data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Smith, Kevin' _publ_contact_author_email kevin.m.smith@ubc.ca _publ_section_title ; Cyclopentadienyl mesityl complexes of chromium(II) and chromium(III) ; loop_ _publ_author_name W.Zhou J.Therrien L.Wence E.Yallits J.Conway B.Patrick K.Smith # Attachment '- CpCrMes.cif' data_2_CpCr(iPrNHC)Mes _database_code_depnum_ccdc_archive 'CCDC 791384' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Cr N2' _chemical_formula_weight 388.51 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' Cr Cr 0.3209 0.6236 '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 8.3577(2) _cell_length_b 8.4155(2) _cell_length_c 18.1329(5) _cell_angle_alpha 97.0890(10) _cell_angle_beta 98.1880(10) _cell_angle_gamma 118.4210(10) _cell_volume 1083.10(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.817 _cell_measurement_theta_max 27.8275 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17616 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.86 _reflns_number_total 5028 _reflns_number_gt 4383 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.6230P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5028 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 C1 C 0.95196(18) 0.22272(19) 0.71223(7) 0.0157(3) Uani 1 1 d . . . C2 C 1.07607(18) 0.41708(19) 0.73075(8) 0.0167(3) Uani 1 1 d . . . C3 C 1.17628(19) 0.51078(19) 0.67964(8) 0.0192(3) Uani 1 1 d . . . H3 H 1.2600 0.6406 0.6949 0.023 Uiso 1 1 calc R . . C4 C 1.1558(2) 0.4177(2) 0.60671(8) 0.0194(3) Uani 1 1 d . . . C5 C 1.03311(19) 0.22716(19) 0.58705(8) 0.0180(3) Uani 1 1 d . . . H5 H 1.0156 0.1607 0.5375 0.022 Uiso 1 1 calc R . . C6 C 0.93474(18) 0.13063(19) 0.63809(8) 0.0165(3) Uani 1 1 d . . . C7 C 0.8099(2) -0.0778(2) 0.61106(8) 0.0222(3) Uani 1 1 d . . . H7A H 0.7544 -0.1083 0.5563 0.033 Uiso 1 1 calc R . . H7B H 0.7103 -0.1218 0.6390 0.033 Uiso 1 1 calc R . . H7C H 0.8843 -0.1377 0.6204 0.033 Uiso 1 1 calc R . . C8 C 1.2601(2) 0.5179(2) 0.55033(9) 0.0276(3) Uani 1 1 d . . . H8A H 1.2963 0.4398 0.5207 0.041 Uiso 1 1 calc R . . H8B H 1.3723 0.6342 0.5780 0.041 Uiso 1 1 calc R . . H8C H 1.1792 0.5446 0.5157 0.041 Uiso 1 1 calc R . . C9 C 1.1022(2) 0.5298(2) 0.80805(8) 0.0225(3) Uani 1 1 d . . . H9A H 1.2040 0.6572 0.8144 0.034 Uiso 1 1 calc R . . H9B H 1.1330 0.4748 0.8484 0.034 Uiso 1 1 calc R . . H9C H 0.9863 0.5302 0.8113 0.034 Uiso 1 1 calc R . . C10 C 0.62587(18) 0.19685(18) 0.78838(7) 0.0154(3) Uani 1 1 d . . . C11 C 0.39881(19) 0.26239(19) 0.74661(8) 0.0193(3) Uani 1 1 d . . . H11 H 0.3044 0.2686 0.7133 0.023 Uiso 1 1 calc R . . C12 C 0.45847(19) 0.32962(19) 0.82256(8) 0.0195(3) Uani 1 1 d . . . H12 H 0.4138 0.3922 0.8534 0.023 Uiso 1 1 calc R . . C13 C 0.4912(2) 0.1067(2) 0.64713(8) 0.0218(3) Uani 1 1 d . . . H13 H 0.5627 0.0394 0.6482 0.026 Uiso 1 1 calc R . . C14 C 0.2893(2) -0.0314(2) 0.60595(9) 0.0275(3) Uani 1 1 d . . . H14A H 0.2360 -0.1303 0.6338 0.041 Uiso 1 1 calc R . . H14B H 0.2852 -0.0848 0.5540 0.041 Uiso 1 1 calc R . . H14C H 0.2167 0.0320 0.6035 0.041 Uiso 1 1 calc R . . C15 C 0.5827(2) 0.2638(3) 0.60649(9) 0.0330(4) Uani 1 1 d . . . H15A H 0.7122 0.3492 0.6347 0.050 Uiso 1 1 calc R . . H15B H 0.5135 0.3305 0.6039 0.050 Uiso 1 1 calc R . . H15C H 0.5815 0.2130 0.5547 0.050 Uiso 1 1 calc R . . C16 C 0.70201(19) 0.3425(2) 0.92701(8) 0.0195(3) Uani 1 1 d . . . H16 H 0.8038 0.3115 0.9277 0.023 Uiso 1 1 calc R . . C17 C 0.5757(3) 0.2296(2) 0.97524(9) 0.0347(4) Uani 1 1 d . . . H17A H 0.5204 0.0974 0.9531 0.052 Uiso 1 1 calc R . . H17B H 0.4760 0.2594 0.9766 0.052 Uiso 1 1 calc R . . H17C H 0.6489 0.2590 1.0273 0.052 Uiso 1 1 calc R . . C18 C 0.7940(2) 0.5505(2) 0.95798(9) 0.0272(3) Uani 1 1 d . . . H18A H 0.8738 0.6170 0.9249 0.041 Uiso 1 1 calc R . . H18B H 0.8700 0.5838 1.0098 0.041 Uiso 1 1 calc R . . H18C H 0.6971 0.5845 0.9592 0.041 Uiso 1 1 calc R . . C19 C 0.7343(2) -0.2206(2) 0.79125(9) 0.0302(4) Uani 1 1 d . . . H19 H 0.6573 -0.3189 0.7480 0.036 Uiso 1 1 calc R . . C20 C 0.9299(2) -0.1074(2) 0.80614(10) 0.0295(3) Uani 1 1 d . . . H20 H 1.0078 -0.1128 0.7737 0.035 Uiso 1 1 calc R . . C21 C 0.9901(2) 0.0156(2) 0.87763(9) 0.0278(3) Uani 1 1 d . . . H21 H 1.1159 0.1053 0.9023 0.033 Uiso 1 1 calc R . . C22 C 0.8324(2) -0.0175(2) 0.90577(9) 0.0254(3) Uani 1 1 d . . . H22 H 0.8320 0.0458 0.9528 0.030 Uiso 1 1 calc R . . C23 C 0.6737(2) -0.1620(2) 0.85190(9) 0.0276(3) Uani 1 1 d . . . H23 H 0.5476 -0.2110 0.8560 0.033 Uiso 1 1 calc R . . N001 N 0.59733(15) 0.29008(16) 0.84718(6) 0.0163(2) Uani 1 1 d . . . N002 N 0.50224(15) 0.18232(16) 0.72664(6) 0.0165(2) Uani 1 1 d . . . Cr01 Cr 0.80697(3) 0.08545(3) 0.790954(12) 0.01514(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0148(6) 0.0200(6) 0.0158(6) 0.0050(5) 0.0028(5) 0.0113(5) C2 0.0166(6) 0.0202(7) 0.0154(6) 0.0035(5) 0.0019(5) 0.0115(5) C3 0.0197(6) 0.0177(6) 0.0209(7) 0.0054(5) 0.0036(5) 0.0099(5) C4 0.0216(7) 0.0241(7) 0.0177(7) 0.0086(5) 0.0063(5) 0.0140(6) C5 0.0194(6) 0.0240(7) 0.0135(6) 0.0033(5) 0.0032(5) 0.0135(6) C6 0.0141(6) 0.0196(6) 0.0167(6) 0.0019(5) 0.0009(5) 0.0103(5) C7 0.0212(7) 0.0212(7) 0.0208(7) 0.0006(6) 0.0056(6) 0.0088(6) C8 0.0349(8) 0.0274(8) 0.0238(8) 0.0105(6) 0.0133(7) 0.0153(7) C9 0.0262(7) 0.0199(7) 0.0192(7) 0.0014(6) 0.0054(6) 0.0105(6) C10 0.0155(6) 0.0175(6) 0.0142(6) 0.0059(5) 0.0045(5) 0.0084(5) C11 0.0179(6) 0.0231(7) 0.0213(7) 0.0050(6) 0.0032(5) 0.0139(6) C12 0.0189(6) 0.0223(7) 0.0214(7) 0.0044(6) 0.0051(5) 0.0136(6) C13 0.0253(7) 0.0349(8) 0.0132(6) 0.0041(6) 0.0033(5) 0.0218(7) C14 0.0319(8) 0.0309(8) 0.0216(7) -0.0024(6) -0.0034(6) 0.0216(7) C15 0.0335(9) 0.0514(11) 0.0217(8) 0.0162(7) 0.0099(7) 0.0244(8) C16 0.0225(7) 0.0235(7) 0.0140(6) 0.0032(5) 0.0012(5) 0.0137(6) C17 0.0412(10) 0.0355(9) 0.0192(8) 0.0096(7) 0.0061(7) 0.0125(8) C18 0.0316(8) 0.0254(8) 0.0203(7) 0.0001(6) -0.0007(6) 0.0138(7) C19 0.0439(9) 0.0185(7) 0.0249(8) 0.0052(6) 0.0013(7) 0.0148(7) C20 0.0409(9) 0.0350(9) 0.0338(9) 0.0180(7) 0.0170(7) 0.0308(8) C21 0.0232(7) 0.0271(8) 0.0336(9) 0.0127(7) -0.0012(6) 0.0138(6) C22 0.0389(9) 0.0260(8) 0.0188(7) 0.0099(6) 0.0065(6) 0.0211(7) C23 0.0240(7) 0.0283(8) 0.0335(9) 0.0184(7) 0.0091(6) 0.0120(6) N001 0.0174(5) 0.0196(6) 0.0145(5) 0.0044(4) 0.0031(4) 0.0113(5) N002 0.0170(5) 0.0214(6) 0.0147(5) 0.0045(4) 0.0035(4) 0.0123(5) Cr01 0.01612(11) 0.01861(12) 0.01451(11) 0.00557(8) 0.00404(8) 0.01108(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.4177(18) . ? C1 C2 1.4192(19) . ? C1 Cr01 2.0995(13) . ? C2 C3 1.398(2) . ? C2 C9 1.5164(19) . ? C3 C4 1.394(2) . ? C3 H3 0.9500 . ? C4 C5 1.392(2) . ? C4 C8 1.511(2) . ? C5 C6 1.3996(19) . ? C5 H5 0.9500 . ? C6 C7 1.5182(19) . ? 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 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N001 1.3614(17) . ? C10 N002 1.3611(17) . ? C10 Cr01 2.1245(13) . ? C11 C12 1.345(2) . ? C11 N002 1.3841(17) . ? C11 H11 0.9500 . ? C12 N001 1.3833(17) . ? C12 H12 0.9500 . ? C13 N002 1.4736(17) . ? C13 C14 1.522(2) . ? C13 C15 1.522(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N001 1.4730(17) . ? C16 C17 1.515(2) . ? C16 C18 1.525(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C23 1.404(2) . ? C19 C20 1.407(2) . ? C19 Cr01 2.3490(15) . ? C19 H19 0.9500 . ? C20 C21 1.412(2) . ? C20 Cr01 2.3194(15) . ? C20 H20 0.9500 . ? C21 C22 1.397(2) . ? C21 Cr01 2.3575(15) . ? C21 H21 0.9500 . ? C22 C23 1.412(2) . ? C22 Cr01 2.3717(14) . ? C22 H22 0.9500 . ? C23 Cr01 2.3469(15) . ? C23 H23 0.9500 . ? 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 C6 C1 C2 115.46(12) . . ? C6 C1 Cr01 123.28(10) . . ? C2 C1 Cr01 121.26(10) . . ? C3 C2 C1 122.19(12) . . ? C3 C2 C9 117.97(12) . . ? C1 C2 C9 119.84(12) . . ? C4 C3 C2 121.38(13) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 117.35(13) . . ? C5 C4 C8 120.73(13) . . ? C3 C4 C8 121.91(13) . . ? C4 C5 C6 121.99(13) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 121.60(13) . . ? C5 C6 C7 117.18(12) . . ? C1 C6 C7 121.22(12) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 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 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N001 C10 N002 103.35(11) . . ? N001 C10 Cr01 129.20(9) . . ? N002 C10 Cr01 127.37(10) . . ? C12 C11 N002 106.41(12) . . ? C12 C11 H11 126.8 . . ? N002 C11 H11 126.8 . . ? C11 C12 N001 106.80(12) . . ? C11 C12 H12 126.6 . . ? N001 C12 H12 126.6 . . ? N002 C13 C14 110.58(12) . . ? N002 C13 C15 109.95(13) . . ? C14 C13 C15 112.11(12) . . ? N002 C13 H13 108.0 . . ? C14 C13 H13 108.0 . . ? C15 C13 H13 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N001 C16 C17 110.22(12) . . ? N001 C16 C18 110.74(11) . . ? C17 C16 C18 112.66(13) . . ? N001 C16 H16 107.7 . . ? C17 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? 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 . . ? C23 C19 C20 107.59(14) . . ? C23 C19 Cr01 72.52(9) . . ? C20 C19 Cr01 71.31(9) . . ? C23 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? Cr01 C19 H19 121.7 . . ? C19 C20 C21 108.13(14) . . ? C19 C20 Cr01 73.61(9) . . ? C21 C20 Cr01 73.91(9) . . ? C19 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? Cr01 C20 H20 118.5 . . ? C22 C21 C20 108.04(14) . . ? C22 C21 Cr01 73.37(9) . . ? C20 C21 Cr01 70.97(8) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Cr01 C21 H21 121.4 . . ? C21 C22 C23 107.91(14) . . ? C21 C22 Cr01 72.26(9) . . ? C23 C22 Cr01 71.63(8) . . ? C21 C22 H22 126.0 . . ? C23 C22 H22 126.0 . . ? Cr01 C22 H22 121.8 . . ? C19 C23 C22 108.27(14) . . ? C19 C23 Cr01 72.68(9) . . ? C22 C23 Cr01 73.55(9) . . ? C19 C23 H23 125.9 . . ? C22 C23 H23 125.9 . . ? Cr01 C23 H23 119.7 . . ? C10 N001 C12 111.61(11) . . ? C10 N001 C16 124.03(11) . . ? C12 N001 C16 124.37(11) . . ? C10 N002 C11 111.83(11) . . ? C10 N002 C13 124.38(11) . . ? C11 N002 C13 123.56(11) . . ? C1 Cr01 C10 96.71(5) . . ? C1 Cr01 C20 99.64(5) . . ? C10 Cr01 C20 162.17(6) . . ? C1 Cr01 C23 154.87(6) . . ? C10 Cr01 C23 104.27(5) . . ? C20 Cr01 C23 58.18(6) . . ? C1 Cr01 C19 120.17(6) . . ? C10 Cr01 C19 128.38(6) . . ? C20 Cr01 C19 35.08(6) . . ? C23 Cr01 C19 34.80(6) . . ? C1 Cr01 C21 112.04(5) . . ? C10 Cr01 C21 140.84(6) . . ? C20 Cr01 C21 35.12(6) . . ? C23 Cr01 C21 57.75(5) . . ? C19 Cr01 C21 58.02(6) . . ? C1 Cr01 C22 145.39(5) . . ? C10 Cr01 C22 110.27(5) . . ? C20 Cr01 C22 57.95(6) . . ? C23 Cr01 C22 34.82(6) . . ? C19 Cr01 C22 57.83(5) . . ? C21 Cr01 C22 34.37(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.80(19) . . . . ? Cr01 C1 C2 C3 178.94(10) . . . . ? C6 C1 C2 C9 178.83(12) . . . . ? Cr01 C1 C2 C9 -1.43(17) . . . . ? C1 C2 C3 C4 1.5(2) . . . . ? C9 C2 C3 C4 -178.17(13) . . . . ? C2 C3 C4 C5 -0.7(2) . . . . ? C2 C3 C4 C8 178.64(13) . . . . ? C3 C4 C5 C6 -0.7(2) . . . . ? C8 C4 C5 C6 179.97(13) . . . . ? C4 C5 C6 C1 1.4(2) . . . . ? C4 C5 C6 C7 -178.02(12) . . . . ? C2 C1 C6 C5 -0.58(18) . . . . ? Cr01 C1 C6 C5 179.69(10) . . . . ? C2 C1 C6 C7 178.78(12) . . . . ? Cr01 C1 C6 C7 -0.96(17) . . . . ? N002 C11 C12 N001 0.30(15) . . . . ? C23 C19 C20 C21 2.50(17) . . . . ? Cr01 C19 C20 C21 66.40(10) . . . . ? C23 C19 C20 Cr01 -63.90(11) . . . . ? C19 C20 C21 C22 -1.71(17) . . . . ? Cr01 C20 C21 C22 64.49(11) . . . . ? C19 C20 C21 Cr01 -66.20(10) . . . . ? C20 C21 C22 C23 0.26(17) . . . . ? Cr01 C21 C22 C23 63.18(11) . . . . ? C20 C21 C22 Cr01 -62.92(10) . . . . ? C20 C19 C23 C22 -2.35(17) . . . . ? Cr01 C19 C23 C22 -65.46(11) . . . . ? C20 C19 C23 Cr01 63.11(10) . . . . ? C21 C22 C23 C19 1.30(17) . . . . ? Cr01 C22 C23 C19 64.88(11) . . . . ? C21 C22 C23 Cr01 -63.59(11) . . . . ? N002 C10 N001 C12 0.79(15) . . . . ? Cr01 C10 N001 C12 -176.09(10) . . . . ? N002 C10 N001 C16 -179.07(12) . . . . ? Cr01 C10 N001 C16 4.05(19) . . . . ? C11 C12 N001 C10 -0.71(16) . . . . ? C11 C12 N001 C16 179.15(13) . . . . ? C17 C16 N001 C10 -110.32(15) . . . . ? C18 C16 N001 C10 124.33(14) . . . . ? C17 C16 N001 C12 69.83(17) . . . . ? C18 C16 N001 C12 -55.51(18) . . . . ? N001 C10 N002 C11 -0.60(15) . . . . ? Cr01 C10 N002 C11 176.36(10) . . . . ? N001 C10 N002 C13 173.98(12) . . . . ? Cr01 C10 N002 C13 -9.06(19) . . . . ? C12 C11 N002 C10 0.19(16) . . . . ? C12 C11 N002 C13 -174.44(13) . . . . ? C14 C13 N002 C10 132.94(14) . . . . ? C15 C13 N002 C10 -102.72(15) . . . . ? C14 C13 N002 C11 -53.10(18) . . . . ? C15 C13 N002 C11 71.24(17) . . . . ? C6 C1 Cr01 C10 -110.77(11) . . . . ? C2 C1 Cr01 C10 69.51(11) . . . . ? C6 C1 Cr01 C20 62.08(12) . . . . ? C2 C1 Cr01 C20 -117.63(11) . . . . ? C6 C1 Cr01 C23 35.87(19) . . . . ? C2 C1 Cr01 C23 -143.85(12) . . . . ? C6 C1 Cr01 C19 31.55(13) . . . . ? C2 C1 Cr01 C19 -148.17(10) . . . . ? C6 C1 Cr01 C21 96.36(11) . . . . ? C2 C1 Cr01 C21 -83.36(11) . . . . ? C6 C1 Cr01 C22 107.54(12) . . . . ? C2 C1 Cr01 C22 -72.18(14) . . . . ? N001 C10 Cr01 C1 -124.99(12) . . . . ? N002 C10 Cr01 C1 58.83(12) . . . . ? N001 C10 Cr01 C20 78.6(2) . . . . ? N002 C10 Cr01 C20 -97.5(2) . . . . ? N001 C10 Cr01 C23 68.96(13) . . . . ? N002 C10 Cr01 C23 -107.22(12) . . . . ? N001 C10 Cr01 C19 97.40(13) . . . . ? N002 C10 Cr01 C19 -78.78(13) . . . . ? N001 C10 Cr01 C21 12.99(17) . . . . ? N002 C10 Cr01 C21 -163.19(11) . . . . ? N001 C10 Cr01 C22 32.97(13) . . . . ? N002 C10 Cr01 C22 -143.21(11) . . . . ? C19 C20 Cr01 C1 -130.16(10) . . . . ? C21 C20 Cr01 C1 114.85(10) . . . . ? C19 C20 Cr01 C10 26.0(2) . . . . ? C21 C20 Cr01 C10 -89.0(2) . . . . ? C19 C20 Cr01 C23 37.08(9) . . . . ? C21 C20 Cr01 C23 -77.91(10) . . . . ? C21 C20 Cr01 C19 -114.99(14) . . . . ? C19 C20 Cr01 C21 114.99(14) . . . . ? C19 C20 Cr01 C22 78.37(10) . . . . ? C21 C20 Cr01 C22 -36.62(9) . . . . ? C19 C23 Cr01 C1 -6.54(18) . . . . ? C22 C23 Cr01 C1 109.21(14) . . . . ? C19 C23 Cr01 C10 139.15(10) . . . . ? C22 C23 Cr01 C10 -105.10(9) . . . . ? C19 C23 Cr01 C20 -37.38(10) . . . . ? C22 C23 Cr01 C20 78.38(10) . . . . ? C22 C23 Cr01 C19 115.75(14) . . . . ? C19 C23 Cr01 C21 -79.07(10) . . . . ? C22 C23 Cr01 C21 36.68(9) . . . . ? C19 C23 Cr01 C22 -115.75(14) . . . . ? C23 C19 Cr01 C1 176.79(9) . . . . ? C20 C19 Cr01 C1 60.62(11) . . . . ? C23 C19 Cr01 C10 -53.96(12) . . . . ? C20 C19 Cr01 C10 -170.13(9) . . . . ? C23 C19 Cr01 C20 116.17(14) . . . . ? C20 C19 Cr01 C23 -116.17(14) . . . . ? C23 C19 Cr01 C21 78.23(10) . . . . ? C20 C19 Cr01 C21 -37.94(9) . . . . ? C23 C19 Cr01 C22 37.41(9) . . . . ? C20 C19 Cr01 C22 -78.75(10) . . . . ? C22 C21 Cr01 C1 168.75(9) . . . . ? C20 C21 Cr01 C1 -74.83(10) . . . . ? C22 C21 Cr01 C10 34.58(14) . . . . ? C20 C21 Cr01 C10 150.99(10) . . . . ? C22 C21 Cr01 C20 -116.42(14) . . . . ? C22 C21 Cr01 C23 -37.17(9) . . . . ? C20 C21 Cr01 C23 79.25(10) . . . . ? C22 C21 Cr01 C19 -78.52(10) . . . . ? C20 C21 Cr01 C19 37.89(10) . . . . ? C20 C21 Cr01 C22 116.42(14) . . . . ? C21 C22 Cr01 C1 -18.56(15) . . . . ? C23 C22 Cr01 C1 -135.08(11) . . . . ? C21 C22 Cr01 C10 -157.54(9) . . . . ? C23 C22 Cr01 C10 85.94(10) . . . . ? C21 C22 Cr01 C20 37.44(10) . . . . ? C23 C22 Cr01 C20 -79.08(10) . . . . ? C21 C22 Cr01 C23 116.52(14) . . . . ? C21 C22 Cr01 C19 79.12(10) . . . . ? C23 C22 Cr01 C19 -37.40(10) . . . . ? C23 C22 Cr01 C21 -116.52(14) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.318 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.047 data_6a_CpCr(OCPhCHCMeO)I _database_code_depnum_ccdc_archive 'CCDC 791385' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Cr I O2' _chemical_formula_weight 405.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 19.6228(14) _cell_length_b 7.4584(6) _cell_length_c 20.5310(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.570(4) _cell_angle_gamma 90.00 _cell_volume 2971.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8397 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.72 _exptl_crystal_description tablet _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 2.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30375 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.96 _reflns_number_total 7098 _reflns_number_gt 5357 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+3.5261P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7098 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 C1 C 0.21723(16) -0.4095(4) 0.78642(15) 0.0310(7) Uani 1 1 d . . . H1A H 0.2256 -0.3340 0.7494 0.046 Uiso 1 1 calc R . . H1B H 0.1760 -0.3669 0.8034 0.046 Uiso 1 1 calc R . . H1C H 0.2102 -0.5338 0.7715 0.046 Uiso 1 1 calc R . . C2 C 0.27803(16) -0.3998(4) 0.83985(14) 0.0237(7) Uani 1 1 d . . . C3 C 0.27200(16) -0.3155(4) 0.89875(15) 0.0262(7) Uani 1 1 d . . . H3 H 0.2285 -0.2655 0.9037 0.031 Uiso 1 1 calc R . . C4 C 0.32538(15) -0.2989(4) 0.95136(14) 0.0206(6) Uani 1 1 d . . . C5 C 0.31513(15) -0.2066(4) 1.01306(14) 0.0215(6) Uani 1 1 d . . . C6 C 0.25059(16) -0.1821(4) 1.03186(16) 0.0291(7) Uani 1 1 d . . . H6 H 0.2105 -0.2230 1.0041 0.035 Uiso 1 1 calc R . . C7 C 0.24443(18) -0.0985(5) 1.09081(17) 0.0354(8) Uani 1 1 d . . . H7 H 0.2003 -0.0850 1.1039 0.042 Uiso 1 1 calc R . . C8 C 0.30208(18) -0.0344(4) 1.13070(16) 0.0340(8) Uani 1 1 d . . . H8 H 0.2976 0.0239 1.1710 0.041 Uiso 1 1 calc R . . C9 C 0.36540(18) -0.0552(5) 1.11207(15) 0.0331(8) Uani 1 1 d . . . H9 H 0.4050 -0.0092 1.1392 0.040 Uiso 1 1 calc R . . C10 C 0.37255(16) -0.1423(4) 1.05420(15) 0.0261(7) Uani 1 1 d . . . H10 H 0.4171 -0.1585 1.0424 0.031 Uiso 1 1 calc R . . C11 C 0.53685(17) -0.4386(5) 0.89710(17) 0.0335(8) Uani 1 1 d . . . H11 H 0.5646 -0.4823 0.9357 0.040 Uiso 1 1 calc R . . C12 C 0.50680(18) -0.2692(5) 0.88943(17) 0.0350(8) Uani 1 1 d . . . H12 H 0.5111 -0.1767 0.9216 0.042 Uiso 1 1 calc R . . C13 C 0.46907(19) -0.2593(5) 0.82607(18) 0.0409(9) Uani 1 1 d . . . H13 H 0.4425 -0.1599 0.8079 0.049 Uiso 1 1 calc R . . C14 C 0.47749(19) -0.4226(5) 0.79417(17) 0.0418(9) Uani 1 1 d . . . H14 H 0.4582 -0.4523 0.7503 0.050 Uiso 1 1 calc R . . C15 C 0.51913(17) -0.5335(5) 0.83807(17) 0.0366(8) Uani 1 1 d . . . H15 H 0.5330 -0.6522 0.8295 0.044 Uiso 1 1 calc R . . C16 C 0.20478(19) 0.2791(5) 0.99122(16) 0.0374(8) Uani 1 1 d . . . H16A H 0.1944 0.4072 0.9857 0.056 Uiso 1 1 calc R . . H16B H 0.2545 0.2603 0.9934 0.056 Uiso 1 1 calc R . . H16C H 0.1900 0.2364 1.0320 0.056 Uiso 1 1 calc R . . C17 C 0.16742(16) 0.1779(4) 0.93419(15) 0.0267(7) Uani 1 1 d . . . C18 C 0.19813(17) 0.1572(4) 0.87786(15) 0.0297(7) Uani 1 1 d . . . H18 H 0.2439 0.2003 0.8791 0.036 Uiso 1 1 calc R . . C19 C 0.16669(15) 0.0780(4) 0.82006(15) 0.0235(7) Uani 1 1 d . . . C20 C 0.20361(16) 0.0648(4) 0.76231(15) 0.0252(7) Uani 1 1 d . . . C21 C 0.27423(17) 0.0872(5) 0.76726(17) 0.0334(8) Uani 1 1 d . . . H21 H 0.3006 0.1136 0.8088 0.040 Uiso 1 1 calc R . . C22 C 0.30683(19) 0.0713(5) 0.71228(19) 0.0421(9) Uani 1 1 d . . . H22 H 0.3553 0.0875 0.7161 0.051 Uiso 1 1 calc R . . C23 C 0.2691(2) 0.0321(5) 0.65207(18) 0.0417(9) Uani 1 1 d . . . H23 H 0.2916 0.0211 0.6143 0.050 Uiso 1 1 calc R . . C24 C 0.19934(19) 0.0089(5) 0.64647(17) 0.0383(8) Uani 1 1 d . . . H24 H 0.1734 -0.0185 0.6048 0.046 Uiso 1 1 calc R . . C25 C 0.16647(17) 0.0249(4) 0.70105(15) 0.0297(7) Uani 1 1 d . . . H25 H 0.1180 0.0086 0.6967 0.036 Uiso 1 1 calc R . . C26 C -0.06794(19) -0.0518(6) 0.8393(4) 0.093(2) Uani 1 1 d . . . H26 H -0.0829 -0.1692 0.8260 0.112 Uiso 1 1 calc R . . C27 C -0.0461(2) 0.0905(8) 0.8006(2) 0.0621(14) Uani 1 1 d . . . H27 H -0.0449 0.0864 0.7546 0.075 Uiso 1 1 calc R . . C28 C -0.0280(2) 0.2281(7) 0.8394(3) 0.0685(14) Uani 1 1 d . . . H28 H -0.0099 0.3375 0.8256 0.082 Uiso 1 1 calc R . . C29 C -0.0382(2) 0.1947(8) 0.8984(3) 0.0706(15) Uani 1 1 d . . . H29 H -0.0300 0.2786 0.9335 0.085 Uiso 1 1 calc R . . C30 C -0.0613(2) 0.0303(9) 0.9048(3) 0.0734(17) Uani 1 1 d . . . H30 H -0.0716 -0.0240 0.9440 0.088 Uiso 1 1 calc R . . O1 O 0.33285(11) -0.4726(3) 0.82591(10) 0.0291(5) Uani 1 1 d . . . O2 O 0.38568(11) -0.3610(3) 0.95083(10) 0.0273(5) Uani 1 1 d . . . O3 O 0.10818(11) 0.1170(3) 0.94115(10) 0.0321(5) Uani 1 1 d . . . O4 O 0.10560(11) 0.0154(3) 0.81165(10) 0.0330(5) Uani 1 1 d . . . Cr1 Cr 0.42249(2) -0.47339(7) 0.87930(2) 0.02267(11) Uani 1 1 d . . . Cr2 Cr 0.04152(3) 0.00602(7) 0.87444(2) 0.02797(12) Uani 1 1 d . . . I1 I 0.415090(12) -0.80660(3) 0.923218(11) 0.03524(7) Uani 1 1 d . . . I2 I 0.067258(12) -0.33250(3) 0.911881(12) 0.03942(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0267(18) 0.0367(18) 0.0267(17) -0.0024(14) -0.0052(14) 0.0049(15) C2 0.0254(17) 0.0221(14) 0.0221(15) 0.0045(12) -0.0013(13) -0.0004(13) C3 0.0208(16) 0.0313(16) 0.0254(16) 0.0002(14) 0.0002(12) 0.0056(13) C4 0.0217(16) 0.0194(14) 0.0208(15) 0.0037(12) 0.0036(12) 0.0012(12) C5 0.0246(16) 0.0199(14) 0.0203(15) 0.0028(12) 0.0047(12) 0.0022(12) C6 0.0242(17) 0.0322(17) 0.0307(17) -0.0006(14) 0.0034(13) 0.0035(14) C7 0.031(2) 0.0407(19) 0.037(2) -0.0003(16) 0.0123(15) 0.0091(16) C8 0.048(2) 0.0303(17) 0.0258(17) -0.0042(14) 0.0137(16) 0.0017(16) C9 0.037(2) 0.0375(18) 0.0245(17) -0.0043(14) 0.0020(14) -0.0089(16) C10 0.0218(17) 0.0326(17) 0.0248(16) -0.0006(13) 0.0062(13) -0.0036(13) C11 0.0223(17) 0.048(2) 0.0308(18) 0.0027(16) 0.0062(14) -0.0050(15) C12 0.036(2) 0.0324(18) 0.038(2) -0.0011(15) 0.0079(16) -0.0126(15) C13 0.044(2) 0.041(2) 0.038(2) 0.0191(17) 0.0084(17) 0.0030(17) C14 0.043(2) 0.065(3) 0.0197(17) -0.0010(17) 0.0106(15) -0.0074(19) C15 0.0295(19) 0.045(2) 0.038(2) -0.0030(17) 0.0145(15) 0.0034(16) C16 0.046(2) 0.0396(19) 0.0247(17) -0.0047(15) -0.0002(15) -0.0046(17) C17 0.0294(18) 0.0236(15) 0.0254(16) 0.0000(13) -0.0013(13) 0.0012(14) C18 0.0256(18) 0.0337(17) 0.0298(17) -0.0051(14) 0.0044(13) -0.0069(14) C19 0.0224(17) 0.0219(15) 0.0261(16) 0.0020(12) 0.0034(13) 0.0017(12) C20 0.0290(18) 0.0221(15) 0.0246(16) -0.0005(12) 0.0044(13) 0.0008(13) C21 0.0289(19) 0.0404(19) 0.0308(18) -0.0059(15) 0.0037(14) -0.0029(15) C22 0.034(2) 0.048(2) 0.047(2) -0.0043(18) 0.0166(17) -0.0010(17) C23 0.054(3) 0.043(2) 0.033(2) -0.0012(17) 0.0231(18) -0.0034(18) C24 0.048(2) 0.041(2) 0.0252(18) -0.0010(16) 0.0051(16) -0.0048(17) C25 0.0283(18) 0.0294(16) 0.0310(18) 0.0026(14) 0.0032(14) -0.0013(14) C26 0.011(2) 0.039(2) 0.214(7) -0.029(4) -0.032(3) 0.0038(18) C27 0.034(2) 0.111(4) 0.037(2) -0.004(3) -0.0100(18) 0.024(3) C28 0.058(3) 0.057(3) 0.089(4) 0.018(3) 0.004(3) 0.021(2) C29 0.041(3) 0.095(4) 0.077(4) -0.013(3) 0.014(3) 0.023(3) C30 0.019(2) 0.127(5) 0.077(3) 0.057(4) 0.018(2) 0.017(3) O1 0.0265(12) 0.0359(12) 0.0227(11) -0.0060(10) -0.0032(9) 0.0071(10) O2 0.0222(12) 0.0371(12) 0.0221(11) -0.0060(9) 0.0012(9) 0.0050(10) O3 0.0319(13) 0.0409(13) 0.0241(12) -0.0026(10) 0.0061(10) -0.0036(11) O4 0.0249(12) 0.0495(14) 0.0250(12) -0.0076(11) 0.0045(9) -0.0078(11) Cr1 0.0211(3) 0.0276(2) 0.0188(2) -0.0013(2) 0.00129(19) 0.0031(2) Cr2 0.0207(3) 0.0360(3) 0.0272(3) 0.0000(2) 0.0035(2) 0.0006(2) I1 0.03240(13) 0.03091(11) 0.03919(13) 0.00614(10) -0.00527(9) -0.00504(10) I2 0.03621(14) 0.03431(12) 0.04721(15) 0.00003(11) 0.00443(10) 0.00281(10) _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 C2 1.497(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.275(4) . ? C2 C3 1.384(4) . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 O2 1.272(3) . ? C4 C5 1.481(4) . ? C5 C10 1.389(4) . ? C5 C6 1.390(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.379(5) . ? C7 H7 0.9500 . ? C8 C9 1.362(5) . ? C8 H8 0.9500 . ? C9 C10 1.380(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.393(5) . ? C11 C15 1.402(5) . ? C11 Cr1 2.234(3) . ? C11 H11 0.9500 . ? C12 C13 1.400(5) . ? C12 Cr1 2.235(3) . ? C12 H12 0.9500 . ? C13 C14 1.404(5) . ? C13 Cr1 2.209(3) . ? C13 H13 0.9500 . ? C14 C15 1.395(5) . ? C14 Cr1 2.219(3) . ? C14 H14 0.9500 . ? C15 Cr1 2.234(3) . ? C15 H15 0.9500 . ? C16 C17 1.491(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O3 1.276(4) . ? C17 C18 1.390(4) . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 O4 1.274(4) . ? C19 C20 1.482(4) . ? C20 C21 1.384(4) . ? C20 C25 1.389(4) . ? C21 C22 1.383(5) . ? C21 H21 0.9500 . ? C22 C23 1.374(5) . ? C22 H22 0.9500 . ? C23 C24 1.368(5) . ? C23 H23 0.9500 . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.428(7) . ? C26 C30 1.466(8) . ? C26 Cr2 2.204(4) . ? C26 H26 0.9500 . ? C27 C28 1.316(7) . ? C27 Cr2 2.208(4) . ? C27 H27 0.9500 . ? C28 C29 1.280(7) . ? C28 Cr2 2.198(4) . ? C28 H28 0.9500 . ? C29 C30 1.321(7) . ? C29 Cr2 2.213(4) . ? C29 H29 0.9500 . ? C30 Cr2 2.206(4) . ? C30 H30 0.9500 . ? O1 Cr1 1.929(2) . ? O2 Cr1 1.923(2) . ? O3 Cr2 1.933(2) . ? O4 Cr2 1.932(2) . ? Cr1 I1 2.6550(6) . ? Cr2 I2 2.6655(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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.1(3) . . ? O1 C2 C1 115.0(3) . . ? C3 C2 C1 120.0(3) . . ? C2 C3 C4 124.4(3) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? O2 C4 C3 123.6(3) . . ? O2 C4 C5 114.9(3) . . ? C3 C4 C5 121.5(3) . . ? C10 C5 C6 118.4(3) . . ? C10 C5 C4 118.6(3) . . ? C6 C5 C4 123.0(3) . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.7(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 120.6(3) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? C12 C11 C15 108.3(3) . . ? C12 C11 Cr1 71.87(19) . . ? C15 C11 Cr1 71.72(19) . . ? C12 C11 H11 125.9 . . ? C15 C11 H11 125.9 . . ? Cr1 C11 H11 122.2 . . ? C11 C12 C13 108.0(3) . . ? C11 C12 Cr1 71.81(19) . . ? C13 C12 Cr1 70.6(2) . . ? C11 C12 H12 126.0 . . ? C13 C12 H12 126.0 . . ? Cr1 C12 H12 123.2 . . ? C12 C13 C14 107.7(3) . . ? C12 C13 Cr1 72.68(19) . . ? C14 C13 Cr1 71.9(2) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? Cr1 C13 H13 121.0 . . ? C15 C14 C13 108.1(3) . . ? C15 C14 Cr1 72.34(19) . . ? C13 C14 Cr1 71.09(19) . . ? C15 C14 H14 125.9 . . ? C13 C14 H14 125.9 . . ? Cr1 C14 H14 122.3 . . ? C14 C15 C11 107.8(3) . . ? C14 C15 Cr1 71.2(2) . . ? C11 C15 Cr1 71.71(19) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Cr1 C15 H15 122.7 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 124.6(3) . . ? O3 C17 C16 116.2(3) . . ? C18 C17 C16 119.1(3) . . ? C19 C18 C17 124.6(3) . . ? C19 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? O4 C19 C18 124.2(3) . . ? O4 C19 C20 115.4(3) . . ? C18 C19 C20 120.3(3) . . ? C21 C20 C25 118.5(3) . . ? C21 C20 C19 122.5(3) . . ? C25 C20 C19 119.1(3) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 120.6(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? C27 C26 C30 101.9(4) . . ? C27 C26 Cr2 71.3(2) . . ? C30 C26 Cr2 70.6(2) . . ? C27 C26 H26 129.1 . . ? C30 C26 H26 129.1 . . ? Cr2 C26 H26 121.2 . . ? C28 C27 C26 108.7(4) . . ? C28 C27 Cr2 72.2(3) . . ? C26 C27 Cr2 71.0(2) . . ? C28 C27 H27 125.7 . . ? C26 C27 H27 125.7 . . ? Cr2 C27 H27 122.8 . . ? C29 C28 C27 110.8(5) . . ? C29 C28 Cr2 73.8(3) . . ? C27 C28 Cr2 73.0(3) . . ? C29 C28 H28 124.6 . . ? C27 C28 H28 124.6 . . ? Cr2 C28 H28 120.2 . . ? C28 C29 C30 112.2(5) . . ? C28 C29 Cr2 72.5(3) . . ? C30 C29 Cr2 72.3(3) . . ? C28 C29 H29 123.9 . . ? C30 C29 H29 123.9 . . ? Cr2 C29 H29 122.8 . . ? C29 C30 C26 106.4(4) . . ? C29 C30 Cr2 72.9(3) . . ? C26 C30 Cr2 70.5(2) . . ? C29 C30 H30 126.8 . . ? C26 C30 H30 126.8 . . ? Cr2 C30 H30 121.6 . . ? C2 O1 Cr1 127.03(19) . . ? C4 O2 Cr1 128.40(19) . . ? C17 O3 Cr2 127.2(2) . . ? C19 O4 Cr2 128.0(2) . . ? O2 Cr1 O1 91.04(9) . . ? O2 Cr1 C13 107.04(13) . . ? O1 Cr1 C13 97.25(12) . . ? O2 Cr1 C14 144.02(13) . . ? O1 Cr1 C14 93.51(12) . . ? C13 Cr1 C14 36.97(14) . . ? O2 Cr1 C15 144.44(11) . . ? O1 Cr1 C15 122.61(11) . . ? C13 Cr1 C15 61.34(14) . . ? C14 Cr1 C15 36.50(13) . . ? O2 Cr1 C11 107.88(11) . . ? O1 Cr1 C11 154.31(11) . . ? C13 Cr1 C11 61.14(13) . . ? C14 Cr1 C11 60.96(13) . . ? C15 Cr1 C11 36.56(12) . . ? O2 Cr1 C12 89.37(12) . . ? O1 Cr1 C12 130.57(12) . . ? C13 Cr1 C12 36.71(13) . . ? C14 Cr1 C12 61.11(13) . . ? C15 Cr1 C12 60.90(13) . . ? C11 Cr1 C12 36.32(13) . . ? O2 Cr1 I1 95.91(7) . . ? O1 Cr1 I1 95.99(7) . . ? C13 Cr1 I1 153.18(10) . . ? C14 Cr1 I1 119.00(11) . . ? C15 Cr1 I1 91.91(10) . . ? C11 Cr1 I1 99.06(9) . . ? C12 Cr1 I1 133.09(9) . . ? O4 Cr2 O3 91.05(9) . . ? O4 Cr2 C28 100.89(17) . . ? O3 Cr2 C28 103.34(17) . . ? O4 Cr2 C26 119.2(2) . . ? O3 Cr2 C26 147.06(19) . . ? C28 Cr2 C26 60.86(19) . . ? O4 Cr2 C30 154.06(14) . . ? O3 Cr2 C30 108.40(18) . . ? C28 Cr2 C30 58.73(19) . . ? C26 Cr2 C30 38.8(2) . . ? O4 Cr2 C27 92.85(14) . . ? O3 Cr2 C27 137.71(17) . . ? C28 Cr2 C27 34.74(18) . . ? C26 Cr2 C27 37.77(19) . . ? C30 Cr2 C27 61.21(17) . . ? O4 Cr2 C29 132.61(18) . . ? O3 Cr2 C29 89.79(16) . . ? C28 Cr2 C29 33.73(18) . . ? C26 Cr2 C29 60.72(19) . . ? C30 Cr2 C29 34.80(19) . . ? C27 Cr2 C29 57.79(18) . . ? O4 Cr2 I2 96.46(7) . . ? O3 Cr2 I2 97.00(7) . . ? C28 Cr2 I2 152.86(14) . . ? C26 Cr2 I2 92.44(13) . . ? C30 Cr2 I2 97.94(16) . . ? C27 Cr2 I2 124.26(16) . . ? C29 Cr2 I2 130.41(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C4 -0.2(5) . . . . ? C1 C2 C3 C4 -179.8(3) . . . . ? C2 C3 C4 O2 -0.4(5) . . . . ? C2 C3 C4 C5 -180.0(3) . . . . ? O2 C4 C5 C10 21.2(4) . . . . ? C3 C4 C5 C10 -159.2(3) . . . . ? O2 C4 C5 C6 -158.5(3) . . . . ? C3 C4 C5 C6 21.1(4) . . . . ? C10 C5 C6 C7 -1.2(5) . . . . ? C4 C5 C6 C7 178.5(3) . . . . ? C5 C6 C7 C8 1.7(5) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C8 C9 C10 C5 1.6(5) . . . . ? C6 C5 C10 C9 -0.4(5) . . . . ? C4 C5 C10 C9 179.8(3) . . . . ? C15 C11 C12 C13 1.2(4) . . . . ? Cr1 C11 C12 C13 -61.7(2) . . . . ? C15 C11 C12 Cr1 62.9(2) . . . . ? C11 C12 C13 C14 -1.4(4) . . . . ? Cr1 C12 C13 C14 -63.8(3) . . . . ? C11 C12 C13 Cr1 62.4(2) . . . . ? C12 C13 C14 C15 1.1(4) . . . . ? Cr1 C13 C14 C15 -63.3(3) . . . . ? C12 C13 C14 Cr1 64.3(2) . . . . ? C13 C14 C15 C11 -0.3(4) . . . . ? Cr1 C14 C15 C11 -62.8(2) . . . . ? C13 C14 C15 Cr1 62.5(2) . . . . ? C12 C11 C15 C14 -0.6(4) . . . . ? Cr1 C11 C15 C14 62.4(2) . . . . ? C12 C11 C15 Cr1 -63.0(2) . . . . ? O3 C17 C18 C19 4.5(5) . . . . ? C16 C17 C18 C19 -175.0(3) . . . . ? C17 C18 C19 O4 0.3(5) . . . . ? C17 C18 C19 C20 179.1(3) . . . . ? O4 C19 C20 C21 -164.7(3) . . . . ? C18 C19 C20 C21 16.5(5) . . . . ? O4 C19 C20 C25 13.9(4) . . . . ? C18 C19 C20 C25 -164.9(3) . . . . ? C25 C20 C21 C22 0.5(5) . . . . ? C19 C20 C21 C22 179.1(3) . . . . ? C20 C21 C22 C23 -0.4(6) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 0.1(6) . . . . ? C23 C24 C25 C20 0.0(5) . . . . ? C21 C20 C25 C24 -0.3(5) . . . . ? C19 C20 C25 C24 -179.0(3) . . . . ? C30 C26 C27 C28 1.8(5) . . . . ? Cr2 C26 C27 C28 -62.8(3) . . . . ? C30 C26 C27 Cr2 64.6(3) . . . . ? C26 C27 C28 C29 -2.6(5) . . . . ? Cr2 C27 C28 C29 -64.6(4) . . . . ? C26 C27 C28 Cr2 62.0(3) . . . . ? C27 C28 C29 C30 2.4(6) . . . . ? Cr2 C28 C29 C30 -61.8(4) . . . . ? C27 C28 C29 Cr2 64.2(3) . . . . ? C28 C29 C30 C26 -1.1(5) . . . . ? Cr2 C29 C30 C26 -63.0(3) . . . . ? C28 C29 C30 Cr2 61.9(4) . . . . ? C27 C26 C30 C29 -0.4(4) . . . . ? Cr2 C26 C30 C29 64.6(3) . . . . ? C27 C26 C30 Cr2 -65.0(3) . . . . ? C3 C2 O1 Cr1 -4.1(4) . . . . ? C1 C2 O1 Cr1 175.6(2) . . . . ? C3 C4 O2 Cr1 5.3(4) . . . . ? C5 C4 O2 Cr1 -175.10(19) . . . . ? C18 C17 O3 Cr2 -7.5(5) . . . . ? C16 C17 O3 Cr2 172.0(2) . . . . ? C18 C19 O4 Cr2 -1.7(5) . . . . ? C20 C19 O4 Cr2 179.5(2) . . . . ? C4 O2 Cr1 O1 -6.9(3) . . . . ? C4 O2 Cr1 C13 91.0(3) . . . . ? C4 O2 Cr1 C14 90.5(3) . . . . ? C4 O2 Cr1 C15 155.3(3) . . . . ? C4 O2 Cr1 C11 155.4(2) . . . . ? C4 O2 Cr1 C12 123.6(3) . . . . ? C4 O2 Cr1 I1 -103.1(2) . . . . ? C2 O1 Cr1 O2 6.2(3) . . . . ? C2 O1 Cr1 C13 -101.1(3) . . . . ? C2 O1 Cr1 C14 -138.1(3) . . . . ? C2 O1 Cr1 C15 -161.6(2) . . . . ? C2 O1 Cr1 C11 -132.0(3) . . . . ? C2 O1 Cr1 C12 -83.8(3) . . . . ? C2 O1 Cr1 I1 102.3(2) . . . . ? C12 C13 Cr1 O2 64.5(2) . . . . ? C14 C13 Cr1 O2 -179.5(2) . . . . ? C12 C13 Cr1 O1 157.9(2) . . . . ? C14 C13 Cr1 O1 -86.2(2) . . . . ? C12 C13 Cr1 C14 -116.0(3) . . . . ? C12 C13 Cr1 C15 -78.8(2) . . . . ? C14 C13 Cr1 C15 37.1(2) . . . . ? C12 C13 Cr1 C11 -36.9(2) . . . . ? C14 C13 Cr1 C11 79.1(2) . . . . ? C14 C13 Cr1 C12 116.0(3) . . . . ? C12 C13 Cr1 I1 -83.1(3) . . . . ? C14 C13 Cr1 I1 32.8(4) . . . . ? C15 C14 Cr1 O2 117.8(2) . . . . ? C13 C14 Cr1 O2 0.8(3) . . . . ? C15 C14 Cr1 O1 -145.6(2) . . . . ? C13 C14 Cr1 O1 97.4(2) . . . . ? C15 C14 Cr1 C13 117.0(3) . . . . ? C13 C14 Cr1 C15 -117.0(3) . . . . ? C15 C14 Cr1 C11 37.4(2) . . . . ? C13 C14 Cr1 C11 -79.6(2) . . . . ? C15 C14 Cr1 C12 79.2(2) . . . . ? C13 C14 Cr1 C12 -37.9(2) . . . . ? C15 C14 Cr1 I1 -46.7(2) . . . . ? C13 C14 Cr1 I1 -163.77(18) . . . . ? C14 C15 Cr1 O2 -116.7(2) . . . . ? C11 C15 Cr1 O2 0.2(3) . . . . ? C14 C15 Cr1 O1 42.1(3) . . . . ? C11 C15 Cr1 O1 158.95(19) . . . . ? C14 C15 Cr1 C13 -37.6(2) . . . . ? C11 C15 Cr1 C13 79.3(2) . . . . ? C11 C15 Cr1 C14 116.9(3) . . . . ? C14 C15 Cr1 C11 -116.9(3) . . . . ? C14 C15 Cr1 C12 -79.8(2) . . . . ? C11 C15 Cr1 C12 37.1(2) . . . . ? C14 C15 Cr1 I1 140.4(2) . . . . ? C11 C15 Cr1 I1 -102.7(2) . . . . ? C12 C11 Cr1 O2 -62.7(2) . . . . ? C15 C11 Cr1 O2 -179.9(2) . . . . ? C12 C11 Cr1 O1 72.9(3) . . . . ? C15 C11 Cr1 O1 -44.3(4) . . . . ? C12 C11 Cr1 C13 37.3(2) . . . . ? C15 C11 Cr1 C13 -79.8(2) . . . . ? C12 C11 Cr1 C14 79.8(2) . . . . ? C15 C11 Cr1 C14 -37.4(2) . . . . ? C12 C11 Cr1 C15 117.1(3) . . . . ? C15 C11 Cr1 C12 -117.1(3) . . . . ? C12 C11 Cr1 I1 -162.00(19) . . . . ? C15 C11 Cr1 I1 80.9(2) . . . . ? C11 C12 Cr1 O2 122.2(2) . . . . ? C13 C12 Cr1 O2 -120.3(2) . . . . ? C11 C12 Cr1 O1 -146.95(19) . . . . ? C13 C12 Cr1 O1 -29.5(3) . . . . ? C11 C12 Cr1 C13 -117.5(3) . . . . ? C11 C12 Cr1 C14 -79.3(2) . . . . ? C13 C12 Cr1 C14 38.1(2) . . . . ? C11 C12 Cr1 C15 -37.4(2) . . . . ? C13 C12 Cr1 C15 80.1(2) . . . . ? C13 C12 Cr1 C11 117.5(3) . . . . ? C11 C12 Cr1 I1 24.7(3) . . . . ? C13 C12 Cr1 I1 142.16(19) . . . . ? C19 O4 Cr2 O3 -0.5(3) . . . . ? C19 O4 Cr2 C28 103.3(3) . . . . ? C19 O4 Cr2 C26 165.9(3) . . . . ? C19 O4 Cr2 C30 138.9(5) . . . . ? C19 O4 Cr2 C27 137.4(3) . . . . ? C19 O4 Cr2 C29 90.2(3) . . . . ? C19 O4 Cr2 I2 -97.7(3) . . . . ? C17 O3 Cr2 O4 5.0(3) . . . . ? C17 O3 Cr2 C28 -96.4(3) . . . . ? C17 O3 Cr2 C26 -152.8(4) . . . . ? C17 O3 Cr2 C30 -157.5(3) . . . . ? C17 O3 Cr2 C27 -90.4(3) . . . . ? C17 O3 Cr2 C29 -127.6(3) . . . . ? C17 O3 Cr2 I2 101.6(2) . . . . ? C29 C28 Cr2 O4 -162.5(3) . . . . ? C27 C28 Cr2 O4 79.1(3) . . . . ? C29 C28 Cr2 O3 -68.8(4) . . . . ? C27 C28 Cr2 O3 172.9(3) . . . . ? C29 C28 Cr2 C26 80.0(4) . . . . ? C27 C28 Cr2 C26 -38.4(3) . . . . ? C29 C28 Cr2 C30 34.9(4) . . . . ? C27 C28 Cr2 C30 -83.5(4) . . . . ? C29 C28 Cr2 C27 118.4(5) . . . . ? C27 C28 Cr2 C29 -118.4(5) . . . . ? C29 C28 Cr2 I2 68.7(5) . . . . ? C27 C28 Cr2 I2 -49.7(6) . . . . ? C27 C26 Cr2 O4 -51.1(3) . . . . ? C30 C26 Cr2 O4 -161.6(3) . . . . ? C27 C26 Cr2 O3 103.3(5) . . . . ? C30 C26 Cr2 O3 -7.2(5) . . . . ? C27 C26 Cr2 C28 35.3(3) . . . . ? C30 C26 Cr2 C28 -75.2(3) . . . . ? C27 C26 Cr2 C30 110.5(4) . . . . ? C30 C26 Cr2 C27 -110.5(4) . . . . ? C27 C26 Cr2 C29 74.1(3) . . . . ? C30 C26 Cr2 C29 -36.4(3) . . . . ? C27 C26 Cr2 I2 -149.9(3) . . . . ? C30 C26 Cr2 I2 99.7(3) . . . . ? C29 C30 Cr2 O4 -75.8(6) . . . . ? C26 C30 Cr2 O4 39.1(7) . . . . ? C29 C30 Cr2 O3 60.9(4) . . . . ? C26 C30 Cr2 O3 175.9(3) . . . . ? C29 C30 Cr2 C28 -33.8(3) . . . . ? C26 C30 Cr2 C28 81.1(3) . . . . ? C29 C30 Cr2 C26 -114.9(4) . . . . ? C29 C30 Cr2 C27 -74.0(3) . . . . ? C26 C30 Cr2 C27 40.9(3) . . . . ? C26 C30 Cr2 C29 114.9(4) . . . . ? C29 C30 Cr2 I2 161.1(3) . . . . ? C26 C30 Cr2 I2 -84.0(3) . . . . ? C28 C27 Cr2 O4 -105.1(3) . . . . ? C26 C27 Cr2 O4 137.2(3) . . . . ? C28 C27 Cr2 O3 -10.4(4) . . . . ? C26 C27 Cr2 O3 -128.1(3) . . . . ? C26 C27 Cr2 C28 -117.8(4) . . . . ? C28 C27 Cr2 C26 117.8(4) . . . . ? C28 C27 Cr2 C30 75.7(4) . . . . ? C26 C27 Cr2 C30 -42.1(3) . . . . ? C28 C27 Cr2 C29 35.3(3) . . . . ? C26 C27 Cr2 C29 -82.5(3) . . . . ? C28 C27 Cr2 I2 155.1(3) . . . . ? C26 C27 Cr2 I2 37.4(4) . . . . ? C28 C29 Cr2 O4 23.7(5) . . . . ? C30 C29 Cr2 O4 144.8(3) . . . . ? C28 C29 Cr2 O3 114.9(4) . . . . ? C30 C29 Cr2 O3 -124.0(3) . . . . ? C30 C29 Cr2 C28 121.1(5) . . . . ? C28 C29 Cr2 C26 -80.5(4) . . . . ? C30 C29 Cr2 C26 40.7(3) . . . . ? C28 C29 Cr2 C30 -121.1(5) . . . . ? C28 C29 Cr2 C27 -36.3(3) . . . . ? C30 C29 Cr2 C27 84.8(4) . . . . ? C28 C29 Cr2 I2 -146.1(3) . . . . ? C30 C29 Cr2 I2 -24.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.685 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.093 data_6b_CpCr(C6H4CHNDpp)I _database_code_depnum_ccdc_archive 'CCDC 791386' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H27 Cr I N O' _chemical_formula_weight 524.37 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' Cr Cr 0.3209 0.6236 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9810(8) _cell_length_b 10.4430(9) _cell_length_c 12.6068(11) _cell_angle_alpha 92.002(4) _cell_angle_beta 107.735(4) _cell_angle_gamma 91.342(5) _cell_volume 1124.77(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8568 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.94 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8161 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.94 _reflns_number_total 8161 _reflns_number_gt 7372 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.8449P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8161 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 C1 C 0.6602(3) 0.0704(2) 0.31366(19) 0.0176(5) Uani 1 1 d . . . C2 C 0.5797(3) -0.0278(3) 0.3494(2) 0.0245(5) Uani 1 1 d . . . H2 H 0.4869 -0.0661 0.2990 0.029 Uiso 1 1 calc R . . C3 C 0.6339(3) -0.0695(3) 0.4568(2) 0.0287(6) Uani 1 1 d . . . H3 H 0.5784 -0.1369 0.4788 0.034 Uiso 1 1 calc R . . C4 C 0.7685(3) -0.0142(3) 0.5333(2) 0.0282(6) Uani 1 1 d . . . H4 H 0.8060 -0.0447 0.6065 0.034 Uiso 1 1 calc R . . C5 C 0.8461(3) 0.0848(3) 0.5016(2) 0.0231(5) Uani 1 1 d . . . H5 H 0.9351 0.1253 0.5546 0.028 Uiso 1 1 calc R . . C6 C 0.7965(3) 0.1280(2) 0.3917(2) 0.0186(5) Uani 1 1 d . . . C7 C 0.8775(3) 0.2363(2) 0.3664(2) 0.0178(5) Uani 1 1 d . . . H7 H 0.9518 0.2807 0.4276 0.021 Uiso 1 1 calc R . . C8 C 0.9286(3) 0.4067(2) 0.26679(19) 0.0162(5) Uani 1 1 d . . . C9 C 1.0630(3) 0.4208(3) 0.2332(2) 0.0200(5) Uani 1 1 d . . . C10 C 1.1219(3) 0.5447(3) 0.2309(2) 0.0255(6) Uani 1 1 d . . . H10 H 1.2128 0.5567 0.2083 0.031 Uiso 1 1 calc R . . C11 C 1.0523(3) 0.6502(3) 0.2602(2) 0.0279(6) Uani 1 1 d . . . H11 H 1.0962 0.7337 0.2595 0.033 Uiso 1 1 calc R . . C12 C 0.9181(3) 0.6342(3) 0.2906(2) 0.0261(6) Uani 1 1 d . . . H12 H 0.8690 0.7076 0.3092 0.031 Uiso 1 1 calc R . . C13 C 0.8531(3) 0.5128(2) 0.2946(2) 0.0187(5) Uani 1 1 d . . . C14 C 1.1441(3) 0.3080(3) 0.2014(3) 0.0303(6) Uani 1 1 d . . . H14 H 1.0714 0.2312 0.1899 0.036 Uiso 1 1 calc R . . C15 C 1.1837(5) 0.3260(4) 0.0925(3) 0.0493(9) Uani 1 1 d . . . H15A H 1.0924 0.3578 0.0362 0.074 Uiso 1 1 calc R . . H15B H 1.2121 0.2437 0.0658 0.074 Uiso 1 1 calc R . . H15C H 1.2717 0.3881 0.1061 0.074 Uiso 1 1 calc R . . C16 C 1.2927(4) 0.2804(3) 0.2947(3) 0.0444(8) Uani 1 1 d . . . H16A H 1.3667 0.3539 0.3073 0.067 Uiso 1 1 calc R . . H16B H 1.3402 0.2040 0.2735 0.067 Uiso 1 1 calc R . . H16C H 1.2664 0.2654 0.3633 0.067 Uiso 1 1 calc R . . C17 C 0.7040(3) 0.5001(3) 0.3289(2) 0.0229(5) Uani 1 1 d . . . H17 H 0.6578 0.4116 0.3061 0.028 Uiso 1 1 calc R . . C18 C 0.5823(3) 0.5949(3) 0.2722(3) 0.0365(7) Uani 1 1 d . . . H18A H 0.6212 0.6824 0.2988 0.055 Uiso 1 1 calc R . . H18B H 0.4851 0.5770 0.2900 0.055 Uiso 1 1 calc R . . H18C H 0.5620 0.5865 0.1914 0.055 Uiso 1 1 calc R . . C19 C 0.7415(4) 0.5171(4) 0.4550(3) 0.0435(8) Uani 1 1 d . . . H19A H 0.7832 0.6045 0.4791 0.065 Uiso 1 1 calc R . . H19B H 0.8194 0.4554 0.4913 0.065 Uiso 1 1 calc R . . H19C H 0.6459 0.5024 0.4756 0.065 Uiso 1 1 calc R . . C20 C 0.6125(4) 0.1424(3) -0.0560(2) 0.0353(7) Uani 1 1 d . . . H20 H 0.5917 0.0580 -0.0888 0.042 Uiso 1 1 calc R . . C21 C 0.7516(4) 0.2176(3) -0.0409(2) 0.0332(7) Uani 1 1 d . . . H21 H 0.8399 0.1932 -0.0623 0.040 Uiso 1 1 calc R . . C22 C 0.7350(4) 0.3337(3) 0.0111(2) 0.0325(7) Uani 1 1 d . . . H22 H 0.8099 0.4032 0.0310 0.039 Uiso 1 1 calc R . . C23 C 0.5877(4) 0.3300(3) 0.0291(2) 0.0339(7) Uani 1 1 d . . . H23 H 0.5469 0.3959 0.0650 0.041 Uiso 1 1 calc R . . C24 C 0.5122(4) 0.2131(3) -0.0148(2) 0.0368(8) Uani 1 1 d . . . H24 H 0.4097 0.1866 -0.0162 0.044 Uiso 1 1 calc R . . N1 N 0.8602(2) 0.28051(19) 0.26857(16) 0.0153(4) Uani 1 1 d . . . O1 O 0.6039(2) 0.10916(18) 0.21083(13) 0.0204(4) Uani 1 1 d . . . Cr1 Cr 0.72817(4) 0.17898(4) 0.12739(3) 0.01598(9) Uani 1 1 d . . . I1 I 0.90765(2) -0.024061(17) 0.150703(14) 0.02560(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0196(12) 0.0174(12) 0.0172(12) 0.0000(9) 0.0080(10) -0.0001(9) C2 0.0251(13) 0.0250(13) 0.0225(12) -0.0006(11) 0.0070(11) -0.0090(12) C3 0.0357(15) 0.0278(15) 0.0256(14) 0.0065(11) 0.0139(13) -0.0061(12) C4 0.0323(14) 0.0312(15) 0.0216(13) 0.0072(11) 0.0084(11) -0.0011(12) C5 0.0263(13) 0.0238(14) 0.0176(12) 0.0009(10) 0.0047(11) -0.0029(11) C6 0.0198(12) 0.0181(12) 0.0182(12) 0.0018(9) 0.0064(10) -0.0001(10) C7 0.0144(11) 0.0183(12) 0.0204(12) -0.0020(9) 0.0050(10) 0.0003(9) C8 0.0175(12) 0.0138(11) 0.0154(11) -0.0004(8) 0.0025(10) -0.0018(9) C9 0.0201(12) 0.0192(13) 0.0216(12) -0.0011(9) 0.0079(10) -0.0024(10) C10 0.0232(13) 0.0238(15) 0.0301(15) 0.0029(11) 0.0095(12) -0.0060(11) C11 0.0296(14) 0.0173(13) 0.0359(15) 0.0045(11) 0.0089(13) -0.0045(11) C12 0.0270(14) 0.0167(13) 0.0315(15) -0.0005(10) 0.0043(12) 0.0015(11) C13 0.0180(12) 0.0179(12) 0.0170(12) 0.0004(9) 0.0006(10) 0.0000(10) C14 0.0289(15) 0.0206(14) 0.0482(18) -0.0072(12) 0.0232(14) -0.0058(11) C15 0.053(2) 0.057(2) 0.046(2) -0.0163(16) 0.0302(18) -0.0027(18) C16 0.0470(19) 0.0320(18) 0.063(2) 0.0140(15) 0.0271(18) 0.0191(15) C17 0.0192(13) 0.0213(14) 0.0270(14) -0.0019(10) 0.0055(11) 0.0011(10) C18 0.0267(15) 0.0327(17) 0.0473(19) 0.0014(14) 0.0066(14) 0.0078(13) C19 0.0321(17) 0.069(3) 0.0323(18) 0.0011(15) 0.0141(15) 0.0101(17) C20 0.057(2) 0.0274(15) 0.0133(13) 0.0013(10) -0.0009(13) -0.0102(14) C21 0.0408(17) 0.0452(19) 0.0186(13) 0.0124(12) 0.0146(13) 0.0097(14) C22 0.0417(17) 0.0277(15) 0.0209(14) 0.0124(11) -0.0017(13) -0.0121(13) C23 0.0443(18) 0.0324(17) 0.0228(14) 0.0096(12) 0.0051(13) 0.0170(14) C24 0.0270(15) 0.051(2) 0.0268(16) 0.0164(14) -0.0012(13) -0.0028(14) N1 0.0156(9) 0.0139(10) 0.0170(10) -0.0005(7) 0.0059(8) 0.0003(8) O1 0.0192(8) 0.0245(10) 0.0165(8) 0.0022(7) 0.0042(7) -0.0043(7) Cr1 0.0196(2) 0.01398(19) 0.01388(19) 0.00091(14) 0.00450(16) -0.00130(15) I1 0.03118(10) 0.01722(8) 0.02835(9) -0.00187(7) 0.00907(7) 0.00457(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.322(3) . ? C1 C2 1.405(3) . ? C1 C6 1.420(3) . ? C2 C3 1.382(4) . ? C2 H2 0.9500 . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 C6 1.413(3) . ? C5 H5 0.9500 . ? C6 C7 1.428(3) . ? C7 N1 1.298(3) . ? C7 H7 0.9500 . ? C8 C13 1.401(3) . ? C8 C9 1.402(3) . ? C8 N1 1.445(3) . ? C9 C10 1.391(4) . ? C9 C14 1.505(4) . ? C10 C11 1.373(4) . ? C10 H10 0.9500 . ? C11 C12 1.379(4) . ? C11 H11 0.9500 . ? C12 C13 1.393(4) . ? C12 H12 0.9500 . ? C13 C17 1.531(4) . ? C14 C16 1.527(4) . ? C14 C15 1.535(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.521(4) . ? C17 C19 1.524(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C24 1.384(5) . ? C20 C21 1.419(4) . ? C20 Cr1 2.242(3) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 Cr1 2.244(3) . ? C21 H21 0.9500 . ? C22 C23 1.409(5) . ? C22 Cr1 2.231(3) . ? C22 H22 0.9500 . ? C23 C24 1.394(5) . ? C23 Cr1 2.212(3) . ? C23 H23 0.9500 . ? C24 Cr1 2.249(3) . ? C24 H24 0.9500 . ? N1 Cr1 2.055(2) . ? O1 Cr1 1.9014(18) . ? Cr1 I1 2.6637(5) . ? 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 C1 C2 119.2(2) . . ? O1 C1 C6 122.5(2) . . ? C2 C1 C6 118.2(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.4(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.3(2) . . ? C5 C6 C7 118.2(2) . . ? C1 C6 C7 122.2(2) . . ? N1 C7 C6 126.8(2) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? C13 C8 C9 121.8(2) . . ? C13 C8 N1 118.2(2) . . ? C9 C8 N1 120.0(2) . . ? C10 C9 C8 117.5(2) . . ? C10 C9 C14 120.0(2) . . ? C8 C9 C14 122.5(2) . . ? C11 C10 C9 121.9(2) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 121.4(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 117.8(2) . . ? C12 C13 C17 119.4(2) . . ? C8 C13 C17 122.8(2) . . ? C9 C14 C16 111.1(2) . . ? C9 C14 C15 112.6(3) . . ? C16 C14 C15 109.7(3) . . ? C9 C14 H14 107.7 . . ? C16 C14 H14 107.7 . . ? C15 C14 H14 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 109.7(3) . . ? C18 C17 C13 112.3(2) . . ? C19 C17 C13 110.8(2) . . ? C18 C17 H17 108.0 . . ? C19 C17 H17 108.0 . . ? C13 C17 H17 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C24 C20 C21 108.3(3) . . ? C24 C20 Cr1 72.34(16) . . ? C21 C20 Cr1 71.63(15) . . ? C24 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? Cr1 C20 H20 121.9 . . ? C22 C21 C20 107.5(3) . . ? C22 C21 Cr1 71.42(15) . . ? C20 C21 Cr1 71.50(15) . . ? C22 C21 H21 126.3 . . ? C20 C21 H21 126.3 . . ? Cr1 C21 H21 122.5 . . ? C21 C22 C23 107.9(3) . . ? C21 C22 Cr1 72.39(16) . . ? C23 C22 Cr1 70.76(16) . . ? C21 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? Cr1 C22 H22 122.5 . . ? C24 C23 C22 108.2(3) . . ? C24 C23 Cr1 73.28(18) . . ? C22 C23 Cr1 72.27(16) . . ? C24 C23 H23 125.9 . . ? C22 C23 H23 125.9 . . ? Cr1 C23 H23 120.3 . . ? C20 C24 C23 108.1(3) . . ? C20 C24 Cr1 71.77(16) . . ? C23 C24 Cr1 70.33(16) . . ? C20 C24 H24 125.9 . . ? C23 C24 H24 125.9 . . ? Cr1 C24 H24 123.6 . . ? C7 N1 C8 116.1(2) . . ? C7 N1 Cr1 120.47(17) . . ? C8 N1 Cr1 123.25(15) . . ? C1 O1 Cr1 124.36(15) . . ? O1 Cr1 N1 89.19(8) . . ? O1 Cr1 C23 105.62(10) . . ? N1 Cr1 C23 102.22(10) . . ? O1 Cr1 C22 142.38(11) . . ? N1 Cr1 C22 95.25(9) . . ? C23 Cr1 C22 36.97(12) . . ? O1 Cr1 C20 110.88(10) . . ? N1 Cr1 C20 155.97(10) . . ? C23 Cr1 C20 60.65(12) . . ? C22 Cr1 C20 60.83(11) . . ? O1 Cr1 C21 147.64(10) . . ? N1 Cr1 C21 121.50(10) . . ? C23 Cr1 C21 61.05(12) . . ? C22 Cr1 C21 36.20(12) . . ? C20 Cr1 C21 36.87(11) . . ? O1 Cr1 C24 90.68(10) . . ? N1 Cr1 C24 136.10(11) . . ? C23 Cr1 C24 36.39(12) . . ? C22 Cr1 C24 60.87(11) . . ? C20 Cr1 C24 35.89(12) . . ? C21 Cr1 C24 60.73(11) . . ? O1 Cr1 I1 93.43(6) . . ? N1 Cr1 I1 96.86(6) . . ? C23 Cr1 I1 153.03(8) . . ? C22 Cr1 I1 122.87(9) . . ? C20 Cr1 I1 95.01(9) . . ? C21 Cr1 I1 92.72(8) . . ? C24 Cr1 I1 126.94(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.0(2) . . . . ? C6 C1 C2 C3 -1.5(4) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C6 -2.9(4) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? C4 C5 C6 C7 176.4(3) . . . . ? O1 C1 C6 C5 177.4(2) . . . . ? C2 C1 C6 C5 0.0(4) . . . . ? O1 C1 C6 C7 3.4(4) . . . . ? C2 C1 C6 C7 -174.0(3) . . . . ? C5 C6 C7 N1 171.9(2) . . . . ? C1 C6 C7 N1 -14.1(4) . . . . ? C13 C8 C9 C10 1.5(3) . . . . ? N1 C8 C9 C10 178.7(2) . . . . ? C13 C8 C9 C14 -179.1(2) . . . . ? N1 C8 C9 C14 -1.9(4) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C14 C9 C10 C11 -179.4(3) . . . . ? C9 C10 C11 C12 -1.5(4) . . . . ? C10 C11 C12 C13 1.4(4) . . . . ? C11 C12 C13 C8 0.1(4) . . . . ? C11 C12 C13 C17 179.9(2) . . . . ? C9 C8 C13 C12 -1.6(4) . . . . ? N1 C8 C13 C12 -178.8(2) . . . . ? C9 C8 C13 C17 178.6(2) . . . . ? N1 C8 C13 C17 1.4(3) . . . . ? C10 C9 C14 C16 76.1(3) . . . . ? C8 C9 C14 C16 -103.3(3) . . . . ? C10 C9 C14 C15 -47.4(4) . . . . ? C8 C9 C14 C15 133.2(3) . . . . ? C12 C13 C17 C18 44.8(3) . . . . ? C8 C13 C17 C18 -135.4(3) . . . . ? C12 C13 C17 C19 -78.3(3) . . . . ? C8 C13 C17 C19 101.6(3) . . . . ? C24 C20 C21 C22 0.7(3) . . . . ? Cr1 C20 C21 C22 -62.77(19) . . . . ? C24 C20 C21 Cr1 63.49(19) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? Cr1 C21 C22 C23 -62.24(18) . . . . ? C20 C21 C22 Cr1 62.83(19) . . . . ? C21 C22 C23 C24 -1.7(3) . . . . ? Cr1 C22 C23 C24 -65.0(2) . . . . ? C21 C22 C23 Cr1 63.29(19) . . . . ? C21 C20 C24 C23 -1.8(3) . . . . ? Cr1 C20 C24 C23 61.26(19) . . . . ? C21 C20 C24 Cr1 -63.03(19) . . . . ? C22 C23 C24 C20 2.1(3) . . . . ? Cr1 C23 C24 C20 -62.2(2) . . . . ? C22 C23 C24 Cr1 64.32(19) . . . . ? C6 C7 N1 C8 166.6(2) . . . . ? C6 C7 N1 Cr1 -9.0(3) . . . . ? C13 C8 N1 C7 -74.8(3) . . . . ? C9 C8 N1 C7 108.0(3) . . . . ? C13 C8 N1 Cr1 100.7(2) . . . . ? C9 C8 N1 Cr1 -76.6(3) . . . . ? C2 C1 O1 Cr1 -151.2(2) . . . . ? C6 C1 O1 Cr1 31.4(3) . . . . ? C1 O1 Cr1 N1 -41.1(2) . . . . ? C1 O1 Cr1 C23 -143.5(2) . . . . ? C1 O1 Cr1 C22 -138.6(2) . . . . ? C1 O1 Cr1 C20 152.5(2) . . . . ? C1 O1 Cr1 C21 156.4(2) . . . . ? C1 O1 Cr1 C24 -177.2(2) . . . . ? C1 O1 Cr1 I1 55.77(19) . . . . ? C7 N1 Cr1 O1 29.47(19) . . . . ? C8 N1 Cr1 O1 -145.80(19) . . . . ? C7 N1 Cr1 C23 135.3(2) . . . . ? C8 N1 Cr1 C23 -40.0(2) . . . . ? C7 N1 Cr1 C22 172.1(2) . . . . ? C8 N1 Cr1 C22 -3.2(2) . . . . ? C7 N1 Cr1 C20 177.0(3) . . . . ? C8 N1 Cr1 C20 1.8(4) . . . . ? C7 N1 Cr1 C21 -161.35(19) . . . . ? C8 N1 Cr1 C21 23.4(2) . . . . ? C7 N1 Cr1 C24 119.6(2) . . . . ? C8 N1 Cr1 C24 -55.7(2) . . . . ? C7 N1 Cr1 I1 -63.89(19) . . . . ? C8 N1 Cr1 I1 120.84(17) . . . . ? C24 C23 Cr1 O1 -69.0(2) . . . . ? C22 C23 Cr1 O1 175.02(16) . . . . ? C24 C23 Cr1 N1 -161.61(18) . . . . ? C22 C23 Cr1 N1 82.41(18) . . . . ? C24 C23 Cr1 C22 116.0(3) . . . . ? C24 C23 Cr1 C20 36.52(19) . . . . ? C22 C23 Cr1 C20 -79.47(19) . . . . ? C24 C23 Cr1 C21 79.0(2) . . . . ? C22 C23 Cr1 C21 -37.01(18) . . . . ? C22 C23 Cr1 C24 -116.0(3) . . . . ? C24 C23 Cr1 I1 64.4(3) . . . . ? C22 C23 Cr1 I1 -51.6(3) . . . . ? C21 C22 Cr1 O1 -124.8(2) . . . . ? C23 C22 Cr1 O1 -7.9(3) . . . . ? C21 C22 Cr1 N1 139.73(18) . . . . ? C23 C22 Cr1 N1 -103.38(18) . . . . ? C21 C22 Cr1 C23 -116.9(3) . . . . ? C21 C22 Cr1 C20 -37.95(18) . . . . ? C23 C22 Cr1 C20 78.9(2) . . . . ? C23 C22 Cr1 C21 116.9(3) . . . . ? C21 C22 Cr1 C24 -79.3(2) . . . . ? C23 C22 Cr1 C24 37.63(18) . . . . ? C21 C22 Cr1 I1 38.1(2) . . . . ? C23 C22 Cr1 I1 154.96(15) . . . . ? C24 C20 Cr1 O1 59.6(2) . . . . ? C21 C20 Cr1 O1 176.53(17) . . . . ? C24 C20 Cr1 N1 -85.3(3) . . . . ? C21 C20 Cr1 N1 31.6(4) . . . . ? C24 C20 Cr1 C23 -37.03(19) . . . . ? C21 C20 Cr1 C23 79.9(2) . . . . ? C24 C20 Cr1 C22 -79.7(2) . . . . ? C21 C20 Cr1 C22 37.25(19) . . . . ? C24 C20 Cr1 C21 -116.9(3) . . . . ? C21 C20 Cr1 C24 116.9(3) . . . . ? C24 C20 Cr1 I1 155.24(18) . . . . ? C21 C20 Cr1 I1 -87.86(18) . . . . ? C22 C21 Cr1 O1 110.4(2) . . . . ? C20 C21 Cr1 O1 -6.1(3) . . . . ? C22 C21 Cr1 N1 -49.0(2) . . . . ? C20 C21 Cr1 N1 -165.52(18) . . . . ? C22 C21 Cr1 C23 37.81(18) . . . . ? C20 C21 Cr1 C23 -78.7(2) . . . . ? C20 C21 Cr1 C22 -116.5(3) . . . . ? C22 C21 Cr1 C20 116.5(3) . . . . ? C22 C21 Cr1 C24 79.7(2) . . . . ? C20 C21 Cr1 C24 -36.82(19) . . . . ? C22 C21 Cr1 I1 -148.77(17) . . . . ? C20 C21 Cr1 I1 94.72(18) . . . . ? C20 C24 Cr1 O1 -126.28(19) . . . . ? C23 C24 Cr1 O1 115.95(19) . . . . ? C20 C24 Cr1 N1 144.18(17) . . . . ? C23 C24 Cr1 N1 26.4(3) . . . . ? C20 C24 Cr1 C23 117.8(3) . . . . ? C20 C24 Cr1 C22 79.5(2) . . . . ? C23 C24 Cr1 C22 -38.24(19) . . . . ? C23 C24 Cr1 C20 -117.8(3) . . . . ? C20 C24 Cr1 C21 37.84(18) . . . . ? C23 C24 Cr1 C21 -79.9(2) . . . . ? C20 C24 Cr1 I1 -31.5(2) . . . . ? C23 C24 Cr1 I1 -149.24(16) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.652 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.095 data_6c_CpCr(OCPhCHCMeNXyl)OTf _database_code_depnum_ccdc_archive 'CCDC 791387' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H23 Cr F3 N O4 S' _chemical_formula_weight 530.49 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' F F 0.0171 0.0103 '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' Cr Cr 0.3209 0.6236 '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 bca' 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' '-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 13.518(9) _cell_length_b 16.712(8) _cell_length_c 21.148(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4778(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.93 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33379 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.04 _reflns_number_total 5769 _reflns_number_gt 4501 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+3.4079P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5769 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.026 _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 C1 C 0.79153(14) 0.03713(12) 0.53100(8) 0.0298(4) Uani 1 1 d . . . H10A H 0.7378 0.0757 0.5371 0.045 Uiso 1 1 calc R . . H10B H 0.8386 0.0414 0.5661 0.045 Uiso 1 1 calc R . . H10C H 0.7642 -0.0171 0.5297 0.045 Uiso 1 1 calc R . . C2 C 0.84385(13) 0.05472(10) 0.46957(8) 0.0232(3) Uani 1 1 d . . . C3 C 0.93940(13) 0.08875(10) 0.47401(8) 0.0252(4) Uani 1 1 d . . . H08 H 0.9653 0.0967 0.5153 0.030 Uiso 1 1 calc R . . C4 C 0.99832(12) 0.11133(9) 0.42415(8) 0.0216(3) Uani 1 1 d . . . C5 C 1.09246(12) 0.15624(10) 0.43398(8) 0.0224(3) Uani 1 1 d . . . C6 C 1.12310(14) 0.18251(11) 0.49326(9) 0.0302(4) Uani 1 1 d . . . H05 H 1.0847 0.1701 0.5296 0.036 Uiso 1 1 calc R . . C7 C 1.20943(14) 0.22673(12) 0.49970(10) 0.0329(4) Uani 1 1 d . . . H04 H 1.2300 0.2439 0.5405 0.040 Uiso 1 1 calc R . . C8 C 1.26561(13) 0.24593(11) 0.44738(10) 0.0325(4) Uani 1 1 d . . . H03 H 1.3243 0.2767 0.4520 0.039 Uiso 1 1 calc R . . C9 C 1.23606(14) 0.22023(12) 0.38831(10) 0.0344(4) Uani 1 1 d . . . H02 H 1.2745 0.2334 0.3522 0.041 Uiso 1 1 calc R . . C10 C 1.15053(13) 0.17530(11) 0.38141(9) 0.0286(4) Uani 1 1 d . . . H01 H 1.1312 0.1573 0.3406 0.034 Uiso 1 1 calc R . . C11 C 0.69950(12) 0.01127(10) 0.41472(8) 0.0233(3) Uani 1 1 d . . . C12 C 0.67940(14) -0.06805(11) 0.40087(8) 0.0264(4) Uani 1 1 d . . . H12 H 0.7322 -0.1046 0.3940 0.032 Uiso 1 1 calc R . . C13 C 0.58173(15) -0.09432(12) 0.39696(9) 0.0327(4) Uani 1 1 d . . . C14 C 0.50644(14) -0.03966(13) 0.40678(9) 0.0353(5) Uani 1 1 d . . . H14 H 0.4398 -0.0574 0.4041 0.042 Uiso 1 1 calc R . . C15 C 0.52512(14) 0.04030(13) 0.42039(9) 0.0326(4) Uani 1 1 d . . . C16 C 0.62304(13) 0.06539(11) 0.42434(9) 0.0281(4) Uani 1 1 d . . . H16 H 0.6376 0.1197 0.4336 0.034 Uiso 1 1 calc R . . C17 C 0.55991(19) -0.18101(14) 0.38323(12) 0.0514(6) Uani 1 1 d . . . H17A H 0.5756 -0.2134 0.4205 0.077 Uiso 1 1 calc R . . H17B H 0.6002 -0.1989 0.3474 0.077 Uiso 1 1 calc R . . H17C H 0.4897 -0.1871 0.3728 0.077 Uiso 1 1 calc R . . C18 C 0.44236(16) 0.09918(16) 0.43132(10) 0.0465(6) Uani 1 1 d . . . H18A H 0.4180 0.0938 0.4748 0.070 Uiso 1 1 calc R . . H18B H 0.3883 0.0883 0.4017 0.070 Uiso 1 1 calc R . . H18C H 0.4669 0.1537 0.4246 0.070 Uiso 1 1 calc R . . C19 C 0.74891(18) 0.02062(14) 0.25776(10) 0.0440(6) Uani 1 1 d . . . H19 H 0.6996 -0.0195 0.2623 0.053 Uiso 1 1 calc R . . C20 C 0.84052(18) 0.01172(13) 0.22805(9) 0.0411(5) Uani 1 1 d . . . H20 H 0.8642 -0.0358 0.2085 0.049 Uiso 1 1 calc R . . C21 C 0.89130(17) 0.08385(13) 0.23180(9) 0.0390(5) Uani 1 1 d . . . H21 H 0.9555 0.0941 0.2155 0.047 Uiso 1 1 calc R . . C22 C 0.83165(19) 0.13838(12) 0.26362(10) 0.0436(5) Uani 1 1 d . . . H22 H 0.8479 0.1924 0.2729 0.052 Uiso 1 1 calc R . . C23 C 0.74319(17) 0.09953(15) 0.27967(10) 0.0458(6) Uani 1 1 d . . . H23 H 0.6889 0.1227 0.3016 0.055 Uiso 1 1 calc R . . C24 C 0.91197(17) -0.20442(12) 0.29757(10) 0.0381(5) Uani 1 1 d . . . N1 N 0.80060(10) 0.03884(8) 0.41515(7) 0.0222(3) Uani 1 1 d . . . O1 O 0.97648(9) 0.09759(8) 0.36538(6) 0.0297(3) Uani 1 1 d . . . O2 O 0.92566(10) -0.06787(8) 0.35056(6) 0.0305(3) Uani 1 1 d . . . O3 O 1.05860(13) -0.16092(11) 0.36611(8) 0.0569(5) Uani 1 1 d . . . O4 O 1.03682(11) -0.09616(10) 0.26317(7) 0.0462(4) Uani 1 1 d . . . F1 F 0.86549(13) -0.23488(9) 0.34770(7) 0.0696(5) Uani 1 1 d . . . F2 F 0.96062(12) -0.26343(8) 0.26986(7) 0.0646(4) Uani 1 1 d . . . F3 F 0.84391(11) -0.17997(8) 0.25776(8) 0.0624(4) Uani 1 1 d . . . S1 S 0.99537(3) -0.12405(3) 0.32092(2) 0.03010(11) Uani 1 1 d . . . Cr1 Cr 0.86715(2) 0.040928(16) 0.330461(13) 0.02185(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0292(9) 0.0358(10) 0.0242(9) 0.0016(8) 0.0036(7) -0.0060(8) C2 0.0248(8) 0.0192(8) 0.0256(9) 0.0008(6) 0.0022(7) 0.0012(6) C3 0.0247(8) 0.0277(9) 0.0231(9) 0.0006(7) -0.0014(7) -0.0026(7) C4 0.0228(8) 0.0174(8) 0.0245(8) -0.0011(6) -0.0010(7) 0.0014(6) C5 0.0203(8) 0.0182(7) 0.0288(9) 0.0008(7) 0.0002(7) 0.0016(6) C6 0.0299(9) 0.0334(10) 0.0273(9) -0.0003(8) 0.0019(8) -0.0062(8) C7 0.0296(9) 0.0360(10) 0.0332(10) -0.0056(8) -0.0044(8) -0.0052(8) C8 0.0226(9) 0.0288(9) 0.0462(12) -0.0037(8) 0.0004(8) -0.0036(7) C9 0.0267(9) 0.0402(11) 0.0363(11) 0.0009(9) 0.0077(8) -0.0055(8) C10 0.0257(9) 0.0328(9) 0.0272(9) -0.0020(7) 0.0022(7) -0.0022(7) C11 0.0220(8) 0.0275(8) 0.0206(8) 0.0010(7) 0.0013(6) -0.0031(7) C12 0.0304(9) 0.0261(8) 0.0227(8) 0.0007(7) 0.0013(7) -0.0049(7) C13 0.0380(11) 0.0375(10) 0.0226(9) 0.0050(8) -0.0040(8) -0.0156(8) C14 0.0239(9) 0.0577(13) 0.0244(9) 0.0097(9) -0.0041(7) -0.0134(9) C15 0.0245(9) 0.0528(12) 0.0204(9) 0.0065(8) 0.0016(7) 0.0031(8) C16 0.0280(9) 0.0294(9) 0.0267(9) -0.0006(7) 0.0025(7) 0.0012(7) C17 0.0608(15) 0.0436(13) 0.0498(14) 0.0050(11) -0.0100(12) -0.0280(12) C18 0.0297(10) 0.0767(16) 0.0333(11) 0.0068(11) 0.0038(9) 0.0158(11) C19 0.0467(12) 0.0534(13) 0.0320(11) 0.0147(10) -0.0177(10) -0.0212(10) C20 0.0651(15) 0.0389(11) 0.0192(9) -0.0025(8) -0.0088(9) 0.0032(10) C21 0.0414(12) 0.0519(13) 0.0239(10) 0.0100(9) -0.0008(8) -0.0075(9) C22 0.0677(15) 0.0283(10) 0.0349(11) 0.0073(8) -0.0138(11) -0.0038(10) C23 0.0417(12) 0.0654(15) 0.0303(11) 0.0116(10) -0.0027(9) 0.0210(11) C24 0.0493(12) 0.0281(10) 0.0370(11) -0.0060(8) 0.0042(10) 0.0009(9) N1 0.0210(7) 0.0213(7) 0.0241(7) -0.0014(6) 0.0014(6) -0.0026(5) O1 0.0290(7) 0.0376(7) 0.0226(6) -0.0037(5) 0.0021(5) -0.0110(6) O2 0.0378(7) 0.0275(6) 0.0262(7) -0.0032(5) 0.0018(6) 0.0060(6) O3 0.0520(10) 0.0689(11) 0.0498(10) -0.0097(8) -0.0200(8) 0.0284(9) O4 0.0393(8) 0.0587(10) 0.0407(9) -0.0069(7) 0.0151(7) -0.0082(7) F1 0.1037(13) 0.0469(8) 0.0580(9) -0.0030(7) 0.0275(9) -0.0259(8) F2 0.0853(11) 0.0384(7) 0.0701(10) -0.0236(7) 0.0110(9) 0.0112(7) F3 0.0605(9) 0.0492(8) 0.0774(10) -0.0072(8) -0.0308(8) -0.0110(7) S1 0.0270(2) 0.0350(2) 0.0283(2) -0.00560(19) -0.00076(18) 0.00530(18) Cr1 0.02418(14) 0.02194(14) 0.01943(14) -0.00120(10) -0.00029(11) -0.00244(11) _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 C2 1.508(3) . ? C1 H10A 0.9800 . ? C1 H10B 0.9800 . ? C1 H10C 0.9800 . ? C2 N1 1.318(2) . ? C2 C3 1.414(2) . ? C3 C4 1.374(2) . ? C3 H08 0.9500 . ? C4 O1 1.298(2) . ? C4 C5 1.492(2) . ? C5 C6 1.392(3) . ? C5 C10 1.398(3) . ? C6 C7 1.388(3) . ? C6 H05 0.9500 . ? C7 C8 1.380(3) . ? C7 H04 0.9500 . ? C8 C9 1.380(3) . ? C8 H03 0.9500 . ? C9 C10 1.386(3) . ? C9 H02 0.9500 . ? C10 H01 0.9500 . ? C11 C12 1.385(3) . ? C11 C16 1.388(3) . ? C11 N1 1.442(2) . ? C12 C13 1.394(3) . ? C12 H12 0.9500 . ? C13 C14 1.383(3) . ? C13 C17 1.507(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.391(3) . ? C15 C18 1.508(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.397(3) . ? C19 C23 1.400(3) . ? C19 Cr1 2.244(2) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 Cr1 2.249(3) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 Cr1 2.230(2) . ? C21 H21 0.9500 . ? C22 C23 1.402(3) . ? C22 Cr1 2.209(2) . ? C22 H22 0.9500 . ? C23 Cr1 2.218(2) . ? C23 H23 0.9500 . ? C24 F3 1.312(3) . ? C24 F2 1.322(2) . ? C24 F1 1.333(3) . ? C24 S1 1.822(2) . ? N1 Cr1 2.0045(19) . ? O1 Cr1 1.9043(15) . ? O2 S1 1.4706(14) . ? O2 Cr1 2.0278(15) . ? O3 S1 1.4224(17) . ? O4 S1 1.4223(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 C2 C1 H10A 109.5 . . ? C2 C1 H10B 109.5 . . ? H10A C1 H10B 109.5 . . ? C2 C1 H10C 109.5 . . ? H10A C1 H10C 109.5 . . ? H10B C1 H10C 109.5 . . ? N1 C2 C3 122.97(16) . . ? N1 C2 C1 120.33(16) . . ? C3 C2 C1 116.70(16) . . ? C4 C3 C2 126.06(17) . . ? C4 C3 H08 117.0 . . ? C2 C3 H08 117.0 . . ? O1 C4 C3 123.66(16) . . ? O1 C4 C5 114.61(15) . . ? C3 C4 C5 121.71(16) . . ? C6 C5 C10 118.52(17) . . ? C6 C5 C4 122.56(16) . . ? C10 C5 C4 118.88(16) . . ? C7 C6 C5 120.44(18) . . ? C7 C6 H05 119.8 . . ? C5 C6 H05 119.8 . . ? C8 C7 C6 120.52(18) . . ? C8 C7 H04 119.7 . . ? C6 C7 H04 119.7 . . ? C7 C8 C9 119.61(18) . . ? C7 C8 H03 120.2 . . ? C9 C8 H03 120.2 . . ? C8 C9 C10 120.35(18) . . ? C8 C9 H02 119.8 . . ? C10 C9 H02 119.8 . . ? C9 C10 C5 120.54(18) . . ? C9 C10 H01 119.7 . . ? C5 C10 H01 119.7 . . ? C12 C11 C16 120.57(17) . . ? C12 C11 N1 119.55(16) . . ? C16 C11 N1 119.76(16) . . ? C11 C12 C13 120.00(18) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 118.70(18) . . ? C14 C13 C17 121.32(19) . . ? C12 C13 C17 120.0(2) . . ? C13 C14 C15 122.16(17) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 118.37(18) . . ? C14 C15 C18 121.62(19) . . ? C16 C15 C18 120.0(2) . . ? C11 C16 C15 120.21(18) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C23 107.4(2) . . ? C20 C19 Cr1 72.10(13) . . ? C23 C19 Cr1 70.73(12) . . ? C20 C19 H19 126.3 . . ? C23 C19 H19 126.3 . . ? Cr1 C19 H19 122.5 . . ? C21 C20 C19 108.7(2) . . ? C21 C20 Cr1 71.20(11) . . ? C19 C20 Cr1 71.68(12) . . ? C21 C20 H20 125.7 . . ? C19 C20 H20 125.7 . . ? Cr1 C20 H20 123.1 . . ? C20 C21 C22 108.0(2) . . ? C20 C21 Cr1 72.67(11) . . ? C22 C21 Cr1 70.92(12) . . ? C20 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? Cr1 C21 H21 122.1 . . ? C21 C22 C23 108.0(2) . . ? C21 C22 Cr1 72.58(12) . . ? C23 C22 Cr1 71.89(12) . . ? C21 C22 H22 126.0 . . ? C23 C22 H22 126.0 . . ? Cr1 C22 H22 121.3 . . ? C19 C23 C22 108.0(2) . . ? C19 C23 Cr1 72.70(12) . . ? C22 C23 Cr1 71.18(13) . . ? C19 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? Cr1 C23 H23 121.8 . . ? F3 C24 F2 107.25(18) . . ? F3 C24 F1 107.4(2) . . ? F2 C24 F1 107.58(18) . . ? F3 C24 S1 112.22(14) . . ? F2 C24 S1 111.23(16) . . ? F1 C24 S1 110.96(15) . . ? C2 N1 C11 119.35(14) . . ? C2 N1 Cr1 125.28(12) . . ? C11 N1 Cr1 115.17(11) . . ? C4 O1 Cr1 129.48(11) . . ? S1 O2 Cr1 137.14(9) . . ? O4 S1 O3 118.83(11) . . ? O4 S1 O2 114.16(9) . . ? O3 S1 O2 112.04(10) . . ? O4 S1 C24 104.63(10) . . ? O3 S1 C24 103.57(11) . . ? O2 S1 C24 100.93(10) . . ? O1 Cr1 N1 90.61(7) . . ? O1 Cr1 O2 93.54(7) . . ? N1 Cr1 O2 88.40(6) . . ? O1 Cr1 C22 92.88(8) . . ? N1 Cr1 C22 119.15(8) . . ? O2 Cr1 C22 151.62(7) . . ? O1 Cr1 C23 123.68(9) . . ? N1 Cr1 C23 95.81(8) . . ? O2 Cr1 C23 142.37(8) . . ? C22 Cr1 C23 36.93(9) . . ? O1 Cr1 C21 95.12(7) . . ? N1 Cr1 C21 155.11(8) . . ? O2 Cr1 C21 115.30(7) . . ? C22 Cr1 C21 36.50(9) . . ? C23 Cr1 C21 61.03(9) . . ? O1 Cr1 C19 153.36(7) . . ? N1 Cr1 C19 106.85(9) . . ? O2 Cr1 C19 106.61(8) . . ? C22 Cr1 C19 61.20(9) . . ? C23 Cr1 C19 36.57(9) . . ? C21 Cr1 C19 60.78(9) . . ? O1 Cr1 C20 127.27(7) . . ? N1 Cr1 C20 141.70(8) . . ? O2 Cr1 C20 94.00(7) . . ? C22 Cr1 C20 60.60(9) . . ? C23 Cr1 C20 60.57(9) . . ? C21 Cr1 C20 36.14(8) . . ? C19 Cr1 C20 36.22(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 1.7(3) . . . . ? C1 C2 C3 C4 -178.06(17) . . . . ? C2 C3 C4 O1 -6.3(3) . . . . ? C2 C3 C4 C5 172.00(16) . . . . ? O1 C4 C5 C6 174.10(16) . . . . ? C3 C4 C5 C6 -4.3(3) . . . . ? O1 C4 C5 C10 -3.5(2) . . . . ? C3 C4 C5 C10 178.07(16) . . . . ? C10 C5 C6 C7 0.1(3) . . . . ? C4 C5 C6 C7 -177.53(17) . . . . ? C5 C6 C7 C8 0.6(3) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? C8 C9 C10 C5 0.8(3) . . . . ? C6 C5 C10 C9 -0.8(3) . . . . ? C4 C5 C10 C9 176.93(16) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? N1 C11 C12 C13 -176.52(16) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C11 C12 C13 C17 -178.71(18) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? C17 C13 C14 C15 179.06(18) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C13 C14 C15 C18 -179.68(18) . . . . ? C12 C11 C16 C15 0.3(3) . . . . ? N1 C11 C16 C15 176.27(16) . . . . ? C14 C15 C16 C11 0.1(3) . . . . ? C18 C15 C16 C11 179.57(17) . . . . ? C23 C19 C20 C21 0.4(2) . . . . ? Cr1 C19 C20 C21 -61.95(14) . . . . ? C23 C19 C20 Cr1 62.34(14) . . . . ? C19 C20 C21 C22 -0.2(2) . . . . ? Cr1 C20 C21 C22 -62.50(14) . . . . ? C19 C20 C21 Cr1 62.25(14) . . . . ? C20 C21 C22 C23 0.0(2) . . . . ? Cr1 C21 C22 C23 -63.62(14) . . . . ? C20 C21 C22 Cr1 63.63(14) . . . . ? C20 C19 C23 C22 -0.4(2) . . . . ? Cr1 C19 C23 C22 62.85(15) . . . . ? C20 C19 C23 Cr1 -63.24(15) . . . . ? C21 C22 C23 C19 0.2(2) . . . . ? Cr1 C22 C23 C19 -63.84(15) . . . . ? C21 C22 C23 Cr1 64.07(15) . . . . ? C3 C2 N1 C11 -174.14(15) . . . . ? C1 C2 N1 C11 5.6(2) . . . . ? C3 C2 N1 Cr1 11.2(2) . . . . ? C1 C2 N1 Cr1 -169.09(12) . . . . ? C12 C11 N1 C2 -107.11(19) . . . . ? C16 C11 N1 C2 76.8(2) . . . . ? C12 C11 N1 Cr1 68.07(18) . . . . ? C16 C11 N1 Cr1 -107.97(16) . . . . ? C3 C4 O1 Cr1 -3.4(3) . . . . ? C5 C4 O1 Cr1 178.24(11) . . . . ? Cr1 O2 S1 O4 2.05(16) . . . . ? Cr1 O2 S1 O3 140.79(13) . . . . ? Cr1 O2 S1 C24 -109.58(14) . . . . ? F3 C24 S1 O4 -58.17(18) . . . . ? F2 C24 S1 O4 61.99(18) . . . . ? F1 C24 S1 O4 -178.30(15) . . . . ? F3 C24 S1 O3 176.68(16) . . . . ? F2 C24 S1 O3 -63.16(18) . . . . ? F1 C24 S1 O3 56.56(18) . . . . ? F3 C24 S1 O2 60.59(17) . . . . ? F2 C24 S1 O2 -179.25(15) . . . . ? F1 C24 S1 O2 -59.53(17) . . . . ? C4 O1 Cr1 N1 11.19(15) . . . . ? C4 O1 Cr1 O2 -77.24(15) . . . . ? C4 O1 Cr1 C22 130.42(16) . . . . ? C4 O1 Cr1 C23 108.59(16) . . . . ? C4 O1 Cr1 C21 166.94(16) . . . . ? C4 O1 Cr1 C19 143.08(19) . . . . ? C4 O1 Cr1 C20 -175.00(14) . . . . ? C2 N1 Cr1 O1 -14.79(14) . . . . ? C11 N1 Cr1 O1 170.36(12) . . . . ? C2 N1 Cr1 O2 78.74(14) . . . . ? C11 N1 Cr1 O2 -96.11(12) . . . . ? C2 N1 Cr1 C22 -108.42(15) . . . . ? C11 N1 Cr1 C22 76.73(14) . . . . ? C2 N1 Cr1 C23 -138.74(15) . . . . ? C11 N1 Cr1 C23 46.41(14) . . . . ? C2 N1 Cr1 C21 -118.37(19) . . . . ? C11 N1 Cr1 C21 66.8(2) . . . . ? C2 N1 Cr1 C19 -174.38(14) . . . . ? C11 N1 Cr1 C19 10.77(14) . . . . ? C2 N1 Cr1 C20 173.17(14) . . . . ? C11 N1 Cr1 C20 -1.68(18) . . . . ? S1 O2 Cr1 O1 -84.93(14) . . . . ? S1 O2 Cr1 N1 -175.44(13) . . . . ? S1 O2 Cr1 C22 17.8(2) . . . . ? S1 O2 Cr1 C23 87.10(17) . . . . ? S1 O2 Cr1 C21 12.43(15) . . . . ? S1 O2 Cr1 C19 77.44(15) . . . . ? S1 O2 Cr1 C20 42.84(14) . . . . ? C21 C22 Cr1 O1 94.72(14) . . . . ? C23 C22 Cr1 O1 -149.01(14) . . . . ? C21 C22 Cr1 N1 -172.98(12) . . . . ? C23 C22 Cr1 N1 -56.71(15) . . . . ? C21 C22 Cr1 O2 -8.2(2) . . . . ? C23 C22 Cr1 O2 108.10(19) . . . . ? C21 C22 Cr1 C23 -116.27(19) . . . . ? C23 C22 Cr1 C21 116.27(19) . . . . ? C21 C22 Cr1 C19 -78.84(15) . . . . ? C23 C22 Cr1 C19 37.44(14) . . . . ? C21 C22 Cr1 C20 -37.16(13) . . . . ? C23 C22 Cr1 C20 79.11(15) . . . . ? C19 C23 Cr1 O1 154.77(12) . . . . ? C22 C23 Cr1 O1 38.17(16) . . . . ? C19 C23 Cr1 N1 -110.61(13) . . . . ? C22 C23 Cr1 N1 132.79(13) . . . . ? C19 C23 Cr1 O2 -15.66(19) . . . . ? C22 C23 Cr1 O2 -132.27(14) . . . . ? C19 C23 Cr1 C22 116.60(19) . . . . ? C19 C23 Cr1 C21 79.03(14) . . . . ? C22 C23 Cr1 C21 -37.57(13) . . . . ? C22 C23 Cr1 C19 -116.60(19) . . . . ? C19 C23 Cr1 C20 37.42(13) . . . . ? C22 C23 Cr1 C20 -79.18(15) . . . . ? C20 C21 Cr1 O1 155.27(14) . . . . ? C22 C21 Cr1 O1 -87.92(14) . . . . ? C20 C21 Cr1 N1 -102.1(2) . . . . ? C22 C21 Cr1 N1 14.7(2) . . . . ? C20 C21 Cr1 O2 58.90(15) . . . . ? C22 C21 Cr1 O2 175.71(12) . . . . ? C20 C21 Cr1 C22 -116.8(2) . . . . ? C20 C21 Cr1 C23 -78.80(16) . . . . ? C22 C21 Cr1 C23 38.01(14) . . . . ? C20 C21 Cr1 C19 -36.73(14) . . . . ? C22 C21 Cr1 C19 80.09(15) . . . . ? C22 C21 Cr1 C20 116.8(2) . . . . ? C20 C19 Cr1 O1 64.1(2) . . . . ? C23 C19 Cr1 O1 -52.3(2) . . . . ? C20 C19 Cr1 N1 -166.93(12) . . . . ? C23 C19 Cr1 N1 76.65(14) . . . . ? C20 C19 Cr1 O2 -73.49(13) . . . . ? C23 C19 Cr1 O2 170.09(12) . . . . ? C20 C19 Cr1 C22 78.60(15) . . . . ? C23 C19 Cr1 C22 -37.81(13) . . . . ? C20 C19 Cr1 C23 116.42(19) . . . . ? C20 C19 Cr1 C21 36.64(13) . . . . ? C23 C19 Cr1 C21 -79.78(14) . . . . ? C23 C19 Cr1 C20 -116.42(19) . . . . ? C21 C20 Cr1 O1 -31.57(17) . . . . ? C19 C20 Cr1 O1 -149.54(12) . . . . ? C21 C20 Cr1 N1 138.40(13) . . . . ? C19 C20 Cr1 N1 20.44(19) . . . . ? C21 C20 Cr1 O2 -129.11(14) . . . . ? C19 C20 Cr1 O2 112.93(13) . . . . ? C21 C20 Cr1 C22 37.54(14) . . . . ? C19 C20 Cr1 C22 -80.42(15) . . . . ? C21 C20 Cr1 C23 80.19(16) . . . . ? C19 C20 Cr1 C23 -37.78(14) . . . . ? C19 C20 Cr1 C21 -118.0(2) . . . . ? C21 C20 Cr1 C19 118.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.406 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.053 data_8_CpCr(DBU)Mes _database_code_depnum_ccdc_archive 'CCDC 791388' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Cr N2' _chemical_formula_weight 388.51 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' Cr Cr 0.3209 0.6236 '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 b c a' 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' '-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 14.3796(11) _cell_length_b 15.9373(12) _cell_length_c 18.4488(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4227.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6290 _cell_measurement_theta_min 2.2065 _cell_measurement_theta_max 17.522 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.180 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7648 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26292 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.03 _reflns_number_total 5111 _reflns_number_gt 3446 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+1.9580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5111 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.001 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 C1 C 0.36476(16) 0.19582(13) 0.50492(12) 0.0427(5) Uani 1 1 d . . . H1A H 0.3252 0.2396 0.4826 0.051 Uiso 1 1 calc R . . H1B H 0.4280 0.2007 0.4840 0.051 Uiso 1 1 calc R . . C2 C 0.36928(18) 0.20958(14) 0.58584(12) 0.0480(6) Uani 1 1 d . . . H2A H 0.3936 0.2664 0.5964 0.058 Uiso 1 1 calc R . . H2B H 0.3064 0.2047 0.6072 0.058 Uiso 1 1 calc R . . C3 C 0.43267(17) 0.14416(16) 0.61787(13) 0.0496(6) Uani 1 1 d . . . H3A H 0.4980 0.1627 0.6128 0.060 Uiso 1 1 calc R . . H3B H 0.4191 0.1381 0.6702 0.060 Uiso 1 1 calc R . . C4 C 0.46308(16) -0.00754(16) 0.62153(12) 0.0480(6) Uani 1 1 d . . . H4A H 0.5158 0.0138 0.6507 0.058 Uiso 1 1 calc R . . H4B H 0.4882 -0.0483 0.5861 0.058 Uiso 1 1 calc R . . C5 C 0.39546(17) -0.05262(15) 0.67141(11) 0.0466(6) Uani 1 1 d . . . H5A H 0.4311 -0.0822 0.7095 0.056 Uiso 1 1 calc R . . H5B H 0.3554 -0.0105 0.6955 0.056 Uiso 1 1 calc R . . C6 C 0.3345(2) -0.11514(14) 0.63256(12) 0.0530(7) Uani 1 1 d . . . H6A H 0.2924 -0.1415 0.6684 0.064 Uiso 1 1 calc R . . H6B H 0.3746 -0.1599 0.6123 0.064 Uiso 1 1 calc R . . C7 C 0.27581(18) -0.07860(14) 0.57136(11) 0.0452(6) Uani 1 1 d . . . H7A H 0.2327 -0.0365 0.5921 0.054 Uiso 1 1 calc R . . H7B H 0.2376 -0.1241 0.5502 0.054 Uiso 1 1 calc R . . C8 C 0.33188(16) -0.03706(12) 0.51055(11) 0.0378(5) Uani 1 1 d . . . H8A H 0.3883 -0.0710 0.5012 0.045 Uiso 1 1 calc R . . H8B H 0.2941 -0.0371 0.4657 0.045 Uiso 1 1 calc R . . C9 C 0.36047(13) 0.05098(12) 0.52716(10) 0.0297(4) Uani 1 1 d . . . C10 C 0.25876(13) 0.02872(12) 0.33677(10) 0.0282(4) Uani 1 1 d . . . C11 C 0.32723(14) 0.05607(12) 0.28745(10) 0.0307(4) Uani 1 1 d . . . C12 C 0.36342(14) 0.00290(13) 0.23488(10) 0.0366(5) Uani 1 1 d . . . H12 H 0.4092 0.0238 0.2025 0.044 Uiso 1 1 calc R . . C13 C 0.33459(15) -0.07958(14) 0.22841(11) 0.0393(5) Uani 1 1 d . . . C14 C 0.26554(15) -0.10701(13) 0.27442(11) 0.0359(5) Uani 1 1 d . . . H14 H 0.2435 -0.1630 0.2702 0.043 Uiso 1 1 calc R . . C15 C 0.22714(13) -0.05448(12) 0.32720(10) 0.0314(4) Uani 1 1 d . . . C16 C 0.36320(16) 0.14544(13) 0.29138(12) 0.0431(5) Uani 1 1 d . . . H16A H 0.4049 0.1560 0.2504 0.065 Uiso 1 1 calc R . . H16B H 0.3972 0.1535 0.3369 0.065 Uiso 1 1 calc R . . H16C H 0.3107 0.1846 0.2894 0.065 Uiso 1 1 calc R . . C17 C 0.3779(2) -0.13763(18) 0.17264(15) 0.0672(8) Uani 1 1 d . . . H17A H 0.3518 -0.1941 0.1781 0.101 Uiso 1 1 calc R . . H17B H 0.4453 -0.1397 0.1799 0.101 Uiso 1 1 calc R . . H17C H 0.3644 -0.1166 0.1238 0.101 Uiso 1 1 calc R . . C18 C 0.14876(16) -0.08905(14) 0.37315(13) 0.0463(6) Uani 1 1 d . . . H18A H 0.0890 -0.0703 0.3534 0.069 Uiso 1 1 calc R . . H18B H 0.1554 -0.0687 0.4230 0.069 Uiso 1 1 calc R . . H18C H 0.1512 -0.1505 0.3728 0.069 Uiso 1 1 calc R . . C19 C 0.06268(16) 0.13548(17) 0.46427(14) 0.0525(6) Uani 1 1 d . . . H19 H 0.0345 0.0995 0.4990 0.063 Uiso 1 1 calc R . . C20 C 0.11603(16) 0.20670(14) 0.47845(12) 0.0430(5) Uani 1 1 d . . . H20 H 0.1327 0.2268 0.5252 0.052 Uiso 1 1 calc R . . C21 C 0.14097(17) 0.24365(15) 0.41258(12) 0.0467(6) Uani 1 1 d . . . H21 H 0.1755 0.2940 0.4069 0.056 Uiso 1 1 calc R . . C22 C 0.10663(19) 0.19419(17) 0.35716(13) 0.0564(7) Uani 1 1 d . . . H22 H 0.1144 0.2042 0.3068 0.068 Uiso 1 1 calc R . . C23 C 0.05880(18) 0.12749(18) 0.38786(16) 0.0615(8) Uani 1 1 d . . . H23 H 0.0285 0.0838 0.3620 0.074 Uiso 1 1 calc R . . N1 N 0.32635(12) 0.11235(10) 0.48818(9) 0.0314(4) Uani 1 1 d . . . N2 N 0.42093(12) 0.06272(11) 0.58211(9) 0.0364(4) Uani 1 1 d . . . Cr01 Cr 0.21342(2) 0.11059(2) 0.418136(16) 0.03095(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0446(13) 0.0351(12) 0.0483(13) 0.0060(9) -0.0110(10) -0.0086(10) C2 0.0556(15) 0.0382(12) 0.0501(13) -0.0056(10) -0.0090(11) -0.0158(11) C3 0.0461(13) 0.0600(15) 0.0427(13) 0.0026(11) -0.0140(11) -0.0201(12) C4 0.0389(13) 0.0699(16) 0.0351(12) 0.0118(11) -0.0032(9) 0.0205(12) C5 0.0609(15) 0.0516(14) 0.0274(11) 0.0072(9) 0.0034(10) 0.0194(12) C6 0.0870(19) 0.0376(13) 0.0344(12) 0.0069(10) 0.0105(12) 0.0132(13) C7 0.0650(16) 0.0303(11) 0.0402(12) -0.0011(9) 0.0017(11) -0.0045(11) C8 0.0541(14) 0.0310(11) 0.0282(10) -0.0013(8) -0.0032(9) 0.0110(10) C9 0.0267(10) 0.0363(11) 0.0260(9) 0.0022(8) 0.0022(8) 0.0053(8) C10 0.0286(10) 0.0286(10) 0.0273(10) 0.0019(7) -0.0072(8) 0.0051(8) C11 0.0324(10) 0.0300(10) 0.0298(10) 0.0024(8) -0.0075(8) 0.0022(8) C12 0.0317(11) 0.0475(13) 0.0307(11) -0.0020(9) -0.0010(8) -0.0037(10) C13 0.0375(12) 0.0436(12) 0.0368(12) -0.0125(9) -0.0044(9) 0.0028(10) C14 0.0416(12) 0.0266(10) 0.0396(11) -0.0031(8) -0.0097(9) -0.0015(9) C15 0.0321(11) 0.0318(10) 0.0302(10) 0.0027(8) -0.0052(8) 0.0014(8) C16 0.0452(13) 0.0336(11) 0.0505(13) 0.0041(10) -0.0005(10) -0.0053(10) C17 0.0643(18) 0.0684(18) 0.0688(18) -0.0373(14) 0.0151(14) -0.0072(15) C18 0.0455(14) 0.0423(13) 0.0510(14) 0.0029(10) 0.0032(11) -0.0086(11) C19 0.0358(13) 0.0580(16) 0.0639(16) 0.0003(12) 0.0057(11) 0.0098(12) C20 0.0474(13) 0.0465(13) 0.0353(12) -0.0106(9) -0.0045(10) 0.0153(11) C21 0.0506(14) 0.0402(12) 0.0491(13) -0.0003(10) -0.0031(11) 0.0204(11) C22 0.0634(17) 0.0676(18) 0.0383(13) -0.0065(12) -0.0151(12) 0.0362(15) C23 0.0405(14) 0.0656(19) 0.0785(19) -0.0336(15) -0.0293(13) 0.0206(13) N1 0.0331(9) 0.0282(8) 0.0329(8) 0.0019(7) -0.0047(7) -0.0006(7) N2 0.0289(9) 0.0484(11) 0.0320(9) 0.0056(8) -0.0045(7) 0.0026(8) Cr01 0.03276(18) 0.03134(18) 0.02875(17) -0.00355(13) -0.00678(13) 0.00807(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 C1 N1 1.473(3) . ? C1 C2 1.510(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.506(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.466(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.466(3) . ? C4 C5 1.519(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.508(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.525(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.532(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.494(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N1 1.309(2) . ? C9 N2 1.349(2) . ? C10 C11 1.410(3) . ? C10 C15 1.413(3) . ? C10 Cr01 2.0931(19) . ? C11 C12 1.389(3) . ? C11 C16 1.517(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C14 1.377(3) . ? C13 C17 1.517(3) . ? C14 C15 1.398(3) . ? C14 H14 0.9500 . ? C15 C18 1.514(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.395(3) . ? C19 C23 1.417(4) . ? C19 Cr01 2.362(2) . ? C19 H19 0.9500 . ? C20 C21 1.397(3) . ? C20 Cr01 2.355(2) . ? C20 H20 0.9500 . ? C21 C22 1.382(3) . ? C21 Cr01 2.365(2) . ? C21 H21 0.9500 . ? C22 C23 1.387(4) . ? C22 Cr01 2.323(2) . ? C22 H22 0.9500 . ? C23 Cr01 2.308(2) . ? C23 H23 0.9500 . ? N1 Cr01 2.0755(16) . ? 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 110.76(18) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C3 C2 C1 108.3(2) . . ? C3 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C2 111.53(17) . . ? N2 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C5 113.39(18) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 113.35(19) . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 114.91(19) . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 114.6(2) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 113.60(17) . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N1 C9 N2 123.42(18) . . ? N1 C9 C8 119.06(17) . . ? N2 C9 C8 117.52(17) . . ? C11 C10 C15 115.74(17) . . ? C11 C10 Cr01 119.19(14) . . ? C15 C10 Cr01 125.06(14) . . ? C12 C11 C10 121.58(18) . . ? C12 C11 C16 118.58(18) . . ? C10 C11 C16 119.84(18) . . ? C13 C12 C11 121.85(19) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C14 C13 C12 117.67(19) . . ? C14 C13 C17 121.3(2) . . ? C12 C13 C17 121.0(2) . . ? C13 C14 C15 121.60(19) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 121.46(19) . . ? C14 C15 C18 117.79(19) . . ? C10 C15 C18 120.74(18) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C23 106.4(2) . . ? C20 C19 Cr01 72.51(13) . . ? C23 C19 Cr01 70.27(14) . . ? C20 C19 H19 126.8 . . ? C23 C19 H19 126.8 . . ? Cr01 C19 H19 122.2 . . ? C19 C20 C21 108.7(2) . . ? C19 C20 Cr01 73.09(13) . . ? C21 C20 Cr01 73.17(12) . . ? C19 C20 H20 125.6 . . ? C21 C20 H20 125.6 . . ? Cr01 C20 H20 119.9 . . ? C22 C21 C20 108.1(2) . . ? C22 C21 Cr01 71.22(13) . . ? C20 C21 Cr01 72.39(12) . . ? C22 C21 H21 125.9 . . ? C20 C21 H21 125.9 . . ? Cr01 C21 H21 122.2 . . ? C21 C22 C23 108.2(2) . . ? C21 C22 Cr01 74.50(13) . . ? C23 C22 Cr01 71.97(14) . . ? C21 C22 H22 125.9 . . ? C23 C22 H22 125.9 . . ? Cr01 C22 H22 119.5 . . ? C22 C23 C19 108.5(2) . . ? C22 C23 Cr01 73.18(14) . . ? C19 C23 Cr01 74.44(13) . . ? C22 C23 H23 125.7 . . ? C19 C23 H23 125.7 . . ? Cr01 C23 H23 118.5 . . ? C9 N1 C1 114.77(17) . . ? C9 N1 Cr01 128.69(13) . . ? C1 N1 Cr01 115.85(12) . . ? C9 N2 C4 122.23(19) . . ? C9 N2 C3 122.38(17) . . ? C4 N2 C3 113.92(17) . . ? N1 Cr01 C10 102.19(7) . . ? N1 Cr01 C23 154.52(8) . . ? C10 Cr01 C23 101.49(8) . . ? N1 Cr01 C22 144.17(8) . . ? C10 Cr01 C22 102.48(8) . . ? C23 Cr01 C22 34.85(10) . . ? N1 Cr01 C20 99.34(7) . . ? C10 Cr01 C20 158.37(7) . . ? C23 Cr01 C20 57.70(8) . . ? C22 Cr01 C20 57.51(8) . . ? N1 Cr01 C19 119.43(8) . . ? C10 Cr01 C19 130.46(8) . . ? C23 Cr01 C19 35.29(9) . . ? C22 Cr01 C19 58.11(10) . . ? C20 Cr01 C19 34.39(8) . . ? N1 Cr01 C21 111.07(8) . . ? C10 Cr01 C21 131.70(7) . . ? C23 Cr01 C21 57.36(9) . . ? C22 Cr01 C21 34.28(8) . . ? C20 Cr01 C21 34.44(8) . . ? C19 Cr01 C21 57.37(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 61.2(2) . . . . ? C1 C2 C3 N2 -38.3(3) . . . . ? N2 C4 C5 C6 81.2(3) . . . . ? C4 C5 C6 C7 -58.0(3) . . . . ? C5 C6 C7 C8 59.5(3) . . . . ? C6 C7 C8 C9 -82.3(2) . . . . ? C7 C8 C9 N1 -114.6(2) . . . . ? C7 C8 C9 N2 65.6(3) . . . . ? C15 C10 C11 C12 -2.5(3) . . . . ? Cr01 C10 C11 C12 176.50(14) . . . . ? C15 C10 C11 C16 177.75(17) . . . . ? Cr01 C10 C11 C16 -3.3(2) . . . . ? C10 C11 C12 C13 -0.3(3) . . . . ? C16 C11 C12 C13 179.44(19) . . . . ? C11 C12 C13 C14 2.4(3) . . . . ? C11 C12 C13 C17 -177.5(2) . . . . ? C12 C13 C14 C15 -1.6(3) . . . . ? C17 C13 C14 C15 178.3(2) . . . . ? C13 C14 C15 C10 -1.3(3) . . . . ? C13 C14 C15 C18 177.5(2) . . . . ? C11 C10 C15 C14 3.3(3) . . . . ? Cr01 C10 C15 C14 -175.63(14) . . . . ? C11 C10 C15 C18 -175.47(18) . . . . ? Cr01 C10 C15 C18 5.6(3) . . . . ? C23 C19 C20 C21 2.5(3) . . . . ? Cr01 C19 C20 C21 65.01(16) . . . . ? C23 C19 C20 Cr01 -62.53(16) . . . . ? C19 C20 C21 C22 -2.3(3) . . . . ? Cr01 C20 C21 C22 62.65(16) . . . . ? C19 C20 C21 Cr01 -64.96(16) . . . . ? C20 C21 C22 C23 1.2(3) . . . . ? Cr01 C21 C22 C23 64.58(16) . . . . ? C20 C21 C22 Cr01 -63.40(16) . . . . ? C21 C22 C23 C19 0.4(3) . . . . ? Cr01 C22 C23 C19 66.61(17) . . . . ? C21 C22 C23 Cr01 -66.25(16) . . . . ? C20 C19 C23 C22 -1.8(3) . . . . ? Cr01 C19 C23 C22 -65.78(17) . . . . ? C20 C19 C23 Cr01 64.03(16) . . . . ? N2 C9 N1 C1 4.7(3) . . . . ? C8 C9 N1 C1 -175.16(18) . . . . ? N2 C9 N1 Cr01 -165.26(14) . . . . ? C8 C9 N1 Cr01 14.9(3) . . . . ? C2 C1 N1 C9 -45.1(3) . . . . ? C2 C1 N1 Cr01 126.16(17) . . . . ? N1 C9 N2 C4 -175.59(18) . . . . ? C8 C9 N2 C4 4.3(3) . . . . ? N1 C9 N2 C3 19.1(3) . . . . ? C8 C9 N2 C3 -161.04(19) . . . . ? C5 C4 N2 C9 -72.4(3) . . . . ? C5 C4 N2 C3 94.0(2) . . . . ? C2 C3 N2 C9 0.5(3) . . . . ? C2 C3 N2 C4 -165.95(19) . . . . ? C9 N1 Cr01 C10 -65.16(18) . . . . ? C1 N1 Cr01 C10 124.99(15) . . . . ? C9 N1 Cr01 C23 92.8(3) . . . . ? C1 N1 Cr01 C23 -77.0(3) . . . . ? C9 N1 Cr01 C22 162.23(17) . . . . ? C1 N1 Cr01 C22 -7.6(2) . . . . ? C9 N1 Cr01 C20 116.83(18) . . . . ? C1 N1 Cr01 C20 -53.01(16) . . . . ? C9 N1 Cr01 C19 86.98(19) . . . . ? C1 N1 Cr01 C19 -82.86(17) . . . . ? C9 N1 Cr01 C21 150.49(17) . . . . ? C1 N1 Cr01 C21 -19.35(17) . . . . ? C11 C10 Cr01 N1 -72.85(15) . . . . ? C15 C10 Cr01 N1 106.03(16) . . . . ? C11 C10 Cr01 C23 116.61(16) . . . . ? C15 C10 Cr01 C23 -64.50(18) . . . . ? C11 C10 Cr01 C22 80.97(17) . . . . ? C15 C10 Cr01 C22 -100.15(17) . . . . ? C11 C10 Cr01 C20 101.8(2) . . . . ? C15 C10 Cr01 C20 -79.3(3) . . . . ? C11 C10 Cr01 C19 139.49(15) . . . . ? C15 C10 Cr01 C19 -41.6(2) . . . . ? C11 C10 Cr01 C21 60.40(19) . . . . ? C15 C10 Cr01 C21 -120.72(17) . . . . ? C22 C23 Cr01 N1 106.5(2) . . . . ? C19 C23 Cr01 N1 -8.9(3) . . . . ? C22 C23 Cr01 C10 -95.39(15) . . . . ? C19 C23 Cr01 C10 149.21(16) . . . . ? C19 C23 Cr01 C22 -115.4(2) . . . . ? C22 C23 Cr01 C20 78.21(15) . . . . ? C19 C23 Cr01 C20 -37.19(14) . . . . ? C22 C23 Cr01 C19 115.4(2) . . . . ? C22 C23 Cr01 C21 37.13(13) . . . . ? C19 C23 Cr01 C21 -78.27(16) . . . . ? C21 C22 Cr01 N1 -19.7(2) . . . . ? C23 C22 Cr01 N1 -135.21(16) . . . . ? C21 C22 Cr01 C10 -152.23(16) . . . . ? C23 C22 Cr01 C10 92.25(15) . . . . ? C21 C22 Cr01 C23 115.5(2) . . . . ? C21 C22 Cr01 C20 36.71(15) . . . . ? C23 C22 Cr01 C20 -78.81(16) . . . . ? C21 C22 Cr01 C19 77.60(16) . . . . ? C23 C22 Cr01 C19 -37.92(15) . . . . ? C23 C22 Cr01 C21 -115.5(2) . . . . ? C19 C20 Cr01 N1 -129.88(14) . . . . ? C21 C20 Cr01 N1 113.85(15) . . . . ? C19 C20 Cr01 C10 55.4(3) . . . . ? C21 C20 Cr01 C10 -60.9(3) . . . . ? C19 C20 Cr01 C23 38.18(16) . . . . ? C21 C20 Cr01 C23 -78.08(17) . . . . ? C19 C20 Cr01 C22 79.73(17) . . . . ? C21 C20 Cr01 C22 -36.54(15) . . . . ? C21 C20 Cr01 C19 -116.3(2) . . . . ? C19 C20 Cr01 C21 116.3(2) . . . . ? C20 C19 Cr01 N1 60.39(16) . . . . ? C23 C19 Cr01 N1 175.64(15) . . . . ? C20 C19 Cr01 C10 -156.50(13) . . . . ? C23 C19 Cr01 C10 -41.3(2) . . . . ? C20 C19 Cr01 C23 -115.2(2) . . . . ? C20 C19 Cr01 C22 -77.81(16) . . . . ? C23 C19 Cr01 C22 37.44(15) . . . . ? C23 C19 Cr01 C20 115.2(2) . . . . ? C20 C19 Cr01 C21 -37.03(13) . . . . ? C23 C19 Cr01 C21 78.22(17) . . . . ? C22 C21 Cr01 N1 167.80(16) . . . . ? C20 C21 Cr01 N1 -75.27(16) . . . . ? C22 C21 Cr01 C10 37.5(2) . . . . ? C20 C21 Cr01 C10 154.47(13) . . . . ? C22 C21 Cr01 C23 -37.77(16) . . . . ? C20 C21 Cr01 C23 79.17(17) . . . . ? C20 C21 Cr01 C22 116.9(2) . . . . ? C22 C21 Cr01 C20 -116.9(2) . . . . ? C22 C21 Cr01 C19 -79.96(18) . . . . ? C20 C21 Cr01 C19 36.97(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.285 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.049 data_9_CpCr(DBU)(Mes)I _database_code_depnum_ccdc_archive 'CCDC 791389' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Cr I N2' _chemical_formula_weight 515.41 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' Cr Cr 0.3209 0.6236 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5521(5) _cell_length_b 13.9206(5) _cell_length_c 14.6207(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.5070(10) _cell_angle_gamma 90.00 _cell_volume 2202.19(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9810 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.01 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.629 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31129 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.01 _reflns_number_total 5314 _reflns_number_gt 4798 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.1246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5314 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.001 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 C1 C -0.09659(17) 0.36760(14) 0.76118(14) 0.0213(4) Uani 1 1 d . . . H1A H -0.1608 0.3605 0.7912 0.026 Uiso 1 1 calc R . . H1B H -0.1176 0.3236 0.7045 0.026 Uiso 1 1 calc R . . C2 C -0.09681(18) 0.46992(14) 0.72631(14) 0.0227(4) Uani 1 1 d . . . H2A H -0.0361 0.4768 0.6928 0.027 Uiso 1 1 calc R . . H2B H -0.1796 0.4865 0.6793 0.027 Uiso 1 1 calc R . . C3 C -0.06362(18) 0.53652(14) 0.81288(14) 0.0234(4) Uani 1 1 d . . . H3A H -0.0459 0.6014 0.7934 0.028 Uiso 1 1 calc R . . H3B H -0.1340 0.5416 0.8365 0.028 Uiso 1 1 calc R . . C4 C 0.11534(19) 0.57339(13) 0.96020(14) 0.0215(4) Uani 1 1 d . . . H4A H 0.1462 0.5456 1.0267 0.026 Uiso 1 1 calc R . . H4B H 0.0590 0.6270 0.9603 0.026 Uiso 1 1 calc R . . C5 C 0.2243(2) 0.61307(14) 0.93658(15) 0.0246(4) Uani 1 1 d . . . H5A H 0.2470 0.6767 0.9680 0.029 Uiso 1 1 calc R . . H5B H 0.1990 0.6224 0.8651 0.029 Uiso 1 1 calc R . . C6 C 0.33727(18) 0.54792(14) 0.97052(15) 0.0239(4) Uani 1 1 d . . . H6A H 0.3681 0.5446 1.0427 0.029 Uiso 1 1 calc R . . H6B H 0.4033 0.5768 0.9508 0.029 Uiso 1 1 calc R . . C7 C 0.31245(17) 0.44624(14) 0.92975(14) 0.0202(4) Uani 1 1 d . . . H7A H 0.3912 0.4101 0.9519 0.024 Uiso 1 1 calc R . . H7B H 0.2835 0.4497 0.8576 0.024 Uiso 1 1 calc R . . C8 C 0.21659(16) 0.39000(12) 0.95968(13) 0.0150(3) Uani 1 1 d . . . H8A H 0.2343 0.3204 0.9599 0.018 Uiso 1 1 calc R . . H8B H 0.2236 0.4087 1.0267 0.018 Uiso 1 1 calc R . . C9 C 0.08722(16) 0.40900(13) 0.89119(12) 0.0139(3) Uani 1 1 d . . . C10 C 0.24408(16) 0.20976(13) 0.83054(13) 0.0157(3) Uani 1 1 d . . . C11 C 0.35073(17) 0.16288(14) 0.89410(13) 0.0189(4) Uani 1 1 d . . . C12 C 0.46815(18) 0.18183(15) 0.89022(14) 0.0225(4) Uani 1 1 d . . . H12 H 0.5379 0.1503 0.9352 0.027 Uiso 1 1 calc R . . C13 C 0.48570(17) 0.24503(15) 0.82293(14) 0.0217(4) Uani 1 1 d . . . C14 C 0.38114(18) 0.28690(14) 0.75680(14) 0.0199(4) Uani 1 1 d . . . H14 H 0.3903 0.3287 0.7084 0.024 Uiso 1 1 calc R . . C15 C 0.26255(17) 0.27010(13) 0.75851(13) 0.0170(3) Uani 1 1 d . . . C16 C 0.3449(2) 0.09019(17) 0.96899(16) 0.0303(5) Uani 1 1 d . . . H16A H 0.4266 0.0613 1.0003 0.045 Uiso 1 1 calc R . . H16B H 0.2851 0.0399 0.9368 0.045 Uiso 1 1 calc R . . H16C H 0.3191 0.1221 1.0185 0.045 Uiso 1 1 calc R . . C17 C 0.61245(19) 0.26738(17) 0.82046(16) 0.0300(5) Uani 1 1 d . . . H17A H 0.6748 0.2314 0.8722 0.045 Uiso 1 1 calc R . . H17B H 0.6286 0.3364 0.8306 0.045 Uiso 1 1 calc R . . H17C H 0.6162 0.2488 0.7569 0.045 Uiso 1 1 calc R . . C18 C 0.15843(19) 0.31852(15) 0.67861(14) 0.0241(4) Uani 1 1 d . . . H18A H 0.0795 0.3025 0.6859 0.036 Uiso 1 1 calc R . . H18B H 0.1577 0.2962 0.6148 0.036 Uiso 1 1 calc R . . H18C H 0.1705 0.3883 0.6832 0.036 Uiso 1 1 calc R . . C19 C 0.0257(2) 0.03417(15) 0.82313(17) 0.0323(5) Uani 1 1 d . . . H19 H 0.0738 -0.0101 0.8708 0.039 Uiso 1 1 calc R . . C20 C 0.0531(2) 0.06767(16) 0.74314(16) 0.0298(5) Uani 1 1 d . . . H20 H 0.1215 0.0488 0.7256 0.036 Uiso 1 1 calc R . . C21 C -0.03921(19) 0.13479(15) 0.69274(15) 0.0255(4) Uani 1 1 d . . . H21 H -0.0424 0.1708 0.6367 0.031 Uiso 1 1 calc R . . C22 C -0.12588(19) 0.13837(16) 0.74114(16) 0.0285(5) Uani 1 1 d . . . H22 H -0.1991 0.1760 0.7222 0.034 Uiso 1 1 calc R . . C23 C -0.0851(2) 0.07722(16) 0.82108(17) 0.0330(5) Uani 1 1 d . . . H23 H -0.1254 0.0663 0.8667 0.040 Uiso 1 1 calc R . . N1 N 0.02494(13) 0.34021(11) 0.83330(11) 0.0146(3) Uani 1 1 d . . . N2 N 0.04519(14) 0.49948(11) 0.89106(11) 0.0169(3) Uani 1 1 d . . . Cr1 Cr 0.06722(3) 0.193742(19) 0.84190(2) 0.01340(6) Uani 1 1 d . . . I1 I 0.084000(12) 0.186223(9) 1.034395(9) 0.02023(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0126(8) 0.0225(10) 0.0241(9) 0.0016(8) 0.0007(7) 0.0020(7) C2 0.0198(9) 0.0244(10) 0.0211(9) 0.0056(8) 0.0038(7) 0.0081(8) C3 0.0241(9) 0.0196(9) 0.0254(10) 0.0074(8) 0.0072(8) 0.0106(8) C4 0.0297(10) 0.0136(9) 0.0226(9) -0.0022(7) 0.0107(8) 0.0035(7) C5 0.0352(11) 0.0140(9) 0.0227(9) -0.0007(7) 0.0079(8) -0.0071(8) C6 0.0246(10) 0.0241(10) 0.0225(9) -0.0050(8) 0.0076(8) -0.0103(8) C7 0.0153(8) 0.0235(10) 0.0216(9) -0.0050(7) 0.0063(7) -0.0033(7) C8 0.0155(8) 0.0134(8) 0.0147(8) -0.0007(6) 0.0036(6) 0.0014(6) C9 0.0141(8) 0.0144(8) 0.0147(8) 0.0029(6) 0.0072(6) 0.0011(6) C10 0.0182(8) 0.0143(8) 0.0154(8) -0.0028(6) 0.0070(7) 0.0010(6) C11 0.0211(9) 0.0209(9) 0.0161(8) -0.0013(7) 0.0082(7) 0.0041(7) C12 0.0183(9) 0.0298(11) 0.0187(9) -0.0054(8) 0.0056(7) 0.0051(8) C13 0.0184(9) 0.0274(10) 0.0211(9) -0.0132(8) 0.0094(7) -0.0057(8) C14 0.0257(9) 0.0189(9) 0.0184(9) -0.0053(7) 0.0118(7) -0.0043(7) C15 0.0205(9) 0.0153(9) 0.0158(8) -0.0039(7) 0.0071(7) -0.0016(7) C16 0.0265(10) 0.0355(12) 0.0301(11) 0.0149(9) 0.0116(9) 0.0137(9) C17 0.0231(10) 0.0402(13) 0.0303(11) -0.0173(9) 0.0138(9) -0.0105(9) C18 0.0271(10) 0.0264(10) 0.0203(9) 0.0068(8) 0.0103(8) 0.0041(8) C19 0.0410(12) 0.0134(9) 0.0346(12) -0.0033(8) 0.0034(10) -0.0071(9) C20 0.0295(10) 0.0247(11) 0.0340(11) -0.0174(9) 0.0096(9) -0.0041(9) C21 0.0278(10) 0.0262(10) 0.0192(9) -0.0078(8) 0.0040(8) -0.0089(8) C22 0.0184(9) 0.0270(11) 0.0362(12) -0.0117(9) 0.0047(8) -0.0084(8) C23 0.0376(12) 0.0298(12) 0.0346(12) -0.0109(9) 0.0162(10) -0.0213(10) N1 0.0118(7) 0.0150(7) 0.0161(7) 0.0025(6) 0.0038(6) 0.0017(5) N2 0.0171(7) 0.0134(7) 0.0197(8) 0.0010(6) 0.0058(6) 0.0030(6) Cr1 0.01411(13) 0.01156(13) 0.01447(13) -0.00130(10) 0.00493(10) -0.00101(10) I1 0.02778(7) 0.01725(7) 0.01806(7) 0.00224(4) 0.01102(5) 0.00292(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 1.480(2) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.506(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.465(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.471(2) . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.524(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.540(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.503(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N1 1.313(2) . ? C9 N2 1.350(2) . ? C10 C11 1.416(3) . ? C10 C15 1.420(3) . ? C10 Cr1 2.1188(18) . ? C11 C12 1.402(3) . ? C11 C16 1.510(3) . ? C12 C13 1.387(3) . ? C12 H12 0.9500 . ? C13 C14 1.384(3) . ? C13 C17 1.510(3) . ? C14 C15 1.398(3) . ? C14 H14 0.9500 . ? C15 C18 1.510(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.394(3) . ? C19 C23 1.405(3) . ? C19 Cr1 2.269(2) . ? C19 H19 0.9500 . ? C20 C21 1.415(3) . ? C20 Cr1 2.242(2) . ? C20 H20 0.9500 . ? C21 C22 1.415(3) . ? C21 Cr1 2.2500(19) . ? C21 H21 0.9500 . ? C22 C23 1.388(3) . ? C22 Cr1 2.332(2) . ? C22 H22 0.9500 . ? C23 Cr1 2.333(2) . ? C23 H23 0.9500 . ? N1 Cr1 2.0901(15) . ? Cr1 I1 2.7545(3) . ? 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 111.83(15) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C1 109.05(16) . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C2 109.60(15) . . ? N2 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C5 113.48(15) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 113.13(16) . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 C7 113.80(16) . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 114.63(15) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 111.56(15) . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 N2 124.34(16) . . ? N1 C9 C8 119.58(15) . . ? N2 C9 C8 116.01(15) . . ? C11 C10 C15 115.91(16) . . ? C11 C10 Cr1 122.77(13) . . ? C15 C10 Cr1 121.32(13) . . ? C12 C11 C10 121.22(18) . . ? C12 C11 C16 116.43(17) . . ? C10 C11 C16 122.35(17) . . ? C13 C12 C11 122.14(18) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C12 117.00(17) . . ? C14 C13 C17 120.87(19) . . ? C12 C13 C17 122.13(19) . . ? C13 C14 C15 122.54(18) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C14 C15 C10 120.97(17) . . ? C14 C15 C18 115.55(17) . . ? C10 C15 C18 123.47(17) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C23 108.2(2) . . ? C20 C19 Cr1 70.95(12) . . ? C23 C19 Cr1 74.76(12) . . ? C20 C19 H19 125.9 . . ? C23 C19 H19 125.9 . . ? Cr1 C19 H19 120.2 . . ? C19 C20 C21 107.9(2) . . ? C19 C20 Cr1 73.05(12) . . ? C21 C20 Cr1 71.95(11) . . ? C19 C20 H20 126.1 . . ? C21 C20 H20 126.1 . . ? Cr1 C20 H20 120.7 . . ? C22 C21 C20 107.39(19) . . ? C22 C21 Cr1 75.20(12) . . ? C20 C21 Cr1 71.33(11) . . ? C22 C21 H21 126.3 . . ? C20 C21 H21 126.3 . . ? Cr1 C21 H21 119.1 . . ? C23 C22 C21 108.0(2) . . ? C23 C22 Cr1 72.75(12) . . ? C21 C22 Cr1 68.88(11) . . ? C23 C22 H22 126.0 . . ? C21 C22 H22 126.0 . . ? Cr1 C22 H22 124.0 . . ? C22 C23 C19 108.5(2) . . ? C22 C23 Cr1 72.63(12) . . ? C19 C23 Cr1 69.74(12) . . ? C22 C23 H23 125.7 . . ? C19 C23 H23 125.7 . . ? Cr1 C23 H23 123.5 . . ? C9 N1 C1 116.11(15) . . ? C9 N1 Cr1 127.51(12) . . ? C1 N1 Cr1 115.94(12) . . ? C9 N2 C3 122.65(16) . . ? C9 N2 C4 122.72(15) . . ? C3 N2 C4 113.93(15) . . ? N1 Cr1 C10 95.97(6) . . ? N1 Cr1 C20 139.65(7) . . ? C10 Cr1 C20 83.49(7) . . ? N1 Cr1 C21 105.11(7) . . ? C10 Cr1 C21 100.19(7) . . ? C20 Cr1 C21 36.72(8) . . ? N1 Cr1 C19 155.90(7) . . ? C10 Cr1 C19 105.20(8) . . ? C20 Cr1 C19 36.00(9) . . ? C21 Cr1 C19 60.34(8) . . ? N1 Cr1 C22 97.63(7) . . ? C10 Cr1 C22 136.10(7) . . ? C20 Cr1 C22 59.78(8) . . ? C21 Cr1 C22 35.92(8) . . ? C19 Cr1 C22 59.01(8) . . ? N1 Cr1 C23 121.37(8) . . ? C10 Cr1 C23 140.06(8) . . ? C20 Cr1 C23 59.36(8) . . ? C21 Cr1 C23 59.27(8) . . ? C19 Cr1 C23 35.50(9) . . ? C22 Cr1 C23 34.62(8) . . ? N1 Cr1 I1 91.71(4) . . ? C10 Cr1 I1 111.06(5) . . ? C20 Cr1 I1 126.26(6) . . ? C21 Cr1 I1 142.70(6) . . ? C19 Cr1 I1 91.30(6) . . ? C22 Cr1 I1 110.01(6) . . ? C23 Cr1 I1 83.50(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -58.4(2) . . . . ? C1 C2 C3 N2 47.3(2) . . . . ? N2 C4 C5 C6 -80.0(2) . . . . ? C4 C5 C6 C7 56.5(2) . . . . ? C5 C6 C7 C8 -61.9(2) . . . . ? C6 C7 C8 C9 86.68(19) . . . . ? C7 C8 C9 N1 111.19(18) . . . . ? C7 C8 C9 N2 -65.9(2) . . . . ? C15 C10 C11 C12 5.0(3) . . . . ? Cr1 C10 C11 C12 -174.14(14) . . . . ? C15 C10 C11 C16 -174.84(18) . . . . ? Cr1 C10 C11 C16 6.0(3) . . . . ? C10 C11 C12 C13 -1.7(3) . . . . ? C16 C11 C12 C13 178.15(18) . . . . ? C11 C12 C13 C14 -2.1(3) . . . . ? C11 C12 C13 C17 178.38(18) . . . . ? C12 C13 C14 C15 2.3(3) . . . . ? C17 C13 C14 C15 -178.15(17) . . . . ? C13 C14 C15 C10 1.2(3) . . . . ? C13 C14 C15 C18 -177.70(17) . . . . ? C11 C10 C15 C14 -4.8(3) . . . . ? Cr1 C10 C15 C14 174.38(13) . . . . ? C11 C10 C15 C18 174.07(17) . . . . ? Cr1 C10 C15 C18 -6.8(2) . . . . ? C23 C19 C20 C21 2.1(2) . . . . ? Cr1 C19 C20 C21 -63.98(14) . . . . ? C23 C19 C20 Cr1 66.04(15) . . . . ? C19 C20 C21 C22 -2.4(2) . . . . ? Cr1 C20 C21 C22 -67.15(14) . . . . ? C19 C20 C21 Cr1 64.70(14) . . . . ? C20 C21 C22 C23 1.9(2) . . . . ? Cr1 C21 C22 C23 -62.64(14) . . . . ? C20 C21 C22 Cr1 64.55(13) . . . . ? C21 C22 C23 C19 -0.7(2) . . . . ? Cr1 C22 C23 C19 -60.83(15) . . . . ? C21 C22 C23 Cr1 60.17(14) . . . . ? C20 C19 C23 C22 -0.9(2) . . . . ? Cr1 C19 C23 C22 62.67(15) . . . . ? C20 C19 C23 Cr1 -63.54(14) . . . . ? N2 C9 N1 C1 2.8(3) . . . . ? C8 C9 N1 C1 -173.95(15) . . . . ? N2 C9 N1 Cr1 -169.19(13) . . . . ? C8 C9 N1 Cr1 14.0(2) . . . . ? C2 C1 N1 C9 33.2(2) . . . . ? C2 C1 N1 Cr1 -153.80(13) . . . . ? N1 C9 N2 C3 -13.1(3) . . . . ? C8 C9 N2 C3 163.81(16) . . . . ? N1 C9 N2 C4 177.06(16) . . . . ? C8 C9 N2 C4 -6.1(2) . . . . ? C2 C3 N2 C9 -14.3(2) . . . . ? C2 C3 N2 C4 156.36(16) . . . . ? C5 C4 N2 C9 74.8(2) . . . . ? C5 C4 N2 C3 -95.87(19) . . . . ? C9 N1 Cr1 C10 -58.25(15) . . . . ? C1 N1 Cr1 C10 129.72(13) . . . . ? C9 N1 Cr1 C20 -145.21(15) . . . . ? C1 N1 Cr1 C20 42.76(18) . . . . ? C9 N1 Cr1 C21 -160.52(15) . . . . ? C1 N1 Cr1 C21 27.45(14) . . . . ? C9 N1 Cr1 C19 150.16(19) . . . . ? C1 N1 Cr1 C19 -21.9(2) . . . . ? C9 N1 Cr1 C22 163.59(15) . . . . ? C1 N1 Cr1 C22 -8.43(14) . . . . ? C9 N1 Cr1 C23 136.57(15) . . . . ? C1 N1 Cr1 C23 -35.46(15) . . . . ? C9 N1 Cr1 I1 53.14(15) . . . . ? C1 N1 Cr1 I1 -118.89(12) . . . . ? C11 C10 Cr1 N1 132.41(15) . . . . ? C15 C10 Cr1 N1 -46.68(15) . . . . ? C11 C10 Cr1 C20 -88.19(16) . . . . ? C15 C10 Cr1 C20 92.72(15) . . . . ? C11 C10 Cr1 C21 -121.03(15) . . . . ? C15 C10 Cr1 C21 59.88(15) . . . . ? C11 C10 Cr1 C19 -59.21(16) . . . . ? C15 C10 Cr1 C19 121.71(15) . . . . ? C11 C10 Cr1 C22 -120.06(16) . . . . ? C15 C10 Cr1 C22 60.85(19) . . . . ? C11 C10 Cr1 C23 -67.5(2) . . . . ? C15 C10 Cr1 C23 113.43(16) . . . . ? C11 C10 Cr1 I1 38.25(16) . . . . ? C15 C10 Cr1 I1 -140.84(13) . . . . ? C19 C20 Cr1 N1 -141.13(13) . . . . ? C21 C20 Cr1 N1 -25.23(18) . . . . ? C19 C20 Cr1 C10 127.30(14) . . . . ? C21 C20 Cr1 C10 -116.80(13) . . . . ? C19 C20 Cr1 C21 -115.90(19) . . . . ? C21 C20 Cr1 C19 115.90(19) . . . . ? C19 C20 Cr1 C22 -77.77(15) . . . . ? C21 C20 Cr1 C22 38.14(12) . . . . ? C19 C20 Cr1 C23 -37.40(14) . . . . ? C21 C20 Cr1 C23 78.50(14) . . . . ? C19 C20 Cr1 I1 15.90(16) . . . . ? C21 C20 Cr1 I1 131.80(11) . . . . ? C22 C21 Cr1 N1 -82.06(13) . . . . ? C20 C21 Cr1 N1 163.39(12) . . . . ? C22 C21 Cr1 C10 178.85(13) . . . . ? C20 C21 Cr1 C10 64.30(14) . . . . ? C22 C21 Cr1 C20 114.55(19) . . . . ? C22 C21 Cr1 C19 77.07(14) . . . . ? C20 C21 Cr1 C19 -37.48(13) . . . . ? C20 C21 Cr1 C22 -114.55(19) . . . . ? C22 C21 Cr1 C23 35.77(13) . . . . ? C20 C21 Cr1 C23 -78.78(14) . . . . ? C22 C21 Cr1 I1 31.86(18) . . . . ? C20 C21 Cr1 I1 -82.69(15) . . . . ? C20 C19 Cr1 N1 95.6(2) . . . . ? C23 C19 Cr1 N1 -20.2(3) . . . . ? C20 C19 Cr1 C10 -54.98(14) . . . . ? C23 C19 Cr1 C10 -170.85(13) . . . . ? C23 C19 Cr1 C20 -115.9(2) . . . . ? C20 C19 Cr1 C21 38.24(13) . . . . ? C23 C19 Cr1 C21 -77.62(14) . . . . ? C20 C19 Cr1 C22 80.07(14) . . . . ? C23 C19 Cr1 C22 -35.79(13) . . . . ? C20 C19 Cr1 C23 115.9(2) . . . . ? C20 C19 Cr1 I1 -167.24(13) . . . . ? C23 C19 Cr1 I1 76.90(13) . . . . ? C23 C22 Cr1 N1 -136.93(13) . . . . ? C21 C22 Cr1 N1 105.27(13) . . . . ? C23 C22 Cr1 C10 116.18(15) . . . . ? C21 C22 Cr1 C10 -1.63(18) . . . . ? C23 C22 Cr1 C20 78.80(15) . . . . ? C21 C22 Cr1 C20 -39.01(13) . . . . ? C23 C22 Cr1 C21 117.80(19) . . . . ? C23 C22 Cr1 C19 36.72(14) . . . . ? C21 C22 Cr1 C19 -81.08(14) . . . . ? C21 C22 Cr1 C23 -117.80(19) . . . . ? C23 C22 Cr1 I1 -42.29(14) . . . . ? C21 C22 Cr1 I1 -160.09(11) . . . . ? C22 C23 Cr1 N1 52.44(15) . . . . ? C19 C23 Cr1 N1 170.49(13) . . . . ? C22 C23 Cr1 C10 -104.21(16) . . . . ? C19 C23 Cr1 C10 13.8(2) . . . . ? C22 C23 Cr1 C20 -80.11(14) . . . . ? C19 C23 Cr1 C20 37.94(14) . . . . ? C22 C23 Cr1 C21 -37.13(13) . . . . ? C19 C23 Cr1 C21 80.91(15) . . . . ? C22 C23 Cr1 C19 -118.0(2) . . . . ? C19 C23 Cr1 C22 118.0(2) . . . . ? C22 C23 Cr1 I1 140.48(13) . . . . ? C19 C23 Cr1 I1 -101.48(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.860 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.070 data_10_CpCrMes_dimer _database_code_depnum_ccdc_archive 'CCDC 791390' #TrackingRef '- CpCrMes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cr2' _chemical_formula_weight 472.54 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' Cr Cr 0.3209 0.6236 '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 8.3398(8) _cell_length_b 11.8870(12) _cell_length_c 12.6085(12) _cell_angle_alpha 94.928(5) _cell_angle_beta 93.544(4) _cell_angle_gamma 108.619(5) _cell_volume 1174.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8667 _cell_measurement_theta_min 2.926 _cell_measurement_theta_max 27.88 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.160 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details ? _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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16929 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.07 _reflns_number_total 5590 _reflns_number_gt 4831 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.7798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5590 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.005 _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 C1 C 0.6375(4) 0.3894(2) -0.0787(2) 0.0335(6) Uani 1 1 d . . . C2 C 0.7546(4) 0.3502(2) -0.0240(2) 0.0303(6) Uani 1 1 d . . . H2 H 0.8636 0.4057 0.0003 0.036 Uiso 1 1 calc R . . C3 C 0.7178(3) 0.2321(2) -0.0033(2) 0.0270(5) Uani 1 1 d . . . C4 C 0.5566(3) 0.1461(2) -0.0383(2) 0.0255(5) Uani 1 1 d . . . C5 C 0.4386(3) 0.1880(2) -0.0965(2) 0.0256(5) Uani 1 1 d . . . C6 C 0.4807(4) 0.3066(2) -0.1156(2) 0.0317(6) Uani 1 1 d . . . H6 H 0.4000 0.3317 -0.1551 0.038 Uiso 1 1 calc R . . C7 C 0.6782(5) 0.5185(3) -0.0965(3) 0.0523(9) Uani 1 1 d . . . H7A H 0.5809 0.5295 -0.1366 0.078 Uiso 1 1 calc R . . H7B H 0.7778 0.5424 -0.1372 0.078 Uiso 1 1 calc R . . H7C H 0.7026 0.5679 -0.0274 0.078 Uiso 1 1 calc R . . C8 C 0.8550(4) 0.2000(3) 0.0575(3) 0.0398(7) Uani 1 1 d . . . H8A H 0.9622 0.2663 0.0620 0.060 Uiso 1 1 calc R . . H8B H 0.8686 0.1282 0.0204 0.060 Uiso 1 1 calc R . . H8C H 0.8234 0.1846 0.1298 0.060 Uiso 1 1 calc R . . C9 C 0.2632(4) 0.1052(3) -0.1385(2) 0.0366(6) Uani 1 1 d . . . H9A H 0.2068 0.1471 -0.1838 0.055 Uiso 1 1 calc R . . H9B H 0.1963 0.0801 -0.0784 0.055 Uiso 1 1 calc R . . H9C H 0.2728 0.0349 -0.1807 0.055 Uiso 1 1 calc R . . C10 C 0.4079(5) 0.0276(3) 0.2625(2) 0.0475(8) Uani 1 1 d . . . H10 H 0.4536 -0.0209 0.3027 0.057 Uiso 1 1 calc R . . C11 C 0.2452(4) -0.0094(3) 0.2068(3) 0.0499(8) Uani 1 1 d . . . H11 H 0.1627 -0.0867 0.2020 0.060 Uiso 1 1 calc R . . C12 C 0.2281(4) 0.0885(4) 0.1600(3) 0.0493(9) Uani 1 1 d . . . H12 H 0.1295 0.0910 0.1196 0.059 Uiso 1 1 calc R . . C13 C 0.3816(5) 0.1826(3) 0.1829(3) 0.0472(8) Uani 1 1 d . . . H13 H 0.4073 0.2587 0.1574 0.057 Uiso 1 1 calc R . . C14 C 0.4909(4) 0.1457(3) 0.2498(2) 0.0436(7) Uani 1 1 d . . . H14 H 0.6013 0.1929 0.2806 0.052 Uiso 1 1 calc R . . C15 C -0.1816(3) 0.0920(2) 0.4423(2) 0.0290(5) Uani 1 1 d . . . C16 C -0.0482(3) 0.1593(2) 0.3902(2) 0.0286(5) Uani 1 1 d . . . H16 H 0.0143 0.1200 0.3493 0.034 Uiso 1 1 calc R . . C17 C -0.0036(3) 0.2832(2) 0.3965(2) 0.0258(5) Uani 1 1 d . . . C18 C -0.0941(3) 0.3465(2) 0.4553(2) 0.0255(5) Uani 1 1 d . . . C19 C -0.2346(3) 0.2750(2) 0.5040(2) 0.0287(5) Uani 1 1 d . . . C20 C -0.2739(3) 0.1515(2) 0.4979(2) 0.0295(5) Uani 1 1 d . . . H20 H -0.3671 0.1067 0.5331 0.035 Uiso 1 1 calc R . . C21 C -0.2247(4) -0.0413(2) 0.4395(3) 0.0402(7) Uani 1 1 d . . . H21A H -0.2647 -0.0663 0.5080 0.060 Uiso 1 1 calc R . . H21B H -0.1232 -0.0634 0.4271 0.060 Uiso 1 1 calc R . . H21C H -0.3142 -0.0811 0.3817 0.060 Uiso 1 1 calc R . . C22 C 0.1450(4) 0.3477(3) 0.3385(3) 0.0386(7) Uani 1 1 d . . . H22A H 0.2489 0.3730 0.3876 0.058 Uiso 1 1 calc R . . H22B H 0.1261 0.4181 0.3121 0.058 Uiso 1 1 calc R . . H22C H 0.1568 0.2943 0.2781 0.058 Uiso 1 1 calc R . . C23 C -0.3478(4) 0.3289(3) 0.5645(3) 0.0513(9) Uani 1 1 d . . . H23A H -0.3078 0.4158 0.5632 0.077 Uiso 1 1 calc R . . H23B H -0.3446 0.3106 0.6387 0.077 Uiso 1 1 calc R . . H23C H -0.4647 0.2955 0.5308 0.077 Uiso 1 1 calc R . . C24 C 0.1069(5) 0.3308(3) 0.6837(3) 0.0481(8) Uani 1 1 d . . . H24 H 0.0307 0.2514 0.6684 0.058 Uiso 1 1 calc R . . C25 C 0.2597(5) 0.3778(3) 0.6407(3) 0.0513(9) Uani 1 1 d . . . H25 H 0.3088 0.3351 0.5926 0.062 Uiso 1 1 calc R . . C26 C 0.3296(4) 0.4979(4) 0.6798(3) 0.0526(9) Uani 1 1 d . . . H26 H 0.4336 0.5517 0.6624 0.063 Uiso 1 1 calc R . . C27 C 0.2201(5) 0.5256(3) 0.7488(3) 0.0512(9) Uani 1 1 d . . . H27 H 0.2349 0.6019 0.7857 0.061 Uiso 1 1 calc R . . C28 C 0.0849(5) 0.4215(3) 0.7540(3) 0.0499(8) Uani 1 1 d . . . H28 H -0.0063 0.4133 0.7975 0.060 Uiso 1 1 calc R . . Cr01 Cr 0.07840(5) 0.47533(3) 0.58010(3) 0.02380(10) Uani 1 1 d . . . Cr02 Cr 0.44315(5) 0.03374(3) 0.08334(3) 0.02215(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0449(16) 0.0235(12) 0.0345(14) 0.0101(11) 0.0119(12) 0.0112(11) C2 0.0317(13) 0.0233(12) 0.0328(14) 0.0049(10) 0.0066(11) 0.0034(10) C3 0.0275(12) 0.0246(12) 0.0284(13) 0.0040(10) 0.0013(10) 0.0077(10) C4 0.0262(12) 0.0218(11) 0.0290(13) 0.0060(9) -0.0007(10) 0.0085(9) C5 0.0279(12) 0.0272(12) 0.0239(12) 0.0076(10) 0.0015(10) 0.0109(10) C6 0.0379(15) 0.0320(14) 0.0312(14) 0.0118(11) 0.0036(11) 0.0176(12) C7 0.065(2) 0.0280(15) 0.067(2) 0.0216(15) 0.0145(19) 0.0139(15) C8 0.0277(14) 0.0320(14) 0.0537(19) 0.0075(13) -0.0098(13) 0.0033(11) C9 0.0317(14) 0.0377(15) 0.0412(16) 0.0100(12) -0.0094(12) 0.0131(12) C10 0.059(2) 0.067(2) 0.0282(15) 0.0142(15) 0.0118(14) 0.0334(18) C11 0.0455(19) 0.055(2) 0.0461(19) 0.0019(16) 0.0229(15) 0.0097(16) C12 0.0403(17) 0.077(2) 0.0398(17) -0.0083(16) 0.0014(14) 0.0366(18) C13 0.071(2) 0.0421(17) 0.0392(17) -0.0024(14) 0.0121(16) 0.0343(17) C14 0.0462(18) 0.0522(19) 0.0292(15) -0.0085(13) 0.0002(13) 0.0155(15) C15 0.0324(14) 0.0238(12) 0.0298(13) 0.0044(10) -0.0064(11) 0.0091(10) C16 0.0336(14) 0.0281(13) 0.0276(13) 0.0002(10) 0.0013(11) 0.0160(11) C17 0.0292(13) 0.0267(12) 0.0231(12) 0.0019(9) 0.0034(10) 0.0115(10) C18 0.0265(12) 0.0225(11) 0.0269(12) 0.0013(9) 0.0044(10) 0.0074(10) C19 0.0259(12) 0.0267(12) 0.0326(14) 0.0011(10) 0.0047(10) 0.0074(10) C20 0.0278(13) 0.0252(12) 0.0328(14) 0.0074(10) 0.0017(11) 0.0042(10) C21 0.0431(17) 0.0250(13) 0.0510(18) 0.0056(12) -0.0035(14) 0.0101(12) C22 0.0465(17) 0.0295(14) 0.0437(17) 0.0035(12) 0.0230(14) 0.0147(12) C23 0.0422(18) 0.0326(15) 0.079(3) 0.0039(16) 0.0355(18) 0.0076(13) C24 0.058(2) 0.0367(16) 0.0501(19) 0.0124(14) -0.0150(16) 0.0176(15) C25 0.059(2) 0.066(2) 0.0440(18) 0.0021(16) -0.0087(16) 0.0448(19) C26 0.0337(17) 0.068(2) 0.050(2) 0.0155(17) -0.0096(14) 0.0091(16) C27 0.074(2) 0.0424(18) 0.0354(17) -0.0032(14) -0.0156(16) 0.0218(17) C28 0.058(2) 0.071(2) 0.0326(16) 0.0225(16) 0.0103(15) 0.0317(18) Cr01 0.0259(2) 0.02196(19) 0.0253(2) 0.00251(15) 0.00329(16) 0.01011(16) Cr02 0.0233(2) 0.02202(19) 0.0228(2) 0.00310(15) 0.00169(15) 0.00959(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 C1 C2 1.382(4) . ? C1 C6 1.386(4) . ? C1 C7 1.503(4) . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.420(4) . ? C3 C8 1.504(4) . ? C4 C5 1.429(3) . ? C4 Cr02 2.165(2) 2_655 ? C4 Cr02 2.181(3) . ? C5 C6 1.386(4) . ? C5 C9 1.512(4) . ? C6 H6 0.9500 . ? 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 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.381(5) . ? C10 C11 1.405(5) . ? C10 Cr02 2.301(3) . ? C10 H10 0.9500 . ? C11 C12 1.392(5) . ? C11 Cr02 2.308(3) . ? C11 H11 0.9500 . ? C12 C13 1.400(5) . ? C12 Cr02 2.330(3) . ? C12 H12 0.9500 . ? C13 C14 1.399(5) . ? C13 Cr02 2.291(3) . ? C13 H13 0.9500 . ? C14 Cr02 2.326(3) . ? C14 H14 0.9500 . ? C15 C20 1.383(4) . ? C15 C16 1.387(4) . ? C15 C21 1.506(4) . ? C16 C17 1.392(4) . ? C16 H16 0.9500 . ? C17 C18 1.422(3) . ? C17 C22 1.503(4) . ? C18 C19 1.420(3) . ? C18 Cr01 2.166(3) 2_566 ? C18 Cr01 2.189(3) . ? C19 C20 1.392(4) . ? C19 C23 1.509(4) . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.383(5) . ? C24 C28 1.400(5) . ? C24 Cr01 2.307(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(5) . ? C25 Cr01 2.312(3) . ? C25 H25 0.9500 . ? C26 C27 1.393(5) . ? C26 Cr01 2.301(3) . ? C26 H26 0.9500 . ? C27 C28 1.393(5) . ? C27 Cr01 2.302(3) . ? C27 H27 0.9500 . ? C28 Cr01 2.338(3) . ? C28 H28 0.9500 . ? Cr01 C18 2.166(3) 2_566 ? Cr01 Cr01 2.5496(8) 2_566 ? Cr02 C4 2.165(2) 2_655 ? Cr02 Cr02 2.5301(8) 2_655 ? 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 C2 C1 C6 118.2(2) . . ? C2 C1 C7 120.9(3) . . ? C6 C1 C7 120.9(3) . . ? C1 C2 C3 122.0(3) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 120.9(2) . . ? C2 C3 C8 117.2(2) . . ? C4 C3 C8 121.9(2) . . ? C3 C4 C5 116.2(2) . . ? C3 C4 Cr02 115.81(18) . 2_655 ? C5 C4 Cr02 118.28(18) . 2_655 ? C3 C4 Cr02 114.11(18) . . ? C5 C4 Cr02 113.20(17) . . ? Cr02 C4 Cr02 71.21(8) 2_655 . ? C6 C5 C4 121.0(2) . . ? C6 C5 C9 117.6(2) . . ? C4 C5 C9 121.4(2) . . ? C1 C6 C5 121.7(3) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 109.4(3) . . ? C14 C10 Cr02 73.66(18) . . ? C11 C10 Cr02 72.52(18) . . ? C14 C10 H10 125.3 . . ? C11 C10 H10 125.3 . . ? Cr02 C10 H10 120.2 . . ? C12 C11 C10 107.0(3) . . ? C12 C11 Cr02 73.40(18) . . ? C10 C11 Cr02 71.97(18) . . ? C12 C11 H11 126.5 . . ? C10 C11 H11 126.5 . . ? Cr02 C11 H11 120.0 . . ? C11 C12 C13 108.0(3) . . ? C11 C12 Cr02 71.68(18) . . ? C13 C12 Cr02 70.86(17) . . ? C11 C12 H12 126.0 . . ? C13 C12 H12 126.0 . . ? Cr02 C12 H12 123.1 . . ? C12 C13 C14 108.5(3) . . ? C12 C13 Cr02 73.88(17) . . ? C14 C13 Cr02 73.75(17) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? Cr02 C13 H13 118.5 . . ? C10 C14 C13 107.0(3) . . ? C10 C14 Cr02 71.61(18) . . ? C13 C14 Cr02 70.98(17) . . ? C10 C14 H14 126.5 . . ? C13 C14 H14 126.5 . . ? Cr02 C14 H14 122.6 . . ? C20 C15 C16 117.8(2) . . ? C20 C15 C21 120.8(3) . . ? C16 C15 C21 121.4(3) . . ? C15 C16 C17 121.5(2) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C18 121.7(2) . . ? C16 C17 C22 117.2(2) . . ? C18 C17 C22 121.1(2) . . ? C19 C18 C17 115.6(2) . . ? C19 C18 Cr01 120.96(18) . 2_566 ? C17 C18 Cr01 119.37(18) . 2_566 ? C19 C18 Cr01 108.05(17) . . ? C17 C18 Cr01 110.01(17) . . ? Cr01 C18 Cr01 71.67(8) 2_566 . ? C20 C19 C18 121.2(2) . . ? C20 C19 C23 117.0(2) . . ? C18 C19 C23 121.7(2) . . ? C15 C20 C19 122.1(2) . . ? C15 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C28 107.6(3) . . ? C25 C24 Cr01 72.79(19) . . ? C28 C24 Cr01 73.67(18) . . ? C25 C24 H24 126.2 . . ? C28 C24 H24 126.2 . . ? Cr01 C24 H24 119.3 . . ? C24 C25 C26 108.5(3) . . ? C24 C25 Cr01 72.37(18) . . ? C26 C25 Cr01 72.02(19) . . ? C24 C25 H25 125.7 . . ? C26 C25 H25 125.7 . . ? Cr01 C25 H25 121.6 . . ? C25 C26 C27 108.0(3) . . ? C25 C26 Cr01 72.88(19) . . ? C27 C26 Cr01 72.40(19) . . ? C25 C26 H26 126.0 . . ? C27 C26 H26 126.0 . . ? Cr01 C26 H26 120.5 . . ? C28 C27 C26 107.7(3) . . ? C28 C27 Cr01 73.97(19) . . ? C26 C27 Cr01 72.38(19) . . ? C28 C27 H27 126.1 . . ? C26 C27 H27 126.1 . . ? Cr01 C27 H27 119.4 . . ? C27 C28 C24 108.0(3) . . ? C27 C28 Cr01 71.11(18) . . ? C24 C28 Cr01 71.25(18) . . ? C27 C28 H28 126.0 . . ? C24 C28 H28 126.0 . . ? Cr01 C28 H28 123.3 . . ? C18 Cr01 C18 108.33(8) 2_566 . ? C18 Cr01 C27 98.08(11) 2_566 . ? C18 Cr01 C27 151.94(11) . . ? C18 Cr01 C26 105.30(12) 2_566 . ? C18 Cr01 C26 137.92(12) . . ? C27 Cr01 C26 35.22(13) . . ? C18 Cr01 C24 156.57(11) 2_566 . ? C18 Cr01 C24 94.12(11) . . ? C27 Cr01 C24 58.73(12) . . ? C26 Cr01 C24 58.49(13) . . ? C18 Cr01 C25 137.98(13) 2_566 . ? C18 Cr01 C25 104.16(12) . . ? C27 Cr01 C25 58.42(13) . . ? C26 Cr01 C25 35.10(13) . . ? C24 Cr01 C25 34.84(13) . . ? C18 Cr01 C28 123.24(12) 2_566 . ? C18 Cr01 C28 118.13(12) . . ? C27 Cr01 C28 34.92(13) . . ? C26 Cr01 C28 58.00(13) . . ? C24 Cr01 C28 35.08(12) . . ? C25 Cr01 C28 57.77(13) . . ? C18 Cr01 Cr01 54.58(7) 2_566 2_566 ? C18 Cr01 Cr01 53.76(7) . 2_566 ? C27 Cr01 Cr01 151.29(9) . 2_566 ? C26 Cr01 Cr01 149.46(10) . 2_566 ? C24 Cr01 Cr01 147.27(9) . 2_566 ? C25 Cr01 Cr01 147.26(9) . 2_566 ? C28 Cr01 Cr01 150.52(9) . 2_566 ? C4 Cr02 C4 108.79(8) 2_655 . ? C4 Cr02 C13 156.54(12) 2_655 . ? C4 Cr02 C13 94.54(11) . . ? C4 Cr02 C10 100.76(11) 2_655 . ? C4 Cr02 C10 145.22(12) . . ? C13 Cr02 C10 58.27(12) . . ? C4 Cr02 C11 98.22(12) 2_655 . ? C4 Cr02 C11 148.04(12) . . ? C13 Cr02 C11 58.82(13) . . ? C10 Cr02 C11 35.51(13) . . ? C4 Cr02 C14 130.97(11) 2_655 . ? C4 Cr02 C14 110.60(11) . . ? C13 Cr02 C14 35.27(12) . . ? C10 Cr02 C14 34.72(12) . . ? C11 Cr02 C14 58.77(12) . . ? C4 Cr02 C12 126.81(12) 2_655 . ? C4 Cr02 C12 113.12(12) . . ? C13 Cr02 C12 35.26(13) . . ? C10 Cr02 C12 58.10(12) . . ? C11 Cr02 C12 34.93(13) . . ? C14 Cr02 C12 58.38(12) . . ? C4 Cr02 Cr02 54.68(7) 2_655 2_655 ? C4 Cr02 Cr02 54.11(7) . 2_655 ? C13 Cr02 Cr02 148.56(9) . 2_655 ? C10 Cr02 Cr02 150.18(9) . 2_655 ? C11 Cr02 Cr02 148.60(9) . 2_655 ? C14 Cr02 Cr02 149.80(9) . 2_655 ? C12 Cr02 Cr02 148.33(9) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.5(4) . . . . ? C7 C1 C2 C3 177.8(3) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C1 C2 C3 C8 -179.7(3) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C8 C3 C4 C5 -179.2(3) . . . . ? C2 C3 C4 Cr02 146.6(2) . . . 2_655 ? C8 C3 C4 Cr02 -33.6(3) . . . 2_655 ? C2 C3 C4 Cr02 -133.5(2) . . . . ? C8 C3 C4 Cr02 46.3(3) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? Cr02 C4 C5 C6 -145.5(2) 2_655 . . . ? Cr02 C4 C5 C6 134.1(2) . . . . ? C3 C4 C5 C9 179.7(2) . . . . ? Cr02 C4 C5 C9 35.0(3) 2_655 . . . ? Cr02 C4 C5 C9 -45.4(3) . . . . ? C2 C1 C6 C5 1.7(4) . . . . ? C7 C1 C6 C5 -177.6(3) . . . . ? C4 C5 C6 C1 -0.5(4) . . . . ? C9 C5 C6 C1 178.9(3) . . . . ? C14 C10 C11 C12 -0.6(4) . . . . ? Cr02 C10 C11 C12 -65.6(2) . . . . ? C14 C10 C11 Cr02 64.9(2) . . . . ? C10 C11 C12 C13 2.7(4) . . . . ? Cr02 C11 C12 C13 -61.9(2) . . . . ? C10 C11 C12 Cr02 64.6(2) . . . . ? C11 C12 C13 C14 -3.7(4) . . . . ? Cr02 C12 C13 C14 -66.2(2) . . . . ? C11 C12 C13 Cr02 62.5(2) . . . . ? C11 C10 C14 C13 -1.7(4) . . . . ? Cr02 C10 C14 C13 62.5(2) . . . . ? C11 C10 C14 Cr02 -64.2(2) . . . . ? C12 C13 C14 C10 3.3(4) . . . . ? Cr02 C13 C14 C10 -63.0(2) . . . . ? C12 C13 C14 Cr02 66.3(2) . . . . ? C20 C15 C16 C17 2.3(4) . . . . ? C21 C15 C16 C17 -177.2(3) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C15 C16 C17 C22 179.0(3) . . . . ? C16 C17 C18 C19 -1.7(4) . . . . ? C22 C17 C18 C19 178.4(3) . . . . ? C16 C17 C18 Cr01 -159.3(2) . . . 2_566 ? C22 C17 C18 Cr01 20.8(3) . . . 2_566 ? C16 C17 C18 Cr01 121.0(2) . . . . ? C22 C17 C18 Cr01 -58.9(3) . . . . ? C17 C18 C19 C20 2.9(4) . . . . ? Cr01 C18 C19 C20 160.1(2) 2_566 . . . ? Cr01 C18 C19 C20 -120.8(2) . . . . ? C17 C18 C19 C23 -177.0(3) . . . . ? Cr01 C18 C19 C23 -19.8(4) 2_566 . . . ? Cr01 C18 C19 C23 59.3(3) . . . . ? C16 C15 C20 C19 -1.1(4) . . . . ? C21 C15 C20 C19 178.5(3) . . . . ? C18 C19 C20 C15 -1.6(4) . . . . ? C23 C19 C20 C15 178.3(3) . . . . ? C28 C24 C25 C26 -2.6(4) . . . . ? Cr01 C24 C25 C26 63.4(2) . . . . ? C28 C24 C25 Cr01 -66.0(2) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? Cr01 C25 C26 C27 64.4(2) . . . . ? C24 C25 C26 Cr01 -63.6(2) . . . . ? C25 C26 C27 C28 1.4(4) . . . . ? Cr01 C26 C27 C28 66.1(2) . . . . ? C25 C26 C27 Cr01 -64.7(2) . . . . ? C26 C27 C28 C24 -2.9(4) . . . . ? Cr01 C27 C28 C24 62.1(2) . . . . ? C26 C27 C28 Cr01 -65.0(2) . . . . ? C25 C24 C28 C27 3.4(4) . . . . ? Cr01 C24 C28 C27 -62.0(2) . . . . ? C25 C24 C28 Cr01 65.4(2) . . . . ? C19 C18 Cr01 C18 -117.52(19) . . . 2_566 ? C17 C18 Cr01 C18 115.42(19) . . . 2_566 ? Cr01 C18 Cr01 C18 0.0 2_566 . . 2_566 ? C19 C18 Cr01 C27 42.0(3) . . . . ? C17 C18 Cr01 C27 -85.1(3) . . . . ? Cr01 C18 Cr01 C27 159.5(2) 2_566 . . . ? C19 C18 Cr01 C26 101.1(2) . . . . ? C17 C18 Cr01 C26 -26.0(3) . . . . ? Cr01 C18 Cr01 C26 -141.42(15) 2_566 . . . ? C19 C18 Cr01 C24 55.7(2) . . . . ? C17 C18 Cr01 C24 -71.4(2) . . . . ? Cr01 C18 Cr01 C24 173.19(11) 2_566 . . . ? C19 C18 Cr01 C25 89.5(2) . . . . ? C17 C18 Cr01 C25 -37.5(2) . . . . ? Cr01 C18 Cr01 C25 -152.96(11) 2_566 . . . ? C19 C18 Cr01 C28 28.8(2) . . . . ? C17 C18 Cr01 C28 -98.3(2) . . . . ? Cr01 C18 Cr01 C28 146.30(11) 2_566 . . . ? C19 C18 Cr01 Cr01 -117.52(19) . . . 2_566 ? C17 C18 Cr01 Cr01 115.42(19) . . . 2_566 ? C28 C27 Cr01 C18 139.8(2) . . . 2_566 ? C26 C27 Cr01 C18 -105.1(2) . . . 2_566 ? C28 C27 Cr01 C18 -20.6(4) . . . . ? C26 C27 Cr01 C18 94.5(3) . . . . ? C28 C27 Cr01 C26 -115.1(3) . . . . ? C28 C27 Cr01 C24 -36.6(2) . . . . ? C26 C27 Cr01 C24 78.5(2) . . . . ? C28 C27 Cr01 C25 -77.7(2) . . . . ? C26 C27 Cr01 C25 37.4(2) . . . . ? C26 C27 Cr01 C28 115.1(3) . . . . ? C28 C27 Cr01 Cr01 123.4(2) . . . 2_566 ? C26 C27 Cr01 Cr01 -121.5(2) . . . 2_566 ? C25 C26 Cr01 C18 -161.9(2) . . . 2_566 ? C27 C26 Cr01 C18 82.3(2) . . . 2_566 ? C25 C26 Cr01 C18 -19.7(3) . . . . ? C27 C26 Cr01 C18 -135.6(2) . . . . ? C25 C26 Cr01 C27 115.9(3) . . . . ? C25 C26 Cr01 C24 36.7(2) . . . . ? C27 C26 Cr01 C24 -79.2(2) . . . . ? C27 C26 Cr01 C25 -115.9(3) . . . . ? C25 C26 Cr01 C28 78.2(2) . . . . ? C27 C26 Cr01 C28 -37.7(2) . . . . ? C25 C26 Cr01 Cr01 -117.8(2) . . . 2_566 ? C27 C26 Cr01 Cr01 126.3(2) . . . 2_566 ? C25 C24 Cr01 C18 -87.4(4) . . . 2_566 ? C28 C24 Cr01 C18 27.5(4) . . . 2_566 ? C25 C24 Cr01 C18 109.0(2) . . . . ? C28 C24 Cr01 C18 -136.1(2) . . . . ? C25 C24 Cr01 C27 -78.5(2) . . . . ? C28 C24 Cr01 C27 36.4(2) . . . . ? C25 C24 Cr01 C26 -37.0(2) . . . . ? C28 C24 Cr01 C26 78.0(2) . . . . ? C28 C24 Cr01 C25 114.9(3) . . . . ? C25 C24 Cr01 C28 -114.9(3) . . . . ? C25 C24 Cr01 Cr01 119.2(2) . . . 2_566 ? C28 C24 Cr01 Cr01 -125.9(2) . . . 2_566 ? C24 C25 Cr01 C18 143.6(2) . . . 2_566 ? C26 C25 Cr01 C18 26.7(3) . . . 2_566 ? C24 C25 Cr01 C18 -76.5(2) . . . . ? C26 C25 Cr01 C18 166.5(2) . . . . ? C24 C25 Cr01 C27 79.4(2) . . . . ? C26 C25 Cr01 C27 -37.5(2) . . . . ? C24 C25 Cr01 C26 116.9(3) . . . . ? C26 C25 Cr01 C24 -116.9(3) . . . . ? C24 C25 Cr01 C28 38.0(2) . . . . ? C26 C25 Cr01 C28 -78.9(2) . . . . ? C24 C25 Cr01 Cr01 -119.2(2) . . . 2_566 ? C26 C25 Cr01 Cr01 123.8(2) . . . 2_566 ? C27 C28 Cr01 C18 -49.8(3) . . . 2_566 ? C24 C28 Cr01 C18 -167.3(2) . . . 2_566 ? C27 C28 Cr01 C18 169.2(2) . . . . ? C24 C28 Cr01 C18 51.7(2) . . . . ? C24 C28 Cr01 C27 -117.5(3) . . . . ? C27 C28 Cr01 C26 38.0(2) . . . . ? C24 C28 Cr01 C26 -79.5(2) . . . . ? C27 C28 Cr01 C24 117.5(3) . . . . ? C27 C28 Cr01 C25 79.7(2) . . . . ? C24 C28 Cr01 C25 -37.8(2) . . . . ? C27 C28 Cr01 Cr01 -125.4(2) . . . 2_566 ? C24 C28 Cr01 Cr01 117.1(2) . . . 2_566 ? C3 C4 Cr02 C4 -110.6(2) . . . 2_655 ? C5 C4 Cr02 C4 113.5(2) . . . 2_655 ? Cr02 C4 Cr02 C4 0.0 2_655 . . 2_655 ? C3 C4 Cr02 C13 71.9(2) . . . . ? C5 C4 Cr02 C13 -64.0(2) . . . . ? Cr02 C4 Cr02 C13 -177.49(11) 2_655 . . . ? C3 C4 Cr02 C10 36.1(3) . . . . ? C5 C4 Cr02 C10 -99.8(2) . . . . ? Cr02 C4 Cr02 C10 146.67(17) 2_655 . . . ? C3 C4 Cr02 C11 103.3(3) . . . . ? C5 C4 Cr02 C11 -32.7(3) . . . . ? Cr02 C4 Cr02 C11 -146.16(19) 2_655 . . . ? C3 C4 Cr02 C14 39.6(2) . . . . ? C5 C4 Cr02 C14 -96.3(2) . . . . ? Cr02 C4 Cr02 C14 150.20(10) 2_655 . . . ? C3 C4 Cr02 C12 103.0(2) . . . . ? C5 C4 Cr02 C12 -32.9(2) . . . . ? Cr02 C4 Cr02 C12 -146.45(10) 2_655 . . . ? C3 C4 Cr02 Cr02 -110.6(2) . . . 2_655 ? C5 C4 Cr02 Cr02 113.5(2) . . . 2_655 ? C12 C13 Cr02 C4 -49.3(4) . . . 2_655 ? C14 C13 Cr02 C4 66.0(4) . . . 2_655 ? C12 C13 Cr02 C4 124.7(2) . . . . ? C14 C13 Cr02 C4 -119.9(2) . . . . ? C12 C13 Cr02 C10 -78.4(2) . . . . ? C14 C13 Cr02 C10 36.9(2) . . . . ? C12 C13 Cr02 C11 -36.5(2) . . . . ? C14 C13 Cr02 C11 78.8(2) . . . . ? C12 C13 Cr02 C14 -115.3(3) . . . . ? C14 C13 Cr02 C12 115.3(3) . . . . ? C12 C13 Cr02 Cr02 120.9(2) . . . 2_655 ? C14 C13 Cr02 Cr02 -123.8(2) . . . 2_655 ? C14 C10 Cr02 C4 153.8(2) . . . 2_655 ? C11 C10 Cr02 C4 -89.1(2) . . . 2_655 ? C14 C10 Cr02 C4 5.8(3) . . . . ? C11 C10 Cr02 C4 122.9(2) . . . . ? C14 C10 Cr02 C13 -37.5(2) . . . . ? C11 C10 Cr02 C13 79.5(2) . . . . ? C14 C10 Cr02 C11 -117.1(3) . . . . ? C11 C10 Cr02 C14 117.1(3) . . . . ? C14 C10 Cr02 C12 -79.3(2) . . . . ? C11 C10 Cr02 C12 37.8(2) . . . . ? C14 C10 Cr02 Cr02 122.3(2) . . . 2_655 ? C11 C10 Cr02 Cr02 -120.7(2) . . . 2_655 ? C12 C11 Cr02 C4 -148.3(2) . . . 2_655 ? C10 C11 Cr02 C4 97.0(2) . . . 2_655 ? C12 C11 Cr02 C4 -0.5(3) . . . . ? C10 C11 Cr02 C4 -115.2(3) . . . . ? C12 C11 Cr02 C13 36.8(2) . . . . ? C10 C11 Cr02 C13 -77.9(2) . . . . ? C12 C11 Cr02 C10 114.7(3) . . . . ? C12 C11 Cr02 C14 78.3(2) . . . . ? C10 C11 Cr02 C14 -36.4(2) . . . . ? C10 C11 Cr02 C12 -114.7(3) . . . . ? C12 C11 Cr02 Cr02 -120.5(2) . . . 2_655 ? C10 C11 Cr02 Cr02 124.8(2) . . . 2_655 ? C10 C14 Cr02 C4 -35.0(3) . . . 2_655 ? C13 C14 Cr02 C4 -151.2(2) . . . 2_655 ? C10 C14 Cr02 C4 -176.47(19) . . . . ? C13 C14 Cr02 C4 67.3(2) . . . . ? C10 C14 Cr02 C13 116.2(3) . . . . ? C13 C14 Cr02 C10 -116.2(3) . . . . ? C10 C14 Cr02 C11 37.2(2) . . . . ? C13 C14 Cr02 C11 -79.0(2) . . . . ? C10 C14 Cr02 C12 78.4(2) . . . . ? C13 C14 Cr02 C12 -37.8(2) . . . . ? C10 C14 Cr02 Cr02 -123.3(2) . . . 2_655 ? C13 C14 Cr02 Cr02 120.5(2) . . . 2_655 ? C11 C12 Cr02 C4 40.5(3) . . . 2_655 ? C13 C12 Cr02 C4 157.86(19) . . . 2_655 ? C11 C12 Cr02 C4 179.7(2) . . . . ? C13 C12 Cr02 C4 -62.9(2) . . . . ? C11 C12 Cr02 C13 -117.3(3) . . . . ? C11 C12 Cr02 C10 -38.4(2) . . . . ? C13 C12 Cr02 C10 78.9(2) . . . . ? C13 C12 Cr02 C11 117.3(3) . . . . ? C11 C12 Cr02 C14 -79.5(2) . . . . ? C13 C12 Cr02 C14 37.8(2) . . . . ? C11 C12 Cr02 Cr02 121.2(2) . . . 2_655 ? C13 C12 Cr02 Cr02 -121.5(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.394 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.066