# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Ba Cd N O13, H2 O' _chemical_formula_sum 'C32 H30 Ba Cd N O14' _chemical_formula_weight 902.31 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2339(4) _cell_length_b 22.3320(14) _cell_length_c 23.4396(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3786.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10765 _cell_measurement_theta_min 3.0836 _cell_measurement_theta_max 27.4565 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7221 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 4900 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24084 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6669 _reflns_number_gt 6460 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+2.7675P] 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 contr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 6669 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.79459(6) 0.486806(19) 0.187075(16) 0.03334(12) Uani 1 1 d . . . Ba1 Ba 0.31748(5) 0.546007(15) 0.227610(14) 0.03364(11) Uani 1 1 d . . . C1 C -0.1617(9) 0.4344(3) 0.6035(3) 0.0397(14) Uani 1 1 d . . . C2 C -0.0846(9) 0.3971(3) 0.5552(3) 0.0389(14) Uani 1 1 d . . . C3 C -0.1729(11) 0.3453(3) 0.5367(3) 0.0487(16) Uani 1 1 d . . . H3A H -0.2801 0.3325 0.5548 0.058 Uiso 1 1 calc R . . C4 C -0.1028(11) 0.3128(3) 0.4916(3) 0.0507(18) Uani 1 1 d . . . H4A H -0.1621 0.2780 0.4798 0.061 Uiso 1 1 calc R . . C5 C 0.0587(12) 0.3322(3) 0.4633(3) 0.0483(17) Uani 1 1 d . . . C6 C 0.1453(11) 0.3834(3) 0.4814(3) 0.057(2) Uani 1 1 d . . . H6A H 0.2514 0.3967 0.4629 0.068 Uiso 1 1 calc R . . C7 C 0.0758(12) 0.4150(3) 0.5265(3) 0.0541(19) Uani 1 1 d . . . H7A H 0.1369 0.4494 0.5385 0.065 Uiso 1 1 calc R . . C8 C 0.2400(10) 0.3229(3) 0.3795(3) 0.0464(17) Uani 1 1 d . . . C9 C 0.1679(11) 0.3594(3) 0.3372(3) 0.0492(16) Uani 1 1 d . . . H9A H 0.0417 0.3672 0.3357 0.059 Uiso 1 1 calc R . . C10 C 0.2856(10) 0.3841(3) 0.2975(3) 0.0452(15) Uani 1 1 d . . . H10A H 0.2379 0.4086 0.2689 0.054 Uiso 1 1 calc R . . C11 C 0.4724(10) 0.3731(3) 0.2994(3) 0.0408(14) Uani 1 1 d . . . C12 C 0.5418(12) 0.3350(4) 0.3397(3) 0.062(2) Uani 1 1 d . . . H12A H 0.6676 0.3265 0.3406 0.074 Uiso 1 1 calc R . . C13 C 0.4215(12) 0.3085(4) 0.3801(4) 0.063(2) Uani 1 1 d . . . H13A H 0.4668 0.2814 0.4068 0.076 Uiso 1 1 calc R . . C14 C 0.6024(9) 0.4064(3) 0.2608(3) 0.0400(15) Uani 1 1 d . . . C15 C 0.8157(8) 0.5728(3) 0.2752(2) 0.0405(14) Uani 1 1 d . . . C16 C 0.8407(8) 0.6045(3) 0.3309(2) 0.0364(13) Uani 1 1 d . . . C17 C 0.9904(10) 0.5874(4) 0.3665(3) 0.064(3) Uani 1 1 d . . . H17A H 1.0685 0.5564 0.3555 0.076 Uiso 1 1 calc R . . C18 C 1.0194(12) 0.6166(4) 0.4172(3) 0.064(2) Uani 1 1 d . . . H18A H 1.1215 0.6067 0.4394 0.076 Uiso 1 1 calc R . . C19 C 0.9001(10) 0.6598(3) 0.4354(3) 0.0391(15) Uani 1 1 d . . . C20 C 0.7506(11) 0.6754(3) 0.4026(3) 0.0524(19) Uani 1 1 d . . . H20A H 0.6687 0.7046 0.4152 0.063 Uiso 1 1 calc R . . C21 C 0.7218(10) 0.6472(3) 0.3502(3) 0.0450(15) Uani 1 1 d . . . H21A H 0.6199 0.6577 0.3281 0.054 Uiso 1 1 calc R . . C22 C 1.0523(10) 0.6647(3) 0.5241(2) 0.0376(14) Uani 1 1 d . . . C23 C 1.2350(11) 0.6808(3) 0.5206(3) 0.0446(16) Uani 1 1 d . . . H23A H 1.2726 0.7102 0.4951 0.054 Uiso 1 1 calc R . . C24 C 1.3638(10) 0.6525(3) 0.5558(3) 0.0400(15) Uani 1 1 d . . . H24A H 1.4885 0.6623 0.5534 0.048 Uiso 1 1 calc R . . C25 C 1.3032(8) 0.6090(2) 0.5946(2) 0.0305(11) Uani 1 1 d . . . C26 C 1.1154(9) 0.5960(3) 0.5994(3) 0.0439(16) Uani 1 1 d . . . H26A H 1.0740 0.5688 0.6267 0.053 Uiso 1 1 calc R . . C27 C 0.9892(9) 0.6244(3) 0.5626(3) 0.0473(17) Uani 1 1 d . . . H27A H 0.8637 0.6156 0.5647 0.057 Uiso 1 1 calc R . . C28 C 1.4416(9) 0.5753(3) 0.6295(2) 0.0341(13) Uani 1 1 d . . . C30 C 0.1577(13) 0.6930(3) 0.2704(4) 0.066(2) Uani 1 1 d . . . H30A H 0.0602 0.6823 0.2466 0.080 Uiso 1 1 calc R . . C31 C 0.292(2) 0.7626(5) 0.3364(5) 0.118(5) Uani 1 1 d . . . H31A H 0.3886 0.7332 0.3360 0.176 Uiso 1 1 calc R . . H31B H 0.2459 0.7671 0.3746 0.176 Uiso 1 1 calc R . . H31C H 0.3398 0.8003 0.3233 0.176 Uiso 1 1 calc R . . C32 C -0.0212(16) 0.7810(4) 0.2922(5) 0.087(3) Uani 1 1 d . . . H32A H -0.1076 0.7606 0.2680 0.130 Uiso 1 1 calc R . . H32B H 0.0129 0.8184 0.2750 0.130 Uiso 1 1 calc R . . H32C H -0.0770 0.7883 0.3287 0.130 Uiso 1 1 calc R . . O1 O -0.0506(7) 0.4657(2) 0.63147(18) 0.0472(11) Uani 1 1 d . . . O2 O -0.3298(7) 0.4337(2) 0.6135(2) 0.0546(12) Uani 1 1 d . . . O3 O 0.1185(9) 0.2967(2) 0.4200(2) 0.0605(16) Uani 1 1 d . . . O4 O 0.7727(7) 0.3967(3) 0.2628(2) 0.0656(15) Uani 1 1 d . . . O5 O 0.5363(6) 0.44608(19) 0.22794(17) 0.0418(10) Uani 1 1 d . . . O6 O 0.9437(6) 0.5387(2) 0.25769(18) 0.0492(12) Uani 1 1 d . . . O7 O 0.6679(7) 0.5793(3) 0.2484(2) 0.0517(12) Uani 1 1 d . . . O8 O 0.9237(7) 0.6898(2) 0.48662(19) 0.0491(12) Uani 1 1 d . . . O9 O 1.6106(6) 0.5839(2) 0.62230(19) 0.0439(11) Uani 1 1 d . . . O10 O 1.3829(6) 0.5373(2) 0.66535(19) 0.0430(11) Uani 1 1 d . . . O11 O 0.2939(10) 0.6589(3) 0.2732(3) 0.0838(19) Uani 1 1 d . . . O12 O 0.4083(9) 0.5203(3) 0.3428(2) 0.0725(16) Uani 1 1 d . . . H13C H 0.5159 0.5044 0.3548 0.087 Uiso 1 1 d R . . H13B H 0.3213 0.5294 0.3635 0.109 Uiso 1 1 d R . . N1 N 0.1448(11) 0.7437(3) 0.2997(3) 0.0662(19) Uani 1 1 d . . . O13 O 0.1418(9) 0.6198(3) 0.1488(3) 0.0725(17) Uani 1 1 d . . . O14 O 0.5639(10) 0.5029(3) 0.4223(3) 0.088(2) Uani 1 1 d . . . H16A H 0.6785 0.4879 0.4264 0.105 Uiso 1 1 d R . . H16B H 0.4936 0.5102 0.4532 0.105 Uiso 1 1 d R . . C33 C 0.191(2) 0.6750(5) 0.1266(5) 0.112(4) Uani 1 1 d . . . H33A H 0.0974 0.6881 0.1003 0.168 Uiso 1 1 calc R . . H33B H 0.3069 0.6716 0.1071 0.168 Uiso 1 1 calc R . . H33C H 0.2015 0.7035 0.1570 0.168 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0228(2) 0.0501(2) 0.0271(2) -0.00357(17) 0.00054(17) 0.00247(18) Ba1 0.02284(17) 0.04387(19) 0.03421(18) -0.00795(14) -0.00401(14) 0.00474(13) C1 0.039(4) 0.051(3) 0.028(3) 0.006(3) 0.004(3) 0.000(3) C2 0.037(3) 0.051(3) 0.029(3) -0.009(3) 0.006(3) -0.005(3) C3 0.046(4) 0.059(4) 0.041(3) -0.004(3) 0.015(3) -0.007(3) C4 0.058(4) 0.048(4) 0.046(4) -0.009(3) 0.012(3) -0.015(3) C5 0.065(5) 0.050(4) 0.030(3) -0.002(3) 0.015(3) -0.004(3) C6 0.055(5) 0.065(4) 0.051(4) -0.010(3) 0.025(4) -0.021(4) C7 0.060(5) 0.056(4) 0.046(4) -0.017(3) 0.016(4) -0.026(4) C8 0.060(5) 0.045(3) 0.034(3) -0.005(3) 0.019(3) -0.009(3) C9 0.042(4) 0.054(4) 0.052(4) 0.000(3) 0.016(3) 0.000(3) C10 0.045(4) 0.055(4) 0.035(3) 0.004(3) 0.004(3) 0.006(3) C11 0.044(4) 0.042(3) 0.036(3) 0.001(3) 0.008(3) 0.010(3) C12 0.049(4) 0.070(5) 0.067(5) 0.029(4) 0.010(4) 0.016(4) C13 0.062(5) 0.071(5) 0.055(4) 0.036(4) 0.014(4) 0.010(4) C14 0.041(4) 0.046(3) 0.034(3) 0.003(3) 0.009(3) 0.007(3) C15 0.027(3) 0.068(4) 0.028(3) -0.010(3) -0.001(3) -0.009(3) C16 0.022(3) 0.058(3) 0.029(3) -0.012(3) -0.002(2) 0.005(3) C17 0.041(4) 0.106(6) 0.044(4) -0.043(4) -0.015(3) 0.032(4) C18 0.053(5) 0.099(6) 0.039(4) -0.023(4) -0.022(4) 0.034(4) C19 0.053(4) 0.038(3) 0.027(3) 0.000(2) -0.008(3) 0.007(3) C20 0.056(5) 0.052(4) 0.049(4) -0.014(3) -0.019(3) 0.021(3) C21 0.040(4) 0.057(4) 0.038(3) -0.012(3) -0.017(3) 0.011(3) C22 0.051(4) 0.034(3) 0.028(3) -0.007(2) -0.011(3) 0.010(3) C23 0.065(5) 0.036(3) 0.033(3) 0.008(2) -0.011(3) -0.006(3) C24 0.042(4) 0.044(3) 0.035(3) 0.001(3) -0.009(3) -0.007(3) C25 0.028(3) 0.039(3) 0.024(2) -0.002(2) -0.002(3) 0.000(3) C26 0.036(3) 0.057(4) 0.038(3) 0.019(3) -0.001(3) 0.001(3) C27 0.021(3) 0.069(5) 0.052(4) 0.003(3) -0.005(3) 0.005(3) C28 0.037(3) 0.041(3) 0.025(3) 0.000(2) -0.001(3) 0.001(3) C30 0.073(6) 0.050(4) 0.076(5) -0.009(4) 0.004(5) 0.009(4) C31 0.138(11) 0.086(7) 0.129(10) -0.056(7) -0.058(9) 0.026(8) C32 0.094(7) 0.067(6) 0.099(7) -0.001(5) 0.012(6) 0.028(5) O1 0.054(3) 0.059(3) 0.028(2) -0.0118(19) 0.000(2) -0.006(2) O2 0.046(3) 0.073(3) 0.045(3) -0.015(2) 0.013(2) 0.002(3) O3 0.087(4) 0.047(3) 0.047(3) -0.011(2) 0.038(3) -0.012(3) O4 0.040(3) 0.095(4) 0.062(3) 0.024(3) 0.014(3) 0.015(3) O5 0.045(2) 0.049(2) 0.031(2) 0.003(2) 0.010(2) 0.0054(19) O6 0.030(2) 0.086(3) 0.032(2) -0.024(2) 0.0020(18) 0.010(2) O7 0.030(2) 0.079(3) 0.046(2) -0.021(2) -0.011(2) -0.001(2) O8 0.063(3) 0.044(2) 0.040(2) -0.0111(19) -0.024(2) 0.022(2) O9 0.030(2) 0.061(3) 0.041(2) 0.014(2) -0.0031(19) -0.005(2) O10 0.034(2) 0.056(3) 0.039(2) 0.021(2) 0.0003(19) -0.0004(19) O11 0.075(4) 0.060(3) 0.116(5) -0.039(3) -0.014(5) 0.019(3) O12 0.073(4) 0.093(4) 0.052(3) 0.000(3) -0.008(3) 0.007(3) N1 0.081(5) 0.051(3) 0.067(4) -0.007(3) 0.006(4) 0.010(3) O13 0.066(4) 0.062(3) 0.089(4) 0.022(3) -0.025(3) -0.009(3) O14 0.078(4) 0.110(5) 0.076(4) -0.001(4) -0.011(4) -0.008(4) C33 0.143(11) 0.078(6) 0.116(9) 0.024(6) -0.010(10) 0.023(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 Cd1 O6 2.290(4) . ? Cd1 O5 2.288(4) . ? Cd1 O9 2.296(4) 2_764 ? Cd1 O1 2.437(5) 2_564 ? Cd1 O10 2.448(4) 2_764 ? Cd1 O2 2.490(5) 2_564 ? Cd1 C28 2.718(6) 2_764 ? Cd1 Ba1 3.8160(5) . ? Cd1 Ba1 4.1181(5) 1_655 ? Ba1 O7 2.687(5) . ? Ba1 O5 2.736(4) . ? Ba1 O11 2.744(5) . ? Ba1 O13 2.783(6) . ? Ba1 O10 2.774(4) 2_664 ? Ba1 O6 2.799(4) 1_455 ? Ba1 O1 2.827(5) 2_564 ? Ba1 O12 2.838(5) . ? Ba1 Cd1 4.1181(5) 1_455 ? C1 O2 1.238(9) . ? C1 O1 1.251(8) . ? C1 C2 1.513(8) . ? C2 C3 1.390(9) . ? C2 C7 1.399(10) . ? C3 C4 1.378(9) . ? C3 H3A 0.9300 . ? C4 C5 1.413(10) . ? C4 H4A 0.9300 . ? C5 C6 1.371(10) . ? C5 O3 1.358(8) . ? C6 C7 1.368(10) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.351(11) . ? C8 C9 1.385(10) . ? C8 O3 1.421(8) . ? C9 C10 1.377(10) . ? C9 H9A 0.9300 . ? C10 C11 1.374(10) . ? C10 H10A 0.9300 . ? C11 C12 1.368(10) . ? C11 C14 1.502(9) . ? C12 C13 1.415(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O4 1.252(8) . ? C14 O5 1.268(8) . ? C15 O7 1.248(8) . ? C15 O6 1.267(8) . ? C15 C16 1.496(8) . ? C16 C21 1.360(9) . ? C16 C17 1.420(9) . ? C17 C18 1.371(10) . ? C17 H17A 0.9300 . ? C18 C19 1.364(10) . ? C18 H18A 0.9300 . ? C19 C20 1.372(9) . ? C19 O8 1.386(7) . ? C20 C21 1.396(9) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.354(10) . ? C22 C23 1.371(10) . ? C22 O8 1.397(7) . ? C23 C24 1.395(9) . ? C23 H23A 0.9300 . ? C24 C25 1.401(9) . ? C24 H24A 0.9300 . ? C25 C26 1.394(9) . ? C25 C28 1.495(8) . ? C26 C27 1.408(9) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 O9 1.249(8) . ? C28 O10 1.267(7) . ? C28 Cd1 2.718(6) 2_765 ? C30 O11 1.247(10) . ? C30 N1 1.327(10) . ? C30 H30A 0.9300 . ? C31 N1 1.433(13) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N1 1.471(13) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O1 Cd1 2.437(5) 2_565 ? O1 Ba1 2.827(5) 2_565 ? O2 Cd1 2.490(5) 2_565 ? O6 Ba1 2.799(4) 1_655 ? O9 Cd1 2.296(4) 2_765 ? O10 Cd1 2.448(4) 2_765 ? O10 Ba1 2.774(4) 2_665 ? O12 H13C 0.8999 . ? O12 H13B 0.8200 . ? O13 C33 1.384(12) . ? O14 H16A 0.8999 . ? O14 H16B 0.9000 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 O6 Cd1 O5 106.44(16) . . ? O6 Cd1 O9 133.26(16) . 2_764 ? O5 Cd1 O9 104.32(16) . 2_764 ? O6 Cd1 O1 120.49(18) . 2_564 ? O5 Cd1 O1 78.78(15) . 2_564 ? O9 Cd1 O1 99.33(16) 2_764 2_564 ? O6 Cd1 O10 79.22(14) . 2_764 ? O5 Cd1 O10 141.06(16) . 2_764 ? O9 Cd1 O10 54.99(15) 2_764 2_764 ? O1 Cd1 O10 132.44(16) 2_564 2_764 ? O6 Cd1 O2 95.26(18) . 2_564 ? O5 Cd1 O2 131.10(16) . 2_564 ? O9 Cd1 O2 90.11(17) 2_764 2_564 ? O1 Cd1 O2 52.63(16) 2_564 2_564 ? O10 Cd1 O2 85.14(17) 2_764 2_564 ? O6 Cd1 C28 106.64(17) . 2_764 ? O5 Cd1 C28 125.32(16) . 2_764 ? O9 Cd1 C28 27.22(17) 2_764 2_764 ? O1 Cd1 C28 117.74(16) 2_564 2_764 ? O10 Cd1 C28 27.77(16) 2_764 2_764 ? O2 Cd1 C28 87.05(18) 2_564 2_764 ? O6 Cd1 Ba1 94.05(11) . . ? O5 Cd1 Ba1 45.17(11) . . ? O9 Cd1 Ba1 132.32(11) 2_764 . ? O1 Cd1 Ba1 47.73(11) 2_564 . ? O10 Cd1 Ba1 171.89(10) 2_764 . ? O2 Cd1 Ba1 91.03(13) 2_564 . ? C28 Cd1 Ba1 159.31(13) 2_764 . ? O6 Cd1 Ba1 40.39(10) . 1_655 ? O5 Cd1 Ba1 141.36(11) . 1_655 ? O9 Cd1 Ba1 95.68(11) 2_764 1_655 ? O1 Cd1 Ba1 130.47(11) 2_564 1_655 ? O10 Cd1 Ba1 40.82(10) 2_764 1_655 ? O2 Cd1 Ba1 80.61(12) 2_564 1_655 ? C28 Cd1 Ba1 68.49(13) 2_764 1_655 ? Ba1 Cd1 Ba1 131.458(14) . 1_655 ? O7 Ba1 O5 71.31(15) . . ? O7 Ba1 O11 74.52(19) . . ? O5 Ba1 O11 141.65(18) . . ? O7 Ba1 O13 112.80(18) . . ? O5 Ba1 O13 138.53(17) . . ? O11 Ba1 O13 71.7(2) . . ? O7 Ba1 O10 140.77(14) . 2_664 ? O5 Ba1 O10 75.92(14) . 2_664 ? O11 Ba1 O10 142.09(17) . 2_664 ? O13 Ba1 O10 79.01(16) . 2_664 ? O7 Ba1 O6 151.86(13) . 1_455 ? O5 Ba1 O6 120.71(15) . 1_455 ? O11 Ba1 O6 84.00(19) . 1_455 ? O13 Ba1 O6 76.14(18) . 1_455 ? O10 Ba1 O6 65.70(12) 2_664 1_455 ? O7 Ba1 O1 66.91(14) . 2_564 ? O5 Ba1 O1 65.27(13) . 2_564 ? O11 Ba1 O1 115.6(2) . 2_564 ? O13 Ba1 O1 78.36(18) . 2_564 ? O10 Ba1 O1 80.22(13) 2_664 2_564 ? O6 Ba1 O1 140.50(13) 1_455 2_564 ? O7 Ba1 O12 70.42(17) . . ? O5 Ba1 O12 72.43(15) . . ? O11 Ba1 O12 80.2(2) . . ? O13 Ba1 O12 149.0(2) . . ? O10 Ba1 O12 119.05(17) 2_664 . ? O6 Ba1 O12 88.40(16) 1_455 . ? O1 Ba1 O12 127.00(17) 2_564 . ? O7 Ba1 Cd1 44.60(11) . . ? O5 Ba1 Cd1 36.37(9) . . ? O11 Ba1 Cd1 118.13(15) . . ? O13 Ba1 Cd1 116.94(15) . . ? O10 Ba1 Cd1 96.27(9) 2_664 . ? O6 Ba1 Cd1 156.38(11) 1_455 . ? O1 Ba1 Cd1 39.64(9) 2_564 . ? O12 Ba1 Cd1 87.55(13) . . ? O7 Ba1 Cd1 175.97(10) . 1_455 ? O5 Ba1 Cd1 105.68(10) . 1_455 ? O11 Ba1 Cd1 109.14(15) . 1_455 ? O13 Ba1 Cd1 67.50(12) . 1_455 ? O10 Ba1 Cd1 35.23(9) 2_664 1_455 ? O6 Ba1 Cd1 32.02(9) 1_455 1_455 ? O1 Ba1 Cd1 109.52(10) 2_564 1_455 ? O12 Ba1 Cd1 111.54(13) . 1_455 ? Cd1 Ba1 Cd1 131.458(14) . 1_455 ? O2 C1 O1 122.7(6) . . ? O2 C1 C2 119.7(6) . . ? O1 C1 C2 117.6(6) . . ? C3 C2 C7 118.0(6) . . ? C3 C2 C1 121.5(6) . . ? C7 C2 C1 120.5(6) . . ? C4 C3 C2 120.6(7) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C6 C5 O3 125.0(7) . . ? C6 C5 C4 119.2(6) . . ? O3 C5 C4 115.8(6) . . ? C5 C6 C7 120.1(7) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C2 121.9(6) . . ? C6 C7 H7A 119.0 . . ? C2 C7 H7A 119.0 . . ? C13 C8 C9 120.9(6) . . ? C13 C8 O3 119.7(7) . . ? C9 C8 O3 119.2(7) . . ? C10 C9 C8 119.1(7) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C11 C10 C9 120.9(7) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 119.6(7) . . ? C12 C11 C14 119.6(7) . . ? C10 C11 C14 120.5(6) . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C8 C13 C12 119.4(7) . . ? C8 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? O4 C14 O5 121.0(6) . . ? O4 C14 C11 120.5(6) . . ? O5 C14 C11 118.4(6) . . ? O7 C15 O6 122.2(5) . . ? O7 C15 C16 119.1(6) . . ? O6 C15 C16 118.6(5) . . ? C21 C16 C17 118.4(5) . . ? C21 C16 C15 123.0(6) . . ? C17 C16 C15 118.5(5) . . ? C18 C17 C16 119.8(7) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C19 C18 C17 120.7(7) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 120.2(6) . . ? C18 C19 O8 122.4(6) . . ? C20 C19 O8 117.4(6) . . ? C19 C20 C21 119.8(6) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C16 C21 C20 120.9(6) . . ? C16 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C27 C22 C23 122.6(6) . . ? C27 C22 O8 117.4(6) . . ? C23 C22 O8 120.0(6) . . ? C22 C23 C24 119.3(6) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C23 C24 C25 119.2(6) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 120.1(6) . . ? C26 C25 C28 120.2(5) . . ? C24 C25 C28 119.6(6) . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? C22 C27 C26 119.3(6) . . ? C22 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? O9 C28 O10 121.4(6) . . ? O9 C28 C25 120.2(5) . . ? O10 C28 C25 118.4(6) . . ? O9 C28 Cd1 57.2(3) . 2_765 ? O10 C28 Cd1 64.2(3) . 2_765 ? C25 C28 Cd1 176.5(4) . 2_765 ? O11 C30 N1 123.3(9) . . ? O11 C30 H30A 118.4 . . ? N1 C30 H30A 118.4 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 O1 Cd1 93.3(4) . 2_565 ? C1 O1 Ba1 138.5(4) . 2_565 ? Cd1 O1 Ba1 92.63(13) 2_565 2_565 ? C1 O2 Cd1 91.2(4) . 2_565 ? C5 O3 C8 117.1(5) . . ? C14 O5 Cd1 103.0(4) . . ? C14 O5 Ba1 142.1(4) . . ? Cd1 O5 Ba1 98.46(15) . . ? C15 O6 Cd1 101.2(3) . . ? C15 O6 Ba1 138.8(4) . 1_655 ? Cd1 O6 Ba1 107.60(15) . 1_655 ? C15 O7 Ba1 150.2(5) . . ? C19 O8 C22 115.7(5) . . ? C28 O9 Cd1 95.6(4) . 2_765 ? C28 O10 Cd1 88.1(4) . 2_765 ? C28 O10 Ba1 166.7(4) . 2_665 ? Cd1 O10 Ba1 103.95(14) 2_765 2_665 ? C30 O11 Ba1 126.1(6) . . ? Ba1 O12 H13C 125.2 . . ? Ba1 O12 H13B 109.5 . . ? H13C O12 H13B 125.3 . . ? C30 N1 C31 120.6(8) . . ? C30 N1 C32 118.6(8) . . ? C31 N1 C32 120.7(8) . . ? C33 O13 Ba1 131.3(7) . . ? H16A O14 H16B 120.0 . . ? O13 C33 H33A 109.5 . . ? O13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.603 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.117 _database_code_depnum_ccdc_archive 'CCDC 960504' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Ba Cd N O13, H2 O' _chemical_formula_sum 'C32 H30 Ba Cd N O14' _chemical_formula_weight 902.31 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2243(6) _cell_length_b 22.315(2) _cell_length_c 23.376(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3768.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9596 _cell_measurement_theta_min 2.7678 _cell_measurement_theta_max 27.4701 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8261 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29401 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8546 _reflns_number_gt 7340 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+6.7545P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 8546 _refine_ls_number_parameters 442 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20569(8) 0.48691(3) 0.18669(2) 0.03821(14) Uani 1 1 d . . . Ba1 Ba 0.68297(7) 0.54600(2) 0.227462(19) 0.03829(12) Uani 1 1 d . . . C1 C 0.3962(14) 0.4058(4) 0.2609(4) 0.046(2) Uani 1 1 d . . . C2 C 0.5272(14) 0.3734(4) 0.2986(4) 0.045(2) Uani 1 1 d . . . C3 C 0.4642(18) 0.3340(5) 0.3405(5) 0.068(3) Uani 1 1 d . . . H3A H 0.3380 0.3260 0.3426 0.081 Uiso 1 1 calc R . . C4 C 0.5779(19) 0.3068(6) 0.3783(6) 0.079(4) Uani 1 1 d . . . H4A H 0.5325 0.2777 0.4030 0.095 Uiso 1 1 calc R . . C5 C 0.7610(15) 0.3227(4) 0.3797(4) 0.050(2) Uani 1 1 d . . . C6 C 0.8312(16) 0.3590(4) 0.3380(5) 0.058(2) Uani 1 1 d . . . H6A H 0.9576 0.3668 0.3369 0.070 Uiso 1 1 calc R . . C7 C 0.7151(14) 0.3842(4) 0.2972(4) 0.047(2) Uani 1 1 d . . . H7A H 0.7645 0.4085 0.2688 0.056 Uiso 1 1 calc R . . C8 C 0.9428(16) 0.3316(4) 0.4636(4) 0.052(2) Uani 1 1 d . . . C9 C 1.1035(16) 0.3130(5) 0.4916(4) 0.056(3) Uani 1 1 d . . . H9A H 1.1656 0.2788 0.4793 0.067 Uiso 1 1 calc R . . C13 C 0.8569(15) 0.3841(5) 0.4802(4) 0.060(3) Uani 1 1 d . . . H13A H 0.7553 0.3985 0.4601 0.072 Uiso 1 1 calc R . . C10 C 1.1684(17) 0.3445(4) 0.5363(4) 0.058(2) Uani 1 1 d . . . H10A H 1.2731 0.3308 0.5554 0.069 Uiso 1 1 calc R . . C11 C 1.0844(14) 0.3966(4) 0.5545(4) 0.048(2) Uani 1 1 d . . . C12 C 0.9231(16) 0.4147(5) 0.5270(5) 0.062(3) Uani 1 1 d . . . H12A H 0.8592 0.4481 0.5404 0.074 Uiso 1 1 calc R . . C14 C 1.1593(14) 0.4340(4) 0.6030(4) 0.046(2) Uani 1 1 d . . . C15 C 0.1848(12) 0.5728(4) 0.2753(3) 0.0437(18) Uani 1 1 d . . . C16 C 0.1595(11) 0.6047(4) 0.3305(3) 0.0414(18) Uani 1 1 d . . . C17 C 0.0078(14) 0.5897(6) 0.3650(4) 0.064(3) Uani 1 1 d . . . H17A H -0.0762 0.5610 0.3526 0.077 Uiso 1 1 calc R . . C18 C -0.0178(16) 0.6169(5) 0.4167(4) 0.064(3) Uani 1 1 d . . . H18A H -0.1174 0.6061 0.4397 0.077 Uiso 1 1 calc R . . C19 C 0.1026(14) 0.6599(4) 0.4345(3) 0.044(2) Uani 1 1 d . . . C20 C 0.2455(14) 0.6756(4) 0.4014(4) 0.053(2) Uani 1 1 d . . . H20A H 0.3228 0.7066 0.4131 0.064 Uiso 1 1 calc R . . C21 C 0.2808(15) 0.6466(4) 0.3500(4) 0.049(2) Uani 1 1 d . . . H21A H 0.3865 0.6557 0.3290 0.058 Uiso 1 1 calc R . . C22 C -0.0536(14) 0.6642(3) 0.5240(3) 0.0396(19) Uani 1 1 d . . . C23 C -0.2362(14) 0.6811(4) 0.5200(4) 0.048(2) Uani 1 1 d . . . H23A H -0.2739 0.7106 0.4945 0.057 Uiso 1 1 calc R . . C24 C -0.3636(13) 0.6522(4) 0.5558(4) 0.0410(19) Uani 1 1 d . . . H24A H -0.4886 0.6618 0.5537 0.049 Uiso 1 1 calc R . . C25 C -0.3038(11) 0.6095(3) 0.5942(3) 0.0335(15) Uani 1 1 d . . . C26 C -0.1178(13) 0.5963(4) 0.5996(4) 0.046(2) Uani 1 1 d . . . H26A H -0.0784 0.5691 0.6272 0.055 Uiso 1 1 calc R . . C27 C 0.0128(13) 0.6242(5) 0.5632(4) 0.049(2) Uani 1 1 d . . . H27A H 0.1385 0.6156 0.5659 0.059 Uiso 1 1 calc R . . C28 C -0.4416(14) 0.5748(4) 0.6302(3) 0.0429(19) Uani 1 1 d . . . C29 C 0.8415(19) 0.6935(5) 0.2687(6) 0.071(3) Uani 1 1 d . . . H29A H 0.9344 0.6834 0.2428 0.085 Uiso 1 1 calc R . . C30 C 0.694(4) 0.7610(8) 0.3391(9) 0.175(11) Uani 1 1 d . . . H30A H 0.5998 0.7306 0.3367 0.262 Uiso 1 1 calc R . . H30B H 0.6431 0.7988 0.3273 0.262 Uiso 1 1 calc R . . H30C H 0.7366 0.7640 0.3779 0.262 Uiso 1 1 calc R . . C31 C 1.023(2) 0.7810(5) 0.2927(7) 0.093(5) Uani 1 1 d . . . H31A H 1.1087 0.7622 0.2668 0.139 Uiso 1 1 calc R . . H31B H 1.0813 0.7860 0.3294 0.139 Uiso 1 1 calc R . . H31C H 0.9879 0.8194 0.2780 0.139 Uiso 1 1 calc R . . O1 O 0.4649(9) 0.4461(3) 0.2270(2) 0.0454(13) Uani 1 1 d . . . O2 O 0.2295(11) 0.3963(4) 0.2615(3) 0.070(2) Uani 1 1 d . . . O3 O 0.8781(13) 0.2965(3) 0.4196(3) 0.068(2) Uani 1 1 d . . . O4 O 1.3316(11) 0.4340(4) 0.6130(3) 0.0630(19) Uani 1 1 d . . . O5 O 1.0486(10) 0.4657(3) 0.6312(3) 0.0548(17) Uani 1 1 d . . . O6 O 0.0568(9) 0.5393(4) 0.2568(3) 0.0547(17) Uani 1 1 d . . . O7 O 0.3304(10) 0.5792(3) 0.2483(3) 0.0565(17) Uani 1 1 d . . . O8 O 0.0754(10) 0.6899(3) 0.4861(3) 0.0494(16) Uani 1 1 d . . . O9 O -0.3834(9) 0.5375(3) 0.6660(2) 0.0476(15) Uani 1 1 d . . . O10 O -0.6113(8) 0.5840(3) 0.6217(3) 0.0444(14) Uani 1 1 d . . . O11 O 0.8613(14) 0.6192(4) 0.1469(5) 0.086(3) Uani 1 1 d . . . O12 O 0.7055(15) 0.6589(4) 0.2730(5) 0.092(3) Uani 1 1 d . . . O13 O 0.5845(14) 0.5208(4) 0.3422(3) 0.083(3) Uani 1 1 d . . . H13B H 0.4663 0.5300 0.3554 0.099 Uiso 1 1 calc R . . H13C H 0.6703 0.5034 0.3668 0.099 Uiso 1 1 calc R . . O14 O 0.4301(18) 0.5018(6) 0.4219(4) 0.121(4) Uani 1 1 d . . . H14A H 0.3152 0.4867 0.4256 0.145 Uiso 1 1 d R . . H14B H 0.4994 0.5087 0.4531 0.145 Uiso 1 1 d R . . N1 N 0.8609(16) 0.7437(4) 0.2988(4) 0.071(3) Uani 1 1 d . . . C32 C 0.813(5) 0.6677(12) 0.1226(12) 0.180(10) Uani 1 1 d U . . H32A H 0.8972 0.6766 0.0921 0.271 Uiso 1 1 calc R . . H32B H 0.8148 0.6998 0.1500 0.271 Uiso 1 1 calc R . . H32C H 0.6900 0.6634 0.1075 0.271 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0262(3) 0.0549(3) 0.0335(2) -0.0050(2) -0.0009(2) -0.0023(3) Ba1 0.0254(2) 0.0485(2) 0.0410(2) -0.00953(19) 0.00392(18) -0.00475(19) C1 0.048(5) 0.046(4) 0.043(5) -0.002(3) -0.011(4) -0.011(4) C2 0.045(5) 0.046(4) 0.045(4) 0.002(3) -0.004(4) -0.008(4) C3 0.065(7) 0.070(7) 0.068(6) 0.028(5) -0.013(6) -0.025(6) C4 0.073(8) 0.090(8) 0.076(7) 0.047(6) -0.006(6) -0.019(7) C5 0.064(7) 0.051(5) 0.035(4) -0.007(3) -0.022(4) -0.004(4) C6 0.039(5) 0.059(5) 0.078(7) 0.006(5) -0.005(5) 0.003(5) C7 0.038(5) 0.054(5) 0.049(4) 0.012(3) -0.007(4) -0.012(4) C8 0.058(6) 0.057(5) 0.040(4) -0.004(4) -0.019(4) -0.006(5) C9 0.064(7) 0.058(5) 0.047(5) -0.007(4) -0.015(4) 0.016(5) C13 0.053(6) 0.071(6) 0.055(5) -0.012(4) -0.025(4) 0.016(5) C10 0.052(6) 0.060(5) 0.062(5) -0.005(4) -0.005(5) 0.014(5) C11 0.048(5) 0.058(5) 0.039(4) 0.000(4) 0.003(4) 0.009(4) C12 0.059(6) 0.060(6) 0.066(6) -0.016(4) -0.031(5) 0.031(5) C14 0.045(5) 0.046(4) 0.046(4) 0.004(3) -0.009(4) 0.001(4) C15 0.025(4) 0.069(5) 0.037(4) -0.016(3) 0.001(4) 0.012(4) C16 0.026(4) 0.063(5) 0.036(4) -0.011(3) 0.001(3) -0.009(4) C17 0.038(5) 0.111(8) 0.044(5) -0.033(5) 0.013(4) -0.031(5) C18 0.061(7) 0.077(7) 0.055(5) -0.027(5) 0.029(5) -0.031(5) C19 0.053(6) 0.046(4) 0.031(4) -0.006(3) 0.003(4) -0.003(4) C20 0.054(6) 0.058(5) 0.047(4) -0.014(4) 0.014(4) -0.023(4) C21 0.050(5) 0.052(4) 0.044(4) -0.012(3) 0.022(4) -0.015(4) C22 0.051(5) 0.036(4) 0.032(4) -0.006(3) 0.010(3) -0.007(4) C23 0.056(6) 0.032(4) 0.055(5) 0.004(3) 0.010(4) 0.008(4) C24 0.039(5) 0.042(4) 0.043(4) 0.009(3) 0.012(3) 0.013(3) C25 0.026(4) 0.048(4) 0.026(3) -0.006(3) 0.003(3) -0.003(3) C26 0.033(4) 0.057(5) 0.048(5) 0.018(4) 0.002(4) -0.003(4) C27 0.030(5) 0.066(6) 0.051(5) 0.008(4) 0.007(4) -0.003(4) C28 0.055(6) 0.040(4) 0.034(4) -0.002(3) -0.001(4) -0.004(4) C29 0.072(8) 0.051(5) 0.088(8) -0.007(5) 0.012(7) -0.005(5) C30 0.26(3) 0.097(11) 0.170(17) -0.071(12) 0.13(2) -0.027(16) C31 0.111(12) 0.049(6) 0.118(11) 0.007(6) -0.015(10) -0.018(7) O1 0.041(3) 0.053(3) 0.042(3) 0.004(3) -0.012(3) -0.005(3) O2 0.049(5) 0.092(5) 0.070(5) 0.022(4) -0.016(4) -0.020(4) O3 0.100(7) 0.048(3) 0.055(4) -0.009(3) -0.035(4) 0.011(4) O4 0.054(5) 0.084(5) 0.051(4) -0.012(3) -0.015(3) 0.000(4) O5 0.055(4) 0.069(4) 0.041(3) -0.011(3) -0.009(3) 0.008(3) O6 0.034(3) 0.088(5) 0.042(3) -0.026(3) -0.005(2) -0.009(3) O7 0.041(4) 0.081(4) 0.047(3) -0.024(3) 0.010(3) 0.004(3) O8 0.062(4) 0.047(3) 0.039(3) -0.006(2) 0.020(3) -0.019(3) O9 0.041(3) 0.066(4) 0.036(3) 0.019(3) -0.002(2) 0.000(3) O10 0.026(3) 0.067(4) 0.041(3) 0.009(3) 0.005(2) 0.004(3) O11 0.084(6) 0.059(4) 0.115(7) 0.027(4) 0.041(5) 0.013(4) O12 0.085(6) 0.066(5) 0.126(7) -0.042(5) 0.012(7) -0.020(5) O13 0.086(6) 0.102(6) 0.060(5) -0.009(4) 0.009(4) 0.021(5) O14 0.119(9) 0.175(11) 0.069(6) 0.015(6) 0.007(6) 0.066(9) N1 0.082(7) 0.052(5) 0.078(6) 0.000(4) 0.002(5) -0.019(5) C32 0.187(13) 0.179(12) 0.175(12) 0.008(9) 0.004(9) -0.002(9) _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 Cd1 O6 2.282(6) . ? Cd1 O1 2.285(6) . ? Cd1 O10 2.297(6) 2_464 ? Cd1 O5 2.439(7) 2_664 ? Cd1 O9 2.440(6) 2_464 ? Cd1 O4 2.480(7) 2_664 ? Cd1 C28 2.698(9) 2_464 ? Cd1 Ba1 3.8125(8) . ? Cd1 Ba1 4.1119(8) 1_455 ? Ba1 O7 2.697(7) . ? Ba1 O1 2.730(6) . ? Ba1 O12 2.741(7) . ? Ba1 O9 2.763(6) 2_564 ? Ba1 O6 2.790(6) 1_655 ? Ba1 O11 2.805(8) . ? Ba1 O5 2.815(7) 2_664 ? Ba1 O13 2.832(8) . ? Ba1 Cd1 4.1119(8) 1_655 ? C1 O2 1.224(12) . ? C1 O1 1.296(11) . ? C1 C2 1.482(13) . ? C2 C7 1.379(14) . ? C2 C3 1.395(13) . ? C3 C4 1.349(17) . ? C3 H3A 0.9300 . ? C4 C5 1.370(16) . ? C4 H4A 0.9300 . ? C5 C6 1.365(14) . ? C5 O3 1.387(11) . ? C6 C7 1.389(14) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 O3 1.374(11) . ? C8 C13 1.382(15) . ? C8 C9 1.396(14) . ? C9 C10 1.343(14) . ? C9 H9A 0.9300 . ? C13 C12 1.375(14) . ? C13 H13A 0.9300 . ? C10 C11 1.379(13) . ? C10 H10A 0.9300 . ? C11 C12 1.391(14) . ? C11 C14 1.508(13) . ? C12 H12A 0.9300 . ? C14 O5 1.255(11) . ? C14 O4 1.266(13) . ? C15 O7 1.235(11) . ? C15 O6 1.265(11) . ? C15 C16 1.486(10) . ? C16 C21 1.359(12) . ? C16 C17 1.401(12) . ? C17 C18 1.364(12) . ? C17 H17A 0.9300 . ? C18 C19 1.360(13) . ? C18 H18A 0.9300 . ? C19 C20 1.337(13) . ? C19 O8 1.394(10) . ? C20 C21 1.390(11) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.368(13) . ? C22 C23 1.375(14) . ? C22 O8 1.407(10) . ? C23 C24 1.401(12) . ? C23 H23A 0.9300 . ? C24 C25 1.377(11) . ? C24 H24A 0.9300 . ? C25 C26 1.382(12) . ? C25 C28 1.517(12) . ? C26 C27 1.414(12) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 O9 1.253(10) . ? C28 O10 1.259(12) . ? C28 Cd1 2.698(9) 2_465 ? C29 O12 1.253(15) . ? C29 N1 1.332(14) . ? C29 H29A 0.9300 . ? C30 N1 1.58(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N1 1.445(18) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O4 Cd1 2.480(7) 2_665 ? O5 Cd1 2.439(7) 2_665 ? O5 Ba1 2.815(7) 2_665 ? O6 Ba1 2.790(6) 1_455 ? O9 Cd1 2.440(6) 2_465 ? O9 Ba1 2.763(6) 2_565 ? O10 Cd1 2.297(6) 2_465 ? O11 C32 1.27(3) . ? O13 H13B 0.9300 . ? O13 H13C 0.9300 . ? O14 H14A 0.8999 . ? O14 H14B 0.9002 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 O6 Cd1 O1 107.1(2) . . ? O6 Cd1 O10 133.4(2) . 2_464 ? O1 Cd1 O10 103.9(2) . 2_464 ? O6 Cd1 O5 120.2(3) . 2_664 ? O1 Cd1 O5 78.2(2) . 2_664 ? O10 Cd1 O5 99.4(2) 2_464 2_664 ? O6 Cd1 O9 78.9(2) . 2_464 ? O1 Cd1 O9 140.8(2) . 2_464 ? O10 Cd1 O9 55.4(2) 2_464 2_464 ? O5 Cd1 O9 133.3(2) 2_664 2_464 ? O6 Cd1 O4 94.8(3) . 2_664 ? O1 Cd1 O4 131.2(2) . 2_664 ? O10 Cd1 O4 90.0(2) 2_464 2_664 ? O5 Cd1 O4 53.3(2) 2_664 2_664 ? O9 Cd1 O4 85.3(2) 2_464 2_664 ? O6 Cd1 C28 106.2(3) . 2_464 ? O1 Cd1 C28 125.3(2) . 2_464 ? O10 Cd1 C28 27.7(2) 2_464 2_464 ? O5 Cd1 C28 118.4(2) 2_664 2_464 ? O9 Cd1 C28 27.6(2) 2_464 2_464 ? O4 Cd1 C28 87.0(3) 2_664 2_464 ? O6 Cd1 Ba1 94.00(16) . . ? O1 Cd1 Ba1 45.07(15) . . ? O10 Cd1 Ba1 132.22(15) 2_464 . ? O5 Cd1 Ba1 47.53(16) 2_664 . ? O9 Cd1 Ba1 171.86(14) 2_464 . ? O4 Cd1 Ba1 91.46(19) 2_664 . ? C28 Cd1 Ba1 159.8(2) 2_464 . ? O6 Cd1 Ba1 40.22(15) . 1_455 ? O1 Cd1 Ba1 141.69(16) . 1_455 ? O10 Cd1 Ba1 95.84(15) 2_464 1_455 ? O5 Cd1 Ba1 130.75(17) 2_664 1_455 ? O9 Cd1 Ba1 40.63(14) 2_464 1_455 ? O4 Cd1 Ba1 80.39(18) 2_664 1_455 ? C28 Cd1 Ba1 68.2(2) 2_464 1_455 ? Ba1 Cd1 Ba1 131.433(19) . 1_455 ? O7 Ba1 O1 71.3(2) . . ? O7 Ba1 O12 74.5(3) . . ? O1 Ba1 O12 141.9(3) . . ? O7 Ba1 O9 140.7(2) . 2_564 ? O1 Ba1 O9 75.51(19) . 2_564 ? O12 Ba1 O9 142.3(3) . 2_564 ? O7 Ba1 O6 152.17(18) . 1_655 ? O1 Ba1 O6 121.1(2) . 1_655 ? O12 Ba1 O6 84.1(3) . 1_655 ? O9 Ba1 O6 65.44(18) 2_564 1_655 ? O7 Ba1 O11 113.3(3) . . ? O1 Ba1 O11 137.5(3) . . ? O12 Ba1 O11 72.4(3) . . ? O9 Ba1 O11 78.6(2) 2_564 . ? O6 Ba1 O11 75.6(3) 1_655 . ? O7 Ba1 O5 66.97(19) . 2_664 ? O1 Ba1 O5 65.03(18) . 2_664 ? O12 Ba1 O5 115.5(3) . 2_664 ? O9 Ba1 O5 80.40(19) 2_564 2_664 ? O6 Ba1 O5 140.03(18) 1_655 2_664 ? O11 Ba1 O5 77.9(3) . 2_664 ? O7 Ba1 O13 69.3(3) . . ? O1 Ba1 O13 72.3(2) . . ? O12 Ba1 O13 80.2(3) . . ? O9 Ba1 O13 119.4(2) 2_564 . ? O6 Ba1 O13 90.0(2) 1_655 . ? O11 Ba1 O13 150.1(3) . . ? O5 Ba1 O13 126.1(3) 2_664 . ? O7 Ba1 Cd1 44.45(15) . . ? O1 Ba1 Cd1 36.34(12) . . ? O12 Ba1 Cd1 118.0(2) . . ? O9 Ba1 Cd1 96.36(13) 2_564 . ? O6 Ba1 Cd1 156.66(16) 1_655 . ? O11 Ba1 Cd1 116.7(2) . . ? O5 Ba1 Cd1 39.71(14) 2_664 . ? O13 Ba1 Cd1 86.6(2) . . ? O7 Ba1 Cd1 175.79(14) . 1_655 ? O1 Ba1 Cd1 105.51(14) . 1_655 ? O12 Ba1 Cd1 109.3(2) . 1_655 ? O9 Ba1 Cd1 35.10(13) 2_564 1_655 ? O6 Ba1 Cd1 31.88(12) 1_655 1_655 ? O11 Ba1 Cd1 67.01(19) . 1_655 ? O5 Ba1 Cd1 109.31(14) 2_664 1_655 ? O13 Ba1 Cd1 112.8(2) . 1_655 ? Cd1 Ba1 Cd1 131.433(19) . 1_655 ? O2 C1 O1 120.3(9) . . ? O2 C1 C2 122.5(9) . . ? O1 C1 C2 117.2(8) . . ? C7 C2 C3 116.6(9) . . ? C7 C2 C1 122.0(8) . . ? C3 C2 C1 121.2(10) . . ? C4 C3 C2 123.0(12) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 119.2(10) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 119.6(9) . . ? C6 C5 O3 120.2(10) . . ? C4 C5 O3 119.8(10) . . ? C5 C6 C7 120.4(10) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C2 C7 C6 120.5(9) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? O3 C8 C13 122.7(9) . . ? O3 C8 C9 117.7(9) . . ? C13 C8 C9 119.5(8) . . ? C10 C9 C8 120.0(10) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C8 C13 C12 119.3(9) . . ? C8 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C9 C10 C11 121.9(10) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C12 118.1(9) . . ? C10 C11 C14 122.8(9) . . ? C12 C11 C14 119.1(8) . . ? C13 C12 C11 121.0(9) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? O5 C14 O4 121.9(9) . . ? O5 C14 C11 118.6(8) . . ? O4 C14 C11 119.4(9) . . ? O7 C15 O6 121.1(7) . . ? O7 C15 C16 119.5(8) . . ? O6 C15 C16 119.3(7) . . ? C21 C16 C17 118.4(7) . . ? C21 C16 C15 122.7(8) . . ? C17 C16 C15 118.8(8) . . ? C18 C17 C16 120.7(9) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 119.8(9) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C20 C19 C18 120.1(8) . . ? C20 C19 O8 118.9(8) . . ? C18 C19 O8 120.9(8) . . ? C19 C20 C21 121.3(8) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C16 C21 C20 119.4(8) . . ? C16 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C27 C22 C23 124.0(8) . . ? C27 C22 O8 117.1(9) . . ? C23 C22 O8 118.8(8) . . ? C22 C23 C24 117.7(8) . . ? C22 C23 H23A 121.2 . . ? C24 C23 H23A 121.2 . . ? C25 C24 C23 120.1(8) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.8(8) . . ? C24 C25 C28 120.5(8) . . ? C26 C25 C28 118.6(7) . . ? C25 C26 C27 120.0(8) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C22 C27 C26 117.2(9) . . ? C22 C27 H27A 121.4 . . ? C26 C27 H27A 121.4 . . ? O9 C28 O10 122.7(8) . . ? O9 C28 C25 119.3(9) . . ? O10 C28 C25 118.0(7) . . ? O9 C28 Cd1 64.6(5) . 2_465 ? O10 C28 Cd1 58.1(4) . 2_465 ? C25 C28 Cd1 175.3(6) . 2_465 ? O12 C29 N1 123.8(12) . . ? O12 C29 H29A 118.1 . . ? N1 C29 H29A 118.1 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 O1 Cd1 102.4(6) . . ? C1 O1 Ba1 141.7(5) . . ? Cd1 O1 Ba1 98.6(2) . . ? C8 O3 C5 118.0(7) . . ? C14 O4 Cd1 91.2(6) . 2_665 ? C14 O5 Cd1 93.4(6) . 2_665 ? C14 O5 Ba1 138.2(6) . 2_665 ? Cd1 O5 Ba1 92.76(19) 2_665 2_665 ? C15 O6 Cd1 101.7(5) . . ? C15 O6 Ba1 139.4(6) . 1_455 ? Cd1 O6 Ba1 107.9(2) . 1_455 ? C15 O7 Ba1 149.9(7) . . ? C19 O8 C22 116.2(7) . . ? C28 O9 Cd1 87.7(6) . 2_465 ? C28 O9 Ba1 166.2(6) . 2_565 ? Cd1 O9 Ba1 104.3(2) 2_465 2_565 ? C28 O10 Cd1 94.2(5) . 2_465 ? C32 O11 Ba1 132.0(16) . . ? C29 O12 Ba1 125.5(8) . . ? Ba1 O13 H13B 120.0 . . ? Ba1 O13 H13C 120.0 . . ? H13B O13 H13C 120.0 . . ? H14A O14 H14B 120.0 . . ? C29 N1 C31 121.2(12) . . ? C29 N1 C30 116.2(11) . . ? C31 N1 C30 122.6(11) . . ? O11 C32 H32A 109.5 . . ? O11 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O11 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.495 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.142 #==END _database_code_depnum_ccdc_archive 'CCDC 960505'