Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Akhil R. Chakravarty' _publ_contact_author_address ; Department of Inorganic & Physical Chemistry Indian Institute of Science Bangalore 560012 INDIA ; _publ_contact_author_email ARC@IPC.IISC.ERNET.IN _publ_contact_author_phone 91-080-22932533 _publ_contact_author_fax 91-080-23600683 _publ_section_title ; Red-light photosensitization of L-lysine in the cleavage of DNA by (L-lysine)(phenanthroline base)copper(II) complexes ; loop_ _publ_author_name 'Akhil R. Chakravarty' 'Munirathinam Nethaji' 'Ashis K. Patra' data_arccif _database_code_depnum_ccdc_archive 'CCDC 262794' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H23 Cl2 Cu N4 O10.50' _chemical_formula_sum 'C18 H23 Cl2 Cu N4 O10.50' _chemical_formula_weight 597.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.735(5) _cell_length_b 13.574(6) _cell_length_c 33.028(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4813(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 28 _exptl_crystal_description rectangular _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7389 _exptl_absorpt_correction_T_max 0.7710 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD Area Detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40875 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.04 _reflns_number_total 11344 _reflns_number_gt 7034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep-3 _computing_publication_material WinGX _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^)+(0.0948P)^2^+3.1454P] 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 0.035(19) _refine_ls_number_reflns 11344 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _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 Cu1 Cu 0.43368(7) 0.64506(6) 0.88634(2) 0.0484(2) Uani 1 1 d . . . Cu2 Cu 0.12142(8) 0.15208(6) 0.87823(2) 0.0560(2) Uani 1 1 d . . . C1 C 0.2599(7) 0.6313(6) 0.9583(2) 0.068(2) Uani 1 1 d . . . H1 H 0.1932 0.6334 0.9404 0.082 Uiso 1 1 calc R . . C2 C 0.2359(9) 0.6247(6) 0.9995(3) 0.082(2) Uani 1 1 d . . . H2 H 0.1542 0.6214 1.0087 0.098 Uiso 1 1 calc R . . C3 C 0.3308(11) 0.6229(5) 1.0259(2) 0.084(3) Uani 1 1 d . . . H3 H 0.3149 0.6203 1.0536 0.101 Uiso 1 1 calc R . . C4 C 0.4524(9) 0.6249(4) 1.01200(19) 0.065(2) Uani 1 1 d . . . C5 C 0.5619(11) 0.6213(6) 1.0367(2) 0.082(3) Uani 1 1 d . . . H5 H 0.5530 0.6182 1.0646 0.098 Uiso 1 1 calc R . . C6 C 0.6763(12) 0.6222(6) 1.0208(3) 0.089(3) Uani 1 1 d . . . H6 H 0.7448 0.6193 1.0380 0.107 Uiso 1 1 calc R . . C7 C 0.6961(8) 0.6274(5) 0.9779(2) 0.069(2) Uani 1 1 d . . . C8 C 0.8129(8) 0.6259(6) 0.9590(3) 0.076(2) Uani 1 1 d . . . H8 H 0.8851 0.6215 0.9745 0.091 Uiso 1 1 calc R . . C9 C 0.8206(7) 0.6308(6) 0.9177(3) 0.079(2) Uani 1 1 d . . . H9 H 0.8974 0.6300 0.9047 0.095 Uiso 1 1 calc R . . C10 C 0.7122(7) 0.6369(6) 0.8960(2) 0.0683(19) Uani 1 1 d . . . H10 H 0.7180 0.6400 0.8679 0.082 Uiso 1 1 calc R . . C11 C 0.5943(6) 0.6314(4) 0.95337(17) 0.0451(15) Uani 1 1 d . . . C12 C 0.4711(6) 0.6313(4) 0.97045(16) 0.0489(15) Uani 1 1 d . . . C13 C 0.4222(6) 0.6644(4) 0.80443(19) 0.0482(15) Uani 1 1 d . . . C14 C 0.2985(6) 0.6154(4) 0.81487(18) 0.0480(15) Uani 1 1 d . . . H14 H 0.3107 0.5441 0.8125 0.058 Uiso 1 1 calc R . . C15 C 0.1909(6) 0.6438(6) 0.7861(2) 0.0634(17) Uani 1 1 d . . . H15A H 0.1806 0.7148 0.7869 0.076 Uiso 1 1 calc R . . H15B H 0.2149 0.6265 0.7587 0.076 Uiso 1 1 calc R . . C16 C 0.0673(8) 0.5968(5) 0.7950(2) 0.0667(19) Uani 1 1 d . . . H16A H 0.0459 0.6090 0.8231 0.080 Uiso 1 1 calc R . . H16B H 0.0040 0.6274 0.7783 0.080 Uiso 1 1 calc R . . C17 C 0.0666(7) 0.4879(6) 0.7875(2) 0.0662(19) Uani 1 1 d . . . H17A H 0.1206 0.4558 0.8070 0.079 Uiso 1 1 calc R . . H17B H 0.0992 0.4748 0.7607 0.079 Uiso 1 1 calc R . . C18 C -0.0632(8) 0.4454(5) 0.7909(2) 0.069(2) Uani 1 1 d . . . H18A H -0.0967 0.4602 0.8175 0.082 Uiso 1 1 calc R . . H18B H -0.1167 0.4763 0.7709 0.082 Uiso 1 1 calc R . . C19 C 0.2601(8) 0.1344(6) 0.9588(2) 0.069(2) Uani 1 1 d . . . H19 H 0.3346 0.1389 0.9446 0.083 Uiso 1 1 calc R . . C20 C 0.2653(10) 0.1273(5) 1.0011(3) 0.079(3) Uani 1 1 d . . . C21 C 0.1519(11) 0.1254(5) 1.0218(2) 0.082(3) Uani 1 1 d . . . H21 H 0.1515 0.1225 1.0499 0.098 Uiso 1 1 calc R . . C22 C 0.0403(9) 0.1279(4) 1.0010(2) 0.071(2) Uani 1 1 d . . . C23 C -0.0832(12) 0.1246(5) 1.0197(3) 0.086(3) Uani 1 1 d . . . H23 H -0.0886 0.1214 1.0478 0.103 Uiso 1 1 calc R . . C24 C -0.1838(12) 0.1259(7) 0.9991(3) 0.095(3) Uani 1 1 d . . . H24 H -0.2593 0.1223 1.0128 0.114 Uiso 1 1 calc R . . C25 C -0.1858(8) 0.1330(5) 0.9548(2) 0.066(2) Uani 1 1 d . . . C26 C -0.2895(8) 0.1363(6) 0.9311(3) 0.083(2) Uani 1 1 d . . . H26 H -0.3686 0.1349 0.9426 0.100 Uiso 1 1 calc R . . C27 C -0.2748(7) 0.1420(6) 0.8898(3) 0.083(2) Uani 1 1 d . . . H27 H -0.3441 0.1427 0.8729 0.100 Uiso 1 1 calc R . . C28 C -0.1560(6) 0.1467(5) 0.8736(2) 0.0567(16) Uani 1 1 d . . . H28 H -0.1480 0.1522 0.8457 0.068 Uiso 1 1 calc R . . C29 C -0.0670(7) 0.1365(4) 0.93668(19) 0.0543(15) Uani 1 1 d . . . C30 C 0.0453(7) 0.1333(4) 0.95936(19) 0.0562(17) Uani 1 1 d . . . C31 C 0.1748(7) 0.1916(5) 0.7990(2) 0.0569(17) Uani 1 1 d . . . C32 C 0.3009(6) 0.1534(5) 0.81402(19) 0.0543(15) Uani 1 1 d . . . H32 H 0.3643 0.2026 0.8072 0.065 Uiso 1 1 calc R . . C33 C 0.3349(6) 0.0583(5) 0.7929(2) 0.0584(17) Uani 1 1 d . . . H33A H 0.3211 0.0657 0.7641 0.070 Uiso 1 1 calc R . . H33B H 0.2808 0.0061 0.8026 0.070 Uiso 1 1 calc R . . C34 C 0.4693(7) 0.0293(5) 0.8002(2) 0.0656(19) Uani 1 1 d . . . H34A H 0.5227 0.0813 0.7900 0.079 Uiso 1 1 calc R . . H34B H 0.4830 0.0247 0.8292 0.079 Uiso 1 1 calc R . . C35 C 0.5079(9) -0.0653(7) 0.7813(4) 0.112(4) Uani 1 1 d . . . H35A H 0.4580 -0.1182 0.7926 0.134 Uiso 1 1 calc R . . H35B H 0.4910 -0.0623 0.7525 0.134 Uiso 1 1 calc R . . C36 C 0.6387(9) -0.0878(8) 0.7874(5) 0.128(5) Uani 1 1 d . . . H36A H 0.6814 -0.0752 0.7620 0.154 Uiso 1 1 calc R . . H36B H 0.6711 -0.0413 0.8070 0.154 Uiso 1 1 calc R . . N1 N 0.3742(5) 0.6349(4) 0.94370(15) 0.0540(13) Uani 1 1 d . . . N2 N 0.6005(5) 0.6387(4) 0.91225(15) 0.0502(12) Uani 1 1 d . . . N3 N 0.2713(4) 0.6370(4) 0.85836(14) 0.0459(11) Uani 1 1 d . . . N4 N -0.0638(6) 0.3392(5) 0.7847(2) 0.0751(18) Uani 1 1 d . . . H4A H -0.1414 0.3166 0.7869 0.113 Uiso 1 1 calc R . . H4B H -0.0159 0.3105 0.8033 0.113 Uiso 1 1 calc R . . H4C H -0.0345 0.3255 0.7601 0.113 Uiso 1 1 calc R . . N5 N 0.1534(5) 0.1350(4) 0.93803(17) 0.0572(14) Uani 1 1 d . . . N6 N -0.0539(5) 0.1438(4) 0.89556(16) 0.0550(13) Uani 1 1 d . . . N7 N 0.2975(5) 0.1431(5) 0.85866(17) 0.0663(16) Uani 1 1 d . . . N8 N 0.6724(8) -0.1819(7) 0.8002(3) 0.117(3) Uani 1 1 d . . . H8A H 0.7538 -0.1834 0.8053 0.176 Uiso 1 1 calc R . . H8B H 0.6544 -0.2253 0.7809 0.176 Uiso 1 1 calc R . . H8C H 0.6306 -0.1970 0.8226 0.176 Uiso 1 1 calc R . . O1 O 0.4989(4) 0.6735(3) 0.83288(12) 0.0558(12) Uani 1 1 d . . . O2 O 0.4447(5) 0.6917(4) 0.76949(13) 0.0647(13) Uani 1 1 d . . . O3 O 0.0832(4) 0.1868(4) 0.82281(14) 0.0626(13) Uani 1 1 d . . . O4 O 0.1673(5) 0.2253(4) 0.76416(15) 0.0771(15) Uani 1 1 d . . . O11 O 0.4309(6) 0.4614(4) 0.88295(16) 0.0874(18) Uani 1 1 d . . . O12 O 0.6014(11) 0.4138(7) 0.8487(4) 0.214(6) Uani 1 1 d . . . O13 O 0.4109(11) 0.3774(5) 0.8227(2) 0.156(4) Uani 1 1 d . . . O14 O 0.4810(7) 0.2956(4) 0.8788(2) 0.108(2) Uani 1 1 d . . . O41 O 0.3984(6) 0.8410(5) 0.8874(2) 0.109(2) Uani 1 1 d . . . O42 O 0.4808(7) 0.8650(7) 0.94991(19) 0.128(3) Uani 1 1 d . . . O43 O 0.6042(6) 0.8879(5) 0.8936(2) 0.109(2) Uani 1 1 d . . . O44 O 0.4524(7) 0.9977(4) 0.9070(2) 0.114(2) Uani 1 1 d . . . O21 O 0.1393(7) 0.3370(4) 0.8932(3) 0.131(3) Uani 1 1 d . . . O22 O 0.0841(6) 0.5009(4) 0.8966(2) 0.104(2) Uani 1 1 d . . . O23 O 0.0385(9) 0.3938(8) 0.9483(2) 0.160(4) Uani 1 1 d . . . O24 O -0.0685(7) 0.3823(5) 0.8919(3) 0.136(3) Uani 1 1 d . . . O31 O 0.0576(10) -0.2079(6) 0.8623(2) 0.141(3) Uani 1 1 d . . . O32 O 0.0761(15) -0.0433(7) 0.8610(4) 0.206(6) Uani 1 1 d . . . O33 O -0.0969(12) -0.1011(13) 0.8499(6) 0.303(10) Uani 1 1 d . . . O34 O 0.031(2) -0.1345(10) 0.8047(3) 0.376(16) Uani 1 1 d . . . OW1 O -0.2991(5) 0.2641(5) 0.79357(16) 0.0836(17) Uani 1 1 d . . . Cl1 Cl 0.4821(2) 0.38706(15) 0.85861(7) 0.0825(6) Uani 1 1 d . . . Cl2 Cl 0.04985(16) 0.40388(12) 0.90710(5) 0.0564(4) Uani 1 1 d . . . Cl3 Cl 0.0120(2) -0.12546(17) 0.84221(6) 0.0834(6) Uani 1 1 d . . . Cl4 Cl 0.48396(15) 0.90024(12) 0.90956(5) 0.0556(4) Uani 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 Cu1 0.0464(4) 0.0602(4) 0.0386(4) 0.0005(3) 0.0019(3) 0.0000(4) Cu2 0.0557(5) 0.0606(5) 0.0516(4) 0.0056(4) -0.0073(3) 0.0108(4) C1 0.067(5) 0.066(5) 0.070(5) -0.003(4) 0.021(4) 0.001(4) C2 0.093(6) 0.081(6) 0.072(5) -0.002(5) 0.032(5) -0.003(5) C3 0.159(9) 0.039(4) 0.054(4) -0.002(3) 0.042(6) -0.006(5) C4 0.119(7) 0.034(3) 0.041(3) -0.003(3) 0.015(4) -0.006(4) C5 0.132(8) 0.068(5) 0.045(4) -0.001(3) -0.011(5) -0.012(6) C6 0.150(9) 0.054(5) 0.063(5) 0.005(4) -0.057(6) -0.009(5) C7 0.101(6) 0.030(3) 0.076(5) 0.006(3) -0.034(5) 0.004(4) C8 0.073(5) 0.058(5) 0.096(6) 0.000(4) -0.031(5) 0.003(4) C9 0.045(4) 0.087(6) 0.104(7) -0.007(5) -0.015(4) 0.007(4) C10 0.074(5) 0.066(5) 0.064(4) -0.009(4) 0.003(4) 0.012(4) C11 0.065(4) 0.028(3) 0.042(3) 0.000(2) -0.010(3) 0.001(3) C12 0.081(5) 0.033(3) 0.032(3) -0.001(2) -0.002(3) -0.006(3) C13 0.051(4) 0.040(3) 0.053(4) -0.001(3) 0.010(3) 0.003(3) C14 0.057(4) 0.043(3) 0.044(3) 0.000(3) -0.001(3) 0.000(3) C15 0.061(4) 0.070(4) 0.059(4) 0.008(4) -0.016(3) -0.009(4) C16 0.069(5) 0.059(4) 0.072(5) 0.005(4) -0.013(4) 0.008(4) C17 0.053(4) 0.080(5) 0.067(4) 0.007(4) 0.002(4) 0.008(4) C18 0.075(5) 0.058(4) 0.073(5) -0.012(3) -0.001(4) 0.006(4) C19 0.077(5) 0.059(5) 0.073(5) -0.005(4) -0.022(4) 0.008(4) C20 0.124(8) 0.044(4) 0.070(5) 0.002(4) -0.039(5) 0.004(4) C21 0.152(9) 0.041(4) 0.052(4) 0.006(3) -0.015(5) 0.008(5) C22 0.129(7) 0.029(3) 0.056(4) -0.002(3) -0.009(5) 0.009(4) C23 0.157(10) 0.042(4) 0.058(4) 0.008(3) 0.014(6) 0.003(5) C24 0.122(8) 0.078(6) 0.085(7) 0.002(5) 0.038(6) -0.006(6) C25 0.087(6) 0.034(4) 0.078(5) 0.004(3) 0.023(4) 0.001(4) C26 0.076(6) 0.074(6) 0.099(7) -0.008(5) 0.009(5) -0.006(5) C27 0.066(5) 0.067(5) 0.118(7) -0.008(5) -0.019(5) 0.003(4) C28 0.044(3) 0.057(4) 0.070(4) -0.001(4) -0.008(3) 0.005(3) C29 0.079(4) 0.028(3) 0.056(4) 0.002(3) 0.000(3) 0.007(3) C30 0.087(5) 0.025(3) 0.057(4) 0.007(3) 0.001(4) 0.002(3) C31 0.064(4) 0.057(4) 0.050(4) -0.003(3) -0.008(3) 0.006(3) C32 0.052(4) 0.055(4) 0.056(4) 0.001(3) -0.010(3) 0.000(3) C33 0.053(4) 0.056(4) 0.066(4) 0.009(3) -0.008(3) 0.001(3) C34 0.052(4) 0.066(5) 0.078(5) 0.000(4) 0.012(4) 0.007(4) C35 0.079(7) 0.076(6) 0.181(11) -0.047(7) 0.005(7) 0.014(5) C36 0.063(6) 0.079(7) 0.244(15) 0.011(8) 0.044(8) 0.018(5) N1 0.067(3) 0.048(3) 0.047(3) 0.001(2) 0.004(3) -0.002(3) N2 0.055(3) 0.048(3) 0.048(3) -0.005(2) -0.001(2) 0.008(3) N3 0.053(3) 0.046(3) 0.039(2) -0.002(2) 0.004(2) 0.004(2) N4 0.054(3) 0.064(4) 0.106(5) 0.006(4) -0.009(3) 0.008(3) N5 0.067(4) 0.044(3) 0.061(3) 0.001(3) -0.012(3) 0.011(3) N6 0.056(3) 0.041(3) 0.068(3) 0.002(3) -0.006(3) 0.000(3) N7 0.064(3) 0.086(4) 0.049(3) 0.008(3) 0.002(3) 0.020(4) N8 0.087(6) 0.111(7) 0.155(8) 0.023(6) 0.007(6) -0.028(5) O1 0.054(3) 0.078(3) 0.035(2) -0.003(2) -0.0035(19) -0.006(2) O2 0.068(3) 0.082(3) 0.044(2) 0.009(2) 0.010(2) -0.001(3) O3 0.047(3) 0.087(3) 0.054(3) 0.009(2) -0.004(2) 0.020(2) O4 0.078(4) 0.096(4) 0.058(3) 0.020(3) -0.013(3) 0.011(3) O11 0.140(5) 0.055(3) 0.068(3) -0.008(2) 0.011(4) 0.021(3) O12 0.199(11) 0.121(7) 0.321(16) -0.060(9) 0.146(11) -0.020(7) O13 0.293(13) 0.091(5) 0.084(5) -0.012(4) -0.036(7) 0.008(7) O14 0.134(6) 0.059(3) 0.131(5) -0.006(4) -0.039(5) 0.027(3) O41 0.089(4) 0.116(5) 0.123(6) -0.022(4) -0.020(4) -0.026(4) O42 0.106(5) 0.197(8) 0.082(4) 0.064(5) -0.016(4) 0.010(6) O43 0.067(4) 0.121(5) 0.139(6) 0.019(5) 0.018(4) 0.006(3) O44 0.127(6) 0.068(4) 0.147(6) 0.002(4) -0.022(5) 0.032(4) O21 0.123(5) 0.057(4) 0.213(8) 0.005(4) 0.080(6) 0.018(4) O22 0.098(4) 0.042(3) 0.171(6) 0.010(3) 0.044(4) -0.006(3) O23 0.154(8) 0.255(11) 0.072(4) 0.039(6) 0.028(5) -0.016(8) O24 0.098(5) 0.080(4) 0.230(10) 0.014(5) -0.078(6) -0.022(4) O31 0.212(9) 0.113(5) 0.100(5) -0.018(4) -0.018(6) 0.062(6) O32 0.304(17) 0.109(7) 0.205(11) -0.038(7) -0.021(11) 0.006(9) O33 0.132(10) 0.296(18) 0.48(3) -0.082(19) -0.070(13) 0.095(12) O34 0.84(5) 0.223(13) 0.062(5) -0.016(6) 0.005(12) 0.23(2) OW1 0.054(3) 0.123(5) 0.073(3) -0.037(3) 0.006(3) -0.006(3) Cl1 0.1023(17) 0.0580(11) 0.0872(14) -0.0167(10) 0.0203(12) 0.0110(11) Cl2 0.0619(10) 0.0469(8) 0.0603(9) 0.0080(7) 0.0053(8) -0.0028(7) Cl3 0.1017(16) 0.0854(15) 0.0631(11) -0.0094(10) -0.0027(11) 0.0180(13) Cl4 0.0509(9) 0.0547(9) 0.0610(9) 0.0105(7) -0.0033(8) 0.0043(7) _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 Cu1 O1 1.938(4) . ? Cu1 N3 1.976(5) . ? Cu1 N2 1.987(5) . ? Cu1 N1 2.004(5) . ? Cu2 O3 1.934(5) . ? Cu2 N6 1.970(6) . ? Cu2 N7 2.002(6) . ? Cu2 N5 2.018(6) . ? C1 N1 1.319(9) . ? C1 C2 1.388(11) . ? C1 H1 0.9300 . ? C2 C3 1.343(13) . ? C2 H2 0.9300 . ? C3 C4 1.384(13) . ? C3 H3 0.9300 . ? C4 C12 1.390(8) . ? C4 C5 1.431(13) . ? C5 C6 1.335(14) . ? C5 H5 0.9300 . ? C6 C7 1.434(12) . ? C6 H6 0.9300 . ? C7 C11 1.362(9) . ? C7 C8 1.401(13) . ? C8 C9 1.368(12) . ? C8 H8 0.9300 . ? C9 C10 1.368(11) . ? C9 H9 0.9300 . ? C10 N2 1.314(9) . ? C10 H10 0.9300 . ? C11 N2 1.363(7) . ? C11 C12 1.438(9) . ? C12 N1 1.365(8) . ? C13 O2 1.236(7) . ? C13 O1 1.256(7) . ? C13 C14 1.524(9) . ? C14 N3 1.495(8) . ? C14 C15 1.545(9) . ? C14 H14 0.9800 . ? C15 C16 1.502(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.498(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.512(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N4 1.457(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.337(9) . ? C19 C20 1.398(11) . ? C19 H19 0.9300 . ? C20 C21 1.397(13) . ? C21 C22 1.381(13) . ? C21 H21 0.9300 . ? C22 C30 1.378(9) . ? C22 C23 1.463(13) . ? C23 C24 1.277(14) . ? C23 H23 0.9300 . ? C24 C25 1.466(13) . ? C24 H24 0.9300 . ? C25 C26 1.362(12) . ? C25 C29 1.410(10) . ? C26 C27 1.375(12) . ? C26 H26 0.9300 . ? C27 C28 1.384(11) . ? C27 H27 0.9300 . ? C28 N6 1.315(8) . ? C28 H28 0.9300 . ? C29 N6 1.369(8) . ? C29 C30 1.420(10) . ? C30 N5 1.357(9) . ? C31 O4 1.241(8) . ? C31 O3 1.260(8) . ? C31 C32 1.532(9) . ? C32 N7 1.481(8) . ? C32 C33 1.511(10) . ? C32 H32 0.9800 . ? C33 C34 1.516(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.485(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.451(14) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N8 1.392(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? N8 H8A 0.8900 . ? N8 H8B 0.8900 . ? N8 H8C 0.8900 . ? O11 Cl1 1.402(5) . ? O12 Cl1 1.371(11) . ? O13 Cl1 1.418(8) . ? O14 Cl1 1.409(6) . ? O41 Cl4 1.424(6) . ? O42 Cl4 1.417(6) . ? O43 Cl4 1.405(6) . ? O44 Cl4 1.368(6) . ? O21 Cl2 1.400(6) . ? O22 Cl2 1.410(5) . ? O23 Cl2 1.372(7) . ? O24 Cl2 1.397(6) . ? O31 Cl3 1.390(8) . ? O32 Cl3 1.450(11) . ? O33 Cl3 1.242(13) . ? O34 Cl3 1.263(9) . ? 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 Cu1 N3 84.49(19) . . ? O1 Cu1 N2 94.3(2) . . ? N3 Cu1 N2 173.8(2) . . ? O1 Cu1 N1 171.9(2) . . ? N3 Cu1 N1 99.1(2) . . ? N2 Cu1 N1 82.9(2) . . ? O3 Cu2 N6 94.9(2) . . ? O3 Cu2 N7 84.8(2) . . ? N6 Cu2 N7 172.9(3) . . ? O3 Cu2 N5 172.0(2) . . ? N6 Cu2 N5 82.6(2) . . ? N7 Cu2 N5 98.5(2) . . ? N1 C1 C2 122.3(8) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.9(8) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.9(7) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C12 117.8(8) . . ? C3 C4 C5 125.8(7) . . ? C12 C4 C5 116.5(8) . . ? C6 C5 C4 122.1(7) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 121.6(8) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C11 C7 C8 116.9(7) . . ? C11 C7 C6 118.1(9) . . ? C8 C7 C6 125.0(8) . . ? C9 C8 C7 119.9(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.3(8) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 124.3(7) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? C7 C11 N2 123.9(7) . . ? C7 C11 C12 120.3(6) . . ? N2 C11 C12 115.8(5) . . ? N1 C12 C4 122.1(7) . . ? N1 C12 C11 116.6(5) . . ? C4 C12 C11 121.3(6) . . ? O2 C13 O1 122.8(6) . . ? O2 C13 C14 120.8(6) . . ? O1 C13 C14 116.4(5) . . ? N3 C14 C13 107.6(5) . . ? N3 C14 C15 113.4(5) . . ? C13 C14 C15 113.8(5) . . ? N3 C14 H14 107.2 . . ? C13 C14 H14 107.2 . . ? C15 C14 H14 107.2 . . ? C16 C15 C14 115.7(6) . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C15 113.1(7) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 111.7(7) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C17 111.8(7) . . ? N4 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? N4 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? N5 C19 C20 123.2(8) . . ? N5 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 117.1(8) . . ? C22 C21 C20 120.8(7) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C30 C22 C21 117.6(9) . . ? C30 C22 C23 117.3(8) . . ? C21 C22 C23 125.1(8) . . ? C24 C23 C22 122.7(8) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.6 . . ? C23 C24 C25 123.1(10) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? C26 C25 C29 119.6(7) . . ? C26 C25 C24 126.0(9) . . ? C29 C25 C24 114.4(8) . . ? C25 C26 C27 118.6(8) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C26 C27 C28 119.4(8) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N6 C28 C27 123.6(7) . . ? N6 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? N6 C29 C25 121.1(7) . . ? N6 C29 C30 116.0(6) . . ? C25 C29 C30 122.9(6) . . ? N5 C30 C22 123.5(7) . . ? N5 C30 C29 116.8(6) . . ? C22 C30 C29 119.7(7) . . ? O4 C31 O3 123.2(7) . . ? O4 C31 C32 118.8(7) . . ? O3 C31 C32 118.0(6) . . ? N7 C32 C33 112.6(6) . . ? N7 C32 C31 109.4(6) . . ? C33 C32 C31 110.7(5) . . ? N7 C32 H32 108.0 . . ? C33 C32 H32 108.0 . . ? C31 C32 H32 108.0 . . ? C32 C33 C34 112.3(6) . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 115.0(7) . . ? C35 C34 H34A 108.5 . . ? C33 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C33 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 113.2(9) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N8 C36 C35 119.1(10) . . ? N8 C36 H36A 107.5 . . ? C35 C36 H36A 107.5 . . ? N8 C36 H36B 107.5 . . ? C35 C36 H36B 107.5 . . ? H36A C36 H36B 107.0 . . ? C1 N1 C12 118.1(6) . . ? C1 N1 Cu1 130.1(5) . . ? C12 N1 Cu1 111.8(4) . . ? C10 N2 C11 116.7(6) . . ? C10 N2 Cu1 130.3(5) . . ? C11 N2 Cu1 112.9(4) . . ? C14 N3 Cu1 106.7(4) . . ? C18 N4 H4A 109.5 . . ? C18 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C18 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C19 N5 C30 117.8(6) . . ? C19 N5 Cu2 130.5(6) . . ? C30 N5 Cu2 111.4(4) . . ? C28 N6 C29 117.6(6) . . ? C28 N6 Cu2 129.4(5) . . ? C29 N6 Cu2 113.0(4) . . ? C32 N7 Cu2 109.8(4) . . ? C36 N8 H8A 109.5 . . ? C36 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? C36 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C13 O1 Cu1 115.2(4) . . ? C31 O3 Cu2 115.9(4) . . ? O12 Cl1 O11 108.2(5) . . ? O12 Cl1 O14 110.7(7) . . ? O11 Cl1 O14 111.0(4) . . ? O12 Cl1 O13 109.2(8) . . ? O11 Cl1 O13 109.6(5) . . ? O14 Cl1 O13 108.1(5) . . ? O23 Cl2 O24 104.7(6) . . ? O23 Cl2 O21 108.7(6) . . ? O24 Cl2 O21 111.7(5) . . ? O23 Cl2 O22 111.1(6) . . ? O24 Cl2 O22 110.2(4) . . ? O21 Cl2 O22 110.3(4) . . ? O33 Cl3 O34 112.5(13) . . ? O33 Cl3 O31 116.6(11) . . ? O34 Cl3 O31 109.4(7) . . ? O33 Cl3 O32 98.9(10) . . ? O34 Cl3 O32 114.6(12) . . ? O31 Cl3 O32 104.4(6) . . ? O44 Cl4 O43 108.6(5) . . ? O44 Cl4 O42 112.3(5) . . ? O43 Cl4 O42 109.6(4) . . ? O44 Cl4 O41 110.7(5) . . ? O43 Cl4 O41 109.4(5) . . ? O42 Cl4 O41 106.1(5) . . ? 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 N1 C1 C2 C3 0.8(13) . . . . ? C1 C2 C3 C4 -1.8(12) . . . . ? C2 C3 C4 C12 1.7(10) . . . . ? C2 C3 C4 C5 -178.6(8) . . . . ? C3 C4 C5 C6 179.1(8) . . . . ? C12 C4 C5 C6 -1.2(11) . . . . ? C4 C5 C6 C7 0.4(13) . . . . ? C5 C6 C7 C11 -0.1(11) . . . . ? C5 C6 C7 C8 -178.1(8) . . . . ? C11 C7 C8 C9 1.6(11) . . . . ? C6 C7 C8 C9 179.6(7) . . . . ? C7 C8 C9 C10 -0.1(12) . . . . ? C8 C9 C10 N2 0.2(13) . . . . ? C8 C7 C11 N2 -3.3(10) . . . . ? C6 C7 C11 N2 178.6(6) . . . . ? C8 C7 C11 C12 178.8(6) . . . . ? C6 C7 C11 C12 0.6(9) . . . . ? C3 C4 C12 N1 -0.5(9) . . . . ? C5 C4 C12 N1 179.8(6) . . . . ? C3 C4 C12 C11 -178.5(6) . . . . ? C5 C4 C12 C11 1.7(9) . . . . ? C7 C11 C12 N1 -179.7(6) . . . . ? N2 C11 C12 N1 2.3(8) . . . . ? C7 C11 C12 C4 -1.5(9) . . . . ? N2 C11 C12 C4 -179.6(5) . . . . ? O2 C13 C14 N3 -151.9(6) . . . . ? O1 C13 C14 N3 29.2(7) . . . . ? O2 C13 C14 C15 -25.4(9) . . . . ? O1 C13 C14 C15 155.7(6) . . . . ? N3 C14 C15 C16 -57.0(8) . . . . ? C13 C14 C15 C16 179.6(6) . . . . ? C14 C15 C16 C17 -68.1(9) . . . . ? C15 C16 C17 C18 -171.7(6) . . . . ? C16 C17 C18 N4 -178.5(6) . . . . ? N5 C19 C20 C21 -3.0(12) . . . . ? C19 C20 C21 C22 1.7(11) . . . . ? C20 C21 C22 C30 -0.7(10) . . . . ? C20 C21 C22 C23 178.9(7) . . . . ? C30 C22 C23 C24 0.5(11) . . . . ? C21 C22 C23 C24 -179.2(9) . . . . ? C22 C23 C24 C25 -1.3(14) . . . . ? C23 C24 C25 C26 -178.9(9) . . . . ? C23 C24 C25 C29 1.0(13) . . . . ? C29 C25 C26 C27 0.7(12) . . . . ? C24 C25 C26 C27 -179.4(8) . . . . ? C25 C26 C27 C28 -1.7(13) . . . . ? C26 C27 C28 N6 1.7(12) . . . . ? C26 C25 C29 N6 0.4(10) . . . . ? C24 C25 C29 N6 -179.5(6) . . . . ? C26 C25 C29 C30 180.0(7) . . . . ? C24 C25 C29 C30 0.1(10) . . . . ? C21 C22 C30 N5 0.9(9) . . . . ? C23 C22 C30 N5 -178.8(6) . . . . ? C21 C22 C30 C29 -179.7(6) . . . . ? C23 C22 C30 C29 0.6(9) . . . . ? N6 C29 C30 N5 -1.8(8) . . . . ? C25 C29 C30 N5 178.6(6) . . . . ? N6 C29 C30 C22 178.7(5) . . . . ? C25 C29 C30 C22 -0.9(9) . . . . ? O4 C31 C32 N7 164.4(7) . . . . ? O3 C31 C32 N7 -15.9(9) . . . . ? O4 C31 C32 C33 -70.9(9) . . . . ? O3 C31 C32 C33 108.7(7) . . . . ? N7 C32 C33 C34 -69.1(8) . . . . ? C31 C32 C33 C34 168.1(6) . . . . ? C32 C33 C34 C35 178.2(8) . . . . ? C33 C34 C35 C36 177.1(10) . . . . ? C34 C35 C36 N8 132.7(12) . . . . ? C2 C1 N1 C12 0.4(11) . . . . ? C2 C1 N1 Cu1 -179.7(6) . . . . ? C4 C12 N1 C1 -0.5(9) . . . . ? C11 C12 N1 C1 177.6(6) . . . . ? C4 C12 N1 Cu1 179.6(4) . . . . ? C11 C12 N1 Cu1 -2.3(6) . . . . ? O1 Cu1 N1 C1 110.9(15) . . . . ? N3 Cu1 N1 C1 -4.4(7) . . . . ? N2 Cu1 N1 C1 -178.5(7) . . . . ? O1 Cu1 N1 C12 -69.2(17) . . . . ? N3 Cu1 N1 C12 175.5(4) . . . . ? N2 Cu1 N1 C12 1.4(4) . . . . ? C9 C10 N2 C11 -1.7(11) . . . . ? C9 C10 N2 Cu1 -178.9(6) . . . . ? C7 C11 N2 C10 3.3(10) . . . . ? C12 C11 N2 C10 -178.7(6) . . . . ? C7 C11 N2 Cu1 -179.0(5) . . . . ? C12 C11 N2 Cu1 -1.0(7) . . . . ? O1 Cu1 N2 C10 -10.6(7) . . . . ? N3 Cu1 N2 C10 68(2) . . . . ? N1 Cu1 N2 C10 177.1(7) . . . . ? O1 Cu1 N2 C11 172.1(4) . . . . ? N3 Cu1 N2 C11 -109.3(19) . . . . ? N1 Cu1 N2 C11 -0.2(4) . . . . ? C13 C14 N3 Cu1 -32.0(5) . . . . ? C15 C14 N3 Cu1 -158.8(4) . . . . ? O1 Cu1 N3 C14 22.7(4) . . . . ? N2 Cu1 N3 C14 -56(2) . . . . ? N1 Cu1 N3 C14 -164.7(4) . . . . ? C20 C19 N5 C30 3.2(10) . . . . ? C20 C19 N5 Cu2 176.1(5) . . . . ? C22 C30 N5 C19 -2.1(9) . . . . ? C29 C30 N5 C19 178.5(6) . . . . ? C22 C30 N5 Cu2 -176.3(5) . . . . ? C29 C30 N5 Cu2 4.2(7) . . . . ? O3 Cu2 N5 C19 -104.7(17) . . . . ? N6 Cu2 N5 C19 -177.3(7) . . . . ? N7 Cu2 N5 C19 9.8(7) . . . . ? O3 Cu2 N5 C30 68.6(18) . . . . ? N6 Cu2 N5 C30 -4.0(4) . . . . ? N7 Cu2 N5 C30 -177.0(4) . . . . ? C27 C28 N6 C29 -0.5(10) . . . . ? C27 C28 N6 Cu2 -178.7(6) . . . . ? C25 C29 N6 C28 -0.5(9) . . . . ? C30 C29 N6 C28 179.9(5) . . . . ? C25 C29 N6 Cu2 178.0(5) . . . . ? C30 C29 N6 Cu2 -1.7(7) . . . . ? O3 Cu2 N6 C28 8.9(6) . . . . ? N7 Cu2 N6 C28 -79(2) . . . . ? N5 Cu2 N6 C28 -178.7(6) . . . . ? O3 Cu2 N6 C29 -169.2(4) . . . . ? N7 Cu2 N6 C29 103.0(18) . . . . ? N5 Cu2 N6 C29 3.1(4) . . . . ? C33 C32 N7 Cu2 -110.1(6) . . . . ? C31 C32 N7 Cu2 13.4(7) . . . . ? O3 Cu2 N7 C32 -7.5(5) . . . . ? N6 Cu2 N7 C32 80.9(19) . . . . ? N5 Cu2 N7 C32 179.8(5) . . . . ? O2 C13 O1 Cu1 170.6(5) . . . . ? C14 C13 O1 Cu1 -10.6(7) . . . . ? N3 Cu1 O1 C13 -7.5(4) . . . . ? N2 Cu1 O1 C13 166.4(4) . . . . ? N1 Cu1 O1 C13 -123.8(15) . . . . ? O4 C31 O3 Cu2 -170.3(6) . . . . ? C32 C31 O3 Cu2 10.1(8) . . . . ? N6 Cu2 O3 C31 -174.3(5) . . . . ? N7 Cu2 O3 C31 -1.4(5) . . . . ? N5 Cu2 O3 C31 114.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.688 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.091