# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- CIF.cif' _publ_contact_author_name 'Vassilios Nastopoulos' _publ_contact_author_address ; Department of Chemistry, University of Patras, GR-265 04 Patras, Greece ; _publ_contact_author_email nastopoulos@chemistry.upatras.gr _publ_contact_author_fax '0030 2610 997118' _publ_contact_author_phone '0030 2610 962953' loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Vassilios Nastopoulos' . ; Department of Chemistry, University of Patras, GR-265 04 Patras, Greece ; 'Konstantina Kounavi' . ; Department of Chemistry, University of Cyprus, 1678 Nicosia, Cyprus ; 'Eleni Moushi' . ; Department of Chemistry, University of Cyprus, 1678 Nicosia, Cyprus ; 'Emmanouil Manos' . ; Department of Chemistry, University of Patras, GR-265 04 Patras, Greece ; ; C.Papatriantafyllopoulou ; . ; Department of Chemistry, University of Cyprus, 1678 Nicosia, Cyprus ; 'Anastasios Tasiopoulos' . ; Department of Chemistry, University of Patras, GR-265 04 Patras, Greece ; _publ_section_title ; Supramolecular patterns of cationic and neutral Ni(II) complexes from the interplay of hydrogen-bonding, stacking interactions and metal-coordination motifs ; data_1-NiL4_{OH}2_H2O #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881062' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 N8 Ni 2+, H2 O, 2(H O 1-)' _chemical_formula_sum 'C64 H60 N8 Ni O3' _chemical_formula_weight 1047.91 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 Orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 11.4027(3) _cell_length_b 23.4885(6) _cell_length_c 22.6238(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6059.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9713 _cell_measurement_theta_min 3.0623 _cell_measurement_theta_max 30.2985 _exptl_crystal_description prism _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85857 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25119 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.49 _reflns_number_total 5996 _reflns_number_gt 4538 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2073 Friedel pairs' _refine_ls_abs_structure_Flack 0.000(17) _refine_ls_number_reflns 5996 _refine_ls_number_parameters 353 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 1.005 _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 N1A N 0.5037(2) -0.10481(10) 0.26484(12) 0.0257(5) Uani 1 1 d . . . C2A C 0.5439(3) -0.06467(13) 0.30069(14) 0.0241(6) Uani 1 1 d . . . H2A H 0.6157 -0.0464 0.2960 0.029 Uiso 1 1 calc R . . N3A N 0.4690(2) -0.05375(11) 0.34403(12) 0.0197(5) Uani 1 1 d . . . C2B C 0.6084(3) 0.04888(14) 0.50503(15) 0.0273(7) Uani 1 1 d . . . H2B H 0.6437 0.0143 0.5143 0.033 Uiso 1 1 calc R . . C4A C 0.3731(3) -0.08931(12) 0.33508(14) 0.0241(6) Uani 1 1 d . . . C4B C 0.4969(2) 0.11317(12) 0.46454(14) 0.0223(6) Uani 1 1 d . . . C5A C 0.3937(3) -0.12109(13) 0.28546(14) 0.0254(7) Uani 1 1 d . . . C5B C 0.5627(3) 0.13969(13) 0.50626(14) 0.0248(6) Uani 1 1 d . . . C6A C 0.5649(4) -0.12299(16) 0.21125(18) 0.0425(9) Uani 1 1 d . . . H6A1 H 0.6301 -0.0981 0.2040 0.064 Uiso 1 1 calc R . . H6A2 H 0.5119 -0.1216 0.1783 0.064 Uiso 1 1 calc R . . H6A3 H 0.5929 -0.1612 0.2163 0.064 Uiso 1 1 calc R . . C6B C 0.7187(4) 0.10508(16) 0.57911(18) 0.0447(10) Uani 1 1 d . . . H6B1 H 0.7672 0.1377 0.5714 0.067 Uiso 1 1 calc R . . H6B2 H 0.7669 0.0716 0.5815 0.067 Uiso 1 1 calc R . . H6B3 H 0.6780 0.1103 0.6158 0.067 Uiso 1 1 calc R . . C7A C 0.2714(2) -0.08956(13) 0.37421(14) 0.0237(6) Uani 1 1 d . . . C7B C 0.4058(3) 0.13759(12) 0.42573(14) 0.0242(6) Uani 1 1 d . . . C8A C 0.2252(3) -0.03911(13) 0.39561(15) 0.0288(7) Uani 1 1 d . . . H8A H 0.2581 -0.0048 0.3836 0.035 Uiso 1 1 calc R . . C8B C 0.2964(3) 0.11209(13) 0.42215(15) 0.0279(7) Uani 1 1 d . . . H8B H 0.2797 0.0806 0.4455 0.034 Uiso 1 1 calc R . . C9A C 0.1311(3) -0.03846(15) 0.43443(18) 0.0358(8) Uani 1 1 d . . . H9A H 0.1033 -0.0041 0.4494 0.043 Uiso 1 1 calc R . . C9B C 0.2111(3) 0.13328(16) 0.38379(16) 0.0362(8) Uani 1 1 d . . . H9B H 0.1381 0.1158 0.3815 0.043 Uiso 1 1 calc R . . C10A C 0.0784(3) -0.08974(16) 0.45082(16) 0.0356(8) Uani 1 1 d . . . H10A H 0.0150 -0.0897 0.4766 0.043 Uiso 1 1 calc R . . C10B C 0.2353(3) 0.17978(17) 0.34955(17) 0.0400(9) Uani 1 1 d . . . H10B H 0.1789 0.1933 0.3234 0.048 Uiso 1 1 calc R . . C11A C 0.1208(3) -0.14038(14) 0.42858(17) 0.0316(7) Uani 1 1 d . . . H11A H 0.0842 -0.1744 0.4386 0.038 Uiso 1 1 calc R . . C11B C 0.3437(3) 0.20712(14) 0.35335(16) 0.0352(8) Uani 1 1 d . . . H11B H 0.3593 0.2392 0.3305 0.042 Uiso 1 1 calc R . . C12A C 0.2176(3) -0.14111(13) 0.39130(14) 0.0268(7) Uani 1 1 d . . . H12A H 0.2469 -0.1756 0.3776 0.032 Uiso 1 1 calc R . . C12B C 0.4287(3) 0.18553(13) 0.39213(14) 0.0294(7) Uani 1 1 d . . . H12B H 0.5010 0.2036 0.3953 0.035 Uiso 1 1 calc R . . C13A C 0.3188(3) -0.16199(15) 0.25356(15) 0.0353(8) Uani 1 1 d . . . C13B C 0.5602(3) 0.19952(13) 0.52682(14) 0.0253(6) Uani 1 1 d . . . C14A C 0.2050(4) -0.1451(2) 0.23928(17) 0.0491(11) Uani 1 1 d . . . H14A H 0.1756 -0.1102 0.2518 0.059 Uiso 1 1 calc R . . C14B C 0.4648(3) 0.21955(14) 0.55813(16) 0.0298(7) Uani 1 1 d . . . H14B H 0.4046 0.1947 0.5684 0.036 Uiso 1 1 calc R . . C15A C 0.1365(5) -0.1823(3) 0.2057(2) 0.0687(16) Uani 1 1 d . . . H15A H 0.0608 -0.1713 0.1956 0.082 Uiso 1 1 calc R . . C15B C 0.4578(3) 0.27626(14) 0.57442(17) 0.0344(8) Uani 1 1 d . . . H15B H 0.3928 0.2893 0.5953 0.041 Uiso 1 1 calc R . . C16A C 0.1740(5) -0.2315(3) 0.18788(19) 0.0691(17) Uani 1 1 d . . . H16A H 0.1258 -0.2543 0.1647 0.083 Uiso 1 1 calc R . . C16B C 0.5471(3) 0.31374(14) 0.55986(15) 0.0288(7) Uani 1 1 d . . . H16B H 0.5421 0.3518 0.5708 0.035 Uiso 1 1 calc R . . C17A C 0.2848(5) -0.2506(2) 0.2030(2) 0.0618(14) Uani 1 1 d . . . H17A H 0.3105 -0.2864 0.1911 0.074 Uiso 1 1 calc R . . C17B C 0.6437(3) 0.29422(14) 0.52903(16) 0.0358(8) Uani 1 1 d . . . H17B H 0.7041 0.3192 0.5193 0.043 Uiso 1 1 calc R . . C18A C 0.3577(4) -0.21509(16) 0.23647(17) 0.0464(10) Uani 1 1 d . . . H18A H 0.4323 -0.2273 0.2472 0.056 Uiso 1 1 calc R . . C18B C 0.6506(3) 0.23729(14) 0.51259(16) 0.0336(8) Uani 1 1 d . . . H18B H 0.7159 0.2242 0.4920 0.040 Uiso 1 1 calc R . . N1B N 0.6332(2) 0.09833(11) 0.53106(13) 0.0294(6) Uani 1 1 d . . . N3B N 0.5259(2) 0.05577(11) 0.46376(13) 0.0231(6) Uani 1 1 d . . . Ni Ni 0.5000 0.0000 0.40457(3) 0.01957(12) Uani 1 2 d S . . O1 O 0.7817(4) -0.05601(14) 0.55613(17) 0.0738(11) Uani 1 1 d DU . . H1 H 0.848(3) -0.042(3) 0.565(3) 0.111 Uiso 1 1 d D . . O2 O 1.0000 0.0000 0.6141(3) 0.0611(12) Uani 1 2 d SDU . . H2 H 0.973(5) 0.0253(13) 0.6368(8) 0.092 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1A 0.0330(13) 0.0244(12) 0.0195(12) -0.0008(10) 0.0017(11) -0.0025(11) C2A 0.0253(15) 0.0218(15) 0.0253(16) 0.0016(12) -0.0008(13) -0.0028(12) N3A 0.0172(12) 0.0215(14) 0.0203(13) 0.0009(11) -0.0022(11) -0.0013(11) C2B 0.0330(17) 0.0249(16) 0.0240(16) -0.0032(12) -0.0034(13) 0.0046(14) C4A 0.0219(15) 0.0226(15) 0.0276(16) 0.0025(12) -0.0028(13) -0.0038(12) C4B 0.0231(14) 0.0222(14) 0.0216(14) 0.0001(11) 0.0028(13) 0.0023(12) C5A 0.0307(17) 0.0237(16) 0.0217(15) -0.0019(12) -0.0035(13) -0.0079(13) C5B 0.0241(16) 0.0265(16) 0.0238(15) -0.0039(12) 0.0044(13) -0.0004(13) C6A 0.052(2) 0.039(2) 0.036(2) -0.0117(16) 0.0118(18) -0.0114(18) C6B 0.056(2) 0.037(2) 0.041(2) -0.0126(17) -0.0215(19) 0.0069(18) C7A 0.0192(14) 0.0271(16) 0.0246(15) 0.0016(13) -0.0017(12) -0.0029(12) C7B 0.0250(15) 0.0258(15) 0.0218(14) -0.0035(12) 0.0025(12) 0.0045(12) C8A 0.0228(14) 0.0260(14) 0.038(2) 0.0042(14) -0.0017(14) -0.0025(11) C8B 0.0236(15) 0.0287(16) 0.0315(18) 0.0000(13) 0.0031(12) 0.0035(12) C9A 0.0247(17) 0.0354(18) 0.047(2) -0.0022(17) -0.0001(16) 0.0008(14) C9B 0.0263(17) 0.045(2) 0.0371(19) 0.0005(15) 0.0013(15) 0.0043(15) C10A 0.0229(15) 0.049(2) 0.0344(18) 0.0062(16) 0.0013(14) 0.0001(15) C10B 0.0325(18) 0.052(2) 0.0354(19) 0.0029(17) -0.0051(16) 0.0177(17) C11A 0.0267(16) 0.0346(18) 0.0334(17) 0.0085(15) -0.0038(14) -0.0083(14) C11B 0.045(2) 0.0274(17) 0.0330(18) 0.0014(14) 0.0047(16) 0.0097(15) C12A 0.0247(15) 0.0264(15) 0.0294(18) 0.0071(12) -0.0071(12) -0.0051(12) C12B 0.0326(16) 0.0264(15) 0.0290(18) -0.0023(12) 0.0022(13) 0.0000(13) C13A 0.045(2) 0.0373(19) 0.0231(16) 0.0027(14) 0.0017(16) -0.0226(16) C13B 0.0258(16) 0.0254(15) 0.0247(16) -0.0041(13) -0.0016(13) -0.0001(13) C14A 0.049(2) 0.062(3) 0.036(2) 0.0155(19) -0.0146(18) -0.025(2) C14B 0.0247(15) 0.0312(17) 0.0334(18) -0.0017(14) 0.0003(14) 0.0000(13) C15A 0.080(3) 0.085(4) 0.040(2) 0.016(3) -0.022(2) -0.054(3) C15B 0.0342(17) 0.0316(17) 0.037(2) -0.0012(15) 0.0048(16) 0.0092(15) C16A 0.097(4) 0.081(4) 0.029(2) 0.003(2) -0.006(3) -0.065(3) C16B 0.0382(18) 0.0218(15) 0.0262(16) -0.0022(12) -0.0062(15) 0.0028(14) C17A 0.105(4) 0.045(2) 0.035(2) -0.0084(19) 0.020(3) -0.032(3) C17B 0.0370(18) 0.0296(17) 0.041(2) 0.0001(16) 0.0029(16) -0.0067(15) C18A 0.072(3) 0.035(2) 0.033(2) -0.0065(15) 0.0128(19) -0.0265(19) C18B 0.0341(18) 0.0301(18) 0.0366(19) -0.0018(14) 0.0079(15) -0.0005(14) N1B 0.0320(15) 0.0271(14) 0.0290(15) -0.0047(12) -0.0045(12) 0.0060(12) N3B 0.0272(14) 0.0191(14) 0.0230(15) -0.0013(11) 0.0017(12) -0.0001(11) Ni 0.0201(2) 0.0189(2) 0.0197(2) 0.000 0.000 -0.0014(2) O1 0.109(3) 0.0497(19) 0.062(2) -0.0209(15) -0.028(2) 0.0411(19) O2 0.0268(18) 0.070(3) 0.087(3) 0.000 0.000 -0.0162(18) _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 N1A C2A 1.325(4) . ? N1A C5A 1.392(4) . ? N1A C6A 1.463(4) . ? C2A N3A 1.326(4) . ? C2A H2A 0.9300 . ? N3A C4A 1.391(4) . ? N3A Ni 1.896(3) . ? C2B N1B 1.333(4) . ? C2B N3B 1.336(4) . ? C2B H2B 0.9300 . ? C4A C5A 1.368(4) . ? C4A C7A 1.459(4) . ? C4B C5B 1.357(4) . ? C4B N3B 1.388(4) . ? C4B C7B 1.476(4) . ? C5A C13A 1.474(4) . ? C5B N1B 1.380(4) . ? C5B C13B 1.480(4) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C6B N1B 1.469(4) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7A C8A 1.385(4) . ? C7A C12A 1.412(4) . ? C7B C12B 1.384(4) . ? C7B C8B 1.385(4) . ? C8A C9A 1.387(5) . ? C8A H8A 0.9300 . ? C8B C9B 1.396(5) . ? C8B H8B 0.9300 . ? C9A C10A 1.396(5) . ? C9A H9A 0.9300 . ? C9B C10B 1.367(5) . ? C9B H9B 0.9300 . ? C10A C11A 1.379(5) . ? C10A H10A 0.9300 . ? C10B C11B 1.396(5) . ? C10B H10B 0.9300 . ? C11A C12A 1.389(5) . ? C11A H11A 0.9300 . ? C11B C12B 1.402(5) . ? C11B H11B 0.9300 . ? C12A H12A 0.9300 . ? C12B H12B 0.9300 . ? C13A C18A 1.379(5) . ? C13A C14A 1.395(5) . ? C13B C14B 1.381(5) . ? C13B C18B 1.398(5) . ? C14A C15A 1.396(6) . ? C14A H14A 0.9300 . ? C14B C15B 1.384(5) . ? C14B H14B 0.9300 . ? C15A C16A 1.297(8) . ? C15A H15A 0.9300 . ? C15B C16B 1.386(5) . ? C15B H15B 0.9300 . ? C16A C17A 1.383(8) . ? C16A H16A 0.9300 . ? C16B C17B 1.382(5) . ? C16B H16B 0.9300 . ? C17A C18A 1.400(6) . ? C17A H17A 0.9300 . ? C17B C18B 1.390(5) . ? C17B H17B 0.9300 . ? C18A H18A 0.9300 . ? C18B H18B 0.9300 . ? N3B Ni 1.896(3) . ? Ni N3A 1.896(3) 2_655 ? Ni N3B 1.897(3) 2_655 ? O1 H1 0.850(15) . ? O2 H2 0.847(10) . ? 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 C2A N1A C5A 107.6(3) . . ? C2A N1A C6A 123.4(3) . . ? C5A N1A C6A 128.9(3) . . ? N1A C2A N3A 111.6(3) . . ? N1A C2A H2A 124.2 . . ? N3A C2A H2A 124.2 . . ? C2A N3A C4A 106.4(3) . . ? C2A N3A Ni 122.9(2) . . ? C4A N3A Ni 130.7(2) . . ? N1B C2B N3B 110.6(3) . . ? N1B C2B H2B 124.7 . . ? N3B C2B H2B 124.7 . . ? C5A C4A N3A 108.2(3) . . ? C5A C4A C7A 129.2(3) . . ? N3A C4A C7A 122.6(3) . . ? C5B C4B N3B 108.8(3) . . ? C5B C4B C7B 128.6(3) . . ? N3B C4B C7B 122.5(3) . . ? C4A C5A N1A 106.3(3) . . ? C4A C5A C13A 131.1(3) . . ? N1A C5A C13A 122.5(3) . . ? C4B C5B N1B 106.4(3) . . ? C4B C5B C13B 130.1(3) . . ? N1B C5B C13B 123.5(3) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C8A C7A C12A 118.2(3) . . ? C8A C7A C4A 120.8(3) . . ? C12A C7A C4A 121.0(3) . . ? C12B C7B C8B 119.3(3) . . ? C12B C7B C4B 120.7(3) . . ? C8B C7B C4B 120.0(3) . . ? C7A C8A C9A 121.7(3) . . ? C7A C8A H8A 119.1 . . ? C9A C8A H8A 119.1 . . ? C7B C8B C9B 120.6(3) . . ? C7B C8B H8B 119.7 . . ? C9B C8B H8B 119.7 . . ? C8A C9A C10A 119.4(3) . . ? C8A C9A H9A 120.3 . . ? C10A C9A H9A 120.3 . . ? C10B C9B C8B 119.8(3) . . ? C10B C9B H9B 120.1 . . ? C8B C9B H9B 120.1 . . ? C11A C10A C9A 119.8(3) . . ? C11A C10A H10A 120.1 . . ? C9A C10A H10A 120.1 . . ? C9B C10B C11B 120.8(3) . . ? C9B C10B H10B 119.6 . . ? C11B C10B H10B 119.6 . . ? C10A C11A C12A 120.7(3) . . ? C10A C11A H11A 119.7 . . ? C12A C11A H11A 119.7 . . ? C10B C11B C12B 119.0(3) . . ? C10B C11B H11B 120.5 . . ? C12B C11B H11B 120.5 . . ? C11A C12A C7A 120.1(3) . . ? C11A C12A H12A 120.0 . . ? C7A C12A H12A 120.0 . . ? C7B C12B C11B 120.5(3) . . ? C7B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C18A C13A C14A 119.4(4) . . ? C18A C13A C5A 122.7(4) . . ? C14A C13A C5A 117.9(3) . . ? C14B C13B C18B 118.9(3) . . ? C14B C13B C5B 120.0(3) . . ? C18B C13B C5B 121.1(3) . . ? C13A C14A C15A 118.0(5) . . ? C13A C14A H14A 121.0 . . ? C15A C14A H14A 121.0 . . ? C13B C14B C15B 120.6(3) . . ? C13B C14B H14B 119.7 . . ? C15B C14B H14B 119.7 . . ? C16A C15A C14A 122.8(5) . . ? C16A C15A H15A 118.6 . . ? C14A C15A H15A 118.6 . . ? C14B C15B C16B 120.4(3) . . ? C14B C15B H15B 119.8 . . ? C16B C15B H15B 119.8 . . ? C15A C16A C17A 120.9(4) . . ? C15A C16A H16A 119.5 . . ? C17A C16A H16A 119.5 . . ? C17B C16B C15B 119.7(3) . . ? C17B C16B H16B 120.2 . . ? C15B C16B H16B 120.2 . . ? C16A C17A C18A 118.9(5) . . ? C16A C17A H17A 120.6 . . ? C18A C17A H17A 120.6 . . ? C16B C17B C18B 120.0(3) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C13A C18A C17A 120.0(5) . . ? C13A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C17B C18B C13B 120.5(3) . . ? C17B C18B H18B 119.8 . . ? C13B C18B H18B 119.8 . . ? C2B N1B C5B 108.1(3) . . ? C2B N1B C6B 124.2(3) . . ? C5B N1B C6B 127.7(3) . . ? C2B N3B C4B 106.1(3) . . ? C2B N3B Ni 121.3(2) . . ? C4B N3B Ni 130.0(2) . . ? N3A Ni N3A 87.50(17) 2_655 . ? N3A Ni N3B 91.21(9) 2_655 . ? N3A Ni N3B 177.54(14) . . ? N3A Ni N3B 177.54(14) 2_655 2_655 ? N3A Ni N3B 91.21(9) . 2_655 ? N3B Ni N3B 90.16(17) . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.803 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.072 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.211 239 42 ' ' 2 0.000 0.500 0.711 239 42 ' ' 3 0.500 0.500 0.211 239 42 ' ' 4 0.500 1.000 0.711 239 42 ' ' # start Validation Reply Form _vrf_PLAT420_1-NiL4_{OH}2_H2O ; RESPONSE: Potential H-bond acceptors for the hydrogens of the lattice O2 water molecule are probably within the disordered solvent area which has been removed with the Platon/Squeeze procedure (see also comment below). ; _vrf_PLAT731_1-NiL4_{OH}2_H2O ; RESPONSE: The distance has been restrainted by means of a DFIX instruction. ; _vrf_REFLT03_1-NiL4_{OH}2_H2O ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 2073 Friedel pairs. ; _vrf_PLAT850_1-NiL4_{OH}2_H2O ; RESPONSE: The BASF/TWIN instructions have been used during refinement with Shelxl97. ; _vrf_PLAT605_1-NiL4_{OH}2_H2O ; RESPONSE: The structure contains an area of disordered crystallization water molecules; attemps to model it with a chemically reasonable geometry were unsuccessful. Therefore, the SQUEEZE procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001) was employed to remove the contribution of the electron density associated with those solvent molecules from the intensity data. The solvent-free model and intensity data were used for the final results reported here. ; # end Validation Reply Form #===END data_2-NiL4_NiCl4_2EtOH #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881063' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 N8 Ni, 2(C2 H6 O), Cl4 Ni' _chemical_formula_sum 'C68 H68 Cl4 N8 Ni2 O2' _chemical_formula_weight 1288.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 11.6264(2) _cell_length_b 24.3482(3) _cell_length_c 22.2375(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6295.03(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13943 _cell_measurement_theta_min 3.1018 _cell_measurement_theta_max 30.2627 _exptl_crystal_description prism _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9806 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27016 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 29.07 _reflns_number_total 8297 _reflns_number_gt 6967 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4001 Friedel pairs' _refine_ls_abs_structure_Flack -0.003(12) _refine_ls_number_reflns 8297 _refine_ls_number_parameters 386 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.0000 1.0000 0.554480(18) 0.01519(8) Uani 1 2 d S . . N1B N 1.13952(16) 0.90100(7) 0.43177(9) 0.0211(4) Uani 1 1 d . . . N3B N 1.02749(16) 0.94588(7) 0.49471(9) 0.0180(4) Uani 1 1 d . . . N3A N 0.97497(16) 1.05280(7) 0.61610(9) 0.0177(4) Uani 1 1 d . . . N1A N 1.02993(16) 1.10520(7) 0.69106(10) 0.0201(4) Uani 1 1 d . . . C7B C 0.89531(19) 0.87060(9) 0.52891(10) 0.0196(4) Uani 1 1 d . . . C13B C 1.05836(19) 0.80481(8) 0.43481(10) 0.0195(4) Uani 1 1 d . . . C10A C 0.5861(2) 1.10181(13) 0.51989(12) 0.0367(6) Uani 1 1 d . . . H10A H 0.5213 1.1036 0.4954 0.044 Uiso 1 1 calc R . . C16B C 1.0468(2) 0.69411(9) 0.40306(12) 0.0274(5) Uani 1 1 d . . . H16B H 1.0421 0.6571 0.3930 0.033 Uiso 1 1 calc R . . C12B C 0.90367(19) 0.82076(9) 0.56014(11) 0.0241(5) Uani 1 1 d . . . H12B H 0.9704 0.7998 0.5575 0.029 Uiso 1 1 calc R . . C2B C 1.1157(2) 0.94965(9) 0.45670(10) 0.0210(4) Uani 1 1 d . . . H2B H 1.1555 0.9819 0.4486 0.025 Uiso 1 1 calc R . . C4A C 0.89141(18) 1.09257(8) 0.62489(10) 0.0178(4) Uani 1 1 d . . . C5B C 1.06151(19) 0.86315(8) 0.45389(10) 0.0184(4) Uani 1 1 d . . . C13A C 0.8670(2) 1.17122(9) 0.70319(11) 0.0240(5) Uani 1 1 d . . . C14B C 0.9645(2) 0.78503(9) 0.40355(12) 0.0243(5) Uani 1 1 d . . . H14B H 0.9052 0.8087 0.3928 0.029 Uiso 1 1 calc R . . C14A C 0.7586(2) 1.16374(11) 0.72722(11) 0.0312(6) Uani 1 1 d . . . H14A H 0.7201 1.1306 0.7219 0.037 Uiso 1 1 calc R . . C11A C 0.6370(2) 1.14971(12) 0.53991(11) 0.0317(6) Uani 1 1 d . . . H11A H 0.6042 1.1836 0.5311 0.038 Uiso 1 1 calc R . . C2A C 1.05548(19) 1.06186(9) 0.65735(10) 0.0192(4) Uani 1 1 d . . . H2A H 1.1213 1.0406 0.6620 0.023 Uiso 1 1 calc R . . C11B C 0.8119(2) 0.80262(10) 0.59511(12) 0.0301(5) Uani 1 1 d . . . H11B H 0.8174 0.7694 0.6155 0.036 Uiso 1 1 calc R . . C9B C 0.7036(2) 0.88263(12) 0.56850(12) 0.0325(6) Uani 1 1 d . . . H9B H 0.6366 0.9033 0.5712 0.039 Uiso 1 1 calc R . . C7A C 0.78511(18) 1.09598(9) 0.58964(10) 0.0193(4) Uani 1 1 d . . . C8A C 0.7282(2) 1.04832(10) 0.57108(12) 0.0293(5) Uani 1 1 d . . . H8A H 0.7564 1.0141 0.5825 0.035 Uiso 1 1 calc R . . C18B C 1.1483(2) 0.76905(10) 0.44868(12) 0.0272(5) Uani 1 1 d . . . H18B H 1.2131 0.7822 0.4685 0.033 Uiso 1 1 calc R . . C17B C 1.1415(2) 0.71402(10) 0.43300(12) 0.0305(6) Uani 1 1 d . . . H17B H 1.2015 0.6904 0.4428 0.037 Uiso 1 1 calc R . . C12A C 0.7385(2) 1.14670(10) 0.57363(11) 0.0240(5) Uani 1 1 d . . . H12A H 0.7752 1.1789 0.5855 0.029 Uiso 1 1 calc R . . C5A C 0.92559(19) 1.12561(9) 0.67197(10) 0.0194(4) Uani 1 1 d . . . C4B C 0.99229(17) 0.89117(9) 0.49294(10) 0.0179(4) Uani 1 1 d . . . C8B C 0.7938(2) 0.90092(10) 0.53314(11) 0.0247(5) Uani 1 1 d . . . H8B H 0.7867 0.9337 0.5120 0.030 Uiso 1 1 calc R . . C15B C 0.9584(2) 0.72969(9) 0.38810(11) 0.0278(5) Uani 1 1 d . . . H15B H 0.8944 0.7165 0.3676 0.033 Uiso 1 1 calc R . . C10B C 0.7126(2) 0.83369(12) 0.59981(12) 0.0349(6) Uani 1 1 d . . . H10B H 0.6522 0.8217 0.6239 0.042 Uiso 1 1 calc R . . C9A C 0.6301(2) 1.05165(13) 0.53568(13) 0.0377(7) Uani 1 1 d . . . H9A H 0.5941 1.0197 0.5226 0.045 Uiso 1 1 calc R . . C18A C 0.9219(3) 1.22185(10) 0.71055(12) 0.0329(6) Uani 1 1 d . . . H18A H 0.9942 1.2275 0.6937 0.040 Uiso 1 1 calc R . . C6B C 1.2323(2) 0.89140(10) 0.38864(12) 0.0299(5) Uani 1 1 d . . . H6B1 H 1.2013 0.8752 0.3528 0.045 Uiso 1 1 calc R . . H6B2 H 1.2881 0.8670 0.4060 0.045 Uiso 1 1 calc R . . H6B3 H 1.2684 0.9257 0.3788 0.045 Uiso 1 1 calc R . . C17A C 0.8699(3) 1.26376(11) 0.74268(14) 0.0448(8) Uani 1 1 d . . . H17A H 0.9071 1.2973 0.7473 0.054 Uiso 1 1 calc R . . C16A C 0.7634(3) 1.25570(12) 0.76761(13) 0.0440(8) Uani 1 1 d U . . H16A H 0.7293 1.2836 0.7899 0.053 Uiso 1 1 calc R . . C6A C 1.0983(2) 1.12250(10) 0.74249(12) 0.0300(6) Uani 1 1 d . . . H6A1 H 1.1501 1.0935 0.7536 0.045 Uiso 1 1 calc R . . H6A2 H 1.0484 1.1307 0.7757 0.045 Uiso 1 1 calc R . . H6A3 H 1.1416 1.1547 0.7321 0.045 Uiso 1 1 calc R . . C15A C 0.7069(3) 1.20666(14) 0.75982(12) 0.0426(7) Uani 1 1 d U . . H15A H 0.6340 1.2018 0.7762 0.051 Uiso 1 1 calc R . . Ni2 Ni 1.0000 1.0000 0.84041(2) 0.03226(12) Uani 1 2 d S . . Cl1 Cl 1.13743(6) 0.96986(3) 0.77648(3) 0.03622(16) Uani 1 1 d . . . Cl2 Cl 0.88722(7) 0.95201(3) 0.90608(3) 0.04125(17) Uani 1 1 d . . . O1 O 0.6881(3) 0.88797(10) 0.83565(16) 0.0770(9) Uani 1 1 d D . . H1 H 0.751(2) 0.9011(9) 0.852(2) 0.115 Uiso 1 1 d D . . C19 C 0.6089(3) 0.93289(18) 0.8272(2) 0.0731(12) Uani 1 1 d D . . H19A H 0.5713 0.9422 0.8648 0.088 Uiso 1 1 calc R . . H19B H 0.6486 0.9651 0.8121 0.088 Uiso 1 1 calc R . . C20 C 0.5265(5) 0.9132(3) 0.7839(4) 0.122(3) Uani 1 1 d D . . H20A H 0.5594 0.9149 0.7444 0.183 Uiso 1 1 calc R . . H20B H 0.4587 0.9357 0.7854 0.183 Uiso 1 1 calc R . . H20C H 0.5065 0.8759 0.7931 0.183 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01516(17) 0.01303(16) 0.01738(18) 0.000 0.000 0.00064(13) N1B 0.0234(10) 0.0200(9) 0.0199(9) -0.0001(7) 0.0045(8) -0.0011(7) N3B 0.0197(9) 0.0149(8) 0.0193(9) 0.0004(7) 0.0004(7) -0.0001(7) N3A 0.0170(9) 0.0175(8) 0.0184(9) 0.0011(7) -0.0002(7) 0.0010(7) N1A 0.0217(9) 0.0190(8) 0.0196(10) -0.0009(8) -0.0042(8) -0.0006(6) C7B 0.0183(11) 0.0199(10) 0.0206(10) -0.0030(8) -0.0003(8) -0.0034(8) C13B 0.0226(11) 0.0164(10) 0.0195(11) -0.0020(8) 0.0019(9) -0.0019(8) C10A 0.0137(11) 0.0677(19) 0.0286(14) -0.0003(13) -0.0023(10) 0.0016(12) C16B 0.0437(14) 0.0163(10) 0.0224(11) -0.0020(9) 0.0053(11) -0.0035(10) C12B 0.0246(11) 0.0222(10) 0.0253(12) -0.0014(10) -0.0008(10) -0.0024(8) C2B 0.0236(11) 0.0181(10) 0.0212(11) -0.0009(9) 0.0007(9) -0.0016(9) C4A 0.0176(10) 0.0158(9) 0.0199(11) 0.0020(8) 0.0014(8) -0.0019(8) C5B 0.0175(11) 0.0179(10) 0.0199(11) 0.0003(8) 0.0003(8) 0.0010(8) C13A 0.0355(12) 0.0200(10) 0.0164(11) -0.0007(9) -0.0049(10) 0.0080(9) C14B 0.0212(11) 0.0204(11) 0.0312(13) 0.0021(10) -0.0041(10) 0.0008(9) C14A 0.0367(14) 0.0311(13) 0.0259(13) 0.0062(10) 0.0039(11) 0.0129(11) C11A 0.0230(12) 0.0433(15) 0.0287(14) 0.0080(11) 0.0000(10) 0.0085(11) C2A 0.0171(11) 0.0177(10) 0.0226(11) 0.0007(8) -0.0002(9) 0.0010(8) C11B 0.0343(13) 0.0283(12) 0.0277(13) 0.0032(10) -0.0017(11) -0.0115(10) C9B 0.0130(11) 0.0464(15) 0.0381(16) -0.0049(12) 0.0006(10) -0.0024(10) C7A 0.0132(10) 0.0264(11) 0.0183(11) -0.0005(9) 0.0028(8) 0.0003(8) C8A 0.0189(11) 0.0321(12) 0.0367(14) -0.0060(10) 0.0005(10) -0.0012(9) C18B 0.0273(13) 0.0251(11) 0.0292(13) -0.0031(10) -0.0032(10) 0.0041(9) C17B 0.0342(14) 0.0236(12) 0.0336(14) -0.0006(10) 0.0020(11) 0.0127(10) C12A 0.0209(11) 0.0302(12) 0.0208(11) 0.0029(9) 0.0008(9) 0.0028(9) C5A 0.0204(11) 0.0179(10) 0.0198(11) 0.0026(8) 0.0001(9) 0.0009(8) C4B 0.0182(10) 0.0153(9) 0.0200(10) 0.0020(8) -0.0025(8) -0.0011(8) C8B 0.0200(12) 0.0270(12) 0.0270(12) -0.0006(9) -0.0042(9) -0.0028(9) C15B 0.0368(13) 0.0207(11) 0.0259(13) 0.0018(9) -0.0066(11) -0.0067(10) C10B 0.0273(13) 0.0467(15) 0.0308(14) -0.0027(12) 0.0050(11) -0.0130(11) C9A 0.0197(13) 0.0549(18) 0.0386(16) -0.0141(13) -0.0020(10) -0.0098(12) C18A 0.0446(16) 0.0261(12) 0.0281(14) -0.0023(10) -0.0114(11) 0.0060(11) C6B 0.0323(13) 0.0292(12) 0.0281(13) -0.0049(10) 0.0120(11) -0.0007(10) C17A 0.077(2) 0.0246(13) 0.0330(15) -0.0051(11) -0.0225(16) 0.0124(14) C16A 0.068(2) 0.0373(14) 0.0269(14) -0.0065(11) -0.0144(14) 0.0291(14) C6A 0.0322(13) 0.0302(12) 0.0276(13) -0.0061(10) -0.0143(11) -0.0005(10) C15A 0.0456(17) 0.0550(17) 0.0273(14) 0.0098(12) 0.0044(12) 0.0272(13) Ni2 0.0432(3) 0.0291(3) 0.0245(2) 0.000 0.000 0.0089(2) Cl1 0.0405(4) 0.0372(3) 0.0310(3) -0.0102(3) -0.0093(3) 0.0173(3) Cl2 0.0645(5) 0.0265(3) 0.0328(3) 0.0065(3) 0.0003(3) -0.0004(3) O1 0.0756(19) 0.0526(14) 0.103(2) -0.0015(16) 0.0452(19) -0.0119(14) C19 0.055(2) 0.069(2) 0.096(3) -0.002(2) 0.029(2) -0.010(2) C20 0.099(4) 0.083(4) 0.184(8) -0.049(5) 0.004(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3B 1.8988(19) . ? Ni1 N3B 1.8988(19) 2_775 ? Ni1 N3A 1.901(2) 2_775 ? Ni1 N3A 1.901(2) . ? N1B C2B 1.337(3) . ? N1B C5B 1.383(3) . ? N1B C6B 1.462(3) . ? N3B C2B 1.332(3) . ? N3B C4B 1.394(3) . ? N3A C2A 1.329(3) . ? N3A C4A 1.386(3) . ? N1A C2A 1.328(3) . ? N1A C5A 1.378(3) . ? N1A C6A 1.455(3) . ? C7B C8B 1.395(3) . ? C7B C12B 1.402(3) . ? C7B C4B 1.470(3) . ? C13B C14B 1.380(3) . ? C13B C18B 1.395(3) . ? C13B C5B 1.483(3) . ? C10A C9A 1.370(4) . ? C10A C11A 1.382(4) . ? C10A H10A 0.9300 . ? C16B C17B 1.375(4) . ? C16B C15B 1.384(4) . ? C16B H16B 0.9300 . ? C12B C11B 1.392(3) . ? C12B H12B 0.9300 . ? C2B H2B 0.9300 . ? C4A C5A 1.379(3) . ? C4A C7A 1.466(3) . ? C5B C4B 1.367(3) . ? C13A C14A 1.382(4) . ? C13A C18A 1.398(3) . ? C13A C5A 1.476(3) . ? C14B C15B 1.392(3) . ? C14B H14B 0.9300 . ? C14A C15A 1.407(4) . ? C14A H14A 0.9300 . ? C11A C12A 1.400(3) . ? C11A H11A 0.9300 . ? C2A H2A 0.9300 . ? C11B C10B 1.385(4) . ? C11B H11B 0.9300 . ? C9B C10B 1.384(4) . ? C9B C8B 1.385(3) . ? C9B H9B 0.9300 . ? C7A C12A 1.395(3) . ? C7A C8A 1.398(3) . ? C8A C9A 1.389(4) . ? C8A H8A 0.9300 . ? C18B C17B 1.387(3) . ? C18B H18B 0.9300 . ? C17B H17B 0.9300 . ? C12A H12A 0.9300 . ? C8B H8B 0.9300 . ? C15B H15B 0.9300 . ? C10B H10B 0.9300 . ? C9A H9A 0.9300 . ? C18A C17A 1.385(4) . ? C18A H18A 0.9300 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C17A C16A 1.370(5) . ? C17A H17A 0.9300 . ? C16A C15A 1.374(5) . ? C16A H16A 0.9300 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C15A H15A 0.9300 . ? Ni2 Cl1 2.2611(8) 2_775 ? Ni2 Cl1 2.2611(8) . ? Ni2 Cl2 2.2841(8) . ? Ni2 Cl2 2.2842(8) 2_775 ? O1 C19 1.442(5) . ? O1 H1 0.883(10) . ? C19 C20 1.441(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3B Ni1 N3B 91.15(12) . 2_775 ? N3B Ni1 N3A 90.55(7) . 2_775 ? N3B Ni1 N3A 178.20(9) 2_775 2_775 ? N3B Ni1 N3A 178.21(9) . . ? N3B Ni1 N3A 90.54(7) 2_775 . ? N3A Ni1 N3A 87.77(11) 2_775 . ? C2B N1B C5B 107.88(18) . . ? C2B N1B C6B 124.50(19) . . ? C5B N1B C6B 127.62(19) . . ? C2B N3B C4B 105.90(18) . . ? C2B N3B Ni1 121.73(15) . . ? C4B N3B Ni1 129.30(16) . . ? C2A N3A C4A 106.28(19) . . ? C2A N3A Ni1 120.13(15) . . ? C4A N3A Ni1 132.97(16) . . ? C2A N1A C5A 108.03(19) . . ? C2A N1A C6A 123.46(19) . . ? C5A N1A C6A 128.23(19) . . ? C8B C7B C12B 118.9(2) . . ? C8B C7B C4B 120.3(2) . . ? C12B C7B C4B 120.8(2) . . ? C14B C13B C18B 119.1(2) . . ? C14B C13B C5B 119.8(2) . . ? C18B C13B C5B 121.1(2) . . ? C9A C10A C11A 120.7(2) . . ? C9A C10A H10A 119.7 . . ? C11A C10A H10A 119.7 . . ? C17B C16B C15B 119.3(2) . . ? C17B C16B H16B 120.3 . . ? C15B C16B H16B 120.3 . . ? C11B C12B C7B 119.9(2) . . ? C11B C12B H12B 120.0 . . ? C7B C12B H12B 120.0 . . ? N3B C2B N1B 111.19(19) . . ? N3B C2B H2B 124.4 . . ? N1B C2B H2B 124.4 . . ? C5A C4A N3A 108.23(19) . . ? C5A C4A C7A 128.0(2) . . ? N3A C4A C7A 123.73(19) . . ? C4B C5B N1B 106.23(18) . . ? C4B C5B C13B 130.2(2) . . ? N1B C5B C13B 123.54(19) . . ? C14A C13A C18A 119.2(2) . . ? C14A C13A C5A 120.2(2) . . ? C18A C13A C5A 120.5(2) . . ? C13B C14B C15B 120.1(2) . . ? C13B C14B H14B 119.9 . . ? C15B C14B H14B 119.9 . . ? C13A C14A C15A 119.4(3) . . ? C13A C14A H14A 120.3 . . ? C15A C14A H14A 120.3 . . ? C10A C11A C12A 119.3(2) . . ? C10A C11A H11A 120.3 . . ? C12A C11A H11A 120.3 . . ? N1A C2A N3A 111.35(19) . . ? N1A C2A H2A 124.3 . . ? N3A C2A H2A 124.3 . . ? C10B C11B C12B 120.5(2) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C10B C9B C8B 120.3(2) . . ? C10B C9B H9B 119.8 . . ? C8B C9B H9B 119.8 . . ? C12A C7A C8A 118.4(2) . . ? C12A C7A C4A 120.9(2) . . ? C8A C7A C4A 120.64(19) . . ? C9A C8A C7A 120.5(2) . . ? C9A C8A H8A 119.8 . . ? C7A C8A H8A 119.8 . . ? C17B C18B C13B 120.3(2) . . ? C17B C18B H18B 119.8 . . ? C13B C18B H18B 119.8 . . ? C16B C17B C18B 120.5(2) . . ? C16B C17B H17B 119.7 . . ? C18B C17B H17B 119.7 . . ? C7A C12A C11A 120.7(2) . . ? C7A C12A H12A 119.6 . . ? C11A C12A H12A 119.6 . . ? N1A C5A C4A 106.10(19) . . ? N1A C5A C13A 122.2(2) . . ? C4A C5A C13A 131.5(2) . . ? C5B C4B N3B 108.79(19) . . ? C5B C4B C7B 128.8(2) . . ? N3B C4B C7B 122.36(19) . . ? C9B C8B C7B 120.6(2) . . ? C9B C8B H8B 119.7 . . ? C7B C8B H8B 119.7 . . ? C16B C15B C14B 120.6(2) . . ? C16B C15B H15B 119.7 . . ? C14B C15B H15B 119.7 . . ? C9B C10B C11B 119.7(2) . . ? C9B C10B H10B 120.1 . . ? C11B C10B H10B 120.1 . . ? C10A C9A C8A 120.3(3) . . ? C10A C9A H9A 119.9 . . ? C8A C9A H9A 119.9 . . ? C17A C18A C13A 120.7(3) . . ? C17A C18A H18A 119.6 . . ? C13A C18A H18A 119.6 . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C16A C17A C18A 119.9(3) . . ? C16A C17A H17A 120.1 . . ? C18A C17A H17A 120.1 . . ? C17A C16A C15A 120.4(3) . . ? C17A C16A H16A 119.8 . . ? C15A C16A H16A 119.8 . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C16A C15A C14A 120.4(3) . . ? C16A C15A H15A 119.8 . . ? C14A C15A H15A 119.8 . . ? Cl1 Ni2 Cl1 102.09(4) 2_775 . ? Cl1 Ni2 Cl2 99.34(3) 2_775 . ? Cl1 Ni2 Cl2 129.91(3) . . ? Cl1 Ni2 Cl2 129.90(3) 2_775 2_775 ? Cl1 Ni2 Cl2 99.34(3) . 2_775 ? Cl2 Ni2 Cl2 100.52(4) . 2_775 ? C19 O1 H1 108.2(12) . . ? C20 C19 O1 105.0(4) . . ? C20 C19 H19A 110.7 . . ? O1 C19 H19A 110.7 . . ? C20 C19 H19B 110.7 . . ? O1 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.600 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.068 # start Validation Reply Form _vrf_PLAT731_2-NiL4_NiCl4_2EtOH ; RESPONSE: The O1-H1 distance of the ethanol molecule has been restrainted by means of a DFIX instruction. ; _vrf_REFLT03_2-NiL4_NiCl4_2EtOH ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 4001 Friedel pairs. ; # end Validation Reply Form #===END data_3-NiL4_Br2_3.4H2O #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881064' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 N8 Ni 2+, 2Br 2-, 3.4(H2 O)' _chemical_formula_sum 'C64 H62.80 Br2 N8 Ni O3.40' _chemical_formula_weight 1216.95 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 11.4808(2) _cell_length_b 23.4663(4) _cell_length_c 22.5673(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6079.90(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7260 _cell_measurement_theta_min 3.0655 _cell_measurement_theta_max 30.3801 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 1.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9729 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19272 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4785 _reflns_number_gt 3791 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; The structure is disordered. The disorder mainly affects the bromide counterion, which was modelled in two sites (Br1 and Br2), as well as the crystallization water molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1453P)^2^] 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, 2031 Friedel pairs' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 4785 _refine_ls_number_parameters 366 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.2007 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.106 _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 Ni Ni 0.0000 0.0000 0.36462(6) 0.0217(3) Uani 1 2 d S . . N1A N 0.0061(5) -0.1060(2) 0.2253(3) 0.0269(13) Uani 1 1 d . . . C2A C 0.0458(6) -0.0646(3) 0.2613(3) 0.0247(14) Uani 1 1 d . . . H2A H 0.1170 -0.0462 0.2570 0.030 Uiso 1 1 calc R . . N3A N -0.0306(5) -0.0536(2) 0.3039(3) 0.0229(13) Uani 1 1 d . . . C4A C -0.1224(6) -0.0906(3) 0.2956(3) 0.0237(14) Uani 1 1 d . . . C5A C -0.1010(6) -0.1218(3) 0.2458(3) 0.0296(17) Uani 1 1 d . . . C6A C 0.0680(8) -0.1250(4) 0.1719(4) 0.051(2) Uani 1 1 d . . . H6A1 H 0.1325 -0.1000 0.1643 0.076 Uiso 1 1 calc R . . H6A2 H 0.0158 -0.1244 0.1387 0.076 Uiso 1 1 calc R . . H6A3 H 0.0964 -0.1631 0.1778 0.076 Uiso 1 1 calc R . . C7A C -0.2268(5) -0.0910(3) 0.3338(3) 0.0238(14) Uani 1 1 d . . . C8A C -0.2752(6) -0.0389(3) 0.3539(4) 0.0381(19) Uani 1 1 d . . . H8A H -0.2440 -0.0044 0.3413 0.046 Uiso 1 1 calc R . . C9A C -0.3691(7) -0.0397(4) 0.3921(4) 0.045(2) Uani 1 1 d . . . H9A H -0.3984 -0.0055 0.4066 0.054 Uiso 1 1 calc R . . C10A C -0.4199(6) -0.0901(4) 0.4090(4) 0.0375(18) Uani 1 1 d . . . H10A H -0.4850 -0.0900 0.4336 0.045 Uiso 1 1 calc R . . C11A C -0.3730(6) -0.1410(3) 0.3891(3) 0.0292(16) Uani 1 1 d . . . H11A H -0.4061 -0.1753 0.4009 0.035 Uiso 1 1 calc R . . C12A C -0.2777(5) -0.1412(3) 0.3519(3) 0.0224(14) Uani 1 1 d . . . H12A H -0.2474 -0.1757 0.3388 0.027 Uiso 1 1 calc R . . C13A C -0.1766(8) -0.1634(3) 0.2132(3) 0.041(2) Uani 1 1 d . . . C14A C -0.2922(7) -0.1459(4) 0.1998(4) 0.047(2) Uani 1 1 d . . . H14A H -0.3210 -0.1110 0.2128 0.056 Uiso 1 1 calc R . . C15A C -0.3617(11) -0.1835(5) 0.1660(4) 0.069(3) Uani 1 1 d . . . H15A H -0.4375 -0.1732 0.1562 0.082 Uiso 1 1 calc R . . C16A C -0.3208(12) -0.2322(6) 0.1486(4) 0.065(3) Uani 1 1 d . . . H16A H -0.3687 -0.2555 0.1259 0.078 Uiso 1 1 calc R . . C17A C -0.2122(13) -0.2511(4) 0.1618(5) 0.070(4) Uani 1 1 d . . . H17A H -0.1869 -0.2865 0.1486 0.084 Uiso 1 1 calc R . . C18A C -0.1377(9) -0.2155(4) 0.1962(4) 0.050(2) Uani 1 1 d . . . H18A H -0.0636 -0.2278 0.2068 0.060 Uiso 1 1 calc R . . N1B N 0.1327(5) 0.0977(2) 0.4912(3) 0.0310(14) Uani 1 1 d . . . C2B C 0.1105(6) 0.0488(3) 0.4658(3) 0.0322(17) Uani 1 1 d . . . H2B H 0.1463 0.0143 0.4749 0.039 Uiso 1 1 calc R . . N3B N 0.0260(5) 0.0566(2) 0.4239(3) 0.0235(13) Uani 1 1 d . . . C4B C -0.0024(5) 0.1131(3) 0.4244(3) 0.0231(14) Uani 1 1 d . . . C5B C 0.0634(6) 0.1398(3) 0.4683(3) 0.0241(15) Uani 1 1 d . . . C6B C 0.2191(7) 0.1054(3) 0.5401(4) 0.042(2) Uani 1 1 d . . . H6B1 H 0.1819 0.0984 0.5775 0.064 Uiso 1 1 calc R . . H6B2 H 0.2484 0.1437 0.5393 0.064 Uiso 1 1 calc R . . H6B3 H 0.2824 0.0792 0.5349 0.064 Uiso 1 1 calc R . . C7B C -0.0959(6) 0.1377(3) 0.3875(3) 0.0287(16) Uani 1 1 d . . . C8B C -0.2021(6) 0.1102(3) 0.3822(3) 0.0320(17) Uani 1 1 d . . . H8B H -0.2164 0.0771 0.4037 0.038 Uiso 1 1 calc R . . C9B C -0.2883(6) 0.1321(4) 0.3445(3) 0.0385(19) Uani 1 1 d . . . H9B H -0.3605 0.1143 0.3425 0.046 Uiso 1 1 calc R . . C10B C -0.2669(7) 0.1794(4) 0.3106(4) 0.043(2) Uani 1 1 d . . . H10B H -0.3237 0.1932 0.2849 0.052 Uiso 1 1 calc R . . C11B C -0.1607(8) 0.2064(4) 0.3149(4) 0.046(2) Uani 1 1 d . . . H11B H -0.1454 0.2382 0.2917 0.056 Uiso 1 1 calc R . . C12B C -0.0766(6) 0.1865(3) 0.3535(3) 0.0286(16) Uani 1 1 d . . . H12B H -0.0063 0.2059 0.3569 0.034 Uiso 1 1 calc R . . C13B C 0.0612(6) 0.2002(3) 0.4874(3) 0.0303(16) Uani 1 1 d . . . C14B C -0.0348(6) 0.2205(3) 0.5181(3) 0.0248(14) Uani 1 1 d . . . H14B H -0.0955 0.1960 0.5279 0.030 Uiso 1 1 calc R . . C15B C -0.0401(7) 0.2774(3) 0.5342(4) 0.0359(17) Uani 1 1 d . . . H15B H -0.1051 0.2910 0.5543 0.043 Uiso 1 1 calc R . . C16B C 0.0497(6) 0.3143(3) 0.5207(3) 0.0269(15) Uani 1 1 d . . . H16B H 0.0470 0.3522 0.5326 0.032 Uiso 1 1 calc R . . C17B C 0.1441(7) 0.2936(3) 0.4892(4) 0.0366(18) Uani 1 1 d . . . H17B H 0.2044 0.3181 0.4789 0.044 Uiso 1 1 calc R . . C18B C 0.1499(6) 0.2380(3) 0.4732(3) 0.0349(18) Uani 1 1 d . . . H18B H 0.2143 0.2250 0.4522 0.042 Uiso 1 1 calc R . . Br1 Br 0.60869(18) 0.08218(9) 0.10292(13) 0.0857(8) Uani 0.55 1 d P . . Br2 Br 0.0000 0.0000 0.0648(2) 0.1766(17) Uani 0.90 2 d SPDU . . O1 O 0.1999(12) 0.0118(4) 0.1677(6) 0.096(3) Uani 0.80 1 d PU . . O2 O 0.3023(10) -0.0547(4) 0.5114(5) 0.104(3) Uani 0.90 1 d PDU . . 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 Ni 0.0236(5) 0.0192(5) 0.0224(6) 0.000 0.000 -0.0012(4) N1A 0.040(3) 0.024(3) 0.017(3) -0.003(2) 0.002(2) -0.001(2) C2A 0.023(3) 0.021(3) 0.030(4) 0.006(3) 0.000(3) 0.000(3) N3A 0.029(3) 0.017(3) 0.023(3) -0.002(2) -0.009(3) 0.002(3) C4A 0.028(3) 0.023(3) 0.021(4) 0.004(3) -0.002(3) -0.001(3) C5A 0.037(4) 0.021(4) 0.030(4) 0.005(3) -0.002(3) -0.010(3) C6A 0.064(6) 0.044(5) 0.045(5) -0.015(4) 0.028(4) -0.010(4) C7A 0.019(3) 0.028(3) 0.025(3) -0.007(3) -0.008(3) -0.007(3) C8A 0.024(3) 0.026(3) 0.064(6) 0.000(4) 0.003(4) -0.003(3) C9A 0.031(4) 0.041(5) 0.064(6) 0.006(4) 0.010(4) 0.004(3) C10A 0.024(3) 0.053(5) 0.036(4) 0.004(4) 0.002(3) -0.007(3) C11A 0.023(3) 0.032(4) 0.033(4) 0.008(3) -0.002(3) -0.015(3) C12A 0.028(3) 0.019(3) 0.020(4) 0.003(3) -0.010(3) -0.006(2) C13A 0.067(6) 0.039(4) 0.016(4) 0.000(3) 0.007(4) -0.030(4) C14A 0.053(5) 0.053(5) 0.035(5) 0.007(4) -0.015(4) -0.026(4) C15A 0.093(8) 0.075(8) 0.038(5) 0.021(5) -0.034(5) -0.056(6) C16A 0.094(9) 0.072(8) 0.030(5) -0.004(5) 0.003(5) -0.046(7) C17A 0.130(11) 0.037(5) 0.042(6) -0.001(4) 0.028(6) -0.036(6) C18A 0.084(6) 0.035(5) 0.031(4) -0.009(4) 0.016(4) -0.030(4) N1B 0.034(3) 0.023(3) 0.037(4) -0.003(3) -0.002(3) -0.002(2) C2B 0.033(4) 0.039(4) 0.024(4) -0.008(3) -0.002(3) 0.001(3) N3B 0.028(3) 0.020(3) 0.022(3) -0.002(2) 0.005(3) 0.004(2) C4B 0.025(3) 0.023(3) 0.020(3) 0.004(3) 0.007(3) -0.005(3) C5B 0.026(4) 0.027(4) 0.019(3) -0.003(3) 0.009(3) -0.002(3) C6B 0.060(5) 0.024(4) 0.044(5) -0.004(3) -0.019(4) -0.003(4) C7B 0.036(4) 0.029(4) 0.021(3) -0.001(3) 0.006(3) 0.002(3) C8B 0.024(3) 0.040(4) 0.032(4) 0.001(3) 0.002(3) 0.002(3) C9B 0.026(4) 0.052(5) 0.037(5) -0.006(4) 0.008(3) 0.008(3) C10B 0.039(5) 0.055(5) 0.036(5) 0.004(4) -0.007(4) 0.016(4) C11B 0.071(6) 0.036(4) 0.032(4) -0.002(4) 0.012(4) 0.019(4) C12B 0.035(4) 0.019(3) 0.032(4) -0.005(3) 0.011(3) 0.005(3) C13B 0.040(4) 0.023(3) 0.028(4) -0.004(3) -0.002(3) 0.000(3) C14B 0.024(3) 0.025(3) 0.026(4) -0.002(3) 0.004(3) -0.002(3) C15B 0.039(4) 0.026(4) 0.042(5) 0.001(3) 0.005(4) 0.013(3) C16B 0.034(4) 0.026(3) 0.021(4) -0.003(3) -0.005(3) 0.003(3) C17B 0.042(4) 0.028(4) 0.040(5) 0.004(4) 0.004(4) -0.014(3) C18B 0.035(4) 0.035(4) 0.035(4) -0.008(3) 0.013(3) 0.000(3) Br1 0.0643(12) 0.0634(12) 0.129(2) 0.0233(13) -0.0108(12) 0.0107(10) Br2 0.205(3) 0.153(3) 0.171(3) 0.000 0.000 -0.088(2) O1 0.129(7) 0.062(5) 0.098(7) -0.022(5) 0.050(6) -0.029(5) O2 0.143(7) 0.054(5) 0.114(7) -0.009(5) -0.001(6) 0.029(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3A 1.893(6) . ? Ni N3A 1.893(6) 2 ? Ni N3B 1.908(6) 2 ? Ni N3B 1.908(6) . ? N1A C2A 1.347(9) . ? N1A C5A 1.365(9) . ? N1A C6A 1.469(10) . ? C2A N3A 1.326(10) . ? C2A H2A 0.9300 . ? N3A C4A 1.379(9) . ? C4A C5A 1.364(10) . ? C4A C7A 1.477(9) . ? C5A C13A 1.498(10) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C12A 1.377(9) . ? C7A C8A 1.416(10) . ? C8A C9A 1.381(11) . ? C8A H8A 0.9300 . ? C9A C10A 1.373(12) . ? C9A H9A 0.9300 . ? C10A C11A 1.386(11) . ? C10A H10A 0.9300 . ? C11A C12A 1.380(10) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C18A 1.357(12) . ? C13A C14A 1.422(12) . ? C14A C15A 1.413(12) . ? C14A H14A 0.9300 . ? C15A C16A 1.296(18) . ? C15A H15A 0.9300 . ? C16A C17A 1.355(18) . ? C16A H16A 0.9300 . ? C17A C18A 1.426(14) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? N1B C2B 1.307(9) . ? N1B C5B 1.370(9) . ? N1B C6B 1.495(10) . ? C2B N3B 1.367(9) . ? C2B H2B 0.9300 . ? N3B C4B 1.366(9) . ? C4B C5B 1.393(10) . ? C4B C7B 1.477(10) . ? C5B C13B 1.484(9) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B C8B 1.386(10) . ? C7B C12B 1.394(10) . ? C8B C9B 1.402(10) . ? C8B H8B 0.9300 . ? C9B C10B 1.371(12) . ? C9B H9B 0.9300 . ? C10B C11B 1.377(12) . ? C10B H10B 0.9300 . ? C11B C12B 1.381(11) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.386(10) . ? C13B C18B 1.388(10) . ? C14B C15B 1.385(10) . ? C14B H14B 0.9300 . ? C15B C16B 1.379(11) . ? C15B H15B 0.9300 . ? C16B C17B 1.384(11) . ? C16B H16B 0.9300 . ? C17B C18B 1.354(10) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? 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 N3A Ni N3A 87.2(4) . 2 ? N3A Ni N3B 91.0(2) . 2 ? N3A Ni N3B 177.2(3) 2 2 ? N3A Ni N3B 177.2(3) . . ? N3A Ni N3B 91.0(2) 2 . ? N3B Ni N3B 90.9(4) 2 . ? C2A N1A C5A 107.2(6) . . ? C2A N1A C6A 123.5(6) . . ? C5A N1A C6A 129.1(6) . . ? N3A C2A N1A 110.8(6) . . ? N3A C2A H2A 124.6 . . ? N1A C2A H2A 124.6 . . ? C2A N3A C4A 106.6(6) . . ? C2A N3A Ni 122.1(5) . . ? C4A N3A Ni 131.2(5) . . ? C5A C4A N3A 108.2(6) . . ? C5A C4A C7A 128.6(6) . . ? N3A C4A C7A 123.0(6) . . ? C4A C5A N1A 107.2(6) . . ? C4A C5A C13A 130.5(7) . . ? N1A C5A C13A 122.1(7) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C12A C7A C8A 118.5(6) . . ? C12A C7A C4A 121.5(6) . . ? C8A C7A C4A 120.0(6) . . ? C9A C8A C7A 119.7(7) . . ? C9A C8A H8A 120.2 . . ? C7A C8A H8A 120.2 . . ? C10A C9A C8A 121.1(8) . . ? C10A C9A H9A 119.5 . . ? C8A C9A H9A 119.5 . . ? C9A C10A C11A 119.2(7) . . ? C9A C10A H10A 120.4 . . ? C11A C10A H10A 120.4 . . ? C12A C11A C10A 120.6(6) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C7A C12A C11A 120.9(6) . . ? C7A C12A H12A 119.5 . . ? C11A C12A H12A 119.5 . . ? C18A C13A C14A 120.4(8) . . ? C18A C13A C5A 122.3(8) . . ? C14A C13A C5A 117.2(7) . . ? C15A C14A C13A 117.5(10) . . ? C15A C14A H14A 121.2 . . ? C13A C14A H14A 121.2 . . ? C16A C15A C14A 120.6(12) . . ? C16A C15A H15A 119.7 . . ? C14A C15A H15A 119.7 . . ? C15A C16A C17A 123.7(10) . . ? C15A C16A H16A 118.1 . . ? C17A C16A H16A 118.1 . . ? C16A C17A C18A 118.6(10) . . ? C16A C17A H17A 120.7 . . ? C18A C17A H17A 120.7 . . ? C13A C18A C17A 119.0(11) . . ? C13A C18A H18A 120.5 . . ? C17A C18A H18A 120.5 . . ? C2B N1B C5B 110.7(6) . . ? C2B N1B C6B 124.0(6) . . ? C5B N1B C6B 125.2(6) . . ? N1B C2B N3B 108.9(6) . . ? N1B C2B H2B 125.6 . . ? N3B C2B H2B 125.6 . . ? C4B N3B C2B 107.0(6) . . ? C4B N3B Ni 130.1(5) . . ? C2B N3B Ni 120.2(5) . . ? N3B C4B C5B 108.3(6) . . ? N3B C4B C7B 123.3(6) . . ? C5B C4B C7B 128.2(6) . . ? N1B C5B C4B 105.0(6) . . ? N1B C5B C13B 126.1(6) . . ? C4B C5B C13B 128.9(6) . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C8B C7B C12B 118.4(7) . . ? C8B C7B C4B 120.3(6) . . ? C12B C7B C4B 121.1(6) . . ? C7B C8B C9B 120.1(7) . . ? C7B C8B H8B 119.9 . . ? C9B C8B H8B 119.9 . . ? C10B C9B C8B 120.6(7) . . ? C10B C9B H9B 119.7 . . ? C8B C9B H9B 119.7 . . ? C9B C10B C11B 119.4(7) . . ? C9B C10B H10B 120.3 . . ? C11B C10B H10B 120.3 . . ? C10B C11B C12B 120.6(8) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C11B C12B C7B 120.9(7) . . ? C11B C12B H12B 119.6 . . ? C7B C12B H12B 119.6 . . ? C14B C13B C18B 118.7(6) . . ? C14B C13B C5B 119.2(6) . . ? C18B C13B C5B 122.1(6) . . ? C15B C14B C13B 119.8(6) . . ? C15B C14B H14B 120.1 . . ? C13B C14B H14B 120.1 . . ? C16B C15B C14B 120.9(7) . . ? C16B C15B H15B 119.5 . . ? C14B C15B H15B 119.5 . . ? C15B C16B C17B 118.6(6) . . ? C15B C16B H16B 120.7 . . ? C17B C16B H16B 120.7 . . ? C18B C17B C16B 120.9(7) . . ? C18B C17B H17B 119.6 . . ? C16B C17B H17B 119.6 . . ? C17B C18B C13B 121.1(7) . . ? C17B C18B H18B 119.4 . . ? C13B C18B H18B 119.4 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.321 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.108 # start Validation Reply Form _vrf_PLAT311_3-NiL4_Br2_3.4H2O ; RESPONSE: It was not possible to locate the H-atoms of the lattice water molecules O1 and O2 from a difference map. ; _vrf_PLAT041_3-NiL4_Br2_3.4H2O ; RESPONSE: The missing (not located by a difference synthesis) H-atoms of the crystallization water molecules O1 and O2 have been included in the sum and moiety formula and the Mr, Dx and F(000) have been modified accordingly. These modifications account for the differences detected in the relevant data items. ; _vrf_PLAT077_3-NiL4_Br2_3.4H2O ; RESPONSE: Due to the partially occupied solvent sites by water molecules O1 and O2. ; _vrf_FORMU01_3-NiL4_Br2_3.4H2O ; RESPONSE: See comment above. ; _vrf_REFLT03_3-NiL4_Br2_3.4H2O ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 2031 Friedel pairs. ; # end Validation Reply Form #===END data_4-NiL4_{NO3}2_2.8MeOH #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881065' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C64 H56 N8 Ni 2+), 2.8(C H4 O), 2(N O3 1-)' _chemical_formula_sum 'C66.80 H67.20 N10 Ni O8.80' _chemical_formula_weight 1209.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1951(2) _cell_length_b 29.4448(4) _cell_length_c 18.0834(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.759(2) _cell_angle_gamma 90.00 _cell_volume 5919.54(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12070 _cell_measurement_theta_min 3.0660 _cell_measurement_theta_max 30.2290 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2545.6 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9024 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50939 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.50 _reflns_number_total 14953 _reflns_number_gt 8408 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)' _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14953 _refine_ls_number_parameters 801 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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 Ni Ni 0.00112(3) 0.784727(10) 0.739040(16) 0.01388(8) Uani 1 1 d . . . N1B N 0.23803(16) 0.69583(6) 0.67262(10) 0.0149(4) Uani 1 1 d . . . C2B C 0.2035(2) 0.73585(8) 0.69732(12) 0.0155(5) Uani 1 1 d . . . H2B H 0.2561 0.7585 0.7168 0.019 Uiso 1 1 calc R . . N3B N 0.08438(16) 0.73933(6) 0.69058(10) 0.0139(4) Uani 1 1 d . . . C4B C 0.0404(2) 0.69897(8) 0.65835(12) 0.0148(5) Uani 1 1 d . . . C5B C 0.1357(2) 0.67133(8) 0.64750(12) 0.0143(5) Uani 1 1 d . . . C6B C 0.36344(19) 0.68298(8) 0.66901(14) 0.0216(6) Uani 1 1 d . . . H6B1 H 0.3893 0.6626 0.7092 0.032 Uiso 1 1 calc R . . H6B2 H 0.4130 0.7097 0.6730 0.032 Uiso 1 1 calc R . . H6B3 H 0.3703 0.6682 0.6224 0.032 Uiso 1 1 calc R . . C7B C -0.0891(2) 0.69142(8) 0.63782(12) 0.0158(5) Uani 1 1 d . . . C8B C -0.1581(2) 0.72460(8) 0.59801(13) 0.0189(5) Uani 1 1 d . . . H8B H -0.1216 0.7512 0.5842 0.023 Uiso 1 1 calc R . . C9B C -0.2804(2) 0.71854(9) 0.57872(13) 0.0253(6) Uani 1 1 d . . . H9B H -0.3257 0.7410 0.5523 0.030 Uiso 1 1 calc R . . C10B C -0.3350(2) 0.67905(9) 0.59883(14) 0.0264(6) Uani 1 1 d . . . H10B H -0.4172 0.6750 0.5862 0.032 Uiso 1 1 calc R . . C11B C -0.2673(2) 0.64560(9) 0.63772(14) 0.0254(6) Uani 1 1 d . . . H11B H -0.3043 0.6190 0.6508 0.030 Uiso 1 1 calc R . . C12B C -0.1448(2) 0.65146(8) 0.65732(13) 0.0200(5) Uani 1 1 d . . . H12B H -0.0998 0.6288 0.6834 0.024 Uiso 1 1 calc R . . C13B C 0.1367(2) 0.62515(8) 0.61630(13) 0.0180(5) Uani 1 1 d . . . C14B C 0.0604(2) 0.61404(9) 0.55258(14) 0.0236(6) Uani 1 1 d . . . H14B H 0.0095 0.6360 0.5292 0.028 Uiso 1 1 calc R . . C15B C 0.0597(2) 0.57047(10) 0.52377(16) 0.0332(7) Uani 1 1 d . . . H15B H 0.0077 0.5632 0.4815 0.040 Uiso 1 1 calc R . . C16B C 0.1352(3) 0.53802(10) 0.55721(18) 0.0376(8) Uani 1 1 d . . . H16B H 0.1363 0.5091 0.5366 0.045 Uiso 1 1 calc R . . C17B C 0.2093(3) 0.54809(9) 0.62108(18) 0.0366(7) Uani 1 1 d . . . H17B H 0.2588 0.5257 0.6444 0.044 Uiso 1 1 calc R . . C18B C 0.2109(2) 0.59153(9) 0.65117(15) 0.0270(6) Uani 1 1 d . . . H18B H 0.2612 0.5982 0.6945 0.032 Uiso 1 1 calc R . . N1A N -0.23023(16) 0.69569(6) 0.81100(10) 0.0154(4) Uani 1 1 d . . . C2A C -0.1978(2) 0.73451(8) 0.78121(12) 0.0164(5) Uani 1 1 d . . . H2A H -0.2514 0.7557 0.7581 0.020 Uiso 1 1 calc R . . N3A N -0.07884(16) 0.73904(6) 0.78883(10) 0.0133(4) Uani 1 1 d . . . C4A C -0.03241(19) 0.70059(7) 0.82627(12) 0.0134(5) Uani 1 1 d . . . C5A C -0.1266(2) 0.67312(8) 0.84035(12) 0.0152(5) Uani 1 1 d . . . C6A C -0.3551(2) 0.68250(9) 0.81609(14) 0.0239(6) Uani 1 1 d . . . H6A1 H -0.4079 0.7065 0.7968 0.036 Uiso 1 1 calc R . . H6A2 H -0.3657 0.6770 0.8672 0.036 Uiso 1 1 calc R . . H6A3 H -0.3735 0.6554 0.7876 0.036 Uiso 1 1 calc R . . C7A C 0.0971(2) 0.69409(8) 0.84747(12) 0.0153(5) Uani 1 1 d . . . C8A C 0.1653(2) 0.72828(8) 0.88541(13) 0.0191(5) Uani 1 1 d . . . H8A H 0.1280 0.7549 0.8980 0.023 Uiso 1 1 calc R . . C9A C 0.2880(2) 0.72303(9) 0.90459(13) 0.0243(6) Uani 1 1 d . . . H9A H 0.3324 0.7460 0.9301 0.029 Uiso 1 1 calc R . . C10A C 0.3445(2) 0.68368(9) 0.88591(13) 0.0243(6) Uani 1 1 d . . . H10A H 0.4270 0.6804 0.8982 0.029 Uiso 1 1 calc R . . C11A C 0.2780(2) 0.64899(9) 0.84879(13) 0.0237(6) Uani 1 1 d . . . H11A H 0.3160 0.6224 0.8367 0.028 Uiso 1 1 calc R . . C12A C 0.1551(2) 0.65405(8) 0.82983(13) 0.0189(5) Uani 1 1 d . . . H12A H 0.1108 0.6307 0.8052 0.023 Uiso 1 1 calc R . . C13A C -0.1260(2) 0.62897(8) 0.87925(13) 0.0169(5) Uani 1 1 d . . . C14A C -0.0585(2) 0.62364(8) 0.94810(14) 0.0212(6) Uani 1 1 d . . . H14A H -0.0152 0.6481 0.9700 0.025 Uiso 1 1 calc R . . C15A C -0.0549(2) 0.58198(9) 0.98477(15) 0.0285(6) Uani 1 1 d . . . H15A H -0.0089 0.5786 1.0307 0.034 Uiso 1 1 calc R . . C16A C -0.1201(2) 0.54569(9) 0.95240(16) 0.0309(7) Uani 1 1 d . . . H16A H -0.1185 0.5179 0.9770 0.037 Uiso 1 1 calc R . . C17A C -0.1874(2) 0.55042(9) 0.88409(16) 0.0292(6) Uani 1 1 d . . . H17A H -0.2308 0.5259 0.8625 0.035 Uiso 1 1 calc R . . C18A C -0.1903(2) 0.59202(8) 0.84731(15) 0.0237(6) Uani 1 1 d . . . H18A H -0.2355 0.5951 0.8010 0.028 Uiso 1 1 calc R . . N1D N -0.14163(19) 0.86449(7) 0.88483(11) 0.0244(5) Uani 1 1 d . . . C2D C -0.0828(2) 0.82876(8) 0.86217(13) 0.0218(6) Uani 1 1 d . . . H2D H -0.0467 0.8065 0.8937 0.026 Uiso 1 1 calc R . . N3D N -0.08252(16) 0.82908(6) 0.78892(10) 0.0164(4) Uani 1 1 d . . . C4D C -0.1462(2) 0.86756(8) 0.76295(13) 0.0154(5) Uani 1 1 d . . . C5D C -0.1837(2) 0.89000(8) 0.82255(13) 0.0214(6) Uani 1 1 d . . . C6D C -0.1556(3) 0.87457(11) 0.96267(15) 0.0447(9) Uani 1 1 d . . . H6D1 H -0.0873 0.8915 0.9847 0.067 Uiso 1 1 calc R . . H6D2 H -0.1614 0.8467 0.9895 0.067 Uiso 1 1 calc R . . H6D3 H -0.2274 0.8921 0.9649 0.067 Uiso 1 1 calc R . . C7D C -0.1740(2) 0.87832(8) 0.68323(13) 0.0158(5) Uani 1 1 d . . . C8D C -0.2286(2) 0.84584(8) 0.63425(13) 0.0191(5) Uani 1 1 d . . . H8D H -0.2451 0.8172 0.6521 0.023 Uiso 1 1 calc R . . C9D C -0.2582(2) 0.85556(9) 0.56016(14) 0.0239(6) Uani 1 1 d . . . H9D H -0.2947 0.8335 0.5283 0.029 Uiso 1 1 calc R . . C10D C -0.2340(2) 0.89812(9) 0.53273(14) 0.0259(6) Uani 1 1 d . . . H10D H -0.2546 0.9048 0.4826 0.031 Uiso 1 1 calc R . . C11D C -0.1792(2) 0.93067(9) 0.58031(14) 0.0258(6) Uani 1 1 d . . . H11D H -0.1625 0.9592 0.5620 0.031 Uiso 1 1 calc R . . C12D C -0.1490(2) 0.92096(8) 0.65537(14) 0.0204(5) Uani 1 1 d . . . H12D H -0.1119 0.9430 0.6871 0.024 Uiso 1 1 calc R . . C13D C -0.2601(3) 0.93042(9) 0.82654(14) 0.0282(6) Uani 1 1 d D . . C14D C -0.3812(3) 0.92696(11) 0.83364(16) 0.0403(8) Uani 1 1 d U . . H14D H -0.4156 0.8983 0.8361 0.048 Uiso 1 1 calc R . . C15D C -0.4525(3) 0.96489(12) 0.83722(16) 0.0487(9) Uani 1 1 d U . . H15D H -0.5339 0.9618 0.8421 0.058 Uiso 1 1 calc R . . C16D C -0.4036(4) 1.00652(13) 0.83354(19) 0.0625(11) Uani 1 1 d U . . H16D H -0.4510 1.0322 0.8370 0.075 Uiso 1 1 calc R . . C17D C -0.2877(4) 1.01107(12) 0.8251(2) 0.0764(13) Uani 1 1 d U . . H17D H -0.2553 1.0400 0.8216 0.092 Uiso 1 1 calc R . . C18D C -0.2141(3) 0.97300(11) 0.8213(2) 0.0627(11) Uani 1 1 d DU . . H18D H -0.1333 0.9767 0.8153 0.075 Uiso 1 1 calc R . . N1C N 0.11755(18) 0.87084(7) 0.59178(10) 0.0188(5) Uani 1 1 d . . . C2C C 0.0697(2) 0.83262(8) 0.61437(13) 0.0178(5) Uani 1 1 d . . . H2C H 0.0333 0.8106 0.5825 0.021 Uiso 1 1 calc R . . N3C N 0.08027(16) 0.82998(6) 0.68817(10) 0.0148(4) Uani 1 1 d . . . C4C C 0.1403(2) 0.86930(8) 0.71464(13) 0.0149(5) Uani 1 1 d . . . C5C C 0.1642(2) 0.89486(8) 0.65415(13) 0.0177(5) Uani 1 1 d . . . C6C C 0.1224(2) 0.88364(9) 0.51384(13) 0.0286(6) Uani 1 1 d . . . H6C1 H 0.0895 0.8596 0.4819 0.043 Uiso 1 1 calc R . . H6C2 H 0.2044 0.8889 0.5057 0.043 Uiso 1 1 calc R . . H6C3 H 0.0763 0.9108 0.5029 0.043 Uiso 1 1 calc R . . C7C C 0.1713(2) 0.87897(8) 0.79405(13) 0.0170(5) Uani 1 1 d . . . C8C C 0.2250(2) 0.84596(9) 0.84257(14) 0.0234(6) Uani 1 1 d . . . H8C H 0.2420 0.8174 0.8243 0.028 Uiso 1 1 calc R . . C9C C 0.2532(2) 0.85538(9) 0.91753(14) 0.0303(7) Uani 1 1 d . . . H9C H 0.2890 0.8331 0.9492 0.036 Uiso 1 1 calc R . . C10C C 0.2288(3) 0.89737(10) 0.94571(15) 0.0360(7) Uani 1 1 d . . . H10C H 0.2471 0.9034 0.9963 0.043 Uiso 1 1 calc R . . C11C C 0.1772(3) 0.93034(9) 0.89827(15) 0.0323(7) Uani 1 1 d . . . H11C H 0.1614 0.9588 0.9171 0.039 Uiso 1 1 calc R . . C12C C 0.1483(2) 0.92168(8) 0.82297(14) 0.0251(6) Uani 1 1 d . . . H12C H 0.1135 0.9443 0.7916 0.030 Uiso 1 1 calc R . . C13C C 0.2296(2) 0.93812(8) 0.64962(13) 0.0203(5) Uani 1 1 d . . . C14C C 0.3530(2) 0.93989(9) 0.66544(15) 0.0321(7) Uani 1 1 d . . . H14C H 0.3954 0.9136 0.6801 0.038 Uiso 1 1 calc R . . C15C C 0.4147(3) 0.98029(10) 0.65977(15) 0.0382(8) Uani 1 1 d . . . H15C H 0.4980 0.9810 0.6706 0.046 Uiso 1 1 calc R . . C16C C 0.3529(3) 1.01930(10) 0.63822(16) 0.0373(7) Uani 1 1 d . . . H16C H 0.3943 1.0465 0.6347 0.045 Uiso 1 1 calc R . . C17C C 0.2288(3) 1.01812(9) 0.62172(18) 0.0442(9) Uani 1 1 d . . . H17C H 0.1869 1.0445 0.6069 0.053 Uiso 1 1 calc R . . C18C C 0.1672(3) 0.97748(9) 0.62743(16) 0.0345(7) Uani 1 1 d . . . H18C H 0.0839 0.9767 0.6163 0.041 Uiso 1 1 calc R . . N1 N 0.8826(2) 0.73131(8) 0.02943(13) 0.0299(5) Uani 1 1 d . . . O1 O 0.8584(2) 0.75405(8) -0.02758(13) 0.0627(7) Uani 1 1 d . . . O2 O 0.98953(18) 0.72168(8) 0.05259(11) 0.0462(6) Uani 1 1 d . . . O3 O 0.80054(16) 0.71760(7) 0.06441(10) 0.0383(5) Uani 1 1 d . . . N2 N 0.5094(2) 0.55849(11) 0.7875(2) 0.0543(8) Uani 1 1 d . . . O4 O 0.4976(2) 0.59103(8) 0.74421(17) 0.0855(9) Uani 1 1 d U . . O5 O 0.5103(3) 0.52025(8) 0.75866(16) 0.0876(9) Uani 1 1 d U . . O6 O 0.5193(2) 0.56534(11) 0.85807(17) 0.0946(10) Uani 1 1 d U . . C19 C 0.4962(3) 0.82262(10) 0.72550(18) 0.0478(9) Uani 1 1 d . . . H19A H 0.4164 0.8268 0.7006 0.072 Uiso 1 1 calc R . . H19B H 0.5475 0.8464 0.7111 0.072 Uiso 1 1 calc R . . H19C H 0.4941 0.8236 0.7784 0.072 Uiso 1 1 calc R . . O7 O 0.54102(17) 0.78037(6) 0.70559(10) 0.0326(5) Uani 1 1 d D . . H7 H 0.520(3) 0.7780(10) 0.6604(10) 0.049 Uiso 1 1 d D . . C20 C 0.5827(3) 0.77871(11) 0.9303(2) 0.0527(9) Uani 1 1 d . . . H20A H 0.5108 0.7785 0.8956 0.079 Uiso 1 1 calc R . . H20B H 0.6516 0.7761 0.9036 0.079 Uiso 1 1 calc R . . H20C H 0.5872 0.8066 0.9578 0.079 Uiso 1 1 calc R . . O8 O 0.58033(18) 0.74202(8) 0.97959(12) 0.0480(6) Uani 1 1 d D . . H8 H 0.652(2) 0.7389(12) 1.0015(18) 0.072 Uiso 1 1 d D . . C21 C 0.5020(4) 0.54115(18) 0.5679(3) 0.0728(15) Uani 0.80 1 d PU . . H21A H 0.4467 0.5413 0.5231 0.109 Uiso 0.80 1 calc PR . . H21B H 0.4797 0.5176 0.6004 0.109 Uiso 0.80 1 calc PR . . H21C H 0.5819 0.5356 0.5557 0.109 Uiso 0.80 1 calc PR . . O9 O 0.4986(3) 0.58203(13) 0.60248(18) 0.0717(10) Uani 0.80 1 d PDU . . H9 H 0.501(5) 0.5746(19) 0.6501(10) 0.108 Uiso 0.80 1 d PD . . 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 Ni 0.01394(15) 0.01075(15) 0.01757(16) 0.00177(13) 0.00444(11) 0.00014(14) N1B 0.0105(10) 0.0140(11) 0.0203(11) -0.0017(8) 0.0022(8) -0.0009(8) C2B 0.0167(13) 0.0141(12) 0.0159(12) -0.0008(10) 0.0022(9) -0.0046(10) N3B 0.0142(10) 0.0120(10) 0.0158(10) 0.0015(8) 0.0033(8) -0.0018(8) C4B 0.0152(12) 0.0134(12) 0.0160(12) 0.0030(9) 0.0027(9) -0.0013(10) C5B 0.0149(12) 0.0129(12) 0.0151(12) 0.0003(9) 0.0018(9) -0.0022(10) C6B 0.0116(13) 0.0226(14) 0.0307(15) -0.0049(11) 0.0036(10) 0.0005(10) C7B 0.0134(12) 0.0170(13) 0.0173(12) -0.0023(10) 0.0030(9) -0.0005(10) C8B 0.0185(13) 0.0172(14) 0.0210(13) -0.0006(10) 0.0022(10) 0.0002(10) C9B 0.0201(14) 0.0330(16) 0.0217(14) -0.0034(12) -0.0016(10) 0.0054(12) C10B 0.0119(13) 0.0433(18) 0.0238(14) -0.0102(12) 0.0011(10) -0.0037(12) C11B 0.0214(14) 0.0288(16) 0.0271(15) -0.0068(12) 0.0075(11) -0.0099(12) C12B 0.0182(13) 0.0194(14) 0.0224(14) -0.0019(11) 0.0024(10) -0.0034(10) C13B 0.0156(13) 0.0148(13) 0.0247(14) -0.0035(10) 0.0068(10) -0.0030(10) C14B 0.0238(14) 0.0229(14) 0.0252(15) -0.0043(11) 0.0077(11) -0.0047(11) C15B 0.0316(17) 0.0330(17) 0.0362(17) -0.0153(13) 0.0091(13) -0.0143(14) C16B 0.0363(18) 0.0183(15) 0.061(2) -0.0169(14) 0.0176(16) -0.0067(13) C17B 0.0303(17) 0.0167(15) 0.063(2) -0.0048(14) 0.0050(15) 0.0021(12) C18B 0.0197(14) 0.0199(15) 0.0404(17) -0.0041(12) 0.0000(12) 0.0006(11) N1A 0.0110(10) 0.0147(11) 0.0207(11) 0.0017(8) 0.0026(8) -0.0012(8) C2A 0.0148(13) 0.0167(13) 0.0176(13) 0.0029(10) 0.0018(10) 0.0011(10) N3A 0.0126(10) 0.0104(10) 0.0174(11) 0.0013(8) 0.0037(8) 0.0005(8) C4A 0.0119(12) 0.0127(12) 0.0158(12) 0.0011(9) 0.0023(9) 0.0006(9) C5A 0.0150(12) 0.0131(12) 0.0175(12) 0.0025(9) 0.0017(9) 0.0018(10) C6A 0.0106(13) 0.0273(15) 0.0342(16) 0.0073(12) 0.0040(11) -0.0013(11) C7A 0.0148(12) 0.0154(13) 0.0158(12) 0.0052(10) 0.0024(9) -0.0008(10) C8A 0.0180(13) 0.0192(14) 0.0200(13) 0.0039(10) 0.0017(10) 0.0021(10) C9A 0.0187(14) 0.0307(16) 0.0227(14) 0.0033(11) -0.0001(10) -0.0057(11) C10A 0.0117(13) 0.0391(17) 0.0224(14) 0.0086(12) 0.0025(10) 0.0011(12) C11A 0.0214(14) 0.0263(15) 0.0246(14) 0.0082(11) 0.0078(11) 0.0079(11) C12A 0.0187(13) 0.0146(13) 0.0238(14) 0.0033(10) 0.0044(10) 0.0009(10) C13A 0.0134(12) 0.0144(13) 0.0241(14) 0.0037(10) 0.0066(10) -0.0004(10) C14A 0.0169(13) 0.0200(14) 0.0273(15) 0.0052(11) 0.0052(10) 0.0009(10) C15A 0.0211(14) 0.0297(16) 0.0346(16) 0.0137(12) 0.0033(12) 0.0058(12) C16A 0.0244(15) 0.0196(15) 0.0499(19) 0.0166(13) 0.0098(13) 0.0032(12) C17A 0.0260(15) 0.0163(15) 0.0461(18) 0.0031(12) 0.0076(13) -0.0021(11) C18A 0.0200(14) 0.0184(14) 0.0336(16) 0.0032(11) 0.0072(11) -0.0006(11) N1D 0.0332(13) 0.0254(13) 0.0163(11) 0.0044(9) 0.0106(9) 0.0112(10) C2D 0.0230(14) 0.0217(14) 0.0216(14) 0.0055(11) 0.0064(11) 0.0074(11) N3D 0.0162(11) 0.0144(11) 0.0192(11) 0.0032(8) 0.0044(8) 0.0009(8) C4D 0.0163(13) 0.0111(12) 0.0189(13) 0.0002(9) 0.0027(9) -0.0003(10) C5D 0.0258(14) 0.0196(14) 0.0200(14) 0.0020(10) 0.0076(11) 0.0069(11) C6D 0.069(2) 0.048(2) 0.0195(15) 0.0034(14) 0.0155(15) 0.0280(17) C7D 0.0138(12) 0.0153(13) 0.0187(13) 0.0009(10) 0.0037(9) 0.0035(10) C8D 0.0204(14) 0.0150(13) 0.0222(14) 0.0011(10) 0.0043(10) 0.0020(10) C9D 0.0230(14) 0.0221(15) 0.0260(15) -0.0048(11) 0.0002(11) 0.0023(11) C10D 0.0281(15) 0.0303(16) 0.0183(14) 0.0038(12) -0.0013(11) 0.0064(12) C11D 0.0309(15) 0.0212(15) 0.0255(15) 0.0071(11) 0.0043(11) 0.0030(12) C12D 0.0218(14) 0.0147(13) 0.0242(14) 0.0015(10) 0.0009(10) 0.0007(11) C13D 0.0442(18) 0.0228(15) 0.0199(14) 0.0036(11) 0.0140(12) 0.0123(13) C14D 0.0386(17) 0.0429(18) 0.0368(17) -0.0129(14) -0.0063(13) 0.0211(14) C15D 0.050(2) 0.064(2) 0.0309(17) -0.0058(16) 0.0005(14) 0.0306(18) C16D 0.082(3) 0.057(2) 0.056(2) 0.0200(18) 0.039(2) 0.041(2) C17D 0.094(3) 0.034(2) 0.111(3) 0.009(2) 0.052(2) 0.014(2) C18D 0.068(2) 0.037(2) 0.092(3) 0.0010(18) 0.047(2) 0.0096(17) N1C 0.0248(12) 0.0163(11) 0.0163(11) 0.0007(8) 0.0065(9) -0.0062(9) C2C 0.0184(13) 0.0138(13) 0.0220(14) -0.0010(10) 0.0054(10) -0.0023(10) N3C 0.0150(11) 0.0133(11) 0.0165(11) 0.0002(8) 0.0029(8) -0.0011(8) C4C 0.0147(12) 0.0112(12) 0.0192(13) 0.0012(10) 0.0036(9) -0.0001(9) C5C 0.0189(13) 0.0151(13) 0.0195(13) -0.0016(10) 0.0046(10) -0.0018(10) C6C 0.0394(17) 0.0298(16) 0.0180(14) 0.0016(11) 0.0087(12) -0.0115(13) C7C 0.0176(13) 0.0147(13) 0.0191(13) 0.0019(10) 0.0040(10) -0.0051(10) C8C 0.0249(15) 0.0194(14) 0.0257(15) 0.0035(11) 0.0018(11) -0.0025(11) C9C 0.0359(17) 0.0319(17) 0.0216(15) 0.0087(12) -0.0031(12) -0.0061(13) C10C 0.054(2) 0.0364(18) 0.0171(15) -0.0018(13) 0.0042(13) -0.0170(15) C11C 0.0536(19) 0.0184(15) 0.0262(16) -0.0047(12) 0.0106(13) -0.0086(13) C12C 0.0346(16) 0.0159(14) 0.0253(15) 0.0027(11) 0.0055(12) -0.0038(12) C13C 0.0302(15) 0.0153(13) 0.0168(13) 0.0010(10) 0.0085(11) -0.0057(11) C14C 0.0345(17) 0.0252(16) 0.0335(17) 0.0118(12) -0.0088(12) -0.0098(13) C15C 0.0390(18) 0.0398(19) 0.0334(17) 0.0088(14) -0.0061(13) -0.0194(15) C16C 0.056(2) 0.0206(16) 0.0375(18) -0.0054(13) 0.0164(15) -0.0191(14) C17C 0.056(2) 0.0167(16) 0.066(2) 0.0077(14) 0.0333(18) -0.0005(14) C18C 0.0338(17) 0.0190(15) 0.054(2) 0.0053(13) 0.0188(14) -0.0028(12) N1 0.0363(15) 0.0284(13) 0.0266(13) -0.0078(10) 0.0097(11) -0.0069(11) O1 0.0794(18) 0.0666(18) 0.0451(15) 0.0274(13) 0.0201(13) 0.0015(14) O2 0.0239(11) 0.0762(17) 0.0385(12) -0.0175(11) 0.0031(9) -0.0136(11) O3 0.0234(11) 0.0596(14) 0.0335(11) 0.0096(10) 0.0099(8) -0.0059(10) N2 0.0253(15) 0.056(2) 0.082(2) -0.0047(18) 0.0090(15) -0.0042(14) O4 0.0862(18) 0.0315(13) 0.124(2) 0.0228(14) -0.0486(16) -0.0002(13) O5 0.129(2) 0.0308(13) 0.118(2) -0.0069(13) 0.0787(17) 0.0080(14) O6 0.0569(19) 0.151(3) 0.077(2) -0.026(2) 0.0136(16) -0.0338(18) C19 0.052(2) 0.0289(18) 0.065(2) -0.0068(16) 0.0169(18) 0.0016(16) O7 0.0359(11) 0.0222(11) 0.0376(11) 0.0005(9) -0.0044(9) 0.0008(9) C20 0.044(2) 0.043(2) 0.072(3) -0.0065(18) 0.0101(18) -0.0029(17) O8 0.0307(12) 0.0707(17) 0.0418(14) 0.0071(12) 0.0003(10) -0.0100(12) C21 0.069(3) 0.087(3) 0.065(3) 0.019(3) 0.018(2) 0.013(3) O9 0.059(2) 0.084(3) 0.067(2) 0.003(2) -0.0097(18) -0.0295(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3D 1.8960(19) . ? Ni N3C 1.8970(18) . ? Ni N3A 1.9003(18) . ? Ni N3B 1.9015(18) . ? N1B C2B 1.333(3) . ? N1B C5B 1.385(3) . ? N1B C6B 1.463(3) . ? C2B N3B 1.329(3) . ? C2B H2B 0.9300 . ? N3B C4B 1.388(3) . ? C4B C5B 1.374(3) . ? C4B C7B 1.470(3) . ? C5B C13B 1.473(3) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B C8B 1.393(3) . ? C7B C12B 1.396(3) . ? C8B C9B 1.384(3) . ? C8B H8B 0.9300 . ? C9B C10B 1.382(3) . ? C9B H9B 0.9300 . ? C10B C11B 1.383(4) . ? C10B H10B 0.9300 . ? C11B C12B 1.386(3) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.390(3) . ? C13B C18B 1.394(3) . ? C14B C15B 1.384(3) . ? C14B H14B 0.9300 . ? C15B C16B 1.368(4) . ? C15B H15B 0.9300 . ? C16B C17B 1.373(4) . ? C16B H16B 0.9300 . ? C17B C18B 1.389(3) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? N1A C2A 1.332(3) . ? N1A C5A 1.387(3) . ? N1A C6A 1.464(3) . ? C2A N3A 1.329(3) . ? C2A H2A 0.9300 . ? N3A C4A 1.389(3) . ? C4A C5A 1.376(3) . ? C4A C7A 1.468(3) . ? C5A C13A 1.478(3) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C8A 1.394(3) . ? C7A C12A 1.400(3) . ? C8A C9A 1.385(3) . ? C8A H8A 0.9300 . ? C9A C10A 1.381(3) . ? C9A H9A 0.9300 . ? C10A C11A 1.389(4) . ? C10A H10A 0.9300 . ? C11A C12A 1.387(3) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C14A 1.387(3) . ? C13A C18A 1.392(3) . ? C14A C15A 1.393(3) . ? C14A H14A 0.9300 . ? C15A C16A 1.385(4) . ? C15A H15A 0.9300 . ? C16A C17A 1.376(4) . ? C16A H16A 0.9300 . ? C17A C18A 1.392(3) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? N1D C2D 1.331(3) . ? N1D C5D 1.389(3) . ? N1D C6D 1.465(3) . ? C2D N3D 1.325(3) . ? C2D H2D 0.9300 . ? N3D C4D 1.390(3) . ? C4D C5D 1.372(3) . ? C4D C7D 1.473(3) . ? C5D C13D 1.473(3) . ? C6D H6D1 0.9600 . ? C6D H6D2 0.9600 . ? C6D H6D3 0.9600 . ? C7D C12D 1.394(3) . ? C7D C8D 1.395(3) . ? C8D C9D 1.372(3) . ? C8D H8D 0.9300 . ? C9D C10D 1.386(3) . ? C9D H9D 0.9300 . ? C10D C11D 1.382(4) . ? C10D H10D 0.9300 . ? C11D C12D 1.389(3) . ? C11D H11D 0.9300 . ? C12D H12D 0.9300 . ? C13D C18D 1.363(3) . ? C13D C14D 1.381(4) . ? C14D C15D 1.379(4) . ? C14D H14D 0.9300 . ? C15D C16D 1.347(5) . ? C15D H15D 0.9300 . ? C16D C17D 1.331(5) . ? C16D H16D 0.9300 . ? C17D C18D 1.398(4) . ? C17D H17D 0.9300 . ? C18D H18D 0.9300 . ? N1C C2C 1.331(3) . ? N1C C5C 1.381(3) . ? N1C C6C 1.466(3) . ? C2C N3C 1.328(3) . ? C2C H2C 0.9300 . ? N3C C4C 1.395(3) . ? C4C C5C 1.379(3) . ? C4C C7C 1.465(3) . ? C5C C13C 1.476(3) . ? C6C H6C1 0.9600 . ? C6C H6C2 0.9600 . ? C6C H6C3 0.9600 . ? C7C C8C 1.397(3) . ? C7C C12C 1.398(3) . ? C8C C9C 1.383(3) . ? C8C H8C 0.9300 . ? C9C C10C 1.377(4) . ? C9C H9C 0.9300 . ? C10C C11C 1.377(4) . ? C10C H10C 0.9300 . ? C11C C12C 1.386(3) . ? C11C H11C 0.9300 . ? C12C H12C 0.9300 . ? C13C C14C 1.378(3) . ? C13C C18C 1.388(3) . ? C14C C15C 1.386(4) . ? C14C H14C 0.9300 . ? C15C C16C 1.373(4) . ? C15C H15C 0.9300 . ? C16C C17C 1.387(4) . ? C16C H16C 0.9300 . ? C17C C18C 1.392(4) . ? C17C H17C 0.9300 . ? C18C H18C 0.9300 . ? N1 O1 1.232(3) . ? N1 O3 1.242(3) . ? N1 O2 1.254(3) . ? N2 O4 1.234(4) . ? N2 O5 1.241(3) . ? N2 O6 1.284(4) . ? C19 O7 1.404(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? O7 H7 0.826(18) . ? C20 O8 1.403(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O8 H8 0.853(19) . ? C21 O9 1.359(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O9 H9 0.886(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3D Ni N3C 91.82(8) . . ? N3D Ni N3A 88.61(8) . . ? N3C Ni N3A 179.28(8) . . ? N3D Ni N3B 178.79(8) . . ? N3C Ni N3B 89.31(7) . . ? N3A Ni N3B 90.26(7) . . ? C2B N1B C5B 108.01(18) . . ? C2B N1B C6B 124.12(19) . . ? C5B N1B C6B 127.73(19) . . ? N3B C2B N1B 111.4(2) . . ? N3B C2B H2B 124.3 . . ? N1B C2B H2B 124.3 . . ? C2B N3B C4B 105.98(18) . . ? C2B N3B Ni 123.58(16) . . ? C4B N3B Ni 128.78(15) . . ? C5B C4B N3B 108.9(2) . . ? C5B C4B C7B 129.3(2) . . ? N3B C4B C7B 121.8(2) . . ? C4B C5B N1B 105.72(19) . . ? C4B C5B C13B 130.0(2) . . ? N1B C5B C13B 124.3(2) . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C8B C7B C12B 119.0(2) . . ? C8B C7B C4B 119.7(2) . . ? C12B C7B C4B 121.4(2) . . ? C9B C8B C7B 120.8(2) . . ? C9B C8B H8B 119.6 . . ? C7B C8B H8B 119.6 . . ? C10B C9B C8B 119.8(2) . . ? C10B C9B H9B 120.1 . . ? C8B C9B H9B 120.1 . . ? C9B C10B C11B 120.0(2) . . ? C9B C10B H10B 120.0 . . ? C11B C10B H10B 120.0 . . ? C10B C11B C12B 120.5(2) . . ? C10B C11B H11B 119.8 . . ? C12B C11B H11B 119.8 . . ? C11B C12B C7B 119.9(2) . . ? C11B C12B H12B 120.1 . . ? C7B C12B H12B 120.1 . . ? C14B C13B C18B 118.9(2) . . ? C14B C13B C5B 120.2(2) . . ? C18B C13B C5B 120.9(2) . . ? C15B C14B C13B 120.4(3) . . ? C15B C14B H14B 119.8 . . ? C13B C14B H14B 119.8 . . ? C16B C15B C14B 120.3(3) . . ? C16B C15B H15B 119.8 . . ? C14B C15B H15B 119.8 . . ? C15B C16B C17B 120.1(3) . . ? C15B C16B H16B 119.9 . . ? C17B C16B H16B 119.9 . . ? C16B C17B C18B 120.4(3) . . ? C16B C17B H17B 119.8 . . ? C18B C17B H17B 119.8 . . ? C17B C18B C13B 119.8(3) . . ? C17B C18B H18B 120.1 . . ? C13B C18B H18B 120.1 . . ? C2A N1A C5A 108.08(18) . . ? C2A N1A C6A 124.1(2) . . ? C5A N1A C6A 127.62(19) . . ? N3A C2A N1A 111.2(2) . . ? N3A C2A H2A 124.4 . . ? N1A C2A H2A 124.4 . . ? C2A N3A C4A 106.36(18) . . ? C2A N3A Ni 122.95(16) . . ? C4A N3A Ni 129.65(15) . . ? C5A C4A N3A 108.56(19) . . ? C5A C4A C7A 129.0(2) . . ? N3A C4A C7A 122.35(19) . . ? C4A C5A N1A 105.80(19) . . ? C4A C5A C13A 130.1(2) . . ? N1A C5A C13A 124.1(2) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A C12A 118.6(2) . . ? C8A C7A C4A 120.1(2) . . ? C12A C7A C4A 121.3(2) . . ? C9A C8A C7A 120.8(2) . . ? C9A C8A H8A 119.6 . . ? C7A C8A H8A 119.6 . . ? C10A C9A C8A 120.1(2) . . ? C10A C9A H9A 119.9 . . ? C8A C9A H9A 119.9 . . ? C9A C10A C11A 120.0(2) . . ? C9A C10A H10A 120.0 . . ? C11A C10A H10A 120.0 . . ? C12A C11A C10A 120.0(2) . . ? C12A C11A H11A 120.0 . . ? C10A C11A H11A 120.0 . . ? C11A C12A C7A 120.5(2) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C14A C13A C18A 119.0(2) . . ? C14A C13A C5A 119.9(2) . . ? C18A C13A C5A 121.1(2) . . ? C13A C14A C15A 120.6(2) . . ? C13A C14A H14A 119.7 . . ? C15A C14A H14A 119.7 . . ? C16A C15A C14A 119.6(3) . . ? C16A C15A H15A 120.2 . . ? C14A C15A H15A 120.2 . . ? C17A C16A C15A 120.5(2) . . ? C17A C16A H16A 119.8 . . ? C15A C16A H16A 119.8 . . ? C16A C17A C18A 119.8(3) . . ? C16A C17A H17A 120.1 . . ? C18A C17A H17A 120.1 . . ? C13A C18A C17A 120.5(3) . . ? C13A C18A H18A 119.8 . . ? C17A C18A H18A 119.8 . . ? C2D N1D C5D 108.10(19) . . ? C2D N1D C6D 124.7(2) . . ? C5D N1D C6D 127.2(2) . . ? N3D C2D N1D 111.2(2) . . ? N3D C2D H2D 124.4 . . ? N1D C2D H2D 124.4 . . ? C2D N3D C4D 106.38(19) . . ? C2D N3D Ni 122.02(16) . . ? C4D N3D Ni 131.51(15) . . ? C5D C4D N3D 108.6(2) . . ? C5D C4D C7D 128.1(2) . . ? N3D C4D C7D 123.14(19) . . ? C4D C5D N1D 105.7(2) . . ? C4D C5D C13D 131.4(2) . . ? N1D C5D C13D 122.7(2) . . ? N1D C6D H6D1 109.5 . . ? N1D C6D H6D2 109.5 . . ? H6D1 C6D H6D2 109.5 . . ? N1D C6D H6D3 109.5 . . ? H6D1 C6D H6D3 109.5 . . ? H6D2 C6D H6D3 109.5 . . ? C12D C7D C8D 118.7(2) . . ? C12D C7D C4D 121.3(2) . . ? C8D C7D C4D 120.0(2) . . ? C9D C8D C7D 121.0(2) . . ? C9D C8D H8D 119.5 . . ? C7D C8D H8D 119.5 . . ? C8D C9D C10D 120.2(2) . . ? C8D C9D H9D 119.9 . . ? C10D C9D H9D 119.9 . . ? C11D C10D C9D 119.7(2) . . ? C11D C10D H10D 120.2 . . ? C9D C10D H10D 120.2 . . ? C10D C11D C12D 120.3(2) . . ? C10D C11D H11D 119.8 . . ? C12D C11D H11D 119.8 . . ? C11D C12D C7D 120.2(2) . . ? C11D C12D H12D 119.9 . . ? C7D C12D H12D 119.9 . . ? C18D C13D C14D 117.2(3) . . ? C18D C13D C5D 120.9(3) . . ? C14D C13D C5D 121.8(2) . . ? C15D C14D C13D 121.7(3) . . ? C15D C14D H14D 119.2 . . ? C13D C14D H14D 119.2 . . ? C16D C15D C14D 119.6(3) . . ? C16D C15D H15D 120.2 . . ? C14D C15D H15D 120.2 . . ? C17D C16D C15D 120.3(3) . . ? C17D C16D H16D 119.8 . . ? C15D C16D H16D 119.8 . . ? C16D C17D C18D 120.9(4) . . ? C16D C17D H17D 119.6 . . ? C18D C17D H17D 119.6 . . ? C13D C18D C17D 120.3(3) . . ? C13D C18D H18D 119.8 . . ? C17D C18D H18D 119.8 . . ? C2C N1C C5C 108.03(19) . . ? C2C N1C C6C 125.0(2) . . ? C5C N1C C6C 126.9(2) . . ? N3C C2C N1C 111.5(2) . . ? N3C C2C H2C 124.3 . . ? N1C C2C H2C 124.3 . . ? C2C N3C C4C 106.18(18) . . ? C2C N3C Ni 122.46(16) . . ? C4C N3C Ni 130.57(15) . . ? C5C C4C N3C 108.1(2) . . ? C5C C4C C7C 128.7(2) . . ? N3C C4C C7C 123.14(19) . . ? C4C C5C N1C 106.2(2) . . ? C4C C5C C13C 131.2(2) . . ? N1C C5C C13C 122.6(2) . . ? N1C C6C H6C1 109.5 . . ? N1C C6C H6C2 109.5 . . ? H6C1 C6C H6C2 109.5 . . ? N1C C6C H6C3 109.5 . . ? H6C1 C6C H6C3 109.5 . . ? H6C2 C6C H6C3 109.5 . . ? C8C C7C C12C 118.4(2) . . ? C8C C7C C4C 121.0(2) . . ? C12C C7C C4C 120.6(2) . . ? C9C C8C C7C 120.5(2) . . ? C9C C8C H8C 119.8 . . ? C7C C8C H8C 119.8 . . ? C10C C9C C8C 120.7(3) . . ? C10C C9C H9C 119.6 . . ? C8C C9C H9C 119.6 . . ? C11C C10C C9C 119.3(3) . . ? C11C C10C H10C 120.3 . . ? C9C C10C H10C 120.3 . . ? C10C C11C C12C 121.0(3) . . ? C10C C11C H11C 119.5 . . ? C12C C11C H11C 119.5 . . ? C11C C12C C7C 120.1(2) . . ? C11C C12C H12C 120.0 . . ? C7C C12C H12C 120.0 . . ? C14C C13C C18C 119.1(2) . . ? C14C C13C C5C 120.9(2) . . ? C18C C13C C5C 120.0(2) . . ? C13C C14C C15C 120.9(3) . . ? C13C C14C H14C 119.5 . . ? C15C C14C H14C 119.5 . . ? C16C C15C C14C 120.0(3) . . ? C16C C15C H15C 120.0 . . ? C14C C15C H15C 120.0 . . ? C15C C16C C17C 119.9(3) . . ? C15C C16C H16C 120.0 . . ? C17C C16C H16C 120.0 . . ? C16C C17C C18C 119.9(3) . . ? C16C C17C H17C 120.0 . . ? C18C C17C H17C 120.0 . . ? C13C C18C C17C 120.1(3) . . ? C13C C18C H18C 119.9 . . ? C17C C18C H18C 119.9 . . ? O1 N1 O3 120.0(3) . . ? O1 N1 O2 120.6(2) . . ? O3 N1 O2 119.4(2) . . ? O4 N2 O5 116.3(3) . . ? O4 N2 O6 119.9(3) . . ? O5 N2 O6 123.8(4) . . ? O7 C19 H19A 109.5 . . ? O7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 O7 H7 105(2) . . ? O8 C20 H20A 109.5 . . ? O8 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O8 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C20 O8 H8 107(2) . . ? O9 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O9 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 O9 H9 103(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.788 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.066 # start Validation Reply Form _vrf_PLAT220_4-NiL4_{NO3}2_2.8MeOH ; RESPONSE: This is due to the high thermal motion of most of the atoms of the phenyl ring C13C to C18C. ; _vrf_PLAT222_4-NiL4_{NO3}2_2.8MeOH ; RESPONSE: As above. ; _vrf_PLAT331_4-NiL4_{NO3}2_2.8MeOH ; RESPONSE: The average ring distance is smaller due to the large thermal motion of the phenyl ring C13C to C18C. ; # end Validation Reply Form #===END data_5-NiL4_{ClO4}2_Me2CO #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881066' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 N8 Ni, 2(Cl O4), C3 H6 O' _chemical_formula_sum 'C67 H62 Cl2 N8 Ni O9' _chemical_formula_weight 1252.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.7034(5) _cell_length_b 11.7726(3) _cell_length_c 22.0772(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6160.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5757 _cell_measurement_theta_min 3.7265 _cell_measurement_theta_max 71.8560 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9097 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14444 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 69.99 _reflns_number_total 8850 _reflns_number_gt 8076 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; One (of the two) perchlorate counterion of the structure is severely disordered. Persistent attempts to model disorder with a chemically reasonable geometry (using several diffraction data collected at 100 K with MoKa and CuKa radiation) were unsuccessful. Therefore, the SQUEEZE procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001) was employed to remove the contribution of the electron density associated with this ion from the intensity data. The solvent-free model and intensity data were used for the final results reported here. The atoms of the perchlorate ion removed have been included in the sum and moiety formula, and the Mr, Dx, Mu and F(000) have been modified accordingly. Examination and statistical analysis of the difraction data used show that the crystal structure is truly non-centrosymmetric and that the space group is Pna2(1) as clearly deduced from the systematic absences. Furthermore, the refined Flack parameter of 0.51(2) indicates that the macroscopic crystal used is twinning by inversion in a ratio of approximately 51:49. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+0.8104P] 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, 2886 Friedel pairs' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 8850 _refine_ls_number_parameters 746 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.056 _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 Ni Ni 0.254247(19) 0.00489(4) 0.20648(4) 0.01722(16) Uani 1 1 d . . . N1A N 0.15680(12) -0.1278(2) 0.07805(14) 0.0199(6) Uani 1 1 d . . . C2A C 0.20571(13) -0.1024(3) 0.10402(17) 0.0214(7) Uani 1 1 d . . . H2A H 0.2398 -0.1376 0.0950 0.026 Uiso 1 1 calc R . . N3A N 0.19960(11) -0.0196(3) 0.14482(14) 0.0187(6) Uani 1 1 d . . . C4A C 0.14262(14) 0.0082(3) 0.14523(18) 0.0202(7) Uani 1 1 d . . . C5A C 0.11534(13) -0.0576(3) 0.10365(16) 0.0195(7) Uani 1 1 d . . . C6A C 0.14864(15) -0.2143(3) 0.03057(18) 0.0276(8) Uani 1 1 d . . . H6A1 H 0.1579 -0.1823 -0.0082 0.041 Uiso 1 1 calc R . . H6A2 H 0.1100 -0.2386 0.0305 0.041 Uiso 1 1 calc R . . H6A3 H 0.1727 -0.2781 0.0385 0.041 Uiso 1 1 calc R . . C7A C 0.12022(14) 0.0996(3) 0.18384(17) 0.0217(7) Uani 1 1 d . . . C8A C 0.14874(15) 0.2024(3) 0.18894(18) 0.0271(8) Uani 1 1 d . . . H8A H 0.1812 0.2147 0.1661 0.032 Uiso 1 1 calc R . . C9A C 0.12945(18) 0.2874(4) 0.2277(2) 0.0363(9) Uani 1 1 d . . . H9A H 0.1488 0.3559 0.2305 0.044 Uiso 1 1 calc R . . C10A C 0.08136(18) 0.2694(4) 0.2619(2) 0.0390(10) Uani 1 1 d . . . H10A H 0.0690 0.3253 0.2885 0.047 Uiso 1 1 calc R . . C11A C 0.05132(16) 0.1678(4) 0.2567(2) 0.0344(9) Uani 1 1 d . . . H11A H 0.0186 0.1567 0.2792 0.041 Uiso 1 1 calc R . . C12A C 0.07076(15) 0.0832(3) 0.21775(18) 0.0277(8) Uani 1 1 d . . . H12A H 0.0508 0.0154 0.2142 0.033 Uiso 1 1 calc R . . C13A C 0.05521(13) -0.0624(3) 0.08547(17) 0.0200(7) Uani 1 1 d . . . C14A C 0.03118(15) 0.0299(3) 0.05441(19) 0.0265(8) Uani 1 1 d . . . H14A H 0.0537 0.0906 0.0425 0.032 Uiso 1 1 calc R . . C15A C -0.02636(16) 0.0304(4) 0.0415(2) 0.0325(9) Uani 1 1 d . . . H15A H -0.0424 0.0926 0.0220 0.039 Uiso 1 1 calc R . . C16A C -0.05950(14) -0.0608(3) 0.05735(19) 0.0280(8) Uani 1 1 d . . . H16A H -0.0977 -0.0606 0.0478 0.034 Uiso 1 1 calc R . . C17A C -0.03622(15) -0.1534(4) 0.08753(19) 0.0306(8) Uani 1 1 d . . . H17A H -0.0588 -0.2147 0.0983 0.037 Uiso 1 1 calc R . . C18A C 0.02082(15) -0.1537(3) 0.10150(19) 0.0284(8) Uani 1 1 d . . . H18A H 0.0363 -0.2155 0.1218 0.034 Uiso 1 1 calc R . . N1B N 0.35443(11) 0.1470(3) 0.08213(15) 0.0230(6) Uani 1 1 d . . . C2B C 0.30450(14) 0.1216(3) 0.10802(17) 0.0224(7) Uani 1 1 d . . . H2B H 0.2707 0.1583 0.0995 0.027 Uiso 1 1 calc R . . N3B N 0.31020(12) 0.0368(3) 0.14750(14) 0.0210(6) Uani 1 1 d . . . C4B C 0.36700(14) 0.0056(3) 0.14626(17) 0.0205(7) Uani 1 1 d . . . C5B C 0.39411(14) 0.0743(3) 0.10524(17) 0.0215(7) Uani 1 1 d . . . C6B C 0.36266(15) 0.2362(3) 0.03617(19) 0.0276(8) Uani 1 1 d . . . H6B1 H 0.3513 0.2081 -0.0028 0.041 Uiso 1 1 calc R . . H6B2 H 0.4018 0.2573 0.0348 0.041 Uiso 1 1 calc R . . H6B3 H 0.3403 0.3014 0.0465 0.041 Uiso 1 1 calc R . . C7B C 0.39059(14) -0.0864(3) 0.18377(17) 0.0237(7) Uani 1 1 d . . . C8B C 0.36316(15) -0.1914(3) 0.18754(18) 0.0267(7) Uani 1 1 d . . . H8B H 0.3309 -0.2044 0.1645 0.032 Uiso 1 1 calc R . . C9B C 0.38351(18) -0.2762(4) 0.2252(2) 0.0353(9) Uani 1 1 d . . . H9B H 0.3648 -0.3455 0.2277 0.042 Uiso 1 1 calc R . . C10B C 0.43219(18) -0.2572(4) 0.25933(19) 0.0373(10) Uani 1 1 d . . . H10B H 0.4456 -0.3135 0.2852 0.045 Uiso 1 1 calc R . . C11B C 0.46042(16) -0.1554(4) 0.2548(2) 0.0360(9) Uani 1 1 d . . . H11B H 0.4934 -0.1438 0.2767 0.043 Uiso 1 1 calc R . . C12B C 0.43966(15) -0.0692(3) 0.21723(18) 0.0281(8) Uani 1 1 d . . . H12B H 0.4587 -0.0003 0.2146 0.034 Uiso 1 1 calc R . . C13B C 0.45415(13) 0.0718(3) 0.08572(17) 0.0224(7) Uani 1 1 d . . . C14B C 0.47515(15) -0.0263(3) 0.05702(19) 0.0267(8) Uani 1 1 d . . . H14B H 0.4511 -0.0864 0.0479 0.032 Uiso 1 1 calc R . . C15B C 0.53246(16) -0.0324(3) 0.0425(2) 0.0300(8) Uani 1 1 d . . . H15B H 0.5467 -0.0975 0.0241 0.036 Uiso 1 1 calc R . . C16B C 0.56805(15) 0.0570(4) 0.05505(18) 0.0289(8) Uani 1 1 d . . . H16B H 0.6060 0.0523 0.0447 0.035 Uiso 1 1 calc R . . C17B C 0.54794(16) 0.1532(4) 0.0828(2) 0.0321(8) Uani 1 1 d . . . H17B H 0.5723 0.2127 0.0918 0.039 Uiso 1 1 calc R . . C18B C 0.49006(15) 0.1617(3) 0.0979(2) 0.0308(8) Uani 1 1 d . . . H18B H 0.4762 0.2274 0.1159 0.037 Uiso 1 1 calc R . . N1C N 0.35991(13) -0.0119(3) 0.34786(15) 0.0237(6) Uani 1 1 d . . . C2C C 0.31820(13) -0.0469(3) 0.31121(18) 0.0213(7) Uani 1 1 d . . . H2C H 0.2996 -0.1162 0.3146 0.026 Uiso 1 1 calc R . . N3C N 0.30721(12) 0.0319(3) 0.26918(15) 0.0205(6) Uani 1 1 d . . . C4C C 0.34415(14) 0.1213(3) 0.27924(18) 0.0233(7) Uani 1 1 d . . . C5C C 0.37715(15) 0.0946(3) 0.32879(17) 0.0262(8) Uani 1 1 d . . . C6C C 0.38135(17) -0.0782(4) 0.3993(2) 0.0365(9) Uani 1 1 d . . . H6C1 H 0.3523 -0.1282 0.4137 0.055 Uiso 1 1 calc R . . H6C2 H 0.3924 -0.0276 0.4313 0.055 Uiso 1 1 calc R . . H6C3 H 0.4133 -0.1222 0.3866 0.055 Uiso 1 1 calc R . . C7C C 0.34447(15) 0.2253(3) 0.24315(18) 0.0256(7) Uani 1 1 d . . . C8C C 0.29392(15) 0.2799(3) 0.2293(2) 0.0332(9) Uani 1 1 d . . . H8C H 0.2601 0.2507 0.2439 0.040 Uiso 1 1 calc R . . C9C C 0.29364(17) 0.3769(3) 0.1941(2) 0.0364(10) Uani 1 1 d . . . H9C H 0.2596 0.4118 0.1844 0.044 Uiso 1 1 calc R . . C10C C 0.34438(18) 0.4227(3) 0.1731(2) 0.0340(9) Uani 1 1 d . . . H10C H 0.3440 0.4872 0.1487 0.041 Uiso 1 1 calc R . . C11C C 0.39470(17) 0.3725(3) 0.1882(2) 0.0319(8) Uani 1 1 d . . . H11C H 0.4285 0.4044 0.1754 0.038 Uiso 1 1 calc R . . C12C C 0.39493(15) 0.2736(3) 0.22295(17) 0.0263(7) Uani 1 1 d . . . H12C H 0.4291 0.2394 0.2328 0.032 Uiso 1 1 calc R . . C13C C 0.41987(17) 0.1641(5) 0.36078(19) 0.0371(10) Uani 1 1 d . . . C14C C 0.4051(2) 0.2770(5) 0.3760(2) 0.0481(12) Uani 1 1 d U . . H14C H 0.3702 0.3062 0.3649 0.058 Uiso 1 1 calc R . . C15C C 0.4436(2) 0.3443(6) 0.4077(3) 0.0599(16) Uani 1 1 d U . . H15C H 0.4348 0.4191 0.4174 0.072 Uiso 1 1 calc R . . C16C C 0.4949(3) 0.2978(7) 0.4243(2) 0.071(2) Uani 1 1 d U . . H16C H 0.5198 0.3420 0.4467 0.085 Uiso 1 1 calc R . . C17C C 0.5105(2) 0.1885(7) 0.4090(3) 0.0649(17) Uani 1 1 d U . . H17C H 0.5457 0.1608 0.4203 0.078 Uiso 1 1 calc R . . C18C C 0.4722(2) 0.1181(6) 0.3758(2) 0.0504(13) Uani 1 1 d U . . H18C H 0.4819 0.0445 0.3646 0.060 Uiso 1 1 calc R . . N1D N 0.15033(13) -0.0024(3) 0.34933(16) 0.0258(7) Uani 1 1 d . . . C2D C 0.18974(14) 0.0397(3) 0.31304(17) 0.0216(7) Uani 1 1 d . . . H2D H 0.2074 0.1094 0.3187 0.026 Uiso 1 1 calc R . . N3D N 0.20060(12) -0.0311(3) 0.26743(15) 0.0214(6) Uani 1 1 d . . . C4D C 0.16586(13) -0.1255(3) 0.27610(17) 0.0212(7) Uani 1 1 d . . . C5D C 0.13415(14) -0.1076(3) 0.32702(17) 0.0247(7) Uani 1 1 d . . . C6D C 0.13238(18) 0.0522(4) 0.4057(2) 0.0396(10) Uani 1 1 d . . . H6D1 H 0.1610 0.1044 0.4189 0.059 Uiso 1 1 calc R . . H6D2 H 0.1266 -0.0045 0.4363 0.059 Uiso 1 1 calc R . . H6D3 H 0.0978 0.0927 0.3989 0.059 Uiso 1 1 calc R . . C7D C 0.16550(14) -0.2250(3) 0.23564(17) 0.0224(7) Uani 1 1 d . . . C8D C 0.21630(14) -0.2688(3) 0.2137(2) 0.0275(8) Uani 1 1 d . . . H8D H 0.2502 -0.2343 0.2244 0.033 Uiso 1 1 calc R . . C9D C 0.21686(17) -0.3630(3) 0.1761(2) 0.0348(9) Uani 1 1 d . . . H9D H 0.2509 -0.3915 0.1617 0.042 Uiso 1 1 calc R . . C10D C 0.16564(19) -0.4151(3) 0.1599(2) 0.0332(9) Uani 1 1 d . . . H10D H 0.1655 -0.4775 0.1340 0.040 Uiso 1 1 calc R . . C11D C 0.11543(16) -0.3731(3) 0.1827(2) 0.0291(8) Uani 1 1 d . . . H11D H 0.0816 -0.4089 0.1731 0.035 Uiso 1 1 calc R . . C12D C 0.11519(15) -0.2778(3) 0.21979(17) 0.0262(7) Uani 1 1 d . . . H12D H 0.0811 -0.2491 0.2341 0.031 Uiso 1 1 calc R . . C13D C 0.09407(17) -0.1830(4) 0.35928(19) 0.0356(10) Uani 1 1 d . . . C14D C 0.1100(2) -0.2960(5) 0.3709(2) 0.0461(12) Uani 1 1 d . . . H14D H 0.1445 -0.3226 0.3568 0.055 Uiso 1 1 calc R . . C15D C 0.0747(3) -0.3686(6) 0.4032(3) 0.0628(16) Uani 1 1 d U . . H15D H 0.0857 -0.4429 0.4114 0.075 Uiso 1 1 calc R . . C16D C 0.0227(3) -0.3284(7) 0.4230(3) 0.0679(18) Uani 1 1 d U . . H16D H -0.0013 -0.3763 0.4444 0.081 Uiso 1 1 calc R . . C17D C 0.0067(2) -0.2196(7) 0.4115(2) 0.0635(17) Uani 1 1 d U . . H17D H -0.0279 -0.1941 0.4260 0.076 Uiso 1 1 calc R . . C18D C 0.04161(19) -0.1430(5) 0.3776(2) 0.0488(13) Uani 1 1 d U . . H18D H 0.0297 -0.0698 0.3684 0.059 Uiso 1 1 calc R . . O5 O 0.1237(3) 0.1046(7) 0.9070(5) 0.154(4) Uani 1 1 d . . . C19 C 0.1723(4) 0.1159(8) 0.9191(5) 0.099(3) Uani 1 1 d . . . C20 C 0.1957(4) 0.1151(6) 0.9831(4) 0.078(2) Uani 1 1 d . . . H20A H 0.2039 0.1914 0.9954 0.117 Uiso 1 1 calc R . . H20B H 0.2296 0.0705 0.9842 0.117 Uiso 1 1 calc R . . H20C H 0.1683 0.0827 1.0101 0.117 Uiso 1 1 calc R . . C21 C 0.2176(6) 0.1422(13) 0.8731(5) 0.145(5) Uani 1 1 d . . . H21A H 0.2433 0.0795 0.8705 0.217 Uiso 1 1 calc R . . H21B H 0.2376 0.2093 0.8852 0.217 Uiso 1 1 calc R . . H21C H 0.2005 0.1546 0.8342 0.217 Uiso 1 1 calc R . . Cl1 Cl 0.25744(4) -0.05299(10) 0.51190(7) 0.0419(3) Uani 1 1 d . . . O1 O 0.24355(13) -0.1105(3) 0.4565(2) 0.0474(8) Uani 1 1 d . . . O2 O 0.29801(13) 0.0343(3) 0.5004(2) 0.0512(9) Uani 1 1 d . . . O3 O 0.20692(14) -0.0015(3) 0.5373(2) 0.0508(9) Uani 1 1 d . . . O4 O 0.28044(17) -0.1341(3) 0.5543(2) 0.0608(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0124(2) 0.0211(3) 0.0182(3) -0.0014(2) 0.0004(3) -0.00013(18) N1A 0.0172(12) 0.0220(13) 0.0205(14) 0.0004(12) -0.0019(11) 0.0037(10) C2A 0.0158(14) 0.0266(16) 0.0217(17) -0.0030(14) -0.0013(13) 0.0026(12) N3A 0.0143(13) 0.0241(13) 0.0177(15) 0.0003(12) 0.0014(11) 0.0001(10) C4A 0.0148(14) 0.0236(16) 0.0223(18) 0.0032(14) 0.0006(14) 0.0017(11) C5A 0.0162(15) 0.0232(15) 0.0190(16) -0.0017(13) -0.0008(13) 0.0042(12) C6A 0.0232(15) 0.0305(18) 0.0291(19) -0.0052(16) -0.0053(15) 0.0022(13) C7A 0.0184(14) 0.0235(15) 0.0233(16) 0.0013(14) -0.0025(14) 0.0041(12) C8A 0.0244(15) 0.0267(17) 0.030(2) 0.0003(15) -0.0001(15) 0.0018(13) C9A 0.040(2) 0.0261(18) 0.043(2) -0.0034(17) -0.0025(19) 0.0051(15) C10A 0.041(2) 0.042(2) 0.035(2) -0.010(2) 0.0050(19) 0.0187(18) C11A 0.0250(17) 0.045(2) 0.033(2) -0.0004(19) 0.0067(17) 0.0081(16) C12A 0.0209(15) 0.0353(18) 0.027(2) -0.0020(16) 0.0026(15) 0.0021(13) C13A 0.0137(14) 0.0250(16) 0.0211(16) 0.0015(14) -0.0002(13) 0.0040(11) C14A 0.0219(17) 0.0278(17) 0.030(2) 0.0030(16) -0.0013(15) 0.0011(13) C15A 0.0198(16) 0.039(2) 0.039(2) 0.0032(19) -0.0042(17) 0.0108(15) C16A 0.0144(14) 0.040(2) 0.030(2) -0.0032(17) -0.0005(14) 0.0008(13) C17A 0.0225(16) 0.040(2) 0.030(2) 0.0036(17) -0.0009(16) -0.0047(14) C18A 0.0238(17) 0.0316(18) 0.030(2) 0.0037(16) 0.0009(15) -0.0019(14) N1B 0.0152(12) 0.0285(14) 0.0253(15) 0.0016(13) 0.0049(12) 0.0035(11) C2B 0.0178(15) 0.0230(16) 0.0264(18) -0.0007(14) 0.0033(14) 0.0004(12) N3B 0.0137(12) 0.0273(14) 0.0221(15) -0.0024(13) 0.0010(11) 0.0013(11) C4B 0.0172(15) 0.0249(16) 0.0195(17) -0.0014(13) 0.0005(14) 0.0009(11) C5B 0.0199(15) 0.0234(16) 0.0211(17) -0.0036(14) 0.0006(13) 0.0018(12) C6B 0.0247(16) 0.0289(18) 0.0292(19) 0.0015(16) 0.0061(15) 0.0023(13) C7B 0.0216(15) 0.0294(17) 0.0202(16) -0.0002(15) 0.0033(14) 0.0032(13) C8B 0.0239(15) 0.0268(17) 0.0293(19) -0.0024(15) 0.0059(15) 0.0029(13) C9B 0.041(2) 0.0313(19) 0.034(2) 0.0013(17) 0.0055(18) 0.0112(16) C10B 0.043(2) 0.044(2) 0.024(2) 0.0070(18) 0.0031(18) 0.0225(18) C11B 0.0254(17) 0.054(2) 0.029(2) 0.0025(19) -0.0062(17) 0.0144(17) C12B 0.0227(15) 0.0327(17) 0.029(2) 0.0007(16) 0.0018(15) 0.0017(13) C13B 0.0157(15) 0.0309(17) 0.0205(16) -0.0006(15) 0.0003(13) 0.0027(12) C14B 0.0208(16) 0.0323(18) 0.027(2) 0.0005(16) 0.0026(15) 0.0020(14) C15B 0.0249(18) 0.0330(18) 0.032(2) -0.0004(17) 0.0045(16) 0.0095(15) C16B 0.0155(14) 0.045(2) 0.0262(19) 0.0088(17) 0.0032(14) 0.0042(14) C17B 0.0239(17) 0.040(2) 0.033(2) -0.0035(18) 0.0002(16) -0.0053(15) C18B 0.0201(16) 0.0329(19) 0.039(2) -0.0070(18) 0.0008(16) 0.0020(14) N1C 0.0227(14) 0.0301(15) 0.0183(16) 0.0010(13) -0.0023(13) 0.0020(12) C2C 0.0165(14) 0.0216(16) 0.0256(18) 0.0007(14) 0.0011(14) 0.0021(12) N3C 0.0205(13) 0.0225(13) 0.0183(15) 0.0010(12) -0.0004(12) -0.0002(11) C4C 0.0165(14) 0.0286(18) 0.0249(18) -0.0053(15) -0.0009(14) -0.0028(13) C5C 0.0240(16) 0.0344(19) 0.0201(18) -0.0014(16) -0.0010(14) -0.0071(15) C6C 0.0274(18) 0.057(3) 0.025(2) 0.015(2) -0.0074(15) -0.0005(18) C7C 0.0281(17) 0.0272(17) 0.0216(17) -0.0058(15) -0.0020(14) -0.0033(14) C8C 0.0232(16) 0.0255(17) 0.051(3) -0.0028(18) 0.0003(17) -0.0033(13) C9C 0.0326(19) 0.0278(18) 0.049(3) 0.0039(18) -0.0020(18) 0.0026(14) C10C 0.038(2) 0.0222(17) 0.041(2) -0.0012(18) 0.0025(18) -0.0007(15) C11C 0.0340(19) 0.0300(18) 0.032(2) -0.0047(16) 0.0100(16) -0.0097(15) C12C 0.0253(16) 0.0282(17) 0.0256(18) -0.0058(14) 0.0024(14) -0.0026(13) C13C 0.0306(19) 0.059(3) 0.0219(18) -0.0035(19) -0.0001(16) -0.0193(19) C14C 0.054(3) 0.057(3) 0.033(2) -0.016(2) 0.010(2) -0.029(2) C15C 0.060(3) 0.080(4) 0.039(3) -0.018(3) 0.019(2) -0.046(3) C16C 0.079(4) 0.107(5) 0.026(2) -0.004(3) 0.008(2) -0.068(4) C17C 0.037(2) 0.117(5) 0.040(3) 0.024(3) -0.009(2) -0.040(3) C18C 0.033(2) 0.081(3) 0.037(2) 0.014(2) -0.0111(19) -0.025(2) N1D 0.0155(13) 0.0385(18) 0.0235(17) -0.0062(14) 0.0009(13) -0.0012(11) C2D 0.0191(14) 0.0260(16) 0.0198(17) -0.0032(14) -0.0007(14) 0.0065(13) N3D 0.0155(13) 0.0253(14) 0.0234(16) -0.0010(13) 0.0000(12) 0.0011(11) C4D 0.0178(14) 0.0238(16) 0.0219(17) 0.0063(14) 0.0012(13) -0.0004(12) C5D 0.0176(15) 0.038(2) 0.0183(17) -0.0014(16) -0.0006(13) -0.0058(14) C6D 0.032(2) 0.059(3) 0.028(2) -0.013(2) 0.0074(18) -0.0004(18) C7D 0.0225(15) 0.0221(16) 0.0227(17) 0.0056(15) -0.0019(14) -0.0002(13) C8D 0.0229(15) 0.0250(16) 0.035(2) -0.0001(16) -0.0012(16) 0.0016(12) C9D 0.0294(18) 0.0279(17) 0.047(3) -0.0037(18) 0.0004(18) 0.0053(14) C10D 0.045(2) 0.0208(16) 0.034(2) -0.0028(16) -0.0032(18) 0.0012(15) C11D 0.0302(18) 0.0252(17) 0.0318(19) 0.0016(16) -0.0092(17) -0.0065(13) C12D 0.0268(16) 0.0292(17) 0.0226(19) 0.0021(14) -0.0041(14) -0.0006(13) C13D 0.0307(19) 0.056(3) 0.0198(18) -0.0038(18) -0.0001(15) -0.0204(19) C14D 0.048(2) 0.054(3) 0.037(2) 0.014(2) -0.013(2) -0.023(2) C15D 0.064(3) 0.088(4) 0.037(3) 0.020(3) -0.017(2) -0.040(3) C16D 0.069(3) 0.104(4) 0.031(2) 0.010(3) -0.010(2) -0.054(3) C17D 0.041(2) 0.120(5) 0.030(2) -0.021(3) 0.008(2) -0.038(3) C18D 0.0282(19) 0.080(3) 0.038(2) -0.021(2) 0.0059(19) -0.022(2) O5 0.084(4) 0.163(7) 0.215(10) 0.034(8) -0.056(6) -0.017(5) C19 0.077(5) 0.108(6) 0.111(7) 0.061(6) -0.024(5) -0.022(4) C20 0.096(5) 0.064(4) 0.074(4) 0.009(4) 0.016(4) -0.014(4) C21 0.188(12) 0.178(13) 0.068(6) 0.051(7) -0.008(7) -0.066(11) Cl1 0.0261(4) 0.0481(6) 0.0515(6) -0.0032(5) -0.0037(5) -0.0063(4) O1 0.0421(16) 0.0434(17) 0.057(2) -0.0100(17) 0.0007(16) -0.0148(14) O2 0.0335(15) 0.0455(18) 0.074(3) -0.0096(19) -0.0016(17) -0.0102(13) O3 0.0274(15) 0.068(2) 0.057(2) -0.0016(19) 0.0052(16) -0.0016(14) O4 0.054(2) 0.057(2) 0.071(3) 0.009(2) -0.023(2) -0.0003(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3C 1.896(3) . ? Ni N3B 1.896(3) . ? Ni N3D 1.899(3) . ? Ni N3A 1.901(3) . ? N1A C2A 1.327(5) . ? N1A C5A 1.403(4) . ? N1A C6A 1.474(5) . ? C2A N3A 1.335(5) . ? C2A H2A 0.9300 . ? N3A C4A 1.390(4) . ? C4A C5A 1.365(5) . ? C4A C7A 1.472(5) . ? C5A C13A 1.482(4) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C8A 1.391(5) . ? C7A C12A 1.404(5) . ? C8A C9A 1.393(6) . ? C8A H8A 0.9300 . ? C9A C10A 1.384(7) . ? C9A H9A 0.9300 . ? C10A C11A 1.396(7) . ? C10A H10A 0.9300 . ? C11A C12A 1.395(6) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C18A 1.395(5) . ? C13A C14A 1.405(5) . ? C14A C15A 1.394(5) . ? C14A H14A 0.9300 . ? C15A C16A 1.376(6) . ? C15A H15A 0.9300 . ? C16A C17A 1.391(6) . ? C16A H16A 0.9300 . ? C17A C18A 1.387(5) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? N1B C2B 1.348(4) . ? N1B C5B 1.370(5) . ? N1B C6B 1.473(5) . ? C2B N3B 1.332(5) . ? C2B H2B 0.9300 . ? N3B C4B 1.396(4) . ? C4B C5B 1.374(5) . ? C4B C7B 1.473(5) . ? C5B C13B 1.487(4) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B C12B 1.393(5) . ? C7B C8B 1.399(5) . ? C8B C9B 1.386(6) . ? C8B H8B 0.9300 . ? C9B C10B 1.396(6) . ? C9B H9B 0.9300 . ? C10B C11B 1.377(7) . ? C10B H10B 0.9300 . ? C11B C12B 1.399(6) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C18B 1.384(5) . ? C13B C14B 1.408(5) . ? C14B C15B 1.398(5) . ? C14B H14B 0.9300 . ? C15B C16B 1.377(6) . ? C15B H15B 0.9300 . ? C16B C17B 1.373(6) . ? C16B H16B 0.9300 . ? C17B C18B 1.415(5) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? N1C C2C 1.342(5) . ? N1C C5C 1.385(5) . ? N1C C6C 1.469(5) . ? C2C N3C 1.338(5) . ? C2C H2C 0.9300 . ? N3C C4C 1.387(5) . ? C4C C5C 1.381(5) . ? C4C C7C 1.461(5) . ? C5C C13C 1.481(5) . ? C6C H6C1 0.9600 . ? C6C H6C2 0.9600 . ? C6C H6C3 0.9600 . ? C7C C8C 1.393(5) . ? C7C C12C 1.397(5) . ? C8C C9C 1.382(6) . ? C8C H8C 0.9300 . ? C9C C10C 1.398(6) . ? C9C H9C 0.9300 . ? C10C C11C 1.372(6) . ? C10C H10C 0.9300 . ? C11C C12C 1.395(6) . ? C11C H11C 0.9300 . ? C12C H12C 0.9300 . ? C13C C18C 1.394(7) . ? C13C C14C 1.414(8) . ? C14C C15C 1.396(7) . ? C14C H14C 0.9300 . ? C15C C16C 1.383(10) . ? C15C H15C 0.9300 . ? C16C C17C 1.381(12) . ? C16C H16C 0.9300 . ? C17C C18C 1.432(7) . ? C17C H17C 0.9300 . ? C18C H18C 0.9300 . ? N1D C2D 1.327(5) . ? N1D C5D 1.387(5) . ? N1D C6D 1.464(5) . ? C2D N3D 1.332(5) . ? C2D H2D 0.9300 . ? N3D C4D 1.397(4) . ? C4D C5D 1.369(5) . ? C4D C7D 1.473(5) . ? C5D C13D 1.482(5) . ? C6D H6D1 0.9600 . ? C6D H6D2 0.9600 . ? C6D H6D3 0.9600 . ? C7D C12D 1.389(5) . ? C7D C8D 1.397(5) . ? C8D C9D 1.384(6) . ? C8D H8D 0.9300 . ? C9D C10D 1.407(6) . ? C9D H9D 0.9300 . ? C10D C11D 1.384(6) . ? C10D H10D 0.9300 . ? C11D C12D 1.389(6) . ? C11D H11D 0.9300 . ? C12D H12D 0.9300 . ? C13D C18D 1.390(7) . ? C13D C14D 1.406(7) . ? C14D C15D 1.392(7) . ? C14D H14D 0.9300 . ? C15D C16D 1.391(11) . ? C15D H15D 0.9300 . ? C16D C17D 1.361(11) . ? C16D H16D 0.9300 . ? C17D C18D 1.433(8) . ? C17D H17D 0.9300 . ? C18D H18D 0.9300 . ? O5 C19 1.191(10) . ? C19 C21 1.511(14) . ? C19 C20 1.516(12) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? Cl1 O2 1.430(3) . ? Cl1 O1 1.437(4) . ? Cl1 O4 1.445(4) . ? Cl1 O3 1.455(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3C Ni N3B 90.29(12) . . ? N3C Ni N3D 87.91(15) . . ? N3B Ni N3D 177.44(14) . . ? N3C Ni N3A 178.34(14) . . ? N3B Ni N3A 90.85(14) . . ? N3D Ni N3A 90.99(12) . . ? C2A N1A C5A 107.8(3) . . ? C2A N1A C6A 125.3(3) . . ? C5A N1A C6A 127.0(3) . . ? N1A C2A N3A 111.2(3) . . ? N1A C2A H2A 124.4 . . ? N3A C2A H2A 124.4 . . ? C2A N3A C4A 106.4(3) . . ? C2A N3A Ni 121.3(2) . . ? C4A N3A Ni 128.4(3) . . ? C5A C4A N3A 108.8(3) . . ? C5A C4A C7A 129.3(3) . . ? N3A C4A C7A 121.8(3) . . ? C4A C5A N1A 105.9(3) . . ? C4A C5A C13A 131.3(3) . . ? N1A C5A C13A 122.9(3) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A C12A 118.8(3) . . ? C8A C7A C4A 120.5(3) . . ? C12A C7A C4A 120.6(3) . . ? C7A C8A C9A 121.0(4) . . ? C7A C8A H8A 119.5 . . ? C9A C8A H8A 119.5 . . ? C10A C9A C8A 119.7(4) . . ? C10A C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? C9A C10A C11A 120.5(4) . . ? C9A C10A H10A 119.8 . . ? C11A C10A H10A 119.8 . . ? C12A C11A C10A 119.6(4) . . ? C12A C11A H11A 120.2 . . ? C10A C11A H11A 120.2 . . ? C11A C12A C7A 120.4(4) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C18A C13A C14A 118.9(3) . . ? C18A C13A C5A 121.5(3) . . ? C14A C13A C5A 119.5(3) . . ? C15A C14A C13A 120.0(3) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C16A C15A C14A 120.2(4) . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C15A C16A C17A 120.5(3) . . ? C15A C16A H16A 119.8 . . ? C17A C16A H16A 119.8 . . ? C18A C17A C16A 119.7(4) . . ? C18A C17A H17A 120.2 . . ? C16A C17A H17A 120.2 . . ? C17A C18A C13A 120.7(4) . . ? C17A C18A H18A 119.6 . . ? C13A C18A H18A 119.6 . . ? C2B N1B C5B 107.8(3) . . ? C2B N1B C6B 124.5(3) . . ? C5B N1B C6B 127.7(3) . . ? N3B C2B N1B 110.8(3) . . ? N3B C2B H2B 124.6 . . ? N1B C2B H2B 124.6 . . ? C2B N3B C4B 106.4(3) . . ? C2B N3B Ni 121.8(2) . . ? C4B N3B Ni 129.5(3) . . ? C5B C4B N3B 108.0(3) . . ? C5B C4B C7B 128.7(3) . . ? N3B C4B C7B 123.2(3) . . ? N1B C5B C4B 107.0(3) . . ? N1B C5B C13B 124.1(3) . . ? C4B C5B C13B 128.8(3) . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C12B C7B C8B 119.0(3) . . ? C12B C7B C4B 120.6(3) . . ? C8B C7B C4B 120.4(3) . . ? C9B C8B C7B 120.7(4) . . ? C9B C8B H8B 119.7 . . ? C7B C8B H8B 119.7 . . ? C8B C9B C10B 119.7(4) . . ? C8B C9B H9B 120.1 . . ? C10B C9B H9B 120.1 . . ? C11B C10B C9B 120.1(4) . . ? C11B C10B H10B 119.9 . . ? C9B C10B H10B 119.9 . . ? C10B C11B C12B 120.2(4) . . ? C10B C11B H11B 119.9 . . ? C12B C11B H11B 119.9 . . ? C7B C12B C11B 120.2(4) . . ? C7B C12B H12B 119.9 . . ? C11B C12B H12B 119.9 . . ? C18B C13B C14B 119.8(3) . . ? C18B C13B C5B 121.2(3) . . ? C14B C13B C5B 119.0(3) . . ? C15B C14B C13B 119.3(3) . . ? C15B C14B H14B 120.4 . . ? C13B C14B H14B 120.4 . . ? C16B C15B C14B 120.6(4) . . ? C16B C15B H15B 119.7 . . ? C14B C15B H15B 119.7 . . ? C17B C16B C15B 120.5(3) . . ? C17B C16B H16B 119.7 . . ? C15B C16B H16B 119.7 . . ? C16B C17B C18B 120.0(4) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C13B C18B C17B 119.8(4) . . ? C13B C18B H18B 120.1 . . ? C17B C18B H18B 120.1 . . ? C2C N1C C5C 108.2(3) . . ? C2C N1C C6C 123.9(3) . . ? C5C N1C C6C 127.9(3) . . ? N3C C2C N1C 110.4(3) . . ? N3C C2C H2C 124.8 . . ? N1C C2C H2C 124.8 . . ? C2C N3C C4C 107.0(3) . . ? C2C N3C Ni 121.3(2) . . ? C4C N3C Ni 131.5(3) . . ? C5C C4C N3C 108.2(3) . . ? C5C C4C C7C 128.3(3) . . ? N3C C4C C7C 123.5(3) . . ? C4C C5C N1C 106.3(3) . . ? C4C C5C C13C 129.7(4) . . ? N1C C5C C13C 123.9(4) . . ? N1C C6C H6C1 109.5 . . ? N1C C6C H6C2 109.5 . . ? H6C1 C6C H6C2 109.5 . . ? N1C C6C H6C3 109.5 . . ? H6C1 C6C H6C3 109.5 . . ? H6C2 C6C H6C3 109.5 . . ? C8C C7C C12C 118.6(4) . . ? C8C C7C C4C 120.1(3) . . ? C12C C7C C4C 121.3(3) . . ? C9C C8C C7C 120.5(4) . . ? C9C C8C H8C 119.7 . . ? C7C C8C H8C 119.7 . . ? C8C C9C C10C 120.1(4) . . ? C8C C9C H9C 119.9 . . ? C10C C9C H9C 119.9 . . ? C11C C10C C9C 120.1(4) . . ? C11C C10C H10C 120.0 . . ? C9C C10C H10C 120.0 . . ? C10C C11C C12C 119.8(4) . . ? C10C C11C H11C 120.1 . . ? C12C C11C H11C 120.1 . . ? C11C C12C C7C 120.8(4) . . ? C11C C12C H12C 119.6 . . ? C7C C12C H12C 119.6 . . ? C18C C13C C14C 121.9(4) . . ? C18C C13C C5C 120.5(5) . . ? C14C C13C C5C 117.6(4) . . ? C15C C14C C13C 119.4(6) . . ? C15C C14C H14C 120.3 . . ? C13C C14C H14C 120.3 . . ? C16C C15C C14C 118.8(6) . . ? C16C C15C H15C 120.6 . . ? C14C C15C H15C 120.6 . . ? C17C C16C C15C 122.7(5) . . ? C17C C16C H16C 118.6 . . ? C15C C16C H16C 118.6 . . ? C16C C17C C18C 119.6(6) . . ? C16C C17C H17C 120.2 . . ? C18C C17C H17C 120.2 . . ? C13C C18C C17C 117.5(6) . . ? C13C C18C H18C 121.3 . . ? C17C C18C H18C 121.3 . . ? C2D N1D C5D 108.3(3) . . ? C2D N1D C6D 123.6(3) . . ? C5D N1D C6D 127.9(3) . . ? N1D C2D N3D 111.0(3) . . ? N1D C2D H2D 124.5 . . ? N3D C2D H2D 124.5 . . ? C2D N3D C4D 106.3(3) . . ? C2D N3D Ni 121.7(3) . . ? C4D N3D Ni 132.0(3) . . ? C5D C4D N3D 108.3(3) . . ? C5D C4D C7D 128.1(3) . . ? N3D C4D C7D 123.6(3) . . ? C4D C5D N1D 106.1(3) . . ? C4D C5D C13D 130.9(4) . . ? N1D C5D C13D 122.8(3) . . ? N1D C6D H6D1 109.5 . . ? N1D C6D H6D2 109.5 . . ? H6D1 C6D H6D2 109.5 . . ? N1D C6D H6D3 109.5 . . ? H6D1 C6D H6D3 109.5 . . ? H6D2 C6D H6D3 109.5 . . ? C12D C7D C8D 119.2(3) . . ? C12D C7D C4D 120.9(3) . . ? C8D C7D C4D 119.9(3) . . ? C9D C8D C7D 120.8(3) . . ? C9D C8D H8D 119.6 . . ? C7D C8D H8D 119.6 . . ? C8D C9D C10D 119.6(4) . . ? C8D C9D H9D 120.2 . . ? C10D C9D H9D 120.2 . . ? C11D C10D C9D 119.6(4) . . ? C11D C10D H10D 120.2 . . ? C9D C10D H10D 120.2 . . ? C10D C11D C12D 120.4(3) . . ? C10D C11D H11D 119.8 . . ? C12D C11D H11D 119.8 . . ? C11D C12D C7D 120.4(3) . . ? C11D C12D H12D 119.8 . . ? C7D C12D H12D 119.8 . . ? C18D C13D C14D 120.5(5) . . ? C18D C13D C5D 120.7(5) . . ? C14D C13D C5D 118.8(4) . . ? C15D C14D C13D 120.9(6) . . ? C15D C14D H14D 119.6 . . ? C13D C14D H14D 119.6 . . ? C16D C15D C14D 119.0(7) . . ? C16D C15D H15D 120.5 . . ? C14D C15D H15D 120.5 . . ? C17D C16D C15D 120.6(5) . . ? C17D C16D H16D 119.7 . . ? C15D C16D H16D 119.7 . . ? C16D C17D C18D 121.9(6) . . ? C16D C17D H17D 119.1 . . ? C18D C17D H17D 119.1 . . ? C13D C18D C17D 117.1(6) . . ? C13D C18D H18D 121.5 . . ? C17D C18D H18D 121.5 . . ? O5 C19 C21 123.9(11) . . ? O5 C19 C20 124.3(10) . . ? C21 C19 C20 111.6(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 Cl1 O1 110.0(2) . . ? O2 Cl1 O4 109.6(2) . . ? O1 Cl1 O4 109.1(2) . . ? O2 Cl1 O3 108.8(2) . . ? O1 Cl1 O3 109.6(2) . . ? O4 Cl1 O3 109.6(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.557 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.091 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.693 0.154 0.429 140 61 ' ' 2 0.307 -0.154 0.929 140 61 ' ' 3 0.942 0.017 0.296 7 2 ' ' 4 0.193 0.346 0.429 140 61 ' ' 5 0.442 0.483 0.296 7 2 ' ' 6 0.807 0.654 0.929 140 61 ' ' 7 0.558 0.517 0.796 7 2 ' ' 8 0.058 0.983 0.796 7 2 ' ' # start Validation Reply Form _vrf_PLAT051_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: One (of the two) perchlorate counterion of the structure is severely disordered. Persistent attempts to model disorder with a chemically reasonable geometry (using several diffraction data collected at 100 K with MoKa and CuKa radiation) were unsuccessful. Therefore, the SQUEEZE procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001) was employed to remove the contribution of the electron density associated with this ion from the intensity data. The solvent-free model and intensity data were used for the final results reported here. However, the role of the disordered perchlorate in the supramolecular organization of the complexes within the crystal structure has been taken into account using a structural model prior to omission. The atoms of the omitted perchlorate ion have been included in the sum and moiety formula, and the Mr, Dx, Mu and F(000) have been modified accordingly; these modifications account for the differences detected in the relevant data items. ; _vrf_CHEMW03_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: See comment above for PLAT051 Alert. ; _vrf_PLAT043_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: See comment above for PLAT051 Alert. ; _vrf_PLAT112_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: Examination and statistical analysis of the difraction data used show that the crystal structure is truly non-centrosymmetric, and that the space group is Pna2(1) as clearly deduced from the systematic absences. Furthermore, the refined Flack parameter of 0.51(2) indicates that the macroscopic crystal used is twinning by inversion in a ratio of approximately 51:49. ; _vrf_STRVA01_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: The crystal studied exhibited inversion twinning with a 51:49 domain ration. ; _vrf_PLAT041_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: See comment above for PLAT051 Alert. ; _vrf_PLAT042_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: See comment above for PLAT051 Alert. ; _vrf_PLAT068_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: See comment above for PLAT051 Alert. ; _vrf_CELLZ01_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: Due to the omission of the disordered density (ClO4 anion) from the model. See comment above for PLAT051 Alert. ; _vrf_PLAT033_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: The crystal studied exhibited inversion twinning with a 51:49 domain ration. ; _vrf_PLAT605_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: Due to the omission of the disordered density of the ClO4 anion from the model. ; _vrf_REFLT03_5-NiL4_{ClO4}2_Me2CO ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 2886 Friedel pairs. ; # end Validation Reply Form #===END data_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881067' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 N8 Ni, 2(C30 H24 Cl2 N4 Ni), 2(Cl), 1.35 (H2 O)' _chemical_formula_sum 'C120 H98.70 Cl6 N16 Ni3 O1.35' _chemical_formula_weight 2175.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.7526(5) _cell_length_b 19.9434(7) _cell_length_c 19.9541(8) _cell_angle_alpha 116.937(4) _cell_angle_beta 103.576(3) _cell_angle_gamma 93.729(3) _cell_volume 5325.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14883 _cell_measurement_theta_min 2.8792 _cell_measurement_theta_max 28.6040 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2255 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58902 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.50 _reflns_number_total 21984 _reflns_number_gt 12535 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Chlorine CL6 counterion and lattice water molecule O1 are disordered over two sites forming two mixed CL/O sites: CL6A/O1B (62:38) and CL6B/O1A (38:62) as was concluded after competitive and detailed refinement. Due to this disorder it was not possible to locate the water H-atoms in the course of the X-ray analysis. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21984 _refine_ls_number_parameters 1367 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.946 _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 C2A C 0.48054(18) -0.02928(16) 0.66399(16) 0.0228(7) Uani 1 1 d . . . H2A H 0.4913 -0.0690 0.6751 0.027 Uiso 1 1 calc R . . C2B C 0.5412(2) 0.23882(17) 0.92969(16) 0.0262(8) Uani 1 1 d . . . H2B H 0.4814 0.2377 0.9271 0.031 Uiso 1 1 calc R . . C2C C 0.85223(19) 0.33497(16) 0.59533(16) 0.0214(7) Uani 1 1 d . . . H2C H 0.8214 0.3750 0.6112 0.026 Uiso 1 1 calc R . . C2D C 1.16788(19) 0.43173(16) 0.79970(16) 0.0251(8) Uani 1 1 d . . . H2D H 1.2077 0.4623 0.7922 0.030 Uiso 1 1 calc R . . C2E C 0.65097(18) 0.34723(16) 0.18708(18) 0.0257(8) Uani 1 1 d . . . H2E H 0.6635 0.3137 0.1414 0.031 Uiso 1 1 calc R . . C2F C 0.86240(18) 0.33599(16) 0.24510(16) 0.0197(7) Uani 1 1 d . . . H2F H 0.8544 0.3834 0.2809 0.024 Uiso 1 1 calc R . . C2G C 0.71371(18) 0.11141(15) 0.24228(15) 0.0180(7) Uani 1 1 d . . . H2G H 0.6529 0.0975 0.2163 0.022 Uiso 1 1 calc R . . C2H C 0.6408(2) 0.25236(15) 0.37423(17) 0.0225(7) Uani 1 1 d . . . H2H H 0.6969 0.2555 0.4051 0.027 Uiso 1 1 calc R . . C4A C 0.46920(18) 0.08399(15) 0.67697(16) 0.0192(7) Uani 1 1 d . . . C4B C 0.66657(19) 0.20461(17) 0.91511(16) 0.0223(7) Uani 1 1 d . . . C4C C 0.95836(18) 0.27033(15) 0.57908(15) 0.0166(7) Uani 1 1 d . . . C4D C 1.04598(18) 0.37180(15) 0.79710(16) 0.0195(7) Uani 1 1 d . . . C4E C 0.64457(18) 0.40599(16) 0.30756(17) 0.0237(8) Uani 1 1 d . . . C4F C 0.84265(18) 0.21356(16) 0.16413(16) 0.0177(7) Uani 1 1 d . . . C4G C 0.84887(17) 0.17823(15) 0.30969(15) 0.0169(7) Uani 1 1 d . . . C4H C 0.53328(18) 0.24459(15) 0.27874(16) 0.0209(7) Uani 1 1 d . . . C5A C 0.44172(18) 0.03311(15) 0.59780(16) 0.0185(7) Uani 1 1 d . . . C5B C 0.6837(2) 0.28294(16) 0.95883(16) 0.0234(7) Uani 1 1 d . . . C5C C 0.87953(18) 0.21802(15) 0.54257(15) 0.0173(7) Uani 1 1 d . . . C5D C 1.11557(19) 0.35589(16) 0.83972(16) 0.0220(7) Uani 1 1 d . . . C5E C 0.60035(19) 0.44134(17) 0.26916(17) 0.0269(8) Uani 1 1 d . . . C5F C 0.92230(19) 0.24774(15) 0.16583(16) 0.0184(7) Uani 1 1 d . . . C5G C 0.85125(18) 0.10350(16) 0.29174(16) 0.0190(7) Uani 1 1 d . . . C5H C 0.49685(19) 0.24416(16) 0.33380(16) 0.0210(7) Uani 1 1 d . . . C7A C 0.47628(19) 0.16798(16) 0.72023(16) 0.0204(7) Uani 1 1 d . . . C7B C 0.72772(19) 0.15342(16) 0.88608(16) 0.0226(7) Uani 1 1 d . . . C7C C 1.05192(18) 0.25953(14) 0.58781(16) 0.0193(7) Uani 1 1 d . . . C7D C 0.94950(18) 0.34372(16) 0.77534(16) 0.0211(7) Uani 1 1 d . . . C7E C 0.66046(19) 0.42676(15) 0.39089(17) 0.0237(8) Uani 1 1 d . . . C7F C 0.79727(19) 0.13226(16) 0.11908(16) 0.0214(7) Uani 1 1 d . . . C7G C 0.91811(18) 0.24913(15) 0.35516(15) 0.0167(7) Uani 1 1 d . . . C7H C 0.48856(18) 0.23984(16) 0.20228(16) 0.0208(7) Uani 1 1 d . . . C8A C 0.40380(19) 0.20010(16) 0.73634(16) 0.0260(8) Uani 1 1 d . . . H8A H 0.3484 0.1685 0.7188 0.031 Uiso 1 1 calc R . . C8B C 0.72882(19) 0.08674(16) 0.89254(16) 0.0243(7) Uani 1 1 d . . . H8B H 0.6889 0.0734 0.9143 0.029 Uiso 1 1 calc R . . C8C C 1.1006(2) 0.27645(16) 0.54617(16) 0.0248(8) Uani 1 1 d . . . H8C H 1.0739 0.2937 0.5117 0.030 Uiso 1 1 calc R . . C8D C 0.8922(2) 0.39530(18) 0.78827(18) 0.0317(8) Uani 1 1 d . . . H8D H 0.9150 0.4477 0.8127 0.038 Uiso 1 1 calc R . . C8E C 0.74692(19) 0.43903(15) 0.43876(17) 0.0240(8) Uani 1 1 d . . . H8E H 0.7945 0.4335 0.4179 0.029 Uiso 1 1 calc R . . C8F C 0.7078(2) 0.11238(17) 0.07631(16) 0.0275(8) Uani 1 1 d . . . H8F H 0.6771 0.1505 0.0758 0.033 Uiso 1 1 calc R . . C8G C 0.90269(18) 0.31234(16) 0.41611(16) 0.0220(7) Uani 1 1 d . . . H8G H 0.8503 0.3090 0.4292 0.026 Uiso 1 1 calc R . . C8H C 0.51039(19) 0.19195(16) 0.13482(17) 0.0258(8) Uani 1 1 d . . . H8H H 0.5526 0.1621 0.1378 0.031 Uiso 1 1 calc R . . C9A C 0.4126(2) 0.27913(17) 0.77846(18) 0.0337(9) Uani 1 1 d . . . H9A H 0.3633 0.3001 0.7892 0.040 Uiso 1 1 calc R . . C9B C 0.7885(2) 0.04016(18) 0.86708(17) 0.0309(8) Uani 1 1 d . . . H9B H 0.7887 -0.0040 0.8720 0.037 Uiso 1 1 calc R . . C9C C 1.1884(2) 0.26814(17) 0.55506(17) 0.0323(8) Uani 1 1 d . . . H9C H 1.2197 0.2781 0.5254 0.039 Uiso 1 1 calc R . . C9D C 0.8010(2) 0.3685(2) 0.7646(2) 0.0426(10) Uani 1 1 d . . . H9D H 0.7629 0.4033 0.7737 0.051 Uiso 1 1 calc R . . C9E C 0.7613(2) 0.45941(17) 0.51747(18) 0.0296(8) Uani 1 1 d . . . H9E H 0.8188 0.4671 0.5490 0.035 Uiso 1 1 calc R . . C9F C 0.6638(2) 0.0365(2) 0.03443(17) 0.0383(9) Uani 1 1 d . . . H9F H 0.6036 0.0239 0.0067 0.046 Uiso 1 1 calc R . . C9G C 0.96526(19) 0.38103(16) 0.45796(17) 0.0252(8) Uani 1 1 d . . . H9G H 0.9545 0.4232 0.4990 0.030 Uiso 1 1 calc R . . C9H C 0.46995(19) 0.18817(17) 0.06328(17) 0.0287(8) Uani 1 1 d . . . H9H H 0.4861 0.1572 0.0188 0.034 Uiso 1 1 calc R . . C10A C 0.4940(2) 0.32662(17) 0.80450(17) 0.0322(9) Uani 1 1 d . . . H10A H 0.4998 0.3796 0.8323 0.039 Uiso 1 1 calc R . . C10B C 0.8480(2) 0.05952(18) 0.83415(18) 0.0333(9) Uani 1 1 d . . . H10B H 0.8880 0.0282 0.8166 0.040 Uiso 1 1 calc R . . C10C C 1.2295(2) 0.24487(17) 0.60816(18) 0.0339(9) Uani 1 1 d . . . H10C H 1.2888 0.2402 0.6150 0.041 Uiso 1 1 calc R . . C10D C 0.7661(2) 0.2911(2) 0.72790(19) 0.0452(10) Uani 1 1 d . . . H10D H 0.7048 0.2736 0.7110 0.054 Uiso 1 1 calc R . . C10E C 0.6916(2) 0.46833(17) 0.54942(18) 0.0315(8) Uani 1 1 d . . . H10E H 0.7021 0.4822 0.6023 0.038 Uiso 1 1 calc R . . C10F C 0.7090(3) -0.02017(19) 0.03381(18) 0.0442(10) Uani 1 1 d U . . H10F H 0.6794 -0.0712 0.0054 0.053 Uiso 1 1 calc R . . C10G C 1.04292(19) 0.38642(16) 0.43861(17) 0.0241(8) Uani 1 1 d . . . H10G H 1.0844 0.4323 0.4664 0.029 Uiso 1 1 calc R . . C10H C 0.4056(2) 0.23072(19) 0.05878(19) 0.0347(9) Uani 1 1 d . . . H10H H 0.3778 0.2279 0.0108 0.042 Uiso 1 1 calc R . . C11A C 0.5667(2) 0.29508(17) 0.78902(18) 0.0326(8) Uani 1 1 d . . . H11A H 0.6218 0.3270 0.8065 0.039 Uiso 1 1 calc R . . C11B C 0.8473(2) 0.12570(18) 0.82773(18) 0.0331(8) Uani 1 1 d . . . H11B H 0.8874 0.1390 0.8061 0.040 Uiso 1 1 calc R . . C11C C 1.18230(19) 0.22864(16) 0.65070(17) 0.0248(8) Uani 1 1 d . . . H11C H 1.2099 0.2130 0.6863 0.030 Uiso 1 1 calc R . . C11D C 0.8226(2) 0.2402(2) 0.71654(18) 0.0386(9) Uani 1 1 d . . . H11D H 0.7996 0.1879 0.6923 0.046 Uiso 1 1 calc R . . C11E C 0.6057(2) 0.45672(17) 0.50301(19) 0.0365(9) Uani 1 1 d . . . H11E H 0.5585 0.4627 0.5245 0.044 Uiso 1 1 calc R . . C11F C 0.7982(2) -0.00184(17) 0.07514(18) 0.0373(9) Uani 1 1 d . . . H11F H 0.8288 -0.0405 0.0742 0.045 Uiso 1 1 calc R . . C11G C 1.05912(19) 0.32416(16) 0.37847(17) 0.0240(8) Uani 1 1 d . . . H11G H 1.1115 0.3279 0.3654 0.029 Uiso 1 1 calc R . . C11H C 0.3821(2) 0.27734(19) 0.12458(19) 0.0335(9) Uani 1 1 d . . . H11H H 0.3384 0.3057 0.1207 0.040 Uiso 1 1 calc R . . C12A C 0.5587(2) 0.21609(16) 0.74756(17) 0.0271(8) Uani 1 1 d . . . H12A H 0.6086 0.1953 0.7380 0.033 Uiso 1 1 calc R . . C12B C 0.7880(2) 0.17212(17) 0.85305(17) 0.0269(8) Uani 1 1 d . . . H12B H 0.7881 0.2163 0.8481 0.032 Uiso 1 1 calc R . . C12C C 1.09381(19) 0.23555(15) 0.64082(16) 0.0224(7) Uani 1 1 d . . . H12C H 1.0622 0.2242 0.6695 0.027 Uiso 1 1 calc R . . C12D C 0.9138(2) 0.26631(17) 0.74095(16) 0.0271(8) Uani 1 1 d . . . H12D H 0.9516 0.2314 0.7342 0.033 Uiso 1 1 calc R . . C12E C 0.5906(2) 0.43599(16) 0.42396(17) 0.0288(8) Uani 1 1 d . . . H12E H 0.5330 0.4282 0.3927 0.035 Uiso 1 1 calc R . . C12F C 0.8421(2) 0.07420(16) 0.11804(17) 0.0259(8) Uani 1 1 d . . . H12F H 0.9021 0.0865 0.1464 0.031 Uiso 1 1 calc R . . C12G C 0.99662(18) 0.25497(16) 0.33684(16) 0.0192(7) Uani 1 1 d . . . H12G H 1.0081 0.2126 0.2965 0.023 Uiso 1 1 calc R . . C12H C 0.42321(19) 0.28222(17) 0.19679(18) 0.0299(8) Uani 1 1 d . . . H12H H 0.4071 0.3137 0.2412 0.036 Uiso 1 1 calc R . . C13A C 0.40312(18) 0.04070(16) 0.52755(16) 0.0198(7) Uani 1 1 d . . . C13B C 0.76595(19) 0.34071(16) 0.98988(16) 0.0240(7) Uani 1 1 d . . . C13C C 0.85551(18) 0.13385(15) 0.49696(16) 0.0188(7) Uani 1 1 d . . . C13D C 1.1199(2) 0.30611(16) 0.87633(17) 0.0254(8) Uani 1 1 d . . . C13E C 0.5531(2) 0.50462(18) 0.29374(18) 0.0331(9) Uani 1 1 d . . . C13F C 0.99364(19) 0.21656(16) 0.13305(16) 0.0205(7) Uani 1 1 d . . . C13G C 0.92181(18) 0.06313(15) 0.30740(16) 0.0194(7) Uani 1 1 d . . . C13H C 0.40495(19) 0.23676(17) 0.33805(17) 0.0223(7) Uani 1 1 d . . . C14A C 0.40835(19) 0.11185(16) 0.53001(17) 0.0250(8) Uani 1 1 d . . . H14A H 0.4385 0.1559 0.5769 0.030 Uiso 1 1 calc R . . C14B C 0.8463(2) 0.33091(17) 1.02851(17) 0.0321(9) Uani 1 1 d . . . H14B H 0.8479 0.2890 1.0374 0.039 Uiso 1 1 calc R . . C14C C 0.90704(19) 0.08739(16) 0.51569(17) 0.0273(8) Uani 1 1 d . . . H14C H 0.9586 0.1095 0.5582 0.033 Uiso 1 1 calc R . . C14D C 1.0582(2) 0.30014(17) 0.91362(17) 0.0300(8) Uani 1 1 d . . . H14D H 1.0134 0.3285 0.9166 0.036 Uiso 1 1 calc R . . C14E C 0.5911(3) 0.5730(2) 0.3607(2) 0.0630(13) Uani 1 1 d U . . H14E H 0.6495 0.5805 0.3905 0.076 Uiso 1 1 calc R . . C14F C 0.9762(2) 0.14856(17) 0.06231(17) 0.0299(8) Uani 1 1 d . . . H14F H 0.9178 0.1257 0.0307 0.036 Uiso 1 1 calc R . . C14G C 0.99988(18) 0.10266(16) 0.36974(16) 0.0243(8) Uani 1 1 d . . . H14G H 1.0070 0.1551 0.4025 0.029 Uiso 1 1 calc R . . C14H C 0.34114(19) 0.17114(17) 0.28315(18) 0.0268(8) Uani 1 1 d . . . H14H H 0.3556 0.1324 0.2417 0.032 Uiso 1 1 calc R . . C15A C 0.36956(19) 0.11783(17) 0.46397(18) 0.0284(8) Uani 1 1 d . . . H15A H 0.3734 0.1659 0.4670 0.034 Uiso 1 1 calc R . . C15B C 0.9242(2) 0.38426(19) 1.05385(18) 0.0386(9) Uani 1 1 d . . . H15B H 0.9779 0.3780 1.0798 0.046 Uiso 1 1 calc R . . C15C C 0.8821(2) 0.00857(16) 0.47165(18) 0.0309(8) Uani 1 1 d . . . H15C H 0.9172 -0.0219 0.4849 0.037 Uiso 1 1 calc R . . C15D C 1.0633(2) 0.25180(19) 0.94658(18) 0.0387(9) Uani 1 1 d . . . H15D H 1.0218 0.2476 0.9715 0.046 Uiso 1 1 calc R . . C15E C 0.5431(3) 0.6315(2) 0.3846(2) 0.0773(16) Uani 1 1 d DU . . H15E H 0.5696 0.6778 0.4302 0.093 Uiso 1 1 calc R . . C15F C 1.0460(2) 0.11503(18) 0.03910(19) 0.0376(9) Uani 1 1 d . . . H15F H 1.0341 0.0693 -0.0078 0.045 Uiso 1 1 calc R . . C15G C 1.0664(2) 0.06478(17) 0.38319(17) 0.0298(8) Uani 1 1 d . . . H15G H 1.1187 0.0919 0.4242 0.036 Uiso 1 1 calc R . . C15H C 0.2567(2) 0.16361(18) 0.29022(19) 0.0296(8) Uani 1 1 d . . . H15H H 0.2144 0.1195 0.2535 0.035 Uiso 1 1 calc R . . C16A C 0.32506(19) 0.05347(18) 0.39338(17) 0.0293(8) Uani 1 1 d . . . H16A H 0.2985 0.0580 0.3492 0.035 Uiso 1 1 calc R . . C16B C 0.9218(2) 0.44589(19) 1.04042(18) 0.0424(10) Uani 1 1 d . . . H16B H 0.9744 0.4802 1.0558 0.051 Uiso 1 1 calc R . . C16C C 0.80622(19) -0.02551(16) 0.40851(17) 0.0270(8) Uani 1 1 d . . . H16C H 0.7901 -0.0787 0.3790 0.032 Uiso 1 1 calc R . . C16D C 1.1307(3) 0.20960(19) 0.94235(19) 0.0424(10) Uani 1 1 d . . . H16D H 1.1339 0.1772 0.9644 0.051 Uiso 1 1 calc R . . C16E C 0.4579(3) 0.6211(3) 0.3418(3) 0.0791(16) Uani 1 1 d DU . . H16E H 0.4251 0.6595 0.3586 0.095 Uiso 1 1 calc R . . C16F C 1.1335(2) 0.1493(2) 0.0855(2) 0.0376(9) Uani 1 1 d . . . H16F H 1.1798 0.1253 0.0708 0.045 Uiso 1 1 calc R . . C16G C 1.0557(2) -0.01335(19) 0.33603(18) 0.0332(9) Uani 1 1 d . . . H16G H 1.1007 -0.0388 0.3453 0.040 Uiso 1 1 calc R . . C16H C 0.2338(2) 0.22056(18) 0.35088(18) 0.0291(8) Uani 1 1 d . . . H16H H 0.1768 0.2145 0.3556 0.035 Uiso 1 1 calc R . . C17A C 0.32055(19) -0.01783(17) 0.38917(17) 0.0311(8) Uani 1 1 d . . . H17A H 0.2918 -0.0616 0.3416 0.037 Uiso 1 1 calc R . . C17B C 0.8427(2) 0.45767(18) 1.00460(18) 0.0407(10) Uani 1 1 d . . . H17B H 0.8414 0.5004 0.9971 0.049 Uiso 1 1 calc R . . C17C C 0.75396(19) 0.02005(16) 0.38930(17) 0.0229(7) Uani 1 1 d . . . H17C H 0.7025 -0.0025 0.3467 0.027 Uiso 1 1 calc R . . C17D C 1.1926(2) 0.21551(18) 0.90579(19) 0.0380(10) Uani 1 1 d . . . H17D H 1.2376 0.1873 0.9031 0.046 Uiso 1 1 calc R . . C17E C 0.4211(3) 0.5544(3) 0.2744(3) 0.0815(16) Uani 1 1 d DU . . H17E H 0.3637 0.5480 0.2436 0.098 Uiso 1 1 calc R . . C17F C 1.1517(2) 0.21861(19) 0.15298(18) 0.0316(8) Uani 1 1 d . . . H17F H 1.2104 0.2430 0.1823 0.038 Uiso 1 1 calc R . . C17G C 0.9786(2) -0.05354(17) 0.27540(18) 0.0306(8) Uani 1 1 d . . . H17G H 0.9709 -0.1063 0.2442 0.037 Uiso 1 1 calc R . . C17H C 0.2959(2) 0.28677(19) 0.40474(19) 0.0366(9) Uani 1 1 d . . . H17H H 0.2804 0.3260 0.4450 0.044 Uiso 1 1 calc R . . C18A C 0.35861(18) -0.02453(16) 0.45554(17) 0.0267(8) Uani 1 1 d . . . H18A H 0.3545 -0.0728 0.4522 0.032 Uiso 1 1 calc R . . C18B C 0.7649(2) 0.40518(17) 0.97981(17) 0.0324(8) Uani 1 1 d . . . H18B H 0.7112 0.4132 0.9561 0.039 Uiso 1 1 calc R . . C18C C 0.77800(18) 0.09873(16) 0.43316(16) 0.0199(7) Uani 1 1 d . . . H18C H 0.7422 0.1289 0.4202 0.024 Uiso 1 1 calc R . . C18D C 1.1876(2) 0.26372(17) 0.87298(17) 0.0310(8) Uani 1 1 d . . . H18D H 1.2295 0.2679 0.8485 0.037 Uiso 1 1 calc R . . C18E C 0.4674(2) 0.4961(2) 0.2510(2) 0.0539(12) Uani 1 1 d . . . H18E H 0.4402 0.4500 0.2053 0.065 Uiso 1 1 calc R . . C18F C 1.08321(19) 0.25180(17) 0.17704(17) 0.0255(8) Uani 1 1 d . . . H18F H 1.0961 0.2984 0.2232 0.031 Uiso 1 1 calc R . . C18G C 0.91238(19) -0.01517(16) 0.26082(17) 0.0257(8) Uani 1 1 d . . . H18G H 0.8608 -0.0425 0.2190 0.031 Uiso 1 1 calc R . . C18H C 0.3811(2) 0.29442(18) 0.39851(18) 0.0322(8) Uani 1 1 d . . . H18H H 0.4231 0.3387 0.4353 0.039 Uiso 1 1 calc R . . N1A N 0.45056(16) -0.03817(13) 0.59118(13) 0.0213(6) Uani 1 1 d D . . H1A H 0.4443(18) -0.0815(12) 0.5500(12) 0.032 Uiso 1 1 d D . . N1B N 0.60392(17) 0.30297(14) 0.96661(14) 0.0261(7) Uani 1 1 d D . . H1B H 0.592(2) 0.3459(12) 0.9910(16) 0.039 Uiso 1 1 d D . . N1C N 0.81404(15) 0.26072(13) 0.55274(13) 0.0192(6) Uani 1 1 d D . . H1C H 0.7576(11) 0.2444(15) 0.5407(16) 0.029 Uiso 1 1 d D . . N1D N 1.19150(16) 0.39470(14) 0.84044(14) 0.0264(7) Uani 1 1 d D . . H1D H 1.2461(13) 0.3974(16) 0.8646(16) 0.040 Uiso 1 1 d D . . N1E N 0.60548(16) 0.40303(14) 0.19344(15) 0.0290(7) Uani 1 1 d D . . H1E H 0.5809(19) 0.4156(17) 0.1587(15) 0.044 Uiso 1 1 d D . . N1F N 0.93183(16) 0.32511(13) 0.21677(14) 0.0200(6) Uani 1 1 d D . . H1F H 0.9748(15) 0.3594(14) 0.2241(17) 0.030 Uiso 1 1 d D . . N1G N 0.76445(15) 0.06363(13) 0.24971(14) 0.0196(6) Uani 1 1 d D . . H1G H 0.7448(17) 0.0171(10) 0.2346(16) 0.029 Uiso 1 1 d D . . N1H N 0.56671(17) 0.24961(13) 0.39400(14) 0.0225(6) Uani 1 1 d D . . H1H H 0.5662(19) 0.2428(16) 0.4343(13) 0.034 Uiso 1 1 d D . . N3A N 0.49282(15) 0.04302(13) 0.71771(13) 0.0202(6) Uani 1 1 d . . . N3B N 0.57569(15) 0.17751(13) 0.89750(13) 0.0226(6) Uani 1 1 d . . . N3C N 0.94010(15) 0.34385(12) 0.61187(13) 0.0179(6) Uani 1 1 d . . . N3D N 1.08019(15) 0.41918(12) 0.77142(13) 0.0214(6) Uani 1 1 d . . . N3E N 0.67589(14) 0.34614(13) 0.25499(13) 0.0210(6) Uani 1 1 d . . . N3F N 0.80622(14) 0.27007(12) 0.21541(13) 0.0185(6) Uani 1 1 d . . . N3G N 0.76137(14) 0.18226(13) 0.27702(13) 0.0196(6) Uani 1 1 d . . . N3H N 0.62532(14) 0.25014(12) 0.30465(13) 0.0184(6) Uani 1 1 d . . . Ni1 Ni 0.50189(2) 0.07221(2) 0.82849(2) 0.02318(10) Uani 1 1 d . . . Ni2 Ni 1.02404(2) 0.44243(2) 0.68633(2) 0.02256(10) Uani 1 1 d . . . Ni3 Ni 0.71715(2) 0.26240(2) 0.26285(2) 0.01964(10) Uani 1 1 d . . . Cl1 Cl 0.36573(5) 0.09997(4) 0.83949(4) 0.0291(2) Uani 1 1 d . . . Cl2 Cl 0.51955(5) -0.03613(4) 0.83337(4) 0.0288(2) Uani 1 1 d . . . Cl3 Cl 1.14156(5) 0.47311(4) 0.65407(4) 0.02801(19) Uani 1 1 d . . . Cl4 Cl 0.92629(5) 0.52326(4) 0.71464(4) 0.0278(2) Uani 1 1 d . . . Cl5 Cl 0.38817(5) 0.78672(4) 0.46896(4) 0.02328(18) Uani 1 1 d . . . Cl6A Cl 0.51690(11) 0.43254(10) 0.06148(10) 0.0325(4) Uani 0.62 1 d PU A 1 O1A O 0.6350(3) 0.5690(2) 0.0722(2) 0.0446(12) Uani 0.62 1 d PU B 1 O1B O 0.5639(4) 0.4475(4) 0.0640(4) 0.0269(19) Uani 0.38 1 d PU C 2 Cl6B Cl 0.63192(15) 0.57215(13) 0.02767(14) 0.0332(6) Uani 0.38 1 d PU D 2 O2 O 0.2496(5) 0.4170(4) 0.0804(4) 0.069(2) Uani 0.35 1 d PU . . 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 C2A 0.0190(17) 0.0250(18) 0.0220(17) 0.0112(16) 0.0030(14) 0.0008(13) C2B 0.0211(18) 0.0293(19) 0.0206(17) 0.0076(16) 0.0049(14) -0.0042(15) C2C 0.0233(18) 0.0173(17) 0.0199(16) 0.0070(14) 0.0045(14) 0.0020(13) C2D 0.0218(18) 0.0212(17) 0.0266(18) 0.0100(15) 0.0021(14) -0.0015(13) C2E 0.0217(18) 0.0176(17) 0.0261(18) 0.0023(15) 0.0043(14) 0.0037(13) C2F 0.0167(17) 0.0150(16) 0.0216(17) 0.0048(14) 0.0034(14) 0.0050(13) C2G 0.0117(16) 0.0202(16) 0.0155(15) 0.0038(14) 0.0034(12) 0.0000(13) C2H 0.0159(17) 0.0212(17) 0.0274(18) 0.0104(15) 0.0041(14) 0.0032(13) C4A 0.0163(16) 0.0191(16) 0.0195(16) 0.0076(14) 0.0048(13) 0.0013(12) C4B 0.0174(17) 0.0288(18) 0.0150(16) 0.0086(15) 0.0014(13) -0.0034(13) C4C 0.0189(17) 0.0150(16) 0.0137(15) 0.0055(14) 0.0039(13) 0.0036(12) C4D 0.0152(16) 0.0166(16) 0.0219(16) 0.0063(14) 0.0036(13) 0.0035(12) C4E 0.0122(16) 0.0201(17) 0.0262(18) 0.0034(15) 0.0005(14) 0.0024(13) C4F 0.0150(16) 0.0192(16) 0.0156(15) 0.0081(14) 0.0003(13) 0.0012(12) C4G 0.0146(16) 0.0163(16) 0.0132(15) 0.0026(13) 0.0030(12) 0.0005(12) C4H 0.0163(17) 0.0167(16) 0.0206(17) 0.0034(14) 0.0023(14) 0.0010(12) C5A 0.0160(16) 0.0169(16) 0.0197(16) 0.0063(14) 0.0055(13) 0.0025(12) C5B 0.0232(18) 0.0236(18) 0.0164(16) 0.0068(15) 0.0019(14) -0.0026(14) C5C 0.0147(16) 0.0187(16) 0.0179(16) 0.0091(14) 0.0027(13) 0.0048(13) C5D 0.0180(17) 0.0205(17) 0.0216(17) 0.0073(15) 0.0028(14) 0.0013(13) C5E 0.0215(18) 0.0243(18) 0.0190(17) 0.0003(15) -0.0008(14) 0.0063(14) C5F 0.0207(17) 0.0155(16) 0.0154(15) 0.0049(14) 0.0049(13) 0.0009(13) C5G 0.0170(17) 0.0211(17) 0.0158(15) 0.0072(14) 0.0039(13) 0.0010(13) C5H 0.0147(17) 0.0220(17) 0.0198(16) 0.0056(15) 0.0031(14) 0.0040(13) C7A 0.0251(18) 0.0194(17) 0.0134(15) 0.0072(14) 0.0032(13) -0.0010(13) C7B 0.0176(17) 0.0251(18) 0.0138(16) 0.0051(15) -0.0029(13) -0.0066(13) C7C 0.0184(17) 0.0093(15) 0.0192(16) 0.0024(13) -0.0027(13) -0.0025(12) C7D 0.0148(16) 0.0260(18) 0.0195(16) 0.0101(15) 0.0030(13) 0.0007(13) C7E 0.0211(18) 0.0158(16) 0.0240(17) 0.0022(15) 0.0048(14) 0.0038(13) C7F 0.0232(18) 0.0207(17) 0.0148(16) 0.0034(14) 0.0084(13) -0.0012(13) C7G 0.0133(16) 0.0188(16) 0.0150(15) 0.0080(14) -0.0004(13) 0.0018(12) C7H 0.0142(16) 0.0236(17) 0.0176(16) 0.0062(15) 0.0028(13) -0.0034(13) C8A 0.0184(18) 0.0214(18) 0.0231(17) 0.0035(15) -0.0034(14) -0.0011(13) C8B 0.0222(18) 0.0262(18) 0.0151(16) 0.0060(15) 0.0007(13) -0.0063(14) C8C 0.0262(19) 0.0248(18) 0.0188(16) 0.0082(15) 0.0041(14) 0.0029(14) C8D 0.0241(19) 0.039(2) 0.0337(19) 0.0208(17) 0.0059(15) 0.0040(15) C8E 0.0192(17) 0.0192(17) 0.0270(18) 0.0063(15) 0.0060(14) 0.0028(13) C8F 0.0289(19) 0.0276(18) 0.0184(16) 0.0055(15) 0.0076(14) -0.0021(14) C8G 0.0149(17) 0.0261(18) 0.0205(17) 0.0093(15) 0.0021(13) 0.0024(13) C8H 0.0179(17) 0.0247(18) 0.0289(18) 0.0099(16) 0.0050(14) -0.0023(13) C9A 0.026(2) 0.029(2) 0.0330(19) 0.0074(17) 0.0016(16) 0.0068(15) C9B 0.030(2) 0.0275(19) 0.0272(18) 0.0102(16) 0.0025(16) -0.0005(15) C9C 0.026(2) 0.042(2) 0.0247(18) 0.0122(17) 0.0085(15) 0.0050(16) C9D 0.022(2) 0.075(3) 0.047(2) 0.041(2) 0.0119(18) 0.0157(19) C9E 0.0234(19) 0.0311(19) 0.0269(19) 0.0116(16) 0.0012(15) 0.0015(14) C9F 0.034(2) 0.043(2) 0.0171(18) 0.0037(18) 0.0028(15) -0.0198(17) C9G 0.0243(18) 0.0171(17) 0.0186(16) 0.0003(14) -0.0022(14) 0.0007(13) C9H 0.0263(19) 0.0292(19) 0.0204(17) 0.0061(16) 0.0044(15) -0.0056(15) C10A 0.041(2) 0.0184(18) 0.0271(19) 0.0058(16) 0.0064(17) -0.0017(16) C10B 0.0224(19) 0.033(2) 0.0292(19) 0.0046(17) 0.0048(15) 0.0020(15) C10C 0.0222(19) 0.034(2) 0.0305(19) 0.0053(17) 0.0022(16) 0.0082(15) C10D 0.020(2) 0.087(3) 0.031(2) 0.036(2) 0.0019(16) -0.008(2) C10E 0.034(2) 0.0288(19) 0.0231(18) 0.0062(16) 0.0064(16) 0.0044(15) C10F 0.066(3) 0.0224(19) 0.0230(19) -0.0047(16) 0.0168(19) -0.0193(18) C10G 0.0178(18) 0.0208(17) 0.0250(17) 0.0090(15) -0.0026(14) -0.0022(13) C10H 0.025(2) 0.044(2) 0.0242(19) 0.0159(18) -0.0061(16) -0.0121(16) C11A 0.031(2) 0.0209(18) 0.033(2) 0.0039(16) 0.0094(16) -0.0105(15) C11B 0.027(2) 0.035(2) 0.0324(19) 0.0130(17) 0.0102(16) -0.0049(16) C11C 0.0210(18) 0.0209(17) 0.0249(17) 0.0077(15) 0.0002(14) 0.0055(13) C11D 0.035(2) 0.048(2) 0.0274(19) 0.0181(18) 0.0055(17) -0.0167(18) C11E 0.031(2) 0.035(2) 0.037(2) 0.0087(18) 0.0148(17) 0.0092(16) C11F 0.063(3) 0.0192(18) 0.0281(19) 0.0039(16) 0.0279(19) 0.0037(17) C11G 0.0173(17) 0.0281(18) 0.0248(17) 0.0141(16) 0.0014(14) 0.0003(14) C11H 0.0195(19) 0.044(2) 0.035(2) 0.0220(19) -0.0006(16) 0.0028(15) C12A 0.0262(19) 0.0246(18) 0.0265(18) 0.0078(16) 0.0110(15) 0.0023(14) C12B 0.0265(19) 0.0212(18) 0.0247(18) 0.0062(15) 0.0055(15) -0.0032(14) C12C 0.0235(18) 0.0168(16) 0.0211(16) 0.0065(14) 0.0035(14) -0.0004(13) C12D 0.0244(19) 0.0331(19) 0.0244(17) 0.0157(16) 0.0063(15) -0.0017(14) C12E 0.0245(19) 0.0225(18) 0.0243(18) 0.0014(16) 0.0021(15) 0.0050(14) C12F 0.0306(19) 0.0200(17) 0.0240(18) 0.0057(15) 0.0138(15) 0.0029(14) C12G 0.0198(17) 0.0181(16) 0.0177(16) 0.0076(14) 0.0041(13) 0.0041(13) C12H 0.0205(18) 0.037(2) 0.0252(18) 0.0121(17) 0.0010(15) 0.0023(15) C13A 0.0134(16) 0.0239(17) 0.0206(16) 0.0105(15) 0.0036(13) 0.0013(13) C13B 0.0199(18) 0.0206(17) 0.0154(16) -0.0028(14) 0.0038(13) -0.0037(13) C13C 0.0191(17) 0.0160(16) 0.0199(16) 0.0065(14) 0.0087(13) 0.0003(12) C13D 0.0230(18) 0.0228(17) 0.0189(17) 0.0053(15) -0.0032(14) 0.0021(14) C13E 0.037(2) 0.0273(19) 0.0293(19) 0.0091(17) 0.0072(16) 0.0156(16) C13F 0.0240(18) 0.0210(17) 0.0191(16) 0.0108(15) 0.0091(14) 0.0024(13) C13G 0.0167(17) 0.0203(17) 0.0205(16) 0.0091(14) 0.0063(13) 0.0026(13) C13H 0.0180(17) 0.0296(18) 0.0218(17) 0.0145(16) 0.0055(14) 0.0059(14) C14A 0.0294(19) 0.0195(17) 0.0204(17) 0.0057(15) 0.0064(14) 0.0037(14) C14B 0.033(2) 0.0260(19) 0.0235(18) 0.0056(16) 0.0008(15) -0.0042(15) C14C 0.0232(18) 0.0185(17) 0.0301(18) 0.0095(15) -0.0034(15) -0.0011(13) C14D 0.031(2) 0.033(2) 0.0265(18) 0.0148(17) 0.0079(16) 0.0077(15) C14E 0.088(3) 0.034(2) 0.041(2) 0.007(2) -0.007(2) 0.026(2) C14F 0.028(2) 0.0296(19) 0.0251(18) 0.0081(16) 0.0081(15) -0.0037(15) C14G 0.0241(18) 0.0207(17) 0.0219(17) 0.0076(15) 0.0022(14) 0.0022(13) C14H 0.0220(18) 0.0254(18) 0.0281(18) 0.0097(16) 0.0055(15) 0.0058(14) C15A 0.0278(19) 0.0264(18) 0.037(2) 0.0191(17) 0.0125(16) 0.0063(14) C15B 0.025(2) 0.040(2) 0.0260(19) 0.0013(18) 0.0001(15) -0.0082(16) C15C 0.0293(19) 0.0180(17) 0.039(2) 0.0121(16) 0.0036(16) 0.0044(14) C15D 0.045(2) 0.044(2) 0.031(2) 0.0204(19) 0.0138(17) 0.0063(18) C15E 0.137(4) 0.047(3) 0.036(2) 0.009(2) 0.018(3) 0.050(3) C15F 0.049(2) 0.030(2) 0.033(2) 0.0079(17) 0.0261(18) 0.0052(17) C15G 0.0253(19) 0.031(2) 0.0256(18) 0.0117(17) -0.0005(15) 0.0024(15) C15H 0.0183(18) 0.0301(19) 0.038(2) 0.0176(17) 0.0021(15) 0.0006(14) C16A 0.0273(19) 0.037(2) 0.0226(18) 0.0170(17) 0.0016(15) 0.0046(15) C16B 0.039(2) 0.033(2) 0.029(2) -0.0030(18) 0.0108(17) -0.0185(17) C16C 0.0244(18) 0.0151(16) 0.0311(19) 0.0047(15) 0.0053(15) -0.0021(13) C16D 0.058(3) 0.033(2) 0.031(2) 0.0179(18) -0.0007(19) 0.0105(19) C16E 0.131(4) 0.082(4) 0.069(3) 0.047(3) 0.066(3) 0.086(3) C16F 0.039(2) 0.046(2) 0.042(2) 0.024(2) 0.0268(18) 0.0202(18) C16G 0.029(2) 0.040(2) 0.037(2) 0.0220(18) 0.0123(16) 0.0164(16) C16H 0.0172(18) 0.040(2) 0.038(2) 0.0243(18) 0.0092(16) 0.0095(15) C17A 0.0290(19) 0.0312(19) 0.0214(17) 0.0099(16) -0.0029(15) -0.0084(15) C17B 0.048(2) 0.026(2) 0.031(2) 0.0045(17) 0.0085(18) -0.0142(17) C17C 0.0188(17) 0.0231(17) 0.0225(17) 0.0085(15) 0.0057(14) -0.0019(13) C17D 0.042(2) 0.029(2) 0.031(2) 0.0117(17) -0.0046(18) 0.0109(17) C17E 0.068(3) 0.079(3) 0.113(4) 0.052(3) 0.032(3) 0.049(3) C17F 0.0230(19) 0.047(2) 0.0276(19) 0.0191(18) 0.0093(15) 0.0065(16) C17G 0.032(2) 0.0240(18) 0.0338(19) 0.0106(16) 0.0132(16) 0.0094(15) C17H 0.033(2) 0.041(2) 0.032(2) 0.0118(18) 0.0139(17) 0.0082(17) C18A 0.0239(18) 0.0221(17) 0.0283(18) 0.0117(16) 0.0008(15) -0.0031(13) C18B 0.036(2) 0.0232(18) 0.0249(18) 0.0038(16) 0.0051(16) -0.0030(15) C18C 0.0186(17) 0.0210(17) 0.0203(16) 0.0096(14) 0.0067(13) 0.0046(13) C18D 0.030(2) 0.0257(18) 0.0213(17) 0.0035(16) -0.0018(15) 0.0006(15) C18E 0.039(2) 0.049(2) 0.070(3) 0.024(2) 0.015(2) 0.0249(19) C18F 0.0213(18) 0.0288(18) 0.0221(17) 0.0083(15) 0.0077(14) 0.0029(14) C18G 0.0215(18) 0.0268(18) 0.0248(17) 0.0092(16) 0.0071(14) 0.0038(14) C18H 0.025(2) 0.031(2) 0.0259(18) 0.0033(17) 0.0053(15) -0.0015(15) N1A 0.0240(15) 0.0158(14) 0.0155(14) 0.0036(11) 0.0002(12) 0.0013(11) N1B 0.0259(16) 0.0231(15) 0.0192(15) 0.0028(13) 0.0067(12) -0.0022(13) N1C 0.0144(14) 0.0165(13) 0.0176(13) 0.0046(12) -0.0020(11) -0.0023(11) N1D 0.0181(15) 0.0284(15) 0.0253(15) 0.0118(13) -0.0025(12) 0.0000(12) N1E 0.0231(16) 0.0272(16) 0.0262(16) 0.0087(14) -0.0029(12) 0.0080(12) N1F 0.0176(15) 0.0161(14) 0.0233(14) 0.0082(12) 0.0045(12) 0.0003(10) N1G 0.0169(14) 0.0175(14) 0.0189(14) 0.0060(13) 0.0036(11) -0.0022(11) N1H 0.0195(15) 0.0251(15) 0.0200(14) 0.0099(13) 0.0030(12) 0.0045(11) N3A 0.0204(14) 0.0177(14) 0.0165(13) 0.0045(12) 0.0041(11) -0.0005(10) N3B 0.0211(15) 0.0220(14) 0.0208(14) 0.0082(12) 0.0054(11) -0.0014(11) N3C 0.0159(14) 0.0143(13) 0.0192(13) 0.0074(11) 0.0000(11) -0.0009(10) N3D 0.0148(14) 0.0185(13) 0.0238(14) 0.0071(12) 0.0006(11) 0.0006(10) N3E 0.0132(14) 0.0188(14) 0.0203(14) 0.0027(12) 0.0012(11) 0.0004(10) N3F 0.0163(14) 0.0145(13) 0.0194(13) 0.0054(12) 0.0021(11) 0.0033(10) N3G 0.0125(13) 0.0194(14) 0.0174(13) 0.0020(12) 0.0033(11) -0.0007(10) N3H 0.0154(14) 0.0164(13) 0.0168(13) 0.0019(11) 0.0058(11) 0.0042(10) Ni1 0.0230(2) 0.0217(2) 0.0168(2) 0.00512(18) 0.00323(17) -0.00413(17) Ni2 0.0191(2) 0.0169(2) 0.0240(2) 0.00808(19) -0.00156(17) -0.00252(16) Ni3 0.0143(2) 0.0183(2) 0.0207(2) 0.00586(18) 0.00347(17) 0.00139(16) Cl1 0.0237(4) 0.0242(4) 0.0259(4) 0.0026(4) 0.0067(3) -0.0058(3) Cl2 0.0231(4) 0.0296(4) 0.0296(4) 0.0152(4) 0.0007(3) -0.0020(3) Cl3 0.0287(5) 0.0195(4) 0.0301(4) 0.0075(4) 0.0091(4) 0.0018(3) Cl4 0.0209(4) 0.0187(4) 0.0347(4) 0.0097(4) 0.0007(3) -0.0015(3) Cl5 0.0205(4) 0.0206(4) 0.0206(4) 0.0053(3) 0.0031(3) -0.0008(3) Cl6A 0.0400(11) 0.0359(9) 0.0254(8) 0.0187(7) 0.0060(9) 0.0148(9) O1A 0.026(2) 0.054(3) 0.043(3) 0.024(2) -0.010(2) 0.0029(18) O1B 0.014(4) 0.038(4) 0.021(3) 0.010(3) 0.003(3) 0.005(3) Cl6B 0.0204(12) 0.0346(13) 0.0353(14) 0.0189(13) -0.0085(11) -0.0072(9) O2 0.078(5) 0.061(5) 0.060(5) 0.028(4) 0.009(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2A N3A 1.316(3) . ? C2A N1A 1.341(3) . ? C2A H2A 0.9300 . ? C2B N3B 1.319(3) . ? C2B N1B 1.340(4) . ? C2B H2B 0.9300 . ? C2C N3C 1.326(3) . ? C2C N1C 1.335(3) . ? C2C H2C 0.9300 . ? C2D N3D 1.323(3) . ? C2D N1D 1.335(3) . ? C2D H2D 0.9300 . ? C2E N3E 1.330(3) . ? C2E N1E 1.337(3) . ? C2E H2E 0.9300 . ? C2F N3F 1.326(3) . ? C2F N1F 1.331(4) . ? C2F H2F 0.9300 . ? C2G N1G 1.319(3) . ? C2G N3G 1.331(3) . ? C2G H2G 0.9300 . ? C2H N1H 1.323(4) . ? C2H N3H 1.331(3) . ? C2H H2H 0.9300 . ? C4A C5A 1.372(4) . ? C4A N3A 1.402(3) . ? C4A C7A 1.478(4) . ? C4B C5B 1.369(4) . ? C4B N3B 1.399(3) . ? C4B C7B 1.470(4) . ? C4C C5C 1.371(4) . ? C4C N3C 1.391(3) . ? C4C C7C 1.485(4) . ? C4D C5D 1.370(4) . ? C4D N3D 1.395(4) . ? C4D C7D 1.473(4) . ? C4E C5E 1.368(4) . ? C4E N3E 1.398(3) . ? C4E C7E 1.472(4) . ? C4F C5F 1.374(4) . ? C4F N3F 1.400(3) . ? C4F C7F 1.475(4) . ? C4G C5G 1.371(4) . ? C4G N3G 1.404(3) . ? C4G C7G 1.478(4) . ? C4H C5H 1.357(4) . ? C4H N3H 1.399(3) . ? C4H C7H 1.479(4) . ? C5A N1A 1.386(3) . ? C5A C13A 1.470(4) . ? C5B N1B 1.365(4) . ? C5B C13B 1.474(4) . ? C5C N1C 1.374(3) . ? C5C C13C 1.470(4) . ? C5D N1D 1.375(4) . ? C5D C13D 1.472(4) . ? C5E N1E 1.376(4) . ? C5E C13E 1.456(4) . ? C5F N1F 1.383(3) . ? C5F C13F 1.465(4) . ? C5G N1G 1.386(3) . ? C5G C13G 1.471(4) . ? C5H N1H 1.382(3) . ? C5H C13H 1.472(4) . ? C7A C8A 1.378(4) . ? C7A C12A 1.391(4) . ? C7B C8B 1.394(4) . ? C7B C12B 1.395(4) . ? C7C C8C 1.383(4) . ? C7C C12C 1.398(4) . ? C7D C12D 1.385(4) . ? C7D C8D 1.388(4) . ? C7E C12E 1.392(4) . ? C7E C8E 1.401(4) . ? C7F C8F 1.388(4) . ? C7F C12F 1.390(4) . ? C7G C12G 1.382(4) . ? C7G C8G 1.384(4) . ? C7H C12H 1.389(4) . ? C7H C8H 1.392(4) . ? C8A C9A 1.388(4) . ? C8A H8A 0.9300 . ? C8B C9B 1.383(4) . ? C8B H8B 0.9300 . ? C8C C9C 1.383(4) . ? C8C H8C 0.9300 . ? C8D C9D 1.389(4) . ? C8D H8D 0.9300 . ? C8E C9E 1.388(4) . ? C8E H8E 0.9300 . ? C8F C9F 1.384(4) . ? C8F H8F 0.9300 . ? C8G C9G 1.395(4) . ? C8G H8G 0.9300 . ? C8H C9H 1.385(4) . ? C8H H8H 0.9300 . ? C9A C10A 1.377(4) . ? C9A H9A 0.9300 . ? C9B C10B 1.391(4) . ? C9B H9B 0.9300 . ? C9C C10C 1.386(4) . ? C9C H9C 0.9300 . ? C9D C10D 1.377(5) . ? C9D H9D 0.9300 . ? C9E C10E 1.378(4) . ? C9E H9E 0.9300 . ? C9F C10F 1.370(4) . ? C9F H9F 0.9300 . ? C9G C10G 1.378(4) . ? C9G H9G 0.9300 . ? C9H C10H 1.376(4) . ? C9H H9H 0.9300 . ? C10A C11A 1.373(4) . ? C10A H10A 0.9300 . ? C10B C11B 1.383(4) . ? C10B H10B 0.9300 . ? C10C C11C 1.375(4) . ? C10C H10C 0.9300 . ? C10D C11D 1.371(4) . ? C10D H10D 0.9300 . ? C10E C11E 1.385(4) . ? C10E H10E 0.9300 . ? C10F C11F 1.380(4) . ? C10F H10F 0.9300 . ? C10G C11G 1.372(4) . ? C10G H10G 0.9300 . ? C10H C11H 1.376(4) . ? C10H H10H 0.9300 . ? C11A C12A 1.388(4) . ? C11A H11A 0.9300 . ? C11B C12B 1.377(4) . ? C11B H11B 0.9300 . ? C11C C12C 1.386(4) . ? C11C H11C 0.9300 . ? C11D C12D 1.383(4) . ? C11D H11D 0.9300 . ? C11E C12E 1.391(4) . ? C11E H11E 0.9300 . ? C11F C12F 1.386(4) . ? C11F H11F 0.9300 . ? C11G C12G 1.402(4) . ? C11G H11G 0.9300 . ? C11H C12H 1.390(4) . ? C11H H11H 0.9300 . ? C12A H12A 0.9300 . ? C12B H12B 0.9300 . ? C12C H12C 0.9300 . ? C12D H12D 0.9300 . ? C12E H12E 0.9300 . ? C12F H12F 0.9300 . ? C12G H12G 0.9300 . ? C12H H12H 0.9300 . ? C13A C14A 1.394(4) . ? C13A C18A 1.401(4) . ? C13B C18B 1.389(4) . ? C13B C14B 1.394(4) . ? C13C C14C 1.388(4) . ? C13C C18C 1.398(3) . ? C13D C14D 1.385(4) . ? C13D C18D 1.398(4) . ? C13E C14E 1.368(4) . ? C13E C18E 1.370(4) . ? C13F C14F 1.394(4) . ? C13F C18F 1.409(4) . ? C13G C18G 1.384(4) . ? C13G C14G 1.396(3) . ? C13H C18H 1.389(4) . ? C13H C14H 1.391(4) . ? C14A C15A 1.378(4) . ? C14A H14A 0.9300 . ? C14B C15B 1.395(4) . ? C14B H14B 0.9300 . ? C14C C15C 1.380(4) . ? C14C H14C 0.9300 . ? C14D C15D 1.389(4) . ? C14D H14D 0.9300 . ? C14E C15E 1.393(5) . ? C14E H14E 0.9300 . ? C14F C15F 1.387(4) . ? C14F H14F 0.9300 . ? C14G C15G 1.377(4) . ? C14G H14G 0.9300 . ? C14H C15H 1.377(4) . ? C14H H14H 0.9300 . ? C15A C16A 1.380(4) . ? C15A H15A 0.9300 . ? C15B C16B 1.373(4) . ? C15B H15B 0.9300 . ? C15C C16C 1.375(4) . ? C15C H15C 0.9300 . ? C15D C16D 1.391(4) . ? C15D H15D 0.9300 . ? C15E C16E 1.357(5) . ? C15E H15E 0.9300 . ? C15F C16F 1.390(4) . ? C15F H15F 0.9300 . ? C15G C16G 1.380(4) . ? C15G H15G 0.9300 . ? C15H C16H 1.377(4) . ? C15H H15H 0.9300 . ? C16A C17A 1.382(4) . ? C16A H16A 0.9300 . ? C16B C17B 1.375(4) . ? C16B H16B 0.9300 . ? C16C C17C 1.384(4) . ? C16C H16C 0.9300 . ? C16D C17D 1.376(5) . ? C16D H16D 0.9300 . ? C16E C17E 1.351(5) . ? C16E H16E 0.9300 . ? C16F C17F 1.374(4) . ? C16F H16F 0.9300 . ? C16G C17G 1.373(4) . ? C16G H16G 0.9300 . ? C16H C17H 1.381(4) . ? C16H H16H 0.9300 . ? C17A C18A 1.389(4) . ? C17A H17A 0.9300 . ? C17B C18B 1.386(4) . ? C17B H17B 0.9300 . ? C17C C18C 1.376(4) . ? C17C H17C 0.9300 . ? C17D C18D 1.384(4) . ? C17D H17D 0.9300 . ? C17E C18E 1.371(5) . ? C17E H17E 0.9300 . ? C17F C18F 1.371(4) . ? C17F H17F 0.9300 . ? C17G C18G 1.386(4) . ? C17G H17G 0.9300 . ? C17H C18H 1.382(4) . ? C17H H17H 0.9300 . ? C18A H18A 0.9300 . ? C18B H18B 0.9300 . ? C18C H18C 0.9300 . ? C18D H18D 0.9300 . ? C18E H18E 0.9300 . ? C18F H18F 0.9300 . ? C18G H18G 0.9300 . ? C18H H18H 0.9300 . ? N1A H1A 0.859(17) . ? N1B H1B 0.831(17) . ? N1C H1C 0.863(17) . ? N1D H1D 0.867(17) . ? N1E H1E 0.860(17) . ? N1F H1F 0.866(17) . ? N1G H1G 0.845(16) . ? N1H H1H 0.876(17) . ? N3A Ni1 1.980(2) . ? N3B Ni1 1.992(2) . ? N3C Ni2 1.978(2) . ? N3D Ni2 1.985(2) . ? N3E Ni3 1.889(2) . ? N3F Ni3 1.901(3) . ? N3G Ni3 1.892(2) . ? N3H Ni3 1.885(2) . ? Ni1 Cl2 2.2385(8) . ? Ni1 Cl1 2.2848(9) . ? Ni2 Cl3 2.2326(9) . ? Ni2 Cl4 2.2793(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 N3A C2A N1A 111.2(2) . . ? N3A C2A H2A 124.4 . . ? N1A C2A H2A 124.4 . . ? N3B C2B N1B 111.0(3) . . ? N3B C2B H2B 124.5 . . ? N1B C2B H2B 124.5 . . ? N3C C2C N1C 110.6(2) . . ? N3C C2C H2C 124.7 . . ? N1C C2C H2C 124.7 . . ? N3D C2D N1D 111.0(3) . . ? N3D C2D H2D 124.5 . . ? N1D C2D H2D 124.5 . . ? N3E C2E N1E 110.7(3) . . ? N3E C2E H2E 124.6 . . ? N1E C2E H2E 124.6 . . ? N3F C2F N1F 110.8(3) . . ? N3F C2F H2F 124.6 . . ? N1F C2F H2F 124.6 . . ? N1G C2G N3G 110.8(2) . . ? N1G C2G H2G 124.6 . . ? N3G C2G H2G 124.6 . . ? N1H C2H N3H 111.6(2) . . ? N1H C2H H2H 124.2 . . ? N3H C2H H2H 124.2 . . ? C5A C4A N3A 108.3(2) . . ? C5A C4A C7A 131.1(3) . . ? N3A C4A C7A 120.6(2) . . ? C5B C4B N3B 108.4(3) . . ? C5B C4B C7B 129.1(3) . . ? N3B C4B C7B 122.5(3) . . ? C5C C4C N3C 108.8(2) . . ? C5C C4C C7C 131.0(3) . . ? N3C C4C C7C 120.1(2) . . ? C5D C4D N3D 108.7(3) . . ? C5D C4D C7D 129.4(3) . . ? N3D C4D C7D 121.8(2) . . ? C5E C4E N3E 108.9(3) . . ? C5E C4E C7E 127.3(3) . . ? N3E C4E C7E 123.8(2) . . ? C5F C4F N3F 108.6(2) . . ? C5F C4F C7F 129.7(3) . . ? N3F C4F C7F 121.7(3) . . ? C5G C4G N3G 108.4(2) . . ? C5G C4G C7G 132.3(2) . . ? N3G C4G C7G 119.3(2) . . ? C5H C4H N3H 109.0(2) . . ? C5H C4H C7H 128.8(3) . . ? N3H C4H C7H 122.2(3) . . ? C4A C5A N1A 105.9(2) . . ? C4A C5A C13A 133.3(3) . . ? N1A C5A C13A 120.6(2) . . ? N1B C5B C4B 106.2(3) . . ? N1B C5B C13B 122.1(3) . . ? C4B C5B C13B 131.6(3) . . ? C4C C5C N1C 105.5(2) . . ? C4C C5C C13C 134.4(3) . . ? N1C C5C C13C 120.1(2) . . ? C4D C5D N1D 105.7(3) . . ? C4D C5D C13D 132.8(3) . . ? N1D C5D C13D 121.5(2) . . ? C4E C5E N1E 105.7(3) . . ? C4E C5E C13E 132.7(3) . . ? N1E C5E C13E 121.6(3) . . ? C4F C5F N1F 105.4(3) . . ? C4F C5F C13F 132.5(3) . . ? N1F C5F C13F 121.7(3) . . ? C4G C5G N1G 105.3(2) . . ? C4G C5G C13G 134.4(3) . . ? N1G C5G C13G 120.4(2) . . ? C4H C5H N1H 106.1(3) . . ? C4H C5H C13H 133.6(3) . . ? N1H C5H C13H 120.2(3) . . ? C8A C7A C12A 118.9(3) . . ? C8A C7A C4A 121.7(3) . . ? C12A C7A C4A 119.3(3) . . ? C8B C7B C12B 118.5(3) . . ? C8B C7B C4B 121.4(3) . . ? C12B C7B C4B 120.0(3) . . ? C8C C7C C12C 118.7(3) . . ? C8C C7C C4C 120.4(3) . . ? C12C C7C C4C 120.8(3) . . ? C12D C7D C8D 118.6(3) . . ? C12D C7D C4D 121.5(3) . . ? C8D C7D C4D 119.9(3) . . ? C12E C7E C8E 118.8(3) . . ? C12E C7E C4E 120.9(2) . . ? C8E C7E C4E 120.2(3) . . ? C8F C7F C12F 118.6(3) . . ? C8F C7F C4F 119.9(3) . . ? C12F C7F C4F 121.5(2) . . ? C12G C7G C8G 119.0(3) . . ? C12G C7G C4G 121.8(3) . . ? C8G C7G C4G 119.2(3) . . ? C12H C7H C8H 119.3(3) . . ? C12H C7H C4H 120.3(3) . . ? C8H C7H C4H 120.4(3) . . ? C7A C8A C9A 120.6(3) . . ? C7A C8A H8A 119.7 . . ? C9A C8A H8A 119.7 . . ? C9B C8B C7B 120.9(3) . . ? C9B C8B H8B 119.5 . . ? C7B C8B H8B 119.5 . . ? C9C C8C C7C 120.9(3) . . ? C9C C8C H8C 119.5 . . ? C7C C8C H8C 119.5 . . ? C9D C8D C7D 119.9(3) . . ? C9D C8D H8D 120.1 . . ? C7D C8D H8D 120.1 . . ? C9E C8E C7E 119.8(3) . . ? C9E C8E H8E 120.1 . . ? C7E C8E H8E 120.1 . . ? C9F C8F C7F 120.8(3) . . ? C9F C8F H8F 119.6 . . ? C7F C8F H8F 119.6 . . ? C7G C8G C9G 120.4(3) . . ? C7G C8G H8G 119.8 . . ? C9G C8G H8G 119.8 . . ? C9H C8H C7H 120.8(3) . . ? C9H C8H H8H 119.6 . . ? C7H C8H H8H 119.6 . . ? C10A C9A C8A 120.4(3) . . ? C10A C9A H9A 119.8 . . ? C8A C9A H9A 119.8 . . ? C8B C9B C10B 119.9(3) . . ? C8B C9B H9B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8C C9C C10C 119.9(3) . . ? C8C C9C H9C 120.1 . . ? C10C C9C H9C 120.1 . . ? C10D C9D C8D 120.8(3) . . ? C10D C9D H9D 119.6 . . ? C8D C9D H9D 119.6 . . ? C10E C9E C8E 120.8(3) . . ? C10E C9E H9E 119.6 . . ? C8E C9E H9E 119.6 . . ? C10F C9F C8F 120.0(3) . . ? C10F C9F H9F 120.0 . . ? C8F C9F H9F 120.0 . . ? C10G C9G C8G 120.0(3) . . ? C10G C9G H9G 120.0 . . ? C8G C9G H9G 120.0 . . ? C10H C9H C8H 119.3(3) . . ? C10H C9H H9H 120.4 . . ? C8H C9H H9H 120.4 . . ? C11A C10A C9A 119.4(3) . . ? C11A C10A H10A 120.3 . . ? C9A C10A H10A 120.3 . . ? C11B C10B C9B 119.4(3) . . ? C11B C10B H10B 120.3 . . ? C9B C10B H10B 120.3 . . ? C11C C10C C9C 119.9(3) . . ? C11C C10C H10C 120.1 . . ? C9C C10C H10C 120.1 . . ? C11D C10D C9D 119.4(3) . . ? C11D C10D H10D 120.3 . . ? C9D C10D H10D 120.3 . . ? C9E C10E C11E 120.2(3) . . ? C9E C10E H10E 119.9 . . ? C11E C10E H10E 119.9 . . ? C9F C10F C11F 120.3(3) . . ? C9F C10F H10F 119.9 . . ? C11F C10F H10F 119.9 . . ? C11G C10G C9G 120.1(3) . . ? C11G C10G H10G 119.9 . . ? C9G C10G H10G 119.9 . . ? C11H C10H C9H 120.7(3) . . ? C11H C10H H10H 119.7 . . ? C9H C10H H10H 119.7 . . ? C10A C11A C12A 120.7(3) . . ? C10A C11A H11A 119.7 . . ? C12A C11A H11A 119.7 . . ? C12B C11B C10B 120.7(3) . . ? C12B C11B H11B 119.6 . . ? C10B C11B H11B 119.6 . . ? C10C C11C C12C 120.3(3) . . ? C10C C11C H11C 119.8 . . ? C12C C11C H11C 119.8 . . ? C10D C11D C12D 120.2(3) . . ? C10D C11D H11D 119.9 . . ? C12D C11D H11D 119.9 . . ? C10E C11E C12E 119.4(3) . . ? C10E C11E H11E 120.3 . . ? C12E C11E H11E 120.3 . . ? C10F C11F C12F 119.9(3) . . ? C10F C11F H11F 120.1 . . ? C12F C11F H11F 120.1 . . ? C10G C11G C12G 119.9(3) . . ? C10G C11G H11G 120.1 . . ? C12G C11G H11G 120.1 . . ? C10H C11H C12H 120.3(3) . . ? C10H C11H H11H 119.8 . . ? C12H C11H H11H 119.8 . . ? C7A C12A C11A 120.1(3) . . ? C7A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C11B C12B C7B 120.5(3) . . ? C11B C12B H12B 119.7 . . ? C7B C12B H12B 119.7 . . ? C11C C12C C7C 120.2(3) . . ? C11C C12C H12C 119.9 . . ? C7C C12C H12C 119.9 . . ? C11D C12D C7D 121.0(3) . . ? C11D C12D H12D 119.5 . . ? C7D C12D H12D 119.5 . . ? C11E C12E C7E 121.0(3) . . ? C11E C12E H12E 119.5 . . ? C7E C12E H12E 119.5 . . ? C11F C12F C7F 120.5(3) . . ? C11F C12F H12F 119.8 . . ? C7F C12F H12F 119.8 . . ? C7G C12G C11G 120.5(3) . . ? C7G C12G H12G 119.7 . . ? C11G C12G H12G 119.7 . . ? C7H C12H C11H 119.6(3) . . ? C7H C12H H12H 120.2 . . ? C11H C12H H12H 120.2 . . ? C14A C13A C18A 117.9(3) . . ? C14A C13A C5A 121.9(2) . . ? C18A C13A C5A 120.2(3) . . ? C18B C13B C14B 118.9(3) . . ? C18B C13B C5B 120.4(3) . . ? C14B C13B C5B 120.7(3) . . ? C14C C13C C18C 118.3(2) . . ? C14C C13C C5C 122.1(2) . . ? C18C C13C C5C 119.6(2) . . ? C14D C13D C18D 119.4(3) . . ? C14D C13D C5D 121.4(3) . . ? C18D C13D C5D 119.2(3) . . ? C14E C13E C18E 118.1(3) . . ? C14E C13E C5E 121.6(3) . . ? C18E C13E C5E 120.3(3) . . ? C14F C13F C18F 118.3(3) . . ? C14F C13F C5F 121.8(3) . . ? C18F C13F C5F 119.6(3) . . ? C18G C13G C14G 118.2(3) . . ? C18G C13G C5G 120.8(2) . . ? C14G C13G C5G 120.9(2) . . ? C18H C13H C14H 118.8(3) . . ? C18H C13H C5H 120.4(3) . . ? C14H C13H C5H 120.8(3) . . ? C15A C14A C13A 120.9(3) . . ? C15A C14A H14A 119.5 . . ? C13A C14A H14A 119.5 . . ? C13B C14B C15B 119.7(3) . . ? C13B C14B H14B 120.1 . . ? C15B C14B H14B 120.1 . . ? C15C C14C C13C 120.4(3) . . ? C15C C14C H14C 119.8 . . ? C13C C14C H14C 119.8 . . ? C13D C14D C15D 120.0(3) . . ? C13D C14D H14D 120.0 . . ? C15D C14D H14D 120.0 . . ? C13E C14E C15E 120.5(3) . . ? C13E C14E H14E 119.8 . . ? C15E C14E H14E 119.8 . . ? C15F C14F C13F 120.0(3) . . ? C15F C14F H14F 120.0 . . ? C13F C14F H14F 120.0 . . ? C15G C14G C13G 120.7(3) . . ? C15G C14G H14G 119.7 . . ? C13G C14G H14G 119.7 . . ? C15H C14H C13H 120.0(3) . . ? C15H C14H H14H 120.0 . . ? C13H C14H H14H 120.0 . . ? C14A C15A C16A 120.9(3) . . ? C14A C15A H15A 119.5 . . ? C16A C15A H15A 119.5 . . ? C16B C15B C14B 120.0(3) . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C16C C15C C14C 120.9(3) . . ? C16C C15C H15C 119.5 . . ? C14C C15C H15C 119.5 . . ? C14D C15D C16D 119.9(3) . . ? C14D C15D H15D 120.0 . . ? C16D C15D H15D 120.0 . . ? C16E C15E C14E 120.3(4) . . ? C16E C15E H15E 119.9 . . ? C14E C15E H15E 119.9 . . ? C14F C15F C16F 120.4(3) . . ? C14F C15F H15F 119.8 . . ? C16F C15F H15F 119.8 . . ? C14G C15G C16G 120.2(3) . . ? C14G C15G H15G 119.9 . . ? C16G C15G H15G 119.9 . . ? C14H C15H C16H 120.9(3) . . ? C14H C15H H15H 119.6 . . ? C16H C15H H15H 119.6 . . ? C17A C16A C15A 119.2(3) . . ? C17A C16A H16A 120.4 . . ? C15A C16A H16A 120.4 . . ? C17B C16B C15B 120.9(3) . . ? C17B C16B H16B 119.5 . . ? C15B C16B H16B 119.5 . . ? C15C C16C C17C 119.4(3) . . ? C15C C16C H16C 120.3 . . ? C17C C16C H16C 120.3 . . ? C17D C16D C15D 120.4(3) . . ? C17D C16D H16D 119.8 . . ? C15D C16D H16D 119.8 . . ? C17E C16E C15E 119.3(4) . . ? C17E C16E H16E 120.4 . . ? C15E C16E H16E 120.4 . . ? C17F C16F C15F 120.0(3) . . ? C17F C16F H16F 120.0 . . ? C15F C16F H16F 120.0 . . ? C17G C16G C15G 120.0(3) . . ? C17G C16G H16G 120.0 . . ? C15G C16G H16G 120.0 . . ? C15H C16H C17H 119.7(3) . . ? C15H C16H H16H 120.1 . . ? C17H C16H H16H 120.1 . . ? C16A C17A C18A 120.4(3) . . ? C16A C17A H17A 119.8 . . ? C18A C17A H17A 119.8 . . ? C16B C17B C18B 119.3(3) . . ? C16B C17B H17B 120.4 . . ? C18B C17B H17B 120.4 . . ? C18C C17C C16C 120.1(3) . . ? C18C C17C H17C 119.9 . . ? C16C C17C H17C 119.9 . . ? C16D C17D C18D 119.7(3) . . ? C16D C17D H17D 120.2 . . ? C18D C17D H17D 120.2 . . ? C16E C17E C18E 120.9(4) . . ? C16E C17E H17E 119.6 . . ? C18E C17E H17E 119.6 . . ? C18F C17F C16F 120.0(3) . . ? C18F C17F H17F 120.0 . . ? C16F C17F H17F 120.0 . . ? C16G C17G C18G 119.8(3) . . ? C16G C17G H17G 120.1 . . ? C18G C17G H17G 120.1 . . ? C18H C17H C16H 119.7(3) . . ? C18H C17H H17H 120.1 . . ? C16H C17H H17H 120.1 . . ? C17A C18A C13A 120.6(3) . . ? C17A C18A H18A 119.7 . . ? C13A C18A H18A 119.7 . . ? C17B C18B C13B 121.0(3) . . ? C17B C18B H18B 119.5 . . ? C13B C18B H18B 119.5 . . ? C17C C18C C13C 120.9(3) . . ? C17C C18C H18C 119.6 . . ? C13C C18C H18C 119.6 . . ? C17D C18D C13D 120.6(3) . . ? C17D C18D H18D 119.7 . . ? C13D C18D H18D 119.7 . . ? C17E C18E C13E 121.0(4) . . ? C17E C18E H18E 119.5 . . ? C13E C18E H18E 119.5 . . ? C17F C18F C13F 121.2(3) . . ? C17F C18F H18F 119.4 . . ? C13F C18F H18F 119.4 . . ? C13G C18G C17G 121.1(3) . . ? C13G C18G H18G 119.5 . . ? C17G C18G H18G 119.5 . . ? C17H C18H C13H 120.8(3) . . ? C17H C18H H18H 119.6 . . ? C13H C18H H18H 119.6 . . ? C2A N1A C5A 108.1(2) . . ? C2A N1A H1A 121.7(19) . . ? C5A N1A H1A 129.9(19) . . ? C2B N1B C5B 108.4(3) . . ? C2B N1B H1B 121(2) . . ? C5B N1B H1B 130(2) . . ? C2C N1C C5C 108.8(2) . . ? C2C N1C H1C 122.9(19) . . ? C5C N1C H1C 127.7(19) . . ? C2D N1D C5D 108.6(2) . . ? C2D N1D H1D 124(2) . . ? C5D N1D H1D 127(2) . . ? C2E N1E C5E 108.8(3) . . ? C2E N1E H1E 130(2) . . ? C5E N1E H1E 121(2) . . ? C2F N1F C5F 109.0(2) . . ? C2F N1F H1F 128(2) . . ? C5F N1F H1F 123(2) . . ? C2G N1G C5G 109.4(2) . . ? C2G N1G H1G 123.9(19) . . ? C5G N1G H1G 126.5(18) . . ? C2H N1H C5H 108.1(3) . . ? C2H N1H H1H 121(2) . . ? C5H N1H H1H 130(2) . . ? C2A N3A C4A 106.5(2) . . ? C2A N3A Ni1 121.28(19) . . ? C4A N3A Ni1 129.11(19) . . ? C2B N3B C4B 106.0(2) . . ? C2B N3B Ni1 122.9(2) . . ? C4B N3B Ni1 130.7(2) . . ? C2C N3C C4C 106.2(2) . . ? C2C N3C Ni2 124.31(19) . . ? C4C N3C Ni2 128.49(18) . . ? C2D N3D C4D 106.0(2) . . ? C2D N3D Ni2 120.9(2) . . ? C4D N3D Ni2 130.85(18) . . ? C2E N3E C4E 105.9(2) . . ? C2E N3E Ni3 122.6(2) . . ? C4E N3E Ni3 129.7(2) . . ? C2F N3F C4F 106.2(3) . . ? C2F N3F Ni3 120.4(2) . . ? C4F N3F Ni3 131.11(19) . . ? C2G N3G C4G 106.1(2) . . ? C2G N3G Ni3 122.89(18) . . ? C4G N3G Ni3 129.90(18) . . ? C2H N3H C4H 105.2(2) . . ? C2H N3H Ni3 122.87(19) . . ? C4H N3H Ni3 131.7(2) . . ? N3A Ni1 N3B 108.52(10) . . ? N3A Ni1 Cl2 103.00(7) . . ? N3B Ni1 Cl2 129.15(7) . . ? N3A Ni1 Cl1 103.68(7) . . ? N3B Ni1 Cl1 98.83(8) . . ? Cl2 Ni1 Cl1 111.30(3) . . ? N3C Ni2 N3D 99.85(9) . . ? N3C Ni2 Cl3 118.69(8) . . ? N3D Ni2 Cl3 102.10(8) . . ? N3C Ni2 Cl4 100.27(7) . . ? N3D Ni2 Cl4 115.03(7) . . ? Cl3 Ni2 Cl4 119.75(3) . . ? N3H Ni3 N3E 90.43(10) . . ? N3H Ni3 N3G 88.80(10) . . ? N3E Ni3 N3G 176.71(10) . . ? N3H Ni3 N3F 176.89(9) . . ? N3E Ni3 N3F 90.32(10) . . ? N3G Ni3 N3F 90.62(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.932 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.071 # start Validation Reply Form _vrf_PLAT220_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O ; RESPONSE: All atomic species have been correctly identified. This alert is due to the higher thermal ellipsoids of the atoms of one phenyl ring compared with the remaining ones of the complex. ; _vrf_PLAT311_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O ; RESPONSE: It was not possible to locate the hydrogen atoms of the lattice water molecules O1 and O2 from a difference map. ; _vrf_PLAT041_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O ; RESPONSE: The missing (not located by a difference synthesis) H-atoms of the crystallization water molecules O1 and O2 have been included in the sum and moiety formula and the Mr, Dx and F(000) have been modified accordingly. These modifications account for the differences detected in the relevant data items. ; _vrf_PLAT077_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O ; RESPONSE: Due to partially occupied (solvent) sites. ; _vrf_FORMU01_6-Ni{HL'}4_{NiCl2{HL'}2}2_Cl2_1.35H2O ; RESPONSE: See comment above for PLAT041 ALERT. ; # end Validation Reply Form #===END data_7-Ni{HL'}4_Br2_4.7MeCN #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881068' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 N8 Ni 2+, 4.7(C2 H3 N), 2(Br 1-)' _chemical_formula_sum 'C69.40 H62.10 Br2 N12.70 Ni' _chemical_formula_weight 1292.55 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2832(4) _cell_length_b 15.2035(6) _cell_length_c 19.4459(6) _cell_angle_alpha 69.188(3) _cell_angle_beta 82.117(2) _cell_angle_gamma 68.905(3) _cell_volume 3166.86(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14849 _cell_measurement_theta_min 3.0916 _cell_measurement_theta_max 30.3256 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1330.8 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9472 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55461 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 28.50 _reflns_number_total 15930 _reflns_number_gt 8870 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)' _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; The structure is disordered. The disorder mainly affects the atoms of the C13D-C18D phenyl ring, Br2 ion (one of the two bromide counterions) which was modelled in two neighbouring sites (Br2A and Br2B) in a 60:40 ratio after competitive refinement, as well as the crystallization acetonitrile molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15930 _refine_ls_number_parameters 801 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.12572(3) 0.70046(2) 0.247685(19) 0.01764(9) Uani 1 1 d . . . N1C N 0.43366(19) 0.74324(16) 0.21053(12) 0.0187(5) Uani 1 1 d D . . H1C H 0.4866(19) 0.7552(19) 0.1812(13) 0.028 Uiso 1 1 d D . . N1B N 0.31259(19) 0.42471(16) 0.24890(12) 0.0197(5) Uani 1 1 d D . . H1B H 0.3642(18) 0.3676(12) 0.2674(14) 0.030 Uiso 1 1 d D . . N1A N -0.17753(19) 0.72150(17) 0.18102(13) 0.0198(5) Uani 1 1 d D . . H1A H -0.2333(17) 0.7544(18) 0.1513(12) 0.030 Uiso 1 1 d D . . N1D N -0.0711(2) 0.90978(18) 0.33572(14) 0.0254(6) Uani 1 1 d . . . H1D H -0.118(3) 0.925(2) 0.3675(17) 0.038 Uiso 1 1 d . . . N3C N 0.27135(18) 0.71433(15) 0.25235(12) 0.0183(5) Uani 1 1 d . . . N3B N 0.20652(17) 0.58217(15) 0.22436(12) 0.0168(5) Uani 1 1 d . . . N3A N -0.01954(18) 0.68673(16) 0.23943(12) 0.0177(5) Uani 1 1 d . . . N3D N 0.04484(18) 0.81691(16) 0.27340(12) 0.0194(5) Uani 1 1 d . . . C2C C 0.3433(2) 0.72722(19) 0.19447(15) 0.0202(6) Uani 1 1 d . . . H2C H 0.3313 0.7252 0.1490 0.024 Uiso 1 1 calc R . . C2B C 0.2829(2) 0.5043(2) 0.27036(15) 0.0200(6) Uani 1 1 d . . . H2B H 0.3117 0.5051 0.3118 0.024 Uiso 1 1 calc R . . C2A C -0.0974(2) 0.7556(2) 0.18919(14) 0.0191(6) Uani 1 1 d . . . H2A H -0.0954 0.8195 0.1632 0.023 Uiso 1 1 calc R . . C2D C -0.0276(2) 0.8193(2) 0.33052(15) 0.0226(7) Uani 1 1 d . . . H2D H -0.0455 0.7642 0.3628 0.027 Uiso 1 1 calc R . . C4C C 0.3212(2) 0.72257(19) 0.30861(15) 0.0184(6) Uani 1 1 d . . . C4B C 0.1879(2) 0.54976(19) 0.16986(15) 0.0172(6) Uani 1 1 d . . . C4A C -0.0552(2) 0.60360(19) 0.26559(14) 0.0179(6) Uani 1 1 d . . . C4D C 0.0474(2) 0.9136(2) 0.24052(15) 0.0189(6) Uani 1 1 d . . . C5C C 0.4240(2) 0.73990(19) 0.28264(15) 0.0185(6) Uani 1 1 d . . . C5B C 0.2540(2) 0.4510(2) 0.18546(15) 0.0194(6) Uani 1 1 d . . . C5A C -0.1550(2) 0.62494(19) 0.22981(15) 0.0182(6) Uani 1 1 d . . . C5D C -0.0254(2) 0.9723(2) 0.27912(15) 0.0233(7) Uani 1 1 d . . . C7C C 0.2663(2) 0.7168(2) 0.38108(15) 0.0204(6) Uani 1 1 d . . . C7B C 0.1104(2) 0.6152(2) 0.10678(14) 0.0198(6) Uani 1 1 d . . . C7A C 0.0089(2) 0.5115(2) 0.32328(15) 0.0187(6) Uani 1 1 d . . . C7D C 0.1193(2) 0.93977(19) 0.17382(15) 0.0188(6) Uani 1 1 d . . . C8C C 0.2265(3) 0.6385(2) 0.42258(16) 0.0297(7) Uani 1 1 d . . . H8C H 0.2359 0.5871 0.4046 0.036 Uiso 1 1 calc R . . C8B C 0.1105(2) 0.7128(2) 0.06933(16) 0.0254(7) Uani 1 1 d . . . H8B H 0.1598 0.7363 0.0847 0.031 Uiso 1 1 calc R . . C8A C 0.0446(2) 0.5149(2) 0.38665(15) 0.0229(7) Uani 1 1 d . . . H8A H 0.0261 0.5764 0.3932 0.027 Uiso 1 1 calc R . . C8D C 0.0927(2) 0.9370(2) 0.10828(15) 0.0243(7) Uani 1 1 d . . . H8D H 0.0284 0.9195 0.1059 0.029 Uiso 1 1 calc R . . C9C C 0.1729(3) 0.6363(3) 0.49070(17) 0.0379(9) Uani 1 1 d . . . H9C H 0.1451 0.5843 0.5175 0.046 Uiso 1 1 calc R . . C9B C 0.0388(3) 0.7743(2) 0.01031(16) 0.0330(8) Uani 1 1 d . . . H9B H 0.0398 0.8389 -0.0140 0.040 Uiso 1 1 calc R . . C9A C 0.1070(2) 0.4291(2) 0.44023(16) 0.0271(7) Uani 1 1 d . . . H9A H 0.1307 0.4330 0.4822 0.033 Uiso 1 1 calc R . . C9D C 0.1605(3) 0.9598(2) 0.04575(16) 0.0297(7) Uani 1 1 d . . . H9D H 0.1414 0.9579 0.0018 0.036 Uiso 1 1 calc R . . C10C C 0.1609(3) 0.7100(3) 0.51829(19) 0.0453(9) Uani 1 1 d . . . H10C H 0.1257 0.7079 0.5641 0.054 Uiso 1 1 calc R . . C10B C -0.0350(3) 0.7397(2) -0.01285(16) 0.0337(8) Uani 1 1 d . . . H10B H -0.0846 0.7814 -0.0522 0.040 Uiso 1 1 calc R . . C10A C 0.1339(2) 0.3373(2) 0.43108(16) 0.0290(8) Uani 1 1 d . . . H10A H 0.1754 0.2790 0.4669 0.035 Uiso 1 1 calc R . . C10D C 0.2557(3) 0.9853(2) 0.04877(17) 0.0302(8) Uani 1 1 d . . . H10D H 0.3014 1.0006 0.0069 0.036 Uiso 1 1 calc R . . C11C C 0.2006(3) 0.7872(3) 0.47900(19) 0.0483(10) Uani 1 1 d . . . H11C H 0.1935 0.8371 0.4982 0.058 Uiso 1 1 calc R . . C11B C -0.0344(2) 0.6434(2) 0.02279(17) 0.0309(7) Uani 1 1 d . . . H11B H -0.0827 0.6198 0.0066 0.037 Uiso 1 1 calc R . . C11A C 0.0988(2) 0.3330(2) 0.36881(16) 0.0274(7) Uani 1 1 d . . . H11A H 0.1174 0.2713 0.3625 0.033 Uiso 1 1 calc R . . C11D C 0.2836(2) 0.9881(2) 0.11450(18) 0.0289(7) Uani 1 1 d . . . H11D H 0.3480 1.0054 0.1168 0.035 Uiso 1 1 calc R . . C12C C 0.2515(3) 0.7905(2) 0.41028(17) 0.0349(8) Uani 1 1 d . . . H12C H 0.2764 0.8441 0.3832 0.042 Uiso 1 1 calc R . . C12B C 0.0371(2) 0.5814(2) 0.08228(15) 0.0238(7) Uani 1 1 d . . . H12B H 0.0361 0.5167 0.1060 0.029 Uiso 1 1 calc R . . C12A C 0.0362(2) 0.4189(2) 0.31508(16) 0.0239(7) Uani 1 1 d . . . H12A H 0.0123 0.4145 0.2734 0.029 Uiso 1 1 calc R . . C12D C 0.2154(2) 0.96521(19) 0.17667(16) 0.0237(7) Uani 1 1 d . . . H12D H 0.2345 0.9670 0.2207 0.028 Uiso 1 1 calc R . . C13C C 0.5176(2) 0.7451(2) 0.31944(15) 0.0219(7) Uani 1 1 d . . . C13B C 0.2694(2) 0.3792(2) 0.14764(15) 0.0198(6) Uani 1 1 d . . . C13A C -0.2355(2) 0.57040(19) 0.23701(15) 0.0187(6) Uani 1 1 d . . . C13D C -0.0646(3) 1.0805(2) 0.26646(18) 0.0354(8) Uani 1 1 d . . . C14C C 0.5529(2) 0.6781(2) 0.38910(16) 0.0325(8) Uani 1 1 d . . . H14C H 0.5139 0.6331 0.4135 0.039 Uiso 1 1 calc R . . C14B C 0.3086(2) 0.3960(2) 0.07504(15) 0.0240(7) Uani 1 1 d . . . H14B H 0.3244 0.4547 0.0493 0.029 Uiso 1 1 calc R . . C14A C -0.2667(2) 0.5157(2) 0.30601(16) 0.0254(7) Uani 1 1 d . . . H14A H -0.2325 0.5100 0.3479 0.030 Uiso 1 1 calc R . . C14D C -0.0208(3) 1.1441(2) 0.2160(2) 0.0561(11) Uani 1 1 d U . . H14D H 0.0378 1.1198 0.1851 0.067 Uiso 1 1 calc R . . C15C C 0.6451(3) 0.6778(3) 0.42231(18) 0.0420(9) Uani 1 1 d . . . H15C H 0.6687 0.6321 0.4688 0.050 Uiso 1 1 calc R . . C15B C 0.3242(2) 0.3273(2) 0.04103(16) 0.0256(7) Uani 1 1 d . . . H15B H 0.3516 0.3392 -0.0073 0.031 Uiso 1 1 calc R . . C15A C -0.3482(3) 0.4697(2) 0.31288(18) 0.0328(8) Uani 1 1 d . . . H15A H -0.3680 0.4326 0.3592 0.039 Uiso 1 1 calc R . . C15D C -0.0573(3) 1.2446(2) 0.2067(2) 0.0506(10) Uani 1 1 d U . . H15D H -0.0200 1.2844 0.1714 0.061 Uiso 1 1 calc R . . C16C C 0.7029(3) 0.7451(3) 0.38693(18) 0.0438(9) Uani 1 1 d . . . H16C H 0.7644 0.7456 0.4096 0.053 Uiso 1 1 calc R . . C16B C 0.2996(2) 0.2407(2) 0.07789(17) 0.0273(7) Uani 1 1 d . . . H16B H 0.3086 0.1949 0.0543 0.033 Uiso 1 1 calc R . . C16A C -0.3998(3) 0.4788(2) 0.25142(19) 0.0354(8) Uani 1 1 d . . . H16A H -0.4556 0.4486 0.2563 0.042 Uiso 1 1 calc R . . C16D C -0.1411(3) 1.2854(3) 0.2452(2) 0.0566(11) Uani 1 1 d U . . H16D H -0.1569 1.3507 0.2435 0.068 Uiso 1 1 calc R . . C17C C 0.6682(3) 0.8111(3) 0.31783(18) 0.0387(9) Uani 1 1 d . . . H17C H 0.7072 0.8562 0.2937 0.046 Uiso 1 1 calc R . . C17B C 0.2613(3) 0.2222(2) 0.15025(17) 0.0318(8) Uani 1 1 d . . . H17B H 0.2453 0.1635 0.1756 0.038 Uiso 1 1 calc R . . C17A C -0.3696(3) 0.5325(2) 0.18214(18) 0.0348(8) Uani 1 1 d . . . H17A H -0.4046 0.5381 0.1406 0.042 Uiso 1 1 calc R . . C17D C -0.2076(5) 1.2277(3) 0.2896(3) 0.112(2) Uani 1 1 d U . . H17D H -0.2759 1.2565 0.3124 0.134 Uiso 1 1 calc R . . C18C C 0.5767(2) 0.8118(2) 0.28359(16) 0.0284(7) Uani 1 1 d . . . H18C H 0.5545 0.8568 0.2367 0.034 Uiso 1 1 calc R . . C18B C 0.2469(2) 0.2903(2) 0.18476(16) 0.0289(7) Uani 1 1 d . . . H18B H 0.2217 0.2770 0.2336 0.035 Uiso 1 1 calc R . . C18A C -0.2871(2) 0.5778(2) 0.17508(16) 0.0253(7) Uani 1 1 d . . . H18A H -0.2661 0.6133 0.1286 0.030 Uiso 1 1 calc R . . C18D C -0.1684(5) 1.1255(3) 0.2987(3) 0.1065(19) Uani 1 1 d U . . H18D H -0.2127 1.0867 0.3270 0.128 Uiso 1 1 calc R . . N1 N 0.4574(2) 0.3522(2) 0.39664(16) 0.0544(9) Uani 1 1 d . . . C19 C 0.4859(3) 0.2714(3) 0.4345(2) 0.0437(9) Uani 1 1 d . . . C20 C 0.5202(4) 0.1693(3) 0.4847(2) 0.0672(12) Uani 1 1 d . . . H20A H 0.4558 0.1450 0.4924 0.101 Uiso 1 1 calc R . . H20B H 0.5422 0.1672 0.5309 0.101 Uiso 1 1 calc R . . H20C H 0.5852 0.1280 0.4641 0.101 Uiso 1 1 calc R . . N2 N 0.4837(3) 0.2197(3) 0.2829(2) 0.0803(12) Uani 1 1 d . . . C21 C 0.4833(4) 0.1405(4) 0.3152(3) 0.0736(14) Uani 1 1 d . . . C22 C 0.4811(5) 0.0405(4) 0.3584(3) 0.117(2) Uani 1 1 d U . . H22A H 0.4187 0.0453 0.3940 0.176 Uiso 1 1 calc R . . H22B H 0.5540 0.0012 0.3832 0.176 Uiso 1 1 calc R . . H22C H 0.4690 0.0093 0.3263 0.176 Uiso 1 1 calc R . . N3 N 0.7867(2) 0.0020(2) 0.15205(16) 0.0456(8) Uani 1 1 d . . . C23 C 0.6932(3) 0.0410(2) 0.13380(18) 0.0337(8) Uani 1 1 d . . . C24 C 0.5729(3) 0.0916(3) 0.1089(2) 0.0552(11) Uani 1 1 d . . . H24A H 0.5696 0.1462 0.0641 0.083 Uiso 1 1 calc R . . H24B H 0.5254 0.1166 0.1459 0.083 Uiso 1 1 calc R . . H24C H 0.5444 0.0453 0.1003 0.083 Uiso 1 1 calc R . . N4 N 0.4075(3) 0.6344(3) 0.0356(2) 0.0768(12) Uani 1 1 d . . . C25 C 0.3820(4) 0.6520(3) -0.0219(3) 0.0560(11) Uani 1 1 d . . . C26 C 0.3461(5) 0.6777(4) -0.0966(3) 0.0988(17) Uani 1 1 d U . . H26A H 0.4127 0.6756 -0.1290 0.148 Uiso 1 1 calc R . . H26B H 0.2895 0.7438 -0.1117 0.148 Uiso 1 1 calc R . . H26C H 0.3122 0.6308 -0.0986 0.148 Uiso 1 1 calc R . . N5 N 0.2360(5) 1.0491(4) 0.3293(3) 0.0598(14) Uani 0.70 1 d PD . . C27 C 0.1610(5) 1.0590(4) 0.3630(3) 0.0471(15) Uani 0.70 1 d PD . . C28 C 0.0556(5) 1.0705(4) 0.4122(3) 0.0767(19) Uani 0.70 1 d P . . H28A H 0.0354 1.0108 0.4274 0.115 Uiso 0.70 1 calc PR . . H28B H -0.0085 1.1264 0.3860 0.115 Uiso 0.70 1 calc PR . . H28C H 0.0721 1.0815 0.4547 0.115 Uiso 0.70 1 calc PR . . Br1 Br 0.40917(2) 0.15243(2) 0.920016(16) 0.02241(8) Uani 1 1 d . . . Br2A Br 0.73512(7) 0.93887(7) 0.46331(5) 0.0387(2) Uani 0.60 1 d PU . . Br2B Br 0.78280(12) 0.93728(11) 0.48517(7) 0.0453(4) Uani 0.40 1 d PU . . 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 Ni 0.01723(18) 0.01680(19) 0.0190(2) -0.00516(16) 0.00155(14) -0.00719(15) N1C 0.0194(12) 0.0206(13) 0.0186(13) -0.0073(11) 0.0050(10) -0.0105(10) N1B 0.0205(12) 0.0140(13) 0.0214(14) -0.0032(11) -0.0026(10) -0.0036(10) N1A 0.0172(12) 0.0187(13) 0.0210(14) -0.0047(11) -0.0043(10) -0.0035(10) N1D 0.0297(14) 0.0274(15) 0.0283(15) -0.0176(12) 0.0126(11) -0.0165(12) N3C 0.0207(12) 0.0176(12) 0.0164(13) -0.0053(10) 0.0020(9) -0.0074(10) N3B 0.0163(11) 0.0161(12) 0.0196(13) -0.0057(10) 0.0004(9) -0.0078(9) N3A 0.0181(11) 0.0162(12) 0.0206(13) -0.0076(10) 0.0011(9) -0.0069(10) N3D 0.0195(12) 0.0181(13) 0.0225(13) -0.0070(11) 0.0020(10) -0.0091(10) C2C 0.0228(15) 0.0174(15) 0.0195(16) -0.0053(12) 0.0007(12) -0.0068(12) C2B 0.0215(14) 0.0215(16) 0.0211(16) -0.0082(13) 0.0021(12) -0.0117(12) C2A 0.0197(14) 0.0172(15) 0.0198(15) -0.0047(12) 0.0027(11) -0.0081(12) C2D 0.0259(15) 0.0227(17) 0.0232(16) -0.0078(13) 0.0041(12) -0.0141(13) C4C 0.0208(14) 0.0180(15) 0.0183(15) -0.0068(12) 0.0021(11) -0.0089(12) C4B 0.0166(13) 0.0170(15) 0.0203(15) -0.0074(12) 0.0024(11) -0.0080(11) C4A 0.0186(14) 0.0168(15) 0.0188(15) -0.0079(12) 0.0037(11) -0.0059(11) C4D 0.0199(14) 0.0195(15) 0.0201(16) -0.0059(13) -0.0008(11) -0.0103(12) C5C 0.0202(14) 0.0206(16) 0.0173(15) -0.0073(13) 0.0007(11) -0.0092(12) C5B 0.0209(14) 0.0208(16) 0.0163(15) -0.0039(13) 0.0018(11) -0.0098(12) C5A 0.0204(14) 0.0173(15) 0.0177(15) -0.0072(12) 0.0025(11) -0.0065(12) C5D 0.0294(16) 0.0248(17) 0.0241(17) -0.0127(14) 0.0077(13) -0.0170(13) C7C 0.0221(14) 0.0244(16) 0.0167(15) -0.0051(13) 0.0001(11) -0.0120(12) C7B 0.0211(14) 0.0208(16) 0.0163(15) -0.0076(13) 0.0018(11) -0.0048(12) C7A 0.0189(14) 0.0174(15) 0.0207(16) -0.0065(13) 0.0036(11) -0.0084(12) C7D 0.0217(14) 0.0125(15) 0.0224(16) -0.0065(12) 0.0044(12) -0.0071(12) C8C 0.0379(18) 0.0330(19) 0.0241(17) -0.0083(15) 0.0014(14) -0.0202(15) C8B 0.0240(15) 0.0272(17) 0.0265(17) -0.0098(14) 0.0014(13) -0.0098(13) C8A 0.0236(15) 0.0200(16) 0.0270(17) -0.0054(14) -0.0003(12) -0.0118(13) C8D 0.0264(15) 0.0254(17) 0.0251(17) -0.0059(14) 0.0020(13) -0.0163(13) C9C 0.043(2) 0.049(2) 0.0224(18) -0.0013(17) 0.0076(15) -0.0292(17) C9B 0.0350(18) 0.0294(18) 0.0270(18) -0.0006(15) -0.0047(14) -0.0092(15) C9A 0.0273(16) 0.0322(19) 0.0206(16) -0.0029(14) -0.0021(12) -0.0136(14) C9D 0.0381(18) 0.0313(18) 0.0213(17) -0.0088(14) 0.0058(13) -0.0154(15) C10C 0.048(2) 0.056(2) 0.033(2) -0.0191(19) 0.0210(16) -0.0226(19) C10B 0.0314(17) 0.037(2) 0.0230(18) -0.0030(15) -0.0080(14) -0.0048(15) C10A 0.0261(16) 0.0253(18) 0.0219(17) 0.0039(14) 0.0010(13) -0.0049(13) C10D 0.0344(17) 0.0227(17) 0.0303(19) -0.0063(14) 0.0154(14) -0.0139(14) C11C 0.070(3) 0.046(2) 0.038(2) -0.0244(19) 0.0244(19) -0.029(2) C11B 0.0273(16) 0.0353(19) 0.0333(19) -0.0138(16) -0.0066(14) -0.0094(14) C11A 0.0317(17) 0.0175(16) 0.0304(19) -0.0068(14) 0.0089(14) -0.0099(13) C11D 0.0223(15) 0.0225(17) 0.044(2) -0.0104(15) 0.0081(14) -0.0136(13) C12C 0.0427(19) 0.0338(19) 0.0292(19) -0.0108(16) 0.0150(15) -0.0193(16) C12B 0.0236(15) 0.0232(16) 0.0260(17) -0.0087(14) -0.0008(12) -0.0090(13) C12A 0.0265(15) 0.0251(17) 0.0209(16) -0.0071(14) 0.0037(12) -0.0115(13) C12D 0.0240(15) 0.0177(15) 0.0306(18) -0.0097(14) 0.0018(13) -0.0074(12) C13C 0.0200(14) 0.0288(17) 0.0217(16) -0.0139(14) 0.0055(12) -0.0102(13) C13B 0.0160(13) 0.0180(15) 0.0265(17) -0.0090(13) 0.0016(11) -0.0059(11) C13A 0.0178(14) 0.0136(15) 0.0257(16) -0.0086(13) -0.0002(12) -0.0045(11) C13D 0.046(2) 0.0294(19) 0.038(2) -0.0209(16) 0.0226(16) -0.0187(16) C14C 0.0241(16) 0.046(2) 0.0266(18) -0.0094(16) 0.0018(13) -0.0135(15) C14B 0.0261(15) 0.0209(16) 0.0216(16) -0.0024(13) 0.0018(12) -0.0094(12) C14A 0.0269(15) 0.0310(18) 0.0228(16) -0.0128(14) 0.0054(12) -0.0131(14) C14D 0.076(2) 0.0276(19) 0.047(2) -0.0152(17) 0.0332(19) -0.0058(17) C15C 0.0304(18) 0.068(3) 0.0254(19) -0.0130(18) -0.0012(14) -0.0155(18) C15B 0.0290(16) 0.0276(18) 0.0192(16) -0.0078(14) 0.0021(12) -0.0091(14) C15A 0.0355(18) 0.036(2) 0.034(2) -0.0123(16) 0.0100(15) -0.0230(16) C15D 0.054(2) 0.0249(18) 0.064(2) -0.0138(17) 0.0253(18) -0.0127(16) C16C 0.0312(18) 0.086(3) 0.031(2) -0.030(2) 0.0019(15) -0.0281(19) C16B 0.0222(15) 0.0314(18) 0.0337(19) -0.0191(15) 0.0000(13) -0.0072(13) C16A 0.0341(18) 0.033(2) 0.049(2) -0.0151(18) 0.0018(16) -0.0221(16) C16D 0.084(3) 0.034(2) 0.056(2) -0.0211(18) 0.027(2) -0.0286(19) C17C 0.0381(19) 0.058(2) 0.040(2) -0.0277(19) 0.0126(16) -0.0328(18) C17B 0.0442(19) 0.0262(18) 0.0334(19) -0.0128(15) 0.0062(15) -0.0208(15) C17A 0.0384(19) 0.0316(19) 0.038(2) -0.0079(16) -0.0120(15) -0.0151(15) C17D 0.140(4) 0.048(3) 0.117(4) -0.029(3) 0.075(3) -0.023(3) C18C 0.0303(17) 0.0400(19) 0.0220(17) -0.0151(15) 0.0055(13) -0.0173(15) C18B 0.0356(17) 0.0308(18) 0.0243(17) -0.0117(15) 0.0101(13) -0.0170(14) C18A 0.0308(16) 0.0209(16) 0.0264(17) -0.0056(14) -0.0027(13) -0.0128(13) C18D 0.138(4) 0.045(3) 0.118(4) -0.027(3) 0.077(3) -0.037(3) N1 0.0415(18) 0.063(2) 0.0374(18) 0.0083(17) -0.0012(14) -0.0167(16) C19 0.043(2) 0.050(2) 0.033(2) -0.0148(19) 0.0055(16) -0.0119(18) C20 0.086(3) 0.043(2) 0.061(3) -0.022(2) 0.010(2) -0.008(2) N2 0.085(3) 0.044(2) 0.099(3) -0.022(2) -0.047(2) 0.008(2) C21 0.070(3) 0.054(3) 0.090(4) -0.031(3) -0.026(3) 0.003(3) C22 0.127(4) 0.070(3) 0.149(4) -0.037(3) 0.011(3) -0.031(3) N3 0.0407(17) 0.0402(18) 0.054(2) -0.0198(16) -0.0125(15) -0.0031(14) C23 0.041(2) 0.0240(18) 0.038(2) -0.0129(16) 0.0015(16) -0.0105(15) C24 0.0295(19) 0.053(2) 0.085(3) -0.031(2) -0.0089(19) -0.0049(17) N4 0.054(2) 0.132(4) 0.061(3) -0.034(3) 0.0132(19) -0.053(2) C25 0.063(3) 0.066(3) 0.058(3) -0.030(3) 0.009(2) -0.037(2) C26 0.147(5) 0.095(4) 0.075(4) -0.037(3) -0.017(3) -0.050(3) N5 0.089(4) 0.059(3) 0.040(3) -0.015(3) -0.006(3) -0.034(3) C27 0.066(4) 0.039(3) 0.046(4) -0.027(3) -0.017(3) -0.010(3) C28 0.081(5) 0.074(5) 0.078(5) -0.029(4) 0.007(4) -0.030(4) Br1 0.02083(15) 0.02351(16) 0.01926(16) -0.00231(13) 0.00185(11) -0.00873(12) Br2A 0.0498(5) 0.0309(4) 0.0340(5) -0.0162(4) 0.0188(3) -0.0133(4) Br2B 0.0651(10) 0.0322(6) 0.0275(7) -0.0106(5) 0.0132(6) -0.0077(7) _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 Ni N3C 1.893(2) . ? Ni N3D 1.897(2) . ? Ni N3B 1.896(2) . ? Ni N3A 1.903(2) . ? N1C C2C 1.316(3) . ? N1C C5C 1.375(3) . ? N1C H1C 0.831(17) . ? N1B C2B 1.330(3) . ? N1B C5B 1.373(3) . ? N1B H1B 0.854(12) . ? N1A C2A 1.315(3) . ? N1A C5A 1.386(3) . ? N1A H1A 0.843(10) . ? N1D C2D 1.320(3) . ? N1D C5D 1.379(3) . ? N1D H1D 0.82(3) . ? N3C C2C 1.335(3) . ? N3C C4C 1.387(3) . ? N3B C2B 1.327(3) . ? N3B C4B 1.392(3) . ? N3A C2A 1.332(3) . ? N3A C4A 1.388(3) . ? N3D C2D 1.327(3) . ? N3D C4D 1.389(3) . ? C2C H2C 0.9300 . ? C2B H2B 0.9300 . ? C2A H2A 0.9300 . ? C2D H2D 0.9300 . ? C4C C5C 1.374(3) . ? C4C C7C 1.464(4) . ? C4B C5B 1.368(3) . ? C4B C7B 1.474(4) . ? C4A C5A 1.372(4) . ? C4A C7A 1.473(4) . ? C4D C5D 1.370(4) . ? C4D C7D 1.481(3) . ? C5C C13C 1.474(4) . ? C5B C13B 1.467(4) . ? C5A C13A 1.468(4) . ? C5D C13D 1.474(4) . ? C7C C12C 1.373(4) . ? C7C C8C 1.391(4) . ? C7B C12B 1.388(4) . ? C7B C8B 1.402(4) . ? C7A C12A 1.388(4) . ? C7A C8A 1.387(4) . ? C7D C12D 1.382(4) . ? C7D C8D 1.376(4) . ? C8C C9C 1.391(4) . ? C8C H8C 0.9300 . ? C8B C9B 1.374(4) . ? C8B H8B 0.9300 . ? C8A C9A 1.381(4) . ? C8A H8A 0.9300 . ? C8D C9D 1.386(4) . ? C8D H8D 0.9300 . ? C9C C10C 1.361(4) . ? C9C H9C 0.9300 . ? C9B C10B 1.387(4) . ? C9B H9B 0.9300 . ? C9A C10A 1.385(4) . ? C9A H9A 0.9300 . ? C9D C10D 1.373(4) . ? C9D H9D 0.9300 . ? C10C C11C 1.368(4) . ? C10C H10C 0.9300 . ? C10B C11B 1.378(4) . ? C10B H10B 0.9300 . ? C10A C11A 1.369(4) . ? C10A H10A 0.9300 . ? C10D C11D 1.386(4) . ? C10D H10D 0.9300 . ? C11C C12C 1.388(4) . ? C11C H11C 0.9300 . ? C11B C12B 1.380(4) . ? C11B H11B 0.9300 . ? C11A C12A 1.385(4) . ? C11A H11A 0.9300 . ? C11D C12D 1.385(4) . ? C11D H11D 0.9300 . ? C12C H12C 0.9300 . ? C12B H12B 0.9300 . ? C12A H12A 0.9300 . ? C12D H12D 0.9300 . ? C13C C18C 1.389(4) . ? C13C C14C 1.387(4) . ? C13B C14B 1.391(4) . ? C13B C18B 1.394(4) . ? C13A C18A 1.388(4) . ? C13A C14A 1.391(4) . ? C13D C14D 1.320(4) . ? C13D C18D 1.394(5) . ? C14C C15C 1.377(4) . ? C14C H14C 0.9300 . ? C14B C15B 1.371(4) . ? C14B H14B 0.9300 . ? C14A C15A 1.382(4) . ? C14A H14A 0.9300 . ? C14D C15D 1.378(4) . ? C14D H14D 0.9300 . ? C15C C16C 1.382(4) . ? C15C H15C 0.9300 . ? C15B C16B 1.377(4) . ? C15B H15B 0.9300 . ? C15A C16A 1.370(4) . ? C15A H15A 0.9300 . ? C15D C16D 1.290(4) . ? C15D H15D 0.9300 . ? C16C C17C 1.373(4) . ? C16C H16C 0.9300 . ? C16B C17B 1.383(4) . ? C16B H16B 0.9300 . ? C16A C17A 1.385(4) . ? C16A H16A 0.9300 . ? C16D C17D 1.402(5) . ? C16D H16D 0.9300 . ? C17C C18C 1.378(4) . ? C17C H17C 0.9300 . ? C17B C18B 1.372(4) . ? C17B H17B 0.9300 . ? C17A C18A 1.385(4) . ? C17A H17A 0.9300 . ? C17D C18D 1.403(5) . ? C17D H17D 0.9300 . ? C18C H18C 0.9300 . ? C18B H18B 0.9300 . ? C18A H18A 0.9300 . ? C18D H18D 0.9300 . ? N1 C19 1.137(4) . ? C19 C20 1.451(5) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N2 C21 1.146(5) . ? C21 C22 1.460(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N3 C23 1.126(4) . ? C23 C24 1.457(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N4 C25 1.115(5) . ? C25 C26 1.451(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N5 C27 1.051(5) . ? C27 C28 1.497(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Br2A Br2B 0.7583(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3C Ni N3D 91.42(9) . . ? N3C Ni N3B 88.70(9) . . ? N3D Ni N3B 178.64(10) . . ? N3C Ni N3A 177.96(9) . . ? N3D Ni N3A 89.65(9) . . ? N3B Ni N3A 90.28(9) . . ? C2C N1C C5C 108.9(2) . . ? C2C N1C H1C 125(2) . . ? C5C N1C H1C 126(2) . . ? C2B N1B C5B 108.7(2) . . ? C2B N1B H1B 127.8(19) . . ? C5B N1B H1B 123.2(19) . . ? C2A N1A C5A 108.6(2) . . ? C2A N1A H1A 124.6(19) . . ? C5A N1A H1A 126.8(19) . . ? C2D N1D C5D 108.4(2) . . ? C2D N1D H1D 125(2) . . ? C5D N1D H1D 127(2) . . ? C2C N3C C4C 106.3(2) . . ? C2C N3C Ni 122.86(19) . . ? C4C N3C Ni 130.64(17) . . ? C2B N3B C4B 106.4(2) . . ? C2B N3B Ni 121.33(19) . . ? C4B N3B Ni 131.20(17) . . ? C2A N3A C4A 106.0(2) . . ? C2A N3A Ni 121.34(18) . . ? C4A N3A Ni 130.79(17) . . ? C2D N3D C4D 105.7(2) . . ? C2D N3D Ni 124.26(19) . . ? C4D N3D Ni 130.01(18) . . ? N1C C2C N3C 110.8(2) . . ? N1C C2C H2C 124.6 . . ? N3C C2C H2C 124.6 . . ? N3B C2B N1B 110.6(2) . . ? N3B C2B H2B 124.7 . . ? N1B C2B H2B 124.7 . . ? N1A C2A N3A 111.3(2) . . ? N1A C2A H2A 124.4 . . ? N3A C2A H2A 124.4 . . ? N1D C2D N3D 111.5(2) . . ? N1D C2D H2D 124.3 . . ? N3D C2D H2D 124.3 . . ? C5C C4C N3C 108.2(2) . . ? C5C C4C C7C 128.5(3) . . ? N3C C4C C7C 123.3(2) . . ? C5B C4B N3B 108.3(2) . . ? C5B C4B C7B 128.2(3) . . ? N3B C4B C7B 123.5(2) . . ? C5A C4A N3A 108.6(2) . . ? C5A C4A C7A 129.2(2) . . ? N3A C4A C7A 122.2(2) . . ? C5D C4D N3D 108.8(2) . . ? C5D C4D C7D 130.1(2) . . ? N3D C4D C7D 121.1(2) . . ? N1C C5C C4C 105.8(2) . . ? N1C C5C C13C 122.0(2) . . ? C4C C5C C13C 131.9(3) . . ? C4B C5B N1B 106.0(2) . . ? C4B C5B C13B 132.3(3) . . ? N1B C5B C13B 121.7(2) . . ? C4A C5A N1A 105.5(2) . . ? C4A C5A C13A 133.6(2) . . ? N1A C5A C13A 120.8(2) . . ? C4D C5D N1D 105.6(2) . . ? C4D C5D C13D 132.8(3) . . ? N1D C5D C13D 121.4(2) . . ? C12C C7C C8C 117.5(3) . . ? C12C C7C C4C 120.3(2) . . ? C8C C7C C4C 122.2(3) . . ? C12B C7B C8B 118.4(3) . . ? C12B C7B C4B 121.0(2) . . ? C8B C7B C4B 120.6(3) . . ? C12A C7A C8A 118.2(3) . . ? C12A C7A C4A 120.6(3) . . ? C8A C7A C4A 121.1(2) . . ? C12D C7D C8D 118.9(3) . . ? C12D C7D C4D 120.7(3) . . ? C8D C7D C4D 120.4(2) . . ? C7C C8C C9C 120.7(3) . . ? C7C C8C H8C 119.6 . . ? C9C C8C H8C 119.6 . . ? C9B C8B C7B 121.0(3) . . ? C9B C8B H8B 119.5 . . ? C7B C8B H8B 119.5 . . ? C9A C8A C7A 121.5(3) . . ? C9A C8A H8A 119.3 . . ? C7A C8A H8A 119.3 . . ? C7D C8D C9D 120.9(3) . . ? C7D C8D H8D 119.5 . . ? C9D C8D H8D 119.5 . . ? C10C C9C C8C 120.2(3) . . ? C10C C9C H9C 119.9 . . ? C8C C9C H9C 119.9 . . ? C8B C9B C10B 119.8(3) . . ? C8B C9B H9B 120.1 . . ? C10B C9B H9B 120.1 . . ? C8A C9A C10A 119.5(3) . . ? C8A C9A H9A 120.2 . . ? C10A C9A H9A 120.2 . . ? C10D C9D C8D 120.0(3) . . ? C10D C9D H9D 120.0 . . ? C8D C9D H9D 120.0 . . ? C9C C10C C11C 120.3(3) . . ? C9C C10C H10C 119.8 . . ? C11C C10C H10C 119.8 . . ? C11B C10B C9B 119.7(3) . . ? C11B C10B H10B 120.2 . . ? C9B C10B H10B 120.2 . . ? C11A C10A C9A 119.5(3) . . ? C11A C10A H10A 120.3 . . ? C9A C10A H10A 120.3 . . ? C9D C10D C11D 119.7(3) . . ? C9D C10D H10D 120.2 . . ? C11D C10D H10D 120.2 . . ? C10C C11C C12C 119.4(3) . . ? C10C C11C H11C 120.3 . . ? C12C C11C H11C 120.3 . . ? C10B C11B C12B 120.8(3) . . ? C10B C11B H11B 119.6 . . ? C12B C11B H11B 119.6 . . ? C10A C11A C12A 121.1(3) . . ? C10A C11A H11A 119.5 . . ? C12A C11A H11A 119.5 . . ? C12D C11D C10D 119.9(3) . . ? C12D C11D H11D 120.0 . . ? C10D C11D H11D 120.0 . . ? C7C C12C C11C 121.9(3) . . ? C7C C12C H12C 119.0 . . ? C11C C12C H12C 119.0 . . ? C11B C12B C7B 120.3(3) . . ? C11B C12B H12B 119.9 . . ? C7B C12B H12B 119.9 . . ? C11A C12A C7A 120.2(3) . . ? C11A C12A H12A 119.9 . . ? C7A C12A H12A 119.9 . . ? C7D C12D C11D 120.6(3) . . ? C7D C12D H12D 119.7 . . ? C11D C12D H12D 119.7 . . ? C18C C13C C14C 119.1(3) . . ? C18C C13C C5C 121.0(3) . . ? C14C C13C C5C 119.7(3) . . ? C14B C13B C18B 118.1(3) . . ? C14B C13B C5B 121.7(2) . . ? C18B C13B C5B 120.2(3) . . ? C18A C13A C14A 119.0(3) . . ? C18A C13A C5A 120.2(3) . . ? C14A C13A C5A 120.7(3) . . ? C14D C13D C18D 114.3(3) . . ? C14D C13D C5D 124.9(3) . . ? C18D C13D C5D 119.8(3) . . ? C15C C14C C13C 120.4(3) . . ? C15C C14C H14C 119.8 . . ? C13C C14C H14C 119.8 . . ? C15B C14B C13B 120.8(3) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C15A C14A C13A 120.5(3) . . ? C15A C14A H14A 119.7 . . ? C13A C14A H14A 119.7 . . ? C13D C14D C15D 123.6(3) . . ? C13D C14D H14D 118.2 . . ? C15D C14D H14D 118.2 . . ? C14C C15C C16C 120.4(3) . . ? C14C C15C H15C 119.8 . . ? C16C C15C H15C 119.8 . . ? C14B C15B C16B 120.5(3) . . ? C14B C15B H15B 119.8 . . ? C16B C15B H15B 119.8 . . ? C16A C15A C14A 119.9(3) . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16D C15D C14D 122.5(3) . . ? C16D C15D H15D 118.8 . . ? C14D C15D H15D 118.8 . . ? C17C C16C C15C 119.2(3) . . ? C17C C16C H16C 120.4 . . ? C15C C16C H16C 120.4 . . ? C15B C16B C17B 119.5(3) . . ? C15B C16B H16B 120.2 . . ? C17B C16B H16B 120.2 . . ? C15A C16A C17A 120.5(3) . . ? C15A C16A H16A 119.8 . . ? C17A C16A H16A 119.8 . . ? C15D C16D C17D 117.5(4) . . ? C15D C16D H16D 121.2 . . ? C17D C16D H16D 121.2 . . ? C18C C17C C16C 121.2(3) . . ? C18C C17C H17C 119.4 . . ? C16C C17C H17C 119.4 . . ? C18B C17B C16B 120.2(3) . . ? C18B C17B H17B 119.9 . . ? C16B C17B H17B 119.9 . . ? C16A C17A C18A 119.7(3) . . ? C16A C17A H17A 120.2 . . ? C18A C17A H17A 120.2 . . ? C16D C17D C18D 118.4(4) . . ? C16D C17D H17D 120.8 . . ? C18D C17D H17D 120.8 . . ? C17C C18C C13C 119.7(3) . . ? C17C C18C H18C 120.1 . . ? C13C C18C H18C 120.1 . . ? C17B C18B C13B 120.9(3) . . ? C17B C18B H18B 119.6 . . ? C13B C18B H18B 119.6 . . ? C17A C18A C13A 120.4(3) . . ? C17A C18A H18A 119.8 . . ? C13A C18A H18A 119.8 . . ? C13D C18D C17D 121.6(4) . . ? C13D C18D H18D 119.2 . . ? C17D C18D H18D 119.2 . . ? N1 C19 C20 178.2(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 C22 178.1(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 C24 179.0(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 178.2(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 178.5(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.935 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.076 # start Validation Reply Form _vrf_PLAT077_7-Ni{HL'}4_Br2_4.7MeCN ; RESPONSE: Because of the partially occupied solvent (acetonitrile) sites. See also _refine_special_details. ; _vrf_PLAT230_7-Ni{HL'}4_Br2_4.7MeCN ; RESPONSE: See comment above. ; _vrf_PLAT241_7-Ni{HL'}4_Br2_4.7MeCN ; RESPONSE: See comment above. ; _vrf_PLAT220_7-Ni{HL'}4_Br2_4.7MeCN ; RESPONSE: All atomic species have been correctly identified; the large U(eq) range is due to the high thermal motion of the atoms of a phenyl ring (C13D to C18D) of the complex. See also _refine_special_details. ; # end Validation Reply Form #===END data_8-Ni{HL'}4_I2_2Me2CO_0.8H2O #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881069' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 N8 Ni, 2(C3 H6 O), 2(I), 0.8(H2 O)' _chemical_formula_sum 'C66 H61.60 I2 N8 Ni O2.80' _chemical_formula_weight 1324.14 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 23.8271(7) _cell_length_b 11.3058(4) _cell_length_c 23.1922(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6247.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8115 _cell_measurement_theta_min 3.0362 _cell_measurement_theta_max 28.9348 _exptl_crystal_description prism _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The iodide counterion of the structure is disordered and has been modelled over two orientations I1A and I1B with a 86:14 domain ratio, respectively. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13235 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6040 _reflns_number_gt 5493 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2560 Friedel pairs' _refine_ls_abs_structure_Flack -0.005(19) _refine_ls_number_reflns 6040 _refine_ls_number_parameters 372 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.044 _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 Ni Ni 0.5000 0.5000 0.41727(3) 0.02111(16) Uani 1 2 d S . . I1A I 0.602425(16) 0.27078(5) 0.661784(19) 0.04423(15) Uani 0.86 1 d P . . I1B I 0.5962(2) 0.3312(6) 0.6737(3) 0.0912(17) Uani 0.14 1 d PU . . C2B C 0.55078(17) 0.6029(4) 0.3195(2) 0.0277(8) Uani 1 1 d . . . H2B H 0.5172 0.6405 0.3103 0.033 Uiso 1 1 calc R . . C2A C 0.43584(18) 0.5517(4) 0.51792(18) 0.0294(9) Uani 1 1 d . . . H2A H 0.4538 0.6242 0.5219 0.035 Uiso 1 1 calc R . . C4B C 0.61308(17) 0.4870(4) 0.3599(2) 0.0280(9) Uani 1 1 d . . . C4A C 0.41193(18) 0.3787(4) 0.4857(2) 0.0287(9) Uani 1 1 d . . . C5B C 0.64005(17) 0.5506(4) 0.3186(2) 0.0308(9) Uani 1 1 d . . . C5A C 0.38070(18) 0.4028(4) 0.5347(2) 0.0303(9) Uani 1 1 d . . . C7B C 0.63637(17) 0.3980(4) 0.3982(2) 0.0310(9) Uani 1 1 d . . . C7A C 0.4115(2) 0.2750(4) 0.4479(2) 0.0326(10) Uani 1 1 d . . . C8B C 0.6118(2) 0.2854(4) 0.4026(3) 0.0407(12) Uani 1 1 d . . . H8B H 0.5811 0.2666 0.3796 0.049 Uiso 1 1 calc R . . C8A C 0.4615(2) 0.2261(4) 0.4281(3) 0.0423(12) Uani 1 1 d . . . H8A H 0.4957 0.2561 0.4408 0.051 Uiso 1 1 calc R . . C9B C 0.6325(3) 0.2022(5) 0.4407(3) 0.0590(16) Uani 1 1 d . . . H9B H 0.6145 0.1296 0.4443 0.071 Uiso 1 1 calc R . . C9A C 0.4602(2) 0.1320(4) 0.3891(3) 0.0565(16) Uani 1 1 d . . . H9A H 0.4938 0.1020 0.3747 0.068 Uiso 1 1 calc R . . C10B C 0.6788(3) 0.2248(6) 0.4728(3) 0.0623(18) Uani 1 1 d . . . H10B H 0.6930 0.1672 0.4974 0.075 Uiso 1 1 calc R . . C10A C 0.4103(2) 0.0828(4) 0.3717(3) 0.0487(13) Uani 1 1 d . . . H10A H 0.4098 0.0189 0.3465 0.058 Uiso 1 1 calc R . . C11B C 0.7048(2) 0.3338(6) 0.4690(3) 0.0533(15) Uani 1 1 d . . . H11B H 0.7361 0.3505 0.4915 0.064 Uiso 1 1 calc R . . C11A C 0.3603(2) 0.1307(4) 0.3927(3) 0.0438(12) Uani 1 1 d . . . H11A H 0.3262 0.0976 0.3818 0.053 Uiso 1 1 calc R . . C12B C 0.68368(19) 0.4188(5) 0.4309(2) 0.0416(11) Uani 1 1 d . . . H12B H 0.7020 0.4912 0.4276 0.050 Uiso 1 1 calc R . . C12A C 0.3608(2) 0.2259(4) 0.4292(2) 0.0365(11) Uani 1 1 d . . . H12A H 0.3271 0.2583 0.4416 0.044 Uiso 1 1 calc R . . C13B C 0.69938(12) 0.5465(4) 0.29955(18) 0.0425(11) Uani 1 1 d G . . C14B C 0.72112(19) 0.4415(3) 0.2778(2) 0.074(2) Uani 1 1 d GU . . H14B H 0.6979 0.3760 0.2732 0.089 Uiso 1 1 calc R . . C15B C 0.7775(2) 0.4343(5) 0.2629(2) 0.092(3) Uani 1 1 d GU . . H15B H 0.7921 0.3641 0.2484 0.110 Uiso 1 1 calc R . . C16B C 0.81220(13) 0.5322(6) 0.2698(3) 0.091(2) Uani 1 1 d GU . . H16B H 0.8499 0.5274 0.2598 0.110 Uiso 1 1 calc R . . C17B C 0.79047(18) 0.6372(5) 0.2915(3) 0.116(4) Uani 1 1 d GU . . H17B H 0.8137 0.7027 0.2961 0.140 Uiso 1 1 calc R . . C18B C 0.73406(19) 0.6444(4) 0.3064(3) 0.102(3) Uani 1 1 d GU . . H18B H 0.7195 0.7147 0.3209 0.123 Uiso 1 1 calc R . . C13A C 0.3396(2) 0.3303(5) 0.5667(2) 0.0416(11) Uani 1 1 d . . . C14A C 0.3486(2) 0.2093(5) 0.5720(3) 0.0470(13) Uani 1 1 d . . . H14A H 0.3797 0.1740 0.5550 0.056 Uiso 1 1 calc R . . C15A C 0.3097(3) 0.1410(6) 0.6034(3) 0.0617(17) Uani 1 1 d . . . H15A H 0.3150 0.0601 0.6082 0.074 Uiso 1 1 calc R . . C16A C 0.2638(3) 0.1970(8) 0.6269(3) 0.069(2) Uani 1 1 d . . . H16A H 0.2379 0.1522 0.6474 0.083 Uiso 1 1 calc R . . C17A C 0.2551(3) 0.3135(8) 0.6214(4) 0.076(2) Uani 1 1 d . . . H17A H 0.2231 0.3475 0.6373 0.092 Uiso 1 1 calc R . . C18A C 0.2932(2) 0.3837(6) 0.5921(3) 0.0544(14) Uani 1 1 d . . . H18A H 0.2879 0.4650 0.5895 0.065 Uiso 1 1 calc R . . C19 C 0.4453(2) 0.2697(6) 0.7281(3) 0.0477(14) Uani 1 1 d . . . C20 C 0.4412(3) 0.3695(7) 0.6859(3) 0.0630(17) Uani 1 1 d . . . H20A H 0.4538 0.4413 0.7039 0.094 Uiso 1 1 calc R . . H20B H 0.4028 0.3786 0.6739 0.094 Uiso 1 1 calc R . . H20C H 0.4642 0.3527 0.6530 0.094 Uiso 1 1 calc R . . C21 C 0.4437(3) 0.1457(7) 0.7042(4) 0.072(2) Uani 1 1 d . . . H21A H 0.4421 0.0901 0.7354 0.107 Uiso 1 1 calc R . . H21B H 0.4769 0.1316 0.6818 0.107 Uiso 1 1 calc R . . H21C H 0.4112 0.1366 0.6803 0.107 Uiso 1 1 calc R . . N1B N 0.59970(15) 0.6243(3) 0.29359(18) 0.0318(8) Uani 1 1 d D . . H1B H 0.600(2) 0.663(5) 0.2618(16) 0.048 Uiso 1 1 d D . . N1A N 0.39648(15) 0.5124(4) 0.55354(17) 0.0302(8) Uani 1 1 d D . . H1A H 0.390(2) 0.554(4) 0.5844(16) 0.045 Uiso 1 1 d D . . N3B N 0.55604(14) 0.5223(3) 0.35956(16) 0.0235(7) Uani 1 1 d . . . N3A N 0.44650(15) 0.4754(3) 0.47601(17) 0.0274(8) Uani 1 1 d . . . O1 O 0.45078(18) 0.2874(5) 0.7792(2) 0.0654(13) Uani 1 1 d . . . O2 O 0.5551(4) 0.1171(7) 0.5843(4) 0.045(2) Uani 0.40 1 d PU . . 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 Ni 0.0197(3) 0.0196(3) 0.0241(3) 0.000 0.000 -0.0010(2) I1A 0.03470(18) 0.0544(3) 0.0436(3) 0.0221(3) 0.00766(19) 0.00024(18) I1B 0.093(3) 0.079(3) 0.102(4) 0.018(3) 0.022(2) -0.018(2) C2B 0.025(2) 0.0284(19) 0.029(2) -0.0009(17) 0.0031(17) 0.0021(14) C2A 0.030(2) 0.035(2) 0.023(2) -0.0014(18) 0.0007(17) -0.0008(16) C4B 0.0227(19) 0.028(2) 0.033(2) -0.0064(17) -0.0009(17) -0.0005(14) C4A 0.028(2) 0.0259(19) 0.032(2) 0.0103(17) -0.0035(17) -0.0021(15) C5B 0.027(2) 0.036(2) 0.030(2) -0.0055(19) 0.0006(18) 0.0016(16) C5A 0.031(2) 0.030(2) 0.030(2) 0.0070(18) 0.0042(18) -0.0040(16) C7B 0.027(2) 0.037(2) 0.029(2) -0.0096(18) -0.0007(18) 0.0076(16) C7A 0.038(2) 0.026(2) 0.035(3) 0.0094(18) -0.003(2) -0.0050(16) C8B 0.048(3) 0.031(2) 0.043(3) -0.007(2) -0.013(2) 0.0128(19) C8A 0.043(3) 0.0216(19) 0.062(3) -0.003(2) -0.003(3) -0.0033(16) C9B 0.080(4) 0.037(3) 0.059(4) -0.003(3) -0.016(3) 0.017(3) C9A 0.050(3) 0.027(2) 0.093(5) -0.008(3) 0.009(3) 0.000(2) C10B 0.079(4) 0.062(4) 0.046(3) 0.000(3) -0.017(3) 0.038(3) C10A 0.064(3) 0.023(2) 0.059(3) -0.010(2) 0.005(3) -0.008(2) C11B 0.044(3) 0.077(4) 0.039(3) -0.010(3) -0.007(2) 0.029(3) C11A 0.048(3) 0.036(2) 0.048(3) 0.002(2) -0.006(2) -0.012(2) C12B 0.028(2) 0.061(3) 0.035(3) -0.007(2) -0.0050(19) 0.0077(19) C12A 0.036(2) 0.035(2) 0.039(3) 0.0024(19) -0.001(2) -0.0094(16) C13B 0.028(2) 0.070(3) 0.029(2) -0.006(2) 0.0061(19) -0.002(2) C14B 0.052(3) 0.112(5) 0.057(4) -0.014(4) 0.002(3) 0.026(3) C15B 0.075(4) 0.133(6) 0.066(4) -0.002(4) 0.001(4) 0.046(4) C16B 0.059(4) 0.153(6) 0.062(4) 0.010(5) 0.014(3) 0.004(4) C17B 0.072(5) 0.130(6) 0.148(7) -0.007(6) 0.002(5) -0.043(4) C18B 0.062(4) 0.113(5) 0.132(6) -0.044(5) 0.035(4) -0.033(4) C13A 0.037(2) 0.054(3) 0.034(2) 0.013(2) -0.003(2) -0.016(2) C14A 0.052(3) 0.053(3) 0.035(3) 0.012(2) -0.010(2) -0.019(2) C15A 0.073(4) 0.060(4) 0.053(3) 0.016(3) -0.013(3) -0.031(3) C16A 0.050(4) 0.108(6) 0.048(4) 0.016(4) 0.010(3) -0.026(4) C17A 0.054(4) 0.088(5) 0.087(5) 0.022(4) 0.031(4) -0.015(4) C18A 0.041(3) 0.066(4) 0.056(4) 0.004(3) 0.013(3) -0.005(2) C19 0.031(3) 0.070(4) 0.042(3) 0.019(3) -0.002(2) 0.006(2) C20 0.050(3) 0.087(5) 0.051(3) 0.030(3) 0.007(3) 0.015(3) C21 0.066(4) 0.079(5) 0.070(5) 0.022(4) -0.025(4) -0.023(3) N1B 0.0304(19) 0.033(2) 0.032(2) 0.0043(16) 0.0072(16) 0.0007(14) N1A 0.0318(19) 0.036(2) 0.0228(18) 0.0012(15) -0.0024(14) -0.0003(14) N3B 0.0211(16) 0.0241(17) 0.0251(18) 0.0010(14) 0.0018(14) 0.0022(12) N3A 0.0271(18) 0.0241(18) 0.031(2) 0.0041(14) -0.0034(15) -0.0033(13) O1 0.058(3) 0.088(3) 0.051(3) 0.019(2) -0.004(2) 0.016(2) O2 0.063(5) 0.024(3) 0.048(4) 0.011(3) 0.004(4) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3A 1.886(4) . ? Ni N3A 1.886(4) 2_665 ? Ni N3B 1.907(4) 2_665 ? Ni N3B 1.907(4) . ? I1A I1B 0.751(7) . ? C2B N3B 1.307(6) . ? C2B N1B 1.334(6) . ? C2B H2B 0.9300 . ? C2A N3A 1.324(6) . ? C2A N1A 1.326(6) . ? C2A H2A 0.9300 . ? C4B C5B 1.359(7) . ? C4B N3B 1.416(5) . ? C4B C7B 1.453(6) . ? C4A C5A 1.386(7) . ? C4A N3A 1.388(5) . ? C4A C7A 1.464(7) . ? C5B N1B 1.398(6) . ? C5B C13B 1.482(5) . ? C5A N1A 1.366(6) . ? C5A C13A 1.478(6) . ? C7B C12B 1.379(6) . ? C7B C8B 1.405(7) . ? C7A C8A 1.391(7) . ? C7A C12A 1.399(7) . ? C8B C9B 1.381(8) . ? C8B H8B 0.9300 . ? C8A C9A 1.397(8) . ? C8A H8A 0.9300 . ? C9B C10B 1.356(10) . ? C9B H9B 0.9300 . ? C9A C10A 1.374(8) . ? C9A H9A 0.9300 . ? C10B C11B 1.382(11) . ? C10B H10B 0.9300 . ? C10A C11A 1.397(8) . ? C10A H10A 0.9300 . ? C11B C12B 1.400(8) . ? C11B H11B 0.9300 . ? C11A C12A 1.369(8) . ? C11A H11A 0.9300 . ? C12B H12B 0.9300 . ? C12A H12A 0.9300 . ? C13B C14B 1.3900 . ? C13B C18B 1.3900 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? C16B C17B 1.3900 . ? C16B H16B 0.9300 . ? C17B C18B 1.3900 . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? C13A C14A 1.390(8) . ? C13A C18A 1.390(8) . ? C14A C15A 1.409(8) . ? C14A H14A 0.9300 . ? C15A C16A 1.376(11) . ? C15A H15A 0.9300 . ? C16A C17A 1.340(12) . ? C16A H16A 0.9300 . ? C17A C18A 1.384(8) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? C19 O1 1.208(8) . ? C19 C20 1.497(8) . ? C19 C21 1.508(11) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N1B H1B 0.859(11) . ? N1A H1A 0.870(10) . ? 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 N3A Ni N3A 87.5(2) . 2_665 ? N3A Ni N3B 90.82(14) . 2_665 ? N3A Ni N3B 177.98(17) 2_665 2_665 ? N3A Ni N3B 177.97(17) . . ? N3A Ni N3B 90.82(14) 2_665 . ? N3B Ni N3B 90.9(2) 2_665 . ? N3B C2B N1B 111.3(4) . . ? N3B C2B H2B 124.4 . . ? N1B C2B H2B 124.4 . . ? N3A C2A N1A 112.0(4) . . ? N3A C2A H2A 124.0 . . ? N1A C2A H2A 124.0 . . ? C5B C4B N3B 107.6(4) . . ? C5B C4B C7B 128.1(4) . . ? N3B C4B C7B 124.4(4) . . ? C5A C4A N3A 107.3(4) . . ? C5A C4A C7A 130.2(4) . . ? N3A C4A C7A 122.5(4) . . ? C4B C5B N1B 106.4(4) . . ? C4B C5B C13B 130.2(4) . . ? N1B C5B C13B 123.4(4) . . ? N1A C5A C4A 107.0(4) . . ? N1A C5A C13A 121.7(4) . . ? C4A C5A C13A 131.2(4) . . ? C12B C7B C8B 117.1(5) . . ? C12B C7B C4B 122.0(4) . . ? C8B C7B C4B 120.9(4) . . ? C8A C7A C12A 118.7(5) . . ? C8A C7A C4A 120.6(4) . . ? C12A C7A C4A 120.6(5) . . ? C9B C8B C7B 121.0(5) . . ? C9B C8B H8B 119.5 . . ? C7B C8B H8B 119.5 . . ? C7A C8A C9A 119.8(5) . . ? C7A C8A H8A 120.1 . . ? C9A C8A H8A 120.1 . . ? C10B C9B C8B 121.0(6) . . ? C10B C9B H9B 119.5 . . ? C8B C9B H9B 119.5 . . ? C10A C9A C8A 121.2(5) . . ? C10A C9A H9A 119.4 . . ? C8A C9A H9A 119.4 . . ? C9B C10B C11B 119.8(6) . . ? C9B C10B H10B 120.1 . . ? C11B C10B H10B 120.1 . . ? C9A C10A C11A 118.7(5) . . ? C9A C10A H10A 120.7 . . ? C11A C10A H10A 120.7 . . ? C10B C11B C12B 119.4(5) . . ? C10B C11B H11B 120.3 . . ? C12B C11B H11B 120.3 . . ? C12A C11A C10A 120.8(5) . . ? C12A C11A H11A 119.6 . . ? C10A C11A H11A 119.6 . . ? C7B C12B C11B 121.6(5) . . ? C7B C12B H12B 119.2 . . ? C11B C12B H12B 119.2 . . ? C11A C12A C7A 120.8(5) . . ? C11A C12A H12A 119.6 . . ? C7A C12A H12A 119.6 . . ? C14B C13B C18B 120.0 . . ? C14B C13B C5B 119.3(3) . . ? C18B C13B C5B 120.6(3) . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C14B C15B C16B 120.0 . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B H16B 120.0 . . ? C15B C16B H16B 120.0 . . ? C18B C17B C16B 120.0 . . ? C18B C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? C17B C18B C13B 120.0 . . ? C17B C18B H18B 120.0 . . ? C13B C18B H18B 120.0 . . ? C14A C13A C18A 120.9(5) . . ? C14A C13A C5A 119.1(5) . . ? C18A C13A C5A 119.9(5) . . ? C13A C14A C15A 118.9(6) . . ? C13A C14A H14A 120.6 . . ? C15A C14A H14A 120.6 . . ? C16A C15A C14A 118.4(7) . . ? C16A C15A H15A 120.8 . . ? C14A C15A H15A 120.8 . . ? C17A C16A C15A 122.5(6) . . ? C17A C16A H16A 118.7 . . ? C15A C16A H16A 118.7 . . ? C16A C17A C18A 120.6(7) . . ? C16A C17A H17A 119.7 . . ? C18A C17A H17A 119.7 . . ? C17A C18A C13A 118.7(7) . . ? C17A C18A H18A 120.7 . . ? C13A C18A H18A 120.7 . . ? O1 C19 C20 121.6(6) . . ? O1 C19 C21 121.1(6) . . ? C20 C19 C21 117.3(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2B N1B C5B 107.8(4) . . ? C2B N1B H1B 119(4) . . ? C5B N1B H1B 131(4) . . ? C2A N1A C5A 107.4(4) . . ? C2A N1A H1A 117(3) . . ? C5A N1A H1A 135(3) . . ? C2B N3B C4B 107.0(3) . . ? C2B N3B Ni 121.6(3) . . ? C4B N3B Ni 129.1(3) . . ? C2A N3A C4A 106.3(4) . . ? C2A N3A Ni 124.3(3) . . ? C4A N3A Ni 129.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.074 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.092 # start Validation Reply Form _vrf_PLAT220_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: All atomic species have been correctly identified. This alert is due to a disordered phenyl ring (C13B to C18B) of the ligand. ; _vrf_PLAT311_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: It was not possible to locate the H atoms of the lattice water molecule O2 (occupancy: 40%) from a difference map. ; _vrf_PLAT411_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: This short intermolecular contact is a consequence of the disorder of a phenyl ring (C13B to C18B) of the ligand. ; _vrf_PLAT041_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: The missing (not located by a difference synthesis) H atoms of the crystallization water molecule O2 have been included in the sum and moiety formula and the Mr, Dx and F(000) have been modified accordingly. These modifications account for the differences detected in the relevant data items. ; _vrf_PLAT077_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: Alert due to a partially occupied (40%) solvent site (O2 water molecule). ; _vrf_PLAT731_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: The distance has been restrainted by means of a DFIX instruction. ; _vrf_CELLZ01_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: See comment above. ; _vrf_REFLT03_8-Ni{HL'}4_I2_2Me2CO_0.8H2O ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 2560 Friedel pairs. ; # end Validation Reply Form #===END data_9-Ni{HL'}4_{NO3}2_2EtOH_2H2O #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881070' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 N8 Ni 2+, 2(C2 H6 O), 2(N O3 1-), 2(H2 O)' _chemical_formula_sum 'C64 H64 N10 Ni O10' _chemical_formula_weight 1191.96 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 Orthorhombic _symmetry_space_group_name_H-M 'I b a 2' _symmetry_space_group_name_Hall 'I 2 -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 11.4752(3) _cell_length_b 22.9510(5) _cell_length_c 22.8593(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6020.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11469 _cell_measurement_theta_min 3.1930 _cell_measurement_theta_max 30.0426 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8374 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5714 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5714 _reflns_number_gt 4585 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)' _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; The structure contains a small volume of disordered solvent, close to the crystallization water molecules O5 and O6, which was treated with the Platon/Squeeze procedure. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1632 Friedel pairs' _refine_ls_abs_structure_Flack -0.008(14) _refine_ls_number_reflns 5714 _refine_ls_number_parameters 403 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2B C 0.1082(2) 0.94718(12) 0.62086(13) 0.0232(6) Uani 1 1 d . . . H2B H 0.1469 0.9817 0.6119 0.028 Uiso 1 1 calc R . . C2A C 0.0476(3) 1.06778(11) 0.82067(12) 0.0215(5) Uani 1 1 d . . . H2A H 0.1215 1.0515 0.8242 0.026 Uiso 1 1 calc R . . C4B C -0.0093(2) 0.88388(11) 0.66037(12) 0.0199(5) Uani 1 1 d . . . C4A C -0.1269(2) 1.08861(11) 0.78910(13) 0.0204(5) Uani 1 1 d . . . C5B C 0.0550(2) 0.85493(11) 0.61948(12) 0.0212(5) Uani 1 1 d . . . C5A C -0.1078(2) 1.12079(12) 0.83901(12) 0.0211(6) Uani 1 1 d . . . C7B C -0.1015(2) 0.86064(11) 0.69872(13) 0.0220(5) Uani 1 1 d . . . C7A C -0.2280(2) 1.08828(12) 0.75071(12) 0.0209(5) Uani 1 1 d . . . C8B C -0.2106(2) 0.88648(12) 0.70100(13) 0.0258(6) Uani 1 1 d . . . H8B H -0.2267 0.9183 0.6771 0.031 Uiso 1 1 calc R . . C8A C -0.2751(2) 1.03536(12) 0.73112(14) 0.0262(6) Uani 1 1 d . . . H8A H -0.2439 1.0004 0.7444 0.031 Uiso 1 1 calc R . . C9B C -0.2956(3) 0.86565(14) 0.73829(15) 0.0322(7) Uani 1 1 d . . . H9B H -0.3689 0.8829 0.7389 0.039 Uiso 1 1 calc R . . C9A C -0.3670(3) 1.03480(13) 0.69238(17) 0.0330(7) Uani 1 1 d . . . H9A H -0.3964 0.9995 0.6790 0.040 Uiso 1 1 calc R . . C10B C -0.2715(3) 0.81920(15) 0.77475(15) 0.0346(7) Uani 1 1 d . . . H10B H -0.3278 0.8061 0.8009 0.042 Uiso 1 1 calc R . . C10A C -0.4161(3) 1.08680(14) 0.67329(15) 0.0318(7) Uani 1 1 d . . . H10A H -0.4782 1.0865 0.6471 0.038 Uiso 1 1 calc R . . C11B C -0.1641(3) 0.79206(13) 0.77257(14) 0.0324(7) Uani 1 1 d . . . H11B H -0.1489 0.7603 0.7966 0.039 Uiso 1 1 calc R . . C11A C -0.3717(2) 1.13909(12) 0.69360(15) 0.0280(6) Uani 1 1 d . . . H11A H -0.4051 1.1740 0.6816 0.034 Uiso 1 1 calc R . . C12B C -0.0788(3) 0.81226(12) 0.73453(13) 0.0261(6) Uani 1 1 d . . . H12B H -0.0068 0.7938 0.7328 0.031 Uiso 1 1 calc R . . C12A C -0.2790(2) 1.13992(11) 0.73122(13) 0.0234(6) Uani 1 1 d . . . H12A H -0.2495 1.1755 0.7440 0.028 Uiso 1 1 calc R . . C13B C 0.0504(2) 0.79379(11) 0.59986(12) 0.0216(5) Uani 1 1 d . . . C13A C -0.1846(3) 1.16043(12) 0.87163(12) 0.0255(6) Uani 1 1 d . . . C14B C -0.0489(3) 0.77222(13) 0.57292(15) 0.0296(6) Uani 1 1 d . . . H14B H -0.1118 0.7969 0.5662 0.036 Uiso 1 1 calc R . . C14A C -0.3012(3) 1.14569(13) 0.88129(14) 0.0286(6) Uani 1 1 d . . . H14A H -0.3310 1.1112 0.8660 0.034 Uiso 1 1 calc R . . C15B C -0.0556(3) 0.71456(13) 0.55589(16) 0.0343(7) Uani 1 1 d . . . H15B H -0.1230 0.7006 0.5382 0.041 Uiso 1 1 calc R . . C15A C -0.3721(3) 1.18209(14) 0.91347(15) 0.0351(7) Uani 1 1 d . . . H15A H -0.4494 1.1718 0.9202 0.042 Uiso 1 1 calc R . . C16B C 0.0376(3) 0.67753(12) 0.56503(14) 0.0317(7) Uani 1 1 d . . . H16B H 0.0337 0.6388 0.5532 0.038 Uiso 1 1 calc R . . C16A C -0.3291(3) 1.23376(15) 0.93568(14) 0.0360(8) Uani 1 1 d . . . H16A H -0.3773 1.2582 0.9572 0.043 Uiso 1 1 calc R . . C17B C 0.1359(3) 0.69843(13) 0.59179(15) 0.0334(7) Uani 1 1 d . . . H17B H 0.1987 0.6736 0.5981 0.040 Uiso 1 1 calc R . . C17A C -0.2155(3) 1.24886(14) 0.92592(16) 0.0368(8) Uani 1 1 d . . . H17A H -0.1868 1.2838 0.9408 0.044 Uiso 1 1 calc R . . C18B C 0.1431(3) 0.75613(13) 0.60953(15) 0.0302(6) Uani 1 1 d . . . H18B H 0.2102 0.7696 0.6279 0.036 Uiso 1 1 calc R . . C18A C -0.1419(3) 1.21214(13) 0.89372(14) 0.0308(7) Uani 1 1 d . . . H18A H -0.0646 1.2226 0.8873 0.037 Uiso 1 1 calc R . . N1B N 0.1294(2) 0.89568(10) 0.59551(11) 0.0229(5) Uani 1 1 d D . . H1B H 0.176(3) 0.8933(15) 0.5653(10) 0.034 Uiso 1 1 d D . . N1A N 0.0027(2) 1.10738(10) 0.85730(11) 0.0221(5) Uani 1 1 d D . . H1A H 0.040(3) 1.1180(15) 0.8882(10) 0.033 Uiso 1 1 d D . . N3B N 0.0247(2) 0.94222(10) 0.66055(11) 0.0206(5) Uani 1 1 d . . . N3A N -0.0273(2) 1.05517(10) 0.77891(12) 0.0204(5) Uani 1 1 d . . . Ni Ni 0.0000 1.0000 0.71885(2) 0.01755(11) Uani 1 2 d S . . N N 0.2202(3) 0.89211(11) 0.45624(11) 0.0330(6) Uani 1 1 d . . . O2 O 0.28674(19) 0.89442(10) 0.49990(10) 0.0356(5) Uani 1 1 d D . . O3 O 0.2550(2) 0.90735(13) 0.40703(11) 0.0511(7) Uani 1 1 d . . . O1 O 0.11843(19) 0.87352(9) 0.46278(11) 0.0352(5) Uani 1 1 d . . . O4 O 0.2882(4) 1.04571(14) 0.56808(15) 0.0730(10) Uani 1 1 d D . . H4 H 0.336(4) 1.021(2) 0.552(3) 0.110 Uiso 1 1 d D . . C19 C 0.2092(7) 1.0724(2) 0.5262(3) 0.093(2) Uani 1 1 d . . . H19A H 0.2492 1.1049 0.5081 0.111 Uiso 1 1 calc R . . H19B H 0.1434 1.0882 0.5477 0.111 Uiso 1 1 calc R . . C20 C 0.1640(6) 1.0349(2) 0.4798(3) 0.095(2) Uani 1 1 d . . . H20A H 0.1100 1.0073 0.4961 0.142 Uiso 1 1 calc R . . H20B H 0.2273 1.0143 0.4616 0.142 Uiso 1 1 calc R . . H20C H 0.1249 1.0583 0.4510 0.142 Uiso 1 1 calc R . . O5 O 0.5215(5) 1.0461(3) 0.4161(4) 0.069(2) Uani 0.50 1 d P . . O6 O 0.4635(7) 0.9865(4) 0.5171(4) 0.085(2) Uani 0.50 1 d PD . . 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 C2B 0.0244(14) 0.0184(13) 0.0269(14) -0.0005(11) -0.0011(12) -0.0022(10) C2A 0.0241(13) 0.0156(12) 0.0248(14) 0.0020(10) 0.0007(12) 0.0021(10) C4B 0.0256(14) 0.0125(12) 0.0216(13) 0.0018(10) -0.0044(11) 0.0001(9) C4A 0.0212(13) 0.0140(11) 0.0262(14) 0.0021(10) 0.0038(11) -0.0005(9) C5B 0.0218(13) 0.0173(12) 0.0245(14) -0.0018(10) -0.0045(11) 0.0008(10) C5A 0.0227(13) 0.0179(13) 0.0225(14) 0.0006(10) 0.0030(11) 0.0012(10) C7B 0.0260(13) 0.0153(12) 0.0247(13) -0.0020(10) -0.0001(11) -0.0052(10) C7A 0.0177(12) 0.0227(14) 0.0224(13) -0.0001(11) 0.0035(10) 0.0011(10) C8B 0.0270(14) 0.0222(13) 0.0281(15) 0.0024(11) -0.0016(11) -0.0034(11) C8A 0.0201(12) 0.0173(12) 0.0412(18) 0.0015(11) 0.0009(12) 0.0004(9) C9B 0.0276(15) 0.0332(16) 0.0359(16) -0.0026(13) 0.0010(13) -0.0060(12) C9A 0.0279(15) 0.0228(14) 0.0482(18) 0.0002(14) -0.0027(14) -0.0035(11) C10B 0.0369(18) 0.0357(17) 0.0312(16) 0.0022(14) 0.0034(14) -0.0134(13) C10A 0.0229(14) 0.0331(16) 0.0395(18) 0.0045(14) -0.0011(13) -0.0015(12) C11B 0.0454(18) 0.0217(14) 0.0302(16) 0.0036(13) -0.0025(14) -0.0102(12) C11A 0.0254(14) 0.0219(14) 0.0365(15) 0.0053(13) 0.0012(13) 0.0047(11) C12B 0.0319(15) 0.0183(13) 0.0281(15) -0.0006(11) -0.0031(11) -0.0022(10) C12A 0.0251(13) 0.0166(12) 0.0285(16) -0.0002(10) 0.0040(11) 0.0026(9) C13B 0.0264(13) 0.0162(12) 0.0222(13) -0.0011(10) 0.0016(11) -0.0015(10) C13A 0.0319(16) 0.0236(13) 0.0209(13) 0.0019(11) 0.0011(11) 0.0085(11) C14B 0.0305(15) 0.0214(14) 0.0369(17) -0.0047(12) -0.0049(14) 0.0024(12) C14A 0.0295(16) 0.0259(14) 0.0305(15) 0.0012(12) 0.0068(13) 0.0025(11) C15B 0.0378(18) 0.0257(16) 0.0394(18) -0.0037(13) -0.0078(15) -0.0081(13) C15A 0.0380(18) 0.0348(17) 0.0327(16) 0.0059(14) 0.0078(14) 0.0089(13) C16B 0.0504(18) 0.0130(13) 0.0316(16) -0.0011(11) 0.0106(14) -0.0057(12) C16A 0.0438(19) 0.0359(18) 0.0283(15) -0.0005(14) 0.0050(15) 0.0225(14) C17B 0.0405(18) 0.0206(14) 0.0390(18) -0.0023(13) -0.0013(14) 0.0097(12) C17A 0.0447(19) 0.0286(16) 0.0371(18) -0.0097(14) -0.0030(15) 0.0119(14) C18B 0.0315(16) 0.0247(14) 0.0345(16) -0.0032(13) -0.0054(13) 0.0040(11) C18A 0.0341(17) 0.0254(15) 0.0328(16) -0.0038(13) -0.0019(13) 0.0064(12) N1B 0.0263(13) 0.0181(11) 0.0245(12) -0.0012(10) 0.0031(10) -0.0017(9) N1A 0.0259(12) 0.0187(11) 0.0217(11) -0.0001(9) -0.0015(10) 0.0009(9) N3B 0.0262(13) 0.0157(12) 0.0199(12) 0.0003(9) -0.0009(10) -0.0020(9) N3A 0.0247(12) 0.0132(11) 0.0234(13) -0.0004(9) 0.0008(10) 0.0037(9) Ni 0.0205(2) 0.01270(18) 0.0195(2) 0.000 0.000 0.00039(17) N 0.0436(15) 0.0301(13) 0.0252(14) -0.0005(10) -0.0014(11) 0.0081(11) O2 0.0357(12) 0.0407(12) 0.0305(12) 0.0040(10) -0.0059(10) 0.0071(10) O3 0.0502(16) 0.071(2) 0.0317(13) 0.0107(13) 0.0028(12) -0.0039(14) O1 0.0404(12) 0.0354(11) 0.0299(12) 0.0020(10) 0.0004(11) -0.0040(9) O4 0.117(3) 0.0562(19) 0.0456(18) 0.0064(15) 0.0003(19) -0.0381(19) C19 0.149(6) 0.057(3) 0.072(3) 0.007(3) 0.008(4) -0.039(4) C20 0.119(5) 0.065(3) 0.100(5) 0.024(3) -0.024(4) -0.033(3) O5 0.047(3) 0.060(4) 0.099(6) 0.011(4) -0.001(3) -0.006(3) O6 0.074(6) 0.089(6) 0.092(6) 0.013(5) -0.003(4) -0.015(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2B N3B 1.325(4) . ? C2B N1B 1.339(4) . ? C2B H2B 0.9300 . ? C2A N3A 1.317(4) . ? C2A N1A 1.339(4) . ? C2A H2A 0.9300 . ? C4B C5B 1.364(4) . ? C4B N3B 1.395(3) . ? C4B C7B 1.474(4) . ? C4A C5A 1.377(4) . ? C4A N3A 1.396(3) . ? C4A C7A 1.454(4) . ? C5B N1B 1.380(4) . ? C5B C13B 1.474(4) . ? C5A N1A 1.370(4) . ? C5A C13A 1.470(4) . ? C7B C8B 1.386(4) . ? C7B C12B 1.404(4) . ? C7A C12A 1.395(4) . ? C7A C8A 1.403(4) . ? C8B C9B 1.381(4) . ? C8B H8B 0.9300 . ? C8A C9A 1.378(5) . ? C8A H8A 0.9300 . ? C9B C10B 1.381(5) . ? C9B H9B 0.9300 . ? C9A C10A 1.390(4) . ? C9A H9A 0.9300 . ? C10B C11B 1.382(5) . ? C10B H10B 0.9300 . ? C10A C11A 1.384(4) . ? C10A H10A 0.9300 . ? C11B C12B 1.389(4) . ? C11B H11B 0.9300 . ? C11A C12A 1.368(4) . ? C11A H11A 0.9300 . ? C12B H12B 0.9300 . ? C12A H12A 0.9300 . ? C13B C14B 1.386(4) . ? C13B C18B 1.389(4) . ? C13A C18A 1.380(4) . ? C13A C14A 1.398(4) . ? C14B C15B 1.381(4) . ? C14B H14B 0.9300 . ? C14A C15A 1.379(4) . ? C14A H14A 0.9300 . ? C15B C16B 1.382(5) . ? C15B H15B 0.9300 . ? C15A C16A 1.381(5) . ? C15A H15A 0.9300 . ? C16B C17B 1.370(5) . ? C16B H16B 0.9300 . ? C16A C17A 1.367(5) . ? C16A H16A 0.9300 . ? C17B C18B 1.388(4) . ? C17B H17B 0.9300 . ? C17A C18A 1.402(4) . ? C17A H17A 0.9300 . ? C18B H18B 0.9300 . ? C18A H18A 0.9300 . ? N1B H1B 0.873(7) . ? N1A H1A 0.861(10) . ? N3B Ni 1.901(3) . ? N3A Ni 1.894(3) . ? Ni N3A 1.894(3) 2_575 ? Ni N3B 1.901(3) 2_575 ? N O3 1.244(4) . ? N O1 1.252(4) . ? N O2 1.258(3) . ? O4 C19 1.453(8) . ? O4 H4 0.872(17) . ? C19 C20 1.463(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O6 O6 1.042(13) 2_675 ? 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 N3B C2B N1B 110.6(2) . . ? N3B C2B H2B 124.7 . . ? N1B C2B H2B 124.7 . . ? N3A C2A N1A 110.5(2) . . ? N3A C2A H2A 124.7 . . ? N1A C2A H2A 124.7 . . ? C5B C4B N3B 108.6(2) . . ? C5B C4B C7B 128.3(2) . . ? N3B C4B C7B 123.1(2) . . ? C5A C4A N3A 107.6(2) . . ? C5A C4A C7A 129.0(2) . . ? N3A C4A C7A 123.3(2) . . ? C4B C5B N1B 106.1(2) . . ? C4B C5B C13B 130.8(3) . . ? N1B C5B C13B 123.1(2) . . ? N1A C5A C4A 106.2(2) . . ? N1A C5A C13A 122.6(3) . . ? C4A C5A C13A 131.1(3) . . ? C8B C7B C12B 118.9(3) . . ? C8B C7B C4B 121.0(2) . . ? C12B C7B C4B 120.0(2) . . ? C12A C7A C8A 118.2(2) . . ? C12A C7A C4A 121.5(2) . . ? C8A C7A C4A 120.3(2) . . ? C9B C8B C7B 120.9(3) . . ? C9B C8B H8B 119.6 . . ? C7B C8B H8B 119.6 . . ? C9A C8A C7A 120.5(3) . . ? C9A C8A H8A 119.7 . . ? C7A C8A H8A 119.7 . . ? C10B C9B C8B 119.9(3) . . ? C10B C9B H9B 120.1 . . ? C8B C9B H9B 120.1 . . ? C8A C9A C10A 120.3(3) . . ? C8A C9A H9A 119.9 . . ? C10A C9A H9A 119.9 . . ? C9B C10B C11B 120.3(3) . . ? C9B C10B H10B 119.8 . . ? C11B C10B H10B 119.8 . . ? C11A C10A C9A 119.3(3) . . ? C11A C10A H10A 120.3 . . ? C9A C10A H10A 120.3 . . ? C10B C11B C12B 120.0(3) . . ? C10B C11B H11B 120.0 . . ? C12B C11B H11B 120.0 . . ? C12A C11A C10A 120.6(3) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C11B C12B C7B 119.9(3) . . ? C11B C12B H12B 120.0 . . ? C7B C12B H12B 120.0 . . ? C11A C12A C7A 121.0(3) . . ? C11A C12A H12A 119.5 . . ? C7A C12A H12A 119.5 . . ? C14B C13B C18B 118.6(3) . . ? C14B C13B C5B 120.3(3) . . ? C18B C13B C5B 121.1(3) . . ? C18A C13A C14A 119.4(3) . . ? C18A C13A C5A 120.4(3) . . ? C14A C13A C5A 120.3(3) . . ? C15B C14B C13B 120.9(3) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C15A C14A C13A 120.2(3) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14B C15B C16B 120.2(3) . . ? C14B C15B H15B 119.9 . . ? C16B C15B H15B 119.9 . . ? C14A C15A C16A 120.3(3) . . ? C14A C15A H15A 119.8 . . ? C16A C15A H15A 119.8 . . ? C17B C16B C15B 119.3(3) . . ? C17B C16B H16B 120.3 . . ? C15B C16B H16B 120.3 . . ? C17A C16A C15A 119.9(3) . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16B C17B C18B 120.9(3) . . ? C16B C17B H17B 119.6 . . ? C18B C17B H17B 119.6 . . ? C16A C17A C18A 120.5(3) . . ? C16A C17A H17A 119.7 . . ? C18A C17A H17A 119.7 . . ? C17B C18B C13B 120.1(3) . . ? C17B C18B H18B 119.9 . . ? C13B C18B H18B 119.9 . . ? C13A C18A C17A 119.7(3) . . ? C13A C18A H18A 120.1 . . ? C17A C18A H18A 120.1 . . ? C2B N1B C5B 108.3(2) . . ? C2B N1B H1B 121(2) . . ? C5B N1B H1B 130(2) . . ? C2A N1A C5A 108.5(2) . . ? C2A N1A H1A 121(3) . . ? C5A N1A H1A 130(3) . . ? C2B N3B C4B 106.4(2) . . ? C2B N3B Ni 121.85(19) . . ? C4B N3B Ni 129.1(2) . . ? C2A N3A C4A 107.0(2) . . ? C2A N3A Ni 124.3(2) . . ? C4A N3A Ni 128.6(2) . . ? N3A Ni N3A 87.07(15) . 2_575 ? N3A Ni N3B 90.99(9) . 2_575 ? N3A Ni N3B 177.64(13) 2_575 2_575 ? N3A Ni N3B 177.64(13) . . ? N3A Ni N3B 90.99(9) 2_575 . ? N3B Ni N3B 90.99(15) 2_575 . ? O3 N O1 120.2(3) . . ? O3 N O2 120.7(3) . . ? O1 N O2 119.1(3) . . ? C19 O4 H4 113(5) . . ? O4 C19 C20 116.8(5) . . ? O4 C19 H19A 108.1 . . ? C20 C19 H19A 108.1 . . ? O4 C19 H19B 108.1 . . ? C20 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.971 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.066 # start Validation Reply Form _vrf_PLAT430_9-Ni{HL'}4_{NO3}2_2EtOH_2H2O ; RESPONSE: Those short distances assume strong H-bonding between the O3 atom of the nitrate counterion and the crystallization waters O5 and O6 (whose H atoms have not been located). ; _vrf_PLAT041_9-Ni{HL'}4_{NO3}2_2EtOH_2H2O ; RESPONSE: The missing (not located by a difference synthesis) hydrogen atoms of the crystallization water molecules have been included in the sum and moiety formula and the Mr, Dx and F(000) have been modified accordingly. These modifications account for the differences detected in the relevant data items. ; _vrf_FORMU01_9-Ni{HL'}4_{NO3}2_2EtOH_2H2O ; RESPONSE: See comment above. ; _vrf_REFLT03_9-Ni{HL'}4_{NO3}2_2EtOH_2H2O ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 1632 Friedel pairs. ; # end Validation Reply Form #===END data_10-Ni{HL'}4_{ClO4}2_2.8Me2CO #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881071' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 N8 Ni, 2.8(C3 H6 O), 2(Cl O4)' _chemical_formula_sum 'C68.40 H64.80 Cl2 N8 Ni O10.80' _chemical_formula_weight 1301.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 13.1954(7) _cell_length_b 23.8866(10) _cell_length_c 11.2041(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.105(7) _cell_angle_gamma 90.00 _cell_volume 3223.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10678 _cell_measurement_theta_min 3.0607 _cell_measurement_theta_max 28.5792 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1359 _exptl_absorpt_coefficient_mu 0.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7107 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ; The crystal studied was a non-merohedral twin with a ratio of the twin components of 36:64. Therefore, the quality of the final analysis is certainly not as good as from an equivalent single crystal. The structure exhibits disorder, affecting the acetone molecules of crystallization, as well as some phenyl rings of the ligands of the complex. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25177 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 24.97 _reflns_number_total 25177 _reflns_number_gt 22003 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+4.2178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.029(17) _refine_ls_number_reflns 25177 _refine_ls_number_parameters 829 _refine_ls_number_restraints 271 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2476 _refine_ls_wR_factor_gt 0.2353 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2A C 0.9085(4) 0.7020(2) 0.7827(5) 0.0210(11) Uani 1 1 d . . . H2A H 0.9236 0.7352 0.7500 0.025 Uiso 1 1 calc R . . C2B C 0.8978(4) 0.8010(2) 0.9877(5) 0.0274(12) Uani 1 1 d . . . H2B H 0.9126 0.7677 1.0348 0.033 Uiso 1 1 calc R . . C2C C 0.5191(4) 0.8125(2) 0.6288(5) 0.0248(12) Uani 1 1 d . . . H2C H 0.5143 0.7954 0.5521 0.030 Uiso 1 1 calc R . . C2D C 0.5202(4) 0.6840(2) 0.7301(5) 0.0237(11) Uani 1 1 d . . . H2D H 0.5079 0.7012 0.7975 0.028 Uiso 1 1 calc R . . C4A C 0.8306(4) 0.6392(2) 0.8608(5) 0.0249(11) Uani 1 1 d . . . C4B C 0.8224(4) 0.8645(2) 0.8321(5) 0.0255(12) Uani 1 1 d . . . C4C C 0.5751(4) 0.8358(2) 0.8356(5) 0.0231(11) Uani 1 1 d . . . C4D C 0.5913(4) 0.6611(2) 0.5906(5) 0.0236(11) Uani 1 1 d . . . C5A C 0.9146(5) 0.6119(3) 0.8404(6) 0.0302(12) Uani 1 1 d . . . C5B C 0.9026(5) 0.8903(2) 0.9343(6) 0.0326(13) Uani 1 1 d . . . C5C C 0.4814(4) 0.8670(2) 0.7641(6) 0.0255(12) Uani 1 1 d . . . C5D C 0.4969(5) 0.6306(2) 0.5594(5) 0.0259(12) Uani 1 1 d . . . C7A C 0.7559(5) 0.6152(2) 0.9141(5) 0.0293(12) Uani 1 1 d . . . C7B C 0.7472(5) 0.8891(3) 0.7025(5) 0.0315(13) Uani 1 1 d DU . . C8C C 0.6795(6) 0.7867(3) 1.0441(6) 0.0414(16) Uani 1 1 d . . . H8C H 0.6549 0.7532 0.9993 0.050 Uiso 1 1 calc R . . C9B C 0.6774(7) 0.8918(4) 0.4718(7) 0.071(2) Uani 1 1 d DU . . H9B H 0.6722 0.8766 0.3931 0.085 Uiso 1 1 calc R . . C10B C 0.6143(7) 0.9405(4) 0.4729(9) 0.070(2) Uani 1 1 d U . . H10B H 0.5715 0.9585 0.3949 0.084 Uiso 1 1 calc R . . C11B C 0.6170(6) 0.9601(3) 0.5868(8) 0.0547(17) Uani 1 1 d U . . H11B H 0.5721 0.9902 0.5861 0.066 Uiso 1 1 calc R . . C12B C 0.6846(5) 0.9365(3) 0.7036(7) 0.0427(14) Uani 1 1 d U . . H12B H 0.6889 0.9515 0.7821 0.051 Uiso 1 1 calc R . . C7C C 0.6457(5) 0.8365(2) 0.9765(5) 0.0259(12) Uani 1 1 d . . . C7D C 0.6708(5) 0.6595(2) 0.5311(5) 0.0287(12) Uani 1 1 d . . . C8A C 0.7454(5) 0.6397(3) 1.0213(6) 0.0341(13) Uani 1 1 d . . . H8A H 0.7889 0.6707 1.0605 0.041 Uiso 1 1 calc R . . C8B C 0.7456(5) 0.8682(3) 0.5883(5) 0.0448(18) Uani 1 1 d D . . H8B H 0.7906 0.8380 0.5897 0.054 Uiso 1 1 calc R . . C8D C 0.7197(6) 0.7075(3) 0.5088(6) 0.0393(15) Uani 1 1 d . . . H8D H 0.6978 0.7422 0.5279 0.047 Uiso 1 1 calc R . . C9A C 0.6732(6) 0.6196(4) 1.0709(6) 0.054(2) Uani 1 1 d . . . H9A H 0.6675 0.6368 1.1424 0.064 Uiso 1 1 calc R . . C9C C 0.7482(7) 0.7848(3) 1.1754(7) 0.055(2) Uani 1 1 d . . . H9C H 0.7670 0.7507 1.2190 0.066 Uiso 1 1 calc R . . C9D C 0.8006(6) 0.7054(3) 0.4587(6) 0.0428(16) Uani 1 1 d . . . H9D H 0.8345 0.7381 0.4487 0.051 Uiso 1 1 calc R . . C10A C 0.6083(6) 0.5729(3) 1.0123(7) 0.0490(18) Uani 1 1 d . . . H10A H 0.5598 0.5586 1.0460 0.059 Uiso 1 1 calc R . . C10C C 0.7897(7) 0.8356(3) 1.2429(6) 0.055(2) Uani 1 1 d . . . H10C H 0.8384 0.8350 1.3307 0.066 Uiso 1 1 calc R . . C10D C 0.8298(6) 0.6548(3) 0.4242(6) 0.0483(18) Uani 1 1 d . . . H10D H 0.8813 0.6534 0.3873 0.058 Uiso 1 1 calc R . . C11A C 0.6153(5) 0.5470(3) 0.9027(7) 0.0450(17) Uani 1 1 d . . . H11A H 0.5716 0.5160 0.8634 0.054 Uiso 1 1 calc R . . C11C C 0.7576(6) 0.8859(3) 1.1776(7) 0.0416(16) Uani 1 1 d . . . H11C H 0.7835 0.9195 1.2217 0.050 Uiso 1 1 calc R . . C11D C 0.7834(6) 0.6062(3) 0.4440(6) 0.0438(16) Uani 1 1 d . . . H11D H 0.8037 0.5719 0.4211 0.053 Uiso 1 1 calc R . . C12A C 0.6881(5) 0.5686(2) 0.8555(6) 0.0365(14) Uani 1 1 d . . . H12A H 0.6929 0.5521 0.7829 0.044 Uiso 1 1 calc R . . C12C C 0.6855(5) 0.8863(3) 1.0442(6) 0.0338(14) Uani 1 1 d . . . H12C H 0.6642 0.9203 1.0005 0.041 Uiso 1 1 calc R . . C12D C 0.7049(5) 0.6085(3) 0.4991(6) 0.0288(13) Uani 1 1 d . . . H12D H 0.6752 0.5753 0.5144 0.035 Uiso 1 1 calc R . . C13A C 0.9549(6) 0.5562(3) 0.8640(7) 0.0530(17) Uani 1 1 d DU . . C14A C 1.0007(7) 0.5349(4) 0.9916(9) 0.089(3) Uani 1 1 d DU . . H14A H 1.0068 0.5601 1.0575 0.133 Uiso 1 1 calc R . . C15A C 1.0383(8) 0.4808(3) 1.0322(11) 0.095(3) Uani 1 1 d DU . . H15A H 1.0609 0.4688 1.1182 0.142 Uiso 1 1 calc R . . C16A C 1.0391(11) 0.4466(5) 0.9333(11) 0.127(4) Uani 1 1 d DU . . H16A H 1.0791 0.4133 0.9540 0.191 Uiso 1 1 calc R . . C17A C 0.9812(12) 0.4613(5) 0.8044(12) 0.128(3) Uani 1 1 d DU . . H17A H 0.9732 0.4360 0.7379 0.192 Uiso 1 1 calc R . . C18A C 0.9346(12) 0.5146(4) 0.7748(13) 0.117(3) Uani 1 1 d DU . . H18A H 0.8866 0.5221 0.6887 0.175 Uiso 1 1 calc R . . C13B C 0.9404(4) 0.9504(2) 0.9466(6) 0.0424(15) Uani 1 1 d GU . . C14B C 0.9850(5) 0.9687(3) 0.8604(6) 0.083(3) Uani 1 1 d GU . . H14B H 0.9923 0.9439 0.8005 0.125 Uiso 1 1 calc R . . C15B C 1.0185(6) 1.0241(3) 0.8638(8) 0.120(4) Uani 1 1 d GU . . H15B H 1.0483 1.0363 0.8062 0.181 Uiso 1 1 calc R . . C16B C 1.0075(6) 1.0612(2) 0.9534(9) 0.092(3) Uani 1 1 d GU . . H16B H 1.0299 1.0982 0.9557 0.138 Uiso 1 1 calc R . . C17B C 0.9629(7) 1.0429(3) 1.0396(8) 0.126(4) Uani 1 1 d GU . . H17B H 0.9556 1.0677 1.0995 0.189 Uiso 1 1 calc R . . C18B C 0.9294(6) 0.9875(3) 1.0362(7) 0.112(4) Uani 1 1 d GU . . H18B H 0.8995 0.9753 1.0938 0.167 Uiso 1 1 calc R . . C13C C 0.4165(4) 0.9072(2) 0.8041(5) 0.0336(14) Uani 1 1 d D . . C13D C 0.4366(5) 0.5920(2) 0.4492(6) 0.0313(13) Uani 1 1 d . . . C14C C 0.4016(5) 0.8993(3) 0.9133(7) 0.0492(18) Uani 1 1 d D . . H14C H 0.4336 0.8681 0.9645 0.059 Uiso 1 1 calc R . . C14D C 0.4286(5) 0.6049(3) 0.3268(6) 0.0416(16) Uani 1 1 d . . . H14D H 0.4648 0.6363 0.3145 0.050 Uiso 1 1 calc R . . C15C C 0.3405(6) 0.9357(4) 0.9532(9) 0.065(2) Uani 1 1 d DU . . H15C H 0.3328 0.9303 1.0313 0.078 Uiso 1 1 calc R . . C15D C 0.3672(6) 0.5715(3) 0.2215(7) 0.0510(18) Uani 1 1 d U . . H15D H 0.3592 0.5809 0.1376 0.061 Uiso 1 1 calc R . . C16C C 0.2908(7) 0.9807(4) 0.8717(11) 0.076(3) Uani 1 1 d U . . H16C H 0.2518 1.0067 0.8984 0.091 Uiso 1 1 calc R . . C16D C 0.3182(6) 0.5243(4) 0.2425(7) 0.060(2) Uani 1 1 d U . . H16D H 0.2813 0.5004 0.1726 0.072 Uiso 1 1 calc R . . C17C C 0.2970(7) 0.9886(4) 0.7527(12) 0.080(3) Uani 1 1 d DU . . H17C H 0.2574 1.0165 0.6943 0.096 Uiso 1 1 calc R . . C17D C 0.3216(6) 0.5111(3) 0.3617(8) 0.057(2) Uani 1 1 d U . . H17D H 0.2834 0.4801 0.3720 0.069 Uiso 1 1 calc R . . C18C C 0.3665(5) 0.9519(2) 0.7275(8) 0.054(2) Uani 1 1 d DU . . H18C H 0.3801 0.9582 0.6534 0.064 Uiso 1 1 calc R . . C18D C 0.3837(6) 0.5449(3) 0.4693(8) 0.0466(16) Uani 1 1 d . . . H18D H 0.3894 0.5359 0.5525 0.056 Uiso 1 1 calc R . . O9 O 0.4911(7) 0.7463(3) 0.3465(6) 0.066(2) Uani 0.80 1 d P . . C19 C 0.4653(7) 0.7671(4) 0.2417(7) 0.056(3) Uani 0.80 1 d PD . . C20 C 0.4375(10) 0.7355(4) 0.1233(8) 0.069(3) Uani 0.80 1 d PDU . . H20A H 0.4596 0.6972 0.1445 0.103 Uiso 0.80 1 calc PR . . H20B H 0.4755 0.7510 0.0739 0.103 Uiso 0.80 1 calc PR . . H20C H 0.3588 0.7372 0.0723 0.103 Uiso 0.80 1 calc PR . . C21 C 0.4588(14) 0.8284(4) 0.2168(14) 0.097(4) Uani 0.80 1 d PDU . . H21A H 0.3952 0.8435 0.2266 0.146 Uiso 0.80 1 calc PR . . H21B H 0.4522 0.8353 0.1295 0.146 Uiso 0.80 1 calc PR . . H21C H 0.5248 0.8461 0.2782 0.146 Uiso 0.80 1 calc PR . . C22 C 0.0897(5) 0.8080(3) 0.7063(7) 0.0390(15) Uani 1 1 d U . . C23 C 0.1663(6) 0.8116(3) 0.6389(9) 0.054(2) Uani 1 1 d . . . H23A H 0.1241 0.8096 0.5461 0.080 Uiso 1 1 calc R . . H23B H 0.2181 0.7811 0.6666 0.080 Uiso 1 1 calc R . . H23C H 0.2059 0.8464 0.6607 0.080 Uiso 1 1 calc R . . C24 C 0.1406(7) 0.8076(4) 0.8508(9) 0.058(2) Uani 1 1 d . . . H24A H 0.0835 0.8109 0.8827 0.087 Uiso 1 1 calc R . . H24B H 0.1912 0.8384 0.8822 0.087 Uiso 1 1 calc R . . H24C H 0.1801 0.7731 0.8813 0.087 Uiso 1 1 calc R . . O10 O -0.0145(4) 0.8050(2) 0.6395(5) 0.0502(12) Uani 1 1 d . . . C25 C 0.0939(6) 0.6931(3) 0.2423(7) 0.0434(17) Uani 1 1 d . . . C26 C 0.1431(7) 0.6927(4) 0.1466(8) 0.058(2) Uani 1 1 d . . . H26A H 0.0854 0.6957 0.0601 0.087 Uiso 1 1 calc R . . H26B H 0.1831 0.6584 0.1541 0.087 Uiso 1 1 calc R . . H26C H 0.1931 0.7238 0.1628 0.087 Uiso 1 1 calc R . . C27 C 0.1709(7) 0.6854(4) 0.3833(8) 0.067(3) Uani 1 1 d . . . H27A H 0.2200 0.7170 0.4122 0.101 Uiso 1 1 calc R . . H27B H 0.2137 0.6519 0.3928 0.101 Uiso 1 1 calc R . . H27C H 0.1284 0.6825 0.4350 0.101 Uiso 1 1 calc R . . O11 O -0.0057(4) 0.6989(2) 0.2119(5) 0.0580(14) Uani 1 1 d . . . N3A N 0.8291(4) 0.69547(19) 0.8245(5) 0.0219(10) Uani 1 1 d . . . N3B N 0.8220(4) 0.8070(2) 0.8648(5) 0.0248(10) Uani 1 1 d . . . N3C N 0.5973(4) 0.8020(2) 0.7482(5) 0.0262(11) Uani 1 1 d . . . N3D N 0.6072(4) 0.6949(2) 0.6996(5) 0.0247(10) Uani 1 1 d . . . O1 O 0.1101(5) 0.8306(3) 0.2951(6) 0.0698(17) Uani 1 1 d . . . O2 O 0.2558(4) 0.8897(2) 0.4235(5) 0.0615(16) Uani 1 1 d D . . O3 O 0.2081(5) 0.8782(3) 0.1982(6) 0.0735(19) Uani 1 1 d . . . O4 O 0.2936(5) 0.8056(2) 0.3472(6) 0.0717(18) Uani 1 1 d . . . O5 O 0.2639(4) 0.6114(2) 0.6930(5) 0.0450(11) Uani 1 1 d D . . O6 O 0.3178(4) 0.6963(2) 0.8083(5) 0.0491(13) Uani 1 1 d . . . O7 O 0.2348(5) 0.6257(3) 0.8837(5) 0.0649(17) Uani 1 1 d . . . O8 O 0.1288(3) 0.6753(2) 0.6947(5) 0.0474(12) Uani 1 1 d . . . Cl1 Cl 0.21641(14) 0.85095(7) 0.31250(18) 0.0503(5) Uani 1 1 d . . . Cl2 Cl 0.23693(11) 0.65169(7) 0.77170(15) 0.0372(4) Uani 1 1 d . . . Ni Ni 0.71475(6) 0.74986(3) 0.78493(7) 0.01960(17) Uani 1 1 d . . . N1A N 0.9644(4) 0.6537(2) 0.7941(5) 0.0330(12) Uani 1 1 d D . . H1A H 1.017(4) 0.658(3) 0.764(7) 0.049 Uiso 1 1 d D . . N1B N 0.9497(4) 0.8501(2) 1.0334(5) 0.0305(11) Uani 1 1 d D . . H1B H 0.996(4) 0.849(3) 1.117(2) 0.046 Uiso 1 1 d D . . N1C N 0.4493(4) 0.85122(19) 0.6360(5) 0.0266(10) Uani 1 1 d D . . H1C H 0.391(3) 0.868(2) 0.576(4) 0.040 Uiso 1 1 d D . . N1D N 0.4536(3) 0.64471(19) 0.6496(4) 0.0240(10) Uani 1 1 d D . . H1D H 0.400(3) 0.633(3) 0.670(6) 0.036 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2A 0.015(2) 0.016(3) 0.029(3) 0.005(2) 0.007(2) 0.002(2) C2B 0.022(3) 0.021(3) 0.033(3) -0.003(2) 0.006(2) -0.008(2) C2C 0.015(3) 0.027(3) 0.024(3) 0.001(2) -0.001(2) 0.003(2) C2D 0.014(2) 0.023(3) 0.030(3) -0.003(2) 0.005(2) -0.002(2) C4A 0.019(3) 0.022(3) 0.026(3) 0.001(2) 0.000(2) 0.005(2) C4B 0.018(3) 0.027(3) 0.029(3) 0.006(2) 0.008(2) 0.004(2) C4C 0.029(3) 0.016(3) 0.029(3) -0.003(2) 0.015(2) -0.003(2) C4D 0.014(3) 0.021(3) 0.029(3) -0.002(2) 0.001(2) 0.000(2) C5A 0.017(3) 0.030(3) 0.040(3) 0.000(3) 0.009(2) 0.002(2) C5B 0.026(3) 0.018(3) 0.046(3) 0.003(3) 0.006(3) -0.003(2) C5C 0.009(2) 0.018(3) 0.044(3) -0.002(2) 0.005(2) 0.003(2) C5D 0.026(3) 0.019(3) 0.024(3) -0.005(2) 0.002(2) 0.001(2) C7A 0.030(3) 0.020(3) 0.032(3) 0.012(2) 0.007(2) 0.004(2) C7B 0.025(3) 0.025(3) 0.045(3) 0.016(3) 0.015(3) 0.004(2) C8C 0.074(5) 0.025(3) 0.030(3) -0.005(3) 0.026(3) -0.008(3) C9B 0.084(5) 0.087(5) 0.049(4) 0.035(4) 0.033(4) 0.046(4) C10B 0.068(4) 0.074(5) 0.067(4) 0.048(4) 0.027(4) 0.036(4) C11B 0.047(3) 0.049(4) 0.077(4) 0.040(3) 0.035(3) 0.022(3) C12B 0.042(3) 0.032(3) 0.062(3) 0.018(3) 0.028(3) 0.006(3) C7C 0.034(3) 0.019(3) 0.036(3) -0.001(2) 0.026(3) -0.002(2) C7D 0.034(3) 0.031(3) 0.024(3) 0.000(2) 0.015(2) 0.000(2) C8A 0.029(3) 0.032(3) 0.032(3) 0.004(3) 0.003(3) -0.010(3) C8B 0.031(3) 0.067(5) 0.042(4) 0.023(4) 0.021(3) 0.021(3) C8D 0.056(4) 0.031(3) 0.028(3) -0.006(3) 0.014(3) -0.009(3) C9A 0.039(4) 0.095(6) 0.026(3) 0.005(4) 0.012(3) -0.019(4) C9C 0.108(7) 0.021(3) 0.043(4) 0.009(3) 0.037(4) 0.014(4) C9D 0.051(4) 0.044(4) 0.034(3) -0.002(3) 0.019(3) -0.009(3) C10A 0.041(4) 0.057(5) 0.050(4) 0.007(4) 0.019(3) -0.018(3) C10C 0.069(5) 0.061(5) 0.021(3) 0.002(3) 0.004(3) 0.013(4) C10D 0.051(4) 0.067(5) 0.035(3) -0.007(3) 0.026(3) -0.014(4) C11A 0.030(3) 0.035(4) 0.058(4) 0.016(3) 0.006(3) -0.010(3) C11C 0.058(4) 0.026(3) 0.047(4) -0.002(3) 0.029(3) 0.000(3) C11D 0.056(4) 0.049(4) 0.034(3) -0.008(3) 0.026(3) -0.004(3) C12A 0.037(3) 0.016(3) 0.044(3) 0.006(3) 0.003(3) 0.005(2) C12C 0.040(3) 0.035(4) 0.027(3) 0.001(3) 0.014(3) -0.003(3) C12D 0.029(3) 0.025(3) 0.030(3) -0.002(2) 0.010(2) -0.003(2) C13A 0.043(4) 0.025(3) 0.083(4) 0.001(3) 0.018(3) 0.006(3) C14A 0.073(5) 0.047(4) 0.104(5) 0.021(4) -0.007(4) -0.001(4) C15A 0.062(5) 0.058(5) 0.142(6) 0.030(4) 0.019(5) 0.017(4) C16A 0.104(6) 0.073(6) 0.172(7) 0.006(5) 0.024(6) 0.047(5) C17A 0.159(6) 0.075(5) 0.138(6) -0.025(5) 0.047(5) 0.034(5) C18A 0.154(6) 0.061(5) 0.115(5) -0.010(4) 0.033(5) 0.034(5) C13B 0.027(3) 0.018(3) 0.070(4) -0.002(3) 0.008(3) -0.006(2) C14B 0.074(5) 0.054(5) 0.115(6) 0.012(4) 0.033(4) -0.007(4) C15B 0.115(7) 0.090(6) 0.141(7) 0.024(5) 0.037(6) -0.005(5) C16B 0.059(5) 0.047(4) 0.143(7) 0.011(5) 0.013(4) 0.002(4) C17B 0.153(8) 0.080(6) 0.146(7) -0.028(6) 0.061(6) -0.005(6) C18B 0.130(6) 0.079(6) 0.149(7) -0.029(5) 0.081(6) -0.033(5) C13C 0.017(3) 0.025(3) 0.059(4) -0.015(3) 0.015(3) -0.009(2) C13D 0.025(3) 0.020(3) 0.043(3) -0.012(3) 0.009(2) 0.000(2) C14C 0.034(4) 0.036(4) 0.079(5) -0.023(4) 0.023(3) -0.014(3) C14D 0.034(3) 0.040(4) 0.043(4) -0.010(3) 0.009(3) 0.000(3) C15C 0.049(4) 0.068(5) 0.090(5) -0.045(4) 0.041(4) -0.022(4) C15D 0.042(4) 0.053(4) 0.041(3) -0.012(3) 0.000(3) 0.003(3) C16C 0.060(5) 0.046(5) 0.133(7) -0.031(5) 0.051(5) 0.003(4) C16D 0.057(4) 0.065(5) 0.047(4) -0.033(4) 0.009(3) -0.004(4) C17C 0.068(5) 0.052(5) 0.135(7) -0.009(5) 0.057(5) 0.012(4) C17D 0.052(4) 0.036(4) 0.084(5) -0.018(4) 0.028(4) -0.011(3) C18C 0.032(3) 0.023(3) 0.103(5) -0.003(3) 0.025(4) 0.010(3) C18D 0.053(4) 0.028(4) 0.061(4) -0.016(3) 0.026(3) -0.010(3) O9 0.085(6) 0.064(5) 0.036(4) 0.007(3) 0.012(4) 0.033(4) C19 0.033(5) 0.088(8) 0.042(5) 0.012(5) 0.012(4) 0.023(5) C20 0.070(6) 0.085(7) 0.045(5) 0.013(5) 0.017(4) 0.001(5) C21 0.115(8) 0.100(8) 0.102(7) 0.011(6) 0.071(7) -0.004(7) C22 0.022(3) 0.025(3) 0.062(4) -0.004(3) 0.009(3) -0.010(2) C23 0.034(4) 0.042(4) 0.093(6) 0.013(4) 0.035(4) 0.004(3) C24 0.043(4) 0.047(5) 0.083(6) -0.022(4) 0.026(4) -0.009(4) O10 0.042(3) 0.034(3) 0.078(3) 0.009(2) 0.027(3) 0.002(2) C25 0.031(4) 0.017(3) 0.060(4) 0.003(3) -0.004(3) -0.002(2) C26 0.054(5) 0.047(5) 0.061(5) -0.012(4) 0.011(4) 0.000(4) C27 0.050(5) 0.047(5) 0.071(5) 0.017(4) -0.009(4) -0.019(4) O11 0.040(3) 0.044(3) 0.066(3) 0.011(3) -0.003(2) -0.001(2) N3A 0.019(2) 0.014(2) 0.031(2) 0.0042(19) 0.0087(19) 0.0021(18) N3B 0.026(3) 0.018(2) 0.024(2) 0.003(2) 0.005(2) -0.001(2) N3C 0.025(2) 0.022(3) 0.030(3) -0.002(2) 0.009(2) -0.0012(19) N3D 0.017(2) 0.026(3) 0.027(2) 0.000(2) 0.004(2) 0.0074(19) O1 0.045(3) 0.069(4) 0.061(3) -0.007(3) -0.014(2) -0.010(3) O2 0.043(3) 0.031(3) 0.064(3) -0.013(2) -0.026(2) 0.008(2) O3 0.061(4) 0.050(4) 0.071(4) 0.026(3) -0.012(3) -0.010(3) O4 0.071(4) 0.040(3) 0.077(4) -0.005(3) 0.003(3) 0.017(3) O5 0.038(3) 0.039(3) 0.062(3) -0.018(2) 0.026(2) -0.009(2) O6 0.037(3) 0.036(3) 0.075(3) -0.027(2) 0.025(2) -0.009(2) O7 0.074(4) 0.079(4) 0.060(3) 0.019(3) 0.046(3) 0.031(3) O8 0.023(2) 0.059(3) 0.056(3) 0.007(2) 0.012(2) 0.013(2) Cl1 0.0426(10) 0.0270(8) 0.0605(11) -0.0081(8) -0.0002(8) -0.0049(7) Cl2 0.0264(8) 0.0374(9) 0.0490(8) -0.0022(7) 0.0166(6) 0.0044(6) Ni 0.0166(3) 0.0147(3) 0.0226(3) -0.0004(2) 0.0029(2) 0.0011(3) N1A 0.031(3) 0.024(3) 0.049(3) 0.006(2) 0.021(2) 0.009(2) N1B 0.022(3) 0.025(3) 0.032(3) -0.001(2) -0.003(2) 0.002(2) N1C 0.017(2) 0.015(2) 0.039(3) 0.002(2) 0.0029(19) 0.0018(18) N1D 0.008(2) 0.023(2) 0.031(2) 0.002(2) -0.0020(18) 0.0032(18) _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 C2A N3A 1.320(7) . ? C2A N1A 1.346(7) . ? C2A H2A 0.9300 . ? C2B N1B 1.350(8) . ? C2B N3B 1.339(7) . ? C2B H2B 0.9300 . ? C2C N1C 1.331(7) . ? C2C N3C 1.338(7) . ? C2C H2C 0.9300 . ? C2D N3D 1.350(7) . ? C2D N1D 1.348(7) . ? C2D H2D 0.9300 . ? C4A C5A 1.384(8) . ? C4A N3A 1.402(7) . ? C4A C7A 1.462(8) . ? C4B C5B 1.350(8) . ? C4B N3B 1.422(7) . ? C4B C7B 1.503(8) . ? C4C N3C 1.391(7) . ? C4C C5C 1.385(8) . ? C4C C7C 1.469(8) . ? C4D C5D 1.360(8) . ? C4D N3D 1.407(7) . ? C4D C7D 1.455(8) . ? C5A N1A 1.406(8) . ? C5A C13A 1.418(9) . ? C5B N1B 1.405(8) . ? C5B C13B 1.508(7) . ? C5C N1C 1.373(8) . ? C5C C13C 1.473(8) . ? C5D N1D 1.391(7) . ? C5D C13D 1.484(8) . ? C7A C12A 1.410(9) . ? C7A C8A 1.393(9) . ? C7B C8B 1.365(7) . ? C7B C12B 1.404(9) . ? C8C C9C 1.378(10) . ? C8C C7C 1.383(9) . ? C8C H8C 0.9300 . ? C9B C8B 1.369(6) . ? C9B C10B 1.433(12) . ? C9B H9B 0.9300 . ? C10B C11B 1.346(12) . ? C10B H10B 0.9300 . ? C11B C12B 1.368(10) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C7C C12C 1.394(8) . ? C7D C8D 1.387(9) . ? C7D C12D 1.396(8) . ? C8A C9A 1.372(9) . ? C8A H8A 0.9300 . ? C8B H8B 0.9300 . ? C8D C9D 1.396(9) . ? C8D H8D 0.9300 . ? C9A C10A 1.397(11) . ? C9A H9A 0.9300 . ? C9C C10C 1.416(11) . ? C9C H9C 0.9300 . ? C9D C10D 1.372(10) . ? C9D H9D 0.9300 . ? C10A C11A 1.412(11) . ? C10A H10A 0.9300 . ? C10C C11C 1.381(10) . ? C10C H10C 0.9300 . ? C10D C11D 1.372(10) . ? C10D H10D 0.9300 . ? C11A C12A 1.373(9) . ? C11A H11A 0.9300 . ? C11C C12C 1.406(10) . ? C11C H11C 0.9300 . ? C11D C12D 1.406(9) . ? C11D H11D 0.9300 . ? C12A H12A 0.9300 . ? C12C H12C 0.9300 . ? C12D H12D 0.9300 . ? C13A C18A 1.356(11) . ? C13A C14A 1.400(7) . ? C14A C15A 1.392(7) . ? C14A H14A 0.9300 . ? C15A C16A 1.381(6) . ? C15A H15A 0.9300 . ? C16A C17A 1.375(7) . ? C16A H16A 0.9300 . ? C17A C18A 1.394(7) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? C13B C14B 1.3900 . ? C13B C18B 1.3900 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? C16B C17B 1.3900 . ? C16B H16B 0.9300 . ? C17B C18B 1.3900 . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? C13C C14C 1.329(6) . ? C13C C18C 1.360(5) . ? C13D C18D 1.391(9) . ? C13D C14D 1.367(9) . ? C14C C15C 1.379(6) . ? C14C H14C 0.9300 . ? C14D C15D 1.380(10) . ? C14D H14D 0.9300 . ? C15C C16C 1.390(14) . ? C15C H15C 0.9300 . ? C15D C16D 1.367(12) . ? C15D H15D 0.9300 . ? C16C C17C 1.381(15) . ? C16C H16C 0.9300 . ? C16D C17D 1.355(12) . ? C16D H16D 0.9300 . ? C17C C18C 1.379(7) . ? C17C H17C 0.9300 . ? C17D C18D 1.403(10) . ? C17D H17D 0.9300 . ? C18C H18C 0.9300 . ? C18D H18D 0.9300 . ? O9 C19 1.189(11) . ? C19 C20 1.438(4) . ? C19 C21 1.487(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O10 1.271(8) . ? C22 C23 1.490(10) . ? C22 C24 1.478(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O11 1.223(8) . ? C25 C26 1.462(12) . ? C25 C27 1.501(11) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N3A Ni 1.901(4) . ? N3B Ni 1.906(5) . ? N3C Ni 1.897(5) . ? N3D Ni 1.882(5) . ? O1 Cl1 1.420(6) . ? O2 Cl1 1.465(5) . ? O3 Cl1 1.401(6) . ? O4 Cl1 1.428(6) . ? O5 Cl2 1.444(5) . ? O6 Cl2 1.443(5) . ? O7 Cl2 1.411(5) . ? O8 Cl2 1.447(5) . ? N1A H1A 0.888(11) . ? N1B H1B 0.887(10) . ? N1C H1C 0.886(10) . ? N1D H1D 0.876(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A C2A N1A 110.4(5) . . ? N3A C2A H2A 124.8 . . ? N1A C2A H2A 124.8 . . ? N1B C2B N3B 110.3(5) . . ? N1B C2B H2B 124.8 . . ? N3B C2B H2B 124.8 . . ? N1C C2C N3C 109.9(5) . . ? N1C C2C H2C 125.1 . . ? N3C C2C H2C 125.1 . . ? N3D C2D N1D 110.8(5) . . ? N3D C2D H2D 124.6 . . ? N1D C2D H2D 124.6 . . ? C5A C4A N3A 108.7(5) . . ? C5A C4A C7A 127.0(5) . . ? N3A C4A C7A 124.3(5) . . ? C5B C4B N3B 107.8(5) . . ? C5B C4B C7B 128.4(5) . . ? N3B C4B C7B 123.7(5) . . ? N3C C4C C5C 107.5(5) . . ? N3C C4C C7C 122.6(5) . . ? C5C C4C C7C 129.9(5) . . ? C5D C4D N3D 109.0(5) . . ? C5D C4D C7D 128.6(5) . . ? N3D C4D C7D 122.2(5) . . ? C4A C5A N1A 104.7(5) . . ? C4A C5A C13A 132.6(6) . . ? N1A C5A C13A 122.7(5) . . ? C4B C5B N1B 107.4(5) . . ? C4B C5B C13B 128.8(5) . . ? N1B C5B C13B 123.7(5) . . ? N1C C5C C4C 106.1(5) . . ? N1C C5C C13C 121.9(5) . . ? C4C C5C C13C 131.8(5) . . ? C4D C5D N1D 106.8(5) . . ? C4D C5D C13D 132.1(5) . . ? N1D C5D C13D 121.0(5) . . ? C12A C7A C8A 117.8(6) . . ? C12A C7A C4A 121.7(5) . . ? C8A C7A C4A 120.5(5) . . ? C8B C7B C12B 121.2(6) . . ? C8B C7B C4B 120.9(5) . . ? C12B C7B C4B 117.7(5) . . ? C9C C8C C7C 122.6(6) . . ? C9C C8C H8C 118.7 . . ? C7C C8C H8C 118.7 . . ? C8B C9B C10B 118.9(7) . . ? C8B C9B H9B 120.5 . . ? C10B C9B H9B 120.5 . . ? C11B C10B C9B 120.0(7) . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C12B C11B C10B 121.2(7) . . ? C12B C11B H11B 119.4 . . ? C10B C11B H11B 119.4 . . ? C11B C12B C7B 118.7(7) . . ? C11B C12B H12B 120.6 . . ? C7B C12B H12B 120.6 . . ? C8C C7C C12C 118.1(6) . . ? C8C C7C C4C 120.1(5) . . ? C12C C7C C4C 121.8(5) . . ? C8D C7D C12D 117.0(5) . . ? C8D C7D C4D 122.4(5) . . ? C12D C7D C4D 120.6(5) . . ? C9A C8A C7A 122.2(6) . . ? C9A C8A H8A 118.9 . . ? C7A C8A H8A 118.9 . . ? C7B C8B C9B 119.7(6) . . ? C7B C8B H8B 120.1 . . ? C9B C8B H8B 120.1 . . ? C7D C8D C9D 122.0(6) . . ? C7D C8D H8D 119.0 . . ? C9D C8D H8D 119.0 . . ? C8A C9A C10A 118.9(7) . . ? C8A C9A H9A 120.5 . . ? C10A C9A H9A 120.5 . . ? C8C C9C C10C 118.9(6) . . ? C8C C9C H9C 120.5 . . ? C10C C9C H9C 120.5 . . ? C10D C9D C8D 119.6(6) . . ? C10D C9D H9D 120.2 . . ? C8D C9D H9D 120.2 . . ? C11A C10A C9A 120.9(6) . . ? C11A C10A H10A 119.6 . . ? C9A C10A H10A 119.6 . . ? C11C C10C C9C 119.7(6) . . ? C11C C10C H10C 120.1 . . ? C9C C10C H10C 120.1 . . ? C11D C10D C9D 120.3(6) . . ? C11D C10D H10D 119.8 . . ? C9D C10D H10D 119.8 . . ? C12A C11A C10A 118.3(6) . . ? C12A C11A H11A 120.8 . . ? C10A C11A H11A 120.8 . . ? C10C C11C C12C 119.8(7) . . ? C10C C11C H11C 120.1 . . ? C12C C11C H11C 120.1 . . ? C10D C11D C12D 119.6(7) . . ? C10D C11D H11D 120.2 . . ? C12D C11D H11D 120.2 . . ? C11A C12A C7A 121.9(6) . . ? C11A C12A H12A 119.0 . . ? C7A C12A H12A 119.0 . . ? C7C C12C C11C 120.9(6) . . ? C7C C12C H12C 119.5 . . ? C11C C12C H12C 119.5 . . ? C11D C12D C7D 121.3(6) . . ? C11D C12D H12D 119.4 . . ? C7D C12D H12D 119.4 . . ? C18A C13A C14A 111.1(8) . . ? C18A C13A C5A 127.2(8) . . ? C14A C13A C5A 120.2(7) . . ? C15A C14A C13A 128.1(10) . . ? C15A C14A H14A 115.9 . . ? C13A C14A H14A 115.9 . . ? C16A C15A C14A 114.0(10) . . ? C16A C15A H15A 123.0 . . ? C14A C15A H15A 123.0 . . ? C15A C16A C17A 120.6(10) . . ? C15A C16A H16A 119.7 . . ? C17A C16A H16A 119.7 . . ? C18A C17A C16A 119.0(11) . . ? C18A C17A H17A 120.5 . . ? C16A C17A H17A 120.5 . . ? C13A C18A C17A 124.0(11) . . ? C13A C18A H18A 118.0 . . ? C17A C18A H18A 118.0 . . ? C14B C13B C18B 120.0 . . ? C14B C13B C5B 117.0(5) . . ? C18B C13B C5B 123.0(5) . . ? C15B C14B C13B 120.0 . . ? C15B C14B H14B 120.0 . . ? C13B C14B H14B 120.0 . . ? C14B C15B C16B 120.0 . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B H16B 120.0 . . ? C15B C16B H16B 120.0 . . ? C16B C17B C18B 120.0 . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C13B 120.0 . . ? C17B C18B H18B 120.0 . . ? C13B C18B H18B 120.0 . . ? C14C C13C C18C 118.5(6) . . ? C14C C13C C5C 120.6(5) . . ? C18C C13C C5C 120.8(5) . . ? C18D C13D C14D 120.4(6) . . ? C18D C13D C5D 120.1(6) . . ? C14D C13D C5D 119.4(6) . . ? C13C C14C C15C 122.3(7) . . ? C13C C14C H14C 118.8 . . ? C15C C14C H14C 118.8 . . ? C13D C14D C15D 120.4(7) . . ? C13D C14D H14D 119.8 . . ? C15D C14D H14D 119.8 . . ? C14C C15C C16C 117.1(8) . . ? C14C C15C H15C 121.4 . . ? C16C C15C H15C 121.4 . . ? C16D C15D C14D 118.9(7) . . ? C16D C15D H15D 120.6 . . ? C14D C15D H15D 120.6 . . ? C17C C16C C15C 122.8(7) . . ? C17C C16C H16C 118.6 . . ? C15C C16C H16C 118.6 . . ? C15D C16D C17D 122.3(7) . . ? C15D C16D H16D 118.9 . . ? C17D C16D H16D 118.9 . . ? C18C C17C C16C 114.7(10) . . ? C18C C17C H17C 122.7 . . ? C16C C17C H17C 122.7 . . ? C16D C17D C18D 119.1(8) . . ? C16D C17D H17D 120.5 . . ? C18D C17D H17D 120.5 . . ? C17C C18C C13C 124.1(8) . . ? C17C C18C H18C 117.9 . . ? C13C C18C H18C 117.9 . . ? C13D C18D C17D 118.8(7) . . ? C13D C18D H18D 120.6 . . ? C17D C18D H18D 120.6 . . ? O9 C19 C20 123.7(9) . . ? O9 C19 C21 124.6(8) . . ? C20 C19 C21 111.7(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O10 C22 C23 119.9(7) . . ? O10 C22 C24 122.9(6) . . ? C23 C22 C24 117.2(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O11 C25 C26 123.0(7) . . ? O11 C25 C27 119.7(8) . . ? C26 C25 C27 117.3(7) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C2A N3A C4A 107.3(4) . . ? C2A N3A Ni 120.4(4) . . ? C4A N3A Ni 129.7(4) . . ? C2B N3B C4B 106.8(5) . . ? C2B N3B Ni 120.3(4) . . ? C4B N3B Ni 130.6(4) . . ? C2C N3C C4C 107.3(5) . . ? C2C N3C Ni 124.6(4) . . ? C4C N3C Ni 128.1(4) . . ? C2D N3D C4D 105.6(5) . . ? C2D N3D Ni 123.3(4) . . ? C4D N3D Ni 130.9(4) . . ? O3 Cl1 O1 109.2(4) . . ? O3 Cl1 O4 112.5(4) . . ? O1 Cl1 O4 109.4(4) . . ? O3 Cl1 O2 110.5(4) . . ? O1 Cl1 O2 108.7(4) . . ? O4 Cl1 O2 106.4(3) . . ? O7 Cl2 O6 110.7(4) . . ? O7 Cl2 O5 110.4(3) . . ? O6 Cl2 O5 109.1(3) . . ? O7 Cl2 O8 109.2(3) . . ? O6 Cl2 O8 108.4(3) . . ? O5 Cl2 O8 109.0(3) . . ? N3D Ni N3C 88.1(2) . . ? N3D Ni N3A 90.23(19) . . ? N3C Ni N3A 177.5(2) . . ? N3D Ni N3B 177.7(2) . . ? N3C Ni N3B 90.9(2) . . ? N3A Ni N3B 90.8(2) . . ? C2A N1A C5A 108.8(5) . . ? C2A N1A H1A 110(5) . . ? C5A N1A H1A 141(5) . . ? C2B N1B C5B 107.6(5) . . ? C2B N1B H1B 114(4) . . ? C5B N1B H1B 138(4) . . ? C2C N1C C5C 109.2(4) . . ? C2C N1C H1C 132(4) . . ? C5C N1C H1C 118(4) . . ? C2D N1D C5D 107.8(4) . . ? C2D N1D H1D 115(4) . . ? C5D N1D H1D 137(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.956 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.116 # start Validation Reply Form _vrf_PLAT021_10-Ni{HL'}4_{ClO4}2_2.8Me2CO ; RESPONSE: The crystal studied was a non-merohedral twin with a ratio of the twin components of 36:64. For least-squares refinement of the batch scale factor it was necessary to suppress the merging of equivalent reflections. ; _vrf_PLAT220_10-Ni{HL'}4_{ClO4}2_2.8Me2CO ; RESPONSE: Due to twinning, the quality of the final analysis is certainly not as good as from an equivalent single crystal. Most of the following Alerts is the result of the disorder which affects the acetone molecules of crystallization, as well as some phenyl rings of the ligands of the complex. ; _vrf_PLAT077_10-Ni{HL'}4_{ClO4}2_2.8Me2CO ; RESPONSE: Alert due to a partially occupied (80%) solvent site (acetone molecule). ; # end Validation Reply Form #===END data_11-NiCl2L2 #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881072' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Cl2 N4 Ni' _chemical_formula_sum 'C32 H28 Cl2 N4 Ni' _chemical_formula_weight 598.19 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.4689(4) _cell_length_b 8.7125(2) _cell_length_c 18.7322(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2851.00(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5411 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 28.99 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87815 _exptl_absorpt_correction_T_max 0.89000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0288 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23736 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 28.99 _reflns_number_total 3777 _reflns_number_gt 2365 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)' _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2009). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3777 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _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 Ni Ni 1.0000 0.32476(4) 0.2500 0.01523(8) Uani 1 2 d S . . Cl Cl 0.90203(2) 0.18119(5) 0.21114(2) 0.01971(11) Uani 1 1 d . . . N1A N 1.15655(8) 0.61067(16) 0.15382(7) 0.0151(3) Uani 1 1 d . . . C2A C 1.13364(10) 0.4854(2) 0.18944(9) 0.0156(4) Uani 1 1 d . . . H2A H 1.1666 0.4142 0.2100 0.019 Uiso 1 1 calc R . . N3A N 1.05780(8) 0.47618(16) 0.19161(7) 0.0133(3) Uani 1 1 d . . . C4A C 1.03092(10) 0.60589(19) 0.15652(9) 0.0125(4) Uani 1 1 d . . . C5A C 1.09163(9) 0.6908(2) 0.13257(9) 0.0134(4) Uani 1 1 d . . . C6A C 1.23633(10) 0.6533(2) 0.14082(10) 0.0243(5) Uani 1 1 d . . . H6A1 H 1.2668 0.6262 0.1816 0.037 Uiso 1 1 calc R . . H6A2 H 1.2396 0.7620 0.1329 0.037 Uiso 1 1 calc R . . H6A3 H 1.2549 0.5998 0.0995 0.037 Uiso 1 1 calc R . . C7A C 0.94782(10) 0.6332(2) 0.14849(9) 0.0140(4) Uani 1 1 d . . . C8A C 0.90285(10) 0.5259(2) 0.11257(9) 0.0166(4) Uani 1 1 d . . . H8A H 0.9254 0.4391 0.0929 0.020 Uiso 1 1 calc R . . C9A C 0.82425(10) 0.5483(2) 0.10609(10) 0.0211(4) Uani 1 1 d . . . H9A H 0.7946 0.4764 0.0821 0.025 Uiso 1 1 calc R . . C10A C 0.79012(10) 0.6772(2) 0.13522(9) 0.0207(4) Uani 1 1 d . . . H10A H 0.7376 0.6917 0.1309 0.025 Uiso 1 1 calc R . . C11A C 0.83441(10) 0.7840(2) 0.17068(9) 0.0186(4) Uani 1 1 d . . . H11A H 0.8115 0.8705 0.1905 0.022 Uiso 1 1 calc R . . C12A C 0.91294(10) 0.7630(2) 0.17689(9) 0.0163(4) Uani 1 1 d . . . H12A H 0.9424 0.8364 0.2002 0.020 Uiso 1 1 calc R . . C13A C 1.09508(9) 0.8339(2) 0.09041(9) 0.0135(4) Uani 1 1 d . . . C14A C 1.12006(10) 0.8310(2) 0.01980(9) 0.0186(4) Uani 1 1 d . . . H14A H 1.1366 0.7392 -0.0003 0.022 Uiso 1 1 calc R . . C15A C 1.12050(10) 0.9641(2) -0.02067(10) 0.0203(4) Uani 1 1 d . . . H15A H 1.1369 0.9610 -0.0679 0.024 Uiso 1 1 calc R . . C16A C 1.09678(10) 1.1010(2) 0.00877(9) 0.0180(4) Uani 1 1 d . . . H16A H 1.0971 1.1902 -0.0185 0.022 Uiso 1 1 calc R . . C17A C 1.07255(10) 1.1052(2) 0.07886(10) 0.0192(4) Uani 1 1 d . . . H17A H 1.0565 1.1976 0.0988 0.023 Uiso 1 1 calc R . . C18A C 1.07196(10) 0.9727(2) 0.11972(10) 0.0175(4) Uani 1 1 d . . . H18A H 1.0560 0.9767 0.1670 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01402(16) 0.01064(15) 0.02103(17) 0.000 0.00372(14) 0.000 Cl 0.0192(2) 0.0176(2) 0.0224(2) -0.0034(2) -0.00280(18) -0.0010(2) N1A 0.0111(8) 0.0150(8) 0.0193(8) 0.0016(6) 0.0016(6) -0.0009(6) C2A 0.0149(9) 0.0143(9) 0.0176(10) 0.0000(7) 0.0000(7) 0.0028(7) N3A 0.0123(8) 0.0126(8) 0.0149(8) -0.0015(6) 0.0009(6) 0.0006(6) C4A 0.0141(9) 0.0100(9) 0.0135(9) -0.0009(7) 0.0003(7) 0.0017(7) C5A 0.0122(8) 0.0141(9) 0.0137(8) -0.0035(7) -0.0001(7) 0.0032(8) C6A 0.0121(9) 0.0255(12) 0.0355(12) 0.0066(9) 0.0013(8) -0.0029(8) C7A 0.0140(9) 0.0153(9) 0.0129(9) 0.0058(7) 0.0021(7) 0.0002(7) C8A 0.0175(9) 0.0116(9) 0.0207(10) 0.0016(8) 0.0005(8) 0.0007(8) C9A 0.0164(10) 0.0179(10) 0.0289(11) 0.0038(8) -0.0043(8) -0.0054(8) C10A 0.0119(9) 0.0228(10) 0.0274(11) 0.0057(9) -0.0002(7) 0.0021(9) C11A 0.0171(9) 0.0192(10) 0.0194(10) 0.0032(8) 0.0036(8) 0.0050(8) C12A 0.0176(10) 0.0147(9) 0.0165(10) 0.0023(8) -0.0001(7) -0.0018(8) C13A 0.0082(8) 0.0148(9) 0.0176(9) 0.0021(8) -0.0026(7) -0.0016(8) C14A 0.0193(9) 0.0175(9) 0.0191(9) -0.0026(9) 0.0028(7) 0.0026(9) C15A 0.0223(10) 0.0250(11) 0.0135(10) 0.0026(8) 0.0023(8) 0.0004(9) C16A 0.0148(9) 0.0178(9) 0.0213(10) 0.0058(8) -0.0029(8) -0.0016(8) C17A 0.0193(10) 0.0136(10) 0.0246(11) -0.0024(8) 0.0018(8) 0.0003(8) C18A 0.0169(10) 0.0197(10) 0.0157(10) -0.0005(8) 0.0030(7) -0.0032(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 Ni N3A 1.9890(14) 4_755 ? Ni N3A 1.9890(14) . ? Ni Cl 2.2413(5) 4_755 ? Ni Cl 2.2414(5) . ? N1A C2A 1.340(2) . ? N1A C5A 1.390(2) . ? N1A C6A 1.463(2) . ? C2A N3A 1.328(2) . ? C2A H2A 0.9300 . ? N3A C4A 1.389(2) . ? C4A C5A 1.368(2) . ? C4A C7A 1.479(2) . ? C5A C13A 1.477(2) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C12A 1.391(2) . ? C7A C8A 1.394(2) . ? C8A C9A 1.392(2) . ? C8A H8A 0.9300 . ? C9A C10A 1.383(2) . ? C9A H9A 0.9300 . ? C10A C11A 1.381(2) . ? C10A H10A 0.9300 . ? C11A C12A 1.389(2) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C18A 1.388(2) . ? C13A C14A 1.393(2) . ? C14A C15A 1.385(2) . ? C14A H14A 0.9300 . ? C15A C16A 1.378(2) . ? C15A H15A 0.9300 . ? C16A C17A 1.380(2) . ? C16A H16A 0.9300 . ? C17A C18A 1.385(2) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? 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 N3A Ni N3A 96.90(8) 4_755 . ? N3A Ni Cl 125.40(4) 4_755 4_755 ? N3A Ni Cl 99.27(4) . 4_755 ? N3A Ni Cl 99.27(4) 4_755 . ? N3A Ni Cl 125.39(4) . . ? Cl Ni Cl 112.15(3) 4_755 . ? C2A N1A C5A 107.92(14) . . ? C2A N1A C6A 125.05(15) . . ? C5A N1A C6A 127.02(14) . . ? N3A C2A N1A 111.25(15) . . ? N3A C2A H2A 124.4 . . ? N1A C2A H2A 124.4 . . ? C2A N3A C4A 105.88(14) . . ? C2A N3A Ni 124.30(12) . . ? C4A N3A Ni 128.91(11) . . ? C5A C4A N3A 109.43(15) . . ? C5A C4A C7A 129.83(16) . . ? N3A C4A C7A 120.73(15) . . ? C4A C5A N1A 105.50(14) . . ? C4A C5A C13A 131.53(15) . . ? N1A C5A C13A 122.93(14) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C12A C7A C8A 118.89(16) . . ? C12A C7A C4A 121.47(16) . . ? C8A C7A C4A 119.64(16) . . ? C9A C8A C7A 120.27(17) . . ? C9A C8A H8A 119.9 . . ? C7A C8A H8A 119.9 . . ? C10A C9A C8A 120.29(17) . . ? C10A C9A H9A 119.9 . . ? C8A C9A H9A 119.9 . . ? C11A C10A C9A 119.70(16) . . ? C11A C10A H10A 120.2 . . ? C9A C10A H10A 120.1 . . ? C10A C11A C12A 120.33(17) . . ? C10A C11A H11A 119.8 . . ? C12A C11A H11A 119.8 . . ? C11A C12A C7A 120.52(17) . . ? C11A C12A H12A 119.7 . . ? C7A C12A H12A 119.7 . . ? C18A C13A C14A 118.81(16) . . ? C18A C13A C5A 120.81(15) . . ? C14A C13A C5A 120.37(16) . . ? C15A C14A C13A 120.45(17) . . ? C15A C14A H14A 119.8 . . ? C13A C14A H14A 119.8 . . ? C16A C15A C14A 120.25(17) . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C15A C16A C17A 119.74(17) . . ? C15A C16A H16A 120.1 . . ? C17A C16A H16A 120.1 . . ? C16A C17A C18A 120.38(17) . . ? C16A C17A H17A 119.8 . . ? C18A C17A H17A 119.8 . . ? C17A C18A C13A 120.37(17) . . ? C17A C18A H18A 119.8 . . ? C13A C18A H18A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.356 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.064 #===END data_12-NiBr2L2 #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881073' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Br2 N4 Ni' _chemical_formula_sum 'C32 H28 Br2 N4 Ni' _chemical_formula_weight 687.11 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x+1/2, z+1/4' 'y, -x+1/2, z+1/4' '-x, y, z+1/2' 'x, -y, z+1/2' 'y+1/2, x, z+1/4' '-y+1/2, -x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' 'y+1/2, -x+1, z+3/4' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' 'y+1, x+1/2, z+3/4' '-y+1, -x+1/2, z+3/4' _cell_length_a 28.6711(3) _cell_length_b 28.6711(3) _cell_length_c 14.0797(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11574.0(2) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19875 _cell_measurement_theta_min 3.0087 _cell_measurement_theta_max 30.3491 _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 3.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7722 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-3 with Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49601 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7673 _reflns_number_gt 6247 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^] 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, 3674 Friedel pairs' _refine_ls_abs_structure_Flack -0.010(5) _refine_ls_number_reflns 7673 _refine_ls_number_parameters 354 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.669738(10) 0.476507(10) 0.55264(2) 0.01627(7) Uani 1 1 d . . . Br2 Br 0.727746(10) 0.485099(9) 0.67091(2) 0.03036(7) Uani 1 1 d . . . Br1 Br 0.660080(8) 0.546456(8) 0.460990(19) 0.02022(6) Uani 1 1 d . . . N1A N 0.57838(6) 0.40212(6) 0.71889(14) 0.0149(4) Uani 1 1 d . . . C2A C 0.61419(8) 0.43109(8) 0.70349(17) 0.0154(5) Uani 1 1 d . . . H2A H 0.6360 0.4394 0.7494 0.019 Uiso 1 1 calc R . . N3A N 0.61472(7) 0.44649(6) 0.61444(13) 0.0153(4) Uani 1 1 d . . . C4A C 0.57733(8) 0.42511(8) 0.57008(17) 0.0149(5) Uani 1 1 d . . . C5A C 0.55411(8) 0.39760(8) 0.63355(17) 0.0141(5) Uani 1 1 d . . . C6A C 0.56713(9) 0.38185(9) 0.81125(17) 0.0223(6) Uani 1 1 d . . . H6A1 H 0.5347 0.3867 0.8248 0.033 Uiso 1 1 calc R . . H6A2 H 0.5857 0.3965 0.8595 0.033 Uiso 1 1 calc R . . H6A3 H 0.5737 0.3490 0.8102 0.033 Uiso 1 1 calc R . . C7A C 0.56779(7) 0.43268(8) 0.46811(17) 0.0139(5) Uani 1 1 d . . . C8A C 0.56178(8) 0.47748(8) 0.43325(17) 0.0179(5) Uani 1 1 d . . . H8A H 0.5618 0.5027 0.4747 0.022 Uiso 1 1 calc R . . C9A C 0.55573(8) 0.48476(9) 0.33652(18) 0.0218(6) Uani 1 1 d . . . H9A H 0.5516 0.5149 0.3136 0.026 Uiso 1 1 calc R . . C10A C 0.55583(9) 0.44793(9) 0.27480(17) 0.0231(6) Uani 1 1 d . . . H10A H 0.5527 0.4531 0.2099 0.028 Uiso 1 1 calc R . . C11A C 0.56065(8) 0.40301(9) 0.30897(18) 0.0201(6) Uani 1 1 d . . . H11A H 0.5602 0.3779 0.2671 0.024 Uiso 1 1 calc R . . C12A C 0.56609(8) 0.39532(8) 0.40504(17) 0.0159(5) Uani 1 1 d . . . H12A H 0.5686 0.3650 0.4278 0.019 Uiso 1 1 calc R . . C13A C 0.51200(8) 0.36829(8) 0.62072(16) 0.0155(5) Uani 1 1 d . . . C14A C 0.47450(8) 0.38616(8) 0.57063(16) 0.0174(5) Uani 1 1 d . . . H14A H 0.4762 0.4162 0.5461 0.021 Uiso 1 1 calc R . . C15A C 0.43448(9) 0.35986(9) 0.55648(17) 0.0225(6) Uani 1 1 d . . . H15A H 0.4093 0.3723 0.5235 0.027 Uiso 1 1 calc R . . C16A C 0.43242(9) 0.31512(9) 0.59182(18) 0.0248(6) Uani 1 1 d . . . H16A H 0.4058 0.2972 0.5825 0.030 Uiso 1 1 calc R . . C17A C 0.46998(9) 0.29679(9) 0.64129(18) 0.0242(6) Uani 1 1 d . . . H17A H 0.4686 0.2665 0.6647 0.029 Uiso 1 1 calc R . . C18A C 0.50911(9) 0.32318(8) 0.65574(17) 0.0196(6) Uani 1 1 d . . . H18A H 0.5341 0.3107 0.6895 0.023 Uiso 1 1 calc R . . N1B N 0.68278(6) 0.39292(6) 0.31983(13) 0.0146(4) Uani 1 1 d . . . C2B C 0.68457(8) 0.43251(8) 0.36936(17) 0.0159(5) Uani 1 1 d . . . H2B H 0.6872 0.4620 0.3425 0.019 Uiso 1 1 calc R . . N3B N 0.68215(6) 0.42426(6) 0.46186(15) 0.0149(4) Uani 1 1 d . . . C4B C 0.67849(8) 0.37579(7) 0.47113(17) 0.0134(5) Uani 1 1 d . . . C5B C 0.67877(8) 0.35654(8) 0.38307(17) 0.0133(5) Uani 1 1 d . . . C6B C 0.68690(10) 0.38950(8) 0.21633(18) 0.0256(6) Uani 1 1 d . . . H6B1 H 0.6938 0.4197 0.1905 0.038 Uiso 1 1 calc R . . H6B2 H 0.6580 0.3783 0.1902 0.038 Uiso 1 1 calc R . . H6B3 H 0.7115 0.3682 0.2005 0.038 Uiso 1 1 calc R . . C7B C 0.67472(8) 0.35268(7) 0.56373(17) 0.0126(5) Uani 1 1 d . . . C8B C 0.70400(9) 0.36560(8) 0.63925(17) 0.0191(6) Uani 1 1 d . . . H8B H 0.7270 0.3880 0.6296 0.023 Uiso 1 1 calc R . . C9B C 0.69888(9) 0.34544(8) 0.72760(18) 0.0228(6) Uani 1 1 d . . . H9B H 0.7181 0.3547 0.7774 0.027 Uiso 1 1 calc R . . C10B C 0.66531(9) 0.31144(9) 0.74272(18) 0.0234(6) Uani 1 1 d . . . H10B H 0.6622 0.2978 0.8023 0.028 Uiso 1 1 calc R . . C11B C 0.63653(9) 0.29795(8) 0.66917(19) 0.0198(5) Uani 1 1 d . . . H11B H 0.6139 0.2753 0.6793 0.024 Uiso 1 1 calc R . . C12B C 0.64134(8) 0.31811(8) 0.58030(17) 0.0167(5) Uani 1 1 d . . . H12B H 0.6221 0.3085 0.5309 0.020 Uiso 1 1 calc R . . C13B C 0.67735(8) 0.30720(8) 0.34945(16) 0.0136(5) Uani 1 1 d . . . C14B C 0.71276(8) 0.27608(8) 0.37328(17) 0.0155(5) Uani 1 1 d . . . H14B H 0.7367 0.2855 0.4136 0.019 Uiso 1 1 calc R . . C15B C 0.71258(8) 0.23124(8) 0.33741(17) 0.0176(5) Uani 1 1 d . . . H15B H 0.7367 0.2109 0.3528 0.021 Uiso 1 1 calc R . . C16B C 0.67722(9) 0.21644(8) 0.27945(17) 0.0197(6) Uani 1 1 d . . . H16B H 0.6773 0.1862 0.2554 0.024 Uiso 1 1 calc R . . C17B C 0.64129(9) 0.24668(9) 0.25694(17) 0.0190(6) Uani 1 1 d . . . H17B H 0.6170 0.2366 0.2182 0.023 Uiso 1 1 calc R . . C18B C 0.64131(8) 0.29165(8) 0.29168(17) 0.0178(5) Uani 1 1 d . . . H18B H 0.6170 0.3117 0.2763 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02121(17) 0.01443(15) 0.01317(16) -0.00299(13) 0.00256(14) -0.00226(14) Br2 0.03804(17) 0.02432(14) 0.02870(15) -0.00538(13) -0.01239(13) 0.00192(13) Br1 0.02143(13) 0.01696(12) 0.02227(13) 0.00112(11) -0.00284(11) -0.00104(10) N1A 0.0167(10) 0.0172(10) 0.0109(10) 0.0008(9) 0.0004(9) 0.0013(8) C2A 0.0172(12) 0.0176(12) 0.0116(12) -0.0037(10) -0.0015(10) 0.0050(10) N3A 0.0182(11) 0.0166(10) 0.0111(11) -0.0011(8) 0.0004(9) 0.0028(9) C4A 0.0158(12) 0.0139(12) 0.0150(13) -0.0016(10) -0.0003(10) 0.0026(10) C5A 0.0151(12) 0.0156(12) 0.0117(12) 0.0001(10) 0.0001(10) 0.0049(10) C6A 0.0260(14) 0.0289(15) 0.0121(13) 0.0001(11) 0.0017(11) 0.0002(12) C7A 0.0093(11) 0.0208(12) 0.0116(12) 0.0017(11) 0.0011(10) -0.0017(9) C8A 0.0192(12) 0.0181(13) 0.0165(13) -0.0014(10) -0.0011(10) -0.0034(10) C9A 0.0224(14) 0.0203(14) 0.0227(14) 0.0071(12) -0.0047(11) -0.0041(11) C10A 0.0250(15) 0.0305(16) 0.0138(14) 0.0043(12) -0.0035(11) -0.0052(12) C11A 0.0199(13) 0.0256(14) 0.0148(13) -0.0038(12) -0.0028(11) 0.0026(11) C12A 0.0144(12) 0.0154(12) 0.0178(14) 0.0017(10) -0.0005(10) 0.0032(10) C13A 0.0190(13) 0.0174(13) 0.0102(12) -0.0030(10) 0.0043(10) 0.0009(10) C14A 0.0218(13) 0.0201(13) 0.0105(12) 0.0015(10) 0.0043(10) -0.0011(11) C15A 0.0227(14) 0.0336(15) 0.0112(12) -0.0014(12) -0.0003(11) -0.0017(12) C16A 0.0271(15) 0.0292(15) 0.0180(14) -0.0048(12) 0.0040(12) -0.0106(13) C17A 0.0289(15) 0.0191(14) 0.0246(15) -0.0018(11) 0.0095(12) -0.0018(12) C18A 0.0209(13) 0.0210(13) 0.0168(14) -0.0027(11) 0.0028(11) 0.0045(11) N1B 0.0216(11) 0.0128(10) 0.0094(10) -0.0030(8) 0.0027(9) 0.0002(9) C2B 0.0207(13) 0.0146(12) 0.0126(13) -0.0001(10) 0.0052(10) 0.0000(10) N3B 0.0204(11) 0.0106(9) 0.0136(10) 0.0019(9) 0.0019(9) -0.0005(8) C4B 0.0120(11) 0.0126(11) 0.0156(13) -0.0022(10) 0.0019(10) 0.0016(9) C5B 0.0136(12) 0.0134(12) 0.0129(12) 0.0003(10) 0.0021(10) 0.0002(10) C6B 0.0494(17) 0.0175(13) 0.0101(12) -0.0013(11) 0.0050(13) -0.0042(12) C7B 0.0137(12) 0.0103(11) 0.0137(12) 0.0009(10) 0.0007(10) 0.0058(10) C8B 0.0251(14) 0.0151(13) 0.0171(13) -0.0005(10) -0.0016(11) 0.0025(11) C9B 0.0341(15) 0.0183(13) 0.0159(14) 0.0015(11) -0.0053(12) 0.0062(12) C10B 0.0362(16) 0.0206(14) 0.0135(13) 0.0068(10) 0.0048(12) 0.0113(12) C11B 0.0211(13) 0.0109(11) 0.0275(14) 0.0053(11) 0.0042(12) 0.0046(10) C12B 0.0178(12) 0.0140(12) 0.0184(14) -0.0009(10) -0.0008(10) 0.0072(10) C13B 0.0166(12) 0.0137(12) 0.0105(12) 0.0012(9) 0.0048(10) -0.0001(10) C14B 0.0158(12) 0.0155(13) 0.0152(13) -0.0010(10) -0.0031(10) -0.0025(10) C15B 0.0199(13) 0.0147(12) 0.0182(13) 0.0047(10) 0.0016(11) 0.0042(11) C16B 0.0329(15) 0.0106(12) 0.0155(14) -0.0009(10) 0.0087(11) -0.0031(11) C17B 0.0232(13) 0.0199(14) 0.0139(12) -0.0029(10) -0.0018(11) -0.0055(11) C18B 0.0179(13) 0.0190(13) 0.0165(13) 0.0003(11) -0.0024(11) 0.0005(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 Ni N3A 1.997(2) . ? Ni N3B 2.0010(19) . ? Ni Br2 2.3663(4) . ? Ni Br1 2.4008(4) . ? N1A C2A 1.338(3) . ? N1A C5A 1.395(3) . ? N1A C6A 1.460(3) . ? C2A N3A 1.329(3) . ? C2A H2A 0.9300 . ? N3A C4A 1.384(3) . ? C4A C5A 1.365(3) . ? C4A C7A 1.477(3) . ? C5A C13A 1.482(3) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C8A 1.386(3) . ? C7A C12A 1.392(3) . ? C8A C9A 1.389(3) . ? C8A H8A 0.9300 . ? C9A C10A 1.368(3) . ? C9A H9A 0.9300 . ? C10A C11A 1.382(3) . ? C10A H10A 0.9300 . ? C11A C12A 1.379(3) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C14A 1.384(3) . ? C13A C18A 1.387(3) . ? C14A C15A 1.388(3) . ? C14A H14A 0.9300 . ? C15A C16A 1.377(3) . ? C15A H15A 0.9300 . ? C16A C17A 1.386(4) . ? C16A H16A 0.9300 . ? C17A C18A 1.368(3) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? N1B C2B 1.333(3) . ? N1B C5B 1.376(3) . ? N1B C6B 1.465(3) . ? C2B N3B 1.325(3) . ? C2B H2B 0.9300 . ? N3B C4B 1.400(3) . ? C4B C5B 1.357(3) . ? C4B C7B 1.466(3) . ? C5B C13B 1.492(3) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B C12B 1.397(3) . ? C7B C8B 1.405(3) . ? C8B C9B 1.379(3) . ? C8B H8B 0.9300 . ? C9B C10B 1.386(4) . ? C9B H9B 0.9300 . ? C10B C11B 1.379(3) . ? C10B H10B 0.9300 . ? C11B C12B 1.385(3) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C18B 1.388(3) . ? C13B C14B 1.393(3) . ? C14B C15B 1.381(3) . ? C14B H14B 0.9300 . ? C15B C16B 1.369(3) . ? C15B H15B 0.9300 . ? C16B C17B 1.383(3) . ? C16B H16B 0.9300 . ? C17B C18B 1.379(3) . ? C17B H17B 0.9300 . ? C18B H18B 0.9300 . ? 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 N3A Ni N3B 95.52(8) . . ? N3A Ni Br2 107.07(6) . . ? N3B Ni Br2 113.73(6) . . ? N3A Ni Br1 120.22(5) . . ? N3B Ni Br1 107.61(6) . . ? Br2 Ni Br1 111.860(15) . . ? C2A N1A C5A 107.51(19) . . ? C2A N1A C6A 124.1(2) . . ? C5A N1A C6A 128.31(19) . . ? N3A C2A N1A 111.6(2) . . ? N3A C2A H2A 124.2 . . ? N1A C2A H2A 124.2 . . ? C2A N3A C4A 105.64(19) . . ? C2A N3A Ni 124.28(16) . . ? C4A N3A Ni 127.32(15) . . ? C5A C4A N3A 109.8(2) . . ? C5A C4A C7A 129.1(2) . . ? N3A C4A C7A 121.1(2) . . ? C4A C5A N1A 105.5(2) . . ? C4A C5A C13A 130.2(2) . . ? N1A C5A C13A 124.4(2) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A C12A 118.9(2) . . ? C8A C7A C4A 120.2(2) . . ? C12A C7A C4A 120.9(2) . . ? C7A C8A C9A 120.2(2) . . ? C7A C8A H8A 119.9 . . ? C9A C8A H8A 119.9 . . ? C10A C9A C8A 120.4(2) . . ? C10A C9A H9A 119.8 . . ? C8A C9A H9A 119.8 . . ? C9A C10A C11A 119.9(2) . . ? C9A C10A H10A 120.0 . . ? C11A C10A H10A 120.0 . . ? C12A C11A C10A 120.1(2) . . ? C12A C11A H11A 119.9 . . ? C10A C11A H11A 119.9 . . ? C11A C12A C7A 120.4(2) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C14A C13A C18A 118.7(2) . . ? C14A C13A C5A 119.0(2) . . ? C18A C13A C5A 122.3(2) . . ? C13A C14A C15A 120.9(2) . . ? C13A C14A H14A 119.5 . . ? C15A C14A H14A 119.5 . . ? C16A C15A C14A 119.3(2) . . ? C16A C15A H15A 120.3 . . ? C14A C15A H15A 120.3 . . ? C15A C16A C17A 120.1(2) . . ? C15A C16A H16A 119.9 . . ? C17A C16A H16A 119.9 . . ? C18A C17A C16A 120.1(2) . . ? C18A C17A H17A 119.9 . . ? C16A C17A H17A 119.9 . . ? C17A C18A C13A 120.8(2) . . ? C17A C18A H18A 119.6 . . ? C13A C18A H18A 119.6 . . ? C2B N1B C5B 108.06(19) . . ? C2B N1B C6B 125.0(2) . . ? C5B N1B C6B 126.83(19) . . ? N3B C2B N1B 111.1(2) . . ? N3B C2B H2B 124.4 . . ? N1B C2B H2B 124.4 . . ? C2B N3B C4B 105.8(2) . . ? C2B N3B Ni 120.22(15) . . ? C4B N3B Ni 132.09(17) . . ? C5B C4B N3B 108.5(2) . . ? C5B C4B C7B 129.0(2) . . ? N3B C4B C7B 122.5(2) . . ? C4B C5B N1B 106.46(19) . . ? C4B C5B C13B 132.5(2) . . ? N1B C5B C13B 121.0(2) . . ? N1B C6B H6B1 109.5 . . ? N1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? N1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C12B C7B C8B 118.0(2) . . ? C12B C7B C4B 121.3(2) . . ? C8B C7B C4B 120.7(2) . . ? C9B C8B C7B 120.6(2) . . ? C9B C8B H8B 119.7 . . ? C7B C8B H8B 119.7 . . ? C8B C9B C10B 120.5(2) . . ? C8B C9B H9B 119.8 . . ? C10B C9B H9B 119.8 . . ? C11B C10B C9B 119.8(2) . . ? C11B C10B H10B 120.1 . . ? C9B C10B H10B 120.1 . . ? C10B C11B C12B 120.1(2) . . ? C10B C11B H11B 119.9 . . ? C12B C11B H11B 119.9 . . ? C11B C12B C7B 121.0(2) . . ? C11B C12B H12B 119.5 . . ? C7B C12B H12B 119.5 . . ? C18B C13B C14B 118.5(2) . . ? C18B C13B C5B 120.7(2) . . ? C14B C13B C5B 120.7(2) . . ? C15B C14B C13B 120.4(2) . . ? C15B C14B H14B 119.8 . . ? C13B C14B H14B 119.8 . . ? C16B C15B C14B 120.6(2) . . ? C16B C15B H15B 119.7 . . ? C14B C15B H15B 119.7 . . ? C15B C16B C17B 119.6(2) . . ? C15B C16B H16B 120.2 . . ? C17B C16B H16B 120.2 . . ? C18B C17B C16B 120.3(2) . . ? C18B C17B H17B 119.9 . . ? C16B C17B H17B 119.9 . . ? C17B C18B C13B 120.6(2) . . ? C17B C18B H18B 119.7 . . ? C13B C18B H18B 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.515 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.062 # start Validation Reply Form _vrf_REFLT03_12-NiBr2L2 ; RESPONSE: The Flack absolute structure parameter x has been reliably determined by means of 3674 Friedel pairs. ; # end Validation Reply Form #===END data_13-Ni{NO2}2L2 #TrackingRef '- Revised_CIF_CE-ART-05-2012-025704.cif' _database_code_depnum_ccdc_archive 'CCDC 881074' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 N6 Ni O4' _chemical_formula_sum 'C32 H28 N6 Ni O4' _chemical_formula_weight 619.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.0809(3) _cell_length_b 7.3878(5) _cell_length_c 16.0562(10) _cell_angle_alpha 100.554(6) _cell_angle_beta 98.892(5) _cell_angle_gamma 94.548(5) _cell_volume 696.28(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2856 _cell_measurement_theta_min 2.8397 _cell_measurement_theta_max 62.4387 _exptl_crystal_description rod _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 322 _exptl_absorpt_coefficient_mu 1.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75820 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction SuperNova with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4223 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2135 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 62.53 _reflns_number_total 2135 _reflns_number_gt 2014 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2010)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990); MERCURY (Bruno et al. 2002) ; _computing_publication_material 'WINGX (Farrugia, 1999)' _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxford, England. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.1023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2135 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1905 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Ni Ni 1.0000 0.0000 0.5000 0.0140(4) Uani 1 2 d S . . N1A N 0.5499(9) -0.4294(7) 0.3520(3) 0.0160(11) Uani 1 1 d . . . N3A N 0.8327(9) -0.2101(7) 0.4041(3) 0.0160(11) Uani 1 1 d . . . C2A C 0.6580(10) -0.3049(9) 0.4215(4) 0.0166(13) Uani 1 1 d . . . H2A H 0.6145 -0.2881 0.4752 0.020 Uiso 1 1 calc R . . C4A C 0.8372(10) -0.2754(9) 0.3172(4) 0.0153(13) Uani 1 1 d . . . C5A C 0.6627(10) -0.4141(8) 0.2846(4) 0.0154(13) Uani 1 1 d . . . C6A C 0.3578(10) -0.5569(9) 0.3520(4) 0.0189(14) Uani 1 1 d . . . H6A1 H 0.4036 -0.6779 0.3532 0.028 Uiso 1 1 calc R . . H6A2 H 0.2499 -0.5620 0.3009 0.028 Uiso 1 1 calc R . . H6A3 H 0.2919 -0.5156 0.4017 0.028 Uiso 1 1 calc R . . C7A C 0.9985(10) -0.1944(8) 0.2711(4) 0.0159(13) Uani 1 1 d . . . C8A C 1.2172(10) -0.1248(8) 0.3128(4) 0.0159(13) Uani 1 1 d . . . H8A H 1.2626 -0.1327 0.3699 0.019 Uiso 1 1 calc R . . C9A C 1.3664(11) -0.0441(9) 0.2691(4) 0.0201(14) Uani 1 1 d . . . H9A H 1.5114 0.0006 0.2970 0.024 Uiso 1 1 calc R . . C10A C 1.2996(11) -0.0297(9) 0.1839(4) 0.0216(15) Uani 1 1 d . . . H10A H 1.3989 0.0249 0.1547 0.026 Uiso 1 1 calc R . . C11A C 1.0832(11) -0.0979(9) 0.1430(4) 0.0203(14) Uani 1 1 d . . . H11A H 1.0379 -0.0898 0.0859 0.024 Uiso 1 1 calc R . . C12A C 0.9337(11) -0.1780(9) 0.1863(4) 0.0184(14) Uani 1 1 d . . . H12A H 0.7884 -0.2211 0.1582 0.022 Uiso 1 1 calc R . . C13A C 0.5953(10) -0.5314(8) 0.1980(4) 0.0167(13) Uani 1 1 d . . . C14A C 0.7458(11) -0.6447(9) 0.1635(4) 0.0216(14) Uani 1 1 d . . . H14A H 0.8841 -0.6513 0.1963 0.026 Uiso 1 1 calc R . . C15A C 0.6877(12) -0.7484(9) 0.0795(4) 0.0245(15) Uani 1 1 d . . . H15A H 0.7883 -0.8227 0.0561 0.029 Uiso 1 1 calc R . . C16A C 0.4808(11) -0.7405(9) 0.0313(4) 0.0214(14) Uani 1 1 d . . . H16A H 0.4417 -0.8106 -0.0242 0.026 Uiso 1 1 calc R . . C17A C 0.3312(11) -0.6275(9) 0.0657(4) 0.0212(14) Uani 1 1 d . . . H17A H 0.1928 -0.6212 0.0330 0.025 Uiso 1 1 calc R . . C18A C 0.3883(10) -0.5241(9) 0.1491(4) 0.0191(14) Uani 1 1 d . . . H18A H 0.2873 -0.4498 0.1721 0.023 Uiso 1 1 calc R . . N1 N 1.1753(10) -0.2428(8) 0.5754(4) 0.0256(13) Uani 1 1 d . . . O1 O 0.9899(8) -0.1845(6) 0.5855(3) 0.0227(10) Uani 1 1 d . . . O2 O 1.2672(8) -0.1642(6) 0.5226(3) 0.0249(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0154(8) 0.0139(8) 0.0122(7) 0.0012(6) 0.0024(6) 0.0015(6) N1A 0.019(3) 0.016(3) 0.012(3) 0.000(2) 0.004(2) 0.000(2) N3A 0.019(3) 0.017(3) 0.011(2) 0.001(2) 0.003(2) -0.004(2) C2A 0.014(3) 0.020(3) 0.014(3) 0.002(2) -0.001(2) 0.000(3) C4A 0.012(3) 0.021(3) 0.014(3) 0.004(2) 0.001(2) 0.007(3) C5A 0.019(3) 0.014(3) 0.015(3) 0.003(2) 0.009(3) 0.002(3) C6A 0.019(3) 0.018(3) 0.018(3) 0.004(3) 0.004(3) -0.004(3) C7A 0.018(3) 0.013(3) 0.017(3) 0.001(2) 0.004(3) 0.003(3) C8A 0.017(3) 0.014(3) 0.015(3) 0.001(2) 0.001(3) 0.005(3) C9A 0.017(3) 0.015(3) 0.027(4) -0.001(3) 0.006(3) 0.002(3) C10A 0.026(4) 0.018(3) 0.025(4) 0.007(3) 0.013(3) 0.005(3) C11A 0.023(4) 0.023(3) 0.017(3) 0.006(3) 0.003(3) 0.006(3) C12A 0.017(3) 0.019(3) 0.019(3) 0.004(3) 0.001(3) -0.001(3) C13A 0.018(3) 0.014(3) 0.017(3) 0.002(2) 0.004(3) 0.000(3) C14A 0.019(3) 0.023(4) 0.023(3) 0.001(3) 0.007(3) 0.002(3) C15A 0.031(4) 0.023(4) 0.020(3) -0.001(3) 0.012(3) 0.005(3) C16A 0.028(4) 0.020(3) 0.016(3) 0.002(3) 0.005(3) -0.003(3) C17A 0.021(4) 0.024(4) 0.017(3) 0.004(3) -0.001(3) -0.001(3) C18A 0.014(3) 0.023(4) 0.020(3) 0.003(3) 0.004(3) 0.005(3) N1 0.027(3) 0.026(3) 0.023(3) 0.001(2) 0.005(3) 0.004(3) O1 0.024(3) 0.025(3) 0.017(2) -0.0007(19) 0.0042(19) -0.002(2) O2 0.022(2) 0.027(3) 0.024(2) -0.001(2) 0.004(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3A 2.050(5) 2_756 ? Ni N3A 2.050(5) . ? Ni O1 2.108(4) 2_756 ? Ni O1 2.108(4) . ? Ni O2 2.129(5) 2_756 ? Ni O2 2.130(5) . ? N1A C2A 1.351(8) . ? N1A C5A 1.385(8) . ? N1A C6A 1.441(8) . ? N3A C2A 1.320(8) . ? N3A C4A 1.396(8) . ? C2A H2A 0.9300 . ? C4A C5A 1.382(9) . ? C4A C7A 1.470(9) . ? C5A C13A 1.476(8) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C12A 1.388(9) . ? C7A C8A 1.404(9) . ? C8A C9A 1.391(9) . ? C8A H8A 0.9300 . ? C9A C10A 1.391(9) . ? C9A H9A 0.9300 . ? C10A C11A 1.387(9) . ? C10A H10A 0.9300 . ? C11A C12A 1.386(9) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C18A 1.387(9) . ? C13A C14A 1.397(9) . ? C14A C15A 1.401(9) . ? C14A H14A 0.9300 . ? C15A C16A 1.383(10) . ? C15A H15A 0.9300 . ? C16A C17A 1.392(10) . ? C16A H16A 0.9300 . ? C17A C18A 1.391(9) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? N1 O1 1.262(7) . ? N1 O2 1.282(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 N3A Ni N3A 180.000(1) 2_756 . ? N3A Ni O1 87.96(18) 2_756 2_756 ? N3A Ni O1 92.04(18) . 2_756 ? N3A Ni O1 92.04(18) 2_756 . ? N3A Ni O1 87.96(18) . . ? O1 Ni O1 179.999(1) 2_756 . ? N3A Ni O2 90.30(19) 2_756 2_756 ? N3A Ni O2 89.70(19) . 2_756 ? O1 Ni O2 59.54(18) 2_756 2_756 ? O1 Ni O2 120.46(18) . 2_756 ? N3A Ni O2 89.70(19) 2_756 . ? N3A Ni O2 90.30(19) . . ? O1 Ni O2 120.46(18) 2_756 . ? O1 Ni O2 59.54(18) . . ? O2 Ni O2 179.999(2) 2_756 . ? C2A N1A C5A 107.4(5) . . ? C2A N1A C6A 124.6(5) . . ? C5A N1A C6A 128.0(5) . . ? C2A N3A C4A 105.9(5) . . ? C2A N3A Ni 116.9(4) . . ? C4A N3A Ni 136.9(4) . . ? N3A C2A N1A 111.9(5) . . ? N3A C2A H2A 124.1 . . ? N1A C2A H2A 124.1 . . ? C5A C4A N3A 108.8(5) . . ? C5A C4A C7A 128.4(5) . . ? N3A C4A C7A 122.7(5) . . ? C4A C5A N1A 106.0(5) . . ? C4A C5A C13A 131.1(5) . . ? N1A C5A C13A 123.0(5) . . ? N1A C6A H6A1 109.5 . . ? N1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? N1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C12A C7A C8A 118.7(6) . . ? C12A C7A C4A 120.3(6) . . ? C8A C7A C4A 120.9(5) . . ? C9A C8A C7A 120.3(6) . . ? C9A C8A H8A 119.8 . . ? C7A C8A H8A 119.8 . . ? C8A C9A C10A 120.3(6) . . ? C8A C9A H9A 119.8 . . ? C10A C9A H9A 119.8 . . ? C11A C10A C9A 119.2(6) . . ? C11A C10A H10A 120.4 . . ? C9A C10A H10A 120.4 . . ? C10A C11A C12A 120.7(6) . . ? C10A C11A H11A 119.6 . . ? C12A C11A H11A 119.6 . . ? C11A C12A C7A 120.7(6) . . ? C11A C12A H12A 119.7 . . ? C7A C12A H12A 119.7 . . ? C18A C13A C14A 119.7(6) . . ? C18A C13A C5A 120.7(6) . . ? C14A C13A C5A 119.5(6) . . ? C13A C14A C15A 119.8(6) . . ? C13A C14A H14A 120.1 . . ? C15A C14A H14A 120.1 . . ? C16A C15A C14A 120.1(6) . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C15A C16A C17A 120.1(6) . . ? C15A C16A H16A 120.0 . . ? C17A C16A H16A 120.0 . . ? C16A C17A C18A 120.1(6) . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C13A C18A C17A 120.3(6) . . ? C13A C18A H18A 119.9 . . ? C17A C18A H18A 119.9 . . ? O1 N1 O2 111.6(5) . . ? N1 O1 Ni 95.2(4) . . ? N1 O2 Ni 93.6(4) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 62.53 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.055 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.121 # start Validation Reply Form _vrf_PLAT029_13-Ni{NO2}2L2 ; RESPONSE: Several (needle-like) crystals of the title compound -from different preparations and at different periods of time- were carefully tested on the X-rays at 100 K. The diffraction quality of the crystals has proven to be moderate and structure determination was eventually carried out by means of the best data set collected (CuKa radiation). As a necessary compromise between resolution and data completeness we have used data up to theta=62.53 degrees with a completeness of 96.2%. The structure was refined as a non-merohedral twin (30:70) and the quality of the final analysis is certainly not as good as from an equivalent single crystal. Therefore, most of the present ALERTS are mainly due to the moderate quality of the difraction data and the twinning. ; _vrf_PLAT083_13-Ni{NO2}2L2 ; RESPONSE: See comment above. ; # end Validation Reply Form #===END