Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'I. Dance' 'John C. McMurtrie' _publ_contact_author_name 'Prof I. Dance' _publ_contact_author_address ; School of Chemistry University of New South Wales Sydney NSW 2052 AUSTRALIA ; _publ_contact_author_email I.DANCE@UNSW.EDU.AU _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Engineering the metal-terpy grid with complexes containing 4'-hydroxy terpyridine ; data_crystal_2a _database_code_depnum_ccdc_archive 'CCDC 261247' _audit_creation_method 'RAELSPUB and manual entry' # _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H22 Fe N6 O2 2+,2(B F4 1-),H2 O' _chemical_formula_sum 'C30 H24 B2 F8 Fe N6 O3' _chemical_formula_iupac ? _chemical_formula_weight 746.0 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.668(5) _cell_length_b 9.278(6) _cell_length_c 20.214(9) _cell_angle_alpha 78.80(4) _cell_angle_beta 78.24(4) _cell_angle_gamma 87.93(3) _cell_volume 1561(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 18 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour purple _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.59 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756.0 _exptl_absorpt_coefficient_mu 0.570 _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 5584 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5415 _reflns_number_gt 4174 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.081 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4174 _refine_ls_number_parameters 149 _refine_ls_goodness_of_fit_ref 1.95 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.81 _refine_diff_density_min -1.11 _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 Fe 0.49326(6) 0.63798(6) 0.24545(3) 0.0299(2) Uani Fe 1.0 O1A 0.7350(4) 0.7789(4) -0.0582(1) 0.068(1) Uani O 1.0 N1A 0.7025(2) 0.7135(3) 0.2453(1) 0.0332(4) Uani N 1.0 N2A 0.5715(3) 0.6775(2) 0.1498(1) 0.0306(5) Uani N 1.0 N3A 0.3113(3) 0.5708(3) 0.2140(1) 0.0337(5) Uani N 1.0 C1A 0.7614(3) 0.7308(3) 0.3001(1) 0.0417(5) Uani C 1.0 C2A 0.9066(4) 0.7952(4) 0.2933(2) 0.0486(5) Uani C 1.0 C3A 0.9951(3) 0.8439(3) 0.2286(2) 0.0466(5) Uani C 1.0 C4A 0.9370(3) 0.8273(3) 0.1714(1) 0.0400(4) Uani C 1.0 C5A 0.7913(3) 0.7622(3) 0.1811(1) 0.0333(4) Uani C 1.0 C6A 0.7161(3) 0.7382(3) 0.1255(1) 0.0331(5) Uani C 1.0 C7A 0.7766(3) 0.7744(3) 0.0559(1) 0.0422(6) Uani C 1.0 C8A 0.6847(3) 0.7468(3) 0.0106(2) 0.0499(8) Uani C 1.0 C9A 0.5355(3) 0.6842(3) 0.0358(1) 0.0461(7) Uani C 1.0 C10A 0.4822(3) 0.6507(3) 0.1060(1) 0.0356(5) Uani C 1.0 C11A 0.3295(3) 0.5849(3) 0.1442(1) 0.0363(5) Uani C 1.0 C12A 0.2167(4) 0.5365(4) 0.1142(1) 0.0458(6) Uani C 1.0 C13A 0.0805(3) 0.4714(4) 0.1561(2) 0.0505(7) Uani C 1.0 C14A 0.0611(3) 0.4567(3) 0.2263(2) 0.0478(8) Uani C 1.0 C15A 0.1778(3) 0.5071(3) 0.2537(1) 0.0403(6) Uani C 1.0 O1B 0.2302(4) 0.5218(3) 0.5479(1) 0.065(1) Uani O 1.0 N1B 0.4011(3) 0.8339(2) 0.2534(1) 0.0315(5) Uani N 1.0 N2B 0.4117(3) 0.6036(2) 0.3411(1) 0.0303(5) Uani N 1.0 N3B 0.5630(3) 0.4332(2) 0.2700(1) 0.0344(6) Uani N 1.0 C1B 0.4082(3) 0.9541(3) 0.2032(1) 0.0383(5) Uani C 1.0 C2B 0.3417(4) 1.0866(3) 0.2153(2) 0.0446(6) Uani C 1.0 C3B 0.2654(4) 1.0975(3) 0.2808(2) 0.0444(5) Uani C 1.0 C4B 0.2565(3) 0.9754(3) 0.3333(1) 0.0391(5) Uani C 1.0 C5B 0.3249(3) 0.8458(3) 0.3183(1) 0.0324(5) Uani C 1.0 C6B 0.3292(3) 0.7101(3) 0.3696(1) 0.0327(5) Uani C 1.0 C7B 0.2657(3) 0.6880(3) 0.4391(1) 0.0416(6) Uani C 1.0 C8B 0.2884(3) 0.5525(3) 0.4796(2) 0.0483(7) Uani C 1.0 C9B 0.3735(3) 0.4428(3) 0.4500(1) 0.0445(6) Uani C 1.0 C10B 0.4338(3) 0.4721(3) 0.3802(1) 0.0351(5) Uani C 1.0 C11B 0.5243(3) 0.3723(3) 0.3385(1) 0.0366(5) Uani C 1.0 C12B 0.5662(4) 0.2307(3) 0.3641(1) 0.0459(8) Uani C 1.0 C13B 0.6503(4) 0.1475(3) 0.3190(2) 0.0519(9) Uani C 1.0 C14B 0.6899(4) 0.2078(3) 0.2500(2) 0.050(1) Uani C 1.0 C15B 0.6449(3) 0.3502(3) 0.2271(1) 0.0419(8) Uani C 1.0 OW 0.0164(5) 0.7070(4) 0.5969(2) 0.070(1) Uani O 1.0 B1A 0.81859(21) 0.20038(22) 0.06134(9) 0.063(2) Uani B 1.0 F1A 0.8463(3) 0.1672(3) -0.0029(1) 0.083(2) Uani F 1.0 F2A 0.6935(3) 0.1198(4) 0.1018(1) 0.109(2) Uani F 1.0 F3A 0.9489(3) 0.1680(4) 0.0895(1) 0.092(2) Uani F 1.0 F4A 0.7856(5) 0.3465(3) 0.0569(2) 0.129(1) Uani F 1.0 B1B 0.7834(6) 0.9208(5) 0.4744(2) 0.064(2) Uani B 0.46 F1B 0.6755(8) 0.8624(9) 0.4463(4) 0.078(2) Uani F 0.46 F2B 0.7454(11) 1.0635(6) 0.4781(4) 0.131(4) Uani F 0.46 F3B 0.7831(9) 0.8421(8) 0.5389(3) 0.100(2) Uani F 0.46 F4B 0.9297(7) 0.9153(10) 0.4341(3) 0.104(3) Uani F 0.46 B1B' 0.8053(5) 0.9155(5) 0.4591(2) 0.061(2) Uani B 0.54 F1B' 0.6743(6) 0.8727(7) 0.4401(3) 0.078(2) Uani F 0.54 F2B' 0.7615(8) 0.9701(7) 0.5181(3) 0.115(3) Uani F 0.54 F3B' 0.9018(7) 0.7975(6) 0.4701(4) 0.107(4) Uani F 0.54 F4B' 0.8834(7) 1.0216(6) 0.4080(3) 0.101(3) Uani F 0.54 HO1A 0.8472 0.8124 -0.0689 0.072 Uani H 1.0 HC1A 0.6978 0.6957 0.3473 0.048 Uani H 1.0 HC2A 0.9468 0.8063 0.3350 0.060 Uani H 1.0 HC3A 1.1003 0.8907 0.2227 0.055 Uani H 1.0 HC4A 0.9996 0.8620 0.1239 0.045 Uani H 1.0 HC7A 0.8838 0.8193 0.0383 0.048 Uani H 1.0 HC9A 0.4688 0.6641 0.0036 0.055 Uani H 1.0 HC12A 0.2330 0.5482 0.0630 0.054 Uani H 1.0 HC13A -0.0028 0.4356 0.1355 0.061 Uani H 1.0 HC14A -0.0365 0.4100 0.2573 0.056 Uani H 1.0 HC15A 0.1627 0.4960 0.3048 0.044 Uani H 1.0 HO1B 0.1521 0.5947 0.5653 0.071 Uani H 1.0 HC1B 0.4635 0.9472 0.1554 0.043 Uani H 1.0 HC2B 0.3492 1.1737 0.1769 0.054 Uani H 1.0 HC3B 0.2167 1.1925 0.2905 0.052 Uani H 1.0 HC4B 0.2015 0.9811 0.3813 0.044 Uani H 1.0 HC7B 0.2047 0.7674 0.4599 0.048 Uani H 1.0 HC9B 0.3903 0.3451 0.4787 0.053 Uani H 1.0 HC12B 0.5363 0.1888 0.4145 0.052 Uani H 1.0 HC13B 0.6820 0.0446 0.3365 0.062 Uani H 1.0 HC14B 0.7505 0.1492 0.2168 0.059 Uani H 1.0 HC15B 0.6741 0.3932 0.1768 0.046 Uani H 1.0 H1OW 0.0716 0.8007 0.5954 0.070 Uani H 1.0 H2OW -0.0705 0.7615 0.5772 0.070 Uani H 1.0 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 Fe 0.0290(3) 0.0353(3) 0.0239(3) -0.0022(2) -0.0025(2) -0.0051(2) Fe O1A 0.066(2) 0.106(3) 0.0258(6) -0.013(2) 0.0000(6) -0.0055(9) O N1A 0.0345(6) 0.0367(8) 0.0293(7) -0.0020(5) -0.0062(5) -0.0082(6) N N2A 0.0328(6) 0.0330(9) 0.0254(7) -0.0014(5) -0.0036(4) -0.0062(6) N N3A 0.0324(6) 0.0348(8) 0.0331(7) -0.0028(5) -0.0041(4) -0.0067(5) N C1A 0.0422(7) 0.052(1) 0.0345(8) -0.0039(6) -0.0112(5) -0.0126(8) C C2A 0.0450(8) 0.060(1) 0.0478(9) -0.0061(8) -0.0167(7) -0.0173(9) C C3A 0.0387(7) 0.050(1) 0.055(1) -0.0070(7) -0.0130(6) -0.0140(9) C C4A 0.0340(6) 0.0406(9) 0.0445(8) -0.0056(6) -0.0056(5) -0.0078(6) C C5A 0.0325(6) 0.0342(8) 0.0325(7) -0.0027(5) -0.0043(4) -0.0067(5) C C6A 0.0337(6) 0.0364(9) 0.0274(7) -0.0026(5) -0.0020(5) -0.0051(5) C C7A 0.0407(7) 0.053(1) 0.0284(6) -0.0058(6) 0.0007(5) -0.0036(7) C C8A 0.0501(9) 0.071(2) 0.0255(6) -0.0072(8) -0.0018(5) -0.0059(7) C C9A 0.0480(8) 0.064(1) 0.0268(6) -0.0052(7) -0.0072(5) -0.0097(7) C C10A 0.0376(6) 0.0426(9) 0.0274(6) -0.0024(5) -0.0063(4) -0.0084(6) C C11A 0.0359(6) 0.0405(8) 0.0344(6) -0.0029(5) -0.0083(4) -0.0098(5) C C12A 0.0422(7) 0.054(1) 0.0463(7) -0.0055(6) -0.0148(6) -0.0155(8) C C13A 0.0405(7) 0.055(1) 0.061(1) -0.0083(7) -0.0153(8) -0.016(1) C C14A 0.0357(6) 0.048(1) 0.058(1) -0.0088(8) -0.0071(6) -0.009(1) C C15A 0.0338(6) 0.042(1) 0.0426(8) -0.0060(7) -0.0025(5) -0.0056(7) C O1B 0.088(2) 0.069(2) 0.0273(9) 0.014(1) 0.0041(7) -0.0016(5) O N1B 0.0281(7) 0.0353(6) 0.0295(6) -0.0033(5) -0.0032(5) -0.0044(5) N N2B 0.0265(7) 0.0365(6) 0.0267(7) -0.0023(5) -0.0034(5) -0.0051(4) N N3B 0.0309(7) 0.0390(7) 0.0328(6) 0.0019(5) -0.0048(5) -0.0079(4) N C1B 0.0402(8) 0.0369(6) 0.0340(6) -0.0026(6) -0.0034(6) -0.0015(6) C C2B 0.052(1) 0.0363(6) 0.0425(8) 0.0006(6) -0.0081(8) -0.0026(6) C C3B 0.052(1) 0.0377(6) 0.0450(9) 0.0049(6) -0.0111(8) -0.0093(5) C C4B 0.0412(9) 0.0399(6) 0.0374(7) 0.0042(6) -0.0076(5) -0.0112(5) C C5B 0.0298(7) 0.0368(6) 0.0304(6) -0.0008(5) -0.0046(5) -0.0074(4) C C6B 0.0306(7) 0.0394(5) 0.0272(7) -0.0004(5) -0.0029(5) -0.0067(4) C C7B 0.046(1) 0.0489(7) 0.0275(7) 0.0046(6) -0.0010(6) -0.0076(5) C C8B 0.059(1) 0.0535(9) 0.0268(8) 0.0061(8) -0.0001(6) -0.0033(5) C C9B 0.054(1) 0.0463(7) 0.0286(7) 0.0034(6) -0.0035(6) -0.0008(5) C C10B 0.0359(7) 0.0388(6) 0.0287(7) 0.0000(5) -0.0048(5) -0.0034(4) C C11B 0.0371(7) 0.0379(7) 0.0339(6) 0.0022(5) -0.0074(5) -0.0052(4) C C12B 0.054(1) 0.0403(7) 0.0424(9) 0.0078(7) -0.0123(8) -0.0046(6) C C13B 0.062(2) 0.0434(8) 0.052(1) 0.0145(8) -0.016(1) -0.0104(7) C C14B 0.055(1) 0.0477(9) 0.050(1) 0.0156(9) -0.011(1) -0.0156(7) C C15B 0.0409(9) 0.0455(8) 0.0392(7) 0.0085(7) -0.0055(7) -0.0125(6) C OW 0.080(3) 0.062(2) 0.055(2) 0.011(2) 0.004(2) -0.001(2) O B1A 0.052(2) 0.082(2) 0.048(1) -0.001(2) 0.006(1) -0.014(1) B F1A 0.084(2) 0.110(3) 0.050(2) -0.009(2) 0.007(1) -0.022(1) F F2A 0.072(3) 0.184(3) 0.058(2) -0.046(2) 0.009(2) -0.009(2) F F3A 0.060(2) 0.138(3) 0.072(2) -0.004(2) -0.010(2) -0.012(2) F F4A 0.206(4) 0.091(2) 0.105(3) 0.036(2) -0.060(3) -0.033(1) F B1B 0.078(3) 0.062(2) 0.055(3) -0.006(2) -0.017(2) -0.017(2) B F1B 0.085(3) 0.078(3) 0.073(3) -0.023(3) -0.032(2) 0.003(2) F F2B 0.216(8) 0.080(4) 0.123(4) 0.031(3) -0.067(5) -0.054(3) F F3B 0.132(6) 0.110(4) 0.062(2) -0.043(3) -0.036(2) 0.002(2) F F4B 0.067(4) 0.136(4) 0.095(4) -0.005(2) -0.012(3) 0.006(3) F B1B' 0.069(3) 0.060(2) 0.056(3) -0.006(2) -0.016(2) -0.014(2) B F1B' 0.085(3) 0.077(3) 0.073(3) -0.022(3) -0.032(2) 0.002(2) F F2B' 0.182(5) 0.106(4) 0.072(2) 0.002(3) -0.033(3) -0.044(3) F F3B' 0.099(4) 0.096(3) 0.129(4) 0.025(3) -0.039(4) -0.014(3) F F4B' 0.098(4) 0.117(3) 0.083(4) -0.046(3) -0.039(4) 0.023(3) F # 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 Fe N1A 1.967(2) 1_555 1_555 no Fe N2A 1.882(2) 1_555 1_555 no Fe N3A 1.979(2) 1_555 1_555 no Fe N1B 1.981(2) 1_555 1_555 no Fe N2B 1.886(2) 1_555 1_555 no Fe N3B 1.973(2) 1_555 1_555 no O1A C8A 1.348(4) 1_555 1_555 no N1A C1A 1.349(2) 1_555 1_555 no N1A C5A 1.367(2) 1_555 1_555 no N2A C6A 1.350(2) 1_555 1_555 no N2A C10A 1.350(2) 1_555 1_555 no N3A C11A 1.367(2) 1_555 1_555 no N3A C15A 1.349(2) 1_555 1_555 no C1A C2A 1.382(3) 1_555 1_555 no C2A C3A 1.375(3) 1_555 1_555 no C3A C4A 1.386(3) 1_555 1_555 no C4A C5A 1.380(3) 1_555 1_555 no C5A C6A 1.464(3) 1_555 1_555 no C6A C7A 1.377(3) 1_555 1_555 no C7A C8A 1.392(3) 1_555 1_555 no C8A C9A 1.392(3) 1_555 1_555 no C9A C10A 1.377(3) 1_555 1_555 no C10A C11A 1.476(3) 1_555 1_555 no C11A C12A 1.380(3) 1_555 1_555 no C12A C13A 1.386(3) 1_555 1_555 no C13A C14A 1.375(3) 1_555 1_555 no C14A C15A 1.382(3) 1_555 1_555 no O1B C8B 1.348(4) 1_555 1_555 no N1B C1B 1.349(2) 1_555 1_555 no N1B C5B 1.367(2) 1_555 1_555 no N2B C6B 1.350(2) 1_555 1_555 no N2B C10B 1.350(2) 1_555 1_555 no N3B C11B 1.367(2) 1_555 1_555 no N3B C15B 1.349(2) 1_555 1_555 no C1B C2B 1.382(3) 1_555 1_555 no C2B C3B 1.375(3) 1_555 1_555 no C3B C4B 1.386(3) 1_555 1_555 no C4B C5B 1.380(3) 1_555 1_555 no C5B C6B 1.471(3) 1_555 1_555 no C6B C7B 1.377(3) 1_555 1_555 no C7B C8B 1.392(3) 1_555 1_555 no C8B C9B 1.392(3) 1_555 1_555 no C9B C10B 1.377(3) 1_555 1_555 no C10B C11B 1.471(3) 1_555 1_555 no C11B C12B 1.380(3) 1_555 1_555 no C12B C13B 1.386(3) 1_555 1_555 no C13B C14B 1.375(3) 1_555 1_555 no C14B C15B 1.382(3) 1_555 1_555 no B1A F1A 1.365(1) 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 N1A Fe N2A 81.4(1) 1_555 1_555 1_555 no N1A Fe N3A 161.8(1) 1_555 1_555 1_555 no N1A Fe N1B 89.9(1) 1_555 1_555 1_555 no N1A Fe N2B 98.9(1) 1_555 1_555 1_555 no N1A Fe N3B 91.4(1) 1_555 1_555 1_555 no N2A Fe N3A 80.4(1) 1_555 1_555 1_555 no N2A Fe N1B 97.5(1) 1_555 1_555 1_555 no N2A Fe N2B 178.3(1) 1_555 1_555 1_555 no N2A Fe N3B 101.0(1) 1_555 1_555 1_555 no N3A Fe N1B 93.7(1) 1_555 1_555 1_555 no N3A Fe N2B 99.3(1) 1_555 1_555 1_555 no N3A Fe N3B 90.8(1) 1_555 1_555 1_555 no N1B Fe N2B 80.9(1) 1_555 1_555 1_555 no N1B Fe N3B 161.5(1) 1_555 1_555 1_555 no N2B Fe N3B 80.7(1) 1_555 1_555 1_555 no Fe N1A C1A 127.6(2) 1_555 1_555 1_555 no Fe N1A C5A 114.4(2) 1_555 1_555 1_555 no C1A N1A C5A 117.8(1) 1_555 1_555 1_555 no Fe N2A C6A 118.9(2) 1_555 1_555 1_555 no Fe N2A C10A 120.6(2) 1_555 1_555 1_555 no C6A N2A C10A 120.5(2) 1_555 1_555 1_555 no Fe N3A C11A 115.0(2) 1_555 1_555 1_555 no Fe N3A C15A 127.1(2) 1_555 1_555 1_555 no C11A N3A C15A 117.8(1) 1_555 1_555 1_555 no N1A C1A C2A 122.4(2) 1_555 1_555 1_555 no C1A C2A C3A 119.3(2) 1_555 1_555 1_555 no C2A C3A C4A 119.3(2) 1_555 1_555 1_555 no C3A C4A C5A 119.0(2) 1_555 1_555 1_555 no N1A C5A C4A 122.1(2) 1_555 1_555 1_555 no N1A C5A C6A 113.3(2) 1_555 1_555 1_555 no C4A C5A C6A 124.6(2) 1_555 1_555 1_555 no N2A C6A C5A 111.9(2) 1_555 1_555 1_555 no N2A C6A C7A 121.2(2) 1_555 1_555 1_555 no C5A C6A C7A 126.8(2) 1_555 1_555 1_555 no C6A C7A C8A 118.4(2) 1_555 1_555 1_555 no O1A C8A C7A 122.1(2) 1_555 1_555 1_555 no O1A C8A C9A 117.6(2) 1_555 1_555 1_555 no C7A C8A C9A 120.3(3) 1_555 1_555 1_555 no C8A C9A C10A 118.4(2) 1_555 1_555 1_555 no N2A C10A C9A 121.2(2) 1_555 1_555 1_555 no N2A C10A C11A 110.7(2) 1_555 1_555 1_555 no C9A C10A C11A 128.1(2) 1_555 1_555 1_555 no N3A C11A C10A 113.3(2) 1_555 1_555 1_555 no N3A C11A C12A 122.1(2) 1_555 1_555 1_555 no C10A C11A C12A 124.6(2) 1_555 1_555 1_555 no C11A C12A C13A 119.0(2) 1_555 1_555 1_555 no C12A C13A C14A 119.3(2) 1_555 1_555 1_555 no C13A C14A C15A 119.3(2) 1_555 1_555 1_555 no N3A C15A C14A 122.4(2) 1_555 1_555 1_555 no Fe N1B C1B 127.6(2) 1_555 1_555 1_555 no Fe N1B C5B 114.5(2) 1_555 1_555 1_555 no C1B N1B C5B 117.8(1) 1_555 1_555 1_555 no Fe N2B C6B 119.6(2) 1_555 1_555 1_555 no Fe N2B C10B 119.8(2) 1_555 1_555 1_555 no C6B N2B C10B 120.5(2) 1_555 1_555 1_555 no Fe N3B C11B 115.0(2) 1_555 1_555 1_555 no Fe N3B C15B 127.2(2) 1_555 1_555 1_555 no C11B N3B C15B 117.8(1) 1_555 1_555 1_555 no N1B C1B C2B 122.4(2) 1_555 1_555 1_555 no C1B C2B C3B 119.3(2) 1_555 1_555 1_555 no C2B C3B C4B 119.3(2) 1_555 1_555 1_555 no C3B C4B C5B 119.0(2) 1_555 1_555 1_555 no N1B C5B C4B 122.1(2) 1_555 1_555 1_555 no N1B C5B C6B 113.4(2) 1_555 1_555 1_555 no C4B C5B C6B 124.4(2) 1_555 1_555 1_555 no N2B C6B C5B 111.5(2) 1_555 1_555 1_555 no N2B C6B C7B 121.2(2) 1_555 1_555 1_555 no C5B C6B C7B 127.3(2) 1_555 1_555 1_555 no C6B C7B C8B 118.4(2) 1_555 1_555 1_555 no O1B C8B C7B 122.1(2) 1_555 1_555 1_555 no O1B C8B C9B 117.6(2) 1_555 1_555 1_555 no C7B C8B C9B 120.3(3) 1_555 1_555 1_555 no C8B C9B C10B 118.4(2) 1_555 1_555 1_555 no N2B C10B C9B 121.2(2) 1_555 1_555 1_555 no N2B C10B C11B 111.3(2) 1_555 1_555 1_555 no C9B C10B C11B 127.5(2) 1_555 1_555 1_555 no N3B C11B C10B 113.2(2) 1_555 1_555 1_555 no N3B C11B C12B 122.1(2) 1_555 1_555 1_555 no C10B C11B C12B 124.7(2) 1_555 1_555 1_555 no C11B C12B C13B 119.0(2) 1_555 1_555 1_555 no C12B C13B C14B 119.3(2) 1_555 1_555 1_555 no C13B C14B C15B 119.3(2) 1_555 1_555 1_555 no N3B C15B C14B 122.4(2) 1_555 1_555 1_555 no F1A B1A F2A 109.47 1_555 1_555 1_555 no data_crystal_3b _database_code_depnum_ccdc_archive 'CCDC 261248' _audit_creation_method SHELXL-97 # CHEMICAL DATA _chemical_name_systematic ; [Ru(terpy)(terpyOH)](BF4)2.H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H22 B2 F8 N6 O2 Ru' _chemical_formula_weight 773.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7533(10) _cell_length_b 8.9226(10) _cell_length_c 19.8607(23) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.557(5) _cell_angle_gamma 90.000(5) _cell_volume 1529.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 3.086 _cell_measurement_theta_max 28.220 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'intense red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.78725 _exptl_absorpt_correction_T_max 0.94901 _exptl_absorpt_process_details 'Gaussian (XPREP,Bruker 1995; Coppens,1965)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 298 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 13657 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6943 _reflns_number_gt 6838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+2.7438P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 6943 _refine_ls_number_parameters 437 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.011 _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 Ru1 Ru 0.73834(3) 0.26487(4) 0.241414(12) 0.01898(8) Uani 1 1 d . . . N1 N 0.8350(4) 0.0566(4) 0.27192(17) 0.0224(6) Uani 1 1 d . . . N2 N 0.7478(3) 0.2763(7) 0.34203(14) 0.0197(6) Uani 1 1 d . . . N3 N 0.6531(3) 0.4796(4) 0.25229(17) 0.0195(6) Uani 1 1 d . . . N4 N 0.9511(4) 0.3537(4) 0.22967(19) 0.0231(7) Uani 1 1 d . . . N5 N 0.7269(4) 0.2476(5) 0.14124(15) 0.0210(8) Uani 1 1 d . . . N6 N 0.5184(4) 0.1749(4) 0.21262(17) 0.0210(6) Uani 1 1 d . . . B1 B 0.2519(8) 0.3208(10) 0.4459(3) 0.067(2) Uani 1 1 d D . . F1 F 0.1110(4) 0.3731(5) 0.4436(2) 0.0611(9) Uiso 1 1 d D . . F2 F 0.3283(5) 0.2931(6) 0.5099(2) 0.0819(13) Uiso 1 1 d D . . F3 F 0.2890(7) 0.2361(8) 0.3970(3) 0.1120(18) Uiso 1 1 d D . . F4 F 0.3339(9) 0.4583(8) 0.4308(4) 0.135(2) Uiso 1 1 d D . . B2 B 0.8107(7) -0.2312(9) 0.0579(2) 0.0447(11) Uani 1 1 d D . . F5 F 0.7045(5) -0.1688(5) 0.09383(17) 0.0629(10) Uani 1 1 d D . . F6 F 0.7814(5) -0.3825(4) 0.0538(2) 0.0718(12) Uani 1 1 d D . . F7 F 0.9626(4) -0.2056(6) 0.09128(18) 0.0718(14) Uani 1 1 d D . . F8 F 0.7901(5) -0.1715(5) -0.00665(19) 0.0659(11) Uani 1 1 d D . . C1 C 0.8795(4) -0.0505(5) 0.2322(2) 0.0253(8) Uani 1 1 d . . . H1 H 0.8636 -0.0353 0.1842 0.030 Uiso 1 1 calc R . . C2 C 0.9484(5) -0.1835(5) 0.2586(3) 0.0322(9) Uani 1 1 d . . . H2 H 0.9782 -0.2580 0.2292 0.039 Uiso 1 1 calc R . . C3 C 0.9726(5) -0.2052(5) 0.3288(3) 0.0341(11) Uani 1 1 d . . . H3 H 1.0203 -0.2945 0.3481 0.041 Uiso 1 1 calc R . . C4 C 0.9262(5) -0.0948(5) 0.3706(2) 0.0304(9) Uani 1 1 d . . . H4 H 0.9418 -0.1079 0.4187 0.037 Uiso 1 1 calc R . . C5 C 0.8569(4) 0.0347(4) 0.3412(2) 0.0219(7) Uani 1 1 d . . . C6 C 0.8039(4) 0.1581(5) 0.3814(2) 0.0220(7) Uani 1 1 d . . . C7 C 0.8078(5) 0.1606(5) 0.4515(2) 0.0271(8) Uani 1 1 d . . . H7 H 0.8492 0.0785 0.4791 0.033 Uiso 1 1 calc R . . C8 C 0.7498(5) 0.2861(6) 0.48055(19) 0.0284(10) Uani 1 1 d . . . C9 C 0.6937(5) 0.4088(5) 0.4391(2) 0.0275(8) Uani 1 1 d . . . H9 H 0.6566 0.4963 0.4584 0.033 Uiso 1 1 calc R . . C10 C 0.6938(4) 0.3983(5) 0.3694(2) 0.0216(7) Uani 1 1 d . . . C11 C 0.6396(4) 0.5151(4) 0.3183(2) 0.0214(7) Uani 1 1 d . . . C12 C 0.5809(5) 0.6528(5) 0.3341(2) 0.0269(8) Uani 1 1 d . . . H12 H 0.5700 0.6749 0.3798 0.032 Uiso 1 1 calc R . . C13 C 0.5386(4) 0.7571(7) 0.2835(2) 0.0296(7) Uani 1 1 d . . . H13 H 0.4968 0.8509 0.2939 0.036 Uiso 1 1 calc R . . C14 C 0.5575(5) 0.7237(4) 0.2175(2) 0.0276(9) Uani 1 1 d . . . H14 H 0.5317 0.7956 0.1821 0.033 Uiso 1 1 calc R . . C15 C 0.6148(4) 0.5838(5) 0.2033(2) 0.0232(8) Uani 1 1 d . . . H15 H 0.6273 0.5611 0.1578 0.028 Uiso 1 1 calc R . . C16 C 1.0595(5) 0.4097(5) 0.2784(3) 0.0294(9) Uani 1 1 d . . . H16 H 1.0451 0.4035 0.3246 0.035 Uiso 1 1 calc R . . C17 C 1.1936(5) 0.4772(6) 0.2631(3) 0.0402(12) Uani 1 1 d . . . H17 H 1.2692 0.5166 0.2986 0.048 Uiso 1 1 calc R . . C18 C 1.2155(6) 0.4862(6) 0.1958(4) 0.0440(14) Uani 1 1 d . . . H18 H 1.3056 0.5330 0.1847 0.053 Uiso 1 1 calc R . . C19 C 1.1050(6) 0.4263(6) 0.1446(3) 0.0389(11) Uani 1 1 d . . . H19 H 1.1186 0.4313 0.0982 0.047 Uiso 1 1 calc R . . C20 C 0.9736(5) 0.3586(4) 0.1626(2) 0.0263(8) Uani 1 1 d . . . C21 C 0.8502(5) 0.2934(4) 0.1128(2) 0.0267(9) Uani 1 1 d . . . C22 C 0.8498(5) 0.2790(7) 0.0434(2) 0.0346(9) Uani 1 1 d . . . H22 H 0.9347 0.3129 0.0232 0.041 Uiso 1 1 calc R . . C23 C 0.7194(7) 0.2126(6) 0.0038(2) 0.0402(12) Uani 1 1 d . . . C24 C 0.5932(6) 0.1678(5) 0.0331(2) 0.0343(10) Uani 1 1 d . . . H24 H 0.5041 0.1254 0.0059 0.041 Uiso 1 1 calc R . . C25 C 0.6001(5) 0.1864(5) 0.1027(2) 0.0259(8) Uani 1 1 d . . . C26 C 0.4812(5) 0.1437(4) 0.1448(2) 0.0234(7) Uani 1 1 d . . . C27 C 0.3398(5) 0.0765(5) 0.1177(2) 0.0317(9) Uani 1 1 d . . . H27 H 0.3166 0.0532 0.0704 0.038 Uiso 1 1 calc R . . C28 C 0.2351(6) 0.0445(6) 0.1599(3) 0.0371(11) Uani 1 1 d . . . H28 H 0.1386 -0.0007 0.1421 0.044 Uiso 1 1 calc R . . C29 C 0.2711(5) 0.0788(6) 0.2293(3) 0.0345(10) Uani 1 1 d . . . H29 H 0.1999 0.0580 0.2593 0.041 Uiso 1 1 calc R . . C30 C 0.4144(5) 0.1445(5) 0.2534(2) 0.0262(8) Uani 1 1 d . . . H30 H 0.4394 0.1686 0.3005 0.031 Uiso 1 1 calc R . . O1A O 0.7507(6) 0.2796(8) 0.5475(2) 0.0222(11) Uani 0.50 1 d P . . O1B O 0.7302(8) 0.1942(8) -0.0622(3) 0.0330(14) Uani 0.50 1 d P . . O2 O 0.5556(6) 0.4702(5) 0.5922(2) 0.0553(10) Uani 1 1 d D . . H1W H 0.494(6) 0.411(7) 0.556(2) 0.066 Uiso 1 1 d D . . H2W H 0.651(5) 0.510(8) 0.577(3) 0.066 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 Ru1 0.01696(12) 0.02006(13) 0.02003(12) 0.00013(18) 0.00342(8) -0.00120(15) N1 0.0171(14) 0.0236(17) 0.0260(16) 0.0003(13) 0.0023(12) -0.0032(12) N2 0.0146(11) 0.0215(18) 0.0221(12) 0.0065(18) 0.0001(9) -0.0034(17) N3 0.0147(14) 0.0186(15) 0.0257(16) 0.0018(12) 0.0048(12) -0.0020(11) N4 0.0177(15) 0.0162(15) 0.0361(18) 0.0021(13) 0.0070(13) 0.0018(12) N5 0.0227(13) 0.018(2) 0.0234(13) -0.0035(15) 0.0059(10) 0.0017(15) N6 0.0170(14) 0.0197(16) 0.0257(16) 0.0029(12) 0.0019(12) -0.0015(12) B1 0.054(4) 0.108(7) 0.040(3) -0.027(4) 0.013(3) 0.005(4) B2 0.062(3) 0.043(3) 0.031(2) -0.003(4) 0.013(2) -0.010(4) F5 0.077(2) 0.078(2) 0.0388(17) -0.0112(16) 0.0260(17) -0.015(2) F6 0.093(3) 0.040(2) 0.069(2) -0.0024(18) -0.024(2) -0.0032(19) F7 0.066(2) 0.099(4) 0.0535(18) -0.030(2) 0.0206(16) -0.038(2) F8 0.098(3) 0.061(2) 0.0477(19) 0.0091(16) 0.040(2) -0.003(2) C1 0.0189(17) 0.027(2) 0.031(2) -0.0030(16) 0.0060(15) -0.0015(15) C2 0.029(2) 0.0234(19) 0.044(2) -0.0062(17) 0.0050(19) 0.0016(15) C3 0.033(2) 0.023(3) 0.044(2) 0.0019(16) 0.0005(18) 0.0048(15) C4 0.033(2) 0.0213(19) 0.034(2) 0.0047(16) -0.0028(18) 0.0052(17) C5 0.0193(17) 0.0198(17) 0.0256(18) 0.0003(14) 0.0009(14) 0.0002(14) C6 0.0185(17) 0.0234(18) 0.0238(18) 0.0031(14) 0.0028(14) -0.0012(14) C7 0.026(2) 0.029(2) 0.025(2) 0.0044(16) 0.0016(15) 0.0002(16) C8 0.0278(17) 0.038(3) 0.0194(15) 0.0005(18) 0.0031(13) 0.0003(19) C9 0.029(2) 0.031(2) 0.0235(19) -0.0023(16) 0.0064(16) 0.0012(17) C10 0.0162(17) 0.0254(19) 0.0235(18) 0.0006(14) 0.0035(14) -0.0035(14) C11 0.0158(16) 0.0222(18) 0.0264(19) 0.0008(14) 0.0041(14) -0.0027(13) C12 0.0267(19) 0.027(2) 0.028(2) -0.0030(16) 0.0075(15) -0.0020(16) C13 0.0290(16) 0.0183(17) 0.0422(19) 0.000(3) 0.0080(14) 0.000(2) C14 0.0247(18) 0.024(2) 0.035(2) 0.0079(14) 0.0052(16) 0.0017(13) C15 0.0196(17) 0.0252(19) 0.0250(18) 0.0052(15) 0.0046(14) -0.0022(14) C16 0.0206(19) 0.024(2) 0.043(2) 0.0004(17) 0.0022(17) 0.0016(15) C17 0.019(2) 0.032(2) 0.068(3) 0.004(2) 0.002(2) -0.0039(17) C18 0.023(2) 0.038(3) 0.074(4) 0.008(3) 0.016(3) -0.008(2) C19 0.032(2) 0.031(2) 0.059(3) 0.008(2) 0.025(2) 0.0032(18) C20 0.0252(19) 0.0181(18) 0.039(2) 0.0023(15) 0.0156(17) 0.0023(14) C21 0.0311(18) 0.022(2) 0.0303(18) 0.0016(14) 0.0130(15) 0.0049(14) C22 0.048(2) 0.027(2) 0.0347(19) 0.006(2) 0.0236(17) 0.007(2) C23 0.065(3) 0.036(2) 0.023(2) 0.0016(16) 0.015(2) 0.010(2) C24 0.048(3) 0.031(2) 0.022(2) -0.0016(16) -0.0009(18) 0.004(2) C25 0.0283(19) 0.025(2) 0.0230(19) -0.0011(15) 0.0011(15) 0.0020(16) C26 0.0245(18) 0.0181(17) 0.0259(18) 0.0036(14) -0.0009(14) -0.0014(14) C27 0.029(2) 0.027(2) 0.035(2) 0.0000(17) -0.0072(17) -0.0004(17) C28 0.024(2) 0.032(2) 0.052(3) 0.004(2) -0.004(2) -0.0070(18) C29 0.024(2) 0.029(2) 0.050(3) 0.012(2) 0.008(2) -0.0029(18) C30 0.0234(19) 0.0235(19) 0.032(2) 0.0041(16) 0.0064(16) 0.0020(15) O1A 0.037(2) 0.021(3) 0.0080(17) 0.003(2) 0.0008(16) 0.006(3) O1B 0.049(4) 0.035(3) 0.014(3) -0.004(2) 0.003(2) 0.003(3) O2 0.061(3) 0.055(3) 0.053(2) -0.012(2) 0.020(2) -0.009(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 Ru1 N5 1.981(3) . ? Ru1 N2 1.989(3) . ? Ru1 N4 2.073(3) . ? Ru1 N6 2.077(3) . ? Ru1 N3 2.081(3) . ? Ru1 N1 2.090(4) . ? N1 C1 1.338(5) . ? N1 C5 1.371(5) . ? N2 C10 1.338(7) . ? N2 C6 1.356(6) . ? N3 C15 1.347(5) . ? N3 C11 1.373(5) . ? N4 C16 1.334(6) . ? N4 C20 1.379(6) . ? N5 C25 1.354(5) . ? N5 C21 1.361(5) . ? N6 C30 1.343(5) . ? N6 C26 1.361(5) . ? B1 F1 1.313(8) . ? B1 F3 1.314(8) . ? B1 F2 1.355(8) . ? B1 F4 1.477(10) . ? B2 F8 1.372(6) . ? B2 F6 1.374(9) . ? B2 F5 1.379(7) . ? B2 F7 1.402(6) . ? C1 C2 1.393(6) . ? C2 C3 1.388(7) . ? C3 C4 1.391(6) . ? C4 C5 1.388(6) . ? C5 C6 1.479(5) . ? C6 C7 1.386(6) . ? C7 C8 1.394(7) . ? C8 O1A 1.331(6) . ? C8 C9 1.408(7) . ? C9 C10 1.388(5) . ? C10 C11 1.477(5) . ? C11 C12 1.388(6) . ? C12 C13 1.374(7) . ? C13 C14 1.382(6) . ? C14 C15 1.392(6) . ? C16 C17 1.397(6) . ? C17 C18 1.383(9) . ? C18 C19 1.389(9) . ? C19 C20 1.397(6) . ? C20 C21 1.459(6) . ? C21 C22 1.385(6) . ? C22 C23 1.405(8) . ? C23 O1B 1.339(7) . ? C23 C24 1.391(7) . ? C24 C25 1.384(6) . ? C25 C26 1.489(6) . ? C26 C27 1.400(6) . ? C27 C28 1.372(8) . ? C28 C29 1.395(8) . ? C29 C30 1.395(6) . ? 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 N5 Ru1 N2 178.4(3) . . ? N5 Ru1 N4 79.24(14) . . ? N2 Ru1 N4 101.83(14) . . ? N5 Ru1 N6 78.67(14) . . ? N2 Ru1 N6 100.29(13) . . ? N4 Ru1 N6 157.85(14) . . ? N5 Ru1 N3 102.51(16) . . ? N2 Ru1 N3 78.72(19) . . ? N4 Ru1 N3 90.21(13) . . ? N6 Ru1 N3 93.02(13) . . ? N5 Ru1 N1 99.93(16) . . ? N2 Ru1 N1 78.86(19) . . ? N4 Ru1 N1 92.57(13) . . ? N6 Ru1 N1 92.76(13) . . ? N3 Ru1 N1 157.51(13) . . ? C1 N1 C5 119.0(4) . . ? C1 N1 Ru1 127.4(3) . . ? C5 N1 Ru1 113.6(3) . . ? C10 N2 C6 121.1(3) . . ? C10 N2 Ru1 119.4(3) . . ? C6 N2 Ru1 119.4(4) . . ? C15 N3 C11 118.7(3) . . ? C15 N3 Ru1 127.7(3) . . ? C11 N3 Ru1 113.6(3) . . ? C16 N4 C20 119.3(4) . . ? C16 N4 Ru1 127.3(3) . . ? C20 N4 Ru1 113.3(3) . . ? C25 N5 C21 121.2(3) . . ? C25 N5 Ru1 119.9(3) . . ? C21 N5 Ru1 118.8(3) . . ? C30 N6 C26 118.7(3) . . ? C30 N6 Ru1 127.1(3) . . ? C26 N6 Ru1 114.2(3) . . ? F1 B1 F3 121.6(6) . . ? F1 B1 F2 114.4(5) . . ? F3 B1 F2 116.4(7) . . ? F1 B1 F4 100.6(7) . . ? F3 B1 F4 98.0(6) . . ? F2 B1 F4 99.3(6) . . ? F8 B2 F6 109.3(5) . . ? F8 B2 F5 109.3(6) . . ? F6 B2 F5 107.0(5) . . ? F8 B2 F7 110.2(5) . . ? F6 B2 F7 109.9(6) . . ? F5 B2 F7 111.0(5) . . ? N1 C1 C2 122.4(4) . . ? C3 C2 C1 118.8(4) . . ? C2 C3 C4 119.3(4) . . ? C5 C4 C3 119.3(4) . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 115.6(3) . . ? C4 C5 C6 123.1(4) . . ? N2 C6 C7 120.9(4) . . ? N2 C6 C5 112.5(4) . . ? C7 C6 C5 126.6(4) . . ? C6 C7 C8 118.6(4) . . ? O1A C8 C7 115.9(5) . . ? O1A C8 C9 124.2(5) . . ? C7 C8 C9 119.9(4) . . ? C10 C9 C8 118.2(4) . . ? N2 C10 C9 121.3(4) . . ? N2 C10 C11 112.9(3) . . ? C9 C10 C11 125.8(4) . . ? N3 C11 C12 120.9(4) . . ? N3 C11 C10 115.2(3) . . ? C12 C11 C10 123.9(4) . . ? C13 C12 C11 120.0(4) . . ? C12 C13 C14 119.2(5) . . ? C13 C14 C15 119.3(4) . . ? N3 C15 C14 121.8(4) . . ? N4 C16 C17 121.7(5) . . ? C18 C17 C16 119.4(5) . . ? C17 C18 C19 119.6(4) . . ? C18 C19 C20 118.9(5) . . ? N4 C20 C19 121.0(4) . . ? N4 C20 C21 115.7(3) . . ? C19 C20 C21 123.2(4) . . ? N5 C21 C22 121.0(4) . . ? N5 C21 C20 112.8(3) . . ? C22 C21 C20 126.2(4) . . ? C21 C22 C23 117.6(4) . . ? O1B C23 C24 124.4(6) . . ? O1B C23 C22 114.6(5) . . ? C24 C23 C22 121.0(4) . . ? C25 C24 C23 118.5(4) . . ? N5 C25 C24 120.6(4) . . ? N5 C25 C26 111.7(3) . . ? C24 C25 C26 127.7(4) . . ? N6 C26 C27 121.3(4) . . ? N6 C26 C25 115.4(3) . . ? C27 C26 C25 123.3(4) . . ? C28 C27 C26 119.4(4) . . ? C27 C28 C29 119.6(4) . . ? C28 C29 C30 118.3(4) . . ? N6 C30 C29 122.6(4) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.243 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.100 data_crystal_2b _database_code_depnum_ccdc_archive 'CCDC 261249' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H22 N6 O2 Ru 2+,2(B F4 1-),H2 O' _chemical_formula_sum 'C30 H24 B2 F8 N6 O3 Ru' _chemical_formula_iupac ? _chemical_formula_weight 791.2 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.737(2) _cell_length_b 9.345(3) _cell_length_c 20.224(5) _cell_angle_alpha 78.64(2) _cell_angle_beta 78.32(2) _cell_angle_gamma 87.73(2) _cell_volume 1585.4(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.66 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792.0 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.91 # 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 5735 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5563 _reflns_number_gt 4866 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.067 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4866 _refine_ls_number_parameters 148 _refine_ls_goodness_of_fit_ref 1.80 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.013 _refine_diff_density_max 1.01 _refine_diff_density_min -1.08 _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 Ru 0.49788(3) 0.64281(3) 0.24479(1) 0.0312(1) Uani Ru 1.0 O1A 0.7339(4) 0.7849(4) -0.0637(1) 0.072(1) Uani O 1.0 N1A 0.7169(2) 0.7234(3) 0.2397(1) 0.0366(4) Uani N 1.0 N2A 0.5777(2) 0.6834(2) 0.1441(1) 0.0324(4) Uani N 1.0 N3A 0.3122(3) 0.5735(3) 0.2094(1) 0.0365(4) Uani N 1.0 C1A 0.7809(3) 0.7436(3) 0.2927(1) 0.0466(4) Uani C 1.0 C2A 0.9256(4) 0.8074(4) 0.2827(2) 0.0546(5) Uani C 1.0 C3A 1.0082(3) 0.8520(3) 0.2168(2) 0.0525(5) Uani C 1.0 C4A 0.9450(3) 0.8325(3) 0.1619(1) 0.0446(4) Uani C 1.0 C5A 0.7992(3) 0.7679(3) 0.1744(1) 0.0364(4) Uani C 1.0 C6A 0.7210(3) 0.7431(3) 0.1195(1) 0.0355(4) Uani C 1.0 C7A 0.7790(3) 0.7793(3) 0.0496(1) 0.0453(6) Uani C 1.0 C8A 0.6860(3) 0.7527(2) 0.0050(2) 0.0528(7) Uani C 1.0 C9A 0.5382(3) 0.6911(3) 0.0307(1) 0.0482(6) Uani C 1.0 C10A 0.4869(3) 0.6573(3) 0.1012(1) 0.0373(5) Uani C 1.0 C11A 0.3345(3) 0.5908(3) 0.1397(1) 0.0384(5) Uani C 1.0 C12A 0.2242(4) 0.5436(4) 0.1082(1) 0.0487(5) Uani C 1.0 C13A 0.0889(3) 0.4778(4) 0.1484(2) 0.0549(6) Uani C 1.0 C14A 0.0661(3) 0.4602(3) 0.2186(2) 0.0529(7) Uani C 1.0 C15A 0.1790(3) 0.5088(3) 0.2478(1) 0.0446(6) Uani C 1.0 O1B 0.2314(4) 0.5257(3) 0.5512(1) 0.066(1) Uani O 1.0 N1B 0.4016(3) 0.8448(2) 0.2563(1) 0.0339(5) Uani N 1.0 N2B 0.4137(3) 0.6076(2) 0.3453(1) 0.0328(5) Uani N 1.0 N3B 0.5666(3) 0.4290(2) 0.2740(1) 0.0366(5) Uani N 1.0 C1B 0.4059(3) 0.9674(3) 0.2076(1) 0.0403(5) Uani C 1.0 C2B 0.3388(4) 1.0965(3) 0.2223(2) 0.0464(5) Uani C 1.0 C3B 0.2652(4) 1.1016(3) 0.2885(2) 0.0463(5) Uani C 1.0 C4B 0.2594(3) 0.9777(3) 0.3391(1) 0.0412(5) Uani C 1.0 C5B 0.3284(3) 0.8503(3) 0.3220(1) 0.0348(4) Uani C 1.0 C6B 0.3330(3) 0.7143(3) 0.3734(1) 0.0352(5) Uani C 1.0 C7B 0.2691(3) 0.6917(3) 0.4429(1) 0.0436(6) Uani C 1.0 C8B 0.2899(3) 0.5561(2) 0.4833(2) 0.0500(7) Uani C 1.0 C9B 0.3734(3) 0.4467(3) 0.4538(1) 0.0465(6) Uani C 1.0 C10B 0.4344(3) 0.4760(3) 0.3840(1) 0.0376(5) Uani C 1.0 C11B 0.5234(3) 0.3739(3) 0.3427(1) 0.0389(5) Uani C 1.0 C12B 0.5612(4) 0.2324(3) 0.3706(1) 0.0481(7) Uani C 1.0 C13B 0.6442(4) 0.1456(3) 0.3279(2) 0.0537(9) Uani C 1.0 C14B 0.6879(4) 0.2006(3) 0.2587(2) 0.0515(9) Uani C 1.0 C15B 0.6478(3) 0.3421(3) 0.2332(1) 0.0434(7) Uani C 1.0 OW 0.0230(5) 0.7113(4) 0.6013(2) 0.072(1) Uani O 1.0 B1A 0.81891(21) 0.20308(22) 0.06753(8) 0.063(1) Uani B 1.0 F1A 0.8470(3) 0.1656(3) 0.0044(1) 0.082(1) Uani F 1.0 F2A 0.6963(3) 0.1236(4) 0.1090(1) 0.107(2) Uani F 1.0 F3A 0.9485(3) 0.1752(3) 0.0959(1) 0.089(1) Uani F 1.0 F4A 0.7839(4) 0.3480(3) 0.0609(2) 0.122(3) Uani F 1.0 B1B 0.7912(5) 0.9118(5) 0.4726(2) 0.062(3) Uani B 0.55 F1B 0.6813(8) 0.8548(8) 0.4460(3) 0.083(3) Uani F 0.55 F2B 0.7525(10) 1.0520(5) 0.4786(4) 0.139(4) Uani F 0.55 F3B 0.7978(8) 0.8305(6) 0.5358(2) 0.098(3) Uani F 0.55 F4B 0.9334(6) 0.9097(9) 0.4299(3) 0.129(4) Uani F 0.55 B1B' 0.8131(6) 0.9083(6) 0.4565(2) 0.063(3) Uani B 0.45 F1B' 0.6880(9) 0.8605(10) 0.4362(4) 0.083(3) Uani F 0.45 F2B' 0.9111(10) 0.7943(8) 0.4706(5) 0.129(2) Uani F 0.45 F3B' 0.8906(10) 1.0129(9) 0.4053(3) 0.127(5) Uani F 0.45 F4B' 0.7626(11) 0.9656(9) 0.5141(3) 0.114(3) Uani F 0.45 HO1A 0.8498 0.7994 -0.0754 0.078 Uani H 1.0 HC1A 0.7213 0.7112 0.3408 0.053 Uani H 1.0 HC2A 0.9699 0.8209 0.3229 0.067 Uani H 1.0 HC3A 1.1132 0.8985 0.2087 0.062 Uani H 1.0 HC4A 1.0039 0.8645 0.1137 0.050 Uani H 1.0 HC7A 0.8852 0.8236 0.0314 0.052 Uani H 1.0 HC9A 0.4708 0.6717 -0.0011 0.058 Uani H 1.0 HC12A 0.2423 0.5570 0.0569 0.057 Uani H 1.0 HC13A 0.0082 0.4431 0.1264 0.066 Uani H 1.0 HC14A -0.0313 0.4128 0.2484 0.063 Uani H 1.0 HC15A 0.1617 0.4958 0.2991 0.050 Uani H 1.0 HO1B 0.1529 0.5956 0.5701 0.072 Uani H 1.0 HC1B 0.4594 0.9643 0.1592 0.045 Uani H 1.0 HC2B 0.3439 1.1854 0.1852 0.055 Uani H 1.0 HC3B 0.2160 1.1944 0.3000 0.054 Uani H 1.0 HC4B 0.2061 0.9799 0.3876 0.046 Uani H 1.0 HC7B 0.2093 0.7707 0.4638 0.049 Uani H 1.0 HC9B 0.3887 0.3491 0.4825 0.054 Uani H 1.0 HC12B 0.5286 0.1937 0.4211 0.054 Uani H 1.0 HC13B 0.6723 0.0433 0.3472 0.063 Uani H 1.0 HC14B 0.7480 0.1390 0.2272 0.060 Uani H 1.0 HC15B 0.6800 0.3816 0.1827 0.047 Uani H 1.0 H1OW -0.0673 0.7343 0.5775 0.072 Uani H 1.0 H2OW 0.0724 0.8043 0.6039 0.072 Uani H 1.0 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 Ru 0.0299(2) 0.0384(2) 0.0242(2) -0.0019(1) -0.0032(1) -0.0057(1) Ru O1A 0.069(2) 0.115(3) 0.0270(6) -0.010(2) 0.0002(6) -0.0058(9) O N1A 0.0370(6) 0.0424(8) 0.0320(7) -0.0015(5) -0.0079(4) -0.0092(6) N N2A 0.0342(6) 0.0360(9) 0.0264(7) -0.0008(5) -0.0041(4) -0.0064(5) N N3A 0.0343(6) 0.0390(8) 0.0351(6) -0.0030(5) -0.0045(4) -0.0066(5) N C1A 0.0455(7) 0.060(1) 0.0389(7) -0.0029(6) -0.0142(6) -0.0150(8) C C2A 0.0481(8) 0.069(1) 0.0552(9) -0.0055(8) -0.0201(7) -0.021(1) C C3A 0.0412(7) 0.058(1) 0.063(1) -0.0076(7) -0.0151(7) -0.0164(9) C C4A 0.0361(6) 0.0474(9) 0.0497(8) -0.0063(5) -0.0066(5) -0.0088(6) C C5A 0.0343(6) 0.0392(7) 0.0355(6) -0.0027(5) -0.0054(4) -0.0073(5) C C6A 0.0351(6) 0.0402(9) 0.0291(6) -0.0023(5) -0.0024(4) -0.0053(5) C C7A 0.0423(7) 0.058(1) 0.0303(6) -0.0053(6) 0.0008(5) -0.0036(6) C C8A 0.0519(9) 0.076(2) 0.0267(6) -0.0057(8) -0.0018(5) -0.0062(7) C C9A 0.0494(8) 0.068(1) 0.0279(6) -0.0033(6) -0.0077(5) -0.0106(6) C C10A 0.0388(6) 0.0455(8) 0.0285(6) -0.0014(5) -0.0068(4) -0.0090(5) C C11A 0.0373(5) 0.0436(7) 0.0363(6) -0.0023(5) -0.0089(4) -0.0106(4) C C12A 0.0439(6) 0.059(1) 0.0497(7) -0.0047(6) -0.0158(6) -0.0176(7) C C13A 0.0429(7) 0.061(1) 0.067(1) -0.0087(7) -0.0165(7) -0.018(1) C C14A 0.0385(6) 0.055(1) 0.064(1) -0.0104(7) -0.0077(6) -0.010(1) C C15A 0.0364(6) 0.048(1) 0.0463(7) -0.0071(6) -0.0027(5) -0.0052(7) C O1B 0.087(2) 0.072(1) 0.0274(8) 0.012(1) 0.0035(6) -0.0018(5) O N1B 0.0316(7) 0.0378(5) 0.0302(6) -0.0042(5) -0.0028(5) -0.0044(4) N N2B 0.0304(7) 0.0395(5) 0.0271(6) -0.0027(5) -0.0031(5) -0.0050(4) N N3B 0.0343(7) 0.0416(6) 0.0331(5) 0.0013(5) -0.0047(5) -0.0076(4) N C1B 0.0430(8) 0.0390(5) 0.0350(6) -0.0038(5) -0.0031(6) -0.0017(5) C C2B 0.055(1) 0.0385(6) 0.0433(7) -0.0006(5) -0.0080(7) -0.0033(5) C C3B 0.054(1) 0.0404(6) 0.0451(8) 0.0039(6) -0.0110(7) -0.0100(5) C C4B 0.0444(9) 0.0428(5) 0.0374(6) 0.0034(6) -0.0076(5) -0.0114(5) C C5B 0.0334(7) 0.0396(5) 0.0308(6) -0.0015(5) -0.0043(4) -0.0074(4) C C6B 0.0343(7) 0.0424(5) 0.0276(6) -0.0009(4) -0.0028(5) -0.0067(4) C C7B 0.048(1) 0.0517(7) 0.0277(7) 0.0041(6) -0.0013(5) -0.0077(4) C C8B 0.061(1) 0.0563(8) 0.0269(7) 0.0055(8) -0.0002(5) -0.0034(4) C C9B 0.056(1) 0.0493(7) 0.0287(7) 0.0029(6) -0.0032(5) -0.0008(5) C C10B 0.0396(7) 0.0418(6) 0.0289(6) -0.0004(5) -0.0044(5) -0.0033(4) C C11B 0.0409(7) 0.0407(6) 0.0338(6) 0.0017(5) -0.0070(4) -0.0049(4) C C12B 0.058(1) 0.0431(7) 0.0417(8) 0.0070(7) -0.0118(7) -0.0041(5) C C13B 0.065(2) 0.0456(8) 0.051(1) 0.0133(8) -0.016(1) -0.0094(6) C C14B 0.057(1) 0.0496(8) 0.049(1) 0.0144(9) -0.0122(9) -0.0148(7) C C15B 0.0432(8) 0.0477(8) 0.0394(7) 0.0077(6) -0.0060(6) -0.0121(5) C OW 0.080(3) 0.067(2) 0.058(2) 0.011(2) 0.005(2) -0.006(2) O B1A 0.054(2) 0.081(2) 0.048(1) -0.002(1) 0.005(1) -0.014(1) B F1A 0.088(2) 0.103(2) 0.049(1) -0.012(2) 0.007(1) -0.020(1) F F2A 0.072(3) 0.176(3) 0.060(2) -0.043(2) 0.013(2) -0.011(2) F F3A 0.066(2) 0.122(2) 0.073(2) -0.012(2) -0.013(2) -0.007(2) F F4A 0.187(4) 0.090(2) 0.104(3) 0.033(2) -0.056(3) -0.033(1) F B1B 0.074(4) 0.064(3) 0.052(3) -0.007(3) -0.019(3) -0.008(2) B F1B 0.095(4) 0.083(3) 0.072(3) -0.028(3) -0.041(3) 0.011(2) F F2B 0.236(8) 0.078(5) 0.133(5) 0.029(3) -0.087(6) -0.045(3) F F3B 0.134(5) 0.099(4) 0.065(3) -0.047(3) -0.048(2) 0.013(2) F F4B 0.070(4) 0.193(6) 0.103(4) -0.007(2) -0.004(5) 0.007(4) F B1B' 0.068(4) 0.070(3) 0.053(3) -0.007(3) -0.017(3) -0.006(2) B F1B' 0.104(4) 0.078(3) 0.071(3) -0.028(3) -0.044(3) 0.009(2) F F2B' 0.107(6) 0.129(4) 0.151(5) 0.044(4) -0.045(5) -0.019(3) F F3B' 0.118(5) 0.167(6) 0.083(5) -0.073(5) -0.043(5) 0.042(4) F F4B' 0.182(5) 0.101(5) 0.073(3) 0.004(3) -0.038(4) -0.038(3) F # 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 Ru N1A 2.060(2) 1_555 1_555 no Ru N2A 1.980(2) 1_555 1_555 no Ru N3A 2.073(2) 1_555 1_555 no Ru N1B 2.072(2) 1_555 1_555 no Ru N2B 1.982(2) 1_555 1_555 no Ru N3B 2.070(2) 1_555 1_555 no O1A C8A 1.343(4) 1_555 1_555 no N1A C1A 1.352(2) 1_555 1_555 no N1A C5A 1.363(3) 1_555 1_555 no N2A C6A 1.349(2) 1_555 1_555 no N2A C10A 1.349(2) 1_555 1_555 no N3A C11A 1.363(3) 1_555 1_555 no N3A C15A 1.352(2) 1_555 1_555 no C1A C2A 1.380(3) 1_555 1_555 no C2A C3A 1.372(3) 1_555 1_555 no C3A C4A 1.381(3) 1_555 1_555 no C4A C5A 1.387(3) 1_555 1_555 no C5A C6A 1.474(3) 1_555 1_555 no C6A C7A 1.381(3) 1_555 1_555 no C7A C8A 1.392(3) 1_555 1_555 no C8A C9A 1.392(3) 1_555 1_555 no C9A C10A 1.381(3) 1_555 1_555 no C10A C11A 1.490(3) 1_555 1_555 no C11A C12A 1.387(3) 1_555 1_555 no C12A C13A 1.381(3) 1_555 1_555 no C13A C14A 1.372(3) 1_555 1_555 no C14A C15A 1.380(3) 1_555 1_555 no O1B C8B 1.343(4) 1_555 1_555 no N1B C1B 1.352(2) 1_555 1_555 no N1B C5B 1.363(3) 1_555 1_555 no N2B C6B 1.349(2) 1_555 1_555 no N2B C10B 1.349(2) 1_555 1_555 no N3B C11B 1.363(3) 1_555 1_555 no N3B C15B 1.352(2) 1_555 1_555 no C1B C2B 1.380(3) 1_555 1_555 no C2B C3B 1.372(3) 1_555 1_555 no C3B C4B 1.381(3) 1_555 1_555 no C4B C5B 1.387(3) 1_555 1_555 no C5B C6B 1.480(3) 1_555 1_555 no C6B C7B 1.381(3) 1_555 1_555 no C7B C8B 1.392(3) 1_555 1_555 no C8B C9B 1.392(3) 1_555 1_555 no C9B C10B 1.381(3) 1_555 1_555 no C10B C11B 1.485(3) 1_555 1_555 no C11B C12B 1.387(3) 1_555 1_555 no C12B C13B 1.381(3) 1_555 1_555 no C13B C14B 1.372(3) 1_555 1_555 no C14B C15B 1.380(3) 1_555 1_555 no B1A F1A 1.363(1) 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 N1A Ru N2A 79.19(9) 1_555 1_555 1_555 no N1A Ru N3A 157.8(1) 1_555 1_555 1_555 no N1A Ru N1B 89.9(1) 1_555 1_555 1_555 no N1A Ru N2B 101.29(9) 1_555 1_555 1_555 no N1A Ru N3B 92.8(1) 1_555 1_555 1_555 no N2A Ru N3A 78.60(9) 1_555 1_555 1_555 no N2A Ru N1B 99.32(9) 1_555 1_555 1_555 no N2A Ru N2B 178.20(8) 1_555 1_555 1_555 no N2A Ru N3B 102.80(9) 1_555 1_555 1_555 no N3A Ru N1B 95.0(1) 1_555 1_555 1_555 no N3A Ru N2B 100.95(9) 1_555 1_555 1_555 no N3A Ru N3B 90.9(1) 1_555 1_555 1_555 no N1B Ru N2B 78.96(9) 1_555 1_555 1_555 no N1B Ru N3B 157.8(1) 1_555 1_555 1_555 no N2B Ru N3B 78.94(9) 1_555 1_555 1_555 no Ru N1A C1A 127.4(2) 1_555 1_555 1_555 no Ru N1A C5A 114.1(2) 1_555 1_555 1_555 no C1A N1A C5A 118.4(1) 1_555 1_555 1_555 no Ru N2A C6A 118.7(2) 1_555 1_555 1_555 no Ru N2A C10A 120.1(2) 1_555 1_555 1_555 no C6A N2A C10A 121.1(2) 1_555 1_555 1_555 no Ru N3A C11A 114.4(2) 1_555 1_555 1_555 no Ru N3A C15A 127.2(2) 1_555 1_555 1_555 no C11A N3A C15A 118.4(1) 1_555 1_555 1_555 no N1A C1A C2A 122.2(2) 1_555 1_555 1_555 no C1A C2A C3A 119.3(2) 1_555 1_555 1_555 no C2A C3A C4A 119.5(2) 1_555 1_555 1_555 no C3A C4A C5A 119.3(2) 1_555 1_555 1_555 no N1A C5A C4A 121.3(2) 1_555 1_555 1_555 no N1A C5A C6A 115.1(2) 1_555 1_555 1_555 no C4A C5A C6A 123.6(2) 1_555 1_555 1_555 no N2A C6A C5A 112.9(2) 1_555 1_555 1_555 no N2A C6A C7A 120.8(2) 1_555 1_555 1_555 no C5A C6A C7A 126.3(2) 1_555 1_555 1_555 no C6A C7A C8A 118.4(2) 1_555 1_555 1_555 no O1A C8A C7A 122.0(2) 1_555 1_555 1_555 no O1A C8A C9A 117.6(2) 1_555 1_555 1_555 no C7A C8A C9A 120.4(3) 1_555 1_555 1_555 no C8A C9A C10A 118.4(2) 1_555 1_555 1_555 no N2A C10A C9A 120.8(2) 1_555 1_555 1_555 no N2A C10A C11A 111.7(2) 1_555 1_555 1_555 no C9A C10A C11A 127.5(2) 1_555 1_555 1_555 no N3A C11A C10A 115.2(2) 1_555 1_555 1_555 no N3A C11A C12A 121.3(2) 1_555 1_555 1_555 no C10A C11A C12A 123.4(2) 1_555 1_555 1_555 no C11A C12A C13A 119.3(2) 1_555 1_555 1_555 no C12A C13A C14A 119.5(2) 1_555 1_555 1_555 no C13A C14A C15A 119.3(2) 1_555 1_555 1_555 no N3A C15A C14A 122.2(2) 1_555 1_555 1_555 no Ru N1B C1B 127.9(2) 1_555 1_555 1_555 no Ru N1B C5B 113.7(2) 1_555 1_555 1_555 no C1B N1B C5B 118.4(1) 1_555 1_555 1_555 no Ru N2B C6B 119.5(2) 1_555 1_555 1_555 no Ru N2B C10B 119.4(2) 1_555 1_555 1_555 no C6B N2B C10B 121.1(2) 1_555 1_555 1_555 no Ru N3B C11B 114.2(2) 1_555 1_555 1_555 no Ru N3B C15B 127.4(2) 1_555 1_555 1_555 no C11B N3B C15B 118.4(1) 1_555 1_555 1_555 no N1B C1B C2B 122.2(2) 1_555 1_555 1_555 no C1B C2B C3B 119.3(2) 1_555 1_555 1_555 no C2B C3B C4B 119.5(2) 1_555 1_555 1_555 no C3B C4B C5B 119.3(2) 1_555 1_555 1_555 no N1B C5B C4B 121.3(2) 1_555 1_555 1_555 no N1B C5B C6B 115.8(2) 1_555 1_555 1_555 no C4B C5B C6B 122.8(2) 1_555 1_555 1_555 no N2B C6B C5B 112.0(2) 1_555 1_555 1_555 no N2B C6B C7B 120.8(2) 1_555 1_555 1_555 no C5B C6B C7B 127.2(2) 1_555 1_555 1_555 no C6B C7B C8B 118.4(2) 1_555 1_555 1_555 no O1B C8B C7B 122.0(2) 1_555 1_555 1_555 no O1B C8B C9B 117.6(2) 1_555 1_555 1_555 no C7B C8B C9B 120.4(3) 1_555 1_555 1_555 no C8B C9B C10B 118.4(2) 1_555 1_555 1_555 no N2B C10B C9B 120.8(2) 1_555 1_555 1_555 no N2B C10B C11B 112.4(2) 1_555 1_555 1_555 no C9B C10B C11B 126.8(2) 1_555 1_555 1_555 no N3B C11B C10B 115.1(2) 1_555 1_555 1_555 no N3B C11B C12B 121.3(2) 1_555 1_555 1_555 no C10B C11B C12B 123.5(2) 1_555 1_555 1_555 no C11B C12B C13B 119.3(2) 1_555 1_555 1_555 no C12B C13B C14B 119.5(2) 1_555 1_555 1_555 no C13B C14B C15B 119.3(2) 1_555 1_555 1_555 no N3B C15B C14B 122.2(2) 1_555 1_555 1_555 no F1A B1A F2A 109.47 1_555 1_555 1_555 no data_crystal_3a _database_code_depnum_ccdc_archive 'CCDC 261250' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H22 Cu N6 O2 2+,2(B F4 1-),H2 O' _chemical_formula_sum 'C30 H24 B2 Cu F8 N6 O3' _chemical_formula_iupac ? _chemical_formula_weight 753.7 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 8.806(2) _cell_length_b 9.047(1) _cell_length_c 20.163(4) _cell_angle_alpha 90 _cell_angle_beta 98.38(1) _cell_angle_gamma 90 _cell_volume 1589.2(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour blue-green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762.0 _exptl_absorpt_coefficient_mu 0.774 _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 3058 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 2972 _reflns_number_gt 2217 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.068 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2217 _refine_ls_number_parameters 155 _refine_ls_goodness_of_fit_ref 1.27 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.56 _refine_diff_density_min -0.66 _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 Cu 0.26388(8) 0.76850 0.75888(4) 0.0402(3) Uani Cu 1.0 O1A 0.2821(8) 0.7052(8) 1.0587(2) 0.094(3) Uani O 1.0 N1A 0.0457(5) 0.8564(6) 0.7739(2) 0.045(1) Uani N 1.0 N2A 0.2741(4) 0.7552(5) 0.8561(2) 0.040(1) Uani N 1.0 N3A 0.4906(4) 0.6778(5) 0.7893(2) 0.043(1) Uani N 1.0 C1A -0.0644(6) 0.9109(7) 0.7279(3) 0.057(2) Uani C 1.0 C2A -0.1964(6) 0.9726(8) 0.7432(4) 0.072(2) Uani C 1.0 C3A -0.2167(7) 0.9788(8) 0.8089(4) 0.076(2) Uani C 1.0 C4A -0.1048(7) 0.9233(8) 0.8578(3) 0.065(2) Uani C 1.0 C5A 0.0259(6) 0.8624(7) 0.8388(3) 0.050(1) Uani C 1.0 C6A 0.1513(6) 0.7980(6) 0.8843(2) 0.047(1) Uani C 1.0 C7A 0.1488(6) 0.7833(7) 0.9524(3) 0.062(2) Uani C 1.0 C8A 0.2765(6) 0.7229(5) 0.9919(3) 0.069(2) Uani C 1.0 C9A 0.4030(7) 0.6789(6) 0.9627(2) 0.061(2) Uani C 1.0 C10A 0.3980(6) 0.6967(6) 0.8943(2) 0.046(1) Uani C 1.0 C11A 0.5217(6) 0.6501(6) 0.8554(3) 0.047(1) Uani C 1.0 C12A 0.6587(7) 0.5862(7) 0.8830(3) 0.062(2) Uani C 1.0 C13A 0.7650(7) 0.5504(8) 0.8415(4) 0.071(2) Uani C 1.0 C14A 0.7332(6) 0.5785(8) 0.7745(4) 0.067(2) Uani C 1.0 C15A 0.5955(6) 0.6420(6) 0.7505(3) 0.053(1) Uani C 1.0 O1B 0.2505(6) 0.7889(8) 0.4568(2) 0.074(2) Uani O 1.0 N1B 0.1660(5) 0.5513(5) 0.7259(2) 0.044(1) Uani N 1.0 N2B 0.2541(4) 0.7802(5) 0.6604(2) 0.0380(9) Uani N 1.0 N3B 0.3514(5) 0.9942(5) 0.7439(2) 0.0416(9) Uani N 1.0 C1B 0.1201(6) 0.4415(6) 0.7624(2) 0.053(1) Uani C 1.0 C2B 0.0519(7) 0.3156(6) 0.7352(3) 0.065(2) Uani C 1.0 C3B 0.0297(7) 0.3015(6) 0.6671(3) 0.068(2) Uani C 1.0 C4B 0.0760(7) 0.4133(7) 0.6278(3) 0.059(1) Uani C 1.0 C5B 0.1442(6) 0.5377(6) 0.6587(3) 0.0463(9) Uani C 1.0 C6B 0.1989(5) 0.6644(6) 0.6221(2) 0.0432(8) Uani C 1.0 C7B 0.1967(5) 0.6652(6) 0.5534(2) 0.0528(9) Uani C 1.0 C8B 0.2530(4) 0.7889(5) 0.5239(3) 0.057(1) Uani C 1.0 C9B 0.3099(5) 0.9082(6) 0.5636(3) 0.0503(9) Uani C 1.0 C10B 0.3088(5) 0.9003(6) 0.6320(2) 0.0411(8) Uani C 1.0 C11B 0.3632(6) 1.0202(6) 0.6792(2) 0.0426(8) Uani C 1.0 C12B 0.4204(6) 1.1525(6) 0.6593(3) 0.0523(9) Uani C 1.0 C13B 0.4659(6) 1.2592(7) 0.7072(3) 0.061(1) Uani C 1.0 C14B 0.4537(7) 1.2325(6) 0.7727(3) 0.060(1) Uani C 1.0 C15B 0.3962(6) 1.0993(6) 0.7890(2) 0.051(1) Uani C 1.0 OW 0.4397(9) 0.9867(9) 0.4162(3) 0.090(2) Uani O 1.0 B1A 0.8219(11) 0.7679(10) 0.0618(4) 0.083(5) Uani B 0.53 F1A 0.9702(13) 0.7856(17) 0.0894(7) 0.103(4) Uani F 0.53 F2A 0.8013(17) 0.8214(18) -0.0014(5) 0.141(6) Uani F 0.53 F3A 0.7303(17) 0.8421(17) 0.0987(6) 0.139(9) Uani F 0.53 F4A 0.7857(16) 0.6226(12) 0.0607(8) 0.147(6) Uani F 0.53 B1A' 0.8742(13) 0.7537(12) 0.0635(4) 0.077(5) Uani B 0.47 F2A' 0.8748(19) 0.6421(17) 0.0190(7) 0.125(6) Uani F 0.47 F1A' 1.0148(16) 0.7656(25) 0.1004(8) 0.121(3) Uani F 0.47 F3A' 0.7690(20) 0.7254(18) 0.1044(7) 0.124(6) Uani F 0.47 F4A' 0.8384(24) 0.8817(16) 0.0303(8) 0.135(7) Uani F 0.47 B1B 0.7362(13) 0.8325(14) 0.5531(5) 0.097(8) Uani B 0.52 F1B 0.6731(21) 0.7661(21) 0.4956(7) 0.160(9) Uani F 0.52 F2B 0.8848(13) 0.8648(20) 0.5498(11) 0.125(9) Uani F 0.52 F3B 0.7281(27) 0.7405(20) 0.6054(7) 0.198(9) Uani F 0.52 F4B 0.6589(16) 0.9585(17) 0.5618(10) 0.184(9) Uani F 0.52 B1B' 0.7563(13) 0.8070(14) 0.5510(6) 0.099(9) Uani B 0.48 F2B' 0.8169(21) 0.6739(16) 0.5393(12) 0.207(9) Uani F 0.48 F1B' 0.8708(17) 0.9055(18) 0.5682(9) 0.104(8) Uani F 0.48 F3B' 0.6717(24) 0.7947(29) 0.6016(9) 0.199(9) Uani F 0.48 F4B' 0.6659(20) 0.8540(21) 0.4950(8) 0.168(9) Uani F 0.48 HC1A -0.0493 0.9063 0.6797 0.061 Uani H 1.0 HC2A -0.2761 1.0122 0.7072 0.086 Uani H 1.0 HC3A -0.3122 1.0233 0.8217 0.093 Uani H 1.0 HC4A -0.1184 0.9272 0.9061 0.075 Uani H 1.0 HC7A 0.0572 0.8153 0.9727 0.074 Uani H 1.0 HC9A 0.4955 0.6353 0.9905 0.072 Uani H 1.0 HC12A 0.6807 0.5661 0.9323 0.072 Uani H 1.0 HC13A 0.8650 0.5040 0.8605 0.087 Uani H 1.0 HC14A 0.8088 0.5533 0.7437 0.080 Uani H 1.0 HC15A 0.5721 0.6627 0.7013 0.057 Uani H 1.0 HO1B 0.3088 0.8809 0.4494 0.077 Uani H 1.0 HC1B 0.1364 0.4520 0.8123 0.057 Uani H 1.0 HC2B 0.0191 0.2358 0.7643 0.076 Uani H 1.0 HC3B -0.0200 0.2106 0.6457 0.081 Uani H 1.0 HC4B 0.0603 0.4043 0.5779 0.066 Uani H 1.0 HC7B 0.1555 0.5788 0.5255 0.062 Uani H 1.0 HC9B 0.3507 0.9978 0.5430 0.057 Uani H 1.0 HC12B 0.4288 1.1708 0.6111 0.058 Uani H 1.0 HC13B 0.5076 1.3558 0.6937 0.072 Uani H 1.0 HC14B 0.4861 1.3085 0.8080 0.072 Uani H 1.0 HC15B 0.3872 1.0796 0.8370 0.055 Uani H 1.0 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 Cu 0.0380(4) 0.0404(4) 0.0430(5) 0.0012(5) 0.0090(3) 0.0005(6) Cu O1A 0.145(5) 0.099(5) 0.042(2) -0.002(4) 0.026(2) 0.008(2) O N1A 0.040(1) 0.042(1) 0.054(2) -0.004(1) 0.006(1) -0.004(1) N N2A 0.046(1) 0.038(2) 0.038(2) -0.005(1) 0.0089(9) -0.002(1) N N3A 0.042(1) 0.039(1) 0.049(2) -0.003(1) 0.008(1) -0.004(1) N C1A 0.044(1) 0.052(2) 0.070(2) 0.001(1) -0.003(2) -0.004(1) C C2A 0.044(1) 0.065(3) 0.103(3) 0.006(2) 0.000(2) -0.006(2) C C3A 0.046(1) 0.069(3) 0.115(3) 0.005(2) 0.021(2) -0.010(3) C C4A 0.052(1) 0.062(3) 0.088(2) -0.001(1) 0.030(1) -0.010(2) C C5A 0.045(1) 0.047(2) 0.060(2) -0.004(1) 0.018(1) -0.006(1) C C6A 0.054(1) 0.046(2) 0.045(2) -0.006(1) 0.0181(9) -0.003(1) C C7A 0.080(2) 0.063(2) 0.048(2) -0.006(2) 0.029(1) -0.002(1) C C8A 0.099(3) 0.071(3) 0.040(2) -0.004(2) 0.019(1) 0.004(2) C C9A 0.081(2) 0.060(2) 0.040(2) -0.002(2) 0.003(1) 0.005(1) C C10A 0.055(1) 0.044(2) 0.039(2) -0.003(1) 0.0034(9) 0.001(1) C C11A 0.047(1) 0.042(1) 0.051(2) -0.001(1) 0.0008(9) -0.001(1) C C12A 0.053(2) 0.054(2) 0.072(2) 0.006(1) -0.007(1) 0.001(2) C C13A 0.049(2) 0.061(2) 0.100(3) 0.010(2) 0.001(2) -0.004(2) C C14A 0.048(1) 0.059(2) 0.095(3) 0.006(2) 0.018(2) -0.009(2) C C15A 0.047(1) 0.048(2) 0.066(2) 0.000(1) 0.018(1) -0.008(1) C O1B 0.100(4) 0.082(3) 0.039(1) -0.007(3) 0.009(1) 0.000(1) O N1B 0.038(1) 0.045(1) 0.049(1) -0.001(1) 0.0091(9) 0.0012(9) N N2B 0.032(1) 0.042(1) 0.040(1) 0.005(1) 0.007(1) 0.0000(9) N N3B 0.040(1) 0.041(1) 0.045(1) 0.005(1) 0.0087(9) -0.002(1) N C1B 0.051(2) 0.051(1) 0.059(2) -0.007(2) 0.012(1) 0.005(1) C C2B 0.066(2) 0.054(1) 0.075(2) -0.016(2) 0.011(2) 0.005(1) C C3B 0.071(3) 0.054(1) 0.076(2) -0.018(2) 0.004(2) -0.003(2) C C4B 0.060(2) 0.052(1) 0.062(1) -0.010(1) 0.002(1) -0.006(1) C C5B 0.043(1) 0.046(1) 0.050(1) -0.002(1) 0.0051(9) -0.002(1) C C6B 0.040(1) 0.046(1) 0.042(1) 0.002(1) 0.005(1) -0.0023(9) C C7B 0.059(2) 0.057(1) 0.042(1) -0.001(1) 0.004(1) -0.004(1) C C8B 0.067(2) 0.063(2) 0.040(1) -0.001(2) 0.007(1) 0.001(1) C C9B 0.055(2) 0.055(1) 0.042(1) 0.001(1) 0.009(1) 0.005(1) C C10B 0.038(1) 0.044(1) 0.041(1) 0.0045(9) 0.008(1) 0.002(1) C C11B 0.040(1) 0.041(1) 0.047(1) 0.004(1) 0.0083(9) 0.0020(9) C C12B 0.056(2) 0.044(1) 0.058(1) -0.001(1) 0.009(1) 0.006(1) C C13B 0.069(2) 0.043(2) 0.069(2) -0.006(1) 0.009(2) 0.001(1) C C14B 0.071(3) 0.044(2) 0.066(2) -0.004(1) 0.008(2) -0.007(1) C C15B 0.056(2) 0.044(1) 0.053(2) 0.002(1) 0.009(1) -0.007(1) C OW 0.106(5) 0.091(5) 0.078(5) -0.008(5) 0.039(4) -0.005(4) O B1A 0.104(6) 0.098(7) 0.052(6) -0.035(5) 0.030(4) -0.006(3) B F1A 0.111(6) 0.127(7) 0.072(6) -0.046(5) 0.022(4) -0.029(4) F F2A 0.153(7) 0.207(9) 0.068(7) 0.018(7) 0.036(6) 0.037(7) F F3A 0.147(8) 0.188(9) 0.092(9) 0.012(9) 0.052(6) -0.017(8) F F4A 0.152(8) 0.115(6) 0.183(9) -0.077(8) 0.058(6) -0.014(6) F B1A' 0.102(6) 0.086(7) 0.047(6) -0.039(5) 0.029(4) -0.006(4) B F2A' 0.146(8) 0.129(6) 0.103(8) -0.039(6) 0.029(5) -0.056(6) F F1A' 0.112(6) 0.174(9) 0.076(6) -0.038(5) 0.014(4) -0.033(5) F F3A' 0.128(7) 0.169(9) 0.087(6) -0.027(5) 0.060(5) 0.022(6) F F4A' 0.172(9) 0.116(8) 0.129(9) -0.004(6) 0.062(7) 0.040(7) F B1B 0.103(9) 0.127(8) 0.060(9) -0.010(6) 0.010(9) 0.006(7) B F1B 0.215(9) 0.160(9) 0.088(9) -0.061(9) -0.030(9) 0.003(9) F F2B 0.101(9) 0.126(8) 0.150(9) -0.003(7) 0.028(8) -0.014(7) F F3B 0.260(9) 0.223(9) 0.096(9) -0.119(9) -0.022(9) 0.057(9) F F4B 0.114(9) 0.151(8) 0.304(9) -0.011(6) 0.083(9) -0.041(9) F B1B' 0.104(9) 0.124(8) 0.067(9) -0.008(7) 0.003(9) 0.006(7) B F2B' 0.135(9) 0.126(9) 0.353(9) -0.003(9) 0.009(9) -0.036(8) F F1B' 0.104(9) 0.124(8) 0.079(9) -0.009(7) 0.000(8) 0.009(7) F F3B' 0.253(9) 0.239(9) 0.123(9) -0.113(9) 0.090(9) -0.008(9) F F4B' 0.204(9) 0.160(9) 0.112(9) -0.064(9) -0.068(9) 0.042(8) F # 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 Cu N1A 2.142(4) 1_555 1_555 no Cu N2A 1.953(4) 1_555 1_555 no Cu N3A 2.163(4) 1_555 1_555 no Cu N1B 2.209(4) 1_555 1_555 no Cu N2B 1.978(4) 1_555 1_555 no Cu N3B 2.218(4) 1_555 1_555 no O1A C8A 1.350(6) 1_555 1_555 no N1A C1A 1.335(4) 1_555 1_555 no N1A C5A 1.345(5) 1_555 1_555 no N2A C6A 1.349(4) 1_555 1_555 no N2A C10A 1.349(4) 1_555 1_555 no N3A C11A 1.345(5) 1_555 1_555 no N3A C15A 1.335(4) 1_555 1_555 no C1A C2A 1.365(5) 1_555 1_555 no C2A C3A 1.363(6) 1_555 1_555 no C3A C4A 1.383(6) 1_555 1_555 no C4A C5A 1.380(5) 1_555 1_555 no C5A C6A 1.451(7) 1_555 1_555 no C6A C7A 1.383(5) 1_555 1_555 no C7A C8A 1.392(5) 1_555 1_555 no C8A C9A 1.392(5) 1_555 1_555 no C9A C10A 1.383(5) 1_555 1_555 no C10A C11A 1.492(7) 1_555 1_555 no C11A C12A 1.380(5) 1_555 1_555 no C12A C13A 1.383(6) 1_555 1_555 no C13A C14A 1.363(6) 1_555 1_555 no C14A C15A 1.365(5) 1_555 1_555 no O1B C8B 1.350(6) 1_555 1_555 no N1B C1B 1.335(4) 1_555 1_555 no N1B C5B 1.345(5) 1_555 1_555 no N2B C6B 1.349(4) 1_555 1_555 no N2B C10B 1.349(4) 1_555 1_555 no N3B C11B 1.345(5) 1_555 1_555 no N3B C15B 1.335(4) 1_555 1_555 no C1B C2B 1.365(5) 1_555 1_555 no C2B C3B 1.363(6) 1_555 1_555 no C3B C4B 1.383(6) 1_555 1_555 no C4B C5B 1.380(5) 1_555 1_555 no C5B C6B 1.481(7) 1_555 1_555 no C6B C7B 1.383(5) 1_555 1_555 no C7B C8B 1.392(5) 1_555 1_555 no C8B C9B 1.392(5) 1_555 1_555 no C9B C10B 1.383(5) 1_555 1_555 no C10B C11B 1.477(7) 1_555 1_555 no C11B C12B 1.380(5) 1_555 1_555 no C12B C13B 1.383(6) 1_555 1_555 no C13B C14B 1.363(6) 1_555 1_555 no C14B C15B 1.365(5) 1_555 1_555 no B1A F1A 1.352(3) 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 N1A Cu N2A 78.0(2) 1_555 1_555 1_555 no N1A Cu N3A 155.6(2) 1_555 1_555 1_555 no N1A Cu N1B 93.1(2) 1_555 1_555 1_555 no N1A Cu N2B 102.3(2) 1_555 1_555 1_555 no N1A Cu N3B 90.8(2) 1_555 1_555 1_555 no N2A Cu N3A 77.7(2) 1_555 1_555 1_555 no N2A Cu N1B 101.9(2) 1_555 1_555 1_555 no N2A Cu N2B 179.5(2) 1_555 1_555 1_555 no N2A Cu N3B 103.1(2) 1_555 1_555 1_555 no N3A Cu N1B 92.9(2) 1_555 1_555 1_555 no N3A Cu N2B 102.0(2) 1_555 1_555 1_555 no N3A Cu N3B 93.6(2) 1_555 1_555 1_555 no N1B Cu N2B 77.7(2) 1_555 1_555 1_555 no N1B Cu N3B 154.9(2) 1_555 1_555 1_555 no N2B Cu N3B 77.3(2) 1_555 1_555 1_555 no Cu N1A C1A 127.9(3) 1_555 1_555 1_555 no Cu N1A C5A 113.5(3) 1_555 1_555 1_555 no C1A N1A C5A 118.5(2) 1_555 1_555 1_555 no Cu N2A C6A 118.8(3) 1_555 1_555 1_555 no Cu N2A C10A 120.8(3) 1_555 1_555 1_555 no C6A N2A C10A 120.3(4) 1_555 1_555 1_555 no Cu N3A C11A 113.4(3) 1_555 1_555 1_555 no Cu N3A C15A 128.0(3) 1_555 1_555 1_555 no C11A N3A C15A 118.5(2) 1_555 1_555 1_555 no N1A C1A C2A 123.3(4) 1_555 1_555 1_555 no C1A C2A C3A 118.3(4) 1_555 1_555 1_555 no C2A C3A C4A 119.8(4) 1_555 1_555 1_555 no C3A C4A C5A 118.9(4) 1_555 1_555 1_555 no N1A C5A C4A 121.2(4) 1_555 1_555 1_555 no N1A C5A C6A 113.9(4) 1_555 1_555 1_555 no C4A C5A C6A 125.0(5) 1_555 1_555 1_555 no N2A C6A C5A 115.6(4) 1_555 1_555 1_555 no N2A C6A C7A 121.3(3) 1_555 1_555 1_555 no C5A C6A C7A 123.1(4) 1_555 1_555 1_555 no C6A C7A C8A 118.6(4) 1_555 1_555 1_555 no O1A C8A C7A 121.8(4) 1_555 1_555 1_555 no O1A C8A C9A 118.3(4) 1_555 1_555 1_555 no C7A C8A C9A 119.9(5) 1_555 1_555 1_555 no C8A C9A C10A 118.6(4) 1_555 1_555 1_555 no N2A C10A C9A 121.3(3) 1_555 1_555 1_555 no N2A C10A C11A 113.8(4) 1_555 1_555 1_555 no C9A C10A C11A 124.9(4) 1_555 1_555 1_555 no N3A C11A C10A 114.2(4) 1_555 1_555 1_555 no N3A C11A C12A 121.2(4) 1_555 1_555 1_555 no C10A C11A C12A 124.7(5) 1_555 1_555 1_555 no C11A C12A C13A 118.9(4) 1_555 1_555 1_555 no C12A C13A C14A 119.8(4) 1_555 1_555 1_555 no C13A C14A C15A 118.3(4) 1_555 1_555 1_555 no N3A C15A C14A 123.3(4) 1_555 1_555 1_555 no Cu N1B C1B 129.2(3) 1_555 1_555 1_555 no Cu N1B C5B 112.1(3) 1_555 1_555 1_555 no C1B N1B C5B 118.5(2) 1_555 1_555 1_555 no Cu N2B C6B 119.4(3) 1_555 1_555 1_555 no Cu N2B C10B 120.2(3) 1_555 1_555 1_555 no C6B N2B C10B 120.3(4) 1_555 1_555 1_555 no Cu N3B C11B 111.8(3) 1_555 1_555 1_555 no Cu N3B C15B 129.6(3) 1_555 1_555 1_555 no C11B N3B C15B 118.5(2) 1_555 1_555 1_555 no N1B C1B C2B 123.3(3) 1_555 1_555 1_555 no C1B C2B C3B 118.3(4) 1_555 1_555 1_555 no C2B C3B C4B 119.8(4) 1_555 1_555 1_555 no C3B C4B C5B 118.9(4) 1_555 1_555 1_555 no N1B C5B C4B 121.2(4) 1_555 1_555 1_555 no N1B C5B C6B 114.9(4) 1_555 1_555 1_555 no C4B C5B C6B 123.9(5) 1_555 1_555 1_555 no N2B C6B C5B 115.6(4) 1_555 1_555 1_555 no N2B C6B C7B 121.3(3) 1_555 1_555 1_555 no C5B C6B C7B 123.0(5) 1_555 1_555 1_555 no C6B C7B C8B 118.6(4) 1_555 1_555 1_555 no O1B C8B C7B 118.3(4) 1_555 1_555 1_555 no O1B C8B C9B 121.8(4) 1_555 1_555 1_555 no C7B C8B C9B 119.9(5) 1_555 1_555 1_555 no C8B C9B C10B 118.6(4) 1_555 1_555 1_555 no N2B C10B C9B 121.3(3) 1_555 1_555 1_555 no N2B C10B C11B 114.8(4) 1_555 1_555 1_555 no C9B C10B C11B 123.8(5) 1_555 1_555 1_555 no N3B C11B C10B 115.7(4) 1_555 1_555 1_555 no N3B C11B C12B 121.2(4) 1_555 1_555 1_555 no C10B C11B C12B 123.2(4) 1_555 1_555 1_555 no C11B C12B C13B 118.9(4) 1_555 1_555 1_555 no C12B C13B C14B 119.8(4) 1_555 1_555 1_555 no C13B C14B C15B 118.3(4) 1_555 1_555 1_555 no N3B C15B C14B 123.3(4) 1_555 1_555 1_555 no F1A B1A F2A 109.47 1_555 1_555 1_555 no data_crystal_1 _database_code_depnum_ccdc_archive 'CCDC 261251' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H22 N6 Ni O2 2+,2(B F4 1-)' _chemical_formula_sum 'C30 H22 B2 F8 N6 Ni O2' _chemical_formula_iupac ? _chemical_formula_weight 730.9 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 8.774(3) _cell_length_b 8.871(2) _cell_length_c 38.795(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3020(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480.0 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.91 # 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 1660 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 20 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 16 # REFINEMENT DATA _refine_special_details ; Data were limited due to decomposition apparently caused by radiation damage. Each ligand was modelled as three refineable planar rings. The anions were refined as identical ideal tetrahedra with a common B-F distance. Thermal motion was refined using 15-parameter TLX group parameters, one for each ligand, and two for the anions. A single atom anisotropic thermal parameter was employed for the Ni atom. ; _reflns_number_total 1660 _reflns_number_gt 1268 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.058 _refine_ls_abs_structure_details ; The enantiomer is confirmed, with the alternative giving R_factor 0.050 ; _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1268 _refine_ls_number_parameters 140 _refine_ls_goodness_of_fit_ref 1.97 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.50 _refine_diff_density_min -0.50 _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 0.65494(14) 0.89391(13) 0.62498(3) 0.0320(4) Uani Ni 1.0 O1A 0.7391(8) 0.9566(7) 0.7799(2) 0.068(4) Uani O 1.0 N1A 0.8766(6) 0.8062(6) 0.6324(2) 0.034(2) Uani N 1.0 N2A 0.6785(6) 0.9067(6) 0.6758(1) 0.032(2) Uani N 1.0 N3A 0.4422(6) 0.9834(6) 0.6405(2) 0.032(2) Uani N 1.0 C1A 0.9703(7) 0.7469(8) 0.6085(2) 0.041(2) Uani C 1.0 C2A 1.1084(8) 0.6811(8) 0.6169(2) 0.052(2) Uani C 1.0 C3A 1.1528(8) 0.6756(8) 0.6508(2) 0.054(3) Uani C 1.0 C4A 1.0570(9) 0.7365(8) 0.6757(2) 0.046(3) Uani C 1.0 C5A 0.9195(8) 0.8011(7) 0.6657(2) 0.037(2) Uani C 1.0 C6A 0.8108(8) 0.8648(7) 0.6905(2) 0.036(2) Uani C 1.0 C7A 0.8343(8) 0.8804(7) 0.7256(2) 0.045(3) Uani C 1.0 C8A 0.7192(5) 0.9402(5) 0.7457(2) 0.051(3) Uani C 1.0 C9A 0.5835(8) 0.9830(7) 0.7305(2) 0.046(3) Uani C 1.0 C10A 0.5661(8) 0.9649(8) 0.6952(2) 0.036(2) Uani C 1.0 C11A 0.4303(8) 1.0106(8) 0.6745(2) 0.036(2) Uani C 1.0 C12A 0.2997(9) 1.0742(9) 0.6887(2) 0.047(3) Uani C 1.0 C13A 0.1781(8) 1.1106(8) 0.6674(2) 0.052(3) Uani C 1.0 C14A 0.1908(7) 1.0826(8) 0.6327(2) 0.047(2) Uani C 1.0 C15A 0.3237(8) 1.0192(7) 0.6201(2) 0.038(2) Uani C 1.0 O1B 0.6504(9) 0.8261(7) 0.4693(1) 0.075(4) Uani O 1.0 N1B 0.7409(6) 1.1043(6) 0.6085(2) 0.034(1) Uani N 1.0 N2B 0.6358(6) 0.8795(6) 0.5741(1) 0.031(2) Uani N 1.0 N3B 0.5676(6) 0.6727(6) 0.6184(2) 0.032(1) Uani N 1.0 C1B 0.7953(8) 1.2161(7) 0.6284(2) 0.040(1) Uani C 1.0 C2B 0.8584(8) 1.3462(7) 0.6148(2) 0.049(2) Uani C 1.0 C3B 0.8662(8) 1.3629(8) 0.5796(2) 0.053(2) Uani C 1.0 C4B 0.8103(9) 1.2482(8) 0.5589(2) 0.048(2) Uani C 1.0 C5B 0.7483(8) 1.1201(8) 0.5740(2) 0.037(2) Uani C 1.0 C6B 0.6903(7) 0.9909(7) 0.5541(2) 0.037(2) Uani C 1.0 C7B 0.6965(7) 0.9759(7) 0.5186(2) 0.049(2) Uani C 1.0 C8B 0.6456(6) 0.8436(5) 0.5037(2) 0.054(3) Uani C 1.0 C9B 0.5897(7) 0.7295(7) 0.5244(2) 0.047(2) Uani C 1.0 C10B 0.5861(7) 0.7505(7) 0.5598(2) 0.035(2) Uani C 1.0 C11B 0.5384(8) 0.6358(8) 0.5854(2) 0.035(2) Uani C 1.0 C12B 0.4754(8) 0.4972(8) 0.5765(2) 0.043(2) Uani C 1.0 C13B 0.4416(8) 0.3939(8) 0.6023(2) 0.049(2) Uani C 1.0 C14B 0.4716(8) 0.4321(8) 0.6359(2) 0.048(2) Uani C 1.0 C15B 0.5344(8) 0.5717(7) 0.6431(2) 0.040(1) Uani C 1.0 B1A 0.8042(12) 0.3967(10) 0.7192(2) 0.064(6) Uani B 0.58 F1A 0.9446(15) 0.3822(17) 0.7047(4) 0.089(7) Uani F 0.58 F2A 0.6989(17) 0.3261(18) 0.6991(3) 0.117(9) Uani F 0.58 F3A 0.7682(17) 0.5455(11) 0.7219(4) 0.123(7) Uani F 0.58 F4A 0.8050(18) 0.3330(16) 0.7512(3) 0.106(8) Uani F 0.58 B1A' 0.8527(18) 0.4056(14) 0.7172(3) 0.062(6) Uani B 0.42 F1A' 0.7317(25) 0.4351(24) 0.6963(5) 0.108(8) Uani F 0.42 F2A' 0.8715(25) 0.5214(18) 0.7398(4) 0.104(4) Uani F 0.42 F3A' 0.9809(24) 0.3902(27) 0.6977(5) 0.112(8) Uani F 0.42 F4A' 0.8267(27) 0.2756(16) 0.7349(5) 0.102(8) Uani F 0.42 B1B 0.1769(5) 1.0786(5) 0.5303(1) 0.075(4) Uani B 1.0 F1B 0.1099(8) 0.9675(6) 0.5492(2) 0.103(3) Uani F 1.0 F2B 0.2085(10) 1.1982(6) 0.5511(2) 0.133(6) Uani F 1.0 F3B 0.0805(7) 1.1229(7) 0.5048(1) 0.092(5) Uani F 1.0 F4B 0.3085(7) 1.0258(9) 0.5162(2) 0.150(5) Uani F 1.0 HC1A 0.9389 0.7504 0.5838 0.044 Uani H 1.0 HC2A 1.1751 0.6381 0.5985 0.062 Uani H 1.0 HC3A 1.2521 0.6286 0.6575 0.064 Uani H 1.0 HC4A 1.0866 0.7340 0.7006 0.052 Uani H 1.0 HC7A 0.9331 0.8489 0.7363 0.053 Uani H 1.0 HC9A 0.4992 1.0265 0.7447 0.055 Uani H 1.0 HC12A 0.2933 1.0934 0.7141 0.054 Uani H 1.0 HC13A 0.0832 1.1564 0.6771 0.063 Uani H 1.0 HC14A 0.1051 1.1077 0.6167 0.054 Uani H 1.0 HC15A 0.3320 0.9991 0.5948 0.039 Uani H 1.0 HC1B 0.7901 1.2049 0.6540 0.044 Uani H 1.0 HC2B 0.8977 1.4271 0.6304 0.058 Uani H 1.0 HC3B 0.9113 1.4559 0.5692 0.064 Uani H 1.0 HC4B 0.8147 1.2575 0.5332 0.056 Uani H 1.0 HC7B 0.7372 1.0594 0.5039 0.058 Uani H 1.0 HC9B 0.5525 0.6332 0.5140 0.054 Uani H 1.0 HC12B 0.4546 0.4722 0.5519 0.051 Uani H 1.0 HC13B 0.3962 0.2937 0.5965 0.059 Uani H 1.0 HC14B 0.4484 0.3599 0.6550 0.057 Uani H 1.0 HC15B 0.5559 0.5985 0.6676 0.044 Uani H 1.0 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 0.0349(7) 0.0267(7) 0.0342(8) 0.0006(8) 0.0000(8) -0.0015(7) Ni O1A 0.099(6) 0.067(5) 0.036(4) -0.004(4) -0.011(2) -0.007(2) O N1A 0.033(2) 0.026(2) 0.043(2) -0.005(2) 0.001(2) -0.001(2) N N2A 0.037(2) 0.024(2) 0.034(2) -0.007(2) -0.002(1) -0.004(2) N N3A 0.033(2) 0.024(2) 0.040(2) -0.006(2) 0.001(1) -0.002(2) N C1A 0.039(2) 0.033(3) 0.052(2) 0.001(2) 0.008(2) 0.001(2) C C2A 0.041(2) 0.043(3) 0.071(3) 0.007(2) 0.012(3) 0.008(3) C C3A 0.037(2) 0.047(4) 0.077(4) 0.003(2) 0.001(3) 0.013(3) C C4A 0.036(3) 0.041(3) 0.062(3) -0.004(2) -0.007(2) 0.009(2) C C5A 0.034(2) 0.030(2) 0.046(2) -0.006(2) -0.004(1) 0.002(2) C C6A 0.040(2) 0.029(2) 0.038(2) -0.008(2) -0.006(1) -0.001(2) C C7A 0.055(3) 0.041(3) 0.040(3) -0.009(2) -0.012(2) -0.001(2) C C8A 0.071(3) 0.048(3) 0.035(3) -0.006(2) -0.007(2) -0.005(2) C C9A 0.064(3) 0.041(3) 0.035(3) -0.002(2) 0.003(1) -0.006(2) C C10A 0.045(2) 0.029(2) 0.035(3) -0.005(2) 0.003(1) -0.004(2) C C11A 0.040(2) 0.028(2) 0.041(3) -0.003(2) 0.006(1) -0.002(2) C C12A 0.048(2) 0.039(3) 0.053(3) 0.004(2) 0.015(2) 0.000(2) C C13A 0.042(2) 0.045(3) 0.068(4) 0.006(2) 0.015(2) 0.007(3) C C14A 0.034(2) 0.041(2) 0.066(3) 0.000(2) 0.003(2) 0.008(2) C C15A 0.033(2) 0.030(2) 0.049(2) -0.005(2) -0.002(2) 0.003(2) C O1B 0.125(8) 0.067(5) 0.031(4) -0.002(5) -0.002(3) -0.003(1) O N1B 0.033(2) 0.029(2) 0.039(2) -0.001(2) 0.001(2) -0.002(1) N N2B 0.032(3) 0.031(2) 0.031(2) 0.001(2) 0.000(3) -0.001(1) N N3B 0.031(3) 0.030(2) 0.037(2) -0.001(2) 0.003(2) -0.001(1) N C1B 0.041(3) 0.031(2) 0.049(2) -0.004(2) -0.001(2) -0.005(2) C C2B 0.051(4) 0.032(2) 0.065(3) -0.008(2) 0.002(3) -0.004(2) C C3B 0.058(4) 0.034(2) 0.068(4) -0.009(2) 0.010(3) 0.004(2) C C4B 0.057(4) 0.035(2) 0.052(3) -0.005(2) 0.010(3) 0.007(2) C C5B 0.040(2) 0.031(2) 0.040(2) -0.001(2) 0.004(2) 0.002(1) C C6B 0.044(3) 0.034(2) 0.033(3) 0.001(2) 0.002(3) 0.002(1) C C7B 0.070(4) 0.044(2) 0.033(3) 0.000(2) 0.004(3) 0.004(1) C C8B 0.082(5) 0.050(3) 0.031(3) -0.001(3) -0.002(3) -0.002(1) C C9B 0.062(4) 0.043(2) 0.034(3) -0.001(2) -0.006(3) -0.006(1) C C10B 0.038(3) 0.034(2) 0.034(3) 0.000(2) -0.003(3) -0.004(1) C C11B 0.033(3) 0.031(2) 0.040(2) -0.002(2) -0.001(2) -0.004(1) C C12B 0.043(3) 0.034(2) 0.053(3) -0.006(2) -0.004(2) -0.007(2) C C13B 0.048(3) 0.033(2) 0.065(3) -0.009(2) 0.003(3) -0.004(2) C C14B 0.051(3) 0.033(2) 0.059(3) -0.007(2) 0.010(3) 0.003(2) C C15B 0.043(3) 0.032(2) 0.044(2) -0.003(2) 0.007(2) 0.003(2) C B1A 0.080(8) 0.075(9) 0.035(8) 0.026(7) -0.005(4) -0.008(4) B F1A 0.092(8) 0.119(9) 0.056(8) 0.027(6) 0.012(4) -0.020(5) F F2A 0.115(8) 0.162(9) 0.075(9) -0.013(9) -0.026(6) -0.021(9) F F3A 0.137(9) 0.087(9) 0.143(9) 0.057(9) -0.005(7) -0.011(5) F F4A 0.127(9) 0.142(9) 0.048(7) 0.002(8) -0.003(6) 0.022(7) F B1A' 0.081(8) 0.072(9) 0.032(8) 0.026(7) -0.004(4) -0.008(4) B F1A' 0.107(9) 0.149(9) 0.068(8) 0.025(9) -0.032(6) 0.018(6) F F2A' 0.133(9) 0.097(9) 0.082(8) 0.013(9) -0.001(6) -0.043(6) F F3A' 0.102(9) 0.164(9) 0.071(9) 0.022(6) 0.025(5) -0.025(7) F F4A' 0.131(9) 0.086(9) 0.090(9) 0.016(7) -0.011(6) 0.020(7) F B1B 0.086(8) 0.073(4) 0.066(6) -0.010(4) -0.011(3) 0.003(2) B F1B 0.173(8) 0.073(4) 0.064(5) -0.007(4) 0.016(5) 0.009(3) F F2B 0.207(9) 0.091(4) 0.100(5) -0.032(5) -0.056(6) -0.008(4) F F3B 0.126(7) 0.079(4) 0.070(6) 0.002(4) -0.026(4) 0.005(3) F F4B 0.090(8) 0.139(8) 0.221(9) 0.009(5) 0.029(5) 0.008(6) F # 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 N1A 2.114(5) 1_555 1_555 no Ni N2A 1.985(5) 1_555 1_555 no Ni N3A 2.116(5) 1_555 1_555 no Ni N1B 2.112(5) 1_555 1_555 no Ni N2B 1.984(5) 1_555 1_555 no Ni N3B 2.122(5) 1_555 1_555 no O1A C8A 1.347(8) 1_555 1_555 no N1A C1A 1.345(5) 1_555 1_555 no N1A C5A 1.346(6) 1_555 1_555 no N2A C6A 1.345(5) 1_555 1_555 no N2A C10A 1.345(5) 1_555 1_555 no N3A C11A 1.346(6) 1_555 1_555 no N3A C15A 1.345(5) 1_555 1_555 no C1A C2A 1.383(6) 1_555 1_555 no C2A C3A 1.374(7) 1_555 1_555 no C3A C4A 1.388(7) 1_555 1_555 no C4A C5A 1.391(7) 1_555 1_555 no C5A C6A 1.467(8) 1_555 1_555 no C6A C7A 1.386(7) 1_555 1_555 no C7A C8A 1.381(6) 1_555 1_555 no C8A C9A 1.381(6) 1_555 1_555 no C9A C10A 1.386(7) 1_555 1_555 no C10A C11A 1.493(8) 1_555 1_555 no C11A C12A 1.391(7) 1_555 1_555 no C12A C13A 1.388(7) 1_555 1_555 no C13A C14A 1.374(7) 1_555 1_555 no C14A C15A 1.383(6) 1_555 1_555 no O1B C8B 1.347(8) 1_555 1_555 no N1B C1B 1.345(5) 1_555 1_555 no N1B C5B 1.346(6) 1_555 1_555 no N2B C6B 1.345(5) 1_555 1_555 no N2B C10B 1.345(5) 1_555 1_555 no N3B C11B 1.346(6) 1_555 1_555 no N3B C15B 1.345(5) 1_555 1_555 no C1B C2B 1.383(6) 1_555 1_555 no C2B C3B 1.374(7) 1_555 1_555 no C3B C4B 1.388(7) 1_555 1_555 no C4B C5B 1.391(7) 1_555 1_555 no C5B C6B 1.472(9) 1_555 1_555 no C6B C7B 1.386(7) 1_555 1_555 no C7B C8B 1.381(6) 1_555 1_555 no C8B C9B 1.381(6) 1_555 1_555 no C9B C10B 1.386(7) 1_555 1_555 no C10B C11B 1.482(8) 1_555 1_555 no C11B C12B 1.391(7) 1_555 1_555 no C12B C13B 1.388(7) 1_555 1_555 no C13B C14B 1.374(7) 1_555 1_555 no C14B C15B 1.383(6) 1_555 1_555 no B1A F1A 1.361(3) 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 N1A Ni N2A 77.9(2) 1_555 1_555 1_555 no N1A Ni N3A 155.6(3) 1_555 1_555 1_555 no N1A Ni N1B 92.2(2) 1_555 1_555 1_555 no N1A Ni N2B 100.9(2) 1_555 1_555 1_555 no N1A Ni N3B 90.5(2) 1_555 1_555 1_555 no N2A Ni N3A 77.8(2) 1_555 1_555 1_555 no N2A Ni N1B 102.3(2) 1_555 1_555 1_555 no N2A Ni N2B 178.8(2) 1_555 1_555 1_555 no N2A Ni N3B 102.1(2) 1_555 1_555 1_555 no N3A Ni N1B 94.0(2) 1_555 1_555 1_555 no N3A Ni N2B 103.4(2) 1_555 1_555 1_555 no N3A Ni N3B 93.6(2) 1_555 1_555 1_555 no N1B Ni N2B 77.7(2) 1_555 1_555 1_555 no N1B Ni N3B 155.4(3) 1_555 1_555 1_555 no N2B Ni N3B 77.8(2) 1_555 1_555 1_555 no Ni N1A C1A 127.8(4) 1_555 1_555 1_555 no Ni N1A C5A 113.6(4) 1_555 1_555 1_555 no C1A N1A C5A 118.4(3) 1_555 1_555 1_555 no Ni N2A C6A 119.6(4) 1_555 1_555 1_555 no Ni N2A C10A 120.1(4) 1_555 1_555 1_555 no C6A N2A C10A 120.1(6) 1_555 1_555 1_555 no Ni N3A C11A 114.5(4) 1_555 1_555 1_555 no Ni N3A C15A 127.1(4) 1_555 1_555 1_555 no C11A N3A C15A 118.4(3) 1_555 1_555 1_555 no N1A C1A C2A 122.7(4) 1_555 1_555 1_555 no C1A C2A C3A 119.2(5) 1_555 1_555 1_555 no C2A C3A C4A 118.7(5) 1_555 1_555 1_555 no C3A C4A C5A 119.4(5) 1_555 1_555 1_555 no N1A C5A C4A 121.6(5) 1_555 1_555 1_555 no N1A C5A C6A 115.7(6) 1_555 1_555 1_555 no C4A C5A C6A 122.6(6) 1_555 1_555 1_555 no N2A C6A C5A 112.9(6) 1_555 1_555 1_555 no N2A C6A C7A 121.1(5) 1_555 1_555 1_555 no C5A C6A C7A 125.9(6) 1_555 1_555 1_555 no C6A C7A C8A 118.9(5) 1_555 1_555 1_555 no O1A C8A C7A 120.1(3) 1_555 1_555 1_555 no O1A C8A C9A 120.1(3) 1_555 1_555 1_555 no C7A C8A C9A 119.7(7) 1_555 1_555 1_555 no C8A C9A C10A 118.9(5) 1_555 1_555 1_555 no N2A C10A C9A 121.1(5) 1_555 1_555 1_555 no N2A C10A C11A 112.8(6) 1_555 1_555 1_555 no C9A C10A C11A 126.0(6) 1_555 1_555 1_555 no N3A C11A C10A 114.6(6) 1_555 1_555 1_555 no N3A C11A C12A 121.6(5) 1_555 1_555 1_555 no C10A C11A C12A 123.7(6) 1_555 1_555 1_555 no C11A C12A C13A 119.4(5) 1_555 1_555 1_555 no C12A C13A C14A 118.7(5) 1_555 1_555 1_555 no C13A C14A C15A 119.2(5) 1_555 1_555 1_555 no N3A C15A C14A 122.7(4) 1_555 1_555 1_555 no Ni N1B C1B 127.3(4) 1_555 1_555 1_555 no Ni N1B C5B 114.2(4) 1_555 1_555 1_555 no C1B N1B C5B 118.4(3) 1_555 1_555 1_555 no Ni N2B C6B 119.8(4) 1_555 1_555 1_555 no Ni N2B C10B 119.6(4) 1_555 1_555 1_555 no C6B N2B C10B 120.1(6) 1_555 1_555 1_555 no Ni N3B C11B 114.1(4) 1_555 1_555 1_555 no Ni N3B C15B 127.5(4) 1_555 1_555 1_555 no C11B N3B C15B 118.4(3) 1_555 1_555 1_555 no N1B C1B C2B 122.7(4) 1_555 1_555 1_555 no C1B C2B C3B 119.2(5) 1_555 1_555 1_555 no C2B C3B C4B 118.7(5) 1_555 1_555 1_555 no C3B C4B C5B 119.4(5) 1_555 1_555 1_555 no N1B C5B C4B 121.6(5) 1_555 1_555 1_555 no N1B C5B C6B 115.1(6) 1_555 1_555 1_555 no C4B C5B C6B 123.3(6) 1_555 1_555 1_555 no N2B C6B C5B 113.1(6) 1_555 1_555 1_555 no N2B C6B C7B 121.1(5) 1_555 1_555 1_555 no C5B C6B C7B 125.7(6) 1_555 1_555 1_555 no C6B C7B C8B 118.9(5) 1_555 1_555 1_555 no O1B C8B C7B 120.1(3) 1_555 1_555 1_555 no O1B C8B C9B 120.1(3) 1_555 1_555 1_555 no C7B C8B C9B 119.7(7) 1_555 1_555 1_555 no C8B C9B C10B 118.9(5) 1_555 1_555 1_555 no N2B C10B C9B 121.1(5) 1_555 1_555 1_555 no N2B C10B C11B 113.5(6) 1_555 1_555 1_555 no C9B C10B C11B 125.3(6) 1_555 1_555 1_555 no N3B C11B C10B 114.6(6) 1_555 1_555 1_555 no N3B C11B C12B 121.6(5) 1_555 1_555 1_555 no C10B C11B C12B 123.7(6) 1_555 1_555 1_555 no C11B C12B C13B 119.4(5) 1_555 1_555 1_555 no C12B C13B C14B 118.7(5) 1_555 1_555 1_555 no C13B C14B C15B 119.2(5) 1_555 1_555 1_555 no N3B C15B C14B 122.7(4) 1_555 1_555 1_555 no F1A B1A F2A 109.47(1) 1_555 1_555 1_555 no