# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Sasankasekhar Mohanta' _publ_contact_author_email 'SM CU CHEM@YAHOO.CO.IN' _publ_section_title ; A unique example of three component cocrystal of metal complexes ; loop_ _publ_author_name 'Sasankasekhar Mohanta' 'Michel Fleck' 'Arpita Jana' 'Malabika Nayak' # Attachment '1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 744570' #TrackingRef '1.CIF' _audit_creation_method 'manual editing of SHELXL-97-output file' _chemical_melting_point 'not determined' _chemical_formula_moiety ? _chemical_formula_sum 'C100 H114 N12 Na2 Ni5 O28' _chemical_formula_weight 2271.56 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' Na Na 0.0362 0.0249 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.905(2) _cell_length_b 25.404(2) _cell_length_c 18.869(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.788(3) _cell_angle_gamma 90.00 _cell_volume 10019.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1220 _cell_measurement_theta_min 5.66 _cell_measurement_theta_max 19.85 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9702 _exptl_absorpt_process_details 'Otwinowski and Minor (1997)' _exptl_special_details ; Single-crystal X-ray intensity data were collected at 293 K on a Bruker X8 APEX-II diffractometer with CCD-area detector, using 933 frames with phi- and omega-increments of 0.5 degrees and a counting time of 220 seconds per frame. The crystal-to-detector-distance was 30mm. The whole ewald sphere was measured. The reflection data were processed with the program suite SAINT-Plus and corrected for Lorentz, polarisation, background and absorption effects (Bruker-Nonius, 2004). The crystal structure was determined by Direct methods (SHELXS-97, Sheldrick, 1997) and subsequent Fourier and difference Fourier syntheses, followed by full-matrix least-squares refinements on F^2^ (SHELXL-97, Sheldrick, 1997). Hydrogen atoms were treated as riding, except for water hydrogen atoms which were refined with a H-O-distance restraint. Using anisotropic treatment of the non-H atoms and isotropic treatment of the H atoms, the refinement converged at an R-value of 0.050. ; _diffrn_ambient_temperature 296(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-Nonius APEX-II diffractometer' _diffrn_measurement_method '\f-scan and \w-scans' _diffrn_detector_area_resol_mean 0.1 _diffrn_standards_number none _diffrn_reflns_number 54371 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.04 _reflns_number_total 9753 _reflns_number_gt 6626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT-Plus (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Bergerhoff et al.,1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0313P)^2^+33.6334P] 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 0 _refine_ls_number_reflns 9753 _refine_ls_number_parameters 672 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _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 Na1 Na 0.0000 0.08949(8) 0.2500 0.0525(5) Uani 1 2 d S . . Ni1 Ni 0.0000 0.21943(3) 0.2500 0.05010(19) Uani 1 2 d S . . C1 C 0.0517(3) -0.0139(2) 0.1537(3) 0.0957(17) Uani 1 1 d . . . H1A H 0.0715 -0.0153 0.1998 0.115 Uiso 1 1 calc R . . H1B H 0.0559 -0.0475 0.1309 0.115 Uiso 1 1 calc R . . H1C H 0.0072 -0.0055 0.1582 0.115 Uiso 1 1 calc R . . C2 C 0.0837(2) 0.02743(19) 0.1101(2) 0.0728(13) Uani 1 1 d . . . H2A H 0.1297 0.0224 0.1109 0.087 Uiso 1 1 calc R . . H2B H 0.0686 0.0258 0.0613 0.087 Uiso 1 1 calc R . . O1 O 0.06768(13) 0.07693(12) 0.14083(14) 0.0616(7) Uani 1 1 d . . . C3 C 0.09247(18) 0.12155(18) 0.11083(19) 0.0530(10) Uani 1 1 d . . . C4 C 0.1334(2) 0.1227(2) 0.0548(2) 0.0704(13) Uani 1 1 d . . . H4 H 0.1478 0.0913 0.0353 0.084 Uiso 1 1 calc R . . C5 C 0.1539(2) 0.1708(3) 0.0267(3) 0.0826(16) Uani 1 1 d . . . H5 H 0.1825 0.1712 -0.0107 0.099 Uiso 1 1 calc R . . C6 C 0.1321(2) 0.2164(2) 0.0539(2) 0.0751(15) Uani 1 1 d . . . H6 H 0.1446 0.2481 0.0337 0.090 Uiso 1 1 calc R . . C7 C 0.09077(18) 0.21699(19) 0.1122(2) 0.0583(11) Uani 1 1 d . . . C8 C 0.06966(17) 0.16911(17) 0.1419(2) 0.0498(10) Uani 1 1 d . . . O2 O 0.03071(12) 0.16567(10) 0.19452(14) 0.0541(7) Uani 1 1 d . . . C9 C 0.0690(2) 0.26621(19) 0.1402(3) 0.0652(13) Uani 1 1 d . . . H9 H 0.0826 0.2967 0.1177 0.078 Uiso 1 1 calc R . . N1 N 0.03233(16) 0.27172(13) 0.1936(2) 0.0597(9) Uani 1 1 d . . . C10 C 0.0093(3) 0.32487(18) 0.2124(3) 0.0866(17) Uani 1 1 d . . . H10A H 0.0428 0.3506 0.2049 0.104 Uiso 1 1 calc R . . H10B H -0.0272 0.3342 0.1827 0.104 Uiso 1 1 calc R . . O11 O 0.09731(14) 0.07409(12) 0.30957(16) 0.0580(7) Uani 1 1 d D . . H1W H 0.109(2) 0.1076(10) 0.319(3) 0.090(17) Uiso 1 1 d D . . H2W H 0.1304(18) 0.059(2) 0.287(3) 0.11(2) Uiso 1 1 d D . . Na2 Na 0.5000 0.16505(8) 0.2500 0.0576(6) Uani 1 2 d S . . Ni2 Ni 0.37149(2) 0.112084(18) 0.30842(2) 0.03923(13) Uani 1 1 d . . . C11 C 0.4615(2) 0.2997(2) 0.1204(3) 0.0813(15) Uani 1 1 d . . . H11A H 0.5039 0.2871 0.1308 0.098 Uiso 1 1 calc R . . H11B H 0.4639 0.3297 0.0896 0.098 Uiso 1 1 calc R . . H11C H 0.4371 0.2724 0.0976 0.098 Uiso 1 1 calc R . . C12 C 0.4298(2) 0.31526(17) 0.1878(3) 0.0713(13) Uani 1 1 d . . . H12A H 0.4551 0.3418 0.2122 0.086 Uiso 1 1 calc R . . H12B H 0.3877 0.3297 0.1776 0.086 Uiso 1 1 calc R . . O3 O 0.42432(13) 0.26944(10) 0.23104(15) 0.0582(7) Uani 1 1 d . . . C13 C 0.38675(18) 0.27285(15) 0.2905(2) 0.0497(10) Uani 1 1 d . . . C14 C 0.3662(2) 0.31906(17) 0.3209(2) 0.0628(12) Uani 1 1 d . . . H14 H 0.3782 0.3513 0.3019 0.075 Uiso 1 1 calc R . . C15 C 0.3271(2) 0.3173(2) 0.3802(3) 0.0712(14) Uani 1 1 d . . . H15 H 0.3139 0.3485 0.4013 0.085 Uiso 1 1 calc R . . C16 C 0.3084(2) 0.27070(19) 0.4072(2) 0.0637(12) Uani 1 1 d . . . H16 H 0.2815 0.2703 0.4461 0.076 Uiso 1 1 calc R . . C17 C 0.32874(17) 0.22264(16) 0.3779(2) 0.0499(10) Uani 1 1 d . . . C18 C 0.37024(16) 0.22333(15) 0.31954(19) 0.0430(9) Uani 1 1 d . . . O4 O 0.39369(11) 0.18104(9) 0.28974(12) 0.0444(6) Uani 1 1 d . . . C19 C 0.30327(18) 0.17428(18) 0.40370(19) 0.0524(10) Uani 1 1 d . . . H19 H 0.2750 0.1763 0.4412 0.063 Uiso 1 1 calc R . . N2 N 0.31598(14) 0.12814(14) 0.37970(15) 0.0485(8) Uani 1 1 d . . . C20 C 0.2787(2) 0.08176(18) 0.4031(2) 0.0635(12) Uani 1 1 d . . . H20A H 0.2661 0.0860 0.4520 0.076 Uiso 1 1 calc R . . H20B H 0.2405 0.0777 0.3739 0.076 Uiso 1 1 calc R . . C21 C 0.3207(2) 0.03518(18) 0.3957(2) 0.0624(12) Uani 1 1 d . . . H21A H 0.3503 0.0328 0.4357 0.075 Uiso 1 1 calc R . . H21B H 0.2954 0.0032 0.3937 0.075 Uiso 1 1 calc R . . N3 N 0.35595(14) 0.04241(12) 0.32910(15) 0.0449(7) Uani 1 1 d . . . C22 C 0.37502(18) 0.00174(15) 0.2944(2) 0.0487(9) Uani 1 1 d . . . H22 H 0.3639 -0.0312 0.3117 0.058 Uiso 1 1 calc R . . C23 C 0.41194(17) 0.00367(14) 0.23131(18) 0.0438(9) Uani 1 1 d . . . C24 C 0.4268(2) -0.04335(16) 0.1961(2) 0.0582(11) Uani 1 1 d . . . H24 H 0.4122 -0.0751 0.2143 0.070 Uiso 1 1 calc R . . C25 C 0.4617(2) -0.04350(17) 0.1363(2) 0.0650(12) Uani 1 1 d . . . H25 H 0.4719 -0.0751 0.1143 0.078 Uiso 1 1 calc R . . C26 C 0.4823(2) 0.00419(17) 0.1078(2) 0.0581(11) Uani 1 1 d . . . H26 H 0.5057 0.0042 0.0662 0.070 Uiso 1 1 calc R . . C27 C 0.46845(17) 0.05112(14) 0.14029(18) 0.0421(8) Uani 1 1 d . . . C28 C 0.43367(15) 0.05220(13) 0.20396(17) 0.0358(8) Uani 1 1 d . . . O5 O 0.42381(11) 0.09800(9) 0.23392(12) 0.0394(5) Uani 1 1 d . . . O6 O 0.48616(13) 0.10012(10) 0.11669(12) 0.0546(7) Uani 1 1 d . . . C29 C 0.5042(2) 0.10520(18) 0.0451(2) 0.0604(11) Uani 1 1 d . . . H29A H 0.4721 0.0891 0.0144 0.072 Uiso 1 1 calc R . . H29B H 0.5446 0.0875 0.0376 0.072 Uiso 1 1 calc R . . C30 C 0.5102(2) 0.16176(19) 0.0284(2) 0.0722(13) Uani 1 1 d . . . H30A H 0.4694 0.1786 0.0338 0.087 Uiso 1 1 calc R . . H30B H 0.5241 0.1658 -0.0195 0.087 Uiso 1 1 calc R . . H30C H 0.5408 0.1776 0.0602 0.087 Uiso 1 1 calc R . . Ni3 Ni 0.23802(2) 0.152560(18) 0.21378(2) 0.03964(13) Uani 1 1 d . . . C31 C 0.1472(3) -0.0469(2) 0.3856(3) 0.0861(16) Uani 1 1 d . . . H31A H 0.1802 -0.0339 0.4170 0.103 Uiso 1 1 calc R . . H31B H 0.1297 -0.0787 0.4047 0.103 Uiso 1 1 calc R . . H31C H 0.1140 -0.0210 0.3809 0.103 Uiso 1 1 calc R . . C32 C 0.1749(2) -0.05784(17) 0.3146(2) 0.0688(12) Uani 1 1 d . . . H32A H 0.2109 -0.0818 0.3193 0.083 Uiso 1 1 calc R . . H32B H 0.1429 -0.0740 0.2838 0.083 Uiso 1 1 calc R . . O7 O 0.19523(13) -0.00916(10) 0.28556(14) 0.0560(7) Uani 1 1 d . . . C33 C 0.22480(17) -0.00908(15) 0.22101(19) 0.0464(9) Uani 1 1 d . . . C34 C 0.2384(2) -0.05330(16) 0.1824(2) 0.0593(11) Uani 1 1 d . . . H34 H 0.2267 -0.0863 0.1993 0.071 Uiso 1 1 calc R . . C35 C 0.2697(2) -0.04903(18) 0.1181(2) 0.0694(13) Uani 1 1 d . . . H35 H 0.2777 -0.0791 0.0914 0.083 Uiso 1 1 calc R . . C36 C 0.2887(2) -0.00138(18) 0.0942(2) 0.0606(11) Uani 1 1 d . . . H36 H 0.3107 0.0009 0.0518 0.073 Uiso 1 1 calc R . . C37 C 0.27546(17) 0.04497(15) 0.13264(18) 0.0462(9) Uani 1 1 d . . . C38 C 0.24153(17) 0.04165(14) 0.19666(18) 0.0425(8) Uani 1 1 d . . . O8 O 0.22489(11) 0.08233(9) 0.23475(12) 0.0440(6) Uani 1 1 d . . . C39 C 0.30149(17) 0.09407(16) 0.10959(19) 0.0466(9) Uani 1 1 d . . . H39 H 0.3272 0.0937 0.0697 0.056 Uiso 1 1 calc R . . N4 N 0.29201(13) 0.13846(12) 0.13979(15) 0.0439(7) Uani 1 1 d . . . C40 C 0.32906(19) 0.18454(17) 0.1172(2) 0.0572(11) Uani 1 1 d . . . H40A H 0.3417 0.1808 0.0682 0.069 Uiso 1 1 calc R . . H40B H 0.3672 0.1885 0.1464 0.069 Uiso 1 1 calc R . . C41 C 0.2860(2) 0.23102(17) 0.1254(2) 0.0590(11) Uani 1 1 d . . . H41A H 0.3110 0.2631 0.1291 0.071 Uiso 1 1 calc R . . H41B H 0.2573 0.2340 0.0848 0.071 Uiso 1 1 calc R . . N5 N 0.24940(14) 0.22255(12) 0.19083(16) 0.0454(7) Uani 1 1 d . . . C42 C 0.22538(17) 0.26275(16) 0.2227(2) 0.0505(10) Uani 1 1 d . . . H42 H 0.2328 0.2958 0.2032 0.061 Uiso 1 1 calc R . . C43 C 0.18847(17) 0.26062(15) 0.2856(2) 0.0488(9) Uani 1 1 d . . . C44 C 0.17074(19) 0.30825(16) 0.3185(3) 0.0607(11) Uani 1 1 d . . . H44 H 0.1816 0.3401 0.2975 0.073 Uiso 1 1 calc R . . C45 C 0.1382(2) 0.30841(18) 0.3802(3) 0.0700(13) Uani 1 1 d . . . H45 H 0.1275 0.3402 0.4015 0.084 Uiso 1 1 calc R . . C46 C 0.1206(2) 0.26076(18) 0.4116(2) 0.0630(12) Uani 1 1 d . . . H46 H 0.0982 0.2610 0.4539 0.076 Uiso 1 1 calc R . . C47 C 0.13637(18) 0.21347(16) 0.3805(2) 0.0499(9) Uani 1 1 d . . . C48 C 0.17149(16) 0.21194(14) 0.31600(19) 0.0415(8) Uani 1 1 d . . . O9 O 0.18587(11) 0.16580(9) 0.28968(12) 0.0441(6) Uani 1 1 d . . . O10 O 0.12211(14) 0.16492(11) 0.40771(14) 0.0619(8) Uani 1 1 d . . . C49 C 0.0760(2) 0.1619(2) 0.4620(2) 0.0638(12) Uani 1 1 d . . . H49A H 0.0356 0.1764 0.4454 0.077 Uiso 1 1 calc R . . H49B H 0.0902 0.1821 0.5030 0.077 Uiso 1 1 calc R . . C50 C 0.0680(3) 0.1057(2) 0.4816(3) 0.0884(16) Uani 1 1 d . . . H50A H 0.0646 0.0847 0.4394 0.106 Uiso 1 1 calc R . . H50B H 0.0298 0.1016 0.5088 0.106 Uiso 1 1 calc R . . H50C H 0.1043 0.0943 0.5093 0.106 Uiso 1 1 calc R . . N6 N 0.1721(2) 0.37737(17) 0.0938(2) 0.0709(11) Uani 1 1 d . . . O12 O 0.1722(2) 0.38062(16) 0.1575(2) 0.1161(15) Uani 1 1 d . . . O13 O 0.2083(4) 0.3497(3) 0.0666(3) 0.213(3) Uani 1 1 d . . . O14 O 0.1298(3) 0.3926(3) 0.0603(3) 0.200(3) Uani 1 1 d . . . 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 Na1 0.0557(12) 0.0434(12) 0.0585(13) 0.000 0.0081(10) 0.000 Ni1 0.0481(4) 0.0387(4) 0.0633(5) 0.000 -0.0074(3) 0.000 C1 0.118(5) 0.062(3) 0.107(4) -0.022(3) 0.001(4) 0.011(3) C2 0.082(3) 0.073(3) 0.063(3) -0.020(3) -0.004(2) 0.017(3) O1 0.0700(19) 0.0588(19) 0.0564(17) -0.0091(15) 0.0105(14) 0.0036(15) C3 0.047(2) 0.074(3) 0.038(2) -0.001(2) -0.0014(17) -0.005(2) C4 0.065(3) 0.107(4) 0.040(2) -0.004(3) -0.001(2) 0.003(3) C5 0.064(3) 0.132(5) 0.051(3) 0.016(3) 0.003(2) -0.013(3) C6 0.065(3) 0.103(4) 0.058(3) 0.029(3) -0.009(2) -0.022(3) C7 0.045(2) 0.074(3) 0.056(3) 0.019(2) -0.0125(19) -0.017(2) C8 0.039(2) 0.066(3) 0.045(2) 0.008(2) -0.0089(17) -0.0036(18) O2 0.0571(16) 0.0498(17) 0.0556(16) 0.0058(13) 0.0120(14) 0.0001(13) C9 0.053(3) 0.061(3) 0.081(3) 0.028(3) -0.024(2) -0.022(2) N1 0.055(2) 0.043(2) 0.081(3) 0.0145(18) -0.0202(19) -0.0072(16) C10 0.086(4) 0.042(3) 0.130(5) 0.014(3) -0.028(4) -0.006(2) O11 0.0603(18) 0.0504(19) 0.0634(19) -0.0045(15) 0.0061(15) 0.0026(15) Na2 0.0467(12) 0.0436(12) 0.0829(16) 0.000 0.0206(11) 0.000 Ni2 0.0416(2) 0.0423(3) 0.0339(2) 0.0032(2) 0.00548(18) -0.0003(2) C11 0.068(3) 0.091(4) 0.085(4) 0.030(3) -0.002(3) -0.013(3) C12 0.075(3) 0.051(3) 0.087(3) 0.015(3) -0.017(3) -0.013(2) O3 0.0644(18) 0.0409(16) 0.0692(19) 0.0092(14) 0.0021(15) 0.0001(13) C13 0.047(2) 0.047(2) 0.055(2) -0.0075(19) -0.0140(18) 0.0058(17) C14 0.068(3) 0.043(2) 0.077(3) -0.009(2) -0.023(2) 0.011(2) C15 0.082(3) 0.064(3) 0.067(3) -0.026(3) -0.022(3) 0.032(3) C16 0.067(3) 0.073(3) 0.051(3) -0.018(2) -0.008(2) 0.030(2) C17 0.045(2) 0.060(3) 0.044(2) -0.0078(19) -0.0065(17) 0.0154(19) C18 0.0373(19) 0.049(2) 0.042(2) -0.0036(17) -0.0112(16) 0.0080(16) O4 0.0490(14) 0.0388(14) 0.0458(14) 0.0002(12) 0.0085(11) 0.0060(11) C19 0.046(2) 0.076(3) 0.035(2) -0.002(2) 0.0063(17) 0.015(2) N2 0.0428(17) 0.065(2) 0.0384(17) 0.0042(16) 0.0048(13) 0.0004(15) C20 0.059(3) 0.084(3) 0.048(2) 0.011(2) 0.018(2) -0.007(2) C21 0.067(3) 0.074(3) 0.046(2) 0.014(2) 0.010(2) -0.021(2) N3 0.0479(17) 0.050(2) 0.0371(16) 0.0081(15) 0.0059(13) -0.0080(15) C22 0.059(2) 0.037(2) 0.049(2) 0.0087(18) -0.0042(19) -0.0093(18) C23 0.052(2) 0.040(2) 0.039(2) 0.0046(16) -0.0042(16) -0.0006(17) C24 0.082(3) 0.037(2) 0.056(3) -0.0011(19) -0.004(2) -0.002(2) C25 0.098(3) 0.042(2) 0.055(3) -0.007(2) 0.001(2) 0.008(2) C26 0.075(3) 0.058(3) 0.041(2) -0.008(2) 0.007(2) 0.007(2) C27 0.056(2) 0.037(2) 0.0330(19) 0.0005(16) 0.0015(16) -0.0015(17) C28 0.0414(19) 0.0325(18) 0.0333(18) 0.0008(15) -0.0047(15) 0.0029(14) O5 0.0472(14) 0.0330(13) 0.0381(13) 0.0025(10) 0.0076(10) -0.0022(10) O6 0.0785(19) 0.0520(17) 0.0336(13) 0.0012(12) 0.0141(13) -0.0079(14) C29 0.069(3) 0.073(3) 0.039(2) 0.005(2) 0.0100(19) -0.001(2) C30 0.079(3) 0.084(4) 0.054(3) 0.017(2) 0.014(2) -0.015(3) Ni3 0.0436(3) 0.0377(3) 0.0376(2) 0.0029(2) 0.00126(19) -0.0046(2) C31 0.111(4) 0.076(4) 0.072(3) 0.024(3) 0.023(3) -0.014(3) C32 0.090(3) 0.044(3) 0.073(3) 0.014(2) 0.005(3) -0.010(2) O7 0.0751(18) 0.0377(15) 0.0557(17) 0.0038(12) 0.0176(14) -0.0048(13) C33 0.053(2) 0.040(2) 0.046(2) -0.0012(17) 0.0002(18) 0.0015(17) C34 0.071(3) 0.042(2) 0.065(3) -0.006(2) 0.005(2) -0.003(2) C35 0.092(3) 0.050(3) 0.066(3) -0.021(2) 0.007(3) 0.004(2) C36 0.070(3) 0.065(3) 0.047(2) -0.015(2) 0.012(2) 0.004(2) C37 0.049(2) 0.053(2) 0.037(2) -0.0027(18) 0.0003(16) -0.0005(18) C38 0.044(2) 0.042(2) 0.041(2) -0.0013(17) -0.0013(16) 0.0007(16) O8 0.0554(15) 0.0349(14) 0.0418(14) 0.0028(11) 0.0102(11) -0.0015(11) C39 0.045(2) 0.060(3) 0.0343(19) 0.0013(18) 0.0047(16) -0.0011(18) N4 0.0437(17) 0.050(2) 0.0382(16) 0.0062(15) -0.0016(13) -0.0082(14) C40 0.058(2) 0.064(3) 0.050(2) 0.009(2) 0.0096(19) -0.016(2) C41 0.064(3) 0.063(3) 0.051(2) 0.018(2) -0.007(2) -0.021(2) N5 0.0480(17) 0.0436(19) 0.0444(18) 0.0044(15) -0.0043(14) -0.0092(14) C42 0.046(2) 0.041(2) 0.063(3) 0.010(2) -0.0145(19) -0.0046(17) C43 0.041(2) 0.045(2) 0.061(2) -0.0020(19) -0.0121(18) 0.0031(17) C44 0.055(2) 0.039(2) 0.088(3) -0.006(2) -0.009(2) 0.0081(19) C45 0.065(3) 0.049(3) 0.096(4) -0.022(3) -0.004(3) 0.013(2) C46 0.058(3) 0.063(3) 0.068(3) -0.018(2) 0.001(2) 0.015(2) C47 0.047(2) 0.047(2) 0.056(2) -0.0063(19) -0.0015(18) 0.0053(18) C48 0.0380(19) 0.039(2) 0.047(2) -0.0017(17) -0.0094(16) 0.0050(15) O9 0.0468(14) 0.0364(14) 0.0492(15) 0.0004(11) 0.0044(11) -0.0004(11) O10 0.0719(19) 0.0581(19) 0.0563(17) -0.0041(14) 0.0213(14) 0.0073(15) C49 0.053(2) 0.093(4) 0.045(2) -0.010(2) 0.0044(19) 0.000(2) C50 0.108(4) 0.100(4) 0.059(3) 0.000(3) 0.024(3) -0.020(3) N6 0.084(3) 0.072(3) 0.057(3) -0.009(2) 0.007(2) 0.000(2) O12 0.190(5) 0.082(3) 0.077(3) -0.004(2) -0.003(3) 0.019(3) O13 0.261(8) 0.239(8) 0.140(5) 0.001(5) 0.092(5) 0.112(6) O14 0.142(5) 0.347(10) 0.109(4) 0.050(5) -0.023(3) 0.062(5) _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 Na1 O2 2.296(3) 2 ? Na1 O2 2.296(3) . ? Na1 O11 2.343(3) . ? Na1 O11 2.343(3) 2 ? Na1 O1 2.535(3) 2 ? Na1 O1 2.535(3) . ? Na1 Ni1 3.301(2) . ? Na1 H1W 2.66(4) . ? Ni1 N1 1.837(4) 2 ? Ni1 N1 1.837(4) . ? Ni1 O2 1.841(3) . ? Ni1 O2 1.841(3) 2 ? C1 C2 1.498(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.427(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O1 C3 1.372(5) . ? C3 C4 1.370(5) . ? C3 C8 1.428(6) . ? C4 C5 1.400(7) . ? C4 H4 0.9300 . ? C5 C6 1.351(7) . ? C5 H5 0.9300 . ? C6 C7 1.408(6) . ? C6 H6 0.9300 . ? C7 C8 1.413(6) . ? C7 C9 1.434(6) . ? C8 O2 1.295(4) . ? C9 N1 1.281(6) . ? C9 H9 0.9300 . ? N1 C10 1.479(6) . ? C10 C10 1.477(10) 2 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O11 H1W 0.906(19) . ? O11 H2W 0.908(19) . ? Na2 O5 2.349(3) . ? Na2 O5 2.349(3) 2_655 ? Na2 O4 2.390(2) 2_655 ? Na2 O4 2.390(2) . ? Na2 O6 3.019(3) . ? Na2 O6 3.019(3) 2_655 ? Na2 O3 3.106(3) . ? Na2 Ni2 3.2131(10) . ? Na2 Ni2 3.2131(10) 2_655 ? Ni2 O5 1.828(2) . ? Ni2 N2 1.834(3) . ? Ni2 N3 1.842(3) . ? Ni2 O4 1.847(2) . ? C11 C12 1.495(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 O3 1.427(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O3 C13 1.381(5) . ? C13 C14 1.378(5) . ? C13 C18 1.417(5) . ? C14 C15 1.395(6) . ? C14 H14 0.9300 . ? C15 C16 1.350(7) . ? C15 H15 0.9300 . ? C16 C17 1.409(5) . ? C16 H16 0.9300 . ? C17 C18 1.411(5) . ? C17 C19 1.427(6) . ? C18 O4 1.311(4) . ? C19 N2 1.286(5) . ? C19 H19 0.9300 . ? N2 C20 1.483(5) . ? C20 C21 1.481(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N3 1.477(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N3 C22 1.289(5) . ? C22 C23 1.429(5) . ? C22 H22 0.9300 . ? C23 C24 1.404(5) . ? C23 C28 1.414(5) . ? C24 C25 1.352(6) . ? C24 H24 0.9300 . ? C25 C26 1.396(6) . ? C25 H25 0.9300 . ? C26 C27 1.373(5) . ? C26 H26 0.9300 . ? C27 O6 1.375(4) . ? C27 C28 1.413(5) . ? C28 O5 1.311(4) . ? O6 C29 1.412(4) . ? C29 C30 1.477(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Ni3 N4 1.842(3) . ? Ni3 O9 1.843(2) . ? Ni3 N5 1.846(3) . ? Ni3 O8 1.849(2) . ? C31 C32 1.493(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O7 1.420(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? O7 C33 1.374(4) . ? C33 C34 1.371(5) . ? C33 C38 1.414(5) . ? C34 C35 1.391(6) . ? C34 H34 0.9300 . ? C35 C36 1.353(6) . ? C35 H35 0.9300 . ? C36 C37 1.413(5) . ? C36 H36 0.9300 . ? C37 C38 1.412(5) . ? C37 C39 1.431(5) . ? C38 O8 1.309(4) . ? C39 N4 1.280(5) . ? C39 H39 0.9300 . ? N4 C40 1.470(5) . ? C40 C41 1.494(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N5 1.478(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N5 C42 1.291(5) . ? C42 C43 1.425(5) . ? C42 H42 0.9300 . ? C43 C48 1.411(5) . ? C43 C44 1.412(5) . ? C44 C45 1.357(6) . ? C44 H44 0.9300 . ? C45 C46 1.399(6) . ? C45 H45 0.9300 . ? C46 C47 1.379(5) . ? C46 H46 0.9300 . ? C47 O10 1.370(5) . ? C47 C48 1.431(5) . ? C48 O9 1.310(4) . ? O10 C49 1.419(4) . ? C49 C50 1.486(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? N6 O14 1.146(6) . ? N6 O13 1.159(6) . ? N6 O12 1.205(5) . ? 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 O2 Na1 O2 65.10(14) 2 . ? O2 Na1 O11 99.69(11) 2 . ? O2 Na1 O11 96.50(11) . . ? O2 Na1 O11 96.50(11) 2 2 ? O2 Na1 O11 99.69(11) . 2 ? O11 Na1 O11 160.77(18) . 2 ? O2 Na1 O1 64.72(10) 2 2 ? O2 Na1 O1 129.73(12) . 2 ? O11 Na1 O1 94.58(10) . 2 ? O11 Na1 O1 83.00(10) 2 2 ? O2 Na1 O1 129.73(12) 2 . ? O2 Na1 O1 64.72(10) . . ? O11 Na1 O1 83.00(10) . . ? O11 Na1 O1 94.58(10) 2 . ? O1 Na1 O1 165.54(16) 2 . ? O2 Na1 Ni1 32.55(7) 2 . ? O2 Na1 Ni1 32.55(7) . . ? O11 Na1 Ni1 99.61(9) . . ? O11 Na1 Ni1 99.61(9) 2 . ? O1 Na1 Ni1 97.23(8) 2 . ? O1 Na1 Ni1 97.23(8) . . ? O2 Na1 H1W 82.7(8) 2 . ? O2 Na1 H1W 80.5(8) . . ? O11 Na1 H1W 19.6(6) . . ? O11 Na1 H1W 179.1(10) 2 . ? O1 Na1 H1W 96.2(10) 2 . ? O1 Na1 H1W 86.3(10) . . ? Ni1 Na1 H1W 80.0(6) . . ? N1 Ni1 N1 87.4(3) 2 . ? N1 Ni1 O2 178.33(15) 2 . ? N1 Ni1 O2 94.17(15) . . ? N1 Ni1 O2 94.17(15) 2 2 ? N1 Ni1 O2 178.33(15) . 2 ? O2 Ni1 O2 84.27(16) . 2 ? N1 Ni1 Na1 136.30(13) 2 . ? N1 Ni1 Na1 136.30(13) . . ? O2 Ni1 Na1 42.14(8) . . ? O2 Ni1 Na1 42.14(8) 2 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 106.6(4) . . ? O1 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? O1 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? C3 O1 C2 117.9(3) . . ? C3 O1 Na1 116.7(2) . . ? C2 O1 Na1 125.3(3) . . ? C4 C3 O1 125.4(4) . . ? C4 C3 C8 121.0(4) . . ? O1 C3 C8 113.5(3) . . ? C3 C4 C5 120.5(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.3(5) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C8 120.0(5) . . ? C6 C7 C9 119.8(4) . . ? C8 C7 C9 120.2(4) . . ? O2 C8 C7 124.4(4) . . ? O2 C8 C3 118.4(4) . . ? C7 C8 C3 117.2(4) . . ? C8 O2 Ni1 127.8(3) . . ? C8 O2 Na1 126.1(2) . . ? Ni1 O2 Na1 105.31(12) . . ? N1 C9 C7 125.5(4) . . ? N1 C9 H9 117.2 . . ? C7 C9 H9 117.2 . . ? C9 N1 C10 119.3(4) . . ? C9 N1 Ni1 127.3(3) . . ? C10 N1 Ni1 113.4(3) . . ? C10 C10 N1 108.8(3) 2 . ? C10 C10 H10A 109.9 2 . ? N1 C10 H10A 109.9 . . ? C10 C10 H10B 109.9 2 . ? N1 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? Na1 O11 H1W 100(3) . . ? Na1 O11 H2W 120(3) . . ? H1W O11 H2W 107(4) . . ? O5 Na2 O5 87.03(13) . 2_655 ? O5 Na2 O4 135.60(10) . 2_655 ? O5 Na2 O4 62.09(8) 2_655 2_655 ? O5 Na2 O4 62.09(8) . . ? O5 Na2 O4 135.60(10) 2_655 . ? O4 Na2 O4 160.43(15) 2_655 . ? O5 Na2 O6 55.88(8) . . ? O5 Na2 O6 76.61(9) 2_655 . ? O4 Na2 O6 84.85(8) 2_655 . ? O4 Na2 O6 105.99(8) . . ? O5 Na2 O6 76.61(9) . 2_655 ? O5 Na2 O6 55.88(8) 2_655 2_655 ? O4 Na2 O6 105.99(8) 2_655 2_655 ? O4 Na2 O6 84.85(8) . 2_655 ? O6 Na2 O6 113.75(12) . 2_655 ? O5 Na2 O3 105.12(8) . . ? O5 Na2 O3 167.80(9) 2_655 . ? O4 Na2 O3 107.05(10) 2_655 . ? O4 Na2 O3 54.32(8) . . ? O6 Na2 O3 109.13(8) . . ? O6 Na2 O3 127.25(7) 2_655 . ? O5 Na2 Ni2 34.10(5) . . ? O5 Na2 Ni2 102.75(8) 2_655 . ? O4 Na2 Ni2 164.63(10) 2_655 . ? O4 Na2 Ni2 34.72(6) . . ? O6 Na2 Ni2 89.20(6) . . ? O6 Na2 Ni2 63.66(6) 2_655 . ? O3 Na2 Ni2 88.29(5) . . ? O5 Na2 Ni2 102.75(8) . 2_655 ? O5 Na2 Ni2 34.10(5) 2_655 2_655 ? O4 Na2 Ni2 34.72(6) 2_655 2_655 ? O4 Na2 Ni2 164.63(10) . 2_655 ? O6 Na2 Ni2 63.66(6) . 2_655 ? O6 Na2 Ni2 89.20(6) 2_655 2_655 ? O3 Na2 Ni2 138.16(7) . 2_655 ? Ni2 Na2 Ni2 130.49(7) . 2_655 ? O5 Ni2 N2 176.80(12) . . ? O5 Ni2 N3 94.82(12) . . ? N2 Ni2 N3 86.74(14) . . ? O5 Ni2 O4 83.36(10) . . ? N2 Ni2 O4 95.28(13) . . ? N3 Ni2 O4 175.50(12) . . ? O5 Ni2 Na2 46.08(8) . . ? N2 Ni2 Na2 134.32(11) . . ? N3 Ni2 Na2 128.73(10) . . ? O4 Ni2 Na2 47.47(8) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 C11 108.2(4) . . ? O3 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O3 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C13 O3 C12 117.7(3) . . ? C13 O3 Na2 104.7(2) . . ? C12 O3 Na2 135.8(3) . . ? C14 C13 O3 125.2(4) . . ? C14 C13 C18 121.1(4) . . ? O3 C13 C18 113.8(3) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 119.2(4) . . ? C16 C17 C19 119.7(4) . . ? C18 C17 C19 120.9(3) . . ? O4 C18 C17 124.2(3) . . ? O4 C18 C13 117.9(3) . . ? C17 C18 C13 117.9(3) . . ? C18 O4 Ni2 126.8(2) . . ? C18 O4 Na2 128.9(2) . . ? Ni2 O4 Na2 97.81(11) . . ? N2 C19 C17 125.8(3) . . ? N2 C19 H19 117.1 . . ? C17 C19 H19 117.1 . . ? C19 N2 C20 120.5(3) . . ? C19 N2 Ni2 126.7(3) . . ? C20 N2 Ni2 112.4(3) . . ? C21 C20 N2 107.0(3) . . ? C21 C20 H20A 110.3 . . ? N2 C20 H20A 110.3 . . ? C21 C20 H20B 110.3 . . ? N2 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? N3 C21 C20 106.5(3) . . ? N3 C21 H21A 110.4 . . ? C20 C21 H21A 110.4 . . ? N3 C21 H21B 110.4 . . ? C20 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? C22 N3 C21 119.6(3) . . ? C22 N3 Ni2 127.3(2) . . ? C21 N3 Ni2 113.0(3) . . ? N3 C22 C23 124.8(3) . . ? N3 C22 H22 117.6 . . ? C23 C22 H22 117.6 . . ? C24 C23 C28 119.7(3) . . ? C24 C23 C22 119.4(3) . . ? C28 C23 C22 120.9(3) . . ? C25 C24 C23 121.5(4) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 119.4(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 O6 125.6(3) . . ? C26 C27 C28 120.7(3) . . ? O6 C27 C28 113.7(3) . . ? O5 C28 C27 118.0(3) . . ? O5 C28 C23 124.3(3) . . ? C27 C28 C23 117.7(3) . . ? C28 O5 Ni2 127.2(2) . . ? C28 O5 Na2 126.1(2) . . ? Ni2 O5 Na2 99.82(10) . . ? C27 O6 C29 118.0(3) . . ? C27 O6 Na2 104.36(18) . . ? C29 O6 Na2 136.3(2) . . ? O6 C29 C30 108.5(3) . . ? O6 C29 H29A 110.0 . . ? C30 C29 H29A 110.0 . . ? O6 C29 H29B 110.0 . . ? C30 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N4 Ni3 O9 178.24(12) . . ? N4 Ni3 N5 85.83(14) . . ? O9 Ni3 N5 94.93(12) . . ? N4 Ni3 O8 93.95(12) . . ? O9 Ni3 O8 85.34(10) . . ? N5 Ni3 O8 178.38(12) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O7 C32 C31 107.8(4) . . ? O7 C32 H32A 110.1 . . ? C31 C32 H32A 110.1 . . ? O7 C32 H32B 110.1 . . ? C31 C32 H32B 110.1 . . ? H32A C32 H32B 108.5 . . ? C33 O7 C32 119.0(3) . . ? C34 C33 O7 124.7(4) . . ? C34 C33 C38 121.4(4) . . ? O7 C33 C38 113.9(3) . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 120.9(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 119.6(4) . . ? C38 C37 C39 120.6(3) . . ? C36 C37 C39 119.5(3) . . ? O8 C38 C37 124.3(3) . . ? O8 C38 C33 118.2(3) . . ? C37 C38 C33 117.5(3) . . ? C38 O8 Ni3 127.1(2) . . ? N4 C39 C37 124.8(3) . . ? N4 C39 H39 117.6 . . ? C37 C39 H39 117.6 . . ? C39 N4 C40 119.1(3) . . ? C39 N4 Ni3 127.5(3) . . ? C40 N4 Ni3 113.3(3) . . ? N4 C40 C41 106.2(3) . . ? N4 C40 H40A 110.5 . . ? C41 C40 H40A 110.5 . . ? N4 C40 H40B 110.5 . . ? C41 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? N5 C41 C40 107.0(3) . . ? N5 C41 H41A 110.3 . . ? C40 C41 H41A 110.3 . . ? N5 C41 H41B 110.3 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C42 N5 C41 118.9(3) . . ? C42 N5 Ni3 126.9(3) . . ? C41 N5 Ni3 114.0(3) . . ? N5 C42 C43 125.2(4) . . ? N5 C42 H42 117.4 . . ? C43 C42 H42 117.4 . . ? C48 C43 C44 120.2(4) . . ? C48 C43 C42 120.9(3) . . ? C44 C43 C42 118.8(4) . . ? C45 C44 C43 121.2(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 119.9(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.5(4) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? O10 C47 C46 124.8(4) . . ? O10 C47 C48 114.3(3) . . ? C46 C47 C48 120.9(4) . . ? O9 C48 C43 124.7(3) . . ? O9 C48 C47 118.0(3) . . ? C43 C48 C47 117.2(3) . . ? C48 O9 Ni3 126.8(2) . . ? C47 O10 C49 118.2(3) . . ? O10 C49 C50 108.1(4) . . ? O10 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? O10 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O14 N6 O13 117.6(6) . . ? O14 N6 O12 121.2(6) . . ? O13 N6 O12 119.4(6) . . ? 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 O11 H2W O7 0.908(19) 2.19(4) 2.982(4) 145(5) . O11 H2W O8 0.908(19) 2.30(4) 3.042(4) 139(5) . O11 H1W O9 0.906(19) 2.26(3) 3.003(4) 140(4) . O11 H1W O10 0.906(19) 2.23(3) 3.000(4) 143(4) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.882 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.066