# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_Compound-1_Zn4Br8(18c6)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Br8 O12 Zn4' _chemical_formula_weight 1429.38 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.559(2) _cell_length_b 14.678(3) _cell_length_c 15.214(3) _cell_angle_alpha 112.82(3) _cell_angle_beta 91.85(3) _cell_angle_gamma 101.76(3) _cell_volume 2111.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 9.863 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0929 _exptl_absorpt_correction_T_max 0.2840 _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15942 _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8087 _reflns_number_gt 6224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'CELL, SELECT (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND, Crystal Impact' _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^)+(0.0542P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00062(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8087 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.21748(6) 0.24214(5) -0.40469(6) 0.0516(2) Uani 1 1 d . . . Br2 Br -0.34233(5) 0.49804(5) -0.29367(5) 0.03856(16) Uani 1 1 d . . . Br3 Br -0.05412(6) 0.45992(5) -0.15314(5) 0.04396(17) Uani 1 1 d . . . Br4 Br 0.00959(5) 0.51271(5) -0.36937(5) 0.03800(16) Uani 1 1 d . . . Br5 Br 0.14165(5) 0.73736(5) -0.11292(5) 0.04250(17) Uani 1 1 d . . . Br6 Br 0.30820(7) 0.50197(7) -0.21937(7) 0.0753(3) Uani 1 1 d . . . Br7 Br 0.76345(5) 0.96371(5) 0.11379(4) 0.03505(15) Uani 1 1 d . . . Br8 Br 0.65756(7) 0.94528(5) 0.59167(5) 0.04522(18) Uani 1 1 d . . . Zn1 Zn -0.16858(6) 0.41780(5) -0.31498(5) 0.03552(18) Uani 1 1 d . . . Zn2 Zn 0.12014(6) 0.56246(6) -0.20511(6) 0.03837(18) Uani 1 1 d . . . Zn3 Zn 0.70616(6) 0.83176(5) 0.16913(5) 0.03197(16) Uani 1 1 d . . . Zn4 Zn 0.68888(6) 0.84715(5) 0.67654(5) 0.03158(16) Uani 1 1 d . . . O1 O 0.4768(4) 0.7710(3) 0.0892(3) 0.0425(11) Uani 1 1 d . . . O2 O 0.6898(4) 0.7142(3) 0.0174(3) 0.0400(10) Uani 1 1 d . . . O3 O 0.8750(4) 0.7592(4) 0.1526(3) 0.0395(10) Uani 1 1 d . . . O4 O 0.8480(4) 0.9116(4) 0.3023(3) 0.0419(10) Uani 1 1 d . . . O5 O 0.6022(4) 0.9217(3) 0.2882(3) 0.0366(10) Uani 1 1 d . . . O6 O 0.6065(4) 0.7237(3) 0.2160(3) 0.0387(10) Uani 1 1 d . . . O7 O 0.7975(4) 0.9914(3) 0.8115(3) 0.0379(10) Uani 1 1 d . . . O8 O 0.5480(4) 0.9030(3) 0.7826(3) 0.0390(10) Uani 1 1 d . . . O9 O 0.5049(4) 0.7246(3) 0.6424(3) 0.0399(10) Uani 1 1 d . . . O10 O 0.6946(4) 0.7108(3) 0.5365(3) 0.0408(10) Uani 1 1 d . . . O11 O 0.9153(4) 0.8419(3) 0.6386(3) 0.0421(10) Uani 1 1 d . . . O12 O 0.7702(3) 0.7909(3) 0.7640(3) 0.0350(9) Uani 1 1 d . . . C1 C 0.4861(6) 0.7460(5) -0.0107(5) 0.0403(14) Uani 1 1 d . . . H1A H 0.5212 0.8090 -0.0202 0.048 Uiso 1 1 calc R . . H1B H 0.3980 0.7148 -0.0472 0.048 Uiso 1 1 calc R . . C2 C 0.5731(6) 0.6733(5) -0.0492(5) 0.0444(15) Uani 1 1 d . . . H2A H 0.5301 0.6048 -0.0538 0.053 Uiso 1 1 calc R . . H2B H 0.5932 0.6680 -0.1139 0.053 Uiso 1 1 calc R . . C3 C 0.7807(7) 0.6522(6) -0.0051(6) 0.059(2) Uani 1 1 d . . . H3A H 0.7946 0.6314 -0.0735 0.071 Uiso 1 1 calc R . . H3B H 0.7486 0.5903 0.0068 0.071 Uiso 1 1 calc R . . C4 C 0.9028(7) 0.7135(7) 0.0573(5) 0.056(2) Uani 1 1 d . . . H4A H 0.9640 0.6697 0.0541 0.068 Uiso 1 1 calc R . . H4B H 0.9443 0.7666 0.0355 0.068 Uiso 1 1 calc R . . C5 C 0.9879(6) 0.8154(6) 0.2188(5) 0.0502(17) Uani 1 1 d . . . H5A H 1.0386 0.8670 0.1985 0.060 Uiso 1 1 calc R . . H5B H 1.0436 0.7695 0.2210 0.060 Uiso 1 1 calc R . . C6 C 0.9490(6) 0.8656(7) 0.3140(6) 0.0548(19) Uani 1 1 d . . . H6A H 0.9177 0.8153 0.3416 0.066 Uiso 1 1 calc R . . H6B H 1.0239 0.9177 0.3580 0.066 Uiso 1 1 calc R . . C7 C 0.8091(6) 0.9779(5) 0.3874(5) 0.0478(17) Uani 1 1 d . . . H7A H 0.8810 1.0384 0.4222 0.057 Uiso 1 1 calc R . . H7B H 0.7847 0.9427 0.4304 0.057 Uiso 1 1 calc R . . C8 C 0.6950(7) 1.0083(5) 0.3566(5) 0.0448(16) Uani 1 1 d . . . H8A H 0.6525 1.0423 0.4135 0.054 Uiso 1 1 calc R . . H8B H 0.7251 1.0575 0.3276 0.054 Uiso 1 1 calc R . . C9 C 0.5242(6) 0.8594(5) 0.3285(5) 0.0442(16) Uani 1 1 d . . . H9A H 0.4326 0.8391 0.2985 0.053 Uiso 1 1 calc R . . H9B H 0.5262 0.8986 0.3983 0.053 Uiso 1 1 calc R . . C10 C 0.5745(6) 0.7659(5) 0.3119(5) 0.0440(16) Uani 1 1 d . . . H10A H 0.6529 0.7839 0.3581 0.053 Uiso 1 1 calc R . . H10B H 0.5073 0.7148 0.3227 0.053 Uiso 1 1 calc R . . C11 C 0.5052(7) 0.6447(5) 0.1472(6) 0.0509(18) Uani 1 1 d . . . H11A H 0.4588 0.6012 0.1776 0.061 Uiso 1 1 calc R . . H11B H 0.5445 0.6016 0.0928 0.061 Uiso 1 1 calc R . . C12 C 0.4092(6) 0.6887(6) 0.1099(6) 0.0523(18) Uani 1 1 d . . . H12A H 0.3557 0.6354 0.0509 0.063 Uiso 1 1 calc R . . H12B H 0.3502 0.7130 0.1586 0.063 Uiso 1 1 calc R . . C13 C 0.7070(6) 1.0534(5) 0.8512(5) 0.0446(16) Uani 1 1 d . . . H13A H 0.6837 1.0832 0.8064 0.053 Uiso 1 1 calc R . . H13B H 0.7485 1.1098 0.9128 0.053 Uiso 1 1 calc R . . C14 C 0.5858(6) 0.9916(5) 0.8677(5) 0.0458(16) Uani 1 1 d . . . H14A H 0.6037 0.9743 0.9229 0.055 Uiso 1 1 calc R . . H14B H 0.5164 1.0297 0.8810 0.055 Uiso 1 1 calc R . . C15 C 0.4387(6) 0.8296(5) 0.7850(5) 0.0469(17) Uani 1 1 d . . . H15A H 0.3687 0.8628 0.8140 0.056 Uiso 1 1 calc R . . H15B H 0.4639 0.7934 0.8232 0.056 Uiso 1 1 calc R . . C16 C 0.3932(5) 0.7570(5) 0.6827(5) 0.0487(18) Uani 1 1 d . . . H16A H 0.3254 0.6980 0.6798 0.058 Uiso 1 1 calc R . . H16B H 0.3561 0.7910 0.6467 0.058 Uiso 1 1 calc R . . C17 C 0.4730(6) 0.6578(5) 0.5427(5) 0.0465(16) Uani 1 1 d . . . H17A H 0.4478 0.6943 0.5047 0.056 Uiso 1 1 calc R . . H17B H 0.4000 0.5994 0.5336 0.056 Uiso 1 1 calc R . . C18 C 0.5937(6) 0.6227(5) 0.5129(5) 0.0468(16) Uani 1 1 d . . . H18A H 0.6144 0.5815 0.5472 0.056 Uiso 1 1 calc R . . H18B H 0.5821 0.5807 0.4429 0.056 Uiso 1 1 calc R . . C19 C 0.8122(6) 0.6924(5) 0.4992(5) 0.0495(18) Uani 1 1 d . . . H19A H 0.7987 0.6633 0.4281 0.059 Uiso 1 1 calc R . . H19B H 0.8430 0.6437 0.5201 0.059 Uiso 1 1 calc R . . C20 C 0.9088(7) 0.7909(6) 0.5364(5) 0.0515(18) Uani 1 1 d . . . H20A H 0.9956 0.7794 0.5194 0.062 Uiso 1 1 calc R . . H20B H 0.8848 0.8344 0.5058 0.062 Uiso 1 1 calc R . . C21 C 0.9702(5) 0.7949(5) 0.6911(5) 0.0418(15) Uani 1 1 d . . . H21A H 1.0285 0.8477 0.7481 0.050 Uiso 1 1 calc R . . H21B H 1.0230 0.7503 0.6504 0.050 Uiso 1 1 calc R . . C22 C 0.8666(5) 0.7340(5) 0.7225(5) 0.0404(15) Uani 1 1 d . . . H22A H 0.8234 0.6708 0.6668 0.048 Uiso 1 1 calc R . . H22B H 0.9059 0.7147 0.7707 0.048 Uiso 1 1 calc R . . C23 C 0.8003(6) 0.8565(5) 0.8636(5) 0.0453(16) Uani 1 1 d . . . H23A H 0.8600 0.8310 0.8949 0.054 Uiso 1 1 calc R . . H23B H 0.7192 0.8560 0.8945 0.054 Uiso 1 1 calc R . . C24 C 0.8629(6) 0.9632(5) 0.8775(5) 0.0444(15) Uani 1 1 d . . . H24A H 0.8589 1.0104 0.9442 0.053 Uiso 1 1 calc R . . H24B H 0.9557 0.9685 0.8672 0.053 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 Br1 0.0443(3) 0.0347(4) 0.0611(5) 0.0046(3) 0.0092(3) 0.0069(2) Br2 0.0312(3) 0.0414(4) 0.0419(4) 0.0141(3) 0.0072(3) 0.0111(2) Br3 0.0521(3) 0.0450(4) 0.0367(4) 0.0193(3) 0.0022(3) 0.0102(3) Br4 0.0358(3) 0.0452(4) 0.0328(4) 0.0152(3) 0.0084(3) 0.0094(2) Br5 0.0378(3) 0.0373(3) 0.0439(4) 0.0073(3) 0.0019(3) 0.0094(2) Br6 0.0434(3) 0.0709(6) 0.0788(7) -0.0124(5) -0.0149(4) 0.0326(3) Br7 0.0342(3) 0.0393(3) 0.0327(4) 0.0174(3) 0.0054(3) 0.0047(2) Br8 0.0625(4) 0.0504(4) 0.0374(4) 0.0252(3) 0.0165(3) 0.0278(3) Zn1 0.0309(3) 0.0352(4) 0.0368(4) 0.0104(3) 0.0053(3) 0.0077(3) Zn2 0.0304(3) 0.0388(4) 0.0398(5) 0.0081(4) 0.0004(3) 0.0111(3) Zn3 0.0333(3) 0.0334(4) 0.0297(4) 0.0128(3) 0.0078(3) 0.0081(2) Zn4 0.0341(3) 0.0333(4) 0.0286(4) 0.0131(3) 0.0037(3) 0.0094(3) O1 0.041(2) 0.046(3) 0.036(3) 0.012(2) 0.007(2) 0.0107(19) O2 0.0337(18) 0.042(3) 0.037(3) 0.006(2) -0.003(2) 0.0136(17) O3 0.0329(18) 0.055(3) 0.038(3) 0.021(2) 0.008(2) 0.0203(18) O4 0.041(2) 0.050(3) 0.030(3) 0.010(2) 0.004(2) 0.0122(19) O5 0.043(2) 0.036(2) 0.029(2) 0.009(2) 0.009(2) 0.0099(17) O6 0.043(2) 0.036(2) 0.043(3) 0.021(2) 0.015(2) 0.0124(17) O7 0.0377(19) 0.037(2) 0.032(3) 0.007(2) 0.007(2) 0.0071(17) O8 0.0331(18) 0.041(3) 0.036(3) 0.011(2) 0.009(2) 0.0044(17) O9 0.0369(19) 0.036(2) 0.045(3) 0.015(2) 0.003(2) 0.0091(17) O10 0.0364(19) 0.032(2) 0.041(3) 0.000(2) 0.000(2) 0.0101(16) O11 0.046(2) 0.038(3) 0.042(3) 0.013(2) 0.010(2) 0.0125(18) O12 0.0298(17) 0.040(2) 0.035(3) 0.014(2) -0.0019(18) 0.0113(16) C1 0.038(3) 0.043(4) 0.033(4) 0.010(3) -0.007(3) 0.009(3) C2 0.051(3) 0.040(4) 0.026(4) -0.002(3) -0.008(3) 0.009(3) C3 0.072(4) 0.058(5) 0.044(5) 0.004(4) 0.007(4) 0.043(4) C4 0.052(4) 0.082(6) 0.039(4) 0.016(4) 0.011(4) 0.041(4) C5 0.040(3) 0.061(5) 0.048(5) 0.019(4) -0.001(3) 0.018(3) C6 0.041(3) 0.079(6) 0.048(5) 0.028(4) -0.001(3) 0.019(3) C7 0.049(3) 0.047(4) 0.028(4) 0.001(3) 0.009(3) -0.002(3) C8 0.063(4) 0.037(4) 0.032(4) 0.009(3) 0.018(3) 0.013(3) C9 0.039(3) 0.051(4) 0.034(4) 0.010(3) 0.013(3) 0.005(3) C10 0.046(3) 0.054(4) 0.038(4) 0.023(4) 0.009(3) 0.011(3) C11 0.065(4) 0.036(4) 0.047(5) 0.016(4) 0.009(4) 0.005(3) C12 0.048(3) 0.047(4) 0.042(5) 0.008(4) 0.000(3) -0.010(3) C13 0.049(3) 0.029(3) 0.044(4) 0.001(3) 0.005(3) 0.010(3) C14 0.046(3) 0.046(4) 0.035(4) 0.003(3) 0.010(3) 0.016(3) C15 0.041(3) 0.049(4) 0.045(4) 0.014(3) 0.018(3) 0.004(3) C16 0.031(3) 0.050(4) 0.056(5) 0.014(4) 0.012(3) 0.005(3) C17 0.041(3) 0.034(4) 0.044(4) -0.004(3) -0.005(3) 0.006(2) C18 0.043(3) 0.036(4) 0.044(5) 0.000(3) -0.011(3) 0.007(3) C19 0.053(3) 0.049(4) 0.037(4) 0.000(3) 0.015(3) 0.024(3) C20 0.057(4) 0.062(5) 0.038(4) 0.018(4) 0.022(4) 0.022(3) C21 0.034(3) 0.040(4) 0.042(4) 0.006(3) 0.000(3) 0.010(2) C22 0.037(3) 0.044(4) 0.043(4) 0.016(3) -0.001(3) 0.018(3) C23 0.049(3) 0.053(4) 0.031(4) 0.016(3) -0.001(3) 0.011(3) C24 0.036(3) 0.052(4) 0.031(4) 0.005(3) -0.008(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Zn1 2.3366(13) . ? Br2 Zn1 2.3411(10) . ? Br3 Zn2 2.4828(12) . ? Br3 Zn1 2.4958(13) . ? Br4 Zn1 2.4680(11) . ? Br4 Zn2 2.4882(13) . ? Br5 Zn2 2.3576(13) . ? Br6 Zn2 2.3184(10) . ? Br7 Zn3 2.3761(10) . ? Br8 Zn4 2.3367(10) . ? Zn3 O6 2.092(4) . ? Zn3 O4 2.229(5) . ? Zn3 O3 2.229(4) . ? Zn3 O5 2.257(4) . ? Zn3 O2 2.259(5) . ? Zn4 O12 2.064(4) . ? Zn4 O9 2.251(4) . ? Zn4 O8 2.261(4) . ? Zn4 O10 2.302(4) . ? Zn4 O7 2.346(5) . ? Zn4 O11 2.487(4) . ? O1 C12 1.423(8) . ? O1 C1 1.430(8) . ? O2 C3 1.415(7) . ? O2 C2 1.432(8) . ? O3 C4 1.411(8) . ? O3 C5 1.412(8) . ? O4 C6 1.414(8) . ? O4 C7 1.418(7) . ? O5 C9 1.432(7) . ? O5 C8 1.435(8) . ? O6 C10 1.429(7) . ? O6 C11 1.437(9) . ? O7 C24 1.432(8) . ? O7 C13 1.439(7) . ? O8 C14 1.406(8) . ? O8 C15 1.420(7) . ? O9 C16 1.428(7) . ? O9 C17 1.434(8) . ? O10 C18 1.411(7) . ? O10 C19 1.415(6) . ? O11 C21 1.418(8) . ? O11 C20 1.433(8) . ? O12 C23 1.427(8) . ? O12 C22 1.452(6) . ? C1 C2 1.508(8) . ? C3 C4 1.470(12) . ? C5 C6 1.465(10) . ? C7 C8 1.489(10) . ? C9 C10 1.505(9) . ? C11 C12 1.510(11) . ? C13 C14 1.499(8) . ? C15 C16 1.499(10) . ? C17 C18 1.490(8) . ? C19 C20 1.475(10) . ? C21 C22 1.480(8) . ? C23 C24 1.500(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn2 Br3 Zn1 82.97(4) . . ? Zn1 Br4 Zn2 83.43(4) . . ? Br1 Zn1 Br2 117.19(5) . . ? Br1 Zn1 Br4 113.72(4) . . ? Br2 Zn1 Br4 108.94(4) . . ? Br1 Zn1 Br3 110.01(5) . . ? Br2 Zn1 Br3 108.14(4) . . ? Br4 Zn1 Br3 96.82(4) . . ? Br6 Zn2 Br5 117.45(5) . . ? Br6 Zn2 Br3 111.73(5) . . ? Br5 Zn2 Br3 110.31(4) . . ? Br6 Zn2 Br4 108.32(5) . . ? Br5 Zn2 Br4 110.39(5) . . ? Br3 Zn2 Br4 96.64(4) . . ? O6 Zn3 O4 93.69(17) . . ? O6 Zn3 O3 89.12(15) . . ? O4 Zn3 O3 70.50(17) . . ? O6 Zn3 O5 76.31(15) . . ? O4 Zn3 O5 71.97(15) . . ? O3 Zn3 O5 138.55(16) . . ? O6 Zn3 O2 92.06(17) . . ? O4 Zn3 O2 140.13(15) . . ? O3 Zn3 O2 70.19(16) . . ? O5 Zn3 O2 147.26(15) . . ? O6 Zn3 Br7 164.66(11) . . ? O4 Zn3 Br7 94.35(12) . . ? O3 Zn3 Br7 105.89(11) . . ? O5 Zn3 Br7 93.82(11) . . ? O2 Zn3 Br7 90.12(12) . . ? O12 Zn4 O9 90.31(16) . . ? O12 Zn4 O8 91.09(16) . . ? O9 Zn4 O8 70.19(15) . . ? O12 Zn4 O10 94.41(17) . . ? O9 Zn4 O10 69.71(15) . . ? O8 Zn4 O10 139.52(15) . . ? O12 Zn4 Br8 162.80(11) . . ? O9 Zn4 Br8 106.89(12) . . ? O8 Zn4 Br8 94.94(12) . . ? O10 Zn4 Br8 91.44(12) . . ? O12 Zn4 O7 75.02(16) . . ? O9 Zn4 O7 136.62(15) . . ? O8 Zn4 O7 69.55(14) . . ? O10 Zn4 O7 150.18(13) . . ? Br8 Zn4 O7 92.01(11) . . ? O12 Zn4 O11 72.60(14) . . ? O9 Zn4 O11 132.40(15) . . ? O8 Zn4 O11 150.48(16) . . ? O10 Zn4 O11 67.87(15) . . ? Br8 Zn4 O11 94.81(11) . . ? O7 Zn4 O11 82.32(15) . . ? C12 O1 C1 114.3(5) . . ? C3 O2 C2 113.9(5) . . ? C3 O2 Zn3 118.5(4) . . ? C2 O2 Zn3 124.3(3) . . ? C4 O3 C5 113.0(5) . . ? C4 O3 Zn3 115.0(4) . . ? C5 O3 Zn3 116.4(4) . . ? C6 O4 C7 116.7(6) . . ? C6 O4 Zn3 118.2(4) . . ? C7 O4 Zn3 119.6(4) . . ? C9 O5 C8 114.7(5) . . ? C9 O5 Zn3 112.2(4) . . ? C8 O5 Zn3 109.2(3) . . ? C10 O6 C11 115.4(5) . . ? C10 O6 Zn3 114.1(4) . . ? C11 O6 Zn3 115.4(4) . . ? C24 O7 C13 115.3(5) . . ? C24 O7 Zn4 110.9(4) . . ? C13 O7 Zn4 108.8(4) . . ? C14 O8 C15 115.2(4) . . ? C14 O8 Zn4 122.4(3) . . ? C15 O8 Zn4 117.5(4) . . ? C16 O9 C17 111.1(5) . . ? C16 O9 Zn4 116.1(4) . . ? C17 O9 Zn4 114.5(3) . . ? C18 O10 C19 114.5(5) . . ? C18 O10 Zn4 116.5(4) . . ? C19 O10 Zn4 122.6(4) . . ? C21 O11 C20 114.4(5) . . ? C21 O11 Zn4 108.9(3) . . ? C20 O11 Zn4 107.3(4) . . ? C23 O12 C22 115.7(5) . . ? C23 O12 Zn4 116.4(4) . . ? C22 O12 Zn4 114.5(3) . . ? O1 C1 C2 111.7(5) . . ? O2 C2 C1 106.2(5) . . ? O2 C3 C4 106.7(6) . . ? O3 C4 C3 109.0(5) . . ? O3 C5 C6 109.0(5) . . ? O4 C6 C5 107.2(6) . . ? O4 C7 C8 106.4(6) . . ? O5 C8 C7 111.1(5) . . ? O5 C9 C10 110.3(4) . . ? O6 C10 C9 110.4(5) . . ? O6 C11 C12 111.2(6) . . ? O1 C12 C11 110.1(5) . . ? O7 C13 C14 110.8(5) . . ? O8 C14 C13 105.7(5) . . ? O8 C15 C16 106.3(5) . . ? O9 C16 C15 106.6(5) . . ? O9 C17 C18 105.3(5) . . ? O10 C18 C17 106.7(5) . . ? O10 C19 C20 107.2(5) . . ? O11 C20 C19 111.3(5) . . ? O11 C21 C22 110.6(5) . . ? O12 C22 C21 111.0(5) . . ? O12 C23 C24 111.2(5) . . ? O7 C24 C23 110.3(5) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.261 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 936448' ####################################################################### # # 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_Compound-2_Zn6Br12(18c6)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Br12 O12 Zn6' _chemical_formula_weight 1879.76 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1203(16) _cell_length_b 10.887(2) _cell_length_c 14.851(3) _cell_angle_alpha 79.16(3) _cell_angle_beta 74.99(3) _cell_angle_gamma 79.78(3) _cell_volume 1234.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 12.66 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_T_max 0.28 _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12074 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.22 _reflns_number_total 6139 _reflns_number_gt 4340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'CELL, SELECT (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND, Crystal Impact' _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^)+(0.0422P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6139 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.35516(7) -0.16462(7) 0.41928(4) 0.04765(17) Uani 1 1 d . . . Br2 Br 1.16290(12) 0.26691(8) 0.34694(5) 0.0696(2) Uani 1 1 d . . . Br3 Br 1.18250(9) 0.05595(6) 0.14077(4) 0.05047(17) Uani 1 1 d . . . Br4 Br 1.37812(7) 0.38053(5) 0.08102(4) 0.03964(14) Uani 1 1 d . . . Br5 Br 1.11709(7) 0.72157(5) 0.10940(4) 0.03632(13) Uani 1 1 d . . . Br6 Br 0.86957(7) 0.43348(5) 0.11298(3) 0.03461(13) Uani 1 1 d . . . Zn1 Zn 1.62653(7) -0.20435(6) 0.32203(4) 0.03216(14) Uani 1 1 d . . . Zn2 Zn 1.28260(8) 0.20043(6) 0.20190(4) 0.03614(15) Uani 1 1 d . . . Zn3 Zn 1.13344(8) 0.53359(6) 0.05571(4) 0.03117(14) Uani 1 1 d . . . O1 O 1.5385(5) 0.1230(3) 0.2007(2) 0.0327(8) Uani 1 1 d . . . O2 O 1.6639(5) -0.1335(3) 0.1806(2) 0.0320(8) Uani 1 1 d . . . O3 O 1.5890(5) -0.3564(3) 0.2590(2) 0.0326(8) Uani 1 1 d . . . O4 O 1.6542(5) -0.4517(4) 0.4318(3) 0.0437(10) Uani 1 1 d . . . O5 O 1.8576(5) -0.2681(4) 0.3513(3) 0.0426(9) Uani 1 1 d . . . O6 O 1.7237(6) -0.0334(4) 0.3371(3) 0.0466(10) Uani 1 1 d . . . C1 C 1.6427(7) 0.0853(5) 0.1128(3) 0.0369(12) Uani 1 1 d . . . H1A H 1.7111 0.1533 0.0777 0.044 Uiso 1 1 calc R . . H1B H 1.5668 0.0726 0.0738 0.044 Uiso 1 1 calc R . . C2 C 1.7610(7) -0.0337(5) 0.1297(4) 0.0349(11) Uani 1 1 d . . . H2A H 1.8304 -0.0576 0.0686 0.042 Uiso 1 1 calc R . . H2B H 1.8407 -0.0204 0.1663 0.042 Uiso 1 1 calc R . . C3 C 1.6237(8) -0.2083(5) 0.1217(3) 0.0367(12) Uani 1 1 d . . . H3A H 1.7301 -0.2561 0.0881 0.044 Uiso 1 1 calc R . . H3B H 1.5660 -0.1537 0.0744 0.044 Uiso 1 1 calc R . . C4 C 1.5078(7) -0.2961(6) 0.1843(4) 0.0378(12) Uani 1 1 d . . . H4A H 1.3943 -0.2492 0.2100 0.045 Uiso 1 1 calc R . . H4B H 1.4907 -0.3596 0.1491 0.045 Uiso 1 1 calc R . . C5 C 1.5025(8) -0.4565(5) 0.3186(4) 0.0421(14) Uani 1 1 d . . . H5A H 1.4727 -0.5103 0.2800 0.050 Uiso 1 1 calc R . . H5B H 1.3950 -0.4214 0.3602 0.050 Uiso 1 1 calc R . . C6 C 1.6213(9) -0.5325(5) 0.3764(4) 0.0424(14) Uani 1 1 d . . . H6A H 1.5674 -0.6045 0.4173 0.051 Uiso 1 1 calc R . . H6B H 1.7300 -0.5659 0.3349 0.051 Uiso 1 1 calc R . . C7 C 1.8262(8) -0.4705(6) 0.4405(4) 0.0424(13) Uani 1 1 d . . . H7A H 1.8716 -0.5615 0.4448 0.051 Uiso 1 1 calc R . . H7B H 1.8318 -0.4409 0.4986 0.051 Uiso 1 1 calc R . . C8 C 1.9322(8) -0.3983(6) 0.3561(4) 0.0474(15) Uani 1 1 d . . . H8A H 2.0525 -0.4075 0.3622 0.057 Uiso 1 1 calc R . . H8B H 1.9321 -0.4308 0.2982 0.057 Uiso 1 1 calc R . . C9 C 1.9620(8) -0.1828(7) 0.3586(5) 0.0560(17) Uani 1 1 d . . . H9A H 2.0430 -0.1625 0.2971 0.067 Uiso 1 1 calc R . . H9B H 2.0301 -0.2212 0.4058 0.067 Uiso 1 1 calc R . . C10 C 1.8534(8) -0.0664(7) 0.3873(5) 0.0506(16) Uani 1 1 d . . . H10A H 1.8013 -0.0802 0.4558 0.061 Uiso 1 1 calc R . . H10B H 1.9246 0.0028 0.3740 0.061 Uiso 1 1 calc R . . C11 C 1.6213(10) 0.0869(6) 0.3490(4) 0.0520(16) Uani 1 1 d . . . H11A H 1.6636 0.1281 0.3910 0.062 Uiso 1 1 calc R . . H11B H 1.5003 0.0746 0.3789 0.062 Uiso 1 1 calc R . . C12 C 1.6303(9) 0.1700(6) 0.2555(4) 0.0446(14) Uani 1 1 d . . . H12A H 1.5789 0.2574 0.2654 0.053 Uiso 1 1 calc R . . H12B H 1.7521 0.1715 0.2210 0.053 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 Br1 0.0333(3) 0.0677(4) 0.0438(3) -0.0254(3) -0.0057(2) 0.0015(3) Br2 0.0843(5) 0.0648(5) 0.0442(3) -0.0188(3) 0.0012(3) 0.0181(4) Br3 0.0525(4) 0.0483(4) 0.0563(3) -0.0077(3) -0.0122(3) -0.0228(3) Br4 0.0330(3) 0.0305(3) 0.0511(3) 0.0048(2) -0.0112(2) -0.0024(2) Br5 0.0384(3) 0.0317(3) 0.0416(3) -0.0123(2) -0.0107(2) -0.0028(2) Br6 0.0374(3) 0.0384(3) 0.0281(2) -0.00289(18) -0.00498(19) -0.0114(2) Zn1 0.0274(3) 0.0395(3) 0.0328(3) -0.0112(2) -0.0093(2) -0.0032(3) Zn2 0.0366(3) 0.0323(3) 0.0378(3) -0.0071(2) -0.0047(2) -0.0041(3) Zn3 0.0338(3) 0.0281(3) 0.0327(3) -0.0061(2) -0.0093(2) -0.0031(3) O1 0.0363(19) 0.0311(19) 0.0304(16) -0.0051(13) -0.0087(14) -0.0016(17) O2 0.0395(19) 0.0287(18) 0.0312(16) -0.0040(13) -0.0146(14) -0.0045(17) O3 0.0340(18) 0.0309(19) 0.0351(17) -0.0051(13) -0.0097(14) -0.0079(17) O4 0.041(2) 0.046(2) 0.0408(19) -0.0122(17) -0.0025(17) -0.002(2) O5 0.034(2) 0.035(2) 0.060(2) -0.0007(17) -0.0192(18) -0.0020(19) O6 0.069(3) 0.033(2) 0.050(2) -0.0134(17) -0.038(2) 0.004(2) C1 0.037(3) 0.034(3) 0.036(2) 0.001(2) -0.007(2) -0.004(3) C2 0.030(2) 0.033(3) 0.039(2) -0.006(2) -0.004(2) -0.004(2) C3 0.044(3) 0.037(3) 0.034(2) -0.007(2) -0.018(2) -0.004(3) C4 0.038(3) 0.044(3) 0.040(3) -0.012(2) -0.019(2) -0.003(3) C5 0.046(3) 0.037(3) 0.045(3) -0.012(2) -0.003(2) -0.018(3) C6 0.061(4) 0.029(3) 0.034(2) -0.009(2) -0.004(2) -0.004(3) C7 0.046(3) 0.040(3) 0.034(2) 0.002(2) -0.007(2) -0.001(3) C8 0.035(3) 0.042(3) 0.056(3) -0.001(3) -0.003(3) 0.002(3) C9 0.042(3) 0.054(4) 0.086(5) -0.016(3) -0.034(3) -0.009(3) C10 0.044(3) 0.053(4) 0.068(4) -0.019(3) -0.027(3) -0.007(3) C11 0.081(5) 0.037(3) 0.048(3) -0.016(2) -0.032(3) 0.003(3) C12 0.054(4) 0.027(3) 0.060(3) -0.009(2) -0.026(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Zn1 2.3189(11) . ? Br2 Zn2 2.3153(11) . ? Br3 Zn2 2.3091(10) . ? Br4 Zn3 2.4170(12) . ? Br4 Zn2 2.4827(12) . ? Br5 Zn3 2.3031(9) . ? Br6 Zn3 2.4573(11) . ? Br6 Zn3 2.4690(9) 2_765 ? Zn1 O5 2.009(4) . ? Zn1 O2 2.060(3) . ? Zn1 O3 2.149(3) . ? Zn1 O6 2.216(4) . ? Zn2 O1 2.096(4) . ? Zn3 Br6 2.4690(9) 2_765 ? O1 C12 1.446(7) . ? O1 C1 1.447(6) . ? O2 C3 1.429(6) . ? O2 C2 1.435(6) . ? O3 C4 1.431(7) . ? O3 C5 1.432(6) . ? O4 C6 1.411(7) . ? O4 C7 1.412(8) . ? O5 C9 1.399(7) . ? O5 C8 1.436(7) . ? O6 C10 1.401(8) . ? O6 C11 1.436(8) . ? C1 C2 1.492(8) . ? C3 C4 1.483(8) . ? C5 C6 1.493(9) . ? C7 C8 1.496(7) . ? C9 C10 1.475(10) . ? C11 C12 1.500(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn3 Br4 Zn2 110.34(4) . . ? Zn3 Br6 Zn3 83.89(4) . 2_765 ? O5 Zn1 O2 108.45(16) . . ? O5 Zn1 O3 101.31(16) . . ? O2 Zn1 O3 75.92(13) . . ? O5 Zn1 O6 75.29(17) . . ? O2 Zn1 O6 86.26(14) . . ? O3 Zn1 O6 159.88(14) . . ? O5 Zn1 Br1 131.54(12) . . ? O2 Zn1 Br1 118.73(12) . . ? O3 Zn1 Br1 100.15(10) . . ? O6 Zn1 Br1 96.56(13) . . ? O1 Zn2 Br3 103.62(10) . . ? O1 Zn2 Br2 107.23(10) . . ? Br3 Zn2 Br2 125.74(4) . . ? O1 Zn2 Br4 91.03(10) . . ? Br3 Zn2 Br4 112.48(4) . . ? Br2 Zn2 Br4 110.43(4) . . ? Br5 Zn3 Br4 114.65(4) . . ? Br5 Zn3 Br6 114.29(4) . . ? Br4 Zn3 Br6 109.54(3) . . ? Br5 Zn3 Br6 111.75(4) . 2_765 ? Br4 Zn3 Br6 108.92(4) . 2_765 ? Br6 Zn3 Br6 96.11(4) . 2_765 ? C12 O1 C1 114.9(4) . . ? C12 O1 Zn2 119.3(3) . . ? C1 O1 Zn2 116.5(3) . . ? C3 O2 C2 114.0(4) . . ? C3 O2 Zn1 116.8(3) . . ? C2 O2 Zn1 127.6(3) . . ? C4 O3 C5 113.0(4) . . ? C4 O3 Zn1 104.9(3) . . ? C5 O3 Zn1 118.5(3) . . ? C6 O4 C7 113.8(5) . . ? C9 O5 C8 116.3(5) . . ? C9 O5 Zn1 120.1(4) . . ? C8 O5 Zn1 123.3(4) . . ? C10 O6 C11 115.3(4) . . ? C10 O6 Zn1 110.4(4) . . ? C11 O6 Zn1 125.2(4) . . ? O1 C1 C2 111.3(4) . . ? O2 C2 C1 110.1(4) . . ? O2 C3 C4 106.8(4) . . ? O3 C4 C3 106.7(4) . . ? O3 C5 C6 107.8(5) . . ? O4 C6 C5 107.3(5) . . ? O4 C7 C8 108.9(5) . . ? O5 C8 C7 107.6(5) . . ? O5 C9 C10 109.5(5) . . ? O6 C10 C9 109.2(5) . . ? O6 C11 C12 110.5(5) . . ? O1 C12 C11 109.8(5) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.837 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.136 _database_code_depnum_ccdc_archive 'CCDC 936449' ####################################################################### # # 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_Compound-4_Zn8Br16(18c6)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Br16 O12 Zn8' _chemical_formula_weight 2330.14 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6801(15) _cell_length_b 12.809(3) _cell_length_c 29.307(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.41(3) _cell_angle_gamma 90.00 _cell_volume 2883.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 14.44 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0763 _exptl_absorpt_correction_T_max 0.2414 _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21276 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5707 _reflns_number_gt 4104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'CELL, SELECT (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND, Crystal Impact' _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^)+(0.0469P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00038(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5707 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.24566(9) 0.03700(6) 0.08569(3) 0.04061(19) Uani 1 1 d . . . Br2 Br 0.72818(8) 0.10333(6) 0.17128(2) 0.03453(17) Uani 1 1 d . . . Br3 Br 0.68984(10) -0.10719(6) 0.26822(2) 0.03922(18) Uani 1 1 d . . . Br4 Br 0.54210(10) 0.15151(6) 0.29247(3) 0.04117(19) Uani 1 1 d . . . Br5 Br 0.97293(10) 0.06261(6) 0.36087(3) 0.0489(2) Uani 1 1 d . . . Br6 Br 0.52310(11) -0.06901(6) 0.38831(3) 0.0462(2) Uani 1 1 d . . . Br7 Br 0.43095(12) 0.22589(7) 0.42753(3) 0.0574(2) Uani 1 1 d . . . Br8 Br 0.73431(10) 0.02486(7) 0.50102(3) 0.0487(2) Uani 1 1 d . . . Zn1 Zn 0.52941(10) 0.08163(6) 0.10649(3) 0.03252(19) Uani 1 1 d . . . Zn2 Zn 0.52010(10) 0.03126(6) 0.22468(3) 0.03290(19) Uani 1 1 d . . . Zn3 Zn 0.70323(11) 0.01591(6) 0.33225(3) 0.03468(19) Uani 1 1 d . . . Zn4 Zn 0.48482(12) 0.05605(7) 0.44973(3) 0.0437(2) Uani 1 1 d . . . O1 O 0.5037(6) 0.2493(4) 0.10649(17) 0.0385(12) Uani 1 1 d . . . O2 O 0.6471(6) 0.1248(4) 0.04580(18) 0.0411(12) Uani 1 1 d . . . O3 O 0.6703(7) -0.0566(4) 0.08694(17) 0.0419(12) Uani 1 1 d . . . O4 O 0.4803(6) -0.0958(3) 0.17114(16) 0.0331(11) Uani 1 1 d . . . O5 O 0.2610(6) -0.0118(4) 0.22974(17) 0.0377(12) Uani 1 1 d . . . O6 O 0.3370(6) 0.1745(4) 0.19382(18) 0.0400(12) Uani 1 1 d . . . C1 C 0.7861(10) 0.0544(7) 0.0328(3) 0.050(2) Uani 1 1 d . . . H1A H 0.8912 0.0670 0.0517 0.059 Uiso 1 1 calc R . . H1B H 0.8166 0.0648 0.0003 0.059 Uiso 1 1 calc R . . C2 C 0.7204(11) -0.0517(7) 0.0401(3) 0.051(2) Uani 1 1 d . . . H2A H 0.6193 -0.0657 0.0199 0.061 Uiso 1 1 calc R . . H2B H 0.8123 -0.1037 0.0336 0.061 Uiso 1 1 calc R . . C3 C 0.6162(11) -0.1575(6) 0.1015(3) 0.0433(18) Uani 1 1 d . . . H3A H 0.6956 -0.2116 0.0895 0.052 Uiso 1 1 calc R . . H3B H 0.4968 -0.1724 0.0904 0.052 Uiso 1 1 calc R . . C4 C 0.6212(10) -0.1570(6) 0.1530(3) 0.0421(18) Uani 1 1 d . . . H4A H 0.6124 -0.2295 0.1644 0.051 Uiso 1 1 calc R . . H4B H 0.7336 -0.1278 0.1637 0.051 Uiso 1 1 calc R . . C5 C 0.3323(10) -0.1576(5) 0.1839(3) 0.0417(18) Uani 1 1 d . . . H5A H 0.3633 -0.2041 0.2097 0.050 Uiso 1 1 calc R . . H5B H 0.2936 -0.2013 0.1579 0.050 Uiso 1 1 calc R . . C6 C 0.1920(10) -0.0852(6) 0.1974(3) 0.0435(18) Uani 1 1 d . . . H6A H 0.1466 -0.0479 0.1703 0.052 Uiso 1 1 calc R . . H6B H 0.0950 -0.1248 0.2112 0.052 Uiso 1 1 calc R . . C7 C 0.1424(10) 0.0745(6) 0.2375(3) 0.0443(19) Uani 1 1 d . . . H7A H 0.1718 0.1091 0.2668 0.053 Uiso 1 1 calc R . . H7B H 0.0216 0.0480 0.2394 0.053 Uiso 1 1 calc R . . C8 C 0.1559(9) 0.1513(6) 0.1993(3) 0.0415(18) Uani 1 1 d . . . H8A H 0.1071 0.1212 0.1709 0.050 Uiso 1 1 calc R . . H8B H 0.0904 0.2156 0.2067 0.050 Uiso 1 1 calc R . . C9 C 0.3734(10) 0.2789(6) 0.1792(3) 0.0460(19) Uani 1 1 d . . . H9A H 0.4928 0.2976 0.1892 0.055 Uiso 1 1 calc R . . H9B H 0.2919 0.3270 0.1946 0.055 Uiso 1 1 calc R . . C10 C 0.3587(10) 0.2950(6) 0.1290(3) 0.047(2) Uani 1 1 d . . . H10A H 0.2495 0.2630 0.1175 0.057 Uiso 1 1 calc R . . H10B H 0.3543 0.3707 0.1222 0.057 Uiso 1 1 calc R . . C11 C 0.5298(12) 0.2881(7) 0.0617(3) 0.054(2) Uani 1 1 d . . . H11A H 0.5506 0.3643 0.0624 0.065 Uiso 1 1 calc R . . H11B H 0.4261 0.2741 0.0424 0.065 Uiso 1 1 calc R . . C12 C 0.6841(13) 0.2329(7) 0.0434(3) 0.060(2) Uani 1 1 d . . . H12A H 0.7051 0.2540 0.0114 0.071 Uiso 1 1 calc R . . H12B H 0.7890 0.2498 0.0618 0.071 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 Br1 0.0345(4) 0.0513(4) 0.0359(4) -0.0017(3) -0.0059(3) -0.0053(3) Br2 0.0277(3) 0.0428(4) 0.0330(4) 0.0040(3) -0.0039(3) -0.0039(3) Br3 0.0541(4) 0.0338(4) 0.0297(4) -0.0017(3) -0.0057(3) 0.0084(3) Br4 0.0537(4) 0.0334(4) 0.0363(4) -0.0045(3) -0.0103(3) 0.0083(3) Br5 0.0440(4) 0.0413(4) 0.0614(6) 0.0047(4) -0.0121(4) -0.0039(3) Br6 0.0559(5) 0.0458(4) 0.0371(4) -0.0039(3) 0.0102(4) -0.0127(4) Br7 0.0670(5) 0.0469(5) 0.0584(6) 0.0006(4) 0.0064(5) 0.0004(4) Br8 0.0374(4) 0.0679(5) 0.0408(5) -0.0045(4) 0.0043(3) -0.0107(4) Zn1 0.0303(4) 0.0378(4) 0.0294(4) 0.0029(3) -0.0014(3) -0.0001(3) Zn2 0.0338(4) 0.0353(4) 0.0296(4) 0.0004(3) -0.0001(3) -0.0017(3) Zn3 0.0395(4) 0.0350(4) 0.0295(4) 0.0020(3) -0.0025(4) -0.0003(3) Zn4 0.0473(5) 0.0459(5) 0.0380(5) -0.0037(4) 0.0059(4) -0.0046(4) O1 0.042(3) 0.037(3) 0.036(3) 0.010(2) 0.000(2) -0.001(2) O2 0.036(3) 0.051(3) 0.036(3) 0.007(2) 0.003(2) 0.001(2) O3 0.050(3) 0.046(3) 0.030(3) -0.001(2) 0.005(2) 0.011(2) O4 0.038(2) 0.027(2) 0.034(3) -0.001(2) 0.002(2) 0.0054(19) O5 0.035(2) 0.043(3) 0.036(3) -0.004(2) 0.003(2) 0.000(2) O6 0.026(2) 0.050(3) 0.044(3) 0.000(2) 0.002(2) -0.002(2) C1 0.040(4) 0.073(6) 0.036(5) -0.001(4) 0.009(4) 0.007(4) C2 0.053(5) 0.071(6) 0.028(4) -0.007(4) 0.005(4) 0.019(4) C3 0.049(4) 0.043(4) 0.038(4) -0.011(3) -0.002(4) 0.012(3) C4 0.053(4) 0.031(4) 0.042(5) -0.006(3) -0.001(4) 0.009(3) C5 0.055(4) 0.028(3) 0.042(4) -0.001(3) 0.000(4) -0.018(3) C6 0.045(4) 0.043(4) 0.043(5) -0.001(3) 0.000(4) -0.013(3) C7 0.035(4) 0.055(5) 0.043(5) -0.008(4) 0.009(4) -0.002(3) C8 0.025(3) 0.046(4) 0.053(5) -0.008(4) 0.002(3) 0.004(3) C9 0.046(4) 0.039(4) 0.053(5) -0.013(4) -0.005(4) -0.010(3) C10 0.044(4) 0.037(4) 0.060(6) 0.001(4) -0.005(4) 0.000(3) C11 0.071(6) 0.048(5) 0.043(5) 0.018(4) -0.001(4) -0.002(4) C12 0.077(6) 0.054(5) 0.047(5) 0.011(4) 0.008(5) -0.015(5) _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 Br1 Zn1 2.3300(12) . ? Br2 Zn2 2.4271(11) . ? Br2 Zn1 2.4438(13) . ? Br3 Zn3 2.4528(12) . ? Br3 Zn2 2.5395(12) . ? Br4 Zn3 2.4263(12) . ? Br4 Zn2 2.5185(11) . ? Br5 Zn3 2.3081(13) . ? Br6 Zn3 2.4143(12) . ? Br6 Zn4 2.4290(12) . ? Br7 Zn4 2.3073(14) . ? Br8 Zn4 2.4544(12) 3_656 ? Br8 Zn4 2.4596(15) . ? Zn1 O2 2.076(5) . ? Zn1 O3 2.154(5) . ? Zn1 O1 2.156(5) . ? Zn2 O5 2.072(5) . ? Zn2 O4 2.280(5) . ? Zn2 O6 2.478(5) . ? Zn4 Br8 2.4544(12) 3_656 ? O1 C11 1.419(9) . ? O1 C10 1.425(9) . ? O2 C12 1.416(10) . ? O2 C1 1.450(9) . ? O3 C3 1.424(9) . ? O3 C2 1.430(9) . ? O4 C5 1.437(8) . ? O4 C4 1.441(8) . ? O5 C6 1.434(9) . ? O5 C7 1.451(9) . ? O6 C9 1.432(9) . ? O6 C8 1.433(8) . ? C1 C2 1.465(12) . ? C3 C4 1.509(11) . ? C5 C6 1.477(11) . ? C7 C8 1.493(11) . ? C9 C10 1.490(12) . ? C11 C12 1.483(12) . ? 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 Zn2 Br2 Zn1 92.71(4) . . ? Zn3 Br3 Zn2 87.36(4) . . ? Zn3 Br4 Zn2 88.42(4) . . ? Zn3 Br6 Zn4 106.26(4) . . ? Zn4 Br8 Zn4 83.89(4) 3_656 . ? O2 Zn1 O3 76.6(2) . . ? O2 Zn1 O1 77.02(19) . . ? O3 Zn1 O1 149.81(19) . . ? O2 Zn1 Br1 104.67(15) . . ? O3 Zn1 Br1 101.49(16) . . ? O1 Zn1 Br1 99.15(14) . . ? O2 Zn1 Br2 111.23(15) . . ? O3 Zn1 Br2 89.32(16) . . ? O1 Zn1 Br2 86.75(14) . . ? Br1 Zn1 Br2 144.01(4) . . ? O5 Zn2 O4 74.64(18) . . ? O5 Zn2 Br2 141.70(15) . . ? O4 Zn2 Br2 85.02(11) . . ? O5 Zn2 O6 71.36(18) . . ? O4 Zn2 O6 101.78(17) . . ? Br2 Zn2 O6 81.82(11) . . ? O5 Zn2 Br4 99.53(14) . . ? O4 Zn2 Br4 170.92(12) . . ? Br2 Zn2 Br4 103.60(4) . . ? O6 Zn2 Br4 82.52(13) . . ? O5 Zn2 Br3 105.55(15) . . ? O4 Zn2 Br3 85.02(12) . . ? Br2 Zn2 Br3 104.57(4) . . ? O6 Zn2 Br3 171.17(12) . . ? Br4 Zn2 Br3 89.97(4) . . ? Br5 Zn3 Br6 112.74(5) . . ? Br5 Zn3 Br4 116.26(5) . . ? Br6 Zn3 Br4 110.91(4) . . ? Br5 Zn3 Br3 118.51(5) . . ? Br6 Zn3 Br3 102.12(4) . . ? Br4 Zn3 Br3 94.25(4) . . ? Br7 Zn4 Br6 115.81(5) . . ? Br7 Zn4 Br8 116.21(5) . 3_656 ? Br6 Zn4 Br8 104.15(5) . 3_656 ? Br7 Zn4 Br8 117.57(5) . . ? Br6 Zn4 Br8 104.35(5) . . ? Br8 Zn4 Br8 96.11(4) 3_656 . ? C11 O1 C10 113.6(6) . . ? C11 O1 Zn1 109.6(5) . . ? C10 O1 Zn1 118.8(4) . . ? C12 O2 C1 116.5(6) . . ? C12 O2 Zn1 113.1(5) . . ? C1 O2 Zn1 112.7(4) . . ? C3 O3 C2 114.2(6) . . ? C3 O3 Zn1 121.2(4) . . ? C2 O3 Zn1 111.0(5) . . ? C5 O4 C4 113.2(5) . . ? C5 O4 Zn2 108.4(4) . . ? C4 O4 Zn2 123.0(4) . . ? C6 O5 C7 112.0(6) . . ? C6 O5 Zn2 118.6(4) . . ? C7 O5 Zn2 114.4(4) . . ? C9 O6 C8 114.8(6) . . ? C9 O6 Zn2 133.5(4) . . ? C8 O6 Zn2 110.7(4) . . ? O2 C1 C2 106.4(6) . . ? O3 C2 C1 106.1(7) . . ? O3 C3 C4 106.9(6) . . ? O4 C4 C3 110.9(6) . . ? O4 C5 C6 107.7(6) . . ? O5 C6 C5 108.8(6) . . ? O5 C7 C8 109.7(5) . . ? O6 C8 C7 107.1(6) . . ? O6 C9 C10 114.3(6) . . ? O1 C10 C9 110.2(7) . . ? O1 C11 C12 106.6(7) . . ? O2 C12 C11 106.7(7) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.000 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 936450' ####################################################################### # # 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_Compound-4_Zn10Br20(18c6)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Br20 O12 Zn10' _chemical_formula_weight 2780.52 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4651(15) _cell_length_b 12.263(3) _cell_length_c 17.910(4) _cell_angle_alpha 101.09(3) _cell_angle_beta 93.90(3) _cell_angle_gamma 90.42(3) _cell_volume 1604.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 16.20 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1409 _exptl_absorpt_correction_T_max 0.3223 _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15653 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 29.27 _reflns_number_total 8003 _reflns_number_gt 5367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'CELL, SELECT (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND, Crystal Impact' _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^)+(0.0543P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00064(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8003 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 Br1 Br 1.23541(11) 0.36180(8) 0.34298(6) 0.0498(2) Uani 1 1 d . . . Br2 Br 0.65182(9) 0.31794(6) 0.22396(4) 0.03077(16) Uani 1 1 d . . . Br3 Br 0.70646(12) 0.40214(7) 0.02774(4) 0.03935(19) Uani 1 1 d . . . Br4 Br 0.71292(12) 0.10640(7) 0.03574(5) 0.0409(2) Uani 1 1 d . . . Br5 Br 0.36317(11) 0.20115(9) -0.12247(5) 0.0489(2) Uani 1 1 d . . . Br6 Br 0.84497(10) 0.19485(7) -0.15846(5) 0.03836(19) Uani 1 1 d . . . Br7 Br 0.52294(13) 0.34050(8) -0.29319(6) 0.0479(2) Uani 1 1 d . . . Br8 Br 0.50556(12) 0.00561(7) -0.30539(4) 0.0423(2) Uani 1 1 d . . . Br9 Br 0.90449(12) 0.13230(7) -0.39699(5) 0.0418(2) Uani 1 1 d . . . Br10 Br 0.61051(12) -0.13356(7) -0.50991(5) 0.03987(19) Uani 1 1 d . . . Zn1 Zn 0.92388(12) 0.35364(8) 0.31623(5) 0.0331(2) Uani 1 1 d . . . Zn2 Zn 0.85222(11) 0.28670(7) 0.12265(5) 0.0317(2) Uani 1 1 d . . . Zn3 Zn 0.65286(13) 0.22493(8) -0.05360(5) 0.0388(2) Uani 1 1 d . . . Zn4 Zn 0.55238(14) 0.19146(8) -0.23357(5) 0.0392(2) Uani 1 1 d . . . Zn5 Zn 0.62626(13) 0.04630(8) -0.42155(5) 0.0367(2) Uani 1 1 d . . . O1 O 0.8666(7) 0.5253(4) 0.3295(3) 0.0364(12) Uani 1 1 d . . . O2 O 0.8288(7) 0.3895(5) 0.4251(3) 0.0402(13) Uani 1 1 d . . . O3 O 0.8687(8) 0.1928(5) 0.3392(3) 0.0388(13) Uani 1 1 d . . . O4 O 1.0034(8) 0.1727(5) 0.1877(3) 0.0398(13) Uani 1 1 d . . . O5 O 1.1013(8) 0.2738(5) 0.0778(3) 0.0421(14) Uani 1 1 d . . . O6 O 0.9955(8) 0.4428(5) 0.1802(3) 0.0405(14) Uani 1 1 d . . . C1 C 0.8512(12) 0.5725(7) 0.4082(5) 0.044(2) Uani 1 1 d . . . H1A H 0.7931 0.6456 0.4134 0.053 Uiso 1 1 calc R . . H1B H 0.9714 0.5829 0.4358 0.053 Uiso 1 1 calc R . . C2 C 0.7396(13) 0.4930(8) 0.4395(5) 0.051(2) Uani 1 1 d . . . H2A H 0.7303 0.5188 0.4950 0.061 Uiso 1 1 calc R . . H2B H 0.6172 0.4856 0.4139 0.061 Uiso 1 1 calc R . . C3 C 0.7406(12) 0.2953(8) 0.4448(5) 0.048(2) Uani 1 1 d . . . H3A H 0.6190 0.2832 0.4185 0.057 Uiso 1 1 calc R . . H3B H 0.7295 0.3069 0.5005 0.057 Uiso 1 1 calc R . . C4 C 0.8548(14) 0.1994(8) 0.4195(5) 0.048(2) Uani 1 1 d . . . H4A H 0.9751 0.2104 0.4470 0.058 Uiso 1 1 calc R . . H4B H 0.7997 0.1302 0.4292 0.058 Uiso 1 1 calc R . . C5 C 0.9629(12) 0.0985(7) 0.3015(5) 0.045(2) Uani 1 1 d . . . H5A H 0.9239 0.0305 0.3187 0.054 Uiso 1 1 calc R . . H5B H 1.0937 0.1096 0.3142 0.054 Uiso 1 1 calc R . . C6 C 0.9237(13) 0.0859(6) 0.2190(5) 0.043(2) Uani 1 1 d . . . H6A H 0.9684 0.0133 0.1935 0.051 Uiso 1 1 calc R . . H6B H 0.7919 0.0854 0.2079 0.051 Uiso 1 1 calc R . . C7 C 1.1843(10) 0.1552(7) 0.1654(5) 0.068(3) Uani 1 1 d . . . H7A H 1.2187 0.0777 0.1664 0.082 Uiso 1 1 calc R . . H7B H 1.2687 0.2057 0.2014 0.082 Uiso 1 1 calc R . . C8 C 1.1933(10) 0.1772(7) 0.0892(5) 0.060(3) Uani 1 1 d R . . H8A H 1.3209 0.1854 0.0789 0.072 Uiso 1 1 calc R . . H8B H 1.1413 0.1125 0.0520 0.072 Uiso 1 1 calc R . . C9 C 1.2000(17) 0.3751(9) 0.0897(10) 0.096(5) Uani 1 1 d . . . H9A H 1.3293 0.3576 0.0906 0.115 Uiso 1 1 calc R . . H9B H 1.1725 0.4104 0.0451 0.115 Uiso 1 1 calc R . . C10 C 1.1729(18) 0.4508(12) 0.1533(9) 0.110(7) Uani 1 1 d . . . H10A H 1.1912 0.5262 0.1428 0.133 Uiso 1 1 calc R . . H10B H 1.2636 0.4407 0.1943 0.133 Uiso 1 1 calc R . . C11 C 0.9099(14) 0.5460(7) 0.2030(5) 0.046(2) Uani 1 1 d . . . H11A H 0.7783 0.5349 0.1931 0.055 Uiso 1 1 calc R . . H11B H 0.9495 0.5994 0.1721 0.055 Uiso 1 1 calc R . . C12 C 0.9526(13) 0.5940(7) 0.2862(5) 0.046(2) Uani 1 1 d . . . H12A H 1.0841 0.5959 0.2983 0.055 Uiso 1 1 calc R . . H12B H 0.9085 0.6708 0.2985 0.055 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 Br1 0.0286(4) 0.0626(6) 0.0552(5) 0.0045(4) 0.0016(4) -0.0026(4) Br2 0.0245(3) 0.0361(4) 0.0311(3) 0.0048(3) 0.0024(3) -0.0022(3) Br3 0.0457(4) 0.0365(4) 0.0351(4) 0.0066(3) -0.0009(4) -0.0008(4) Br4 0.0475(5) 0.0338(4) 0.0387(4) 0.0027(3) -0.0027(4) -0.0050(4) Br5 0.0307(4) 0.0745(6) 0.0382(4) 0.0028(4) 0.0022(3) -0.0050(4) Br6 0.0305(4) 0.0444(4) 0.0387(4) 0.0042(3) 0.0023(3) 0.0006(3) Br7 0.0456(5) 0.0435(5) 0.0549(5) 0.0132(4) -0.0043(4) 0.0009(4) Br8 0.0529(5) 0.0400(4) 0.0330(4) 0.0038(3) 0.0060(4) -0.0132(4) Br9 0.0401(4) 0.0417(4) 0.0440(4) 0.0116(3) -0.0032(4) -0.0099(4) Br10 0.0414(4) 0.0367(4) 0.0385(4) 0.0008(3) -0.0008(4) 0.0023(3) Zn1 0.0297(4) 0.0384(5) 0.0304(4) 0.0052(3) 0.0015(4) -0.0020(4) Zn2 0.0285(4) 0.0351(4) 0.0307(4) 0.0042(3) 0.0031(4) -0.0019(4) Zn3 0.0365(5) 0.0456(5) 0.0320(4) 0.0026(4) -0.0003(4) -0.0026(4) Zn4 0.0414(5) 0.0398(5) 0.0343(5) 0.0032(4) -0.0002(4) -0.0030(4) Zn5 0.0395(5) 0.0388(5) 0.0308(4) 0.0052(4) 0.0001(4) -0.0069(4) O1 0.039(3) 0.034(3) 0.031(3) -0.004(2) 0.002(2) 0.000(2) O2 0.031(3) 0.058(4) 0.032(3) 0.009(3) 0.004(2) 0.001(3) O3 0.040(3) 0.042(3) 0.038(3) 0.019(2) 0.005(3) 0.002(3) O4 0.032(3) 0.043(3) 0.049(3) 0.019(3) 0.009(3) 0.006(2) O5 0.036(3) 0.043(3) 0.049(3) 0.007(3) 0.024(3) 0.003(2) O6 0.040(3) 0.040(3) 0.039(3) 0.000(2) 0.007(3) -0.013(3) C1 0.046(5) 0.042(4) 0.037(4) -0.007(3) -0.004(4) 0.002(4) C2 0.050(5) 0.062(6) 0.037(4) -0.001(4) 0.008(4) 0.011(5) C3 0.043(5) 0.071(6) 0.034(4) 0.020(4) 0.007(4) -0.016(5) C4 0.056(6) 0.060(5) 0.034(4) 0.023(4) 0.000(4) -0.014(5) C5 0.040(4) 0.039(4) 0.059(5) 0.022(4) -0.002(4) 0.001(4) C6 0.048(5) 0.028(4) 0.053(5) 0.008(3) 0.004(4) -0.004(4) C7 0.047(6) 0.095(9) 0.072(7) 0.034(7) 0.021(6) 0.019(6) C8 0.048(5) 0.052(6) 0.085(8) 0.018(5) 0.024(6) 0.019(5) C9 0.067(7) 0.052(6) 0.174(15) 0.015(8) 0.072(9) -0.012(6) C10 0.082(9) 0.110(11) 0.116(11) -0.054(9) 0.072(9) -0.059(8) C11 0.066(6) 0.030(4) 0.041(4) 0.001(3) 0.006(4) -0.009(4) C12 0.047(5) 0.041(4) 0.049(5) 0.005(4) 0.006(4) -0.008(4) _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 Br1 Zn1 2.3398(13) . ? Br2 Zn2 2.4057(12) . ? Br2 Zn1 2.5099(14) . ? Br3 Zn3 2.3863(14) . ? Br3 Zn2 2.6028(15) . ? Br4 Zn3 2.3835(15) . ? Br4 Zn2 2.6104(15) . ? Br5 Zn3 2.4027(15) . ? Br5 Zn4 2.5023(14) . ? Br6 Zn3 2.4140(14) . ? Br6 Zn4 2.4818(15) . ? Br7 Zn4 2.2920(15) . ? Br8 Zn4 2.4022(14) . ? Br8 Zn5 2.4569(13) . ? Br9 Zn5 2.2988(14) . ? Br10 Zn5 2.4517(14) . ? Br10 Zn5 2.4524(16) 2_654 ? Zn1 O2 2.089(5) . ? Zn1 O1 2.122(6) . ? Zn1 O3 2.134(5) . ? Zn2 O5 2.071(5) . ? Zn2 O6 2.221(5) . ? Zn2 O4 2.249(6) . ? Zn5 Br10 2.4524(16) 2_654 ? O1 C12 1.427(10) . ? O1 C1 1.429(9) . ? O2 C2 1.424(11) . ? O2 C3 1.439(10) . ? O3 C4 1.435(9) . ? O3 C5 1.437(11) . ? O4 C6 1.438(9) . ? O4 C7 1.440(8) . ? O5 C9 1.412(11) . ? O5 C8 1.415(10) . ? O6 C11 1.423(11) . ? O6 C10 1.448(11) . ? C1 C2 1.491(13) . ? C3 C4 1.476(14) . ? C5 C6 1.464(13) . ? C7 C8 1.4478 . ? C9 C10 1.353(16) . ? C11 C12 1.504(12) . ? 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 Zn2 Br2 Zn1 87.82(4) . . ? Zn3 Br3 Zn2 84.03(5) . . ? Zn3 Br4 Zn2 83.92(4) . . ? Zn3 Br5 Zn4 81.60(4) . . ? Zn3 Br6 Zn4 81.80(4) . . ? Zn4 Br8 Zn5 94.67(5) . . ? Zn5 Br10 Zn5 83.96(5) . 2_654 ? O2 Zn1 O1 77.4(2) . . ? O2 Zn1 O3 77.1(2) . . ? O1 Zn1 O3 150.3(2) . . ? O2 Zn1 Br1 102.32(16) . . ? O1 Zn1 Br1 100.77(16) . . ? O3 Zn1 Br1 99.24(17) . . ? O2 Zn1 Br2 106.35(16) . . ? O1 Zn1 Br2 87.22(16) . . ? O3 Zn1 Br2 85.65(17) . . ? Br1 Zn1 Br2 151.28(5) . . ? O5 Zn2 O6 76.3(2) . . ? O5 Zn2 O4 75.9(2) . . ? O6 Zn2 O4 96.8(2) . . ? O5 Zn2 Br2 154.73(18) . . ? O6 Zn2 Br2 87.30(14) . . ? O4 Zn2 Br2 87.31(14) . . ? O5 Zn2 Br3 96.17(18) . . ? O6 Zn2 Br3 86.60(17) . . ? O4 Zn2 Br3 170.26(14) . . ? Br2 Zn2 Br3 102.01(5) . . ? O5 Zn2 Br4 95.87(16) . . ? O6 Zn2 Br4 170.61(14) . . ? O4 Zn2 Br4 86.20(16) . . ? Br2 Zn2 Br4 101.77(4) . . ? Br3 Zn2 Br4 89.11(4) . . ? Br4 Zn3 Br3 100.13(5) . . ? Br4 Zn3 Br5 116.15(5) . . ? Br3 Zn3 Br5 114.91(6) . . ? Br4 Zn3 Br6 113.77(6) . . ? Br3 Zn3 Br6 112.32(5) . . ? Br5 Zn3 Br6 100.22(5) . . ? Br7 Zn4 Br8 120.26(5) . . ? Br7 Zn4 Br6 112.27(5) . . ? Br8 Zn4 Br6 106.85(6) . . ? Br7 Zn4 Br5 113.92(6) . . ? Br8 Zn4 Br5 104.79(5) . . ? Br6 Zn4 Br5 95.71(5) . . ? Br9 Zn5 Br10 116.30(6) . . ? Br9 Zn5 Br10 118.62(5) . 2_654 ? Br10 Zn5 Br10 96.04(5) . 2_654 ? Br9 Zn5 Br8 111.99(5) . . ? Br10 Zn5 Br8 103.93(5) . . ? Br10 Zn5 Br8 108.04(5) 2_654 . ? C12 O1 C1 115.9(6) . . ? C12 O1 Zn1 120.8(5) . . ? C1 O1 Zn1 110.3(5) . . ? C2 O2 C3 117.2(6) . . ? C2 O2 Zn1 112.7(5) . . ? C3 O2 Zn1 112.5(5) . . ? C4 O3 C5 115.3(7) . . ? C4 O3 Zn1 110.2(5) . . ? C5 O3 Zn1 119.6(4) . . ? C6 O4 C7 116.3(6) . . ? C6 O4 Zn2 125.2(5) . . ? C7 O4 Zn2 112.5(4) . . ? C9 O5 C8 118.1(8) . . ? C9 O5 Zn2 114.2(5) . . ? C8 O5 Zn2 113.1(4) . . ? C11 O6 C10 115.3(8) . . ? C11 O6 Zn2 124.1(5) . . ? C10 O6 Zn2 111.6(5) . . ? O1 C1 C2 106.6(6) . . ? O2 C2 C1 105.9(7) . . ? O2 C3 C4 105.8(6) . . ? O3 C4 C3 106.2(7) . . ? O3 C5 C6 108.8(8) . . ? O4 C6 C5 113.1(7) . . ? O4 C7 C8 108.7(4) . . ? O5 C8 C7 113.3(4) . . ? C10 C9 O5 117.4(9) . . ? C9 C10 O6 113.5(9) . . ? O6 C11 C12 111.8(8) . . ? O1 C12 C11 108.0(6) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.159 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.194 _database_code_depnum_ccdc_archive 'CCDC 936451' ####################################################################### # # 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_Compound-5_[Zn5Br9(18c6)2][N(Tf)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H48 Br9 F6 N O16 S2 Zn5' _chemical_formula_weight 1854.81 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 16.130(3) _cell_length_b 10.592(2) _cell_length_c 15.477(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.88(3) _cell_angle_gamma 90.00 _cell_volume 2577.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 9.430 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1615 _exptl_absorpt_correction_T_max 0.4113 _exptl_absorpt_process_details '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18871 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.38 _reflns_number_total 9927 _reflns_number_gt 9123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'CELL, SELECT (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND, Crystal Impact' _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^)+(0.0713P)^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 constr _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(2) _refine_ls_number_reflns 9927 _refine_ls_number_parameters 631 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_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_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 Br1 Br 0.47259(6) -0.00264(8) 0.34571(7) 0.0432(2) Uani 1 1 d . . . Br2 Br 0.71118(5) 0.09559(6) 0.25022(5) 0.02793(16) Uani 1 1 d . . . Br3 Br 0.63555(6) 0.43356(8) 0.10887(6) 0.0419(2) Uani 1 1 d . . . Br4 Br 0.80498(5) 0.42353(8) 0.31225(5) 0.03451(18) Uani 1 1 d . . . Br5 Br 0.86517(6) 0.72867(7) 0.19432(5) 0.03686(19) Uani 1 1 d . . . Br6 Br 0.85631(5) 0.41374(8) 0.05799(5) 0.03520(19) Uani 1 1 d . . . Br7 Br 1.01904(5) 0.42303(7) 0.25768(5) 0.03104(17) Uani 1 1 d . . . Br8 Br 0.96885(6) 0.09180(7) 0.15094(5) 0.0375(2) Uani 1 1 d . . . Br9 Br 1.16321(6) 0.04634(8) -0.02209(7) 0.0439(2) Uani 1 1 d . . . Zn1 Zn 0.58946(6) -0.01394(8) 0.28269(7) 0.0325(2) Uani 1 1 d . . . Zn2 Zn 0.66140(6) 0.31326(8) 0.23699(5) 0.02624(18) Uani 1 1 d . . . Zn3 Zn 0.87378(6) 0.50898(7) 0.20318(6) 0.02704(18) Uani 1 1 d . . . Zn4 Zn 0.99670(6) 0.30659(7) 0.11286(6) 0.02549(18) Uani 1 1 d . . . Zn5 Zn 1.06850(7) 0.00506(8) 0.06735(7) 0.0354(2) Uani 1 1 d . . . S1 S 1.35600(13) -0.41868(19) 0.02398(14) 0.0333(4) Uani 1 1 d . D . S2 S 1.29614(13) -0.54133(18) -0.13617(13) 0.0307(4) Uani 1 1 d . . . F4 F 1.4444(4) -0.6471(7) -0.0984(5) 0.0647(18) Uani 1 1 d . . . F5 F 1.3423(5) -0.7721(5) -0.0948(4) 0.0597(17) Uani 1 1 d . . . F6 F 1.3621(5) -0.7105(7) -0.2199(4) 0.069(2) Uani 1 1 d . . . O1 O 0.5260(4) -0.0131(5) 0.1368(4) 0.0367(14) Uani 1 1 d . . . O2 O 0.5960(4) -0.1991(5) 0.2420(4) 0.0347(13) Uani 1 1 d . . . O3 O 0.6783(4) -0.1157(5) 0.3989(4) 0.0343(13) Uani 1 1 d . . . O4 O 0.6705(4) 0.1471(5) 0.4639(4) 0.0328(12) Uani 1 1 d . . . O5 O 0.6092(4) 0.3582(5) 0.3417(4) 0.0343(12) Uani 1 1 d . . . O6 O 0.5269(4) 0.2321(5) 0.2016(4) 0.0347(13) Uani 1 1 d . . . O7 O 0.9560(4) -0.0379(5) -0.0459(4) 0.0392(14) Uani 1 1 d . B . O11 O 1.0858(4) 0.4027(5) 0.0636(4) 0.0325(12) Uani 1 1 d . . . O12 O 0.9820(3) 0.2360(5) -0.0256(3) 0.0265(11) Uani 1 1 d . B . O13 O 1.3581(5) -0.4469(7) 0.1138(5) 0.0519(17) Uani 1 1 d . . . O14 O 1.4334(4) -0.3822(6) 0.0006(5) 0.0452(16) Uani 1 1 d . . . O15 O 1.3305(5) -0.4424(6) -0.1791(4) 0.0475(16) Uani 1 1 d . . . O16 O 1.2148(5) -0.5890(6) -0.1770(5) 0.0464(16) Uani 1 1 d . . . N1 N 1.3006(5) -0.5215(6) -0.0346(5) 0.0333(15) Uani 1 1 d . . . C1 C 0.5098(7) -0.1403(8) 0.1078(7) 0.049(2) Uani 1 1 d . . . H1A H 0.4999 -0.1447 0.0424 0.059 Uiso 1 1 calc R . . H1B H 0.4584 -0.1724 0.1256 0.059 Uiso 1 1 calc R . . C2 C 0.5838(8) -0.2169(9) 0.1484(6) 0.050(2) Uani 1 1 d . . . H2A H 0.5732 -0.3071 0.1329 0.060 Uiso 1 1 calc R . . H2B H 0.6347 -0.1889 0.1278 0.060 Uiso 1 1 calc R . . C3 C 0.6571(6) -0.2810(8) 0.2940(7) 0.046(2) Uani 1 1 d . . . H3A H 0.7137 -0.2681 0.2804 0.055 Uiso 1 1 calc R . . H3B H 0.6403 -0.3703 0.2823 0.055 Uiso 1 1 calc R . . C4 C 0.6595(7) -0.2470(7) 0.3894(6) 0.043(2) Uani 1 1 d . . . H4A H 0.6039 -0.2650 0.4038 0.052 Uiso 1 1 calc R . . H4B H 0.7038 -0.2967 0.4298 0.052 Uiso 1 1 calc R . . C5 C 0.6851(7) -0.0745(8) 0.4893(6) 0.041(2) Uani 1 1 d . . . H5A H 0.7183 -0.1367 0.5308 0.049 Uiso 1 1 calc R . . H5B H 0.6277 -0.0677 0.5019 0.049 Uiso 1 1 calc R . . C6 C 0.7284(6) 0.0514(8) 0.5017(5) 0.0361(19) Uani 1 1 d . . . H6A H 0.7499 0.0681 0.5657 0.043 Uiso 1 1 calc R . . H6B H 0.7775 0.0511 0.4730 0.043 Uiso 1 1 calc R . . C7 C 0.7156(6) 0.2615(8) 0.4640(6) 0.0371(19) Uani 1 1 d . . . H7A H 0.7559 0.2534 0.4245 0.044 Uiso 1 1 calc R . . H7B H 0.7488 0.2793 0.5246 0.044 Uiso 1 1 calc R . . C8 C 0.6556(7) 0.3686(8) 0.4330(5) 0.039(2) Uani 1 1 d . . . H8A H 0.6142 0.3734 0.4715 0.046 Uiso 1 1 calc R . . H8B H 0.6883 0.4484 0.4401 0.046 Uiso 1 1 calc R . . C9 C 0.5224(6) 0.3281(9) 0.3369(7) 0.041(2) Uani 1 1 d . . . H9A H 0.4958 0.3951 0.3662 0.049 Uiso 1 1 calc R . . H9B H 0.5185 0.2476 0.3682 0.049 Uiso 1 1 calc R . . C10 C 0.4765(6) 0.3164(10) 0.2426(7) 0.048(2) Uani 1 1 d . . . H10A H 0.4188 0.2812 0.2384 0.057 Uiso 1 1 calc R . . H10B H 0.4710 0.3999 0.2132 0.057 Uiso 1 1 calc R . . C11 C 0.4882(7) 0.2005(8) 0.1118(6) 0.044(2) Uani 1 1 d . . . H11A H 0.5302 0.2113 0.0744 0.053 Uiso 1 1 calc R . . H11B H 0.4401 0.2585 0.0894 0.053 Uiso 1 1 calc R . . C12 C 0.4570(6) 0.0693(8) 0.1046(7) 0.041(2) Uani 1 1 d . . . H12A H 0.4131 0.0587 0.1396 0.050 Uiso 1 1 calc R . . H12B H 0.4310 0.0492 0.0420 0.050 Uiso 1 1 calc R . . C13 C 0.9719(9) -0.1609(9) -0.0777(8) 0.060(3) Uani 1 1 d . . . H13A H 1.0215 -0.1585 -0.1055 0.073 Uiso 1 1 calc R B . H13B H 0.9217 -0.1907 -0.1223 0.073 Uiso 1 1 calc R . . C14 C 0.9888(9) -0.2451(9) -0.0004(9) 0.064(3) Uani 1 1 d . B . H14A H 0.9363 -0.2576 0.0217 0.077 Uiso 1 1 calc R . . H14B H 1.0083 -0.3285 -0.0168 0.077 Uiso 1 1 calc R . . C17 C 1.2051(8) 0.0232(13) 0.2477(8) 0.066(4) Uani 1 1 d . . . H17A H 1.1727 0.0632 0.2877 0.080 Uiso 1 1 calc R A 1 H17B H 1.2488 -0.0311 0.2850 0.080 Uiso 1 1 calc R A 1 C20 C 1.1686(5) 0.4205(7) 0.1209(6) 0.0357(19) Uani 1 1 d . . . H20A H 1.1619 0.4599 0.1770 0.043 Uiso 1 1 calc R B . H20B H 1.2020 0.4791 0.0922 0.043 Uiso 1 1 calc R . . C21 C 1.0926(6) 0.3805(8) -0.0267(5) 0.0348(18) Uani 1 1 d . . . H21A H 1.1369 0.3164 -0.0282 0.042 Uiso 1 1 calc R B . H21B H 1.1082 0.4595 -0.0533 0.042 Uiso 1 1 calc R . . C22 C 1.0082(6) 0.3347(8) -0.0770(5) 0.0359(19) Uani 1 1 d . B . H22A H 0.9663 0.4045 -0.0860 0.043 Uiso 1 1 calc R . . H22B H 1.0128 0.3022 -0.1357 0.043 Uiso 1 1 calc R . . C23 C 0.9063(5) 0.1733(8) -0.0734(5) 0.0325(17) Uani 1 1 d . . . H23A H 0.8746 0.2300 -0.1201 0.039 Uiso 1 1 calc R B . H23B H 0.8691 0.1529 -0.0324 0.039 Uiso 1 1 calc R . . C24 C 0.9296(6) 0.0547(8) -0.1147(6) 0.040(2) Uani 1 1 d . B . H24A H 0.8800 0.0229 -0.1591 0.048 Uiso 1 1 calc R . . H24B H 0.9764 0.0715 -0.1450 0.048 Uiso 1 1 calc R . . C25 C 1.2893(7) -0.2776(9) 0.0038(8) 0.050(2) Uani 1 1 d . . . C26 C 1.3669(7) -0.6770(9) -0.1383(6) 0.044(2) Uani 1 1 d . . . C181 C 1.2456(14) 0.114(2) 0.2162(13) 0.051(5) Uani 0.50 1 d P B 1 H18A H 1.2766 0.0792 0.1731 0.061 Uiso 0.50 1 calc PR B 1 H18B H 1.2872 0.1547 0.2649 0.061 Uiso 0.50 1 calc PR B 1 O101 O 1.1834(11) 0.2045(13) 0.1735(10) 0.037(3) Uani 0.50 1 d P B 1 C182 C 1.1713(14) 0.161(2) 0.2536(11) 0.046(5) Uani 0.50 1 d P B 2 H18C H 1.1243 0.1580 0.2852 0.056 Uiso 0.50 1 calc PR B 2 H18D H 1.2176 0.2119 0.2903 0.056 Uiso 0.50 1 calc PR B 2 O102 O 1.1419(10) 0.2248(13) 0.1731(9) 0.030(3) Uani 0.50 1 d P B 2 C19 C 1.2160(7) 0.3003(9) 0.1413(7) 0.048(2) Uani 1 1 d . B . H19A H 1.2308 0.2716 0.0857 0.058 Uiso 1 1 calc R C 1 H19B H 1.2702 0.3205 0.1833 0.058 Uiso 1 1 calc R C 1 O9 O 1.1484(6) -0.0572(7) 0.1905(6) 0.063(2) Uani 1 1 d . B . O8 O 1.0528(6) -0.1882(6) 0.0664(6) 0.061(2) Uani 1 1 d . B . C15 C 1.0897(9) -0.2531(11) 0.1455(11) 0.078(4) Uani 1 1 d . . . H15A H 1.1107 -0.3364 0.1307 0.093 Uiso 1 1 calc R B 1 H15B H 1.0459 -0.2676 0.1803 0.093 Uiso 1 1 calc R B 1 C161 C 1.1618(18) -0.180(2) 0.2002(17) 0.060(6) Uiso 0.50 1 d P B 1 H16A H 1.1685 -0.2023 0.2635 0.072 Uiso 0.50 1 calc PR B 1 H16B H 1.2152 -0.2017 0.1823 0.072 Uiso 0.50 1 calc PR B 1 C162 C 1.1153(17) -0.175(2) 0.2120(15) 0.052(5) Uiso 0.50 1 d P B 2 H16C H 1.1598 -0.2180 0.2569 0.063 Uiso 0.50 1 calc PR B 2 H16D H 1.0668 -0.1581 0.2398 0.063 Uiso 0.50 1 calc PR B 2 F31 F 1.312(2) -0.210(3) 0.079(2) 0.091(12) Uani 0.50 1 d P D 1 F41 F 1.211(2) -0.308(3) -0.0217(17) 0.062(8) Uani 0.50 1 d P D 1 F21 F 1.3161(12) -0.2076(19) -0.0540(16) 0.061(5) Uani 0.50 1 d P D 1 F42 F 1.210(2) -0.303(3) 0.0122(19) 0.062(7) Uani 0.50 1 d P D 2 F32 F 1.3076(14) -0.190(3) 0.059(2) 0.082(11) Uani 0.50 1 d P D 2 F22 F 1.2760(19) -0.236(2) -0.0797(18) 0.101(9) Uani 0.50 1 d P D 2 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 Br1 0.0365(4) 0.0411(4) 0.0566(5) 0.0059(4) 0.0205(4) -0.0010(4) Br2 0.0258(3) 0.0223(3) 0.0362(4) 0.0020(3) 0.0078(3) 0.0024(3) Br3 0.0524(5) 0.0400(4) 0.0350(4) 0.0151(3) 0.0131(4) 0.0046(4) Br4 0.0309(4) 0.0403(4) 0.0338(4) 0.0034(3) 0.0104(3) -0.0100(3) Br5 0.0532(5) 0.0243(3) 0.0308(4) 0.0010(3) 0.0043(3) 0.0024(3) Br6 0.0304(4) 0.0442(4) 0.0282(4) -0.0097(3) 0.0005(3) 0.0103(3) Br7 0.0249(4) 0.0388(4) 0.0286(3) -0.0088(3) 0.0042(3) 0.0030(3) Br8 0.0597(5) 0.0250(3) 0.0337(4) 0.0047(3) 0.0232(4) 0.0034(3) Br9 0.0466(5) 0.0355(4) 0.0585(5) 0.0015(4) 0.0308(5) 0.0029(4) Zn1 0.0348(5) 0.0233(4) 0.0422(5) -0.0019(4) 0.0146(4) -0.0020(4) Zn2 0.0320(5) 0.0226(4) 0.0269(4) 0.0027(3) 0.0123(4) 0.0032(3) Zn3 0.0308(4) 0.0242(4) 0.0279(4) -0.0007(3) 0.0104(4) 0.0012(3) Zn4 0.0279(4) 0.0229(4) 0.0280(4) -0.0022(3) 0.0113(4) -0.0019(3) Zn5 0.0460(6) 0.0241(4) 0.0404(5) 0.0062(3) 0.0192(5) 0.0044(4) S1 0.0282(10) 0.0344(9) 0.0388(10) -0.0049(8) 0.0102(9) -0.0036(8) S2 0.0264(9) 0.0316(9) 0.0328(9) 0.0003(7) 0.0040(8) 0.0019(7) F4 0.035(3) 0.073(4) 0.085(5) -0.002(3) 0.010(3) 0.020(3) F5 0.084(5) 0.038(3) 0.060(4) 0.007(3) 0.022(4) 0.014(3) F6 0.098(5) 0.071(4) 0.043(3) -0.007(3) 0.027(4) 0.033(4) O1 0.039(3) 0.030(3) 0.035(3) -0.009(2) -0.003(3) -0.005(2) O2 0.038(3) 0.028(3) 0.040(3) -0.004(2) 0.015(3) 0.003(2) O3 0.044(3) 0.025(3) 0.032(3) 0.003(2) 0.004(3) -0.004(2) O4 0.035(3) 0.031(3) 0.033(3) 0.001(2) 0.009(2) -0.006(2) O5 0.035(3) 0.037(3) 0.032(3) -0.008(2) 0.011(3) -0.002(2) O6 0.033(3) 0.035(3) 0.035(3) -0.003(2) 0.006(3) 0.007(2) O7 0.056(4) 0.024(3) 0.043(3) -0.009(2) 0.021(3) -0.012(3) O11 0.026(3) 0.036(3) 0.036(3) -0.004(2) 0.006(2) -0.007(2) O12 0.029(3) 0.029(2) 0.021(2) -0.0021(19) 0.004(2) -0.007(2) O13 0.055(4) 0.063(4) 0.039(3) -0.008(3) 0.012(3) -0.004(3) O14 0.032(3) 0.050(4) 0.058(4) -0.019(3) 0.018(3) -0.016(3) O15 0.062(4) 0.044(3) 0.037(3) 0.012(3) 0.011(3) -0.006(3) O16 0.040(4) 0.044(3) 0.051(4) -0.008(3) 0.003(3) -0.005(3) N1 0.027(3) 0.035(3) 0.039(4) -0.005(3) 0.010(3) -0.009(3) C1 0.068(7) 0.029(4) 0.047(5) -0.014(4) 0.009(5) -0.008(4) C2 0.069(7) 0.040(5) 0.041(5) -0.015(4) 0.010(5) 0.004(5) C3 0.043(5) 0.025(4) 0.063(6) -0.002(4) -0.002(5) 0.012(3) C4 0.051(5) 0.023(4) 0.048(5) 0.011(3) -0.003(4) 0.000(3) C5 0.049(5) 0.037(4) 0.037(4) 0.007(3) 0.011(4) 0.003(4) C6 0.042(5) 0.039(4) 0.025(4) -0.002(3) 0.001(4) 0.004(4) C7 0.041(5) 0.037(4) 0.034(4) 0.000(3) 0.007(4) -0.014(3) C8 0.055(6) 0.042(4) 0.018(3) -0.005(3) 0.008(4) -0.005(4) C9 0.036(4) 0.038(4) 0.054(5) -0.017(4) 0.022(4) -0.003(4) C10 0.029(4) 0.050(5) 0.065(6) -0.009(4) 0.010(4) 0.010(4) C11 0.052(6) 0.036(4) 0.038(5) 0.003(4) -0.003(4) 0.002(4) C12 0.036(5) 0.036(4) 0.046(5) -0.003(4) -0.004(4) 0.002(4) C13 0.085(8) 0.034(5) 0.077(7) -0.028(5) 0.048(7) -0.017(5) C14 0.083(9) 0.027(4) 0.098(9) -0.009(5) 0.054(8) -0.012(5) C17 0.062(7) 0.083(8) 0.046(6) 0.017(6) -0.006(5) 0.037(7) C20 0.027(4) 0.032(4) 0.048(5) -0.007(3) 0.010(4) -0.011(3) C21 0.039(5) 0.037(4) 0.032(4) 0.003(3) 0.016(4) -0.011(3) C22 0.040(5) 0.041(4) 0.027(4) 0.012(3) 0.010(4) 0.000(4) C23 0.028(4) 0.038(4) 0.030(4) -0.001(3) 0.002(3) -0.006(3) C24 0.045(5) 0.038(4) 0.035(4) -0.009(3) 0.006(4) -0.014(4) C25 0.050(6) 0.041(5) 0.061(6) 0.001(4) 0.018(5) 0.009(4) C26 0.047(5) 0.045(5) 0.040(5) -0.002(4) 0.008(4) 0.008(4) C181 0.046(11) 0.074(13) 0.032(9) 0.023(9) 0.005(9) 0.018(10) O101 0.039(8) 0.032(7) 0.042(7) 0.007(5) 0.010(8) 0.006(6) C182 0.055(12) 0.061(11) 0.021(7) 0.003(7) 0.006(8) 0.010(9) O102 0.030(7) 0.039(7) 0.023(6) 0.003(5) 0.009(6) 0.015(6) C19 0.056(6) 0.039(5) 0.046(5) -0.008(4) 0.002(5) 0.000(4) O9 0.070(5) 0.054(4) 0.063(5) 0.041(4) 0.006(4) 0.005(4) O8 0.091(6) 0.021(3) 0.080(5) 0.010(3) 0.043(5) 0.002(3) C15 0.072(8) 0.051(6) 0.124(12) 0.055(7) 0.050(8) 0.017(6) F31 0.15(3) 0.064(14) 0.053(9) -0.016(8) 0.019(12) 0.050(13) F41 0.036(10) 0.061(10) 0.079(17) -0.017(13) -0.008(13) 0.019(7) F21 0.063(11) 0.042(7) 0.077(12) 0.019(7) 0.015(8) 0.003(7) F42 0.047(11) 0.053(9) 0.10(2) -0.022(14) 0.034(15) -0.001(7) F32 0.041(9) 0.044(11) 0.14(3) -0.056(15) -0.015(12) 0.013(7) F22 0.14(2) 0.084(17) 0.099(19) 0.028(13) 0.069(19) 0.071(17) _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 Br1 Zn1 2.3106(15) . ? Br2 Zn1 2.4276(13) . ? Br2 Zn2 2.4350(11) . ? Br3 Zn2 2.3153(12) . ? Br4 Zn3 2.3949(14) . ? Br4 Zn2 2.6233(13) . ? Br5 Zn3 2.3333(11) . ? Br6 Zn3 2.4215(12) . ? Br6 Zn4 2.5059(13) . ? Br7 Zn3 2.4797(13) . ? Br7 Zn4 2.5129(12) . ? Br8 Zn4 2.4173(12) . ? Br8 Zn5 2.4552(15) . ? Br9 Zn5 2.3204(16) . ? Zn1 O2 2.069(5) . ? Zn1 O1 2.262(6) . ? Zn1 O3 2.302(5) . ? Zn2 O5 2.042(6) . ? Zn2 O6 2.284(6) . ? Zn4 O11 2.043(6) . ? Zn4 O12 2.233(5) . ? Zn4 O102 2.476(14) . ? Zn5 O8 2.063(6) . ? Zn5 O9 2.153(7) . ? Zn5 O7 2.270(6) . ? S1 O13 1.415(8) . ? S1 O14 1.428(7) . ? S1 N1 1.564(7) . ? S1 C25 1.827(10) . ? S2 O16 1.417(7) . ? S2 O15 1.418(7) . ? S2 N1 1.571(8) . ? S2 C26 1.841(10) . ? F4 C26 1.304(12) . ? F5 C26 1.322(12) . ? F6 C26 1.297(11) . ? O1 C12 1.415(10) . ? O1 C1 1.426(10) . ? O2 C3 1.421(10) . ? O2 C2 1.431(11) . ? O3 C4 1.424(9) . ? O3 C5 1.447(11) . ? O4 C7 1.413(9) . ? O4 C6 1.413(10) . ? O5 C9 1.422(11) . ? O5 C8 1.449(9) . ? O6 C11 1.431(10) . ? O6 C10 1.447(11) . ? O7 C13 1.435(11) . ? O7 C24 1.441(11) . ? O11 C20 1.442(9) . ? O11 C21 1.444(10) . ? O12 C22 1.433(9) . ? O12 C23 1.440(9) . ? C1 C2 1.464(15) . ? C3 C4 1.512(15) . ? C5 C6 1.497(12) . ? C7 C8 1.499(13) . ? C9 C10 1.486(14) . ? C11 C12 1.473(12) . ? C13 C14 1.469(18) . ? C14 O8 1.422(16) . ? C17 C181 1.32(3) . ? C17 O9 1.408(16) . ? C17 C182 1.57(2) . ? C20 C19 1.482(12) . ? C21 C22 1.490(12) . ? C23 C24 1.494(12) . ? C25 F32 1.25(3) . ? C25 F41 1.28(4) . ? C25 F21 1.31(3) . ? C25 F42 1.35(4) . ? C25 F22 1.34(3) . ? C25 F31 1.35(3) . ? C181 O101 1.44(2) . ? O101 C19 1.292(18) . ? C182 O102 1.40(2) . ? O102 C19 1.60(2) . ? O9 C161 1.32(2) . ? O9 C162 1.43(2) . ? O8 C15 1.415(15) . ? C15 C162 1.31(3) . ? C15 C161 1.50(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 Zn1 Br2 Zn2 101.72(4) . . ? Zn3 Br4 Zn2 110.93(5) . . ? Zn3 Br6 Zn4 87.99(4) . . ? Zn3 Br7 Zn4 86.56(4) . . ? Zn4 Br8 Zn5 92.56(4) . . ? O2 Zn1 O1 75.1(2) . . ? O2 Zn1 O3 74.3(2) . . ? O1 Zn1 O3 147.8(2) . . ? O2 Zn1 Br1 106.19(18) . . ? O1 Zn1 Br1 101.01(18) . . ? O3 Zn1 Br1 96.82(17) . . ? O2 Zn1 Br2 106.97(18) . . ? O1 Zn1 Br2 89.91(17) . . ? O3 Zn1 Br2 89.68(16) . . ? Br1 Zn1 Br2 146.74(5) . . ? O5 Zn2 O6 74.9(2) . . ? O5 Zn2 Br3 121.59(17) . . ? O6 Zn2 Br3 91.25(15) . . ? O5 Zn2 Br2 109.91(17) . . ? O6 Zn2 Br2 86.64(14) . . ? Br3 Zn2 Br2 125.89(5) . . ? O5 Zn2 Br4 91.35(16) . . ? O6 Zn2 Br4 166.29(16) . . ? Br3 Zn2 Br4 96.19(5) . . ? Br2 Zn2 Br4 98.18(4) . . ? Br5 Zn3 Br4 112.80(5) . . ? Br5 Zn3 Br6 111.58(5) . . ? Br4 Zn3 Br6 121.35(5) . . ? Br5 Zn3 Br7 115.18(5) . . ? Br4 Zn3 Br7 99.94(5) . . ? Br6 Zn3 Br7 93.92(5) . . ? O11 Zn4 O12 75.0(2) . . ? O11 Zn4 Br8 138.13(17) . . ? O12 Zn4 Br8 86.16(13) . . ? O11 Zn4 O102 68.3(4) . . ? O12 Zn4 O102 97.6(3) . . ? Br8 Zn4 O102 77.9(3) . . ? O11 Zn4 Br6 107.79(16) . . ? O12 Zn4 Br6 86.10(14) . . ? Br8 Zn4 Br6 107.81(5) . . ? O102 Zn4 Br6 173.4(3) . . ? O11 Zn4 Br7 96.63(16) . . ? O12 Zn4 Br7 169.83(14) . . ? Br8 Zn4 Br7 104.00(4) . . ? O102 Zn4 Br7 84.3(3) . . ? Br6 Zn4 Br7 91.09(4) . . ? O8 Zn5 O9 75.5(3) . . ? O8 Zn5 O7 73.7(3) . . ? O9 Zn5 O7 147.1(3) . . ? O8 Zn5 Br9 106.2(2) . . ? O9 Zn5 Br9 104.0(3) . . ? O7 Zn5 Br9 95.52(18) . . ? O8 Zn5 Br8 106.3(2) . . ? O9 Zn5 Br8 88.9(3) . . ? O7 Zn5 Br8 88.72(18) . . ? Br9 Zn5 Br8 147.06(5) . . ? O13 S1 O14 118.4(5) . . ? O13 S1 N1 107.9(4) . . ? O14 S1 N1 117.4(4) . . ? O13 S1 C25 103.0(5) . . ? O14 S1 C25 104.5(5) . . ? N1 S1 C25 103.4(5) . . ? O16 S2 O15 118.3(4) . . ? O16 S2 N1 109.0(4) . . ? O15 S2 N1 115.8(4) . . ? O16 S2 C26 103.3(4) . . ? O15 S2 C26 105.0(5) . . ? N1 S2 C26 103.4(4) . . ? C12 O1 C1 113.4(7) . . ? C12 O1 Zn1 120.0(5) . . ? C1 O1 Zn1 108.8(5) . . ? C3 O2 C2 114.5(7) . . ? C3 O2 Zn1 118.8(5) . . ? C2 O2 Zn1 115.4(5) . . ? C4 O3 C5 111.3(6) . . ? C4 O3 Zn1 107.2(4) . . ? C5 O3 Zn1 120.9(5) . . ? C7 O4 C6 108.9(6) . . ? C9 O5 C8 110.9(7) . . ? C9 O5 Zn2 118.8(5) . . ? C8 O5 Zn2 125.2(6) . . ? C11 O6 C10 113.8(7) . . ? C11 O6 Zn2 120.4(6) . . ? C10 O6 Zn2 105.0(5) . . ? C13 O7 C24 114.2(8) . . ? C13 O7 Zn5 105.9(7) . . ? C24 O7 Zn5 119.2(5) . . ? C20 O11 C21 110.9(7) . . ? C20 O11 Zn4 117.9(5) . . ? C21 O11 Zn4 119.4(4) . . ? C22 O12 C23 111.9(6) . . ? C22 O12 Zn4 107.8(4) . . ? C23 O12 Zn4 122.9(5) . . ? S1 N1 S2 124.5(5) . . ? O1 C1 C2 108.3(8) . . ? O2 C2 C1 106.0(8) . . ? O2 C3 C4 105.7(7) . . ? O3 C4 C3 106.9(7) . . ? O3 C5 C6 109.0(7) . . ? O4 C6 C5 109.9(7) . . ? O4 C7 C8 110.7(7) . . ? O5 C8 C7 114.3(7) . . ? O5 C9 C10 109.8(8) . . ? O6 C10 C9 106.0(7) . . ? O6 C11 C12 111.2(8) . . ? O1 C12 C11 109.1(7) . . ? O7 C13 C14 106.6(9) . . ? O8 C14 C13 107.9(8) . . ? C181 C17 O9 121.0(13) . . ? C181 C17 C182 63.2(14) . . ? O9 C17 C182 114.5(11) . . ? O11 C20 C19 112.4(7) . . ? O11 C21 C22 107.5(7) . . ? O12 C22 C21 107.2(6) . . ? O12 C23 C24 110.0(7) . . ? O7 C24 C23 108.5(7) . . ? F32 C25 F41 117.5(19) . . ? F32 C25 F21 89(2) . . ? F41 C25 F21 112.7(19) . . ? F32 C25 F42 99.5(19) . . ? F41 C25 F42 23.2(17) . . ? F21 C25 F42 130.3(19) . . ? F32 C25 F22 112(2) . . ? F41 C25 F22 81(2) . . ? F21 C25 F22 32.7(14) . . ? F42 C25 F22 102(2) . . ? F32 C25 F31 16(3) . . ? F41 C25 F31 117(2) . . ? F21 C25 F31 103(2) . . ? F42 C25 F31 96(2) . . ? F22 C25 F31 128(2) . . ? F32 C25 S1 116.6(16) . . ? F41 C25 S1 110.7(17) . . ? F21 C25 S1 108.0(12) . . ? F42 C25 S1 111.1(17) . . ? F22 C25 S1 113.3(12) . . ? F31 C25 S1 104.7(16) . . ? F6 C26 F4 111.8(10) . . ? F6 C26 F5 109.2(8) . . ? F4 C26 F5 108.0(8) . . ? F6 C26 S2 109.2(6) . . ? F4 C26 S2 109.5(7) . . ? F5 C26 S2 109.1(8) . . ? C17 C181 O101 107.8(17) . . ? C19 O101 C181 113.5(16) . . ? O102 C182 C17 116.6(14) . . ? C182 O102 C19 112.6(14) . . ? C182 O102 Zn4 127.3(13) . . ? C19 O102 Zn4 114.7(8) . . ? O101 C19 C20 121.4(12) . . ? O101 C19 O102 25.2(7) . . ? C20 C19 O102 96.3(9) . . ? C161 O9 C17 117.2(13) . . ? C161 O9 C162 34.1(13) . . ? C17 O9 C162 127.4(11) . . ? C161 O9 Zn5 117.0(12) . . ? C17 O9 Zn5 123.2(6) . . ? C162 O9 Zn5 107.1(10) . . ? C15 O8 C14 121.4(9) . . ? C15 O8 Zn5 116.7(8) . . ? C14 O8 Zn5 119.6(6) . . ? C162 C15 O8 111.8(12) . . ? C162 C15 C161 32.8(14) . . ? O8 C15 C161 111.2(12) . . ? O9 C161 C15 111.1(18) . . ? C15 C162 O9 115.8(19) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.883 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 936452'