Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address ' Michaele J. Hardie ' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Nino Malic ' ; School of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; ' Colin L. Raston' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name ' Colin L. Raston' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_email ' c.l.raston@chem.leeds.ac.uk ' _publ_contact_author_fax ' 44-113-233 6401 ' _publ_section_title ; Mineralomimetic host-guest chemistry: the encapsulation of [M+[2.2.2]cryptate] (M=Na, K) by saddle shaped Ni(II) macrocycles ; data_compound1 _database_code_CSD 157600 _chemical_name_systematic ; {potassium 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane} {carbadodecaborane(12)} tris-{5,7,12,14-tetramethyldibenzo[b,i]-1,4,8,11, tetraazacyclotetrdecinenickel(II)} ; _chemical_name_common '{potassium[2.2.2]cryptate}{carborane}tris{Ni(TMTAA)}' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H114 B11 K N14 Ni3 O6' _chemical_formula_weight 1762.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'K' 'K' 0.2009 0.2494 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'trigonal (hexagonal)' _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 18.0689(2) _cell_length_b 18.0689(2) _cell_length_c 46.1059(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13036.2(4) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35176 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6885 _reflns_number_gt 5589 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.397(11) _refine_ls_number_reflns 6885 _refine_ls_number_parameters 366 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 B4 B 0.36494(18) 0.63240(19) 1.17173(6) 0.0297(7) Uani 0.92 1 d P . 1 H4 H 0.3858 0.6096 1.1910 0.036 Uiso 1 1 calc R . 1 B3 B 0.3976(2) 0.69747(19) 1.11451(7) 0.0305(7) Uani 0.92 1 d P . 1 H3 H 0.4409 0.7182 1.0952 0.037 Uiso 1 1 calc R . 1 B2 B 0.38426(17) 0.61215(17) 1.13584(7) 0.0266(6) Uani 0.92 1 d P . 1 H2 H 0.4182 0.5759 1.1310 0.032 Uiso 1 1 calc R . 1 B1 B 0.27798(17) 0.56039(19) 1.14954(7) 0.0268(6) Uani 0.92 1 d P . 1 H1 H 0.2414 0.4900 1.1540 0.032 Uiso 1 1 calc R . 1 C22 C 0.71748(15) 0.74658(15) 0.98937(5) 0.0276(5) Uani 1 1 d . . . H22A H 0.7377 0.7483 0.9695 0.041 Uiso 1 1 calc R . . H22B H 0.7600 0.7491 1.0031 0.041 Uiso 1 1 calc R . . H22C H 0.7090 0.7955 0.9925 0.041 Uiso 1 1 calc R . . C21 C 0.63361(14) 0.66437(14) 0.99387(5) 0.0180(4) Uani 1 1 d . . . C20 C 0.57763(14) 0.66929(14) 1.01348(5) 0.0204(5) Uani 1 1 d . . . H20 H 0.5979 0.7228 1.0229 0.024 Uiso 1 1 calc R . . C19 C 0.45089(16) 0.62981(16) 1.04347(5) 0.0255(5) Uani 1 1 d . . . H19A H 0.4537 0.6064 1.0623 0.038 Uiso 1 1 calc R . . H19B H 0.3910 0.6069 1.0380 0.038 Uiso 1 1 calc R . . H19C H 0.4793 0.6922 1.0447 0.038 Uiso 1 1 calc R . . C18 C 0.49491(14) 0.60502(15) 1.02103(4) 0.0197(5) Uani 1 1 d . . . C17 C 0.37827(14) 0.45880(14) 1.01556(4) 0.0180(5) Uani 1 1 d . . . C16 C 0.34160(15) 0.44128(15) 1.04341(5) 0.0241(5) Uani 1 1 d . . . H16 H 0.3682 0.4819 1.0585 0.029 Uiso 1 1 calc R . . C15 C 0.26666(15) 0.36503(16) 1.04896(5) 0.0272(5) Uani 1 1 d . . . H15 H 0.2411 0.3544 1.0676 0.033 Uiso 1 1 calc R . . C14 C 0.22924(15) 0.30428(16) 1.02712(5) 0.0273(6) Uani 1 1 d . . . H14 H 0.1781 0.2521 1.0309 0.033 Uiso 1 1 calc R . . C13 C 0.26602(14) 0.31929(15) 0.99993(5) 0.0243(5) Uani 1 1 d . . . H13 H 0.2414 0.2762 0.9855 0.029 Uiso 1 1 calc R . . C12 C 0.33863(14) 0.39676(14) 0.99347(5) 0.0181(4) Uani 1 1 d . . . C11 C 0.25625(15) 0.33399(15) 0.93595(5) 0.0264(5) Uani 1 1 d . . . H11A H 0.2250 0.3477 0.9503 0.040 Uiso 1 1 calc R . . H11B H 0.2404 0.2738 0.9379 0.040 Uiso 1 1 calc R . . H11C H 0.2418 0.3441 0.9164 0.040 Uiso 1 1 calc R . . C10 C 0.35082(14) 0.38971(13) 0.94089(5) 0.0184(5) Uani 1 1 d . . . C9 C 0.40218(15) 0.41069(14) 0.91622(5) 0.0219(5) Uani 1 1 d . . . H9 H 0.3729 0.3937 0.8982 0.026 Uiso 1 1 calc R . . C8 C 0.52916(16) 0.46640(17) 0.88465(5) 0.0280(5) Uani 1 1 d . . . H8A H 0.5373 0.4182 0.8797 0.042 Uiso 1 1 calc R . . H8B H 0.5844 0.5195 0.8842 0.042 Uiso 1 1 calc R . . H8C H 0.4905 0.4699 0.8705 0.042 Uiso 1 1 calc R . . C7 C 0.49088(15) 0.45339(15) 0.91470(5) 0.0206(5) Uani 1 1 d . . . C6 C 0.62873(14) 0.52107(14) 0.93860(4) 0.0185(5) Uani 1 1 d . . . C5 C 0.67634(15) 0.49640(15) 0.92182(5) 0.0232(5) Uani 1 1 d . . . H5 H 0.6486 0.4526 0.9077 0.028 Uiso 1 1 calc R . . C4 C 0.76421(15) 0.53508(16) 0.92539(5) 0.0258(5) Uani 1 1 d . . . H4A H 0.7965 0.5195 0.9131 0.031 Uiso 1 1 calc R . . C3 C 0.80472(15) 0.59586(17) 0.94659(6) 0.0260(5) Uani 1 1 d . . . H3A H 0.8649 0.6223 0.9489 0.031 Uiso 1 1 calc R . . C2 C 0.75772(14) 0.61874(15) 0.96479(5) 0.0225(5) Uani 1 1 d . . . H2A H 0.7856 0.6589 0.9799 0.027 Uiso 1 1 calc R . . C1 C 0.66978(14) 0.58261(13) 0.96076(5) 0.0178(5) Uani 1 1 d . . . N4 N 0.45741(11) 0.52933(11) 1.00733(4) 0.0170(4) Uani 1 1 d . . . N3 N 0.38547(11) 0.42004(11) 0.96714(4) 0.0174(4) Uani 1 1 d . . . N2 N 0.53909(12) 0.48517(11) 0.93851(4) 0.0176(4) Uani 1 1 d . . . N1 N 0.61196(11) 0.59387(11) 0.97834(4) 0.0171(4) Uani 1 1 d . . . Ni1 Ni 0.498753(16) 0.505983(17) 0.973080(8) 0.01437(7) Uani 1 1 d . . . C28 C 0.42139(16) 0.72274(15) 0.96932(5) 0.0236(5) Uani 1 1 d . . . H28A H 0.4229 0.7179 0.9907 0.028 Uiso 1 1 calc R . . H28B H 0.4382 0.7826 0.9647 0.028 Uiso 1 1 calc R . . C27 C 0.48620(15) 0.70317(16) 0.95613(5) 0.0262(5) Uani 1 1 d . . . H27A H 0.5434 0.7417 0.9645 0.031 Uiso 1 1 calc R . . H27B H 0.4706 0.6436 0.9607 0.031 Uiso 1 1 calc R . . C24 C 0.48062(17) 0.69029(18) 0.83806(5) 0.0327(6) Uani 1 1 d . . . H24A H 0.5218 0.6767 0.8288 0.039 Uiso 1 1 calc R . . H24B H 0.5045 0.7529 0.8372 0.039 Uiso 1 1 calc R . . C23 C 0.39746(17) 0.64620(19) 0.82224(5) 0.0328(6) Uani 1 1 d . . . H23A H 0.4081 0.6619 0.8015 0.039 Uiso 1 1 calc R . . H23B H 0.3739 0.5837 0.8237 0.039 Uiso 1 1 calc R . . N6 N 0.3333 0.6667 0.95927(7) 0.0197(7) Uani 1 3 d S . . N5 N 0.3333 0.6667 0.83303(7) 0.0258(8) Uani 1 3 d S . . O2 O 0.48871(10) 0.71432(12) 0.92574(3) 0.0280(4) Uani 1 1 d . . . O1 O 0.46828(10) 0.66345(12) 0.86724(3) 0.0303(4) Uani 1 1 d . . . K1 K 0.3333 0.6667 0.896139(15) 0.01604(17) Uani 1 3 d S . . C4A C 0.36494(18) 0.63240(19) 1.17173(6) 0.0297(7) Uani 0.08 1 d P . 2 C1A C 0.27798(17) 0.56039(19) 1.14954(7) 0.0268(6) Uani 0.08 1 d P . 2 C2A C 0.38426(17) 0.61215(17) 1.13584(7) 0.0266(6) Uani 0.08 1 d P . 2 C3A C 0.3976(2) 0.69747(19) 1.11451(7) 0.0305(7) Uani 0.08 1 d P . 2 C25 C 0.54921(16) 0.7018(2) 0.88164(6) 0.0375(6) Uani 1 1 d . . . H25A H 0.5785 0.7646 0.8794 0.045 Uiso 1 1 calc R . . H25B H 0.5856 0.6813 0.8728 0.045 Uiso 1 1 calc R . . C26 C 0.53645(18) 0.6793(2) 0.91250(6) 0.0404(7) Uani 1 1 d . . . H26A H 0.5051 0.6164 0.9147 0.048 Uiso 1 1 calc R . . H26B H 0.5925 0.7022 0.9222 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B4 0.0287(16) 0.0313(16) 0.0276(14) 0.0046(12) -0.0059(12) 0.0138(14) B3 0.0317(17) 0.0330(17) 0.0281(15) -0.0007(12) 0.0080(12) 0.0171(14) B2 0.0191(14) 0.0159(13) 0.0457(17) 0.0011(12) 0.0022(12) 0.0094(12) B1 0.0178(14) 0.0169(14) 0.0450(17) 0.0039(12) 0.0021(12) 0.0082(12) C22 0.0199(12) 0.0208(13) 0.0374(14) -0.0021(10) -0.0006(10) 0.0067(10) C21 0.0177(11) 0.0147(11) 0.0196(10) 0.0006(8) -0.0056(9) 0.0066(9) C20 0.0216(12) 0.0185(12) 0.0209(12) -0.0040(9) -0.0039(9) 0.0100(10) C19 0.0289(13) 0.0261(13) 0.0235(11) -0.0034(10) 0.0001(10) 0.0153(12) C18 0.0247(13) 0.0234(12) 0.0151(10) 0.0002(9) -0.0037(9) 0.0151(11) C17 0.0148(11) 0.0200(12) 0.0217(11) 0.0047(9) 0.0010(9) 0.0105(10) C16 0.0223(12) 0.0278(13) 0.0233(12) 0.0040(10) 0.0044(10) 0.0132(11) C15 0.0225(13) 0.0340(14) 0.0279(12) 0.0145(11) 0.0093(10) 0.0162(11) C14 0.0144(12) 0.0311(14) 0.0335(13) 0.0135(11) 0.0042(10) 0.0091(11) C13 0.0161(12) 0.0220(12) 0.0327(13) 0.0059(10) -0.0011(10) 0.0080(10) C12 0.0133(11) 0.0203(12) 0.0216(10) 0.0056(9) 0.0016(9) 0.0089(10) C11 0.0221(13) 0.0269(14) 0.0245(12) -0.0034(10) -0.0055(10) 0.0079(11) C10 0.0177(11) 0.0128(11) 0.0243(11) -0.0011(9) -0.0038(9) 0.0074(9) C9 0.0230(12) 0.0185(12) 0.0213(11) -0.0045(9) -0.0067(9) 0.0082(10) C8 0.0288(13) 0.0346(14) 0.0190(11) -0.0019(10) 0.0000(10) 0.0146(12) C7 0.0260(13) 0.0179(11) 0.0196(11) 0.0016(9) -0.0013(10) 0.0122(10) C6 0.0196(12) 0.0197(12) 0.0183(10) 0.0073(9) 0.0029(9) 0.0114(10) C5 0.0287(13) 0.0262(13) 0.0187(11) 0.0078(10) 0.0066(10) 0.0168(11) C4 0.0255(13) 0.0301(13) 0.0277(13) 0.0114(10) 0.0101(10) 0.0182(12) C3 0.0178(12) 0.0305(14) 0.0315(13) 0.0130(11) 0.0048(10) 0.0134(11) C2 0.0174(12) 0.0229(13) 0.0270(12) 0.0059(10) 0.0003(10) 0.0099(10) C1 0.0172(11) 0.0170(11) 0.0206(10) 0.0062(9) 0.0038(9) 0.0096(9) N4 0.0145(9) 0.0197(10) 0.0161(9) 0.0016(7) 0.0021(7) 0.0081(8) N3 0.0152(10) 0.0151(9) 0.0207(9) 0.0011(7) -0.0013(7) 0.0067(8) N2 0.0198(10) 0.0143(9) 0.0192(10) 0.0006(7) 0.0011(8) 0.0089(9) N1 0.0150(9) 0.0171(9) 0.0185(10) 0.0041(7) 0.0007(7) 0.0074(8) Ni1 0.01249(13) 0.01358(13) 0.01490(13) 0.00045(11) 0.00045(11) 0.00491(11) C28 0.0233(12) 0.0242(13) 0.0188(12) -0.0015(9) -0.0053(10) 0.0084(10) C27 0.0232(13) 0.0288(14) 0.0256(12) 0.0044(10) -0.0032(10) 0.0122(11) C24 0.0306(15) 0.0372(15) 0.0286(13) -0.0064(11) 0.0069(11) 0.0155(13) C23 0.0370(16) 0.0404(16) 0.0240(13) -0.0059(11) 0.0044(11) 0.0216(13) N6 0.0200(11) 0.0200(11) 0.0192(16) 0.000 0.000 0.0100(5) N5 0.0268(12) 0.0268(12) 0.0239(18) 0.000 0.000 0.0134(6) O2 0.0222(9) 0.0426(11) 0.0246(8) -0.0002(8) -0.0005(7) 0.0202(9) O1 0.0209(9) 0.0452(11) 0.0278(8) -0.0050(8) -0.0005(7) 0.0186(8) K1 0.0159(2) 0.0159(2) 0.0163(4) 0.000 0.000 0.00796(11) C4A 0.0287(16) 0.0313(16) 0.0276(14) 0.0046(12) -0.0059(12) 0.0138(14) C1A 0.0178(14) 0.0169(14) 0.0450(17) 0.0039(12) 0.0021(12) 0.0082(12) C2A 0.0191(14) 0.0159(13) 0.0457(17) 0.0011(12) 0.0022(12) 0.0094(12) C3A 0.0317(17) 0.0330(17) 0.0281(15) -0.0007(12) 0.0080(12) 0.0171(14) C25 0.0206(13) 0.0534(18) 0.0417(14) -0.0052(13) 0.0007(11) 0.0209(13) C26 0.0311(15) 0.0603(19) 0.0430(14) -0.0054(14) -0.0044(12) 0.0327(15) _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 B4 B2 1.767(4) . ? B4 B1 1.778(4) 2_665 ? B4 B1 1.779(4) . ? B4 B4 1.786(5) 2_665 ? B4 B4 1.786(5) 3_565 ? B3 B2 1.741(4) . ? B3 B3 1.742(6) 3_565 ? B3 B3 1.742(6) 2_665 ? B3 B1 1.744(4) 2_665 ? B3 B2 1.748(4) 2_665 ? B2 B3 1.748(4) 3_565 ? B2 B1 1.767(4) 2_665 ? B2 B1 1.779(4) . ? B1 B3 1.744(4) 3_565 ? B1 B2 1.767(4) 3_565 ? B1 B4 1.778(4) 3_565 ? C22 C21 1.515(3) . ? C21 N1 1.338(3) . ? C21 C20 1.393(3) . ? C20 C18 1.403(3) . ? C19 C18 1.503(3) . ? C18 N4 1.342(3) . ? C17 C16 1.407(3) . ? C17 N4 1.411(3) . ? C17 C12 1.416(3) . ? C16 C15 1.390(3) . ? C15 C14 1.391(4) . ? C14 C13 1.380(3) . ? C13 C12 1.390(3) . ? C12 N3 1.418(3) . ? C11 C10 1.505(3) . ? C10 N3 1.347(3) . ? C10 C9 1.395(3) . ? C9 C7 1.390(3) . ? C8 C7 1.514(3) . ? C7 N2 1.339(3) . ? C6 C5 1.386(3) . ? C6 N2 1.412(3) . ? C6 C1 1.416(3) . ? C5 C4 1.388(3) . ? C4 C3 1.376(4) . ? C3 C2 1.396(3) . ? C2 C1 1.396(3) . ? C1 N1 1.415(3) . ? N4 Ni1 1.8827(19) . ? N3 Ni1 1.8703(18) . ? N2 Ni1 1.8673(19) . ? N1 Ni1 1.8753(18) . ? C28 N6 1.470(3) . ? C28 C27 1.510(3) . ? C27 O2 1.413(3) . ? C24 O1 1.409(3) . ? C24 C23 1.493(4) . ? C23 N5 1.468(3) . ? N6 C28 1.470(3) 2_665 ? N6 C28 1.470(3) 3_565 ? N6 K1 2.911(3) . ? N5 C23 1.468(3) 2_665 ? N5 C23 1.468(3) 3_565 ? N5 K1 2.910(4) . ? O2 C26 1.436(3) . ? O2 K1 2.8404(16) . ? O1 C25 1.430(3) . ? O1 K1 2.8047(16) . ? K1 O1 2.8048(16) 2_665 ? K1 O1 2.8048(16) 3_565 ? K1 O2 2.8404(16) 2_665 ? K1 O2 2.8404(17) 3_565 ? C25 C26 1.466(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B2 B4 B1 59.81(16) . 2_665 ? B2 B4 B1 60.23(16) . . ? B1 B4 B1 108.2(2) 2_665 . ? B2 B4 B4 107.57(14) . 2_665 ? B1 B4 B4 59.90(19) 2_665 2_665 ? B1 B4 B4 107.91(17) . 2_665 ? B2 B4 B4 107.77(14) . 3_565 ? B1 B4 B4 107.97(17) 2_665 3_565 ? B1 B4 B4 59.82(19) . 3_565 ? B4 B4 B4 60.000(2) 2_665 3_565 ? B2 B3 B3 60.2(2) . 3_565 ? B2 B3 B3 108.83(18) . 2_665 ? B3 B3 B3 60.000(3) 3_565 2_665 ? B2 B3 B1 60.95(17) . 2_665 ? B3 B3 B1 109.06(16) 3_565 2_665 ? B3 B3 B1 109.08(15) 2_665 2_665 ? B2 B3 B2 110.1(3) . 2_665 ? B3 B3 B2 108.52(17) 3_565 2_665 ? B3 B3 B2 59.86(19) 2_665 2_665 ? B1 B3 B2 61.27(16) 2_665 2_665 ? B3 B2 B3 59.9(2) . 3_565 ? B3 B2 B4 107.4(2) . . ? B3 B2 B4 107.2(2) 3_565 . ? B3 B2 B1 59.61(16) . 2_665 ? B3 B2 B1 107.7(2) 3_565 2_665 ? B4 B2 B1 60.39(17) . 2_665 ? B3 B2 B1 107.5(2) . . ? B3 B2 B1 59.26(17) 3_565 . ? B4 B2 B1 60.22(17) . . ? B1 B2 B1 108.7(3) 2_665 . ? B3 B1 B2 59.44(16) 3_565 3_565 ? B3 B1 B4 106.8(2) 3_565 3_565 ? B2 B1 B4 59.79(16) 3_565 3_565 ? B3 B1 B4 106.8(2) 3_565 . ? B2 B1 B4 107.9(2) 3_565 . ? B4 B1 B4 60.3(2) 3_565 . ? B3 B1 B2 59.47(16) 3_565 . ? B2 B1 B2 107.4(3) 3_565 . ? B4 B1 B2 107.6(2) 3_565 . ? B4 B1 B2 59.55(16) . . ? N1 C21 C20 122.2(2) . . ? N1 C21 C22 122.2(2) . . ? C20 C21 C22 115.4(2) . . ? C21 C20 C18 128.0(2) . . ? N4 C18 C20 120.9(2) . . ? N4 C18 C19 123.7(2) . . ? C20 C18 C19 115.3(2) . . ? C16 C17 N4 126.8(2) . . ? C16 C17 C12 118.9(2) . . ? N4 C17 C12 113.87(18) . . ? C15 C16 C17 120.5(2) . . ? C16 C15 C14 119.8(2) . . ? C13 C14 C15 120.4(2) . . ? C14 C13 C12 120.8(2) . . ? C13 C12 C17 119.5(2) . . ? C13 C12 N3 127.2(2) . . ? C17 C12 N3 112.99(19) . . ? N3 C10 C9 120.8(2) . . ? N3 C10 C11 123.3(2) . . ? C9 C10 C11 115.91(19) . . ? C7 C9 C10 128.1(2) . . ? N2 C7 C9 121.3(2) . . ? N2 C7 C8 122.3(2) . . ? C9 C7 C8 116.3(2) . . ? C5 C6 N2 127.2(2) . . ? C5 C6 C1 119.3(2) . . ? N2 C6 C1 113.14(19) . . ? C6 C5 C4 120.6(2) . . ? C3 C4 C5 120.3(2) . . ? C4 C3 C2 120.3(2) . . ? C3 C2 C1 120.0(2) . . ? C2 C1 N1 127.3(2) . . ? C2 C1 C6 119.3(2) . . ? N1 C1 C6 113.06(19) . . ? C18 N4 C17 124.13(19) . . ? C18 N4 Ni1 124.62(15) . . ? C17 N4 Ni1 111.09(14) . . ? C10 N3 C12 124.17(19) . . ? C10 N3 Ni1 124.24(15) . . ? C12 N3 Ni1 111.34(14) . . ? C7 N2 C6 123.4(2) . . ? C7 N2 Ni1 123.38(16) . . ? C6 N2 Ni1 112.25(14) . . ? C21 N1 C1 123.92(19) . . ? C21 N1 Ni1 123.47(15) . . ? C1 N1 Ni1 112.04(14) . . ? N2 Ni1 N3 94.77(8) . . ? N2 Ni1 N1 84.87(8) . . ? N3 Ni1 N1 178.55(8) . . ? N2 Ni1 N4 178.26(9) . . ? N3 Ni1 N4 85.22(8) . . ? N1 Ni1 N4 95.09(8) . . ? N6 C28 C27 114.24(19) . . ? O2 C27 C28 109.83(19) . . ? O1 C24 C23 109.8(2) . . ? N5 C23 C24 114.2(2) . . ? C28 N6 C28 110.55(14) 2_665 . ? C28 N6 C28 110.55(14) 2_665 3_565 ? C28 N6 C28 110.55(14) . 3_565 ? C28 N6 K1 108.37(15) 2_665 . ? C28 N6 K1 108.37(15) . . ? C28 N6 K1 108.37(15) 3_565 . ? C23 N5 C23 109.14(17) 2_665 3_565 ? C23 N5 C23 109.14(17) 2_665 . ? C23 N5 C23 109.14(17) 3_565 . ? C23 N5 K1 109.80(16) 2_665 . ? C23 N5 K1 109.80(16) 3_565 . ? C23 N5 K1 109.80(16) . . ? C27 O2 C26 110.00(18) . . ? C27 O2 K1 118.48(13) . . ? C26 O2 K1 112.49(14) . . ? C24 O1 C25 109.20(19) . . ? C24 O1 K1 115.84(14) . . ? C25 O1 K1 117.28(13) . . ? O1 K1 O1 99.29(5) 2_665 3_565 ? O1 K1 O1 99.29(5) 2_665 . ? O1 K1 O1 99.29(5) 3_565 . ? O1 K1 O2 59.79(5) 2_665 2_665 ? O1 K1 O2 112.39(5) 3_565 2_665 ? O1 K1 O2 143.81(6) . 2_665 ? O1 K1 O2 143.81(5) 2_665 3_565 ? O1 K1 O2 59.79(5) 3_565 3_565 ? O1 K1 O2 112.39(5) . 3_565 ? O2 K1 O2 98.85(5) 2_665 3_565 ? O1 K1 O2 112.39(5) 2_665 . ? O1 K1 O2 143.81(5) 3_565 . ? O1 K1 O2 59.79(5) . . ? O2 K1 O2 98.85(5) 2_665 . ? O2 K1 O2 98.85(4) 3_565 . ? O1 K1 N5 61.63(4) 2_665 . ? O1 K1 N5 61.63(4) 3_565 . ? O1 K1 N5 61.63(4) . . ? O2 K1 N5 118.71(4) 2_665 . ? O2 K1 N5 118.71(4) 3_565 . ? O2 K1 N5 118.71(4) . . ? O1 K1 N6 118.37(4) 2_665 . ? O1 K1 N6 118.37(4) 3_565 . ? O1 K1 N6 118.37(4) . . ? O2 K1 N6 61.29(4) 2_665 . ? O2 K1 N6 61.29(4) 3_565 . ? O2 K1 N6 61.29(4) . . ? N5 K1 N6 180.000(1) . . ? O1 C25 C26 109.6(2) . . ? O2 C26 C25 109.7(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.527 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.099 #=== END data_c_2: _database_code_CSD 157601 _audit_creation_method SHELXL-97 _chemical_name_systematic ; {sodium 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane} {carbadodecaborane(12)}tris-{5,7,12,14-tetramethyldibenzo[b,i]-1,4,8,11, tetraazacyclotetrdecinenickel(II)} ; _chemical_name_common '{sodium[2.2.2]cryptate}{carborane}tris{Ni(TMTAA)}' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H114 B11 N14 Na Ni3 O6' _chemical_formula_weight 1745.93 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting 'trigonal (hexagonal)' _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 18.0480(1) _cell_length_b 18.0480(1) _cell_length_c 45.4396(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12818.1(2) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5520 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28096 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6810 _reflns_number_gt 6347 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+10.0022P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.274(9) _refine_ls_number_reflns 6810 _refine_ls_number_parameters 366 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 B4 B 0.36532(13) 0.63263(13) 1.17121(5) 0.0242(4) Uani 0.92 1 d P . 1 H4 H 0.3864 0.6100 1.1907 0.029 Uiso 1 1 calc R . 1 B3 B 0.39739(16) 0.69814(14) 1.11314(5) 0.0252(5) Uani 0.92 1 d P . 1 H3 H 0.4406 0.7195 1.0935 0.030 Uiso 1 1 calc R . 1 B2 B 0.38501(12) 0.61257(12) 1.13480(5) 0.0216(4) Uani 0.92 1 d P . 1 H2 H 0.4194 0.5767 1.1299 0.026 Uiso 1 1 calc R . 1 B1 B 0.27885(12) 0.56032(13) 1.14875(6) 0.0214(4) Uani 0.92 1 d P . 1 H1 H 0.2427 0.4899 1.1533 0.026 Uiso 1 1 calc R . 1 C22 C 0.71259(11) 0.74766(11) 0.98636(4) 0.0227(3) Uani 1 1 d . . . H22A H 0.7324 0.7479 0.9663 0.034 Uiso 1 1 calc R . . H22B H 0.7561 0.7529 1.0004 0.034 Uiso 1 1 calc R . . H22C H 0.7026 0.7959 0.9889 0.034 Uiso 1 1 calc R . . C21 C 0.63013(10) 0.66474(10) 0.99181(3) 0.0160(3) Uani 1 1 d . . . C20 C 0.57296(10) 0.66941(11) 1.01149(4) 0.0184(3) Uani 1 1 d . . . H20 H 0.5910 0.7238 1.0201 0.022 Uiso 1 1 calc R . . C19 C 0.44697(11) 0.62711(12) 1.04270(4) 0.0221(3) Uani 1 1 d . . . H19A H 0.4560 0.6101 1.0623 0.033 Uiso 1 1 calc R . . H19B H 0.3856 0.5977 1.0383 0.033 Uiso 1 1 calc R . . H19C H 0.4700 0.6891 1.0423 0.033 Uiso 1 1 calc R . . C18 C 0.49226(10) 0.60307(10) 1.01990(3) 0.0168(3) Uani 1 1 d . . . C17 C 0.37916(10) 0.45407(10) 1.01629(4) 0.0165(3) Uani 1 1 d . . . C16 C 0.34355(11) 0.43807(12) 1.04455(4) 0.0227(3) Uani 1 1 d . . . H16 H 0.3714 0.4790 1.0597 0.027 Uiso 1 1 calc R . . C15 C 0.26803(12) 0.36299(13) 1.05053(4) 0.0272(4) Uani 1 1 d . . . H15 H 0.2429 0.3538 1.0695 0.033 Uiso 1 1 calc R . . C14 C 0.22922(11) 0.30135(12) 1.02889(4) 0.0257(4) Uani 1 1 d . . . H14 H 0.1774 0.2500 1.0331 0.031 Uiso 1 1 calc R . . C13 C 0.26548(11) 0.31409(11) 1.00111(4) 0.0222(3) Uani 1 1 d . . . H13 H 0.2400 0.2701 0.9867 0.027 Uiso 1 1 calc R . . C12 C 0.33912(10) 0.39091(10) 0.99408(4) 0.0168(3) Uani 1 1 d . . . C11 C 0.25648(11) 0.31959(11) 0.93604(4) 0.0227(3) Uani 1 1 d . . . H11A H 0.2236 0.3343 0.9496 0.034 Uiso 1 1 calc R . . H11B H 0.2430 0.2606 0.9397 0.034 Uiso 1 1 calc R . . H11C H 0.2415 0.3248 0.9157 0.034 Uiso 1 1 calc R . . C10 C 0.35139(10) 0.37997(10) 0.94085(4) 0.0169(3) Uani 1 1 d . . . C9 C 0.40151(10) 0.40035(10) 0.91558(4) 0.0187(3) Uani 1 1 d . . . H9 H 0.3716 0.3816 0.8974 0.022 Uiso 1 1 calc R . . C8 C 0.52862(11) 0.45537(11) 0.88348(4) 0.0230(4) Uani 1 1 d . . . H8A H 0.5338 0.4051 0.8788 0.034 Uiso 1 1 calc R . . H8B H 0.5853 0.5068 0.8829 0.034 Uiso 1 1 calc R . . H8C H 0.4912 0.4607 0.8690 0.034 Uiso 1 1 calc R . . C7 C 0.49086(11) 0.44525(10) 0.91388(3) 0.0166(3) Uani 1 1 d . . . C6 C 0.62873(10) 0.51705(10) 0.93843(3) 0.0161(3) Uani 1 1 d . . . C5 C 0.67703(11) 0.49083(11) 0.92204(4) 0.0204(3) Uani 1 1 d . . . H5 H 0.6498 0.4458 0.9081 0.024 Uiso 1 1 calc R . . C4 C 0.76527(11) 0.53084(12) 0.92613(4) 0.0227(4) Uani 1 1 d . . . H4A H 0.7985 0.5147 0.9144 0.027 Uiso 1 1 calc R . . C3 C 0.80483(11) 0.59419(13) 0.94733(4) 0.0228(4) Uani 1 1 d . . . H3A H 0.8650 0.6214 0.9500 0.027 Uiso 1 1 calc R . . C2 C 0.75667(11) 0.61807(11) 0.96474(4) 0.0208(3) Uani 1 1 d . . . H2A H 0.7836 0.6599 0.9797 0.025 Uiso 1 1 calc R . . C1 C 0.66881(10) 0.58050(10) 0.96011(4) 0.0153(3) Uani 1 1 d . . . N4 N 0.45696(9) 0.52581(9) 1.00719(3) 0.0153(3) Uani 1 1 d . . . N3 N 0.38514(8) 0.41296(8) 0.96722(3) 0.0155(3) Uani 1 1 d . . . N2 N 0.53888(9) 0.48011(9) 0.93792(3) 0.0153(3) Uani 1 1 d . . . N1 N 0.61014(8) 0.59280(9) 0.97723(3) 0.0148(3) Uani 1 1 d . . . Ni1 Ni 0.498017(12) 0.501826(13) 0.972830(7) 0.01253(5) Uani 1 1 d . . . C28 C 0.41989(12) 0.72817(12) 0.96847(4) 0.0232(4) Uani 1 1 d . . . H28A H 0.4231 0.7188 0.9898 0.028 Uiso 1 1 calc R . . H28B H 0.4298 0.7869 0.9659 0.028 Uiso 1 1 calc R . . C27 C 0.48988(12) 0.72121(13) 0.95284(4) 0.0258(4) Uani 1 1 d . . . H27A H 0.5457 0.7593 0.9623 0.031 Uiso 1 1 calc R . . H27B H 0.4787 0.6617 0.9539 0.031 Uiso 1 1 calc R . . C26 C 0.55169(12) 0.73334(13) 0.90588(5) 0.0312(4) Uani 1 1 d . . . H26A H 0.6008 0.7438 0.9184 0.037 Uiso 1 1 calc R . . H26B H 0.5736 0.7753 0.8896 0.037 Uiso 1 1 calc R . . C25 C 0.51096(13) 0.64429(13) 0.89351(5) 0.0331(4) Uani 1 1 d . . . H25A H 0.5542 0.6375 0.8823 0.040 Uiso 1 1 calc R . . H25B H 0.4906 0.6025 0.9099 0.040 Uiso 1 1 calc R . . C24 C 0.46765(14) 0.66326(16) 0.84610(4) 0.0378(5) Uani 1 1 d . . . H24A H 0.5051 0.6439 0.8372 0.045 Uiso 1 1 calc R . . H24B H 0.5001 0.7265 0.8474 0.045 Uiso 1 1 calc R . . C23 C 0.38833(16) 0.63417(16) 0.82756(5) 0.0399(5) Uani 1 1 d . . . H23A H 0.4056 0.6540 0.8071 0.048 Uiso 1 1 calc R . . H23B H 0.3553 0.5709 0.8273 0.048 Uiso 1 1 calc R . . N6 N 0.3333 0.6667 0.95782(6) 0.0189(5) Uani 1 3 d S . . N5 N 0.3333 0.6667 0.83851(7) 0.0317(7) Uani 1 3 d S . . O2 O 0.49180(9) 0.74545(8) 0.92290(3) 0.0254(3) Uani 1 1 d . . . O1 O 0.44083(9) 0.62694(9) 0.87473(3) 0.0308(3) Uani 1 1 d . . . Na1 Na 0.3333 0.6667 0.89775(3) 0.0218(3) Uani 1 3 d S . . C4A C 0.36532(13) 0.63263(13) 1.17121(5) 0.0242(4) Uani 0.08 1 d P . 2 C1A C 0.27885(12) 0.56032(13) 1.14875(6) 0.0214(4) Uani 0.08 1 d P . 2 C2A C 0.38501(12) 0.61257(12) 1.13480(5) 0.0216(4) Uani 0.08 1 d P . 2 C3A C 0.39739(16) 0.69814(14) 1.11314(5) 0.0252(5) Uani 0.08 1 d P . 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 B4 0.0251(10) 0.0236(10) 0.0241(11) 0.0036(7) -0.0047(8) 0.0124(9) B3 0.0306(11) 0.0287(10) 0.0197(10) 0.0008(7) 0.0070(8) 0.0173(9) B2 0.0179(9) 0.0154(9) 0.0331(11) -0.0005(7) 0.0006(7) 0.0097(8) B1 0.0161(9) 0.0135(9) 0.0338(12) 0.0047(8) 0.0026(7) 0.0068(7) C22 0.0167(8) 0.0179(8) 0.0290(9) -0.0003(7) 0.0004(7) 0.0053(7) C21 0.0147(7) 0.0155(7) 0.0165(7) -0.0007(6) -0.0043(6) 0.0064(6) C20 0.0211(8) 0.0176(8) 0.0165(8) -0.0032(6) -0.0025(6) 0.0097(7) C19 0.0250(9) 0.0267(9) 0.0183(8) -0.0025(6) 0.0011(6) 0.0158(8) C18 0.0174(7) 0.0201(8) 0.0148(7) -0.0021(6) -0.0026(6) 0.0109(6) C17 0.0127(7) 0.0171(7) 0.0201(8) 0.0043(6) 0.0012(6) 0.0077(6) C16 0.0221(8) 0.0269(9) 0.0204(8) 0.0033(7) 0.0020(7) 0.0132(7) C15 0.0236(9) 0.0329(10) 0.0247(9) 0.0134(7) 0.0090(7) 0.0140(8) C14 0.0165(8) 0.0260(9) 0.0305(9) 0.0122(7) 0.0032(7) 0.0075(7) C13 0.0162(8) 0.0194(8) 0.0285(9) 0.0051(7) -0.0006(6) 0.0070(7) C12 0.0133(7) 0.0189(8) 0.0201(8) 0.0031(6) 0.0004(6) 0.0094(6) C11 0.0163(8) 0.0209(8) 0.0260(9) -0.0021(7) -0.0054(6) 0.0055(6) C10 0.0151(7) 0.0125(7) 0.0230(8) -0.0006(6) -0.0038(6) 0.0068(6) C9 0.0212(8) 0.0167(7) 0.0185(8) -0.0042(6) -0.0043(6) 0.0097(6) C8 0.0262(9) 0.0256(8) 0.0167(8) -0.0013(6) 0.0008(7) 0.0127(7) C7 0.0227(8) 0.0133(7) 0.0155(8) -0.0007(6) -0.0004(6) 0.0102(6) C6 0.0156(7) 0.0175(7) 0.0165(8) 0.0050(6) 0.0030(6) 0.0093(6) C5 0.0237(8) 0.0240(8) 0.0182(8) 0.0046(6) 0.0042(6) 0.0156(7) C4 0.0230(8) 0.0300(10) 0.0237(9) 0.0092(7) 0.0077(7) 0.0197(7) C3 0.0151(7) 0.0305(10) 0.0242(9) 0.0085(8) 0.0030(6) 0.0124(7) C2 0.0161(8) 0.0220(8) 0.0227(8) 0.0041(6) -0.0004(6) 0.0085(7) C1 0.0137(7) 0.0169(7) 0.0163(8) 0.0038(6) 0.0027(6) 0.0083(6) N4 0.0143(6) 0.0171(7) 0.0139(7) 0.0011(5) 0.0009(5) 0.0075(6) N3 0.0131(6) 0.0136(6) 0.0192(7) 0.0017(5) 0.0005(5) 0.0062(5) N2 0.0154(6) 0.0148(6) 0.0164(7) 0.0004(5) 0.0007(5) 0.0080(5) N1 0.0121(6) 0.0164(6) 0.0152(7) 0.0012(5) 0.0008(5) 0.0065(5) Ni1 0.01038(9) 0.01227(9) 0.01378(10) -0.00038(6) 0.00076(6) 0.00480(7) C28 0.0236(9) 0.0240(8) 0.0197(8) -0.0041(7) -0.0041(7) 0.0101(7) C27 0.0216(8) 0.0285(9) 0.0269(9) 0.0016(7) -0.0031(7) 0.0122(8) C26 0.0214(9) 0.0364(11) 0.0348(10) -0.0063(8) 0.0006(7) 0.0137(8) C25 0.0321(10) 0.0342(11) 0.0409(11) -0.0073(9) -0.0048(8) 0.0225(9) C24 0.0377(11) 0.0475(13) 0.0303(11) -0.0055(9) 0.0057(8) 0.0229(10) C23 0.0491(13) 0.0514(14) 0.0259(11) -0.0117(9) -0.0016(9) 0.0302(11) N6 0.0182(7) 0.0182(7) 0.0203(14) 0.000 0.000 0.0091(4) N5 0.0338(10) 0.0338(10) 0.0273(16) 0.000 0.000 0.0169(5) O2 0.0257(7) 0.0293(7) 0.0249(7) 0.0003(5) 0.0018(5) 0.0166(5) O1 0.0275(7) 0.0310(7) 0.0323(7) -0.0064(6) -0.0030(5) 0.0134(6) Na1 0.0219(4) 0.0219(4) 0.0218(6) 0.000 0.000 0.01093(18) C4A 0.0251(10) 0.0236(10) 0.0241(11) 0.0036(7) -0.0047(8) 0.0124(9) C1A 0.0161(9) 0.0135(9) 0.0338(12) 0.0047(8) 0.0026(7) 0.0068(7) C2A 0.0179(9) 0.0154(9) 0.0331(11) -0.0005(7) 0.0006(7) 0.0097(8) C3A 0.0306(11) 0.0287(10) 0.0197(10) 0.0008(7) 0.0070(8) 0.0173(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 B4 B2 1.767(3) . ? B4 B1 1.773(3) . ? B4 B1 1.779(3) 2_665 ? B4 B4 1.788(4) 3_565 ? B4 B4 1.788(4) 2_665 ? B3 B3 1.734(4) 3_565 ? B3 B3 1.734(4) 2_665 ? B3 B2 1.744(3) 2_665 ? B3 B1 1.748(3) 2_665 ? B3 B2 1.749(3) . ? B2 B3 1.744(3) 3_565 ? B2 B1 1.774(3) 2_665 ? B2 B1 1.776(3) . ? B1 B3 1.748(3) 3_565 ? B1 B2 1.774(3) 3_565 ? B1 B4 1.779(3) 3_565 ? C22 C21 1.513(2) . ? C21 N1 1.336(2) . ? C21 C20 1.400(2) . ? C20 C18 1.399(2) . ? C19 C18 1.512(2) . ? C18 N4 1.340(2) . ? C17 C16 1.400(2) . ? C17 N4 1.415(2) . ? C17 C12 1.420(2) . ? C16 C15 1.386(3) . ? C15 C14 1.384(3) . ? C14 C13 1.387(3) . ?