# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1 _database_code_depnum_ccdc_archive 'CCDC 908090' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H Ir N O' _chemical_formula_weight 235.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 8.76200(10) _cell_length_b 9.7180(2) _cell_length_c 38.7815(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.8220(10) _cell_angle_gamma 90.00 _cell_volume 3294.87(9) _cell_formula_units_Z 37 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3663 _exptl_absorpt_coefficient_mu 70.710 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _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 13540 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 72.65 _reflns_number_total 6348 _reflns_number_gt 5534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^2^+12.3642P] 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 6348 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ir1 Ir -0.90451(3) 0.36518(3) 0.149870(6) 0.04213(11) Uani 1 1 d . . . C25 C -0.7780(9) 0.1806(8) 0.03784(18) 0.0546(18) Uani 1 1 d . . . N3 N -1.1028(6) 0.2571(6) 0.13018(13) 0.0428(12) Uani 1 1 d . . . N2 N -0.9470(7) 0.5452(6) 0.12402(16) 0.0504(13) Uani 1 1 d . . . N1 N -0.8629(6) 0.1928(6) 0.17954(13) 0.0436(12) Uani 1 1 d . . . C22 C -0.7034(7) 0.4634(8) 0.16173(17) 0.0484(16) Uani 1 1 d . . . O3 O -0.6134(7) 0.1464(8) -0.00622(16) 0.089(2) Uani 1 1 d . . . O2 O -1.5847(6) -0.0101(6) 0.10880(16) 0.0749(18) Uani 1 1 d . . . N4 N -0.8397(6) 0.2821(5) 0.10210(11) 0.0366(11) Uani 1 1 d . . . C34 C -1.4686(9) -0.0101(8) 0.09213(19) 0.0555(18) Uani 1 1 d . . . C11 C -0.9805(8) 0.4325(8) 0.19464(17) 0.0520(17) Uani 1 1 d . . . C28 C -1.0924(7) 0.1876(7) 0.10007(15) 0.0406(13) Uani 1 1 d . . . C26 C -0.9189(8) 0.1543(7) 0.05150(16) 0.0471(15) Uani 1 1 d . . . H26 H -0.9925 0.1012 0.0393 0.057 Uiso 1 1 calc R . . C16 C -0.8269(10) 0.6344(8) 0.1239(2) 0.063(2) Uani 1 1 d . . . O1 O -1.4475(8) -0.0857(8) 0.06721(16) 0.092(2) Uani 1 1 d . . . C27 C -0.9468(8) 0.2088(7) 0.08350(15) 0.0416(14) Uani 1 1 d . . . C17 C -0.6890(8) 0.5880(9) 0.1447(2) 0.0595(19) Uani 1 1 d . . . C30 C -1.3409(8) 0.0868(7) 0.10437(17) 0.0471(15) Uani 1 1 d . . . C31 C -1.3524(8) 0.1605(8) 0.1345(2) 0.059(2) Uani 1 1 d . . . H31 H -1.4403 0.1542 0.1466 0.071 Uiso 1 1 calc R . . C29 C -1.2096(8) 0.1026(7) 0.08666(16) 0.0450(14) Uani 1 1 d . . . H29 H -1.1999 0.0565 0.0659 0.054 Uiso 1 1 calc R . . C6 C -0.9824(9) 0.3304(10) 0.22059(18) 0.062(2) Uani 1 1 d . . . C5 C -0.9151(9) 0.1975(10) 0.21154(18) 0.061(2) Uani 1 1 d . . . O4 O -0.8447(9) 0.0637(11) -0.01429(18) 0.126(4) Uani 1 1 d . . . C32 C -1.2336(8) 0.2430(8) 0.1465(2) 0.0587(19) Uani 1 1 d . . . H32 H -1.2434 0.2918 0.1668 0.070 Uiso 1 1 calc R . . C24 C -0.6678(9) 0.2554(8) 0.05709(18) 0.0566(19) Uani 1 1 d . . . H24 H -0.5721 0.2720 0.0489 0.068 Uiso 1 1 calc R . . C33 C -0.7494(9) 0.1201(10) 0.0032(2) 0.065(2) Uani 1 1 d . . . C23 C -0.7052(8) 0.3045(7) 0.08891(17) 0.0479(15) Uani 1 1 d . . . H23 H -0.6325 0.3560 0.1018 0.057 Uiso 1 1 calc R . . C1 C -0.7952(9) 0.0769(8) 0.16886(19) 0.0564(17) Uani 1 1 d . . . H1 H -0.7594 0.0744 0.1468 0.068 Uiso 1 1 calc R . . C21 C -0.5805(8) 0.4170(10) 0.1832(2) 0.067(2) Uani 1 1 d . . . H21 H -0.5886 0.3353 0.1954 0.080 Uiso 1 1 calc R . . C10 C -1.0318(9) 0.5634(10) 0.2032(2) 0.068(2) Uani 1 1 d . . . H10 H -1.0290 0.6338 0.1870 0.082 Uiso 1 1 calc R . . C12 C -1.0810(10) 0.5789(9) 0.1072(2) 0.069(2) Uani 1 1 d . . . H12 H -1.1628 0.5183 0.1077 0.083 Uiso 1 1 calc R . . C19 C -0.4334(10) 0.6126(13) 0.1688(3) 0.089(4) Uani 1 1 d . . . H19 H -0.3421 0.6616 0.1709 0.107 Uiso 1 1 calc R . . C18 C -0.5553(11) 0.6632(10) 0.1477(3) 0.079(3) Uani 1 1 d . . . H18 H -0.5468 0.7459 0.1359 0.095 Uiso 1 1 calc R . . C7 C -1.0420(11) 0.3556(12) 0.2526(2) 0.084(3) Uani 1 1 d . . . H7 H -1.0465 0.2858 0.2690 0.101 Uiso 1 1 calc R . . C15 C -0.8461(13) 0.7574(10) 0.1057(3) 0.089(3) Uani 1 1 d . . . H15 H -0.7653 0.8194 0.1056 0.107 Uiso 1 1 calc R . . C2 C -0.7778(12) -0.0364(10) 0.1894(2) 0.082(3) Uani 1 1 d . . . H2 H -0.7298 -0.1147 0.1816 0.098 Uiso 1 1 calc R . . C9 C -1.0865(11) 0.5909(14) 0.2349(3) 0.094(4) Uani 1 1 d . . . H9 H -1.1184 0.6795 0.2399 0.112 Uiso 1 1 calc R . . C20 C -0.4457(10) 0.4924(12) 0.1864(3) 0.079(3) Uani 1 1 d . . . H20 H -0.3636 0.4608 0.2007 0.095 Uiso 1 1 calc R . . C4 C -0.9012(13) 0.0807(13) 0.2329(2) 0.088(3) Uani 1 1 d . . . H4 H -0.9394 0.0822 0.2547 0.105 Uiso 1 1 calc R . . C8 C -1.0945(13) 0.4877(16) 0.2595(3) 0.102(4) Uani 1 1 d . . . H8 H -1.1349 0.5067 0.2806 0.122 Uiso 1 1 calc R . . C13 C -1.1006(13) 0.7001(11) 0.0893(3) 0.096(3) Uani 1 1 d . . . H13 H -1.1945 0.7220 0.0780 0.115 Uiso 1 1 calc R . . C3 C -0.8324(14) -0.0331(13) 0.2218(3) 0.095(3) Uani 1 1 d . . . H3 H -0.8218 -0.1098 0.2360 0.114 Uiso 1 1 calc R . . C14 C -0.9784(14) 0.7881(11) 0.0884(3) 0.101(4) Uani 1 1 d . . . H14 H -0.9879 0.8692 0.0757 0.121 Uiso 1 1 calc R . . HW H -0.6130 0.0827 -0.0248 0.152 Uiso 1 1 d 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 Ir1 0.03903(16) 0.04614(17) 0.04133(16) -0.00953(12) 0.00349(10) -0.00276(12) C25 0.052(4) 0.066(4) 0.047(4) 0.004(3) 0.014(3) -0.021(3) N3 0.040(3) 0.046(3) 0.043(3) -0.010(2) 0.007(2) -0.003(2) N2 0.047(3) 0.033(3) 0.071(4) -0.007(3) -0.001(3) 0.000(2) N1 0.042(3) 0.050(3) 0.040(3) 0.004(2) 0.006(2) 0.000(2) C22 0.028(3) 0.064(4) 0.053(4) -0.025(3) -0.002(3) -0.005(3) O3 0.068(4) 0.133(6) 0.069(3) -0.044(4) 0.031(3) -0.030(4) O2 0.061(3) 0.076(4) 0.093(4) -0.028(3) 0.042(3) -0.032(3) N4 0.041(3) 0.034(3) 0.035(2) -0.007(2) 0.009(2) -0.003(2) C34 0.051(4) 0.060(4) 0.057(4) -0.013(3) 0.018(3) -0.009(3) C11 0.044(4) 0.064(5) 0.048(4) -0.023(3) 0.000(3) 0.003(3) C28 0.043(3) 0.039(3) 0.040(3) -0.006(3) 0.004(2) -0.008(3) C26 0.048(4) 0.051(4) 0.043(3) -0.007(3) 0.009(3) -0.010(3) C16 0.061(5) 0.046(4) 0.083(5) -0.010(4) 0.006(4) -0.010(4) O1 0.087(4) 0.117(5) 0.076(4) -0.053(4) 0.042(3) -0.054(4) C27 0.047(4) 0.041(3) 0.037(3) -0.001(2) 0.004(3) -0.008(3) C17 0.045(4) 0.062(5) 0.072(5) -0.019(4) 0.003(3) -0.012(3) C30 0.044(3) 0.045(3) 0.054(4) -0.008(3) 0.012(3) -0.012(3) C31 0.048(4) 0.073(5) 0.060(4) -0.021(4) 0.021(3) -0.010(4) C29 0.052(4) 0.041(3) 0.043(3) -0.007(3) 0.012(3) -0.003(3) C6 0.048(4) 0.095(6) 0.044(4) -0.020(4) 0.007(3) 0.004(4) C5 0.057(5) 0.086(6) 0.041(3) -0.001(4) 0.009(3) -0.002(4) O4 0.092(5) 0.209(9) 0.083(4) -0.085(6) 0.046(4) -0.084(6) C32 0.047(4) 0.069(5) 0.062(4) -0.026(4) 0.017(3) -0.007(4) C24 0.050(4) 0.068(5) 0.053(4) -0.011(3) 0.011(3) -0.023(4) C33 0.057(4) 0.086(6) 0.053(4) -0.015(4) 0.019(3) -0.022(4) C23 0.046(4) 0.053(4) 0.046(3) -0.010(3) 0.013(3) -0.014(3) C1 0.057(4) 0.060(4) 0.053(4) 0.002(3) 0.010(3) 0.006(4) C21 0.042(4) 0.099(6) 0.058(4) -0.040(4) -0.002(3) 0.010(4) C10 0.048(4) 0.077(6) 0.079(5) -0.036(5) 0.005(4) 0.009(4) C12 0.057(5) 0.056(5) 0.094(6) 0.008(4) -0.011(4) -0.003(4) C19 0.042(4) 0.107(9) 0.118(8) -0.061(7) 0.003(5) -0.012(5) C18 0.063(5) 0.074(6) 0.101(7) -0.026(5) 0.008(5) -0.019(5) C7 0.075(6) 0.126(9) 0.053(4) -0.020(5) 0.013(4) 0.003(6) C15 0.088(7) 0.061(6) 0.117(8) 0.005(5) 0.000(6) -0.026(5) C2 0.100(7) 0.069(6) 0.078(6) 0.009(5) 0.010(5) 0.029(5) C9 0.063(6) 0.127(9) 0.089(7) -0.061(7) -0.004(5) 0.016(6) C20 0.048(5) 0.102(8) 0.086(6) -0.049(6) -0.008(4) 0.013(5) C4 0.098(7) 0.112(8) 0.055(5) 0.021(5) 0.025(5) 0.011(7) C8 0.078(7) 0.155(12) 0.073(6) -0.048(8) 0.009(5) 0.017(7) C13 0.075(7) 0.075(7) 0.133(9) 0.022(6) -0.027(6) 0.006(5) C3 0.112(9) 0.104(8) 0.071(6) 0.038(6) 0.012(6) 0.024(7) C14 0.098(8) 0.062(6) 0.139(10) 0.034(6) -0.023(7) -0.012(6) _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 Ir1 C11 2.010(6) . ? Ir1 C22 2.029(6) . ? Ir1 N2 2.038(6) . ? Ir1 N1 2.051(5) . ? Ir1 N3 2.128(5) . ? Ir1 N4 2.132(4) . ? C25 C24 1.387(10) . ? C25 C26 1.399(9) . ? C25 C33 1.503(10) . ? N3 C32 1.352(8) . ? N3 C28 1.357(8) . ? N2 C12 1.345(10) . ? N2 C16 1.364(9) . ? N1 C1 1.351(9) . ? N1 C5 1.352(8) . ? C22 C21 1.392(10) . ? C22 C17 1.389(11) . ? O3 C33 1.295(9) . ? O2 C34 1.241(8) . ? N4 C23 1.334(8) . ? N4 C27 1.348(8) . ? C34 O1 1.238(9) . ? C34 C30 1.514(9) . ? C11 C10 1.396(11) . ? C11 C6 1.414(12) . ? C28 C29 1.391(9) . ? C28 C27 1.481(9) . ? C26 C27 1.386(9) . ? C16 C15 1.393(13) . ? C16 C17 1.477(12) . ? C17 C18 1.379(11) . ? C30 C31 1.380(9) . ? C30 C29 1.387(9) . ? C31 C32 1.371(10) . ? C6 C7 1.402(10) . ? C6 C5 1.472(12) . ? C5 C4 1.406(13) . ? O4 C33 1.176(10) . ? C24 C23 1.383(9) . ? C1 C2 1.361(12) . ? C21 C20 1.388(13) . ? C10 C9 1.377(13) . ? C12 C13 1.372(13) . ? C19 C20 1.361(15) . ? C19 C18 1.391(15) . ? C7 C8 1.396(16) . ? C15 C14 1.334(14) . ? C2 C3 1.373(13) . ? C9 C8 1.390(17) . ? C4 C3 1.344(15) . ? C13 C14 1.373(15) . ? 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 C11 Ir1 C22 89.1(3) . . ? C11 Ir1 N2 94.9(3) . . ? C22 Ir1 N2 80.5(3) . . ? C11 Ir1 N1 80.7(3) . . ? C22 Ir1 N1 97.9(3) . . ? N2 Ir1 N1 175.4(2) . . ? C11 Ir1 N3 99.3(2) . . ? C22 Ir1 N3 171.6(2) . . ? N2 Ir1 N3 97.4(2) . . ? N1 Ir1 N3 84.8(2) . . ? C11 Ir1 N4 175.2(2) . . ? C22 Ir1 N4 95.6(2) . . ? N2 Ir1 N4 87.0(2) . . ? N1 Ir1 N4 97.5(2) . . ? N3 Ir1 N4 76.10(19) . . ? C24 C25 C26 119.5(6) . . ? C24 C25 C33 122.3(6) . . ? C26 C25 C33 118.1(6) . . ? C32 N3 C28 117.4(6) . . ? C32 N3 Ir1 125.4(4) . . ? C28 N3 Ir1 117.0(4) . . ? C12 N2 C16 119.4(7) . . ? C12 N2 Ir1 125.0(5) . . ? C16 N2 Ir1 115.6(5) . . ? C1 N1 C5 119.5(6) . . ? C1 N1 Ir1 125.0(4) . . ? C5 N1 Ir1 115.4(5) . . ? C21 C22 C17 118.4(7) . . ? C21 C22 Ir1 127.5(7) . . ? C17 C22 Ir1 114.0(5) . . ? C23 N4 C27 118.8(5) . . ? C23 N4 Ir1 124.4(4) . . ? C27 N4 Ir1 116.7(4) . . ? O1 C34 O2 125.3(7) . . ? O1 C34 C30 117.9(6) . . ? O2 C34 C30 116.8(6) . . ? C10 C11 C6 116.8(7) . . ? C10 C11 Ir1 129.2(7) . . ? C6 C11 Ir1 114.0(5) . . ? N3 C28 C29 121.8(6) . . ? N3 C28 C27 114.4(5) . . ? C29 C28 C27 123.8(5) . . ? C27 C26 C25 118.8(6) . . ? N2 C16 C15 118.7(8) . . ? N2 C16 C17 114.0(7) . . ? C15 C16 C17 127.3(8) . . ? N4 C27 C26 121.6(6) . . ? N4 C27 C28 115.5(5) . . ? C26 C27 C28 122.9(6) . . ? C18 C17 C22 121.7(8) . . ? C18 C17 C16 122.9(9) . . ? C22 C17 C16 115.4(6) . . ? C31 C30 C29 118.2(6) . . ? C31 C30 C34 119.6(6) . . ? C29 C30 C34 122.3(6) . . ? C32 C31 C30 119.6(6) . . ? C28 C29 C30 119.8(6) . . ? C7 C6 C11 122.1(9) . . ? C7 C6 C5 122.9(9) . . ? C11 C6 C5 115.0(6) . . ? N1 C5 C4 119.5(8) . . ? N1 C5 C6 114.4(7) . . ? C4 C5 C6 126.0(7) . . ? N3 C32 C31 123.3(6) . . ? C23 C24 C25 117.6(6) . . ? O4 C33 O3 124.1(7) . . ? O4 C33 C25 122.9(7) . . ? O3 C33 C25 112.7(7) . . ? N4 C23 C24 123.7(6) . . ? C2 C1 N1 121.9(7) . . ? C22 C21 C20 120.2(10) . . ? C9 C10 C11 121.7(10) . . ? N2 C12 C13 122.1(8) . . ? C20 C19 C18 121.0(9) . . ? C19 C18 C17 118.5(10) . . ? C8 C7 C6 118.6(11) . . ? C14 C15 C16 121.2(9) . . ? C1 C2 C3 119.0(9) . . ? C10 C9 C8 120.7(11) . . ? C19 C20 C21 120.2(9) . . ? C3 C4 C5 119.8(8) . . ? C9 C8 C7 119.9(9) . . ? C12 C13 C14 118.4(9) . . ? C4 C3 C2 120.3(9) . . ? C15 C14 C13 120.1(10) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 72.65 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.012 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.112 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.040 0.500 0.000 268 52 ' ' 2 -0.004 0.000 0.500 268 52 ' ' 3 0.150 0.100 0.830 29 4 ' ' 4 0.349 0.600 0.670 29 4 ' ' 5 0.651 0.400 0.330 29 4 ' ' 6 0.849 0.900 0.170 29 4 ' ' _platon_squeeze_details ; ;