# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Catalina Ruiz-Perez' _publ_contact_author_email CARUIZ@ULL.ES _publ_section_title ; Building-block process for the synthesis of new Chromium(III) Malonate Complexes ; loop_ _publ_author_name 'Catalina Ruiz-Perez' 'Fernando S Delgado' 'Miguel Julve' 'F Lloret' 'Joaquin Sanchiz' # Attachment 'compound-2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 294300' #TrackingRef 'compound-2.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Cr2 K4 O24' _chemical_formula_weight 810.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2948(7) _cell_length_b 9.4737(10) _cell_length_c 9.7296(8) _cell_angle_alpha 102.028(6) _cell_angle_beta 100.085(6) _cell_angle_gamma 106.708(6) _cell_volume 693.31(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.351 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7745 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 6.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3945 _reflns_number_gt 3086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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)' _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^)+(0.0446P)^2^+0.5092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.036(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3945 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.13468(4) 0.01171(4) 0.13171(4) 0.01459(11) Uani 1 1 d . . . K1 K 0.08665(8) 0.40164(7) 0.14948(7) 0.03473(16) Uani 1 1 d . . . K2 K -0.36500(8) -0.30783(6) 0.18024(7) 0.03566(16) Uani 1 1 d . . . C1 C 0.4444(3) 0.2696(2) 0.1484(2) 0.0204(4) Uani 1 1 d . . . C2 C 0.5538(3) 0.1937(3) 0.2295(3) 0.0279(5) Uani 1 1 d . . . H1 H 0.6739 0.2387 0.2275 0.034 Uiso 1 1 calc R . . H2 H 0.5486 0.2171 0.3302 0.034 Uiso 1 1 calc R . . C3 C 0.4999(3) 0.0223(3) 0.1706(2) 0.0189(4) Uani 1 1 d . . . O1 O 0.2795(2) 0.20906(18) 0.11348(18) 0.0219(3) Uani 1 1 d . . . O2 O 0.33872(19) -0.05679(18) 0.15089(17) 0.0207(3) Uani 1 1 d . . . O3 O 0.5187(2) 0.38909(19) 0.1207(2) 0.0310(4) Uani 1 1 d . . . O4 O 0.6082(2) -0.0385(2) 0.1470(2) 0.0299(4) Uani 1 1 d . . . C11 C 0.0342(3) -0.2317(3) 0.2729(3) 0.0245(5) Uani 1 1 d . . . C12 C 0.1764(4) -0.1271(3) 0.4049(3) 0.0337(6) Uani 1 1 d . . . H12 H 0.2864 -0.1353 0.3903 0.040 Uiso 1 1 calc R . . H11 H 0.1564 -0.1643 0.4881 0.040 Uiso 1 1 calc R . . C13 C 0.1937(4) 0.0408(3) 0.4416(3) 0.0403(7) Uani 1 1 d . . . O11 O 0.0006(2) -0.18349(18) 0.16134(17) 0.0215(3) Uani 1 1 d . . . O12 O 0.1827(2) 0.1069(2) 0.34014(18) 0.0286(4) Uani 1 1 d . . . O13 O -0.0462(3) -0.3626(2) 0.2762(2) 0.0373(5) Uani 1 1 d . . . O14 O 0.2163(6) 0.1102(4) 0.5688(3) 0.0947(12) Uani 1 1 d . . . O20 O 0.06805(18) -0.07682(17) -0.08142(16) 0.0164(3) Uani 1 1 d . . . H20 H 0.1506 -0.0429 -0.1148 0.025 Uiso 1 1 calc R . . O1W O 0.2312(3) 0.6275(2) 0.0317(2) 0.0381(5) Uani 1 1 d . . . O2W O 0.1474(6) 0.3934(4) 0.4539(4) 0.0959(12) Uani 1 1 d . . . O3W O -0.5804(6) -0.3921(5) 0.3928(4) 0.1100(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01386(17) 0.01227(17) 0.01793(18) 0.00347(12) 0.00473(12) 0.00487(12) K1 0.0350(3) 0.0246(3) 0.0482(4) 0.0115(2) 0.0117(3) 0.0136(2) K2 0.0423(3) 0.0194(3) 0.0377(3) 0.0033(2) -0.0012(3) 0.0089(2) C1 0.0200(11) 0.0145(10) 0.0257(11) 0.0024(8) 0.0063(9) 0.0061(8) C2 0.0169(11) 0.0225(12) 0.0374(14) 0.0058(10) -0.0025(10) 0.0034(9) C3 0.0192(10) 0.0207(10) 0.0195(10) 0.0094(8) 0.0042(8) 0.0083(9) O1 0.0171(7) 0.0165(8) 0.0323(9) 0.0086(7) 0.0053(6) 0.0052(6) O2 0.0168(7) 0.0168(7) 0.0299(8) 0.0068(6) 0.0061(6) 0.0073(6) O3 0.0261(9) 0.0160(8) 0.0501(11) 0.0110(8) 0.0126(8) 0.0029(7) O4 0.0226(8) 0.0300(9) 0.0471(11) 0.0172(8) 0.0156(8) 0.0151(7) C11 0.0267(12) 0.0240(12) 0.0288(12) 0.0109(9) 0.0121(10) 0.0115(10) C12 0.0384(15) 0.0359(15) 0.0252(12) 0.0136(11) 0.0018(11) 0.0104(12) C13 0.0521(18) 0.0373(16) 0.0211(12) 0.0015(11) -0.0012(12) 0.0104(14) O11 0.0226(8) 0.0192(8) 0.0231(8) 0.0078(6) 0.0066(6) 0.0055(6) O12 0.0369(10) 0.0246(9) 0.0208(8) 0.0001(7) 0.0049(7) 0.0109(8) O13 0.0506(12) 0.0251(10) 0.0410(11) 0.0171(8) 0.0167(9) 0.0110(9) O14 0.179(4) 0.066(2) 0.0222(12) -0.0021(12) 0.0049(16) 0.040(2) O20 0.0136(7) 0.0168(7) 0.0198(7) 0.0047(6) 0.0071(6) 0.0052(6) O1W 0.0374(11) 0.0247(9) 0.0537(12) 0.0079(9) 0.0215(9) 0.0085(8) O2W 0.179(4) 0.0557(18) 0.084(2) 0.0398(16) 0.067(2) 0.050(2) O3W 0.120(3) 0.122(3) 0.084(2) 0.016(2) 0.038(2) 0.035(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O12 1.9577(17) . ? Cr1 O20 1.9702(14) 2 ? Cr1 O11 1.9726(16) . ? Cr1 O1 1.9727(16) . ? Cr1 O2 1.9728(15) . ? Cr1 O20 1.9790(15) . ? Cr1 K1 3.7998(7) . ? Cr1 K1 3.9790(8) 2 ? K1 O1W 2.713(2) . ? K1 O1 2.7600(16) . ? K1 O1W 2.808(2) 2_565 ? K1 O20 2.8525(16) 2 ? K1 O13 2.910(2) 1_565 ? K1 O2W 2.937(3) . ? K1 O11 3.1159(17) 2 ? K1 O3W 3.119(4) 1_665 ? K1 C1 3.537(2) . ? K1 Cr1 3.9790(8) 2 ? K1 K1 4.0418(12) 2_565 ? K2 O14 2.589(3) 2_556 ? K2 O3 2.6513(18) 1_445 ? K2 O4 2.7034(19) 1_455 ? K2 O3 2.825(2) 2 ? K2 O13 2.874(2) . ? K2 O11 2.9752(17) . ? K2 O3W 3.044(4) . ? K2 C11 3.100(2) . ? K2 O1W 3.231(2) 1_445 ? K2 C1 3.267(2) 2 ? K2 K2 4.2205(12) 2_445 ? C1 O3 1.232(3) . ? C1 O1 1.273(3) . ? C1 C2 1.525(3) . ? C1 K2 3.267(2) 2 ? C2 C3 1.507(3) . ? C3 O4 1.227(3) . ? C3 O2 1.288(3) . ? O1 K2 3.3148(18) 2 ? O3 K2 2.6513(18) 1_665 ? O3 K2 2.825(2) 2 ? O4 K2 2.7034(19) 1_655 ? C11 O13 1.238(3) . ? C11 O11 1.280(3) . ? C11 C12 1.513(4) . ? C12 C13 1.513(4) . ? C13 O14 1.229(4) . ? C13 O12 1.278(3) . ? O11 K1 3.1159(17) 2 ? O13 K1 2.910(2) 1_545 ? O14 K2 2.589(3) 2_556 ? O1W K1 2.808(2) 2_565 ? O1W K2 3.231(2) 1_665 ? O3W K1 3.119(4) 1_445 ? 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 O12 Cr1 O20 94.14(7) . 2 ? O12 Cr1 O11 88.86(7) . . ? O20 Cr1 O11 95.10(6) 2 . ? O12 Cr1 O1 88.41(7) . . ? O20 Cr1 O1 87.41(6) 2 . ? O11 Cr1 O1 176.42(7) . . ? O12 Cr1 O2 94.03(7) . . ? O20 Cr1 O2 171.27(6) 2 . ? O11 Cr1 O2 88.14(7) . . ? O1 Cr1 O2 89.74(7) . . ? O12 Cr1 O20 174.66(7) . . ? O20 Cr1 O20 80.52(6) 2 . ? O11 Cr1 O20 91.74(6) . . ? O1 Cr1 O20 91.20(7) . . ? O2 Cr1 O20 91.29(6) . . ? O12 Cr1 K1 76.49(5) . . ? O20 Cr1 K1 47.15(4) 2 . ? O11 Cr1 K1 136.88(5) . . ? O1 Cr1 K1 44.39(5) . . ? O2 Cr1 K1 132.55(5) . . ? O20 Cr1 K1 99.55(4) . . ? O12 Cr1 K1 138.94(6) . 2 ? O20 Cr1 K1 94.15(5) 2 2 ? O11 Cr1 K1 50.36(5) . 2 ? O1 Cr1 K1 132.10(5) . 2 ? O2 Cr1 K1 81.65(5) . 2 ? O20 Cr1 K1 42.50(4) . 2 ? K1 Cr1 K1 134.483(12) . 2 ? O1W K1 O1 104.11(6) . . ? O1W K1 O1W 85.88(6) . 2_565 ? O1 K1 O1W 127.42(6) . 2_565 ? O1W K1 O20 141.70(6) . 2 ? O1 K1 O20 58.05(4) . 2 ? O1W K1 O20 82.14(5) 2_565 2 ? O1W K1 O13 79.37(6) . 1_565 ? O1 K1 O13 162.42(6) . 1_565 ? O1W K1 O13 69.65(6) 2_565 1_565 ? O20 K1 O13 128.59(5) 2 1_565 ? O1W K1 O2W 129.81(9) . . ? O1 K1 O2W 86.24(8) . . ? O1W K1 O2W 126.28(10) 2_565 . ? O20 K1 O2W 85.47(7) 2 . ? O13 K1 O2W 78.67(8) 1_565 . ? O1W K1 O11 85.40(5) . 2 ? O1 K1 O11 64.19(5) . 2 ? O1W K1 O11 65.46(5) 2_565 2 ? O20 K1 O11 56.54(4) 2 2 ? O13 K1 O11 133.37(5) 1_565 2 ? O2W K1 O11 139.97(7) . 2 ? O1W K1 O3W 77.19(10) . 1_665 ? O1 K1 O3W 82.52(9) . 1_665 ? O1W K1 O3W 148.82(10) 2_565 1_665 ? O20 K1 O3W 126.73(9) 2 1_665 ? O13 K1 O3W 81.49(9) 1_565 1_665 ? O2W K1 O3W 55.27(12) . 1_665 ? O11 K1 O3W 137.25(8) 2 1_665 ? O1W K1 C1 91.18(6) . . ? O1 K1 C1 18.58(5) . . ? O1W K1 C1 141.03(6) 2_565 . ? O20 K1 C1 76.39(5) 2 . ? O13 K1 C1 147.66(6) 1_565 . ? O2W K1 C1 84.24(9) . . ? O11 K1 C1 75.56(5) 2 . ? O3W K1 C1 66.22(9) 1_665 . ? O1W K1 Cr1 131.95(4) . . ? O1 K1 Cr1 30.00(3) . . ? O1W K1 Cr1 110.96(4) 2_565 . ? O20 K1 Cr1 30.42(3) 2 . ? O13 K1 Cr1 148.41(4) 1_565 . ? O2W K1 Cr1 76.49(6) . . ? O11 K1 Cr1 64.36(3) 2 . ? O3W K1 Cr1 99.76(9) 1_665 . ? C1 K1 Cr1 47.17(4) . . ? O1W K1 Cr1 114.49(5) . 2 ? O1 K1 Cr1 60.95(4) . 2 ? O1W K1 Cr1 67.89(4) 2_565 2 ? O20 K1 Cr1 27.95(3) 2 2 ? O13 K1 Cr1 133.77(5) 1_565 2 ? O2W K1 Cr1 113.34(7) . 2 ? O11 K1 Cr1 29.18(3) 2 2 ? O3W K1 Cr1 143.14(9) 1_665 2 ? C1 K1 Cr1 78.30(4) . 2 ? Cr1 K1 Cr1 45.517(12) . 2 ? O1W K1 K1 43.86(5) . 2_565 ? O1 K1 K1 125.86(4) . 2_565 ? O1W K1 K1 42.02(4) 2_565 2_565 ? O20 K1 K1 115.57(4) 2 2_565 ? O13 K1 K1 68.57(4) 1_565 2_565 ? O2W K1 K1 147.23(7) . 2_565 ? O11 K1 K1 69.98(3) 2 2_565 ? O3W K1 K1 116.46(9) 1_665 2_565 ? C1 K1 K1 123.64(5) . 2_565 ? Cr1 K1 K1 134.20(3) . 2_565 ? Cr1 K1 K1 90.96(2) 2 2_565 ? O14 K2 O3 127.91(9) 2_556 1_445 ? O14 K2 O4 74.07(8) 2_556 1_455 ? O3 K2 O4 152.60(6) 1_445 1_455 ? O14 K2 O3 152.61(8) 2_556 2 ? O3 K2 O3 79.22(6) 1_445 2 ? O4 K2 O3 78.90(6) 1_455 2 ? O14 K2 O13 75.21(10) 2_556 . ? O3 K2 O13 79.71(6) 1_445 . ? O4 K2 O13 125.69(6) 1_455 . ? O3 K2 O13 118.82(6) 2 . ? O14 K2 O11 77.53(11) 2_556 . ? O3 K2 O11 112.84(5) 1_445 . ? O4 K2 O11 85.85(5) 1_455 . ? O3 K2 O11 96.34(5) 2 . ? O13 K2 O11 44.17(5) . . ? O14 K2 O3W 71.41(13) 2_556 . ? O3 K2 O3W 72.48(9) 1_445 . ? O4 K2 O3W 105.65(10) 1_455 . ? O3 K2 O3W 121.24(9) 2 . ? O13 K2 O3W 105.41(10) . . ? O11 K2 O3W 141.95(9) . . ? O14 K2 C11 65.95(11) 2_556 . ? O3 K2 C11 102.21(6) 1_445 . ? O4 K2 C11 102.25(6) 1_455 . ? O3 K2 C11 116.71(6) 2 . ? O13 K2 C11 23.54(6) . . ? O11 K2 C11 24.22(5) . . ? O3W K2 C11 119.00(10) . . ? O14 K2 O1W 119.90(11) 2_556 1_445 ? O3 K2 O1W 80.80(5) 1_445 1_445 ? O4 K2 O1W 73.04(5) 1_455 1_445 ? O3 K2 O1W 54.02(5) 2 1_445 ? O13 K2 O1W 160.31(5) . 1_445 ? O11 K2 O1W 145.85(5) . 1_445 ? O3W K2 O1W 71.10(9) . 1_445 ? C11 K2 O1W 169.89(6) . 1_445 ? O14 K2 C1 132.21(9) 2_556 2 ? O3 K2 C1 99.78(6) 1_445 2 ? O4 K2 C1 61.82(6) 1_455 2 ? O3 K2 C1 21.82(5) 2 2 ? O13 K2 C1 116.01(6) . 2 ? O11 K2 C1 81.71(5) . 2 ? O3W K2 C1 135.88(10) . 2 ? C11 K2 C1 105.12(6) . 2 ? O1W K2 C1 64.78(5) 1_445 2 ? O14 K2 O1 118.63(9) 2_556 2 ? O3 K2 O1 109.12(5) 1_445 2 ? O4 K2 O1 62.03(5) 1_455 2 ? O3 K2 O1 40.87(4) 2 2 ? O13 K2 O1 97.05(5) . 2 ? O11 K2 O1 59.53(4) . 2 ? O3W K2 O1 157.30(9) . 2 ? C11 K2 O1 83.25(5) . 2 ? O1W K2 O1 86.64(5) 1_445 2 ? C1 K2 O1 22.29(5) 2 2 ? O14 K2 K2 168.62(8) 2_556 2_445 ? O3 K2 K2 41.12(4) 1_445 2_445 ? O4 K2 K2 115.40(5) 1_455 2_445 ? O3 K2 K2 38.11(4) 2 2_445 ? O13 K2 K2 102.15(5) . 2_445 ? O11 K2 K2 108.53(4) . 2_445 ? O3W K2 K2 99.09(8) . 2_445 ? C11 K2 K2 115.71(5) . 2_445 ? O1W K2 K2 60.42(4) 1_445 2_445 ? C1 K2 K2 59.02(4) 2 2_445 ? O1 K2 K2 72.52(3) 2 2_445 ? O3 C1 O1 122.2(2) . . ? O3 C1 C2 118.8(2) . . ? O1 C1 C2 119.1(2) . . ? O3 C1 K2 58.48(13) . 2 ? O1 C1 K2 80.98(13) . 2 ? C2 C1 K2 135.48(15) . 2 ? O3 C1 K1 86.67(13) . . ? O1 C1 K1 43.69(10) . . ? C2 C1 K1 143.23(16) . . ? K2 C1 K1 79.58(5) 2 . ? C3 C2 C1 115.14(19) . . ? O4 C3 O2 121.9(2) . . ? O4 C3 C2 120.4(2) . . ? O2 C3 C2 117.62(19) . . ? C1 O1 Cr1 129.05(14) . . ? C1 O1 K1 117.73(13) . . ? Cr1 O1 K1 105.61(6) . . ? C1 O1 K2 76.73(13) . 2 ? Cr1 O1 K2 129.68(7) . 2 ? K1 O1 K2 91.23(5) . 2 ? C3 O2 Cr1 128.84(14) . . ? C1 O3 K2 151.60(16) . 1_665 ? C1 O3 K2 99.70(15) . 2 ? K2 O3 K2 100.78(6) 1_665 2 ? C3 O4 K2 130.75(15) . 1_655 ? O13 C11 O11 121.8(2) . . ? O13 C11 C12 118.6(2) . . ? O11 C11 C12 119.6(2) . . ? O13 C11 K2 67.95(14) . . ? O11 C11 K2 72.43(13) . . ? C12 C11 K2 134.38(17) . . ? C11 C12 C13 116.4(2) . . ? O14 C13 O12 121.4(3) . . ? O14 C13 C12 119.0(3) . . ? O12 C13 C12 119.7(2) . . ? C11 O11 Cr1 126.25(15) . . ? C11 O11 K2 83.35(13) . . ? Cr1 O11 K2 132.23(7) . . ? C11 O11 K1 120.19(14) . 2 ? Cr1 O11 K1 100.46(6) . 2 ? K2 O11 K1 91.35(5) . 2 ? C13 O12 Cr1 126.81(17) . . ? C11 O13 K2 88.52(15) . . ? C11 O13 K1 114.70(16) . 1_545 ? K2 O13 K1 130.91(8) . 1_545 ? C13 O14 K2 159.9(3) . 2_556 ? K1 O1W K1 94.12(6) . 2_565 ? K1 O1W K2 98.32(7) . 1_665 ? K1 O1W K2 166.13(8) 2_565 1_665 ? K2 O3W K1 94.04(11) . 1_445 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.918 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.083 # Attachment 'compound-3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 294301' #TrackingRef 'compound-3.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H98 Cl4 Cr2 Cu4 N16 O42' _chemical_formula_weight 1927.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.7161(4) _cell_length_b 11.3208(10) _cell_length_c 20.1947(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.637(5) _cell_angle_gamma 90.00 _cell_volume 3729.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 0.597 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23087 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 6.40 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9739 _reflns_number_gt 5835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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)' _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. In the refinement EQIV $1 -x, -y, -z FREE O20 CR1_$1 SADI CL2 O25 CL2 O26 CL2 O27 CL2 O28 SADI O25 O26 O25 O27 O25 O28 O26 O27 O26 O28 O27 O28 BLOC 1 -1 CR1 > C56 BLOC 2 -2 CL1 > O4w ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+7.4274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9739 _refine_ls_number_parameters 470 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1997 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.06841(4) 0.05533(6) 0.05111(3) 0.01820(16) Uani 1 1 d . . . C1 C -0.0040(3) 0.2909(4) 0.0391(2) 0.0234(9) Uani 1 1 d . . . C2 C 0.0612(3) 0.3307(4) 0.0020(2) 0.0247(9) Uani 1 1 d . . . H1 H 0.0435 0.3095 -0.0455 0.030 Uiso 1 1 calc R . . H2 H 0.0652 0.4161 0.0046 0.030 Uiso 1 1 calc R . . C3 C 0.1448(3) 0.2795(4) 0.0287(2) 0.0220(9) Uani 1 1 d . . . O1 O -0.00068(18) 0.1902(3) 0.06603(15) 0.0246(6) Uani 1 1 d . . . O2 O 0.15335(17) 0.1719(3) 0.04628(16) 0.0236(6) Uani 1 1 d . . . O3 O -0.0603(2) 0.3622(3) 0.04013(19) 0.0351(8) Uani 1 1 d . . . O4 O 0.20665(19) 0.3426(3) 0.03183(18) 0.0312(7) Uani 1 1 d . . . C11 C 0.1815(3) -0.1420(4) 0.0833(3) 0.0317(10) Uani 1 1 d . . . C12 C 0.1441(3) -0.1600(5) 0.1444(3) 0.0369(11) Uani 1 1 d . . . H11 H 0.0908 -0.1966 0.1292 0.044 Uiso 1 1 calc R . . H12 H 0.1783 -0.2151 0.1749 0.044 Uiso 1 1 calc R . . C13 C 0.1336(3) -0.0518(4) 0.1836(2) 0.0309(10) Uani 1 1 d . . . O11 O 0.15014(18) -0.0640(3) 0.04029(15) 0.0262(7) Uani 1 1 d . . . O12 O 0.1060(2) 0.0428(3) 0.15022(15) 0.0292(7) Uani 1 1 d . . . O13 O 0.2400(3) -0.2035(4) 0.0770(2) 0.0592(12) Uani 1 1 d . . . O14 O 0.1498(3) -0.0542(4) 0.24593(18) 0.0527(11) Uani 1 1 d . . . O20 O 0.01951(17) 0.0598(3) -0.04595(14) 0.0234(6) Uani 1 1 d . . . H20 H 0.0553 0.0501 -0.0674 0.035 Uiso 1 1 calc R . . Cu1 Cu -0.13999(3) 0.34609(5) 0.09877(3) 0.03053(16) Uani 1 1 d . . . Cu2 Cu 0.30941(3) 0.25572(5) 0.07554(3) 0.02672(15) Uani 1 1 d . . . N31 N -0.2382(3) 0.4206(5) 0.0289(3) 0.0520(13) Uani 1 1 d . . . H30 H -0.2202 0.4774 0.0046 0.062 Uiso 1 1 calc R . . H31 H -0.2641 0.3650 0.0001 0.062 Uiso 1 1 calc R . . N32 N -0.1529(3) 0.1656(4) 0.1028(3) 0.0432(11) Uani 1 1 d . . . H36 H -0.1631 0.1354 0.0606 0.052 Uiso 1 1 calc R . . H37 H -0.1063 0.1332 0.1266 0.052 Uiso 1 1 calc R . . N33 N -0.0663(3) 0.4483(6) 0.1710(3) 0.076(2) Uani 1 1 d . . . H42 H -0.0137 0.4249 0.1768 0.092 Uiso 1 1 calc R . . H43 H -0.0696 0.5245 0.1581 0.092 Uiso 1 1 calc R . . N34 N -0.2194(3) 0.3480(4) 0.1633(2) 0.0420(11) Uani 1 1 d . . . C31 C -0.2940(4) 0.4707(6) 0.0687(4) 0.065(2) Uani 1 1 d . . . H33 H -0.3476 0.4846 0.0397 0.078 Uiso 1 1 calc R . . H32 H -0.2726 0.5454 0.0887 0.078 Uiso 1 1 calc R . . C32 C -0.3004(4) 0.3824(7) 0.1242(4) 0.0626(19) Uani 1 1 d . . . H34 H -0.3317 0.4172 0.1545 0.075 Uiso 1 1 calc R . . H35 H -0.3295 0.3127 0.1038 0.075 Uiso 1 1 calc R . . C33 C -0.2207(4) 0.1378(5) 0.1352(4) 0.0568(17) Uani 1 1 d . . . H39 H -0.2138 0.0590 0.1546 0.068 Uiso 1 1 calc R . . H38 H -0.2723 0.1404 0.1020 0.068 Uiso 1 1 calc R . . C34 C -0.2211(5) 0.2259(6) 0.1892(4) 0.068(2) Uani 1 1 d . . . H41 H -0.1736 0.2134 0.2259 0.081 Uiso 1 1 calc R . . H40 H -0.2698 0.2152 0.2072 0.081 Uiso 1 1 calc R . . C35 C -0.0941(5) 0.4346(8) 0.2338(4) 0.075(2) Uani 1 1 d . . . H45 H -0.0737 0.4993 0.2644 0.090 Uiso 1 1 calc R . . H44 H -0.0733 0.3613 0.2559 0.090 Uiso 1 1 calc R . . C36 C -0.1857(5) 0.4338(7) 0.2183(4) 0.072(2) Uani 1 1 d . . . H46 H -0.2046 0.4130 0.2589 0.087 Uiso 1 1 calc R . . H47 H -0.2060 0.5123 0.2044 0.087 Uiso 1 1 calc R . . N51 N 0.3099(4) 0.1526(8) -0.0073(3) 0.092(3) Uani 1 1 d . . . H50 H 0.2618 0.1141 -0.0194 0.111 Uiso 1 1 calc R . . H51 H 0.3159 0.1983 -0.0423 0.111 Uiso 1 1 calc R . . N52 N 0.2772(3) 0.2394(4) 0.1677(2) 0.0425(11) Uani 1 1 d . . . H56 H 0.2948 0.3024 0.1940 0.051 Uiso 1 1 calc R . . H57 H 0.2224 0.2343 0.1618 0.051 Uiso 1 1 calc R . . N53 N 0.3975(3) 0.3937(5) 0.0852(3) 0.0613(15) Uani 1 1 d . . . H62 H 0.4080 0.4113 0.0445 0.074 Uiso 1 1 calc R . . H63 H 0.3787 0.4591 0.1022 0.074 Uiso 1 1 calc R . . N54 N 0.4072(3) 0.1527(4) 0.1197(2) 0.0412(11) Uani 1 1 d . . . C51 C 0.3763(6) 0.0684(7) 0.0082(4) 0.076(2) Uani 1 1 d . . . H53 H 0.4218 0.0975 -0.0097 0.091 Uiso 1 1 calc R . . H52 H 0.3583 -0.0055 -0.0145 0.091 Uiso 1 1 calc R . . C52 C 0.4049(6) 0.0457(7) 0.0813(5) 0.089(3) Uani 1 1 d . . . H54 H 0.3686 -0.0105 0.0960 0.107 Uiso 1 1 calc R . . H55 H 0.4594 0.0113 0.0897 0.107 Uiso 1 1 calc R . . C53 C 0.3157(4) 0.1331(6) 0.1987(3) 0.0556(16) Uani 1 1 d . . . H58 H 0.3132 0.1308 0.2462 0.067 Uiso 1 1 calc R . . H59 H 0.2871 0.0644 0.1764 0.067 Uiso 1 1 calc R . . C54 C 0.3990(5) 0.1317(8) 0.1924(4) 0.077(2) Uani 1 1 d . . . H61 H 0.4231 0.0559 0.2078 0.092 Uiso 1 1 calc R . . H60 H 0.4292 0.1923 0.2215 0.092 Uiso 1 1 calc R . . C55 C 0.4703(4) 0.3517(6) 0.1306(4) 0.065(2) Uani 1 1 d . . . H65 H 0.4674 0.3704 0.1769 0.078 Uiso 1 1 calc R . . H64 H 0.5175 0.3924 0.1208 0.078 Uiso 1 1 calc R . . C56 C 0.4817(4) 0.2220(7) 0.1246(4) 0.067(2) Uani 1 1 d . . . H66 H 0.5036 0.2069 0.0847 0.081 Uiso 1 1 calc R . . H67 H 0.5221 0.1953 0.1639 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.61888(10) 0.29837(15) 0.32691(7) 0.0517(4) Uani 1 1 d . . . O21 O 0.6802(13) 0.2218(15) 0.3528(10) 0.301(10) Uani 1 1 d . . . O22 O 0.6254(6) 0.3273(16) 0.2654(4) 0.229(7) Uani 1 1 d . . . O23 O 0.6390(5) 0.3792(8) 0.3797(5) 0.148(4) Uani 1 1 d . . . O24 O 0.5450(5) 0.2395(9) 0.3281(4) 0.146(4) Uani 1 1 d . . . Cl2 Cl 0.5003(3) -0.3018(2) 0.0863(2) 0.1459(16) Uani 1 1 d D . . O25 O 0.5237(7) -0.3721(9) 0.0462(5) 0.177(5) Uani 1 1 d D . . O26 O 0.4508(12) -0.2201(10) 0.0492(10) 0.87(6) Uani 1 1 d D . . O27 O 0.4521(10) -0.3506(10) 0.1219(7) 0.276(10) Uani 1 1 d D . . O28 O 0.5542(8) -0.2459(19) 0.1209(6) 0.348(16) Uani 1 1 d D . . O1W O 0.3605(7) -0.1841(11) 0.2153(6) 0.183(4) Uani 1 1 d . . . O2W O 0.4921(5) -0.3348(7) 0.2740(4) 0.125(3) Uani 1 1 d . . . O3W O 0.3839(4) -0.0745(7) 0.3430(3) 0.107(2) Uani 1 1 d . . . O4W O 0.2410(4) 0.0661(4) 0.3595(3) 0.0841(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0177(3) 0.0169(3) 0.0196(3) 0.0023(3) 0.0032(2) -0.0011(3) C1 0.020(2) 0.025(2) 0.026(2) -0.0019(18) 0.0070(16) -0.0010(17) C2 0.020(2) 0.024(2) 0.032(2) 0.0080(18) 0.0096(17) 0.0012(17) C3 0.021(2) 0.023(2) 0.024(2) 0.0001(17) 0.0074(16) -0.0026(17) O1 0.0254(16) 0.0193(14) 0.0314(16) 0.0043(13) 0.0116(13) 0.0010(12) O2 0.0148(14) 0.0204(15) 0.0345(17) 0.0011(13) 0.0028(12) -0.0024(11) O3 0.0273(17) 0.0292(17) 0.055(2) 0.0140(16) 0.0232(16) 0.0101(14) O4 0.0228(16) 0.0237(16) 0.047(2) 0.0081(14) 0.0077(14) -0.0050(13) C11 0.032(3) 0.027(2) 0.035(3) 0.002(2) 0.005(2) 0.003(2) C12 0.044(3) 0.033(3) 0.033(3) 0.009(2) 0.008(2) 0.009(2) C13 0.030(2) 0.036(3) 0.026(2) 0.005(2) 0.0019(18) 0.000(2) O11 0.0258(16) 0.0252(16) 0.0281(16) 0.0028(13) 0.0069(12) 0.0036(13) O12 0.0380(18) 0.0267(16) 0.0211(15) 0.0007(13) 0.0023(13) 0.0022(14) O13 0.056(3) 0.060(3) 0.066(3) 0.014(2) 0.023(2) 0.036(2) O14 0.078(3) 0.053(2) 0.0218(18) 0.0060(17) -0.0007(18) 0.008(2) O20 0.0209(15) 0.0253(15) 0.0233(14) 0.0032(12) 0.0036(11) -0.0081(12) Cu1 0.0256(3) 0.0254(3) 0.0457(4) 0.0046(3) 0.0189(2) 0.0035(2) Cu2 0.0196(3) 0.0302(3) 0.0295(3) -0.0008(2) 0.0033(2) -0.0012(2) N31 0.041(3) 0.052(3) 0.067(3) 0.028(3) 0.020(2) 0.006(2) N32 0.055(3) 0.030(2) 0.054(3) 0.002(2) 0.031(2) -0.002(2) N33 0.047(3) 0.102(5) 0.087(5) -0.045(4) 0.030(3) -0.019(3) N34 0.044(3) 0.036(2) 0.055(3) 0.002(2) 0.030(2) 0.004(2) C31 0.037(3) 0.058(4) 0.103(6) 0.025(4) 0.025(4) 0.018(3) C32 0.039(3) 0.071(4) 0.090(5) 0.010(4) 0.039(3) 0.008(3) C33 0.062(4) 0.037(3) 0.086(5) 0.002(3) 0.048(4) -0.010(3) C34 0.099(6) 0.046(4) 0.079(5) 0.011(3) 0.064(5) 0.003(4) C35 0.067(5) 0.089(6) 0.069(5) -0.030(4) 0.014(4) -0.006(4) C36 0.078(5) 0.073(5) 0.079(5) -0.026(4) 0.043(4) -0.004(4) N51 0.052(3) 0.168(7) 0.051(3) -0.054(4) -0.002(3) 0.036(4) N52 0.031(2) 0.065(3) 0.030(2) -0.009(2) 0.0039(17) -0.002(2) N53 0.044(3) 0.047(3) 0.093(4) 0.006(3) 0.014(3) -0.011(2) N54 0.030(2) 0.039(2) 0.052(3) 0.005(2) 0.0025(19) 0.0061(19) C51 0.110(6) 0.059(4) 0.077(5) -0.022(4) 0.058(5) 0.005(4) C52 0.082(6) 0.064(5) 0.110(7) -0.028(5) -0.003(5) 0.033(4) C53 0.075(5) 0.052(4) 0.043(3) -0.001(3) 0.019(3) -0.014(3) C54 0.077(5) 0.077(5) 0.071(5) 0.032(4) 0.004(4) 0.009(4) C55 0.038(3) 0.073(5) 0.074(5) 0.011(4) -0.010(3) -0.021(3) C56 0.022(3) 0.076(5) 0.098(6) -0.004(4) 0.000(3) 0.003(3) Cl1 0.0662(10) 0.0578(9) 0.0353(7) -0.0094(6) 0.0201(6) 0.0001(8) O21 0.32(2) 0.213(14) 0.32(2) 0.014(13) -0.034(16) 0.153(14) O22 0.117(6) 0.53(2) 0.048(4) 0.047(8) 0.033(4) -0.005(10) O23 0.164(7) 0.160(7) 0.159(7) -0.088(6) 0.116(6) -0.080(6) O24 0.119(6) 0.217(10) 0.111(6) -0.042(6) 0.047(5) -0.079(6) Cl2 0.254(4) 0.0648(14) 0.173(3) -0.0176(17) 0.165(3) -0.028(2) O25 0.222(11) 0.197(10) 0.139(7) 0.005(7) 0.098(8) 0.106(9) O26 1.52(13) 0.114(11) 1.42(12) 0.31(3) 1.30(12) 0.32(3) O27 0.43(2) 0.216(13) 0.267(16) -0.034(11) 0.264(18) -0.108(14) O28 0.231(15) 0.68(4) 0.115(9) -0.170(16) 0.001(9) -0.18(2) O1W 0.167(9) 0.191(10) 0.195(10) -0.069(8) 0.047(8) 0.013(8) O2W 0.135(6) 0.155(7) 0.086(5) 0.007(5) 0.028(4) -0.060(5) O3W 0.076(4) 0.154(6) 0.091(4) 0.025(4) 0.018(3) 0.015(4) O4W 0.123(5) 0.055(3) 0.063(3) -0.002(2) -0.006(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O20 1.950(3) 3 ? Cr1 O20 1.953(3) . ? Cr1 O2 1.956(3) . ? Cr1 O11 1.967(3) . ? Cr1 O12 1.967(3) . ? Cr1 O1 1.977(3) . ? C1 O3 1.243(5) . ? C1 O1 1.259(5) . ? C1 C2 1.519(6) . ? C2 C3 1.501(6) . ? C3 O4 1.246(5) . ? C3 O2 1.268(5) . ? O3 Cu1 1.975(3) . ? O4 Cu2 2.008(3) . ? C11 O13 1.230(6) . ? C11 O11 1.269(5) . ? C11 C12 1.514(7) . ? C12 C13 1.489(7) . ? C13 O14 1.229(6) . ? C13 O12 1.296(5) . ? Cu1 N33 2.049(6) . ? Cu1 N34 2.053(4) . ? Cu1 N32 2.058(4) . ? Cu1 N31 2.094(5) . ? Cu2 N51 2.041(5) . ? Cu2 N54 2.046(4) . ? Cu2 N52 2.055(4) . ? Cu2 N53 2.126(5) . ? N31 C31 1.472(8) . ? N32 C33 1.461(7) . ? N33 C35 1.452(10) . ? N34 C32 1.464(8) . ? N34 C34 1.480(7) . ? N34 C36 1.490(8) . ? C31 C32 1.524(10) . ? C33 C34 1.479(9) . ? C35 C36 1.495(11) . ? N51 C51 1.445(10) . ? N52 C53 1.441(8) . ? N53 C55 1.435(8) . ? N54 C52 1.434(9) . ? N54 C56 1.458(8) . ? N54 C54 1.524(9) . ? C51 C52 1.471(12) . ? C53 C54 1.425(11) . ? C55 C56 1.489(10) . ? Cl1 O22 1.312(7) . ? Cl1 O21 1.356(13) . ? Cl1 O23 1.389(7) . ? Cl1 O24 1.408(7) . ? Cl2 O28 1.193(9) . ? Cl2 O25 1.257(7) . ? Cl2 O27 1.312(9) . ? Cl2 O26 1.353(14) . ? 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 O20 Cr1 O20 79.56(13) 3 . ? O20 Cr1 O2 174.20(13) 3 . ? O20 Cr1 O2 94.66(12) . . ? O20 Cr1 O11 93.94(13) 3 . ? O20 Cr1 O11 93.14(13) . . ? O2 Cr1 O11 85.88(13) . . ? O20 Cr1 O12 94.31(13) 3 . ? O20 Cr1 O12 173.52(13) . . ? O2 Cr1 O12 91.48(13) . . ? O11 Cr1 O12 89.34(13) . . ? O20 Cr1 O1 93.78(13) 3 . ? O20 Cr1 O1 90.14(13) . . ? O2 Cr1 O1 86.63(12) . . ? O11 Cr1 O1 172.04(13) . . ? O12 Cr1 O1 88.16(13) . . ? O3 C1 O1 122.9(4) . . ? O3 C1 C2 116.3(4) . . ? O1 C1 C2 120.8(4) . . ? C3 C2 C1 114.9(4) . . ? O4 C3 O2 119.7(4) . . ? O4 C3 C2 119.6(4) . . ? O2 C3 C2 120.7(4) . . ? C1 O1 Cr1 127.3(3) . . ? C3 O2 Cr1 128.6(3) . . ? C1 O3 Cu1 124.2(3) . . ? C3 O4 Cu2 111.2(3) . . ? O13 C11 O11 122.9(5) . . ? O13 C11 C12 119.2(4) . . ? O11 C11 C12 118.0(4) . . ? C13 C12 C11 116.2(4) . . ? O14 C13 O12 121.7(5) . . ? O14 C13 C12 120.1(4) . . ? O12 C13 C12 118.2(4) . . ? C11 O11 Cr1 126.5(3) . . ? C13 O12 Cr1 126.0(3) . . ? O3 Cu1 N33 89.7(2) . . ? O3 Cu1 N34 173.67(17) . . ? N33 Cu1 N34 85.0(2) . . ? O3 Cu1 N32 101.90(16) . . ? N33 Cu1 N32 125.8(3) . . ? N34 Cu1 N32 84.08(17) . . ? O3 Cu1 N31 95.21(17) . . ? N33 Cu1 N31 120.9(3) . . ? N34 Cu1 N31 84.4(2) . . ? N32 Cu1 N31 110.6(2) . . ? O4 Cu2 N51 94.3(2) . . ? O4 Cu2 N54 174.38(15) . . ? N51 Cu2 N54 83.4(2) . . ? O4 Cu2 N52 94.24(16) . . ? N51 Cu2 N52 137.7(3) . . ? N54 Cu2 N52 84.07(19) . . ? O4 Cu2 N53 100.91(17) . . ? N51 Cu2 N53 111.7(3) . . ? N54 Cu2 N53 84.7(2) . . ? N52 Cu2 N53 107.2(2) . . ? C31 N31 Cu1 106.5(4) . . ? C33 N32 Cu1 109.3(3) . . ? C35 N33 Cu1 107.7(4) . . ? C32 N34 C34 110.6(6) . . ? C32 N34 C36 112.5(5) . . ? C34 N34 C36 112.3(6) . . ? C32 N34 Cu1 108.1(4) . . ? C34 N34 Cu1 106.2(3) . . ? C36 N34 Cu1 106.8(4) . . ? N31 C31 C32 107.7(5) . . ? N34 C32 C31 111.4(5) . . ? N32 C33 C34 108.3(5) . . ? C33 C34 N34 111.5(5) . . ? N33 C35 C36 109.1(6) . . ? N34 C36 C35 111.3(5) . . ? C51 N51 Cu2 109.9(4) . . ? C53 N52 Cu2 106.8(4) . . ? C55 N53 Cu2 106.8(4) . . ? C52 N54 C56 114.4(6) . . ? C52 N54 C54 113.1(6) . . ? C56 N54 C54 105.9(6) . . ? C52 N54 Cu2 108.8(4) . . ? C56 N54 Cu2 108.2(4) . . ? C54 N54 Cu2 106.1(4) . . ? N51 C51 C52 113.5(6) . . ? N54 C52 C51 111.0(7) . . ? C54 C53 N52 108.8(5) . . ? C53 C54 N54 112.3(6) . . ? N53 C55 C56 112.4(6) . . ? N54 C56 C55 114.5(5) . . ? O22 Cl1 O21 108.2(11) . . ? O22 Cl1 O23 120.4(9) . . ? O21 Cl1 O23 95.1(10) . . ? O22 Cl1 O24 112.9(6) . . ? O21 Cl1 O24 106.4(12) . . ? O23 Cl1 O24 111.4(4) . . ? O28 Cl2 O25 114.3(9) . . ? O28 Cl2 O27 112.2(8) . . ? O25 Cl2 O27 113.6(7) . . ? O28 Cl2 O26 104.7(9) . . ? O25 Cl2 O26 108.4(8) . . ? O27 Cl2 O26 102.5(9) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.225 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.121 # Attachment 'compound-4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 294302' #TrackingRef 'compound-4.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H64 Cr2 N8 Ni O26' _chemical_formula_weight 1043.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1804(5) _cell_length_b 9.6532(5) _cell_length_c 13.0261(6) _cell_angle_alpha 106.313(4) _cell_angle_beta 103.821(4) _cell_angle_gamma 95.435(5) _cell_volume 1059.48(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12468 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 6.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5987 _reflns_number_gt 3564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _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)' _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^)+(0.0654P)^2^+0.2130P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5987 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr -0.05174(6) -0.04499(5) 0.08883(4) 0.02298(15) Uani 1 1 d . . . C1 C 0.0603(4) -0.3155(3) 0.1068(3) 0.0260(7) Uani 1 1 d . . . C2 C -0.0691(4) -0.3516(5) 0.1519(4) 0.0354(8) Uani 1 1 d . . . C3 C -0.2183(4) -0.3070(4) 0.1100(3) 0.0296(7) Uani 1 1 d . . . O1 O 0.0757(3) -0.1989(2) 0.0809(2) 0.0317(5) Uani 1 1 d . . . O2 O -0.2206(3) -0.1890(3) 0.0867(2) 0.0331(5) Uani 1 1 d . . . O3 O 0.1549(3) -0.4001(3) 0.0980(2) 0.0409(6) Uani 1 1 d . . . O4 O -0.3372(3) -0.3881(3) 0.1020(3) 0.0498(7) Uani 1 1 d . . . C11 C -0.1863(4) 0.2066(4) 0.1778(3) 0.0326(8) Uani 1 1 d . . . C12 C -0.0454(5) 0.2615(4) 0.2733(4) 0.0394(9) Uani 1 1 d . . . C13 C 0.0359(4) 0.1527(4) 0.3166(3) 0.0310(7) Uani 1 1 d . . . O11 O -0.1937(3) 0.0942(3) 0.09934(18) 0.0306(5) Uani 1 1 d . . . O12 O 0.0254(3) 0.0235(3) 0.25360(18) 0.0314(5) Uani 1 1 d . . . O13 O -0.2945(4) 0.2765(3) 0.1782(2) 0.0567(8) Uani 1 1 d . . . O14 O 0.1126(3) 0.1937(3) 0.4145(2) 0.0502(7) Uani 1 1 d . . . O20 O -0.1104(3) -0.0876(3) -0.0720(2) 0.0277(6) Uani 1 1 d . . . Ni1 Ni -0.5000 -1.0000 0.5000 0.02315(16) Uani 1 2 d S . . C31 C -0.2142(4) -0.9845(6) 0.4439(3) 0.0414(10) Uani 1 1 d . . . C32 C -0.3109(4) -0.9368(5) 0.3542(3) 0.0355(8) Uani 1 1 d . . . C34 C -0.5617(4) -0.8645(4) 0.3199(3) 0.0327(8) Uani 1 1 d . . . C33 C -0.5253(5) -0.7344(4) 0.4233(3) 0.0401(9) Uani 1 1 d . . . C35 C -0.5580(4) -1.1094(4) 0.1299(3) 0.0313(7) Uani 1 1 d . . . C36 C -0.5391(4) -1.1202(4) 0.2468(3) 0.0299(7) Uani 1 1 d . . . N31 N -0.2627(3) -0.9341(4) 0.5464(3) 0.0337(7) Uani 1 1 d . . . N32 N -0.5407(5) -0.7806(4) 0.5198(3) 0.0364(7) Uani 1 1 d . . . N33 N -0.5965(4) -1.2584(4) 0.0488(3) 0.0318(7) Uani 1 1 d . . . N34 N -0.4761(3) -0.9818(3) 0.3390(2) 0.0258(6) Uani 1 1 d . . . O1W O -0.4303(4) -0.4966(4) 0.2581(3) 0.0706(10) Uani 1 1 d . . . O2W O 0.2470(4) -0.6014(3) 0.1969(3) 0.0664(9) Uani 1 1 d . . . O3W O 0.1925(6) -0.3946(4) 0.3867(4) 0.1083(15) Uani 1 1 d . . . O4W O 0.1481(14) 0.4472(12) 0.5649(8) 0.358(9) Uani 1 1 d . . . H1 H -0.080(5) -0.443(5) 0.146(3) 0.051(13) Uiso 1 1 d . . . H2 H -0.042(4) -0.314(4) 0.225(3) 0.031(10) Uiso 1 1 d . . . H11 H -0.056(5) 0.333(5) 0.336(4) 0.053(12) Uiso 1 1 d . . . H12 H 0.021(5) 0.308(5) 0.261(4) 0.053(14) Uiso 1 1 d . . . H20 H -0.122(6) -0.148(5) -0.098(4) 0.043(17) Uiso 1 1 d . . . H30 H -0.243(4) -0.841(4) 0.578(3) 0.022(9) Uiso 1 1 d . . . H31 H -0.210(4) -0.966(4) 0.597(3) 0.033(10) Uiso 1 1 d . . . H32 H -0.103(5) -0.950(4) 0.455(3) 0.040(10) Uiso 1 1 d . . . H33 H -0.225(5) -1.089(5) 0.419(3) 0.047(12) Uiso 1 1 d . . . H34 H -0.292(5) -0.827(5) 0.378(3) 0.044(11) Uiso 1 1 d . . . H35 H -0.294(4) -0.963(4) 0.284(3) 0.036(10) Uiso 1 1 d . . . H36 H -0.637(6) -0.782(5) 0.526(3) 0.053(13) Uiso 1 1 d . . . H37 H -0.482(5) -0.723(5) 0.569(4) 0.043(13) Uiso 1 1 d . . . H38 H -0.594(5) -0.665(5) 0.415(3) 0.050(12) Uiso 1 1 d . . . H39 H -0.422(5) -0.683(4) 0.446(3) 0.033(10) Uiso 1 1 d . . . H40 H -0.661(5) -0.903(4) 0.301(3) 0.033(10) Uiso 1 1 d . . . H41 H -0.542(4) -0.835(4) 0.264(3) 0.035(10) Uiso 1 1 d . . . H42 H -0.532(5) -1.298(4) 0.065(3) 0.029(11) Uiso 1 1 d . . . H43 H -0.674(4) -1.307(3) 0.055(2) 0.016(8) Uiso 1 1 d . . . H44 H -0.623(4) -1.256(4) -0.016(3) 0.027(9) Uiso 1 1 d . . . H45 H -0.464(4) -1.056(4) 0.120(3) 0.034(9) Uiso 1 1 d . . . H46 H -0.640(4) -1.058(4) 0.106(3) 0.031(9) Uiso 1 1 d . . . H47 H -0.482(5) -1.182(4) 0.256(3) 0.045(12) Uiso 1 1 d . . . H48 H -0.632(4) -1.159(4) 0.248(3) 0.030(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0179(3) 0.0257(3) 0.0326(3) 0.0164(2) 0.0105(2) 0.0075(2) C1 0.0194(15) 0.0251(17) 0.0330(17) 0.0108(14) 0.0038(13) 0.0049(13) C2 0.0237(18) 0.043(2) 0.051(2) 0.032(2) 0.0114(17) 0.0070(16) C3 0.0191(15) 0.0370(19) 0.0391(18) 0.0190(15) 0.0116(14) 0.0050(14) O1 0.0242(12) 0.0294(12) 0.0535(15) 0.0230(11) 0.0186(11) 0.0105(10) O2 0.0214(12) 0.0353(13) 0.0561(15) 0.0288(12) 0.0171(11) 0.0090(10) O3 0.0291(13) 0.0325(14) 0.0703(18) 0.0254(13) 0.0166(13) 0.0134(11) O4 0.0228(13) 0.0520(17) 0.089(2) 0.0437(15) 0.0164(14) 0.0039(12) C11 0.039(2) 0.038(2) 0.0369(19) 0.0269(16) 0.0171(16) 0.0181(16) C12 0.042(2) 0.032(2) 0.046(2) 0.0134(18) 0.0141(19) 0.0070(18) C13 0.0204(16) 0.043(2) 0.0328(18) 0.0159(16) 0.0092(14) 0.0055(15) O11 0.0267(12) 0.0380(13) 0.0338(12) 0.0165(11) 0.0097(10) 0.0179(10) O12 0.0301(13) 0.0370(14) 0.0351(13) 0.0194(11) 0.0109(10) 0.0142(10) O13 0.067(2) 0.071(2) 0.0495(16) 0.0285(15) 0.0215(15) 0.0550(17) O14 0.0439(16) 0.0601(18) 0.0394(15) 0.0125(13) 0.0007(13) 0.0131(14) O20 0.0243(13) 0.0272(15) 0.0340(14) 0.0132(12) 0.0089(10) 0.0024(11) Ni1 0.0160(3) 0.0301(3) 0.0264(3) 0.0147(2) 0.0050(2) 0.0027(2) C31 0.0197(18) 0.072(3) 0.044(2) 0.032(2) 0.0133(16) 0.0084(19) C32 0.0190(16) 0.056(3) 0.038(2) 0.0250(18) 0.0089(15) 0.0030(16) C34 0.0306(19) 0.041(2) 0.0365(19) 0.0248(17) 0.0101(16) 0.0109(16) C33 0.047(2) 0.038(2) 0.043(2) 0.0216(18) 0.0140(19) 0.010(2) C35 0.0293(18) 0.038(2) 0.0298(17) 0.0153(15) 0.0082(15) 0.0074(16) C36 0.0281(18) 0.035(2) 0.0304(18) 0.0164(15) 0.0089(15) 0.0059(16) N31 0.0212(15) 0.047(2) 0.0344(17) 0.0210(16) 0.0017(13) 0.0021(14) N32 0.041(2) 0.0361(19) 0.0336(18) 0.0141(15) 0.0088(16) 0.0079(16) N33 0.0241(16) 0.045(2) 0.0304(17) 0.0189(15) 0.0064(13) 0.0099(15) N34 0.0168(13) 0.0356(16) 0.0276(13) 0.0151(12) 0.0050(11) 0.0048(11) O1W 0.085(3) 0.067(2) 0.077(2) 0.0283(18) 0.044(2) 0.0256(19) O2W 0.067(2) 0.0538(19) 0.092(2) 0.0411(17) 0.0260(19) 0.0111(16) O3W 0.118(4) 0.064(2) 0.099(3) 0.011(2) -0.022(3) -0.019(2) O4W 0.325(13) 0.298(11) 0.222(9) -0.160(8) -0.123(9) 0.227(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O20 1.945(3) . ? Cr1 O11 1.959(2) . ? Cr1 O20 1.963(3) 2 ? Cr1 O2 1.971(2) . ? Cr1 O1 1.972(2) . ? Cr1 O12 1.983(2) . ? C1 O3 1.250(4) . ? C1 O1 1.268(4) . ? C1 C2 1.499(5) . ? C2 C3 1.499(5) . ? C3 O4 1.246(4) . ? C3 O2 1.259(4) . ? C11 O11 1.247(4) . ? C11 O13 1.253(4) . ? C11 C12 1.494(5) . ? C12 C13 1.502(5) . ? C13 O14 1.230(4) . ? C13 O12 1.266(4) . ? O20 Cr1 1.963(3) 2 ? Ni1 N31 2.100(3) . ? Ni1 N31 2.100(3) 2_436 ? Ni1 N32 2.140(3) . ? Ni1 N32 2.140(3) 2_436 ? Ni1 N34 2.213(2) . ? Ni1 N34 2.213(2) 2_436 ? C31 N31 1.475(5) . ? C31 C32 1.500(5) . ? C32 N34 1.487(4) . ? C34 N34 1.482(4) . ? C34 C33 1.503(5) . ? C33 N32 1.479(5) . ? C35 N33 1.477(5) . ? C35 C36 1.524(5) . ? C36 N34 1.478(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 O20 Cr1 O11 89.21(11) . . ? O20 Cr1 O20 79.45(13) . 2 ? O11 Cr1 O20 95.43(11) . 2 ? O20 Cr1 O2 94.01(11) . . ? O11 Cr1 O2 85.86(10) . . ? O20 Cr1 O2 173.30(11) 2 . ? O20 Cr1 O1 92.20(11) . . ? O11 Cr1 O1 174.17(9) . . ? O20 Cr1 O1 90.38(11) 2 . ? O2 Cr1 O1 88.40(9) . . ? O20 Cr1 O12 172.10(11) . . ? O11 Cr1 O12 89.12(9) . . ? O20 Cr1 O12 93.03(11) 2 . ? O2 Cr1 O12 93.57(10) . . ? O1 Cr1 O12 90.23(10) . . ? O3 C1 O1 120.6(3) . . ? O3 C1 C2 119.0(3) . . ? O1 C1 C2 120.4(3) . . ? C3 C2 C1 118.5(3) . . ? O4 C3 O2 122.1(3) . . ? O4 C3 C2 117.9(3) . . ? O2 C3 C2 120.0(3) . . ? C1 O1 Cr1 129.4(2) . . ? C3 O2 Cr1 130.2(2) . . ? O11 C11 O13 121.4(3) . . ? O11 C11 C12 120.0(3) . . ? O13 C11 C12 118.6(3) . . ? C11 C12 C13 119.0(3) . . ? O14 C13 O12 121.6(3) . . ? O14 C13 C12 117.8(3) . . ? O12 C13 C12 120.6(3) . . ? C11 O11 Cr1 128.6(2) . . ? C13 O12 Cr1 125.9(2) . . ? Cr1 O20 Cr1 100.55(13) . 2 ? N31 Ni1 N31 180.0 . 2_436 ? N31 Ni1 N32 92.68(16) . . ? N31 Ni1 N32 87.32(16) 2_436 . ? N31 Ni1 N32 87.32(16) . 2_436 ? N31 Ni1 N32 92.68(16) 2_436 2_436 ? N32 Ni1 N32 180.00 . 2_436 ? N31 Ni1 N34 81.61(10) . . ? N31 Ni1 N34 98.39(10) 2_436 . ? N32 Ni1 N34 80.94(11) . . ? N32 Ni1 N34 99.06(11) 2_436 . ? N31 Ni1 N34 98.39(10) . 2_436 ? N31 Ni1 N34 81.61(10) 2_436 2_436 ? N32 Ni1 N34 99.06(11) . 2_436 ? N32 Ni1 N34 80.94(11) 2_436 2_436 ? N34 Ni1 N34 180.0 . 2_436 ? N31 C31 C32 109.3(3) . . ? N34 C32 C31 111.7(3) . . ? N34 C34 C33 111.4(3) . . ? N32 C33 C34 110.7(3) . . ? N33 C35 C36 109.3(3) . . ? N34 C36 C35 115.7(3) . . ? C31 N31 Ni1 106.5(2) . . ? C33 N32 Ni1 111.3(2) . . ? C36 N34 C34 110.6(3) . . ? C36 N34 C32 111.2(3) . . ? C34 N34 C32 110.8(3) . . ? C36 N34 Ni1 112.31(19) . . ? C34 N34 Ni1 104.79(19) . . ? C32 N34 Ni1 106.87(19) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.880 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.089 # Attachment 'compound1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 753109' #TrackingRef 'compound1.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H21 Gd O13' _chemical_formula_weight 470.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3c1' _symmetry_space_group_name_Hall 'P 3-2"c' _symmetry_Int_Tables_number 158 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, z+1/2' '-x+y, -x, z' 'x, x-y, z+1/2' '-x+y, y, z+1/2' _cell_length_a 8.6708(17) _cell_length_b 8.6708(29) _cell_length_c 11.4236(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 743.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 4.522 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.2649 _exptl_absorpt_correction_T_max 0.4966 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1987 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 6.50 _diffrn_reflns_theta_max 27.45 _reflns_number_total 864 _reflns_number_gt 713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-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)' _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^)+(0.0091P)^2^+0.4636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 864 _refine_ls_number_parameters 75 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0440 _refine_ls_wR_factor_gt 0.0413 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.6667 0.3333 0.92113(12) 0.02127(10) Uani 1 3 d S . . C1 C 0.8855(7) 0.2203(7) 1.0363(4) 0.0227(10) Uani 1 1 d . . . C2 C 1.0042(8) 0.1690(8) 1.1003(5) 0.0258(12) Uani 1 1 d . . . C3 C 1.0000 0.0000 1.0592(8) 0.0235(17) Uani 1 3 d S . . O1 O 0.8867(5) 0.3613(4) 1.0643(3) 0.0261(8) Uani 1 1 d . . . O2 O 0.7876(5) 0.1266(5) 0.9530(3) 0.0300(8) Uani 1 1 d . . . O1W O 0.8952(6) 0.3986(6) 0.7781(3) 0.0339(9) Uani 1 1 d . . . O2W O 1.3333 0.6667 1.1203(13) 0.138(6) Uani 1 3 d S . . O3W O 0.5786(8) -0.2170(7) 0.8540(5) 0.0690(15) Uani 1 1 d . . . H2A H 1.082(7) 0.255(7) 1.106(4) 0.012(14) Uiso 1 1 d . . . H2B H 0.971(9) 0.171(8) 1.178(5) 0.043(16) Uiso 1 1 d . . . H3 H 1.0000 0.0000 0.982(8) 0.02(2) Uiso 1 3 d S . . 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 Gd1 0.02102(12) 0.02102(12) 0.02175(15) 0.000 0.000 0.01051(6) C1 0.028(3) 0.024(3) 0.017(2) 0.004(2) 0.004(2) 0.014(2) C2 0.024(3) 0.018(3) 0.034(3) -0.005(2) -0.005(3) 0.009(3) C3 0.021(3) 0.021(3) 0.029(4) 0.000 0.000 0.0104(13) O1 0.036(2) 0.0173(19) 0.0308(18) -0.0053(16) -0.0020(17) 0.0182(18) O2 0.031(2) 0.028(2) 0.0343(19) -0.0060(16) -0.0075(17) 0.0178(18) O1W 0.034(3) 0.037(2) 0.032(2) 0.005(2) 0.006(2) 0.018(2) O2W 0.157(10) 0.157(10) 0.101(9) 0.000 0.000 0.078(5) O3W 0.073(4) 0.043(3) 0.102(4) -0.006(3) -0.018(3) 0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1W 2.408(4) 4_665 ? Gd1 O1W 2.408(4) . ? Gd1 O1W 2.408(4) 2_655 ? Gd1 O1 2.431(4) . ? Gd1 O1 2.431(4) 4_665 ? Gd1 O1 2.431(4) 2_655 ? Gd1 O2 2.515(4) . ? Gd1 O2 2.515(4) 2_655 ? Gd1 O2 2.515(4) 4_665 ? Gd1 C1 2.855(6) . ? Gd1 C1 2.855(6) 2_655 ? Gd1 C1 2.855(6) 4_665 ? C1 O1 1.259(6) . ? C1 O2 1.264(6) . ? C1 C2 1.500(7) . ? C2 C3 1.521(6) . ? C2 H2A 0.72(5) . ? C2 H2B 0.94(6) . ? C3 C2 1.521(6) 2_645 ? C3 C2 1.521(6) 4_765 ? C3 H3 0.88(9) . ? 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 O1W Gd1 O1W 78.98(17) 4_665 . ? O1W Gd1 O1W 78.98(17) 4_665 2_655 ? O1W Gd1 O1W 78.98(17) . 2_655 ? O1W Gd1 O1 130.39(14) 4_665 . ? O1W Gd1 O1 85.44(13) . . ? O1W Gd1 O1 143.25(14) 2_655 . ? O1W Gd1 O1 85.44(13) 4_665 4_665 ? O1W Gd1 O1 143.25(14) . 4_665 ? O1W Gd1 O1 130.39(14) 2_655 4_665 ? O1 Gd1 O1 79.70(14) . 4_665 ? O1W Gd1 O1 143.25(14) 4_665 2_655 ? O1W Gd1 O1 130.39(14) . 2_655 ? O1W Gd1 O1 85.44(13) 2_655 2_655 ? O1 Gd1 O1 79.70(14) . 2_655 ? O1 Gd1 O1 79.70(14) 4_665 2_655 ? O1W Gd1 O2 78.15(13) 4_665 . ? O1W Gd1 O2 71.22(13) . . ? O1W Gd1 O2 145.24(15) 2_655 . ? O1 Gd1 O2 52.26(11) . . ? O1 Gd1 O2 73.11(12) 4_665 . ? O1 Gd1 O2 127.66(14) 2_655 . ? O1W Gd1 O2 145.24(15) 4_665 2_655 ? O1W Gd1 O2 78.15(13) . 2_655 ? O1W Gd1 O2 71.22(13) 2_655 2_655 ? O1 Gd1 O2 73.11(12) . 2_655 ? O1 Gd1 O2 127.66(14) 4_665 2_655 ? O1 Gd1 O2 52.26(11) 2_655 2_655 ? O2 Gd1 O2 117.95(5) . 2_655 ? O1W Gd1 O2 71.22(13) 4_665 4_665 ? O1W Gd1 O2 145.24(15) . 4_665 ? O1W Gd1 O2 78.15(13) 2_655 4_665 ? O1 Gd1 O2 127.66(14) . 4_665 ? O1 Gd1 O2 52.26(11) 4_665 4_665 ? O1 Gd1 O2 73.11(12) 2_655 4_665 ? O2 Gd1 O2 117.95(4) . 4_665 ? O2 Gd1 O2 117.95(4) 2_655 4_665 ? O1W Gd1 C1 104.40(15) 4_665 . ? O1W Gd1 C1 77.49(15) . . ? O1W Gd1 C1 155.03(14) 2_655 . ? O1 Gd1 C1 25.99(12) . . ? O1 Gd1 C1 74.49(14) 4_665 . ? O1 Gd1 C1 103.66(15) 2_655 . ? O2 Gd1 C1 26.27(12) . . ? O2 Gd1 C1 95.76(14) 2_655 . ? O2 Gd1 C1 126.62(14) 4_665 . ? O1W Gd1 C1 155.03(13) 4_665 2_655 ? O1W Gd1 C1 104.40(15) . 2_655 ? O1W Gd1 C1 77.49(15) 2_655 2_655 ? O1 Gd1 C1 74.49(14) . 2_655 ? O1 Gd1 C1 103.66(15) 4_665 2_655 ? O1 Gd1 C1 25.99(12) 2_655 2_655 ? O2 Gd1 C1 126.62(14) . 2_655 ? O2 Gd1 C1 26.27(12) 2_655 2_655 ? O2 Gd1 C1 95.76(13) 4_665 2_655 ? C1 Gd1 C1 100.45(13) . 2_655 ? O1W Gd1 C1 77.49(15) 4_665 4_665 ? O1W Gd1 C1 155.03(13) . 4_665 ? O1W Gd1 C1 104.40(15) 2_655 4_665 ? O1 Gd1 C1 103.66(15) . 4_665 ? O1 Gd1 C1 25.99(12) 4_665 4_665 ? O1 Gd1 C1 74.49(14) 2_655 4_665 ? O2 Gd1 C1 95.76(14) . 4_665 ? O2 Gd1 C1 126.62(14) 2_655 4_665 ? O2 Gd1 C1 26.27(12) 4_665 4_665 ? C1 Gd1 C1 100.45(13) . 4_665 ? C1 Gd1 C1 100.45(13) 2_655 4_665 ? O1 C1 O2 119.5(5) . . ? O1 C1 C2 119.4(5) . . ? O2 C1 C2 121.1(5) . . ? O1 C1 Gd1 57.8(3) . . ? O2 C1 Gd1 61.7(3) . . ? C2 C1 Gd1 177.2(4) . . ? C1 C2 C3 116.5(5) . . ? C1 C2 H2A 99(4) . . ? C3 C2 H2A 126(4) . . ? C1 C2 H2B 101(4) . . ? C3 C2 H2B 117(4) . . ? H2A C2 H2B 92(5) . . ? C2 C3 C2 110.9(4) 2_645 . ? C2 C3 C2 110.9(4) 2_645 4_765 ? C2 C3 C2 110.9(4) . 4_765 ? C2 C3 H3 108.0(4) 2_645 . ? C2 C3 H3 108.0(4) . . ? C2 C3 H3 108.0(4) 4_765 . ? C1 O1 Gd1 96.2(3) . . ? C1 O2 Gd1 92.1(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.298 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.080