Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vefa Ahsen' _publ_contact_author_address ; Department of Chemistry Gebze Institute of Technology, P.O. Box: 141, Gebze Kocaeli 41400 TURKEY ; _publ_contact_author_email AHSEN@GYTE.EDU.TR _publ_section_title ; Channel architecture via self assembly of oxamide oximes complexes ; _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. ; _publ_section_figure_captions ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). Gorbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; loop_ _publ_author_name 'Vefa Ahsen' 'Yurii M. Chumakov' 'Gulay Gumus' 'Ilke Gurol' 'Erwan Jeanneau' 'Dominique Luneau' ; F.Yuksel ; data_VAC4Ni4 _database_code_depnum_ccdc_archive 'CCDC 648644' _audit_creation_date 07-07-10 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '97172bis in space group P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.0434(3) _cell_length_b 11.3454(3) _cell_length_c 12.0362(4) _cell_angle_alpha 115.947(1) _cell_angle_beta 106.043(1) _cell_angle_gamma 90.939(1) _cell_volume 1286.66(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -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' 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' _cell_formula_units_Z 2 # Given Formula = C20 H42 N8 Ni1 O4 # Dc = 1.34 Fooo = 556.00 Mu = 7.95 M = 517.32 # Found Formula = C20 H42 N8 Ni1 O4 # Dc = 1.34 FOOO = 556.00 Mu = 7.95 M = 517.32 _chemical_formula_sum 'C20 H42 N8 Ni1 O4' _chemical_formula_moiety 'C20 H42 N8 Ni1 O4' _chemical_compound_source ? _chemical_formula_weight 517.32 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.795 # Sheldrick geometric approximatio 0.92 0.92 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 150 _diffrn_reflns_number 10009 _reflns_number_total 5656 _diffrn_reflns_av_R_equivalents 0.058 # Number of reflections with Friedels Law is 5656 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5855 _diffrn_reflns_theta_min 2.022 _diffrn_reflns_theta_max 27.405 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.212 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.39 _refine_diff_density_max 0.56 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3398 _refine_ls_number_restraints 0 _refine_ls_number_parameters 301 _oxford_refine_ls_R_factor_ref 0.0494 _refine_ls_wR_factor_ref 0.0507 _refine_ls_goodness_of_fit_ref 1.1311 _refine_ls_shift/su_max 0.000139 # The values computed from all data _oxford_reflns_number_all 5647 _refine_ls_R_factor_all 0.1015 _refine_ls_wR_factor_all 0.0832 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3398 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_gt 0.0507 # 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: 0.357 0.692E-01 0.159 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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 Ni1 Ni 1.0000 1.0000 1.0000 0.0264 1.0000 Uani S . . . . . . Ni2 Ni 0.5000 0.5000 0.0000 0.0270 1.0000 Uani S . . . . . . O2A O 0.7838(2) 0.9995(2) 0.8018(2) 0.0305 1.0000 Uani . . . . . . . O1A O 1.0164(3) 0.8585(3) 1.1502(3) 0.0405 1.0000 Uani . . . . . . . N2A N 0.8345(3) 0.9447(3) 0.8813(3) 0.0282 1.0000 Uani . . . . . . . N1A N 0.9418(3) 0.8839(3) 1.0518(3) 0.0296 1.0000 Uani . . . . . . . N3A N 0.6383(3) 0.8048(3) 0.8129(3) 0.0321 1.0000 Uani . . . . . . . N4A N 0.7645(3) 0.7299(4) 1.0070(3) 0.0411 1.0000 Uani . . . . . . . C1A C 0.7618(3) 0.8553(3) 0.8847(3) 0.0279 1.0000 Uani . . . . . . . C2A C 0.8274(3) 0.8187(3) 0.9889(3) 0.0296 1.0000 Uani . . . . . . . C11A C 0.5822(4) 0.7785(4) 0.6766(4) 0.0347 1.0000 Uani . . . . . . . C12A C 0.6561(4) 0.6975(4) 0.5889(4) 0.0380 1.0000 Uani . . . . . . . C13A C 0.6810(4) 0.5677(4) 0.5925(4) 0.0410 1.0000 Uani . . . . . . . C14A C 0.7450(5) 0.4844(5) 0.4933(5) 0.0608 1.0000 Uani . . . . . . . C21A C 0.8026(4) 0.6963(4) 1.1159(4) 0.0400 1.0000 Uani . . . . . . . C22A C 0.8786(4) 0.5827(4) 1.0917(4) 0.0401 1.0000 Uani . . . . . . . C23A C 0.9079(5) 0.5456(5) 1.2032(5) 0.0512 1.0000 Uani . . . . . . . C24A C 0.9919(5) 0.4374(6) 1.1836(6) 0.0653 1.0000 Uani . . . . . . . O1B O 0.5446(3) 0.4311(3) -0.2436(3) 0.0507 1.0000 Uani . . . . . . . O2B O 0.4726(3) 0.6447(3) -0.1458(2) 0.0334 1.0000 Uani . . . . . . . N1B N 0.5513(3) 0.3980(3) -0.1442(3) 0.0316 1.0000 Uani . . . . . . . N2B N 0.4541(3) 0.6378(3) -0.0400(3) 0.0266 1.0000 Uani . . . . . . . N3B N 0.6510(4) 0.2114(3) -0.2388(3) 0.0424 1.0000 Uani . . . . . . . N4B N 0.3759(3) 0.8452(3) 0.0359(3) 0.0378 1.0000 Uani . . . . . . . C1B C 0.5987(3) 0.2931(4) -0.1493(3) 0.0300 1.0000 Uani . . . . . . . C2B C 0.4079(3) 0.7323(3) 0.0386(3) 0.0274 1.0000 Uani . . . . . . . C11B C 0.6904(5) 0.2409(5) -0.3331(5) 0.0520 1.0000 Uani . . . . . . . C12B C 0.7518(5) 0.1320(5) -0.4123(4) 0.0480 1.0000 Uani . . . . . . . C13B C 0.6701(5) 0.0003(5) -0.4988(5) 0.0543 1.0000 Uani . . . . . . . C14B C 0.7349(7) -0.1057(6) -0.5797(6) 0.0779 1.0000 Uani . . . . . . . C21B C 0.3522(4) 0.8761(4) -0.0735(4) 0.0330 1.0000 Uani . . . . . . . C22B C 0.2223(4) 0.8127(4) -0.1738(4) 0.0350 1.0000 Uani . . . . . . . C23B C 0.1911(4) 0.8642(4) -0.2738(4) 0.0424 1.0000 Uani . . . . . . . C24B C 0.0574(5) 0.8087(6) -0.3698(5) 0.0654 1.0000 Uani . . . . . . . H11A H 0.5760 0.8631 0.6741 0.0405 1.0000 Uiso R . . . . . . H112 H 0.4985 0.7298 0.6457 0.0399 1.0000 Uiso R . . . . . . H121 H 0.7371 0.7514 0.6137 0.0440 1.0000 Uiso R . . . . . . H122 H 0.6082 0.6782 0.5002 0.0440 1.0000 Uiso R . . . . . . H131 H 0.7346 0.5876 0.6791 0.0459 1.0000 Uiso R . . . . . . H132 H 0.6004 0.5170 0.5749 0.0465 1.0000 Uiso R . . . . . . H141 H 0.7599 0.4042 0.4997 0.0821 1.0000 Uiso R . . . . . . H142 H 0.8263 0.5332 0.5101 0.0818 1.0000 Uiso R . . . . . . H143 H 0.6904 0.4624 0.4066 0.0821 1.0000 Uiso R . . . . . . H21A H 0.7252 0.6702 1.1273 0.0498 1.0000 Uiso R . . . . . . H212 H 0.8524 0.7732 1.1933 0.0495 1.0000 Uiso R . . . . . . H221 H 0.8303 0.5058 1.0116 0.0491 1.0000 Uiso R . . . . . . H222 H 0.9588 0.6083 1.0831 0.0492 1.0000 Uiso R . . . . . . H231 H 0.8274 0.5136 1.2060 0.0630 1.0000 Uiso R . . . . . . H232 H 0.9503 0.6239 1.2846 0.0627 1.0000 Uiso R . . . . . . H241 H 1.0056 0.4128 1.2525 0.1099 1.0000 Uiso R . . . . . . H242 H 0.9498 0.3606 1.1011 0.1098 1.0000 Uiso R . . . . . . H243 H 1.0729 0.4714 1.1832 0.1098 1.0000 Uiso R . . . . . . H271 H 0.6139 0.2496 -0.3923 0.0741 1.0000 Uiso R . . . . . . H272 H 0.7490 0.3238 -0.2861 0.0738 1.0000 Uiso R . . . . . . H14D H 0.8250 0.1189 -0.3522 0.0610 1.0000 Uiso R . . . . . . H282 H 0.7829 0.1619 -0.4655 0.0610 1.0000 Uiso R . . . . . . H291 H 0.6413 -0.0305 -0.4458 0.0678 1.0000 Uiso R . . . . . . H292 H 0.5970 0.0109 -0.5594 0.0680 1.0000 Uiso R . . . . . . H301 H 0.6757 -0.1877 -0.6367 0.1289 1.0000 Uiso R . . . . . . H302 H 0.8064 -0.1199 -0.5214 0.1290 1.0000 Uiso R . . . . . . H303 H 0.7668 -0.0743 -0.6307 0.1289 1.0000 Uiso R . . . . . . H311 H 0.3572 0.9715 -0.0383 0.0425 1.0000 Uiso R . . . . . . H21C H 0.4175 0.8492 -0.1138 0.0426 1.0000 Uiso R . . . . . . H22C H 0.1579 0.8320 -0.1307 0.0428 1.0000 Uiso R . . . . . . H322 H 0.2193 0.7173 -0.2171 0.0428 1.0000 Uiso R . . . . . . H331 H 0.2011 0.9608 -0.2284 0.0517 1.0000 Uiso R . . . . . . H332 H 0.2523 0.8391 -0.3219 0.0515 1.0000 Uiso R . . . . . . H341 H 0.0408 0.8453 -0.4298 0.0950 1.0000 Uiso R . . . . . . H24E H -0.0045 0.8297 -0.3245 0.0948 1.0000 Uiso R . . . . . . H343 H 0.0488 0.7131 -0.4176 0.0949 1.0000 Uiso R . . . . . . H3BA H 0.6659 0.1376 -0.2380 0.0596 1.0000 Uiso R . . . . . . H4 H 0.5131 0.4996 -0.2181 0.0906 1.0000 Uiso R . . . . . . H5 H 0.5905 0.7811 0.8466 0.0403 1.0000 Uiso R . . . . . . H7 H 1.0851 0.9060 1.1735 0.0617 1.0000 Uiso R . . . . . . H4BA H 0.3618 0.9032 0.1027 0.0484 1.0000 Uiso R . . . . . . H4AA H 0.6932 0.6874 0.9486 0.0513 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0263(4) 0.0262(4) 0.0274(4) 0.0137(3) 0.0071(3) 0.0051(3) Ni2 0.0310(4) 0.0262(4) 0.0268(4) 0.0139(3) 0.0104(3) 0.0071(3) O2A 0.0301(13) 0.0301(13) 0.0315(13) 0.0184(11) 0.0030(10) 0.0046(10) O1A 0.0311(16) 0.0485(18) 0.0452(18) 0.0339(15) -0.0035(13) -0.0044(13) N1A 0.0296(15) 0.0290(15) 0.0280(15) 0.0151(13) 0.0087(12) 0.0094(12) N2A 0.0296(16) 0.0347(16) 0.0284(15) 0.0194(13) 0.0065(13) 0.0077(13) N3A 0.0298(16) 0.0386(17) 0.0316(16) 0.0178(14) 0.0122(13) 0.0068(13) N4A 0.0362(19) 0.050(2) 0.0410(18) 0.0304(17) 0.0020(15) -0.0045(15) C1A 0.0274(18) 0.0279(18) 0.0264(17) 0.0106(14) 0.0085(14) 0.0059(14) C2A 0.0314(19) 0.0284(18) 0.0319(19) 0.0150(15) 0.0125(15) 0.0050(15) C11A 0.0300(19) 0.038(2) 0.0322(19) 0.0187(17) 0.0002(15) 0.0019(16) C12A 0.043(2) 0.038(2) 0.0281(19) 0.0132(17) 0.0074(16) 0.0001(17) C13A 0.041(2) 0.037(2) 0.036(2) 0.0116(18) 0.0089(18) 0.0078(18) C14A 0.061(3) 0.053(3) 0.049(3) 0.006(2) 0.019(2) 0.013(2) C21A 0.040(2) 0.046(2) 0.038(2) 0.0269(19) 0.0070(18) -0.0018(18) C22A 0.039(2) 0.041(2) 0.042(2) 0.0226(19) 0.0087(18) 0.0022(17) C23A 0.052(3) 0.056(3) 0.050(3) 0.035(2) 0.005(2) 0.000(2) C24A 0.053(3) 0.075(4) 0.093(4) 0.063(3) 0.017(3) 0.012(3) O1B 0.085(2) 0.0528(18) 0.0439(16) 0.0353(15) 0.0399(17) 0.0387(17) O2B 0.0481(18) 0.0331(15) 0.0298(15) 0.0198(12) 0.0186(13) 0.0109(13) N1B 0.0414(18) 0.0331(17) 0.0271(15) 0.0172(13) 0.0146(13) 0.0122(13) N2B 0.0285(15) 0.0291(15) 0.0268(15) 0.0154(13) 0.0113(12) 0.0050(12) N3B 0.061(2) 0.0413(19) 0.046(2) 0.0293(17) 0.0313(18) 0.0262(17) N4B 0.053(2) 0.0339(17) 0.0320(17) 0.0160(14) 0.0187(15) 0.0177(15) C1B 0.0320(19) 0.0316(19) 0.0277(18) 0.0143(15) 0.0103(15) 0.0077(15) C2B 0.0257(17) 0.0277(18) 0.0293(18) 0.0135(15) 0.0087(14) 0.0061(14) C11B 0.082(3) 0.046(3) 0.057(3) 0.033(2) 0.049(3) 0.027(2) C12B 0.057(3) 0.056(3) 0.040(2) 0.025(2) 0.023(2) 0.013(2) C13B 0.071(3) 0.054(3) 0.046(3) 0.023(2) 0.029(2) 0.021(2) C14B 0.116(5) 0.061(4) 0.078(4) 0.033(3) 0.061(4) 0.028(3) C21B 0.038(2) 0.0314(19) 0.039(2) 0.0223(17) 0.0145(17) 0.0105(16) C22B 0.039(2) 0.033(2) 0.035(2) 0.0136(17) 0.0172(17) 0.0098(16) C23B 0.048(2) 0.048(2) 0.034(2) 0.0201(19) 0.0158(18) 0.0154(19) C24B 0.044(3) 0.102(4) 0.045(3) 0.033(3) 0.008(2) 0.016(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2566(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1A 1.857(4) . . yes Ni1 N2A 1.874(3) . . yes Ni1 N1A 1.857(4) . 2_777 yes Ni1 N2A 1.874(3) . 2_777 yes Ni2 N1B 1.865(3) . 2_665 yes Ni2 N2B 1.866(4) . 2_665 yes Ni2 N1B 1.865(3) . . yes Ni2 N2B 1.866(4) . . yes O1A N1A 1.390(5) . . yes O2A N2A 1.361(4) . . yes O1A H7 0.8300 . . no O1B N1B 1.387(5) . . yes O2B N2B 1.378(4) . . yes O1B H4 0.8200 . . no N1A C2A 1.291(5) . . yes N2A C1A 1.305(5) . . yes N3A C1A 1.351(5) . . yes N3A C11A 1.472(5) . . yes N4A C21A 1.476(6) . . yes N4A C2A 1.341(6) . . yes N3A H5 0.8500 . . no N4A H4AA 0.8600 . . no N1B C1B 1.292(6) . . yes N2B C2B 1.305(5) . . yes N3B C1B 1.357(5) . . yes N3B C11B 1.480(7) . . yes N4B C2B 1.346(5) . . yes N4B C21B 1.464(6) . . yes N3B H3BA 0.8600 . . no N4B H4BA 0.8400 . . no C1A C2A 1.495(5) . . no C11A C12A 1.509(6) . . no C12A C13A 1.519(7) . . no C13A C14A 1.523(7) . . no C21A C22A 1.514(7) . . no C22A C23A 1.530(7) . . no C23A C24A 1.526(9) . . no C11A H112 0.9500 . . no C11A H11A 0.9800 . . no C12A H121 0.9700 . . no C12A H122 0.9700 . . no C13A H132 0.9700 . . no C13A H131 0.9700 . . no C14A H143 0.9700 . . no C14A H141 0.9600 . . no C14A H142 0.9700 . . no C21A H212 0.9600 . . no C21A H21A 0.9600 . . no C22A H222 0.9700 . . no C22A H221 0.9700 . . no C23A H232 0.9700 . . no C23A H231 0.9700 . . no C24A H242 0.9700 . . no C24A H243 0.9700 . . no C24A H241 0.9600 . . no C1B C2B 1.501(5) . 2_665 no C11B C12B 1.500(8) . . no C12B C13B 1.485(8) . . no C13B C14B 1.515(9) . . no C21B C22B 1.511(6) . . no C22B C23B 1.517(7) . . no C23B C24B 1.517(7) . . no C11B H271 0.9800 . . no C11B H272 0.9700 . . no C12B H14D 0.9900 . . no C12B H282 0.9800 . . no C13B H291 0.9700 . . no C13B H292 0.9800 . . no C14B H301 0.9700 . . no C14B H302 0.9700 . . no C14B H303 0.9700 . . no C21B H21C 0.9600 . . no C21B H311 0.9700 . . no C22B H22C 0.9700 . . no C22B H322 0.9700 . . no C23B H331 0.9700 . . no C23B H332 0.9800 . . no C24B H24E 0.9600 . . no C24B H341 0.9600 . . no C24B H343 0.9700 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ni1 N2A 82.18(15) . . . yes N1A Ni1 N1A 180.00 . . 2_777 yes N1A Ni1 N2A 97.82(15) . . 2_777 yes N1A Ni1 N2A 97.82(15) 2_777 . . yes N2A Ni1 N2A 180.00 . . 2_777 yes N1A Ni1 N2A 82.18(15) 2_777 . 2_777 yes N1B Ni2 N2B 81.59(15) 2_665 . . yes N2B Ni2 N2B 180.00 . . 2_665 yes N1B Ni2 N2B 98.41(15) 2_665 . 2_665 yes N1B Ni2 N2B 81.59(15) . . 2_665 yes N1B Ni2 N2B 98.41(15) . . . yes N1B Ni2 N1B 180.00 . . 2_665 yes N1A O1A H7 102.00 . . . no N1B O1B H4 100.00 . . . no O1A N1A C2A 118.2(3) . . . yes Ni1 N1A C2A 118.1(3) . . . yes Ni1 N1A O1A 123.7(3) . . . yes Ni1 N2A C1A 116.4(3) . . . yes Ni1 N2A O2A 124.3(3) . . . yes O2A N2A C1A 119.1(3) . . . yes C1A N3A C11A 124.7(3) . . . yes C2A N4A C21A 128.1(3) . . . yes C11A N3A H5 117.00 . . . no C1A N3A H5 118.00 . . . no C21A N4A H4AA 116.00 . . . no C2A N4A H4AA 116.00 . . . no O1B N1B C1B 118.6(3) . . . yes Ni2 N1B C1B 117.9(3) . . . yes Ni2 N1B O1B 123.5(3) . . . yes Ni2 N2B C2B 118.0(3) . . . yes Ni2 N2B O2B 122.0(3) . . . yes O2B N2B C2B 119.9(3) . . . yes C1B N3B C11B 125.8(4) . . . yes C2B N4B C21B 127.7(3) . . . yes C11B N3B H3BA 117.00 . . . no C1B N3B H3BA 117.00 . . . no C21B N4B H4BA 115.00 . . . no C2B N4B H4BA 117.00 . . . no N3A C1A C2A 120.8(3) . . . yes N2A C1A N3A 127.0(3) . . . yes N2A C1A C2A 112.0(3) . . . yes N1A C2A N4A 129.3(3) . . . yes N1A C2A C1A 111.3(3) . . . yes N4A C2A C1A 119.5(3) . . . yes N3A C11A C12A 113.5(4) . . . yes C11A C12A C13A 114.9(4) . . . no C12A C13A C14A 112.5(4) . . . no N4A C21A C22A 113.7(4) . . . yes C21A C22A C23A 111.6(4) . . . no C22A C23A C24A 111.8(4) . . . no H11A C11A H112 109.00 . . . no C12A C11A H11A 110.00 . . . no C12A C11A H112 108.00 . . . no N3A C11A H11A 109.00 . . . no N3A C11A H112 107.00 . . . no H121 C12A H122 108.00 . . . no C13A C12A H122 109.00 . . . no C13A C12A H121 109.00 . . . no C11A C12A H121 108.00 . . . no C11A C12A H122 108.00 . . . no C12A C13A H131 109.00 . . . no C12A C13A H132 109.00 . . . no C14A C13A H131 110.00 . . . no C14A C13A H132 109.00 . . . no H131 C13A H132 108.00 . . . no C13A C14A H143 110.00 . . . no H141 C14A H143 109.00 . . . no H142 C14A H143 110.00 . . . no H141 C14A H142 109.00 . . . no C13A C14A H141 110.00 . . . no C13A C14A H142 110.00 . . . no H21A C21A H212 110.00 . . . no C22A C21A H212 109.00 . . . no N4A C21A H21A 107.00 . . . no N4A C21A H212 109.00 . . . no C22A C21A H21A 108.00 . . . no C21A C22A H222 109.00 . . . no C23A C22A H221 109.00 . . . no C23A C22A H222 109.00 . . . no C21A C22A H221 109.00 . . . no H221 C22A H222 109.00 . . . no H231 C23A H232 109.00 . . . no C22A C23A H232 109.00 . . . no C24A C23A H232 110.00 . . . no C22A C23A H231 108.00 . . . no C24A C23A H231 109.00 . . . no C23A C24A H241 110.00 . . . no H241 C24A H243 110.00 . . . no H242 C24A H243 110.00 . . . no C23A C24A H242 109.00 . . . no C23A C24A H243 108.00 . . . no H241 C24A H242 109.00 . . . no N3B C1B C2B 120.7(4) . . 2_665 yes N1B C1B C2B 111.7(3) . . 2_665 yes N1B C1B N3B 127.7(4) . . . yes N2B C2B C1B 110.6(3) . . 2_665 yes N2B C2B N4B 129.3(3) . . . yes N4B C2B C1B 119.9(3) . . 2_665 yes N3B C11B C12B 111.7(5) . . . yes C11B C12B C13B 116.6(5) . . . no C12B C13B C14B 114.8(5) . . . no N4B C21B C22B 113.4(4) . . . yes C21B C22B C23B 112.4(4) . . . no C22B C23B C24B 113.2(4) . . . no N3B C11B H271 108.00 . . . no N3B C11B H272 109.00 . . . no C12B C11B H271 108.00 . . . no C12B C11B H272 110.00 . . . no H271 C11B H272 109.00 . . . no C11B C12B H14D 108.00 . . . no C11B C12B H282 107.00 . . . no C13B C12B H14D 107.00 . . . no C13B C12B H282 109.00 . . . no H14D C12B H282 109.00 . . . no C12B C13B H291 109.00 . . . no C12B C13B H292 108.00 . . . no C14B C13B H291 108.00 . . . no C14B C13B H292 107.00 . . . no H291 C13B H292 110.00 . . . no C13B C14B H301 111.00 . . . no C13B C14B H302 109.00 . . . no C13B C14B H303 109.00 . . . no H301 C14B H302 110.00 . . . no H301 C14B H303 110.00 . . . no H302 C14B H303 109.00 . . . no N4B C21B H21C 109.00 . . . no N4B C21B H311 107.00 . . . no C22B C21B H21C 110.00 . . . no C22B C21B H311 108.00 . . . no H21C C21B H311 109.00 . . . no C21B C22B H22C 109.00 . . . no C21B C22B H322 109.00 . . . no C23B C22B H22C 108.00 . . . no C23B C22B H322 110.00 . . . no H22C C22B H322 109.00 . . . no C22B C23B H331 109.00 . . . no C22B C23B H332 108.00 . . . no C24B C23B H331 110.00 . . . no C24B C23B H332 109.00 . . . no H331 C23B H332 109.00 . . . no C23B C24B H24E 110.00 . . . no C23B C24B H341 111.00 . . . no C23B C24B H343 109.00 . . . no H24E C24B H341 109.00 . . . no H24E C24B H343 109.00 . . . no H341 C24B H343 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2A Ni1 N1A O1A 178.9(3) . . . . no N2A Ni1 N1A C2A 2.1(3) . . . . no N2A Ni1 N1A O1A -1.1(3) 2_777 . . . no N2A Ni1 N1A C2A -177.9(3) 2_777 . . . no N1A Ni1 N2A O2A 172.0(3) . . . . no N1A Ni1 N2A C1A -2.2(3) . . . . no N1A Ni1 N2A O2A -8.0(3) 2_777 . . . no N1A Ni1 N2A C1A 177.8(3) 2_777 . . . no N2B Ni2 N1B O1B -2.1(3) . . . . no N2B Ni2 N1B C1B 176.0(3) . . . . no N2B Ni2 N1B O1B 178.0(3) 2_665 . . . no N2B Ni2 N1B C1B -4.0(3) 2_665 . . . no N1B Ni2 N2B O2B -4.6(3) . . . . no N1B Ni2 N2B C2B 178.2(3) . . . . no N1B Ni2 N2B O2B 175.4(3) 2_665 . . . no N1B Ni2 N2B C2B -1.9(3) 2_665 . . . no Ni1 N1A C2A C1A -1.6(4) . . . . no O1A N1A C2A N4A 2.8(6) . . . . no O1A N1A C2A C1A -178.5(3) . . . . no Ni1 N1A C2A N4A 179.7(3) . . . . no Ni1 N2A C1A C2A 1.9(4) . . . . no O2A N2A C1A N3A 2.5(5) . . . . no Ni1 N2A C1A N3A 177.0(3) . . . . no O2A N2A C1A C2A -172.6(3) . . . . no C11A N3A C1A N2A 36.2(6) . . . . no C11A N3A C1A C2A -149.1(4) . . . . no C1A N3A C11A C12A 51.1(6) . . . . no C21A N4A C2A N1A 9.5(7) . . . . no C21A N4A C2A C1A -169.1(4) . . . . no C2A N4A C21A C22A -91.4(5) . . . . no Ni2 N1B C1B N3B -174.3(3) . . . . no Ni2 N1B C1B C2B 5.0(4) . . . 2_665 no O1B N1B C1B N3B 3.9(6) . . . . no O1B N1B C1B C2B -176.8(3) . . . 2_665 no Ni2 N2B C2B N4B 175.3(3) . . . . no Ni2 N2B C2B C1B -0.3(4) . . . 2_665 no O2B N2B C2B N4B -2.0(6) . . . . no O2B N2B C2B C1B -177.6(3) . . . 2_665 no C11B N3B C1B C2B -165.0(4) . . . 2_665 no C11B N3B C1B N1B 14.3(7) . . . . no C1B N3B C11B C12B 176.6(4) . . . . no C2B N4B C21B C22B 78.0(5) . . . . no C21B N4B C2B N2B 17.8(6) . . . . no C21B N4B C2B C1B -167.0(4) . . . 2_665 no N2A C1A C2A N1A -0.2(4) . . . . no N2A C1A C2A N4A 178.6(3) . . . . no N3A C1A C2A N1A -175.7(3) . . . . no N3A C1A C2A N4A 3.2(5) . . . . no N3A C11A C12A C13A 53.4(5) . . . . no C11A C12A C13A C14A 174.7(4) . . . . no N4A C21A C22A C23A -176.1(4) . . . . no C21A C22A C23A C24A -176.2(4) . . . . no N1B C1B C2B N2B -3.3(4) . . 2_665 2_665 no N1B C1B C2B N4B 172.7(3) . . 2_665 2_665 no N3B C1B C2B N2B 176.0(4) . . 2_665 2_665 no N3B C1B C2B N4B -8.0(5) . . 2_665 2_665 no N3B C11B C12B C13B 63.8(6) . . . . no C11B C12B C13B C14B 178.4(5) . . . . no N4B C21B C22B C23B 170.3(4) . . . . no C21B C22B C23B C24B -176.0(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni1 C22B 3.747(5) . 1_656 no Ni1 C23B 4.147(4) . 1_656 no Ni1 C23B 4.147(4) . 2_676 no Ni1 C22B 3.747(5) . 2_676 no Ni2 C21A 3.540(5) . 1_554 no Ni2 C22A 3.999(5) . 1_554 no Ni2 C22A 3.999(5) . 2_666 no Ni2 C21A 3.540(5) . 2_666 no Ni2 N4A 3.843(4) . 2_666 no Ni2 N4A 3.843(4) . 1_554 no Ni1 H24E 3.5000 . 1_656 no Ni1 H22C 2.8500 . 1_656 no Ni1 H22C 2.8500 . 2_676 no Ni1 H24E 3.5000 . 2_676 no Ni2 H221 3.6100 . 1_554 no Ni2 H4AA 3.3400 . 1_554 no Ni2 H21A 2.7200 . 1_554 no Ni2 H4AA 3.3400 . 2_666 no Ni2 H21A 2.7200 . 2_666 no Ni2 H221 3.6100 . 2_666 no O1A N4A 2.803(5) . . no O1A C21A 2.790(6) . . no O1A C22A 3.151(6) . . no O1A O2A 2.482(4) . 2_777 no O1A N2A 2.967(5) . 2_777 no O1B C11B 2.729(7) . . no O1B N3B 2.790(5) . . no O1B N2B 2.984(5) . . no O1B O2B 2.444(5) . . no O2A N3B 2.986(5) . 1_566 no O2A C11A 2.858(5) . . no O2A N3A 2.782(4) . . no O2A N4B 3.004(4) . 2_676 no O2A C12A 3.234(5) . . no O2A N1A 2.986(4) . 2_777 no O2A O1A 2.482(4) . 2_777 no O2B N4B 2.849(4) . . no O2B C22B 3.407(6) . . no O2B N4A 3.126(5) . 1_554 no O2B N3A 2.842(5) . 1_554 no O2B O1B 2.444(5) . . no O2B C21B 2.859(6) . . no O2B N1B 2.951(5) . . no O1A H14D 2.4800 . 2_766 no O1A H222 2.6000 . . no O1A H212 2.3200 . . no O1B H122 2.7600 . 2_665 no O1B H4AA 2.8900 . 1_554 no O1B H271 2.3700 . . no O1B H272 2.6500 . . no O2A H4BA 2.2600 . 2_676 no O2A H7 1.6600 . 2_777 no O2A H14D 2.8500 . 1_566 no O2A H3BA 2.1800 . 1_566 no O2A H11A 2.4200 . . no O2A H121 2.6500 . . no O2A H291 2.8200 . 1_566 no O2B H143 2.8400 . 2_665 no O2B H4AA 2.3300 . 1_554 no O2B H4 1.6300 . . no O2B H5 2.0500 . 1_554 no O2B H21C 2.3000 . . no N1A C1A 2.302(5) . . no N1A N2A 2.452(5) . . no N1A O2A 2.986(4) . 2_777 no N1A N2A 2.812(5) . 2_777 no N1B C2B 2.314(5) . 2_665 no N1B N2B 2.825(5) . . no N1B N2B 2.438(5) . 2_665 no N1B O2B 2.951(5) . . no N2A C2A 2.324(5) . . no N2A C12A 3.389(5) . . no N2A N1A 2.452(5) . . no N2A O1A 2.967(5) . 2_777 no N2A N1A 2.812(5) . 2_777 no N2B N1B 2.438(5) . 2_665 no N2B O1B 2.984(5) . . no N2B N1B 2.825(5) . . no N2B C1B 2.309(5) . 2_665 no N3A N4A 2.846(5) . . no N3A O2B 2.842(5) . 1_556 no N3A O2A 2.782(4) . . no N3B O2A 2.986(5) . 1_544 no N3B O1B 2.790(5) . . no N3B N4B 2.869(5) . 2_665 no N4A O2B 3.126(5) . 1_556 no N4A N3A 2.846(5) . . no N4A Ni2 3.843(4) . 2_666 no N4A O1A 2.803(5) . . no N4A Ni2 3.843(4) . 1_556 no N4B O2A 3.004(4) . 2_676 no N4B O2B 2.849(4) . . no N4B N3B 2.869(5) . 2_665 no N1A H212 2.8700 . . no N2A H22C 2.9400 . 2_676 no N2A H4BA 2.7900 . 2_676 no N2A H121 2.8600 . . no N2A H7 2.3100 . 2_777 no N2B H4 2.3100 . . no N2B H21C 2.9000 . . no N2B H4AA 2.7400 . 1_554 no N3A H311 2.7700 . 2_676 no N3A H21C 2.8000 . 1_556 no N3A H131 2.7100 . . no N3A H4AA 2.4900 . . no N3B H291 2.7600 . . no N3B H4BA 2.5300 . 2_665 no N4A H5 2.5900 . . no N4B H3BA 2.5300 . 2_665 no C1A C13A 3.455(5) . . no C1A C21B 3.418(6) . 2_676 no C11A O2A 2.858(5) . . no C11B O1B 2.729(7) . . no C12A N2A 3.389(5) . . no C12A O2A 3.234(5) . . no C13A C1A 3.455(5) . . no C21A O1A 2.790(6) . . no C21A Ni2 3.540(5) . 2_666 no C21A Ni2 3.540(5) . 1_556 no C21B C1A 3.418(6) . 2_676 no C21B O2B 2.859(6) . . no C22A Ni2 3.999(5) . 2_666 no C22A Ni2 3.999(5) . 1_556 no C22A O1A 3.151(6) . . no C22B Ni1 3.747(5) . 1_454 no C22B O2B 3.407(6) . . no C22B Ni1 3.747(5) . 2_676 no C23B Ni1 4.147(4) . 1_454 no C23B Ni1 4.147(4) . 2_676 no C1A H4BA 3.0400 . 2_676 no C1A H131 2.9000 . . no C1A H121 2.8700 . . no C1A H311 2.6900 . 2_676 no C1B H221 3.0100 . 1_554 no C2A H331 2.9800 . 2_676 no C13A H132 3.0600 . 2_666 no C13B H3BA 2.8400 . . no C21B H5 3.1000 . 1_554 no H3BA H291 2.3200 . . no H3BA N4B 2.5300 . 2_665 no H3BA H4BA 1.9700 . 2_665 no H3BA H14D 2.4700 . . no H3BA O2A 2.1800 . 1_544 no H3BA C13B 2.8400 . . no H4BA O2A 2.2600 . 2_676 no H4BA H3BA 1.9700 . 2_665 no H4BA N2A 2.7900 . 2_676 no H4BA N3B 2.5300 . 2_665 no H4BA C1A 3.0400 . 2_676 no H4AA O1B 2.8900 . 1_556 no H4AA O2B 2.3300 . 1_556 no H4AA N2B 2.7400 . 1_556 no H4AA Ni2 3.3400 . 1_556 no H4AA Ni2 3.3400 . 2_666 no H4AA N3A 2.4900 . . no H4AA H4 2.5400 . 1_556 no H4AA H5 2.0800 . . no H4 N2B 2.3100 . . no H4 H4AA 2.5400 . 1_554 no H4 O2B 1.6300 . . no H5 C21B 3.1000 . 1_556 no H5 O2B 2.0500 . 1_556 no H5 N4A 2.5900 . . no H5 H4AA 2.0800 . . no H5 H21C 2.1700 . 1_556 no H7 O2A 1.6600 . 2_777 no H7 N2A 2.3100 . 2_777 no H7 H14D 2.2500 . 2_766 no H11A H291 2.4800 . 1_566 no H11A O2A 2.4200 . . no H14D O2A 2.8500 . 1_544 no H14D O1A 2.4800 . 2_766 no H14D H3BA 2.4700 . . no H14D H302 2.5400 . . no H14D H7 2.2500 . 2_766 no H21A Ni2 2.7200 . 1_556 no H21A Ni2 2.7200 . 2_666 no H21A H231 2.5100 . . no H21C N2B 2.9000 . . no H21C O2B 2.3000 . . no H21C N3A 2.8000 . 1_554 no H21C H5 2.1700 . 1_554 no H22C Ni1 2.8500 . 1_454 no H22C N2A 2.9400 . 2_676 no H22C H24E 2.5100 . . no H22C Ni1 2.8500 . 2_676 no H24E Ni1 3.5000 . 1_454 no H24E H22C 2.5100 . . no H24E Ni1 3.5000 . 2_676 no H112 H132 2.5800 . . no H121 H142 2.5900 . . no H121 O2A 2.6500 . . no H121 N2A 2.8600 . . no H121 C1A 2.8700 . . no H122 H143 2.5100 . . no H122 O1B 2.7600 . 2_665 no H131 N3A 2.7100 . . no H131 C1A 2.9000 . . no H132 H132 2.3400 . 2_666 no H132 H112 2.5800 . . no H132 C13A 3.0600 . 2_666 no H142 H121 2.5900 . . no H143 H122 2.5100 . . no H143 O2B 2.8400 . 2_665 no H212 O1A 2.3200 . . no H212 H303 2.5200 . 1_567 no H212 N1A 2.8700 . . no H212 H232 2.5100 . . no H221 Ni2 3.6100 . 1_556 no H221 Ni2 3.6100 . 2_666 no H221 C1B 3.0100 . 1_556 no H221 H242 2.5400 . . no H222 O1A 2.6000 . . no H222 H243 2.5100 . . no H231 H21A 2.5100 . . no H232 H212 2.5100 . . no H242 H221 2.5400 . . no H243 H222 2.5100 . . no H271 O1B 2.3700 . . no H271 H292 2.5300 . . no H272 O1B 2.6500 . . no H282 H303 2.5100 . . no H282 H332 2.4700 . 2_664 no H282 H341 2.5800 . 2_664 no H291 O2A 2.8200 . 1_544 no H291 N3B 2.7600 . . no H291 H3BA 2.3200 . . no H291 H11A 2.4800 . 1_544 no H292 H271 2.5300 . . no H302 H14D 2.5400 . . no H303 H212 2.5200 . 1_543 no H303 H282 2.5100 . . no H311 H331 2.4100 . . no H311 N3A 2.7700 . 2_676 no H311 C1A 2.6900 . 2_676 no H322 H343 2.6000 . . no H331 H311 2.4100 . . no H331 C2A 2.9800 . 2_676 no H332 H282 2.4700 . 2_664 no H341 H282 2.5800 . 2_664 no H343 H322 2.6000 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # N3B H3BA O2A 0.8600 2.1800 2.986(5) 156.00 1_544 yes N4B H4BA O2A 0.8400 2.2600 3.004(4) 148.00 2_676 yes N4A H4AA O2B 0.8600 2.3300 3.126(5) 156.00 1_556 yes O1B H4 O2B 0.8200 1.6300 2.444(5) 170.00 . yes N3A H5 O2B 0.8500 2.0500 2.842(5) 154.00 1_556 yes O1A H7 O2A 0.8300 1.6600 2.482(4) 171.00 2_777 yes C11A H11A O2A 0.9800 2.4200 2.858(5) 106.00 . yes C12B H14D O1A 0.9900 2.4800 3.427(6) 162.00 2_766 yes C21B H21C O2B 0.9600 2.3000 2.859(6) 116.00 . yes C21A H212 O1A 0.9600 2.3200 2.790(6) 109.00 . yes C11B H271 O1B 0.9800 2.3700 2.729(7) 101.00 . yes # Attachment 'VAC4Pd4.cif' data_VAC4Pd4 _database_code_depnum_ccdc_archive 'CCDC 648645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H42 N8 O4 Pd1' _chemical_formula_weight 565.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.7406(6) _cell_length_b 15.4165(10) _cell_length_c 16.4463(11) _cell_angle_alpha 114.2040(10) _cell_angle_beta 101.9000(10) _cell_angle_gamma 98.5760(10) _cell_volume 2127.3(2) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13177 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.83 _reflns_number_total 9622 _reflns_number_gt 5073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9622 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.06161(15) Uani 1 2 d S . . O1A O -0.2225(3) 0.0326(2) 0.0980(2) 0.0857(9) Uani 1 1 d . . . H1AA H -0.264(5) -0.021(4) 0.038(3) 0.103(17) Uiso 1 1 d . . . O2A O 0.2923(3) 0.12417(19) 0.06273(19) 0.0763(8) Uani 1 1 d . . . N1A N -0.0799(4) 0.0682(2) 0.1019(2) 0.0694(9) Uani 1 1 d . . . N3A N -0.0280(6) 0.2033(4) 0.2502(3) 0.0987(16) Uani 1 1 d . . . H3AA H 0.030(5) 0.240(4) 0.277(4) 0.08(2) Uiso 1 1 d . . . N2A N 0.1675(3) 0.1129(2) 0.0872(2) 0.0658(8) Uani 1 1 d . . . N4A N 0.2532(5) 0.2530(4) 0.2350(3) 0.1060(17) Uani 1 1 d . . . H4AA H 0.221(5) 0.287(3) 0.267(3) 0.084(18) Uiso 1 1 d . . . C1A C 0.0029(5) 0.1468(3) 0.1733(3) 0.0691(11) Uani 1 1 d . . . C11A C -0.1552(7) 0.1881(5) 0.2792(4) 0.152(3) Uani 1 1 d . . . H11A H -0.1958 0.2440 0.2889 0.182 Uiso 1 1 calc R . . H11B H -0.2267 0.1303 0.2285 0.182 Uiso 1 1 calc R . . C12A C -0.1346(16) 0.1757(14) 0.3598(12) 0.335(11) Uani 1 1 d . . . H12A H -0.2301 0.1795 0.3672 0.402 Uiso 1 1 calc R . . H12B H -0.1433 0.1055 0.3300 0.402 Uiso 1 1 calc R . . C13A C -0.085(2) 0.1887(11) 0.4253(8) 0.378(14) Uani 1 1 d . . . H13A H -0.0505 0.2600 0.4577 0.454 Uiso 1 1 calc R . . H13B H 0.0008 0.1655 0.4191 0.454 Uiso 1 1 calc R . . C14A C -0.1192(16) 0.1662(14) 0.4959(12) 0.373(11) Uani 1 1 d . . . H14A H -0.1095 0.2262 0.5500 0.560 Uiso 1 1 calc R . . H14B H -0.0536 0.1312 0.5122 0.560 Uiso 1 1 calc R . . H14C H -0.2172 0.1259 0.4729 0.560 Uiso 1 1 calc R . . C2A C 0.1510(5) 0.1740(3) 0.1645(3) 0.0700(11) Uani 1 1 d . . . C21A C 0.4076(6) 0.2768(5) 0.2539(4) 0.135(2) Uani 1 1 d . . . H21A H 0.4354 0.3170 0.2245 0.161 Uiso 1 1 calc R . . H21B H 0.4375 0.2165 0.2269 0.161 Uiso 1 1 calc R . . C22A C 0.4827(8) 0.3297(7) 0.3538(6) 0.188(4) Uani 1 1 d . . . H22A H 0.5832 0.3566 0.3603 0.226 Uiso 1 1 calc R . . H22B H 0.4424 0.3855 0.3791 0.226 Uiso 1 1 calc R . . C23A C 0.4852(14) 0.2863(9) 0.4112(8) 0.227(5) Uani 1 1 d . . . H23A H 0.5101 0.2243 0.3827 0.273 Uiso 1 1 calc R . . H23B H 0.3884 0.2715 0.4171 0.273 Uiso 1 1 calc R . . C24A C 0.5917(10) 0.3488(8) 0.5080(7) 0.221(4) Uani 1 1 d . . . H24A H 0.5928 0.3122 0.5432 0.331 Uiso 1 1 calc R . . H24B H 0.5626 0.4076 0.5392 0.331 Uiso 1 1 calc R . . H24C H 0.6872 0.3662 0.5028 0.331 Uiso 1 1 calc R . . Pd2 Pd 1.0000 0.5000 0.5000 0.06443(15) Uani 1 2 d S . . O1B O 0.7445(4) 0.5742(3) 0.4654(3) 0.0944(11) Uani 1 1 d . . . H1BA H 0.753(6) 0.578(4) 0.514(4) 0.12(2) Uiso 1 1 d . . . O2B O 1.1465(3) 0.4033(2) 0.36540(18) 0.0807(8) Uani 1 1 d . . . N1B N 0.8440(4) 0.5287(2) 0.4269(2) 0.0719(9) Uani 1 1 d . . . N3B N 0.7419(4) 0.5184(3) 0.2780(3) 0.0934(13) Uani 1 1 d . . . H3BA H 0.751(5) 0.496(4) 0.221(4) 0.078(2) Uiso 1 1 d P . . N2B N 1.0384(4) 0.4485(2) 0.3782(2) 0.0683(8) Uani 1 1 d . . . N4B N 0.9619(5) 0.4281(3) 0.2237(3) 0.0897(13) Uani 1 1 d . . . H4BA H 0.895(4) 0.425(3) 0.188(3) 0.061(14) Uiso 1 1 d . . . C1B C 0.8360(4) 0.5050(3) 0.3405(3) 0.0686(10) Uani 1 1 d . . . C11B C 0.6314(7) 0.5730(6) 0.2928(4) 0.140(3) Uani 1 1 d . . . H11C H 0.5540 0.5465 0.2346 0.168 Uiso 1 1 calc R . . H11D H 0.5899 0.5634 0.3382 0.168 Uiso 1 1 calc R . . C12B C 0.6887(16) 0.6785(8) 0.3254(9) 0.278(8) Uani 1 1 d . . . H12C H 0.6877 0.7068 0.3899 0.334 Uiso 1 1 calc R . . H12D H 0.7904 0.6846 0.3286 0.334 Uiso 1 1 calc R . . C13B C 0.6629(19) 0.7345(14) 0.3038(14) 0.383(13) Uani 1 1 d . . . H13C H 0.5575 0.7165 0.2834 0.459 Uiso 1 1 calc R . . H13D H 0.6913 0.7169 0.2471 0.459 Uiso 1 1 calc R . . C14B C 0.6971(18) 0.8311(13) 0.3430(15) 0.376(12) Uani 1 1 d . . . H14D H 0.6643 0.8523 0.2968 0.565 Uiso 1 1 calc R . . H14E H 0.8006 0.8563 0.3695 0.565 Uiso 1 1 calc R . . H14F H 0.6513 0.8552 0.3912 0.565 Uiso 1 1 calc R . . C2B C 0.9526(4) 0.4580(3) 0.3115(3) 0.0686(10) Uani 1 1 d . . . C21B C 1.0907(8) 0.4321(6) 0.1965(5) 0.137(2) Uani 1 1 d . . . H21C H 1.1647 0.4256 0.2415 0.164 Uiso 1 1 calc R . . H21D H 1.0716 0.3748 0.1369 0.164 Uiso 1 1 calc R . . C22B C 1.1480(15) 0.5129(12) 0.1880(14) 0.348(11) Uani 1 1 d . . . H22C H 1.2460 0.5051 0.1933 0.418 Uiso 1 1 calc R . . H22D H 1.1040 0.4864 0.1212 0.418 Uiso 1 1 calc R . . C23B C 1.1748(19) 0.5947(9) 0.2053(11) 0.328(11) Uani 1 1 d . . . H23C H 1.2432 0.6262 0.2675 0.394 Uiso 1 1 calc R . . H23D H 1.0856 0.6127 0.2137 0.394 Uiso 1 1 calc R . . C24B C 1.2254(12) 0.6492(11) 0.1639(11) 0.289(7) Uani 1 1 d . . . H24D H 1.2320 0.7174 0.2014 0.434 Uiso 1 1 calc R . . H24E H 1.1596 0.6265 0.1029 0.434 Uiso 1 1 calc R . . H24F H 1.3197 0.6417 0.1588 0.434 Uiso 1 1 calc R . . Pd3 Pd 0.5000 0.5000 0.0000 0.06431(15) Uani 1 2 d S . . O1C O 0.1863(3) 0.4049(3) -0.0649(2) 0.0940(11) Uani 1 1 d . . . H1CA H 0.203(4) 0.451(3) -0.070(2) 0.048(12) Uiso 1 1 d . . . O2C O 0.7282(4) 0.4356(3) 0.0851(3) 0.0800(12) Uani 1 1 d . . . N1C N 0.3224(3) 0.4010(3) -0.0253(2) 0.0729(9) Uani 1 1 d . . . N3C N 0.2346(4) 0.2580(3) -0.0112(3) 0.0904(13) Uani 1 1 d . . . H3CA H 0.268(5) 0.219(3) -0.002(3) 0.079(17) Uiso 1 1 d . . . N2C N 0.5836(4) 0.4136(3) 0.0453(2) 0.0686(9) Uani 1 1 d . . . N4C N 0.5305(5) 0.2699(3) 0.0656(3) 0.0850(11) Uani 1 1 d . . . H4CA H 0.452(4) 0.234(3) 0.075(3) 0.071(12) Uiso 1 1 d . . . C1C C 0.3375(4) 0.3311(3) -0.0030(3) 0.0678(10) Uani 1 1 d . . . C11C C 0.0810(5) 0.2238(5) -0.0657(5) 0.117(2) Uani 1 1 d . . . H11E H 0.0447 0.2804 -0.0611 0.141 Uiso 1 1 calc R . . H11F H 0.0262 0.1901 -0.0393 0.141 Uiso 1 1 calc R . . C12C C 0.0557(9) 0.1539(7) -0.1690(5) 0.185(3) Uani 1 1 d . . . H12E H 0.0865 0.1931 -0.1987 0.222 Uiso 1 1 calc R . . H12F H 0.1186 0.1101 -0.1723 0.222 Uiso 1 1 calc R . . C13C C -0.0859(12) 0.0961(8) -0.2213(9) 0.248(5) Uani 1 1 d . . . H13E H -0.1129 0.0525 -0.1950 0.298 Uiso 1 1 calc R . . H13F H -0.1499 0.1396 -0.2126 0.298 Uiso 1 1 calc R . . C14C C -0.1138(13) 0.0395(10) -0.3155(8) 0.301(8) Uani 1 1 d . . . H14G H -0.2150 0.0053 -0.3429 0.452 Uiso 1 1 calc R . . H14H H -0.0565 -0.0074 -0.3261 0.452 Uiso 1 1 calc R . . H14I H -0.0892 0.0811 -0.3435 0.452 Uiso 1 1 calc R . . C2C C 0.4928(4) 0.3368(3) 0.0380(3) 0.0678(10) Uani 1 1 d . . . C21C C 0.6535(6) 0.2270(4) 0.0478(5) 0.118(2) Uani 1 1 d . . . H21E H 0.7357 0.2797 0.0608 0.142 Uiso 1 1 calc R . . H21F H 0.6804 0.2013 0.0920 0.142 Uiso 1 1 calc R . . C22C C 0.6302(15) 0.1514(11) -0.0427(8) 0.273(7) Uani 1 1 d . . . H22E H 0.7058 0.1793 -0.0619 0.328 Uiso 1 1 calc R . . H22F H 0.6656 0.1019 -0.0289 0.328 Uiso 1 1 calc R . . C23C C 0.5386(12) 0.1008(11) -0.1164(9) 0.265(7) Uani 1 1 d . . . H23E H 0.5106 0.1477 -0.1374 0.318 Uiso 1 1 calc R . . H23F H 0.4565 0.0768 -0.0995 0.318 Uiso 1 1 calc R . . C24C C 0.5353(13) 0.0197(8) -0.1991(9) 0.286(7) Uani 1 1 d . . . H24G H 0.4404 -0.0033 -0.2432 0.429 Uiso 1 1 calc R . . H24H H 0.5570 -0.0323 -0.1851 0.429 Uiso 1 1 calc R . . H24I H 0.6062 0.0395 -0.2252 0.429 Uiso 1 1 calc 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 Pd1 0.0726(3) 0.0528(3) 0.0633(3) 0.0255(2) 0.0313(2) 0.0140(2) O1A 0.080(2) 0.078(2) 0.089(2) 0.0223(19) 0.0437(18) 0.0110(17) O2A 0.0752(19) 0.0680(17) 0.0786(19) 0.0236(15) 0.0351(15) 0.0109(14) N1A 0.072(2) 0.063(2) 0.072(2) 0.0246(19) 0.0355(19) 0.0116(18) N3A 0.087(3) 0.099(4) 0.079(3) 0.011(3) 0.037(3) 0.007(3) N2A 0.071(2) 0.0579(19) 0.069(2) 0.0270(17) 0.0296(18) 0.0120(16) N4A 0.086(3) 0.096(3) 0.085(3) -0.005(3) 0.031(3) 0.013(3) C1A 0.076(3) 0.063(3) 0.070(3) 0.026(2) 0.032(2) 0.020(2) C11A 0.135(5) 0.148(5) 0.108(5) -0.009(4) 0.077(4) 0.002(4) C12A 0.326(17) 0.63(3) 0.42(2) 0.45(2) 0.293(18) 0.29(2) C13A 0.71(4) 0.257(13) 0.117(8) 0.077(8) -0.011(14) 0.195(18) C14A 0.274(15) 0.62(3) 0.36(2) 0.37(2) 0.098(15) 0.062(17) C2A 0.080(3) 0.060(3) 0.064(3) 0.021(2) 0.028(2) 0.016(2) C21A 0.087(4) 0.144(5) 0.100(4) 0.000(4) 0.028(3) -0.008(4) C22A 0.110(5) 0.213(9) 0.146(8) 0.010(7) 0.012(5) 0.029(5) C23A 0.298(15) 0.250(13) 0.148(9) 0.093(9) 0.068(10) 0.101(11) C24A 0.190(9) 0.251(11) 0.149(8) 0.049(8) 0.014(7) 0.037(8) Pd2 0.0651(3) 0.0624(3) 0.0476(2) 0.0103(2) 0.0075(2) 0.0229(2) O1B 0.096(2) 0.117(3) 0.068(2) 0.031(2) 0.0210(19) 0.058(2) O2B 0.0772(19) 0.092(2) 0.0595(17) 0.0171(15) 0.0171(15) 0.0415(17) N1B 0.070(2) 0.079(2) 0.057(2) 0.0173(17) 0.0175(17) 0.0354(18) N3B 0.089(3) 0.129(4) 0.065(2) 0.042(2) 0.018(2) 0.049(3) N2B 0.067(2) 0.067(2) 0.0493(18) 0.0087(16) 0.0085(16) 0.0226(17) N4B 0.080(3) 0.125(4) 0.057(3) 0.035(2) 0.016(2) 0.035(3) C1B 0.067(3) 0.071(3) 0.059(3) 0.024(2) 0.009(2) 0.023(2) C11B 0.136(5) 0.196(7) 0.080(4) 0.048(4) 0.009(4) 0.101(5) C12B 0.390(19) 0.150(9) 0.276(15) 0.073(9) 0.046(13) 0.167(12) C13B 0.33(2) 0.29(2) 0.51(3) 0.29(2) -0.069(18) -0.020(17) C14B 0.314(19) 0.304(18) 0.70(4) 0.34(3) 0.23(2) 0.161(16) C2B 0.071(3) 0.061(2) 0.055(3) 0.015(2) 0.008(2) 0.017(2) C21B 0.138(6) 0.222(8) 0.109(4) 0.101(5) 0.067(4) 0.092(6) C22B 0.288(16) 0.35(2) 0.58(3) 0.30(2) 0.29(2) 0.101(15) C23B 0.43(2) 0.184(12) 0.326(18) 0.160(13) -0.039(16) 0.018(13) C24B 0.220(12) 0.321(17) 0.45(2) 0.282(18) 0.105(13) 0.082(11) Pd3 0.0550(3) 0.0774(3) 0.0528(3) 0.0329(2) 0.0049(2) 0.0018(2) O1C 0.059(2) 0.107(3) 0.119(3) 0.071(2) 0.0075(17) 0.0008(18) O2C 0.058(2) 0.099(3) 0.079(2) 0.049(2) 0.0065(18) 0.0041(19) N1C 0.050(2) 0.089(2) 0.076(2) 0.046(2) 0.0059(17) 0.0036(17) N3C 0.067(3) 0.095(3) 0.113(4) 0.061(3) 0.017(2) 0.006(2) N2C 0.057(2) 0.085(2) 0.0583(19) 0.0372(18) 0.0068(16) 0.0070(18) N4C 0.085(3) 0.084(3) 0.097(3) 0.053(2) 0.025(2) 0.018(2) C1C 0.055(2) 0.077(3) 0.065(2) 0.032(2) 0.0133(19) 0.004(2) C11C 0.070(3) 0.141(5) 0.151(6) 0.097(5) 0.013(3) -0.006(3) C12C 0.165(8) 0.198(8) 0.124(6) 0.054(6) -0.020(6) 0.000(6) C13C 0.198(10) 0.196(10) 0.218(12) 0.036(9) -0.036(9) -0.004(8) C14C 0.240(12) 0.290(15) 0.181(10) -0.024(10) -0.036(10) 0.059(11) C2C 0.070(3) 0.074(3) 0.053(2) 0.029(2) 0.014(2) 0.008(2) C21C 0.083(4) 0.097(4) 0.169(6) 0.069(4) 0.010(4) 0.022(3) C22C 0.288(16) 0.369(19) 0.175(10) 0.071(12) 0.103(11) 0.228(16) C23C 0.192(11) 0.294(15) 0.151(9) -0.008(10) 0.015(8) 0.001(10) C24C 0.285(14) 0.212(11) 0.235(13) -0.009(10) 0.116(11) -0.009(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1A 1.964(3) . . yes Pd1 N2A 1.972(3) . . yes Pd1 N1A 1.964(3) . 2_555 yes Pd1 N2A 1.972(3) . 2_555 yes Pd2 N1B 1.958(4) . 2_766 yes Pd2 N2B 1.969(3) . 2_766 yes Pd2 N1B 1.958(4) . . yes Pd2 N2B 1.969(3) . . yes Pd3 N1C 1.972(4) . 2_665 yes Pd3 N2C 1.970(4) . 2_665 yes Pd3 N1C 1.972(4) . . yes Pd3 N2C 1.970(4) . . yes O1A N1A 1.394(5) . . yes O2A N2A 1.366(4) . . yes O1A H1AA 0.94(5) . . no O1B N1B 1.387(6) . . yes O2B N2B 1.352(5) . . yes O1B H1BA 0.76(6) . . no O1C N1C 1.373(5) . . yes O2C N2C 1.350(6) . . yes O1C H1CA 0.75(5) . . no N1A C1A 1.284(6) . . yes N2A C2A 1.295(5) . . yes N3A C1A 1.334(7) . . yes N3A C11A 1.438(9) . . yes N4A C2A 1.350(7) . . yes N4A C21A 1.429(8) . . yes N3A H3AA 0.66(6) . . no N4A H4AA 0.74(5) . . no N1B C1B 1.296(5) . . yes N2B C2B 1.309(6) . . yes N3B C1B 1.335(6) . . yes N3B C11B 1.462(9) . . yes N4B C2B 1.351(6) . . yes N4B C21B 1.417(10) . . yes N3B H3BA 0.84(6) . . no N4B H4BA 0.76(4) . . no N1C C1C 1.291(7) . . yes N2C C2C 1.314(7) . . yes N3C C1C 1.333(7) . . yes N3C C11C 1.464(7) . . yes N4C C2C 1.354(7) . . yes N4C C21C 1.477(8) . . yes N3C H3CA 0.78(5) . . no N4C H4CA 0.95(4) . . no C1A C2A 1.494(7) . . no C11A C12A 1.39(2) . . no C12A C13A 1.01(2) . . no C13A C14A 1.43(2) . . no C21A C22A 1.459(10) . . no C22A C23A 1.361(17) . . no C23A C24A 1.517(16) . . no C11A H11A 0.9700 . . no C11A H11B 0.9700 . . no C12A H12A 0.9700 . . no C12A H12B 0.9700 . . no C13A H13A 0.9700 . . no C13A H13B 0.9600 . . no C14A H14A 0.9600 . . no C14A H14C 0.9600 . . no C14A H14B 0.9600 . . no C21A H21A 0.9700 . . no C21A H21B 0.9700 . . no C22A H22B 0.9700 . . no C22A H22A 0.9700 . . no C23A H23A 0.9700 . . no C23A H23B 0.9700 . . no C24A H24B 0.9600 . . no C24A H24A 0.9600 . . no C24A H24C 0.9600 . . no C1B C2B 1.493(6) . . no C11B C12B 1.461(17) . . no C12B C13B 1.10(3) . . no C13B C14B 1.31(3) . . no C21B C22B 1.36(2) . . no C22B C23B 1.15(3) . . no C23B C24B 1.38(2) . . no C11B H11D 0.9700 . . no C11B H11C 0.9700 . . no C12B H12C 0.9700 . . no C12B H12D 0.9700 . . no C13B H13D 0.9700 . . no C13B H13C 0.9700 . . no C14B H14F 0.9600 . . no C14B H14D 0.9600 . . no C14B H14E 0.9600 . . no C21B H21D 0.9700 . . no C21B H21C 0.9700 . . no C22B H22D 0.9700 . . no C22B H22C 0.9700 . . no C23B H23D 0.9700 . . no C23B H23C 0.9700 . . no C24B H24E 0.9600 . . no C24B H24F 0.9600 . . no C24B H24D 0.9600 . . no C1C C2C 1.497(6) . . no C11C C12C 1.535(10) . . no C12C C13C 1.397(15) . . no C13C C14C 1.372(17) . . no C21C C22C 1.409(14) . . no C22C C23C 1.202(18) . . no C23C C24C 1.411(19) . . no C11C H11E 0.9700 . . no C11C H11F 0.9700 . . no C12C H12E 0.9700 . . no C12C H12F 0.9700 . . no C13C H13E 0.9700 . . no C13C H13F 0.9700 . . no C14C H14G 0.9600 . . no C14C H14H 0.9600 . . no C14C H14I 0.9600 . . no C21C H21E 0.9700 . . no C21C H21F 0.9700 . . no C22C H22E 0.9700 . . no C22C H22F 0.9700 . . no C23C H23E 0.9700 . . no C23C H23F 0.9700 . . no C24C H24G 0.9600 . . no C24C H24H 0.9600 . . no C24C H24I 0.9600 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Pd1 N2A 78.65(14) . . . yes N1A Pd1 N1A 180.00 . . 2_555 yes N1A Pd1 N2A 101.35(14) . . 2_555 yes N1A Pd1 N2A 101.35(14) 2_555 . . yes N2A Pd1 N2A 180.00 . . 2_555 yes N1A Pd1 N2A 78.65(14) 2_555 . 2_555 yes N1B Pd2 N2B 100.78(14) 2_766 . . yes N2B Pd2 N2B 180.00 . . 2_766 yes N1B Pd2 N2B 79.22(14) 2_766 . 2_766 yes N1B Pd2 N2B 100.78(14) . . 2_766 yes N1B Pd2 N2B 79.22(14) . . . yes N1B Pd2 N1B 180.00 . . 2_766 yes N1C Pd3 N2C 79.16(17) 2_665 . 2_665 yes N1C Pd3 N2C 100.84(17) . . 2_665 yes N1C Pd3 N2C 100.84(17) 2_665 . . yes N2C Pd3 N2C 180.00 . . 2_665 yes N1C Pd3 N2C 79.16(17) . . . yes N1C Pd3 N1C 180.00 . . 2_665 yes N1A O1A H1AA 105(3) . . . no N1B O1B H1BA 111(5) . . . no N1C O1C H1CA 102(3) . . . no Pd1 N1A C1A 118.4(3) . . . yes O1A N1A C1A 120.2(4) . . . yes Pd1 N1A O1A 121.4(2) . . . yes Pd1 N2A C2A 117.3(3) . . . yes O2A N2A C2A 123.5(3) . . . yes Pd1 N2A O2A 119.1(2) . . . yes C1A N3A C11A 129.7(5) . . . yes C2A N4A C21A 129.4(5) . . . yes C11A N3A H3AA 123(5) . . . no C1A N3A H3AA 107(5) . . . no C21A N4A H4AA 119(4) . . . no C2A N4A H4AA 112(4) . . . no O1B N1B C1B 119.9(4) . . . yes Pd2 N1B C1B 118.2(3) . . . yes Pd2 N1B O1B 121.9(3) . . . yes O2B N2B C2B 122.8(3) . . . yes Pd2 N2B C2B 116.9(3) . . . yes Pd2 N2B O2B 120.3(2) . . . yes C1B N3B C11B 128.4(4) . . . yes C2B N4B C21B 126.9(5) . . . yes C1B N3B H3BA 119(4) . . . no C11B N3B H3BA 112(4) . . . no C2B N4B H4BA 116(3) . . . no C21B N4B H4BA 114(3) . . . no Pd3 N1C C1C 117.7(3) . . . yes Pd3 N1C O1C 122.2(4) . . . yes O1C N1C C1C 120.1(4) . . . yes Pd3 N2C O2C 120.5(4) . . . yes O2C N2C C2C 122.2(4) . . . yes Pd3 N2C C2C 117.3(3) . . . yes C1C N3C C11C 128.5(5) . . . yes C2C N4C C21C 124.0(5) . . . yes C11C N3C H3CA 116(4) . . . no C1C N3C H3CA 111(4) . . . no C21C N4C H4CA 119(3) . . . no C2C N4C H4CA 113(3) . . . no N3A C1A C2A 119.2(4) . . . yes N1A C1A C2A 112.5(4) . . . yes N1A C1A N3A 128.3(5) . . . yes N2A C2A C1A 113.1(4) . . . yes N2A C2A N4A 126.7(5) . . . yes N4A C2A C1A 120.1(4) . . . yes N3A C11A C12A 116.2(8) . . . yes C11A C12A C13A 157(2) . . . no C12A C13A C14A 138(2) . . . no N4A C21A C22A 112.0(5) . . . yes C21A C22A C23A 122.9(10) . . . no C22A C23A C24A 113.9(12) . . . no N3A C11A H11B 108.00 . . . no C12A C11A H11B 108.00 . . . no C12A C11A H11A 108.00 . . . no H11A C11A H11B 107.00 . . . no N3A C11A H11A 108.00 . . . no C11A C12A H12A 97.00 . . . no H12A C12A H12B 104.00 . . . no C13A C12A H12A 97.00 . . . no C13A C12A H12B 97.00 . . . no C11A C12A H12B 97.00 . . . no C14A C13A H13A 102.00 . . . no C12A C13A H13A 102.00 . . . no C14A C13A H13B 103.00 . . . no C12A C13A H13B 103.00 . . . no H13A C13A H13B 105.00 . . . no H14B C14A H14C 109.00 . . . no C13A C14A H14C 110.00 . . . no H14A C14A H14B 110.00 . . . no C13A C14A H14B 109.00 . . . no C13A C14A H14A 109.00 . . . no H14A C14A H14C 110.00 . . . no H21A C21A H21B 108.00 . . . no N4A C21A H21B 109.00 . . . no C22A C21A H21A 109.00 . . . no C22A C21A H21B 109.00 . . . no N4A C21A H21A 109.00 . . . no C21A C22A H22B 107.00 . . . no C23A C22A H22A 107.00 . . . no H22A C22A H22B 107.00 . . . no C21A C22A H22A 107.00 . . . no C23A C22A H22B 107.00 . . . no C24A C23A H23B 109.00 . . . no C22A C23A H23A 109.00 . . . no H23A C23A H23B 108.00 . . . no C24A C23A H23A 109.00 . . . no C22A C23A H23B 109.00 . . . no C23A C24A H24B 109.00 . . . no C23A C24A H24C 109.00 . . . no C23A C24A H24A 110.00 . . . no H24B C24A H24C 109.00 . . . no H24A C24A H24B 109.00 . . . no H24A C24A H24C 109.00 . . . no N3B C1B C2B 118.4(4) . . . yes N1B C1B N3B 129.1(4) . . . yes N1B C1B C2B 112.5(4) . . . yes N2B C2B N4B 125.7(4) . . . yes N2B C2B C1B 113.2(4) . . . yes N4B C2B C1B 121.1(4) . . . yes N3B C11B C12B 113.0(8) . . . yes C11B C12B C13B 137.0(16) . . . no C12B C13B C14B 136(2) . . . no N4B C21B C22B 118.5(10) . . . yes C21B C22B C23B 155.9(19) . . . no C22B C23B C24B 135.7(18) . . . no H11C C11B H11D 108.00 . . . no C12B C11B H11C 109.00 . . . no C12B C11B H11D 109.00 . . . no N3B C11B H11C 109.00 . . . no N3B C11B H11D 109.00 . . . no H12C C12B H12D 105.00 . . . no C13B C12B H12D 103.00 . . . no C13B C12B H12C 103.00 . . . no C11B C12B H12C 103.00 . . . no C11B C12B H12D 103.00 . . . no C12B C13B H13C 103.00 . . . no C12B C13B H13D 103.00 . . . no C14B C13B H13C 103.00 . . . no C14B C13B H13D 103.00 . . . no H13C C13B H13D 105.00 . . . no C13B C14B H14F 109.00 . . . no H14D C14B H14F 109.00 . . . no H14E C14B H14F 110.00 . . . no H14D C14B H14E 110.00 . . . no C13B C14B H14D 109.00 . . . no C13B C14B H14E 109.00 . . . no H21C C21B H21D 107.00 . . . no C22B C21B H21D 108.00 . . . no N4B C21B H21C 108.00 . . . no N4B C21B H21D 108.00 . . . no C22B C21B H21C 108.00 . . . no C21B C22B H22D 97.00 . . . no C23B C22B H22C 97.00 . . . no C23B C22B H22D 97.00 . . . no C21B C22B H22C 97.00 . . . no H22C C22B H22D 104.00 . . . no H23C C23B H23D 105.00 . . . no C22B C23B H23D 103.00 . . . no C24B C23B H23D 103.00 . . . no C22B C23B H23C 103.00 . . . no C24B C23B H23C 103.00 . . . no C23B C24B H24D 109.00 . . . no H24D C24B H24F 110.00 . . . no H24E C24B H24F 110.00 . . . no C23B C24B H24E 109.00 . . . no C23B C24B H24F 109.00 . . . no H24D C24B H24E 110.00 . . . no N3C C1C C2C 118.1(4) . . . yes N1C C1C C2C 113.4(4) . . . yes N1C C1C N3C 128.5(4) . . . yes N2C C2C C1C 112.5(4) . . . yes N2C C2C N4C 125.5(4) . . . yes N4C C2C C1C 122.0(4) . . . yes N3C C11C C12C 112.7(5) . . . yes C11C C12C C13C 117.2(8) . . . no C12C C13C C14C 118.2(11) . . . no N4C C21C C22C 116.6(8) . . . yes C21C C22C C23C 142.8(14) . . . no C22C C23C C24C 133.5(14) . . . no N3C C11C H11E 109.00 . . . no N3C C11C H11F 109.00 . . . no C12C C11C H11E 109.00 . . . no C12C C11C H11F 109.00 . . . no H11E C11C H11F 108.00 . . . no C11C C12C H12E 108.00 . . . no C11C C12C H12F 108.00 . . . no C13C C12C H12E 108.00 . . . no C13C C12C H12F 108.00 . . . no H12E C12C H12F 107.00 . . . no C12C C13C H13E 108.00 . . . no C12C C13C H13F 108.00 . . . no C14C C13C H13E 108.00 . . . no C14C C13C H13F 108.00 . . . no H13E C13C H13F 107.00 . . . no C13C C14C H14G 110.00 . . . no C13C C14C H14H 109.00 . . . no C13C C14C H14I 109.00 . . . no H14G C14C H14H 110.00 . . . no H14G C14C H14I 109.00 . . . no H14H C14C H14I 109.00 . . . no N4C C21C H21E 108.00 . . . no N4C C21C H21F 108.00 . . . no C22C C21C H21E 108.00 . . . no C22C C21C H21F 108.00 . . . no H21E C21C H21F 107.00 . . . no C21C C22C H22E 101.00 . . . no C21C C22C H22F 101.00 . . . no C23C C22C H22E 101.00 . . . no C23C C22C H22F 101.00 . . . no H22E C22C H22F 104.00 . . . no C22C C23C H23E 104.00 . . . no C22C C23C H23F 104.00 . . . no C24C C23C H23E 104.00 . . . no C24C C23C H23F 104.00 . . . no H23E C23C H23F 105.00 . . . no C23C C24C H24G 109.00 . . . no C23C C24C H24H 109.00 . . . no C23C C24C H24I 109.00 . . . no H24G C24C H24H 109.00 . . . no H24G C24C H24I 109.00 . . . no H24H C24C H24I 110.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2A Pd1 N1A O1A 179.6(3) . . . . no N2A Pd1 N1A C1A -0.9(3) . . . . no N2A Pd1 N1A O1A -0.5(3) 2_555 . . . no N2A Pd1 N1A C1A 179.1(3) 2_555 . . . no N1A Pd1 N2A O2A -177.9(3) . . . . no N1A Pd1 N2A C2A 0.6(3) . . . . no N1A Pd1 N2A O2A 2.1(3) 2_555 . . . no N1A Pd1 N2A C2A -179.4(3) 2_555 . . . no N2B Pd2 N1B O1B -179.9(4) . . . . no N2B Pd2 N1B C1B -0.7(3) . . . . no N2B Pd2 N1B O1B 0.1(4) 2_766 . . . no N2B Pd2 N1B C1B 179.3(3) 2_766 . . . no N1B Pd2 N2B O2B -176.9(3) . . . . no N1B Pd2 N2B C2B 1.3(3) . . . . no N1B Pd2 N2B O2B 3.1(3) 2_766 . . . no N1B Pd2 N2B C2B -178.7(3) 2_766 . . . no N1C Pd3 N2C C2C -179.4(3) 2_665 . . . no N2C Pd3 N1C C1C 0.3(3) . . . . no N2C Pd3 N1C O1C 0.1(3) 2_665 . . . no N2C Pd3 N1C C1C -179.7(3) 2_665 . . . no N1C Pd3 N2C O2C -177.1(3) . . . . no N2C Pd3 N1C O1C -179.9(3) . . . . no N1C Pd3 N2C O2C 2.9(3) 2_665 . . . no N1C Pd3 N2C C2C 0.6(3) . . . . no Pd1 N1A C1A C2A 1.0(5) . . . . no O1A N1A C1A N3A 0.7(8) . . . . no Pd1 N1A C1A N3A -178.9(5) . . . . no O1A N1A C1A C2A -179.4(4) . . . . no Pd1 N2A C2A C1A -0.2(5) . . . . no Pd1 N2A C2A N4A 176.8(5) . . . . no O2A N2A C2A C1A 178.2(4) . . . . no O2A N2A C2A N4A -4.8(8) . . . . no C1A N3A C11A C12A 115.2(12) . . . . no C11A N3A C1A N1A 6.6(10) . . . . no C11A N3A C1A C2A -173.2(6) . . . . no C2A N4A C21A C22A -147.1(7) . . . . no C21A N4A C2A N2A -16.3(10) . . . . no C21A N4A C2A C1A 160.5(6) . . . . no Pd2 N1B C1B N3B -178.9(4) . . . . no O1B N1B C1B N3B 0.4(8) . . . . no Pd2 N1B C1B C2B 0.0(5) . . . . no O1B N1B C1B C2B 179.3(4) . . . . no O2B N2B C2B C1B 176.5(4) . . . . no Pd2 N2B C2B C1B -1.6(5) . . . . no Pd2 N2B C2B N4B 179.5(4) . . . . no O2B N2B C2B N4B -2.3(7) . . . . no C1B N3B C11B C12B 84.5(9) . . . . no C11B N3B C1B N1B 7.2(10) . . . . no C11B N3B C1B C2B -171.7(6) . . . . no C21B N4B C2B C1B 143.9(7) . . . . no C21B N4B C2B N2B -37.4(9) . . . . no C2B N4B C21B C22B -92.3(12) . . . . no Pd3 N1C C1C C2C -1.1(5) . . . . no O1C N1C C1C N3C -1.5(7) . . . . no Pd3 N1C C1C N3C 178.3(4) . . . . no O1C N1C C1C C2C 179.1(3) . . . . no O2C N2C C2C C1C 176.4(4) . . . . no Pd3 N2C C2C N4C -179.8(4) . . . . no Pd3 N2C C2C C1C -1.3(5) . . . . no O2C N2C C2C N4C -2.1(7) . . . . no C11C N3C C1C C2C -165.7(5) . . . . no C1C N3C C11C C12C 82.0(9) . . . . no C11C N3C C1C N1C 15.0(8) . . . . no C2C N4C C21C C22C -78.4(10) . . . . no C21C N4C C2C N2C -43.8(7) . . . . no C21C N4C C2C C1C 137.9(5) . . . . no N3A C1A C2A N2A 179.4(5) . . . . no N1A C1A C2A N4A -177.8(5) . . . . no N3A C1A C2A N4A 2.1(8) . . . . no N1A C1A C2A N2A -0.5(6) . . . . no N3A C11A C12A C13A 42(6) . . . . no C11A C12A C13A C14A 164(4) . . . . no N4A C21A C22A C23A 70.2(12) . . . . no C21A C22A C23A C24A 169.2(8) . . . . no N1B C1B C2B N2B 1.0(6) . . . . no N1B C1B C2B N4B 179.9(5) . . . . no N3B C1B C2B N2B -180.0(4) . . . . no N3B C1B C2B N4B -1.1(7) . . . . no N3B C11B C12B C13B 126(2) . . . . no C11B C12B C13B C14B 164(2) . . . . no N4B C21B C22B C23B 32(5) . . . . no C21B C22B C23B C24B -167(3) . . . . no N1C C1C C2C N2C 1.5(5) . . . . no N1C C1C C2C N4C -179.9(4) . . . . no N3C C1C C2C N2C -177.9(4) . . . . no N3C C1C C2C N4C 0.7(6) . . . . no N3C C11C C12C C13C 162.7(9) . . . . no C11C C12C C13C C14C 174.4(12) . . . . no N4C C21C C22C C23C -5(3) . . . . no C21C C22C C23C C24C -172.9(19) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd1 C11C 4.036(8) . . no Pd1 C11C 4.036(8) . 2_555 no Pd1 H11F 3.2400 . . no Pd1 H13E 3.6200 . . no Pd1 H11F 3.2400 . 2_555 no Pd1 H13E 3.6200 . 2_555 no Pd2 H13A 3.4100 . 1_655 no Pd2 H24C 3.4400 . . no Pd2 H13A 3.4100 . 2_666 no Pd2 H24C 3.4400 . 2_766 no Pd3 H24F 3.6100 . 1_455 no Pd3 H11C 3.5300 . 2_665 no Pd3 H11C 3.5300 . . no Pd3 H24F 3.6100 . 2_765 no O1A O2A 2.612(4) . 2_555 no O1A N2A 3.166(4) . 2_555 no O1A C11A 2.815(7) . . no O1A N3A 2.817(6) . . no O1B C12B 3.311(14) . . no O1B N2B 3.151(6) . 2_766 no O1B O2B 2.621(5) . 2_766 no O1B N3B 2.833(6) . . no O1B C11B 2.817(8) . . no O1C C11C 2.821(10) . . no O1C N3C 2.814(7) . . no O1C O2C 2.650(7) . 2_665 no O1C N2C 3.170(6) . 2_665 no O2A C21A 2.894(7) . . no O2A N4A 2.859(5) . . no O2A N3C 2.859(6) . . no O2A N1A 3.112(4) . 2_555 no O2A N4C 2.957(6) . . no O2A O1A 2.612(4) . 2_555 no O2B C21B 2.944(9) . . no O2B N4B 2.832(5) . . no O2B O1B 2.621(5) . 2_766 no O2B N3A 2.882(7) . 1_655 no O2B N1B 3.111(4) . 2_766 no O2B N4A 2.935(6) . 1_655 no O2C N3B 2.858(6) . . no O2C C21C 2.958(9) . . no O2C O1C 2.650(7) . 2_665 no O2C N4C 2.818(7) . . no O2C N1C 3.124(7) . 2_665 no O2C N4B 2.923(6) . . no O1A H11B 2.0700 . . no O1A H22F 2.8100 . 1_455 no O1A H23F 2.6400 . 2_555 no O1B H11D 2.2400 . . no O1B H12C 2.8600 . . no O1C H11E 2.2200 . . no O2A H4CA 2.03(5) . . no O2A H1AA 1.69(5) . 2_555 no O2A H21B 2.4500 . . no O2A H3CA 2.15(5) . . no O2B H3AA 2.28(6) . 1_655 no O2B H1BA 1.90(6) . 2_766 no O2B H21C 2.2400 . . no O2B H4AA 2.20(5) . 1_655 no O2B H22B 2.9100 . 1_655 no O2C H3BA 2.03(6) . . no O2C H21E 2.2800 . . no O2C H1CA 1.91(5) . 2_665 no O2C H4BA 2.17(4) . . no N1A N2A 2.494(5) . . no N1A C2A 2.314(6) . . no N1A O2A 3.112(4) . 2_555 no N1A N2A 3.045(4) . 2_555 no N1B C2B 2.321(5) . . no N1B O2B 3.111(4) . 2_766 no N1B N2B 3.025(4) . 2_766 no N1B N2B 2.504(5) . . no N1C N2C 3.038(7) . 2_665 no N1C O2C 3.124(7) . 2_665 no N1C N2C 2.512(5) . . no N1C C2C 2.333(6) . . no N2A O1A 3.166(4) . 2_555 no N2A N1A 3.045(4) . 2_555 no N2A N1A 2.494(5) . . no N2A C1A 2.330(6) . . no N2B N1B 2.504(5) . . no N2B C1B 2.341(6) . . no N2B O1B 3.151(6) . 2_766 no N2B N1B 3.025(4) . 2_766 no N2C N1C 2.512(5) . . no N2C C1C 2.339(6) . . no N2C N1C 3.038(7) . 2_665 no N2C O1C 3.170(6) . 2_665 no N3A N4A 2.822(8) . . no N3A O2B 2.882(7) . 1_455 no N3A O1A 2.817(6) . . no N3B O1B 2.833(6) . . no N3B N4B 2.826(7) . . no N3B O2C 2.858(6) . . no N3C N4C 2.844(6) . . no N3C O1C 2.814(7) . . no N3C O2A 2.859(6) . . no N4A N3A 2.822(8) . . no N4A O2A 2.859(5) . . no N4A O2B 2.935(6) . 1_455 no N4B N3B 2.826(7) . . no N4B O2C 2.923(6) . . no N4B O2B 2.832(5) . . no N4C O2C 2.818(7) . . no N4C N3C 2.844(6) . . no N4C O2A 2.957(6) . . no N1A H11B 2.7000 . . no N1B H11D 2.8400 . . no N1C H11E 2.8400 . . no N2A H1AA 2.44(5) . 2_555 no N2A H3CA 2.81(5) . . no N2A H21B 2.8300 . . no N2B H21C 2.7000 . . no N2B H3AA 2.93(6) . 1_655 no N2B H1BA 2.61(6) . 2_766 no N2C H3BA 2.69(6) . . no N2C H21E 2.7800 . . no N2C H1CA 2.55(4) . 2_665 no N3A H4AA 2.47(5) . . no N3B H4BA 2.51(4) . . no N3C H4CA 2.46(4) . . no N4A H3AA 2.42(5) . . no N4A H23B 2.8900 . . no N4A H21C 2.8900 . 1_455 no N4B H3BA 2.48(6) . . no N4B H21E 2.8800 . . no N4C H23F 2.9500 . . no N4C H3CA 2.43(5) . . no N4C H21A 2.8000 . . no C11A O1A 2.815(7) . . no C11B O1B 2.817(8) . . no C11C O1C 2.821(10) . . no C11C Pd1 4.036(8) . . no C11C Pd1 4.036(8) . . no C12B O1B 3.311(14) . . no C21A O2A 2.894(7) . . no C21B O2B 2.944(9) . . no C21C O2C 2.958(9) . . no C1B H12D 2.9500 . . no C13C H24I 2.9800 . 1_455 no C21A H4CA 2.88(4) . . no H1AA N2A 2.44(5) . 2_555 no H1AA H23F 2.5100 . 2_555 no H1AA O2A 1.69(5) . 2_555 no H3AA O2B 2.28(6) . 1_455 no H3AA H4AA 1.96(7) . . no H3AA N2B 2.93(6) . 1_455 no H3AA N4A 2.42(5) . . no H4AA H3AA 1.96(7) . . no H4AA N3A 2.47(5) . . no H4AA H21C 2.4600 . 1_455 no H4AA H22B 2.3300 . . no H4AA O2B 2.20(5) . 1_455 no H1BA O2B 1.90(6) . 2_766 no H1BA N2B 2.61(6) . 2_766 no H3BA N2C 2.69(6) . . no H3BA N4B 2.48(6) . . no H3BA O2C 2.03(6) . . no H3BA H12D 2.5800 . . no H3BA H4BA 1.99(7) . . no H4BA H3BA 1.99(7) . . no H4BA O2C 2.17(4) . . no H4BA N3B 2.51(4) . . no H4BA H21E 2.3600 . . no H1CA N2C 2.55(4) . 2_665 no H1CA O2C 1.91(5) . 2_665 no H3CA N2A 2.81(5) . . no H3CA N4C 2.43(5) . . no H3CA H4CA 1.89(6) . . no H3CA H12F 2.5500 . . no H3CA O2A 2.15(5) . . no H4CA C21A 2.88(4) . . no H4CA H21A 2.3100 . . no H4CA H3CA 1.89(6) . . no H4CA O2A 2.03(5) . . no H4CA N3C 2.46(4) . . no H11B O1A 2.0700 . . no H11B N1A 2.7000 . . no H11C Pd3 3.5300 . . no H11C Pd3 3.5300 . . no H11C H13C 2.4000 . . no H11D N1B 2.8400 . . no H11D O1B 2.2400 . . no H11E N1C 2.8400 . . no H11E O1C 2.2200 . . no H11F Pd1 3.2400 . . no H11F Pd1 3.2400 . . no H11F H13E 2.4800 . . no H12A H14C 2.2000 . . no H12B H14C 2.5100 . . no H12C H14E 2.5800 . . no H12C O1B 2.8600 . . no H12C H14F 2.3600 . . no H12D H3BA 2.5800 . . no H12D H14E 2.4300 . . no H12D C1B 2.9500 . . no H12E H14I 2.3800 . . no H12F H3CA 2.5500 . . no H12F H14H 2.4800 . . no H13A Pd2 3.4100 . 2_666 no H13A Pd2 3.4100 . 1_455 no H13B H14H 2.5000 . 2_555 no H13C H24F 2.4900 . 1_455 no H13C H11C 2.4000 . . no H13E Pd1 3.6200 . . no H13E H11F 2.4800 . . no H13E Pd1 3.6200 . . no H13F H24I 2.5500 . 1_455 no H13F H24D 2.4100 . 2_665 no H14C H12B 2.5100 . . no H14C H12A 2.2000 . . no H14E H12C 2.5800 . . no H14E H12D 2.4300 . . no H14F H12C 2.3600 . . no H14H H12F 2.4800 . . no H14H H13B 2.5000 . 2_555 no H14I H12E 2.3800 . . no H21A H4CA 2.3100 . . no H21A N4C 2.8000 . . no H21B H23A 2.4600 . . no H21B N2A 2.8300 . . no H21B O2A 2.4500 . . no H21C N4A 2.8900 . 1_655 no H21C H4AA 2.4600 . 1_655 no H21C O2B 2.2400 . . no H21C N2B 2.7000 . . no H21E H4BA 2.3600 . . no H21E O2C 2.2800 . . no H21E N2C 2.7800 . . no H21E N4B 2.8800 . . no H22A H24C 2.2900 . . no H22B H24B 2.5100 . . no H22B H4AA 2.3300 . . no H22B O2B 2.9100 . 1_455 no H22C H24F 2.4400 . . no H22D H24E 2.3000 . . no H22E H24I 2.5200 . . no H22F H24H 2.4200 . . no H22F O1A 2.8100 . 1_655 no H23A H21B 2.4600 . . no H23B N4A 2.8900 . . no H23F H1AA 2.5100 . 2_555 no H23F O1A 2.6400 . 2_555 no H23F N4C 2.9500 . . no H24B H22B 2.5100 . . no H24C Pd2 3.4400 . . no H24C H22A 2.2900 . . no H24C Pd2 3.4400 . . no H24D H13F 2.4100 . 2_665 no H24E H22D 2.3000 . . no H24F H13C 2.4900 . 1_655 no H24F H22C 2.4400 . . no H24F Pd3 3.6100 . 2_765 no H24F Pd3 3.6100 . 1_655 no H24H H22F 2.4200 . . no H24I C13C 2.9800 . 1_655 no H24I H13F 2.5500 . 1_655 no H24I H22E 2.5200 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1A H1AA O2A 0.94(5) 1.69(5) 2.612(4) 164(5) 2_555 yes N3A H3AA O2B 0.66(6) 2.28(6) 2.882(7) 153(6) 1_455 yes N4A H4AA O2B 0.74(5) 2.20(5) 2.935(6) 173(4) 1_455 yes O1B H1BA O2B 0.76(6) 1.90(6) 2.621(5) 157(6) 2_766 yes N4B H4BA O2C 0.76(4) 2.17(4) 2.923(6) 171(4) . yes O1C H1CA O2C 0.75(5) 1.91(5) 2.650(7) 172(4) 2_665 yes N3C H3CA O2A 0.78(5) 2.15(5) 2.859(6) 153(5) . yes N4C H4CA O2A 0.95(4) 2.03(5) 2.957(6) 163(4) . yes C11A H11B O1A 0.9700 2.0700 2.815(7) 132.00 . yes C11B H11D O1B 0.9700 2.2400 2.817(8) 117.00 . yes C11C H11E O1C 0.9700 2.2200 2.821(10) 119.00 . yes C21A H21B O2A 0.9700 2.4500 2.894(7) 108.00 . yes C21B H21C O2B 0.9700 2.2400 2.944(9) 129.00 . yes C21C H21E O2C 0.9700 2.2800 2.958(9) 126.00 . yes _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 0.680 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.073 # Attachment 'VAC5Ni4.CIF' data_VAC5N14 _database_code_depnum_ccdc_archive 'CCDC 648646' _audit_creation_date 07-07-10 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '02201 in space group P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.7343(4) _cell_length_b 8.5124(2) _cell_length_c 14.2237(4) _cell_angle_alpha 90 _cell_angle_beta 118.488(1) _cell_angle_gamma 90 _cell_volume 1461.57(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+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' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' _cell_formula_units_Z 2 # Given Formula = C24 H50 N8 Ni1 O4 # Dc = 1.30 Fooo = 620.00 Mu = 7.07 M = 286.71 # Found Formula = C24 H50 N8 Ni1 O4 # Dc = 1.30 FOOO = 620.00 Mu = 7.07 M = 286.71 _chemical_formula_sum 'C24 H50 N8 Ni1 O4' _chemical_formula_moiety 'C24 H50 N8 Ni1 O4' _chemical_compound_source ? _chemical_formula_weight 573.42 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 298 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.707 # Sheldrick geometric approximatio 0.93 0.93 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 298 _diffrn_reflns_number 7082 _reflns_number_total 3599 _diffrn_reflns_av_R_equivalents 0.055 # Number of reflections with Friedels Law is 3599 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3841 _diffrn_reflns_theta_min 1.696 _diffrn_reflns_theta_max 28.875 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 27.143 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.36 _refine_diff_density_max 0.42 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2588 _refine_ls_number_restraints 0 _refine_ls_number_parameters 169 _oxford_refine_ls_R_factor_ref 0.0445 _refine_ls_wR_factor_ref 0.0515 _refine_ls_goodness_of_fit_ref 1.0728 _refine_ls_shift/su_max 0.000236 # The values computed from all data _oxford_reflns_number_all 3581 _refine_ls_R_factor_all 0.0718 _refine_ls_wR_factor_all 0.0620 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2588 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_gt 0.0515 # 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: 1.53 1.51 1.08 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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 Ni1 Ni 0.5000 0.0000 0.5000 0.0321 1.0000 Uani S . . . . . . N1 N 0.35075(13) -0.0098(2) 0.39467(12) 0.0354 1.0000 Uani . . . . . . . O1 O 0.26874(12) 0.0684(2) 0.40189(11) 0.0431 1.0000 Uani . . . . . . . H4 H 0.3011 0.1060 0.4653 0.0620 1.0000 Uiso R . . . . . . C1 C 0.32848(15) -0.0932(2) 0.31083(15) 0.0363 1.0000 Uani . . . . . . . N3 N 0.22728(15) -0.1133(3) 0.22345(15) 0.0541 1.0000 Uani . . . . . . . C11 C 0.12743(17) -0.1550(3) 0.23023(17) 0.0424 1.0000 Uani . . . . . . . C12 C 0.02538(17) -0.1179(3) 0.12502(16) 0.0428 1.0000 Uani . . . . . . . C13 C -0.08037(18) -0.1818(3) 0.12008(18) 0.0447 1.0000 Uani . . . . . . . C14 C -0.18362(19) -0.1303(3) 0.0200(2) 0.0530 1.0000 Uani . . . . . . . C15 C -0.2894(2) -0.2058(4) 0.0080(3) 0.0685 1.0000 Uani . . . . . . . H12 H -0.3505 -0.1741 -0.0588 0.0971 1.0000 Uiso R . . . . . . H13 H -0.3008 -0.1745 0.0676 0.0964 1.0000 Uiso R . . . . . . H14 H -0.2811 -0.3175 0.0077 0.0967 1.0000 Uiso R . . . . . . H15 H -0.1747 -0.1554 -0.0421 0.0599 1.0000 Uiso R . . . . . . H16 H -0.1890 -0.0173 0.0248 0.0605 1.0000 Uiso R . . . . . . H17 H -0.0790 -0.2941 0.1212 0.0520 1.0000 Uiso R . . . . . . H18 H -0.0859 -0.1447 0.1808 0.0509 1.0000 Uiso R . . . . . . H19 H 0.0347 -0.1626 0.0671 0.0487 1.0000 Uiso R . . . . . . H20 H 0.0173 -0.0020 0.1160 0.0476 1.0000 Uiso R . . . . . . H21 H 0.1255 -0.0988 0.2876 0.0482 1.0000 Uiso R . . . . . . H22 H 0.1300 -0.2656 0.2439 0.0480 1.0000 Uiso R . . . . . . H23 H 0.2256 -0.1119 0.1630 0.0614 1.0000 Uiso R . . . . . . C2 C 0.43037(15) -0.1576(2) 0.31225(15) 0.0354 1.0000 Uani . . . . . . . N2 N 0.51915(13) -0.1157(2) 0.39891(13) 0.0378 1.0000 Uani . . . . . . . O2 O 0.61978(13) -0.1764(2) 0.41548(14) 0.0566 1.0000 Uani . . . . . . . N4 N 0.42103(14) -0.2443(2) 0.22960(15) 0.0428 1.0000 Uani . . . . . . . C21 C 0.51172(18) -0.2888(3) 0.20861(18) 0.0461 1.0000 Uani . . . . . . . C22 C 0.4667(2) -0.3398(3) 0.0925(2) 0.0491 1.0000 Uani . . . . . . . C23 C 0.4100(2) -0.2117(3) 0.01069(19) 0.0519 1.0000 Uani . . . . . . . C24 C 0.3690(3) -0.2634(4) -0.1041(2) 0.0663 1.0000 Uani . . . . . . . C25 C 0.3174(3) -0.1314(5) -0.1844(2) 0.0819 1.0000 Uani . . . . . . . H33 H 0.2850 -0.1750 -0.2558 0.1210 1.0000 Uiso R . . . . . . H34 H 0.3737 -0.0567 -0.1757 0.1209 1.0000 Uiso R . . . . . . H35 H 0.2603 -0.0785 -0.1748 0.1211 1.0000 Uiso R . . . . . . H36 H 0.3156 -0.3483 -0.1206 0.0819 1.0000 Uiso R . . . . . . H37 H 0.4315 -0.3049 -0.1097 0.0821 1.0000 Uiso R . . . . . . H38 H 0.3459 -0.1775 0.0188 0.0648 1.0000 Uiso R . . . . . . H39 H 0.4616 -0.1248 0.0281 0.0652 1.0000 Uiso R . . . . . . H40 H 0.5292 -0.3789 0.0840 0.0608 1.0000 Uiso R . . . . . . H41 H 0.4144 -0.4260 0.0767 0.0611 1.0000 Uiso R . . . . . . H42 H 0.5528 -0.3746 0.2545 0.0550 1.0000 Uiso R . . . . . . H43 H 0.5607 -0.1989 0.2234 0.0551 1.0000 Uiso R . . . . . . H44 H 0.3582 -0.2812 0.1901 0.0505 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02331(17) 0.03172(18) 0.03164(17) 0.00098(15) 0.00526(12) 0.00268(14) N1 0.0253(7) 0.0372(8) 0.0355(7) 0.0030(7) 0.0078(6) 0.0054(6) O1 0.0270(6) 0.0552(9) 0.0354(7) -0.0024(6) 0.0055(5) 0.0109(6) C1 0.0261(8) 0.0427(11) 0.0336(8) 0.0024(7) 0.0090(7) 0.0000(7) N3 0.0277(8) 0.0943(16) 0.0326(8) -0.0080(9) 0.0082(7) -0.0021(9) C11 0.0298(9) 0.0530(12) 0.0373(10) -0.0031(8) 0.0104(8) -0.0012(8) C12 0.0296(9) 0.0536(12) 0.0364(9) -0.0071(8) 0.0085(8) -0.0003(8) C13 0.0334(10) 0.0473(12) 0.0465(11) -0.0096(9) 0.0134(8) -0.0046(8) C18 0.0324(11) 0.0656(15) 0.0488(12) -0.0107(10) 0.0096(9) 0.0009(10) C15 0.0340(12) 0.085(2) 0.0723(17) -0.0204(15) 0.0136(11) -0.0071(11) C2 0.0286(9) 0.0370(9) 0.0350(9) 0.0023(7) 0.0106(7) -0.0011(7) N2 0.0259(8) 0.0406(8) 0.0380(8) -0.0019(7) 0.0079(6) 0.0033(6) O2 0.0258(7) 0.0728(12) 0.0561(9) -0.0184(8) 0.0072(7) 0.0101(7) N4 0.0299(8) 0.0513(10) 0.0424(8) -0.0115(8) 0.0134(7) -0.0082(7) C21 0.0360(10) 0.0523(12) 0.0469(11) -0.0019(9) 0.0173(9) 0.0019(9) C22 0.0454(12) 0.0508(12) 0.0549(12) -0.0090(10) 0.0269(10) -0.0022(10) C23 0.0532(13) 0.0547(13) 0.0485(12) -0.0067(10) 0.0247(11) -0.0022(10) C24 0.0696(17) 0.0787(19) 0.0516(13) -0.0102(13) 0.0298(13) 0.0005(15) C25 0.081(2) 0.102(3) 0.0507(15) 0.0019(16) 0.0224(15) 0.0028(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5274(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.8772(18) . . yes Ni1 N2 1.8621(17) . . yes Ni1 N1 1.8772(18) . 3_656 yes Ni1 N2 1.8621(17) . 3_656 yes O1 N1 1.354(3) . . yes O2 N2 1.386(3) . . yes O1 H4 0.8600 . . no N1 C1 1.293(2) . . yes N2 C2 1.304(3) . . yes N3 C11 1.464(3) . . yes N3 C1 1.363(3) . . yes N4 C2 1.341(3) . . yes N4 C21 1.463(3) . . yes N3 H23 0.8500 . . no N4 H44 0.8300 . . no C1 C2 1.494(3) . . no C11 C12 1.518(3) . . no C12 C13 1.521(4) . . no C13 C14 1.518(4) . . no C14 C15 1.522(4) . . no C21 C22 1.525(3) . . no C22 C23 1.512(4) . . no C23 C24 1.516(4) . . no C24 C25 1.516(5) . . no C11 H21 0.9600 . . no C11 H22 0.9600 . . no C12 H19 0.9700 . . no C12 H20 0.9900 . . no C13 H17 0.9600 . . no C13 H18 0.9600 . . no C14 H15 0.9700 . . no C14 H16 0.9700 . . no C15 H12 0.9600 . . no C15 H13 0.9700 . . no C15 H14 0.9600 . . no C21 H42 0.9600 . . no C21 H43 0.9700 . . no C22 H40 0.9800 . . no C22 H41 0.9800 . . no C23 H38 0.9800 . . no C23 H39 0.9700 . . no C24 H36 0.9800 . . no C24 H37 0.9700 . . no C25 H33 0.9700 . . no C25 H34 0.9600 . . no C25 H35 0.9700 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 82.12(8) . . . yes N1 Ni1 N1 180.00 . . 3_656 yes N1 Ni1 N2 97.88(8) . . 3_656 yes N1 Ni1 N2 97.88(8) 3_656 . . yes N2 Ni1 N2 180.00 . . 3_656 yes N1 Ni1 N2 82.12(8) 3_656 . 3_656 yes N1 O1 H4 103.00 . . . no Ni1 N1 C1 116.64(16) . . . yes O1 N1 C1 120.04(17) . . . yes Ni1 N1 O1 123.29(12) . . . yes Ni1 N2 O2 124.22(13) . . . yes O2 N2 C2 117.76(17) . . . yes Ni1 N2 C2 117.51(16) . . . yes C1 N3 C11 123.39(19) . . . yes C2 N4 C21 125.9(2) . . . yes C11 N3 H23 120.00 . . . no C1 N3 H23 116.00 . . . no C2 N4 H44 116.00 . . . no C21 N4 H44 118.00 . . . no N1 C1 N3 126.9(2) . . . yes N1 C1 C2 112.40(18) . . . yes N3 C1 C2 120.49(18) . . . yes N4 C2 C1 119.51(18) . . . yes N2 C2 C1 111.10(17) . . . yes N2 C2 N4 129.4(2) . . . yes N3 C11 C12 109.77(19) . . . yes C11 C12 C13 112.56(19) . . . no C12 C13 C14 112.6(2) . . . no C13 C14 C15 113.5(2) . . . no N4 C21 C22 110.5(2) . . . yes C21 C22 C23 115.0(2) . . . no C22 C23 C24 114.2(2) . . . no C23 C24 C25 113.3(3) . . . no N3 C11 H21 110.00 . . . no N3 C11 H22 108.00 . . . no C12 C11 H21 110.00 . . . no C12 C11 H22 109.00 . . . no H21 C11 H22 109.00 . . . no C11 C12 H19 109.00 . . . no C11 C12 H20 109.00 . . . no C13 C12 H19 109.00 . . . no C13 C12 H20 108.00 . . . no H19 C12 H20 109.00 . . . no C12 C13 H17 110.00 . . . no C12 C13 H18 109.00 . . . no C14 C13 H17 108.00 . . . no C14 C13 H18 108.00 . . . no H17 C13 H18 109.00 . . . no C13 C14 H15 109.00 . . . no C13 C14 H16 107.00 . . . no C15 C14 H15 109.00 . . . no C15 C14 H16 109.00 . . . no H15 C14 H16 109.00 . . . no C14 C15 H12 109.00 . . . no C14 C15 H13 109.00 . . . no C14 C15 H14 108.00 . . . no H12 C15 H13 111.00 . . . no H12 C15 H14 109.00 . . . no H13 C15 H14 110.00 . . . no N4 C21 H42 110.00 . . . no N4 C21 H43 109.00 . . . no C22 C21 H42 109.00 . . . no C22 C21 H43 110.00 . . . no H42 C21 H43 109.00 . . . no C21 C22 H40 108.00 . . . no C21 C22 H41 110.00 . . . no C23 C22 H40 108.00 . . . no C23 C22 H41 108.00 . . . no H40 C22 H41 108.00 . . . no C22 C23 H38 107.00 . . . no C22 C23 H39 108.00 . . . no C24 C23 H38 109.00 . . . no C24 C23 H39 110.00 . . . no H38 C23 H39 109.00 . . . no C23 C24 H36 109.00 . . . no C23 C24 H37 108.00 . . . no C25 C24 H36 110.00 . . . no C25 C24 H37 109.00 . . . no H36 C24 H37 108.00 . . . no C24 C25 H33 109.00 . . . no C24 C25 H34 110.00 . . . no C24 C25 H35 111.00 . . . no H33 C25 H34 109.00 . . . no H33 C25 H35 109.00 . . . no H34 C25 H35 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 O1 -173.72(16) . . . . no N2 Ni1 N1 C1 4.45(15) . . . . no N2 Ni1 N1 O1 6.28(16) 3_656 . . . no N2 Ni1 N1 C1 -175.55(15) 3_656 . . . no N1 Ni1 N2 O2 -175.76(17) . . . . no N1 Ni1 N2 C2 -4.14(15) . . . . no N1 Ni1 N2 O2 4.24(17) 3_656 . . . no N1 Ni1 N2 C2 175.86(15) 3_656 . . . no Ni1 N1 C1 N3 -177.93(18) . . . . no Ni1 N1 C1 C2 -3.9(2) . . . . no O1 N1 C1 N3 0.3(3) . . . . no O1 N1 C1 C2 174.34(16) . . . . no Ni1 N2 C2 N4 -177.72(16) . . . . no Ni1 N2 C2 C1 3.1(2) . . . . no O2 N2 C2 N4 -5.6(3) . . . . no O2 N2 C2 C1 175.25(16) . . . . no C11 N3 C1 N1 -48.7(3) . . . . no C11 N3 C1 C2 137.7(2) . . . . no C1 N3 C11 C12 162.0(2) . . . . no C21 N4 C2 N2 -12.1(3) . . . . no C21 N4 C2 C1 167.01(19) . . . . no C2 N4 C21 C22 -161.8(2) . . . . no N1 C1 C2 N2 0.6(2) . . . . no N1 C1 C2 N4 -178.74(17) . . . . no N3 C1 C2 N2 175.02(19) . . . . no N3 C1 C2 N4 -4.3(3) . . . . no N3 C11 C12 C13 170.9(2) . . . . no C11 C12 C13 C14 174.0(2) . . . . no C12 C13 C14 C15 174.3(2) . . . . no N4 C21 C22 C23 65.4(3) . . . . no C21 C22 C23 C24 178.2(3) . . . . no C22 C23 C24 C25 -177.2(3) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni1 C11 4.116(2) . 2_555 no Ni1 C12 3.643(2) . 2_555 no Ni1 C13 3.643(3) . 2_555 no Ni1 C14 4.127(3) . 2_555 no Ni1 C14 4.127(3) . 4_545 no Ni1 C11 4.116(2) . 4_545 no Ni1 C12 3.643(2) . 4_545 no Ni1 C13 3.643(3) . 4_545 no Ni1 H17 3.0000 . 2_555 no Ni1 H19 2.9900 . 2_555 no Ni1 H22 3.6500 . 2_555 no Ni1 H15 3.6500 . 2_555 no Ni1 H15 3.6500 . 4_545 no Ni1 H17 3.0000 . 4_545 no Ni1 H19 2.9900 . 4_545 no Ni1 H22 3.6500 . 4_545 no O1 N3 2.789(3) . . no O1 C11 2.971(3) . . no O1 O2 2.479(2) . 3_656 no O1 N3 3.258(3) . 2_555 no O1 N4 2.861(3) . 2_555 no O1 C22 3.364(4) . 2_555 no O1 N2 2.967(2) . 3_656 no O2 C21 2.759(3) . . no O2 N1 2.988(2) . 3_656 no O2 O1 2.479(2) . 3_656 no O2 N4 2.809(3) . . no O1 H44 2.0500 . 2_555 no O1 H14 2.8800 . 4_545 no O1 H41 2.6700 . 2_555 no O1 H21 2.3400 . . no O1 H23 2.8900 . 2_555 no O2 H43 2.4600 . . no O2 H42 2.6300 . . no O2 H4 1.6300 . 3_656 no N1 N2 2.456(3) . . no N1 C2 2.319(3) . . no N1 O2 2.988(2) . 3_656 no N1 N2 2.820(2) . 3_656 no N2 O1 2.967(2) . 3_656 no N2 N1 2.456(3) . . no N2 C1 2.310(3) . . no N2 N1 2.820(2) . 3_656 no N3 O1 3.258(3) . 2_545 no N3 O1 2.789(3) . . no N3 N4 2.848(3) . . no N4 O1 2.861(3) . 2_545 no N4 N3 2.848(3) . . no N4 O2 2.809(3) . . no N1 H21 2.8200 . . no N2 H17 2.9100 . 2_555 no N2 H43 2.9000 . . no N2 H4 2.3000 . 3_656 no N3 H44 2.5100 . . no N4 H23 2.6400 . . no N4 H38 2.7300 . . no N4 H20 2.9300 . 2_545 no C11 O1 2.971(3) . . no C11 Ni1 4.116(2) . 2_545 no C11 Ni1 4.116(2) . 4_444 no C12 Ni1 3.643(2) . 4_444 no C12 Ni1 3.643(2) . 2_545 no C13 Ni1 3.643(3) . 2_545 no C13 Ni1 3.643(3) . 4_444 no C14 Ni1 4.127(3) . 2_545 no C14 Ni1 4.127(3) . 4_444 no C21 O2 2.759(3) . . no C22 O1 3.364(4) . 2_545 no C1 H15 3.0100 . 4_545 no C1 H22 3.0200 . 2_555 no C2 H20 3.0700 . 2_545 no C13 H42 3.0900 . 2_555 no C23 H44 3.0200 . . no H4 H44 2.4500 . 2_555 no H4 O2 1.6300 . 3_656 no H4 N2 2.3000 . 3_656 no H13 H35 2.5400 . 3_555 no H13 H33 2.5500 . 4_445 no H14 H17 2.4600 . . no H14 O1 2.8800 . 4_444 no H15 H19 2.5300 . . no H15 Ni1 3.6500 . 2_545 no H15 Ni1 3.6500 . 4_444 no H15 C1 3.0100 . 4_444 no H16 H20 2.4900 . . no H16 H38 2.5500 . 3_555 no H17 H14 2.4600 . . no H17 H22 2.5600 . . no H17 Ni1 3.0000 . 2_545 no H17 N2 2.9100 . 2_545 no H17 Ni1 3.0000 . 4_444 no H18 H21 2.5900 . . no H18 H42 2.4400 . 2_555 no H19 H15 2.5300 . . no H19 H23 2.3500 . . no H19 Ni1 2.9900 . 2_545 no H19 Ni1 2.9900 . 4_444 no H20 H16 2.4900 . . no H20 N4 2.9300 . 2_555 no H20 C2 3.0700 . 2_555 no H21 O1 2.3400 . . no H21 N1 2.8200 . . no H21 H18 2.5900 . . no H22 H17 2.5600 . . no H22 Ni1 3.6500 . 2_545 no H22 C1 3.0200 . 2_545 no H22 Ni1 3.6500 . 4_444 no H23 N4 2.6400 . . no H23 H19 2.3500 . . no H23 H44 2.2100 . . no H23 O1 2.8900 . 2_545 no H33 H13 2.5500 . 4_544 no H34 H43 2.5700 . 3_655 no H35 H38 2.5700 . . no H35 H13 2.5400 . 3_555 no H35 H42 2.5600 . 4_444 no H36 H41 2.5500 . . no H37 H40 2.5000 . . no H38 N4 2.7300 . . no H38 H35 2.5700 . . no H38 H44 2.5200 . . no H38 H16 2.5500 . 3_555 no H39 H43 2.5200 . . no H40 H37 2.5000 . . no H41 H36 2.5500 . . no H41 H44 2.4300 . . no H41 O1 2.6700 . 2_545 no H42 O2 2.6300 . . no H42 C13 3.0900 . 2_545 no H42 H18 2.4400 . 2_545 no H42 H35 2.5600 . 4_545 no H43 O2 2.4600 . . no H43 N2 2.9000 . . no H43 H39 2.5200 . . no H43 H34 2.5700 . 3_655 no H44 N3 2.5100 . . no H44 C23 3.0200 . . no H44 H23 2.2100 . . no H44 H38 2.5200 . . no H44 H41 2.4300 . . no H44 O1 2.0500 . 2_545 no H44 H4 2.4500 . 2_545 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H4 O2 0.8600 1.6300 2.479(2) 171.00 3_656 yes O1 H4 N2 0.8600 2.3000 2.967(2) 135.00 3_656 yes N4 H44 O1 0.8300 2.0500 2.861(3) 163.00 2_545 yes C11 H21 O1 0.9600 2.3400 2.971(3) 123.00 . yes # Attachment 'VAC5Pd4.CIF' data_vac5pd2 _database_code_depnum_ccdc_archive 'CCDC 648647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H50 N8 O4 Pd' _chemical_formula_weight 621.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3528(2) _cell_length_b 15.2183(2) _cell_length_c 16.3836(3) _cell_angle_alpha 111.7170(10) _cell_angle_beta 101.7720(10) _cell_angle_gamma 95.9320(10) _cell_volume 2301.78(7) _cell_formula_units_Z 3 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19223 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.39 _reflns_number_total 10302 _reflns_number_gt 8334 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.8781P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10302 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.5000 -0.5000 0.01788(5) Uani 1 2 d S . . O1A O -0.08845(13) 0.66441(10) -0.38332(8) 0.0232(3) Uani 1 1 d . . . H1AA H -0.1342 0.6150 -0.3842 0.035 Uiso 1 1 calc R . . O2A O 0.21000(13) 0.50438(11) -0.59686(9) 0.0292(4) Uani 1 1 d . . . N1A N -0.00399(15) 0.63760(11) -0.43804(10) 0.0187(4) Uani 1 1 d . . . N2A N 0.13589(15) 0.55982(12) -0.54234(10) 0.0208(4) Uani 1 1 d . . . N3A N 0.09271(16) 0.79751(12) -0.41369(11) 0.0242(4) Uani 1 1 d . . . H3AA H 0.1727 0.8308 -0.4049 0.029 Uiso 1 1 calc R . . N4A N 0.26255(16) 0.70985(13) -0.52210(11) 0.0278(4) Uani 1 1 d . . . H4AA H 0.2779 0.7716 -0.4866 0.033 Uiso 1 1 calc R . . C1A C 0.07847(18) 0.70069(14) -0.44936(11) 0.0196(5) Uani 1 1 d . . . C2A C 0.16634(18) 0.65333(14) -0.51001(11) 0.0204(5) Uani 1 1 d . . . C21A C 0.3454(2) 0.68230(18) -0.58655(14) 0.0360(6) Uani 1 1 d . . . H21A H 0.3653 0.6180 -0.5936 0.043 Uiso 1 1 calc R . . H21B H 0.4320 0.7290 -0.5611 0.043 Uiso 1 1 calc R . . C12A C -0.1382(2) 0.82469(17) -0.46161(16) 0.0362(6) Uani 1 1 d . . . H12A H -0.2044 0.8618 -0.4366 0.043 Uiso 1 1 calc R . . H12B H -0.1753 0.7555 -0.4805 0.043 Uiso 1 1 calc R . . C11A C -0.0100(2) 0.85308(16) -0.38801(14) 0.0298(5) Uani 1 1 d . . . H11A H 0.0272 0.9222 -0.3696 0.036 Uiso 1 1 calc R . . H11B H -0.0310 0.8456 -0.3343 0.036 Uiso 1 1 calc R . . C13A C -0.1215(3) 0.84138(19) -0.54421(16) 0.0450(7) Uani 1 1 d . . . H13A H -0.0614 0.8001 -0.5725 0.054 Uiso 1 1 calc R . . H13B H -0.0780 0.9095 -0.5250 0.054 Uiso 1 1 calc R . . C23A C 0.3726(3) 0.6620(2) -0.74174(16) 0.0517(8) Uani 1 1 d . . . H23A H 0.4573 0.7106 -0.7103 0.062 Uiso 1 1 calc R . . H23B H 0.3959 0.5977 -0.7535 0.062 Uiso 1 1 calc R . . C22A C 0.2810(3) 0.6789(2) -0.67720(17) 0.0585(8) Uani 1 1 d . . . H22A H 0.2508 0.7405 -0.6693 0.070 Uiso 1 1 calc R . . H22B H 0.2001 0.6266 -0.7057 0.070 Uiso 1 1 calc R . . C14A C -0.2541(3) 0.8194(2) -0.61386(18) 0.0536(8) Uani 1 1 d . . . H14A H -0.2962 0.7509 -0.6337 0.064 Uiso 1 1 calc R . . H14B H -0.3147 0.8595 -0.5847 0.064 Uiso 1 1 calc R . . C15A C -0.2417(4) 0.8374(2) -0.6952(2) 0.0851(12) Uani 1 1 d . . . H15A H -0.3311 0.8225 -0.7369 0.128 Uiso 1 1 calc R . . H15B H -0.1845 0.7962 -0.7259 0.128 Uiso 1 1 calc R . . H15C H -0.2011 0.9053 -0.6764 0.128 Uiso 1 1 calc R . . C24A C 0.3177(4) 0.6666(3) -0.8293(2) 0.0819(11) Uani 1 1 d . . . H24A H 0.2978 0.7317 -0.8176 0.098 Uiso 1 1 calc R . . H24B H 0.2313 0.6197 -0.8598 0.098 Uiso 1 1 calc R . . C25A C 0.4060(4) 0.6464(3) -0.8935(2) 0.1015(15) Uani 1 1 d . . . H25A H 0.3613 0.6527 -0.9493 0.152 Uiso 1 1 calc R . . H25B H 0.4227 0.5807 -0.9086 0.152 Uiso 1 1 calc R . . H25C H 0.4918 0.6926 -0.8646 0.152 Uiso 1 1 calc R . . Pd2 Pd 0.0000 0.0000 0.0000 0.01769(5) Uani 1 2 d S . . O1B O -0.22628(12) 0.10245(11) 0.03098(9) 0.0273(4) Uani 1 1 d . . . H1BA H -0.2559 0.0586 -0.0216 0.041 Uiso 1 1 calc R . . O2B O 0.26266(12) 0.04673(10) 0.12694(8) 0.0210(3) Uani 1 1 d . . . N1B N -0.09417(15) 0.09720(12) 0.06780(10) 0.0208(4) Uani 1 1 d . . . N2B N 0.14374(15) 0.07359(12) 0.11335(10) 0.0196(4) Uani 1 1 d . . . N3B N -0.06340(16) 0.23695(13) 0.20467(11) 0.0260(4) Uani 1 1 d . . . H3BA H -0.0020 0.2723 0.2558 0.031 Uiso 1 1 calc R . . N4B N 0.20518(15) 0.20467(12) 0.25650(10) 0.0227(4) Uani 1 1 d . . . H4BA H 0.1891 0.2073 0.3080 0.027 Uiso 1 1 calc R . . C1B C -0.02644(18) 0.16231(14) 0.14734(11) 0.0183(4) Uani 1 1 d . . . C2B C 0.11493(18) 0.14676(14) 0.17468(11) 0.0197(4) Uani 1 1 d . . . C21B C 0.3287(2) 0.26207(16) 0.25712(14) 0.0302(5) Uani 1 1 d . . . H21C H 0.3060 0.3121 0.2346 0.036 Uiso 1 1 calc R . . H21D H 0.3763 0.2199 0.2165 0.036 Uiso 1 1 calc R . . C11B C -0.1935(2) 0.26841(16) 0.19400(14) 0.0303(6) Uani 1 1 d . . . H11C H -0.2103 0.2983 0.2548 0.036 Uiso 1 1 calc R . . H11D H -0.2659 0.2110 0.1569 0.036 Uiso 1 1 calc R . . C12B C -0.2009(2) 0.33916(18) 0.14989(16) 0.0390(6) Uani 1 1 d . . . H12C H -0.1948 0.3065 0.0865 0.047 Uiso 1 1 calc R . . H12D H -0.2901 0.3578 0.1471 0.047 Uiso 1 1 calc R . . C22B C 0.4189(2) 0.30958(18) 0.35380(16) 0.0376(6) Uani 1 1 d . . . H22C H 0.4430 0.2584 0.3743 0.045 Uiso 1 1 calc R . . H22D H 0.3672 0.3473 0.3941 0.045 Uiso 1 1 calc R . . C23B C 0.5481(3) 0.3761(2) 0.36516(19) 0.0499(8) Uani 1 1 d . . . H23C H 0.6035 0.3987 0.4287 0.060 Uiso 1 1 calc R . . H23D H 0.5997 0.3384 0.3247 0.060 Uiso 1 1 calc R . . C25B C 0.6582(3) 0.5370(2) 0.3764(2) 0.0610(9) Uani 1 1 d . . . H25D H 0.6374 0.5915 0.3613 0.092 Uiso 1 1 calc R . . H25E H 0.7246 0.5086 0.3453 0.092 Uiso 1 1 calc R . . H25F H 0.6950 0.5597 0.4424 0.092 Uiso 1 1 calc R . . C13B C -0.0937(3) 0.4295(2) 0.1971(2) 0.0572(9) Uani 1 1 d . . . H13C H -0.0044 0.4114 0.1983 0.069 Uiso 1 1 calc R . . H13D H -0.0981 0.4618 0.2609 0.069 Uiso 1 1 calc R . . C24B C 0.5276(3) 0.4597(2) 0.3450(3) 0.0757(10) Uani 1 1 d . . . H24C H 0.4601 0.4897 0.3752 0.091 Uiso 1 1 calc R . . H24D H 0.4904 0.4380 0.2785 0.091 Uiso 1 1 calc R . . C14B C -0.1073(4) 0.5013(2) 0.1510(3) 0.0755(11) Uani 1 1 d . . . H14C H -0.0253 0.5526 0.1784 0.091 Uiso 1 1 calc R . . H14D H -0.1126 0.4670 0.0856 0.091 Uiso 1 1 calc R . . C15B C -0.2272(5) 0.5470(3) 0.1597(3) 0.1045(14) Uani 1 1 d . . . H15D H -0.2300 0.5911 0.1286 0.157 Uiso 1 1 calc R . . H15E H -0.2213 0.5831 0.2242 0.157 Uiso 1 1 calc R . . H15F H -0.3091 0.4969 0.1318 0.157 Uiso 1 1 calc R . . Pd3 Pd 0.5000 1.0000 -0.5000 0.01719(5) Uani 1 2 d S . . O1C O 0.68929(12) 1.08827(10) -0.56964(8) 0.0219(3) Uani 1 1 d . . . H1CA H 0.7338 1.0865 -0.5215 0.033 Uiso 1 1 calc R . . O2C O 0.20690(12) 0.92996(10) -0.58195(9) 0.0267(3) Uani 1 1 d . . . N1C N 0.55797(15) 1.04626(11) -0.58738(10) 0.0193(4) Uani 1 1 d . . . N2C N 0.32674(15) 0.97139(12) -0.59085(10) 0.0198(4) Uani 1 1 d . . . N3C N 0.47425(16) 1.07186(12) -0.72288(10) 0.0246(4) Uani 1 1 d . . . H3CA H 0.3974 1.0704 -0.7587 0.030 Uiso 1 1 calc R . . N4C N 0.22489(16) 0.96541(13) -0.73642(10) 0.0273(4) Uani 1 1 d . . . H4CA H 0.2271 1.0006 -0.7685 0.033 Uiso 1 1 calc R . . C1C C 0.46427(18) 1.03978(14) -0.65765(11) 0.0188(4) Uani 1 1 d . . . C2C C 0.32815(18) 0.98896(14) -0.66238(12) 0.0201(5) Uani 1 1 d . . . C11C C 0.5953(2) 1.10888(16) -0.74239(13) 0.0284(5) Uani 1 1 d . . . H11E H 0.6584 1.1552 -0.6845 0.034 Uiso 1 1 calc R . . H11F H 0.5702 1.1444 -0.7812 0.034 Uiso 1 1 calc R . . C22C C 0.0613(2) 0.84291(17) -0.87099(14) 0.0325(6) Uani 1 1 d . . . H22E H 0.0248 0.8914 -0.8909 0.039 Uiso 1 1 calc R . . H22F H 0.1393 0.8281 -0.8963 0.039 Uiso 1 1 calc R . . C23C C -0.0456(2) 0.75188(17) -0.90955(14) 0.0343(6) Uani 1 1 d . . . H23E H -0.1220 0.7658 -0.8822 0.041 Uiso 1 1 calc R . . H23F H -0.0078 0.7022 -0.8922 0.041 Uiso 1 1 calc R . . C21C C 0.1089(2) 0.88587(17) -0.76804(13) 0.0304(5) Uani 1 1 d . . . H21E H 0.0349 0.9101 -0.7420 0.036 Uiso 1 1 calc R . . H21F H 0.1347 0.8355 -0.7469 0.036 Uiso 1 1 calc R . . C12C C 0.6661(2) 1.03076(17) -0.78959(14) 0.0332(6) Uani 1 1 d . . . H12E H 0.6927 0.9960 -0.7503 0.040 Uiso 1 1 calc R . . H12F H 0.7492 1.0610 -0.7977 0.040 Uiso 1 1 calc R . . C13C C 0.5798(2) 0.95876(18) -0.88174(15) 0.0367(6) Uani 1 1 d . . . H13E H 0.5501 0.9942 -0.9199 0.044 Uiso 1 1 calc R . . H13F H 0.4984 0.9270 -0.8731 0.044 Uiso 1 1 calc R . . C14C C 0.6504(3) 0.8814(2) -0.93248(16) 0.0441(7) Uani 1 1 d . . . H14E H 0.6781 0.8445 -0.8955 0.053 Uiso 1 1 calc R . . H14F H 0.7328 0.9127 -0.9406 0.053 Uiso 1 1 calc R . . C24C C -0.0974(3) 0.7119(2) -1.01272(16) 0.0491(8) Uani 1 1 d . . . H24E H -0.1407 0.7600 -1.0297 0.059 Uiso 1 1 calc R . . H24F H -0.0201 0.7023 -1.0398 0.059 Uiso 1 1 calc R . . C15C C 0.5610(3) 0.8120(2) -1.02550(17) 0.0558(9) Uani 1 1 d . . . H15G H 0.6104 0.7634 -1.0555 0.084 Uiso 1 1 calc R . . H15H H 0.5352 0.8480 -1.0630 0.084 Uiso 1 1 calc R . . H15I H 0.4800 0.7800 -1.0178 0.084 Uiso 1 1 calc R . . C25C C -0.1971(4) 0.6177(2) -1.0524(2) 0.0687(10) Uani 1 1 d . . . H25G H -0.2268 0.5958 -1.1187 0.103 Uiso 1 1 calc R . . H25H H -0.2750 0.6268 -1.0270 0.103 Uiso 1 1 calc R . . H25I H -0.1544 0.5691 -1.0373 0.103 Uiso 1 1 calc 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 Pd1 0.01728(8) 0.01851(10) 0.01606(8) 0.00487(7) 0.00632(7) 0.00001(8) O1A 0.0251(6) 0.0198(7) 0.0235(6) 0.0045(5) 0.0139(5) 0.0006(6) O2A 0.0282(6) 0.0290(8) 0.0317(6) 0.0065(6) 0.0208(5) 0.0067(6) N1A 0.0179(7) 0.0187(8) 0.0177(6) 0.0046(6) 0.0069(5) 0.0013(6) N2A 0.0220(7) 0.0204(8) 0.0204(6) 0.0060(6) 0.0112(6) 0.0032(7) N3A 0.0188(7) 0.0192(8) 0.0325(8) 0.0085(6) 0.0077(6) -0.0003(7) N4A 0.0273(8) 0.0254(9) 0.0335(7) 0.0120(7) 0.0157(6) 0.0011(7) C1A 0.0169(8) 0.0242(10) 0.0156(7) 0.0079(7) 0.0016(6) 0.0009(8) C2A 0.0191(8) 0.0265(10) 0.0158(7) 0.0102(7) 0.0029(6) 0.0024(8) C21A 0.0337(10) 0.0405(12) 0.0434(10) 0.0209(9) 0.0235(8) 0.0050(10) C12A 0.0276(10) 0.0315(11) 0.0530(12) 0.0201(9) 0.0112(9) 0.0080(9) C11A 0.0338(10) 0.0209(10) 0.0360(9) 0.0098(8) 0.0158(8) 0.0043(9) C13A 0.0446(13) 0.0398(13) 0.0477(12) 0.0228(10) -0.0002(11) 0.0000(11) C23A 0.0482(13) 0.0705(18) 0.0422(12) 0.0249(12) 0.0180(10) 0.0152(13) C22A 0.0708(16) 0.0771(18) 0.0403(12) 0.0273(12) 0.0227(11) 0.0373(15) C14A 0.0518(15) 0.0515(15) 0.0568(14) 0.0283(12) 0.0029(12) 0.0047(13) C15A 0.106(3) 0.0727(19) 0.0632(16) 0.0428(14) -0.0216(17) -0.013(2) C24A 0.096(2) 0.112(2) 0.0575(15) 0.0463(15) 0.0304(15) 0.039(2) C25A 0.092(2) 0.171(4) 0.0497(14) 0.0528(18) 0.0282(15) 0.005(3) Pd2 0.01728(9) 0.02179(10) 0.01327(7) 0.00673(7) 0.00230(7) 0.00539(8) O1B 0.0169(6) 0.0368(8) 0.0216(6) 0.0067(6) -0.0014(5) 0.0097(6) O2B 0.0167(6) 0.0279(7) 0.0174(5) 0.0085(5) 0.0012(5) 0.0082(5) N1B 0.0170(7) 0.0255(8) 0.0192(7) 0.0074(6) 0.0042(6) 0.0084(6) N2B 0.0175(7) 0.0243(8) 0.0171(6) 0.0097(6) 0.0023(5) 0.0043(6) N3B 0.0232(7) 0.0293(9) 0.0215(7) 0.0047(7) 0.0052(6) 0.0104(7) N4B 0.0199(7) 0.0280(9) 0.0156(6) 0.0057(6) 0.0038(6) -0.0012(7) C1B 0.0196(8) 0.0216(9) 0.0167(7) 0.0099(6) 0.0061(6) 0.0054(7) C2B 0.0204(8) 0.0234(9) 0.0162(7) 0.0085(7) 0.0059(6) 0.0030(8) C21B 0.0283(10) 0.0287(11) 0.0307(9) 0.0093(8) 0.0106(8) -0.0016(9) C11B 0.0241(9) 0.0353(12) 0.0290(9) 0.0074(9) 0.0093(8) 0.0120(9) C12B 0.0373(11) 0.0360(13) 0.0400(11) 0.0137(10) 0.0036(9) 0.0111(10) C22B 0.0302(11) 0.0325(13) 0.0364(11) 0.0033(10) 0.0037(9) -0.0013(10) C23B 0.0382(13) 0.0484(16) 0.0504(14) 0.0122(12) 0.0024(11) 0.0025(12) C25B 0.0533(16) 0.0527(16) 0.0773(17) 0.0350(13) 0.0092(14) -0.0066(14) C13B 0.0566(16) 0.0407(15) 0.0644(16) 0.0212(13) -0.0027(13) 0.0044(13) C24B 0.0509(16) 0.0743(19) 0.117(2) 0.0584(17) 0.0165(16) 0.0096(15) C14B 0.074(2) 0.0515(17) 0.099(2) 0.0415(15) 0.0019(18) 0.0014(17) C15B 0.153(4) 0.079(2) 0.125(2) 0.0682(18) 0.063(2) 0.046(2) Pd3 0.01513(8) 0.02062(10) 0.01576(8) 0.00971(7) 0.00135(7) -0.00052(8) O1C 0.0155(6) 0.0294(7) 0.0197(5) 0.0136(5) -0.0005(5) -0.0047(5) O2C 0.0146(6) 0.0401(8) 0.0272(6) 0.0191(5) 0.0031(5) -0.0041(6) N1C 0.0157(7) 0.0230(8) 0.0194(6) 0.0111(6) 0.0031(5) -0.0018(6) N2C 0.0144(7) 0.0246(8) 0.0212(6) 0.0121(6) 0.0029(5) -0.0008(6) N3C 0.0180(7) 0.0371(9) 0.0228(6) 0.0193(6) 0.0022(6) 0.0007(7) N4C 0.0205(8) 0.0367(9) 0.0252(7) 0.0208(6) -0.0032(6) -0.0060(7) C1C 0.0183(8) 0.0197(9) 0.0177(7) 0.0083(7) 0.0027(6) 0.0014(7) C2C 0.0182(8) 0.0207(9) 0.0196(8) 0.0077(7) 0.0030(7) 0.0022(7) C11C 0.0243(9) 0.0408(11) 0.0249(8) 0.0205(8) 0.0053(7) 0.0008(9) C22C 0.0295(10) 0.0367(12) 0.0275(9) 0.0154(8) -0.0002(8) -0.0038(9) C23C 0.0345(11) 0.0340(12) 0.0282(9) 0.0141(8) -0.0019(9) -0.0051(10) C21C 0.0227(9) 0.0383(12) 0.0280(9) 0.0164(8) 0.0007(8) -0.0030(9) C12C 0.0272(10) 0.0420(12) 0.0352(9) 0.0228(8) 0.0050(8) 0.0047(9) C13C 0.0323(11) 0.0459(13) 0.0331(10) 0.0178(9) 0.0070(9) 0.0092(10) C14C 0.0436(12) 0.0518(14) 0.0440(11) 0.0234(10) 0.0153(10) 0.0152(12) C24C 0.0568(15) 0.0450(15) 0.0291(11) 0.0085(10) 0.0000(11) -0.0131(13) C15C 0.0665(16) 0.0608(18) 0.0363(12) 0.0114(12) 0.0165(12) 0.0214(15) C25C 0.081(2) 0.0475(18) 0.0463(15) 0.0100(13) -0.0152(15) -0.0203(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1A 1.9693(16) . ? Pd1 N1A 1.9693(16) 2_564 ? Pd1 N2A 1.9723(16) . ? Pd1 N2A 1.9723(16) 2_564 ? O1A N1A 1.363(2) . ? O1A H1AA 0.8400 . ? O2A N2A 1.398(2) . ? N1A C1A 1.308(3) . ? N2A C2A 1.299(3) . ? N3A C1A 1.348(3) . ? N3A C11A 1.459(3) . ? N3A H3AA 0.8800 . ? N4A C2A 1.342(3) . ? N4A C21A 1.463(3) . ? N4A H4AA 0.8800 . ? C1A C2A 1.519(3) . ? C21A C22A 1.478(4) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C12A C11A 1.498(3) . ? C12A C13A 1.506(4) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C13A C14A 1.511(4) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C23A C24A 1.462(4) . ? C23A C22A 1.531(4) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C14A C15A 1.482(5) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C24A C25A 1.500(5) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? Pd2 N1B 1.9740(16) 2 ? Pd2 N1B 1.9740(16) . ? Pd2 N2B 1.9763(13) . ? Pd2 N2B 1.9763(13) 2 ? O1B N1B 1.401(2) . ? O1B H1BA 0.8400 . ? O2B N2B 1.339(2) . ? N1B C1B 1.304(2) . ? N2B C2B 1.304(2) . ? N3B C1B 1.329(2) . ? N3B C11B 1.474(3) . ? N3B H3BA 0.8800 . ? N4B C2B 1.376(2) . ? N4B C21B 1.468(3) . ? N4B H4BA 0.8800 . ? C1B C2B 1.510(3) . ? C21B C22B 1.521(3) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C11B C12B 1.502(4) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.507(4) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C22B C23B 1.526(4) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C23B C24B 1.453(5) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C25B C24B 1.555(4) . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C13B C14B 1.544(5) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C14B C15B 1.490(6) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? Pd3 N2C 1.9729(14) 2_674 ? Pd3 N2C 1.9729(14) . ? Pd3 N1C 1.9786(16) 2_674 ? Pd3 N1C 1.9786(16) . ? O1C N1C 1.3647(19) . ? O1C H1CA 0.8400 . ? O2C N2C 1.392(2) . ? N1C C1C 1.310(2) . ? N2C C2C 1.297(3) . ? N3C C1C 1.346(3) . ? N3C C11C 1.463(3) . ? N3C H3CA 0.8800 . ? N4C C2C 1.346(2) . ? N4C C21C 1.468(3) . ? N4C H4CA 0.8800 . ? C1C C2C 1.509(3) . ? C11C C12C 1.510(3) . ? C11C H11E 0.9900 . ? C11C H11F 0.9900 . ? C22C C23C 1.514(3) . ? C22C C21C 1.514(3) . ? C22C H22E 0.9900 . ? C22C H22F 0.9900 . ? C23C C24C 1.521(3) . ? C23C H23E 0.9900 . ? C23C H23F 0.9900 . ? C21C H21E 0.9900 . ? C21C H21F 0.9900 . ? C12C C13C 1.517(3) . ? C12C H12E 0.9900 . ? C12C H12F 0.9900 . ? C13C C14C 1.521(4) . ? C13C H13E 0.9900 . ? C13C H13F 0.9900 . ? C14C C15C 1.525(3) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C24C C25C 1.509(4) . ? C24C H24E 0.9900 . ? C24C H24F 0.9900 . ? C15C H15G 0.9800 . ? C15C H15H 0.9800 . ? C15C H15I 0.9800 . ? C25C H25G 0.9800 . ? C25C H25H 0.9800 . ? C25C H25I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Pd1 N1A 180.00(9) . 2_564 ? N1A Pd1 N2A 78.99(7) . . ? N1A Pd1 N2A 101.01(7) 2_564 . ? N1A Pd1 N2A 101.01(7) . 2_564 ? N1A Pd1 N2A 78.99(7) 2_564 2_564 ? N2A Pd1 N2A 180.000(1) . 2_564 ? N1A O1A H1AA 109.5 . . ? C1A N1A O1A 122.19(16) . . ? C1A N1A Pd1 118.02(13) . . ? O1A N1A Pd1 119.76(12) . . ? C2A N2A O2A 119.96(16) . . ? C2A N2A Pd1 118.31(13) . . ? O2A N2A Pd1 121.27(12) . . ? C1A N3A C11A 127.10(16) . . ? C1A N3A H3AA 116.4 . . ? C11A N3A H3AA 116.4 . . ? C2A N4A C21A 128.55(18) . . ? C2A N4A H4AA 115.7 . . ? C21A N4A H4AA 115.7 . . ? N1A C1A N3A 127.94(18) . . ? N1A C1A C2A 112.29(17) . . ? N3A C1A C2A 119.77(17) . . ? N2A C2A N4A 129.13(18) . . ? N2A C2A C1A 112.17(17) . . ? N4A C2A C1A 118.69(17) . . ? N4A C21A C22A 113.4(2) . . ? N4A C21A H21A 108.9 . . ? C22A C21A H21A 108.9 . . ? N4A C21A H21B 108.9 . . ? C22A C21A H21B 108.9 . . ? H21A C21A H21B 107.7 . . ? C11A C12A C13A 113.7(2) . . ? C11A C12A H12A 108.8 . . ? C13A C12A H12A 108.8 . . ? C11A C12A H12B 108.8 . . ? C13A C12A H12B 108.8 . . ? H12A C12A H12B 107.7 . . ? N3A C11A C12A 114.43(17) . . ? N3A C11A H11A 108.7 . . ? C12A C11A H11A 108.7 . . ? N3A C11A H11B 108.7 . . ? C12A C11A H11B 108.7 . . ? H11A C11A H11B 107.6 . . ? C12A C13A C14A 112.4(2) . . ? C12A C13A H13A 109.1 . . ? C14A C13A H13A 109.1 . . ? C12A C13A H13B 109.1 . . ? C14A C13A H13B 109.1 . . ? H13A C13A H13B 107.9 . . ? C24A C23A C22A 116.1(3) . . ? C24A C23A H23A 108.3 . . ? C22A C23A H23A 108.3 . . ? C24A C23A H23B 108.3 . . ? C22A C23A H23B 108.3 . . ? H23A C23A H23B 107.4 . . ? C21A C22A C23A 114.0(2) . . ? C21A C22A H22A 108.8 . . ? C23A C22A H22A 108.8 . . ? C21A C22A H22B 108.8 . . ? C23A C22A H22B 108.8 . . ? H22A C22A H22B 107.6 . . ? C15A C14A C13A 113.8(3) . . ? C15A C14A H14A 108.8 . . ? C13A C14A H14A 108.8 . . ? C15A C14A H14B 108.8 . . ? C13A C14A H14B 108.8 . . ? H14A C14A H14B 107.7 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C23A C24A C25A 115.7(3) . . ? C23A C24A H24A 108.3 . . ? C25A C24A H24A 108.3 . . ? C23A C24A H24B 108.3 . . ? C25A C24A H24B 108.3 . . ? H24A C24A H24B 107.4 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? N1B Pd2 N1B 180.00(14) 2 . ? N1B Pd2 N2B 100.46(6) 2 . ? N1B Pd2 N2B 79.54(6) . . ? N1B Pd2 N2B 79.54(6) 2 2 ? N1B Pd2 N2B 100.46(6) . 2 ? N2B Pd2 N2B 180.00(7) . 2 ? N1B O1B H1BA 109.5 . . ? C1B N1B O1B 119.50(16) . . ? C1B N1B Pd2 117.82(13) . . ? O1B N1B Pd2 122.53(10) . . ? C2B N2B O2B 122.24(14) . . ? C2B N2B Pd2 116.70(12) . . ? O2B N2B Pd2 121.01(11) . . ? C1B N3B C11B 128.68(15) . . ? C1B N3B H3BA 115.7 . . ? C11B N3B H3BA 115.7 . . ? C2B N4B C21B 119.34(16) . . ? C2B N4B H4BA 120.3 . . ? C21B N4B H4BA 120.3 . . ? N1B C1B N3B 129.96(17) . . ? N1B C1B C2B 112.08(16) . . ? N3B C1B C2B 117.97(14) . . ? N2B C2B N4B 123.07(17) . . ? N2B C2B C1B 113.81(14) . . ? N4B C2B C1B 123.12(16) . . ? N4B C21B C22B 109.14(18) . . ? N4B C21B H21C 109.9 . . ? C22B C21B H21C 109.9 . . ? N4B C21B H21D 109.9 . . ? C22B C21B H21D 109.9 . . ? H21C C21B H21D 108.3 . . ? N3B C11B C12B 113.87(19) . . ? N3B C11B H11C 108.8 . . ? C12B C11B H11C 108.8 . . ? N3B C11B H11D 108.8 . . ? C12B C11B H11D 108.8 . . ? H11C C11B H11D 107.7 . . ? C11B C12B C13B 115.0(2) . . ? C11B C12B H12C 108.5 . . ? C13B C12B H12C 108.5 . . ? C11B C12B H12D 108.5 . . ? C13B C12B H12D 108.5 . . ? H12C C12B H12D 107.5 . . ? C21B C22B C23B 114.6(2) . . ? C21B C22B H22C 108.6 . . ? C23B C22B H22C 108.6 . . ? C21B C22B H22D 108.6 . . ? C23B C22B H22D 108.6 . . ? H22C C22B H22D 107.6 . . ? C24B C23B C22B 114.6(2) . . ? C24B C23B H23C 108.6 . . ? C22B C23B H23C 108.6 . . ? C24B C23B H23D 108.6 . . ? C22B C23B H23D 108.6 . . ? H23C C23B H23D 107.6 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C12B C13B C14B 113.4(2) . . ? C12B C13B H13C 108.9 . . ? C14B C13B H13C 108.9 . . ? C12B C13B H13D 108.9 . . ? C14B C13B H13D 108.9 . . ? H13C C13B H13D 107.7 . . ? C23B C24B C25B 113.6(3) . . ? C23B C24B H24C 108.8 . . ? C25B C24B H24C 108.8 . . ? C23B C24B H24D 108.8 . . ? C25B C24B H24D 108.8 . . ? H24C C24B H24D 107.7 . . ? C15B C14B C13B 113.8(3) . . ? C15B C14B H14C 108.8 . . ? C13B C14B H14C 108.8 . . ? C15B C14B H14D 108.8 . . ? C13B C14B H14D 108.8 . . ? H14C C14B H14D 107.7 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2C Pd3 N2C 180.000(1) 2_674 . ? N2C Pd3 N1C 79.36(6) 2_674 2_674 ? N2C Pd3 N1C 100.64(6) . 2_674 ? N2C Pd3 N1C 100.64(6) 2_674 . ? N2C Pd3 N1C 79.36(6) . . ? N1C Pd3 N1C 180.000(1) 2_674 . ? N1C O1C H1CA 109.5 . . ? C1C N1C O1C 123.18(16) . . ? C1C N1C Pd3 117.04(13) . . ? O1C N1C Pd3 119.64(11) . . ? C2C N2C O2C 120.14(14) . . ? C2C N2C Pd3 117.61(12) . . ? O2C N2C Pd3 122.19(11) . . ? C1C N3C C11C 128.93(16) . . ? C1C N3C H3CA 115.5 . . ? C11C N3C H3CA 115.5 . . ? C2C N4C C21C 125.40(18) . . ? C2C N4C H4CA 117.3 . . ? C21C N4C H4CA 117.3 . . ? N1C C1C N3C 129.16(17) . . ? N1C C1C C2C 112.67(17) . . ? N3C C1C C2C 118.16(15) . . ? N2C C2C N4C 127.07(18) . . ? N2C C2C C1C 112.87(15) . . ? N4C C2C C1C 120.05(17) . . ? N3C C11C C12C 113.29(18) . . ? N3C C11C H11E 108.9 . . ? C12C C11C H11E 108.9 . . ? N3C C11C H11F 108.9 . . ? C12C C11C H11F 108.9 . . ? H11E C11C H11F 107.7 . . ? C23C C22C C21C 113.37(19) . . ? C23C C22C H22E 108.9 . . ? C21C C22C H22E 108.9 . . ? C23C C22C H22F 108.9 . . ? C21C C22C H22F 108.9 . . ? H22E C22C H22F 107.7 . . ? C22C C23C C24C 113.0(2) . . ? C22C C23C H23E 109.0 . . ? C24C C23C H23E 109.0 . . ? C22C C23C H23F 109.0 . . ? C24C C23C H23F 109.0 . . ? H23E C23C H23F 107.8 . . ? N4C C21C C22C 110.22(18) . . ? N4C C21C H21E 109.6 . . ? C22C C21C H21E 109.6 . . ? N4C C21C H21F 109.6 . . ? C22C C21C H21F 109.6 . . ? H21E C21C H21F 108.1 . . ? C11C C12C C13C 113.03(18) . . ? C11C C12C H12E 109.0 . . ? C13C C12C H12E 109.0 . . ? C11C C12C H12F 109.0 . . ? C13C C12C H12F 109.0 . . ? H12E C12C H12F 107.8 . . ? C12C C13C C14C 114.19(19) . . ? C12C C13C H13E 108.7 . . ? C14C C13C H13E 108.7 . . ? C12C C13C H13F 108.7 . . ? C14C C13C H13F 108.7 . . ? H13E C13C H13F 107.6 . . ? C13C C14C C15C 112.4(2) . . ? C13C C14C H14E 109.1 . . ? C15C C14C H14E 109.1 . . ? C13C C14C H14F 109.1 . . ? C15C C14C H14F 109.1 . . ? H14E C14C H14F 107.9 . . ? C25C C24C C23C 113.4(2) . . ? C25C C24C H24E 108.9 . . ? C23C C24C H24E 108.9 . . ? C25C C24C H24F 108.9 . . ? C23C C24C H24F 108.9 . . ? H24E C24C H24F 107.7 . . ? C14C C15C H15G 109.5 . . ? C14C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? C14C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? C24C C25C H25G 109.5 . . ? C24C C25C H25H 109.5 . . ? H25G C25C H25H 109.5 . . ? C24C C25C H25I 109.5 . . ? H25G C25C H25I 109.5 . . ? H25H C25C H25I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.664 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.100 # Attachment 'VAC7Pd4.cif' data_VAC7Pd4 _database_code_depnum_ccdc_archive 'CCDC 648648' _audit_creation_date 07-07-10 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'va252 in space group I4(1)/a' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 17.4724(4) _cell_length_b 17.4724(4) _cell_length_c 26.4145(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8063.9(4) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 3/4-y,1/4+x,1/4+z 3 1/2-x,-y,1/2+z 4 3/4+y,3/4-x,3/4+z 5 -x,-y,-z 6 1/4+y,3/4-x,3/4-z 7 1/2+x,y,1/2-z 8 1/4-y,1/4+x,1/4-z 9 1/2+x,1/2+y,1/2+z 10 1/4-y,3/4+x,3/4+z 11 -x,1/2-y,z 12 1/4+y,1/4-x,1/4+z 13 1/2-x,1/2-y,1/2-z 14 3/4+y,1/4-x,1/4-z 15 x,1/2+y,-z 16 3/4-y,3/4+x,3/4-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' 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' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C32 H66 N8 O4 Pd1 # Dc = 1.21 Fooo = 3136.00 Mu = 5.02 M = 366.66 # Found Formula = C32 H66 N8 O4 Pd1 # Dc = 1.21 FOOO = 3136.00 Mu = 5.02 M = 366.66 _chemical_formula_sum 'C32 H66 N8 O4 Pd1' _chemical_formula_moiety 'C32 H66 N8 O4 Pd1' _chemical_compound_source ? _chemical_formula_weight 733.33 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 130 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.502 # Sheldrick geometric approximatio 0.90 0.93 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 130 _diffrn_reflns_number 6835 _reflns_number_total 4591 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections with Friedels Law is 4591 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4618 _diffrn_reflns_theta_min 1.397 _diffrn_reflns_theta_max 27.471 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.098 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -15 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.49 _refine_diff_density_max 1.38 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2889 _refine_ls_number_restraints 0 _refine_ls_number_parameters 205 _oxford_refine_ls_R_factor_ref 0.0471 _refine_ls_wR_factor_ref 0.0465 _refine_ls_goodness_of_fit_ref 1.1258 _refine_ls_shift/su_max 0.000312 # The values computed from all data _oxford_reflns_number_all 4573 _refine_ls_R_factor_all 0.0967 _refine_ls_wR_factor_all 0.0725 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2889 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_gt 0.0465 # 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: 0.460 0.147 0.248 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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 Pd1 Pd 0.7500 0.2500 0.7500 0.0272 1.0000 Uani S . . . . . . N1 N 0.72959(19) 0.32757(18) 0.69703(12) 0.0325 1.0000 Uani . . . . . . . O1 O 0.68606(18) 0.39270(16) 0.70663(10) 0.0424 1.0000 Uani . . . . . . . H4 H 0.6664 0.3828 0.7338 0.0660 1.0000 Uiso R . . . . . . C1 C 0.7745(2) 0.3253(2) 0.65759(13) 0.0297 1.0000 Uani . . . . . . . N3 N 0.78504(19) 0.37803(19) 0.62139(12) 0.0340 1.0000 Uani . . . . . . . C11 C 0.7478(3) 0.4532(2) 0.61679(16) 0.0390 1.0000 Uani . . . . . . . C12 C 0.6719(3) 0.4488(3) 0.58934(16) 0.0454 1.0000 Uani . . . . . . . C13 C 0.6806(3) 0.4291(3) 0.53338(18) 0.0540 1.0000 Uani . . . . . . . C14 C 0.6064(3) 0.4231(4) 0.5046(2) 0.0646 1.0000 Uani . . . . . . . C15 C 0.6181(3) 0.4152(4) 0.4465(2) 0.0655 1.0000 Uani . . . . . . . C16 C 0.5460(4) 0.4065(5) 0.4176(2) 0.0922 1.0000 Uani . . . . . . . C17 C 0.5580(4) 0.4016(4) 0.3613(2) 0.0842 1.0000 Uani . . . . . . . H14 H 0.5095 0.3975 0.3443 0.1291 1.0000 Uiso R . . . . . . H15 H 0.5844 0.4467 0.3495 0.1289 1.0000 Uiso R . . . . . . H16 H 0.5886 0.3572 0.3534 0.1289 1.0000 Uiso R . . . . . . H17 H 0.5214 0.3595 0.4293 0.1112 1.0000 Uiso R . . . . . . H18 H 0.5132 0.4504 0.4249 0.1111 1.0000 Uiso R . . . . . . H19 H 0.6499 0.3706 0.4404 0.0801 1.0000 Uiso R . . . . . . H20 H 0.6439 0.4606 0.4341 0.0801 1.0000 Uiso R . . . . . . H21 H 0.5779 0.3788 0.5174 0.0799 1.0000 Uiso R . . . . . . H22 H 0.5769 0.4690 0.5115 0.0798 1.0000 Uiso R . . . . . . H23 H 0.7061 0.3797 0.5314 0.0659 1.0000 Uiso R . . . . . . H24 H 0.7126 0.4677 0.5174 0.0662 1.0000 Uiso R . . . . . . H25 H 0.6465 0.4982 0.5917 0.0581 1.0000 Uiso R . . . . . . H26 H 0.6401 0.4099 0.6056 0.0579 1.0000 Uiso R . . . . . . H27 H 0.7402 0.4749 0.6503 0.0489 1.0000 Uiso R . . . . . . H28 H 0.7817 0.4856 0.5975 0.0489 1.0000 Uiso R . . . . . . H29 H 0.8175 0.3670 0.5986 0.0421 1.0000 Uiso R . . . . . . C2 C 0.8206(2) 0.2533(2) 0.65505(13) 0.0287 1.0000 Uani . . . . . . . N2 N 0.81615(18) 0.21125(18) 0.69567(11) 0.0291 1.0000 Uani . . . . . . . O2 O 0.85711(16) 0.14794(15) 0.70129(10) 0.0343 1.0000 Uani . . . . . . . N4 N 0.86915(18) 0.23845(18) 0.61463(11) 0.0308 1.0000 Uani . . . . . . . C21 C 0.8333(2) 0.2170(2) 0.56578(13) 0.0345 1.0000 Uani . . . . . . . C22 C 0.8915(2) 0.2099(2) 0.52377(14) 0.0351 1.0000 Uani . . . . . . . C23 C 0.8560(3) 0.1850(3) 0.47409(15) 0.0492 1.0000 Uani . . . . . . . C24 C 0.9130(3) 0.1771(3) 0.43147(15) 0.0487 1.0000 Uani . . . . . . . C25 C 0.8814(3) 0.1544(3) 0.38034(16) 0.0548 1.0000 Uani . . . . . . . C26 C 0.9405(4) 0.1420(4) 0.33965(18) 0.0710 1.0000 Uani . . . . . . . C27 C 0.9077(5) 0.1247(4) 0.28790(18) 0.0843 1.0000 Uani . . . . . . . H41 H 0.9481 0.1208 0.2637 0.1240 1.0000 Uiso R . . . . . . H42 H 0.8804 0.0769 0.2889 0.1239 1.0000 Uiso R . . . . . . H43 H 0.8735 0.1645 0.2780 0.1239 1.0000 Uiso R . . . . . . H44 H 0.9698 0.1889 0.3370 0.0869 1.0000 Uiso R . . . . . . H45 H 0.9742 0.1004 0.3496 0.0873 1.0000 Uiso R . . . . . . H46 H 0.8534 0.1074 0.3844 0.0654 1.0000 Uiso R . . . . . . H47 H 0.8467 0.1944 0.3693 0.0655 1.0000 Uiso R . . . . . . H48 H 0.9381 0.2264 0.4276 0.0583 1.0000 Uiso R . . . . . . H49 H 0.9506 0.1398 0.4415 0.0584 1.0000 Uiso R . . . . . . H50 H 0.8321 0.1356 0.4792 0.0593 1.0000 Uiso R . . . . . . H51 H 0.8176 0.2217 0.4636 0.0592 1.0000 Uiso R . . . . . . H52 H 0.9301 0.1726 0.5339 0.0420 1.0000 Uiso R . . . . . . H53 H 0.9153 0.2597 0.5197 0.0422 1.0000 Uiso R . . . . . . H54 H 0.8074 0.1682 0.5699 0.0420 1.0000 Uiso R . . . . . . H55 H 0.7962 0.2560 0.5565 0.0419 1.0000 Uiso R . . . . . . H56 H 0.9165 0.2393 0.6182 0.0393 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 Pd1 0.0332(2) 0.0282(2) 0.02026(16) -0.00001(16) 0.00473(16) 0.00222(19) N1 0.0386(19) 0.0315(17) 0.0273(15) 0.0027(13) 0.0063(14) 0.0084(14) O1 0.0536(18) 0.0388(16) 0.0348(15) 0.0051(12) 0.0169(13) 0.0194(14) C1 0.032(2) 0.034(2) 0.0230(17) 0.0001(15) 0.0023(14) -0.0030(16) N3 0.0377(19) 0.0381(19) 0.0261(16) 0.0050(13) 0.0067(13) 0.0054(15) C11 0.050(3) 0.029(2) 0.037(2) 0.0053(17) 0.0070(18) 0.0049(19) C12 0.047(3) 0.052(3) 0.037(2) 0.007(2) 0.0028(19) 0.013(2) C13 0.053(3) 0.067(3) 0.042(2) 0.003(2) -0.002(2) 0.020(3) C14 0.051(3) 0.092(4) 0.050(3) 0.006(3) -0.007(2) 0.008(3) C15 0.057(3) 0.083(4) 0.056(3) -0.005(3) -0.004(3) 0.006(3) C16 0.072(4) 0.139(7) 0.065(4) 0.016(4) -0.018(3) 0.004(4) C17 0.091(5) 0.104(5) 0.057(4) 0.001(3) -0.014(3) 0.005(4) C2 0.032(2) 0.033(2) 0.0211(16) -0.0006(14) 0.0011(14) -0.0029(16) N2 0.0322(17) 0.0292(17) 0.0260(15) -0.0001(12) 0.0042(13) 0.0019(13) O2 0.0433(16) 0.0321(15) 0.0275(13) 0.0006(11) 0.0083(12) 0.0098(12) N4 0.0293(17) 0.0398(19) 0.0235(15) 0.0004(13) 0.0044(12) -0.0036(14) C21 0.039(2) 0.041(2) 0.0239(18) -0.0037(16) 0.0023(16) -0.0031(18) C22 0.041(2) 0.041(2) 0.0235(18) 0.0003(16) 0.0031(16) 0.0062(18) C23 0.057(3) 0.067(3) 0.023(2) -0.0053(19) 0.0042(19) -0.012(2) C24 0.056(3) 0.059(3) 0.031(2) -0.007(2) 0.0050(19) 0.007(2) C25 0.080(4) 0.057(3) 0.027(2) -0.006(2) 0.007(2) -0.003(3) C26 0.106(5) 0.077(4) 0.030(2) -0.009(2) 0.015(3) 0.004(4) C27 0.154(7) 0.071(4) 0.028(2) -0.004(2) 0.009(3) 0.027(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.06788(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.980(3) . . yes Pd1 N2 1.963(3) . . yes Pd1 N1 1.980(3) . 13_656 yes Pd1 N2 1.963(3) . 13_656 yes O1 N1 1.392(4) . . yes O2 N2 1.326(4) . . yes O1 H4 0.8100 . . no N1 C1 1.305(5) . . yes N2 C2 1.303(5) . . yes N3 C1 1.341(5) . . yes N3 C11 1.471(5) . . yes N4 C21 1.483(5) . . yes N4 C2 1.388(5) . . yes N3 H29 0.8500 . . no N4 H56 0.8300 . . no C1 C2 1.495(5) . . no C11 C12 1.513(7) . . no C12 C13 1.525(6) . . no C13 C14 1.507(7) . . no C14 C15 1.554(7) . . no C15 C16 1.481(8) . . no C16 C17 1.504(8) . . no C21 C22 1.510(5) . . no C22 C23 1.515(6) . . no C23 C24 1.509(6) . . no C24 C25 1.512(6) . . no C25 C26 1.506(8) . . no C26 C27 1.513(8) . . no C11 H27 0.9700 . . no C11 H28 0.9600 . . no C12 H25 0.9700 . . no C12 H26 0.9800 . . no C13 H23 0.9700 . . no C13 H24 0.9700 . . no C14 H21 0.9800 . . no C14 H22 0.9700 . . no C15 H19 0.9700 . . no C15 H20 0.9700 . . no C16 H17 0.9800 . . no C16 H18 0.9800 . . no C17 H14 0.9600 . . no C17 H15 0.9600 . . no C17 H16 0.9700 . . no C21 H54 0.9700 . . no C21 H55 0.9700 . . no C22 H52 0.9800 . . no C22 H53 0.9700 . . no C23 H50 0.9700 . . no C23 H51 0.9700 . . no C24 H48 0.9700 . . no C24 H49 0.9600 . . no C25 H46 0.9600 . . no C25 H47 0.9700 . . no C26 H44 0.9700 . . no C26 H45 0.9700 . . no C27 H41 0.9500 . . no C27 H42 0.9600 . . no C27 H43 0.9500 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 79.95(13) . . . yes N1 Pd1 N1 180.00 . . 13_656 yes N1 Pd1 N2 100.05(13) . . 13_656 yes N1 Pd1 N2 100.05(13) 13_656 . . yes N2 Pd1 N2 180.00 . . 13_656 yes N1 Pd1 N2 79.95(13) 13_656 . 13_656 yes N1 O1 H4 103.00 . . . no Pd1 N1 O1 122.0(2) . . . yes O1 N1 C1 119.9(3) . . . yes Pd1 N1 C1 115.8(3) . . . yes Pd1 N2 O2 121.6(2) . . . yes O2 N2 C2 122.0(3) . . . yes Pd1 N2 C2 116.3(2) . . . yes C1 N3 C11 127.7(3) . . . yes C2 N4 C21 117.3(3) . . . yes C1 N3 H29 116.00 . . . no C11 N3 H29 116.00 . . . no C21 N4 H56 122.00 . . . no C2 N4 H56 121.00 . . . no N1 C1 C2 112.7(3) . . . yes N3 C1 C2 118.2(3) . . . yes N1 C1 N3 129.1(3) . . . yes N2 C2 N4 124.4(3) . . . yes N2 C2 C1 113.9(3) . . . yes N4 C2 C1 121.4(3) . . . yes N3 C11 C12 112.5(3) . . . yes C11 C12 C13 112.9(4) . . . no C12 C13 C14 114.8(4) . . . no C13 C14 C15 113.0(4) . . . no C14 C15 C16 114.0(4) . . . no C15 C16 C17 113.4(5) . . . no N4 C21 C22 112.1(3) . . . yes C21 C22 C23 112.6(3) . . . no C22 C23 C24 113.7(4) . . . no C23 C24 C25 116.7(4) . . . no C24 C25 C26 115.1(5) . . . no C25 C26 C27 114.5(6) . . . no N3 C11 H27 109.00 . . . no N3 C11 H28 107.00 . . . no C12 C11 H27 110.00 . . . no C12 C11 H28 108.00 . . . no H27 C11 H28 110.00 . . . no C11 C12 H25 109.00 . . . no C11 C12 H26 109.00 . . . no C13 C12 H25 108.00 . . . no C13 C12 H26 109.00 . . . no H25 C12 H26 109.00 . . . no C12 C13 H23 107.00 . . . no C12 C13 H24 109.00 . . . no C14 C13 H23 108.00 . . . no C14 C13 H24 109.00 . . . no H23 C13 H24 109.00 . . . no C13 C14 H21 109.00 . . . no C13 C14 H22 108.00 . . . no C15 C14 H21 110.00 . . . no C15 C14 H22 109.00 . . . no H21 C14 H22 109.00 . . . no C14 C15 H19 108.00 . . . no C14 C15 H20 109.00 . . . no C16 C15 H19 109.00 . . . no C16 C15 H20 108.00 . . . no H19 C15 H20 110.00 . . . no C15 C16 H17 107.00 . . . no C15 C16 H18 108.00 . . . no C17 C16 H17 109.00 . . . no C17 C16 H18 109.00 . . . no H17 C16 H18 110.00 . . . no C16 C17 H14 110.00 . . . no C16 C17 H15 110.00 . . . no C16 C17 H16 110.00 . . . no H14 C17 H15 109.00 . . . no H14 C17 H16 109.00 . . . no H15 C17 H16 109.00 . . . no N4 C21 H54 109.00 . . . no N4 C21 H55 109.00 . . . no C22 C21 H54 109.00 . . . no C22 C21 H55 109.00 . . . no H54 C21 H55 109.00 . . . no C21 C22 H52 109.00 . . . no C21 C22 H53 107.00 . . . no C23 C22 H52 109.00 . . . no C23 C22 H53 110.00 . . . no H52 C22 H53 109.00 . . . no C22 C23 H50 108.00 . . . no C22 C23 H51 110.00 . . . no C24 C23 H50 108.00 . . . no C24 C23 H51 108.00 . . . no H50 C23 H51 109.00 . . . no C23 C24 H48 107.00 . . . no C23 C24 H49 108.00 . . . no C25 C24 H48 108.00 . . . no C25 C24 H49 109.00 . . . no H48 C24 H49 109.00 . . . no C24 C25 H46 108.00 . . . no C24 C25 H47 108.00 . . . no C26 C25 H46 108.00 . . . no C26 C25 H47 109.00 . . . no H46 C25 H47 109.00 . . . no C25 C26 H44 107.00 . . . no C25 C26 H45 109.00 . . . no C27 C26 H44 108.00 . . . no C27 C26 H45 109.00 . . . no H44 C26 H45 109.00 . . . no C26 C27 H41 110.00 . . . no C26 C27 H42 110.00 . . . no C26 C27 H43 110.00 . . . no H41 C27 H42 109.00 . . . no H41 C27 H43 109.00 . . . no H42 C27 H43 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 N1 O1 -172.9(3) . . . . no N2 Pd1 N1 C1 -10.3(3) . . . . no N2 Pd1 N1 O1 7.1(3) 13_656 . . . no N2 Pd1 N1 C1 169.7(3) 13_656 . . . no N1 Pd1 N2 O2 -178.8(3) . . . . no N1 Pd1 N2 C2 4.7(3) . . . . no N1 Pd1 N2 O2 1.2(3) 13_656 . . . no N1 Pd1 N2 C2 -175.3(3) 13_656 . . . no Pd1 N1 C1 N3 -165.1(3) . . . . no Pd1 N1 C1 C2 13.3(4) . . . . no O1 N1 C1 N3 -2.2(6) . . . . no O1 N1 C1 C2 176.2(3) . . . . no Pd1 N2 C2 N4 174.4(3) . . . . no Pd1 N2 C2 C1 0.8(4) . . . . no O2 N2 C2 N4 -2.0(5) . . . . no O2 N2 C2 C1 -175.6(3) . . . . no C11 N3 C1 N1 -0.2(6) . . . . no C11 N3 C1 C2 -178.5(4) . . . . no C1 N3 C11 C12 -86.3(5) . . . . no C21 N4 C2 N2 113.3(4) . . . . no C21 N4 C2 C1 -73.6(4) . . . . no C2 N4 C21 C22 174.4(3) . . . . no N1 C1 C2 N2 -9.3(5) . . . . no N1 C1 C2 N4 176.9(3) . . . . no N3 C1 C2 N2 169.3(3) . . . . no N3 C1 C2 N4 -4.5(5) . . . . no N3 C11 C12 C13 -68.4(5) . . . . no C11 C12 C13 C14 179.3(4) . . . . no C12 C13 C14 C15 171.3(5) . . . . no C13 C14 C15 C16 178.0(6) . . . . no C14 C15 C16 C17 178.0(6) . . . . no N4 C21 C22 C23 177.8(3) . . . . no C21 C22 C23 C24 -179.7(4) . . . . no C22 C23 C24 C25 -178.5(4) . . . . no C23 C24 C25 C26 -176.1(5) . . . . no C24 C25 C26 C27 -176.0(5) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd1 C22 4.176(4) . 2_545 no Pd1 C23 4.153(5) . 2_545 no Pd1 C24 3.894(5) . 2_545 no Pd1 C23 4.153(5) . 14_566 no Pd1 C24 3.894(5) . 14_566 no Pd1 C22 4.176(4) . 14_566 no Pd1 H49 3.0200 . 2_545 no Pd1 H52 3.3700 . 2_545 no Pd1 H49 3.0200 . 14_566 no Pd1 H52 3.3700 . 14_566 no O1 N3 2.851(4) . . no O1 C11 2.813(5) . . no O1 C12 3.259(5) . . no O1 N2 3.156(4) . 13_656 no O1 O2 2.644(4) . 13_656 no O2 C11 3.351(5) . 8_646 no O2 N1 3.113(4) . 13_656 no O2 N4 2.790(4) . . no O2 O1 2.644(4) . 13_656 no O2 N3 2.765(4) . 8_646 no O2 N4 3.251(4) . 8_646 no O2 C21 3.305(4) . 8_646 no O2 C22 3.266(4) . 8_646 no O1 H27 2.2700 . . no O1 H26 2.8000 . . no O2 H56 2.9100 . . no O2 H53 2.4700 . 8_646 no O2 H28 2.9000 . 8_646 no O2 H29 1.9800 . 8_646 no O2 H4 1.8400 . 13_656 no N1 N2 2.534(4) . . no N1 C2 2.333(5) . . no N1 O2 3.113(4) . 13_656 no N1 N2 3.022(4) . 13_656 no N2 N1 2.534(4) . . no N2 N1 3.022(4) . 13_656 no N2 C1 2.348(5) . . no N2 O1 3.156(4) . 13_656 no N3 O2 2.765(4) . 14_566 no N3 N4 2.853(5) . . no N3 C21 3.284(5) . . no N3 O1 2.851(4) . . no N4 O2 2.790(4) . . no N4 N4 3.292(4) . 14_566 no N4 N4 3.292(4) . 8_646 no N4 O2 3.251(4) . 14_566 no N4 N3 2.853(5) . . no N1 H27 2.8600 . . no N2 H52 2.7100 . 14_566 no N2 H4 2.5000 . 13_656 no N3 H55 2.7400 . . no N3 H23 2.7500 . . no N4 H56 2.8100 . 8_646 no N4 H29 2.4600 . . no N4 H56 2.7100 . 14_566 no C2 C22 3.583(5) . 14_566 no C11 O1 2.813(5) . . no C11 O2 3.351(5) . 14_566 no C12 O1 3.259(5) . . no C21 O2 3.305(4) . 14_566 no C21 N3 3.284(5) . . no C22 O2 3.266(4) . 14_566 no C22 Pd1 4.176(4) . 8_646 no C22 C2 3.583(5) . 8_646 no C22 Pd1 4.176(4) . 4_554 no C23 Pd1 4.153(5) . 4_554 no C23 Pd1 4.153(5) . 8_646 no C24 Pd1 3.894(5) . 8_646 no C24 Pd1 3.894(5) . 4_554 no C1 H52 3.0200 . 14_566 no C1 H26 3.1000 . . no C1 H55 2.9600 . . no C2 H52 2.6700 . 14_566 no C16 H16 2.9800 . 16_545 no C21 H29 2.7700 . . no H4 O2 1.8400 . 13_656 no H4 N2 2.5000 . 13_656 no H14 H19 2.4500 . 16_545 no H15 H20 2.4800 . . no H16 H19 2.5500 . . no H16 C16 2.9800 . 6_555 no H16 H17 2.4300 . 6_555 no H17 H21 2.5500 . . no H17 H16 2.4300 . 16_545 no H18 H22 2.5600 . . no H19 H16 2.5500 . . no H19 H14 2.4500 . 6_555 no H20 H15 2.4800 . . no H20 H24 2.5100 . . no H20 H27 2.5100 . 10_644 no H21 H17 2.5500 . . no H22 H18 2.5600 . . no H22 H25 2.5000 . . no H23 N3 2.7500 . . no H24 H20 2.5100 . . no H24 H28 2.4600 . . no H25 H22 2.5000 . . no H26 O1 2.8000 . . no H26 C1 3.1000 . . no H27 O1 2.2700 . . no H27 N1 2.8600 . . no H27 H20 2.5100 . 12_565 no H28 H24 2.4600 . . no H28 O2 2.9000 . 14_566 no H28 H46 2.5200 . 15_556 no H29 N4 2.4600 . . no H29 C21 2.7700 . . no H29 H55 2.2700 . . no H29 O2 1.9800 . 14_566 no H42 H54 2.5700 . 4_554 no H43 H47 2.5100 . . no H44 H48 2.5400 . . no H44 H44 2.3800 . 11_755 no H45 H49 2.5600 . . no H46 H50 2.5800 . . no H46 H28 2.5200 . 15_546 no H47 H43 2.5100 . . no H47 H51 2.5900 . . no H48 H44 2.5400 . . no H48 H53 2.5300 . . no H48 H48 2.3100 . 11_755 no H49 H45 2.5600 . . no H49 H52 2.5300 . . no H49 Pd1 3.0200 . 4_554 no H49 Pd1 3.0200 . 8_646 no H50 H46 2.5800 . . no H50 H54 2.5000 . . no H51 H47 2.5900 . . no H51 H55 2.5500 . . no H52 H49 2.5300 . . no H52 H56 2.5200 . . no H52 Pd1 3.3700 . 4_554 no H52 Pd1 3.3700 . 8_646 no H52 N2 2.7100 . 8_646 no H52 C1 3.0200 . 8_646 no H52 C2 2.6700 . 8_646 no H53 H48 2.5300 . . no H53 O2 2.4700 . 14_566 no H54 H50 2.5000 . . no H54 H42 2.5700 . 2_545 no H55 N3 2.7400 . . no H55 C1 2.9600 . . no H55 H29 2.2700 . . no H55 H51 2.5500 . . no H56 O2 2.9100 . . no H56 H52 2.5200 . . no H56 N4 2.7100 . 8_646 no H56 H56 2.1100 . 8_646 no H56 N4 2.8100 . 14_566 no H56 H56 2.1100 . 14_566 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H4 O2 0.8100 1.8400 2.644(4) 167.00 13_656 yes N3 H29 O2 0.8500 1.9800 2.765(4) 153.00 14_566 yes C11 H27 O1 0.9700 2.2700 2.813(5) 114.00 . yes C22 H53 O2 0.9700 2.4700 3.266(4) 139.00 14_566 yes # Attachment 'VAC8Pd4.cif' data_VAC8Pd4 _database_code_depnum_ccdc_archive 'CCDC 648649' _audit_creation_date 07-07-13 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title va402 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 18.0572(4) _cell_length_b 18.0572(4) _cell_length_c 26.8507(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8755.0(4) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 3/4-y,1/4+x,1/4+z 3 1/2-x,-y,1/2+z 4 3/4+y,3/4-x,3/4+z 5 -x,-y,-z 6 1/4+y,3/4-x,3/4-z 7 1/2+x,y,1/2-z 8 1/4-y,1/4+x,1/4-z 9 1/2+x,1/2+y,1/2+z 10 1/4-y,3/4+x,3/4+z 11 -x,1/2-y,z 12 1/4+y,1/4-x,1/4+z 13 1/2-x,1/2-y,1/2-z 14 3/4+y,1/4-x,1/4-z 15 x,1/2+y,-z 16 3/4-y,3/4+x,3/4-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' 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' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 16 # Given Formula = C288 H592 N64 O40 Pd8 # Dc = 19.55 Fooo = 3392.00 Mu = 75.14 M = 6443.48 # Found Formula = C18 H37 N4 O2 Pd0.50 # Dc = 1.20 FOOO = 3392.00 Mu = 4.67 M = 394.72 _chemical_formula_sum 'C18 H37 N4 O2 Pd0.50' _chemical_formula_moiety 'C18 H37 N4 O2 Pd0.50' _chemical_compound_source ? _chemical_formula_weight 394.72 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_max 0.2 _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.467 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 _diffrn_measurement_device_type Unknown _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _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 293 _diffrn_reflns_number 7561 _reflns_number_total 4979 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 4979 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5019 _diffrn_reflns_theta_min 1.359 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.931 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.45 _refine_diff_density_max 1.82 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3016 _refine_ls_number_restraints 2 _refine_ls_number_parameters 223 _oxford_refine_ls_R_factor_ref 0.0642 _refine_ls_wR_factor_ref 0.0688 _refine_ls_goodness_of_fit_ref 1.1553 _refine_ls_shift/su_max 0.000119 # The values computed from all data _oxford_reflns_number_all 4964 _refine_ls_R_factor_all 0.1173 _refine_ls_wR_factor_all 0.0879 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3016 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_gt 0.0688 # 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: 1.11 0.232 0.699 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. 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 Pd1 Pd 0.5000 0.5000 0.5000 0.0364 1.0000 Uani S . . . . . . N1 N 0.5827(2) 0.5104(3) 0.45253(16) 0.0425 1.0000 Uani . . . . . . . O1 O 0.6470(2) 0.5496(3) 0.46423(16) 0.0623 1.0000 Uani . . . . . . . H4 H 0.6337 0.5693 0.4900 0.0929 1.0000 Uiso R . . . . . . C1 C 0.5817(3) 0.4672(3) 0.41380(19) 0.0414 1.0000 Uani . . . . . . . N3 N 0.6349(3) 0.4531(3) 0.38032(18) 0.0544 1.0000 Uani . . . . . . . C11 C 0.7085(4) 0.4853(5) 0.3777(3) 0.0744 1.0000 Uani . . . . . . . C12 C 0.7108(8) 0.5547(8) 0.3519(5) 0.1422 1.0000 Uani . . . . . . . C13 C 0.6911(6) 0.5538(6) 0.2995(3) 0.1136 1.0000 Uani . . . . . . . C14 C 0.7018(10) 0.6234(9) 0.2721(7) 0.1809 1.0000 Uani . . . . . . . C15 C 0.6789(10) 0.6277(11) 0.2189(6) 0.1807 1.0000 Uani . . . . . . . C16 C 0.6924(11) 0.6936(11) 0.1877(8) 0.2040 1.0000 Uani D . . . . . . C17 C 0.6659(17) 0.7064(17) 0.1368(7) 0.2838 1.0000 Uani D . . . . . . C18 C 0.6994(19) 0.7605(15) 0.1062(10) 0.3159 1.0000 Uani . . . . . . . H18 H 0.6126 0.7135 0.1380 0.3160 1.0000 Uiso R . . . . . . H19 H 0.6773 0.6600 0.1206 0.3160 1.0000 Uiso R . . . . . . H20 H 0.6672 0.7339 0.2047 0.2460 1.0000 Uiso R . . . . . . H21 H 0.7454 0.7024 0.1878 0.2459 1.0000 Uiso R . . . . . . H22 H 0.7030 0.5866 0.2019 0.2111 1.0000 Uiso R . . . . . . H23 H 0.6257 0.6195 0.2192 0.2110 1.0000 Uiso R . . . . . . H24 H 0.7549 0.6333 0.2728 0.2231 1.0000 Uiso R . . . . . . H25 H 0.6756 0.6620 0.2902 0.2232 1.0000 Uiso R . . . . . . H26 H 0.6392 0.5404 0.2975 0.1379 1.0000 Uiso R . . . . . . H27 H 0.7212 0.5157 0.2840 0.1382 1.0000 Uiso R . . . . . . H28 H 0.7611 0.5741 0.3544 0.1692 1.0000 Uiso R . . . . . . H29 H 0.6766 0.5883 0.3687 0.1692 1.0000 Uiso R . . . . . . H30 H 0.7274 0.4925 0.4113 0.0882 1.0000 Uiso R . . . . . . H31 H 0.7401 0.4514 0.3600 0.0880 1.0000 Uiso R . . . . . . H32 H 0.6248 0.4205 0.3580 0.0648 1.0000 Uiso R . . . . . . C2 C 0.5103(3) 0.4262(3) 0.40883(18) 0.0402 1.0000 Uani . . . . . . . N2 N 0.4651(2) 0.4347(2) 0.44590(15) 0.0397 1.0000 Uani . . . . . . . O2 O 0.40032(19) 0.4003(2) 0.44837(13) 0.0452 1.0000 Uani . . . . . . . N4 N 0.4973(3) 0.3780(3) 0.36895(15) 0.0420 1.0000 Uani . . . . . . . C21 C 0.4800(4) 0.4132(3) 0.32088(19) 0.0490 1.0000 Uani . . . . . . . C22 C 0.4697(4) 0.3547(4) 0.28050(19) 0.0524 1.0000 Uani . . . . . . . C23 C 0.4404(6) 0.3853(5) 0.2327(3) 0.0939 1.0000 Uani . . . . . . . C24 C 0.4271(6) 0.3294(6) 0.1915(3) 0.1059 1.0000 Uani . . . . . . . C25 C 0.3997(10) 0.3560(11) 0.1438(5) 0.1782 1.0000 Uani . . . . . . . C26 C 0.3893(7) 0.2955(11) 0.1026(4) 0.1690 1.0000 Uani . . . . . . . C27 C 0.3735(11) 0.3383(13) 0.0505(6) 0.2205 1.0000 Uani D . . . . . . C28 C 0.3821(17) 0.2802(15) 0.0123(9) 0.3080 1.0000 Uani D . . . . . . H45 H 0.3745 0.3109 -0.0223 0.4750 1.0000 Uiso R . . . . . . H46 H 0.3403 0.2374 0.0181 0.4750 1.0000 Uiso R . . . . . . H47 H 0.4384 0.2592 0.0168 0.4750 1.0000 Uiso R . . . . . . H48 H 0.3233 0.3568 0.0497 0.2760 1.0000 Uiso R . . . . . . H49 H 0.4079 0.3789 0.0460 0.2760 1.0000 Uiso R . . . . . . H50 H 0.3483 0.2638 0.1111 0.2030 1.0000 Uiso R . . . . . . H51 H 0.4338 0.2661 0.1005 0.2030 1.0000 Uiso R . . . . . . H52 H 0.4343 0.3932 0.1315 0.2171 1.0000 Uiso R . . . . . . H53 H 0.3516 0.3787 0.1497 0.2171 1.0000 Uiso R . . . . . . H54 H 0.4750 0.3066 0.1851 0.1292 1.0000 Uiso R . . . . . . H55 H 0.3922 0.2923 0.2040 0.1291 1.0000 Uiso R . . . . . . H56 H 0.4756 0.4225 0.2196 0.1125 1.0000 Uiso R . . . . . . H57 H 0.3932 0.4086 0.2396 0.1131 1.0000 Uiso R . . . . . . H58 H 0.5171 0.3314 0.2740 0.0631 1.0000 Uiso R . . . . . . H59 H 0.4352 0.3180 0.2930 0.0630 1.0000 Uiso R . . . . . . H60 H 0.5198 0.4464 0.3121 0.0590 1.0000 Uiso R . . . . . . H61 H 0.4348 0.4412 0.3243 0.0590 1.0000 Uiso R . . . . . . H62 H 0.4986 0.3316 0.3725 0.0511 1.0000 Uiso R . . . . . . H141 H 0.6650 0.7599 0.0743 0.4460 1.0000 Uiso R . . . . . . H142 H 0.7552 0.7466 0.0976 0.4460 1.0000 Uiso R . . . . . . H143 H 0.6953 0.8110 0.1261 0.4460 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 Pd1 0.0312(3) 0.0486(4) 0.0294(2) -0.0171(2) -0.0008(2) -0.0003(3) N1 0.033(2) 0.057(3) 0.038(2) -0.020(2) 0.0045(18) -0.008(2) O1 0.046(2) 0.087(3) 0.053(2) -0.037(2) 0.0077(19) -0.020(2) C1 0.040(3) 0.046(3) 0.037(3) -0.012(2) 0.000(2) -0.003(2) N3 0.046(3) 0.070(3) 0.047(3) -0.026(2) 0.011(2) -0.007(2) C11 0.056(4) 0.097(6) 0.070(5) -0.044(4) 0.019(3) -0.017(4) C12 0.145(11) 0.153(12) 0.129(10) -0.037(9) 0.049(9) -0.057(9) C13 0.135(9) 0.129(9) 0.077(6) -0.034(6) 0.036(6) -0.069(7) C14 0.181(15) 0.165(14) 0.197(17) 0.077(13) -0.032(13) -0.059(11) C15 0.194(16) 0.24(2) 0.110(10) -0.016(12) 0.015(11) -0.097(14) C16 0.194(17) 0.194(17) 0.22(2) 0.106(17) -0.029(16) -0.034(14) C17 0.36(4) 0.35(4) 0.137(16) -0.01(2) -0.04(2) -0.13(3) C18 0.43(5) 0.27(3) 0.25(3) 0.10(2) 0.17(3) 0.08(3) C2 0.039(3) 0.048(3) 0.034(2) -0.013(2) 0.003(2) 0.004(2) N2 0.037(2) 0.051(3) 0.031(2) -0.0160(19) -0.0041(17) -0.0026(19) O2 0.0343(19) 0.065(2) 0.0364(18) -0.0225(17) -0.0025(15) -0.0062(17) N4 0.055(3) 0.042(2) 0.028(2) -0.0148(18) -0.0023(19) 0.006(2) C21 0.064(4) 0.050(3) 0.033(3) -0.010(2) -0.002(2) 0.008(3) C22 0.065(4) 0.062(4) 0.030(2) -0.014(2) 0.002(2) -0.002(3) C23 0.126(7) 0.110(7) 0.046(4) -0.016(4) -0.032(4) 0.031(6) C24 0.109(7) 0.148(9) 0.061(5) -0.021(5) -0.008(5) 0.013(7) C25 0.190(14) 0.251(18) 0.093(8) -0.003(10) -0.066(9) -0.005(13) C26 0.116(9) 0.31(2) 0.085(7) -0.069(11) -0.028(7) 0.046(11) C27 0.179(16) 0.38(3) 0.106(10) -0.056(15) 0.013(11) -0.092(18) C28 0.33(4) 0.38(4) 0.21(2) -0.06(3) 0.11(2) -0.01(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1176(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.972(4) . . yes Pd1 N2 1.974(4) . . yes Pd1 N1 1.972(4) . 5_666 yes Pd1 N2 1.974(4) . 5_666 yes O1 N1 1.396(6) . . yes O2 N2 1.326(5) . . yes O1 H4 0.8100 . . no N1 C1 1.300(7) . . yes N2 C2 1.296(6) . . yes N3 C1 1.340(7) . . yes N3 C11 1.452(9) . . yes N4 C2 1.400(7) . . yes N4 C21 1.472(7) . . yes N3 H32 0.8600 . . no N4 H62 0.8400 . . no C1 C2 1.493(8) . . no C11 C12 1.433(17) . . no C12 C13 1.451(16) . . no C13 C14 1.47(2) . . no C14 C15 1.49(2) . . no C15 C16 1.48(3) . . no C16 C17 1.47(3) . . no C17 C18 1.41(4) . . no C21 C22 1.525(8) . . no C22 C23 1.494(10) . . no C23 C24 1.517(13) . . no C24 C25 1.455(17) . . no C25 C26 1.57(2) . . no C26 C27 1.62(2) . . no C27 C28 1.48(3) . . no C11 H30 0.9700 . . no C11 H31 0.9600 . . no C12 H28 0.9800 . . no C12 H29 0.9800 . . no C13 H26 0.9700 . . no C13 H27 0.9700 . . no C14 H24 0.9800 . . no C14 H25 0.9700 . . no C15 H22 0.9700 . . no C15 H23 0.9700 . . no C16 H20 0.9700 . . no C16 H21 0.9700 . . no C17 H18 0.9700 . . no C17 H19 0.9700 . . no C18 H141 1.0600 . . no C18 H142 1.0600 . . no C18 H143 1.0600 . . no C21 H60 0.9700 . . no C21 H61 0.9600 . . no C22 H58 0.9700 . . no C22 H59 0.9700 . . no C23 H56 0.9900 . . no C23 H57 0.9700 . . no C24 H54 0.9700 . . no C24 H55 0.9800 . . no C25 H52 0.9800 . . no C25 H53 0.9700 . . no C26 H50 0.9600 . . no C26 H51 0.9600 . . no C27 H48 0.9700 . . no C27 H49 0.9700 . . no C28 H45 1.0900 . . no C28 H46 1.0900 . . no C28 H47 1.0900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 79.81(17) . . . yes N1 Pd1 N1 180.00 . . 5_666 yes N1 Pd1 N2 100.19(17) . . 5_666 yes N1 Pd1 N2 100.19(17) 5_666 . . yes N2 Pd1 N2 180.00 . . 5_666 yes N1 Pd1 N2 79.81(17) 5_666 . 5_666 yes N1 O1 H4 100.00 . . . no Pd1 N1 C1 116.7(4) . . . yes O1 N1 C1 119.7(4) . . . yes Pd1 N1 O1 122.2(3) . . . yes Pd1 N2 C2 115.8(3) . . . yes O2 N2 C2 122.6(4) . . . yes Pd1 N2 O2 121.6(3) . . . yes C1 N3 C11 127.8(6) . . . yes C2 N4 C21 116.0(5) . . . yes C11 N3 H32 116.00 . . . no C1 N3 H32 116.00 . . . no C2 N4 H62 122.00 . . . no C21 N4 H62 122.00 . . . no N1 C1 N3 129.8(5) . . . yes N3 C1 C2 117.7(5) . . . yes N1 C1 C2 112.4(4) . . . yes N2 C2 C1 114.6(4) . . . yes N2 C2 N4 123.7(5) . . . yes N4 C2 C1 121.4(5) . . . yes N3 C11 C12 113.6(8) . . . yes C11 C12 C13 116.9(11) . . . no C12 C13 C14 116.3(11) . . . no C13 C14 C15 119.2(14) . . . no C14 C15 C16 122.7(16) . . . no C15 C16 C17 127(2) . . . no C16 C17 C18 121(2) . . . no N4 C21 C22 110.5(5) . . . yes C21 C22 C23 113.4(6) . . . no C22 C23 C24 115.9(7) . . . no C23 C24 C25 118.5(11) . . . no C24 C25 C26 115.6(14) . . . no C25 C26 C27 107.3(15) . . . no C26 C27 C28 104.0(18) . . . no N3 C11 H30 109.00 . . . no N3 C11 H31 108.00 . . . no C12 C11 H30 109.00 . . . no C12 C11 H31 107.00 . . . no H30 C11 H31 110.00 . . . no C11 C12 H28 108.00 . . . no C11 C12 H29 108.00 . . . no C13 C12 H28 107.00 . . . no C13 C12 H29 107.00 . . . no H28 C12 H29 110.00 . . . no C12 C13 H26 107.00 . . . no C12 C13 H27 107.00 . . . no C14 C13 H26 108.00 . . . no C14 C13 H27 109.00 . . . no H26 C13 H27 110.00 . . . no C13 C14 H24 106.00 . . . no C13 C14 H25 107.00 . . . no C15 C14 H24 106.00 . . . no C15 C14 H25 108.00 . . . no H24 C14 H25 110.00 . . . no C14 C15 H22 107.00 . . . no C14 C15 H23 105.00 . . . no C16 C15 H22 106.00 . . . no C16 C15 H23 107.00 . . . no H22 C15 H23 109.00 . . . no C15 C16 H20 105.00 . . . no C15 C16 H21 107.00 . . . no C17 C16 H20 100.00 . . . no C17 C16 H21 107.00 . . . no H20 C16 H21 110.00 . . . no C16 C17 H18 108.00 . . . no C16 C17 H19 102.00 . . . no C18 C17 H18 111.00 . . . no C18 C17 H19 104.00 . . . no H18 C17 H19 110.00 . . . no C17 C18 H141 102.00 . . . no C17 C18 H142 112.00 . . . no C17 C18 H143 106.00 . . . no H141 C18 H142 112.00 . . . no H141 C18 H143 112.00 . . . no H142 C18 H143 112.00 . . . no N4 C21 H60 109.00 . . . no N4 C21 H61 109.00 . . . no C22 C21 H60 110.00 . . . no C22 C21 H61 109.00 . . . no H60 C21 H61 109.00 . . . no C21 C22 H58 109.00 . . . no C21 C22 H59 108.00 . . . no C23 C22 H58 109.00 . . . no C23 C22 H59 109.00 . . . no H58 C22 H59 109.00 . . . no C22 C23 H56 109.00 . . . no C22 C23 H57 108.00 . . . no C24 C23 H56 107.00 . . . no C24 C23 H57 107.00 . . . no H56 C23 H57 110.00 . . . no C23 C24 H54 106.00 . . . no C23 C24 H55 108.00 . . . no C25 C24 H54 107.00 . . . no C25 C24 H55 108.00 . . . no H54 C24 H55 110.00 . . . no C24 C25 H52 108.00 . . . no C24 C25 H53 107.00 . . . no C26 C25 H52 109.00 . . . no C26 C25 H53 108.00 . . . no H52 C25 H53 110.00 . . . no C25 C26 H50 110.00 . . . no C25 C26 H51 109.00 . . . no C27 C26 H50 111.00 . . . no C27 C26 H51 111.00 . . . no H50 C26 H51 109.00 . . . no C26 C27 H48 110.00 . . . no C26 C27 H49 111.00 . . . no C28 C27 H48 109.00 . . . no C28 C27 H49 113.00 . . . no H48 C27 H49 110.00 . . . no C27 C28 H45 103.00 . . . no C27 C28 H46 109.00 . . . no C27 C28 H47 106.00 . . . no H45 C28 H46 113.00 . . . no H45 C28 H47 113.00 . . . no H46 C28 H47 112.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 N1 O1 -174.0(4) . . . . no N2 Pd1 N1 C1 -7.5(4) . . . . no N2 Pd1 N1 O1 6.0(4) 5_666 . . . no N2 Pd1 N1 C1 172.5(4) 5_666 . . . no N1 Pd1 N2 O2 -178.4(4) . . . . no N1 Pd1 N2 C2 3.5(4) . . . . no N1 Pd1 N2 O2 1.6(4) 5_666 . . . no N1 Pd1 N2 C2 -176.5(4) 5_666 . . . no Pd1 N1 C1 N3 -167.8(5) . . . . no Pd1 N1 C1 C2 9.5(6) . . . . no O1 N1 C1 N3 -0.9(9) . . . . no O1 N1 C1 C2 176.4(5) . . . . no Pd1 N2 C2 N4 175.3(4) . . . . no Pd1 N2 C2 C1 0.5(6) . . . . no O2 N2 C2 N4 -2.8(8) . . . . no O2 N2 C2 C1 -177.7(4) . . . . no C11 N3 C1 N1 -2.4(10) . . . . no C11 N3 C1 C2 -179.5(6) . . . . no C1 N3 C11 C12 -84.8(10) . . . . no C21 N4 C2 N2 109.2(6) . . . . no C21 N4 C2 C1 -76.4(7) . . . . no C2 N4 C21 C22 178.1(5) . . . . no N1 C1 C2 N2 -6.5(7) . . . . no N1 C1 C2 N4 178.6(5) . . . . no N3 C1 C2 N2 171.1(5) . . . . no N3 C1 C2 N4 -3.8(8) . . . . no N3 C11 C12 C13 -63.7(13) . . . . no C11 C12 C13 C14 -173.3(12) . . . . no C12 C13 C14 C15 -176.7(14) . . . . no C13 C14 C15 C16 -175.6(16) . . . . no C14 C15 C16 C17 -174(2) . . . . no C15 C16 C17 C18 -162(2) . . . . no N4 C21 C22 C23 170.9(6) . . . . no C21 C22 C23 C24 -178.5(8) . . . . no C22 C23 C24 C25 -179.0(11) . . . . no C23 C24 C25 C26 178.4(11) . . . . no C24 C25 C26 C27 -169.7(13) . . . . no C25 C26 C27 C28 167.0(17) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd1 C24 3.841(10) . 2_555 no Pd1 C24 3.841(10) . 6_555 no Pd1 H55 2.9500 . 2_555 no Pd1 H55 2.9500 . 6_555 no O1 N3 2.857(7) . . no O1 C11 2.825(9) . . no O1 C12 3.230(14) . . no O1 N2 3.162(6) . 5_666 no O1 O2 2.656(6) . 5_666 no O2 C21 3.323(8) . 16_545 no O2 N1 3.126(6) . 5_666 no O2 C11 3.358(9) . 16_545 no O2 N4 2.789(6) . . no O2 O1 2.656(6) . 5_666 no O2 N3 2.834(6) . 16_545 no O2 C22 3.311(8) . 16_545 no O1 H30 2.2800 . . no O1 H27 2.8700 . 12_565 no O1 H29 2.7100 . . no O2 H4 1.8500 . 5_666 no O2 H31 2.9100 . 16_545 no O2 H32 2.0300 . 16_545 no O2 H58 2.5400 . 16_545 no N1 N2 2.532(6) . . no N1 C2 2.323(7) . . no N1 O2 3.126(6) . 5_666 no N1 N2 3.028(6) . 5_666 no N2 N1 2.532(6) . . no N2 N1 3.028(6) . 5_666 no N2 C1 2.350(7) . . no N2 O1 3.162(6) . 5_666 no N3 O2 2.834(6) . 6_555 no N3 N4 2.847(8) . . no N3 C21 3.300(9) . . no N3 O1 2.857(7) . . no N4 O2 2.789(6) . . no N4 N4 3.286(8) . 16_545 no N4 N4 3.286(8) . 6_555 no N4 N3 2.847(8) . . no N1 H30 2.8600 . . no N2 H59 2.8700 . 6_555 no N2 H4 2.4800 . 5_666 no N3 H60 2.7700 . . no N3 H26 2.7300 . . no N4 H32 2.4400 . . no N4 H59 2.9200 . 6_555 no N4 H62 2.7600 . 6_555 no N4 H62 2.7500 . 16_545 no C2 C22 3.536(9) . 6_555 no C11 O1 2.825(9) . . no C11 O2 3.358(9) . 6_555 no C12 O1 3.230(14) . . no C18 C28 3.58(4) . 5_665 no C21 N3 3.300(9) . . no C21 O2 3.323(8) . 6_555 no C22 C2 3.536(9) . 16_545 no C22 O2 3.311(8) . 6_555 no C24 Pd1 3.841(10) . 4_454 no C24 Pd1 3.841(10) . 16_545 no C28 C18 3.58(4) . 5_665 no C1 H29 3.0300 . . no C1 H59 3.0000 . 6_555 no C1 H60 2.9700 . . no C2 H59 2.6100 . 6_555 no C12 H143 3.0200 . 13_665 no C18 H45 2.9200 . 5_665 no C21 H32 2.8000 . . no C23 H142 3.1000 . 14_465 no C24 H54 3.0300 . 11_655 no C25 H142 3.0700 . 14_465 no C28 H23 3.0500 . 4_454 no C28 H141 2.5800 . 5_665 no H4 O2 1.8500 . 5_666 no H4 N2 2.4800 . 5_666 no H19 H22 2.6000 . . no H20 H143 2.5800 . . no H21 H142 2.5600 . . no H21 H49 2.4500 . 8_655 no H22 H19 2.6000 . . no H22 H27 2.5700 . . no H22 H30 2.4600 . 10_644 no H23 H26 2.5500 . . no H23 C28 3.0500 . 2_555 no H23 H46 2.4800 . 2_555 no H23 H141 2.4700 . 14_465 no H24 H28 2.4400 . . no H25 H29 2.4900 . . no H26 N3 2.7300 . . no H26 H23 2.5500 . . no H26 H46 2.5800 . 2_555 no H27 H22 2.5700 . . no H27 H31 2.3700 . . no H27 O1 2.8700 . 10_644 no H28 H24 2.4400 . . no H28 H143 2.2800 . 13_665 no H29 O1 2.7100 . . no H29 C1 3.0300 . . no H29 H25 2.4900 . . no H30 O1 2.2800 . . no H30 N1 2.8600 . . no H30 H22 2.4600 . 12_565 no H31 H27 2.3700 . . no H31 O2 2.9100 . 6_555 no H31 H53 2.4200 . 7_555 no H32 N4 2.4400 . . no H32 C21 2.8000 . . no H32 H60 2.3100 . . no H32 O2 2.0300 . 6_555 no H45 C18 2.9200 . 5_665 no H45 H141 2.0200 . 5_665 no H46 H50 2.5500 . . no H46 H23 2.4800 . 4_454 no H46 H26 2.5800 . 4_454 no H46 H141 2.4800 . 5_665 no H47 H51 2.2500 . . no H47 H47 2.2500 . 11_655 no H48 H61 2.5900 . 4_454 no H49 H52 2.3600 . . no H49 H21 2.4500 . 14_465 no H50 H46 2.5500 . . no H51 H47 2.2500 . . no H51 H54 2.5000 . . no H51 H51 2.4600 . 11_655 no H52 H49 2.3600 . . no H52 H56 2.5400 . . no H52 H142 2.2200 . 14_465 no H53 H57 2.5900 . . no H53 H31 2.4200 . 7_455 no H54 H51 2.5000 . . no H54 H58 2.5400 . . no H54 C24 3.0300 . 11_655 no H54 H54 2.2300 . 11_655 no H55 H59 2.5600 . . no H55 Pd1 2.9500 . 4_454 no H55 Pd1 2.9500 . 16_545 no H56 H52 2.5400 . . no H56 H142 2.2600 . 14_465 no H57 H53 2.5900 . . no H57 H61 2.4700 . . no H58 H54 2.5400 . . no H58 O2 2.5400 . 6_555 no H59 H55 2.5600 . . no H59 H62 2.4300 . . no H59 N2 2.8700 . 16_545 no H59 N4 2.9200 . 16_545 no H59 C1 3.0000 . 16_545 no H59 C2 2.6100 . 16_545 no H60 N3 2.7700 . . no H60 C1 2.9700 . . no H60 H32 2.3100 . . no H61 H57 2.4700 . . no H61 H48 2.5900 . 2_555 no H62 H59 2.4300 . . no H62 N4 2.7500 . 6_555 no H62 H62 2.0900 . 6_555 no H62 N4 2.7600 . 16_545 no H62 H62 2.0900 . 16_545 no H141 C28 2.5800 . 5_665 no H141 H45 2.0200 . 5_665 no H141 H46 2.4800 . 5_665 no H141 H23 2.4700 . 8_655 no H142 H21 2.5600 . . no H142 C23 3.1000 . 8_655 no H142 C25 3.0700 . 8_655 no H142 H52 2.2200 . 8_655 no H142 H56 2.2600 . 8_655 no H143 H20 2.5800 . . no H143 C12 3.0200 . 13_665 no H143 H28 2.2800 . 13_665 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H4 O2 0.8100 1.8500 2.656(6) 171.00 5_666 yes N3 H32 O2 0.8600 2.0300 2.834(6) 154.00 6_555 yes C11 H30 O1 0.9700 2.2800 2.825(9) 115.00 . yes C22 H58 O2 0.9700 2.5400 3.311(8) 137.00 6_555 yes # Attachment 'VAC8Ni4.CIF' data_VAC8Ni4 _database_code_depnum_ccdc_archive 'CCDC 648650' _audit_creation_date 07-07-10 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '401 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.9868(3) _cell_length_b 9.3738(3) _cell_length_c 15.3050(6) _cell_angle_alpha 75.7560(10) _cell_angle_beta 81.4240(10) _cell_angle_gamma 83.2600(10) _cell_volume 1231.31(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -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' 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' 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' _cell_formula_units_Z 1 # Given Formula = C38 H82 N8 Ni1 O6 # Dc = 1.09 Fooo = 442.00 Mu = 4.39 M = 402.91 # Found Formula = C38 H82 N8 Ni1 O6 # Dc = 1.09 FOOO = 442.00 Mu = 4.39 M = 402.91 _chemical_formula_sum 'C38 H82 N8 Ni1 O6' _chemical_formula_moiety 'C36 H74 N8 Ni O4, 2(C H4 O)' _chemical_compound_source ? _chemical_formula_weight 805.83 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 160 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 0.439 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 293 _diffrn_reflns_number 8758 _reflns_number_total 5573 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 5573 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5561 _diffrn_reflns_theta_min 1.384 _diffrn_reflns_theta_max 27.466 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.818 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -11 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.13 _refine_diff_density_max 0.96 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2656 _refine_ls_number_restraints 6 _refine_ls_number_parameters 241 _oxford_refine_ls_R_factor_ref 0.0873 _refine_ls_wR_factor_ref 0.0977 _refine_ls_goodness_of_fit_ref 1.0743 _refine_ls_shift/su_max 0.000153 # The values computed from all data _oxford_reflns_number_all 5553 _refine_ls_R_factor_all 0.1830 _refine_ls_wR_factor_all 0.1525 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2656 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_gt 0.0977 # 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: 1.55 1.04 1.03 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. 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 Ni1 Ni 0.0000 0.0000 1.0000 0.0584 1.0000 Uani S . . . . . . N1 N -0.0026(5) -0.2015(5) 1.0538(3) 0.0612 1.0000 Uani . . . . . . . O1 O -0.1007(4) -0.2573(4) 1.1281(2) 0.0733 1.0000 Uani . . . . . . . H4 H -0.1377 -0.1865 1.1500 0.1043 1.0000 Uiso R . . . . . . C1 C 0.0949(6) -0.2906(6) 1.0167(4) 0.0609 1.0000 Uani . . . . . . . N3 N 0.1193(6) -0.4380(5) 1.0462(3) 0.0793 1.0000 Uani . . . . . . . C11 C 0.0805(8) -0.5275(6) 1.1377(4) 0.0799 1.0000 Uani . . . . . . . C12 C 0.1740(8) -0.4998(8) 1.2036(4) 0.0898 1.0000 Uani . . . . . . . C13 C 0.1380(9) -0.5914(9) 1.2983(5) 0.1019 1.0000 Uani . . . . . . . C14 C 0.2227(9) -0.5595(10) 1.3665(5) 0.1120 1.0000 Uani . . . . . . . C15 C 0.1935(11) -0.6490(11) 1.4617(5) 0.1212 1.0000 Uani . . . . . . . C16 C 0.2806(10) -0.6049(10) 1.5269(5) 0.1171 1.0000 Uani . . . . . . . C17 C 0.2624(12) -0.6896(12) 1.6209(6) 0.1325 1.0000 Uani . . . . . . . C18 C 0.3504(11) -0.6469(11) 1.6828(6) 0.1239 1.0000 Uani . . . . . . . H15 H 0.3394 -0.7139 1.7412 0.1768 1.0000 Uiso R . . . . . . H16 H 0.4558 -0.6482 1.6583 0.1768 1.0000 Uiso R . . . . . . H17 H 0.3148 -0.5491 1.6892 0.1770 1.0000 Uiso R . . . . . . H18 H 0.2926 -0.7926 1.6201 0.1491 1.0000 Uiso R . . . . . . H19 H 0.1554 -0.6785 1.6441 0.1490 1.0000 Uiso R . . . . . . H20 H 0.2460 -0.5026 1.5279 0.1300 1.0000 Uiso R . . . . . . H21 H 0.3873 -0.6117 1.5044 0.1300 1.0000 Uiso R . . . . . . H22 H 0.0866 -0.6378 1.4821 0.1400 1.0000 Uiso R . . . . . . H23 H 0.2233 -0.7523 1.4617 0.1400 1.0000 Uiso R . . . . . . H24 H 0.3294 -0.5776 1.3462 0.1260 1.0000 Uiso R . . . . . . H25 H 0.2001 -0.4555 1.3674 0.1260 1.0000 Uiso R . . . . . . H26 H 0.1615 -0.6948 1.2968 0.1181 1.0000 Uiso R . . . . . . H27 H 0.0305 -0.5741 1.3170 0.1179 1.0000 Uiso R . . . . . . H28 H 0.2802 -0.5241 1.1835 0.0999 1.0000 Uiso R . . . . . . H29 H 0.1571 -0.3971 1.2054 0.1000 1.0000 Uiso R . . . . . . H30 H -0.0255 -0.5045 1.1580 0.0917 1.0000 Uiso R . . . . . . H31 H 0.0966 -0.6310 1.1360 0.0921 1.0000 Uiso R . . . . . . H32 H 0.1646 -0.4853 1.0068 0.0907 1.0000 Uiso R . . . . . . C2 C -0.1821(6) 0.2095(6) 1.0682(3) 0.0595 1.0000 Uani . . . . . . . N2 N -0.1501(5) 0.0697(5) 1.0817(3) 0.0620 1.0000 Uani . . . . . . . O2 O -0.2263(5) -0.0219(4) 1.1558(3) 0.0817 1.0000 Uani . . . . . . . N4 N -0.2830(5) 0.2860(5) 1.1176(3) 0.0755 1.0000 Uani . . . . . . . C21 C -0.3557(7) 0.2320(7) 1.2110(4) 0.0769 1.0000 Uani . . . . . . . C22 C -0.2505(7) 0.2091(7) 1.2812(4) 0.0800 1.0000 Uani . . . . . . . C23 C -0.3270(7) 0.1698(8) 1.3773(4) 0.0871 1.0000 Uani . . . . . . . C24 C -0.2241(8) 0.1430(9) 1.4496(4) 0.0935 1.0000 Uani . . . . . . . C25 C -0.2976(8) 0.1129(9) 1.5457(5) 0.1012 1.0000 Uani . . . . . . . C26 C -0.1953(8) 0.0854(10) 1.6180(5) 0.1020 1.0000 Uani . . . . . . . C27 C -0.2679(10) 0.0597(12) 1.7150(5) 0.1249 1.0000 Uani . . . . . . . C28 C -0.1652(12) 0.0378(13) 1.7824(6) 0.1384 1.0000 Uani . . . . . . . H45 H -0.2208 0.0234 1.8423 0.1948 1.0000 Uiso R . . . . . . H46 H -0.1080 0.1220 1.7716 0.1950 1.0000 Uiso R . . . . . . H47 H -0.0971 -0.0479 1.7785 0.1950 1.0000 Uiso R . . . . . . H48 H -0.3379 0.1443 1.7215 0.1409 1.0000 Uiso R . . . . . . H49 H -0.3231 -0.0277 1.7274 0.1409 1.0000 Uiso R . . . . . . H50 H -0.1349 0.1692 1.6060 0.1178 1.0000 Uiso R . . . . . . H51 H -0.1286 -0.0022 1.6127 0.1180 1.0000 Uiso R . . . . . . H52 H -0.3524 0.0261 1.5559 0.1149 1.0000 Uiso R . . . . . . H53 H -0.3680 0.1973 1.5523 0.1149 1.0000 Uiso R . . . . . . H54 H -0.1515 0.0607 1.4419 0.1092 1.0000 Uiso R . . . . . . H55 H -0.1705 0.2306 1.4398 0.1090 1.0000 Uiso R . . . . . . H56 H -0.3995 0.2520 1.3862 0.1000 1.0000 Uiso R . . . . . . H57 H -0.3804 0.0820 1.3852 0.0999 1.0000 Uiso R . . . . . . H58 H -0.2021 0.2999 1.2725 0.0941 1.0000 Uiso R . . . . . . H59 H -0.1744 0.1290 1.2726 0.0940 1.0000 Uiso R . . . . . . H60 H -0.3967 0.1393 1.2146 0.0899 1.0000 Uiso R . . . . . . H61 H -0.4363 0.3048 1.2228 0.0900 1.0000 Uiso R . . . . . . H62 H -0.3064 0.3776 1.0924 0.0872 1.0000 Uiso R . . . . . . O1M O 0.2996(6) 0.3933(6) 0.9266(4) 0.1131 1.0000 Uani . U . . . . . C1M C 0.4338(9) 0.2887(9) 0.9598(6) 0.1165 1.0000 Uani . U . . . . . H65 H 0.5010 0.3413 0.9846 0.1749 1.0000 Uiso R . . . . . . H66 H 0.4955 0.2457 0.9115 0.1737 1.0000 Uiso R . . . . . . H67 H 0.3999 0.2030 1.0098 0.1739 1.0000 Uiso R . . . . . . H68 H 0.2365 0.3517 0.9126 0.1716 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0675(7) 0.0522(6) 0.0548(6) -0.0121(4) -0.0030(4) -0.0094(4) N1 0.071(3) 0.052(2) 0.057(2) -0.0093(19) -0.002(2) -0.007(2) O1 0.090(3) 0.057(2) 0.064(2) -0.0089(17) 0.0118(19) -0.0122(19) C1 0.068(3) 0.053(3) 0.063(3) -0.013(2) -0.014(3) -0.005(3) N3 0.103(4) 0.060(3) 0.070(3) -0.013(2) -0.002(3) -0.003(3) C11 0.094(4) 0.055(3) 0.084(4) -0.005(3) -0.008(3) -0.007(3) C12 0.095(4) 0.088(4) 0.080(4) -0.003(3) -0.012(3) -0.012(4) C13 0.127(6) 0.096(5) 0.080(4) -0.005(4) -0.018(4) -0.028(4) C14 0.109(5) 0.127(6) 0.096(5) -0.010(5) -0.020(4) -0.015(5) C15 0.146(7) 0.129(7) 0.088(5) -0.012(5) -0.024(5) -0.024(6) C16 0.124(6) 0.124(6) 0.093(5) -0.010(5) -0.006(5) -0.012(5) C17 0.150(8) 0.154(8) 0.089(5) -0.018(5) 0.004(5) -0.041(6) C18 0.135(7) 0.141(8) 0.096(5) -0.028(5) -0.009(5) -0.020(6) C2 0.058(3) 0.063(3) 0.064(3) -0.027(3) -0.012(2) -0.003(2) N2 0.070(3) 0.059(3) 0.055(2) -0.0146(19) 0.005(2) -0.011(2) O2 0.097(3) 0.067(2) 0.073(2) -0.0151(19) 0.023(2) -0.020(2) N4 0.079(3) 0.065(3) 0.080(3) -0.020(2) -0.003(3) 0.005(2) C21 0.073(4) 0.073(4) 0.081(4) -0.026(3) 0.014(3) -0.009(3) C22 0.073(4) 0.089(4) 0.081(4) -0.030(3) 0.004(3) -0.016(3) C23 0.087(4) 0.089(4) 0.081(4) -0.022(3) 0.010(3) -0.012(3) C24 0.086(4) 0.113(5) 0.079(4) -0.026(4) 0.006(4) -0.013(4) C25 0.090(5) 0.118(6) 0.089(5) -0.022(4) 0.004(4) -0.006(4) C26 0.093(5) 0.116(6) 0.093(5) -0.018(4) -0.006(4) -0.013(4) C27 0.110(6) 0.166(9) 0.090(5) -0.022(5) -0.011(5) 0.006(6) C28 0.155(8) 0.159(9) 0.102(6) -0.028(6) -0.033(6) -0.005(7) O1M 0.111(3) 0.096(3) 0.146(4) -0.048(3) -0.039(3) 0.009(2) C1M 0.113(3) 0.100(3) 0.148(4) -0.046(3) -0.039(3) 0.010(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.636(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.867(5) . . yes Ni1 N2 1.871(5) . . yes Ni1 N1 1.867(5) . 2_557 yes Ni1 N2 1.871(5) . 2_557 yes O1 N1 1.364(6) . . yes O2 N2 1.386(6) . . yes O1 H4 0.8300 . . no O1M C1M 1.528(10) . . yes O1M H68 0.8100 . . no N1 C1 1.304(7) . . yes N2 C2 1.280(7) . . yes N3 C1 1.346(7) . . yes N3 C11 1.460(7) . . yes N4 C2 1.348(7) . . yes N4 C21 1.473(7) . . yes N3 H32 0.8600 . . no N4 H62 0.8700 . . no C1 C2 1.494(8) . 2_557 no C11 C12 1.491(9) . . no C12 C13 1.502(10) . . no C13 C14 1.484(11) . . no C14 C15 1.494(11) . . no C15 C16 1.514(12) . . no C16 C17 1.458(12) . . no C17 C18 1.472(14) . . no C21 C22 1.495(9) . . no C22 C23 1.504(8) . . no C23 C24 1.502(9) . . no C24 C25 1.493(10) . . no C25 C26 1.498(10) . . no C26 C27 1.503(11) . . no C27 C28 1.447(13) . . no C11 H30 0.9700 . . no C11 H31 0.9700 . . no C12 H28 0.9800 . . no C12 H29 0.9600 . . no C13 H26 0.9700 . . no C13 H27 0.9700 . . no C14 H25 0.9800 . . no C14 H24 0.9700 . . no C15 H22 0.9700 . . no C15 H23 0.9700 . . no C16 H21 0.9700 . . no C16 H20 0.9800 . . no C17 H19 0.9800 . . no C17 H18 0.9700 . . no C18 H16 0.9700 . . no C18 H15 0.9600 . . no C18 H17 0.9600 . . no C21 H61 0.9600 . . no C21 H60 0.9700 . . no C22 H59 0.9700 . . no C22 H58 0.9700 . . no C23 H57 0.9700 . . no C23 H56 0.9700 . . no C24 H54 0.9700 . . no C24 H55 0.9700 . . no C25 H53 0.9700 . . no C25 H52 0.9700 . . no C26 H51 0.9700 . . no C26 H50 0.9700 . . no C27 H49 0.9700 . . no C27 H48 0.9700 . . no C28 H47 0.9600 . . no C28 H45 0.9600 . . no C28 H46 0.9600 . . no C1M H65 0.9900 . . no C1M H66 0.9900 . . no C1M H67 1.0000 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 98.1(2) . . . yes N1 Ni1 N1 180.00 . . 2_557 yes N1 Ni1 N2 81.9(2) . . 2_557 yes N1 Ni1 N2 81.9(2) 2_557 . . yes N2 Ni1 N2 180.00 . . 2_557 yes N1 Ni1 N2 98.1(2) 2_557 . 2_557 yes N1 O1 H4 106.00 . . . no C1M O1M H68 113.00 . . . no O1 N1 C1 119.9(5) . . . yes Ni1 N1 O1 123.2(3) . . . yes Ni1 N1 C1 116.9(4) . . . yes O2 N2 C2 118.9(4) . . . yes Ni1 N2 O2 123.4(3) . . . yes Ni1 N2 C2 117.7(4) . . . yes C1 N3 C11 127.7(5) . . . yes C2 N4 C21 127.2(5) . . . yes C1 N3 H32 116.00 . . . no C11 N3 H32 116.00 . . . no C2 N4 H62 117.00 . . . no C21 N4 H62 116.00 . . . no N3 C1 C2 121.0(5) . . 2_557 yes N1 C1 N3 127.4(5) . . . yes N1 C1 C2 111.6(5) . . 2_557 yes N2 C2 N4 128.9(5) . . . yes N2 C2 C1 111.7(5) . . 2_557 yes N4 C2 C1 119.3(5) . . 2_557 yes N3 C11 C12 111.9(5) . . . yes C11 C12 C13 113.3(6) . . . no C12 C13 C14 114.4(7) . . . no C13 C14 C15 116.9(8) . . . no C14 C15 C16 113.0(8) . . . no C15 C16 C17 116.8(8) . . . no C16 C17 C18 115.9(9) . . . no N4 C21 C22 113.4(5) . . . yes C21 C22 C23 113.8(5) . . . no C22 C23 C24 115.2(5) . . . no C23 C24 C25 116.6(6) . . . no C24 C25 C26 116.7(6) . . . no C25 C26 C27 117.4(7) . . . no C26 C27 C28 115.5(8) . . . no N3 C11 H30 109.00 . . . no C12 C11 H30 109.00 . . . no C12 C11 H31 109.00 . . . no N3 C11 H31 109.00 . . . no H30 C11 H31 109.00 . . . no C11 C12 H29 109.00 . . . no C13 C12 H28 108.00 . . . no C13 C12 H29 108.00 . . . no H28 C12 H29 110.00 . . . no C11 C12 H28 109.00 . . . no C12 C13 H26 108.00 . . . no C12 C13 H27 108.00 . . . no C14 C13 H27 109.00 . . . no H26 C13 H27 109.00 . . . no C14 C13 H26 108.00 . . . no C13 C14 H24 107.00 . . . no C15 C14 H24 107.00 . . . no C15 C14 H25 108.00 . . . no C13 C14 H25 108.00 . . . no H24 C14 H25 109.00 . . . no C14 C15 H23 108.00 . . . no C16 C15 H22 109.00 . . . no C16 C15 H23 108.00 . . . no H22 C15 H23 109.00 . . . no C14 C15 H22 109.00 . . . no C15 C16 H20 107.00 . . . no C17 C16 H20 107.00 . . . no C17 C16 H21 108.00 . . . no C15 C16 H21 109.00 . . . no H20 C16 H21 110.00 . . . no C16 C17 H19 107.00 . . . no C18 C17 H18 108.00 . . . no C16 C17 H18 107.00 . . . no H18 C17 H19 110.00 . . . no C18 C17 H19 108.00 . . . no C17 C18 H15 110.00 . . . no C17 C18 H17 109.00 . . . no H15 C18 H16 109.00 . . . no H15 C18 H17 109.00 . . . no H16 C18 H17 109.00 . . . no C17 C18 H16 110.00 . . . no N4 C21 H61 107.00 . . . no C22 C21 H60 109.00 . . . no N4 C21 H60 108.00 . . . no H60 C21 H61 110.00 . . . no C22 C21 H61 109.00 . . . no C21 C22 H58 108.00 . . . no C21 C22 H59 109.00 . . . no C23 C22 H59 108.00 . . . no H58 C22 H59 110.00 . . . no C23 C22 H58 109.00 . . . no C22 C23 H57 109.00 . . . no C24 C23 H56 107.00 . . . no C24 C23 H57 109.00 . . . no H56 C23 H57 109.00 . . . no C22 C23 H56 108.00 . . . no C23 C24 H54 108.00 . . . no C25 C24 H54 109.00 . . . no C25 C24 H55 107.00 . . . no C23 C24 H55 108.00 . . . no H54 C24 H55 109.00 . . . no C24 C25 H53 107.00 . . . no C26 C25 H52 107.00 . . . no C24 C25 H52 108.00 . . . no H52 C25 H53 110.00 . . . no C26 C25 H53 108.00 . . . no C25 C26 H50 108.00 . . . no C27 C26 H50 108.00 . . . no C27 C26 H51 107.00 . . . no H50 C26 H51 109.00 . . . no C25 C26 H51 107.00 . . . no C26 C27 H48 108.00 . . . no C28 C27 H48 108.00 . . . no C28 C27 H49 108.00 . . . no C26 C27 H49 108.00 . . . no H48 C27 H49 109.00 . . . no C27 C28 H46 110.00 . . . no C27 C28 H47 109.00 . . . no C27 C28 H45 110.00 . . . no H45 C28 H47 109.00 . . . no H46 C28 H47 109.00 . . . no H45 C28 H46 109.00 . . . no O1M C1M H65 110.00 . . . no O1M C1M H66 113.00 . . . no O1M C1M H67 111.00 . . . no H65 C1M H66 108.00 . . . no H65 C1M H67 107.00 . . . no H66 C1M H67 106.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 O1 2.9(4) . . . . no N2 Ni1 N1 C1 -177.5(4) . . . . no N2 Ni1 N1 O1 -177.1(4) 2_557 . . . no N2 Ni1 N1 C1 2.5(4) 2_557 . . . no N1 Ni1 N2 O2 -0.1(4) . . . . no N1 Ni1 N2 C2 179.3(4) . . . . no N1 Ni1 N2 O2 179.9(4) 2_557 . . . no N1 Ni1 N2 C2 -0.8(4) 2_557 . . . no Ni1 N1 C1 N3 176.1(5) . . . . no Ni1 N1 C1 C2 -4.7(6) . . . 2_557 no O1 N1 C1 N3 -4.2(9) . . . . no O1 N1 C1 C2 174.9(4) . . . 2_557 no Ni1 N2 C2 N4 -178.9(4) . . . . no Ni1 N2 C2 C1 3.3(6) . . . 2_557 no O2 N2 C2 N4 0.5(8) . . . . no O2 N2 C2 C1 -177.3(4) . . . 2_557 no C11 N3 C1 N1 -20.8(10) . . . . no C11 N3 C1 C2 160.1(6) . . . 2_557 no C1 N3 C11 C12 -68.8(8) . . . . no C21 N4 C2 N2 16.0(9) . . . . no C21 N4 C2 C1 -166.4(5) . . . 2_557 no C2 N4 C21 C22 71.4(8) . . . . no N1 C1 C2 N2 5.1(7) . . 2_557 2_557 no N1 C1 C2 N4 -176.9(5) . . 2_557 2_557 no N3 C1 C2 N2 -175.7(5) . . 2_557 2_557 no N3 C1 C2 N4 2.3(8) . . 2_557 2_557 no N3 C11 C12 C13 -179.4(6) . . . . no C11 C12 C13 C14 -176.4(7) . . . . no C12 C13 C14 C15 -179.0(7) . . . . no C13 C14 C15 C16 -177.9(8) . . . . no C14 C15 C16 C17 -178.2(8) . . . . no C15 C16 C17 C18 178.8(9) . . . . no N4 C21 C22 C23 173.8(5) . . . . no C21 C22 C23 C24 178.8(6) . . . . no C22 C23 C24 C25 176.4(7) . . . . no C23 C24 C25 C26 179.7(7) . . . . no C24 C25 C26 C27 178.1(8) . . . . no C25 C26 C27 C28 -178.3(9) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni1 C28 3.767(9) . 1_554 no Ni1 C28 3.767(10) . 2_558 no Ni1 H45 3.3000 . 1_554 no Ni1 H46 3.6400 . 1_554 no Ni1 H45 3.3000 . 2_558 no Ni1 H46 3.6400 . 2_558 no O1 O2 2.461(5) . . no O1 N2 2.967(6) . . no O1 N3 2.805(6) . . no O1 C11 2.830(7) . . no O1 C12 3.292(8) . . no O1 C18 3.388(10) . 2_548 no O1 O1M 2.651(7) . 2_557 no O1M N4 2.905(7) . 2_567 no O1M N3 2.901(7) . 1_565 no O1M O1 2.651(7) . 2_557 no O2 N4 2.801(6) . . no O2 O1 2.461(5) . . no O2 N1 2.979(6) . . no O2 C21 2.789(8) . . no O2 C22 3.198(8) . . no O1 H30 2.2900 . . no O1 H29 2.8000 . . no O1 H68 1.8500 . 2_557 no O1 H15 2.7000 . 2_548 no O1M H32 2.0500 . 1_565 no O1M H30 2.9200 . 2_557 no O1M H62 2.1000 . 2_567 no O2 H60 2.2700 . . no O2 H4 1.6700 . . no O2 H59 2.6600 . . no O2 H15 2.8000 . 2_548 no N1 N2 2.824(7) . . no N1 O2 2.979(6) . . no N1 N2 2.449(6) . 2_557 no N1 C2 2.316(7) . 2_557 no N2 N1 2.449(6) . 2_557 no N2 O1 2.967(6) . . no N2 N1 2.824(7) . . no N2 C1 2.299(7) . 2_557 no N3 O1M 2.901(7) . 1_545 no N3 O1 2.805(6) . . no N3 N3 3.201(7) . 2_547 no N3 N4 2.848(6) . 2_557 no N4 O2 2.801(6) . . no N4 O1M 2.905(7) . 2_567 no N4 N3 2.848(6) . 2_557 no N1 H68 2.5800 . 2_557 no N1 H30 2.9100 . . no N2 H60 2.9100 . . no N2 H4 2.3700 . . no N3 H62 2.4900 . 2_557 no N4 H65 2.9300 . 1_455 no N4 H32 2.5200 . 2_557 no C11 O1 2.830(7) . . no C12 O1 3.292(8) . . no C18 O1 3.388(10) . 2_548 no C21 O2 2.789(8) . . no C22 O2 3.198(8) . . no C28 Ni1 3.767(9) . 2_558 no C28 Ni1 3.767(9) . 1_556 no C1 H29 2.9300 . . no C1 H68 3.0800 . 2_557 no C2 H59 3.0400 . . no H4 N2 2.3700 . . no H4 O2 1.6700 . . no H4 H68 2.3300 . 2_557 no H4 H15 2.3800 . 2_548 no H15 O1 2.7000 . 2_548 no H15 H4 2.3800 . 2_548 no H15 O2 2.8000 . 2_548 no H16 H21 2.4600 . . no H17 H20 2.5600 . . no H18 H23 2.5200 . . no H19 H22 2.5700 . . no H20 H25 2.4700 . . no H20 H17 2.5600 . . no H21 H16 2.4600 . . no H21 H24 2.4900 . . no H22 H27 2.5600 . . no H22 H19 2.5700 . . no H23 H18 2.5200 . . no H23 H26 2.5800 . . no H24 H28 2.5100 . . no H24 H21 2.4900 . . no H25 H20 2.4700 . . no H25 H29 2.4800 . . no H26 H23 2.5800 . . no H26 H31 2.5300 . . no H27 H30 2.4700 . . no H27 H22 2.5600 . . no H28 H24 2.5100 . . no H29 C1 2.9300 . . no H29 O1 2.8000 . . no H29 H25 2.4800 . . no H30 H27 2.4700 . . no H30 O1 2.2900 . . no H30 N1 2.9100 . . no H30 H68 2.4500 . 2_557 no H30 O1M 2.9200 . 2_557 no H31 H26 2.5300 . . no H32 H62 1.9800 . 2_557 no H32 N4 2.5200 . 2_557 no H32 O1M 2.0500 . 1_545 no H32 H68 2.3200 . 1_545 no H45 Ni1 3.3000 . 1_556 no H45 Ni1 3.3000 . 2_558 no H46 H50 2.5100 . . no H46 Ni1 3.6400 . 1_556 no H46 Ni1 3.6400 . 2_558 no H47 H59 2.5400 . 2_558 no H47 H51 2.5200 . . no H48 H53 2.5600 . . no H49 H52 2.6000 . . no H50 H46 2.5100 . . no H50 H55 2.5300 . . no H51 H54 2.5700 . 2_558 no H51 H54 2.5700 . . no H51 H47 2.5200 . . no H52 H49 2.6000 . . no H52 H57 2.5800 . . no H53 H48 2.5600 . . no H53 H56 2.5200 . . no H54 H59 2.5500 . . no H54 H51 2.5700 . . no H54 H51 2.5700 . 2_558 no H55 H58 2.5300 . . no H55 H50 2.5300 . . no H56 H53 2.5200 . . no H56 H61 2.4900 . . no H57 H52 2.5800 . . no H57 H60 2.5600 . . no H58 H55 2.5300 . . no H59 H54 2.5500 . . no H59 H47 2.5400 . 2_558 no H59 O2 2.6600 . . no H59 C2 3.0400 . . no H60 H57 2.5600 . . no H60 O2 2.2700 . . no H60 N2 2.9100 . . no H61 H56 2.4900 . . no H62 H32 1.9800 . 2_557 no H62 O1M 2.1000 . 2_567 no H62 N3 2.4900 . 2_557 no H65 N4 2.9300 . 1_655 no H68 H32 2.3200 . 1_565 no H68 O1 1.8500 . 2_557 no H68 N1 2.5800 . 2_557 no H68 C1 3.0800 . 2_557 no H68 H4 2.3300 . 2_557 no H68 H30 2.4500 . 2_557 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O1 H4 O2 0.8300 1.6700 2.461(5) 159.00 . yes N3 H32 O1M 0.8600 2.0500 2.901(7) 171.00 1_545 yes N4 H62 O1M 0.8700 2.1000 2.905(7) 154.00 2_567 yes O1M H68 O1 0.8100 1.8500 2.651(7) 176.00 2_557 yes O1M H68 N1 0.8100 2.5800 3.327(7) 154.00 2_557 yes C11 H30 O1 0.9700 2.2900 2.830(7) 114.00 . yes C21 H60 O2 0.9700 2.2700 2.789(8) 113.00 . yes # Attachment 'VAC6Ni4.cif' data_VAC6Ni4 _database_code_depnum_ccdc_archive 'CCDC 660380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H58 N8 Ni O4' _chemical_formula_weight 629.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 27.3962(16) _cell_length_b 27.3962(16) _cell_length_c 12.6672(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8233.6(9) _cell_formula_units_Z 9 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3078 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 13959 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.90 _reflns_number_total 4275 _reflns_number_gt 2534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4275 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.5000 0.0000 0.0426(2) Uani 1 2 d S . . O1 O 0.40422(8) 0.41876(8) 0.11600(15) 0.0567(5) Uani 1 1 d . . . O2 O 0.53589(9) 0.49070(9) -0.20889(17) 0.0764(7) Uani 1 1 d . . . H2A H 0.5599 0.5225 -0.1906 0.115 Uiso 1 1 calc R . . N1 N 0.43525(9) 0.42997(9) 0.02644(17) 0.0462(5) Uani 1 1 d . . . N2 N 0.49670(9) 0.46536(9) -0.12841(18) 0.0519(6) Uani 1 1 d . . . N3 N 0.37395(10) 0.33936(10) -0.0449(2) 0.0587(7) Uani 1 1 d . . . H3A H 0.3553 0.3267 -0.1026 0.070 Uiso 1 1 calc R . . N4 N 0.44751(12) 0.37908(11) -0.2239(2) 0.0719(8) Uani 1 1 d . . . H4A H 0.4182 0.3461 -0.2197 0.086 Uiso 1 1 calc R . . C1 C 0.41961(11) 0.39226(11) -0.0474(2) 0.0456(6) Uani 1 1 d . . . C2 C 0.45709(12) 0.41362(11) -0.1415(2) 0.0499(7) Uani 1 1 d . . . C11 C 0.35415(16) 0.30274(13) 0.0453(3) 0.0743(10) Uani 1 1 d . . . H11A H 0.3242 0.2658 0.0237 0.089 Uiso 1 1 calc R . . H11B H 0.3388 0.3177 0.0966 0.089 Uiso 1 1 calc R . . C12 C 0.4015(2) 0.29685(19) 0.0966(4) 0.1099(15) Uani 1 1 d . . . H12A H 0.4161 0.2811 0.0452 0.132 Uiso 1 1 calc R . . H12B H 0.4320 0.3340 0.1154 0.132 Uiso 1 1 calc R . . C13 C 0.3840(3) 0.2613(2) 0.1908(5) 0.167(3) Uani 1 1 d . . . H13A H 0.3528 0.2243 0.1734 0.200 Uiso 1 1 calc R . . H13B H 0.3713 0.2778 0.2443 0.200 Uiso 1 1 calc R . . C14 C 0.4345(4) 0.2556(4) 0.2350(7) 0.224(5) Uani 1 1 d . . . H14A H 0.4443 0.2350 0.1852 0.269 Uiso 1 1 calc R . . H14B H 0.4672 0.2927 0.2447 0.269 Uiso 1 1 calc R . . C15 C 0.4188(6) 0.2271(7) 0.3311(10) 0.337(9) Uani 1 1 d . . . H15A H 0.4153 0.2512 0.3829 0.404 Uiso 1 1 calc R . . H15B H 0.3820 0.1938 0.3229 0.404 Uiso 1 1 calc R . . C16 C 0.4546(7) 0.2115(6) 0.3683(9) 0.316(8) Uani 1 1 d . . . H16A H 0.4403 0.1913 0.4334 0.475 Uiso 1 1 calc R . . H16B H 0.4907 0.2443 0.3806 0.475 Uiso 1 1 calc R . . H16C H 0.4585 0.1876 0.3177 0.475 Uiso 1 1 calc R . . C21 C 0.4816(2) 0.39132(17) -0.3207(3) 0.1028(16) Uani 1 1 d . . . H21A H 0.4705 0.4117 -0.3686 0.123 Uiso 1 1 calc R . . H21B H 0.5207 0.4165 -0.3019 0.123 Uiso 1 1 calc R . . C22 C 0.4789(6) 0.3497(4) -0.3711(7) 0.332(9) Uani 1 1 d . . . H22A H 0.5096 0.3665 -0.4216 0.398 Uiso 1 1 calc R . . H22B H 0.4446 0.3348 -0.4124 0.398 Uiso 1 1 calc R . . C23 C 0.4797(4) 0.3028(3) -0.3330(7) 0.209(4) Uani 1 1 d . . . H23A H 0.4472 0.2700 -0.3627 0.251 Uiso 1 1 calc R . . H23B H 0.4736 0.3016 -0.2574 0.251 Uiso 1 1 calc R . . C24 C 0.5268(4) 0.2955(4) -0.3492(8) 0.213(4) Uani 1 1 d . . . H24A H 0.5580 0.3235 -0.3076 0.256 Uiso 1 1 calc R . . H24B H 0.5377 0.3030 -0.4229 0.256 Uiso 1 1 calc R . . C25 C 0.5183(5) 0.2387(4) -0.3219(10) 0.259(6) Uani 1 1 d . . . H25A H 0.5076 0.2319 -0.2480 0.311 Uiso 1 1 calc R . . H25B H 0.4863 0.2111 -0.3624 0.311 Uiso 1 1 calc R . . C26 C 0.5604(5) 0.2281(6) -0.3363(13) 0.393(11) Uani 1 1 d . . . H26A H 0.5483 0.1899 -0.3160 0.590 Uiso 1 1 calc R . . H26B H 0.5921 0.2534 -0.2938 0.590 Uiso 1 1 calc R . . H26C H 0.5712 0.2333 -0.4094 0.590 Uiso 1 1 calc 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 Ni 0.0398(3) 0.0397(3) 0.0419(4) -0.0059(2) 0.0065(2) 0.0149(2) O1 0.0497(11) 0.0531(11) 0.0504(12) -0.0006(9) 0.0183(9) 0.0132(9) O2 0.0756(14) 0.0625(13) 0.0551(14) -0.0119(11) 0.0281(11) 0.0074(11) N1 0.0420(12) 0.0445(12) 0.0453(15) -0.0043(10) 0.0090(10) 0.0165(10) N2 0.0507(13) 0.0475(13) 0.0440(15) -0.0062(10) 0.0113(11) 0.0146(10) N3 0.0562(14) 0.0457(13) 0.0543(16) -0.0077(12) -0.0011(12) 0.0106(11) N4 0.0819(19) 0.0543(15) 0.0566(18) -0.0162(13) 0.0128(14) 0.0169(14) C1 0.0427(14) 0.0412(14) 0.0487(17) -0.0051(12) 0.0027(12) 0.0179(12) C2 0.0544(16) 0.0485(15) 0.0444(17) -0.0088(13) 0.0015(13) 0.0240(13) C11 0.082(2) 0.0449(17) 0.073(3) -0.0025(17) 0.0094(19) 0.0142(17) C12 0.147(4) 0.076(3) 0.093(3) 0.007(2) -0.017(3) 0.045(3) C13 0.266(9) 0.103(4) 0.111(5) 0.017(3) -0.024(5) 0.077(5) C14 0.345(14) 0.194(8) 0.167(8) 0.034(6) -0.072(8) 0.160(9) C15 0.328(18) 0.43(2) 0.326(18) 0.106(15) -0.031(13) 0.249(18) C16 0.45(2) 0.368(19) 0.231(13) 0.002(11) -0.076(13) 0.282(18) C21 0.146(4) 0.068(2) 0.056(3) -0.0189(19) 0.030(2) 0.025(2) C22 0.61(2) 0.271(11) 0.272(10) 0.165(9) 0.333(13) 0.340(14) C23 0.256(9) 0.170(6) 0.269(9) 0.084(6) 0.161(8) 0.157(7) C24 0.189(8) 0.211(9) 0.255(11) -0.016(8) 0.043(7) 0.112(8) C25 0.276(13) 0.209(10) 0.363(16) -0.028(10) -0.007(11) 0.174(10) C26 0.311(18) 0.44(2) 0.58(3) -0.214(19) -0.115(16) 0.296(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 1.862(2) . ? Ni N2 1.862(2) 10_665 ? Ni N1 1.881(2) . ? Ni N1 1.881(2) 10_665 ? O1 N1 1.358(3) . ? O2 N2 1.389(3) . ? O2 H2A 0.8200 . ? N1 C1 1.298(3) . ? N2 C2 1.295(3) . ? N3 C1 1.361(3) . ? N3 C11 1.436(4) . ? N3 H3A 0.8600 . ? N4 C2 1.344(3) . ? N4 C21 1.474(4) . ? N4 H4A 0.8600 . ? C1 C2 1.488(4) . ? C11 C12 1.530(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.462(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.571(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.392(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.337(14) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 C22 1.276(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.384(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.415(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.494(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.336(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni N2 180.00(15) . 10_665 ? N2 Ni N1 81.66(9) . . ? N2 Ni N1 98.34(9) 10_665 . ? N2 Ni N1 98.34(9) . 10_665 ? N2 Ni N1 81.66(9) 10_665 10_665 ? N1 Ni N1 180.0(2) . 10_665 ? N2 O2 H2A 109.5 . . ? C1 N1 O1 120.2(2) . . ? C1 N1 Ni 116.83(18) . . ? O1 N1 Ni 122.97(15) . . ? C2 N2 O2 117.9(2) . . ? C2 N2 Ni 118.05(19) . . ? O2 N2 Ni 123.92(17) . . ? C1 N3 C11 126.0(3) . . ? C1 N3 H3A 117.0 . . ? C11 N3 H3A 117.0 . . ? C2 N4 C21 127.4(3) . . ? C2 N4 H4A 116.3 . . ? C21 N4 H4A 116.3 . . ? N1 C1 N3 126.3(2) . . ? N1 C1 C2 112.1(2) . . ? N3 C1 C2 121.6(2) . . ? N2 C2 N4 129.2(3) . . ? N2 C2 C1 111.3(2) . . ? N4 C2 C1 119.4(2) . . ? N3 C11 C12 111.5(3) . . ? N3 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N3 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 113.8(5) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 110.1(7) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 109.1(10) . . ? C15 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C14 114.7(14) . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C21 N4 117.8(5) . . ? C22 C21 H21A 107.9 . . ? N4 C21 H21A 107.9 . . ? C22 C21 H21B 107.9 . . ? N4 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C21 C22 C23 129.4(10) . . ? C21 C22 H22A 104.9 . . ? C23 C22 H22A 104.9 . . ? C21 C22 H22B 104.9 . . ? C23 C22 H22B 104.9 . . ? H22A C22 H22B 105.8 . . ? C22 C23 C24 121.3(8) . . ? C22 C23 H23A 107.0 . . ? C24 C23 H23A 107.0 . . ? C22 C23 H23B 107.0 . . ? C24 C23 H23B 107.0 . . ? H23A C23 H23B 106.7 . . ? C23 C24 C25 115.8(9) . . ? C23 C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? C23 C24 H24B 108.3 . . ? C25 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C24 119.6(12) . . ? C26 C25 H25A 107.4 . . ? C24 C25 H25A 107.4 . . ? C26 C25 H25B 107.4 . . ? C24 C25 H25B 107.4 . . ? H25A C25 H25B 107.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 28.90 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.779 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.147 # Attachment 'VAC6Pd4.cif' data_VAC6Pd4 _database_code_depnum_ccdc_archive 'CCDC 660381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H58 N8 O4 Pd' _chemical_formula_weight 677.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 27.8737(19) _cell_length_b 27.8737(19) _cell_length_c 12.4102(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8350.2(12) _cell_formula_units_Z 9 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11101 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.1911 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 29.60 _reflns_number_total 4622 _reflns_number_gt 1752 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4622 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.651 _refine_ls_restrained_S_all 0.651 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.5000 0.5000 0.0000 0.0527(2) Uani 1 2 d S . . O1 O 0.40604(11) 0.41985(11) 0.1238(2) 0.0673(9) Uani 1 1 d . . . O2 O 0.53195(13) 0.48357(13) -0.2173(3) 0.0861(11) Uani 1 1 d . . . H2A H 0.5553 0.5153 -0.2006 0.129 Uiso 1 1 calc R . . N1 N 0.43370(14) 0.42778(14) 0.0309(3) 0.0571(9) Uani 1 1 d . . . N2 N 0.49367(15) 0.45978(15) -0.1341(3) 0.0633(10) Uani 1 1 d . . . N3 N 0.37353(15) 0.33765(15) -0.0368(3) 0.0725(11) Uani 1 1 d . . . H3A H 0.3539 0.3243 -0.0940 0.087 Uiso 1 1 calc R . . N4 N 0.44209(18) 0.37283(17) -0.2233(3) 0.0853(13) Uani 1 1 d . . . H4A H 0.4142 0.3401 -0.2144 0.102 Uiso 1 1 calc R . . C1 C 0.41851(17) 0.38989(18) -0.0436(4) 0.0579(12) Uani 1 1 d . . . C2 C 0.45390(19) 0.40885(19) -0.1415(4) 0.0603(12) Uani 1 1 d . . . C11 C 0.3563(3) 0.3032(2) 0.0571(5) 0.099(2) Uani 1 1 d . . . H11A H 0.3255 0.2670 0.0386 0.119 Uiso 1 1 calc R . . H11B H 0.3435 0.3193 0.1112 0.119 Uiso 1 1 calc R . . C12 C 0.4033(3) 0.2967(3) 0.1034(7) 0.143(3) Uani 1 1 d . . . H12A H 0.4165 0.2821 0.0472 0.172 Uiso 1 1 calc R . . H12B H 0.4335 0.3333 0.1216 0.172 Uiso 1 1 calc R . . C13 C 0.3908(5) 0.2622(4) 0.1962(9) 0.216(5) Uani 1 1 d . . . H13A H 0.3608 0.2255 0.1781 0.259 Uiso 1 1 calc R . . H13B H 0.3774 0.2767 0.2525 0.259 Uiso 1 1 calc R . . C14 C 0.4389(7) 0.2565(6) 0.2419(12) 0.266(8) Uani 1 1 d . . . H14A H 0.4509 0.2390 0.1892 0.319 Uiso 1 1 calc R . . H14B H 0.4700 0.2928 0.2583 0.319 Uiso 1 1 calc R . . C15 C 0.4215(10) 0.2251(13) 0.333(2) 0.408(17) Uani 1 1 d . . . H15A H 0.4161 0.2463 0.3892 0.490 Uiso 1 1 calc R . . H15B H 0.3859 0.1926 0.3190 0.490 Uiso 1 1 calc R . . C16 C 0.4527(11) 0.2103(11) 0.3668(17) 0.372(14) Uani 1 1 d . . . H16A H 0.4375 0.1887 0.4310 0.558 Uiso 1 1 calc R . . H16B H 0.4879 0.2422 0.3831 0.558 Uiso 1 1 calc R . . H16C H 0.4575 0.1882 0.3131 0.558 Uiso 1 1 calc R . . C21 C 0.4717(3) 0.3835(3) -0.3254(5) 0.125(3) Uani 1 1 d . . . H21A H 0.4470 0.3828 -0.3813 0.150 Uiso 1 1 calc R . . H21B H 0.5027 0.4211 -0.3223 0.150 Uiso 1 1 calc R . . C22 C 0.4900(7) 0.3542(6) -0.3561(11) 0.359(13) Uani 1 1 d . . . H22A H 0.5298 0.3788 -0.3553 0.431 Uiso 1 1 calc R . . H22B H 0.4797 0.3480 -0.4316 0.431 Uiso 1 1 calc R . . C23 C 0.4832(4) 0.3040(4) -0.3215(9) 0.199(4) Uani 1 1 d . . . H23A H 0.4502 0.2745 -0.3552 0.239 Uiso 1 1 calc R . . H23B H 0.4768 0.3012 -0.2444 0.239 Uiso 1 1 calc R . . C24 C 0.5298(5) 0.2939(5) -0.3437(12) 0.236(6) Uani 1 1 d . . . H24A H 0.5618 0.3203 -0.3026 0.283 Uiso 1 1 calc R . . H24B H 0.5393 0.3008 -0.4195 0.283 Uiso 1 1 calc R . . C25 C 0.5182(6) 0.2385(6) -0.3176(13) 0.260(7) Uani 1 1 d . . . H25A H 0.5074 0.2312 -0.2425 0.312 Uiso 1 1 calc R . . H25B H 0.4869 0.2123 -0.3605 0.312 Uiso 1 1 calc R . . C26 C 0.5626(6) 0.2288(7) -0.3349(15) 0.378(12) Uani 1 1 d . . . H26A H 0.5514 0.1913 -0.3154 0.568 Uiso 1 1 calc R . . H26B H 0.5936 0.2538 -0.2914 0.568 Uiso 1 1 calc R . . H26C H 0.5729 0.2346 -0.4095 0.568 Uiso 1 1 calc 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 Pd 0.0435(3) 0.0444(3) 0.0639(4) -0.0067(2) 0.0086(2) 0.0174(2) O1 0.0524(18) 0.0583(19) 0.078(2) -0.0032(16) 0.0215(17) 0.0177(16) O2 0.076(2) 0.070(2) 0.084(3) -0.0118(18) 0.031(2) 0.0154(18) N1 0.047(2) 0.050(2) 0.069(3) -0.005(2) 0.008(2) 0.0197(18) N2 0.055(2) 0.052(2) 0.068(3) -0.004(2) 0.016(2) 0.016(2) N3 0.059(3) 0.053(3) 0.085(3) -0.009(2) -0.004(2) 0.013(2) N4 0.092(3) 0.062(3) 0.078(3) -0.017(2) 0.015(3) 0.021(2) C1 0.046(3) 0.050(3) 0.075(3) -0.007(3) 0.003(2) 0.022(2) C2 0.057(3) 0.056(3) 0.070(3) -0.010(3) 0.005(3) 0.030(3) C11 0.104(5) 0.058(4) 0.103(5) 0.004(3) 0.013(4) 0.017(3) C12 0.159(8) 0.088(5) 0.160(8) 0.020(5) -0.029(6) 0.045(5) C13 0.294(15) 0.123(8) 0.196(10) 0.033(7) -0.032(10) 0.078(9) C14 0.36(2) 0.235(14) 0.225(14) 0.067(11) -0.069(14) 0.164(14) C15 0.32(3) 0.52(4) 0.36(3) 0.21(3) 0.00(2) 0.19(3) C16 0.49(4) 0.45(3) 0.27(2) 0.056(19) -0.02(2) 0.30(3) C21 0.186(8) 0.078(4) 0.072(5) -0.029(3) 0.019(5) 0.037(5) C22 0.61(3) 0.288(16) 0.356(19) 0.199(14) 0.36(2) 0.35(2) C23 0.207(10) 0.153(8) 0.277(12) 0.050(8) 0.100(9) 0.119(8) C24 0.181(10) 0.174(11) 0.358(18) -0.011(11) 0.064(11) 0.093(10) C25 0.244(15) 0.223(15) 0.358(19) -0.026(13) 0.037(13) 0.150(13) C26 0.33(2) 0.47(3) 0.51(3) -0.16(2) -0.081(19) 0.33(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N2 1.961(4) 10_665 ? Pd N2 1.961(4) . ? Pd N1 1.975(3) 10_665 ? Pd N1 1.975(3) . ? O1 N1 1.342(4) . ? O2 N2 1.392(4) . ? O2 H2A 0.8200 . ? N1 C1 1.303(5) . ? N2 C2 1.299(5) . ? N3 C1 1.368(5) . ? N3 C11 1.433(6) . ? N3 H3A 0.8600 . ? N4 C2 1.347(5) . ? N4 C21 1.458(7) . ? N4 H4A 0.8600 . ? C1 C2 1.481(6) . ? C11 C12 1.517(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.426(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.538(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.40(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.21(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 C22 1.224(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.384(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.485(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.456(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.414(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd N2 180.0(2) 10_665 . ? N2 Pd N1 79.07(15) 10_665 10_665 ? N2 Pd N1 100.93(15) . 10_665 ? N2 Pd N1 100.93(15) 10_665 . ? N2 Pd N1 79.07(15) . . ? N1 Pd N1 180.00(19) 10_665 . ? N2 O2 H2A 109.5 . . ? C1 N1 O1 123.4(3) . . ? C1 N1 Pd 116.5(3) . . ? O1 N1 Pd 120.1(3) . . ? C2 N2 O2 120.0(4) . . ? C2 N2 Pd 118.0(3) . . ? O2 N2 Pd 121.9(3) . . ? C1 N3 C11 125.8(4) . . ? C1 N3 H3A 117.1 . . ? C11 N3 H3A 117.1 . . ? C2 N4 C21 127.2(4) . . ? C2 N4 H4A 116.4 . . ? C21 N4 H4A 116.4 . . ? N1 C1 N3 124.8(4) . . ? N1 C1 C2 113.9(4) . . ? N3 C1 C2 121.3(4) . . ? N2 C2 N4 128.6(4) . . ? N2 C2 C1 112.5(4) . . ? N4 C2 C1 118.9(4) . . ? N3 C11 C12 111.7(5) . . ? N3 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N3 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 117.0(8) . . ? C13 C12 H12A 108.0 . . ? C11 C12 H12A 108.0 . . ? C13 C12 H12B 108.0 . . ? C11 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? C12 C13 C14 115.9(10) . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13B 108.3 . . ? C14 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 108.2(16) . . ? C15 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? C15 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C16 C15 C14 111(3) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C21 N4 121.2(7) . . ? C22 C21 H21A 107.0 . . ? N4 C21 H21A 107.0 . . ? C22 C21 H21B 107.0 . . ? N4 C21 H21B 107.0 . . ? H21A C21 H21B 106.8 . . ? C21 C22 C23 134.1(9) . . ? C21 C22 H22A 103.7 . . ? C23 C22 H22A 103.7 . . ? C21 C22 H22B 103.7 . . ? C23 C22 H22B 103.7 . . ? H22A C22 H22B 105.3 . . ? C22 C23 C24 116.3(10) . . ? C22 C23 H23A 108.2 . . ? C24 C23 H23A 108.2 . . ? C22 C23 H23B 108.2 . . ? C24 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C23 113.3(10) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 112.8(13) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.793 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.150