data_005CPI07 _audit_creation_method SHELXL-97 loop_ _publ_contact_author_name _publ_contact_author_address _publ_contact_author_email _publ_contact_author_fax _publ_contact_author_phone 'Castillo, Ivan' ; Instituto de Qu\'imica Universidad Nacional Aut\'onoma de M\'exico Circuito Exterior, CU M\'exico, D.F. 04510 Mexico ; 'joseivan@servidor.unam.mx' '+(5255) 56162217' '+(5255) 56224449' _publ_requested_journal 'Inorganic Chemistry' _publ_section_title ; Discrete and Polymeric Complexes of a Cu(I)-Stabilizing Aminotrithioether Ligand ; loop_ _publ_author_name _publ_author_address "Huerta, Ra\'ul" ; Instituto de Qu\'imica Universidad Nacional Aut\'onoma de M\'exico Circuito Exterior, CU M\'exico, D.F. 04510 Mexico ; "Flores-Figueroa, Aar\'on" ; Instituto de Qu\'imica Universidad Nacional Aut\'onoma de M\'exico Circuito Exterior, CU M\'exico, D.F. 04510 Mexico ; "Ugalde-Sald\'ivar, V\'ictor M." ; Facultad de Qu\'imica Divisi\'on de Estudios de Posgrado Universidad Nacional Aut\'onoma de M\'exico CU M\'exico, D.F. 04510 Mexico ; "Castillo, Ivan" ; Instituto de Qu\'imica Universidad Nacional Aut\'onoma de M\'exico Circuito Exterior, CU M\'exico, D.F. 04510 Mexico ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 377-380 _chemical_formula_moiety 'C29 H36 Cu2 I2 N2 S3, C2 H3 N' _chemical_formula_sum 'C31 H39 Cu2 I2 N3 S3' _chemical_formula_weight 930.71 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' 'S' 'S' 0.1246 0.1234 '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' 'I' 'I' -0.4742 1.8119 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.686(2) _cell_length_b 13.399(3) _cell_length_c 14.177(3) _cell_angle_alpha 84.473(3) _cell_angle_beta 68.200(3) _cell_angle_gamma 73.740(3) _cell_volume 1809.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.224 _cell_measurement_theta_max 25.419 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 3.079 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4782 _exptl_absorpt_correction_T_max 0.5924 _exptl_absorpt_process_details '(Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Apex CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20073 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.42 _reflns_number_total 6646 _reflns_number_gt 6145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23C (Bruker, 1999)' _computing_structure_solution 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _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^)+(0.0300P)^2^+0.5634P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6646 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.004 _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 I1 I 0.452621(16) 1.152886(12) 0.081863(12) 0.03117(5) Uani 1 1 d . . . I2 I 0.329205(16) 0.646806(12) 0.515428(13) 0.03495(6) Uani 1 1 d . . . Cu1 Cu 0.54828(3) 0.95190(2) 0.06908(2) 0.02997(8) Uani 1 1 d . . . Cu2 Cu 0.56251(3) 0.51731(2) 0.39889(2) 0.03365(8) Uani 1 1 d . . . N1 N 0.6342(2) 0.73231(15) 0.20718(15) 0.0291(4) Uani 1 1 d . . . S1 S 0.75164(6) 0.88667(5) 0.10180(4) 0.02838(13) Uani 1 1 d . . . S2 S 0.39101(6) 0.87479(5) 0.19306(4) 0.02778(13) Uani 1 1 d . . . S3 S 0.73674(6) 0.60483(5) 0.33463(5) 0.02863(13) Uani 1 1 d . . . C1 C 0.7466(2) 0.74688(18) 0.11849(18) 0.0296(5) Uani 1 1 d . . . H1A H 0.7368 0.7232 0.0582 0.035 Uiso 1 1 calc R . . H1B H 0.8359 0.7038 0.1232 0.035 Uiso 1 1 calc R . . C2 C 0.5008(2) 0.74125(18) 0.20218(19) 0.0293(5) Uani 1 1 d . . . H2A H 0.4469 0.7081 0.2634 0.035 Uiso 1 1 calc R . . H2B H 0.5153 0.7006 0.1426 0.035 Uiso 1 1 calc R . . C3 C 0.6476(3) 0.73634(18) 0.30301(18) 0.0308(5) Uani 1 1 d . . . H3A H 0.5540 0.7607 0.3562 0.037 Uiso 1 1 calc R . . H3B H 0.7025 0.7859 0.3001 0.037 Uiso 1 1 calc R . . C4 C 0.9129(2) 0.87322(18) -0.00323(18) 0.0284(5) Uani 1 1 d . . . C5 C 1.0390(3) 0.84817(19) 0.01429(19) 0.0321(5) Uani 1 1 d . . . C6 C 1.1620(3) 0.8368(2) -0.0700(2) 0.0363(6) Uani 1 1 d . . . H6 H 1.2482 0.8206 -0.0594 0.044 Uiso 1 1 calc R . . C7 C 1.1645(3) 0.8481(2) -0.1686(2) 0.0351(6) Uani 1 1 d . . . C8 C 1.0379(3) 0.8744(2) -0.1831(2) 0.0408(6) Uani 1 1 d . . . H8 H 1.0369 0.8835 -0.2501 0.049 Uiso 1 1 calc R . . C9 C 0.9132(3) 0.8873(2) -0.1014(2) 0.0371(6) Uani 1 1 d . . . H9 H 0.8273 0.9059 -0.1127 0.044 Uiso 1 1 calc R . . C10 C 1.0453(3) 0.8342(3) 0.1192(2) 0.0494(8) Uani 1 1 d . . . H10A H 1.1401 0.8302 0.1152 0.074 Uiso 1 1 calc R . . H10B H 1.0207 0.7699 0.1484 0.074 Uiso 1 1 calc R . . H10C H 0.9792 0.8934 0.1622 0.074 Uiso 1 1 calc R . . C11 C 1.3028(3) 0.8298(2) -0.2563(2) 0.0453(7) Uani 1 1 d . . . H11A H 1.2862 0.8479 -0.3201 0.068 Uiso 1 1 calc R . . H11B H 1.3541 0.7564 -0.2584 0.068 Uiso 1 1 calc R . . H11C H 1.3578 0.8732 -0.2474 0.068 Uiso 1 1 calc R . . C12 C 0.3434(2) 0.92669(18) 0.31607(18) 0.0265(5) Uani 1 1 d . . . C13 C 0.2233(2) 0.91181(17) 0.39468(18) 0.0258(5) Uani 1 1 d . . . C14 C 0.1885(2) 0.95711(18) 0.48845(19) 0.0289(5) Uani 1 1 d . . . H14 H 0.1077 0.9477 0.5427 0.035 Uiso 1 1 calc R . . C15 C 0.2660(2) 1.01528(18) 0.50632(18) 0.0286(5) Uani 1 1 d . . . C16 C 0.3855(3) 1.02777(19) 0.42676(19) 0.0314(5) Uani 1 1 d . . . H16 H 0.4412 1.0665 0.4375 0.038 Uiso 1 1 calc R . . C17 C 0.4234(2) 0.98435(19) 0.33263(19) 0.0301(5) Uani 1 1 d . . . H17 H 0.5046 0.9938 0.2788 0.036 Uiso 1 1 calc R . . C18 C 0.1347(3) 0.85063(19) 0.37839(19) 0.0323(5) Uani 1 1 d . . . H18A H 0.0527 0.8529 0.4404 0.048 Uiso 1 1 calc R . . H18B H 0.1893 0.7783 0.3619 0.048 Uiso 1 1 calc R . . H18C H 0.1043 0.8808 0.3222 0.048 Uiso 1 1 calc R . . C19 C 0.2213(3) 1.0679(2) 0.6073(2) 0.0368(6) Uani 1 1 d . . . H19A H 0.1793 1.1422 0.6019 0.055 Uiso 1 1 calc R . . H19B H 0.3028 1.0586 0.6266 0.055 Uiso 1 1 calc R . . H19C H 0.1526 1.0370 0.6591 0.055 Uiso 1 1 calc R . . C20 C 0.7854(2) 0.63625(18) 0.43383(18) 0.0278(5) Uani 1 1 d . . . C21 C 0.9263(3) 0.61983(19) 0.41881(19) 0.0313(5) Uani 1 1 d . . . C22 C 0.9576(3) 0.6512(2) 0.4963(2) 0.0355(6) Uani 1 1 d . . . H22 H 1.0529 0.6395 0.4880 0.043 Uiso 1 1 calc R . . C23 C 0.8558(3) 0.6988(2) 0.5850(2) 0.0353(6) Uani 1 1 d . . . C24 C 0.7169(3) 0.7123(2) 0.59811(19) 0.0343(6) Uani 1 1 d . . . H24 H 0.6453 0.7439 0.6587 0.041 Uiso 1 1 calc R . . C25 C 0.6818(3) 0.6802(2) 0.52389(19) 0.0318(5) Uani 1 1 d . . . H25 H 0.5864 0.6882 0.5344 0.038 Uiso 1 1 calc R . . C26 C 1.0435(3) 0.5709(2) 0.3239(2) 0.0475(7) Uani 1 1 d . . . H26A H 1.1333 0.5655 0.3304 0.071 Uiso 1 1 calc R . . H26B H 1.0366 0.6141 0.2653 0.071 Uiso 1 1 calc R . . H26C H 1.0368 0.5014 0.3144 0.071 Uiso 1 1 calc R . . C27 C 0.8947(3) 0.7379(3) 0.6641(2) 0.0520(8) Uani 1 1 d . . . H27A H 0.8697 0.8140 0.6637 0.078 Uiso 1 1 calc R . . H27B H 0.9955 0.7110 0.6486 0.078 Uiso 1 1 calc R . . H27C H 0.8441 0.7138 0.7313 0.078 Uiso 1 1 calc R . . N2 N 0.5154(3) 0.47995(17) 0.28487(18) 0.0416(5) Uani 1 1 d . . . C28 C 0.4788(3) 0.4624(2) 0.2249(2) 0.0434(7) Uani 1 1 d . . . C29 C 0.4299(5) 0.4411(3) 0.1472(3) 0.0755(11) Uani 1 1 d . . . H29A H 0.3857 0.3837 0.1692 0.113 Uiso 1 1 calc R . . H29B H 0.5094 0.4220 0.0832 0.113 Uiso 1 1 calc R . . H29C H 0.3618 0.5034 0.1370 0.113 Uiso 1 1 calc R . . N3 N 0.2177(6) 0.5161(5) 0.9927(4) 0.145(2) Uani 1 1 d . . . C30 C 0.1638(5) 0.5518(4) 0.9394(4) 0.0850(13) Uani 1 1 d . . . C31 C 0.0934(4) 0.5955(3) 0.8698(3) 0.0719(11) Uani 1 1 d . . . H31A H 0.0438 0.5476 0.8614 0.108 Uiso 1 1 calc R . . H31B H 0.1622 0.6066 0.8039 0.108 Uiso 1 1 calc R . . H31C H 0.0264 0.6621 0.8969 0.108 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 I1 0.03555(10) 0.03028(9) 0.02951(9) -0.00343(6) -0.01329(7) -0.00816(7) I2 0.02818(9) 0.03292(10) 0.04548(11) 0.00545(7) -0.01745(8) -0.00670(7) Cu1 0.03037(16) 0.03200(16) 0.02759(16) 0.00306(12) -0.01135(13) -0.00801(13) Cu2 0.03949(18) 0.03270(17) 0.03580(17) 0.00378(13) -0.01864(14) -0.01456(14) N1 0.0319(11) 0.0323(11) 0.0254(10) 0.0045(8) -0.0112(9) -0.0121(9) S1 0.0268(3) 0.0311(3) 0.0283(3) 0.0026(2) -0.0103(2) -0.0096(2) S2 0.0284(3) 0.0336(3) 0.0238(3) 0.0004(2) -0.0100(2) -0.0112(2) S3 0.0320(3) 0.0293(3) 0.0284(3) 0.0018(2) -0.0133(3) -0.0110(2) C1 0.0308(13) 0.0285(12) 0.0295(13) 0.0021(10) -0.0111(11) -0.0083(10) C2 0.0326(13) 0.0286(12) 0.0291(12) 0.0000(10) -0.0104(10) -0.0126(10) C3 0.0408(14) 0.0279(12) 0.0285(13) 0.0054(10) -0.0161(11) -0.0134(11) C4 0.0267(12) 0.0301(12) 0.0298(13) 0.0028(10) -0.0090(10) -0.0121(10) C5 0.0306(13) 0.0331(13) 0.0353(14) -0.0028(11) -0.0129(11) -0.0102(11) C6 0.0285(13) 0.0401(15) 0.0423(15) -0.0030(12) -0.0128(12) -0.0109(11) C7 0.0330(13) 0.0346(14) 0.0388(14) 0.0011(11) -0.0097(12) -0.0152(11) C8 0.0399(15) 0.0580(18) 0.0289(13) 0.0094(12) -0.0119(12) -0.0234(13) C9 0.0297(13) 0.0465(16) 0.0374(14) 0.0107(12) -0.0137(12) -0.0150(12) C10 0.0365(15) 0.080(2) 0.0367(15) -0.0060(15) -0.0173(13) -0.0152(15) C11 0.0358(15) 0.0551(18) 0.0389(15) -0.0003(13) -0.0038(12) -0.0159(13) C12 0.0263(11) 0.0266(12) 0.0265(12) -0.0004(9) -0.0105(10) -0.0055(9) C13 0.0240(11) 0.0245(12) 0.0288(12) 0.0021(9) -0.0112(10) -0.0045(9) C14 0.0240(11) 0.0296(12) 0.0307(13) 0.0009(10) -0.0084(10) -0.0056(10) C15 0.0286(12) 0.0292(12) 0.0276(12) -0.0010(10) -0.0120(10) -0.0041(10) C16 0.0325(13) 0.0326(13) 0.0348(13) -0.0014(11) -0.0153(11) -0.0124(11) C17 0.0273(12) 0.0348(13) 0.0293(13) 0.0019(10) -0.0092(10) -0.0119(10) C18 0.0283(12) 0.0363(14) 0.0333(13) -0.0017(11) -0.0086(11) -0.0128(11) C19 0.0357(14) 0.0421(15) 0.0338(14) -0.0094(12) -0.0131(12) -0.0082(12) C20 0.0311(13) 0.0266(12) 0.0296(12) 0.0043(10) -0.0135(10) -0.0115(10) C21 0.0297(13) 0.0306(13) 0.0340(13) 0.0037(11) -0.0125(11) -0.0084(10) C22 0.0260(13) 0.0433(15) 0.0413(15) 0.0017(12) -0.0151(12) -0.0117(11) C23 0.0363(14) 0.0402(14) 0.0368(14) 0.0015(11) -0.0184(12) -0.0146(12) C24 0.0332(13) 0.0404(14) 0.0297(13) -0.0018(11) -0.0097(11) -0.0120(11) C25 0.0267(12) 0.0406(14) 0.0311(13) 0.0008(11) -0.0115(11) -0.0120(11) C26 0.0320(14) 0.0590(19) 0.0448(17) -0.0106(14) -0.0105(13) -0.0026(13) C27 0.0427(17) 0.076(2) 0.0464(17) -0.0141(16) -0.0191(14) -0.0204(15) N2 0.0545(14) 0.0388(13) 0.0425(13) 0.0026(10) -0.0250(12) -0.0196(11) C28 0.0594(18) 0.0354(15) 0.0442(16) 0.0008(12) -0.0256(15) -0.0166(13) C29 0.107(3) 0.079(3) 0.067(2) -0.008(2) -0.055(2) -0.030(2) N3 0.167(5) 0.174(5) 0.132(4) 0.061(4) -0.082(4) -0.083(4) C30 0.099(3) 0.085(3) 0.077(3) 0.007(2) -0.023(3) -0.047(3) C31 0.085(3) 0.054(2) 0.072(3) -0.0138(18) -0.016(2) -0.0234(19) _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 I1 Cu1 2.5971(6) . ? I1 Cu1 2.6742(5) 2_675 ? I2 Cu2 2.5989(5) 2_666 ? I2 Cu2 2.6507(5) . ? Cu1 S1 2.3041(8) . ? Cu1 S2 2.3258(7) . ? Cu1 Cu1 2.6138(7) 2_675 ? Cu1 I1 2.6742(5) 2_675 ? Cu2 N2 2.004(2) . ? Cu2 S3 2.3300(7) . ? Cu2 I2 2.5989(5) 2_666 ? Cu2 Cu2 2.7321(8) 2_666 ? N1 C1 1.423(3) . ? N1 C2 1.424(3) . ? N1 C3 1.426(3) . ? S1 C4 1.787(2) . ? S1 C1 1.878(2) . ? S2 C12 1.778(2) . ? S2 C2 1.867(2) . ? S3 C20 1.790(2) . ? S3 C3 1.854(2) . ? C4 C9 1.386(4) . ? C4 C5 1.403(3) . ? C5 C6 1.392(4) . ? C5 C10 1.505(4) . ? C6 C7 1.382(4) . ? C7 C8 1.387(4) . ? C7 C11 1.511(4) . ? C8 C9 1.382(4) . ? C12 C17 1.392(3) . ? C12 C13 1.402(3) . ? C13 C14 1.391(3) . ? C13 C18 1.502(3) . ? C14 C15 1.384(3) . ? C15 C16 1.394(3) . ? C15 C19 1.507(3) . ? C16 C17 1.378(3) . ? C20 C25 1.390(3) . ? C20 C21 1.395(3) . ? C21 C22 1.391(4) . ? C21 C26 1.505(4) . ? C22 C23 1.386(4) . ? C23 C24 1.387(4) . ? C23 C27 1.511(4) . ? C24 C25 1.380(4) . ? N2 C28 1.127(3) . ? C28 C29 1.463(4) . ? N3 C30 1.109(6) . ? C30 C31 1.440(6) . ? 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 Cu1 I1 Cu1 59.432(14) . 2_675 ? Cu2 I2 Cu2 62.715(17) 2_666 . ? S1 Cu1 S2 103.12(3) . . ? S1 Cu1 I1 114.978(19) . . ? S2 Cu1 I1 109.94(2) . . ? S1 Cu1 Cu1 142.48(2) . 2_675 ? S2 Cu1 Cu1 113.11(3) . 2_675 ? I1 Cu1 Cu1 61.753(14) . 2_675 ? S1 Cu1 I1 111.42(2) . 2_675 ? S2 Cu1 I1 93.01(2) . 2_675 ? I1 Cu1 I1 120.568(14) . 2_675 ? Cu1 Cu1 I1 58.815(18) 2_675 2_675 ? N2 Cu2 S3 109.55(7) . . ? N2 Cu2 I2 111.81(7) . 2_666 ? S3 Cu2 I2 104.52(2) . 2_666 ? N2 Cu2 I2 104.63(7) . . ? S3 Cu2 I2 108.96(2) . . ? I2 Cu2 I2 117.285(17) 2_666 . ? N2 Cu2 Cu2 126.75(7) . 2_666 ? S3 Cu2 Cu2 123.63(2) . 2_666 ? I2 Cu2 Cu2 59.569(14) 2_666 2_666 ? I2 Cu2 Cu2 57.716(14) . 2_666 ? C1 N1 C2 120.21(19) . . ? C1 N1 C3 117.6(2) . . ? C2 N1 C3 120.1(2) . . ? C4 S1 C1 99.65(11) . . ? C4 S1 Cu1 117.38(8) . . ? C1 S1 Cu1 97.72(8) . . ? C12 S2 C2 101.97(11) . . ? C12 S2 Cu1 111.95(8) . . ? C2 S2 Cu1 102.99(8) . . ? C20 S3 C3 100.47(11) . . ? C20 S3 Cu2 110.91(8) . . ? C3 S3 Cu2 104.94(8) . . ? N1 C1 S1 111.94(17) . . ? N1 C2 S2 117.50(16) . . ? N1 C3 S3 109.22(16) . . ? C9 C4 C5 120.3(2) . . ? C9 C4 S1 120.04(19) . . ? C5 C4 S1 119.66(18) . . ? C6 C5 C4 117.5(2) . . ? C6 C5 C10 119.7(2) . . ? C4 C5 C10 122.8(2) . . ? C7 C6 C5 122.9(2) . . ? C6 C7 C8 118.0(2) . . ? C6 C7 C11 119.8(2) . . ? C8 C7 C11 122.2(2) . . ? C9 C8 C7 120.9(2) . . ? C8 C9 C4 120.3(2) . . ? C17 C12 C13 120.6(2) . . ? C17 C12 S2 119.62(18) . . ? C13 C12 S2 119.72(17) . . ? C14 C13 C12 117.3(2) . . ? C14 C13 C18 121.2(2) . . ? C12 C13 C18 121.6(2) . . ? C15 C14 C13 123.0(2) . . ? C14 C15 C16 118.2(2) . . ? C14 C15 C19 121.7(2) . . ? C16 C15 C19 120.0(2) . . ? C17 C16 C15 120.5(2) . . ? C16 C17 C12 120.3(2) . . ? C25 C20 C21 120.7(2) . . ? C25 C20 S3 119.43(18) . . ? C21 C20 S3 119.85(19) . . ? C22 C21 C20 117.3(2) . . ? C22 C21 C26 119.4(2) . . ? C20 C21 C26 123.3(2) . . ? C23 C22 C21 123.0(2) . . ? C22 C23 C24 118.2(2) . . ? C22 C23 C27 121.1(2) . . ? C24 C23 C27 120.7(2) . . ? C25 C24 C23 120.5(2) . . ? C24 C25 C20 120.3(2) . . ? C28 N2 Cu2 174.8(3) . . ? N2 C28 C29 179.1(4) . . ? N3 C30 C31 178.5(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.658 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.070 #===END data_042CPI07 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-(2,4-Dimethyl-phenylsulfanylmethyl)-6,8-dimethyl-2H-benzo[e][1,3] thiazin-3-ium perchlorate ; _chemical_name_common ? _chemical_melting_point 421-425 _chemical_formula_moiety 'C19 H22 N S2, Cl O4' _chemical_formula_sum 'C19 H22 Cl N O4 S2' _chemical_formula_weight 427.95 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.887(3) _cell_length_b 14.107(4) _cell_length_c 16.121(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.751(5) _cell_angle_gamma 90.00 _cell_volume 1997.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2125 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 23.21 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.93234 _exptl_absorpt_correction_T_max 0.98431 _exptl_absorpt_process_details '(Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Apex CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 0.661 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14304 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.37 _reflns_number_total 3643 _reflns_number_gt 1851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V 5.625 (Bruker, 1999)' _computing_cell_refinement 'SMART V 5.625 (Bruker, 1999)' _computing_data_reduction 'SAINT V 6.23C (Bruker, 1999)' _computing_structure_solution 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL V 6.12 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V 6.12 (Sheldrick, 2000)' _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^)+(0.0304P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3643 _refine_ls_number_parameters 327 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.889 _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 S1 S 0.36856(15) 0.36518(10) -0.0027(2) 0.0476(7) Uani 0.950(9) 1 d PD A 1 S1B S 0.3727(15) 0.3565(16) -0.044(4) 0.0476(7) Uani 0.050(9) 1 d PD A 2 S2 S 0.36724(15) 0.14415(9) 0.18645(8) 0.0484(4) Uani 1 1 d . A . C2 C 0.3650(5) 0.2400(3) -0.0052(3) 0.0526(14) Uani 1 1 d D . . H2A H 0.3587 0.2187 -0.0642 0.063 Uiso 0.950(9) 1 calc PR A 1 H2B H 0.4615 0.2156 0.0263 0.063 Uiso 0.950(9) 1 calc PR A 1 H2C H 0.3856 0.1949 -0.0492 0.063 Uiso 0.050(9) 1 d PR A 2 H2D H 0.4543 0.2368 0.0396 0.063 Uiso 0.050(9) 1 d PR A 2 N3 N 0.2362(4) 0.1988(3) 0.0308(2) 0.0358(9) Uani 1 1 d . A . C4 C 0.1027(5) 0.2347(3) 0.0121(2) 0.0328(11) Uani 1 1 d . . . H4 H 0.0209 0.2023 0.0314 0.039 Uiso 1 1 calc R A . C5 C -0.0858(5) 0.3375(3) -0.0666(3) 0.0350(11) Uani 1 1 d . . . H5 H -0.1607 0.2923 -0.0573 0.042 Uiso 1 1 calc R A . C6 C -0.1298(5) 0.4195(3) -0.1104(3) 0.0366(12) Uani 1 1 d . A . C7 C -0.0146(5) 0.4848(3) -0.1194(3) 0.0395(12) Uani 1 1 d . . . H7 H -0.0430 0.5425 -0.1480 0.047 Uiso 1 1 calc R A . C8 C 0.1377(5) 0.4707(3) -0.0891(3) 0.0371(12) Uani 1 1 d . A . C9 C 0.1787(5) 0.3854(3) -0.0486(3) 0.0333(11) Uani 1 1 d D . . C10 C 0.0669(5) 0.3199(3) -0.0359(2) 0.0305(11) Uani 1 1 d . A . C11 C -0.2921(5) 0.4374(3) -0.1487(3) 0.0508(14) Uani 1 1 d . . . H11A H -0.3051 0.4231 -0.2089 0.076 Uiso 1 1 calc R A . H11B H -0.3175 0.5041 -0.1408 0.076 Uiso 1 1 calc R . . H11C H -0.3597 0.3968 -0.1216 0.076 Uiso 1 1 calc R . . C12 C 0.2562(5) 0.5438(3) -0.1003(3) 0.0577(15) Uani 1 1 d . . . H12A H 0.3104 0.5624 -0.0452 0.087 Uiso 1 1 calc R A . H12B H 0.2054 0.5999 -0.1282 0.087 Uiso 1 1 calc R . . H12C H 0.3273 0.5177 -0.1345 0.087 Uiso 1 1 calc R . . C13 C 0.2347(5) 0.2202(3) 0.2259(2) 0.0350(11) Uani 1 1 d . . . C14 C 0.2877(5) 0.3056(3) 0.2651(3) 0.0401(12) Uani 1 1 d . . . C15 C 0.1811(6) 0.3616(3) 0.2972(3) 0.0441(13) Uani 1 1 d . . . H15 H 0.2153 0.4186 0.3252 0.053 Uiso 1 1 calc R . . C16 C 0.0279(6) 0.3391(3) 0.2909(3) 0.0382(12) Uani 1 1 d . . . C17 C -0.0198(5) 0.2555(3) 0.2507(3) 0.0380(12) Uani 1 1 d . . . H17 H -0.1244 0.2387 0.2442 0.046 Uiso 1 1 calc R . . C18 C 0.0817(5) 0.1961(3) 0.2198(3) 0.0405(12) Uani 1 1 d . . . H18 H 0.0467 0.1379 0.1940 0.049 Uiso 1 1 calc R . . C19 C 0.4514(5) 0.3355(3) 0.2731(3) 0.0575(15) Uani 1 1 d . . . H19A H 0.4623 0.4001 0.2957 0.086 Uiso 1 1 calc R . . H19B H 0.4842 0.3339 0.2178 0.086 Uiso 1 1 calc R . . H19C H 0.5145 0.2922 0.3112 0.086 Uiso 1 1 calc R . . C20 C -0.0828(5) 0.4033(3) 0.3256(3) 0.0544(14) Uani 1 1 d . . . H20A H -0.0415 0.4208 0.3834 0.082 Uiso 1 1 calc R . . H20B H -0.1800 0.3702 0.3248 0.082 Uiso 1 1 calc R . . H20C H -0.0990 0.4607 0.2910 0.082 Uiso 1 1 calc R . . C21 C 0.2671(5) 0.1150(3) 0.0847(3) 0.0419(12) Uani 1 1 d . . . H21A H 0.3282 0.0692 0.0573 0.050 Uiso 1 1 calc R A . H21B H 0.1695 0.0841 0.0910 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.72978(14) 0.10653(8) 0.05492(9) 0.0477(4) Uani 1 1 d D . . O1 O 0.8788(12) 0.0651(13) 0.0616(11) 0.039(3) Uani 0.418(8) 1 d PDU B 1 O2 O 0.7379(16) 0.2010(5) 0.0878(7) 0.049(2) Uani 0.418(8) 1 d PDU B 1 O3 O 0.6661(11) 0.1153(7) -0.0342(4) 0.052(2) Uani 0.418(8) 1 d PDU B 1 O4 O 0.6287(10) 0.0471(6) 0.0923(7) 0.0498(17) Uani 0.418(8) 1 d PDU B 1 O1B O 0.869(3) 0.059(3) 0.0427(17) 0.038(3) Uani 0.302(8) 1 d PDU B 2 O2B O 0.763(2) 0.2066(7) 0.0553(17) 0.045(3) Uani 0.302(8) 1 d PDU B 2 O3B O 0.6133(14) 0.0836(10) -0.0160(8) 0.049(2) Uani 0.302(8) 1 d PDU B 2 O4B O 0.6741(18) 0.0756(10) 0.1299(9) 0.0500(18) Uani 0.302(8) 1 d PDU B 2 O1C O 0.866(4) 0.068(4) 0.030(2) 0.037(3) Uani 0.281(5) 1 d PDU B 3 O2C O 0.717(3) 0.2082(6) 0.0494(18) 0.046(3) Uani 0.281(5) 1 d PDU B 3 O3C O 0.5964(11) 0.0484(9) 0.0371(11) 0.0509(17) Uani 0.281(5) 1 d PDU B 3 O4C O 0.7565(15) 0.1001(8) 0.1465(5) 0.0511(18) Uani 0.281(5) 1 d PDU B 3 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 S1 0.0275(8) 0.0631(10) 0.0497(18) 0.0101(8) -0.0019(7) -0.0097(6) S1B 0.0275(8) 0.0631(10) 0.0497(18) 0.0101(8) -0.0019(7) -0.0097(6) S2 0.0431(9) 0.0563(9) 0.0431(8) 0.0006(7) -0.0015(6) 0.0131(7) C2 0.031(3) 0.084(4) 0.044(3) 0.000(3) 0.009(2) 0.016(3) N3 0.027(2) 0.045(2) 0.036(2) -0.0017(19) 0.0040(19) 0.006(2) C4 0.026(3) 0.040(3) 0.033(3) -0.008(2) 0.005(2) 0.002(2) C5 0.025(3) 0.044(3) 0.037(3) -0.003(2) 0.009(2) -0.004(2) C6 0.034(3) 0.048(3) 0.027(3) 0.000(2) 0.003(2) 0.003(2) C7 0.041(3) 0.041(3) 0.035(3) 0.005(2) 0.002(2) 0.000(3) C8 0.038(3) 0.046(3) 0.027(3) -0.004(2) 0.003(2) -0.010(2) C9 0.025(3) 0.048(3) 0.027(2) -0.002(2) 0.004(2) -0.006(2) C10 0.027(3) 0.037(3) 0.028(3) -0.004(2) 0.005(2) 0.001(2) C11 0.032(3) 0.062(3) 0.056(3) 0.009(3) -0.001(3) 0.006(3) C12 0.048(4) 0.062(4) 0.062(4) 0.015(3) 0.003(3) -0.021(3) C13 0.043(3) 0.036(3) 0.024(3) 0.003(2) 0.000(2) 0.002(2) C14 0.045(3) 0.041(3) 0.033(3) 0.007(2) -0.001(2) -0.003(3) C15 0.065(4) 0.035(3) 0.030(3) -0.002(2) 0.000(3) -0.007(3) C16 0.052(4) 0.034(3) 0.028(3) 0.006(2) 0.006(2) 0.005(3) C17 0.042(3) 0.036(3) 0.036(3) 0.000(2) 0.006(2) 0.002(2) C18 0.045(3) 0.035(3) 0.041(3) -0.002(2) 0.004(2) -0.004(3) C19 0.054(4) 0.061(3) 0.054(3) -0.005(3) -0.001(3) -0.016(3) C20 0.068(4) 0.045(3) 0.054(3) -0.001(3) 0.021(3) 0.006(3) C21 0.040(3) 0.041(3) 0.045(3) -0.006(2) 0.007(2) 0.009(2) Cl1 0.0347(8) 0.0389(7) 0.0720(9) -0.0012(7) 0.0157(7) 0.0004(6) O1 0.024(3) 0.065(5) 0.026(8) -0.002(5) 0.001(4) 0.010(3) O2 0.035(4) 0.042(3) 0.070(5) -0.011(3) 0.011(5) -0.008(2) O3 0.031(4) 0.059(4) 0.063(4) 0.000(3) 0.002(3) -0.007(3) O4 0.028(4) 0.050(3) 0.072(4) -0.004(3) 0.010(3) -0.020(3) O1B 0.023(3) 0.064(5) 0.025(9) -0.003(6) 0.002(4) 0.009(3) O2B 0.033(6) 0.038(3) 0.067(5) -0.009(3) 0.013(6) -0.005(3) O3B 0.020(4) 0.051(4) 0.073(4) -0.007(4) -0.002(4) -0.020(3) O4B 0.028(4) 0.050(3) 0.076(4) -0.001(3) 0.020(4) -0.021(3) O1C 0.022(3) 0.064(5) 0.026(9) -0.003(6) 0.003(5) 0.008(3) O2C 0.034(6) 0.040(3) 0.066(5) -0.008(4) 0.012(6) -0.007(3) O3C 0.028(3) 0.053(3) 0.072(4) -0.005(3) 0.008(3) -0.018(3) O4C 0.031(4) 0.049(3) 0.076(4) -0.008(3) 0.015(4) -0.017(3) _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 S1 C9 1.759(4) . ? S1 C2 1.767(5) . ? S1B C9 1.762(7) . ? S1B C2 1.766(7) . ? S2 C13 1.781(4) . ? S2 C21 1.791(4) . ? C2 N3 1.479(5) . ? N3 C4 1.284(5) . ? N3 C21 1.467(5) . ? C4 C10 1.439(5) . ? C5 C6 1.381(5) . ? C5 C10 1.394(5) . ? C6 C7 1.401(6) . ? C6 C11 1.502(5) . ? C7 C8 1.382(6) . ? C8 C9 1.392(6) . ? C8 C12 1.504(5) . ? C9 C10 1.395(5) . ? C13 C18 1.391(6) . ? C13 C14 1.407(6) . ? C14 C15 1.392(6) . ? C14 C19 1.502(6) . ? C15 C16 1.386(6) . ? C16 C17 1.380(5) . ? C16 C20 1.507(6) . ? C17 C18 1.379(6) . ? Cl1 O4 1.427(6) . ? Cl1 O2 1.431(7) . ? Cl1 O3C 1.434(8) . ? Cl1 O2C 1.440(9) . ? Cl1 O1 1.437(7) . ? Cl1 O1C 1.444(9) . ? Cl1 O2B 1.442(9) . ? Cl1 O4B 1.442(9) . ? Cl1 O1B 1.446(9) . ? Cl1 O3B 1.457(9) . ? Cl1 O4C 1.462(8) . ? Cl1 O3 1.467(6) . ? 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 C9 S1 C2 98.0(2) . . ? C9 S1B C2 97.9(4) . . ? C13 S2 C21 101.7(2) . . ? N3 C2 S1B 125.5(6) . . ? N3 C2 S1 113.3(3) . . ? C4 N3 C21 122.6(4) . . ? C4 N3 C2 119.7(4) . . ? C21 N3 C2 117.6(4) . . ? N3 C4 C10 125.2(4) . . ? C6 C5 C10 121.0(4) . . ? C5 C6 C7 116.7(4) . . ? C5 C6 C11 122.1(4) . . ? C7 C6 C11 121.2(4) . . ? C8 C7 C6 124.1(4) . . ? C9 C8 C7 117.6(4) . . ? C9 C8 C12 120.8(4) . . ? C7 C8 C12 121.7(4) . . ? C8 C9 C10 120.0(4) . . ? C8 C9 S1 120.2(3) . . ? C10 C9 S1 119.4(3) . . ? C8 C9 S1B 113.7(5) . . ? C10 C9 S1B 123.8(5) . . ? C5 C10 C9 120.5(4) . . ? C5 C10 C4 117.6(4) . . ? C9 C10 C4 121.9(4) . . ? C18 C13 C14 119.9(4) . . ? C18 C13 S2 121.3(3) . . ? C14 C13 S2 118.8(4) . . ? C15 C14 C13 116.9(4) . . ? C15 C14 C19 120.9(4) . . ? C13 C14 C19 122.2(4) . . ? C16 C15 C14 124.0(4) . . ? C17 C16 C15 117.3(4) . . ? C17 C16 C20 121.1(5) . . ? C15 C16 C20 121.6(4) . . ? C18 C17 C16 121.2(5) . . ? C17 C18 C13 120.7(4) . . ? N3 C21 S2 112.3(3) . . ? O4 Cl1 O2 112.9(5) . . ? O3C Cl1 O2C 120.0(10) . . ? O4 Cl1 O1 111.2(8) . . ? O2 Cl1 O1 110.9(8) . . ? O3C Cl1 O1C 116(2) . . ? O2C Cl1 O1C 115(2) . . ? O2B Cl1 O4B 112.9(12) . . ? O2B Cl1 O1B 106(2) . . ? O4B Cl1 O1B 112.5(14) . . ? O2B Cl1 O3B 109.9(11) . . ? O4B Cl1 O3B 107.3(7) . . ? O1B Cl1 O3B 108.0(16) . . ? O3C Cl1 O4C 99.7(8) . . ? O2C Cl1 O4C 97.1(12) . . ? O1C Cl1 O4C 104.3(14) . . ? O4 Cl1 O3 106.8(4) . . ? O2 Cl1 O3 105.9(5) . . ? O1 Cl1 O3 108.8(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.506 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.059