# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1882 data_global _publ_contact_author_name 'F.A. Cotton' _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, P.O. Box 300012 College Station, TX 77842-3012, USA ; _publ_contact_author_email cotton@tamu.edu _publ_contact_author_fax '(409) 845 9351' _publ_contact_author_phone '(409) 845 4432' _publ_requested_journal ChemComm _publ_section_title ; A remarkable Cr(III) organometallic compound formed by unprecedented rearrangement of a formamidinate anion ; data_xl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H32 Cl2 Cr2 N8 O3' _chemical_formula_weight 667.49 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 15.507(2) _cell_length_b 9.7562(6) _cell_length_c 19.920(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.597(7) _cell_angle_gamma 90.00 _cell_volume 2979.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 9.05 _cell_measurement_theta_max 20.9 _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7768 _exptl_absorpt_correction_T_max 0.8327 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Nonius FAST' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15663 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 24.31 _reflns_number_total 4711 _reflns_number_gt 4257 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+3.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4711 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.55048(3) 0.54626(4) 0.068601(19) 0.02194(13) Uani 1 d . . . Cr2 Cr 0.03303(3) 0.58986(4) 0.061783(19) 0.02463(13) Uani 1 d . . . Cl1 Cl 0.42879(4) 0.52914(7) 0.13489(3) 0.03279(18) Uani 1 d . . . Cl2 Cl -0.09534(4) 0.73597(7) 0.05510(3) 0.03431(18) Uani 1 d . . . O1 O 0.51985(11) 0.37995(18) 0.01407(8) 0.0260(4) Uani 1 d . . . O2 O -0.03458(12) 0.41966(18) 0.03782(9) 0.0268(4) Uani 1 d . . . N1 N 0.58450(14) 0.7402(2) 0.10881(11) 0.0273(5) Uani 1 d . . . N2 N 0.69141(17) 0.7185(3) 0.04168(13) 0.0376(6) Uani 1 d . . . H2N H 0.738(2) 0.748(4) 0.0362(18) 0.048(11) Uiso 1 d . . . N3 N 0.73384(19) 0.4905(3) 0.07576(13) 0.0399(6) Uani 1 d . . . H3N H 0.779(2) 0.490(3) 0.0716(16) 0.032(9) Uiso 1 d . . . N4 N 0.63335(14) 0.4438(2) 0.14558(10) 0.0251(5) Uani 1 d . . . N5 N 0.03808(16) 0.5663(2) 0.16664(11) 0.0312(5) Uani 1 d . . . N6 N 0.15793(19) 0.4400(3) 0.15419(14) 0.0479(8) Uani 1 d . . . H6N H 0.196(2) 0.400(3) 0.1667(16) 0.028(9) Uiso 1 d . . . N7 N 0.21864(19) 0.5900(3) 0.07900(14) 0.0389(7) Uani 1 d . . . H7N H 0.259(2) 0.574(3) 0.0855(15) 0.014(8) Uiso 1 d . . . N8 N 0.11621(14) 0.7590(2) 0.07127(11) 0.0289(5) Uani 1 d . . . C1 C 0.5429(2) 0.8176(3) 0.15085(15) 0.0393(7) Uani 1 d . . . H1 H 0.497(2) 0.773(3) 0.1661(17) 0.045(9) Uiso 1 d . . . C2 C 0.5707(3) 0.9459(4) 0.17203(18) 0.0512(9) Uani 1 d . . . H2 H 0.537(3) 0.989(4) 0.201(2) 0.060(11) Uiso 1 d . . . C3 C 0.6436(3) 0.9997(4) 0.14935(18) 0.0507(9) Uani 1 d . . . H3 H 0.660(2) 1.085(4) 0.1628(18) 0.053(10) Uiso 1 d . . . C4 C 0.6857(2) 0.9267(3) 0.10694(18) 0.0436(8) Uani 1 d . . . H4 H 0.733(3) 0.955(4) 0.090(2) 0.059(12) Uiso 1 d . . . C5 C 0.65495(18) 0.7949(3) 0.08624(13) 0.0315(6) Uani 1 d . . . C6 C 0.66852(18) 0.5751(3) 0.03513(14) 0.0291(6) Uani 1 d . . . H6 H 0.6672(17) 0.555(3) -0.0098(15) 0.021(7) Uiso 1 d . . . C7 C 0.71680(17) 0.4360(3) 0.13423(14) 0.0302(6) Uani 1 d . . . C8 C 0.7813(2) 0.3719(4) 0.18159(17) 0.0428(7) Uani 1 d . . . H8 H 0.839(2) 0.368(3) 0.1715(17) 0.048(9) Uiso 1 d . . . C9 C 0.7578(2) 0.3129(3) 0.23831(15) 0.0419(7) Uani 1 d . . . H9 H 0.801(2) 0.269(3) 0.2661(17) 0.038(8) Uiso 1 d . . . C10 C 0.6715(2) 0.3159(3) 0.24872(15) 0.0377(7) Uani 1 d . . . H10 H 0.652(2) 0.276(3) 0.2889(18) 0.045(9) Uiso 1 d . . . C11 C 0.61227(19) 0.3826(3) 0.20218(13) 0.0299(6) Uani 1 d . . . H11 H 0.553(2) 0.391(3) 0.2049(14) 0.026(7) Uiso 1 d . . . C12 C 0.5258(3) 0.2445(3) 0.03809(18) 0.0552(10) Uani 1 d . . . H12A H 0.4809 0.2284 0.0663 0.16(3) Uiso 1 calc R . . H12B H 0.5828 0.2299 0.0647 0.164 Uiso 1 calc R . . H12C H 0.5180 0.1817 -0.0001 0.164 Uiso 1 calc R . . C13 C 0.10514(19) 0.4859(3) 0.19564(15) 0.0369(7) Uani 1 d . . . C14 C 0.1141(3) 0.4532(4) 0.26528(17) 0.0499(9) Uani 1 d . . . H14 H 0.158(3) 0.402(4) 0.284(2) 0.052(11) Uiso 1 d . . . C15 C 0.0559(3) 0.5017(4) 0.30318(17) 0.0569(10) Uani 1 d . . . H15 H 0.056(2) 0.484(4) 0.348(2) 0.061(11) Uiso 1 d . . . C16 C -0.0125(3) 0.5835(4) 0.27392(17) 0.0555(10) Uani 1 d . . . H16 H -0.052(3) 0.611(5) 0.301(2) 0.078(14) Uiso 1 d . . . C17 C -0.0186(2) 0.6137(3) 0.20644(15) 0.0409(7) Uani 1 d . . . H17 H -0.064(2) 0.668(3) 0.1839(16) 0.038(8) Uiso 1 d . . . C18 C 0.15167(18) 0.4910(3) 0.08543(14) 0.0330(6) Uani 1 d . . . H18 H 0.1604(19) 0.419(3) 0.0591(15) 0.028(7) Uiso 1 d . . . C19 C 0.20114(18) 0.7241(3) 0.07353(13) 0.0308(6) Uani 1 d . . . C20 C 0.2656(2) 0.8242(4) 0.06944(16) 0.0433(8) Uani 1 d . . . H20 H 0.315(3) 0.797(4) 0.0679(18) 0.050(11) Uiso 1 d . . . C21 C 0.2427(2) 0.9577(4) 0.06470(18) 0.0507(9) Uani 1 d . . . H21 H 0.287(2) 1.029(4) 0.0628(18) 0.052(10) Uiso 1 d . . . C22 C 0.1559(2) 0.9957(4) 0.06416(18) 0.0500(8) Uani 1 d . . . H22 H 0.138(2) 1.084(4) 0.0641(17) 0.045(9) Uiso 1 d . . . C23 C 0.0959(2) 0.8947(3) 0.06709(16) 0.0384(7) Uani 1 d . . . H23 H 0.041(2) 0.912(4) 0.0626(16) 0.042(10) Uiso 1 d . . . C24 C -0.0345(2) 0.3013(3) 0.07839(14) 0.0364(7) Uani 1 d . . . H24A H 0.0127 0.2413 0.0701 0.062(11) Uiso 1 calc R . . H24B H -0.0897 0.2537 0.0671 0.062 Uiso 1 calc R . . H24C H -0.0265 0.3274 0.1259 0.062 Uiso 1 calc R . . O3 O 0.3108(2) 0.2698(3) 0.1563(2) 0.1020(13) Uani 1 d . . . H3O H 0.3392 0.3411 0.1661 0.153 Uiso 1 calc R . . C25 C 0.3417(4) 0.1699(5) 0.1996(3) 0.104(2) Uani 1 d . . . H25A H 0.3974 0.1383 0.1888 0.155 Uiso 1 calc R . . H25B H 0.3007 0.0942 0.1955 0.155 Uiso 1 calc R . . H25C H 0.3494 0.2049 0.2457 0.155 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0204(2) 0.0272(2) 0.0179(2) -0.00053(15) 0.00204(16) 0.00334(15) Cr2 0.0239(2) 0.0307(2) 0.0186(2) 0.00218(16) 0.00091(16) 0.00570(17) Cl1 0.0232(3) 0.0491(4) 0.0267(3) 0.0016(3) 0.0058(3) 0.0035(3) Cl2 0.0263(3) 0.0424(4) 0.0339(4) -0.0012(3) 0.0036(3) 0.0100(3) O1 0.0288(10) 0.0260(9) 0.0216(9) 0.0010(7) -0.0008(7) 0.0040(7) O2 0.0299(10) 0.0304(10) 0.0195(9) 0.0033(7) 0.0021(7) 0.0034(7) N1 0.0278(12) 0.0316(12) 0.0215(11) -0.0009(9) 0.0004(9) 0.0022(9) N2 0.0288(14) 0.0410(14) 0.0452(15) -0.0001(11) 0.0134(11) -0.0037(11) N3 0.0209(14) 0.0584(17) 0.0418(15) 0.0098(12) 0.0096(11) 0.0131(12) N4 0.0254(12) 0.0300(11) 0.0192(11) -0.0030(9) 0.0011(9) 0.0028(9) N5 0.0387(13) 0.0342(12) 0.0201(11) -0.0006(9) 0.0021(10) -0.0014(10) N6 0.0345(15) 0.0663(19) 0.0401(16) 0.0214(14) -0.0033(12) 0.0211(14) N7 0.0188(14) 0.0536(18) 0.0439(16) -0.0032(12) 0.0031(11) 0.0109(12) N8 0.0293(12) 0.0352(13) 0.0219(11) -0.0006(9) 0.0026(9) 0.0044(10) C1 0.0486(19) 0.0383(17) 0.0320(16) -0.0045(13) 0.0092(14) 0.0072(14) C2 0.073(3) 0.0397(18) 0.0399(19) -0.0117(15) 0.0048(17) 0.0106(17) C3 0.067(2) 0.0316(17) 0.047(2) -0.0059(15) -0.0112(17) -0.0031(16) C4 0.0427(19) 0.0384(17) 0.0461(19) 0.0025(14) -0.0051(15) -0.0074(14) C5 0.0307(15) 0.0348(15) 0.0259(14) 0.0040(12) -0.0059(11) 0.0001(12) C6 0.0262(14) 0.0382(15) 0.0230(14) -0.0012(11) 0.0042(11) 0.0044(11) C7 0.0231(14) 0.0350(15) 0.0322(15) -0.0023(12) 0.0028(11) 0.0045(11) C8 0.0263(16) 0.0534(19) 0.0472(19) 0.0028(15) 0.0002(13) 0.0113(14) C9 0.0423(18) 0.0477(18) 0.0310(16) 0.0028(14) -0.0099(13) 0.0135(14) C10 0.0452(18) 0.0417(17) 0.0248(15) 0.0006(13) 0.0007(13) 0.0040(14) C11 0.0270(15) 0.0387(15) 0.0237(14) -0.0023(11) 0.0030(11) 0.0027(12) C12 0.087(3) 0.0291(17) 0.0411(18) 0.0061(14) -0.0180(19) 0.0032(16) C13 0.0361(16) 0.0402(16) 0.0306(15) 0.0078(13) -0.0071(13) -0.0062(13) C14 0.056(2) 0.053(2) 0.0348(18) 0.0157(15) -0.0129(17) -0.0135(17) C15 0.084(3) 0.064(2) 0.0215(16) 0.0071(16) 0.0035(17) -0.022(2) C16 0.082(3) 0.059(2) 0.0270(17) -0.0040(16) 0.0147(18) -0.007(2) C17 0.056(2) 0.0408(17) 0.0273(15) -0.0056(13) 0.0090(14) 0.0007(15) C18 0.0302(15) 0.0382(16) 0.0282(15) -0.0022(13) -0.0033(11) 0.0116(12) C19 0.0298(15) 0.0437(17) 0.0179(13) -0.0015(11) 0.0003(10) 0.0041(12) C20 0.0304(17) 0.062(2) 0.0363(17) 0.0060(15) 0.0015(13) -0.0048(15) C21 0.050(2) 0.056(2) 0.0442(19) 0.0092(16) 0.0034(16) -0.0162(17) C22 0.061(2) 0.0387(19) 0.049(2) 0.0077(15) 0.0042(16) -0.0008(17) C23 0.0359(18) 0.0379(17) 0.0415(17) 0.0037(13) 0.0063(13) 0.0067(13) C24 0.0468(18) 0.0356(16) 0.0283(14) 0.0057(12) 0.0103(12) 0.0053(13) O3 0.0547(18) 0.069(2) 0.179(4) 0.057(2) 0.004(2) 0.0078(15) C25 0.130(5) 0.059(3) 0.101(4) 0.006(3) -0.050(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.9704(16) 3_665 ? Cr1 O1 1.9708(17) . ? Cr1 C6 2.059(3) . ? Cr1 N1 2.091(2) . ? Cr1 N4 2.101(2) . ? Cr1 Cl1 2.4653(8) . ? Cr2 O2 1.9836(18) . ? Cr2 O2 1.9900(18) 3_565 ? Cr2 C18 2.068(3) . ? Cr2 N8 2.086(2) . ? Cr2 N5 2.091(2) . ? Cr2 Cl2 2.4359(8) . ? O1 C12 1.404(4) . ? O1 Cr1 1.9705(16) 3_665 ? O2 C24 1.410(3) . ? O2 Cr2 1.9899(18) 3_565 ? N1 C5 1.352(4) . ? N1 C1 1.360(4) . ? N2 C5 1.346(4) . ? N2 C6 1.444(4) . ? N2 H2N 0.80(4) . ? N3 C7 1.342(4) . ? N3 C6 1.455(4) . ? N3 H3N 0.72(3) . ? N4 C7 1.349(3) . ? N4 C11 1.358(4) . ? N5 C17 1.351(4) . ? N5 C13 1.361(4) . ? N6 C13 1.325(4) . ? N6 C18 1.447(4) . ? N6 H6N 0.71(3) . ? N7 C19 1.338(4) . ? N7 C18 1.438(4) . ? N7 H7N 0.64(3) . ? N8 C19 1.355(4) . ? N8 C23 1.361(4) . ? C1 C2 1.370(5) . ? C1 H1 0.93(4) . ? C2 C3 1.383(6) . ? C2 H2 0.94(4) . ? C3 C4 1.346(5) . ? C3 H3 0.91(4) . ? C4 C5 1.411(4) . ? C4 H4 0.90(4) . ? C6 H6 0.91(3) . ? C7 C8 1.413(4) . ? C8 C9 1.365(5) . ? C8 H8 0.95(4) . ? C9 C10 1.386(5) . ? C9 H9 0.91(3) . ? C10 C11 1.368(4) . ? C10 H10 0.98(4) . ? C11 H11 0.93(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.410(4) . ? C14 C15 1.346(6) . ? C14 H14 0.88(4) . ? C15 C16 1.384(6) . ? C15 H15 0.91(4) . ? C16 C17 1.365(5) . ? C16 H16 0.91(5) . ? C17 H17 0.94(3) . ? C18 H18 0.90(3) . ? C19 C20 1.408(4) . ? C20 C21 1.349(5) . ? C20 H20 0.82(4) . ? C21 C22 1.396(5) . ? C21 H21 0.98(4) . ? C22 C23 1.363(5) . ? C22 H22 0.90(4) . ? C23 H23 0.86(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? O3 C25 1.341(5) . ? O3 H3O 0.8300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cr1 O1 77.44(8) 3_665 . ? O1 Cr1 C6 95.00(9) 3_665 . ? O1 Cr1 C6 94.98(10) . . ? O1 Cr1 N1 93.78(8) 3_665 . ? O1 Cr1 N1 169.17(8) . . ? C6 Cr1 N1 79.32(10) . . ? O1 Cr1 N4 170.29(8) 3_665 . ? O1 Cr1 N4 94.66(8) . . ? C6 Cr1 N4 79.92(10) . . ? N1 Cr1 N4 93.40(8) . . ? O1 Cr1 Cl1 95.74(6) 3_665 . ? O1 Cr1 Cl1 95.67(6) . . ? C6 Cr1 Cl1 166.28(8) . . ? N1 Cr1 Cl1 91.47(6) . . ? N4 Cr1 Cl1 90.61(6) . . ? O2 Cr2 O2 78.79(8) . 3_565 ? O2 Cr2 C18 94.85(10) . . ? O2 Cr2 C18 93.58(10) 3_565 . ? O2 Cr2 N8 169.00(8) . . ? O2 Cr2 N8 91.60(8) 3_565 . ? C18 Cr2 N8 80.29(11) . . ? O2 Cr2 N5 95.04(8) . . ? O2 Cr2 N5 170.58(9) 3_565 . ? C18 Cr2 N5 79.75(10) . . ? N8 Cr2 N5 93.80(9) . . ? O2 Cr2 Cl2 94.50(6) . . ? O2 Cr2 Cl2 95.99(6) 3_565 . ? C18 Cr2 Cl2 167.74(9) . . ? N8 Cr2 Cl2 91.78(6) . . ? N5 Cr2 Cl2 91.56(7) . . ? C12 O1 Cr1 128.98(17) . 3_665 ? C12 O1 Cr1 126.07(17) . . ? Cr1 O1 Cr1 102.56(8) 3_665 . ? C24 O2 Cr2 126.36(17) . . ? C24 O2 Cr2 122.31(16) . 3_565 ? Cr2 O2 Cr2 101.21(8) . 3_565 ? C5 N1 C1 117.9(2) . . ? C5 N1 Cr1 113.58(17) . . ? C1 N1 Cr1 128.5(2) . . ? C5 N2 C6 118.3(3) . . ? C5 N2 H2N 111(3) . . ? C6 N2 H2N 124(3) . . ? C7 N3 C6 119.8(3) . . ? C7 N3 H3N 115(3) . . ? C6 N3 H3N 123(3) . . ? C7 N4 C11 118.1(2) . . ? C7 N4 Cr1 113.72(17) . . ? C11 N4 Cr1 128.18(18) . . ? C17 N5 C13 118.1(3) . . ? C17 N5 Cr2 128.2(2) . . ? C13 N5 Cr2 113.56(19) . . ? C13 N6 C18 120.9(3) . . ? C13 N6 H6N 121(3) . . ? C18 N6 H6N 117(3) . . ? C19 N7 C18 121.6(3) . . ? C19 N7 H7N 116(3) . . ? C18 N7 H7N 121(3) . . ? C19 N8 C23 117.5(3) . . ? C19 N8 Cr2 112.90(18) . . ? C23 N8 Cr2 129.0(2) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 114(2) . . ? C2 C1 H1 124(2) . . ? C1 C2 C3 118.8(3) . . ? C1 C2 H2 115(2) . . ? C3 C2 H2 126(2) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 122(2) . . ? C2 C3 H3 118(2) . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 125(3) . . ? C5 C4 H4 115(3) . . ? N2 C5 N1 116.1(2) . . ? N2 C5 C4 122.7(3) . . ? N1 C5 C4 121.1(3) . . ? N2 C6 N3 111.0(2) . . ? N2 C6 Cr1 108.76(18) . . ? N3 C6 Cr1 108.72(19) . . ? N2 C6 H6 105.3(17) . . ? N3 C6 H6 109.7(17) . . ? Cr1 C6 H6 113.4(17) . . ? N3 C7 N4 116.2(2) . . ? N3 C7 C8 122.9(3) . . ? N4 C7 C8 120.9(3) . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 122(2) . . ? C7 C8 H8 118(2) . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 116(2) . . ? C10 C9 H9 124(2) . . ? C11 C10 C9 118.3(3) . . ? C11 C10 H10 119(2) . . ? C9 C10 H10 123(2) . . ? N4 C11 C10 123.5(3) . . ? N4 C11 H11 111.9(17) . . ? C10 C11 H11 124.7(18) . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 N5 115.8(3) . . ? N6 C13 C14 123.9(3) . . ? N5 C13 C14 120.3(3) . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 121(2) . . ? C13 C14 H14 119(3) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 125(3) . . ? C16 C15 H15 114(3) . . ? C17 C16 C15 118.4(4) . . ? C17 C16 H16 124(3) . . ? C15 C16 H16 118(3) . . ? N5 C17 C16 123.3(3) . . ? N5 C17 H17 114.9(19) . . ? C16 C17 H17 122(2) . . ? N7 C18 N6 111.6(3) . . ? N7 C18 Cr2 107.2(2) . . ? N6 C18 Cr2 107.9(2) . . ? N7 C18 H18 107.4(19) . . ? N6 C18 H18 106.8(19) . . ? Cr2 C18 H18 115.9(19) . . ? N7 C19 N8 115.7(3) . . ? N7 C19 C20 123.1(3) . . ? N8 C19 C20 121.2(3) . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 123(3) . . ? C19 C20 H20 117(3) . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 121(2) . . ? C22 C21 H21 119(2) . . ? C23 C22 C21 118.2(3) . . ? C23 C22 H22 118(2) . . ? C21 C22 H22 124(2) . . ? N8 C23 C22 123.5(3) . . ? N8 C23 H23 114(2) . . ? C22 C23 H23 122(2) . . ? O2 C24 H24A 109.5 . . ? O2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 O3 H3O 109.5 . . ? O3 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 24.31 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.620 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.065 #===END