# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2038 data_gk001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 Cl N5 O6 Ru' _chemical_formula_weight 675.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2200(10) _cell_length_b 19.906(3) _cell_length_c 15.722(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.760(10) _cell_angle_gamma 90.00 _cell_volume 2885.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour violet _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5405 _diffrn_reflns_av_R_equivalents 0.0062 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.92 _reflns_number_total 5052 _reflns_number_gt 4430 _reflns_threshold_expression >2sigma(I) _computing_data_collection Argus _computing_cell_refinement Argus _computing_data_reduction Maxus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Platon _computing_publication_material Ciftab _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^)+(0.1623P)^2^+0.7327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5052 _refine_ls_number_parameters 417 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.2030 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.95532(3) 0.773422(15) 0.51058(2) 0.0358(2) Uani 1 d . . . N1 N 1.0457(4) 0.86256(18) 0.4739(3) 0.0431(8) Uani 1 d . . . C1 C 1.1189(6) 0.9052(3) 0.5255(4) 0.0623(14) Uani 1 d . . . H1A H 1.1295 0.8942 0.5848 0.080 Uiso 1 d R . . C2 C 1.1793(8) 0.9634(3) 0.4953(5) 0.084(2) Uani 1 d . . . H2A H 1.2326 0.9923 0.5333 0.080 Uiso 1 d R . . C3 C 1.1641(7) 0.9806(3) 0.4092(5) 0.0817(19) Uani 1 d . . . H3A H 1.2065 1.0210 0.3871 0.080 Uiso 1 d R . . C4 C 1.0852(7) 0.9374(3) 0.3583(4) 0.0690(15) Uani 1 d . . . H4A H 1.0684 0.9483 0.2995 0.080 Uiso 1 d R . . C5 C 1.0285(5) 0.8782(2) 0.3907(3) 0.0477(10) Uani 1 d . . . C6 C 0.9492(5) 0.8278(2) 0.3393(3) 0.0496(11) Uani 1 d . . . C7 C 0.9111(8) 0.8355(3) 0.2558(4) 0.0729(16) Uani 1 d . . . H7A H 0.9384 0.8755 0.2258 0.080 Uiso 1 d R . . C8 C 0.8364(9) 0.7851(4) 0.2134(4) 0.080(2) Uani 1 d . . . H8A H 0.8086 0.7897 0.1547 0.080 Uiso 1 d R . . C9 C 0.8021(8) 0.7289(3) 0.2585(4) 0.0645(16) Uani 1 d . . . H9A H 0.7491 0.6933 0.2310 0.080 Uiso 1 d R . . C10 C 0.8393(6) 0.7230(2) 0.3419(3) 0.0503(12) Uani 1 d . . . H10A H 0.8154 0.6824 0.3715 0.080 Uiso 1 d R . . N2 N 0.9120(4) 0.77236(14) 0.3851(3) 0.0366(8) Uani 1 d . . . N3 N 0.8770(4) 0.68093(18) 0.5451(2) 0.0441(8) Uani 1 d . . . C11 C 0.7391(6) 0.6665(3) 0.5671(3) 0.0543(12) Uani 1 d . . . H11A H 0.6665 0.7008 0.5606 0.080 Uiso 1 d R . . C12 C 0.6998(7) 0.6050(3) 0.5984(4) 0.0673(15) Uani 1 d . . . H12A H 0.6013 0.5968 0.6144 0.080 Uiso 1 d R . . C13 C 0.8020(8) 0.5547(3) 0.6062(4) 0.0747(17) Uani 1 d . . . H13A H 0.7763 0.5110 0.6272 0.080 Uiso 1 d R . . C14 C 0.9408(7) 0.5681(3) 0.5832(4) 0.0665(14) Uani 1 d . . . H14A H 1.0141 0.5342 0.5901 0.080 Uiso 1 d R . . C15 C 0.9781(5) 0.6302(2) 0.5509(3) 0.0468(10) Uani 1 d . . . C16 C 1.1212(5) 0.6498(2) 0.5212(3) 0.0472(11) Uani 1 d . . . C17 C 1.2360(6) 0.6046(3) 0.5143(3) 0.0609(13) Uani 1 d . . . H17A H 1.2232 0.5584 0.5302 0.080 Uiso 1 d R . . C18 C 1.3657(6) 0.6261(3) 0.4837(4) 0.0683(15) Uani 1 d . . . H18A H 1.4467 0.5959 0.4804 0.080 Uiso 1 d R . . C19 C 1.3789(6) 0.6910(3) 0.4583(4) 0.0679(15) Uani 1 d . . . H19A H 1.4684 0.7061 0.4343 0.080 Uiso 1 d R . . C20 C 1.2650(6) 0.7363(3) 0.4672(4) 0.0545(12) Uani 1 d . . . H20A H 1.2775 0.7824 0.4508 0.080 Uiso 1 d R . . N4 N 1.1349(4) 0.71524(19) 0.4985(2) 0.0414(8) Uani 1 d . . . O4 O 0.7584(3) 0.82126(15) 0.5228(2) 0.0461(7) Uani 1 d . . . C21 C 0.7069(5) 0.8441(2) 0.5931(3) 0.0451(10) Uani 1 d . . . C22 C 0.5662(5) 0.8740(3) 0.5914(4) 0.0596(13) Uani 1 d . . . H22A H 0.5130 0.8757 0.5385 0.080 Uiso 1 d R . . C23 C 0.5046(7) 0.9001(3) 0.6613(5) 0.0728(16) Uani 1 d . . . H23A H 0.4090 0.9190 0.6572 0.080 Uiso 1 d R . . C24 C 0.5764(7) 0.9001(3) 0.7411(4) 0.0754(17) Uani 1 d . . . H24A H 0.5337 0.9207 0.7900 0.080 Uiso 1 d R . . C25 C 0.7091(7) 0.8703(4) 0.7447(4) 0.0767(17) Uani 1 d . . . H25A H 0.7575 0.8681 0.7991 0.080 Uiso 1 d R . . C26 C 0.7786(5) 0.8422(2) 0.6740(3) 0.0508(11) Uani 1 d . . . C222 C 0.9162(6) 0.8137(2) 0.6896(3) 0.0517(11) Uani 1 d . . . H22B H 0.9517 0.8170 0.7472 0.080 Uiso 1 d R . . O5 O 1.0002(4) 0.78389(16) 0.6373(2) 0.0492(8) Uani 1 d . . . Cl1 Cl 0.65495(14) 0.53950(6) 0.31811(8) 0.0548(3) Uani 1 d D . . O21 O 0.536(2) 0.5007(10) 0.3402(11) 0.134(9) Uani 0.525(14) d PD A 1 O22 O 0.6072(12) 0.6043(4) 0.3444(10) 0.097(4) Uani 0.525(14) d PD A 1 O23 O 0.6692(19) 0.5432(8) 0.2315(6) 0.105(6) Uani 0.525(14) d PD A 1 O24 O 0.734(3) 0.5648(11) 0.3856(9) 0.165(9) Uani 0.525(14) d PD A 1 O21' O 0.563(2) 0.4925(10) 0.3532(17) 0.119(8) Uani 0.475(14) d PD A 2 O22' O 0.630(3) 0.5803(13) 0.2511(16) 0.202(17) Uani 0.475(14) d PD A 2 O23' O 0.739(2) 0.4867(9) 0.2884(18) 0.169(9) Uani 0.475(14) d PD A 2 O24' O 0.7966(10) 0.5350(11) 0.3508(11) 0.113(7) Uani 0.475(14) d PD A 2 C41 C 1.4644(15) 0.8634(6) 0.3177(7) 0.123(4) Uani 1 d . . . N6 N 1.3831(16) 0.8221(5) 0.3023(7) 0.170(5) Uani 1 d . . . C42 C 1.5781(17) 0.9118(8) 0.3339(12) 0.188(7) Uani 1 d . . . H42A H 1.6589 0.8900 0.3613 0.282 Uiso 1 calc R . . H42B H 1.5423 0.9468 0.3701 0.282 Uiso 1 calc R . . H42C H 1.6087 0.9310 0.2810 0.282 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0380(3) 0.0348(3) 0.0343(3) 0.00218(11) -0.00879(18) -0.00130(11) N1 0.045(2) 0.0316(19) 0.053(2) 0.0026(15) -0.0059(16) -0.0006(14) C1 0.073(4) 0.047(3) 0.066(3) -0.006(2) -0.022(3) -0.011(2) C2 0.080(4) 0.050(3) 0.122(6) -0.011(3) -0.024(4) -0.024(3) C3 0.086(4) 0.044(3) 0.115(6) 0.017(3) -0.008(4) -0.020(3) C4 0.079(4) 0.047(3) 0.080(4) 0.017(3) -0.009(3) -0.015(3) C5 0.054(3) 0.037(2) 0.052(3) -0.0014(19) -0.005(2) 0.0042(19) C6 0.056(3) 0.049(3) 0.044(2) 0.019(2) -0.005(2) -0.005(2) C7 0.107(5) 0.066(3) 0.045(3) 0.008(2) -0.012(3) -0.015(3) C8 0.104(5) 0.094(4) 0.040(3) 0.011(3) -0.020(3) -0.016(4) C9 0.078(4) 0.064(4) 0.051(3) -0.008(2) -0.020(3) -0.005(2) C10 0.058(3) 0.045(3) 0.047(3) -0.0076(18) -0.018(2) -0.0094(19) N2 0.044(2) 0.0266(18) 0.039(2) -0.0012(12) -0.0082(17) -0.0032(12) N3 0.049(2) 0.044(2) 0.0398(19) 0.0067(15) -0.0100(16) -0.0008(16) C11 0.052(3) 0.055(3) 0.056(3) 0.011(2) -0.002(2) -0.012(2) C12 0.071(4) 0.061(3) 0.070(4) 0.011(3) 0.003(3) -0.020(3) C13 0.093(5) 0.060(3) 0.070(4) 0.013(3) 0.002(3) -0.031(3) C14 0.083(4) 0.050(3) 0.066(3) 0.004(2) -0.006(3) 0.004(3) C15 0.062(3) 0.039(2) 0.040(2) 0.0038(17) -0.011(2) -0.0010(19) C16 0.056(3) 0.049(2) 0.036(2) -0.0020(19) -0.0123(19) 0.012(2) C17 0.067(3) 0.060(3) 0.055(3) 0.005(2) -0.014(2) 0.017(3) C18 0.061(3) 0.083(4) 0.061(3) -0.004(3) -0.006(3) 0.030(3) C19 0.047(3) 0.096(5) 0.061(3) 0.008(3) 0.002(2) 0.007(3) C20 0.048(3) 0.065(3) 0.051(3) 0.007(2) 0.001(2) -0.001(2) N4 0.041(2) 0.048(2) 0.0341(18) 0.0007(15) -0.0084(15) -0.0001(15) O4 0.0477(17) 0.0461(17) 0.0442(17) -0.0006(13) -0.0101(13) 0.0104(13) C21 0.052(3) 0.028(2) 0.055(3) 0.0129(19) -0.004(2) -0.0057(18) C22 0.045(3) 0.057(3) 0.076(4) -0.001(3) 0.004(2) -0.002(2) C23 0.053(3) 0.068(4) 0.098(5) -0.005(3) 0.010(3) 0.009(3) C24 0.085(4) 0.068(4) 0.074(4) -0.013(3) 0.023(3) 0.012(3) C25 0.080(4) 0.098(5) 0.052(3) -0.012(3) 0.009(3) -0.004(3) C26 0.058(3) 0.046(3) 0.048(3) -0.006(2) -0.001(2) -0.011(2) C222 0.067(3) 0.051(3) 0.036(2) 0.0023(19) -0.008(2) -0.002(2) O5 0.057(2) 0.0495(18) 0.0404(19) -0.0018(14) -0.0124(16) 0.0085(15) Cl1 0.0555(7) 0.0511(7) 0.0581(7) 0.0067(5) 0.0091(5) -0.0016(5) O21 0.155(15) 0.156(16) 0.094(9) -0.058(11) 0.065(10) -0.115(14) O22 0.104(8) 0.056(5) 0.132(11) 0.008(5) 0.023(7) 0.007(5) O23 0.131(11) 0.133(14) 0.050(6) 0.005(7) 0.030(6) -0.022(10) O24 0.25(2) 0.157(15) 0.083(9) -0.016(9) -0.023(12) -0.125(16) O21' 0.112(12) 0.085(10) 0.159(18) 0.069(11) -0.025(11) -0.029(9) O22' 0.20(2) 0.18(2) 0.23(3) 0.17(2) -0.10(2) -0.080(19) O23' 0.153(15) 0.143(16) 0.21(2) -0.058(16) 0.020(15) 0.025(12) O24' 0.051(5) 0.174(16) 0.113(11) 0.080(11) 0.000(6) 0.026(7) C41 0.174(10) 0.088(6) 0.108(7) 0.008(5) 0.050(7) 0.011(6) N6 0.260(14) 0.105(7) 0.148(9) -0.025(6) 0.079(9) -0.045(8) C42 0.177(13) 0.135(12) 0.25(2) 0.024(10) -0.018(13) -0.027(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.007(4) . ? Ru1 N4 2.032(4) . ? Ru1 O5 2.040(4) . ? Ru1 N1 2.046(4) . ? Ru1 N3 2.053(4) . ? Ru1 O4 2.062(3) . ? N1 C1 1.349(6) . ? N1 C5 1.352(6) . ? C1 C2 1.373(9) . ? C2 C3 1.401(11) . ? C3 C4 1.377(9) . ? C4 C5 1.389(7) . ? C5 C6 1.475(7) . ? C6 C7 1.364(7) . ? C6 N2 1.365(5) . ? C7 C8 1.383(9) . ? C8 C9 1.363(9) . ? C9 C10 1.355(9) . ? C10 N2 1.365(6) . ? N3 C11 1.353(6) . ? N3 C15 1.376(6) . ? C11 C12 1.370(7) . ? C12 C13 1.380(9) . ? C13 C14 1.361(9) . ? C14 C15 1.381(7) . ? C15 C16 1.459(7) . ? C16 N4 1.358(6) . ? C16 C17 1.394(7) . ? C17 C18 1.364(8) . ? C18 C19 1.359(9) . ? C19 C20 1.393(8) . ? C20 N4 1.368(7) . ? O4 C21 1.291(6) . ? C21 C26 1.427(7) . ? C21 C22 1.428(7) . ? C22 C23 1.348(8) . ? C23 C24 1.410(10) . ? C24 C25 1.361(9) . ? C25 C26 1.406(8) . ? C26 C222 1.408(7) . ? C222 O5 1.284(6) . ? Cl1 O22' 1.347(11) . ? Cl1 O23 1.372(9) . ? Cl1 O24 1.374(10) . ? Cl1 O21' 1.384(12) . ? Cl1 O21 1.387(10) . ? Cl1 O23' 1.393(12) . ? Cl1 O24' 1.400(9) . ? Cl1 O22 1.426(8) . ? O22 O24 1.54(3) . ? O23' O24' 1.47(3) . ? C41 N6 1.136(15) . ? C41 C42 1.444(18) . ? 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 N2 Ru1 N4 93.07(15) . . ? N2 Ru1 O5 174.73(13) . . ? N4 Ru1 O5 89.70(15) . . ? N2 Ru1 N1 78.98(14) . . ? N4 Ru1 N1 97.62(14) . . ? O5 Ru1 N1 96.21(15) . . ? N2 Ru1 N3 100.61(13) . . ? N4 Ru1 N3 78.66(15) . . ? O5 Ru1 N3 84.33(14) . . ? N1 Ru1 N3 176.24(15) . . ? N2 Ru1 O4 86.10(14) . . ? N4 Ru1 O4 172.73(14) . . ? O5 Ru1 O4 91.71(13) . . ? N1 Ru1 O4 89.32(14) . . ? N3 Ru1 O4 94.38(14) . . ? C1 N1 C5 119.3(4) . . ? C1 N1 Ru1 125.3(4) . . ? C5 N1 Ru1 115.4(3) . . ? N1 C1 C2 121.6(6) . . ? C1 C2 C3 120.4(6) . . ? C4 C3 C2 117.0(5) . . ? C3 C4 C5 121.0(6) . . ? N1 C5 C4 120.7(4) . . ? N1 C5 C6 115.2(4) . . ? C4 C5 C6 124.1(5) . . ? C7 C6 N2 122.3(5) . . ? C7 C6 C5 124.9(4) . . ? N2 C6 C5 112.7(4) . . ? C6 C7 C8 120.2(5) . . ? C9 C8 C7 117.5(6) . . ? C10 C9 C8 121.1(5) . . ? C9 C10 N2 122.4(5) . . ? C10 N2 C6 116.4(4) . . ? C10 N2 Ru1 125.9(3) . . ? C6 N2 Ru1 117.5(3) . . ? C11 N3 C15 117.7(4) . . ? C11 N3 Ru1 126.3(3) . . ? C15 N3 Ru1 115.8(3) . . ? N3 C11 C12 122.4(5) . . ? C11 C12 C13 119.8(6) . . ? C14 C13 C12 118.5(5) . . ? C13 C14 C15 120.9(6) . . ? N3 C15 C14 120.6(5) . . ? N3 C15 C16 113.4(4) . . ? C14 C15 C16 126.0(5) . . ? N4 C16 C17 121.7(5) . . ? N4 C16 C15 115.3(4) . . ? C17 C16 C15 122.9(5) . . ? C18 C17 C16 119.7(5) . . ? C19 C18 C17 119.0(5) . . ? C18 C19 C20 121.1(5) . . ? N4 C20 C19 120.2(5) . . ? C16 N4 C20 118.3(4) . . ? C16 N4 Ru1 116.4(3) . . ? C20 N4 Ru1 125.3(3) . . ? C21 O4 Ru1 125.2(3) . . ? O4 C21 C26 125.7(4) . . ? O4 C21 C22 118.4(4) . . ? C26 C21 C22 115.9(5) . . ? C23 C22 C21 122.5(6) . . ? C22 C23 C24 121.9(6) . . ? C25 C24 C23 116.6(5) . . ? C24 C25 C26 124.0(6) . . ? C25 C26 C222 116.2(5) . . ? C25 C26 C21 119.0(5) . . ? C222 C26 C21 124.9(4) . . ? O5 C222 C26 128.7(4) . . ? C222 O5 Ru1 123.9(3) . . ? O22' Cl1 O23 37.7(15) . . ? O22' Cl1 O24 117.7(14) . . ? O23 Cl1 O24 133.6(12) . . ? O22' Cl1 O21' 128.4(14) . . ? O23 Cl1 O21' 120.0(14) . . ? O24 Cl1 O21' 105.1(13) . . ? O22' Cl1 O21 113.9(16) . . ? O23 Cl1 O21 111.3(11) . . ? O24 Cl1 O21 115.0(10) . . ? O21' Cl1 O21 14.8(17) . . ? O22' Cl1 O23' 106.3(18) . . ? O23 Cl1 O23' 69.2(13) . . ? O24 Cl1 O23' 104.0(17) . . ? O21' Cl1 O23' 88.4(14) . . ? O21 Cl1 O23' 96.3(13) . . ? O22' Cl1 O24' 118.2(13) . . ? O23 Cl1 O24' 105.5(10) . . ? O24 Cl1 O24' 42.1(10) . . ? O21' Cl1 O24' 112.6(10) . . ? O21 Cl1 O24' 127.4(13) . . ? O23' Cl1 O24' 63.4(13) . . ? O22' Cl1 O22 68.4(15) . . ? O23 Cl1 O22 105.8(8) . . ? O24 Cl1 O22 66.9(13) . . ? O21' Cl1 O22 107.6(12) . . ? O21 Cl1 O22 100.6(10) . . ? O23' Cl1 O22 163.0(10) . . ? O24' Cl1 O22 104.0(11) . . ? Cl1 O22 O24 54.9(6) . . ? Cl1 O24 O22 58.2(9) . . ? Cl1 O23' O24' 58.6(7) . . ? Cl1 O24' O23' 58.1(9) . . ? N6 C41 C42 174.5(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.886 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.164