# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1249 data_1 _audit_creation_method SHELXL-97 _publ_contact_author_name ' Colin L. Raston' _publ_contact_author_email ' c.raston@sci.monash.edu.au ' _publ_contact_author_fax ' 61 - 3 - 9905 4597 ' loop_ _publ_author_name _publ_author_address ' Alexander Drljaca ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Michaele J. Hardie ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Samantha Airey ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Colin L. Raston' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; _publ_requested_journal ' Chemical Communications' _chemical_name_systematic ; 1,4,8,11-tetraazacyclotetradecane ; _chemical_name_common cyclam _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 N4' _chemical_formula_weight 200.33 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' _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 4.6353(2) _cell_length_b 8.5958(6) _cell_length_c 15.2418(10) _cell_angle_alpha 90.704(3) _cell_angle_beta 96.743(3) _cell_angle_gamma 99.336(4) _cell_volume 594.80(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 mm _exptl_crystal_size_mid 0.18 mm _exptl_crystal_size_min 0.13 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 224 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4366 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 30.07 _reflns_number_total 2989 _reflns_number_gt 2198 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+0.2014P] 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 refal _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2989 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9301(3) 0.22984(17) 0.12773(9) 0.0224(3) Uani 1 d . . . H1A H 0.771(3) 0.2461(17) 0.1655(10) 0.022(4) Uiso 1 d . . . H1A H 1.077(3) 0.3281(19) 0.1352(10) 0.025(4) Uiso 1 d . . . C2 C -0.0723(3) -0.09206(18) -0.16377(9) 0.0243(3) Uani 1 d . . . H2B H -0.218(4) -0.0719(18) -0.1250(10) 0.025(4) Uiso 1 d . . . H2A H -0.179(3) -0.1244(18) -0.2232(11) 0.029(4) Uiso 1 d . . . C3 C 0.1427(3) 0.05853(17) -0.17311(9) 0.0228(3) Uani 1 d . . . H3B H 0.297(3) 0.0339(17) -0.2098(10) 0.025(4) Uiso 1 d . . . H3A H 0.036(4) 0.1361(19) -0.2078(10) 0.027(4) Uiso 1 d . . . C4 C 0.4889(3) 0.27126(16) -0.09166(9) 0.0226(3) Uani 1 d . . . H4B H 0.638(3) 0.2528(17) -0.1308(10) 0.023(4) Uiso 1 d . . . H4A H 0.392(4) 0.3598(19) -0.1177(11) 0.032(4) Uiso 1 d . . . C5 C 0.6412(3) 0.32170(16) 0.00012(9) 0.0211(3) Uani 1 d . . . H5A H 0.770(3) 0.4249(19) -0.0001(10) 0.028(4) Uiso 1 d . . . H5B H 0.488(3) 0.3385(17) 0.0404(10) 0.022(4) Uiso 1 d . . . C6 C 0.6909(3) 0.25339(16) 0.38440(9) 0.0205(3) Uani 1 d . . . H6A H 0.776(3) 0.2311(17) 0.3300(10) 0.022(4) Uiso 1 d . . . H6B H 0.489(4) 0.1842(18) 0.3802(10) 0.025(4) Uiso 1 d . . . C7 C 0.1193(3) 0.79579(16) 0.53540(9) 0.0209(3) Uani 1 d . . . H7A H -0.070(4) 0.7248(18) 0.5268(10) 0.025(4) Uiso 1 d . . . H7B H 0.081(3) 0.9002(19) 0.5484(10) 0.025(4) Uiso 1 d . . . C8 C 0.2578(3) 0.79867(15) 0.44949(9) 0.0202(3) Uani 1 d . . . H8A H 0.455(3) 0.8633(17) 0.4586(10) 0.021(4) Uiso 1 d . . . H8B H 0.137(3) 0.8530(17) 0.4033(10) 0.023(4) Uiso 1 d . . . C9 C 0.4219(3) 0.63724(16) 0.33821(9) 0.0215(3) Uani 1 d . . . H9B H 0.618(4) 0.7111(18) 0.3465(10) 0.028(4) Uiso 1 d . . . H9A H 0.298(4) 0.6756(18) 0.2874(11) 0.029(4) Uiso 1 d . . . C10 C 0.4713(3) 0.47078(16) 0.31817(9) 0.0209(3) Uani 1 d . . . H10A H 0.273(3) 0.3989(18) 0.3111(10) 0.023(4) Uiso 1 d . . . H10B H 0.549(3) 0.4639(18) 0.2621(11) 0.026(4) Uiso 1 d . . . N1 N 0.8174(2) 0.20457(14) 0.03412(7) 0.0187(3) Uani 1 d . . . H1C H 0.707(3) 0.1112(18) 0.0280(10) 0.020(4) Uiso 1 d . . . N2 N 0.2839(3) 0.12496(13) -0.08712(7) 0.0183(2) Uani 1 d . . . H2C H 0.146(4) 0.1460(18) -0.0545(11) 0.026(4) Uiso 1 d . . . N3 N 0.6738(2) 0.42127(13) 0.38899(7) 0.0178(2) Uani 1 d . . . H3C H 0.615(3) 0.4415(18) 0.4390(11) 0.025(4) Uiso 1 d . . . N4 N 0.2908(3) 0.64070(13) 0.42053(7) 0.0175(2) Uani 1 d . . . H4C H 0.117(4) 0.5814(19) 0.4133(10) 0.026(4) Uiso 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 C1 0.0202(7) 0.0254(7) 0.0204(7) -0.0064(5) 0.0006(5) 0.0017(6) C2 0.0200(7) 0.0343(8) 0.0174(7) -0.0066(6) -0.0043(5) 0.0064(6) C3 0.0240(8) 0.0310(8) 0.0149(7) 0.0009(5) -0.0007(5) 0.0108(6) C4 0.0253(8) 0.0213(7) 0.0229(7) 0.0064(5) 0.0063(6) 0.0060(6) C5 0.0211(7) 0.0153(6) 0.0272(7) 0.0011(5) 0.0055(6) 0.0014(5) C6 0.0243(8) 0.0173(6) 0.0204(7) -0.0034(5) 0.0036(5) 0.0051(6) C7 0.0240(8) 0.0150(6) 0.0253(7) -0.0008(5) 0.0028(5) 0.0079(6) C8 0.0221(7) 0.0152(6) 0.0237(7) 0.0022(5) 0.0018(5) 0.0047(5) C9 0.0262(8) 0.0239(7) 0.0164(7) 0.0065(5) 0.0036(5) 0.0085(6) C10 0.0263(8) 0.0252(7) 0.0122(6) 0.0001(5) 0.0017(5) 0.0073(6) N1 0.0192(6) 0.0185(6) 0.0180(6) -0.0021(4) 0.0018(4) 0.0024(5) N2 0.0187(6) 0.0215(6) 0.0151(5) 0.0006(4) 0.0025(4) 0.0048(5) N3 0.0214(6) 0.0177(5) 0.0151(6) -0.0007(4) 0.0018(4) 0.0061(4) N4 0.0209(6) 0.0146(5) 0.0175(6) 0.0017(4) 0.0039(4) 0.0030(5) _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 C1 N1 1.4617(17) . ? C1 C2 1.524(2) 2_655 ? C1 H1A 1.013(15) . ? C1 H1A 0.990(16) . ? C2 C3 1.519(2) . ? C2 C1 1.524(2) 2_655 ? C2 H2B 0.981(16) . ? C2 H2A 0.993(16) . ? C3 N2 1.4598(17) . ? C3 H3B 1.006(16) . ? C3 H3A 1.011(16) . ? C4 N2 1.4558(17) . ? C4 C5 1.516(2) . ? C4 H4B 0.996(16) . ? C4 H4A 1.008(17) . ? C5 N1 1.4592(17) . ? C5 H5A 0.986(16) . ? C5 H5B 1.017(15) . ? C6 N3 1.4592(17) . ? C6 C7 1.5257(19) 2_666 ? C6 H6A 0.988(15) . ? C6 H6B 1.020(16) . ? C7 C8 1.523(2) . ? C7 C6 1.5257(19) 2_666 ? C7 H7A 0.978(16) . ? C7 H7B 0.965(15) . ? C8 N4 1.4596(17) . ? C8 H8A 0.982(16) . ? C8 H8B 1.014(15) . ? C9 N4 1.4591(17) . ? C9 C10 1.5181(19) . ? C9 H9B 1.015(16) . ? C9 H9A 1.000(16) . ? C10 N3 1.4597(17) . ? C10 H10A 1.014(15) . ? C10 H10B 0.971(16) . ? N1 H1C 0.876(16) . ? N2 H2C 0.892(17) . ? N3 H3C 0.864(16) . ? N4 H4C 0.876(17) . ? 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 N1 C1 C2 111.69(11) . 2_655 ? N1 C1 H1A 112.4(8) . . ? C2 C1 H1A 108.2(8) 2_655 . ? N1 C1 H1A 108.9(9) . . ? C2 C1 H1A 109.6(9) 2_655 . ? H1A C1 H1A 105.9(12) . . ? C3 C2 C1 114.65(12) . 2_655 ? C3 C2 H2B 109.9(9) . . ? C1 C2 H2B 108.2(9) 2_655 . ? C3 C2 H2A 107.9(9) . . ? C1 C2 H2A 108.0(9) 2_655 . ? H2B C2 H2A 107.9(12) . . ? N2 C3 C2 111.49(11) . . ? N2 C3 H3B 109.4(9) . . ? C2 C3 H3B 108.7(9) . . ? N2 C3 H3A 111.9(9) . . ? C2 C3 H3A 109.2(9) . . ? H3B C3 H3A 105.9(12) . . ? N2 C4 C5 109.51(11) . . ? N2 C4 H4B 108.7(9) . . ? C5 C4 H4B 109.5(9) . . ? N2 C4 H4A 113.2(9) . . ? C5 C4 H4A 109.2(9) . . ? H4B C4 H4A 106.7(13) . . ? N1 C5 C4 110.10(11) . . ? N1 C5 H5A 109.0(9) . . ? C4 C5 H5A 111.4(9) . . ? N1 C5 H5B 111.7(8) . . ? C4 C5 H5B 109.5(8) . . ? H5A C5 H5B 105.0(12) . . ? N3 C6 C7 111.68(11) . 2_666 ? N3 C6 H6A 108.4(9) . . ? C7 C6 H6A 109.5(9) 2_666 . ? N3 C6 H6B 112.4(9) . . ? C7 C6 H6B 108.0(9) 2_666 . ? H6A C6 H6B 106.6(12) . . ? C8 C7 C6 114.67(12) . 2_666 ? C8 C7 H7A 108.5(9) . . ? C6 C7 H7A 109.6(9) 2_666 . ? C8 C7 H7B 108.7(9) . . ? C6 C7 H7B 107.4(9) 2_666 . ? H7A C7 H7B 107.8(13) . . ? N4 C8 C7 111.59(11) . . ? N4 C8 H8A 107.9(9) . . ? C7 C8 H8A 109.3(9) . . ? N4 C8 H8B 112.7(8) . . ? C7 C8 H8B 108.9(9) . . ? H8A C8 H8B 106.3(12) . . ? N4 C9 C10 109.53(11) . . ? N4 C9 H9B 107.7(9) . . ? C10 C9 H9B 109.7(9) . . ? N4 C9 H9A 112.4(9) . . ? C10 C9 H9A 110.1(9) . . ? H9B C9 H9A 107.3(13) . . ? N3 C10 C9 109.78(11) . . ? N3 C10 H10A 111.8(9) . . ? C9 C10 H10A 108.3(9) . . ? N3 C10 H10B 109.7(9) . . ? C9 C10 H10B 111.3(9) . . ? H10A C10 H10B 106.0(12) . . ? C5 N1 C1 113.53(11) . . ? C5 N1 H1C 108.7(10) . . ? C1 N1 H1C 107.4(10) . . ? C4 N2 C3 114.08(11) . . ? C4 N2 H2C 107.0(10) . . ? C3 N2 H2C 109.3(10) . . ? C6 N3 C10 113.65(11) . . ? C6 N3 H3C 107.9(10) . . ? C10 N3 H3C 108.5(10) . . ? C9 N4 C8 113.66(10) . . ? C9 N4 H4C 108.7(10) . . ? C8 N4 H4C 108.6(10) . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 0.250 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.044 _END _audit_creation_method SHELXL-97 _publ_contact_author_name ' Colin L. Raston' _publ_contact_author_email ' c.raston@sci.monash.edu.au ' _publ_contact_author_fax ' 61 - 3 - 9905 4597 ' loop_ _publ_author_name _publ_author_address ' Alexander Drljaca ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Michaele J. Hardie ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Samantha Airey ' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ' Colin L. Raston' ; Department of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; _publ_requested_journal ' Chemical Communications' _chemical_name_systematic ; ? ; _chemical_name_common ; [Cr2(OH)2(H2O)8][H4(1,4,8,11-tetraazacyclodecane)][{(p- sulfonatocalix[4]arene)2}].6(H2O) ; _chemical_formula_moiety ? _chemical_formula_sum 'C33 H77 Cr N2 O27 S4' _chemical_formula_weight 1114.21 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' 'S' 'S' 0.1246 0.1234 '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' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9916(3) _cell_length_b 14.8774(5) _cell_length_c 15.3517(6) _cell_angle_alpha 63.836(1) _cell_angle_beta 86.583(2) _cell_angle_gamma 80.499(2) _cell_volume 2222.03(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'pale green ' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1186 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37347 _diffrn_reflns_av_R_equivalents 0.146 _diffrn_reflns_av_sigmaI/netI 0.1400 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.22 _reflns_number_total 9727 _reflns_number_gt 5814 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9727 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2347 _refine_ls_R_factor_gt 0.1644 _refine_ls_wR_factor_ref 0.4139 _refine_ls_wR_factor_gt 0.3927 _refine_ls_goodness_of_fit_ref 2.277 _refine_ls_restrained_S_all 2.277 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.1260(2) -0.00143(16) 0.03210(15) 0.0363(6) Uani 1 d . . . N1 N 0.2600(8) 0.0932(7) 0.4754(7) 0.018(2) Uani 1 d . . . N2 N 0.3899(8) -0.0780(7) 0.6716(7) 0.021(2) Uani 1 d . . . S1 S -0.4468(3) 0.2008(2) -0.9449(3) 0.0281(8) Uani 1 d . . . S2 S -1.0543(3) 0.1621(2) -0.7450(2) 0.0217(7) Uani 1 d . . . S3 S -0.9340(3) 0.2313(2) -0.2944(2) 0.0214(7) Uani 1 d . . . S4 S -0.3251(2) 0.1801(2) -0.4734(2) 0.0175(6) Uani 1 d . . . C1 C 0.5267(10) -0.0783(9) 0.6566(10) 0.027(3) Uani 1 d . . . H1A H 0.5609 -0.0648 0.7056 0.032 Uiso 1 calc R . . H1B H 0.5406 -0.0245 0.5936 0.032 Uiso 1 calc R . . C2 C 0.4068(9) 0.1790(9) 0.3377(8) 0.022(3) Uani 1 d . . . H2A H 0.4054 0.2303 0.2710 0.027 Uiso 1 calc R . . H2B H 0.4517 0.1998 0.3765 0.027 Uiso 1 calc R . . C3 C 0.2736(10) 0.1714(9) 0.3744(8) 0.023(3) Uani 1 d . . . H3A H 0.2360 0.2370 0.3702 0.028 Uiso 1 calc R . . H3B H 0.2277 0.1574 0.3310 0.028 Uiso 1 calc R . . C4 C 0.3274(11) 0.1085(9) 0.5484(9) 0.027(3) Uani 1 d . . . H4A H 0.2936 0.1737 0.5468 0.032 Uiso 1 calc R . . H4B H 0.4136 0.1097 0.5308 0.032 Uiso 1 calc R . . C5 C 0.3185(10) 0.0262(9) 0.6505(9) 0.025(3) Uani 1 d . . . H5A H 0.2322 0.0197 0.6639 0.030 Uiso 1 calc R . . H5B H 0.3472 0.0482 0.6954 0.030 Uiso 1 calc R . . C6 C -0.6241(9) 0.4696(8) -0.8931(8) 0.017(2) Uani 1 d . . . C7 C -0.5002(9) 0.4309(8) -0.8670(7) 0.013(2) Uani 1 d . . . C8 C -0.4471(10) 0.3474(8) -0.8835(8) 0.019(2) Uani 1 d . . . H8 H -0.3644 0.3209 -0.8677 0.022 Uiso 1 calc R . . C9 C -0.5155(9) 0.3037(8) -0.9227(8) 0.018(2) Uani 1 d . . . C10 C -0.6384(9) 0.3459(8) -0.9510(7) 0.015(2) Uani 1 d . . . H10 H -0.6832 0.3182 -0.9800 0.018 Uiso 1 calc R . . C11 C -0.6942(9) 0.4288(8) -0.9361(8) 0.013(2) Uani 1 d . . . C12 C -0.8289(9) 0.4687(8) -0.9608(8) 0.015(2) Uani 1 d . . . H12A H -0.8519 0.4535 -1.0124 0.018 Uiso 1 calc R . . H12B H -0.8421 0.5418 -0.9848 0.018 Uiso 1 calc R . . C13 C -0.9563(9) 0.4691(8) -0.8134(8) 0.015(2) Uani 1 d . . . C14 C -0.9113(9) 0.4236(8) -0.8747(8) 0.016(2) Uani 1 d . . . C15 C -0.9430(8) 0.3292(8) -0.8524(8) 0.016(2) Uani 1 d . . . H15 H -0.9153 0.2976 -0.8920 0.019 Uiso 1 calc R . . C16 C -1.0139(9) 0.2809(8) -0.7738(8) 0.016(2) Uani 1 d . . . C17 C -1.0500(9) 0.3247(8) -0.7095(8) 0.015(2) Uani 1 d . . . H17 H -1.0923 0.2901 -0.6533 0.017 Uiso 1 calc R . . C18 C -1.0221(9) 0.4190(8) -0.7306(8) 0.016(2) Uani 1 d . . . C19 C -1.0619(9) 0.4652(8) -0.6602(8) 0.017(2) Uani 1 d . . . H19A H -1.0717 0.5385 -0.6953 0.020 Uiso 1 calc R . . H19B H -1.1412 0.4468 -0.6335 0.020 Uiso 1 calc R . . C20 C -0.8640(9) 0.4740(8) -0.5892(8) 0.013(2) Uani 1 d . . . C21 C -0.9687(9) 0.4294(8) -0.5775(8) 0.014(2) Uani 1 d . . . C22 C -0.9879(9) 0.3537(8) -0.4884(8) 0.018(2) Uani 1 d . . . H22 H -1.0576 0.3228 -0.4796 0.022 Uiso 1 calc R . . C23 C -0.9082(9) 0.3219(8) -0.4120(8) 0.014(2) Uani 1 d . . . C24 C -0.8030(9) 0.3668(8) -0.4242(9) 0.017(2) Uani 1 d . . . H24 H -0.7480 0.3448 -0.3726 0.020 Uiso 1 calc R . . C25 C -0.7804(9) 0.4429(8) -0.5118(7) 0.011(2) Uani 1 d . . . C26 C -0.6639(9) 0.4925(8) -0.5300(8) 0.017(2) Uani 1 d . . . H26A H -0.6834 0.5640 -0.5738 0.021 Uiso 1 calc R . . H26B H -0.6340 0.4866 -0.4692 0.021 Uiso 1 calc R . . C27 C -0.5341(9) 0.4854(8) -0.6708(8) 0.017(2) Uani 1 d . . . C28 C -0.5648(9) 0.4422(8) -0.5733(8) 0.017(2) Uani 1 d . . . C29 C -0.5010(9) 0.3474(8) -0.5134(8) 0.015(2) Uani 1 d . . . H29 H -0.5188 0.3172 -0.4476 0.018 Uiso 1 calc R . . C30 C -0.4114(9) 0.2978(8) -0.5505(8) 0.014(2) Uani 1 d . . . C31 C -0.3854(9) 0.3395(8) -0.6479(8) 0.014(2) Uani 1 d . . . H31 H -0.3254 0.3046 -0.6718 0.017 Uiso 1 calc R . . C32 C -0.4483(9) 0.4343(8) -0.7115(8) 0.015(2) Uani 1 d . . . C33 C -0.4244(9) 0.4746(8) -0.8203(8) 0.017(2) Uani 1 d . . . H33A H -0.4450 0.5479 -0.8509 0.020 Uiso 1 calc R . . H33B H -0.3375 0.4571 -0.8305 0.020 Uiso 1 calc R . . O1 O -0.0195(8) 0.0945(6) -0.0399(6) 0.036(2) Uani 1 d . . . O2 O 0.0726(11) -0.0116(7) 0.1622(7) 0.058(3) Uani 1 d . . . O3 O 0.2175(9) 0.1067(8) 0.0253(8) 0.056(3) Uani 1 d . . . O4 O 0.2668(9) -0.1094(7) 0.1031(7) 0.045(3) Uani 1 d . . . O5 O 0.2065(8) 0.0040(7) -0.0901(6) 0.045(3) Uani 1 d . . . O6 O -0.6854(6) 0.5489(6) -0.8775(6) 0.0190(17) Uani 1 d . . . O7 O -0.9455(7) 0.5676(5) -0.8360(5) 0.0198(17) Uani 1 d . . . O8 O -0.8352(6) 0.5512(6) -0.6736(5) 0.0202(18) Uani 1 d . . . O9 O -0.5880(7) 0.5814(5) -0.7367(6) 0.0207(18) Uani 1 d . . . O10 O -0.3486(7) 0.1466(6) -0.8723(6) 0.029(2) Uani 1 d . . . O11 O -0.3956(11) 0.2423(8) -1.0413(7) 0.058(3) Uani 1 d . . . O12 O -0.5394(8) 0.1401(8) -0.9343(10) 0.064(4) Uani 1 d . . . O13 O -1.1751(7) 0.1602(7) -0.7033(7) 0.037(2) Uani 1 d . . . O14 O -1.0515(8) 0.1534(6) -0.8356(6) 0.034(2) Uani 1 d . . . O15 O -0.9612(8) 0.0852(6) -0.6782(6) 0.033(2) Uani 1 d . . . O16 O -0.9625(7) 0.2853(6) -0.2347(6) 0.0273(19) Uani 1 d . . . O17 O -1.0352(8) 0.1856(7) -0.3047(6) 0.036(2) Uani 1 d . . . O18 O -0.8193(7) 0.1591(6) -0.2621(6) 0.034(2) Uani 1 d . . . O19 O -0.3730(7) 0.1530(6) -0.3772(6) 0.028(2) Uani 1 d . . . O20 O -0.1985(6) 0.1977(6) -0.4837(6) 0.028(2) Uani 1 d . . . O21 O -0.3488(7) 0.1078(6) -0.5099(5) 0.0192(17) Uani 1 d . . . O22 O 0.4853(15) 0.0801(15) 0.7983(16) 0.046(5) Uani 0.50 d P . . O23 O 0.2668(17) 0.0506(16) 0.2224(13) 0.045(5) Uani 0.50 d P . . O24 O 0.7212(8) 0.2499(7) 0.7173(6) 0.035(2) Uani 1 d . . . O25 O 0.8645(8) 0.2690(7) 0.9794(7) 0.040(2) Uani 1 d . . . O26 O 0.2118(9) 0.2866(8) 0.8915(8) 0.052(3) Uani 1 d . . . O27 O 0.4078(10) 0.2807(9) 0.7705(9) 0.062(3) Uani 1 d . . . O28 O 0.0342(7) 0.0872(7) 0.5384(7) 0.036(2) Uani 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 0.0518(14) 0.0241(12) 0.0200(13) -0.0039(10) 0.0043(10) 0.0107(10) N1 0.016(5) 0.019(5) 0.020(5) -0.009(4) -0.001(4) 0.002(4) N2 0.010(4) 0.023(5) 0.022(6) -0.007(5) 0.005(4) 0.005(4) S1 0.0262(16) 0.0282(18) 0.037(2) -0.0238(16) -0.0020(14) 0.0045(13) S2 0.0207(14) 0.0219(16) 0.0284(18) -0.0163(14) 0.0031(12) -0.0042(12) S3 0.0248(15) 0.0201(16) 0.0140(16) -0.0041(13) 0.0029(12) -0.0004(12) S4 0.0165(13) 0.0172(15) 0.0183(16) -0.0081(13) -0.0018(11) 0.0008(11) C1 0.017(6) 0.024(7) 0.048(9) -0.019(6) 0.009(5) -0.018(5) C2 0.019(6) 0.024(7) 0.015(6) -0.006(5) -0.001(5) 0.011(5) C3 0.020(6) 0.023(7) 0.020(7) -0.004(5) 0.004(5) -0.007(5) C4 0.028(6) 0.022(7) 0.035(8) -0.016(6) 0.004(6) -0.008(5) C5 0.020(6) 0.034(7) 0.031(8) -0.023(6) 0.000(5) -0.010(5) C6 0.016(5) 0.018(6) 0.012(6) -0.004(5) 0.005(4) -0.002(5) C7 0.013(5) 0.017(6) 0.007(5) -0.003(5) 0.005(4) -0.004(4) C8 0.015(5) 0.022(6) 0.014(6) -0.006(5) 0.004(4) 0.004(5) C9 0.020(6) 0.017(6) 0.012(6) -0.008(5) 0.001(4) 0.009(5) C10 0.017(5) 0.020(6) 0.005(6) -0.003(5) 0.006(4) -0.008(5) C11 0.011(5) 0.016(6) 0.015(6) -0.011(5) 0.005(4) -0.004(4) C12 0.018(5) 0.017(6) 0.008(6) -0.005(5) 0.003(4) -0.001(5) C13 0.013(5) 0.019(6) 0.011(6) -0.004(5) -0.001(4) 0.000(4) C14 0.013(5) 0.020(6) 0.014(6) -0.008(5) 0.000(4) 0.001(4) C15 0.005(5) 0.026(6) 0.025(7) -0.021(6) 0.000(4) 0.005(4) C16 0.015(5) 0.019(6) 0.014(6) -0.008(5) -0.003(4) 0.002(5) C17 0.014(5) 0.021(6) 0.007(6) -0.005(5) 0.006(4) -0.003(5) C18 0.013(5) 0.023(6) 0.014(6) -0.014(5) -0.001(4) 0.007(5) C19 0.017(5) 0.019(6) 0.011(6) -0.005(5) -0.002(4) 0.004(5) C20 0.015(5) 0.011(5) 0.014(6) -0.007(5) 0.009(4) -0.005(4) C21 0.016(5) 0.017(6) 0.013(6) -0.010(5) 0.006(4) -0.002(4) C22 0.015(5) 0.024(6) 0.020(7) -0.015(6) 0.002(5) 0.002(5) C23 0.014(5) 0.012(5) 0.013(6) -0.004(5) 0.004(4) -0.001(4) C24 0.012(5) 0.016(6) 0.025(7) -0.011(5) -0.004(4) 0.003(4) C25 0.019(5) 0.008(5) 0.007(6) -0.004(4) 0.004(4) -0.004(4) C26 0.017(5) 0.017(6) 0.019(6) -0.009(5) -0.008(5) 0.001(5) C27 0.020(6) 0.012(6) 0.017(6) -0.005(5) -0.006(5) -0.001(5) C28 0.014(5) 0.022(6) 0.019(6) -0.016(5) -0.007(4) 0.003(5) C29 0.016(5) 0.017(6) 0.013(6) -0.008(5) 0.004(4) -0.002(5) C30 0.015(5) 0.013(5) 0.010(6) -0.002(5) -0.001(4) 0.000(4) C31 0.012(5) 0.019(6) 0.012(6) -0.009(5) -0.005(4) 0.001(4) C32 0.005(5) 0.028(6) 0.019(6) -0.013(5) 0.011(4) -0.013(5) C33 0.014(5) 0.016(6) 0.015(6) -0.002(5) -0.004(4) 0.003(4) O1 0.054(6) 0.023(5) 0.021(5) -0.007(4) 0.006(4) 0.010(4) O2 0.113(9) 0.024(6) 0.024(6) -0.008(5) 0.009(6) 0.014(6) O3 0.050(6) 0.054(7) 0.050(7) -0.010(6) -0.019(5) -0.002(5) O4 0.055(6) 0.035(6) 0.034(6) -0.013(5) -0.011(5) 0.019(5) O5 0.051(6) 0.050(7) 0.022(5) -0.013(5) 0.012(4) 0.011(5) O6 0.020(4) 0.016(4) 0.027(5) -0.017(4) -0.002(3) 0.005(3) O7 0.029(4) 0.011(4) 0.020(5) -0.008(4) 0.001(3) -0.001(3) O8 0.022(4) 0.018(4) 0.016(4) 0.000(4) 0.006(3) -0.011(3) O9 0.029(4) 0.012(4) 0.017(5) -0.005(4) -0.003(3) 0.003(3) O10 0.032(5) 0.028(5) 0.028(5) -0.016(4) 0.001(4) 0.009(4) O11 0.094(8) 0.040(6) 0.030(6) -0.021(5) 0.006(6) 0.030(6) O12 0.034(6) 0.044(7) 0.143(12) -0.068(8) -0.019(6) 0.005(5) O13 0.025(5) 0.041(6) 0.070(7) -0.042(6) 0.017(4) -0.020(4) O14 0.058(6) 0.022(5) 0.025(5) -0.012(4) -0.004(4) -0.010(4) O15 0.044(5) 0.021(5) 0.023(5) 0.001(4) -0.019(4) -0.002(4) O16 0.034(5) 0.028(5) 0.015(5) -0.009(4) 0.003(4) 0.002(4) O17 0.046(5) 0.041(6) 0.017(5) -0.003(4) -0.008(4) -0.024(5) O18 0.036(5) 0.025(5) 0.025(5) -0.001(4) 0.009(4) 0.004(4) O19 0.041(5) 0.024(5) 0.012(5) -0.005(4) 0.001(4) 0.005(4) O20 0.011(4) 0.022(5) 0.044(6) -0.007(4) -0.008(4) -0.005(3) O21 0.029(4) 0.018(4) 0.014(4) -0.010(4) -0.005(3) -0.001(3) O22 0.023(9) 0.047(12) 0.079(16) -0.033(12) 0.020(9) -0.028(9) O23 0.046(11) 0.063(14) 0.019(11) -0.016(10) -0.016(8) 0.005(10) O24 0.046(5) 0.031(5) 0.028(5) -0.015(4) 0.000(4) 0.001(4) O25 0.049(6) 0.033(6) 0.029(6) -0.010(5) 0.010(4) -0.003(4) O26 0.055(6) 0.051(7) 0.051(7) -0.019(6) -0.009(5) -0.016(5) O27 0.060(7) 0.057(8) 0.074(9) -0.025(7) -0.018(6) -0.023(6) O28 0.021(4) 0.026(5) 0.048(6) -0.007(5) 0.014(4) -0.002(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 Cr1 O1 1.916(9) 2 ? Cr1 O1 1.971(9) . ? Cr1 O2 1.995(10) . ? Cr1 O3 1.996(11) . ? Cr1 O5 2.000(9) . ? Cr1 O4 2.000(9) . ? N1 C3 1.491(14) . ? N1 C4 1.495(14) . ? N2 C1 1.507(13) . ? N2 C5 1.520(15) . ? S1 O12 1.425(9) . ? S1 O11 1.448(11) . ? S1 O10 1.456(9) . ? S1 C9 1.755(11) . ? S2 O13 1.439(8) . ? S2 O14 1.451(9) . ? S2 O15 1.453(8) . ? S2 C16 1.751(11) . ? S3 O17 1.445(8) . ? S3 O16 1.456(8) . ? S3 O18 1.465(9) . ? S3 C23 1.753(11) . ? S4 O19 1.439(8) . ? S4 O20 1.445(7) . ? S4 O21 1.478(7) . ? S4 C30 1.768(11) . ? C1 C2 1.522(16) 2_656 ? C2 C1 1.522(16) 2_656 ? C2 C3 1.540(14) . ? C4 C5 1.515(17) . ? C6 O6 1.367(12) . ? C6 C7 1.396(14) . ? C6 C11 1.403(14) . ? C7 C8 1.403(15) . ? C7 C33 1.513(14) . ? C8 C9 1.383(15) . ? C9 C10 1.399(14) . ? C10 C11 1.391(14) . ? C11 C12 1.506(14) . ? C12 C14 1.515(14) . ? C13 O7 1.372(12) . ? C13 C18 1.388(15) . ? C13 C14 1.409(15) . ? C14 C15 1.392(14) . ? C15 C16 1.374(15) . ? C16 C17 1.410(14) . ? C17 C18 1.378(14) . ? C18 C19 1.526(14) . ? C19 C21 1.524(15) . ? C20 O8 1.362(12) . ? C20 C21 1.385(14) . ? C20 C25 1.405(15) . ? C21 C22 1.367(15) . ? C22 C23 1.366(15) . ? C23 C24 1.391(14) . ? C24 C25 1.365(15) . ? C25 C26 1.533(13) . ? C26 C28 1.508(14) . ? C27 C28 1.389(16) . ? C27 O9 1.390(13) . ? C27 C32 1.404(15) . ? C28 C29 1.390(15) . ? C29 C30 1.380(14) . ? C30 C31 1.376(15) . ? C31 C32 1.401(15) . ? C32 C33 1.527(15) . ? O1 Cr1 1.916(9) 2 ? 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 79.8(4) 2 . ? O1 Cr1 O2 91.1(4) 2 . ? O1 Cr1 O2 95.9(4) . . ? O1 Cr1 O3 172.7(4) 2 . ? O1 Cr1 O3 94.3(4) . . ? O2 Cr1 O3 85.3(5) . . ? O1 Cr1 O5 94.5(4) 2 . ? O1 Cr1 O5 92.0(4) . . ? O2 Cr1 O5 171.0(5) . . ? O3 Cr1 O5 89.8(4) . . ? O1 Cr1 O4 94.7(4) 2 . ? O1 Cr1 O4 174.3(4) . . ? O2 Cr1 O4 85.9(4) . . ? O3 Cr1 O4 91.3(4) . . ? O5 Cr1 O4 86.7(4) . . ? C3 N1 C4 112.5(9) . . ? C1 N2 C5 113.3(8) . . ? O12 S1 O11 113.8(7) . . ? O12 S1 O10 111.9(6) . . ? O11 S1 O10 110.3(6) . . ? O12 S1 C9 107.6(5) . . ? O11 S1 C9 107.0(6) . . ? O10 S1 C9 105.8(5) . . ? O13 S2 O14 112.8(5) . . ? O13 S2 O15 112.5(6) . . ? O14 S2 O15 109.8(5) . . ? O13 S2 C16 107.4(5) . . ? O14 S2 C16 106.0(5) . . ? O15 S2 C16 108.0(5) . . ? O17 S3 O16 113.6(5) . . ? O17 S3 O18 112.6(6) . . ? O16 S3 O18 111.4(5) . . ? O17 S3 C23 105.2(5) . . ? O16 S3 C23 106.8(5) . . ? O18 S3 C23 106.6(5) . . ? O19 S4 O20 114.5(5) . . ? O19 S4 O21 110.7(5) . . ? O20 S4 O21 113.4(5) . . ? O19 S4 C30 106.9(5) . . ? O20 S4 C30 105.0(5) . . ? O21 S4 C30 105.5(5) . . ? N2 C1 C2 112.2(8) . 2_656 ? C1 C2 C3 111.6(9) 2_656 . ? N1 C3 C2 115.8(9) . . ? N1 C4 C5 112.5(9) . . ? C4 C5 N2 116.3(9) . . ? O6 C6 C7 122.4(9) . . ? O6 C6 C11 115.6(9) . . ? C7 C6 C11 122.1(10) . . ? C6 C7 C8 117.7(9) . . ? C6 C7 C33 122.2(9) . . ? C8 C7 C33 120.1(9) . . ? C9 C8 C7 121.2(10) . . ? C8 C9 C10 119.9(10) . . ? C8 C9 S1 120.6(8) . . ? C10 C9 S1 119.4(8) . . ? C11 C10 C9 120.5(9) . . ? C10 C11 C6 118.5(9) . . ? C10 C11 C12 119.7(9) . . ? C6 C11 C12 121.7(9) . . ? C11 C12 C14 112.7(9) . . ? O7 C13 C18 116.5(9) . . ? O7 C13 C14 121.9(9) . . ? C18 C13 C14 121.5(10) . . ? C15 C14 C13 117.1(9) . . ? C15 C14 C12 118.1(9) . . ? C13 C14 C12 124.8(9) . . ? C16 C15 C14 122.1(10) . . ? C15 C16 C17 119.6(10) . . ? C15 C16 S2 122.5(8) . . ? C17 C16 S2 117.8(8) . . ? C18 C17 C16 119.5(9) . . ? C17 C18 C13 120.0(9) . . ? C17 C18 C19 118.8(9) . . ? C13 C18 C19 121.2(10) . . ? C21 C19 C18 112.2(8) . . ? O8 C20 C21 123.8(10) . . ? O8 C20 C25 115.1(8) . . ? C21 C20 C25 121.1(10) . . ? C22 C21 C20 118.0(10) . . ? C22 C21 C19 120.7(9) . . ? C20 C21 C19 121.4(10) . . ? C23 C22 C21 122.2(10) . . ? C22 C23 C24 119.6(10) . . ? C22 C23 S3 123.9(8) . . ? C24 C23 S3 116.4(8) . . ? C25 C24 C23 120.2(10) . . ? C24 C25 C20 118.9(9) . . ? C24 C25 C26 122.2(9) . . ? C20 C25 C26 118.8(9) . . ? C28 C26 C25 110.5(8) . . ? C28 C27 O9 123.0(10) . . ? C28 C27 C32 122.6(10) . . ? O9 C27 C32 114.3(10) . . ? C27 C28 C29 117.9(10) . . ? C27 C28 C26 123.3(10) . . ? C29 C28 C26 118.8(10) . . ? C30 C29 C28 120.6(10) . . ? C31 C30 C29 120.9(10) . . ? C31 C30 S4 118.4(8) . . ? C29 C30 S4 120.6(8) . . ? C30 C31 C32 120.6(10) . . ? C31 C32 C27 117.1(10) . . ? C31 C32 C33 119.2(9) . . ? C27 C32 C33 123.6(10) . . ? C7 C33 C32 111.3(8) . . ? Cr1 O1 Cr1 100.2(4) 2 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.376 _refine_diff_density_min -1.755 _refine_diff_density_rms 0.260