# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sqz _database_code_depnum_ccdc_archive 'CCDC 874637' #TrackingRef '10492_web_deposit_cif_file_0_GregoryNocton_1333444742.Ruacac2tmed.cif' _database_code_depnum_ccdc_archive ? #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# #TrackingRef '10492_web_deposit_cif_file_0_GregoryNocton_1333444742.Ruacac2tmed.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H30 N2 O4 Ru' _chemical_formula_sum 'C16 H30 N2 O4 Ru' _chemical_formula_weight 415.49 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9351(3) _cell_length_b 9.8757(4) _cell_length_c 13.0361(6) _cell_angle_alpha 75.5720(10) _cell_angle_beta 88.3220(10) _cell_angle_gamma 70.2400(10) _cell_volume 929.40(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9367 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 25.34 _exptl_crystal_description Plates _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.723 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD' _diffrn_measurement_method '\f or \w oscillation scans' _diffrn_reflns_number 14197 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3394 _reflns_number_gt 3084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 software' _computing_cell_refinement 'SAINT V7.68A integration software' _computing_data_reduction 'SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^)+(0.0282P)^2^+0.5443P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3394 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.61656(2) 0.617982(19) 0.748479(15) 0.01302(7) Uani 1 1 d . . . N1 N 0.4466(2) 0.4856(2) 0.77436(16) 0.0154(4) Uani 1 1 d . . . N2 N 0.4438(3) 0.7420(2) 0.60839(16) 0.0161(4) Uani 1 1 d . . . C2 C 0.9105(3) 0.3850(2) 0.8911(2) 0.0171(5) Uani 1 1 d . . . O4 O 0.4494(2) 0.74419(16) 0.83839(13) 0.0152(3) Uani 1 1 d . . . O2 O 0.7849(2) 0.49079(17) 0.65840(13) 0.0161(3) Uani 1 1 d . . . O1 O 0.7693(2) 0.49765(17) 0.88633(13) 0.0160(3) Uani 1 1 d . . . O3 O 0.7727(2) 0.75078(17) 0.71711(13) 0.0173(4) Uani 1 1 d . . . C7 C 0.7424(3) 0.8645(2) 0.7543(2) 0.0179(5) Uani 1 1 d . . . C9 C 0.4712(3) 0.8579(2) 0.85763(19) 0.0171(5) Uani 1 1 d . . . C12 C 0.5233(4) 0.3437(3) 0.7438(2) 0.0217(6) Uani 1 1 d . . . C5 C 1.0349(4) 0.3027(3) 0.6204(2) 0.0231(6) Uani 1 1 d . . . C8 C 0.6049(3) 0.9170(3) 0.8192(2) 0.0188(5) Uani 1 1 d . . . C15 C 0.3290(3) 0.8926(3) 0.6154(2) 0.0202(5) Uani 1 1 d . . . C4 C 0.9273(3) 0.3820(2) 0.6983(2) 0.0168(5) Uani 1 1 d . . . C3 C 0.9872(3) 0.3290(3) 0.8052(2) 0.0176(5) Uani 1 1 d . . . C1 C 0.9982(4) 0.3058(3) 1.0006(2) 0.0229(6) Uani 1 1 d . . . C13 C 0.2805(3) 0.5821(3) 0.7060(2) 0.0216(6) Uani 1 1 d . . . C14 C 0.3291(4) 0.6534(3) 0.5979(2) 0.0229(6) Uani 1 1 d . . . C10 C 0.3351(4) 0.9344(3) 0.9261(2) 0.0233(6) Uani 1 1 d . . . C16 C 0.5457(4) 0.7615(3) 0.5124(2) 0.0231(6) Uani 1 1 d . . . C11 C 0.3984(4) 0.4502(3) 0.8864(2) 0.0226(6) Uani 1 1 d . . . C6 C 0.8733(4) 0.9466(3) 0.7241(3) 0.0249(6) Uani 1 1 d . . . H15C H 0.258(3) 0.887(3) 0.671(2) 0.015(7) Uiso 1 1 d . . . H13B H 0.216(3) 0.654(3) 0.7425(19) 0.012(6) Uiso 1 1 d . . . H11A H 0.505(3) 0.386(3) 0.929(2) 0.018(7) Uiso 1 1 d . . . H3 H 1.095(3) 0.246(3) 0.822(2) 0.018(6) Uiso 1 1 d . . . H15A H 0.405(3) 0.950(3) 0.626(2) 0.020(7) Uiso 1 1 d . . . H15B H 0.251(3) 0.947(3) 0.549(2) 0.020(7) Uiso 1 1 d . . . H12A H 0.439(3) 0.287(3) 0.7549(19) 0.014(6) Uiso 1 1 d . . . H12C H 0.630(4) 0.281(3) 0.787(2) 0.021(7) Uiso 1 1 d . . . H12B H 0.555(4) 0.358(3) 0.673(2) 0.026(7) Uiso 1 1 d . . . H13A H 0.205(3) 0.527(3) 0.701(2) 0.025(7) Uiso 1 1 d . . . H11C H 0.313(4) 0.398(3) 0.894(2) 0.030(7) Uiso 1 1 d . . . H11B H 0.352(4) 0.537(3) 0.908(2) 0.027(7) Uiso 1 1 d . . . H8 H 0.600(4) 0.997(3) 0.839(2) 0.038(8) Uiso 1 1 d . . . H10B H 0.359(3) 1.018(3) 0.938(2) 0.025(7) Uiso 1 1 d . . . H14B H 0.224(3) 0.712(3) 0.553(2) 0.017(6) Uiso 1 1 d . . . H16A H 0.620(3) 0.814(3) 0.522(2) 0.024(7) Uiso 1 1 d . . . H6A H 0.981(4) 0.896(3) 0.770(3) 0.041(9) Uiso 1 1 d . . . H1A H 1.090(4) 0.221(4) 1.001(2) 0.043(9) Uiso 1 1 d . . . H16C H 0.618(4) 0.669(3) 0.498(2) 0.027(7) Uiso 1 1 d . . . H6B H 0.908(4) 0.947(3) 0.654(3) 0.036(9) Uiso 1 1 d . . . H10C H 0.220(4) 0.963(3) 0.892(2) 0.034(8) Uiso 1 1 d . . . H5A H 1.047(4) 0.367(3) 0.556(3) 0.039(9) Uiso 1 1 d . . . H5B H 0.972(4) 0.239(4) 0.605(3) 0.048(9) Uiso 1 1 d . . . H1B H 0.914(4) 0.285(3) 1.043(2) 0.031(8) Uiso 1 1 d . . . H14A H 0.399(4) 0.575(3) 0.563(2) 0.029(7) Uiso 1 1 d . . . H1C H 1.043(4) 0.364(4) 1.029(3) 0.046(9) Uiso 1 1 d . . . H10A H 0.341(4) 0.871(4) 0.991(3) 0.041(9) Uiso 1 1 d . . . H16B H 0.465(4) 0.821(3) 0.445(3) 0.041(9) Uiso 1 1 d . . . H6C H 0.827(4) 1.039(4) 0.724(3) 0.054(10) Uiso 1 1 d . . . H5C H 1.148(5) 0.242(4) 0.645(3) 0.048(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01386(11) 0.01206(10) 0.01284(12) -0.00377(7) 0.00077(7) -0.00362(7) N1 0.0163(10) 0.0143(9) 0.0151(11) -0.0044(8) 0.0010(8) -0.0041(8) N2 0.0162(10) 0.0168(10) 0.0156(11) -0.0042(8) 0.0010(8) -0.0058(8) C2 0.0168(12) 0.0159(11) 0.0191(14) -0.0031(10) -0.0019(10) -0.0068(10) O4 0.0167(8) 0.0147(8) 0.0133(9) -0.0039(7) 0.0002(7) -0.0039(7) O2 0.0159(8) 0.0151(8) 0.0153(9) -0.0040(7) 0.0015(7) -0.0026(7) O1 0.0155(8) 0.0154(8) 0.0150(9) -0.0036(7) -0.0005(7) -0.0028(7) O3 0.0161(8) 0.0159(8) 0.0191(10) -0.0044(7) 0.0008(7) -0.0044(7) C7 0.0180(12) 0.0153(11) 0.0176(14) -0.0004(10) -0.0051(10) -0.0044(10) C9 0.0191(12) 0.0146(11) 0.0144(13) -0.0035(10) -0.0032(10) -0.0016(10) C12 0.0265(15) 0.0167(12) 0.0250(17) -0.0089(11) 0.0031(12) -0.0088(11) C5 0.0229(15) 0.0226(13) 0.0216(16) -0.0084(12) 0.0049(12) -0.0031(12) C8 0.0222(13) 0.0139(12) 0.0205(15) -0.0059(10) -0.0016(10) -0.0052(10) C15 0.0192(13) 0.0186(12) 0.0178(15) -0.0016(11) -0.0010(11) -0.0023(11) C4 0.0175(12) 0.0143(11) 0.0211(14) -0.0060(10) 0.0042(10) -0.0078(10) C3 0.0127(12) 0.0141(12) 0.0221(15) -0.0039(10) -0.0005(10) 0.0000(10) C1 0.0206(14) 0.0212(13) 0.0225(16) -0.0050(11) -0.0027(12) -0.0016(12) C13 0.0161(13) 0.0197(13) 0.0289(16) -0.0041(11) -0.0018(11) -0.0074(11) C14 0.0250(14) 0.0217(13) 0.0227(15) -0.0022(11) -0.0077(12) -0.0106(11) C10 0.0271(15) 0.0173(13) 0.0234(17) -0.0073(12) 0.0025(12) -0.0033(11) C16 0.0269(15) 0.0224(13) 0.0174(15) -0.0029(11) 0.0032(11) -0.0066(12) C11 0.0278(15) 0.0214(13) 0.0197(15) -0.0028(11) 0.0049(12) -0.0117(12) C6 0.0222(15) 0.0191(14) 0.0340(19) -0.0058(12) 0.0008(13) -0.0084(11) _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 O1 2.0495(16) . ? Ru1 O4 2.0509(16) . ? Ru1 O3 2.0552(15) . ? Ru1 O2 2.0614(16) . ? Ru1 N1 2.1416(18) . ? Ru1 N2 2.147(2) . ? N1 C12 1.476(3) . ? N1 C11 1.485(3) . ? N1 C13 1.496(3) . ? N2 C16 1.478(3) . ? N2 C15 1.482(3) . ? N2 C14 1.490(3) . ? C2 O1 1.274(3) . ? C2 C3 1.404(3) . ? C2 C1 1.506(3) . ? O4 C9 1.276(3) . ? O2 C4 1.279(3) . ? O3 C7 1.278(3) . ? C7 C8 1.399(3) . ? C7 C6 1.509(3) . ? C9 C8 1.400(3) . ? C9 C10 1.504(3) . ? C5 C4 1.505(3) . ? C4 C3 1.396(3) . ? C13 C14 1.512(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O4 86.68(6) . . ? O1 Ru1 O3 89.90(6) . . ? O4 Ru1 O3 93.26(6) . . ? O1 Ru1 O2 93.20(6) . . ? O4 Ru1 O2 179.88(7) . . ? O3 Ru1 O2 86.76(6) . . ? O1 Ru1 N1 92.78(7) . . ? O4 Ru1 N1 86.91(7) . . ? O3 Ru1 N1 177.32(7) . . ? O2 Ru1 N1 93.07(7) . . ? O1 Ru1 N2 176.81(7) . . ? O4 Ru1 N2 91.40(7) . . ? O3 Ru1 N2 92.75(7) . . ? O2 Ru1 N2 88.72(7) . . ? N1 Ru1 N2 84.57(7) . . ? C12 N1 C11 107.50(19) . . ? C12 N1 C13 109.72(19) . . ? C11 N1 C13 108.9(2) . . ? C12 N1 Ru1 113.91(15) . . ? C11 N1 Ru1 112.71(14) . . ? C13 N1 Ru1 103.95(13) . . ? C16 N2 C15 107.1(2) . . ? C16 N2 C14 109.50(19) . . ? C15 N2 C14 109.67(19) . . ? C16 N2 Ru1 112.14(15) . . ? C15 N2 Ru1 112.80(15) . . ? C14 N2 Ru1 105.67(14) . . ? O1 C2 C3 126.2(2) . . ? O1 C2 C1 115.3(2) . . ? C3 C2 C1 118.5(2) . . ? C9 O4 Ru1 123.27(15) . . ? C4 O2 Ru1 122.47(15) . . ? C2 O1 Ru1 123.21(15) . . ? C7 O3 Ru1 122.30(15) . . ? O3 C7 C8 127.0(2) . . ? O3 C7 C6 114.6(2) . . ? C8 C7 C6 118.4(2) . . ? O4 C9 C8 126.1(2) . . ? O4 C9 C10 115.1(2) . . ? C8 C9 C10 118.8(2) . . ? C7 C8 C9 128.1(2) . . ? O2 C4 C3 126.6(2) . . ? O2 C4 C5 115.1(2) . . ? C3 C4 C5 118.2(2) . . ? C4 C3 C2 128.3(2) . . ? N1 C13 C14 110.2(2) . . ? N2 C14 C13 110.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru1 N1 C12 -80.91(17) . . . . ? O4 Ru1 N1 C12 -167.43(17) . . . . ? O3 Ru1 N1 C12 98.8(14) . . . . ? O2 Ru1 N1 C12 12.45(17) . . . . ? N2 Ru1 N1 C12 100.87(17) . . . . ? O1 Ru1 N1 C11 41.92(16) . . . . ? O4 Ru1 N1 C11 -44.60(16) . . . . ? O3 Ru1 N1 C11 -138.4(14) . . . . ? O2 Ru1 N1 C11 135.28(16) . . . . ? N2 Ru1 N1 C11 -136.30(16) . . . . ? O1 Ru1 N1 C13 159.71(15) . . . . ? O4 Ru1 N1 C13 73.19(15) . . . . ? O3 Ru1 N1 C13 -20.6(15) . . . . ? O2 Ru1 N1 C13 -106.93(15) . . . . ? N2 Ru1 N1 C13 -18.51(15) . . . . ? O1 Ru1 N2 C16 -163.0(11) . . . . ? O4 Ru1 N2 C16 144.14(15) . . . . ? O3 Ru1 N2 C16 50.81(16) . . . . ? O2 Ru1 N2 C16 -35.89(16) . . . . ? N1 Ru1 N2 C16 -129.09(16) . . . . ? O1 Ru1 N2 C15 76.0(12) . . . . ? O4 Ru1 N2 C15 23.19(16) . . . . ? O3 Ru1 N2 C15 -70.15(16) . . . . ? O2 Ru1 N2 C15 -156.84(16) . . . . ? N1 Ru1 N2 C15 109.95(16) . . . . ? O1 Ru1 N2 C14 -43.8(12) . . . . ? O4 Ru1 N2 C14 -96.62(15) . . . . ? O3 Ru1 N2 C14 170.04(15) . . . . ? O2 Ru1 N2 C14 83.35(15) . . . . ? N1 Ru1 N2 C14 -9.86(15) . . . . ? O1 Ru1 O4 C9 87.90(17) . . . . ? O3 Ru1 O4 C9 -1.81(17) . . . . ? O2 Ru1 O4 C9 100(34) . . . . ? N1 Ru1 O4 C9 -179.13(17) . . . . ? N2 Ru1 O4 C9 -94.65(17) . . . . ? O1 Ru1 O2 C4 -0.64(16) . . . . ? O4 Ru1 O2 C4 -13(29) . . . . ? O3 Ru1 O2 C4 89.08(16) . . . . ? N1 Ru1 O2 C4 -93.60(16) . . . . ? N2 Ru1 O2 C4 -178.09(16) . . . . ? C3 C2 O1 Ru1 2.5(3) . . . . ? C1 C2 O1 Ru1 -176.49(16) . . . . ? O4 Ru1 O1 C2 178.14(17) . . . . ? O3 Ru1 O1 C2 -88.59(17) . . . . ? O2 Ru1 O1 C2 -1.83(17) . . . . ? N1 Ru1 O1 C2 91.40(17) . . . . ? N2 Ru1 O1 C2 125.2(11) . . . . ? O1 Ru1 O3 C7 -85.79(17) . . . . ? O4 Ru1 O3 C7 0.87(18) . . . . ? O2 Ru1 O3 C7 -179.00(17) . . . . ? N1 Ru1 O3 C7 94.5(14) . . . . ? N2 Ru1 O3 C7 92.43(18) . . . . ? Ru1 O3 C7 C8 -0.2(3) . . . . ? Ru1 O3 C7 C6 178.99(17) . . . . ? Ru1 O4 C9 C8 2.2(3) . . . . ? Ru1 O4 C9 C10 -179.42(16) . . . . ? O3 C7 C8 C9 0.0(4) . . . . ? C6 C7 C8 C9 -179.2(2) . . . . ? O4 C9 C8 C7 -1.1(4) . . . . ? C10 C9 C8 C7 -179.5(2) . . . . ? Ru1 O2 C4 C3 2.7(3) . . . . ? Ru1 O2 C4 C5 -179.38(15) . . . . ? O2 C4 C3 C2 -2.6(4) . . . . ? C5 C4 C3 C2 179.5(2) . . . . ? O1 C2 C3 C4 -0.4(4) . . . . ? C1 C2 C3 C4 178.6(2) . . . . ? C12 N1 C13 C14 -77.6(2) . . . . ? C11 N1 C13 C14 164.98(19) . . . . ? Ru1 N1 C13 C14 44.6(2) . . . . ? C16 N2 C14 C13 158.2(2) . . . . ? C15 N2 C14 C13 -84.6(3) . . . . ? Ru1 N2 C14 C13 37.3(2) . . . . ? N1 C13 C14 N2 -57.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.538 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.072