# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_Cd5(BO3)3F _database_code_depnum_ccdc_archive 'CCDC 901334' #TrackingRef '901334.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B3 Cd5 F O9' _chemical_formula_sum 'B3 Cd5 F O9' _chemical_formula_weight 757.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M Cm _symmetry_space_group_name_Hall 'C -2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 8.057(3) _cell_length_b 15.966(6) _cell_length_c 3.4470(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.06(3) _cell_angle_gamma 90.00 _cell_volume 436.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 672 _cell_measurement_theta_min 4.6073 _cell_measurement_theta_max 27.5438 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 12.031 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5510 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number ? _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 1663 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 27.47 _reflns_number_total 853 _reflns_number_gt 822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0133P)^2^+20.7319P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _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 -0.07(17) _refine_ls_number_reflns 853 _refine_ls_number_parameters 75 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.23890(17) 0.0000 0.7823(3) 0.0057(3) Uani 1 2 d S . . Cd2 Cd 0.35343(15) 0.38054(6) 1.0834(3) 0.0110(2) Uani 1 1 d . . . Cd3 Cd -0.02387(14) 0.32415(7) 0.4105(2) 0.0144(3) Uani 1 1 d . . . O1 O 0.1687(17) 0.2706(8) 1.025(4) 0.029(3) Uiso 1 1 d . . . O2 O 0.6835(14) -0.0754(6) 0.520(3) 0.013(2) Uani 1 1 d . . . O3 O 0.2991(13) 0.1437(7) 0.844(3) 0.015(2) Uani 1 1 d . . . O4 O 0.4228(19) 0.0000 0.365(4) 0.012(3) Uiso 1 2 d S . . O5 O 0.0031(17) 0.1728(9) 0.640(4) 0.032(3) Uani 1 1 d . . . F1 F 0.0278(18) 0.0000 0.171(5) 0.029(3) Uani 1 2 d S . . B1 B 0.159(2) 0.1955(10) 0.833(5) 0.011(3) Uiso 1 1 d . . . B2 B 0.597(3) 0.0000 0.474(8) 0.017(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0048(7) 0.0095(7) 0.0033(6) 0.000 0.0019(5) 0.000 Cd2 0.0094(5) 0.0138(5) 0.0101(5) 0.0021(4) 0.0028(4) 0.0024(4) Cd3 0.0143(6) 0.0188(6) 0.0110(5) 0.0009(4) 0.0047(4) 0.0015(5) O2 0.020(6) 0.008(5) 0.012(5) 0.000(4) 0.002(4) 0.006(4) O3 0.010(6) 0.017(5) 0.016(5) 0.003(4) -0.002(4) 0.009(4) O5 0.018(6) 0.068(10) 0.011(6) -0.004(5) 0.007(5) -0.014(6) F1 0.018(8) 0.013(6) 0.057(10) 0.000 0.008(7) 0.000 B2 0.014(13) 0.019(12) 0.018(12) 0.000 0.002(11) 0.000 _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 O4 2.239(17) . ? Cd1 O4 2.278(14) 1_556 ? Cd1 F1 2.342(16) 1_556 ? Cd1 O3 2.348(11) . ? Cd1 O3 2.348(11) 2 ? Cd1 F1 2.466(15) . ? Cd1 Cd1 3.4470(16) 1_554 ? Cd1 Cd1 3.4470(16) 1_556 ? Cd1 Cd3 3.7463(17) 4 ? Cd1 Cd3 3.7463(17) 3_545 ? Cd1 Cd3 3.8444(17) 4_556 ? Cd1 Cd3 3.8444(17) 3_546 ? Cd2 O5 2.247(12) 4_556 ? Cd2 O5 2.272(14) 4 ? Cd2 O2 2.282(10) 3_455 ? Cd2 O1 2.287(13) . ? Cd2 O2 2.314(11) 3_456 ? Cd2 F1 2.357(9) 3_556 ? Cd2 B1 3.003(18) 4 ? Cd2 Cd2 3.4470(16) 1_554 ? Cd2 Cd3 3.538(2) 1_556 ? Cd2 Cd3 3.5412(19) 4_556 ? Cd2 Cd3 3.601(2) . ? Cd2 Cd2 3.814(2) 2_565 ? Cd3 O3 2.266(11) 4_454 ? Cd3 O3 2.297(12) 4_455 ? Cd3 O2 2.299(11) 3_455 ? Cd3 O1 2.372(14) 1_554 ? Cd3 O5 2.540(15) . ? Cd3 O1 2.544(12) . ? Cd3 B1 2.785(16) . ? Cd3 O4 2.841(3) 3_455 ? Cd3 B2 2.967(8) 3_455 ? Cd3 B1 2.971(16) 4_454 ? Cd3 Cd3 3.4470(16) 1_554 ? Cd3 Cd3 3.4470(16) 1_556 ? O1 B1 1.37(2) . ? O1 Cd3 2.372(14) 1_556 ? O2 B2 1.387(16) . ? O2 Cd2 2.282(10) 3_545 ? O2 Cd3 2.299(11) 3_545 ? O2 Cd2 2.314(11) 3_544 ? O3 B1 1.395(19) . ? O3 Cd3 2.266(10) 4_556 ? O3 Cd3 2.297(12) 4 ? O4 B2 1.39(3) . ? O4 Cd1 2.278(14) 1_554 ? O4 Cd3 2.841(3) 4 ? O4 Cd3 2.841(3) 3_545 ? O5 B1 1.362(19) . ? O5 Cd2 2.247(12) 4_454 ? O5 Cd2 2.272(14) 4_455 ? F1 Cd1 2.342(16) 1_554 ? F1 Cd2 2.357(8) 4_454 ? F1 Cd2 2.357(8) 3_444 ? B1 Cd3 2.971(16) 4_556 ? B1 Cd2 3.003(18) 4_455 ? B2 O2 1.387(16) 2 ? B2 Cd3 2.967(8) 4 ? B2 Cd3 2.967(8) 3_545 ? 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 Cd1 O4 99.5(6) . 1_556 ? O4 Cd1 F1 175.0(5) . 1_556 ? O4 Cd1 F1 85.5(6) 1_556 1_556 ? O4 Cd1 O3 84.8(3) . . ? O4 Cd1 O3 80.1(3) 1_556 . ? F1 Cd1 O3 96.2(3) 1_556 . ? O4 Cd1 O3 84.8(3) . 2 ? O4 Cd1 O3 80.1(3) 1_556 2 ? F1 Cd1 O3 96.2(3) 1_556 2 ? O3 Cd1 O3 155.7(5) . 2 ? O4 Cd1 F1 83.4(5) . . ? O4 Cd1 F1 177.1(6) 1_556 . ? F1 Cd1 F1 91.6(5) 1_556 . ? O3 Cd1 F1 100.3(3) . . ? O3 Cd1 F1 100.3(3) 2 . ? O4 Cd1 Cd1 40.7(4) . 1_554 ? O4 Cd1 Cd1 140.2(4) 1_556 1_554 ? F1 Cd1 Cd1 134.4(4) 1_556 1_554 ? O3 Cd1 Cd1 93.1(3) . 1_554 ? O3 Cd1 Cd1 93.1(3) 2 1_554 ? F1 Cd1 Cd1 42.8(4) . 1_554 ? O4 Cd1 Cd1 139.3(4) . 1_556 ? O4 Cd1 Cd1 39.8(4) 1_556 1_556 ? F1 Cd1 Cd1 45.6(4) 1_556 1_556 ? O3 Cd1 Cd1 86.9(3) . 1_556 ? O3 Cd1 Cd1 86.9(3) 2 1_556 ? F1 Cd1 Cd1 137.2(4) . 1_556 ? Cd1 Cd1 Cd1 180.00(4) 1_554 1_556 ? O4 Cd1 Cd3 49.12(6) . 4 ? O4 Cd1 Cd3 90.5(3) 1_556 4 ? F1 Cd1 Cd3 131.35(3) 1_556 4 ? O3 Cd1 Cd3 35.8(3) . 4 ? O3 Cd1 Cd3 130.8(3) 2 4 ? F1 Cd1 Cd3 91.4(3) . 4 ? Cd1 Cd1 Cd3 64.45(3) 1_554 4 ? Cd1 Cd1 Cd3 115.55(3) 1_556 4 ? O4 Cd1 Cd3 49.12(6) . 3_545 ? O4 Cd1 Cd3 90.5(3) 1_556 3_545 ? F1 Cd1 Cd3 131.35(4) 1_556 3_545 ? O3 Cd1 Cd3 130.8(3) . 3_545 ? O3 Cd1 Cd3 35.8(3) 2 3_545 ? F1 Cd1 Cd3 91.4(3) . 3_545 ? Cd1 Cd1 Cd3 64.45(3) 1_554 3_545 ? Cd1 Cd1 Cd3 115.55(3) 1_556 3_545 ? Cd3 Cd1 Cd3 97.09(5) 4 3_545 ? O4 Cd1 Cd3 92.4(2) . 4_556 ? O4 Cd1 Cd3 47.20(5) 1_556 4_556 ? F1 Cd1 Cd3 91.0(3) 1_556 4_556 ? O3 Cd1 Cd3 32.9(2) . 4_556 ? O3 Cd1 Cd3 126.0(2) 2 4_556 ? F1 Cd1 Cd3 133.01(3) . 4_556 ? Cd1 Cd1 Cd3 118.45(3) 1_554 4_556 ? Cd1 Cd1 Cd3 61.55(3) 1_556 4_556 ? Cd3 Cd1 Cd3 54.00(3) 4 4_556 ? Cd3 Cd1 Cd3 120.45(5) 3_545 4_556 ? O4 Cd1 Cd3 92.4(2) . 3_546 ? O4 Cd1 Cd3 47.20(5) 1_556 3_546 ? F1 Cd1 Cd3 91.0(3) 1_556 3_546 ? O3 Cd1 Cd3 126.0(2) . 3_546 ? O3 Cd1 Cd3 32.9(3) 2 3_546 ? F1 Cd1 Cd3 133.01(3) . 3_546 ? Cd1 Cd1 Cd3 118.45(3) 1_554 3_546 ? Cd1 Cd1 Cd3 61.55(3) 1_556 3_546 ? Cd3 Cd1 Cd3 120.45(5) 4 3_546 ? Cd3 Cd1 Cd3 54.00(3) 3_545 3_546 ? Cd3 Cd1 Cd3 93.83(5) 4_556 3_546 ? O5 Cd2 O5 99.4(5) 4_556 4 ? O5 Cd2 O2 174.5(5) 4_556 3_455 ? O5 Cd2 O2 81.6(4) 4 3_455 ? O5 Cd2 O1 91.6(5) 4_556 . ? O5 Cd2 O1 93.8(5) 4 . ? O2 Cd2 O1 82.9(4) 3_455 . ? O5 Cd2 O2 81.4(4) 4_556 3_456 ? O5 Cd2 O2 174.6(5) 4 3_456 ? O2 Cd2 O2 97.2(4) 3_455 3_456 ? O1 Cd2 O2 80.8(4) . 3_456 ? O5 Cd2 F1 88.8(5) 4_556 3_556 ? O5 Cd2 F1 90.9(5) 4 3_556 ? O2 Cd2 F1 96.6(4) 3_455 3_556 ? O1 Cd2 F1 175.2(5) . 3_556 ? O2 Cd2 F1 94.5(5) 3_456 3_556 ? O5 Cd2 B1 75.4(5) 4_556 4 ? O5 Cd2 B1 25.4(4) 4 4 ? O2 Cd2 B1 106.2(4) 3_455 4 ? O1 Cd2 B1 102.6(5) . 4 ? O2 Cd2 B1 156.6(4) 3_456 4 ? F1 Cd2 B1 82.2(4) 3_556 4 ? O5 Cd2 Cd2 139.4(4) 4_556 1_554 ? O5 Cd2 Cd2 40.0(3) 4 1_554 ? O2 Cd2 Cd2 41.8(3) 3_455 1_554 ? O1 Cd2 Cd2 91.5(3) . 1_554 ? O2 Cd2 Cd2 138.9(2) 3_456 1_554 ? F1 Cd2 Cd2 91.4(4) 3_556 1_554 ? B1 Cd2 Cd2 64.5(3) 4 1_554 ? O5 Cd2 Cd3 89.7(4) 4_556 1_556 ? O5 Cd2 Cd3 134.9(4) 4 1_556 ? O2 Cd2 Cd3 85.9(3) 3_455 1_556 ? O1 Cd2 Cd3 41.5(3) . 1_556 ? O2 Cd2 Cd3 39.8(3) 3_456 1_556 ? F1 Cd2 Cd3 133.7(4) 3_556 1_556 ? B1 Cd2 Cd3 141.4(3) 4 1_556 ? Cd2 Cd2 Cd3 117.95(3) 1_554 1_556 ? O5 Cd2 Cd3 45.6(4) 4_556 4_556 ? O5 Cd2 Cd3 73.5(3) 4 4_556 ? O2 Cd2 Cd3 130.4(3) 3_455 4_556 ? O1 Cd2 Cd3 57.4(3) . 4_556 ? O2 Cd2 Cd3 103.7(2) 3_456 4_556 ? F1 Cd2 Cd3 125.4(3) 3_556 4_556 ? B1 Cd2 Cd3 61.4(3) 4 4_556 ? Cd2 Cd2 Cd3 105.64(3) 1_554 4_556 ? Cd3 Cd2 Cd3 82.60(3) 1_556 4_556 ? O5 Cd2 Cd3 136.2(4) 4_556 . ? O5 Cd2 Cd3 87.7(3) 4 . ? O2 Cd2 Cd3 38.4(3) 3_455 . ? O1 Cd2 Cd3 44.6(3) . . ? O2 Cd2 Cd3 88.1(3) 3_456 . ? F1 Cd2 Cd3 134.6(3) 3_556 . ? B1 Cd2 Cd3 110.8(3) 4 . ? Cd2 Cd2 Cd3 60.22(4) 1_554 . ? Cd3 Cd2 Cd3 57.73(4) 1_556 . ? Cd3 Cd2 Cd3 97.56(3) 4_556 . ? O5 Cd2 Cd2 112.3(4) 4_556 2_565 ? O5 Cd2 Cd2 112.0(4) 4 2_565 ? O2 Cd2 Cd2 72.1(2) 3_455 2_565 ? O1 Cd2 Cd2 140.1(3) . 2_565 ? O2 Cd2 Cd2 72.3(3) 3_456 2_565 ? F1 Cd2 Cd2 36.0(3) 3_556 2_565 ? B1 Cd2 Cd2 113.8(3) 4 2_565 ? Cd2 Cd2 Cd2 90.0 1_554 2_565 ? Cd3 Cd2 Cd2 104.74(2) 1_556 2_565 ? Cd3 Cd2 Cd2 157.35(3) 4_556 2_565 ? Cd3 Cd2 Cd2 104.48(2) . 2_565 ? O3 Cd3 O3 98.1(4) 4_454 4_455 ? O3 Cd3 O2 108.3(4) 4_454 3_455 ? O3 Cd3 O2 104.7(4) 4_455 3_455 ? O3 Cd3 O1 88.5(4) 4_454 1_554 ? O3 Cd3 O1 170.6(4) 4_455 1_554 ? O2 Cd3 O1 79.4(4) 3_455 1_554 ? O3 Cd3 O5 119.3(4) 4_454 . ? O3 Cd3 O5 92.2(4) 4_455 . ? O2 Cd3 O5 126.3(4) 3_455 . ? O1 Cd3 O5 78.6(4) 1_554 . ? O3 Cd3 O1 173.5(4) 4_454 . ? O3 Cd3 O1 83.7(4) 4_455 . ? O2 Cd3 O1 77.1(4) 3_455 . ? O1 Cd3 O1 89.0(4) 1_554 . ? O5 Cd3 O1 54.2(4) . . ? O3 Cd3 B1 144.3(4) 4_454 . ? O3 Cd3 B1 99.0(5) 4_455 . ? O2 Cd3 B1 97.2(4) 3_455 . ? O1 Cd3 B1 71.9(5) 1_554 . ? O5 Cd3 B1 29.2(4) . . ? O1 Cd3 B1 29.3(4) . . ? O3 Cd3 O4 70.3(4) 4_454 3_455 ? O3 Cd3 O4 73.2(4) 4_455 3_455 ? O2 Cd3 O4 54.4(4) 3_455 3_455 ? O1 Cd3 O4 115.6(5) 1_554 3_455 ? O5 Cd3 O4 164.1(4) . 3_455 ? O1 Cd3 O4 116.3(4) . 3_455 ? B1 Cd3 O4 145.0(4) . 3_455 ? O3 Cd3 B2 89.9(5) 4_454 3_455 ? O3 Cd3 B2 88.5(6) 4_455 3_455 ? O2 Cd3 B2 26.9(5) 3_455 3_455 ? O1 Cd3 B2 98.3(6) 1_554 3_455 ? O5 Cd3 B2 150.2(5) . 3_455 ? O1 Cd3 B2 96.4(5) . 3_455 ? B1 Cd3 B2 121.5(5) . 3_455 ? O4 Cd3 B2 27.5(6) 3_455 3_455 ? O3 Cd3 B1 26.8(4) 4_454 4_454 ? O3 Cd3 B1 84.3(4) 4_455 4_454 ? O2 Cd3 B1 134.4(4) 3_455 4_454 ? O1 Cd3 B1 99.0(5) 1_554 4_454 ? O5 Cd3 B1 97.2(4) . 4_454 ? O1 Cd3 B1 148.3(4) . 4_454 ? B1 Cd3 B1 125.9(2) . 4_454 ? O4 Cd3 B1 87.9(4) 3_455 4_454 ? B2 Cd3 B1 112.5(5) 3_455 4_454 ? O3 Cd3 Cd3 41.3(3) 4_454 1_554 ? O3 Cd3 Cd3 139.4(3) 4_455 1_554 ? O2 Cd3 Cd3 92.2(3) 3_455 1_554 ? O1 Cd3 Cd3 47.6(3) 1_554 1_554 ? O5 Cd3 Cd3 107.2(3) . 1_554 ? O1 Cd3 Cd3 136.5(3) . 1_554 ? B1 Cd3 Cd3 115.5(4) . 1_554 ? O4 Cd3 Cd3 88.3(3) 3_455 1_554 ? B2 Cd3 Cd3 90.9(5) 3_455 1_554 ? B1 Cd3 Cd3 58.6(3) 4_454 1_554 ? O3 Cd3 Cd3 138.7(3) 4_454 1_556 ? O3 Cd3 Cd3 40.6(3) 4_455 1_556 ? O2 Cd3 Cd3 87.8(3) 3_455 1_556 ? O1 Cd3 Cd3 132.4(3) 1_554 1_556 ? O5 Cd3 Cd3 72.8(3) . 1_556 ? O1 Cd3 Cd3 43.5(3) . 1_556 ? B1 Cd3 Cd3 64.5(4) . 1_556 ? O4 Cd3 Cd3 91.7(3) 3_455 1_556 ? B2 Cd3 Cd3 89.1(5) 3_455 1_556 ? B1 Cd3 Cd3 121.4(3) 4_454 1_556 ? Cd3 Cd3 Cd3 180.0 1_554 1_556 ? B1 O1 Cd2 134.3(12) . . ? B1 O1 Cd3 126.8(11) . 1_556 ? Cd2 O1 Cd3 98.8(5) . 1_556 ? B1 O1 Cd3 85.2(9) . . ? Cd2 O1 Cd3 96.2(5) . . ? Cd3 O1 Cd3 89.0(4) 1_556 . ? B2 O2 Cd2 125.5(12) . 3_545 ? B2 O2 Cd3 104.5(11) . 3_545 ? Cd2 O2 Cd3 103.6(4) 3_545 3_545 ? B2 O2 Cd2 122.1(13) . 3_544 ? Cd2 O2 Cd2 97.2(4) 3_545 3_544 ? Cd3 O2 Cd2 100.2(4) 3_545 3_544 ? B1 O3 Cd3 106.0(9) . 4_556 ? B1 O3 Cd3 116.2(9) . 4 ? Cd3 O3 Cd3 98.1(4) 4_556 4 ? B1 O3 Cd1 115.0(9) . . ? Cd3 O3 Cd1 112.9(4) 4_556 . ? Cd3 O3 Cd1 107.5(4) 4 . ? B2 O4 Cd1 125.3(13) . . ? B2 O4 Cd1 135.2(15) . 1_554 ? Cd1 O4 Cd1 99.5(6) . 1_554 ? B2 O4 Cd3 81.3(3) . 4 ? Cd1 O4 Cd3 94.3(3) . 4 ? Cd1 O4 Cd3 96.8(3) 1_554 4 ? B2 O4 Cd3 81.3(3) . 3_545 ? Cd1 O4 Cd3 94.3(3) . 3_545 ? Cd1 O4 Cd3 96.8(3) 1_554 3_545 ? Cd3 O4 Cd3 162.5(6) 4 3_545 ? B1 O5 Cd2 145.9(12) . 4_454 ? B1 O5 Cd2 108.9(10) . 4_455 ? Cd2 O5 Cd2 99.4(5) 4_454 4_455 ? B1 O5 Cd3 85.4(9) . . ? Cd2 O5 Cd3 95.2(5) 4_454 . ? Cd2 O5 Cd3 122.7(6) 4_455 . ? Cd1 F1 Cd2 113.8(5) 1_554 4_454 ? Cd1 F1 Cd2 113.8(5) 1_554 3_444 ? Cd2 F1 Cd2 108.0(6) 4_454 3_444 ? Cd1 F1 Cd1 91.6(5) 1_554 . ? Cd2 F1 Cd1 114.6(5) 4_454 . ? Cd2 F1 Cd1 114.6(5) 3_444 . ? O5 B1 O1 116.2(15) . . ? O5 B1 O3 122.0(14) . . ? O1 B1 O3 121.8(14) . . ? O5 B1 Cd3 65.4(9) . . ? O1 B1 Cd3 65.6(8) . . ? O3 B1 Cd3 143.5(11) . . ? O5 B1 Cd3 155.6(11) . 4_556 ? O1 B1 Cd3 78.3(9) . 4_556 ? O3 B1 Cd3 47.2(7) . 4_556 ? Cd3 B1 Cd3 137.9(6) . 4_556 ? O5 B1 Cd2 45.7(8) . 4_455 ? O1 B1 Cd2 101.3(11) . 4_455 ? O3 B1 Cd2 116.9(10) . 4_455 ? Cd3 B1 Cd2 93.7(5) . 4_455 ? Cd3 B1 Cd2 114.6(5) 4_556 4_455 ? O4 B2 O2 119.7(10) . 2 ? O4 B2 O2 119.7(10) . . ? O2 B2 O2 121(2) 2 . ? O4 B2 Cd3 71.1(5) . 4 ? O2 B2 Cd3 48.6(6) 2 4 ? O2 B2 Cd3 169.1(15) . 4 ? O4 B2 Cd3 71.1(5) . 3_545 ? O2 B2 Cd3 169.1(15) 2 3_545 ? O2 B2 Cd3 48.6(6) . 3_545 ? Cd3 B2 Cd3 142.2(9) 4 3_545 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.457 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.303 #===END