# 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_k07alj10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H84 N4 Si4 Zn4' _chemical_formula_weight 1511.38 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 26.2840(3) _cell_length_b 9.4770(2) _cell_length_c 32.3190(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.2770(10) _cell_angle_gamma 90.00 _cell_volume 7551.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37195 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.365 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37195 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.49 _reflns_number_total 15356 _reflns_number_gt 12241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0655P)^2^+9.0879P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 15356 _refine_ls_number_parameters 861 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Zn1 Zn -0.42684(2) -0.96651(6) -0.219354(18) 0.02965(14) Uani 1 1 d . . . Zn3 Zn -0.38974(2) -0.99516(6) 0.027927(18) 0.02841(14) Uani 1 1 d . . . Zn2 Zn -0.41155(2) -0.68107(6) -0.189941(17) 0.02873(14) Uani 1 1 d . . . Zn4 Zn -0.40874(2) -1.27389(6) -0.005928(18) 0.02870(14) Uani 1 1 d . . . Si3 Si -0.28392(6) -1.19509(15) 0.03367(4) 0.0250(3) Uani 1 1 d . . . Si2 Si -0.31650(6) -0.80281(15) -0.22608(5) 0.0250(3) Uani 1 1 d . . . Si4 Si -0.50642(6) -1.15554(15) 0.02629(4) 0.0240(3) Uani 1 1 d . . . Si1 Si -0.53199(6) -0.78923(15) -0.22549(4) 0.0243(3) Uani 1 1 d . . . N3 N -0.34775(17) -1.1324(4) 0.00383(12) 0.0254(9) Uani 1 1 d . . . H3 H -0.3479 -1.1000 -0.0234 0.031 Uiso 1 1 calc R . . N1 N -0.46666(16) -0.8347(4) -0.19236(12) 0.0222(8) Uani 1 1 d . . . H1 H -0.4649 -0.8637 -0.1644 0.027 Uiso 1 1 calc R . . N2 N -0.38384(18) -0.7996(4) -0.23029(15) 0.0279(9) Uani 1 1 d . . . H2 H -0.4030 -0.7690 -0.2588 0.034 Uiso 1 1 calc R . . N4 N -0.43814(17) -1.1565(4) 0.03401(14) 0.0271(9) Uani 1 1 d . . . H4 H -0.4212 -1.1922 0.0623 0.033 Uiso 1 1 calc R . . C401 C -0.5448(2) -1.0723(6) -0.02859(16) 0.0286(11) Uani 1 1 d . . . C413 C -0.5214(2) -1.0447(5) 0.06948(15) 0.0239(10) Uani 1 1 d . . . C307 C -0.2543(2) -1.2942(5) -0.00317(17) 0.0290(12) Uani 1 1 d . . . C412 C -0.5860(2) -1.3722(6) 0.01738(17) 0.0336(12) Uani 1 1 d . . . H412 H -0.6122 -1.3008 0.0049 0.040 Uiso 1 1 calc R . . C106 C -0.5146(2) -0.7623(6) -0.30816(17) 0.0337(12) Uani 1 1 d . . . H106 H -0.5205 -0.8613 -0.3109 0.040 Uiso 1 1 calc R . . C207 C -0.2904(2) -0.6208(5) -0.22908(15) 0.0265(11) Uani 1 1 d . . . C3 C -0.3877(3) -0.7944(6) 0.04104(19) 0.0384(14) Uani 1 1 d . . . H3A H -0.3529 -0.7550 0.0418 0.058 Uiso 1 1 calc R . . H3B H -0.3919 -0.7806 0.0698 0.058 Uiso 1 1 calc R . . H3C H -0.4173 -0.7465 0.0181 0.058 Uiso 1 1 calc R . . C301 C -0.2918(2) -1.3195(5) 0.07627(16) 0.0292(12) Uani 1 1 d . . . C408 C -0.4942(2) -1.4499(6) 0.04604(16) 0.0291(11) Uani 1 1 d . . . H408 H -0.4564 -1.4322 0.0542 0.035 Uiso 1 1 calc R . . C201 C -0.2749(2) -0.8888(6) -0.17224(16) 0.0282(11) Uani 1 1 d . . . C312 C -0.1982(2) -1.3095(6) 0.00872(19) 0.0366(13) Uani 1 1 d . . . H312 H -0.1751 -1.2676 0.0353 0.044 Uiso 1 1 calc R . . C113 C -0.5757(2) -0.9491(6) -0.24742(17) 0.0312(12) Uani 1 1 d . . . C313 C -0.2352(2) -1.0507(6) 0.06221(18) 0.0336(12) Uani 1 1 d . . . C211 C -0.2161(3) -0.4572(6) -0.22304(18) 0.0375(13) Uani 1 1 d . . . H211 H -0.1784 -0.4394 -0.2152 0.045 Uiso 1 1 calc R . . C407 C -0.5310(2) -1.3393(5) 0.02921(15) 0.0263(11) Uani 1 1 d . . . C28 C -0.3475(2) -0.9958(6) -0.29971(17) 0.0354(13) Uani 1 1 d . . . H28 H -0.3827 -0.9945 -0.2978 0.043 Uiso 1 1 calc R . . C101 C -0.5223(2) -0.6909(5) -0.27264(16) 0.0279(11) Uani 1 1 d . . . C202 C -0.2730(3) -1.0343(7) -0.16901(19) 0.0379(14) Uani 1 1 d . . . H202 H -0.2932 -1.0886 -0.1940 0.045 Uiso 1 1 calc R . . C212 C -0.2345(2) -0.5910(6) -0.21814(17) 0.0346(12) Uani 1 1 d . . . H212 H -0.2089 -0.6648 -0.2071 0.042 Uiso 1 1 calc R . . C107 C -0.5644(2) -0.6700(6) -0.19558(17) 0.0291(11) Uani 1 1 d . . . C309 C -0.2638(3) -1.4322(7) -0.0689(2) 0.0459(15) Uani 1 1 d . . . H309 H -0.2868 -1.4739 -0.0956 0.055 Uiso 1 1 calc R . . C6S C -0.3560(3) -0.9836(7) -0.10065(19) 0.0405(15) Uani 1 1 d . . . H6S H -0.3215 -0.9726 -0.1036 0.049 Uiso 1 1 calc R . . C410 C -0.5660(3) -1.6136(6) 0.03979(17) 0.0362(13) Uani 1 1 d . . . H410 H -0.5777 -1.7063 0.0433 0.043 Uiso 1 1 calc R . . C403 C -0.6009(3) -1.0798(8) -0.10613(19) 0.0512(18) Uani 1 1 d . . . H403 H -0.6208 -1.1332 -0.1315 0.061 Uiso 1 1 calc R . . C402 C -0.5737(2) -1.1504(7) -0.06600(18) 0.0369(13) Uani 1 1 d . . . H402 H -0.5750 -1.2504 -0.0645 0.044 Uiso 1 1 calc R . . C311 C -0.1752(2) -1.3852(7) -0.01770(19) 0.0427(15) Uani 1 1 d . . . H311 H -0.1369 -1.3938 -0.0091 0.051 Uiso 1 1 calc R . . C409 C -0.5117(3) -1.5836(6) 0.05102(17) 0.0347(13) Uani 1 1 d . . . H409 H -0.4858 -1.6565 0.0624 0.042 Uiso 1 1 calc R . . C303 C -0.3154(3) -1.3668(8) 0.14096(19) 0.0545(19) Uani 1 1 d . . . H303 H -0.3279 -1.3334 0.1635 0.065 Uiso 1 1 calc R . . C209 C -0.3079(3) -0.3746(6) -0.25039(19) 0.0396(14) Uani 1 1 d . . . H209 H -0.3332 -0.3001 -0.2615 0.047 Uiso 1 1 calc R . . C302 C -0.3098(3) -1.2728(7) 0.1094(2) 0.0452(15) Uani 1 1 d . . . H302 H -0.3183 -1.1759 0.1108 0.054 Uiso 1 1 calc R . . C417 C -0.5848(3) -0.9654(7) 0.1039(2) 0.0435(15) Uani 1 1 d . . . H417 H -0.6204 -0.9670 0.1051 0.052 Uiso 1 1 calc R . . C414 C -0.4823(2) -0.9622(6) 0.09940(16) 0.0325(12) Uani 1 1 d . . . H414 H -0.4467 -0.9604 0.0982 0.039 Uiso 1 1 calc R . . C418 C -0.5729(2) -1.0437(6) 0.07265(18) 0.0364(13) Uani 1 1 d . . . H418 H -0.6007 -1.0991 0.0525 0.044 Uiso 1 1 calc R . . C102 C -0.5144(3) -0.5464(6) -0.27068(17) 0.0358(13) Uani 1 1 d . . . H102 H -0.5198 -0.4943 -0.2474 0.043 Uiso 1 1 calc R . . C214 C -0.3373(3) -1.0805(6) -0.33144(18) 0.0430(14) Uani 1 1 d . . . H214 H -0.3656 -1.1375 -0.3504 0.052 Uiso 1 1 calc R . . C5S C -0.3846(3) -1.1050(7) -0.11581(19) 0.0469(16) Uani 1 1 d . . . H5S H -0.3697 -1.1769 -0.1287 0.056 Uiso 1 1 calc R . . C1 C -0.4322(3) -1.1625(6) -0.2366(2) 0.0476(17) Uani 1 1 d . . . H1A H -0.4431 -1.1691 -0.2688 0.071 Uiso 1 1 calc R . . H1B H -0.4594 -1.2095 -0.2269 0.071 Uiso 1 1 calc R . . H1C H -0.3970 -1.2084 -0.2229 0.071 Uiso 1 1 calc R . . C213 C -0.3064(2) -0.9131(6) -0.27079(16) 0.0296(11) Uani 1 1 d . . . C310 C -0.2082(3) -1.4468(7) -0.05595(19) 0.0427(14) Uani 1 1 d . . . H310 H -0.1927 -1.4996 -0.0736 0.051 Uiso 1 1 calc R . . C208 C -0.3264(3) -0.5088(6) -0.24519(18) 0.0336(12) Uani 1 1 d . . . H208 H -0.3642 -0.5246 -0.2527 0.040 Uiso 1 1 calc R . . C2S C -0.4264(3) -0.8942(8) -0.07755(19) 0.0466(17) Uani 1 1 d . . . H2S H -0.4410 -0.8227 -0.0643 0.056 Uiso 1 1 calc R . . C411 C -0.6033(3) -1.5067(6) 0.02339(19) 0.0407(14) Uani 1 1 d . . . H411 H -0.6409 -1.5253 0.0162 0.049 Uiso 1 1 calc R . . C108 C -0.5343(3) -0.5989(7) -0.1574(2) 0.0448(15) Uani 1 1 d . . . H108 H -0.4960 -0.6110 -0.1457 0.054 Uiso 1 1 calc R . . C2 C -0.3956(3) -0.4968(6) -0.1623(2) 0.0459(16) Uani 1 1 d . . . H2A H -0.4236 -0.4295 -0.1787 0.069 Uiso 1 1 calc R . . H2B H -0.3601 -0.4647 -0.1622 0.069 Uiso 1 1 calc R . . H2C H -0.3950 -0.5032 -0.1318 0.069 Uiso 1 1 calc R . . C105 C -0.4987(3) -0.6923(8) -0.3391(2) 0.0548(19) Uani 1 1 d . . . H105 H -0.4933 -0.7435 -0.3625 0.066 Uiso 1 1 calc R . . C1S C -0.3756(3) -0.8752(7) -0.08102(18) 0.0440(15) Uani 1 1 d . . . C316 C -0.1601(3) -0.8383(9) 0.1008(3) 0.067(2) Uani 1 1 d . . . H316 H -0.1345 -0.7660 0.1138 0.081 Uiso 1 1 calc R . . C4 C -0.4311(3) -1.4522(7) -0.0373(2) 0.0478(16) Uani 1 1 d . . . H4A H -0.4368 -1.4386 -0.0686 0.072 Uiso 1 1 calc R . . H4B H -0.4649 -1.4843 -0.0340 0.072 Uiso 1 1 calc R . . H4C H -0.4027 -1.5231 -0.0249 0.072 Uiso 1 1 calc R . . C103 C -0.4989(3) -0.4759(7) -0.30215(19) 0.0534(18) Uani 1 1 d . . . H103 H -0.4939 -0.3766 -0.3003 0.064 Uiso 1 1 calc R . . C406 C -0.5443(2) -0.9257(6) -0.03271(18) 0.0366(13) Uani 1 1 d . . . H406 H -0.5249 -0.8706 -0.0076 0.044 Uiso 1 1 calc R . . C114 C -0.5653(3) -1.0737(7) -0.2230(2) 0.0482(16) Uani 1 1 d . . . H114 H -0.5371 -1.0760 -0.1950 0.058 Uiso 1 1 calc R . . C304 C -0.3030(3) -1.5059(8) 0.1396(2) 0.059(2) Uani 1 1 d . . . H304 H -0.3074 -1.5697 0.1608 0.071 Uiso 1 1 calc R . . C405 C -0.5712(3) -0.8581(7) -0.0724(2) 0.0455(15) Uani 1 1 d . . . H405 H -0.5704 -0.7582 -0.0742 0.055 Uiso 1 1 calc R . . C404 C -0.5993(3) -0.9369(8) -0.1092(2) 0.0520(18) Uani 1 1 d . . . H404 H -0.6174 -0.8913 -0.1365 0.062 Uiso 1 1 calc R . . C112 C -0.6204(2) -0.6488(7) -0.2111(2) 0.0426(14) Uani 1 1 d . . . H112 H -0.6422 -0.6962 -0.2371 0.051 Uiso 1 1 calc R . . C318 C -0.1920(3) -1.0748(8) 0.10112(19) 0.0476(16) Uani 1 1 d . . . H318 H -0.1881 -1.1646 0.1150 0.057 Uiso 1 1 calc R . . C210 C -0.2534(3) -0.3497(7) -0.23952(19) 0.0433(15) Uani 1 1 d . . . H210 H -0.2411 -0.2580 -0.2434 0.052 Uiso 1 1 calc R . . C203 C -0.2428(3) -1.1032(8) -0.1310(2) 0.0517(17) Uani 1 1 d . . . H203 H -0.2419 -1.2034 -0.1300 0.062 Uiso 1 1 calc R . . C415 C -0.4936(3) -0.8813(7) 0.13130(18) 0.0433(15) Uani 1 1 d . . . H415 H -0.4660 -0.8249 0.1512 0.052 Uiso 1 1 calc R . . C116 C -0.6374(4) -1.1937(9) -0.2793(3) 0.068(3) Uani 1 1 d . . . H116 H -0.6581 -1.2762 -0.2903 0.082 Uiso 1 1 calc R . . C216 C -0.2461(3) -1.0008(7) -0.3079(2) 0.0517(17) Uani 1 1 d . . . H216 H -0.2111 -1.0017 -0.3104 0.062 Uiso 1 1 calc R . . C317 C -0.1540(3) -0.9685(10) 0.1202(2) 0.063(2) Uani 1 1 d . . . H317 H -0.1243 -0.9867 0.1464 0.075 Uiso 1 1 calc R . . C110 C -0.6144(3) -0.4924(7) -0.1526(2) 0.0521(18) Uani 1 1 d . . . H110 H -0.6314 -0.4317 -0.1379 0.062 Uiso 1 1 calc R . . C115 C -0.5960(4) -1.1955(8) -0.2391(3) 0.067(2) Uani 1 1 d . . . H115 H -0.5882 -1.2798 -0.2222 0.081 Uiso 1 1 calc R . . C111 C -0.6444(3) -0.5607(7) -0.1896(2) 0.0536(17) Uani 1 1 d . . . H111 H -0.6826 -0.5477 -0.2009 0.064 Uiso 1 1 calc R . . C306 C -0.2790(3) -1.4610(6) 0.0757(2) 0.0495(16) Uani 1 1 d . . . H306 H -0.2665 -1.4953 0.0533 0.059 Uiso 1 1 calc R . . C308 C -0.2861(3) -1.3549(7) -0.04210(18) 0.0407(14) Uani 1 1 d . . . H308 H -0.3244 -1.3445 -0.0512 0.049 Uiso 1 1 calc R . . C217 C -0.2556(3) -0.9178(7) -0.2764(2) 0.0435(15) Uani 1 1 d . . . H217 H -0.2269 -0.8615 -0.2578 0.052 Uiso 1 1 calc R . . C215 C -0.2869(3) -1.0826(6) -0.33561(18) 0.0426(15) Uani 1 1 d . . . H215 H -0.2804 -1.1399 -0.3574 0.051 Uiso 1 1 calc R . . C109 C -0.5593(3) -0.5109(8) -0.1362(2) 0.0552(18) Uani 1 1 d . . . H109 H -0.5381 -0.4629 -0.1101 0.066 Uiso 1 1 calc R . . C416 C -0.5448(3) -0.8839(6) 0.13375(18) 0.0391(14) Uani 1 1 d . . . H416 H -0.5528 -0.8304 0.1556 0.047 Uiso 1 1 calc R . . C204 C -0.2136(3) -1.0249(9) -0.0941(2) 0.057(2) Uani 1 1 d . . . H204 H -0.1926 -1.0712 -0.0675 0.068 Uiso 1 1 calc R . . C4S C -0.4348(3) -1.1226(8) -0.11232(18) 0.0482(16) Uani 1 1 d . . . H4S H -0.4550 -1.2063 -0.1228 0.058 Uiso 1 1 calc R . . C206 C -0.2455(3) -0.8103(7) -0.13472(18) 0.0388(14) Uani 1 1 d . . . H206 H -0.2463 -0.7101 -0.1357 0.047 Uiso 1 1 calc R . . C118 C -0.6182(3) -0.9500(8) -0.2877(2) 0.0458(15) Uani 1 1 d . . . H118 H -0.6269 -0.8663 -0.3049 0.055 Uiso 1 1 calc R . . C117 C -0.6480(3) -1.0713(10) -0.3030(2) 0.063(2) Uani 1 1 d . . . H117 H -0.6767 -1.0695 -0.3307 0.076 Uiso 1 1 calc R . . C315 C -0.2025(3) -0.8112(8) 0.0627(3) 0.063(2) Uani 1 1 d . . . H315 H -0.2065 -0.7207 0.0494 0.075 Uiso 1 1 calc R . . C205 C -0.2152(3) -0.8793(9) -0.0962(2) 0.0539(18) Uani 1 1 d . . . H205 H -0.1953 -0.8257 -0.0709 0.065 Uiso 1 1 calc R . . C104 C -0.4906(4) -0.5499(9) -0.3362(2) 0.069(2) Uani 1 1 d . . . H104 H -0.4794 -0.5019 -0.3574 0.082 Uiso 1 1 calc R . . C3S C -0.4558(3) -1.0154(9) -0.0930(2) 0.054(2) Uani 1 1 d . . . H3S H -0.4906 -1.0263 -0.0906 0.064 Uiso 1 1 calc R . . C314 C -0.2402(3) -0.9187(7) 0.0436(2) 0.0503(16) Uani 1 1 d . . . H314 H -0.2698 -0.8996 0.0173 0.060 Uiso 1 1 calc R . . C305 C -0.2841(4) -1.5534(8) 0.1074(2) 0.065(2) Uani 1 1 d . . . H305 H -0.2745 -1.6499 0.1068 0.078 Uiso 1 1 calc R . . C7S C -0.3434(4) -0.7476(8) -0.0637(2) 0.068(2) Uani 1 1 d . . . H7S1 H -0.3414 -0.7315 -0.0333 0.102 Uiso 1 1 calc R . . H7S2 H -0.3607 -0.6663 -0.0819 0.102 Uiso 1 1 calc R . . H7S3 H -0.3068 -0.7599 -0.0645 0.102 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 Zn1 0.0234(3) 0.0256(3) 0.0402(3) -0.0019(2) 0.0114(3) -0.0008(3) Zn3 0.0227(3) 0.0257(3) 0.0367(3) 0.0011(2) 0.0102(2) 0.0010(2) Zn2 0.0240(3) 0.0290(3) 0.0341(3) -0.0038(2) 0.0112(2) -0.0025(3) Zn4 0.0218(3) 0.0302(3) 0.0350(3) -0.0028(2) 0.0109(2) 0.0002(3) Si3 0.0185(7) 0.0289(7) 0.0281(7) -0.0009(5) 0.0087(6) 0.0003(5) Si2 0.0202(7) 0.0279(8) 0.0293(7) -0.0033(5) 0.0114(6) -0.0018(6) Si4 0.0210(7) 0.0240(7) 0.0294(7) -0.0025(5) 0.0116(6) -0.0017(6) Si1 0.0190(7) 0.0284(7) 0.0267(7) -0.0008(5) 0.0094(6) -0.0009(6) N3 0.021(2) 0.033(2) 0.026(2) 0.0012(17) 0.0123(17) 0.0003(18) N1 0.017(2) 0.026(2) 0.026(2) 0.0024(16) 0.0093(16) 0.0015(16) N2 0.020(2) 0.027(2) 0.041(2) -0.0010(17) 0.0144(19) -0.0027(18) N4 0.018(2) 0.024(2) 0.043(2) -0.0011(17) 0.0159(18) -0.0018(17) C401 0.024(3) 0.037(3) 0.027(3) -0.002(2) 0.012(2) -0.004(2) C413 0.024(3) 0.024(3) 0.023(2) 0.0030(18) 0.0078(19) 0.003(2) C307 0.027(3) 0.029(3) 0.033(3) 0.006(2) 0.012(2) 0.003(2) C412 0.027(3) 0.039(3) 0.038(3) -0.001(2) 0.014(2) -0.004(2) C106 0.034(3) 0.036(3) 0.033(3) -0.008(2) 0.013(2) -0.005(3) C207 0.028(3) 0.031(3) 0.024(2) -0.0049(19) 0.013(2) -0.005(2) C3 0.041(4) 0.029(3) 0.048(4) -0.003(2) 0.019(3) -0.002(3) C301 0.029(3) 0.032(3) 0.024(3) -0.003(2) 0.006(2) -0.006(2) C408 0.023(3) 0.031(3) 0.035(3) -0.002(2) 0.012(2) -0.001(2) C201 0.019(3) 0.037(3) 0.033(3) -0.001(2) 0.015(2) -0.001(2) C312 0.022(3) 0.044(3) 0.045(3) -0.005(2) 0.014(2) 0.001(2) C113 0.021(3) 0.041(3) 0.038(3) -0.007(2) 0.017(2) -0.004(2) C313 0.023(3) 0.038(3) 0.043(3) -0.010(2) 0.015(2) -0.007(2) C211 0.034(3) 0.045(4) 0.039(3) -0.007(2) 0.019(3) -0.014(3) C407 0.027(3) 0.026(3) 0.028(3) -0.0046(19) 0.012(2) -0.002(2) C28 0.030(3) 0.035(3) 0.038(3) -0.004(2) 0.008(2) -0.004(2) C101 0.023(3) 0.032(3) 0.024(3) -0.0004(19) 0.003(2) -0.001(2) C202 0.035(3) 0.046(4) 0.038(3) 0.005(2) 0.020(3) 0.005(3) C212 0.028(3) 0.038(3) 0.038(3) -0.001(2) 0.012(2) -0.005(2) C107 0.024(3) 0.034(3) 0.033(3) 0.002(2) 0.015(2) 0.001(2) C309 0.033(3) 0.061(4) 0.044(3) -0.018(3) 0.013(3) -0.003(3) C6S 0.037(4) 0.057(4) 0.035(3) 0.011(3) 0.022(3) 0.008(3) C410 0.050(4) 0.026(3) 0.038(3) -0.002(2) 0.022(3) -0.008(3) C403 0.033(4) 0.083(5) 0.029(3) 0.002(3) -0.001(3) -0.010(3) C402 0.030(3) 0.042(3) 0.039(3) -0.006(2) 0.013(2) -0.009(3) C311 0.021(3) 0.057(4) 0.057(4) -0.003(3) 0.021(3) 0.005(3) C409 0.044(4) 0.031(3) 0.033(3) 0.004(2) 0.018(3) 0.002(3) C303 0.066(5) 0.078(5) 0.025(3) 0.001(3) 0.023(3) -0.012(4) C209 0.046(4) 0.033(3) 0.048(3) -0.002(2) 0.027(3) 0.005(3) C302 0.055(4) 0.039(4) 0.045(3) 0.003(3) 0.022(3) 0.002(3) C417 0.039(4) 0.049(4) 0.051(4) -0.007(3) 0.027(3) -0.002(3) C414 0.034(3) 0.040(3) 0.028(3) -0.007(2) 0.016(2) -0.008(2) C418 0.028(3) 0.041(3) 0.042(3) -0.011(2) 0.015(2) -0.002(3) C102 0.050(4) 0.028(3) 0.027(3) 0.000(2) 0.011(2) 0.002(3) C214 0.047(4) 0.041(3) 0.034(3) -0.006(2) 0.005(3) -0.005(3) C5S 0.048(4) 0.053(4) 0.038(3) 0.006(3) 0.013(3) 0.011(3) C1 0.068(5) 0.032(3) 0.053(4) -0.004(3) 0.034(3) -0.007(3) C213 0.030(3) 0.028(3) 0.034(3) -0.002(2) 0.015(2) -0.001(2) C310 0.042(4) 0.049(4) 0.043(3) -0.009(3) 0.023(3) 0.005(3) C208 0.038(3) 0.030(3) 0.038(3) -0.002(2) 0.019(3) -0.003(2) C2S 0.042(4) 0.077(5) 0.030(3) 0.016(3) 0.024(3) 0.019(3) C411 0.041(4) 0.036(3) 0.048(3) -0.005(2) 0.018(3) -0.013(3) C108 0.029(3) 0.064(4) 0.042(3) -0.007(3) 0.012(3) 0.008(3) C2 0.055(4) 0.038(3) 0.040(3) -0.009(3) 0.010(3) -0.008(3) C105 0.070(5) 0.065(5) 0.035(3) -0.013(3) 0.025(3) -0.022(4) C1S 0.051(4) 0.053(4) 0.027(3) 0.012(2) 0.014(3) 0.008(3) C316 0.058(5) 0.073(6) 0.090(6) -0.046(5) 0.050(4) -0.042(4) C4 0.057(4) 0.037(4) 0.052(4) -0.011(3) 0.022(3) -0.005(3) C103 0.077(5) 0.039(4) 0.035(3) 0.007(2) 0.007(3) -0.021(3) C406 0.036(3) 0.041(3) 0.038(3) 0.003(2) 0.020(3) 0.002(3) C114 0.046(4) 0.042(4) 0.067(4) -0.001(3) 0.032(3) -0.013(3) C304 0.085(6) 0.057(5) 0.038(3) 0.006(3) 0.024(4) -0.024(4) C405 0.044(4) 0.050(4) 0.049(4) 0.020(3) 0.023(3) 0.011(3) C404 0.040(4) 0.076(5) 0.039(4) 0.023(3) 0.011(3) 0.010(3) C112 0.025(3) 0.049(4) 0.054(4) -0.017(3) 0.013(3) -0.002(3) C318 0.040(4) 0.072(5) 0.029(3) -0.004(3) 0.010(3) -0.017(3) C210 0.056(4) 0.036(3) 0.046(3) -0.010(3) 0.028(3) -0.017(3) C203 0.046(4) 0.053(4) 0.067(5) 0.017(3) 0.034(3) 0.019(3) C415 0.051(4) 0.046(4) 0.032(3) -0.006(2) 0.013(3) -0.011(3) C116 0.073(6) 0.065(5) 0.091(6) -0.043(4) 0.060(5) -0.047(4) C216 0.052(4) 0.055(4) 0.063(4) -0.017(3) 0.039(4) -0.007(3) C317 0.046(4) 0.107(7) 0.039(4) -0.018(4) 0.019(3) -0.038(4) C110 0.057(5) 0.048(4) 0.068(4) -0.005(3) 0.044(4) 0.009(3) C115 0.077(6) 0.041(4) 0.105(6) -0.001(4) 0.057(5) -0.009(4) C111 0.032(3) 0.054(4) 0.080(5) -0.018(3) 0.027(3) -0.004(3) C306 0.078(5) 0.035(3) 0.044(3) 0.005(3) 0.032(3) -0.002(3) C308 0.030(3) 0.052(4) 0.044(3) -0.005(3) 0.017(3) 0.001(3) C217 0.035(3) 0.054(4) 0.048(3) -0.019(3) 0.022(3) -0.011(3) C215 0.064(4) 0.035(3) 0.036(3) -0.006(2) 0.027(3) 0.003(3) C109 0.054(5) 0.074(5) 0.040(3) -0.020(3) 0.020(3) 0.006(4) C416 0.051(4) 0.037(3) 0.034(3) -0.001(2) 0.020(3) 0.002(3) C204 0.041(4) 0.092(6) 0.043(4) 0.028(4) 0.020(3) 0.016(4) C4S 0.040(4) 0.072(5) 0.029(3) 0.013(3) 0.008(3) -0.002(3) C206 0.035(3) 0.049(4) 0.035(3) 0.002(2) 0.015(2) -0.003(3) C118 0.031(3) 0.063(4) 0.047(4) -0.009(3) 0.019(3) -0.013(3) C117 0.044(4) 0.093(6) 0.061(4) -0.033(4) 0.028(3) -0.038(4) C315 0.049(5) 0.039(4) 0.113(7) -0.018(4) 0.045(5) -0.011(3) C205 0.037(4) 0.089(6) 0.033(3) -0.001(3) 0.008(3) -0.008(4) C104 0.092(6) 0.080(6) 0.028(3) 0.002(3) 0.014(4) -0.039(5) C3S 0.035(4) 0.095(6) 0.034(3) 0.026(3) 0.015(3) 0.007(4) C314 0.031(3) 0.033(4) 0.089(5) -0.001(3) 0.024(3) 0.000(3) C305 0.106(7) 0.035(4) 0.064(5) 0.006(3) 0.044(4) -0.007(4) C7S 0.093(6) 0.064(5) 0.046(4) 0.007(3) 0.022(4) -0.002(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 Zn1 C1 1.930(6) . ? Zn1 N1 2.012(4) . ? Zn1 N2 2.045(4) . ? Zn1 Zn2 2.8492(8) . ? Zn3 C3 1.946(5) . ? Zn3 N3 2.028(4) . ? Zn3 N4 2.042(4) . ? Zn3 Zn4 2.8365(8) . ? Zn2 C2 1.941(6) . ? Zn2 N2 2.038(4) . ? Zn2 N1 2.036(4) . ? Zn4 C4 1.953(6) . ? Zn4 N3 2.029(4) . ? Zn4 N4 2.047(4) . ? Si3 N3 1.725(4) . ? Si3 C301 1.878(5) . ? Si3 C307 1.883(6) . ? Si3 C313 1.883(6) . ? Si2 N2 1.728(5) . ? Si2 C207 1.871(5) . ? Si2 C213 1.875(5) . ? Si2 C201 1.889(5) . ? Si4 N4 1.724(4) . ? Si4 C407 1.871(5) . ? Si4 C401 1.883(5) . ? Si4 C413 1.894(5) . ? Si1 N1 1.734(4) . ? Si1 C107 1.873(5) . ? Si1 C101 1.877(5) . ? Si1 C113 1.885(6) . ? N3 H3 0.9300 . ? N1 H1 0.9300 . ? N2 H2 0.9300 . ? N4 H4 0.9300 . ? C401 C406 1.396(8) . ? C401 C402 1.397(7) . ? C413 C414 1.383(7) . ? C413 C418 1.392(7) . ? C307 C308 1.373(8) . ? C307 C312 1.397(8) . ? C412 C411 1.390(8) . ? C412 C407 1.397(7) . ? C412 H412 0.9500 . ? C106 C105 1.380(8) . ? C106 C101 1.406(7) . ? C106 H106 0.9500 . ? C207 C208 1.396(8) . ? C207 C212 1.415(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C301 C306 1.384(8) . ? C301 C302 1.384(8) . ? C408 C409 1.377(8) . ? C408 C407 1.401(7) . ? C408 H408 0.9500 . ? C201 C202 1.382(8) . ? C201 C206 1.405(8) . ? C312 C311 1.403(8) . ? C312 H312 0.9500 . ? C113 C118 1.391(8) . ? C113 C114 1.394(9) . ? C313 C314 1.374(8) . ? C313 C318 1.391(9) . ? C211 C210 1.385(9) . ? C211 C212 1.386(8) . ? C211 H211 0.9500 . ? C28 C213 1.397(7) . ? C28 C214 1.399(8) . ? C28 H28 0.9500 . ? C101 C102 1.383(7) . ? C202 C203 1.375(9) . ? C202 H202 0.9500 . ? C212 H212 0.9500 . ? C107 C112 1.393(8) . ? C107 C108 1.389(8) . ? C309 C310 1.383(8) . ? C309 C308 1.408(8) . ? C309 H309 0.9500 . ? C6S C5S 1.369(9) . ? C6S C1S 1.397(9) . ? C6S H6S 0.9500 . ? C410 C409 1.375(8) . ? C410 C411 1.381(8) . ? C410 H410 0.9500 . ? C403 C404 1.360(10) . ? C403 C402 1.414(8) . ? C403 H403 0.9500 . ? C402 H402 0.9500 . ? C311 C310 1.370(8) . ? C311 H311 0.9500 . ? C409 H409 0.9500 . ? C303 C304 1.362(10) . ? C303 C302 1.400(9) . ? C303 H303 0.9500 . ? C209 C210 1.374(9) . ? C209 C208 1.392(8) . ? C209 H209 0.9500 . ? C302 H302 0.9500 . ? C417 C418 1.375(8) . ? C417 C416 1.389(9) . ? C417 H417 0.9500 . ? C414 C415 1.396(8) . ? C414 H414 0.9500 . ? C418 H418 0.9500 . ? C102 C103 1.392(8) . ? C102 H102 0.9500 . ? C214 C215 1.378(9) . ? C214 H214 0.9500 . ? C5S C4S 1.374(9) . ? C5S H5S 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C213 C217 1.410(8) . ? C310 H310 0.9500 . ? C208 H208 0.9500 . ? C2S C3S 1.378(10) . ? C2S C1S 1.389(9) . ? C2S H2S 0.9500 . ? C411 H411 0.9500 . ? C108 C109 1.381(9) . ? C108 H108 0.9500 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C105 C104 1.364(10) . ? C105 H105 0.9500 . ? C1S C7S 1.471(10) . ? C316 C317 1.368(11) . ? C316 C315 1.368(12) . ? C316 H316 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C103 C104 1.384(10) . ? C103 H103 0.9500 . ? C406 C405 1.387(8) . ? C406 H406 0.9500 . ? C114 C115 1.402(9) . ? C114 H114 0.9500 . ? C304 C305 1.376(10) . ? C304 H304 0.9500 . ? C405 C404 1.381(10) . ? C405 H405 0.9500 . ? C404 H404 0.9500 . ? C112 C111 1.374(8) . ? C112 H112 0.9500 . ? C318 C317 1.401(9) . ? C318 H318 0.9500 . ? C210 H210 0.9500 . ? C203 C204 1.389(11) . ? C203 H203 0.9500 . ? C415 C416 1.376(9) . ? C415 H415 0.9500 . ? C116 C117 1.365(12) . ? C116 C115 1.373(12) . ? C116 H116 0.9500 . ? C216 C215 1.375(9) . ? C216 C217 1.376(8) . ? C216 H216 0.9500 . ? C317 H317 0.9500 . ? C110 C111 1.349(10) . ? C110 C109 1.371(10) . ? C110 H110 0.9500 . ? C115 H115 0.9500 . ? C111 H111 0.9500 . ? C306 C305 1.389(8) . ? C306 H306 0.9500 . ? C308 H308 0.9500 . ? C217 H217 0.9500 . ? C215 H215 0.9500 . ? C109 H109 0.9500 . ? C416 H416 0.9500 . ? C204 C205 1.382(10) . ? C204 H204 0.9500 . ? C4S C3S 1.402(10) . ? C4S H4S 0.9500 . ? C206 C205 1.388(9) . ? C206 H206 0.9500 . ? C118 C117 1.383(9) . ? C118 H118 0.9500 . ? C117 H117 0.9500 . ? C315 C314 1.406(9) . ? C315 H315 0.9500 . ? C205 H205 0.9500 . ? C104 H104 0.9500 . ? C3S H3S 0.9500 . ? C314 H314 0.9500 . ? C305 H305 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? 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 C1 Zn1 N1 136.5(2) . . ? C1 Zn1 N2 133.1(2) . . ? N1 Zn1 N2 89.80(17) . . ? C1 Zn1 Zn2 176.1(2) . . ? N1 Zn1 Zn2 45.61(11) . . ? N2 Zn1 Zn2 45.63(12) . . ? C3 Zn3 N3 137.2(2) . . ? C3 Zn3 N4 133.0(2) . . ? N3 Zn3 N4 89.83(17) . . ? C3 Zn3 Zn4 169.24(19) . . ? N3 Zn3 Zn4 45.67(12) . . ? N4 Zn3 Zn4 46.16(12) . . ? C2 Zn2 N2 136.3(3) . . ? C2 Zn2 N1 134.3(2) . . ? N2 Zn2 N1 89.34(16) . . ? C2 Zn2 Zn1 172.4(2) . . ? N2 Zn2 Zn1 45.84(12) . . ? N1 Zn2 Zn1 44.93(11) . . ? C4 Zn4 N3 137.0(2) . . ? C4 Zn4 N4 133.3(2) . . ? N3 Zn4 N4 89.62(16) . . ? C4 Zn4 Zn3 170.7(2) . . ? N3 Zn4 Zn3 45.62(11) . . ? N4 Zn4 Zn3 46.00(12) . . ? N3 Si3 C301 107.0(2) . . ? N3 Si3 C307 110.7(2) . . ? C301 Si3 C307 109.0(2) . . ? N3 Si3 C313 112.8(2) . . ? C301 Si3 C313 109.1(2) . . ? C307 Si3 C313 108.2(3) . . ? N2 Si2 C207 111.3(2) . . ? N2 Si2 C213 111.3(2) . . ? C207 Si2 C213 108.8(2) . . ? N2 Si2 C201 109.3(2) . . ? C207 Si2 C201 109.9(2) . . ? C213 Si2 C201 106.2(2) . . ? N4 Si4 C407 110.3(2) . . ? N4 Si4 C401 109.2(2) . . ? C407 Si4 C401 110.9(2) . . ? N4 Si4 C413 111.6(2) . . ? C407 Si4 C413 108.4(2) . . ? C401 Si4 C413 106.4(2) . . ? N1 Si1 C107 111.2(2) . . ? N1 Si1 C101 103.9(2) . . ? C107 Si1 C101 109.5(2) . . ? N1 Si1 C113 112.1(2) . . ? C107 Si1 C113 110.6(2) . . ? C101 Si1 C113 109.3(2) . . ? Si3 N3 Zn3 124.0(2) . . ? Si3 N3 Zn4 115.0(2) . . ? Zn3 N3 Zn4 88.72(16) . . ? Si3 N3 H3 109.1 . . ? Zn3 N3 H3 109.1 . . ? Zn4 N3 H3 109.1 . . ? Si1 N1 Zn1 116.0(2) . . ? Si1 N1 Zn2 112.7(2) . . ? Zn1 N1 Zn2 89.46(16) . . ? Si1 N1 H1 112.3 . . ? Zn1 N1 H1 112.3 . . ? Zn2 N1 H1 112.3 . . ? Si2 N2 Zn2 122.9(2) . . ? Si2 N2 Zn1 125.8(2) . . ? Zn2 N2 Zn1 88.53(17) . . ? Si2 N2 H2 105.7 . . ? Zn2 N2 H2 105.7 . . ? Zn1 N2 H2 105.7 . . ? Si4 N4 Zn3 129.3(2) . . ? Si4 N4 Zn4 120.9(2) . . ? Zn3 N4 Zn4 87.84(16) . . ? Si4 N4 H4 105.3 . . ? Zn3 N4 H4 105.3 . . ? Zn4 N4 H4 105.3 . . ? C406 C401 C402 117.7(5) . . ? C406 C401 Si4 119.1(4) . . ? C402 C401 Si4 123.1(4) . . ? C414 C413 C418 116.7(5) . . ? C414 C413 Si4 122.4(4) . . ? C418 C413 Si4 120.9(4) . . ? C308 C307 C312 117.2(5) . . ? C308 C307 Si3 122.4(4) . . ? C312 C307 Si3 120.4(4) . . ? C411 C412 C407 121.6(6) . . ? C411 C412 H412 119.2 . . ? C407 C412 H412 119.2 . . ? C105 C106 C101 121.7(6) . . ? C105 C106 H106 119.1 . . ? C101 C106 H106 119.1 . . ? C208 C207 C212 116.9(5) . . ? C208 C207 Si2 120.4(4) . . ? C212 C207 Si2 122.5(4) . . ? Zn3 C3 H3A 109.5 . . ? Zn3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Zn3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C306 C301 C302 118.1(5) . . ? C306 C301 Si3 120.5(4) . . ? C302 C301 Si3 121.4(4) . . ? C409 C408 C407 121.3(5) . . ? C409 C408 H408 119.3 . . ? C407 C408 H408 119.3 . . ? C202 C201 C206 117.9(5) . . ? C202 C201 Si2 119.6(4) . . ? C206 C201 Si2 122.4(4) . . ? C307 C312 C311 121.5(5) . . ? C307 C312 H312 119.2 . . ? C311 C312 H312 119.2 . . ? C118 C113 C114 117.5(6) . . ? C118 C113 Si1 123.0(5) . . ? C114 C113 Si1 119.5(5) . . ? C314 C313 C318 118.0(6) . . ? C314 C313 Si3 120.1(5) . . ? C318 C313 Si3 121.8(5) . . ? C210 C211 C212 119.3(6) . . ? C210 C211 H211 120.3 . . ? C212 C211 H211 120.3 . . ? C412 C407 C408 116.7(5) . . ? C412 C407 Si4 122.4(4) . . ? C408 C407 Si4 120.8(4) . . ? C213 C28 C214 120.9(6) . . ? C213 C28 H28 119.5 . . ? C214 C28 H28 119.5 . . ? C102 C101 C106 116.9(5) . . ? C102 C101 Si1 121.0(4) . . ? C106 C101 Si1 121.5(4) . . ? C203 C202 C201 122.4(6) . . ? C203 C202 H202 118.8 . . ? C201 C202 H202 118.8 . . ? C211 C212 C207 121.8(6) . . ? C211 C212 H212 119.1 . . ? C207 C212 H212 119.1 . . ? C112 C107 C108 117.1(5) . . ? C112 C107 Si1 120.8(4) . . ? C108 C107 Si1 122.0(4) . . ? C310 C309 C308 119.2(5) . . ? C310 C309 H309 120.4 . . ? C308 C309 H309 120.4 . . ? C5S C6S C1S 122.5(6) . . ? C5S C6S H6S 118.8 . . ? C1S C6S H6S 118.8 . . ? C409 C410 C411 118.9(5) . . ? C409 C410 H410 120.5 . . ? C411 C410 H410 120.5 . . ? C404 C403 C402 121.2(6) . . ? C404 C403 H403 119.4 . . ? C402 C403 H403 119.4 . . ? C401 C402 C403 119.6(6) . . ? C401 C402 H402 120.2 . . ? C403 C402 H402 120.2 . . ? C310 C311 C312 119.8(5) . . ? C310 C311 H311 120.1 . . ? C312 C311 H311 120.1 . . ? C410 C409 C408 121.2(5) . . ? C410 C409 H409 119.4 . . ? C408 C409 H409 119.4 . . ? C304 C303 C302 120.4(6) . . ? C304 C303 H303 119.8 . . ? C302 C303 H303 119.8 . . ? C210 C209 C208 120.2(6) . . ? C210 C209 H209 119.9 . . ? C208 C209 H209 119.9 . . ? C301 C302 C303 120.7(6) . . ? C301 C302 H302 119.7 . . ? C303 C302 H302 119.7 . . ? C418 C417 C416 120.0(6) . . ? C418 C417 H417 120.0 . . ? C416 C417 H417 120.0 . . ? C413 C414 C415 122.1(5) . . ? C413 C414 H414 119.0 . . ? C415 C414 H414 119.0 . . ? C417 C418 C413 122.2(5) . . ? C417 C418 H418 118.9 . . ? C413 C418 H418 118.9 . . ? C101 C102 C103 121.3(5) . . ? C101 C102 H102 119.4 . . ? C103 C102 H102 119.4 . . ? C215 C214 C28 120.9(5) . . ? C215 C214 H214 119.6 . . ? C28 C214 H214 119.6 . . ? C4S C5S C6S 119.8(6) . . ? C4S C5S H5S 120.1 . . ? C6S C5S H5S 120.1 . . ? Zn1 C1 H1A 109.5 . . ? Zn1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Zn1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C28 C213 C217 116.2(5) . . ? C28 C213 Si2 123.1(4) . . ? C217 C213 Si2 120.7(4) . . ? C311 C310 C309 120.2(5) . . ? C311 C310 H310 119.9 . . ? C309 C310 H310 119.9 . . ? C209 C208 C207 121.3(6) . . ? C209 C208 H208 119.4 . . ? C207 C208 H208 119.4 . . ? C3S C2S C1S 120.8(7) . . ? C3S C2S H2S 119.6 . . ? C1S C2S H2S 119.6 . . ? C412 C411 C410 120.2(6) . . ? C412 C411 H411 119.9 . . ? C410 C411 H411 119.9 . . ? C109 C108 C107 120.7(6) . . ? C109 C108 H108 119.6 . . ? C107 C108 H108 119.6 . . ? Zn2 C2 H2A 109.5 . . ? Zn2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Zn2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C104 C105 C106 120.3(6) . . ? C104 C105 H105 119.8 . . ? C106 C105 H105 119.8 . . ? C2S C1S C6S 117.3(7) . . ? C2S C1S C7S 121.2(7) . . ? C6S C1S C7S 121.5(7) . . ? C317 C316 C315 120.7(6) . . ? C317 C316 H316 119.7 . . ? C315 C316 H316 119.7 . . ? Zn4 C4 H4A 109.5 . . ? Zn4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Zn4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C104 C103 C102 120.3(6) . . ? C104 C103 H103 119.8 . . ? C102 C103 H103 119.8 . . ? C405 C406 C401 121.9(6) . . ? C405 C406 H406 119.0 . . ? C401 C406 H406 119.0 . . ? C113 C114 C115 120.8(7) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C303 C304 C305 119.6(6) . . ? C303 C304 H304 120.2 . . ? C305 C304 H304 120.2 . . ? C406 C405 C404 119.7(6) . . ? C406 C405 H405 120.1 . . ? C404 C405 H405 120.1 . . ? C403 C404 C405 119.8(5) . . ? C403 C404 H404 120.1 . . ? C405 C404 H404 120.1 . . ? C111 C112 C107 121.2(6) . . ? C111 C112 H112 119.4 . . ? C107 C112 H112 119.4 . . ? C313 C318 C317 120.9(7) . . ? C313 C318 H318 119.6 . . ? C317 C318 H318 119.6 . . ? C209 C210 C211 120.5(6) . . ? C209 C210 H210 119.7 . . ? C211 C210 H210 119.7 . . ? C202 C203 C204 119.4(7) . . ? C202 C203 H203 120.3 . . ? C204 C203 H203 120.3 . . ? C416 C415 C414 119.7(5) . . ? C416 C415 H415 120.2 . . ? C414 C415 H415 120.2 . . ? C117 C116 C115 118.8(6) . . ? C117 C116 H116 120.6 . . ? C115 C116 H116 120.6 . . ? C215 C216 C217 120.2(6) . . ? C215 C216 H216 119.9 . . ? C217 C216 H216 119.9 . . ? C316 C317 C318 119.7(7) . . ? C316 C317 H317 120.2 . . ? C318 C317 H317 120.2 . . ? C111 C110 C109 119.8(6) . . ? C111 C110 H110 120.1 . . ? C109 C110 H110 120.1 . . ? C116 C115 C114 120.4(7) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C110 C111 C112 120.7(6) . . ? C110 C111 H111 119.7 . . ? C112 C111 H111 119.7 . . ? C301 C306 C305 121.0(6) . . ? C301 C306 H306 119.5 . . ? C305 C306 H306 119.5 . . ? C307 C308 C309 122.1(6) . . ? C307 C308 H308 118.9 . . ? C309 C308 H308 118.9 . . ? C216 C217 C213 122.5(6) . . ? C216 C217 H217 118.8 . . ? C213 C217 H217 118.8 . . ? C216 C215 C214 119.2(5) . . ? C216 C215 H215 120.4 . . ? C214 C215 H215 120.4 . . ? C110 C109 C108 120.4(6) . . ? C110 C109 H109 119.8 . . ? C108 C109 H109 119.8 . . ? C415 C416 C417 119.3(5) . . ? C415 C416 H416 120.3 . . ? C417 C416 H416 120.3 . . ? C205 C204 C203 119.5(6) . . ? C205 C204 H204 120.3 . . ? C203 C204 H204 120.3 . . ? C5S C4S C3S 119.1(7) . . ? C5S C4S H4S 120.4 . . ? C3S C4S H4S 120.4 . . ? C205 C206 C201 119.9(6) . . ? C205 C206 H206 120.1 . . ? C201 C206 H206 120.1 . . ? C117 C118 C113 120.8(7) . . ? C117 C118 H118 119.6 . . ? C113 C118 H118 119.6 . . ? C116 C117 C118 121.7(7) . . ? C116 C117 H117 119.2 . . ? C118 C117 H117 119.2 . . ? C316 C315 C314 119.3(7) . . ? C316 C315 H315 120.3 . . ? C314 C315 H315 120.3 . . ? C204 C205 C206 120.9(6) . . ? C204 C205 H205 119.5 . . ? C206 C205 H205 119.5 . . ? C105 C104 C103 119.5(6) . . ? C105 C104 H104 120.3 . . ? C103 C104 H104 120.3 . . ? C2S C3S C4S 120.5(7) . . ? C2S C3S H3S 119.8 . . ? C4S C3S H3S 119.8 . . ? C313 C314 C315 121.4(7) . . ? C313 C314 H314 119.3 . . ? C315 C314 H314 119.3 . . ? C304 C305 C306 120.3(7) . . ? C304 C305 H305 119.9 . . ? C306 C305 H305 119.9 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.759 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 960127' ####################################################################### # # 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_h07alj11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H44 N8 Si2 Zn2' _chemical_formula_weight 511.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.83400(10) _cell_length_b 10.0490(2) _cell_length_c 15.9980(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.4860(10) _cell_angle_gamma 90.00 _cell_volume 1259.00(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26752 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 2.015 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7257 _exptl_absorpt_correction_T_max 0.8554 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26752 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2892 _reflns_number_gt 2421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0415P)^2^+0.3362P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0136(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2892 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Zn1 Zn 0.54928(3) 0.13774(2) -0.016400(13) 0.02508(10) Uani 1 1 d . . . Si1 Si 0.25834(7) 0.12557(5) 0.08385(3) 0.02310(13) Uani 1 1 d . . . N1 N 0.3156(2) 0.03165(15) 0.00063(10) 0.0242(3) Uani 1 1 d . . . N2 N 0.4611(2) 0.18591(15) 0.11877(10) 0.0277(3) Uani 1 1 d . . . N3 N 0.1722(2) 0.04010(16) 0.16477(10) 0.0308(4) Uani 1 1 d . . . N4 N 0.1274(2) 0.25320(15) 0.05195(10) 0.0293(4) Uani 1 1 d . . . C1 C 0.5984(3) 0.3022(2) -0.07892(15) 0.0410(5) Uani 1 1 d . . . H1A H 0.5781 0.3796 -0.0433 0.062 Uiso 1 1 calc R . . H1B H 0.5236 0.3069 -0.1289 0.062 Uiso 1 1 calc R . . H1C H 0.7179 0.3016 -0.0956 0.062 Uiso 1 1 calc R . . C21 C 0.5652(3) 0.1028(2) 0.17624(12) 0.0365(5) Uani 1 1 d . . . H21A H 0.6862 0.1247 0.1703 0.055 Uiso 1 1 calc R . . H21B H 0.5467 0.0087 0.1628 0.055 Uiso 1 1 calc R . . H21C H 0.5320 0.1198 0.2339 0.055 Uiso 1 1 calc R . . C22 C 0.4809(3) 0.3273(2) 0.14075(15) 0.0414(5) Uani 1 1 d . . . H22A H 0.4453 0.3413 0.1983 0.062 Uiso 1 1 calc R . . H22B H 0.4098 0.3814 0.1027 0.062 Uiso 1 1 calc R . . H22C H 0.6008 0.3532 0.1359 0.062 Uiso 1 1 calc R . . C31 C 0.1734(3) 0.0889(2) 0.25029(13) 0.0400(5) Uani 1 1 d . . . H31A H 0.0562 0.1082 0.2665 0.060 Uiso 1 1 calc R . . H31B H 0.2419 0.1704 0.2543 0.060 Uiso 1 1 calc R . . H31C H 0.2228 0.0212 0.2877 0.060 Uiso 1 1 calc R . . C32 C 0.0636(3) -0.0749(2) 0.15223(14) 0.0387(5) Uani 1 1 d . . . H32A H 0.1040 -0.1475 0.1886 0.058 Uiso 1 1 calc R . . H32B H 0.0672 -0.1033 0.0937 0.058 Uiso 1 1 calc R . . H32C H -0.0539 -0.0519 0.1660 0.058 Uiso 1 1 calc R . . C41 C 0.0131(3) 0.3208(3) 0.10759(16) 0.0503(6) Uani 1 1 d . . . H41A H 0.0638 0.4056 0.1254 0.075 Uiso 1 1 calc R . . H41B H -0.0057 0.2650 0.1568 0.075 Uiso 1 1 calc R . . H41C H -0.0963 0.3374 0.0783 0.075 Uiso 1 1 calc R . . C42 C 0.1488(3) 0.3284(2) -0.02511(13) 0.0347(4) Uani 1 1 d . . . H42A H 0.0372 0.3414 -0.0530 0.052 Uiso 1 1 calc R . . H42B H 0.2238 0.2791 -0.0622 0.052 Uiso 1 1 calc R . . H42C H 0.1998 0.4152 -0.0119 0.052 Uiso 1 1 calc R . . H1 H 0.237(3) 0.025(2) -0.0375(17) 0.046(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03096(15) 0.01834(13) 0.02602(14) 0.00141(8) 0.00247(9) 0.00120(8) Si1 0.0285(3) 0.0196(2) 0.0213(3) 0.00024(17) 0.0022(2) 0.00300(18) N1 0.0280(8) 0.0219(7) 0.0227(8) -0.0009(6) -0.0014(6) 0.0029(6) N2 0.0344(9) 0.0219(8) 0.0269(8) -0.0020(6) -0.0007(6) 0.0011(6) N3 0.0399(9) 0.0268(8) 0.0258(8) 0.0022(6) 0.0050(7) -0.0004(7) N4 0.0341(9) 0.0248(8) 0.0293(8) 0.0023(6) 0.0049(7) 0.0080(6) C1 0.0444(12) 0.0306(11) 0.0484(13) 0.0139(9) 0.0057(10) 0.0014(9) C21 0.0420(12) 0.0422(11) 0.0248(10) -0.0039(8) -0.0058(8) 0.0073(9) C22 0.0449(13) 0.0296(11) 0.0496(13) -0.0150(9) -0.0007(10) -0.0033(9) C31 0.0512(13) 0.0431(12) 0.0261(10) 0.0028(9) 0.0090(9) 0.0034(10) C32 0.0365(11) 0.0381(11) 0.0420(12) 0.0039(9) 0.0084(9) -0.0055(9) C41 0.0583(15) 0.0483(14) 0.0450(13) 0.0048(11) 0.0158(11) 0.0267(12) C42 0.0396(11) 0.0271(10) 0.0376(11) 0.0087(8) 0.0020(9) 0.0059(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 1.975(2) . ? Zn1 N1 2.0168(15) 3_655 ? Zn1 N1 2.1419(16) . ? Zn1 N2 2.3379(16) . ? Zn1 Si1 2.8234(5) . ? Zn1 Zn1 2.9250(4) 3_655 ? Si1 N1 1.7016(15) . ? Si1 N3 1.7071(16) . ? Si1 N4 1.7119(16) . ? Si1 N2 1.7766(17) . ? N1 Zn1 2.0168(15) 3_655 ? N1 H1 0.86(3) . ? N2 C22 1.471(2) . ? N2 C21 1.473(3) . ? N3 C32 1.446(3) . ? N3 C31 1.453(3) . ? N4 C41 1.448(3) . ? N4 C42 1.459(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 C1 Zn1 N1 131.38(8) . 3_655 ? C1 Zn1 N1 131.25(8) . . ? N1 Zn1 N1 90.66(6) 3_655 . ? C1 Zn1 N2 111.19(8) . . ? N1 Zn1 N2 103.05(6) 3_655 . ? N1 Zn1 N2 73.22(6) . . ? C1 Zn1 Si1 119.66(7) . . ? N1 Zn1 Si1 108.73(4) 3_655 . ? N1 Zn1 Si1 36.96(4) . . ? N2 Zn1 Si1 38.85(4) . . ? C1 Zn1 Zn1 159.83(7) . 3_655 ? N1 Zn1 Zn1 47.07(5) 3_655 3_655 ? N1 Zn1 Zn1 43.59(4) . 3_655 ? N2 Zn1 Zn1 86.81(4) . 3_655 ? Si1 Zn1 Zn1 68.676(12) . 3_655 ? N1 Si1 N3 115.57(8) . . ? N1 Si1 N4 110.51(8) . . ? N3 Si1 N4 110.95(8) . . ? N1 Si1 N2 100.58(8) . . ? N3 Si1 N2 107.52(8) . . ? N4 Si1 N2 111.22(8) . . ? N1 Si1 Zn1 49.19(6) . . ? N3 Si1 Zn1 142.50(6) . . ? N4 Si1 Zn1 106.53(6) . . ? N2 Si1 Zn1 55.64(5) . . ? Si1 N1 Zn1 121.23(9) . 3_655 ? Si1 N1 Zn1 93.84(7) . . ? Zn1 N1 Zn1 89.34(6) 3_655 . ? Si1 N1 H1 113.4(16) . . ? Zn1 N1 H1 113.1(16) 3_655 . ? Zn1 N1 H1 123.1(16) . . ? C22 N2 C21 110.18(16) . . ? C22 N2 Si1 119.52(14) . . ? C21 N2 Si1 118.62(13) . . ? C22 N2 Zn1 112.91(13) . . ? C21 N2 Zn1 106.73(12) . . ? Si1 N2 Zn1 85.51(6) . . ? C32 N3 C31 112.94(17) . . ? C32 N3 Si1 122.66(14) . . ? C31 N3 Si1 123.44(14) . . ? C41 N4 C42 111.29(16) . . ? C41 N4 Si1 122.91(14) . . ? C42 N4 Si1 123.97(13) . . ? Zn1 C1 H1A 109.5 . . ? Zn1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Zn1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.631 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 960128' ####################################################################### # # 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_h11alj19 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H84 N4 Si6 Zn2' _chemical_formula_weight 1184.61 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' Si Si 0.0817 0.0704 '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' _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 11.4310(4) _cell_length_b 11.9430(5) _cell_length_c 12.9460(5) _cell_angle_alpha 87.265(2) _cell_angle_beta 71.794(2) _cell_angle_gamma 73.697(2) _cell_volume 1609.86(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29835 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8273 _exptl_absorpt_correction_T_max 0.8626 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; This crystal was weakly diffracting and there was very little data above the 2theta limit recorded. ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29835 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6615 _reflns_number_gt 5415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0352P)^2^+0.7730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6615 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Zn1 Zn 0.50664(2) 0.07834(2) 0.414455(18) 0.02394(8) Uani 1 1 d . . . N1 N 0.36522(16) 0.06233(16) 0.54981(15) 0.0246(4) Uani 1 1 d . . . N10 N 0.51054(16) 0.18523(14) 0.30208(13) 0.0250(4) Uani 1 1 d . . . Si1 Si 0.22322(5) 0.04557(5) 0.53704(4) 0.02427(13) Uani 1 1 d . . . Si20 Si 0.48807(6) 0.33040(5) 0.32756(5) 0.02980(14) Uani 1 1 d . . . Si10 Si 0.55473(6) 0.12223(6) 0.17380(5) 0.03127(15) Uani 1 1 d . . . C15 C 0.0177(2) -0.1440(2) 0.76757(19) 0.0360(5) Uani 1 1 d . . . H15 H -0.0033 -0.2157 0.7695 0.043 Uiso 1 1 calc R . . C22 C 0.4099(3) 0.4262(2) 0.2345(2) 0.0447(6) Uani 1 1 d . . . H22A H 0.4677 0.4113 0.1595 0.067 Uiso 1 1 calc R . . H22B H 0.3917 0.5083 0.2563 0.067 Uiso 1 1 calc R . . H22C H 0.3296 0.4089 0.2391 0.067 Uiso 1 1 calc R . . C21 C 0.6410(2) 0.3684(2) 0.3120(2) 0.0447(6) Uani 1 1 d . . . H21A H 0.6813 0.3261 0.3645 0.067 Uiso 1 1 calc R . . H21B H 0.6221 0.4526 0.3256 0.067 Uiso 1 1 calc R . . H21C H 0.6994 0.3463 0.2380 0.067 Uiso 1 1 calc R . . C23 C 0.3808(2) 0.3774(2) 0.47016(19) 0.0401(6) Uani 1 1 d . . . H23A H 0.2958 0.3680 0.4789 0.060 Uiso 1 1 calc R . . H23B H 0.3728 0.4596 0.4841 0.060 Uiso 1 1 calc R . . H23C H 0.4177 0.3292 0.5218 0.060 Uiso 1 1 calc R . . C13 C 0.6072(2) -0.0404(2) 0.1796(2) 0.0414(6) Uani 1 1 d . . . H13A H 0.6841 -0.0636 0.2028 0.062 Uiso 1 1 calc R . . H13B H 0.6265 -0.0759 0.1073 0.062 Uiso 1 1 calc R . . H13C H 0.5383 -0.0667 0.2317 0.062 Uiso 1 1 calc R . . C12 C 0.4196(3) 0.1582(2) 0.1136(2) 0.0493(7) Uani 1 1 d . . . H12A H 0.3480 0.1318 0.1612 0.074 Uiso 1 1 calc R . . H12B H 0.4492 0.1187 0.0416 0.074 Uiso 1 1 calc R . . H12C H 0.3912 0.2428 0.1066 0.074 Uiso 1 1 calc R . . C11 C 0.6904(3) 0.1692(3) 0.0769(2) 0.0518(7) Uani 1 1 d . . . H11A H 0.6622 0.2533 0.0669 0.078 Uiso 1 1 calc R . . H11B H 0.7176 0.1267 0.0066 0.078 Uiso 1 1 calc R . . H11C H 0.7625 0.1522 0.1063 0.078 Uiso 1 1 calc R . . C101 C 0.12747(18) -0.00705(18) 0.66566(17) 0.0269(4) Uani 1 1 d . . . C102 C 0.0824(2) 0.0627(2) 0.76220(17) 0.0305(5) Uani 1 1 d . . . H102 H 0.1049 0.1336 0.7616 0.037 Uiso 1 1 calc R . . C103 C 0.0063(2) 0.0305(2) 0.85775(18) 0.0349(5) Uani 1 1 d . . . H103 H -0.0238 0.0796 0.9217 0.042 Uiso 1 1 calc R . . C104 C -0.0261(2) -0.0733(2) 0.86048(19) 0.0377(6) Uani 1 1 d . . . H104 H -0.0784 -0.0955 0.9262 0.045 Uiso 1 1 calc R . . C105 C 0.0928(2) -0.1106(2) 0.67087(18) 0.0314(5) Uani 1 1 d . . . H105 H 0.1210 -0.1595 0.6070 0.038 Uiso 1 1 calc R . . C106 C 0.27829(18) -0.06547(18) 0.42170(16) 0.0261(4) Uani 1 1 d . . . C107 C 0.3621(2) -0.17586(19) 0.42552(18) 0.0314(5) Uani 1 1 d . . . H107 H 0.3883 -0.1947 0.4885 0.038 Uiso 1 1 calc R . . C108 C 0.4075(2) -0.2582(2) 0.3397(2) 0.0371(5) Uani 1 1 d . . . H108 H 0.4640 -0.3322 0.3444 0.045 Uiso 1 1 calc R . . C109 C 0.3704(2) -0.2324(2) 0.24740(19) 0.0378(5) Uani 1 1 d . . . H109 H 0.4026 -0.2879 0.1879 0.045 Uiso 1 1 calc R . . C110 C 0.2863(2) -0.1254(2) 0.24229(19) 0.0382(5) Uani 1 1 d . . . H110 H 0.2591 -0.1079 0.1796 0.046 Uiso 1 1 calc R . . C111 C 0.2412(2) -0.0432(2) 0.32802(18) 0.0319(5) Uani 1 1 d . . . H111 H 0.1836 0.0301 0.3229 0.038 Uiso 1 1 calc R . . C112 C 0.11726(19) 0.18408(18) 0.50278(17) 0.0268(4) Uani 1 1 d . . . C113 C 0.1628(2) 0.2445(2) 0.41018(19) 0.0331(5) Uani 1 1 d . . . H113 H 0.2499 0.2174 0.3664 0.040 Uiso 1 1 calc R . . C114 C 0.0830(2) 0.3432(2) 0.3813(2) 0.0384(6) Uani 1 1 d . . . H114 H 0.1155 0.3820 0.3175 0.046 Uiso 1 1 calc R . . C115 C -0.0438(2) 0.3852(2) 0.4451(2) 0.0393(6) Uani 1 1 d . . . H115 H -0.0982 0.4531 0.4258 0.047 Uiso 1 1 calc R . . C116 C -0.0905(2) 0.3278(2) 0.5370(2) 0.0373(5) Uani 1 1 d . . . H116 H -0.1772 0.3566 0.5813 0.045 Uiso 1 1 calc R . . C117 C -0.0113(2) 0.2281(2) 0.56514(18) 0.0326(5) Uani 1 1 d . . . H117 H -0.0453 0.1890 0.6282 0.039 Uiso 1 1 calc R . . C1S C -0.0215(4) 0.3697(4) 0.8818(4) 0.0564(15) Uani 0.694(8) 1 d PG A -1 C2S C 0.0738(5) 0.3827(5) 0.7882(3) 0.068(2) Uani 0.694(8) 1 d PG A -1 H2S H 0.0548 0.3994 0.7217 0.082 Uiso 0.694(8) 1 calc PR A -1 C3S C 0.1968(5) 0.3714(5) 0.7917(4) 0.086(3) Uani 0.694(8) 1 d PG A -1 H3S H 0.2619 0.3803 0.7277 0.103 Uiso 0.694(8) 1 calc PR A -1 C4S C 0.2246(5) 0.3470(5) 0.8889(5) 0.088(2) Uani 0.694(8) 1 d PG A -1 H4S H 0.3087 0.3392 0.8914 0.106 Uiso 0.694(8) 1 calc PR A -1 C5S C 0.1294(6) 0.3339(4) 0.9826(3) 0.074(2) Uani 0.694(8) 1 d PG A -1 H5S H 0.1484 0.3172 1.0490 0.089 Uiso 0.694(8) 1 calc PR A -1 C6S C 0.0063(5) 0.3452(4) 0.9790(3) 0.053(2) Uani 0.694(8) 1 d PG A -1 H6S H -0.0588 0.3363 1.0430 0.064 Uiso 0.694(8) 1 calc PR A -1 C7S C -0.1495(7) 0.3801(6) 0.8766(6) 0.091(2) Uani 0.694(8) 1 d P A -1 H7S1 H -0.1554 0.4088 0.8057 0.136 Uiso 0.694(8) 1 calc PR A -1 H7S2 H -0.2131 0.4351 0.9345 0.136 Uiso 0.694(8) 1 calc PR A -1 H7S3 H -0.1661 0.3035 0.8861 0.136 Uiso 0.694(8) 1 calc PR A -1 C21S C 0.1566(9) 0.3752(8) 0.8892(7) 0.057(3) Uani 0.306(8) 1 d PG A -2 C22S C 0.1359(11) 0.3938(9) 0.7887(6) 0.063(5) Uani 0.306(8) 1 d PG A -2 H22S H 0.2000 0.4110 0.7283 0.075 Uiso 0.306(8) 1 calc PR A -2 C23S C 0.0212(13) 0.3873(11) 0.7767(9) 0.099(8) Uani 0.306(8) 1 d PG A -2 H23S H 0.0071 0.4001 0.7081 0.118 Uiso 0.306(8) 1 calc PR A -2 C24S C -0.0726(10) 0.3622(10) 0.8652(13) 0.110(9) Uani 0.306(8) 1 d PG A -2 H24S H -0.1509 0.3578 0.8569 0.131 Uiso 0.306(8) 1 calc PR A -2 C25S C -0.0519(10) 0.3436(9) 0.9656(10) 0.075(5) Uani 0.306(8) 1 d PG A -2 H25S H -0.1160 0.3264 1.0260 0.090 Uiso 0.306(8) 1 calc PR A -2 C26S C 0.0628(12) 0.3500(8) 0.9776(6) 0.059(5) Uani 0.306(8) 1 d PG A -2 H26S H 0.0769 0.3373 1.0463 0.071 Uiso 0.306(8) 1 calc PR A -2 C27S C 0.2804(12) 0.3811(12) 0.9060(11) 0.073(4) Uani 0.306(8) 1 d P A -2 H27A H 0.3494 0.3112 0.8721 0.110 Uiso 0.306(8) 1 calc PR A -2 H27B H 0.2689 0.3852 0.9841 0.110 Uiso 0.306(8) 1 calc PR A -2 H27C H 0.3028 0.4507 0.8726 0.110 Uiso 0.306(8) 1 calc PR A -2 H1 H 0.352(2) 0.111(2) 0.5914(19) 0.028(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02375(13) 0.02353(14) 0.02329(13) 0.00416(9) -0.00685(10) -0.00574(9) N1 0.0242(9) 0.0236(10) 0.0231(9) 0.0000(8) -0.0053(7) -0.0044(7) N10 0.0280(9) 0.0233(9) 0.0214(8) 0.0042(7) -0.0060(7) -0.0061(7) Si1 0.0205(3) 0.0246(3) 0.0244(3) 0.0017(2) -0.0051(2) -0.0034(2) Si20 0.0331(3) 0.0225(3) 0.0330(3) 0.0036(2) -0.0114(3) -0.0057(2) Si10 0.0330(3) 0.0341(3) 0.0230(3) -0.0003(2) -0.0082(3) -0.0039(3) C15 0.0344(12) 0.0364(13) 0.0406(13) 0.0109(10) -0.0133(11) -0.0149(10) C22 0.0538(15) 0.0294(13) 0.0517(15) 0.0117(11) -0.0223(13) -0.0078(11) C21 0.0472(15) 0.0351(14) 0.0560(16) 0.0057(12) -0.0174(13) -0.0172(11) C23 0.0399(13) 0.0343(13) 0.0413(14) -0.0086(11) -0.0139(11) -0.0002(10) C13 0.0466(14) 0.0363(14) 0.0391(13) -0.0104(10) -0.0171(11) -0.0018(11) C12 0.0568(16) 0.0509(16) 0.0433(15) -0.0029(12) -0.0273(13) -0.0060(13) C11 0.0472(15) 0.0661(19) 0.0279(13) 0.0029(12) 0.0026(11) -0.0101(13) C101 0.0208(10) 0.0301(11) 0.0285(11) 0.0057(9) -0.0083(9) -0.0050(8) C102 0.0278(11) 0.0323(12) 0.0305(11) 0.0022(9) -0.0085(9) -0.0078(9) C103 0.0326(12) 0.0417(14) 0.0259(11) 0.0002(10) -0.0057(10) -0.0071(10) C104 0.0283(11) 0.0501(15) 0.0316(12) 0.0117(11) -0.0050(10) -0.0126(10) C105 0.0285(11) 0.0328(12) 0.0315(11) 0.0012(9) -0.0091(9) -0.0068(9) C106 0.0212(10) 0.0285(11) 0.0267(10) -0.0005(8) -0.0054(8) -0.0059(8) C107 0.0328(11) 0.0298(12) 0.0328(12) 0.0017(9) -0.0129(10) -0.0076(9) C108 0.0365(12) 0.0282(12) 0.0446(14) -0.0028(10) -0.0132(11) -0.0047(10) C109 0.0401(13) 0.0372(13) 0.0350(12) -0.0095(10) -0.0080(11) -0.0113(10) C110 0.0398(13) 0.0457(15) 0.0322(12) 0.0000(10) -0.0157(11) -0.0119(11) C111 0.0288(11) 0.0327(12) 0.0334(12) 0.0024(9) -0.0114(10) -0.0058(9) C112 0.0232(10) 0.0258(11) 0.0315(11) -0.0007(9) -0.0106(9) -0.0042(8) C113 0.0248(11) 0.0319(12) 0.0383(12) 0.0040(10) -0.0069(10) -0.0046(9) C114 0.0345(12) 0.0323(13) 0.0462(14) 0.0104(11) -0.0120(11) -0.0078(10) C115 0.0332(12) 0.0287(12) 0.0540(15) 0.0051(11) -0.0178(11) -0.0014(10) C116 0.0217(11) 0.0355(13) 0.0478(14) -0.0030(11) -0.0078(10) 0.0003(9) C117 0.0249(11) 0.0337(12) 0.0358(12) 0.0025(10) -0.0066(10) -0.0064(9) C1S 0.064(4) 0.034(2) 0.072(4) 0.013(2) -0.026(3) -0.012(2) C2S 0.095(6) 0.049(3) 0.057(4) 0.010(3) -0.004(4) -0.037(4) C3S 0.094(6) 0.069(5) 0.077(5) -0.008(3) 0.011(4) -0.037(5) C4S 0.064(5) 0.052(4) 0.140(7) -0.009(4) -0.018(5) -0.016(3) C5S 0.071(5) 0.048(3) 0.095(4) 0.012(3) -0.019(4) -0.012(3) C6S 0.046(5) 0.049(3) 0.059(3) 0.015(2) -0.012(3) -0.009(3) C7S 0.083(5) 0.075(4) 0.125(5) 0.029(4) -0.049(4) -0.025(4) C21S 0.067(8) 0.023(5) 0.066(8) -0.006(4) -0.020(6) 0.012(5) C22S 0.066(12) 0.041(7) 0.064(9) 0.009(6) -0.003(7) -0.011(7) C23S 0.16(2) 0.030(7) 0.146(17) 0.018(8) -0.101(16) -0.029(9) C24S 0.061(11) 0.039(7) 0.25(3) -0.012(11) -0.074(15) -0.022(8) C25S 0.071(12) 0.063(8) 0.091(11) 0.004(7) -0.023(8) -0.022(8) C26S 0.041(11) 0.048(7) 0.071(8) 0.006(6) 0.010(7) -0.016(7) C27S 0.071(9) 0.060(8) 0.077(8) 0.002(6) -0.020(7) 0.000(6) _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 Zn1 N10 1.8873(16) . ? Zn1 N1 2.0228(17) . ? Zn1 N1 2.0371(17) 2_656 ? Zn1 Zn1 2.8257(5) 2_656 ? N1 Si1 1.7480(18) . ? N1 Zn1 2.0371(17) 2_656 ? N1 H1 0.76(2) . ? N10 Si20 1.7124(18) . ? N10 Si10 1.7208(17) . ? Si1 C101 1.874(2) . ? Si1 C106 1.875(2) . ? Si1 C112 1.882(2) . ? Si20 C21 1.876(3) . ? Si20 C22 1.877(2) . ? Si20 C23 1.878(2) . ? Si10 C13 1.870(2) . ? Si10 C11 1.871(3) . ? Si10 C12 1.877(3) . ? C15 C104 1.376(3) . ? C15 C105 1.391(3) . ? C15 H15 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C101 C105 1.393(3) . ? C101 C102 1.406(3) . ? C102 C103 1.380(3) . ? C102 H102 0.9500 . ? C103 C104 1.387(3) . ? C103 H103 0.9500 . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C111 1.396(3) . ? C106 C107 1.404(3) . ? C107 C108 1.388(3) . ? C107 H107 0.9500 . ? C108 C109 1.382(3) . ? C108 H108 0.9500 . ? C109 C110 1.380(3) . ? C109 H109 0.9500 . ? C110 C111 1.387(3) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 C117 1.398(3) . ? C112 C113 1.403(3) . ? C113 C114 1.388(3) . ? C113 H113 0.9500 . ? C114 C115 1.385(3) . ? C114 H114 0.9500 . ? C115 C116 1.378(3) . ? C115 H115 0.9500 . ? C116 C117 1.388(3) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C7S 1.456(8) . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S C6S 1.3900 . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C21S C22S 1.3900 . ? C21S C26S 1.3900 . ? C21S C27S 1.518(17) . ? C22S C23S 1.3900 . ? C22S H22S 0.9500 . ? C23S C24S 1.3900 . ? C23S H23S 0.9500 . ? C24S C25S 1.3900 . ? C24S H24S 0.9500 . ? C25S C26S 1.3900 . ? C25S H25S 0.9500 . ? C26S H26S 0.9500 . ? C27S H27A 0.9800 . ? C27S H27B 0.9800 . ? C27S H27C 0.9800 . ? 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 N10 Zn1 N1 132.27(7) . . ? N10 Zn1 N1 135.94(7) . 2_656 ? N1 Zn1 N1 91.79(7) . 2_656 ? N10 Zn1 Zn1 178.37(5) . 2_656 ? N1 Zn1 Zn1 46.10(5) . 2_656 ? N1 Zn1 Zn1 45.69(5) 2_656 2_656 ? Si1 N1 Zn1 119.30(10) . . ? Si1 N1 Zn1 119.18(10) . 2_656 ? Zn1 N1 Zn1 88.21(7) . 2_656 ? Si1 N1 H1 111.3(18) . . ? Zn1 N1 H1 109.6(18) . . ? Zn1 N1 H1 106.9(18) 2_656 . ? Si20 N10 Si10 123.96(10) . . ? Si20 N10 Zn1 121.17(9) . . ? Si10 N10 Zn1 114.52(9) . . ? N1 Si1 C101 111.04(9) . . ? N1 Si1 C106 104.29(9) . . ? C101 Si1 C106 111.15(10) . . ? N1 Si1 C112 113.30(9) . . ? C101 Si1 C112 107.84(9) . . ? C106 Si1 C112 109.24(9) . . ? N10 Si20 C21 113.41(10) . . ? N10 Si20 C22 112.32(10) . . ? C21 Si20 C22 106.36(12) . . ? N10 Si20 C23 110.90(10) . . ? C21 Si20 C23 106.86(12) . . ? C22 Si20 C23 106.58(11) . . ? N10 Si10 C13 109.80(10) . . ? N10 Si10 C11 111.79(11) . . ? C13 Si10 C11 108.07(13) . . ? N10 Si10 C12 112.78(10) . . ? C13 Si10 C12 106.75(12) . . ? C11 Si10 C12 107.41(13) . . ? C104 C15 C105 120.1(2) . . ? C104 C15 H15 119.9 . . ? C105 C15 H15 119.9 . . ? Si20 C22 H22A 109.5 . . ? Si20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si20 C21 H21A 109.5 . . ? Si20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si20 C23 H23A 109.5 . . ? Si20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si10 C13 H13A 109.5 . . ? Si10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si10 C12 H12A 109.5 . . ? Si10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si10 C11 H11A 109.5 . . ? Si10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C105 C101 C102 117.10(19) . . ? C105 C101 Si1 123.56(17) . . ? C102 C101 Si1 119.29(16) . . ? C103 C102 C101 121.5(2) . . ? C103 C102 H102 119.3 . . ? C101 C102 H102 119.3 . . ? C102 C103 C104 120.1(2) . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? C15 C104 C103 119.7(2) . . ? C15 C104 H104 120.1 . . ? C103 C104 H104 120.1 . . ? C15 C105 C101 121.5(2) . . ? C15 C105 H105 119.3 . . ? C101 C105 H105 119.3 . . ? C111 C106 C107 116.69(19) . . ? C111 C106 Si1 122.68(16) . . ? C107 C106 Si1 120.62(16) . . ? C108 C107 C106 121.7(2) . . ? C108 C107 H107 119.1 . . ? C106 C107 H107 119.1 . . ? C109 C108 C107 120.0(2) . . ? C109 C108 H108 120.0 . . ? C107 C108 H108 120.0 . . ? C110 C109 C108 119.5(2) . . ? C110 C109 H109 120.3 . . ? C108 C109 H109 120.3 . . ? C109 C110 C111 120.4(2) . . ? C109 C110 H110 119.8 . . ? C111 C110 H110 119.8 . . ? C110 C111 C106 121.7(2) . . ? C110 C111 H111 119.2 . . ? C106 C111 H111 119.2 . . ? C117 C112 C113 117.14(19) . . ? C117 C112 Si1 121.70(16) . . ? C113 C112 Si1 121.09(15) . . ? C114 C113 C112 121.3(2) . . ? C114 C113 H113 119.4 . . ? C112 C113 H113 119.4 . . ? C115 C114 C113 120.2(2) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C116 C115 C114 119.5(2) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C115 C116 C117 120.3(2) . . ? C115 C116 H116 119.8 . . ? C117 C116 H116 119.8 . . ? C116 C117 C112 121.5(2) . . ? C116 C117 H117 119.3 . . ? C112 C117 H117 119.3 . . ? C2S C1S C6S 120.0 . . ? C2S C1S C7S 119.4(4) . . ? C6S C1S C7S 120.6(4) . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C22S C21S C26S 120.0 . . ? C22S C21S C27S 121.8(8) . . ? C26S C21S C27S 118.2(8) . . ? C23S C22S C21S 120.0 . . ? C23S C22S H22S 120.0 . . ? C21S C22S H22S 120.0 . . ? C22S C23S C24S 120.0 . . ? C22S C23S H23S 120.0 . . ? C24S C23S H23S 120.0 . . ? C25S C24S C23S 120.0 . . ? C25S C24S H24S 120.0 . . ? C23S C24S H24S 120.0 . . ? C24S C25S C26S 120.0 . . ? C24S C25S H25S 120.0 . . ? C26S C25S H25S 120.0 . . ? C25S C26S C21S 120.0 . . ? C25S C26S H26S 120.0 . . ? C21S C26S H26S 120.0 . . ? C21S C27S H27A 109.5 . . ? C21S C27S H27B 109.5 . . ? H27A C27S H27B 109.5 . . ? C21S C27S H27C 109.5 . . ? H27A C27S H27C 109.5 . . ? H27B C27S H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.327 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 960129' ####################################################################### # # 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_h11alj18 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H74 N10 Si6 Zn2' _chemical_formula_weight 802.21 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.05200(10) _cell_length_b 21.7480(3) _cell_length_c 10.9160(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.0760(10) _cell_angle_gamma 90.00 _cell_volume 2108.93(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26367 _cell_measurement_theta_min 3.89 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7310 _exptl_absorpt_correction_T_max 0.7997 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26367 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4834 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0366P)^2^+0.9725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0099(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4834 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Zn1 Zn 0.60023(2) 0.045455(9) 0.567552(19) 0.02042(8) Uani 1 1 d . . . Si20 Si 0.88218(5) 0.11926(2) 0.69457(5) 0.02327(12) Uani 1 1 d . . . Si1 Si 0.35908(6) 0.10587(2) 0.40235(5) 0.02142(12) Uani 1 1 d . . . Si10 Si 0.65012(6) 0.09342(2) 0.84851(5) 0.02360(12) Uani 1 1 d . . . N1 N 0.36789(17) 0.04112(7) 0.49436(14) 0.0200(3) Uani 1 1 d . . . N10 N 0.71002(16) 0.09018(7) 0.70840(14) 0.0203(3) Uani 1 1 d . . . N4 N 0.23890(18) 0.09934(7) 0.26178(15) 0.0266(3) Uani 1 1 d . . . N2 N 0.54889(18) 0.10727(7) 0.37890(15) 0.0255(3) Uani 1 1 d . . . N3 N 0.32115(19) 0.17267(7) 0.47360(15) 0.0297(4) Uani 1 1 d . . . C42 C 0.0938(2) 0.06883(10) 0.2460(2) 0.0337(5) Uani 1 1 d . . . H42A H 0.0152 0.0993 0.2503 0.050 Uiso 1 1 calc R . . H42B H 0.0958 0.0383 0.3123 0.050 Uiso 1 1 calc R . . H42C H 0.0723 0.0483 0.1646 0.050 Uiso 1 1 calc R . . C102 C 0.7254(3) 0.02926(10) 0.9563(2) 0.0367(5) Uani 1 1 d . . . H10A H 0.6969 -0.0102 0.9151 0.055 Uiso 1 1 calc R . . H10B H 0.6834 0.0321 1.0325 0.055 Uiso 1 1 calc R . . H10C H 0.8353 0.0322 0.9779 0.055 Uiso 1 1 calc R . . C201 C 1.0350(2) 0.10240(11) 0.8330(2) 0.0393(5) Uani 1 1 d . . . H20A H 1.0040 0.1169 0.9092 0.059 Uiso 1 1 calc R . . H20B H 1.1277 0.1235 0.8231 0.059 Uiso 1 1 calc R . . H20C H 1.0531 0.0580 0.8389 0.059 Uiso 1 1 calc R . . C103 C 0.4396(2) 0.09104(11) 0.8304(2) 0.0365(5) Uani 1 1 d . . . H10D H 0.3985 0.1324 0.8113 0.055 Uiso 1 1 calc R . . H10E H 0.4128 0.0765 0.9083 0.055 Uiso 1 1 calc R . . H10F H 0.3978 0.0630 0.7623 0.055 Uiso 1 1 calc R . . C203 C 0.9482(2) 0.08498(10) 0.5563(2) 0.0352(5) Uani 1 1 d . . . H20D H 0.9724 0.0414 0.5724 0.053 Uiso 1 1 calc R . . H20E H 1.0382 0.1069 0.5424 0.053 Uiso 1 1 calc R . . H20F H 0.8685 0.0888 0.4820 0.053 Uiso 1 1 calc R . . C22 C 0.5806(2) 0.06739(10) 0.27788(18) 0.0314(4) Uani 1 1 d . . . H22A H 0.5532 0.0889 0.1979 0.047 Uiso 1 1 calc R . . H22B H 0.5217 0.0295 0.2753 0.047 Uiso 1 1 calc R . . H22C H 0.6881 0.0573 0.2933 0.047 Uiso 1 1 calc R . . C32 C 0.1980(3) 0.21378(10) 0.4212(2) 0.0406(5) Uani 1 1 d . . . H32A H 0.1380 0.2229 0.4847 0.061 Uiso 1 1 calc R . . H32B H 0.1341 0.1940 0.3494 0.061 Uiso 1 1 calc R . . H32C H 0.2391 0.2521 0.3943 0.061 Uiso 1 1 calc R . . C31 C 0.4129(3) 0.19887(10) 0.5855(2) 0.0413(5) Uani 1 1 d . . . H31A H 0.4530 0.2387 0.5653 0.062 Uiso 1 1 calc R . . H31B H 0.4964 0.1710 0.6175 0.062 Uiso 1 1 calc R . . H31C H 0.3510 0.2046 0.6491 0.062 Uiso 1 1 calc R . . C101 C 0.7054(3) 0.16695(11) 0.9358(2) 0.0424(5) Uani 1 1 d . . . H10G H 0.8154 0.1703 0.9553 0.064 Uiso 1 1 calc R . . H10H H 0.6662 0.1670 1.0134 0.064 Uiso 1 1 calc R . . H10I H 0.6634 0.2020 0.8841 0.064 Uiso 1 1 calc R . . C41 C 0.2483(3) 0.14177(10) 0.1597(2) 0.0375(5) Uani 1 1 d . . . H41A H 0.2412 0.1186 0.0818 0.056 Uiso 1 1 calc R . . H41B H 0.3446 0.1637 0.1779 0.056 Uiso 1 1 calc R . . H41C H 0.1654 0.1714 0.1511 0.056 Uiso 1 1 calc R . . C21 C 0.6217(3) 0.16759(10) 0.3707(2) 0.0379(5) Uani 1 1 d . . . H21A H 0.7300 0.1617 0.3754 0.057 Uiso 1 1 calc R . . H21B H 0.6054 0.1937 0.4401 0.057 Uiso 1 1 calc R . . H21C H 0.5780 0.1873 0.2914 0.057 Uiso 1 1 calc R . . C202 C 0.8823(2) 0.20539(10) 0.6762(2) 0.0361(5) Uani 1 1 d . . . H20G H 0.8063 0.2172 0.6035 0.054 Uiso 1 1 calc R . . H20H H 0.9818 0.2190 0.6643 0.054 Uiso 1 1 calc R . . H20I H 0.8588 0.2247 0.7513 0.054 Uiso 1 1 calc R . . H1 H 0.307(3) 0.0406(11) 0.546(2) 0.041(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02029(12) 0.01890(12) 0.02022(12) -0.00244(8) -0.00076(8) -0.00192(7) Si20 0.0200(2) 0.0231(3) 0.0253(3) -0.0020(2) 0.0010(2) -0.00320(19) Si1 0.0255(3) 0.0180(2) 0.0186(2) 0.00006(19) -0.00119(19) 0.00096(19) Si10 0.0281(3) 0.0218(3) 0.0207(3) -0.00272(19) 0.0044(2) 0.00059(19) N1 0.0207(7) 0.0197(8) 0.0182(7) 0.0000(6) 0.0003(6) 0.0002(6) N10 0.0203(7) 0.0207(7) 0.0187(7) -0.0026(6) 0.0005(6) -0.0018(6) N4 0.0300(8) 0.0246(8) 0.0217(8) 0.0034(6) -0.0034(7) -0.0014(6) N2 0.0292(8) 0.0233(8) 0.0235(8) -0.0026(6) 0.0038(6) -0.0055(6) N3 0.0387(9) 0.0209(8) 0.0263(8) -0.0023(7) -0.0019(7) 0.0071(7) C42 0.0299(10) 0.0366(12) 0.0301(11) -0.0002(9) -0.0051(8) -0.0013(9) C102 0.0504(13) 0.0346(11) 0.0250(10) 0.0037(9) 0.0072(9) 0.0053(10) C201 0.0231(10) 0.0456(13) 0.0441(13) 0.0010(10) -0.0062(9) -0.0029(9) C103 0.0354(11) 0.0384(12) 0.0394(12) 0.0007(10) 0.0161(10) 0.0025(9) C203 0.0353(11) 0.0344(11) 0.0393(12) -0.0024(9) 0.0158(9) -0.0030(9) C22 0.0358(11) 0.0349(11) 0.0232(10) -0.0012(8) 0.0052(8) -0.0021(9) C32 0.0461(13) 0.0282(11) 0.0435(13) -0.0033(10) -0.0016(10) 0.0136(9) C31 0.0566(14) 0.0297(11) 0.0323(11) -0.0094(9) -0.0043(10) 0.0108(10) C101 0.0588(15) 0.0338(12) 0.0356(12) -0.0134(10) 0.0120(11) -0.0033(10) C41 0.0459(12) 0.0334(11) 0.0282(10) 0.0084(9) -0.0058(9) -0.0008(9) C21 0.0417(12) 0.0309(11) 0.0397(12) 0.0018(9) 0.0044(10) -0.0126(9) C202 0.0373(11) 0.0285(11) 0.0413(12) -0.0006(9) 0.0046(10) -0.0082(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N10 1.9264(14) . ? Zn1 N1 2.0397(15) 3_656 ? Zn1 N1 2.1035(15) . ? Zn1 N2 2.4282(16) . ? Zn1 Si1 2.8689(5) . ? Zn1 Zn1 2.8893(4) 3_656 ? Si20 N10 1.7152(15) . ? Si20 C201 1.879(2) . ? Si20 C203 1.881(2) . ? Si20 C202 1.884(2) . ? Si1 N4 1.7079(16) . ? Si1 N3 1.7135(17) . ? Si1 N1 1.7225(15) . ? Si1 N2 1.7854(17) . ? Si10 N10 1.7195(16) . ? Si10 C102 1.868(2) . ? Si10 C103 1.878(2) . ? Si10 C101 1.879(2) . ? N1 Zn1 2.0397(15) 3_656 ? N1 H1 0.86(3) . ? N4 C42 1.452(3) . ? N4 C41 1.462(3) . ? N2 C22 1.474(2) . ? N2 C21 1.479(2) . ? N3 C31 1.455(3) . ? N3 C32 1.457(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C203 H20D 0.9800 . ? C203 H20E 0.9800 . ? C203 H20F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C101 H10I 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C202 H20G 0.9800 . ? C202 H20H 0.9800 . ? C202 H20I 0.9800 . ? 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 N10 Zn1 N1 130.28(6) . 3_656 ? N10 Zn1 N1 130.59(6) . . ? N1 Zn1 N1 91.58(6) 3_656 . ? N10 Zn1 N2 112.50(6) . . ? N1 Zn1 N2 104.26(6) 3_656 . ? N1 Zn1 N2 71.83(6) . . ? N10 Zn1 Si1 118.95(5) . . ? N1 Zn1 Si1 110.70(4) 3_656 . ? N1 Zn1 Si1 36.61(4) . . ? N2 Zn1 Si1 38.26(4) . . ? N10 Zn1 Zn1 158.44(5) . 3_656 ? N1 Zn1 Zn1 46.70(4) 3_656 3_656 ? N1 Zn1 Zn1 44.88(4) . 3_656 ? N2 Zn1 Zn1 86.95(4) . 3_656 ? Si1 Zn1 Zn1 70.435(12) . 3_656 ? N10 Si20 C201 113.48(9) . . ? N10 Si20 C203 111.02(9) . . ? C201 Si20 C203 105.64(11) . . ? N10 Si20 C202 113.26(9) . . ? C201 Si20 C202 105.32(10) . . ? C203 Si20 C202 107.59(10) . . ? N4 Si1 N3 109.25(8) . . ? N4 Si1 N1 113.96(8) . . ? N3 Si1 N1 114.79(8) . . ? N4 Si1 N2 109.70(8) . . ? N3 Si1 N2 109.44(8) . . ? N1 Si1 N2 99.18(8) . . ? N4 Si1 Zn1 143.43(6) . . ? N3 Si1 Zn1 107.31(6) . . ? N1 Si1 Zn1 46.74(5) . . ? N2 Si1 Zn1 57.38(5) . . ? N10 Si10 C102 113.00(9) . . ? N10 Si10 C103 113.10(9) . . ? C102 Si10 C103 106.59(11) . . ? N10 Si10 C101 112.76(9) . . ? C102 Si10 C101 106.68(11) . . ? C103 Si10 C101 104.04(11) . . ? Si1 N1 Zn1 123.71(9) . 3_656 ? Si1 N1 Zn1 96.65(7) . . ? Zn1 N1 Zn1 88.42(6) 3_656 . ? Si1 N1 H1 115.5(17) . . ? Zn1 N1 H1 110.8(16) 3_656 . ? Zn1 N1 H1 117.9(17) . . ? Si20 N10 Si10 120.69(9) . . ? Si20 N10 Zn1 117.01(8) . . ? Si10 N10 Zn1 121.87(8) . . ? C42 N4 C41 112.45(16) . . ? C42 N4 Si1 123.39(14) . . ? C41 N4 Si1 120.79(13) . . ? C22 N2 C21 108.89(16) . . ? C22 N2 Si1 115.37(13) . . ? C21 N2 Si1 118.44(14) . . ? C22 N2 Zn1 106.01(12) . . ? C21 N2 Zn1 121.83(13) . . ? Si1 N2 Zn1 84.35(6) . . ? C31 N3 C32 111.06(16) . . ? C31 N3 Si1 125.55(14) . . ? C32 N3 Si1 123.15(14) . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si10 C102 H10A 109.5 . . ? Si10 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? Si10 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? Si20 C201 H20A 109.5 . . ? Si20 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? Si20 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? Si10 C103 H10D 109.5 . . ? Si10 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? Si10 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? Si20 C203 H20D 109.5 . . ? Si20 C203 H20E 109.5 . . ? H20D C203 H20E 109.5 . . ? Si20 C203 H20F 109.5 . . ? H20D C203 H20F 109.5 . . ? H20E C203 H20F 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si10 C101 H10G 109.5 . . ? Si10 C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? Si10 C101 H10I 109.5 . . ? H10G C101 H10I 109.5 . . ? H10H C101 H10I 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si20 C202 H20G 109.5 . . ? Si20 C202 H20H 109.5 . . ? H20G C202 H20H 109.5 . . ? Si20 C202 H20I 109.5 . . ? H20G C202 H20I 109.5 . . ? H20H C202 H20I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.356 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 960130' ####################################################################### # # 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_k11alj28 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 N8 Si2 Zn2' _chemical_formula_weight 539.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 7.9730(2) _cell_length_b 18.1740(4) _cell_length_c 9.3130(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.8530(10) _cell_angle_gamma 90.00 _cell_volume 1333.39(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24560 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.907 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24560 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3061 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0279P)^2^+0.6853P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3061 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Zn1 Zn 0.56567(3) 0.062821(11) 0.08918(2) 0.02071(8) Uani 1 1 d . . . Si1 Si 0.75823(6) -0.09176(3) 0.07202(5) 0.02006(12) Uani 1 1 d . . . N1 N 0.6774(2) -0.01508(8) -0.01870(17) 0.0199(3) Uani 1 1 d . . . N3 N 0.8700(2) -0.14394(9) -0.03378(18) 0.0259(3) Uani 1 1 d . . . N2 N 0.56806(19) -0.13700(8) 0.10024(16) 0.0219(3) Uani 1 1 d . . . N4 N 0.8759(2) -0.07538(9) 0.23861(18) 0.0265(4) Uani 1 1 d . . . C21 C 0.4930(3) -0.11976(11) 0.2310(2) 0.0282(4) Uani 1 1 d . . . H21A H 0.3699 -0.1271 0.2107 0.042 Uiso 1 1 calc R . . H21B H 0.5173 -0.0684 0.2590 0.042 Uiso 1 1 calc R . . H21C H 0.5418 -0.1522 0.3106 0.042 Uiso 1 1 calc R . . C42 C 0.9926(2) -0.01354(11) 0.2635(2) 0.0295(4) Uani 1 1 d . . . H42A H 0.9742 0.0125 0.3519 0.044 Uiso 1 1 calc R . . H42B H 0.9724 0.0201 0.1805 0.044 Uiso 1 1 calc R . . H42C H 1.1097 -0.0316 0.2750 0.044 Uiso 1 1 calc R . . C1 C 0.6495(2) 0.12036(11) 0.2672(2) 0.0274(4) Uani 1 1 d . . . H1A H 0.7723 0.1298 0.2699 0.033 Uiso 1 1 calc R . . H1B H 0.5912 0.1686 0.2602 0.033 Uiso 1 1 calc R . . C22 C 0.5472(3) -0.21551(11) 0.0661(2) 0.0308(4) Uani 1 1 d . . . H22A H 0.6073 -0.2446 0.1466 0.046 Uiso 1 1 calc R . . H22B H 0.5941 -0.2263 -0.0229 0.046 Uiso 1 1 calc R . . H22C H 0.4263 -0.2281 0.0517 0.046 Uiso 1 1 calc R . . C2 C 0.6238(3) 0.08372(14) 0.4100(2) 0.0405(5) Uani 1 1 d . . . H2A H 0.5024 0.0753 0.4100 0.061 Uiso 1 1 calc R . . H2B H 0.6684 0.1158 0.4915 0.061 Uiso 1 1 calc R . . H2C H 0.6840 0.0366 0.4199 0.061 Uiso 1 1 calc R . . C31 C 0.8140(3) -0.15760(12) -0.1881(2) 0.0348(5) Uani 1 1 d . . . H31A H 0.9082 -0.1485 -0.2420 0.052 Uiso 1 1 calc R . . H31B H 0.7194 -0.1247 -0.2238 0.052 Uiso 1 1 calc R . . H31C H 0.7767 -0.2088 -0.2021 0.052 Uiso 1 1 calc R . . C32 C 1.0110(3) -0.19133(13) 0.0247(3) 0.0422(6) Uani 1 1 d . . . H32A H 0.9731 -0.2427 0.0203 0.063 Uiso 1 1 calc R . . H32B H 1.0515 -0.1778 0.1260 0.063 Uiso 1 1 calc R . . H32C H 1.1033 -0.1855 -0.0327 0.063 Uiso 1 1 calc R . . C41 C 0.8998(3) -0.12869(13) 0.3560(3) 0.0408(5) Uani 1 1 d . . . H41A H 1.0195 -0.1433 0.3756 0.061 Uiso 1 1 calc R . . H41B H 0.8293 -0.1721 0.3280 0.061 Uiso 1 1 calc R . . H41C H 0.8669 -0.1067 0.4436 0.061 Uiso 1 1 calc R . . H1N H 0.728(3) 0.0012(12) -0.072(2) 0.026(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02312(13) 0.01944(12) 0.01920(12) -0.00298(8) 0.00208(8) -0.00009(8) Si1 0.0212(2) 0.0183(2) 0.0204(3) 0.00015(19) 0.00241(19) 0.00104(19) N1 0.0222(8) 0.0194(7) 0.0186(8) 0.0015(6) 0.0052(6) -0.0004(6) N3 0.0237(8) 0.0254(8) 0.0285(9) -0.0015(7) 0.0040(7) 0.0047(6) N2 0.0257(8) 0.0178(7) 0.0230(8) 0.0004(6) 0.0060(7) -0.0007(6) N4 0.0291(9) 0.0255(8) 0.0231(8) 0.0039(6) -0.0014(7) -0.0020(7) C21 0.0312(10) 0.0312(10) 0.0234(10) 0.0039(8) 0.0080(8) 0.0001(8) C42 0.0257(10) 0.0341(11) 0.0275(10) -0.0017(8) -0.0002(8) -0.0039(8) C1 0.0266(10) 0.0292(10) 0.0260(10) -0.0086(8) 0.0027(8) -0.0018(8) C22 0.0318(11) 0.0216(10) 0.0394(12) 0.0022(8) 0.0069(9) -0.0010(8) C2 0.0385(12) 0.0575(15) 0.0244(11) -0.0049(10) 0.0014(9) 0.0014(11) C31 0.0324(11) 0.0372(12) 0.0362(12) -0.0119(9) 0.0097(9) 0.0019(9) C32 0.0365(12) 0.0417(13) 0.0491(14) 0.0026(11) 0.0086(11) 0.0170(10) C41 0.0423(13) 0.0420(13) 0.0329(12) 0.0132(10) -0.0106(10) -0.0058(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 1.9867(19) . ? Zn1 N1 2.0208(15) . ? Zn1 N1 2.1327(16) 3_655 ? Zn1 N2 2.3425(15) 3_655 ? Si1 N1 1.7039(16) . ? Si1 N4 1.7111(17) . ? Si1 N3 1.7129(16) . ? Si1 N2 1.7795(15) . ? Si1 Zn1 2.8295(5) 3_655 ? N1 Zn1 2.1327(16) 3_655 ? N1 H1N 0.74(2) . ? N3 C32 1.454(3) . ? N3 C31 1.459(3) . ? N2 C22 1.466(2) . ? N2 C21 1.471(2) . ? N2 Zn1 2.3425(15) 3_655 ? N4 C41 1.451(3) . ? N4 C42 1.454(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C1 C2 1.529(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? 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 C1 Zn1 N1 131.76(7) . . ? C1 Zn1 N1 130.10(7) . 3_655 ? N1 Zn1 N1 90.65(6) . 3_655 ? C1 Zn1 N2 112.40(7) . 3_655 ? N1 Zn1 N2 102.31(6) . 3_655 ? N1 Zn1 N2 73.48(6) 3_655 3_655 ? N1 Si1 N4 114.84(8) . . ? N1 Si1 N3 110.97(8) . . ? N4 Si1 N3 110.90(8) . . ? N1 Si1 N2 100.69(8) . . ? N4 Si1 N2 107.90(8) . . ? N3 Si1 N2 111.07(8) . . ? N1 Si1 Zn1 48.73(5) . 3_655 ? N4 Si1 Zn1 140.99(6) . 3_655 ? N3 Si1 Zn1 108.10(6) . 3_655 ? N2 Si1 Zn1 55.63(5) . 3_655 ? Si1 N1 Zn1 119.24(9) . . ? Si1 N1 Zn1 94.37(7) . 3_655 ? Zn1 N1 Zn1 89.35(6) . 3_655 ? Si1 N1 H1N 116.9(17) . . ? Zn1 N1 H1N 112.1(17) . . ? Zn1 N1 H1N 121.0(17) 3_655 . ? C32 N3 C31 111.72(17) . . ? C32 N3 Si1 123.57(15) . . ? C31 N3 Si1 123.61(13) . . ? C22 N2 C21 109.87(15) . . ? C22 N2 Si1 119.25(12) . . ? C21 N2 Si1 119.22(12) . . ? C22 N2 Zn1 111.94(12) . 3_655 ? C21 N2 Zn1 107.76(11) . 3_655 ? Si1 N2 Zn1 85.54(6) . 3_655 ? C41 N4 C42 112.89(16) . . ? C41 N4 Si1 123.85(14) . . ? C42 N4 Si1 121.81(13) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C2 C1 Zn1 115.05(14) . . ? C2 C1 H1A 108.5 . . ? Zn1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? Zn1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.537 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 960131' ####################################################################### # # 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_h11alj22 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H110 N18 Si8 Zn4' _chemical_formula_weight 1281.62 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.8580(4) _cell_length_b 18.2210(4) _cell_length_c 15.5450(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.7600(10) _cell_angle_gamma 90.00 _cell_volume 6638.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52385 _cell_measurement_theta_min 3.48 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7387 _exptl_absorpt_correction_T_max 0.8178 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 52385 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7541 _reflns_number_gt 5644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 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^)+(0.0371P)^2^+7.4212P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7541 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Zn1 Zn 0.508596(11) 0.299835(14) 0.338294(17) 0.02753(8) Uani 1 1 d . . . Zn2 Zn 0.403795(11) 0.226399(15) 0.303040(17) 0.02799(8) Uani 1 1 d . . . N1 N 0.43425(8) 0.30932(10) 0.24859(12) 0.0285(4) Uani 1 1 d . . . N2 N 0.44202(10) 0.39172(12) 0.10478(14) 0.0409(5) Uani 1 1 d . . . N3 N 0.38713(12) 0.45703(13) 0.23284(16) 0.0538(7) Uani 1 1 d . . . N4 N 0.33132(10) 0.34391(15) 0.13210(14) 0.0493(6) Uani 1 1 d . . . N5 N 0.47986(8) 0.21181(11) 0.39565(12) 0.0278(4) Uani 1 1 d . . . N6 N 0.54302(10) 0.22855(15) 0.56884(14) 0.0500(6) Uani 1 1 d . . . N7 N 0.42657(10) 0.26212(13) 0.52883(14) 0.0429(5) Uani 1 1 d . . . N8 N 0.46520(10) 0.11543(13) 0.53259(15) 0.0466(6) Uani 1 1 d . . . N10 N 0.33957(8) 0.16127(12) 0.28431(13) 0.0354(5) Uani 1 1 d . . . Si1 Si 0.39632(3) 0.37393(4) 0.18587(4) 0.03719(17) Uani 1 1 d . . . Si2 Si 0.47863(3) 0.20394(4) 0.50626(4) 0.03335(16) Uani 1 1 d . . . Si10 Si 0.28012(3) 0.18952(5) 0.32203(5) 0.0451(2) Uani 1 1 d . . . Si20 Si 0.34695(3) 0.08311(4) 0.22736(5) 0.04475(19) Uani 1 1 d . . . C21 C 0.48044(15) 0.45612(16) 0.1179(2) 0.0568(8) Uani 1 1 d . . . H21A H 0.5095 0.4511 0.0813 0.085 Uiso 1 1 calc R . . H21B H 0.4990 0.4590 0.1796 0.085 Uiso 1 1 calc R . . H21C H 0.4582 0.5009 0.1016 0.085 Uiso 1 1 calc R . . C22 C 0.41361(14) 0.38905(19) 0.01161(18) 0.0572(8) Uani 1 1 d . . . H22A H 0.3884 0.4316 -0.0019 0.086 Uiso 1 1 calc R . . H22B H 0.3911 0.3439 0.0007 0.086 Uiso 1 1 calc R . . H22C H 0.4425 0.3898 -0.0256 0.086 Uiso 1 1 calc R . . C31 C 0.37323(15) 0.46239(18) 0.3201(2) 0.0616(9) Uani 1 1 d . . . H31A H 0.3938 0.5040 0.3514 0.092 Uiso 1 1 calc R . . H31B H 0.3845 0.4170 0.3526 0.092 Uiso 1 1 calc R . . H31C H 0.3321 0.4698 0.3151 0.092 Uiso 1 1 calc R . . C32 C 0.3700(2) 0.5237(2) 0.1815(3) 0.0899(14) Uani 1 1 d . . . H32A H 0.3315 0.5380 0.1883 0.135 Uiso 1 1 calc R . . H32B H 0.3703 0.5141 0.1195 0.135 Uiso 1 1 calc R . . H32C H 0.3967 0.5635 0.2023 0.135 Uiso 1 1 calc R . . C41 C 0.32229(13) 0.27319(19) 0.0895(2) 0.0575(8) Uani 1 1 d . . . H41A H 0.2933 0.2459 0.1136 0.086 Uiso 1 1 calc R . . H41B H 0.3581 0.2455 0.0997 0.086 Uiso 1 1 calc R . . H41C H 0.3093 0.2802 0.0265 0.086 Uiso 1 1 calc R . . C42 C 0.27873(16) 0.3870(3) 0.1186(3) 0.0884(14) Uani 1 1 d . . . H42A H 0.2692 0.4028 0.0574 0.133 Uiso 1 1 calc R . . H42B H 0.2841 0.4302 0.1568 0.133 Uiso 1 1 calc R . . H42C H 0.2476 0.3569 0.1327 0.133 Uiso 1 1 calc R . . C61 C 0.54813(16) 0.2646(2) 0.6542(2) 0.0732(11) Uani 1 1 d . . . H61A H 0.5555 0.2276 0.7007 0.110 Uiso 1 1 calc R . . H61B H 0.5125 0.2904 0.6573 0.110 Uiso 1 1 calc R . . H61C H 0.5797 0.2997 0.6617 0.110 Uiso 1 1 calc R . . C62 C 0.59466(13) 0.1884(2) 0.5599(2) 0.0641(9) Uani 1 1 d . . . H62A H 0.6272 0.2221 0.5686 0.096 Uiso 1 1 calc R . . H62B H 0.5898 0.1668 0.5013 0.096 Uiso 1 1 calc R . . H62C H 0.6016 0.1493 0.6039 0.096 Uiso 1 1 calc R . . C71 C 0.39042(14) 0.2434(2) 0.5919(2) 0.0623(9) Uani 1 1 d . . . H71A H 0.4048 0.2681 0.6477 0.093 Uiso 1 1 calc R . . H71B H 0.3910 0.1901 0.6010 0.093 Uiso 1 1 calc R . . H71C H 0.3512 0.2593 0.5694 0.093 Uiso 1 1 calc R . . C72 C 0.42925(15) 0.34050(16) 0.5159(2) 0.0578(8) Uani 1 1 d . . . H72A H 0.3905 0.3603 0.5004 0.087 Uiso 1 1 calc R . . H72B H 0.4501 0.3507 0.4686 0.087 Uiso 1 1 calc R . . H72C H 0.4490 0.3637 0.5701 0.087 Uiso 1 1 calc R . . C81 C 0.48561(15) 0.0869(2) 0.6211(2) 0.0702(10) Uani 1 1 d . . . H81A H 0.4548 0.0895 0.6548 0.105 Uiso 1 1 calc R . . H81B H 0.5180 0.1164 0.6502 0.105 Uiso 1 1 calc R . . H81C H 0.4976 0.0357 0.6176 0.105 Uiso 1 1 calc R . . C82 C 0.42159(14) 0.06960(17) 0.4835(2) 0.0574(8) Uani 1 1 d . . . H82A H 0.4366 0.0198 0.4797 0.086 Uiso 1 1 calc R . . H82B H 0.4098 0.0897 0.4244 0.086 Uiso 1 1 calc R . . H82C H 0.3887 0.0680 0.5128 0.086 Uiso 1 1 calc R . . C101 C 0.26831(13) 0.1372(2) 0.4208(2) 0.0652(9) Uani 1 1 d . . . H10D H 0.2675 0.0845 0.4080 0.098 Uiso 1 1 calc R . . H10E H 0.2319 0.1520 0.4360 0.098 Uiso 1 1 calc R . . H10F H 0.2994 0.1477 0.4700 0.098 Uiso 1 1 calc R . . C102 C 0.21284(12) 0.1807(2) 0.2382(2) 0.0670(10) Uani 1 1 d . . . H10G H 0.2155 0.2116 0.1876 0.101 Uiso 1 1 calc R . . H10H H 0.1803 0.1964 0.2638 0.101 Uiso 1 1 calc R . . H10I H 0.2076 0.1294 0.2195 0.101 Uiso 1 1 calc R . . C103 C 0.28814(15) 0.2889(2) 0.3525(3) 0.0686(10) Uani 1 1 d . . . H10A H 0.3229 0.2957 0.3966 0.103 Uiso 1 1 calc R . . H10B H 0.2550 0.3049 0.3766 0.103 Uiso 1 1 calc R . . H10C H 0.2907 0.3180 0.3004 0.103 Uiso 1 1 calc R . . C201 C 0.33166(19) -0.00310(19) 0.2837(3) 0.0827(12) Uani 1 1 d . . . H20D H 0.3566 -0.0059 0.3413 0.124 Uiso 1 1 calc R . . H20E H 0.3386 -0.0455 0.2484 0.124 Uiso 1 1 calc R . . H20F H 0.2917 -0.0031 0.2909 0.124 Uiso 1 1 calc R . . C202 C 0.30114(19) 0.0771(2) 0.1161(2) 0.0866(12) Uani 1 1 d . . . H20G H 0.2609 0.0793 0.1214 0.130 Uiso 1 1 calc R . . H20H H 0.3086 0.0307 0.0885 0.130 Uiso 1 1 calc R . . H20I H 0.3099 0.1181 0.0801 0.130 Uiso 1 1 calc R . . C203 C 0.42217(15) 0.0796(2) 0.2106(3) 0.0812(13) Uani 1 1 d . . . H20A H 0.4305 0.1237 0.1792 0.122 Uiso 1 1 calc R . . H20B H 0.4276 0.0360 0.1762 0.122 Uiso 1 1 calc R . . H20C H 0.4479 0.0773 0.2675 0.122 Uiso 1 1 calc R . . H5 H 0.4954(12) 0.1726(16) 0.3825(18) 0.042(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03074(15) 0.02892(15) 0.02258(14) -0.00160(11) 0.00406(11) -0.00414(11) Zn2 0.02433(14) 0.03256(15) 0.02699(14) -0.00084(11) 0.00460(10) 0.00081(11) N1 0.0316(11) 0.0289(10) 0.0246(10) 0.0009(8) 0.0044(8) 0.0050(8) N2 0.0541(14) 0.0364(12) 0.0327(11) 0.0108(9) 0.0092(10) 0.0135(10) N3 0.0782(18) 0.0393(13) 0.0489(14) 0.0075(11) 0.0245(13) 0.0266(12) N4 0.0369(12) 0.0718(17) 0.0370(12) 0.0041(12) 0.0013(10) 0.0233(12) N5 0.0271(10) 0.0306(11) 0.0255(10) 0.0021(8) 0.0045(8) 0.0007(9) N6 0.0395(13) 0.0797(18) 0.0284(12) 0.0048(12) 0.0004(10) -0.0043(12) N7 0.0457(13) 0.0522(14) 0.0333(12) -0.0012(10) 0.0138(10) 0.0014(11) N8 0.0467(13) 0.0524(14) 0.0415(13) 0.0194(11) 0.0101(11) -0.0002(11) N10 0.0236(10) 0.0452(12) 0.0371(11) -0.0035(10) 0.0052(9) -0.0035(9) Si1 0.0437(4) 0.0375(4) 0.0308(4) 0.0054(3) 0.0079(3) 0.0172(3) Si2 0.0315(4) 0.0434(4) 0.0246(3) 0.0064(3) 0.0038(3) -0.0009(3) Si10 0.0249(4) 0.0655(5) 0.0457(4) -0.0005(4) 0.0088(3) 0.0009(3) Si20 0.0369(4) 0.0449(4) 0.0527(5) -0.0092(4) 0.0091(3) -0.0111(3) C21 0.079(2) 0.0368(16) 0.0587(19) 0.0127(14) 0.0244(17) 0.0083(15) C22 0.070(2) 0.069(2) 0.0335(15) 0.0171(14) 0.0121(14) 0.0262(17) C31 0.080(2) 0.0555(19) 0.0542(19) -0.0075(16) 0.0252(17) 0.0190(17) C32 0.138(4) 0.056(2) 0.087(3) 0.024(2) 0.048(3) 0.054(2) C41 0.0422(17) 0.083(2) 0.0432(17) -0.0008(16) -0.0031(13) 0.0045(16) C42 0.059(2) 0.123(4) 0.075(3) -0.005(2) -0.0083(19) 0.051(2) C61 0.066(2) 0.118(3) 0.0311(15) -0.0073(18) -0.0024(15) -0.022(2) C62 0.0377(17) 0.095(3) 0.0544(19) 0.0172(18) -0.0037(14) 0.0016(16) C71 0.0550(19) 0.093(3) 0.0442(17) 0.0045(17) 0.0226(15) 0.0097(18) C72 0.073(2) 0.0461(18) 0.0586(19) -0.0080(15) 0.0225(17) 0.0050(16) C81 0.071(2) 0.084(3) 0.055(2) 0.0377(19) 0.0097(17) 0.0002(19) C82 0.062(2) 0.0483(18) 0.062(2) 0.0125(15) 0.0128(16) -0.0103(15) C101 0.0411(17) 0.103(3) 0.0553(19) 0.0076(19) 0.0185(15) 0.0006(17) C102 0.0269(15) 0.111(3) 0.061(2) 0.012(2) 0.0043(14) 0.0022(17) C103 0.055(2) 0.076(2) 0.081(3) -0.0131(19) 0.0285(19) 0.0122(17) C201 0.105(3) 0.055(2) 0.088(3) -0.008(2) 0.019(2) -0.029(2) C202 0.100(3) 0.086(3) 0.065(2) -0.026(2) -0.009(2) -0.011(2) C203 0.061(2) 0.063(2) 0.132(4) -0.048(2) 0.049(2) -0.0133(18) _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 Zn1 N5 2.0164(19) . ? Zn1 N1 2.0487(19) . ? Zn1 N1 2.0979(19) 2_655 ? Zn1 N2 2.141(2) 2_655 ? Zn2 N10 1.917(2) . ? Zn2 N1 1.9382(19) . ? Zn2 N5 2.1121(19) . ? N1 Si1 1.681(2) . ? N1 Zn1 2.0979(19) 2_655 ? N2 C21 1.480(4) . ? N2 C22 1.481(4) . ? N2 Si1 1.843(2) . ? N2 Zn1 2.141(2) 2_655 ? N3 C31 1.459(4) . ? N3 C32 1.469(4) . ? N3 Si1 1.713(2) . ? N4 C41 1.446(4) . ? N4 C42 1.461(4) . ? N4 Si1 1.708(3) . ? N5 Si2 1.731(2) . ? N5 H5 0.85(3) . ? N6 C62 1.462(4) . ? N6 C61 1.465(4) . ? N6 Si2 1.717(2) . ? N7 C72 1.445(4) . ? N7 C71 1.463(4) . ? N7 Si2 1.718(2) . ? N8 C82 1.438(4) . ? N8 C81 1.467(4) . ? N8 Si2 1.709(2) . ? N10 Si20 1.703(2) . ? N10 Si10 1.712(2) . ? Si1 Zn1 2.7255(7) 2_655 ? Si10 C103 1.873(4) . ? Si10 C101 1.873(3) . ? Si10 C102 1.876(3) . ? Si20 C203 1.862(3) . ? Si20 C201 1.867(4) . ? Si20 C202 1.869(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C102 H10I 0.9800 . ? C103 H10A 0.9800 . ? C103 H10B 0.9800 . ? C103 H10C 0.9800 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 0.9800 . ? C202 H20G 0.9800 . ? C202 H20H 0.9800 . ? C202 H20I 0.9800 . ? C203 H20A 0.9800 . ? C203 H20B 0.9800 . ? C203 H20C 0.9800 . ? 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 N5 Zn1 N1 92.60(8) . . ? N5 Zn1 N1 131.74(8) . 2_655 ? N1 Zn1 N1 98.00(7) . 2_655 ? N5 Zn1 N2 130.20(8) . 2_655 ? N1 Zn1 N2 123.71(8) . 2_655 ? N1 Zn1 N2 80.10(8) 2_655 2_655 ? N10 Zn2 N1 140.39(9) . . ? N10 Zn2 N5 125.90(8) . . ? N1 Zn2 N5 92.94(8) . . ? Si1 N1 Zn2 126.45(11) . . ? Si1 N1 Zn1 139.27(12) . . ? Zn2 N1 Zn1 89.11(8) . . ? Si1 N1 Zn1 91.63(9) . 2_655 ? Zn2 N1 Zn1 123.96(9) . 2_655 ? Zn1 N1 Zn1 81.20(7) . 2_655 ? C21 N2 C22 108.7(2) . . ? C21 N2 Si1 118.37(18) . . ? C22 N2 Si1 116.23(19) . . ? C21 N2 Zn1 106.50(17) . 2_655 ? C22 N2 Zn1 119.64(17) . 2_655 ? Si1 N2 Zn1 85.98(8) . 2_655 ? C31 N3 C32 111.2(2) . . ? C31 N3 Si1 121.7(2) . . ? C32 N3 Si1 123.0(2) . . ? C41 N4 C42 111.3(3) . . ? C41 N4 Si1 123.59(19) . . ? C42 N4 Si1 125.1(3) . . ? Si2 N5 Zn1 125.12(11) . . ? Si2 N5 Zn2 121.04(11) . . ? Zn1 N5 Zn2 85.31(7) . . ? Si2 N5 H5 105.1(19) . . ? Zn1 N5 H5 111.3(19) . . ? Zn2 N5 H5 107.5(19) . . ? C62 N6 C61 112.4(3) . . ? C62 N6 Si2 119.8(2) . . ? C61 N6 Si2 123.0(2) . . ? C72 N7 C71 111.8(2) . . ? C72 N7 Si2 121.95(19) . . ? C71 N7 Si2 122.1(2) . . ? C82 N8 C81 111.9(2) . . ? C82 N8 Si2 124.78(19) . . ? C81 N8 Si2 121.0(2) . . ? Si20 N10 Si10 127.02(12) . . ? Si20 N10 Zn2 116.05(11) . . ? Si10 N10 Zn2 116.86(12) . . ? N1 Si1 N4 113.62(12) . . ? N1 Si1 N3 118.01(11) . . ? N4 Si1 N3 108.35(13) . . ? N1 Si1 N2 101.35(10) . . ? N4 Si1 N2 108.70(11) . . ? N3 Si1 N2 105.98(12) . . ? N1 Si1 Zn1 50.30(7) . 2_655 ? N4 Si1 Zn1 118.48(8) . 2_655 ? N3 Si1 Zn1 132.28(10) . 2_655 ? N2 Si1 Zn1 51.60(7) . 2_655 ? N8 Si2 N6 107.38(12) . . ? N8 Si2 N7 111.00(11) . . ? N6 Si2 N7 109.12(12) . . ? N8 Si2 N5 110.78(11) . . ? N6 Si2 N5 111.21(10) . . ? N7 Si2 N5 107.38(11) . . ? N10 Si10 C103 109.00(13) . . ? N10 Si10 C101 112.88(13) . . ? C103 Si10 C101 107.97(17) . . ? N10 Si10 C102 113.11(13) . . ? C103 Si10 C102 107.01(18) . . ? C101 Si10 C102 106.60(15) . . ? N10 Si20 C203 107.29(13) . . ? N10 Si20 C201 114.31(15) . . ? C203 Si20 C201 108.3(2) . . ? N10 Si20 C202 115.52(16) . . ? C203 Si20 C202 106.3(2) . . ? C201 Si20 C202 104.64(19) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C61 H61A 109.5 . . ? N6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N6 C62 H62A 109.5 . . ? N6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N7 C71 H71A 109.5 . . ? N7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N7 C72 H72A 109.5 . . ? N7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N8 C81 H81A 109.5 . . ? N8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N8 C82 H82A 109.5 . . ? N8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? Si10 C101 H10D 109.5 . . ? Si10 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? Si10 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? Si10 C102 H10G 109.5 . . ? Si10 C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? Si10 C102 H10I 109.5 . . ? H10G C102 H10I 109.5 . . ? H10H C102 H10I 109.5 . . ? Si10 C103 H10A 109.5 . . ? Si10 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? Si10 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 109.5 . . ? Si20 C201 H20D 109.5 . . ? Si20 C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? Si20 C201 H20F 109.5 . . ? H20D C201 H20F 109.5 . . ? H20E C201 H20F 109.5 . . ? Si20 C202 H20G 109.5 . . ? Si20 C202 H20H 109.5 . . ? H20G C202 H20H 109.5 . . ? Si20 C202 H20I 109.5 . . ? H20G C202 H20I 109.5 . . ? H20H C202 H20I 109.5 . . ? Si20 C203 H20A 109.5 . . ? Si20 C203 H20B 109.5 . . ? H20A C203 H20B 109.5 . . ? Si20 C203 H20C 109.5 . . ? H20A C203 H20C 109.5 . . ? H20B C203 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.406 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.071 #===END _database_code_depnum_ccdc_archive 'CCDC 960132'