# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'P Braunstein' 'Suyun Jie.' 'Jens Kortus' 'Claudia Loose' 'Roberto Pattacini' 'Guillaume Rogez' _publ_contact_author_name 'P Braunstein' _publ_contact_author_email BRAUNST@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis, Structure, Magnetic and Catalytic Properties of New Dinuclear Chromium(III) Complexes with Oxazoline Alcoholate Ligands ; # Attachment 'CIF_COMBINED_Cr.cif' data_Complex6 _database_code_depnum_ccdc_archive 'CCDC 690755' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Cl3 Cr2 N3 O6' _chemical_formula_sum 'C18 H30 Cl3 Cr2 N3 O6' _chemical_formula_weight 594.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7526(2) _cell_length_b 14.4126(5) _cell_length_c 19.5866(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2470.80(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3064 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18007 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5646 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 version2.0' _computing_publication_material PLATON _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^)+(0.0317P)^2^+0.3497P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(17) _refine_ls_number_reflns 5646 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _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 Cr1 Cr 0.06814(5) 0.46220(3) 0.46969(2) 0.01929(11) Uani 1 1 d . . . Cr2 Cr 0.10579(5) 0.36226(3) 0.35195(2) 0.01903(11) Uani 1 1 d . . . O1 O -0.0685(2) 0.37607(12) 0.41712(9) 0.0192(4) Uani 1 1 d . . . O2 O -0.3578(2) 0.55401(15) 0.42026(11) 0.0307(5) Uani 1 1 d . . . O3 O 0.1160(2) 0.49682(13) 0.37140(10) 0.0225(4) Uani 1 1 d . . . O4 O 0.4630(2) 0.50928(15) 0.27342(11) 0.0364(5) Uani 1 1 d . . . O5 O 0.2141(2) 0.36193(14) 0.44181(9) 0.0200(4) Uani 1 1 d . . . O6 O 0.1369(2) 0.11664(14) 0.45173(11) 0.0279(5) Uani 1 1 d . . . N1 N -0.1231(2) 0.54343(16) 0.46609(12) 0.0211(5) Uani 1 1 d . . . N2 N 0.3018(3) 0.39300(16) 0.29871(12) 0.0224(5) Uani 1 1 d . . . N3 N 0.1123(2) 0.22116(16) 0.36721(12) 0.0209(5) Uani 1 1 d . . . Cl1 Cl 0.23909(8) 0.56728(5) 0.51501(4) 0.02948(18) Uani 1 1 d . . . Cl2 Cl 0.00465(8) 0.40441(5) 0.57542(4) 0.02640(17) Uani 1 1 d . . . Cl3 Cl -0.03786(8) 0.36059(5) 0.25308(4) 0.02709(16) Uani 1 1 d . . . C1 C -0.2139(3) 0.4126(2) 0.39954(15) 0.0237(7) Uani 1 1 d . . . H1A H -0.2956 0.3714 0.4168 0.028 Uiso 1 1 calc R . . H1B H -0.2236 0.4170 0.3493 0.028 Uiso 1 1 calc R . . C2 C -0.2287(3) 0.5059(2) 0.43051(15) 0.0228(6) Uani 1 1 d . . . C3 C -0.3421(3) 0.6366(2) 0.46367(17) 0.0311(7) Uani 1 1 d . . . H3A H -0.4053 0.6307 0.5054 0.037 Uiso 1 1 calc R . . H3B H -0.3734 0.6932 0.4387 0.037 Uiso 1 1 calc R . . C4 C -0.1705(3) 0.6403(2) 0.48194(16) 0.0250(6) Uani 1 1 d . . . C5 C -0.1443(4) 0.6635(2) 0.55666(16) 0.0313(8) Uani 1 1 d . . . H5A H -0.2029 0.6206 0.5853 0.047 Uiso 1 1 calc R . . H5B H -0.1778 0.7273 0.5656 0.047 Uiso 1 1 calc R . . H5C H -0.0353 0.6577 0.5673 0.047 Uiso 1 1 calc R . . C6 C -0.0810(4) 0.7048(2) 0.43508(16) 0.0315(7) Uani 1 1 d . . . H6A H 0.0285 0.6980 0.4441 0.047 Uiso 1 1 calc R . . H6B H -0.1119 0.7691 0.4436 0.047 Uiso 1 1 calc R . . H6C H -0.1022 0.6888 0.3874 0.047 Uiso 1 1 calc R . . C7 C 0.2495(3) 0.5433(2) 0.34817(17) 0.0310(7) Uani 1 1 d . . . H7A H 0.3111 0.5644 0.3876 0.037 Uiso 1 1 calc R . . H7B H 0.2208 0.5983 0.3207 0.037 Uiso 1 1 calc R . . C8 C 0.3387(3) 0.4779(2) 0.30614(15) 0.0266(7) Uani 1 1 d . . . C9 C 0.5179(3) 0.4310(2) 0.23302(16) 0.0322(8) Uani 1 1 d . . . H9A H 0.6262 0.4176 0.2438 0.039 Uiso 1 1 calc R . . H9B H 0.5094 0.4447 0.1836 0.039 Uiso 1 1 calc R . . C10 C 0.4152(3) 0.3474(2) 0.25239(14) 0.0262(7) Uani 1 1 d . . . C11 C 0.5015(4) 0.2731(2) 0.29138(18) 0.0386(8) Uani 1 1 d . . . H11A H 0.5463 0.3003 0.3327 0.058 Uiso 1 1 calc R . . H11B H 0.5829 0.2479 0.2625 0.058 Uiso 1 1 calc R . . H11C H 0.4310 0.2232 0.3042 0.058 Uiso 1 1 calc R . . C12 C 0.3355(4) 0.3067(3) 0.19067(17) 0.0430(9) Uani 1 1 d . . . H12A H 0.2573 0.2625 0.2057 0.064 Uiso 1 1 calc R . . H12B H 0.4104 0.2745 0.1620 0.064 Uiso 1 1 calc R . . H12C H 0.2873 0.3566 0.1644 0.064 Uiso 1 1 calc R . . C13 C 0.2238(3) 0.27343(19) 0.47390(16) 0.0249(7) Uani 1 1 d . . . H13A H 0.1675 0.2744 0.5177 0.030 Uiso 1 1 calc R . . H13B H 0.3319 0.2581 0.4835 0.030 Uiso 1 1 calc R . . C14 C 0.1571(3) 0.2029(2) 0.42806(16) 0.0211(6) Uani 1 1 d . . . C15 C 0.0925(4) 0.0614(2) 0.39144(16) 0.0321(7) Uani 1 1 d . . . H15A H 0.0084 0.0180 0.4027 0.039 Uiso 1 1 calc R . . H15B H 0.1803 0.0254 0.3738 0.039 Uiso 1 1 calc R . . C16 C 0.0399(3) 0.1342(2) 0.33914(15) 0.0233(6) Uani 1 1 d . . . C17 C 0.0973(4) 0.1134(2) 0.26797(16) 0.0347(8) Uani 1 1 d . . . H17A H 0.0626 0.1620 0.2366 0.052 Uiso 1 1 calc R . . H17B H 0.0573 0.0532 0.2530 0.052 Uiso 1 1 calc R . . H17C H 0.2092 0.1114 0.2682 0.052 Uiso 1 1 calc R . . C18 C -0.1339(3) 0.1459(2) 0.34003(17) 0.0342(8) Uani 1 1 d . . . H18A H -0.1630 0.1960 0.3088 0.051 Uiso 1 1 calc R . . H18B H -0.1674 0.1613 0.3864 0.051 Uiso 1 1 calc R . . H18C H -0.1824 0.0880 0.3254 0.051 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 Cr1 0.0215(2) 0.0173(2) 0.0190(2) -0.00196(19) -0.0045(2) 0.00029(18) Cr2 0.0220(2) 0.0172(2) 0.0178(2) -0.00095(19) -0.00173(19) -0.00086(19) O1 0.0199(9) 0.0186(10) 0.0191(10) -0.0010(8) -0.0031(8) 0.0003(8) O2 0.0267(11) 0.0340(13) 0.0314(12) -0.0088(10) -0.0087(9) 0.0092(9) O3 0.0288(10) 0.0186(10) 0.0201(10) 0.0000(8) -0.0020(9) -0.0036(9) O4 0.0409(13) 0.0370(13) 0.0312(13) -0.0016(10) 0.0084(11) -0.0192(10) O5 0.0239(9) 0.0174(10) 0.0187(10) -0.0006(9) -0.0043(8) 0.0016(9) O6 0.0347(11) 0.0195(12) 0.0295(12) 0.0048(9) -0.0021(9) -0.0005(9) N1 0.0247(11) 0.0194(12) 0.0193(13) -0.0031(11) -0.0057(11) 0.0025(10) N2 0.0251(12) 0.0239(13) 0.0182(14) 0.0013(11) 0.0016(11) -0.0012(10) N3 0.0223(12) 0.0167(12) 0.0238(14) -0.0024(10) 0.0006(11) 0.0016(10) Cl1 0.0296(4) 0.0279(4) 0.0309(4) -0.0075(3) -0.0073(3) -0.0064(3) Cl2 0.0287(4) 0.0297(4) 0.0207(4) 0.0021(3) -0.0024(3) 0.0014(3) Cl3 0.0310(4) 0.0291(4) 0.0212(4) -0.0016(3) -0.0061(3) 0.0011(3) C1 0.0216(14) 0.0296(17) 0.0200(16) -0.0048(13) -0.0048(12) 0.0004(13) C2 0.0225(14) 0.0274(16) 0.0185(16) 0.0025(13) -0.0017(13) 0.0018(12) C3 0.0336(16) 0.0285(16) 0.0312(18) -0.0085(16) -0.0082(14) 0.0083(14) C4 0.0293(14) 0.0201(14) 0.0257(16) -0.0031(14) -0.0044(13) 0.0079(13) C5 0.0381(18) 0.0285(18) 0.0275(18) -0.0054(14) -0.0028(14) 0.0051(14) C6 0.0416(18) 0.0224(16) 0.0307(18) 0.0015(14) -0.0032(16) 0.0034(15) C7 0.0396(17) 0.0232(16) 0.0302(18) -0.0021(14) -0.0002(15) -0.0087(15) C8 0.0335(16) 0.0295(18) 0.0167(16) 0.0013(13) -0.0033(13) -0.0098(14) C9 0.0282(15) 0.0400(19) 0.0283(18) 0.0014(15) 0.0042(14) -0.0077(14) C10 0.0250(14) 0.0331(17) 0.0204(15) -0.0042(13) 0.0045(13) -0.0037(14) C11 0.0354(17) 0.035(2) 0.045(2) 0.0000(16) 0.0011(17) 0.0039(16) C12 0.0386(18) 0.065(3) 0.0253(19) -0.0087(18) 0.0037(16) -0.0165(18) C13 0.0300(15) 0.0246(16) 0.0201(16) 0.0012(13) -0.0028(14) 0.0077(12) C14 0.0230(14) 0.0161(14) 0.0242(17) -0.0002(13) 0.0020(13) 0.0046(11) C15 0.0399(17) 0.0185(16) 0.038(2) -0.0016(14) -0.0054(16) -0.0032(14) C16 0.0255(14) 0.0183(14) 0.0260(16) -0.0026(12) -0.0006(13) -0.0049(12) C17 0.0442(19) 0.0257(17) 0.0342(19) -0.0077(14) 0.0070(16) -0.0053(15) C18 0.0296(16) 0.0341(19) 0.039(2) -0.0003(17) -0.0025(14) -0.0080(14) _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 Cr1 O5 2.0048(19) . ? Cr1 O1 2.0078(18) . ? Cr1 O3 2.032(2) . ? Cr1 N1 2.044(2) . ? Cr1 Cl2 2.3003(9) . ? Cr1 Cl1 2.3066(8) . ? Cr1 Cr2 2.7388(6) . ? Cr2 O3 1.9784(19) . ? Cr2 O5 1.9992(18) . ? Cr2 O1 1.9989(19) . ? Cr2 N2 2.056(2) . ? Cr2 N3 2.056(2) . ? Cr2 Cl3 2.3091(8) . ? O1 C1 1.420(3) . ? O2 C2 1.340(3) . ? O2 C3 1.469(4) . ? O3 C7 1.422(3) . ? O4 C8 1.341(3) . ? O4 C9 1.460(4) . ? O5 C13 1.424(3) . ? O6 C14 1.338(3) . ? O6 C15 1.476(4) . ? N1 C2 1.278(4) . ? N1 C4 1.489(4) . ? N2 C8 1.274(4) . ? N2 C10 1.496(4) . ? N3 C14 1.282(4) . ? N3 C16 1.509(4) . ? C1 C2 1.481(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.545(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.519(4) . ? C4 C6 1.523(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.475(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.551(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.514(4) . ? C10 C11 1.517(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.477(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.537(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.512(4) . ? C16 C18 1.531(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 O5 Cr1 O1 78.13(7) . . ? O5 Cr1 O3 77.74(8) . . ? O1 Cr1 O3 77.80(7) . . ? O5 Cr1 N1 157.74(9) . . ? O1 Cr1 N1 81.30(8) . . ? O3 Cr1 N1 89.73(9) . . ? O5 Cr1 Cl2 97.94(6) . . ? O1 Cr1 Cl2 95.39(6) . . ? O3 Cr1 Cl2 172.51(6) . . ? N1 Cr1 Cl2 92.33(7) . . ? O5 Cr1 Cl1 99.48(6) . . ? O1 Cr1 Cl1 171.76(6) . . ? O3 Cr1 Cl1 94.00(6) . . ? N1 Cr1 Cl1 99.70(7) . . ? Cl2 Cr1 Cl1 92.75(3) . . ? O5 Cr1 Cr2 46.76(5) . . ? O1 Cr1 Cr2 46.74(5) . . ? O3 Cr1 Cr2 46.11(5) . . ? N1 Cr1 Cr2 111.76(7) . . ? Cl2 Cr1 Cr2 126.63(3) . . ? Cl1 Cr1 Cr2 126.25(3) . . ? O3 Cr2 O5 79.13(8) . . ? O3 Cr2 O1 79.27(8) . . ? O5 Cr2 O1 78.46(7) . . ? O3 Cr2 N2 81.31(9) . . ? O5 Cr2 N2 92.94(8) . . ? O1 Cr2 N2 159.92(9) . . ? O3 Cr2 N3 160.09(9) . . ? O5 Cr2 N3 81.75(9) . . ? O1 Cr2 N3 91.54(8) . . ? N2 Cr2 N3 105.28(9) . . ? O3 Cr2 Cl3 101.31(6) . . ? O5 Cr2 Cl3 175.26(6) . . ? O1 Cr2 Cl3 96.95(6) . . ? N2 Cr2 Cl3 91.79(7) . . ? N3 Cr2 Cl3 97.29(7) . . ? O3 Cr2 Cr1 47.76(6) . . ? O5 Cr2 Cr1 46.93(5) . . ? O1 Cr2 Cr1 47.01(5) . . ? N2 Cr2 Cr1 114.46(7) . . ? N3 Cr2 Cr1 113.65(7) . . ? Cl3 Cr2 Cr1 130.25(3) . . ? C1 O1 Cr2 124.47(17) . . ? C1 O1 Cr1 115.38(16) . . ? Cr2 O1 Cr1 86.24(7) . . ? C2 O2 C3 104.7(2) . . ? C7 O3 Cr2 115.95(17) . . ? C7 O3 Cr1 126.02(17) . . ? Cr2 O3 Cr1 86.13(8) . . ? C8 O4 C9 105.4(2) . . ? C13 O5 Cr2 114.76(16) . . ? C13 O5 Cr1 124.27(16) . . ? Cr2 O5 Cr1 86.32(7) . . ? C14 O6 C15 105.0(2) . . ? C2 N1 C4 108.0(2) . . ? C2 N1 Cr1 111.67(19) . . ? C4 N1 Cr1 139.28(18) . . ? C8 N2 C10 108.9(2) . . ? C8 N2 Cr2 111.1(2) . . ? C10 N2 Cr2 140.01(19) . . ? C14 N3 C16 107.2(2) . . ? C14 N3 Cr2 110.32(19) . . ? C16 N3 Cr2 139.22(18) . . ? O1 C1 C2 108.5(2) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N1 C2 O2 118.2(3) . . ? N1 C2 C1 122.9(3) . . ? O2 C2 C1 118.8(2) . . ? O2 C3 C4 104.6(2) . . ? O2 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? O2 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? N1 C4 C5 111.5(2) . . ? N1 C4 C6 107.7(2) . . ? C5 C4 C6 111.6(3) . . ? N1 C4 C3 101.0(2) . . ? C5 C4 C3 112.2(3) . . ? C6 C4 C3 112.4(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 108.2(2) . . ? O3 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O3 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N2 C8 O4 118.3(3) . . ? N2 C8 C7 122.9(3) . . ? O4 C8 C7 118.7(3) . . ? O4 C9 C10 106.1(2) . . ? O4 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O4 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N2 C10 C12 110.4(2) . . ? N2 C10 C11 109.6(2) . . ? C12 C10 C11 111.0(3) . . ? N2 C10 C9 101.1(2) . . ? C12 C10 C9 111.9(3) . . ? C11 C10 C9 112.5(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C14 109.0(2) . . ? O5 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? O5 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N3 C14 O6 118.2(3) . . ? N3 C14 C13 123.0(3) . . ? O6 C14 C13 118.8(3) . . ? O6 C15 C16 104.1(2) . . ? O6 C15 H15A 110.9 . . ? C16 C15 H15A 110.9 . . ? O6 C15 H15B 110.9 . . ? C16 C15 H15B 110.9 . . ? H15A C15 H15B 109.0 . . ? N3 C16 C17 111.2(2) . . ? N3 C16 C18 108.7(2) . . ? C17 C16 C18 111.3(3) . . ? N3 C16 C15 101.5(2) . . ? C17 C16 C15 112.3(2) . . ? C18 C16 C15 111.4(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.264 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.069 data_Complex7 _database_code_depnum_ccdc_archive 'CCDC 690756' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Cl4 Cr2 N2 O6' _chemical_formula_sum 'C20 H40 Cl4 Cr2 N2 O6' _chemical_formula_weight 650.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 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 19.4810(7) _cell_length_b 9.5507(3) _cell_length_c 16.9528(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.479(2) _cell_angle_gamma 90.00 _cell_volume 2893.04(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7900 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12332 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4234 _reflns_number_gt 3321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 version2.0' _computing_publication_material PLATON _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^)+(0.0487P)^2^+1.9445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4234 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Cr1 Cr 0.582138(15) 0.04367(3) 0.551302(19) 0.02006(9) Uani 1 1 d . . . O1 O 0.47895(6) 0.10303(13) 0.52885(8) 0.0212(3) Uani 1 1 d . . . O2 O 0.55221(8) 0.39954(16) 0.66598(11) 0.0366(4) Uani 1 1 d . . . O3 O 0.56856(8) 0.16616(15) 0.44689(9) 0.0284(3) Uani 1 1 d . . . N1 N 0.60383(8) 0.22349(16) 0.62189(10) 0.0240(3) Uani 1 1 d . . . Cl1 Cl 0.70105(3) -0.01614(5) 0.56794(3) 0.03124(13) Uani 1 1 d . . . Cl2 Cl 0.59044(3) -0.08545(5) 0.67203(3) 0.03017(12) Uani 1 1 d . . . C1 C 0.46688(10) 0.2291(2) 0.56713(13) 0.0270(4) Uani 1 1 d . . . C2 C 0.54463(11) 0.2829(2) 0.61943(13) 0.0260(4) Uani 1 1 d . . . C3 C 0.63275(12) 0.4255(2) 0.70817(15) 0.0332(5) Uani 1 1 d . . . H3A H 0.6492 0.4259 0.7715 0.040 Uiso 1 1 calc R . . H3B H 0.6456 0.5169 0.6900 0.040 Uiso 1 1 calc R . . C4 C 0.67074(11) 0.3043(2) 0.67975(13) 0.0275(4) Uani 1 1 d . . . C5 C 0.42696(13) 0.1978(3) 0.62644(16) 0.0401(5) Uani 1 1 d . . . H5A H 0.3763 0.1637 0.5923 0.060 Uiso 1 1 calc R . . H5B H 0.4241 0.2834 0.6569 0.060 Uiso 1 1 calc R . . H5C H 0.4548 0.1260 0.6683 0.060 Uiso 1 1 calc R . . C6 C 0.42434(13) 0.3361(2) 0.49815(16) 0.0409(5) Uani 1 1 d . . . H6A H 0.4521 0.3549 0.4622 0.061 Uiso 1 1 calc R . . H6B H 0.4188 0.4232 0.5256 0.061 Uiso 1 1 calc R . . H6C H 0.3748 0.2990 0.4623 0.061 Uiso 1 1 calc R . . C7 C 0.71793(12) 0.2130(2) 0.75481(15) 0.0373(5) Uani 1 1 d . . . H7A H 0.6874 0.1801 0.7851 0.056 Uiso 1 1 calc R . . H7B H 0.7603 0.2674 0.7944 0.056 Uiso 1 1 calc R . . H7C H 0.7366 0.1323 0.7335 0.056 Uiso 1 1 calc R . . C8 C 0.71435(12) 0.3570(2) 0.62896(16) 0.0382(5) Uani 1 1 d . . . H8A H 0.7333 0.2771 0.6074 0.057 Uiso 1 1 calc R . . H8B H 0.7565 0.4144 0.6663 0.057 Uiso 1 1 calc R . . H8C H 0.6814 0.4136 0.5804 0.057 Uiso 1 1 calc R . . C9 C 0.61484(16) 0.1865(3) 0.39972(19) 0.0482(6) Uani 1 1 d . . . H9A H 0.6056 0.1095 0.3576 0.058 Uiso 1 1 calc R . . H9B H 0.6681 0.1821 0.4401 0.058 Uiso 1 1 calc R . . C10 C 0.6008(2) 0.3208(3) 0.3540(2) 0.0638(9) Uani 1 1 d . . . H10A H 0.5475 0.3282 0.3163 0.096 Uiso 1 1 calc R . . H10B H 0.6307 0.3264 0.3193 0.096 Uiso 1 1 calc R . . H10C H 0.6147 0.3977 0.3957 0.096 Uiso 1 1 calc R . . H3O H 0.5281(16) 0.162(3) 0.4155(19) 0.049(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01606(14) 0.02433(16) 0.01937(16) -0.00057(11) 0.00661(11) 0.00048(10) O1 0.0171(6) 0.0238(6) 0.0225(7) -0.0042(5) 0.0076(5) 0.0010(5) O2 0.0276(7) 0.0337(8) 0.0467(10) -0.0173(7) 0.0131(7) -0.0020(6) O3 0.0224(7) 0.0375(8) 0.0257(8) 0.0046(6) 0.0101(6) -0.0022(6) N1 0.0208(7) 0.0263(8) 0.0229(8) -0.0037(6) 0.0065(6) -0.0018(6) Cl1 0.0185(2) 0.0392(3) 0.0352(3) -0.0016(2) 0.0098(2) 0.00288(18) Cl2 0.0264(2) 0.0381(3) 0.0222(2) 0.00593(18) 0.00569(19) -0.00025(19) C1 0.0220(9) 0.0284(9) 0.0304(10) -0.0082(8) 0.0104(8) 0.0012(7) C2 0.0262(9) 0.0259(9) 0.0262(10) -0.0045(7) 0.0107(8) -0.0008(7) C3 0.0268(10) 0.0322(10) 0.0369(12) -0.0103(9) 0.0087(9) -0.0042(8) C4 0.0231(9) 0.0277(9) 0.0289(10) -0.0065(8) 0.0073(8) -0.0041(7) C5 0.0321(11) 0.0544(14) 0.0407(13) -0.0189(11) 0.0218(10) -0.0086(10) C6 0.0326(11) 0.0330(11) 0.0451(14) -0.0027(10) 0.0030(10) 0.0088(9) C7 0.0301(11) 0.0395(12) 0.0318(12) -0.0052(9) 0.0012(9) 0.0005(9) C8 0.0322(11) 0.0388(12) 0.0462(14) -0.0057(10) 0.0184(10) -0.0092(9) C9 0.0534(15) 0.0533(15) 0.0523(16) 0.0120(12) 0.0362(14) 0.0070(12) C10 0.091(2) 0.0459(15) 0.077(2) 0.0193(14) 0.058(2) 0.0063(15) _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 Cr1 O1 1.9743(12) . ? Cr1 O1 1.9842(12) 5_656 ? Cr1 N1 2.0389(16) . ? Cr1 O3 2.0490(14) . ? Cr1 Cl1 2.2916(5) . ? Cr1 Cl2 2.3393(6) . ? O1 C1 1.431(2) . ? O1 Cr1 1.9842(12) 5_656 ? O2 C2 1.339(2) . ? O2 C3 1.463(2) . ? O3 C9 1.437(3) . ? O3 H3O 0.76(3) . ? N1 C2 1.271(2) . ? N1 C4 1.496(2) . ? C1 C2 1.508(3) . ? C1 C6 1.525(3) . ? C1 C5 1.526(3) . ? C3 C4 1.551(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.514(3) . ? C4 C8 1.516(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.468(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 Cr1 O1 77.52(5) . 5_656 ? O1 Cr1 N1 80.11(6) . . ? O1 Cr1 N1 157.55(6) 5_656 . ? O1 Cr1 O3 84.17(6) . . ? O1 Cr1 O3 88.61(6) 5_656 . ? N1 Cr1 O3 87.21(6) . . ? O1 Cr1 Cl1 175.58(4) . . ? O1 Cr1 Cl1 102.08(4) 5_656 . ? N1 Cr1 Cl1 100.07(5) . . ? O3 Cr1 Cl1 91.43(4) . . ? O1 Cr1 Cl2 91.73(4) . . ? O1 Cr1 Cl2 92.32(4) 5_656 . ? N1 Cr1 Cl2 90.26(5) . . ? O3 Cr1 Cl2 175.50(4) . . ? Cl1 Cr1 Cl2 92.68(2) . . ? C1 O1 Cr1 119.52(10) . . ? C1 O1 Cr1 137.96(11) . 5_656 ? Cr1 O1 Cr1 102.48(5) . 5_656 ? C2 O2 C3 105.91(15) . . ? C9 O3 Cr1 131.63(14) . . ? C9 O3 H3O 109(2) . . ? Cr1 O3 H3O 109(2) . . ? C2 N1 C4 109.48(15) . . ? C2 N1 Cr1 112.56(13) . . ? C4 N1 Cr1 137.89(12) . . ? O1 C1 C2 104.20(14) . . ? O1 C1 C6 110.68(17) . . ? C2 C1 C6 109.54(17) . . ? O1 C1 C5 110.62(16) . . ? C2 C1 C5 109.61(17) . . ? C6 C1 C5 111.90(18) . . ? N1 C2 O2 117.81(17) . . ? N1 C2 C1 123.56(17) . . ? O2 C2 C1 118.63(16) . . ? O2 C3 C4 105.86(15) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? N1 C4 C7 109.44(16) . . ? N1 C4 C8 109.75(17) . . ? C7 C4 C8 112.25(18) . . ? N1 C4 C3 100.93(15) . . ? C7 C4 C3 111.96(18) . . ? C8 C4 C3 111.90(18) . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C10 112.7(2) . . ? O3 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? O3 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.417 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.076 data_Complex8 _database_code_depnum_ccdc_archive 'CCDC 690757' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Cl4 Cr2 N2 O6, (C4 H8 O)' _chemical_formula_sum 'C20 H40 Cl4 Cr2 N2 O7' _chemical_formula_weight 666.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3470(4) _cell_length_b 10.8770(4) _cell_length_c 14.7240(7) _cell_angle_alpha 98.425(2) _cell_angle_beta 102.112(3) _cell_angle_gamma 109.096(2) _cell_volume 1488.96(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7164 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12878 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.42 _reflns_number_total 6718 _reflns_number_gt 4481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 version2.0' _computing_publication_material PLATON _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^)+(0.0559P)^2^+0.2512P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6718 _refine_ls_number_parameters 340 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Cr1A Cr 0.44193(5) 0.52590(5) 0.40206(3) 0.02982(14) Uani 1 1 d . . . N1A N 0.5798(3) 0.5965(2) 0.32389(17) 0.0337(6) Uani 1 1 d . . . O1A O 0.61960(19) 0.53364(19) 0.48747(13) 0.0305(5) Uani 1 1 d . . . O2A O 0.8045(2) 0.6504(2) 0.31892(17) 0.0503(6) Uani 1 1 d . . . O3WA O 0.4946(3) 0.7185(2) 0.47301(18) 0.0395(5) Uani 1 1 d D . . Cl1A Cl 0.24017(9) 0.53505(9) 0.30879(6) 0.0500(2) Uani 1 1 d . . . Cl2A Cl 0.38951(9) 0.30524(8) 0.32032(6) 0.0449(2) Uani 1 1 d . . . C1A C 0.7473(3) 0.5717(3) 0.4582(2) 0.0341(7) Uani 1 1 d . . . C2A C 0.7061(3) 0.6079(3) 0.3641(2) 0.0349(7) Uani 1 1 d . . . C3A C 0.7344(4) 0.6748(4) 0.2316(3) 0.0523(10) Uani 1 1 d . . . H3A1 H 0.7433 0.6205 0.1766 0.063 Uiso 1 1 calc R . . H3A2 H 0.7759 0.7683 0.2304 0.063 Uiso 1 1 calc R . . C4A C 0.5762(4) 0.6366(3) 0.2306(2) 0.0406(8) Uani 1 1 d . . . C6A C 0.8632(4) 0.6916(4) 0.5317(3) 0.0536(10) Uani 1 1 d . . . H6A1 H 0.8294 0.7634 0.5414 0.080 Uiso 1 1 calc R . . H6A2 H 0.9461 0.7202 0.5089 0.080 Uiso 1 1 calc R . . H6A3 H 0.8871 0.6665 0.5910 0.080 Uiso 1 1 calc R . . C7A C 0.4790(4) 0.5170(4) 0.1489(2) 0.0627(12) Uani 1 1 d . . . H7A1 H 0.5086 0.4427 0.1535 0.094 Uiso 1 1 calc R . . H7A2 H 0.4846 0.5401 0.0889 0.094 Uiso 1 1 calc R . . H7A3 H 0.3828 0.4930 0.1527 0.094 Uiso 1 1 calc R . . C8A C 0.5287(4) 0.7536(4) 0.2297(3) 0.0578(10) Uani 1 1 d . . . H8A1 H 0.4333 0.7277 0.2353 0.087 Uiso 1 1 calc R . . H8A2 H 0.5318 0.7809 0.1708 0.087 Uiso 1 1 calc R . . H8A3 H 0.5909 0.8266 0.2823 0.087 Uiso 1 1 calc R . . C5A C 0.7956(4) 0.4541(4) 0.4420(3) 0.0505(9) Uani 1 1 d . . . H5A1 H 0.8196 0.4291 0.5013 0.076 Uiso 1 1 calc R . . H5A2 H 0.8775 0.4794 0.4179 0.076 Uiso 1 1 calc R . . H5A3 H 0.7201 0.3797 0.3966 0.076 Uiso 1 1 calc R . . Cr1B Cr 0.93748(5) 0.03933(5) 0.08111(3) 0.02997(14) Uani 1 1 d . . . N1B N 0.8187(3) 0.1559(2) 0.06313(17) 0.0336(6) Uani 1 1 d . . . O1B O 0.9418(2) 0.05989(19) -0.04885(13) 0.0298(5) Uani 1 1 d . . . O2B O 0.7280(3) 0.2581(3) -0.03925(17) 0.0529(6) Uani 1 1 d . . . O3WB O 1.1150(2) 0.2120(2) 0.12691(16) 0.0378(5) Uani 1 1 d D . . Cl1B Cl 0.95238(9) 0.03673(9) 0.23810(6) 0.0460(2) Uani 1 1 d . . . Cl2B Cl 0.73140(8) -0.15546(8) 0.02525(6) 0.0435(2) Uani 1 1 d . . . C1B C 0.8620(3) 0.1298(3) -0.0949(2) 0.0335(7) Uani 1 1 d . . . C2B C 0.8026(3) 0.1817(3) -0.0188(2) 0.0359(7) Uani 1 1 d . . . C3B C 0.6795(4) 0.2870(4) 0.0441(3) 0.0610(11) Uani 1 1 d . . . H3B1 H 0.5767 0.2466 0.0287 0.073 Uiso 1 1 calc R . . H3B2 H 0.7085 0.3828 0.0673 0.073 Uiso 1 1 calc R . . C4B C 0.7490(3) 0.2272(4) 0.1196(2) 0.0439(8) Uani 1 1 d . . . C5B C 0.9594(4) 0.2476(4) -0.1234(3) 0.0523(9) Uani 1 1 d . . . H5B1 H 1.0353 0.3039 -0.0683 0.078 Uiso 1 1 calc R . . H5B2 H 0.9059 0.2981 -0.1488 0.078 Uiso 1 1 calc R . . H5B3 H 0.9985 0.2149 -0.1710 0.078 Uiso 1 1 calc R . . C6B C 0.7400(4) 0.0346(4) -0.1783(2) 0.0471(9) Uani 1 1 d . . . H6B1 H 0.7772 -0.0001 -0.2263 0.071 Uiso 1 1 calc R . . H6B2 H 0.6828 0.0814 -0.2048 0.071 Uiso 1 1 calc R . . H6B3 H 0.6828 -0.0380 -0.1566 0.071 Uiso 1 1 calc R . . C7B C 0.8618(4) 0.3359(4) 0.2009(3) 0.0704(13) Uani 1 1 d . . . H7B1 H 0.9041 0.2958 0.2466 0.106 Uiso 1 1 calc R . . H7B2 H 0.8191 0.3903 0.2312 0.106 Uiso 1 1 calc R . . H7B3 H 0.9337 0.3904 0.1764 0.106 Uiso 1 1 calc R . . C8B C 0.6396(4) 0.1288(5) 0.1540(3) 0.0724(13) Uani 1 1 d . . . H8B1 H 0.5709 0.0615 0.1002 0.109 Uiso 1 1 calc R . . H8B2 H 0.5925 0.1752 0.1873 0.109 Uiso 1 1 calc R . . H8B3 H 0.6860 0.0873 0.1963 0.109 Uiso 1 1 calc R . . H1W H 1.163(4) 0.243(3) 0.1831(15) 0.060(12) Uiso 1 1 d D . . H2W H 1.165(4) 0.213(4) 0.089(2) 0.070(14) Uiso 1 1 d D . . H3W H 0.539(4) 0.734(4) 0.5296(16) 0.074(15) Uiso 1 1 d D . . H4W H 0.420(3) 0.737(4) 0.465(3) 0.068(14) Uiso 1 1 d D . . O4 O 0.3140(4) 0.8417(4) 0.4811(2) 0.0949(11) Uani 1 1 d . . . C9 C 0.2151(8) 0.8481(7) 0.4052(4) 0.136(3) Uani 1 1 d . . . H9A H 0.1394 0.7608 0.3794 0.163 Uiso 1 1 calc R . . H9B H 0.2598 0.8717 0.3552 0.163 Uiso 1 1 calc R . . C10 C 0.1573(6) 0.9427(5) 0.4327(3) 0.0817(14) Uani 1 1 d . . . H10A H 0.0543 0.9025 0.4145 0.098 Uiso 1 1 calc R . . H10B H 0.1855 1.0170 0.4026 0.098 Uiso 1 1 calc R . . C11 C 0.2147(5) 0.9892(4) 0.5387(3) 0.0653(12) Uani 1 1 d . . . H11A H 0.2635 1.0856 0.5573 0.078 Uiso 1 1 calc R . . H11B H 0.1386 0.9642 0.5693 0.078 Uiso 1 1 calc R . . C12 C 0.3145(7) 0.9217(5) 0.5651(3) 0.0996(19) Uani 1 1 d . . . H12A H 0.4094 0.9874 0.5962 0.120 Uiso 1 1 calc R . . H12B H 0.2851 0.8669 0.6089 0.120 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 Cr1A 0.0258(3) 0.0341(3) 0.0264(3) 0.0057(2) 0.00321(19) 0.0100(2) N1A 0.0346(14) 0.0346(14) 0.0305(14) 0.0085(11) 0.0066(11) 0.0120(11) O1A 0.0226(10) 0.0377(11) 0.0291(11) 0.0083(9) 0.0043(8) 0.0101(9) O2A 0.0356(12) 0.0708(16) 0.0500(15) 0.0268(12) 0.0217(11) 0.0152(12) O3WA 0.0414(14) 0.0374(12) 0.0381(15) 0.0070(10) 0.0058(12) 0.0162(11) Cl1A 0.0357(4) 0.0686(6) 0.0433(5) 0.0152(4) -0.0011(4) 0.0227(4) Cl2A 0.0489(5) 0.0380(4) 0.0354(5) -0.0017(3) 0.0014(4) 0.0112(4) C1A 0.0244(15) 0.0420(17) 0.0338(17) 0.0089(14) 0.0073(13) 0.0102(13) C2A 0.0327(17) 0.0339(16) 0.0388(18) 0.0100(14) 0.0123(14) 0.0110(14) C3A 0.051(2) 0.070(2) 0.047(2) 0.0296(18) 0.0219(18) 0.0248(19) C4A 0.0469(19) 0.0464(19) 0.0323(18) 0.0143(14) 0.0138(15) 0.0179(16) C6A 0.0329(18) 0.060(2) 0.048(2) 0.0095(17) -0.0014(16) 0.0008(17) C7A 0.072(3) 0.066(2) 0.035(2) 0.0041(18) 0.0126(19) 0.011(2) C8A 0.069(3) 0.061(2) 0.056(2) 0.0291(19) 0.017(2) 0.034(2) C5A 0.049(2) 0.071(2) 0.054(2) 0.0279(19) 0.0236(18) 0.0392(19) Cr1B 0.0241(2) 0.0404(3) 0.0240(3) 0.0060(2) 0.00604(19) 0.0112(2) N1B 0.0279(13) 0.0446(15) 0.0290(14) 0.0042(11) 0.0085(11) 0.0155(12) O1B 0.0271(10) 0.0406(11) 0.0262(11) 0.0086(9) 0.0092(8) 0.0167(9) O2B 0.0579(15) 0.0770(17) 0.0417(14) 0.0157(12) 0.0146(12) 0.0464(14) O3WB 0.0319(12) 0.0451(13) 0.0285(13) 0.0005(10) 0.0057(10) 0.0094(10) Cl1B 0.0486(5) 0.0635(5) 0.0281(4) 0.0122(4) 0.0126(4) 0.0215(4) Cl2B 0.0290(4) 0.0499(5) 0.0439(5) 0.0074(4) 0.0116(3) 0.0053(4) C1B 0.0330(16) 0.0466(18) 0.0280(16) 0.0148(13) 0.0098(13) 0.0203(14) C2B 0.0285(16) 0.0421(18) 0.0380(19) 0.0089(14) 0.0064(13) 0.0163(14) C3B 0.063(2) 0.090(3) 0.048(2) 0.009(2) 0.0167(19) 0.053(2) C4B 0.0371(18) 0.060(2) 0.0390(19) 0.0020(16) 0.0119(15) 0.0268(17) C5B 0.053(2) 0.056(2) 0.060(2) 0.0279(18) 0.0238(19) 0.0250(18) C6B 0.0422(19) 0.067(2) 0.0308(18) 0.0050(16) 0.0009(15) 0.0274(17) C7B 0.068(3) 0.074(3) 0.058(3) -0.017(2) 0.001(2) 0.036(2) C8B 0.056(2) 0.100(3) 0.081(3) 0.027(3) 0.042(2) 0.038(2) O4 0.131(3) 0.120(3) 0.060(2) 0.0101(19) 0.0062(19) 0.098(2) C9 0.227(8) 0.194(7) 0.050(3) 0.021(4) 0.010(4) 0.179(6) C10 0.087(3) 0.081(3) 0.076(3) 0.012(3) 0.006(3) 0.043(3) C11 0.064(3) 0.065(3) 0.067(3) 0.008(2) 0.020(2) 0.027(2) C12 0.159(5) 0.091(4) 0.054(3) -0.001(2) -0.003(3) 0.080(4) _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 Cr1A O1A 1.966(2) . ? Cr1A O1A 1.9859(19) 2_666 ? Cr1A O3WA 2.037(2) . ? Cr1A N1A 2.044(2) . ? Cr1A Cl1A 2.2862(10) . ? Cr1A Cl2A 2.3519(9) . ? N1A C2A 1.273(4) . ? N1A C4A 1.498(4) . ? O1A C1A 1.427(3) . ? O1A Cr1A 1.9859(19) 2_666 ? O2A C2A 1.326(4) . ? O2A C3A 1.444(4) . ? O3WA H3W 0.826(19) . ? O3WA H4W 0.846(19) . ? C1A C2A 1.510(4) . ? C1A C5A 1.524(5) . ? C1A C6A 1.525(4) . ? C3A C4A 1.547(5) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A C8A 1.507(5) . ? C4A C7A 1.526(5) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8A H8A3 0.9600 . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C5A H5A3 0.9600 . ? Cr1B O1B 1.9669(19) . ? Cr1B O1B 1.983(2) 2_755 ? Cr1B N1B 2.042(3) . ? Cr1B O3WB 2.051(2) . ? Cr1B Cl1B 2.2890(9) . ? Cr1B Cl2B 2.3473(8) . ? N1B C2B 1.267(4) . ? N1B C4B 1.496(4) . ? O1B C1B 1.430(4) . ? O1B Cr1B 1.983(2) 2_755 ? O2B C2B 1.332(4) . ? O2B C3B 1.451(4) . ? O3WB H1W 0.825(18) . ? O3WB H2W 0.840(19) . ? C1B C2B 1.511(4) . ? C1B C6B 1.515(4) . ? C1B C5B 1.524(4) . ? C3B C4B 1.536(5) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B C7B 1.513(5) . ? C4B C8B 1.514(5) . ? C5B H5B1 0.9600 . ? C5B H5B2 0.9600 . ? C5B H5B3 0.9600 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B H8B1 0.9600 . ? C8B H8B2 0.9600 . ? C8B H8B3 0.9600 . ? O4 C9 1.376(6) . ? O4 C12 1.402(5) . ? C9 C10 1.401(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.492(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.472(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 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 O1A Cr1A O1A 77.16(9) . 2_666 ? O1A Cr1A O3WA 86.11(10) . . ? O1A Cr1A O3WA 88.58(9) 2_666 . ? O1A Cr1A N1A 80.28(9) . . ? O1A Cr1A N1A 157.39(10) 2_666 . ? O3WA Cr1A N1A 88.30(10) . . ? O1A Cr1A Cl1A 175.25(7) . . ? O1A Cr1A Cl1A 102.92(6) 2_666 . ? O3WA Cr1A Cl1A 89.14(8) . . ? N1A Cr1A Cl1A 99.42(8) . . ? O1A Cr1A Cl2A 92.35(6) . . ? O1A Cr1A Cl2A 92.34(6) 2_666 . ? O3WA Cr1A Cl2A 177.99(8) . . ? N1A Cr1A Cl2A 90.17(7) . . ? Cl1A Cr1A Cl2A 92.39(4) . . ? C2A N1A C4A 109.1(3) . . ? C2A N1A Cr1A 112.2(2) . . ? C4A N1A Cr1A 138.7(2) . . ? C1A O1A Cr1A 119.56(17) . . ? C1A O1A Cr1A 137.57(18) . 2_666 ? Cr1A O1A Cr1A 102.84(9) . 2_666 ? C2A O2A C3A 106.6(3) . . ? Cr1A O3WA H3W 112(3) . . ? Cr1A O3WA H4W 109(3) . . ? H3W O3WA H4W 114(4) . . ? O1A C1A C2A 104.5(2) . . ? O1A C1A C5A 110.5(2) . . ? C2A C1A C5A 109.0(3) . . ? O1A C1A C6A 110.4(3) . . ? C2A C1A C6A 110.9(3) . . ? C5A C1A C6A 111.3(3) . . ? N1A C2A O2A 117.7(3) . . ? N1A C2A C1A 123.3(3) . . ? O2A C2A C1A 119.0(3) . . ? O2A C3A C4A 106.1(3) . . ? O2A C3A H3A1 110.5 . . ? C4A C3A H3A1 110.5 . . ? O2A C3A H3A2 110.5 . . ? C4A C3A H3A2 110.5 . . ? H3A1 C3A H3A2 108.7 . . ? N1A C4A C8A 110.6(3) . . ? N1A C4A C7A 109.6(3) . . ? C8A C4A C7A 111.4(3) . . ? N1A C4A C3A 100.6(3) . . ? C8A C4A C3A 112.3(3) . . ? C7A C4A C3A 111.8(3) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C4A C7A H7A1 109.5 . . ? C4A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4A C8A H8A1 109.5 . . ? C4A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C4A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C1A C5A H5A1 109.5 . . ? C1A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C1A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? O1B Cr1B O1B 77.16(9) . 2_755 ? O1B Cr1B N1B 80.25(9) . . ? O1B Cr1B N1B 157.35(9) 2_755 . ? O1B Cr1B O3WB 85.94(9) . . ? O1B Cr1B O3WB 88.99(9) 2_755 . ? N1B Cr1B O3WB 87.78(10) . . ? O1B Cr1B Cl1B 173.91(6) . . ? O1B Cr1B Cl1B 103.19(6) 2_755 . ? N1B Cr1B Cl1B 99.09(8) . . ? O3WB Cr1B Cl1B 87.98(7) . . ? O1B Cr1B Cl2B 92.77(6) . . ? O1B Cr1B Cl2B 91.82(6) 2_755 . ? N1B Cr1B Cl2B 90.90(7) . . ? O3WB Cr1B Cl2B 178.30(8) . . ? Cl1B Cr1B Cl2B 93.29(3) . . ? C2B N1B C4B 108.7(3) . . ? C2B N1B Cr1B 112.1(2) . . ? C4B N1B Cr1B 139.1(2) . . ? C1B O1B Cr1B 119.61(17) . . ? C1B O1B Cr1B 137.49(17) . 2_755 ? Cr1B O1B Cr1B 102.84(9) . 2_755 ? C2B O2B C3B 105.8(3) . . ? Cr1B O3WB H1W 124(3) . . ? Cr1B O3WB H2W 109(3) . . ? H1W O3WB H2W 113(4) . . ? O1B C1B C2B 103.9(2) . . ? O1B C1B C6B 110.6(3) . . ? C2B C1B C6B 109.1(3) . . ? O1B C1B C5B 110.6(3) . . ? C2B C1B C5B 109.3(3) . . ? C6B C1B C5B 112.9(3) . . ? N1B C2B O2B 118.1(3) . . ? N1B C2B C1B 123.9(3) . . ? O2B C2B C1B 118.1(3) . . ? O2B C3B C4B 106.0(3) . . ? O2B C3B H3B1 110.5 . . ? C4B C3B H3B1 110.5 . . ? O2B C3B H3B2 110.5 . . ? C4B C3B H3B2 110.5 . . ? H3B1 C3B H3B2 108.7 . . ? N1B C4B C7B 109.4(3) . . ? N1B C4B C8B 110.4(3) . . ? C7B C4B C8B 112.4(3) . . ? N1B C4B C3B 101.0(3) . . ? C7B C4B C3B 111.2(3) . . ? C8B C4B C3B 111.9(3) . . ? C1B C5B H5B1 109.5 . . ? C1B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C1B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C4B C7B H7B1 109.5 . . ? C4B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C4B C8B H8B1 109.5 . . ? C4B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C4B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C9 O4 C12 109.3(4) . . ? O4 C9 C10 111.3(4) . . ? O4 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? O4 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 106.0(4) . . ? C9 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? C9 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 105.1(4) . . ? C12 C11 H11A 110.7 . . ? C10 C11 H11A 110.7 . . ? C12 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? O4 C12 C11 107.8(4) . . ? O4 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O4 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.385 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.080