# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_b256 _database_code_depnum_ccdc_archive 'CCDC 918624' #TrackingRef 'web_deposit_cif_file_0_XiaoluSong_1360938597.b256.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H72 N6 Na6 O6 S6' _chemical_formula_weight 1591.78 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Na Na 0.0362 0.0249 '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 12.5133(8) _cell_length_b 13.8309(9) _cell_length_c 25.5673(16) _cell_angle_alpha 84.192(2) _cell_angle_beta 84.067(2) _cell_angle_gamma 65.0260(10) _cell_volume 3981.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5696 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.24 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8587 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52330 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18232 _reflns_number_gt 14456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0599P)^2^+1.7532P] 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 18232 _refine_ls_number_parameters 979 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.48999(8) 0.15434(7) 0.56724(3) 0.0327(2) Uani 1 1 d . . . Na2 Na 0.34728(7) 0.08693(7) 0.49867(3) 0.03139(19) Uani 1 1 d . . . Na3 Na 0.51227(8) 0.05435(8) 0.39118(3) 0.0366(2) Uani 1 1 d . . . Na4 Na -0.10401(8) 0.60005(7) 0.90329(4) 0.0350(2) Uani 1 1 d . . . Na5 Na 0.11459(7) 0.39887(7) 0.90791(3) 0.03090(19) Uani 1 1 d . . . Na6 Na -0.04782(8) 0.39641(8) 1.00312(3) 0.0391(2) Uani 1 1 d . . . S1 S 0.55448(6) 0.31348(6) 0.60724(3) 0.04842(17) Uani 1 1 d . . . S2 S 0.12473(6) 0.26251(6) 0.45992(3) 0.05078(18) Uani 1 1 d . . . S3 S 0.59612(6) 0.12225(6) 0.29179(3) 0.05000(17) Uani 1 1 d . . . S4 S -0.25839(6) 0.70364(6) 0.81956(3) 0.04505(16) Uani 1 1 d . . . S5 S 0.29824(5) 0.30995(5) 0.82732(3) 0.03981(15) Uani 1 1 d . . . S6 S -0.05464(7) 0.18052(6) 1.01418(3) 0.05224(18) Uani 1 1 d . . . O1 O 0.33493(13) 0.10546(12) 0.58908(6) 0.0320(3) Uani 1 1 d . . . O2 O 0.52310(13) 0.10872(12) 0.47567(6) 0.0315(3) Uani 1 1 d . . . O3 O 0.35674(13) 0.01484(12) 0.41882(6) 0.0332(3) Uani 1 1 d . . . O4 O 0.08493(13) 0.57521(12) 0.90873(6) 0.0315(3) Uani 1 1 d . . . O5 O -0.08182(13) 0.42663(12) 0.91625(6) 0.0319(3) Uani 1 1 d . . . O6 O 0.13975(13) 0.39443(12) 1.00073(6) 0.0337(3) Uani 1 1 d . . . N1 N 0.45529(17) 0.17035(16) 0.66142(7) 0.0354(4) Uani 1 1 d . . . N2 N 0.31095(18) 0.28933(16) 0.50426(8) 0.0399(5) Uani 1 1 d . . . N3 N 0.35980(17) 0.18094(16) 0.34137(8) 0.0380(4) Uani 1 1 d . . . N4 N -0.10567(16) 0.76758(15) 0.87113(8) 0.0343(4) Uani 1 1 d . . . N5 N 0.04626(16) 0.43883(16) 0.81717(7) 0.0338(4) Uani 1 1 d . . . N6 N 0.13445(19) 0.21600(16) 0.95512(9) 0.0434(5) Uani 1 1 d . . . C1 C 0.24776(19) 0.13854(17) 0.62481(9) 0.0316(5) Uani 1 1 d . . . C2 C 0.1366(2) 0.1416(2) 0.61645(10) 0.0409(6) Uani 1 1 d . . . H2 H 0.1258 0.1220 0.5839 0.049 Uiso 1 1 calc R . . C3 C 0.0432(2) 0.1722(2) 0.65402(11) 0.0498(7) Uani 1 1 d . . . H3 H -0.0291 0.1726 0.6467 0.060 Uiso 1 1 calc R . . C4 C 0.0548(2) 0.2023(2) 0.70261(12) 0.0550(8) Uani 1 1 d . . . H4 H -0.0088 0.2231 0.7283 0.066 Uiso 1 1 calc R . . C5 C 0.1603(2) 0.2012(2) 0.71216(10) 0.0498(7) Uani 1 1 d . . . H5 H 0.1685 0.2209 0.7451 0.060 Uiso 1 1 calc R . . C6 C 0.2579(2) 0.17173(19) 0.67476(9) 0.0355(5) Uani 1 1 d . . . C7 C 0.3628(2) 0.1768(2) 0.69066(9) 0.0387(5) Uani 1 1 d . . . H7 H 0.3636 0.1858 0.7266 0.046 Uiso 1 1 calc R . . C8 C 0.5515(2) 0.1687(2) 0.68688(9) 0.0369(5) Uani 1 1 d . . . C9 C 0.5950(2) 0.1008(2) 0.73072(10) 0.0472(6) Uani 1 1 d . . . H9 H 0.5576 0.0568 0.7451 0.057 Uiso 1 1 calc R . . C10 C 0.6924(3) 0.0962(3) 0.75384(11) 0.0591(8) Uani 1 1 d . . . H10 H 0.7213 0.0494 0.7834 0.071 Uiso 1 1 calc R . . C11 C 0.7464(2) 0.1615(3) 0.73281(12) 0.0583(8) Uani 1 1 d . . . H11 H 0.8119 0.1597 0.7486 0.070 Uiso 1 1 calc R . . C12 C 0.7056(2) 0.2289(2) 0.68925(11) 0.0502(7) Uani 1 1 d . . . H12 H 0.7431 0.2733 0.6756 0.060 Uiso 1 1 calc R . . C13 C 0.6092(2) 0.2325(2) 0.66489(10) 0.0390(5) Uani 1 1 d . . . C14 C 0.6826(3) 0.3293(3) 0.57666(13) 0.0610(8) Uani 1 1 d . . . H14A H 0.6958 0.3814 0.5946 0.092 Uiso 1 1 calc R . . H14B H 0.6702 0.3536 0.5399 0.092 Uiso 1 1 calc R . . H14C H 0.7511 0.2612 0.5789 0.092 Uiso 1 1 calc R . . C15 C 0.5632(2) 0.18048(19) 0.46008(8) 0.0321(5) Uani 1 1 d . . . C16 C 0.6811(2) 0.1501(2) 0.43917(10) 0.0459(6) Uani 1 1 d . . . H16 H 0.7297 0.0771 0.4359 0.055 Uiso 1 1 calc R . . C17 C 0.7276(3) 0.2236(3) 0.42339(11) 0.0579(8) Uani 1 1 d . . . H17 H 0.8069 0.1993 0.4102 0.070 Uiso 1 1 calc R . . C18 C 0.6606(3) 0.3313(3) 0.42648(12) 0.0605(8) Uani 1 1 d . . . H18 H 0.6929 0.3808 0.4154 0.073 Uiso 1 1 calc R . . C19 C 0.5455(3) 0.3650(2) 0.44614(12) 0.0562(7) Uani 1 1 d . . . H19 H 0.4989 0.4387 0.4481 0.067 Uiso 1 1 calc R . . C20 C 0.4941(2) 0.2931(2) 0.46360(10) 0.0401(5) Uani 1 1 d . . . C21 C 0.3737(2) 0.3391(2) 0.48659(10) 0.0438(6) Uani 1 1 d . . . H21 H 0.3383 0.4136 0.4886 0.053 Uiso 1 1 calc R . . C22 C 0.1990(2) 0.34752(19) 0.53071(10) 0.0441(6) Uani 1 1 d . . . C23 C 0.1882(3) 0.4047(2) 0.57393(12) 0.0623(8) Uani 1 1 d . . . H23 H 0.2546 0.4103 0.5849 0.075 Uiso 1 1 calc R . . C24 C 0.0782(4) 0.4537(3) 0.60102(15) 0.0832(11) Uani 1 1 d . . . H24 H 0.0704 0.4917 0.6307 0.100 Uiso 1 1 calc R . . C25 C -0.0188(3) 0.4465(3) 0.58414(16) 0.0811(11) Uani 1 1 d . . . H25 H -0.0927 0.4800 0.6025 0.097 Uiso 1 1 calc R . . C26 C -0.0097(3) 0.3913(2) 0.54099(13) 0.0618(8) Uani 1 1 d . . . H26 H -0.0772 0.3885 0.5295 0.074 Uiso 1 1 calc R . . C27 C 0.1003(2) 0.3393(2) 0.51435(11) 0.0460(6) Uani 1 1 d . . . C28 C -0.0142(3) 0.2546(3) 0.45827(18) 0.0855(12) Uani 1 1 d . . . H28A H -0.0329 0.2237 0.4918 0.128 Uiso 1 1 calc R . . H28B H -0.0093 0.2100 0.4304 0.128 Uiso 1 1 calc R . . H28C H -0.0756 0.3257 0.4517 0.128 Uiso 1 1 calc R . . C29 C 0.25974(19) 0.03101(18) 0.39833(9) 0.0341(5) Uani 1 1 d . . . C30 C 0.1903(2) -0.0235(2) 0.42054(12) 0.0477(6) Uani 1 1 d . . . H30 H 0.2147 -0.0692 0.4509 0.057 Uiso 1 1 calc R . . C31 C 0.0895(3) -0.0124(2) 0.39959(15) 0.0612(8) Uani 1 1 d . . . H31 H 0.0471 -0.0510 0.4155 0.073 Uiso 1 1 calc R . . C32 C 0.0488(2) 0.0546(3) 0.35546(15) 0.0647(9) Uani 1 1 d . . . H32 H -0.0194 0.0601 0.3406 0.078 Uiso 1 1 calc R . . C33 C 0.1097(2) 0.1131(2) 0.33356(12) 0.0545(7) Uani 1 1 d . . . H33 H 0.0811 0.1599 0.3039 0.065 Uiso 1 1 calc R . . C34 C 0.2140(2) 0.10498(19) 0.35419(10) 0.0389(5) Uani 1 1 d . . . C35 C 0.2621(2) 0.1791(2) 0.33146(9) 0.0409(6) Uani 1 1 d . . . H35 H 0.2171 0.2318 0.3067 0.049 Uiso 1 1 calc R . . C36 C 0.3822(2) 0.2707(2) 0.32360(9) 0.0413(6) Uani 1 1 d . . . C37 C 0.2971(3) 0.3746(2) 0.33098(11) 0.0538(7) Uani 1 1 d . . . H37 H 0.2203 0.3855 0.3444 0.065 Uiso 1 1 calc R . . C38 C 0.3245(3) 0.4606(3) 0.31888(13) 0.0654(8) Uani 1 1 d . . . H38 H 0.2667 0.5300 0.3242 0.078 Uiso 1 1 calc R . . C39 C 0.4365(3) 0.4457(3) 0.29903(13) 0.0673(9) Uani 1 1 d . . . H39 H 0.4548 0.5050 0.2910 0.081 Uiso 1 1 calc R . . C40 C 0.5222(3) 0.3438(3) 0.29085(11) 0.0578(8) Uani 1 1 d . . . H40 H 0.5982 0.3342 0.2768 0.069 Uiso 1 1 calc R . . C41 C 0.4962(2) 0.2561(2) 0.30332(9) 0.0421(6) Uani 1 1 d . . . C42 C 0.7389(3) 0.1225(3) 0.29290(12) 0.0684(9) Uani 1 1 d . . . H42A H 0.7524 0.1645 0.2623 0.103 Uiso 1 1 calc R . . H42B H 0.7990 0.0497 0.2922 0.103 Uiso 1 1 calc R . . H42C H 0.7425 0.1533 0.3247 0.103 Uiso 1 1 calc R . . C43 C 0.15164(19) 0.62069(18) 0.88680(8) 0.0308(5) Uani 1 1 d . . . C44 C 0.2756(2) 0.5700(2) 0.88949(10) 0.0427(6) Uani 1 1 d . . . H44 H 0.3090 0.5023 0.9074 0.051 Uiso 1 1 calc R . . C45 C 0.3495(2) 0.6155(2) 0.86706(12) 0.0523(7) Uani 1 1 d . . . H45 H 0.4316 0.5781 0.8693 0.063 Uiso 1 1 calc R . . C46 C 0.3037(2) 0.7162(3) 0.84113(12) 0.0576(8) Uani 1 1 d . . . H46 H 0.3541 0.7476 0.8258 0.069 Uiso 1 1 calc R . . C47 C 0.1841(2) 0.7689(2) 0.83833(11) 0.0511(7) Uani 1 1 d . . . H47 H 0.1530 0.8374 0.8210 0.061 Uiso 1 1 calc R . . C48 C 0.1058(2) 0.72454(19) 0.86038(9) 0.0366(5) Uani 1 1 d . . . C49 C -0.0185(2) 0.79152(19) 0.85647(9) 0.0379(5) Uani 1 1 d . . . H49 H -0.0377 0.8612 0.8413 0.045 Uiso 1 1 calc R . . C50 C -0.2212(2) 0.84984(18) 0.86907(9) 0.0372(5) Uani 1 1 d . . . C51 C -0.2529(2) 0.9465(2) 0.89155(11) 0.0500(7) Uani 1 1 d . . . H51 H -0.1957 0.9597 0.9070 0.060 Uiso 1 1 calc R . . C52 C -0.3675(3) 1.0228(2) 0.89131(14) 0.0635(8) Uani 1 1 d . . . H52 H -0.3885 1.0880 0.9065 0.076 Uiso 1 1 calc R . . C53 C -0.4510(3) 1.0037(2) 0.86894(14) 0.0669(9) Uani 1 1 d . . . H53 H -0.5289 1.0564 0.8686 0.080 Uiso 1 1 calc R . . C54 C -0.4221(2) 0.9081(2) 0.84686(12) 0.0565(8) Uani 1 1 d . . . H54 H -0.4804 0.8961 0.8317 0.068 Uiso 1 1 calc R . . C55 C -0.3065(2) 0.8291(2) 0.84698(10) 0.0406(6) Uani 1 1 d . . . C56 C -0.3895(3) 0.6806(3) 0.82463(12) 0.0598(8) Uani 1 1 d . . . H56A H -0.4254 0.6911 0.8603 0.090 Uiso 1 1 calc R . . H56B H -0.3695 0.6079 0.8161 0.090 Uiso 1 1 calc R . . H56C H -0.4448 0.7302 0.8002 0.090 Uiso 1 1 calc R . . C57 C -0.14638(19) 0.40318(17) 0.88762(9) 0.0318(5) Uani 1 1 d . . . C58 C -0.2413(2) 0.3798(2) 0.91166(11) 0.0420(6) Uani 1 1 d . . . H58 H -0.2548 0.3798 0.9485 0.050 Uiso 1 1 calc R . . C59 C -0.3135(2) 0.3575(2) 0.88285(13) 0.0552(7) Uani 1 1 d . . . H59 H -0.3754 0.3426 0.9002 0.066 Uiso 1 1 calc R . . C60 C -0.2969(2) 0.3564(3) 0.82858(13) 0.0633(9) Uani 1 1 d . . . H60 H -0.3465 0.3407 0.8090 0.076 Uiso 1 1 calc R . . C61 C -0.2069(2) 0.3787(2) 0.80389(12) 0.0544(7) Uani 1 1 d . . . H61 H -0.1957 0.3785 0.7670 0.065 Uiso 1 1 calc R . . C62 C -0.1299(2) 0.40210(19) 0.83198(10) 0.0372(5) Uani 1 1 d . . . C63 C -0.0406(2) 0.4262(2) 0.80045(9) 0.0371(5) Uani 1 1 d . . . H63 H -0.0462 0.4335 0.7638 0.045 Uiso 1 1 calc R . . C64 C 0.1172(2) 0.4711(2) 0.77893(9) 0.0373(5) Uani 1 1 d . . . C65 C 0.0686(3) 0.5578(2) 0.74310(10) 0.0527(7) Uani 1 1 d . . . H65 H -0.0138 0.5959 0.7433 0.063 Uiso 1 1 calc R . . C66 C 0.1412(3) 0.5887(3) 0.70690(12) 0.0688(9) Uani 1 1 d . . . H66 H 0.1079 0.6480 0.6830 0.083 Uiso 1 1 calc R . . C67 C 0.2618(3) 0.5321(3) 0.70632(12) 0.0690(9) Uani 1 1 d . . . H67 H 0.3107 0.5520 0.6814 0.083 Uiso 1 1 calc R . . C68 C 0.3115(3) 0.4468(3) 0.74184(11) 0.0557(7) Uani 1 1 d . . . H68 H 0.3940 0.4082 0.7407 0.067 Uiso 1 1 calc R . . C69 C 0.2403(2) 0.4172(2) 0.77948(9) 0.0378(5) Uani 1 1 d . . . C70 C 0.4424(2) 0.3042(2) 0.83485(14) 0.0598(8) Uani 1 1 d . . . H70A H 0.4961 0.2689 0.8056 0.090 Uiso 1 1 calc R . . H70B H 0.4717 0.2646 0.8677 0.090 Uiso 1 1 calc R . . H70C H 0.4371 0.3762 0.8353 0.090 Uiso 1 1 calc R . . C71 C 0.2517(2) 0.33204(19) 1.00343(8) 0.0331(5) Uani 1 1 d . . . C72 C 0.3298(2) 0.3691(2) 1.02219(10) 0.0467(6) Uani 1 1 d . . . H72 H 0.2995 0.4400 1.0320 0.056 Uiso 1 1 calc R . . C73 C 0.4477(3) 0.3055(3) 1.02661(12) 0.0616(8) Uani 1 1 d . . . H73 H 0.4957 0.3338 1.0393 0.074 Uiso 1 1 calc R . . C74 C 0.4969(3) 0.2020(3) 1.01288(14) 0.0693(9) Uani 1 1 d . . . H74 H 0.5776 0.1589 1.0164 0.083 Uiso 1 1 calc R . . C75 C 0.4263(2) 0.1623(2) 0.99392(13) 0.0590(8) Uani 1 1 d . . . H75 H 0.4598 0.0911 0.9844 0.071 Uiso 1 1 calc R . . C76 C 0.3047(2) 0.2247(2) 0.98822(10) 0.0395(5) Uani 1 1 d . . . C77 C 0.2424(2) 0.1739(2) 0.96475(11) 0.0447(6) Uani 1 1 d . . . H77 H 0.2865 0.1028 0.9559 0.054 Uiso 1 1 calc R . . C78 C 0.0899(2) 0.16012(19) 0.92644(11) 0.0455(6) Uani 1 1 d . . . C79 C 0.1348(3) 0.1302(2) 0.87609(12) 0.0605(8) Uani 1 1 d . . . H79 H 0.2028 0.1389 0.8618 0.073 Uiso 1 1 calc R . . C80 C 0.0801(4) 0.0873(3) 0.84633(14) 0.0766(11) Uani 1 1 d . . . H80 H 0.1102 0.0677 0.8119 0.092 Uiso 1 1 calc R . . C81 C -0.0186(4) 0.0740(3) 0.86783(15) 0.0750(10) Uani 1 1 d . . . H81 H -0.0567 0.0463 0.8477 0.090 Uiso 1 1 calc R . . C82 C -0.0622(3) 0.1008(2) 0.91859(13) 0.0595(8) Uani 1 1 d . . . H82 H -0.1287 0.0897 0.9330 0.071 Uiso 1 1 calc R . . C83 C -0.0089(2) 0.1437(2) 0.94835(11) 0.0458(6) Uani 1 1 d . . . C84 C -0.1880(3) 0.1605(3) 1.02647(14) 0.0705(9) Uani 1 1 d . . . H84A H -0.2420 0.2006 0.9996 0.106 Uiso 1 1 calc R . . H84B H -0.2245 0.1850 1.0608 0.106 Uiso 1 1 calc R . . H84C H -0.1694 0.0851 1.0257 0.106 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 Na1 0.0333(5) 0.0366(5) 0.0305(4) -0.0083(4) 0.0028(4) -0.0165(4) Na2 0.0262(4) 0.0379(5) 0.0310(4) -0.0096(4) 0.0016(3) -0.0135(4) Na3 0.0278(5) 0.0477(5) 0.0322(5) 0.0001(4) -0.0026(4) -0.0142(4) Na4 0.0331(5) 0.0344(5) 0.0419(5) 0.0035(4) -0.0076(4) -0.0185(4) Na5 0.0286(4) 0.0317(4) 0.0326(4) -0.0047(4) 0.0008(3) -0.0128(4) Na6 0.0397(5) 0.0574(6) 0.0306(5) -0.0060(4) -0.0002(4) -0.0301(5) S1 0.0462(4) 0.0468(4) 0.0582(4) -0.0029(3) -0.0069(3) -0.0244(3) S2 0.0321(3) 0.0493(4) 0.0652(4) -0.0221(3) -0.0001(3) -0.0081(3) S3 0.0396(4) 0.0604(4) 0.0419(4) -0.0039(3) 0.0040(3) -0.0143(3) S4 0.0337(3) 0.0576(4) 0.0442(4) -0.0070(3) -0.0043(3) -0.0181(3) S5 0.0284(3) 0.0422(3) 0.0513(4) -0.0106(3) 0.0042(3) -0.0170(3) S6 0.0524(4) 0.0601(4) 0.0533(4) 0.0007(3) -0.0022(3) -0.0335(4) O1 0.0265(8) 0.0409(9) 0.0284(8) -0.0117(7) 0.0050(6) -0.0133(7) O2 0.0297(8) 0.0340(8) 0.0328(8) -0.0060(6) 0.0031(6) -0.0154(7) O3 0.0241(8) 0.0400(9) 0.0345(8) -0.0077(7) -0.0029(6) -0.0110(7) O4 0.0313(8) 0.0314(8) 0.0353(8) -0.0008(6) -0.0012(6) -0.0171(7) O5 0.0320(8) 0.0357(8) 0.0338(8) -0.0050(6) -0.0017(6) -0.0195(7) O6 0.0275(8) 0.0383(9) 0.0356(8) -0.0067(7) -0.0012(6) -0.0134(7) N1 0.0322(10) 0.0453(11) 0.0323(10) -0.0126(8) 0.0040(8) -0.0186(9) N2 0.0350(11) 0.0336(10) 0.0469(12) -0.0056(9) -0.0026(9) -0.0096(9) N3 0.0333(11) 0.0408(11) 0.0346(10) -0.0032(9) -0.0014(8) -0.0103(9) N4 0.0310(10) 0.0314(10) 0.0392(11) 0.0019(8) -0.0015(8) -0.0130(8) N5 0.0279(10) 0.0421(11) 0.0320(10) -0.0078(8) 0.0006(8) -0.0146(8) N6 0.0420(12) 0.0359(11) 0.0578(13) -0.0050(10) -0.0025(10) -0.0214(10) C1 0.0303(11) 0.0320(11) 0.0319(11) -0.0080(9) 0.0065(9) -0.0130(9) C2 0.0344(13) 0.0480(14) 0.0440(14) -0.0168(11) 0.0041(10) -0.0192(11) C3 0.0286(13) 0.0609(17) 0.0646(18) -0.0233(14) 0.0099(12) -0.0220(12) C4 0.0380(14) 0.074(2) 0.0584(17) -0.0310(15) 0.0256(13) -0.0293(14) C5 0.0449(15) 0.0706(19) 0.0411(14) -0.0279(13) 0.0169(12) -0.0300(14) C6 0.0321(12) 0.0412(13) 0.0348(12) -0.0133(10) 0.0081(9) -0.0167(10) C7 0.0407(13) 0.0494(14) 0.0290(12) -0.0165(10) 0.0061(10) -0.0205(12) C8 0.0313(12) 0.0495(14) 0.0301(12) -0.0179(10) 0.0052(9) -0.0153(11) C9 0.0431(15) 0.0660(18) 0.0325(13) -0.0094(12) 0.0049(11) -0.0229(13) C10 0.0443(16) 0.087(2) 0.0399(15) -0.0107(15) -0.0041(12) -0.0196(16) C11 0.0381(15) 0.088(2) 0.0506(17) -0.0236(16) -0.0062(13) -0.0230(15) C12 0.0406(14) 0.0647(18) 0.0533(16) -0.0218(14) 0.0015(12) -0.0269(14) C13 0.0330(12) 0.0446(14) 0.0412(13) -0.0200(11) 0.0031(10) -0.0153(11) C14 0.0628(19) 0.067(2) 0.0644(19) -0.0006(15) 0.0005(15) -0.0397(17) C15 0.0345(12) 0.0458(13) 0.0213(10) -0.0016(9) -0.0032(9) -0.0216(11) C16 0.0396(14) 0.0622(17) 0.0405(14) -0.0072(12) 0.0039(11) -0.0262(13) C17 0.0524(17) 0.096(3) 0.0426(15) -0.0023(15) 0.0055(13) -0.0502(18) C18 0.074(2) 0.081(2) 0.0503(17) 0.0138(15) -0.0061(15) -0.059(2) C19 0.0662(19) 0.0517(17) 0.0601(18) 0.0147(14) -0.0134(15) -0.0357(15) C20 0.0413(14) 0.0418(14) 0.0395(13) 0.0068(11) -0.0089(11) -0.0204(11) C21 0.0465(15) 0.0299(12) 0.0542(16) 0.0008(11) -0.0103(12) -0.0145(11) C22 0.0444(14) 0.0299(12) 0.0497(15) -0.0079(11) 0.0008(12) -0.0073(11) C23 0.073(2) 0.0455(16) 0.0627(19) -0.0231(14) -0.0049(16) -0.0142(15) C24 0.100(3) 0.062(2) 0.075(2) -0.0408(19) 0.017(2) -0.019(2) C25 0.073(2) 0.058(2) 0.090(3) -0.0309(19) 0.035(2) -0.0089(18) C26 0.0447(16) 0.0442(16) 0.083(2) -0.0198(15) 0.0151(15) -0.0060(13) C27 0.0397(14) 0.0329(13) 0.0566(16) -0.0129(11) 0.0066(12) -0.0067(11) C28 0.0367(16) 0.084(3) 0.140(4) -0.048(2) -0.0076(19) -0.0196(17) C29 0.0260(11) 0.0343(12) 0.0411(13) -0.0184(10) 0.0008(9) -0.0089(9) C30 0.0366(14) 0.0442(15) 0.0647(18) -0.0154(13) -0.0001(12) -0.0173(12) C31 0.0400(15) 0.0553(18) 0.098(3) -0.0227(17) -0.0025(16) -0.0262(14) C32 0.0335(15) 0.067(2) 0.100(3) -0.0321(19) -0.0150(16) -0.0196(14) C33 0.0372(14) 0.0555(17) 0.0646(18) -0.0185(14) -0.0184(13) -0.0068(13) C34 0.0279(12) 0.0402(13) 0.0455(14) -0.0157(11) -0.0066(10) -0.0073(10) C35 0.0357(13) 0.0408(13) 0.0352(13) -0.0058(10) -0.0097(10) -0.0028(11) C36 0.0439(14) 0.0447(14) 0.0316(12) -0.0022(10) -0.0037(10) -0.0146(12) C37 0.0553(17) 0.0462(16) 0.0528(17) -0.0059(13) 0.0020(13) -0.0149(14) C38 0.073(2) 0.0477(17) 0.070(2) -0.0069(15) -0.0021(17) -0.0203(16) C39 0.090(3) 0.0567(19) 0.067(2) -0.0003(16) -0.0079(18) -0.0423(19) C40 0.0642(19) 0.072(2) 0.0469(16) -0.0055(14) -0.0020(14) -0.0372(17) C41 0.0466(15) 0.0510(15) 0.0279(12) -0.0015(11) -0.0043(10) -0.0193(12) C42 0.0437(17) 0.102(3) 0.0522(18) 0.0080(17) 0.0003(14) -0.0266(17) C43 0.0322(11) 0.0346(12) 0.0287(11) -0.0074(9) 0.0023(9) -0.0166(10) C44 0.0351(13) 0.0392(13) 0.0528(15) -0.0033(11) -0.0012(11) -0.0150(11) C45 0.0283(13) 0.0604(18) 0.0694(19) -0.0064(15) 0.0045(12) -0.0208(13) C46 0.0419(15) 0.0662(19) 0.070(2) 0.0038(15) 0.0119(14) -0.0331(15) C47 0.0447(15) 0.0492(16) 0.0591(17) 0.0095(13) 0.0061(13) -0.0241(13) C48 0.0346(12) 0.0401(13) 0.0373(12) -0.0001(10) 0.0036(10) -0.0194(11) C49 0.0392(13) 0.0330(12) 0.0414(13) 0.0060(10) 0.0025(10) -0.0179(11) C50 0.0333(12) 0.0336(12) 0.0415(13) 0.0064(10) 0.0012(10) -0.0135(10) C51 0.0488(16) 0.0354(14) 0.0609(17) -0.0004(12) 0.0070(13) -0.0159(12) C52 0.0553(19) 0.0369(15) 0.086(2) -0.0047(15) 0.0103(17) -0.0101(14) C53 0.0393(16) 0.0410(16) 0.096(3) 0.0083(16) 0.0045(16) 0.0025(13) C54 0.0326(14) 0.0586(18) 0.0692(19) 0.0120(15) -0.0057(13) -0.0132(13) C55 0.0332(12) 0.0397(13) 0.0419(13) 0.0084(11) -0.0003(10) -0.0112(11) C56 0.0464(16) 0.086(2) 0.0610(18) -0.0088(16) -0.0091(14) -0.0385(16) C57 0.0251(11) 0.0287(11) 0.0438(13) -0.0092(9) -0.0024(9) -0.0117(9) C58 0.0346(13) 0.0433(14) 0.0524(15) -0.0091(11) 0.0035(11) -0.0205(11) C59 0.0353(14) 0.0631(18) 0.081(2) -0.0199(16) 0.0059(14) -0.0324(14) C60 0.0378(15) 0.092(2) 0.078(2) -0.0378(18) -0.0012(14) -0.0380(16) C61 0.0387(14) 0.080(2) 0.0541(16) -0.0310(15) -0.0014(12) -0.0284(15) C62 0.0275(11) 0.0420(13) 0.0442(13) -0.0161(11) -0.0003(10) -0.0140(10) C63 0.0328(12) 0.0480(14) 0.0318(12) -0.0134(10) -0.0013(9) -0.0159(11) C64 0.0408(13) 0.0480(14) 0.0293(11) -0.0092(10) 0.0006(10) -0.0238(11) C65 0.0560(17) 0.0624(18) 0.0397(14) -0.0010(13) -0.0064(12) -0.0245(15) C66 0.089(3) 0.081(2) 0.0464(17) 0.0155(16) -0.0083(16) -0.048(2) C67 0.082(2) 0.100(3) 0.0487(17) 0.0040(17) 0.0083(16) -0.065(2) C68 0.0519(17) 0.079(2) 0.0496(16) -0.0121(15) 0.0117(13) -0.0419(16) C69 0.0395(13) 0.0487(14) 0.0338(12) -0.0126(10) 0.0053(10) -0.0263(12) C70 0.0265(13) 0.0504(17) 0.102(2) -0.0140(16) -0.0044(14) -0.0139(12) C71 0.0321(12) 0.0398(13) 0.0258(11) 0.0006(9) 0.0001(9) -0.0144(10) C72 0.0360(13) 0.0623(17) 0.0468(15) -0.0096(13) -0.0027(11) -0.0240(13) C73 0.0376(15) 0.089(2) 0.0630(19) -0.0090(17) -0.0082(14) -0.0291(16) C74 0.0275(14) 0.082(2) 0.088(2) -0.0053(19) -0.0108(15) -0.0108(15) C75 0.0369(15) 0.0458(16) 0.082(2) -0.0006(15) -0.0023(14) -0.0065(13) C76 0.0314(12) 0.0410(13) 0.0430(14) 0.0042(11) -0.0015(10) -0.0138(11) C77 0.0440(15) 0.0320(13) 0.0546(16) -0.0010(11) 0.0039(12) -0.0145(11) C78 0.0525(16) 0.0309(12) 0.0576(16) -0.0011(11) -0.0042(13) -0.0220(12) C79 0.079(2) 0.0512(17) 0.0653(19) -0.0132(14) 0.0139(16) -0.0422(17) C80 0.120(3) 0.066(2) 0.065(2) -0.0229(17) 0.011(2) -0.058(2) C81 0.106(3) 0.067(2) 0.083(2) -0.0199(18) -0.009(2) -0.061(2) C82 0.068(2) 0.0527(17) 0.075(2) -0.0101(15) -0.0006(16) -0.0414(16) C83 0.0523(16) 0.0345(13) 0.0572(16) -0.0005(12) -0.0050(13) -0.0248(12) C84 0.060(2) 0.086(2) 0.079(2) 0.0008(19) 0.0068(17) -0.0475(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 Na1 O1 2.3112(17) . ? Na1 O3 2.3375(17) 2_656 ? Na1 N1 2.418(2) . ? Na1 S1 2.9441(11) . ? Na1 Na3 2.9839(13) 2_656 ? Na1 Na2 3.5795(12) 2_656 ? Na2 O3 2.3320(17) . ? Na2 O1 2.3335(16) . ? Na2 O2 2.3523(16) . ? Na2 O2 2.5570(18) 2_656 ? Na2 S2 3.0012(11) . ? Na2 Na3 3.4420(12) 2_656 ? Na2 Na2 3.5573(17) 2_656 ? Na2 Na1 3.5795(12) 2_656 ? Na3 O3 2.2630(17) . ? Na3 O1 2.2805(18) 2_656 ? Na3 N3 2.357(2) . ? Na3 O2 2.3929(17) . ? Na3 S3 2.8702(11) . ? Na3 Na1 2.9839(13) 2_656 ? Na3 C1 3.083(2) 2_656 ? Na3 Na2 3.4420(12) 2_656 ? Na4 O4 2.2583(17) . ? Na4 O5 2.2881(17) . ? Na4 N4 2.371(2) . ? Na4 O6 2.4513(18) 2_567 ? Na4 C71 2.839(2) 2_567 ? Na4 S4 2.8749(11) . ? Na4 Na6 3.2217(12) 2_567 ? Na5 O4 2.3088(17) . ? Na5 O5 2.3119(17) . ? Na5 O6 2.4175(17) . ? Na5 N5 2.484(2) . ? Na5 N6 2.613(2) . ? Na5 S5 2.8612(10) . ? Na5 Na6 3.5780(13) 2_567 ? Na6 O5 2.2686(17) . ? Na6 O4 2.2929(17) 2_567 ? Na6 O6 2.3302(17) . ? Na6 O6 2.6186(19) 2_567 ? Na6 N6 2.858(2) . ? Na6 C43 3.006(2) 2_567 ? Na6 S6 3.0071(12) . ? Na6 Na4 3.2217(12) 2_567 ? Na6 Na6 3.5259(18) 2_567 ? Na6 Na5 3.5780(13) 2_567 ? S1 C13 1.767(3) . ? S1 C14 1.798(3) . ? S2 C27 1.759(3) . ? S2 C28 1.793(3) . ? S3 C41 1.777(3) . ? S3 C42 1.791(3) . ? S4 C55 1.772(3) . ? S4 C56 1.789(3) . ? S5 C69 1.769(3) . ? S5 C70 1.802(3) . ? S6 C83 1.774(3) . ? S6 C84 1.795(3) . ? O1 C1 1.300(2) . ? O1 Na3 2.2805(18) 2_656 ? O2 C15 1.302(3) . ? O2 Na2 2.5570(18) 2_656 ? O3 C29 1.295(3) . ? O3 Na1 2.3375(17) 2_656 ? O4 C43 1.297(3) . ? O4 Na6 2.2929(17) 2_567 ? O5 C57 1.298(3) . ? O6 C71 1.303(3) . ? O6 Na4 2.4513(18) 2_567 ? O6 Na6 2.6186(19) 2_567 ? N1 C7 1.286(3) . ? N1 C8 1.418(3) . ? N2 C21 1.270(3) . ? N2 C22 1.425(3) . ? N3 C35 1.285(3) . ? N3 C36 1.407(3) . ? N4 C49 1.279(3) . ? N4 C50 1.415(3) . ? N5 C63 1.290(3) . ? N5 C64 1.417(3) . ? N6 C77 1.265(3) . ? N6 C78 1.417(3) . ? C1 C2 1.412(3) . ? C1 C6 1.435(3) . ? C1 Na3 3.083(2) 2_656 ? C2 C3 1.378(3) . ? C3 C4 1.390(4) . ? C4 C5 1.361(4) . ? C5 C6 1.411(3) . ? C6 C7 1.444(3) . ? C8 C9 1.384(4) . ? C8 C13 1.404(3) . ? C9 C10 1.384(4) . ? C10 C11 1.379(4) . ? C11 C12 1.370(4) . ? C12 C13 1.394(3) . ? C15 C16 1.414(3) . ? C15 C20 1.435(3) . ? C16 C17 1.378(4) . ? C17 C18 1.374(5) . ? C18 C19 1.370(4) . ? C19 C20 1.411(4) . ? C20 C21 1.450(4) . ? C22 C23 1.386(4) . ? C22 C27 1.396(4) . ? C23 C24 1.394(5) . ? C24 C25 1.374(5) . ? C25 C26 1.373(5) . ? C26 C27 1.394(4) . ? C29 C30 1.418(3) . ? C29 C34 1.433(3) . ? C30 C31 1.364(4) . ? C31 C32 1.378(5) . ? C32 C33 1.374(4) . ? C33 C34 1.415(3) . ? C34 C35 1.442(4) . ? C36 C37 1.399(4) . ? C36 C41 1.403(4) . ? C37 C38 1.370(4) . ? C38 C39 1.375(5) . ? C39 C40 1.384(5) . ? C40 C41 1.383(4) . ? C43 C44 1.413(3) . ? C43 C48 1.427(3) . ? C43 Na6 3.006(2) 2_567 ? C44 C45 1.373(4) . ? C45 C46 1.388(4) . ? C46 C47 1.366(4) . ? C47 C48 1.407(3) . ? C48 C49 1.444(3) . ? C50 C51 1.391(4) . ? C50 C55 1.399(3) . ? C51 C52 1.377(4) . ? C52 C53 1.369(5) . ? C53 C54 1.380(5) . ? C54 C55 1.397(4) . ? C57 C62 1.417(3) . ? C57 C58 1.423(3) . ? C58 C59 1.369(4) . ? C59 C60 1.382(4) . ? C60 C61 1.367(4) . ? C61 C62 1.415(3) . ? C62 C63 1.444(3) . ? C64 C65 1.387(4) . ? C64 C69 1.401(3) . ? C65 C66 1.392(4) . ? C66 C67 1.375(5) . ? C67 C68 1.373(5) . ? C68 C69 1.392(3) . ? C71 C72 1.421(3) . ? C71 C76 1.424(3) . ? C71 Na4 2.839(2) 2_567 ? C72 C73 1.372(4) . ? C73 C74 1.366(5) . ? C74 C75 1.366(4) . ? C75 C76 1.411(4) . ? C76 C77 1.451(4) . ? C78 C79 1.381(4) . ? C78 C83 1.401(4) . ? C79 C80 1.394(4) . ? C80 C81 1.375(5) . ? C81 C82 1.378(5) . ? C82 C83 1.382(4) . ? 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 O1 Na1 O3 97.32(6) . 2_656 ? O1 Na1 N1 76.34(6) . . ? O3 Na1 N1 89.85(7) 2_656 . ? O1 Na1 S1 132.77(5) . . ? O3 Na1 S1 108.50(5) 2_656 . ? N1 Na1 S1 65.20(5) . . ? O1 Na1 Na3 49.02(4) . 2_656 ? O3 Na1 Na3 48.48(4) 2_656 2_656 ? N1 Na1 Na3 76.16(6) . 2_656 ? S1 Na1 Na3 135.58(4) . 2_656 ? O1 Na1 Na2 90.70(5) . 2_656 ? O3 Na1 Na2 39.90(4) 2_656 2_656 ? N1 Na1 Na2 126.49(6) . 2_656 ? S1 Na1 Na2 133.97(3) . 2_656 ? Na3 Na1 Na2 57.73(3) 2_656 2_656 ? O3 Na2 O1 160.83(7) . . ? O3 Na2 O2 92.35(6) . . ? O1 Na2 O2 98.52(6) . . ? O3 Na2 O2 81.40(6) . 2_656 ? O1 Na2 O2 83.41(6) . 2_656 ? O2 Na2 O2 87.22(6) . 2_656 ? O3 Na2 S2 83.94(5) . . ? O1 Na2 S2 104.93(5) . . ? O2 Na2 S2 116.42(5) . . ? O2 Na2 S2 152.65(5) 2_656 . ? O3 Na2 Na3 125.38(5) . 2_656 ? O1 Na2 Na3 41.17(4) . 2_656 ? O2 Na2 Na3 84.57(5) . 2_656 ? O2 Na2 Na3 44.01(4) 2_656 2_656 ? S2 Na2 Na3 144.72(3) . 2_656 ? O3 Na2 Na2 85.39(5) . 2_656 ? O1 Na2 Na2 90.88(5) . 2_656 ? O2 Na2 Na2 45.89(4) . 2_656 ? O2 Na2 Na2 41.34(4) 2_656 2_656 ? S2 Na2 Na2 158.86(5) . 2_656 ? Na3 Na2 Na2 54.58(3) 2_656 2_656 ? O3 Na2 Na1 40.01(4) . 2_656 ? O1 Na2 Na1 126.24(5) . 2_656 ? O2 Na2 Na1 81.36(4) . 2_656 ? O2 Na2 Na1 42.84(4) 2_656 2_656 ? S2 Na2 Na1 123.29(3) . 2_656 ? Na3 Na2 Na1 85.97(3) 2_656 2_656 ? Na2 Na2 Na1 51.22(3) 2_656 2_656 ? O3 Na3 O1 100.38(6) . 2_656 ? O3 Na3 N3 77.33(7) . . ? O1 Na3 N3 156.86(7) 2_656 . ? O3 Na3 O2 93.04(6) . . ? O1 Na3 O2 88.35(6) 2_656 . ? N3 Na3 O2 114.69(7) . . ? O3 Na3 S3 134.71(5) . . ? O1 Na3 S3 102.39(5) 2_656 . ? N3 Na3 S3 66.58(5) . . ? O2 Na3 S3 126.07(5) . . ? O3 Na3 Na1 50.66(5) . 2_656 ? O1 Na3 Na1 49.92(4) 2_656 2_656 ? N3 Na3 Na1 121.68(6) . 2_656 ? O2 Na3 Na1 94.77(5) . 2_656 ? S3 Na3 Na1 132.32(4) . 2_656 ? O3 Na3 C1 115.86(7) . 2_656 ? O1 Na3 C1 22.25(5) 2_656 2_656 ? N3 Na3 C1 139.83(7) . 2_656 ? O2 Na3 C1 102.78(6) . 2_656 ? S3 Na3 C1 80.19(5) . 2_656 ? Na1 Na3 C1 66.17(5) 2_656 2_656 ? O3 Na3 Na2 89.23(5) . 2_656 ? O1 Na3 Na2 42.35(4) 2_656 2_656 ? N3 Na3 Na2 158.00(6) . 2_656 ? O2 Na3 Na2 47.94(4) . 2_656 ? S3 Na3 Na2 132.72(3) . 2_656 ? Na1 Na3 Na2 56.84(3) 2_656 2_656 ? C1 Na3 Na2 61.87(5) 2_656 2_656 ? O4 Na4 O5 99.67(6) . . ? O4 Na4 N4 76.87(6) . . ? O5 Na4 N4 167.16(8) . . ? O4 Na4 O6 90.95(6) . 2_567 ? O5 Na4 O6 85.61(6) . 2_567 ? N4 Na4 O6 106.68(7) . 2_567 ? O4 Na4 C71 114.58(7) . 2_567 ? O5 Na4 C71 94.74(7) . 2_567 ? N4 Na4 C71 97.94(7) . 2_567 ? O6 Na4 C71 27.28(6) 2_567 2_567 ? O4 Na4 S4 129.20(5) . . ? O5 Na4 S4 108.78(5) . . ? N4 Na4 S4 66.06(5) . . ? O6 Na4 S4 131.44(5) 2_567 . ? C71 Na4 S4 104.18(5) 2_567 . ? O4 Na4 Na6 45.37(4) . 2_567 ? O5 Na4 Na6 99.06(5) . 2_567 ? N4 Na4 Na6 87.34(6) . 2_567 ? O6 Na4 Na6 46.07(4) 2_567 2_567 ? C71 Na4 Na6 69.47(5) 2_567 2_567 ? S4 Na4 Na6 151.97(4) . 2_567 ? O4 Na5 O5 97.51(6) . . ? O4 Na5 O6 83.70(6) . . ? O5 Na5 O6 97.00(6) . . ? O4 Na5 N5 88.35(6) . . ? O5 Na5 N5 73.83(6) . . ? O6 Na5 N5 167.02(7) . . ? O4 Na5 N6 152.18(7) . . ? O5 Na5 N6 80.17(6) . . ? O6 Na5 N6 69.22(6) . . ? N5 Na5 N6 116.97(7) . . ? O4 Na5 S5 105.49(5) . . ? O5 Na5 S5 132.20(5) . . ? O6 Na5 S5 126.35(5) . . ? N5 Na5 S5 65.74(5) . . ? N6 Na5 S5 95.97(6) . . ? O4 Na5 Na6 38.80(4) . 2_567 ? O5 Na5 Na6 89.27(5) . 2_567 ? O6 Na5 Na6 47.04(4) . 2_567 ? N5 Na5 Na6 122.33(6) . 2_567 ? N6 Na5 Na6 113.42(6) . 2_567 ? S5 Na5 Na6 133.63(3) . 2_567 ? O5 Na6 O4 156.82(7) . 2_567 ? O5 Na6 O6 100.77(6) . . ? O4 Na6 O6 93.25(6) 2_567 . ? O5 Na6 O6 82.17(6) . 2_567 ? O4 Na6 O6 79.62(6) 2_567 2_567 ? O6 Na6 O6 89.32(6) . 2_567 ? O5 Na6 N6 75.69(6) . . ? O4 Na6 N6 127.23(7) 2_567 . ? O6 Na6 N6 66.05(6) . . ? O6 Na6 N6 142.47(6) 2_567 . ? O5 Na6 C43 145.77(7) . 2_567 ? O4 Na6 C43 23.82(5) 2_567 2_567 ? O6 Na6 C43 113.11(6) . 2_567 ? O6 Na6 C43 93.16(6) 2_567 2_567 ? N6 Na6 C43 121.89(7) . 2_567 ? O5 Na6 S6 95.28(5) . . ? O4 Na6 S6 95.22(5) 2_567 . ? O6 Na6 S6 115.41(6) . . ? O6 Na6 S6 155.09(5) 2_567 . ? N6 Na6 S6 58.42(5) . . ? C43 Na6 S6 75.00(5) 2_567 . ? O5 Na6 Na4 148.43(5) . 2_567 ? O4 Na6 Na4 44.50(4) 2_567 2_567 ? O6 Na6 Na4 49.25(4) . 2_567 ? O6 Na6 Na4 87.20(4) 2_567 2_567 ? N6 Na6 Na4 96.03(5) . 2_567 ? C43 Na6 Na4 64.13(5) 2_567 2_567 ? S6 Na6 Na4 106.28(4) . 2_567 ? O5 Na6 Na6 91.28(5) . 2_567 ? O4 Na6 Na6 84.47(5) 2_567 2_567 ? O6 Na6 Na6 47.96(4) . 2_567 ? O6 Na6 Na6 41.36(4) 2_567 2_567 ? N6 Na6 Na6 108.70(6) . 2_567 ? C43 Na6 Na6 107.48(6) 2_567 2_567 ? S6 Na6 Na6 163.17(5) . 2_567 ? Na4 Na6 Na6 62.11(3) 2_567 2_567 ? O5 Na6 Na5 124.68(5) . 2_567 ? O4 Na6 Na5 39.12(4) 2_567 2_567 ? O6 Na6 Na5 81.93(5) . 2_567 ? O6 Na6 Na5 42.50(4) 2_567 2_567 ? N6 Na6 Na5 145.61(5) . 2_567 ? C43 Na6 Na5 58.92(5) 2_567 2_567 ? S6 Na6 Na5 133.74(3) . 2_567 ? Na4 Na6 Na5 51.44(2) 2_567 2_567 ? Na6 Na6 Na5 50.18(3) 2_567 2_567 ? C13 S1 C14 102.41(14) . . ? C13 S1 Na1 92.85(8) . . ? C14 S1 Na1 118.08(11) . . ? C27 S2 C28 102.40(15) . . ? C27 S2 Na2 93.87(9) . . ? C28 S2 Na2 125.89(14) . . ? C41 S3 C42 103.99(15) . . ? C41 S3 Na3 89.03(8) . . ? C42 S3 Na3 113.52(10) . . ? C55 S4 C56 103.16(14) . . ? C55 S4 Na4 90.99(8) . . ? C56 S4 Na4 114.44(11) . . ? C69 S5 C70 102.88(13) . . ? C69 S5 Na5 96.27(8) . . ? C70 S5 Na5 118.84(11) . . ? C83 S6 C84 102.90(15) . . ? C83 S6 Na6 98.81(8) . . ? C84 S6 Na6 123.97(13) . . ? C1 O1 Na3 116.13(14) . 2_656 ? C1 O1 Na1 130.98(14) . . ? Na3 O1 Na1 81.06(6) 2_656 . ? C1 O1 Na2 133.93(14) . . ? Na3 O1 Na2 96.48(6) 2_656 . ? Na1 O1 Na2 83.23(5) . . ? C15 O2 Na2 142.56(14) . . ? C15 O2 Na3 98.54(12) . . ? Na2 O2 Na3 85.16(6) . . ? C15 O2 Na2 124.47(14) . 2_656 ? Na2 O2 Na2 92.78(6) . 2_656 ? Na3 O2 Na2 88.05(6) . 2_656 ? C29 O3 Na3 133.79(15) . . ? C29 O3 Na2 119.39(13) . . ? Na3 O3 Na2 88.65(6) . . ? C29 O3 Na1 123.58(14) . 2_656 ? Na3 O3 Na1 80.86(6) . 2_656 ? Na2 O3 Na1 100.09(6) . 2_656 ? C43 O4 Na4 135.51(14) . . ? C43 O4 Na6 110.62(13) . 2_567 ? Na4 O4 Na6 90.12(6) . 2_567 ? C43 O4 Na5 128.39(14) . . ? Na4 O4 Na5 81.07(5) . . ? Na6 O4 Na5 102.07(6) 2_567 . ? C57 O5 Na6 133.02(14) . . ? C57 O5 Na4 114.03(14) . . ? Na6 O5 Na4 100.00(6) . . ? C57 O5 Na5 132.91(14) . . ? Na6 O5 Na5 82.25(6) . . ? Na4 O5 Na5 80.38(5) . . ? C71 O6 Na6 143.73(15) . . ? C71 O6 Na5 101.80(13) . . ? Na6 O6 Na5 78.75(5) . . ? C71 O6 Na4 93.17(12) . 2_567 ? Na6 O6 Na4 84.68(6) . 2_567 ? Na5 O6 Na4 163.20(7) . 2_567 ? C71 O6 Na6 125.43(14) . 2_567 ? Na6 O6 Na6 90.68(6) . 2_567 ? Na5 O6 Na6 90.46(6) . 2_567 ? Na4 O6 Na6 86.96(5) 2_567 2_567 ? C7 N1 C8 117.20(19) . . ? C7 N1 Na1 128.00(16) . . ? C8 N1 Na1 114.76(14) . . ? C21 N2 C22 118.4(2) . . ? C35 N3 C36 119.3(2) . . ? C35 N3 Na3 128.77(18) . . ? C36 N3 Na3 111.88(15) . . ? C49 N4 C50 118.1(2) . . ? C49 N4 Na4 129.03(16) . . ? C50 N4 Na4 112.82(14) . . ? C63 N5 C64 116.8(2) . . ? C63 N5 Na5 127.45(16) . . ? C64 N5 Na5 115.51(14) . . ? C77 N6 C78 119.4(2) . . ? C77 N6 Na5 101.22(16) . . ? C78 N6 Na5 113.06(16) . . ? C77 N6 Na6 126.39(18) . . ? C78 N6 Na6 112.96(16) . . ? Na5 N6 Na6 66.64(5) . . ? O1 C1 C2 120.8(2) . . ? O1 C1 C6 123.2(2) . . ? C2 C1 C6 116.0(2) . . ? O1 C1 Na3 41.62(10) . 2_656 ? C2 C1 Na3 125.62(15) . 2_656 ? C6 C1 Na3 101.72(14) . 2_656 ? C3 C2 C1 122.7(2) . . ? C2 C3 C4 120.7(2) . . ? C5 C4 C3 118.5(2) . . ? C4 C5 C6 122.9(2) . . ? C5 C6 C1 119.2(2) . . ? C5 C6 C7 116.0(2) . . ? C1 C6 C7 124.8(2) . . ? N1 C7 C6 127.5(2) . . ? C9 C8 C13 119.1(2) . . ? C9 C8 N1 121.8(2) . . ? C13 C8 N1 118.9(2) . . ? C10 C9 C8 121.4(3) . . ? C11 C10 C9 119.1(3) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 120.8(3) . . ? C12 C13 C8 118.9(2) . . ? C12 C13 S1 123.7(2) . . ? C8 C13 S1 117.42(18) . . ? O2 C15 C16 120.8(2) . . ? O2 C15 C20 123.5(2) . . ? C16 C15 C20 115.8(2) . . ? C17 C16 C15 122.5(3) . . ? C18 C17 C16 121.5(3) . . ? C19 C18 C17 118.4(3) . . ? C18 C19 C20 122.5(3) . . ? C19 C20 C15 119.5(2) . . ? C19 C20 C21 116.7(2) . . ? C15 C20 C21 123.7(2) . . ? N2 C21 C20 127.0(2) . . ? C23 C22 C27 120.2(3) . . ? C23 C22 N2 121.6(3) . . ? C27 C22 N2 118.1(2) . . ? C22 C23 C24 119.6(3) . . ? C25 C24 C23 119.8(3) . . ? C26 C25 C24 121.3(3) . . ? C25 C26 C27 119.6(3) . . ? C26 C27 C22 119.5(3) . . ? C26 C27 S2 124.2(2) . . ? C22 C27 S2 116.33(19) . . ? O3 C29 C30 120.1(2) . . ? O3 C29 C34 123.7(2) . . ? C30 C29 C34 116.2(2) . . ? C31 C30 C29 122.7(3) . . ? C30 C31 C32 121.1(3) . . ? C33 C32 C31 118.8(3) . . ? C32 C33 C34 122.1(3) . . ? C33 C34 C29 119.0(2) . . ? C33 C34 C35 116.7(2) . . ? C29 C34 C35 124.2(2) . . ? N3 C35 C34 127.1(2) . . ? C37 C36 C41 118.8(3) . . ? C37 C36 N3 121.4(2) . . ? C41 C36 N3 119.4(2) . . ? C38 C37 C36 120.6(3) . . ? C37 C38 C39 120.2(3) . . ? C38 C39 C40 120.4(3) . . ? C41 C40 C39 120.1(3) . . ? C40 C41 C36 119.8(3) . . ? C40 C41 S3 124.3(2) . . ? C36 C41 S3 115.7(2) . . ? O4 C43 C44 120.9(2) . . ? O4 C43 C48 123.0(2) . . ? C44 C43 C48 116.1(2) . . ? O4 C43 Na6 45.56(10) . 2_567 ? C44 C43 Na6 106.21(15) . 2_567 ? C48 C43 Na6 115.96(15) . 2_567 ? C45 C44 C43 122.8(2) . . ? C44 C45 C46 120.4(2) . . ? C47 C46 C45 118.7(2) . . ? C46 C47 C48 122.4(3) . . ? C47 C48 C43 119.5(2) . . ? C47 C48 C49 116.2(2) . . ? C43 C48 C49 124.2(2) . . ? N4 C49 C48 127.9(2) . . ? C51 C50 C55 120.0(2) . . ? C51 C50 N4 121.6(2) . . ? C55 C50 N4 118.2(2) . . ? C52 C51 C50 120.3(3) . . ? C53 C52 C51 120.0(3) . . ? C52 C53 C54 120.9(3) . . ? C53 C54 C55 120.2(3) . . ? C54 C55 C50 118.7(3) . . ? C54 C55 S4 124.4(2) . . ? C50 C55 S4 116.89(18) . . ? O5 C57 C62 123.2(2) . . ? O5 C57 C58 120.2(2) . . ? C62 C57 C58 116.6(2) . . ? C59 C58 C57 122.1(3) . . ? C58 C59 C60 121.0(3) . . ? C61 C60 C59 118.7(2) . . ? C60 C61 C62 122.3(3) . . ? C61 C62 C57 119.3(2) . . ? C61 C62 C63 116.0(2) . . ? C57 C62 C63 124.7(2) . . ? N5 C63 C62 127.1(2) . . ? C65 C64 C69 119.2(2) . . ? C65 C64 N5 122.1(2) . . ? C69 C64 N5 118.6(2) . . ? C64 C65 C66 120.5(3) . . ? C67 C66 C65 119.7(3) . . ? C68 C67 C66 120.7(3) . . ? C67 C68 C69 120.4(3) . . ? C68 C69 C64 119.5(3) . . ? C68 C69 S5 122.9(2) . . ? C64 C69 S5 117.61(18) . . ? O6 C71 C72 120.7(2) . . ? O6 C71 C76 123.9(2) . . ? C72 C71 C76 115.4(2) . . ? O6 C71 Na4 59.55(11) . 2_567 ? C72 C71 Na4 88.22(15) . 2_567 ? C76 C71 Na4 124.40(15) . 2_567 ? C73 C72 C71 122.6(3) . . ? C74 C73 C72 121.4(3) . . ? C73 C74 C75 118.7(3) . . ? C74 C75 C76 122.2(3) . . ? C75 C76 C71 119.8(2) . . ? C75 C76 C77 116.0(2) . . ? C71 C76 C77 124.1(2) . . ? N6 C77 C76 126.3(2) . . ? C79 C78 C83 119.7(3) . . ? C79 C78 N6 121.7(2) . . ? C83 C78 N6 118.4(2) . . ? C78 C79 C80 120.4(3) . . ? C81 C80 C79 119.3(3) . . ? C80 C81 C82 120.7(3) . . ? C81 C82 C83 120.4(3) . . ? C82 C83 C78 119.4(3) . . ? C82 C83 S6 125.2(2) . . ? C78 C83 S6 115.4(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.808 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.060 data_b300 _database_code_depnum_ccdc_archive 'CCDC 918625' #TrackingRef 'web_deposit_cif_file_1_XiaoluSong_1360938597.B300.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H54 Cl4 N6 Ni3 O4' _chemical_formula_weight 964.79 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' Cl Cl 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.031(8) _cell_length_b 17.991(14) _cell_length_c 21.829(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.77(2) _cell_angle_gamma 90.00 _cell_volume 4317(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1003 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 19.84 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6474 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25122 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7582 _reflns_number_gt 4917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. One of the (CH2)3 groups and two methyl groups were disordered into two positions with occupancy ratio=60:40.The following restraints were used: SADI 0.005 C35 C36 C35A C36A DFIX 1.52 0.005 C32 C33 C33 C34 C32A C33A C33A C34A SADI 0.001 N5 C32 N5 C32A N6 C34 N6 C34A sadi 0.001 N6 C35 N6 C36 N6 C35A N6 C36A isor 0.001 0.002 c35 c35A C36 c36A SIMU 0.001 0.001 C32 C33 C34 C32A C33A C34A C35 C35A C36 C36A DELU 0.01 0.01 C32 C33 C34 C32A C33A C34A C35 C35A C36 C36A ; _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^)+(0.0739P)^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 7582 _refine_ls_number_parameters 540 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.047 _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 C32A C -0.043(4) 0.1301(10) 0.1077(16) 0.0622(17) Uani 0.404(9) 1 d PDU A 2 H32C H -0.0270 0.1455 0.0657 0.075 Uiso 0.404(9) 1 calc PR A 2 H32D H -0.1324 0.1279 0.1103 0.075 Uiso 0.404(9) 1 calc PR A 2 C33A C 0.0149(12) 0.0550(12) 0.1235(11) 0.0622(17) Uani 0.404(9) 1 d PDU A 2 H33C H -0.0208 0.0175 0.0941 0.075 Uiso 0.404(9) 1 calc PR A 2 H33D H -0.0056 0.0402 0.1651 0.075 Uiso 0.404(9) 1 calc PR A 2 C34A C 0.1528(11) 0.0540(11) 0.1220(8) 0.0623(17) Uani 0.404(9) 1 d PDU A 2 H34C H 0.1782 0.0017 0.1291 0.075 Uiso 0.404(9) 1 calc PR A 2 H34D H 0.1691 0.0658 0.0792 0.075 Uiso 0.404(9) 1 calc PR A 2 C35A C 0.3602(10) 0.0826(11) 0.1395(8) 0.045(3) Uani 0.404(9) 1 d PDU A 2 H35D H 0.3796 0.0302 0.1479 0.068 Uiso 0.404(9) 1 calc PR A 2 H35E H 0.4236 0.1141 0.1603 0.068 Uiso 0.404(9) 1 calc PR A 2 H35F H 0.3562 0.0916 0.0951 0.068 Uiso 0.404(9) 1 calc PR A 2 C36A C 0.2400(19) 0.0720(11) 0.2269(5) 0.068(4) Uani 0.404(9) 1 d PDU A 2 H36D H 0.2660 0.0199 0.2280 0.103 Uiso 0.404(9) 1 calc PR A 2 H36E H 0.1576 0.0756 0.2403 0.103 Uiso 0.404(9) 1 calc PR A 2 H36F H 0.2959 0.1014 0.2543 0.103 Uiso 0.404(9) 1 calc PR A 2 C32 C -0.032(2) 0.1234(9) 0.1108(11) 0.0622(17) Uani 0.596(9) 1 d PDU A 1 H32A H -0.0452 0.1450 0.0690 0.075 Uiso 0.596(9) 1 calc PR A 1 H32B H -0.1114 0.1059 0.1229 0.075 Uiso 0.596(9) 1 calc PR A 1 C33 C 0.0530(13) 0.0566(9) 0.1081(6) 0.0623(17) Uani 0.596(9) 1 d PDU A 1 H33A H 0.0033 0.0112 0.1008 0.075 Uiso 0.596(9) 1 calc PR A 1 H33B H 0.1031 0.0628 0.0729 0.075 Uiso 0.596(9) 1 calc PR A 1 C34 C 0.1367(9) 0.0462(7) 0.1665(6) 0.0623(17) Uani 0.596(9) 1 d PDU A 1 H34A H 0.0923 0.0564 0.2032 0.075 Uiso 0.596(9) 1 calc PR A 1 H34B H 0.1680 -0.0053 0.1691 0.075 Uiso 0.596(9) 1 calc PR A 1 C35 C 0.3287(9) 0.0761(7) 0.1189(5) 0.045(3) Uani 0.596(9) 1 d PDU A 1 H35A H 0.3513 0.0242 0.1272 0.068 Uiso 0.596(9) 1 calc PR A 1 H35B H 0.4016 0.1074 0.1237 0.068 Uiso 0.596(9) 1 calc PR A 1 H35C H 0.2912 0.0806 0.0767 0.068 Uiso 0.596(9) 1 calc PR A 1 C36 C 0.3040(13) 0.0983(8) 0.2259(4) 0.068(4) Uani 0.596(9) 1 d PDU A 1 H36A H 0.3309 0.0474 0.2354 0.102 Uiso 0.596(9) 1 calc PR A 1 H36B H 0.2480 0.1144 0.2559 0.102 Uiso 0.596(9) 1 calc PR A 1 H36C H 0.3746 0.1315 0.2279 0.102 Uiso 0.596(9) 1 calc PR A 1 Ni1 Ni 0.28445(7) 0.32871(4) 0.06450(4) 0.0320(2) Uani 1 1 d . . . Ni2 Ni 0.29499(7) 0.35007(4) 0.19653(4) 0.0312(2) Uani 1 1 d . . . Ni3 Ni 0.18674(7) 0.21413(4) 0.14764(4) 0.0341(2) Uani 1 1 d . A . Cl1 Cl 0.18427(16) 0.21068(9) 0.03358(8) 0.0461(4) Uani 1 1 d . . . Cl2 Cl 0.62182(17) 0.17589(12) 0.16345(10) 0.0591(5) Uani 1 1 d . . . O1 O 0.3508(4) 0.4170(2) 0.11633(18) 0.0343(10) Uani 1 1 d . . . O2 O 0.1507(4) 0.3325(2) 0.13218(19) 0.0333(10) Uani 1 1 d . . . O3 O 0.2015(4) 0.2558(2) 0.2369(2) 0.0375(11) Uani 1 1 d . . . O4 O 0.3496(4) 0.2678(2) 0.1412(2) 0.0331(10) Uani 1 1 d . . . H4O H 0.421(6) 0.244(4) 0.142(3) 0.040 Uiso 1 1 d . . . N5 N 0.0148(5) 0.1839(3) 0.1549(3) 0.0445(14) Uani 1 1 d D . . N3 N 0.2063(5) 0.4355(3) 0.2344(2) 0.0379(13) Uani 1 1 d . . . N1 N 0.1928(5) 0.3954(3) 0.0030(2) 0.0385(13) Uani 1 1 d . . . C1 C 0.3092(6) 0.4863(4) 0.1095(3) 0.0368(16) Uani 1 1 d . . . C2 C 0.3618(8) 0.5408(4) 0.1488(3) 0.057(2) Uani 1 1 d . . . H2 H 0.4306 0.5281 0.1759 0.068 Uiso 1 1 calc R . . C3 C 0.3165(9) 0.6134(5) 0.1495(4) 0.074(3) Uani 1 1 d . . . H3 H 0.3534 0.6491 0.1772 0.089 Uiso 1 1 calc R . . C4 C 0.2169(9) 0.6331(4) 0.1093(4) 0.073(3) Uani 1 1 d . . . H4 H 0.1807 0.6808 0.1116 0.088 Uiso 1 1 calc R . . C5 C 0.1718(8) 0.5817(4) 0.0660(4) 0.062(2) Uani 1 1 d . . . H5 H 0.1089 0.5966 0.0361 0.075 Uiso 1 1 calc R . . C6 C 0.2157(6) 0.5083(4) 0.0645(3) 0.0441(17) Uani 1 1 d . . . C7 C 0.1684(6) 0.4633(4) 0.0127(3) 0.0458(18) Uani 1 1 d . . . H7 H 0.1138 0.4870 -0.0171 0.055 Uiso 1 1 calc R . . C8 C 0.1600(7) 0.3639(4) -0.0589(3) 0.053(2) Uani 1 1 d . . . H8A H 0.1017 0.3971 -0.0825 0.064 Uiso 1 1 calc R . . H8B H 0.1212 0.3146 -0.0552 0.064 Uiso 1 1 calc R . . C9 C 0.2760(7) 0.3563(5) -0.0918(3) 0.057(2) Uani 1 1 d . . . H9A H 0.3139 0.4060 -0.0942 0.068 Uiso 1 1 calc R . . H9B H 0.2537 0.3394 -0.1345 0.068 Uiso 1 1 calc R . . C10 C 0.3707(7) 0.3022(4) -0.0614(3) 0.051(2) Uani 1 1 d . . . H10A H 0.3327 0.2524 -0.0600 0.062 Uiso 1 1 calc R . . H10B H 0.4388 0.2983 -0.0880 0.062 Uiso 1 1 calc R . . N2 N 0.4222(5) 0.3214(3) 0.0019(2) 0.0417(14) Uani 1 1 d . . . C11 C 0.4917(7) 0.3942(4) 0.0016(3) 0.056(2) Uani 1 1 d . . . H11A H 0.5583 0.3896 -0.0252 0.083 Uiso 1 1 calc R . . H11B H 0.5252 0.4060 0.0435 0.083 Uiso 1 1 calc R . . H11C H 0.4366 0.4341 -0.0137 0.083 Uiso 1 1 calc R . . C12 C 0.5094(7) 0.2620(5) 0.0234(4) 0.064(2) Uani 1 1 d . . . H12A H 0.4661 0.2146 0.0252 0.097 Uiso 1 1 calc R . . H12B H 0.5468 0.2745 0.0644 0.097 Uiso 1 1 calc R . . H12C H 0.5729 0.2577 -0.0053 0.097 Uiso 1 1 calc R . . C13 C 0.0398(5) 0.3638(4) 0.1296(3) 0.0345(15) Uani 1 1 d . . . C14 C -0.0524(6) 0.3358(4) 0.0868(3) 0.0467(18) Uani 1 1 d . . . H14 H -0.0333 0.2980 0.0587 0.056 Uiso 1 1 calc R . . C15 C -0.1705(6) 0.3627(5) 0.0853(4) 0.058(2) Uani 1 1 d . . . H15 H -0.2325 0.3413 0.0580 0.070 Uiso 1 1 calc R . . C16 C -0.1991(7) 0.4220(5) 0.1244(4) 0.059(2) Uani 1 1 d . . . H16 H -0.2795 0.4412 0.1232 0.071 Uiso 1 1 calc R . . C17 C -0.1081(6) 0.4511(4) 0.1641(4) 0.055(2) Uani 1 1 d . . . H17 H -0.1264 0.4918 0.1895 0.066 Uiso 1 1 calc R . . C18 C 0.0125(6) 0.4225(4) 0.1685(3) 0.0408(17) Uani 1 1 d . . . C19 C 0.0976(6) 0.4561(4) 0.2159(3) 0.0468(18) Uani 1 1 d . . . H19 H 0.0685 0.4988 0.2356 0.056 Uiso 1 1 calc R . . C20 C 0.2590(6) 0.4806(4) 0.2880(3) 0.0489(19) Uani 1 1 d . . . H20A H 0.2393 0.5336 0.2799 0.059 Uiso 1 1 calc R . . H20B H 0.2187 0.4656 0.3249 0.059 Uiso 1 1 calc R . . C21 C 0.3937(7) 0.4736(5) 0.3020(4) 0.072(3) Uani 1 1 d . . . H21A H 0.4327 0.4966 0.2674 0.087 Uiso 1 1 calc R . . H21B H 0.4162 0.5044 0.3388 0.087 Uiso 1 1 calc R . . C22 C 0.4477(8) 0.4024(5) 0.3126(4) 0.072(3) Uani 1 1 d . . . H22A H 0.4010 0.3760 0.3427 0.086 Uiso 1 1 calc R . . H22B H 0.5310 0.4101 0.3322 0.086 Uiso 1 1 calc R . . N4 N 0.4568(5) 0.3510(3) 0.2573(3) 0.0421(14) Uani 1 1 d . . . C23 C 0.5609(6) 0.3716(4) 0.2242(4) 0.060(2) Uani 1 1 d . . . H23A H 0.6353 0.3679 0.2519 0.090 Uiso 1 1 calc R . . H23B H 0.5510 0.4228 0.2093 0.090 Uiso 1 1 calc R . . H23C H 0.5665 0.3380 0.1892 0.090 Uiso 1 1 calc R . . C24 C 0.4809(7) 0.2750(4) 0.2837(3) 0.057(2) Uani 1 1 d . . . H24A H 0.4974 0.2404 0.2507 0.085 Uiso 1 1 calc R . . H24B H 0.4096 0.2579 0.3037 0.085 Uiso 1 1 calc R . . H24C H 0.5516 0.2769 0.3141 0.085 Uiso 1 1 calc R . . C25 C 0.1054(6) 0.2715(4) 0.2687(3) 0.0377(16) Uani 1 1 d . A . C26 C 0.1248(7) 0.3068(4) 0.3257(3) 0.0501(19) Uani 1 1 d . . . H26 H 0.2055 0.3161 0.3427 0.060 Uiso 1 1 calc R . . C27 C 0.0273(9) 0.3281(4) 0.3576(4) 0.070(3) Uani 1 1 d . . . H27 H 0.0424 0.3535 0.3956 0.084 Uiso 1 1 calc R . . C28 C -0.0913(8) 0.3136(5) 0.3357(4) 0.069(3) Uani 1 1 d . . . H28 H -0.1571 0.3304 0.3576 0.083 Uiso 1 1 calc R . . C29 C -0.1124(7) 0.2754(4) 0.2831(4) 0.057(2) Uani 1 1 d . A . H29 H -0.1940 0.2636 0.2691 0.069 Uiso 1 1 calc R . . C30 C -0.0175(6) 0.2519(4) 0.2477(3) 0.0443(18) Uani 1 1 d . . . C31 C -0.0521(6) 0.2067(4) 0.1965(3) 0.0464(18) Uani 1 1 d . A . H31 H -0.1348 0.1914 0.1922 0.056 Uiso 1 1 calc R . . N6 N 0.2405(5) 0.1008(3) 0.1629(2) 0.0495(16) Uani 1 1 d D . . C1S C 0.3546(11) 0.5753(7) 0.4777(5) 0.112(4) Uani 1 1 d . . . H1S1 H 0.4413 0.5728 0.4935 0.134 Uiso 1 1 calc R . . H1S2 H 0.3493 0.6050 0.4394 0.134 Uiso 1 1 calc R . . Cl1A Cl 0.2727(5) 0.6197(2) 0.53154(17) 0.1650(17) Uani 1 1 d . . . Cl1B Cl 0.3019(4) 0.4859(2) 0.46116(15) 0.1481(15) 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 C32A 0.063(4) 0.055(3) 0.068(4) -0.007(3) 0.005(3) -0.019(3) C33A 0.063(4) 0.055(3) 0.068(4) -0.007(3) 0.005(3) -0.019(3) C34A 0.063(4) 0.055(3) 0.069(4) -0.007(3) 0.005(3) -0.019(3) C35A 0.046(3) 0.046(3) 0.045(3) 0.0000(15) 0.0027(15) 0.0011(15) C36A 0.069(4) 0.068(4) 0.068(4) 0.0000(15) 0.0069(15) -0.0003(15) C32 0.063(4) 0.055(3) 0.068(4) -0.007(3) 0.005(3) -0.019(3) C33 0.063(4) 0.055(3) 0.068(4) -0.007(3) 0.005(3) -0.019(3) C34 0.063(4) 0.055(3) 0.068(4) -0.007(3) 0.005(3) -0.019(3) C35 0.046(3) 0.046(3) 0.045(3) 0.0000(15) 0.0027(15) 0.0012(15) C36 0.069(4) 0.068(4) 0.068(4) 0.0001(15) 0.0068(15) -0.0004(15) Ni1 0.0360(5) 0.0312(5) 0.0291(5) -0.0004(4) 0.0038(4) -0.0001(4) Ni2 0.0307(4) 0.0319(5) 0.0307(5) -0.0024(4) 0.0015(3) 0.0006(4) Ni3 0.0336(4) 0.0322(5) 0.0371(5) -0.0004(4) 0.0069(4) -0.0036(4) Cl1 0.0584(11) 0.0403(10) 0.0393(10) -0.0049(8) 0.0026(8) -0.0078(9) Cl2 0.0457(10) 0.0645(13) 0.0664(14) -0.0087(10) 0.0004(10) 0.0059(10) O1 0.045(3) 0.028(2) 0.030(2) -0.0001(19) 0.005(2) 0.001(2) O2 0.028(2) 0.039(3) 0.032(3) -0.0022(19) 0.0014(19) 0.002(2) O3 0.031(2) 0.040(3) 0.043(3) 0.000(2) 0.014(2) -0.005(2) O4 0.032(2) 0.030(2) 0.039(3) -0.0033(19) 0.007(2) 0.003(2) N5 0.040(3) 0.047(4) 0.046(4) -0.003(3) 0.003(3) -0.007(3) N3 0.038(3) 0.037(3) 0.040(3) -0.001(3) 0.005(3) 0.000(3) N1 0.050(3) 0.040(3) 0.024(3) -0.001(2) -0.001(3) 0.001(3) C1 0.049(4) 0.031(4) 0.032(4) 0.001(3) 0.012(3) -0.007(3) C2 0.080(6) 0.040(4) 0.049(5) 0.001(4) -0.006(4) -0.013(4) C3 0.106(8) 0.042(5) 0.072(6) -0.008(4) 0.000(6) -0.017(5) C4 0.113(8) 0.029(4) 0.079(7) -0.003(4) 0.022(6) 0.013(5) C5 0.086(6) 0.039(5) 0.063(6) 0.007(4) 0.015(5) 0.017(4) C6 0.055(4) 0.035(4) 0.044(4) 0.005(3) 0.013(4) 0.001(4) C7 0.048(4) 0.046(5) 0.043(5) 0.012(3) 0.004(3) 0.004(4) C8 0.069(5) 0.056(5) 0.033(4) 0.001(3) -0.008(4) 0.000(4) C9 0.076(5) 0.067(5) 0.029(4) -0.003(4) 0.005(4) -0.003(5) C10 0.066(5) 0.048(5) 0.043(5) -0.008(4) 0.022(4) -0.003(4) N2 0.046(3) 0.044(3) 0.036(3) 0.006(3) 0.009(3) 0.002(3) C11 0.058(5) 0.067(5) 0.045(5) -0.003(4) 0.018(4) -0.013(4) C12 0.062(5) 0.070(6) 0.064(6) 0.005(4) 0.024(4) 0.027(5) C13 0.031(3) 0.046(4) 0.027(4) 0.004(3) 0.001(3) 0.000(3) C14 0.041(4) 0.057(5) 0.042(4) 0.003(3) -0.001(3) 0.009(4) C15 0.035(4) 0.077(6) 0.060(5) 0.012(5) -0.013(4) -0.005(4) C16 0.039(4) 0.068(6) 0.071(6) 0.016(5) 0.006(4) 0.014(4) C17 0.042(4) 0.060(5) 0.064(6) -0.003(4) 0.018(4) 0.017(4) C18 0.032(4) 0.042(4) 0.050(5) 0.001(3) 0.011(3) 0.003(3) C19 0.052(4) 0.048(4) 0.043(5) -0.003(3) 0.017(4) 0.010(4) C20 0.055(5) 0.043(4) 0.048(5) -0.015(3) 0.002(4) -0.001(4) C21 0.065(5) 0.079(7) 0.068(6) -0.031(5) -0.018(5) 0.001(5) C22 0.080(6) 0.069(6) 0.060(6) -0.024(4) -0.030(5) 0.018(5) N4 0.037(3) 0.048(4) 0.041(4) -0.004(3) -0.002(3) 0.004(3) C23 0.046(4) 0.061(5) 0.070(6) 0.007(4) -0.010(4) 0.002(4) C24 0.070(5) 0.060(5) 0.039(5) 0.009(4) -0.002(4) 0.019(4) C25 0.041(4) 0.038(4) 0.035(4) 0.011(3) 0.008(3) -0.003(3) C26 0.055(4) 0.051(5) 0.045(5) 0.001(4) 0.011(4) 0.002(4) C27 0.107(8) 0.045(5) 0.065(6) -0.004(4) 0.048(6) -0.007(5) C28 0.069(6) 0.062(6) 0.084(7) -0.002(5) 0.046(5) 0.002(5) C29 0.050(5) 0.049(5) 0.076(6) 0.002(4) 0.026(4) 0.002(4) C30 0.040(4) 0.043(4) 0.051(5) 0.014(4) 0.011(3) 0.003(3) C31 0.032(4) 0.048(5) 0.058(5) 0.009(4) 0.003(4) -0.003(4) N6 0.047(3) 0.038(3) 0.063(4) 0.005(3) 0.003(3) 0.001(3) C1S 0.118(9) 0.137(11) 0.085(8) 0.021(7) 0.035(7) -0.031(8) Cl1A 0.242(5) 0.158(4) 0.102(3) 0.003(2) 0.054(3) -0.044(3) Cl1B 0.220(4) 0.147(3) 0.077(2) 0.011(2) 0.007(2) -0.040(3) _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 C32A N5 1.515(7) . ? C32A C33A 1.524(5) . ? C33A C34A 1.524(5) . ? C34A N6 1.516(7) . ? C35A N6 1.491(7) . ? C36A N6 1.490(7) . ? C32 N5 1.515(7) . ? C32 C33 1.525(5) . ? C33 C34 1.521(5) . ? C34 N6 1.515(7) . ? C35 N6 1.491(7) . ? C36 N6 1.491(7) . ? Ni1 N1 2.009(5) . ? Ni1 O1 2.050(4) . ? Ni1 O4 2.079(5) . ? Ni1 N2 2.130(5) . ? Ni1 O2 2.174(4) . ? Ni1 Cl1 2.462(2) . ? Ni1 Ni2 2.901(2) . ? Ni2 O4 2.033(4) . ? Ni2 N3 2.034(5) . ? Ni2 O2 2.058(4) . ? Ni2 N4 2.133(5) . ? Ni2 O3 2.207(4) . ? Ni2 O1 2.252(4) . ? Ni2 Ni3 2.887(2) . ? Ni3 N5 1.992(6) . ? Ni3 O4 2.055(4) . ? Ni3 O3 2.081(5) . ? Ni3 N6 2.142(6) . ? Ni3 O2 2.187(4) . ? Ni3 Cl1 2.488(3) . ? O1 C1 1.333(7) . ? O2 C13 1.345(7) . ? O3 C25 1.345(7) . ? N5 C31 1.283(8) . ? N3 C19 1.287(8) . ? N3 C20 1.501(8) . ? N1 C7 1.271(8) . ? N1 C8 1.483(8) . ? C1 C2 1.396(9) . ? C1 C6 1.419(9) . ? C2 C3 1.400(11) . ? C3 C4 1.392(12) . ? C4 C5 1.386(11) . ? C5 C6 1.408(9) . ? C6 C7 1.454(10) . ? C8 C9 1.525(10) . ? C9 C10 1.538(10) . ? C10 N2 1.490(9) . ? N2 C12 1.487(9) . ? N2 C11 1.519(9) . ? C13 C18 1.404(9) . ? C13 C14 1.416(9) . ? C14 C15 1.388(10) . ? C15 C16 1.417(11) . ? C16 C17 1.374(10) . ? C17 C18 1.422(9) . ? C18 C19 1.468(10) . ? C20 C21 1.497(10) . ? C21 C22 1.424(11) . ? C22 N4 1.531(9) . ? N4 C23 1.454(9) . ? N4 C24 1.501(8) . ? C25 C26 1.397(9) . ? C25 C30 1.439(9) . ? C26 C27 1.384(10) . ? C27 C28 1.380(12) . ? C28 C29 1.342(11) . ? C29 C30 1.417(10) . ? C30 C31 1.409(10) . ? C1S Cl1A 1.735(12) . ? C1S Cl1B 1.738(12) . ? 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 N5 C32A C33A 105.5(15) . . ? C32A C33A C34A 114(2) . . ? N6 C34A C33A 124.8(14) . . ? N5 C32 C33 114.4(11) . . ? C34 C33 C32 113.4(12) . . ? N6 C34 C33 106.6(9) . . ? N1 Ni1 O1 92.4(2) . . ? N1 Ni1 O4 166.87(19) . . ? O1 Ni1 O4 83.12(17) . . ? N1 Ni1 N2 87.4(2) . . ? O1 Ni1 N2 99.3(2) . . ? O4 Ni1 N2 105.5(2) . . ? N1 Ni1 O2 95.9(2) . . ? O1 Ni1 O2 80.32(16) . . ? O4 Ni1 O2 71.20(17) . . ? N2 Ni1 O2 176.65(19) . . ? N1 Ni1 Cl1 98.19(17) . . ? O1 Ni1 Cl1 162.02(13) . . ? O4 Ni1 Cl1 83.30(13) . . ? N2 Ni1 Cl1 95.67(17) . . ? O2 Ni1 Cl1 84.19(12) . . ? N1 Ni1 Ni2 124.12(16) . . ? O1 Ni1 Ni2 50.64(12) . . ? O4 Ni1 Ni2 44.50(12) . . ? N2 Ni1 Ni2 132.35(16) . . ? O2 Ni1 Ni2 45.08(11) . . ? Cl1 Ni1 Ni2 111.50(5) . . ? O4 Ni2 N3 165.4(2) . . ? O4 Ni2 O2 74.52(17) . . ? N3 Ni2 O2 91.3(2) . . ? O4 Ni2 N4 95.8(2) . . ? N3 Ni2 N4 98.5(2) . . ? O2 Ni2 N4 170.13(19) . . ? O4 Ni2 O3 81.30(17) . . ? N3 Ni2 O3 99.4(2) . . ? O2 Ni2 O3 78.10(17) . . ? N4 Ni2 O3 98.8(2) . . ? O4 Ni2 O1 79.27(17) . . ? N3 Ni2 O1 94.78(19) . . ? O2 Ni2 O1 78.31(16) . . ? N4 Ni2 O1 102.13(19) . . ? O3 Ni2 O1 152.67(16) . . ? O4 Ni2 Ni3 45.38(12) . . ? N3 Ni2 Ni3 126.32(16) . . ? O2 Ni2 Ni3 49.06(12) . . ? N4 Ni2 Ni3 122.40(16) . . ? O3 Ni2 Ni3 45.86(12) . . ? O1 Ni2 Ni3 107.27(12) . . ? O4 Ni2 Ni1 45.79(13) . . ? N3 Ni2 Ni1 121.51(16) . . ? O2 Ni2 Ni1 48.42(12) . . ? N4 Ni2 Ni1 125.53(16) . . ? O3 Ni2 Ni1 108.27(12) . . ? O1 Ni2 Ni1 44.71(11) . . ? Ni3 Ni2 Ni1 62.56(3) . . ? N5 Ni3 O4 167.8(2) . . ? N5 Ni3 O3 91.4(2) . . ? O4 Ni3 O3 83.92(16) . . ? N5 Ni3 N6 88.9(2) . . ? O4 Ni3 N6 103.03(19) . . ? O3 Ni3 N6 101.42(19) . . ? N5 Ni3 O2 96.7(2) . . ? O4 Ni3 O2 71.38(16) . . ? O3 Ni3 O2 78.07(16) . . ? N6 Ni3 O2 174.40(18) . . ? N5 Ni3 Cl1 98.13(17) . . ? O4 Ni3 Cl1 83.13(13) . . ? O3 Ni3 Cl1 159.92(13) . . ? N6 Ni3 Cl1 96.40(15) . . ? O2 Ni3 Cl1 83.29(12) . . ? N5 Ni3 Ni2 124.69(17) . . ? O4 Ni3 Ni2 44.77(12) . . ? O3 Ni3 Ni2 49.55(12) . . ? N6 Ni3 Ni2 130.42(16) . . ? O2 Ni3 Ni2 45.29(11) . . ? Cl1 Ni3 Ni2 111.15(5) . . ? Ni1 Cl1 Ni3 74.75(6) . . ? C1 O1 Ni1 124.0(4) . . ? C1 O1 Ni2 118.2(4) . . ? Ni1 O1 Ni2 84.65(16) . . ? C13 O2 Ni2 127.9(4) . . ? C13 O2 Ni1 130.6(4) . . ? Ni2 O2 Ni1 86.50(16) . . ? C13 O2 Ni3 124.6(4) . . ? Ni2 O2 Ni3 85.65(15) . . ? Ni1 O2 Ni3 87.12(15) . . ? C25 O3 Ni3 123.8(4) . . ? C25 O3 Ni2 117.3(4) . . ? Ni3 O3 Ni2 84.58(16) . . ? Ni2 O4 Ni3 89.85(17) . . ? Ni2 O4 Ni1 89.70(18) . . ? Ni3 O4 Ni1 93.26(18) . . ? C31 N5 C32A 117(2) . . ? C31 N5 C32 119.7(14) . . ? C32A N5 C32 7.0(13) . . ? C31 N5 Ni3 125.2(5) . . ? C32A N5 Ni3 118(2) . . ? C32 N5 Ni3 114.8(12) . . ? C19 N3 C20 112.3(6) . . ? C19 N3 Ni2 123.9(5) . . ? C20 N3 Ni2 123.8(4) . . ? C7 N1 C8 118.6(6) . . ? C7 N1 Ni1 124.4(5) . . ? C8 N1 Ni1 116.8(4) . . ? O1 C1 C2 117.8(6) . . ? O1 C1 C6 124.2(6) . . ? C2 C1 C6 118.0(6) . . ? C1 C2 C3 122.1(8) . . ? C4 C3 C2 119.6(8) . . ? C5 C4 C3 118.7(8) . . ? C4 C5 C6 122.4(8) . . ? C5 C6 C1 118.5(7) . . ? C5 C6 C7 116.0(7) . . ? C1 C6 C7 125.2(6) . . ? N1 C7 C6 126.7(6) . . ? N1 C8 C9 108.3(6) . . ? C8 C9 C10 114.8(6) . . ? N2 C10 C9 116.6(6) . . ? C12 N2 C10 108.2(6) . . ? C12 N2 C11 107.9(6) . . ? C10 N2 C11 110.5(5) . . ? C12 N2 Ni1 108.7(4) . . ? C10 N2 Ni1 111.8(4) . . ? C11 N2 Ni1 109.7(4) . . ? O2 C13 C18 122.0(6) . . ? O2 C13 C14 118.7(6) . . ? C18 C13 C14 119.3(6) . . ? C15 C14 C13 120.8(7) . . ? C14 C15 C16 120.3(7) . . ? C17 C16 C15 118.6(7) . . ? C16 C17 C18 122.3(7) . . ? C13 C18 C17 118.5(6) . . ? C13 C18 C19 125.4(6) . . ? C17 C18 C19 116.0(6) . . ? N3 C19 C18 128.8(6) . . ? C21 C20 N3 115.3(6) . . ? C22 C21 C20 120.3(8) . . ? C21 C22 N4 117.9(7) . . ? C23 N4 C24 107.5(6) . . ? C23 N4 C22 110.1(6) . . ? C24 N4 C22 105.5(6) . . ? C23 N4 Ni2 110.4(4) . . ? C24 N4 Ni2 110.2(4) . . ? C22 N4 Ni2 112.9(4) . . ? O3 C25 C26 119.1(6) . . ? O3 C25 C30 123.1(6) . . ? C26 C25 C30 117.8(6) . . ? C27 C26 C25 120.5(8) . . ? C28 C27 C26 121.8(8) . . ? C29 C28 C27 119.0(8) . . ? C28 C29 C30 122.5(8) . . ? C31 C30 C29 116.2(7) . . ? C31 C30 C25 125.5(6) . . ? C29 C30 C25 118.2(7) . . ? N5 C31 C30 127.7(6) . . ? C36A N6 C35A 108.5(7) . . ? C36A N6 C35 123.7(10) . . ? C35A N6 C35 21.6(8) . . ? C36A N6 C36 33.2(8) . . ? C35A N6 C36 87.0(10) . . ? C35 N6 C36 107.7(7) . . ? C36A N6 C34 70.4(10) . . ? C35A N6 C34 124.8(10) . . ? C35 N6 C34 112.2(8) . . ? C36 N6 C34 103.4(8) . . ? C36A N6 C34A 107.8(12) . . ? C35A N6 C34A 102.6(10) . . ? C35 N6 C34A 82.8(8) . . ? C36 N6 C34A 138.9(11) . . ? C34 N6 C34A 38.9(8) . . ? C36A N6 Ni3 117.0(8) . . ? C35A N6 Ni3 113.4(8) . . ? C35 N6 Ni3 111.7(6) . . ? C36 N6 Ni3 105.9(6) . . ? C34 N6 Ni3 115.1(6) . . ? C34A N6 Ni3 106.4(9) . . ? Cl1A C1S Cl1B 112.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.614 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.103 data_b348 _database_code_depnum_ccdc_archive 'CCDC 918626' #TrackingRef 'web_deposit_cif_file_2_XiaoluSong_1360938597.b348.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Cl3 N3 Ni3 O7' _chemical_formula_weight 931.28 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' Cl Cl 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.722(2) _cell_length_b 10.9768(13) _cell_length_c 20.175(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.568(3) _cell_angle_gamma 90.00 _cell_volume 4012.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 889 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 24.25 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6561 _exptl_absorpt_correction_T_max 0.8529 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28117 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9204 _reflns_number_gt 7002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0560P)^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 9204 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.022 _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 Ni1 Ni 0.78429(2) 0.73841(4) 0.571759(18) 0.01813(10) Uani 1 1 d . . . Ni2 Ni 0.88264(2) 0.93238(4) 0.643487(18) 0.01854(10) Uani 1 1 d . . . Ni3 Ni 0.75638(2) 0.98769(4) 0.524654(19) 0.01985(11) Uani 1 1 d . . . Cl1 Cl 0.88411(4) 0.71203(7) 0.67205(4) 0.02183(17) Uani 1 1 d . . . Cl2 Cl 0.83936(4) 1.13304(7) 0.60111(4) 0.02314(17) Uani 1 1 d . . . Cl3 Cl 0.76909(5) 1.07335(8) 0.42341(4) 0.02826(19) Uani 1 1 d . . . O1 O 0.85338(11) 0.8749(2) 0.54626(10) 0.0191(4) Uani 1 1 d . . . O2 O 0.90302(11) 0.9892(2) 0.74567(10) 0.0243(5) Uani 1 1 d . . . O3 O 0.76592(11) 0.9036(2) 0.61907(10) 0.0191(4) Uani 1 1 d . . . O4 O 0.52878(13) 1.3213(2) 0.39456(12) 0.0347(6) Uani 1 1 d . . . O5 O 0.71680(11) 0.8119(2) 0.48939(10) 0.0212(5) Uani 1 1 d . . . O6 O 0.67459(15) 0.3310(3) 0.70310(13) 0.0510(8) Uani 1 1 d . . . O7 O 0.81997(11) 0.5959(2) 0.52099(10) 0.0231(5) Uani 1 1 d . . . N1 N 0.98955(14) 0.9357(2) 0.64458(12) 0.0207(6) Uani 1 1 d . . . N2 N 0.65402(14) 1.0497(3) 0.52483(13) 0.0244(6) Uani 1 1 d . . . N3 N 0.70174(14) 0.6415(2) 0.59413(12) 0.0217(6) Uani 1 1 d . . . C1 C 0.89779(16) 0.8509(3) 0.50461(14) 0.0188(6) Uani 1 1 d . . . C2 C 0.86579(17) 0.8142(3) 0.43720(15) 0.0211(7) Uani 1 1 d . . . H2 H 0.8136 0.8097 0.4212 0.025 Uiso 1 1 calc R . . C3 C 0.90997(18) 0.7843(3) 0.39368(15) 0.0227(7) Uani 1 1 d . . . H3 H 0.8877 0.7596 0.3480 0.027 Uiso 1 1 calc R . . C4 C 0.98617(18) 0.7901(3) 0.41607(16) 0.0240(7) Uani 1 1 d . . . H4 H 1.0160 0.7668 0.3865 0.029 Uiso 1 1 calc R . . C5 C 1.01847(17) 0.8301(3) 0.48169(16) 0.0221(7) Uani 1 1 d . . . H5 H 1.0706 0.8372 0.4964 0.026 Uiso 1 1 calc R . . C6 C 0.97505(16) 0.8604(3) 0.52712(15) 0.0180(6) Uani 1 1 d . . . C7 C 1.01598(17) 0.9024(3) 0.59454(15) 0.0213(7) Uani 1 1 d . . . H7 H 1.0681 0.9054 0.6023 0.026 Uiso 1 1 calc R . . C8 C 1.04318(17) 0.9735(3) 0.70789(15) 0.0266(7) Uani 1 1 d . . . H8A H 1.0399 1.0628 0.7137 0.032 Uiso 1 1 calc R . . H8B H 1.0937 0.9542 0.7043 0.032 Uiso 1 1 calc R . . C9 C 1.02871(18) 0.9095(3) 0.76981(15) 0.0268(7) Uani 1 1 d . . . H9A H 1.0115 0.8254 0.7569 0.032 Uiso 1 1 calc R . . H9B H 1.0754 0.9042 0.8061 0.032 Uiso 1 1 calc R . . C10 C 0.97141(17) 0.9753(3) 0.79776(15) 0.0254(7) Uani 1 1 d . . . H10A H 0.9621 0.9288 0.8368 0.031 Uiso 1 1 calc R . . H10B H 0.9904 1.0566 0.8148 0.031 Uiso 1 1 calc R . . C11 C 0.85560(19) 1.0730(3) 0.76728(17) 0.0309(8) Uani 1 1 d . . . H11A H 0.8436 1.0422 0.8088 0.046 Uiso 1 1 calc R . . H11B H 0.8101 1.0827 0.7310 0.046 Uiso 1 1 calc R . . H11C H 0.8804 1.1521 0.7770 0.046 Uiso 1 1 calc R . . C12 C 0.71674(17) 0.9034(3) 0.65790(15) 0.0224(7) Uani 1 1 d . . . C13 C 0.73508(18) 0.8508(3) 0.72283(16) 0.0254(7) Uani 1 1 d . . . H13 H 0.7835 0.8194 0.7404 0.030 Uiso 1 1 calc R . . C14 C 0.6851(2) 0.8429(3) 0.76211(17) 0.0325(8) Uani 1 1 d . . . H14 H 0.6994 0.8062 0.8061 0.039 Uiso 1 1 calc R . . C15 C 0.6140(2) 0.8879(4) 0.73832(19) 0.0367(9) Uani 1 1 d . . . H15 H 0.5789 0.8805 0.7649 0.044 Uiso 1 1 calc R . . C16 C 0.59559(19) 0.9435(3) 0.67511(19) 0.0342(8) Uani 1 1 d . . . H16 H 0.5474 0.9762 0.6589 0.041 Uiso 1 1 calc R . . C17 C 0.64531(18) 0.9537(3) 0.63367(16) 0.0255(7) Uani 1 1 d . . . C18 C 0.61907(17) 1.0206(3) 0.56965(17) 0.0260(7) Uani 1 1 d . . . H18 H 0.5690 1.0462 0.5598 0.031 Uiso 1 1 calc R . . C19 C 0.61273(18) 1.1265(3) 0.46773(17) 0.0280(7) Uani 1 1 d . . . H19A H 0.5591 1.1178 0.4633 0.034 Uiso 1 1 calc R . . H19B H 0.6231 1.0990 0.4243 0.034 Uiso 1 1 calc R . . C20 C 0.63479(18) 1.2586(3) 0.48031(16) 0.0258(7) Uani 1 1 d . . . H20A H 0.6160 1.2897 0.5188 0.031 Uiso 1 1 calc R . . H20B H 0.6893 1.2643 0.4940 0.031 Uiso 1 1 calc R . . C21 C 0.60570(18) 1.3381(3) 0.41822(17) 0.0307(8) Uani 1 1 d . . . H21A H 0.6166 1.4247 0.4304 0.037 Uiso 1 1 calc R . . H21B H 0.6301 1.3162 0.3817 0.037 Uiso 1 1 calc R . . C22 C 0.4991(2) 1.3858(4) 0.33308(18) 0.0414(10) Uani 1 1 d . . . H22A H 0.5051 1.4735 0.3417 0.062 Uiso 1 1 calc R . . H22B H 0.4465 1.3666 0.3164 0.062 Uiso 1 1 calc R . . H22C H 0.5250 1.3619 0.2986 0.062 Uiso 1 1 calc R . . C23 C 0.64765(17) 0.7819(3) 0.46039(15) 0.0225(7) Uani 1 1 d . . . C24 C 0.61297(18) 0.8314(3) 0.39575(15) 0.0245(7) Uani 1 1 d . . . H24 H 0.6396 0.8856 0.3741 0.029 Uiso 1 1 calc R . . C25 C 0.54117(18) 0.8021(3) 0.36373(17) 0.0298(8) Uani 1 1 d . . . H25 H 0.5190 0.8361 0.3201 0.036 Uiso 1 1 calc R . . C26 C 0.50004(18) 0.7230(3) 0.39426(17) 0.0312(8) Uani 1 1 d . . . H26 H 0.4505 0.7031 0.3719 0.037 Uiso 1 1 calc R . . C27 C 0.53300(18) 0.6756(3) 0.45682(17) 0.0307(8) Uani 1 1 d . . . H27 H 0.5052 0.6231 0.4782 0.037 Uiso 1 1 calc R . . C28 C 0.60654(17) 0.7012(3) 0.49101(16) 0.0237(7) Uani 1 1 d . . . C29 C 0.63515(17) 0.6419(3) 0.55662(16) 0.0253(7) Uani 1 1 d . . . H29 H 0.6002 0.5977 0.5741 0.030 Uiso 1 1 calc R . . C30 C 0.71570(18) 0.5641(3) 0.65615(16) 0.0271(7) Uani 1 1 d . . . H30A H 0.6690 0.5521 0.6699 0.033 Uiso 1 1 calc R . . H30B H 0.7511 0.6055 0.6942 0.033 Uiso 1 1 calc R . . C31 C 0.7463(2) 0.4425(3) 0.64326(18) 0.0327(8) Uani 1 1 d . . . H31A H 0.7970 0.4533 0.6378 0.039 Uiso 1 1 calc R . . H31B H 0.7156 0.4078 0.6001 0.039 Uiso 1 1 calc R . . C32 C 0.7478(2) 0.3542(4) 0.70196(19) 0.0368(9) Uani 1 1 d . . . H32A H 0.7727 0.2775 0.6948 0.044 Uiso 1 1 calc R . . H32B H 0.7752 0.3905 0.7460 0.044 Uiso 1 1 calc R . . C33 C 0.6693(3) 0.2544(5) 0.7580(2) 0.0654(16) Uani 1 1 d . . . H33A H 0.6894 0.1740 0.7519 0.098 Uiso 1 1 calc R . . H33B H 0.6174 0.2463 0.7588 0.098 Uiso 1 1 calc R . . H33C H 0.6973 0.2900 0.8013 0.098 Uiso 1 1 calc R . . C34 C 0.77031(19) 0.5298(3) 0.46560(17) 0.0304(8) Uani 1 1 d . . . H34A H 0.7559 0.5811 0.4240 0.036 Uiso 1 1 calc R . . H34B H 0.7252 0.5046 0.4791 0.036 Uiso 1 1 calc R . . C35 C 0.8139(2) 0.4188(3) 0.45270(19) 0.0339(8) Uani 1 1 d . . . H35A H 0.8083 0.3497 0.4825 0.041 Uiso 1 1 calc R . . H35B H 0.7986 0.3928 0.4042 0.041 Uiso 1 1 calc R . . C36 C 0.89232(18) 0.4679(3) 0.47123(17) 0.0293(8) Uani 1 1 d . . . H36A H 0.9289 0.4010 0.4822 0.035 Uiso 1 1 calc R . . H36B H 0.9022 0.5177 0.4336 0.035 Uiso 1 1 calc R . . C37 C 0.89373(17) 0.5445(3) 0.53336(16) 0.0247(7) Uani 1 1 d . . . H37A H 0.9051 0.4940 0.5753 0.030 Uiso 1 1 calc R . . H37B H 0.9312 0.6099 0.5384 0.030 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 Ni1 0.0162(2) 0.0231(2) 0.01491(19) 0.00105(16) 0.00358(15) 0.00013(15) Ni2 0.0167(2) 0.0246(2) 0.01413(18) -0.00039(16) 0.00357(15) -0.00038(15) Ni3 0.0177(2) 0.0247(2) 0.01694(19) 0.00219(16) 0.00391(16) 0.00143(16) Cl1 0.0213(4) 0.0251(4) 0.0176(3) 0.0027(3) 0.0019(3) 0.0013(3) Cl2 0.0222(4) 0.0259(4) 0.0221(4) 0.0010(3) 0.0072(3) -0.0002(3) Cl3 0.0321(4) 0.0321(5) 0.0213(4) 0.0079(3) 0.0081(3) 0.0052(3) O1 0.0178(11) 0.0239(12) 0.0158(10) 0.0010(9) 0.0047(8) -0.0014(9) O2 0.0216(11) 0.0330(14) 0.0162(10) -0.0021(9) 0.0010(9) 0.0021(9) O3 0.0177(11) 0.0254(12) 0.0152(10) -0.0006(9) 0.0059(8) 0.0006(9) O4 0.0253(13) 0.0430(16) 0.0328(13) 0.0083(12) 0.0018(11) 0.0017(11) O5 0.0190(11) 0.0280(13) 0.0159(10) 0.0016(9) 0.0031(9) -0.0001(9) O6 0.0462(17) 0.066(2) 0.0338(14) 0.0192(14) -0.0033(13) -0.0307(15) O7 0.0211(11) 0.0264(13) 0.0205(10) -0.0048(9) 0.0027(9) 0.0011(9) N1 0.0190(13) 0.0258(15) 0.0169(12) -0.0010(11) 0.0038(11) -0.0022(11) N2 0.0192(13) 0.0241(16) 0.0284(14) -0.0018(12) 0.0037(12) -0.0006(11) N3 0.0232(14) 0.0232(15) 0.0206(13) 0.0015(11) 0.0089(11) 0.0010(11) C1 0.0228(16) 0.0181(16) 0.0174(14) 0.0021(12) 0.0086(13) 0.0027(12) C2 0.0199(16) 0.0231(17) 0.0202(15) -0.0003(13) 0.0051(13) -0.0014(12) C3 0.0308(18) 0.0229(17) 0.0155(14) -0.0009(13) 0.0081(13) -0.0024(13) C4 0.0270(17) 0.0251(18) 0.0250(16) -0.0001(14) 0.0159(14) -0.0028(13) C5 0.0203(16) 0.0213(17) 0.0270(16) -0.0003(13) 0.0105(13) -0.0010(12) C6 0.0181(15) 0.0171(16) 0.0191(14) 0.0013(12) 0.0054(12) 0.0019(12) C7 0.0153(15) 0.0244(18) 0.0240(15) 0.0042(13) 0.0046(13) -0.0005(12) C8 0.0184(16) 0.041(2) 0.0184(15) -0.0031(14) 0.0014(13) -0.0044(14) C9 0.0227(17) 0.034(2) 0.0188(15) 0.0025(14) -0.0033(13) -0.0020(14) C10 0.0235(17) 0.035(2) 0.0162(15) -0.0009(14) 0.0013(13) -0.0035(14) C11 0.0329(19) 0.037(2) 0.0223(16) -0.0030(15) 0.0063(15) 0.0060(16) C12 0.0242(17) 0.0242(18) 0.0211(15) -0.0031(13) 0.0095(13) -0.0037(13) C13 0.0247(17) 0.0285(19) 0.0238(16) -0.0018(14) 0.0077(14) -0.0002(14) C14 0.044(2) 0.032(2) 0.0272(18) -0.0013(15) 0.0210(17) -0.0043(16) C15 0.042(2) 0.036(2) 0.043(2) 0.0009(18) 0.0313(19) -0.0029(17) C16 0.0276(19) 0.034(2) 0.047(2) -0.0015(17) 0.0208(17) 0.0017(15) C17 0.0240(17) 0.0255(19) 0.0294(17) -0.0031(14) 0.0111(14) -0.0003(13) C18 0.0173(16) 0.0281(19) 0.0321(18) -0.0008(15) 0.0053(14) 0.0030(13) C19 0.0199(17) 0.033(2) 0.0290(17) 0.0011(15) 0.0027(14) 0.0061(14) C20 0.0203(16) 0.0290(19) 0.0272(17) 0.0006(14) 0.0041(14) 0.0018(13) C21 0.0254(18) 0.034(2) 0.0331(18) 0.0044(16) 0.0074(15) 0.0004(15) C22 0.039(2) 0.053(3) 0.0295(19) 0.0041(18) 0.0034(17) 0.0059(19) C23 0.0203(16) 0.0258(18) 0.0203(15) -0.0054(13) 0.0030(13) 0.0051(13) C24 0.0259(17) 0.0302(19) 0.0165(15) -0.0036(13) 0.0038(13) 0.0034(14) C25 0.0238(17) 0.039(2) 0.0228(16) -0.0059(15) -0.0020(14) 0.0091(15) C26 0.0189(17) 0.038(2) 0.0326(18) -0.0090(16) -0.0017(15) 0.0024(14) C27 0.0222(17) 0.036(2) 0.0339(18) -0.0004(16) 0.0074(15) -0.0005(14) C28 0.0196(16) 0.0285(19) 0.0225(15) -0.0026(14) 0.0042(13) 0.0013(13) C29 0.0213(17) 0.0286(19) 0.0282(17) 0.0002(14) 0.0106(14) 0.0006(13) C30 0.0254(17) 0.032(2) 0.0250(16) 0.0057(15) 0.0085(14) -0.0017(14) C31 0.036(2) 0.033(2) 0.0305(18) 0.0049(16) 0.0101(16) 0.0011(16) C32 0.042(2) 0.032(2) 0.038(2) 0.0081(17) 0.0118(18) 0.0054(16) C33 0.069(3) 0.080(4) 0.038(2) 0.021(2) -0.005(2) -0.042(3) C34 0.0284(18) 0.032(2) 0.0286(17) -0.0095(15) 0.0024(15) -0.0058(15) C35 0.040(2) 0.031(2) 0.0370(19) -0.0105(16) 0.0209(17) -0.0112(16) C36 0.0306(19) 0.028(2) 0.0322(18) 0.0009(15) 0.0138(15) 0.0036(14) C37 0.0167(15) 0.0302(19) 0.0276(16) 0.0034(14) 0.0066(13) 0.0032(13) _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 Ni1 O5 1.988(2) . ? Ni1 N3 2.019(3) . ? Ni1 O7 2.070(2) . ? Ni1 O3 2.117(2) . ? Ni1 O1 2.125(2) . ? Ni1 Cl1 2.4017(8) . ? Ni1 Ni3 2.9007(6) . ? Ni1 Ni2 2.9458(6) . ? Ni2 N1 1.996(2) . ? Ni2 O1 2.001(2) . ? Ni2 O2 2.095(2) . ? Ni2 O3 2.139(2) . ? Ni2 Cl2 2.4270(9) . ? Ni2 Cl1 2.4850(9) . ? Ni2 Ni3 2.9753(6) . ? Ni3 N2 2.034(3) . ? Ni3 O3 2.084(2) . ? Ni3 O5 2.125(2) . ? Ni3 O1 2.150(2) . ? Ni3 Cl3 2.3145(9) . ? Ni3 Cl2 2.4764(9) . ? O1 C1 1.348(3) . ? O2 C11 1.421(4) . ? O2 C10 1.446(4) . ? O3 C12 1.351(3) . ? O4 C21 1.411(4) . ? O4 C22 1.415(4) . ? O5 C23 1.321(4) . ? O6 C32 1.401(4) . ? O6 C33 1.413(4) . ? O7 C37 1.454(4) . ? O7 C34 1.455(4) . ? N1 C7 1.284(4) . ? N1 C8 1.472(4) . ? N2 C18 1.283(4) . ? N2 C19 1.479(4) . ? N3 C29 1.285(4) . ? N3 C30 1.480(4) . ? C1 C2 1.400(4) . ? C1 C6 1.407(4) . ? C2 C3 1.388(4) . ? C3 C4 1.385(4) . ? C4 C5 1.381(4) . ? C5 C6 1.410(4) . ? C6 C7 1.458(4) . ? C8 C9 1.516(4) . ? C9 C10 1.515(5) . ? C12 C13 1.394(4) . ? C12 C17 1.415(4) . ? C13 C14 1.373(4) . ? C14 C15 1.388(5) . ? C15 C16 1.377(5) . ? C16 C17 1.403(4) . ? C17 C18 1.459(5) . ? C19 C20 1.512(5) . ? C20 C21 1.511(5) . ? C23 C24 1.411(4) . ? C23 C28 1.413(5) . ? C24 C25 1.375(5) . ? C25 C26 1.401(5) . ? C26 C27 1.361(5) . ? C27 C28 1.405(5) . ? C28 C29 1.451(4) . ? C30 C31 1.501(5) . ? C31 C32 1.525(5) . ? C34 C35 1.525(5) . ? C35 C36 1.520(5) . ? C36 C37 1.504(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 O5 Ni1 N3 92.26(10) . . ? O5 Ni1 O7 96.28(9) . . ? N3 Ni1 O7 94.17(10) . . ? O5 Ni1 O3 83.58(8) . . ? N3 Ni1 O3 97.49(9) . . ? O7 Ni1 O3 168.33(8) . . ? O5 Ni1 O1 79.00(8) . . ? N3 Ni1 O1 166.52(10) . . ? O7 Ni1 O1 96.96(8) . . ? O3 Ni1 O1 71.53(8) . . ? O5 Ni1 Cl1 161.69(7) . . ? N3 Ni1 Cl1 103.02(8) . . ? O7 Ni1 Cl1 92.65(6) . . ? O3 Ni1 Cl1 84.47(6) . . ? O1 Ni1 Cl1 84.08(6) . . ? O5 Ni1 Ni3 47.09(6) . . ? N3 Ni1 Ni3 119.05(8) . . ? O7 Ni1 Ni3 127.20(6) . . ? O3 Ni1 Ni3 45.85(5) . . ? O1 Ni1 Ni3 47.64(6) . . ? Cl1 Ni1 Ni3 115.31(2) . . ? O5 Ni1 Ni2 107.73(7) . . ? N3 Ni1 Ni2 133.65(7) . . ? O7 Ni1 Ni2 123.34(6) . . ? O3 Ni1 Ni2 46.51(5) . . ? O1 Ni1 Ni2 42.79(5) . . ? Cl1 Ni1 Ni2 54.23(2) . . ? Ni3 Ni1 Ni2 61.177(15) . . ? N1 Ni2 O1 92.48(9) . . ? N1 Ni2 O2 92.85(9) . . ? O1 Ni2 O2 174.59(8) . . ? N1 Ni2 O3 165.58(9) . . ? O1 Ni2 O3 73.49(8) . . ? O2 Ni2 O3 101.14(8) . . ? N1 Ni2 Cl2 103.42(8) . . ? O1 Ni2 Cl2 87.49(7) . . ? O2 Ni2 Cl2 92.21(7) . . ? O3 Ni2 Cl2 79.73(6) . . ? N1 Ni2 Cl1 93.60(8) . . ? O1 Ni2 Cl1 84.53(7) . . ? O2 Ni2 Cl1 94.18(7) . . ? O3 Ni2 Cl1 82.00(6) . . ? Cl2 Ni2 Cl1 161.50(3) . . ? N1 Ni2 Ni1 121.32(8) . . ? O1 Ni2 Ni1 46.16(6) . . ? O2 Ni2 Ni1 129.44(6) . . ? O3 Ni2 Ni1 45.90(6) . . ? Cl2 Ni2 Ni1 111.77(2) . . ? Cl1 Ni2 Ni1 51.65(2) . . ? N1 Ni2 Ni3 126.60(7) . . ? O1 Ni2 Ni3 46.25(6) . . ? O2 Ni2 Ni3 130.04(6) . . ? O3 Ni2 Ni3 44.45(5) . . ? Cl2 Ni2 Ni3 53.40(2) . . ? Cl1 Ni2 Ni3 110.23(2) . . ? Ni1 Ni2 Ni3 58.664(14) . . ? N2 Ni3 O3 90.61(9) . . ? N2 Ni3 O5 93.15(10) . . ? O3 Ni3 O5 81.16(8) . . ? N2 Ni3 O1 160.07(10) . . ? O3 Ni3 O1 71.68(8) . . ? O5 Ni3 O1 75.55(8) . . ? N2 Ni3 Cl3 99.89(8) . . ? O3 Ni3 Cl3 169.29(6) . . ? O5 Ni3 Cl3 100.26(6) . . ? O1 Ni3 Cl3 98.27(6) . . ? N2 Ni3 Cl2 103.13(8) . . ? O3 Ni3 Cl2 79.62(6) . . ? O5 Ni3 Cl2 154.83(6) . . ? O1 Ni3 Cl2 83.06(6) . . ? Cl3 Ni3 Cl2 95.76(3) . . ? N2 Ni3 Ni1 114.01(8) . . ? O3 Ni3 Ni1 46.81(6) . . ? O5 Ni3 Ni1 43.27(6) . . ? O1 Ni3 Ni1 46.91(6) . . ? Cl3 Ni3 Ni1 128.49(3) . . ? Cl2 Ni3 Ni1 111.75(2) . . ? N2 Ni3 Ni2 128.65(8) . . ? O3 Ni3 Ni2 45.97(6) . . ? O5 Ni3 Ni2 102.94(6) . . ? O1 Ni3 Ni2 42.25(5) . . ? Cl3 Ni3 Ni2 123.84(3) . . ? Cl2 Ni3 Ni2 51.89(2) . . ? Ni1 Ni3 Ni2 60.159(13) . . ? Ni1 Cl1 Ni2 74.12(2) . . ? Ni2 Cl2 Ni3 74.71(3) . . ? C1 O1 Ni2 127.78(18) . . ? C1 O1 Ni1 121.43(18) . . ? Ni2 O1 Ni1 91.05(8) . . ? C1 O1 Ni3 127.43(17) . . ? Ni2 O1 Ni3 91.50(8) . . ? Ni1 O1 Ni3 85.45(7) . . ? C11 O2 C10 110.7(2) . . ? C11 O2 Ni2 121.43(18) . . ? C10 O2 Ni2 126.35(18) . . ? C12 O3 Ni3 128.07(19) . . ? C12 O3 Ni1 118.16(18) . . ? Ni3 O3 Ni1 87.34(7) . . ? C12 O3 Ni2 132.27(18) . . ? Ni3 O3 Ni2 89.59(8) . . ? Ni1 O3 Ni2 87.59(8) . . ? C21 O4 C22 111.9(3) . . ? C23 O5 Ni1 128.0(2) . . ? C23 O5 Ni3 126.5(2) . . ? Ni1 O5 Ni3 89.65(8) . . ? C32 O6 C33 112.5(3) . . ? C37 O7 C34 109.5(2) . . ? C37 O7 Ni1 128.22(18) . . ? C34 O7 Ni1 122.22(19) . . ? C7 N1 C8 116.7(3) . . ? C7 N1 Ni2 124.7(2) . . ? C8 N1 Ni2 118.56(19) . . ? C18 N2 C19 115.6(3) . . ? C18 N2 Ni3 124.5(2) . . ? C19 N2 Ni3 119.8(2) . . ? C29 N3 C30 116.0(3) . . ? C29 N3 Ni1 123.4(2) . . ? C30 N3 Ni1 120.6(2) . . ? O1 C1 C2 118.8(3) . . ? O1 C1 C6 122.0(3) . . ? C2 C1 C6 119.3(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 119.6(3) . . ? C4 C5 C6 120.9(3) . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C7 125.5(3) . . ? C5 C6 C7 115.3(3) . . ? N1 C7 C6 127.4(3) . . ? N1 C8 C9 111.1(3) . . ? C10 C9 C8 112.1(3) . . ? O2 C10 C9 111.1(2) . . ? O3 C12 C13 120.2(3) . . ? O3 C12 C17 121.5(3) . . ? C13 C12 C17 118.3(3) . . ? C14 C13 C12 121.8(3) . . ? C13 C14 C15 120.8(3) . . ? C16 C15 C14 118.2(3) . . ? C15 C16 C17 122.6(3) . . ? C16 C17 C12 118.3(3) . . ? C16 C17 C18 116.2(3) . . ? C12 C17 C18 125.5(3) . . ? N2 C18 C17 129.2(3) . . ? N2 C19 C20 110.4(3) . . ? C21 C20 C19 112.9(3) . . ? O4 C21 C20 109.2(3) . . ? O5 C23 C24 119.0(3) . . ? O5 C23 C28 122.9(3) . . ? C24 C23 C28 118.1(3) . . ? C25 C24 C23 120.8(3) . . ? C24 C25 C26 121.2(3) . . ? C27 C26 C25 118.3(3) . . ? C26 C27 C28 122.6(3) . . ? C27 C28 C23 119.0(3) . . ? C27 C28 C29 116.7(3) . . ? C23 C28 C29 124.3(3) . . ? N3 C29 C28 128.3(3) . . ? N3 C30 C31 111.0(3) . . ? C30 C31 C32 111.3(3) . . ? O6 C32 C31 107.5(3) . . ? O7 C34 C35 105.3(3) . . ? C36 C35 C34 101.5(3) . . ? C37 C36 C35 102.5(3) . . ? O7 C37 C36 104.9(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.834 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.105 data_b400 _database_code_depnum_ccdc_archive 'CCDC 918627' #TrackingRef 'web_deposit_cif_file_3_XiaoluSong_1360938597.B400.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 N2 Ni O4' _chemical_formula_weight 443.17 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5049(11) _cell_length_b 7.3081(7) _cell_length_c 13.8761(14) _cell_angle_alpha 90.00 _cell_angle_beta 111.595(2) _cell_angle_gamma 90.00 _cell_volume 1084.80(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1966 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 24.40 _exptl_crystal_description BLock _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6568 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7397 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2491 _reflns_number_gt 2058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0641P)^2^+0.0845P] 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 2491 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ni1 Ni 0.0000 0.5000 0.5000 0.03171(15) Uani 1 2 d S . . O1 O 0.16303(16) 0.5193(2) 0.51158(15) 0.0476(4) Uani 1 1 d . . . O2 O -0.25169(17) 1.0674(3) 0.62749(17) 0.0711(6) Uani 1 1 d . . . N1 N 0.01724(15) 0.6895(2) 0.60013(12) 0.0338(4) Uani 1 1 d . . . C1 C 0.25839(19) 0.5922(3) 0.58634(17) 0.0376(5) Uani 1 1 d . . . C2 C 0.3804(2) 0.5545(3) 0.5912(2) 0.0469(6) Uani 1 1 d . . . H2 H 0.3921 0.4782 0.5410 0.056 Uiso 1 1 calc R . . C3 C 0.4829(2) 0.6281(3) 0.66877(19) 0.0486(6) Uani 1 1 d . . . H3 H 0.5636 0.6006 0.6707 0.058 Uiso 1 1 calc R . . C4 C 0.4692(2) 0.7419(3) 0.7439(2) 0.0519(6) Uani 1 1 d . . . H4 H 0.5397 0.7912 0.7964 0.062 Uiso 1 1 calc R . . C5 C 0.3515(2) 0.7811(3) 0.74035(18) 0.0458(5) Uani 1 1 d . . . H5 H 0.3417 0.8583 0.7910 0.055 Uiso 1 1 calc R . . C6 C 0.24416(19) 0.7079(3) 0.66199(16) 0.0364(5) Uani 1 1 d . . . C7 C 0.12349(19) 0.7558(3) 0.66098(16) 0.0380(5) Uani 1 1 d . . . H7 H 0.1207 0.8443 0.7093 0.046 Uiso 1 1 calc R . . C8 C -0.09362(19) 0.7697(3) 0.61391(16) 0.0385(5) Uani 1 1 d . . . H8A H -0.0669 0.8372 0.6795 0.046 Uiso 1 1 calc R . . H8B H -0.1495 0.6711 0.6177 0.046 Uiso 1 1 calc R . . C9 C -0.1645(2) 0.8979(3) 0.52589(19) 0.0478(6) Uani 1 1 d . . . H9A H -0.1109 1.0019 0.5255 0.057 Uiso 1 1 calc R . . H9B H -0.1855 0.8332 0.4598 0.057 Uiso 1 1 calc R . . C10 C -0.2830(2) 0.9674(3) 0.5362(2) 0.0512(6) Uani 1 1 d . . . H10A H -0.3289 1.0451 0.4768 0.061 Uiso 1 1 calc R . . H10B H -0.3367 0.8641 0.5376 0.061 Uiso 1 1 calc R . . C11 C -0.3532(3) 1.1496(5) 0.6429(3) 0.0882(11) Uani 1 1 d . . . H11A H -0.4007 1.2208 0.5821 0.132 Uiso 1 1 calc R . . H11B H -0.3230 1.2292 0.7029 0.132 Uiso 1 1 calc R . . H11C H -0.4064 1.0557 0.6542 0.132 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 Ni1 0.0330(2) 0.0319(2) 0.0291(2) -0.00336(14) 0.01016(16) 0.00254(14) O1 0.0375(9) 0.0571(10) 0.0484(10) -0.0215(7) 0.0158(8) -0.0049(7) O2 0.0463(11) 0.0897(13) 0.0740(14) -0.0273(12) 0.0184(10) 0.0174(10) N1 0.0379(9) 0.0318(8) 0.0318(9) -0.0003(7) 0.0129(7) 0.0043(7) C1 0.0361(11) 0.0324(10) 0.0410(12) -0.0009(9) 0.0104(9) -0.0012(8) C2 0.0425(13) 0.0444(11) 0.0548(15) -0.0061(11) 0.0189(11) 0.0007(10) C3 0.0351(12) 0.0461(13) 0.0607(15) 0.0042(11) 0.0133(11) 0.0022(9) C4 0.0404(13) 0.0488(13) 0.0541(15) -0.0023(11) 0.0029(11) -0.0040(10) C5 0.0468(13) 0.0402(12) 0.0440(13) -0.0068(10) 0.0091(10) -0.0008(10) C6 0.0382(11) 0.0294(10) 0.0369(11) 0.0005(8) 0.0081(9) 0.0015(8) C7 0.0445(12) 0.0325(10) 0.0346(11) -0.0046(8) 0.0118(9) 0.0025(9) C8 0.0427(12) 0.0386(11) 0.0362(11) -0.0076(9) 0.0167(9) 0.0039(9) C9 0.0525(14) 0.0442(13) 0.0489(14) 0.0054(11) 0.0212(11) 0.0130(11) C10 0.0431(14) 0.0484(13) 0.0565(16) -0.0001(11) 0.0117(12) 0.0083(10) C11 0.082(2) 0.112(3) 0.088(2) 0.001(2) 0.0518(19) 0.040(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 Ni1 O1 1.8281(17) 3_566 ? Ni1 O1 1.8281(17) . ? Ni1 N1 1.9196(16) 3_566 ? Ni1 N1 1.9196(16) . ? O1 C1 1.314(3) . ? O2 C10 1.390(3) . ? O2 C11 1.398(3) . ? N1 C7 1.297(3) . ? N1 C8 1.479(2) . ? C1 C6 1.404(3) . ? C1 C2 1.407(3) . ? C2 C3 1.381(3) . ? C3 C4 1.387(3) . ? C4 C5 1.367(3) . ? C5 C6 1.416(3) . ? C6 C7 1.427(3) . ? C8 C9 1.517(3) . ? C9 C10 1.510(3) . ? 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 O1 Ni1 O1 180.0 3_566 . ? O1 Ni1 N1 92.95(7) 3_566 3_566 ? O1 Ni1 N1 87.05(7) . 3_566 ? O1 Ni1 N1 87.05(7) 3_566 . ? O1 Ni1 N1 92.95(7) . . ? N1 Ni1 N1 180.0 3_566 . ? C1 O1 Ni1 129.22(15) . . ? C10 O2 C11 114.5(2) . . ? C7 N1 C8 114.76(17) . . ? C7 N1 Ni1 124.21(14) . . ? C8 N1 Ni1 121.02(13) . . ? O1 C1 C6 122.79(19) . . ? O1 C1 C2 119.1(2) . . ? C6 C1 C2 118.1(2) . . ? C3 C2 C1 120.8(2) . . ? C2 C3 C4 121.3(2) . . ? C5 C4 C3 118.9(2) . . ? C4 C5 C6 121.4(2) . . ? C1 C6 C5 119.53(19) . . ? C1 C6 C7 121.41(18) . . ? C5 C6 C7 119.06(19) . . ? N1 C7 C6 126.54(19) . . ? N1 C8 C9 111.98(16) . . ? C10 C9 C8 111.57(19) . . ? O2 C10 C9 108.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.093 data_b632 _database_code_depnum_ccdc_archive 'CCDC 918628' #TrackingRef 'web_deposit_cif_file_4_XiaoluSong_1360938597.B632.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 Cl N3 Ni2 O3 S3' _chemical_formula_weight 879.79 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3237(8) _cell_length_b 13.6103(9) _cell_length_c 13.7343(9) _cell_angle_alpha 60.4860(10) _cell_angle_beta 79.9780(10) _cell_angle_gamma 79.0150(10) _cell_volume 1959.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2257 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.97 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8086 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25496 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8969 _reflns_number_gt 5410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. One of the methyl groups was disordered into two positions with occupancy ratio=40:60. The following restraints were applied on the disordered atoms: delu 0.005 C42 c42A SADI 0.02 S3 C42 S3 C42A SIMU 0.001 0.001 C42 C42A ; _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^)+(0.0537P)^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 8969 _refine_ls_number_parameters 501 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C42 C 0.725(3) 1.484(3) 0.626(3) 0.101(6) Uani 0.40(5) 1 d PDU A 1 H42A H 0.7669 1.4617 0.5719 0.151 Uiso 0.40(5) 1 calc PR A 1 H42B H 0.7739 1.5153 0.6498 0.151 Uiso 0.40(5) 1 calc PR A 1 H42C H 0.6640 1.5416 0.5917 0.151 Uiso 0.40(5) 1 calc PR A 1 C42A C 0.766(2) 1.464(2) 0.655(3) 0.101(6) Uani 0.60(5) 1 d PDU A 2 H42D H 0.7879 1.4580 0.5868 0.152 Uiso 0.60(5) 1 calc PR A 2 H42E H 0.8319 1.4496 0.6926 0.152 Uiso 0.60(5) 1 calc PR A 2 H42F H 0.7298 1.5402 0.6365 0.152 Uiso 0.60(5) 1 calc PR A 2 Ni1 Ni 0.81367(5) 0.74475(5) 0.99788(5) 0.03451(18) Uani 1 1 d . . . Ni2 Ni 0.81079(5) 0.98159(5) 0.84179(5) 0.03349(18) Uani 1 1 d . . . Cl1 Cl 0.91337(11) 0.63059(10) 1.15749(11) 0.0447(3) Uani 1 1 d . . . S1 S 0.64306(11) 0.67156(11) 1.08229(12) 0.0444(3) Uani 1 1 d . . . S2 S 0.95058(11) 1.07623(10) 0.85195(11) 0.0413(3) Uani 1 1 d . . . S3 S 0.67208(16) 1.36099(14) 0.74738(17) 0.0801(6) Uani 1 1 d D . . O1 O 0.9333(3) 0.8313(2) 0.8945(3) 0.0371(8) Uani 1 1 d . . . O2 O 0.7255(3) 0.8732(3) 0.8368(3) 0.0381(8) Uani 1 1 d . . . O3 O 0.7714(3) 0.8960(3) 1.0059(3) 0.0415(9) Uani 1 1 d . A . N1 N 0.8453(3) 0.6241(3) 0.9482(3) 0.0328(9) Uani 1 1 d . . . N2 N 0.8660(3) 1.0494(3) 0.6784(3) 0.0362(10) Uani 1 1 d . . . N3 N 0.6758(3) 1.1032(3) 0.8269(3) 0.0376(10) Uani 1 1 d . A . C1 C 0.6728(4) 0.5539(4) 1.0551(4) 0.0370(12) Uani 1 1 d . . . C2 C 0.5967(5) 0.4756(5) 1.0981(5) 0.0532(15) Uani 1 1 d . . . H2 H 0.5309 0.4861 1.1401 0.064 Uiso 1 1 calc R . . C3 C 0.6169(5) 0.3834(5) 1.0797(5) 0.0624(17) Uani 1 1 d . . . H3 H 0.5653 0.3305 1.1093 0.075 Uiso 1 1 calc R . . C4 C 0.7123(5) 0.3683(5) 1.0181(5) 0.0551(16) Uani 1 1 d . . . H4 H 0.7264 0.3041 1.0067 0.066 Uiso 1 1 calc R . . C5 C 0.7880(5) 0.4460(4) 0.9725(4) 0.0451(13) Uani 1 1 d . . . H5 H 0.8519 0.4357 0.9282 0.054 Uiso 1 1 calc R . . C6 C 0.7702(4) 0.5403(4) 0.9917(4) 0.0342(11) Uani 1 1 d . . . C7 C 0.9348(4) 0.6173(4) 0.8858(4) 0.0372(12) Uani 1 1 d . . . H7 H 0.9472 0.5543 0.8727 0.045 Uiso 1 1 calc R . . C8 C 1.0180(4) 0.6941(4) 0.8339(4) 0.0329(11) Uani 1 1 d . . . C9 C 1.1088(4) 0.6611(4) 0.7745(4) 0.0409(12) Uani 1 1 d . . . H9 H 1.1120 0.5921 0.7734 0.049 Uiso 1 1 calc R . . C10 C 1.1930(5) 0.7276(4) 0.7181(4) 0.0488(14) Uani 1 1 d . . . H10 H 1.2529 0.7049 0.6779 0.059 Uiso 1 1 calc R . . C11 C 1.1884(4) 0.8283(4) 0.7211(4) 0.0463(13) Uani 1 1 d . . . H11 H 1.2463 0.8738 0.6833 0.056 Uiso 1 1 calc R . . C12 C 1.1015(4) 0.8629(4) 0.7777(4) 0.0449(13) Uani 1 1 d . . . H12 H 1.1003 0.9326 0.7768 0.054 Uiso 1 1 calc R . . C13 C 1.0138(4) 0.7978(4) 0.8374(4) 0.0332(11) Uani 1 1 d . . . C14 C 0.6393(5) 0.6028(5) 1.2335(4) 0.0575(16) Uani 1 1 d . . . H14A H 0.5767 0.5592 1.2668 0.086 Uiso 1 1 calc R . . H14B H 0.6317 0.6599 1.2578 0.086 Uiso 1 1 calc R . . H14C H 0.7076 0.5522 1.2572 0.086 Uiso 1 1 calc R . . C15 C 0.9617(4) 1.1737(4) 0.7065(4) 0.0402(12) Uani 1 1 d . . . C16 C 1.0141(5) 1.2710(4) 0.6638(5) 0.0517(15) Uani 1 1 d . . . H16 H 1.0437 1.2867 0.7126 0.062 Uiso 1 1 calc R . . C17 C 1.0223(5) 1.3438(5) 0.5505(5) 0.0660(18) Uani 1 1 d . . . H17 H 1.0578 1.4093 0.5219 0.079 Uiso 1 1 calc R . . C18 C 0.9793(6) 1.3222(5) 0.4786(5) 0.074(2) Uani 1 1 d . . . H18 H 0.9853 1.3733 0.4011 0.089 Uiso 1 1 calc R . . C19 C 0.9272(5) 1.2262(5) 0.5184(5) 0.0593(16) Uani 1 1 d . . . H19 H 0.8960 1.2134 0.4685 0.071 Uiso 1 1 calc R . . C20 C 0.9211(4) 1.1479(4) 0.6334(4) 0.0409(12) Uani 1 1 d . . . C21 C 0.8588(4) 1.0027(4) 0.6185(4) 0.0451(13) Uani 1 1 d . . . H21 H 0.8988 1.0320 0.5471 0.054 Uiso 1 1 calc R . . C22 C 0.7965(5) 0.9103(4) 0.6475(4) 0.0442(13) Uani 1 1 d . . . C23 C 0.7986(5) 0.8794(5) 0.5635(5) 0.0631(17) Uani 1 1 d . . . H23 H 0.8429 0.9157 0.4955 0.076 Uiso 1 1 calc R . . C24 C 0.7379(6) 0.7978(6) 0.5779(6) 0.079(2) Uani 1 1 d . . . H24 H 0.7413 0.7775 0.5210 0.095 Uiso 1 1 calc R . . C25 C 0.6709(6) 0.7451(5) 0.6782(5) 0.0677(19) Uani 1 1 d . . . H25 H 0.6277 0.6901 0.6885 0.081 Uiso 1 1 calc R . . C26 C 0.6681(5) 0.7729(4) 0.7606(5) 0.0507(14) Uani 1 1 d . . . H26 H 0.6219 0.7366 0.8271 0.061 Uiso 1 1 calc R . . C27 C 0.7314(4) 0.8541(4) 0.7511(4) 0.0385(12) Uani 1 1 d . . . C28 C 0.9014(5) 1.1652(4) 0.9182(4) 0.0518(15) Uani 1 1 d . . . H28A H 0.9611 1.2053 0.9131 0.078 Uiso 1 1 calc R . . H28B H 0.8769 1.1182 0.9966 0.078 Uiso 1 1 calc R . . H28C H 0.8398 1.2199 0.8803 0.078 Uiso 1 1 calc R . . C29 C 0.6372(5) 1.3001(4) 0.6703(5) 0.0537(15) Uani 1 1 d . A . C30 C 0.6044(5) 1.3686(5) 0.5607(6) 0.072(2) Uani 1 1 d . . . H30 H 0.6048 1.4478 0.5261 0.086 Uiso 1 1 calc R A . C31 C 0.5719(6) 1.3217(6) 0.5038(6) 0.082(2) Uani 1 1 d . A . H31 H 0.5474 1.3694 0.4320 0.098 Uiso 1 1 calc R . . C32 C 0.5747(6) 1.2068(6) 0.5498(6) 0.080(2) Uani 1 1 d . . . H32 H 0.5550 1.1746 0.5094 0.096 Uiso 1 1 calc R A . C33 C 0.6073(5) 1.1386(5) 0.6574(5) 0.0587(16) Uani 1 1 d . A . H33 H 0.6080 1.0595 0.6897 0.070 Uiso 1 1 calc R . . C34 C 0.6387(4) 1.1818(4) 0.7192(4) 0.0444(13) Uani 1 1 d . . . C35 C 0.6214(4) 1.1091(4) 0.9129(4) 0.0416(13) Uani 1 1 d . . . H35 H 0.5598 1.1654 0.8980 0.050 Uiso 1 1 calc R A . C36 C 0.6423(4) 1.0411(4) 1.0285(4) 0.0391(12) Uani 1 1 d . A . C37 C 0.5877(5) 1.0799(5) 1.1035(5) 0.0555(16) Uani 1 1 d . . . H37 H 0.5379 1.1472 1.0762 0.067 Uiso 1 1 calc R A . C38 C 0.6039(5) 1.0245(6) 1.2136(5) 0.0684(19) Uani 1 1 d . A . H38 H 0.5677 1.0540 1.2616 0.082 Uiso 1 1 calc R . . C39 C 0.6746(6) 0.9239(6) 1.2549(5) 0.0700(19) Uani 1 1 d . . . H39 H 0.6859 0.8846 1.3316 0.084 Uiso 1 1 calc R A . C40 C 0.7287(5) 0.8801(5) 1.1854(4) 0.0509(14) Uani 1 1 d . A . H40 H 0.7750 0.8106 1.2157 0.061 Uiso 1 1 calc R . . C41 C 0.7158(4) 0.9373(4) 1.0711(4) 0.0362(12) 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 C42 0.053(12) 0.053(8) 0.167(15) -0.030(8) -0.003(11) -0.010(10) C42A 0.053(12) 0.053(8) 0.167(15) -0.030(8) -0.003(11) -0.010(10) Ni1 0.0383(4) 0.0208(3) 0.0380(4) -0.0112(3) 0.0023(3) -0.0026(3) Ni2 0.0407(4) 0.0202(3) 0.0311(4) -0.0072(3) -0.0011(3) -0.0018(3) Cl1 0.0548(9) 0.0270(6) 0.0480(8) -0.0133(6) -0.0108(6) -0.0035(6) S1 0.0370(8) 0.0307(7) 0.0516(8) -0.0129(6) 0.0039(6) -0.0003(6) S2 0.0502(9) 0.0253(6) 0.0418(8) -0.0100(6) -0.0093(6) -0.0026(6) S3 0.0851(14) 0.0395(9) 0.0963(14) -0.0131(9) -0.0152(11) -0.0144(9) O1 0.040(2) 0.0190(16) 0.043(2) -0.0102(15) 0.0016(16) 0.0000(14) O2 0.043(2) 0.0331(18) 0.0341(19) -0.0130(16) -0.0023(16) -0.0054(16) O3 0.060(2) 0.0211(16) 0.0332(19) -0.0104(15) 0.0006(17) 0.0058(16) N1 0.039(3) 0.0214(19) 0.034(2) -0.0111(18) -0.0030(19) -0.0034(17) N2 0.041(3) 0.029(2) 0.035(2) -0.0117(19) -0.0024(19) -0.0059(19) N3 0.043(3) 0.020(2) 0.036(2) -0.0048(19) -0.006(2) 0.0017(18) C1 0.030(3) 0.027(3) 0.046(3) -0.011(2) -0.009(2) -0.001(2) C2 0.040(3) 0.044(3) 0.064(4) -0.017(3) -0.007(3) -0.005(3) C3 0.047(4) 0.049(4) 0.088(5) -0.025(4) -0.006(3) -0.019(3) C4 0.063(4) 0.040(3) 0.071(4) -0.029(3) -0.009(3) -0.016(3) C5 0.051(4) 0.039(3) 0.050(3) -0.023(3) 0.000(3) -0.011(3) C6 0.038(3) 0.027(2) 0.037(3) -0.013(2) -0.011(2) -0.003(2) C7 0.046(3) 0.026(3) 0.036(3) -0.013(2) -0.010(2) 0.005(2) C8 0.036(3) 0.029(2) 0.031(3) -0.012(2) -0.003(2) -0.003(2) C9 0.047(3) 0.034(3) 0.038(3) -0.017(2) 0.000(3) -0.001(2) C10 0.056(4) 0.045(3) 0.041(3) -0.022(3) 0.010(3) -0.004(3) C11 0.044(3) 0.040(3) 0.044(3) -0.011(3) 0.007(3) -0.016(3) C12 0.047(3) 0.030(3) 0.053(3) -0.016(3) 0.002(3) -0.012(2) C13 0.032(3) 0.026(2) 0.035(3) -0.012(2) -0.006(2) 0.005(2) C14 0.054(4) 0.056(4) 0.055(4) -0.024(3) 0.016(3) -0.014(3) C15 0.041(3) 0.034(3) 0.038(3) -0.014(2) -0.001(2) -0.001(2) C16 0.050(4) 0.039(3) 0.061(4) -0.019(3) -0.001(3) -0.012(3) C17 0.083(5) 0.039(3) 0.059(4) -0.005(3) 0.009(4) -0.035(3) C18 0.101(6) 0.055(4) 0.044(4) -0.002(3) 0.007(4) -0.039(4) C19 0.082(5) 0.048(4) 0.038(3) -0.010(3) -0.001(3) -0.021(3) C20 0.043(3) 0.031(3) 0.038(3) -0.010(2) 0.004(2) -0.009(2) C21 0.053(4) 0.044(3) 0.028(3) -0.010(3) 0.005(2) -0.010(3) C22 0.054(4) 0.033(3) 0.044(3) -0.016(3) -0.003(3) -0.009(3) C23 0.091(5) 0.049(4) 0.049(4) -0.023(3) 0.005(3) -0.017(3) C24 0.123(7) 0.066(5) 0.064(5) -0.037(4) -0.023(5) -0.018(5) C25 0.099(6) 0.049(4) 0.063(4) -0.023(3) -0.023(4) -0.023(4) C26 0.057(4) 0.040(3) 0.055(4) -0.017(3) -0.016(3) -0.011(3) C27 0.037(3) 0.023(2) 0.045(3) -0.008(2) -0.012(2) 0.003(2) C28 0.068(4) 0.042(3) 0.047(3) -0.020(3) -0.007(3) -0.010(3) C29 0.050(4) 0.034(3) 0.050(4) -0.004(3) 0.001(3) 0.000(3) C30 0.069(5) 0.041(4) 0.059(4) 0.006(3) 0.003(4) 0.001(3) C31 0.088(6) 0.069(5) 0.051(4) -0.008(4) -0.014(4) 0.020(4) C32 0.084(5) 0.074(5) 0.073(5) -0.030(4) -0.035(4) 0.022(4) C33 0.070(4) 0.038(3) 0.056(4) -0.013(3) -0.024(3) 0.009(3) C34 0.037(3) 0.033(3) 0.044(3) -0.007(3) -0.002(2) 0.004(2) C35 0.036(3) 0.029(3) 0.052(3) -0.016(3) -0.004(3) 0.005(2) C36 0.042(3) 0.033(3) 0.042(3) -0.018(2) 0.002(2) -0.004(2) C37 0.058(4) 0.044(3) 0.058(4) -0.027(3) 0.010(3) 0.001(3) C38 0.073(5) 0.082(5) 0.055(4) -0.046(4) 0.003(3) 0.008(4) C39 0.075(5) 0.081(5) 0.041(4) -0.026(4) -0.002(3) 0.004(4) C40 0.050(4) 0.047(3) 0.044(3) -0.019(3) 0.000(3) 0.006(3) C41 0.040(3) 0.028(3) 0.033(3) -0.009(2) 0.002(2) -0.008(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 C42 S3 1.819(15) . ? C42A S3 1.813(11) . ? Ni1 O1 1.965(3) . ? Ni1 N1 2.020(4) . ? Ni1 O3 2.077(3) . ? Ni1 O2 2.332(3) . ? Ni1 S1 2.3599(15) . ? Ni1 Cl1 2.3629(14) . ? Ni1 Ni2 2.8569(8) . ? Ni2 O3 1.980(3) . ? Ni2 O2 2.000(3) . ? Ni2 N2 2.005(4) . ? Ni2 N3 2.070(4) . ? Ni2 O1 2.176(3) . ? Ni2 S2 2.3986(15) . ? S1 C1 1.776(5) . ? S1 C14 1.805(5) . ? S2 C15 1.770(5) . ? S2 C28 1.810(5) . ? S3 C29 1.775(6) . ? O1 C13 1.310(5) . ? O2 C27 1.312(6) . ? O3 C41 1.312(5) . ? N1 C7 1.292(6) . ? N1 C6 1.433(6) . ? N2 C21 1.285(6) . ? N2 C20 1.423(6) . ? N3 C35 1.284(6) . ? N3 C34 1.425(6) . ? C1 C2 1.391(7) . ? C1 C6 1.395(7) . ? C2 C3 1.369(7) . ? C3 C4 1.369(8) . ? C4 C5 1.378(7) . ? C5 C6 1.404(6) . ? C7 C8 1.440(7) . ? C8 C9 1.405(6) . ? C8 C13 1.427(6) . ? C9 C10 1.371(7) . ? C10 C11 1.383(7) . ? C11 C12 1.361(7) . ? C12 C13 1.401(7) . ? C15 C16 1.394(7) . ? C15 C20 1.405(7) . ? C16 C17 1.370(7) . ? C17 C18 1.367(8) . ? C18 C19 1.383(8) . ? C19 C20 1.402(7) . ? C21 C22 1.448(7) . ? C22 C23 1.405(7) . ? C22 C27 1.420(7) . ? C23 C24 1.372(8) . ? C24 C25 1.396(9) . ? C25 C26 1.352(7) . ? C26 C27 1.414(7) . ? C29 C34 1.404(7) . ? C29 C30 1.408(8) . ? C30 C31 1.371(9) . ? C31 C32 1.363(9) . ? C32 C33 1.385(8) . ? C33 C34 1.382(7) . ? C35 C36 1.430(7) . ? C36 C37 1.397(7) . ? C36 C41 1.429(6) . ? C37 C38 1.350(8) . ? C38 C39 1.381(8) . ? C39 C40 1.378(7) . ? C40 C41 1.389(7) . ? 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 O1 Ni1 N1 94.10(14) . . ? O1 Ni1 O3 79.52(13) . . ? N1 Ni1 O3 165.03(14) . . ? O1 Ni1 O2 76.89(12) . . ? N1 Ni1 O2 91.65(13) . . ? O3 Ni1 O2 73.77(12) . . ? O1 Ni1 S1 165.24(10) . . ? N1 Ni1 S1 85.98(12) . . ? O3 Ni1 S1 96.75(10) . . ? O2 Ni1 S1 88.35(9) . . ? O1 Ni1 Cl1 98.33(10) . . ? N1 Ni1 Cl1 92.55(11) . . ? O3 Ni1 Cl1 101.73(10) . . ? O2 Ni1 Cl1 173.86(9) . . ? S1 Ni1 Cl1 96.41(5) . . ? O1 Ni1 Ni2 49.51(9) . . ? N1 Ni1 Ni2 122.31(11) . . ? O3 Ni1 Ni2 43.87(9) . . ? O2 Ni1 Ni2 43.91(8) . . ? S1 Ni1 Ni2 118.69(4) . . ? Cl1 Ni1 Ni2 129.97(4) . . ? O3 Ni2 O2 83.64(13) . . ? O3 Ni2 N2 172.04(14) . . ? O2 Ni2 N2 94.24(14) . . ? O3 Ni2 N3 90.64(15) . . ? O2 Ni2 N3 95.43(14) . . ? N2 Ni2 N3 97.21(16) . . ? O3 Ni2 O1 76.85(12) . . ? O2 Ni2 O1 79.99(12) . . ? N2 Ni2 O1 95.23(14) . . ? N3 Ni2 O1 167.03(14) . . ? O3 Ni2 S2 96.17(11) . . ? O2 Ni2 S2 165.94(10) . . ? N2 Ni2 S2 84.01(12) . . ? N3 Ni2 S2 98.63(11) . . ? O1 Ni2 S2 86.27(9) . . ? O3 Ni2 Ni1 46.65(9) . . ? O2 Ni2 Ni1 53.94(9) . . ? N2 Ni2 Ni1 126.35(11) . . ? N3 Ni2 Ni1 124.50(11) . . ? O1 Ni2 Ni1 43.40(8) . . ? S2 Ni2 Ni1 116.51(4) . . ? C1 S1 C14 102.1(2) . . ? C1 S1 Ni1 96.05(17) . . ? C14 S1 Ni1 110.6(2) . . ? C15 S2 C28 104.1(2) . . ? C15 S2 Ni2 94.91(18) . . ? C28 S2 Ni2 114.64(19) . . ? C29 S3 C42A 107.3(12) . . ? C29 S3 C42 96.1(18) . . ? C42A S3 C42 20.0(12) . . ? C13 O1 Ni1 127.1(3) . . ? C13 O1 Ni2 131.6(3) . . ? Ni1 O1 Ni2 87.09(12) . . ? C27 O2 Ni2 124.8(3) . . ? C27 O2 Ni1 121.8(3) . . ? Ni2 O2 Ni1 82.14(11) . . ? C41 O3 Ni2 127.0(3) . . ? C41 O3 Ni1 141.4(3) . . ? Ni2 O3 Ni1 89.48(12) . . ? C7 N1 C6 120.6(4) . . ? C7 N1 Ni1 121.1(3) . . ? C6 N1 Ni1 118.0(3) . . ? C21 N2 C20 121.2(4) . . ? C21 N2 Ni2 122.1(3) . . ? C20 N2 Ni2 116.6(3) . . ? C35 N3 C34 117.9(4) . . ? C35 N3 Ni2 121.9(3) . . ? C34 N3 Ni2 120.2(3) . . ? C2 C1 C6 120.5(5) . . ? C2 C1 S1 118.6(4) . . ? C6 C1 S1 120.9(4) . . ? C3 C2 C1 120.4(6) . . ? C2 C3 C4 119.9(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C6 120.4(5) . . ? C1 C6 C5 117.9(5) . . ? C1 C6 N1 118.3(4) . . ? C5 C6 N1 123.8(4) . . ? N1 C7 C8 128.1(4) . . ? C9 C8 C13 119.5(4) . . ? C9 C8 C7 114.8(4) . . ? C13 C8 C7 125.7(4) . . ? C10 C9 C8 121.3(5) . . ? C9 C10 C11 119.1(5) . . ? C12 C11 C10 121.1(5) . . ? C11 C12 C13 122.1(5) . . ? O1 C13 C12 120.7(4) . . ? O1 C13 C8 122.4(4) . . ? C12 C13 C8 116.9(4) . . ? C16 C15 C20 120.2(5) . . ? C16 C15 S2 121.5(4) . . ? C20 C15 S2 118.2(4) . . ? C17 C16 C15 119.8(5) . . ? C18 C17 C16 120.7(5) . . ? C17 C18 C19 120.8(6) . . ? C18 C19 C20 119.9(6) . . ? C19 C20 C15 118.4(5) . . ? C19 C20 N2 121.8(5) . . ? C15 C20 N2 119.5(4) . . ? N2 C21 C22 127.8(5) . . ? C23 C22 C27 119.2(5) . . ? C23 C22 C21 116.0(5) . . ? C27 C22 C21 124.8(5) . . ? C24 C23 C22 121.8(6) . . ? C23 C24 C25 119.1(6) . . ? C26 C25 C24 120.1(6) . . ? C25 C26 C27 122.9(6) . . ? O2 C27 C26 118.5(5) . . ? O2 C27 C22 124.7(4) . . ? C26 C27 C22 116.8(5) . . ? C34 C29 C30 118.5(6) . . ? C34 C29 S3 120.2(4) . . ? C30 C29 S3 121.2(5) . . ? C31 C30 C29 121.0(6) . . ? C32 C31 C30 120.9(6) . . ? C31 C32 C33 118.4(7) . . ? C34 C33 C32 122.9(6) . . ? C33 C34 C29 118.2(5) . . ? C33 C34 N3 118.0(5) . . ? C29 C34 N3 123.8(5) . . ? N3 C35 C36 128.5(5) . . ? C37 C36 C41 118.4(5) . . ? C37 C36 C35 117.5(5) . . ? C41 C36 C35 124.1(4) . . ? C38 C37 C36 122.5(5) . . ? C37 C38 C39 119.0(5) . . ? C40 C39 C38 121.0(6) . . ? C39 C40 C41 121.0(5) . . ? O3 C41 C40 119.8(4) . . ? O3 C41 C36 122.2(4) . . ? C40 C41 C36 118.0(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.692 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.091 data_b745 _database_code_depnum_ccdc_archive 'CCDC 918629' #TrackingRef 'web_deposit_cif_file_5_XiaoluSong_1360938597.B745.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 N4 Na4 O8' _chemical_formula_weight 996.94 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 16.3906(9) _cell_length_b 16.5378(9) _cell_length_c 18.1746(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.2930(10) _cell_angle_gamma 90.00 _cell_volume 4847.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2169 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.26 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9483 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16970 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10146 _reflns_number_gt 8334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0392P)^2^+2.0623P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(3) _refine_ls_number_reflns 10146 _refine_ls_number_parameters 653 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.10883(7) 0.84848(7) 0.00533(7) 0.0175(3) Uani 1 1 d . . . Na2 Na 0.06055(8) 1.03907(8) 0.00326(7) 0.0197(3) Uani 1 1 d . . . Na3 Na 0.23646(7) 0.97691(7) 0.09592(7) 0.0171(3) Uani 1 1 d . . . Na4 Na 0.07109(8) 0.92640(8) 0.15391(7) 0.0177(3) Uani 1 1 d . . . O1 O -0.00061(13) 0.91621(14) 0.03048(13) 0.0187(5) Uani 1 1 d . . . O2 O 0.15351(13) 0.71890(14) -0.01189(13) 0.0215(5) Uani 1 1 d . . . O3 O 0.12455(14) 1.04504(13) 0.13070(13) 0.0175(5) Uani 1 1 d . . . O4 O -0.02627(14) 0.85128(14) 0.20034(13) 0.0215(5) Uani 1 1 d . . . O5 O 0.16661(13) 0.96804(13) -0.02739(13) 0.0183(5) Uani 1 1 d . . . O6 O 0.01056(15) 1.16822(15) 0.01384(14) 0.0249(6) Uani 1 1 d . . . O7 O 0.18719(13) 0.85715(13) 0.12832(12) 0.0158(5) Uani 1 1 d . . . O8 O 0.34726(14) 1.04916(14) 0.06843(14) 0.0219(5) Uani 1 1 d . . . N1 N -0.00402(16) 0.76273(16) -0.05411(15) 0.0163(6) Uani 1 1 d . . . N2 N 0.01505(16) 1.00317(17) 0.24221(15) 0.0165(6) Uani 1 1 d . . . N3 N 0.10690(17) 1.12922(17) -0.08518(16) 0.0193(6) Uani 1 1 d . . . N4 N 0.36492(16) 0.90696(16) 0.13845(15) 0.0162(6) Uani 1 1 d . . . C1 C -0.07996(19) 0.90549(19) 0.01991(18) 0.0161(7) Uani 1 1 d . . . C2 C -0.1310(2) 0.9561(2) 0.0558(2) 0.0222(8) Uani 1 1 d . . . H2 H -0.1053 0.9970 0.0887 0.027 Uiso 1 1 calc R . . C3 C -0.2156(2) 0.9486(2) 0.0453(2) 0.0273(8) Uani 1 1 d . . . H3 H -0.2466 0.9832 0.0716 0.033 Uiso 1 1 calc R . . C4 C -0.2566(2) 0.8905(2) -0.0037(2) 0.0305(9) Uani 1 1 d . . . H4 H -0.3154 0.8866 -0.0127 0.037 Uiso 1 1 calc R . . C5 C -0.2099(2) 0.8395(2) -0.0384(2) 0.0252(8) Uani 1 1 d . . . H5 H -0.2374 0.7995 -0.0714 0.030 Uiso 1 1 calc R . . C6 C -0.1226(2) 0.84356(19) -0.02743(19) 0.0190(7) Uani 1 1 d . . . C7 C -0.0820(2) 0.7789(2) -0.06096(18) 0.0187(7) Uani 1 1 d . . . H7 H -0.1180 0.7434 -0.0925 0.022 Uiso 1 1 calc R . . C8 C 0.0225(2) 0.69067(19) -0.08544(17) 0.0158(7) Uani 1 1 d . . . C9 C -0.0274(2) 0.6406(2) -0.13685(19) 0.0215(7) Uani 1 1 d . . . H9 H -0.0840 0.6542 -0.1533 0.026 Uiso 1 1 calc R . . C10 C 0.0044(2) 0.5710(2) -0.1644(2) 0.0262(8) Uani 1 1 d . . . H10 H -0.0302 0.5381 -0.1998 0.031 Uiso 1 1 calc R . . C11 C 0.0858(2) 0.5500(2) -0.1401(2) 0.0291(9) Uani 1 1 d . . . H11 H 0.1073 0.5023 -0.1586 0.035 Uiso 1 1 calc R . . C12 C 0.1370(2) 0.5981(2) -0.0885(2) 0.0209(7) Uani 1 1 d . . . H12 H 0.1932 0.5832 -0.0713 0.025 Uiso 1 1 calc R . . C13 C 0.1055(2) 0.66769(19) -0.06271(18) 0.0171(7) Uani 1 1 d . . . C14 C 0.2393(2) 0.6987(2) 0.0118(2) 0.0248(8) Uani 1 1 d . . . H14A H 0.2437 0.6477 0.0397 0.037 Uiso 1 1 calc R . . H14B H 0.2669 0.7418 0.0440 0.037 Uiso 1 1 calc R . . H14C H 0.2659 0.6929 -0.0321 0.037 Uiso 1 1 calc R . . C15 C 0.13228(19) 1.1126(2) 0.16833(19) 0.0172(7) Uani 1 1 d . . . C16 C 0.1768(2) 1.1781(2) 0.1436(2) 0.0224(8) Uani 1 1 d . . . H16 H 0.2008 1.1709 0.1002 0.027 Uiso 1 1 calc R . . C17 C 0.1865(2) 1.2514(2) 0.1798(2) 0.0267(8) Uani 1 1 d . . . H17 H 0.2157 1.2938 0.1605 0.032 Uiso 1 1 calc R . . C18 C 0.1541(2) 1.2639(2) 0.2443(2) 0.0288(9) Uani 1 1 d . . . H18 H 0.1625 1.3138 0.2703 0.035 Uiso 1 1 calc R . . C19 C 0.1094(2) 1.2027(2) 0.2701(2) 0.0246(8) Uani 1 1 d . . . H19 H 0.0862 1.2117 0.3137 0.030 Uiso 1 1 calc R . . C20 C 0.0970(2) 1.1271(2) 0.23380(19) 0.0189(7) Uani 1 1 d . . . C21 C 0.0450(2) 1.0715(2) 0.26712(19) 0.0196(7) Uani 1 1 d . . . H21 H 0.0315 1.0882 0.3135 0.023 Uiso 1 1 calc R . . C22 C -0.0408(2) 0.9615(2) 0.28039(19) 0.0201(7) Uani 1 1 d . . . C23 C -0.0765(2) 0.9931(2) 0.3388(2) 0.0267(8) Uani 1 1 d . . . H23 H -0.0604 1.0454 0.3577 0.032 Uiso 1 1 calc R . . C24 C -0.1343(2) 0.9503(3) 0.3696(2) 0.0338(10) Uani 1 1 d . . . H24 H -0.1577 0.9732 0.4090 0.041 Uiso 1 1 calc R . . C25 C -0.1582(2) 0.8741(3) 0.3430(2) 0.0324(9) Uani 1 1 d . . . H25 H -0.1988 0.8451 0.3637 0.039 Uiso 1 1 calc R . . C26 C -0.1234(2) 0.8399(2) 0.2867(2) 0.0263(8) Uani 1 1 d . . . H26 H -0.1395 0.7872 0.2688 0.032 Uiso 1 1 calc R . . C27 C -0.0646(2) 0.8829(2) 0.25606(18) 0.0207(7) Uani 1 1 d . . . C28 C -0.0620(2) 0.7799(2) 0.1638(2) 0.0246(8) Uani 1 1 d . . . H28A H -0.0563 0.7351 0.1996 0.037 Uiso 1 1 calc R . . H28B H -0.0334 0.7663 0.1224 0.037 Uiso 1 1 calc R . . H28C H -0.1209 0.7893 0.1442 0.037 Uiso 1 1 calc R . . C29 C 0.20588(19) 0.9700(2) -0.08357(18) 0.0168(7) Uani 1 1 d . . . C30 C 0.2556(2) 0.9037(2) -0.09749(19) 0.0217(7) Uani 1 1 d . . . H30 H 0.2604 0.8588 -0.0644 0.026 Uiso 1 1 calc R . . C31 C 0.2977(2) 0.9012(2) -0.1570(2) 0.0241(8) Uani 1 1 d . . . H31 H 0.3292 0.8547 -0.1646 0.029 Uiso 1 1 calc R . . C32 C 0.2941(2) 0.9662(2) -0.2058(2) 0.0244(8) Uani 1 1 d . . . H32 H 0.3229 0.9649 -0.2468 0.029 Uiso 1 1 calc R . . C33 C 0.2476(2) 1.0328(2) -0.1934(2) 0.0240(8) Uani 1 1 d . . . H33 H 0.2460 1.0779 -0.2260 0.029 Uiso 1 1 calc R . . C34 C 0.2023(2) 1.0369(2) -0.13416(19) 0.0178(7) Uani 1 1 d . . . C35 C 0.1561(2) 1.1110(2) -0.1303(2) 0.0227(8) Uani 1 1 d . . . H35 H 0.1632 1.1514 -0.1658 0.027 Uiso 1 1 calc R . . C36 C 0.06919(19) 1.2078(2) -0.0906(2) 0.0191(7) Uani 1 1 d . . . C37 C 0.0753(2) 1.2646(2) -0.1456(2) 0.0277(8) Uani 1 1 d . . . H37 H 0.1049 1.2513 -0.1843 0.033 Uiso 1 1 calc R . . C38 C 0.0392(2) 1.3406(2) -0.1453(2) 0.0327(9) Uani 1 1 d . . . H38 H 0.0433 1.3780 -0.1841 0.039 Uiso 1 1 calc R . . C39 C -0.0027(2) 1.3617(2) -0.0889(2) 0.0306(9) Uani 1 1 d . . . H39 H -0.0245 1.4147 -0.0868 0.037 Uiso 1 1 calc R . . C40 C -0.0127(2) 1.3050(2) -0.0350(2) 0.0279(9) Uani 1 1 d . . . H40 H -0.0431 1.3190 0.0030 0.034 Uiso 1 1 calc R . . C41 C 0.0211(2) 1.2282(2) -0.0360(2) 0.0214(8) Uani 1 1 d . . . C42 C -0.0338(2) 1.1889(2) 0.0720(2) 0.0301(9) Uani 1 1 d . . . H42A H -0.0043 1.2322 0.1027 0.045 Uiso 1 1 calc R . . H42B H -0.0379 1.1414 0.1032 0.045 Uiso 1 1 calc R . . H42C H -0.0896 1.2075 0.0499 0.045 Uiso 1 1 calc R . . C43 C 0.2208(2) 0.79491(19) 0.16614(17) 0.0157(7) Uani 1 1 d . . . C44 C 0.1704(2) 0.7304(2) 0.18319(19) 0.0211(7) Uani 1 1 d . . . H44 H 0.1121 0.7342 0.1672 0.025 Uiso 1 1 calc R . . C45 C 0.2020(2) 0.6627(2) 0.2218(2) 0.0275(8) Uani 1 1 d . . . H45 H 0.1654 0.6214 0.2322 0.033 Uiso 1 1 calc R . . C46 C 0.2869(2) 0.6539(2) 0.2459(2) 0.0287(9) Uani 1 1 d . . . H46 H 0.3089 0.6069 0.2724 0.034 Uiso 1 1 calc R . . C47 C 0.3382(2) 0.7147(2) 0.23071(19) 0.0222(8) Uani 1 1 d . . . H47 H 0.3962 0.7089 0.2475 0.027 Uiso 1 1 calc R . . C48 C 0.30881(19) 0.78596(19) 0.19097(17) 0.0145(6) Uani 1 1 d . . . C49 C 0.37269(19) 0.8404(2) 0.17576(18) 0.0174(7) Uani 1 1 d . . . H49 H 0.4280 0.8249 0.1960 0.021 Uiso 1 1 calc R . . C50 C 0.4382(2) 0.9477(2) 0.12697(19) 0.0193(7) Uani 1 1 d . . . C51 C 0.5199(2) 0.9200(2) 0.1481(2) 0.0255(8) Uani 1 1 d . . . H51 H 0.5294 0.8699 0.1737 0.031 Uiso 1 1 calc R . . C52 C 0.5866(2) 0.9631(2) 0.1331(2) 0.0304(9) Uani 1 1 d . . . H52 H 0.6413 0.9432 0.1490 0.036 Uiso 1 1 calc R . . C53 C 0.5743(2) 1.0353(2) 0.0949(2) 0.0273(8) Uani 1 1 d . . . H53 H 0.6204 1.0646 0.0837 0.033 Uiso 1 1 calc R . . C54 C 0.4948(2) 1.0652(2) 0.0727(2) 0.0240(8) Uani 1 1 d . . . H54 H 0.4866 1.1152 0.0467 0.029 Uiso 1 1 calc R . . C55 C 0.4272(2) 1.0223(2) 0.08848(18) 0.0187(7) Uani 1 1 d . . . C56 C 0.3334(2) 1.1163(2) 0.0181(2) 0.0235(8) Uani 1 1 d . . . H56A H 0.3576 1.1652 0.0436 0.035 Uiso 1 1 calc R . . H56B H 0.2736 1.1241 0.0017 0.035 Uiso 1 1 calc R . . H56C H 0.3594 1.1056 -0.0254 0.035 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 Na1 0.0133(6) 0.0192(7) 0.0197(7) -0.0034(5) 0.0027(5) -0.0008(5) Na2 0.0192(7) 0.0194(7) 0.0211(7) 0.0009(6) 0.0057(5) 0.0026(5) Na3 0.0139(6) 0.0162(7) 0.0211(7) 0.0021(6) 0.0027(5) 0.0002(5) Na4 0.0169(7) 0.0180(7) 0.0195(7) -0.0021(5) 0.0065(5) 0.0006(5) O1 0.0108(11) 0.0213(13) 0.0242(13) -0.0010(10) 0.0037(9) -0.0018(9) O2 0.0145(12) 0.0253(13) 0.0238(13) -0.0083(10) 0.0013(10) 0.0022(10) O3 0.0189(12) 0.0149(12) 0.0188(12) -0.0025(9) 0.0035(9) 0.0036(9) O4 0.0203(13) 0.0204(13) 0.0250(13) -0.0021(10) 0.0069(10) -0.0028(10) O5 0.0180(12) 0.0183(12) 0.0196(12) 0.0019(10) 0.0061(10) 0.0012(9) O6 0.0241(14) 0.0265(14) 0.0245(13) 0.0031(11) 0.0051(11) 0.0131(11) O7 0.0137(11) 0.0146(12) 0.0197(12) 0.0009(9) 0.0047(9) -0.0003(9) O8 0.0140(12) 0.0235(13) 0.0278(13) 0.0129(11) 0.0029(10) 0.0001(10) N1 0.0142(14) 0.0178(15) 0.0166(14) 0.0003(11) 0.0019(11) -0.0017(11) N2 0.0108(13) 0.0218(15) 0.0170(13) -0.0033(12) 0.0025(11) 0.0027(11) N3 0.0171(15) 0.0195(15) 0.0209(15) -0.0012(12) 0.0021(12) -0.0012(11) N4 0.0135(13) 0.0180(15) 0.0173(14) 0.0008(11) 0.0038(11) -0.0022(11) C1 0.0135(16) 0.0167(17) 0.0177(16) 0.0070(13) 0.0011(13) 0.0015(13) C2 0.0227(19) 0.0203(19) 0.0244(18) 0.0031(15) 0.0064(15) 0.0038(14) C3 0.0202(19) 0.032(2) 0.031(2) 0.0092(17) 0.0091(16) 0.0093(15) C4 0.0099(17) 0.035(2) 0.044(2) 0.0048(19) -0.0019(16) 0.0001(15) C5 0.0155(18) 0.029(2) 0.030(2) 0.0049(17) -0.0007(15) -0.0027(15) C6 0.0204(18) 0.0175(17) 0.0191(17) 0.0060(14) 0.0038(14) 0.0012(14) C7 0.0196(18) 0.0192(18) 0.0158(17) 0.0030(13) -0.0009(13) -0.0051(13) C8 0.0205(17) 0.0149(17) 0.0133(15) 0.0040(12) 0.0070(13) -0.0042(13) C9 0.0209(18) 0.0232(19) 0.0197(18) 0.0016(14) 0.0013(14) -0.0064(14) C10 0.031(2) 0.023(2) 0.0258(19) -0.0063(15) 0.0057(16) -0.0131(15) C11 0.040(2) 0.0123(18) 0.038(2) -0.0073(16) 0.0143(18) -0.0051(15) C12 0.0191(18) 0.0164(18) 0.0279(19) 0.0005(14) 0.0061(15) -0.0009(13) C13 0.0211(18) 0.0143(17) 0.0171(16) -0.0005(13) 0.0062(13) -0.0057(13) C14 0.0165(18) 0.034(2) 0.0242(19) -0.0083(16) 0.0046(15) 0.0039(15) C15 0.0093(15) 0.0152(17) 0.0239(17) -0.0027(14) -0.0056(13) 0.0055(12) C16 0.0152(17) 0.0210(19) 0.031(2) -0.0009(15) 0.0035(14) 0.0015(14) C17 0.0191(18) 0.0181(19) 0.040(2) -0.0017(16) -0.0024(16) -0.0009(14) C18 0.028(2) 0.0146(18) 0.040(2) -0.0114(16) -0.0054(17) 0.0043(15) C19 0.0239(19) 0.026(2) 0.0218(18) -0.0095(15) -0.0013(15) 0.0080(15) C20 0.0138(17) 0.0218(18) 0.0199(17) -0.0074(14) -0.0005(14) 0.0072(13) C21 0.0155(17) 0.0249(19) 0.0179(17) -0.0048(14) 0.0020(14) 0.0075(14) C22 0.0106(16) 0.033(2) 0.0158(16) -0.0003(15) -0.0010(13) 0.0050(14) C23 0.0208(19) 0.038(2) 0.0216(19) -0.0094(16) 0.0049(15) -0.0001(16) C24 0.025(2) 0.059(3) 0.0207(19) -0.0064(19) 0.0115(16) 0.0019(19) C25 0.024(2) 0.050(3) 0.0250(19) 0.0068(18) 0.0100(16) -0.0029(18) C26 0.0200(18) 0.039(2) 0.0213(19) 0.0048(16) 0.0070(15) -0.0035(16) C27 0.0175(17) 0.032(2) 0.0133(16) 0.0026(14) 0.0033(13) 0.0054(14) C28 0.027(2) 0.0186(19) 0.029(2) -0.0041(15) 0.0086(16) -0.0039(14) C29 0.0093(15) 0.0242(19) 0.0154(16) 0.0006(14) -0.0018(12) -0.0032(13) C30 0.0217(18) 0.0233(19) 0.0203(17) 0.0041(14) 0.0047(14) -0.0010(14) C31 0.0178(18) 0.028(2) 0.0258(19) -0.0032(16) 0.0033(15) 0.0017(15) C32 0.0179(18) 0.036(2) 0.0202(18) -0.0030(16) 0.0067(14) -0.0017(15) C33 0.0202(18) 0.031(2) 0.0193(18) 0.0065(15) 0.0005(14) -0.0015(15) C34 0.0129(16) 0.0225(19) 0.0163(16) 0.0001(14) -0.0019(13) -0.0020(13) C35 0.0219(18) 0.025(2) 0.0204(18) 0.0073(15) 0.0010(14) -0.0029(15) C36 0.0114(16) 0.0179(18) 0.0248(18) -0.0022(14) -0.0055(13) -0.0012(13) C37 0.032(2) 0.020(2) 0.030(2) 0.0029(16) 0.0040(17) -0.0013(15) C38 0.039(2) 0.017(2) 0.040(2) 0.0052(17) -0.0011(19) -0.0019(16) C39 0.026(2) 0.016(2) 0.044(2) -0.0004(17) -0.0097(18) 0.0048(14) C40 0.0168(18) 0.030(2) 0.035(2) -0.0023(17) -0.0001(16) 0.0066(15) C41 0.0180(18) 0.0189(18) 0.0246(18) 0.0009(15) -0.0039(14) 0.0005(14) C42 0.0197(19) 0.041(2) 0.030(2) 0.0002(18) 0.0076(16) 0.0107(16) C43 0.0198(17) 0.0137(17) 0.0136(16) -0.0030(13) 0.0026(13) 0.0010(13) C44 0.0167(18) 0.0244(19) 0.0224(18) -0.0010(15) 0.0039(14) -0.0027(13) C45 0.031(2) 0.020(2) 0.032(2) 0.0074(16) 0.0079(17) -0.0087(15) C46 0.033(2) 0.021(2) 0.031(2) 0.0090(16) 0.0001(17) 0.0028(16) C47 0.0204(18) 0.0198(19) 0.0231(18) 0.0018(14) -0.0051(14) 0.0016(14) C48 0.0161(16) 0.0147(16) 0.0125(15) -0.0024(13) 0.0014(13) -0.0017(12) C49 0.0097(15) 0.0216(18) 0.0199(17) -0.0037(14) -0.0003(13) 0.0054(13) C50 0.0167(17) 0.0200(18) 0.0228(18) -0.0001(14) 0.0079(14) -0.0011(13) C51 0.0155(18) 0.023(2) 0.039(2) 0.0067(16) 0.0074(16) -0.0004(14) C52 0.0148(18) 0.036(2) 0.041(2) 0.0053(18) 0.0073(16) 0.0025(15) C53 0.0156(18) 0.035(2) 0.033(2) 0.0051(17) 0.0079(15) -0.0077(15) C54 0.0208(18) 0.025(2) 0.0252(19) 0.0081(16) 0.0027(15) -0.0012(15) C55 0.0147(17) 0.0260(19) 0.0150(16) -0.0009(14) 0.0016(13) 0.0008(14) C56 0.0205(18) 0.024(2) 0.0248(19) 0.0062(15) -0.0008(15) -0.0025(14) _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 O1 2.230(3) . ? Na1 O2 2.304(3) . ? Na1 O5 2.315(3) . ? Na1 O7 2.375(2) . ? Na1 N1 2.426(3) . ? Na1 Na4 3.1515(18) . ? Na1 Na3 3.2198(17) . ? Na1 Na2 3.2483(18) . ? Na2 O5 2.249(3) . ? Na2 O6 2.308(3) . ? Na2 O1 2.357(3) . ? Na2 O3 2.368(3) . ? Na2 N3 2.412(3) . ? Na2 Na3 3.2358(17) . ? Na2 Na4 3.2908(18) . ? Na3 O7 2.256(2) . ? Na3 O8 2.302(3) . ? Na3 O5 2.332(3) . ? Na3 O3 2.334(3) . ? Na3 N4 2.406(3) . ? Na3 Na4 3.1899(18) . ? Na4 O3 2.220(3) . ? Na4 O4 2.299(3) . ? Na4 O7 2.338(3) . ? Na4 O1 2.345(3) . ? Na4 N2 2.358(3) . ? O1 C1 1.293(4) . ? O2 C13 1.390(4) . ? O2 C14 1.434(4) . ? O3 C15 1.304(4) . ? O4 C27 1.386(4) . ? O4 C28 1.429(4) . ? O5 C29 1.301(4) . ? O6 C41 1.374(4) . ? O6 C42 1.427(4) . ? O7 C43 1.304(4) . ? O8 C55 1.370(4) . ? O8 C56 1.431(4) . ? N1 C7 1.290(4) . ? N1 C8 1.422(4) . ? N2 C21 1.283(4) . ? N2 C22 1.421(4) . ? N3 C35 1.285(5) . ? N3 C36 1.434(4) . ? N4 C49 1.288(4) . ? N4 C50 1.424(4) . ? C1 C2 1.422(5) . ? C1 C6 1.436(5) . ? C2 C3 1.370(5) . ? C3 C4 1.398(5) . ? C4 C5 1.367(5) . ? C5 C6 1.411(5) . ? C6 C7 1.450(5) . ? C8 C9 1.398(5) . ? C8 C13 1.402(5) . ? C9 C10 1.391(5) . ? C10 C11 1.374(5) . ? C11 C12 1.391(5) . ? C12 C13 1.378(5) . ? C15 C16 1.424(5) . ? C15 C20 1.433(5) . ? C16 C17 1.375(5) . ? C17 C18 1.387(6) . ? C18 C19 1.380(6) . ? C19 C20 1.411(5) . ? C20 C21 1.457(5) . ? C22 C23 1.402(5) . ? C22 C27 1.406(5) . ? C23 C24 1.380(5) . ? C24 C25 1.380(6) . ? C25 C26 1.381(5) . ? C26 C27 1.391(5) . ? C29 C30 1.415(5) . ? C29 C34 1.433(5) . ? C30 C31 1.383(5) . ? C31 C32 1.388(5) . ? C32 C33 1.381(5) . ? C33 C34 1.414(5) . ? C34 C35 1.449(5) . ? C36 C37 1.388(5) . ? C36 C41 1.415(5) . ? C37 C38 1.389(5) . ? C38 C39 1.376(6) . ? C39 C40 1.386(6) . ? C40 C41 1.388(5) . ? C43 C44 1.416(5) . ? C43 C48 1.440(4) . ? C44 C45 1.373(5) . ? C45 C46 1.390(5) . ? C46 C47 1.370(5) . ? C47 C48 1.421(4) . ? C48 C49 1.444(5) . ? C50 C51 1.402(5) . ? C50 C55 1.414(5) . ? C51 C52 1.373(5) . ? C52 C53 1.377(5) . ? C53 C54 1.384(5) . ? C54 C55 1.388(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 O1 Na1 O2 141.42(10) . . ? O1 Na1 O5 90.26(9) . . ? O2 Na1 O5 127.22(10) . . ? O1 Na1 O7 95.53(9) . . ? O2 Na1 O7 93.00(9) . . ? O5 Na1 O7 90.74(8) . . ? O1 Na1 N1 78.91(9) . . ? O2 Na1 N1 68.37(9) . . ? O5 Na1 N1 134.35(10) . . ? O7 Na1 N1 134.06(10) . . ? O1 Na1 Na4 48.00(7) . . ? O2 Na1 Na4 127.77(8) . . ? O5 Na1 Na4 91.31(7) . . ? O7 Na1 Na4 47.53(6) . . ? N1 Na1 Na4 111.70(8) . . ? O1 Na1 Na3 92.11(7) . . ? O2 Na1 Na3 119.33(7) . . ? O5 Na1 Na3 46.36(6) . . ? O7 Na1 Na3 44.46(6) . . ? N1 Na1 Na3 170.86(9) . . ? Na4 Na1 Na3 60.08(4) . . ? O1 Na1 Na2 46.52(6) . . ? O2 Na1 Na2 169.62(8) . . ? O5 Na1 Na2 43.81(6) . . ? O7 Na1 Na2 92.41(7) . . ? N1 Na1 Na2 113.41(8) . . ? Na4 Na1 Na2 61.87(4) . . ? Na3 Na1 Na2 60.03(4) . . ? O5 Na2 O6 143.67(10) . . ? O5 Na2 O1 88.75(9) . . ? O6 Na2 O1 127.56(10) . . ? O5 Na2 O3 92.13(9) . . ? O6 Na2 O3 88.96(9) . . ? O1 Na2 O3 87.78(9) . . ? O5 Na2 N3 78.95(10) . . ? O6 Na2 N3 69.05(10) . . ? O1 Na2 N3 150.34(11) . . ? O3 Na2 N3 119.26(10) . . ? O5 Na2 Na3 46.11(6) . . ? O6 Na2 Na3 123.18(8) . . ? O1 Na2 Na3 89.41(7) . . ? O3 Na2 Na3 46.08(6) . . ? N3 Na2 Na3 100.70(8) . . ? O5 Na2 Na1 45.46(6) . . ? O6 Na2 Na1 170.54(9) . . ? O1 Na2 Na1 43.36(6) . . ? O3 Na2 Na1 87.98(7) . . ? N3 Na2 Na1 120.15(9) . . ? Na3 Na2 Na1 59.54(4) . . ? O5 Na2 Na4 88.99(7) . . ? O6 Na2 Na4 114.92(8) . . ? O1 Na2 Na4 45.44(6) . . ? O3 Na2 Na4 42.40(6) . . ? N3 Na2 Na4 158.17(8) . . ? Na3 Na2 Na4 58.51(4) . . ? Na1 Na2 Na4 57.62(4) . . ? O7 Na3 O8 147.69(10) . . ? O7 Na3 O5 93.35(9) . . ? O8 Na3 O5 95.45(9) . . ? O7 Na3 O3 91.02(9) . . ? O8 Na3 O3 119.79(9) . . ? O5 Na3 O3 90.92(9) . . ? O7 Na3 N4 80.07(9) . . ? O8 Na3 N4 68.91(9) . . ? O5 Na3 N4 121.99(10) . . ? O3 Na3 N4 146.12(10) . . ? O7 Na3 Na4 47.09(6) . . ? O8 Na3 Na4 163.22(8) . . ? O5 Na3 Na4 90.05(7) . . ? O3 Na3 Na4 44.08(6) . . ? N4 Na3 Na4 120.97(8) . . ? O7 Na3 Na1 47.49(6) . . ? O8 Na3 Na1 134.19(8) . . ? O5 Na3 Na1 45.93(6) . . ? O3 Na3 Na1 89.24(7) . . ? N4 Na3 Na1 107.36(8) . . ? Na4 Na3 Na1 58.90(4) . . ? O7 Na3 Na2 95.02(7) . . ? O8 Na3 Na2 112.72(7) . . ? O5 Na3 Na2 44.03(6) . . ? O3 Na3 Na2 46.95(6) . . ? N4 Na3 Na2 165.30(8) . . ? Na4 Na3 Na2 61.61(4) . . ? Na1 Na3 Na2 60.42(4) . . ? O3 Na4 O4 150.58(10) . . ? O3 Na4 O7 91.85(9) . . ? O4 Na4 O7 116.84(9) . . ? O3 Na4 O1 91.67(9) . . ? O4 Na4 O1 92.88(9) . . ? O7 Na4 O1 93.50(9) . . ? O3 Na4 N2 82.44(10) . . ? O4 Na4 N2 70.16(10) . . ? O7 Na4 N2 146.02(10) . . ? O1 Na4 N2 120.02(10) . . ? O3 Na4 Na1 93.10(8) . . ? O4 Na4 Na1 110.43(8) . . ? O7 Na4 Na1 48.54(6) . . ? O1 Na4 Na1 44.97(6) . . ? N2 Na4 Na1 164.47(8) . . ? O3 Na4 Na3 47.02(7) . . ? O4 Na4 Na3 161.70(8) . . ? O7 Na4 Na3 44.98(6) . . ? O1 Na4 Na3 90.74(7) . . ? N2 Na4 Na3 122.77(8) . . ? Na1 Na4 Na3 61.02(4) . . ? O3 Na4 Na2 45.99(7) . . ? O4 Na4 Na2 132.44(8) . . ? O7 Na4 Na2 92.03(7) . . ? O1 Na4 Na2 45.73(6) . . ? N2 Na4 Na2 107.01(8) . . ? Na1 Na4 Na2 60.51(4) . . ? Na3 Na4 Na2 59.88(4) . . ? C1 O1 Na1 136.5(2) . . ? C1 O1 Na4 118.1(2) . . ? Na1 O1 Na4 87.03(9) . . ? C1 O1 Na2 122.8(2) . . ? Na1 O1 Na2 90.12(9) . . ? Na4 O1 Na2 88.83(9) . . ? C13 O2 C14 117.8(3) . . ? C13 O2 Na1 120.06(19) . . ? C14 O2 Na1 119.6(2) . . ? C15 O3 Na4 131.5(2) . . ? C15 O3 Na3 123.2(2) . . ? Na4 O3 Na3 88.90(9) . . ? C15 O3 Na2 122.2(2) . . ? Na4 O3 Na2 91.61(9) . . ? Na3 O3 Na2 86.97(9) . . ? C27 O4 C28 116.7(3) . . ? C27 O4 Na4 120.0(2) . . ? C28 O4 Na4 122.0(2) . . ? C29 O5 Na2 134.0(2) . . ? C29 O5 Na1 120.3(2) . . ? Na2 O5 Na1 90.73(9) . . ? C29 O5 Na3 121.73(19) . . ? Na2 O5 Na3 89.86(9) . . ? Na1 O5 Na3 87.71(9) . . ? C41 O6 C42 117.1(3) . . ? C41 O6 Na2 121.6(2) . . ? C42 O6 Na2 121.3(2) . . ? C43 O7 Na3 133.9(2) . . ? C43 O7 Na4 124.3(2) . . ? Na3 O7 Na4 87.93(9) . . ? C43 O7 Na1 123.71(19) . . ? Na3 O7 Na1 88.05(9) . . ? Na4 O7 Na1 83.93(8) . . ? C55 O8 C56 117.2(3) . . ? C55 O8 Na3 121.9(2) . . ? C56 O8 Na3 120.00(19) . . ? C7 N1 C8 120.2(3) . . ? C7 N1 Na1 125.8(2) . . ? C8 N1 Na1 113.9(2) . . ? C21 N2 C22 119.6(3) . . ? C21 N2 Na4 122.9(2) . . ? C22 N2 Na4 115.7(2) . . ? C35 N3 C36 118.7(3) . . ? C35 N3 Na2 126.1(2) . . ? C36 N3 Na2 115.0(2) . . ? C49 N4 C50 118.4(3) . . ? C49 N4 Na3 125.4(2) . . ? C50 N4 Na3 116.0(2) . . ? O1 C1 C2 120.7(3) . . ? O1 C1 C6 123.7(3) . . ? C2 C1 C6 115.6(3) . . ? C3 C2 C1 123.1(3) . . ? C2 C3 C4 120.7(4) . . ? C5 C4 C3 118.2(3) . . ? C4 C5 C6 122.9(3) . . ? C5 C6 C1 119.4(3) . . ? C5 C6 C7 115.8(3) . . ? C1 C6 C7 124.6(3) . . ? N1 C7 C6 129.3(3) . . ? C9 C8 C13 117.2(3) . . ? C9 C8 N1 125.5(3) . . ? C13 C8 N1 117.3(3) . . ? C10 C9 C8 121.3(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 120.4(3) . . ? C13 C12 C11 119.3(3) . . ? C12 C13 O2 122.2(3) . . ? C12 C13 C8 122.0(3) . . ? O2 C13 C8 115.8(3) . . ? O3 C15 C16 119.6(3) . . ? O3 C15 C20 124.3(3) . . ? C16 C15 C20 116.1(3) . . ? C17 C16 C15 122.9(4) . . ? C16 C17 C18 120.4(4) . . ? C19 C18 C17 119.1(3) . . ? C18 C19 C20 122.1(4) . . ? C19 C20 C15 119.5(3) . . ? C19 C20 C21 114.2(3) . . ? C15 C20 C21 126.3(3) . . ? N2 C21 C20 128.7(3) . . ? C23 C22 C27 116.9(3) . . ? C23 C22 N2 125.6(3) . . ? C27 C22 N2 117.5(3) . . ? C24 C23 C22 121.7(4) . . ? C23 C24 C25 120.0(4) . . ? C24 C25 C26 120.3(4) . . ? C25 C26 C27 119.7(4) . . ? O4 C27 C26 122.4(3) . . ? O4 C27 C22 116.2(3) . . ? C26 C27 C22 121.4(3) . . ? O5 C29 C30 120.2(3) . . ? O5 C29 C34 123.6(3) . . ? C30 C29 C34 116.2(3) . . ? C31 C30 C29 123.1(3) . . ? C30 C31 C32 120.5(3) . . ? C33 C32 C31 118.3(3) . . ? C32 C33 C34 122.9(3) . . ? C33 C34 C29 119.0(3) . . ? C33 C34 C35 115.3(3) . . ? C29 C34 C35 125.7(3) . . ? N3 C35 C34 128.5(3) . . ? C37 C36 C41 117.6(3) . . ? C37 C36 N3 125.3(3) . . ? C41 C36 N3 117.1(3) . . ? C38 C37 C36 121.6(4) . . ? C39 C38 C37 120.1(4) . . ? C38 C39 C40 119.5(4) . . ? C39 C40 C41 120.8(4) . . ? O6 C41 C40 123.7(3) . . ? O6 C41 C36 116.2(3) . . ? C40 C41 C36 120.1(3) . . ? O7 C43 C44 120.1(3) . . ? O7 C43 C48 123.5(3) . . ? C44 C43 C48 116.4(3) . . ? C45 C44 C43 123.0(3) . . ? C44 C45 C46 120.7(3) . . ? C47 C46 C45 118.4(3) . . ? C46 C47 C48 123.1(3) . . ? C47 C48 C43 118.3(3) . . ? C47 C48 C49 115.0(3) . . ? C43 C48 C49 126.6(3) . . ? N4 C49 C48 128.8(3) . . ? C51 C50 C55 116.8(3) . . ? C51 C50 N4 126.5(3) . . ? C55 C50 N4 116.7(3) . . ? C52 C51 C50 122.1(3) . . ? C51 C52 C53 120.0(3) . . ? C52 C53 C54 120.2(3) . . ? C53 C54 C55 120.1(3) . . ? O8 C55 C54 122.7(3) . . ? O8 C55 C50 116.5(3) . . ? C54 C55 C50 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.320 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.060 data_b757 _database_code_depnum_ccdc_archive 'CCDC 918630' #TrackingRef 'web_deposit_cif_file_6_XiaoluSong_1360938597.B757.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H32.75 Cl4 N3.25 Ni3 O2.50 S2' _chemical_formula_weight 890.92 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2929(14) _cell_length_b 13.6662(16) _cell_length_c 22.289(3) _cell_angle_alpha 96.290(2) _cell_angle_beta 95.839(2) _cell_angle_gamma 98.850(2) _cell_volume 3650.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 995 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.26 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1818 _exptl_absorpt_coefficient_mu 1.975 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7429 _exptl_absorpt_correction_T_max 0.8580 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48584 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16709 _reflns_number_gt 14419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. S and C atoms of one of the terminal S Methyl group were disordered into two positions with occupancy ratio= 42: 58. Restraints were applied to atoms C13 and C14 and the CH3CN solvent. For C13 and C14, the ISOR was used to contain the thermal parameters. For CH3CN, restraints were used because the CH3CN is disordered at a point of symmetry. Restraints used: DFIX 2.6 0.001 C66 N7 DFIX 1.1 0.001 C65 N7 DFIX 1.5 0.001 C66 C65 EADP C65 C66 ISOR 0.005 0.008 N7 C65 C66 C13 C14 ; _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^)+(0.0457P)^2^+2.7870P] 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 16709 _refine_ls_number_parameters 886 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.003 _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 Ni1 Ni 0.56787(2) 0.16634(2) 0.371667(13) 0.01314(7) Uani 1 1 d . . . Ni2 Ni 0.38377(2) 0.27310(2) 0.363458(13) 0.01326(7) Uani 1 1 d . . . Ni3 Ni 0.59401(2) 0.35789(2) 0.320381(13) 0.01397(7) Uani 1 1 d . . . Ni4 Ni 0.85704(3) 0.87525(2) 0.120499(15) 0.01783(7) Uani 1 1 d . A . Ni5 Ni 0.90558(3) 0.68192(2) 0.140549(14) 0.01739(7) Uani 1 1 d . . . Ni6 Ni 0.74202(3) 0.69793(3) 0.035187(16) 0.02407(8) Uani 1 1 d . A . Cl1 Cl 0.39022(5) 0.11837(4) 0.40577(3) 0.01716(12) Uani 1 1 d . . . Cl2 Cl 0.72710(5) 0.24599(4) 0.32882(3) 0.01764(12) Uani 1 1 d . . . Cl3 Cl 0.41998(5) 0.41930(4) 0.31102(3) 0.01677(12) Uani 1 1 d . . . Cl4 Cl 0.70184(5) 0.50665(4) 0.36621(3) 0.01858(12) Uani 1 1 d . . . Cl5 Cl 0.98772(5) 0.83805(5) 0.20063(3) 0.02114(13) Uani 1 1 d . A . Cl6 Cl 0.72007(6) 0.87083(5) 0.03331(3) 0.02976(15) Uani 1 1 d . . . Cl7 Cl 0.80180(6) 0.54733(5) 0.06830(3) 0.02787(15) Uani 1 1 d . A . Cl8 Cl 0.74568(6) 0.66052(6) -0.06722(3) 0.03321(16) Uani 1 1 d . . . S1 S 0.68065(5) 0.12800(4) 0.45421(3) 0.01595(12) Uani 1 1 d . . . S2 S 0.20151(5) 0.23297(5) 0.31567(3) 0.02007(13) Uani 1 1 d . . . S3 S 0.78047(5) 0.99450(5) 0.17805(3) 0.02279(14) Uani 1 1 d . . . S4 S 1.0882(2) 0.6335(2) 0.15253(15) 0.0145(5) Uani 0.421(7) 1 d P A 1 S4A S 1.0599(3) 0.6065(3) 0.13660(14) 0.0309(6) Uani 0.579(7) 1 d P A 2 O1 O 0.48122(13) 0.21160(12) 0.30158(7) 0.0146(3) Uani 1 1 d . . . O2 O 0.54353(13) 0.31229(12) 0.40062(7) 0.0127(3) Uani 1 1 d . . . O3 O 0.90931(16) 0.76691(13) 0.06752(8) 0.0209(4) Uani 1 1 d . A . O4 O 0.76362(14) 0.73966(12) 0.13464(8) 0.0173(3) Uani 1 1 d . A . O5 O 0.1506(2) 0.8664(3) 0.37152(14) 0.0722(10) Uani 1 1 d . . . N1 N 0.56868(17) 0.02946(15) 0.33159(9) 0.0174(4) Uani 1 1 d . . . N2 N 0.32322(16) 0.33329(14) 0.43593(9) 0.0143(4) Uani 1 1 d . . . N3 N 0.96876(18) 0.98690(15) 0.10237(10) 0.0188(4) Uani 1 1 d . . . N4 N 0.87483(17) 0.61372(15) 0.21276(9) 0.0168(4) Uani 1 1 d . A . N5 N 0.61043(19) 0.36915(16) 0.23163(10) 0.0212(5) Uani 1 1 d . . . N6 N 0.5777(2) 0.64167(18) 0.03289(11) 0.0298(5) Uani 1 1 d . . . C1 C 0.6070(2) 0.12129(19) 0.52056(11) 0.0215(5) Uani 1 1 d . . . H1A H 0.5283 0.0956 0.5076 0.032 Uiso 1 1 calc R . . H1B H 0.6151 0.1881 0.5433 0.032 Uiso 1 1 calc R . . H1C H 0.6379 0.0765 0.5466 0.032 Uiso 1 1 calc R . . C2 C 0.6691(2) -0.00083(18) 0.42549(11) 0.0164(5) Uani 1 1 d . . . C3 C 0.7178(2) -0.06294(19) 0.46207(12) 0.0208(5) Uani 1 1 d . . . H3 H 0.7546 -0.0365 0.5014 0.025 Uiso 1 1 calc R . . C4 C 0.7124(2) -0.1624(2) 0.44122(13) 0.0249(6) Uani 1 1 d . . . H4 H 0.7451 -0.2047 0.4662 0.030 Uiso 1 1 calc R . . C5 C 0.6590(2) -0.2009(2) 0.38343(13) 0.0253(6) Uani 1 1 d . . . H5 H 0.6556 -0.2695 0.3689 0.030 Uiso 1 1 calc R . . C6 C 0.6110(2) -0.13940(19) 0.34716(12) 0.0234(5) Uani 1 1 d . . . H6 H 0.5738 -0.1665 0.3080 0.028 Uiso 1 1 calc R . . C7 C 0.6161(2) -0.03817(18) 0.36712(11) 0.0169(5) Uani 1 1 d . . . C8 C 0.5282(3) 0.0021(2) 0.27594(13) 0.0303(7) Uani 1 1 d . . . H8 H 0.5380 -0.0625 0.2592 0.036 Uiso 1 1 calc R . . C9 C 0.4690(3) 0.0578(2) 0.23508(13) 0.0332(7) Uani 1 1 d . . . C10 C 0.4460(2) 0.15560(19) 0.24782(11) 0.0189(5) Uani 1 1 d . . . C11 C 0.3841(2) 0.19534(19) 0.20292(12) 0.0210(5) Uani 1 1 d . . . H11 H 0.3678 0.2608 0.2114 0.025 Uiso 1 1 calc R . . C12 C 0.3466(3) 0.1417(2) 0.14694(14) 0.0375(8) Uani 1 1 d . . . H12 H 0.3061 0.1707 0.1170 0.045 Uiso 1 1 calc R . . C13 C 0.3674(4) 0.0453(3) 0.13398(17) 0.0631(12) Uani 1 1 d U . . H13 H 0.3401 0.0074 0.0956 0.076 Uiso 1 1 calc R . . C14 C 0.4283(4) 0.0052(3) 0.17740(17) 0.0600(12) Uani 1 1 d U . . H14 H 0.4434 -0.0605 0.1680 0.072 Uiso 1 1 calc R . . C15 C 0.1544(3) 0.0994(2) 0.30293(16) 0.0351(7) Uani 1 1 d . . . H15A H 0.1781 0.0698 0.3391 0.053 Uiso 1 1 calc R . . H15B H 0.1862 0.0703 0.2680 0.053 Uiso 1 1 calc R . . H15C H 0.0733 0.0857 0.2948 0.053 Uiso 1 1 calc R . . C16 C 0.1399(2) 0.27212(19) 0.38131(12) 0.0190(5) Uani 1 1 d . . . C17 C 0.0246(2) 0.2550(2) 0.37859(13) 0.0267(6) Uani 1 1 d . . . H17 H -0.0194 0.2194 0.3431 0.032 Uiso 1 1 calc R . . C18 C -0.0257(2) 0.2899(2) 0.42754(14) 0.0315(7) Uani 1 1 d . . . H18 H -0.1040 0.2752 0.4266 0.038 Uiso 1 1 calc R . . C19 C 0.0381(2) 0.3462(2) 0.47757(13) 0.0287(6) Uani 1 1 d . . . H19 H 0.0030 0.3724 0.5104 0.034 Uiso 1 1 calc R . . C20 C 0.1521(2) 0.3651(2) 0.48076(12) 0.0214(5) Uani 1 1 d . . . H20 H 0.1948 0.4053 0.5152 0.026 Uiso 1 1 calc R . . C21 C 0.2053(2) 0.32507(18) 0.43333(11) 0.0164(5) Uani 1 1 d . . . C22 C 0.3841(2) 0.36578(17) 0.48695(11) 0.0151(5) Uani 1 1 d . . . H22 H 0.3464 0.3884 0.5196 0.018 Uiso 1 1 calc R . . C23 C 0.50329(19) 0.37189(17) 0.50050(11) 0.0142(4) Uani 1 1 d . . . C24 C 0.57840(19) 0.35004(17) 0.45939(10) 0.0137(4) Uani 1 1 d . . . C25 C 0.6916(2) 0.36477(17) 0.47962(11) 0.0159(5) Uani 1 1 d . . . H25 H 0.7430 0.3551 0.4513 0.019 Uiso 1 1 calc R . . C26 C 0.7297(2) 0.39343(18) 0.54077(11) 0.0183(5) Uani 1 1 d . . . H26 H 0.8068 0.4014 0.5542 0.022 Uiso 1 1 calc R . . C27 C 0.6560(2) 0.41050(18) 0.58250(11) 0.0186(5) Uani 1 1 d . . . H27 H 0.6818 0.4276 0.6246 0.022 Uiso 1 1 calc R . . C28 C 0.5451(2) 0.40235(18) 0.56221(11) 0.0177(5) Uani 1 1 d . . . H28 H 0.4953 0.4176 0.5904 0.021 Uiso 1 1 calc R . . C29 C 0.8123(3) 0.9850(2) 0.25791(13) 0.0323(7) Uani 1 1 d . A . H29A H 0.8901 0.9774 0.2664 0.048 Uiso 1 1 calc R . . H29B H 0.7645 0.9268 0.2686 0.048 Uiso 1 1 calc R . . H29C H 0.7995 1.0456 0.2821 0.048 Uiso 1 1 calc R . . C30 C 0.8832(2) 1.09687(19) 0.16896(12) 0.0208(5) Uani 1 1 d . A . C31 C 0.8769(2) 1.1907(2) 0.19878(13) 0.0258(6) Uani 1 1 d . . . H31 H 0.8182 1.1983 0.2226 0.031 Uiso 1 1 calc R A . C32 C 0.9554(3) 1.2725(2) 0.19398(13) 0.0288(6) Uani 1 1 d . A . H32 H 0.9517 1.3361 0.2149 0.035 Uiso 1 1 calc R . . C33 C 1.0397(2) 1.2608(2) 0.15821(13) 0.0272(6) Uani 1 1 d . . . H33 H 1.0941 1.3168 0.1549 0.033 Uiso 1 1 calc R A . C34 C 1.0454(2) 1.1689(2) 0.12736(12) 0.0235(5) Uani 1 1 d . A . H34 H 1.1031 1.1625 0.1026 0.028 Uiso 1 1 calc R . . C35 C 0.9671(2) 1.08471(18) 0.13215(12) 0.0198(5) Uani 1 1 d . A . C36 C 1.0441(2) 0.97132(19) 0.06806(12) 0.0218(5) Uani 1 1 d . A . H36 H 1.0947 1.0287 0.0626 0.026 Uiso 1 1 calc R . . C37 C 1.0615(2) 0.8769(2) 0.03658(12) 0.0228(5) Uani 1 1 d . . . C38 C 0.9974(2) 0.78153(19) 0.03612(12) 0.0221(5) Uani 1 1 d . A . C39 C 1.0266(2) 0.6990(2) 0.00279(12) 0.0263(6) Uani 1 1 d . . . H39 H 0.9829 0.6350 0.0018 0.032 Uiso 1 1 calc R A . C40 C 1.1177(3) 0.7085(2) -0.02871(13) 0.0310(6) Uani 1 1 d . A . H40 H 1.1364 0.6513 -0.0509 0.037 Uiso 1 1 calc R . . C41 C 1.1824(3) 0.8015(2) -0.02809(14) 0.0316(6) Uani 1 1 d . . . H41 H 1.2456 0.8079 -0.0495 0.038 Uiso 1 1 calc R A . C42 C 1.1543(2) 0.8839(2) 0.00354(13) 0.0283(6) Uani 1 1 d . A . H42 H 1.1983 0.9474 0.0033 0.034 Uiso 1 1 calc R . . C43 C 1.1788(6) 0.6942(6) 0.1491(3) 0.0319(18) Uani 0.421(7) 1 d P A 1 H43A H 1.2424 0.6596 0.1554 0.048 Uiso 0.421(7) 1 calc PR A 1 H43B H 1.1865 0.7518 0.1804 0.048 Uiso 0.421(7) 1 calc PR A 1 H43C H 1.1759 0.7169 0.1088 0.048 Uiso 0.421(7) 1 calc PR A 1 C43A C 1.0856(5) 0.5214(4) 0.0970(2) 0.0305(13) Uani 0.579(7) 1 d P A 2 H43D H 1.1615 0.5113 0.1093 0.046 Uiso 0.579(7) 1 calc PR A 2 H43E H 1.0788 0.5353 0.0547 0.046 Uiso 0.579(7) 1 calc PR A 2 H43F H 1.0335 0.4610 0.1006 0.046 Uiso 0.579(7) 1 calc PR A 2 C44 C 1.0576(2) 0.5669(2) 0.21292(13) 0.0261(6) Uani 1 1 d . . . C45 C 1.1434(2) 0.5231(2) 0.23821(15) 0.0311(7) Uani 1 1 d . A . H45 H 1.2078 0.5207 0.2182 0.037 Uiso 1 1 calc R . . C46 C 1.1360(2) 0.4833(2) 0.29175(14) 0.0282(6) Uani 1 1 d . . . H46 H 1.1940 0.4521 0.3084 0.034 Uiso 1 1 calc R A . C47 C 1.0425(2) 0.4889(2) 0.32146(13) 0.0261(6) Uani 1 1 d . A . H47 H 1.0379 0.4632 0.3592 0.031 Uiso 1 1 calc R . . C48 C 0.9563(2) 0.5315(2) 0.29663(12) 0.0220(5) Uani 1 1 d . . . H48 H 0.8930 0.5347 0.3174 0.026 Uiso 1 1 calc R A . C49 C 0.9614(2) 0.56979(18) 0.24113(12) 0.0194(5) Uani 1 1 d . A . C50 C 0.7796(2) 0.60427(18) 0.23236(11) 0.0181(5) Uani 1 1 d . . . H50 H 0.7696 0.5628 0.2636 0.022 Uiso 1 1 calc R A . C51 C 0.6848(2) 0.65037(18) 0.21189(11) 0.0169(5) Uani 1 1 d . A . C52 C 0.6810(2) 0.71849(17) 0.16876(11) 0.0168(5) Uani 1 1 d . . . C53 C 0.5868(2) 0.76340(18) 0.15972(11) 0.0194(5) Uani 1 1 d . A . H53 H 0.5857 0.8128 0.1329 0.023 Uiso 1 1 calc R . . C54 C 0.4951(2) 0.73670(19) 0.18929(12) 0.0221(5) Uani 1 1 d . . . H54 H 0.4315 0.7673 0.1821 0.026 Uiso 1 1 calc R A . C55 C 0.4952(2) 0.6657(2) 0.22929(12) 0.0228(5) Uani 1 1 d . A . H55 H 0.4310 0.6454 0.2482 0.027 Uiso 1 1 calc R . . C56 C 0.5897(2) 0.62495(19) 0.24112(12) 0.0207(5) Uani 1 1 d . . . H56 H 0.5909 0.5784 0.2698 0.025 Uiso 1 1 calc R A . C57 C 0.5945(2) 0.3680(2) 0.18053(13) 0.0294(6) Uani 1 1 d . . . C58 C 0.5713(3) 0.3676(3) 0.11475(15) 0.0506(10) Uani 1 1 d . . . H58A H 0.4917 0.3658 0.1038 0.076 Uiso 1 1 calc R . . H58B H 0.5940 0.3087 0.0936 0.076 Uiso 1 1 calc R . . H58C H 0.6127 0.4281 0.1028 0.076 Uiso 1 1 calc R . . C59 C 0.4875(3) 0.6191(2) 0.04042(13) 0.0299(6) Uani 1 1 d . A . C60 C 0.3737(3) 0.5930(3) 0.05290(16) 0.0425(8) Uani 1 1 d . . . H60A H 0.3703 0.6063 0.0967 0.064 Uiso 1 1 calc R A . H60B H 0.3470 0.5220 0.0391 0.064 Uiso 1 1 calc R . . H60C H 0.3269 0.6331 0.0313 0.064 Uiso 1 1 calc R . . C61 C 0.1910(4) 0.7963(3) 0.33220(19) 0.0562(11) Uani 1 1 d . B . H61A H 0.1315 0.7654 0.2993 0.067 Uiso 1 1 calc R . . H61B H 0.2126 0.7427 0.3551 0.067 Uiso 1 1 calc R . . C62 C 0.2854(4) 0.8424(4) 0.3060(2) 0.0674(12) Uani 1 1 d . . . H62A H 0.2607 0.8840 0.2759 0.101 Uiso 1 1 calc R B . H62B H 0.3213 0.7906 0.2862 0.101 Uiso 1 1 calc R . . H62C H 0.3382 0.8841 0.3381 0.101 Uiso 1 1 calc R . . C63 C 0.0545(5) 0.8263(6) 0.3937(3) 0.113(3) Uani 1 1 d . B 2 H63A H 0.0689 0.7732 0.4188 0.135 Uiso 1 1 calc R B 2 H63B H -0.0039 0.7973 0.3598 0.135 Uiso 1 1 calc R B 2 C64 C 0.0182(5) 0.9113(7) 0.4320(4) 0.170(5) Uani 1 1 d . B 2 H64A H 0.0678 0.9289 0.4702 0.255 Uiso 1 1 calc R B 2 H64B H -0.0579 0.8906 0.4408 0.255 Uiso 1 1 calc R B 2 H64C H 0.0211 0.9695 0.4097 0.255 Uiso 1 1 calc R B 2 N7 N 0.4280(6) 0.8452(5) 0.0386(4) 0.088(3) Uani 0.50 1 d PDU C -1 C65 C 0.4707(9) 0.9201(6) 0.0332(5) 0.085(2) Uani 0.50 1 d PDU C -1 C66 C 0.5258(9) 1.0254(6) 0.0312(5) 0.085(2) Uani 0.50 1 d PDU C -1 H66A H 0.5421 1.0609 0.0726 0.127 Uiso 0.50 1 calc PR C -1 H66B H 0.4763 1.0593 0.0066 0.127 Uiso 0.50 1 calc PR C -1 H66C H 0.5951 1.0247 0.0130 0.127 Uiso 0.50 1 calc PR C -1 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 0.01301(15) 0.01422(14) 0.01256(14) 0.00144(11) 0.00121(11) 0.00386(11) Ni2 0.01136(14) 0.01552(15) 0.01310(14) 0.00113(11) 0.00157(11) 0.00328(11) Ni3 0.01424(15) 0.01582(15) 0.01273(14) 0.00240(11) 0.00356(11) 0.00359(12) Ni4 0.02051(17) 0.01318(15) 0.01963(16) 0.00309(12) 0.00318(13) 0.00111(12) Ni5 0.02265(17) 0.01438(15) 0.01639(15) 0.00295(12) 0.00538(13) 0.00431(12) Ni6 0.02895(19) 0.02099(17) 0.02132(17) 0.00570(13) 0.00169(14) -0.00003(14) Cl1 0.0161(3) 0.0163(3) 0.0195(3) 0.0041(2) 0.0034(2) 0.0019(2) Cl2 0.0139(3) 0.0225(3) 0.0181(3) 0.0029(2) 0.0048(2) 0.0058(2) Cl3 0.0183(3) 0.0171(3) 0.0163(3) 0.0027(2) 0.0022(2) 0.0071(2) Cl4 0.0198(3) 0.0186(3) 0.0166(3) 0.0030(2) 0.0036(2) -0.0005(2) Cl5 0.0219(3) 0.0199(3) 0.0206(3) 0.0014(2) 0.0008(2) 0.0024(2) Cl6 0.0358(4) 0.0218(3) 0.0299(4) 0.0087(3) -0.0071(3) 0.0028(3) Cl7 0.0451(4) 0.0162(3) 0.0203(3) -0.0008(2) 0.0049(3) 0.0004(3) Cl8 0.0375(4) 0.0388(4) 0.0235(3) 0.0080(3) 0.0049(3) 0.0032(3) S1 0.0157(3) 0.0162(3) 0.0158(3) 0.0029(2) -0.0003(2) 0.0031(2) S2 0.0148(3) 0.0254(3) 0.0188(3) -0.0015(2) -0.0016(2) 0.0049(2) S3 0.0200(3) 0.0167(3) 0.0320(4) 0.0026(3) 0.0083(3) 0.0010(2) S4 0.0116(11) 0.0093(10) 0.0196(12) -0.0043(7) 0.0026(8) -0.0033(7) S4A 0.0294(13) 0.0401(15) 0.0313(12) 0.0133(10) 0.0136(10) 0.0186(11) O1 0.0149(8) 0.0162(8) 0.0128(8) 0.0007(6) 0.0013(6) 0.0041(6) O2 0.0117(8) 0.0138(8) 0.0122(8) 0.0012(6) 0.0011(6) 0.0016(6) O3 0.0297(10) 0.0154(8) 0.0182(9) 0.0028(7) 0.0073(7) 0.0019(7) O4 0.0202(9) 0.0138(8) 0.0179(8) 0.0038(7) 0.0023(7) 0.0017(7) O5 0.0464(17) 0.092(2) 0.064(2) -0.0133(17) 0.0152(15) -0.0205(16) N1 0.0168(10) 0.0170(10) 0.0191(10) 0.0023(8) 0.0004(8) 0.0055(8) N2 0.0138(10) 0.0137(9) 0.0164(10) 0.0037(8) 0.0031(8) 0.0036(8) N3 0.0210(11) 0.0148(10) 0.0206(11) 0.0027(8) 0.0035(9) 0.0021(8) N4 0.0196(11) 0.0142(10) 0.0173(10) 0.0020(8) 0.0031(8) 0.0045(8) N5 0.0266(12) 0.0199(11) 0.0185(11) 0.0038(8) 0.0071(9) 0.0043(9) N6 0.0354(15) 0.0288(13) 0.0245(12) 0.0065(10) 0.0037(10) 0.0014(11) C1 0.0303(14) 0.0205(12) 0.0145(12) 0.0029(10) 0.0052(10) 0.0049(11) C2 0.0154(11) 0.0152(11) 0.0196(12) 0.0038(9) 0.0057(9) 0.0018(9) C3 0.0193(12) 0.0230(13) 0.0220(13) 0.0081(10) 0.0033(10) 0.0053(10) C4 0.0267(14) 0.0224(13) 0.0303(15) 0.0133(11) 0.0068(11) 0.0092(11) C5 0.0323(15) 0.0180(12) 0.0284(14) 0.0060(11) 0.0089(12) 0.0074(11) C6 0.0267(14) 0.0208(13) 0.0223(13) 0.0018(10) 0.0031(11) 0.0038(11) C7 0.0155(12) 0.0173(12) 0.0196(12) 0.0050(9) 0.0045(9) 0.0044(9) C8 0.0452(18) 0.0211(13) 0.0243(14) -0.0048(11) -0.0078(13) 0.0176(13) C9 0.0515(19) 0.0250(14) 0.0219(14) -0.0057(11) -0.0136(13) 0.0206(14) C10 0.0185(12) 0.0198(12) 0.0180(12) 0.0000(10) -0.0005(10) 0.0054(10) C11 0.0219(13) 0.0205(12) 0.0212(13) 0.0020(10) -0.0003(10) 0.0074(10) C12 0.052(2) 0.0347(17) 0.0238(15) -0.0032(12) -0.0167(14) 0.0198(15) C13 0.103(3) 0.044(2) 0.0372(18) -0.0160(15) -0.0324(19) 0.037(2) C14 0.098(3) 0.0374(18) 0.0404(19) -0.0134(15) -0.0299(19) 0.0368(19) C15 0.0246(15) 0.0278(15) 0.0473(19) -0.0083(13) 0.0011(13) -0.0019(12) C16 0.0166(12) 0.0211(12) 0.0211(12) 0.0055(10) 0.0039(10) 0.0054(10) C17 0.0167(13) 0.0350(15) 0.0262(14) 0.0004(12) -0.0023(11) 0.0035(11) C18 0.0122(12) 0.0469(18) 0.0357(16) 0.0042(14) 0.0046(11) 0.0051(12) C19 0.0181(13) 0.0453(17) 0.0259(14) 0.0047(12) 0.0088(11) 0.0106(12) C20 0.0162(12) 0.0275(14) 0.0209(13) 0.0018(10) 0.0030(10) 0.0052(10) C21 0.0131(11) 0.0180(12) 0.0191(12) 0.0059(9) 0.0024(9) 0.0035(9) C22 0.0157(11) 0.0145(11) 0.0166(11) 0.0027(9) 0.0053(9) 0.0045(9) C23 0.0136(11) 0.0125(10) 0.0165(11) 0.0018(9) 0.0011(9) 0.0032(9) C24 0.0164(11) 0.0108(10) 0.0140(11) 0.0024(8) 0.0011(9) 0.0020(9) C25 0.0153(11) 0.0150(11) 0.0175(12) 0.0008(9) 0.0035(9) 0.0024(9) C26 0.0142(11) 0.0189(12) 0.0211(12) 0.0011(10) -0.0014(9) 0.0038(9) C27 0.0201(12) 0.0191(12) 0.0157(12) -0.0007(9) -0.0006(10) 0.0042(10) C28 0.0188(12) 0.0188(12) 0.0156(12) -0.0007(9) 0.0039(9) 0.0040(10) C29 0.0435(18) 0.0284(15) 0.0276(15) 0.0049(12) 0.0201(13) 0.0026(13) C30 0.0222(13) 0.0169(12) 0.0222(13) 0.0030(10) 0.0036(10) -0.0011(10) C31 0.0327(15) 0.0204(13) 0.0241(14) -0.0006(10) 0.0107(12) 0.0017(11) C32 0.0390(17) 0.0171(13) 0.0276(14) -0.0033(11) 0.0071(12) -0.0014(12) C33 0.0316(15) 0.0197(13) 0.0274(14) 0.0014(11) 0.0066(12) -0.0056(11) C34 0.0240(14) 0.0219(13) 0.0242(13) 0.0021(10) 0.0076(11) 0.0003(11) C35 0.0222(13) 0.0163(12) 0.0198(12) 0.0011(10) 0.0023(10) 0.0012(10) C36 0.0234(13) 0.0195(12) 0.0225(13) 0.0045(10) 0.0051(10) 0.0005(10) C37 0.0270(14) 0.0227(13) 0.0203(13) 0.0045(10) 0.0063(11) 0.0052(11) C38 0.0316(15) 0.0203(13) 0.0169(12) 0.0062(10) 0.0053(11) 0.0075(11) C39 0.0376(16) 0.0210(13) 0.0218(13) 0.0041(10) 0.0056(12) 0.0071(12) C40 0.0427(18) 0.0286(15) 0.0260(14) 0.0029(12) 0.0096(13) 0.0162(13) C41 0.0331(16) 0.0367(16) 0.0299(15) 0.0074(13) 0.0129(13) 0.0132(13) C42 0.0310(15) 0.0295(15) 0.0256(14) 0.0041(11) 0.0079(12) 0.0055(12) C43 0.022(4) 0.039(4) 0.036(4) 0.007(3) 0.006(3) 0.007(3) C43A 0.040(3) 0.026(3) 0.029(3) 0.001(2) 0.013(2) 0.012(2) C44 0.0270(14) 0.0234(13) 0.0321(15) 0.0089(11) 0.0097(12) 0.0096(11) C45 0.0237(14) 0.0259(14) 0.0483(19) 0.0095(13) 0.0111(13) 0.0107(12) C46 0.0196(13) 0.0214(13) 0.0414(17) -0.0005(12) -0.0081(12) 0.0071(11) C47 0.0293(15) 0.0259(14) 0.0229(13) 0.0030(11) -0.0048(11) 0.0091(11) C48 0.0190(13) 0.0256(13) 0.0220(13) 0.0041(10) 0.0006(10) 0.0064(10) C49 0.0195(12) 0.0153(11) 0.0236(13) 0.0025(10) 0.0010(10) 0.0046(10) C50 0.0217(13) 0.0165(11) 0.0172(12) 0.0038(9) 0.0025(10) 0.0054(10) C51 0.0203(12) 0.0147(11) 0.0162(11) 0.0012(9) 0.0021(9) 0.0047(9) C52 0.0194(12) 0.0126(11) 0.0169(12) -0.0009(9) -0.0005(9) 0.0012(9) C53 0.0234(13) 0.0137(11) 0.0197(12) 0.0016(9) -0.0026(10) 0.0030(10) C54 0.0181(12) 0.0185(12) 0.0283(14) -0.0019(10) -0.0024(10) 0.0061(10) C55 0.0202(13) 0.0228(13) 0.0261(14) 0.0017(11) 0.0061(11) 0.0045(10) C56 0.0237(13) 0.0188(12) 0.0210(13) 0.0046(10) 0.0044(10) 0.0051(10) C57 0.0304(15) 0.0314(15) 0.0258(15) 0.0046(12) 0.0078(12) -0.0001(12) C58 0.054(2) 0.072(3) 0.0220(16) 0.0101(16) 0.0041(15) -0.002(2) C59 0.0366(17) 0.0266(15) 0.0237(14) -0.0016(11) -0.0016(12) 0.0030(13) C60 0.0291(17) 0.045(2) 0.0443(19) -0.0173(15) 0.0010(14) -0.0039(14) C61 0.074(3) 0.039(2) 0.052(2) 0.0027(17) -0.017(2) 0.0173(19) C62 0.067(3) 0.076(3) 0.054(3) -0.011(2) 0.007(2) 0.011(2) C63 0.071(4) 0.160(7) 0.089(4) -0.014(4) 0.033(3) -0.032(4) C64 0.060(4) 0.252(11) 0.166(8) -0.083(7) 0.052(5) -0.026(5) N7 0.054(4) 0.072(5) 0.125(6) -0.033(4) -0.031(4) 0.026(4) C65 0.073(4) 0.086(4) 0.098(4) 0.013(3) 0.008(3) 0.023(3) C66 0.073(4) 0.086(4) 0.098(4) 0.013(3) 0.008(3) 0.023(3) _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 Ni1 N1 1.985(2) . ? Ni1 O1 2.0083(16) . ? Ni1 O2 2.1036(16) . ? Ni1 S1 2.3445(7) . ? Ni1 Cl1 2.4049(7) . ? Ni1 Cl2 2.4251(7) . ? Ni1 Ni2 2.8765(5) . ? Ni1 Ni3 2.9555(5) . ? Ni2 N2 1.995(2) . ? Ni2 O2 2.0194(16) . ? Ni2 O1 2.1060(16) . ? Ni2 S2 2.3373(7) . ? Ni2 Cl1 2.4167(7) . ? Ni2 Cl3 2.4290(7) . ? Ni2 Ni3 2.9617(5) . ? Ni3 N5 2.029(2) . ? Ni3 O2 2.0792(16) . ? Ni3 O1 2.2228(17) . ? Ni3 Cl4 2.3180(7) . ? Ni3 Cl2 2.4126(7) . ? Ni3 Cl3 2.4134(7) . ? Ni4 N3 1.995(2) . ? Ni4 O3 2.0157(18) . ? Ni4 O4 2.0972(17) . ? Ni4 S3 2.3339(7) . ? Ni4 Cl6 2.4275(8) . ? Ni4 Cl5 2.4280(7) . ? Ni4 Ni5 2.8680(5) . ? Ni4 Ni6 2.9793(5) . ? Ni5 N4 1.986(2) . ? Ni5 O4 2.0211(18) . ? Ni5 O3 2.1008(18) . ? Ni5 S4A 2.299(2) . ? Ni5 Cl5 2.4086(7) . ? Ni5 Cl7 2.4114(7) . ? Ni5 S4 2.433(3) . ? Ni5 Ni6 2.9820(5) . ? Ni6 N6 2.041(3) . ? Ni6 O3 2.1425(19) . ? Ni6 O4 2.2059(17) . ? Ni6 Cl8 2.2903(8) . ? Ni6 Cl6 2.4235(8) . ? Ni6 Cl7 2.4513(8) . ? S1 C2 1.785(2) . ? S1 C1 1.814(3) . ? S2 C16 1.783(3) . ? S2 C15 1.810(3) . ? S3 C30 1.779(3) . ? S3 C29 1.806(3) . ? S4 C43 1.296(8) . ? S4 C44 1.746(4) . ? S4A C43A 1.475(6) . ? S4A C44 1.842(4) . ? O1 C10 1.342(3) . ? O2 C24 1.355(3) . ? O3 C38 1.349(3) . ? O4 C52 1.345(3) . ? O5 C63 1.386(6) . ? O5 C61 1.409(5) . ? N1 C8 1.281(3) . ? N1 C7 1.433(3) . ? N2 C22 1.290(3) . ? N2 C21 1.431(3) . ? N3 C36 1.287(3) . ? N3 C35 1.430(3) . ? N4 C50 1.283(3) . ? N4 C49 1.427(3) . ? N5 C57 1.134(4) . ? N6 C59 1.139(4) . ? C2 C3 1.397(3) . ? C2 C7 1.399(3) . ? C3 C4 1.377(4) . ? C4 C5 1.393(4) . ? C5 C6 1.384(4) . ? C6 C7 1.396(4) . ? C8 C9 1.458(4) . ? C9 C14 1.405(4) . ? C9 C10 1.414(4) . ? C10 C11 1.402(3) . ? C11 C12 1.373(4) . ? C12 C13 1.386(5) . ? C13 C14 1.374(5) . ? C16 C17 1.395(4) . ? C16 C21 1.401(4) . ? C17 C18 1.384(4) . ? C18 C19 1.378(4) . ? C19 C20 1.379(4) . ? C20 C21 1.403(3) . ? C22 C23 1.454(3) . ? C23 C24 1.407(3) . ? C23 C28 1.412(3) . ? C24 C25 1.395(3) . ? C25 C26 1.388(3) . ? C26 C27 1.389(3) . ? C27 C28 1.376(3) . ? C30 C31 1.395(4) . ? C30 C35 1.399(4) . ? C31 C32 1.382(4) . ? C32 C33 1.388(4) . ? C33 C34 1.380(4) . ? C34 C35 1.403(4) . ? C36 C37 1.455(4) . ? C37 C38 1.414(4) . ? C37 C42 1.417(4) . ? C38 C39 1.396(4) . ? C39 C40 1.378(4) . ? C40 C41 1.388(4) . ? C41 C42 1.372(4) . ? C44 C45 1.392(4) . ? C44 C49 1.398(4) . ? C45 C46 1.370(4) . ? C46 C47 1.392(4) . ? C47 C48 1.381(4) . ? C48 C49 1.399(4) . ? C50 C51 1.465(3) . ? C51 C56 1.411(4) . ? C51 C52 1.412(3) . ? C52 C53 1.399(3) . ? C53 C54 1.383(4) . ? C54 C55 1.388(4) . ? C55 C56 1.378(4) . ? C57 C58 1.464(4) . ? C59 C60 1.453(4) . ? C61 C62 1.441(6) . ? C63 C64 1.515(10) . ? N7 C65 1.1011(10) . ? C65 C66 1.5009(9) . ? 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 N1 Ni1 O1 96.26(8) . . ? N1 Ni1 O2 169.14(7) . . ? O1 Ni1 O2 73.22(6) . . ? N1 Ni1 S1 87.54(6) . . ? O1 Ni1 S1 174.53(5) . . ? O2 Ni1 S1 103.15(5) . . ? N1 Ni1 Cl1 92.52(6) . . ? O1 Ni1 Cl1 85.18(5) . . ? O2 Ni1 Cl1 84.06(5) . . ? S1 Ni1 Cl1 98.62(2) . . ? N1 Ni1 Cl2 96.11(6) . . ? O1 Ni1 Cl2 83.74(5) . . ? O2 Ni1 Cl2 85.58(5) . . ? S1 Ni1 Cl2 91.96(2) . . ? Cl1 Ni1 Cl2 166.63(2) . . ? N1 Ni1 Ni2 125.83(6) . . ? O1 Ni1 Ni2 47.05(5) . . ? O2 Ni1 Ni2 44.57(4) . . ? S1 Ni1 Ni2 132.86(2) . . ? Cl1 Ni1 Ni2 53.563(17) . . ? Cl2 Ni1 Ni2 113.09(2) . . ? N1 Ni1 Ni3 129.51(6) . . ? O1 Ni1 Ni3 48.75(5) . . ? O2 Ni1 Ni3 44.71(4) . . ? S1 Ni1 Ni3 125.81(2) . . ? Cl1 Ni1 Ni3 114.556(18) . . ? Cl2 Ni1 Ni3 52.153(16) . . ? Ni2 Ni1 Ni3 61.021(11) . . ? N2 Ni2 O2 94.27(7) . . ? N2 Ni2 O1 166.53(7) . . ? O2 Ni2 O1 72.95(6) . . ? N2 Ni2 S2 87.57(6) . . ? O2 Ni2 S2 176.61(5) . . ? O1 Ni2 S2 105.41(5) . . ? N2 Ni2 Cl1 92.13(6) . . ? O2 Ni2 Cl1 85.56(5) . . ? O1 Ni2 Cl1 82.83(5) . . ? S2 Ni2 Cl1 97.23(2) . . ? N2 Ni2 Cl3 99.66(6) . . ? O2 Ni2 Cl3 85.10(5) . . ? O1 Ni2 Cl3 83.78(5) . . ? S2 Ni2 Cl3 91.79(2) . . ? Cl1 Ni2 Cl3 165.45(2) . . ? N2 Ni2 Ni1 123.39(6) . . ? O2 Ni2 Ni1 46.97(5) . . ? O1 Ni2 Ni1 44.27(4) . . ? S2 Ni2 Ni1 133.75(2) . . ? Cl1 Ni2 Ni1 53.185(16) . . ? Cl3 Ni2 Ni1 112.584(19) . . ? N2 Ni2 Ni3 124.32(6) . . ? O2 Ni2 Ni3 44.54(5) . . ? O1 Ni2 Ni3 48.50(5) . . ? S2 Ni2 Ni3 132.17(2) . . ? Cl1 Ni2 Ni3 113.962(19) . . ? Cl3 Ni2 Ni3 52.054(16) . . ? Ni1 Ni2 Ni3 60.805(12) . . ? N5 Ni3 O2 163.85(8) . . ? N5 Ni3 O1 94.58(8) . . ? O2 Ni3 O1 69.45(6) . . ? N5 Ni3 Cl4 100.61(7) . . ? O2 Ni3 Cl4 95.32(5) . . ? O1 Ni3 Cl4 164.76(5) . . ? N5 Ni3 Cl2 93.25(6) . . ? O2 Ni3 Cl2 86.44(5) . . ? O1 Ni3 Cl2 79.75(5) . . ? Cl4 Ni3 Cl2 100.45(3) . . ? N5 Ni3 Cl3 91.24(7) . . ? O2 Ni3 Cl3 84.24(5) . . ? O1 Ni3 Cl3 81.76(5) . . ? Cl4 Ni3 Cl3 96.59(2) . . ? Cl2 Ni3 Cl3 161.25(2) . . ? N5 Ni3 Ni1 123.56(6) . . ? O2 Ni3 Ni1 45.38(4) . . ? O1 Ni3 Ni1 42.79(4) . . ? Cl4 Ni3 Ni1 126.01(2) . . ? Cl2 Ni3 Ni1 52.535(17) . . ? Cl3 Ni3 Ni1 110.441(19) . . ? N5 Ni3 Ni2 123.42(7) . . ? O2 Ni3 Ni2 42.94(4) . . ? O1 Ni3 Ni2 45.20(4) . . ? Cl4 Ni3 Ni2 122.62(2) . . ? Cl2 Ni3 Ni2 110.63(2) . . ? Cl3 Ni3 Ni2 52.534(17) . . ? Ni1 Ni3 Ni2 58.173(10) . . ? N3 Ni4 O3 95.91(8) . . ? N3 Ni4 O4 168.25(8) . . ? O3 Ni4 O4 73.40(7) . . ? N3 Ni4 S3 87.64(6) . . ? O3 Ni4 S3 174.90(6) . . ? O4 Ni4 S3 103.36(5) . . ? N3 Ni4 Cl6 98.15(7) . . ? O3 Ni4 Cl6 83.83(6) . . ? O4 Ni4 Cl6 85.75(5) . . ? S3 Ni4 Cl6 92.06(3) . . ? N3 Ni4 Cl5 90.77(6) . . ? O3 Ni4 Cl5 85.40(6) . . ? O4 Ni4 Cl5 83.63(5) . . ? S3 Ni4 Cl5 98.24(3) . . ? Cl6 Ni4 Cl5 166.65(3) . . ? N3 Ni4 Ni5 124.05(6) . . ? O3 Ni4 Ni5 47.07(5) . . ? O4 Ni4 Ni5 44.78(5) . . ? S3 Ni4 Ni5 133.06(2) . . ? Cl6 Ni4 Ni5 113.33(2) . . ? Cl5 Ni4 Ni5 53.319(17) . . ? N3 Ni4 Ni6 127.38(6) . . ? O3 Ni4 Ni6 45.96(5) . . ? O4 Ni4 Ni6 47.71(5) . . ? S3 Ni4 Ni6 128.95(2) . . ? Cl6 Ni4 Ni6 52.048(19) . . ? Cl5 Ni4 Ni6 114.60(2) . . ? Ni5 Ni4 Ni6 61.290(13) . . ? N4 Ni5 O4 95.21(8) . . ? N4 Ni5 O3 168.31(8) . . ? O4 Ni5 O3 73.21(7) . . ? N4 Ni5 S4A 87.83(8) . . ? O4 Ni5 S4A 173.54(11) . . ? O3 Ni5 S4A 103.86(8) . . ? N4 Ni5 Cl5 93.59(6) . . ? O4 Ni5 Cl5 85.74(5) . . ? O3 Ni5 Cl5 84.09(5) . . ? S4A Ni5 Cl5 99.79(11) . . ? N4 Ni5 Cl7 94.53(6) . . ? O4 Ni5 Cl7 84.61(5) . . ? O3 Ni5 Cl7 86.15(5) . . ? S4A Ni5 Cl7 89.46(11) . . ? Cl5 Ni5 Cl7 167.91(3) . . ? N4 Ni5 S4 86.82(9) . . ? O4 Ni5 S4 172.82(8) . . ? O3 Ni5 S4 104.48(9) . . ? S4A Ni5 S4 12.65(7) . . ? Cl5 Ni5 S4 87.26(7) . . ? Cl7 Ni5 S4 102.12(7) . . ? N4 Ni5 Ni4 125.63(6) . . ? O4 Ni5 Ni4 46.96(5) . . ? O3 Ni5 Ni4 44.63(5) . . ? S4A Ni5 Ni4 134.56(9) . . ? Cl5 Ni5 Ni4 53.943(18) . . ? Cl7 Ni5 Ni4 113.96(2) . . ? S4 Ni5 Ni4 126.70(6) . . ? N4 Ni5 Ni6 126.68(6) . . ? O4 Ni5 Ni6 47.71(5) . . ? O3 Ni5 Ni6 45.92(5) . . ? S4A Ni5 Ni6 126.15(9) . . ? Cl5 Ni5 Ni6 115.13(2) . . ? Cl7 Ni5 Ni6 52.78(2) . . ? S4 Ni5 Ni6 135.22(8) . . ? Ni4 Ni5 Ni6 61.195(11) . . ? N6 Ni6 O3 161.81(8) . . ? N6 Ni6 O4 92.97(8) . . ? O3 Ni6 O4 68.85(6) . . ? N6 Ni6 Cl8 94.89(7) . . ? O3 Ni6 Cl8 103.30(5) . . ? O4 Ni6 Cl8 172.07(5) . . ? N6 Ni6 Cl6 96.59(7) . . ? O3 Ni6 Cl6 81.36(5) . . ? O4 Ni6 Cl6 83.54(5) . . ? Cl8 Ni6 Cl6 96.58(3) . . ? N6 Ni6 Cl7 93.28(7) . . ? O3 Ni6 Cl7 84.26(5) . . ? O4 Ni6 Cl7 79.93(5) . . ? Cl8 Ni6 Cl7 98.54(3) . . ? Cl6 Ni6 Cl7 161.15(3) . . ? N6 Ni6 Ni4 123.14(7) . . ? O3 Ni6 Ni4 42.56(5) . . ? O4 Ni6 Ni4 44.69(4) . . ? Cl8 Ni6 Ni4 130.03(2) . . ? Cl6 Ni6 Ni4 52.170(19) . . ? Cl7 Ni6 Ni4 109.07(2) . . ? N6 Ni6 Ni5 121.21(7) . . ? O3 Ni6 Ni5 44.78(5) . . ? O4 Ni6 Ni5 42.67(5) . . ? Cl8 Ni6 Ni5 130.83(3) . . ? Cl6 Ni6 Ni5 109.68(2) . . ? Cl7 Ni6 Ni5 51.572(18) . . ? Ni4 Ni6 Ni5 57.515(12) . . ? Ni1 Cl1 Ni2 73.252(19) . . ? Ni3 Cl2 Ni1 75.31(2) . . ? Ni3 Cl3 Ni2 75.412(19) . . ? Ni5 Cl5 Ni4 72.74(2) . . ? Ni6 Cl6 Ni4 75.78(2) . . ? Ni5 Cl7 Ni6 75.65(2) . . ? C2 S1 C1 101.80(12) . . ? C2 S1 Ni1 94.75(8) . . ? C1 S1 Ni1 111.01(9) . . ? C16 S2 C15 103.35(14) . . ? C16 S2 Ni2 95.05(9) . . ? C15 S2 Ni2 111.73(11) . . ? C30 S3 C29 100.84(13) . . ? C30 S3 Ni4 95.15(9) . . ? C29 S3 Ni4 109.48(10) . . ? C43 S4 C44 126.9(4) . . ? C43 S4 Ni5 122.9(4) . . ? C44 S4 Ni5 92.97(15) . . ? C43A S4A C44 106.1(3) . . ? C43A S4A Ni5 133.3(3) . . ? C44 S4A Ni5 94.93(13) . . ? C10 O1 Ni1 124.53(15) . . ? C10 O1 Ni2 127.51(15) . . ? Ni1 O1 Ni2 88.69(6) . . ? C10 O1 Ni3 128.36(15) . . ? Ni1 O1 Ni3 88.46(6) . . ? Ni2 O1 Ni3 86.30(6) . . ? C24 O2 Ni2 125.54(14) . . ? C24 O2 Ni3 130.74(14) . . ? Ni2 O2 Ni3 92.53(6) . . ? C24 O2 Ni1 117.76(13) . . ? Ni2 O2 Ni1 88.46(6) . . ? Ni3 O2 Ni1 89.91(6) . . ? C38 O3 Ni4 124.52(16) . . ? C38 O3 Ni5 122.75(16) . . ? Ni4 O3 Ni5 88.30(7) . . ? C38 O3 Ni6 128.87(16) . . ? Ni4 O3 Ni6 91.48(7) . . ? Ni5 O3 Ni6 89.29(7) . . ? C52 O4 Ni5 124.53(15) . . ? C52 O4 Ni4 132.00(15) . . ? Ni5 O4 Ni4 88.26(7) . . ? C52 O4 Ni6 122.26(15) . . ? Ni5 O4 Ni6 89.63(7) . . ? Ni4 O4 Ni6 87.60(6) . . ? C63 O5 C61 112.9(4) . . ? C8 N1 C7 120.9(2) . . ? C8 N1 Ni1 121.41(18) . . ? C7 N1 Ni1 117.67(16) . . ? C22 N2 C21 119.1(2) . . ? C22 N2 Ni2 122.52(16) . . ? C21 N2 Ni2 117.58(16) . . ? C36 N3 C35 120.7(2) . . ? C36 N3 Ni4 121.63(18) . . ? C35 N3 Ni4 117.56(16) . . ? C50 N4 C49 119.9(2) . . ? C50 N4 Ni5 122.41(17) . . ? C49 N4 Ni5 117.61(16) . . ? C57 N5 Ni3 164.4(2) . . ? C59 N6 Ni6 169.1(2) . . ? C3 C2 C7 120.7(2) . . ? C3 C2 S1 118.22(19) . . ? C7 C2 S1 121.06(18) . . ? C4 C3 C2 120.1(2) . . ? C3 C4 C5 119.9(2) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C7 121.1(3) . . ? C6 C7 C2 118.2(2) . . ? C6 C7 N1 123.7(2) . . ? C2 C7 N1 118.1(2) . . ? N1 C8 C9 128.1(2) . . ? C14 C9 C10 117.7(3) . . ? C14 C9 C8 114.9(3) . . ? C10 C9 C8 127.4(2) . . ? O1 C10 C11 118.9(2) . . ? O1 C10 C9 122.1(2) . . ? C11 C10 C9 119.0(2) . . ? C12 C11 C10 121.4(2) . . ? C11 C12 C13 120.3(3) . . ? C14 C13 C12 119.1(3) . . ? C13 C14 C9 122.6(3) . . ? C17 C16 C21 120.3(2) . . ? C17 C16 S2 118.8(2) . . ? C21 C16 S2 120.81(19) . . ? C18 C17 C16 120.0(3) . . ? C19 C18 C17 119.8(3) . . ? C18 C19 C20 121.0(3) . . ? C19 C20 C21 120.2(3) . . ? C16 C21 C20 118.5(2) . . ? C16 C21 N2 118.1(2) . . ? C20 C21 N2 123.4(2) . . ? N2 C22 C23 127.8(2) . . ? C24 C23 C28 118.3(2) . . ? C24 C23 C22 127.1(2) . . ? C28 C23 C22 114.6(2) . . ? O2 C24 C25 118.7(2) . . ? O2 C24 C23 121.7(2) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 120.5(2) . . ? C25 C26 C27 120.5(2) . . ? C28 C27 C26 119.2(2) . . ? C27 C28 C23 121.7(2) . . ? C31 C30 C35 120.6(2) . . ? C31 C30 S3 118.1(2) . . ? C35 C30 S3 121.3(2) . . ? C32 C31 C30 120.5(3) . . ? C31 C32 C33 119.2(3) . . ? C34 C33 C32 120.8(3) . . ? C33 C34 C35 120.8(2) . . ? C30 C35 C34 118.1(2) . . ? C30 C35 N3 118.0(2) . . ? C34 C35 N3 123.9(2) . . ? N3 C36 C37 128.2(2) . . ? C38 C37 C42 117.9(2) . . ? C38 C37 C36 127.4(2) . . ? C42 C37 C36 114.7(2) . . ? O3 C38 C39 118.5(2) . . ? O3 C38 C37 122.3(2) . . ? C39 C38 C37 119.2(3) . . ? C40 C39 C38 121.2(3) . . ? C39 C40 C41 120.2(3) . . ? C42 C41 C40 119.6(3) . . ? C41 C42 C37 121.7(3) . . ? C45 C44 C49 120.7(3) . . ? C45 C44 S4 115.4(2) . . ? C49 C44 S4 123.2(2) . . ? C45 C44 S4A 120.5(2) . . ? C49 C44 S4A 118.3(2) . . ? S4 C44 S4A 16.98(8) . . ? C46 C45 C44 120.6(3) . . ? C45 C46 C47 119.3(3) . . ? C48 C47 C46 120.7(3) . . ? C47 C48 C49 120.6(3) . . ? C44 C49 C48 118.1(2) . . ? C44 C49 N4 118.5(2) . . ? C48 C49 N4 123.4(2) . . ? N4 C50 C51 127.1(2) . . ? C56 C51 C52 118.3(2) . . ? C56 C51 C50 114.6(2) . . ? C52 C51 C50 127.1(2) . . ? O4 C52 C53 118.6(2) . . ? O4 C52 C51 122.3(2) . . ? C53 C52 C51 119.1(2) . . ? C54 C53 C52 120.8(2) . . ? C53 C54 C55 120.7(2) . . ? C56 C55 C54 119.0(2) . . ? C55 C56 C51 121.9(2) . . ? N5 C57 C58 178.5(4) . . ? N6 C59 C60 177.3(3) . . ? O5 C61 C62 111.3(3) . . ? O5 C63 C64 106.6(6) . . ? N7 C65 C66 175.0(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.931 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.095 data_c097 _database_code_depnum_ccdc_archive 'CCDC 918631' #TrackingRef 'web_deposit_cif_file_7_XiaoluSong_1360938597.C097.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H68 N8 Na4 O4' _chemical_formula_weight 913.06 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+3/4' 'y+1/4, -x+1/4, z+1/4' '-x, -y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+5/4' 'y+3/4, -x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' '-x, -y, -z' 'y-1/4, -x-3/4, -z-3/4' '-y-1/4, x-1/4, -z-1/4' 'x, y-1/2, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z-1/4' '-y+1/4, x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' _cell_length_a 20.2549(14) _cell_length_b 20.2549(14) _cell_length_c 12.4783(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5119.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8893 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 28.27 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9396 _exptl_absorpt_correction_T_max 0.9513 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25665 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2952 _reflns_number_gt 2685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0528P)^2^+4.6678P] 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 2952 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.57035(2) 0.70096(2) 0.04118(4) 0.01731(14) Uani 1 1 d . . . O1 O 0.56577(4) 0.70874(4) 0.22379(7) 0.01824(19) Uani 1 1 d . . . N1 N 0.59486(5) 0.59079(5) 0.10289(8) 0.0200(2) Uani 1 1 d . . . N2 N 0.65170(5) 0.66403(5) -0.10835(8) 0.0196(2) Uani 1 1 d . . . C1 C 0.59229(6) 0.67659(6) 0.30240(9) 0.0175(2) Uani 1 1 d . . . C2 C 0.60269(6) 0.70749(7) 0.40332(10) 0.0233(3) Uani 1 1 d . . . H2A H 0.5928 0.7531 0.4105 0.028 Uiso 1 1 calc R . . C3 C 0.62654(7) 0.67385(7) 0.49109(10) 0.0275(3) Uani 1 1 d . . . H3A H 0.6328 0.6966 0.5569 0.033 Uiso 1 1 calc R . . C4 C 0.64152(6) 0.60683(7) 0.48447(11) 0.0271(3) Uani 1 1 d . . . H4A H 0.6568 0.5833 0.5455 0.033 Uiso 1 1 calc R . . C5 C 0.63372(6) 0.57545(7) 0.38725(10) 0.0240(3) Uani 1 1 d . . . H5A H 0.6443 0.5299 0.3822 0.029 Uiso 1 1 calc R . . C6 C 0.61077(6) 0.60837(6) 0.29539(9) 0.0186(2) Uani 1 1 d . . . C7 C 0.60526(6) 0.56930(6) 0.19750(10) 0.0197(3) Uani 1 1 d . . . H7A H 0.6099 0.5229 0.2051 0.024 Uiso 1 1 calc R . . C8 C 0.59325(7) 0.54040(6) 0.01849(11) 0.0238(3) Uani 1 1 d . . . H8A H 0.5537 0.5472 -0.0267 0.029 Uiso 1 1 calc R . . H8B H 0.5899 0.4961 0.0517 0.029 Uiso 1 1 calc R . . C9 C 0.65496(7) 0.54316(6) -0.05177(10) 0.0239(3) Uani 1 1 d . . . H9A H 0.6935 0.5521 -0.0051 0.029 Uiso 1 1 calc R . . H9B H 0.6616 0.4991 -0.0844 0.029 Uiso 1 1 calc R . . C10 C 0.65425(7) 0.59436(6) -0.14128(10) 0.0235(3) Uani 1 1 d . . . H10A H 0.6943 0.5879 -0.1855 0.028 Uiso 1 1 calc R . . H10B H 0.6156 0.5854 -0.1877 0.028 Uiso 1 1 calc R . . C11 C 0.71124(6) 0.68245(7) -0.04849(11) 0.0260(3) Uani 1 1 d . . . H11A H 0.7504 0.6724 -0.0916 0.039 Uiso 1 1 calc R . . H11B H 0.7130 0.6574 0.0187 0.039 Uiso 1 1 calc R . . H11C H 0.7101 0.7298 -0.0325 0.039 Uiso 1 1 calc R . . C12 C 0.64801(7) 0.70448(7) -0.20584(10) 0.0256(3) Uani 1 1 d . . . H12A H 0.6798 0.6880 -0.2587 0.038 Uiso 1 1 calc R . . H12B H 0.6584 0.7505 -0.1882 0.038 Uiso 1 1 calc R . . H12C H 0.6033 0.7020 -0.2357 0.038 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 Na1 0.0183(2) 0.0189(2) 0.0147(2) 0.00071(17) 0.00098(17) 0.00244(17) O1 0.0206(4) 0.0188(4) 0.0153(4) 0.0017(3) -0.0017(3) 0.0015(3) N1 0.0227(5) 0.0179(5) 0.0193(5) -0.0004(4) 0.0008(4) 0.0007(4) N2 0.0224(5) 0.0198(5) 0.0167(5) -0.0013(4) 0.0000(4) 0.0032(4) C1 0.0146(5) 0.0219(6) 0.0161(5) 0.0028(4) 0.0009(4) -0.0029(4) C2 0.0263(6) 0.0253(6) 0.0182(6) -0.0001(5) -0.0006(5) -0.0045(5) C3 0.0277(7) 0.0392(8) 0.0157(6) 0.0013(5) -0.0028(5) -0.0088(5) C4 0.0226(6) 0.0391(7) 0.0196(6) 0.0134(5) -0.0044(5) -0.0050(5) C5 0.0213(6) 0.0263(6) 0.0244(6) 0.0096(5) -0.0006(5) -0.0016(5) C6 0.0157(5) 0.0219(6) 0.0182(6) 0.0050(4) 0.0003(4) -0.0016(4) C7 0.0188(6) 0.0162(5) 0.0241(6) 0.0032(4) 0.0009(5) 0.0006(4) C8 0.0302(7) 0.0172(6) 0.0239(6) -0.0021(5) -0.0025(5) -0.0010(5) C9 0.0314(7) 0.0185(6) 0.0219(6) -0.0050(5) -0.0023(5) 0.0055(5) C10 0.0301(7) 0.0226(6) 0.0179(6) -0.0051(5) 0.0007(5) 0.0035(5) C11 0.0242(6) 0.0258(6) 0.0280(7) -0.0040(5) -0.0025(5) 0.0018(5) C12 0.0315(7) 0.0275(6) 0.0177(6) 0.0021(5) 0.0048(5) 0.0051(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 O1 2.2860(10) . ? Na1 O1 2.2935(9) 10_576 ? Na1 O1 2.4061(10) 15_655 ? Na1 N1 2.4123(11) . ? Na1 N2 2.5991(11) . ? Na1 C1 3.0923(12) 15_655 ? Na1 Na1 3.2266(8) 10_576 ? Na1 Na1 3.2266(8) 15_655 ? Na1 Na1 3.4740(9) 4_665 ? O1 C1 1.2943(14) . ? O1 Na1 2.2935(9) 15_655 ? O1 Na1 2.4062(10) 10_576 ? N1 C7 1.2757(16) . ? N1 C8 1.4670(16) . ? N2 C11 1.4669(16) . ? N2 C12 1.4686(16) . ? N2 C10 1.4706(16) . ? C1 C2 1.4219(17) . ? C1 C6 1.4342(17) . ? C1 Na1 3.0924(12) 10_576 ? C2 C3 1.3773(18) . ? C2 H2A 0.9500 . ? C3 C4 1.394(2) . ? C3 H3A 0.9500 . ? C4 C5 1.3787(19) . ? C4 H4A 0.9500 . ? C5 C6 1.4051(16) . ? C5 H5A 0.9500 . ? C6 C7 1.4596(17) . ? C7 H7A 0.9500 . ? C8 C9 1.5277(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.5243(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 O1 Na1 O1 92.94(4) . 10_576 ? O1 Na1 O1 90.04(3) . 15_655 ? O1 Na1 O1 83.97(3) 10_576 15_655 ? O1 Na1 N1 75.76(3) . . ? O1 Na1 N1 95.29(4) 10_576 . ? O1 Na1 N1 165.74(4) 15_655 . ? O1 Na1 N2 139.57(4) . . ? O1 Na1 N2 121.59(4) 10_576 . ? O1 Na1 N2 112.19(3) 15_655 . ? N1 Na1 N2 80.35(4) . . ? O1 Na1 C1 108.26(3) . 15_655 ? O1 Na1 C1 97.22(3) 10_576 15_655 ? O1 Na1 C1 23.21(3) 15_655 15_655 ? N1 Na1 C1 166.60(4) . 15_655 ? N2 Na1 C1 89.01(3) . 15_655 ? O1 Na1 Na1 48.13(3) . 10_576 ? O1 Na1 Na1 45.11(2) 10_576 10_576 ? O1 Na1 Na1 89.77(2) 15_655 10_576 ? N1 Na1 Na1 79.84(3) . 10_576 ? N2 Na1 Na1 154.43(3) . 10_576 ? C1 Na1 Na1 112.56(2) 15_655 10_576 ? O1 Na1 Na1 45.30(2) . 15_655 ? O1 Na1 Na1 91.81(2) 10_576 15_655 ? O1 Na1 Na1 45.03(2) 15_655 15_655 ? N1 Na1 Na1 120.92(3) . 15_655 ? N2 Na1 Na1 139.99(3) . 15_655 ? C1 Na1 Na1 63.49(2) 15_655 15_655 ? Na1 Na1 Na1 65.142(16) 10_576 15_655 ? O1 Na1 Na1 85.83(2) . 4_665 ? O1 Na1 Na1 43.60(2) 10_576 4_665 ? O1 Na1 Na1 41.10(2) 15_655 4_665 ? N1 Na1 Na1 134.25(3) . 4_665 ? N2 Na1 Na1 133.20(2) . 4_665 ? C1 Na1 Na1 59.14(2) 15_655 4_665 ? Na1 Na1 Na1 57.429(8) 10_576 4_665 ? Na1 Na1 Na1 57.429(8) 15_655 4_665 ? C1 O1 Na1 134.74(8) . . ? C1 O1 Na1 128.24(8) . 15_655 ? Na1 O1 Na1 89.59(3) . 15_655 ? C1 O1 Na1 109.68(7) . 10_576 ? Na1 O1 Na1 86.85(3) . 10_576 ? Na1 O1 Na1 95.30(3) 15_655 10_576 ? C7 N1 C8 115.51(10) . . ? C7 N1 Na1 130.16(8) . . ? C8 N1 Na1 114.20(8) . . ? C11 N2 C12 108.76(10) . . ? C11 N2 C10 110.95(10) . . ? C12 N2 C10 107.80(10) . . ? C11 N2 Na1 94.73(7) . . ? C12 N2 Na1 113.69(7) . . ? C10 N2 Na1 119.94(8) . . ? O1 C1 C2 120.74(11) . . ? O1 C1 C6 123.15(11) . . ? C2 C1 C6 116.07(11) . . ? O1 C1 Na1 47.11(5) . 10_576 ? C2 C1 Na1 117.56(8) . 10_576 ? C6 C1 Na1 103.76(7) . 10_576 ? C3 C2 C1 122.57(12) . . ? C3 C2 H2A 118.7 . . ? C1 C2 H2A 118.7 . . ? C2 C3 C4 120.74(12) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 118.44(12) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 C6 122.48(12) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 119.59(11) . . ? C5 C6 C7 116.79(11) . . ? C1 C6 C7 123.60(10) . . ? N1 C7 C6 127.02(11) . . ? N1 C7 H7A 116.5 . . ? C6 C7 H7A 116.5 . . ? N1 C8 C9 111.61(10) . . ? N1 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 115.97(11) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C9 116.64(10) . . ? N2 C10 H10A 108.1 . . ? C9 C10 H10A 108.1 . . ? N2 C10 H10B 108.1 . . ? C9 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.367 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.061