# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_Cambridge 1500 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Sasankasekhar Mohanta' _publ_contact_author_email sm_cu_chem@yahoo.co.in _publ_section_title ; Syntheses, crystal structures and supramolecular topologies of nickel(II)-s/p/d10/NH4+ complexes derived from a compartmental ligand+ ; loop_ _publ_author_name S.Mohanta S.Sarkar # Attachment '- 1-10 CIF.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 813955' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H70 Cl Li N6 Ni3 O18' _chemical_formula_weight 1381.74 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' Li Li -0.0003 0.0001 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8610(16) _cell_length_b 15.811(2) _cell_length_c 17.483(2) _cell_angle_alpha 84.901(2) _cell_angle_beta 73.443(2) _cell_angle_gamma 80.682(2) _cell_volume 3098.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2551 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 19.10 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7916 _exptl_absorpt_correction_T_max 0.8618 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22237 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10803 _reflns_number_gt 5130 _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^)+(0.0500P)^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 10803 _refine_ls_number_parameters 860 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1460 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 C1 C 0.4004(5) 0.2246(4) 0.0133(3) 0.0586(15) Uani 1 1 d . . . C2 C 0.4557(5) 0.2930(4) 0.0234(4) 0.0646(17) Uani 1 1 d . . . C3 C 0.4436(6) 0.3703(4) -0.0180(4) 0.089(2) Uani 1 1 d . . . H3 H 0.4800 0.4151 -0.0093 0.107 Uiso 1 1 calc R . . C4 C 0.3774(7) 0.3814(5) -0.0724(5) 0.104(3) Uani 1 1 d . . . H4 H 0.3688 0.4342 -0.0997 0.125 Uiso 1 1 calc R . . C5 C 0.3245(6) 0.3164(5) -0.0868(4) 0.094(2) Uani 1 1 d . . . H5 H 0.2820 0.3241 -0.1247 0.113 Uiso 1 1 calc R . . C6 C 0.3353(5) 0.2372(4) -0.0433(4) 0.0648(16) Uani 1 1 d . . . C7 C 0.2804(5) 0.1700(5) -0.0591(4) 0.0763(19) Uani 1 1 d . . . H7 H 0.2362 0.1825 -0.0959 0.092 Uiso 1 1 calc R . . C8 C 0.2191(5) 0.0309(4) -0.0476(4) 0.0836(19) Uani 1 1 d . . . H8A H 0.2183 0.0396 -0.1031 0.100 Uiso 1 1 calc R . . H8B H 0.1378 0.0377 -0.0141 0.100 Uiso 1 1 calc R . . C9 C 0.2822(5) -0.0563(4) -0.0332(3) 0.0738(18) Uani 1 1 d . . . H9A H 0.2292 -0.0989 -0.0254 0.089 Uiso 1 1 calc R . . H9B H 0.3501 -0.0713 -0.0785 0.089 Uiso 1 1 calc R . . C10 C 0.3269(5) -0.1200(4) 0.0846(4) 0.0704(18) Uani 1 1 d . . . H10 H 0.2964 -0.1669 0.0740 0.084 Uiso 1 1 calc R . . C11 C 0.3756(5) -0.1292(4) 0.1506(4) 0.0615(16) Uani 1 1 d . . . C12 C 0.3709(6) -0.2052(4) 0.1980(5) 0.093(2) Uani 1 1 d . . . H12 H 0.3300 -0.2469 0.1884 0.112 Uiso 1 1 calc R . . C13 C 0.4242(7) -0.2193(5) 0.2572(5) 0.107(3) Uani 1 1 d . . . H13 H 0.4167 -0.2691 0.2897 0.128 Uiso 1 1 calc R . . C14 C 0.4913(6) -0.1593(5) 0.2701(4) 0.096(2) Uani 1 1 d . . . H14 H 0.5313 -0.1703 0.3094 0.115 Uiso 1 1 calc R . . C15 C 0.4974(5) -0.0840(4) 0.2241(4) 0.0695(17) Uani 1 1 d . . . C16 C 0.4366(5) -0.0654(4) 0.1649(3) 0.0563(15) Uani 1 1 d . . . C17 C 0.5998(6) 0.3336(4) 0.0805(4) 0.096(2) Uani 1 1 d . . . H17A H 0.5551 0.3868 0.1031 0.115 Uiso 1 1 calc R . . H17B H 0.6485 0.3466 0.0272 0.115 Uiso 1 1 calc R . . C18 C 0.6746(6) 0.2925(5) 0.1303(5) 0.120(3) Uani 1 1 d . . . H18A H 0.6255 0.2784 0.1823 0.180 Uiso 1 1 calc R . . H18B H 0.7269 0.3310 0.1350 0.180 Uiso 1 1 calc R . . H18C H 0.7208 0.2411 0.1063 0.180 Uiso 1 1 calc R . . C19 C 0.6338(6) -0.0319(5) 0.2820(4) 0.107(2) Uani 1 1 d . . . H19A H 0.6920 -0.0828 0.2683 0.128 Uiso 1 1 calc R . . H19B H 0.5864 -0.0400 0.3366 0.128 Uiso 1 1 calc R . . C20 C 0.6957(6) 0.0448(5) 0.2747(4) 0.112(3) Uani 1 1 d . . . H20A H 0.7518 0.0474 0.2230 0.167 Uiso 1 1 calc R . . H20B H 0.7366 0.0405 0.3153 0.167 Uiso 1 1 calc R . . H20C H 0.6382 0.0958 0.2812 0.167 Uiso 1 1 calc R . . C36 C 0.3149(5) 0.3959(4) 0.2411(3) 0.0595(16) Uani 1 1 d . . . C35 C 0.3902(5) 0.3858(4) 0.2936(4) 0.0653(17) Uani 1 1 d . . . C34 C 0.4535(5) 0.4500(5) 0.2985(4) 0.090(2) Uani 1 1 d . . . H34 H 0.5029 0.4423 0.3321 0.107 Uiso 1 1 calc R . . C33 C 0.4432(7) 0.5261(5) 0.2532(5) 0.106(3) Uani 1 1 d . . . H33 H 0.4856 0.5693 0.2573 0.128 Uiso 1 1 calc R . . C32 C 0.3728(7) 0.5389(4) 0.2031(4) 0.090(2) Uani 1 1 d . . . H32 H 0.3676 0.5900 0.1728 0.108 Uiso 1 1 calc R . . C31 C 0.3076(5) 0.4740(4) 0.1975(4) 0.0655(17) Uani 1 1 d . . . C30 C 0.2340(6) 0.4888(4) 0.1449(4) 0.083(2) Uani 1 1 d . . . H30 H 0.2309 0.5422 0.1179 0.099 Uiso 1 1 calc R . . C29 C 0.1014(7) 0.4610(5) 0.0731(5) 0.121(3) Uani 1 1 d . . . H29A H 0.0451 0.5119 0.0909 0.145 Uiso 1 1 calc R . . H29B H 0.1543 0.4757 0.0218 0.145 Uiso 1 1 calc R . . C28 C 0.0378(8) 0.3946(5) 0.0631(5) 0.126(3) Uani 1 1 d . . . H28A H 0.0584 0.3822 0.0070 0.151 Uiso 1 1 calc R . . H28B H -0.0470 0.4140 0.0807 0.151 Uiso 1 1 calc R . . C27 C 0.0275(5) 0.2466(5) 0.1031(4) 0.075(2) Uani 1 1 d . . . H27 H -0.0185 0.2499 0.0676 0.090 Uiso 1 1 calc R . . C26 C 0.0462(5) 0.1658(5) 0.1441(4) 0.0655(17) Uani 1 1 d . . . C25 C -0.0018(5) 0.0951(5) 0.1287(4) 0.086(2) Uani 1 1 d . . . H25 H -0.0481 0.1024 0.0931 0.104 Uiso 1 1 calc R . . C24 C 0.0177(6) 0.0177(5) 0.1643(4) 0.088(2) Uani 1 1 d . . . H24 H -0.0131 -0.0281 0.1519 0.105 Uiso 1 1 calc R . . C23 C 0.0837(5) 0.0052(4) 0.2197(4) 0.0769(19) Uani 1 1 d . . . H23 H 0.0964 -0.0485 0.2445 0.092 Uiso 1 1 calc R . . C22 C 0.1303(5) 0.0737(4) 0.2377(4) 0.0609(16) Uani 1 1 d . . . C21 C 0.1136(5) 0.1554(4) 0.1992(3) 0.0572(15) Uani 1 1 d . . . C39 C 0.4753(5) 0.2863(5) 0.3810(4) 0.089(2) Uani 1 1 d . . . H39A H 0.4602 0.3269 0.4225 0.107 Uiso 1 1 calc R . . H39B H 0.5559 0.2868 0.3474 0.107 Uiso 1 1 calc R . . C40 C 0.4592(6) 0.1981(5) 0.4175(4) 0.108(2) Uani 1 1 d . . . H40A H 0.3799 0.1989 0.4520 0.161 Uiso 1 1 calc R . . H40B H 0.5153 0.1800 0.4480 0.161 Uiso 1 1 calc R . . H40C H 0.4721 0.1589 0.3760 0.161 Uiso 1 1 calc R . . C37 C 0.2043(6) -0.0052(4) 0.3406(4) 0.082(2) Uani 1 1 d . . . H37A H 0.2424 -0.0541 0.3083 0.098 Uiso 1 1 calc R . . H37B H 0.1259 -0.0161 0.3720 0.098 Uiso 1 1 calc R . . C38 C 0.2783(6) 0.0102(4) 0.3946(4) 0.103(2) Uani 1 1 d . . . H38A H 0.3528 0.0260 0.3626 0.154 Uiso 1 1 calc R . . H38B H 0.2924 -0.0412 0.4260 0.154 Uiso 1 1 calc R . . H38C H 0.2364 0.0557 0.4292 0.154 Uiso 1 1 calc R . . C41 C 0.7804(5) 0.6050(4) 0.4813(3) 0.0534(14) Uani 1 1 d . . . C42 C 0.7604(5) 0.6804(4) 0.4333(3) 0.0664(17) Uani 1 1 d . . . C43 C 0.6780(6) 0.6868(5) 0.3907(4) 0.096(2) Uani 1 1 d . . . H43 H 0.6660 0.7359 0.3589 0.115 Uiso 1 1 calc R . . C44 C 0.6119(7) 0.6198(6) 0.3949(5) 0.111(3) Uani 1 1 d . . . H44 H 0.5525 0.6261 0.3689 0.133 Uiso 1 1 calc R . . C45 C 0.6343(6) 0.5464(5) 0.4363(4) 0.094(2) Uani 1 1 d . . . H45 H 0.5929 0.5012 0.4364 0.112 Uiso 1 1 calc R . . C46 C 0.7192(5) 0.5369(4) 0.4795(3) 0.0649(16) Uani 1 1 d . . . C47 C 0.7485(5) 0.4549(4) 0.5168(4) 0.0679(17) Uani 1 1 d . . . H47 H 0.7103 0.4101 0.5106 0.082 Uiso 1 1 calc R . . C48 C 0.8623(6) 0.3498(3) 0.5825(4) 0.0782(19) Uani 1 1 d . . . H48A H 0.8006 0.3147 0.5869 0.094 Uiso 1 1 calc R . . H48B H 0.9337 0.3257 0.5434 0.094 Uiso 1 1 calc R . . C49 C 0.8857(5) 0.3526(4) 0.6605(4) 0.0797(19) Uani 1 1 d . . . H49A H 0.8119 0.3573 0.7029 0.096 Uiso 1 1 calc R . . H49B H 0.9367 0.3010 0.6709 0.096 Uiso 1 1 calc R . . C50 C 1.0160(5) 0.4294(4) 0.6988(3) 0.0691(18) Uani 1 1 d . . . H50 H 1.0300 0.3797 0.7295 0.083 Uiso 1 1 calc R . . C51 C 1.0753(5) 0.4982(4) 0.7044(3) 0.0627(16) Uani 1 1 d . . . C52 C 1.1559(6) 0.4878(5) 0.7516(4) 0.084(2) Uani 1 1 d . . . H52 H 1.1695 0.4357 0.7789 0.101 Uiso 1 1 calc R . . C53 C 1.2133(6) 0.5532(5) 0.7570(4) 0.092(2) Uani 1 1 d . . . H53 H 1.2665 0.5454 0.7880 0.110 Uiso 1 1 calc R . . C54 C 1.1942(5) 0.6313(5) 0.7172(4) 0.083(2) Uani 1 1 d . . . H54 H 1.2334 0.6760 0.7223 0.100 Uiso 1 1 calc R . . C55 C 1.1175(5) 0.6429(4) 0.6704(3) 0.0605(15) Uani 1 1 d . . . C56 C 1.0546(5) 0.5767(4) 0.6620(3) 0.0555(15) Uani 1 1 d . . . C57 C 0.8170(6) 0.8181(4) 0.3865(4) 0.098(2) Uani 1 1 d . . . H57A H 0.7372 0.8491 0.4039 0.118 Uiso 1 1 calc R . . H57B H 0.8329 0.8049 0.3309 0.118 Uiso 1 1 calc R . . C58 C 0.9062(7) 0.8710(4) 0.3960(4) 0.117(3) Uani 1 1 d . . . H58A H 0.8976 0.8759 0.4518 0.175 Uiso 1 1 calc R . . H58B H 0.8930 0.9272 0.3715 0.175 Uiso 1 1 calc R . . H59C H 0.9850 0.8438 0.3708 0.175 Uiso 1 1 calc R . . C59 C 1.1523(6) 0.7873(4) 0.6304(4) 0.091(2) Uani 1 1 d . . . H59A H 1.2378 0.7707 0.6140 0.110 Uiso 1 1 calc R . . H59B H 1.1293 0.8066 0.6845 0.110 Uiso 1 1 calc R . . C60 C 1.1160(6) 0.8569(4) 0.5755(4) 0.112(3) Uani 1 1 d . . . H60A H 1.1426 0.8381 0.5218 0.167 Uiso 1 1 calc R . . H60B H 1.1510 0.9068 0.5785 0.167 Uiso 1 1 calc R . . H60C H 1.0310 0.8710 0.5909 0.167 Uiso 1 1 calc R . . Cl1 Cl 0.03941(18) 0.75022(12) 0.12027(12) 0.0754(5) Uani 1 1 d . . . H10C H 0.170(5) 0.266(3) 0.423(3) 0.12(3) Uiso 1 1 d D . . H9C H 0.440(5) 0.1108(11) 0.210(3) 0.08(2) Uiso 1 1 d D . . H10D H 0.093(3) 0.256(3) 0.386(3) 0.10(3) Uiso 1 1 d D . . H9D H 0.437(7) 0.190(3) 0.1816(18) 0.15(4) Uiso 1 1 d D . . Li1 Li 0.2695(8) 0.2136(5) 0.2894(5) 0.058(2) Uani 1 1 d . . . N1 N 0.2861(4) 0.0928(3) -0.0272(3) 0.0587(12) Uani 1 1 d . . . N2 N 0.3210(4) -0.0530(3) 0.0382(3) 0.0585(12) Uani 1 1 d . . . N4 N 0.1710(5) 0.4358(3) 0.1306(3) 0.0722(15) Uani 1 1 d . . . N3 N 0.0678(4) 0.3155(4) 0.1102(3) 0.0674(14) Uani 1 1 d . . . N5 N 0.8236(4) 0.4393(3) 0.5579(3) 0.0597(13) Uani 1 1 d . . . N6 N 0.9445(4) 0.4283(3) 0.6556(3) 0.0595(13) Uani 1 1 d . . . Ni1 Ni 0.36517(5) 0.05061(4) 0.04816(4) 0.0519(2) Uani 1 1 d . . . Ni2 Ni 0.16358(6) 0.32592(4) 0.17324(4) 0.0573(2) Uani 1 1 d . . . Ni3 Ni 0.90139(6) 0.51597(4) 0.58838(4) 0.0510(2) Uani 1 1 d . . . O1 O 0.4142(3) 0.1534(2) 0.0559(2) 0.0555(9) Uani 1 1 d . . . O2 O 0.4413(3) 0.0098(2) 0.12576(19) 0.0526(9) Uani 1 1 d . . . O3 O 0.5601(3) -0.0198(3) 0.2303(2) 0.0780(12) Uani 1 1 d . . . O4 O 0.5211(4) 0.2760(2) 0.0772(3) 0.0784(12) Uani 1 1 d . . . O6 O 0.2609(3) 0.3318(2) 0.23698(19) 0.0560(10) Uani 1 1 d . . . O5 O 0.1596(3) 0.2174(2) 0.21893(19) 0.0563(9) Uani 1 1 d . . . O8 O 0.3920(3) 0.3090(3) 0.3343(2) 0.0698(11) Uani 1 1 d . . . O7 O 0.1958(3) 0.0704(2) 0.2915(2) 0.0698(11) Uani 1 1 d . . . O10 O 0.1538(4) 0.2323(3) 0.3964(3) 0.0654(10) Uani 1 1 d D . . O9 O 0.4258(4) 0.1603(3) 0.2233(3) 0.0640(10) Uani 1 1 d D . . O11 O 0.8567(3) 0.6047(2) 0.5227(2) 0.0539(9) Uani 1 1 d . . . O12 O 0.9826(3) 0.5928(2) 0.6159(2) 0.0564(9) Uani 1 1 d . . . O13 O 0.8283(4) 0.7414(3) 0.4344(2) 0.0749(12) Uani 1 1 d . . . O14 O 1.0939(3) 0.7167(3) 0.6264(2) 0.0717(11) Uani 1 1 d . . . O15A O 0.0572(19) 0.8097(12) 0.0580(11) 0.127(8) Uani 0.60 1 d P A . O16A O -0.003(2) 0.6803(11) 0.1031(14) 0.167(11) Uani 0.60 1 d P A . O15B O 0.030(3) 0.8196(15) 0.065(2) 0.134(13) Uani 0.40 1 d P A . O16B O -0.056(3) 0.710(3) 0.134(3) 0.21(2) Uani 0.40 1 d P A . O17A O 0.143(2) 0.6974(12) 0.0985(18) 0.230(11) Uani 0.60 1 d P A 1 O18A O -0.047(2) 0.7851(13) 0.1827(9) 0.189(7) Uani 0.60 1 d P A 1 O17B O 0.134(2) 0.7220(19) 0.1479(16) 0.118(10) Uani 0.40 1 d P A 2 O18B O 0.064(4) 0.7819(17) 0.1878(12) 0.145(10) Uani 0.40 1 d P A 2 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 C1 0.051(4) 0.058(4) 0.056(4) -0.001(3) -0.003(3) 0.000(3) C2 0.064(4) 0.049(4) 0.067(5) 0.001(3) 0.002(3) -0.007(3) C3 0.084(5) 0.062(5) 0.103(6) 0.005(4) 0.004(4) -0.014(4) C4 0.105(7) 0.074(6) 0.103(7) 0.028(5) 0.000(5) 0.007(5) C5 0.088(5) 0.096(6) 0.079(5) 0.028(5) -0.018(4) 0.016(5) C6 0.057(4) 0.064(4) 0.063(4) 0.001(4) -0.008(3) 0.004(3) C7 0.059(4) 0.100(6) 0.060(4) 0.001(4) -0.014(3) 0.008(4) C8 0.064(4) 0.122(6) 0.076(5) -0.013(4) -0.028(4) -0.024(4) C9 0.076(4) 0.094(5) 0.066(4) -0.021(4) -0.023(4) -0.036(4) C10 0.062(4) 0.062(4) 0.079(5) -0.022(4) 0.001(4) -0.016(3) C11 0.056(4) 0.049(4) 0.069(5) 0.002(3) 0.000(3) -0.008(3) C12 0.099(6) 0.058(5) 0.108(6) 0.012(4) -0.013(5) -0.007(4) C13 0.126(7) 0.057(5) 0.124(7) 0.029(5) -0.023(6) -0.014(5) C14 0.102(5) 0.085(5) 0.097(6) 0.033(5) -0.044(5) 0.007(4) C15 0.064(4) 0.066(4) 0.075(5) 0.003(4) -0.024(4) 0.006(3) C16 0.043(3) 0.047(4) 0.068(4) 0.002(3) -0.004(3) 0.001(3) C17 0.085(5) 0.079(5) 0.120(6) -0.015(4) -0.010(5) -0.028(4) C18 0.109(6) 0.125(7) 0.146(7) -0.044(6) -0.050(6) -0.031(5) C19 0.092(5) 0.145(7) 0.090(6) -0.002(5) -0.053(5) 0.013(5) C20 0.077(5) 0.173(8) 0.100(6) -0.035(5) -0.044(4) -0.013(5) C36 0.060(4) 0.044(4) 0.059(4) 0.003(3) 0.006(3) -0.007(3) C35 0.064(4) 0.059(4) 0.068(5) -0.013(4) -0.005(4) -0.014(3) C34 0.074(5) 0.085(5) 0.105(6) -0.029(5) 0.000(4) -0.030(4) C33 0.114(7) 0.077(6) 0.118(8) -0.035(5) 0.012(5) -0.050(5) C32 0.104(6) 0.057(4) 0.094(6) -0.018(4) 0.016(5) -0.033(4) C31 0.067(4) 0.048(4) 0.070(5) -0.007(3) 0.003(4) -0.010(3) C30 0.086(5) 0.054(4) 0.075(5) 0.014(4) 0.018(4) 0.001(4) C29 0.142(8) 0.114(7) 0.091(6) 0.018(5) -0.037(6) 0.025(6) C28 0.156(8) 0.125(8) 0.103(6) 0.015(6) -0.076(6) 0.025(6) C27 0.052(4) 0.115(6) 0.058(4) -0.020(4) -0.019(3) 0.005(4) C26 0.048(4) 0.091(5) 0.061(4) -0.017(4) -0.014(3) -0.011(3) C25 0.060(4) 0.118(6) 0.086(5) -0.036(5) -0.019(4) -0.012(4) C24 0.073(5) 0.095(6) 0.100(6) -0.033(5) -0.015(4) -0.030(4) C23 0.065(4) 0.075(5) 0.083(5) -0.009(4) -0.002(4) -0.022(4) C22 0.050(4) 0.065(4) 0.064(4) -0.017(4) 0.001(3) -0.020(3) C21 0.047(3) 0.069(4) 0.054(4) -0.015(3) -0.007(3) -0.012(3) C39 0.062(4) 0.137(7) 0.076(5) -0.021(5) -0.027(4) -0.014(4) C40 0.108(6) 0.119(6) 0.093(6) 0.013(5) -0.041(5) 0.009(5) C37 0.092(5) 0.058(4) 0.080(5) 0.022(4) -0.005(4) -0.014(4) C38 0.142(7) 0.083(5) 0.078(5) 0.022(4) -0.035(5) -0.007(5) C41 0.046(3) 0.061(4) 0.048(4) -0.010(3) -0.005(3) -0.002(3) C42 0.071(4) 0.072(5) 0.061(4) -0.004(4) -0.033(4) 0.000(4) C43 0.098(6) 0.109(6) 0.090(6) -0.006(4) -0.056(5) 0.012(5) C44 0.083(5) 0.159(9) 0.108(7) -0.019(6) -0.059(5) 0.001(6) C45 0.073(5) 0.122(7) 0.098(6) -0.028(5) -0.038(4) -0.014(5) C46 0.048(4) 0.082(5) 0.065(4) -0.010(4) -0.012(3) -0.014(3) C47 0.063(4) 0.067(4) 0.073(5) -0.019(4) -0.004(4) -0.028(3) C48 0.101(5) 0.049(4) 0.077(5) 0.000(3) -0.008(4) -0.022(3) C49 0.088(5) 0.062(4) 0.079(5) 0.016(4) -0.011(4) -0.017(4) C50 0.065(4) 0.074(5) 0.053(4) 0.015(3) -0.006(3) 0.006(4) C51 0.055(4) 0.071(4) 0.058(4) -0.001(3) -0.010(3) -0.005(3) C52 0.081(5) 0.100(6) 0.074(5) -0.002(4) -0.034(4) 0.005(4) C53 0.077(5) 0.117(7) 0.087(5) -0.005(5) -0.040(4) 0.004(5) C54 0.066(4) 0.113(6) 0.081(5) -0.009(4) -0.035(4) -0.015(4) C55 0.050(3) 0.071(4) 0.057(4) -0.008(3) -0.009(3) -0.005(3) C56 0.048(3) 0.064(4) 0.052(4) -0.010(3) -0.008(3) -0.006(3) C57 0.127(6) 0.081(5) 0.067(5) 0.018(4) -0.020(5) 0.016(5) C58 0.151(7) 0.064(5) 0.112(6) 0.023(4) -0.011(6) -0.012(5) C59 0.085(5) 0.092(5) 0.104(6) -0.009(5) -0.020(4) -0.037(4) C60 0.129(6) 0.079(5) 0.132(7) -0.015(5) -0.022(5) -0.050(5) Cl1 0.0893(13) 0.0714(12) 0.0749(14) 0.0135(11) -0.0354(12) -0.0243(11) Li1 0.067(6) 0.054(6) 0.049(6) 0.003(4) -0.009(5) -0.012(5) N1 0.050(3) 0.078(4) 0.048(3) -0.005(3) -0.016(2) -0.005(3) N2 0.048(3) 0.065(3) 0.063(3) -0.010(3) -0.010(3) -0.016(2) N4 0.077(4) 0.069(4) 0.051(3) 0.018(3) -0.008(3) 0.019(3) N3 0.058(3) 0.089(4) 0.051(3) -0.002(3) -0.018(3) 0.007(3) N5 0.058(3) 0.058(3) 0.060(3) -0.002(2) -0.005(3) -0.020(2) N6 0.060(3) 0.048(3) 0.064(3) 0.007(2) -0.011(3) -0.008(2) Ni1 0.0457(4) 0.0570(5) 0.0523(5) -0.0054(3) -0.0111(4) -0.0087(3) Ni2 0.0567(5) 0.0607(5) 0.0500(5) 0.0037(4) -0.0141(4) -0.0003(4) Ni3 0.0497(4) 0.0484(4) 0.0515(5) 0.0000(3) -0.0082(4) -0.0093(3) O1 0.062(2) 0.051(2) 0.058(2) 0.0039(19) -0.022(2) -0.0141(18) O2 0.053(2) 0.048(2) 0.059(2) 0.0000(18) -0.0185(19) -0.0095(17) O3 0.074(3) 0.089(3) 0.083(3) 0.012(2) -0.048(2) -0.010(2) O4 0.084(3) 0.067(3) 0.088(3) 0.001(2) -0.020(3) -0.034(2) O6 0.060(2) 0.047(2) 0.065(3) 0.0068(18) -0.023(2) -0.0134(18) O5 0.063(2) 0.055(2) 0.059(2) -0.0018(19) -0.026(2) -0.0129(19) O8 0.068(3) 0.067(3) 0.084(3) -0.009(2) -0.029(2) -0.019(2) O7 0.081(3) 0.057(3) 0.077(3) 0.011(2) -0.026(2) -0.025(2) O10 0.069(3) 0.060(3) 0.072(3) -0.001(2) -0.029(2) -0.011(2) O9 0.071(3) 0.052(3) 0.067(3) -0.001(2) -0.018(2) -0.008(2) O11 0.057(2) 0.054(2) 0.056(2) 0.0062(18) -0.022(2) -0.0146(18) O12 0.056(2) 0.054(2) 0.064(3) -0.0020(19) -0.022(2) -0.0118(18) O13 0.100(3) 0.062(3) 0.068(3) 0.012(2) -0.038(2) -0.008(2) O14 0.067(3) 0.071(3) 0.087(3) 0.000(2) -0.030(2) -0.025(2) O15A 0.188(14) 0.153(17) 0.064(10) 0.075(10) -0.048(9) -0.111(12) O16A 0.28(3) 0.087(8) 0.212(18) 0.019(9) -0.15(2) -0.102(13) O15B 0.24(3) 0.038(10) 0.17(3) 0.026(12) -0.15(2) 0.006(13) O16B 0.089(14) 0.28(5) 0.29(5) 0.19(4) -0.10(2) -0.13(2) O17A 0.155(17) 0.098(11) 0.38(3) -0.008(16) -0.004(18) 0.031(11) O18A 0.238(18) 0.177(15) 0.100(11) -0.017(9) 0.003(12) 0.037(14) O17B 0.13(2) 0.12(2) 0.16(2) 0.031(15) -0.13(2) -0.041(16) O18B 0.30(3) 0.117(15) 0.069(11) -0.003(9) -0.114(17) -0.076(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 C1 O1 1.308(6) . ? C1 C2 1.400(7) . ? C1 C6 1.402(7) . ? C2 O4 1.364(7) . ? C2 C3 1.373(8) . ? C3 C4 1.380(9) . ? C4 C5 1.364(9) . ? C5 C6 1.413(8) . ? C6 C7 1.417(8) . ? C7 N1 1.295(7) . ? C8 N1 1.480(6) . ? C8 C9 1.495(7) . ? C9 N2 1.455(6) . ? C10 N2 1.280(7) . ? C10 C11 1.418(8) . ? C11 C12 1.397(8) . ? C11 C16 1.409(7) . ? C12 C13 1.344(9) . ? C13 C14 1.404(9) . ? C14 C15 1.376(8) . ? C15 O3 1.379(7) . ? C15 C16 1.408(7) . ? C16 O2 1.319(6) . ? C17 O4 1.422(6) . ? C17 C18 1.455(8) . ? C19 O3 1.408(6) . ? C19 C20 1.494(8) . ? C36 O6 1.300(6) . ? C36 C31 1.395(7) . ? C36 C35 1.436(8) . ? C35 O8 1.352(6) . ? C35 C34 1.377(7) . ? C34 C33 1.389(9) . ? C33 C32 1.354(9) . ? C32 C31 1.407(8) . ? C31 C30 1.420(8) . ? C30 N4 1.293(7) . ? C29 C28 1.437(9) . ? C29 N4 1.466(8) . ? C28 N3 1.487(8) . ? C27 N3 1.286(7) . ? C27 C26 1.425(8) . ? C26 C21 1.400(7) . ? C26 C25 1.413(8) . ? C25 C24 1.339(8) . ? C24 C23 1.392(8) . ? C23 C22 1.389(7) . ? C22 O7 1.373(6) . ? C22 C21 1.414(7) . ? C21 O5 1.311(6) . ? C39 O8 1.437(6) . ? C39 C40 1.499(8) . ? C37 O7 1.415(6) . ? C37 C38 1.517(8) . ? C41 O11 1.309(6) . ? C41 C46 1.400(7) . ? C41 C42 1.423(7) . ? C42 O13 1.358(6) . ? C42 C43 1.375(8) . ? C43 C44 1.402(9) . ? C44 C45 1.342(9) . ? C45 C46 1.405(8) . ? C46 C47 1.434(8) . ? C47 N5 1.278(6) . ? C48 C49 1.472(7) . ? C48 N5 1.480(6) . ? C49 N6 1.464(6) . ? C50 N6 1.290(6) . ? C50 C51 1.413(7) . ? C51 C56 1.411(7) . ? C51 C52 1.412(8) . ? C52 C53 1.351(8) . ? C53 C54 1.381(8) . ? C54 C55 1.370(7) . ? C55 O14 1.373(6) . ? C55 C56 1.421(7) . ? C56 O12 1.314(6) . ? C57 O13 1.422(6) . ? C57 C58 1.503(8) . ? C59 O14 1.423(6) . ? C59 C60 1.487(8) . ? Cl1 O16B 1.34(2) . ? Cl1 O17A 1.346(18) . ? Cl1 O18A 1.351(14) . ? Cl1 O17B 1.340(17) . ? Cl1 O15A 1.366(14) . ? Cl1 O16A 1.376(13) . ? Cl1 O15B 1.41(2) . ? Cl1 O18B 1.443(14) . ? Li1 O9 1.983(9) . ? Li1 O10 1.993(9) . ? Li1 O6 2.008(9) . ? Li1 O5 2.024(10) . ? Li1 O7 2.549(9) . ? Li1 O8 2.565(10) . ? Li1 Ni2 2.991(9) . ? N1 Ni1 1.847(4) . ? N2 Ni1 1.836(5) . ? N4 Ni2 1.834(5) . ? N3 Ni2 1.827(5) . ? N5 Ni3 1.834(5) . ? N6 Ni3 1.840(5) . ? Ni1 O1 1.840(3) . ? Ni1 O2 1.851(3) . ? Ni2 O5 1.829(3) . ? Ni2 O6 1.836(3) . ? Ni3 O12 1.839(3) . ? Ni3 O11 1.841(3) . ? O16A O16B 0.81(5) . ? O16A O17A 1.78(3) . ? O16B O18A 1.56(4) . ? O17B O18B 1.26(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 C1 C2 118.3(6) . . ? O1 C1 C6 124.6(6) . . ? C2 C1 C6 117.1(6) . . ? O4 C2 C3 123.7(7) . . ? O4 C2 C1 114.5(6) . . ? C3 C2 C1 121.8(7) . . ? C2 C3 C4 119.8(7) . . ? C5 C4 C3 121.2(7) . . ? C4 C5 C6 119.0(7) . . ? C1 C6 C5 121.0(7) . . ? C1 C6 C7 120.5(6) . . ? C5 C6 C7 118.5(7) . . ? N1 C7 C6 126.3(6) . . ? N1 C8 C9 106.1(5) . . ? N2 C9 C8 107.1(5) . . ? N2 C10 C11 126.1(6) . . ? C12 C11 C16 119.9(7) . . ? C12 C11 C10 119.4(7) . . ? C16 C11 C10 120.5(6) . . ? C13 C12 C11 121.2(7) . . ? C12 C13 C14 120.3(7) . . ? C15 C14 C13 119.4(7) . . ? C14 C15 O3 125.4(7) . . ? C14 C15 C16 121.3(7) . . ? O3 C15 C16 113.3(6) . . ? O2 C16 C15 118.2(6) . . ? O2 C16 C11 124.2(6) . . ? C15 C16 C11 117.6(6) . . ? O4 C17 C18 107.8(6) . . ? O3 C19 C20 109.4(6) . . ? O6 C36 C31 125.5(6) . . ? O6 C36 C35 117.9(5) . . ? C31 C36 C35 116.6(6) . . ? O8 C35 C34 125.8(7) . . ? O8 C35 C36 113.3(5) . . ? C34 C35 C36 120.9(6) . . ? C35 C34 C33 119.9(7) . . ? C32 C33 C34 121.4(8) . . ? C33 C32 C31 119.3(7) . . ? C36 C31 C32 121.9(7) . . ? C36 C31 C30 119.8(6) . . ? C32 C31 C30 118.4(7) . . ? N4 C30 C31 126.7(6) . . ? C28 C29 N4 112.8(7) . . ? C29 C28 N3 110.3(7) . . ? N3 C27 C26 126.7(6) . . ? C21 C26 C25 119.3(6) . . ? C21 C26 C27 120.4(6) . . ? C25 C26 C27 120.2(7) . . ? C24 C25 C26 121.6(7) . . ? C25 C24 C23 120.6(7) . . ? C22 C23 C24 119.6(7) . . ? O7 C22 C23 125.5(6) . . ? O7 C22 C21 113.7(5) . . ? C23 C22 C21 120.8(6) . . ? O5 C21 C26 124.0(6) . . ? O5 C21 C22 117.8(6) . . ? C26 C21 C22 118.2(6) . . ? O8 C39 C40 107.1(5) . . ? O7 C37 C38 106.3(5) . . ? O11 C41 C46 125.3(5) . . ? O11 C41 C42 116.8(5) . . ? C46 C41 C42 117.9(6) . . ? O13 C42 C43 125.5(6) . . ? O13 C42 C41 114.4(5) . . ? C43 C42 C41 120.1(7) . . ? C42 C43 C44 120.4(7) . . ? C45 C44 C43 120.1(7) . . ? C44 C45 C46 121.0(7) . . ? C41 C46 C45 120.1(6) . . ? C41 C46 C47 120.5(6) . . ? C45 C46 C47 119.3(7) . . ? N5 C47 C46 124.5(6) . . ? C49 C48 N5 106.9(5) . . ? N6 C49 C48 106.1(5) . . ? N6 C50 C51 126.7(6) . . ? C56 C51 C52 120.5(6) . . ? C56 C51 C50 119.6(6) . . ? C52 C51 C50 119.9(6) . . ? C53 C52 C51 120.3(7) . . ? C52 C53 C54 121.0(7) . . ? C55 C54 C53 120.0(7) . . ? C54 C55 O14 125.3(6) . . ? C54 C55 C56 121.8(6) . . ? O14 C55 C56 112.9(5) . . ? O12 C56 C51 125.4(6) . . ? O12 C56 C55 118.2(5) . . ? C51 C56 C55 116.5(6) . . ? O13 C57 C58 106.9(6) . . ? O14 C59 C60 107.2(6) . . ? O16B Cl1 O17A 113.2(19) . . ? O16B Cl1 O18A 70.7(17) . . ? O17A Cl1 O18A 145.0(12) . . ? O16B Cl1 O17B 124.1(17) . . ? O17A Cl1 O17B 41.4(11) . . ? O18A Cl1 O17B 105.9(12) . . ? O16B Cl1 O15A 117.9(18) . . ? O17A Cl1 O15A 99.6(14) . . ? O18A Cl1 O15A 109.0(11) . . ? O17B Cl1 O15A 115.5(14) . . ? O16B Cl1 O16A 35(2) . . ? O17A Cl1 O16A 81.5(12) . . ? O18A Cl1 O16A 104.9(12) . . ? O17B Cl1 O16A 108.4(13) . . ? O15A Cl1 O16A 112.3(14) . . ? O16B Cl1 O15B 109(2) . . ? O17A Cl1 O15B 112.8(17) . . ? O18A Cl1 O15B 96.9(14) . . ? O17B Cl1 O15B 126.0(18) . . ? O15A Cl1 O15B 13(2) . . ? O16A Cl1 O15B 111.8(17) . . ? O16B Cl1 O18B 118(2) . . ? O17A Cl1 O18B 95.0(13) . . ? O18A Cl1 O18B 56.9(10) . . ? O17B Cl1 O18B 53.9(11) . . ? O15A Cl1 O18B 109.6(12) . . ? O16A Cl1 O18B 137.9(12) . . ? O15B Cl1 O18B 108.1(17) . . ? O9 Li1 O10 149.7(5) . . ? O9 Li1 O6 100.2(4) . . ? O10 Li1 O6 102.3(4) . . ? O9 Li1 O5 104.1(4) . . ? O10 Li1 O5 101.6(4) . . ? O6 Li1 O5 73.6(3) . . ? O9 Li1 O7 87.5(3) . . ? O10 Li1 O7 87.7(3) . . ? O6 Li1 O7 141.1(5) . . ? O5 Li1 O7 67.6(3) . . ? O9 Li1 O8 84.5(3) . . ? O10 Li1 O8 85.6(3) . . ? O6 Li1 O8 67.5(3) . . ? O5 Li1 O8 141.1(4) . . ? O7 Li1 O8 151.4(4) . . ? O9 Li1 Ni2 104.3(3) . . ? O10 Li1 Ni2 105.9(4) . . ? O6 Li1 Ni2 36.87(18) . . ? O5 Li1 Ni2 36.78(18) . . ? O7 Li1 Ni2 104.3(3) . . ? O8 Li1 Ni2 104.3(3) . . ? C7 N1 C8 119.6(6) . . ? C7 N1 Ni1 126.3(5) . . ? C8 N1 Ni1 114.0(4) . . ? C10 N2 C9 120.0(5) . . ? C10 N2 Ni1 126.6(5) . . ? C9 N2 Ni1 113.4(4) . . ? C30 N4 C29 119.6(7) . . ? C30 N4 Ni2 125.9(5) . . ? C29 N4 Ni2 114.4(5) . . ? C27 N3 C28 119.2(6) . . ? C27 N3 Ni2 125.7(5) . . ? C28 N3 Ni2 115.1(5) . . ? C47 N5 C48 120.1(5) . . ? C47 N5 Ni3 127.7(4) . . ? C48 N5 Ni3 112.1(4) . . ? C50 N6 C49 119.3(5) . . ? C50 N6 Ni3 126.5(4) . . ? C49 N6 Ni3 114.2(4) . . ? N2 Ni1 O1 178.14(16) . . ? N2 Ni1 N1 85.9(2) . . ? O1 Ni1 N1 94.41(19) . . ? N2 Ni1 O2 94.56(19) . . ? O1 Ni1 O2 85.20(15) . . ? N1 Ni1 O2 178.52(16) . . ? N3 Ni2 O5 95.4(2) . . ? N3 Ni2 N4 87.1(3) . . ? O5 Ni2 N4 177.4(2) . . ? N3 Ni2 O6 177.8(2) . . ? O5 Ni2 O6 82.48(15) . . ? N4 Ni2 O6 95.0(2) . . ? N3 Ni2 Li1 136.8(2) . . ? O5 Ni2 Li1 41.5(2) . . ? N4 Ni2 Li1 136.0(3) . . ? O6 Ni2 Li1 41.02(19) . . ? N5 Ni3 O12 178.29(17) . . ? N5 Ni3 N6 85.9(2) . . ? O12 Ni3 N6 94.8(2) . . ? N5 Ni3 O11 94.52(19) . . ? O12 Ni3 O11 84.87(16) . . ? N6 Ni3 O11 178.99(17) . . ? C1 O1 Ni1 127.7(4) . . ? C16 O2 Ni1 126.4(4) . . ? C15 O3 C19 120.0(5) . . ? C2 O4 C17 119.2(5) . . ? C36 O6 Ni2 127.1(4) . . ? C36 O6 Li1 130.7(4) . . ? Ni2 O6 Li1 102.1(3) . . ? C21 O5 Ni2 127.3(4) . . ? C21 O5 Li1 130.0(4) . . ? Ni2 O5 Li1 101.7(3) . . ? C35 O8 C39 118.9(5) . . ? C35 O8 Li1 110.5(4) . . ? C39 O8 Li1 129.3(4) . . ? C22 O7 C37 117.9(5) . . ? C22 O7 Li1 110.4(4) . . ? C37 O7 Li1 131.5(4) . . ? C41 O11 Ni3 126.3(3) . . ? C56 O12 Ni3 126.7(3) . . ? C42 O13 C57 118.5(5) . . ? C55 O14 C59 117.7(5) . . ? O16B O16A Cl1 70(2) . . ? O16B O16A O17A 115(3) . . ? Cl1 O16A O17A 48.5(7) . . ? O16A O16B Cl1 75(2) . . ? O16A O16B O18A 129(3) . . ? Cl1 O16B O18A 55.0(12) . . ? Cl1 O17A O16A 50.0(9) . . ? Cl1 O18A O16B 54.3(11) . . ? O18B O17B Cl1 67.2(13) . . ? O17B O18B Cl1 58.9(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.257 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.061 #END=== data_10 _database_code_depnum_ccdc_archive 'CCDC 813956' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 F6 N5 Ni2 O8 P' _chemical_formula_weight 989.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 15.934(3) _cell_length_b 14.920(2) _cell_length_c 18.255(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.114(6) _cell_angle_gamma 90.00 _cell_volume 4337.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.50 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8270 _exptl_absorpt_correction_T_max 0.8580 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 80861 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 32.70 _reflns_number_total 15792 _reflns_number_gt 9657 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5249P] 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 15792 _refine_ls_number_parameters 579 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.002 _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 C1 C 0.49742(12) 0.52696(12) 0.65361(10) 0.0414(4) Uani 1 1 d . . . C2 C 0.52486(14) 0.47779(14) 0.71648(11) 0.0508(5) Uani 1 1 d . . . C3 C 0.47081(19) 0.46056(18) 0.77271(14) 0.0703(7) Uani 1 1 d . . . H3 H 0.4897 0.4288 0.8139 0.084 Uiso 1 1 calc R . . C4 C 0.38823(19) 0.4910(2) 0.76717(16) 0.0779(8) Uani 1 1 d . . . H4 H 0.3524 0.4802 0.8053 0.094 Uiso 1 1 calc R . . C5 C 0.35942(17) 0.53600(19) 0.70724(16) 0.0694(7) Uani 1 1 d . . . H5 H 0.3039 0.5553 0.7045 0.083 Uiso 1 1 calc R . . C6 C 0.41249(13) 0.55422(14) 0.64855(12) 0.0488(5) Uani 1 1 d . . . C7 C 0.37854(13) 0.59491(14) 0.58286(13) 0.0497(5) Uani 1 1 d . . . H7 H 0.3212 0.6065 0.5803 0.060 Uiso 1 1 calc R . . C8 C 0.37756(13) 0.64858(15) 0.45969(12) 0.0536(5) Uani 1 1 d . . . H8A H 0.3250 0.6775 0.4708 0.064 Uiso 1 1 calc R . . H8B H 0.3656 0.5989 0.4266 0.064 Uiso 1 1 calc R . . C9 C 0.43563(14) 0.71381(15) 0.42574(13) 0.0564(5) Uani 1 1 d . . . H9A H 0.4204 0.7220 0.3742 0.068 Uiso 1 1 calc R . . H9B H 0.4329 0.7715 0.4501 0.068 Uiso 1 1 calc R . . C10 C 0.57683(15) 0.69611(14) 0.38817(11) 0.0525(5) Uani 1 1 d . . . H10 H 0.5603 0.7326 0.3490 0.063 Uiso 1 1 calc R . . C11 C 0.66240(14) 0.66698(14) 0.39211(10) 0.0493(5) Uani 1 1 d . . . C12 C 0.71572(19) 0.68908(19) 0.33434(13) 0.0692(7) Uani 1 1 d . . . H12 H 0.6955 0.7244 0.2956 0.083 Uiso 1 1 calc R . . C13 C 0.7959(2) 0.6591(2) 0.33512(14) 0.0808(9) Uani 1 1 d . . . H13 H 0.8302 0.6737 0.2967 0.097 Uiso 1 1 calc R . . C14 C 0.82748(17) 0.6070(2) 0.39237(14) 0.0703(7) Uani 1 1 d . . . H14 H 0.8826 0.5866 0.3921 0.084 Uiso 1 1 calc R . . C15 C 0.77728(14) 0.58509(16) 0.45042(11) 0.0510(5) Uani 1 1 d . . . C16 C 0.69329(12) 0.61482(13) 0.45157(10) 0.0408(4) Uani 1 1 d . . . C17 C 0.63466(19) 0.37833(18) 0.76126(13) 0.0687(7) Uani 1 1 d . . . H17A H 0.5954 0.3288 0.7564 0.082 Uiso 1 1 calc R . . H17B H 0.6380 0.3970 0.8122 0.082 Uiso 1 1 calc R . . C18 C 0.7186(2) 0.3507(2) 0.73708(15) 0.0793(8) Uani 1 1 d . . . H18A H 0.7152 0.3362 0.6858 0.119 Uiso 1 1 calc R . . H18B H 0.7373 0.2991 0.7645 0.119 Uiso 1 1 calc R . . H18C H 0.7577 0.3990 0.7452 0.119 Uiso 1 1 calc R . . C19 C 0.88463(15) 0.4982(2) 0.51385(16) 0.0720(7) Uani 1 1 d . . . H19A H 0.9245 0.5469 0.5204 0.086 Uiso 1 1 calc R . . H19B H 0.8970 0.4665 0.4692 0.086 Uiso 1 1 calc R . . C20 C 0.89107(19) 0.4365(2) 0.5774(2) 0.0903(9) Uani 1 1 d . . . H20A H 0.8781 0.4683 0.6212 0.136 Uiso 1 1 calc R . . H20B H 0.9472 0.4131 0.5821 0.136 Uiso 1 1 calc R . . H20C H 0.8522 0.3879 0.5699 0.136 Uiso 1 1 calc R . . C21 C 0.68570(12) 0.80860(12) 0.56605(10) 0.0431(4) Uani 1 1 d . . . C22 C 0.60603(13) 0.80672(14) 0.59770(12) 0.0507(5) Uani 1 1 d . . . C23 C 0.53812(15) 0.85036(16) 0.56454(16) 0.0669(7) Uani 1 1 d . . . H23 H 0.4859 0.8481 0.5857 0.080 Uiso 1 1 calc R . . C24 C 0.54745(19) 0.89722(17) 0.50032(19) 0.0764(9) Uani 1 1 d . . . H24 H 0.5011 0.9254 0.4781 0.092 Uiso 1 1 calc R . . C25 C 0.6222(2) 0.90282(16) 0.46938(17) 0.0754(9) Uani 1 1 d . . . H25 H 0.6272 0.9358 0.4265 0.091 Uiso 1 1 calc R . . C26 C 0.69441(15) 0.85871(14) 0.50143(12) 0.0538(5) Uani 1 1 d . . . C27 C 0.77326(19) 0.86757(17) 0.46908(13) 0.0661(7) Uani 1 1 d . . . H27 H 0.7753 0.9013 0.4263 0.079 Uiso 1 1 calc R . . C28 C 0.9190(2) 0.8484(4) 0.4553(2) 0.1360(19) Uani 1 1 d . . . H28A H 0.9133 0.8216 0.4070 0.163 Uiso 1 1 calc R . . H28B H 0.9264 0.9124 0.4490 0.163 Uiso 1 1 calc R . . C29 C 0.9889(2) 0.8141(4) 0.4908(2) 0.1330(19) Uani 1 1 d . . . H29A H 1.0247 0.8632 0.5073 0.160 Uiso 1 1 calc R . . H29B H 1.0200 0.7787 0.4564 0.160 Uiso 1 1 calc R . . C30 C 1.02981(15) 0.7169(2) 0.58995(15) 0.0661(6) Uani 1 1 d . . . H30 H 1.0838 0.7229 0.5729 0.079 Uiso 1 1 calc R . . C31 C 1.02025(13) 0.66357(17) 0.65298(14) 0.0568(5) Uani 1 1 d . . . C32 C 1.09167(17) 0.6232(2) 0.68808(19) 0.0796(9) Uani 1 1 d . . . H32 H 1.1443 0.6326 0.6692 0.095 Uiso 1 1 calc R . . C33 C 1.08505(19) 0.5716(2) 0.7480(2) 0.0895(10) Uani 1 1 d . . . H33 H 1.1327 0.5450 0.7695 0.107 Uiso 1 1 calc R . . C34 C 1.00653(19) 0.5579(2) 0.77802(16) 0.0775(8) Uani 1 1 d . . . H34 H 1.0022 0.5224 0.8196 0.093 Uiso 1 1 calc R . . C35 C 0.93542(16) 0.59691(15) 0.74630(13) 0.0565(6) Uani 1 1 d . . . C36 C 0.94053(12) 0.64958(14) 0.68195(11) 0.0463(4) Uani 1 1 d . . . C37 C 0.52906(18) 0.7653(2) 0.7021(2) 0.0812(9) Uani 1 1 d . . . H37A H 0.4832 0.7359 0.6753 0.097 Uiso 1 1 calc R . . H37B H 0.5138 0.8275 0.7096 0.097 Uiso 1 1 calc R . . C38 C 0.5452(2) 0.7204(3) 0.77388(19) 0.1009(11) Uani 1 1 d . . . H38A H 0.5647 0.6604 0.7659 0.151 Uiso 1 1 calc R . . H38B H 0.4943 0.7185 0.8003 0.151 Uiso 1 1 calc R . . H38C H 0.5872 0.7532 0.8018 0.151 Uiso 1 1 calc R . . C39 C 0.8440(2) 0.5519(2) 0.84171(13) 0.0782(9) Uani 1 1 d . . . H39A H 0.8813 0.5808 0.8776 0.094 Uiso 1 1 calc R . . H39B H 0.8561 0.4882 0.8418 0.094 Uiso 1 1 calc R . . C40 C 0.7549(2) 0.5676(3) 0.85999(17) 0.0995(11) Uani 1 1 d . . . H40A H 0.7441 0.6309 0.8613 0.149 Uiso 1 1 calc R . . H40B H 0.7446 0.5419 0.9070 0.149 Uiso 1 1 calc R . . H40C H 0.7185 0.5402 0.8234 0.149 Uiso 1 1 calc R . . F1 F 0.82446(12) 0.62865(17) 0.02739(11) 0.1119(7) Uani 1 1 d . . . F2 F 0.72279(12) 0.73162(14) 0.03481(12) 0.1073(7) Uani 1 1 d . . . F3 F 0.82507(16) 0.71769(17) 0.12183(17) 0.1343(9) Uani 1 1 d . . . F4 F 0.69245(13) 0.67754(14) 0.14505(11) 0.1070(7) Uani 1 1 d . . . F5 F 0.79132(13) 0.57392(13) 0.13722(10) 0.0973(6) Uani 1 1 d . . . F6 F 0.69324(15) 0.58697(17) 0.04897(13) 0.1203(8) Uani 1 1 d . . . N1 N 0.42093(10) 0.61655(11) 0.52745(10) 0.0437(4) Uani 1 1 d . . . N2 N 0.52097(11) 0.67585(11) 0.43442(9) 0.0441(4) Uani 1 1 d . . . N3 N 0.84255(14) 0.83268(14) 0.49403(10) 0.0607(5) Uani 1 1 d . . . N4 N 0.97004(13) 0.75799(14) 0.55394(12) 0.0604(5) Uani 1 1 d . . . Ni1 Ni 0.535424(14) 0.606749(15) 0.517943(12) 0.03520(7) Uani 1 1 d . . . Ni2 Ni 0.857863(15) 0.759142(17) 0.574256(13) 0.04045(7) Uani 1 1 d . . . O1 O 0.55207(8) 0.54251(9) 0.60331(7) 0.0411(3) Uani 1 1 d . . . O2 O 0.64921(8) 0.59129(9) 0.50756(7) 0.0400(3) Uani 1 1 d . . . O3 O 0.60740(11) 0.45162(11) 0.71520(8) 0.0608(4) Uani 1 1 d . . . O4 O 0.80164(9) 0.53230(12) 0.50926(9) 0.0591(4) Uani 1 1 d . . . O5 O 0.74746(9) 0.76352(9) 0.59893(7) 0.0442(3) Uani 1 1 d . . . O6 O 0.87066(8) 0.68297(10) 0.65321(7) 0.0453(3) Uani 1 1 d . . . O7 O 0.60394(10) 0.76003(11) 0.66197(9) 0.0574(4) Uani 1 1 d . . . O8 O 0.85579(12) 0.58845(13) 0.77085(9) 0.0705(5) Uani 1 1 d . . . P1 P 0.75815(4) 0.65262(5) 0.08644(4) 0.05899(16) Uani 1 1 d . . . N5 N 0.71414(12) 0.59372(14) 0.65143(10) 0.0473(4) Uani 1 1 d D . . H5A H 0.7626(15) 0.593(2) 0.6693(16) 0.108(12) Uiso 1 1 d D . . H5B H 0.7151(19) 0.583(2) 0.6057(9) 0.096(11) Uiso 1 1 d D . . H5C H 0.689(2) 0.5528(18) 0.6711(16) 0.128(14) Uiso 1 1 d D . . H5D H 0.6925(18) 0.6422(16) 0.6558(16) 0.100(12) Uiso 1 1 d 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 C1 0.0451(10) 0.0359(9) 0.0435(9) -0.0046(7) 0.0071(8) -0.0106(8) C2 0.0584(12) 0.0470(11) 0.0475(10) 0.0035(8) 0.0103(9) -0.0110(9) C3 0.094(2) 0.0621(15) 0.0564(13) 0.0071(11) 0.0220(13) -0.0186(14) C4 0.0804(19) 0.0775(18) 0.0789(17) -0.0013(14) 0.0433(15) -0.0160(15) C5 0.0573(14) 0.0711(16) 0.0819(17) -0.0088(14) 0.0319(13) -0.0098(12) C6 0.0446(11) 0.0416(10) 0.0612(12) -0.0117(9) 0.0149(9) -0.0086(8) C7 0.0342(9) 0.0465(11) 0.0686(13) -0.0167(9) 0.0032(9) -0.0010(8) C8 0.0445(11) 0.0541(13) 0.0606(12) -0.0147(10) -0.0180(9) 0.0108(9) C9 0.0592(13) 0.0477(12) 0.0605(12) -0.0032(10) -0.0210(10) 0.0121(10) C10 0.0738(15) 0.0439(11) 0.0390(9) 0.0039(8) -0.0097(9) -0.0053(10) C11 0.0627(13) 0.0473(11) 0.0382(9) -0.0009(8) 0.0061(8) -0.0110(10) C12 0.0858(19) 0.0773(18) 0.0451(11) 0.0089(11) 0.0125(11) -0.0166(14) C13 0.085(2) 0.106(2) 0.0531(14) 0.0034(14) 0.0270(13) -0.0263(17) C14 0.0575(14) 0.094(2) 0.0614(14) -0.0141(13) 0.0237(11) -0.0153(13) C15 0.0465(11) 0.0610(13) 0.0460(10) -0.0081(9) 0.0083(8) -0.0088(9) C16 0.0455(10) 0.0412(10) 0.0360(8) -0.0074(7) 0.0051(7) -0.0092(8) C17 0.096(2) 0.0617(15) 0.0474(12) 0.0208(10) -0.0046(12) -0.0023(14) C18 0.091(2) 0.0813(19) 0.0645(15) 0.0220(14) -0.0194(14) 0.0126(16) C19 0.0432(13) 0.088(2) 0.0849(18) -0.0105(15) 0.0092(12) 0.0122(12) C20 0.0587(17) 0.099(2) 0.113(2) -0.003(2) -0.0035(16) 0.0204(16) C21 0.0472(10) 0.0349(9) 0.0461(9) -0.0059(7) -0.0116(8) 0.0029(8) C22 0.0460(11) 0.0420(11) 0.0628(12) -0.0175(9) -0.0133(9) 0.0040(8) C23 0.0485(12) 0.0486(13) 0.102(2) -0.0255(13) -0.0221(13) 0.0106(10) C24 0.0683(18) 0.0479(14) 0.109(2) -0.0070(13) -0.0451(16) 0.0152(12) C25 0.097(2) 0.0410(13) 0.0851(18) 0.0086(11) -0.0424(17) 0.0015(13) C26 0.0669(14) 0.0381(10) 0.0548(11) 0.0032(9) -0.0201(10) -0.0009(10) C27 0.0886(19) 0.0560(14) 0.0528(12) 0.0188(11) -0.0095(12) -0.0080(13) C28 0.095(3) 0.190(5) 0.125(3) 0.098(3) 0.046(2) 0.010(3) C29 0.074(2) 0.207(5) 0.120(3) 0.088(3) 0.031(2) -0.006(3) C30 0.0380(12) 0.0819(18) 0.0788(16) -0.0075(14) 0.0079(11) -0.0064(11) C31 0.0395(11) 0.0602(14) 0.0699(14) -0.0137(11) -0.0089(10) 0.0035(10) C32 0.0450(14) 0.094(2) 0.098(2) -0.0180(18) -0.0166(14) 0.0166(13) C33 0.0640(18) 0.098(2) 0.104(2) -0.0059(19) -0.0333(17) 0.0302(16) C34 0.0803(19) 0.0747(18) 0.0749(16) 0.0074(14) -0.0337(15) 0.0138(15) C35 0.0578(14) 0.0523(13) 0.0579(12) 0.0022(10) -0.0195(10) 0.0000(10) C36 0.0407(10) 0.0451(11) 0.0521(10) -0.0072(8) -0.0116(8) 0.0027(8) C37 0.0499(14) 0.085(2) 0.111(2) -0.0317(18) 0.0254(15) -0.0083(13) C38 0.099(3) 0.119(3) 0.088(2) -0.016(2) 0.0453(19) -0.013(2) C39 0.107(2) 0.0789(18) 0.0472(12) 0.0212(12) -0.0238(14) -0.0142(17) C40 0.112(3) 0.129(3) 0.0577(15) 0.0170(18) 0.0047(16) -0.020(2) F1 0.0787(12) 0.1591(19) 0.1007(13) 0.0281(13) 0.0393(10) 0.0296(12) F2 0.0737(11) 0.1203(15) 0.1300(16) 0.0765(13) 0.0328(11) 0.0211(10) F3 0.1205(18) 0.0952(15) 0.184(2) 0.0042(16) -0.0327(17) -0.0316(13) F4 0.1244(16) 0.1009(14) 0.0996(13) 0.0251(11) 0.0566(12) 0.0425(12) F5 0.1135(15) 0.0847(12) 0.0949(12) 0.0336(10) 0.0183(11) 0.0304(11) F6 0.1130(17) 0.1241(18) 0.1226(17) -0.0017(14) -0.0104(14) -0.0406(13) N1 0.0359(8) 0.0409(9) 0.0538(9) -0.0128(7) -0.0061(7) 0.0044(6) N2 0.0524(9) 0.0364(8) 0.0427(8) -0.0029(6) -0.0101(7) 0.0030(7) N3 0.0677(13) 0.0634(12) 0.0514(10) 0.0143(9) 0.0071(9) -0.0072(10) N4 0.0449(11) 0.0751(14) 0.0619(12) 0.0054(10) 0.0110(9) -0.0084(9) Ni1 0.03470(12) 0.03384(13) 0.03681(12) -0.00275(8) -0.00197(9) 0.00132(9) Ni2 0.03934(14) 0.04403(14) 0.03802(12) 0.00239(9) 0.00222(10) -0.00361(10) O1 0.0366(6) 0.0448(7) 0.0422(6) 0.0060(5) 0.0061(5) 0.0004(5) O2 0.0372(7) 0.0471(7) 0.0358(6) 0.0013(5) 0.0025(5) 0.0002(5) O3 0.0671(10) 0.0599(10) 0.0553(8) 0.0252(7) 0.0020(7) -0.0016(8) O4 0.0386(7) 0.0771(11) 0.0620(9) -0.0002(8) 0.0078(7) 0.0060(7) O5 0.0384(7) 0.0517(8) 0.0423(7) 0.0060(6) -0.0017(5) 0.0050(6) O6 0.0356(7) 0.0541(8) 0.0458(7) 0.0084(6) -0.0046(5) 0.0004(6) O7 0.0394(8) 0.0710(11) 0.0619(9) -0.0132(8) 0.0041(7) 0.0004(7) O8 0.0663(11) 0.0889(13) 0.0549(9) 0.0296(9) -0.0172(8) -0.0070(9) P1 0.0539(3) 0.0585(4) 0.0655(4) 0.0139(3) 0.0150(3) 0.0004(3) N5 0.0431(10) 0.0553(12) 0.0430(9) 0.0075(8) -0.0046(7) -0.0090(9) _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 C1 O1 1.3094(18) . ? C1 C6 1.413(3) . ? C1 C2 1.418(3) . ? C2 O3 1.373(2) . ? C2 C3 1.388(3) . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.350(4) . ? C4 H4 0.9300 . ? C5 C6 1.416(3) . ? C5 H5 0.9300 . ? C6 C7 1.432(3) . ? C7 N1 1.278(2) . ? C7 H7 0.9300 . ? C8 N1 1.474(2) . ? C8 C9 1.493(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.476(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.285(2) . ? C10 C11 1.430(3) . ? C10 H10 0.9300 . ? C11 C16 1.409(3) . ? C11 C12 1.417(3) . ? C12 C13 1.353(4) . ? C12 H12 0.9300 . ? C13 C14 1.382(4) . ? C13 H13 0.9300 . ? C14 C15 1.390(3) . ? C14 H14 0.9300 . ? C15 O4 1.376(2) . ? C15 C16 1.411(3) . ? C16 O2 1.3093(18) . ? C17 O3 1.437(2) . ? C17 C18 1.483(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.416(2) . ? C19 C20 1.481(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.3182(18) . ? C21 C26 1.408(2) . ? C21 C22 1.414(3) . ? C22 O7 1.366(2) . ? C22 C23 1.383(3) . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 C25 1.339(5) . ? C24 H24 0.9300 . ? C25 C26 1.432(3) . ? C25 H25 0.9300 . ? C26 C27 1.414(4) . ? C27 N3 1.289(3) . ? C27 H27 0.9300 . ? C28 C29 1.367(5) . ? C28 N3 1.450(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.464(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.292(3) . ? C30 C31 1.411(4) . ? C30 H30 0.9300 . ? C31 C36 1.409(3) . ? C31 C32 1.420(3) . ? C32 C33 1.344(5) . ? C32 H32 0.9300 . ? C33 C34 1.400(5) . ? C33 H33 0.9300 . ? C34 C35 1.382(3) . ? C34 H34 0.9300 . ? C35 O8 1.367(3) . ? C35 C36 1.418(3) . ? C36 O6 1.312(2) . ? C37 O7 1.425(3) . ? C37 C38 1.486(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O8 1.423(3) . ? C39 C40 1.489(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? F1 P1 1.5780(19) . ? F2 P1 1.5986(18) . ? F3 P1 1.564(2) . ? F4 P1 1.5691(17) . ? F5 P1 1.5752(17) . ? F6 P1 1.564(2) . ? N1 Ni1 1.8447(17) . ? N2 Ni1 1.8478(16) . ? N3 Ni2 1.8390(19) . ? N4 Ni2 1.839(2) . ? Ni1 O1 1.8404(13) . ? Ni1 O2 1.8443(14) . ? Ni2 O5 1.8331(14) . ? Ni2 O6 1.8409(13) . ? N5 H5A 0.83(2) . ? N5 H5B 0.851(15) . ? N5 H5C 0.819(16) . ? N5 H5D 0.81(2) . ? 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 C1 C6 124.28(17) . . ? O1 C1 C2 117.79(17) . . ? C6 C1 C2 117.91(18) . . ? O3 C2 C3 125.5(2) . . ? O3 C2 C1 113.61(16) . . ? C3 C2 C1 120.9(2) . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.9(2) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.5(2) . . ? C1 C6 C7 120.54(18) . . ? C5 C6 C7 119.8(2) . . ? N1 C7 C6 125.12(17) . . ? N1 C7 H7 117.4 . . ? C6 C7 H7 117.4 . . ? N1 C8 C9 106.33(15) . . ? N1 C8 H8A 110.5 . . ? C9 C8 H8A 110.5 . . ? N1 C8 H8B 110.5 . . ? C9 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? N2 C9 C8 106.72(16) . . ? N2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? N2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 125.27(17) . . ? N2 C10 H10 117.4 . . ? C11 C10 H10 117.4 . . ? C16 C11 C12 120.0(2) . . ? C16 C11 C10 120.77(18) . . ? C12 C11 C10 119.2(2) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.7(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? O4 C15 C14 125.2(2) . . ? O4 C15 C16 114.13(16) . . ? C14 C15 C16 120.7(2) . . ? O2 C16 C11 124.55(18) . . ? O2 C16 C15 117.63(17) . . ? C11 C16 C15 117.82(18) . . ? O3 C17 C18 107.09(19) . . ? O3 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O3 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 107.9(2) . . ? O4 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O4 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C26 123.88(16) . . ? O5 C21 C22 118.04(17) . . ? C26 C21 C22 118.07(15) . . ? O7 C22 C23 124.9(2) . . ? O7 C22 C21 114.31(16) . . ? C23 C22 C21 120.7(2) . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 121.1(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.8(2) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C27 121.08(18) . . ? C21 C26 C25 118.95(18) . . ? C27 C26 C25 119.96(18) . . ? N3 C27 C26 125.3(2) . . ? N3 C27 H27 117.4 . . ? C26 C27 H27 117.4 . . ? C29 C28 N3 113.2(3) . . ? C29 C28 H28A 108.9 . . ? N3 C28 H28A 108.9 . . ? C29 C28 H28B 108.9 . . ? N3 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C28 C29 N4 113.5(3) . . ? C28 C29 H29A 108.9 . . ? N4 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? N4 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N4 C30 C31 125.6(2) . . ? N4 C30 H30 117.2 . . ? C31 C30 H30 117.2 . . ? C36 C31 C30 121.0(2) . . ? C36 C31 C32 119.1(3) . . ? C30 C31 C32 119.9(2) . . ? C33 C32 C31 121.6(3) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? O8 C35 C34 125.5(2) . . ? O8 C35 C36 113.90(19) . . ? C34 C35 C36 120.6(3) . . ? O6 C36 C31 123.9(2) . . ? O6 C36 C35 117.9(2) . . ? C31 C36 C35 118.2(2) . . ? O7 C37 C38 107.9(3) . . ? O7 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O7 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 107.6(2) . . ? O8 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O8 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C7 N1 C8 120.06(13) . . ? C7 N1 Ni1 127.42(11) . . ? C8 N1 Ni1 112.42(11) . . ? C10 N2 C9 119.78(14) . . ? C10 N2 Ni1 127.23(11) . . ? C9 N2 Ni1 112.89(10) . . ? C27 N3 C28 119.2(2) . . ? C27 N3 Ni2 127.54(18) . . ? C28 N3 Ni2 113.3(2) . . ? C30 N4 C29 120.2(2) . . ? C30 N4 Ni2 127.26(18) . . ? C29 N4 Ni2 112.5(2) . . ? O1 Ni1 O2 84.86(6) . . ? O1 Ni1 N1 94.23(7) . . ? O2 Ni1 N1 177.31(6) . . ? O1 Ni1 N2 177.31(6) . . ? O2 Ni1 N2 94.48(7) . . ? N1 Ni1 N2 86.55(8) . . ? O5 Ni2 N3 94.25(8) . . ? O5 Ni2 N4 177.00(8) . . ? N3 Ni2 N4 86.93(10) . . ? O5 Ni2 O6 84.79(6) . . ? N3 Ni2 O6 178.13(8) . . ? N4 Ni2 O6 94.11(8) . . ? C1 O1 Ni1 127.40(9) . . ? C16 O2 Ni1 127.18(9) . . ? C2 O3 C17 118.40(15) . . ? C15 O4 C19 119.18(15) . . ? C21 O5 Ni2 127.84(9) . . ? C36 O6 Ni2 127.99(13) . . ? C22 O7 C37 117.43(19) . . ? C35 O8 C39 119.3(2) . . ? F6 P1 F3 178.12(17) . . ? F6 P1 F4 89.97(14) . . ? F3 P1 F4 91.90(15) . . ? F6 P1 F5 89.58(13) . . ? F3 P1 F5 90.62(13) . . ? F4 P1 F5 89.60(10) . . ? F6 P1 F1 90.46(14) . . ? F3 P1 F1 87.67(15) . . ? F4 P1 F1 179.39(13) . . ? F5 P1 F1 90.83(11) . . ? F6 P1 F2 89.48(13) . . ? F3 P1 F2 90.34(13) . . ? F4 P1 F2 89.88(10) . . ? F5 P1 F2 178.92(12) . . ? F1 P1 F2 89.70(11) . . ? H5A N5 H5B 110(2) . . ? H5A N5 H5C 107(2) . . ? H5B N5 H5C 108(2) . . ? H5A N5 H5D 111(2) . . ? H5B N5 H5D 107(2) . . ? H5C N5 H5D 114(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 32.70 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.529 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.069 #END=== data_2 _database_code_depnum_ccdc_archive 'CCDC 813957' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 Cl N2 Na Ni O9' _chemical_formula_weight 567.59 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' 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 8.2000(6) _cell_length_b 21.5329(14) _cell_length_c 14.1163(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.627(3) _cell_angle_gamma 90.00 _cell_volume 2411.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8401 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.65 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8121 _exptl_absorpt_correction_T_max 0.8423 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42069 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 35.38 _reflns_number_total 10820 _reflns_number_gt 5798 _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. Ueq for O6 is high giving an indication of disorder but could not be modelled successfully. ; _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^)+(0.0700P)^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 10820 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.63927(3) 0.994975(10) 0.863732(16) 0.03842(8) Uani 1 1 d . . . N1 N 0.6823(2) 1.03930(7) 0.97925(12) 0.0463(4) Uani 1 1 d . . . N2 N 0.4966(2) 1.05861(8) 0.80898(13) 0.0484(4) Uani 1 1 d . . . O1 O 0.77425(16) 0.92844(6) 0.91641(9) 0.0428(3) Uani 1 1 d . . . O2 O 0.59920(16) 0.94947(6) 0.75024(9) 0.0453(3) Uani 1 1 d . . . Na1 Na 0.74779(9) 0.85763(4) 0.79119(5) 0.04483(18) Uani 1 1 d . . . O3 O 0.93192(17) 0.82284(6) 0.95743(9) 0.0470(3) Uani 1 1 d . . . O4 O 0.57617(18) 0.86598(7) 0.61540(9) 0.0491(3) Uani 1 1 d . . . O5 O 1.0013(2) 0.86159(10) 0.74288(14) 0.0675(5) Uani 1 1 d . . . O6 O 0.5601(2) 0.78031(14) 0.81869(17) 0.1099(9) Uani 1 1 d . . . Cl1 Cl 0.39072(6) 0.76338(2) 0.79231(3) 0.04710(12) Uani 1 1 d . . . O7 O 0.3187(2) 0.77302(10) 0.69074(12) 0.0803(6) Uani 1 1 d . . . O8 O 0.3008(3) 0.79646(18) 0.84767(18) 0.1360(12) Uani 1 1 d . . . O9 O 0.3761(4) 0.69983(11) 0.81305(17) 0.1291(11) Uani 1 1 d . . . C1 C 0.8661(2) 0.92200(9) 1.00679(13) 0.0393(4) Uani 1 1 d . . . C2 C 0.9542(2) 0.86544(9) 1.03251(13) 0.0429(4) Uani 1 1 d . . . C3 C 1.0516(3) 0.85592(12) 1.12647(15) 0.0566(5) Uani 1 1 d . . . H3 H 1.1081 0.8185 1.1431 0.068 Uiso 1 1 calc R . . C4 C 1.0651(3) 0.90280(14) 1.19672(15) 0.0687(7) Uani 1 1 d . . . H4 H 1.1323 0.8963 1.2596 0.082 Uiso 1 1 calc R . . C5 C 0.9837(3) 0.95661(13) 1.17527(15) 0.0640(6) Uani 1 1 d . . . H5 H 0.9953 0.9872 1.2230 0.077 Uiso 1 1 calc R . . C6 C 0.8790(3) 0.96756(10) 1.07955(14) 0.0483(5) Uani 1 1 d . . . C7 C 0.7851(3) 1.02457(10) 1.06020(16) 0.0522(5) Uani 1 1 d . . . H7 H 0.8006 1.0532 1.1110 0.063 Uiso 1 1 calc R . . C8 C 0.5790(3) 1.09557(11) 0.97484(19) 0.0653(6) Uani 1 1 d . . . H8A H 0.6473 1.1290 1.0105 0.078 Uiso 1 1 calc R . . H8B H 0.4873 1.0876 1.0052 0.078 Uiso 1 1 calc R . . C9 C 0.5103(4) 1.11405(11) 0.8715(2) 0.0681(6) Uani 1 1 d . . . H9A H 0.4002 1.1329 0.8634 0.082 Uiso 1 1 calc R . . H9B H 0.5841 1.1443 0.8528 0.082 Uiso 1 1 calc R . . C10 C 0.3953(3) 1.05946(10) 0.72213(17) 0.0546(5) Uani 1 1 d . . . H10 H 0.3276 1.0944 0.7049 0.066 Uiso 1 1 calc R . . C11 C 0.3787(3) 1.01183(10) 0.65104(16) 0.0502(5) Uani 1 1 d . . . C12 C 0.2571(3) 1.01811(14) 0.55929(19) 0.0688(7) Uani 1 1 d . . . H12 H 0.1869 1.0527 0.5477 0.083 Uiso 1 1 calc R . . C13 C 0.2430(3) 0.97461(16) 0.48949(19) 0.0779(8) Uani 1 1 d . . . H13 H 0.1618 0.9791 0.4306 0.094 Uiso 1 1 calc R . . C14 C 0.3490(3) 0.92257(13) 0.50412(15) 0.0621(6) Uani 1 1 d . . . H14 H 0.3399 0.8933 0.4546 0.075 Uiso 1 1 calc R . . C15 C 0.4673(2) 0.91490(10) 0.59272(13) 0.0466(4) Uani 1 1 d . . . C16 C 0.4838(2) 0.95932(9) 0.66781(13) 0.0422(4) Uani 1 1 d . . . C17 C 1.0225(3) 0.76538(10) 0.97691(17) 0.0524(5) Uani 1 1 d . . . H17A H 1.0071 0.7472 1.0369 0.063 Uiso 1 1 calc R . . H17B H 1.1419 0.7727 0.9848 0.063 Uiso 1 1 calc R . . C18 C 0.9574(3) 0.72239(11) 0.8933(2) 0.0661(6) Uani 1 1 d . . . H18A H 0.8424 0.7119 0.8903 0.099 Uiso 1 1 calc R . . H18B H 1.0245 0.6853 0.9024 0.099 Uiso 1 1 calc R . . H18C H 0.9633 0.7423 0.8334 0.099 Uiso 1 1 calc R . . C19 C 0.5586(3) 0.81719(12) 0.54462(15) 0.0607(6) Uani 1 1 d . . . H19A H 0.5856 0.8326 0.4858 0.073 Uiso 1 1 calc R . . H19B H 0.4434 0.8022 0.5272 0.073 Uiso 1 1 calc R . . C20 C 0.6749(4) 0.76615(12) 0.5875(2) 0.0698(7) Uani 1 1 d . . . H20A H 0.7877 0.7820 0.6088 0.105 Uiso 1 1 calc R . . H20B H 0.6708 0.7345 0.5392 0.105 Uiso 1 1 calc R . . H20C H 0.6417 0.7489 0.6425 0.105 Uiso 1 1 calc R . . C21 C 1.0251(4) 0.89071(13) 0.6588(2) 0.0742(7) Uani 1 1 d . . . H21A H 1.0717 0.8615 0.6214 0.111 Uiso 1 1 calc R . . H21B H 1.1011 0.9251 0.6774 0.111 Uiso 1 1 calc R . . H21C H 0.9187 0.9055 0.6199 0.111 Uiso 1 1 calc R . . H5A H 1.067(4) 0.8401(16) 0.772(2) 0.092(11) Uiso 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 Ni1 0.03998(14) 0.03134(13) 0.04473(14) -0.00123(9) 0.01213(10) 0.00285(8) N1 0.0514(9) 0.0350(8) 0.0563(9) -0.0080(7) 0.0205(7) -0.0045(7) N2 0.0487(9) 0.0340(8) 0.0657(10) 0.0017(7) 0.0205(8) 0.0068(7) O1 0.0466(7) 0.0399(7) 0.0377(6) -0.0035(5) 0.0029(5) 0.0068(5) O2 0.0475(7) 0.0432(7) 0.0408(6) -0.0018(5) 0.0028(5) 0.0120(6) Na1 0.0448(4) 0.0427(4) 0.0462(4) -0.0042(3) 0.0100(3) 0.0065(3) O3 0.0487(7) 0.0416(7) 0.0470(7) 0.0033(6) 0.0052(6) 0.0084(6) O4 0.0546(8) 0.0494(8) 0.0406(6) -0.0054(6) 0.0074(6) 0.0025(6) O5 0.0557(9) 0.0820(13) 0.0687(10) 0.0191(9) 0.0230(8) 0.0147(9) O6 0.0452(10) 0.173(2) 0.1016(15) 0.0453(16) 0.0009(9) -0.0269(13) Cl1 0.0403(2) 0.0572(3) 0.0435(2) -0.0031(2) 0.00986(18) -0.00422(19) O7 0.0789(12) 0.1001(15) 0.0524(9) 0.0161(9) -0.0013(8) -0.0088(11) O8 0.0885(16) 0.225(3) 0.0968(17) -0.061(2) 0.0271(13) 0.0348(19) O9 0.203(3) 0.0734(15) 0.0808(14) 0.0151(12) -0.0206(15) -0.0344(17) C1 0.0360(8) 0.0426(10) 0.0390(8) 0.0003(7) 0.0093(7) -0.0050(7) C2 0.0377(9) 0.0466(10) 0.0422(9) 0.0048(8) 0.0062(7) -0.0043(7) C3 0.0533(12) 0.0631(14) 0.0478(10) 0.0100(10) 0.0025(9) -0.0002(10) C4 0.0703(15) 0.0852(19) 0.0407(10) 0.0026(11) -0.0042(10) -0.0059(14) C5 0.0695(15) 0.0767(17) 0.0404(10) -0.0129(11) 0.0039(9) -0.0098(13) C6 0.0488(11) 0.0515(12) 0.0429(9) -0.0063(8) 0.0085(8) -0.0102(9) C7 0.0603(12) 0.0445(11) 0.0539(11) -0.0172(9) 0.0182(10) -0.0119(9) C8 0.0780(16) 0.0422(12) 0.0824(16) -0.0146(11) 0.0327(13) 0.0033(11) C9 0.0821(17) 0.0372(11) 0.0867(17) -0.0002(11) 0.0245(13) 0.0143(11) C10 0.0484(11) 0.0438(11) 0.0724(14) 0.0176(10) 0.0165(10) 0.0131(9) C11 0.0434(11) 0.0493(11) 0.0560(11) 0.0136(9) 0.0090(9) 0.0065(8) C12 0.0602(14) 0.0732(16) 0.0643(14) 0.0246(13) -0.0005(11) 0.0182(12) C13 0.0639(16) 0.098(2) 0.0580(14) 0.0185(15) -0.0101(11) 0.0099(15) C14 0.0603(13) 0.0760(16) 0.0432(10) 0.0041(10) 0.0003(9) -0.0029(12) C15 0.0435(10) 0.0537(12) 0.0414(9) 0.0058(8) 0.0085(7) -0.0026(8) C16 0.0380(9) 0.0435(10) 0.0438(9) 0.0092(8) 0.0080(7) 0.0026(7) C17 0.0470(11) 0.0483(12) 0.0626(12) 0.0122(10) 0.0151(9) 0.0099(9) C18 0.0631(14) 0.0471(13) 0.0875(17) 0.0010(12) 0.0180(12) 0.0087(11) C19 0.0737(15) 0.0650(15) 0.0472(11) -0.0170(10) 0.0223(10) -0.0139(12) C20 0.0876(19) 0.0550(14) 0.0777(16) -0.0166(12) 0.0409(15) -0.0057(13) C21 0.0876(18) 0.0631(16) 0.0783(16) 0.0089(13) 0.0331(14) -0.0050(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 Ni1 O2 1.8355(13) . ? Ni1 N2 1.8404(16) . ? Ni1 N1 1.8450(16) . ? Ni1 O1 1.8480(13) . ? N1 C7 1.277(3) . ? N1 C8 1.470(3) . ? N2 C10 1.296(3) . ? N2 C9 1.472(3) . ? O1 C1 1.315(2) . ? O1 Na1 2.3027(14) . ? O2 C16 1.318(2) . ? O2 Na1 2.3182(15) . ? Na1 O5 2.3471(19) . ? Na1 O6 2.365(2) . ? Na1 O4 2.5312(15) . ? Na1 O3 2.5610(14) . ? O3 C2 1.378(2) . ? O3 C17 1.433(2) . ? O4 C15 1.366(2) . ? O4 C19 1.432(2) . ? O5 C21 1.399(3) . ? O5 H5A 0.75(3) . ? O6 Cl1 1.3925(19) . ? Cl1 O8 1.397(2) . ? Cl1 O9 1.411(2) . ? Cl1 O7 1.4212(17) . ? C1 C6 1.405(3) . ? C1 C2 1.416(3) . ? C2 C3 1.380(3) . ? C3 C4 1.400(4) . ? C3 H3 0.9300 . ? C4 C5 1.333(4) . ? C4 H4 0.9300 . ? C5 C6 1.426(3) . ? C5 H5 0.9300 . ? C6 C7 1.438(3) . ? C7 H7 0.9300 . ? C8 C9 1.479(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.417(3) . ? C10 H10 0.9300 . ? C11 C16 1.406(3) . ? C11 C12 1.428(3) . ? C12 C13 1.343(4) . ? C12 H12 0.9300 . ? C13 C14 1.401(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(3) . ? C14 H14 0.9300 . ? C15 C16 1.409(3) . ? C17 C18 1.488(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.481(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 N2 94.37(7) . . ? O2 Ni1 N1 178.75(7) . . ? N2 Ni1 N1 86.87(8) . . ? O2 Ni1 O1 83.93(5) . . ? N2 Ni1 O1 177.27(7) . . ? N1 Ni1 O1 94.82(7) . . ? C7 N1 C8 119.04(18) . . ? C7 N1 Ni1 126.74(15) . . ? C8 N1 Ni1 114.16(14) . . ? C10 N2 C9 119.32(18) . . ? C10 N2 Ni1 126.54(15) . . ? C9 N2 Ni1 114.07(15) . . ? C1 O1 Ni1 127.60(12) . . ? C1 O1 Na1 126.51(12) . . ? Ni1 O1 Na1 105.89(6) . . ? C16 O2 Ni1 127.95(12) . . ? C16 O2 Na1 124.90(12) . . ? Ni1 O2 Na1 105.71(6) . . ? O1 Na1 O2 64.42(5) . . ? O1 Na1 O5 106.28(7) . . ? O2 Na1 O5 110.17(7) . . ? O1 Na1 O6 106.21(9) . . ? O2 Na1 O6 108.58(8) . . ? O5 Na1 O6 137.23(10) . . ? O1 Na1 O4 128.82(5) . . ? O2 Na1 O4 64.40(5) . . ? O5 Na1 O4 91.52(6) . . ? O6 Na1 O4 89.26(7) . . ? O1 Na1 O3 64.58(5) . . ? O2 Na1 O3 128.99(5) . . ? O5 Na1 O3 85.20(6) . . ? O6 Na1 O3 84.33(6) . . ? O4 Na1 O3 166.48(6) . . ? C2 O3 C17 117.74(15) . . ? C2 O3 Na1 116.28(10) . . ? C17 O3 Na1 125.82(12) . . ? C15 O4 C19 117.25(16) . . ? C15 O4 Na1 116.96(11) . . ? C19 O4 Na1 124.41(13) . . ? C21 O5 Na1 125.89(17) . . ? C21 O5 H5A 121(3) . . ? Na1 O5 H5A 112(3) . . ? Cl1 O6 Na1 141.90(15) . . ? O6 Cl1 O8 110.38(18) . . ? O6 Cl1 O9 109.24(18) . . ? O8 Cl1 O9 107.1(2) . . ? O6 Cl1 O7 111.34(12) . . ? O8 Cl1 O7 110.25(15) . . ? O9 Cl1 O7 108.40(13) . . ? O1 C1 C6 123.70(17) . . ? O1 C1 C2 118.00(16) . . ? C6 C1 C2 118.29(17) . . ? O3 C2 C3 124.90(19) . . ? O3 C2 C1 114.54(15) . . ? C3 C2 C1 120.55(19) . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 121.4(2) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 119.6(2) . . ? C1 C6 C7 121.29(18) . . ? C5 C6 C7 119.1(2) . . ? N1 C7 C6 125.64(19) . . ? N1 C7 H7 117.2 . . ? C6 C7 H7 117.2 . . ? N1 C8 C9 109.59(18) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 109.00(18) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 125.74(18) . . ? N2 C10 H10 117.1 . . ? C11 C10 H10 117.1 . . ? C16 C11 C10 121.17(19) . . ? C16 C11 C12 119.2(2) . . ? C10 C11 C12 119.6(2) . . ? C13 C12 C11 120.7(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 121.0(2) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? O4 C15 C14 124.8(2) . . ? O4 C15 C16 114.48(15) . . ? C14 C15 C16 120.7(2) . . ? O2 C16 C11 123.44(18) . . ? O2 C16 C15 117.79(17) . . ? C11 C16 C15 118.76(18) . . ? O3 C17 C18 108.67(17) . . ? O3 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O3 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 108.55(18) . . ? O4 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O4 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 35.38 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.663 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.064 #END=== data_3 _database_code_depnum_ccdc_archive 'CCDC 813958' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H64 B N4 Na Ni2 O8' _chemical_formula_weight 1168.41 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 18.056(3) _cell_length_b 19.572(3) _cell_length_c 18.290(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.934(2) _cell_angle_gamma 90.00 _cell_volume 6076.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8745 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 21.86 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8532 _exptl_absorpt_correction_T_max 0.8986 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45408 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11842 _reflns_number_gt 7556 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4614P] 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 11842 _refine_ls_number_parameters 723 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.892 _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 B1 B 0.46131(17) 0.84881(17) 0.65534(19) 0.0495(8) Uani 1 1 d . . . C1 C -0.08609(19) 0.50058(14) 0.85777(17) 0.0559(7) Uani 1 1 d . . . C2 C -0.0068(2) 0.47980(14) 0.89005(16) 0.0569(8) Uani 1 1 d . . . C3 C 0.0156(2) 0.43042(15) 0.94669(17) 0.0716(10) Uani 1 1 d . . . H3 H 0.0681 0.4173 0.9673 0.086 Uiso 1 1 calc R . . C4 C -0.0398(3) 0.39996(18) 0.9734(2) 0.0833(12) Uani 1 1 d . . . H4 H -0.0239 0.3675 1.0128 0.100 Uiso 1 1 calc R . . C5 C -0.1161(3) 0.41703(17) 0.9428(2) 0.0812(12) Uani 1 1 d . . . H5 H -0.1533 0.3950 0.9593 0.097 Uiso 1 1 calc R . . C6 C -0.1401(2) 0.46874(16) 0.88514(19) 0.0687(9) Uani 1 1 d . . . C7 C -0.2214(2) 0.48669(18) 0.8541(2) 0.0856(12) Uani 1 1 d . . . H7 H -0.2559 0.4614 0.8713 0.103 Uiso 1 1 calc R . . C8 C -0.3377(2) 0.5475(2) 0.7726(3) 0.1225(17) Uani 1 1 d D . . H8A H -0.3638 0.5308 0.8076 0.147 Uiso 1 1 calc R A 1 H8B H -0.3612 0.5258 0.7222 0.147 Uiso 1 1 calc R A 1 C10 C -0.30594(18) 0.68686(18) 0.6669(2) 0.0845(11) Uani 1 1 d . B . H10 H -0.3551 0.7076 0.6535 0.101 Uiso 1 1 calc R . . C11 C -0.25308(17) 0.71159(16) 0.6302(2) 0.0665(9) Uani 1 1 d . . . C12 C -0.2786(2) 0.76259(19) 0.5730(2) 0.0845(12) Uani 1 1 d . . . H12 H -0.3295 0.7797 0.5595 0.101 Uiso 1 1 calc R . . C13 C -0.2296(2) 0.78677(18) 0.5375(2) 0.0836(11) Uani 1 1 d . . . H13 H -0.2477 0.8195 0.4986 0.100 Uiso 1 1 calc R . . C14 C -0.1523(2) 0.76340(15) 0.55831(18) 0.0674(9) Uani 1 1 d . . . H14 H -0.1188 0.7810 0.5340 0.081 Uiso 1 1 calc R . . C15 C -0.12553(16) 0.71417(14) 0.61505(16) 0.0525(7) Uani 1 1 d . . . C16 C -0.17518(15) 0.68699(13) 0.65192(16) 0.0507(7) Uani 1 1 d . . . C17 C 0.12575(18) 0.49592(16) 0.88762(19) 0.0674(9) Uani 1 1 d . . . H17A H 0.1431 0.4852 0.9427 0.081 Uiso 1 1 calc R . . H17B H 0.1563 0.5345 0.8806 0.081 Uiso 1 1 calc R . . C18 C 0.1403(2) 0.43622(18) 0.8443(2) 0.0866(11) Uani 1 1 d . . . H18A H 0.1119 0.3974 0.8531 0.130 Uiso 1 1 calc R . . H18B H 0.1956 0.4261 0.8622 0.130 Uiso 1 1 calc R . . H18C H 0.1227 0.4465 0.7898 0.130 Uiso 1 1 calc R . . C19 C 0.01171(19) 0.72423(18) 0.6256(2) 0.0733(10) Uani 1 1 d . . . H19A H -0.0066 0.7391 0.5718 0.088 Uiso 1 1 calc R . . H19B H 0.0560 0.6937 0.6330 0.088 Uiso 1 1 calc R . . C20 C 0.03845(19) 0.78458(18) 0.6770(2) 0.0792(10) Uani 1 1 d . . . H20A H -0.0046 0.8160 0.6682 0.119 Uiso 1 1 calc R . . H20B H 0.0807 0.8067 0.6656 0.119 Uiso 1 1 calc R . . H20C H 0.0565 0.7701 0.7303 0.119 Uiso 1 1 calc R . . C21 C 0.09275(16) 0.52723(14) 0.66115(16) 0.0503(7) Uani 1 1 d . . . C22 C 0.01970(17) 0.49426(13) 0.62619(16) 0.0505(7) Uani 1 1 d . . . C23 C 0.0105(2) 0.44457(15) 0.57094(17) 0.0614(8) Uani 1 1 d . . . H23 H -0.0383 0.4237 0.5482 0.074 Uiso 1 1 calc R . . C24 C 0.0747(2) 0.42513(16) 0.54870(19) 0.0695(9) Uani 1 1 d . . . H24 H 0.0684 0.3914 0.5113 0.083 Uiso 1 1 calc R . . C25 C 0.1455(2) 0.45524(17) 0.58144(19) 0.0697(9) Uani 1 1 d . . . H25 H 0.1876 0.4419 0.5663 0.084 Uiso 1 1 calc R . . C26 C 0.15684(18) 0.50673(16) 0.63826(17) 0.0608(8) Uani 1 1 d . . . C27 C 0.2318(2) 0.5366(2) 0.6724(2) 0.0823(11) Uani 1 1 d . C . H27 H 0.2717 0.5211 0.6551 0.099 Uiso 1 1 calc R . . C30 C 0.27691(18) 0.71089(16) 0.88764(19) 0.0684(9) Uani 1 1 d . C . H30 H 0.3259 0.7298 0.9143 0.082 Uiso 1 1 calc R . . C31 C 0.21228(16) 0.73351(15) 0.90908(16) 0.0543(7) Uani 1 1 d . . . C32 C 0.22481(19) 0.78358(16) 0.96757(18) 0.0658(9) Uani 1 1 d . . . H32 H 0.2750 0.8015 0.9913 0.079 Uiso 1 1 calc R . . C33 C 0.1648(2) 0.80570(16) 0.98937(18) 0.0658(8) Uani 1 1 d . . . H33 H 0.1738 0.8385 1.0283 0.079 Uiso 1 1 calc R . . C34 C 0.08905(18) 0.77938(14) 0.95350(16) 0.0555(7) Uani 1 1 d . . . H34 H 0.0479 0.7948 0.9689 0.067 Uiso 1 1 calc R . . C35 C 0.07477(15) 0.73112(13) 0.89590(15) 0.0449(6) Uani 1 1 d . . . C36 C 0.13648(15) 0.70640(13) 0.87265(15) 0.0460(6) Uani 1 1 d . . . C37 C -0.11379(19) 0.48634(17) 0.6246(2) 0.0693(9) Uani 1 1 d . . . H37A H -0.1270 0.4750 0.5700 0.083 Uiso 1 1 calc R . . H37B H -0.1531 0.5181 0.6294 0.083 Uiso 1 1 calc R . . C38 C -0.1158(3) 0.42326(19) 0.6689(2) 0.0977(13) Uani 1 1 d . . . H38A H -0.0778 0.3912 0.6633 0.147 Uiso 1 1 calc R . . H38B H -0.1674 0.4034 0.6493 0.147 Uiso 1 1 calc R . . H38C H -0.1033 0.4344 0.7229 0.147 Uiso 1 1 calc R . . C39 C -0.06663(18) 0.73440(17) 0.86225(19) 0.0670(9) Uani 1 1 d . . . H39A H -0.0576 0.7479 0.9157 0.080 Uiso 1 1 calc R . . H39B H -0.1099 0.7020 0.8472 0.080 Uiso 1 1 calc R . . C40 C -0.0888(2) 0.79518(19) 0.8117(2) 0.0890(12) Uani 1 1 d . . . H40A H -0.0460 0.8273 0.8262 0.133 Uiso 1 1 calc R . . H40B H -0.1346 0.8160 0.8174 0.133 Uiso 1 1 calc R . . H40C H -0.1001 0.7818 0.7585 0.133 Uiso 1 1 calc R . . C41 C 0.46388(15) 0.79028(16) 0.59267(17) 0.0572(7) Uani 1 1 d . . . C42 C 0.45178(19) 0.72239(19) 0.6027(2) 0.0809(10) Uani 1 1 d . . . H42 H 0.4367 0.7094 0.6445 0.097 Uiso 1 1 calc R . . C43 C 0.4614(3) 0.6712(3) 0.5520(4) 0.1162(17) Uani 1 1 d . . . H43 H 0.4522 0.6256 0.5604 0.139 Uiso 1 1 calc R . . C44 C 0.4840(3) 0.6890(3) 0.4908(4) 0.122(2) Uani 1 1 d . . . H44 H 0.4900 0.6557 0.4569 0.147 Uiso 1 1 calc R . . C45 C 0.4979(2) 0.7552(3) 0.4794(2) 0.1125(19) Uani 1 1 d . . . H45 H 0.5140 0.7675 0.4380 0.135 Uiso 1 1 calc R . . C46 C 0.48812(18) 0.8050(2) 0.52923(19) 0.0759(10) Uani 1 1 d . . . H46 H 0.4981 0.8502 0.5202 0.091 Uiso 1 1 calc R . . C47 C 0.54844(16) 0.84158(15) 0.72264(17) 0.0534(7) Uani 1 1 d . . . C48 C 0.61609(17) 0.86797(17) 0.7140(2) 0.0683(9) Uani 1 1 d . . . H48 H 0.6112 0.8942 0.6702 0.082 Uiso 1 1 calc R . . C49 C 0.69136(18) 0.8570(2) 0.7679(2) 0.0850(12) Uani 1 1 d . . . H49 H 0.7354 0.8755 0.7599 0.102 Uiso 1 1 calc R . . C50 C 0.6995(2) 0.8184(2) 0.8331(3) 0.0950(13) Uani 1 1 d . . . H50 H 0.7490 0.8110 0.8700 0.114 Uiso 1 1 calc R . . C51 C 0.6351(2) 0.7914(2) 0.8430(2) 0.0886(11) Uani 1 1 d . . . H51 H 0.6405 0.7650 0.8868 0.106 Uiso 1 1 calc R . . C52 C 0.56123(18) 0.80224(17) 0.78923(18) 0.0679(9) Uani 1 1 d . . . H52 H 0.5181 0.7824 0.7977 0.081 Uiso 1 1 calc R . . C53 C 0.39012(15) 0.83778(14) 0.69037(16) 0.0492(6) Uani 1 1 d . . . C54 C 0.39144(19) 0.86625(17) 0.76037(19) 0.0661(8) Uani 1 1 d . . . H54 H 0.4364 0.8898 0.7900 0.079 Uiso 1 1 calc R . . C55 C 0.3293(2) 0.86143(19) 0.7885(2) 0.0735(10) Uani 1 1 d . . . H55 H 0.3335 0.8806 0.8363 0.088 Uiso 1 1 calc R . . C56 C 0.2618(2) 0.82828(19) 0.7454(2) 0.0758(10) Uani 1 1 d . . . H56 H 0.2197 0.8248 0.7636 0.091 Uiso 1 1 calc R . . C57 C 0.25664(18) 0.80045(18) 0.6757(2) 0.0734(9) Uani 1 1 d . . . H57 H 0.2108 0.7781 0.6460 0.088 Uiso 1 1 calc R . . C58 C 0.31929(16) 0.80536(17) 0.64907(19) 0.0630(8) Uani 1 1 d . . . H58 H 0.3141 0.7861 0.6011 0.076 Uiso 1 1 calc R . . C59 C 0.44318(17) 0.92394(17) 0.61351(18) 0.0600(8) Uani 1 1 d . . . C60 C 0.3796(2) 0.9312(2) 0.5439(2) 0.0819(10) Uani 1 1 d . . . H60 H 0.3511 0.8927 0.5209 0.098 Uiso 1 1 calc R . . C61 C 0.3578(3) 0.9941(3) 0.5082(3) 0.1166(17) Uani 1 1 d . . . H61 H 0.3149 0.9973 0.4623 0.140 Uiso 1 1 calc R . . C62 C 0.3994(3) 1.0514(3) 0.5403(4) 0.128(2) Uani 1 1 d . . . H62 H 0.3858 1.0933 0.5153 0.154 Uiso 1 1 calc R . . C63 C 0.4606(3) 1.0474(2) 0.6088(4) 0.1203(19) Uani 1 1 d . . . H63 H 0.4881 1.0866 0.6314 0.144 Uiso 1 1 calc R . . C64 C 0.48151(19) 0.98421(18) 0.6443(2) 0.0809(11) Uani 1 1 d . . . H64 H 0.5233 0.9822 0.6912 0.097 Uiso 1 1 calc R . . C9A C -0.3425(5) 0.6213(4) 0.7660(5) 0.070(2) Uiso 0.50 1 d PD B 1 H9A1 H -0.3965 0.6360 0.7403 0.084 Uiso 0.50 1 calc PR B 1 H9A2 H -0.3221 0.6427 0.8167 0.084 Uiso 0.50 1 calc PR B 1 C28A C 0.3366(5) 0.5892(5) 0.7716(6) 0.107(3) Uiso 0.50 1 d PD C 1 H28A H 0.3680 0.5864 0.7380 0.129 Uiso 0.50 1 calc PR C 1 H28B H 0.3531 0.5535 0.8106 0.129 Uiso 0.50 1 calc PR C 1 C29A C 0.3444(4) 0.6590(4) 0.8094(5) 0.070(2) Uiso 0.50 1 d PD C 1 H29A H 0.3928 0.6619 0.8537 0.084 Uiso 0.50 1 calc PR C 1 H29B H 0.3448 0.6945 0.7725 0.084 Uiso 0.50 1 calc PR C 1 C9B C -0.3614(5) 0.6171(4) 0.7319(6) 0.090(3) Uiso 0.50 1 d PD B 2 H9B1 H -0.3751 0.6494 0.7654 0.108 Uiso 0.50 1 calc PR B 2 H9B2 H -0.4057 0.6123 0.6839 0.108 Uiso 0.50 1 calc PR B 2 C28B C 0.3269(4) 0.6253(4) 0.7438(4) 0.0668(18) Uiso 0.50 1 d PD C 2 H28C H 0.3675 0.5998 0.7321 0.080 Uiso 0.50 1 calc PR C 2 H28D H 0.3177 0.6681 0.7154 0.080 Uiso 0.50 1 calc PR C 2 C29B C 0.3487(5) 0.6373(4) 0.8320(4) 0.077(2) Uiso 0.50 1 d PD C 2 H29C H 0.3922 0.6692 0.8515 0.092 Uiso 0.50 1 calc PR C 2 H29D H 0.3619 0.5949 0.8610 0.092 Uiso 0.50 1 calc PR C 2 N1 N -0.25176(16) 0.53471(15) 0.80458(18) 0.0793(8) Uani 1 1 d . B . N2 N -0.29136(16) 0.63853(14) 0.7167(2) 0.0804(9) Uani 1 1 d D . . N3 N 0.25028(15) 0.58334(16) 0.72545(18) 0.0787(8) Uani 1 1 d D . . N4 N 0.27370(13) 0.66682(14) 0.83495(15) 0.0662(7) Uani 1 1 d D . . Na1 Na -0.00912(6) 0.60527(5) 0.75819(6) 0.0477(3) Uani 1 1 d . . . Ni1 Ni -0.19872(2) 0.59062(2) 0.75792(2) 0.05823(13) Uani 1 1 d . B . Ni2 Ni 0.186000(19) 0.621290(19) 0.77264(2) 0.05222(12) Uani 1 1 d . B . O1 O -0.10343(11) 0.54947(9) 0.80466(11) 0.0550(5) Uani 1 1 d . B . O2 O -0.14590(11) 0.64034(9) 0.70579(11) 0.0545(5) Uani 1 1 d . B . O3 O 0.04329(12) 0.51429(10) 0.86134(11) 0.0594(5) Uani 1 1 d . B . O4 O -0.05101(11) 0.68743(10) 0.64087(12) 0.0593(5) Uani 1 1 d . B . O5 O 0.09749(10) 0.57496(9) 0.71294(11) 0.0525(5) Uani 1 1 d . B . O6 O 0.11917(10) 0.65990(9) 0.81728(11) 0.0492(4) Uani 1 1 d . B . O7 O -0.03840(11) 0.51821(10) 0.65169(11) 0.0580(5) Uani 1 1 d . B . O8 O 0.00320(10) 0.70183(9) 0.85758(11) 0.0521(5) Uani 1 1 d . B . 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 B1 0.0366(15) 0.060(2) 0.0508(19) -0.0005(15) 0.0136(14) 0.0008(14) C1 0.084(2) 0.0421(16) 0.0520(17) -0.0118(13) 0.0369(16) -0.0203(15) C2 0.091(2) 0.0369(15) 0.0446(17) -0.0023(13) 0.0259(16) -0.0105(15) C3 0.118(3) 0.0449(17) 0.0492(18) 0.0001(15) 0.0253(19) -0.0131(18) C4 0.150(4) 0.053(2) 0.053(2) -0.0022(16) 0.042(3) -0.025(2) C5 0.141(4) 0.059(2) 0.062(2) -0.0128(18) 0.058(2) -0.043(2) C6 0.095(3) 0.0587(19) 0.065(2) -0.0197(17) 0.0445(19) -0.0297(18) C7 0.116(3) 0.082(2) 0.084(3) -0.024(2) 0.068(2) -0.047(2) C8 0.067(2) 0.147(4) 0.179(5) -0.006(4) 0.074(3) -0.025(3) C10 0.0379(16) 0.075(2) 0.130(3) -0.020(2) 0.0151(19) 0.0025(16) C11 0.0427(16) 0.0600(19) 0.081(2) -0.0118(17) 0.0002(16) -0.0013(14) C12 0.0475(19) 0.074(2) 0.103(3) -0.001(2) -0.013(2) 0.0083(17) C13 0.068(2) 0.067(2) 0.083(3) 0.0055(19) -0.018(2) 0.0086(19) C14 0.077(2) 0.0538(18) 0.0591(19) 0.0028(15) 0.0065(17) 0.0022(16) C15 0.0485(16) 0.0451(16) 0.0551(17) -0.0033(13) 0.0064(13) 0.0025(12) C16 0.0444(15) 0.0461(16) 0.0524(17) -0.0113(13) 0.0046(13) -0.0007(12) C17 0.069(2) 0.0585(19) 0.067(2) 0.0138(16) 0.0133(17) 0.0044(16) C18 0.099(3) 0.072(2) 0.089(3) 0.011(2) 0.033(2) 0.022(2) C19 0.073(2) 0.090(3) 0.073(2) 0.034(2) 0.0464(18) 0.0249(19) C20 0.064(2) 0.076(2) 0.092(3) 0.031(2) 0.0187(19) -0.0078(18) C21 0.0567(17) 0.0478(16) 0.0514(16) 0.0108(13) 0.0248(14) 0.0131(13) C22 0.0616(18) 0.0432(15) 0.0511(16) 0.0068(13) 0.0248(14) 0.0083(13) C23 0.081(2) 0.0506(18) 0.0543(18) 0.0066(15) 0.0248(16) 0.0041(16) C24 0.106(3) 0.0540(19) 0.057(2) 0.0043(15) 0.038(2) 0.0205(19) C25 0.087(2) 0.072(2) 0.063(2) 0.0094(17) 0.0418(19) 0.0292(19) C26 0.0617(19) 0.068(2) 0.0579(19) 0.0105(16) 0.0272(15) 0.0214(16) C27 0.062(2) 0.111(3) 0.090(3) -0.003(2) 0.0450(19) 0.018(2) C30 0.0434(16) 0.068(2) 0.082(2) 0.0071(17) 0.0066(15) -0.0030(15) C31 0.0452(15) 0.0544(17) 0.0542(17) 0.0116(14) 0.0050(13) 0.0020(13) C32 0.0554(19) 0.064(2) 0.0591(19) 0.0066(16) -0.0051(15) -0.0078(15) C33 0.073(2) 0.0617(19) 0.0496(18) -0.0050(15) 0.0032(16) -0.0078(17) C34 0.0651(19) 0.0535(17) 0.0483(16) 0.0057(13) 0.0197(14) 0.0020(14) C35 0.0494(15) 0.0378(14) 0.0451(15) 0.0093(11) 0.0131(12) -0.0009(12) C36 0.0470(15) 0.0423(15) 0.0451(15) 0.0100(13) 0.0111(12) 0.0009(12) C37 0.066(2) 0.068(2) 0.074(2) -0.0167(17) 0.0245(17) -0.0090(17) C38 0.147(4) 0.082(3) 0.084(3) -0.020(2) 0.065(3) -0.037(3) C39 0.0522(18) 0.081(2) 0.071(2) -0.0275(18) 0.0259(16) -0.0087(16) C40 0.071(2) 0.092(3) 0.089(3) -0.024(2) 0.007(2) 0.019(2) C41 0.0361(14) 0.070(2) 0.0608(19) -0.0054(16) 0.0112(13) 0.0087(14) C42 0.056(2) 0.084(3) 0.097(3) -0.018(2) 0.0187(19) 0.0104(18) C43 0.077(3) 0.090(3) 0.162(5) -0.042(3) 0.015(3) 0.009(2) C44 0.079(3) 0.146(5) 0.121(4) -0.070(4) 0.006(3) 0.038(3) C45 0.064(2) 0.194(6) 0.068(3) -0.035(3) 0.008(2) 0.050(3) C46 0.0506(18) 0.113(3) 0.063(2) -0.011(2) 0.0179(16) 0.0200(18) C47 0.0421(15) 0.0597(18) 0.0590(18) -0.0045(15) 0.0180(13) 0.0020(13) C48 0.0441(17) 0.083(2) 0.076(2) 0.0021(18) 0.0184(16) 0.0038(16) C49 0.0385(18) 0.101(3) 0.110(3) -0.009(2) 0.0175(19) -0.0036(17) C50 0.054(2) 0.113(3) 0.094(3) -0.002(3) -0.005(2) 0.010(2) C51 0.067(2) 0.106(3) 0.080(3) 0.019(2) 0.009(2) 0.011(2) C52 0.0506(18) 0.080(2) 0.065(2) 0.0077(18) 0.0093(16) 0.0030(16) C53 0.0424(15) 0.0548(16) 0.0487(16) 0.0046(13) 0.0132(12) 0.0051(12) C54 0.0539(18) 0.079(2) 0.065(2) -0.0075(17) 0.0191(16) -0.0025(16) C55 0.070(2) 0.094(3) 0.064(2) 0.0001(18) 0.0328(18) 0.0128(19) C56 0.055(2) 0.093(3) 0.090(3) 0.016(2) 0.0381(19) 0.0096(18) C57 0.0452(17) 0.088(2) 0.088(3) 0.000(2) 0.0244(17) -0.0004(16) C58 0.0445(16) 0.079(2) 0.064(2) -0.0050(16) 0.0168(15) -0.0015(15) C59 0.0436(16) 0.075(2) 0.069(2) 0.0109(16) 0.0288(15) 0.0105(15) C60 0.066(2) 0.098(3) 0.079(2) 0.021(2) 0.0217(19) 0.022(2) C61 0.074(3) 0.160(5) 0.118(4) 0.069(4) 0.036(3) 0.047(3) C62 0.089(3) 0.109(4) 0.214(6) 0.082(4) 0.087(4) 0.034(3) C63 0.065(3) 0.083(3) 0.224(6) 0.046(3) 0.063(3) 0.011(2) C64 0.0535(19) 0.069(2) 0.124(3) 0.016(2) 0.036(2) 0.0024(17) N1 0.0693(18) 0.0786(19) 0.108(2) -0.0186(17) 0.0532(17) -0.0256(15) N2 0.0485(15) 0.079(2) 0.122(2) -0.0166(18) 0.0401(16) -0.0098(13) N3 0.0435(15) 0.107(2) 0.090(2) -0.0154(17) 0.0294(14) 0.0019(14) N4 0.0358(12) 0.0789(18) 0.0829(18) 0.0045(15) 0.0188(12) 0.0051(12) Na1 0.0405(6) 0.0468(6) 0.0583(7) 0.0035(5) 0.0201(5) 0.0012(4) Ni1 0.0481(2) 0.0574(2) 0.0779(3) -0.0145(2) 0.0329(2) -0.01272(17) Ni2 0.03600(19) 0.0586(2) 0.0631(3) 0.00786(18) 0.01825(17) 0.00725(16) O1 0.0576(12) 0.0524(11) 0.0623(12) 0.0014(9) 0.0300(10) -0.0088(9) O2 0.0451(11) 0.0538(11) 0.0657(13) 0.0026(9) 0.0203(10) -0.0001(9) O3 0.0661(13) 0.0540(11) 0.0585(12) 0.0135(10) 0.0216(10) 0.0012(10) O4 0.0554(12) 0.0551(12) 0.0699(13) 0.0144(10) 0.0244(10) 0.0081(9) O5 0.0428(10) 0.0578(11) 0.0607(12) -0.0031(9) 0.0225(9) 0.0064(9) O6 0.0383(10) 0.0482(11) 0.0612(12) -0.0002(9) 0.0170(9) 0.0016(8) O7 0.0525(11) 0.0567(12) 0.0693(13) -0.0116(10) 0.0265(10) -0.0026(9) O8 0.0473(11) 0.0493(11) 0.0634(12) -0.0078(9) 0.0236(9) -0.0033(9) _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 B1 C41 1.632(3) . ? B1 C53 1.634(3) . ? B1 C59 1.638(3) . ? B1 C47 1.640(3) . ? C1 O1 1.323(3) . ? C1 C6 1.386(4) . ? C1 C2 1.410(5) . ? C2 O3 1.368(3) . ? C2 C3 1.373(4) . ? C3 C4 1.388(5) . ? C3 H3 0.9300 . ? C4 C5 1.340(6) . ? C4 H4 0.9300 . ? C5 C6 1.418(5) . ? C5 H5 0.9300 . ? C6 C7 1.426(5) . ? C7 N1 1.291(4) . ? C7 H7 0.9300 . ? C8 C9B 1.541(15) . ? C8 N1 1.482(4) . ? C8 C9A 1.450(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 N2 1.277(4) . ? C10 C11 1.426(5) . ? C10 H10 0.9300 . ? C11 C12 1.406(5) . ? C11 C16 1.410(4) . ? C12 C13 1.349(6) . ? C12 H12 0.9300 . ? C13 C14 1.393(5) . ? C13 H13 0.9300 . ? C14 C15 1.377(4) . ? C14 H14 0.9300 . ? C15 O4 1.369(3) . ? C15 C16 1.398(4) . ? C16 O2 1.315(3) . ? C17 O3 1.445(3) . ? C17 C18 1.484(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.448(3) . ? C19 C20 1.484(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.312(3) . ? C21 C22 1.411(4) . ? C21 C26 1.416(4) . ? C22 O7 1.368(3) . ? C22 C23 1.371(4) . ? C23 C24 1.407(5) . ? C23 H23 0.9300 . ? C24 C25 1.348(5) . ? C24 H24 0.9300 . ? C25 C26 1.411(5) . ? C25 H25 0.9300 . ? C26 C27 1.409(5) . ? C27 N3 1.292(4) . ? C27 H27 0.9300 . ? C30 N4 1.280(4) . ? C30 C31 1.422(4) . ? C30 H30 0.9300 . ? C31 C36 1.406(3) . ? C31 C32 1.411(5) . ? C32 C33 1.347(5) . ? C32 H32 0.9300 . ? C33 C34 1.399(4) . ? C33 H33 0.9300 . ? C34 C35 1.372(3) . ? C34 H34 0.9300 . ? C35 O8 1.368(3) . ? C35 C36 1.407(4) . ? C36 O6 1.318(3) . ? C37 O7 1.424(4) . ? C37 C38 1.484(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O8 1.441(4) . ? C39 C40 1.476(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.369(5) . ? C41 C46 1.403(5) . ? C42 C43 1.415(6) . ? C42 H42 0.9300 . ? C43 C44 1.362(8) . ? C43 H43 0.9300 . ? C44 C45 1.350(8) . ? C44 H44 0.9300 . ? C45 C46 1.385(6) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.384(4) . ? C47 C52 1.392(4) . ? C48 C49 1.397(5) . ? C48 H48 0.9300 . ? C49 C50 1.377(6) . ? C49 H49 0.9300 . ? C50 C51 1.344(6) . ? C50 H50 0.9300 . ? C51 C52 1.377(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.389(4) . ? C53 C58 1.396(4) . ? C54 C55 1.388(5) . ? C54 H54 0.9300 . ? C55 C56 1.369(5) . ? C55 H55 0.9300 . ? C56 C57 1.359(5) . ? C56 H56 0.9300 . ? C57 C58 1.380(4) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C64 1.387(5) . ? C59 C60 1.401(5) . ? C60 C61 1.386(6) . ? C60 H60 0.9300 . ? C61 C62 1.367(7) . ? C61 H61 0.9300 . ? C62 C63 1.360(8) . ? C62 H62 0.9300 . ? C63 C64 1.389(6) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C9A N2 1.531(14) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C28A N3 1.503(10) . ? C28A C29A 1.515(13) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A N4 1.510(10) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C9B N2 1.446(15) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C28B C29B 1.542(14) . ? C28B N3 1.544(8) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29B N4 1.491(14) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? N1 Ni1 1.844(3) . ? N2 Ni1 1.840(3) . ? N3 Ni2 1.824(3) . ? N4 Ni2 1.836(3) . ? Na1 O1 2.409(2) . ? Na1 O5 2.414(2) . ? Na1 O2 2.424(2) . ? Na1 O6 2.443(2) . ? Na1 O7 2.505(2) . ? Na1 O3 2.531(2) . ? Na1 O4 2.580(2) . ? Na1 O8 2.579(2) . ? Na1 Ni1 3.4338(12) . ? Na1 Ni2 3.4561(12) . ? Ni1 O1 1.827(2) . ? Ni1 O2 1.840(2) . ? Ni2 O6 1.8346(19) . ? Ni2 O5 1.838(2) . ? 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 C41 B1 C53 113.4(2) . . ? C41 B1 C59 110.5(2) . . ? C53 B1 C59 104.06(18) . . ? C41 B1 C47 102.53(18) . . ? C53 B1 C47 112.1(2) . . ? C59 B1 C47 114.6(2) . . ? O1 C1 C6 124.8(3) . . ? O1 C1 C2 117.9(2) . . ? C6 C1 C2 117.3(3) . . ? O3 C2 C3 125.1(3) . . ? O3 C2 C1 114.0(2) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 121.0(4) . . ? C1 C6 C7 120.1(3) . . ? C5 C6 C7 118.9(4) . . ? N1 C7 C6 126.3(3) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? C9B C8 N1 114.8(9) . . ? C9B C8 C9A 23(2) . . ? N1 C8 C9A 103.0(8) . . ? C9B C8 H8A 119.9 . . ? N1 C8 H8A 111.2 . . ? C9A C8 H8A 111.2 . . ? C9B C8 H8B 88.1 . . ? N1 C8 H8B 111.2 . . ? C9A C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? N2 C10 C11 125.4(3) . . ? N2 C10 H10 117.3 . . ? C11 C10 H10 117.3 . . ? C12 C11 C16 119.6(3) . . ? C12 C11 C10 119.3(3) . . ? C16 C11 C10 121.0(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.9(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? O4 C15 C14 125.3(3) . . ? O4 C15 C16 113.9(2) . . ? C14 C15 C16 120.8(3) . . ? O2 C16 C15 117.7(2) . . ? O2 C16 C11 123.8(3) . . ? C15 C16 C11 118.5(3) . . ? O3 C17 C18 111.6(3) . . ? O3 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O3 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 112.4(3) . . ? O4 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? O4 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C22 118.3(2) . . ? O5 C21 C26 123.8(3) . . ? C22 C21 C26 117.9(3) . . ? O7 C22 C23 125.4(3) . . ? O7 C22 C21 113.3(2) . . ? C23 C22 C21 121.2(3) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 121.1(3) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 119.9(3) . . ? C27 C26 C21 120.6(3) . . ? C25 C26 C21 119.5(3) . . ? N3 C27 C26 126.1(3) . . ? N3 C27 H27 116.9 . . ? C26 C27 H27 116.9 . . ? N4 C30 C31 125.9(3) . . ? N4 C30 H30 117.0 . . ? C31 C30 H30 117.0 . . ? C36 C31 C32 120.0(3) . . ? C36 C31 C30 120.6(3) . . ? C32 C31 C30 119.4(3) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? O8 C35 C34 125.4(2) . . ? O8 C35 C36 114.1(2) . . ? C34 C35 C36 120.5(2) . . ? O6 C36 C31 124.2(2) . . ? O6 C36 C35 117.7(2) . . ? C31 C36 C35 118.1(2) . . ? O7 C37 C38 111.9(3) . . ? O7 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? O7 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 112.0(3) . . ? O8 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O8 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 114.8(3) . . ? C42 C41 B1 122.9(3) . . ? C46 C41 B1 121.9(3) . . ? C41 C42 C43 122.6(5) . . ? C41 C42 H42 118.7 . . ? C43 C42 H42 118.7 . . ? C44 C43 C42 119.8(5) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 123.1(5) . . ? C45 C46 H46 118.5 . . ? C41 C46 H46 118.5 . . ? C48 C47 C52 114.6(3) . . ? C48 C47 B1 122.7(3) . . ? C52 C47 B1 122.3(2) . . ? C47 C48 C49 123.1(4) . . ? C47 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C50 C49 C48 119.1(4) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 119.4(4) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 120.9(4) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C47 122.8(3) . . ? C51 C52 H52 118.6 . . ? C47 C52 H52 118.6 . . ? C54 C53 C58 113.9(3) . . ? C54 C53 B1 122.7(2) . . ? C58 C53 B1 123.1(2) . . ? C53 C54 C55 123.5(3) . . ? C53 C54 H54 118.2 . . ? C55 C54 H54 118.2 . . ? C56 C55 C54 119.5(3) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C57 C56 C55 119.6(3) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 120.1(3) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C57 C58 C53 123.4(3) . . ? C57 C58 H58 118.3 . . ? C53 C58 H58 118.3 . . ? C64 C59 C60 115.1(3) . . ? C64 C59 B1 125.5(3) . . ? C60 C59 B1 119.2(3) . . ? C61 C60 C59 122.1(4) . . ? C61 C60 H60 118.9 . . ? C59 C60 H60 118.9 . . ? C62 C61 C60 120.0(5) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C63 C62 C61 120.2(5) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C62 C63 C64 119.2(5) . . ? C62 C63 H63 120.4 . . ? C64 C63 H63 120.4 . . ? C59 C64 C63 123.3(4) . . ? C59 C64 H64 118.3 . . ? C63 C64 H64 118.3 . . ? N2 C9A C8 103.8(10) . . ? N2 C9A H9A1 111.0 . . ? C8 C9A H9A1 111.0 . . ? N2 C9A H9A2 111.0 . . ? C8 C9A H9A2 111.0 . . ? H9A1 C9A H9A2 109.0 . . ? N3 C28A C29A 104.0(8) . . ? N3 C28A H28A 110.9 . . ? C29A C28A H28A 110.9 . . ? N3 C28A H28B 110.9 . . ? C29A C28A H28B 110.9 . . ? H28A C28A H28B 109.0 . . ? N4 C29A C28A 106.0(8) . . ? N4 C29A H29A 110.5 . . ? C28A C29A H29A 110.5 . . ? N4 C29A H29B 110.5 . . ? C28A C29A H29B 110.5 . . ? H29A C29A H29B 108.7 . . ? C8 C9B N2 103.5(11) . . ? C8 C9B H9B1 111.1 . . ? N2 C9B H9B1 111.1 . . ? C8 C9B H9B2 111.1 . . ? N2 C9B H9B2 111.1 . . ? H9B1 C9B H9B2 109.0 . . ? C29B C28B N3 101.5(9) . . ? C29B C28B H28C 111.5 . . ? N3 C28B H28C 111.5 . . ? C29B C28B H28D 111.5 . . ? N3 C28B H28D 111.5 . . ? H28C C28B H28D 109.3 . . ? C28B C29B N4 100.6(11) . . ? C28B C29B H29C 111.6 . . ? N4 C29B H29C 111.6 . . ? C28B C29B H29D 111.6 . . ? N4 C29B H29D 111.6 . . ? H29C C29B H29D 109.4 . . ? C7 N1 C8 122.5(3) . . ? C7 N1 Ni1 126.44(19) . . ? C8 N1 Ni1 110.9(2) . . ? C10 N2 C9A 124.3(7) . . ? C10 N2 C9B 111.8(8) . . ? C9A N2 C9B 23(2) . . ? C10 N2 Ni1 127.4(2) . . ? C9A N2 Ni1 107.1(8) . . ? C9B N2 Ni1 120.4(8) . . ? C27 N3 C28A 115.4(5) . . ? C27 N3 C28B 121.6(4) . . ? C28A N3 C28B 32.5(5) . . ? C27 N3 Ni2 126.92(19) . . ? C28A N3 Ni2 114.1(5) . . ? C28B N3 Ni2 110.3(4) . . ? C30 N4 C29A 118.4(5) . . ? C30 N4 C29B 118.7(6) . . ? C29A N4 C29B 22.3(12) . . ? C30 N4 Ni2 127.07(17) . . ? C29A N4 Ni2 113.6(5) . . ? C29B N4 Ni2 113.1(6) . . ? O1 Na1 O5 138.75(8) . . ? O1 Na1 O2 61.34(7) . . ? O5 Na1 O2 139.29(8) . . ? O1 Na1 O6 136.06(8) . . ? O5 Na1 O6 60.84(7) . . ? O2 Na1 O6 137.35(8) . . ? O1 Na1 O7 88.78(8) . . ? O5 Na1 O7 63.12(7) . . ? O2 Na1 O7 88.20(7) . . ? O6 Na1 O7 123.96(8) . . ? O1 Na1 O3 63.11(7) . . ? O5 Na1 O3 86.76(8) . . ? O2 Na1 O3 124.44(8) . . ? O6 Na1 O3 85.47(7) . . ? O7 Na1 O3 91.56(8) . . ? O1 Na1 O4 122.28(8) . . ? O5 Na1 O4 84.83(7) . . ? O2 Na1 O4 61.60(7) . . ? O6 Na1 O4 93.44(7) . . ? O7 Na1 O4 81.54(8) . . ? O3 Na1 O4 170.91(8) . . ? O1 Na1 O8 89.14(7) . . ? O5 Na1 O8 122.31(8) . . ? O2 Na1 O8 84.41(7) . . ? O6 Na1 O8 61.74(7) . . ? O7 Na1 O8 172.42(8) . . ? O3 Na1 O8 93.99(7) . . ? O4 Na1 O8 93.43(8) . . ? O1 Na1 Ni1 30.48(5) . . ? O5 Na1 Ni1 152.88(6) . . ? O2 Na1 Ni1 30.92(5) . . ? O6 Na1 Ni1 146.26(6) . . ? O7 Na1 Ni1 89.77(5) . . ? O3 Na1 Ni1 93.53(6) . . ? O4 Na1 Ni1 92.37(5) . . ? O8 Na1 Ni1 84.75(5) . . ? O1 Na1 Ni2 147.04(6) . . ? O5 Na1 Ni2 30.39(5) . . ? O2 Na1 Ni2 151.54(6) . . ? O6 Na1 Ni2 30.52(5) . . ? O7 Na1 Ni2 93.48(5) . . ? O3 Na1 Ni2 83.95(6) . . ? O4 Na1 Ni2 90.53(6) . . ? O8 Na1 Ni2 92.23(5) . . ? Ni1 Na1 Ni2 175.93(4) . . ? O1 Ni1 O2 84.47(9) . . ? O1 Ni1 N2 174.90(12) . . ? O2 Ni1 N2 94.47(12) . . ? O1 Ni1 N1 94.40(12) . . ? O2 Ni1 N1 175.13(11) . . ? N2 Ni1 N1 87.07(15) . . ? O1 Ni1 Na1 41.97(6) . . ? O2 Ni1 Na1 42.60(6) . . ? N2 Ni1 Na1 136.45(10) . . ? N1 Ni1 Na1 136.36(11) . . ? N3 Ni2 N4 86.45(13) . . ? N3 Ni2 O6 178.32(12) . . ? N4 Ni2 O6 94.75(11) . . ? N3 Ni2 O5 94.74(12) . . ? N4 Ni2 O5 178.24(11) . . ? O6 Ni2 O5 84.09(9) . . ? N3 Ni2 Na1 136.33(10) . . ? N4 Ni2 Na1 137.10(9) . . ? O6 Ni2 Na1 42.56(6) . . ? O5 Ni2 Na1 41.65(6) . . ? C1 O1 Ni1 127.72(15) . . ? C1 O1 Na1 124.64(15) . . ? Ni1 O1 Na1 107.54(9) . . ? C16 O2 Ni1 127.48(13) . . ? C16 O2 Na1 126.03(13) . . ? Ni1 O2 Na1 106.48(9) . . ? C2 O3 C17 119.3(2) . . ? C2 O3 Na1 120.34(14) . . ? C17 O3 Na1 120.25(14) . . ? C15 O4 C19 118.99(19) . . ? C15 O4 Na1 120.01(13) . . ? C19 O4 Na1 116.37(14) . . ? C21 O5 Ni2 127.56(13) . . ? C21 O5 Na1 123.98(13) . . ? Ni2 O5 Na1 107.96(9) . . ? C36 O6 Ni2 127.37(18) . . ? C36 O6 Na1 125.66(17) . . ? Ni2 O6 Na1 106.93(9) . . ? C22 O7 C37 119.0(2) . . ? C22 O7 Na1 121.00(13) . . ? C37 O7 Na1 119.48(18) . . ? C35 O8 C39 118.5(2) . . ? C35 O8 Na1 120.50(16) . . ? C39 O8 Na1 119.94(17) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 281 59 ' ' 2 0.500 0.500 0.500 281 60 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.492 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.044 #END=== data_4 _database_code_depnum_ccdc_archive 'CCDC 813959' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H64 B1 N4 Ni2 O8 Rb1' _chemical_formula_weight 1230.89 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' B B 0.0013 0.0007 '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' Rb Rb -0.9393 2.9676 '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 16.0343(19) _cell_length_b 16.0435(19) _cell_length_c 25.379(3) _cell_angle_alpha 83.810(2) _cell_angle_beta 83.857(2) _cell_angle_gamma 68.346(2) _cell_volume 6016.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8507 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 19.87 _exptl_crystal_description square _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7553 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61237 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.33 _reflns_number_total 23600 _reflns_number_gt 11717 _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.SQUEEZE was performed to get rid of solvent molecule acetone as the SQEEZE details gave a void volume of 157 A 3 and electron per unit cell = 32. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.1000P] 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 23600 _refine_ls_number_parameters 1456 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.906 _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 B1 B 0.3872(3) 0.9758(2) 0.34744(15) 0.0480(10) Uani 1 1 d . . . B2 B 0.0293(3) 0.3298(3) 0.86839(16) 0.0523(11) Uani 1 1 d . . . C1 C 0.5433(3) 0.2676(3) 0.05510(14) 0.0729(12) Uani 1 1 d . . . C2 C 0.6201(4) 0.1883(4) 0.04915(15) 0.0852(14) Uani 1 1 d . . . C3 C 0.6111(5) 0.1078(4) 0.04076(18) 0.1165(19) Uani 1 1 d . . . H3 H 0.6619 0.0559 0.0371 0.140 Uiso 1 1 calc R . . C4 C 0.5260(6) 0.1050(5) 0.0379(2) 0.130(3) Uani 1 1 d . . . H4 H 0.5204 0.0511 0.0320 0.156 Uiso 1 1 calc R . . C5 C 0.4519(5) 0.1791(5) 0.0435(2) 0.118(2) Uani 1 1 d . . . H5 H 0.3955 0.1755 0.0424 0.141 Uiso 1 1 calc R . . C6 C 0.4583(4) 0.2616(4) 0.05111(16) 0.0845(14) Uani 1 1 d . . . C7 C 0.3803(4) 0.3395(4) 0.05554(16) 0.0960(16) Uani 1 1 d . . . H7 H 0.3258 0.3312 0.0558 0.115 Uiso 1 1 calc R . . C8 C 0.2877(3) 0.4953(4) 0.06523(19) 0.1085(18) Uani 1 1 d . . . H8A H 0.2436 0.4858 0.0456 0.130 Uiso 1 1 calc R . . H8B H 0.2658 0.4993 0.1024 0.130 Uiso 1 1 calc R . . C9 C 0.3028(3) 0.5782(4) 0.04388(18) 0.1007(16) Uani 1 1 d . . . H9A H 0.3039 0.5838 0.0054 0.121 Uiso 1 1 calc R . . H9B H 0.2551 0.6305 0.0575 0.121 Uiso 1 1 calc R . . C10 C 0.4045(3) 0.6430(3) 0.06692(15) 0.0859(14) Uani 1 1 d . . . H10 H 0.3565 0.6975 0.0638 0.103 Uiso 1 1 calc R . . C11 C 0.4887(3) 0.6460(3) 0.07792(15) 0.0733(12) Uani 1 1 d . . . C12 C 0.4941(4) 0.7305(3) 0.08550(17) 0.0962(16) Uani 1 1 d . . . H12 H 0.4425 0.7821 0.0854 0.115 Uiso 1 1 calc R . . C13 C 0.5735(5) 0.7355(4) 0.0928(2) 0.1109(19) Uani 1 1 d . . . H13 H 0.5763 0.7909 0.0981 0.133 Uiso 1 1 calc R . . C14 C 0.6518(4) 0.6597(4) 0.09268(17) 0.0913(14) Uani 1 1 d . . . H14 H 0.7067 0.6643 0.0972 0.110 Uiso 1 1 calc R . . C15 C 0.6470(3) 0.5774(3) 0.08582(15) 0.0726(12) Uani 1 1 d . . . C16 C 0.5656(3) 0.5676(3) 0.07818(13) 0.0593(10) Uani 1 1 d . . . C17 C 0.7818(4) 0.1233(3) 0.0440(2) 0.1184(18) Uani 1 1 d . . . H17A H 0.7837 0.0996 0.0102 0.142 Uiso 1 1 calc R . . H17B H 0.7850 0.0761 0.0720 0.142 Uiso 1 1 calc R . . C18 C 0.8590(4) 0.1541(4) 0.0450(2) 0.142(2) Uani 1 1 d . . . H18A H 0.8554 0.2004 0.0171 0.214 Uiso 1 1 calc R . . H18B H 0.9146 0.1043 0.0398 0.214 Uiso 1 1 calc R . . H18C H 0.8566 0.1772 0.0787 0.214 Uiso 1 1 calc R . . C19 C 0.8069(3) 0.5017(3) 0.07450(17) 0.0892(14) Uani 1 1 d . . . H19A H 0.8242 0.5229 0.1045 0.107 Uiso 1 1 calc R . . H19B H 0.8081 0.5425 0.0435 0.107 Uiso 1 1 calc R . . C20 C 0.8697(3) 0.4091(3) 0.06458(17) 0.0976(16) Uani 1 1 d . . . H20A H 0.8741 0.3712 0.0969 0.146 Uiso 1 1 calc R . . H20B H 0.9280 0.4102 0.0524 0.146 Uiso 1 1 calc R . . H20C H 0.8474 0.3859 0.0381 0.146 Uiso 1 1 calc R . . C21 C 0.8313(3) 0.1145(3) 0.19402(15) 0.0705(11) Uani 1 1 d . A . C22 C 0.8943(3) 0.1564(3) 0.19777(17) 0.0791(12) Uani 1 1 d . A . C23 C 0.9844(3) 0.1058(4) 0.2042(2) 0.1099(17) Uani 1 1 d . . . H23 H 1.0248 0.1342 0.2068 0.132 Uiso 1 1 calc R . . C24 C 1.0143(4) 0.0119(4) 0.2067(3) 0.134(2) Uani 1 1 d . . . H24 H 1.0746 -0.0219 0.2109 0.161 Uiso 1 1 calc R . . C25 C 0.9562(4) -0.0302(4) 0.2030(2) 0.124(2) Uani 1 1 d . . . H25 H 0.9770 -0.0927 0.2050 0.148 Uiso 1 1 calc R . . C26 C 0.8644(4) 0.0196(3) 0.19619(18) 0.0893(14) Uani 1 1 d . . . C27 C 0.8038(4) -0.0258(3) 0.19286(18) 0.1057(17) Uani 1 1 d . A . H27 H 0.8287 -0.0881 0.1930 0.127 Uiso 1 1 calc R . . C28A C 0.6499(11) -0.0439(11) 0.2041(7) 0.086(5) Uani 0.50 1 d PD A 1 H28A H 0.6765 -0.1041 0.1921 0.103 Uiso 0.50 1 calc PR A 1 H28B H 0.6349 -0.0479 0.2421 0.103 Uiso 0.50 1 calc PR A 1 C29A C 0.5706(14) 0.009(2) 0.1760(11) 0.087(7) Uani 0.50 1 d PD A 1 H29A H 0.5825 0.0020 0.1381 0.105 Uiso 0.50 1 calc PR A 1 H29B H 0.5204 -0.0094 0.1887 0.105 Uiso 0.50 1 calc PR A 1 C28B C 0.6793(12) -0.0489(10) 0.1731(6) 0.116(6) Uani 0.50 1 d PD A 2 H28C H 0.7080 -0.1101 0.1880 0.140 Uiso 0.50 1 calc PR A 2 H28D H 0.6821 -0.0483 0.1347 0.140 Uiso 0.50 1 calc PR A 2 C29B C 0.5874(15) -0.008(2) 0.1956(12) 0.129(15) Uani 0.50 1 d PD A 2 H29C H 0.5847 -0.0257 0.2334 0.155 Uiso 0.50 1 calc PR A 2 H29D H 0.5486 -0.0308 0.1792 0.155 Uiso 0.50 1 calc PR A 2 C30 C 0.4698(3) 0.1505(4) 0.18683(16) 0.0926(15) Uani 1 1 d . A . H30 H 0.4275 0.1245 0.1838 0.111 Uiso 1 1 calc R . . C31 C 0.4368(3) 0.2450(3) 0.19126(15) 0.0738(12) Uani 1 1 d . . . C32 C 0.3436(4) 0.2932(5) 0.19075(17) 0.0948(16) Uani 1 1 d . . . H32 H 0.3049 0.2634 0.1868 0.114 Uiso 1 1 calc R . . C33 C 0.3101(3) 0.3828(5) 0.19600(18) 0.1031(18) Uani 1 1 d . . . H33 H 0.2485 0.4144 0.1953 0.124 Uiso 1 1 calc R . . C34 C 0.3669(3) 0.4279(3) 0.20243(15) 0.0824(13) Uani 1 1 d . . . H34 H 0.3433 0.4894 0.2065 0.099 Uiso 1 1 calc R . . C35 C 0.4579(3) 0.3818(3) 0.20281(14) 0.0665(11) Uani 1 1 d . A . C36 C 0.4959(3) 0.2888(3) 0.19595(13) 0.0620(10) Uani 1 1 d . A . C37 C 0.9096(3) 0.2943(3) 0.21136(19) 0.0971(15) Uani 1 1 d . A . H37A H 0.9592 0.2919 0.1853 0.117 Uiso 1 1 calc R . . H37B H 0.9339 0.2670 0.2451 0.117 Uiso 1 1 calc R . . C38 C 0.8474(3) 0.3905(3) 0.21704(17) 0.0989(15) Uani 1 1 d . . . H38A H 0.8240 0.4168 0.1834 0.148 Uiso 1 1 calc R . . H38B H 0.8800 0.4240 0.2286 0.148 Uiso 1 1 calc R . . H38C H 0.7985 0.3919 0.2428 0.148 Uiso 1 1 calc R . . C39 C 0.4883(3) 0.5119(3) 0.22010(18) 0.0862(13) Uani 1 1 d . A . H39A H 0.4467 0.5216 0.2515 0.103 Uiso 1 1 calc R . . H39B H 0.4574 0.5504 0.1906 0.103 Uiso 1 1 calc R . . C40 C 0.5680(3) 0.5327(3) 0.2293(2) 0.1166(18) Uani 1 1 d . . . H40A H 0.5971 0.4952 0.2591 0.175 Uiso 1 1 calc R . . H40B H 0.5493 0.5947 0.2365 0.175 Uiso 1 1 calc R . . H40C H 0.6092 0.5215 0.1983 0.175 Uiso 1 1 calc R . . C41 C -0.0008(2) 0.8502(2) 0.44523(14) 0.0479(9) Uani 1 1 d . . . C42 C 0.0259(2) 0.8158(2) 0.39464(15) 0.0525(9) Uani 1 1 d . . . C43 C -0.0311(3) 0.8482(3) 0.35415(15) 0.0624(10) Uani 1 1 d . . . H43 H -0.0132 0.8253 0.3209 0.075 Uiso 1 1 calc R . . C44 C -0.1150(3) 0.9147(3) 0.36259(17) 0.0723(12) Uani 1 1 d . . . H44 H -0.1528 0.9365 0.3349 0.087 Uiso 1 1 calc R . . C45 C -0.1421(3) 0.9479(3) 0.41044(18) 0.0693(11) Uani 1 1 d . . . H45 H -0.1988 0.9920 0.4156 0.083 Uiso 1 1 calc R . . C46 C -0.0860(2) 0.9171(2) 0.45296(15) 0.0537(9) Uani 1 1 d . . . C47 C -0.1144(2) 0.9580(2) 0.50222(15) 0.0583(10) Uani 1 1 d . . . H47 H -0.1718 1.0017 0.5050 0.070 Uiso 1 1 calc R . . C48 C -0.1055(2) 0.9957(3) 0.58884(15) 0.0662(11) Uani 1 1 d . . . H48A H -0.1689 1.0054 0.5961 0.079 Uiso 1 1 calc R . . H48B H -0.0994 1.0537 0.5811 0.079 Uiso 1 1 calc R . . C49 C -0.0548(3) 0.9471(3) 0.63584(16) 0.0762(12) Uani 1 1 d . . . H49A H -0.0511 0.9902 0.6586 0.091 Uiso 1 1 calc R . . H49B H -0.0862 0.9114 0.6562 0.091 Uiso 1 1 calc R . . C50 C 0.1010(3) 0.8628(3) 0.64934(15) 0.0682(11) Uani 1 1 d . . . H50 H 0.0886 0.8894 0.6815 0.082 Uiso 1 1 calc R . . C51 C 0.1886(3) 0.7984(3) 0.63976(15) 0.0610(10) Uani 1 1 d . . . C52 C 0.2518(3) 0.7764(3) 0.67795(18) 0.0833(13) Uani 1 1 d . . . H52 H 0.2370 0.8068 0.7088 0.100 Uiso 1 1 calc R . . C53 C 0.3348(4) 0.7111(4) 0.6706(2) 0.0942(16) Uani 1 1 d . . . H53 H 0.3757 0.6967 0.6966 0.113 Uiso 1 1 calc R . . C54 C 0.3581(3) 0.6660(3) 0.6240(2) 0.0835(14) Uani 1 1 d . . . H54 H 0.4149 0.6220 0.6190 0.100 Uiso 1 1 calc R . . C55 C 0.2982(3) 0.6856(3) 0.58562(16) 0.0634(11) Uani 1 1 d . . . C56 C 0.2107(2) 0.7540(2) 0.59310(15) 0.0581(10) Uani 1 1 d . . . C57 C 0.1453(3) 0.7192(3) 0.33946(14) 0.0734(12) Uani 1 1 d . . . H57A H 0.1428 0.7696 0.3141 0.088 Uiso 1 1 calc R . . H57B H 0.1101 0.6880 0.3274 0.088 Uiso 1 1 calc R . . C58 C 0.2406(3) 0.6567(3) 0.34376(16) 0.0896(14) Uani 1 1 d . . . H58A H 0.2760 0.6893 0.3529 0.134 Uiso 1 1 calc R . . H58B H 0.2643 0.6313 0.3103 0.134 Uiso 1 1 calc R . . H58C H 0.2428 0.6094 0.3708 0.134 Uiso 1 1 calc R . . C59 C 0.3997(3) 0.5999(3) 0.5183(2) 0.1034(16) Uani 1 1 d . . . H59A H 0.4265 0.5433 0.5389 0.124 Uiso 1 1 calc R . . H59B H 0.4366 0.6359 0.5193 0.124 Uiso 1 1 calc R . . C60 C 0.3940(3) 0.5834(3) 0.4623(2) 0.1087(17) Uani 1 1 d . . . H60A H 0.3618 0.5435 0.4620 0.163 Uiso 1 1 calc R . . H60B H 0.4535 0.5566 0.4458 0.163 Uiso 1 1 calc R . . H60C H 0.3629 0.6394 0.4430 0.163 Uiso 1 1 calc R . . C61 C 0.3084(2) 0.4100(2) 0.55152(14) 0.0467(9) Uani 1 1 d . . . C62 C 0.2822(2) 0.4529(2) 0.60000(14) 0.0506(9) Uani 1 1 d . . . C63 C 0.3359(2) 0.4248(3) 0.64168(15) 0.0626(10) Uani 1 1 d . . . H63 H 0.3185 0.4550 0.6726 0.075 Uiso 1 1 calc R . . C64 C 0.4160(3) 0.3520(3) 0.63824(15) 0.0736(12) Uani 1 1 d . . . H64 H 0.4516 0.3335 0.6670 0.088 Uiso 1 1 calc R . . C65 C 0.4432(2) 0.3072(2) 0.59349(15) 0.0681(11) Uani 1 1 d . . . H65 H 0.4969 0.2579 0.5919 0.082 Uiso 1 1 calc R . . C66 C 0.3901(2) 0.3355(2) 0.54889(15) 0.0531(9) Uani 1 1 d . . . C67 C 0.4196(2) 0.2874(2) 0.50214(18) 0.0637(11) Uani 1 1 d . . . H67 H 0.4721 0.2368 0.5032 0.076 Uiso 1 1 calc R . . C68 C 0.4152(3) 0.2496(3) 0.41390(18) 0.0879(14) Uani 1 1 d . . . H68A H 0.4803 0.2227 0.4130 0.105 Uiso 1 1 calc R . . H68B H 0.3910 0.2019 0.4178 0.105 Uiso 1 1 calc R . . C69 C 0.3868(3) 0.3074(3) 0.36446(17) 0.0857(14) Uani 1 1 d . . . H69A H 0.3874 0.2713 0.3361 0.103 Uiso 1 1 calc R . . H69B H 0.4271 0.3397 0.3534 0.103 Uiso 1 1 calc R . . C70 C 0.2380(3) 0.4002(2) 0.34048(15) 0.0630(11) Uani 1 1 d . . . H70 H 0.2570 0.3769 0.3074 0.076 Uiso 1 1 calc R . . C71 C 0.1487(2) 0.4652(2) 0.34689(14) 0.0523(9) Uani 1 1 d . . . C72 C 0.0925(3) 0.4876(3) 0.30386(14) 0.0658(11) Uani 1 1 d . . . H72 H 0.1144 0.4611 0.2719 0.079 Uiso 1 1 calc R . . C73 C 0.0067(3) 0.5480(3) 0.30936(15) 0.0703(11) Uani 1 1 d . . . H73 H -0.0301 0.5618 0.2813 0.084 Uiso 1 1 calc R . . C74 C -0.0263(3) 0.5892(2) 0.35684(15) 0.0615(10) Uani 1 1 d . . . H74 H -0.0851 0.6301 0.3603 0.074 Uiso 1 1 calc R . . C75 C 0.0273(2) 0.5698(2) 0.39818(14) 0.0500(9) Uani 1 1 d . . . C76 C 0.1171(2) 0.5072(2) 0.39439(14) 0.0474(9) Uani 1 1 d . . . C77 C 0.1626(2) 0.5594(2) 0.64934(14) 0.0621(10) Uani 1 1 d . . . H77A H 0.1998 0.5880 0.6618 0.075 Uiso 1 1 calc R . . H77B H 0.1587 0.5124 0.6759 0.075 Uiso 1 1 calc R . . C78 C 0.0705(2) 0.6272(2) 0.64042(15) 0.0706(11) Uani 1 1 d . . . H78A H 0.0754 0.6749 0.6155 0.106 Uiso 1 1 calc R . . H78B H 0.0420 0.6514 0.6735 0.106 Uiso 1 1 calc R . . H78C H 0.0351 0.5987 0.6266 0.106 Uiso 1 1 calc R . . C79 C -0.0925(2) 0.6623(3) 0.45506(15) 0.0644(11) Uani 1 1 d . . . H79A H -0.1296 0.6274 0.4517 0.077 Uiso 1 1 calc R . . H79B H -0.1093 0.7140 0.4294 0.077 Uiso 1 1 calc R . . C80 C -0.1053(3) 0.6922(3) 0.51008(15) 0.0777(12) Uani 1 1 d . . . H80A H -0.0856 0.6405 0.5349 0.117 Uiso 1 1 calc R . . H80B H -0.1678 0.7261 0.5183 0.117 Uiso 1 1 calc R . . H80C H -0.0707 0.7292 0.5123 0.117 Uiso 1 1 calc R . . C81 C 0.3954(2) 0.9010(2) 0.30589(13) 0.0483(9) Uani 1 1 d . . . C82 C 0.4731(2) 0.8549(2) 0.27569(14) 0.0563(10) Uani 1 1 d . . . H82 H 0.5260 0.8635 0.2806 0.068 Uiso 1 1 calc R . . C83 C 0.4755(3) 0.7969(2) 0.23855(15) 0.0694(11) Uani 1 1 d . . . H83 H 0.5292 0.7680 0.2190 0.083 Uiso 1 1 calc R . . C84 C 0.3999(4) 0.7814(3) 0.23021(16) 0.0767(13) Uani 1 1 d . . . H84 H 0.4016 0.7423 0.2053 0.092 Uiso 1 1 calc R . . C85 C 0.3216(3) 0.8247(3) 0.25920(16) 0.0757(12) Uani 1 1 d . . . H85 H 0.2694 0.8148 0.2543 0.091 Uiso 1 1 calc R . . C86 C 0.3202(3) 0.8832(3) 0.29582(15) 0.0647(11) Uani 1 1 d . . . H86 H 0.2660 0.9123 0.3148 0.078 Uiso 1 1 calc R . . C87 C 0.3742(2) 0.9383(2) 0.40962(14) 0.0504(9) Uani 1 1 d . . . C88 C 0.3371(2) 0.8731(2) 0.42613(15) 0.0565(10) Uani 1 1 d . . . H88 H 0.3204 0.8465 0.4003 0.068 Uiso 1 1 calc R . . C89 C 0.3237(2) 0.8453(2) 0.47916(18) 0.0686(12) Uani 1 1 d . . . H89 H 0.2981 0.8017 0.4880 0.082 Uiso 1 1 calc R . . C90 C 0.3480(3) 0.8822(3) 0.51817(17) 0.0728(12) Uani 1 1 d . . . H90 H 0.3399 0.8636 0.5537 0.087 Uiso 1 1 calc R . . C91 C 0.3847(3) 0.9471(3) 0.50427(16) 0.0708(12) Uani 1 1 d . . . H91 H 0.4015 0.9728 0.5305 0.085 Uiso 1 1 calc R . . C92 C 0.3966(2) 0.9742(2) 0.45175(15) 0.0622(10) Uani 1 1 d . . . H92 H 0.4209 1.0188 0.4436 0.075 Uiso 1 1 calc R . . C93 C 0.3018(2) 1.0676(2) 0.33290(14) 0.0470(9) Uani 1 1 d . . . C94 C 0.2505(2) 1.1290(2) 0.36969(15) 0.0591(10) Uani 1 1 d . . . H94 H 0.2626 1.1155 0.4053 0.071 Uiso 1 1 calc R . . C95 C 0.1823(3) 1.2093(3) 0.35550(18) 0.0711(12) Uani 1 1 d . . . H95 H 0.1513 1.2488 0.3813 0.085 Uiso 1 1 calc R . . C96 C 0.1607(3) 1.2308(3) 0.3041(2) 0.0722(12) Uani 1 1 d . . . H96 H 0.1142 1.2841 0.2949 0.087 Uiso 1 1 calc R . . C97 C 0.2079(3) 1.1733(3) 0.26594(16) 0.0666(11) Uani 1 1 d . . . H97 H 0.1943 1.1870 0.2306 0.080 Uiso 1 1 calc R . . C98 C 0.2767(2) 1.0938(3) 0.28120(15) 0.0632(10) Uani 1 1 d . . . H98 H 0.3082 1.0556 0.2549 0.076 Uiso 1 1 calc R . . C99 C 0.4804(2) 0.9994(2) 0.34199(13) 0.0480(9) Uani 1 1 d . . . C100 C 0.4842(2) 1.0812(2) 0.32057(13) 0.0484(9) Uani 1 1 d . . . H100 H 0.4329 1.1244 0.3070 0.058 Uiso 1 1 calc R . . C101 C 0.5615(3) 1.1013(3) 0.31863(14) 0.0580(10) Uani 1 1 d . . . H101 H 0.5607 1.1577 0.3047 0.070 Uiso 1 1 calc R . . C102 C 0.6394(3) 1.0386(3) 0.33704(15) 0.0675(11) Uani 1 1 d . . . H102 H 0.6914 1.0517 0.3356 0.081 Uiso 1 1 calc R . . C103 C 0.6387(3) 0.9556(3) 0.35774(15) 0.0672(11) Uani 1 1 d . . . H103 H 0.6909 0.9119 0.3700 0.081 Uiso 1 1 calc R . . C104 C 0.5606(3) 0.9379(2) 0.36008(14) 0.0583(10) Uani 1 1 d . . . H104 H 0.5616 0.8818 0.3746 0.070 Uiso 1 1 calc R . . C105 C -0.0541(2) 0.2953(3) 0.86196(14) 0.0558(10) Uani 1 1 d . . . C106 C -0.1212(3) 0.3414(3) 0.82842(19) 0.0898(14) Uani 1 1 d . . . H106 H -0.1200 0.3945 0.8102 0.108 Uiso 1 1 calc R . . C107 C -0.1903(3) 0.3128(4) 0.8204(2) 0.1006(16) Uani 1 1 d . . . H107 H -0.2330 0.3456 0.7966 0.121 Uiso 1 1 calc R . . C108 C -0.1959(3) 0.2367(4) 0.8474(2) 0.0968(17) Uani 1 1 d . . . H108 H -0.2433 0.2182 0.8434 0.116 Uiso 1 1 calc R . . C109 C -0.1312(4) 0.1891(4) 0.8799(2) 0.1119(18) Uani 1 1 d . . . H109 H -0.1329 0.1360 0.8978 0.134 Uiso 1 1 calc R . . C110 C -0.0613(3) 0.2182(3) 0.88719(17) 0.0856(13) Uani 1 1 d . . . H110 H -0.0178 0.1836 0.9102 0.103 Uiso 1 1 calc R . . C111 C 0.0882(2) 0.26932(18) 0.91965(11) 0.0632(10) Uani 1 1 d G . . C112 C 0.04138(19) 0.2632(2) 0.96839(14) 0.1017(16) Uani 1 1 d G . . H112 H -0.0208 0.2922 0.9721 0.122 Uiso 1 1 calc R . . C113 C 0.0874(3) 0.2139(3) 1.01164(10) 0.136(2) Uani 1 1 d G . . H113 H 0.0561 0.2098 1.0442 0.163 Uiso 1 1 calc R . . C114 C 0.1803(3) 0.1706(2) 1.00615(14) 0.155(3) Uani 1 1 d GD . . H114 H 0.2111 0.1376 1.0351 0.186 Uiso 1 1 calc R . . C115 C 0.22711(19) 0.1767(2) 0.95741(19) 0.148(3) Uani 1 1 d GD . . H115 H 0.2892 0.1477 0.9537 0.178 Uiso 1 1 calc R . . C116 C 0.1810(2) 0.2261(2) 0.91416(13) 0.1179(19) Uani 1 1 d GD . . H116 H 0.2124 0.2301 0.8815 0.142 Uiso 1 1 calc R . . C117 C -0.0148(2) 0.4381(2) 0.87841(14) 0.0533(9) Uani 1 1 d . . . C118 C -0.0406(2) 0.4734(3) 0.92794(15) 0.0597(10) Uani 1 1 d . . . H118 H -0.0279 0.4340 0.9582 0.072 Uiso 1 1 calc R . . C119 C -0.0841(3) 0.5638(3) 0.93408(18) 0.0718(12) Uani 1 1 d . . . H119 H -0.0996 0.5836 0.9681 0.086 Uiso 1 1 calc R . . C120 C -0.1049(2) 0.6251(3) 0.8913(2) 0.0697(12) Uani 1 1 d . . . H120 H -0.1351 0.6860 0.8957 0.084 Uiso 1 1 calc R . . C121 C -0.0800(3) 0.5942(3) 0.84231(18) 0.0751(12) Uani 1 1 d . . . H121 H -0.0927 0.6345 0.8124 0.090 Uiso 1 1 calc R . . C122 C -0.0362(3) 0.5038(3) 0.83629(15) 0.0705(11) Uani 1 1 d . . . H122 H -0.0199 0.4854 0.8019 0.085 Uiso 1 1 calc R . . C123 C 0.0971(2) 0.3148(2) 0.81474(13) 0.0517(9) Uani 1 1 d . . . C124 C 0.1652(3) 0.3513(3) 0.80668(16) 0.0720(12) Uani 1 1 d . . . H124 H 0.1668 0.3897 0.8312 0.086 Uiso 1 1 calc R . . C125 C 0.2301(3) 0.3337(3) 0.76452(17) 0.0752(12) Uani 1 1 d . . . H125 H 0.2739 0.3594 0.7618 0.090 Uiso 1 1 calc R . . C126 C 0.2301(3) 0.2794(3) 0.72705(17) 0.0742(12) Uani 1 1 d . . . H126 H 0.2741 0.2664 0.6990 0.089 Uiso 1 1 calc R . . C127 C 0.1639(3) 0.2444(2) 0.73167(16) 0.0683(11) Uani 1 1 d . . . H127 H 0.1620 0.2081 0.7059 0.082 Uiso 1 1 calc R . . C128 C 0.0989(2) 0.2619(2) 0.77435(15) 0.0583(10) Uani 1 1 d . . . H128 H 0.0546 0.2370 0.7759 0.070 Uiso 1 1 calc R . . N1 N 0.3752(2) 0.4209(2) 0.05925(12) 0.0801(10) Uani 1 1 d . . . N2 N 0.38925(19) 0.5715(2) 0.06092(11) 0.0755(10) Uani 1 1 d . . . N3 N 0.7183(3) 0.0107(2) 0.18964(14) 0.0945(12) Uani 1 1 d . . . N4 N 0.5521(2) 0.0979(2) 0.18661(12) 0.0816(10) Uani 1 1 d . . . N5 N -0.06830(17) 0.94022(17) 0.54323(11) 0.0506(7) Uani 1 1 d . . . N6 N 0.03679(19) 0.88806(18) 0.61772(11) 0.0569(8) Uani 1 1 d . . . N7 N 0.37953(19) 0.30846(18) 0.45872(13) 0.0590(8) Uani 1 1 d . . . N8 N 0.2941(2) 0.37149(19) 0.37697(12) 0.0585(8) Uani 1 1 d . . . Ni1 Ni 0.47156(3) 0.45502(4) 0.063792(18) 0.06478(15) Uani 1 1 d . . . Ni2 Ni 0.65069(4) 0.13001(3) 0.190335(19) 0.06693(16) Uani 1 1 d . A . Ni3 Ni 0.04482(3) 0.85544(3) 0.549752(17) 0.04922(13) Uani 1 1 d . . . Ni4 Ni 0.27441(3) 0.40312(3) 0.445761(18) 0.04999(13) Uani 1 1 d . . . O1 O 0.55589(16) 0.34066(17) 0.06271(9) 0.0700(7) Uani 1 1 d . . . O2 O 0.56763(15) 0.48753(16) 0.07231(9) 0.0638(7) Uani 1 1 d . . . O3 O 0.70076(19) 0.19851(18) 0.05191(11) 0.0914(9) Uani 1 1 d . . . O4 O 0.72007(16) 0.49827(18) 0.08538(11) 0.0820(8) Uani 1 1 d . . . O5 O 0.74771(16) 0.16575(15) 0.19016(10) 0.0684(7) Uani 1 1 d . . . O6 O 0.58330(16) 0.24930(15) 0.19560(9) 0.0643(7) Uani 1 1 d . . . O7 O 0.85767(17) 0.24798(17) 0.19450(11) 0.0781(8) Uani 1 1 d . . . O8 O 0.52000(16) 0.42017(15) 0.20842(10) 0.0725(7) Uani 1 1 d . . . O9 O 0.05618(14) 0.81855(14) 0.48227(8) 0.0525(6) Uani 1 1 d . . . O10 O 0.15765(14) 0.77001(15) 0.55454(9) 0.0565(6) Uani 1 1 d . . . O11 O 0.11007(15) 0.75037(15) 0.39073(8) 0.0604(7) Uani 1 1 d . . . O12 O 0.31171(15) 0.64570(16) 0.53923(10) 0.0735(8) Uani 1 1 d . . . O13 O 0.25545(13) 0.44075(14) 0.51296(8) 0.0517(6) Uani 1 1 d . . . O14 O 0.16487(14) 0.49279(14) 0.43536(9) 0.0520(6) Uani 1 1 d . . . O15 O 0.20047(15) 0.52230(15) 0.60012(9) 0.0602(7) Uani 1 1 d . . . O16 O 0.00092(15) 0.60830(15) 0.44584(9) 0.0565(6) Uani 1 1 d . . . Rb1 Rb 0.68572(3) 0.33608(3) 0.132761(16) 0.06844(12) Uani 1 1 d . A . Rb2 Rb 0.15014(3) 0.63004(2) 0.497563(15) 0.06310(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 B1 0.051(3) 0.039(2) 0.050(3) -0.0076(19) 0.005(2) -0.013(2) B2 0.055(3) 0.056(3) 0.048(3) -0.009(2) -0.007(2) -0.020(2) C1 0.101(4) 0.093(4) 0.040(2) -0.006(2) 0.001(2) -0.055(3) C2 0.139(5) 0.095(4) 0.043(3) -0.011(2) 0.003(3) -0.068(4) C3 0.207(7) 0.096(4) 0.068(3) -0.009(3) -0.014(4) -0.078(5) C4 0.227(9) 0.146(6) 0.080(4) -0.010(4) -0.017(5) -0.140(6) C5 0.176(7) 0.156(6) 0.074(4) -0.013(4) -0.008(4) -0.121(6) C6 0.119(4) 0.116(4) 0.052(3) -0.003(3) -0.011(3) -0.082(4) C7 0.111(4) 0.170(5) 0.050(3) 0.001(3) -0.012(3) -0.101(4) C8 0.055(3) 0.194(6) 0.084(4) 0.003(4) -0.007(2) -0.056(4) C9 0.056(3) 0.166(5) 0.070(3) 0.001(3) -0.013(2) -0.027(3) C10 0.082(3) 0.102(4) 0.053(3) -0.004(2) 0.005(2) -0.012(3) C11 0.087(4) 0.082(4) 0.045(3) 0.001(2) 0.004(2) -0.027(3) C12 0.139(5) 0.071(4) 0.065(3) -0.006(3) 0.001(3) -0.023(4) C13 0.162(6) 0.093(5) 0.097(4) -0.009(3) -0.017(4) -0.066(5) C14 0.114(4) 0.099(4) 0.080(3) -0.003(3) -0.018(3) -0.060(4) C15 0.091(3) 0.077(3) 0.060(3) 0.002(2) -0.005(2) -0.044(3) C16 0.067(3) 0.073(3) 0.043(2) -0.0011(19) 0.001(2) -0.034(2) C17 0.141(5) 0.097(4) 0.098(4) -0.025(3) 0.015(4) -0.023(4) C18 0.108(5) 0.144(6) 0.147(6) -0.039(4) 0.019(4) -0.012(4) C19 0.087(3) 0.134(4) 0.076(3) -0.003(3) -0.005(3) -0.077(3) C20 0.063(3) 0.162(5) 0.082(3) -0.023(3) 0.005(3) -0.057(3) C21 0.083(3) 0.061(3) 0.062(3) -0.008(2) 0.004(2) -0.021(3) C22 0.077(3) 0.065(3) 0.082(3) -0.003(2) 0.002(3) -0.014(3) C23 0.078(4) 0.095(4) 0.145(5) -0.006(4) -0.002(3) -0.020(3) C24 0.085(4) 0.089(5) 0.184(6) 0.005(4) 0.021(4) 0.008(4) C25 0.108(5) 0.066(4) 0.159(6) 0.002(3) 0.024(4) 0.000(4) C26 0.104(4) 0.054(3) 0.096(4) -0.007(3) 0.006(3) -0.016(3) C27 0.161(5) 0.044(3) 0.109(4) -0.004(3) -0.035(3) -0.027(3) C28A 0.140(16) 0.045(9) 0.079(10) -0.020(8) 0.013(11) -0.043(9) C29A 0.130(14) 0.084(14) 0.075(14) -0.001(11) -0.005(10) -0.072(10) C28B 0.20(2) 0.089(9) 0.091(11) -0.017(9) 0.003(11) -0.088(12) C29B 0.21(4) 0.07(2) 0.12(3) -0.017(18) 0.05(2) -0.09(2) C30 0.118(4) 0.129(4) 0.063(3) -0.009(3) 0.009(3) -0.086(4) C31 0.088(4) 0.098(4) 0.047(3) -0.002(2) 0.008(2) -0.052(3) C32 0.088(4) 0.156(5) 0.060(3) 0.006(3) 0.003(3) -0.073(4) C33 0.067(4) 0.160(6) 0.072(3) 0.005(4) 0.011(3) -0.038(4) C34 0.071(3) 0.108(4) 0.061(3) -0.002(2) 0.007(2) -0.028(3) C35 0.066(3) 0.089(3) 0.046(2) -0.003(2) 0.003(2) -0.033(3) C36 0.077(3) 0.077(3) 0.041(2) -0.003(2) 0.002(2) -0.041(3) C37 0.105(4) 0.105(4) 0.100(4) 0.000(3) -0.016(3) -0.060(3) C38 0.138(4) 0.104(4) 0.076(3) -0.015(3) -0.015(3) -0.065(4) C39 0.088(3) 0.061(3) 0.094(3) -0.014(2) -0.009(3) -0.005(3) C40 0.135(5) 0.077(4) 0.138(5) -0.026(3) -0.031(4) -0.027(3) C41 0.048(2) 0.042(2) 0.056(2) 0.0006(18) -0.0056(18) -0.0196(18) C42 0.050(2) 0.050(2) 0.055(2) -0.0071(19) 0.000(2) -0.0156(19) C43 0.067(3) 0.072(3) 0.053(3) -0.007(2) -0.007(2) -0.030(2) C44 0.056(3) 0.080(3) 0.078(3) -0.009(3) -0.019(2) -0.016(2) C45 0.047(2) 0.071(3) 0.085(3) -0.012(3) -0.013(2) -0.011(2) C46 0.045(2) 0.053(2) 0.062(3) -0.005(2) -0.004(2) -0.0156(19) C47 0.045(2) 0.049(2) 0.076(3) -0.007(2) 0.001(2) -0.0125(18) C48 0.056(3) 0.067(3) 0.081(3) -0.025(2) 0.010(2) -0.027(2) C49 0.083(3) 0.076(3) 0.070(3) -0.029(2) 0.016(2) -0.029(3) C50 0.090(3) 0.076(3) 0.056(3) -0.011(2) -0.001(2) -0.050(3) C51 0.068(3) 0.073(3) 0.053(3) 0.008(2) -0.015(2) -0.040(2) C52 0.098(4) 0.098(4) 0.075(3) 0.011(3) -0.028(3) -0.060(3) C53 0.106(4) 0.117(4) 0.086(4) 0.028(3) -0.045(3) -0.070(4) C54 0.064(3) 0.095(4) 0.098(4) 0.026(3) -0.032(3) -0.039(3) C55 0.056(3) 0.062(3) 0.078(3) 0.015(2) -0.018(2) -0.030(2) C56 0.055(3) 0.060(3) 0.066(3) 0.013(2) -0.012(2) -0.032(2) C57 0.073(3) 0.077(3) 0.065(3) -0.005(2) 0.010(2) -0.024(2) C58 0.080(3) 0.090(3) 0.075(3) -0.008(3) 0.016(2) -0.009(3) C59 0.047(3) 0.083(3) 0.152(5) -0.001(3) -0.009(3) 0.008(2) C60 0.064(3) 0.104(4) 0.134(5) -0.024(4) 0.013(3) -0.004(3) C61 0.040(2) 0.039(2) 0.058(2) 0.0000(17) 0.0004(17) -0.0122(16) C62 0.048(2) 0.050(2) 0.050(2) 0.0053(19) -0.0062(19) -0.0156(18) C63 0.061(3) 0.071(3) 0.051(2) 0.005(2) -0.009(2) -0.020(2) C64 0.064(3) 0.084(3) 0.063(3) 0.009(2) -0.019(2) -0.015(2) C65 0.044(2) 0.066(3) 0.081(3) 0.006(2) -0.013(2) -0.006(2) C66 0.043(2) 0.047(2) 0.065(3) -0.001(2) -0.004(2) -0.0131(18) C67 0.040(2) 0.046(2) 0.093(3) -0.011(2) -0.004(2) -0.0006(18) C68 0.074(3) 0.073(3) 0.098(4) -0.043(3) -0.007(3) 0.006(2) C69 0.066(3) 0.088(3) 0.083(3) -0.037(3) 0.005(3) 0.001(3) C70 0.077(3) 0.060(3) 0.050(3) -0.022(2) 0.006(2) -0.020(2) C71 0.064(3) 0.047(2) 0.045(2) -0.0061(18) -0.002(2) -0.018(2) C72 0.088(3) 0.068(3) 0.042(2) -0.012(2) -0.004(2) -0.027(3) C73 0.080(3) 0.077(3) 0.047(3) 0.002(2) -0.017(2) -0.018(3) C74 0.064(3) 0.061(3) 0.051(3) -0.002(2) -0.012(2) -0.011(2) C75 0.055(2) 0.047(2) 0.044(2) -0.0039(18) -0.0025(19) -0.0137(19) C76 0.056(2) 0.040(2) 0.045(2) -0.0022(18) -0.0040(19) -0.0166(19) C77 0.065(3) 0.068(3) 0.048(2) -0.007(2) 0.006(2) -0.019(2) C78 0.067(3) 0.068(3) 0.070(3) -0.015(2) 0.008(2) -0.017(2) C79 0.054(3) 0.074(3) 0.063(3) -0.010(2) 0.000(2) -0.020(2) C80 0.071(3) 0.081(3) 0.078(3) -0.016(2) 0.017(2) -0.027(2) C81 0.053(2) 0.045(2) 0.047(2) -0.0024(17) 0.0019(18) -0.0189(19) C82 0.061(3) 0.051(2) 0.054(2) -0.006(2) -0.002(2) -0.017(2) C83 0.082(3) 0.054(3) 0.058(3) -0.014(2) 0.007(2) -0.009(2) C84 0.115(4) 0.058(3) 0.061(3) -0.018(2) -0.012(3) -0.030(3) C85 0.096(4) 0.078(3) 0.069(3) -0.012(2) -0.009(3) -0.046(3) C86 0.066(3) 0.071(3) 0.063(3) -0.020(2) 0.007(2) -0.032(2) C87 0.046(2) 0.043(2) 0.054(2) -0.0072(18) 0.0092(18) -0.0081(18) C88 0.054(2) 0.050(2) 0.059(3) -0.009(2) 0.0093(19) -0.014(2) C89 0.061(3) 0.050(3) 0.078(3) 0.007(2) 0.020(2) -0.010(2) C90 0.064(3) 0.068(3) 0.055(3) 0.003(2) 0.008(2) 0.007(2) C91 0.069(3) 0.076(3) 0.056(3) -0.010(2) 0.002(2) -0.014(2) C92 0.074(3) 0.065(3) 0.050(3) -0.006(2) 0.006(2) -0.029(2) C93 0.043(2) 0.051(2) 0.050(2) -0.0027(19) 0.0029(18) -0.0224(18) C94 0.058(3) 0.060(3) 0.060(3) -0.011(2) 0.002(2) -0.022(2) C95 0.068(3) 0.056(3) 0.076(3) -0.020(2) 0.012(2) -0.008(2) C96 0.052(3) 0.057(3) 0.096(4) 0.005(3) 0.004(3) -0.011(2) C97 0.055(3) 0.073(3) 0.065(3) 0.011(2) -0.006(2) -0.018(2) C98 0.057(3) 0.064(3) 0.062(3) -0.006(2) 0.006(2) -0.016(2) C99 0.050(2) 0.047(2) 0.043(2) -0.0091(18) 0.0019(17) -0.0139(19) C100 0.044(2) 0.051(2) 0.047(2) -0.0086(18) -0.0001(17) -0.0128(19) C101 0.063(3) 0.060(3) 0.059(3) -0.013(2) 0.004(2) -0.030(2) C102 0.063(3) 0.080(3) 0.069(3) -0.017(2) 0.007(2) -0.038(3) C103 0.048(3) 0.080(3) 0.071(3) -0.007(2) -0.006(2) -0.020(2) C104 0.061(3) 0.054(2) 0.059(3) -0.0002(19) -0.004(2) -0.022(2) C105 0.061(3) 0.061(3) 0.048(2) -0.015(2) 0.001(2) -0.022(2) C106 0.077(3) 0.091(3) 0.115(4) 0.006(3) -0.036(3) -0.042(3) C107 0.083(4) 0.103(4) 0.119(4) -0.013(3) -0.033(3) -0.030(3) C108 0.078(4) 0.134(5) 0.102(4) -0.045(4) 0.004(3) -0.059(4) C109 0.138(5) 0.131(5) 0.108(4) 0.000(4) -0.012(4) -0.099(4) C110 0.097(4) 0.097(4) 0.081(3) 0.012(3) -0.025(3) -0.056(3) C111 0.075(3) 0.066(3) 0.053(3) -0.004(2) -0.004(2) -0.030(2) C112 0.124(4) 0.098(4) 0.074(4) 0.001(3) -0.023(3) -0.027(3) C113 0.176(6) 0.140(5) 0.087(4) 0.013(4) -0.039(4) -0.050(5) C114 0.184(7) 0.128(5) 0.162(7) 0.044(5) -0.124(6) -0.049(5) C115 0.094(4) 0.217(7) 0.120(5) 0.075(5) -0.026(4) -0.058(4) C116 0.090(4) 0.141(5) 0.107(4) 0.042(4) -0.024(3) -0.033(4) C117 0.055(2) 0.066(3) 0.046(2) -0.008(2) -0.0087(19) -0.027(2) C118 0.064(3) 0.065(3) 0.053(3) -0.009(2) 0.002(2) -0.028(2) C119 0.066(3) 0.081(3) 0.072(3) -0.025(3) 0.007(2) -0.028(3) C120 0.056(3) 0.060(3) 0.098(4) -0.024(3) -0.005(3) -0.021(2) C121 0.088(3) 0.053(3) 0.082(3) -0.003(2) -0.021(3) -0.020(2) C122 0.095(3) 0.064(3) 0.048(3) -0.009(2) -0.013(2) -0.021(3) C123 0.058(2) 0.046(2) 0.051(2) -0.0036(18) -0.0157(19) -0.0165(19) C124 0.086(3) 0.080(3) 0.063(3) -0.014(2) -0.010(2) -0.042(3) C125 0.069(3) 0.097(3) 0.073(3) -0.009(3) 0.004(2) -0.047(3) C126 0.072(3) 0.078(3) 0.067(3) -0.011(2) 0.007(2) -0.022(3) C127 0.079(3) 0.057(3) 0.061(3) -0.015(2) -0.003(2) -0.014(2) C128 0.060(3) 0.055(2) 0.061(3) -0.006(2) -0.009(2) -0.020(2) N1 0.065(2) 0.138(3) 0.054(2) -0.001(2) -0.0040(17) -0.056(2) N2 0.057(2) 0.111(3) 0.048(2) 0.0000(18) -0.0052(16) -0.019(2) N3 0.145(3) 0.056(2) 0.093(3) 0.0042(19) -0.034(2) -0.045(2) N4 0.130(3) 0.079(2) 0.061(2) -0.0116(18) 0.007(2) -0.069(2) N5 0.0478(18) 0.0458(17) 0.0582(19) -0.0129(14) 0.0053(14) -0.0170(14) N6 0.066(2) 0.0562(19) 0.0561(19) -0.0129(15) 0.0037(15) -0.0307(16) N7 0.0463(19) 0.0455(19) 0.076(2) -0.0195(17) -0.0036(17) -0.0019(15) N8 0.049(2) 0.056(2) 0.063(2) -0.0212(17) 0.0038(17) -0.0086(16) Ni1 0.0576(3) 0.0982(4) 0.0468(3) -0.0041(3) -0.0018(2) -0.0386(3) Ni2 0.1017(4) 0.0554(3) 0.0533(3) -0.0038(2) -0.0048(3) -0.0400(3) Ni3 0.0507(3) 0.0469(3) 0.0510(3) -0.0067(2) -0.0005(2) -0.0188(2) Ni4 0.0463(3) 0.0418(3) 0.0564(3) -0.0115(2) -0.0013(2) -0.0081(2) O1 0.0803(18) 0.088(2) 0.0608(17) -0.0105(14) -0.0025(14) -0.0524(16) O2 0.0585(16) 0.0723(17) 0.0673(17) -0.0060(13) 0.0001(13) -0.0325(14) O3 0.106(2) 0.084(2) 0.084(2) -0.0178(16) 0.0031(17) -0.0330(18) O4 0.0630(17) 0.092(2) 0.106(2) 0.0026(17) -0.0034(15) -0.0486(16) O5 0.0776(18) 0.0487(15) 0.0787(19) -0.0026(13) -0.0116(14) -0.0214(14) O6 0.0745(18) 0.0572(16) 0.0676(17) -0.0055(13) -0.0012(14) -0.0319(14) O7 0.0750(19) 0.0683(18) 0.095(2) -0.0086(15) -0.0101(15) -0.0282(15) O8 0.0738(18) 0.0572(17) 0.0821(19) -0.0104(14) -0.0021(14) -0.0182(14) O9 0.0499(14) 0.0498(14) 0.0512(15) -0.0045(11) -0.0064(11) -0.0093(12) O10 0.0541(15) 0.0590(16) 0.0559(15) -0.0042(12) -0.0119(12) -0.0178(13) O11 0.0590(16) 0.0679(17) 0.0458(15) -0.0109(12) 0.0038(12) -0.0135(13) O12 0.0477(15) 0.0755(19) 0.090(2) -0.0057(15) -0.0080(14) -0.0136(14) O13 0.0418(13) 0.0465(14) 0.0575(15) -0.0086(11) -0.0091(11) -0.0024(11) O14 0.0468(14) 0.0520(15) 0.0479(15) -0.0119(12) -0.0064(12) -0.0040(12) O15 0.0573(16) 0.0617(16) 0.0435(15) -0.0086(12) -0.0033(12) 0.0005(13) O16 0.0482(16) 0.0594(16) 0.0512(16) -0.0117(12) -0.0033(12) -0.0049(13) Rb1 0.0671(3) 0.0675(3) 0.0749(3) 0.0037(2) -0.0077(2) -0.0310(2) Rb2 0.0697(3) 0.0468(2) 0.0644(3) -0.01107(18) -0.0160(2) -0.00639(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 B1 C93 1.639(4) . ? B1 C81 1.642(4) . ? B1 C87 1.647(4) . ? B1 C99 1.660(4) . ? B2 C123 1.628(4) . ? B2 C117 1.654(4) . ? B2 C105 1.654(4) . ? B2 C111 1.685(4) . ? C1 O1 1.298(4) . ? C1 C2 1.415(6) . ? C1 C6 1.415(6) . ? C2 O3 1.372(5) . ? C2 C3 1.392(6) . ? C3 C4 1.392(8) . ? C3 H3 0.9300 . ? C4 C5 1.343(7) . ? C4 H4 0.9300 . ? C5 C6 1.401(7) . ? C5 H5 0.9300 . ? C6 C7 1.409(6) . ? C7 N1 1.291(5) . ? C7 H7 0.9300 . ? C8 C9 1.476(6) . ? C8 N1 1.475(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.459(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.285(5) . ? C10 C11 1.425(6) . ? C10 H10 0.9300 . ? C11 C16 1.399(5) . ? C11 C12 1.425(6) . ? C12 C13 1.339(6) . ? C12 H12 0.9300 . ? C13 C14 1.388(6) . ? C13 H13 0.9300 . ? C14 C15 1.381(5) . ? C14 H14 0.9300 . ? C15 O4 1.374(4) . ? C15 C16 1.408(5) . ? C16 O2 1.297(4) . ? C17 O3 1.422(5) . ? C17 C18 1.496(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.411(4) . ? C19 C20 1.486(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.296(4) . ? C21 C26 1.413(5) . ? C21 C22 1.419(5) . ? C22 O7 1.363(4) . ? C22 C23 1.390(6) . ? C23 C24 1.398(7) . ? C23 H23 0.9300 . ? C24 C25 1.352(7) . ? C24 H24 0.9300 . ? C25 C26 1.411(7) . ? C25 H25 0.9300 . ? C26 C27 1.426(6) . ? C27 N3 1.285(5) . ? C27 H27 0.9300 . ? C28A C29A 1.45(2) . ? C28A N3 1.629(19) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A N4 1.40(4) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C28B N3 1.437(14) . ? C28B C29B 1.453(19) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29B N4 1.58(3) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30 N4 1.277(5) . ? C30 C31 1.423(6) . ? C30 H30 0.9300 . ? C31 C36 1.395(5) . ? C31 C32 1.407(6) . ? C32 C33 1.351(6) . ? C32 H32 0.9300 . ? C33 C34 1.387(6) . ? C33 H33 0.9300 . ? C34 C35 1.372(5) . ? C34 H34 0.9300 . ? C35 O8 1.375(4) . ? C35 C36 1.410(5) . ? C36 O6 1.307(4) . ? C37 O7 1.424(4) . ? C37 C38 1.510(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O8 1.422(4) . ? C39 C40 1.480(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O9 1.309(3) . ? C41 C46 1.401(4) . ? C41 C42 1.414(4) . ? C42 O11 1.371(3) . ? C42 C43 1.378(5) . ? C43 C44 1.388(5) . ? C43 H43 0.9300 . ? C44 C45 1.342(5) . ? C44 H44 0.9300 . ? C45 C46 1.407(5) . ? C45 H45 0.9300 . ? C46 C47 1.427(5) . ? C47 N5 1.287(4) . ? C47 H47 0.9300 . ? C48 N5 1.473(3) . ? C48 C49 1.493(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 N6 1.480(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N6 1.291(4) . ? C50 C51 1.418(5) . ? C50 H50 0.9300 . ? C51 C56 1.394(5) . ? C51 C52 1.402(5) . ? C52 C53 1.365(6) . ? C52 H52 0.9300 . ? C53 C54 1.398(6) . ? C53 H53 0.9300 . ? C54 C55 1.372(5) . ? C54 H54 0.9300 . ? C55 O12 1.360(4) . ? C55 C56 1.435(5) . ? C56 O10 1.307(4) . ? C57 O11 1.427(4) . ? C57 C58 1.494(5) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O12 1.405(4) . ? C59 C60 1.492(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 O13 1.298(3) . ? C61 C66 1.412(3) . ? C61 C62 1.422(4) . ? C62 C63 1.367(4) . ? C62 O15 1.371(3) . ? C63 C64 1.383(5) . ? C63 H63 0.9300 . ? C64 C65 1.354(4) . ? C64 H64 0.9300 . ? C65 C66 1.423(5) . ? C65 H65 0.9300 . ? C66 C67 1.427(5) . ? C67 N7 1.286(4) . ? C67 H67 0.9300 . ? C68 C69 1.484(5) . ? C68 N7 1.485(4) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 N8 1.486(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 N8 1.288(4) . ? C70 C71 1.431(5) . ? C70 H70 0.9300 . ? C71 C76 1.399(4) . ? C71 C72 1.421(5) . ? C72 C73 1.362(5) . ? C72 H72 0.9300 . ? C73 C74 1.395(5) . ? C73 H73 0.9300 . ? C74 C75 1.365(4) . ? C74 H74 0.9300 . ? C75 O16 1.372(4) . ? C75 C76 1.419(4) . ? C76 O14 1.307(4) . ? C77 O15 1.419(4) . ? C77 C78 1.500(4) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 O16 1.435(4) . ? C79 C80 1.494(5) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 C82 1.387(4) . ? C81 C86 1.392(5) . ? C82 C83 1.383(5) . ? C82 H82 0.9300 . ? C83 C84 1.366(5) . ? C83 H83 0.9300 . ? C84 C85 1.367(5) . ? C84 H84 0.9300 . ? C85 C86 1.383(5) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 C88 1.390(5) . ? C87 C92 1.404(5) . ? C88 C89 1.391(5) . ? C88 H88 0.9300 . ? C89 C90 1.365(5) . ? C89 H89 0.9300 . ? C90 C91 1.372(5) . ? C90 H90 0.9300 . ? C91 C92 1.372(5) . ? C91 H91 0.9300 . ? C92 H92 0.9300 . ? C93 C98 1.389(5) . ? C93 C94 1.398(4) . ? C94 C95 1.389(5) . ? C94 H94 0.9300 . ? C95 C96 1.361(5) . ? C95 H95 0.9300 . ? C96 C97 1.373(5) . ? C96 H96 0.9300 . ? C97 C98 1.392(5) . ? C97 H97 0.9300 . ? C98 H98 0.9300 . ? C99 C100 1.387(4) . ? C99 C104 1.390(4) . ? C100 C101 1.385(4) . ? C100 H100 0.9300 . ? C101 C102 1.373(5) . ? C101 H101 0.9300 . ? C102 C103 1.380(5) . ? C102 H102 0.9300 . ? C103 C104 1.377(5) . ? C103 H103 0.9300 . ? C104 H104 0.9300 . ? C105 C110 1.368(5) . ? C105 C106 1.379(5) . ? C106 C107 1.388(6) . ? C106 H106 0.9300 . ? C107 C108 1.361(6) . ? C107 H107 0.9300 . ? C108 C109 1.342(6) . ? C108 H108 0.9300 . ? C109 C110 1.400(6) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C112 C113 1.3900 . ? C112 H112 0.9300 . ? C113 C114 1.3900 . ? C113 H113 0.9300 . ? C114 C115 1.3900 . ? C114 H114 0.9300 . ? C115 C116 1.3900 . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C117 C118 1.393(4) . ? C117 C122 1.393(5) . ? C118 C119 1.377(5) . ? C118 H118 0.9300 . ? C119 C120 1.364(5) . ? C119 H119 0.9300 . ? C120 C121 1.354(5) . ? C120 H120 0.9300 . ? C121 C122 1.376(5) . ? C121 H121 0.9300 . ? C122 H122 0.9300 . ? C123 C128 1.391(4) . ? C123 C124 1.406(5) . ? C124 C125 1.384(5) . ? C124 H124 0.9300 . ? C125 C126 1.358(5) . ? C125 H125 0.9300 . ? C126 C127 1.361(5) . ? C126 H126 0.9300 . ? C127 C128 1.396(5) . ? C127 H127 0.9300 . ? C128 H128 0.9300 . ? N1 Ni1 1.838(3) . ? N2 Ni1 1.847(3) . ? N3 Ni2 1.820(3) . ? N4 Ni2 1.849(3) . ? N5 Ni3 1.834(3) . ? N6 Ni3 1.834(3) . ? N7 Ni4 1.838(3) . ? N8 Ni4 1.833(3) . ? Ni1 O1 1.835(3) . ? Ni1 O2 1.839(2) . ? Ni2 O6 1.829(2) . ? Ni2 O5 1.845(2) . ? Ni3 O10 1.830(2) . ? Ni3 O9 1.841(2) . ? Ni4 O13 1.828(2) . ? Ni4 O14 1.838(2) . ? O1 Rb1 2.855(2) . ? O2 Rb1 2.875(2) . ? O3 Rb1 3.101(3) . ? O4 Rb1 2.960(3) . ? O5 Rb1 2.833(2) . ? O6 Rb1 2.798(2) . ? O7 Rb1 3.102(3) . ? O8 Rb1 3.064(2) . ? O9 Rb2 2.842(2) . ? O10 Rb2 2.844(2) . ? O11 Rb2 3.134(2) . ? O12 Rb2 3.003(2) . ? O13 Rb2 2.886(2) . ? O14 Rb2 2.772(2) . ? O15 Rb2 2.977(2) . ? O16 Rb2 2.993(2) . ? 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 C93 B1 C81 108.4(2) . . ? C93 B1 C87 110.4(2) . . ? C81 B1 C87 111.6(2) . . ? C93 B1 C99 109.1(2) . . ? C81 B1 C99 110.4(2) . . ? C87 B1 C99 106.8(2) . . ? C123 B2 C117 109.6(2) . . ? C123 B2 C105 110.4(2) . . ? C117 B2 C105 107.8(2) . . ? C123 B2 C111 108.3(2) . . ? C117 B2 C111 111.5(2) . . ? C105 B2 C111 109.2(2) . . ? O1 C1 C2 117.8(4) . . ? O1 C1 C6 124.8(5) . . ? C2 C1 C6 117.4(4) . . ? O3 C2 C3 124.5(5) . . ? O3 C2 C1 114.9(4) . . ? C3 C2 C1 120.6(5) . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.8(7) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.0(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 120.5(5) . . ? C5 C6 C1 120.3(6) . . ? C7 C6 C1 119.2(5) . . ? N1 C7 C6 127.9(4) . . ? N1 C7 H7 116.0 . . ? C6 C7 H7 116.0 . . ? C9 C8 N1 106.6(3) . . ? C9 C8 H8A 110.4 . . ? N1 C8 H8A 110.4 . . ? C9 C8 H8B 110.4 . . ? N1 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N2 C9 C8 107.0(4) . . ? N2 C9 H9A 110.3 . . ? C8 C9 H9A 110.3 . . ? N2 C9 H9B 110.3 . . ? C8 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 125.7(4) . . ? N2 C10 H10 117.2 . . ? C11 C10 H10 117.2 . . ? C16 C11 C12 120.8(5) . . ? C16 C11 C10 120.1(4) . . ? C12 C11 C10 119.0(5) . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.3(5) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C15 C14 C13 119.1(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? O4 C15 C14 123.9(4) . . ? O4 C15 C16 113.8(4) . . ? C14 C15 C16 122.3(4) . . ? O2 C16 C11 125.5(4) . . ? O2 C16 C15 117.9(4) . . ? C11 C16 C15 116.5(4) . . ? O3 C17 C18 107.9(4) . . ? O3 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? O3 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 107.2(3) . . ? O4 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O4 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C26 124.9(4) . . ? O5 C21 C22 117.9(4) . . ? C26 C21 C22 117.2(4) . . ? O7 C22 C23 125.0(4) . . ? O7 C22 C21 113.8(4) . . ? C23 C22 C21 121.2(4) . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.7(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.7(5) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 120.4(5) . . ? C21 C26 C27 119.4(5) . . ? C25 C26 C27 120.1(5) . . ? N3 C27 C26 126.7(4) . . ? N3 C27 H27 116.6 . . ? C26 C27 H27 116.6 . . ? C29A C28A N3 104.4(18) . . ? C29A C28A H28A 110.9 . . ? N3 C28A H28A 110.9 . . ? C29A C28A H28B 110.9 . . ? N3 C28A H28B 110.9 . . ? H28A C28A H28B 108.9 . . ? N4 C29A C28A 105(2) . . ? N4 C29A H29A 110.7 . . ? C28A C29A H29A 110.7 . . ? N4 C29A H29B 110.7 . . ? C28A C29A H29B 110.7 . . ? H29A C29A H29B 108.8 . . ? N3 C28B C29B 100.2(18) . . ? N3 C28B H28C 111.7 . . ? C29B C28B H28C 111.7 . . ? N3 C28B H28D 111.7 . . ? C29B C28B H28D 111.7 . . ? H28C C28B H28D 109.5 . . ? C28B C29B N4 111(2) . . ? C28B C29B H29C 109.3 . . ? N4 C29B H29C 109.3 . . ? C28B C29B H29D 109.3 . . ? N4 C29B H29D 109.3 . . ? H29C C29B H29D 108.0 . . ? N4 C30 C31 126.1(4) . . ? N4 C30 H30 116.9 . . ? C31 C30 H30 116.9 . . ? C36 C31 C32 120.8(5) . . ? C36 C31 C30 120.4(5) . . ? C32 C31 C30 118.9(5) . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 O8 124.6(4) . . ? C34 C35 C36 121.4(4) . . ? O8 C35 C36 114.0(4) . . ? O6 C36 C31 124.5(4) . . ? O6 C36 C35 118.3(3) . . ? C31 C36 C35 117.2(4) . . ? O7 C37 C38 107.0(3) . . ? O7 C37 H37A 110.3 . . ? C38 C37 H37A 110.3 . . ? O7 C37 H37B 110.3 . . ? C38 C37 H37B 110.3 . . ? H37A C37 H37B 108.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 107.1(3) . . ? O8 C39 H39A 110.3 . . ? C40 C39 H39A 110.3 . . ? O8 C39 H39B 110.3 . . ? C40 C39 H39B 110.3 . . ? H39A C39 H39B 108.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O9 C41 C46 123.5(3) . . ? O9 C41 C42 118.0(3) . . ? C46 C41 C42 118.5(3) . . ? O11 C42 C43 125.3(3) . . ? O11 C42 C41 114.6(3) . . ? C43 C42 C41 120.1(3) . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 121.2(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C41 C46 C45 119.4(4) . . ? C41 C46 C47 120.9(3) . . ? C45 C46 C47 119.7(4) . . ? N5 C47 C46 126.4(3) . . ? N5 C47 H47 116.8 . . ? C46 C47 H47 116.8 . . ? N5 C48 C49 108.1(3) . . ? N5 C48 H48A 110.1 . . ? C49 C48 H48A 110.1 . . ? N5 C48 H48B 110.1 . . ? C49 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? N6 C49 C48 109.6(3) . . ? N6 C49 H49A 109.7 . . ? C48 C49 H49A 109.7 . . ? N6 C49 H49B 109.7 . . ? C48 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? N6 C50 C51 126.2(3) . . ? N6 C50 H50 116.9 . . ? C51 C50 H50 116.9 . . ? C56 C51 C52 119.8(4) . . ? C56 C51 C50 119.8(4) . . ? C52 C51 C50 120.4(4) . . ? C53 C52 C51 121.1(5) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 119.8(5) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C55 C54 C53 120.9(5) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? O12 C55 C54 126.7(4) . . ? O12 C55 C56 113.6(3) . . ? C54 C55 C56 119.7(4) . . ? O10 C56 C51 125.0(3) . . ? O10 C56 C55 116.3(3) . . ? C51 C56 C55 118.7(3) . . ? O11 C57 C58 108.0(3) . . ? O11 C57 H57A 110.1 . . ? C58 C57 H57A 110.1 . . ? O11 C57 H57B 110.1 . . ? C58 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O12 C59 C60 107.4(3) . . ? O12 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O12 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O13 C61 C66 124.2(3) . . ? O13 C61 C62 118.3(3) . . ? C66 C61 C62 117.4(3) . . ? C63 C62 O15 125.1(3) . . ? C63 C62 C61 121.1(3) . . ? O15 C62 C61 113.9(3) . . ? C62 C63 C64 120.6(4) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C65 C64 C63 120.9(3) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C61 C66 C65 119.8(3) . . ? C61 C66 C67 120.7(3) . . ? C65 C66 C67 119.4(3) . . ? N7 C67 C66 125.3(3) . . ? N7 C67 H67 117.4 . . ? C66 C67 H67 117.4 . . ? C69 C68 N7 106.8(3) . . ? C69 C68 H68A 110.4 . . ? N7 C68 H68A 110.4 . . ? C69 C68 H68B 110.4 . . ? N7 C68 H68B 110.4 . . ? H68A C68 H68B 108.6 . . ? C68 C69 N8 106.5(3) . . ? C68 C69 H69A 110.4 . . ? N8 C69 H69A 110.4 . . ? C68 C69 H69B 110.4 . . ? N8 C69 H69B 110.4 . . ? H69A C69 H69B 108.6 . . ? N8 C70 C71 125.0(3) . . ? N8 C70 H70 117.5 . . ? C71 C70 H70 117.5 . . ? C76 C71 C72 120.1(3) . . ? C76 C71 C70 120.9(3) . . ? C72 C71 C70 119.0(3) . . ? C73 C72 C71 120.0(4) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.5(4) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C75 C74 C73 120.2(4) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 O16 124.2(3) . . ? C74 C75 C76 121.4(3) . . ? O16 C75 C76 114.5(3) . . ? O14 C76 C71 124.3(3) . . ? O14 C76 C75 118.0(3) . . ? C71 C76 C75 117.7(3) . . ? O15 C77 C78 107.6(3) . . ? O15 C77 H77A 110.2 . . ? C78 C77 H77A 110.2 . . ? O15 C77 H77B 110.2 . . ? C78 C77 H77B 110.2 . . ? H77A C77 H77B 108.5 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O16 C79 C80 107.2(3) . . ? O16 C79 H79A 110.3 . . ? C80 C79 H79A 110.3 . . ? O16 C79 H79B 110.3 . . ? C80 C79 H79B 110.3 . . ? H79A C79 H79B 108.5 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 C86 114.1(3) . . ? C82 C81 B1 124.9(3) . . ? C86 C81 B1 120.8(3) . . ? C83 C82 C81 122.9(4) . . ? C83 C82 H82 118.5 . . ? C81 C82 H82 118.5 . . ? C84 C83 C82 120.7(4) . . ? C84 C83 H83 119.6 . . ? C82 C83 H83 119.6 . . ? C83 C84 C85 118.7(4) . . ? C83 C84 H84 120.6 . . ? C85 C84 H84 120.6 . . ? C84 C85 C86 119.8(4) . . ? C84 C85 H85 120.1 . . ? C86 C85 H85 120.1 . . ? C85 C86 C81 123.7(4) . . ? C85 C86 H86 118.2 . . ? C81 C86 H86 118.2 . . ? C88 C87 C92 113.5(3) . . ? C88 C87 B1 125.0(3) . . ? C92 C87 B1 121.4(3) . . ? C89 C88 C87 123.6(4) . . ? C89 C88 H88 118.2 . . ? C87 C88 H88 118.2 . . ? C90 C89 C88 119.8(4) . . ? C90 C89 H89 120.1 . . ? C88 C89 H89 120.1 . . ? C89 C90 C91 119.1(4) . . ? C89 C90 H90 120.4 . . ? C91 C90 H90 120.4 . . ? C92 C91 C90 120.1(4) . . ? C92 C91 H91 120.0 . . ? C90 C91 H91 120.0 . . ? C91 C92 C87 123.8(4) . . ? C91 C92 H92 118.1 . . ? C87 C92 H92 118.1 . . ? C98 C93 C94 113.5(3) . . ? C98 C93 B1 122.0(3) . . ? C94 C93 B1 124.4(3) . . ? C95 C94 C93 123.0(4) . . ? C95 C94 H94 118.5 . . ? C93 C94 H94 118.5 . . ? C96 C95 C94 120.5(4) . . ? C96 C95 H95 119.7 . . ? C94 C95 H95 119.7 . . ? C95 C96 C97 119.5(4) . . ? C95 C96 H96 120.2 . . ? C97 C96 H96 120.2 . . ? C96 C97 C98 118.7(4) . . ? C96 C97 H97 120.7 . . ? C98 C97 H97 120.7 . . ? C93 C98 C97 124.7(4) . . ? C93 C98 H98 117.6 . . ? C97 C98 H98 117.6 . . ? C100 C99 C104 114.9(3) . . ? C100 C99 B1 123.5(3) . . ? C104 C99 B1 121.6(3) . . ? C101 C100 C99 122.6(3) . . ? C101 C100 H100 118.7 . . ? C99 C100 H100 118.7 . . ? C102 C101 C100 120.5(4) . . ? C102 C101 H101 119.8 . . ? C100 C101 H101 119.8 . . ? C101 C102 C103 118.6(4) . . ? C101 C102 H102 120.7 . . ? C103 C102 H102 120.7 . . ? C104 C103 C102 119.7(4) . . ? C104 C103 H103 120.1 . . ? C102 C103 H103 120.1 . . ? C103 C104 C99 123.6(4) . . ? C103 C104 H104 118.2 . . ? C99 C104 H104 118.2 . . ? C110 C105 C106 114.3(4) . . ? C110 C105 B2 123.9(3) . . ? C106 C105 B2 121.8(3) . . ? C105 C106 C107 123.5(4) . . ? C105 C106 H106 118.3 . . ? C107 C106 H106 118.3 . . ? C108 C107 C106 120.1(5) . . ? C108 C107 H107 119.9 . . ? C106 C107 H107 119.9 . . ? C109 C108 C107 118.3(5) . . ? C109 C108 H108 120.9 . . ? C107 C108 H108 120.9 . . ? C108 C109 C110 121.0(5) . . ? C108 C109 H109 119.5 . . ? C110 C109 H109 119.5 . . ? C105 C110 C109 122.8(4) . . ? C105 C110 H110 118.6 . . ? C109 C110 H110 118.6 . . ? C112 C111 C116 120.0 . . ? C112 C111 B2 118.2(2) . . ? C116 C111 B2 121.8(2) . . ? C111 C112 C113 120.0 . . ? C111 C112 H112 120.0 . . ? C113 C112 H112 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 C111 120.0 . . ? C115 C116 H116 120.0 . . ? C111 C116 H116 120.0 . . ? C118 C117 C122 113.1(3) . . ? C118 C117 B2 125.2(3) . . ? C122 C117 B2 121.6(3) . . ? C119 C118 C117 123.0(4) . . ? C119 C118 H118 118.5 . . ? C117 C118 H118 118.5 . . ? C120 C119 C118 121.5(4) . . ? C120 C119 H119 119.3 . . ? C118 C119 H119 119.3 . . ? C121 C120 C119 117.8(4) . . ? C121 C120 H120 121.1 . . ? C119 C120 H120 121.1 . . ? C120 C121 C122 120.6(4) . . ? C120 C121 H121 119.7 . . ? C122 C121 H121 119.7 . . ? C121 C122 C117 124.1(4) . . ? C121 C122 H122 118.0 . . ? C117 C122 H122 118.0 . . ? C128 C123 C124 112.8(3) . . ? C128 C123 B2 125.5(3) . . ? C124 C123 B2 121.6(3) . . ? C125 C124 C123 124.1(4) . . ? C125 C124 H124 117.9 . . ? C123 C124 H124 117.9 . . ? C126 C125 C124 120.5(4) . . ? C126 C125 H125 119.8 . . ? C124 C125 H125 119.8 . . ? C125 C126 C127 118.2(4) . . ? C125 C126 H126 120.9 . . ? C127 C126 H126 120.9 . . ? C126 C127 C128 121.2(4) . . ? C126 C127 H127 119.4 . . ? C128 C127 H127 119.4 . . ? C123 C128 C127 123.1(4) . . ? C123 C128 H128 118.4 . . ? C127 C128 H128 118.4 . . ? C7 N1 C8 121.5(3) . . ? C7 N1 Ni1 125.1(2) . . ? C8 N1 Ni1 113.2(2) . . ? C10 N2 C9 120.3(3) . . ? C10 N2 Ni1 126.7(2) . . ? C9 N2 Ni1 112.6(2) . . ? C27 N3 C28B 113.3(7) . . ? C27 N3 C28A 123.5(5) . . ? C28B N3 C28A 32.1(7) . . ? C27 N3 Ni2 126.5(2) . . ? C28B N3 Ni2 118.8(7) . . ? C28A N3 Ni2 107.2(5) . . ? C30 N4 C29A 116.6(9) . . ? C30 N4 C29B 126.0(10) . . ? C29A N4 C29B 21(2) . . ? C30 N4 Ni2 126.8(2) . . ? C29A N4 Ni2 116.2(9) . . ? C29B N4 Ni2 106.1(11) . . ? C47 N5 C48 118.5(2) . . ? C47 N5 Ni3 126.27(17) . . ? C48 N5 Ni3 115.10(16) . . ? C50 N6 C49 120.2(2) . . ? C50 N6 Ni3 126.45(19) . . ? C49 N6 Ni3 113.32(17) . . ? C67 N7 C68 119.6(3) . . ? C67 N7 Ni4 126.9(3) . . ? C68 N7 Ni4 113.4(3) . . ? C70 N8 C69 119.8(3) . . ? C70 N8 Ni4 127.0(3) . . ? C69 N8 Ni4 113.1(3) . . ? O1 Ni1 O2 84.56(10) . . ? O1 Ni1 N1 95.04(13) . . ? O2 Ni1 N1 176.83(12) . . ? O1 Ni1 N2 176.65(12) . . ? O2 Ni1 N2 94.53(13) . . ? N1 Ni1 N2 86.04(15) . . ? N3 Ni2 O6 176.36(13) . . ? N3 Ni2 O5 94.88(14) . . ? O6 Ni2 O5 84.63(10) . . ? N3 Ni2 N4 86.61(16) . . ? O6 Ni2 N4 94.07(13) . . ? O5 Ni2 N4 176.60(13) . . ? O10 Ni3 N6 94.13(11) . . ? O10 Ni3 N5 178.52(11) . . ? N6 Ni3 N5 87.34(12) . . ? O10 Ni3 O9 83.84(9) . . ? N6 Ni3 O9 177.81(12) . . ? N5 Ni3 O9 94.68(11) . . ? O13 Ni4 N8 176.73(12) . . ? O13 Ni4 O14 84.27(9) . . ? N8 Ni4 O14 94.49(12) . . ? O13 Ni4 N7 94.84(12) . . ? N8 Ni4 N7 86.61(14) . . ? O14 Ni4 N7 175.85(12) . . ? C1 O1 Ni1 127.5(2) . . ? C1 O1 Rb1 120.4(2) . . ? Ni1 O1 Rb1 104.98(10) . . ? C16 O2 Ni1 127.07(19) . . ? C16 O2 Rb1 119.39(18) . . ? Ni1 O2 Rb1 104.14(10) . . ? C2 O3 C17 118.8(3) . . ? C2 O3 Rb1 111.6(2) . . ? C17 O3 Rb1 120.6(2) . . ? C15 O4 C19 118.9(3) . . ? C15 O4 Rb1 115.79(18) . . ? C19 O4 Rb1 123.6(2) . . ? C21 O5 Ni2 127.3(2) . . ? C21 O5 Rb1 125.45(19) . . ? Ni2 O5 Rb1 101.61(10) . . ? C36 O6 Ni2 128.15(19) . . ? C36 O6 Rb1 116.55(17) . . ? Ni2 O6 Rb1 103.34(10) . . ? C22 O7 C37 117.1(3) . . ? C22 O7 Rb1 116.5(2) . . ? C37 O7 Rb1 125.4(2) . . ? C35 O8 C39 118.5(3) . . ? C35 O8 Rb1 108.49(18) . . ? C39 O8 Rb1 122.92(19) . . ? C41 O9 Ni3 128.23(15) . . ? C41 O9 Rb2 119.61(14) . . ? Ni3 O9 Rb2 102.51(9) . . ? C56 O10 Ni3 127.63(18) . . ? C56 O10 Rb2 122.07(17) . . ? Ni3 O10 Rb2 102.75(9) . . ? C42 O11 C57 117.6(2) . . ? C42 O11 Rb2 110.60(15) . . ? C57 O11 Rb2 124.31(16) . . ? C55 O12 C59 119.9(3) . . ? C55 O12 Rb2 116.83(16) . . ? C59 O12 Rb2 122.2(2) . . ? C61 O13 Ni4 127.79(14) . . ? C61 O13 Rb2 120.91(14) . . ? Ni4 O13 Rb2 103.17(9) . . ? C76 O14 Ni4 127.0(2) . . ? C76 O14 Rb2 121.68(19) . . ? Ni4 O14 Rb2 107.20(10) . . ? C62 O15 C77 117.5(2) . . ? C62 O15 Rb2 117.10(14) . . ? C77 O15 Rb2 120.90(19) . . ? C75 O16 C79 117.2(3) . . ? C75 O16 Rb2 113.94(19) . . ? C79 O16 Rb2 124.31(19) . . ? O6 Rb1 O5 52.12(7) . . ? O6 Rb1 O1 77.40(7) . . ? O5 Rb1 O1 109.59(7) . . ? O6 Rb1 O2 109.05(7) . . ? O5 Rb1 O2 158.57(7) . . ? O1 Rb1 O2 51.10(7) . . ? O6 Rb1 O4 152.90(7) . . ? O5 Rb1 O4 149.10(7) . . ? O1 Rb1 O4 97.80(7) . . ? O2 Rb1 O4 52.27(7) . . ? O6 Rb1 O8 52.25(7) . . ? O5 Rb1 O8 96.09(7) . . ? O1 Rb1 O8 83.81(7) . . ? O2 Rb1 O8 74.42(7) . . ? O4 Rb1 O8 100.93(7) . . ? O6 Rb1 O7 95.98(7) . . ? O5 Rb1 O7 51.26(7) . . ? O1 Rb1 O7 155.48(7) . . ? O2 Rb1 O7 150.01(6) . . ? O4 Rb1 O7 98.28(7) . . ? O8 Rb1 O7 111.02(7) . . ? O6 Rb1 O3 83.73(7) . . ? O5 Rb1 O3 74.78(7) . . ? O1 Rb1 O3 51.57(7) . . ? O2 Rb1 O3 94.57(7) . . ? O4 Rb1 O3 114.46(8) . . ? O8 Rb1 O3 124.61(7) . . ? O7 Rb1 O3 104.61(7) . . ? O14 Rb2 O9 130.28(6) . . ? O14 Rb2 O10 172.31(6) . . ? O9 Rb2 O10 51.10(6) . . ? O14 Rb2 O13 51.48(6) . . ? O9 Rb2 O13 176.55(6) . . ? O10 Rb2 O13 126.66(6) . . ? O14 Rb2 O15 99.15(7) . . ? O9 Rb2 O15 127.27(6) . . ? O10 Rb2 O15 82.60(6) . . ? O13 Rb2 O15 52.53(6) . . ? O14 Rb2 O16 53.53(6) . . ? O9 Rb2 O16 86.76(6) . . ? O10 Rb2 O16 132.30(6) . . ? O13 Rb2 O16 96.33(6) . . ? O15 Rb2 O16 116.36(7) . . ? O14 Rb2 O12 121.90(7) . . ? O9 Rb2 O12 95.02(6) . . ? O10 Rb2 O12 51.86(6) . . ? O13 Rb2 O12 81.76(6) . . ? O15 Rb2 O12 66.83(7) . . ? O16 Rb2 O12 174.13(7) . . ? O14 Rb2 O11 83.90(6) . . ? O9 Rb2 O11 51.31(6) . . ? O10 Rb2 O11 93.86(6) . . ? O13 Rb2 O11 128.52(6) . . ? O15 Rb2 O11 175.00(6) . . ? O16 Rb2 O11 68.65(6) . . ? O12 Rb2 O11 108.20(7) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.248 0.019 0.105 157 23 ' ' 2 0.290 0.183 0.548 32 0 ' ' 3 0.447 0.528 0.349 21 0 ' ' 4 0.553 0.472 0.651 21 0 ' ' 5 0.751 -0.019 0.895 157 22 ' ' 6 0.710 0.817 0.452 32 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.685 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.053 #END=== data_5 _database_code_depnum_ccdc_archive 'CCDC 813960' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H47 Cl Cs N5 Ni2 O12' _chemical_formula_weight 1099.63 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' Cs Cs -0.3680 2.1192 '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 13.5600(19) _cell_length_b 14.089(2) _cell_length_c 14.473(2) _cell_angle_alpha 68.785(6) _cell_angle_beta 68.942(5) _cell_angle_gamma 67.311(5) _cell_volume 2299.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5715 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 23.12 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7245 _exptl_absorpt_correction_T_max 0.7822 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29152 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10139 _reflns_number_gt 6406 _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^)+(0.1100P)^2^+0.4500P] 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 10139 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _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 C1 C 0.2772(4) 0.5717(4) 0.1072(3) 0.0595(12) Uani 1 1 d . . . C2 C 0.1724(5) 0.5697(5) 0.1073(3) 0.0670(13) Uani 1 1 d . . . C3 C 0.0870(5) 0.6627(6) 0.0918(4) 0.0887(19) Uani 1 1 d . . . H3 H 0.0186 0.6601 0.0943 0.106 Uiso 1 1 calc R . . C4 C 0.1038(7) 0.7610(6) 0.0723(4) 0.097(2) Uani 1 1 d . . . H4 H 0.0463 0.8234 0.0618 0.117 Uiso 1 1 calc R . . C5 C 0.2034(6) 0.7658(5) 0.0686(4) 0.0882(19) Uani 1 1 d . . . H5 H 0.2139 0.8316 0.0546 0.106 Uiso 1 1 calc R . . C6 C 0.2906(5) 0.6718(4) 0.0858(3) 0.0712(15) Uani 1 1 d . . . C7 C 0.3953(6) 0.6810(5) 0.0773(4) 0.0764(17) Uani 1 1 d . . . H7 H 0.4005 0.7495 0.0600 0.092 Uiso 1 1 calc R . . C8 C 0.5876(6) 0.6266(5) 0.0659(5) 0.0882(19) Uani 1 1 d . . . H8A H 0.5744 0.6944 0.0779 0.106 Uiso 1 1 calc R . . H8B H 0.6259 0.6297 -0.0056 0.106 Uiso 1 1 calc R . . C9 C 0.6550(5) 0.5392(6) 0.1330(5) 0.0875(18) Uani 1 1 d . . . H9A H 0.7330 0.5329 0.1024 0.105 Uiso 1 1 calc R . . H9B H 0.6346 0.5530 0.1994 0.105 Uiso 1 1 calc R . . C10 C 0.7056(5) 0.3519(6) 0.1663(4) 0.0792(17) Uani 1 1 d . . . H10 H 0.7707 0.3549 0.1714 0.095 Uiso 1 1 calc R . . C11 C 0.6972(4) 0.2494(5) 0.1837(4) 0.0722(14) Uani 1 1 d . . . C12 C 0.7872(5) 0.1570(7) 0.2053(4) 0.096(2) Uani 1 1 d . . . H12 H 0.8504 0.1647 0.2097 0.115 Uiso 1 1 calc R . . C13 C 0.7823(6) 0.0600(7) 0.2192(6) 0.104(2) Uani 1 1 d . . . H13 H 0.8415 0.0007 0.2343 0.125 Uiso 1 1 calc R . . C14 C 0.6897(6) 0.0466(5) 0.2113(5) 0.0927(19) Uani 1 1 d . . . H14 H 0.6881 -0.0213 0.2191 0.111 Uiso 1 1 calc R . . C15 C 0.6005(5) 0.1333(4) 0.1920(4) 0.0720(14) Uani 1 1 d . . . C16 C 0.6005(4) 0.2371(4) 0.1791(3) 0.0596(12) Uani 1 1 d . . . C17 C 0.0665(5) 0.4627(6) 0.1157(4) 0.0890(19) Uani 1 1 d . . . H17A H 0.0522 0.5067 0.0500 0.107 Uiso 1 1 calc R . . H17B H 0.0039 0.4874 0.1695 0.107 Uiso 1 1 calc R . . C18 C 0.0831(6) 0.3488(6) 0.1254(5) 0.097(2) Uani 1 1 d . . . H18A H 0.1450 0.3253 0.0716 0.145 Uiso 1 1 calc R . . H18B H 0.0179 0.3418 0.1200 0.145 Uiso 1 1 calc R . . H18C H 0.0972 0.3061 0.1907 0.145 Uiso 1 1 calc R . . C19 C 0.5091(7) 0.0298(5) 0.1750(7) 0.109(2) Uani 1 1 d . . . H19A H 0.5189 -0.0252 0.2378 0.130 Uiso 1 1 calc R . . H19B H 0.5710 0.0087 0.1191 0.130 Uiso 1 1 calc R . . C20 C 0.4025(8) 0.0427(7) 0.1552(8) 0.139(3) Uani 1 1 d . . . H20A H 0.3418 0.0618 0.2116 0.209 Uiso 1 1 calc R . . H20B H 0.4046 -0.0232 0.1479 0.209 Uiso 1 1 calc R . . H20C H 0.3930 0.0977 0.0934 0.209 Uiso 1 1 calc R . . C21 C -0.0248(3) 0.3659(3) 0.3953(3) 0.0456(9) Uani 1 1 d . . . C22 C -0.0075(4) 0.2563(4) 0.4100(3) 0.0540(11) Uani 1 1 d . . . C23 C -0.0889(5) 0.2218(5) 0.4074(4) 0.0699(14) Uani 1 1 d . . . H23 H -0.0756 0.1497 0.4160 0.084 Uiso 1 1 calc R . . C24 C -0.1904(5) 0.2928(5) 0.3923(4) 0.0749(15) Uani 1 1 d . . . H24 H -0.2439 0.2687 0.3895 0.090 Uiso 1 1 calc R . . C25 C -0.2101(4) 0.3976(5) 0.3817(4) 0.0647(13) Uani 1 1 d . . . H25 H -0.2786 0.4449 0.3736 0.078 Uiso 1 1 calc R . . C26 C -0.1290(3) 0.4364(4) 0.3827(3) 0.0496(10) Uani 1 1 d . . . C27 C -0.1556(4) 0.5453(4) 0.3786(3) 0.0555(11) Uani 1 1 d . . . H27 H -0.2273 0.5874 0.3756 0.067 Uiso 1 1 calc R . . C28 C -0.1330(4) 0.7009(4) 0.3887(3) 0.0647(13) Uani 1 1 d . . . H28A H -0.1557 0.7010 0.4604 0.078 Uiso 1 1 calc R . . H28B H -0.1964 0.7401 0.3600 0.078 Uiso 1 1 calc R . . C29 C -0.0422(4) 0.7509(4) 0.3319(4) 0.0658(13) Uani 1 1 d . . . H29A H -0.0544 0.8109 0.3567 0.079 Uiso 1 1 calc R . . H29B H -0.0388 0.7761 0.2592 0.079 Uiso 1 1 calc R . . C30 C 0.1467(5) 0.6957(4) 0.3409(3) 0.0660(14) Uani 1 1 d . . . H30 H 0.1377 0.7682 0.3245 0.079 Uiso 1 1 calc R . . C31 C 0.2523(4) 0.6242(4) 0.3542(3) 0.0597(12) Uani 1 1 d . . . C32 C 0.3336(5) 0.6674(5) 0.3484(4) 0.0759(16) Uani 1 1 d . . . H32 H 0.3192 0.7408 0.3324 0.091 Uiso 1 1 calc R . . C33 C 0.4318(6) 0.6022(7) 0.3662(4) 0.089(2) Uani 1 1 d . . . H33 H 0.4848 0.6311 0.3622 0.107 Uiso 1 1 calc R . . C34 C 0.4552(5) 0.4909(6) 0.3907(4) 0.0808(17) Uani 1 1 d . . . H34 H 0.5229 0.4466 0.4037 0.097 Uiso 1 1 calc R . . C35 C 0.3778(4) 0.4478(5) 0.3954(3) 0.0614(12) Uani 1 1 d . . . C36 C 0.2740(4) 0.5146(4) 0.3758(3) 0.0513(11) Uani 1 1 d . . . C37 C 0.1092(5) 0.0797(4) 0.4615(5) 0.0766(15) Uani 1 1 d . . . H37A H 0.1041 0.0527 0.4111 0.092 Uiso 1 1 calc R . . H37B H 0.0524 0.0650 0.5240 0.092 Uiso 1 1 calc R . . C38 C 0.2210(6) 0.0274(5) 0.4824(6) 0.101(2) Uani 1 1 d . . . H38A H 0.2769 0.0372 0.4191 0.151 Uiso 1 1 calc R . . H38B H 0.2305 -0.0474 0.5133 0.151 Uiso 1 1 calc R . . H38C H 0.2273 0.0587 0.5281 0.151 Uiso 1 1 calc R . . C39 C 0.4864(5) 0.2671(6) 0.4546(5) 0.0917(19) Uani 1 1 d . . . H39A H 0.4902 0.2819 0.5134 0.110 Uiso 1 1 calc R . . H39B H 0.5528 0.2737 0.4003 0.110 Uiso 1 1 calc R . . C40 C 0.4777(6) 0.1578(6) 0.4827(7) 0.125(3) Uani 1 1 d . . . H40A H 0.4110 0.1523 0.5355 0.187 Uiso 1 1 calc R . . H40B H 0.5403 0.1073 0.5073 0.187 Uiso 1 1 calc R . . H40C H 0.4761 0.1430 0.4236 0.187 Uiso 1 1 calc R . . C41 C 0.1249(10) 0.0700(8) 0.0798(7) 0.174(5) Uani 1 1 d . . . H41A H 0.1143 0.0291 0.0454 0.260 Uiso 1 1 calc R . . H41B H 0.1998 0.0731 0.0542 0.260 Uiso 1 1 calc R . . H41C H 0.0752 0.1409 0.0673 0.260 Uiso 1 1 calc R . . C42 C 0.1030(7) 0.0205(6) 0.1881(7) 0.108(2) Uani 1 1 d . . . Cl1 Cl 0.73568(13) 0.75425(11) 0.15864(10) 0.0734(4) Uani 1 1 d . . . Cs1 Cs 0.29003(2) 0.29071(2) 0.28173(2) 0.05896(12) Uani 1 1 d . . . N1 N 0.4822(4) 0.6041(4) 0.0911(3) 0.0685(11) Uani 1 1 d . . . N2 N 0.6327(4) 0.4406(4) 0.1442(3) 0.0666(11) Uani 1 1 d . . . N3 N -0.0903(3) 0.5913(3) 0.3787(2) 0.0516(9) Uani 1 1 d . . . N4 N 0.0623(3) 0.6676(3) 0.3498(2) 0.0549(9) Uani 1 1 d . . . N5 N 0.0850(9) -0.0178(7) 0.2687(6) 0.164(4) Uani 1 1 d . . . Ni2 Ni 0.05792(4) 0.53137(4) 0.37573(4) 0.04496(15) Uani 1 1 d . . . Ni1 Ni 0.49517(5) 0.46117(5) 0.13034(4) 0.05481(17) Uani 1 1 d . . . O1 O 0.3543(3) 0.4812(2) 0.1237(2) 0.0587(8) Uani 1 1 d . . . O2 O 0.5130(3) 0.3172(3) 0.1614(2) 0.0602(8) Uani 1 1 d . . . O3 O 0.1652(3) 0.4695(3) 0.1243(2) 0.0682(9) Uani 1 1 d . . . O4 O 0.5055(4) 0.1272(3) 0.1837(3) 0.0871(11) Uani 1 1 d . . . O5 O 0.0565(2) 0.3943(2) 0.3949(2) 0.0476(6) Uani 1 1 d . . . O6 O 0.2042(2) 0.4686(2) 0.3797(2) 0.0505(7) Uani 1 1 d . . . O7 O 0.0947(3) 0.1905(3) 0.4242(3) 0.0648(8) Uani 1 1 d . . . O8 O 0.3906(3) 0.3409(3) 0.4205(3) 0.0689(9) Uani 1 1 d . . . O9 O 0.6829(5) 0.8101(4) 0.0781(4) 0.1165(17) Uani 1 1 d . . . O10 O 0.7995(4) 0.8123(4) 0.1596(4) 0.1061(14) Uani 1 1 d . . . O11 O 0.6554(4) 0.7413(5) 0.2520(4) 0.130(2) Uani 1 1 d . . . O12 O 0.8043(4) 0.6532(4) 0.1456(4) 0.1144(16) 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 C1 0.067(3) 0.057(3) 0.040(2) -0.0141(19) -0.008(2) -0.008(2) C2 0.066(4) 0.079(4) 0.042(2) -0.015(2) -0.010(2) -0.011(3) C3 0.078(4) 0.103(5) 0.056(3) -0.016(3) -0.018(3) -0.001(4) C4 0.103(6) 0.079(4) 0.064(3) -0.008(3) -0.018(3) 0.008(4) C5 0.107(5) 0.063(3) 0.064(3) -0.015(3) -0.013(3) -0.002(4) C6 0.091(4) 0.062(3) 0.043(2) -0.014(2) -0.010(2) -0.012(3) C7 0.112(5) 0.063(3) 0.054(3) -0.020(2) -0.002(3) -0.039(4) C8 0.110(5) 0.101(5) 0.074(3) -0.030(3) 0.000(3) -0.066(4) C9 0.078(4) 0.123(5) 0.083(4) -0.042(4) -0.001(3) -0.055(4) C10 0.056(4) 0.132(6) 0.057(3) -0.031(3) -0.009(2) -0.034(4) C11 0.052(3) 0.101(4) 0.052(3) -0.017(3) -0.010(2) -0.017(3) C12 0.055(4) 0.139(7) 0.072(4) -0.020(4) -0.021(3) -0.008(4) C13 0.074(5) 0.098(5) 0.112(5) -0.021(4) -0.037(4) 0.009(4) C14 0.088(5) 0.076(4) 0.090(4) -0.017(3) -0.029(4) 0.002(4) C15 0.056(3) 0.070(3) 0.072(3) -0.019(3) -0.017(2) 0.002(3) C16 0.046(3) 0.076(3) 0.045(2) -0.015(2) -0.0080(19) -0.009(2) C17 0.060(4) 0.144(6) 0.064(3) -0.016(3) -0.022(3) -0.037(4) C18 0.091(5) 0.145(6) 0.077(4) -0.026(4) -0.019(3) -0.062(5) C19 0.115(6) 0.073(4) 0.138(6) -0.034(4) -0.046(5) -0.008(4) C20 0.164(9) 0.107(6) 0.183(9) -0.046(6) -0.073(7) -0.043(6) C21 0.038(2) 0.062(3) 0.0347(17) -0.0121(17) -0.0061(15) -0.016(2) C22 0.051(3) 0.060(3) 0.052(2) -0.0064(19) -0.0105(19) -0.027(2) C23 0.070(4) 0.075(3) 0.073(3) -0.012(3) -0.018(3) -0.037(3) C24 0.055(3) 0.100(4) 0.086(3) -0.023(3) -0.021(3) -0.038(3) C25 0.040(3) 0.091(4) 0.061(3) -0.021(3) -0.011(2) -0.018(3) C26 0.040(2) 0.064(3) 0.0406(19) -0.0121(18) -0.0088(17) -0.014(2) C27 0.036(2) 0.074(3) 0.041(2) -0.010(2) -0.0124(17) -0.003(2) C28 0.065(3) 0.062(3) 0.051(2) -0.012(2) -0.017(2) -0.003(3) C29 0.082(4) 0.050(3) 0.054(2) -0.011(2) -0.019(2) -0.009(3) C30 0.096(4) 0.063(3) 0.042(2) -0.012(2) -0.007(2) -0.037(3) C31 0.067(3) 0.078(3) 0.043(2) -0.018(2) -0.004(2) -0.037(3) C32 0.083(4) 0.102(4) 0.065(3) -0.030(3) -0.005(3) -0.055(4) C33 0.077(4) 0.152(7) 0.074(3) -0.051(4) 0.000(3) -0.069(5) C34 0.060(3) 0.140(6) 0.064(3) -0.044(3) -0.001(2) -0.048(4) C35 0.053(3) 0.089(4) 0.048(2) -0.022(2) -0.008(2) -0.028(3) C36 0.048(3) 0.075(3) 0.0386(19) -0.0188(19) -0.0023(17) -0.031(2) C37 0.076(4) 0.059(3) 0.098(4) -0.013(3) -0.023(3) -0.029(3) C38 0.093(5) 0.063(4) 0.137(6) 0.000(4) -0.048(4) -0.019(3) C39 0.048(3) 0.126(6) 0.098(4) -0.035(4) -0.034(3) -0.001(3) C40 0.089(5) 0.104(6) 0.154(7) -0.014(5) -0.065(5) 0.013(4) C41 0.238(13) 0.140(8) 0.107(6) 0.001(6) -0.029(7) -0.064(9) C42 0.128(7) 0.082(5) 0.107(5) -0.004(4) -0.039(5) -0.036(5) Cl1 0.0837(10) 0.0648(8) 0.0776(8) -0.0166(6) -0.0343(7) -0.0172(7) Cs1 0.0474(2) 0.0593(2) 0.06317(19) -0.01635(14) -0.00604(13) -0.01556(14) N1 0.080(3) 0.076(3) 0.055(2) -0.024(2) 0.000(2) -0.039(3) N2 0.057(3) 0.098(3) 0.052(2) -0.031(2) 0.0011(19) -0.035(3) N3 0.052(2) 0.056(2) 0.0397(16) -0.0140(15) -0.0131(15) -0.0062(18) N4 0.062(2) 0.052(2) 0.0449(18) -0.0120(15) -0.0092(16) -0.0158(19) N5 0.255(11) 0.127(6) 0.115(6) -0.006(5) -0.048(6) -0.084(7) Ni2 0.0424(3) 0.0480(3) 0.0407(3) -0.0096(2) -0.0103(2) -0.0114(2) Ni1 0.0541(4) 0.0656(4) 0.0467(3) -0.0202(3) -0.0020(2) -0.0244(3) O1 0.059(2) 0.0561(19) 0.0540(16) -0.0154(14) -0.0098(14) -0.0134(16) O2 0.0473(19) 0.0621(19) 0.0624(18) -0.0188(15) -0.0063(14) -0.0117(16) O3 0.049(2) 0.092(3) 0.0608(18) -0.0219(17) -0.0158(15) -0.0143(18) O4 0.083(3) 0.056(2) 0.117(3) -0.031(2) -0.025(2) -0.007(2) O5 0.0371(16) 0.0521(16) 0.0548(15) -0.0108(13) -0.0139(12) -0.0152(13) O6 0.0447(17) 0.0585(18) 0.0497(15) -0.0111(13) -0.0123(12) -0.0190(15) O7 0.053(2) 0.0501(18) 0.086(2) -0.0035(16) -0.0208(17) -0.0210(16) O8 0.0458(19) 0.086(3) 0.072(2) -0.0163(18) -0.0224(16) -0.0128(18) O9 0.152(5) 0.102(3) 0.115(3) 0.000(3) -0.087(3) -0.034(3) O10 0.129(4) 0.094(3) 0.128(4) -0.028(3) -0.058(3) -0.044(3) O11 0.084(3) 0.158(5) 0.100(3) -0.016(3) -0.008(3) -0.016(3) O12 0.107(4) 0.084(3) 0.171(5) -0.059(3) -0.056(3) -0.005(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 C1 O1 1.307(5) . ? C1 C6 1.399(7) . ? C1 C2 1.432(7) . ? C2 O3 1.378(6) . ? C2 C3 1.383(8) . ? C3 C4 1.400(10) . ? C3 H3 0.9300 . ? C4 C5 1.360(10) . ? C4 H4 0.9300 . ? C5 C6 1.407(8) . ? C5 H5 0.9300 . ? C6 C7 1.433(8) . ? C7 N1 1.276(7) . ? C7 H7 0.9300 . ? C8 N1 1.472(7) . ? C8 C9 1.483(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.473(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.275(7) . ? C10 C11 1.416(9) . ? C10 H10 0.9300 . ? C11 C16 1.414(7) . ? C11 C12 1.427(9) . ? C12 C13 1.333(10) . ? C12 H12 0.9300 . ? C13 C14 1.388(10) . ? C13 H13 0.9300 . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 O4 1.373(7) . ? C15 C16 1.406(8) . ? C16 O2 1.313(6) . ? C17 O3 1.429(6) . ? C17 C18 1.492(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.404(7) . ? C19 C20 1.505(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.307(5) . ? C21 C26 1.410(6) . ? C21 C22 1.415(6) . ? C21 Cs1 3.844(4) . ? C22 O7 1.377(6) . ? C22 C23 1.384(7) . ? C23 C24 1.392(8) . ? C23 H23 0.9300 . ? C24 C25 1.354(8) . ? C24 H24 0.9300 . ? C25 C26 1.412(6) . ? C25 H25 0.9300 . ? C26 C27 1.417(6) . ? C27 N3 1.285(6) . ? C27 H27 0.9300 . ? C28 N3 1.467(6) . ? C28 C29 1.486(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.488(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.300(6) . ? C30 C31 1.431(8) . ? C30 H30 0.9300 . ? C31 C36 1.391(7) . ? C31 C32 1.418(7) . ? C32 C33 1.347(9) . ? C32 H32 0.9300 . ? C33 C34 1.407(9) . ? C33 H33 0.9300 . ? C34 C35 1.373(7) . ? C34 H34 0.9300 . ? C35 O8 1.371(6) . ? C35 C36 1.421(7) . ? C36 O6 1.315(5) . ? C37 O7 1.413(6) . ? C37 C38 1.496(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O8 1.435(6) . ? C39 C40 1.484(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.438(12) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N5 1.073(9) . ? Cl1 O11 1.401(5) . ? Cl1 O12 1.405(5) . ? Cl1 O10 1.408(4) . ? Cl1 O9 1.412(4) . ? Cs1 O6 2.963(3) . ? Cs1 O2 2.988(3) . ? Cs1 O1 3.021(3) . ? Cs1 O5 3.047(3) . ? Cs1 O3 3.119(3) . ? Cs1 O4 3.170(4) . ? Cs1 O7 3.180(3) . ? Cs1 O8 3.183(3) . ? Cs1 Ni1 3.9079(8) . ? Cs1 Ni2 3.9091(7) . ? N1 Ni1 1.839(5) . ? N2 Ni1 1.848(5) . ? N3 Ni2 1.846(4) . ? N4 Ni2 1.838(4) . ? Ni2 O6 1.846(3) . ? Ni2 O5 1.855(3) . ? Ni1 O2 1.849(3) . ? Ni1 O1 1.853(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 C1 C6 124.7(5) . . ? O1 C1 C2 118.2(5) . . ? C6 C1 C2 117.1(5) . . ? O3 C2 C3 124.3(6) . . ? O3 C2 C1 114.7(5) . . ? C3 C2 C1 121.0(6) . . ? C2 C3 C4 119.8(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.6(6) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.3(7) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 121.2(6) . . ? C1 C6 C7 120.4(5) . . ? C5 C6 C7 118.3(6) . . ? N1 C7 C6 126.3(5) . . ? N1 C7 H7 116.8 . . ? C6 C7 H7 116.8 . . ? N1 C8 C9 107.3(5) . . ? N1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 106.8(5) . . ? N2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? N2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 126.5(5) . . ? N2 C10 H10 116.8 . . ? C11 C10 H10 116.8 . . ? C16 C11 C10 120.7(5) . . ? C16 C11 C12 119.2(6) . . ? C10 C11 C12 120.1(6) . . ? C13 C12 C11 121.1(7) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 120.5(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 120.3(7) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? O4 C15 C14 124.2(6) . . ? O4 C15 C16 114.5(4) . . ? C14 C15 C16 121.3(6) . . ? O2 C16 C15 119.0(5) . . ? O2 C16 C11 123.5(5) . . ? C15 C16 C11 117.5(5) . . ? O3 C17 C18 107.6(5) . . ? O3 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O3 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 108.7(6) . . ? O4 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O4 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C26 124.7(4) . . ? O5 C21 C22 117.8(4) . . ? C26 C21 C22 117.4(4) . . ? O5 C21 Cs1 44.23(18) . . ? C26 C21 Cs1 146.8(3) . . ? C22 C21 Cs1 82.9(2) . . ? O7 C22 C23 124.4(4) . . ? O7 C22 C21 115.1(4) . . ? C23 C22 C21 120.5(5) . . ? C22 C23 C24 121.4(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 119.1(5) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 121.4(5) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C21 C26 C25 120.1(4) . . ? C21 C26 C27 120.1(4) . . ? C25 C26 C27 119.6(4) . . ? N3 C27 C26 126.2(4) . . ? N3 C27 H27 116.9 . . ? C26 C27 H27 116.9 . . ? N3 C28 C29 107.1(4) . . ? N3 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? N3 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? C28 C29 N4 106.9(4) . . ? C28 C29 H29A 110.3 . . ? N4 C29 H29A 110.3 . . ? C28 C29 H29B 110.3 . . ? N4 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? N4 C30 C31 125.4(5) . . ? N4 C30 H30 117.3 . . ? C31 C30 H30 117.3 . . ? C36 C31 C32 120.4(5) . . ? C36 C31 C30 121.2(4) . . ? C32 C31 C30 118.4(5) . . ? C33 C32 C31 120.0(6) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.9(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 119.8(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? O8 C35 C34 124.9(5) . . ? O8 C35 C36 114.5(4) . . ? C34 C35 C36 120.6(6) . . ? O6 C36 C31 124.1(4) . . ? O6 C36 C35 117.8(4) . . ? C31 C36 C35 118.2(4) . . ? O7 C37 C38 107.8(4) . . ? O7 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O7 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 108.2(5) . . ? O8 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? O8 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 C41 177.9(11) . . ? O11 Cl1 O12 108.8(3) . . ? O11 Cl1 O10 109.6(4) . . ? O12 Cl1 O10 109.5(3) . . ? O11 Cl1 O9 109.2(4) . . ? O12 Cl1 O9 110.3(3) . . ? O10 Cl1 O9 109.5(3) . . ? O6 Cs1 O2 99.23(8) . . ? O6 Cs1 O1 71.71(8) . . ? O2 Cs1 O1 49.64(9) . . ? O6 Cs1 O5 49.29(7) . . ? O2 Cs1 O5 146.32(8) . . ? O1 Cs1 O5 101.79(8) . . ? O6 Cs1 O3 80.00(8) . . ? O2 Cs1 O3 95.09(9) . . ? O1 Cs1 O3 50.67(9) . . ? O5 Cs1 O3 70.57(8) . . ? O6 Cs1 O4 145.20(10) . . ? O2 Cs1 O4 50.14(10) . . ? O1 Cs1 O4 92.72(9) . . ? O5 Cs1 O4 163.54(9) . . ? O3 Cs1 O4 114.46(10) . . ? O6 Cs1 O7 93.19(8) . . ? O2 Cs1 O7 163.00(9) . . ? O1 Cs1 O7 146.79(9) . . ? O5 Cs1 O7 49.55(8) . . ? O3 Cs1 O7 98.48(9) . . ? O4 Cs1 O7 114.18(10) . . ? O6 Cs1 O8 49.94(8) . . ? O2 Cs1 O8 71.21(9) . . ? O1 Cs1 O8 83.94(9) . . ? O5 Cs1 O8 90.56(8) . . ? O3 Cs1 O8 122.46(10) . . ? O4 Cs1 O8 98.74(10) . . ? O7 Cs1 O8 109.24(9) . . ? O6 Cs1 C21 66.60(8) . . ? O2 Cs1 C21 159.26(9) . . ? O1 Cs1 C21 109.94(9) . . ? O5 Cs1 C21 17.42(8) . . ? O3 Cs1 C21 68.32(8) . . ? O4 Cs1 C21 147.43(10) . . ? O7 Cs1 C21 37.73(9) . . ? O8 Cs1 C21 106.44(8) . . ? O6 Cs1 Ni1 75.68(5) . . ? O2 Cs1 Ni1 27.14(6) . . ? O1 Cs1 Ni1 27.39(6) . . ? O5 Cs1 Ni1 119.51(5) . . ? O3 Cs1 Ni1 77.94(7) . . ? O4 Cs1 Ni1 76.87(8) . . ? O7 Cs1 Ni1 168.70(6) . . ? O8 Cs1 Ni1 65.13(6) . . ? C21 Cs1 Ni1 132.55(7) . . ? O6 Cs1 Ni2 26.94(6) . . ? O2 Cs1 Ni2 118.79(6) . . ? O1 Cs1 Ni2 77.02(6) . . ? O5 Cs1 Ni2 27.53(5) . . ? O3 Cs1 Ni2 62.18(6) . . ? O4 Cs1 Ni2 168.89(8) . . ? O7 Cs1 Ni2 76.92(6) . . ? O8 Cs1 Ni2 76.19(6) . . ? C21 Cs1 Ni2 43.02(6) . . ? Ni1 Cs1 Ni2 92.023(17) . . ? C7 N1 C8 119.7(5) . . ? C7 N1 Ni1 126.5(4) . . ? C8 N1 Ni1 113.6(4) . . ? C10 N2 C9 118.4(5) . . ? C10 N2 Ni1 127.1(4) . . ? C9 N2 Ni1 114.4(4) . . ? C27 N3 C28 120.3(4) . . ? C27 N3 Ni2 126.9(3) . . ? C28 N3 Ni2 112.7(3) . . ? C30 N4 C29 119.6(4) . . ? C30 N4 Ni2 126.8(4) . . ? C29 N4 Ni2 113.5(3) . . ? N4 Ni2 N3 86.53(18) . . ? N4 Ni2 O6 94.39(16) . . ? N3 Ni2 O6 177.17(13) . . ? N4 Ni2 O5 177.14(13) . . ? N3 Ni2 O5 93.94(15) . . ? O6 Ni2 O5 85.28(12) . . ? N4 Ni2 Cs1 128.74(12) . . ? N3 Ni2 Cs1 134.21(11) . . ? O6 Ni2 Cs1 46.65(9) . . ? O5 Ni2 Cs1 49.39(9) . . ? N1 Ni1 N2 85.7(2) . . ? N1 Ni1 O2 176.39(15) . . ? N2 Ni1 O2 93.95(19) . . ? N1 Ni1 O1 94.67(19) . . ? N2 Ni1 O1 177.04(14) . . ? O2 Ni1 O1 85.91(14) . . ? N1 Ni1 Cs1 134.90(15) . . ? N2 Ni1 Cs1 129.66(14) . . ? O2 Ni1 Cs1 47.50(10) . . ? O1 Ni1 Cs1 48.58(9) . . ? C1 O1 Ni1 127.0(3) . . ? C1 O1 Cs1 118.8(3) . . ? Ni1 O1 Cs1 104.03(13) . . ? C16 O2 Ni1 128.1(3) . . ? C16 O2 Cs1 118.3(3) . . ? Ni1 O2 Cs1 105.36(13) . . ? C2 O3 C17 117.4(5) . . ? C2 O3 Cs1 114.9(3) . . ? C17 O3 Cs1 119.7(3) . . ? C15 O4 C19 116.8(5) . . ? C15 O4 Cs1 112.6(3) . . ? C19 O4 Cs1 124.9(4) . . ? C21 O5 Ni2 127.2(3) . . ? C21 O5 Cs1 118.4(2) . . ? Ni2 O5 Cs1 103.08(11) . . ? C36 O6 Ni2 127.7(3) . . ? C36 O6 Cs1 118.4(2) . . ? Ni2 O6 Cs1 106.41(11) . . ? C22 O7 C37 118.0(4) . . ? C22 O7 Cs1 113.0(2) . . ? C37 O7 Cs1 123.4(3) . . ? C35 O8 C39 118.6(4) . . ? C35 O8 Cs1 110.7(3) . . ? C39 O8 Cs1 121.4(3) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.448 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.100 #END=== data_6 _database_code_depnum_ccdc_archive 'CCDC 813961' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H66 Cl2 Mg N6 Ni3 O24' _chemical_formula_weight 1526.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.4418(13) _cell_length_b 22.4552(18) _cell_length_c 18.8479(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.555(2) _cell_angle_gamma 90.00 _cell_volume 6514.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2101 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 18.01 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8519 _exptl_absorpt_correction_T_max 0.8858 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; Theta(max) is low. Data collected with different single crystals did not yield better theta values. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19136 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.39 _reflns_number_total 4592 _reflns_number_gt 2683 _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^)+(0.1000P)^2^+0.5000P] 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 4592 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 C1 C 0.6951(4) 0.3613(3) 0.0759(3) 0.0540(15) Uani 1 1 d . . . C2 C 0.6305(4) 0.4047(3) 0.0714(3) 0.0663(18) Uani 1 1 d . . . C3 C 0.6508(5) 0.4638(3) 0.0728(4) 0.082(2) Uani 1 1 d . . . H3 H 0.6069 0.4921 0.0729 0.099 Uiso 1 1 calc R . . C4 C 0.7370(5) 0.4816(3) 0.0739(4) 0.083(2) Uani 1 1 d . . . H4 H 0.7508 0.5219 0.0729 0.100 Uiso 1 1 calc R . . C5 C 0.8001(5) 0.4407(4) 0.0764(3) 0.077(2) Uani 1 1 d . . . H5 H 0.8577 0.4531 0.0772 0.093 Uiso 1 1 calc R . . C6 C 0.7818(4) 0.3805(3) 0.0778(3) 0.0565(16) Uani 1 1 d . . . C7 C 0.8515(4) 0.3393(3) 0.0784(3) 0.0617(18) Uani 1 1 d . . . H7 H 0.9069 0.3547 0.0752 0.074 Uiso 1 1 calc R . . C8 C 0.9217(4) 0.2438(3) 0.0792(3) 0.0683(19) Uani 1 1 d . . . H8A H 0.9733 0.2648 0.0981 0.082 Uiso 1 1 calc R . . H8B H 0.9290 0.2327 0.0303 0.082 Uiso 1 1 calc R . . C9 C 0.9066(4) 0.1898(3) 0.1231(4) 0.076(2) Uani 1 1 d . . . H9A H 0.9435 0.1573 0.1100 0.092 Uiso 1 1 calc R . . H9B H 0.9193 0.1984 0.1733 0.092 Uiso 1 1 calc R . . C10 C 0.7899(4) 0.1194(3) 0.1138(3) 0.0664(18) Uani 1 1 d . . . H10 H 0.8329 0.0914 0.1261 0.080 Uiso 1 1 calc R . . C11 C 0.7028(4) 0.0978(3) 0.1026(3) 0.0602(16) Uani 1 1 d . . . C12 C 0.6870(5) 0.0358(3) 0.1031(3) 0.077(2) Uani 1 1 d . . . H12 H 0.7324 0.0092 0.1134 0.092 Uiso 1 1 calc R . . C13 C 0.6041(6) 0.0153(3) 0.0884(4) 0.083(2) Uani 1 1 d . . . H13 H 0.5940 -0.0255 0.0891 0.100 Uiso 1 1 calc R . . C14 C 0.5352(5) 0.0531(3) 0.0726(3) 0.075(2) Uani 1 1 d . . . H14 H 0.4799 0.0379 0.0612 0.091 Uiso 1 1 calc R . . C15 C 0.5488(4) 0.1140(3) 0.0737(3) 0.0625(17) Uani 1 1 d . . . C16 C 0.6333(4) 0.1376(3) 0.0898(3) 0.0552(16) Uani 1 1 d . . . C17 C 0.4795(5) 0.4159(4) 0.0360(5) 0.119(3) Uani 1 1 d . . . H17A H 0.4993 0.4356 -0.0056 0.143 Uiso 1 1 calc R . . H17B H 0.4621 0.4464 0.0684 0.143 Uiso 1 1 calc R . . C18 C 0.4043(5) 0.3779(4) 0.0143(5) 0.118(3) Uani 1 1 d . . . H18A H 0.3536 0.4023 0.0048 0.176 Uiso 1 1 calc R . . H18B H 0.3946 0.3504 0.0519 0.176 Uiso 1 1 calc R . . H18C H 0.4155 0.3562 -0.0278 0.176 Uiso 1 1 calc R . . C19 C 0.3997(4) 0.1386(3) 0.0378(4) 0.089(2) Uani 1 1 d . . . H19A H 0.3762 0.1156 0.0754 0.107 Uiso 1 1 calc R . . H19B H 0.3984 0.1141 -0.0046 0.107 Uiso 1 1 calc R . . C20 C 0.3469(4) 0.1938(3) 0.0234(4) 0.106(3) Uani 1 1 d . . . H20A H 0.3530 0.2194 0.0642 0.158 Uiso 1 1 calc R . . H20B H 0.2869 0.1832 0.0138 0.158 Uiso 1 1 calc R . . H20C H 0.3668 0.2141 -0.0170 0.158 Uiso 1 1 calc R . . C21 C 0.6646(3) 0.1842(3) 0.2764(3) 0.0503(15) Uani 1 1 d . . . C22 C 0.7121(4) 0.2382(3) 0.2809(3) 0.0547(15) Uani 1 1 d . . . C23 C 0.8000(4) 0.2371(3) 0.2949(4) 0.075(2) Uani 1 1 d . . . H23 H 0.8307 0.2727 0.2992 0.090 Uiso 1 1 calc R . . C24 C 0.8439(4) 0.1837(4) 0.3029(3) 0.081(2) Uani 1 1 d . . . H24 H 0.9040 0.1835 0.3120 0.097 Uiso 1 1 calc R . . C25 C 0.7996(4) 0.1311(3) 0.2975(3) 0.076(2) Uani 1 1 d . . . H25 H 0.8298 0.0953 0.3028 0.091 Uiso 1 1 calc R . . C26 C 0.7080(4) 0.1304(3) 0.2840(3) 0.0577(16) Uani 1 1 d . . . C27 C 0.6630(4) 0.0740(3) 0.2776(3) 0.0643(18) Uani 1 1 d . . . H27 H 0.6965 0.0396 0.2825 0.077 Uiso 1 1 calc R . . C28 C 0.5450(4) 0.0071(3) 0.2680(3) 0.0706(18) Uani 1 1 d . . . H28A H 0.5437 -0.0058 0.3170 0.085 Uiso 1 1 calc R . . H28B H 0.5815 -0.0202 0.2438 0.085 Uiso 1 1 calc R . . C29 C 0.7056(4) 0.3434(3) 0.2573(4) 0.088(2) Uani 1 1 d . . . H29A H 0.7566 0.3348 0.2322 0.105 Uiso 1 1 calc R . . H29B H 0.6672 0.3680 0.2265 0.105 Uiso 1 1 calc R . . C30 C 0.7320(6) 0.3766(4) 0.3205(5) 0.147(4) Uani 1 1 d . . . H30A H 0.6823 0.3844 0.3465 0.221 Uiso 1 1 calc R . . H30B H 0.7574 0.4137 0.3074 0.221 Uiso 1 1 calc R . . H30C H 0.7739 0.3540 0.3496 0.221 Uiso 1 1 calc R . . Cl2 Cl 1.0000 0.02028(16) 0.2500 0.1417(16) Uani 1 2 d S . . Mg1 Mg 0.5000 0.26952(11) 0.2500 0.0474(7) Uani 1 2 d S . . N1 N 0.8440(3) 0.2816(3) 0.0830(2) 0.0572(13) Uani 1 1 d . . . N2 N 0.8143(3) 0.1740(2) 0.1083(2) 0.0560(13) Uani 1 1 d . . . N3 N 0.5805(3) 0.0676(2) 0.2658(2) 0.0560(13) Uani 1 1 d . . . Ni1 Ni 0.74320(4) 0.23872(3) 0.08992(4) 0.0520(3) Uani 1 1 d . . . Ni2 Ni 0.5000 0.12675(4) 0.2500 0.0507(3) Uani 1 2 d S . . O1 O 0.6717(2) 0.30487(17) 0.0777(2) 0.0577(10) Uani 1 1 d . . . O2 O 0.6416(2) 0.19588(17) 0.09027(19) 0.0560(11) Uani 1 1 d . . . O3 O 0.5463(3) 0.3833(2) 0.0687(3) 0.0981(17) Uani 1 1 d . . . O4 O 0.4863(3) 0.15597(19) 0.0588(2) 0.0704(12) Uani 1 1 d . . . O5 O 0.5780(2) 0.18826(16) 0.26381(19) 0.0536(10) Uani 1 1 d . . . O6 O 0.6619(3) 0.28798(19) 0.2703(2) 0.0686(12) Uani 1 1 d . . . O7 O 0.4838(2) 0.27116(18) 0.3602(2) 0.0726(12) Uani 1 1 d . . . O8 O 0.5000 0.3634(4) 0.2500 0.194(5) Uani 1 2 d S . . O13 O 0.9987(6) 0.0566(4) 0.1901(5) 0.251(5) Uani 1 1 d . . . O12 O 0.9261(6) -0.0107(4) 0.2489(6) 0.293(6) Uani 1 1 d . . . Cl1 Cl 1.0000 0.34684(12) 0.2500 0.0917(9) Uani 1 2 d S . . O9 O 1.0000 0.2839(3) 0.2500 0.114(3) Uani 1 2 d S . . O10 O 0.9211(5) 0.3664(3) 0.2252(5) 0.167(3) Uani 1 1 d . . . O11 O 1.0260(8) 0.3690(5) 0.1782(5) 0.260(5) 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 C1 0.060(4) 0.052(4) 0.048(4) 0.004(3) -0.005(3) -0.011(3) C2 0.060(4) 0.061(5) 0.077(5) 0.007(4) 0.001(3) -0.008(4) C3 0.085(5) 0.055(5) 0.105(6) 0.006(4) -0.003(4) -0.004(4) C4 0.098(6) 0.058(5) 0.092(6) 0.004(4) -0.005(5) -0.022(5) C5 0.080(5) 0.086(6) 0.064(5) 0.001(4) -0.008(4) -0.040(5) C6 0.058(4) 0.064(4) 0.046(4) 0.007(3) -0.007(3) -0.014(4) C7 0.057(4) 0.078(5) 0.050(4) 0.005(4) 0.004(3) -0.026(4) C8 0.051(4) 0.089(5) 0.066(4) -0.003(4) 0.013(3) -0.006(4) C9 0.043(4) 0.107(6) 0.079(5) 0.002(4) -0.001(3) 0.010(4) C10 0.066(4) 0.075(5) 0.057(4) 0.008(4) 0.000(3) 0.019(4) C11 0.077(5) 0.053(4) 0.051(4) 0.002(3) 0.006(3) 0.003(4) C12 0.099(6) 0.064(5) 0.069(5) -0.005(4) 0.012(4) 0.011(4) C13 0.127(7) 0.049(5) 0.076(5) -0.005(4) 0.018(5) -0.015(5) C14 0.094(5) 0.063(5) 0.070(5) -0.010(4) 0.006(4) -0.021(4) C15 0.071(5) 0.069(5) 0.049(4) -0.006(3) 0.010(3) -0.015(4) C16 0.066(4) 0.051(4) 0.050(4) -0.001(3) 0.008(3) -0.012(3) C17 0.089(6) 0.093(6) 0.166(9) 0.038(6) -0.041(6) -0.004(5) C18 0.087(6) 0.112(7) 0.149(8) 0.018(6) -0.020(5) -0.006(5) C19 0.069(5) 0.109(6) 0.087(5) -0.012(5) -0.003(4) -0.028(5) C20 0.065(5) 0.125(7) 0.121(7) -0.002(6) -0.021(5) -0.007(5) C21 0.043(4) 0.068(5) 0.040(3) -0.001(3) 0.005(3) 0.009(3) C22 0.042(3) 0.071(5) 0.050(4) -0.001(3) 0.000(3) -0.005(3) C23 0.049(4) 0.091(5) 0.084(5) 0.005(4) 0.003(4) -0.005(4) C24 0.040(4) 0.119(7) 0.081(5) 0.007(5) -0.009(3) -0.006(4) C25 0.058(4) 0.096(6) 0.074(5) 0.017(4) 0.005(4) 0.024(4) C26 0.047(4) 0.072(5) 0.055(4) 0.001(3) 0.003(3) 0.007(4) C27 0.068(5) 0.072(5) 0.052(4) 0.006(3) -0.001(3) 0.021(4) C28 0.087(5) 0.052(4) 0.073(5) -0.001(3) 0.009(4) 0.006(3) C29 0.079(5) 0.090(6) 0.095(6) -0.006(5) 0.007(4) -0.025(4) C30 0.130(8) 0.136(8) 0.180(10) -0.068(8) 0.033(7) -0.025(7) Cl2 0.113(3) 0.063(2) 0.256(5) 0.000 0.059(3) 0.000 Mg1 0.0419(15) 0.0415(16) 0.0592(17) 0.000 0.0066(12) 0.000 N1 0.042(3) 0.082(4) 0.048(3) 0.000(3) 0.006(2) -0.009(3) N2 0.053(3) 0.064(4) 0.051(3) 0.006(3) 0.002(2) 0.004(3) N3 0.065(3) 0.047(3) 0.056(3) 0.001(2) 0.006(3) 0.003(3) Ni1 0.0454(5) 0.0588(6) 0.0515(5) 0.0006(4) 0.0017(3) -0.0041(4) Ni2 0.0498(6) 0.0481(7) 0.0542(7) 0.000 0.0049(5) 0.000 O1 0.049(2) 0.051(3) 0.072(3) 0.004(2) 0.0033(19) -0.002(2) O2 0.048(2) 0.054(3) 0.065(3) 0.005(2) 0.0022(19) -0.004(2) O3 0.061(3) 0.065(3) 0.167(5) 0.044(3) 0.000(3) 0.007(3) O4 0.053(3) 0.073(3) 0.083(3) -0.005(2) -0.003(2) -0.018(2) O5 0.043(2) 0.056(2) 0.062(3) -0.0002(19) 0.0020(18) 0.0039(18) O6 0.055(3) 0.057(3) 0.094(3) 0.005(2) 0.007(2) -0.008(2) O7 0.063(3) 0.067(3) 0.089(3) -0.008(2) 0.017(2) 0.001(2) O8 0.062(5) 0.085(6) 0.431(17) 0.000 0.007(7) 0.000 O13 0.157(7) 0.197(9) 0.396(14) 0.136(9) 0.018(9) -0.007(7) O12 0.260(11) 0.230(9) 0.409(15) -0.123(10) 0.153(11) -0.174(9) Cl1 0.0674(17) 0.0586(17) 0.142(3) 0.000 -0.0344(18) 0.000 O9 0.096(5) 0.043(4) 0.199(8) 0.000 -0.004(5) 0.000 O10 0.150(7) 0.134(6) 0.208(8) -0.011(5) -0.051(6) 0.032(5) O11 0.322(14) 0.256(11) 0.200(10) 0.043(8) 0.017(10) -0.097(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.318(6) . ? C1 C2 1.392(8) . ? C1 C6 1.405(8) . ? C2 C3 1.362(9) . ? C2 O3 1.384(7) . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.338(9) . ? C4 H4 0.9300 . ? C5 C6 1.381(8) . ? C5 H5 0.9300 . ? C6 C7 1.418(8) . ? C7 N1 1.303(7) . ? C7 H7 0.9300 . ? C8 N1 1.476(7) . ? C8 C9 1.497(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.473(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.290(7) . ? C10 C11 1.429(8) . ? C10 H10 0.9300 . ? C11 C16 1.402(8) . ? C11 C12 1.415(8) . ? C12 C13 1.367(9) . ? C12 H12 0.9300 . ? C13 C14 1.375(9) . ? C13 H13 0.9300 . ? C14 C15 1.382(8) . ? C14 H14 0.9300 . ? C15 O4 1.363(7) . ? C15 C16 1.418(8) . ? C16 O2 1.316(6) . ? C17 O3 1.370(7) . ? C17 C18 1.474(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.418(7) . ? C19 C20 1.497(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.342(6) . ? C21 C26 1.385(8) . ? C21 C22 1.417(7) . ? C22 C23 1.361(8) . ? C22 O6 1.366(7) . ? C23 C24 1.381(8) . ? C23 H23 0.9300 . ? C24 C25 1.365(9) . ? C24 H24 0.9300 . ? C25 C26 1.417(8) . ? C25 H25 0.9300 . ? C26 C27 1.444(8) . ? C27 N3 1.285(7) . ? C27 H27 0.9300 . ? C28 N3 1.465(7) . ? C28 C28 1.498(11) 2_655 ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.436(9) . ? C29 O6 1.446(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl2 O12 1.335(7) . ? Cl2 O12 1.335(7) 2_755 ? Cl2 O13 1.393(8) 2_755 ? Cl2 O13 1.393(8) . ? Mg1 O8 2.108(9) . ? Mg1 O7 2.112(4) 2_655 ? Mg1 O7 2.112(4) . ? Mg1 O5 2.191(4) . ? Mg1 O5 2.191(4) 2_655 ? Mg1 O6 2.532(4) . ? Mg1 O6 2.532(4) 2_655 ? N1 Ni1 1.844(5) . ? N2 Ni1 1.837(5) . ? N3 Ni2 1.828(5) . ? Ni1 O2 1.840(3) . ? Ni1 O1 1.855(4) . ? Ni2 N3 1.828(5) 2_655 ? Ni2 O5 1.838(4) 2_655 ? Ni2 O5 1.838(4) . ? Cl1 O10 1.345(7) 2_755 ? Cl1 O10 1.345(7) . ? Cl1 O9 1.413(6) . ? Cl1 O11 1.525(9) 2_755 ? Cl1 O11 1.525(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 O1 C1 C2 118.6(5) . . ? O1 C1 C6 123.9(6) . . ? C2 C1 C6 117.5(6) . . ? C3 C2 O3 123.6(6) . . ? C3 C2 C1 121.3(6) . . ? O3 C2 C1 115.1(6) . . ? C2 C3 C4 120.0(7) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.5(6) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.8(6) . . ? C5 C6 C7 118.9(6) . . ? C1 C6 C7 121.3(6) . . ? N1 C7 C6 125.3(5) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? N1 C8 C9 106.1(5) . . ? N1 C8 H8A 110.5 . . ? C9 C8 H8A 110.5 . . ? N1 C8 H8B 110.5 . . ? C9 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? N2 C9 C8 106.3(5) . . ? N2 C9 H9A 110.5 . . ? C8 C9 H9A 110.5 . . ? N2 C9 H9B 110.5 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N2 C10 C11 126.0(6) . . ? N2 C10 H10 117.0 . . ? C11 C10 H10 117.0 . . ? C16 C11 C12 119.8(6) . . ? C16 C11 C10 120.6(6) . . ? C12 C11 C10 119.5(6) . . ? C13 C12 C11 119.3(7) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 122.1(7) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C15 119.6(7) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? O4 C15 C14 125.2(6) . . ? O4 C15 C16 114.2(6) . . ? C14 C15 C16 120.5(7) . . ? O2 C16 C11 123.9(5) . . ? O2 C16 C15 117.5(6) . . ? C11 C16 C15 118.6(6) . . ? O3 C17 C18 111.3(7) . . ? O3 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O3 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 108.1(6) . . ? O4 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O4 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C26 123.0(5) . . ? O5 C21 C22 117.2(5) . . ? C26 C21 C22 119.8(5) . . ? C23 C22 O6 126.1(6) . . ? C23 C22 C21 120.0(6) . . ? O6 C22 C21 113.9(5) . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.3(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.7(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 118.5(6) . . ? C21 C26 C27 122.1(5) . . ? C25 C26 C27 119.4(6) . . ? N3 C27 C26 125.2(6) . . ? N3 C27 H27 117.4 . . ? C26 C27 H27 117.4 . . ? N3 C28 C28 108.8(3) . 2_655 ? N3 C28 H28A 109.9 . . ? C28 C28 H28A 109.9 2_655 . ? N3 C28 H28B 109.9 . . ? C28 C28 H28B 109.9 2_655 . ? H28A C28 H28B 108.3 . . ? C30 C29 O6 114.3(7) . . ? C30 C29 H29A 108.7 . . ? O6 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? O6 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O12 Cl2 O12 117.1(10) . 2_755 ? O12 Cl2 O13 106.0(6) . 2_755 ? O12 Cl2 O13 109.6(7) 2_755 2_755 ? O12 Cl2 O13 109.6(7) . . ? O12 Cl2 O13 106.0(6) 2_755 . ? O13 Cl2 O13 108.2(9) 2_755 . ? O8 Mg1 O7 89.00(13) . 2_655 ? O8 Mg1 O7 89.00(13) . . ? O7 Mg1 O7 178.0(3) 2_655 . ? O8 Mg1 O5 146.40(10) . . ? O7 Mg1 O5 91.39(15) 2_655 . ? O7 Mg1 O5 90.27(15) . . ? O8 Mg1 O5 146.40(10) . 2_655 ? O7 Mg1 O5 90.27(15) 2_655 2_655 ? O7 Mg1 O5 91.39(15) . 2_655 ? O5 Mg1 O5 67.2(2) . 2_655 ? O8 Mg1 O6 80.58(11) . . ? O7 Mg1 O6 87.32(14) 2_655 . ? O7 Mg1 O6 92.35(14) . . ? O5 Mg1 O6 65.89(13) . . ? O5 Mg1 O6 132.93(16) 2_655 . ? O8 Mg1 O6 80.58(11) . 2_655 ? O7 Mg1 O6 92.35(14) 2_655 2_655 ? O7 Mg1 O6 87.32(14) . 2_655 ? O5 Mg1 O6 132.93(16) . 2_655 ? O5 Mg1 O6 65.89(13) 2_655 2_655 ? O6 Mg1 O6 161.2(2) . 2_655 ? C7 N1 C8 119.5(5) . . ? C7 N1 Ni1 127.1(4) . . ? C8 N1 Ni1 113.4(4) . . ? C10 N2 C9 119.9(5) . . ? C10 N2 Ni1 126.4(4) . . ? C9 N2 Ni1 113.6(4) . . ? C27 N3 C28 117.8(5) . . ? C27 N3 Ni2 126.8(4) . . ? C28 N3 Ni2 115.3(4) . . ? N2 Ni1 O2 94.74(19) . . ? N2 Ni1 N1 86.1(2) . . ? O2 Ni1 N1 176.14(18) . . ? N2 Ni1 O1 176.29(18) . . ? O2 Ni1 O1 85.40(16) . . ? N1 Ni1 O1 94.0(2) . . ? N3 Ni2 N3 86.7(3) . 2_655 ? N3 Ni2 O5 177.74(19) . 2_655 ? N3 Ni2 O5 95.38(18) 2_655 2_655 ? N3 Ni2 O5 95.38(18) . . ? N3 Ni2 O5 177.74(19) 2_655 . ? O5 Ni2 O5 82.6(2) 2_655 . ? C1 O1 Ni1 127.6(4) . . ? C16 O2 Ni1 127.1(4) . . ? C17 O3 C2 120.2(5) . . ? C15 O4 C19 120.2(5) . . ? C21 O5 Ni2 127.4(4) . . ? C21 O5 Mg1 127.4(4) . . ? Ni2 O5 Mg1 105.13(16) . . ? C22 O6 C29 117.4(5) . . ? C22 O6 Mg1 115.5(3) . . ? C29 O6 Mg1 125.7(4) . . ? O10 Cl1 O10 141.8(6) 2_755 . ? O10 Cl1 O9 109.1(3) 2_755 . ? O10 Cl1 O9 109.1(3) . . ? O10 Cl1 O11 83.1(5) 2_755 2_755 ? O10 Cl1 O11 84.7(4) . 2_755 ? O9 Cl1 O11 109.0(4) . 2_755 ? O10 Cl1 O11 84.7(4) 2_755 . ? O10 Cl1 O11 83.1(5) . . ? O9 Cl1 O11 109.0(4) . . ? O11 Cl1 O11 142.0(9) 2_755 . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.327 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.066 #END=== data_7 _database_code_depnum_ccdc_archive 'CCDC 813962' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 Ca2 N8 Ni2 O23' _chemical_formula_weight 1202.41 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' Ca Ca 0.2262 0.3064 '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 16.101(5) _cell_length_b 13.981(5) _cell_length_c 13.162(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.378(4) _cell_angle_gamma 90.00 _cell_volume 2719.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7848 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.41 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7108 _exptl_absorpt_correction_T_max 0.8159 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26444 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5305 _reflns_number_gt 3642 _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.SQUEEZE was performed to get rid of solvent molecule acetone as the SQEEZE details gave a void volume of 307.6 A^3^ and electron per unit cell = 62. ADPs could not be restrained for C8 and O6 ; _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^)+(0.0977P)^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 5305 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1705 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 C1 C 0.2820(2) 0.2342(3) 0.5580(3) 0.0664(8) Uani 1 1 d . . . C2 C 0.2194(2) 0.2286(3) 0.6077(3) 0.0718(9) Uani 1 1 d . . . C3 C 0.2040(3) 0.1432(3) 0.6482(3) 0.0891(12) Uani 1 1 d . . . H3 H 0.1647 0.1408 0.6842 0.107 Uiso 1 1 calc R . . C4 C 0.2468(3) 0.0598(3) 0.6361(4) 0.0995(13) Uani 1 1 d . . . H4 H 0.2349 0.0016 0.6618 0.119 Uiso 1 1 calc R . . C5 C 0.3055(3) 0.0647(3) 0.5868(3) 0.0917(12) Uani 1 1 d . . . H5 H 0.3342 0.0089 0.5796 0.110 Uiso 1 1 calc R . . C6 C 0.3252(3) 0.1502(3) 0.5461(3) 0.0734(9) Uani 1 1 d . . . C7 C 0.3875(3) 0.1514(3) 0.4947(3) 0.0834(11) Uani 1 1 d . . . H7 H 0.4149 0.0937 0.4911 0.100 Uiso 1 1 calc R . . C8 C 0.4750(5) 0.2139(4) 0.4026(8) 0.177(4) Uani 1 1 d . . . H8A H 0.5314 0.1902 0.4579 0.213 Uiso 1 1 calc R . . H8B H 0.4526 0.1668 0.3438 0.213 Uiso 1 1 calc R . . C9 C 0.4909(4) 0.2975(5) 0.3604(5) 0.129(2) Uani 1 1 d . . . H9A H 0.4727 0.2904 0.2811 0.154 Uiso 1 1 calc R . . H9B H 0.5554 0.3106 0.3927 0.154 Uiso 1 1 calc R . . C10 C 0.4555(3) 0.4627(4) 0.3504(3) 0.0941(14) Uani 1 1 d . . . H10 H 0.5000 0.4693 0.3226 0.113 Uiso 1 1 calc R . . C11 C 0.4071(3) 0.5460(3) 0.3552(3) 0.0861(12) Uani 1 1 d . . . C12 C 0.4231(5) 0.6310(4) 0.3109(5) 0.128(2) Uani 1 1 d . . . H12 H 0.4690 0.6339 0.2851 0.153 Uiso 1 1 calc R . . C13 C 0.3726(6) 0.7084(4) 0.3053(6) 0.151(3) Uani 1 1 d . . . H13 H 0.3836 0.7640 0.2740 0.181 Uiso 1 1 calc R . . C14 C 0.3045(5) 0.7083(3) 0.3446(5) 0.1232(19) Uani 1 1 d . . . H14 H 0.2691 0.7625 0.3378 0.148 Uiso 1 1 calc R . . C15 C 0.2898(3) 0.6264(3) 0.3942(3) 0.0849(11) Uani 1 1 d . . . C16 C 0.3404(3) 0.5444(3) 0.4001(3) 0.0724(9) Uani 1 1 d . . . C17 C 0.1055(3) 0.3144(3) 0.6530(4) 0.0927(12) Uani 1 1 d . . . H17A H 0.0632 0.3662 0.6206 0.111 Uiso 1 1 calc R . . H17B H 0.0724 0.2544 0.6360 0.111 Uiso 1 1 calc R . . C18 C 0.1506(5) 0.3269(5) 0.7725(5) 0.139(2) Uani 1 1 d . . . H18A H 0.1882 0.2724 0.8044 0.209 Uiso 1 1 calc R . . H18B H 0.1060 0.3331 0.8035 0.209 Uiso 1 1 calc R . . H18C H 0.1872 0.3836 0.7884 0.209 Uiso 1 1 calc R . . C19 C 0.1629(4) 0.6944(4) 0.4250(6) 0.1225(18) Uani 1 1 d . . . H19A H 0.1086 0.6700 0.4311 0.147 Uiso 1 1 calc R . . H19B H 0.1456 0.7235 0.3526 0.147 Uiso 1 1 calc R . . C20 C 0.2074(7) 0.7694(7) 0.5152(9) 0.231(5) Uani 1 1 d . . . H20A H 0.1657 0.8209 0.5067 0.346 Uiso 1 1 calc R . . H20B H 0.2608 0.7937 0.5087 0.346 Uiso 1 1 calc R . . H20C H 0.2234 0.7406 0.5867 0.346 Uiso 1 1 calc R . . Ca1 Ca 0.21616(5) 0.46095(5) 0.52820(6) 0.0710(2) Uani 1 1 d . . . N1 N 0.4096(2) 0.2252(3) 0.4525(3) 0.0849(9) Uani 1 1 d . . . N2 N 0.4429(2) 0.3791(3) 0.3812(3) 0.0818(8) Uani 1 1 d . . . N3 N 0.0483(3) 0.4155(3) 0.3365(3) 0.1012(11) Uani 1 1 d . . . N4 N 0.3647(2) 0.5208(3) 0.7702(4) 0.0911(10) Uani 1 1 d . . . Ni1 Ni 0.36872(3) 0.34735(3) 0.45079(4) 0.0687(2) Uani 1 1 d . . . O1 O 0.29505(17) 0.31950(17) 0.5228(2) 0.0743(6) Uani 1 1 d . . . O2 O 0.32364(16) 0.46916(17) 0.4470(2) 0.0729(6) Uani 1 1 d . . . O3 O 0.17626(19) 0.31409(19) 0.6078(2) 0.0849(7) Uani 1 1 d . . . O4 O 0.22508(19) 0.61660(19) 0.4366(2) 0.0886(8) Uani 1 1 d . . . O5 O 0.04335(19) 0.4522(2) 0.4191(2) 0.0983(9) Uani 1 1 d . . . O6 O 0.1240(2) 0.4079(4) 0.3354(3) 0.1378(15) Uani 1 1 d . . . O7 O -0.0192(3) 0.3873(4) 0.2584(4) 0.179(2) Uani 1 1 d . . . O9A O 0.3428(5) 0.4938(7) 0.6839(8) 0.092(2) Uani 0.50 1 d P . . O8A O 0.3037(3) 0.5491(4) 0.8125(4) 0.0860(15) Uani 0.50 1 d P . . O10 O 0.4378(2) 0.5306(3) 0.8423(3) 0.1148(11) Uani 1 1 d . . . O12 O 0.2128(8) 0.5754(7) 0.8581(7) 0.164(3) Uani 0.50 1 d P . . O11 O 0.14576(19) 0.5505(2) 0.6233(2) 0.0932(8) Uani 1 1 d . . . O9B O 0.3472(5) 0.5582(7) 0.6756(7) 0.100(2) Uani 0.50 1 d P . . O8B O 0.3252(6) 0.4379(6) 0.7429(7) 0.145(3) Uani 0.50 1 d P . . 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 C1 0.062(2) 0.080(2) 0.0603(18) 0.0027(16) 0.0280(15) 0.0027(17) C2 0.073(2) 0.081(2) 0.072(2) 0.0061(17) 0.0403(18) 0.0033(18) C3 0.097(3) 0.098(3) 0.086(3) 0.021(2) 0.052(2) 0.002(2) C4 0.118(4) 0.087(3) 0.101(3) 0.027(2) 0.052(3) 0.012(3) C5 0.108(3) 0.083(3) 0.079(2) 0.016(2) 0.032(2) 0.025(2) C6 0.069(2) 0.085(2) 0.065(2) 0.0070(17) 0.0254(17) 0.0185(18) C7 0.075(2) 0.091(3) 0.086(2) -0.012(2) 0.034(2) 0.024(2) C8 0.208(7) 0.113(4) 0.329(10) -0.041(5) 0.231(8) -0.008(4) C9 0.119(4) 0.170(6) 0.144(4) 0.024(4) 0.103(4) 0.058(4) C10 0.074(3) 0.145(4) 0.089(3) -0.023(3) 0.060(2) -0.022(3) C11 0.089(3) 0.104(3) 0.091(3) -0.020(2) 0.063(2) -0.035(2) C12 0.172(5) 0.119(4) 0.155(5) -0.027(3) 0.131(5) -0.052(4) C13 0.239(8) 0.094(4) 0.201(6) -0.004(4) 0.173(6) -0.030(4) C14 0.197(6) 0.077(3) 0.148(4) 0.002(3) 0.124(4) -0.017(3) C15 0.105(3) 0.082(2) 0.094(3) -0.014(2) 0.069(2) -0.022(2) C16 0.077(2) 0.084(2) 0.074(2) -0.0160(18) 0.0496(19) -0.0212(19) C17 0.096(3) 0.103(3) 0.106(3) 0.002(2) 0.069(3) -0.001(2) C18 0.182(6) 0.145(5) 0.119(4) -0.003(3) 0.089(4) -0.010(4) C19 0.136(4) 0.090(3) 0.184(5) 0.015(3) 0.109(4) 0.022(3) C20 0.292(13) 0.171(8) 0.302(13) -0.026(8) 0.194(11) 0.025(8) Ca1 0.0692(5) 0.0729(5) 0.0965(5) -0.0033(4) 0.0600(4) 0.0016(3) N1 0.0720(19) 0.096(2) 0.108(2) -0.0189(19) 0.0581(18) 0.0068(17) N2 0.0653(18) 0.115(2) 0.090(2) -0.0109(19) 0.0569(16) 0.0013(18) N3 0.088(3) 0.126(3) 0.103(3) -0.024(2) 0.053(2) 0.015(2) N4 0.069(2) 0.079(2) 0.123(3) 0.020(2) 0.037(2) -0.0194(18) Ni1 0.0594(3) 0.0880(4) 0.0775(3) -0.0138(2) 0.0472(2) -0.0017(2) O1 0.0775(15) 0.0739(14) 0.1002(17) -0.0042(13) 0.0655(14) 0.0018(12) O2 0.0749(15) 0.0800(15) 0.0907(15) -0.0008(12) 0.0613(13) -0.0008(12) O3 0.0927(18) 0.0868(16) 0.109(2) 0.0076(14) 0.0761(16) 0.0061(14) O4 0.103(2) 0.0788(15) 0.112(2) 0.0082(14) 0.0732(17) 0.0059(15) O5 0.0858(18) 0.140(3) 0.0865(17) -0.0168(16) 0.0525(15) 0.0200(16) O6 0.094(2) 0.214(4) 0.130(3) -0.048(3) 0.070(2) 0.015(2) O7 0.115(3) 0.262(6) 0.139(3) -0.096(4) 0.027(3) 0.000(3) O9A 0.080(4) 0.122(6) 0.089(5) -0.030(5) 0.050(4) -0.013(5) O8A 0.077(3) 0.108(4) 0.099(4) -0.028(3) 0.063(3) -0.009(3) O10 0.093(2) 0.134(3) 0.103(2) 0.0032(19) 0.0240(19) -0.025(2) O12 0.212(9) 0.153(7) 0.135(6) -0.012(5) 0.076(6) 0.004(6) O11 0.0878(18) 0.112(2) 0.1016(19) -0.0170(15) 0.0605(16) 0.0064(15) O9B 0.080(4) 0.134(6) 0.093(5) 0.004(5) 0.042(3) -0.016(5) O8B 0.148(7) 0.115(5) 0.143(6) 0.035(5) 0.026(5) -0.042(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 C1 O1 1.326(4) . ? C1 C6 1.406(5) . ? C1 C2 1.405(5) . ? C2 C3 1.369(5) . ? C2 O3 1.383(4) . ? C3 C4 1.396(6) . ? C3 H3 0.9300 . ? C4 C5 1.344(6) . ? C4 H4 0.9300 . ? C5 C6 1.397(6) . ? C5 H5 0.9300 . ? C6 C7 1.414(6) . ? C7 N1 1.288(5) . ? C7 H7 0.9300 . ? C8 C9 1.362(8) . ? C8 N1 1.453(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.463(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.279(6) . ? C10 C11 1.417(6) . ? C10 H10 0.9300 . ? C11 C12 1.391(7) . ? C11 C16 1.415(5) . ? C12 C13 1.337(8) . ? C12 H12 0.9300 . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C15 O4 1.371(4) . ? C15 C16 1.390(6) . ? C16 O2 1.302(4) . ? C17 C18 1.459(7) . ? C17 O3 1.479(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.445(5) . ? C19 C20 1.532(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? Ca1 O9A 2.292(9) . ? Ca1 O11 2.355(3) . ? Ca1 O1 2.367(3) . ? Ca1 O2 2.370(2) . ? Ca1 O6 2.490(4) . ? Ca1 O3 2.502(3) . ? Ca1 O4 2.519(3) . ? Ca1 O5 2.578(3) . ? Ca1 O9B 2.610(9) . ? Ca1 O8B 2.690(8) . ? Ca1 Ni1 3.4030(10) . ? N1 Ni1 1.827(3) . ? N2 Ni1 1.825(3) . ? N3 O7 1.227(5) . ? N3 O6 1.230(4) . ? N3 O5 1.233(4) . ? N4 O9A 1.113(8) . ? N4 O10 1.191(4) . ? N4 O9B 1.274(9) . ? N4 O8B 1.303(8) . ? N4 O8A 1.366(6) . ? Ni1 O1 1.830(2) . ? Ni1 O2 1.844(2) . ? O9A O9B 0.913(9) . ? O9A O8B 1.212(11) . ? 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 C1 C6 123.9(3) . . ? O1 C1 C2 117.1(3) . . ? C6 C1 C2 118.9(3) . . ? C3 C2 O3 125.8(3) . . ? C3 C2 C1 120.3(4) . . ? O3 C2 C1 113.9(3) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.6(4) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 118.3(4) . . ? C5 C6 C7 120.4(4) . . ? C1 C6 C7 121.3(3) . . ? N1 C7 C6 125.9(3) . . ? N1 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? C9 C8 N1 112.2(5) . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? N1 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 N2 113.2(4) . . ? C8 C9 H9A 108.9 . . ? N2 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? N2 C9 H9B 108.9 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C11 125.3(3) . . ? N2 C10 H10 117.4 . . ? C11 C10 H10 117.4 . . ? C12 C11 C16 119.0(5) . . ? C12 C11 C10 119.1(4) . . ? C16 C11 C10 121.8(4) . . ? C13 C12 C11 120.3(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 122.1(5) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 119.0(5) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O4 C15 C14 125.1(4) . . ? O4 C15 C16 114.8(3) . . ? C14 C15 C16 120.1(4) . . ? O2 C16 C15 117.7(3) . . ? O2 C16 C11 123.0(4) . . ? C15 C16 C11 119.3(4) . . ? C18 C17 O3 107.5(4) . . ? C18 C17 H17A 110.2 . . ? O3 C17 H17A 110.2 . . ? C18 C17 H17B 110.2 . . ? O3 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 110.0(6) . . ? O4 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? O4 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9A Ca1 O11 82.13(19) . . ? O9A Ca1 O1 84.1(2) . . ? O11 Ca1 O1 146.89(10) . . ? O9A Ca1 O2 81.0(2) . . ? O11 Ca1 O2 143.66(10) . . ? O1 Ca1 O2 61.98(8) . . ? O9A Ca1 O6 158.40(18) . . ? O11 Ca1 O6 118.83(11) . . ? O1 Ca1 O6 80.22(12) . . ? O2 Ca1 O6 78.55(10) . . ? O9A Ca1 O3 94.3(3) . . ? O11 Ca1 O3 87.47(10) . . ? O1 Ca1 O3 63.71(8) . . ? O2 Ca1 O3 125.69(8) . . ? O6 Ca1 O3 91.95(14) . . ? O9A Ca1 O4 93.2(3) . . ? O11 Ca1 O4 85.75(10) . . ? O1 Ca1 O4 125.04(9) . . ? O2 Ca1 O4 63.38(8) . . ? O6 Ca1 O4 83.92(14) . . ? O3 Ca1 O4 169.13(9) . . ? O9A Ca1 O5 152.63(18) . . ? O11 Ca1 O5 71.37(10) . . ? O1 Ca1 O5 114.65(10) . . ? O2 Ca1 O5 124.81(9) . . ? O6 Ca1 O5 48.97(9) . . ? O3 Ca1 O5 78.15(10) . . ? O4 Ca1 O5 91.62(10) . . ? O9A Ca1 O9B 20.1(2) . . ? O11 Ca1 O9B 75.3(2) . . ? O1 Ca1 O9B 99.9(2) . . ? O2 Ca1 O9B 77.91(19) . . ? O6 Ca1 O9B 153.1(2) . . ? O3 Ca1 O9B 112.45(19) . . ? O4 Ca1 O9B 73.9(2) . . ? O5 Ca1 O9B 144.5(2) . . ? O9A Ca1 O8B 26.7(3) . . ? O11 Ca1 O8B 75.9(2) . . ? O1 Ca1 O8B 78.3(2) . . ? O2 Ca1 O8B 101.0(2) . . ? O6 Ca1 O8B 155.7(2) . . ? O3 Ca1 O8B 68.31(17) . . ? O4 Ca1 O8B 117.97(17) . . ? O5 Ca1 O8B 133.6(2) . . ? O9B Ca1 O8B 44.2(2) . . ? O9A Ca1 Ni1 82.50(17) . . ? O11 Ca1 Ni1 164.61(8) . . ? O1 Ca1 Ni1 30.81(6) . . ? O2 Ca1 Ni1 31.21(6) . . ? O6 Ca1 Ni1 76.40(8) . . ? O3 Ca1 Ni1 94.49(6) . . ? O4 Ca1 Ni1 94.30(6) . . ? O5 Ca1 Ni1 123.97(7) . . ? O9B Ca1 Ni1 89.95(19) . . ? O8B Ca1 Ni1 90.6(2) . . ? C7 N1 C8 118.8(4) . . ? C7 N1 Ni1 126.5(3) . . ? C8 N1 Ni1 114.7(4) . . ? C10 N2 C9 119.4(4) . . ? C10 N2 Ni1 126.8(3) . . ? C9 N2 Ni1 113.8(4) . . ? O7 N3 O6 121.0(4) . . ? O7 N3 O5 121.8(4) . . ? O6 N3 O5 117.2(4) . . ? O9A N4 O10 131.7(6) . . ? O9A N4 O9B 44.3(5) . . ? O10 N4 O9B 119.8(5) . . ? O9A N4 O8B 59.6(7) . . ? O10 N4 O8B 122.8(5) . . ? O9B N4 O8B 101.6(8) . . ? O9A N4 O8A 121.7(5) . . ? O10 N4 O8A 106.6(5) . . ? O9B N4 O8A 111.3(5) . . ? O8B N4 O8A 91.1(6) . . ? N2 Ni1 N1 85.92(16) . . ? N2 Ni1 O1 178.09(13) . . ? N1 Ni1 O1 95.70(14) . . ? N2 Ni1 O2 95.21(14) . . ? N1 Ni1 O2 178.16(13) . . ? O1 Ni1 O2 83.19(11) . . ? N2 Ni1 Ca1 136.94(12) . . ? N1 Ni1 Ca1 137.06(11) . . ? O1 Ni1 Ca1 41.50(8) . . ? O2 Ni1 Ca1 41.75(7) . . ? C1 O1 Ni1 126.7(2) . . ? C1 O1 Ca1 125.4(2) . . ? Ni1 O1 Ca1 107.69(11) . . ? C16 O2 Ni1 127.3(2) . . ? C16 O2 Ca1 125.4(2) . . ? Ni1 O2 Ca1 107.04(10) . . ? C2 O3 C17 118.0(3) . . ? C2 O3 Ca1 119.76(19) . . ? C17 O3 Ca1 122.2(2) . . ? C15 O4 C19 119.3(3) . . ? C15 O4 Ca1 118.6(2) . . ? C19 O4 Ca1 122.1(3) . . ? N3 O5 Ca1 94.5(2) . . ? N3 O6 Ca1 98.9(3) . . ? O9B O9A N4 77.2(9) . . ? O9B O9A O8B 139.6(12) . . ? N4 O9A O8B 68.0(7) . . ? O9B O9A Ca1 100.0(11) . . ? N4 O9A Ca1 142.2(5) . . ? O8B O9A Ca1 95.3(6) . . ? O9A O9B N4 58.5(7) . . ? O9A O9B Ca1 59.8(9) . . ? N4 O9B Ca1 108.3(5) . . ? O9A O8B N4 52.4(4) . . ? O9A O8B Ca1 58.0(5) . . ? N4 O8B Ca1 103.1(5) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 153 31 ' ' 2 1.000 0.000 0.500 153 31 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.746 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.059 #END=== data_8 _database_code_depnum_ccdc_archive 'CCDC 813963' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H25 Cd N5 Ni O10' _chemical_formula_weight 690.58 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' Cd Cd -0.8075 1.2024 '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 8.0768(13) _cell_length_b 12.074(2) _cell_length_c 14.348(2) _cell_angle_alpha 67.471(5) _cell_angle_beta 89.983(5) _cell_angle_gamma 83.029(6) _cell_volume 1281.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2547 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 19.45 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.630 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7580 _exptl_absorpt_correction_T_max 0.8039 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16171 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.16 _reflns_number_total 5414 _reflns_number_gt 3136 _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^)+(0.0900P)^2^+0.1500P] 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 5414 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1724 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _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 C1 C -0.0103(9) 0.1221(7) 0.5855(6) 0.0438(19) Uani 1 1 d . . . C2 C -0.0819(10) 0.0472(8) 0.6751(7) 0.049(2) Uani 1 1 d . . . C3 C -0.2143(10) -0.0045(8) 0.6723(7) 0.056(2) Uani 1 1 d . . . H3 H -0.2554 -0.0541 0.7324 0.067 Uiso 1 1 calc R . . C4 C -0.2962(11) 0.0138(9) 0.5787(8) 0.060(2) Uani 1 1 d . . . H4 H -0.3908 -0.0226 0.5775 0.072 Uiso 1 1 calc R . . C5 C -0.2338(11) 0.0858(8) 0.4903(8) 0.057(2) Uani 1 1 d . . . H5 H -0.2858 0.0978 0.4287 0.069 Uiso 1 1 calc R . . C6 C -0.0943(9) 0.1405(7) 0.4923(6) 0.0424(19) Uani 1 1 d . . . C7 C -0.0338(12) 0.2197(8) 0.3984(7) 0.060(2) Uani 1 1 d . . . H7 H -0.0954 0.2333 0.3395 0.072 Uiso 1 1 calc R . . C8 C 0.1377(13) 0.3575(10) 0.2889(7) 0.069(3) Uani 1 1 d . . . H8A H 0.0878 0.4393 0.2771 0.082 Uiso 1 1 calc R . . H8B H 0.0951 0.3346 0.2366 0.082 Uiso 1 1 calc R . . C9 C 0.3240(14) 0.3502(9) 0.2882(7) 0.067(3) Uani 1 1 d . . . H9A H 0.3713 0.2811 0.2737 0.081 Uiso 1 1 calc R . . H9B H 0.3566 0.4228 0.2370 0.081 Uiso 1 1 calc R . . C10 C 0.5183(11) 0.3782(7) 0.4018(6) 0.050(2) Uani 1 1 d . . . H10 H 0.5715 0.4198 0.3436 0.060 Uiso 1 1 calc R . . C11 C 0.5943(9) 0.3661(7) 0.4953(6) 0.0410(18) Uani 1 1 d . . . C12 C 0.7390(11) 0.4235(7) 0.4956(7) 0.055(2) Uani 1 1 d . . . H12 H 0.7798 0.4723 0.4350 0.065 Uiso 1 1 calc R . . C13 C 0.8164(11) 0.4061(8) 0.5853(7) 0.058(2) Uani 1 1 d . . . H13 H 0.9130 0.4409 0.5854 0.069 Uiso 1 1 calc R . . C14 C 0.7547(11) 0.3381(8) 0.6759(7) 0.054(2) Uani 1 1 d . . . H14 H 0.8074 0.3304 0.7361 0.065 Uiso 1 1 calc R . . C15 C 0.6143(9) 0.2805(7) 0.6786(6) 0.0440(19) Uani 1 1 d . . . C16 C 0.5314(10) 0.2981(7) 0.5874(6) 0.0440(19) Uani 1 1 d . . . C17 C -0.0425(14) -0.0424(9) 0.8595(7) 0.068(3) Uani 1 1 d . . . H17A H -0.1634 -0.0328 0.8605 0.082 Uiso 1 1 calc R . . H17B H 0.0006 -0.0212 0.9127 0.082 Uiso 1 1 calc R . . C18 C 0.0195(15) -0.1704(9) 0.8800(8) 0.087(3) Uani 1 1 d . . . H18A H -0.0106 -0.1890 0.8234 0.130 Uiso 1 1 calc R . . H18B H -0.0295 -0.2218 0.9393 0.130 Uiso 1 1 calc R . . H18C H 0.1389 -0.1835 0.8905 0.130 Uiso 1 1 calc R . . C19 C 0.6142(12) 0.1913(9) 0.8623(7) 0.063(3) Uani 1 1 d . . . H19A H 0.7352 0.1780 0.8636 0.075 Uiso 1 1 calc R . . H19B H 0.5767 0.1204 0.9132 0.075 Uiso 1 1 calc R . . C20 C 0.5592(16) 0.3005(10) 0.8866(8) 0.084(3) Uani 1 1 d . . . H20A H 0.5626 0.3726 0.8273 0.127 Uiso 1 1 calc R . . H20B H 0.6326 0.3010 0.9390 0.127 Uiso 1 1 calc R . . H20C H 0.4472 0.2975 0.9091 0.127 Uiso 1 1 calc R . . C21 C 0.7316(12) 0.4557(10) 0.0924(10) 0.071(3) Uani 1 1 d . . . C22 C 0.7532(16) 0.5286(12) -0.0130(8) 0.103(4) Uani 1 1 d . . . H22A H 0.7621 0.6101 -0.0205 0.155 Uiso 1 1 calc R . . H22B H 0.6587 0.5281 -0.0533 0.155 Uiso 1 1 calc R . . H22C H 0.8530 0.4957 -0.0347 0.155 Uiso 1 1 calc R . . Cd1 Cd 0.27224(7) 0.13740(5) 0.73900(4) 0.0447(2) Uani 1 1 d . . . N1 N 0.0989(9) 0.2737(6) 0.3888(5) 0.0503(17) Uani 1 1 d . . . N2 N 0.3831(9) 0.3374(6) 0.3894(5) 0.0503(17) Uani 1 1 d . . . N3 N 0.4474(10) -0.0938(7) 0.8224(6) 0.061(2) Uani 1 1 d . . . N4 N 0.1172(10) 0.2949(8) 0.8249(6) 0.059(2) Uani 1 1 d . . . N5 N 0.7156(14) 0.4011(11) 0.1752(8) 0.101(3) Uani 1 1 d . . . Ni1 Ni 0.25058(12) 0.25667(8) 0.48967(7) 0.0398(3) Uani 1 1 d . . . O1 O 0.1228(6) 0.1729(5) 0.5924(4) 0.0436(13) Uani 1 1 d . . . O2 O 0.3952(6) 0.2416(5) 0.5931(4) 0.0466(13) Uani 1 1 d . . . O3 O 0.0073(7) 0.0404(5) 0.7616(4) 0.0554(15) Uani 1 1 d . . . O4 O 0.5473(7) 0.2074(5) 0.7644(4) 0.0544(15) Uani 1 1 d . . . O5 O 0.4013(9) -0.0533(6) 0.7325(5) 0.0721(19) Uani 1 1 d . . . O6 O 0.3988(9) -0.0338(6) 0.8740(5) 0.0721(19) Uani 1 1 d . . . O7 O 0.5395(10) -0.1916(7) 0.8621(6) 0.094(2) Uani 1 1 d . . . O8 O 0.1561(9) 0.3373(6) 0.7362(5) 0.0740(19) Uani 1 1 d . . . O9 O 0.1602(10) 0.1825(6) 0.8740(5) 0.077(2) Uani 1 1 d . . . O10 O 0.0382(9) 0.3563(7) 0.8653(6) 0.079(2) 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 C1 0.034(4) 0.041(4) 0.056(5) -0.021(4) 0.003(4) 0.003(3) C2 0.041(5) 0.056(5) 0.066(6) -0.038(5) 0.008(4) -0.014(4) C3 0.042(5) 0.055(5) 0.074(7) -0.026(5) 0.015(4) -0.010(4) C4 0.046(5) 0.066(6) 0.081(7) -0.041(6) 0.003(5) -0.010(5) C5 0.051(5) 0.062(6) 0.069(7) -0.041(5) -0.017(5) 0.009(4) C6 0.034(4) 0.045(4) 0.055(5) -0.027(4) -0.002(4) -0.004(3) C7 0.065(6) 0.057(6) 0.063(6) -0.037(5) -0.015(5) 0.016(5) C8 0.083(7) 0.084(7) 0.041(5) -0.019(5) -0.009(5) -0.032(6) C9 0.095(8) 0.070(6) 0.042(5) -0.020(5) 0.010(5) -0.033(6) C10 0.057(5) 0.045(5) 0.049(5) -0.016(4) 0.020(4) -0.016(4) C11 0.034(4) 0.044(4) 0.053(5) -0.025(4) 0.013(4) -0.012(3) C12 0.050(5) 0.045(5) 0.071(6) -0.022(4) 0.019(5) -0.014(4) C13 0.043(5) 0.062(6) 0.075(7) -0.029(5) 0.009(5) -0.020(4) C14 0.045(5) 0.065(6) 0.059(6) -0.031(5) -0.001(4) -0.009(4) C15 0.029(4) 0.056(5) 0.046(5) -0.016(4) 0.004(3) -0.012(4) C16 0.043(4) 0.039(4) 0.051(5) -0.018(4) 0.006(4) -0.008(4) C17 0.088(7) 0.070(6) 0.054(6) -0.026(5) 0.026(5) -0.030(6) C18 0.099(9) 0.074(7) 0.080(8) -0.017(6) 0.011(7) -0.028(7) C19 0.059(6) 0.078(7) 0.051(6) -0.022(5) -0.013(4) -0.015(5) C20 0.113(10) 0.090(8) 0.058(7) -0.036(6) 0.010(6) -0.019(7) C21 0.045(6) 0.078(7) 0.092(9) -0.037(7) -0.006(6) -0.007(5) C22 0.101(10) 0.117(11) 0.062(8) -0.009(7) -0.011(7) 0.009(8) Cd1 0.0457(4) 0.0492(4) 0.0402(4) -0.0166(3) 0.0024(3) -0.0121(3) N1 0.059(5) 0.047(4) 0.048(4) -0.021(3) 0.000(3) -0.011(4) N2 0.064(5) 0.052(4) 0.040(4) -0.023(3) 0.003(3) -0.009(4) N3 0.062(5) 0.051(5) 0.059(6) -0.009(4) 0.010(4) -0.008(4) N4 0.053(5) 0.079(6) 0.060(5) -0.043(5) -0.002(4) -0.012(4) N5 0.095(8) 0.109(8) 0.086(8) -0.024(7) 0.016(6) -0.018(6) Ni1 0.0439(6) 0.0395(6) 0.0370(6) -0.0155(4) 0.0021(4) -0.0069(5) O1 0.037(3) 0.054(3) 0.044(3) -0.022(3) 0.001(2) -0.015(3) O2 0.043(3) 0.063(4) 0.034(3) -0.016(3) 0.007(2) -0.014(3) O3 0.059(4) 0.057(4) 0.047(4) -0.015(3) 0.006(3) -0.013(3) O4 0.056(4) 0.067(4) 0.043(3) -0.022(3) 0.003(3) -0.021(3) O5 0.077(5) 0.078(5) 0.046(4) -0.012(3) 0.008(3) 0.005(4) O6 0.084(5) 0.060(4) 0.075(5) -0.030(4) -0.006(4) -0.004(4) O7 0.101(6) 0.075(5) 0.084(5) -0.014(4) 0.006(5) 0.011(5) O8 0.085(5) 0.084(5) 0.051(4) -0.027(4) -0.001(4) 0.000(4) O9 0.095(5) 0.058(4) 0.080(5) -0.029(4) 0.016(4) -0.009(4) O10 0.082(5) 0.081(5) 0.085(5) -0.046(4) 0.008(4) 0.001(4) _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 C1 O1 1.322(9) . ? C1 C6 1.427(11) . ? C1 C2 1.428(11) . ? C2 C3 1.310(11) . ? C2 O3 1.405(10) . ? C3 C4 1.424(13) . ? C3 H3 0.9300 . ? C4 C5 1.371(13) . ? C4 H4 0.9300 . ? C5 C6 1.379(11) . ? C5 H5 0.9300 . ? C6 C7 1.446(12) . ? C7 N1 1.301(11) . ? C7 H7 0.9300 . ? C8 N1 1.463(11) . ? C8 C9 1.496(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.474(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.290(10) . ? C10 C11 1.424(11) . ? C10 H10 0.9300 . ? C11 C16 1.396(11) . ? C11 C12 1.430(11) . ? C12 C13 1.362(12) . ? C12 H12 0.9300 . ? C13 C14 1.376(12) . ? C13 H13 0.9300 . ? C14 C15 1.394(11) . ? C14 H14 0.9300 . ? C15 O4 1.367(9) . ? C15 C16 1.399(11) . ? C16 O2 1.350(9) . ? C17 O3 1.469(10) . ? C17 C18 1.480(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.439(10) . ? C19 C20 1.506(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N5 1.133(13) . ? C21 C22 1.451(16) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? Cd1 O2 2.288(5) . ? Cd1 O1 2.291(5) . ? Cd1 O6 2.343(7) . ? Cd1 O9 2.357(7) . ? Cd1 O5 2.445(7) . ? Cd1 O8 2.467(7) . ? Cd1 O3 2.524(6) . ? Cd1 O4 2.544(6) . ? N1 Ni1 1.830(7) . ? N2 Ni1 1.828(7) . ? N3 O5 1.230(9) . ? N3 O7 1.242(10) . ? N3 O6 1.253(10) . ? N4 O10 1.228(9) . ? N4 O8 1.233(9) . ? N4 O9 1.270(10) . ? Ni1 O2 1.828(5) . ? Ni1 O1 1.836(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 C1 C6 123.9(7) . . ? O1 C1 C2 120.0(7) . . ? C6 C1 C2 116.1(7) . . ? C3 C2 O3 127.1(8) . . ? C3 C2 C1 122.3(8) . . ? O3 C2 C1 110.6(7) . . ? C2 C3 C4 121.1(9) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.2(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.3(8) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 121.1(8) . . ? C5 C6 C7 119.5(8) . . ? C1 C6 C7 119.4(7) . . ? N1 C7 C6 126.1(8) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? N1 C8 C9 106.5(7) . . ? N1 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? N1 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N2 C9 C8 106.8(7) . . ? N2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? N2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 126.7(7) . . ? N2 C10 H10 116.7 . . ? C11 C10 H10 116.7 . . ? C16 C11 C10 121.3(7) . . ? C16 C11 C12 119.0(8) . . ? C10 C11 C12 119.7(7) . . ? C13 C12 C11 119.4(8) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.4(8) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 120.8(8) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? O4 C15 C14 125.3(7) . . ? O4 C15 C16 115.9(7) . . ? C14 C15 C16 118.8(7) . . ? O2 C16 C11 122.3(7) . . ? O2 C16 C15 117.1(7) . . ? C11 C16 C15 120.5(7) . . ? O3 C17 C18 112.4(8) . . ? O3 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? O3 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 110.9(8) . . ? O4 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C22 178.3(13) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 Cd1 O1 64.54(18) . . ? O2 Cd1 O6 125.9(2) . . ? O1 Cd1 O6 135.9(2) . . ? O2 Cd1 O9 135.5(2) . . ? O1 Cd1 O9 123.7(2) . . ? O6 Cd1 O9 81.0(3) . . ? O2 Cd1 O5 89.8(2) . . ? O1 Cd1 O5 88.1(2) . . ? O6 Cd1 O5 52.8(2) . . ? O9 Cd1 O5 131.0(2) . . ? O2 Cd1 O8 86.1(2) . . ? O1 Cd1 O8 91.0(2) . . ? O6 Cd1 O8 129.4(2) . . ? O9 Cd1 O8 52.5(2) . . ? O5 Cd1 O8 175.8(2) . . ? O2 Cd1 O3 129.15(19) . . ? O1 Cd1 O3 64.84(18) . . ? O6 Cd1 O3 88.8(2) . . ? O9 Cd1 O3 79.2(2) . . ? O5 Cd1 O3 84.0(2) . . ? O8 Cd1 O3 99.3(2) . . ? O2 Cd1 O4 65.17(18) . . ? O1 Cd1 O4 129.60(18) . . ? O6 Cd1 O4 79.2(2) . . ? O9 Cd1 O4 90.8(2) . . ? O5 Cd1 O4 94.9(2) . . ? O8 Cd1 O4 82.5(2) . . ? O3 Cd1 O4 165.54(18) . . ? C7 N1 C8 119.5(7) . . ? C7 N1 Ni1 126.6(6) . . ? C8 N1 Ni1 113.8(6) . . ? C10 N2 C9 120.9(7) . . ? C10 N2 Ni1 125.9(6) . . ? C9 N2 Ni1 113.2(6) . . ? O5 N3 O7 121.7(9) . . ? O5 N3 O6 118.2(8) . . ? O7 N3 O6 120.1(9) . . ? O10 N4 O8 122.7(9) . . ? O10 N4 O9 120.2(9) . . ? O8 N4 O9 117.1(8) . . ? O2 Ni1 N2 95.0(3) . . ? O2 Ni1 N1 177.7(3) . . ? N2 Ni1 N1 86.6(3) . . ? O2 Ni1 O1 83.7(2) . . ? N2 Ni1 O1 178.4(3) . . ? N1 Ni1 O1 94.7(3) . . ? C1 O1 Ni1 127.7(5) . . ? C1 O1 Cd1 125.4(5) . . ? Ni1 O1 Cd1 105.7(2) . . ? C16 O2 Ni1 127.6(5) . . ? C16 O2 Cd1 125.3(5) . . ? Ni1 O2 Cd1 106.1(2) . . ? C2 O3 C17 116.9(7) . . ? C2 O3 Cd1 118.5(5) . . ? C17 O3 Cd1 123.5(5) . . ? C15 O4 C19 120.5(7) . . ? C15 O4 Cd1 115.8(4) . . ? C19 O4 Cd1 122.7(5) . . ? N3 O5 Cd1 92.1(5) . . ? N3 O6 Cd1 96.4(5) . . ? N4 O8 Cd1 93.0(5) . . ? N4 O9 Cd1 97.2(5) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.16 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.901 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.174 #END=== data_9 _database_code_depnum_ccdc_archive 'CCDC 813964' #TrackingRef '- 1-10 CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 N8 Ni2 O20 Pb2' _chemical_formula_weight 1488.63 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' Pb Pb -3.3944 10.1111 '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 14.2881(12) _cell_length_b 13.7472(11) _cell_length_c 12.8579(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.288(2) _cell_angle_gamma 90.00 _cell_volume 2436.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5999 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 24.02 _exptl_crystal_description square _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 7.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2479 _exptl_absorpt_correction_T_max 0.3365 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24691 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.99 _reflns_number_total 5205 _reflns_number_gt 3687 _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. C17-C18, C19-C20 distances are fixed to 1.5 ^A^. ; _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^)+(0.0600P)^2^+3.0500P] 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 5205 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.998 _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 C1 C 0.2512(5) 0.2323(5) 0.3809(6) 0.0593(19) Uani 1 1 d . . . C2 C 0.3140(6) 0.2292(7) 0.3121(6) 0.069(2) Uani 1 1 d . . . C3 C 0.3454(8) 0.1415(8) 0.2833(8) 0.095(3) Uani 1 1 d . . . H3 H 0.3889 0.1410 0.2407 0.114 Uiso 1 1 calc R . . C4 C 0.3152(10) 0.0552(8) 0.3147(10) 0.107(4) Uani 1 1 d . . . H4 H 0.3377 -0.0032 0.2937 0.128 Uiso 1 1 calc R . . C5 C 0.2517(8) 0.0551(7) 0.3770(8) 0.091(3) Uani 1 1 d . . . H5 H 0.2296 -0.0037 0.3975 0.109 Uiso 1 1 calc R . . C6 C 0.2192(6) 0.1431(6) 0.4107(6) 0.0615(19) Uani 1 1 d . . . C7 C 0.1504(6) 0.1381(6) 0.4737(7) 0.071(2) Uani 1 1 d . . . H7 H 0.1268 0.0767 0.4839 0.085 Uiso 1 1 calc R . . C8 C 0.0450(10) 0.1937(8) 0.5749(11) 0.125(5) Uani 1 1 d . . . H8A H -0.0175 0.1844 0.5234 0.150 Uiso 1 1 calc R . . H8B H 0.0606 0.1347 0.6174 0.150 Uiso 1 1 calc R . . C10 C 0.0646(6) 0.4410(7) 0.6488(6) 0.070(2) Uani 1 1 d . . . H10 H 0.0245 0.4405 0.6951 0.084 Uiso 1 1 calc R . . C11 C 0.1054(7) 0.5321(6) 0.6290(7) 0.070(2) Uani 1 1 d . . . C12 C 0.0822(8) 0.6138(7) 0.6832(8) 0.096(3) Uani 1 1 d . . . H12 H 0.0372 0.6081 0.7236 0.115 Uiso 1 1 calc R . . C13 C 0.1242(9) 0.6988(7) 0.6770(9) 0.108(4) Uani 1 1 d . . . H13 H 0.1091 0.7520 0.7143 0.130 Uiso 1 1 calc R . . C14 C 0.1895(8) 0.7097(7) 0.6163(8) 0.092(3) Uani 1 1 d . . . H14 H 0.2180 0.7700 0.6127 0.110 Uiso 1 1 calc R . . C15 C 0.2130(6) 0.6318(6) 0.5610(7) 0.066(2) Uani 1 1 d . . . C16 C 0.1714(6) 0.5396(5) 0.5656(7) 0.0561(18) Uani 1 1 d . . . C9 C 0.0391(8) 0.2716(8) 0.6428(8) 0.099(3) Uani 1 1 d . . . H9A H 0.0747 0.2562 0.7162 0.119 Uiso 1 1 calc R . . H9B H -0.0281 0.2830 0.6418 0.119 Uiso 1 1 calc R . . N1 N 0.1179(5) 0.2103(5) 0.5176(5) 0.0648(17) Uani 1 1 d . . . N2 N 0.0801(5) 0.3598(5) 0.6065(5) 0.0626(16) Uani 1 1 d . . . N4 N 0.4778(5) 0.4118(6) 0.5919(5) 0.0649(17) Uani 1 1 d . . . Ni1 Ni 0.15390(6) 0.33782(6) 0.51257(7) 0.0498(2) Uani 1 1 d . . . O1 O 0.2241(3) 0.3172(3) 0.4117(4) 0.0557(12) Uani 1 1 d . . . O2 O 0.1961(4) 0.4660(3) 0.5133(4) 0.0557(12) Uani 1 1 d . . . O3 O 0.3388(4) 0.3193(5) 0.2806(5) 0.0781(16) Uani 1 1 d . . . O4 O 0.2754(5) 0.6366(4) 0.4967(6) 0.089(2) Uani 1 1 d . . . O8 O 0.4244(5) 0.3540(5) 0.5328(5) 0.0916(19) Uani 1 1 d . . . O9 O 0.4530(7) 0.5001(6) 0.5857(6) 0.115(3) Uani 1 1 d . . . O10 O 0.5528(5) 0.3888(5) 0.6575(5) 0.0913(19) Uani 1 1 d . . . Pb1 Pb 0.307664(19) 0.47275(2) 0.39805(2) 0.05263(12) Uani 1 1 d . . . O5A O 0.2168(9) 0.5484(8) 0.1811(10) 0.130(4) Uiso 0.80 1 d P . . O6A O 0.1324(11) 0.5158(11) 0.2777(13) 0.146(5) Uiso 0.80 1 d P . . N3 N 0.1346(6) 0.5381(5) 0.1943(8) 0.081(2) Uani 1 1 d . . . O7 O 0.0610(7) 0.5556(6) 0.1292(7) 0.134(3) Uani 1 1 d . . . C17 C 0.3884(8) 0.3187(8) 0.1969(8) 0.096(3) Uani 1 1 d D . . H17A H 0.4494 0.2841 0.2218 0.115 Uiso 1 1 calc R . . H17B H 0.3492 0.2848 0.1344 0.115 Uiso 1 1 calc R . . C18 C 0.4066(10) 0.4149(10) 0.1674(9) 0.132(5) Uani 1 1 d D . . H18A H 0.3510 0.4549 0.1648 0.198 Uiso 1 1 calc R . . H18B H 0.4193 0.4142 0.0977 0.198 Uiso 1 1 calc R . . H18C H 0.4619 0.4408 0.2196 0.198 Uiso 1 1 calc R . . C19 C 0.3034(12) 0.7408(12) 0.4598(13) 0.155(6) Uani 1 1 d D . . H19A H 0.3215 0.7386 0.3922 0.186 Uiso 1 1 calc R . . H19B H 0.2529 0.7888 0.4559 0.186 Uiso 1 1 calc R . . C20 C 0.3833(12) 0.7547(17) 0.5489(16) 0.225(11) Uani 1 1 d D . . H20A H 0.3673 0.7328 0.6131 0.338 Uiso 1 1 calc R . . H20B H 0.3997 0.8225 0.5557 0.338 Uiso 1 1 calc R . . H20C H 0.4376 0.7181 0.5390 0.338 Uiso 1 1 calc R . . O5B O 0.1445(17) 0.4513(17) 0.2470(19) 0.049(6) Uiso 0.20 1 d P . . O6B O 0.1514(19) 0.575(2) 0.300(2) 0.063(7) Uiso 0.20 1 d P . . 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 C1 0.048(4) 0.061(4) 0.062(4) -0.018(4) 0.004(4) -0.002(4) C2 0.059(5) 0.083(6) 0.065(5) -0.019(4) 0.019(4) 0.005(4) C3 0.103(8) 0.099(8) 0.091(7) -0.032(6) 0.038(6) 0.022(6) C4 0.134(10) 0.078(7) 0.111(9) -0.035(6) 0.039(8) 0.022(7) C5 0.107(8) 0.067(5) 0.089(7) -0.021(5) 0.009(6) 0.012(5) C6 0.062(5) 0.069(5) 0.047(4) -0.008(3) 0.003(4) -0.002(4) C7 0.074(6) 0.069(5) 0.065(5) -0.003(4) 0.012(4) -0.013(4) C8 0.163(12) 0.090(7) 0.165(11) -0.012(8) 0.119(10) -0.038(8) C10 0.077(6) 0.091(6) 0.056(4) 0.005(4) 0.042(4) 0.004(5) C11 0.077(6) 0.069(5) 0.081(6) 0.012(4) 0.049(5) 0.022(4) C12 0.135(9) 0.076(6) 0.108(8) 0.008(5) 0.086(7) 0.029(6) C13 0.175(12) 0.072(6) 0.113(8) -0.016(6) 0.099(9) 0.021(7) C14 0.130(9) 0.057(5) 0.106(7) 0.002(5) 0.063(7) 0.024(5) C15 0.078(6) 0.060(5) 0.073(5) -0.001(4) 0.042(5) 0.011(4) C16 0.055(4) 0.053(4) 0.064(4) 0.008(3) 0.022(4) 0.012(3) C9 0.115(8) 0.113(8) 0.091(7) -0.010(6) 0.064(7) -0.045(7) N1 0.068(4) 0.062(4) 0.070(4) 0.004(3) 0.030(4) -0.010(3) N2 0.066(4) 0.071(4) 0.063(4) 0.000(3) 0.038(3) -0.005(3) N4 0.059(4) 0.080(5) 0.058(4) 0.009(4) 0.019(4) -0.019(4) Ni1 0.0423(5) 0.0558(5) 0.0546(5) 0.0011(4) 0.0188(4) -0.0017(4) O1 0.057(3) 0.058(3) 0.058(3) -0.008(2) 0.026(2) -0.004(2) O2 0.057(3) 0.052(3) 0.069(3) -0.003(2) 0.034(3) 0.001(2) O3 0.083(4) 0.090(4) 0.075(4) -0.016(3) 0.046(3) 0.002(3) O4 0.108(5) 0.056(3) 0.129(5) -0.013(3) 0.078(4) -0.017(3) O8 0.073(4) 0.092(4) 0.099(5) 0.014(4) 0.002(4) -0.028(4) O9 0.153(8) 0.096(5) 0.085(5) -0.009(4) 0.015(5) 0.010(5) O10 0.067(4) 0.118(5) 0.083(4) 0.017(4) 0.009(4) -0.016(4) Pb1 0.04721(18) 0.06178(19) 0.05531(18) -0.00115(13) 0.02483(13) -0.00217(13) N3 0.071(5) 0.071(5) 0.096(6) 0.010(4) 0.010(5) 0.005(4) O7 0.114(6) 0.112(6) 0.135(7) 0.002(5) -0.043(6) 0.031(5) C17 0.102(8) 0.126(9) 0.074(6) -0.019(6) 0.048(6) -0.007(7) C18 0.144(11) 0.185(14) 0.085(8) -0.030(9) 0.062(8) -0.040(11) C19 0.154(15) 0.175(15) 0.168(14) -0.048(12) 0.101(13) -0.026(12) C20 0.132(15) 0.32(3) 0.24(2) -0.10(2) 0.086(16) 0.014(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.323(8) . ? C1 C6 1.398(11) . ? C1 C2 1.417(11) . ? C2 C3 1.371(12) . ? C2 O3 1.378(10) . ? C3 C4 1.360(16) . ? C3 H3 0.9300 . ? C4 C5 1.360(16) . ? C4 H4 0.9300 . ? C5 C6 1.405(12) . ? C5 H5 0.9300 . ? C6 C7 1.430(11) . ? C7 N1 1.288(10) . ? C7 H7 0.9300 . ? C8 C9 1.399(14) . ? C8 N1 1.444(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 N2 1.285(10) . ? C10 C11 1.433(12) . ? C10 H10 0.9300 . ? C11 C16 1.404(10) . ? C11 C12 1.407(11) . ? C12 C13 1.326(14) . ? C12 H12 0.9300 . ? C13 C14 1.374(13) . ? C13 H13 0.9300 . ? C14 C15 1.376(11) . ? C14 H14 0.9300 . ? C15 O4 1.368(9) . ? C15 C16 1.407(11) . ? C16 O2 1.313(8) . ? C9 N2 1.475(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N1 Ni1 1.833(6) . ? N2 Ni1 1.826(6) . ? N4 O10 1.219(8) . ? N4 O8 1.218(8) . ? N4 O9 1.260(10) . ? Ni1 O1 1.859(4) . ? Ni1 O2 1.862(5) . ? O1 Pb1 2.478(5) . ? O2 Pb1 2.448(5) . ? O3 C17 1.436(10) . ? O3 Pb1 2.699(5) . ? O4 C19 1.592(17) . ? O4 Pb1 2.684(6) . ? O8 Pb1 2.631(6) . ? O9 Pb1 2.763(8) . ? Pb1 O5B 2.63(2) . ? Pb1 O6A 2.640(16) . ? Pb1 O6B 2.66(3) . ? Pb1 O5A 2.940(12) . ? O5A N3 1.238(13) . ? O5A O5B 2.01(3) . ? O5A O6B 2.02(3) . ? O6A O6B 0.88(3) . ? O6A N3 1.124(15) . ? O6A O5B 1.00(2) . ? N3 O7 1.184(10) . ? N3 O6B 1.41(3) . ? N3 O5B 1.36(2) . ? C17 C18 1.419(13) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.401(15) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 123.3(7) . . ? O1 C1 C2 119.8(7) . . ? C6 C1 C2 116.9(7) . . ? C3 C2 O3 125.7(8) . . ? C3 C2 C1 120.1(9) . . ? O3 C2 C1 114.2(7) . . ? C4 C3 C2 122.3(10) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 119.3(9) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.5(10) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.8(8) . . ? C1 C6 C7 121.5(7) . . ? C5 C6 C7 117.7(9) . . ? N1 C7 C6 126.3(8) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? C9 C8 N1 111.6(8) . . ? C9 C8 H8A 109.3 . . ? N1 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? N1 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C10 C11 124.1(7) . . ? N2 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C16 C11 C12 120.8(8) . . ? C16 C11 C10 122.3(7) . . ? C12 C11 C10 116.7(8) . . ? C13 C12 C11 120.2(8) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.1(8) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.3(9) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? O4 C15 C14 124.1(8) . . ? O4 C15 C16 114.8(6) . . ? C14 C15 C16 121.0(7) . . ? O2 C16 C11 123.6(7) . . ? O2 C16 C15 119.9(6) . . ? C11 C16 C15 116.5(7) . . ? C8 C9 N2 109.7(7) . . ? C8 C9 H9A 109.7 . . ? N2 C9 H9A 109.7 . . ? C8 C9 H9B 109.7 . . ? N2 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C7 N1 C8 119.6(7) . . ? C7 N1 Ni1 125.8(6) . . ? C8 N1 Ni1 114.6(6) . . ? C10 N2 C9 116.9(7) . . ? C10 N2 Ni1 128.1(5) . . ? C9 N2 Ni1 114.9(6) . . ? O10 N4 O8 123.6(8) . . ? O10 N4 O9 118.4(8) . . ? O8 N4 O9 118.0(8) . . ? N2 Ni1 N1 85.3(3) . . ? N2 Ni1 O1 177.3(3) . . ? N1 Ni1 O1 95.0(3) . . ? N2 Ni1 O2 94.8(3) . . ? N1 Ni1 O2 177.0(3) . . ? O1 Ni1 O2 85.1(2) . . ? C1 O1 Ni1 126.8(5) . . ? C1 O1 Pb1 123.7(4) . . ? Ni1 O1 Pb1 106.0(2) . . ? C16 O2 Ni1 127.0(4) . . ? C16 O2 Pb1 125.9(4) . . ? Ni1 O2 Pb1 107.13(19) . . ? C2 O3 C17 115.5(7) . . ? C2 O3 Pb1 116.5(4) . . ? C17 O3 Pb1 127.6(6) . . ? C15 O4 C19 118.6(7) . . ? C15 O4 Pb1 117.7(5) . . ? C19 O4 Pb1 121.8(6) . . ? N4 O8 Pb1 101.0(5) . . ? N4 O9 Pb1 93.3(5) . . ? O2 Pb1 O1 61.42(14) . . ? O2 Pb1 O5B 81.4(5) . . ? O1 Pb1 O5B 66.8(5) . . ? O2 Pb1 O6A 72.3(4) . . ? O1 Pb1 O6A 80.5(4) . . ? O5B Pb1 O6A 22.0(5) . . ? O2 Pb1 O6B 73.1(6) . . ? O1 Pb1 O6B 97.5(6) . . ? O5B Pb1 O6B 40.4(8) . . ? O6A Pb1 O6B 19.1(6) . . ? O2 Pb1 O8 88.79(19) . . ? O1 Pb1 O8 69.61(18) . . ? O5B Pb1 O8 134.6(5) . . ? O6A Pb1 O8 149.7(4) . . ? O6B Pb1 O8 161.5(6) . . ? O2 Pb1 O4 61.66(15) . . ? O1 Pb1 O4 123.02(16) . . ? O5B Pb1 O4 102.4(5) . . ? O6A Pb1 O4 80.5(4) . . ? O6B Pb1 O4 63.5(6) . . ? O8 Pb1 O4 111.6(2) . . ? O2 Pb1 O3 122.61(16) . . ? O1 Pb1 O3 61.22(16) . . ? O5B Pb1 O3 75.2(5) . . ? O6A Pb1 O3 96.8(4) . . ? O6B Pb1 O3 112.9(6) . . ? O8 Pb1 O3 73.4(2) . . ? O4 Pb1 O3 174.09(19) . . ? O2 Pb1 O9 86.3(2) . . ? O1 Pb1 O9 108.7(2) . . ? O5B Pb1 O9 167.6(6) . . ? O6A Pb1 O9 149.3(4) . . ? O6B Pb1 O9 133.4(6) . . ? O8 Pb1 O9 46.3(2) . . ? O4 Pb1 O9 69.9(2) . . ? O3 Pb1 O9 113.5(2) . . ? O2 Pb1 O5A 113.1(3) . . ? O1 Pb1 O5A 105.8(3) . . ? O5B Pb1 O5A 41.8(6) . . ? O6A Pb1 O5A 41.5(4) . . ? O6B Pb1 O5A 41.9(6) . . ? O8 Pb1 O5A 152.8(3) . . ? O4 Pb1 O5A 93.6(3) . . ? O3 Pb1 O5A 80.9(3) . . ? O9 Pb1 O5A 145.4(3) . . ? N3 O5A O5B 41.7(9) . . ? N3 O5A O6B 43.4(10) . . ? O5B O5A O6B 53.9(11) . . ? N3 O5A Pb1 91.6(8) . . ? O5B O5A Pb1 60.8(7) . . ? O6B O5A Pb1 61.6(8) . . ? O6B O6A N3 88(2) . . ? O6B O6A O5B 151(3) . . ? N3 O6A O5B 79.3(19) . . ? O6B O6A Pb1 82(2) . . ? N3 O6A Pb1 111.1(11) . . ? O5B O6A Pb1 78.3(17) . . ? O6A N3 O7 119.1(13) . . ? O6A N3 O6B 38.7(12) . . ? O7 N3 O6B 120.1(14) . . ? O6A N3 O5A 115.3(13) . . ? O7 N3 O5A 125.3(12) . . ? O6B N3 O5A 99.4(14) . . ? O6A N3 O5B 46.5(11) . . ? O7 N3 O5B 119.1(13) . . ? O6B N3 O5B 82.4(16) . . ? O5A N3 O5B 101.0(13) . . ? C18 C17 O3 110.9(9) . . ? C18 C17 H17A 109.5 . . ? O3 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 O4 95.4(16) . . ? C20 C19 H19A 112.7 . . ? O4 C19 H19A 112.7 . . ? C20 C19 H19B 112.7 . . ? O4 C19 H19B 112.7 . . ? H19A C19 H19B 110.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6A O5B N3 54.2(15) . . ? O6A O5B O5A 74.9(17) . . ? N3 O5B O5A 37.2(7) . . ? O6A O5B Pb1 79.7(17) . . ? N3 O5B Pb1 103.0(13) . . ? O5A O5B Pb1 77.4(8) . . ? O6A O6B N3 52.9(18) . . ? O6A O6B O5A 76(2) . . ? N3 O6B O5A 37.2(8) . . ? O6A O6B Pb1 79(2) . . ? N3 O6B Pb1 100.1(14) . . ? O5A O6B Pb1 76.5(9) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.945 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.131