0138(3) 0.0132(3) -0.0009(3) -0.0027(3) -0.0018(3) C1 0.0427(8) 0.0350(7) 0.0212(5) -0.0152(5) -0.0112(5) 0.0112(6) C2 0.0234(5) 0.0184(5) 0.0218(5) -0.0061(4) -0.0057(4) 0.0037(4) C3 0.0300(6) 0.0186(5) 0.0345(7) -0.0098(5) -0.0083(5) 0.0009(5) C4 0.0303(7) 0.0159(5) 0.0421(7) -0.0046(5) -0.0040(6) -0.0026(5) C5 0.0252(5) 0.0157(4) 0.0306(6) 0.0015(4) 0.0013(5) -0.0019(4) C6 0.0194(5) 0.0142(4) 0.0195(4) 0.0000(3) 0.0007(4) 0.0001(3) C7 0.0174(4) 0.0145(4) 0.0163(4) -0.0020(3) -0.0009(3) 0.0010(4) C8 0.0215(5) 0.0165(4) 0.0161(4) 0.0031(3) 0.0010(4) 0.0011(4) C9 0.0229(5) 0.0222(5) 0.0149(4) 0.0021(4) -0.0053(4) 0.0018(4) C10 0.0195(7) 0.0272(8) 0.0109(5) 0.0000 -0.0029(5) 0.0000 C11 0.0224(8) 0.0501(12) 0.0164(7) 0.0000 0.0041(6) 0.0000 C12 0.0355(11) 0.0379(10) 0.0188(7) 0.0000 -0.0130(7) 0.0000 C13 0.0217(7) 0.0282(8) 0.0180(7) 0.0000 0.0028(6) 0.0000 Cu1 0.02240(10) 0.01235(8) 0.00984(8) 0.0000 -0.00287(6) 0.0000 K1 0.01843(15) 0.02898(17) 0.01577(14) 0.0000 -0.00087(11) 0.0000 S1 0.0177(2) 0.0724(4) 0.0255(2) 0.0000 -0.00314(17) 0.0000 N1 0.0183(4) 0.0176(4) 0.0116(3) 0.0013(3) -0.0008(3) 0.0006(3) N2 0.0359(10) 0.0446(11) 0.0251(8) 0.0000 -0.0058(7) 0.0000 _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 O1 . C1 . 1.4272(16) yes O1 . C2 . 1.3685(17) yes O2 . C7 . 1.3015(14) yes O2 . Cu1 . 1.9363(8) yes C1 . H11 . 0.963 no C1 . H12 . 0.959 no C1 . H13 . 0.976 no C2 . C3 . 1.3800(19) yes C2 . C7 . 1.4315(16) yes C3 . C4 . 1.407(2) yes C3 . H31 . 0.946 no C4 . C5 . 1.370(2) yes C4 . H41 . 0.974 no C5 . C6 . 1.4188(17) yes C5 . H51 . 0.939 no C6 . C7 . 1.4128(16) yes C6 . C8 . 1.4384(17) yes C8 . N1 . 1.2932(15) yes C8 . H81 . 0.939 no C9 . C10 . 1.5261(15) yes C9 . N1 . 1.4705(15) yes C9 . H91 . 0.978 no C9 . H92 . 0.969 no C10 . C11 . 1.527(3) yes C10 . C12 . 1.533(2) yes C11 . H111 5_565 0.960 no C11 . H111 . 0.960 no C11 . H112 . 0.937 no C12 . H122 5_565 0.940 no C12 . H121 . 0.940 no C12 . H122 . 0.940 no C13 . S1 . 1.636(2) yes C13 . N2 . 1.165(3) yes Cu1 . S1 5_465 3.0012(6) yes Cu1 . N1 5_565 1.9882(10) yes Cu1 . N1 . 1.9882(10) yes Cu1 . N2 . 2.696(2) 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 C1 . O1 . C2 . 116.62(12) yes C7 . O2 . Cu1 . 127.13(7) yes O1 . C1 . H11 . 109.7 no O1 . C1 . H12 . 109.7 no H11 . C1 . H12 . 109.1 no O1 . C1 . H13 . 106.5 no H11 . C1 . H13 . 110.2 no H12 . C1 . H13 . 111.5 no O1 . C2 . C3 . 125.29(12) yes O1 . C2 . C7 . 113.50(11) yes C3 . C2 . C7 . 121.20(12) yes C2 . C3 . C4 . 120.40(12) yes C2 . C3 . H31 . 121.1 no C4 . C3 . H31 . 118.5 no C3 . C4 . C5 . 119.98(13) yes C3 . C4 . H41 . 119.3 no C5 . C4 . H41 . 120.7 no C4 . C5 . C6 . 120.56(13) yes C4 . C5 . H51 . 120.7 no C6 . C5 . H51 . 118.7 no C5 . C6 . C7 . 120.52(11) yes C5 . C6 . C8 . 117.09(11) yes C7 . C6 . C8 . 121.57(10) yes C2 . C7 . C6 . 117.24(11) yes C2 . C7 . O2 . 118.07(10) yes C6 . C7 . O2 . 124.65(10) yes C6 . C8 . N1 . 127.91(10) yes C6 . C8 . H81 . 114.2 no N1 . C8 . H81 . 117.8 no C10 . C9 . N1 . 115.77(11) yes C10 . C9 . H91 . 110.7 no N1 . C9 . H91 . 108.1 no C10 . C9 . H92 . 104.7 no N1 . C9 . H92 . 109.1 no H91 . C9 . H92 . 108.1 no C9 . C10 . C9 5_565 110.63(13) yes C9 . C10 . C11 . 111.73(10) yes C9 5_565 C10 . C11 . 111.73(10) yes C9 . C10 . C12 . 106.54(10) yes C9 5_565 C10 . C12 . 106.54(10) yes C11 . C10 . C12 . 109.38(15) yes C10 . C11 . H111 5_565 113.9 no C10 . C11 . H111 . 113.9 no H111 5_565 C11 . H111 . 104.2 no C10 . C11 . H112 . 106.8 no H111 5_565 C11 . H112 . 109.0 no H111 . C11 . H112 . 109.0 no C10 . C12 . H122 5_565 109.4 no C10 . C12 . H121 . 110.0 no H122 5_565 C12 . H121 . 109.3 no C10 . C12 . H122 . 109.4 no H122 5_565 C12 . H122 . 109.5 no H121 . C12 . H122 . 109.3 no S1 . C13 . N2 . 179.29(19) yes S1 5_465 Cu1 . N1 5_565 86.47(3) yes S1 5_465 Cu1 . O2 . 93.21(3) yes N1 5_565 Cu1 . O2 . 173.49(4) yes S1 5_465 Cu1 . O2 5_565 93.21(3) yes N1 5_565 Cu1 . O2 5_565 92.01(4) yes O2 . Cu1 . O2 5_565 81.51(5) yes S1 5_465 Cu1 . N1 . 86.47(3) yes N1 5_565 Cu1 . N1 . 94.47(6) yes O2 . Cu1 . N1 . 92.01(4) yes O2 5_565 Cu1 . N1 . 173.49(4) yes S1 5_465 Cu1 . N2 . 177.63(4) yes N1 5_565 Cu1 . N2 . 91.92(4) yes O2 . Cu1 . N2 . 88.59(4) yes O2 5_565 Cu1 . N2 . 88.59(4) yes N1 . Cu1 . N2 . 91.92(4) yes C13 . S1 . Cu1 1_655 115.66(7) yes C9 . N1 . C8 . 115.70(10) yes C9 . N1 . Cu1 . 122.01(8) yes C8 . N1 . Cu1 . 122.26(8) yes Cu1 . N2 . C13 . 118.75(16) yes # Attachment '3910_web_deposit_cif_file_4_Jean-PascalSutter_1295611074.cif' data_cpd1102 _database_code_depnum_ccdc_archive 'CCDC 809271' #TrackingRef '3910_web_deposit_cif_file_4_Jean-PascalSutter_1295611074.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 ; ? ; #--------------------------------------------------------------- # _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 18.190(9) _cell_length_b 18.190(9) _cell_length_c 11.780(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3376(3) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1 ' _symmetry_space_group_name_Hall 'P 31 2" ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+y,-x,z+2/3 -x,-x+y,-z+1/3 -y,x-y,z+1/3 x-y,-y,-z+2/3 y,x,-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' 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' 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 3 _chemical_formula_sum 'C40 H47 K1 N4 Ni2 O10' _chemical_formula_moiety 'C40 H47 K1 N4 Ni2 O10' _chemical_compound_source ? _chemical_formula_weight 900.36 _cell_measurement_reflns_used 9625 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 110 _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1401 _exptl_absorpt_coefficient_mu 0.985 # Sheldrick geometric approximatio 0.95 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.95 _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 110 _diffrn_reflns_number 65962 _reflns_number_total 5715 _diffrn_reflns_av_R_equivalents 0.084 # Number of reflections without Friedels Law is 5715 # Number of reflections with Friedels Law is 3121 # Theoretical number of reflections is about 2875 _diffrn_reflns_theta_min 1.293 _diffrn_reflns_theta_max 28.583 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.011 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -24 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.73 _refine_diff_density_max 1.06 # 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>3.0\s(I) _refine_ls_number_reflns 3624 _refine_ls_number_restraints 0 _refine_ls_number_parameters 262 _oxford_refine_ls_R_factor_ref 0.0797 _refine_ls_wR_factor_ref 0.0859 _refine_ls_goodness_of_fit_ref 1.0524 _refine_ls_shift/su_max 0.0002136 _refine_ls_shift/su_mean 0.0000109 # The values computed from all data _oxford_reflns_number_all 5696 _refine_ls_R_factor_all 0.1189 _refine_ls_wR_factor_all 0.1274 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4037 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_gt 0.0892 _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_abs_structure_details 'Flack (1983), 2576 Friedel-pairs' # 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 ad _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: 2.26 1.17 1.62 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Flack, H. D. (1983). Acta Cryst. A39, 876-881. 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 0.40991(6) 0.54078(6) 0.50771(6) 0.0416 1.0000 Uani . . . . . . K1 K 0.64565(12) 0.64565(12) 0.5000 0.0434 1.0000 Uani S T . . . . C1 C 0.4782(4) 0.6805(4) 0.3585(4) 0.0314 1.0000 Uani . . . . . . C2 C 0.5455(5) 0.7601(4) 0.3236(4) 0.0376 1.0000 Uani . . . . . . C3 C 0.5400(6) 0.8036(6) 0.2300(5) 0.0530 1.0000 Uani . . . . . . C4 C 0.4607(7) 0.7651(7) 0.1687(5) 0.0639 1.0000 Uani . . . . . . C5 C 0.3951(6) 0.6891(7) 0.1987(6) 0.0593 1.0000 Uani . . . . . . C6 C 0.4018(5) 0.6445(6) 0.2944(5) 0.0487 1.0000 Uani . . . . . . C7 C 0.3288(5) 0.5655(6) 0.3243(7) 0.0537 1.0000 Uani . . . . . . C8 C 0.6872(6) 0.8687(6) 0.3559(7) 0.0619 1.0000 Uani . . . . . . C9 C 0.2398(7) 0.4379(6) 0.4506(11) 0.0877 1.0000 Uani . . . . . . C10 C 0.2646(8) 0.3843(8) 0.5055(13) 0.0960 1.0000 Uani . . . . . . C11 C 0.1855(7) 0.3977(8) 0.3481(9) 0.0870 1.0000 Uani . . . . . . C12 C 0.1967(5) 0.4672(6) 0.5437(8) 0.0601 1.0000 Uani . . . . . . C13 C 0.4914(6) 0.5171(5) 0.6985(5) 0.0490 1.0000 Uani . . . . . . C14 C 0.5605(6) 0.5471(6) 0.7719(5) 0.0527 1.0000 Uani . . . . . . C15 C 0.5607(8) 0.4996(7) 0.8642(6) 0.0798 1.0000 Uani . . . . . . C16 C 0.4937(11) 0.4222(9) 0.8878(10) 0.0958 1.0000 Uani . . . . . . C17 C 0.4249(10) 0.3907(7) 0.8194(11) 0.0935 1.0000 Uani . . . . . . C18 C 0.4194(6) 0.4368(5) 0.7223(7) 0.0600 1.0000 Uani . . . . . . C19 C 0.3458(7) 0.4026(5) 0.6551(8) 0.0753 1.0000 Uani . . . . . . C20 C 0.6951(6) 0.6640(7) 0.8218(5) 0.0631 1.0000 Uani . . . . . . N1 N 0.3243(4) 0.5185(4) 0.4071(7) 0.0575 1.0000 Uani . . . . . . N2 N 0.3344(5) 0.4376(5) 0.5675(6) 0.0714 1.0000 Uani . . . . . . O1 O 0.4875(3) 0.6445(3) 0.4470(3) 0.0367 1.0000 Uani . . . . . . O2 O 0.4934(3) 0.5641(3) 0.6124(3) 0.0424 1.0000 Uani . . . . . . O3 O 0.6164(3) 0.7890(3) 0.3893(4) 0.0462 1.0000 Uani . . . . . . O4 O 0.6263(4) 0.6236(4) 0.7429(3) 0.0485 1.0000 Uani . . . . . . O5 O 0.7825(11) 0.8129(13) 0.5811(18) 0.1126 0.5000 Uani . . . . . . O6 O 0.9894(15) 0.8003(11) 0.9248(18) 0.1230 0.5000 Uani . . . . . . H31 H 0.5855 0.8563 0.2088 0.0607 1.0000 Uiso R . . . . . H41 H 0.4547 0.7934 0.1064 0.0728 1.0000 Uiso R . . . . . H51 H 0.3450 0.6661 0.1580 0.0742 1.0000 Uiso R . . . . . H71 H 0.2795 0.5459 0.2802 0.0623 1.0000 Uiso R . . . . . H81 H 0.7319 0.8881 0.4110 0.0948 1.0000 Uiso R . . . . . H82 H 0.6707 0.9111 0.3482 0.0946 1.0000 Uiso R . . . . . H83 H 0.7101 0.8640 0.2839 0.0947 1.0000 Uiso R . . . . . H112 H 0.1683 0.4354 0.3145 0.1331 1.0000 Uiso R . . . . . H111 H 0.1362 0.3462 0.3746 0.1329 1.0000 Uiso R . . . . . H113 H 0.2163 0.3839 0.2925 0.1330 1.0000 Uiso R . . . . . H123 H 0.1618 0.4862 0.5077 0.0880 1.0000 Uiso R . . . . . H121 H 0.2397 0.5126 0.5876 0.0879 1.0000 Uiso R . . . . . H122 H 0.1614 0.4193 0.5915 0.0885 1.0000 Uiso R . . . . . H151 H 0.6086 0.5217 0.9107 0.0932 1.0000 Uiso R . . . . . H161 H 0.4946 0.3915 0.9508 0.1120 1.0000 Uiso R . . . . . H171 H 0.3791 0.3366 0.8355 0.1120 1.0000 Uiso R . . . . . H191 H 0.3009 0.3499 0.6764 0.0870 1.0000 Uiso R . . . . . H202 H 0.7377 0.7184 0.7928 0.0980 1.0000 Uiso R . . . . . H201 H 0.6743 0.6713 0.8945 0.0978 1.0000 Uiso R . . . . . H203 H 0.7202 0.6290 0.8320 0.0979 1.0000 Uiso R . . . . . H101 H 0.2206 0.3490 0.5540 0.1299 1.0000 Uiso R . . . . . H102 H 0.2728 0.3547 0.4540 0.1299 1.0000 Uiso . . . . . . 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 0.0448(5) 0.0476(5) 0.0301(3) -0.0032(4) 0.0081(3) 0.0213(4) K1 0.0563(9) 0.0563(9) 0.0190(6) 0.0010(4) -0.0010(4) 0.0293(11) C1 0.049(4) 0.040(3) 0.019(2) -0.008(2) -0.001(2) 0.031(3) C2 0.064(4) 0.050(4) 0.017(2) -0.004(2) 0.000(2) 0.042(4) C3 0.089(6) 0.077(5) 0.023(2) 0.012(3) 0.015(3) 0.064(5) C4 0.109(8) 0.106(7) 0.020(3) -0.001(4) -0.007(4) 0.087(7) C5 0.080(6) 0.106(7) 0.021(3) -0.013(4) -0.013(3) 0.069(6) C6 0.063(5) 0.084(6) 0.027(3) -0.020(3) -0.017(3) 0.058(5) C7 0.050(4) 0.067(5) 0.058(5) -0.031(4) -0.022(3) 0.040(4) C8 0.069(5) 0.054(5) 0.049(4) 0.009(4) 0.018(4) 0.019(4) C9 0.055(4) 0.058(4) 0.135(7) -0.023(4) -0.014(4) 0.017(3) C10 0.063(4) 0.066(4) 0.144(7) -0.023(4) -0.014(4) 0.021(3) C11 0.075(7) 0.095(8) 0.072(6) -0.017(6) -0.003(5) 0.028(6) C12 0.043(4) 0.076(6) 0.064(5) -0.008(4) 0.007(4) 0.032(4) C13 0.087(6) 0.057(4) 0.024(3) 0.006(3) 0.017(3) 0.051(4) C14 0.089(6) 0.086(6) 0.019(3) 0.013(3) 0.016(3) 0.070(5) C15 0.142(10) 0.119(9) 0.032(3) 0.037(4) 0.042(5) 0.105(8) C16 0.175(14) 0.122(11) 0.059(6) 0.053(7) 0.062(8) 0.126(12) C17 0.168(13) 0.066(6) 0.081(7) 0.042(6) 0.081(9) 0.084(8) C18 0.087(6) 0.041(4) 0.045(4) 0.009(3) 0.043(4) 0.026(4) C19 0.088(7) 0.038(4) 0.057(5) -0.008(4) 0.039(5) 0.000(5) C20 0.083(6) 0.109(8) 0.027(3) -0.012(4) -0.014(3) 0.070(6) N1 0.046(4) 0.046(4) 0.079(5) -0.021(3) -0.010(3) 0.021(3) N2 0.070(5) 0.061(4) 0.042(3) -0.004(3) 0.030(3) 0.002(4) O1 0.042(2) 0.044(3) 0.0278(19) 0.0057(18) 0.0008(17) 0.024(2) O2 0.060(3) 0.044(3) 0.0188(16) 0.0089(17) 0.0072(17) 0.022(2) O3 0.056(3) 0.048(3) 0.028(2) 0.0069(19) 0.009(2) 0.022(2) O4 0.072(3) 0.077(3) 0.0189(17) 0.0013(19) 0.0001(19) 0.053(3) O5 0.071(10) 0.122(14) 0.125(14) 0.026(12) -0.008(10) 0.034(10) O6 0.147(18) 0.074(10) 0.119(15) 0.028(10) 0.040(13) 0.033(11) _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 . 1.833(7) yes Ni1 . N2 . 1.823(7) yes Ni1 . O1 . 1.844(5) yes Ni1 . O2 . 1.834(5) yes C1 . C2 . 1.410(10) yes C1 . C6 . 1.422(10) yes C1 . O1 . 1.286(7) yes C2 . C3 . 1.391(8) yes C2 . O3 . 1.364(8) yes C3 . C4 . 1.443(13) yes C3 . H31 . 0.934 no C4 . C5 . 1.346(14) yes C4 . H41 . 0.934 no C5 . C6 . 1.428(11) yes C5 . H51 . 0.924 no C6 . C7 . 1.430(13) yes C7 . N1 . 1.273(12) yes C7 . H71 . 0.939 no C8 . O3 . 1.431(9) yes C8 . H81 . 0.959 no C8 . H82 . 0.962 no C8 . H83 . 0.968 no C9 . C10 . 1.418(18) yes C9 . C11 . 1.498(15) yes C9 . C12 . 1.588(14) yes C9 . N1 . 1.588(13) yes C10 . N2 . 1.362(14) yes C10 . H101 . 0.930 no C10 . H102 . 0.872 no C11 . H112 . 0.970 no C11 . H111 . 0.970 no C11 . H113 . 0.973 no C12 . H123 . 0.959 no C12 . H121 . 0.957 no C12 . H122 . 0.963 no C13 . C14 . 1.393(12) yes C13 . C18 . 1.420(12) yes C13 . O2 . 1.315(8) yes C14 . C15 . 1.389(10) yes C14 . O4 . 1.350(11) yes C15 . C16 . 1.352(18) yes C15 . H151 . 0.933 no C16 . C17 . 1.35(2) yes C16 . H161 . 0.934 no C17 . C18 . 1.450(15) yes C17 . H171 . 0.938 no C18 . C19 . 1.404(15) yes C19 . N2 . 1.283(14) yes C19 . H191 . 0.931 no C20 . O4 . 1.432(9) yes C20 . H202 . 0.964 no C20 . H201 . 0.972 no C20 . H203 . 0.959 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 . N2 . 84.4(4) yes N1 . Ni1 . O1 . 96.1(3) yes N2 . Ni1 . O1 . 179.0(3) yes N1 . Ni1 . O2 . 177.8(3) yes N2 . Ni1 . O2 . 95.1(3) yes O1 . Ni1 . O2 . 84.38(19) yes C2 . C1 . C6 . 117.7(6) yes C2 . C1 . O1 . 119.4(6) yes C6 . C1 . O1 . 122.9(6) yes C1 . C2 . C3 . 122.9(7) yes C1 . C2 . O3 . 113.5(5) yes C3 . C2 . O3 . 123.6(7) yes C2 . C3 . C4 . 117.4(8) yes C2 . C3 . H31 . 121.2 no C4 . C3 . H31 . 121.5 no C3 . C4 . C5 . 121.6(7) yes C3 . C4 . H41 . 119.3 no C5 . C4 . H41 . 119.0 no C4 . C5 . C6 . 120.5(8) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.8 no C5 . C6 . C1 . 119.9(8) yes C5 . C6 . C7 . 117.7(8) yes C1 . C6 . C7 . 122.3(7) yes C6 . C7 . N1 . 125.4(7) yes C6 . C7 . H71 . 118.4 no N1 . C7 . H71 . 116.2 no O3 . C8 . H81 . 110.8 no O3 . C8 . H82 . 110.9 no H81 . C8 . H82 . 108.4 no O3 . C8 . H83 . 111.2 no H81 . C8 . H83 . 107.5 no H82 . C8 . H83 . 108.0 no C10 . C9 . C11 . 113.0(10) yes C10 . C9 . C12 . 107.2(11) yes C11 . C9 . C12 . 113.8(9) yes C10 . C9 . N1 . 106.8(9) yes C11 . C9 . N1 . 106.7(10) yes C12 . C9 . N1 . 109.0(7) yes C9 . C10 . N2 . 104.9(10) yes C9 . C10 . H101 . 107.1 no N2 . C10 . H101 . 109.7 no C9 . C10 . H102 . 108.5 no N2 . C10 . H102 . 115.2 no H101 . C10 . H102 . 110.9 no C9 . C11 . H112 . 110.6 no C9 . C11 . H111 . 106.1 no H112 . C11 . H111 . 110.2 no C9 . C11 . H113 . 110.2 no H112 . C11 . H113 . 109.8 no H111 . C11 . H113 . 109.8 no C9 . C12 . H123 . 110.1 no C9 . C12 . H121 . 109.5 no H123 . C12 . H121 . 109.3 no C9 . C12 . H122 . 108.5 no H123 . C12 . H122 . 108.8 no H121 . C12 . H122 . 110.6 no C14 . C13 . C18 . 117.9(7) yes C14 . C13 . O2 . 119.9(7) yes C18 . C13 . O2 . 122.2(8) yes C13 . C14 . C15 . 121.6(9) yes C13 . C14 . O4 . 114.1(6) yes C15 . C14 . O4 . 124.3(9) yes C14 . C15 . C16 . 121.8(12) yes C14 . C15 . H151 . 118.9 no C16 . C15 . H151 . 119.3 no C15 . C16 . C17 . 118.7(9) yes C15 . C16 . H161 . 120.6 no C17 . C16 . H161 . 120.7 no C16 . C17 . C18 . 122.8(11) yes C16 . C17 . H171 . 118.1 no C18 . C17 . H171 . 119.0 no C17 . C18 . C13 . 117.1(10) yes C17 . C18 . C19 . 121.0(10) yes C13 . C18 . C19 . 121.9(8) yes C18 . C19 . N2 . 126.1(7) yes C18 . C19 . H191 . 117.1 no N2 . C19 . H191 . 116.8 no O4 . C20 . H202 . 110.0 no O4 . C20 . H201 . 109.9 no H202 . C20 . H201 . 109.8 no O4 . C20 . H203 . 109.0 no H202 . C20 . H203 . 108.8 no H201 . C20 . H203 . 109.3 no C9 . N1 . C7 . 125.1(8) yes C9 . N1 . Ni1 . 108.6(7) yes C7 . N1 . Ni1 . 125.8(6) yes C10 . N2 . C19 . 113.7(9) yes C10 . N2 . Ni1 . 118.7(8) yes C19 . N2 . Ni1 . 126.6(7) yes C1 . O1 . Ni1 . 127.4(4) yes C13 . O2 . Ni1 . 128.1(5) yes C8 . O3 . C2 . 115.6(6) yes C20 . O4 . C14 . 117.5(6) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C19 . H191 . O6 5_566 174 0.93 2.58 3.504(15) yes