# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_RD330 _database_code_depnum_ccdc_archive 'CCDC 897967' _vrf_CHEMW03_RD330 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. The two lattice solvent dichloromethane molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT043_RD330 ; PROBLEM: Check Reported Molecular Weight ................ 1225.16 RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. The two lattice solvent dichloromethane molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT051_RD330 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 30.73 Perc. RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. The two lattice solvent dichloromethane molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H82 Cl4 Cr2 N4 O6, 2(C H2 Cl2)' _chemical_formula_sum 'C62 H82 Cl4 Cr2 N4 O6' _chemical_formula_weight 1225.16 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.239(7) _cell_length_b 13.204(7) _cell_length_c 18.420(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.586(6) _cell_angle_gamma 90.00 _cell_volume 3447(3) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 8502 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 29.7 _exptl_crystal_description Prism _exptl_crystal_colour Black-Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 32578 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7115 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_structure_solution 'SHELXL-97 (Acta Cryst.2008, A64, 112-122)' _computing_structure_refinement 'SHELXL-97 (Acta Cryst.2008, A64, 112-122)' _computing_molecular_graphics 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _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. All non-hydrogen atoms were introduced in difference map positions and refined anisotropically, while all H-atoms were introduced in calculated positions and refined on a riding model, except H3A. H3A was located in its difference map position, and was refined with a fixed displacement ellipsoid, 1.5 times that of O3, and was refined positionally with a distance restraint. All atoms were introduced prior to the application of Squeeze. ; _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^)+(0.1312P)^2^+3.6988P] 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 7115 _refine_ls_number_parameters 336 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2384 _refine_ls_wR_factor_gt 0.2262 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.019 -0.011 1009 173 '4 Disordered CH2Cl2' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 173 electrons per unit cell in one void (total volume 1009 ^A^3); that is 86.5 electrons per formula unit. Disordered solvent lattice dichloromethane molecules (42 electrons per CH2Cl2; 2 molecules per formula unit) were present prior to the application of Squeeze, however, a satisfactory point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.50403(3) 0.04986(3) 0.92517(3) 0.03588(19) Uani 1 1 d . . . O1 O 0.60749(16) 0.13348(17) 0.96197(13) 0.0454(5) Uani 1 1 d . . . O2 O 0.43907(16) 0.16340(16) 0.87601(11) 0.0405(5) Uani 1 1 d . . . O3 O 0.44165(16) 0.06884(16) 1.01622(12) 0.0397(5) Uani 1 1 d D . . N1 N 0.5710(2) 0.0132(2) 0.83318(15) 0.0444(6) Uani 1 1 d . . . N2 N 0.4002(2) -0.04177(18) 0.87177(15) 0.0416(6) Uani 1 1 d . . . C1 C 0.6845(2) 0.1588(3) 0.9309(2) 0.0506(8) Uani 1 1 d . . . C2 C 0.7285(3) 0.2545(3) 0.9467(2) 0.0607(10) Uani 1 1 d . . . C3 C 0.8155(3) 0.2705(4) 0.9180(3) 0.0769(14) Uani 1 1 d . . . H3 H 0.8485 0.3314 0.9309 0.092 Uiso 1 1 calc R . . C4 C 0.8563(3) 0.2037(4) 0.8726(3) 0.0806(15) Uani 1 1 d . . . C5 C 0.8074(3) 0.1170(4) 0.8528(3) 0.0710(12) Uani 1 1 d . . . H5 H 0.8318 0.0720 0.8191 0.085 Uiso 1 1 calc R . . C6 C 0.7228(3) 0.0932(3) 0.8811(2) 0.0559(9) Uani 1 1 d . . . C7 C 0.6734(3) -0.0030(3) 0.8574(2) 0.0548(9) Uani 1 1 d . . . H7A H 0.6793 -0.0518 0.8984 0.066 Uiso 1 1 calc R . . H7B H 0.7046 -0.0330 0.8167 0.066 Uiso 1 1 calc R . . C8 C 0.5607(3) 0.0948(3) 0.77715(19) 0.0486(8) Uani 1 1 d . . . H8A H 0.5898 0.0710 0.7336 0.058 Uiso 1 1 calc R . . H8B H 0.5972 0.1543 0.7966 0.058 Uiso 1 1 calc R . . C9 C 0.4625(3) 0.1289(2) 0.75321(18) 0.0445(7) Uani 1 1 d . . . C10 C 0.4305(3) 0.1342(3) 0.67938(18) 0.0513(8) Uani 1 1 d . . . H10 H 0.4675 0.1050 0.6446 0.062 Uiso 1 1 calc R . . C11 C 0.3462(3) 0.1811(3) 0.65546(19) 0.0555(9) Uani 1 1 d . . . C12 C 0.2950(3) 0.2238(3) 0.70765(19) 0.0495(8) Uani 1 1 d . . . H12 H 0.2377 0.2573 0.6916 0.059 Uiso 1 1 calc R . . C13 C 0.3223(2) 0.2207(2) 0.78227(18) 0.0432(7) Uani 1 1 d . . . C14 C 0.4084(2) 0.1700(2) 0.80613(17) 0.0388(6) Uani 1 1 d . . . C15 C 0.5290(3) -0.0820(3) 0.8035(2) 0.0553(9) Uani 1 1 d . . . H15A H 0.5604 -0.1401 0.8297 0.066 Uiso 1 1 calc R . . H15B H 0.5395 -0.0878 0.7513 0.066 Uiso 1 1 calc R . . C16 C 0.4250(3) -0.0860(2) 0.81103(19) 0.0500(8) Uani 1 1 d . . . C17 C 0.3588(4) -0.1342(3) 0.7628(2) 0.0661(11) Uani 1 1 d . . . H17 H 0.3777 -0.1661 0.7204 0.079 Uiso 1 1 calc R . . C18 C 0.2660(4) -0.1356(4) 0.7766(3) 0.0800(14) Uani 1 1 d . . . H18 H 0.2199 -0.1677 0.7435 0.096 Uiso 1 1 calc R . . C19 C 0.2410(3) -0.0910(4) 0.8377(3) 0.0710(12) Uani 1 1 d . . . H19 H 0.1771 -0.0915 0.8483 0.085 Uiso 1 1 calc R . . C20 C 0.3093(3) -0.0444(3) 0.8848(2) 0.0511(8) Uani 1 1 d . . . H20 H 0.2911 -0.0132 0.9278 0.061 Uiso 1 1 calc R . . C21 C 0.6825(4) 0.3355(3) 0.9891(3) 0.0738(13) Uani 1 1 d . . . C22 C 0.5847(4) 0.3600(3) 0.9502(3) 0.0834(15) Uani 1 1 d . . . H22A H 0.5920 0.4018 0.9071 0.100 Uiso 1 1 calc R . . H22B H 0.5475 0.3970 0.9835 0.100 Uiso 1 1 calc R . . H22C H 0.5523 0.2969 0.9351 0.100 Uiso 1 1 calc R . . C23 C 0.7380(7) 0.4344(5) 0.9929(4) 0.134(3) Uani 1 1 d . . . H23A H 0.7900 0.4298 1.0317 0.160 Uiso 1 1 calc R . . H23B H 0.6962 0.4904 1.0034 0.160 Uiso 1 1 calc R . . H23C H 0.7634 0.4465 0.9461 0.160 Uiso 1 1 calc R . . C24 C 0.6708(5) 0.3029(4) 1.0668(3) 0.099(2) Uani 1 1 d . . . H24A H 0.6268 0.2457 1.0661 0.119 Uiso 1 1 calc R . . H24B H 0.6458 0.3595 1.0935 0.119 Uiso 1 1 calc R . . H24C H 0.7321 0.2823 1.0911 0.119 Uiso 1 1 calc R . . C25 C 0.9501(4) 0.2295(6) 0.8456(4) 0.113(2) Uani 1 1 d . . . H25A H 0.9876 0.1676 0.8428 0.136 Uiso 1 1 calc R . . H25B H 0.9840 0.2774 0.8793 0.136 Uiso 1 1 calc R . . H25C H 0.9396 0.2602 0.7970 0.136 Uiso 1 1 calc R . . C26 C 0.3135(4) 0.1916(4) 0.5759(2) 0.0756(13) Uani 1 1 d . . . H26A H 0.3684 0.1944 0.5478 0.091 Uiso 1 1 calc R . . H26B H 0.2767 0.2540 0.5680 0.091 Uiso 1 1 calc R . . H26C H 0.2742 0.1333 0.5600 0.091 Uiso 1 1 calc R . . C27 C 0.2657(3) 0.2750(3) 0.8361(2) 0.0534(9) Uani 1 1 d . . . C28 C 0.2321(3) 0.2002(3) 0.8925(2) 0.0599(10) Uani 1 1 d . . . H28A H 0.2870 0.1693 0.9202 0.072 Uiso 1 1 calc R . . H28B H 0.1934 0.1472 0.8672 0.072 Uiso 1 1 calc R . . H28C H 0.1945 0.2366 0.9259 0.072 Uiso 1 1 calc R . . C29 C 0.1754(3) 0.3251(4) 0.7985(3) 0.0743(13) Uani 1 1 d . . . H29A H 0.1378 0.3528 0.8357 0.089 Uiso 1 1 calc R . . H29B H 0.1381 0.2743 0.7695 0.089 Uiso 1 1 calc R . . H29C H 0.1930 0.3798 0.7665 0.089 Uiso 1 1 calc R . . C30 C 0.3255(3) 0.3565(3) 0.8755(2) 0.0629(11) Uani 1 1 d . . . H30A H 0.3846 0.3266 0.8976 0.076 Uiso 1 1 calc R . . H30B H 0.2910 0.3863 0.9138 0.076 Uiso 1 1 calc R . . H30C H 0.3397 0.4092 0.8408 0.076 Uiso 1 1 calc R . . H3A H 0.461(3) 0.1276(19) 1.031(2) 0.060 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0439(3) 0.0292(3) 0.0362(3) 0.00179(17) 0.0120(2) 0.00243(18) O1 0.0503(12) 0.0392(11) 0.0479(13) 0.0000(9) 0.0111(10) -0.0043(9) O2 0.0539(12) 0.0351(10) 0.0337(11) 0.0019(8) 0.0110(9) 0.0076(9) O3 0.0486(12) 0.0330(10) 0.0392(12) 0.0023(9) 0.0126(9) 0.0069(9) N1 0.0532(15) 0.0345(13) 0.0492(15) 0.0033(11) 0.0231(12) 0.0075(11) N2 0.0541(16) 0.0318(12) 0.0395(14) 0.0031(10) 0.0078(11) -0.0052(11) C1 0.0483(18) 0.0454(18) 0.059(2) 0.0113(15) 0.0072(15) -0.0009(14) C2 0.060(2) 0.055(2) 0.066(2) 0.0152(18) -0.0016(18) -0.0156(17) C3 0.063(2) 0.072(3) 0.092(3) 0.038(3) -0.011(2) -0.023(2) C4 0.045(2) 0.082(3) 0.116(4) 0.045(3) 0.012(2) -0.001(2) C5 0.051(2) 0.071(3) 0.095(3) 0.029(2) 0.029(2) 0.0140(19) C6 0.0468(18) 0.051(2) 0.072(2) 0.0190(18) 0.0176(17) 0.0081(15) C7 0.055(2) 0.0504(19) 0.064(2) 0.0088(16) 0.0279(17) 0.0168(16) C8 0.064(2) 0.0412(17) 0.0457(18) 0.0067(14) 0.0287(16) 0.0059(15) C9 0.063(2) 0.0317(14) 0.0408(16) -0.0002(12) 0.0151(14) -0.0013(13) C10 0.081(2) 0.0373(16) 0.0377(17) -0.0036(13) 0.0183(16) -0.0086(16) C11 0.082(3) 0.0431(18) 0.0400(18) 0.0020(14) 0.0008(17) -0.0209(17) C12 0.0514(18) 0.0490(18) 0.0477(19) 0.0083(14) 0.0028(14) -0.0140(15) C13 0.0463(16) 0.0412(16) 0.0431(17) 0.0056(13) 0.0099(13) -0.0041(13) C14 0.0481(16) 0.0314(13) 0.0384(15) 0.0027(11) 0.0116(12) -0.0024(12) C15 0.079(3) 0.0364(16) 0.054(2) -0.0065(15) 0.0252(18) 0.0039(16) C16 0.081(2) 0.0301(14) 0.0411(17) -0.0016(13) 0.0146(16) -0.0018(15) C17 0.105(4) 0.0427(19) 0.049(2) -0.0046(16) 0.002(2) -0.007(2) C18 0.096(4) 0.073(3) 0.067(3) 0.002(2) -0.015(3) -0.028(3) C19 0.062(2) 0.075(3) 0.074(3) 0.002(2) -0.004(2) -0.018(2) C20 0.0516(19) 0.0486(19) 0.054(2) 0.0040(15) 0.0088(15) -0.0074(14) C21 0.109(4) 0.049(2) 0.063(3) 0.0010(19) 0.005(2) -0.030(2) C22 0.131(5) 0.044(2) 0.076(3) -0.001(2) 0.015(3) 0.017(2) C23 0.228(9) 0.078(4) 0.101(5) -0.016(3) 0.050(5) -0.084(5) C24 0.154(6) 0.080(3) 0.064(3) 0.000(3) 0.007(3) -0.040(4) C25 0.054(3) 0.125(5) 0.163(6) 0.062(5) 0.022(3) -0.010(3) C26 0.114(4) 0.066(3) 0.045(2) -0.0023(19) -0.003(2) -0.023(3) C27 0.055(2) 0.053(2) 0.055(2) 0.0154(16) 0.0224(16) 0.0137(16) C28 0.059(2) 0.066(2) 0.059(2) 0.0225(18) 0.0266(17) 0.0153(18) C29 0.061(2) 0.088(3) 0.078(3) 0.036(2) 0.026(2) 0.026(2) C30 0.094(3) 0.048(2) 0.051(2) 0.0025(16) 0.032(2) 0.018(2) _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 1.912(2) . ? Cr1 O2 1.939(2) . ? Cr1 O3 1.989(2) . ? Cr1 O3 2.014(2) 3_657 ? Cr1 N1 2.081(3) . ? Cr1 N2 2.081(3) . ? O1 C1 1.328(4) . ? O2 C14 1.321(4) . ? O3 Cr1 2.014(2) 3_657 ? O3 H3A 0.861(19) . ? N1 C15 1.475(5) . ? N1 C8 1.490(4) . ? N1 C7 1.498(5) . ? N2 C16 1.339(4) . ? N2 C20 1.341(5) . ? C1 C6 1.410(6) . ? C1 C2 1.428(5) . ? C2 C3 1.409(6) . ? C2 C21 1.511(7) . ? C3 C4 1.381(8) . ? C3 H3 0.9500 . ? C4 C5 1.371(7) . ? C4 C25 1.510(6) . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 C7 1.497(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.494(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.393(5) . ? C9 C14 1.409(4) . ? C10 C11 1.384(6) . ? C10 H10 0.9500 . ? C11 C12 1.382(6) . ? C11 C26 1.500(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.427(5) . ? C13 C27 1.517(5) . ? C15 C16 1.501(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.386(6) . ? C17 C18 1.369(7) . ? C17 H17 0.9500 . ? C18 C19 1.350(7) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C24 1.520(7) . ? C21 C23 1.524(6) . ? C21 C22 1.537(8) . ? 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 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.514(6) . ? C27 C28 1.543(5) . ? C27 C29 1.549(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cr1 O2 92.01(11) . . ? O1 Cr1 O3 91.16(10) . . ? O2 Cr1 O3 93.70(9) . . ? O1 Cr1 O3 90.97(10) . 3_657 ? O2 Cr1 O3 173.05(9) . 3_657 ? O3 Cr1 O3 79.97(10) . 3_657 ? O1 Cr1 N1 91.41(11) . . ? O2 Cr1 N1 92.02(10) . . ? O3 Cr1 N1 173.64(10) . . ? O3 Cr1 N1 94.18(10) 3_657 . ? O1 Cr1 N2 172.09(10) . . ? O2 Cr1 N2 86.81(11) . . ? O3 Cr1 N2 96.71(11) . . ? O3 Cr1 N2 91.09(11) 3_657 . ? N1 Cr1 N2 80.83(12) . . ? C1 O1 Cr1 129.3(2) . . ? C14 O2 Cr1 127.13(19) . . ? Cr1 O3 Cr1 100.04(10) . 3_657 ? Cr1 O3 H3A 103(3) . . ? Cr1 O3 H3A 116(3) 3_657 . ? C15 N1 C8 110.5(3) . . ? C15 N1 C7 109.7(3) . . ? C8 N1 C7 109.7(3) . . ? C15 N1 Cr1 107.4(2) . . ? C8 N1 Cr1 111.93(19) . . ? C7 N1 Cr1 107.5(2) . . ? C16 N2 C20 118.4(3) . . ? C16 N2 Cr1 114.5(2) . . ? C20 N2 Cr1 125.8(2) . . ? O1 C1 C6 120.9(3) . . ? O1 C1 C2 120.0(4) . . ? C6 C1 C2 119.1(4) . . ? C3 C2 C1 116.1(4) . . ? C3 C2 C21 122.0(4) . . ? C1 C2 C21 121.9(4) . . ? C4 C3 C2 124.7(4) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C5 C4 C3 117.5(4) . . ? C5 C4 C25 122.9(6) . . ? C3 C4 C25 119.6(5) . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 C7 118.7(4) . . ? C1 C6 C7 120.7(3) . . ? C6 C7 N1 112.4(3) . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? N1 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C9 116.7(3) . . ? N1 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? N1 C8 H8B 108.1 . . ? C9 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C14 120.5(3) . . ? C10 C9 C8 120.7(3) . . ? C14 C9 C8 118.1(3) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 C10 117.4(3) . . ? C12 C11 C26 120.5(4) . . ? C10 C11 C26 121.9(4) . . ? C11 C12 C13 124.0(4) . . ? C11 C12 H12 118.0 . . ? C13 C12 H12 118.0 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 C27 121.1(3) . . ? C14 C13 C27 121.0(3) . . ? O2 C14 C9 119.8(3) . . ? O2 C14 C13 121.6(3) . . ? C9 C14 C13 118.6(3) . . ? N1 C15 C16 111.3(3) . . ? N1 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N1 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N2 C16 C17 121.1(4) . . ? N2 C16 C15 113.9(3) . . ? C17 C16 C15 124.9(4) . . ? C18 C17 C16 119.8(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.5(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N2 C20 C19 122.1(4) . . ? N2 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C2 C21 C24 112.3(4) . . ? C2 C21 C23 112.4(5) . . ? C24 C21 C23 107.7(4) . . ? C2 C21 C22 109.1(4) . . ? C24 C21 C22 108.7(5) . . ? C23 C21 C22 106.5(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 C25 H25A 109.5 . . ? C4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C11 C26 H26A 109.5 . . ? C11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C13 109.9(3) . . ? C30 C27 C28 109.2(3) . . ? C13 C27 C28 110.9(3) . . ? C30 C27 C29 108.4(4) . . ? C13 C27 C29 112.4(3) . . ? C28 C27 C29 106.0(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 O2 Cr1 O1 C1 -86.9(3) . . . . ? O3 Cr1 O1 C1 179.4(3) . . . . ? O3 Cr1 O1 C1 99.4(3) 3_657 . . . ? N1 Cr1 O1 C1 5.2(3) . . . . ? O1 Cr1 O2 C14 125.0(2) . . . . ? O3 Cr1 O2 C14 -143.7(2) . . . . ? N1 Cr1 O2 C14 33.5(3) . . . . ? N2 Cr1 O2 C14 -47.2(3) . . . . ? O1 Cr1 O3 Cr1 -90.78(11) . . . 3_657 ? O2 Cr1 O3 Cr1 177.13(10) . . . 3_657 ? O3 Cr1 O3 Cr1 0.0 3_657 . . 3_657 ? N2 Cr1 O3 Cr1 89.92(11) . . . 3_657 ? O1 Cr1 N1 C15 158.5(2) . . . . ? O2 Cr1 N1 C15 -109.4(2) . . . . ? O3 Cr1 N1 C15 67.4(2) 3_657 . . . ? N2 Cr1 N1 C15 -23.0(2) . . . . ? O1 Cr1 N1 C8 -80.0(2) . . . . ? O2 Cr1 N1 C8 12.0(2) . . . . ? O3 Cr1 N1 C8 -171.1(2) 3_657 . . . ? N2 Cr1 N1 C8 98.5(3) . . . . ? O1 Cr1 N1 C7 40.5(2) . . . . ? O2 Cr1 N1 C7 132.6(2) . . . . ? O3 Cr1 N1 C7 -50.5(2) 3_657 . . . ? N2 Cr1 N1 C7 -141.0(2) . . . . ? O2 Cr1 N2 C16 97.8(2) . . . . ? O3 Cr1 N2 C16 -168.9(2) . . . . ? O3 Cr1 N2 C16 -88.9(2) 3_657 . . . ? N1 Cr1 N2 C16 5.2(2) . . . . ? O2 Cr1 N2 C20 -69.1(3) . . . . ? O3 Cr1 N2 C20 24.3(3) . . . . ? O3 Cr1 N2 C20 104.3(3) 3_657 . . . ? N1 Cr1 N2 C20 -161.7(3) . . . . ? Cr1 O1 C1 C6 -29.7(5) . . . . ? Cr1 O1 C1 C2 149.0(3) . . . . ? O1 C1 C2 C3 173.0(3) . . . . ? C6 C1 C2 C3 -8.2(5) . . . . ? O1 C1 C2 C21 -9.3(6) . . . . ? C6 C1 C2 C21 169.4(4) . . . . ? C1 C2 C3 C4 4.7(6) . . . . ? C21 C2 C3 C4 -173.0(4) . . . . ? C2 C3 C4 C5 1.5(7) . . . . ? C2 C3 C4 C25 -179.9(5) . . . . ? C3 C4 C5 C6 -4.2(7) . . . . ? C25 C4 C5 C6 177.3(5) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C4 C5 C6 C7 -179.7(4) . . . . ? O1 C1 C6 C5 -175.2(4) . . . . ? C2 C1 C6 C5 6.0(6) . . . . ? O1 C1 C6 C7 4.9(5) . . . . ? C2 C1 C6 C7 -173.8(3) . . . . ? C5 C6 C7 N1 -130.4(4) . . . . ? C1 C6 C7 N1 49.5(5) . . . . ? C15 N1 C7 C6 174.1(3) . . . . ? C8 N1 C7 C6 52.6(4) . . . . ? Cr1 N1 C7 C6 -69.4(3) . . . . ? C15 N1 C8 C9 65.7(4) . . . . ? C7 N1 C8 C9 -173.2(3) . . . . ? Cr1 N1 C8 C9 -54.0(4) . . . . ? N1 C8 C9 C10 -129.1(3) . . . . ? N1 C8 C9 C14 60.5(4) . . . . ? C14 C9 C10 C11 1.1(5) . . . . ? C8 C9 C10 C11 -169.1(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C9 C10 C11 C26 177.0(3) . . . . ? C10 C11 C12 C13 -1.3(5) . . . . ? C26 C11 C12 C13 -177.5(3) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? C11 C12 C13 C27 176.1(3) . . . . ? Cr1 O2 C14 C9 -38.3(4) . . . . ? Cr1 O2 C14 C13 143.5(2) . . . . ? C10 C9 C14 O2 179.2(3) . . . . ? C8 C9 C14 O2 -10.3(4) . . . . ? C10 C9 C14 C13 -2.5(5) . . . . ? C8 C9 C14 C13 167.9(3) . . . . ? C12 C13 C14 O2 -179.8(3) . . . . ? C27 C13 C14 O2 4.0(5) . . . . ? C12 C13 C14 C9 2.0(4) . . . . ? C27 C13 C14 C9 -174.2(3) . . . . ? C8 N1 C15 C16 -85.4(3) . . . . ? C7 N1 C15 C16 153.5(3) . . . . ? Cr1 N1 C15 C16 36.9(3) . . . . ? C20 N2 C16 C17 -0.5(5) . . . . ? Cr1 N2 C16 C17 -168.4(3) . . . . ? C20 N2 C16 C15 -177.7(3) . . . . ? Cr1 N2 C16 C15 14.4(4) . . . . ? N1 C15 C16 N2 -34.9(4) . . . . ? N1 C15 C16 C17 148.0(4) . . . . ? N2 C16 C17 C18 1.0(6) . . . . ? C15 C16 C17 C18 177.9(4) . . . . ? C16 C17 C18 C19 -0.9(7) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? C16 N2 C20 C19 0.0(5) . . . . ? Cr1 N2 C20 C19 166.4(3) . . . . ? C18 C19 C20 N2 0.1(7) . . . . ? C3 C2 C21 C24 -118.6(5) . . . . ? C1 C2 C21 C24 63.9(6) . . . . ? C3 C2 C21 C23 3.0(7) . . . . ? C1 C2 C21 C23 -174.5(5) . . . . ? C3 C2 C21 C22 120.8(5) . . . . ? C1 C2 C21 C22 -56.7(5) . . . . ? C12 C13 C27 C30 -117.2(4) . . . . ? C14 C13 C27 C30 58.9(4) . . . . ? C12 C13 C27 C28 122.0(4) . . . . ? C14 C13 C27 C28 -61.9(4) . . . . ? C12 C13 C27 C29 3.6(5) . . . . ? C14 C13 C27 C29 179.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.795 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.099