# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mitsuhiko Shionoya' _publ_contact_author_email shionoya@chem.s.u-tokyo.ac.jp loop_ _publ_author_name R.Miyake M.Shionoya data_i-4_93K _database_code_depnum_ccdc_archive 'CCDC 856057' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.4881(7) _cell_length_b 15.4881(7) _cell_length_c 19.3282(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4636.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 93 _cell_measurement_reflns_used 8660 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.78 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8679 _exptl_absorpt_correction_T_max 0.9144 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17487 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6693 _reflns_number_gt 6216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1212P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.097(15) _refine_ls_number_reflns 6693 _refine_ls_number_parameters 345 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.195 _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 0.7128(4) 1.0891(3) 0.8056(4) 0.0599(16) Uani 1 1 d . . . H1A H 0.6840 1.0665 0.7642 0.090 Uiso 1 1 calc R . . H1B H 0.7428 1.1429 0.7940 0.090 Uiso 1 1 calc R . . H1C H 0.6697 1.1003 0.8416 0.090 Uiso 1 1 calc R . . C2 C 0.7774(3) 1.0235(2) 0.8316(2) 0.0369(9) Uani 1 1 d . . . C3 C 0.8090(3) 0.9092(2) 0.91621(19) 0.0300(7) Uani 1 1 d . . . H3A H 0.8069 0.9186 0.9669 0.036 Uiso 1 1 calc R . . H3B H 0.8691 0.9196 0.9009 0.036 Uiso 1 1 calc R . . C4 C 0.7853(2) 0.8147(2) 0.90091(17) 0.0230(6) Uani 1 1 d . . . C5 C 0.8507(2) 0.7576(2) 0.94111(19) 0.0279(6) Uani 1 1 d . . . H5A H 0.9095 0.7812 0.9344 0.033 Uiso 1 1 calc R . . H5B H 0.8372 0.7607 0.9911 0.033 Uiso 1 1 calc R . . C6 C 0.6919(2) 0.7984(2) 0.92558(19) 0.0284(7) Uani 1 1 d . . . H6A H 0.6815 0.8325 0.9681 0.034 Uiso 1 1 calc R . . H6B H 0.6515 0.8195 0.8897 0.034 Uiso 1 1 calc R . . C7 C 0.7918(2) 0.7910(2) 0.82379(16) 0.0212(5) Uani 1 1 d . . . C8 C 0.8446(2) 0.8254(2) 0.70758(16) 0.0215(5) Uani 1 1 d . . . H8A H 0.8238 0.8774 0.6829 0.026 Uiso 1 1 calc R . . H8B H 0.8064 0.7767 0.6948 0.026 Uiso 1 1 calc R . . C9 C 0.9368(2) 0.8049(2) 0.68355(16) 0.0211(5) Uani 1 1 d . . . C10 C 0.9979(2) 0.8753(2) 0.71100(17) 0.0233(6) Uani 1 1 d . . . H10A H 0.9684 0.9318 0.7077 0.028 Uiso 1 1 calc R . . H10B H 1.0095 0.8640 0.7606 0.028 Uiso 1 1 calc R . . C11 C 0.9320(2) 0.8069(2) 0.60302(17) 0.0232(6) Uani 1 1 d . . . H11A H 0.8814 0.7726 0.5881 0.028 Uiso 1 1 calc R . . H11B H 0.9224 0.8672 0.5879 0.028 Uiso 1 1 calc R . . C12 C 0.9704(2) 0.7178(2) 0.70667(16) 0.0208(6) Uani 1 1 d . . . N1 N 0.7528(2) 0.9721(2) 0.88282(19) 0.0356(7) Uani 1 1 d . . . H1 H 0.6992 0.9762 0.8975 0.043 Uiso 1 1 calc R . . N2 N 0.84990(19) 0.66609(19) 0.91930(16) 0.0258(5) Uani 1 1 d . . . H2A H 0.8607 0.6323 0.9575 0.031 Uiso 1 1 calc R . . H2B H 0.8945 0.6576 0.8886 0.031 Uiso 1 1 calc R . . N3 N 0.67250(19) 0.70635(18) 0.94013(15) 0.0244(5) Uani 1 1 d . . . H3C H 0.6138 0.6979 0.9374 0.029 Uiso 1 1 calc R . . H3D H 0.6894 0.6936 0.9846 0.029 Uiso 1 1 calc R . . N4 N 0.83816(18) 0.84021(18) 0.78199(14) 0.0220(5) Uani 1 1 d . . . H4 H 0.8665 0.8841 0.7999 0.026 Uiso 1 1 calc R . . N5 N 1.08168(18) 0.88094(18) 0.67383(15) 0.0223(5) Uani 1 1 d . . . H5C H 1.1234 0.8986 0.7046 0.027 Uiso 1 1 calc R . . H5D H 1.0772 0.9227 0.6402 0.027 Uiso 1 1 calc R . . N6 N 1.00988(18) 0.7731(2) 0.56755(14) 0.0234(5) Uani 1 1 d . . . H6C H 1.0210 0.8074 0.5298 0.028 Uiso 1 1 calc R . . H6D H 0.9977 0.7185 0.5514 0.028 Uiso 1 1 calc R . . N7 N 0.91896(19) 0.6629(2) 0.73916(17) 0.0274(6) Uani 1 1 d . . . H7A H 0.9391 0.6126 0.7530 0.033 Uiso 1 1 calc R . . H7B H 0.8647 0.6766 0.7469 0.033 Uiso 1 1 calc R . . O4M O 0.1059(3) 0.5996(3) 0.9224(3) 0.0552(12) Uani 0.75 1 d PDU . . Ni1 Ni 0.73358(2) 0.62209(2) 0.872297(19) 0.01978(12) Uani 1 1 d . . . O1 O 0.85093(19) 1.01943(16) 0.80464(15) 0.0329(6) Uani 1 1 d . . . O2 O 0.75555(15) 0.72317(14) 0.80282(12) 0.0215(4) Uani 1 1 d . . . O3 O 1.04745(15) 0.69807(16) 0.69586(14) 0.0249(5) Uani 1 1 d . . . O5M O 0.1611(3) 0.7335(3) 0.9062(3) 0.0543(12) Uani 0.75 1 d PDU . . O6M O 0.0326(4) 0.7072(5) 0.8790(5) 0.086(2) Uani 0.75 1 d PDU . . O7M O 0.5138(4) 0.5686(3) -0.0341(3) 0.0349(12) Uani 0.50 1 d PDU A -1 O2S O 0.0371(3) 0.8892(2) 0.89450(19) 0.0464(8) Uani 1 1 d . . . O3S O 0.6012(4) 0.0091(5) 0.9566(5) 0.117(3) Uani 1 1 d . . . O1M O 0.4886(3) 0.7186(4) 0.8992(4) 0.106(2) Uani 1 1 d DU . . O3M O 0.3803(3) 0.7815(3) 0.9362(2) 0.0691(12) Uani 1 1 d DU . . N1MA N 0.4523(4) 0.7860(5) 0.9070(5) 0.041(2) Uani 0.626(13) 1 d PDU B 1 O2MA O 0.4832(6) 0.8548(6) 0.8830(6) 0.095(3) Uani 0.626(13) 1 d PDU B 1 N1MB N 0.4561(8) 0.7837(9) 0.9213(10) 0.059(6) Uani 0.374(13) 1 d PDU B 2 O2MB O 0.4910(7) 0.8488(7) 0.9474(7) 0.067(4) Uani 0.374(13) 1 d PDU B 2 N2M N 0.1021(4) 0.6784(4) 0.9031(3) 0.0538(14) Uani 0.75 1 d PDU . . O8M O 0.4885(14) 0.5029(18) 0.0618(4) 0.034(4) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8310(4) 0.082(2) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.0370(12) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.0235(10) Uani 1 4 d SDU . . 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 0.058(3) 0.037(2) 0.085(4) 0.024(3) 0.031(3) 0.015(2) C2 0.049(2) 0.0183(15) 0.043(2) -0.0021(14) 0.0126(18) -0.0015(14) C3 0.0419(19) 0.0265(15) 0.0215(15) -0.0050(12) 0.0028(13) -0.0077(14) C4 0.0296(15) 0.0230(14) 0.0163(13) -0.0044(10) 0.0025(11) -0.0047(11) C5 0.0326(16) 0.0238(14) 0.0273(16) 0.0003(12) -0.0042(13) -0.0056(13) C6 0.0360(17) 0.0254(15) 0.0238(15) -0.0045(12) 0.0086(13) -0.0011(13) C7 0.0232(14) 0.0213(13) 0.0191(13) -0.0027(11) 0.0025(11) -0.0010(11) C8 0.0208(13) 0.0258(14) 0.0180(13) 0.0008(10) -0.0001(10) -0.0003(11) C9 0.0210(13) 0.0236(14) 0.0187(13) 0.0014(10) 0.0022(10) 0.0019(10) C10 0.0237(14) 0.0253(14) 0.0207(14) -0.0027(11) 0.0040(11) -0.0044(11) C11 0.0222(13) 0.0289(15) 0.0186(13) 0.0003(11) -0.0001(11) 0.0037(11) C12 0.0213(13) 0.0246(14) 0.0164(13) 0.0022(10) 0.0006(10) -0.0002(11) N1 0.0449(18) 0.0211(12) 0.0408(19) -0.0030(12) 0.0187(15) 0.0000(11) N2 0.0276(13) 0.0245(13) 0.0252(13) 0.0014(10) -0.0024(11) -0.0034(10) N3 0.0284(13) 0.0241(12) 0.0207(12) -0.0036(10) 0.0049(10) -0.0027(10) N4 0.0258(12) 0.0220(12) 0.0181(11) -0.0017(9) 0.0035(9) -0.0015(10) N5 0.0200(12) 0.0259(13) 0.0210(12) 0.0029(10) 0.0003(9) -0.0021(9) N6 0.0207(12) 0.0334(14) 0.0162(11) 0.0008(10) 0.0010(9) -0.0003(10) N7 0.0236(13) 0.0271(13) 0.0317(15) 0.0086(11) 0.0042(11) -0.0005(10) O4M 0.054(3) 0.049(2) 0.062(3) -0.009(2) -0.014(2) 0.009(2) Ni1 0.0226(2) 0.01887(19) 0.01783(18) -0.00021(14) 0.00324(14) -0.00071(13) O1 0.0437(15) 0.0209(11) 0.0342(14) -0.0004(10) 0.0090(12) -0.0075(10) O2 0.0266(10) 0.0199(10) 0.0179(10) 0.0000(8) 0.0034(8) -0.0023(8) O3 0.0195(10) 0.0278(11) 0.0273(11) 0.0088(9) 0.0020(8) 0.0006(8) O5M 0.053(3) 0.054(3) 0.056(3) -0.016(2) 0.008(2) -0.003(2) O6M 0.067(4) 0.079(4) 0.111(6) 0.019(4) -0.002(4) 0.004(3) O7M 0.050(3) 0.028(2) 0.027(3) 0.000(2) 0.002(2) 0.000(2) O2S 0.060(2) 0.0400(16) 0.0391(16) -0.0003(13) 0.0083(15) -0.0085(14) O3S 0.097(4) 0.106(4) 0.147(7) 0.060(4) 0.074(5) 0.047(4) O1M 0.059(2) 0.124(4) 0.135(4) -0.089(3) -0.028(3) 0.008(2) O3M 0.071(2) 0.088(3) 0.048(2) 0.021(2) 0.0153(18) 0.028(2) N1MA 0.037(3) 0.053(4) 0.034(3) 0.000(2) -0.026(3) 0.007(3) O2MA 0.074(4) 0.112(5) 0.100(6) 0.020(4) 0.020(4) -0.013(4) N1MB 0.058(7) 0.062(7) 0.058(8) 0.002(5) -0.003(5) -0.007(5) O2MB 0.066(5) 0.064(5) 0.069(6) 0.002(4) -0.017(4) -0.005(4) N2M 0.051(3) 0.062(4) 0.049(3) 0.005(3) 0.009(3) 0.007(3) O8M 0.034(10) 0.040(5) 0.027(4) -0.006(6) 0.000(5) -0.005(7) O4S 0.056(3) 0.114(5) 0.076(4) 0.000 0.000 -0.036(4) O1S 0.0409(19) 0.0409(19) 0.029(3) 0.000 0.000 0.000 N3M 0.0229(14) 0.0229(14) 0.025(2) 0.000 0.000 0.000 _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 C2 1.511(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.255(5) . ? C2 N1 1.326(5) . ? C3 N1 1.457(5) . ? C3 C4 1.538(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.538(4) . ? C4 C6 1.545(5) . ? C4 C5 1.552(5) . ? C5 N2 1.478(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.484(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.258(4) . ? C7 N4 1.322(4) . ? C8 N4 1.460(4) . ? C8 C9 1.534(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.514(4) . ? C9 C10 1.538(4) . ? C9 C11 1.558(5) . ? C10 N5 1.485(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N6 1.483(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.250(4) . ? C12 N7 1.324(4) . ? N1 H1 0.8800 . ? N2 Ni1 2.130(3) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 Ni1 2.078(3) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4 0.8800 . ? N5 Ni1 2.081(3) 7_566 ? N5 H5C 0.9200 . ? N5 H5D 0.9200 . ? N6 Ni1 2.093(3) 7_566 ? N6 H6C 0.9200 . ? N6 H6D 0.9200 . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? O4M N2M 1.278(7) . ? Ni1 O3 2.047(2) 8_646 ? Ni1 N5 2.081(3) 8_646 ? Ni1 O2 2.090(2) . ? Ni1 N6 2.094(3) 8_646 ? O3 Ni1 2.047(2) 7_566 ? O5M N2M 1.252(7) . ? O6M N2M 1.255(8) . ? O7M N3M 1.268(5) . ? O1M N1MA 1.195(9) . ? O1M N1MB 1.205(12) . ? O3M N1MB 1.208(13) . ? O3M N1MA 1.251(9) . ? N1MA O2MA 1.258(10) . ? N1MB O2MB 1.251(13) . ? O8M N3M 1.209(9) . ? N3M O8M 1.209(9) 4_655 ? N3M O8M 1.209(9) 2_665 ? N3M O8M 1.209(9) 3_565 ? N3M O7M 1.268(5) 2_665 ? N3M O7M 1.268(5) 3_565 ? N3M O7M 1.268(5) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.7(4) . . ? O1 C2 C1 119.8(4) . . ? N1 C2 C1 117.5(4) . . ? N1 C3 C4 114.1(3) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C3 113.4(3) . . ? C7 C4 C6 108.7(3) . . ? C3 C4 C6 108.6(3) . . ? C7 C4 C5 107.9(3) . . ? C3 C4 C5 106.9(3) . . ? C6 C4 C5 111.3(3) . . ? N2 C5 C4 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.9(3) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 121.8(3) . . ? O2 C7 C4 118.8(3) . . ? N4 C7 C4 119.3(3) . . ? N4 C8 C9 113.2(3) . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C12 C9 C8 114.5(3) . . ? C12 C9 C10 108.5(3) . . ? C8 C9 C10 108.8(3) . . ? C12 C9 C11 109.2(3) . . ? C8 C9 C11 104.7(2) . . ? C10 C9 C11 111.1(3) . . ? N5 C10 C9 114.4(3) . . ? N5 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? N5 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C9 114.6(3) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 119.8(3) . . ? O3 C12 C9 119.8(3) . . ? N7 C12 C9 120.4(3) . . ? C2 N1 C3 124.1(4) . . ? C2 N1 H1 117.9 . . ? C3 N1 H1 117.9 . . ? C5 N2 Ni1 115.8(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 113.1(2) . . ? C6 N3 H3C 109.0 . . ? Ni1 N3 H3C 109.0 . . ? C6 N3 H3D 109.0 . . ? Ni1 N3 H3D 109.0 . . ? H3C N3 H3D 107.8 . . ? C7 N4 C8 123.3(3) . . ? C7 N4 H4 118.4 . . ? C8 N4 H4 118.4 . . ? C10 N5 Ni1 114.8(2) . 7_566 ? C10 N5 H5C 108.6 . . ? Ni1 N5 H5C 108.6 7_566 . ? C10 N5 H5D 108.6 . . ? Ni1 N5 H5D 108.6 7_566 . ? H5C N5 H5D 107.5 . . ? C11 N6 Ni1 115.8(2) . 7_566 ? C11 N6 H6C 108.3 . . ? Ni1 N6 H6C 108.3 7_566 . ? C11 N6 H6D 108.3 . . ? Ni1 N6 H6D 108.3 7_566 . ? H6C N6 H6D 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.87(11) 8_646 . ? O3 Ni1 N5 89.73(11) 8_646 8_646 ? N3 Ni1 N5 94.08(11) . 8_646 ? O3 Ni1 O2 85.72(9) 8_646 . ? N3 Ni1 O2 90.52(10) . . ? N5 Ni1 O2 95.09(10) 8_646 . ? O3 Ni1 N6 85.07(10) 8_646 8_646 ? N3 Ni1 N6 98.55(11) . 8_646 ? N5 Ni1 N6 86.93(11) 8_646 8_646 ? O2 Ni1 N6 170.56(10) . 8_646 ? O3 Ni1 N2 91.02(12) 8_646 . ? N3 Ni1 N2 85.12(12) . . ? N5 Ni1 N2 178.83(12) 8_646 . ? O2 Ni1 N2 84.07(10) . . ? N6 Ni1 N2 94.03(11) 8_646 . ? C7 O2 Ni1 119.4(2) . . ? C12 O3 Ni1 121.3(2) . 7_566 ? O1M N1MA O3M 115.3(7) . . ? O1M N1MA O2MA 120.9(8) . . ? O3M N1MA O2MA 123.6(7) . . ? O1M N1MB O3M 117.8(11) . . ? O1M N1MB O2MB 129.5(13) . . ? O3M N1MB O2MB 110.3(11) . . ? O5M N2M O6M 113.7(6) . . ? O5M N2M O4M 127.1(6) . . ? O6M N2M O4M 119.2(6) . . ? O8M N3M O8M 167.7(15) . 4_655 ? O8M N3M O8M 167.7(15) 4_655 2_665 ? O8M N3M O8M 167.7(15) . 3_565 ? O8M N3M O8M 167.7(15) 2_665 3_565 ? O8M N3M O7M 120.5(13) . . ? O8M N3M O7M 67.4(10) 4_655 . ? O8M N3M O7M 121.4(14) 2_665 . ? O8M N3M O7M 50.0(11) 3_565 . ? O8M N3M O7M 121.4(14) . 2_665 ? O8M N3M O7M 50.0(11) 4_655 2_665 ? O8M N3M O7M 120.5(13) 2_665 2_665 ? O8M N3M O7M 67.4(10) 3_565 2_665 ? O7M N3M O7M 117.4(5) . 2_665 ? O8M N3M O7M 67.4(10) . 3_565 ? O8M N3M O7M 121.4(14) 4_655 3_565 ? O8M N3M O7M 50.0(11) 2_665 3_565 ? O8M N3M O7M 120.5(13) 3_565 3_565 ? O7M N3M O7M 105.7(2) . 3_565 ? O7M N3M O7M 105.7(2) 2_665 3_565 ? O8M N3M O7M 50.0(11) . 4_655 ? O8M N3M O7M 120.5(13) 4_655 4_655 ? O8M N3M O7M 67.4(10) 2_665 4_655 ? O8M N3M O7M 121.4(14) 3_565 4_655 ? O7M N3M O7M 105.7(2) . 4_655 ? O7M N3M O7M 105.7(2) 2_665 4_655 ? O7M N3M O7M 117.4(5) 3_565 4_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.611 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.116 #===END data_i-4_123K _database_code_depnum_ccdc_archive 'CCDC 856058' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.5024(7) _cell_length_b 15.5024(7) _cell_length_c 19.3585(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4652.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 8478 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.74 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8683 _exptl_absorpt_correction_T_max 0.9146 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17533 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6711 _reflns_number_gt 6176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.0963P)^2^+3.0183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.088(15) _refine_ls_number_reflns 6711 _refine_ls_number_parameters 345 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.199 _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 0.7130(4) 1.0888(3) 0.8056(4) 0.0634(17) Uani 1 1 d . . . H1A H 0.6855 1.0670 0.7635 0.095 Uiso 1 1 calc R . . H1B H 0.7426 1.1432 0.7953 0.095 Uiso 1 1 calc R . . H1C H 0.6689 1.0988 0.8410 0.095 Uiso 1 1 calc R . . C2 C 0.7776(3) 1.0234(2) 0.8316(2) 0.0386(9) Uani 1 1 d . . . C3 C 0.8093(3) 0.9089(2) 0.91576(19) 0.0315(7) Uani 1 1 d . . . H3A H 0.8077 0.9182 0.9663 0.038 Uiso 1 1 calc R . . H3B H 0.8692 0.9193 0.9000 0.038 Uiso 1 1 calc R . . C4 C 0.7854(2) 0.8146(2) 0.90048(17) 0.0243(6) Uani 1 1 d . . . C5 C 0.8506(2) 0.7573(2) 0.94067(19) 0.0300(7) Uani 1 1 d . . . H5A H 0.9094 0.7807 0.9339 0.036 Uiso 1 1 calc R . . H5B H 0.8372 0.7605 0.9906 0.036 Uiso 1 1 calc R . . C6 C 0.6917(2) 0.7982(2) 0.92516(19) 0.0292(7) Uani 1 1 d . . . H6A H 0.6813 0.8321 0.9677 0.035 Uiso 1 1 calc R . . H6B H 0.6514 0.8194 0.8893 0.035 Uiso 1 1 calc R . . C7 C 0.7917(2) 0.7909(2) 0.82375(16) 0.0224(6) Uani 1 1 d . . . C8 C 0.8446(2) 0.8252(2) 0.70781(16) 0.0233(6) Uani 1 1 d . . . H8A H 0.8239 0.8772 0.6831 0.028 Uiso 1 1 calc R . . H8B H 0.8064 0.7766 0.6950 0.028 Uiso 1 1 calc R . . C9 C 0.93690(19) 0.8047(2) 0.68374(16) 0.0217(5) Uani 1 1 d . . . C10 C 0.9978(2) 0.8753(2) 0.71097(17) 0.0249(6) Uani 1 1 d . . . H10A H 0.9682 0.9317 0.7074 0.030 Uiso 1 1 calc R . . H10B H 1.0092 0.8643 0.7605 0.030 Uiso 1 1 calc R . . C11 C 0.9317(2) 0.8071(2) 0.60343(17) 0.0248(6) Uani 1 1 d . . . H11A H 0.8813 0.7727 0.5885 0.030 Uiso 1 1 calc R . . H11B H 0.9220 0.8674 0.5886 0.030 Uiso 1 1 calc R . . C12 C 0.9705(2) 0.7179(2) 0.70673(16) 0.0218(6) Uani 1 1 d . . . N1 N 0.7523(2) 0.97170(19) 0.88262(19) 0.0367(7) Uani 1 1 d . . . H1 H 0.6987 0.9755 0.8971 0.044 Uiso 1 1 calc R . . N2 N 0.84956(19) 0.66591(19) 0.91894(17) 0.0277(6) Uani 1 1 d . . . H2A H 0.8603 0.6322 0.9571 0.033 Uiso 1 1 calc R . . H2B H 0.8941 0.6573 0.8883 0.033 Uiso 1 1 calc R . . N3 N 0.67248(19) 0.70637(19) 0.93947(15) 0.0259(5) Uani 1 1 d . . . H3C H 0.6138 0.6980 0.9366 0.031 Uiso 1 1 calc R . . H3D H 0.6892 0.6937 0.9839 0.031 Uiso 1 1 calc R . . N4 N 0.83794(18) 0.84008(18) 0.78195(14) 0.0234(5) Uani 1 1 d . . . H4 H 0.8661 0.8840 0.7998 0.028 Uiso 1 1 calc R . . N5 N 1.08148(18) 0.88096(18) 0.67415(15) 0.0238(5) Uani 1 1 d . . . H5C H 1.1231 0.8984 0.7050 0.029 Uiso 1 1 calc R . . H5D H 1.0772 0.9228 0.6406 0.029 Uiso 1 1 calc R . . N6 N 1.00976(18) 0.7735(2) 0.56794(14) 0.0247(5) Uani 1 1 d . . . H6C H 1.0208 0.8081 0.5303 0.030 Uiso 1 1 calc R . . H6D H 0.9976 0.7191 0.5516 0.030 Uiso 1 1 calc R . . N7 N 0.91902(19) 0.66289(19) 0.73921(17) 0.0289(6) Uani 1 1 d . . . H7A H 0.9391 0.6127 0.7531 0.035 Uiso 1 1 calc R . . H7B H 0.8647 0.6765 0.7468 0.035 Uiso 1 1 calc R . . O4M O 0.1057(4) 0.5998(3) 0.9221(3) 0.0611(13) Uani 0.75 1 d PDU . . Ni1 Ni 0.73348(2) 0.62198(2) 0.872093(19) 0.02093(11) Uani 1 1 d . . . O1 O 0.85076(19) 1.01920(17) 0.80474(15) 0.0353(6) Uani 1 1 d . . . O2 O 0.75549(15) 0.72298(14) 0.80282(12) 0.0230(4) Uani 1 1 d . . . O3 O 1.04744(15) 0.69836(16) 0.69599(13) 0.0265(5) Uani 1 1 d . . . O5M O 0.1605(4) 0.7335(3) 0.9061(3) 0.0610(13) Uani 0.75 1 d PDU . . O6M O 0.0333(4) 0.7066(5) 0.8779(5) 0.094(2) Uani 0.75 1 d PDU . . O7M O 0.5144(4) 0.5684(4) -0.0341(3) 0.0375(12) Uani 0.50 1 d PDU A -1 O2S O 0.0373(3) 0.8890(2) 0.89445(19) 0.0512(8) Uani 1 1 d . . . O3S O 0.6018(4) 0.0086(5) 0.9562(4) 0.117(3) Uani 1 1 d . . . O1M O 0.4883(3) 0.7187(4) 0.8987(4) 0.109(2) Uani 1 1 d DU . . O3M O 0.3799(3) 0.7810(3) 0.9361(2) 0.0751(13) Uani 1 1 d DU . . N1MA N 0.4523(4) 0.7854(4) 0.9083(4) 0.0420(18) Uani 0.672(12) 1 d PDU B 1 O2MA O 0.4825(7) 0.8522(7) 0.8802(6) 0.118(4) Uani 0.672(12) 1 d PDU B 1 N1MB N 0.4558(9) 0.7829(10) 0.9224(11) 0.080(9) Uani 0.328(12) 1 d PDU B 2 O2MB O 0.4910(7) 0.8485(7) 0.9457(7) 0.059(4) Uani 0.328(12) 1 d PDU B 2 N2M N 0.1018(4) 0.6785(4) 0.9030(3) 0.0609(16) Uani 0.75 1 d PDU . . O8M O 0.4876(12) 0.5047(16) 0.0619(4) 0.038(4) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8309(4) 0.088(2) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.0409(13) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.0253(10) Uani 1 4 d SDU . . 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 0.059(3) 0.040(2) 0.091(4) 0.025(3) 0.031(3) 0.017(2) C2 0.050(2) 0.0204(15) 0.045(2) -0.0025(14) 0.0109(18) -0.0005(15) C3 0.045(2) 0.0259(15) 0.0237(15) -0.0064(12) 0.0035(14) -0.0082(14) C4 0.0302(15) 0.0232(14) 0.0195(13) -0.0034(11) 0.0031(11) -0.0040(11) C5 0.0359(17) 0.0256(15) 0.0286(16) 0.0009(12) -0.0047(13) -0.0061(13) C6 0.0363(17) 0.0258(15) 0.0255(15) -0.0038(12) 0.0083(13) -0.0009(13) C7 0.0244(14) 0.0225(13) 0.0205(13) -0.0020(11) 0.0027(11) -0.0003(11) C8 0.0228(13) 0.0280(14) 0.0192(13) 0.0014(11) 0.0007(10) 0.0013(11) C9 0.0211(13) 0.0238(13) 0.0200(13) 0.0018(10) 0.0030(10) 0.0020(10) C10 0.0247(14) 0.0267(14) 0.0231(14) -0.0031(12) 0.0031(11) -0.0042(11) C11 0.0235(14) 0.0305(15) 0.0202(13) 0.0012(11) 0.0000(11) 0.0031(11) C12 0.0225(13) 0.0247(13) 0.0182(13) 0.0019(10) -0.0004(10) -0.0008(10) N1 0.0463(18) 0.0222(12) 0.0415(19) -0.0032(12) 0.0194(15) 0.0004(11) N2 0.0286(14) 0.0252(13) 0.0294(14) 0.0014(11) -0.0021(11) -0.0013(10) N3 0.0291(13) 0.0255(13) 0.0230(12) -0.0042(10) 0.0053(10) -0.0035(10) N4 0.0274(13) 0.0231(12) 0.0198(11) -0.0018(9) 0.0038(10) -0.0013(10) N5 0.0222(12) 0.0258(12) 0.0234(12) 0.0028(10) 0.0005(10) -0.0030(10) N6 0.0227(12) 0.0345(14) 0.0170(11) 0.0007(10) 0.0018(9) -0.0008(10) N7 0.0247(13) 0.0269(13) 0.0349(15) 0.0082(11) 0.0055(11) 0.0002(10) O4M 0.060(3) 0.057(3) 0.066(3) -0.011(2) -0.012(2) 0.010(2) Ni1 0.02344(19) 0.01983(18) 0.01951(17) -0.00038(14) 0.00336(14) -0.00078(14) O1 0.0446(15) 0.0236(12) 0.0377(14) 0.0003(10) 0.0110(12) -0.0072(10) O2 0.0271(10) 0.0212(10) 0.0208(10) -0.0003(8) 0.0031(8) -0.0020(8) O3 0.0207(10) 0.0290(11) 0.0297(11) 0.0099(9) 0.0031(9) -0.0001(8) O5M 0.061(3) 0.056(3) 0.066(3) -0.015(2) 0.007(2) -0.002(2) O6M 0.072(4) 0.091(4) 0.118(6) 0.016(5) 0.004(4) 0.006(3) O7M 0.055(3) 0.029(3) 0.028(3) 0.002(2) 0.004(2) -0.002(2) O2S 0.065(2) 0.0447(17) 0.0436(17) -0.0020(14) 0.0085(16) -0.0105(15) O3S 0.096(4) 0.106(4) 0.147(6) 0.051(4) 0.073(4) 0.042(3) O1M 0.063(3) 0.126(4) 0.139(4) -0.089(3) -0.030(3) 0.011(3) O3M 0.076(3) 0.096(3) 0.053(2) 0.020(2) 0.014(2) 0.029(2) N1MA 0.039(3) 0.049(3) 0.038(3) -0.001(2) -0.025(2) 0.007(2) O2MA 0.096(5) 0.133(6) 0.125(6) 0.023(5) 0.018(4) -0.012(4) N1MB 0.080(10) 0.081(10) 0.079(10) 0.004(5) -0.003(5) -0.006(5) O2MB 0.061(5) 0.053(5) 0.063(6) -0.002(4) -0.018(4) -0.006(4) N2M 0.055(3) 0.072(4) 0.056(3) 0.005(3) 0.009(3) 0.013(3) O8M 0.041(10) 0.044(6) 0.031(4) -0.010(6) 0.002(5) -0.002(7) O4S 0.058(4) 0.122(6) 0.085(5) 0.000 0.000 -0.034(4) O1S 0.045(2) 0.045(2) 0.032(3) 0.000 0.000 0.000 N3M 0.0248(15) 0.0248(15) 0.026(3) 0.000 0.000 0.000 _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 C2 1.513(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.249(5) . ? C2 N1 1.330(5) . ? C3 N1 1.463(5) . ? C3 C4 1.537(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.533(4) . ? C4 C6 1.549(5) . ? C4 C5 1.555(5) . ? C5 N2 1.478(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.481(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.260(4) . ? C7 N4 1.323(4) . ? C8 N4 1.457(4) . ? C8 C9 1.537(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.510(4) . ? C9 C10 1.538(4) . ? C9 C11 1.557(5) . ? C10 N5 1.483(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N6 1.485(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.248(4) . ? C12 N7 1.327(4) . ? N1 H1 0.8800 . ? N2 Ni1 2.127(3) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 Ni1 2.075(3) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4 0.8800 . ? N5 Ni1 2.084(3) 7_566 ? N5 H5C 0.9200 . ? N5 H5D 0.9200 . ? N6 Ni1 2.094(3) 7_566 ? N6 H6C 0.9200 . ? N6 H6D 0.9200 . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? O4M N2M 1.277(8) . ? Ni1 O3 2.047(2) 8_646 ? Ni1 N5 2.084(3) 8_646 ? Ni1 O2 2.090(2) . ? Ni1 N6 2.094(3) 8_646 ? O3 Ni1 2.047(2) 7_566 ? O5M N2M 1.247(8) . ? O6M N2M 1.247(8) . ? O7M N3M 1.268(5) . ? O1M N1MA 1.189(8) . ? O1M N1MB 1.206(13) . ? O3M N1MB 1.207(13) . ? O3M N1MA 1.246(8) . ? N1MA O2MA 1.261(10) . ? N1MB O2MB 1.238(13) . ? O8M N3M 1.215(9) . ? N3M O8M 1.215(9) 4_655 ? N3M O8M 1.215(9) 2_665 ? N3M O8M 1.215(9) 3_565 ? N3M O7M 1.268(5) 2_665 ? N3M O7M 1.268(5) 3_565 ? N3M O7M 1.268(5) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 123.1(4) . . ? O1 C2 C1 119.8(4) . . ? N1 C2 C1 117.1(4) . . ? N1 C3 C4 113.8(3) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C7 113.5(3) . . ? C3 C4 C6 108.8(3) . . ? C7 C4 C6 108.6(3) . . ? C3 C4 C5 106.9(3) . . ? C7 C4 C5 107.8(3) . . ? C6 C4 C5 111.2(3) . . ? N2 C5 C4 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.8(3) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 121.7(3) . . ? O2 C7 C4 118.9(3) . . ? N4 C7 C4 119.3(3) . . ? N4 C8 C9 113.4(3) . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C12 C9 C8 114.6(3) . . ? C12 C9 C10 108.7(3) . . ? C8 C9 C10 108.7(3) . . ? C12 C9 C11 109.4(3) . . ? C8 C9 C11 104.5(2) . . ? C10 C9 C11 110.9(3) . . ? N5 C10 C9 114.5(3) . . ? N5 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? N5 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C9 114.3(3) . . ? N6 C11 H11A 108.7 . . ? C9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? C9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 119.8(3) . . ? O3 C12 C9 119.8(3) . . ? N7 C12 C9 120.3(3) . . ? C2 N1 C3 123.2(4) . . ? C2 N1 H1 118.4 . . ? C3 N1 H1 118.4 . . ? C5 N2 Ni1 115.9(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 113.4(2) . . ? C6 N3 H3C 108.9 . . ? Ni1 N3 H3C 108.9 . . ? C6 N3 H3D 108.9 . . ? Ni1 N3 H3D 108.9 . . ? H3C N3 H3D 107.7 . . ? C7 N4 C8 123.4(3) . . ? C7 N4 H4 118.3 . . ? C8 N4 H4 118.3 . . ? C10 N5 Ni1 114.8(2) . 7_566 ? C10 N5 H5C 108.6 . . ? Ni1 N5 H5C 108.6 7_566 . ? C10 N5 H5D 108.6 . . ? Ni1 N5 H5D 108.6 7_566 . ? H5C N5 H5D 107.5 . . ? C11 N6 Ni1 116.0(2) . 7_566 ? C11 N6 H6C 108.3 . . ? Ni1 N6 H6C 108.3 7_566 . ? C11 N6 H6D 108.3 . . ? Ni1 N6 H6D 108.3 7_566 . ? H6C N6 H6D 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.79(11) 8_646 . ? O3 Ni1 N5 89.59(11) 8_646 8_646 ? N3 Ni1 N5 94.13(11) . 8_646 ? O3 Ni1 O2 85.73(9) 8_646 . ? N3 Ni1 O2 90.31(10) . . ? N5 Ni1 O2 95.11(10) 8_646 . ? O3 Ni1 N6 85.11(10) 8_646 8_646 ? N3 Ni1 N6 98.73(11) . 8_646 ? N5 Ni1 N6 86.78(12) 8_646 8_646 ? O2 Ni1 N6 170.63(10) . 8_646 ? O3 Ni1 N2 91.06(12) 8_646 . ? N3 Ni1 N2 85.16(12) . . ? N5 Ni1 N2 178.86(12) 8_646 . ? O2 Ni1 N2 84.00(10) . . ? N6 Ni1 N2 94.21(11) 8_646 . ? C7 O2 Ni1 119.5(2) . . ? C12 O3 Ni1 121.4(2) . 7_566 ? O1M N1MA O3M 116.3(7) . . ? O1M N1MA O2MA 118.1(8) . . ? O3M N1MA O2MA 124.5(7) . . ? O1M N1MB O3M 118.1(12) . . ? O1M N1MB O2MB 129.2(13) . . ? O3M N1MB O2MB 111.6(12) . . ? O5M N2M O6M 113.7(7) . . ? O5M N2M O4M 127.2(6) . . ? O6M N2M O4M 119.1(7) . . ? O8M N3M O8M 166.3(13) . 4_655 ? O8M N3M O8M 166.3(13) 4_655 2_665 ? O8M N3M O8M 166.3(13) . 3_565 ? O8M N3M O8M 166.3(13) 2_665 3_565 ? O8M N3M O7M 119.4(12) . . ? O8M N3M O7M 68.3(9) 4_655 . ? O8M N3M O7M 122.3(12) 2_665 . ? O8M N3M O7M 49.1(9) 3_565 . ? O8M N3M O7M 122.3(12) . 2_665 ? O8M N3M O7M 49.1(9) 4_655 2_665 ? O8M N3M O7M 119.4(12) 2_665 2_665 ? O8M N3M O7M 68.3(9) 3_565 2_665 ? O7M N3M O7M 117.3(5) . 2_665 ? O8M N3M O7M 68.3(9) . 3_565 ? O8M N3M O7M 122.3(12) 4_655 3_565 ? O8M N3M O7M 49.1(9) 2_665 3_565 ? O8M N3M O7M 119.4(12) 3_565 3_565 ? O7M N3M O7M 105.7(2) . 3_565 ? O7M N3M O7M 105.7(2) 2_665 3_565 ? O8M N3M O7M 49.1(9) . 4_655 ? O8M N3M O7M 119.4(12) 4_655 4_655 ? O8M N3M O7M 68.3(9) 2_665 4_655 ? O8M N3M O7M 122.3(12) 3_565 4_655 ? O7M N3M O7M 105.7(2) . 4_655 ? O7M N3M O7M 105.7(2) 2_665 4_655 ? O7M N3M O7M 117.3(5) 3_565 4_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.494 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.109 #===END data_i-4_173K _database_code_depnum_ccdc_archive 'CCDC 856059' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.5252(6) _cell_length_b 15.5252(6) _cell_length_c 19.3983(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4675.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8710 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 30.69 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8689 _exptl_absorpt_correction_T_max 0.9150 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17695 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6755 _reflns_number_gt 6254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.0963P)^2^+0.8972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.089(14) _refine_ls_number_reflns 6755 _refine_ls_number_parameters 345 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.200 _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 0.7128(4) 1.0892(3) 0.8065(4) 0.0686(17) Uani 1 1 d . . . H1A H 0.6849 1.0677 0.7646 0.103 Uiso 1 1 calc R . . H1B H 0.7423 1.1435 0.7964 0.103 Uiso 1 1 calc R . . H1C H 0.6692 1.0988 0.8422 0.103 Uiso 1 1 calc R . . C2 C 0.7780(3) 1.0232(2) 0.8319(2) 0.0409(8) Uani 1 1 d . . . C3 C 0.8089(2) 0.9084(2) 0.91568(17) 0.0322(6) Uani 1 1 d . . . H3A H 0.8069 0.9176 0.9662 0.039 Uiso 1 1 calc R . . H3B H 0.8688 0.9188 0.9004 0.039 Uiso 1 1 calc R . . C4 C 0.7852(2) 0.81409(19) 0.90033(15) 0.0246(5) Uani 1 1 d . . . C5 C 0.8503(2) 0.7574(2) 0.94010(17) 0.0307(6) Uani 1 1 d . . . H5A H 0.9090 0.7807 0.9329 0.037 Uiso 1 1 calc R . . H5B H 0.8375 0.7611 0.9900 0.037 Uiso 1 1 calc R . . C6 C 0.6920(2) 0.7984(2) 0.92479(17) 0.0306(6) Uani 1 1 d . . . H6A H 0.6819 0.8321 0.9674 0.037 Uiso 1 1 calc R . . H6B H 0.6518 0.8201 0.8891 0.037 Uiso 1 1 calc R . . C7 C 0.79155(18) 0.79057(18) 0.82364(15) 0.0232(5) Uani 1 1 d . . . C8 C 0.84495(19) 0.8249(2) 0.70804(15) 0.0248(5) Uani 1 1 d . . . H8A H 0.8242 0.8768 0.6834 0.030 Uiso 1 1 calc R . . H8B H 0.8069 0.7763 0.6952 0.030 Uiso 1 1 calc R . . C9 C 0.93696(18) 0.80469(19) 0.68401(14) 0.0225(5) Uani 1 1 d . . . C10 C 0.99754(19) 0.87488(19) 0.71114(16) 0.0259(5) Uani 1 1 d . . . H10A H 0.9680 0.9312 0.7075 0.031 Uiso 1 1 calc R . . H10B H 1.0087 0.8640 0.7606 0.031 Uiso 1 1 calc R . . C11 C 0.93197(19) 0.8068(2) 0.60388(15) 0.0270(6) Uani 1 1 d . . . H11A H 0.8818 0.7722 0.5890 0.032 Uiso 1 1 calc R . . H11B H 0.9218 0.8670 0.5890 0.032 Uiso 1 1 calc R . . C12 C 0.97059(18) 0.71800(18) 0.70696(14) 0.0228(5) Uani 1 1 d . . . N1 N 0.7529(2) 0.97133(18) 0.88265(18) 0.0383(7) Uani 1 1 d . . . H1 H 0.6993 0.9753 0.8971 0.046 Uiso 1 1 calc R . . N2 N 0.84905(18) 0.66596(17) 0.91893(15) 0.0294(5) Uani 1 1 d . . . H2A H 0.8594 0.6326 0.9573 0.035 Uiso 1 1 calc R . . H2B H 0.8937 0.6569 0.8886 0.035 Uiso 1 1 calc R . . N3 N 0.67205(18) 0.70670(17) 0.93869(14) 0.0273(5) Uani 1 1 d . . . H3C H 0.6135 0.6987 0.9354 0.033 Uiso 1 1 calc R . . H3D H 0.6882 0.6938 0.9831 0.033 Uiso 1 1 calc R . . N4 N 0.83805(17) 0.83968(16) 0.78202(13) 0.0249(5) Uani 1 1 d . . . H4 H 0.8662 0.8835 0.8000 0.030 Uiso 1 1 calc R . . N5 N 1.08124(17) 0.88070(16) 0.67476(14) 0.0252(5) Uani 1 1 d . . . H5C H 1.1226 0.8979 0.7058 0.030 Uiso 1 1 calc R . . H5D H 1.0772 0.9227 0.6415 0.030 Uiso 1 1 calc R . . N6 N 1.00988(16) 0.77392(18) 0.56839(13) 0.0269(5) Uani 1 1 d . . . H6C H 1.0208 0.8088 0.5311 0.032 Uiso 1 1 calc R . . H6D H 0.9979 0.7197 0.5517 0.032 Uiso 1 1 calc R . . N7 N 0.91969(17) 0.66315(18) 0.73960(16) 0.0306(5) Uani 1 1 d . . . H7A H 0.9400 0.6131 0.7535 0.037 Uiso 1 1 calc R . . H7B H 0.8655 0.6767 0.7475 0.037 Uiso 1 1 calc R . . O4M O 0.1067(4) 0.5991(3) 0.9211(3) 0.0674(13) Uani 0.75 1 d PDU . . Ni1 Ni 0.73321(2) 0.62204(2) 0.871773(17) 0.02184(10) Uani 1 1 d . . . O1 O 0.85078(18) 1.01876(16) 0.80497(15) 0.0387(6) Uani 1 1 d . . . O2 O 0.75568(14) 0.72287(13) 0.80264(10) 0.0240(4) Uani 1 1 d . . . O3 O 1.04759(14) 0.69830(14) 0.69598(12) 0.0278(4) Uani 1 1 d . . . O5M O 0.1595(4) 0.7320(3) 0.9068(3) 0.0743(15) Uani 0.75 1 d PDU . . O6M O 0.0329(5) 0.7054(5) 0.8790(5) 0.108(2) Uani 0.75 1 d PDU . . O7M O 0.5161(4) 0.5678(4) -0.0340(3) 0.0455(13) Uani 0.50 1 d PDU A -1 O2S O 0.0378(3) 0.8891(2) 0.89521(19) 0.0590(9) Uani 1 1 d . . . O3S O 0.6027(4) 0.0091(4) 0.9573(4) 0.113(2) Uani 1 1 d . . . O1M O 0.4879(3) 0.7182(4) 0.8984(3) 0.1133(19) Uani 1 1 d DU . . O3M O 0.3790(3) 0.7800(3) 0.9364(2) 0.0821(13) Uani 1 1 d DU . . N1MA N 0.4516(3) 0.7844(4) 0.9092(4) 0.0399(16) Uani 0.644(12) 1 d PDU B 1 O2MA O 0.4823(7) 0.8509(6) 0.8822(7) 0.125(4) Uani 0.644(12) 1 d PDU B 1 N1MB N 0.4548(9) 0.7817(10) 0.9224(11) 0.090(9) Uani 0.356(12) 1 d PDU B 2 O2MB O 0.4898(6) 0.8477(6) 0.9453(6) 0.061(3) Uani 0.356(12) 1 d PDU B 2 N2M N 0.1017(4) 0.6778(4) 0.9030(3) 0.0651(15) Uani 0.75 1 d PDU . . O8M O 0.4888(16) 0.5047(17) 0.0613(5) 0.050(4) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8302(4) 0.094(2) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.0482(13) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.0296(10) Uani 1 4 d SDU . . 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 0.064(3) 0.045(2) 0.097(4) 0.028(3) 0.029(3) 0.019(2) C2 0.053(2) 0.0205(14) 0.049(2) -0.0006(13) 0.0127(17) 0.0013(14) C3 0.0435(18) 0.0265(14) 0.0264(14) -0.0059(11) 0.0031(12) -0.0066(12) C4 0.0305(14) 0.0234(13) 0.0198(12) -0.0046(9) 0.0030(10) -0.0035(10) C5 0.0358(15) 0.0264(14) 0.0298(14) -0.0003(11) -0.0053(12) -0.0044(12) C6 0.0365(15) 0.0256(13) 0.0296(15) -0.0038(11) 0.0108(12) -0.0001(12) C7 0.0241(13) 0.0226(12) 0.0230(12) -0.0021(10) 0.0026(10) 0.0000(10) C8 0.0228(12) 0.0301(13) 0.0216(12) 0.0015(10) 0.0020(10) 0.0024(10) C9 0.0217(12) 0.0257(12) 0.0201(12) 0.0019(9) 0.0029(9) 0.0014(9) C10 0.0244(12) 0.0267(13) 0.0265(13) -0.0028(11) 0.0037(10) -0.0025(10) C11 0.0220(12) 0.0367(15) 0.0222(12) 0.0021(11) 0.0005(10) 0.0033(11) C12 0.0232(12) 0.0250(12) 0.0201(12) 0.0005(9) 0.0008(9) 0.0005(10) N1 0.0455(16) 0.0233(12) 0.0461(18) -0.0027(11) 0.0199(13) 0.0014(10) N2 0.0306(13) 0.0259(12) 0.0318(13) 0.0018(10) -0.0028(10) -0.0018(10) N3 0.0314(12) 0.0252(11) 0.0253(11) -0.0038(9) 0.0066(9) -0.0038(10) N4 0.0275(12) 0.0246(11) 0.0227(11) -0.0016(9) 0.0039(9) -0.0015(9) N5 0.0228(11) 0.0268(11) 0.0262(11) 0.0032(9) 0.0005(9) -0.0038(9) N6 0.0237(11) 0.0381(14) 0.0191(10) -0.0007(9) 0.0013(9) -0.0004(10) N7 0.0252(12) 0.0277(12) 0.0388(14) 0.0079(11) 0.0069(10) 0.0004(9) O4M 0.071(3) 0.058(3) 0.073(3) -0.010(2) -0.008(3) 0.009(2) Ni1 0.02420(18) 0.01996(17) 0.02137(16) -0.00084(13) 0.00306(13) -0.00053(12) O1 0.0478(15) 0.0254(11) 0.0429(14) 0.0025(10) 0.0133(12) -0.0063(10) O2 0.0286(10) 0.0223(9) 0.0212(9) -0.0004(7) 0.0031(7) -0.0024(7) O3 0.0213(9) 0.0288(10) 0.0334(11) 0.0094(9) 0.0032(8) 0.0009(8) O5M 0.079(3) 0.058(3) 0.086(4) -0.013(3) 0.006(3) -0.003(3) O6M 0.078(4) 0.106(5) 0.139(6) 0.021(5) 0.002(4) 0.008(3) O7M 0.066(3) 0.036(3) 0.034(3) 0.001(2) 0.002(2) -0.003(2) O2S 0.072(2) 0.0508(18) 0.0539(19) -0.0002(15) 0.0109(17) -0.0098(16) O3S 0.092(4) 0.101(4) 0.146(6) 0.041(4) 0.067(4) 0.033(3) O1M 0.064(2) 0.130(4) 0.146(4) -0.088(3) -0.028(3) 0.012(2) O3M 0.080(3) 0.103(3) 0.063(2) 0.017(2) 0.018(2) 0.028(2) N1MA 0.035(3) 0.046(3) 0.038(3) -0.002(2) -0.022(2) 0.004(2) O2MA 0.102(5) 0.141(6) 0.132(6) 0.021(5) 0.016(4) -0.009(4) N1MB 0.089(10) 0.091(10) 0.091(10) 0.001(5) -0.004(5) -0.008(5) O2MB 0.065(5) 0.054(5) 0.065(5) -0.001(4) -0.019(4) -0.005(4) N2M 0.056(3) 0.080(4) 0.059(3) 0.003(3) 0.008(3) 0.014(3) O8M 0.053(10) 0.053(6) 0.043(4) -0.012(7) -0.002(6) -0.010(7) O4S 0.056(3) 0.136(6) 0.091(4) 0.000 0.000 -0.022(4) O1S 0.054(2) 0.054(2) 0.037(3) 0.000 0.000 0.000 N3M 0.0303(15) 0.0303(15) 0.028(2) 0.000 0.000 0.000 _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 C2 1.522(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.246(5) . ? C2 N1 1.330(5) . ? C3 N1 1.457(5) . ? C3 C4 1.539(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.535(4) . ? C4 C6 1.543(4) . ? C4 C5 1.546(5) . ? C5 N2 1.479(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.482(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.257(4) . ? C7 N4 1.324(4) . ? C8 N4 1.457(4) . ? C8 C9 1.535(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.511(4) . ? C9 C10 1.533(4) . ? C9 C11 1.557(4) . ? C10 N5 1.481(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N6 1.483(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.252(4) . ? C12 N7 1.323(4) . ? N1 H1 0.8800 . ? N2 Ni1 2.130(3) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 Ni1 2.077(3) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4 0.8800 . ? N5 Ni1 2.084(3) 7_566 ? N5 H5C 0.9200 . ? N5 H5D 0.9200 . ? N6 Ni1 2.096(3) 7_566 ? N6 H6C 0.9200 . ? N6 H6D 0.9200 . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? O4M N2M 1.275(7) . ? Ni1 O3 2.048(2) 8_646 ? Ni1 N5 2.084(3) 8_646 ? Ni1 O2 2.091(2) . ? Ni1 N6 2.096(3) 8_646 ? O3 Ni1 2.048(2) 7_566 ? O5M N2M 1.232(8) . ? O6M N2M 1.242(8) . ? O7M N3M 1.266(5) . ? O1M N1MA 1.192(7) . ? O1M N1MB 1.207(12) . ? O3M N1MB 1.208(13) . ? O3M N1MA 1.246(7) . ? N1MA O2MA 1.252(9) . ? N1MB O2MB 1.241(13) . ? O8M N3M 1.204(9) . ? N3M O8M 1.204(9) 4_655 ? N3M O8M 1.204(9) 2_665 ? N3M O8M 1.204(9) 3_565 ? N3M O7M 1.266(5) 2_665 ? N3M O7M 1.266(5) 3_565 ? N3M O7M 1.266(5) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.9(4) . . ? O1 C2 C1 120.3(4) . . ? N1 C2 C1 116.8(4) . . ? N1 C3 C4 114.2(3) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C3 113.5(2) . . ? C7 C4 C6 108.7(3) . . ? C3 C4 C6 108.3(2) . . ? C7 C4 C5 107.8(2) . . ? C3 C4 C5 106.8(3) . . ? C6 C4 C5 111.7(3) . . ? N2 C5 C4 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.8(2) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 121.7(3) . . ? O2 C7 C4 119.0(3) . . ? N4 C7 C4 119.3(3) . . ? N4 C8 C9 113.6(2) . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C12 C9 C10 108.7(2) . . ? C12 C9 C8 114.5(2) . . ? C10 C9 C8 108.7(2) . . ? C12 C9 C11 109.3(2) . . ? C10 C9 C11 111.0(2) . . ? C8 C9 C11 104.6(2) . . ? N5 C10 C9 114.7(2) . . ? N5 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? N5 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C9 114.6(2) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 119.6(3) . . ? O3 C12 C9 119.8(2) . . ? N7 C12 C9 120.5(3) . . ? C2 N1 C3 123.8(3) . . ? C2 N1 H1 118.1 . . ? C3 N1 H1 118.1 . . ? C5 N2 Ni1 116.0(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 113.51(18) . . ? C6 N3 H3C 108.9 . . ? Ni1 N3 H3C 108.9 . . ? C6 N3 H3D 108.9 . . ? Ni1 N3 H3D 108.9 . . ? H3C N3 H3D 107.7 . . ? C7 N4 C8 123.4(3) . . ? C7 N4 H4 118.3 . . ? C8 N4 H4 118.3 . . ? C10 N5 Ni1 114.90(18) . 7_566 ? C10 N5 H5C 108.5 . . ? Ni1 N5 H5C 108.5 7_566 . ? C10 N5 H5D 108.5 . . ? Ni1 N5 H5D 108.5 7_566 . ? H5C N5 H5D 107.5 . . ? C11 N6 Ni1 116.03(19) . 7_566 ? C11 N6 H6C 108.3 . . ? Ni1 N6 H6C 108.3 7_566 . ? C11 N6 H6D 108.3 . . ? Ni1 N6 H6D 108.3 7_566 . ? H6C N6 H6D 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.62(10) 8_646 . ? O3 Ni1 N5 89.49(10) 8_646 8_646 ? N3 Ni1 N5 94.30(11) . 8_646 ? O3 Ni1 O2 85.66(9) 8_646 . ? N3 Ni1 O2 90.19(9) . . ? N5 Ni1 O2 95.24(9) 8_646 . ? O3 Ni1 N6 85.07(10) 8_646 8_646 ? N3 Ni1 N6 98.94(10) . 8_646 ? N5 Ni1 N6 86.70(11) 8_646 8_646 ? O2 Ni1 N6 170.51(10) . 8_646 ? O3 Ni1 N2 91.03(11) 8_646 . ? N3 Ni1 N2 85.13(11) . . ? N5 Ni1 N2 179.02(11) 8_646 . ? O2 Ni1 N2 83.96(10) . . ? N6 Ni1 N2 94.17(11) 8_646 . ? C7 O2 Ni1 119.48(19) . . ? C12 O3 Ni1 121.41(19) . 7_566 ? O1M N1MA O3M 117.0(6) . . ? O1M N1MA O2MA 117.3(8) . . ? O3M N1MA O2MA 124.5(7) . . ? O1M N1MB O3M 118.9(12) . . ? O1M N1MB O2MB 128.8(13) . . ? O3M N1MB O2MB 111.4(11) . . ? O5M N2M O6M 114.5(7) . . ? O5M N2M O4M 126.4(6) . . ? O6M N2M O4M 119.1(7) . . ? O8M N3M O8M 167.3(18) . 4_655 ? O8M N3M O8M 167.3(18) 4_655 2_665 ? O8M N3M O8M 167.3(18) . 3_565 ? O8M N3M O8M 167.3(18) 2_665 3_565 ? O8M N3M O7M 122.4(13) . 2_665 ? O8M N3M O7M 49.8(13) 4_655 2_665 ? O8M N3M O7M 119.5(13) 2_665 2_665 ? O8M N3M O7M 67.5(13) 3_565 2_665 ? O8M N3M O7M 67.5(13) . 3_565 ? O8M N3M O7M 122.4(13) 4_655 3_565 ? O8M N3M O7M 49.8(13) 2_665 3_565 ? O8M N3M O7M 119.5(13) 3_565 3_565 ? O7M N3M O7M 105.7(2) 2_665 3_565 ? O8M N3M O7M 49.8(13) . 4_655 ? O8M N3M O7M 119.5(13) 4_655 4_655 ? O8M N3M O7M 67.5(13) 2_665 4_655 ? O8M N3M O7M 122.4(13) 3_565 4_655 ? O7M N3M O7M 105.7(2) 2_665 4_655 ? O7M N3M O7M 117.3(5) 3_565 4_655 ? O8M N3M O7M 119.5(13) . . ? O8M N3M O7M 67.5(13) 4_655 . ? O8M N3M O7M 122.4(13) 2_665 . ? O8M N3M O7M 49.8(13) 3_565 . ? O7M N3M O7M 117.3(5) 2_665 . ? O7M N3M O7M 105.7(2) 3_565 . ? O7M N3M O7M 105.7(2) 4_655 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.378 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.105 #===END data_i-4_223K _database_code_depnum_ccdc_archive 'CCDC 856060' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.4928(7) _cell_length_b 15.4928(7) _cell_length_c 19.4045(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4657.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223 _cell_measurement_reflns_used 7649 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 29.68 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8684 _exptl_absorpt_correction_T_max 0.9147 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 223 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17519 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6713 _reflns_number_gt 5991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1043P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.096(15) _refine_ls_number_reflns 6713 _refine_ls_number_parameters 345 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.170 _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 0.7105(5) 1.0884(4) 0.8056(4) 0.080(2) Uani 1 1 d . . . H1A H 0.6930 1.0731 0.7592 0.121 Uiso 1 1 calc R . . H1B H 0.7361 1.1456 0.8053 0.121 Uiso 1 1 calc R . . H1C H 0.6605 1.0881 0.8356 0.121 Uiso 1 1 calc R . . C2 C 0.7758(3) 1.0239(3) 0.8314(3) 0.0516(11) Uani 1 1 d . . . C3 C 0.8082(3) 0.9100(3) 0.9158(2) 0.0405(8) Uani 1 1 d . . . H3A H 0.8063 0.9193 0.9657 0.049 Uiso 1 1 calc R . . H3B H 0.8676 0.9206 0.9004 0.049 Uiso 1 1 calc R . . C4 C 0.7846(2) 0.8149(2) 0.90040(17) 0.0292(6) Uani 1 1 d . . . C5 C 0.8502(3) 0.7585(2) 0.94011(19) 0.0365(7) Uani 1 1 d . . . H5A H 0.9084 0.7814 0.9323 0.044 Uiso 1 1 calc R . . H5B H 0.8380 0.7627 0.9896 0.044 Uiso 1 1 calc R . . C6 C 0.6912(3) 0.7986(2) 0.9254(2) 0.0365(7) Uani 1 1 d . . . H6A H 0.6815 0.8314 0.9678 0.044 Uiso 1 1 calc R . . H6B H 0.6510 0.8205 0.8905 0.044 Uiso 1 1 calc R . . C7 C 0.7911(2) 0.7914(2) 0.82394(17) 0.0268(6) Uani 1 1 d . . . C8 C 0.8447(2) 0.8251(2) 0.70829(17) 0.0287(6) Uani 1 1 d . . . H8A H 0.8241 0.8765 0.6838 0.034 Uiso 1 1 calc R . . H8B H 0.8070 0.7769 0.6957 0.034 Uiso 1 1 calc R . . C9 C 0.93694(19) 0.8048(2) 0.68440(16) 0.0266(6) Uani 1 1 d . . . C10 C 0.9977(2) 0.8754(2) 0.71144(19) 0.0310(6) Uani 1 1 d . . . H10A H 0.9685 0.9312 0.7074 0.037 Uiso 1 1 calc R . . H10B H 1.0085 0.8649 0.7605 0.037 Uiso 1 1 calc R . . C11 C 0.9319(2) 0.8066(2) 0.60448(17) 0.0312(6) Uani 1 1 d . . . H11A H 0.8822 0.7720 0.5899 0.037 Uiso 1 1 calc R . . H11B H 0.9213 0.8662 0.5897 0.037 Uiso 1 1 calc R . . C12 C 0.9706(2) 0.7179(2) 0.70727(16) 0.0260(6) Uani 1 1 d . . . N1 N 0.7510(3) 0.9723(2) 0.8823(2) 0.0486(9) Uani 1 1 d . . . H1 H 0.6979 0.9757 0.8966 0.058 Uiso 1 1 calc R . . N2 N 0.8485(2) 0.6668(2) 0.91970(17) 0.0342(6) Uani 1 1 d . . . H2A H 0.8580 0.6342 0.9580 0.041 Uiso 1 1 calc R . . H2B H 0.8933 0.6572 0.8903 0.041 Uiso 1 1 calc R . . N3 N 0.6715(2) 0.70693(19) 0.93860(16) 0.0328(6) Uani 1 1 d . . . H3C H 0.6134 0.6989 0.9350 0.039 Uiso 1 1 calc R . . H3D H 0.6871 0.6939 0.9826 0.039 Uiso 1 1 calc R . . N4 N 0.83760(18) 0.84023(18) 0.78237(15) 0.0285(5) Uani 1 1 d . . . H4 H 0.8655 0.8837 0.8000 0.034 Uiso 1 1 calc R . . N5 N 1.08175(18) 0.88067(18) 0.67535(16) 0.0297(5) Uani 1 1 d . . . H5C H 1.1227 0.8972 0.7063 0.036 Uiso 1 1 calc R . . H5D H 1.0782 0.9226 0.6427 0.036 Uiso 1 1 calc R . . N6 N 1.00974(18) 0.7741(2) 0.56847(15) 0.0324(6) Uani 1 1 d . . . H6C H 1.0204 0.8091 0.5317 0.039 Uiso 1 1 calc R . . H6D H 0.9979 0.7206 0.5517 0.039 Uiso 1 1 calc R . . N7 N 0.9200(2) 0.6628(2) 0.74011(18) 0.0362(6) Uani 1 1 d . . . H7A H 0.9403 0.6133 0.7536 0.043 Uiso 1 1 calc R . . H7B H 0.8664 0.6761 0.7482 0.043 Uiso 1 1 calc R . . O4M O 0.1015(6) 0.5968(5) 0.9191(5) 0.109(3) Uani 0.75 1 d PDU . . Ni1 Ni 0.73325(2) 0.62233(2) 0.871834(19) 0.02538(11) Uani 1 1 d . . . O1 O 0.8489(2) 1.02011(19) 0.80460(18) 0.0499(8) Uani 1 1 d . . . O2 O 0.75522(15) 0.72384(14) 0.80318(11) 0.0276(4) Uani 1 1 d . . . O3 O 1.04761(15) 0.69788(16) 0.69604(13) 0.0316(5) Uani 1 1 d . . . O5M O 0.1569(6) 0.7303(5) 0.9061(5) 0.111(3) Uani 0.75 1 d PDU . . O6M O 0.0314(6) 0.7055(8) 0.8765(7) 0.146(4) Uani 0.75 1 d PDU . . O7M O 0.5147(5) 0.5678(4) -0.0342(3) 0.0514(15) Uani 0.50 1 d PDU A -1 O2S O 0.0384(4) 0.8882(4) 0.8965(3) 0.0985(17) Uani 1 1 d . . . O3S O 0.5971(6) 0.0049(7) 0.9553(6) 0.177(5) Uani 1 1 d . . . O1M O 0.4867(4) 0.7141(4) 0.9016(4) 0.121(2) Uani 1 1 d DU . . O3M O 0.3769(3) 0.7784(4) 0.9361(3) 0.0853(14) Uani 1 1 d DU . . N1MA N 0.4500(4) 0.7834(4) 0.9104(4) 0.0464(19) Uani 0.612(14) 1 d PDU B 1 O2MA O 0.4823(7) 0.8433(7) 0.8789(7) 0.126(4) Uani 0.612(14) 1 d PDU B 1 N1MB N 0.4536(9) 0.7818(10) 0.9221(12) 0.115(10) Uani 0.388(14) 1 d PDU B 2 O2MB O 0.4889(8) 0.8478(7) 0.9448(8) 0.086(5) Uani 0.388(14) 1 d PDU B 2 N2M N 0.0987(5) 0.6770(6) 0.9031(5) 0.088(2) Uani 0.75 1 d PDU . . O8M O 0.4862(15) 0.5036(17) 0.0606(5) 0.062(5) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8259(7) 0.128(3) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.082(3) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.0369(12) Uani 1 4 d SDU . . 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 0.081(4) 0.055(3) 0.105(5) 0.027(3) 0.033(4) 0.022(3) C2 0.066(3) 0.0270(17) 0.062(3) -0.0013(17) 0.019(2) -0.0004(17) C3 0.054(2) 0.0337(17) 0.0335(17) -0.0076(14) 0.0061(16) -0.0124(15) C4 0.0358(16) 0.0287(15) 0.0231(13) -0.0053(11) 0.0039(12) -0.0050(11) C5 0.0428(18) 0.0347(17) 0.0319(16) -0.0005(13) -0.0052(14) -0.0067(15) C6 0.0416(18) 0.0314(16) 0.0365(17) -0.0063(13) 0.0145(14) -0.0027(13) C7 0.0277(14) 0.0265(14) 0.0263(14) -0.0011(11) 0.0048(11) 0.0019(11) C8 0.0271(14) 0.0322(14) 0.0269(14) 0.0043(11) 0.0020(11) 0.0011(11) C9 0.0240(13) 0.0313(14) 0.0246(14) 0.0019(11) 0.0026(10) 0.0022(11) C10 0.0299(15) 0.0288(14) 0.0343(16) -0.0030(12) 0.0061(12) -0.0005(12) C11 0.0258(14) 0.0412(17) 0.0265(14) 0.0021(13) -0.0002(11) 0.0027(12) C12 0.0255(13) 0.0306(14) 0.0219(13) 0.0024(11) 0.0014(10) -0.0001(11) N1 0.061(2) 0.0313(14) 0.053(2) -0.0051(14) 0.0251(18) 0.0006(13) N2 0.0325(14) 0.0347(14) 0.0353(14) 0.0025(12) -0.0051(11) -0.0020(11) N3 0.0373(14) 0.0301(13) 0.0311(14) -0.0052(11) 0.0086(11) -0.0033(11) N4 0.0289(12) 0.0280(12) 0.0286(12) -0.0016(10) 0.0052(10) -0.0010(10) N5 0.0265(13) 0.0290(13) 0.0336(14) 0.0025(10) 0.0013(10) -0.0033(10) N6 0.0279(13) 0.0467(16) 0.0226(12) 0.0007(11) 0.0013(10) -0.0009(11) N7 0.0315(14) 0.0314(13) 0.0458(17) 0.0101(12) 0.0101(12) 0.0010(11) O4M 0.133(6) 0.100(5) 0.094(5) -0.029(4) 0.002(5) 0.017(4) Ni1 0.0278(2) 0.02385(19) 0.02448(17) -0.00109(14) 0.00409(14) -0.00105(14) O1 0.0613(19) 0.0353(14) 0.0530(18) 0.0028(13) 0.0176(15) -0.0085(13) O2 0.0324(11) 0.0254(10) 0.0251(10) -0.0005(8) 0.0033(8) -0.0031(8) O3 0.0257(10) 0.0327(11) 0.0363(12) 0.0111(10) 0.0034(9) 0.0025(9) O5M 0.112(5) 0.078(4) 0.142(7) -0.018(4) 0.007(5) -0.003(4) O6M 0.114(6) 0.156(7) 0.166(8) 0.006(7) 0.016(6) -0.009(6) O7M 0.072(4) 0.045(3) 0.037(3) -0.001(2) 0.006(3) -0.006(3) O2S 0.109(4) 0.094(4) 0.092(4) -0.002(3) 0.014(3) -0.025(3) O3S 0.137(7) 0.158(7) 0.237(12) 0.069(7) 0.112(8) 0.053(6) O1M 0.082(3) 0.137(4) 0.145(4) -0.080(3) -0.022(3) 0.012(3) O3M 0.083(3) 0.105(3) 0.067(2) 0.011(2) 0.016(2) 0.017(2) N1MA 0.042(3) 0.052(3) 0.045(3) 0.001(2) -0.025(2) -0.002(2) O2MA 0.103(5) 0.146(6) 0.129(7) 0.021(5) 0.024(5) -0.008(4) N1MB 0.113(11) 0.115(11) 0.116(11) 0.000(5) -0.005(5) -0.007(5) O2MB 0.090(6) 0.081(6) 0.088(6) -0.008(4) -0.018(4) -0.014(4) N2M 0.077(5) 0.096(5) 0.093(5) 0.000(4) 0.009(4) 0.019(4) O8M 0.064(11) 0.065(6) 0.056(6) -0.017(7) 0.001(6) -0.006(8) O4S 0.081(5) 0.142(7) 0.161(8) 0.000 0.000 -0.007(5) O1S 0.089(4) 0.089(4) 0.069(5) 0.000 0.000 0.000 N3M 0.0376(18) 0.0376(18) 0.036(3) 0.000 0.000 0.000 _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 C2 1.508(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 O1 1.247(6) . ? C2 N1 1.328(6) . ? C3 N1 1.463(6) . ? C3 C4 1.547(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C7 1.531(5) . ? C4 C5 1.547(5) . ? C4 C6 1.547(5) . ? C5 N2 1.475(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N3 1.475(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.252(4) . ? C7 N4 1.320(4) . ? C8 N4 1.461(4) . ? C8 C9 1.535(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C12 1.509(4) . ? C9 C10 1.535(5) . ? C9 C11 1.553(5) . ? C10 N5 1.481(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 N6 1.482(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 O3 1.253(4) . ? C12 N7 1.323(4) . ? N1 H1 0.8700 . ? N2 Ni1 2.128(3) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 Ni1 2.077(3) . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N4 H4 0.8700 . ? N5 Ni1 2.085(3) 7_566 ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N6 Ni1 2.097(3) 7_566 ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N7 H7A 0.8700 . ? N7 H7B 0.8700 . ? O4M N2M 1.280(10) . ? Ni1 O3 2.053(2) 8_646 ? Ni1 N5 2.085(3) 8_646 ? Ni1 O2 2.089(2) . ? Ni1 N6 2.097(3) 8_646 ? O3 Ni1 2.053(2) 7_566 ? O5M N2M 1.226(10) . ? O6M N2M 1.244(10) . ? O7M N3M 1.263(6) . ? O1M N1MA 1.227(8) . ? O1M N1MB 1.235(13) . ? O3M N1MB 1.219(14) . ? O3M N1MA 1.239(8) . ? N1MA O2MA 1.219(10) . ? N1MB O2MB 1.239(13) . ? O8M N3M 1.197(10) . ? N3M O8M 1.197(10) 4_655 ? N3M O8M 1.197(10) 2_665 ? N3M O8M 1.197(10) 3_565 ? N3M O7M 1.263(6) 2_665 ? N3M O7M 1.263(6) 3_565 ? N3M O7M 1.263(6) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 123.0(5) . . ? O1 C2 C1 120.1(5) . . ? N1 C2 C1 116.9(5) . . ? N1 C3 C4 113.5(3) . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C7 C4 C5 107.8(3) . . ? C7 C4 C6 109.1(3) . . ? C5 C4 C6 111.5(3) . . ? C7 C4 C3 113.4(3) . . ? C5 C4 C3 106.6(3) . . ? C6 C4 C3 108.5(3) . . ? N2 C5 C4 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.9(3) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 121.7(3) . . ? O2 C7 C4 118.8(3) . . ? N4 C7 C4 119.5(3) . . ? N4 C8 C9 113.6(3) . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C12 C9 C10 108.8(3) . . ? C12 C9 C8 114.6(3) . . ? C10 C9 C8 108.7(3) . . ? C12 C9 C11 109.1(3) . . ? C10 C9 C11 111.1(3) . . ? C8 C9 C11 104.5(3) . . ? N5 C10 C9 114.6(3) . . ? N5 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? N5 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C9 115.0(3) . . ? N6 C11 H11A 108.5 . . ? C9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? C9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O3 C12 N7 119.2(3) . . ? O3 C12 C9 119.9(3) . . ? N7 C12 C9 120.8(3) . . ? C2 N1 C3 123.5(4) . . ? C2 N1 H1 118.2 . . ? C3 N1 H1 118.2 . . ? C5 N2 Ni1 116.4(2) . . ? C5 N2 H2A 108.2 . . ? Ni1 N2 H2A 108.2 . . ? C5 N2 H2B 108.2 . . ? Ni1 N2 H2B 108.2 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 113.8(2) . . ? C6 N3 H3C 108.8 . . ? Ni1 N3 H3C 108.8 . . ? C6 N3 H3D 108.8 . . ? Ni1 N3 H3D 108.8 . . ? H3C N3 H3D 107.7 . . ? C7 N4 C8 123.4(3) . . ? C7 N4 H4 118.3 . . ? C8 N4 H4 118.3 . . ? C10 N5 Ni1 115.2(2) . 7_566 ? C10 N5 H5C 108.5 . . ? Ni1 N5 H5C 108.5 7_566 . ? C10 N5 H5D 108.5 . . ? Ni1 N5 H5D 108.5 7_566 . ? H5C N5 H5D 107.5 . . ? C11 N6 Ni1 115.8(2) . 7_566 ? C11 N6 H6C 108.3 . . ? Ni1 N6 H6C 108.3 7_566 . ? C11 N6 H6D 108.3 . . ? Ni1 N6 H6D 108.3 7_566 . ? H6C N6 H6D 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.78(11) 8_646 . ? O3 Ni1 N5 89.32(11) 8_646 8_646 ? N3 Ni1 N5 94.24(12) . 8_646 ? O3 Ni1 O2 86.03(9) 8_646 . ? N3 Ni1 O2 89.87(11) . . ? N5 Ni1 O2 94.87(11) 8_646 . ? O3 Ni1 N6 85.05(11) 8_646 8_646 ? N3 Ni1 N6 98.93(12) . 8_646 ? N5 Ni1 N6 86.88(12) 8_646 8_646 ? O2 Ni1 N6 170.89(11) . 8_646 ? O3 Ni1 N2 91.51(12) 8_646 . ? N3 Ni1 N2 84.85(13) . . ? N5 Ni1 N2 178.66(12) 8_646 . ? O2 Ni1 N2 84.14(11) . . ? N6 Ni1 N2 94.24(12) 8_646 . ? C7 O2 Ni1 119.8(2) . . ? C12 O3 Ni1 121.3(2) . 7_566 ? O2MA N1MA O1M 113.9(8) . . ? O2MA N1MA O3M 128.6(8) . . ? O1M N1MA O3M 115.1(7) . . ? O3M N1MB O1M 116.1(12) . . ? O3M N1MB O2MB 112.8(12) . . ? O1M N1MB O2MB 129.2(14) . . ? O5M N2M O6M 113.4(9) . . ? O5M N2M O4M 128.2(9) . . ? O6M N2M O4M 118.2(9) . . ? O8M N3M O8M 165.1(16) . 4_655 ? O8M N3M O8M 165.1(16) 4_655 2_665 ? O8M N3M O8M 165.1(16) . 3_565 ? O8M N3M O8M 165.1(16) 2_665 3_565 ? O8M N3M O7M 121.5(13) . 2_665 ? O8M N3M O7M 47.7(11) 4_655 2_665 ? O8M N3M O7M 120.7(12) 2_665 2_665 ? O8M N3M O7M 68.9(12) 3_565 2_665 ? O8M N3M O7M 68.9(12) . 3_565 ? O8M N3M O7M 121.5(13) 4_655 3_565 ? O8M N3M O7M 47.7(11) 2_665 3_565 ? O8M N3M O7M 120.7(13) 3_565 3_565 ? O7M N3M O7M 106.0(3) 2_665 3_565 ? O8M N3M O7M 47.7(11) . 4_655 ? O8M N3M O7M 120.7(13) 4_655 4_655 ? O8M N3M O7M 68.9(12) 2_665 4_655 ? O8M N3M O7M 121.5(13) 3_565 4_655 ? O7M N3M O7M 106.0(3) 2_665 4_655 ? O7M N3M O7M 116.7(6) 3_565 4_655 ? O8M N3M O7M 120.7(12) . . ? O8M N3M O7M 68.9(12) 4_655 . ? O8M N3M O7M 121.5(13) 2_665 . ? O8M N3M O7M 47.7(11) 3_565 . ? O7M N3M O7M 116.7(6) 2_665 . ? O7M N3M O7M 106.0(3) 3_565 . ? O7M N3M O7M 106.0(3) 4_655 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.322 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.104 #===END data_i-4_233K _database_code_depnum_ccdc_archive 'CCDC 856061' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.619(2) _cell_length_b 14.619(2) _cell_length_c 18.944(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4048.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 233 _cell_measurement_reflns_used 1453 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 18.13 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8868 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 233 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 10729 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3585 _reflns_number_gt 2568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.0584P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 3585 _refine_ls_number_parameters 336 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.028 _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 0.6655(5) 1.0882(5) 0.7713(4) 0.057(2) Uani 1 1 d . . . H1A H 0.6753 1.1538 0.7742 0.086 Uiso 1 1 calc R . . H1B H 0.6095 1.0723 0.7959 0.086 Uiso 1 1 calc R . . H1C H 0.6607 1.0702 0.7222 0.086 Uiso 1 1 calc R . . C2 C 0.7444(6) 1.0395(4) 0.8047(4) 0.0473(18) Uani 1 1 d . . . C3 C 0.7917(5) 0.9480(4) 0.9072(4) 0.0450(16) Uani 1 1 d . . . H3A H 0.7901 0.9716 0.9556 0.054 Uiso 1 1 calc R . . H3B H 0.8522 0.9616 0.8877 0.054 Uiso 1 1 calc R . . C4 C 0.7789(4) 0.8442(4) 0.9093(4) 0.0367(14) Uani 1 1 d . . . C5 C 0.8550(5) 0.8066(5) 0.9573(4) 0.0473(18) Uani 1 1 d . . . H5A H 0.9120 0.8392 0.9470 0.057 Uiso 1 1 calc R . . H5B H 0.8389 0.8190 1.0066 0.057 Uiso 1 1 calc R . . C6 C 0.6845(5) 0.8227(4) 0.9387(4) 0.0448(17) Uani 1 1 d . . . H6A H 0.6714 0.8648 0.9777 0.054 Uiso 1 1 calc R . . H6B H 0.6389 0.8336 0.9017 0.054 Uiso 1 1 calc R . . C7 C 0.7905(4) 0.7986(4) 0.8379(3) 0.0325(14) Uani 1 1 d . . . C8 C 0.8479(4) 0.7942(5) 0.7182(3) 0.0409(16) Uani 1 1 d . . . H8A H 0.8215 0.8307 0.6799 0.049 Uiso 1 1 calc R . . H8B H 0.8150 0.7358 0.7197 0.049 Uiso 1 1 calc R . . C9 C 0.9494(4) 0.7750(4) 0.7008(3) 0.0368(14) Uani 1 1 d . . . C10 C 0.9844(5) 0.8622(5) 0.6651(4) 0.0518(19) Uani 1 1 d . . . H10A H 0.9425 0.8777 0.6265 0.062 Uiso 1 1 calc R . . H10B H 0.9817 0.9122 0.6995 0.062 Uiso 1 1 calc R . . C11 C 0.9481(4) 0.6926(4) 0.6511(3) 0.0395(15) Uani 1 1 d . . . H11A H 0.9123 0.6436 0.6731 0.047 Uiso 1 1 calc R . . H11B H 0.9170 0.7102 0.6073 0.047 Uiso 1 1 calc R . . C12 C 0.9953(4) 0.7466(5) 0.7706(4) 0.0402(17) Uani 1 1 d . . . N1 N 0.7233(4) 0.9958(3) 0.8658(3) 0.0433(13) Uani 1 1 d . . . H1 H 0.6670 0.9965 0.8807 0.052 Uiso 1 1 calc R . . N2 N 0.8709(4) 0.7074(4) 0.9489(3) 0.0444(14) Uani 1 1 d . . . H2A H 0.8896 0.6842 0.9910 0.053 Uiso 1 1 calc R . . H2B H 0.9171 0.6991 0.9174 0.053 Uiso 1 1 calc R . . N3 N 0.6751(4) 0.7285(3) 0.9642(3) 0.0421(14) Uani 1 1 d . . . H3C H 0.6155 0.7114 0.9595 0.051 Uiso 1 1 calc R . . H3D H 0.6886 0.7275 1.0110 0.051 Uiso 1 1 calc R . . N4 N 0.8326(3) 0.8427(3) 0.7855(3) 0.0365(13) Uani 1 1 d . . . H4 H 0.8508 0.8990 0.7909 0.044 Uiso 1 1 calc R . . N5 N 1.0770(4) 0.8578(4) 0.6367(3) 0.0481(15) Uani 1 1 d . . . H5C H 1.1151 0.8706 0.6734 0.058 Uiso 1 1 calc R . . H5D H 1.0821 0.9053 0.6060 0.058 Uiso 1 1 calc R . . N6 N 1.0388(3) 0.6570(3) 0.6335(3) 0.0388(13) Uani 1 1 d . . . H6C H 1.0310 0.6080 0.6045 0.047 Uiso 1 1 calc R . . H6D H 1.0646 0.6357 0.6741 0.047 Uiso 1 1 calc R . . N7 N 1.0520(4) 0.8062(5) 0.8008(3) 0.0684(19) Uani 1 1 d . . . H7A H 1.0772 0.7933 0.8412 0.082 Uiso 1 1 calc R . . H7B H 1.0639 0.8580 0.7802 0.082 Uiso 1 1 calc R . . N1M N 0.7607(4) 0.5686(4) 1.0666(3) 0.0590(17) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9678(5) 0.054(2) Uani 1 2 d SD . . N3M N 0.5009(15) 0.4886(14) 1.0074(13) 0.058(3) Uani 0.25 1 d PDU A -1 N2MB N 0.996(5) 0.011(2) 0.9607(12) 0.063(3) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75539(5) 0.63249(5) 0.91413(4) 0.0366(2) Uani 1 1 d . . . O1 O 0.8213(4) 1.0375(3) 0.7791(3) 0.0590(14) Uani 1 1 d . . . O2 O 0.7631(3) 0.7193(3) 0.8291(2) 0.0348(10) Uani 1 1 d . . . O3 O 0.9771(3) 0.6742(3) 0.7975(3) 0.0489(12) Uani 1 1 d . . . O1M O 0.7460(4) 0.5111(4) 1.1123(3) 0.0764(18) Uani 1 1 d . . . O2M O 0.7572(4) 0.5414(3) 1.0019(3) 0.0667(15) Uani 1 1 d . . . O3M O 0.7780(4) 0.6479(3) 1.0803(3) 0.0631(13) Uani 1 1 d D . . O4MA O 0.5688(5) 1.0041(5) 0.9977(6) 0.166(5) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9047(6) 0.162(6) Uani 1 2 d SD . . O9M O 0.5668(14) 0.5337(15) 1.0199(13) 0.060(3) Uani 0.25 1 d PDU A -1 O7M O 0.5012(13) 0.4238(12) 0.9676(16) 0.058(3) Uani 0.25 1 d PDU A -1 O8M O 0.4446(14) 0.4825(17) 1.0545(11) 0.058(3) Uani 0.25 1 d PDU A -1 O4MB O 0.9608(14) 0.0802(12) 0.9417(11) 0.061(3) Uani 0.25 1 d PDU B -2 O5MB O 1.0180(15) -0.0492(12) 0.9224(10) 0.064(3) Uani 0.25 1 d PDU B -2 O6MB O 0.9809(16) -0.011(2) 1.0235(9) 0.063(3) Uani 0.25 1 d PDU B -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 0.082(6) 0.049(5) 0.041(5) 0.009(3) -0.001(4) 0.010(4) C2 0.071(6) 0.029(4) 0.042(5) -0.003(3) -0.003(4) -0.007(3) C3 0.067(4) 0.038(4) 0.030(4) 0.001(3) -0.004(4) 0.004(3) C4 0.047(4) 0.032(3) 0.032(3) -0.004(3) 0.003(3) 0.000(2) C5 0.063(5) 0.044(4) 0.034(4) -0.006(3) -0.016(3) -0.002(3) C6 0.057(4) 0.039(4) 0.038(4) -0.003(3) 0.012(3) -0.002(3) C7 0.036(3) 0.034(4) 0.028(4) 0.005(3) 0.001(3) 0.004(3) C8 0.034(4) 0.059(4) 0.030(4) 0.003(3) -0.001(3) -0.004(3) C9 0.037(4) 0.044(4) 0.030(4) 0.004(3) 0.004(3) -0.003(3) C10 0.045(4) 0.061(5) 0.049(5) 0.014(4) 0.002(3) 0.000(3) C11 0.034(4) 0.052(4) 0.032(4) 0.000(3) 0.001(3) -0.003(3) C12 0.033(4) 0.048(4) 0.040(4) -0.006(3) 0.000(3) -0.007(3) N1 0.053(3) 0.040(3) 0.037(3) 0.002(3) 0.002(3) -0.001(3) N2 0.051(4) 0.044(3) 0.038(3) 0.001(3) -0.006(3) 0.000(3) N3 0.050(3) 0.041(3) 0.035(3) -0.003(3) 0.010(3) 0.007(3) N4 0.041(3) 0.035(3) 0.033(3) 0.000(2) 0.003(2) 0.001(2) N5 0.042(3) 0.048(4) 0.054(4) 0.021(3) 0.010(3) 0.003(3) N6 0.044(3) 0.041(3) 0.032(3) -0.002(2) 0.000(2) 0.000(2) N7 0.066(5) 0.090(5) 0.049(4) -0.003(4) -0.017(3) -0.024(4) N1M 0.081(4) 0.056(4) 0.040(4) 0.003(3) 0.018(3) 0.015(4) N2MA 0.052(6) 0.044(5) 0.065(7) 0.000 0.000 -0.009(4) N3M 0.058(3) 0.058(3) 0.058(3) -0.0002(8) -0.0001(8) 0.0001(8) N2MB 0.062(3) 0.063(3) 0.063(3) -0.0001(8) 0.0001(8) -0.0001(8) Ni1 0.0457(5) 0.0344(4) 0.0297(4) -0.0029(4) 0.0068(4) 0.0007(4) O1 0.069(4) 0.055(3) 0.053(3) 0.004(2) 0.014(3) -0.014(3) O2 0.043(3) 0.038(3) 0.024(2) -0.0008(19) -0.0026(19) 0.000(2) O3 0.050(3) 0.057(3) 0.040(3) 0.013(2) -0.005(2) -0.007(2) O1M 0.126(5) 0.068(4) 0.035(3) 0.012(3) 0.019(3) 0.009(3) O2M 0.114(5) 0.049(3) 0.037(3) -0.004(2) 0.014(3) 0.011(3) O3M 0.106(4) 0.051(3) 0.032(3) -0.006(3) 0.008(3) 0.003(3) O4MA 0.095(6) 0.094(5) 0.309(14) -0.109(7) -0.090(7) 0.036(4) O5MA 0.303(19) 0.128(10) 0.057(8) 0.000 0.000 0.073(11) O9M 0.060(3) 0.060(3) 0.059(3) 0.0000(10) 0.0000(10) -0.0002(10) O7M 0.058(3) 0.058(3) 0.058(3) -0.0003(10) -0.0006(10) 0.0001(10) O8M 0.058(3) 0.058(3) 0.057(4) 0.0000(10) 0.0001(10) 0.0002(10) O4MB 0.061(3) 0.061(3) 0.061(3) -0.0001(10) 0.0002(10) 0.0001(10) O5MB 0.063(3) 0.064(3) 0.064(3) -0.0005(10) 0.0003(10) -0.0004(10) O6MB 0.063(3) 0.063(3) 0.063(3) -0.0001(10) -0.0002(10) 0.0001(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 C2 1.495(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 O1 1.224(8) . ? C2 N1 1.358(9) . ? C3 N1 1.450(8) . ? C3 C4 1.530(8) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C7 1.517(9) . ? C4 C6 1.520(9) . ? C4 C5 1.539(9) . ? C5 N2 1.477(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N3 1.467(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.238(7) . ? C7 N4 1.334(7) . ? C8 N4 1.476(8) . ? C8 C9 1.546(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C11 1.529(9) . ? C9 C10 1.530(9) . ? C9 C12 1.539(9) . ? C10 N5 1.459(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 N6 1.464(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 O3 1.205(7) . ? C12 N7 1.332(9) . ? N1 H1 0.8700 . ? N2 Ni1 2.118(5) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 Ni1 2.060(5) . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N4 H4 0.8700 . ? N5 Ni1 2.079(6) 7_566 ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N6 Ni1 2.081(5) 7_566 ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? N7 H7A 0.8700 . ? N7 H7B 0.8700 . ? N1M O1M 1.226(7) . ? N1M O3M 1.215(7) . ? N1M O2M 1.290(7) . ? N2MA O4MA 1.155(7) 2_675 ? N2MA O4MA 1.155(7) . ? N2MA O5MA 1.196(10) . ? N3M O9M 1.191(14) . ? N3M O7M 1.211(13) . ? N3M O8M 1.218(14) . ? N2MB O5MB 1.188(14) . ? N2MB O4MB 1.189(15) . ? N2MB O6MB 1.26(3) . ? Ni1 O2 2.054(4) . ? Ni1 N5 2.079(6) 8_646 ? Ni1 N6 2.081(5) 8_646 ? Ni1 O2M 2.130(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.3(7) . . ? O1 C2 C1 123.5(7) . . ? N1 C2 C1 114.2(7) . . ? N1 C3 C4 114.1(5) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C6 109.7(5) . . ? C7 C4 C3 113.5(6) . . ? C6 C4 C3 109.0(5) . . ? C7 C4 C5 106.8(5) . . ? C6 C4 C5 111.5(6) . . ? C3 C4 C5 106.4(5) . . ? N2 C5 C4 113.7(5) . . ? N2 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.6(5) . . ? N3 C6 H6A 108.9 . . ? C4 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 120.1(6) . . ? O2 C7 C4 119.7(5) . . ? N4 C7 C4 120.2(5) . . ? N4 C8 C9 114.6(5) . . ? N4 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N4 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C11 C9 C10 112.8(6) . . ? C11 C9 C12 108.8(5) . . ? C10 C9 C12 117.4(6) . . ? C11 C9 C8 105.2(5) . . ? C10 C9 C8 105.3(5) . . ? C12 C9 C8 106.5(5) . . ? N5 C10 C9 115.8(6) . . ? N5 C10 H10A 108.3 . . ? C9 C10 H10A 108.3 . . ? N5 C10 H10B 108.3 . . ? C9 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? N6 C11 C9 114.1(5) . . ? N6 C11 H11A 108.7 . . ? C9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? C9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 122.0(7) . . ? O3 C12 C9 120.3(6) . . ? N7 C12 C9 117.6(6) . . ? C2 N1 C3 122.1(6) . . ? C2 N1 H1 119.0 . . ? C3 N1 H1 119.0 . . ? C5 N2 Ni1 114.6(4) . . ? C5 N2 H2A 108.6 . . ? Ni1 N2 H2A 108.6 . . ? C5 N2 H2B 108.6 . . ? Ni1 N2 H2B 108.6 . . ? H2A N2 H2B 107.6 . . ? C6 N3 Ni1 115.8(4) . . ? C6 N3 H3C 108.3 . . ? Ni1 N3 H3C 108.3 . . ? C6 N3 H3D 108.3 . . ? Ni1 N3 H3D 108.3 . . ? H3C N3 H3D 107.4 . . ? C7 N4 C8 118.8(5) . . ? C7 N4 H4 120.6 . . ? C8 N4 H4 120.6 . . ? C10 N5 Ni1 124.6(5) . 7_566 ? C10 N5 H5C 106.2 . . ? Ni1 N5 H5C 106.2 7_566 . ? C10 N5 H5D 106.2 . . ? Ni1 N5 H5D 106.2 7_566 . ? H5C N5 H5D 106.4 . . ? C11 N6 Ni1 118.4(4) . 7_566 ? C11 N6 H6C 107.7 . . ? Ni1 N6 H6C 107.7 7_566 . ? C11 N6 H6D 107.7 . . ? Ni1 N6 H6D 107.7 7_566 . ? H6C N6 H6D 107.1 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O1M N1M O3M 122.6(6) . . ? O1M N1M O2M 117.0(6) . . ? O3M N1M O2M 120.4(6) . . ? O4MA N2MA O4MA 121.4(15) 2_675 . ? O4MA N2MA O5MA 119.3(8) 2_675 . ? O4MA N2MA O5MA 119.3(8) . . ? O9M N3M O7M 123.7(16) . . ? O9M N3M O8M 116.2(15) . . ? O7M N3M O8M 113.7(14) . . ? O5MB N2MB O4MB 124.2(19) . . ? O5MB N2MB O6MB 115(3) . . ? O4MB N2MB O6MB 116(2) . . ? O2 Ni1 N3 88.34(19) . . ? O2 Ni1 N5 85.5(2) . 8_646 ? N3 Ni1 N5 91.4(2) . 8_646 ? O2 Ni1 N6 91.88(18) . 8_646 ? N3 Ni1 N6 176.7(2) . 8_646 ? N5 Ni1 N6 91.8(2) 8_646 8_646 ? O2 Ni1 N2 83.12(19) . . ? N3 Ni1 N2 87.7(2) . . ? N5 Ni1 N2 168.6(2) 8_646 . ? N6 Ni1 N2 89.1(2) 8_646 . ? O2 Ni1 O2M 176.1(2) . . ? N3 Ni1 O2M 94.2(2) . . ? N5 Ni1 O2M 97.4(2) 8_646 . ? N6 Ni1 O2M 85.4(2) 8_646 . ? N2 Ni1 O2M 94.1(2) . . ? C7 O2 Ni1 119.4(4) . . ? N1M O2M Ni1 123.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.743 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.071 #===END data_i-4_273K _database_code_depnum_ccdc_archive 'CCDC 856062' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.6608(14) _cell_length_b 14.6608(14) _cell_length_c 18.9712(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4077.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 273 _cell_measurement_reflns_used 5509 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.42 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8539 _exptl_absorpt_correction_T_max 0.9050 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 273 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 14209 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 29.11 _reflns_number_total 5452 _reflns_number_gt 4300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.0514P)^2^+1.5592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.056(13) _refine_ls_number_reflns 5452 _refine_ls_number_parameters 336 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.081 _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 0.6658(3) 1.0879(3) 0.7710(2) 0.0629(11) Uani 1 1 d . . . H1A H 0.6719 1.1524 0.7786 0.094 Uiso 1 1 calc R . . H1B H 0.6094 1.0671 0.7909 0.094 Uiso 1 1 calc R . . H1C H 0.6663 1.0755 0.7213 0.094 Uiso 1 1 calc R . . C2 C 0.7435(3) 1.0392(2) 0.8054(2) 0.0472(8) Uani 1 1 d . . . C3 C 0.7920(2) 0.9482(2) 0.90740(19) 0.0454(7) Uani 1 1 d . . . H3A H 0.7900 0.9715 0.9552 0.054 Uiso 1 1 calc R . . H3B H 0.8518 0.9618 0.8883 0.054 Uiso 1 1 calc R . . C4 C 0.7794(2) 0.84391(18) 0.90956(17) 0.0356(6) Uani 1 1 d . . . C5 C 0.8560(3) 0.8058(2) 0.95738(18) 0.0447(8) Uani 1 1 d . . . H5A H 0.9125 0.8372 0.9465 0.054 Uiso 1 1 calc R . . H5B H 0.8409 0.8188 1.0062 0.054 Uiso 1 1 calc R . . C6 C 0.6846(2) 0.8222(2) 0.93882(18) 0.0427(7) Uani 1 1 d . . . H6A H 0.6716 0.8638 0.9773 0.051 Uiso 1 1 calc R . . H6B H 0.6398 0.8329 0.9021 0.051 Uiso 1 1 calc R . . C7 C 0.79063(19) 0.79844(19) 0.83750(15) 0.0310(6) Uani 1 1 d . . . C8 C 0.8472(2) 0.7942(3) 0.71820(17) 0.0407(7) Uani 1 1 d . . . H8A H 0.8216 0.8305 0.6804 0.049 Uiso 1 1 calc R . . H8B H 0.8146 0.7366 0.7193 0.049 Uiso 1 1 calc R . . C9 C 0.9489(2) 0.7751(2) 0.70157(16) 0.0367(6) Uani 1 1 d . . . C10 C 0.9843(2) 0.8617(2) 0.6657(2) 0.0469(8) Uani 1 1 d . . . H10A H 0.9426 0.8771 0.6278 0.056 Uiso 1 1 calc R . . H10B H 0.9818 0.9110 0.6997 0.056 Uiso 1 1 calc R . . C11 C 0.9483(2) 0.6933(2) 0.65107(17) 0.0388(6) Uani 1 1 d . . . H11A H 0.9124 0.6449 0.6721 0.047 Uiso 1 1 calc R . . H11B H 0.9181 0.7114 0.6077 0.047 Uiso 1 1 calc R . . C12 C 0.9954(2) 0.7478(2) 0.77033(16) 0.0381(7) Uani 1 1 d . . . N1 N 0.7233(2) 0.99558(18) 0.86539(16) 0.0455(6) Uani 1 1 d . . . H1 H 0.6677 0.9955 0.8798 0.055 Uiso 1 1 calc R . . N2 N 0.8701(2) 0.70777(19) 0.94938(15) 0.0437(6) Uani 1 1 d . . . H2A H 0.8880 0.6850 0.9912 0.052 Uiso 1 1 calc R . . H2B H 0.9161 0.6990 0.9187 0.052 Uiso 1 1 calc R . . N3 N 0.6747(2) 0.72870(18) 0.96430(15) 0.0419(6) Uani 1 1 d . . . H3C H 0.6160 0.7121 0.9594 0.050 Uiso 1 1 calc R . . H3D H 0.6878 0.7278 1.0106 0.050 Uiso 1 1 calc R . . N4 N 0.83227(18) 0.84197(18) 0.78552(14) 0.0381(5) Uani 1 1 d . . . H4 H 0.8503 0.8973 0.7910 0.046 Uiso 1 1 calc R . . N5 N 1.07639(19) 0.85847(19) 0.63669(16) 0.0446(6) Uani 1 1 d . . . H5C H 1.1144 0.8719 0.6725 0.054 Uiso 1 1 calc R . . H5D H 1.0804 0.9050 0.6059 0.054 Uiso 1 1 calc R . . N6 N 1.03871(18) 0.65708(18) 0.63352(14) 0.0374(5) Uani 1 1 d . . . H6C H 1.0308 0.6088 0.6048 0.045 Uiso 1 1 calc R . . H6D H 1.0640 0.6361 0.6736 0.045 Uiso 1 1 calc R . . N7 N 1.0526(3) 0.8069(3) 0.80054(18) 0.0684(10) Uani 1 1 d . . . H7A H 1.0780 0.7937 0.8401 0.082 Uiso 1 1 calc R . . H7B H 1.0641 0.8582 0.7804 0.082 Uiso 1 1 calc R . . N1M N 0.7600(3) 0.5672(2) 1.06603(15) 0.0560(8) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9687(3) 0.0504(10) Uani 1 2 d SD . . N3M N 0.5055(14) 0.4906(12) 1.0067(9) 0.034(4) Uani 0.25 1 d PDU A -1 N2MB N 0.997(4) 0.0087(18) 0.9619(9) 0.059(4) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75562(3) 0.63230(2) 0.914211(19) 0.03430(10) Uani 1 1 d . . . O1 O 0.8212(2) 1.03756(19) 0.77915(15) 0.0616(7) Uani 1 1 d . . . O2 O 0.76309(14) 0.71894(14) 0.82941(10) 0.0342(4) Uani 1 1 d . . . O3 O 0.97778(18) 0.67479(19) 0.79731(14) 0.0534(6) Uani 1 1 d . . . O1M O 0.7462(3) 0.5112(2) 1.11257(15) 0.0811(11) Uani 1 1 d . . . O2M O 0.7569(2) 0.54147(17) 1.00180(12) 0.0618(8) Uani 1 1 d . . . O3M O 0.7773(2) 0.64730(19) 1.08046(14) 0.0668(8) Uani 1 1 d D . . O4MA O 0.5687(3) 1.0032(3) 0.9994(4) 0.165(3) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9066(4) 0.173(4) Uani 1 2 d SD . . O9M O 0.5695(15) 0.5388(15) 1.0167(10) 0.105(7) Uani 0.25 1 d PDU A -1 O7M O 0.5071(10) 0.4265(8) 0.9687(7) 0.053(4) Uani 0.25 1 d PDU A -1 O8M O 0.4523(11) 0.4856(11) 1.0546(7) 0.069(4) Uani 0.25 1 d PDU A -1 O4MB O 0.9638(10) 0.0778(9) 0.9411(6) 0.055(3) Uani 0.25 1 d PDU B -2 O5MB O 1.0173(13) -0.0492(11) 0.9217(8) 0.090(5) Uani 0.25 1 d PDU B -2 O6MB O 0.9776(17) -0.0146(16) 1.0230(8) 0.089(7) Uani 0.25 1 d PDU B -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 0.093(3) 0.0430(19) 0.053(2) 0.0081(17) -0.007(2) 0.0084(19) C2 0.064(2) 0.0281(15) 0.0491(19) -0.0017(13) 0.0005(17) -0.0045(14) C3 0.060(2) 0.0329(14) 0.0428(17) 0.0005(14) -0.0063(16) -0.0017(13) C4 0.0458(16) 0.0299(13) 0.0311(13) -0.0025(13) 0.0011(13) 0.0007(11) C5 0.058(2) 0.0380(16) 0.0382(17) -0.0011(13) -0.0139(15) -0.0032(15) C6 0.0527(19) 0.0366(16) 0.0389(16) -0.0019(13) 0.0111(14) 0.0044(13) C7 0.0298(13) 0.0336(14) 0.0296(13) -0.0018(11) -0.0027(11) 0.0032(11) C8 0.0322(15) 0.057(2) 0.0327(15) -0.0004(13) 0.0032(12) 0.0022(14) C9 0.0359(15) 0.0399(16) 0.0343(14) 0.0023(12) 0.0046(12) -0.0021(12) C10 0.0417(18) 0.0449(18) 0.054(2) 0.0105(16) 0.0079(15) 0.0037(13) C11 0.0339(15) 0.0479(17) 0.0345(14) -0.0010(13) 0.0013(12) -0.0024(13) C12 0.0296(14) 0.0510(18) 0.0337(15) 0.0010(13) 0.0038(12) 0.0010(13) N1 0.0556(17) 0.0358(14) 0.0449(15) -0.0007(12) 0.0034(13) 0.0024(12) N2 0.0467(15) 0.0422(15) 0.0421(14) 0.0013(12) -0.0080(12) -0.0015(12) N3 0.0505(16) 0.0375(14) 0.0376(14) -0.0039(11) 0.0121(12) 0.0032(12) N4 0.0363(13) 0.0401(13) 0.0378(13) 0.0021(11) 0.0068(10) -0.0001(11) N5 0.0402(14) 0.0452(15) 0.0485(15) 0.0165(12) 0.0099(12) 0.0038(12) N6 0.0381(13) 0.0405(14) 0.0336(12) 0.0023(11) 0.0026(11) -0.0030(11) N7 0.070(2) 0.085(3) 0.0502(18) -0.0016(18) -0.0147(17) -0.0299(19) N1M 0.080(2) 0.0490(17) 0.0394(16) 0.0063(13) 0.0168(14) 0.0135(16) N2MA 0.046(2) 0.041(2) 0.064(3) 0.000 0.000 -0.0036(18) N3M 0.049(7) 0.031(7) 0.023(6) 0.007(5) -0.007(6) 0.009(7) N2MB 0.046(6) 0.061(8) 0.069(7) -0.015(7) 0.006(8) -0.008(7) Ni1 0.0422(2) 0.03034(18) 0.03031(16) -0.00330(15) 0.00585(16) 0.00031(16) O1 0.0725(19) 0.0515(15) 0.0607(16) 0.0047(13) 0.0106(14) -0.0077(13) O2 0.0395(11) 0.0357(10) 0.0274(9) -0.0017(8) 0.0005(8) -0.0030(9) O3 0.0508(14) 0.0599(16) 0.0495(14) 0.0203(12) -0.0049(11) -0.0048(12) O1M 0.130(3) 0.070(2) 0.0436(15) 0.0150(14) 0.0185(17) 0.012(2) O2M 0.110(2) 0.0417(13) 0.0337(12) 0.0008(10) 0.0159(14) 0.0055(14) O3M 0.111(2) 0.0536(15) 0.0357(12) -0.0047(12) 0.0040(15) 0.0070(14) O4MA 0.095(3) 0.095(3) 0.305(8) -0.107(4) -0.094(4) 0.031(2) O5MA 0.318(13) 0.127(6) 0.075(4) 0.000 0.000 0.071(7) O9M 0.106(10) 0.116(10) 0.092(9) -0.009(8) -0.003(8) -0.031(8) O7M 0.069(7) 0.043(5) 0.046(6) -0.012(5) -0.038(6) 0.030(5) O8M 0.099(8) 0.066(7) 0.043(6) 0.000(6) 0.007(6) 0.006(6) O4MB 0.052(6) 0.065(6) 0.048(5) -0.010(5) 0.000(5) -0.001(5) O5MB 0.077(8) 0.105(8) 0.090(8) -0.034(7) 0.020(7) -0.020(7) O6MB 0.091(10) 0.089(9) 0.085(9) -0.005(8) -0.016(8) 0.022(8) _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 C2 1.494(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.243(5) . ? C2 N1 1.339(5) . ? C3 N1 1.460(4) . ? C3 C4 1.540(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C6 1.529(5) . ? C4 C7 1.530(4) . ? C4 C5 1.547(4) . ? C5 N2 1.461(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.461(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.243(4) . ? C7 N4 1.324(4) . ? C8 N4 1.473(4) . ? C8 C9 1.549(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.526(4) . ? C9 C10 1.530(4) . ? C9 C11 1.535(5) . ? C10 N5 1.459(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.467(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.214(4) . ? C12 N7 1.336(5) . ? N1 H1 0.8600 . ? N2 Ni1 2.118(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.075(3) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.098(3) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.083(3) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N1M O1M 1.223(4) . ? N1M O3M 1.232(4) . ? N1M O2M 1.277(4) . ? N2MA O4MA 1.164(5) 2_675 ? N2MA O4MA 1.164(5) . ? N2MA O5MA 1.179(7) . ? N3M O7M 1.185(13) . ? N3M O9M 1.189(13) . ? N3M O8M 1.200(13) . ? N2MB O5MB 1.180(13) . ? N2MB O4MB 1.190(14) . ? N2MB O6MB 1.24(3) . ? Ni1 O2 2.053(2) . ? Ni1 N6 2.083(3) 8_646 ? Ni1 N5 2.098(3) 8_646 ? Ni1 O2M 2.130(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.2(4) . . ? O1 C2 C1 122.2(4) . . ? N1 C2 C1 115.5(4) . . ? N1 C3 C4 113.9(3) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C6 C4 C7 109.4(2) . . ? C6 C4 C3 109.0(2) . . ? C7 C4 C3 113.3(3) . . ? C6 C4 C5 111.8(3) . . ? C7 C4 C5 106.8(2) . . ? C3 C4 C5 106.7(2) . . ? N2 C5 C4 113.4(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.9(3) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 120.6(3) . . ? O2 C7 C4 118.9(2) . . ? N4 C7 C4 120.4(3) . . ? N4 C8 C9 113.9(3) . . ? N4 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N4 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C12 C9 C10 116.5(3) . . ? C12 C9 C11 109.3(3) . . ? C10 C9 C11 111.9(3) . . ? C12 C9 C8 107.7(2) . . ? C10 C9 C8 105.5(3) . . ? C11 C9 C8 105.2(2) . . ? N5 C10 C9 117.0(3) . . ? N5 C10 H10A 108.0 . . ? C9 C10 H10A 108.0 . . ? N5 C10 H10B 108.0 . . ? C9 C10 H10B 108.0 . . ? H10A C10 H10B 107.3 . . ? N6 C11 C9 114.8(2) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? O3 C12 N7 121.7(3) . . ? O3 C12 C9 119.8(3) . . ? N7 C12 C9 118.5(3) . . ? C2 N1 C3 122.6(3) . . ? C2 N1 H1 118.7 . . ? C3 N1 H1 118.7 . . ? C5 N2 Ni1 115.8(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 115.5(2) . . ? C6 N3 H3C 108.4 . . ? Ni1 N3 H3C 108.4 . . ? C6 N3 H3D 108.4 . . ? Ni1 N3 H3D 108.4 . . ? H3C N3 H3D 107.5 . . ? C7 N4 C8 119.0(3) . . ? C7 N4 H4 120.5 . . ? C8 N4 H4 120.5 . . ? C10 N5 Ni1 124.1(2) . 7_566 ? C10 N5 H5C 106.3 . . ? Ni1 N5 H5C 106.3 7_566 . ? C10 N5 H5D 106.3 . . ? Ni1 N5 H5D 106.3 7_566 . ? H5C N5 H5D 106.4 . . ? C11 N6 Ni1 118.1(2) . 7_566 ? C11 N6 H6C 107.8 . . ? Ni1 N6 H6C 107.8 7_566 . ? C11 N6 H6D 107.8 . . ? Ni1 N6 H6D 107.8 7_566 . ? H6C N6 H6D 107.1 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O1M N1M O3M 120.9(3) . . ? O1M N1M O2M 119.0(3) . . ? O3M N1M O2M 120.1(3) . . ? O4MA N2MA O4MA 120.0(9) 2_675 . ? O4MA N2MA O5MA 120.0(4) 2_675 . ? O4MA N2MA O5MA 120.0(4) . . ? O7M N3M O9M 123.6(15) . . ? O7M N3M O8M 115.1(14) . . ? O9M N3M O8M 115.4(13) . . ? O5MB N2MB O4MB 120.1(16) . . ? O5MB N2MB O6MB 118(2) . . ? O4MB N2MB O6MB 117(2) . . ? O2 Ni1 N3 88.17(10) . . ? O2 Ni1 N6 91.96(9) . 8_646 ? N3 Ni1 N6 176.93(12) . 8_646 ? O2 Ni1 N5 85.62(10) . 8_646 ? N3 Ni1 N5 91.21(11) . 8_646 ? N6 Ni1 N5 91.85(10) 8_646 8_646 ? O2 Ni1 N2 83.19(10) . . ? N3 Ni1 N2 87.30(12) . . ? N6 Ni1 N2 89.67(11) 8_646 . ? N5 Ni1 N2 168.75(12) 8_646 . ? O2 Ni1 O2M 176.43(11) . . ? N3 Ni1 O2M 94.21(11) . . ? N6 Ni1 O2M 85.53(11) 8_646 . ? N5 Ni1 O2M 96.99(12) 8_646 . ? N2 Ni1 O2M 94.25(12) . . ? C7 O2 Ni1 120.05(18) . . ? N1M O2M Ni1 124.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.557 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.060 #===END data_i-4_293K _database_code_depnum_ccdc_archive 'CCDC 856063' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.6619(12) _cell_length_b 14.6619(12) _cell_length_c 18.9721(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4078.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 6857 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 28.57 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8540 _exptl_absorpt_correction_T_max 0.9050 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 14097 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 29.09 _reflns_number_total 5408 _reflns_number_gt 4448 _reflns_threshold_expression >2sigma _computing_data_collection 'APEX2 ' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.0503P)^2^+3.1173P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.062(14) _refine_ls_number_reflns 5408 _refine_ls_number_parameters 336 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.078 _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 0.6661(4) 1.0880(3) 0.7710(2) 0.0666(11) Uani 1 1 d . . . H1A H 0.6735 1.1525 0.7774 0.100 Uiso 1 1 calc R . . H1B H 0.6098 1.0687 0.7921 0.100 Uiso 1 1 calc R . . H1C H 0.6653 1.0741 0.7216 0.100 Uiso 1 1 calc R . . C2 C 0.7439(3) 1.0389(2) 0.8053(2) 0.0502(8) Uani 1 1 d . . . C3 C 0.7917(3) 0.9478(2) 0.9075(2) 0.0481(7) Uani 1 1 d . . . H3A H 0.7893 0.9710 0.9553 0.058 Uiso 1 1 calc R . . H3B H 0.8517 0.9615 0.8887 0.058 Uiso 1 1 calc R . . C4 C 0.7795(2) 0.84376(18) 0.90946(17) 0.0374(6) Uani 1 1 d . . . C5 C 0.8560(3) 0.8056(2) 0.95727(18) 0.0471(8) Uani 1 1 d . . . H5A H 0.9126 0.8368 0.9462 0.057 Uiso 1 1 calc R . . H5B H 0.8411 0.8189 1.0060 0.057 Uiso 1 1 calc R . . C6 C 0.6847(2) 0.8221(2) 0.93890(19) 0.0451(7) Uani 1 1 d . . . H6A H 0.6718 0.8635 0.9775 0.054 Uiso 1 1 calc R . . H6B H 0.6397 0.8330 0.9024 0.054 Uiso 1 1 calc R . . C7 C 0.79072(19) 0.79830(19) 0.83746(15) 0.0325(5) Uani 1 1 d . . . C8 C 0.8472(2) 0.7938(3) 0.71838(17) 0.0428(7) Uani 1 1 d . . . H8A H 0.8214 0.8301 0.6806 0.051 Uiso 1 1 calc R . . H8B H 0.8148 0.7362 0.7195 0.051 Uiso 1 1 calc R . . C9 C 0.9491(2) 0.7749(2) 0.70151(16) 0.0383(6) Uani 1 1 d . . . C10 C 0.9843(2) 0.8616(2) 0.6657(2) 0.0487(8) Uani 1 1 d . . . H10A H 0.9426 0.8769 0.6277 0.058 Uiso 1 1 calc R . . H10B H 0.9818 0.9109 0.6997 0.058 Uiso 1 1 calc R . . C11 C 0.9482(2) 0.6934(2) 0.65112(17) 0.0408(6) Uani 1 1 d . . . H11A H 0.9123 0.6450 0.6722 0.049 Uiso 1 1 calc R . . H11B H 0.9179 0.7116 0.6079 0.049 Uiso 1 1 calc R . . C12 C 0.9954(2) 0.7476(2) 0.77019(16) 0.0403(7) Uani 1 1 d . . . N1 N 0.7235(2) 0.99535(19) 0.86528(16) 0.0474(6) Uani 1 1 d . . . H1 H 0.6678 0.9954 0.8795 0.057 Uiso 1 1 calc R . . N2 N 0.8700(2) 0.7075(2) 0.94963(16) 0.0460(6) Uani 1 1 d . . . H2A H 0.8874 0.6849 0.9916 0.055 Uiso 1 1 calc R . . H2B H 0.9161 0.6984 0.9192 0.055 Uiso 1 1 calc R . . N3 N 0.6749(2) 0.72856(19) 0.96408(15) 0.0441(6) Uani 1 1 d . . . H3C H 0.6161 0.7119 0.9591 0.053 Uiso 1 1 calc R . . H3D H 0.6878 0.7275 1.0105 0.053 Uiso 1 1 calc R . . N4 N 0.83222(18) 0.84148(19) 0.78539(14) 0.0402(6) Uani 1 1 d . . . H4 H 0.8502 0.8969 0.7907 0.048 Uiso 1 1 calc R . . N5 N 1.07636(19) 0.8584(2) 0.63661(16) 0.0461(6) Uani 1 1 d . . . H5C H 1.1143 0.8720 0.6724 0.055 Uiso 1 1 calc R . . H5D H 1.0803 0.9049 0.6058 0.055 Uiso 1 1 calc R . . N6 N 1.03853(18) 0.65714(18) 0.63341(14) 0.0388(5) Uani 1 1 d . . . H6C H 1.0305 0.6090 0.6046 0.047 Uiso 1 1 calc R . . H6D H 1.0639 0.6360 0.6734 0.047 Uiso 1 1 calc R . . N7 N 1.0526(3) 0.8068(3) 0.8005(2) 0.0733(11) Uani 1 1 d . . . H7A H 1.0780 0.7936 0.8401 0.088 Uiso 1 1 calc R . . H7B H 1.0640 0.8582 0.7805 0.088 Uiso 1 1 calc R . . N1M N 0.7600(3) 0.5673(2) 1.06617(16) 0.0588(8) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9688(3) 0.0525(10) Uani 1 2 d SD . . N3M N 0.5047(15) 0.4916(13) 1.0068(10) 0.040(4) Uani 0.25 1 d PDU A -1 N2MB N 0.996(4) 0.0085(18) 0.9621(10) 0.062(4) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75567(3) 0.63220(2) 0.914201(19) 0.03586(10) Uani 1 1 d . . . O1 O 0.8214(2) 1.0373(2) 0.77925(16) 0.0648(7) Uani 1 1 d . . . O2 O 0.76323(15) 0.71863(14) 0.82944(10) 0.0366(4) Uani 1 1 d . . . O3 O 0.97794(19) 0.6747(2) 0.79705(14) 0.0569(6) Uani 1 1 d . . . O1M O 0.7460(3) 0.5112(2) 1.11238(16) 0.0847(11) Uani 1 1 d . . . O2M O 0.7569(2) 0.54131(18) 1.00176(13) 0.0636(8) Uani 1 1 d . . . O3M O 0.7769(3) 0.6473(2) 1.08047(14) 0.0701(8) Uani 1 1 d D . . O4MA O 0.5688(3) 1.0028(4) 0.9990(4) 0.170(3) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9065(4) 0.177(4) Uani 1 2 d SD . . O9M O 0.5652(16) 0.5451(16) 1.0144(12) 0.118(7) Uani 0.25 1 d PDU A -1 O7M O 0.5093(10) 0.4267(8) 0.9695(7) 0.054(3) Uani 0.25 1 d PDU A -1 O8M O 0.4510(12) 0.4866(11) 1.0548(7) 0.072(4) Uani 0.25 1 d PDU A -1 O4MB O 0.9635(10) 0.0782(9) 0.9411(7) 0.057(3) Uani 0.25 1 d PDU B -2 O5MB O 1.0180(14) -0.0498(11) 0.9220(9) 0.095(5) Uani 0.25 1 d PDU B -2 O6MB O 0.9769(17) -0.0146(16) 1.0233(8) 0.088(6) Uani 0.25 1 d PDU B -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 0.096(3) 0.047(2) 0.057(2) 0.0092(18) -0.007(2) 0.010(2) C2 0.070(2) 0.0296(15) 0.0511(19) -0.0020(13) 0.0002(17) -0.0039(14) C3 0.063(2) 0.0356(14) 0.0454(17) 0.0008(14) -0.0062(16) -0.0016(13) C4 0.0471(16) 0.0317(13) 0.0334(13) -0.0026(13) 0.0006(13) 0.0015(11) C5 0.060(2) 0.0396(16) 0.0414(17) -0.0022(13) -0.0146(15) -0.0035(15) C6 0.0541(19) 0.0383(16) 0.0428(17) -0.0042(13) 0.0101(14) 0.0045(14) C7 0.0323(13) 0.0343(13) 0.0308(13) -0.0007(10) -0.0019(11) 0.0035(11) C8 0.0341(15) 0.060(2) 0.0346(15) -0.0004(13) 0.0030(12) 0.0023(14) C9 0.0373(15) 0.0415(16) 0.0360(14) 0.0034(12) 0.0038(12) -0.0020(12) C10 0.0448(18) 0.0464(18) 0.055(2) 0.0107(15) 0.0097(15) 0.0028(13) C11 0.0363(15) 0.0493(17) 0.0367(15) -0.0021(13) 0.0015(12) -0.0032(13) C12 0.0324(14) 0.0540(19) 0.0347(15) 0.0008(13) 0.0031(11) 0.0012(13) N1 0.0595(17) 0.0368(14) 0.0458(15) 0.0003(12) 0.0044(13) 0.0042(12) N2 0.0487(16) 0.0437(15) 0.0457(15) 0.0021(12) -0.0087(12) -0.0010(12) N3 0.0528(16) 0.0396(14) 0.0398(14) -0.0036(11) 0.0138(12) 0.0030(12) N4 0.0392(13) 0.0419(13) 0.0395(13) 0.0027(11) 0.0072(10) -0.0002(11) N5 0.0427(15) 0.0453(15) 0.0503(16) 0.0166(12) 0.0095(12) 0.0046(12) N6 0.0397(13) 0.0417(13) 0.0349(12) 0.0009(10) 0.0026(11) -0.0036(11) N7 0.074(3) 0.093(3) 0.0528(19) -0.0011(19) -0.0156(17) -0.033(2) N1M 0.083(2) 0.0524(18) 0.0413(16) 0.0066(13) 0.0173(15) 0.0153(16) N2MA 0.046(2) 0.046(2) 0.065(3) 0.000 0.000 -0.0047(18) N3M 0.054(7) 0.038(7) 0.027(6) -0.004(5) -0.006(6) 0.006(7) N2MB 0.050(6) 0.062(8) 0.073(7) -0.013(7) 0.006(8) -0.008(7) Ni1 0.0440(2) 0.03194(18) 0.03164(16) -0.00342(15) 0.00570(16) 0.00027(16) O1 0.0748(19) 0.0557(16) 0.0638(17) 0.0055(13) 0.0118(15) -0.0086(14) O2 0.0426(11) 0.0376(10) 0.0297(10) -0.0021(8) 0.0009(8) -0.0029(9) O3 0.0530(15) 0.0655(17) 0.0522(14) 0.0218(12) -0.0059(11) -0.0046(12) O1M 0.138(3) 0.072(2) 0.0442(16) 0.0156(15) 0.0179(18) 0.011(2) O2M 0.110(2) 0.0440(13) 0.0366(12) 0.0006(10) 0.0171(14) 0.0042(14) O3M 0.116(2) 0.0556(15) 0.0385(12) -0.0050(13) 0.0041(16) 0.0069(15) O4MA 0.095(3) 0.102(3) 0.312(9) -0.111(5) -0.086(4) 0.027(3) O5MA 0.311(14) 0.141(7) 0.078(5) 0.000 0.000 0.065(8) O9M 0.117(10) 0.127(10) 0.110(10) -0.012(8) 0.006(8) -0.030(8) O7M 0.067(6) 0.045(5) 0.048(6) -0.015(5) -0.032(5) 0.029(5) O8M 0.103(8) 0.069(7) 0.046(6) -0.006(6) 0.007(6) -0.001(6) O4MB 0.054(6) 0.065(6) 0.052(6) -0.007(5) 0.002(5) -0.004(5) O5MB 0.082(8) 0.109(9) 0.093(8) -0.028(8) 0.023(7) -0.017(7) O6MB 0.094(10) 0.087(9) 0.084(9) -0.005(8) -0.015(7) 0.022(8) _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 C2 1.497(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.240(5) . ? C2 N1 1.339(5) . ? C3 N1 1.459(5) . ? C3 C4 1.536(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.529(4) . ? C4 C6 1.531(5) . ? C4 C5 1.548(5) . ? C5 N2 1.460(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.459(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.245(4) . ? C7 N4 1.322(4) . ? C8 N4 1.467(4) . ? C8 C9 1.553(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.523(4) . ? C9 C11 1.530(5) . ? C9 C10 1.530(4) . ? C10 N5 1.459(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.467(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.211(4) . ? C12 N7 1.338(5) . ? N1 H1 0.8600 . ? N2 Ni1 2.116(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.073(3) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.097(3) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.082(3) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N1M O1M 1.220(4) . ? N1M O3M 1.228(4) . ? N1M O2M 1.281(4) . ? N2MA O4MA 1.161(5) . ? N2MA O4MA 1.161(5) 2_675 ? N2MA O5MA 1.181(8) . ? N3M O7M 1.188(13) . ? N3M O9M 1.193(13) . ? N3M O8M 1.206(13) . ? N2MB O5MB 1.188(13) . ? N2MB O4MB 1.198(14) . ? N2MB O6MB 1.24(3) . ? Ni1 O2 2.050(2) . ? Ni1 N6 2.082(3) 8_646 ? Ni1 N5 2.097(3) 8_646 ? Ni1 O2M 2.130(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.3(4) . . ? O1 C2 C1 122.3(4) . . ? N1 C2 C1 115.3(4) . . ? N1 C3 C4 114.1(3) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C6 109.5(2) . . ? C7 C4 C3 113.5(3) . . ? C6 C4 C3 108.8(3) . . ? C7 C4 C5 106.7(2) . . ? C6 C4 C5 111.7(3) . . ? C3 C4 C5 106.8(3) . . ? N2 C5 C4 113.5(3) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 113.9(3) . . ? N3 C6 H6A 108.8 . . ? C4 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N4 120.5(3) . . ? O2 C7 C4 118.9(2) . . ? N4 C7 C4 120.6(3) . . ? N4 C8 C9 114.1(3) . . ? N4 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N4 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C12 C9 C11 109.4(3) . . ? C12 C9 C10 116.7(3) . . ? C11 C9 C10 111.9(3) . . ? C12 C9 C8 107.4(2) . . ? C11 C9 C8 105.0(3) . . ? C10 C9 C8 105.5(3) . . ? N5 C10 C9 117.0(3) . . ? N5 C10 H10A 108.1 . . ? C9 C10 H10A 108.1 . . ? N5 C10 H10B 108.1 . . ? C9 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N6 C11 C9 114.7(3) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 121.6(3) . . ? O3 C12 C9 119.9(3) . . ? N7 C12 C9 118.5(3) . . ? C2 N1 C3 122.8(3) . . ? C2 N1 H1 118.6 . . ? C3 N1 H1 118.6 . . ? C5 N2 Ni1 115.8(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 115.7(2) . . ? C6 N3 H3C 108.3 . . ? Ni1 N3 H3C 108.3 . . ? C6 N3 H3D 108.3 . . ? Ni1 N3 H3D 108.3 . . ? H3C N3 H3D 107.4 . . ? C7 N4 C8 119.3(3) . . ? C7 N4 H4 120.4 . . ? C8 N4 H4 120.4 . . ? C10 N5 Ni1 124.1(2) . 7_566 ? C10 N5 H5C 106.3 . . ? Ni1 N5 H5C 106.3 7_566 . ? C10 N5 H5D 106.3 . . ? Ni1 N5 H5D 106.3 7_566 . ? H5C N5 H5D 106.4 . . ? C11 N6 Ni1 118.2(2) . 7_566 ? C11 N6 H6C 107.8 . . ? Ni1 N6 H6C 107.8 7_566 . ? C11 N6 H6D 107.8 . . ? Ni1 N6 H6D 107.8 7_566 . ? H6C N6 H6D 107.1 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O1M N1M O3M 121.3(3) . . ? O1M N1M O2M 118.6(3) . . ? O3M N1M O2M 120.1(3) . . ? O4MA N2MA O4MA 120.9(9) . 2_675 ? O4MA N2MA O5MA 119.5(5) . . ? O4MA N2MA O5MA 119.5(5) 2_675 . ? O7M N3M O9M 123.8(15) . . ? O7M N3M O8M 116.0(14) . . ? O9M N3M O8M 115.7(13) . . ? O5MB N2MB O4MB 120.6(17) . . ? O5MB N2MB O6MB 118(2) . . ? O4MB N2MB O6MB 117(2) . . ? O2 Ni1 N3 88.15(10) . . ? O2 Ni1 N6 91.96(9) . 8_646 ? N3 Ni1 N6 176.97(13) . 8_646 ? O2 Ni1 N5 85.64(10) . 8_646 ? N3 Ni1 N5 91.14(12) . 8_646 ? N6 Ni1 N5 91.88(10) 8_646 8_646 ? O2 Ni1 N2 83.33(10) . . ? N3 Ni1 N2 87.25(13) . . ? N6 Ni1 N2 89.76(11) 8_646 . ? N5 Ni1 N2 168.89(12) 8_646 . ? O2 Ni1 O2M 176.38(12) . . ? N3 Ni1 O2M 94.31(11) . . ? N6 Ni1 O2M 85.44(11) 8_646 . ? N5 Ni1 O2M 96.95(13) 8_646 . ? N2 Ni1 O2M 94.13(12) . . ? C7 O2 Ni1 120.11(18) . . ? N1M O2M Ni1 123.9(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.484 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.059 #===END data_i-4_333K _database_code_depnum_ccdc_archive 'CCDC 856064' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.6824(8) _cell_length_b 14.6824(8) _cell_length_c 18.985(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4092.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 333 _cell_measurement_reflns_used 7415 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.28 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8544 _exptl_absorpt_correction_T_max 0.9053 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas. ; _diffrn_ambient_temperature 333 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 13641 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.59 _reflns_number_total 5179 _reflns_number_gt 4279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.0419P)^2^+4.6753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.058(15) _refine_ls_number_reflns 5179 _refine_ls_number_parameters 336 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.093 _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 0.6668(4) 1.0876(3) 0.7713(3) 0.0743(13) Uani 1 1 d . . . H1A H 0.6716 1.1516 0.7810 0.111 Uiso 1 1 calc R . . H1B H 0.6103 1.0649 0.7898 0.111 Uiso 1 1 calc R . . H1C H 0.6686 1.0779 0.7214 0.111 Uiso 1 1 calc R . . C2 C 0.7443(3) 1.0386(2) 0.8053(2) 0.0541(9) Uani 1 1 d . . . C3 C 0.7921(3) 0.9473(2) 0.9072(2) 0.0515(8) Uani 1 1 d . . . H3A H 0.7902 0.9706 0.9550 0.062 Uiso 1 1 calc R . . H3B H 0.8519 0.9607 0.8881 0.062 Uiso 1 1 calc R . . C4 C 0.7795(2) 0.8434(2) 0.90948(18) 0.0401(6) Uani 1 1 d . . . C5 C 0.8561(3) 0.8053(2) 0.9570(2) 0.0512(9) Uani 1 1 d . . . H5A H 0.9127 0.8360 0.9455 0.061 Uiso 1 1 calc R . . H5B H 0.8417 0.8191 1.0057 0.061 Uiso 1 1 calc R . . C6 C 0.6850(3) 0.8216(2) 0.9388(2) 0.0479(8) Uani 1 1 d . . . H6A H 0.6722 0.8628 0.9775 0.057 Uiso 1 1 calc R . . H6B H 0.6402 0.8328 0.9023 0.057 Uiso 1 1 calc R . . C7 C 0.7907(2) 0.7978(2) 0.83746(16) 0.0349(6) Uani 1 1 d . . . C8 C 0.8472(2) 0.7935(3) 0.71842(19) 0.0463(8) Uani 1 1 d . . . H8A H 0.8213 0.8296 0.6806 0.056 Uiso 1 1 calc R . . H8B H 0.8149 0.7359 0.7196 0.056 Uiso 1 1 calc R . . C9 C 0.9490(2) 0.7748(2) 0.70151(18) 0.0415(7) Uani 1 1 d . . . C10 C 0.9843(3) 0.8613(3) 0.6656(2) 0.0526(9) Uani 1 1 d . . . H10A H 0.9426 0.8767 0.6278 0.063 Uiso 1 1 calc R . . H10B H 0.9820 0.9105 0.6996 0.063 Uiso 1 1 calc R . . C11 C 0.9482(2) 0.6934(3) 0.65115(19) 0.0441(7) Uani 1 1 d . . . H11A H 0.9124 0.6450 0.6722 0.053 Uiso 1 1 calc R . . H11B H 0.9180 0.7115 0.6079 0.053 Uiso 1 1 calc R . . C12 C 0.9956(2) 0.7476(3) 0.76993(18) 0.0440(7) Uani 1 1 d . . . N1 N 0.7237(2) 0.9949(2) 0.86529(17) 0.0513(7) Uani 1 1 d . . . H1 H 0.6681 0.9949 0.8796 0.062 Uiso 1 1 calc R . . N2 N 0.8695(2) 0.7074(2) 0.94996(17) 0.0490(7) Uani 1 1 d . . . H2A H 0.8864 0.6852 0.9922 0.059 Uiso 1 1 calc R . . H2B H 0.9159 0.6979 0.9199 0.059 Uiso 1 1 calc R . . N3 N 0.6749(2) 0.7284(2) 0.96365(16) 0.0477(7) Uani 1 1 d . . . H3C H 0.6162 0.7120 0.9584 0.057 Uiso 1 1 calc R . . H3D H 0.6874 0.7273 1.0100 0.057 Uiso 1 1 calc R . . N4 N 0.8323(2) 0.8410(2) 0.78535(15) 0.0439(6) Uani 1 1 d . . . H4 H 0.8503 0.8963 0.7907 0.053 Uiso 1 1 calc R . . N5 N 1.0757(2) 0.8582(2) 0.63657(17) 0.0498(7) Uani 1 1 d . . . H5C H 1.1136 0.8720 0.6722 0.060 Uiso 1 1 calc R . . H5D H 1.0794 0.9046 0.6057 0.060 Uiso 1 1 calc R . . N6 N 1.03837(19) 0.65717(19) 0.63338(15) 0.0418(6) Uani 1 1 d . . . H6C H 1.0303 0.6092 0.6046 0.050 Uiso 1 1 calc R . . H6D H 1.0637 0.6359 0.6733 0.050 Uiso 1 1 calc R . . N7 N 1.0522(3) 0.8065(3) 0.8004(2) 0.0809(13) Uani 1 1 d . . . H7A H 1.0777 0.7929 0.8399 0.097 Uiso 1 1 calc R . . H7B H 1.0633 0.8580 0.7807 0.097 Uiso 1 1 calc R . . N1M N 0.7593(3) 0.5674(2) 1.06619(17) 0.0638(9) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9691(3) 0.0589(11) Uani 1 2 d SD . . N3M N 0.5001(17) 0.5020(12) 1.0002(11) 0.0579(17) Uani 0.25 1 d PDU A -1 N2MB N 0.995(3) 0.0067(15) 0.9637(9) 0.068(5) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75565(3) 0.63197(3) 0.91415(2) 0.03840(10) Uani 1 1 d . . . O1 O 0.8213(2) 1.0369(2) 0.77951(17) 0.0708(8) Uani 1 1 d . . . O2 O 0.76350(16) 0.71836(15) 0.82944(11) 0.0392(5) Uani 1 1 d . . . O3 O 0.9787(2) 0.6745(2) 0.79654(16) 0.0630(7) Uani 1 1 d . . . O1M O 0.7454(3) 0.5112(3) 1.11222(17) 0.0926(13) Uani 1 1 d . . . O2M O 0.7564(3) 0.54119(19) 1.00188(14) 0.0674(9) Uani 1 1 d . . . O3M O 0.7761(3) 0.6471(2) 1.08051(15) 0.0774(9) Uani 1 1 d D . . O4MA O 0.5687(3) 1.0022(4) 0.9991(5) 0.177(3) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9063(4) 0.183(5) Uani 1 2 d SD . . O9M O 0.4977(13) 0.5778(9) 0.9736(9) 0.064(4) Uani 0.25 1 d PDU A -1 O7M O 0.5465(18) 0.4409(15) 0.9752(12) 0.112(7) Uani 0.25 1 d PDU A -1 O8M O 0.4551(12) 0.4856(10) 1.0528(7) 0.074(4) Uani 0.25 1 d PDU A -1 O4MB O 0.9635(11) 0.0793(10) 0.9417(7) 0.067(4) Uani 0.25 1 d PDU B -2 O5MB O 1.0176(13) -0.0504(11) 0.9211(9) 0.097(5) Uani 0.25 1 d PDU B -2 O6MB O 0.9736(17) -0.0168(16) 1.0240(9) 0.100(7) Uani 0.25 1 d PDU B -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 0.109(4) 0.051(2) 0.063(3) 0.012(2) -0.009(3) 0.011(2) C2 0.075(3) 0.0321(16) 0.055(2) -0.0019(15) 0.0017(19) -0.0043(16) C3 0.068(2) 0.0373(16) 0.0495(19) 0.0000(16) -0.0068(18) -0.0015(14) C4 0.0505(18) 0.0335(14) 0.0361(14) -0.0043(14) 0.0015(15) 0.0011(11) C5 0.066(2) 0.0428(18) 0.0453(19) -0.0027(15) -0.0152(17) -0.0020(16) C6 0.059(2) 0.0404(17) 0.0441(18) -0.0039(14) 0.0122(16) 0.0047(15) C7 0.0343(14) 0.0380(15) 0.0325(14) -0.0003(11) -0.0009(11) 0.0039(12) C8 0.0361(16) 0.064(2) 0.0391(17) 0.0003(15) 0.0046(13) 0.0039(15) C9 0.0399(16) 0.0451(17) 0.0395(16) 0.0039(13) 0.0041(13) -0.0011(13) C10 0.048(2) 0.050(2) 0.060(2) 0.0109(17) 0.0106(17) 0.0033(15) C11 0.0380(16) 0.0536(19) 0.0407(16) -0.0038(14) 0.0017(13) -0.0041(14) C12 0.0344(15) 0.059(2) 0.0386(16) 0.0013(15) 0.0039(13) 0.0017(14) N1 0.0639(19) 0.0394(15) 0.0508(17) 0.0002(13) 0.0061(15) 0.0042(13) N2 0.0523(17) 0.0452(16) 0.0496(16) 0.0021(13) -0.0099(14) -0.0014(13) N3 0.0571(18) 0.0430(15) 0.0430(16) -0.0047(12) 0.0149(14) 0.0020(13) N4 0.0429(15) 0.0445(15) 0.0442(15) 0.0031(12) 0.0091(12) -0.0011(12) N5 0.0465(16) 0.0487(16) 0.0542(17) 0.0163(13) 0.0102(13) 0.0056(13) N6 0.0437(15) 0.0441(15) 0.0376(14) 0.0011(11) 0.0040(12) -0.0040(12) N7 0.082(3) 0.102(3) 0.059(2) -0.002(2) -0.018(2) -0.037(2) N1M 0.089(3) 0.058(2) 0.0452(18) 0.0068(15) 0.0185(17) 0.0159(18) N2MA 0.052(3) 0.049(3) 0.076(3) 0.000 0.000 -0.005(2) N3M 0.068(6) 0.054(6) 0.051(4) 0.002(8) 0.012(8) 0.008(8) N2MB 0.054(7) 0.064(8) 0.085(7) -0.011(7) 0.002(7) -0.002(6) Ni1 0.0468(2) 0.03420(19) 0.03424(17) -0.00372(16) 0.00584(17) 0.00011(17) O1 0.082(2) 0.0600(18) 0.0702(19) 0.0068(15) 0.0131(17) -0.0095(15) O2 0.0465(12) 0.0392(11) 0.0318(10) -0.0024(9) 0.0013(9) -0.0036(9) O3 0.0588(17) 0.0713(19) 0.0588(16) 0.0261(14) -0.0073(13) -0.0053(14) O1M 0.152(4) 0.078(2) 0.0483(17) 0.0176(16) 0.019(2) 0.012(2) O2M 0.117(3) 0.0462(14) 0.0389(13) -0.0001(11) 0.0176(15) 0.0023(15) O3M 0.129(3) 0.0611(18) 0.0420(13) -0.0055(14) 0.0030(18) 0.0060(17) O4MA 0.100(3) 0.104(3) 0.327(9) -0.111(5) -0.087(5) 0.024(3) O5MA 0.315(15) 0.151(8) 0.083(5) 0.000 0.000 0.062(9) O9M 0.074(7) 0.044(5) 0.075(7) 0.008(5) 0.020(6) 0.015(5) O7M 0.119(10) 0.104(10) 0.113(10) 0.002(8) 0.022(8) 0.018(8) O8M 0.103(8) 0.062(7) 0.055(6) -0.004(6) 0.017(6) 0.005(6) O4MB 0.065(7) 0.072(7) 0.062(6) -0.008(6) 0.004(5) -0.001(6) O5MB 0.082(8) 0.108(9) 0.101(8) -0.029(8) 0.018(7) -0.017(7) O6MB 0.103(10) 0.093(9) 0.105(9) -0.004(8) -0.014(8) 0.026(8) _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 C2 1.492(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.233(5) . ? C2 N1 1.343(5) . ? C3 N1 1.459(5) . ? C3 C4 1.537(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C6 1.529(5) . ? C4 C7 1.531(4) . ? C4 C5 1.546(5) . ? C5 N2 1.456(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.454(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.242(4) . ? C7 N4 1.324(4) . ? C8 N4 1.466(5) . ? C8 C9 1.554(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.521(5) . ? C9 C11 1.530(5) . ? C9 C10 1.532(5) . ? C10 N5 1.451(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.466(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.212(5) . ? C12 N7 1.332(5) . ? N1 H1 0.8600 . ? N2 Ni1 2.117(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.073(3) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.099(3) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.084(3) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N1M O1M 1.219(5) . ? N1M O3M 1.227(5) . ? N1M O2M 1.281(4) . ? N2MA O4MA 1.159(5) 2_675 ? N2MA O4MA 1.159(5) . ? N2MA O5MA 1.191(8) . ? N3M O8M 1.221(13) . ? N3M O9M 1.221(13) . ? N3M O7M 1.222(13) . ? N2MB O5MB 1.214(13) . ? N2MB O4MB 1.232(14) . ? N2MB O6MB 1.234(14) . ? Ni1 O2 2.051(2) . ? Ni1 N6 2.084(3) 8_646 ? Ni1 N5 2.099(3) 8_646 ? Ni1 O2M 2.133(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.2(4) . . ? O1 C2 C1 122.6(4) . . ? N1 C2 C1 115.2(4) . . ? N1 C3 C4 114.1(3) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C6 C4 C7 109.3(3) . . ? C6 C4 C3 109.1(3) . . ? C7 C4 C3 113.3(3) . . ? C6 C4 C5 111.8(3) . . ? C7 C4 C5 106.6(3) . . ? C3 C4 C5 106.7(3) . . ? N2 C5 C4 113.6(3) . . ? N2 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 114.1(3) . . ? N3 C6 H6A 108.7 . . ? C4 C6 H6A 108.7 . . ? N3 C6 H6B 108.7 . . ? C4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N4 120.4(3) . . ? O2 C7 C4 119.0(3) . . ? N4 C7 C4 120.5(3) . . ? N4 C8 C9 114.0(3) . . ? N4 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N4 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.6 . . ? C12 C9 C11 109.4(3) . . ? C12 C9 C10 116.4(3) . . ? C11 C9 C10 111.8(3) . . ? C12 C9 C8 107.6(3) . . ? C11 C9 C8 105.1(3) . . ? C10 C9 C8 105.7(3) . . ? N5 C10 C9 117.1(3) . . ? N5 C10 H10A 108.0 . . ? C9 C10 H10A 108.0 . . ? N5 C10 H10B 108.0 . . ? C9 C10 H10B 108.0 . . ? H10A C10 H10B 107.3 . . ? N6 C11 C9 114.9(3) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? O3 C12 N7 121.4(4) . . ? O3 C12 C9 119.8(3) . . ? N7 C12 C9 118.8(4) . . ? C2 N1 C3 122.5(4) . . ? C2 N1 H1 118.8 . . ? C3 N1 H1 118.8 . . ? C5 N2 Ni1 116.1(2) . . ? C5 N2 H2A 108.3 . . ? Ni1 N2 H2A 108.3 . . ? C5 N2 H2B 108.3 . . ? Ni1 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 115.9(2) . . ? C6 N3 H3C 108.3 . . ? Ni1 N3 H3C 108.3 . . ? C6 N3 H3D 108.3 . . ? Ni1 N3 H3D 108.3 . . ? H3C N3 H3D 107.4 . . ? C7 N4 C8 119.2(3) . . ? C7 N4 H4 120.4 . . ? C8 N4 H4 120.4 . . ? C10 N5 Ni1 124.3(3) . 7_566 ? C10 N5 H5C 106.3 . . ? Ni1 N5 H5C 106.3 7_566 . ? C10 N5 H5D 106.3 . . ? Ni1 N5 H5D 106.3 7_566 . ? H5C N5 H5D 106.4 . . ? C11 N6 Ni1 118.2(2) . 7_566 ? C11 N6 H6C 107.8 . . ? Ni1 N6 H6C 107.8 7_566 . ? C11 N6 H6D 107.8 . . ? Ni1 N6 H6D 107.8 7_566 . ? H6C N6 H6D 107.1 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O1M N1M O3M 121.4(3) . . ? O1M N1M O2M 118.4(4) . . ? O3M N1M O2M 120.3(3) . . ? O4MA N2MA O4MA 121.2(10) 2_675 . ? O4MA N2MA O5MA 119.4(5) 2_675 . ? O4MA N2MA O5MA 119.4(5) . . ? O8M N3M O9M 120.2(14) . . ? O8M N3M O7M 118.2(14) . . ? O9M N3M O7M 121.6(14) . . ? O5MB N2MB O4MB 118.4(15) . . ? O5MB N2MB O6MB 119.7(18) . . ? O4MB N2MB O6MB 117.6(15) . . ? O2 Ni1 N3 88.00(11) . . ? O2 Ni1 N6 91.94(10) . 8_646 ? N3 Ni1 N6 176.99(13) . 8_646 ? O2 Ni1 N5 85.91(11) . 8_646 ? N3 Ni1 N5 91.23(13) . 8_646 ? N6 Ni1 N5 91.77(11) 8_646 8_646 ? O2 Ni1 N2 83.33(11) . . ? N3 Ni1 N2 87.04(14) . . ? N6 Ni1 N2 89.96(12) 8_646 . ? N5 Ni1 N2 169.15(13) 8_646 . ? O2 Ni1 O2M 176.46(13) . . ? N3 Ni1 O2M 94.36(12) . . ? N6 Ni1 O2M 85.57(12) 8_646 . ? N5 Ni1 O2M 96.67(14) 8_646 . ? N2 Ni1 O2M 94.15(13) . . ? C7 O2 Ni1 120.2(2) . . ? N1M O2M Ni1 123.9(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.59 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.531 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.059 #===END data_i-4_93K_after_333K _database_code_depnum_ccdc_archive 'CCDC 856065' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.567(7) _cell_length_b 14.567(7) _cell_length_c 18.717(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3972(3) _cell_formula_units_Z 2 _cell_measurement_temperature 93 _cell_measurement_reflns_used 981 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 16.45 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8847 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was measured under dry N2 gas after heating up to 333K. In cooling process, the sample was always set under dry N2 gas. ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 10416 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.1248 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3521 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.1140P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 3521 _refine_ls_number_parameters 336 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.023 _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 0.6599(11) 1.0893(8) 0.7729(7) 0.073(4) Uani 1 1 d . . . H1A H 0.6736 1.1548 0.7677 0.110 Uiso 1 1 calc R . . H1B H 0.6060 1.0816 0.8037 0.110 Uiso 1 1 calc R . . H1C H 0.6473 1.0628 0.7258 0.110 Uiso 1 1 calc R . . C2 C 0.7403(9) 1.0416(7) 0.8058(6) 0.047(3) Uani 1 1 d . . . C3 C 0.7856(8) 0.9504(8) 0.9097(6) 0.057(3) Uani 1 1 d . . . H3A H 0.7835 0.9744 0.9591 0.069 Uiso 1 1 calc R . . H3B H 0.8465 0.9659 0.8896 0.069 Uiso 1 1 calc R . . C4 C 0.7765(7) 0.8473(8) 0.9124(6) 0.048(3) Uani 1 1 d . . . C5 C 0.8495(9) 0.8080(7) 0.9605(6) 0.054(3) Uani 1 1 d . . . H5A H 0.9072 0.8425 0.9527 0.064 Uiso 1 1 calc R . . H5B H 0.8307 0.8178 1.0108 0.064 Uiso 1 1 calc R . . C6 C 0.6818(9) 0.8210(8) 0.9394(6) 0.055(3) Uani 1 1 d . . . H6A H 0.6645 0.8639 0.9781 0.066 Uiso 1 1 calc R . . H6B H 0.6372 0.8294 0.9000 0.066 Uiso 1 1 calc R . . C7 C 0.7889(7) 0.7985(7) 0.8381(5) 0.034(2) Uani 1 1 d . . . C8 C 0.8485(8) 0.7987(9) 0.7179(6) 0.054(3) Uani 1 1 d . . . H8A H 0.8256 0.8375 0.6783 0.065 Uiso 1 1 calc R . . H8B H 0.8125 0.7410 0.7179 0.065 Uiso 1 1 calc R . . C9 C 0.9506(8) 0.7758(8) 0.7046(6) 0.051(3) Uani 1 1 d . . . C10 C 0.9870(9) 0.8653(9) 0.6674(7) 0.067(4) Uani 1 1 d . . . H10A H 0.9444 0.8815 0.6281 0.080 Uiso 1 1 calc R . . H10B H 0.9854 0.9160 0.7025 0.080 Uiso 1 1 calc R . . C11 C 0.9481(7) 0.6954(7) 0.6508(5) 0.039(2) Uani 1 1 d . . . H11A H 0.9089 0.6460 0.6706 0.047 Uiso 1 1 calc R . . H11B H 0.9194 0.7170 0.6060 0.047 Uiso 1 1 calc R . . C12 C 0.9946(8) 0.7441(9) 0.7746(6) 0.048(3) Uani 1 1 d . . . N1 N 0.7167(7) 0.9965(6) 0.8684(4) 0.051(2) Uani 1 1 d . . . H1 H 0.6592 0.9962 0.8828 0.061 Uiso 1 1 calc R . . N2 N 0.8680(7) 0.7091(6) 0.9498(4) 0.049(2) Uani 1 1 d . . . H2A H 0.8882 0.6845 0.9922 0.059 Uiso 1 1 calc R . . H2B H 0.9147 0.7030 0.9170 0.059 Uiso 1 1 calc R . . N3 N 0.6730(8) 0.7284(6) 0.9661(5) 0.058(3) Uani 1 1 d . . . H3C H 0.6126 0.7105 0.9620 0.070 Uiso 1 1 calc R . . H3D H 0.6877 0.7281 1.0139 0.070 Uiso 1 1 calc R . . N4 N 0.8332(6) 0.8474(6) 0.7869(4) 0.042(2) Uani 1 1 d . . . H4 H 0.8517 0.9042 0.7940 0.051 Uiso 1 1 calc R . . N5 N 1.0786(7) 0.8590(7) 0.6386(6) 0.062(3) Uani 1 1 d . . . H5C H 1.1176 0.8708 0.6761 0.075 Uiso 1 1 calc R . . H5D H 1.0845 0.9076 0.6075 0.075 Uiso 1 1 calc R . . N6 N 1.0378(6) 0.6573(6) 0.6344(4) 0.044(2) Uani 1 1 d . . . H6C H 1.0295 0.6075 0.6049 0.053 Uiso 1 1 calc R . . H6D H 1.0632 0.6360 0.6762 0.053 Uiso 1 1 calc R . . N7 N 1.0505(8) 0.8035(8) 0.8050(6) 0.072(3) Uani 1 1 d . . . H7A H 1.0778 0.7895 0.8455 0.087 Uiso 1 1 calc R . . H7B H 1.0606 0.8570 0.7847 0.087 Uiso 1 1 calc R . . N1M N 0.7603(8) 0.5683(9) 1.0697(5) 0.076(3) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9690(6) 0.052(3) Uani 1 2 d SD . . N3M N 0.4980(17) 0.4793(15) 1.0116(13) 0.037(7) Uani 0.25 1 d PDU A -1 N2MB N 1.012(3) 0.015(4) 0.9623(16) 0.084(6) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75458(10) 0.63308(9) 0.91422(7) 0.0459(4) Uani 1 1 d . . . O1 O 0.8173(7) 1.0399(5) 0.7808(4) 0.065(2) Uani 1 1 d . . . O2 O 0.7626(5) 0.7204(5) 0.8286(3) 0.0379(16) Uani 1 1 d . . . O3 O 0.9767(5) 0.6708(6) 0.7975(4) 0.052(2) Uani 1 1 d . . . O1M O 0.7473(8) 0.5122(7) 1.1143(4) 0.080(3) Uani 1 1 d . . . O2M O 0.7559(8) 0.5408(6) 1.0030(4) 0.080(3) Uani 1 1 d . . . O3M O 0.7820(6) 0.6471(6) 1.0821(4) 0.070(2) Uani 1 1 d D . . O4MA O 0.5720(7) 1.0033(8) 1.0024(6) 0.099(4) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9035(6) 0.108(5) Uani 1 2 d SD . . O9M O 0.5688(18) 0.523(2) 1.0190(14) 0.035(7) Uani 0.25 1 d PDU A -1 O7M O 0.493(2) 0.419(2) 0.966(2) 0.062(10) Uani 0.25 1 d PDU A -1 O8M O 0.4409(19) 0.479(2) 1.0603(15) 0.054(8) Uani 0.25 1 d PDU A -1 O4MB O 1.028(3) -0.053(3) 0.926(2) 0.084(7) Uani 0.25 1 d PDU B -2 O5MB O 0.961(3) 0.076(3) 0.9408(19) 0.083(7) Uani 0.25 1 d PDU B -2 O6MB O 1.033(3) 0.013(4) 1.0266(16) 0.085(7) Uani 0.25 1 d PDU B -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 0.134(13) 0.046(8) 0.039(7) 0.003(6) 0.004(8) -0.013(8) C2 0.076(9) 0.026(6) 0.038(7) -0.006(5) -0.001(6) -0.010(6) C3 0.086(9) 0.062(8) 0.023(5) 0.002(6) 0.005(6) -0.020(6) C4 0.065(7) 0.057(7) 0.023(5) -0.016(6) -0.002(6) 0.003(5) C5 0.095(10) 0.032(6) 0.033(7) -0.012(5) -0.014(6) -0.016(6) C6 0.082(9) 0.058(8) 0.025(6) -0.008(5) 0.004(5) -0.004(6) C7 0.037(6) 0.050(7) 0.016(5) 0.016(4) -0.008(4) -0.001(5) C8 0.069(8) 0.069(8) 0.024(6) 0.006(5) 0.006(5) 0.002(6) C9 0.051(7) 0.065(8) 0.037(7) -0.003(5) -0.001(5) -0.004(6) C10 0.075(10) 0.082(10) 0.043(7) 0.000(6) -0.009(6) 0.001(7) C11 0.040(6) 0.054(7) 0.024(5) -0.009(5) 0.000(4) -0.005(5) C12 0.046(7) 0.058(9) 0.040(7) -0.013(6) 0.018(5) -0.003(6) N1 0.075(7) 0.056(6) 0.022(5) -0.001(4) 0.005(4) -0.008(5) N2 0.070(7) 0.053(6) 0.025(5) 0.002(4) -0.010(4) 0.003(5) N3 0.084(8) 0.065(7) 0.024(5) -0.014(5) 0.012(5) -0.003(6) N4 0.056(6) 0.045(5) 0.027(5) -0.001(4) 0.000(4) -0.003(4) N5 0.052(6) 0.060(7) 0.075(8) 0.019(5) 0.010(5) 0.013(5) N6 0.047(5) 0.070(6) 0.015(4) 0.002(4) -0.001(4) -0.002(5) N7 0.073(8) 0.086(8) 0.058(7) -0.011(6) -0.015(6) -0.008(6) N1M 0.103(9) 0.086(9) 0.039(7) 0.011(7) 0.023(6) 0.037(8) N2MA 0.060(10) 0.057(9) 0.039(8) 0.000 0.000 -0.003(7) N3M 0.040(9) 0.037(10) 0.034(10) 0.000(7) -0.008(8) 0.007(8) N2MB 0.084(7) 0.084(7) 0.084(7) 0.0000(8) 0.0001(8) 0.0001(8) Ni1 0.0659(10) 0.0486(9) 0.0233(6) -0.0028(6) 0.0065(7) 0.0009(7) O1 0.099(7) 0.054(5) 0.043(5) -0.003(4) 0.016(5) -0.013(5) O2 0.047(4) 0.038(4) 0.029(4) 0.001(3) -0.005(3) -0.002(3) O3 0.056(5) 0.079(6) 0.021(4) 0.004(4) 0.001(3) -0.009(4) O1M 0.133(9) 0.085(7) 0.024(4) 0.017(5) 0.025(5) 0.034(6) O2M 0.157(9) 0.059(6) 0.022(4) -0.008(4) 0.022(5) 0.004(6) O3M 0.117(7) 0.062(6) 0.030(4) -0.011(5) 0.005(5) 0.005(5) O4MA 0.084(8) 0.096(8) 0.119(10) -0.046(7) -0.017(7) 0.009(6) O5MA 0.216(18) 0.093(10) 0.016(7) 0.000 0.000 0.019(11) O9M 0.046(10) 0.038(10) 0.023(9) 0.012(8) 0.006(8) 0.002(8) O7M 0.065(12) 0.061(12) 0.061(12) -0.001(9) -0.008(9) -0.004(9) O8M 0.064(11) 0.053(11) 0.046(11) -0.002(8) -0.004(8) 0.013(8) O4MB 0.084(7) 0.084(7) 0.084(7) -0.0004(9) 0.0002(9) -0.0001(9) O5MB 0.083(7) 0.083(7) 0.083(7) 0.0001(9) 0.0000(9) 0.0001(9) O6MB 0.085(7) 0.085(7) 0.085(7) 0.0001(9) 0.0002(9) 0.0001(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 C2 1.494(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.214(14) . ? C2 N1 1.388(14) . ? C3 N1 1.434(15) . ? C3 C4 1.509(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.506(15) . ? C4 C6 1.520(16) . ? C4 C7 1.571(14) . ? C5 N2 1.480(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.444(14) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.214(11) . ? C7 N4 1.357(12) . ? C8 N4 1.491(14) . ? C8 C9 1.546(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.529(16) . ? C9 C11 1.545(15) . ? C9 C10 1.570(17) . ? C10 N5 1.442(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N6 1.453(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.180(13) . ? C12 N7 1.316(15) . ? N1 H1 0.8800 . ? N2 Ni1 2.097(9) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 Ni1 2.069(9) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4 0.8800 . ? N5 Ni1 2.084(10) 7_566 ? N5 H5C 0.9200 . ? N5 H5D 0.9200 . ? N6 Ni1 2.097(8) 7_566 ? N6 H6C 0.9200 . ? N6 H6D 0.9200 . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? N1M O1M 1.184(12) . ? N1M O3M 1.213(11) . ? N1M O2M 1.311(13) . ? N2MA O4MA 1.222(9) . ? N2MA O4MA 1.222(9) 2_675 ? N2MA O5MA 1.226(12) . ? N3M O9M 1.223(15) . ? N3M O7M 1.227(15) . ? N3M O8M 1.235(15) . ? N2MB O4MB 1.224(15) . ? N2MB O5MB 1.228(16) . ? N2MB O6MB 1.239(15) . ? Ni1 O2 2.050(7) . ? Ni1 N5 2.084(10) 8_646 ? Ni1 N6 2.097(8) 8_646 ? Ni1 O2M 2.138(8) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 123.0(12) . . ? O1 C2 C1 125.1(12) . . ? N1 C2 C1 111.9(12) . . ? N1 C3 C4 115.0(9) . . ? N1 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N1 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 109.7(9) . . ? C5 C4 C6 110.3(10) . . ? C3 C4 C6 110.0(9) . . ? C5 C4 C7 106.1(8) . . ? C3 C4 C7 114.2(9) . . ? C6 C4 C7 106.6(8) . . ? N2 C5 C4 114.6(8) . . ? N2 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N3 C6 C4 115.5(10) . . ? N3 C6 H6A 108.4 . . ? C4 C6 H6A 108.4 . . ? N3 C6 H6B 108.4 . . ? C4 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N4 122.5(9) . . ? O2 C7 C4 121.2(8) . . ? N4 C7 C4 116.2(9) . . ? N4 C8 C9 112.7(9) . . ? N4 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C12 C9 C11 109.8(10) . . ? C12 C9 C8 109.3(9) . . ? C11 C9 C8 104.2(9) . . ? C12 C9 C10 119.3(10) . . ? C11 C9 C10 110.4(9) . . ? C8 C9 C10 102.6(10) . . ? N5 C10 C9 115.2(11) . . ? N5 C10 H10A 108.5 . . ? C9 C10 H10A 108.5 . . ? N5 C10 H10B 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N6 C11 C9 114.0(8) . . ? N6 C11 H11A 108.8 . . ? C9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? C9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? O3 C12 N7 125.0(12) . . ? O3 C12 C9 119.5(11) . . ? N7 C12 C9 115.5(12) . . ? C2 N1 C3 120.2(10) . . ? C2 N1 H1 119.9 . . ? C3 N1 H1 119.9 . . ? C5 N2 Ni1 114.4(7) . . ? C5 N2 H2A 108.6 . . ? Ni1 N2 H2A 108.6 . . ? C5 N2 H2B 108.6 . . ? Ni1 N2 H2B 108.6 . . ? H2A N2 H2B 107.6 . . ? C6 N3 Ni1 114.4(7) . . ? C6 N3 H3C 108.7 . . ? Ni1 N3 H3C 108.7 . . ? C6 N3 H3D 108.7 . . ? Ni1 N3 H3D 108.7 . . ? H3C N3 H3D 107.6 . . ? C7 N4 C8 115.6(9) . . ? C7 N4 H4 122.2 . . ? C8 N4 H4 122.2 . . ? C10 N5 Ni1 125.5(8) . 7_566 ? C10 N5 H5C 106.0 . . ? Ni1 N5 H5C 106.0 7_566 . ? C10 N5 H5D 106.0 . . ? Ni1 N5 H5D 106.0 7_566 . ? H5C N5 H5D 106.3 . . ? C11 N6 Ni1 117.0(6) . 7_566 ? C11 N6 H6C 108.0 . . ? Ni1 N6 H6C 108.0 7_566 . ? C11 N6 H6D 108.0 . . ? Ni1 N6 H6D 108.0 7_566 . ? H6C N6 H6D 107.3 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O1M N1M O3M 124.0(11) . . ? O1M N1M O2M 117.0(12) . . ? O3M N1M O2M 118.9(10) . . ? O4MA N2MA O4MA 118.4(15) . 2_675 ? O4MA N2MA O5MA 120.8(8) . . ? O4MA N2MA O5MA 120.8(7) 2_675 . ? O9M N3M O7M 120.2(15) . . ? O9M N3M O8M 119.2(14) . . ? O7M N3M O8M 118.2(14) . . ? O4MB N2MB O5MB 121.1(17) . . ? O4MB N2MB O6MB 118.7(16) . . ? O5MB N2MB O6MB 118.6(17) . . ? O2 Ni1 N3 89.0(3) . . ? O2 Ni1 N5 84.9(4) . 8_646 ? N3 Ni1 N5 91.3(4) . 8_646 ? O2 Ni1 N2 82.8(3) . . ? N3 Ni1 N2 87.1(4) . . ? N5 Ni1 N2 167.7(4) 8_646 . ? O2 Ni1 N6 92.1(3) . 8_646 ? N3 Ni1 N6 177.0(4) . 8_646 ? N5 Ni1 N6 91.6(4) 8_646 8_646 ? N2 Ni1 N6 90.3(3) . 8_646 ? O2 Ni1 O2M 176.2(4) . . ? N3 Ni1 O2M 93.6(4) . . ? N5 Ni1 O2M 97.8(4) 8_646 . ? N2 Ni1 O2M 94.5(4) . . ? N6 Ni1 O2M 85.2(3) 8_646 . ? C7 O2 Ni1 119.0(6) . . ? N1M O2M Ni1 123.2(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.126 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.110 #===END data_i-4_93K_after_333K_and_outside_dry_gas _database_code_depnum_ccdc_archive 'CCDC 856066' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.488(7) _cell_length_b 15.488(7) _cell_length_c 19.360(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4644(4) _cell_formula_units_Z 2 _cell_measurement_temperature 93 _cell_measurement_reflns_used 685 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 18.48 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8986 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; The crystal which measured at 333K under dry N2 gas was used for this measurement. After bringing out to normal condition, the sample was measured under dry N2 gas at 93K. ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 5322 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1562 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 24.95 _reflns_number_total 3871 _reflns_number_gt 2205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1212P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 3871 _refine_ls_number_parameters 345 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2304 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.023 _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 0.7137(10) 1.0903(10) 0.8061(9) 0.072(5) Uani 1 1 d . . . H1A H 0.6935 1.0738 0.7600 0.107 Uiso 1 1 calc R . . H1B H 0.7421 1.1468 0.8037 0.107 Uiso 1 1 calc R . . H1C H 0.6644 1.0935 0.8378 0.107 Uiso 1 1 calc R . . C2 C 0.7777(11) 1.0232(8) 0.8323(8) 0.051(4) Uani 1 1 d . . . C3 C 0.8100(9) 0.9083(8) 0.9148(7) 0.041(3) Uani 1 1 d . . . H3A H 0.8103 0.9183 0.9653 0.049 Uiso 1 1 calc R . . H3B H 0.8693 0.9184 0.8976 0.049 Uiso 1 1 calc R . . C4 C 0.7853(8) 0.8118(8) 0.9009(6) 0.035(3) Uani 1 1 d . . . C5 C 0.8510(9) 0.7580(8) 0.9400(7) 0.044(3) Uani 1 1 d . . . H5A H 0.9094 0.7818 0.9318 0.053 Uiso 1 1 calc R . . H5B H 0.8389 0.7619 0.9901 0.053 Uiso 1 1 calc R . . C6 C 0.6925(9) 0.7984(8) 0.9266(6) 0.040(3) Uani 1 1 d . . . H6A H 0.6837 0.8318 0.9696 0.049 Uiso 1 1 calc R . . H6B H 0.6515 0.8204 0.8915 0.049 Uiso 1 1 calc R . . C7 C 0.7904(8) 0.7925(9) 0.8249(6) 0.037(3) Uani 1 1 d . . . C8 C 0.8431(8) 0.8265(8) 0.7075(6) 0.037(3) Uani 1 1 d . . . H8B H 0.8232 0.8794 0.6837 0.044 Uiso 1 1 calc R . . H8A H 0.8042 0.7786 0.6942 0.044 Uiso 1 1 calc R . . C9 C 0.9374(7) 0.8047(8) 0.6833(6) 0.035(3) Uani 1 1 d . . . C10 C 0.9973(8) 0.8763(8) 0.7104(7) 0.038(3) Uani 1 1 d . . . H10B H 0.9674 0.9325 0.7062 0.045 Uiso 1 1 calc R . . H10A H 1.0087 0.8661 0.7601 0.045 Uiso 1 1 calc R . . C11 C 0.9312(7) 0.8065(7) 0.6031(5) 0.029(3) Uani 1 1 d . . . H11B H 0.8810 0.7713 0.5887 0.035 Uiso 1 1 calc R . . H11A H 0.9205 0.8666 0.5880 0.035 Uiso 1 1 calc R . . C12 C 0.9718(9) 0.7175(8) 0.7060(6) 0.035(3) Uani 1 1 d . . . N1 N 0.7521(7) 0.9710(6) 0.8826(5) 0.045(3) Uani 1 1 d . . . H1 H 0.6983 0.9742 0.8971 0.054 Uiso 1 1 calc R . . N2 N 0.8494(6) 0.6668(6) 0.9188(5) 0.037(2) Uani 1 1 d . . . H2A H 0.8601 0.6334 0.9572 0.044 Uiso 1 1 calc R . . H2B H 0.8940 0.6578 0.8883 0.044 Uiso 1 1 calc R . . N3 N 0.6743(6) 0.7063(6) 0.9400(5) 0.032(2) Uani 1 1 d . . . H3C H 0.6156 0.6977 0.9378 0.038 Uiso 1 1 calc R . . H3D H 0.6918 0.6932 0.9842 0.038 Uiso 1 1 calc R . . N4 N 0.8377(6) 0.8396(6) 0.7819(4) 0.031(2) Uani 1 1 d . . . H4 H 0.8682 0.8821 0.7997 0.037 Uiso 1 1 calc R . . N5 N 1.0811(6) 0.8813(6) 0.6732(5) 0.029(2) Uani 1 1 d . . . H5D H 1.1228 0.8992 0.7039 0.035 Uiso 1 1 calc R . . H5C H 1.0767 0.9227 0.6394 0.035 Uiso 1 1 calc R . . N6 N 1.0099(6) 0.7735(6) 0.5669(4) 0.031(2) Uani 1 1 d . . . H6D H 1.0209 0.8087 0.5297 0.037 Uiso 1 1 calc R . . H6C H 0.9981 0.7192 0.5501 0.037 Uiso 1 1 calc R . . N7 N 0.9175(7) 0.6621(7) 0.7392(5) 0.044(3) Uani 1 1 d . . . H7A H 0.9367 0.6116 0.7534 0.052 Uiso 1 1 calc R . . H7B H 0.8634 0.6767 0.7464 0.052 Uiso 1 1 calc R . . O4M O 0.1048(8) 0.6012(8) 0.9223(7) 0.067(4) Uani 0.75 1 d PDU . . Ni1 Ni 0.73358(9) 0.62218(10) 0.87234(7) 0.0317(4) Uani 1 1 d . . . O1 O 0.8514(6) 1.0192(6) 0.8056(5) 0.048(2) Uani 1 1 d . . . O2 O 0.7549(5) 0.7236(5) 0.8022(4) 0.0330(19) Uani 1 1 d . . . O3 O 1.0474(5) 0.6983(6) 0.6955(4) 0.035(2) Uani 1 1 d . . . O5M O 0.1613(8) 0.7338(8) 0.9052(7) 0.057(4) Uani 0.75 1 d PDU . . O6M O 0.0304(11) 0.7056(11) 0.8788(12) 0.128(7) Uani 0.75 1 d PDU . . O7M O 0.5139(11) 0.5690(9) -0.0334(8) 0.043(4) Uani 0.50 1 d PDU A -1 O2S O 0.0372(6) 0.8893(6) 0.8939(5) 0.058(3) Uani 1 1 d . . . O3S O 0.6015(9) 1.0070(10) 0.9584(8) 0.116(5) Uani 1 1 d . . . O1M O 0.4907(8) 0.7154(8) 0.8993(7) 0.107(4) Uani 1 1 d DU . . O3M O 0.3806(7) 0.7834(7) 0.9367(6) 0.080(3) Uani 1 1 d DU . . N1MA N 0.4527(8) 0.7846(8) 0.9057(9) 0.050(5) Uani 0.70(3) 1 d PDU B 1 O2MA O 0.4814(13) 0.8508(11) 0.8769(13) 0.136(10) Uani 0.70(3) 1 d PDU B 1 N1MB N 0.4598(11) 0.7820(12) 0.9257(15) 0.099(14) Uani 0.30(3) 1 d PDU B 2 O2MB O 0.5050(15) 0.8449(18) 0.944(3) 0.111(18) Uani 0.30(3) 1 d PDU B 2 N2M N 0.1016(10) 0.6803(9) 0.9036(8) 0.074(5) Uani 0.75 1 d PDU . . O8M O 0.483(2) 0.505(2) 0.0630(8) 0.036(8) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8340(10) 0.099(6) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.051(5) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.040(4) Uani 1 4 d SDU . . 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 0.053(10) 0.070(11) 0.091(13) 0.020(10) 0.040(9) 0.020(9) C2 0.079(12) 0.021(7) 0.053(9) -0.006(7) 0.007(9) -0.001(7) C3 0.045(9) 0.039(8) 0.038(7) -0.004(6) 0.013(6) 0.011(6) C4 0.040(8) 0.038(8) 0.026(6) -0.006(5) 0.004(5) -0.006(6) C5 0.061(9) 0.028(7) 0.044(8) 0.001(6) -0.014(7) -0.020(7) C6 0.061(9) 0.023(7) 0.037(7) -0.005(6) 0.003(6) -0.003(6) C7 0.028(7) 0.039(8) 0.043(8) 0.007(6) 0.010(6) 0.003(6) C8 0.036(7) 0.039(8) 0.036(7) 0.000(6) 0.003(6) 0.000(6) C9 0.027(7) 0.037(7) 0.041(7) -0.003(6) -0.002(6) -0.001(6) C10 0.026(7) 0.045(8) 0.042(7) -0.004(6) 0.005(6) -0.006(6) C11 0.032(7) 0.031(7) 0.024(6) 0.008(5) -0.007(5) 0.005(5) C12 0.053(9) 0.032(7) 0.018(6) 0.001(5) -0.008(6) -0.015(6) N1 0.062(7) 0.028(6) 0.044(7) -0.010(5) 0.019(6) -0.004(5) N2 0.040(6) 0.035(6) 0.035(6) 0.003(5) -0.002(5) 0.008(5) N3 0.031(6) 0.039(6) 0.025(5) -0.005(5) 0.005(4) -0.010(5) N4 0.031(6) 0.037(6) 0.025(5) -0.004(4) 0.002(4) 0.000(5) N5 0.029(6) 0.027(5) 0.031(5) 0.002(4) 0.002(4) -0.002(4) N6 0.039(6) 0.031(6) 0.022(5) 0.000(4) -0.003(4) 0.003(5) N7 0.045(7) 0.046(7) 0.040(6) 0.006(5) -0.002(5) 0.008(6) O4M 0.061(7) 0.071(7) 0.068(7) -0.015(6) -0.014(6) 0.015(6) Ni1 0.0326(9) 0.0317(9) 0.0307(7) 0.0002(8) 0.0026(7) -0.0021(8) O1 0.052(6) 0.040(6) 0.052(6) -0.006(4) 0.010(5) -0.007(5) O2 0.035(5) 0.029(5) 0.035(4) -0.002(4) 0.007(4) 0.002(4) O3 0.010(4) 0.048(5) 0.048(5) 0.011(4) 0.002(4) -0.001(4) O5M 0.053(7) 0.057(7) 0.061(7) -0.014(6) 0.010(6) -0.007(6) O6M 0.114(10) 0.136(10) 0.133(10) 0.009(9) -0.013(9) 0.012(8) O7M 0.049(8) 0.043(7) 0.037(7) 0.009(7) 0.008(6) 0.003(7) O2S 0.070(7) 0.062(7) 0.044(6) 0.006(5) 0.001(5) 0.006(5) O3S 0.106(11) 0.127(12) 0.115(12) -0.007(10) 0.061(9) 0.019(9) O1M 0.097(6) 0.110(6) 0.115(6) -0.035(5) -0.014(5) 0.002(5) O3M 0.081(5) 0.089(5) 0.071(5) 0.009(4) 0.004(4) 0.009(4) N1MA 0.050(6) 0.047(6) 0.052(6) 0.009(4) -0.017(4) 0.000(5) O2MA 0.132(10) 0.139(10) 0.138(11) 0.008(5) 0.001(5) -0.003(5) N1MB 0.099(15) 0.100(15) 0.099(15) 0.001(5) -0.003(5) 0.000(5) O2MB 0.113(19) 0.110(19) 0.111(19) 0.000(5) -0.001(5) -0.001(5) N2M 0.075(9) 0.087(9) 0.059(8) -0.006(7) -0.005(7) 0.017(8) O8M 0.036(12) 0.042(10) 0.031(9) 0.004(9) 0.000(8) 0.002(9) O4S 0.089(9) 0.107(10) 0.102(9) 0.000 0.000 -0.004(8) O1S 0.060(8) 0.060(8) 0.034(10) 0.000 0.000 0.000 N3M 0.041(6) 0.041(6) 0.040(8) 0.000 0.000 0.000 _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 C2 1.52(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.255(17) . ? C2 N1 1.326(17) . ? C3 N1 1.462(15) . ? C3 C4 1.565(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.504(17) . ? C4 C5 1.518(19) . ? C4 C6 1.535(18) . ? C5 N2 1.472(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.477(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.279(15) . ? C7 N4 1.327(15) . ? C8 N4 1.456(14) . ? C8 C9 1.570(17) . ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C9 C12 1.517(18) . ? C9 C10 1.539(16) . ? C9 C11 1.556(16) . ? C10 N5 1.486(14) . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? C11 N6 1.496(14) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 O3 1.226(14) . ? C12 N7 1.362(15) . ? N1 H1 0.8800 . ? N2 Ni1 2.122(10) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 Ni1 2.063(9) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4 0.8800 . ? N5 Ni1 2.085(9) 7_566 ? N5 H5D 0.9200 . ? N5 H5C 0.9200 . ? N6 Ni1 2.102(9) 7_566 ? N6 H6D 0.9200 . ? N6 H6C 0.9200 . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? O4M N2M 1.279(12) . ? Ni1 O3 2.045(8) 8_646 ? Ni1 N5 2.085(9) 8_646 ? Ni1 N6 2.102(9) 8_646 ? Ni1 O2 2.102(8) . ? O3 Ni1 2.045(8) 7_566 ? O5M N2M 1.242(12) . ? O6M N2M 1.264(13) . ? O7M N3M 1.267(11) . ? O1M N1MA 1.229(12) . ? O1M N1MB 1.247(14) . ? O3M N1MB 1.245(14) . ? O3M N1MA 1.267(12) . ? N1MA O2MA 1.250(13) . ? N1MB O2MB 1.248(14) . ? O8M N3M 1.249(14) . ? N3M O8M 1.249(14) 4_655 ? N3M O8M 1.249(14) 2_665 ? N3M O8M 1.249(14) 3_565 ? N3M O7M 1.267(11) 2_665 ? N3M O7M 1.267(11) 3_565 ? N3M O7M 1.267(11) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 123.1(14) . . ? O1 C2 C1 119.2(13) . . ? N1 C2 C1 117.7(14) . . ? N1 C3 C4 114.3(11) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C5 110.1(11) . . ? C7 C4 C6 109.9(11) . . ? C5 C4 C6 113.1(11) . . ? C7 C4 C3 110.2(11) . . ? C5 C4 C3 105.9(10) . . ? C6 C4 C3 107.6(10) . . ? N2 C5 C4 112.1(10) . . ? N2 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N3 C6 C4 111.5(10) . . ? N3 C6 H6A 109.3 . . ? C4 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? C4 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? O2 C7 N4 118.7(11) . . ? O2 C7 C4 118.7(11) . . ? N4 C7 C4 122.3(12) . . ? N4 C8 C9 112.3(10) . . ? N4 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? N4 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? H8B C8 H8A 107.9 . . ? C12 C9 C10 109.4(10) . . ? C12 C9 C11 109.1(10) . . ? C10 C9 C11 111.4(10) . . ? C12 C9 C8 115.5(11) . . ? C10 C9 C8 107.7(10) . . ? C11 C9 C8 103.7(9) . . ? N5 C10 C9 113.5(10) . . ? N5 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? N5 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? H10B C10 H10A 107.7 . . ? N6 C11 C9 114.3(9) . . ? N6 C11 H11B 108.7 . . ? C9 C11 H11B 108.7 . . ? N6 C11 H11A 108.7 . . ? C9 C11 H11A 108.7 . . ? H11B C11 H11A 107.6 . . ? O3 C12 N7 120.9(12) . . ? O3 C12 C9 120.3(11) . . ? N7 C12 C9 118.8(12) . . ? C2 N1 C3 122.3(12) . . ? C2 N1 H1 118.9 . . ? C3 N1 H1 118.9 . . ? C5 N2 Ni1 116.4(8) . . ? C5 N2 H2A 108.2 . . ? Ni1 N2 H2A 108.2 . . ? C5 N2 H2B 108.2 . . ? Ni1 N2 H2B 108.2 . . ? H2A N2 H2B 107.3 . . ? C6 N3 Ni1 114.5(7) . . ? C6 N3 H3C 108.6 . . ? Ni1 N3 H3C 108.6 . . ? C6 N3 H3D 108.6 . . ? Ni1 N3 H3D 108.6 . . ? H3C N3 H3D 107.6 . . ? C7 N4 C8 125.1(10) . . ? C7 N4 H4 117.4 . . ? C8 N4 H4 117.4 . . ? C10 N5 Ni1 115.3(7) . 7_566 ? C10 N5 H5D 108.5 . . ? Ni1 N5 H5D 108.5 7_566 . ? C10 N5 H5C 108.5 . . ? Ni1 N5 H5C 108.5 7_566 . ? H5D N5 H5C 107.5 . . ? C11 N6 Ni1 115.5(6) . 7_566 ? C11 N6 H6D 108.4 . . ? Ni1 N6 H6D 108.4 7_566 . ? C11 N6 H6C 108.4 . . ? Ni1 N6 H6C 108.4 7_566 . ? H6D N6 H6C 107.5 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.4(4) 8_646 . ? O3 Ni1 N5 89.8(4) 8_646 8_646 ? N3 Ni1 N5 94.7(4) . 8_646 ? O3 Ni1 N6 85.3(3) 8_646 8_646 ? N3 Ni1 N6 98.3(4) . 8_646 ? N5 Ni1 N6 86.6(4) 8_646 8_646 ? O3 Ni1 O2 85.8(3) 8_646 . ? N3 Ni1 O2 90.5(3) . . ? N5 Ni1 O2 95.1(3) 8_646 . ? N6 Ni1 O2 170.9(3) 8_646 . ? O3 Ni1 N2 91.2(4) 8_646 . ? N3 Ni1 N2 84.3(4) . . ? N5 Ni1 N2 178.7(4) 8_646 . ? N6 Ni1 N2 94.4(4) 8_646 . ? O2 Ni1 N2 84.1(4) . . ? C7 O2 Ni1 118.0(7) . . ? C12 O3 Ni1 121.5(8) . 7_566 ? N1MA O1M N1MB 18.8(15) . . ? N1MB O3M N1MA 18.5(15) . . ? O1M N1MA O2MA 120.1(12) . . ? O1M N1MA O3M 117.2(11) . . ? O2MA N1MA O3M 122.4(12) . . ? O3M N1MB O1M 117.6(13) . . ? O3M N1MB O2MB 119.5(14) . . ? O1M N1MB O2MB 122.9(15) . . ? O5M N2M O6M 116.9(12) . . ? O5M N2M O4M 127.1(12) . . ? O6M N2M O4M 116.0(12) . . ? O8M N3M O8M 162(2) . 4_655 ? O8M N3M O8M 25(3) . 2_665 ? O8M N3M O8M 162(2) 4_655 2_665 ? O8M N3M O8M 162(2) . 3_565 ? O8M N3M O8M 25(3) 4_655 3_565 ? O8M N3M O8M 162(2) 2_665 3_565 ? O8M N3M O7M 118.9(16) . . ? O8M N3M O7M 72(2) 4_655 . ? O8M N3M O7M 121(2) 2_665 . ? O8M N3M O7M 46.9(16) 3_565 . ? O8M N3M O7M 121(2) . 2_665 ? O8M N3M O7M 46.9(16) 4_655 2_665 ? O8M N3M O7M 118.9(16) 2_665 2_665 ? O8M N3M O7M 72(2) 3_565 2_665 ? O7M N3M O7M 118.7(16) . 2_665 ? O8M N3M O7M 72(2) . 3_565 ? O8M N3M O7M 121(2) 4_655 3_565 ? O8M N3M O7M 46.9(16) 2_665 3_565 ? O8M N3M O7M 118.9(16) 3_565 3_565 ? O7M N3M O7M 105.0(7) . 3_565 ? O7M N3M O7M 105.0(7) 2_665 3_565 ? O8M N3M O7M 46.9(16) . 4_655 ? O8M N3M O7M 118.9(16) 4_655 4_655 ? O8M N3M O7M 72(2) 2_665 4_655 ? O8M N3M O7M 121(2) 3_565 4_655 ? O7M N3M O7M 105.0(7) . 4_655 ? O7M N3M O7M 105.0(7) 2_665 4_655 ? O7M N3M O7M 118.7(16) 3_565 4_655 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.042 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.124 #===END data_i-4_273K_in_capillary _database_code_depnum_ccdc_archive 'CCDC 856067' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.560(2) _cell_length_b 15.560(2) _cell_length_c 19.491(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4719.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 273 _cell_measurement_reflns_used 1121 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 16.79 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set in a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 273 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17365 _diffrn_reflns_av_R_equivalents 0.1289 _diffrn_reflns_av_sigmaI/netI 0.1917 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.31 _reflns_number_total 6443 _reflns_number_gt 3052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.0970P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 6443 _refine_ls_number_parameters 345 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.1844 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 1.009 _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 0.7155(8) 1.0901(8) 0.8098(8) 0.094(5) Uani 1 1 d . . . H1A H 0.6842 1.0703 0.7705 0.141 Uiso 1 1 calc R . . H1B H 0.7461 1.1417 0.7983 0.141 Uiso 1 1 calc R . . H1C H 0.6762 1.1017 0.8466 0.141 Uiso 1 1 calc R . . C2 C 0.7773(8) 1.0234(6) 0.8315(6) 0.055(3) Uani 1 1 d . . . C3 C 0.8085(6) 0.9068(5) 0.9146(5) 0.041(2) Uani 1 1 d . . . H3A H 0.8068 0.9156 0.9639 0.049 Uiso 1 1 calc R . . H3B H 0.8670 0.9172 0.8995 0.049 Uiso 1 1 calc R . . C4 C 0.7848(5) 0.8118(5) 0.8990(4) 0.0317(19) Uani 1 1 d . . . C5 C 0.8506(6) 0.7573(6) 0.9376(5) 0.047(2) Uani 1 1 d . . . H5A H 0.9078 0.7794 0.9285 0.056 Uiso 1 1 calc R . . H5B H 0.8401 0.7623 0.9865 0.056 Uiso 1 1 calc R . . C6 C 0.6914(6) 0.7969(5) 0.9242(5) 0.042(2) Uani 1 1 d . . . H6A H 0.6824 0.8291 0.9663 0.051 Uiso 1 1 calc R . . H6B H 0.6517 0.8189 0.8901 0.051 Uiso 1 1 calc R . . C7 C 0.7913(5) 0.7894(6) 0.8242(4) 0.0328(19) Uani 1 1 d . . . C8 C 0.8452(5) 0.8237(5) 0.7088(4) 0.0311(17) Uani 1 1 d . . . H8B H 0.8246 0.8741 0.6846 0.037 Uiso 1 1 calc R . . H8A H 0.8081 0.7760 0.6964 0.037 Uiso 1 1 calc R . . C9 C 0.9369(5) 0.8037(5) 0.6843(4) 0.0281(17) Uani 1 1 d . . . C10 C 0.9962(5) 0.8743(5) 0.7111(4) 0.0347(18) Uani 1 1 d . . . H10B H 0.9670 0.9291 0.7066 0.042 Uiso 1 1 calc R . . H10A H 1.0061 0.8646 0.7597 0.042 Uiso 1 1 calc R . . C11 C 0.9315(5) 0.8062(5) 0.6051(4) 0.0345(19) Uani 1 1 d . . . H11B H 0.8833 0.7713 0.5904 0.041 Uiso 1 1 calc R . . H11A H 0.9204 0.8648 0.5907 0.041 Uiso 1 1 calc R . . C12 C 0.9700(5) 0.7183(5) 0.7070(4) 0.0300(17) Uani 1 1 d . . . N1 N 0.7517(5) 0.9695(4) 0.8818(4) 0.052(2) Uani 1 1 d . . . H1 H 0.6992 0.9721 0.8952 0.062 Uiso 1 1 calc R . . N2 N 0.8474(4) 0.6662(4) 0.9181(4) 0.0373(17) Uani 1 1 d . . . H2A H 0.8563 0.6346 0.9561 0.045 Uiso 1 1 calc R . . H2B H 0.8914 0.6558 0.8893 0.045 Uiso 1 1 calc R . . N3 N 0.6720(4) 0.7060(4) 0.9369(4) 0.0372(17) Uani 1 1 d . . . H3C H 0.6148 0.6983 0.9335 0.045 Uiso 1 1 calc R . . H3D H 0.6874 0.6930 0.9802 0.045 Uiso 1 1 calc R . . N4 N 0.8374(4) 0.8388(4) 0.7823(3) 0.0317(15) Uani 1 1 d . . . H4 H 0.8640 0.8821 0.7996 0.038 Uiso 1 1 calc R . . N5 N 1.0809(4) 0.8803(4) 0.6760(4) 0.0348(16) Uani 1 1 d . . . H5D H 1.1207 0.8964 0.7069 0.042 Uiso 1 1 calc R . . H5C H 1.0779 0.9218 0.6439 0.042 Uiso 1 1 calc R . . N6 N 1.0104(4) 0.7751(5) 0.5700(3) 0.0367(17) Uani 1 1 d . . . H6D H 1.0211 0.8101 0.5343 0.044 Uiso 1 1 calc R . . H6C H 0.9994 0.7225 0.5528 0.044 Uiso 1 1 calc R . . N7 N 0.9190(5) 0.6632(4) 0.7397(4) 0.0423(18) Uani 1 1 d . . . H7A H 0.9389 0.6146 0.7535 0.051 Uiso 1 1 calc R . . H7B H 0.8661 0.6762 0.7470 0.051 Uiso 1 1 calc R . . O4M O 0.1060(9) 0.6015(8) 0.9206(8) 0.112(5) Uani 0.75 1 d PDU . . Ni1 Ni 0.73274(6) 0.62165(6) 0.87066(5) 0.0292(2) Uani 1 1 d . . . O1 O 0.8506(4) 1.0177(4) 0.8061(4) 0.0543(18) Uani 1 1 d . . . O2 O 0.7557(3) 0.7224(3) 0.8018(3) 0.0311(12) Uani 1 1 d . . . O3 O 1.0472(3) 0.6991(4) 0.6964(3) 0.0368(13) Uani 1 1 d . . . O5M O 0.1571(8) 0.7322(7) 0.9056(8) 0.106(4) Uani 0.75 1 d PDU . . O6M O 0.0316(11) 0.7027(12) 0.8766(12) 0.190(8) Uani 0.75 1 d PDU . . O7M O 0.5197(10) 0.5678(8) -0.0312(7) 0.065(4) Uani 0.50 1 d PDU A -1 O2S O 0.0392(6) 0.8880(6) 0.8962(5) 0.097(3) Uani 1 1 d . . . O3S O 0.6021(8) 1.0037(8) 0.9598(7) 0.144(5) Uani 1 1 d . . . O1M O 0.4879(6) 0.7174(7) 0.8990(6) 0.133(4) Uani 1 1 d DU . . O3M O 0.3767(6) 0.7771(6) 0.9348(5) 0.109(3) Uani 1 1 d DU . . N1MA N 0.4490(8) 0.7844(9) 0.9085(11) 0.066(6) Uani 0.57(2) 1 d PDU B 1 O2MA O 0.4728(13) 0.8430(12) 0.8702(14) 0.169(11) Uani 0.57(2) 1 d PDU B 1 N1MB N 0.4527(11) 0.7836(14) 0.919(2) 0.103(13) Uani 0.43(2) 1 d PDU B 2 O2MB O 0.4893(10) 0.8447(10) 0.9459(11) 0.085(8) Uani 0.43(2) 1 d PDU B 2 N2M N 0.0993(10) 0.6801(10) 0.9039(9) 0.113(6) Uani 0.75 1 d PDU . . O8M O 0.4763(16) 0.5090(17) 0.0604(7) 0.051(7) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8351(9) 0.138(6) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.079(5) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.047(3) Uani 1 4 d SDU . . 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 0.078(9) 0.064(8) 0.140(13) 0.041(8) 0.052(9) 0.033(7) C2 0.070(7) 0.020(4) 0.074(7) -0.002(5) 0.007(6) 0.006(5) C3 0.052(6) 0.037(5) 0.033(5) -0.009(4) 0.006(4) -0.012(4) C4 0.036(4) 0.026(4) 0.033(4) -0.008(3) 0.002(4) -0.004(4) C5 0.053(6) 0.041(5) 0.047(6) -0.005(4) -0.004(5) -0.005(5) C6 0.055(6) 0.030(4) 0.042(5) -0.005(4) 0.012(4) -0.008(4) C7 0.026(4) 0.039(5) 0.034(5) -0.003(4) 0.006(3) 0.000(4) C8 0.032(4) 0.035(4) 0.027(4) -0.001(3) -0.003(3) 0.003(4) C9 0.023(4) 0.034(4) 0.028(4) 0.001(3) 0.000(3) 0.003(3) C10 0.033(4) 0.038(5) 0.033(5) -0.005(4) 0.006(4) 0.000(4) C11 0.028(4) 0.044(5) 0.031(4) 0.002(4) 0.000(3) 0.009(4) C12 0.031(4) 0.032(4) 0.026(4) -0.001(3) 0.004(3) -0.005(3) N1 0.064(5) 0.025(4) 0.067(6) -0.003(4) 0.024(5) 0.003(3) N2 0.037(4) 0.036(4) 0.039(4) 0.002(3) 0.004(3) 0.003(3) N3 0.041(4) 0.037(4) 0.034(4) -0.005(3) 0.006(3) -0.006(3) N4 0.036(4) 0.028(3) 0.031(4) -0.001(3) 0.001(3) -0.005(3) N5 0.031(4) 0.029(4) 0.044(4) -0.001(3) 0.001(3) -0.005(3) N6 0.041(4) 0.043(4) 0.026(4) 0.000(3) -0.001(3) 0.000(3) N7 0.040(4) 0.034(4) 0.053(5) 0.008(4) 0.008(4) -0.004(3) O4M 0.116(8) 0.111(8) 0.109(8) -0.022(7) -0.014(7) 0.017(7) Ni1 0.0297(5) 0.0272(5) 0.0306(5) -0.0019(5) 0.0042(5) -0.0017(5) O1 0.050(4) 0.041(4) 0.072(5) -0.002(3) 0.022(4) -0.013(3) O2 0.034(3) 0.031(3) 0.029(3) -0.006(2) 0.003(2) -0.002(2) O3 0.026(3) 0.033(3) 0.052(4) 0.011(3) 0.004(3) -0.002(2) O5M 0.103(8) 0.088(7) 0.126(8) -0.016(7) 0.005(7) 0.002(6) O6M 0.161(11) 0.209(12) 0.199(11) 0.006(10) -0.003(9) 0.020(9) O7M 0.080(8) 0.061(7) 0.054(7) 0.004(6) 0.004(6) -0.006(6) O2S 0.109(7) 0.092(7) 0.090(7) -0.007(5) 0.018(5) -0.012(6) O3S 0.125(9) 0.123(9) 0.184(13) 0.010(9) 0.080(9) 0.040(7) O1M 0.090(6) 0.146(7) 0.164(8) -0.075(7) -0.033(6) 0.001(6) O3M 0.108(6) 0.140(7) 0.081(6) 0.002(5) 0.014(5) 0.011(6) N1MA 0.056(8) 0.061(9) 0.081(9) 0.017(7) -0.048(7) -0.007(7) O2MA 0.155(13) 0.177(14) 0.173(14) 0.021(10) 0.008(10) -0.015(9) N1MB 0.096(15) 0.107(15) 0.107(15) 0.009(9) -0.022(9) -0.005(10) O2MB 0.094(11) 0.072(10) 0.090(12) -0.012(8) -0.015(8) -0.008(8) N2M 0.102(9) 0.130(10) 0.107(9) 0.001(8) -0.009(8) 0.027(8) O8M 0.055(11) 0.052(10) 0.046(9) -0.008(8) 0.007(8) 0.002(9) O4S 0.107(9) 0.153(10) 0.154(10) 0.000 0.000 0.001(8) O1S 0.089(7) 0.089(7) 0.060(10) 0.000 0.000 0.000 N3M 0.048(5) 0.048(5) 0.043(7) 0.000 0.000 0.000 _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 C2 1.477(15) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.247(12) . ? C2 N1 1.349(13) . ? C3 N1 1.464(11) . ? C3 C4 1.554(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.501(11) . ? C4 C5 1.528(13) . ? C4 C6 1.553(12) . ? C5 N2 1.468(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.467(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.260(10) . ? C7 N4 1.332(10) . ? C8 N4 1.456(10) . ? C8 C9 1.537(10) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 C12 1.494(11) . ? C9 C10 1.528(11) . ? C9 C11 1.546(11) . ? C10 N5 1.489(10) . ? C10 H10B 0.9700 . ? C10 H10A 0.9700 . ? C11 N6 1.486(10) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C12 O3 1.255(9) . ? C12 N7 1.331(10) . ? N1 H1 0.8600 . ? N2 Ni1 2.126(7) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.070(7) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.079(7) 7_566 ? N5 H5D 0.9000 . ? N5 H5C 0.9000 . ? N6 Ni1 2.086(7) 7_566 ? N6 H6D 0.9000 . ? N6 H6C 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? O4M N2M 1.269(12) . ? Ni1 O3 2.043(5) 8_646 ? Ni1 N5 2.079(7) 8_646 ? Ni1 N6 2.086(7) 8_646 ? Ni1 O2 2.094(5) . ? O3 Ni1 2.043(5) 7_566 ? O5M N2M 1.212(12) . ? O6M N2M 1.232(13) . ? O7M N3M 1.256(10) . ? O1M N1MA 1.219(13) . ? O1M N1MB 1.228(14) . ? O3M N1MB 1.228(14) . ? O3M N1MA 1.241(12) . ? N1MA O2MA 1.236(14) . ? N1MB O2MB 1.229(15) . ? O8M N3M 1.242(13) . ? N3M O8M 1.242(13) 4_655 ? N3M O8M 1.242(13) 2_665 ? N3M O8M 1.242(13) 3_565 ? N3M O7M 1.256(10) 2_665 ? N3M O7M 1.256(10) 3_565 ? N3M O7M 1.256(10) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 121.0(9) . . ? O1 C2 C1 122.1(10) . . ? N1 C2 C1 117.0(10) . . ? N1 C3 C4 113.8(7) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C7 C4 C5 107.7(7) . . ? C7 C4 C6 109.6(7) . . ? C5 C4 C6 112.8(7) . . ? C7 C4 C3 113.3(7) . . ? C5 C4 C3 105.8(7) . . ? C6 C4 C3 107.6(6) . . ? N2 C5 C4 112.7(7) . . ? N2 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N3 C6 C4 113.0(7) . . ? N3 C6 H6A 109.0 . . ? C4 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N4 120.1(7) . . ? O2 C7 C4 120.0(7) . . ? N4 C7 C4 119.9(7) . . ? N4 C8 C9 114.6(6) . . ? N4 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? N4 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? H8B C8 H8A 107.6 . . ? C12 C9 C10 109.3(6) . . ? C12 C9 C8 114.1(6) . . ? C10 C9 C8 108.0(6) . . ? C12 C9 C11 109.7(7) . . ? C10 C9 C11 110.9(7) . . ? C8 C9 C11 104.8(6) . . ? N5 C10 C9 114.9(6) . . ? N5 C10 H10B 108.5 . . ? C9 C10 H10B 108.5 . . ? N5 C10 H10A 108.5 . . ? C9 C10 H10A 108.5 . . ? H10B C10 H10A 107.5 . . ? N6 C11 C9 114.0(6) . . ? N6 C11 H11B 108.8 . . ? C9 C11 H11B 108.8 . . ? N6 C11 H11A 108.8 . . ? C9 C11 H11A 108.8 . . ? H11B C11 H11A 107.6 . . ? O3 C12 N7 119.8(7) . . ? O3 C12 C9 119.6(7) . . ? N7 C12 C9 120.6(7) . . ? C2 N1 C3 123.6(8) . . ? C2 N1 H1 118.2 . . ? C3 N1 H1 118.2 . . ? C5 N2 Ni1 117.2(5) . . ? C5 N2 H2A 108.0 . . ? Ni1 N2 H2A 108.0 . . ? C5 N2 H2B 108.0 . . ? Ni1 N2 H2B 108.0 . . ? H2A N2 H2B 107.3 . . ? C6 N3 Ni1 114.3(5) . . ? C6 N3 H3C 108.7 . . ? Ni1 N3 H3C 108.7 . . ? C6 N3 H3D 108.7 . . ? Ni1 N3 H3D 108.7 . . ? H3C N3 H3D 107.6 . . ? C7 N4 C8 123.7(7) . . ? C7 N4 H4 118.1 . . ? C8 N4 H4 118.1 . . ? C10 N5 Ni1 114.8(5) . 7_566 ? C10 N5 H5D 108.6 . . ? Ni1 N5 H5D 108.6 7_566 . ? C10 N5 H5C 108.6 . . ? Ni1 N5 H5C 108.6 7_566 . ? H5D N5 H5C 107.6 . . ? C11 N6 Ni1 116.7(5) . 7_566 ? C11 N6 H6D 108.1 . . ? Ni1 N6 H6D 108.1 7_566 . ? C11 N6 H6C 108.1 . . ? Ni1 N6 H6C 108.1 7_566 . ? H6D N6 H6C 107.3 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.7(3) 8_646 . ? O3 Ni1 N5 89.2(2) 8_646 8_646 ? N3 Ni1 N5 94.6(3) . 8_646 ? O3 Ni1 N6 85.1(2) 8_646 8_646 ? N3 Ni1 N6 98.8(3) . 8_646 ? N5 Ni1 N6 86.6(3) 8_646 8_646 ? O3 Ni1 O2 85.7(2) 8_646 . ? N3 Ni1 O2 90.2(2) . . ? N5 Ni1 O2 95.3(2) 8_646 . ? N6 Ni1 O2 170.6(2) 8_646 . ? O3 Ni1 N2 91.6(2) 8_646 . ? N3 Ni1 N2 84.6(3) . . ? N5 Ni1 N2 178.7(3) 8_646 . ? N6 Ni1 N2 94.5(3) 8_646 . ? O2 Ni1 N2 83.8(2) . . ? C7 O2 Ni1 118.2(5) . . ? C12 O3 Ni1 121.6(5) . 7_566 ? O1M N1MA O2MA 113.0(14) . . ? O1M N1MA O3M 115.8(11) . . ? O2MA N1MA O3M 126.1(14) . . ? O3M N1MB O1M 116.1(14) . . ? O3M N1MB O2MB 113.5(16) . . ? O1M N1MB O2MB 125.2(18) . . ? O5M N2M O6M 117.1(13) . . ? O5M N2M O4M 125.2(13) . . ? O6M N2M O4M 117.2(13) . . ? O8M N3M O8M 154.1(15) 4_655 2_665 ? O8M N3M O8M 154.1(15) 2_665 3_565 ? O8M N3M O8M 154.1(15) 4_655 . ? O8M N3M O8M 154.1(15) 3_565 . ? O8M N3M O7M 79.5(15) 4_655 . ? O8M N3M O7M 118.8(16) 2_665 . ? O8M N3M O7M 115.9(13) . . ? O8M N3M O7M 115.9(13) 2_665 2_665 ? O8M N3M O7M 79.5(15) 3_565 2_665 ? O8M N3M O7M 118.8(16) . 2_665 ? O7M N3M O7M 122.0(14) . 2_665 ? O8M N3M O7M 118.8(16) 4_655 3_565 ? O8M N3M O7M 115.9(13) 3_565 3_565 ? O8M N3M O7M 79.5(15) . 3_565 ? O7M N3M O7M 103.6(6) . 3_565 ? O7M N3M O7M 103.6(6) 2_665 3_565 ? O8M N3M O7M 115.9(13) 4_655 4_655 ? O8M N3M O7M 79.5(15) 2_665 4_655 ? O8M N3M O7M 118.8(16) 3_565 4_655 ? O7M N3M O7M 103.6(6) . 4_655 ? O7M N3M O7M 103.6(6) 2_665 4_655 ? O7M N3M O7M 122.0(14) 3_565 4_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.823 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.116 #===END data_i-4_293K_in_capillary _database_code_depnum_ccdc_archive 'CCDC 856068' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.5400(16) _cell_length_b 15.5400(16) _cell_length_c 19.493(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4707.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1948 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 20.91 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9236 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set in a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 17265 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.16 _reflns_number_total 6295 _reflns_number_gt 3840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.0930P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 6295 _refine_ls_number_parameters 345 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 1.076 _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 0.7116(7) 1.0892(7) 0.8086(7) 0.094(4) Uani 1 1 d . . . H1A H 0.6971 1.0800 0.7613 0.140 Uiso 1 1 calc R . . H1B H 0.7360 1.1455 0.8140 0.140 Uiso 1 1 calc R . . H1C H 0.6607 1.0844 0.8362 0.140 Uiso 1 1 calc R . . C2 C 0.7755(7) 1.0232(5) 0.8308(5) 0.066(3) Uani 1 1 d . . . C3 C 0.8066(5) 0.9082(5) 0.9147(4) 0.0487(18) Uani 1 1 d . . . H3A H 0.8044 0.9177 0.9639 0.058 Uiso 1 1 calc R . . H3B H 0.8652 0.9189 0.8999 0.058 Uiso 1 1 calc R . . C4 C 0.7844(4) 0.8136(4) 0.9002(3) 0.0341(14) Uani 1 1 d . . . C5 C 0.8498(5) 0.7586(5) 0.9380(4) 0.0491(18) Uani 1 1 d . . . H5A H 0.9069 0.7807 0.9286 0.059 Uiso 1 1 calc R . . H5B H 0.8397 0.7640 0.9869 0.059 Uiso 1 1 calc R . . C6 C 0.6905(5) 0.7979(5) 0.9247(4) 0.0457(17) Uani 1 1 d . . . H6A H 0.6808 0.8298 0.9668 0.055 Uiso 1 1 calc R . . H6B H 0.6510 0.8199 0.8904 0.055 Uiso 1 1 calc R . . C7 C 0.7904(4) 0.7899(4) 0.8233(3) 0.0337(14) Uani 1 1 d . . . C8 C 0.8443(4) 0.8245(4) 0.7084(3) 0.0356(14) Uani 1 1 d . . . H8B H 0.8241 0.8752 0.6842 0.043 Uiso 1 1 calc R . . H8A H 0.8072 0.7768 0.6958 0.043 Uiso 1 1 calc R . . C9 C 0.9374(4) 0.8041(4) 0.6849(3) 0.0325(13) Uani 1 1 d . . . C10 C 0.9962(4) 0.8752(4) 0.7110(4) 0.0371(14) Uani 1 1 d . . . H10B H 0.9672 0.9300 0.7053 0.045 Uiso 1 1 calc R . . H10A H 1.0056 0.8667 0.7597 0.045 Uiso 1 1 calc R . . C11 C 0.9315(4) 0.8060(4) 0.6054(3) 0.0366(14) Uani 1 1 d . . . H11B H 0.8831 0.7707 0.5913 0.044 Uiso 1 1 calc R . . H11A H 0.9196 0.8645 0.5910 0.044 Uiso 1 1 calc R . . C12 C 0.9705(4) 0.7181(4) 0.7075(3) 0.0320(13) Uani 1 1 d . . . N1 N 0.7502(5) 0.9703(4) 0.8815(3) 0.0573(17) Uani 1 1 d . . . H1 H 0.6976 0.9733 0.8951 0.069 Uiso 1 1 calc R . . N2 N 0.8474(4) 0.6669(4) 0.9195(3) 0.0414(13) Uani 1 1 d . . . H2A H 0.8556 0.6359 0.9579 0.050 Uiso 1 1 calc R . . H2B H 0.8920 0.6561 0.8913 0.050 Uiso 1 1 calc R . . N3 N 0.6713(4) 0.7065(4) 0.9370(3) 0.0398(13) Uani 1 1 d . . . H3C H 0.6141 0.6986 0.9333 0.048 Uiso 1 1 calc R . . H3D H 0.6863 0.6935 0.9804 0.048 Uiso 1 1 calc R . . N4 N 0.8369(3) 0.8396(3) 0.7828(2) 0.0342(11) Uani 1 1 d . . . H4 H 0.8640 0.8824 0.8006 0.041 Uiso 1 1 calc R . . N5 N 1.0813(3) 0.8798(3) 0.6762(3) 0.0357(12) Uani 1 1 d . . . H5D H 1.1211 0.8951 0.7074 0.043 Uiso 1 1 calc R . . H5C H 1.0791 0.9217 0.6444 0.043 Uiso 1 1 calc R . . N6 N 1.0096(3) 0.7753(4) 0.5691(3) 0.0387(13) Uani 1 1 d . . . H6D H 1.0199 0.8109 0.5336 0.046 Uiso 1 1 calc R . . H6C H 0.9985 0.7229 0.5515 0.046 Uiso 1 1 calc R . . N7 N 0.9202(4) 0.6630(4) 0.7396(3) 0.0429(14) Uani 1 1 d . . . H7A H 0.9401 0.6139 0.7525 0.051 Uiso 1 1 calc R . . H7B H 0.8674 0.6761 0.7478 0.051 Uiso 1 1 calc R . . O4M O 0.1028(9) 0.5981(8) 0.9196(7) 0.131(4) Uani 0.75 1 d PDU . . Ni1 Ni 0.73283(5) 0.62179(5) 0.87106(4) 0.03033(19) Uani 1 1 d . . . O1 O 0.8482(4) 1.0191(3) 0.8047(3) 0.0633(15) Uani 1 1 d . . . O2 O 0.7553(3) 0.7233(3) 0.8026(2) 0.0337(9) Uani 1 1 d . . . O3 O 1.0474(3) 0.6980(3) 0.6960(2) 0.0374(10) Uani 1 1 d . . . O5M O 0.1539(9) 0.7301(8) 0.9054(8) 0.136(5) Uani 0.75 1 d PDU . . O6M O 0.0292(10) 0.7009(12) 0.8773(11) 0.206(8) Uani 0.75 1 d PDU . . O7M O 0.5186(9) 0.5665(7) -0.0331(6) 0.068(3) Uani 0.50 1 d PDU A -1 O2S O 0.0402(7) 0.8873(7) 0.8969(5) 0.130(3) Uani 1 1 d . . . O3S O 0.5971(8) 0.0010(9) 0.9574(8) 0.184(6) Uani 1 1 d . . . O1M O 0.4860(5) 0.7179(7) 0.8982(5) 0.142(4) Uani 1 1 d DU . . O3M O 0.3772(5) 0.7779(6) 0.9356(4) 0.108(3) Uani 1 1 d DU . . N1MA N 0.4487(9) 0.7845(8) 0.9098(11) 0.071(7) Uani 0.55(2) 1 d PDU B 1 O2MA O 0.4761(11) 0.8448(10) 0.8750(12) 0.146(8) Uani 0.55(2) 1 d PDU B 1 N1MB N 0.4514(11) 0.7849(12) 0.9162(19) 0.098(12) Uani 0.45(2) 1 d PDU B 2 O2MB O 0.4889(10) 0.8441(9) 0.9457(10) 0.107(8) Uani 0.45(2) 1 d PDU B 2 N2M N 0.0963(10) 0.6766(10) 0.9041(8) 0.128(6) Uani 0.75 1 d PDU . . O8M O 0.4790(17) 0.5096(18) 0.0598(7) 0.072(7) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8326(9) 0.155(6) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.105(5) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.049(3) Uani 1 4 d SDU . . 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 0.088(7) 0.064(6) 0.129(10) 0.024(6) 0.037(7) 0.023(6) C2 0.093(7) 0.031(4) 0.073(6) -0.008(4) 0.025(5) 0.000(4) C3 0.065(5) 0.037(4) 0.044(4) -0.010(3) 0.011(3) -0.009(3) C4 0.042(4) 0.032(3) 0.028(3) -0.008(2) 0.003(3) -0.007(3) C5 0.057(4) 0.050(4) 0.041(4) 0.002(3) -0.010(3) -0.010(4) C6 0.053(4) 0.042(4) 0.042(4) -0.007(3) 0.021(3) -0.008(3) C7 0.031(3) 0.032(3) 0.038(3) -0.002(3) 0.003(3) 0.003(3) C8 0.034(3) 0.039(3) 0.034(3) 0.006(3) 0.003(3) 0.003(3) C9 0.030(3) 0.035(3) 0.032(3) 0.000(3) 0.004(2) 0.003(3) C10 0.035(3) 0.033(3) 0.044(4) -0.001(3) 0.006(3) 0.000(3) C11 0.031(3) 0.049(4) 0.029(3) 0.004(3) 0.000(2) 0.002(3) C12 0.029(3) 0.037(3) 0.030(3) 0.000(3) -0.001(2) -0.002(2) N1 0.075(4) 0.037(3) 0.060(4) -0.009(3) 0.033(4) -0.002(3) N2 0.039(3) 0.042(3) 0.043(3) 0.002(3) -0.002(2) 0.002(3) N3 0.041(3) 0.044(3) 0.035(3) -0.004(2) 0.006(2) -0.009(3) N4 0.036(3) 0.033(3) 0.033(3) -0.003(2) 0.008(2) -0.004(2) N5 0.032(3) 0.037(3) 0.038(3) 0.001(2) 0.001(2) -0.003(2) N6 0.041(3) 0.050(3) 0.025(3) 0.001(2) -0.002(2) 0.001(3) N7 0.040(3) 0.036(3) 0.054(4) 0.012(3) 0.012(3) 0.002(2) O4M 0.140(8) 0.138(8) 0.116(8) -0.024(7) 0.001(7) 0.022(7) Ni1 0.0322(4) 0.0289(4) 0.0298(3) -0.0017(3) 0.0051(3) -0.0013(3) O1 0.073(4) 0.048(3) 0.070(4) -0.003(3) 0.027(3) -0.012(3) O2 0.040(2) 0.033(2) 0.029(2) -0.0023(17) 0.0058(18) -0.0036(19) O3 0.027(2) 0.038(2) 0.047(3) 0.010(2) 0.0050(19) 0.0045(19) O5M 0.140(8) 0.112(8) 0.156(9) -0.016(7) 0.003(7) 0.011(7) O6M 0.176(10) 0.230(12) 0.212(11) -0.001(10) -0.005(9) 0.018(9) O7M 0.092(7) 0.059(6) 0.052(6) 0.004(5) 0.008(5) -0.012(6) O2S 0.140(8) 0.137(8) 0.113(7) -0.001(6) 0.019(6) -0.035(6) O3S 0.147(10) 0.158(10) 0.247(15) 0.005(10) 0.098(10) 0.035(8) O1M 0.089(5) 0.155(7) 0.182(8) -0.087(6) -0.036(5) 0.006(5) O3M 0.102(5) 0.144(6) 0.076(4) -0.002(4) 0.009(4) 0.015(5) N1MA 0.067(9) 0.070(9) 0.076(9) 0.008(7) -0.042(7) 0.003(7) O2MA 0.121(10) 0.163(11) 0.154(12) 0.028(9) 0.012(9) -0.008(8) N1MB 0.091(14) 0.103(14) 0.099(14) 0.006(9) -0.021(9) -0.001(9) O2MB 0.120(11) 0.091(10) 0.109(11) -0.009(8) -0.020(8) -0.014(8) N2M 0.113(9) 0.148(10) 0.123(9) -0.015(8) -0.015(7) 0.022(8) O8M 0.074(11) 0.070(10) 0.071(9) -0.005(8) 0.006(8) -0.004(9) O4S 0.109(8) 0.165(10) 0.191(10) 0.000 0.000 0.002(8) O1S 0.124(8) 0.124(8) 0.068(9) 0.000 0.000 0.000 N3M 0.053(4) 0.053(4) 0.042(6) 0.000 0.000 0.000 _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 C2 1.491(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.240(10) . ? C2 N1 1.345(11) . ? C3 N1 1.455(10) . ? C3 C4 1.536(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.518(10) . ? C4 C7 1.546(9) . ? C4 C6 1.556(9) . ? C5 N2 1.470(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.470(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.238(7) . ? C7 N4 1.320(8) . ? C8 N4 1.474(8) . ? C8 C9 1.551(8) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 C12 1.499(9) . ? C9 C10 1.522(9) . ? C9 C11 1.552(9) . ? C10 N5 1.487(8) . ? C10 H10B 0.9700 . ? C10 H10A 0.9700 . ? C11 N6 1.484(8) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C12 O3 1.256(7) . ? C12 N7 1.318(8) . ? N1 H1 0.8600 . ? N2 Ni1 2.133(5) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.074(5) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.076(5) 7_566 ? N5 H5D 0.9000 . ? N5 H5C 0.9000 . ? N6 Ni1 2.102(5) 7_566 ? N6 H6D 0.9000 . ? N6 H6C 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? O4M N2M 1.261(12) . ? Ni1 O3 2.049(4) 8_646 ? Ni1 N5 2.076(5) 8_646 ? Ni1 O2 2.096(4) . ? Ni1 N6 2.102(5) 8_646 ? O3 Ni1 2.049(4) 7_566 ? O5M N2M 1.223(12) . ? O6M N2M 1.226(12) . ? O7M N3M 1.253(9) . ? O1M N1MA 1.207(12) . ? O1M N1MB 1.223(14) . ? O3M N1MB 1.219(14) . ? O3M N1MA 1.225(12) . ? N1MA O2MA 1.232(14) . ? N1MB O2MB 1.231(15) . ? O8M N3M 1.219(13) . ? N3M O8M 1.219(13) 4_655 ? N3M O8M 1.219(13) 2_665 ? N3M O8M 1.219(13) 3_565 ? N3M O7M 1.253(9) 2_665 ? N3M O7M 1.253(9) 3_565 ? N3M O7M 1.253(9) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.4(8) . . ? O1 C2 C1 121.5(8) . . ? N1 C2 C1 116.1(8) . . ? N1 C3 C4 114.6(6) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 107.4(6) . . ? C5 C4 C7 107.2(5) . . ? C3 C4 C7 113.2(6) . . ? C5 C4 C6 112.9(6) . . ? C3 C4 C6 107.7(5) . . ? C7 C4 C6 108.5(5) . . ? N2 C5 C4 114.2(5) . . ? N2 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N3 C6 C4 113.1(6) . . ? N3 C6 H6A 109.0 . . ? C4 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N4 122.4(6) . . ? O2 C7 C4 119.3(6) . . ? N4 C7 C4 118.2(5) . . ? N4 C8 C9 113.3(5) . . ? N4 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? N4 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? H8B C8 H8A 107.7 . . ? C12 C9 C10 110.1(5) . . ? C12 C9 C8 114.5(5) . . ? C10 C9 C8 108.3(5) . . ? C12 C9 C11 109.3(5) . . ? C10 C9 C11 110.9(5) . . ? C8 C9 C11 103.6(5) . . ? N5 C10 C9 114.6(5) . . ? N5 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? N5 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? H10B C10 H10A 107.6 . . ? N6 C11 C9 115.0(5) . . ? N6 C11 H11B 108.5 . . ? C9 C11 H11B 108.5 . . ? N6 C11 H11A 108.5 . . ? C9 C11 H11A 108.5 . . ? H11B C11 H11A 107.5 . . ? O3 C12 N7 119.2(6) . . ? O3 C12 C9 119.7(5) . . ? N7 C12 C9 121.0(5) . . ? C2 N1 C3 123.8(7) . . ? C2 N1 H1 118.1 . . ? C3 N1 H1 118.1 . . ? C5 N2 Ni1 116.6(4) . . ? C5 N2 H2A 108.1 . . ? Ni1 N2 H2A 108.1 . . ? C5 N2 H2B 108.1 . . ? Ni1 N2 H2B 108.1 . . ? H2A N2 H2B 107.3 . . ? C6 N3 Ni1 114.7(4) . . ? C6 N3 H3C 108.6 . . ? Ni1 N3 H3C 108.6 . . ? C6 N3 H3D 108.6 . . ? Ni1 N3 H3D 108.6 . . ? H3C N3 H3D 107.6 . . ? C7 N4 C8 122.5(5) . . ? C7 N4 H4 118.7 . . ? C8 N4 H4 118.7 . . ? C10 N5 Ni1 115.6(4) . 7_566 ? C10 N5 H5D 108.4 . . ? Ni1 N5 H5D 108.4 7_566 . ? C10 N5 H5C 108.4 . . ? Ni1 N5 H5C 108.4 7_566 . ? H5D N5 H5C 107.4 . . ? C11 N6 Ni1 115.7(4) . 7_566 ? C11 N6 H6D 108.4 . . ? Ni1 N6 H6D 108.4 7_566 . ? C11 N6 H6C 108.4 . . ? Ni1 N6 H6C 108.4 7_566 . ? H6D N6 H6C 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N3 174.4(2) 8_646 . ? O3 Ni1 N5 89.30(19) 8_646 8_646 ? N3 Ni1 N5 94.5(2) . 8_646 ? O3 Ni1 O2 86.04(16) 8_646 . ? N3 Ni1 O2 89.63(19) . . ? N5 Ni1 O2 94.93(19) 8_646 . ? O3 Ni1 N6 85.29(19) 8_646 8_646 ? N3 Ni1 N6 98.9(2) . 8_646 ? N5 Ni1 N6 86.8(2) 8_646 8_646 ? O2 Ni1 N6 171.1(2) . 8_646 ? O3 Ni1 N2 91.7(2) 8_646 . ? N3 Ni1 N2 84.4(2) . . ? N5 Ni1 N2 178.5(2) 8_646 . ? O2 Ni1 N2 84.0(2) . . ? N6 Ni1 N2 94.4(2) 8_646 . ? C7 O2 Ni1 119.7(4) . . ? C12 O3 Ni1 121.4(4) . 7_566 ? O1M N1MA O3M 116.1(11) . . ? O1M N1MA O2MA 112.6(13) . . ? O3M N1MA O2MA 127.1(13) . . ? O3M N1MB O1M 115.3(14) . . ? O3M N1MB O2MB 111.7(16) . . ? O1M N1MB O2MB 124.3(19) . . ? O5M N2M O6M 115.0(13) . . ? O5M N2M O4M 126.5(13) . . ? O6M N2M O4M 117.9(13) . . ? O8M N3M O8M 156.0(17) . 4_655 ? O8M N3M O8M 156.0(17) 4_655 2_665 ? O8M N3M O8M 156.0(17) . 3_565 ? O8M N3M O8M 156.0(17) 2_665 3_565 ? O8M N3M O7M 122.2(16) . 2_665 ? O8M N3M O7M 117.0(13) 2_665 2_665 ? O8M N3M O7M 75.9(16) 3_565 2_665 ? O8M N3M O7M 75.9(16) . 3_565 ? O8M N3M O7M 122.2(16) 4_655 3_565 ? O8M N3M O7M 117.0(13) 3_565 3_565 ? O7M N3M O7M 105.4(5) 2_665 3_565 ? O8M N3M O7M 117.0(13) 4_655 4_655 ? O8M N3M O7M 75.9(16) 2_665 4_655 ? O8M N3M O7M 122.2(16) 3_565 4_655 ? O7M N3M O7M 105.4(5) 2_665 4_655 ? O7M N3M O7M 117.9(11) 3_565 4_655 ? O8M N3M O7M 117.0(13) . . ? O8M N3M O7M 75.9(16) 4_655 . ? O8M N3M O7M 122.2(16) 2_665 . ? O7M N3M O7M 117.9(11) 2_665 . ? O7M N3M O7M 105.4(5) 3_565 . ? O7M N3M O7M 105.4(5) 4_655 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.035 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.097 #===END data_i-4_313K_in_capillary _database_code_depnum_ccdc_archive 'CCDC 856069' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H116 N36 Ni4 O40' _chemical_formula_weight 2072.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.476(3) _cell_length_b 15.476(3) _cell_length_c 19.445(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4657.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 313 _cell_measurement_reflns_used 1844 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 18.03 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9156 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set in a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 313 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 14767 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.1005 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5124 _reflns_number_gt 3283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1288P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 5124 _refine_ls_number_parameters 381 _refine_ls_number_restraints 411 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.966 _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 0.7148(11) 1.0914(9) 0.8091(9) 0.134(6) Uani 1 1 d . . . H1A H 0.6645 1.0623 0.7918 0.201 Uiso 1 1 calc R . . H1B H 0.7409 1.1244 0.7728 0.201 Uiso 1 1 calc R . . H1C H 0.6984 1.1294 0.8459 0.201 Uiso 1 1 calc R . . C2 C 0.7784(9) 1.0258(7) 0.8353(7) 0.092(4) Uani 1 1 d . . . C3 C 0.8104(7) 0.9100(6) 0.9176(5) 0.068(3) Uani 1 1 d . . . H3A H 0.8089 0.9186 0.9670 0.081 Uiso 1 1 calc R . . H3B H 0.8690 0.9209 0.9022 0.081 Uiso 1 1 calc R . . C4 C 0.7876(6) 0.8142(5) 0.9020(4) 0.0487(19) Uani 1 1 d . . . C5 C 0.8546(6) 0.7570(6) 0.9395(5) 0.060(2) Uani 1 1 d . . . H5A H 0.9121 0.7779 0.9288 0.072 Uiso 1 1 calc R . . H5B H 0.8462 0.7627 0.9887 0.072 Uiso 1 1 calc R . . C6 C 0.6934(6) 0.8003(5) 0.9278(4) 0.057(2) Uani 1 1 d . . . H6A H 0.6856 0.8311 0.9708 0.068 Uiso 1 1 calc R . . H6B H 0.6536 0.8246 0.8945 0.068 Uiso 1 1 calc R . . C7 C 0.7918(5) 0.7922(5) 0.8251(4) 0.0416(17) Uani 1 1 d . . . C8 C 0.8455(5) 0.8257(5) 0.7100(3) 0.0454(17) Uani 1 1 d . . . H8A H 0.8251 0.8765 0.6857 0.055 Uiso 1 1 calc R . . H8B H 0.8079 0.7779 0.6978 0.055 Uiso 1 1 calc R . . C9 C 0.9379(4) 0.8048(4) 0.6852(3) 0.0365(15) Uani 1 1 d . . . C10 C 1.0000(5) 0.8761(5) 0.7113(4) 0.0463(17) Uani 1 1 d . . . H10A H 0.9716 0.9317 0.7068 0.056 Uiso 1 1 calc R . . H10B H 1.0110 0.8666 0.7598 0.056 Uiso 1 1 calc R . . C11 C 0.9315(5) 0.8063(5) 0.6065(3) 0.0432(17) Uani 1 1 d . . . H11A H 0.8828 0.7709 0.5927 0.052 Uiso 1 1 calc R . . H11B H 0.9197 0.8650 0.5919 0.052 Uiso 1 1 calc R . . C12 C 0.9712(5) 0.7187(5) 0.7074(3) 0.0380(15) Uani 1 1 d . . . N1 N 0.7527(6) 0.9731(5) 0.8851(4) 0.074(2) Uani 1 1 d . . . H1 H 0.7000 0.9761 0.8989 0.088 Uiso 1 1 calc R . . N2 N 0.8489(4) 0.6658(5) 0.9209(3) 0.0521(16) Uani 1 1 d . . . H2A H 0.8559 0.6344 0.9594 0.063 Uiso 1 1 calc R . . H2B H 0.8936 0.6535 0.8930 0.063 Uiso 1 1 calc R . . N3 N 0.6719(4) 0.7074(4) 0.9386(3) 0.0464(15) Uani 1 1 d . . . H3C H 0.6144 0.7007 0.9340 0.056 Uiso 1 1 calc R . . H3D H 0.6859 0.6929 0.9820 0.056 Uiso 1 1 calc R . . N4 N 0.8383(4) 0.8411(4) 0.7838(3) 0.0428(14) Uani 1 1 d . . . H4 H 0.8657 0.8843 0.8012 0.051 Uiso 1 1 calc R . . N5 N 1.0827(4) 0.8796(4) 0.6750(3) 0.0453(15) Uani 1 1 d . . . H5C H 1.1237 0.8960 0.7052 0.054 Uiso 1 1 calc R . . H5D H 1.0793 0.9210 0.6426 0.054 Uiso 1 1 calc R . . N6 N 1.0097(4) 0.7751(4) 0.5699(3) 0.0475(16) Uani 1 1 d . . . H6C H 1.0198 0.8107 0.5341 0.057 Uiso 1 1 calc R . . H6D H 0.9982 0.7224 0.5525 0.057 Uiso 1 1 calc R . . N7 N 0.9212(4) 0.6645(4) 0.7412(4) 0.0516(16) Uani 1 1 d . . . H7A H 0.9418 0.6162 0.7557 0.062 Uiso 1 1 calc R . . H7B H 0.8680 0.6774 0.7488 0.062 Uiso 1 1 calc R . . O4MA O 0.0961(15) 0.5441(16) 0.9466(18) 0.122(5) Uani 0.25 1 d PDU A 3 O4MB O 0.0968(11) 0.6045(8) 0.9174(10) 0.127(4) Uani 0.50 1 d PDU B 4 N3M N 1.0000 0.0000 0.5000 0.061(3) Uani 1 4 d SDU . . Ni1 Ni 0.73348(5) 0.62287(5) 0.87160(4) 0.0367(2) Uani 1 1 d . . . O1 O 0.8513(6) 1.0186(5) 0.8066(4) 0.089(2) Uani 1 1 d . . . O2 O 0.7564(3) 0.7253(3) 0.8036(2) 0.0415(11) Uani 1 1 d . . . O3 O 1.0483(3) 0.6987(3) 0.6969(3) 0.0446(12) Uani 1 1 d . . . O5MA O 0.0089(19) 0.5675(17) 0.8655(17) 0.129(5) Uani 0.25 1 d PDU A 3 O5MB O 0.1548(9) 0.7273(9) 0.9098(11) 0.142(5) Uani 0.50 1 d PDU B 4 O6MA O 0.044(3) 0.6685(14) 0.9326(19) 0.135(5) Uani 0.25 1 d PDU A 3 O6MB O 0.0305(9) 0.7066(11) 0.8689(11) 0.137(5) Uani 0.50 1 d PDU B 4 O7M O 0.9355(5) 0.0169(9) 0.5331(5) 0.072(3) Uani 0.50 1 d PDU . . O1M O 0.4897(5) 0.7177(6) 0.8999(5) 0.141(3) Uani 1 1 d DU . . O3M O 0.3765(5) 0.7786(6) 0.9352(5) 0.128(3) Uani 1 1 d DU . . N1MA N 0.4444(5) 0.7816(5) 0.9039(4) 0.133(3) Uani 0.479(12) 1 d PDU C 1 O2MA O 0.4670(9) 0.8486(7) 0.8765(11) 0.146(4) Uani 0.479(12) 1 d PDU C 1 N1MB N 0.4542(5) 0.7795(5) 0.9261(4) 0.134(3) Uani 0.521(12) 1 d PDU C 2 O2MB O 0.4964(7) 0.8422(8) 0.9433(11) 0.143(4) Uani 0.521(12) 1 d PDU C 2 N2MA N 0.049(3) 0.5933(15) 0.915(2) 0.129(4) Uani 0.25 1 d PDU A 3 N2MB N 0.0936(9) 0.6797(8) 0.8994(10) 0.130(4) Uani 0.50 1 d PDU B 4 O8M O 1.0048(12) 0.0215(14) 0.4400(4) 0.069(5) Uani 0.25 1 d PDU . . O4S O 1.0000 0.5000 0.6805(10) 0.076(5) Uani 0.50 2 d SPU . . O3SA O 0.513(3) 0.066(3) 0.565(2) 0.123(6) Uani 0.29(2) 1 d PU D 2 O3SB O 0.4995(16) 0.1042(18) 0.5314(15) 0.123(6) Uani 0.46(2) 1 d PU D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.147(13) 0.062(8) 0.192(17) 0.003(9) 0.054(12) 0.034(8) C2 0.123(10) 0.041(6) 0.112(9) -0.015(6) 0.041(8) 0.001(6) C3 0.091(8) 0.059(6) 0.053(5) -0.025(4) 0.020(5) -0.024(5) C4 0.060(5) 0.049(5) 0.037(4) -0.008(3) 0.013(3) -0.013(4) C5 0.074(6) 0.056(5) 0.051(5) -0.006(4) -0.003(4) -0.022(4) C6 0.076(6) 0.043(5) 0.050(4) -0.008(4) 0.017(4) -0.011(4) C7 0.049(5) 0.036(4) 0.040(4) -0.001(3) 0.010(3) 0.003(3) C8 0.043(4) 0.052(5) 0.041(4) 0.011(3) 0.001(3) 0.000(3) C9 0.035(4) 0.034(4) 0.040(3) 0.001(3) 0.000(3) 0.004(3) C10 0.036(4) 0.047(4) 0.056(4) -0.010(3) 0.009(3) -0.003(3) C11 0.039(4) 0.053(5) 0.037(3) 0.011(3) -0.005(3) 0.009(3) C12 0.040(4) 0.039(4) 0.036(3) 0.001(3) 0.000(3) 0.000(3) N1 0.105(6) 0.041(4) 0.075(5) -0.012(4) 0.040(5) -0.005(4) N2 0.049(4) 0.062(4) 0.046(4) 0.007(3) -0.006(3) -0.003(3) N3 0.047(4) 0.047(4) 0.045(3) -0.005(3) 0.011(3) -0.009(3) N4 0.047(4) 0.041(4) 0.040(3) -0.001(2) 0.009(3) -0.003(3) N5 0.042(4) 0.042(4) 0.053(4) 0.001(3) 0.000(3) -0.008(3) N6 0.050(4) 0.064(4) 0.029(3) 0.003(3) -0.004(3) 0.000(3) N7 0.043(4) 0.040(4) 0.072(4) 0.011(3) 0.015(3) 0.006(3) O4MA 0.122(5) 0.122(5) 0.122(5) 0.0000(10) 0.0000(10) 0.0000(10) O4MB 0.127(4) 0.127(4) 0.127(4) -0.0003(10) 0.0000(10) 0.0000(10) N3M 0.068(5) 0.068(5) 0.047(6) 0.000 0.000 0.000 Ni1 0.0385(5) 0.0361(5) 0.0354(4) -0.0016(4) 0.0052(4) -0.0022(4) O1 0.120(7) 0.064(4) 0.083(5) -0.004(4) 0.051(5) -0.029(4) O2 0.048(3) 0.039(3) 0.037(2) -0.003(2) 0.007(2) -0.004(2) O3 0.036(3) 0.041(3) 0.058(3) 0.014(2) 0.005(2) 0.002(2) O5MA 0.129(5) 0.129(5) 0.129(5) 0.0001(10) 0.0000(10) 0.0001(10) O5MB 0.142(5) 0.142(5) 0.142(5) -0.0002(10) 0.0003(10) 0.0000(10) O6MA 0.135(5) 0.135(5) 0.135(5) 0.0000(10) -0.0001(10) 0.0000(10) O6MB 0.137(5) 0.137(5) 0.137(5) -0.0002(10) -0.0001(10) 0.0001(10) O7M 0.080(7) 0.087(7) 0.049(6) -0.002(5) 0.012(6) 0.012(6) O1M 0.136(4) 0.144(4) 0.143(4) -0.018(3) -0.009(3) 0.003(3) O3M 0.128(4) 0.135(4) 0.120(3) -0.001(3) 0.000(3) 0.006(3) N1MA 0.132(4) 0.135(4) 0.132(4) -0.004(3) -0.009(3) 0.003(3) O2MA 0.145(5) 0.147(5) 0.146(5) -0.001(4) -0.004(4) -0.004(4) N1MB 0.133(4) 0.137(4) 0.133(4) -0.006(3) -0.006(3) 0.002(3) O2MB 0.146(5) 0.141(5) 0.143(5) 0.000(4) -0.005(4) -0.003(4) N2MA 0.129(4) 0.129(4) 0.129(4) 0.0000(10) 0.0000(10) -0.0001(10) N2MB 0.130(4) 0.130(4) 0.130(4) 0.0000(10) -0.0001(10) 0.0000(10) O8M 0.079(9) 0.076(11) 0.052(8) -0.008(8) 0.005(9) -0.005(9) O4S 0.076(5) 0.076(5) 0.076(5) 0.000 0.000 0.0000(10) O3SA 0.123(6) 0.123(6) 0.123(6) -0.0002(10) 0.0001(10) 0.0000(10) O3SB 0.123(6) 0.123(6) 0.123(6) -0.0003(10) -0.0002(10) 0.0001(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 C2 1.503(19) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.264(13) . ? C2 N1 1.328(14) . ? C3 N1 1.466(13) . ? C3 C4 1.553(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.534(10) . ? C4 C5 1.546(13) . ? C4 C6 1.557(12) . ? C5 N2 1.460(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.489(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.242(9) . ? C7 N4 1.319(9) . ? C8 N4 1.459(9) . ? C8 C9 1.542(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.493(10) . ? C9 C11 1.534(9) . ? C9 C10 1.549(10) . ? C10 N5 1.463(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.484(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.249(8) . ? C12 N7 1.317(9) . ? N1 H1 0.8600 . ? N2 Ni1 2.133(6) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.078(6) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.067(6) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.093(6) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? O4MA N2MA 1.216(5) . ? O4MB N2MB 1.216(5) . ? N3M O8M 1.216(5) 2_755 ? N3M O8M 1.216(5) 3_666 ? N3M O8M 1.216(5) 4_646 ? N3M O8M 1.216(5) . ? N3M O7M 1.216(5) 4_646 ? N3M O7M 1.216(5) 2_755 ? N3M O7M 1.216(5) 3_666 ? N3M O7M 1.216(5) . ? Ni1 O3 2.052(5) 8_646 ? Ni1 N5 2.067(6) 8_646 ? Ni1 N6 2.093(6) 8_646 ? Ni1 O2 2.094(5) . ? O3 Ni1 2.052(5) 7_566 ? O5MA N2MA 1.216(5) . ? O5MA O4S 1.38(3) 7_466 ? O5MB N2MB 1.216(5) . ? O6MA N2MA 1.216(5) . ? O6MB N2MB 1.216(5) . ? O7M O8M 0.87(2) 4_646 ? O7M O8M 1.47(3) 3_666 ? O1M N1MA 1.216(5) . ? O1M N1MB 1.216(5) . ? O3M N1MB 1.216(5) . ? O3M N1MA 1.216(5) . ? N1MA O2MA 1.216(5) . ? N1MB O2MB 1.216(5) . ? O8M O8M 0.68(5) 2_755 ? O8M O7M 0.87(2) 3_666 ? O8M O7M 1.47(3) 4_646 ? O4S O5MA 1.38(3) 8_656 ? O4S O5MA 1.38(3) 7_556 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.4(11) . . ? O1 C2 C1 119.7(12) . . ? N1 C2 C1 117.8(12) . . ? N1 C3 C4 114.4(8) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C7 C4 C5 107.7(7) . . ? C7 C4 C3 113.1(7) . . ? C5 C4 C3 107.5(8) . . ? C7 C4 C6 108.8(7) . . ? C5 C4 C6 113.4(7) . . ? C3 C4 C6 106.4(7) . . ? N2 C5 C4 113.3(7) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 112.9(7) . . ? N3 C6 H6A 109.0 . . ? C4 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N4 120.9(6) . . ? O2 C7 C4 119.6(6) . . ? N4 C7 C4 119.3(7) . . ? N4 C8 C9 114.4(6) . . ? N4 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N4 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C12 C9 C11 108.9(6) . . ? C12 C9 C8 114.6(6) . . ? C11 C9 C8 104.4(5) . . ? C12 C9 C10 109.1(6) . . ? C11 C9 C10 110.9(6) . . ? C8 C9 C10 108.9(6) . . ? N5 C10 C9 114.3(6) . . ? N5 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? N5 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C9 114.9(6) . . ? N6 C11 H11A 108.5 . . ? C9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? C9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O3 C12 N7 119.0(7) . . ? O3 C12 C9 120.3(6) . . ? N7 C12 C9 120.7(6) . . ? C2 N1 C3 122.8(10) . . ? C2 N1 H1 118.6 . . ? C3 N1 H1 118.6 . . ? C5 N2 Ni1 117.6(5) . . ? C5 N2 H2A 107.9 . . ? Ni1 N2 H2A 107.9 . . ? C5 N2 H2B 107.9 . . ? Ni1 N2 H2B 107.9 . . ? H2A N2 H2B 107.2 . . ? C6 N3 Ni1 114.6(5) . . ? C6 N3 H3C 108.6 . . ? Ni1 N3 H3C 108.6 . . ? C6 N3 H3D 108.6 . . ? Ni1 N3 H3D 108.6 . . ? H3C N3 H3D 107.6 . . ? C7 N4 C8 123.1(6) . . ? C7 N4 H4 118.4 . . ? C8 N4 H4 118.4 . . ? C10 N5 Ni1 116.3(4) . 7_566 ? C10 N5 H5C 108.2 . . ? Ni1 N5 H5C 108.2 7_566 . ? C10 N5 H5D 108.2 . . ? Ni1 N5 H5D 108.2 7_566 . ? H5C N5 H5D 107.4 . . ? C11 N6 Ni1 116.2(4) . 7_566 ? C11 N6 H6C 108.2 . . ? Ni1 N6 H6C 108.2 7_566 . ? C11 N6 H6D 108.2 . . ? Ni1 N6 H6D 108.2 7_566 . ? H6C N6 H6D 107.4 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O8M N3M O8M 157.1(16) 2_755 3_666 ? O8M N3M O8M 157.1(16) 2_755 4_646 ? O8M N3M O8M 157.1(16) 3_666 . ? O8M N3M O8M 157.1(16) 4_646 . ? O8M N3M O7M 121.0(13) 3_666 4_646 ? O8M N3M O7M 119.97(12) 4_646 4_646 ? O8M N3M O7M 74.4(15) . 4_646 ? O8M N3M O7M 119.97(12) 2_755 2_755 ? O8M N3M O7M 74.3(15) 4_646 2_755 ? O8M N3M O7M 121.1(13) . 2_755 ? O7M N3M O7M 106.2(5) 4_646 2_755 ? O8M N3M O7M 74.3(15) 2_755 3_666 ? O8M N3M O7M 119.97(12) 3_666 3_666 ? O8M N3M O7M 121.0(13) 4_646 3_666 ? O7M N3M O7M 116.1(11) 4_646 3_666 ? O7M N3M O7M 106.2(5) 2_755 3_666 ? O8M N3M O7M 121.1(13) 2_755 . ? O8M N3M O7M 74.3(15) 3_666 . ? O8M N3M O7M 119.97(11) . . ? O7M N3M O7M 106.2(5) 4_646 . ? O7M N3M O7M 116.1(11) 2_755 . ? O7M N3M O7M 106.2(5) 3_666 . ? O3 Ni1 N5 88.8(2) 8_646 8_646 ? O3 Ni1 N3 174.9(2) 8_646 . ? N5 Ni1 N3 94.3(3) 8_646 . ? O3 Ni1 N6 85.1(2) 8_646 8_646 ? N5 Ni1 N6 86.2(3) 8_646 8_646 ? N3 Ni1 N6 99.0(2) . 8_646 ? O3 Ni1 O2 85.95(19) 8_646 . ? N5 Ni1 O2 95.4(2) 8_646 . ? N3 Ni1 O2 89.8(2) . . ? N6 Ni1 O2 170.9(2) 8_646 . ? O3 Ni1 N2 92.2(2) 8_646 . ? N5 Ni1 N2 179.0(3) 8_646 . ? N3 Ni1 N2 84.6(3) . . ? N6 Ni1 N2 94.0(3) 8_646 . ? O2 Ni1 N2 84.6(2) . . ? C7 O2 Ni1 119.5(4) . . ? C12 O3 Ni1 121.1(4) . 7_566 ? N2MA O5MA O4S 144(2) . 7_466 ? O8M O7M N3M 69.1(6) 4_646 . ? N3M O7M O8M 52.8(7) . 3_666 ? O1M N1MA O2MA 119.99(7) . . ? O1M N1MA O3M 119.99(7) . . ? O2MA N1MA O3M 120.02(7) . . ? O3M N1MB O2MB 119.99(7) . . ? O3M N1MB O1M 120.00(7) . . ? O2MB N1MB O1M 120.01(7) . . ? O4MA N2MA O5MA 120.00(9) . . ? O4MA N2MA O6MA 120.00(8) . . ? O5MA N2MA O6MA 120.00(8) . . ? O6MB N2MB O4MB 119.99(10) . . ? O6MB N2MB O5MB 119.98(9) . . ? O4MB N2MB O5MB 119.99(9) . . ? O8M O8M O7M 142.7(5) 2_755 3_666 ? O8M O8M N3M 73.7(12) 2_755 . ? O7M O8M N3M 69.1(6) 3_666 . ? O7M O8M O7M 121.9(6) 3_666 4_646 ? N3M O8M O7M 52.8(7) . 4_646 ? O5MA O4S O5MA 99(3) 8_656 7_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.941 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.107 #===END data_i-4_333K_in_capillary _database_code_depnum_ccdc_archive 'CCDC 856070' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 N36 Ni4 O36' _chemical_formula_weight 2000.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.694(4) _cell_length_b 14.694(4) _cell_length_c 19.014(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4106(3) _cell_formula_units_Z 2 _cell_measurement_temperature 333 _cell_measurement_reflns_used 794 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 16.03 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8713 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set in a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 333 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 10761 _diffrn_reflns_av_R_equivalents 0.1715 _diffrn_reflns_av_sigmaI/netI 0.2217 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3641 _reflns_number_gt 1566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate (N3M, O7M, O8M, and O9M). SIMU and ISOR restraints are applied for [(N2MB, O4MB, O5MB, and O6MB) and (N3M, O7M, O8M, and O9M)]. ; _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^)+(0.0244P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 3641 _refine_ls_number_parameters 336 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1988 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 0.6669(8) 1.0878(7) 0.7724(5) 0.083(4) Uani 1 1 d . . . H1A H 0.6755 1.1523 0.7771 0.124 Uiso 1 1 calc R . . H1B H 0.6116 1.0703 0.7955 0.124 Uiso 1 1 calc R . . H1C H 0.6634 1.0722 0.7235 0.124 Uiso 1 1 calc R . . C2 C 0.7460(9) 1.0388(7) 0.8056(6) 0.059(3) Uani 1 1 d . . . C3 C 0.7926(6) 0.9463(6) 0.9069(5) 0.057(3) Uani 1 1 d . . . H3A H 0.7910 0.9690 0.9548 0.068 Uiso 1 1 calc R . . H3B H 0.8523 0.9599 0.8878 0.068 Uiso 1 1 calc R . . C4 C 0.7797(6) 0.8432(6) 0.9082(5) 0.045(3) Uani 1 1 d . . . C5 C 0.8557(6) 0.8059(6) 0.9572(5) 0.058(3) Uani 1 1 d . . . H5A H 0.9122 0.8375 0.9471 0.069 Uiso 1 1 calc R . . H5B H 0.8396 0.8185 1.0057 0.069 Uiso 1 1 calc R . . C6 C 0.6861(7) 0.8211(6) 0.9387(5) 0.058(3) Uani 1 1 d . . . H6A H 0.6741 0.8622 0.9775 0.070 Uiso 1 1 calc R . . H6B H 0.6405 0.8326 0.9029 0.070 Uiso 1 1 calc R . . C7 C 0.7913(6) 0.7960(7) 0.8375(5) 0.041(3) Uani 1 1 d . . . C8 C 0.8493(6) 0.7934(6) 0.7193(5) 0.050(3) Uani 1 1 d . . . H8A H 0.8220 0.8286 0.6816 0.060 Uiso 1 1 calc R . . H8B H 0.8180 0.7353 0.7210 0.060 Uiso 1 1 calc R . . C9 C 0.9489(6) 0.7756(6) 0.7002(5) 0.041(2) Uani 1 1 d . . . C10 C 0.9850(7) 0.8604(6) 0.6653(5) 0.059(3) Uani 1 1 d . . . H10A H 0.9431 0.8772 0.6281 0.071 Uiso 1 1 calc R . . H10B H 0.9843 0.9091 0.6997 0.071 Uiso 1 1 calc R . . C11 C 0.9478(6) 0.6946(6) 0.6510(5) 0.052(3) Uani 1 1 d . . . H11A H 0.9112 0.6469 0.6720 0.062 Uiso 1 1 calc R . . H11B H 0.9185 0.7125 0.6074 0.062 Uiso 1 1 calc R . . C12 C 0.9951(7) 0.7462(8) 0.7700(5) 0.047(3) Uani 1 1 d . . . N1 N 0.7237(6) 0.9947(5) 0.8652(4) 0.054(2) Uani 1 1 d . . . H1 H 0.6681 0.9949 0.8792 0.064 Uiso 1 1 calc R . . N2 N 0.8697(5) 0.7084(5) 0.9487(4) 0.055(2) Uani 1 1 d . . . H2A H 0.8881 0.6855 0.9903 0.066 Uiso 1 1 calc R . . H2B H 0.9154 0.7000 0.9178 0.066 Uiso 1 1 calc R . . N3 N 0.6760(5) 0.7286(5) 0.9633(4) 0.048(2) Uani 1 1 d . . . H3C H 0.6173 0.7124 0.9583 0.057 Uiso 1 1 calc R . . H3D H 0.6888 0.7275 1.0096 0.057 Uiso 1 1 calc R . . N4 N 0.8326(5) 0.8410(5) 0.7856(4) 0.046(2) Uani 1 1 d . . . H4 H 0.8490 0.8967 0.7910 0.055 Uiso 1 1 calc R . . N5 N 1.0766(5) 0.8559(5) 0.6350(4) 0.056(2) Uani 1 1 d . . . H5C H 1.1151 0.8704 0.6701 0.067 Uiso 1 1 calc R . . H5D H 1.0799 0.9017 0.6037 0.067 Uiso 1 1 calc R . . N6 N 1.0388(5) 0.6568(5) 0.6341(4) 0.049(2) Uani 1 1 d . . . H6C H 1.0309 0.6084 0.6058 0.059 Uiso 1 1 calc R . . H6D H 1.0638 0.6364 0.6743 0.059 Uiso 1 1 calc R . . N7 N 1.0515(6) 0.8044(6) 0.8003(5) 0.088(3) Uani 1 1 d . . . H7A H 1.0767 0.7908 0.8397 0.105 Uiso 1 1 calc R . . H7B H 1.0629 0.8558 0.7806 0.105 Uiso 1 1 calc R . . N1M N 0.7608(7) 0.5689(7) 1.0668(5) 0.077(3) Uani 1 1 d D . . N2MA N 0.5000 1.0000 0.9682(9) 0.081(5) Uani 1 2 d SD . . N3M N 0.5065(19) 0.4872(19) 1.0098(17) 0.061(7) Uani 0.25 1 d PDU A -1 N2MB N 0.988(5) 0.011(2) 0.9593(12) 0.072(9) Uani 0.25 1 d PDU B -2 Ni1 Ni 0.75564(8) 0.63214(8) 0.91395(6) 0.0468(3) Uani 1 1 d . . . O1 O 0.8227(6) 1.0363(5) 0.7792(4) 0.078(2) Uani 1 1 d . . . O2 O 0.7621(4) 0.7171(4) 0.8293(3) 0.0461(18) Uani 1 1 d . . . O3 O 0.9777(5) 0.6728(5) 0.7968(4) 0.072(2) Uani 1 1 d . . . O1M O 0.7449(6) 0.5102(6) 1.1115(4) 0.099(3) Uani 1 1 d . . . O2M O 0.7554(5) 0.5414(4) 1.0030(4) 0.074(2) Uani 1 1 d . . . O3M O 0.7763(6) 0.6481(5) 1.0801(4) 0.084(2) Uani 1 1 d D . . O4MA O 0.5682(7) 1.0028(8) 0.9980(7) 0.200(7) Uani 1 1 d D . . O5MA O 0.5000 1.0000 0.9066(9) 0.194(9) Uani 1 2 d SD . . O9M O 0.567(2) 0.541(3) 1.011(2) 0.106(11) Uani 0.25 1 d PDU A -1 O7M O 0.505(2) 0.4262(17) 0.968(2) 0.061(9) Uani 0.25 1 d PDU A -1 O8M O 0.453(2) 0.487(2) 1.0567(15) 0.069(9) Uani 0.25 1 d PDU A -1 O4MB O 0.9562(18) 0.0810(15) 0.9399(12) 0.053(7) Uani 0.25 1 d PDU B -2 O5MB O 1.015(3) -0.0429(18) 0.9164(14) 0.103(10) Uani 0.25 1 d PDU B -2 O6MB O 0.973(3) -0.014(3) 1.0189(13) 0.088(12) Uani 0.25 1 d PDU B -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 0.126(11) 0.072(9) 0.050(8) 0.007(7) 0.003(8) 0.013(8) C2 0.095(11) 0.022(6) 0.059(9) 0.003(6) -0.006(8) 0.004(7) C3 0.078(7) 0.056(7) 0.036(6) -0.002(6) -0.003(7) 0.009(6) C4 0.067(8) 0.024(5) 0.044(6) -0.001(6) 0.001(6) 0.001(4) C5 0.078(8) 0.046(7) 0.049(7) -0.022(6) -0.017(6) 0.015(7) C6 0.093(9) 0.046(7) 0.037(7) -0.009(5) 0.013(6) 0.000(6) C7 0.032(6) 0.061(8) 0.030(6) 0.010(6) -0.001(5) 0.011(6) C8 0.054(7) 0.048(7) 0.049(7) -0.006(5) -0.001(6) 0.002(6) C9 0.037(6) 0.044(7) 0.043(6) 0.012(5) 0.008(5) 0.004(5) C10 0.059(8) 0.071(9) 0.048(7) 0.007(6) 0.009(6) -0.001(6) C11 0.046(7) 0.058(7) 0.052(7) -0.003(6) 0.015(6) 0.003(6) C12 0.041(7) 0.062(9) 0.038(7) -0.020(6) 0.008(6) 0.010(7) N1 0.065(6) 0.033(5) 0.063(6) 0.003(5) -0.005(5) -0.005(5) N2 0.069(6) 0.052(6) 0.044(5) 0.001(4) 0.000(5) -0.004(5) N3 0.062(6) 0.048(6) 0.033(5) -0.007(4) 0.007(5) 0.002(5) N4 0.041(5) 0.042(5) 0.055(6) 0.001(5) 0.006(4) -0.001(4) N5 0.045(5) 0.065(6) 0.058(6) 0.014(5) 0.016(5) 0.005(5) N6 0.054(6) 0.059(6) 0.034(5) -0.002(4) 0.006(4) -0.010(5) N7 0.086(8) 0.117(9) 0.061(6) -0.012(6) -0.022(6) -0.026(7) N1M 0.101(8) 0.076(8) 0.053(8) -0.006(7) 0.037(7) 0.010(8) N2MA 0.087(14) 0.079(12) 0.078(13) 0.000 0.000 0.002(12) N3M 0.060(10) 0.061(10) 0.063(10) -0.003(8) 0.001(8) 0.001(8) N2MB 0.072(11) 0.078(11) 0.067(11) -0.007(8) 0.005(8) -0.005(8) Ni1 0.0569(9) 0.0441(8) 0.0394(6) -0.0033(7) 0.0076(8) 0.0006(8) O1 0.086(6) 0.067(6) 0.080(6) 0.009(5) 0.017(5) -0.007(5) O2 0.070(5) 0.033(4) 0.035(4) -0.004(3) 0.003(3) -0.007(4) O3 0.081(6) 0.069(6) 0.064(5) 0.029(5) -0.005(4) 0.001(5) O1M 0.164(9) 0.086(6) 0.048(6) 0.016(5) 0.022(5) -0.002(6) O2M 0.116(6) 0.054(5) 0.053(4) -0.005(4) 0.017(5) 0.013(5) O3M 0.140(7) 0.061(5) 0.051(4) -0.016(5) 0.007(6) 0.006(5) O4MA 0.128(10) 0.115(8) 0.357(18) -0.115(11) -0.105(11) 0.031(8) O5MA 0.28(2) 0.199(18) 0.100(14) 0.000 0.000 0.077(16) O9M 0.105(13) 0.110(13) 0.104(13) 0.001(9) 0.003(9) -0.004(9) O7M 0.065(12) 0.067(12) 0.051(12) -0.009(9) -0.015(9) 0.013(9) O8M 0.080(12) 0.074(11) 0.054(12) 0.008(9) 0.015(8) 0.000(9) O4MB 0.058(10) 0.048(10) 0.054(11) -0.006(8) 0.009(8) 0.002(8) O5MB 0.096(12) 0.102(13) 0.112(12) -0.019(9) 0.008(9) -0.002(9) O6MB 0.091(14) 0.083(14) 0.090(14) -0.001(9) -0.006(9) 0.009(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 C2 1.506(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.235(12) . ? C2 N1 1.346(12) . ? C3 N1 1.469(10) . ? C3 C4 1.527(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.522(12) . ? C4 C6 1.528(12) . ? C4 C5 1.555(11) . ? C5 N2 1.457(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.446(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.245(10) . ? C7 N4 1.335(10) . ? C8 N4 1.462(9) . ? C8 C9 1.530(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.508(11) . ? C9 C11 1.515(12) . ? C9 C12 1.551(12) . ? C10 N5 1.466(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.482(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.221(11) . ? C12 N7 1.322(12) . ? N1 H1 0.8600 . ? N2 Ni1 2.122(7) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.064(7) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.054(8) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.091(7) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N1M O3M 1.213(8) . ? N1M O1M 1.235(10) . ? N1M O2M 1.280(10) . ? N2MA O4MA 1.152(9) 2_675 ? N2MA O4MA 1.152(9) . ? N2MA O5MA 1.170(12) . ? N3M O9M 1.190(15) . ? N3M O8M 1.191(14) . ? N3M O7M 1.199(14) . ? N2MB O4MB 1.193(15) . ? N2MB O5MB 1.198(15) . ? N2MB O6MB 1.211(16) . ? Ni1 O2 2.039(6) . ? Ni1 N5 2.054(8) 8_646 ? Ni1 N6 2.091(7) 8_646 ? Ni1 O2M 2.156(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 123.4(11) . . ? O1 C2 C1 123.2(11) . . ? N1 C2 C1 113.3(11) . . ? N1 C3 C4 113.8(7) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C7 C4 C3 115.1(9) . . ? C7 C4 C6 109.8(8) . . ? C3 C4 C6 109.2(7) . . ? C7 C4 C5 106.7(7) . . ? C3 C4 C5 105.7(7) . . ? C6 C4 C5 110.1(8) . . ? N2 C5 C4 112.4(7) . . ? N2 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N3 C6 C4 114.5(8) . . ? N3 C6 H6A 108.6 . . ? C4 C6 H6A 108.6 . . ? N3 C6 H6B 108.6 . . ? C4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N4 121.7(9) . . ? O2 C7 C4 119.8(9) . . ? N4 C7 C4 118.5(9) . . ? N4 C8 C9 116.6(8) . . ? N4 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? N4 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C11 112.4(8) . . ? C10 C9 C8 107.4(7) . . ? C11 C9 C8 105.7(8) . . ? C10 C9 C12 116.9(9) . . ? C11 C9 C12 108.4(8) . . ? C8 C9 C12 105.3(7) . . ? N5 C10 C9 117.4(9) . . ? N5 C10 H10A 108.0 . . ? C9 C10 H10A 108.0 . . ? N5 C10 H10B 108.0 . . ? C9 C10 H10B 108.0 . . ? H10A C10 H10B 107.2 . . ? N6 C11 C9 114.7(7) . . ? N6 C11 H11A 108.6 . . ? C9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 121.3(11) . . ? O3 C12 C9 120.8(10) . . ? N7 C12 C9 117.9(10) . . ? C2 N1 C3 121.3(9) . . ? C2 N1 H1 119.4 . . ? C3 N1 H1 119.4 . . ? C5 N2 Ni1 116.3(6) . . ? C5 N2 H2A 108.2 . . ? Ni1 N2 H2A 108.2 . . ? C5 N2 H2B 108.2 . . ? Ni1 N2 H2B 108.2 . . ? H2A N2 H2B 107.4 . . ? C6 N3 Ni1 116.1(6) . . ? C6 N3 H3C 108.3 . . ? Ni1 N3 H3C 108.3 . . ? C6 N3 H3D 108.3 . . ? Ni1 N3 H3D 108.3 . . ? H3C N3 H3D 107.4 . . ? C7 N4 C8 118.5(8) . . ? C7 N4 H4 120.8 . . ? C8 N4 H4 120.8 . . ? C10 N5 Ni1 125.3(6) . 7_566 ? C10 N5 H5C 106.0 . . ? Ni1 N5 H5C 106.0 7_566 . ? C10 N5 H5D 106.0 . . ? Ni1 N5 H5D 106.0 7_566 . ? H5C N5 H5D 106.3 . . ? C11 N6 Ni1 117.1(5) . 7_566 ? C11 N6 H6C 108.0 . . ? Ni1 N6 H6C 108.0 7_566 . ? C11 N6 H6D 108.0 . . ? Ni1 N6 H6D 108.0 7_566 . ? H6C N6 H6D 107.3 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3M N1M O1M 124.3(10) . . ? O3M N1M O2M 120.8(10) . . ? O1M N1M O2M 114.8(9) . . ? O4MA N2MA O4MA 121(2) 2_675 . ? O4MA N2MA O5MA 119.5(11) 2_675 . ? O4MA N2MA O5MA 119.5(11) . . ? O9M N3M O8M 119.1(15) . . ? O9M N3M O7M 121.7(15) . . ? O8M N3M O7M 118.4(15) . . ? O4MB N2MB O5MB 119.2(18) . . ? O4MB N2MB O6MB 118.4(18) . . ? O5MB N2MB O6MB 120.0(19) . . ? O2 Ni1 N5 85.6(3) . 8_646 ? O2 Ni1 N3 88.0(3) . . ? N5 Ni1 N3 91.5(3) 8_646 . ? O2 Ni1 N6 91.6(3) . 8_646 ? N5 Ni1 N6 91.8(3) 8_646 8_646 ? N3 Ni1 N6 176.6(3) . 8_646 ? O2 Ni1 N2 83.5(3) . . ? N5 Ni1 N2 168.9(3) 8_646 . ? N3 Ni1 N2 86.8(3) . . ? N6 Ni1 N2 89.8(3) 8_646 . ? O2 Ni1 O2M 177.4(3) . . ? N5 Ni1 O2M 96.3(3) 8_646 . ? N3 Ni1 O2M 93.8(3) . . ? N6 Ni1 O2M 86.5(3) 8_646 . ? N2 Ni1 O2M 94.8(3) . . ? C7 O2 Ni1 119.2(6) . . ? N1M O2M Ni1 123.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.333 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.071 #===END data_i-4_313K_in_capillary_after_333K _database_code_depnum_ccdc_archive 'CCDC 856071' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H116 N36 Ni4 O40' _chemical_formula_weight 2072.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.470(3) _cell_length_b 15.470(3) _cell_length_c 19.437(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4652(2) _cell_formula_units_Z 2 _cell_measurement_temperature 313 _cell_measurement_reflns_used 1135 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 18.03 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9235 _exptl_absorpt_correction_T_max 0.9564 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set to 313K after measuring at 333K. Measurement was done by using a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 313 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 8909 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.1734 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.17 _reflns_number_total 4178 _reflns_number_gt 2014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1234P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 4178 _refine_ls_number_parameters 380 _refine_ls_number_restraints 411 _refine_ls_R_factor_all 0.1807 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.913 _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 0.7118(14) 1.0901(13) 0.8072(11) 0.149(9) Uani 1 1 d . . . H1A H 0.6651 1.0592 0.7858 0.223 Uiso 1 1 calc R . . H1B H 0.7369 1.1293 0.7745 0.223 Uiso 1 1 calc R . . H1C H 0.6902 1.1222 0.8458 0.223 Uiso 1 1 calc R . . C2 C 0.7817(14) 1.0249(9) 0.8321(9) 0.096(5) Uani 1 1 d . . . C3 C 0.8106(9) 0.9095(8) 0.9176(6) 0.066(4) Uani 1 1 d . . . H3A H 0.8087 0.9177 0.9670 0.079 Uiso 1 1 calc R . . H3B H 0.8692 0.9210 0.9024 0.079 Uiso 1 1 calc R . . C4 C 0.7877(9) 0.8129(9) 0.9009(6) 0.060(3) Uani 1 1 d . . . C5 C 0.8541(10) 0.7573(8) 0.9383(7) 0.071(4) Uani 1 1 d . . . H5A H 0.9115 0.7788 0.9279 0.085 Uiso 1 1 calc R . . H5B H 0.8451 0.7629 0.9875 0.085 Uiso 1 1 calc R . . C6 C 0.6909(9) 0.8005(8) 0.9292(7) 0.066(4) Uani 1 1 d . . . H6A H 0.6843 0.8307 0.9727 0.079 Uiso 1 1 calc R . . H6B H 0.6500 0.8247 0.8967 0.079 Uiso 1 1 calc R . . C7 C 0.7932(8) 0.7926(8) 0.8255(6) 0.051(3) Uani 1 1 d . . . C8 C 0.8445(7) 0.8251(7) 0.7107(5) 0.046(3) Uani 1 1 d . . . H8A H 0.8238 0.8757 0.6862 0.055 Uiso 1 1 calc R . . H8B H 0.8066 0.7774 0.6992 0.055 Uiso 1 1 calc R . . C9 C 0.9376(7) 0.8034(7) 0.6846(5) 0.045(3) Uani 1 1 d . . . C10 C 0.9978(7) 0.8773(7) 0.7112(6) 0.052(3) Uani 1 1 d . . . H10A H 0.9690 0.9325 0.7050 0.062 Uiso 1 1 calc R . . H10B H 1.0081 0.8694 0.7600 0.062 Uiso 1 1 calc R . . C11 C 0.9317(7) 0.8053(7) 0.6061(5) 0.045(3) Uani 1 1 d . . . H11A H 0.8835 0.7695 0.5919 0.054 Uiso 1 1 calc R . . H11B H 0.9195 0.8641 0.5917 0.054 Uiso 1 1 calc R . . C12 C 0.9713(8) 0.7190(7) 0.7073(6) 0.050(3) Uani 1 1 d . . . N1 N 0.7514(9) 0.9727(7) 0.8846(6) 0.085(4) Uani 1 1 d . . . H1 H 0.6986 0.9768 0.8980 0.102 Uiso 1 1 calc R . . N2 N 0.8496(6) 0.6659(7) 0.9196(5) 0.063(3) Uani 1 1 d . . . H2A H 0.8577 0.6345 0.9581 0.076 Uiso 1 1 calc R . . H2B H 0.8939 0.6543 0.8911 0.076 Uiso 1 1 calc R . . N3 N 0.6730(6) 0.7073(6) 0.9390(4) 0.049(2) Uani 1 1 d . . . H3C H 0.6155 0.6992 0.9356 0.059 Uiso 1 1 calc R . . H3D H 0.6885 0.6929 0.9821 0.059 Uiso 1 1 calc R . . N4 N 0.8383(6) 0.8413(6) 0.7833(4) 0.048(2) Uani 1 1 d . . . H4 H 0.8655 0.8850 0.8000 0.058 Uiso 1 1 calc R . . N5 N 1.0819(6) 0.8790(6) 0.6745(5) 0.053(2) Uani 1 1 d . . . H5C H 1.1228 0.8954 0.7047 0.064 Uiso 1 1 calc R . . H5D H 1.0790 0.9202 0.6419 0.064 Uiso 1 1 calc R . . N6 N 1.0113(6) 0.7749(6) 0.5701(4) 0.056(3) Uani 1 1 d . . . H6C H 1.0216 0.8109 0.5347 0.068 Uiso 1 1 calc R . . H6D H 1.0004 0.7224 0.5523 0.068 Uiso 1 1 calc R . . N7 N 0.9216(6) 0.6635(6) 0.7419(5) 0.063(3) Uani 1 1 d . . . H7A H 0.9428 0.6153 0.7562 0.075 Uiso 1 1 calc R . . H7B H 0.8683 0.6758 0.7499 0.075 Uiso 1 1 calc R . . O4MA O 0.0971(16) 0.5440(18) 0.945(2) 0.132(6) Uani 0.25 1 d PDU A 3 O4MB O 0.0961(13) 0.6067(9) 0.9190(12) 0.136(5) Uani 0.50 1 d PDU B 4 N3M N 1.0000 0.0000 0.5000 0.085(6) Uani 1 4 d SDU . . Ni1 Ni 0.73345(8) 0.62273(9) 0.87170(7) 0.0461(4) Uani 1 1 d . . . O1 O 0.8514(8) 1.0194(6) 0.8061(6) 0.100(4) Uani 1 1 d . . . O2 O 0.7559(5) 0.7253(5) 0.8031(4) 0.0493(18) Uani 1 1 d . . . O3 O 1.0492(5) 0.6987(5) 0.6965(4) 0.0520(19) Uani 1 1 d . . . O5MA O 0.012(2) 0.5598(19) 0.862(2) 0.138(6) Uani 0.25 1 d PDU A 3 O5MB O 0.1550(10) 0.7284(11) 0.9093(13) 0.148(6) Uani 0.50 1 d PDU B 4 O6MA O 0.041(3) 0.6653(17) 0.926(2) 0.142(5) Uani 0.25 1 d PDU A 3 O6MB O 0.0316(10) 0.7072(13) 0.8675(12) 0.144(6) Uani 0.50 1 d PDU B 4 O7M O 0.9347(7) 0.0163(13) 0.5321(8) 0.091(5) Uani 0.50 1 d PDU . . O1M O 0.4899(7) 0.7215(7) 0.8979(6) 0.161(4) Uani 1 1 d DU . . O3M O 0.3770(7) 0.7806(7) 0.9352(6) 0.153(4) Uani 1 1 d DU . . N1MA N 0.4445(6) 0.7850(6) 0.9037(5) 0.157(4) Uani 0.482(16) 1 d PDU C 1 O2MA O 0.4666(12) 0.8529(9) 0.8779(14) 0.164(5) Uani 0.482(16) 1 d PDU C 1 N1MB N 0.4544(6) 0.7822(6) 0.9256(6) 0.157(4) Uani 0.518(16) 1 d PDU C 2 O2MB O 0.4964(9) 0.8444(11) 0.9435(15) 0.164(5) Uani 0.518(16) 1 d PDU C 2 N2MA N 0.0515(17) 0.5901(14) 0.9101(18) 0.139(5) Uani 0.25 1 d PDU A 3 N2MB N 0.0933(9) 0.6814(8) 0.9001(9) 0.141(5) Uani 0.50 1 d PDU B 4 O8M O 1.0050(17) 0.019(2) 0.4396(6) 0.091(7) Uani 0.25 1 d PDU . . O4S O 1.0000 0.5000 0.6822(12) 0.070(6) Uani 0.50 2 d SPU . . O3SA O 0.504(3) 0.073(3) 0.560(3) 0.129(8) Uani 0.36(4) 1 d PU D 2 O3SB O 0.502(2) 0.112(3) 0.529(2) 0.129(8) Uani 0.39(4) 1 d PU D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.158(19) 0.108(15) 0.18(2) 0.044(15) 0.068(17) 0.038(15) C2 0.141(17) 0.035(8) 0.111(13) -0.001(8) 0.025(12) -0.009(10) C3 0.080(10) 0.069(9) 0.050(8) -0.003(7) 0.015(7) -0.024(8) C4 0.068(9) 0.066(9) 0.046(7) -0.001(6) 0.002(6) -0.015(7) C5 0.083(10) 0.073(9) 0.056(8) -0.023(7) -0.003(7) -0.008(8) C6 0.074(9) 0.056(8) 0.068(9) -0.008(7) 0.014(7) -0.005(7) C7 0.048(7) 0.046(7) 0.059(8) -0.003(6) 0.008(6) 0.000(6) C8 0.037(6) 0.057(7) 0.043(7) 0.016(5) -0.003(5) 0.000(5) C9 0.038(6) 0.048(7) 0.048(7) -0.012(5) 0.002(5) 0.005(5) C10 0.052(7) 0.044(7) 0.059(7) -0.002(5) 0.007(5) -0.013(6) C11 0.039(6) 0.052(7) 0.044(7) 0.011(5) -0.005(5) 0.008(5) C12 0.052(8) 0.045(7) 0.054(7) -0.007(5) -0.001(5) -0.008(6) N1 0.126(10) 0.052(6) 0.076(8) -0.013(6) 0.047(8) 0.003(7) N2 0.066(7) 0.065(7) 0.058(6) -0.003(5) 0.008(5) -0.009(6) N3 0.056(6) 0.044(6) 0.047(6) 0.000(4) 0.008(4) -0.011(5) N4 0.048(5) 0.047(6) 0.050(6) -0.004(4) 0.014(4) -0.004(5) N5 0.045(6) 0.036(5) 0.079(7) 0.017(5) 0.005(5) -0.002(4) N6 0.067(7) 0.062(6) 0.040(6) 0.009(4) 0.008(5) 0.002(5) N7 0.059(6) 0.050(6) 0.080(7) 0.010(5) 0.022(5) 0.010(5) O4MA 0.132(6) 0.132(6) 0.132(6) 0.0000(10) 0.0000(10) 0.0000(10) O4MB 0.136(5) 0.136(5) 0.136(5) -0.0002(10) -0.0001(10) 0.0000(10) N3M 0.102(9) 0.102(9) 0.052(12) 0.000 0.000 0.000 Ni1 0.0461(8) 0.0452(8) 0.0469(7) -0.0011(7) 0.0060(7) -0.0020(8) O1 0.118(9) 0.070(7) 0.113(9) -0.008(6) 0.071(7) -0.023(6) O2 0.043(4) 0.052(5) 0.054(5) -0.006(4) 0.007(3) 0.000(4) O3 0.035(4) 0.055(5) 0.066(5) 0.014(4) 0.007(4) -0.001(4) O5MA 0.138(6) 0.138(6) 0.138(6) 0.0000(10) 0.0000(10) 0.0001(10) O5MB 0.148(6) 0.148(6) 0.148(6) -0.0002(10) 0.0001(10) -0.0001(10) O6MA 0.142(6) 0.142(6) 0.142(6) 0.0001(10) 0.0000(10) 0.0000(10) O6MB 0.144(6) 0.144(6) 0.144(6) -0.0001(10) -0.0001(10) 0.0001(10) O7M 0.108(11) 0.110(10) 0.054(11) -0.009(7) 0.010(7) 0.011(8) O1M 0.157(5) 0.163(5) 0.162(5) -0.013(3) -0.007(3) 0.002(3) O3M 0.154(5) 0.157(5) 0.149(4) -0.001(3) -0.002(3) 0.004(3) N1MA 0.156(5) 0.158(4) 0.156(4) -0.003(3) -0.007(3) 0.002(3) O2MA 0.163(6) 0.165(6) 0.164(6) 0.000(4) -0.005(4) -0.003(4) N1MB 0.156(5) 0.159(4) 0.156(4) -0.004(3) -0.006(3) 0.001(3) O2MB 0.165(6) 0.163(6) 0.163(6) 0.000(4) -0.003(4) -0.001(4) N2MA 0.139(5) 0.139(5) 0.139(5) 0.0000(10) 0.0001(10) 0.0000(10) N2MB 0.141(5) 0.141(5) 0.141(5) 0.0000(10) 0.0000(10) 0.0001(10) O8M 0.108(12) 0.105(13) 0.060(13) -0.001(9) 0.003(10) -0.002(10) O4S 0.070(6) 0.070(6) 0.070(6) 0.000 0.000 0.0001(10) O3SA 0.129(8) 0.129(8) 0.129(8) -0.0002(10) 0.0000(10) -0.0001(10) O3SB 0.129(8) 0.129(8) 0.129(8) -0.0002(10) -0.0001(10) -0.0001(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 C2 1.56(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.193(19) . ? C2 N1 1.383(19) . ? C3 N1 1.485(16) . ? C3 C4 1.570(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.500(17) . ? C4 C5 1.524(19) . ? C4 C6 1.608(18) . ? C5 N2 1.461(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.480(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.268(13) . ? C7 N4 1.314(14) . ? C8 N4 1.436(12) . ? C8 C9 1.564(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.473(16) . ? C9 C11 1.527(14) . ? C9 C10 1.563(14) . ? C10 N5 1.484(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.493(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.263(13) . ? C12 N7 1.334(14) . ? N1 H1 0.8600 . ? N2 Ni1 2.132(10) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.073(9) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.057(9) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.065(9) 7_566 ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? O4MA N2MA 1.213(6) . ? O4MB N2MB 1.213(6) . ? N3M O8M 1.213(6) 2_755 ? N3M O8M 1.213(6) 3_666 ? N3M O8M 1.213(6) 4_646 ? N3M O8M 1.213(6) . ? N3M O7M 1.213(6) . ? N3M O7M 1.213(6) 4_646 ? N3M O7M 1.213(6) 2_755 ? N3M O7M 1.213(6) 3_666 ? Ni1 O3 2.038(7) 8_646 ? Ni1 N5 2.057(9) 8_646 ? Ni1 N6 2.065(9) 8_646 ? Ni1 O2 2.102(7) . ? O3 Ni1 2.038(7) 7_566 ? O5MA N2MA 1.213(6) . ? O5MA O4S 1.27(3) 7_466 ? O5MB N2MB 1.213(6) . ? O6MA N2MA 1.213(6) . ? O6MB N2MB 1.213(6) . ? O7M O8M 0.92(4) 4_646 ? O7M O8M 1.46(4) 3_666 ? O1M N1MA 1.213(6) . ? O1M N1MB 1.213(6) . ? O3M N1MB 1.213(6) . ? O3M N1MA 1.213(6) . ? N1MA O2MA 1.213(6) . ? N1MB O2MB 1.213(6) . ? O8M O8M 0.62(8) 2_755 ? O8M O7M 0.92(4) 3_666 ? O8M O7M 1.46(4) 4_646 ? O4S O5MA 1.27(3) 8_656 ? O4S O5MA 1.27(3) 7_556 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 125.2(16) . . ? O1 C2 C1 122.8(16) . . ? N1 C2 C1 111.9(17) . . ? N1 C3 C4 113.5(11) . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C7 C4 C5 108.0(11) . . ? C7 C4 C3 112.8(10) . . ? C5 C4 C3 106.7(11) . . ? C7 C4 C6 111.3(10) . . ? C5 C4 C6 113.4(11) . . ? C3 C4 C6 104.6(10) . . ? N2 C5 C4 113.3(10) . . ? N2 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N3 C6 C4 109.5(10) . . ? N3 C6 H6A 109.8 . . ? C4 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C4 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? O2 C7 N4 119.8(10) . . ? O2 C7 C4 118.8(11) . . ? N4 C7 C4 121.3(11) . . ? N4 C8 C9 114.7(8) . . ? N4 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N4 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C12 C9 C11 109.8(9) . . ? C12 C9 C10 109.8(9) . . ? C11 C9 C10 110.6(9) . . ? C12 C9 C8 114.7(9) . . ? C11 C9 C8 105.3(8) . . ? C10 C9 C8 106.5(8) . . ? N5 C10 C9 112.1(9) . . ? N5 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N5 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N6 C11 C9 114.3(8) . . ? N6 C11 H11A 108.7 . . ? C9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? C9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N7 118.2(11) . . ? O3 C12 C9 120.5(10) . . ? N7 C12 C9 121.2(11) . . ? C2 N1 C3 119.6(13) . . ? C2 N1 H1 120.2 . . ? C3 N1 H1 120.2 . . ? C5 N2 Ni1 116.8(8) . . ? C5 N2 H2A 108.1 . . ? Ni1 N2 H2A 108.1 . . ? C5 N2 H2B 108.1 . . ? Ni1 N2 H2B 108.1 . . ? H2A N2 H2B 107.3 . . ? C6 N3 Ni1 116.7(7) . . ? C6 N3 H3C 108.1 . . ? Ni1 N3 H3C 108.1 . . ? C6 N3 H3D 108.1 . . ? Ni1 N3 H3D 108.1 . . ? H3C N3 H3D 107.3 . . ? C7 N4 C8 123.3(10) . . ? C7 N4 H4 118.3 . . ? C8 N4 H4 118.3 . . ? C10 N5 Ni1 117.7(7) . 7_566 ? C10 N5 H5C 107.9 . . ? Ni1 N5 H5C 107.9 7_566 . ? C10 N5 H5D 107.9 . . ? Ni1 N5 H5D 107.9 7_566 . ? H5C N5 H5D 107.2 . . ? C11 N6 Ni1 116.9(6) . 7_566 ? C11 N6 H6C 108.1 . . ? Ni1 N6 H6C 108.1 7_566 . ? C11 N6 H6D 108.1 . . ? Ni1 N6 H6D 108.1 7_566 . ? H6C N6 H6D 107.3 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O8M N3M O8M 159(3) 2_755 3_666 ? O8M N3M O8M 159(3) 2_755 4_646 ? O8M N3M O8M 159(3) 3_666 . ? O8M N3M O8M 159(3) 4_646 . ? O8M N3M O7M 119.7(18) 2_755 . ? O8M N3M O7M 74(2) 3_666 . ? O8M N3M O7M 119.96(12) . . ? O8M N3M O7M 119.7(18) 3_666 4_646 ? O8M N3M O7M 119.96(12) 4_646 4_646 ? O8M N3M O7M 74(2) . 4_646 ? O7M N3M O7M 105.3(8) . 4_646 ? O8M N3M O7M 119.96(12) 2_755 2_755 ? O8M N3M O7M 74(2) 4_646 2_755 ? O8M N3M O7M 119.7(18) . 2_755 ? O7M N3M O7M 118.1(16) . 2_755 ? O7M N3M O7M 105.3(7) 4_646 2_755 ? O8M N3M O7M 74(2) 2_755 3_666 ? O8M N3M O7M 119.96(12) 3_666 3_666 ? O8M N3M O7M 119.7(18) 4_646 3_666 ? O7M N3M O7M 105.3(7) . 3_666 ? O7M N3M O7M 118.1(16) 4_646 3_666 ? O7M N3M O7M 105.3(8) 2_755 3_666 ? O3 Ni1 N5 88.9(3) 8_646 8_646 ? O3 Ni1 N6 85.6(3) 8_646 8_646 ? N5 Ni1 N6 85.9(4) 8_646 8_646 ? O3 Ni1 N3 174.3(3) 8_646 . ? N5 Ni1 N3 95.0(4) 8_646 . ? N6 Ni1 N3 98.8(3) 8_646 . ? O3 Ni1 O2 85.6(3) 8_646 . ? N5 Ni1 O2 95.4(3) 8_646 . ? N6 Ni1 O2 171.0(3) 8_646 . ? N3 Ni1 O2 89.9(3) . . ? O3 Ni1 N2 91.4(4) 8_646 . ? N5 Ni1 N2 179.6(4) 8_646 . ? N6 Ni1 N2 94.3(4) 8_646 . ? N3 Ni1 N2 84.7(4) . . ? O2 Ni1 N2 84.3(3) . . ? C7 O2 Ni1 118.5(7) . . ? C12 O3 Ni1 120.8(7) . 7_566 ? N2MA O5MA O4S 151(2) . 7_466 ? O8M O7M N3M 67.8(10) 4_646 . ? N3M O7M O8M 53.1(12) . 3_666 ? O1M N1MA O2MA 119.98(7) . . ? O1M N1MA O3M 120.00(7) . . ? O2MA N1MA O3M 120.01(7) . . ? O3M N1MB O2MB 119.99(7) . . ? O3M N1MB O1M 120.00(7) . . ? O2MB N1MB O1M 120.00(7) . . ? O4MA N2MA O6MA 119.95(12) . . ? O4MA N2MA O5MA 119.95(11) . . ? O6MA N2MA O5MA 119.95(12) . . ? O6MB N2MB O4MB 119.93(12) . . ? O6MB N2MB O5MB 119.92(12) . . ? O4MB N2MB O5MB 119.93(11) . . ? O8M O8M O7M 143.1(13) 2_755 3_666 ? O8M O8M N3M 75(2) 2_755 . ? O7M O8M N3M 67.8(10) 3_666 . ? O7M O8M O7M 120.9(8) 3_666 4_646 ? N3M O8M O7M 53.1(12) . 4_646 ? O5MA O4S O5MA 95(4) 8_656 7_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.728 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.102 #===END data_i-4_293K_in_capillary_after_333K _database_code_depnum_ccdc_archive 'CCDC 856072' #TrackingRef '- Revised-CC-COM-04-2012-032857-CCDC856057-856072.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H130 N36 Ni4 O47' _chemical_formula_weight 2198.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I-4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.535(6) _cell_length_b 15.535(6) _cell_length_c 19.504(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4707(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1202 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 16.82 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8846 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; Sample was set to 293K after measuring at 333K. Measurement was done by using a glass capillary to prevent from drying. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 12455 _diffrn_reflns_av_R_equivalents 0.1400 _diffrn_reflns_av_sigmaI/netI 0.1778 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.13 _reflns_number_total 4239 _reflns_number_gt 2252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. SADI restraint is applied to keep same N-O and O-O distance for all nitrate. FLAT restraints are used for disordered nitrate [(N1MA, O1M, O2MA, and O3M) and (N1MB, O1M, O2MB, and O3M)]. SIMU and ISOR restraints are applied for all atoms of nitrate and included water molecules. ; _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^)+(0.1005P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 4239 _refine_ls_number_parameters 345 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.1608 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 1.008 _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 0.7103(11) 1.0895(11) 0.8091(10) 0.112(7) Uani 1 1 d . . . H1A H 0.6821 1.0700 0.7681 0.168 Uiso 1 1 calc R . . H1B H 0.7385 1.1433 0.8002 0.168 Uiso 1 1 calc R . . H1C H 0.6684 1.0970 0.8448 0.168 Uiso 1 1 calc R . . C2 C 0.7755(11) 1.0241(8) 0.8311(8) 0.069(4) Uani 1 1 d . . . C3 C 0.8063(8) 0.9091(8) 0.9140(6) 0.053(3) Uani 1 1 d . . . H3A H 0.8045 0.9185 0.9632 0.063 Uiso 1 1 calc R . . H3B H 0.8647 0.9204 0.8989 0.063 Uiso 1 1 calc R . . C4 C 0.7851(8) 0.8127(8) 0.8996(6) 0.046(3) Uani 1 1 d . . . C5 C 0.8517(9) 0.7590(8) 0.9377(7) 0.060(4) Uani 1 1 d . . . H5A H 0.9087 0.7810 0.9276 0.072 Uiso 1 1 calc R . . H5B H 0.8422 0.7645 0.9866 0.072 Uiso 1 1 calc R . . C6 C 0.6908(8) 0.7982(8) 0.9253(6) 0.050(3) Uani 1 1 d . . . H6A H 0.6820 0.8300 0.9675 0.060 Uiso 1 1 calc R . . H6B H 0.6509 0.8203 0.8913 0.060 Uiso 1 1 calc R . . C7 C 0.7911(7) 0.7912(8) 0.8245(6) 0.037(3) Uani 1 1 d . . . C8 C 0.8447(6) 0.8245(7) 0.7090(5) 0.036(2) Uani 1 1 d . . . H8A H 0.8246 0.8751 0.6846 0.043 Uiso 1 1 calc R . . H8B H 0.8072 0.7770 0.6966 0.043 Uiso 1 1 calc R . . C9 C 0.9366(6) 0.8034(7) 0.6846(5) 0.033(2) Uani 1 1 d . . . C10 C 0.9970(6) 0.8756(7) 0.7115(6) 0.038(3) Uani 1 1 d . . . H10A H 0.9683 0.9306 0.7061 0.045 Uiso 1 1 calc R . . H10B H 1.0067 0.8667 0.7601 0.045 Uiso 1 1 calc R . . C11 C 0.9313(6) 0.8053(7) 0.6059(5) 0.039(3) Uani 1 1 d . . . H11A H 0.8828 0.7703 0.5917 0.047 Uiso 1 1 calc R . . H11B H 0.9196 0.8640 0.5915 0.047 Uiso 1 1 calc R . . C12 C 0.9702(7) 0.7191(7) 0.7076(5) 0.038(3) Uani 1 1 d . . . N1 N 0.7492(7) 0.9708(6) 0.8812(6) 0.068(3) Uani 1 1 d . . . H1 H 0.6965 0.9734 0.8944 0.082 Uiso 1 1 calc R . . N2 N 0.8476(6) 0.6670(6) 0.9184(5) 0.043(2) Uani 1 1 d . . . H2A H 0.8563 0.6356 0.9566 0.052 Uiso 1 1 calc R . . H2B H 0.8917 0.6560 0.8898 0.052 Uiso 1 1 calc R . . N3 N 0.6725(6) 0.7067(6) 0.9374(5) 0.043(2) Uani 1 1 d . . . H3C H 0.6153 0.6985 0.9342 0.051 Uiso 1 1 calc R . . H3D H 0.6882 0.6936 0.9806 0.051 Uiso 1 1 calc R . . N4 N 0.8362(5) 0.8402(5) 0.7829(4) 0.039(2) Uani 1 1 d . . . H4 H 0.8623 0.8841 0.8000 0.047 Uiso 1 1 calc R . . N5 N 1.0819(5) 0.8793(5) 0.6760(5) 0.040(2) Uani 1 1 d . . . H5C H 1.1221 0.8947 0.7068 0.048 Uiso 1 1 calc R . . H5D H 1.0795 0.9210 0.6441 0.048 Uiso 1 1 calc R . . N6 N 1.0098(5) 0.7744(6) 0.5689(5) 0.044(2) Uani 1 1 d . . . H6D H 1.0200 0.8100 0.5333 0.052 Uiso 1 1 calc R . . H6C H 0.9988 0.7219 0.5515 0.052 Uiso 1 1 calc R . . N7 N 0.9189(6) 0.6632(6) 0.7404(5) 0.048(2) Uani 1 1 d . . . H7A H 0.9386 0.6139 0.7529 0.057 Uiso 1 1 calc R . . H7B H 0.8662 0.6766 0.7490 0.057 Uiso 1 1 calc R . . O4M O 0.0968(12) 0.5964(11) 0.9194(10) 0.144(7) Uani 0.75 1 d PDU . . Ni1 Ni 0.73302(8) 0.62203(8) 0.87120(6) 0.0346(3) Uani 1 1 d . . . O1 O 0.8483(7) 1.0195(6) 0.8055(5) 0.074(3) Uani 1 1 d . . . O2 O 0.7553(5) 0.7236(5) 0.8026(3) 0.0383(18) Uani 1 1 d . . . O3 O 1.0471(4) 0.6986(5) 0.6955(4) 0.0408(18) Uani 1 1 d . . . O5M O 0.1521(12) 0.7268(10) 0.9068(10) 0.146(7) Uani 0.75 1 d PDU . . O6M O 0.0267(15) 0.7020(16) 0.8753(17) 0.249(13) Uani 0.75 1 d PDU . . O7M O 0.5198(12) 0.5671(9) -0.0316(8) 0.067(5) Uani 0.50 1 d PDU A -1 O2S O 0.0403(11) 0.8868(12) 0.8967(8) 0.167(6) Uani 1 1 d . . . O3S O 0.5967(12) 1.0009(12) 0.9561(10) 0.205(9) Uani 1 1 d . . . O1M O 0.4875(8) 0.7162(9) 0.9001(7) 0.145(5) Uani 1 1 d DU . . O3M O 0.3769(8) 0.7780(7) 0.9354(6) 0.113(4) Uani 1 1 d DU . . N1MA N 0.4499(10) 0.7845(10) 0.9104(13) 0.078(7) Uani 0.60(3) 1 d PDU B 1 O2MA O 0.4762(14) 0.8452(13) 0.8756(17) 0.165(12) Uani 0.60(3) 1 d PDU B 1 N1MB N 0.4524(12) 0.7855(14) 0.915(2) 0.115(14) Uani 0.40(3) 1 d PDU B 2 O2MB O 0.4926(13) 0.8445(13) 0.9444(16) 0.107(13) Uani 0.40(3) 1 d PDU B 2 N2M N 0.0905(15) 0.6747(13) 0.9056(16) 0.192(13) Uani 0.75 1 d PDU . . O8M O 0.478(2) 0.507(2) 0.0607(9) 0.067(9) Uani 0.25 1 d PDU A -1 O4S O 0.0000 0.5000 0.8365(14) 0.195(10) Uani 1 2 d SU . . O1S O 0.0000 0.0000 0.0000 0.134(10) Uani 1 4 d S . . N3M N 0.5000 0.5000 0.0000 0.055(5) Uani 1 4 d SDU . . 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 0.104(13) 0.093(13) 0.139(17) 0.031(12) 0.060(13) 0.026(12) C2 0.100(12) 0.036(8) 0.070(10) -0.014(7) 0.012(9) 0.006(8) C3 0.066(9) 0.044(8) 0.048(7) -0.006(6) 0.018(6) -0.022(6) C4 0.047(7) 0.044(7) 0.048(7) -0.005(6) 0.008(6) -0.008(6) C5 0.067(9) 0.068(9) 0.045(8) 0.003(7) -0.014(7) -0.007(7) C6 0.071(9) 0.042(7) 0.036(7) -0.005(5) 0.018(6) -0.008(6) C7 0.026(6) 0.047(7) 0.039(7) 0.001(6) 0.005(5) 0.008(6) C8 0.035(6) 0.042(6) 0.031(6) 0.001(5) -0.001(5) -0.003(5) C9 0.028(6) 0.037(6) 0.035(6) -0.002(5) 0.001(5) 0.002(5) C10 0.031(6) 0.043(6) 0.039(6) 0.005(5) 0.003(5) -0.002(5) C11 0.027(6) 0.055(7) 0.037(6) 0.001(5) 0.000(5) 0.006(5) C12 0.031(6) 0.039(6) 0.044(7) -0.002(5) -0.001(5) -0.006(5) N1 0.090(8) 0.039(6) 0.075(8) -0.006(6) 0.040(7) -0.004(6) N2 0.051(6) 0.036(5) 0.043(6) 0.000(4) 0.003(5) -0.003(5) N3 0.044(6) 0.043(6) 0.041(6) -0.008(5) -0.001(5) -0.008(5) N4 0.037(5) 0.040(5) 0.041(6) 0.002(4) 0.007(4) -0.005(4) N5 0.036(5) 0.038(5) 0.045(6) 0.006(4) 0.007(4) -0.010(4) N6 0.041(6) 0.050(6) 0.040(6) 0.003(4) -0.002(5) -0.002(5) N7 0.037(5) 0.047(6) 0.060(7) 0.012(5) 0.011(5) -0.002(5) O4M 0.151(10) 0.150(11) 0.130(10) -0.029(9) 0.001(8) 0.005(9) Ni1 0.0358(8) 0.0325(8) 0.0356(6) -0.0023(7) 0.0048(7) -0.0018(7) O1 0.083(7) 0.050(6) 0.088(7) -0.004(5) 0.034(6) -0.006(5) O2 0.041(4) 0.044(5) 0.030(4) -0.003(3) 0.005(3) -0.001(4) O3 0.032(4) 0.041(4) 0.049(5) 0.009(4) 0.003(4) -0.001(4) O5M 0.146(10) 0.136(11) 0.155(11) -0.021(9) 0.015(9) 0.011(8) O6M 0.237(16) 0.264(16) 0.246(15) -0.006(10) -0.008(10) 0.005(10) O7M 0.080(8) 0.065(8) 0.055(8) 0.003(7) 0.009(7) -0.010(7) O2S 0.170(14) 0.216(17) 0.115(12) 0.002(11) 0.013(10) -0.034(13) O3S 0.191(16) 0.158(14) 0.27(2) 0.019(15) 0.126(16) 0.047(13) O1M 0.117(8) 0.150(9) 0.169(9) -0.060(7) -0.027(7) 0.004(7) O3M 0.116(8) 0.141(8) 0.081(6) -0.003(6) 0.005(6) 0.016(7) N1MA 0.075(10) 0.080(10) 0.080(10) 0.007(8) -0.053(8) 0.005(8) O2MA 0.154(14) 0.174(14) 0.168(15) 0.021(10) 0.007(10) -0.008(9) N1MB 0.111(16) 0.117(16) 0.116(16) 0.003(10) -0.023(10) 0.002(10) O2MB 0.119(15) 0.094(15) 0.108(16) -0.008(9) -0.015(9) -0.017(9) N2M 0.185(16) 0.204(16) 0.189(16) -0.006(10) -0.011(10) 0.006(10) O8M 0.068(13) 0.074(12) 0.061(11) -0.007(9) 0.008(9) 0.003(9) O4S 0.174(13) 0.199(13) 0.212(14) 0.000 0.000 0.012(10) O1S 0.156(15) 0.156(15) 0.090(18) 0.000 0.000 0.000 N3M 0.059(6) 0.059(6) 0.049(8) 0.000 0.000 0.000 _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 C2 1.50(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.239(16) . ? C2 N1 1.345(18) . ? C3 N1 1.455(15) . ? C3 C4 1.559(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C7 1.506(15) . ? C4 C5 1.521(17) . ? C4 C6 1.565(16) . ? C5 N2 1.480(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.469(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O2 1.262(13) . ? C7 N4 1.315(13) . ? C8 N4 1.468(12) . ? C8 C9 1.541(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.480(15) . ? C9 C11 1.538(14) . ? C9 C10 1.553(14) . ? C10 N5 1.490(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.497(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O3 1.260(12) . ? C12 N7 1.341(13) . ? N1 H1 0.8600 . ? N2 Ni1 2.122(9) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 Ni1 2.069(9) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4 0.8600 . ? N5 Ni1 2.069(9) 7_566 ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 Ni1 2.102(9) 7_566 ? N6 H6D 0.9000 . ? N6 H6C 0.9000 . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? O4M N2M 1.250(14) . ? Ni1 O3 2.043(7) 8_646 ? Ni1 N5 2.069(9) 8_646 ? Ni1 O2 2.098(7) . ? Ni1 N6 2.102(9) 8_646 ? O3 Ni1 2.043(7) 7_566 ? O5M N2M 1.254(14) . ? O6M N2M 1.229(15) . ? O7M N3M 1.249(12) . ? O1M N1MA 1.228(14) . ? O1M N1MB 1.243(16) . ? O3M N1MA 1.238(13) . ? O3M N1MB 1.242(16) . ? N1MA O2MA 1.232(14) . ? N1MB O2MB 1.245(17) . ? O8M N3M 1.237(15) . ? N3M O8M 1.237(15) 4_655 ? N3M O8M 1.237(15) 2_665 ? N3M O8M 1.237(15) 3_565 ? N3M O7M 1.249(12) 2_665 ? N3M O7M 1.249(12) 3_565 ? N3M O7M 1.249(12) 4_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.3(13) . . ? O1 C2 C1 122.8(14) . . ? N1 C2 C1 114.9(14) . . ? N1 C3 C4 115.2(11) . . ? N1 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N1 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C7 C4 C5 108.1(10) . . ? C7 C4 C3 112.1(10) . . ? C5 C4 C3 107.2(10) . . ? C7 C4 C6 109.7(10) . . ? C5 C4 C6 113.7(10) . . ? C3 C4 C6 106.2(9) . . ? N2 C5 C4 112.1(9) . . ? N2 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N3 C6 C4 111.9(10) . . ? N3 C6 H6A 109.2 . . ? C4 C6 H6A 109.2 . . ? N3 C6 H6B 109.2 . . ? C4 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O2 C7 N4 120.5(10) . . ? O2 C7 C4 119.1(10) . . ? N4 C7 C4 120.3(11) . . ? N4 C8 C9 114.9(8) . . ? N4 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? N4 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C12 C9 C11 109.8(9) . . ? C12 C9 C8 114.8(9) . . ? C11 C9 C8 104.7(8) . . ? C12 C9 C10 108.9(8) . . ? C11 C9 C10 110.9(8) . . ? C8 C9 C10 107.6(8) . . ? N5 C10 C9 113.9(8) . . ? N5 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? N5 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N6 C11 C9 115.6(8) . . ? N6 C11 H11A 108.4 . . ? C9 C11 H11A 108.4 . . ? N6 C11 H11B 108.4 . . ? C9 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? O3 C12 N7 119.3(10) . . ? O3 C12 C9 120.0(9) . . ? N7 C12 C9 120.6(10) . . ? C2 N1 C3 122.7(11) . . ? C2 N1 H1 118.6 . . ? C3 N1 H1 118.6 . . ? C5 N2 Ni1 117.6(7) . . ? C5 N2 H2A 107.9 . . ? Ni1 N2 H2A 107.9 . . ? C5 N2 H2B 107.9 . . ? Ni1 N2 H2B 107.9 . . ? H2A N2 H2B 107.2 . . ? C6 N3 Ni1 115.2(7) . . ? C6 N3 H3C 108.5 . . ? Ni1 N3 H3C 108.5 . . ? C6 N3 H3D 108.5 . . ? Ni1 N3 H3D 108.5 . . ? H3C N3 H3D 107.5 . . ? C7 N4 C8 123.8(9) . . ? C7 N4 H4 118.1 . . ? C8 N4 H4 118.1 . . ? C10 N5 Ni1 116.2(6) . 7_566 ? C10 N5 H5C 108.2 . . ? Ni1 N5 H5C 108.2 7_566 . ? C10 N5 H5D 108.2 . . ? Ni1 N5 H5D 108.2 7_566 . ? H5C N5 H5D 107.4 . . ? C11 N6 Ni1 115.2(6) . 7_566 ? C11 N6 H6D 108.5 . . ? Ni1 N6 H6D 108.5 7_566 . ? C11 N6 H6C 108.5 . . ? Ni1 N6 H6C 108.5 7_566 . ? H6D N6 H6C 107.5 . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? O3 Ni1 N5 89.0(3) 8_646 8_646 ? O3 Ni1 N3 174.6(3) 8_646 . ? N5 Ni1 N3 94.9(3) 8_646 . ? O3 Ni1 O2 86.4(3) 8_646 . ? N5 Ni1 O2 94.7(3) 8_646 . ? N3 Ni1 O2 89.7(3) . . ? O3 Ni1 N6 84.9(3) 8_646 8_646 ? N5 Ni1 N6 87.2(4) 8_646 8_646 ? N3 Ni1 N6 98.9(4) . 8_646 ? O2 Ni1 N6 171.0(3) . 8_646 ? O3 Ni1 N2 91.6(3) 8_646 . ? N5 Ni1 N2 178.3(4) 8_646 . ? N3 Ni1 N2 84.3(4) . . ? O2 Ni1 N2 83.7(3) . . ? N6 Ni1 N2 94.4(3) 8_646 . ? C7 O2 Ni1 118.8(6) . . ? C12 O3 Ni1 121.9(7) . 7_566 ? O1M N1MA O2MA 114.4(15) . . ? O1M N1MA O3M 115.5(13) . . ? O2MA N1MA O3M 125.6(14) . . ? O3M N1MB O1M 114.1(17) . . ? O3M N1MB O2MB 113.5(19) . . ? O1M N1MB O2MB 122(2) . . ? O6M N2M O4M 120.2(16) . . ? O6M N2M O5M 113.6(15) . . ? O4M N2M O5M 124.4(16) . . ? O8M N3M O8M 156(2) 4_655 2_665 ? O8M N3M O8M 156(2) 2_665 3_565 ? O8M N3M O8M 156(2) 4_655 . ? O8M N3M O8M 156(2) 3_565 . ? O8M N3M O7M 77(2) 4_655 . ? O8M N3M O7M 119(2) 2_665 . ? O8M N3M O7M 117.7(17) . . ? O8M N3M O7M 117.7(17) 2_665 2_665 ? O8M N3M O7M 77(2) 3_565 2_665 ? O8M N3M O7M 119(2) . 2_665 ? O7M N3M O7M 120.8(17) . 2_665 ? O8M N3M O7M 119(2) 4_655 3_565 ? O8M N3M O7M 117.7(17) 3_565 3_565 ? O8M N3M O7M 77(2) . 3_565 ? O7M N3M O7M 104.1(7) . 3_565 ? O7M N3M O7M 104.1(7) 2_665 3_565 ? O8M N3M O7M 117.7(17) 4_655 4_655 ? O8M N3M O7M 77(2) 2_665 4_655 ? O8M N3M O7M 119(2) 3_565 4_655 ? O7M N3M O7M 104.1(7) . 4_655 ? O7M N3M O7M 104.1(7) 2_665 4_655 ? O7M N3M O7M 120.8(17) 3_565 4_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.821 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.099