Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'Dr Konstantin V. Domasevitch' _publ_contact_author_address ; Department of Inorganic Chemistry Kiev University Volodimirska Str. 64 Kiev 252033 UKRAINE ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@anorgchemie.univ.kiev.ua _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Two-step construction of molecular and polymeric mixed-metal Cu(Co)/Be complexes employing functionality of a pyridyl substituted acetylacetonate ; loop_ _publ_author_name _publ_author_address 'Vreshch, Volodimir D.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; 'Chernega, Alexander N.' ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; 'Howard, Judith A.K.' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; 'Sieler, Joachim' ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; 'Domasevitch, Konstantin V.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; #============================================================================== _publ_section_acknowledgements ; KVD and JS acknowledge support from Deutsche Forschungsgemeinschaft; INTAS Fellowships 2002-310 (KVD), Royal Society Fellowship (ANCh). JAKH acknowledges the EPSRC for a Senior Research Fellowship. ; #============================================================================== data_d23 _database_code_CSD 200510 _audit_creation_method SHELXL _chemical_name_systematic ; Beryllium 3-(4-Pyridyl)-2,4-pentanedionate, Methanol Solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H24 Be N2 O5' _chemical_formula_weight 393.43 _chemical_melting_point ? _chemical_compound_source ? 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' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.6272(3) _cell_length_b 10.6028(3) _cell_length_c 11.3100(5) _cell_angle_alpha 94.020(2) _cell_angle_beta 114.8270(10) _cell_angle_gamma 102.1680(10) _cell_volume 1007.73(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method ? _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12286 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.50 _reflns_number_total 6048 _reflns_number_observed 4365 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 913 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+0.1799P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5135 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_obs 0.0519 _refine_ls_wR_factor_all 0.1647 _refine_ls_wR_factor_obs 0.1530 _refine_ls_goodness_of_fit_all 1.091 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Be1 Be 0.1054(2) 0.3955(2) 0.2881(2) 0.0240(3) Uani 1 d . . O1 O -0.05255(12) 0.27616(10) 0.22934(9) 0.0254(2) Uani 1 d . . O2 O 0.14709(11) 0.42033(9) 0.16590(9) 0.0237(2) Uani 1 d . . O3 O 0.24827(11) 0.36053(9) 0.40759(9) 0.0243(2) Uani 1 d . . O4 O 0.07771(12) 0.52518(10) 0.34641(9) 0.0250(2) Uani 1 d . . N1 N -0.30004(15) 0.00030(12) -0.37142(11) 0.0276(3) Uani 1 d . . N2 N 0.57513(14) 0.76108(12) 0.95621(11) 0.0272(3) Uani 1 d . . C1 C -0.1213(2) 0.21429(13) 0.10990(12) 0.0214(3) Uani 1 d . . C2 C -0.06519(15) 0.24400(12) 0.01605(12) 0.0198(2) Uani 1 d . . C3 C 0.06843(15) 0.35067(13) 0.05013(12) 0.0204(2) Uani 1 d . . C4 C 0.1225(2) 0.39113(14) -0.05100(13) 0.0255(3) Uani 1 d . . H4C H 0.2143(2) 0.46491(14) -0.01049(13) 0.031 Uiso 1 d R . H4B H 0.1489(2) 0.31947(14) -0.08594(13) 0.031 Uiso 1 d R . H4A H 0.0389(2) 0.41492(14) -0.12150(13) 0.031 Uiso 1 d R . C5 C -0.2667(2) 0.10503(14) 0.07674(14) 0.0266(3) Uani 1 d . . H5C H -0.2857(2) 0.10040(14) 0.15334(14) 0.032 Uiso 1 d R . H5B H -0.3564(2) 0.12170(14) 0.00596(14) 0.032 Uiso 1 d R . H5A H -0.2511(2) 0.02336(14) 0.04982(14) 0.032 Uiso 1 d R . C6 C -0.1600(2) -0.00733(14) -0.28011(13) 0.0270(3) Uani 1 d . . H6A H -0.1117(2) -0.06979(14) -0.30230(13) 0.032 Uiso 1 d R . C7 C -0.0797(2) 0.07089(14) -0.15514(13) 0.0242(3) Uani 1 d . . H7A H 0.0209(2) 0.06124(14) -0.09305(13) 0.029 Uiso 1 d R . C8 C -0.14564(15) 0.16251(12) -0.11933(12) 0.0207(2) Uani 1 d . . C9 C -0.2911(2) 0.17172(15) -0.21503(13) 0.0291(3) Uani 1 d . . H9A H -0.3419(2) 0.23385(15) -0.19627(13) 0.035 Uiso 1 d R . C10 C -0.3626(2) 0.0896(2) -0.33762(14) 0.0311(3) Uani 1 d . . H10A H -0.4627(2) 0.0977(2) -0.40220(14) 0.037 Uiso 1 d R . C11 C 0.32374(15) 0.43119(12) 0.52347(12) 0.0203(2) Uani 1 d . . C12 C 0.28698(15) 0.54538(12) 0.55878(12) 0.0199(2) Uani 1 d . . C13 C 0.1631(2) 0.58794(13) 0.46531(12) 0.0212(3) Uani 1 d . . C14 C 0.1225(2) 0.71015(14) 0.49884(14) 0.0280(3) Uani 1 d . . H14C H 0.0353(2) 0.72288(14) 0.42270(14) 0.034 Uiso 1 d R . H14B H 0.0933(2) 0.70177(14) 0.56989(14) 0.034 Uiso 1 d R . H14A H 0.2130(2) 0.78405(14) 0.52576(14) 0.034 Uiso 1 d R . C15 C 0.4571(2) 0.38633(14) 0.62154(13) 0.0258(3) Uani 1 d . . H15C H 0.4652(2) 0.30745(14) 0.58075(13) 0.031 Uiso 1 d R . H15B H 0.5547(2) 0.45336(14) 0.65091(13) 0.031 Uiso 1 d R . H15A H 0.4370(2) 0.36956(14) 0.69601(13) 0.031 Uiso 1 d R . C16 C 0.4588(2) 0.65327(14) 0.92904(13) 0.0280(3) Uani 1 d . . H16A H 0.4409(2) 0.62370(14) 1.00104(13) 0.034 Uiso 1 d R . C17 C 0.3609(2) 0.58134(14) 0.80232(13) 0.0260(3) Uani 1 d . . H17A H 0.2794(2) 0.50394(14) 0.78845(13) 0.031 Uiso 1 d R . C18 C 0.38365(15) 0.62198(12) 0.69615(12) 0.0208(2) Uani 1 d . . C19 C 0.5041(2) 0.73440(14) 0.72371(14) 0.0286(3) Uani 1 d . . H19A H 0.5252(2) 0.76591(14) 0.65380(14) 0.034 Uiso 1 d R . C20 C 0.5955(2) 0.80010(15) 0.85347(14) 0.0302(3) Uani 1 d . . H20A H 0.6774(2) 0.87822(15) 0.87012(14) 0.036 Uiso 1 d R . O5 O 0.2523(5) 0.2085(2) 0.7582(2) 0.0467(9) Uani 0.762(10) d P . O5A O 0.3488(16) 0.1724(14) 0.7776(7) 0.081(6) Uani 0.238(10) d P . C21 C 0.2208(2) 0.0973(2) 0.6671(2) 0.0465(4) Uani 1 d . . H1O H 0.3092(2) 0.1990(2) 0.8404(2) 0.056 Uiso 1 d R . H21A H 0.1994(2) 0.1172(2) 0.5802(2) 0.056 Uiso 1 d R . H21B H 0.1340(2) 0.0173(2) 0.6630(2) 0.056 Uiso 1 d R . H21C H 0.3189(2) 0.0574(2) 0.6963(2) 0.056 Uiso 1 d 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 Be1 0.0264(8) 0.0257(8) 0.0148(7) -0.0019(6) 0.0063(6) 0.0048(6) O1 0.0264(5) 0.0297(5) 0.0166(4) -0.0014(4) 0.0094(4) 0.0028(4) O2 0.0225(4) 0.0254(5) 0.0162(4) -0.0016(3) 0.0053(3) 0.0016(4) O3 0.0274(5) 0.0236(5) 0.0170(4) -0.0013(3) 0.0063(4) 0.0064(4) O4 0.0279(5) 0.0273(5) 0.0150(4) 0.0006(3) 0.0050(4) 0.0086(4) N1 0.0293(6) 0.0277(6) 0.0185(5) -0.0019(4) 0.0069(4) 0.0034(5) N2 0.0252(6) 0.0280(6) 0.0214(5) -0.0036(4) 0.0057(4) 0.0055(5) C1 0.0219(6) 0.0214(6) 0.0188(5) -0.0002(4) 0.0073(5) 0.0062(5) C2 0.0202(6) 0.0217(6) 0.0142(5) -0.0004(4) 0.0049(4) 0.0058(5) C3 0.0200(6) 0.0234(6) 0.0158(5) 0.0019(4) 0.0058(4) 0.0071(5) C4 0.0284(6) 0.0279(7) 0.0198(6) 0.0043(5) 0.0113(5) 0.0056(5) C5 0.0242(6) 0.0266(7) 0.0264(6) -0.0013(5) 0.0122(5) 0.0018(5) C6 0.0288(7) 0.0288(7) 0.0221(6) -0.0020(5) 0.0113(5) 0.0071(5) C7 0.0212(6) 0.0293(7) 0.0193(6) 0.0003(5) 0.0067(5) 0.0073(5) C8 0.0212(6) 0.0218(6) 0.0150(5) 0.0002(4) 0.0060(4) 0.0033(5) C9 0.0288(7) 0.0319(7) 0.0204(6) -0.0021(5) 0.0035(5) 0.0137(6) C10 0.0288(7) 0.0341(8) 0.0193(6) -0.0018(5) 0.0007(5) 0.0098(6) C11 0.0215(6) 0.0202(6) 0.0163(5) 0.0020(4) 0.0077(4) 0.0020(5) C12 0.0217(6) 0.0194(6) 0.0146(5) 0.0002(4) 0.0068(4) 0.0014(4) C13 0.0243(6) 0.0216(6) 0.0169(5) 0.0020(4) 0.0099(5) 0.0036(5) C14 0.0351(7) 0.0254(7) 0.0237(6) 0.0024(5) 0.0122(5) 0.0111(6) C15 0.0265(6) 0.0274(7) 0.0207(6) 0.0038(5) 0.0073(5) 0.0087(5) C16 0.0323(7) 0.0282(7) 0.0175(6) 0.0006(5) 0.0083(5) 0.0035(5) C17 0.0277(7) 0.0246(6) 0.0188(6) 0.0002(5) 0.0083(5) -0.0009(5) C18 0.0220(6) 0.0207(6) 0.0164(5) 0.0001(4) 0.0067(4) 0.0043(5) C19 0.0328(7) 0.0263(7) 0.0228(6) -0.0020(5) 0.0143(6) -0.0019(5) C20 0.0266(7) 0.0277(7) 0.0268(7) -0.0072(5) 0.0104(5) -0.0048(5) O5 0.068(2) 0.0447(11) 0.0233(8) 0.0032(6) 0.0182(9) 0.0124(10) O5A 0.068(8) 0.111(9) 0.028(3) -0.011(4) 0.026(4) -0.049(7) C21 0.0529(11) 0.0478(10) 0.0303(8) -0.0027(7) 0.0189(8) -0.0012(8) _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 Be1 O4 1.604(2) . ? Be1 O1 1.606(2) . ? Be1 O3 1.606(2) . ? Be1 O2 1.616(2) . ? O1 C1 1.2787(15) . ? O2 C3 1.2764(15) . ? O3 C11 1.2807(15) . ? O4 C13 1.2816(15) . ? N1 C6 1.334(2) . ? N1 C10 1.337(2) . ? N2 C16 1.333(2) . ? N2 C20 1.336(2) . ? C1 C2 1.405(2) . ? C1 C5 1.502(2) . ? C2 C3 1.411(2) . ? C2 C8 1.492(2) . ? C3 C4 1.496(2) . ? C6 C7 1.390(2) . ? C7 C8 1.390(2) . ? C8 C9 1.394(2) . ? C9 C10 1.390(2) . ? C11 C12 1.408(2) . ? C11 C15 1.497(2) . ? C12 C13 1.406(2) . ? C12 C18 1.493(2) . ? C13 C14 1.498(2) . ? C16 C17 1.390(2) . ? C17 C18 1.389(2) . ? C18 C19 1.387(2) . ? C19 C20 1.388(2) . ? O5 O5A 1.02(2) . ? O5 C21 1.400(3) . ? O5A C21 1.367(7) . ? 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 O4 Be1 O1 111.24(12) . . ? O4 Be1 O3 106.85(10) . . ? O1 Be1 O3 110.95(12) . . ? O4 Be1 O2 110.41(11) . . ? O1 Be1 O2 105.99(10) . . ? O3 Be1 O2 111.46(12) . . ? C1 O1 Be1 124.06(10) . . ? C3 O2 Be1 123.87(11) . . ? C11 O3 Be1 123.21(10) . . ? C13 O4 Be1 123.84(10) . . ? C6 N1 C10 116.47(11) . . ? C16 N2 C20 116.55(12) . . ? O1 C1 C2 123.06(12) . . ? O1 C1 C5 115.05(11) . . ? C2 C1 C5 121.88(11) . . ? C1 C2 C3 119.94(11) . . ? C1 C2 C8 120.24(11) . . ? C3 C2 C8 119.82(11) . . ? O2 C3 C2 122.95(11) . . ? O2 C3 C4 116.06(11) . . ? C2 C3 C4 120.96(11) . . ? N1 C6 C7 123.57(12) . . ? C6 C7 C8 120.00(12) . . ? C7 C8 C9 116.56(11) . . ? C7 C8 C2 121.14(11) . . ? C9 C8 C2 122.28(11) . . ? C10 C9 C8 119.44(13) . . ? N1 C10 C9 123.95(13) . . ? O3 C11 C12 123.09(11) . . ? O3 C11 C15 116.02(11) . . ? C12 C11 C15 120.89(11) . . ? C13 C12 C11 120.47(11) . . ? C13 C12 C18 120.57(11) . . ? C11 C12 C18 118.95(11) . . ? O4 C13 C12 122.47(11) . . ? O4 C13 C14 115.64(11) . . ? C12 C13 C14 121.89(11) . . ? N2 C16 C17 123.88(12) . . ? C18 C17 C16 119.23(12) . . ? C19 C18 C17 117.17(11) . . ? C19 C18 C12 121.21(11) . . ? C17 C18 C12 121.58(11) . . ? C18 C19 C20 119.54(12) . . ? N2 C20 C19 123.64(13) . . ? O5A O5 C21 66.6(4) . . ? O5 O5A C21 70.0(7) . . ? O5A C21 O5 43.4(7) . . ? _refine_diff_density_max 0.378 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.054 #============================================================================== data_st13 _database_code_CSD 200511 _audit_creation_method SHELXL _chemical_name_systematic ; Cobalt(I) Chloride 1:2 Complex with Beryllium 3-(4-Pyridyl)-2,4-pentanedionate, monohydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H42 Be2 Cl2 Co N4 O9' _chemical_formula_weight 870.63 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.473(2) _cell_length_b 11.2165(5) _cell_length_c 13.7859(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.000(8) _cell_angle_gamma 90.00 _cell_volume 4139.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method ? _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'IPDS Stoe' _diffrn_measurement_method 'phi rotation' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12187 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.04 _reflns_number_total 4881 _reflns_number_observed 3172 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 346 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4535 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_obs 0.0457 _refine_ls_wR_factor_all 0.1231 _refine_ls_wR_factor_obs 0.1111 _refine_ls_goodness_of_fit_all 0.905 _refine_ls_goodness_of_fit_obs 1.033 _refine_ls_restrained_S_all 0.911 _refine_ls_restrained_S_obs 1.033 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 -0.40339(5) -0.2500 0.03069(14) Uani 1 d S . Be1 Be 0.30263(11) 0.0102(3) 0.0905(3) 0.0299(6) Uani 1 d . . Cl1 Cl 0.55702(2) -0.50154(7) -0.13681(6) 0.0443(2) Uani 1 d . . O1 O 0.25975(6) 0.0736(2) 0.00613(13) 0.0309(4) Uani 1 d . . O2 O 0.28918(6) 0.0396(2) 0.19537(13) 0.0335(4) Uani 1 d . . O3 O 0.30260(6) -0.1313(2) 0.06853(14) 0.0308(4) Uani 1 d . . O4 O 0.35777(6) 0.0570(2) 0.08856(14) 0.0322(4) Uani 1 d . . O5 O 0.0000 0.4076(3) 0.2500 0.0613(10) Uani 1 d S . N1 N 0.46325(7) -0.3003(2) -0.1680(2) 0.0312(4) Uani 1 d . . N2 N 0.07705(8) 0.2705(2) 0.1860(2) 0.0458(6) Uani 1 d . . C1 C 0.21907(8) 0.1166(2) 0.0230(2) 0.0277(5) Uani 1 d . . C2 C 0.21087(8) 0.1248(2) 0.1200(2) 0.0292(5) Uani 1 d . . C3 C 0.24759(8) 0.0880(2) 0.2022(2) 0.0303(5) Uani 1 d . . C4 C 0.24097(11) 0.1019(3) 0.3066(2) 0.0452(7) Uani 1 d . . H4A H 0.27006(11) 0.0707(3) 0.3515(2) 0.054 Uiso 1 d R . H4B H 0.23724(11) 0.1847(3) 0.3208(2) 0.054 Uiso 1 d R . H4C H 0.21196(11) 0.0588(3) 0.3148(2) 0.054 Uiso 1 d R . C5 C 0.18135(9) 0.1579(2) -0.0655(2) 0.0349(5) Uani 1 d . . H5A H 0.19359(9) 0.1447(2) -0.1246(2) 0.042 Uiso 1 d R . H5B H 0.15087(9) 0.1142(2) -0.0700(2) 0.042 Uiso 1 d R . H5C H 0.17514(9) 0.2414(2) -0.0590(2) 0.042 Uiso 1 d R . C6 C 0.07796(10) 0.1617(3) 0.1489(2) 0.0448(7) Uani 1 d . . H6A H 0.04792(10) 0.1151(3) 0.1385(2) 0.054 Uiso 1 d R . C7 C 0.11942(9) 0.1115(3) 0.1240(2) 0.0404(6) Uani 1 d . . H7A H 0.11824(9) 0.0320(3) 0.0978(2) 0.048 Uiso 1 d R . C8 C 0.16347(8) 0.1774(2) 0.1381(2) 0.0304(5) Uani 1 d . . C9 C 0.16226(9) 0.2927(3) 0.1740(2) 0.0397(6) Uani 1 d . . H9A H 0.19127(9) 0.3428(3) 0.1829(2) 0.048 Uiso 1 d R . C10 C 0.11901(10) 0.3340(3) 0.1977(3) 0.0460(7) Uani 1 d . . H10A H 0.11897(10) 0.4133(3) 0.2239(3) 0.055 Uiso 1 d R . C11 C 0.33402(8) -0.1786(2) 0.0240(2) 0.0268(5) Uani 1 d . . C12 C 0.37483(8) -0.1146(2) 0.0035(2) 0.0274(5) Uani 1 d . . C13 C 0.38650(8) -0.0010(2) 0.0435(2) 0.0286(5) Uani 1 d . . C14 C 0.43470(9) 0.0598(3) 0.0410(2) 0.0390(6) Uani 1 d . . H14A H 0.43549(9) 0.1367(3) 0.0720(2) 0.047 Uiso 1 d R . H14B H 0.46194(9) 0.0123(3) 0.0767(2) 0.047 Uiso 1 d R . H14C H 0.43772(9) 0.0695(3) -0.0266(2) 0.047 Uiso 1 d R . C15 C 0.32607(10) -0.3078(2) -0.0019(2) 0.0395(6) Uani 1 d . . H15A H 0.29666(10) -0.3363(2) 0.0173(2) 0.047 Uiso 1 d R . H15B H 0.32235(10) -0.3184(2) -0.0723(2) 0.047 Uiso 1 d R . H15C H 0.35462(10) -0.3519(2) 0.0331(2) 0.047 Uiso 1 d R . C16 C 0.42263(10) -0.2382(3) -0.2129(2) 0.0389(6) Uani 1 d . . H16A H 0.41315(10) -0.2376(3) -0.2843(2) 0.047 Uiso 1 d R . C17 C 0.39440(9) -0.1745(3) -0.1584(2) 0.0379(6) Uani 1 d . . H17A H 0.36593(9) -0.1294(3) -0.1923(2) 0.045 Uiso 1 d R . C18 C 0.40722(8) -0.1759(2) -0.0558(2) 0.0276(5) Uani 1 d . . C19 C 0.44975(9) -0.2387(3) -0.0093(2) 0.0362(6) Uani 1 d . . H19A H 0.46022(9) -0.2395(3) 0.0620(2) 0.043 Uiso 1 d R . C20 C 0.47615(9) -0.2997(3) -0.0690(2) 0.0363(6) Uani 1 d . . H20A H 0.50531(9) -0.3436(3) -0.0367(2) 0.044 Uiso 1 d R . H1O H 0.0210(14) 0.3615(37) 0.2297(32) 0.070(12) Uiso 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 Co1 0.0287(2) 0.0363(3) 0.0300(3) 0.000 0.0127(2) 0.000 Be1 0.0283(13) 0.032(2) 0.030(2) -0.0012(13) 0.0084(12) 0.0026(12) Cl1 0.0402(3) 0.0498(4) 0.0424(4) 0.0056(3) 0.0084(3) 0.0088(3) O1 0.0299(8) 0.0381(10) 0.0259(9) -0.0024(7) 0.0087(7) 0.0061(7) O2 0.0309(8) 0.0433(11) 0.0268(9) -0.0014(8) 0.0070(7) 0.0091(7) O3 0.0263(7) 0.0327(9) 0.0371(10) -0.0021(7) 0.0151(7) 0.0016(6) O4 0.0290(7) 0.0303(9) 0.0390(10) -0.0067(7) 0.0110(7) 0.0014(7) O5 0.047(2) 0.061(2) 0.085(3) 0.000 0.036(2) 0.000 N1 0.0295(9) 0.0359(12) 0.0308(11) 0.0008(9) 0.0121(8) 0.0008(8) N2 0.0369(11) 0.061(2) 0.0438(15) 0.0072(12) 0.0176(10) 0.0111(11) C1 0.0277(10) 0.0279(13) 0.0277(12) -0.0022(9) 0.0063(9) -0.0005(8) C2 0.0287(10) 0.0313(13) 0.0293(13) -0.0024(9) 0.0096(9) 0.0018(9) C3 0.0307(10) 0.0332(13) 0.0287(12) -0.0024(10) 0.0099(9) 0.0020(9) C4 0.0498(15) 0.060(2) 0.0287(14) 0.0014(13) 0.0145(12) 0.0145(14) C5 0.0368(12) 0.0355(14) 0.0315(14) 0.0021(11) 0.0060(10) 0.0047(10) C6 0.0322(12) 0.057(2) 0.048(2) 0.0099(14) 0.0137(12) -0.0018(12) C7 0.0353(12) 0.043(2) 0.044(2) 0.0004(12) 0.0115(11) -0.0020(11) C8 0.0278(10) 0.0370(14) 0.0273(12) -0.0018(10) 0.0084(9) 0.0021(9) C9 0.0319(12) 0.041(2) 0.046(2) -0.0100(12) 0.0103(11) 0.0011(11) C10 0.0404(13) 0.048(2) 0.051(2) -0.0085(14) 0.0115(12) 0.0143(12) C11 0.0264(10) 0.0289(12) 0.0259(12) 0.0004(9) 0.0078(9) 0.0035(8) C12 0.0248(9) 0.0302(13) 0.0288(12) -0.0010(9) 0.0096(9) 0.0013(9) C13 0.0259(10) 0.0315(13) 0.0293(12) 0.0012(10) 0.0084(9) 0.0008(9) C14 0.0316(11) 0.0388(15) 0.049(2) -0.0059(12) 0.0147(11) -0.0076(10) C15 0.0391(12) 0.0310(14) 0.054(2) -0.0056(12) 0.0220(12) -0.0029(10) C16 0.0432(13) 0.051(2) 0.0247(13) 0.0014(11) 0.0114(10) 0.0119(12) C17 0.0378(12) 0.046(2) 0.0320(14) 0.0039(11) 0.0117(11) 0.0119(11) C18 0.0265(10) 0.0280(12) 0.0308(12) -0.0016(9) 0.0117(9) -0.0010(9) C19 0.0345(12) 0.049(2) 0.0256(13) -0.0022(11) 0.0081(10) 0.0110(11) C20 0.0324(11) 0.047(2) 0.0309(14) -0.0015(11) 0.0099(10) 0.0099(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.037(2) . ? Co1 N1 2.037(2) 2_654 ? Co1 Cl1 2.2363(7) 2_654 ? Co1 Cl1 2.2363(7) . ? Be1 O2 1.605(4) . ? Be1 O4 1.609(3) . ? Be1 O3 1.616(4) . ? Be1 O1 1.621(4) . ? O1 C1 1.286(3) . ? O2 C3 1.288(3) . ? O3 C11 1.281(3) . ? O4 C13 1.286(3) . ? N1 C20 1.330(3) . ? N1 C16 1.342(3) . ? N2 C6 1.325(4) . ? N2 C10 1.334(4) . ? C1 C2 1.408(3) . ? C1 C5 1.486(4) . ? C2 C3 1.399(4) . ? C2 C8 1.501(3) . ? C3 C4 1.498(4) . ? C6 C7 1.381(4) . ? C7 C8 1.394(3) . ? C8 C9 1.388(4) . ? C9 C10 1.381(3) . ? C11 C12 1.412(3) . ? C11 C15 1.497(4) . ? C12 C13 1.397(3) . ? C12 C18 1.503(3) . ? C13 C14 1.497(3) . ? C16 C17 1.393(3) . ? C17 C18 1.379(4) . ? C18 C19 1.391(3) . ? C19 C20 1.393(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 110.81(12) . 2_654 ? N1 Co1 Cl1 108.06(6) . 2_654 ? N1 Co1 Cl1 104.42(6) 2_654 2_654 ? N1 Co1 Cl1 104.42(6) . . ? N1 Co1 Cl1 108.06(6) 2_654 . ? Cl1 Co1 Cl1 121.02(5) 2_654 . ? O2 Be1 O4 110.9(2) . . ? O2 Be1 O3 112.3(2) . . ? O4 Be1 O3 106.1(2) . . ? O2 Be1 O1 106.2(2) . . ? O4 Be1 O1 112.3(2) . . ? O3 Be1 O1 109.1(2) . . ? C1 O1 Be1 123.7(2) . . ? C3 O2 Be1 122.7(2) . . ? C11 O3 Be1 121.6(2) . . ? C13 O4 Be1 121.7(2) . . ? C20 N1 C16 118.2(2) . . ? C20 N1 Co1 121.4(2) . . ? C16 N1 Co1 120.2(2) . . ? C6 N2 C10 116.6(2) . . ? O1 C1 C2 121.8(2) . . ? O1 C1 C5 116.3(2) . . ? C2 C1 C5 121.9(2) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 C8 118.4(2) . . ? C1 C2 C8 120.9(2) . . ? O2 C3 C2 123.7(2) . . ? O2 C3 C4 114.6(2) . . ? C2 C3 C4 121.7(2) . . ? N2 C6 C7 124.0(3) . . ? C6 C7 C8 119.2(3) . . ? C9 C8 C7 117.0(2) . . ? C9 C8 C2 121.1(2) . . ? C7 C8 C2 121.8(2) . . ? C10 C9 C8 119.2(3) . . ? N2 C10 C9 123.9(3) . . ? O3 C11 C12 122.4(2) . . ? O3 C11 C15 115.9(2) . . ? C12 C11 C15 121.6(2) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 C18 121.3(2) . . ? C11 C12 C18 118.1(2) . . ? O4 C13 C12 122.7(2) . . ? O4 C13 C14 115.0(2) . . ? C12 C13 C14 122.2(2) . . ? N1 C16 C17 121.6(3) . . ? C18 C17 C16 120.2(2) . . ? C17 C18 C19 118.2(2) . . ? C17 C18 C12 120.4(2) . . ? C19 C18 C12 121.3(2) . . ? C18 C19 C20 118.2(3) . . ? N1 C20 C19 123.6(2) . . ? _refine_diff_density_max 0.350 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.067 #============================================================================== data_c1239 _database_code_CSD 200512 _audit_creation_method SHELXL _chemical_name_systematic ; Bis-Methanol Cobalt(II) Sulfate Complex with Beryllium 3-(4-Pyridyl)-2,4-pentanedionate, Solvate with 1 Methanol and 1 Water ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H34 Be Co N2 O12 S' _chemical_formula_weight 630.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5489(10) _cell_length_b 10.7797(12) _cell_length_c 15.7127(13) _cell_angle_alpha 82.427(4) _cell_angle_beta 86.698(5) _cell_angle_gamma 71.158(5) _cell_volume 1517.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method ? _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8474 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.52 _reflns_number_total 5018 _reflns_number_observed 4477 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 296 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+2.8722P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4722 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_obs 0.0645 _refine_ls_wR_factor_all 0.1789 _refine_ls_wR_factor_obs 0.1480 _refine_ls_goodness_of_fit_all 1.121 _refine_ls_goodness_of_fit_obs 1.129 _refine_ls_restrained_S_all 1.370 _refine_ls_restrained_S_obs 1.129 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.0000 0.0308(2) Uani 1 d S . Co2 Co 0.0000 -0.5000 0.0000 0.0245(2) Uani 1 d S . Be1 Be -0.3197(7) 0.1710(8) 0.5625(4) 0.048(2) Uani 1 d . . S1 S 0.20892(11) -0.31278(11) 0.05579(6) 0.0300(3) Uani 1 d . . O1 O -0.1683(3) 0.1902(3) 0.5199(2) 0.0382(7) Uani 1 d . . O2 O -0.3521(7) 0.0671(8) 0.5101(3) 0.119(3) Uani 1 d . . O3 O -0.4506(4) 0.3077(5) 0.5548(2) 0.077(2) Uani 1 d . . O4 O -0.3095(4) 0.1168(3) 0.6624(2) 0.0435(8) Uani 1 d . . O5 O 0.1697(3) -0.1678(3) 0.0435(2) 0.0347(7) Uani 1 d . . O6 O 0.0922(3) -0.3486(3) 0.0138(2) 0.0326(7) Uani 1 d . . O7 O 0.3530(3) -0.3706(3) 0.0159(2) 0.0411(8) Uani 1 d . . O8 O 0.2114(4) -0.3586(4) 0.1478(2) 0.0490(9) Uani 1 d . . O9 O 0.1418(3) 0.1104(3) 0.0101(2) 0.0384(7) Uani 1 d . . O10 O 0.1473(3) -0.6397(3) 0.0854(2) 0.0357(7) Uani 1 d . . O11 O 0.4359(5) -0.6920(8) 0.0994(3) 0.107(2) Uani 1 d . . N1 N -0.0716(4) 0.0305(4) 0.1334(2) 0.0374(9) Uani 1 d . . N2 N -0.8439(4) 0.4333(3) 0.8973(2) 0.0286(7) Uani 1 d . . C1 C -0.1257(5) 0.1624(5) 0.4435(3) 0.0354(10) Uani 1 d . . C2 C -0.1928(6) 0.0977(6) 0.3960(3) 0.0504(14) Uani 1 d . . C3 C -0.2986(10) 0.0457(12) 0.4343(5) 0.117(4) Uani 1 d . . C4 C -0.3541(19) -0.0435(22) 0.3927(9) 0.299(16) Uani 1 d . . H4A H -0.4284(19) -0.0684(22) 0.4279(9) 0.080 Uiso 1 d R . H4B H -0.3952(19) 0.0000(22) 0.3382(9) 0.080 Uiso 1 d R . H4C H -0.2722(19) -0.1209(22) 0.3841(9) 0.080 Uiso 1 d R . C5 C 0.0025(7) 0.2031(7) 0.4077(4) 0.058(2) Uani 1 d . . H5A H 0.0819(7) 0.1240(7) 0.3990(4) 0.080 Uiso 1 d R . H5B H 0.0366(7) 0.2483(7) 0.4466(4) 0.080 Uiso 1 d R . H5C H -0.0183(7) 0.2564(7) 0.3531(4) 0.080 Uiso 1 d R . C6 C -0.1818(6) 0.1355(6) 0.1531(3) 0.0478(12) Uani 1 d . . H6A H -0.2373(6) 0.1957(6) 0.1072(3) 0.080 Uiso 1 d R . C7 C -0.2203(6) 0.1607(6) 0.2380(3) 0.0529(14) Uani 1 d . . H7A H -0.2982(6) 0.2396(6) 0.2490(3) 0.080 Uiso 1 d R . C8 C -0.1469(5) 0.0759(6) 0.3048(3) 0.0470(13) Uani 1 d . . C9 C -0.0332(6) -0.0334(7) 0.2848(3) 0.062(2) Uani 1 d . . H9A H 0.0227(6) -0.0960(7) 0.3296(3) 0.080 Uiso 1 d R . C10 C -0.0004(6) -0.0536(7) 0.1993(3) 0.056(2) Uani 1 d . . H10A H 0.0776(6) -0.1315(7) 0.1868(3) 0.080 Uiso 1 d R . C11 C -0.5402(6) 0.3506(7) 0.6167(3) 0.062(2) Uani 1 d . . C12 C -0.5268(5) 0.2813(5) 0.6992(2) 0.0316(9) Uani 1 d . . C13 C -0.4084(5) 0.1653(5) 0.7182(3) 0.0338(10) Uani 1 d . . C14 C -0.3906(6) 0.0900(6) 0.8058(3) 0.0520(13) Uani 1 d . . H14A H -0.3036(6) 0.0139(6) 0.8068(3) 0.080 Uiso 1 d R . H14B H -0.3809(6) 0.1458(6) 0.8465(3) 0.080 Uiso 1 d R . H14C H -0.4758(6) 0.0624(6) 0.8208(3) 0.080 Uiso 1 d R . C15 C -0.6577(10) 0.4750(11) 0.5953(5) 0.132(5) Uani 1 d . . H15A H -0.6485(10) 0.5079(11) 0.5361(5) 0.080 Uiso 1 d R . H15B H -0.7513(10) 0.4598(11) 0.6048(5) 0.080 Uiso 1 d R . H15C H -0.6519(10) 0.5388(11) 0.6311(5) 0.080 Uiso 1 d R . C16 C -0.7043(4) 0.4357(4) 0.8977(3) 0.0308(9) Uani 1 d . . H16A H -0.6757(4) 0.4720(4) 0.9439(3) 0.080 Uiso 1 d R . C17 C -0.5996(5) 0.3886(5) 0.8351(3) 0.0341(10) Uani 1 d . . H17A H -0.5012(5) 0.3930(5) 0.8382(3) 0.080 Uiso 1 d R . C18 C -0.6369(4) 0.3342(4) 0.7681(2) 0.0287(9) Uani 1 d . . C19 C -0.7809(5) 0.3320(5) 0.7678(3) 0.0396(11) Uani 1 d . . H19A H -0.8125(5) 0.2964(5) 0.7223(3) 0.080 Uiso 1 d R . C20 C -0.8794(5) 0.3811(5) 0.8320(3) 0.0366(10) Uani 1 d . . H20A H -0.9784(5) 0.3777(5) 0.8300(3) 0.080 Uiso 1 d R . C21 C 0.2893(5) 0.0836(5) -0.0227(3) 0.0450(11) Uani 1 d . . H21A H 0.3396(5) -0.0097(5) -0.0126(3) 0.080 Uiso 1 d R . H21B H 0.3414(5) 0.1292(5) 0.0052(3) 0.080 Uiso 1 d R . H21C H 0.2892(5) 0.1116(5) -0.0833(3) 0.080 Uiso 1 d R . C22 C 0.1098(6) -0.6997(5) 0.1669(3) 0.0439(11) Uani 1 d . . H22A H 0.1873(6) -0.7798(5) 0.1849(3) 0.080 Uiso 1 d R . H22B H 0.0188(6) -0.7178(5) 0.1616(3) 0.080 Uiso 1 d R . H22C H 0.0939(6) -0.6387(5) 0.2086(3) 0.080 Uiso 1 d R . O12 O 0.3932(17) -0.5912(17) 0.2434(10) 0.073(4) Uani 0.33 d P . C23 C 0.3675(29) -0.5974(21) 0.3278(12) 0.081(7) Uani 0.33 d P . O12A O 0.2277(25) -0.4896(21) 0.3009(9) 0.127(9) Uani 0.33 d P . C23A C 0.0861(73) -0.4009(29) 0.3882(42) 0.306(49) Uani 0.33 d P . O12B O 0.4388(17) -0.6929(20) 0.2776(10) 0.080(4) Uani 0.33 d P . C23B C 0.4143(26) -0.7904(28) 0.3397(16) 0.086(7) Uani 0.33 d P . H1 H 0.0999 0.2000 -0.0017 0.050 Uiso 1 d . . H2 H 0.2439 -0.6383 0.0805 0.050 Uiso 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 Co1 0.0247(4) 0.0435(5) 0.0272(4) -0.0213(3) 0.0079(3) -0.0098(3) Co2 0.0196(4) 0.0332(5) 0.0206(4) -0.0119(3) 0.0049(3) -0.0056(3) Be1 0.038(3) 0.083(5) 0.033(3) -0.031(3) 0.018(3) -0.027(3) S1 0.0219(5) 0.0425(6) 0.0288(5) -0.0176(4) 0.0038(4) -0.0100(4) O1 0.033(2) 0.057(2) 0.0303(15) -0.0241(14) 0.0116(12) -0.0161(14) O2 0.125(4) 0.226(7) 0.086(3) -0.119(4) 0.088(3) -0.142(5) O3 0.042(2) 0.134(4) 0.022(2) 0.000(2) 0.0134(15) 0.013(2) O4 0.038(2) 0.050(2) 0.039(2) -0.0200(15) 0.0187(14) -0.0062(15) O5 0.0264(14) 0.045(2) 0.038(2) -0.0240(14) 0.0028(12) -0.0105(13) O6 0.0273(15) 0.041(2) 0.0325(15) -0.0136(13) 0.0016(12) -0.0123(13) O7 0.0235(15) 0.051(2) 0.052(2) -0.030(2) 0.0082(13) -0.0086(14) O8 0.039(2) 0.080(3) 0.031(2) -0.008(2) -0.0039(14) -0.022(2) O9 0.029(2) 0.042(2) 0.047(2) -0.0187(14) 0.0054(13) -0.0107(13) O10 0.0275(15) 0.049(2) 0.0307(15) -0.0040(13) 0.0028(12) -0.0129(13) O11 0.033(2) 0.200(7) 0.070(3) 0.035(4) -0.008(2) -0.031(3) N1 0.029(2) 0.056(2) 0.031(2) -0.024(2) 0.0076(15) -0.011(2) N2 0.025(2) 0.036(2) 0.024(2) -0.0131(14) 0.0061(13) -0.0075(14) C1 0.032(2) 0.043(3) 0.029(2) -0.013(2) 0.009(2) -0.008(2) C2 0.043(3) 0.083(4) 0.039(3) -0.039(3) 0.021(2) -0.029(3) C3 0.117(6) 0.230(11) 0.083(5) -0.117(6) 0.078(5) -0.138(8) C4 0.337(21) 0.601(36) 0.207(13) -0.331(21) 0.243(15) -0.422(26) C5 0.064(3) 0.079(4) 0.051(3) -0.034(3) 0.029(3) -0.044(3) C6 0.047(3) 0.054(3) 0.040(3) -0.020(2) 0.017(2) -0.009(2) C7 0.053(3) 0.063(4) 0.044(3) -0.032(3) 0.023(2) -0.013(3) C8 0.036(2) 0.078(4) 0.037(3) -0.034(3) 0.016(2) -0.025(2) C9 0.042(3) 0.103(5) 0.029(2) -0.030(3) 0.007(2) 0.003(3) C10 0.040(3) 0.088(4) 0.032(2) -0.032(3) 0.007(2) 0.001(3) C11 0.040(3) 0.090(4) 0.028(2) -0.002(3) 0.011(2) 0.013(3) C12 0.028(2) 0.043(2) 0.022(2) -0.016(2) 0.008(2) -0.007(2) C13 0.032(2) 0.039(2) 0.032(2) -0.016(2) 0.012(2) -0.011(2) C14 0.049(3) 0.050(3) 0.043(3) -0.002(2) 0.018(2) 0.000(2) C15 0.085(5) 0.155(9) 0.060(4) 0.050(5) 0.035(4) 0.061(6) C16 0.026(2) 0.041(2) 0.028(2) -0.015(2) 0.007(2) -0.011(2) C17 0.023(2) 0.046(3) 0.034(2) -0.015(2) 0.009(2) -0.010(2) C18 0.026(2) 0.035(2) 0.023(2) -0.010(2) 0.0054(15) -0.005(2) C19 0.030(2) 0.065(3) 0.028(2) -0.025(2) 0.007(2) -0.015(2) C20 0.025(2) 0.061(3) 0.028(2) -0.018(2) 0.005(2) -0.016(2) C21 0.031(2) 0.050(3) 0.054(3) -0.005(2) 0.008(2) -0.014(2) C22 0.046(3) 0.051(3) 0.034(2) -0.006(2) 0.003(2) -0.014(2) O12 0.076(9) 0.068(9) 0.068(9) -0.003(7) -0.005(7) -0.016(8) C23 0.115(18) 0.061(12) 0.036(9) 0.011(8) -0.032(10) 0.010(12) O12A 0.152(17) 0.114(14) 0.043(8) 0.009(8) 0.043(9) 0.045(12) C23A 0.450(83) 0.070(18) 0.432(79) 0.104(31) -0.438(80) -0.109(32) O12B 0.069(9) 0.096(12) 0.065(9) 0.006(9) 0.000(7) -0.017(9) C23B 0.064(13) 0.109(19) 0.079(14) 0.007(13) -0.006(11) -0.027(13) _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 Co1 O5 2.067(3) 2 ? Co1 O5 2.067(3) . ? Co1 O9 2.095(3) . ? Co1 O9 2.095(3) 2 ? Co1 N1 2.200(3) 2 ? Co1 N1 2.200(3) . ? Co2 O10 2.089(3) 2_545 ? Co2 O10 2.089(3) . ? Co2 O6 2.128(3) . ? Co2 O6 2.128(3) 2_545 ? Co2 N2 2.163(3) 1_644 ? Co2 N2 2.163(3) 2_456 ? Be1 O2 1.589(8) . ? Be1 O3 1.590(9) . ? Be1 O4 1.598(8) . ? Be1 O1 1.621(7) . ? S1 O7 1.457(3) . ? S1 O8 1.464(3) . ? S1 O5 1.474(3) . ? S1 O6 1.502(3) . ? O1 C1 1.288(5) . ? O2 C3 1.288(7) . ? O3 C11 1.288(6) . ? O4 C13 1.281(5) . ? O9 C21 1.424(5) . ? O10 C22 1.436(6) . ? N1 C6 1.331(6) . ? N1 C10 1.339(7) . ? N2 C20 1.341(5) . ? N2 C16 1.342(5) . ? N2 Co2 2.163(3) 1_466 ? C1 C2 1.390(6) . ? C1 C5 1.487(7) . ? C2 C3 1.379(8) . ? C2 C8 1.502(6) . ? C3 C4 1.472(10) . ? C6 C7 1.400(7) . ? C7 C8 1.358(8) . ? C8 C9 1.378(8) . ? C9 C10 1.390(6) . ? C11 C12 1.399(7) . ? C11 C15 1.457(9) . ? C12 C13 1.399(6) . ? C12 C18 1.499(5) . ? C13 C14 1.493(7) . ? C16 C17 1.384(5) . ? C17 C18 1.386(6) . ? C18 C19 1.383(6) . ? C19 C20 1.376(6) . ? O12 O12B 1.12(2) . ? O12 C23 1.33(2) . ? C23 O12B 1.36(3) . ? C23 O12A 1.50(3) . ? C23 C23B 1.97(4) . ? O12B C23B 1.41(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 O5 Co1 O5 180.0 2 . ? O5 Co1 O9 91.59(12) 2 . ? O5 Co1 O9 88.41(12) . . ? O5 Co1 O9 88.41(12) 2 2 ? O5 Co1 O9 91.59(12) . 2 ? O9 Co1 O9 180.0 . 2 ? O5 Co1 N1 89.98(13) 2 2 ? O5 Co1 N1 90.02(13) . 2 ? O9 Co1 N1 92.12(13) . 2 ? O9 Co1 N1 87.88(13) 2 2 ? O5 Co1 N1 90.02(13) 2 . ? O5 Co1 N1 89.98(13) . . ? O9 Co1 N1 87.88(13) . . ? O9 Co1 N1 92.12(13) 2 . ? N1 Co1 N1 180.0 2 . ? O10 Co2 O10 180.0 2_545 . ? O10 Co2 O6 86.32(12) 2_545 . ? O10 Co2 O6 93.68(12) . . ? O10 Co2 O6 93.68(12) 2_545 2_545 ? O10 Co2 O6 86.32(12) . 2_545 ? O6 Co2 O6 180.0 . 2_545 ? O10 Co2 N2 91.76(12) 2_545 1_644 ? O10 Co2 N2 88.24(12) . 1_644 ? O6 Co2 N2 90.75(12) . 1_644 ? O6 Co2 N2 89.25(12) 2_545 1_644 ? O10 Co2 N2 88.24(12) 2_545 2_456 ? O10 Co2 N2 91.76(12) . 2_456 ? O6 Co2 N2 89.25(12) . 2_456 ? O6 Co2 N2 90.75(12) 2_545 2_456 ? N2 Co2 N2 180.0 1_644 2_456 ? O2 Be1 O3 111.8(5) . . ? O2 Be1 O4 109.4(5) . . ? O3 Be1 O4 105.8(4) . . ? O2 Be1 O1 104.6(4) . . ? O3 Be1 O1 110.8(5) . . ? O4 Be1 O1 114.5(4) . . ? O7 S1 O8 110.7(2) . . ? O7 S1 O5 109.4(2) . . ? O8 S1 O5 109.2(2) . . ? O7 S1 O6 110.1(2) . . ? O8 S1 O6 109.7(2) . . ? O5 S1 O6 107.8(2) . . ? C1 O1 Be1 121.7(4) . . ? C3 O2 Be1 123.1(5) . . ? C11 O3 Be1 124.4(4) . . ? C13 O4 Be1 123.6(4) . . ? S1 O5 Co1 141.2(2) . . ? S1 O6 Co2 146.0(2) . . ? C21 O9 Co1 126.7(3) . . ? C22 O10 Co2 126.3(3) . . ? C6 N1 C10 116.5(4) . . ? C6 N1 Co1 122.4(3) . . ? C10 N1 Co1 121.0(3) . . ? C20 N2 C16 116.4(3) . . ? C20 N2 Co2 121.7(3) . 1_466 ? C16 N2 Co2 121.8(3) . 1_466 ? O1 C1 C2 123.2(4) . . ? O1 C1 C5 115.9(4) . . ? C2 C1 C5 120.9(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C8 118.5(4) . . ? C1 C2 C8 121.5(4) . . ? O2 C3 C2 122.8(5) . . ? O2 C3 C4 114.9(6) . . ? C2 C3 C4 122.2(5) . . ? N1 C6 C7 122.6(5) . . ? C8 C7 C6 120.7(5) . . ? C7 C8 C9 117.0(4) . . ? C7 C8 C2 121.2(5) . . ? C9 C8 C2 121.7(5) . . ? C8 C9 C10 119.7(5) . . ? N1 C10 C9 123.4(5) . . ? O3 C11 C12 122.1(5) . . ? O3 C11 C15 115.9(5) . . ? C12 C11 C15 122.0(5) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 C18 120.0(4) . . ? C11 C12 C18 119.8(4) . . ? O4 C13 C12 122.8(4) . . ? O4 C13 C14 115.8(4) . . ? C12 C13 C14 121.4(4) . . ? N2 C16 C17 123.4(4) . . ? C16 C17 C18 119.8(4) . . ? C19 C18 C17 116.6(3) . . ? C19 C18 C12 121.8(4) . . ? C17 C18 C12 121.5(4) . . ? C20 C19 C18 120.5(4) . . ? N2 C20 C19 123.2(4) . . ? O12B O12 C23 66.7(14) . . ? O12 C23 O12B 49.0(11) . . ? O12 C23 O12A 82.4(12) . . ? O12B C23 O12A 122.4(16) . . ? O12 C23 C23B 92.2(16) . . ? O12B C23 C23B 45.6(12) . . ? O12A C23 C23B 130.4(21) . . ? O12 O12B C23 64.3(14) . . ? O12 O12B C23B 146.9(19) . . ? C23 O12B C23B 90.8(18) . . ? O12B C23B C23 43.7(13) . . ? _refine_diff_density_max 0.608 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.070 #============================================================================== data_d24 _database_code_CSD 200513 _audit_creation_method SHELXL _chemical_name_systematic ; Copper(I) Copper(II) Chloride Complex with Beryllium 3-(4-Pyridyl)-2,4-pentanedionate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H40 Be2 Cl3 Cu2 N4 O8' _chemical_formula_weight 956.21 _chemical_melting_point ? _chemical_compound_source ? 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' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.9766(8) _cell_length_b 10.9883(3) _cell_length_c 14.3431(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.0730(10) _cell_angle_gamma 90.00 _cell_volume 4124.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method ? _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15058 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.50 _reflns_number_total 6254 _reflns_number_observed 4598 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 852 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+2.3843P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5402 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_obs 0.0425 _refine_ls_wR_factor_all 0.1361 _refine_ls_wR_factor_obs 0.1182 _refine_ls_goodness_of_fit_all 1.106 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.165 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.5000 0.62011(3) 0.2500 0.02751(11) Uani 1 d S . Cu2 Cu 0.5000 0.31330(3) 0.2500 0.02179(10) Uani 1 d S . Cl1 Cl 0.44962(2) 0.47073(4) 0.14135(3) 0.02240(12) Uani 1 d . . Cl2 Cl 0.5000 0.10591(6) 0.2500 0.0305(2) Uani 1 d S . Be1 Be 0.69774(10) 1.0131(2) -0.0941(2) 0.0233(5) Uani 1 d . . O1 O 0.69667(5) 0.86956(12) -0.07137(10) 0.0237(3) Uani 1 d . . O2 O 0.64284(5) 1.06389(13) -0.08832(11) 0.0256(3) Uani 1 d . . O3 O 0.71086(6) 1.03403(14) -0.19609(11) 0.0288(3) Uani 1 d . . O4 O 0.74362(5) 1.07825(13) -0.01568(10) 0.0236(3) Uani 1 d . . N1 N 0.53927(6) 0.7104(2) 0.17159(11) 0.0228(3) Uani 1 d . . N2 N 0.93942(6) 1.1846(2) -0.18961(12) 0.0230(3) Uani 1 d . . C1 C 0.66662(7) 0.8252(2) -0.02356(13) 0.0205(3) Uani 1 d . . C2 C 0.62696(7) 0.8931(2) 0.00010(13) 0.0202(3) Uani 1 d . . C3 C 0.61542(7) 1.0101(2) -0.03924(15) 0.0218(4) Uani 1 d . . C4 C 0.56882(8) 1.0774(2) -0.0283(2) 0.0303(4) Uani 1 d . . H4A H 0.56735(8) 1.1550(2) -0.0596(2) 0.036 Uiso 1 d R . H4B H 0.53878(8) 1.0312(2) -0.0571(2) 0.036 Uiso 1 d R . H4C H 0.57055(8) 1.0893(2) 0.0387(2) 0.036 Uiso 1 d R . C5 C 0.67385(8) 0.6937(2) 0.0027(2) 0.0280(4) Uani 1 d . . H5A H 0.70249(8) 0.6623(2) -0.0184(2) 0.034 Uiso 1 d R . H5B H 0.68003(8) 0.6849(2) 0.0711(2) 0.034 Uiso 1 d R . H5C H 0.64360(8) 0.6494(2) -0.0279(2) 0.034 Uiso 1 d R . C6 C 0.52486(8) 0.7103(2) 0.07535(13) 0.0233(4) Uani 1 d . . H6A H 0.49499(8) 0.6646(2) 0.04472(13) 0.028 Uiso 1 d R . C7 C 0.55101(8) 0.7710(2) 0.01770(13) 0.0236(4) Uani 1 d . . H7A H 0.53858(8) 0.7696(2) -0.05095(13) 0.028 Uiso 1 d R . C8 C 0.59488(7) 0.8347(2) 0.05925(13) 0.0205(3) Uani 1 d . . C9 C 0.60952(10) 0.8377(3) 0.1591(2) 0.0372(5) Uani 1 d . . H9A H 0.63904(10) 0.8835(3) 0.1912(2) 0.045 Uiso 1 d R . C10 C 0.58093(10) 0.7764(3) 0.21192(15) 0.0370(5) Uani 1 d . . H10A H 0.59154(10) 0.7797(3) 0.28079(15) 0.044 Uiso 1 d R . C11 C 0.75430(8) 1.0717(2) -0.20551(14) 0.0261(4) Uani 1 d . . C12 C 0.79388(7) 1.1101(2) -0.12763(14) 0.0226(4) Uani 1 d . . C13 C 0.78568(7) 1.1119(2) -0.03376(13) 0.0211(3) Uani 1 d . . C14 C 0.82593(8) 1.1543(2) 0.05075(14) 0.0259(4) Uani 1 d . . H14A H 0.81333(8) 1.1488(2) 0.10770(14) 0.031 Uiso 1 d R . H14B H 0.85579(8) 1.1043(2) 0.05796(14) 0.031 Uiso 1 d R . H14C H 0.83455(8) 1.2373(2) 0.04097(14) 0.031 Uiso 1 d R . C15 C 0.76032(10) 1.0719(3) -0.3071(2) 0.0402(6) Uani 1 d . . H15A H 0.72932(10) 1.0434(3) -0.3496(2) 0.048 Uiso 1 d R . H15B H 0.76757(10) 1.1528(3) -0.3252(2) 0.048 Uiso 1 d R . H15C H 0.78799(10) 1.0188(3) -0.3111(2) 0.048 Uiso 1 d R . C16 C 0.89893(8) 1.2579(2) -0.22371(15) 0.0288(4) Uani 1 d . . H16A H 0.90284(8) 1.3251(2) -0.26408(15) 0.035 Uiso 1 d R . C17 C 0.85188(8) 1.2403(2) -0.2023(2) 0.0302(4) Uani 1 d . . H17A H 0.82422(8) 1.2952(2) -0.2276(2) 0.036 Uiso 1 d R . C18 C 0.84473(7) 1.1432(2) -0.14440(14) 0.0234(4) Uani 1 d . . C19 C 0.88762(7) 1.0719(2) -0.10557(14) 0.0247(4) Uani 1 d . . H19A H 0.88542(7) 1.0071(2) -0.06184(14) 0.030 Uiso 1 d R . C20 C 0.93333(8) 1.0947(2) -0.12989(14) 0.0238(4) Uani 1 d . . H20A H 0.96204(8) 1.0433(2) -0.10304(14) 0.029 Uiso 1 d 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 Cu1 0.0333(2) 0.0286(2) 0.0251(2) 0.000 0.01571(15) 0.000 Cu2 0.0185(2) 0.0240(2) 0.0239(2) 0.000 0.00728(12) 0.000 Cl1 0.0171(2) 0.0267(2) 0.0217(2) 0.00114(15) 0.0013(2) 0.0013(2) Cl2 0.0264(3) 0.0243(3) 0.0417(4) 0.000 0.0099(3) 0.000 Be1 0.0169(11) 0.0272(12) 0.0253(11) 0.0041(9) 0.0039(9) 0.0003(9) O1 0.0196(6) 0.0232(6) 0.0296(7) 0.0016(5) 0.0086(5) 0.0005(5) O2 0.0207(7) 0.0229(6) 0.0329(7) 0.0063(6) 0.0063(6) 0.0015(5) O3 0.0209(7) 0.0412(9) 0.0227(7) 0.0034(5) 0.0025(5) -0.0034(6) O4 0.0215(7) 0.0267(7) 0.0231(6) 0.0021(5) 0.0063(5) 0.0000(5) N1 0.0231(8) 0.0257(8) 0.0208(7) -0.0005(6) 0.0077(6) -0.0006(6) N2 0.0198(8) 0.0271(8) 0.0223(7) -0.0002(6) 0.0053(6) 0.0002(6) C1 0.0167(8) 0.0199(8) 0.0234(8) -0.0005(6) 0.0021(6) -0.0012(6) C2 0.0165(8) 0.0219(8) 0.0219(8) 0.0004(6) 0.0042(6) -0.0010(6) C3 0.0164(8) 0.0211(8) 0.0270(9) 0.0001(7) 0.0034(7) -0.0001(7) C4 0.0230(10) 0.0243(9) 0.0451(12) 0.0005(8) 0.0109(9) 0.0032(8) C5 0.0243(10) 0.0200(9) 0.0399(11) 0.0034(7) 0.0084(8) 0.0035(7) C6 0.0212(9) 0.0265(9) 0.0212(8) 0.0003(7) 0.0034(7) -0.0041(7) C7 0.0226(9) 0.0281(9) 0.0186(8) -0.0005(7) 0.0020(7) -0.0041(7) C8 0.0188(8) 0.0225(8) 0.0204(8) 0.0003(6) 0.0051(6) -0.0005(7) C9 0.0348(12) 0.0531(14) 0.0216(9) -0.0039(9) 0.0030(8) -0.0208(11) C10 0.0369(12) 0.0539(14) 0.0184(9) -0.0023(9) 0.0034(8) -0.0187(11) C11 0.0216(9) 0.0336(10) 0.0219(8) 0.0029(7) 0.0031(7) 0.0008(8) C12 0.0171(8) 0.0275(9) 0.0231(8) 0.0044(7) 0.0043(7) 0.0016(7) C13 0.0196(9) 0.0190(8) 0.0238(8) 0.0023(6) 0.0037(7) 0.0028(6) C14 0.0233(9) 0.0272(9) 0.0263(9) -0.0023(7) 0.0040(7) -0.0019(7) C15 0.0314(11) 0.067(2) 0.0214(9) -0.0012(10) 0.0060(8) -0.0042(12) C16 0.0250(10) 0.0322(10) 0.0296(9) 0.0112(8) 0.0076(8) 0.0026(8) C17 0.0212(9) 0.0364(11) 0.0323(10) 0.0115(9) 0.0051(8) 0.0047(8) C18 0.0179(8) 0.0298(9) 0.0223(8) 0.0027(7) 0.0045(6) 0.0003(7) C19 0.0196(9) 0.0285(9) 0.0257(9) 0.0039(7) 0.0050(7) 0.0017(7) C20 0.0202(9) 0.0256(9) 0.0251(8) 0.0017(7) 0.0044(7) 0.0031(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.988(2) . ? Cu1 N1 1.988(2) 2_655 ? Cu1 Cl1 2.4372(5) . ? Cu1 Cl1 2.4372(5) 2_655 ? Cu2 N2 2.027(2) 7_665 ? Cu2 N2 2.027(2) 8_466 ? Cu2 Cl2 2.2789(8) . ? Cu2 Cl1 2.4977(5) 2_655 ? Cu2 Cl1 2.4977(5) . ? Be1 O3 1.603(3) . ? Be1 O2 1.604(3) . ? Be1 O1 1.612(3) . ? Be1 O4 1.623(3) . ? O1 C1 1.279(2) . ? O2 C3 1.283(2) . ? O3 C11 1.281(3) . ? O4 C13 1.279(2) . ? N1 C6 1.340(2) . ? N1 C10 1.344(3) . ? N2 C20 1.344(3) . ? N2 C16 1.349(3) . ? N2 Cu2 2.027(2) 7_665 ? C1 C2 1.412(3) . ? C1 C5 1.494(3) . ? C2 C3 1.408(3) . ? C2 C8 1.496(3) . ? C3 C4 1.499(3) . ? C6 C7 1.382(3) . ? C7 C8 1.380(3) . ? C8 C9 1.390(3) . ? C9 C10 1.381(3) . ? C11 C12 1.409(3) . ? C11 C15 1.504(3) . ? C12 C13 1.417(3) . ? C12 C18 1.494(3) . ? C13 C14 1.492(3) . ? C16 C17 1.390(3) . ? C17 C18 1.394(3) . ? C18 C19 1.396(3) . ? C19 C20 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 120.10(10) . 2_655 ? N1 Cu1 Cl1 105.40(5) . . ? N1 Cu1 Cl1 114.01(5) 2_655 . ? N1 Cu1 Cl1 114.01(5) . 2_655 ? N1 Cu1 Cl1 105.40(5) 2_655 2_655 ? Cl1 Cu1 Cl1 95.33(2) . 2_655 ? N2 Cu2 N2 178.70(10) 7_665 8_466 ? N2 Cu2 Cl2 90.65(5) 7_665 . ? N2 Cu2 Cl2 90.65(5) 8_466 . ? N2 Cu2 Cl1 83.44(5) 7_665 2_655 ? N2 Cu2 Cl1 95.65(5) 8_466 2_655 ? Cl2 Cu2 Cl1 133.838(11) . 2_655 ? N2 Cu2 Cl1 95.65(5) 7_665 . ? N2 Cu2 Cl1 83.44(5) 8_466 . ? Cl2 Cu2 Cl1 133.838(12) . . ? Cl1 Cu2 Cl1 92.32(2) 2_655 . ? Cu1 Cl1 Cu2 86.18(2) . . ? O3 Be1 O2 114.1(2) . . ? O3 Be1 O1 110.1(2) . . ? O2 Be1 O1 105.5(2) . . ? O3 Be1 O4 105.6(2) . . ? O2 Be1 O4 111.6(2) . . ? O1 Be1 O4 109.8(2) . . ? C1 O1 Be1 121.7(2) . . ? C3 O2 Be1 122.1(2) . . ? C11 O3 Be1 123.6(2) . . ? C13 O4 Be1 123.5(2) . . ? C6 N1 C10 116.5(2) . . ? C6 N1 Cu1 121.40(13) . . ? C10 N1 Cu1 122.05(13) . . ? C20 N2 C16 117.2(2) . . ? C20 N2 Cu2 121.12(14) . 7_665 ? C16 N2 Cu2 120.26(13) . 7_665 ? O1 C1 C2 123.0(2) . . ? O1 C1 C5 116.3(2) . . ? C2 C1 C5 120.7(2) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 C8 121.1(2) . . ? C1 C2 C8 119.1(2) . . ? O2 C3 C2 122.7(2) . . ? O2 C3 C4 116.1(2) . . ? C2 C3 C4 121.2(2) . . ? N1 C6 C7 123.6(2) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 117.1(2) . . ? C7 C8 C2 121.8(2) . . ? C9 C8 C2 121.0(2) . . ? C10 C9 C8 119.8(2) . . ? N1 C10 C9 123.2(2) . . ? O3 C11 C12 123.3(2) . . ? O3 C11 C15 114.8(2) . . ? C12 C11 C15 121.9(2) . . ? C11 C12 C13 119.6(2) . . ? C11 C12 C18 119.6(2) . . ? C13 C12 C18 120.7(2) . . ? O4 C13 C12 122.7(2) . . ? O4 C13 C14 115.6(2) . . ? C12 C13 C14 121.7(2) . . ? N2 C16 C17 122.6(2) . . ? C16 C17 C18 120.3(2) . . ? C17 C18 C19 116.5(2) . . ? C17 C18 C12 123.2(2) . . ? C19 C18 C12 120.2(2) . . ? C20 C19 C18 120.0(2) . . ? N2 C20 C19 123.3(2) . . ? _refine_diff_density_max 0.748 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.095 #============================================================================== data_c1208 _database_code_CSD 200514 _audit_creation_method SHELXL _chemical_name_systematic ; Copper(I) Copper(II) Bromide Complex with Beryllium 3-(4-Pyridyl)-2,4-pentanedionate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H40 Be2 Br3 Cu2 N4 O8' _chemical_formula_weight 1089.59 _chemical_melting_point ? _chemical_compound_source ? 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' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.199(3) _cell_length_b 11.0752(10) _cell_length_c 14.516(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.649(2) _cell_angle_gamma 90.00 _cell_volume 4266.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method ? _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 3.862 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13615 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.99 _reflns_number_total 5126 _reflns_number_observed 3549 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 597 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4529 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_all 0.1184 _refine_ls_wR_factor_obs 0.0914 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.237 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 1.0000 -0.12722(6) 0.7500 0.0396(2) Uani 1 d S . Cu2 Cu 1.0000 0.18865(5) 0.7500 0.03171(15) Uani 1 d S . Be1 Be 1.19847(15) -0.5114(4) 0.4030(3) 0.0296(9) Uani 1 d . . Br1 Br 0.946678(11) 0.02355(3) 0.63669(2) 0.03364(11) Uani 1 d . . Br2 Br 1.0000 0.40760(5) 0.7500 0.0451(2) Uani 1 d S . O1 O 1.14441(8) -0.5631(2) 0.4127(2) 0.0330(5) Uani 1 d . . O2 O 1.19733(8) -0.3695(2) 0.4287(2) 0.0316(5) Uani 1 d . . O3 O 1.21157(8) -0.5320(2) 0.3032(2) 0.0382(6) Uani 1 d . . O4 O 1.24332(8) -0.5768(2) 0.47987(15) 0.0305(5) Uani 1 d . . N1 N 1.03995(10) -0.2150(2) 0.6720(2) 0.0311(6) Uani 1 d . . N2 N 1.43869(10) -0.6855(3) 0.3088(2) 0.0324(6) Uani 1 d . . C1 C 1.11741(12) -0.5107(3) 0.4631(2) 0.0298(7) Uani 1 d . . C2 C 1.12855(11) -0.3956(3) 0.5017(2) 0.0265(6) Uani 1 d . . C3 C 1.16770(11) -0.3268(3) 0.4776(2) 0.0265(6) Uani 1 d . . C4 C 1.17515(13) -0.1971(3) 0.5049(3) 0.0386(8) Uani 1 d . . H4A H 1.16893(13) -0.1848(3) 0.5668(3) 0.046 Uiso 1 d R . H4B H 1.15264(13) -0.1484(3) 0.4596(3) 0.046 Uiso 1 d R . H4C H 1.20900(13) -0.1739(3) 0.5037(3) 0.046 Uiso 1 d R . C5 C 1.07228(13) -0.5784(3) 0.4763(3) 0.0418(8) Uani 1 d . . H5A H 1.05986(13) -0.5420(3) 0.5268(3) 0.050 Uiso 1 d R . H5B H 1.08103(13) -0.6610(3) 0.4922(3) 0.050 Uiso 1 d R . H5C H 1.04623(13) -0.5770(3) 0.4198(3) 0.050 Uiso 1 d R . C6 C 1.02620(12) -0.2176(3) 0.5780(2) 0.0312(7) Uani 1 d . . H6A H 0.99634(12) -0.1741(3) 0.5485(2) 0.037 Uiso 1 d R . C7 C 1.05283(12) -0.2770(3) 0.5214(2) 0.0320(7) Uani 1 d . . H7A H 1.04062(12) -0.2774(3) 0.4541(2) 0.038 Uiso 1 d R . C8 C 1.09653(11) -0.3381(3) 0.5609(2) 0.0280(6) Uani 1 d . . C9 C 1.10995(14) -0.3399(4) 0.6586(3) 0.0477(10) Uani 1 d . . H9A H 1.13917(14) -0.3843(4) 0.6899(3) 0.057 Uiso 1 d R . C10 C 1.0813(2) -0.2791(4) 0.7110(3) 0.0524(11) Uani 1 d . . H10A H 1.0913(2) -0.2820(4) 0.7787(3) 0.063 Uiso 1 d R . C11 C 1.25497(12) -0.5690(3) 0.2932(2) 0.0368(8) Uani 1 d . . C12 C 1.29313(11) -0.6075(3) 0.3677(2) 0.0297(7) Uani 1 d . . C13 C 1.28485(11) -0.6114(3) 0.4611(2) 0.0258(6) Uani 1 d . . C14 C 1.32361(12) -0.6566(3) 0.5422(2) 0.0358(7) Uani 1 d . . H14A H 1.30764(12) -0.6841(3) 0.5911(2) 0.043 Uiso 1 d R . H14B H 1.34705(12) -0.5932(3) 0.5658(2) 0.043 Uiso 1 d R . H14C H 1.34196(12) -0.7217(3) 0.5217(2) 0.043 Uiso 1 d R . C15 C 1.2613(2) -0.5645(5) 0.1929(3) 0.0628(13) Uani 1 d . . H15A H 1.2940(2) -0.5326(5) 0.1919(3) 0.075 Uiso 1 d R . H15B H 1.2359(2) -0.5144(5) 0.1552(3) 0.075 Uiso 1 d R . H15C H 1.2582(2) -0.6444(5) 0.1665(3) 0.075 Uiso 1 d R . C16 C 1.39852(13) -0.7549(4) 0.2729(3) 0.0398(8) Uani 1 d . . H16A H 1.40296(13) -0.8213(4) 0.2330(3) 0.048 Uiso 1 d R . C17 C 1.35142(13) -0.7358(4) 0.2925(3) 0.0431(9) Uani 1 d . . H17A H 1.32384(13) -0.7878(4) 0.2652(3) 0.052 Uiso 1 d R . C18 C 1.34376(11) -0.6408(3) 0.3507(2) 0.0310(7) Uani 1 d . . C19 C 1.38647(12) -0.5734(3) 0.3898(2) 0.0336(7) Uani 1 d . . H19A H 1.38396(12) -0.5083(3) 0.4322(2) 0.040 Uiso 1 d R . C20 C 1.43202(12) -0.5978(3) 0.3679(2) 0.0341(7) Uani 1 d . . H20A H 1.46060(12) -0.5494(3) 0.3964(2) 0.041 Uiso 1 d 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 Cu1 0.0411(3) 0.0462(4) 0.0385(3) 0.000 0.0237(3) 0.000 Cu2 0.0251(3) 0.0356(3) 0.0380(3) 0.000 0.0147(2) 0.000 Be1 0.018(2) 0.031(2) 0.040(2) -0.007(2) 0.008(2) 0.001(2) Br1 0.0231(2) 0.0423(2) 0.0340(2) -0.00216(14) 0.00300(12) -0.00021(14) Br2 0.0350(3) 0.0355(3) 0.0674(4) 0.000 0.0166(2) 0.000 O1 0.0226(10) 0.0311(11) 0.0462(13) -0.0090(10) 0.0100(10) -0.0012(9) O2 0.0230(11) 0.0323(12) 0.0422(13) -0.0031(10) 0.0134(9) -0.0011(9) O3 0.0220(11) 0.060(2) 0.0312(12) -0.0065(11) 0.0030(9) 0.0069(11) O4 0.0242(10) 0.0371(12) 0.0317(11) -0.0033(9) 0.0096(9) 0.0016(9) N1 0.0277(14) 0.037(2) 0.0302(14) 0.0013(11) 0.0101(11) 0.0016(11) N2 0.0247(13) 0.039(2) 0.0342(14) -0.0031(12) 0.0080(11) -0.0023(11) C1 0.0201(14) 0.028(2) 0.041(2) 0.0019(13) 0.0059(13) 0.0018(12) C2 0.0207(14) 0.0291(15) 0.030(2) 0.0001(13) 0.0062(12) 0.0029(12) C3 0.0201(14) 0.028(2) 0.030(2) 0.0011(12) 0.0028(12) 0.0018(12) C4 0.034(2) 0.028(2) 0.056(2) -0.006(2) 0.014(2) -0.0037(14) C5 0.028(2) 0.033(2) 0.068(2) -0.001(2) 0.020(2) -0.0031(14) C6 0.0228(15) 0.036(2) 0.034(2) -0.0006(14) 0.0059(13) 0.0046(13) C7 0.029(2) 0.038(2) 0.028(2) -0.0025(13) 0.0033(13) 0.0067(14) C8 0.0229(15) 0.027(2) 0.035(2) 0.0026(13) 0.0091(13) 0.0004(12) C9 0.040(2) 0.071(3) 0.032(2) 0.006(2) 0.007(2) 0.026(2) C10 0.051(2) 0.081(3) 0.026(2) 0.004(2) 0.010(2) 0.023(2) C11 0.026(2) 0.053(2) 0.032(2) -0.005(2) 0.0081(13) -0.0007(15) C12 0.0183(14) 0.038(2) 0.033(2) -0.0061(14) 0.0074(12) -0.0005(13) C13 0.0189(13) 0.0227(14) 0.037(2) -0.0051(13) 0.0086(12) -0.0040(11) C14 0.029(2) 0.037(2) 0.042(2) 0.005(2) 0.0096(15) 0.0017(14) C15 0.044(2) 0.114(4) 0.033(2) -0.001(2) 0.012(2) 0.011(3) C16 0.030(2) 0.048(2) 0.045(2) -0.016(2) 0.0149(15) -0.003(2) C17 0.026(2) 0.054(2) 0.050(2) -0.022(2) 0.0089(15) -0.006(2) C18 0.0193(14) 0.042(2) 0.033(2) -0.0032(14) 0.0090(13) -0.0012(13) C19 0.029(2) 0.037(2) 0.037(2) -0.0068(15) 0.0111(14) -0.0024(14) C20 0.025(2) 0.042(2) 0.037(2) -0.002(2) 0.0106(13) -0.0041(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.987(3) . ? Cu1 N1 1.986(3) 2_756 ? Cu1 Br1 2.5598(5) 2_756 ? Cu1 Br1 2.5598(5) . ? Cu2 N2 2.034(3) 8_446 ? Cu2 N2 2.034(3) 7_746 ? Cu2 Br2 2.4249(8) . ? Cu2 Br1 2.6660(5) . ? Cu2 Br1 2.6660(5) 2_756 ? Be1 O3 1.582(5) . ? Be1 O1 1.612(4) . ? Be1 O2 1.618(5) . ? Be1 O4 1.631(5) . ? O1 C1 1.283(4) . ? O2 C3 1.276(4) . ? O3 C11 1.288(4) . ? O4 C13 1.277(3) . ? N1 C6 1.334(4) . ? N1 C10 1.346(5) . ? N2 C20 1.334(4) . ? N2 C16 1.345(4) . ? N2 Cu2 2.034(3) 7_746 ? C1 C2 1.398(4) . ? C1 C5 1.487(5) . ? C2 C3 1.414(4) . ? C2 C8 1.494(4) . ? C3 C4 1.491(4) . ? C6 C7 1.376(4) . ? C7 C8 1.379(4) . ? C8 C9 1.385(5) . ? C9 C10 1.378(5) . ? C11 C12 1.392(5) . ? C11 C15 1.503(5) . ? C12 C13 1.423(4) . ? C12 C18 1.497(4) . ? C13 C14 1.484(5) . ? C16 C17 1.388(5) . ? C17 C18 1.393(5) . ? C18 C19 1.393(4) . ? C19 C20 1.372(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 N1 Cu1 N1 121.4(2) . 2_756 ? N1 Cu1 Br1 112.45(8) . 2_756 ? N1 Cu1 Br1 104.87(8) 2_756 2_756 ? N1 Cu1 Br1 104.87(8) . . ? N1 Cu1 Br1 112.45(8) 2_756 . ? Br1 Cu1 Br1 98.57(3) 2_756 . ? N2 Cu2 N2 178.0(2) 8_446 7_746 ? N2 Cu2 Br2 91.00(8) 8_446 . ? N2 Cu2 Br2 91.00(8) 7_746 . ? N2 Cu2 Br1 82.06(8) 8_446 . ? N2 Cu2 Br1 96.56(8) 7_746 . ? Br2 Cu2 Br1 133.303(12) . . ? N2 Cu2 Br1 96.56(8) 8_446 2_756 ? N2 Cu2 Br1 82.06(8) 7_746 2_756 ? Br2 Cu2 Br1 133.303(12) . 2_756 ? Br1 Cu2 Br1 93.39(2) . 2_756 ? O3 Be1 O1 115.0(3) . . ? O3 Be1 O2 111.7(3) . . ? O1 Be1 O2 105.1(2) . . ? O3 Be1 O4 106.1(2) . . ? O1 Be1 O4 110.0(3) . . ? O2 Be1 O4 108.8(3) . . ? Cu1 Br1 Cu2 84.02(2) . . ? C1 O1 Be1 122.4(3) . . ? C3 O2 Be1 122.3(2) . . ? C11 O3 Be1 123.0(3) . . ? C13 O4 Be1 123.5(3) . . ? C6 N1 C10 116.1(3) . . ? C6 N1 Cu1 121.9(2) . . ? C10 N1 Cu1 122.0(2) . . ? C20 N2 C16 116.9(3) . . ? C20 N2 Cu2 121.5(2) . 7_746 ? C16 N2 Cu2 119.9(2) . 7_746 ? O1 C1 C2 122.7(3) . . ? O1 C1 C5 115.9(3) . . ? C2 C1 C5 121.4(3) . . ? C1 C2 C3 120.1(3) . . ? C1 C2 C8 121.1(3) . . ? C3 C2 C8 118.5(3) . . ? O2 C3 C2 122.6(3) . . ? O2 C3 C4 116.0(3) . . ? C2 C3 C4 121.3(3) . . ? N1 C6 C7 123.7(3) . . ? C6 C7 C8 120.3(3) . . ? C7 C8 C9 116.3(3) . . ? C7 C8 C2 121.8(3) . . ? C9 C8 C2 121.8(3) . . ? C10 C9 C8 120.3(3) . . ? N1 C10 C9 123.2(3) . . ? O3 C11 C12 123.8(3) . . ? O3 C11 C15 113.7(3) . . ? C12 C11 C15 122.6(3) . . ? C11 C12 C13 120.2(3) . . ? C11 C12 C18 120.2(3) . . ? C13 C12 C18 119.5(3) . . ? O4 C13 C12 121.7(3) . . ? O4 C13 C14 116.1(3) . . ? C12 C13 C14 122.2(3) . . ? N2 C16 C17 122.8(3) . . ? C16 C17 C18 120.5(3) . . ? C19 C18 C17 115.4(3) . . ? C19 C18 C12 121.1(3) . . ? C17 C18 C12 123.5(3) . . ? C20 C19 C18 121.0(3) . . ? N2 C20 C19 123.3(3) . . ? _refine_diff_density_max 1.589 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.085 #============================================================================== data_d25 _database_code_CSD 200515 _audit_creation_method SHELXL _chemical_name_systematic ; Copper(I) Bromide Complex with Beryllium 3-(Pyridyl-4)-2,4-Pentanedionate, Solvate with Chloroform ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45.33 H45.33 Be2 Br2 Cl16 Cu2 N4 O8' _chemical_formula_weight 1646.31 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.0193(9) _cell_length_b 25.1798(11) _cell_length_c 21.7707(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.6180(10) _cell_angle_gamma 90.00 _cell_volume 10114.7(7) _cell_formula_units_Z 6 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method ? _exptl_crystal_F_000 4904 _exptl_absorpt_coefficient_mu 2.498 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93413 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 30.52 _reflns_number_total 30833 _reflns_number_observed 16408 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7562 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+22.6051P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23271 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_obs 0.0758 _refine_ls_wR_factor_all 0.2942 _refine_ls_wR_factor_obs 0.2088 _refine_ls_goodness_of_fit_all 1.110 _refine_ls_goodness_of_fit_obs 1.238 _refine_ls_restrained_S_all 1.358 _refine_ls_restrained_S_obs 1.240 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.00018(3) 0.44472(2) 1.00923(3) 0.01911(14) Uani 1 d . . Cu2 Cu 0.33271(3) 0.05511(2) 0.49790(3) 0.01914(14) Uani 1 d . . Cu3 Cu 0.33995(4) -0.05295(2) 0.51257(3) 0.0219(2) Uani 1 d . . Br1 Br 0.09809(3) 0.50245(2) 1.08957(3) 0.02095(12) Uani 1 d . . Br2 Br 0.22781(3) -0.00419(2) 0.42340(3) 0.02277(13) Uani 1 d . . Br3 Br 0.44571(3) 0.00696(2) 0.58514(3) 0.02003(12) Uani 1 d . . Be1 Be -0.2266(4) 0.2180(3) 1.1758(4) 0.030(2) Uani 1 d . . Be2 Be 0.1689(4) 0.2413(3) 0.7617(4) 0.030(2) Uani 1 d . . Be3 Be 0.4920(4) 0.2427(3) 0.2322(4) 0.029(2) Uani 1 d . . O1 O -0.2207(2) 0.2809(2) 1.1884(2) 0.0303(9) Uani 1 d . . O2 O -0.2050(2) 0.2069(2) 1.1156(2) 0.0334(9) Uani 1 d . . O3 O -0.3055(2) 0.1942(2) 1.1525(2) 0.0295(9) Uani 1 d . . O4 O -0.1714(2) 0.1901(2) 1.2493(3) 0.0376(11) Uani 1 d . . O5 O 0.2143(2) 0.2585(2) 0.8428(2) 0.0312(9) Uani 1 d . . O6 O 0.0877(2) 0.2630(2) 0.7345(2) 0.0353(10) Uani 1 d . . O7 O 0.1727(2) 0.1777(2) 0.7573(2) 0.0318(9) Uani 1 d . . O8 O 0.2031(2) 0.2644(2) 0.7156(2) 0.0323(9) Uani 1 d . . O9 O 0.4932(2) 0.1792(2) 0.2400(2) 0.0290(9) Uani 1 d . . O10 O 0.4505(2) 0.2650(2) 0.2722(2) 0.0299(9) Uani 1 d . . O11 O 0.4538(2) 0.2581(2) 0.1506(2) 0.0311(9) Uani 1 d . . O12 O 0.5731(2) 0.2669(2) 0.2664(2) 0.0268(8) Uani 1 d . . N1 N -0.0476(2) 0.4018(2) 1.0541(2) 0.0217(9) Uani 1 d . . N2 N -0.3225(2) 0.0847(2) 1.4117(2) 0.0204(8) Uani 1 d . . N3 N 0.0377(2) 0.3975(2) 0.9572(2) 0.0195(8) Uani 1 d . . N4 N 0.3006(2) 0.0915(2) 0.5606(2) 0.0189(8) Uani 1 d . . N5 N 0.3611(2) 0.0895(2) 0.4312(2) 0.0195(8) Uani 1 d . . N6 N 0.6358(2) 0.4002(2) 0.0486(2) 0.0226(9) Uani 1 d . . C1 C -0.1864(3) 0.3115(2) 1.1676(3) 0.0270(11) Uani 1 d . . C2 C -0.1596(3) 0.2940(2) 1.1226(3) 0.0254(11) Uani 1 d . . C3 C -0.1742(3) 0.2423(2) 1.0957(3) 0.0303(12) Uani 1 d . . C4 C -0.1549(5) 0.2243(3) 1.0419(4) 0.044(2) Uani 1 d . . H4A H -0.1685(5) 0.1878(3) 1.0302(4) 0.080 Uiso 1 d R . H4B H -0.1805(5) 0.2458(3) 1.0009(4) 0.080 Uiso 1 d R . H4C H -0.1037(5) 0.2280(3) 1.0591(4) 0.080 Uiso 1 d R . C5 C -0.1773(4) 0.3674(3) 1.1922(4) 0.0378(14) Uani 1 d . . H5A H -0.1983(4) 0.3718(3) 1.2225(4) 0.080 Uiso 1 d R . H5B H -0.1266(4) 0.3759(3) 1.2173(4) 0.080 Uiso 1 d R . H5C H -0.2010(4) 0.3907(3) 1.1527(4) 0.080 Uiso 1 d R . C6 C -0.0123(3) 0.3642(2) 1.1019(3) 0.0303(12) Uani 1 d . . H6A H 0.0392(3) 0.3616(2) 1.1205(3) 0.080 Uiso 1 d R . C7 C -0.0458(3) 0.3290(2) 1.1264(3) 0.0321(13) Uani 1 d . . H7A H -0.0178(3) 0.3032(2) 1.1615(3) 0.080 Uiso 1 d R . C8 C -0.1209(3) 0.3317(2) 1.0996(3) 0.0239(11) Uani 1 d . . C9 C -0.1564(3) 0.3710(2) 1.0513(3) 0.0272(11) Uani 1 d . . H9A H -0.2078(3) 0.3751(2) 1.0324(3) 0.080 Uiso 1 d R . C10 C -0.1190(3) 0.4049(2) 1.0296(3) 0.0279(12) Uani 1 d . . H10A H -0.1456(3) 0.4318(2) 0.9956(3) 0.080 Uiso 1 d R . C11 C -0.3213(3) 0.1688(2) 1.1947(3) 0.0235(10) Uani 1 d . . C12 C -0.2687(3) 0.1563(2) 1.2633(3) 0.0254(11) Uani 1 d . . C13 C -0.1949(3) 0.1680(2) 1.2883(3) 0.0308(13) Uani 1 d . . C14 C -0.1380(3) 0.1551(3) 1.3608(4) 0.045(2) Uani 1 d . . H14A H -0.0918(3) 0.1665(3) 1.3670(4) 0.080 Uiso 1 d R . H14B H -0.1484(3) 0.1729(3) 1.3940(4) 0.080 Uiso 1 d R . H14C H -0.1371(3) 0.1174(3) 1.3680(4) 0.080 Uiso 1 d R . C15 C -0.3979(3) 0.1516(2) 1.1655(3) 0.0280(11) Uani 1 d . . H15A H -0.4249(3) 0.1640(2) 1.1181(3) 0.080 Uiso 1 d R . H15B H -0.4003(3) 0.1136(2) 1.1663(3) 0.080 Uiso 1 d R . H15C H -0.4180(3) 0.1664(2) 1.1931(3) 0.080 Uiso 1 d R . C16 C -0.2873(3) 0.0575(2) 1.3845(3) 0.0233(10) Uani 1 d . . H16A H -0.2722(3) 0.0218(2) 1.4005(3) 0.080 Uiso 1 d R . C17 C -0.2709(3) 0.0783(2) 1.3350(3) 0.0242(11) Uani 1 d . . H17A H -0.2467(3) 0.0569(2) 1.3161(3) 0.080 Uiso 1 d R . C18 C -0.2901(3) 0.1305(2) 1.3120(3) 0.0224(10) Uani 1 d . . C19 C -0.3287(3) 0.1582(2) 1.3391(3) 0.0259(11) Uani 1 d . . H19A H -0.3444(3) 0.1939(2) 1.3241(3) 0.080 Uiso 1 d R . C20 C -0.3437(3) 0.1343(2) 1.3872(3) 0.0270(11) Uani 1 d . . H20A H -0.3712(3) 0.1537(2) 1.4043(3) 0.080 Uiso 1 d R . C21 C 0.1877(3) 0.2845(2) 0.8755(3) 0.0267(11) Uani 1 d . . C22 C 0.1158(3) 0.3037(2) 0.8416(3) 0.0254(11) Uani 1 d . . C23 C 0.0688(3) 0.2915(2) 0.7716(3) 0.0324(13) Uani 1 d . . C24 C -0.0082(4) 0.3102(4) 0.7362(4) 0.050(2) Uani 1 d . . H24A H -0.0315(4) 0.2982(4) 0.6885(4) 0.080 Uiso 1 d R . H24B H -0.0330(4) 0.2957(4) 0.7597(4) 0.080 Uiso 1 d R . H24C H -0.0098(4) 0.3483(4) 0.7372(4) 0.080 Uiso 1 d R . C25 C 0.2377(3) 0.2939(3) 0.9512(3) 0.0349(13) Uani 1 d . . H25A H 0.2837(3) 0.2779(3) 0.9637(3) 0.080 Uiso 1 d R . H25B H 0.2439(3) 0.3314(3) 0.9600(3) 0.080 Uiso 1 d R . H25C H 0.2177(3) 0.2784(3) 0.9786(3) 0.080 Uiso 1 d R . C26 C 0.0444(3) 0.3445(2) 0.9644(3) 0.0246(11) Uani 1 d . . H26A H 0.0311(3) 0.3278(2) 0.9963(3) 0.080 Uiso 1 d R . C27 C 0.0695(3) 0.3127(2) 0.9286(3) 0.0269(11) Uani 1 d . . H27A H 0.0732(3) 0.2750(2) 0.9356(3) 0.080 Uiso 1 d R . C28 C 0.0888(3) 0.3361(2) 0.8824(3) 0.0248(11) Uani 1 d . . C29 C 0.0828(3) 0.3910(2) 0.8747(3) 0.0259(11) Uani 1 d . . H29A H 0.0963(3) 0.4084(2) 0.8435(3) 0.080 Uiso 1 d R . C30 C 0.0569(3) 0.4205(2) 0.9127(3) 0.0251(11) Uani 1 d . . H30A H 0.0526(3) 0.4583(2) 0.9063(3) 0.080 Uiso 1 d R . C31 C 0.2014(3) 0.1531(2) 0.7248(3) 0.0235(10) Uani 1 d . . C32 C 0.2269(3) 0.1796(2) 0.6842(3) 0.0241(11) Uani 1 d . . C33 C 0.2251(3) 0.2358(2) 0.6806(3) 0.0286(12) Uani 1 d . . C34 C 0.2488(4) 0.2666(2) 0.6362(4) 0.041(2) Uani 1 d . . H34A H 0.2433(4) 0.3039(2) 0.6413(4) 0.080 Uiso 1 d R . H34B H 0.2988(4) 0.2589(2) 0.6508(4) 0.080 Uiso 1 d R . H34C H 0.2197(4) 0.2566(2) 0.5880(4) 0.080 Uiso 1 d R . C35 C 0.2083(4) 0.0948(2) 0.7360(4) 0.0355(14) Uani 1 d . . H35A H 0.1876(4) 0.0844(2) 0.7650(4) 0.080 Uiso 1 d R . H35B H 0.1834(4) 0.0770(2) 0.6917(4) 0.080 Uiso 1 d R . H35C H 0.2587(4) 0.0852(2) 0.7585(4) 0.080 Uiso 1 d R . C36 C 0.2336(3) 0.0856(2) 0.5524(3) 0.0161(9) Uani 1 d . . H36A H 0.2012(3) 0.0612(2) 0.5175(3) 0.080 Uiso 1 d R . C37 C 0.2090(3) 0.1130(2) 0.5922(3) 0.0179(9) Uani 1 d . . H37A H 0.1607(3) 0.1071(2) 0.5848(3) 0.080 Uiso 1 d R . C38 C 0.2538(3) 0.1489(2) 0.6429(3) 0.0219(10) Uani 1 d . . C39 C 0.3237(3) 0.1541(2) 0.6524(3) 0.0322(13) Uani 1 d . . H39A H 0.3573(3) 0.1779(2) 0.6873(3) 0.080 Uiso 1 d R . C40 C 0.3449(3) 0.1250(2) 0.6113(3) 0.0293(12) Uani 1 d . . H40A H 0.3936(3) 0.1291(2) 0.6190(3) 0.080 Uiso 1 d R . C41 C 0.4650(3) 0.1538(2) 0.2722(3) 0.0261(11) Uani 1 d . . C42 C 0.4336(3) 0.1799(2) 0.3089(3) 0.0235(10) Uani 1 d . . C43 C 0.4289(3) 0.2356(2) 0.3070(3) 0.0270(11) Uani 1 d . . C44 C 0.3987(4) 0.2653(2) 0.3468(4) 0.0349(14) Uani 1 d . . H44A H 0.4000(4) 0.3027(2) 0.3389(4) 0.080 Uiso 1 d R . H44B H 0.3496(4) 0.2544(2) 0.3311(4) 0.080 Uiso 1 d R . H44C H 0.4273(4) 0.2579(2) 0.3959(4) 0.080 Uiso 1 d R . C45 C 0.4666(4) 0.0950(2) 0.2673(3) 0.0318(13) Uani 1 d . . H45A H 0.4900(4) 0.0854(2) 0.2403(3) 0.080 Uiso 1 d R . H45B H 0.4932(4) 0.0803(2) 0.3135(3) 0.080 Uiso 1 d R . H45C H 0.4181(4) 0.0812(2) 0.2451(3) 0.080 Uiso 1 d R . C46 C 0.3146(3) 0.1179(2) 0.3759(3) 0.0309(13) Uani 1 d . . H46A H 0.2644(3) 0.1180(2) 0.3642(3) 0.080 Uiso 1 d R . C47 C 0.3355(3) 0.1475(3) 0.3350(3) 0.0339(14) Uani 1 d . . H47A H 0.3001(3) 0.1676(3) 0.2961(3) 0.080 Uiso 1 d R . C48 C 0.4079(3) 0.1476(2) 0.3499(3) 0.0230(10) Uani 1 d . . C49 C 0.4549(3) 0.1168(2) 0.4054(3) 0.0202(10) Uani 1 d . . H49A H 0.5051(3) 0.1150(2) 0.4173(3) 0.080 Uiso 1 d R . C50 C 0.4303(3) 0.0885(2) 0.4443(3) 0.0196(10) Uani 1 d . . H50A H 0.4643(3) 0.0668(2) 0.4822(3) 0.080 Uiso 1 d R . C51 C 0.4860(3) 0.2829(2) 0.1221(3) 0.0269(11) Uani 1 d . . C52 C 0.5554(3) 0.3044(2) 0.1601(3) 0.0221(10) Uani 1 d . . C53 C 0.5969(3) 0.2947(2) 0.2324(3) 0.0242(11) Uani 1 d . . C54 C 0.6724(3) 0.3153(3) 0.2738(3) 0.0319(12) Uani 1 d . . H54A H 0.6915(3) 0.3047(3) 0.3217(3) 0.080 Uiso 1 d R . H54B H 0.7022(3) 0.3011(3) 0.2554(3) 0.080 Uiso 1 d R . H54C H 0.6721(3) 0.3534(3) 0.2710(3) 0.080 Uiso 1 d R . C55 C 0.4428(3) 0.2888(3) 0.0438(3) 0.0364(14) Uani 1 d . . H55A H 0.3969(3) 0.2713(3) 0.0275(3) 0.080 Uiso 1 d R . H55B H 0.4349(3) 0.3258(3) 0.0317(3) 0.080 Uiso 1 d R . H55C H 0.4686(3) 0.2730(3) 0.0221(3) 0.080 Uiso 1 d R . C56 C 0.6086(3) 0.4221(2) 0.0868(3) 0.0242(11) Uani 1 d . . H56A H 0.6069(3) 0.4601(2) 0.0888(3) 0.080 Uiso 1 d R . C57 C 0.5835(3) 0.3924(2) 0.1247(3) 0.0244(11) Uani 1 d . . H57A H 0.5641(3) 0.4099(2) 0.1513(3) 0.080 Uiso 1 d R . C58 C 0.5861(3) 0.3372(2) 0.1233(3) 0.0201(10) Uani 1 d . . C59 C 0.6163(3) 0.3146(2) 0.0849(3) 0.0232(10) Uani 1 d . . H59A H 0.6205(3) 0.2767(2) 0.0834(3) 0.080 Uiso 1 d R . C60 C 0.6402(3) 0.3472(2) 0.0490(3) 0.0237(11) Uani 1 d . . H60A H 0.6618(3) 0.3308(2) 0.0235(3) 0.080 Uiso 1 d R . C1S C 0.3580(6) 0.8360(4) 0.0148(5) 0.068(2) Uani 1 d . . Cl11 Cl 0.3185(2) 0.87545(12) 0.0519(2) 0.0874(8) Uani 1 d . . Cl12 Cl 0.3769(2) 0.77287(13) 0.0539(2) 0.1071(11) Uani 1 d . . Cl13 Cl 0.4397(2) 0.8653(2) 0.0258(2) 0.1054(11) Uani 1 d . . C2S C 0.1788(7) 0.5785(4) 0.3387(6) 0.082(3) Uani 1 d . . Cl21 Cl 0.1361(2) 0.55089(11) 0.2547(2) 0.0808(7) Uani 1 d . . Cl22 Cl 0.1299(3) 0.5646(2) 0.3839(3) 0.128(2) Uani 1 d . . Cl23 Cl 0.2675(3) 0.5566(2) 0.3838(2) 0.1260(13) Uani 1 d . . C3S C 0.4827(7) 0.4596(5) 0.2744(7) 0.358(34) Uani 1 d D . Cl31 Cl 0.5005(2) 0.38862(11) 0.27834(15) 0.0845(8) Uani 1 d D . Cl32 Cl 0.5352(4) 0.4912(2) 0.3520(3) 0.162(2) Uani 1 d D . Cl33 Cl 0.3921(4) 0.4674(3) 0.2575(4) 0.177(3) Uani 1 d D . C4S C 0.1310(12) 0.1438(7) 0.8807(13) 0.136(7) Uani 1 d . . Cl41 Cl 0.1443(4) 0.0751(2) 0.8766(3) 0.142(2) Uani 1 d . . Cl42 Cl 0.1594(3) 0.1677(2) 0.9609(3) 0.135(2) Uani 1 d . . Cl43 Cl 0.0371(3) 0.1621(2) 0.8272(3) 0.151(2) Uani 1 d . . C5S C 0.3539(10) 0.1075(6) 0.9951(7) 0.225(14) Uiso 1 d D . Cl51 Cl 0.4023(7) 0.1374(5) 1.0750(5) 0.107(5) Uani 0.45(2) d PD . Cl52 Cl 0.3148(5) 0.1554(3) 0.9286(3) 0.063(3) Uani 0.45(2) d PD . Cl53 Cl 0.4073(6) 0.0622(4) 0.9786(7) 0.146(7) Uani 0.45(2) d PD . Cl54 Cl 0.3782(19) 0.1478(11) 1.0703(8) 0.223(13) Uani 0.55(2) d PD . Cl55 Cl 0.3264(14) 0.1475(10) 0.9231(8) 0.215(11) Uani 0.55(2) d PD . Cl56 Cl 0.2919(16) 0.0601(7) 0.9883(16) 0.360(24) Uani 0.55(2) d PD . C7S C -0.0545(10) 0.1571(7) 0.9363(10) 0.222(31) Uani 0.58(2) d PD . Cl71 Cl -0.1025(4) 0.1990(3) 0.8637(4) 0.115(3) Uani 0.58(2) d PD . Cl72 Cl -0.1205(9) 0.1221(3) 0.9487(7) 0.197(8) Uani 0.58(2) d PD . Cl73 Cl 0.0023(5) 0.1966(5) 1.0102(6) 0.152(5) Uani 0.58(2) d PD . C9S C -0.0137(11) 0.1666(7) 0.9864(9) 0.143(4) Uiso 0.42(2) d PD . Cl91 Cl 0.0380(8) 0.2092(6) 1.0560(9) 0.143(4) Uiso 0.42(2) d PD . Cl92 Cl -0.0770(8) 0.2021(6) 0.9139(8) 0.143(4) Uiso 0.42(2) d PD . Cl93 Cl -0.0538(7) 0.1187(5) 1.0143(8) 0.143(4) Uiso 0.42(2) d PD . C6S C 0.7560(11) 0.5147(6) 0.3250(9) 0.158(8) Uiso 1 d D . Cl61 Cl 0.7277(4) 0.5082(3) 0.2359(4) 0.174(2) Uiso 1 d D . Cl62 Cl 0.7043(9) 0.4709(6) 0.3467(9) 0.295(6) Uiso 1 d D . Cl63 Cl 0.7345(4) 0.5800(3) 0.3408(4) 0.181(2) Uiso 1 d D . C8S C 0.0993(10) 0.4981(6) 0.7462(9) 0.153(7) Uiso 1 d D . Cl81 Cl 0.0327(6) 0.5161(5) 0.7674(6) 0.232(4) Uiso 1 d D . Cl82 Cl 0.0975(12) 0.4302(6) 0.7285(12) 0.346(8) Uiso 1 d D . Cl83 Cl 0.1022(9) 0.5302(6) 0.6763(8) 0.286(5) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0214(3) 0.0152(3) 0.0291(3) -0.0020(2) 0.0188(3) -0.0016(2) Cu2 0.0236(3) 0.0173(3) 0.0261(3) 0.0018(2) 0.0195(3) 0.0010(2) Cu3 0.0280(3) 0.0177(3) 0.0275(3) -0.0034(2) 0.0194(3) 0.0007(2) Br1 0.0210(2) 0.0146(2) 0.0263(2) -0.0008(2) 0.0106(2) -0.0009(2) Br2 0.0207(2) 0.0205(2) 0.0272(3) -0.0048(2) 0.0116(2) 0.0007(2) Br3 0.0204(2) 0.0161(2) 0.0256(2) 0.0034(2) 0.0126(2) 0.0003(2) Be1 0.025(4) 0.030(4) 0.039(4) 0.016(3) 0.020(3) 0.003(3) Be2 0.027(4) 0.028(4) 0.043(4) -0.020(3) 0.023(3) -0.005(3) Be3 0.028(4) 0.026(3) 0.044(4) 0.017(3) 0.026(4) 0.009(3) O1 0.029(2) 0.034(2) 0.038(2) 0.012(2) 0.023(2) 0.000(2) O2 0.038(2) 0.022(2) 0.055(3) 0.009(2) 0.034(2) -0.001(2) O3 0.024(2) 0.028(2) 0.039(2) 0.017(2) 0.018(2) 0.004(2) O4 0.023(2) 0.037(2) 0.056(3) 0.027(2) 0.023(2) 0.004(2) O5 0.021(2) 0.035(2) 0.043(2) -0.017(2) 0.020(2) -0.001(2) O6 0.029(2) 0.040(2) 0.040(2) -0.021(2) 0.019(2) -0.003(2) O7 0.037(2) 0.030(2) 0.041(2) -0.016(2) 0.029(2) -0.008(2) O8 0.041(2) 0.022(2) 0.045(2) -0.013(2) 0.029(2) -0.002(2) O9 0.033(2) 0.029(2) 0.041(2) 0.017(2) 0.031(2) 0.011(2) O10 0.030(2) 0.026(2) 0.046(2) 0.020(2) 0.028(2) 0.013(2) O11 0.021(2) 0.036(2) 0.044(2) 0.021(2) 0.022(2) 0.004(2) O12 0.026(2) 0.029(2) 0.035(2) 0.014(2) 0.022(2) 0.006(2) N1 0.018(2) 0.024(2) 0.028(2) 0.002(2) 0.015(2) -0.001(2) N2 0.020(2) 0.018(2) 0.028(2) 0.000(2) 0.015(2) -0.003(2) N3 0.016(2) 0.018(2) 0.027(2) -0.005(2) 0.012(2) -0.002(2) N4 0.022(2) 0.015(2) 0.026(2) -0.002(2) 0.016(2) -0.003(2) N5 0.021(2) 0.019(2) 0.026(2) 0.005(2) 0.017(2) 0.003(2) N6 0.022(2) 0.021(2) 0.028(2) 0.004(2) 0.014(2) -0.001(2) C1 0.027(3) 0.026(3) 0.034(3) 0.014(2) 0.019(2) 0.004(2) C2 0.024(3) 0.023(2) 0.037(3) 0.013(2) 0.021(2) 0.003(2) C3 0.031(3) 0.027(3) 0.044(3) 0.010(2) 0.027(3) 0.000(2) C4 0.061(5) 0.034(3) 0.059(4) -0.007(3) 0.047(4) -0.010(3) C5 0.049(4) 0.032(3) 0.049(4) 0.003(3) 0.037(3) -0.003(3) C6 0.020(3) 0.033(3) 0.043(3) 0.013(2) 0.018(3) 0.002(2) C7 0.020(3) 0.036(3) 0.039(3) 0.020(3) 0.014(2) 0.003(2) C8 0.024(3) 0.023(2) 0.033(3) 0.007(2) 0.020(2) 0.001(2) C9 0.016(2) 0.033(3) 0.034(3) 0.013(2) 0.014(2) 0.002(2) C10 0.025(3) 0.028(3) 0.039(3) 0.015(2) 0.022(3) 0.005(2) C11 0.021(3) 0.019(2) 0.034(3) 0.009(2) 0.017(2) 0.003(2) C12 0.021(3) 0.019(2) 0.040(3) 0.010(2) 0.018(2) 0.001(2) C13 0.023(3) 0.028(3) 0.043(3) 0.018(2) 0.017(3) 0.002(2) C14 0.024(3) 0.051(4) 0.053(4) 0.030(3) 0.011(3) -0.004(3) C15 0.020(3) 0.035(3) 0.029(3) 0.005(2) 0.011(2) -0.004(2) C16 0.024(3) 0.016(2) 0.036(3) 0.004(2) 0.019(2) 0.002(2) C17 0.030(3) 0.017(2) 0.034(3) 0.009(2) 0.022(2) 0.007(2) C18 0.019(2) 0.019(2) 0.030(3) 0.007(2) 0.013(2) 0.000(2) C19 0.024(3) 0.018(2) 0.036(3) 0.007(2) 0.015(2) 0.007(2) C20 0.027(3) 0.022(2) 0.037(3) 0.003(2) 0.020(3) 0.005(2) C21 0.022(3) 0.026(3) 0.039(3) -0.013(2) 0.020(2) -0.005(2) C22 0.022(3) 0.024(2) 0.036(3) -0.013(2) 0.018(2) -0.002(2) C23 0.026(3) 0.036(3) 0.039(3) -0.014(3) 0.019(3) -0.003(2) C24 0.026(3) 0.069(5) 0.045(4) -0.030(4) 0.010(3) 0.005(3) C25 0.027(3) 0.040(3) 0.039(3) -0.011(3) 0.017(3) 0.002(2) C26 0.024(3) 0.019(2) 0.036(3) -0.005(2) 0.019(2) -0.002(2) C27 0.026(3) 0.017(2) 0.040(3) -0.008(2) 0.019(3) -0.001(2) C28 0.017(2) 0.025(3) 0.033(3) -0.015(2) 0.012(2) -0.002(2) C29 0.027(3) 0.022(2) 0.036(3) -0.006(2) 0.022(2) -0.001(2) C30 0.028(3) 0.020(2) 0.035(3) -0.003(2) 0.022(2) 0.001(2) C31 0.020(3) 0.026(2) 0.026(3) -0.011(2) 0.012(2) -0.003(2) C32 0.021(3) 0.023(2) 0.034(3) -0.013(2) 0.017(2) -0.002(2) C33 0.031(3) 0.022(2) 0.039(3) -0.010(2) 0.022(3) -0.002(2) C34 0.058(4) 0.024(3) 0.062(4) -0.006(3) 0.045(4) -0.004(3) C35 0.055(4) 0.025(3) 0.040(3) -0.007(2) 0.033(3) -0.002(3) C36 0.014(2) 0.015(2) 0.022(2) 0.001(2) 0.010(2) 0.000(2) C37 0.017(2) 0.016(2) 0.025(2) -0.001(2) 0.014(2) 0.000(2) C38 0.025(3) 0.019(2) 0.030(3) -0.008(2) 0.019(2) -0.002(2) C39 0.028(3) 0.032(3) 0.044(3) -0.021(3) 0.024(3) -0.011(2) C40 0.024(3) 0.032(3) 0.043(3) -0.015(2) 0.025(3) -0.010(2) C41 0.024(3) 0.028(3) 0.033(3) 0.012(2) 0.019(2) 0.004(2) C42 0.022(3) 0.027(3) 0.029(3) 0.011(2) 0.018(2) 0.005(2) C43 0.024(3) 0.030(3) 0.036(3) 0.013(2) 0.021(2) 0.007(2) C44 0.039(3) 0.032(3) 0.051(4) 0.017(3) 0.036(3) 0.015(3) C45 0.045(3) 0.026(3) 0.041(3) 0.007(2) 0.033(3) 0.001(2) C46 0.021(3) 0.039(3) 0.042(3) 0.019(3) 0.022(3) 0.007(2) C47 0.023(3) 0.044(3) 0.042(3) 0.026(3) 0.022(3) 0.011(2) C48 0.023(3) 0.022(2) 0.033(3) 0.007(2) 0.021(2) 0.003(2) C49 0.019(2) 0.021(2) 0.026(3) 0.002(2) 0.015(2) 0.002(2) C50 0.021(2) 0.020(2) 0.023(2) 0.003(2) 0.015(2) 0.002(2) C51 0.026(3) 0.025(3) 0.036(3) 0.015(2) 0.020(2) 0.007(2) C52 0.023(3) 0.019(2) 0.032(3) 0.011(2) 0.020(2) 0.005(2) C53 0.025(3) 0.021(2) 0.032(3) 0.008(2) 0.019(2) 0.008(2) C54 0.028(3) 0.036(3) 0.033(3) 0.011(2) 0.015(3) 0.000(2) C55 0.026(3) 0.047(4) 0.034(3) 0.015(3) 0.012(3) -0.006(3) C56 0.028(3) 0.019(2) 0.031(3) 0.007(2) 0.019(2) 0.000(2) C57 0.031(3) 0.020(2) 0.030(3) 0.007(2) 0.021(2) 0.002(2) C58 0.017(2) 0.019(2) 0.027(3) 0.008(2) 0.013(2) 0.003(2) C59 0.025(3) 0.017(2) 0.036(3) 0.011(2) 0.022(2) 0.004(2) C60 0.025(3) 0.018(2) 0.036(3) 0.008(2) 0.022(2) 0.006(2) C1S 0.080(6) 0.073(6) 0.041(4) -0.002(4) 0.021(4) -0.009(5) Cl11 0.100(2) 0.076(2) 0.083(2) -0.0177(14) 0.042(2) -0.0018(15) Cl12 0.154(3) 0.065(2) 0.075(2) 0.0081(14) 0.034(2) 0.016(2) Cl13 0.095(2) 0.151(3) 0.073(2) -0.006(2) 0.043(2) -0.032(2) C2S 0.114(9) 0.050(5) 0.086(7) -0.014(5) 0.052(7) -0.025(6) Cl21 0.105(2) 0.0672(14) 0.077(2) -0.0183(12) 0.048(2) -0.0233(14) Cl22 0.203(4) 0.101(2) 0.140(3) -0.024(2) 0.131(3) -0.044(3) Cl23 0.126(3) 0.137(3) 0.090(2) -0.017(2) 0.031(2) -0.017(3) C3S 0.202(22) 0.332(35) 0.231(25) 0.248(28) -0.145(21) -0.220(26) Cl31 0.092(2) 0.0655(15) 0.072(2) -0.0003(12) 0.0205(14) 0.0214(13) Cl32 0.243(7) 0.089(3) 0.121(3) -0.011(2) 0.061(4) -0.026(3) Cl33 0.189(6) 0.172(5) 0.192(6) 0.007(4) 0.110(5) 0.079(5) C4S 0.168(17) 0.094(10) 0.214(20) 0.005(11) 0.145(17) -0.037(10) Cl41 0.199(5) 0.093(3) 0.171(4) -0.030(3) 0.119(4) -0.022(3) Cl42 0.199(5) 0.108(3) 0.118(3) -0.028(2) 0.092(3) -0.033(3) Cl43 0.163(5) 0.133(4) 0.153(4) -0.005(3) 0.074(4) -0.042(3) Cl51 0.082(6) 0.103(7) 0.069(6) 0.031(5) -0.018(4) -0.031(5) Cl52 0.076(5) 0.066(4) 0.036(3) 0.006(2) 0.018(3) 0.000(3) Cl53 0.118(8) 0.092(7) 0.206(14) -0.016(6) 0.061(8) 0.016(5) Cl54 0.283(26) 0.253(21) 0.090(8) -0.042(10) 0.055(11) -0.163(19) Cl55 0.252(19) 0.256(21) 0.149(11) -0.002(11) 0.107(12) -0.139(17) Cl56 0.459(43) 0.155(14) 0.671(69) -0.119(24) 0.435(51) -0.099(20) C7S 0.380(68) 0.198(37) 0.227(43) 0.142(37) 0.258(52) 0.232(48) Cl71 0.104(5) 0.097(4) 0.106(6) -0.001(3) 0.021(4) 0.040(3) Cl72 0.391(23) 0.081(5) 0.244(15) -0.050(6) 0.252(18) -0.044(7) Cl73 0.141(8) 0.196(10) 0.146(9) 0.059(8) 0.089(7) 0.053(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.018(4) . ? Cu1 N3 2.042(4) . ? Cu1 Br1 2.4413(8) . ? Cu1 Br1 2.5312(8) 3_567 ? Cu1 Cu1 2.8124(12) 3_567 ? Cu2 N5 2.009(4) . ? Cu2 N4 2.010(4) . ? Cu2 Br2 2.5093(8) . ? Cu2 Br3 2.5293(8) . ? Cu2 Cu3 2.7353(9) . ? Cu3 N6 2.017(4) 2_645 ? Cu3 N2 2.019(4) 3_557 ? Cu3 Br3 2.5195(8) . ? Cu3 Br2 2.5393(8) . ? Br1 Cu1 2.5312(8) 3_567 ? Be1 O3 1.599(9) . ? Be1 O1 1.603(9) . ? Be1 O2 1.603(9) . ? Be1 O4 1.619(9) . ? Be2 O8 1.598(9) . ? Be2 O7 1.608(8) . ? Be2 O6 1.610(9) . ? Be2 O5 1.615(9) . ? Be3 O10 1.602(8) . ? Be3 O11 1.607(9) . ? Be3 O9 1.609(8) . ? Be3 O12 1.615(9) . ? O1 C1 1.277(6) . ? O2 C3 1.292(6) . ? O3 C11 1.287(6) . ? O4 C13 1.296(7) . ? O5 C21 1.276(6) . ? O6 C23 1.280(7) . ? O7 C31 1.286(6) . ? O8 C33 1.284(6) . ? O9 C41 1.284(6) . ? O10 C43 1.286(6) . ? O11 C51 1.279(6) . ? O12 C53 1.283(6) . ? N1 C10 1.332(7) . ? N1 C6 1.338(7) . ? N2 C16 1.337(7) . ? N2 C20 1.347(7) . ? N2 Cu3 2.019(4) 3_557 ? N3 C26 1.344(7) . ? N3 C30 1.346(7) . ? N4 C36 1.341(6) . ? N4 C40 1.346(7) . ? N5 C46 1.338(7) . ? N5 C50 1.342(6) . ? N6 C56 1.334(7) . ? N6 C60 1.339(7) . ? N6 Cu3 2.017(4) 2_655 ? C1 C2 1.414(8) . ? C1 C5 1.485(9) . ? C2 C3 1.400(8) . ? C2 C8 1.485(7) . ? C3 C4 1.484(9) . ? C6 C7 1.386(7) . ? C7 C8 1.398(8) . ? C8 C9 1.375(8) . ? C9 C10 1.389(7) . ? C11 C12 1.404(8) . ? C11 C15 1.484(8) . ? C12 C13 1.406(8) . ? C12 C18 1.486(7) . ? C13 C14 1.489(9) . ? C16 C17 1.381(7) . ? C17 C18 1.397(7) . ? C18 C19 1.396(8) . ? C19 C20 1.370(8) . ? C21 C22 1.412(8) . ? C21 C25 1.488(9) . ? C22 C23 1.396(8) . ? C22 C28 1.504(7) . ? C23 C24 1.496(9) . ? C26 C27 1.386(7) . ? C27 C28 1.382(8) . ? C28 C29 1.391(8) . ? C29 C30 1.401(7) . ? C31 C32 1.402(8) . ? C31 C35 1.485(8) . ? C32 C33 1.417(8) . ? C32 C38 1.488(6) . ? C33 C34 1.499(9) . ? C36 C37 1.388(6) . ? C37 C38 1.388(7) . ? C38 C39 1.388(8) . ? C39 C40 1.385(7) . ? C41 C42 1.417(8) . ? C41 C45 1.488(8) . ? C42 C43 1.406(8) . ? C42 C48 1.488(7) . ? C43 C44 1.498(8) . ? C46 C47 1.384(7) . ? C47 C48 1.396(8) . ? C48 C49 1.376(7) . ? C49 C50 1.383(7) . ? C51 C52 1.396(8) . ? C51 C55 1.508(9) . ? C52 C53 1.408(8) . ? C52 C58 1.493(6) . ? C53 C54 1.494(9) . ? C56 C57 1.390(7) . ? C57 C58 1.393(7) . ? C58 C59 1.391(7) . ? C59 C60 1.383(7) . ? C1S Cl11 1.724(12) . ? C1S Cl12 1.756(11) . ? C1S Cl13 1.777(12) . ? C2S Cl23 1.73(2) . ? C2S Cl21 1.750(12) . ? C2S Cl22 1.766(13) . ? C3S Cl32 1.710(14) . ? C3S Cl33 1.77(2) . ? C3S Cl31 1.818(13) . ? C4S Cl42 1.66(2) . ? C4S Cl41 1.76(2) . ? C4S Cl43 1.81(3) . ? C5S Cl51 1.71(2) . ? C5S Cl55 1.71(2) . ? C5S Cl56 1.72(2) . ? C5S Cl53 1.75(2) . ? C5S Cl52 1.76(2) . ? C5S Cl54 1.78(2) . ? Cl51 Cl54 0.54(4) . ? C7S C9S 1.04(2) . ? C7S Cl92 1.24(2) . ? C7S Cl71 1.76(2) . ? C7S Cl72 1.77(2) . ? C7S Cl73 1.78(2) . ? C7S Cl93 1.95(2) . ? Cl71 Cl92 0.962(14) . ? Cl72 Cl93 1.45(2) . ? Cl72 Cl92 2.48(2) . ? Cl73 C9S 0.89(2) . ? Cl73 Cl91 0.971(14) . ? Cl73 Cl92 1.96(2) . ? Cl73 Cl93 2.31(2) . ? C9S Cl93 1.740(10) . ? C9S Cl92 1.746(10) . ? C9S Cl91 1.747(10) . ? C6S Cl61 1.74(2) . ? C6S Cl62 1.77(2) . ? C6S Cl63 1.78(2) . ? C8S Cl81 1.733(9) . ? C8S Cl83 1.748(9) . ? C8S Cl82 1.749(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 111.7(2) . . ? N1 Cu1 Br1 114.59(13) . . ? N3 Cu1 Br1 109.09(12) . . ? N1 Cu1 Br1 107.49(13) . 3_567 ? N3 Cu1 Br1 102.07(13) . 3_567 ? Br1 Cu1 Br1 111.14(3) . 3_567 ? N1 Cu1 Cu1 129.18(13) . 3_567 ? N3 Cu1 Cu1 118.18(12) . 3_567 ? Br1 Cu1 Cu1 57.08(2) . 3_567 ? Br1 Cu1 Cu1 54.06(2) 3_567 3_567 ? N5 Cu2 N4 127.3(2) . . ? N5 Cu2 Br2 105.19(13) . . ? N4 Cu2 Br2 103.52(12) . . ? N5 Cu2 Br3 104.58(12) . . ? N4 Cu2 Br3 102.05(13) . . ? Br2 Cu2 Br3 114.73(3) . . ? N5 Cu2 Cu3 119.55(12) . . ? N4 Cu2 Cu3 113.13(12) . . ? Br2 Cu2 Cu3 57.72(2) . . ? Br3 Cu2 Cu3 57.02(2) . . ? N6 Cu3 N2 120.7(2) 2_645 3_557 ? N6 Cu3 Br3 109.76(13) 2_645 . ? N2 Cu3 Br3 100.13(13) 3_557 . ? N6 Cu3 Br2 102.31(13) 2_645 . ? N2 Cu3 Br2 110.51(13) 3_557 . ? Br3 Cu3 Br2 114.02(3) . . ? N6 Cu3 Cu2 121.46(13) 2_645 . ? N2 Cu3 Cu2 117.87(12) 3_557 . ? Br3 Cu3 Cu2 57.37(2) . . ? Br2 Cu3 Cu2 56.67(2) . . ? Cu1 Br1 Cu1 68.86(3) . 3_567 ? Cu2 Br2 Cu3 65.61(2) . . ? Cu3 Br3 Cu2 65.61(2) . . ? O3 Be1 O1 114.1(5) . . ? O3 Be1 O2 109.4(6) . . ? O1 Be1 O2 106.4(4) . . ? O3 Be1 O4 107.1(4) . . ? O1 Be1 O4 107.4(5) . . ? O2 Be1 O4 112.4(5) . . ? O8 Be2 O7 105.9(4) . . ? O8 Be2 O6 111.3(6) . . ? O7 Be2 O6 113.0(5) . . ? O8 Be2 O5 112.4(5) . . ? O7 Be2 O5 108.2(6) . . ? O6 Be2 O5 106.1(4) . . ? O10 Be3 O11 113.8(5) . . ? O10 Be3 O9 106.0(4) . . ? O11 Be3 O9 109.3(6) . . ? O10 Be3 O12 110.3(6) . . ? O11 Be3 O12 106.1(4) . . ? O9 Be3 O12 111.5(5) . . ? C1 O1 Be1 123.2(5) . . ? C3 O2 Be1 122.5(5) . . ? C11 O3 Be1 122.9(5) . . ? C13 O4 Be1 121.1(5) . . ? C21 O5 Be2 124.1(5) . . ? C23 O6 Be2 123.7(5) . . ? C31 O7 Be2 124.2(5) . . ? C33 O8 Be2 124.5(4) . . ? C41 O9 Be3 124.3(4) . . ? C43 O10 Be3 123.8(4) . . ? C51 O11 Be3 123.6(5) . . ? C53 O12 Be3 123.8(5) . . ? C10 N1 C6 116.8(4) . . ? C10 N1 Cu1 120.0(4) . . ? C6 N1 Cu1 122.5(3) . . ? C16 N2 C20 116.7(4) . . ? C16 N2 Cu3 121.0(3) . 3_557 ? C20 N2 Cu3 122.3(3) . 3_557 ? C26 N3 C30 117.4(4) . . ? C26 N3 Cu1 124.0(3) . . ? C30 N3 Cu1 118.5(3) . . ? C36 N4 C40 116.6(4) . . ? C36 N4 Cu2 122.1(3) . . ? C40 N4 Cu2 121.2(3) . . ? C46 N5 C50 116.8(4) . . ? C46 N5 Cu2 122.6(3) . . ? C50 N5 Cu2 120.3(3) . . ? C56 N6 C60 117.1(4) . . ? C56 N6 Cu3 119.3(3) . 2_655 ? C60 N6 Cu3 123.3(4) . 2_655 ? O1 C1 C2 122.4(5) . . ? O1 C1 C5 116.2(5) . . ? C2 C1 C5 121.4(5) . . ? C3 C2 C1 120.0(5) . . ? C3 C2 C8 119.9(5) . . ? C1 C2 C8 119.9(5) . . ? O2 C3 C2 123.1(5) . . ? O2 C3 C4 115.2(5) . . ? C2 C3 C4 121.8(5) . . ? N1 C6 C7 123.8(5) . . ? C6 C7 C8 119.3(5) . . ? C9 C8 C7 116.3(5) . . ? C9 C8 C2 122.3(5) . . ? C7 C8 C2 121.4(5) . . ? C8 C9 C10 121.0(5) . . ? N1 C10 C9 122.7(5) . . ? O3 C11 C12 122.0(5) . . ? O3 C11 C15 115.9(5) . . ? C12 C11 C15 122.0(4) . . ? C11 C12 C13 121.7(5) . . ? C11 C12 C18 120.2(5) . . ? C13 C12 C18 118.0(5) . . ? O4 C13 C12 122.1(5) . . ? O4 C13 C14 115.1(5) . . ? C12 C13 C14 122.8(5) . . ? N2 C16 C17 123.2(5) . . ? C16 C17 C18 120.0(5) . . ? C19 C18 C17 116.4(5) . . ? C19 C18 C12 121.3(5) . . ? C17 C18 C12 122.2(5) . . ? C20 C19 C18 119.7(5) . . ? N2 C20 C19 123.8(5) . . ? O5 C21 C22 121.9(5) . . ? O5 C21 C25 115.7(5) . . ? C22 C21 C25 122.4(5) . . ? C23 C22 C21 121.1(5) . . ? C23 C22 C28 119.5(5) . . ? C21 C22 C28 119.3(5) . . ? O6 C23 C22 122.7(5) . . ? O6 C23 C24 115.9(5) . . ? C22 C23 C24 121.3(5) . . ? N3 C26 C27 123.6(5) . . ? C28 C27 C26 119.2(5) . . ? C27 C28 C29 118.0(5) . . ? C27 C28 C22 121.6(5) . . ? C29 C28 C22 120.4(5) . . ? C28 C29 C30 119.6(5) . . ? N3 C30 C29 122.1(5) . . ? O7 C31 C32 122.6(5) . . ? O7 C31 C35 115.0(5) . . ? C32 C31 C35 122.4(5) . . ? C31 C32 C33 120.1(4) . . ? C31 C32 C38 120.4(5) . . ? C33 C32 C38 119.5(5) . . ? O8 C33 C32 122.3(5) . . ? O8 C33 C34 114.7(5) . . ? C32 C33 C34 123.0(5) . . ? N4 C36 C37 122.9(4) . . ? C36 C37 C38 120.4(4) . . ? C39 C38 C37 116.5(4) . . ? C39 C38 C32 122.9(5) . . ? C37 C38 C32 120.6(4) . . ? C40 C39 C38 119.9(5) . . ? N4 C40 C39 123.5(5) . . ? O9 C41 C42 122.7(5) . . ? O9 C41 C45 115.0(5) . . ? C42 C41 C45 122.3(4) . . ? C43 C42 C41 119.3(4) . . ? C43 C42 C48 121.6(5) . . ? C41 C42 C48 119.1(5) . . ? O10 C43 C42 123.6(5) . . ? O10 C43 C44 114.8(5) . . ? C42 C43 C44 121.6(5) . . ? N5 C46 C47 123.2(5) . . ? C46 C47 C48 119.8(5) . . ? C49 C48 C47 116.6(4) . . ? C49 C48 C42 121.3(5) . . ? C47 C48 C42 122.0(5) . . ? C48 C49 C50 120.4(5) . . ? N5 C50 C49 123.0(5) . . ? O11 C51 C52 123.2(5) . . ? O11 C51 C55 115.2(5) . . ? C52 C51 C55 121.6(5) . . ? C51 C52 C53 120.5(4) . . ? C51 C52 C58 119.6(5) . . ? C53 C52 C58 120.0(5) . . ? O12 C53 C52 122.4(5) . . ? O12 C53 C54 115.9(5) . . ? C52 C53 C54 121.7(5) . . ? N6 C56 C57 123.2(5) . . ? C56 C57 C58 119.6(5) . . ? C59 C58 C57 117.0(4) . . ? C59 C58 C52 122.3(4) . . ? C57 C58 C52 120.6(4) . . ? C60 C59 C58 119.5(5) . . ? N6 C60 C59 123.6(5) . . ? Cl11 C1S Cl12 110.0(6) . . ? Cl11 C1S Cl13 110.4(6) . . ? Cl12 C1S Cl13 109.4(6) . . ? Cl23 C2S Cl21 109.9(7) . . ? Cl23 C2S Cl22 112.1(7) . . ? Cl21 C2S Cl22 111.0(6) . . ? Cl32 C3S Cl33 105.9(11) . . ? Cl32 C3S Cl31 112.9(6) . . ? Cl33 C3S Cl31 107.2(6) . . ? Cl42 C4S Cl41 115.1(13) . . ? Cl42 C4S Cl43 108.5(10) . . ? Cl41 C4S Cl43 111.6(11) . . ? Cl51 C5S Cl55 116.6(12) . . ? Cl51 C5S Cl56 116.7(15) . . ? Cl55 C5S Cl56 114.8(14) . . ? Cl51 C5S Cl53 111.5(11) . . ? Cl55 C5S Cl53 99.4(15) . . ? Cl56 C5S Cl53 93.7(11) . . ? Cl51 C5S Cl52 110.6(9) . . ? Cl55 C5S Cl52 12.3(12) . . ? Cl56 C5S Cl52 111.7(15) . . ? Cl53 C5S Cl52 111.7(10) . . ? Cl51 C5S Cl54 17.5(14) . . ? Cl55 C5S Cl54 109.1(11) . . ? Cl56 C5S Cl54 110.3(12) . . ? Cl53 C5S Cl54 129.0(18) . . ? Cl52 C5S Cl54 100.4(11) . . ? Cl54 Cl51 C5S 88.4(20) . . ? Cl51 Cl54 C5S 74.1(22) . . ? C9S C7S Cl92 99.8(18) . . ? C9S C7S Cl71 129.2(17) . . ? Cl92 C7S Cl71 31.7(8) . . ? C9S C7S Cl72 105.6(17) . . ? Cl92 C7S Cl72 109.8(13) . . ? Cl71 C7S Cl72 106.3(10) . . ? C9S C7S Cl73 20.8(12) . . ? Cl92 C7S Cl73 79.0(12) . . ? Cl71 C7S Cl73 108.9(10) . . ? Cl72 C7S Cl73 112.2(10) . . ? C9S C7S Cl93 62.9(12) . . ? Cl92 C7S Cl93 130.0(15) . . ? Cl71 C7S Cl93 147.3(12) . . ? Cl72 C7S Cl93 45.5(8) . . ? Cl73 C7S Cl93 76.6(9) . . ? Cl92 Cl71 C7S 42.4(11) . . ? Cl93 Cl72 C7S 73.7(10) . . ? Cl93 Cl72 Cl92 91.4(8) . . ? C7S Cl72 Cl92 28.0(6) . . ? C9S Cl73 Cl91 140.4(20) . . ? C9S Cl73 C7S 24.7(13) . . ? Cl91 Cl73 C7S 165.1(15) . . ? C9S Cl73 Cl92 62.9(12) . . ? Cl91 Cl73 Cl92 156.7(15) . . ? C7S Cl73 Cl92 38.2(7) . . ? C9S Cl73 Cl93 40.8(13) . . ? Cl91 Cl73 Cl93 113.4(12) . . ? C7S Cl73 Cl93 55.0(7) . . ? Cl92 Cl73 Cl93 85.0(6) . . ? Cl73 C9S C7S 134.5(23) . . ? Cl73 C9S Cl93 119.8(19) . . ? C7S C9S Cl93 84.9(14) . . ? Cl73 C9S Cl92 90.3(16) . . ? C7S C9S Cl92 44.2(12) . . ? Cl93 C9S Cl92 112.5(11) . . ? Cl73 C9S Cl91 20.7(10) . . ? C7S C9S Cl91 155.2(18) . . ? Cl93 C9S Cl91 109.1(10) . . ? Cl92 C9S Cl91 111.0(11) . . ? Cl73 Cl91 C9S 18.8(11) . . ? Cl71 Cl92 C7S 105.9(16) . . ? Cl71 Cl92 C9S 138.9(14) . . ? C7S Cl92 C9S 36.0(10) . . ? Cl71 Cl92 Cl73 159.1(14) . . ? C7S Cl92 Cl73 62.8(10) . . ? C9S Cl92 Cl73 26.8(7) . . ? Cl71 Cl92 Cl72 101.2(11) . . ? C7S Cl92 Cl72 42.3(9) . . ? C9S Cl92 Cl72 62.6(7) . . ? Cl73 Cl92 Cl72 82.2(6) . . ? Cl72 Cl93 C9S 91.0(9) . . ? Cl72 Cl93 C7S 60.8(7) . . ? C9S Cl93 C7S 32.2(7) . . ? Cl72 Cl93 Cl73 100.6(7) . . ? C9S Cl93 Cl73 19.4(7) . . ? C7S Cl93 Cl73 48.4(6) . . ? Cl61 C6S Cl62 108.3(11) . . ? Cl61 C6S Cl63 108.6(10) . . ? Cl62 C6S Cl63 106.2(10) . . ? Cl81 C8S Cl83 118.7(10) . . ? Cl81 C8S Cl82 112.4(10) . . ? Cl83 C8S Cl82 105.5(9) . . ? _refine_diff_density_max 1.806 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.117 #==============================================================================