# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Iain May' _publ_contact_author_email IAINMAY@LANL.GOV _publ_section_title ; Neptunium(VI) Chain and Neptunium(VI/V) Mixed Valence Cluster Complexes ; loop_ _publ_author_name 'Iain May' 'David Collison' 'Stephanie M Cornet' 'Jonas L Haller' 'Madeleine Helliwell' ; N.Kaltsoyannis ; 'Mark J. Sarsfield' # Attachment 'npVINpVthf.cif' data_g:\bim83\bim83a _database_code_depnum_ccdc_archive 'CCDC 679580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 Cl4 Np3 O13' _chemical_formula_weight 1453.53 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' 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' Np Np -11.4937 4.1493 '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 12.384(3) _cell_length_b 13.733(3) _cell_length_c 13.829(3) _cell_angle_alpha 61.578(4) _cell_angle_beta 89.393(4) _cell_angle_gamma 86.284(4) _cell_volume 2063.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1990 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.63 _exptl_crystal_description prismatic _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1350 _exptl_absorpt_coefficient_mu 7.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 1.000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14379 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_av_sigmaI/netI 0.1619 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7189 _reflns_number_gt 3971 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0490P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7189 _refine_ls_number_parameters 433 _refine_ls_number_restraints 161 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.965 _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 Np1 Np 0.75084(6) 0.00415(7) 0.74932(6) 0.0230(2) Uani 1 1 d . . . Np2 Np 0.68799(6) 0.29321(6) 0.46122(6) 0.0241(2) Uani 1 1 d . . . Np3 Np 0.76747(6) 0.29362(6) 0.76596(6) 0.0236(2) Uani 1 1 d . . . Cl1 Cl 0.8103(4) -0.1433(5) 0.9520(4) 0.0386(13) Uani 1 1 d . . . Cl2 Cl 0.7123(4) -0.1344(4) 0.6750(4) 0.0383(13) Uani 1 1 d . . . Cl3 Cl 0.8531(4) 0.3569(4) 0.5532(4) 0.0320(12) Uani 1 1 d . . . Cl4 Cl 0.5919(3) 0.3440(4) 0.6204(4) 0.0291(11) Uani 1 1 d . . . O1 O 0.7054(9) 0.1420(10) 0.5739(9) 0.028(3) Uani 1 1 d . . . O2 O 0.7770(9) 0.1460(9) 0.7905(9) 0.025(3) Uani 1 1 d . . . O3 O 0.6134(8) 0.0042(9) 0.7914(8) 0.018(3) Uani 1 1 d . . . O4 O 0.8867(9) 0.0086(10) 0.7069(9) 0.027(3) Uani 1 1 d . . . O5 O 0.8610(10) 0.2496(12) 0.3885(10) 0.039(4) Uani 1 1 d . . . O6 O 0.6406(9) 0.2197(10) 0.3351(10) 0.029(3) Uani 1 1 d . . . O7 O 0.4912(9) 0.2810(10) 0.4580(9) 0.026(3) Uani 1 1 d . . . O8 O 0.6726(10) 0.4328(10) 0.3485(11) 0.035(3) Uani 1 1 d . . . O9 O 0.6024(10) 0.2551(11) 0.8837(10) 0.034(3) Uani 1 1 d . . . O10 O 0.8290(9) 0.2107(10) 0.9618(10) 0.027(3) Uani 1 1 d . . . O11 O 0.9643(9) 0.2949(10) 0.7764(9) 0.027(3) Uani 1 1 d . . . O12 O 0.7632(9) 0.4284(11) 0.7496(10) 0.032(3) Uani 1 1 d . . . O13 O 0.6832(15) 0.4811(17) 0.9995(18) 0.097(7) Uani 1 1 d . . . C1 C 0.9300(15) 0.1422(17) 0.4357(16) 0.037(4) Uani 1 1 d U . . H1A H 0.9472 0.1203 0.3799 0.045 Uiso 1 1 calc R . . H1B H 0.8944 0.0831 0.4958 0.045 Uiso 1 1 calc R . . C2 C 1.0317(15) 0.1713(16) 0.4763(15) 0.035(4) Uani 1 1 d U . . H2A H 1.0945 0.1253 0.4760 0.042 Uiso 1 1 calc R . . H2B H 1.0224 0.1611 0.5502 0.042 Uiso 1 1 calc R . . C3 C 1.0443(14) 0.2954(16) 0.3931(15) 0.033(4) Uani 1 1 d U . . H3A H 1.0514 0.3390 0.4306 0.040 Uiso 1 1 calc R . . H3B H 1.1066 0.3038 0.3473 0.040 Uiso 1 1 calc R . . C4 C 0.9385(13) 0.3289(15) 0.3250(15) 0.028(4) Uani 1 1 d U . . H4A H 0.9117 0.4030 0.3094 0.034 Uiso 1 1 calc R . . H4B H 0.9505 0.3285 0.2558 0.034 Uiso 1 1 calc R . . C5 C 0.6709(17) 0.1124(17) 0.3521(16) 0.038(4) Uani 1 1 d U . . H5A H 0.6612 0.0583 0.4283 0.046 Uiso 1 1 calc R . . H5B H 0.7463 0.1072 0.3343 0.046 Uiso 1 1 calc R . . C6 C 0.5966(17) 0.0910(17) 0.2752(15) 0.040(4) Uani 1 1 d U . . H6A H 0.5326 0.0549 0.3126 0.048 Uiso 1 1 calc R . . H6B H 0.6350 0.0461 0.2471 0.048 Uiso 1 1 calc R . . C7 C 0.5672(16) 0.2113(16) 0.1814(15) 0.034(3) Uani 1 1 d U . . H7A H 0.6223 0.2358 0.1259 0.041 Uiso 1 1 calc R . . H7B H 0.4979 0.2164 0.1468 0.041 Uiso 1 1 calc R . . C8 C 0.5630(15) 0.2772(17) 0.2426(14) 0.032(4) Uani 1 1 d U . . H8A H 0.5826 0.3524 0.1950 0.038 Uiso 1 1 calc R . . H8B H 0.4906 0.2803 0.2691 0.038 Uiso 1 1 calc R . . C9 C 0.4134(15) 0.3796(18) 0.4211(18) 0.042(4) Uani 1 1 d U . . H9A H 0.3812 0.4005 0.3497 0.051 Uiso 1 1 calc R . . H9B H 0.4476 0.4426 0.4181 0.051 Uiso 1 1 calc R . . C10 C 0.3306(16) 0.3365(17) 0.5113(18) 0.041(4) Uani 1 1 d U . . H10A H 0.3543 0.3432 0.5744 0.050 Uiso 1 1 calc R . . H10B H 0.2612 0.3779 0.4849 0.050 Uiso 1 1 calc R . . C11 C 0.3222(15) 0.2196(17) 0.5408(18) 0.040(4) Uani 1 1 d U . . H11A H 0.2754 0.2122 0.4892 0.048 Uiso 1 1 calc R . . H11B H 0.2951 0.1779 0.6145 0.048 Uiso 1 1 calc R . . C12 C 0.4389(14) 0.1814(17) 0.5341(17) 0.038(4) Uani 1 1 d U . . H12A H 0.4745 0.1474 0.6060 0.046 Uiso 1 1 calc R . . H12B H 0.4416 0.1278 0.5071 0.046 Uiso 1 1 calc R . . C13 C 0.5515(16) 0.149(2) 0.9302(19) 0.050(5) Uani 1 1 d U . . H13A H 0.5449 0.1172 1.0092 0.060 Uiso 1 1 calc R . . H13B H 0.5924 0.0961 0.9137 0.060 Uiso 1 1 calc R . . C14 C 0.4397(18) 0.182(2) 0.872(2) 0.068(5) Uani 1 1 d U . . H14A H 0.4428 0.1875 0.7995 0.082 Uiso 1 1 calc R . . H14B H 0.3868 0.1295 0.9152 0.082 Uiso 1 1 calc R . . C15 C 0.4156(17) 0.293(2) 0.867(2) 0.067(5) Uani 1 1 d U . . H15A H 0.3731 0.2846 0.9291 0.081 Uiso 1 1 calc R . . H15B H 0.3742 0.3419 0.7999 0.081 Uiso 1 1 calc R . . C16 C 0.5247(15) 0.343(2) 0.8675(18) 0.053(5) Uani 1 1 d U . . H16A H 0.5351 0.4093 0.7983 0.064 Uiso 1 1 calc R . . H16B H 0.5283 0.3614 0.9271 0.064 Uiso 1 1 calc R . . C17 C 0.8961(17) 0.2698(17) 1.0023(16) 0.042(4) Uani 1 1 d U . . H17A H 0.8621 0.3419 0.9853 0.050 Uiso 1 1 calc R . . H17B H 0.9677 0.2792 0.9711 0.050 Uiso 1 1 calc R . . C18 C 0.9016(17) 0.1915(17) 1.1266(17) 0.043(4) Uani 1 1 d U . . H18A H 0.9701 0.1941 1.1584 0.051 Uiso 1 1 calc R . . H18B H 0.8431 0.2103 1.1632 0.051 Uiso 1 1 calc R . . C19 C 0.8905(17) 0.0820(17) 1.1351(17) 0.042(4) Uani 1 1 d U . . H19A H 0.8650 0.0310 1.2071 0.051 Uiso 1 1 calc R . . H19B H 0.9597 0.0519 1.1238 0.051 Uiso 1 1 calc R . . C20 C 0.8112(17) 0.0989(18) 1.0484(17) 0.047(4) Uani 1 1 d U . . H20A H 0.8251 0.0447 1.0229 0.056 Uiso 1 1 calc R . . H20B H 0.7378 0.0943 1.0747 0.056 Uiso 1 1 calc R . . C21 C 1.0240(13) 0.3941(15) 0.7303(16) 0.030(4) Uani 1 1 d U . . H21A H 1.0067 0.4375 0.7676 0.036 Uiso 1 1 calc R . . H21B H 1.0065 0.4396 0.6526 0.036 Uiso 1 1 calc R . . C22 C 1.1403(14) 0.3551(15) 0.7471(17) 0.035(3) Uani 1 1 d U . . H22A H 1.1666 0.3359 0.8202 0.042 Uiso 1 1 calc R . . H22B H 1.1850 0.4094 0.6925 0.042 Uiso 1 1 calc R . . C23 C 1.1344(14) 0.2536(15) 0.7314(18) 0.037(3) Uani 1 1 d U . . H23A H 1.1273 0.2745 0.6541 0.045 Uiso 1 1 calc R . . H23B H 1.1985 0.2035 0.7623 0.045 Uiso 1 1 calc R . . C24 C 1.0372(14) 0.2018(15) 0.7910(17) 0.034(4) Uani 1 1 d U . . H24A H 1.0058 0.1596 0.7600 0.041 Uiso 1 1 calc R . . H24B H 1.0542 0.1530 0.8683 0.041 Uiso 1 1 calc R . . C25 C 0.7601(16) 0.4731(19) 1.0797(17) 0.048(5) Uani 1 1 d U . . H25A H 0.7271 0.5044 1.1236 0.057 Uiso 1 1 calc R . . H25B H 0.7817 0.3957 1.1284 0.057 Uiso 1 1 calc R . . C26 C 0.8524(16) 0.5308(19) 1.0275(16) 0.046(4) Uani 1 1 d U . . H26A H 0.9155 0.4790 1.0462 0.056 Uiso 1 1 calc R . . H26B H 0.8660 0.5843 1.0522 0.056 Uiso 1 1 calc R . . C27 C 0.8327(17) 0.5873(19) 0.9094(17) 0.049(4) Uani 1 1 d U . . H27A H 0.8752 0.5510 0.8750 0.058 Uiso 1 1 calc R . . H27B H 0.8506 0.6641 0.8772 0.058 Uiso 1 1 calc R . . C28 C 0.7159(18) 0.580(2) 0.8961(18) 0.060(5) Uani 1 1 d U . . H28A H 0.7022 0.5706 0.8324 0.072 Uiso 1 1 calc R . . H28B H 0.6755 0.6471 0.8868 0.072 Uiso 1 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 Np1 0.0188(4) 0.0263(5) 0.0253(4) -0.0133(4) -0.0029(3) -0.0019(3) Np2 0.0214(4) 0.0259(5) 0.0256(4) -0.0125(4) -0.0043(3) -0.0024(3) Np3 0.0191(4) 0.0272(5) 0.0275(4) -0.0154(4) -0.0038(3) -0.0018(3) Cl1 0.036(3) 0.045(3) 0.028(3) -0.011(3) -0.008(2) -0.003(3) Cl2 0.046(3) 0.031(3) 0.041(3) -0.021(3) 0.001(2) -0.005(2) Cl3 0.027(3) 0.042(3) 0.034(3) -0.023(3) -0.001(2) -0.010(2) Cl4 0.023(2) 0.036(3) 0.034(3) -0.022(2) -0.008(2) 0.002(2) O1 0.029(7) 0.020(7) 0.028(7) -0.006(6) -0.012(6) -0.006(6) O2 0.025(7) 0.018(7) 0.029(8) -0.010(6) -0.001(6) 0.005(6) O3 0.016(6) 0.015(7) 0.018(6) -0.004(6) -0.002(5) -0.008(5) O4 0.028(7) 0.024(8) 0.032(8) -0.017(7) -0.006(6) 0.008(6) O5 0.033(8) 0.059(10) 0.017(7) -0.008(7) -0.009(6) -0.024(7) O6 0.027(7) 0.032(8) 0.037(8) -0.022(7) 0.004(6) -0.011(6) O7 0.033(7) 0.022(7) 0.023(7) -0.010(6) 0.001(6) -0.008(6) O8 0.031(7) 0.020(8) 0.050(9) -0.014(7) -0.016(6) 0.007(6) O9 0.032(8) 0.034(9) 0.031(8) -0.013(7) 0.004(6) -0.001(7) O10 0.028(7) 0.026(8) 0.028(7) -0.012(7) 0.001(6) -0.007(6) O11 0.030(7) 0.024(8) 0.021(7) -0.005(6) 0.004(6) -0.011(6) O12 0.015(6) 0.052(9) 0.033(8) -0.023(7) -0.010(6) 0.005(6) O13 0.081(14) 0.091(16) 0.118(18) -0.045(15) 0.009(13) -0.025(12) C1 0.037(9) 0.036(9) 0.034(9) -0.012(8) 0.001(7) -0.005(7) C2 0.033(8) 0.037(8) 0.032(8) -0.015(6) 0.001(6) 0.000(6) C3 0.029(7) 0.036(7) 0.034(8) -0.016(6) -0.005(6) 0.000(6) C4 0.024(8) 0.028(8) 0.036(9) -0.018(7) -0.002(6) -0.005(7) C5 0.051(10) 0.042(9) 0.023(8) -0.017(7) 0.006(6) -0.005(8) C6 0.049(8) 0.041(7) 0.028(7) -0.015(6) 0.000(6) -0.003(7) C7 0.042(8) 0.035(8) 0.030(7) -0.019(6) 0.002(6) -0.008(7) C8 0.036(9) 0.044(8) 0.023(8) -0.020(7) -0.003(7) -0.007(8) C9 0.028(9) 0.045(9) 0.065(10) -0.037(8) 0.007(7) 0.011(7) C10 0.031(7) 0.048(8) 0.066(9) -0.046(8) 0.009(6) 0.003(6) C11 0.031(7) 0.048(8) 0.063(9) -0.043(8) 0.004(7) 0.004(6) C12 0.030(8) 0.046(9) 0.059(10) -0.041(9) 0.000(8) 0.005(7) C13 0.043(9) 0.064(11) 0.053(10) -0.035(9) 0.018(8) -0.007(8) C14 0.041(8) 0.080(10) 0.061(10) -0.016(9) 0.016(7) -0.010(8) C15 0.035(8) 0.074(10) 0.060(10) -0.005(9) 0.017(8) -0.004(7) C16 0.030(9) 0.069(11) 0.042(10) -0.012(9) 0.017(8) 0.005(8) C17 0.056(10) 0.041(8) 0.042(8) -0.030(7) -0.019(8) -0.003(8) C18 0.048(8) 0.043(8) 0.043(8) -0.026(7) -0.013(7) 0.000(7) C19 0.048(8) 0.044(8) 0.042(8) -0.026(7) -0.015(7) 0.002(7) C20 0.053(10) 0.047(10) 0.046(9) -0.027(8) -0.019(7) 0.003(8) C21 0.023(7) 0.018(8) 0.046(9) -0.011(7) -0.002(7) -0.003(6) C22 0.022(6) 0.021(7) 0.052(9) -0.008(6) 0.000(7) -0.004(6) C23 0.023(7) 0.018(7) 0.060(9) -0.009(6) 0.011(6) -0.005(5) C24 0.023(8) 0.014(8) 0.054(10) -0.008(8) 0.012(7) -0.001(6) C25 0.038(9) 0.054(11) 0.034(8) -0.007(8) -0.011(7) -0.007(8) C26 0.043(8) 0.053(10) 0.036(7) -0.015(8) -0.006(6) -0.012(7) C27 0.050(8) 0.051(10) 0.036(7) -0.013(8) -0.001(7) -0.006(8) C28 0.055(9) 0.065(11) 0.041(9) -0.010(9) -0.017(7) -0.005(9) _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 Np1 O4 1.771(12) . ? Np1 O3 1.793(10) . ? Np1 O1 2.303(11) . ? Np1 O2 2.317(11) . ? Np1 Cl2 2.626(5) . ? Np1 Cl1 2.636(5) . ? Np2 O8 1.805(12) . ? Np2 O1 1.912(11) . ? Np2 O7 2.456(11) . ? Np2 O6 2.486(11) . ? Np2 O5 2.514(14) . ? Np2 Cl3 2.813(4) . ? Np2 Cl4 2.836(5) . ? Np3 O12 1.751(13) . ? Np3 O2 1.885(11) . ? Np3 O11 2.445(11) . ? Np3 O10 2.491(11) . ? Np3 O9 2.522(12) . ? Np3 Cl4 2.798(4) . ? Np3 Cl3 2.856(5) . ? O5 C4 1.44(2) . ? O5 C1 1.50(2) . ? O6 C5 1.40(2) . ? O6 C8 1.47(2) . ? O7 C12 1.46(2) . ? O7 C9 1.49(2) . ? O9 C16 1.43(2) . ? O9 C13 1.47(2) . ? O10 C20 1.46(2) . ? O10 C17 1.48(2) . ? O11 C24 1.449(19) . ? O11 C21 1.45(2) . ? O13 C25 1.43(2) . ? O13 C28 1.50(3) . ? C1 C2 1.53(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.55(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.53(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.56(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.56(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.50(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.52(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.47(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.52(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.54(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.50(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.56(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.53(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.47(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.48(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.48(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.51(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.47(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.42(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.45(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.48(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? 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 O4 Np1 O3 178.1(5) . . ? O4 Np1 O1 87.8(5) . . ? O3 Np1 O1 91.3(4) . . ? O4 Np1 O2 89.7(5) . . ? O3 Np1 O2 88.6(4) . . ? O1 Np1 O2 86.3(4) . . ? O4 Np1 Cl2 90.5(4) . . ? O3 Np1 Cl2 91.1(3) . . ? O1 Np1 Cl2 85.6(3) . . ? O2 Np1 Cl2 171.9(3) . . ? O4 Np1 Cl1 90.7(4) . . ? O3 Np1 Cl1 90.1(3) . . ? O1 Np1 Cl1 176.0(3) . . ? O2 Np1 Cl1 89.9(3) . . ? Cl2 Np1 Cl1 98.13(16) . . ? O8 Np2 O1 176.4(6) . . ? O8 Np2 O7 89.5(5) . . ? O1 Np2 O7 90.5(4) . . ? O8 Np2 O6 89.9(5) . . ? O1 Np2 O6 86.6(4) . . ? O7 Np2 O6 70.4(4) . . ? O8 Np2 O5 92.8(5) . . ? O1 Np2 O5 84.9(5) . . ? O7 Np2 O5 142.3(4) . . ? O6 Np2 O5 72.0(4) . . ? O8 Np2 Cl3 89.7(4) . . ? O1 Np2 Cl3 92.5(3) . . ? O7 Np2 Cl3 142.8(3) . . ? O6 Np2 Cl3 146.8(3) . . ? O5 Np2 Cl3 74.9(3) . . ? O8 Np2 Cl4 95.8(4) . . ? O1 Np2 Cl4 87.7(4) . . ? O7 Np2 Cl4 70.4(3) . . ? O6 Np2 Cl4 140.3(3) . . ? O5 Np2 Cl4 146.3(3) . . ? Cl3 Np2 Cl4 72.70(13) . . ? O12 Np3 O2 176.8(5) . . ? O12 Np3 O11 86.2(5) . . ? O2 Np3 O11 91.8(4) . . ? O12 Np3 O10 92.1(5) . . ? O2 Np3 O10 84.9(4) . . ? O11 Np3 O10 70.2(4) . . ? O12 Np3 O9 89.8(5) . . ? O2 Np3 O9 90.2(5) . . ? O11 Np3 O9 141.5(4) . . ? O10 Np3 O9 71.7(4) . . ? O12 Np3 Cl4 93.0(4) . . ? O2 Np3 Cl4 90.1(3) . . ? O11 Np3 Cl4 143.4(3) . . ? O10 Np3 Cl4 146.3(3) . . ? O9 Np3 Cl4 75.0(3) . . ? O12 Np3 Cl3 93.9(4) . . ? O2 Np3 Cl3 87.8(4) . . ? O11 Np3 Cl3 71.0(3) . . ? O10 Np3 Cl3 140.2(3) . . ? O9 Np3 Cl3 147.5(3) . . ? Cl4 Np3 Cl3 72.60(13) . . ? Np2 Cl3 Np3 99.94(14) . . ? Np3 Cl4 Np2 100.79(14) . . ? Np2 O1 Np1 153.5(6) . . ? Np3 O2 Np1 155.6(6) . . ? C4 O5 C1 101.6(13) . . ? C4 O5 Np2 125.4(11) . . ? C1 O5 Np2 128.3(11) . . ? C5 O6 C8 111.0(13) . . ? C5 O6 Np2 124.8(10) . . ? C8 O6 Np2 123.6(10) . . ? C12 O7 C9 109.8(13) . . ? C12 O7 Np2 122.1(10) . . ? C9 O7 Np2 122.6(10) . . ? C16 O9 C13 110.7(15) . . ? C16 O9 Np3 120.3(11) . . ? C13 O9 Np3 122.8(11) . . ? C20 O10 C17 111.4(13) . . ? C20 O10 Np3 126.1(10) . . ? C17 O10 Np3 122.4(10) . . ? C24 O11 C21 108.6(12) . . ? C24 O11 Np3 123.0(10) . . ? C21 O11 Np3 124.8(10) . . ? C25 O13 C28 103.1(17) . . ? O5 C1 C2 102.5(14) . . ? O5 C1 H1A 111.3 . . ? C2 C1 H1A 111.3 . . ? O5 C1 H1B 111.3 . . ? C2 C1 H1B 111.3 . . ? H1A C1 H1B 109.2 . . ? C1 C2 C3 104.5(15) . . ? C1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? C1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? C4 C3 C2 102.6(14) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.2 . . ? O5 C4 C3 107.7(15) . . ? O5 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? O5 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? O6 C5 C6 106.7(16) . . ? O6 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O6 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? C5 C6 C7 101.8(16) . . ? C5 C6 H6A 111.4 . . ? C7 C6 H6A 111.4 . . ? C5 C6 H6B 111.4 . . ? C7 C6 H6B 111.4 . . ? H6A C6 H6B 109.3 . . ? C8 C7 C6 102.2(15) . . ? C8 C7 H7A 111.3 . . ? C6 C7 H7A 111.3 . . ? C8 C7 H7B 111.3 . . ? C6 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? O6 C8 C7 106.2(15) . . ? O6 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O6 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O7 C9 C10 101.2(16) . . ? O7 C9 H9A 111.5 . . ? C10 C9 H9A 111.5 . . ? O7 C9 H9B 111.5 . . ? C10 C9 H9B 111.5 . . ? H9A C9 H9B 109.4 . . ? C11 C10 C9 105.7(16) . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10B 110.6 . . ? C9 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C10 C11 C12 102.5(16) . . ? C10 C11 H11A 111.3 . . ? C12 C11 H11A 111.3 . . ? C10 C11 H11B 111.3 . . ? C12 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? O7 C12 C11 105.9(16) . . ? O7 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O7 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? O9 C13 C14 102.9(18) . . ? O9 C13 H13A 111.2 . . ? C14 C13 H13A 111.2 . . ? O9 C13 H13B 111.2 . . ? C14 C13 H13B 111.2 . . ? H13A C13 H13B 109.1 . . ? C15 C14 C13 100(2) . . ? C15 C14 H14A 111.7 . . ? C13 C14 H14A 111.7 . . ? C15 C14 H14B 111.7 . . ? C13 C14 H14B 111.7 . . ? H14A C14 H14B 109.4 . . ? C14 C15 C16 108.8(18) . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O9 C16 C15 102.2(18) . . ? O9 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? O9 C16 H16B 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? O10 C17 C18 102.4(15) . . ? O10 C17 H17A 111.3 . . ? C18 C17 H17A 111.3 . . ? O10 C17 H17B 111.3 . . ? C18 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? C19 C18 C17 103.3(16) . . ? C19 C18 H18A 111.1 . . ? C17 C18 H18A 111.1 . . ? C19 C18 H18B 111.1 . . ? C17 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? C18 C19 C20 106.3(17) . . ? C18 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? C18 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? O10 C20 C19 102.9(16) . . ? O10 C20 H20A 111.2 . . ? C19 C20 H20A 111.2 . . ? O10 C20 H20B 111.2 . . ? C19 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? O11 C21 C22 106.0(14) . . ? O11 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O11 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C21 C22 C23 99.3(15) . . ? C21 C22 H22A 111.9 . . ? C23 C22 H22A 111.9 . . ? C21 C22 H22B 111.9 . . ? C23 C22 H22B 111.9 . . ? H22A C22 H22B 109.6 . . ? C24 C23 C22 104.0(16) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? O11 C24 C23 104.1(14) . . ? O11 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O11 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 109.0 . . ? C26 C25 O13 110.3(18) . . ? C26 C25 H25A 109.6 . . ? O13 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? O13 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C27 108.7(18) . . ? C25 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? C25 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? C26 C27 C28 104.6(18) . . ? C26 C27 H27A 110.8 . . ? C28 C27 H27A 110.8 . . ? C26 C27 H27B 110.8 . . ? C28 C27 H27B 110.8 . . ? H27A C27 H27B 108.9 . . ? C27 C28 O13 106.1(17) . . ? C27 C28 H28A 110.5 . . ? O13 C28 H28A 110.5 . . ? C27 C28 H28B 110.5 . . ? O13 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? 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 O8 Np2 Cl3 Np3 123.9(4) . . . . ? O1 Np2 Cl3 Np3 -59.0(4) . . . . ? O7 Np2 Cl3 Np3 35.1(5) . . . . ? O6 Np2 Cl3 Np3 -146.6(5) . . . . ? O5 Np2 Cl3 Np3 -143.1(3) . . . . ? Cl4 Np2 Cl3 Np3 27.78(14) . . . . ? O12 Np3 Cl3 Np2 -120.1(4) . . . . ? O2 Np3 Cl3 Np2 62.6(3) . . . . ? O11 Np3 Cl3 Np2 155.3(3) . . . . ? O10 Np3 Cl3 Np2 141.8(4) . . . . ? O9 Np3 Cl3 Np2 -24.2(6) . . . . ? Cl4 Np3 Cl3 Np2 -28.20(14) . . . . ? O12 Np3 Cl4 Np2 121.2(4) . . . . ? O2 Np3 Cl4 Np2 -59.6(4) . . . . ? O11 Np3 Cl4 Np2 33.6(5) . . . . ? O10 Np3 Cl4 Np2 -140.4(5) . . . . ? O9 Np3 Cl4 Np2 -149.7(3) . . . . ? Cl3 Np3 Cl4 Np2 28.04(14) . . . . ? O8 Np2 Cl4 Np3 -116.4(4) . . . . ? O1 Np2 Cl4 Np3 64.8(3) . . . . ? O7 Np2 Cl4 Np3 156.2(3) . . . . ? O6 Np2 Cl4 Np3 146.7(5) . . . . ? O5 Np2 Cl4 Np3 -12.4(6) . . . . ? Cl3 Np2 Cl4 Np3 -28.50(14) . . . . ? O8 Np2 O1 Np1 155(7) . . . . ? O7 Np2 O1 Np1 -114.4(14) . . . . ? O6 Np2 O1 Np1 175.3(14) . . . . ? O5 Np2 O1 Np1 103.1(14) . . . . ? Cl3 Np2 O1 Np1 28.5(14) . . . . ? Cl4 Np2 O1 Np1 -44.1(14) . . . . ? O4 Np1 O1 Np2 -84.9(14) . . . . ? O3 Np1 O1 Np2 93.5(14) . . . . ? O2 Np1 O1 Np2 4.9(14) . . . . ? Cl2 Np1 O1 Np2 -175.5(14) . . . . ? Cl1 Np1 O1 Np2 -17(6) . . . . ? O12 Np3 O2 Np1 -173(9) . . . . ? O11 Np3 O2 Np1 -121.0(15) . . . . ? O10 Np3 O2 Np1 169.1(15) . . . . ? O9 Np3 O2 Np1 97.4(15) . . . . ? Cl4 Np3 O2 Np1 22.4(14) . . . . ? Cl3 Np3 O2 Np1 -50.1(14) . . . . ? O4 Np1 O2 Np3 100.6(15) . . . . ? O3 Np1 O2 Np3 -78.6(15) . . . . ? O1 Np1 O2 Np3 12.8(15) . . . . ? Cl2 Np1 O2 Np3 10(4) . . . . ? Cl1 Np1 O2 Np3 -168.7(15) . . . . ? O8 Np2 O5 C4 30.5(12) . . . . ? O1 Np2 O5 C4 -152.4(12) . . . . ? O7 Np2 O5 C4 123.4(11) . . . . ? O6 Np2 O5 C4 119.5(12) . . . . ? Cl3 Np2 O5 C4 -58.5(11) . . . . ? Cl4 Np2 O5 C4 -74.4(13) . . . . ? O8 Np2 O5 C1 -178.5(12) . . . . ? O1 Np2 O5 C1 -1.4(12) . . . . ? O7 Np2 O5 C1 -85.6(13) . . . . ? O6 Np2 O5 C1 -89.5(12) . . . . ? Cl3 Np2 O5 C1 92.5(12) . . . . ? Cl4 Np2 O5 C1 76.6(14) . . . . ? O8 Np2 O6 C5 156.1(14) . . . . ? O1 Np2 O6 C5 -22.7(13) . . . . ? O7 Np2 O6 C5 -114.4(14) . . . . ? O5 Np2 O6 C5 63.1(13) . . . . ? Cl3 Np2 O6 C5 66.6(15) . . . . ? Cl4 Np2 O6 C5 -104.9(13) . . . . ? O8 Np2 O6 C8 -34.1(13) . . . . ? O1 Np2 O6 C8 147.1(13) . . . . ? O7 Np2 O6 C8 55.4(12) . . . . ? O5 Np2 O6 C8 -127.1(13) . . . . ? Cl3 Np2 O6 C8 -123.5(11) . . . . ? Cl4 Np2 O6 C8 64.9(14) . . . . ? O8 Np2 O7 C12 179.9(12) . . . . ? O1 Np2 O7 C12 3.6(12) . . . . ? O6 Np2 O7 C12 89.8(12) . . . . ? O5 Np2 O7 C12 85.9(13) . . . . ? Cl3 Np2 O7 C12 -91.1(12) . . . . ? Cl4 Np2 O7 C12 -83.7(11) . . . . ? O8 Np2 O7 C9 -29.0(13) . . . . ? O1 Np2 O7 C9 154.6(13) . . . . ? O6 Np2 O7 C9 -119.1(13) . . . . ? O5 Np2 O7 C9 -123.0(12) . . . . ? Cl3 Np2 O7 C9 59.9(14) . . . . ? Cl4 Np2 O7 C9 67.3(12) . . . . ? O12 Np3 O9 C16 28.6(14) . . . . ? O2 Np3 O9 C16 -154.5(14) . . . . ? O11 Np3 O9 C16 112.3(14) . . . . ? O10 Np3 O9 C16 120.9(14) . . . . ? Cl4 Np3 O9 C16 -64.5(13) . . . . ? Cl3 Np3 O9 C16 -68.4(15) . . . . ? O12 Np3 O9 C13 178.4(14) . . . . ? O2 Np3 O9 C13 -4.8(14) . . . . ? O11 Np3 O9 C13 -97.9(14) . . . . ? O10 Np3 O9 C13 -89.3(14) . . . . ? Cl4 Np3 O9 C13 85.2(13) . . . . ? Cl3 Np3 O9 C13 81.3(15) . . . . ? O12 Np3 O10 C20 153.4(14) . . . . ? O2 Np3 O10 C20 -27.6(14) . . . . ? O11 Np3 O10 C20 -121.4(15) . . . . ? O9 Np3 O10 C20 64.2(14) . . . . ? Cl4 Np3 O10 C20 54.8(16) . . . . ? Cl3 Np3 O10 C20 -107.9(14) . . . . ? O12 Np3 O10 C17 -30.6(13) . . . . ? O2 Np3 O10 C17 148.4(13) . . . . ? O11 Np3 O10 C17 54.5(13) . . . . ? O9 Np3 O10 C17 -119.8(13) . . . . ? Cl4 Np3 O10 C17 -129.3(12) . . . . ? Cl3 Np3 O10 C17 68.1(14) . . . . ? O12 Np3 O11 C24 -179.7(13) . . . . ? O2 Np3 O11 C24 2.8(13) . . . . ? O10 Np3 O11 C24 86.6(13) . . . . ? O9 Np3 O11 C24 95.3(13) . . . . ? Cl4 Np3 O11 C24 -89.8(13) . . . . ? Cl3 Np3 O11 C24 -84.2(12) . . . . ? O12 Np3 O11 C21 -23.8(13) . . . . ? O2 Np3 O11 C21 158.8(13) . . . . ? O10 Np3 O11 C21 -117.4(13) . . . . ? O9 Np3 O11 C21 -108.7(13) . . . . ? Cl4 Np3 O11 C21 66.2(14) . . . . ? Cl3 Np3 O11 C21 71.7(12) . . . . ? C4 O5 C1 C2 45.8(16) . . . . ? Np2 O5 C1 C2 -110.4(13) . . . . ? O5 C1 C2 C3 -33.2(18) . . . . ? C1 C2 C3 C4 8.8(19) . . . . ? C1 O5 C4 C3 -41.3(17) . . . . ? Np2 O5 C4 C3 115.8(13) . . . . ? C2 C3 C4 O5 20.1(19) . . . . ? C8 O6 C5 C6 -8(2) . . . . ? Np2 O6 C5 C6 163.1(11) . . . . ? O6 C5 C6 C7 26(2) . . . . ? C5 C6 C7 C8 -33.9(19) . . . . ? C5 O6 C8 C7 -15(2) . . . . ? Np2 O6 C8 C7 174.1(11) . . . . ? C6 C7 C8 O6 30.5(19) . . . . ? C12 O7 C9 C10 20.2(19) . . . . ? Np2 O7 C9 C10 -134.0(12) . . . . ? O7 C9 C10 C11 -36(2) . . . . ? C9 C10 C11 C12 38(2) . . . . ? C9 O7 C12 C11 2.4(19) . . . . ? Np2 O7 C12 C11 156.7(11) . . . . ? C10 C11 C12 O7 -25(2) . . . . ? C16 O9 C13 C14 37(2) . . . . ? Np3 O9 C13 C14 -115.2(15) . . . . ? O9 C13 C14 C15 -37(2) . . . . ? C13 C14 C15 C16 26(2) . . . . ? C13 O9 C16 C15 -20(2) . . . . ? Np3 O9 C16 C15 133.1(14) . . . . ? C14 C15 C16 O9 -5(2) . . . . ? C20 O10 C17 C18 -9(2) . . . . ? Np3 O10 C17 C18 174.1(11) . . . . ? O10 C17 C18 C19 28(2) . . . . ? C17 C18 C19 C20 -38(2) . . . . ? C17 O10 C20 C19 -13(2) . . . . ? Np3 O10 C20 C19 163.3(11) . . . . ? C18 C19 C20 O10 32(2) . . . . ? C24 O11 C21 C22 -16(2) . . . . ? Np3 O11 C21 C22 -174.9(11) . . . . ? O11 C21 C22 C23 35.1(19) . . . . ? C21 C22 C23 C24 -42(2) . . . . ? C21 O11 C24 C23 -11(2) . . . . ? Np3 O11 C24 C23 148.2(12) . . . . ? C22 C23 C24 O11 34(2) . . . . ? C28 O13 C25 C26 -20(3) . . . . ? O13 C25 C26 C27 5(3) . . . . ? C25 C26 C27 C28 12(3) . . . . ? C26 C27 C28 O13 -24(3) . . . . ? C25 O13 C28 C27 27(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.361 _refine_diff_density_min -2.116 _refine_diff_density_rms 0.294 # Attachment 'bim95ba1.cif' data_bim95ba _database_code_depnum_ccdc_archive 'CCDC 679581' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl2 Np O3' _chemical_formula_weight 412.00 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Np Np -11.4937 4.1493 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.925(3) _cell_length_b 10.137(2) _cell_length_c 8.675(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.519(5) _cell_angle_gamma 90.00 _cell_volume 905.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 167 _cell_measurement_theta_min 12.47 _cell_measurement_theta_max 25.46 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 12.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 1.000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2575 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.02 _reflns_number_total 791 _reflns_number_gt 727 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The highest residual electron density peaks, which are approximately 1 A from the Np atom, arise from Fourier series truncation, leading to ripples around the Np atom. ; _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^)+(0.0677P)^2^+13.3156P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 791 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Np1 Np 0.0000 0.43716(6) 0.2500 0.0149(3) Uani 1 2 d S . . Cl1 Cl 0.0010(3) 0.6554(3) 0.0566(3) 0.0262(7) Uani 1 1 d . . . O1 O 0.1715(9) 0.4344(8) 0.3245(11) 0.027(2) Uani 1 1 d . . . O2 O 0.0000 0.2009(12) 0.2500 0.020(2) Uani 1 2 d S . . C1 C 0.1174(13) 0.1172(14) 0.289(2) 0.035(3) Uani 1 1 d . . . H1A H 0.1815 0.1425 0.3955 0.042 Uiso 1 1 calc R . . H1B H 0.1583 0.1259 0.2033 0.042 Uiso 1 1 calc R . . C2 C 0.0709(15) -0.0193(14) 0.295(2) 0.040(4) Uani 1 1 d . . . H2A H 0.0890 -0.0474 0.4094 0.048 Uiso 1 1 calc R . . H2B H 0.1153 -0.0809 0.2420 0.048 Uiso 1 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 Np1 0.0141(4) 0.0162(4) 0.0128(3) 0.000 0.0026(3) 0.000 Cl1 0.043(2) 0.0192(15) 0.0169(13) 0.0001(11) 0.0113(13) 0.0018(13) O1 0.024(5) 0.028(5) 0.031(5) -0.001(4) 0.011(4) -0.001(4) O2 0.014(6) 0.022(6) 0.020(5) 0.000 0.000(5) 0.000 C1 0.021(7) 0.026(7) 0.056(9) 0.000(6) 0.011(7) 0.010(6) C2 0.037(9) 0.020(7) 0.060(10) 0.004(7) 0.014(8) 0.006(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 Np1 O1 1.766(9) 2 ? Np1 O1 1.766(9) . ? Np1 O2 2.395(12) . ? Np1 Cl1 2.779(3) 2 ? Np1 Cl1 2.779(3) . ? Np1 Cl1 2.817(3) 5_565 ? Np1 Cl1 2.817(3) 6_566 ? Cl1 Np1 2.817(3) 5_565 ? O2 C1 1.479(15) . ? O2 C1 1.479(15) 2 ? C1 C2 1.48(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C2 1.48(3) 2 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? 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 Np1 O1 178.2(5) 2 . ? O1 Np1 O2 89.1(3) 2 . ? O1 Np1 O2 89.1(3) . . ? O1 Np1 Cl1 90.9(3) 2 2 ? O1 Np1 Cl1 90.5(3) . 2 ? O2 Np1 Cl1 142.77(6) . 2 ? O1 Np1 Cl1 90.5(3) 2 . ? O1 Np1 Cl1 90.9(3) . . ? O2 Np1 Cl1 142.77(6) . . ? Cl1 Np1 Cl1 74.46(12) 2 . ? O1 Np1 Cl1 88.9(3) 2 5_565 ? O1 Np1 Cl1 90.5(3) . 5_565 ? O2 Np1 Cl1 70.54(6) . 5_565 ? Cl1 Np1 Cl1 146.69(7) 2 5_565 ? Cl1 Np1 Cl1 72.23(9) . 5_565 ? O1 Np1 Cl1 90.5(3) 2 6_566 ? O1 Np1 Cl1 88.9(3) . 6_566 ? O2 Np1 Cl1 70.54(6) . 6_566 ? Cl1 Np1 Cl1 72.23(9) 2 6_566 ? Cl1 Np1 Cl1 146.69(7) . 6_566 ? Cl1 Np1 Cl1 141.08(12) 5_565 6_566 ? Np1 Cl1 Np1 107.77(9) . 5_565 ? C1 O2 C1 110.0(14) . 2 ? C1 O2 Np1 125.0(7) . . ? C1 O2 Np1 125.0(7) 2 . ? O2 C1 C2 105.2(11) . . ? O2 C1 H1A 110.7 . . ? C2 C1 H1A 110.7 . . ? O2 C1 H1B 110.7 . . ? C2 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C1 C2 C2 107.0(9) . 2 ? C1 C2 H2A 110.3 . . ? C2 C2 H2A 110.3 2 . ? C1 C2 H2B 110.3 . . ? C2 C2 H2B 110.3 2 . ? H2A C2 H2B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.304 _refine_diff_density_min -1.693 _refine_diff_density_rms 0.372