# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Cr2bpy3_4.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-01-18 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name ; Juri\'c , Marijana ; _publ_contact_author_address ; Rudjer Bo\2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0962P)^2^+1.0931P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef none _refine_ls_number_reflns 3942 _refine_ls_number_parameters 274 _refine_ls_number_restraints 18 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.146 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(7) _refine_diff_density_max 0.744 _refine_diff_density_min -0.275 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_group _atom_site_disorder_assembly Cr1 Cr 0.66084(3) 0.32168(6) 0 0.0452(2) Uani 1 d S . . Cr2 Cr 0.31715(3) 0.68285(3) 0.1667 0.0423(2) Uani 1 d S . . O1 O 0.7820(2) 0.4468(2) 0.02788(5) 0.0556(6) Uani 1 d . . . O2 O 0.8824(3) 0.6410(3) 0.03018(9) 0.0902(11) Uani 1 d . . . O3 O 0.3102(2) 0.5586(2) 0.13667(5) 0.0527(5) Uani 1 d . . . O4 O 0.19611(19) 0.5516(2) 0.19429(5) 0.0510(5) Uani 1 d . . . O5 O 0.2373(3) 0.3681(3) 0.13650(8) 0.0772(8) Uani 1 d . . . O6 O 0.1100(2) 0.3592(2) 0.19756(7) 0.0686(7) Uani 1 d . . . O7 O 0.9355(7) 0.8711(14) 0 0.330(8) Uani 1 d SU . . O8 O 0 1 0.0899(3) 0.268(8) Uani 1 d SU . . O9 O 0.1562(6) 1.1348(6) 0.1488(3) 0.125(3) Uani 0.5 d PU . . N1 N 0.5283(2) 0.3079(2) 0.03215(6) 0.0502(6) Uani 1 d . . . N2 N 0.5171(2) 0.2000(2) -0.02806(6) 0.0453(5) Uani 1 d . . . N3 N 0.1950(2) 0.6996(2) 0.13698(6) 0.0448(5) Uani 1 d . . . C1 C 0.5426(4) 0.3631(3) 0.06378(8) 0.0632(9) Uani 1 d . . . C2 C 0.4506(5) 0.3541(4) 0.08317(9) 0.0735(12) Uani 1 d . . . C3 C 0.3398(5) 0.2888(4) 0.06883(11) 0.0804(12) Uani 1 d . . . C4 C 0.3246(4) 0.2322(4) 0.03653(11) 0.0721(10) Uani 1 d . . . C5 C 0.4203(3) 0.2413(3) 0.01890(8) 0.0513(7) Uani 1 d . . . C6 C 0.4138(3) 0.1807(3) -0.01503(8) 0.0487(6) Uani 1 d . . . C7 C 0.3106(3) 0.1075(3) -0.03269(9) 0.0604(8) Uani 1 d . . . C8 C 0.3132(3) 0.0523(3) -0.06397(9) 0.0603(8) Uani 1 d . . . C9 C 0.4181(3) 0.0738(3) -0.07747(9) 0.0572(8) Uani 1 d . . . C10 C 0.5180(3) 0.1476(3) -0.05896(7) 0.0530(7) Uani 1 d . . . C11 C 0.8094(3) 0.5504(3) 0.01665(9) 0.0590(8) Uani 1 d . . . C12 C 0.1447(3) 0.6402(3) 0.10682(8) 0.0542(7) Uani 1 d . . . C13 C 0.0596(3) 0.6526(3) 0.08892(10) 0.0631(9) Uani 1 d . . . C14 C 0.0261(3) 0.7276(4) 0.10278(9) 0.0633(9) Uani 1 d . . . C16 C 0.1634(3) 0.7741(3) 0.15021(8) 0.0474(6) Uani 1 d . . . C15 C 0.0773(3) 0.7885(4) 0.13384(9) 0.0610(8) Uani 1 d . . . C17 C 0.2457(3) 0.4553(3) 0.14941(9) 0.0514(7) Uani 1 d . . . C18 C 0.1765(3) 0.4516(3) 0.18344(8) 0.0476(6) Uani 1 d . . . H1 H 0.6175 0.4088 0.0728 0.076 Uiso 1 calc R . . H2 H 0.4622 0.3907 0.1053 0.088 Uiso 1 calc R . . H3 H 0.276 0.2834 0.081 0.096 Uiso 1 calc R . . H4 H 0.2506 0.1883 0.0267 0.087 Uiso 1 calc R . . H7 H 0.2402 0.0956 -0.0236 0.072 Uiso 1 calc R . . H8 H 0.2444 0.0011 -0.0757 0.072 Uiso 1 calc R . . H9 H 0.4217 0.0391 -0.0988 0.069 Uiso 1 calc R . . H10 H 0.5891 0.1619 -0.0682 0.064 Uiso 1 calc R . . H12 H 0.1674 0.5893 0.0976 0.065 Uiso 1 calc R . . H13 H 0.0259 0.6111 0.068 0.076 Uiso 1 calc R . . H14 H -0.0308 0.737 0.0912 0.076 Uiso 1 calc R . . H15 H 0.0546 0.8385 0.1437 0.073 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 0.0518(3) 0.0473(3) 0.0351(3) 0 -0.0063(2) 0.02366(17) Cr2 0.0457(3) 0.0457(3) 0.0353(3) 0.0003(2) 0.0003(2) 0.0225(3) O1 0.0651(13) 0.0515(12) 0.0463(10) -0.0019(9) -0.0202(10) 0.0263(11) O2 0.101(2) 0.0592(16) 0.092(2) -0.0099(15) -0.0523(19) 0.0262(16) O3 0.0602(13) 0.0555(12) 0.0439(9) 0.0009(9) 0.0120(9) 0.0300(10) O4 0.0541(12) 0.0532(12) 0.0442(9) 0.0004(9) 0.0112(9) 0.0256(10) O5 0.099(2) 0.0621(15) 0.0788(16) -0.0079(14) 0.0210(16) 0.0460(15) O6 0.0670(15) 0.0547(14) 0.0719(15) 0.0113(12) 0.0215(13) 0.0213(12) O7 0.273(9) 0.351(10) 0.392(12) 0 0.025(8) 0.176(5) O8 0.311(12) 0.238(10) 0.321(13) 0 0 0.187(9) O9 0.062(3) 0.081(4) 0.223(8) 0.046(5) -0.015(5) 0.029(3) N1 0.0667(16) 0.0547(14) 0.0378(10) -0.0021(10) -0.0036(11) 0.0367(14) N2 0.0505(13) 0.0449(12) 0.0398(10) -0.0033(10) -0.0046(10) 0.0234(10) N3 0.0431(12) 0.0488(13) 0.0394(10) -0.0005(10) -0.0024(9) 0.0208(11) C1 0.090(3) 0.067(2) 0.0440(14) -0.0075(15) -0.0052(16) 0.048(2) C2 0.118(4) 0.073(2) 0.0461(15) -0.0013(16) 0.0105(19) 0.060(3) C3 0.101(4) 0.083(3) 0.071(2) 0.003(2) 0.027(2) 0.057(3) C4 0.071(2) 0.075(2) 0.072(2) -0.0010(19) 0.013(2) 0.038(2) C5 0.0617(18) 0.0516(16) 0.0448(14) 0.0028(13) 0.0010(13) 0.0316(15) C6 0.0546(16) 0.0464(15) 0.0451(13) 0.0041(12) 0.0010(12) 0.0252(13) C7 0.0532(18) 0.0581(18) 0.0596(17) 0.0037(15) -0.0009(15) 0.0202(15) C8 0.060(2) 0.0490(17) 0.0572(17) -0.0034(14) -0.0152(16) 0.0166(15) C9 0.069(2) 0.0489(16) 0.0503(15) -0.0070(14) -0.0092(15) 0.0270(15) C10 0.0626(19) 0.0545(17) 0.0443(13) -0.0077(13) -0.0037(13) 0.0311(15) C11 0.064(2) 0.0568(18) 0.0533(16) -0.0009(15) -0.0177(16) 0.0278(16) C12 0.0519(17) 0.0521(17) 0.0500(14) -0.0030(13) -0.0081(13) 0.0196(14) C13 0.0551(19) 0.060(2) 0.0557(17) 0.0028(15) -0.0131(15) 0.0150(16) C14 0.054(2) 0.075(2) 0.0580(17) 0.0080(17) -0.0073(14) 0.0298(18) C15 0.0561(18) 0.074(2) 0.0589(17) 0.0062(17) -0.0001(15) 0.0375(17) C16 0.0451(14) 0.0482(15) 0.0451(13) 0.0063(13) 0.0020(12) 0.0206(12) C17 0.0553(18) 0.0556(16) 0.0480(14) 0.0007(13) 0.0071(13) 0.0312(14) C18 0.0447(14) 0.0494(15) 0.0458(13) 0.0005(12) 0.0042(12) 0.0212(12) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 1.936(2) . ? Cr1 O1 1.936(2) 6_655 ? Cr1 N1 2.058(3) 6_655 ? Cr1 N1 2.058(3) . ? Cr1 N2 2.063(2) 6_655 ? Cr1 N2 2.063(2) . ? Cr2 O3 1.954(2) 3_665 ? Cr2 O3 1.954(2) . ? Cr2 O4 1.968(2) . ? Cr2 O4 1.968(2) 3_665 ? Cr2 N3 2.063(3) 3_665 ? Cr2 N3 2.063(3) . ? O1 C11 1.304(4) . ? O2 C11 1.214(4) . ? O3 C17 1.290(4) . ? O4 C18 1.283(4) . ? O5 C17 1.206(4) . ? O6 C18 1.216(4) . ? O9 O9 1.414(19) 4_465 ? N1 C5 1.346(4) . ? N2 C6 1.353(4) . ? N2 C10 1.346(4) . ? N3 C12 1.341(4) . ? N3 C16 1.345(4) . ? C1 N1 1.348(4) . ? C1 C2 1.371(6) . ? C1 H1 0.93 . ? C2 C3 1.388(7) . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 C3 1.377(6) . ? C4 C5 1.380(5) . ? C4 H4 0.93 . ? C6 C5 1.475(5) . ? C6 C7 1.385(5) . ? C7 C8 1.384(5) . ? C7 H7 0.93 . ? C8 C9 1.369(6) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? C10 C9 1.376(5) . ? C10 H10 0.93 . ? C11 C11 1.534(6) 6_655 ? C12 H12 0.93 . ? C12 C13 1.391(5) . ? C13 C14 1.376(6) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C14 1.378(5) . ? C15 H15 0.93 . ? C16 C15 1.390(4) . ? C16 C16 1.478(6) 3_665 ? C18 C17 1.550(4) . ? 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 84.07(13) . 6_655 ? O1 Cr1 N1 92.42(11) . 6_655 ? O1 Cr1 N1 94.14(11) 6_655 6_655 ? O1 Cr1 N1 94.14(11) . . ? O1 Cr1 N1 92.42(11) 6_655 . ? O1 Cr1 N2 91.04(10) . 6_655 ? O1 Cr1 N2 171.41(11) 6_655 6_655 ? O1 Cr1 N2 171.41(11) . . ? O1 Cr1 N2 91.04(10) 6_655 . ? O1 C11 C11 113.92(16) . 6_655 ? O2 C11 O1 125.2(3) . . ? O2 C11 C11 120.9(2) . 6_655 ? O3 Cr2 O3 92.76(14) 3_665 . ? O3 Cr2 O4 92.30(9) 3_665 . ? O3 Cr2 O4 82.99(9) . . ? O3 Cr2 O4 82.99(9) 3_665 3_665 ? O3 Cr2 O4 92.30(9) . 3_665 ? O3 Cr2 N3 94.46(10) 3_665 3_665 ? O3 Cr2 N3 171.96(11) . 3_665 ? O3 Cr2 N3 171.96(11) 3_665 . ? O3 Cr2 N3 94.46(10) . . ? O3 C17 C18 113.7(3) . . ? O4 Cr2 O4 173.19(14) . 3_665 ? O4 Cr2 N3 93.17(9) . 3_665 ? O4 Cr2 N3 92.10(10) 3_665 3_665 ? O4 Cr2 N3 92.10(10) . . ? O4 Cr2 N3 93.17(9) 3_665 . ? O4 C18 C17 114.4(3) . . ? O5 C17 O3 124.6(3) . . ? O5 C17 C18 121.7(3) . . ? O6 C18 O4 125.3(3) . . ? O6 C18 C17 120.3(3) . . ? N1 Cr1 N1 171.16(16) 6_655 . ? N1 Cr1 N2 78.98(10) 6_655 6_655 ? N1 Cr1 N2 94.98(10) . 6_655 ? N1 Cr1 N2 94.98(10) 6_655 . ? N1 Cr1 N2 78.98(10) . . ? N1 C1 C2 122.3(4) . . ? N1 C1 H1 118.9 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 115.1(3) . . ? N2 Cr1 N2 94.65(14) 6_655 . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 115.2(3) . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10 118.6 . . ? N3 Cr2 N3 78.58(14) 3_665 . ? N3 C16 C15 121.4(3) . . ? N3 C16 C16 114.92(16) . 3_665 ? N3 C12 C13 121.7(3) . . ? N3 C12 H12 119.2 . . ? C1 N1 Cr1 125.2(3) . . ? C1 C2 C3 118.2(3) . . ? C1 C2 H2 120.9 . . ? C2 C1 H1 118.9 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.3(4) . . ? C3 C2 H2 120.9 . . ? C3 C4 H4 120.4 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.1 . . ? C4 C5 C6 123.9(3) . . ? C5 C4 H4 120.4 . . ? C5 N1 C1 119.4(3) . . ? C5 N1 Cr1 115.4(2) . . ? C6 N2 Cr1 114.87(19) . . ? C6 C7 H7 120.2 . . ? C7 C6 C5 123.8(3) . . ? C7 C8 H8 120.4 . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.2 . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9 120.6 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.4 . . ? C9 C10 H10 118.6 . . ? C10 N2 Cr1 126.3(2) . . ? C10 N2 C6 118.6(3) . . ? C10 C9 H9 120.6 . . ? C11 O1 Cr1 114.04(19) . . ? C12 N3 Cr2 124.8(2) . . ? C12 N3 C16 119.5(3) . . ? C12 C13 H13 120.6 . . ? C13 C12 H12 119.2 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C14 C15 C16 118.9(4) . . ? C14 C15 H15 120.5 . . ? C15 C16 C16 123.7(2) . 3_665 ? C15 C14 H14 120.2 . . ? C16 N3 Cr2 115.74(19) . . ? C16 C15 H15 120.5 . . ? C17 O3 Cr2 114.42(18) . . ? C18 O4 Cr2 113.90(18) . . ? 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 Cr1 O1 C11 O2 179.6(4) . . . . ? Cr1 O1 C11 C11 -1.1(5) . . . 6_655 ? Cr1 N1 C5 C4 -175.0(3) . . . . ? Cr1 N2 C6 C5 -5.5(3) . . . . ? Cr1 N1 C5 C6 5.1(4) . . . . ? Cr1 N2 C6 C7 175.4(3) . . . . ? Cr1 N2 C10 C9 -174.9(2) . . . . ? Cr2 O3 C17 O5 -173.9(3) . . . . ? Cr2 O3 C17 C18 6.8(4) . . . . ? Cr2 O4 C18 O6 176.1(3) . . . . ? Cr2 O4 C18 C17 -4.1(3) . . . . ? Cr2 N3 C12 C13 177.5(2) . . . . ? Cr2 N3 C16 C15 -176.5(3) . . . . ? Cr2 N3 C16 C16 2.9(4) . . . 3_665 ? O1 Cr1 O1 C11 0.4(2) 6_655 . . . ? O1 Cr1 N1 C5 168.6(2) . . . . ? O1 Cr1 N1 C5 84.4(2) 6_655 . . . ? O1 Cr1 N1 C1 -8.6(3) . . . . ? O1 Cr1 N1 C1 -92.9(3) 6_655 . . . ? O1 Cr1 N2 C10 143.2(5) . . . . ? O1 Cr1 N2 C10 88.0(3) 6_655 . . . ? O1 Cr1 N2 C6 -30.9(7) . . . . ? O1 Cr1 N2 C6 -86.0(2) 6_655 . . . ? O3 Cr2 O3 C17 84.7(2) 3_665 . . . ? O3 Cr2 O4 C18 -86.4(2) 3_665 . . . ? O3 Cr2 O4 C18 6.1(2) . . . . ? O3 Cr2 N3 C16 -31.4(7) 3_665 . . . ? O3 Cr2 N3 C16 174.8(2) . . . . ? O3 Cr2 N3 C12 150.4(6) 3_665 . . . ? O3 Cr2 N3 C12 -3.3(3) . . . . ? O4 Cr2 O3 C17 -7.2(2) . . . . ? O4 Cr2 O4 C18 -40.3(2) 3_665 . . . ? O4 Cr2 O3 C17 167.8(2) 3_665 . . . ? O4 Cr2 N3 C12 -86.4(3) . . . . ? O4 Cr2 N3 C12 89.3(3) 3_665 . . . ? O4 Cr2 N3 C16 91.7(2) . . . . ? O4 Cr2 N3 C16 -92.6(2) 3_665 . . . ? O4 C18 C17 O3 -1.8(4) . . . . ? O4 C18 C17 O5 178.9(3) . . . . ? O6 C18 C17 O5 -1.3(6) . . . . ? O6 C18 C17 O3 178.0(3) . . . . ? N1 Cr1 O1 C11 94.4(3) 6_655 . . . ? N1 Cr1 O1 C11 -91.6(3) . . . . ? N1 Cr1 N1 C1 129.2(3) 6_655 . . . ? N1 Cr1 N1 C5 -53.5(2) 6_655 . . . ? N1 Cr1 N2 C6 179.8(2) 6_655 . . . ? N1 Cr1 N2 C6 6.3(2) . . . . ? N1 Cr1 N2 C10 -6.2(3) 6_655 . . . ? N1 Cr1 N2 C10 -179.7(3) . . . . ? N1 C1 C2 C3 -2.2(6) . . . . ? N2 Cr1 O1 C11 173.4(3) 6_655 . . . ? N2 Cr1 O1 C11 -55.1(7) . . . . ? N2 Cr1 N1 C5 -99.9(2) 6_655 . . . ? N2 Cr1 N1 C5 -6.2(2) . . . . ? N2 Cr1 N1 C1 82.8(3) 6_655 . . . ? N2 Cr1 N1 C1 176.5(3) . . . . ? N2 Cr1 N2 C6 100.5(2) 6_655 . . . ? N2 Cr1 N2 C10 -85.5(3) 6_655 . . . ? N2 C6 C5 N1 0.3(4) . . . . ? N2 C6 C5 C4 -179.6(3) . . . . ? N2 C6 C7 C8 0.6(5) . . . . ? N2 C10 C9 C8 -0.1(5) . . . . ? N3 Cr2 O3 C17 -69.0(7) 3_665 . . . ? N3 Cr2 O3 C17 -98.8(2) . . . . ? N3 Cr2 O4 C18 179.0(2) 3_665 . . . ? N3 Cr2 O4 C18 100.4(2) . . . . ? N3 Cr2 N3 C12 -179.2(3) 3_665 . . . ? N3 Cr2 N3 C16 -1.10(16) 3_665 . . . ? N3 C16 C15 C14 -2.0(5) . . . . ? N3 C12 C13 C14 -0.3(5) . . . . ? C1 N1 C5 C4 2.4(5) . . . . ? C1 N1 C5 C6 -177.4(3) . . . . ? C1 C2 C3 C4 2.2(6) . . . . ? C2 C1 N1 Cr1 177.1(3) . . . . ? C2 C1 N1 C5 -0.1(5) . . . . ? C3 C4 C5 N1 -2.4(6) . . . . ? C3 C4 C5 C6 177.5(4) . . . . ? C5 C4 C3 C2 0.0(7) . . . . ? C6 N2 C10 C9 -1.1(5) . . . . ? C5 C6 C7 C8 -178.4(3) . . . . ? C6 C7 C8 C9 -1.9(5) . . . . ? C7 C6 C5 N1 179.4(3) . . . . ? C7 C6 C5 C4 -0.5(6) . . . . ? C7 C8 C9 C10 1.6(5) . . . . ? C10 N2 C6 C7 0.8(5) . . . . ? C10 N2 C6 C5 180.0(3) . . . . ? C12 N3 C16 C15 1.8(5) . . . . ? C12 N3 C16 C16 -178.8(3) . . . 3_665 ? C12 C13 C14 C15 0.1(6) . . . . ? C16 N3 C12 C13 -0.6(5) . . . . ? C16 C16 C15 C14 178.7(4) 3_665 . . . ? C16 C15 C14 C13 1.0(6) . . . . ? # Attachment 'Cr2phen3_3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-01-05 at 13:28:33 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : lidija-482 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_lidija-482 _database_code_depnum_ccdc_archive 'CCDC 847273' #TrackingRef 'Cr2phen3_3.cif' _audit_creation_date 2011-01-05T13:28:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C26 H16 Cr N4 O4, C16 H8 Cr N2 O8, 3(H2 O)' _chemical_formula_sum 'C42 H30 Cr2 N6 O15' _chemical_formula_weight 962.72 _chemical_absolute_configuration unk #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 62 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, -x, -z+2/3' 'y, x, -z+2/3' 'x-y, -y, -z' '-x+y, y, -z' 'x, x-y, -z+1/3' '-x, -x+y, -z+1/3' '-y, x-y, z+2/3' 'y, -x+y, z+2/3' 'x-y, x, z+1/3' '-x+y, -x, z+1/3' _cell_length_a 13.7894(2) _cell_length_b 13.7894(2) _cell_length_c 36.2999(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5977.60(16) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9278 _cell_measurement_theta_min 2.4324 _cell_measurement_theta_max 76.0594 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 5.219 _cell_oxdiff_measurement_reflns_used 9256 _exptl_absorpt_correction_T_min 0.44440 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(3) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4323 _diffrn_reflns_number 21473 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 76.25 _diffrn_reflns_theta_full 76.25 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 4164 _reflns_number_gt 3679 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0570P)^2^+0.6487P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00012(3) _refine_ls_number_reflns 4164 _refine_ls_number_parameters 308 _refine_ls_number_restraints 4 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1017 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(5) _refine_diff_density_max 0.161 _refine_diff_density_min -0.261 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_group _atom_site_disorder_assembly Cr1 Cr 0.68246(4) 0.341230(18) 0.1667 0.03229(13) Uani 1 d S . . Cr2 Cr 0.676101(18) 0.35220(4) 0 0.03120(13) Uani 1 d S . . O1 O 0.56237(13) 0.33629(13) 0.13779(4) 0.0403(3) Uani 1 d . . . O2 O 0.37702(16) 0.2381(2) 0.13260(6) 0.0708(6) Uani 1 d . . . O3 O 0.68748(14) 0.23958(13) -0.02948(4) 0.0424(3) Uani 1 d . . . O4 O 0.79081(13) 0.34499(13) 0.02994(4) 0.0397(3) Uani 1 d . . . O5 O 0.7653(2) 0.13250(18) -0.02872(6) 0.0715(6) Uani 1 d . . . O6 O 0.88159(17) 0.25077(17) 0.03462(6) 0.0627(5) Uani 1 d . . . O7 O -0.13805(19) 0.0365(2) 0.04363(8) 0.0756(6) Uani 1 d D . . O8 O 0 0 0.09177(11) 0.0788(9) Uani 1 d SD . . N1 N 0.69050(16) 0.46719(15) 0.19935(4) 0.0376(4) Uani 1 d . . . N2 N 0.80142(14) 0.47976(15) 0.13782(4) 0.0360(4) Uani 1 d . . . N3 N 0.68727(15) 0.48553(15) 0.03004(4) 0.0343(3) Uani 1 d . . . C1 C 0.6370(2) 0.4587(2) 0.23073(6) 0.0467(5) Uani 1 d . . . C2 C 0.6393(2) 0.5514(3) 0.24730(6) 0.0566(6) Uani 1 d . . . C3 C 0.6951(2) 0.6544(2) 0.23071(7) 0.0543(6) Uani 1 d . . . C4 C 0.7548(2) 0.6661(2) 0.19807(6) 0.0466(5) Uani 1 d . . . C5 C 0.8201(2) 0.7709(2) 0.17923(8) 0.0554(6) Uani 1 d . . . C6 C 0.8793(2) 0.7777(2) 0.14871(8) 0.0569(6) Uani 1 d . . . C7 C 0.87925(18) 0.6818(2) 0.13409(6) 0.0453(5) Uani 1 d . . . C8 C 0.93996(19) 0.6823(2) 0.10257(6) 0.0513(6) Uani 1 d . . . C9 C 0.9287(2) 0.5850(2) 0.08949(6) 0.0519(6) Uani 1 d . . . C10 C 0.85718(19) 0.4834(2) 0.10736(6) 0.0450(5) Uani 1 d . . . C11 C 0.81222(17) 0.57748(18) 0.15106(6) 0.0368(4) Uani 1 d . . . C12 C 0.75158(18) 0.57065(18) 0.18377(6) 0.0376(4) Uani 1 d . . . C13 C 0.46222(19) 0.2617(2) 0.14847(6) 0.0422(5) Uani 1 d . . . C14 C 0.6316(2) 0.4829(2) 0.06027(6) 0.0433(5) Uani 1 d . . . C15 C 0.6460(2) 0.5806(2) 0.07705(6) 0.0507(6) Uani 1 d . . . C16 C 0.7192(2) 0.6829(2) 0.06237(7) 0.0511(6) Uani 1 d . . . C17 C 0.7821(2) 0.6890(2) 0.03092(6) 0.0432(5) Uani 1 d . . . C18 C 0.8653(2) 0.7913(2) 0.01475(7) 0.0541(6) Uani 1 d . . . C19 C 0.76309(17) 0.58740(17) 0.01602(6) 0.0339(4) Uani 1 d . . . C20 C 0.7521(2) 0.20601(19) -0.01591(6) 0.0427(5) Uani 1 d . . . C21 C 0.81575(19) 0.27085(19) 0.01948(6) 0.0400(5) Uani 1 d . . . H1 H 0.5967 0.3891 0.242 0.056 Uiso 1 calc R . . H2 H 0.6029 0.5431 0.2696 0.068 Uiso 1 calc R . . H3 H 0.6934 0.7154 0.2409 0.065 Uiso 1 calc R . . H5 H 0.8215 0.8349 0.1881 0.066 Uiso 1 calc R . . H6 H 0.9211 0.8465 0.137 0.068 Uiso 1 calc R . . H7A H -0.137(3) 0.102(2) 0.0398(10) 0.101(14) Uiso 1 d D . . H7B H -0.189(3) -0.011(3) 0.0265(9) 0.119(17) Uiso 1 d D . . H8 H 0.9877 0.7496 0.0908 0.062 Uiso 1 calc R . . H8A H -0.038(3) 0.013(3) 0.0744(7) 0.069(10) Uiso 1 d D . . H9 H 0.9684 0.5855 0.0687 0.062 Uiso 1 calc R . . H10 H 0.8485 0.4171 0.0977 0.054 Uiso 1 calc R . . H14 H 0.5816 0.4139 0.0706 0.052 Uiso 1 calc R . . H15 H 0.6058 0.576 0.0982 0.061 Uiso 1 calc R . . H16 H 0.7275 0.748 0.073 0.061 Uiso 1 calc R . . H18 H 0.8782 0.8591 0.0245 0.065 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 0.0314(2) 0.03412(18) 0.0304(2) 0.00469(13) 0 0.01572(12) Cr2 0.03155(18) 0.0308(2) 0.0310(2) 0 -0.00198(13) 0.01542(11) O1 0.0375(8) 0.0445(8) 0.0386(7) 0.0126(6) -0.0011(6) 0.0202(7) O2 0.0405(10) 0.0939(16) 0.0727(11) 0.0277(11) -0.0059(9) 0.0294(10) O3 0.0495(9) 0.0422(8) 0.0396(7) -0.0105(6) -0.0120(7) 0.0259(7) O4 0.0408(8) 0.0407(8) 0.0401(7) -0.0099(6) -0.0140(6) 0.0223(7) O5 0.0943(16) 0.0640(12) 0.0788(12) -0.0298(10) -0.0248(12) 0.0566(13) O6 0.0613(11) 0.0622(11) 0.0792(12) -0.0194(10) -0.0337(10) 0.0417(10) O7 0.0579(12) 0.0642(14) 0.1117(18) 0.0025(13) 0.0001(12) 0.0357(11) O8 0.094(3) 0.074(2) 0.0684(17) 0 0 0.0419(19) N1 0.0400(9) 0.0402(9) 0.0333(7) 0.0029(7) 0.0014(7) 0.0207(8) N2 0.0312(8) 0.0387(9) 0.0334(7) 0.0064(7) 0.0036(6) 0.0141(7) N3 0.0371(9) 0.0372(9) 0.0326(7) -0.0002(6) 0.0006(6) 0.0216(7) C1 0.0443(12) 0.0572(14) 0.0383(9) 0.0043(9) 0.0039(9) 0.0251(11) C2 0.0559(15) 0.0805(19) 0.0412(10) -0.0081(12) 0.0025(11) 0.0401(15) C3 0.0556(15) 0.0636(16) 0.0545(12) -0.0185(11) -0.0112(11) 0.0378(14) C4 0.0427(12) 0.0487(13) 0.0530(12) -0.0073(10) -0.0100(10) 0.0262(10) C5 0.0523(14) 0.0386(12) 0.0761(15) -0.0059(11) -0.0124(13) 0.0234(11) C6 0.0465(13) 0.0385(12) 0.0766(16) 0.0098(11) -0.0082(12) 0.0145(11) C7 0.0331(10) 0.0428(12) 0.0519(11) 0.0107(10) -0.0036(9) 0.0129(9) C8 0.0349(12) 0.0554(14) 0.0508(12) 0.0182(11) 0.0048(9) 0.0130(11) C9 0.0404(12) 0.0687(16) 0.0421(10) 0.0146(11) 0.0089(9) 0.0240(11) C10 0.0388(11) 0.0562(14) 0.0382(9) 0.0049(9) 0.0046(8) 0.0223(10) C11 0.0298(9) 0.0382(10) 0.0389(9) 0.0047(8) -0.0022(8) 0.0143(8) C12 0.0331(10) 0.0386(11) 0.0403(10) 0.0011(8) -0.0043(8) 0.0173(9) C13 0.0391(11) 0.0473(12) 0.0434(10) 0.0083(9) 0.0001(9) 0.0241(10) C14 0.0442(12) 0.0525(13) 0.0381(9) 0.0001(9) 0.0020(9) 0.0279(11) C15 0.0509(13) 0.0714(16) 0.0420(10) -0.0117(11) -0.0012(10) 0.0397(13) C16 0.0573(14) 0.0562(14) 0.0530(12) -0.0193(11) -0.0112(11) 0.0383(13) C17 0.0465(12) 0.0429(11) 0.0473(10) -0.0073(10) -0.0113(9) 0.0276(10) C18 0.0515(14) 0.0349(11) 0.0740(15) -0.0069(11) -0.0116(11) 0.0200(10) C19 0.0325(10) 0.0348(10) 0.0366(8) -0.0013(8) -0.0055(8) 0.0185(8) C20 0.0465(12) 0.0375(11) 0.0458(10) -0.0082(9) -0.0096(9) 0.0223(10) C21 0.0365(11) 0.0371(10) 0.0453(10) -0.0031(9) -0.0064(9) 0.0175(9) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 1.9321(15) 7 ? Cr1 O1 1.9321(15) . ? Cr1 N1 2.0602(18) 7 ? Cr1 N2 2.0744(17) 7 ? Cr1 N2 2.0744(17) . ? Cr2 O3 1.9559(15) 6_655 ? Cr2 O4 1.9623(14) 6_655 ? Cr2 O4 1.9623(14) . ? Cr2 N3 2.0761(17) . ? Cr2 N3 2.0761(17) 6_655 ? O1 C13 1.302(3) . ? O3 Cr2 1.9559(15) . ? O4 C21 1.288(3) . ? O5 C20 1.209(3) . ? O7 H7B 0.916(18) . ? O7 H7A 0.910(18) . ? O8 H8A 0.900(17) . ? N1 C1 1.331(3) . ? N1 Cr1 2.0602(18) . ? N2 C11 1.367(3) . ? N3 C19 1.363(3) . ? C1 C2 1.397(4) . ? C1 H1 0.93 . ? C2 C3 1.371(4) . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 C3 1.405(4) . ? C4 C5 1.437(4) . ? C4 C12 1.395(3) . ? C5 H5 0.93 . ? C6 C5 1.352(4) . ? C6 H6 0.93 . ? C7 C11 1.405(3) . ? C7 C6 1.425(4) . ? C8 C9 1.358(4) . ? C8 C7 1.416(3) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? C10 N2 1.333(3) . ? C10 C9 1.405(3) . ? C10 H10 0.93 . ? C12 N1 1.365(3) . ? C12 C11 1.428(3) . ? C13 O2 1.198(3) . ? C13 C13 1.567(4) 7 ? C14 N3 1.329(3) . ? C14 C15 1.400(3) . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 C15 1.367(4) . ? C16 C17 1.410(3) . ? C16 H16 0.93 . ? C18 C18 1.360(6) 6_655 ? C18 C17 1.426(4) . ? C18 H18 0.93 . ? C20 O3 1.290(3) . ? C20 C21 1.560(3) . ? C19 C17 1.399(3) . ? C19 C19 1.437(4) 6_655 ? C21 O6 1.206(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 O1 Cr1 O1 84.15(9) 7 . ? O1 Cr1 N1 92.48(7) 7 . ? O1 Cr1 N1 91.49(7) . . ? O1 Cr1 N1 91.49(7) 7 7 ? O1 Cr1 N1 92.48(7) . 7 ? O1 Cr1 N2 91.59(6) 7 7 ? O1 Cr1 N2 171.46(7) . 7 ? O1 Cr1 N2 171.46(7) 7 . ? O1 Cr1 N2 91.59(7) . . ? O1 C13 C13 113.00(11) . 7 ? O2 C13 O1 125.5(2) . . ? O2 C13 C13 121.53(15) . 7 ? O3 Cr2 O3 93.11(10) 6_655 . ? O3 Cr2 O4 82.88(6) 6_655 6_655 ? O3 Cr2 O4 93.65(7) . 6_655 ? O3 Cr2 O4 93.65(7) 6_655 . ? O3 Cr2 O4 82.88(6) . . ? O3 Cr2 N3 93.67(7) 6_655 . ? O3 Cr2 N3 172.19(8) . . ? O3 Cr2 N3 172.19(8) 6_655 6_655 ? O3 Cr2 N3 93.67(7) . 6_655 ? O3 C20 C21 113.59(18) . . ? O4 Cr2 O4 174.97(9) 6_655 . ? O4 Cr2 N3 91.04(7) 6_655 . ? O4 Cr2 N3 92.82(7) . . ? O4 Cr2 N3 92.82(7) 6_655 6_655 ? O4 Cr2 N3 91.04(7) . 6_655 ? O4 C21 C20 113.62(18) . . ? O5 C20 O3 125.1(2) . . ? O5 C20 C21 121.4(2) . . ? O6 C21 O4 125.3(2) . . ? O6 C21 C20 121.0(2) . . ? N1 Cr1 N1 174.66(11) . 7 ? N1 Cr1 N2 96.10(7) . 7 ? N1 Cr1 N2 80.21(7) 7 7 ? N1 Cr1 N2 80.21(7) . . ? N1 Cr1 N2 96.10(7) 7 . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1 119 . . ? N1 C12 C4 123.0(2) . . ? N1 C12 C11 116.65(19) . . ? N2 Cr1 N2 93.56(10) 7 . ? N2 C11 C7 123.1(2) . . ? N2 C11 C12 117.12(18) . . ? N2 C10 C9 121.7(2) . . ? N2 C10 H10 119.2 . . ? N3 Cr2 N3 79.84(10) . 6_655 ? N3 C14 C15 122.0(2) . . ? N3 C14 H14 119 . . ? N3 C19 C17 123.4(2) . . ? N3 C19 C19 116.76(11) . 6_655 ? C1 N1 C12 118.1(2) . . ? C1 N1 Cr1 128.73(17) . . ? C1 C2 H2 119.9 . . ? C2 C1 H1 119 . . ? C2 C3 C4 118.9(2) . . ? C2 C3 H3 120.6 . . ? C3 C2 C1 120.2(2) . . ? C3 C4 C5 123.6(2) . . ? C3 C2 H2 119.9 . . ? C4 C12 C11 120.4(2) . . ? C4 C3 H3 120.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.4(2) . . ? C5 C6 H6 119.3 . . ? C6 C5 C4 120.8(2) . . ? C6 C5 H5 119.6 . . ? C7 C11 C12 119.7(2) . . ? C7 C6 H6 119.3 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.0(2) . . ? C8 C9 H9 120 . . ? C9 C8 C7 120.2(2) . . ? C8 C7 C6 124.8(2) . . ? C9 C8 H8 119.9 . . ? C9 C10 H10 119.2 . . ? C10 N2 C11 118.55(19) . . ? C10 N2 Cr1 128.99(16) . . ? C10 C9 H9 120 . . ? C11 N2 Cr1 112.11(13) . . ? C11 C7 C8 116.4(2) . . ? C11 C7 C6 118.8(2) . . ? C12 N1 Cr1 112.80(14) . . ? C12 C4 C3 117.7(2) . . ? C12 C4 C5 118.7(2) . . ? C13 O1 Cr1 114.71(13) . . ? C14 N3 C19 118.16(19) . . ? C14 N3 Cr2 128.54(16) . . ? C14 C15 H15 120 . . ? C15 C14 H14 119 . . ? C15 C16 C17 119.4(2) . . ? C15 C16 H16 120.3 . . ? C16 C15 C14 120.0(2) . . ? C16 C17 C18 123.9(2) . . ? C16 C15 H15 120 . . ? C17 C19 C19 119.81(13) . 6_655 ? C17 C16 H16 120.3 . . ? C17 C18 H18 119.5 . . ? C18 C18 C17 121.00(14) 6_655 . ? C18 C18 H18 119.5 6_655 . ? C19 N3 Cr2 113.30(13) . . ? C19 C17 C16 116.9(2) . . ? C19 C17 C18 119.2(2) . . ? C20 O3 Cr2 114.85(13) . . ? C21 O4 Cr2 114.77(13) . . ? H7B O7 H7A 103(3) . . ? 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 Cr1 O1 C13 O2 -173.1(2) . . . . ? Cr1 O1 C13 C13 5.5(3) . . . 7 ? Cr1 N1 C1 C2 -171.19(18) . . . . ? Cr1 N2 C11 C7 -173.70(16) . . . . ? Cr1 N2 C11 C12 6.4(2) . . . . ? Cr2 O4 C21 O6 -177.9(2) . . . . ? Cr2 O4 C21 C20 2.3(2) . . . . ? Cr2 N3 C19 C17 177.74(16) . . . . ? Cr2 N3 C19 C19 -1.5(3) . . . 6_655 ? O1 Cr1 O1 C13 -2.26(13) 7 . . . ? O1 Cr1 N2 C10 -150.0(4) 7 . . . ? O1 Cr1 N2 C10 -90.15(19) . . . . ? O1 Cr1 N2 C11 22.9(5) 7 . . . ? O1 Cr1 N2 C11 82.81(14) . . . . ? O3 Cr2 N3 C14 5.35(19) 6_655 . . . ? O3 Cr2 N3 C14 -144.8(4) . . . . ? O3 Cr2 N3 C19 -175.08(14) 6_655 . . . ? O3 Cr2 N3 C19 34.7(5) . . . . ? O3 Cr2 O4 C21 88.66(16) 6_655 . . . ? O3 Cr2 O4 C21 -4.02(16) . . . . ? O3 C20 C21 O6 -177.9(2) . . . . ? O3 C20 C21 O4 1.9(3) . . . . ? O4 Cr2 O4 C21 42.49(15) 6_655 . . . ? O4 Cr2 N3 C14 88.27(18) 6_655 . . . ? O4 Cr2 N3 C14 -88.50(19) . . . . ? O4 Cr2 N3 C19 -92.15(14) 6_655 . . . ? O4 Cr2 N3 C19 91.08(14) . . . . ? O5 C20 O3 Cr2 175.5(2) . . . . ? O5 C20 C21 O6 1.5(4) . . . . ? O5 C20 C21 O4 -178.7(2) . . . . ? N1 Cr1 O1 C13 88.98(17) 7 . . . ? N1 Cr1 O1 C13 -94.60(17) . . . . ? N1 Cr1 N2 C10 178.6(2) . . . . ? N1 Cr1 N2 C10 2.51(19) 7 . . . ? N1 Cr1 N2 C11 -8.42(14) . . . . ? N1 Cr1 N2 C11 175.48(14) 7 . . . ? N1 C1 C2 C3 2.0(4) . . . . ? N1 C12 C11 N2 1.6(3) . . . . ? N1 C12 C11 C7 -178.30(19) . . . . ? N2 Cr1 O1 C13 58.1(5) 7 . . . ? N2 Cr1 O1 C13 -174.84(17) . . . . ? N2 Cr1 N2 C10 83.03(19) 7 . . . ? N2 Cr1 N2 C11 -104.01(15) 7 . . . ? N2 C10 C9 C8 -1.9(4) . . . . ? N3 Cr2 O4 C21 -177.48(16) . . . . ? N3 Cr2 O4 C21 -97.60(16) 6_655 . . . ? N3 Cr2 N3 C19 0.53(10) 6_655 . . . ? N3 Cr2 N3 C14 -179.0(2) 6_655 . . . ? N3 C14 C15 C16 -0.1(4) . . . . ? N3 C19 C17 C16 0.9(3) . . . . ? N3 C19 C17 C18 178.5(2) . . . . ? C1 N1 Cr1 O1 91.2(2) . . . . ? C1 N1 Cr1 O1 7.0(2) . . . 7 ? C1 N1 Cr1 N1 -130.85(19) . . . 7 ? C1 N1 Cr1 N2 -177.4(2) . . . . ? C1 N1 Cr1 N2 -84.8(2) . . . 7 ? C1 C2 C3 C4 -3.6(4) . . . . ? C3 C4 C12 N1 2.3(3) . . . . ? C3 C4 C12 C11 -178.8(2) . . . . ? C3 C4 C5 C6 177.3(2) . . . . ? C4 C12 N1 Cr1 170.11(17) . . . . ? C4 C12 N1 C1 -3.9(3) . . . . ? C4 C12 C11 N2 -177.35(19) . . . . ? C4 C12 C11 C7 2.7(3) . . . . ? C5 C4 C12 N1 -178.9(2) . . . . ? C5 C4 C3 C2 -177.2(2) . . . . ? C5 C4 C12 C11 0.1(3) . . . . ? C6 C7 C11 N2 176.0(2) . . . . ? C6 C7 C11 C12 -4.0(3) . . . . ? C7 C6 C5 C4 0.1(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C8 C7 C6 C5 -179.3(2) . . . . ? C8 C7 C11 N2 -2.2(3) . . . . ? C8 C7 C11 C12 177.8(2) . . . . ? C9 C8 C7 C11 2.2(3) . . . . ? C9 C8 C7 C6 -175.9(2) . . . . ? C9 C10 N2 C11 2.0(3) . . . . ? C9 C10 N2 Cr1 174.59(17) . . . . ? C10 N2 C11 C7 0.1(3) . . . . ? C10 N2 C11 C12 -179.86(19) . . . . ? C11 C7 C6 C5 2.7(4) . . . . ? C11 C12 N1 C1 177.1(2) . . . . ? C11 C12 N1 Cr1 -8.9(2) . . . . ? C12 N1 Cr1 O1 -166.22(15) . . . 7 ? C12 N1 Cr1 O1 -82.02(15) . . . . ? C12 N1 Cr1 N1 55.90(15) . . . 7 ? C12 N1 Cr1 N2 101.91(15) . . . 7 ? C12 N1 Cr1 N2 9.34(15) . . . . ? C12 N1 C1 C2 1.8(3) . . . . ? C12 C4 C3 C2 1.6(4) . . . . ? C12 C4 C5 C6 -1.5(4) . . . . ? C14 N3 C19 C17 -2.6(3) . . . . ? C14 N3 C19 C19 178.1(2) . . . 6_655 ? C15 C14 N3 Cr2 -178.22(17) . . . . ? C15 C14 N3 C19 2.2(3) . . . . ? C15 C16 C17 C19 1.3(3) . . . . ? C15 C16 C17 C18 -176.2(2) . . . . ? C17 C16 C15 C14 -1.7(4) . . . . ? C18 C18 C17 C16 177.4(3) 6_655 . . . ? C18 C18 C17 C19 -0.1(4) 6_655 . . . ? C19 C19 C17 C16 -179.9(2) 6_655 . . . ? C19 C19 C17 C18 -2.3(4) 6_655 . . . ? C20 O3 Cr2 O3 -88.11(17) . . . 6_655 ? C20 O3 Cr2 O4 -171.16(17) . . . 6_655 ? C20 O3 Cr2 O4 5.18(17) . . . . ? C20 O3 Cr2 N3 62.1(5) . . . . ? C20 O3 Cr2 N3 95.77(17) . . . 6_655 ? C21 C20 O3 Cr2 -5.2(3) . . . . ? # Attachment 'Crox2NO3-bpy_5.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-03-02 at 13:01:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : lidija_504 lidija_504-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_lidija_504 _database_code_depnum_ccdc_archive 'CCDC 847274' #TrackingRef 'Crox2NO3-bpy_5.cif' _audit_creation_date 2011-03-02T13:01:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C22 H16 Cr N4 O4, 0.5(C2 H2 O4), N O3, 4(H2 O)' _chemical_formula_sum 'C23 H25 Cr N5 O13' _chemical_formula_weight 631.47 #------------------ UNIT CELL INFORMATION -----------------------------------# _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 10.55650(10) _cell_length_b 17.1770(3) _cell_length_c 14.8525(2) _cell_angle_alpha 90 _cell_angle_beta 99.2720(10) _cell_angle_gamma 90 _cell_volume 2658.00(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8517 _cell_measurement_theta_min 2.5702 _cell_measurement_theta_max 75.9148 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 4.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64946 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4323 _diffrn_reflns_number 13456 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 76.1 _diffrn_reflns_theta_full 76.1 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measured_fraction_theta_full 0.984 _reflns_number_total 5467 _reflns_number_gt 4811 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.1120P)^2^+2.5972P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5467 _refine_ls_number_parameters 410 _refine_ls_number_restraints 12 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.193 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0 _refine_diff_density_max 0.744 _refine_diff_density_min -1.405 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_group _atom_site_disorder_assembly Cr1 Cr 0.14580(4) 0.22092(3) 0.03786(3) 0.01587(18) Uani 1 d . . . O1 O 0.2249(2) 0.13964(13) -0.02552(14) 0.0189(4) Uani 1 d . . . O2 O 0.0847(2) 0.13455(13) 0.10135(14) 0.0201(4) Uani 1 d . . . O3 O 0.2326(2) 0.01013(15) -0.03763(17) 0.0272(5) Uani 1 d . . . O4 O 0.0988(3) 0.00449(16) 0.11187(19) 0.0368(6) Uani 1 d . . . O5 O 0.6990(3) 0.0289(2) 0.3305(2) 0.0446(7) Uani 1 d . . . O6 O 0.7474(3) 0.1344(2) 0.4091(2) 0.0481(8) Uani 1 d . . . O7 O 0.6409(3) 0.04257(18) 0.46250(19) 0.0381(6) Uani 1 d . . . O8 O 0.5160(2) 0.09628(14) -0.03633(16) 0.0236(5) Uani 1 d . . . O9 O 0.5888(2) 0.14890(17) 0.59671(17) 0.0318(6) Uani 1 d D . . O10 O 0.4752(3) -0.04852(18) 0.27086(18) 0.0358(6) Uani 1 d D . . O11 O 0.1907(2) -0.09056(16) -0.18639(17) 0.0313(6) Uani 1 d D . . O12 O -0.3157(3) 0.20365(16) 0.07286(19) 0.0327(6) Uani 1 d D . . O13 O 0.5142(2) -0.01656(15) -0.11415(16) 0.0270(5) Uani 1 d . . . N1 N -0.0107(2) 0.21865(16) -0.06234(18) 0.0201(6) Uani 1 d . . . N2 N 0.1962(2) 0.30541(16) -0.04742(17) 0.0181(5) Uani 1 d . . . N3 N 0.0772(2) 0.30585(16) 0.11448(17) 0.0183(5) Uani 1 d . . . N4 N 0.2982(2) 0.23465(16) 0.14273(17) 0.0185(5) Uani 1 d . . . N5 N 0.6982(3) 0.06874(19) 0.4014(2) 0.0293(6) Uani 1 d . . . C1 C -0.1112(3) 0.1700(2) -0.0649(2) 0.0240(7) Uani 1 d . . . C2 C -0.2071(3) 0.1652(2) -0.1403(2) 0.0261(7) Uani 1 d . . . C3 C -0.1973(3) 0.2109(2) -0.2156(2) 0.0272(7) Uani 1 d . . . C4 C -0.0937(3) 0.2607(2) -0.2138(2) 0.0248(7) Uani 1 d . . . C5 C -0.0021(3) 0.2641(2) -0.1356(2) 0.0212(6) Uani 1 d . . . C6 C 0.1110(3) 0.3162(2) -0.1252(2) 0.0210(6) Uani 1 d . . . C7 C 0.1300(3) 0.3719(2) -0.1893(2) 0.0236(6) Uani 1 d . . . C8 C 0.2416(3) 0.4161(2) -0.1742(2) 0.0260(7) Uani 1 d . . . C9 C 0.3294(3) 0.4054(2) -0.0954(2) 0.0257(7) Uani 1 d . . . C10 C 0.3024(3) 0.3499(2) -0.0333(2) 0.0229(6) Uani 1 d . . . C11 C -0.0347(3) 0.3444(2) 0.0904(2) 0.0239(6) Uani 1 d . . . C12 C -0.0696(3) 0.4066(2) 0.1411(2) 0.0259(7) Uani 1 d . . . C13 C 0.0120(3) 0.4292(2) 0.2195(2) 0.0255(7) Uani 1 d . . . C14 C 0.1269(3) 0.3897(2) 0.2447(2) 0.0237(6) Uani 1 d . . . C15 C 0.1569(3) 0.3286(2) 0.1910(2) 0.0204(6) Uani 1 d . . . C16 C 0.2780(3) 0.28348(18) 0.2107(2) 0.0190(6) Uani 1 d . . . C17 C 0.3639(3) 0.2895(2) 0.2913(2) 0.0213(6) Uani 1 d . . . C18 C 0.4736(3) 0.2433(2) 0.3025(2) 0.0240(6) Uani 1 d . . . C19 C 0.4949(3) 0.1939(2) 0.2333(2) 0.0239(7) Uani 1 d . . . C20 C 0.4055(3) 0.1909(2) 0.1540(2) 0.0217(6) Uani 1 d . . . C21 C 0.1997(3) 0.0691(2) -0.0025(2) 0.0219(6) Uani 1 d . . . C22 C 0.1205(3) 0.0655(2) 0.0775(2) 0.0236(6) Uani 1 d . . . C23 C 0.5088(3) 0.0255(2) -0.0411(2) 0.0212(6) Uani 1 d . . . H1 H -0.1165 0.1388 -0.0145 0.029 Uiso 1 calc R . . H2 H -0.2765 0.1319 -0.1404 0.031 Uiso 1 calc R . . H3 H -0.2601 0.2083 -0.2673 0.033 Uiso 1 calc R . . H4 H -0.0856 0.2914 -0.2641 0.03 Uiso 1 calc R . . H7 H 0.0693 0.3795 -0.2414 0.028 Uiso 1 calc R . . H8 H 0.2573 0.4529 -0.217 0.031 Uiso 1 calc R . . H9 H 0.4045 0.4345 -0.0844 0.031 Uiso 1 calc R . . H9A H 0.621(7) 0.1999(19) 0.593(5) 0.09(3) Uiso 1 d D . . H9B H 0.622(7) 0.121(4) 0.550(4) 0.1 Uiso 1 d D . . H10 H 0.3602 0.3433 0.0204 0.027 Uiso 1 calc R . . H10A H 0.447(4) -0.082(3) 0.313(3) 0.047(14) Uiso 1 d D . . H10B H 0.554(3) -0.029(3) 0.301(3) 0.040(13) Uiso 1 d D . . H11 H -0.0901 0.3289 0.0383 0.029 Uiso 1 calc R . . H11A H 0.204(4) -0.0482(19) -0.148(2) 0.032(11) Uiso 1 d D . . H12 H -0.1466 0.4327 0.1227 0.031 Uiso 1 calc R . . H11B H 0.225(6) -0.074(3) -0.238(3) 0.08(2) Uiso 1 d D . . H12A H -0.375(4) 0.172(2) 0.035(3) 0.041(13) Uiso 1 d D . . H12B H -0.274(4) 0.168(2) 0.117(2) 0.032(11) Uiso 1 d D . . H13 H -0.01 0.4704 0.2546 0.031 Uiso 1 calc R . . H13A H 0.5235 0.0121 -0.1567 0.041 Uiso 1 calc R . . H14 H 0.1829 0.4039 0.297 0.028 Uiso 1 calc R . . H17 H 0.3486 0.3237 0.3369 0.026 Uiso 1 calc R . . H18 H 0.5323 0.2458 0.3563 0.029 Uiso 1 calc R . . H19 H 0.5681 0.163 0.2397 0.029 Uiso 1 calc R . . H20 H 0.42 0.1577 0.1072 0.026 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 0.0118(3) 0.0210(3) 0.0149(3) -0.00049(16) 0.00273(18) 0.00114(16) O1 0.0184(9) 0.0197(11) 0.0194(10) -0.0033(8) 0.0049(8) 0.0013(8) O2 0.0213(10) 0.0206(11) 0.0195(10) 0.0010(8) 0.0066(8) 0.0000(8) O3 0.0232(11) 0.0279(13) 0.0302(12) -0.0081(10) 0.0031(9) 0.0042(9) O4 0.0521(16) 0.0232(13) 0.0388(14) 0.0069(11) 0.0183(12) -0.0016(11) O5 0.0432(15) 0.0554(19) 0.0391(15) -0.0119(14) 0.0192(12) -0.0145(14) O6 0.0515(17) 0.0492(19) 0.0420(16) -0.0003(14) 0.0026(13) -0.0268(15) O7 0.0434(15) 0.0396(16) 0.0350(14) 0.0054(12) 0.0171(11) -0.0047(12) O8 0.0204(10) 0.0209(11) 0.0292(11) -0.0021(9) 0.0028(8) 0.0017(8) O9 0.0260(12) 0.0407(16) 0.0282(12) 0.0028(11) 0.0029(9) -0.0069(11) O10 0.0405(14) 0.0395(15) 0.0277(12) 0.0016(11) 0.0063(10) -0.0095(12) O11 0.0338(13) 0.0298(14) 0.0305(12) -0.0082(10) 0.0055(10) -0.0028(10) O12 0.0305(13) 0.0316(14) 0.0361(14) -0.0047(11) 0.0060(11) 0.0009(11) O13 0.0288(11) 0.0304(13) 0.0223(10) -0.0012(9) 0.0053(9) 0.0004(10) N1 0.0139(11) 0.0287(15) 0.0177(12) -0.0010(10) 0.0027(9) 0.0039(9) N2 0.0161(11) 0.0213(13) 0.0171(11) -0.0007(10) 0.0031(9) 0.0014(10) N3 0.0174(11) 0.0194(13) 0.0184(11) -0.0033(10) 0.0035(9) -0.0019(10) N4 0.0140(11) 0.0245(13) 0.0171(11) 0.0028(10) 0.0023(9) -0.0011(10) N5 0.0201(12) 0.0378(17) 0.0294(14) 0.0037(12) 0.0016(11) -0.0036(12) C1 0.0165(13) 0.0317(18) 0.0243(15) -0.0015(13) 0.0048(11) 0.0006(12) C2 0.0139(13) 0.0298(18) 0.0338(17) -0.0068(14) 0.0009(12) -0.0021(12) C3 0.0186(14) 0.0319(18) 0.0281(16) -0.0071(13) -0.0057(12) 0.0051(13) C4 0.0232(15) 0.0296(17) 0.0207(14) -0.0010(13) 0.0008(12) 0.0065(13) C5 0.0157(13) 0.0291(16) 0.0189(14) -0.0019(12) 0.0037(11) 0.0046(12) C6 0.0182(13) 0.0283(17) 0.0169(13) -0.0037(12) 0.0040(10) 0.0031(12) C7 0.0250(15) 0.0274(17) 0.0187(14) -0.0018(12) 0.0048(11) 0.0039(13) C8 0.0327(16) 0.0208(16) 0.0277(16) 0.0025(12) 0.0142(13) 0.0057(13) C9 0.0230(14) 0.0248(17) 0.0312(16) -0.0042(13) 0.0102(12) -0.0020(12) C10 0.0180(14) 0.0279(17) 0.0234(14) -0.0013(12) 0.0054(11) 0.0002(12) C11 0.0171(13) 0.0305(18) 0.0244(15) 0.0003(13) 0.0039(11) 0.0024(12) C12 0.0193(14) 0.0270(17) 0.0324(16) 0.0002(14) 0.0072(12) 0.0059(12) C13 0.0253(15) 0.0226(16) 0.0299(16) -0.0054(13) 0.0085(12) 0.0020(12) C14 0.0204(14) 0.0290(18) 0.0223(14) -0.0004(12) 0.0051(11) -0.0013(12) C15 0.0168(13) 0.0253(16) 0.0202(14) 0.0014(12) 0.0068(11) -0.0001(12) C16 0.0139(13) 0.0246(16) 0.0193(14) 0.0040(11) 0.0056(11) -0.0004(11) C17 0.0177(14) 0.0283(17) 0.0178(14) -0.0013(12) 0.0031(11) -0.0047(12) C18 0.0177(14) 0.0323(18) 0.0205(14) 0.0029(13) -0.0010(11) -0.0056(13) C19 0.0138(13) 0.0310(18) 0.0265(16) 0.0054(13) 0.0020(11) 0.0015(12) C20 0.0171(13) 0.0266(17) 0.0222(14) 0.0030(12) 0.0057(11) 0.0020(12) C21 0.0129(12) 0.0314(18) 0.0209(14) -0.0010(12) 0.0014(10) 0.0014(11) C22 0.0227(14) 0.0286(17) 0.0199(14) -0.0014(12) 0.0052(11) -0.0010(12) C23 0.0126(12) 0.0258(16) 0.0246(15) -0.0004(13) 0.0009(10) 0.0022(11) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 1.946(2) . ? Cr1 O2 1.924(2) . ? Cr1 N1 2.038(3) . ? Cr1 N2 2.052(3) . ? Cr1 N3 2.053(3) . ? Cr1 N4 2.065(3) . ? O1 C21 1.298(4) . ? O2 C22 1.312(4) . ? O3 C21 1.216(4) . ? O4 C22 1.204(4) . ? O8 C23 1.219(4) . ? O9 H9A 0.94(2) . ? O9 H9B 0.95(2) . ? O10 H10A 0.929(19) . ? O10 H10B 0.939(19) . ? O11 H11A 0.925(19) . ? O11 H11B 0.94(2) . ? O12 H12A 0.943(19) . ? O12 H12B 0.951(19) . ? O13 C23 1.312(4) . ? O13 H13A 0.82 . ? N1 C1 1.346(4) . ? N1 C5 1.353(4) . ? N2 C6 1.357(4) . ? N2 C10 1.346(4) . ? N3 C11 1.352(4) . ? N3 C15 1.357(4) . ? N4 C16 1.355(4) . ? N4 C20 1.347(4) . ? N5 O6 1.240(4) . ? N5 O5 1.257(4) . ? N5 O7 1.252(4) . ? C1 C2 1.386(5) . ? C1 H1 0.93 . ? C3 H3 0.93 . ? C2 H2 0.93 . ? C3 C2 1.384(5) . ? C3 C4 1.386(5) . ? C4 H4 0.93 . ? C5 C4 1.387(4) . ? C5 C6 1.480(4) . ? C6 C7 1.387(5) . ? C7 C8 1.389(5) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C8 1.383(5) . ? C9 C10 1.387(5) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? C11 C12 1.390(5) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C12 1.388(5) . ? C13 C14 1.388(5) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C14 1.386(5) . ? C16 C15 1.483(4) . ? C16 C17 1.384(4) . ? C17 C18 1.392(5) . ? C17 H17 0.93 . ? C18 C19 1.380(5) . ? C18 H18 0.93 . ? C19 H19 0.93 . ? C21 C22 1.560(4) . ? C23 C23 1.540(6) 3_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 O1 Cr1 N1 89.64(10) . . ? O1 Cr1 N2 91.99(10) . . ? O1 Cr1 N3 174.52(10) . . ? O1 Cr1 N4 95.96(10) . . ? O1 C21 C22 113.3(3) . . ? O2 Cr1 O1 83.56(10) . . ? O2 Cr1 N1 92.68(10) . . ? O2 Cr1 N2 171.31(10) . . ? O2 Cr1 N3 95.75(10) . . ? O2 Cr1 N4 90.02(10) . . ? O2 C22 C21 112.5(3) . . ? O3 C21 O1 125.5(3) . . ? O3 C21 C22 121.2(3) . . ? O4 C22 O2 126.1(3) . . ? O4 C22 C21 121.4(3) . . ? O6 N5 O5 120.8(3) . . ? O6 N5 O7 120.3(3) . . ? O7 N5 O5 118.7(3) . . ? O8 C23 O13 126.0(3) . . ? O8 C23 C23 122.4(4) . 3_655 ? O13 C23 C23 111.6(4) . 3_655 ? N1 Cr1 N2 79.80(11) . . ? N1 Cr1 N3 95.83(10) . . ? N1 Cr1 N4 174.02(11) . . ? N1 C1 C2 122.0(3) . . ? N1 C1 H1 119 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 115.0(3) . . ? N2 Cr1 N3 89.38(11) . . ? N2 Cr1 N4 97.88(10) . . ? N2 C6 C7 122.0(3) . . ? N2 C6 C5 114.7(3) . . ? N2 C10 C9 122.8(3) . . ? N2 C10 H10 118.6 . . ? N3 Cr1 N4 78.59(11) . . ? N3 C11 C12 122.0(3) . . ? N3 C11 H11 119 . . ? N3 C15 C14 122.1(3) . . ? N3 C15 C16 114.4(3) . . ? N4 C16 C17 122.0(3) . . ? N4 C16 C15 114.2(3) . . ? N4 C20 C19 121.9(3) . . ? N4 C20 H20 119 . . ? C1 N1 Cr1 125.1(2) . . ? C1 N1 C5 119.3(3) . . ? C1 C2 H2 120.7 . . ? C2 C1 H1 119 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2 120.7 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C4 C3 H3 120.2 . . ? C4 C5 C6 123.6(3) . . ? C5 N1 Cr1 115.1(2) . . ? C5 C4 H4 120.5 . . ? C6 N2 Cr1 114.8(2) . . ? C6 C7 C8 118.6(3) . . ? C6 C7 H7 120.7 . . ? C7 C6 C5 123.3(3) . . ? C7 C8 H8 120 . . ? C8 C7 H7 120.7 . . ? C8 C9 C10 118.2(3) . . ? C8 C9 H9 120.9 . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120 . . ? C9 C10 H10 118.6 . . ? C10 N2 Cr1 126.7(2) . . ? C10 N2 C6 118.4(3) . . ? C10 C9 H9 120.9 . . ? C11 N3 Cr1 125.0(2) . . ? C11 N3 C15 118.6(3) . . ? C11 C12 H12 120.4 . . ? C12 C11 H11 119 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H13 120.4 . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12 120.4 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 123.5(3) . . ? C14 C13 H13 120.4 . . ? C15 N3 Cr1 116.2(2) . . ? C15 C14 C13 119.1(3) . . ? C15 C14 H14 120.5 . . ? C16 N4 Cr1 115.8(2) . . ? C16 C17 C18 118.5(3) . . ? C16 C17 H17 120.7 . . ? C17 C16 C15 123.7(3) . . ? C17 C18 H18 120.2 . . ? C18 C17 H17 120.7 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2 . . ? C19 C20 H20 119 . . ? C20 N4 Cr1 124.6(2) . . ? C20 N4 C16 118.9(3) . . ? C20 C19 H19 120.5 . . ? C21 O1 Cr1 114.84(19) . . ? C22 O2 Cr1 115.52(19) . . ? C23 O13 H13A 109.5 . . ? H9B O9 H9A 104(4) . . ? H10B O10 H10A 105(3) . . ? H11A O11 H11B 104(3) . . ? H12B O12 H12A 103(3) . . ? 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 Cr1 O1 C21 O3 175.2(2) . . . . ? Cr1 O1 C21 C22 -5.0(3) . . . . ? Cr1 O2 C22 O4 175.8(3) . . . . ? Cr1 O2 C22 C21 -3.4(3) . . . . ? Cr1 N1 C1 C2 -172.1(2) . . . . ? Cr1 N1 C5 C4 171.6(2) . . . . ? Cr1 N1 C5 C6 -8.3(3) . . . . ? Cr1 N2 C6 C5 -1.1(3) . . . . ? Cr1 N2 C6 C7 179.0(2) . . . . ? Cr1 N2 C10 C9 179.3(2) . . . . ? Cr1 N3 C11 C12 -173.5(2) . . . . ? Cr1 N3 C15 C14 174.6(2) . . . . ? Cr1 N3 C15 C16 -4.5(3) . . . . ? Cr1 N4 C16 C15 -9.3(3) . . . . ? Cr1 N4 C16 C17 170.3(2) . . . . ? Cr1 N4 C20 C19 -169.0(2) . . . . ? O1 Cr1 O2 C22 0.7(2) . . . . ? O1 Cr1 N1 C1 86.0(3) . . . . ? O1 Cr1 N1 C5 -86.1(2) . . . . ? O1 Cr1 N2 C6 86.7(2) . . . . ? O1 Cr1 N2 C10 -93.6(3) . . . . ? O1 Cr1 N3 C11 -18E1(6) . . . . ? O1 Cr1 N3 C15 6.1(12) . . . . ? O1 Cr1 N4 C16 -174.0(2) . . . . ? O1 Cr1 N4 C20 -4.0(3) . . . . ? O1 C21 C22 O2 5.6(4) . . . . ? O1 C21 C22 O4 -173.6(3) . . . . ? O2 Cr1 O1 C21 2.73(19) . . . . ? O2 Cr1 N1 C1 2.5(3) . . . . ? O2 Cr1 N1 C5 -169.6(2) . . . . ? O2 Cr1 N2 C6 27.8(7) . . . . ? O2 Cr1 N2 C10 -152.6(6) . . . . ? O2 Cr1 N4 C16 -90.4(2) . . . . ? O2 Cr1 N4 C20 79.5(2) . . . . ? O2 Cr1 N3 C11 -97.2(3) . . . . ? O2 Cr1 N3 C15 88.6(2) . . . . ? O3 C21 C22 O2 -174.6(3) . . . . ? O3 C21 C22 O4 6.2(5) . . . . ? N1 Cr1 O1 C21 -90.0(2) . . . . ? N1 Cr1 O2 C22 90.0(2) . . . . ? N1 Cr1 N2 C6 -2.5(2) . . . . ? N1 Cr1 N2 C10 177.1(3) . . . . ? N1 Cr1 N3 C11 -3.9(3) . . . . ? N1 Cr1 N3 C15 -178.1(2) . . . . ? N1 Cr1 N4 C16 26.5(11) . . . . ? N1 Cr1 N4 C20 -163.5(9) . . . . ? N1 C5 C4 C3 1.4(5) . . . . ? N1 C1 C2 C3 1.1(5) . . . . ? N1 C5 C6 N2 6.2(4) . . . . ? N1 C5 C6 C7 -173.9(3) . . . . ? N2 Cr1 O1 C21 -169.8(2) . . . . ? N2 Cr1 O2 C22 60.2(7) . . . . ? N2 Cr1 N1 C1 178.1(3) . . . . ? N2 Cr1 N1 C5 6.0(2) . . . . ? N2 Cr1 N3 C11 75.7(3) . . . . ? N2 Cr1 N3 C15 -98.4(2) . . . . ? N2 Cr1 N4 C16 93.2(2) . . . . ? N2 Cr1 N4 C20 -96.8(3) . . . . ? N2 C6 C7 C8 1.9(5) . . . . ? N3 Cr1 O1 C21 85.8(11) . . . . ? N3 Cr1 O2 C22 -173.8(2) . . . . ? N3 Cr1 N1 C1 -93.6(3) . . . . ? N3 Cr1 N1 C5 94.3(2) . . . . ? N3 Cr1 N2 C6 -98.6(2) . . . . ? N3 Cr1 N2 C10 81.1(3) . . . . ? N3 Cr1 N4 C16 5.4(2) . . . . ? N3 Cr1 N4 C20 175.4(3) . . . . ? N3 C11 C12 C13 -0.9(5) . . . . ? N3 C15 C14 C13 -0.3(5) . . . . ? N4 Cr1 O1 C21 92.1(2) . . . . ? N4 Cr1 O2 C22 -95.3(2) . . . . ? N4 Cr1 N1 C1 -114.4(10) . . . . ? N4 Cr1 N1 C5 73.6(10) . . . . ? N4 Cr1 N2 C6 -177.0(2) . . . . ? N4 Cr1 N2 C10 2.7(3) . . . . ? N4 Cr1 N3 C11 173.9(3) . . . . ? N4 Cr1 N3 C15 -0.2(2) . . . . ? N4 C16 C15 N3 9.1(4) . . . . ? N4 C16 C15 C14 -170.1(3) . . . . ? N4 C16 C17 C18 -0.5(5) . . . . ? N4 C20 C19 C18 -0.3(5) . . . . ? C1 N1 C5 C4 -1.0(5) . . . . ? C1 N1 C5 C6 179.1(3) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C4 C3 C2 C1 -0.6(5) . . . . ? C4 C5 C6 N2 -173.7(3) . . . . ? C4 C5 C6 C7 6.2(5) . . . . ? C5 N1 C1 C2 -0.3(5) . . . . ? C5 C6 C7 C8 -178.0(3) . . . . ? C6 N2 C10 C9 -1.0(5) . . . . ? C6 C5 C4 C3 -178.7(3) . . . . ? C6 C7 C8 C9 -1.6(5) . . . . ? C8 C9 C10 N2 1.4(5) . . . . ? C10 N2 C6 C5 179.3(3) . . . . ? C10 N2 C6 C7 -0.7(4) . . . . ? C10 C9 C8 C7 0.0(5) . . . . ? C11 N3 C15 C14 0.1(5) . . . . ? C11 N3 C15 C16 -179.0(3) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C14 C13 C12 C11 0.6(5) . . . . ? C15 N3 C11 C12 0.5(5) . . . . ? C15 C16 C17 C18 179.1(3) . . . . ? C16 N4 C20 C19 0.6(5) . . . . ? C16 C15 C14 C13 178.7(3) . . . . ? C16 C17 C18 C19 0.8(5) . . . . ? C17 C16 C15 N3 -170.6(3) . . . . ? C17 C16 C15 C14 10.3(5) . . . . ? C17 C18 C19 C20 -0.5(5) . . . . ? C20 N4 C16 C17 -0.2(4) . . . . ? C20 N4 C16 C15 -179.9(3) . . . . ? # Attachment 'Crox2NO3_2.cif' data_Crox2NO3_2 _database_code_depnum_ccdc_archive 'CCDC 847275' #TrackingRef 'Crox2NO3_2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; bis(1,10-phenanthroline-N,N')(oxalato-O,O')chromium(III) nitrate oxalic acid monohydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H16 Cr N4 O4, C2 H2 O4, N O3, H2 O' _chemical_formula_structural 'Cr (C12 H8 N2)2(C2 O4)2 N O3 H2 C2 O4 H2 O' _chemical_formula_sum 'C28 H20 Cr N5 O12' _chemical_formula_iupac ? _chemical_formula_weight 670.49 _chemical_compound_source 'synthesized by the authors, see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0180 0.0090 '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 -0.1630 2.4440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0490 0.0320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C c' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _cell_length_a 15.856(5) _cell_length_b 14.353(5) _cell_length_c 13.141(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.517(5) _cell_angle_gamma 90.00 _cell_volume 2867.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5239 _cell_measurement_theta_min 3.5052 _cell_measurement_theta_max 76.0448 _cell_special_details ; ? ; _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 3.954 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.54785 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ;? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4 # number of measured reflections (redundant set) _diffrn_reflns_number 6664 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.5052 _diffrn_reflns_theta_max 76.0448 _diffrn_reflns_theta_full 76.23 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_reduction_process ;? ; # number of unique reflections _reflns_number_total 3760 # number of observed reflections (> n sig(I)) _reflns_number_gt 3557 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SIR92 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3 (Farrugia, 1997), MERCURY (Bruno et al., 2002)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0702P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.522(8) _refine_ls_number_reflns 3760 _refine_ls_number_parameters 424 _refine_ls_number_restraints 5 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.386 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.042 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cr1 Cr Uani 0.50097(6) 0.28941(2) 0.50075(7) 1.000 0.0384(1) . . O1 O Uani 0.41692(19) 0.3902(2) 0.4885(2) 1.000 0.0473(9) . . O2 O Uani 0.58440(19) 0.3900(2) 0.5138(3) 1.000 0.0483(10) . . O3 O Uani 0.4081(2) 0.5444(2) 0.4686(3) 1.000 0.0659(13) . . O4 O Uani 0.5943(2) 0.5435(2) 0.5319(3) 1.000 0.0675(13) . . O5 O Uani -0.0140(4) 0.4871(3) 0.1114(5) 1.000 0.131(2) . . O6 O Uani 0.0771(3) 0.5892(3) 0.1040(3) 1.000 0.0978(14) . . O7 O Uani 0.0557(3) 0.5550(3) 0.2523(3) 1.000 0.0999(16) . . O8 O Uani 0.3578(3) 0.1574(4) 0.7725(4) 1.000 0.1094(17) . . O9 O Uani 0.2702(5) 0.2961(6) 0.6519(7) 1.000 0.193(4) . . O10 O Uani 0.2644(5) 0.1607(5) 0.8642(6) 1.000 0.165(3) . . O11 O Uani 0.1746(4) 0.2911(4) 0.7363(5) 1.000 0.134(3) . . O12 O Uani 0.4585(3) 0.0324(3) 0.8775(4) 1.000 0.0850(12) . . N1 N Uani 0.5245(3) 0.2793(2) 0.6628(3) 1.000 0.0480(14) . . N2 N Uani 0.6009(3) 0.1928(3) 0.5349(3) 1.000 0.0416(11) . . N3 N Uani 0.3986(3) 0.1934(3) 0.4646(3) 1.000 0.0438(11) . . N4 N Uani 0.4772(3) 0.2806(2) 0.3383(3) 1.000 0.0446(11) . . N5 N Uani 0.0385(3) 0.5433(3) 0.1570(4) 1.000 0.0732(13) . . C1 C Uani 0.4844(4) 0.3257(4) 0.7240(4) 1.000 0.0589(17) . . C2 C Uani 0.5128(5) 0.3160(4) 0.8349(5) 1.000 0.0724(19) . . C3 C Uani 0.5816(4) 0.2583(4) 0.8823(4) 1.000 0.069(2) . . C4 C Uani 0.6250(4) 0.2092(3) 0.8204(5) 1.000 0.0622(19) . . C5 C Uani 0.6969(4) 0.1491(4) 0.8609(4) 1.000 0.0751(19) . . C6 C Uani 0.7360(4) 0.1049(4) 0.7949(5) 1.000 0.0700(19) . . C7 C Uani 0.7062(3) 0.1160(3) 0.6829(4) 1.000 0.0593(16) . . C8 C Uani 0.7446(4) 0.0750(4) 0.6099(5) 1.000 0.0690(19) . . C9 C Uani 0.7127(4) 0.0932(4) 0.5052(5) 1.000 0.072(2) . . C10 C Uani 0.6408(3) 0.1529(3) 0.4681(4) 1.000 0.0537(14) . . C11 C Uani 0.6339(3) 0.1749(3) 0.6401(3) 1.000 0.0435(12) . . C12 C Uani 0.5930(3) 0.2220(3) 0.7081(3) 1.000 0.0437(11) . . C13 C Uani 0.3599(3) 0.1541(3) 0.5291(4) 1.000 0.0547(16) . . C14 C Uani 0.2862(3) 0.0958(4) 0.4945(5) 1.000 0.0656(18) . . C15 C Uani 0.2544(3) 0.0780(3) 0.3874(5) 1.000 0.0693(16) . . C16 C Uani 0.2943(3) 0.1196(3) 0.3155(4) 1.000 0.0562(14) . . C17 C Uani 0.2654(4) 0.1065(4) 0.2038(5) 1.000 0.0752(19) . . C18 C Uani 0.3033(4) 0.1495(4) 0.1399(5) 1.000 0.076(2) . . C19 C Uani 0.3789(4) 0.2115(3) 0.1812(4) 1.000 0.0586(19) . . C20 C Uani 0.4224(5) 0.2606(5) 0.1185(5) 1.000 0.078(2) . . C21 C Uani 0.4911(5) 0.3157(5) 0.1654(5) 1.000 0.075(2) . . C22 C Uani 0.5173(4) 0.3241(4) 0.2760(4) 1.000 0.0590(17) . . C23 C Uani 0.4086(3) 0.2241(3) 0.2893(4) 1.000 0.0483(14) . . C24 C Uani 0.3665(3) 0.1781(3) 0.3582(3) 1.000 0.0451(12) . . C25 C Uani 0.4496(3) 0.4725(3) 0.4874(3) 1.000 0.0468(12) . . C26 C Uani 0.5518(3) 0.4731(3) 0.5132(3) 1.000 0.0465(12) . . C27 C Uani 0.2904(4) 0.1887(4) 0.7968(4) 1.000 0.0720(16) . . C28 C Uani 0.2435(3) 0.2665(4) 0.7207(4) 1.000 0.0728(16) . . H1 H Uiso 0.43736 0.36472 0.69291 1.000 0.0709 . . H2 H Uiso 0.48458 0.34903 0.87656 1.000 0.0865 . . H3 H Uiso 0.59937 0.25179 0.95571 1.000 0.0829 . . H5 H Uiso 0.71784 0.13950 0.93371 1.000 0.0896 . . H6 H Uiso 0.78385 0.06611 0.82397 1.000 0.0840 . . H8 H Uiso 0.79233 0.03506 0.63376 1.000 0.0825 . . H8A H Uiso 0.38031 0.11534 0.81356 1.000 0.1640 . . H9 H Uiso 0.73873 0.06592 0.45741 1.000 0.0866 . . H10 H Uiso 0.62013 0.16532 0.39576 1.000 0.0646 . . H11A H Uiso 0.15283 0.33332 0.69515 1.000 0.2012 . . H12A H Uiso 0.477(5) 0.009(6) 0.821(5) 1.000 0.16(4) . . H12B H Uiso 0.502(3) 0.073(3) 0.916(4) 1.000 0.098(19) . . H13 H Uiso 0.38236 0.16535 0.60146 1.000 0.0661 . . H14 H Uiso 0.25957 0.07003 0.54251 1.000 0.0784 . . H15 H Uiso 0.20653 0.03836 0.36243 1.000 0.0833 . . H17 H Uiso 0.21849 0.06647 0.17505 1.000 0.0902 . . H18 H Uiso 0.28175 0.14036 0.06701 1.000 0.0910 . . H20 H Uiso 0.40379 0.25495 0.04495 1.000 0.0942 . . H21 H Uiso 0.52088 0.34789 0.12468 1.000 0.0902 . . H22 H Uiso 0.56510 0.36211 0.30745 1.000 0.0709 . . 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 0.0315(2) 0.0470(2) 0.0355(2) 0.0002(3) 0.0073(1) 0.0004(3) O1 0.0330(15) 0.0516(16) 0.0548(17) -0.0011(13) 0.0087(12) -0.0006(14) O2 0.0319(15) 0.0526(17) 0.0585(18) -0.0042(13) 0.0097(12) -0.0022(14) O3 0.0475(19) 0.0560(17) 0.092(3) 0.0036(17) 0.0162(18) 0.0088(16) O4 0.0493(19) 0.0554(17) 0.099(3) -0.0036(17) 0.0230(19) -0.0105(16) O5 0.112(3) 0.113(3) 0.147(5) -0.045(3) 0.001(3) -0.040(3) O6 0.111(3) 0.106(2) 0.084(2) -0.0160(19) 0.040(2) -0.015(2) O7 0.108(3) 0.117(3) 0.069(2) -0.0067(19) 0.0162(19) -0.031(2) O8 0.099(3) 0.145(3) 0.103(3) 0.059(3) 0.059(2) 0.052(3) O9 0.174(6) 0.246(8) 0.212(8) 0.151(7) 0.143(6) 0.120(6) O10 0.192(6) 0.198(6) 0.153(5) 0.102(5) 0.125(5) 0.094(5) O11 0.107(4) 0.156(4) 0.165(5) 0.074(4) 0.081(4) 0.061(3) O12 0.084(2) 0.092(2) 0.076(2) 0.0038(19) 0.0180(19) 0.008(2) N1 0.051(3) 0.055(2) 0.039(2) -0.0034(14) 0.0146(19) -0.0023(16) N2 0.038(2) 0.0462(16) 0.0394(19) -0.0030(14) 0.0093(15) 0.0019(14) N3 0.035(2) 0.0482(17) 0.047(2) 0.0002(15) 0.0097(16) -0.0004(15) N4 0.039(2) 0.0547(19) 0.038(2) 0.0039(13) 0.0074(17) 0.0031(15) N5 0.063(2) 0.0660(18) 0.080(3) -0.0196(18) 0.0033(19) 0.0046(16) C1 0.061(3) 0.071(3) 0.048(3) -0.010(2) 0.021(2) -0.001(3) C2 0.088(4) 0.083(3) 0.054(3) -0.015(3) 0.033(3) -0.010(3) C3 0.082(4) 0.090(4) 0.033(2) -0.007(2) 0.012(2) -0.022(3) C4 0.067(4) 0.064(3) 0.049(3) -0.0039(18) 0.006(3) -0.011(2) C5 0.083(4) 0.071(3) 0.048(3) 0.016(2) -0.019(3) -0.009(3) C6 0.054(3) 0.064(3) 0.074(4) 0.016(3) -0.011(2) 0.005(2) C7 0.043(3) 0.058(2) 0.066(3) 0.007(2) -0.002(2) -0.005(2) C8 0.047(3) 0.065(3) 0.092(4) -0.006(3) 0.015(3) 0.013(2) C9 0.064(3) 0.065(3) 0.096(5) -0.010(3) 0.037(3) 0.009(3) C10 0.045(2) 0.064(3) 0.054(2) -0.0096(19) 0.0172(19) 0.007(2) C11 0.039(2) 0.043(2) 0.043(2) 0.0003(16) 0.0030(16) -0.0013(17) C12 0.038(2) 0.056(2) 0.0293(18) 0.0041(14) -0.0029(16) -0.0086(17) C13 0.049(3) 0.058(2) 0.061(3) 0.0067(19) 0.022(2) 0.002(2) C14 0.044(2) 0.069(3) 0.086(4) 0.013(3) 0.022(2) -0.008(2) C15 0.040(2) 0.056(2) 0.106(4) -0.007(2) 0.011(3) -0.009(2) C16 0.037(2) 0.048(2) 0.075(3) -0.0044(19) 0.002(2) 0.0002(18) C17 0.059(3) 0.075(3) 0.071(4) -0.014(3) -0.015(3) 0.004(3) C18 0.068(4) 0.088(4) 0.055(3) -0.011(3) -0.009(3) 0.013(3) C19 0.063(4) 0.072(3) 0.033(3) -0.0035(16) 0.001(2) 0.022(2) C20 0.093(5) 0.094(4) 0.043(3) 0.011(3) 0.011(3) 0.019(4) C21 0.092(5) 0.088(4) 0.053(3) 0.026(3) 0.032(3) 0.015(4) C22 0.060(3) 0.068(3) 0.055(3) 0.011(2) 0.026(2) 0.002(2) C23 0.050(3) 0.049(2) 0.045(2) 0.0074(16) 0.012(2) 0.0088(18) C24 0.034(2) 0.048(2) 0.048(2) -0.0016(17) 0.0033(16) 0.0077(18) C25 0.034(2) 0.052(2) 0.053(2) -0.0085(18) 0.0099(17) 0.0001(19) C26 0.042(2) 0.055(2) 0.043(2) -0.0066(17) 0.0131(17) -0.002(2) C27 0.072(3) 0.092(3) 0.062(2) 0.010(2) 0.035(2) -0.001(2) C28 0.067(2) 0.098(3) 0.063(3) 0.009(2) 0.034(2) 0.010(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.942(3) . . yes Cr1 O2 1.933(3) . . yes Cr1 N1 2.060(4) . . yes Cr1 N2 2.057(5) . . yes Cr1 N3 2.079(5) . . yes Cr1 N4 2.063(4) . . yes O1 C25 1.292(5) . . yes O2 C26 1.299(5) . . yes O3 C25 1.211(5) . . yes O4 C26 1.201(5) . . yes O5 N5 1.191(7) . . yes O6 N5 1.239(7) . . yes O7 N5 1.215(6) . . yes O8 C27 1.281(8) . . yes O8 H8A 0.8200 . . no O9 C28 1.181(10) . . yes O10 C27 1.151(10) . . yes O11 C28 1.220(8) . . yes O11 H11A 0.8200 . . no O12 H12B 0.93(5) . . no O12 H12A 0.94(7) . . no N1 C12 1.358(6) . . yes N1 C1 1.336(7) . . yes N2 C10 1.347(7) . . yes N2 C11 1.356(5) . . yes N3 C24 1.363(5) . . yes N3 C13 1.307(7) . . yes N4 C23 1.363(6) . . yes N4 C22 1.327(7) . . yes C1 C2 1.405(8) . . no C2 C3 1.370(9) . . no C3 C4 1.397(8) . . no C4 C12 1.429(7) . . no C4 C5 1.408(8) . . no C5 C6 1.358(9) . . no C6 C7 1.421(8) . . no C7 C11 1.407(7) . . no C7 C8 1.403(8) . . no C8 C9 1.350(9) . . no C9 C10 1.398(8) . . no C11 C12 1.416(6) . . no C13 C14 1.404(7) . . no C14 C15 1.377(9) . . no C15 C16 1.410(7) . . no C16 C17 1.420(8) . . no C16 C24 1.402(7) . . no C17 C18 1.317(9) . . no C18 C19 1.468(8) . . no C19 C23 1.376(7) . . no C19 C20 1.405(9) . . no C20 C21 1.345(11) . . no C21 C22 1.399(8) . . no C23 C24 1.430(7) . . no C25 C26 1.558(7) . . no C1 H1 0.9300 . . no C2 H2 0.9300 . . no C3 H3 0.9300 . . no C5 H5 0.9300 . . no C6 H6 0.9300 . . no C8 H8 0.9300 . . no C9 H9 0.9300 . . no C10 H10 0.9300 . . no C13 H13 0.9300 . . no C14 H14 0.9300 . . no C15 H15 0.9300 . . no C17 H17 0.9300 . . no C18 H18 0.9300 . . no C20 H20 0.9300 . . no C21 H21 0.9300 . . no C22 H22 0.9300 . . no C27 C28 1.542(8) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr1 O1 C25 114.5(3) . . . yes Cr1 O2 C26 115.1(3) . . . yes Cr1 N1 C1 127.6(3) . . . yes Cr1 N1 C12 112.5(3) . . . yes Cr1 N2 C10 128.3(3) . . . yes Cr1 N2 C11 113.6(3) . . . yes Cr1 N3 C13 128.2(3) . . . yes Cr1 N3 C24 112.4(3) . . . yes Cr1 N4 C23 114.3(3) . . . yes Cr1 N4 C22 129.1(3) . . . yes O1 Cr1 O2 83.52(13) . . . yes O1 Cr1 N1 93.24(14) . . . yes O1 Cr1 N2 171.13(14) . . . yes O1 Cr1 N3 90.12(16) . . . yes O1 Cr1 N4 92.33(14) . . . yes O1 C25 O3 125.8(4) . . . yes O1 C25 C26 113.5(4) . . . yes O2 Cr1 N1 92.45(16) . . . yes O2 Cr1 N2 91.08(16) . . . yes O2 Cr1 N3 170.36(16) . . . yes O2 Cr1 N4 93.25(16) . . . yes O2 C26 C25 112.6(4) . . . yes O2 C26 O4 124.9(4) . . . yes O3 C25 C26 120.7(4) . . . yes O4 C26 C25 122.5(4) . . . yes O5 N5 O7 122.1(5) . . . yes O5 N5 O6 117.6(5) . . . yes O6 N5 O7 120.2(5) . . . yes O8 C27 C28 112.0(5) . . . yes O8 C27 O10 125.2(7) . . . yes O9 C28 O11 123.9(7) . . . yes O9 C28 C27 123.1(6) . . . yes O10 C27 C28 122.7(6) . . . yes O11 C28 C27 113.0(5) . . . yes N1 Cr1 N2 79.93(16) . . . yes N1 Cr1 N3 95.15(16) . . . yes N1 Cr1 N4 172.45(11) . . . yes N1 C1 C2 120.5(6) . . . yes N1 C12 C4 122.4(4) . . . yes N1 C12 C11 117.7(4) . . . yes N1 C1 H1 120.00 . . . no N2 Cr1 N3 96.08(18) . . . yes N2 Cr1 N4 95.00(16) . . . yes N2 C10 C9 121.4(5) . . . yes N2 C11 C7 123.8(4) . . . yes N2 C11 C12 116.1(4) . . . yes N2 C10 H10 119.00 . . . no N3 Cr1 N4 79.74(16) . . . yes N3 C13 C14 123.3(5) . . . yes N3 C24 C16 122.1(4) . . . yes N3 C24 C23 118.0(4) . . . yes N3 C13 H13 118.00 . . . no N4 C22 C21 123.2(6) . . . yes N4 C23 C19 124.0(5) . . . yes N4 C23 C24 115.4(4) . . . yes N4 C22 H22 118.00 . . . no C1 N1 C12 119.8(4) . . . yes C1 C2 C3 120.7(6) . . . no C2 C3 C4 120.1(5) . . . no C3 C4 C5 124.7(5) . . . no C3 C4 C12 116.6(5) . . . no C4 C5 C6 120.8(5) . . . no C4 C12 C11 119.9(4) . . . no C5 C4 C12 118.7(5) . . . no C5 C6 C7 122.1(5) . . . no C6 C7 C8 125.4(5) . . . no C6 C7 C11 118.3(5) . . . no C7 C8 C9 120.4(6) . . . no C7 C11 C12 120.1(4) . . . no C8 C7 C11 116.2(5) . . . no C8 C9 C10 120.4(6) . . . no C10 N2 C11 117.9(4) . . . yes C13 N3 C24 119.2(4) . . . yes C13 C14 C15 118.1(5) . . . no C14 C15 C16 120.2(5) . . . no C15 C16 C17 124.2(5) . . . no C15 C16 C24 117.1(4) . . . no C16 C17 C18 121.7(6) . . . no C16 C24 C23 119.9(4) . . . no C17 C16 C24 118.7(5) . . . no C17 C18 C19 121.4(6) . . . no C18 C19 C23 117.7(5) . . . no C18 C19 C20 125.0(5) . . . no C19 C20 C21 119.7(6) . . . no C19 C23 C24 120.6(4) . . . no C20 C19 C23 117.3(5) . . . no C20 C21 C22 119.3(7) . . . no C22 N4 C23 116.5(4) . . . yes C1 C2 H2 120.00 . . . no C2 C1 H1 120.00 . . . no C2 C3 H3 120.00 . . . no C3 C2 H2 120.00 . . . no C4 C3 H3 120.00 . . . no C4 C5 H5 120.00 . . . no C5 C6 H6 119.00 . . . no C6 C5 H5 120.00 . . . no C7 C6 H6 119.00 . . . no C7 C8 H8 120.00 . . . no C8 C9 H9 120.00 . . . no C9 C8 H8 120.00 . . . no C9 C10 H10 119.00 . . . no C10 C9 H9 120.00 . . . no C13 C14 H14 121.00 . . . no C14 C13 H13 118.00 . . . no C14 C15 H15 120.00 . . . no C15 C14 H14 121.00 . . . no C16 C15 H15 120.00 . . . no C16 C17 H17 119.00 . . . no C17 C18 H18 119.00 . . . no C18 C17 H17 119.00 . . . no C19 C18 H18 119.00 . . . no C19 C20 H20 120.00 . . . no C20 C21 H21 120.00 . . . no C21 C22 H22 118.00 . . . no C21 C20 H20 120.00 . . . no C22 C21 H21 120.00 . . . no C27 O8 H8A 109.00 . . . no C28 O11 H11A 109.00 . . . no H12A O12 H12B 108(6) . . . no 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 C25 4.1(3) . . . . no N1 Cr1 O1 C25 96.1(3) . . . . no N3 Cr1 O1 C25 -168.7(3) . . . . no N4 Cr1 O1 C25 -89.0(3) . . . . no N3 Cr1 N1 C12 98.7(3) . . . . no O1 Cr1 N1 C1 4.8(5) . . . . no O1 Cr1 O2 C26 2.5(3) . . . . no N1 Cr1 O2 C26 -90.5(3) . . . . no N2 Cr1 O2 C26 -170.5(3) . . . . no N4 Cr1 O2 C26 94.5(3) . . . . no N1 Cr1 N3 C13 7.9(5) . . . . no N2 Cr1 N3 C13 88.3(5) . . . . no O2 Cr1 N2 C10 -84.7(4) . . . . no O2 Cr1 N1 C1 88.5(5) . . . . no N2 Cr1 N1 C1 179.2(5) . . . . no N3 Cr1 N1 C1 -85.6(5) . . . . no O1 Cr1 N1 C12 -170.9(3) . . . . no O2 Cr1 N1 C12 -87.2(3) . . . . no N2 Cr1 N1 C12 3.5(3) . . . . no N4 Cr1 N2 C11 -177.4(3) . . . . no N1 Cr1 N2 C10 -177.0(5) . . . . no N3 Cr1 N2 C10 88.9(4) . . . . no N4 Cr1 N2 C10 8.7(5) . . . . no O1 Cr1 N4 C22 90.8(5) . . . . no O2 Cr1 N4 C22 7.1(5) . . . . no N2 Cr1 N4 C22 -84.2(5) . . . . no O1 Cr1 N3 C13 -85.4(4) . . . . no O2 Cr1 N2 C11 89.2(4) . . . . no N3 Cr1 N4 C22 -179.5(5) . . . . no N4 Cr1 N3 C13 -177.7(5) . . . . no N4 Cr1 N3 C24 -3.2(3) . . . . no N1 Cr1 N2 C11 -3.1(3) . . . . no N3 Cr1 N2 C11 -97.2(4) . . . . no N2 Cr1 N3 C24 -97.2(3) . . . . no O1 Cr1 N3 C24 89.2(3) . . . . no N1 Cr1 N3 C24 -177.6(3) . . . . no O2 Cr1 N4 C23 -170.5(3) . . . . no N3 Cr1 N4 C23 2.8(3) . . . . no O1 Cr1 N4 C23 -86.9(3) . . . . no N2 Cr1 N4 C23 98.1(3) . . . . no Cr1 O1 C25 O3 171.2(4) . . . . no Cr1 O1 C25 C26 -8.7(4) . . . . no Cr1 O2 C26 O4 171.5(4) . . . . no Cr1 O2 C26 C25 -7.4(4) . . . . no Cr1 N1 C1 C2 -175.1(4) . . . . no C12 N1 C1 C2 0.3(8) . . . . no Cr1 N1 C12 C4 175.8(4) . . . . no C1 N1 C12 C4 -0.3(7) . . . . no C1 N1 C12 C11 -179.5(5) . . . . no Cr1 N1 C12 C11 -3.4(5) . . . . no C11 N2 C10 C9 1.4(7) . . . . no Cr1 N2 C10 C9 175.1(4) . . . . no C10 N2 C11 C7 -1.1(7) . . . . no Cr1 N2 C11 C7 -175.7(4) . . . . no Cr1 N2 C11 C12 2.2(5) . . . . no C10 N2 C11 C12 176.8(4) . . . . no C24 N3 C13 C14 0.3(7) . . . . no Cr1 N3 C24 C16 -176.6(4) . . . . no Cr1 N3 C13 C14 174.5(4) . . . . no C13 N3 C24 C16 -1.6(7) . . . . no C13 N3 C24 C23 178.3(4) . . . . no Cr1 N3 C24 C23 3.2(5) . . . . no Cr1 N4 C22 C21 -176.2(5) . . . . no C23 N4 C22 C21 1.4(8) . . . . no Cr1 N4 C23 C19 177.0(4) . . . . no Cr1 N4 C23 C24 -2.0(5) . . . . no C22 N4 C23 C19 -1.0(7) . . . . no C22 N4 C23 C24 -180.0(4) . . . . no N1 C1 C2 C3 -0.5(10) . . . . no C1 C2 C3 C4 0.8(10) . . . . no C2 C3 C4 C5 179.2(6) . . . . no C2 C3 C4 C12 -0.8(8) . . . . no C3 C4 C5 C6 -179.2(6) . . . . no C12 C4 C5 C6 0.8(8) . . . . no C3 C4 C12 N1 0.6(7) . . . . no C3 C4 C12 C11 179.7(5) . . . . no C5 C4 C12 N1 -179.4(5) . . . . no C5 C4 C12 C11 -0.3(7) . . . . no C4 C5 C6 C7 -0.7(9) . . . . no C5 C6 C7 C8 178.0(6) . . . . no C5 C6 C7 C11 0.1(8) . . . . no C6 C7 C8 C9 -177.5(6) . . . . no C11 C7 C8 C9 0.5(8) . . . . no C6 C7 C11 N2 178.3(5) . . . . no C6 C7 C11 C12 0.5(7) . . . . no C8 C7 C11 N2 0.2(7) . . . . no C8 C7 C11 C12 -177.7(5) . . . . no C7 C8 C9 C10 -0.2(9) . . . . no C8 C9 C10 N2 -0.8(8) . . . . no N2 C11 C12 N1 0.8(6) . . . . no N2 C11 C12 C4 -178.4(4) . . . . no C7 C11 C12 N1 178.8(4) . . . . no C7 C11 C12 C4 -0.4(7) . . . . no N3 C13 C14 C15 1.3(8) . . . . no C13 C14 C15 C16 -1.5(7) . . . . no C14 C15 C16 C17 -179.1(5) . . . . no C14 C15 C16 C24 0.3(7) . . . . no C15 C16 C17 C18 177.7(5) . . . . no C24 C16 C17 C18 -1.7(8) . . . . no C15 C16 C24 N3 1.2(7) . . . . no C15 C16 C24 C23 -178.6(4) . . . . no C17 C16 C24 N3 -179.3(5) . . . . no C17 C16 C24 C23 0.9(7) . . . . no C16 C17 C18 C19 1.5(9) . . . . no C17 C18 C19 C20 -179.3(6) . . . . no C17 C18 C19 C23 -0.6(8) . . . . no C18 C19 C20 C21 179.9(6) . . . . no C23 C19 C20 C21 1.2(10) . . . . no C18 C19 C23 N4 -179.0(5) . . . . no C18 C19 C23 C24 -0.2(7) . . . . no C20 C19 C23 N4 -0.2(8) . . . . no C20 C19 C23 C24 178.6(5) . . . . no C19 C20 C21 C22 -0.9(11) . . . . no C20 C21 C22 N4 -0.5(11) . . . . no N4 C23 C24 N3 -0.8(6) . . . . no N4 C23 C24 C16 179.0(4) . . . . no C19 C23 C24 N3 -179.8(5) . . . . no C19 C23 C24 C16 0.0(7) . . . . no O1 C25 C26 O2 10.7(5) . . . . no O1 C25 C26 O4 -168.1(4) . . . . no O3 C25 C26 O2 -169.2(4) . . . . no O3 C25 C26 O4 11.9(6) . . . . no O8 C27 C28 O9 -3.6(9) . . . . no O8 C27 C28 O11 173.5(6) . . . . no O10 C27 C28 O9 179.4(8) . . . . no O10 C27 C28 O11 -3.5(9) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O2 2.581(5) . . no O1 N1 2.910(5) . . no O1 N3 2.848(5) . . no O1 N4 2.891(5) . . no O1 C1 3.114(6) . . no O1 C26 2.388(6) . . no O1 C6 3.249(7) . 4_454 no O2 C22 3.147(6) . . no O2 N2 2.849(5) . . no O2 O1 2.581(5) . . no O2 N1 2.884(5) . . no O2 C25 2.381(6) . . no O2 N4 2.906(5) . . no O2 C17 3.225(7) . 4_555 no O3 C9 3.342(7) . 3_455 no O3 O4 2.831(5) . . no O3 C21 3.243(8) . 2_565 no O3 C20 3.393(8) . 2_565 no O3 C2 3.394(8) . 2_564 no O4 C2 3.246(7) . 2_564 no O4 C21 3.387(8) . 2_565 no O4 C14 3.304(6) . 3_555 no O4 O3 2.831(5) . . no O5 C11 3.247(7) . 4_454 no O5 C13 2.836(7) . 4_454 no O5 O12 3.049(8) . 3_454 no O5 C14 3.323(8) . 4_454 no O6 O11 2.615(7) . 2_564 no O6 C28 3.362(7) . 2_564 no O6 O12 3.143(6) . 3_454 no O7 C10 3.108(6) . 3_455 no O7 O11 2.950(8) . 2_564 no O7 O12 2.846(7) . 4_454 no O8 C13 3.209(7) . . no O8 C1 3.316(8) . . no O8 O9 2.674(10) . . no O8 C2 3.279(9) . . no O8 O12 2.534(7) . . no O9 O8 2.674(10) . . no O9 C1 3.284(11) . . no O9 C13 3.176(10) . . no O10 O11 2.645(10) . . no O11 C21 3.185(10) . 4_455 no O11 O7 2.950(8) . 2_565 no O11 C10 3.338(8) . 4_455 no O11 N5 3.180(8) . 2_565 no O11 O10 2.645(10) . . no O11 C22 3.157(9) . 4_455 no O11 O6 2.615(7) . 2_565 no O12 C27 3.414(8) . . no O12 C24 3.333(6) . 2_555 no O12 O5 3.049(8) . 3_546 no O12 O7 2.846(7) . 4_555 no O12 O8 2.534(7) . . no O12 O6 3.143(6) . 3_546 no O12 C16 3.316(7) . 2_555 no O1 H6 2.6300 . 4_454 no O1 H1 2.6400 . . no O2 H22 2.6700 . . no O2 H17 2.6200 . 4_555 no O3 H2 2.4700 . 2_564 no O3 H21 2.7800 . 2_565 no O3 H9 2.6700 . 3_455 no O3 H6 2.8100 . 4_454 no O4 H14 2.6100 . 3_555 no O4 H2 2.7500 . 2_564 no O4 H21 2.4700 . 2_565 no O4 H17 2.7900 . 4_555 no O5 H12A 2.80(7) . 4_454 no O5 H13 2.7200 . 4_454 no O6 H11A 1.8200 . 2_564 no O6 H12B 2.43(5) . 3_454 no O7 H10 2.4500 . 3_455 no O7 H12A 1.96(8) . 4_454 no O7 H11A 2.4800 . 2_564 no O8 H12A 2.80(8) . . no O8 H13 2.3900 . . no O8 H12B 2.79(5) . . no O9 H5 2.9000 . 4_454 no O9 H13 2.7900 . . no O9 H1 2.7300 . . no O10 H18 2.6200 . 1_556 no O11 H10 2.5600 . 4_455 no O12 H8A 1.7500 . . no N1 O2 2.884(5) . . no N1 C13 3.244(6) . . no N1 O1 2.910(5) . . no N1 N3 3.055(6) . . no N1 C11 2.374(6) . . no N1 N2 2.644(6) . . no N2 O2 2.849(5) . . no N2 C12 2.352(6) . . no N2 N4 3.038(6) . . no N2 N1 2.644(6) . . no N2 N3 3.075(7) . . no N3 C23 2.395(6) . . no N3 N4 2.655(6) . . no N3 N1 3.055(6) . . no N3 N2 3.075(7) . . no N3 O1 2.848(5) . . no N4 N2 3.038(6) . . no N4 C10 3.238(6) . . no N4 O2 2.906(5) . . no N4 C24 2.361(6) . . no N4 N3 2.655(6) . . no N4 O1 2.891(5) . . no N5 O11 3.180(8) . 2_564 no N5 C7 3.450(7) . 4_454 no N1 H13 2.7100 . . no N4 H10 2.7300 . . no N5 H11A 2.4800 . 2_564 no N5 H12A 2.71(7) . 4_454 no C1 O9 3.284(11) . . no C1 O8 3.316(8) . . no C2 O8 3.279(9) . . no C2 O3 3.394(8) . 2_565 no C2 O4 3.246(7) . 2_565 no C3 C15 3.596(8) . 4_555 no C6 O1 3.249(7) . 4_555 no C7 N5 3.450(7) . 4_555 no C9 O3 3.342(7) . 3_545 no C10 O11 3.338(8) . 4_554 no C10 O7 3.108(6) . 3_545 no C11 O5 3.247(7) . 4_555 no C13 O9 3.176(10) . . no C13 O5 2.836(7) . 4_555 no C13 O8 3.209(7) . . no C14 O4 3.304(6) . 3_445 no C14 O5 3.323(8) . 4_555 no C15 C3 3.596(8) . 4_454 no C16 O12 3.316(7) . 2_554 no C17 O2 3.225(7) . 4_454 no C20 O3 3.393(8) . 2_564 no C21 O11 3.185(10) . 4_554 no C21 O3 3.243(8) . 2_564 no C21 O4 3.387(8) . 2_564 no C22 O11 3.157(9) . 4_554 no C24 O12 3.333(6) . 2_554 no C27 O12 3.414(8) . . no C28 O6 3.362(7) . 2_565 no C1 H13 3.0000 . . no C3 H12B 3.03(4) . . no C22 H10 2.9800 . . no C25 H6 2.9400 . 4_454 no C25 H2 3.0700 . 2_564 no C26 H21 3.0700 . 2_565 no C26 H17 2.9400 . 4_555 no H1 O1 2.6400 . . no H1 O9 2.7300 . . no H2 C25 3.0700 . 2_565 no H2 O3 2.4700 . 2_565 no H2 O4 2.7500 . 2_565 no H3 H5 2.5500 . . no H5 H3 2.5500 . . no H5 O9 2.9000 . 4_555 no H6 H8 2.5800 . . no H6 O1 2.6300 . 4_555 no H6 C25 2.9400 . 4_555 no H6 O3 2.8100 . 4_555 no H8 H6 2.5800 . . no H8A H12A 2.1500 . . no H8A O12 1.7500 . . no H8A H12B 2.1000 . . no H9 O3 2.6700 . 3_545 no H10 C22 2.9800 . . no H10 N4 2.7300 . . no H10 O7 2.4500 . 3_545 no H10 O11 2.5600 . 4_554 no H11A O7 2.4800 . 2_565 no H11A O6 1.8200 . 2_565 no H11A N5 2.4800 . 2_565 no H12A O8 2.80(8) . . no H12A H8A 2.1500 . . no H12A N5 2.71(7) . 4_555 no H12A O5 2.80(7) . 4_555 no H12A O7 1.96(8) . 4_555 no H12B O6 2.43(5) . 3_546 no H12B O8 2.79(5) . . no H12B C3 3.03(4) . . no H12B H8A 2.1000 . . no H13 O8 2.3900 . . no H13 C1 3.0000 . . no H13 O9 2.7900 . . no H13 N1 2.7100 . . no H13 O5 2.7200 . 4_555 no H14 O4 2.6100 . 3_445 no H15 H17 2.5500 . . no H17 O2 2.6200 . 4_454 no H17 H15 2.5500 . . no H17 O4 2.7900 . 4_454 no H17 C26 2.9400 . 4_454 no H18 O10 2.6200 . 1_554 no H21 O3 2.7800 . 2_564 no H21 O4 2.4700 . 2_564 no H21 C26 3.0700 . 2_564 no H22 O2 2.6700 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O8 H8A O12 0.8200 1.7500 2.534(7) 159.00 . yes O11 H11A O6 0.8200 1.8200 2.615(7) 164.00 2_565 yes O11 H11A O7 0.8200 2.4800 2.950(8) 117.00 2_565 yes O12 H12A O7 0.94(7) 1.96(8) 2.846(7) 157(7) 4_555 yes O12 H12B O6 0.93(5) 2.43(5) 3.143(6) 133(4) 3_546 yes C2 H2 O3 0.9300 2.4700 3.394(8) 172.00 2_565 yes C10 H10 O7 0.9300 2.4500 3.108(6) 128.00 3_545 yes C10 H10 O11 0.9300 2.5600 3.338(8) 141.00 4_554 yes C13 H13 O8 0.9300 2.3900 3.209(7) 147.00 . yes C21 H21 O4 0.9300 2.4700 3.387(8) 170.00 2_564 yes #===END # Attachment 'HphenCrox2_1.cif' data_HphenCrox2_1 _database_code_depnum_ccdc_archive 'CCDC 847276' #TrackingRef 'HphenCrox2_1.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; 1,10-phenanthrolinium (1,10-phenanthroline-N,N')bis(oxalato-O,O')chromium(III) dihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H8 Cr N2 O8, C12 H9 N2, 2(H2 O)' _chemical_formula_structural 'Cr (C12 H9 N2)(C12 H8 N2) (C2 O4)2 (H2 O)2' _chemical_formula_sum 'C28 H21 Cr N4 O10' _chemical_formula_iupac ? _chemical_formula_weight 625.49 _chemical_compound_source 'synthesized by the authors, see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 18.662(5) _cell_length_b 18.923(5) _cell_length_c 7.637(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.760(5) _cell_angle_gamma 90.00 _cell_volume 2678(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8998 _cell_measurement_theta_min 3.3352 _cell_measurement_theta_max 76.0916 _cell_special_details ; ? ; _exptl_crystal_description needle _exptl_crystal_colour 'red violet' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'Not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 4.117 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.38420 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ;? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'CCD, \w scans' # number of measured reflections (redundant set) _diffrn_reflns_number 15040 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.3352 _diffrn_reflns_theta_max 76.0916 _diffrn_reflns_theta_full 76.27 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_reduction_process ;? ; # number of unique reflections _reflns_number_total 5540 # number of observed reflections (> n sig(I)) _reflns_number_gt 4759 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SIR92 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3 (Farrugia, 1997), MERCURY (Bruno et al., 2002)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0702P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5540 _refine_ls_number_parameters 408 _refine_ls_number_restraints 6 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.311 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.045 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cr1 Cr Uani 0.24054(1) 0.56189(1) 0.51894(3) 1.000 0.0372(1) . . O1 O Uani 0.33548(6) 0.56111(6) 0.43504(15) 1.000 0.0466(3) . . O2 O Uani 0.29782(6) 0.56253(6) 0.75112(14) 1.000 0.0436(3) . . O3 O Uani 0.45165(7) 0.57080(9) 0.5329(2) 1.000 0.0663(5) . . O4 O Uani 0.41145(8) 0.57435(9) 0.87214(19) 1.000 0.0690(5) . . O5 O Uani 0.22592(6) 0.45947(6) 0.50877(14) 1.000 0.0462(3) . . O6 O Uani 0.18846(7) 0.55804(6) 0.28113(15) 1.000 0.0472(3) . . O7 O Uani 0.16998(8) 0.37669(7) 0.33617(19) 1.000 0.0611(4) . . O8 O Uani 0.13599(8) 0.48194(8) 0.08502(18) 1.000 0.0675(5) . . O9 O Uani 0.10816(11) 0.15676(11) 0.4390(2) 1.000 0.0815(6) . . O10 O Uani 0.11247(12) 0.20859(12) 0.0969(3) 1.000 0.0913(7) . . N1 N Uani 0.23664(7) 0.67163(7) 0.51482(16) 1.000 0.0423(3) . . N2 N Uani 0.14391(7) 0.57833(8) 0.62224(18) 1.000 0.0459(4) . . N3 N Uani 0.43038(7) 0.38433(8) 0.23028(19) 1.000 0.0477(4) . . N4 N Uani 0.49121(9) 0.25493(10) 0.3095(2) 1.000 0.0637(5) . . C1 C Uani 0.28552(10) 0.71671(9) 0.4669(2) 1.000 0.0503(5) . . C2 C Uani 0.27532(12) 0.78968(10) 0.4676(3) 1.000 0.0608(6) . . C3 C Uani 0.21313(13) 0.81679(10) 0.5176(2) 1.000 0.0628(6) . . C4 C Uani 0.16052(11) 0.77095(10) 0.5707(2) 1.000 0.0561(5) . . C5 C Uani 0.09401(13) 0.79357(13) 0.6265(3) 1.000 0.0703(7) . . C6 C Uani 0.04582(12) 0.74654(15) 0.6751(3) 1.000 0.0740(8) . . C7 C Uani 0.05982(9) 0.67169(12) 0.6766(2) 1.000 0.0603(6) . . C8 C Uani 0.01394(10) 0.61960(17) 0.7332(3) 1.000 0.0770(8) . . C9 C Uani 0.03438(11) 0.55037(16) 0.7378(3) 1.000 0.0750(8) . . C10 C Uani 0.10031(10) 0.53084(12) 0.6814(3) 1.000 0.0604(6) . . C11 C Uani 0.12458(8) 0.64802(10) 0.6215(2) 1.000 0.0472(5) . . C12 C Uani 0.17482(8) 0.69809(9) 0.56663(19) 1.000 0.0446(4) . . C13 C Uani 0.40421(11) 0.44870(10) 0.1995(3) 1.000 0.0569(6) . . C14 C Uani 0.33802(11) 0.45792(11) 0.0985(3) 1.000 0.0609(6) . . C15 C Uani 0.30025(10) 0.40003(11) 0.0335(3) 1.000 0.0575(6) . . C16 C Uani 0.32712(8) 0.33158(10) 0.0693(2) 1.000 0.0478(5) . . C17 C Uani 0.28945(9) 0.26871(12) 0.0104(3) 1.000 0.0605(6) . . C18 C Uani 0.31740(12) 0.20467(11) 0.0523(3) 1.000 0.0650(6) . . C19 C Uani 0.38596(11) 0.19686(10) 0.1530(3) 1.000 0.0567(6) . . C20 C Uani 0.41657(17) 0.13053(12) 0.2023(3) 1.000 0.0788(8) . . C21 C Uani 0.48137(18) 0.12816(14) 0.3019(3) 1.000 0.0870(9) . . C22 C Uani 0.51677(14) 0.19086(15) 0.3511(3) 1.000 0.0830(9) . . C23 C Uani 0.42573(9) 0.25700(9) 0.2125(2) 1.000 0.0480(5) . . C24 C Uani 0.39491(8) 0.32490(8) 0.1704(2) 1.000 0.0428(4) . . C25 C Uani 0.38899(9) 0.56655(8) 0.5572(2) 1.000 0.0442(4) . . C26 C Uani 0.36641(9) 0.56783(8) 0.7467(2) 1.000 0.0438(4) . . C27 C Uani 0.18907(8) 0.43725(8) 0.3663(2) 1.000 0.0434(4) . . C28 C Uani 0.16842(8) 0.49609(9) 0.2279(2) 1.000 0.0446(4) . . H1 H Uiso 0.32799 0.69888 0.43159 1.000 0.0603 . . H2 H Uiso 0.31074 0.81972 0.43421 1.000 0.0729 . . H3 H Uiso 0.20558 0.86537 0.51651 1.000 0.0754 . . H3A H Uiso 0.4704(14) 0.3824(12) 0.289(3) 1.000 0.063(6) . . H5 H Uiso 0.08368 0.84160 0.62946 1.000 0.0843 . . H6 H Uiso 0.00242 0.76284 0.70846 1.000 0.0888 . . H8 H Uiso -0.03045 0.63240 0.76750 1.000 0.0924 . . H9 H Uiso 0.00457 0.51618 0.77839 1.000 0.0900 . . H9A H Uiso 0.1178(18) 0.1197(12) 0.511(4) 1.000 0.107(11) . . H9B H Uiso 0.1109(13) 0.1959(9) 0.504(3) 1.000 0.060(6) . . H10 H Uiso 0.11384 0.48351 0.68552 1.000 0.0725 . . H10A H Uiso 0.1413(14) 0.2000(16) 0.196(3) 1.000 0.091(9) . . H10B H Uiso 0.1297(19) 0.1751(16) 0.022(4) 1.000 0.123(13) . . H13 H Uiso 0.43016 0.48777 0.24564 1.000 0.0683 . . H14 H Uiso 0.31964 0.50307 0.07525 1.000 0.0730 . . H15 H Uiso 0.25613 0.40597 -0.03528 1.000 0.0690 . . H17 H Uiso 0.24493 0.27215 -0.05799 1.000 0.0727 . . H18 H Uiso 0.29129 0.16451 0.01451 1.000 0.0780 . . H20 H Uiso 0.39246 0.08901 0.16672 1.000 0.0945 . . H21 H Uiso 0.50204 0.08496 0.33705 1.000 0.1044 . . H22 H Uiso 0.56164 0.18776 0.41801 1.000 0.0996 . . 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 0.0348(1) 0.0354(1) 0.0405(1) 0.0018(1) 0.0010(1) 0.0007(1) O1 0.0420(5) 0.0534(7) 0.0445(5) -0.0045(4) 0.0061(4) 0.0012(4) O2 0.0415(5) 0.0486(6) 0.0402(5) 0.0002(4) 0.0024(4) 0.0005(4) O3 0.0409(6) 0.0895(10) 0.0696(8) -0.0120(7) 0.0114(6) -0.0084(6) O4 0.0535(7) 0.0956(11) 0.0546(7) -0.0020(7) -0.0075(6) -0.0150(7) O5 0.0497(6) 0.0378(5) 0.0484(6) 0.0048(4) -0.0049(4) 0.0008(4) O6 0.0506(6) 0.0431(6) 0.0452(5) 0.0071(4) -0.0056(5) -0.0003(4) O7 0.0698(8) 0.0436(6) 0.0662(7) 0.0021(5) -0.0077(6) -0.0107(6) O8 0.0793(9) 0.0613(8) 0.0553(7) 0.0008(6) -0.0194(6) -0.0029(7) O9 0.0949(12) 0.0829(12) 0.0662(9) 0.0182(9) 0.0073(8) 0.0178(9) O10 0.1103(14) 0.0868(13) 0.0795(11) 0.0005(9) 0.0224(10) 0.0232(11) N1 0.0457(6) 0.0375(6) 0.0423(6) 0.0015(4) -0.0012(5) 0.0022(5) N2 0.0348(6) 0.0550(7) 0.0472(7) 0.0026(5) 0.0022(5) -0.0001(5) N3 0.0393(6) 0.0482(7) 0.0554(7) -0.0018(6) 0.0048(6) -0.0050(5) N4 0.0551(8) 0.0715(10) 0.0630(9) 0.0026(8) 0.0005(7) 0.0170(8) C1 0.0558(9) 0.0430(8) 0.0505(8) 0.0065(6) -0.0002(7) -0.0062(7) C2 0.0808(12) 0.0424(9) 0.0552(9) 0.0056(7) -0.0085(9) -0.0092(8) C3 0.0938(14) 0.0390(8) 0.0497(9) -0.0023(6) -0.0162(9) 0.0064(9) C4 0.0696(11) 0.0524(9) 0.0412(7) -0.0085(6) -0.0145(7) 0.0179(8) C5 0.0772(13) 0.0714(13) 0.0568(10) -0.0166(9) -0.0145(9) 0.0366(11) C6 0.0573(11) 0.1030(17) 0.0578(10) -0.0226(11) -0.0097(9) 0.0404(12) C7 0.0400(8) 0.0914(14) 0.0473(8) -0.0106(8) -0.0043(7) 0.0159(8) C8 0.0393(9) 0.128(2) 0.0636(11) -0.0112(12) 0.0060(8) 0.0076(11) C9 0.0459(10) 0.113(2) 0.0673(12) 0.0057(12) 0.0112(9) -0.0153(11) C10 0.0471(9) 0.0746(12) 0.0594(10) 0.0072(9) 0.0058(7) -0.0106(8) C11 0.0385(7) 0.0611(10) 0.0397(7) -0.0036(6) -0.0051(5) 0.0097(7) C12 0.0465(7) 0.0464(8) 0.0381(7) -0.0034(6) -0.0072(6) 0.0091(6) C13 0.0626(10) 0.0453(9) 0.0661(10) -0.0034(7) 0.0210(9) -0.0086(7) C14 0.0670(11) 0.0515(10) 0.0671(11) 0.0125(8) 0.0204(9) 0.0129(8) C15 0.0458(8) 0.0689(12) 0.0579(9) 0.0096(8) 0.0061(7) 0.0104(8) C16 0.0376(7) 0.0575(9) 0.0487(8) 0.0017(7) 0.0068(6) -0.0012(6) C17 0.0426(8) 0.0753(13) 0.0625(10) -0.0061(9) 0.0012(7) -0.0137(8) C18 0.0682(11) 0.0591(11) 0.0691(11) -0.0129(9) 0.0140(9) -0.0222(9) C19 0.0717(11) 0.0462(9) 0.0553(9) -0.0024(7) 0.0201(8) -0.0005(8) C20 0.124(2) 0.0473(10) 0.0699(12) -0.0025(9) 0.0321(13) 0.0116(11) C21 0.122(2) 0.0685(14) 0.0734(13) 0.0080(11) 0.0237(14) 0.0462(15) C22 0.0805(14) 0.0930(18) 0.0739(13) 0.0089(12) 0.0030(11) 0.0409(13) C23 0.0478(8) 0.0494(9) 0.0477(8) 0.0012(6) 0.0093(6) 0.0056(6) C24 0.0376(7) 0.0450(8) 0.0463(7) 0.0003(6) 0.0077(5) -0.0030(6) C25 0.0397(7) 0.0395(7) 0.0535(9) -0.0050(6) 0.0055(6) -0.0001(5) C26 0.0412(7) 0.0401(7) 0.0485(8) -0.0014(5) -0.0013(6) -0.0034(5) C27 0.0392(7) 0.0411(8) 0.0489(8) 0.0030(6) 0.0009(6) -0.0005(5) C28 0.0402(7) 0.0467(8) 0.0456(8) 0.0035(6) -0.0006(6) 0.0009(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.9538(17) . . yes Cr1 O2 1.9598(17) . . yes Cr1 O5 1.9575(17) . . yes Cr1 O6 1.9578(17) . . yes Cr1 N1 2.0780(19) . . yes Cr1 N2 2.0751(19) . . yes O1 C25 1.288(2) . . yes O2 C26 1.288(2) . . yes O3 C25 1.208(2) . . yes O4 C26 1.204(2) . . yes O5 C27 1.287(2) . . yes O6 C28 1.282(2) . . yes O7 C27 1.214(2) . . yes O8 C28 1.214(2) . . yes O9 H9B 0.890(19) . . no O9 H9A 0.90(3) . . no O10 H10B 0.94(3) . . no O10 H10A 0.89(2) . . no N1 C1 1.331(2) . . yes N1 C12 1.359(2) . . yes N2 C11 1.367(3) . . yes N2 C10 1.327(3) . . yes N3 C13 1.323(3) . . yes N3 C24 1.357(2) . . yes N4 C22 1.328(3) . . yes N4 C23 1.353(2) . . yes N3 H3A 0.83(3) . . no C1 C2 1.394(3) . . no C2 C3 1.364(3) . . no C3 C4 1.405(3) . . no C4 C12 1.405(3) . . no C4 C5 1.425(3) . . no C5 C6 1.348(4) . . no C6 C7 1.440(4) . . no C7 C11 1.399(3) . . no C7 C8 1.407(3) . . no C8 C9 1.364(4) . . no C9 C10 1.400(3) . . no C11 C12 1.430(2) . . no C13 C14 1.388(3) . . no C14 C15 1.364(3) . . no C15 C16 1.404(3) . . no C16 C24 1.408(2) . . no C16 C17 1.427(3) . . no C17 C18 1.343(3) . . no C18 C19 1.421(3) . . no C19 C23 1.405(3) . . no C19 C20 1.412(3) . . no C20 C21 1.352(4) . . no C21 C22 1.388(4) . . no C23 C24 1.429(2) . . no C25 C26 1.554(2) . . no C27 C28 1.552(2) . . no C1 H1 0.9300 . . no C2 H2 0.9300 . . no C3 H3 0.9300 . . no C5 H5 0.9300 . . no C6 H6 0.9300 . . no C8 H8 0.9300 . . no C9 H9 0.9300 . . no C10 H10 0.9300 . . no C13 H13 0.9300 . . no C14 H14 0.9300 . . no C15 H15 0.9300 . . no C17 H17 0.9300 . . no C18 H18 0.9300 . . no C20 H20 0.9300 . . no C21 H21 0.9300 . . no C22 H22 0.9300 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr1 O1 C25 114.68(10) . . . yes Cr1 O2 C26 114.49(10) . . . yes Cr1 O5 C27 114.52(10) . . . yes Cr1 O6 C28 115.00(10) . . . yes Cr1 N1 C12 113.16(10) . . . yes Cr1 N1 C1 128.36(11) . . . yes Cr1 N2 C11 112.57(10) . . . yes Cr1 N2 C10 128.55(13) . . . yes O1 Cr1 O2 82.97(5) . . . yes O1 Cr1 O5 96.15(5) . . . yes O1 Cr1 O6 93.77(5) . . . yes O1 Cr1 N1 91.95(5) . . . yes O1 Cr1 N2 171.12(5) . . . yes O1 C25 O3 125.17(15) . . . yes O1 C25 C26 113.80(14) . . . yes O2 Cr1 O5 95.78(5) . . . yes O2 Cr1 O6 176.31(5) . . . yes O2 Cr1 N1 91.26(5) . . . yes O2 Cr1 N2 93.50(5) . . . yes O2 C26 O4 126.14(15) . . . yes O2 C26 C25 113.72(13) . . . yes O3 C25 C26 121.02(15) . . . yes O4 C26 C25 120.13(15) . . . yes O5 C27 O7 125.74(15) . . . yes O5 Cr1 O6 82.80(5) . . . yes O5 Cr1 N1 169.86(5) . . . yes O5 Cr1 N2 92.31(5) . . . yes O6 Cr1 N1 90.60(5) . . . yes O6 Cr1 N2 89.97(5) . . . yes O7 C27 C28 120.28(14) . . . yes O5 C27 C28 113.97(13) . . . yes O6 C28 C27 113.59(13) . . . yes O6 C28 O8 125.65(16) . . . yes O8 C28 C27 120.76(15) . . . yes N1 Cr1 N2 79.95(6) . . . yes N1 C1 C2 122.37(17) . . . yes N1 C1 H1 119.00 . . . no N1 C12 C4 122.55(15) . . . yes N1 C12 C11 116.72(15) . . . yes N2 C10 H10 119.00 . . . no N2 C10 C9 121.5(2) . . . yes N2 C11 C7 122.98(16) . . . yes N2 C11 C12 117.30(14) . . . yes N3 C13 C14 120.01(18) . . . yes N3 C24 C23 120.14(14) . . . yes N3 C24 C16 118.79(15) . . . yes N3 C13 H13 120.00 . . . no N4 C22 H22 118.00 . . . no N4 C22 C21 124.7(2) . . . yes N4 C23 C24 117.58(16) . . . yes N4 C23 C19 124.23(17) . . . yes C1 N1 C12 118.47(14) . . . yes C1 C2 C3 119.65(19) . . . no C1 C2 H2 120.00 . . . no C2 C1 H1 119.00 . . . no C2 C3 C4 119.68(18) . . . no C2 C3 H3 120.00 . . . no C3 C2 H2 120.00 . . . no C3 C4 C5 124.32(19) . . . no C3 C4 C12 117.28(17) . . . no C4 C5 C6 121.1(2) . . . no C4 C12 C11 120.72(15) . . . no C4 C3 H3 120.00 . . . no C4 C5 H5 119.00 . . . no C5 C4 C12 118.41(18) . . . no C5 C6 C7 121.7(2) . . . no C5 C6 H6 119.00 . . . no C6 C7 C8 125.12(19) . . . no C6 C7 C11 118.34(18) . . . no C6 C5 H5 119.00 . . . no C7 C8 C9 120.17(19) . . . no C7 C11 C12 119.69(17) . . . no C7 C6 H6 119.00 . . . no C7 C8 H8 120.00 . . . no C8 C7 C11 116.5(2) . . . no C8 C9 C10 119.9(2) . . . no C8 C9 H9 120.00 . . . no C9 C8 H8 120.00 . . . no C9 C10 H10 119.00 . . . no C10 N2 C11 118.86(15) . . . yes C10 C9 H9 120.00 . . . no C13 N3 C24 123.23(15) . . . yes C13 N3 H3A 115.4(16) . . . no C13 C14 C15 119.29(19) . . . no C13 C14 H14 120.00 . . . no C14 C15 C16 120.83(18) . . . no C14 C13 H13 120.00 . . . no C14 C15 H15 120.00 . . . no C15 C16 C17 123.79(16) . . . no C15 C16 C24 117.83(16) . . . no C15 C14 H14 120.00 . . . no C16 C17 C18 120.93(18) . . . no C16 C24 C23 121.07(15) . . . no C16 C15 H15 120.00 . . . no C16 C17 H17 120.00 . . . no C17 C16 C24 118.38(16) . . . no C17 C18 C19 121.51(19) . . . no C17 C18 H18 119.00 . . . no C18 C19 C20 123.2(2) . . . no C18 C19 C23 119.91(17) . . . no C18 C17 H17 120.00 . . . no C19 C20 C21 119.1(2) . . . no C19 C23 C24 118.19(15) . . . no C19 C18 H18 119.00 . . . no C19 C20 H20 120.00 . . . no C20 C19 C23 116.9(2) . . . no C20 C21 H21 120.00 . . . no C20 C21 C22 119.3(2) . . . no C21 C20 H20 120.00 . . . no C21 C22 H22 118.00 . . . no C22 N4 C23 115.68(19) . . . yes C22 C21 H21 120.00 . . . no C24 N3 H3A 121.4(16) . . . no H9A O9 H9B 108(2) . . . no H10A O10 H10B 100(3) . . . no 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 Cr1 O1 C25 O3 -175.97(15) . . . . no Cr1 O1 C25 C26 3.64(16) . . . . no Cr1 O2 C26 O4 174.32(15) . . . . no Cr1 O2 C26 C25 -4.59(16) . . . . no Cr1 O5 C27 O7 -175.45(14) . . . . no Cr1 O5 C27 C28 3.79(16) . . . . no Cr1 O6 C28 O8 -179.52(14) . . . . no Cr1 O6 C28 C27 0.88(17) . . . . no Cr1 N1 C1 C2 178.83(14) . . . . no Cr1 N1 C12 C4 -178.88(12) . . . . no Cr1 N1 C12 C11 2.44(16) . . . . no Cr1 N2 C10 C9 -176.14(15) . . . . no Cr1 N2 C11 C7 176.78(12) . . . . no Cr1 N2 C11 C12 -5.25(17) . . . . no O1 Cr1 O2 C26 5.23(11) . . . . no O1 Cr1 O5 C27 -95.76(11) . . . . no O1 Cr1 O6 C28 96.56(12) . . . . no O1 Cr1 N1 C1 0.60(13) . . . . no O1 Cr1 N1 C12 179.68(10) . . . . no O1 C25 C26 O2 0.66(19) . . . . no O1 C25 C26 O4 -178.33(16) . . . . no O2 Cr1 O1 C25 -4.84(11) . . . . no O2 Cr1 O5 C27 -179.28(10) . . . . no O2 Cr1 N1 C1 83.61(13) . . . . no O2 Cr1 N1 C12 -97.32(10) . . . . no O2 Cr1 N2 C10 -86.27(17) . . . . no O2 Cr1 N2 C11 95.60(11) . . . . no O3 C25 C26 O4 1.3(2) . . . . no O3 C25 C26 O2 -179.72(16) . . . . no O5 Cr1 O1 C25 -99.93(11) . . . . no O5 Cr1 O2 C26 100.73(11) . . . . no O5 Cr1 O6 C28 0.83(11) . . . . no O5 Cr1 N2 C10 9.67(17) . . . . no O5 Cr1 N2 C11 -168.47(11) . . . . no O5 C27 C28 O6 -3.14(19) . . . . no O5 C27 C28 O8 177.24(15) . . . . no O6 Cr1 O1 C25 176.92(11) . . . . no O6 Cr1 O5 C27 -2.71(11) . . . . no O6 Cr1 N1 C1 -93.20(13) . . . . no O6 Cr1 N1 C12 85.88(10) . . . . no O6 Cr1 N2 C10 92.46(16) . . . . no O6 Cr1 N2 C11 -85.67(11) . . . . no O7 C27 C28 O8 -3.5(2) . . . . no O7 C27 C28 O6 176.15(15) . . . . no N1 Cr1 O1 C25 86.19(11) . . . . no N1 Cr1 O2 C26 -86.59(11) . . . . no N1 Cr1 O6 C28 -171.45(12) . . . . no N1 Cr1 N2 C10 -176.92(17) . . . . no N1 Cr1 N2 C11 4.94(10) . . . . no N1 C1 C2 C3 -0.5(3) . . . . no N2 Cr1 O2 C26 -166.59(11) . . . . no N2 Cr1 O5 C27 86.97(11) . . . . no N2 Cr1 O6 C28 -91.50(12) . . . . no N2 Cr1 N1 C1 176.94(14) . . . . no N2 Cr1 N1 C12 -3.99(10) . . . . no N2 C11 C12 N1 1.9(2) . . . . no N2 C11 C12 C4 -176.78(14) . . . . no N3 C13 C14 C15 0.7(3) . . . . no N4 C23 C24 N3 -1.4(2) . . . . no N4 C23 C24 C16 179.70(15) . . . . no C1 N1 C12 C4 0.3(2) . . . . no C1 N1 C12 C11 -178.39(14) . . . . no C1 C2 C3 C4 1.1(3) . . . . no C2 C3 C4 C5 179.56(19) . . . . no C2 C3 C4 C12 -1.0(2) . . . . no C3 C4 C5 C6 179.74(19) . . . . no C3 C4 C12 N1 0.3(2) . . . . no C3 C4 C12 C11 178.92(14) . . . . no C4 C5 C6 C7 1.4(3) . . . . no C5 C4 C12 N1 179.80(16) . . . . no C5 C4 C12 C11 -1.6(2) . . . . no C5 C6 C7 C8 176.9(2) . . . . no C5 C6 C7 C11 -1.7(3) . . . . no C6 C7 C8 C9 -176.5(2) . . . . no C6 C7 C11 N2 178.25(16) . . . . no C6 C7 C11 C12 0.3(2) . . . . no C7 C8 C9 C10 -1.8(3) . . . . no C7 C11 C12 C4 1.3(2) . . . . no C7 C11 C12 N1 179.97(14) . . . . no C8 C7 C11 N2 -0.4(2) . . . . no C8 C7 C11 C12 -178.33(16) . . . . no C8 C9 C10 N2 -0.3(3) . . . . no C10 N2 C11 C7 -1.6(2) . . . . no C10 N2 C11 C12 176.41(16) . . . . no C11 N2 C10 C9 1.9(3) . . . . no C11 C7 C8 C9 2.1(3) . . . . no C12 N1 C1 C2 -0.2(2) . . . . no C12 C4 C5 C6 0.3(3) . . . . no C13 N3 C24 C16 0.5(2) . . . . no C13 N3 C24 C23 -178.45(17) . . . . no C13 C14 C15 C16 0.8(3) . . . . no C14 C15 C16 C17 177.9(2) . . . . no C14 C15 C16 C24 -1.6(3) . . . . no C15 C16 C17 C18 -178.5(2) . . . . no C15 C16 C24 N3 1.0(2) . . . . no C15 C16 C24 C23 179.89(16) . . . . no C16 C17 C18 C19 -1.5(3) . . . . no C17 C16 C24 N3 -178.55(16) . . . . no C17 C16 C24 C23 0.4(2) . . . . no C17 C18 C19 C20 178.9(2) . . . . no C17 C18 C19 C23 0.6(3) . . . . no C18 C19 C20 C21 -178.4(2) . . . . no C18 C19 C23 N4 179.74(18) . . . . no C18 C19 C23 C24 0.7(3) . . . . no C19 C20 C21 C22 -1.0(4) . . . . no C19 C23 C24 N3 177.77(16) . . . . no C19 C23 C24 C16 -1.2(2) . . . . no C20 C19 C23 N4 1.4(3) . . . . no C20 C19 C23 C24 -177.66(18) . . . . no C20 C21 C22 N4 1.0(4) . . . . no C22 N4 C23 C24 177.67(17) . . . . no C22 N4 C23 C19 -1.4(3) . . . . no C23 N4 C22 C21 0.2(3) . . . . no C23 C19 C20 C21 -0.2(3) . . . . no C24 N3 C13 C14 -1.4(3) . . . . no C24 C16 C17 C18 0.9(3) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O2 2.593(2) . . no O1 O5 2.910(2) . . no O1 O6 2.855(3) . . no O1 N1 2.900(3) . . no O1 C1 3.107(3) . . no O1 C13 3.154(3) . . no O1 C14 3.233(3) . . no O1 C26 2.386(2) . . no O2 C25 2.385(3) . . no O2 N1 2.887(3) . . no O2 O1 2.593(2) . . no O2 O5 2.906(2) . . no O2 N2 2.940(3) . . no O2 C14 3.324(3) . 1_556 no O2 C2 3.301(3) . 4_565 no O3 C13 3.202(3) . 3_666 no O3 N3 2.811(3) . 3_666 no O3 O4 2.782(3) . . no O3 C20 3.405(4) . 2_655 no O3 C21 3.167(4) . 2_655 no O4 O3 2.782(3) . . no O4 N3 3.237(3) . 3_666 no O4 C22 3.234(4) . 2_656 no O4 C21 3.172(4) . 2_656 no O4 C14 3.206(3) . 1_556 no O5 N2 2.909(3) . . no O5 C10 3.128(3) . . no O5 O6 2.589(2) . . no O5 O2 2.906(2) . . no O5 C28 2.386(2) . . no O5 O1 2.910(2) . . no O6 C27 2.376(2) . . no O6 N1 2.870(3) . . no O6 N2 2.852(3) . . no O6 O5 2.589(2) . . no O6 O1 2.855(3) . . no O6 C3 3.177(3) . 4_564 no O7 C18 3.405(3) . 4_555 no O7 O9 3.179(3) . 4_554 no O7 C8 3.412(3) . 3_566 no O7 O8 2.786(3) . . no O7 O10 2.868(3) . 4_555 no O8 O9 2.875(3) . 4_554 no O8 O7 2.786(3) . . no O8 C9 3.335(4) . 1_554 no O8 C10 3.212(3) . 1_554 no O9 O10 2.801(3) . . no O9 O10 2.816(4) . 4_555 no O9 O8 2.875(3) . 4_555 no O9 O7 3.179(3) . 4_555 no O10 O9 2.801(3) . . no O10 O9 2.816(4) . 4_554 no O10 O7 2.868(3) . 4_554 no O1 H13 2.7800 . . no O1 H1 2.6100 . . no O2 H14 2.7100 . 1_556 no O2 H2 2.6300 . 4_565 no O3 H13 2.6900 . . no O3 H13 2.8400 . 3_666 no O3 H3A 2.07(2) . 3_666 no O4 H3A 2.77(3) . 3_666 no O4 H14 2.7900 . 1_556 no O4 H21 2.6000 . 2_656 no O4 H2 2.8300 . 4_565 no O4 H22 2.6900 . 2_656 no O5 H18 2.6400 . 4_555 no O5 H10 2.6600 . . no O6 H3 2.5400 . 4_564 no O6 H5 2.8700 . 4_564 no O7 H18 2.6200 . 4_555 no O7 H8 2.6400 . 3_566 no O7 H9A 2.56(3) . 4_554 no O7 H10B 1.95(3) . 4_555 no O8 H15 2.9000 . . no O8 H9A 2.02(2) . 4_554 no O9 H10A 2.18(2) . . no O9 H6 2.7000 . 3_566 no O9 H8 2.8500 . 2_546 no O9 H17 2.8800 . 4_555 no O10 H6 2.8000 . 3_566 no O10 H9B 1.941(18) . 4_554 no N1 C11 2.374(3) . . no N1 O1 2.900(3) . . no N1 O2 2.887(3) . . no N1 O6 2.870(3) . . no N1 N2 2.668(3) . . no N1 C26 3.442(3) . . no N2 C12 2.389(3) . . no N2 O2 2.940(3) . . no N2 O5 2.909(3) . . no N2 N1 2.668(3) . . no N2 O6 2.852(3) . . no N3 O3 2.811(3) . 3_666 no N3 N4 2.737(3) . . no N3 O4 3.237(3) . 3_666 no N4 N3 2.737(3) . . no N4 C23 3.450(3) . 4_555 no N4 H3A 2.45(2) . . no C1 C3 3.593(3) . 4_564 no C1 C25 3.459(3) . . no C2 O2 3.301(3) . 4_564 no C2 C12 3.405(3) . 4_564 no C3 C11 3.339(3) . 4_564 no C3 C1 3.593(3) . 4_565 no C3 C12 3.446(3) . 4_564 no C3 O6 3.177(3) . 4_565 no C4 C7 3.527(3) . 4_564 no C4 C6 3.507(4) . 4_564 no C5 C12 3.522(4) . 4_565 no C5 C8 3.591(4) . 4_564 no C5 C7 3.483(4) . 4_564 no C5 C6 3.541(4) . 4_564 no C6 C5 3.541(4) . 4_565 no C6 C4 3.507(4) . 4_565 no C7 C4 3.527(3) . 4_565 no C7 C5 3.483(4) . 4_565 no C8 C5 3.591(4) . 4_565 no C8 O7 3.412(3) . 3_566 no C9 O8 3.335(4) . 1_556 no C10 C27 3.551(4) . . no C10 O8 3.212(3) . 1_556 no C11 C3 3.339(3) . 4_565 no C12 C5 3.522(4) . 4_564 no C12 C2 3.405(3) . 4_565 no C12 C3 3.446(3) . 4_565 no C13 O1 3.154(3) . . no C13 O3 3.202(3) . 3_666 no C13 C25 3.564(4) . . no C14 C28 3.500(3) . . no C14 O2 3.324(3) . 1_554 no C14 O4 3.206(3) . 1_554 no C14 C26 3.487(4) . 1_554 no C14 O1 3.233(3) . . no C15 C28 3.524(3) . . no C15 C20 3.569(4) . 4_554 no C15 C27 3.536(3) . . no C16 C19 3.525(4) . 4_554 no C16 C20 3.501(4) . 4_554 no C17 C19 3.504(4) . 4_554 no C18 C24 3.450(4) . 4_554 no C18 O7 3.405(3) . 4_554 no C18 C23 3.547(4) . 4_554 no C19 C17 3.504(4) . 4_555 no C19 C16 3.525(4) . 4_555 no C20 C15 3.569(4) . 4_555 no C20 C16 3.501(4) . 4_555 no C20 O3 3.405(4) . 2_645 no C21 O3 3.167(4) . 2_645 no C21 O4 3.172(4) . 2_646 no C21 C24 3.519(4) . 4_555 no C22 C24 3.537(4) . 4_555 no C22 O4 3.234(4) . 2_646 no C22 C23 3.547(4) . 4_555 no C23 N4 3.450(3) . 4_554 no C23 C22 3.547(4) . 4_554 no C23 C18 3.547(4) . 4_555 no C24 C21 3.519(4) . 4_554 no C24 C22 3.537(4) . 4_554 no C24 C18 3.450(4) . 4_555 no C25 C13 3.564(4) . . no C25 C1 3.459(3) . . no C26 C14 3.487(4) . 1_556 no C27 C10 3.551(4) . . no C27 C15 3.536(3) . . no C28 C14 3.500(3) . . no C28 C15 3.524(3) . . no C2 H22 3.0900 . 3_666 no C25 H20 3.0600 . 4_555 no C25 H3A 2.91(3) . 3_666 no C25 H1 2.8700 . . no C25 H13 2.9800 . . no C26 H14 3.0100 . 1_556 no C26 H20 3.0800 . 4_555 no C26 H2 2.8300 . 4_565 no C27 H18 2.8500 . 4_555 no C27 H10 3.0800 . . no C27 H9A 3.07(3) . 4_554 no C27 H10B 2.73(3) . 4_555 no C28 H9A 2.84(3) . 4_554 no H1 C25 2.8700 . . no H1 O1 2.6100 . . no H2 H22 2.5200 . 3_666 no H2 O2 2.6300 . 4_564 no H2 O4 2.8300 . 4_564 no H2 C26 2.8300 . 4_564 no H3 H5 2.5700 . . no H3 O6 2.5400 . 4_565 no H3A C25 2.91(3) . 3_666 no H3A O3 2.07(2) . 3_666 no H3A O4 2.77(3) . 3_666 no H3A N4 2.45(2) . . no H5 H3 2.5700 . . no H5 O6 2.8700 . 4_565 no H6 H8 2.6000 . . no H6 O9 2.7000 . 3_566 no H6 O10 2.8000 . 3_566 no H8 H9A 2.5000 . 2_556 no H8 O7 2.6400 . 3_566 no H8 O9 2.8500 . 2_556 no H8 H6 2.6000 . . no H9A H8 2.5000 . 2_546 no H9A O7 2.56(3) . 4_555 no H9A O8 2.02(2) . 4_555 no H9A C27 3.07(3) . 4_555 no H9A C28 2.84(3) . 4_555 no H9B H10A 2.48(3) . 4_555 no H9B O10 1.941(18) . 4_555 no H9B H10B 2.47(3) . 4_555 no H9B H10A 2.49(3) . . no H10 O5 2.6600 . . no H10 C27 3.0800 . . no H10A H9B 2.49(3) . . no H10A O9 2.18(2) . . no H10A H9B 2.48(3) . 4_554 no H10A H17 2.5900 . 4_555 no H10B O7 1.95(3) . 4_554 no H10B C27 2.73(3) . 4_554 no H10B H9B 2.47(3) . 4_554 no H13 O1 2.7800 . . no H13 C25 2.9800 . . no H13 H21 2.3600 . 2_655 no H13 O3 2.6900 . . no H13 O3 2.8400 . 3_666 no H14 C26 3.0100 . 1_554 no H14 O4 2.7900 . 1_554 no H14 O2 2.7100 . 1_554 no H15 O8 2.9000 . . no H15 H17 2.5500 . . no H17 H15 2.5500 . . no H17 O9 2.8800 . 4_554 no H17 H10A 2.5900 . 4_554 no H18 O5 2.6400 . 4_554 no H18 O7 2.6200 . 4_554 no H18 H20 2.5400 . . no H18 C27 2.8500 . 4_554 no H20 H18 2.5400 . . no H20 C25 3.0600 . 4_554 no H20 C26 3.0800 . 4_554 no H21 H13 2.3600 . 2_645 no H21 O4 2.6000 . 2_646 no H22 H2 2.5200 . 3_666 no H22 C2 3.0900 . 3_666 no H22 O4 2.6900 . 2_646 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # N3 H3A N4 0.83(3) 2.45(2) 2.737(3) 101.8(18) . yes N3 H3A O3 0.83(3) 2.07(2) 2.811(3) 149(2) 3_666 yes O9 H9A O7 0.90(3) 2.56(3) 3.179(3) 127(2) 4_555 yes O9 H9A O8 0.90(3) 2.02(2) 2.875(3) 159(3) 4_555 yes O9 H9B O10 0.890(19) 1.941(18) 2.816(4) 168(2) 4_555 yes O10 H10A O9 0.89(2) 2.18(2) 2.801(3) 126(2) . yes O10 H10B O7 0.94(3) 1.95(3) 2.868(3) 168(3) 4_554 yes C3 H3 O6 0.9300 2.5400 3.177(3) 126.00 4_565 yes C21 H21 O4 0.9300 2.6000 3.172(4) 121.00 2_646 yes #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_lidija_crii_2 _database_code_depnum_ccdc_archive 'CCDC 891474' #TrackingRef 'cifdoc_Ca.cif' _audit_creation_date 2012-07-02T15:07:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C28 H16 Ca Cr2 N4 O16, 0.83(O)' _chemical_formula_sum 'C28 H18 Ca Cr2 N4 O16.83' _chemical_formula_weight 821.79 #------------------ UNIT CELL INFORMATION -----------------------------------# _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 8.9224(3) _cell_length_b 9.9414(3) _cell_length_c 19.3344(6) _cell_angle_alpha 87.969(2) _cell_angle_beta 83.228(3) _cell_angle_gamma 72.600(3) _cell_volume 1625.09(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9217 _cell_measurement_theta_min 4.6023 _cell_measurement_theta_max 76.2259 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1206 _exptl_absorpt_coefficient_mu 7.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43031 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method 'CCD, \w scans' _diffrn_reflns_number 15175 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 76.41 _diffrn_reflns_theta_full 76.41 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _reflns_number_total 6705 _reflns_number_gt 5622 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0949P)^2^+0.5538P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6705 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1598 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.507 _refine_diff_density_min -0.718 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_group _atom_site_disorder_assembly Cr1 Cr 0.62102(6) 0.22483(5) 0.12428(2) 0.03756(16) Uani 1 d . . . Cr2 Cr 1.37776(5) 0.75610(5) 0.38427(2) 0.03709(16) Uani 1 d . . . Ca1 Ca 0.99923(6) 0.49171(6) 0.25365(3) 0.04273(18) Uani 1 d . . . O1 O 0.8222(2) 0.1630(2) 0.16534(11) 0.0429(5) Uani 1 d . . . O2 O 0.6537(3) 0.4111(2) 0.12741(12) 0.0473(5) Uani 1 d . . . O3 O 0.9764(3) 0.2559(2) 0.21862(14) 0.0539(6) Uani 1 d . . . O4 O 0.8065(3) 0.5163(2) 0.17275(15) 0.0583(7) Uani 1 d . . . O5 O 1.0593(3) 0.5605(3) 0.36827(12) 0.0515(6) Uani 1 d . . . O6 O 1.1579(3) 0.6510(3) 0.23943(11) 0.0515(6) Uani 1 d . . . O7 O 1.3109(3) 0.7462(2) 0.29198(11) 0.0446(5) Uani 1 d . . . O8 O 1.2090(3) 0.6700(2) 0.41455(10) 0.0434(5) Uani 1 d . . . O9 O 0.4103(3) 0.3113(2) 0.09384(11) 0.0452(5) Uani 1 d . . . O10 O 0.5018(3) 0.2449(2) 0.21671(10) 0.0450(5) Uani 1 d . . . O11 O 0.1661(3) 0.4274(3) 0.13903(12) 0.0509(5) Uani 1 d . . . O12 O 0.2577(3) 0.3360(3) 0.26886(11) 0.0518(6) Uani 1 d . . . O13 O 1.5319(3) 0.5682(2) 0.37594(13) 0.0491(5) Uani 1 d . . . O14 O 1.5585(3) 0.8165(2) 0.34009(12) 0.0454(5) Uani 1 d . . . O15 O 1.7780(3) 0.4607(2) 0.33028(15) 0.0536(6) Uani 1 d . . . O16 O 1.7981(3) 0.7209(2) 0.28329(15) 0.0545(6) Uani 1 d . . . O17 O 0.8982(8) 0.9567(6) 0.2785(4) 0.093(2) Uani 0.624(11) d P . . O18 O 1 0.5 0 0.188(15) Uani 0.41(2) d SP . . N1 N 0.6146(3) 0.0215(3) 0.11214(14) 0.0447(6) Uani 1 d . . . N2 N 0.7293(3) 0.1828(3) 0.02447(13) 0.0462(6) Uani 1 d . . . N3 N 1.2301(3) 0.9565(3) 0.40476(13) 0.0424(5) Uani 1 d . . . N4 N 1.4217(3) 0.7857(3) 0.48424(14) 0.0448(6) Uani 1 d . . . C1 C 0.8662(4) 0.2657(3) 0.18475(16) 0.0429(6) Uani 1 d . . . C2 C 0.7698(4) 0.4119(3) 0.16067(17) 0.0434(6) Uani 1 d . . . C3 C 1.2084(3) 0.6790(3) 0.29093(15) 0.0396(6) Uani 1 d . . . C4 C 1.1512(3) 0.6302(3) 0.36377(15) 0.0395(6) Uani 1 d . . . C5 C 0.5497(5) -0.0521(4) 0.1597(2) 0.0565(8) Uani 1 d . . . H5 H 0.5082 -0.0119 0.2031 0.068 Uiso 1 calc R . . C6 C 0.5422(6) -0.1854(5) 0.1466(2) 0.0692(11) Uani 1 d . . . H6 H 0.4952 -0.2337 0.1802 0.083 Uiso 1 calc R . . C7 C 0.6059(6) -0.2447(4) 0.0827(2) 0.0694(11) Uani 1 d . . . H7 H 0.6013 -0.3339 0.0722 0.083 Uiso 1 calc R . . C8 C 0.6760(5) -0.1720(4) 0.0346(2) 0.0633(10) Uani 1 d . . . H8 H 0.7212 -0.2125 -0.0085 0.076 Uiso 1 calc R . . C9 C 0.6800(4) -0.0376(3) 0.04977(17) 0.0452(7) Uani 1 d . . . C10 C 0.7483(4) 0.0505(4) 0.00097(17) 0.0473(7) Uani 1 d . . . C11 C 0.8243(6) 0.0102(5) -0.0643(2) 0.0708(12) Uani 1 d . . . H11 H 0.8391 -0.0808 -0.0799 0.085 Uiso 1 calc R . . C12 C 0.8788(7) 0.1034(6) -0.1066(2) 0.0884(17) Uani 1 d . . . H12 H 0.929 0.0764 -0.1511 0.106 Uiso 1 calc R . . C13 C 0.8583(7) 0.2366(6) -0.0827(2) 0.0847(15) Uani 1 d . . . H13 H 0.8948 0.3012 -0.1104 0.102 Uiso 1 calc R . . C14 C 0.7822(6) 0.2728(4) -0.0165(2) 0.0650(10) Uani 1 d . . . H14 H 0.7674 0.3632 -0.0001 0.078 Uiso 1 calc R . . C15 C 1.1338(4) 1.0355(4) 0.36100(18) 0.0547(8) Uani 1 d . . . H15 H 1.1378 1.002 0.3163 0.066 Uiso 1 calc R . . C16 C 1.0285(5) 1.1652(4) 0.3802(2) 0.0663(10) Uani 1 d . . . H16 H 0.9622 1.2177 0.349 0.08 Uiso 1 calc R . . C17 C 1.0230(6) 1.2153(4) 0.4457(2) 0.0733(12) Uani 1 d . . . H17 H 0.9524 1.302 0.4597 0.088 Uiso 1 calc R . . C18 C 1.1228(5) 1.1360(4) 0.4904(2) 0.0622(10) Uani 1 d . . . H18 H 1.1219 1.17 0.5347 0.075 Uiso 1 calc R . . C19 C 1.2258(4) 1.0049(3) 0.46977(16) 0.0430(6) Uani 1 d . . . C20 C 1.3357(4) 0.9109(3) 0.51352(15) 0.0434(7) Uani 1 d . . . C21 C 1.3538(6) 0.9438(5) 0.5802(2) 0.0648(10) Uani 1 d . . . H21 H 1.2929 1.0292 0.6003 0.078 Uiso 1 calc R . . C22 C 1.4630(7) 0.8488(5) 0.6167(2) 0.0775(14) Uani 1 d . . . H22 H 1.4777 0.8704 0.6613 0.093 Uiso 1 calc R . . C23 C 1.5491(7) 0.7233(5) 0.5868(2) 0.0773(14) Uani 1 d . . . H23 H 1.6228 0.6581 0.6109 0.093 Uiso 1 calc R . . C24 C 1.5256(5) 0.6939(4) 0.5202(2) 0.0613(10) Uani 1 d . . . H24 H 1.5838 0.6079 0.4999 0.074 Uiso 1 calc R . . C25 C 0.3015(4) 0.3563(3) 0.14436(15) 0.0403(6) Uani 1 d . . . C26 C 0.3548(4) 0.3109(3) 0.21719(15) 0.0409(6) Uani 1 d . . . C27 C 1.6638(4) 0.5658(3) 0.34285(17) 0.0419(6) Uani 1 d . . . C28 C 1.6777(4) 0.7133(3) 0.31887(16) 0.0418(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0399(3) 0.0421(3) 0.0299(3) -0.01455(19) -0.00377(18) -0.0095(2) Cr2 0.0356(3) 0.0406(3) 0.0351(3) -0.01470(19) -0.00381(18) -0.00979(19) Ca1 0.0354(3) 0.0508(3) 0.0434(4) -0.0140(3) -0.0061(2) -0.0126(3) O1 0.0410(11) 0.0391(10) 0.0468(12) -0.0129(9) -0.0073(9) -0.0068(8) O2 0.0499(12) 0.0410(10) 0.0509(13) -0.0098(9) -0.0203(10) -0.0067(9) O3 0.0477(12) 0.0503(12) 0.0634(15) -0.0105(11) -0.0213(11) -0.0074(10) O4 0.0596(14) 0.0428(11) 0.0784(18) -0.0096(11) -0.0303(13) -0.0145(10) O5 0.0524(13) 0.0722(15) 0.0383(11) -0.0120(10) 0.0004(9) -0.0323(12) O6 0.0579(13) 0.0711(15) 0.0346(11) -0.0080(10) -0.0100(9) -0.0302(12) O7 0.0476(11) 0.0577(12) 0.0332(10) -0.0134(9) 0.0002(8) -0.0232(10) O8 0.0440(11) 0.0574(12) 0.0312(10) -0.0132(9) -0.0025(8) -0.0182(9) O9 0.0435(11) 0.0606(12) 0.0308(10) -0.0152(9) -0.0071(8) -0.0115(9) O10 0.0435(11) 0.0579(12) 0.0282(10) -0.0113(9) -0.0073(8) -0.0046(9) O11 0.0429(12) 0.0647(14) 0.0415(12) -0.0085(10) -0.0118(9) -0.0067(10) O12 0.0406(11) 0.0737(15) 0.0343(11) -0.0088(10) -0.0023(9) -0.0064(10) O13 0.0418(11) 0.0408(10) 0.0629(14) -0.0141(10) 0.0049(10) -0.0120(9) O14 0.0426(11) 0.0376(10) 0.0564(13) -0.0147(9) -0.0035(9) -0.0119(8) O15 0.0388(11) 0.0404(11) 0.0758(17) -0.0098(11) 0.0015(10) -0.0051(9) O16 0.0442(12) 0.0478(12) 0.0728(16) -0.0094(11) 0.0045(11) -0.0185(10) O17 0.110(5) 0.069(3) 0.107(5) 0.002(3) -0.014(4) -0.037(3) O18 0.115(16) 0.31(4) 0.141(19) -0.08(2) -0.019(13) -0.050(19) N1 0.0493(14) 0.0458(13) 0.0395(13) -0.0115(10) -0.0089(10) -0.0123(11) N2 0.0533(15) 0.0522(14) 0.0299(12) -0.0095(10) 0.0020(10) -0.0123(12) N3 0.0468(13) 0.0453(13) 0.0330(12) -0.0103(10) -0.0026(10) -0.0102(11) N4 0.0559(15) 0.0441(13) 0.0391(13) -0.0051(10) -0.0148(11) -0.0178(12) C1 0.0389(14) 0.0440(14) 0.0432(16) -0.0116(12) -0.0059(12) -0.0067(12) C2 0.0425(15) 0.0418(14) 0.0426(16) -0.0119(12) -0.0094(12) -0.0045(12) C3 0.0382(14) 0.0482(14) 0.0332(13) -0.0138(11) -0.0018(11) -0.0133(12) C4 0.0357(13) 0.0476(15) 0.0335(14) -0.0114(11) -0.0024(10) -0.0091(11) C5 0.071(2) 0.0551(18) 0.0486(19) -0.0011(15) -0.0084(16) -0.0257(17) C6 0.080(3) 0.067(2) 0.071(3) 0.011(2) -0.023(2) -0.034(2) C7 0.091(3) 0.0487(18) 0.078(3) -0.0012(18) -0.036(2) -0.024(2) C8 0.083(3) 0.0510(18) 0.055(2) -0.0203(16) -0.0253(19) -0.0099(18) C9 0.0521(17) 0.0418(14) 0.0407(16) -0.0114(12) -0.0177(13) -0.0065(12) C10 0.0488(16) 0.0490(16) 0.0358(15) -0.0155(13) -0.0070(12) 0.0005(13) C11 0.083(3) 0.069(2) 0.0417(19) -0.0203(17) 0.0040(18) 0.004(2) C12 0.104(4) 0.096(3) 0.037(2) -0.009(2) 0.021(2) 0.003(3) C13 0.101(4) 0.086(3) 0.054(2) 0.011(2) 0.020(2) -0.019(3) C14 0.079(3) 0.062(2) 0.0463(19) -0.0057(16) 0.0073(18) -0.014(2) C15 0.0568(19) 0.0588(19) 0.0400(17) -0.0020(14) -0.0069(14) -0.0036(15) C16 0.063(2) 0.058(2) 0.062(2) 0.0049(17) 0.0007(18) 0.0037(17) C17 0.071(3) 0.055(2) 0.072(3) -0.0097(19) 0.019(2) 0.0048(18) C18 0.071(2) 0.0562(19) 0.051(2) -0.0211(16) 0.0137(17) -0.0121(18) C19 0.0482(16) 0.0470(15) 0.0324(14) -0.0119(12) 0.0066(12) -0.0152(13) C20 0.0575(17) 0.0493(15) 0.0295(13) -0.0087(12) -0.0036(12) -0.0246(14) C21 0.092(3) 0.072(2) 0.0425(19) -0.0137(17) -0.0096(18) -0.040(2) C22 0.125(4) 0.089(3) 0.044(2) 0.0031(19) -0.032(2) -0.062(3) C23 0.116(4) 0.074(3) 0.065(3) 0.025(2) -0.054(3) -0.049(3) C24 0.078(3) 0.0511(18) 0.064(2) 0.0037(16) -0.035(2) -0.0218(17) C25 0.0433(15) 0.0467(14) 0.0332(14) -0.0109(11) -0.0090(11) -0.0140(12) C26 0.0427(15) 0.0470(14) 0.0330(14) -0.0108(11) -0.0096(11) -0.0100(12) C27 0.0385(14) 0.0386(13) 0.0500(17) -0.0122(12) -0.0066(12) -0.0113(11) C28 0.0408(15) 0.0409(14) 0.0473(16) -0.0116(12) -0.0090(12) -0.0147(12) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 O10 1.953(2) . ? Cr1 O2 1.963(2) . ? Cr1 O1 1.967(2) . ? Cr1 O9 1.970(2) . ? Cr1 N2 2.051(2) . ? Cr1 N1 2.061(3) . ? Cr2 O13 1.960(2) . ? Cr2 O7 1.962(2) . ? Cr2 O8 1.967(2) . ? Cr2 O14 1.977(2) . ? Cr2 N3 2.056(3) . ? Cr2 N4 2.065(2) . ? Ca1 O12 2.407(2) 1_655 ? Ca1 O6 2.410(2) . ? Ca1 O4 2.412(2) . ? Ca1 O15 2.414(3) 1_455 ? Ca1 O16 2.479(2) 1_455 ? Ca1 O5 2.505(2) . ? Ca1 O11 2.508(2) 1_655 ? Ca1 O3 2.535(2) . ? Ca1 C26 3.154(3) 1_655 ? Ca1 C3 3.156(3) . ? Ca1 C2 3.161(3) . ? Ca1 C27 3.167(3) 1_455 ? O1 C1 1.281(4) . ? O2 C2 1.284(4) . ? O3 C1 1.223(4) . ? O4 C2 1.216(4) . ? O5 C4 1.216(4) . ? O6 C3 1.213(4) . ? O7 C3 1.286(4) . ? O8 C4 1.287(3) . ? O9 C25 1.282(4) . ? O10 C26 1.278(4) . ? O11 C25 1.217(4) . ? O11 Ca1 2.508(2) 1_455 ? O12 C26 1.223(4) . ? O12 Ca1 2.407(2) 1_455 ? O13 C27 1.265(4) . ? O14 C28 1.275(4) . ? O15 C27 1.230(4) . ? O15 Ca1 2.414(3) 1_655 ? O16 C28 1.226(4) . ? O16 Ca1 2.479(2) 1_655 ? N1 C5 1.340(5) . ? N1 C9 1.349(4) . ? N2 C14 1.328(5) . ? N2 C10 1.362(4) . ? N3 C15 1.339(4) . ? N3 C19 1.354(4) . ? N4 C24 1.332(5) . ? N4 C20 1.354(4) . ? C1 C2 1.539(4) . ? C3 C4 1.552(4) . ? C5 C6 1.380(5) . ? C5 H5 0.93 . ? C6 C7 1.372(7) . ? C6 H6 0.93 . ? C7 C8 1.366(7) . ? C7 H7 0.93 . ? C8 C9 1.390(5) . ? C8 H8 0.93 . ? C9 C10 1.468(5) . ? C10 C11 1.373(5) . ? C11 C12 1.373(7) . ? C11 H11 0.93 . ? C12 C13 1.371(8) . ? C12 H12 0.93 . ? C13 C14 1.382(6) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C16 1.382(5) . ? C15 H15 0.93 . ? C16 C17 1.368(6) . ? C16 H16 0.93 . ? C17 C18 1.369(7) . ? C17 H17 0.93 . ? C18 C19 1.392(5) . ? C18 H18 0.93 . ? C19 C20 1.464(5) . ? C20 C21 1.380(4) . ? C21 C22 1.380(7) . ? C21 H21 0.93 . ? C22 C23 1.362(7) . ? C22 H22 0.93 . ? C23 C24 1.384(6) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C26 1.549(4) . ? C25 Ca1 3.199(3) 1_455 ? C26 Ca1 3.154(3) 1_455 ? C27 C28 1.558(4) . ? C27 Ca1 3.167(3) 1_655 ? C28 Ca1 3.200(3) 1_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 O10 Cr1 O2 93.49(10) . . ? O10 Cr1 O1 90.97(9) . . ? O2 Cr1 O1 83.10(9) . . ? O10 Cr1 O9 83.10(9) . . ? O2 Cr1 O9 90.43(10) . . ? O1 Cr1 O9 170.96(8) . . ? O10 Cr1 N2 171.59(11) . . ? O2 Cr1 N2 94.23(11) . . ? O1 Cr1 N2 93.27(11) . . ? O9 Cr1 N2 93.50(10) . . ? O10 Cr1 N1 93.34(11) . . ? O2 Cr1 N1 172.30(11) . . ? O1 Cr1 N1 93.22(10) . . ? O9 Cr1 N1 93.93(10) . . ? N2 Cr1 N1 79.19(11) . . ? O13 Cr2 O7 93.22(10) . . ? O13 Cr2 O8 89.83(9) . . ? O7 Cr2 O8 83.12(9) . . ? O13 Cr2 O14 83.11(9) . . ? O7 Cr2 O14 89.49(9) . . ? O8 Cr2 O14 169.49(8) . . ? O13 Cr2 N3 172.20(10) . . ? O7 Cr2 N3 94.44(10) . . ? O8 Cr2 N3 92.58(10) . . ? O14 Cr2 N3 95.45(10) . . ? O13 Cr2 N4 93.46(11) . . ? O7 Cr2 N4 172.88(10) . . ? O8 Cr2 N4 94.42(10) . . ? O14 Cr2 N4 93.77(10) . . ? N3 Cr2 N4 78.96(11) . . ? O12 Ca1 O6 78.32(9) 1_655 . ? O12 Ca1 O4 136.84(8) 1_655 . ? O6 Ca1 O4 116.83(9) . . ? O12 Ca1 O15 117.55(9) 1_655 1_455 ? O6 Ca1 O15 138.51(8) . 1_455 ? O4 Ca1 O15 79.03(10) . 1_455 ? O12 Ca1 O16 147.11(9) 1_655 1_455 ? O6 Ca1 O16 78.53(8) . 1_455 ? O4 Ca1 O16 75.10(9) . 1_455 ? O15 Ca1 O16 68.66(8) 1_455 1_455 ? O12 Ca1 O5 75.01(8) 1_655 . ? O6 Ca1 O5 68.15(8) . . ? O4 Ca1 O5 147.59(9) . . ? O15 Ca1 O5 79.02(8) 1_455 . ? O16 Ca1 O5 74.84(9) 1_455 . ? O12 Ca1 O11 68.57(8) 1_655 1_655 ? O6 Ca1 O11 74.62(8) . 1_655 ? O4 Ca1 O11 76.83(9) . 1_655 ? O15 Ca1 O11 145.99(8) 1_455 1_655 ? O16 Ca1 O11 126.11(9) 1_455 1_655 ? O5 Ca1 O11 132.00(8) . 1_655 ? O12 Ca1 O3 78.08(8) 1_655 . ? O6 Ca1 O3 145.35(9) . . ? O4 Ca1 O3 67.64(8) . . ? O15 Ca1 O3 75.53(8) 1_455 . ? O16 Ca1 O3 132.15(8) 1_455 . ? O5 Ca1 O3 128.21(9) . . ? O11 Ca1 O3 73.32(9) 1_655 . ? O12 Ca1 C26 20.25(8) 1_655 1_655 ? O6 Ca1 C26 72.08(9) . 1_655 ? O4 Ca1 C26 121.59(8) . 1_655 ? O15 Ca1 C26 134.68(9) 1_455 1_655 ? O16 Ca1 C26 150.39(8) 1_455 1_655 ? O5 Ca1 C26 90.75(8) . 1_655 ? O11 Ca1 C26 48.58(7) 1_655 1_655 ? O3 Ca1 C26 77.03(8) . 1_655 ? O12 Ca1 C3 72.44(9) 1_655 . ? O6 Ca1 C3 19.98(8) . . ? O4 Ca1 C3 134.01(9) . . ? O15 Ca1 C3 123.56(8) 1_455 . ? O16 Ca1 C3 77.84(8) 1_455 . ? O5 Ca1 C3 48.40(8) . . ? O11 Ca1 C3 90.44(8) 1_655 . ? O3 Ca1 C3 149.96(8) . . ? C26 Ca1 C3 73.35(8) 1_655 . ? O12 Ca1 C2 122.51(8) 1_655 . ? O6 Ca1 C2 134.02(9) . . ? O4 Ca1 C2 19.98(8) . . ? O15 Ca1 C2 72.32(9) 1_455 . ? O16 Ca1 C2 90.38(8) 1_455 . ? O5 Ca1 C2 150.99(8) . . ? O11 Ca1 C2 76.85(8) 1_655 . ? O3 Ca1 C2 48.08(8) . . ? C26 Ca1 C2 112.55(7) 1_655 . ? C3 Ca1 C2 152.95(9) . . ? O12 Ca1 C27 134.72(9) 1_655 1_455 ? O6 Ca1 C27 123.18(8) . 1_455 ? O4 Ca1 C27 73.21(9) . 1_455 ? O15 Ca1 C27 20.25(8) 1_455 1_455 ? O16 Ca1 C27 48.60(8) 1_455 1_455 ? O5 Ca1 C27 77.96(8) . 1_455 ? O11 Ca1 C27 149.76(8) 1_655 1_455 ? O3 Ca1 C27 91.40(8) . 1_455 ? C26 Ca1 C27 153.82(9) 1_655 1_455 ? C3 Ca1 C27 113.39(7) . 1_455 ? C2 Ca1 C27 73.61(8) . 1_455 ? C1 O1 Cr1 113.10(19) . . ? C2 O2 Cr1 113.4(2) . . ? C1 O3 Ca1 113.7(2) . . ? C2 O4 Ca1 117.4(2) . . ? C4 O5 Ca1 114.4(2) . . ? C3 O6 Ca1 117.3(2) . . ? C3 O7 Cr2 114.1(2) . . ? C4 O8 Cr2 113.54(19) . . ? C25 O9 Cr1 113.46(18) . . ? C26 O10 Cr1 114.11(19) . . ? C25 O11 Ca1 113.8(2) . 1_455 ? C26 O12 Ca1 116.8(2) . 1_455 ? C27 O13 Cr2 114.2(2) . . ? C28 O14 Cr2 112.96(19) . . ? C27 O15 Ca1 117.0(2) . 1_655 ? C28 O16 Ca1 115.2(2) . 1_655 ? C5 N1 C9 119.3(3) . . ? C5 N1 Cr1 125.6(2) . . ? C9 N1 Cr1 115.1(2) . . ? C14 N2 C10 119.6(3) . . ? C14 N2 Cr1 125.0(2) . . ? C10 N2 Cr1 115.3(2) . . ? C15 N3 C19 119.4(3) . . ? C15 N3 Cr2 125.1(2) . . ? C19 N3 Cr2 115.4(2) . . ? C24 N4 C20 119.5(3) . . ? C24 N4 Cr2 125.6(2) . . ? C20 N4 Cr2 115.0(2) . . ? O3 C1 O1 125.9(3) . . ? O3 C1 C2 119.5(3) . . ? O1 C1 C2 114.6(3) . . ? O3 C1 Ca1 46.01(16) . . ? O1 C1 Ca1 170.9(2) . . ? C2 C1 Ca1 73.72(16) . . ? O4 C2 O2 125.1(3) . . ? O4 C2 C1 120.4(3) . . ? O2 C2 C1 114.5(3) . . ? O4 C2 Ca1 42.66(16) . . ? O2 C2 Ca1 165.3(2) . . ? C1 C2 Ca1 78.43(16) . . ? O6 C3 O7 125.9(3) . . ? O6 C3 C4 120.0(3) . . ? O7 C3 C4 114.0(2) . . ? O6 C3 Ca1 42.76(16) . . ? O7 C3 Ca1 166.6(2) . . ? C4 C3 Ca1 77.66(15) . . ? O5 C4 O8 126.4(3) . . ? O5 C4 C3 119.3(2) . . ? O8 C4 C3 114.3(3) . . ? O5 C4 Ca1 45.35(15) . . ? O8 C4 Ca1 170.9(2) . . ? C3 C4 Ca1 74.11(14) . . ? N1 C5 C6 122.5(4) . . ? N1 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C7 C6 C5 118.4(4) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? N1 C9 C8 120.1(3) . . ? N1 C9 C10 115.6(3) . . ? C8 C9 C10 124.3(3) . . ? N2 C10 C11 119.9(4) . . ? N2 C10 C9 114.7(3) . . ? C11 C10 C9 125.3(3) . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 118.5(4) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? N2 C14 C13 122.2(4) . . ? N2 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? N3 C15 C16 122.0(3) . . ? N3 C15 H15 119 . . ? C16 C15 H15 119 . . ? C17 C16 C15 119.2(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? N3 C19 C18 120.1(3) . . ? N3 C19 C20 115.1(3) . . ? C18 C19 C20 124.8(3) . . ? N4 C20 C21 120.8(3) . . ? N4 C20 C19 115.4(2) . . ? C21 C20 C19 123.8(3) . . ? C22 C21 C20 119.4(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 119.5(4) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.2(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? N4 C24 C23 121.7(4) . . ? N4 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? O11 C25 O9 126.0(3) . . ? O11 C25 C26 120.1(3) . . ? O9 C25 C26 114.0(3) . . ? O11 C25 Ca1 45.83(16) . 1_455 ? O9 C25 Ca1 171.8(2) . 1_455 ? C26 C25 Ca1 74.26(16) . 1_455 ? O12 C26 O10 125.6(3) . . ? O12 C26 C25 119.8(3) . . ? O10 C26 C25 114.5(3) . . ? O12 C26 Ca1 42.93(16) . 1_455 ? O10 C26 Ca1 166.80(19) . 1_455 ? C25 C26 Ca1 77.53(16) . 1_455 ? O15 C27 O13 126.2(3) . . ? O15 C27 C28 119.3(3) . . ? O13 C27 C28 114.5(3) . . ? O15 C27 Ca1 42.80(16) . 1_655 ? O13 C27 Ca1 167.7(2) . 1_655 ? C28 C27 Ca1 77.01(16) . 1_655 ? O16 C28 O14 126.4(3) . . ? O16 C28 C27 119.1(3) . . ? O14 C28 C27 114.4(3) . . ? O16 C28 Ca1 44.48(15) . 1_655 ? O14 C28 Ca1 170.9(2) . 1_655 ? C27 C28 Ca1 74.67(16) . 1_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 O10 Cr1 O1 C1 -83.2(2) . . . . ? O2 Cr1 O1 C1 10.2(2) . . . . ? O9 Cr1 O1 C1 -34.3(8) . . . . ? N2 Cr1 O1 C1 104.1(2) . . . . ? N1 Cr1 O1 C1 -176.6(2) . . . . ? O10 Cr1 O2 C2 82.2(2) . . . . ? O1 Cr1 O2 C2 -8.4(2) . . . . ? O9 Cr1 O2 C2 165.3(2) . . . . ? N2 Cr1 O2 C2 -101.1(2) . . . . ? N1 Cr1 O2 C2 -70.1(8) . . . . ? O12 Ca1 O3 C1 -162.0(3) 1_655 . . . ? O6 Ca1 O3 C1 -114.0(3) . . . . ? O4 Ca1 O3 C1 -8.7(2) . . . . ? O15 Ca1 O3 C1 75.2(2) 1_455 . . . ? O16 Ca1 O3 C1 32.9(3) 1_455 . . . ? O5 Ca1 O3 C1 138.2(2) . . . . ? O11 Ca1 O3 C1 -91.0(3) 1_655 . . . ? C26 Ca1 O3 C1 -141.3(3) 1_655 . . . ? C3 Ca1 O3 C1 -150.9(2) . . . . ? C2 Ca1 O3 C1 -3.9(2) . . . . ? C27 Ca1 O3 C1 62.5(3) 1_455 . . . ? O12 Ca1 O4 C2 50.7(3) 1_655 . . . ? O6 Ca1 O4 C2 152.7(3) . . . . ? O15 Ca1 O4 C2 -68.2(3) 1_455 . . . ? O16 Ca1 O4 C2 -138.8(3) 1_455 . . . ? O5 Ca1 O4 C2 -116.3(3) . . . . ? O11 Ca1 O4 C2 87.7(3) 1_655 . . . ? O3 Ca1 O4 C2 10.6(3) . . . . ? C26 Ca1 O4 C2 68.0(3) 1_655 . . . ? C3 Ca1 O4 C2 165.3(2) . . . . ? C27 Ca1 O4 C2 -88.1(3) 1_455 . . . ? O12 Ca1 O5 C4 76.7(2) 1_655 . . . ? O6 Ca1 O5 C4 -6.5(2) . . . . ? O4 Ca1 O5 C4 -112.5(2) . . . . ? O15 Ca1 O5 C4 -160.7(2) 1_455 . . . ? O16 Ca1 O5 C4 -90.0(2) 1_455 . . . ? O11 Ca1 O5 C4 35.3(3) 1_655 . . . ? O3 Ca1 O5 C4 137.8(2) . . . . ? C26 Ca1 O5 C4 63.8(2) 1_655 . . . ? C3 Ca1 O5 C4 -3.0(2) . . . . ? C2 Ca1 O5 C4 -151.7(2) . . . . ? C27 Ca1 O5 C4 -140.0(2) 1_455 . . . ? O12 Ca1 O6 C3 -70.5(2) 1_655 . . . ? O4 Ca1 O6 C3 152.6(2) . . . . ? O15 Ca1 O6 C3 48.1(3) 1_455 . . . ? O16 Ca1 O6 C3 85.9(2) 1_455 . . . ? O5 Ca1 O6 C3 7.8(2) . . . . ? O11 Ca1 O6 C3 -141.3(3) 1_655 . . . ? O3 Ca1 O6 C3 -118.5(2) . . . . ? C26 Ca1 O6 C3 -90.5(2) 1_655 . . . ? C2 Ca1 O6 C3 165.2(2) . . . . ? C27 Ca1 O6 C3 65.8(3) 1_455 . . . ? O13 Cr2 O7 C3 82.3(2) . . . . ? O8 Cr2 O7 C3 -7.1(2) . . . . ? O14 Cr2 O7 C3 165.4(2) . . . . ? N3 Cr2 O7 C3 -99.2(2) . . . . ? N4 Cr2 O7 C3 -77.3(9) . . . . ? O13 Cr2 O8 C4 -84.3(2) . . . . ? O7 Cr2 O8 C4 8.9(2) . . . . ? O14 Cr2 O8 C4 -36.7(6) . . . . ? N3 Cr2 O8 C4 103.1(2) . . . . ? N4 Cr2 O8 C4 -177.8(2) . . . . ? O10 Cr1 O9 C25 8.6(2) . . . . ? O2 Cr1 O9 C25 -84.9(2) . . . . ? O1 Cr1 O9 C25 -40.7(8) . . . . ? N2 Cr1 O9 C25 -179.2(2) . . . . ? N1 Cr1 O9 C25 101.5(2) . . . . ? O2 Cr1 O10 C26 84.5(2) . . . . ? O1 Cr1 O10 C26 167.6(2) . . . . ? O9 Cr1 O10 C26 -5.6(2) . . . . ? N2 Cr1 O10 C26 -72.1(8) . . . . ? N1 Cr1 O10 C26 -99.1(2) . . . . ? O7 Cr2 O13 C27 83.1(2) . . . . ? O8 Cr2 O13 C27 166.2(2) . . . . ? O14 Cr2 O13 C27 -6.0(2) . . . . ? N3 Cr2 O13 C27 -85.8(8) . . . . ? N4 Cr2 O13 C27 -99.3(2) . . . . ? O13 Cr2 O14 C28 8.6(2) . . . . ? O7 Cr2 O14 C28 -84.7(2) . . . . ? O8 Cr2 O14 C28 -39.5(6) . . . . ? N3 Cr2 O14 C28 -179.1(2) . . . . ? N4 Cr2 O14 C28 101.7(2) . . . . ? O10 Cr1 N1 C5 -2.2(3) . . . . ? O2 Cr1 N1 C5 150.1(7) . . . . ? O1 Cr1 N1 C5 88.9(3) . . . . ? O9 Cr1 N1 C5 -85.5(3) . . . . ? N2 Cr1 N1 C5 -178.4(3) . . . . ? O10 Cr1 N1 C9 176.5(2) . . . . ? O2 Cr1 N1 C9 -31.2(9) . . . . ? O1 Cr1 N1 C9 -92.4(2) . . . . ? O9 Cr1 N1 C9 93.2(2) . . . . ? N2 Cr1 N1 C9 0.3(2) . . . . ? O10 Cr1 N2 C14 151.5(6) . . . . ? O2 Cr1 N2 C14 -5.0(3) . . . . ? O1 Cr1 N2 C14 -88.3(3) . . . . ? O9 Cr1 N2 C14 85.7(3) . . . . ? N1 Cr1 N2 C14 179.1(4) . . . . ? O10 Cr1 N2 C10 -29.5(9) . . . . ? O2 Cr1 N2 C10 174.0(2) . . . . ? O1 Cr1 N2 C10 90.6(2) . . . . ? O9 Cr1 N2 C10 -95.4(2) . . . . ? N1 Cr1 N2 C10 -2.0(2) . . . . ? O13 Cr2 N3 C15 167.4(7) . . . . ? O7 Cr2 N3 C15 -1.5(3) . . . . ? O8 Cr2 N3 C15 -84.8(3) . . . . ? O14 Cr2 N3 C15 88.4(3) . . . . ? N4 Cr2 N3 C15 -178.8(3) . . . . ? O13 Cr2 N3 C19 -17.2(9) . . . . ? O7 Cr2 N3 C19 173.9(2) . . . . ? O8 Cr2 N3 C19 90.6(2) . . . . ? O14 Cr2 N3 C19 -96.2(2) . . . . ? N4 Cr2 N3 C19 -3.4(2) . . . . ? O13 Cr2 N4 C24 0.3(3) . . . . ? O7 Cr2 N4 C24 159.9(7) . . . . ? O8 Cr2 N4 C24 90.4(3) . . . . ? O14 Cr2 N4 C24 -83.0(3) . . . . ? N3 Cr2 N4 C24 -177.8(3) . . . . ? O13 Cr2 N4 C20 179.9(2) . . . . ? O7 Cr2 N4 C20 -20.5(10) . . . . ? O8 Cr2 N4 C20 -90.0(2) . . . . ? O14 Cr2 N4 C20 96.6(2) . . . . ? N3 Cr2 N4 C20 1.8(2) . . . . ? Ca1 O3 C1 O1 -174.4(3) . . . . ? Ca1 O3 C1 C2 6.8(4) . . . . ? Cr1 O1 C1 O3 171.2(3) . . . . ? Cr1 O1 C1 C2 -10.0(3) . . . . ? Cr1 O1 C1 Ca1 145.2(13) . . . . ? O12 Ca1 C1 O3 17.8(3) 1_655 . . . ? O6 Ca1 C1 O3 97.5(3) . . . . ? O4 Ca1 C1 O3 169.1(3) . . . . ? O15 Ca1 C1 O3 -98.9(3) 1_455 . . . ? O16 Ca1 C1 O3 -153.7(2) 1_455 . . . ? O5 Ca1 C1 O3 -57.4(3) . . . . ? O11 Ca1 C1 O3 83.1(2) 1_655 . . . ? C26 Ca1 C1 O3 37.6(3) 1_655 . . . ? C3 Ca1 C1 O3 65.8(4) . . . . ? C2 Ca1 C1 O3 173.8(4) . . . . ? C27 Ca1 C1 O3 -116.5(3) 1_455 . . . ? O12 Ca1 C1 O1 47.4(14) 1_655 . . . ? O6 Ca1 C1 O1 127.1(13) . . . . ? O4 Ca1 C1 O1 -161.4(14) . . . . ? O15 Ca1 C1 O1 -69.3(13) 1_455 . . . ? O16 Ca1 C1 O1 -124.2(13) 1_455 . . . ? O5 Ca1 C1 O1 -27.8(14) . . . . ? O11 Ca1 C1 O1 112.7(14) 1_655 . . . ? O3 Ca1 C1 O1 29.6(12) . . . . ? C26 Ca1 C1 O1 67.2(14) 1_655 . . . ? C3 Ca1 C1 O1 95.3(14) . . . . ? C2 Ca1 C1 O1 -156.6(15) . . . . ? C27 Ca1 C1 O1 -86.9(14) 1_455 . . . ? O12 Ca1 C1 C2 -156.01(18) 1_655 . . . ? O6 Ca1 C1 C2 -76.3(2) . . . . ? O4 Ca1 C1 C2 -4.74(18) . . . . ? O15 Ca1 C1 C2 87.35(18) 1_455 . . . ? O16 Ca1 C1 C2 32.5(2) 1_455 . . . ? O5 Ca1 C1 C2 128.79(19) . . . . ? O11 Ca1 C1 C2 -90.68(18) 1_655 . . . ? O3 Ca1 C1 C2 -173.8(4) . . . . ? C26 Ca1 C1 C2 -136.15(18) 1_655 . . . ? C3 Ca1 C1 C2 -108.0(3) . . . . ? C27 Ca1 C1 C2 69.70(18) 1_455 . . . ? Ca1 O4 C2 O2 169.2(3) . . . . ? Ca1 O4 C2 C1 -11.7(4) . . . . ? Cr1 O2 C2 O4 -175.6(3) . . . . ? Cr1 O2 C2 C1 5.3(4) . . . . ? Cr1 O2 C2 Ca1 -145.6(9) . . . . ? O3 C1 C2 O4 2.9(5) . . . . ? O1 C1 C2 O4 -175.9(3) . . . . ? Ca1 C1 C2 O4 8.1(3) . . . . ? O3 C1 C2 O2 -177.9(3) . . . . ? O1 C1 C2 O2 3.3(4) . . . . ? Ca1 C1 C2 O2 -172.8(3) . . . . ? O3 C1 C2 Ca1 -5.1(3) . . . . ? O1 C1 C2 Ca1 176.0(3) . . . . ? O12 Ca1 C2 O4 -141.1(3) 1_655 . . . ? O6 Ca1 C2 O4 -34.8(3) . . . . ? O15 Ca1 C2 O4 107.0(3) 1_455 . . . ? O16 Ca1 C2 O4 39.6(3) 1_455 . . . ? O5 Ca1 C2 O4 97.7(3) . . . . ? O11 Ca1 C2 O4 -87.6(3) 1_655 . . . ? O3 Ca1 C2 O4 -166.8(3) . . . . ? C26 Ca1 C2 O4 -121.2(3) 1_655 . . . ? C3 Ca1 C2 O4 -23.7(4) . . . . ? C27 Ca1 C2 O4 85.8(3) 1_455 . . . ? O12 Ca1 C2 O2 -178.3(10) 1_655 . . . ? O6 Ca1 C2 O2 -71.9(10) . . . . ? O4 Ca1 C2 O2 -37.2(9) . . . . ? O15 Ca1 C2 O2 69.8(10) 1_455 . . . ? O16 Ca1 C2 O2 2.4(10) 1_455 . . . ? O5 Ca1 C2 O2 60.6(11) . . . . ? O11 Ca1 C2 O2 -124.7(10) 1_655 . . . ? O3 Ca1 C2 O2 156.0(10) . . . . ? C26 Ca1 C2 O2 -158.4(10) 1_655 . . . ? C3 Ca1 C2 O2 -60.9(11) . . . . ? C27 Ca1 C2 O2 48.7(10) 1_455 . . . ? O12 Ca1 C2 C1 28.6(2) 1_655 . . . ? O6 Ca1 C2 C1 134.94(18) . . . . ? O4 Ca1 C2 C1 169.7(4) . . . . ? O15 Ca1 C2 C1 -83.31(18) 1_455 . . . ? O16 Ca1 C2 C1 -150.73(18) 1_455 . . . ? O5 Ca1 C2 C1 -92.6(2) . . . . ? O11 Ca1 C2 C1 82.14(18) 1_655 . . . ? O3 Ca1 C2 C1 2.89(16) . . . . ? C26 Ca1 C2 C1 48.5(2) 1_655 . . . ? C3 Ca1 C2 C1 146.03(19) . . . . ? C27 Ca1 C2 C1 -104.46(19) 1_455 . . . ? Ca1 O6 C3 O7 170.3(2) . . . . ? Ca1 O6 C3 C4 -8.6(4) . . . . ? Cr2 O7 C3 O6 -174.7(3) . . . . ? Cr2 O7 C3 C4 4.3(3) . . . . ? Cr2 O7 C3 Ca1 -145.1(9) . . . . ? O12 Ca1 C3 O6 104.4(2) 1_655 . . . ? O4 Ca1 C3 O6 -34.9(3) . . . . ? O15 Ca1 C3 O6 -143.7(2) 1_455 . . . ? O16 Ca1 C3 O6 -89.8(3) 1_455 . . . ? O5 Ca1 C3 O6 -170.3(3) . . . . ? O11 Ca1 C3 O6 37.1(2) 1_655 . . . ? O3 Ca1 C3 O6 93.0(3) . . . . ? C26 Ca1 C3 O6 83.3(2) 1_655 . . . ? C2 Ca1 C3 O6 -23.9(3) . . . . ? C27 Ca1 C3 O6 -123.7(2) 1_455 . . . ? O12 Ca1 C3 O7 68.4(10) 1_655 . . . ? O6 Ca1 C3 O7 -36.0(9) . . . . ? O4 Ca1 C3 O7 -70.9(10) . . . . ? O15 Ca1 C3 O7 -179.8(10) 1_455 . . . ? O16 Ca1 C3 O7 -125.9(10) 1_455 . . . ? O5 Ca1 C3 O7 153.7(10) . . . . ? O11 Ca1 C3 O7 1.1(10) 1_655 . . . ? O3 Ca1 C3 O7 57.0(11) . . . . ? C26 Ca1 C3 O7 47.2(10) 1_655 . . . ? C2 Ca1 C3 O7 -59.9(10) . . . . ? C27 Ca1 C3 O7 -159.8(10) 1_455 . . . ? O12 Ca1 C3 C4 -83.15(16) 1_655 . . . ? O6 Ca1 C3 C4 172.4(3) . . . . ? O4 Ca1 C3 C4 137.56(17) . . . . ? O15 Ca1 C3 C4 28.70(19) 1_455 . . . ? O16 Ca1 C3 C4 82.57(16) 1_455 . . . ? O5 Ca1 C3 C4 2.16(15) . . . . ? O11 Ca1 C3 C4 -150.47(16) 1_655 . . . ? O3 Ca1 C3 C4 -94.5(2) . . . . ? C26 Ca1 C3 C4 -104.33(17) 1_655 . . . ? C2 Ca1 C3 C4 148.55(18) . . . . ? C27 Ca1 C3 C4 48.70(18) 1_455 . . . ? Ca1 O5 C4 O8 -174.9(2) . . . . ? Ca1 O5 C4 C3 5.2(4) . . . . ? Cr2 O8 C4 O5 171.1(3) . . . . ? Cr2 O8 C4 C3 -8.9(3) . . . . ? Cr2 O8 C4 Ca1 147.6(12) . . . . ? O6 C3 C4 O5 2.1(5) . . . . ? O7 C3 C4 O5 -176.9(3) . . . . ? Ca1 C3 C4 O5 -3.8(3) . . . . ? O6 C3 C4 O8 -177.8(3) . . . . ? O7 C3 C4 O8 3.2(4) . . . . ? Ca1 C3 C4 O8 176.2(2) . . . . ? O6 C3 C4 Ca1 5.9(3) . . . . ? O7 C3 C4 Ca1 -173.0(3) . . . . ? O12 Ca1 C4 O5 -97.3(2) 1_655 . . . ? O6 Ca1 C4 O5 171.8(3) . . . . ? O4 Ca1 C4 O5 101.3(3) . . . . ? O15 Ca1 C4 O5 19.2(2) 1_455 . . . ? O16 Ca1 C4 O5 84.6(2) 1_455 . . . ? O11 Ca1 C4 O5 -151.8(2) 1_655 . . . ? O3 Ca1 C4 O5 -57.8(3) . . . . ? C26 Ca1 C4 O5 -115.0(2) 1_655 . . . ? C3 Ca1 C4 O5 175.3(3) . . . . ? C2 Ca1 C4 O5 66.8(5) . . . . ? C27 Ca1 C4 O5 39.0(2) 1_455 . . . ? O12 Ca1 C4 O8 -70.4(13) 1_655 . . . ? O6 Ca1 C4 O8 -161.3(13) . . . . ? O4 Ca1 C4 O8 128.2(12) . . . . ? O15 Ca1 C4 O8 46.1(13) 1_455 . . . ? O16 Ca1 C4 O8 111.5(13) 1_455 . . . ? O5 Ca1 C4 O8 26.9(12) . . . . ? O11 Ca1 C4 O8 -124.9(12) 1_655 . . . ? O3 Ca1 C4 O8 -30.9(13) . . . . ? C26 Ca1 C4 O8 -88.1(13) 1_655 . . . ? C3 Ca1 C4 O8 -157.8(13) . . . . ? C2 Ca1 C4 O8 93.7(13) . . . . ? C27 Ca1 C4 O8 65.9(13) 1_455 . . . ? O12 Ca1 C4 C3 87.42(16) 1_655 . . . ? O6 Ca1 C4 C3 -3.47(16) . . . . ? O4 Ca1 C4 C3 -74.0(2) . . . . ? O15 Ca1 C4 C3 -156.16(16) 1_455 . . . ? O16 Ca1 C4 C3 -90.69(16) 1_455 . . . ? O5 Ca1 C4 C3 -175.3(3) . . . . ? O11 Ca1 C4 C3 32.86(18) 1_655 . . . ? O3 Ca1 C4 C3 126.89(18) . . . . ? C26 Ca1 C4 C3 69.64(16) 1_655 . . . ? C2 Ca1 C4 C3 -108.5(4) . . . . ? C27 Ca1 C4 C3 -136.30(16) 1_455 . . . ? C9 N1 C5 C6 -2.2(6) . . . . ? Cr1 N1 C5 C6 176.4(3) . . . . ? N1 C5 C6 C7 0.9(6) . . . . ? C5 C6 C7 C8 0.8(7) . . . . ? C6 C7 C8 C9 -1.3(6) . . . . ? C5 N1 C9 C8 1.7(5) . . . . ? Cr1 N1 C9 C8 -177.1(3) . . . . ? C5 N1 C9 C10 -180.0(3) . . . . ? Cr1 N1 C9 C10 1.3(4) . . . . ? C7 C8 C9 N1 0.0(6) . . . . ? C7 C8 C9 C10 -178.2(4) . . . . ? C14 N2 C10 C11 1.2(6) . . . . ? Cr1 N2 C10 C11 -177.8(3) . . . . ? C14 N2 C10 C9 -177.8(3) . . . . ? Cr1 N2 C10 C9 3.2(4) . . . . ? N1 C9 C10 N2 -3.0(4) . . . . ? C8 C9 C10 N2 175.3(3) . . . . ? N1 C9 C10 C11 178.1(4) . . . . ? C8 C9 C10 C11 -3.6(6) . . . . ? N2 C10 C11 C12 -1.3(7) . . . . ? C9 C10 C11 C12 177.6(4) . . . . ? C10 C11 C12 C13 0.9(8) . . . . ? C11 C12 C13 C14 -0.4(9) . . . . ? C10 N2 C14 C13 -0.8(7) . . . . ? Cr1 N2 C14 C13 178.1(4) . . . . ? C12 C13 C14 N2 0.3(9) . . . . ? C19 N3 C15 C16 -0.5(6) . . . . ? Cr2 N3 C15 C16 174.8(3) . . . . ? N3 C15 C16 C17 0.5(7) . . . . ? C15 C16 C17 C18 0.5(7) . . . . ? C16 C17 C18 C19 -1.5(7) . . . . ? C15 N3 C19 C18 -0.5(5) . . . . ? Cr2 N3 C19 C18 -176.2(3) . . . . ? C15 N3 C19 C20 -180.0(3) . . . . ? Cr2 N3 C19 C20 4.3(4) . . . . ? C17 C18 C19 N3 1.5(6) . . . . ? C17 C18 C19 C20 -179.1(4) . . . . ? C24 N4 C20 C21 -0.4(5) . . . . ? Cr2 N4 C20 C21 180.0(3) . . . . ? C24 N4 C20 C19 179.6(3) . . . . ? Cr2 N4 C20 C19 -0.1(4) . . . . ? N3 C19 C20 N4 -2.8(4) . . . . ? C18 C19 C20 N4 177.8(3) . . . . ? N3 C19 C20 C21 177.1(3) . . . . ? C18 C19 C20 C21 -2.3(6) . . . . ? N4 C20 C21 C22 1.2(6) . . . . ? C19 C20 C21 C22 -178.8(4) . . . . ? C20 C21 C22 C23 -1.1(7) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C20 N4 C24 C23 -0.5(6) . . . . ? Cr2 N4 C24 C23 179.1(3) . . . . ? C22 C23 C24 N4 0.5(7) . . . . ? Ca1 O11 C25 O9 -179.2(2) 1_455 . . . ? Ca1 O11 C25 C26 1.5(3) 1_455 . . . ? Cr1 O9 C25 O11 171.1(3) . . . . ? Cr1 O9 C25 C26 -9.5(3) . . . . ? Cr1 O9 C25 Ca1 167.0(14) . . . 1_455 ? Ca1 O12 C26 O10 171.3(2) 1_455 . . . ? Ca1 O12 C26 C25 -10.8(4) 1_455 . . . ? Cr1 O10 C26 O12 -180.0(3) . . . . ? Cr1 O10 C26 C25 2.0(3) . . . . ? Cr1 O10 C26 Ca1 -153.1(9) . . . 1_455 ? O11 C25 C26 O12 6.4(5) . . . . ? O9 C25 C26 O12 -173.0(3) . . . . ? Ca1 C25 C26 O12 7.5(3) 1_455 . . . ? O11 C25 C26 O10 -175.5(3) . . . . ? O9 C25 C26 O10 5.1(4) . . . . ? Ca1 C25 C26 O10 -174.4(3) 1_455 . . . ? O11 C25 C26 Ca1 -1.1(3) . . . 1_455 ? O9 C25 C26 Ca1 179.5(2) . . . 1_455 ? Ca1 O15 C27 O13 172.7(2) 1_655 . . . ? Ca1 O15 C27 C28 -9.3(4) 1_655 . . . ? Cr2 O13 C27 O15 -179.2(3) . . . . ? Cr2 O13 C27 C28 2.6(3) . . . . ? Cr2 O13 C27 Ca1 -155.2(10) . . . 1_655 ? Ca1 O16 C28 O14 -179.7(2) 1_655 . . . ? Ca1 O16 C28 C27 1.3(4) 1_655 . . . ? Cr2 O14 C28 O16 171.6(3) . . . . ? Cr2 O14 C28 C27 -9.3(3) . . . . ? Cr2 O14 C28 Ca1 170.1(12) . . . 1_655 ? O15 C27 C28 O16 5.5(4) . . . . ? O13 C27 C28 O16 -176.2(3) . . . . ? Ca1 C27 C28 O16 -1.0(3) 1_655 . . . ? O15 C27 C28 O14 -173.6(3) . . . . ? O13 C27 C28 O14 4.7(4) . . . . ? Ca1 C27 C28 O14 179.9(2) 1_655 . . . ? O15 C27 C28 Ca1 6.4(3) . . . 1_655 ? O13 C27 C28 Ca1 -175.3(3) . . . 1_655 ?