Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Paul K Bowyer' _publ_contact_author_address ; Dr Paul K Bowyer School of Wine & Food Sciences Charles Sturt University Locked Bag 588 Wagga Wagga NSW 2678 AUSTRALIA ; _publ_contact_author_email 'PBOWYER@CSU.EDU.AU' #--------------------------------------------------------------------------- loop_ _publ_author_name _publ_author_address ' A. David Rae ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; ' David StC. Black ' ; School of Chemistry, University of New South Wales, Sydney, N.S.W., 2052, Australia ; ' Paul V. Bowyer ' ; School of Wine and Food Services, Charles Sturt University, Locked Bag 588, Wagga Wagga, N.S.W., 2678, Australia ; 'Craig, Donald C.' ; ? ; _publ_section_title ; Indole-based mono- and polynuclear acyclic chelating systems: syntheses and selected transition metal complexes ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. Rae, A. D. (1996). RAELS96: A Comprehensive Constrained Least-Square Refinement Program. Australian National University, Canberra, A. C. T., Australia. Rae, A. D. (1975). Acta Crystallogr., Section A, A31, 560-570, 570-574. Wilson, A. J. C. (1995). Editor, International Tables for Crystallography, Vol. C, Kluwer Academic Publishers, Dordrecht, Tables 6.1.1.1, 4.2.6.8.and 4.2.4.3. Hall, S. R., King, G. S. D. & Stewart, J. M. (1995). Editors. Xtal3.4 Reference Manual. Univ. of Western Australia: Lamb, Perth, Australia. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_9a _database_code_CSD 159043 #--------------------------------------------------------------------------- _audit_creation_date '1999-12-13' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1997 data collected and structure solved in xtal/texsan 1999 solution improved with use of RAELS report and rough cif from adr to acw 2000-03-31 - Report and cif on pxb15 compiled by Anthony C. Willis 2000-04-03 - sent to checkcif. Reply gives anticipated alerts 2001-04-09 - response to referees' reports ; #--------------------------------------------------------------------------- #--------------------------------------------------------------------------- _computing_data_collection ; Philips PW1100/20 software 1976 ; _computing_cell_refinement xtal_LATCON _computing_data_reduction xtal_DIFDAT_ADDREF _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'RAELS96' _computing_publication_material 'teXsan (MSC, 1992-1997)' #--------------------------------------------------------------------------- _cell_length_a 12.952(12) _cell_length_b 14.602(12) _cell_length_c 15.286(13) _cell_angle_alpha 70.36(6) _cell_angle_beta 71.35(6) _cell_angle_gamma 85.15(7) _cell_volume 2579(4) _cell_formula_units_Z 1 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.64 _cell_measurement_theta_max 12.69 #--------------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #--------------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 2032.28 _chemical_formula_analytical ? _chemical_formula_sum 'C101 H109 Cl4 N15 Ni2 O15' _chemical_formula_moiety 'C80 H60 Cl4 N8 Ni2 O8, 7(C3 H7 N O) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1064.00 _exptl_absorpt_coefficient_mu 0.537 # units are mm-1 _exptl_absorpt_correction_type none _exptl_special_details ; crystal mounted in capillary ; #--------------------------------------------------------------------------- _diffrn_special_details ; The scan width was (1.0+0.34tan\q)\% with an \w scan speed of 3.0\% per minute. Stationary background counts were recorded for 5 sec at each end of each scan. ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Philips PW1100/20' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5 #loop_ #_diffrn_standard_refln_index_h #_diffrn_standard_refln_index_k #_diffrn_standard_refln_index_l _diffrn_reflns_number 9527 _reflns_number_total 9135 _reflns_number_gt 4299 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 101 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 109 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 15 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 2 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 15 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni1 0.2273(1) 0.3693(1) 0.3943(1) 1.0 0.054(0) . Uani d ? N1 0.3600(4) 0.4308(4) 0.2997(3) 1.0 0.053(1) . Uani d ? C1 0.4653(5) 0.4084(5) 0.2997(4) 1.0 0.055(1) . Uani d ? C2 0.5415(4) 0.4610(4) 0.2139(3) 1.0 0.054(1) . Uani d ? C3 0.4793(4) 0.5190(4) 0.1554(3) 1.0 0.053(1) . Uani d ? C4 0.3689(5) 0.5005(4) 0.2113(3) 1.0 0.051(1) . Uani d ? C5 0.5016(5) 0.5927(4) 0.0636(4) 1.0 0.060(1) . Uani d ? C6 0.4193(5) 0.6429(4) 0.0315(4) 1.0 0.063(1) . Uani d ? C7 0.3112(4) 0.6231(4) 0.0882(4) 1.0 0.057(1) . Uani d ? C8 0.2820(4) 0.5501(4) 0.1813(4) 1.0 0.051(1) . Uani d ? C9 0.1714(6) 0.5329(5) 0.2388(4) 1.0 0.050(1) . Uani d ? N2 0.1360(4) 0.4643(4) 0.3246(3) 1.0 0.051(1) . Uani d ? O1 0.6094(4) 0.6071(4) 0.0098(3) 1.0 0.068(2) . Uani d ? C10' 0.6521(13) 0.6704(16) -0.0901(6) 0.5 0.086(3) . Uani d ? C10" 0.6266(13) 0.6689(16) -0.0903(6) 0.5 0.085(3) . Uani d ? O2 0.2276(4) 0.6722(3) 0.0604(3) 1.0 0.061(1) . Uani d ? C11' 0.2426(14) 0.7556(13) -0.0266(7) 0.5 0.076(2) . Uani d ? C11" 0.2619(14) 0.7601(13) -0.0214(7) 0.5 0.076(2) . Uani d ? C12 0.6598(5) 0.4483(2) 0.1980(2) 1.0 0.058(1) . Uani d ? C13 0.7297(4) 0.4427(4) 0.1101(3) 1.0 0.067(1) . Uani d ? C14 0.8399(4) 0.4308(4) 0.0946(4) 1.0 0.074(2) . Uani d ? C15 0.8819(5) 0.4243(4) 0.1684(4) 1.0 0.074(1) . Uani d ? C16 0.8151(4) 0.4296(4) 0.2567(4) 1.0 0.080(1) . Uani d ? C17 0.7051(4) 0.4415(4) 0.2705(3) 1.0 0.070(1) . Uani d ? Cl1 1.0205(2) 0.4065(2) 0.1530(2) 1.0 0.091(2) . Uani d ? N3 -0.2092(5) 0.7686(3) 0.5739(3) 1.0 0.061(1) . Uani d ? C18 -0.2133(6) 0.8211(4) 0.6346(4) 1.0 0.064(1) . Uani d ? C19 -0.1945(4) 0.9196(4) 0.5850(3) 1.0 0.061(1) . Uani d ? C20 -0.1778(5) 0.9288(4) 0.4862(4) 1.0 0.067(1) . Uani d ? C21 -0.1857(4) 0.8350(4) 0.4820(4) 1.0 0.059(1) . Uani d ? C22 -0.1528(5) 1.0057(4) 0.3966(4) 1.0 0.100(2) . Uani d ? C23 -0.1371(6) 0.9889(4) 0.3103(4) 1.0 0.121(3) . Uani d ? C24 -0.1454(6) 0.8957(4) 0.3083(4) 1.0 0.097(2) . Uani d ? C25 -0.1704(5) 0.8145(4) 0.3954(4) 1.0 0.066(1) . Uani d ? C26 -0.1559(6) 0.7195(4) 0.3890(5) 1.0 0.060(1) . Uani d ? N4 -0.1720(4) 0.6395(3) 0.4653(4) 1.0 0.051(1) . Uani d ? O3 -0.1482(6) 1.0965(3) 0.4027(4) 1.0 0.125(3) . Uani d ? C27' -0.1285(29) 1.1827(12) 0.3174(15) 0.5 0.195(6) . Uani d ? C27" -0.0764(28) 1.1655(12) 0.3170(11) 0.5 0.185(6) . Uani d ? O4 -0.1298(6) 0.8748(4) 0.2254(3) 1.0 0.119(3) . Uani d ? C28' -0.0743(34) 0.9473(14) 0.1346(12) 0.5 0.181(6) . Uani d ? C28" -0.1092(33) 0.9524(14) 0.1335(15) 0.5 0.186(5) . Uani d ? C29 -0.1886(3) 0.9889(3) 0.6350(3) 1.0 0.069(1) . Uani d ? C30 -0.1126(5) 1.0651(4) 0.5913(4) 1.0 0.081(2) . Uani d ? C31 -0.1063(5) 1.1300(4) 0.6372(5) 1.0 0.093(2) . Uani d ? C32 -0.1774(4) 1.1190(4) 0.7290(4) 1.0 0.103(2) . Uani d ? C33 -0.2540(6) 1.0443(5) 0.7747(4) 1.0 0.125(3) . Uani d ? C34 -0.2587(5) 0.9803(4) 0.7274(4) 1.0 0.102(2) . Uani d ? Cl2 -0.1683(3) 1.1996(2) 0.7885(2) 1.0 0.138(2) . Uani d ? C35 0.0243(4) 0.4655(4) 0.3790(3) 1.0 0.051(1) . Uani d ? C36 -0.0234(4) 0.5517(4) 0.3874(4) 1.0 0.051(1) . Uani d ? C37 -0.1290(5) 0.5525(4) 0.4470(3) 1.0 0.051(1) . Uani d ? C38 -0.1889(4) 0.4644(4) 0.5000(3) 1.0 0.051(1) . Uani d ? C39 -0.1405(4) 0.3788(4) 0.4911(4) 1.0 0.051(1) . Uani d ? C40 -0.0352(5) 0.3772(4) 0.4318(4) 1.0 0.051(1) . Uani d ? O5 0.0104(9) 0.8253(7) -0.0787(7) 1.0 0.174(7) . Uani d ? N5 -0.1295(9) 0.7470(8) 0.0457(8) 1.0 0.150(6) . Uani d ? C51 -0.0940(13) 0.8042(10) -0.0349(10) 1.0 0.171(7) . Uani d ? C52 -0.0612(13) 0.6948(11) 0.1030(10) 1.0 0.167(5) . Uani d ? C53 -0.2348(13) 0.7138(13) 0.1001(14) 1.0 0.240(10) . Uani d ? O6 0.4476(27) 0.7345(23) 0.4916(16) 1.0 0.667(21) . Uani d ? N6 0.4805(11) 0.6962(11) 0.3572(10) 1.0 0.195(11) . Uani d ? C61 0.4370(18) 0.7463(13) 0.4060(16) 1.0 0.316(11) . Uani d ? C62 0.5306(24) 0.6172(21) 0.4140(22) 1.0 0.374(11) . Uani d ? C63 0.4434(18) 0.6969(17) 0.2820(15) 1.0 0.265(13) . Uani d ? O7 -0.4885(11) 0.1491(11) 0.1846(10) 1.0 0.260(13) . Uani d ? N7 -0.4614(14) 0.1056(13) 0.3286(13) 1.0 0.273(15) . Uani d ? C71 -0.4921(14) 0.1635(11) 0.2657(15) 1.0 0.245(17) . Uani d ? C72 -0.4307(26) 0.0226(18) 0.2961(27) 1.0 0.412(12) . Uani d ? C73 -0.4535(37) 0.1502(21) 0.3925(30) 1.0 0.573(31) . Uani d ? O8 0.5445(32) -0.1468(19) -0.0084(32) 0.5 0.310(12) . Uani d ? N8 0.5252(25) 0.0019(15) 0.0013(28) 0.5 0.205(10) . Uani d ? C81 0.5062(35) -0.0587(20) -0.0288(33) 0.5 0.243(9) . Uani d ? C82 0.5918(36) -0.0164(22) 0.0646(34) 0.5 0.275(16) . Uani d ? C83 0.4885(35) 0.0953(17) -0.0096(41) 0.5 0.241(8) . Uani d ? H1C1 0.4846 0.3594 0.3556 1.0 0.060 . Uani c ? H1C6 0.4375 0.6948 -0.0339 1.0 0.074 . Uani c ? H1C9 0.1162 0.5756 0.2127 1.0 0.051 . Uani c ? H1C10' 0.7335 0.6677 -0.1121 0.5 0.092 . Uani c ? H2C10' 0.6224 0.6488 -0.1330 0.5 0.091 . Uani c ? H3C10' 0.6300 0.7387 -0.0942 0.5 0.091 . Uani c ? H1C10" 0.7066 0.6769 -0.1261 0.5 0.094 . Uani c ? H2C10" 0.5901 0.6386 -0.1228 0.5 0.088 . Uani c ? H3C10" 0.5951 0.7341 -0.0913 0.5 0.089 . Uani c ? H1C11' 0.1698 0.7801 -0.0326 0.5 0.078 . Uani c ? H2C11' 0.2841 0.8080 -0.0227 0.5 0.083 . Uani c ? H3C11' 0.2842 0.7365 -0.0851 0.5 0.081 . Uani c ? H1C11" 0.1967 0.7930 -0.0384 0.5 0.081 . Uani c ? H2C11" 0.3006 0.8045 -0.0040 0.5 0.081 . Uani c ? H3C11" 0.3123 0.7437 -0.0788 0.5 0.081 . Uani c ? H1C13 0.6993 0.4474 0.0563 1.0 0.079 . Uani c ? H1C14 0.8888 0.4270 0.0304 1.0 0.089 . Uani c ? H1C16 0.8460 0.4248 0.3102 1.0 0.101 . Uani c ? H1C17 0.6566 0.4453 0.3348 1.0 0.083 . Uani c ? H1C18 -0.2281 0.7913 0.7068 1.0 0.080 . Uani c ? H1C23 -0.1194 1.0448 0.2478 1.0 0.166 . Uani c ? H1C26 -0.1320 0.7127 0.3225 1.0 0.067 . Uani c ? H1C27' -0.1281 1.2414 0.3371 0.5 0.215 . Uani c ? H2C27' -0.0563 1.1784 0.2694 0.5 0.215 . Uani c ? H3C27' -0.1873 1.1881 0.2868 0.5 0.222 . Uani c ? H1C27" -0.0779 1.2296 0.3277 0.5 0.211 . Uani c ? H2C27" -0.0004 1.1410 0.3047 0.5 0.185 . Uani c ? H3C27" -0.1011 1.1737 0.2592 0.5 0.219 . Uani c ? H1C28' -0.0680 0.9231 0.0792 0.5 0.201 . Uani c ? H2C28' -0.1165 1.0085 0.1269 0.5 0.214 . Uani c ? H3C28' 0.0002 0.9606 0.1346 0.5 0.190 . Uani c ? H1C28" -0.0996 0.9246 0.0800 0.5 0.203 . Uani c ? H2C28" -0.1722 0.9971 0.1361 0.5 0.212 . Uani c ? H3C28" -0.0414 0.9895 0.1206 0.5 0.207 . Uani c ? H1C30 -0.0608 1.0732 0.5246 1.0 0.105 . Uani c ? H1C31 -0.0507 1.1844 0.6042 1.0 0.118 . Uani c ? H1C33 -0.3055 1.0365 0.8415 1.0 0.180 . Uani c ? H1C34 -0.3145 0.9259 0.7608 1.0 0.134 . Uani c ? H1C36 0.0190 0.6144 0.3498 1.0 0.051 . Uani c ? H1C38 -0.2654 0.4639 0.5435 1.0 0.051 . Uani c ? H1C39 -0.1830 0.3162 0.5287 1.0 0.051 . Uani c ? H1C40 -0.0017 0.3143 0.4264 1.0 0.051 . Uani c ? H1C51 -0.1465 0.8374 -0.0707 1.0 0.272 . Uani c ? H1C52 0.0165 0.7164 0.0665 1.0 0.189 . Uani c ? H2C52 -0.0837 0.7081 0.1664 1.0 0.210 . Uani c ? H3C52 -0.0690 0.6234 0.1160 1.0 0.243 . Uani c ? H1C53 -0.2858 0.7482 0.0631 1.0 0.343 . Uani c ? H2C53 -0.2401 0.6422 0.1131 1.0 0.329 . Uani c ? H3C53 -0.2548 0.7269 0.1635 1.0 0.235 . Uani c ? H1C61 0.3903 0.7999 0.3801 1.0 0.377 . Uani c ? H1C62 0.5492 0.6376 0.4635 1.0 0.605 . Uani c ? H2C62 0.4789 0.5598 0.4481 1.0 0.436 . Uani c ? H3C62 0.5987 0.5991 0.3699 1.0 0.466 . Uani c ? H1C63 0.4125 0.7618 0.2561 1.0 0.338 . Uani c ? H2C63 0.5053 0.6844 0.2285 1.0 0.363 . Uani c ? H3C63 0.3856 0.6451 0.3067 1.0 0.411 . Uani c ? H1C71 -0.5219 0.2260 0.2756 1.0 0.497 . Uani c ? H1C72 -0.4617 0.0277 0.2426 1.0 0.388 . Uani c ? H2C72 -0.3494 0.0206 0.2710 1.0 0.731 . Uani c ? H3C72 -0.4595 -0.0382 0.3519 1.0 0.656 . Uani c ? H1C73 -0.4944 0.2121 0.3826 1.0 0.805 . Uani c ? H2C73 -0.4852 0.1060 0.4611 1.0 0.812 . Uani c ? H3C73 -0.3751 0.1648 0.3802 1.0 0.744 . Uani c ? H1C81 0.4585 -0.0410 -0.0719 0.5 0.309 . Uani c ? H1C82 0.6205 -0.0837 0.0748 0.5 0.268 . Uani c ? H2C82 0.6541 0.0319 0.0340 0.5 0.365 . Uani c ? H3C82 0.5469 -0.0101 0.1290 0.5 0.359 . Uani c ? H1C83 0.4415 0.1116 -0.0533 0.5 0.232 . Uani c ? H2C83 0.4450 0.1001 0.0557 0.5 0.313 . Uani c ? H3C83 0.5522 0.1421 -0.0393 0.5 0.319 . Uani c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.065(1) 0.036(1) 0.042(1) -0.009(0) 0.000(0) 0.000(0) N1 0.063(1) 0.051(2) 0.038(1) -0.011(1) -0.009(1) -0.008(1) C1 0.063(1) 0.051(2) 0.042(1) -0.011(1) -0.011(1) -0.007(1) C2 0.062(1) 0.050(2) 0.043(1) -0.010(1) -0.010(1) -0.010(1) C3 0.061(1) 0.050(2) 0.040(1) -0.011(1) -0.008(1) -0.009(1) C4 0.061(1) 0.047(2) 0.037(1) -0.011(1) -0.008(1) -0.009(1) C5 0.062(1) 0.061(2) 0.043(1) -0.014(1) -0.008(1) -0.003(1) C6 0.063(1) 0.063(2) 0.046(1) -0.017(1) -0.010(1) 0.003(1) C7 0.063(1) 0.052(2) 0.043(1) -0.014(1) -0.010(1) -0.002(1) C8 0.062(1) 0.046(2) 0.037(1) -0.011(1) -0.008(1) -0.009(1) C9 0.062(1) 0.047(2) 0.036(1) -0.010(1) -0.008(1) -0.011(1) N2 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) O1 0.062(1) 0.077(3) 0.046(2) -0.016(1) -0.007(1) 0.000(1) C10' 0.064(1) 0.108(4) 0.051(2) -0.022(1) -0.007(1) 0.012(2) C10" 0.064(1) 0.107(4) 0.050(2) -0.022(1) -0.007(1) 0.011(2) O2 0.064(1) 0.052(2) 0.050(2) -0.015(1) -0.013(1) 0.002(1) C11' 0.069(1) 0.065(2) 0.065(2) -0.021(1) -0.019(1) 0.016(2) C11" 0.069(1) 0.064(2) 0.068(3) -0.021(1) -0.020(1) 0.016(2) C12 0.062(1) 0.055(2) 0.050(1) -0.010(1) -0.011(1) -0.011(1) C13 0.062(1) 0.075(3) 0.060(1) -0.009(1) -0.009(1) -0.024(2) C14 0.062(1) 0.081(3) 0.073(2) -0.007(1) -0.010(1) -0.028(2) C15 0.063(1) 0.074(2) 0.074(2) -0.008(1) -0.015(1) -0.013(1) C16 0.066(1) 0.098(3) 0.064(2) -0.011(1) -0.019(1) -0.010(2) C17 0.065(1) 0.084(2) 0.054(2) -0.012(1) -0.015(1) -0.012(1) Cl1 0.064(1) 0.094(3) 0.096(2) -0.005(1) -0.019(1) -0.013(2) N3 0.082(3) 0.041(1) 0.044(2) -0.013(1) -0.006(1) -0.002(1) C18 0.085(3) 0.045(1) 0.045(2) -0.014(1) -0.005(1) -0.005(1) C19 0.076(3) 0.043(1) 0.052(1) -0.007(1) -0.010(1) -0.007(1) C20 0.100(3) 0.038(1) 0.052(1) -0.005(1) -0.019(2) -0.003(1) C21 0.079(3) 0.038(1) 0.046(1) -0.006(1) -0.012(1) -0.002(1) C22 0.190(5) 0.038(1) 0.059(1) -0.009(2) -0.038(2) 0.002(1) C23 0.251(7) 0.043(1) 0.056(1) -0.016(2) -0.048(3) 0.006(1) C24 0.183(5) 0.046(1) 0.050(1) -0.012(2) -0.035(2) 0.002(1) C25 0.097(3) 0.041(1) 0.047(1) -0.006(1) -0.017(2) -0.002(1) C26 0.077(2) 0.044(1) 0.047(2) -0.009(1) -0.009(1) -0.005(1) N4 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) O3 0.254(8) 0.037(1) 0.073(2) -0.012(2) -0.051(3) 0.000(1) C27' 0.444(14) 0.039(1) 0.090(3) -0.024(2) -0.089(5) 0.008(1) C27" 0.401(13) 0.047(1) 0.072(2) -0.062(3) -0.040(4) 0.009(1) O4 0.237(7) 0.058(1) 0.050(2) -0.019(3) -0.042(3) 0.001(1) C28' 0.395(12) 0.074(2) 0.047(2) -0.060(4) -0.044(3) 0.008(1) C28" 0.417(13) 0.070(2) 0.056(2) -0.035(4) -0.074(4) 0.007(1) C29 0.083(3) 0.051(1) 0.062(1) -0.010(1) -0.008(1) -0.016(1) C30 0.099(4) 0.055(1) 0.075(2) -0.020(1) -0.003(2) -0.023(1) C31 0.112(4) 0.067(2) 0.093(2) -0.023(2) -0.006(2) -0.036(2) C32 0.136(3) 0.079(2) 0.090(2) -0.027(1) -0.006(2) -0.042(2) C33 0.165(3) 0.098(2) 0.092(2) -0.051(2) 0.023(2) -0.055(2) C34 0.124(3) 0.082(2) 0.081(2) -0.037(2) 0.018(2) -0.042(2) Cl2 0.195(4) 0.105(2) 0.116(2) -0.043(2) -0.007(2) -0.066(2) C35 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) C36 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) C37 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) C38 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) C39 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) C40 0.057(2) 0.043(1) 0.045(1) -0.013(1) -0.009(1) -0.009(1) O5 0.212(9) 0.134(9) 0.138(8) -0.012(7) -0.038(6) -0.009(6) N5 0.189(9) 0.123(9) 0.153(7) -0.057(6) -0.066(6) -0.035(6) C51 0.209(9) 0.179(9) 0.133(7) -0.034(7) -0.075(6) -0.031(6) C52 0.196(9) 0.126(10) 0.144(7) -0.020(6) -0.041(6) -0.006(6) C53 0.196(11) 0.209(17) 0.273(13) -0.088(8) -0.068(7) -0.009(12) O6 0.974(60) 0.822(49) 0.358(19) -0.061(35) -0.181(21) -0.391(28) N6 0.220(14) 0.187(15) 0.200(14) -0.044(11) -0.046(11) -0.095(11) C61 0.430(18) 0.285(15) 0.260(14) -0.051(12) -0.031(13) -0.183(13) C62 0.288(21) 0.411(23) 0.293(20) 0.032(19) -0.059(17) 0.013(16) C63 0.307(14) 0.296(15) 0.253(17) -0.067(10) -0.094(11) -0.142(11) O7 0.213(26) 0.248(15) 0.234(21) -0.042(11) -0.037(22) 0.008(11) N7 0.344(27) 0.150(16) 0.369(21) 0.060(9) -0.213(22) -0.054(10) C71 0.265(31) 0.141(14) 0.341(23) 0.030(9) -0.164(25) -0.033(9) C72 0.528(34) 0.274(20) 0.657(36) 0.247(23) -0.448(34) -0.238(21) C73 1.079(74) 0.267(27) 0.697(45) 0.285(34) -0.696(55) -0.229(28) O8 0.347(36) 0.165(17) 0.402(52) -0.028(18) -0.003(29) -0.173(23) N8 0.198(26) 0.132(15) 0.221(21) -0.083(15) 0.083(14) -0.096(15) C81 0.268(20) 0.156(15) 0.273(20) -0.058(15) 0.040(14) -0.134(15) C82 0.289(32) 0.188(28) 0.327(32) -0.074(20) -0.016(24) -0.114(23) C83 0.241(21) 0.136(15) 0.297(23) -0.072(15) 0.050(15) -0.117(15) H1C1 0.066 0.057 0.047 -0.012 -0.014 -0.003 H1C6 0.065 0.077 0.052 -0.021 -0.012 0.012 H1C9 0.062 0.046 0.040 -0.010 -0.009 -0.011 H1C10' 0.064 0.122 0.054 -0.023 -0.007 0.012 H2C10' 0.064 0.131 0.044 -0.020 -0.004 0.006 H3C10' 0.067 0.099 0.066 -0.027 -0.014 0.025 H1C10" 0.065 0.126 0.053 -0.024 -0.006 0.014 H2C10" 0.064 0.127 0.042 -0.019 -0.004 0.003 H3C10" 0.067 0.097 0.063 -0.027 -0.013 0.023 H1C11' 0.070 0.064 0.072 -0.021 -0.022 0.018 H2C11' 0.072 0.060 0.088 -0.022 -0.027 0.019 H3C11' 0.068 0.087 0.054 -0.023 -0.014 0.020 H1C11" 0.071 0.065 0.077 -0.022 -0.024 0.020 H2C11" 0.072 0.057 0.090 -0.021 -0.027 0.016 H3C11" 0.068 0.084 0.057 -0.024 -0.015 0.021 H1C13 0.063 0.113 0.061 -0.010 -0.006 -0.039 H1C14 0.063 0.118 0.087 -0.006 -0.006 -0.049 H1C16 0.070 0.153 0.069 -0.014 -0.023 -0.015 H1C17 0.068 0.124 0.053 -0.014 -0.017 -0.022 H1C18 0.122 0.053 0.044 -0.024 -0.006 -0.005 H1C23 0.372 0.048 0.062 -0.028 -0.068 0.011 H1C26 0.089 0.051 0.049 -0.013 -0.008 -0.009 H1C27' 0.490 0.038 0.105 -0.026 -0.098 0.005 H2C27' 0.477 0.053 0.071 -0.082 -0.041 0.013 H3C27' 0.524 0.043 0.123 0.026 -0.160 -0.002 H1C27" 0.466 0.046 0.087 -0.065 -0.053 0.007 H2C27" 0.360 0.074 0.067 -0.110 0.018 -0.007 H3C27" 0.507 0.044 0.081 -0.046 -0.084 0.015 H1C28' 0.441 0.088 0.048 -0.067 -0.049 0.004 H2C28' 0.500 0.068 0.065 -0.031 -0.101 0.012 H3C28' 0.380 0.094 0.045 -0.110 0.012 -0.004 H1C28" 0.456 0.084 0.056 -0.044 -0.077 0.004 H2C28" 0.497 0.070 0.089 0.014 -0.145 -0.001 H3C28" 0.451 0.081 0.046 -0.088 -0.030 0.010 H1C30 0.133 0.068 0.088 -0.045 0.020 -0.033 H1C31 0.136 0.085 0.122 -0.045 0.009 -0.055 H1C33 0.246 0.142 0.117 -0.098 0.065 -0.088 H1C34 0.158 0.111 0.101 -0.068 0.051 -0.066 H1C36 0.057 0.043 0.045 -0.013 -0.009 -0.009 H1C38 0.057 0.043 0.045 -0.013 -0.009 -0.009 H1C39 0.057 0.043 0.045 -0.013 -0.009 -0.009 H1C40 0.057 0.043 0.045 -0.013 -0.009 -0.009 H1C51 0.246 0.372 0.169 -0.014 -0.108 -0.007 H1C52 0.189 0.180 0.156 -0.019 -0.055 0.007 H2C52 0.242 0.232 0.129 0.000 -0.065 -0.016 H3C52 0.263 0.110 0.234 -0.011 0.020 0.010 H1C53 0.205 0.412 0.353 -0.109 -0.121 0.010 H2C53 0.283 0.237 0.425 -0.164 -0.061 -0.062 H3C53 0.200 0.164 0.224 -0.014 -0.013 0.039 H1C61 0.446 0.198 0.359 -0.019 0.096 -0.133 H1C62 0.533 0.889 0.372 0.019 -0.271 -0.056 H2C62 0.322 0.325 0.363 0.080 0.079 0.068 H3C62 0.264 0.407 0.435 0.060 0.015 0.101 H1C63 0.296 0.416 0.274 -0.012 -0.110 -0.050 H2C63 0.506 0.374 0.253 -0.042 -0.057 -0.204 H3C63 0.415 0.438 0.500 -0.166 -0.164 -0.239 H1C71 0.834 0.236 0.723 0.275 -0.624 -0.237 H1C72 0.485 0.306 0.561 0.264 -0.364 -0.249 H2C72 0.555 0.904 1.157 0.585 -0.617 -0.671 H3C72 1.266 0.152 0.912 0.130 -0.919 -0.105 H1C73 1.526 0.489 0.979 0.606 -1.018 -0.511 H2C73 1.514 0.644 0.560 0.326 -0.675 -0.286 H3C73 1.296 0.192 1.214 0.168 -1.108 -0.176 H1C81 0.387 0.216 0.360 -0.031 -0.062 -0.183 H1C82 0.233 0.183 0.304 -0.085 0.034 -0.064 H2C82 0.340 0.193 0.559 -0.101 -0.130 -0.102 H3C82 0.474 0.312 0.336 0.014 -0.090 -0.195 H1C83 0.198 0.141 0.263 -0.081 0.086 -0.076 H2C83 0.386 0.213 0.329 0.006 0.010 -0.191 H3C83 0.280 0.136 0.494 -0.090 -0.031 -0.105 #--------------------------------------------------------------------------- _refine_special_details ; The dimer has a centre of inversion coincident with a crystallographic inversion centre of P-1. The reflection data quality was limited and only 4299 of the 9135 independent reflections collected had I > 3\s(I) and only these 4299 reflections were used in the refinement of 75 non Hydrogen atom positions in the unit cell. One half of the dimer shows distinctly more thermal motion than the other and the C atoms of the four methoxy groups were regarded as 1:1 disordered. There are 7 solvent molecules per unit cell, one of them disordered about 1/2,0,0 and all have large thermal motion. Refinement used the constrained refinement program RAELS96 (Rae, 1996) so as to allow anisotropic thermal parameters to be defined by rigid body parameterisations. This allowed just 270 independent variables to adequately refine the structure down to R(F) = 0.074 for the 4299 reflections with I > 3\s(I) used in the refinement The Ni atom was refined as an isolated anisotropic atom but the remaining atoms were described using local coordinates defined relative to orthonormal axial systems (Rae,1975). 9 axial systems were used, 5 for the ligand to define atoms [C1-C11, N1, O1-O2], [C12-C17, Cl1]. [C18-C28, N3, O3-O4], [C29-C34, Cl2], [N2,N4,C35-C40] and one for each of the 4 solvent molecules. The ligand has an inherent mirror symmetry and constraints were imposed by using the same refinable local coordinates for atoms [C3-C8] and [C20-C25], and these fragments were also constrained to be planar. The two phenyl groups [C12-C17] and [C29-C34] were constrained to have identical planar geometry with local 2mm symmetry relative to origins centred on C2 and C19 respectively. Atoms [C35-C40] were also constrained to be coplanar with local 2mm symmetry. Bond lengths not already constrained to be equal for the two halves of the ligand were restrained to approach equality. The N-C- O part of each solvent molecule was constrained to be equal with the remaining two sets of corresponding bond lengths restrained to approach equality. These molecules show a shortened bonds consistent with a disorder associated with the tetrahedral N atoms being above and below the plane of their coordinated atoms. Further complication of the model for the solvent molecules was not attempted. The four solvent molecules were each described by TLX rigid body parameterisations (Rae,1975). [N2,N4,C35-C40] was described by a T rigid body parameterisation. TLX models were also used for the fragments [C1-C17, N1, O1-O2, Cl1] and [C18-C34, N3, O3-O4, Cl2] with additional L models (libration only) for the fragments [C12-C17, Cl1] and [C29-C34, Cl2] centred on C2 and C19 respectively. The separation of C10 into C10prime and C10doubleprime, likewise C11, C27, C28, was obtained by describing their thermal motion using the relevant TLX model and refining the positional parameters with restraints to have bonds to the same O approach equality. Hydrogen atoms were recalculated to be in chemically sensible positions after each refinement cycle and asssigned thermal parameters by the rigid body parameters of the relevant fragments they were associated with. Errors quoted for the atom parameters are conditional on the appropriateness of the various constraints and restraints used. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + (0.05Fo)^2^] ' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4299 _refine_ls_number_parameters 270 _refine_ls_number_restraints 21 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.152 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_all 0.121 _refine_ls_wR_factor_ref 0.101 _refine_ls_goodness_of_fit_all 1.296 _refine_ls_goodness_of_fit_ref 1.530 _refine_ls_shift/su_max 0.3 _refine_ls_shift/su_mean 0.1 _refine_diff_density_min -0.30 _refine_diff_density_max 0.26 #--------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.910(5) . . yes Ni1 N2 1.998(5) . . yes Ni1 N3 1.922(5) . 2_566 yes Ni1 N4 1.996(5) . 2_566 yes N1 C1 1.376(6) . . yes N1 C4 1.367(6) . . yes C1 C2 1.381(6) . . yes C2 C3 1.414(6) . . yes C2 C12 1.479(7) . . yes C3 C4 1.406(6) . . yes C3 C5 1.410(6) . . yes C4 C8 1.403(7) . . yes C5 C6 1.370(7) . . yes C5 O1 1.367(6) . . yes C6 C7 1.385(7) . . yes C7 C8 1.418(6) . . yes C7 O2 1.352(6) . . yes C8 C9 1.412(8) . . yes C9 N2 1.320(6) . . yes N2 C35 1.422(6) . . yes O1 C10' 1.446(8) . . yes O1 C10" 1.448(8) . . yes O2 C11' 1.441(9) . . yes O2 C11" 1.439(10) . . yes C12 C13 1.384(4) . . yes C12 C17 1.384(4) . . yes C13 C14 1.376(6) . . yes C14 C15 1.374(5) . . yes C15 C16 1.374(5) . . yes C15 Cl1 1.743(6) . . yes C16 C17 1.376(6) . . yes N3 C18 1.376(7) . . yes N3 C21 1.367(6) . . yes C18 C19 1.382(6) . . yes C19 C20 1.415(7) . . yes C19 C29 1.479(7) . . yes C20 C21 1.406(6) . . yes C20 C22 1.410(6) . . yes C21 C25 1.403(7) . . yes C22 C23 1.370(7) . . yes C22 O3 1.367(7) . . yes C23 C24 1.385(7) . . yes C24 C25 1.418(6) . . yes C24 O4 1.351(7) . . yes C25 C26 1.416(8) . . yes C26 N4 1.318(6) . . yes N4 C37 1.422(6) . . yes O3 C27' 1.445(13) . . yes O3 C27" 1.446(14) . . yes O4 C28' 1.438(15) . . yes O4 C28" 1.439(12) . . yes C29 C30 1.384(4) . . yes C29 C34 1.384(4) . . yes C30 C31 1.376(6) . . yes C31 C32 1.374(5) . . yes C32 C33 1.374(5) . . yes C32 Cl2 1.744(7) . . yes C33 C34 1.376(6) . . yes C35 C36 1.382(5) . . yes C35 C40 1.406(6) . . yes C36 C37 1.382(5) . . yes C37 C38 1.406(6) . . yes C38 C39 1.379(5) . . yes C39 C40 1.379(5) . . yes O5 C51 1.312(14) . . no N5 C51 1.199(12) . . no N5 C52 1.437(14) . . no N5 C53 1.379(14) . . no O6 C61 1.312(14) . . no N6 C61 1.199(12) . . no N6 C62 1.438(16) . . no N6 C63 1.377(15) . . no O7 C71 1.312(14) . . no N7 C71 1.199(12) . . no N7 C72 1.439(16) . . no N7 C73 1.375(17) . . no O8 C81 1.311(14) . . no N8 C81 1.200(12) . . no N8 C82 1.438(16) . . no N8 C83 1.380(17) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 92.5(2) . . . yes N1 Ni1 N3 118.0(2) . . 2_566 yes N1 Ni1 N4 127.1(2) . . 2_566 yes N2 Ni1 N3 121.7(2) . . 2_566 yes N2 Ni1 N4 107.6(2) . . 2_566 yes N3 Ni1 N4 92.3(2) 2_566 . 2_566 yes Ni1 N1 C1 128.4(4) . . . yes Ni1 N1 C4 125.7(4) . . . yes C1 N1 C4 105.5(5) . . . yes N1 C1 C2 112.5(5) . . . yes C1 C2 C3 104.8(5) . . . yes C1 C2 C12 121.6(4) . . . yes C3 C2 C12 133.6(3) . . . yes C2 C3 C4 107.2(4) . . . yes C2 C3 C5 136.0(5) . . . yes C4 C3 C5 116.5(5) . . . yes N1 C4 C3 110.0(5) . . . yes N1 C4 C8 125.7(5) . . . yes C3 C4 C8 124.3(4) . . . yes C3 C5 C6 121.1(5) . . . yes C3 C5 O1 115.1(5) . . . yes C6 C5 O1 123.7(5) . . . yes C5 C6 C7 121.1(5) . . . yes C6 C7 C8 121.2(5) . . . yes C6 C7 O2 123.1(5) . . . yes C8 C7 O2 115.7(5) . . . yes C4 C8 C7 115.8(4) . . . yes C4 C8 C9 124.0(5) . . . yes C7 C8 C9 120.1(5) . . . yes C8 C9 N2 124.5(6) . . . yes Ni1 N2 C9 126.5(4) . . . yes Ni1 N2 C35 115.8(3) . . . yes C9 N2 C35 117.2(5) . . . yes C5 O1 C10' 125.6(8) . . . yes C5 O1 C10" 112.9(8) . . . yes C7 O2 C11' 123.2(8) . . . yes C7 O2 C11" 113.2(8) . . . yes C2 C12 C13 121.4(3) . . . yes C2 C12 C17 121.3(3) . . . yes C13 C12 C17 117.3(5) . . . yes C12 C13 C14 121.9(4) . . . yes C13 C14 C15 119.2(4) . . . yes C14 C15 C16 120.7(6) . . . yes C14 C15 Cl1 120.8(4) . . . yes C16 C15 Cl1 118.5(4) . . . yes C15 C16 C17 119.2(4) . . . yes C12 C17 C16 121.9(4) . . . yes Ni1 N3 C18 129.1(4) 2_566 . . yes Ni1 N3 C21 125.3(4) 2_566 . . yes C18 N3 C21 105.6(5) . . . yes N3 C18 C19 112.6(5) . . . yes C18 C19 C20 104.4(5) . . . yes C18 C19 C29 121.8(4) . . . yes C20 C19 C29 133.7(3) . . . yes C19 C20 C21 107.6(4) . . . yes C19 C20 C22 135.8(5) . . . yes C21 C20 C22 116.5(5) . . . yes N3 C21 C20 109.6(5) . . . yes N3 C21 C25 126.1(5) . . . yes C20 C21 C25 124.3(4) . . . yes C20 C22 C23 121.1(5) . . . yes C20 C22 O3 115.5(6) . . . yes C23 C22 O3 123.3(5) . . . yes C22 C23 C24 121.1(5) . . . yes C23 C24 C25 121.2(5) . . . yes C23 C24 O4 123.6(5) . . . yes C25 C24 O4 115.2(5) . . . yes C21 C25 C24 115.8(4) . . . yes C21 C25 C26 123.5(5) . . . yes C24 C25 C26 119.3(5) . . . yes C25 C26 N4 124.0(6) . . . yes Ni1 N4 C26 126.7(4) 2_566 . . yes Ni1 N4 C37 115.5(3) 2_566 . . yes C26 N4 C37 116.9(5) . . . yes C22 O3 C27' 121.7(11) . . . yes C22 O3 C27" 114.8(10) . . . yes C24 O4 C28' 117.3(12) . . . yes C24 O4 C28" 119.7(12) . . . yes C19 C29 C30 121.4(3) . . . yes C19 C29 C34 121.3(3) . . . yes C30 C29 C34 117.3(5) . . . yes C29 C30 C31 121.9(4) . . . yes C30 C31 C32 119.2(4) . . . yes C31 C32 C33 120.7(6) . . . yes C31 C32 Cl2 119.4(4) . . . yes C33 C32 Cl2 119.9(4) . . . yes C32 C33 C34 119.2(4) . . . yes C29 C34 C33 121.9(4) . . . yes C10' C35 C36 102.4(4) . . . yes C10' C35 C40 137.5(4) . . . yes C36 C35 C40 119.7(5) . . . yes C35 C36 C37 120.9(6) . . . yes N4 C37 C36 120.2(5) . . . yes N4 C37 C38 119.6(5) . . . yes C36 C37 C38 119.7(5) . . . yes C37 C38 C39 118.9(5) . . . yes C38 C39 C40 121.9(6) . . . yes C35 C40 C39 118.9(5) . . . yes C51 N5 C52 122.8(13) . . . yes C51 N5 C53 130.8(17) . . . yes C52 N5 C53 106.4(14) . . . yes O5 C51 N5 123.3(14) . . . yes C61 N6 C62 108.4(19) . . . yes C61 N6 C63 118.8(20) . . . yes C62 N6 C63 127.2(21) . . . yes O6 C61 N6 123.3(14) . . . yes C71 N7 C72 104.9(17) . . . yes C71 N7 C73 108.8(22) . . . yes C72 N7 C73 145.0(22) . . . yes O7 C71 N7 123.3(14) . . . yes C81 N8 C82 122.6(13) . . . yes C81 N8 C83 130.8(17) . . . yes C82 N8 C83 106.5(14) . . . yes O8 C81 N8 123.5(14) . . . yes #--------------------------------------------------------------------------- #===END data_6a _database_code_CSD 159044 _audit_creation_method 'RAELSPUB and manual entry' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C46 H34 Cl2 N4 Ni O4, C H Cl3' _chemical_formula_sum 'C47 H35 Cl5 N4 Ni O4' _chemical_formula_iupac ? _chemical_formula_weight 955.8 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 13.342(3) _cell_length_b 20.470(5) _cell_length_c 20.763(5) _cell_angle_alpha 90 _cell_angle_beta 128.417(8) _cell_angle_gamma 90 _cell_volume 4443(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 20 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.43 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960.0 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T-min ? _exptl_absorpt_correction_T-max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5973 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 23 _diffrn_reflns_h_min -14 _diffrn_reflns_h_max 14 _diffrn_reflns_k_min -22 _diffrn_reflns_k_max 0 _diffrn_reflns_l_min 0 _diffrn_reflns_l_max 22 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ;The chlorophenyl groups were maintained identical and planar with refineable mm2 symmetry. The chloroform solvate was disordered, and was modelled as two identical refineable rigid groups with 3-fold symmetry about the C-H bond, and occupancies constrained to total 1.0. ; _reflns_number_total 5784 _reflns_number_gt 3641 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_ref 0.101 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3641 _refine_ls_number_parameters 467 _refine_ls_goodness_of_fit_ref 1.79 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0016F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 1.26 _refine_diff_density_min -0.87 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Ni 0.79409(9) 0.19229(5) 0.44691(6) 0.0423(4) Uani Ni ? Cl1 0.0638(2) 0.4732(1) 0.2768(1) 0.067(2) Uani Cl ? Cl2 0.0817(3) -0.0501(2) -0.0337(2) 0.120(3) Uani Cl ? O1 0.4366(5) 0.2640(3) 0.5499(3) 0.054(2) Uani O ? O2 0.8192(6) 0.1330(4) 0.7147(4) 0.078(2) Uani O ? O3 0.6084(5) 0.0830(3) 0.0953(3) 0.048(1) Uani O ? O4 0.9902(5) 0.2102(3) 0.2773(3) 0.056(2) Uani O ? N1 0.6719(6) 0.2289(3) 0.4576(4) 0.042(2) Uani N ? N2 0.8878(6) 0.1449(3) 0.5526(4) 0.041(2) Uani N ? N3 0.7058(6) 0.1558(3) 0.3390(4) 0.041(2) Uani N ? N4 0.9415(6) 0.2183(3) 0.4512(4) 0.039(2) Uani N ? C1 0.5688(7) 0.2696(4) 0.4048(5) 0.044(2) Uani C ? C2 0.4975(7) 0.2815(4) 0.4304(4) 0.038(2) Uani C ? C3 0.5590(7) 0.2457(4) 0.5058(5) 0.039(2) Uani C ? C4 0.5395(7) 0.2351(4) 0.5642(5) 0.041(2) Uani C ? C5 0.6250(9) 0.1976(4) 0.6340(5) 0.054(2) Uani C ? C6 0.7303(8) 0.1689(4) 0.6458(5) 0.054(2) Uani C ? C7 0.7515(7) 0.1752(4) 0.5877(5) 0.038(2) Uani C ? C8 0.6665(7) 0.2144(4) 0.5197(5) 0.038(2) Uani C ? C9 0.3829(5) 0.3254(2) 0.3846(3) 0.040(2) Uani C ? C10 0.3890(4) 0.3856(3) 0.3561(3) 0.045(1) Uani C ? C11 0.2916(5) 0.4310(3) 0.3231(3) 0.050(2) Uani C ? C12 0.1866(4) 0.4163(2) 0.3183(2) 0.052(2) Uani C ? C13 0.1772(5) 0.3573(2) 0.3458(3) 0.056(1) Uani C ? C14 0.2752(5) 0.3123(2) 0.3788(3) 0.049(2) Uani C ? C15 0.4062(9) 0.2495(5) 0.6033(6) 0.068(3) Uani C ? C16 0.7995(11) 0.1202(6) 0.7717(6) 0.089(4) Uani C ? C17 0.8572(7) 0.1408(4) 0.6018(5) 0.043(2) Uani C ? C18 0.9949(8) 0.1040(4) 0.5764(5) 0.045(2) Uani C ? C19 0.9840(9) 0.0377(4) 0.5807(5) 0.052(2) Uani C ? C20 1.0854(10) -0.0030(4) 0.6042(6) 0.063(3) Uani C ? C21 1.1937(10) 0.0243(6) 0.6214(6) 0.070(3) Uani C ? C22 1.2045(8) 0.0917(5) 0.6174(5) 0.052(2) Uani C ? C23 1.1051(7) 0.1327(4) 0.5952(4) 0.043(2) Uani C ? C24 0.5932(8) 0.1206(4) 0.2932(5) 0.047(2) Uani C ? C25 0.5587(7) 0.0997(4) 0.2189(5) 0.041(2) Uani C ? C26 0.6590(7) 0.1250(4) 0.2179(4) 0.036(2) Uani C ? C27 0.6903(7) 0.1184(4) 0.1643(5) 0.043(2) Uani C ? C28 0.7993(7) 0.1483(4) 0.1837(5) 0.041(2) Uani C ? C29 0.8833(7) 0.1813(4) 0.2573(5) 0.042(2) Uani C ? C30 0.8613(7) 0.1871(4) 0.3154(4) 0.038(2) Uani C ? C31 0.7471(7) 0.1586(4) 0.2930(4) 0.037(2) Uani C ? C32 0.4425(5) 0.0625(2) 0.1564(3) 0.042(2) Uani C ? C33 0.4056(5) 0.0089(3) 0.1784(3) 0.062(2) Uani C ? C34 0.2953(5) -0.0258(3) 0.1205(3) 0.079(2) Uani C ? C35 0.2206(5) -0.0067(2) 0.0395(3) 0.065(2) Uani C ? C36 0.2539(5) 0.0461(3) 0.0154(3) 0.053(2) Uani C ? C37 0.3645(5) 0.0803(3) 0.0739(3) 0.047(1) Uani C ? C38 0.6459(8) 0.0679(4) 0.0462(5) 0.048(2) Uani C ? C39 1.0213(9) 0.2040(5) 0.2229(6) 0.071(3) Uani C ? C40 0.9534(7) 0.2137(4) 0.3932(5) 0.039(2) Uani C ? C41 1.0468(6) 0.2457(4) 0.5286(4) 0.034(2) Uani C ? C42 1.0733(8) 0.3116(4) 0.5374(5) 0.045(2) Uani C ? C43 1.1692(8) 0.3394(4) 0.6106(6) 0.049(2) Uani C ? C44 1.2462(8) 0.2991(5) 0.6796(5) 0.055(2) Uani C ? C45 1.2228(7) 0.2324(5) 0.6729(5) 0.049(2) Uani C ? C46 1.1229(7) 0.2042(4) 0.5979(5) 0.041(2) Uani C ? C1Ch 0.2765(14) 0.0735(8) 0.3809(11) 0.335(7) Uani C 0.57 Cl1Ch 0.2446(25) 0.1100(9) 0.4380(20) 0.362(6) Uani Cl 0.57 Cl2Ch 0.4067(23) 0.1068(7) 0.4003(19) 0.439(9) Uani Cl 0.57 Cl3Ch 0.3020(22) -0.0058(7) 0.4037(18) 0.395(9) Uani Cl 0.57 C1Ch' 0.3449(21) 0.0840(8) 0.4441(16) 0.323(8) Uani C 0.43 Cl1Ch' 0.2106(38) 0.1197(17) 0.4155(24) 0.404(7) Uani Cl 0.43 Cl3Ch' 0.3865(23) 0.0256(13) 0.5126(15) 0.378(9) Uani Cl 0.43 Cl2Ch' 0.3212(21) 0.0512(11) 0.3622(16) 0.343(9) Uani Cl 0.43 HC1 0.5485 0.2884 0.3534 0.044 Uani H ? HC5 0.6111 0.1912 0.6757 0.054 Uani H ? HC10 0.4653 0.3963 0.3596 0.052 Uani H ? HC11 0.2976 0.4741 0.3029 0.060 Uani H ? HC13 0.1005 0.3470 0.3421 0.072 Uani H ? HC14 0.2685 0.2693 0.3988 0.058 Uani H ? H1C15 0.3281 0.2743 0.5851 0.068 Uani H ? H2C15 0.3899 0.2016 0.6014 0.068 Uani H ? H3C15 0.4795 0.2624 0.6608 0.068 Uani H ? H1C16 0.8724 0.0938 0.8179 0.089 Uani H ? H2C16 0.7941 0.1624 0.7937 0.089 Uani H ? H3C16 0.7179 0.0954 0.7447 0.089 Uani H ? HC17 0.9103 0.1123 0.6515 0.043 Uani H ? HC19 0.9038 0.0187 0.5671 0.052 Uani H ? HC20 1.0795 -0.0513 0.6086 0.063 Uani H ? HC21 1.2661 -0.0046 0.6370 0.070 Uani H ? HC22 1.2845 0.1106 0.6306 0.052 Uani H ? HC24 0.5417 0.1113 0.3121 0.047 Uani H ? HC28 0.8177 0.1459 0.1438 0.041 Uani H ? HC33 0.4599 -0.0050 0.2373 0.079 Uani H ? HC34 0.2702 -0.0643 0.1374 0.113 Uani H ? HC36 0.1990 0.0596 -0.0436 0.064 Uani H ? HC37 0.3888 0.1187 0.0565 0.058 Uani H ? H1C38 0.5771 0.0417 -0.0026 0.048 Uani H ? H2C38 0.6599 0.1093 0.0272 0.048 Uani H ? H3C38 0.7270 0.0420 0.0794 0.048 Uani H ? H1C39 1.1027 0.2279 0.2463 0.071 Uani H ? H2C39 1.0323 0.1568 0.2163 0.071 Uani H ? H3C39 0.9507 0.2229 0.1681 0.071 Uani H ? HC40 1.0341 0.2306 0.4056 0.039 Uani H ? HC42 1.0199 0.3403 0.4878 0.045 Uani H ? HC43 1.1843 0.3876 0.6150 0.049 Uani H ? HC44 1.3182 0.3183 0.7337 0.055 Uani H ? HC45 1.2784 0.2041 0.7226 0.049 Uani H ? H1Ch 0.2024 0.0791 0.3214 0.436 Uani H 0.57 H1Ch' 0.4147 0.1173 0.4694 0.436 Uani H 0.43 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Ni 0.0402(6) 0.0632(7) 0.0322(6) 0.0083(5) 0.0269(5) 0.0035(5) Ni Cl1 0.050(1) 0.067(2) 0.054(1) 0.016(1) 0.018(1) -0.007(1) Cl Cl2 0.115(3) 0.159(3) 0.111(3) -0.094(2) 0.082(2) -0.063(2) Cl O1 0.057(4) 0.068(4) 0.062(4) 0.010(3) 0.049(3) 0.006(3) O O2 0.079(4) 0.118(6) 0.065(4) 0.042(4) 0.059(4) 0.049(4) O O3 0.050(3) 0.060(4) 0.040(3) -0.004(3) 0.031(3) -0.011(3) O O4 0.058(4) 0.080(4) 0.051(4) -0.019(3) 0.044(3) -0.017(3) O N1 0.043(4) 0.057(4) 0.034(4) 0.003(3) 0.028(3) 0.000(3) N N2 0.039(4) 0.048(4) 0.042(4) 0.008(3) 0.028(3) 0.002(3) N N3 0.044(4) 0.056(4) 0.037(4) 0.005(3) 0.032(4) 0.006(3) N N4 0.041(4) 0.044(4) 0.034(4) 0.009(3) 0.025(3) 0.006(3) N C1 0.044(5) 0.053(5) 0.035(5) 0.004(4) 0.025(4) 0.002(4) C C2 0.030(4) 0.052(5) 0.031(4) 0.000(4) 0.018(4) -0.008(4) C C3 0.043(5) 0.045(5) 0.038(5) -0.006(4) 0.030(4) -0.009(4) C C4 0.042(5) 0.045(5) 0.050(5) -0.004(4) 0.034(4) -0.009(4) C C5 0.068(6) 0.064(6) 0.061(6) 0.008(5) 0.055(5) 0.008(5) C C6 0.057(6) 0.066(6) 0.055(6) 0.011(5) 0.043(5) 0.019(5) C C7 0.044(5) 0.044(5) 0.041(5) 0.002(4) 0.033(4) 0.004(4) C C8 0.037(4) 0.049(5) 0.039(5) -0.004(4) 0.029(4) -0.001(4) C C9 0.041(2) 0.047(3) 0.030(3) 0.000(2) 0.022(2) -0.008(2) C C10 0.047(2) 0.049(3) 0.038(3) 0.003(2) 0.026(2) -0.003(2) C C11 0.051(3) 0.051(3) 0.043(3) 0.006(2) 0.026(3) -0.002(2) C C12 0.047(3) 0.056(3) 0.046(4) 0.007(3) 0.025(3) -0.006(3) C C13 0.046(2) 0.061(4) 0.061(4) 0.006(2) 0.033(2) -0.002(3) C C14 0.043(2) 0.054(2) 0.050(3) 0.002(2) 0.030(2) -0.004(2) C C15 0.076(7) 0.076(7) 0.095(8) 0.002(6) 0.075(7) 0.007(6) C C16 0.113(9) 0.116(9) 0.069(7) 0.014(8) 0.071(7) 0.026(7) C C17 0.046(5) 0.052(5) 0.040(5) 0.004(4) 0.032(4) 0.008(4) C C18 0.051(5) 0.051(6) 0.039(5) 0.010(4) 0.032(4) 0.002(4) C C19 0.074(7) 0.047(6) 0.050(5) 0.001(5) 0.045(5) -0.002(4) C C20 0.077(7) 0.052(6) 0.058(6) 0.023(6) 0.040(6) 0.015(5) C C21 0.069(7) 0.080(8) 0.058(6) 0.034(6) 0.038(6) 0.010(6) C C22 0.046(5) 0.060(6) 0.051(5) 0.022(5) 0.031(5) 0.011(5) C C23 0.043(5) 0.060(6) 0.029(4) 0.013(4) 0.024(4) 0.006(4) C C24 0.048(5) 0.060(5) 0.043(5) -0.001(4) 0.033(4) 0.003(4) C C25 0.050(5) 0.041(5) 0.044(5) -0.001(4) 0.035(4) 0.001(4) C C26 0.043(5) 0.043(5) 0.031(4) 0.007(4) 0.027(4) 0.005(4) C C27 0.047(5) 0.048(5) 0.041(5) 0.010(4) 0.031(5) 0.007(4) C C28 0.047(5) 0.055(5) 0.035(5) -0.007(4) 0.032(4) -0.005(4) C C29 0.046(5) 0.047(5) 0.046(5) -0.004(4) 0.034(4) 0.000(4) C C30 0.041(4) 0.048(5) 0.033(4) 0.001(4) 0.026(4) 0.003(4) C C31 0.040(5) 0.047(5) 0.032(4) 0.009(4) 0.026(4) 0.000(4) C C32 0.049(3) 0.044(3) 0.049(2) -0.002(2) 0.038(2) -0.002(2) C C33 0.073(3) 0.064(4) 0.056(2) -0.024(3) 0.044(2) -0.004(2) C C34 0.088(4) 0.089(4) 0.065(3) -0.044(4) 0.050(3) -0.013(3) C C35 0.064(3) 0.084(5) 0.062(3) -0.025(3) 0.046(2) -0.019(3) C C36 0.050(3) 0.068(4) 0.052(2) -0.004(2) 0.037(2) -0.009(2) C C37 0.050(3) 0.052(3) 0.049(3) 0.000(2) 0.036(2) -0.002(2) C C38 0.056(5) 0.064(6) 0.037(5) -0.001(5) 0.036(5) -0.012(4) C C39 0.074(7) 0.101(8) 0.079(7) -0.029(6) 0.067(6) -0.024(6) C C40 0.044(5) 0.042(5) 0.041(5) 0.010(4) 0.031(4) 0.007(4) C C41 0.031(4) 0.047(5) 0.031(4) 0.006(4) 0.023(4) 0.003(4) C C42 0.053(5) 0.051(6) 0.046(5) 0.003(4) 0.040(5) 0.004(4) C C43 0.051(5) 0.058(6) 0.050(5) -0.003(5) 0.038(5) -0.010(5) C C44 0.041(5) 0.074(7) 0.051(6) -0.013(5) 0.030(5) -0.021(5) C C45 0.042(5) 0.070(7) 0.037(5) 0.006(5) 0.026(5) 0.004(5) C C46 0.036(4) 0.052(6) 0.043(5) 0.003(4) 0.030(4) -0.004(4) C C1Ch 0.301(9) 0.237(9) 0.537(9) -0.038(9) 0.295(9) -0.024(9) C Cl1Ch 0.373(9) 0.238(9) 0.570(9) -0.003(8) 0.340(9) -0.006(9) Cl Cl2Ch 0.475(9) 0.295(9) 0.743(9) -0.134(9) 0.475(9) -0.049(9) Cl Cl3Ch 0.454(9) 0.195(9) 0.662(9) -0.114(9) 0.409(9) -0.096(9) Cl C1Ch' 0.302(9) 0.184(9) 0.557(9) -0.096(9) 0.304(9) -0.060(9) C Cl1Ch' 0.427(9) 0.310(9) 0.589(9) 0.063(9) 0.372(9) 0.036(9) Cl Cl3Ch' 0.371(9) 0.294(9) 0.570(9) 0.026(9) 0.343(9) 0.022(9) Cl Cl2Ch' 0.301(9) 0.259(9) 0.534(9) -0.031(9) 0.293(9) -0.025(9) Cl # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N1 1.928(6) 1_555 1_555 no Ni N2 1.977(6) 1_555 1_555 no Ni N3 1.920(6) 1_555 1_555 no Ni N4 1.985(6) 1_555 1_555 no Cl1 C12 1.741(6) 1_555 1_555 no Cl2 C35 1.741(6) 1_555 1_555 no O1 C4 1.348(8) 1_555 1_555 no O1 C15 1.428(9) 1_555 1_555 no O2 C6 1.372(10) 1_555 1_555 no O2 C16 1.387(10) 1_555 1_555 no O3 C27 1.351(9) 1_555 1_555 no O3 C38 1.422(8) 1_555 1_555 no O4 C29 1.350(8) 1_555 1_555 no O4 C39 1.430(9) 1_555 1_555 no N1 C1 1.384(9) 1_555 1_555 no N1 C8 1.368(9) 1_555 1_555 no N2 C17 1.318(9) 1_555 1_555 no N2 C18 1.452(9) 1_555 1_555 no N3 C24 1.381(10) 1_555 1_555 no N3 C31 1.368(8) 1_555 1_555 no N4 C40 1.313(9) 1_555 1_555 no N4 C41 1.436(9) 1_555 1_555 no C1 C2 1.368(10) 1_555 1_555 no C2 C3 1.437(10) 1_555 1_555 no C2 C9 1.497(9) 1_555 1_555 no C3 C4 1.407(10) 1_555 1_555 no C3 C8 1.427(10) 1_555 1_555 no C4 C5 1.392(11) 1_555 1_555 no C5 C6 1.397(11) 1_555 1_555 no C6 C7 1.407(10) 1_555 1_555 no C7 C8 1.390(10) 1_555 1_555 no C7 C17 1.434(10) 1_555 1_555 no C9 C10 1.391(5) 1_555 1_555 no C9 C14 1.391(5) 1_555 1_555 no C10 C11 1.384(6) 1_555 1_555 no C11 C12 1.376(5) 1_555 1_555 no C12 C13 1.376(5) 1_555 1_555 no C13 C14 1.384(6) 1_555 1_555 no C18 C19 1.375(11) 1_555 1_555 no C18 C23 1.395(10) 1_555 1_555 no C19 C20 1.394(12) 1_555 1_555 no C20 C21 1.374(13) 1_555 1_555 no C21 C22 1.395(13) 1_555 1_555 no C22 C23 1.383(10) 1_555 1_555 no C23 C46 1.479(11) 1_555 1_555 no C24 C25 1.375(10) 1_555 1_555 no C25 C26 1.448(9) 1_555 1_555 no C25 C32 1.472(9) 1_555 1_555 no C26 C27 1.419(9) 1_555 1_555 no C26 C31 1.416(10) 1_555 1_555 no C27 C28 1.386(10) 1_555 1_555 no C28 C29 1.386(10) 1_555 1_555 no C29 C30 1.411(10) 1_555 1_555 no C30 C31 1.415(10) 1_555 1_555 no C30 C40 1.397(10) 1_555 1_555 no C32 C33 1.391(5) 1_555 1_555 no C32 C37 1.391(5) 1_555 1_555 no C33 C34 1.384(6) 1_555 1_555 no C34 C35 1.376(5) 1_555 1_555 no C35 C36 1.376(5) 1_555 1_555 no C36 C37 1.384(6) 1_555 1_555 no C41 C42 1.378(10) 1_555 1_555 no C41 C46 1.417(10) 1_555 1_555 no C42 C43 1.362(11) 1_555 1_555 no C43 C44 1.399(12) 1_555 1_555 no C44 C45 1.387(12) 1_555 1_555 no C45 C46 1.399(11) 1_555 1_555 no C1Ch Cl1Ch 1.666(7) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni N2 93.4(2) 1_555 1_555 1_555 no N1 Ni N3 109.7(2) 1_555 1_555 1_555 no N1 Ni N4 140.8(3) 1_555 1_555 1_555 no N2 Ni N3 127.6(3) 1_555 1_555 1_555 no N2 Ni N4 99.0(2) 1_555 1_555 1_555 no N3 Ni N4 91.7(2) 1_555 1_555 1_555 no C4 O1 C15 118.6(6) 1_555 1_555 1_555 no C6 O2 C16 119.4(7) 1_555 1_555 1_555 no C27 O3 C38 117.6(6) 1_555 1_555 1_555 no C29 O4 C39 119.2(6) 1_555 1_555 1_555 no Ni N1 C1 129.7(5) 1_555 1_555 1_555 no Ni N1 C8 124.6(5) 1_555 1_555 1_555 no C1 N1 C8 105.6(6) 1_555 1_555 1_555 no Ni N2 C17 127.2(5) 1_555 1_555 1_555 no Ni N2 C18 118.1(5) 1_555 1_555 1_555 no C17 N2 C18 114.3(6) 1_555 1_555 1_555 no Ni N3 C24 128.5(5) 1_555 1_555 1_555 no Ni N3 C31 125.3(5) 1_555 1_555 1_555 no C24 N3 C31 106.2(6) 1_555 1_555 1_555 no Ni N4 C40 128.4(5) 1_555 1_555 1_555 no Ni N4 C41 114.1(4) 1_555 1_555 1_555 no C40 N4 C41 117.5(6) 1_555 1_555 1_555 no N1 C1 C2 112.9(6) 1_555 1_555 1_555 no C1 C2 C3 105.5(6) 1_555 1_555 1_555 no C1 C2 C9 122.8(6) 1_555 1_555 1_555 no C3 C2 C9 131.6(6) 1_555 1_555 1_555 no C2 C3 C4 137.1(7) 1_555 1_555 1_555 no C2 C3 C8 105.8(6) 1_555 1_555 1_555 no C4 C3 C8 117.2(7) 1_555 1_555 1_555 no O1 C4 C3 116.8(7) 1_555 1_555 1_555 no O1 C4 C5 122.3(7) 1_555 1_555 1_555 no C3 C4 C5 120.9(7) 1_555 1_555 1_555 no C4 C5 C6 119.9(7) 1_555 1_555 1_555 no O2 C6 C5 122.1(7) 1_555 1_555 1_555 no O2 C6 C7 116.1(7) 1_555 1_555 1_555 no C5 C6 C7 121.8(8) 1_555 1_555 1_555 no C6 C7 C8 117.0(7) 1_555 1_555 1_555 no C6 C7 C17 118.4(7) 1_555 1_555 1_555 no C8 C7 C17 124.7(6) 1_555 1_555 1_555 no N1 C8 C3 110.2(7) 1_555 1_555 1_555 no N1 C8 C7 126.5(7) 1_555 1_555 1_555 no C3 C8 C7 123.2(7) 1_555 1_555 1_555 no C2 C9 C10 119.7(5) 1_555 1_555 1_555 no C2 C9 C14 122.1(4) 1_555 1_555 1_555 no C10 C9 C14 117.6(5) 1_555 1_555 1_555 no C9 C10 C11 121.5(4) 1_555 1_555 1_555 no C10 C11 C12 119.2(4) 1_555 1_555 1_555 no Cl1 C12 C11 119.5(3) 1_555 1_555 1_555 no Cl1 C12 C13 119.5(3) 1_555 1_555 1_555 no C11 C12 C13 121.0(6) 1_555 1_555 1_555 no C12 C13 C14 119.2(4) 1_555 1_555 1_555 no C9 C14 C13 121.5(4) 1_555 1_555 1_555 no N2 C17 C7 123.3(7) 1_555 1_555 1_555 no N2 C18 C19 118.0(7) 1_555 1_555 1_555 no N2 C18 C23 119.7(7) 1_555 1_555 1_555 no C19 C18 C23 122.2(8) 1_555 1_555 1_555 no C18 C19 C20 119.6(8) 1_555 1_555 1_555 no C19 C20 C21 118.9(9) 1_555 1_555 1_555 no C20 C21 C22 121.2(8) 1_555 1_555 1_555 no C21 C22 C23 120.4(8) 1_555 1_555 1_555 no C18 C23 C22 117.7(8) 1_555 1_555 1_555 no C18 C23 C46 122.9(7) 1_555 1_555 1_555 no C22 C23 C46 119.2(7) 1_555 1_555 1_555 no N3 C24 C25 113.4(6) 1_555 1_555 1_555 no C24 C25 C26 103.7(6) 1_555 1_555 1_555 no C24 C25 C32 125.8(6) 1_555 1_555 1_555 no C26 C25 C32 130.5(6) 1_555 1_555 1_555 no C25 C26 C27 134.7(7) 1_555 1_555 1_555 no C25 C26 C31 107.4(6) 1_555 1_555 1_555 no C27 C26 C31 117.6(7) 1_555 1_555 1_555 no O3 C27 C26 116.4(7) 1_555 1_555 1_555 no O3 C27 C28 123.8(6) 1_555 1_555 1_555 no C26 C27 C28 119.8(7) 1_555 1_555 1_555 no C27 C28 C29 121.3(7) 1_555 1_555 1_555 no O4 C29 C28 121.9(6) 1_555 1_555 1_555 no O4 C29 C30 116.2(7) 1_555 1_555 1_555 no C28 C29 C30 121.9(7) 1_555 1_555 1_555 no C29 C30 C31 116.0(7) 1_555 1_555 1_555 no C29 C30 C40 121.4(7) 1_555 1_555 1_555 no C31 C30 C40 122.3(6) 1_555 1_555 1_555 no N3 C31 C26 109.3(6) 1_555 1_555 1_555 no N3 C31 C30 127.4(7) 1_555 1_555 1_555 no C26 C31 C30 123.3(6) 1_555 1_555 1_555 no C25 C32 C33 120.8(5) 1_555 1_555 1_555 no C25 C32 C37 121.5(5) 1_555 1_555 1_555 no C33 C32 C37 117.6(5) 1_555 1_555 1_555 no C32 C33 C34 121.5(4) 1_555 1_555 1_555 no C33 C34 C35 119.2(4) 1_555 1_555 1_555 no Cl2 C35 C34 119.5(3) 1_555 1_555 1_555 no Cl2 C35 C36 119.5(3) 1_555 1_555 1_555 no C34 C35 C36 121.0(6) 1_555 1_555 1_555 no C35 C36 C37 119.2(4) 1_555 1_555 1_555 no C32 C37 C36 121.5(4) 1_555 1_555 1_555 no N4 C40 C30 124.6(7) 1_555 1_555 1_555 no N4 C41 C42 121.5(7) 1_555 1_555 1_555 no N4 C41 C46 119.2(7) 1_555 1_555 1_555 no C42 C41 C46 119.3(7) 1_555 1_555 1_555 no C41 C42 C43 122.8(8) 1_555 1_555 1_555 no C42 C43 C44 118.7(8) 1_555 1_555 1_555 no C43 C44 C45 120.1(8) 1_555 1_555 1_555 no C44 C45 C46 121.2(8) 1_555 1_555 1_555 no C23 C46 C41 123.9(7) 1_555 1_555 1_555 no C23 C46 C45 118.1(7) 1_555 1_555 1_555 no C41 C46 C45 117.9(7) 1_555 1_555 1_555 no Cl1Ch C1Ch Cl2Ch 109.4 1_555 1_555 1_555 no #===END