# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1600 # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-05-28 at 15:04:30 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : c:\wingx\files\archive.dat # CIF files read : wdiol dreduc struct psi_scan absorb # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_global # #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Sullivan Alice C.' _publ_contact_author_email A.C.Sullivan@qmw.ac.uk #------------------------------------------------------------------------- #3 Publication details # # Provide these details if the structure has been published, # accepted or submitted for publication # # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal # loop_ _publ_author_name 'Sullivan Alice C.' _journal_name_full 'private communication' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? # #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ; ? ; # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection ? _ccdc_ls_R_squared ? _ccdc_disorder ? _ccdc_comments ; ? ; #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_wdiol _audit_creation_date 1999-05-28T15:04:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H64 N2 O4 Si4 W1' _chemical_formula_structural 'C56 H64 O4 N2 SI4 W' _chemical_formula_sum 'C63 H66 N2 O6 Si4 W' _chemical_formula_weight 1243.39 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall 'P-1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.333(4) _cell_length_b 10.733(8) _cell_length_c 14.149(7) _cell_angle_alpha 110.88(6) _cell_angle_beta 90.08(4) _cell_angle_gamma 99.91(4) _cell_volume 1440.9(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'COLOURLESS, TRANSPARENT' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.31 0 0 -1 0.31 -1 0 0 0.25 1 0 0 0.25 0 1 0 0.12 0 -1 0 0.12 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.14 _exptl_absorpt_factor_muR 0.443 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.4091 _exptl_absorpt_correction_T_max 0.6394 _exptl_absorpt_correction_T_ave 0.5529 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.71874E-1 _diffrn_orient_matrix_ub_12 -0.26556E-1 _diffrn_orient_matrix_ub_13 -0.04606 _diffrn_orient_matrix_ub_21 -0.67239E-1 _diffrn_orient_matrix_ub_22 -0.50682E-1 _diffrn_orient_matrix_ub_23 -0.57802E-1 _diffrn_orient_matrix_ub_31 0.4106E-2 _diffrn_orient_matrix_ub_32 0.08405 _diffrn_orient_matrix_ub_33 -0.16236E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.08 _diffrn_standards_decay_corr_min 0.997 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 4 -3 -6 2 -5 _diffrn_reflns_number 5351 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5054 _reflns_number_gt 4787 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4/PC (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4/PC (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 5054 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.258 _refine_ls_restrained_S_all 1.258 _refine_ls_shift/su_max 0.208 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 2.059 _refine_diff_density_min -6.047 _refine_diff_density_rms 0.164 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 W1 W 0 0 0 0.0488(2) Uani 1 2 d S . . Si1 Si -0.00439(17) -0.17391(19) -0.24582(14) 0.0211(4) Uani 1 1 d . . . Si2 Si -0.23958(17) -0.04898(19) -0.17377(14) 0.0215(4) Uani 1 1 d . . . O1 O 0.0415(5) -0.1246(5) -0.1268(4) 0.0251(10) Uani 1 1 d . . . O2 O -0.1497(4) -0.1374(5) -0.2578(3) 0.0240(10) Uani 1 1 d . . . O3 O -0.1556(5) 0.0192(5) -0.0655(4) 0.0254(10) Uani 1 1 d . . . N1 N 0.1046(8) 0.1561(6) -0.0303(5) 0.0405(17) Uani 1 1 d . . . C1 C 0.1168(4) -0.0780(5) -0.3063(4) 0.0250(15) Uani 1 1 d G . . C2 C 0.2502(4) -0.0716(6) -0.2868(5) 0.052(3) Uani 1 1 d G . . H2 H 0.2769 -0.1174 -0.2477 0.077(16) Uiso 1 1 calc R . . C3 C 0.3435(3) 0.0033(7) -0.3258(5) 0.058(3) Uani 1 1 d G . . H3 H 0.4327 0.0076 -0.3128 0.077(16) Uiso 1 1 calc R . . C4 C 0.3035(4) 0.0717(6) -0.3843(4) 0.0391(19) Uani 1 1 d G . . H4 H 0.366 0.1218 -0.4104 0.077(16) Uiso 1 1 calc R . . C5 C 0.1701(5) 0.0653(6) -0.4038(4) 0.045(2) Uani 1 1 d G . . H5 H 0.1434 0.1111 -0.4429 0.077(16) Uiso 1 1 calc R . . C6 C 0.0768(3) -0.0095(6) -0.3647(4) 0.040(2) Uani 1 1 d G . . H6 H -0.0124 -0.0138 -0.3777 0.077(16) Uiso 1 1 calc R . . C7 C -0.0164(5) -0.3623(4) -0.3083(4) 0.0261(15) Uani 1 1 d G . . C8 C -0.1157(4) -0.4382(5) -0.3831(4) 0.0343(17) Uani 1 1 d G . . H8 H -0.1785 -0.3963 -0.4007 0.059(13) Uiso 1 1 calc R . . C9 C -0.1212(5) -0.5769(5) -0.4317(4) 0.044(2) Uani 1 1 d G . . H9 H -0.1876 -0.6277 -0.4818 0.059(13) Uiso 1 1 calc R . . C10 C -0.0273(6) -0.6395(4) -0.4055(4) 0.044(2) Uani 1 1 d G . . H10 H -0.031 -0.7323 -0.4381 0.059(13) Uiso 1 1 calc R . . C11 C 0.0720(5) -0.5636(5) -0.3307(4) 0.047(2) Uani 1 1 d G . . H11 H 0.1348 -0.6055 -0.3132 0.059(13) Uiso 1 1 calc R . . C12 C 0.0774(4) -0.4249(5) -0.2821(4) 0.041(2) Uani 1 1 d G . . H12 H 0.1439 -0.3741 -0.2321 0.059(13) Uiso 1 1 calc R . . C13 C -0.3923(3) -0.1681(4) -0.1650(4) 0.0230(14) Uani 1 1 d G . . C14 C -0.3940(4) -0.3066(4) -0.1949(4) 0.0316(17) Uani 1 1 d G . . H14 H -0.3215 -0.3424 -0.224 0.044(11) Uiso 1 1 calc R . . C15 C -0.5040(4) -0.3917(3) -0.1813(4) 0.0367(18) Uani 1 1 d G . . H15 H -0.5051 -0.4844 -0.2013 0.044(11) Uiso 1 1 calc R . . C16 C -0.6124(4) -0.3383(4) -0.1379(4) 0.0359(18) Uani 1 1 d G . . H16 H -0.686 -0.3952 -0.1288 0.044(11) Uiso 1 1 calc R . . C17 C -0.6107(4) -0.1998(5) -0.1080(4) 0.0342(17) Uani 1 1 d G . . H17 H -0.6832 -0.1641 -0.0789 0.044(11) Uiso 1 1 calc R . . C18 C -0.5006(4) -0.1147(3) -0.1215(4) 0.0277(16) Uani 1 1 d G . . H18 H -0.4995 -0.022 -0.1015 0.044(11) Uiso 1 1 calc R . . C19 C -0.2850(5) 0.0856(4) -0.2177(3) 0.0257(15) Uani 1 1 d G . . C20 C -0.3253(5) 0.1995(5) -0.1496(3) 0.0353(18) Uani 1 1 d G . . H20 H -0.3289 0.2106 -0.0814 0.038(10) Uiso 1 1 calc R . . C21 C -0.3601(6) 0.2967(4) -0.1834(3) 0.042(2) Uani 1 1 d G . . H21 H -0.3871 0.3729 -0.1378 0.038(10) Uiso 1 1 calc R . . C22 C -0.3547(6) 0.2800(5) -0.2852(4) 0.0387(19) Uani 1 1 d G . . H22 H -0.3781 0.3451 -0.3078 0.038(10) Uiso 1 1 calc R . . C23 C -0.3144(5) 0.1662(5) -0.3533(3) 0.0338(17) Uani 1 1 d G . . H23 H -0.3108 0.155 -0.4214 0.038(10) Uiso 1 1 calc R . . C24 C -0.2795(5) 0.0689(4) -0.3195(3) 0.0258(15) Uani 1 1 d G . . H24 H -0.2526 -0.0073 -0.3651 0.038(10) Uiso 1 1 calc R . . C25 C 0.1427(11) 0.2862(10) -0.0427(7) 0.052(2) Uani 1 1 d . . . C26 C 0.0585(14) 0.2830(13) -0.1304(10) 0.078(4) Uani 1 1 d . . . H26A H 0.0818 0.3675 -0.1408 0.31(9) Uiso 1 1 calc R . . H26B H -0.0325 0.2696 -0.116 0.31(9) Uiso 1 1 calc R . . H26C H 0.0725 0.21 -0.1904 0.31(9) Uiso 1 1 calc R . . C27 C 0.2817(13) 0.3064(16) -0.0666(11) 0.094(5) Uani 1 1 d . . . H27A H 0.3351 0.2902 -0.0182 0.18(5) Uiso 1 1 calc R . . H27B H 0.3094 0.3978 -0.0637 0.18(5) Uiso 1 1 calc R . . H27C H 0.2912 0.2443 -0.1335 0.18(5) Uiso 1 1 calc R . . C28 C 0.1179(15) 0.3937(12) 0.0544(10) 0.080(4) Uani 1 1 d . . . H28A H 0.1727 0.393 0.109 0.28(8) Uiso 1 1 calc R . . H28B H 0.0271 0.3758 0.0682 0.28(8) Uiso 1 1 calc R . . H28C H 0.1382 0.4809 0.0481 0.28(8) Uiso 1 1 calc R . . C01 C -0.4892(19) -0.4319(19) -0.4814(15) 0.047(4) Uiso 0.5 1 d P . . C02 C -0.395(2) -0.350(3) -0.5161(19) 0.068(6) Uiso 0.5 1 d P . . C03 C -0.4763(13) -0.2826(13) -0.4483(10) 0.072(3) Uiso 1 1 d . . . C04 C -0.578(3) -0.358(3) -0.4159(19) 0.072(6) Uiso 0.5 1 d P . . C05 C -0.4086(11) -0.4969(11) -0.5514(8) 0.060(3) 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 W1 0.0365(3) 0.0795(4) 0.0206(2) -0.0082(2) -0.00709(18) 0.0422(3) Si1 0.0184(9) 0.0216(9) 0.0221(9) 0.0050(7) 0.0012(7) 0.0072(7) Si2 0.0177(9) 0.0236(9) 0.0229(9) 0.0062(8) -0.0002(7) 0.0076(7) O1 0.023(2) 0.027(3) 0.025(2) 0.005(2) -0.0001(19) 0.012(2) O2 0.020(2) 0.028(3) 0.023(2) 0.005(2) -0.0004(19) 0.008(2) O3 0.025(2) 0.027(3) 0.025(2) 0.007(2) 0.001(2) 0.012(2) N1 0.072(5) 0.019(3) 0.028(3) 0.004(3) -0.007(3) 0.011(3) C1 0.023(3) 0.027(4) 0.024(3) 0.005(3) 0.002(3) 0.009(3) C2 0.027(4) 0.077(7) 0.077(7) 0.058(6) 0.004(4) 0.010(4) C3 0.020(4) 0.094(8) 0.078(7) 0.051(7) 0.005(4) 0.009(5) C4 0.038(5) 0.042(5) 0.041(5) 0.021(4) 0.012(4) 0.002(4) C5 0.044(5) 0.060(6) 0.048(5) 0.035(5) 0.015(4) 0.021(4) C6 0.028(4) 0.059(6) 0.044(5) 0.030(4) 0.007(3) 0.016(4) C7 0.026(4) 0.029(4) 0.023(3) 0.007(3) 0.006(3) 0.010(3) C8 0.032(4) 0.032(4) 0.033(4) 0.006(3) 0.000(3) 0.005(3) C9 0.045(5) 0.032(4) 0.042(5) 0.001(4) 0.002(4) -0.001(4) C10 0.049(5) 0.024(4) 0.053(5) 0.004(4) 0.015(4) 0.009(4) C11 0.052(5) 0.035(5) 0.060(6) 0.016(4) 0.006(4) 0.024(4) C12 0.040(5) 0.035(4) 0.044(5) 0.007(4) -0.007(4) 0.014(4) C13 0.021(3) 0.025(4) 0.025(3) 0.010(3) -0.001(3) 0.006(3) C14 0.023(4) 0.030(4) 0.045(4) 0.015(3) 0.002(3) 0.010(3) C15 0.033(4) 0.026(4) 0.056(5) 0.020(4) -0.002(4) 0.005(3) C16 0.023(4) 0.040(5) 0.047(5) 0.021(4) -0.004(3) 0.001(3) C17 0.024(4) 0.047(5) 0.034(4) 0.014(4) 0.005(3) 0.014(3) C18 0.025(4) 0.030(4) 0.029(4) 0.011(3) 0.004(3) 0.006(3) C19 0.017(3) 0.028(4) 0.030(4) 0.007(3) -0.001(3) 0.004(3) C20 0.042(5) 0.037(4) 0.028(4) 0.009(3) 0.005(3) 0.016(4) C21 0.049(5) 0.036(5) 0.046(5) 0.014(4) 0.009(4) 0.024(4) C22 0.042(5) 0.036(4) 0.049(5) 0.024(4) 0.008(4) 0.015(4) C23 0.033(4) 0.037(4) 0.036(4) 0.019(4) 0.004(3) 0.008(3) C24 0.019(3) 0.027(4) 0.031(4) 0.011(3) 0.005(3) 0.005(3) C25 0.065(6) 0.042(5) 0.046(5) 0.018(4) 0.000(5) 0.002(5) C26 0.110(10) 0.071(8) 0.073(8) 0.045(7) -0.003(7) 0.029(7) C27 0.060(8) 0.118(12) 0.087(10) 0.035(9) 0.032(7) -0.022(7) C28 0.117(11) 0.056(7) 0.071(8) 0.016(6) 0.004(7) 0.038(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 W1 O1 1.919(5) . ? W1 O1 1.919(5) 2 ? W1 O3 1.932(5) 2 ? W1 O3 1.932(5) . ? W1 N1 2.013(7) . ? W1 N1 2.013(7) 2 ? Si1 O1 1.617(5) . ? Si1 O2 1.640(5) . ? Si1 C7 1.877(4) . ? Si1 C1 1.883(4) . ? Si2 O3 1.617(5) . ? Si2 O2 1.636(5) . ? Si2 C13 1.886(4) . ? Si2 C19 1.888(4) . ? N1 C25 1.456(11) . ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C2 H2 0.93 . ? C3 C4 1.39 . ? C3 H3 0.93 . ? C4 C5 1.39 . ? C4 H4 0.93 . ? C5 C6 1.39 . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.39 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C8 H8 0.93 . ? C9 C10 1.39 . ? C9 H9 0.93 . ? C10 C11 1.39 . ? C10 H10 0.93 . ? C11 C12 1.39 . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C14 H14 0.93 . ? C15 C16 1.39 . ? C15 H15 0.93 . ? C16 C17 1.39 . ? C16 H16 0.93 . ? C17 C18 1.39 . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C20 H20 0.93 . ? C21 C22 1.39 . ? C21 H21 0.93 . ? C22 C23 1.39 . ? C22 H22 0.93 . ? C23 C24 1.39 . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C27 1.473(15) . ? C25 C26 1.501(15) . ? C25 C28 1.503(15) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C01 C01 1.34(4) 2_444 ? C01 C05 1.37(2) . ? C01 C05 1.37(2) 2_444 ? C01 C02 1.41(3) . ? C01 C04 1.43(3) . ? C01 C03 1.48(2) . ? C02 C03 1.37(3) . ? C02 C05 1.45(3) . ? C03 C04 1.39(3) . ? C04 C05 1.43(3) 2_444 ? C05 C01 1.37(2) 2_444 ? C05 C04 1.43(3) 2_444 ? 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 O1 W1 O1 180.0(3) . 2 ? O1 W1 O3 90.0(2) . 2 ? O1 W1 O3 90.0(2) 2 2 ? O1 W1 O3 90.0(2) . . ? O1 W1 O3 90.0(2) 2 . ? O3 W1 O3 180.0(3) 2 . ? O1 W1 N1 90.2(2) . . ? O1 W1 N1 89.8(2) 2 . ? O3 W1 N1 90.3(3) 2 . ? O3 W1 N1 89.7(3) . . ? O1 W1 N1 89.8(2) . 2 ? O1 W1 N1 90.2(2) 2 2 ? O3 W1 N1 89.7(3) 2 2 ? O3 W1 N1 90.3(3) . 2 ? N1 W1 N1 180.0(6) . 2 ? O1 Si1 O2 109.5(3) . . ? O1 Si1 C7 110.4(3) . . ? O2 Si1 C7 108.4(2) . . ? O1 Si1 C1 108.3(3) . . ? O2 Si1 C1 108.3(2) . . ? C7 Si1 C1 111.8(3) . . ? O3 Si2 O2 108.9(3) . . ? O3 Si2 C13 110.3(3) . . ? O2 Si2 C13 108.0(2) . . ? O3 Si2 C19 110.8(2) . . ? O2 Si2 C19 108.3(2) . . ? C13 Si2 C19 110.4(2) . . ? Si1 O1 W1 138.2(3) . . ? Si2 O2 Si1 131.2(3) . . ? Si2 O3 W1 139.0(3) . . ? C25 N1 W1 161.9(7) . . ? C2 C1 C6 120 . . ? C2 C1 Si1 117.9(3) . . ? C6 C1 Si1 122.1(3) . . ? C1 C2 C3 120 . . ? C1 C2 H2 120 . . ? C3 C2 H2 120 . . ? C4 C3 C2 120 . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120 . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C8 C7 C12 120 . . ? C8 C7 Si1 120.3(3) . . ? C12 C7 Si1 119.7(3) . . ? C9 C8 C7 120 . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 120 . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C11 C10 C9 120 . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C12 C11 C10 120 . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C11 C12 C7 120 . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C14 C13 C18 120 . . ? C14 C13 Si2 120.7(2) . . ? C18 C13 Si2 119.1(2) . . ? C13 C14 C15 120 . . ? C13 C14 H14 120 . . ? C15 C14 H14 120 . . ? C16 C15 C14 120 . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C15 C16 C17 120 . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C18 C17 C16 120 . . ? C18 C17 H17 120 . . ? C16 C17 H17 120 . . ? C17 C18 C13 120 . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? C20 C19 C24 120 . . ? C20 C19 Si2 120.7(3) . . ? C24 C19 Si2 119.3(3) . . ? C19 C20 C21 120 . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C22 C21 C20 120 . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C23 C22 C21 120 . . ? C23 C22 H22 120 . . ? C21 C22 H22 120 . . ? C24 C23 C22 120 . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C19 120 . . ? C23 C24 H24 120 . . ? C19 C24 H24 120 . . ? N1 C25 C27 110.5(10) . . ? N1 C25 C26 107.4(8) . . ? C27 C25 C26 108.5(10) . . ? N1 C25 C28 107.0(8) . . ? C27 C25 C28 112.0(10) . . ? C26 C25 C28 111.4(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C01 C01 C05 60.9(15) 2_444 . ? C01 C01 C05 60.4(15) 2_444 2_444 ? C05 C01 C05 121.4(15) . 2_444 ? C01 C01 C02 124(2) 2_444 . ? C05 C01 C02 63.2(14) . . ? C05 C01 C02 174(2) 2_444 . ? C01 C01 C04 122(2) 2_444 . ? C05 C01 C04 174(2) . . ? C05 C01 C04 61.5(14) 2_444 . ? C02 C01 C04 113.5(19) . . ? C01 C01 C03 174(2) 2_444 . ? C05 C01 C03 119.6(15) . . ? C05 C01 C03 118.7(15) 2_444 . ? C02 C01 C03 56.4(13) . . ? C04 C01 C03 57.2(13) . . ? C03 C02 C01 64.5(14) . . ? C03 C02 C05 121.5(19) . . ? C01 C02 C05 57.0(13) . . ? C02 C03 C04 118.5(18) . . ? C02 C03 C01 59.1(14) . . ? C04 C03 C01 59.5(14) . . ? C03 C04 C01 63.3(14) . . ? C03 C04 C05 121(2) . 2_444 ? C01 C04 C05 57.3(13) . 2_444 ? C01 C05 C01 58.6(15) . 2_444 ? C01 C05 C04 119.5(16) . 2_444 ? C01 C05 C04 61.1(14) 2_444 2_444 ? C01 C05 C02 59.8(13) . . ? C01 C05 C02 118.2(15) 2_444 . ? C04 C05 C02 178.9(17) 2_444 . ? data_motetr _audit_creation_date 1999-05-14T15:44:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_structural 'C64 H76 O6 SI2 N2 MO' _chemical_formula_sum 'C62 H59 Mo N3 O6 Si4' _chemical_formula_weight 1150.42 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 13.655(9) _cell_length_b 14.524(10) _cell_length_c 16.072(12) _cell_angle_alpha 102.67(8) _cell_angle_beta 87.75(6) _cell_angle_gamma 107.62(6) _cell_volume 2963(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 11.6 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'transparent yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.29 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_factor_muR 0.047 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.4872 _exptl_absorpt_correction_T_max 0.9525 _exptl_absorpt_correction_T_ave 0.6754 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.7119E-2 _diffrn_orient_matrix_ub_12 -0.72265E-1 _diffrn_orient_matrix_ub_13 -0.16325E-1 _diffrn_orient_matrix_ub_21 0.63605E-1 _diffrn_orient_matrix_ub_22 0.14404E-1 _diffrn_orient_matrix_ub_23 -0.34015E-1 _diffrn_orient_matrix_ub_31 0.42628E-1 _diffrn_orient_matrix_ub_32 0.6933E-2 _diffrn_orient_matrix_ub_33 0.51534E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_standards_decay_corr_max 1.083 _diffrn_standards_decay_corr_min 0.991 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 0 -3 -1 -6 -1 _diffrn_reflns_number 10401 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.2165 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 10401 _reflns_number_gt 3858 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 /PC (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 /PC (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 10401 _refine_ls_number_parameters 552 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.2446 _refine_ls_R_factor_gt 0.113 _refine_ls_wR_factor_ref 0.3015 _refine_ls_wR_factor_gt 0.2557 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 2.837 _refine_ls_shift/su_mean 0.095 _refine_diff_density_max 2.812 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.136 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Mo Mo -1.6832 0.6857 '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' 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 Mo1 Mo 0.23347(5) 0.00196(5) 0.24435(4) 0.0496(2) Uani 1 1 d U . . Si1 Si 0.15430(14) -0.24098(13) 0.16463(12) 0.0389(5) Uani 1 1 d U . . Si2 Si 0.10308(14) -0.17135(14) 0.34492(12) 0.0406(5) Uani 1 1 d U . . Si3 Si 0.34840(14) 0.23735(13) 0.33441(13) 0.0397(5) Uani 1 1 d U . . Si4 Si 0.40032(14) 0.16894(13) 0.15363(12) 0.0379(5) Uani 1 1 d U . . N1 N 0.1208(3) 0.0308(4) 0.2171(4) 0.0400(14) Uani 1 1 d U . . O1 O 0.2010(3) -0.1229(3) 0.1648(3) 0.0379(12) Uani 1 1 d U . . O2 O 0.1032(3) -0.2519(3) 0.2569(3) 0.0418(12) Uani 1 1 d U . . O3 O 0.1797(3) -0.0646(3) 0.3364(3) 0.0403(12) Uani 1 1 d U . . O4 O 0.2960(3) 0.1197(3) 0.3309(3) 0.0377(12) Uani 1 1 d U . . O5 O 0.4025(3) 0.2484(3) 0.2426(3) 0.0445(13) Uani 1 1 d U . . O6 O 0.3189(3) 0.0635(3) 0.1618(3) 0.0379(12) Uani 1 1 d U . . C1 C 0.0522(3) -0.3042(3) 0.0787(3) 0.0432(18) Uani 1 1 d GU . . C2 C -0.0283(3) -0.3847(3) 0.0917(3) 0.082(3) Uani 1 1 d GU . . H2 H -0.0336 -0.4034 0.1439 0.21(2) Uiso 1 1 calc R . . C3 C -0.1011(3) -0.4374(4) 0.0267(4) 0.095(3) Uani 1 1 d GU . . H3 H -0.155 -0.4912 0.0354 0.21(2) Uiso 1 1 calc R . . C4 C -0.0932(4) -0.4095(5) -0.0512(4) 0.089(3) Uani 1 1 d GU . . H4 H -0.1419 -0.4447 -0.0947 0.21(2) Uiso 1 1 calc R . . C5 C -0.0127(5) -0.3289(5) -0.0642(3) 0.110(3) Uani 1 1 d GU . . H5 H -0.0075 -0.3103 -0.1164 0.21(2) Uiso 1 1 calc R . . C6 C 0.0600(4) -0.2763(4) 0.0007(3) 0.094(3) Uani 1 1 d GU . . H6 H 0.1139 -0.2224 -0.008 0.21(2) Uiso 1 1 calc R . . C7 C 0.2581(3) -0.3022(3) 0.1501(3) 0.0481(17) Uani 1 1 d GU . . C8 C 0.3098(4) -0.3070(4) 0.0737(3) 0.069(2) Uani 1 1 d GU . . H8 H 0.2893 -0.2843 0.0295 0.135(15) Uiso 1 1 calc R . . C9 C 0.3920(4) -0.3457(5) 0.0634(4) 0.084(2) Uani 1 1 d GU . . H9 H 0.4266 -0.3489 0.0124 0.135(15) Uiso 1 1 calc R . . C10 C 0.4227(4) -0.3795(5) 0.1295(5) 0.086(2) Uani 1 1 d GU . . H10 H 0.4777 -0.4054 0.1226 0.135(15) Uiso 1 1 calc R . . C11 C 0.3710(4) -0.3747(5) 0.2058(4) 0.122(3) Uani 1 1 d GU . . H11 H 0.3915 -0.3974 0.25 0.135(15) Uiso 1 1 calc R . . C12 C 0.2887(4) -0.3360(4) 0.2161(3) 0.090(2) Uani 1 1 d GU . . H12 H 0.2542 -0.3328 0.2672 0.135(15) Uiso 1 1 calc R . . C13 C 0.1480(3) -0.2115(3) 0.4352(2) 0.0419(16) Uani 1 1 d GU . . C14 C 0.1301(3) -0.3121(3) 0.4301(3) 0.0555(19) Uani 1 1 d GU . . H14 H 0.098 -0.3579 0.3816 0.142(16) Uiso 1 1 calc R . . C15 C 0.1602(5) -0.3442(3) 0.4975(4) 0.077(2) Uani 1 1 d GU . . H15 H 0.1482 -0.4115 0.4941 0.142(16) Uiso 1 1 calc R . . C16 C 0.2082(5) -0.2758(5) 0.5700(3) 0.085(3) Uani 1 1 d GU . . H16 H 0.2283 -0.2973 0.615 0.142(16) Uiso 1 1 calc R . . C17 C 0.2261(4) -0.1752(4) 0.5751(3) 0.096(3) Uani 1 1 d GU . . H17 H 0.2582 -0.1294 0.6235 0.142(16) Uiso 1 1 calc R . . C18 C 0.1960(4) -0.1431(3) 0.5077(3) 0.085(3) Uani 1 1 d GU . . H18 H 0.208 -0.0758 0.5111 0.142(16) Uiso 1 1 calc R . . C19 C -0.0311(2) -0.1651(3) 0.3629(3) 0.0454(18) Uani 1 1 d GU . . C20 C -0.0569(3) -0.1225(4) 0.4436(3) 0.060(2) Uani 1 1 d GU . . H20 H -0.0086 -0.1002 0.4884 0.103(12) Uiso 1 1 calc R . . C21 C -0.1549(4) -0.1132(4) 0.4572(3) 0.068(2) Uani 1 1 d GU . . H21 H -0.1722 -0.0847 0.5112 0.103(12) Uiso 1 1 calc R . . C22 C -0.2272(3) -0.1465(5) 0.3902(4) 0.084(3) Uani 1 1 d GU . . H22 H -0.2928 -0.1403 0.3993 0.103(12) Uiso 1 1 calc R . . C23 C -0.2013(3) -0.1891(5) 0.3095(4) 0.114(4) Uani 1 1 d GU . . H23 H -0.2496 -0.2114 0.2647 0.103(12) Uiso 1 1 calc R . . C24 C -0.1033(3) -0.1984(4) 0.2959(3) 0.085(3) Uani 1 1 d GU . . H24 H -0.086 -0.2269 0.2419 0.103(12) Uiso 1 1 calc R . . C25 C 0.2484(3) 0.3025(3) 0.3480(3) 0.0431(17) Uani 1 1 d GU . . C26 C 0.1759(4) 0.2846(4) 0.4103(3) 0.110(2) Uani 1 1 d GU . . H26 H 0.179 0.2422 0.4452 0.19(2) Uiso 1 1 calc R . . C27 C 0.0987(4) 0.3300(5) 0.4203(4) 0.132(3) Uani 1 1 d GU . . H27 H 0.0501 0.3179 0.462 0.19(2) Uiso 1 1 calc R . . C28 C 0.0940(4) 0.3933(5) 0.3681(5) 0.106(3) Uani 1 1 d GU . . H28 H 0.0424 0.4236 0.3748 0.19(2) Uiso 1 1 calc R . . C29 C 0.1666(5) 0.4112(4) 0.3058(5) 0.112(3) Uani 1 1 d GU . . H29 H 0.1635 0.4535 0.2708 0.19(2) Uiso 1 1 calc R . . C30 C 0.2438(4) 0.3658(4) 0.2957(3) 0.077(2) Uani 1 1 d GU . . H30 H 0.2924 0.3778 0.2541 0.19(2) Uiso 1 1 calc R . . C31 C 0.4495(3) 0.2915(4) 0.4215(3) 0.0513(19) Uani 1 1 d GU . . C32 C 0.5219(4) 0.3826(4) 0.4219(4) 0.145(4) Uani 1 1 d GU . . H32 H 0.5209 0.4151 0.3782 0.51(6) Uiso 1 1 calc R . . C33 C 0.5958(5) 0.4250(5) 0.4875(5) 0.161(4) Uani 1 1 d GU . . H33 H 0.6442 0.486 0.4878 0.51(6) Uiso 1 1 calc R . . C34 C 0.5972(5) 0.3765(7) 0.5528(4) 0.108(3) Uani 1 1 d GU . . H34 H 0.6466 0.4049 0.5967 0.51(6) Uiso 1 1 calc R . . C35 C 0.5248(6) 0.2854(7) 0.5524(4) 0.216(5) Uani 1 1 d GU . . H35 H 0.5257 0.2529 0.596 0.51(6) Uiso 1 1 calc R . . C36 C 0.4509(5) 0.2429(5) 0.4867(4) 0.170(4) Uani 1 1 d GU . . H36 H 0.4024 0.182 0.4865 0.51(6) Uiso 1 1 calc R . . C37 C 0.3581(3) 0.2163(3) 0.0666(2) 0.0433(16) Uani 1 1 d GU . . C38 C 0.3701(3) 0.3167(3) 0.0767(3) 0.062(2) Uani 1 1 d GU . . H38 H 0.3999 0.3607 0.1267 0.091(12) Uiso 1 1 calc R . . C39 C 0.3376(4) 0.3512(3) 0.0119(4) 0.079(3) Uani 1 1 d GU . . H39 H 0.3456 0.4184 0.0186 0.091(12) Uiso 1 1 calc R . . C40 C 0.2931(4) 0.2854(5) -0.0630(3) 0.081(2) Uani 1 1 d GU . . H40 H 0.2714 0.3085 -0.1063 0.091(12) Uiso 1 1 calc R . . C41 C 0.2811(4) 0.1850(4) -0.0730(2) 0.078(3) Uani 1 1 d GU . . H41 H 0.2513 0.1409 -0.1231 0.091(12) Uiso 1 1 calc R . . C42 C 0.3136(3) 0.1505(3) -0.0083(3) 0.065(2) Uani 1 1 d GU . . H42 H 0.3055 0.0833 -0.015 0.091(12) Uiso 1 1 calc R . . C43 C 0.5330(2) 0.1567(3) 0.1359(2) 0.0435(18) Uani 1 1 d GU . . C44 C 0.6001(3) 0.1768(4) 0.2050(2) 0.078(3) Uani 1 1 d GU . . H44 H 0.5808 0.2001 0.2598 0.135(15) Uiso 1 1 calc R . . C45 C 0.6960(3) 0.1620(5) 0.1922(3) 0.103(4) Uani 1 1 d GU . . H45 H 0.7408 0.1755 0.2384 0.135(15) Uiso 1 1 calc R . . C46 C 0.7248(3) 0.1272(4) 0.1103(3) 0.058(2) Uani 1 1 d GU . . H46 H 0.789 0.1174 0.1017 0.135(15) Uiso 1 1 calc R . . C47 C 0.6578(3) 0.1072(4) 0.0412(3) 0.055(2) Uani 1 1 d GU . . H47 H 0.6771 0.0839 -0.0136 0.135(15) Uiso 1 1 calc R . . C48 C 0.5619(3) 0.1219(4) 0.0540(2) 0.0450(19) Uani 1 1 d GU . . H48 H 0.517 0.1085 0.0078 0.135(15) Uiso 1 1 calc R . . N2 N 0.3782(3) -0.0378(3) 0.2669(3) 0.0560(15) Uani 1 1 d GU . . C49 C 0.4327(4) -0.0710(4) 0.1980(3) 0.076(2) Uani 1 1 d GU . . H49 H 0.4095 -0.0783 0.1426 0.52(5) Uiso 1 1 calc R . . C50 C 0.5220(4) -0.0934(5) 0.2119(5) 0.100(3) Uani 1 1 d GU . . H50 H 0.5585 -0.1156 0.1658 0.52(5) Uiso 1 1 calc R . . C51 C 0.5567(4) -0.0825(6) 0.2947(5) 0.149(4) Uani 1 1 d GU . . H51 H 0.6164 -0.0974 0.304 0.52(5) Uiso 1 1 calc R . . C52 C 0.5021(5) -0.0493(7) 0.3636(4) 0.179(4) Uani 1 1 d GU . . H52 H 0.5253 -0.042 0.419 0.52(5) Uiso 1 1 calc R . . C53 C 0.4129(4) -0.0270(5) 0.3497(3) 0.109(3) Uani 1 1 d GU . . H53 H 0.3764 -0.0047 0.3958 0.52(5) Uiso 1 1 calc R . . C54 C 0.0341(6) 0.0454(6) 0.1796(6) 0.073(2) Uani 1 1 d U . . C55 C -0.0136(9) -0.0429(9) 0.1142(7) 0.163(4) Uani 1 1 d U . . H55A H 0.0334 -0.0497 0.0689 0.31(3) Uiso 1 1 calc R . . H55B H -0.0751 -0.037 0.0919 0.31(3) Uiso 1 1 calc R . . H55C H -0.0306 -0.1002 0.1388 0.31(3) Uiso 1 1 calc R . . C56 C -0.0360(6) 0.0688(9) 0.2607(8) 0.157(4) Uani 1 1 d U . . H56A H -0.0721 0.0082 0.2776 0.31(3) Uiso 1 1 calc R . . H56B H -0.0847 0.0984 0.2452 0.31(3) Uiso 1 1 calc R . . H56C H 0.0072 0.1135 0.3074 0.31(3) Uiso 1 1 calc R . . C57 C 0.0688(8) 0.1339(7) 0.1454(7) 0.134(4) Uani 1 1 d U . . H57A H 0.0995 0.1899 0.1905 0.31(3) Uiso 1 1 calc R . . H57B H 0.0113 0.144 0.1203 0.31(3) Uiso 1 1 calc R . . H57C H 0.1187 0.1263 0.1027 0.31(3) Uiso 1 1 calc R . . N3A N -0.2452(14) -0.5679(10) 0.1869(10) 0.268(5) Uiso 0.6 1 d PGU A 1 C58A C -0.3270(14) -0.5297(15) 0.2075(13) 0.268(5) Uiso 0.6 1 d PGU A 1 H58A H -0.3817 -0.5465 0.1687 0.322 Uiso 0.6 1 calc PR A 1 C59A C -0.3272(19) -0.4664(17) 0.2860(15) 0.268(5) Uiso 0.6 1 d PGU A 1 H59A H -0.3819 -0.4408 0.2998 0.322 Uiso 0.6 1 calc PR A 1 C60A C -0.245(2) -0.4412(15) 0.3440(11) 0.268(5) Uiso 0.6 1 d PGU A 1 H60A H -0.2456 -0.3989 0.3966 0.322 Uiso 0.6 1 calc PR A 1 C61A C -0.1636(18) -0.4794(16) 0.3235(12) 0.268(5) Uiso 0.6 1 d PGU A 1 H61A H -0.109 -0.4626 0.3623 0.322 Uiso 0.6 1 calc PR A 1 C62A C -0.1635(14) -0.5427(14) 0.2449(12) 0.268(5) Uiso 0.6 1 d PGU A 1 H62A H -0.1087 -0.5683 0.2311 0.322 Uiso 0.6 1 calc PR A 1 N3B N -0.2993(19) -0.5615(17) 0.1785(14) 0.268(5) Uiso 0.4 1 d PGU B 2 C58B C -0.348(2) -0.500(2) 0.2306(17) 0.268(5) Uiso 0.4 1 d PGU B 2 H58B H -0.4108 -0.4967 0.2137 0.322 Uiso 0.4 1 calc PR B 2 C59B C -0.301(3) -0.442(2) 0.3079(17) 0.268(5) Uiso 0.4 1 d PGU B 2 H59B H -0.3337 -0.4002 0.3428 0.322 Uiso 0.4 1 calc PR B 2 C60A C -0.207(3) -0.446(2) 0.3332(15) 0.202(15) Uiso 0.4 1 d PGU B 2 H60B H -0.176 -0.4071 0.3849 0.243 Uiso 0.4 1 calc PR B 2 C61B C -0.159(2) -0.508(2) 0.2811(18) 0.198(14) Uiso 0.4 1 d PGU B 2 H61B H -0.0954 -0.5106 0.298 0.238 Uiso 0.4 1 calc PR B 2 C62B C -0.205(2) -0.5657(19) 0.2037(16) 0.188(13) Uiso 0.4 1 d PGU B 2 H62B H -0.1725 -0.6072 0.1689 0.225 Uiso 0.4 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0789(4) 0.0299(3) 0.0273(3) 0.0003(2) 0.0217(3) 0.0045(3) Si1 0.0499(10) 0.0310(9) 0.0320(11) 0.0009(8) 0.0045(8) 0.0111(8) Si2 0.0466(10) 0.0411(10) 0.0347(11) 0.0108(8) 0.0098(8) 0.0133(8) Si3 0.0475(10) 0.0336(10) 0.0339(11) 0.0009(8) 0.0065(9) 0.0115(8) Si4 0.0438(10) 0.0369(10) 0.0317(11) 0.0079(8) 0.0120(8) 0.0111(8) N1 0.028(2) 0.036(2) 0.062(3) 0.016(2) 0.007(2) 0.0167(19) O1 0.052(2) 0.0284(18) 0.031(2) 0.0006(17) 0.0083(19) 0.0135(17) O2 0.053(2) 0.033(2) 0.035(2) 0.0054(18) 0.0071(19) 0.0089(19) O3 0.058(2) 0.0304(19) 0.032(2) 0.0089(17) 0.0064(19) 0.0119(18) O4 0.045(2) 0.0364(19) 0.026(2) 0.0045(17) 0.0068(18) 0.0056(17) O5 0.056(2) 0.036(2) 0.032(2) 0.0009(19) 0.0211(19) 0.0058(19) O6 0.039(2) 0.033(2) 0.032(2) -0.0003(17) 0.0118(18) 0.0032(17) C1 0.045(3) 0.044(3) 0.035(3) -0.001(3) 0.005(3) 0.014(3) C2 0.070(5) 0.080(5) 0.075(5) 0.020(4) -0.021(4) -0.012(4) C3 0.074(5) 0.085(6) 0.093(5) -0.011(4) -0.030(4) -0.005(4) C4 0.059(4) 0.113(6) 0.080(5) -0.027(5) -0.045(4) 0.031(4) C5 0.158(7) 0.086(6) 0.073(5) 0.007(5) -0.055(5) 0.016(5) C6 0.115(6) 0.082(6) 0.061(4) 0.028(4) -0.036(4) -0.017(5) C7 0.055(3) 0.044(3) 0.044(4) -0.002(3) -0.003(3) 0.021(3) C8 0.078(4) 0.077(4) 0.076(4) 0.035(4) 0.032(3) 0.048(3) C9 0.095(4) 0.094(5) 0.087(5) 0.024(4) 0.038(4) 0.063(4) C10 0.090(4) 0.094(5) 0.095(5) 0.014(4) 0.015(4) 0.065(4) C11 0.163(5) 0.192(7) 0.080(5) 0.042(5) 0.020(5) 0.146(4) C12 0.075(4) 0.167(6) 0.071(4) 0.054(4) 0.022(4) 0.080(4) C13 0.052(3) 0.040(3) 0.039(3) 0.018(2) 0.021(3) 0.018(3) C14 0.057(4) 0.060(3) 0.067(4) 0.024(3) 0.005(3) 0.035(3) C15 0.100(6) 0.067(4) 0.088(5) 0.037(3) -0.002(5) 0.046(4) C16 0.122(6) 0.105(4) 0.064(5) 0.038(4) 0.002(4) 0.074(4) C17 0.141(8) 0.085(4) 0.063(5) 0.019(4) -0.021(5) 0.030(6) C18 0.137(7) 0.064(4) 0.053(4) 0.012(3) -0.018(4) 0.027(5) C19 0.046(3) 0.046(4) 0.045(4) 0.019(3) 0.015(2) 0.010(3) C20 0.060(3) 0.066(5) 0.051(4) 0.007(4) 0.007(3) 0.019(3) C21 0.081(4) 0.080(5) 0.058(4) 0.026(4) 0.031(3) 0.041(4) C22 0.054(4) 0.127(7) 0.090(5) 0.044(5) 0.028(3) 0.045(4) C23 0.064(4) 0.230(11) 0.062(5) 0.032(6) 0.006(4) 0.062(5) C24 0.056(3) 0.146(8) 0.054(5) 0.009(5) 0.002(3) 0.039(4) C25 0.057(3) 0.028(3) 0.035(4) -0.014(3) 0.015(3) 0.016(2) C26 0.116(4) 0.137(5) 0.140(6) 0.086(4) 0.081(4) 0.099(3) C27 0.125(5) 0.139(6) 0.183(7) 0.067(5) 0.087(5) 0.102(4) C28 0.118(4) 0.101(5) 0.132(7) 0.003(4) 0.016(4) 0.096(4) C29 0.136(5) 0.139(6) 0.099(6) 0.029(5) 0.002(5) 0.094(4) C30 0.087(4) 0.101(4) 0.067(5) 0.033(4) 0.013(4) 0.055(3) C31 0.063(4) 0.033(3) 0.048(3) -0.005(3) -0.002(3) 0.010(3) C32 0.133(7) 0.096(6) 0.166(7) 0.036(5) -0.087(5) -0.041(5) C33 0.117(7) 0.121(7) 0.194(8) 0.020(5) -0.090(6) -0.041(6) C34 0.070(5) 0.160(7) 0.067(6) -0.030(5) -0.011(5) 0.033(5) C35 0.193(9) 0.276(9) 0.108(6) 0.087(6) -0.090(6) -0.077(8) C36 0.118(7) 0.223(7) 0.145(6) 0.113(5) -0.089(5) -0.047(6) C37 0.040(3) 0.053(3) 0.047(3) 0.011(2) 0.007(3) 0.030(3) C38 0.088(5) 0.042(3) 0.058(4) 0.013(3) 0.000(4) 0.022(4) C39 0.104(6) 0.069(4) 0.080(5) 0.030(3) 0.012(5) 0.041(4) C40 0.089(5) 0.111(4) 0.072(5) 0.041(4) -0.002(4) 0.058(4) C41 0.094(6) 0.098(4) 0.047(4) 0.007(4) -0.010(4) 0.040(5) C42 0.088(5) 0.047(4) 0.054(4) 0.014(3) -0.011(4) 0.007(4) C43 0.039(3) 0.053(4) 0.040(4) 0.016(3) 0.012(2) 0.014(3) C44 0.079(3) 0.137(7) 0.030(4) 0.001(4) 0.003(3) 0.064(4) C45 0.066(4) 0.183(9) 0.060(4) -0.006(6) 0.000(4) 0.060(5) C46 0.042(3) 0.074(5) 0.063(4) 0.008(4) -0.001(3) 0.031(3) C47 0.044(3) 0.085(5) 0.051(4) 0.020(4) 0.004(3) 0.039(3) C48 0.042(3) 0.062(4) 0.034(3) 0.005(3) -0.001(3) 0.023(3) N2 0.075(3) 0.051(3) 0.032(3) -0.005(2) 0.016(2) 0.017(2) C49 0.074(4) 0.075(5) 0.087(5) 0.017(4) 0.026(4) 0.035(3) C50 0.065(4) 0.105(6) 0.148(5) 0.034(6) 0.000(5) 0.047(4) C51 0.122(5) 0.217(10) 0.140(6) 0.003(6) -0.005(5) 0.124(5) C52 0.120(5) 0.336(11) 0.150(6) 0.052(7) 0.022(5) 0.175(5) C53 0.116(4) 0.168(7) 0.079(4) 0.021(5) 0.006(4) 0.100(4) C54 0.065(4) 0.056(4) 0.097(6) 0.021(3) -0.006(3) 0.012(3) C55 0.183(9) 0.135(6) 0.121(7) 0.020(5) -0.090(6) -0.031(8) C56 0.093(4) 0.218(9) 0.221(7) 0.082(6) 0.085(5) 0.122(5) C57 0.176(9) 0.112(4) 0.142(7) 0.080(4) -0.029(6) 0.043(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Mo1 N1 1.805(5) . ? Mo1 O1 1.914(4) . ? Mo1 O6 1.921(4) . ? Mo1 O4 1.937(4) . ? Mo1 O3 1.943(5) . ? Mo1 N2 2.283(4) . ? Si1 O2 1.632(5) . ? Si1 O1 1.638(4) . ? Si1 C7 1.871(4) . ? Si1 C1 1.875(4) . ? Si2 O3 1.617(4) . ? Si2 O2 1.627(5) . ? Si2 C13 1.865(4) . ? Si2 C19 1.869(4) . ? Si3 O4 1.630(4) . ? Si3 O5 1.641(5) . ? Si3 C25 1.864(5) . ? Si3 C31 1.869(5) . ? Si4 O5 1.624(5) . ? Si4 O6 1.626(4) . ? Si4 C37 1.868(4) . ? Si4 C43 1.878(4) . ? N1 C54 1.440(10) . ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C2 H2 0.93 . ? C3 C4 1.39 . ? C3 H3 0.93 . ? C4 C5 1.39 . ? C4 H4 0.93 . ? C5 C6 1.39 . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.39 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C8 H8 0.93 . ? C9 C10 1.39 . ? C9 H9 0.93 . ? C10 C11 1.39 . ? C10 H10 0.93 . ? C11 C12 1.39 . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C14 H14 0.93 . ? C15 C16 1.39 . ? C15 H15 0.93 . ? C16 C17 1.39 . ? C16 H16 0.93 . ? C17 C18 1.39 . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C20 H20 0.93 . ? C21 C22 1.39 . ? C21 H21 0.93 . ? C22 C23 1.39 . ? C22 H22 0.93 . ? C23 C24 1.39 . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C26 1.39 . ? C25 C30 1.39 . ? C26 C27 1.39 . ? C26 H26 0.93 . ? C27 C28 1.39 . ? C27 H27 0.93 . ? C28 C29 1.39 . ? C28 H28 0.93 . ? C29 C30 1.39 . ? C29 H29 0.93 . ? C30 H30 0.93 . ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C32 H32 0.93 . ? C33 C34 1.39 . ? C33 H33 0.93 . ? C34 C35 1.39 . ? C34 H34 0.93 . ? C35 C36 1.39 . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C37 C38 1.39 . ? C37 C42 1.39 . ? C38 C39 1.39 . ? C38 H38 0.93 . ? C39 C40 1.39 . ? C39 H39 0.93 . ? C40 C41 1.39 . ? C40 H40 0.93 . ? C41 C42 1.39 . ? C41 H41 0.93 . ? C42 H42 0.93 . ? C43 C44 1.39 . ? C43 C48 1.39 . ? C44 C45 1.39 . ? C44 H44 0.93 . ? C45 C46 1.39 . ? C45 H45 0.93 . ? C46 C47 1.39 . ? C46 H46 0.93 . ? C47 C48 1.39 . ? C47 H47 0.93 . ? C48 H48 0.93 . ? N2 C49 1.39 . ? N2 C53 1.39 . ? C49 C50 1.39 . ? C49 H49 0.93 . ? C50 C51 1.39 . ? C50 H50 0.93 . ? C51 C52 1.39 . ? C51 H51 0.93 . ? C52 C53 1.39 . ? C52 H52 0.93 . ? C53 H53 0.93 . ? C54 C57 1.449(12) . ? C54 C55 1.460(13) . ? C54 C56 1.624(14) . ? C55 H55A 0.96 . ? C55 H55B 0.96 . ? C55 H55C 0.96 . ? C56 H56A 0.96 . ? C56 H56B 0.96 . ? C56 H56C 0.96 . ? C57 H57A 0.96 . ? C57 H57B 0.96 . ? C57 H57C 0.96 . ? N3A C58A 1.39 . ? N3A C62A 1.39 . ? C58A C59A 1.39 . ? C58A H58A 0.93 . ? C59A C60A 1.39 . ? C59A H59A 0.93 . ? C60A C61A 1.39 . ? C60A H60A 0.93 . ? C61A C62A 1.39 . ? C61A H61A 0.93 . ? C62A H62A 0.93 . ? N3B C58B 1.39 . ? N3B C62B 1.39 . ? C58B C59B 1.39 . ? C58B H58B 0.93 . ? C59B C60A 1.39 . ? C59B H59B 0.93 . ? C60A C61B 1.39 . ? C60A H60B 0.93 . ? C61B C62B 1.39 . ? C61B H61B 0.93 . ? C62B H62B 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O1 94.6(2) . . ? N1 Mo1 O6 95.0(2) . . ? O1 Mo1 O6 89.90(18) . . ? N1 Mo1 O4 99.6(2) . . ? O1 Mo1 O4 165.83(18) . . ? O6 Mo1 O4 88.68(18) . . ? N1 Mo1 O3 99.6(2) . . ? O1 Mo1 O3 90.24(19) . . ? O6 Mo1 O3 165.32(18) . . ? O4 Mo1 O3 87.59(18) . . ? N1 Mo1 N2 175.2(2) . . ? O1 Mo1 N2 82.21(17) . . ? O6 Mo1 N2 81.46(18) . . ? O4 Mo1 N2 83.64(18) . . ? O3 Mo1 N2 84.01(18) . . ? O2 Si1 O1 108.3(2) . . ? O2 Si1 C7 108.0(2) . . ? O1 Si1 C7 111.1(2) . . ? O2 Si1 C1 108.8(2) . . ? O1 Si1 C1 110.6(2) . . ? C7 Si1 C1 110.0(2) . . ? O3 Si2 O2 109.1(2) . . ? O3 Si2 C13 109.7(2) . . ? O2 Si2 C13 109.1(2) . . ? O3 Si2 C19 110.5(2) . . ? O2 Si2 C19 108.5(2) . . ? C13 Si2 C19 109.9(2) . . ? O4 Si3 O5 107.7(2) . . ? O4 Si3 C25 110.5(2) . . ? O5 Si3 C25 107.9(3) . . ? O4 Si3 C31 109.8(3) . . ? O5 Si3 C31 109.0(2) . . ? C25 Si3 C31 111.8(2) . . ? O5 Si4 O6 108.2(2) . . ? O5 Si4 C37 107.7(2) . . ? O6 Si4 C37 110.5(2) . . ? O5 Si4 C43 108.4(2) . . ? O6 Si4 C43 110.5(2) . . ? C37 Si4 C43 111.4(2) . . ? C54 N1 Mo1 169.5(5) . . ? Si1 O1 Mo1 139.0(3) . . ? Si2 O2 Si1 132.4(3) . . ? Si2 O3 Mo1 136.7(3) . . ? Si3 O4 Mo1 136.7(3) . . ? Si4 O5 Si3 132.5(3) . . ? Si4 O6 Mo1 140.3(3) . . ? C2 C1 C6 120 . . ? C2 C1 Si1 118.8(2) . . ? C6 C1 Si1 121.0(2) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 120 . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C3 C4 C5 120 . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C8 C7 C12 120 . . ? C8 C7 Si1 118.8(3) . . ? C12 C7 Si1 121.1(3) . . ? C9 C8 C7 120 . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 120 . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C9 C10 C11 120 . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C12 C11 C10 120 . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C11 C12 C7 120 . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C14 C13 C18 120 . . ? C14 C13 Si2 118.8(2) . . ? C18 C13 Si2 121.2(2) . . ? C15 C14 C13 120 . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C14 C15 C16 120 . . ? C14 C15 H15 120 . . ? C16 C15 H15 120 . . ? C17 C16 C15 120 . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C18 C17 C16 120 . . ? C18 C17 H17 120 . . ? C16 C17 H17 120 . . ? C17 C18 C13 120 . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? C20 C19 C24 120 . . ? C20 C19 Si2 119.2(2) . . ? C24 C19 Si2 120.7(2) . . ? C21 C20 C19 120 . . ? C21 C20 H20 120 . . ? C19 C20 H20 120 . . ? C22 C21 C20 120 . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C21 C22 C23 120 . . ? C21 C22 H22 120 . . ? C23 C22 H22 120 . . ? C24 C23 C22 120 . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C19 120 . . ? C23 C24 H24 120 . . ? C19 C24 H24 120 . . ? C26 C25 C30 120 . . ? C26 C25 Si3 118.7(3) . . ? C30 C25 Si3 121.3(3) . . ? C27 C26 C25 120 . . ? C27 C26 H26 120 . . ? C25 C26 H26 120 . . ? C26 C27 C28 120 . . ? C26 C27 H27 120 . . ? C28 C27 H27 120 . . ? C27 C28 C29 120 . . ? C27 C28 H28 120 . . ? C29 C28 H28 120 . . ? C30 C29 C28 120 . . ? C30 C29 H29 120 . . ? C28 C29 H29 120 . . ? C29 C30 C25 120 . . ? C29 C30 H30 120 . . ? C25 C30 H30 120 . . ? C32 C31 C36 120 . . ? C32 C31 Si3 119.4(3) . . ? C36 C31 Si3 120.6(3) . . ? C33 C32 C31 120 . . ? C33 C32 H32 120 . . ? C31 C32 H32 120 . . ? C32 C33 C34 120 . . ? C32 C33 H33 120 . . ? C34 C33 H33 120 . . ? C35 C34 C33 120 . . ? C35 C34 H34 120 . . ? C33 C34 H34 120 . . ? C36 C35 C34 120 . . ? C36 C35 H35 120 . . ? C34 C35 H35 120 . . ? C35 C36 C31 120 . . ? C35 C36 H36 120 . . ? C31 C36 H36 120 . . ? C38 C37 C42 120 . . ? C38 C37 Si4 120.4(2) . . ? C42 C37 Si4 119.6(2) . . ? C37 C38 C39 120 . . ? C37 C38 H38 120 . . ? C39 C38 H38 120 . . ? C40 C39 C38 120 . . ? C40 C39 H39 120 . . ? C38 C39 H39 120 . . ? C39 C40 C41 120 . . ? C39 C40 H40 120 . . ? C41 C40 H40 120 . . ? C42 C41 C40 120 . . ? C42 C41 H41 120 . . ? C40 C41 H41 120 . . ? C41 C42 C37 120 . . ? C41 C42 H42 120 . . ? C37 C42 H42 120 . . ? C44 C43 C48 120 . . ? C44 C43 Si4 120.1(2) . . ? C48 C43 Si4 119.8(2) . . ? C43 C44 C45 120 . . ? C43 C44 H44 120 . . ? C45 C44 H44 120 . . ? C44 C45 C46 120 . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C47 C46 C45 120 . . ? C47 C46 H46 120 . . ? C45 C46 H46 120 . . ? C48 C47 C46 120 . . ? C48 C47 H47 120 . . ? C46 C47 H47 120 . . ? C47 C48 C43 120 . . ? C47 C48 H48 120 . . ? C43 C48 H48 120 . . ? C49 N2 C53 120 . . ? C49 N2 Mo1 120.1(2) . . ? C53 N2 Mo1 119.9(2) . . ? C50 C49 N2 120 . . ? C50 C49 H49 120 . . ? N2 C49 H49 120 . . ? C51 C50 C49 120 . . ? C51 C50 H50 120 . . ? C49 C50 H50 120 . . ? C50 C51 C52 120 . . ? C50 C51 H51 120 . . ? C52 C51 H51 120 . . ? C51 C52 C53 120 . . ? C51 C52 H52 120 . . ? C53 C52 H52 120 . . ? C52 C53 N2 120 . . ? C52 C53 H53 120 . . ? N2 C53 H53 120 . . ? C57 C54 N1 109.1(7) . . ? C57 C54 C55 112.4(9) . . ? N1 C54 C55 108.3(8) . . ? C57 C54 C56 107.1(8) . . ? N1 C54 C56 103.6(7) . . ? C55 C54 C56 115.9(8) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.4 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.4 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C58A N3A C62A 120 . . ? C59A C58A N3A 120 . . ? C59A C58A H58A 120 . . ? N3A C58A H58A 120 . . ? C60A C59A C58A 120 . . ? C60A C59A H59A 120 . . ? C58A C59A H59A 120 . . ? C59A C60A C61A 120 . . ? C59A C60A H60A 120 . . ? C61A C60A H60A 120 . . ? C60A C61A C62A 120 . . ? C60A C61A H61A 120 . . ? C62A C61A H61A 120 . . ? C61A C62A N3A 120 . . ? C61A C62A H62A 120 . . ? N3A C62A H62A 120 . . ? C58B N3B C62B 120 . . ? C59B C58B N3B 120 . . ? C59B C58B H58B 120 . . ? N3B C58B H58B 120 . . ? C58B C59B C60A 120 . . ? C58B C59B H59B 120 . . ? C60A C59B H59B 120 . . ? C61B C60A C59B 120 . . ? C61B C60A H60B 120 . . ? C59B C60A H60B 120 . . ? C60A C61B C62B 120 . . ? C60A C61B H61B 120 . . ? C62B C61B H61B 120 . . ? C61B C62B N3B 120 . . ? C61B C62B H62B 120 . . ? N3B C62B H62B 120 . . ? data_lkcr4 _audit_creation_date 1999-05-14T11:28:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H58 O8 N2 SI4 CR2' _chemical_formula_structural 'C56 H58 O8 N2 SI4 CR2' _chemical_formula_sum 'C63 H66 Cr2 N2 O8 Si4' _chemical_formula_weight 1195.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.931(7) _cell_length_b 15.948(9) _cell_length_c 16.469(8) _cell_angle_alpha 68.08(6) _cell_angle_beta 111.08(5) _cell_angle_gamma 89.96(7) _cell_volume 3129(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_factor_muR 0.106 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7806 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_correction_T_ave 0.8551 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 23 _diffrn_standards_decay_corr_max 1.624 _diffrn_standards_decay_corr_min 0.899 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -5 2 0 -8 _diffrn_reflns_number 9964 _diffrn_reflns_av_R_equivalents 0.3003 _diffrn_reflns_av_sigmaI/netI 0.2745 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.874 _diffrn_measured_fraction_theta_max 0.874 _reflns_number_total 9614 _reflns_number_gt 3953 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 /PC (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4 /PC (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 9614 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2487 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2077 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.441 _refine_ls_shift/su_mean 0.017 _refine_diff_density_max 0.801 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cr1 Cr 0.38563(10) 0.20024(8) 0.44324(9) 0.0297(4) Uani 1 1 d . . . Cr2 Cr 0.11228(10) -0.33970(8) 0.55428(9) 0.0284(4) Uani 1 1 d . . . Si1 Si 0.42650(19) 0.05827(15) 0.65475(16) 0.0324(6) Uani 1 1 d . . . Si2 Si 0.41973(19) 0.10694(15) 0.31270(16) 0.0322(6) Uani 1 1 d . . . Si3 Si 0.07488(18) -0.32498(14) 0.34641(16) 0.0288(6) Uani 1 1 d . . . Si4 Si -0.07756(18) -0.46586(14) 0.31699(16) 0.0282(6) Uani 1 1 d . . . O1 O 0.3967(5) 0.3046(3) 0.4106(4) 0.0433(16) Uani 1 1 d . . . O2 O 0.4478(4) 0.1463(3) 0.3950(4) 0.0308(14) Uani 1 1 d . . . O3 O 0.4347(4) 0.1475(4) 0.5687(4) 0.0365(14) Uani 1 1 d . . . O4 O 0.5177(4) 0.0319(4) 0.3437(4) 0.0424(15) Uani 1 1 d . . . O5 O 0.1002(4) -0.2598(4) 0.5858(4) 0.0419(15) Uani 1 1 d . . . O6 O 0.0494(4) -0.4302(3) 0.6026(4) 0.0293(13) Uani 1 1 d . . . O7 O 0.0648(4) -0.2968(3) 0.4287(4) 0.0322(14) Uani 1 1 d . . . O8 O 0.0218(4) -0.4157(3) 0.3497(4) 0.0352(14) Uani 1 1 d . . . N1 N 0.2623(5) 0.1947(4) 0.3995(4) 0.0332(17) Uani 1 1 d . . . N2 N 0.2355(5) -0.3796(4) 0.5998(4) 0.0346(18) Uani 1 1 d . . . C1 C 0.5005(5) 0.0765(4) 0.7654(3) 0.038(2) Uani 1 1 d G . . C2 C 0.5996(5) 0.0994(4) 0.7784(4) 0.052(3) Uani 1 1 d G . . H2 H 0.6279 0.103 0.7342 0.104(17) Uiso 1 1 calc R . . C3 C 0.6565(4) 0.1167(4) 0.8576(5) 0.078(4) Uani 1 1 d G . . H3 H 0.7228 0.132 0.8664 0.104(17) Uiso 1 1 calc R . . C4 C 0.6142(7) 0.1112(5) 0.9238(4) 0.094(5) Uani 1 1 d G . . H4 H 0.6523 0.1228 0.9768 0.104(17) Uiso 1 1 calc R . . C5 C 0.5151(7) 0.0884(5) 0.9108(4) 0.082(4) Uani 1 1 d G . . H5 H 0.4868 0.0847 0.9551 0.104(17) Uiso 1 1 calc R . . C6 C 0.4582(5) 0.0710(4) 0.8316(5) 0.056(3) Uani 1 1 d G . . H6 H 0.3919 0.0557 0.8229 0.104(17) Uiso 1 1 calc R . . C7 C 0.2884(4) 0.0437(4) 0.6370(4) 0.032(2) Uani 1 1 d G . . C8 C 0.2206(5) 0.1099(3) 0.6339(4) 0.050(3) Uani 1 1 d G . . H8 H 0.2442 0.1619 0.642 0.068(13) Uiso 1 1 calc R . . C9 C 0.1175(4) 0.0984(4) 0.6185(5) 0.056(3) Uani 1 1 d G . . H9 H 0.0722 0.1427 0.6164 0.068(13) Uiso 1 1 calc R . . C10 C 0.0823(4) 0.0208(5) 0.6063(5) 0.053(3) Uani 1 1 d G . . H10 H 0.0133 0.0131 0.596 0.068(13) Uiso 1 1 calc R . . C11 C 0.1501(5) -0.0454(4) 0.6094(5) 0.065(3) Uani 1 1 d G . . H11 H 0.1265 -0.0974 0.6013 0.068(13) Uiso 1 1 calc R . . C12 C 0.2531(5) -0.0339(3) 0.6248(5) 0.051(3) Uani 1 1 d G . . H12 H 0.2985 -0.0782 0.6269 0.068(13) Uiso 1 1 calc R . . C13 C 0.4035(5) 0.2014(4) 0.1976(4) 0.041(2) Uani 1 1 d G . . C14 C 0.3846(5) 0.2921(4) 0.1844(4) 0.054(3) Uani 1 1 d G . . H14 H 0.379 0.3059 0.2328 0.103(18) Uiso 1 1 calc R . . C15 C 0.3741(6) 0.3622(3) 0.0988(5) 0.068(3) Uani 1 1 d G . . H15 H 0.3615 0.4229 0.09 0.103(18) Uiso 1 1 calc R . . C16 C 0.3825(7) 0.3416(5) 0.0265(4) 0.093(4) Uani 1 1 d G . . H16 H 0.3755 0.3885 -0.0307 0.103(18) Uiso 1 1 calc R . . C17 C 0.4014(7) 0.2508(6) 0.0398(4) 0.108(5) Uani 1 1 d G . . H17 H 0.407 0.2371 -0.0086 0.103(18) Uiso 1 1 calc R . . C18 C 0.4119(6) 0.1807(4) 0.1253(5) 0.081(4) Uani 1 1 d G . . H18 H 0.4245 0.1201 0.1342 0.103(18) Uiso 1 1 calc R . . C19 C 0.3006(4) 0.0507(4) 0.3038(4) 0.033(2) Uani 1 1 d G . . C20 C 0.2203(5) 0.0691(4) 0.2165(3) 0.053(3) Uani 1 1 d G . . H20 H 0.2239 0.1117 0.1612 0.078(14) Uiso 1 1 calc R . . C21 C 0.1344(4) 0.0239(5) 0.2119(4) 0.065(3) Uani 1 1 d G . . H21 H 0.0807 0.0362 0.1535 0.078(14) Uiso 1 1 calc R . . C22 C 0.1290(4) -0.0397(4) 0.2946(6) 0.059(3) Uani 1 1 d G . . H22 H 0.0715 -0.0699 0.2915 0.078(14) Uiso 1 1 calc R . . C23 C 0.2093(6) -0.0581(4) 0.3818(5) 0.060(3) Uani 1 1 d G . . H23 H 0.2056 -0.1006 0.4371 0.078(14) Uiso 1 1 calc R . . C24 C 0.2951(4) -0.0129(4) 0.3864(3) 0.046(2) Uani 1 1 d G . . H24 H 0.3489 -0.0252 0.4448 0.078(14) Uiso 1 1 calc R . . C25 C 0.1581(7) 0.2468(6) 0.3424(7) 0.042(2) Uani 1 1 d . . . C26 C 0.0816(7) 0.1776(7) 0.3485(7) 0.065(3) Uani 1 1 d . . . H26A H 0.0116 0.2093 0.3107 0.112(14) Uiso 1 1 calc R . . H26B H 0.0894 0.1461 0.4134 0.112(14) Uiso 1 1 calc R . . H26C H 0.0959 0.1341 0.3253 0.112(14) Uiso 1 1 calc R . . C27 C 0.1420(8) 0.3132(7) 0.3855(8) 0.071(3) Uani 1 1 d . . . H27A H 0.0712 0.3437 0.3534 0.112(14) Uiso 1 1 calc R . . H27B H 0.1881 0.3577 0.3782 0.112(14) Uiso 1 1 calc R . . H27C H 0.1567 0.2799 0.4517 0.112(14) Uiso 1 1 calc R . . C28 C 0.1491(8) 0.2951(7) 0.2415(7) 0.075(4) Uani 1 1 d . . . H28A H 0.1899 0.3439 0.2371 0.112(14) Uiso 1 1 calc R . . H28B H 0.0775 0.3197 0.2007 0.112(14) Uiso 1 1 calc R . . H28C H 0.1742 0.2525 0.2224 0.112(14) Uiso 1 1 calc R . . C29 C 0.2129(4) -0.3548(4) 0.3650(4) 0.036(2) Uani 1 1 d G . . C30 C 0.2820(5) -0.2923(3) 0.3703(4) 0.048(3) Uani 1 1 d G . . H30 H 0.2594 -0.2344 0.3639 0.080(14) Uiso 1 1 calc R . . C31 C 0.3847(4) -0.3163(4) 0.3852(5) 0.049(3) Uani 1 1 d G . . H31 H 0.4309 -0.2745 0.3888 0.080(14) Uiso 1 1 calc R . . C32 C 0.4184(4) -0.4028(4) 0.3948(5) 0.058(3) Uani 1 1 d G . . H32 H 0.4872 -0.4189 0.4047 0.080(14) Uiso 1 1 calc R . . C33 C 0.3494(5) -0.4653(3) 0.3894(5) 0.058(3) Uani 1 1 d G . . H33 H 0.3719 -0.5232 0.3958 0.080(14) Uiso 1 1 calc R . . C34 C 0.2466(4) -0.4413(3) 0.3745(5) 0.047(3) Uani 1 1 d G . . H34 H 0.2004 -0.4831 0.371 0.080(14) Uiso 1 1 calc R . . C35 C 0.0025(4) -0.2264(3) 0.2312(3) 0.032(2) Uani 1 1 d G . . C36 C 0.0461(4) -0.1925(4) 0.1637(4) 0.045(2) Uani 1 1 d G . . H36 H 0.1134 -0.217 0.1771 0.113(18) Uiso 1 1 calc R . . C37 C -0.0107(6) -0.1221(4) 0.0763(4) 0.074(3) Uani 1 1 d G . . H37 H 0.0184 -0.0995 0.0312 0.113(18) Uiso 1 1 calc R . . C38 C -0.1112(6) -0.0855(4) 0.0564(4) 0.084(4) Uani 1 1 d G . . H38 H -0.1493 -0.0384 -0.0021 0.113(18) Uiso 1 1 calc R . . C39 C -0.1548(4) -0.1194(4) 0.1238(5) 0.076(4) Uani 1 1 d G . . H39 H -0.222 -0.0949 0.1105 0.113(18) Uiso 1 1 calc R . . C40 C -0.0979(5) -0.1898(4) 0.2112(4) 0.051(3) Uani 1 1 d G . . H40 H -0.1271 -0.2124 0.2564 0.113(18) Uiso 1 1 calc R . . C41 C -0.0942(5) -0.4694(4) 0.1998(3) 0.036(2) Uani 1 1 d G . . C42 C -0.0788(6) -0.3944(4) 0.1307(5) 0.077(4) Uani 1 1 d G . . H42 H -0.0623 -0.3421 0.1418 0.073(14) Uiso 1 1 calc R . . C43 C -0.0880(7) -0.3975(5) 0.0450(4) 0.100(5) Uani 1 1 d G . . H43 H -0.0776 -0.3473 -0.0012 0.073(14) Uiso 1 1 calc R . . C44 C -0.1125(6) -0.4757(6) 0.0285(4) 0.079(4) Uani 1 1 d G . . H44 H -0.1187 -0.4778 -0.0289 0.073(14) Uiso 1 1 calc R . . C45 C -0.1279(5) -0.5507(4) 0.0976(5) 0.064(3) Uani 1 1 d G . . H45 H -0.1444 -0.603 0.0865 0.073(14) Uiso 1 1 calc R . . C46 C -0.1187(5) -0.5476(3) 0.1832(4) 0.053(3) Uani 1 1 d G . . H46 H -0.129 -0.5978 0.2295 0.073(14) Uiso 1 1 calc R . . C47 C -0.1959(4) -0.4045(3) 0.3115(4) 0.032(2) Uani 1 1 d G . . C48 C -0.2790(5) -0.3593(4) 0.2252(3) 0.048(3) Uani 1 1 d G . . H48 H -0.2764 -0.36 0.1698 0.054(12) Uiso 1 1 calc R . . C49 C -0.3661(4) -0.3132(4) 0.2217(4) 0.058(3) Uani 1 1 d G . . H49 H -0.4217 -0.2829 0.1639 0.054(12) Uiso 1 1 calc R . . C50 C -0.3700(4) -0.3122(4) 0.3045(5) 0.051(3) Uani 1 1 d G . . H50 H -0.4282 -0.2813 0.3021 0.054(12) Uiso 1 1 calc R . . C51 C -0.2868(5) -0.3573(4) 0.3908(4) 0.054(3) Uani 1 1 d G . . H51 H -0.2894 -0.3567 0.4462 0.054(12) Uiso 1 1 calc R . . C52 C -0.1998(4) -0.4035(4) 0.3944(3) 0.045(2) Uani 1 1 d G . . H52 H -0.1441 -0.4337 0.4521 0.054(12) Uiso 1 1 calc R . . C53 C -0.3406(7) -0.6297(5) 0.3454(7) 0.043(2) Uani 1 1 d . . . C54 C 0.3557(8) -0.2710(6) 0.6102(7) 0.065(3) Uani 1 1 d . . . H54A H 0.4222 -0.2622 0.6484 0.097(13) Uiso 1 1 calc R . . H54B H 0.3015 -0.2311 0.6069 0.097(13) Uiso 1 1 calc R . . H54C H 0.3528 -0.2574 0.5474 0.097(13) Uiso 1 1 calc R . . C55 C -0.4188(7) -0.5658(7) 0.3503(7) 0.065(3) Uani 1 1 d . . . H55A H -0.4884 -0.5706 0.3139 0.097(13) Uiso 1 1 calc R . . H55B H -0.4068 -0.5038 0.3248 0.097(13) Uiso 1 1 calc R . . H55C H -0.4102 -0.5828 0.4152 0.097(13) Uiso 1 1 calc R . . C56 C -0.3493(8) -0.6036(8) 0.2452(7) 0.076(4) Uani 1 1 d . . . H56A H -0.4163 -0.6127 0.2079 0.097(13) Uiso 1 1 calc R . . H56B H -0.2956 -0.6411 0.2449 0.097(13) Uiso 1 1 calc R . . H56C H -0.3417 -0.5405 0.2188 0.097(13) Uiso 1 1 calc R . . C57 C -0.280(3) -0.6721(12) -0.0587(12) 0.24(2) Uani 1 1 d G . . C58 C -0.3297(11) -0.6951(19) 0.004(3) 0.181(13) Uani 1 1 d G . . H58 H -0.3959 -0.6646 -0.0144 0.48(10) Uiso 1 1 calc R . . C59 C -0.281(3) -0.764(2) 0.095(2) 0.229(18) Uani 1 1 d G . . H59 H -0.3147 -0.7792 0.1366 0.48(10) Uiso 1 1 calc R . . C60 C -0.182(3) -0.8093(11) 0.1222(14) 0.23(2) Uani 1 1 d G . . H60 H -0.1497 -0.8553 0.1828 0.48(10) Uiso 1 1 calc R . . C61 C -0.1321(12) -0.786(2) 0.059(3) 0.27(3) Uani 1 1 d G . . H61 H -0.0659 -0.8168 0.0779 0.48(10) Uiso 1 1 calc R . . C62 C -0.181(3) -0.718(2) -0.031(3) 0.222(18) Uani 1 1 d G . . H62 H -0.1471 -0.7023 -0.0731 0.48(10) Uiso 1 1 calc R . . C63 C -0.301(4) -0.611(2) -0.143(2) 0.41(4) Uani 1 1 d . . . H63A H -0.239 -0.5891 -0.148 0.9(3) Uiso 1 1 calc R . . H63B H -0.3505 -0.5615 -0.1546 0.9(3) Uiso 1 1 calc R . . H63C H -0.3311 -0.6378 -0.188 0.9(3) 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 Cr1 0.0297(9) 0.0250(8) 0.0376(8) -0.0133(6) 0.0156(7) -0.0060(6) Cr2 0.0272(9) 0.0233(7) 0.0386(8) -0.0147(6) 0.0144(7) -0.0076(6) Si1 0.0302(16) 0.0325(14) 0.0379(14) -0.0154(11) 0.0153(12) -0.0039(11) Si2 0.0311(16) 0.0314(13) 0.0366(14) -0.0145(11) 0.0149(11) -0.0032(11) Si3 0.0269(15) 0.0238(12) 0.0345(14) -0.0097(10) 0.0127(11) -0.0078(10) Si4 0.0266(15) 0.0263(13) 0.0352(14) -0.0135(11) 0.0146(11) -0.0078(10) O1 0.058(4) 0.021(3) 0.057(4) -0.017(3) 0.026(3) -0.011(3) O2 0.025(3) 0.032(3) 0.038(3) -0.015(3) 0.015(3) -0.007(3) O3 0.031(4) 0.044(4) 0.030(3) -0.015(3) 0.007(3) -0.007(3) O4 0.031(4) 0.044(4) 0.061(4) -0.033(3) 0.016(3) 0.000(3) O5 0.048(4) 0.037(3) 0.058(4) -0.033(3) 0.025(3) -0.016(3) O6 0.019(3) 0.025(3) 0.045(3) -0.012(3) 0.015(3) -0.008(2) O7 0.033(4) 0.031(3) 0.038(3) -0.015(3) 0.019(3) -0.006(3) O8 0.034(4) 0.027(3) 0.041(4) -0.011(3) 0.013(3) -0.014(3) N1 0.023(5) 0.040(4) 0.036(4) -0.020(3) 0.005(3) 0.000(3) N2 0.026(5) 0.033(4) 0.032(4) -0.005(3) 0.006(3) -0.007(3) C1 0.046(7) 0.019(4) 0.031(5) -0.004(4) 0.002(4) 0.004(4) C2 0.045(7) 0.053(6) 0.058(7) -0.033(5) 0.009(5) -0.012(5) C3 0.093(10) 0.049(7) 0.066(8) -0.027(6) -0.001(7) -0.007(6) C4 0.144(14) 0.068(8) 0.055(8) -0.045(7) 0.001(9) -0.005(8) C5 0.141(13) 0.066(8) 0.040(7) -0.026(6) 0.031(8) -0.013(8) C6 0.085(9) 0.041(6) 0.048(6) -0.016(5) 0.036(6) -0.009(5) C7 0.024(6) 0.033(5) 0.048(5) -0.018(4) 0.020(4) -0.010(4) C8 0.032(7) 0.054(6) 0.076(7) -0.032(5) 0.030(5) -0.007(5) C9 0.054(8) 0.045(6) 0.084(8) -0.036(6) 0.032(6) -0.007(5) C10 0.028(6) 0.073(7) 0.072(7) -0.038(6) 0.026(5) -0.015(5) C11 0.057(8) 0.049(7) 0.105(9) -0.042(6) 0.038(7) -0.025(6) C12 0.039(7) 0.047(6) 0.086(8) -0.035(6) 0.037(6) -0.011(5) C13 0.025(6) 0.048(6) 0.035(5) -0.010(4) 0.004(4) 0.003(4) C14 0.046(7) 0.051(6) 0.046(6) -0.006(5) 0.010(5) -0.004(5) C15 0.066(8) 0.049(7) 0.064(8) -0.008(6) 0.011(6) -0.012(6) C16 0.114(12) 0.095(11) 0.048(8) -0.011(7) 0.028(8) -0.034(9) C17 0.183(16) 0.076(9) 0.073(10) -0.022(8) 0.069(10) -0.003(9) C18 0.120(11) 0.077(8) 0.040(7) -0.016(6) 0.032(7) 0.001(7) C19 0.026(5) 0.035(5) 0.042(5) -0.023(4) 0.009(4) -0.001(4) C20 0.039(7) 0.061(7) 0.071(8) -0.041(6) 0.019(6) -0.020(5) C21 0.034(7) 0.091(9) 0.077(8) -0.055(7) 0.006(6) -0.015(6) C22 0.057(8) 0.058(7) 0.095(9) -0.058(7) 0.037(7) -0.026(6) C23 0.068(9) 0.041(6) 0.067(8) -0.010(5) 0.036(7) 0.004(6) C24 0.046(7) 0.036(5) 0.056(7) -0.015(5) 0.022(5) -0.015(5) C25 0.020(6) 0.052(6) 0.065(7) -0.034(5) 0.014(5) -0.005(5) C26 0.027(6) 0.092(8) 0.082(8) -0.050(7) 0.012(6) -0.004(6) C27 0.043(7) 0.076(8) 0.102(9) -0.054(7) 0.019(6) 0.009(6) C28 0.049(7) 0.095(9) 0.052(7) -0.001(6) 0.017(6) 0.023(6) C29 0.043(6) 0.027(5) 0.042(5) -0.012(4) 0.024(5) -0.014(4) C30 0.040(7) 0.039(6) 0.070(7) -0.021(5) 0.030(5) -0.006(5) C31 0.037(7) 0.042(6) 0.070(7) -0.020(5) 0.025(5) -0.015(5) C32 0.043(7) 0.064(7) 0.071(7) -0.017(6) 0.036(6) -0.002(6) C33 0.056(8) 0.032(6) 0.104(9) -0.028(6) 0.050(7) -0.015(5) C34 0.031(7) 0.037(6) 0.088(8) -0.027(5) 0.037(5) -0.018(5) C35 0.035(6) 0.030(5) 0.036(5) -0.014(4) 0.017(4) -0.007(4) C36 0.057(7) 0.040(5) 0.035(6) -0.009(4) 0.022(5) -0.008(5) C37 0.087(10) 0.070(8) 0.054(7) -0.003(6) 0.037(7) -0.010(7) C38 0.097(11) 0.068(8) 0.059(8) 0.000(6) 0.025(8) -0.011(8) C39 0.062(8) 0.057(7) 0.087(9) -0.018(7) 0.015(7) 0.013(6) C40 0.053(7) 0.042(6) 0.050(6) -0.017(5) 0.013(5) 0.000(5) C41 0.023(5) 0.043(5) 0.052(6) -0.023(5) 0.021(4) -0.006(4) C42 0.106(10) 0.101(9) 0.063(8) -0.050(7) 0.058(7) -0.068(8) C43 0.154(14) 0.115(11) 0.064(8) -0.045(8) 0.067(9) -0.079(10) C44 0.058(8) 0.142(12) 0.050(7) -0.056(8) 0.019(6) -0.009(8) C45 0.053(7) 0.072(8) 0.061(7) -0.047(6) -0.006(6) 0.014(6) C46 0.048(7) 0.062(7) 0.048(6) -0.031(5) 0.007(5) 0.001(5) C47 0.022(5) 0.029(5) 0.051(6) -0.019(4) 0.017(4) -0.019(4) C48 0.033(6) 0.060(6) 0.046(6) -0.019(5) 0.012(5) 0.005(5) C49 0.042(7) 0.052(6) 0.056(7) -0.004(5) 0.011(5) 0.019(5) C50 0.053(7) 0.032(5) 0.083(8) -0.024(5) 0.041(7) -0.003(5) C51 0.068(8) 0.039(6) 0.072(8) -0.028(5) 0.042(7) -0.015(5) C52 0.054(7) 0.050(6) 0.041(6) -0.023(5) 0.024(5) -0.008(5) C53 0.033(6) 0.030(5) 0.058(7) -0.011(5) 0.016(5) -0.010(4) C54 0.046(7) 0.054(7) 0.089(8) -0.027(6) 0.021(6) -0.021(5) C55 0.025(6) 0.066(7) 0.086(8) -0.013(6) 0.021(6) 0.002(5) C56 0.047(8) 0.109(10) 0.066(8) -0.036(7) 0.013(6) -0.029(7) C57 0.38(6) 0.26(4) 0.25(4) -0.23(3) 0.19(4) -0.21(4) C58 0.15(2) 0.21(3) 0.21(3) -0.16(3) 0.02(2) -0.062(18) C59 0.20(3) 0.31(6) 0.32(6) -0.26(5) 0.11(3) -0.14(3) C60 0.24(4) 0.18(2) 0.23(3) -0.14(2) -0.01(3) -0.04(3) C61 0.21(3) 0.33(6) 0.36(6) -0.30(6) 0.06(4) -0.05(3) C62 0.21(3) 0.24(4) 0.32(5) -0.24(4) 0.09(3) -0.07(3) C63 0.76(10) 0.19(3) 0.12(2) -0.04(2) 0.00(3) -0.08(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cr1 O1 1.573(5) . ? Cr1 N1 1.624(7) . ? Cr1 O2 1.767(5) . ? Cr1 O3 1.769(5) . ? Cr2 O5 1.574(5) . ? Cr2 N2 1.621(7) . ? Cr2 O6 1.769(5) . ? Cr2 O7 1.772(5) . ? Si1 O4 1.621(6) 2_656 ? Si1 O3 1.630(6) . ? Si1 C7 1.868(5) . ? Si1 C1 1.874(5) . ? Si2 O4 1.611(6) . ? Si2 O2 1.625(5) . ? Si2 C13 1.863(5) . ? Si2 C19 1.872(5) . ? Si3 O8 1.617(5) . ? Si3 O7 1.629(5) . ? Si3 C29 1.867(5) . ? Si3 C35 1.867(5) . ? Si4 O8 1.623(5) . ? Si4 O6 1.625(5) 2_546 ? Si4 C47 1.873(5) . ? Si4 C41 1.883(5) . ? O4 Si1 1.621(6) 2_656 ? O6 Si4 1.625(5) 2_546 ? N1 C25 1.454(10) . ? N2 C53 1.460(10) 2_546 ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C2 H2 0.93 . ? C3 C4 1.39 . ? C3 H3 0.93 . ? C4 C5 1.39 . ? C4 H4 0.93 . ? C5 C6 1.39 . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.39 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C8 H8 0.93 . ? C9 C10 1.39 . ? C9 H9 0.93 . ? C10 C11 1.39 . ? C10 H10 0.93 . ? C11 C12 1.39 . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C14 H14 0.93 . ? C15 C16 1.39 . ? C15 H15 0.93 . ? C16 C17 1.39 . ? C16 H16 0.93 . ? C17 C18 1.39 . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C20 H20 0.93 . ? C21 C22 1.39 . ? C21 H21 0.93 . ? C22 C23 1.39 . ? C22 H22 0.93 . ? C23 C24 1.39 . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C28 1.505(13) . ? C25 C27 1.533(12) . ? C25 C26 1.536(12) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C30 1.39 . ? C29 C34 1.39 . ? C30 C31 1.39 . ? C30 H30 0.93 . ? C31 C32 1.39 . ? C31 H31 0.93 . ? C32 C33 1.39 . ? C32 H32 0.93 . ? C33 C34 1.39 . ? C33 H33 0.93 . ? C34 H34 0.93 . ? C35 C36 1.39 . ? C35 C40 1.39 . ? C36 C37 1.39 . ? C36 H36 0.93 . ? C37 C38 1.39 . ? C37 H37 0.93 . ? C38 C39 1.39 . ? C38 H38 0.93 . ? C39 C40 1.39 . ? C39 H39 0.93 . ? C40 H40 0.93 . ? C41 C42 1.39 . ? C41 C46 1.39 . ? C42 C43 1.39 . ? C42 H42 0.93 . ? C43 C44 1.39 . ? C43 H43 0.93 . ? C44 C45 1.39 . ? C44 H44 0.93 . ? C45 C46 1.39 . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C47 C48 1.39 . ? C47 C52 1.39 . ? C48 C49 1.39 . ? C48 H48 0.93 . ? C49 C50 1.39 . ? C49 H49 0.93 . ? C50 C51 1.39 . ? C50 H50 0.93 . ? C51 C52 1.39 . ? C51 H51 0.93 . ? C52 H52 0.93 . ? C53 N2 1.460(10) 2_546 ? C53 C56 1.502(13) . ? C53 C54 1.526(11) 2_546 ? C53 C55 1.535(12) . ? C54 C53 1.526(11) 2_546 ? C54 H54A 0.96 . ? C54 H54B 0.96 . ? C54 H54C 0.96 . ? C55 H55A 0.96 . ? C55 H55B 0.96 . ? C55 H55C 0.96 . ? C56 H56A 0.96 . ? C56 H56B 0.96 . ? C56 H56C 0.96 . ? C57 C63 1.28(3) . ? C57 C58 1.39 . ? C57 C62 1.39 . ? C58 C59 1.39 . ? C58 H58 0.93 . ? C59 C60 1.39 . ? C59 H59 0.93 . ? C60 C61 1.39 . ? C60 H60 0.93 . ? C61 C62 1.39 . ? C61 H61 0.93 . ? C62 H62 0.93 . ? C63 H63A 0.9652 . ? C63 H63B 0.9653 . ? C63 H63C 0.9653 . ? 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 O1 Cr1 N1 107.0(3) . . ? O1 Cr1 O2 110.6(3) . . ? N1 Cr1 O2 107.2(3) . . ? O1 Cr1 O3 109.6(3) . . ? N1 Cr1 O3 109.9(3) . . ? O2 Cr1 O3 112.4(3) . . ? O5 Cr2 N2 107.1(3) . . ? O5 Cr2 O6 110.4(3) . . ? N2 Cr2 O6 107.0(3) . . ? O5 Cr2 O7 109.8(3) . . ? N2 Cr2 O7 110.0(3) . . ? O6 Cr2 O7 112.5(2) . . ? O4 Si1 O3 108.1(3) 2_656 . ? O4 Si1 C7 107.6(3) 2_656 . ? O3 Si1 C7 112.0(3) . . ? O4 Si1 C1 110.5(3) 2_656 . ? O3 Si1 C1 104.9(3) . . ? C7 Si1 C1 113.6(3) . . ? O4 Si2 O2 106.7(3) . . ? O4 Si2 C13 108.9(3) . . ? O2 Si2 C13 109.6(3) . . ? O4 Si2 C19 109.2(3) . . ? O2 Si2 C19 110.6(3) . . ? C13 Si2 C19 111.7(3) . . ? O8 Si3 O7 108.5(3) . . ? O8 Si3 C29 106.3(3) . . ? O7 Si3 C29 112.8(3) . . ? O8 Si3 C35 110.6(3) . . ? O7 Si3 C35 106.3(3) . . ? C29 Si3 C35 112.3(3) . . ? O8 Si4 O6 106.4(3) . 2_546 ? O8 Si4 C47 109.5(3) . . ? O6 Si4 C47 110.1(3) 2_546 . ? O8 Si4 C41 108.8(3) . . ? O6 Si4 C41 109.1(3) 2_546 . ? C47 Si4 C41 112.6(3) . . ? Si2 O2 Cr1 140.3(3) . . ? Si1 O3 Cr1 141.0(3) . . ? Si2 O4 Si1 154.2(4) . 2_656 ? Si4 O6 Cr2 140.0(3) 2_546 . ? Si3 O7 Cr2 139.2(3) . . ? Si3 O8 Si4 151.8(4) . . ? C25 N1 Cr1 145.6(6) . . ? C53 N2 Cr2 146.4(6) 2_546 . ? C2 C1 C6 120 . . ? C2 C1 Si1 117.6(4) . . ? C6 C1 Si1 122.4(4) . . ? C1 C2 C3 120 . . ? C1 C2 H2 120 . . ? C3 C2 H2 120 . . ? C4 C3 C2 120 . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C8 C7 C12 120 . . ? C8 C7 Si1 121.1(4) . . ? C12 C7 Si1 118.9(4) . . ? C9 C8 C7 120 . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 120 . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C11 C10 C9 120 . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C10 C11 C12 120 . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C11 C12 C7 120 . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C14 C13 C18 120 . . ? C14 C13 Si2 120.3(4) . . ? C18 C13 Si2 119.7(4) . . ? C13 C14 C15 120 . . ? C13 C14 H14 120 . . ? C15 C14 H14 120 . . ? C16 C15 C14 120 . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C17 C16 C15 120 . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 120 . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? C17 C18 C13 120 . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? C20 C19 C24 120 . . ? C20 C19 Si2 121.4(4) . . ? C24 C19 Si2 118.6(4) . . ? C19 C20 C21 120 . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C20 C21 C22 120 . . ? C20 C21 H21 120 . . ? C22 C21 H21 120 . . ? C23 C22 C21 120 . . ? C23 C22 H22 120 . . ? C21 C22 H22 120 . . ? C22 C23 C24 120 . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C23 C24 C19 120 . . ? C23 C24 H24 120 . . ? C19 C24 H24 120 . . ? N1 C25 C28 108.3(7) . . ? N1 C25 C27 107.8(7) . . ? C28 C25 C27 112.7(9) . . ? N1 C25 C26 106.9(7) . . ? C28 C25 C26 110.3(8) . . ? C27 C25 C26 110.7(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120 . . ? C30 C29 Si3 121.0(4) . . ? C34 C29 Si3 119.0(4) . . ? C31 C30 C29 120 . . ? C31 C30 H30 120 . . ? C29 C30 H30 120 . . ? C30 C31 C32 120 . . ? C30 C31 H31 120 . . ? C32 C31 H31 120 . . ? C31 C32 C33 120 . . ? C31 C32 H32 120 . . ? C33 C32 H32 120 . . ? C34 C33 C32 120 . . ? C34 C33 H33 120 . . ? C32 C33 H33 120 . . ? C33 C34 C29 120 . . ? C33 C34 H34 120 . . ? C29 C34 H34 120 . . ? C36 C35 C40 120 . . ? C36 C35 Si3 120.6(4) . . ? C40 C35 Si3 119.3(4) . . ? C35 C36 C37 120 . . ? C35 C36 H36 120 . . ? C37 C36 H36 120 . . ? C36 C37 C38 120 . . ? C36 C37 H37 120 . . ? C38 C37 H37 120 . . ? C39 C38 C37 120 . . ? C39 C38 H38 120 . . ? C37 C38 H38 120 . . ? C38 C39 C40 120 . . ? C38 C39 H39 120 . . ? C40 C39 H39 120 . . ? C39 C40 C35 120 . . ? C39 C40 H40 120 . . ? C35 C40 H40 120 . . ? C42 C41 C46 120 . . ? C42 C41 Si4 119.7(4) . . ? C46 C41 Si4 120.3(4) . . ? C43 C42 C41 120 . . ? C43 C42 H42 120 . . ? C41 C42 H42 120 . . ? C42 C43 C44 120 . . ? C42 C43 H43 120 . . ? C44 C43 H43 120 . . ? C45 C44 C43 120 . . ? C45 C44 H44 120 . . ? C43 C44 H44 120 . . ? C44 C45 C46 120 . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C45 C46 C41 120 . . ? C45 C46 H46 120 . . ? C41 C46 H46 120 . . ? C48 C47 C52 120 . . ? C48 C47 Si4 120.4(4) . . ? C52 C47 Si4 119.6(4) . . ? C49 C48 C47 120 . . ? C49 C48 H48 120 . . ? C47 C48 H48 120 . . ? C50 C49 C48 120 . . ? C50 C49 H49 120 . . ? C48 C49 H49 120 . . ? C49 C50 C51 120 . . ? C49 C50 H50 120 . . ? C51 C50 H50 120 . . ? C52 C51 C50 120 . . ? C52 C51 H51 120 . . ? C50 C51 H51 120 . . ? C51 C52 C47 120 . . ? C51 C52 H52 120 . . ? C47 C52 H52 120 . . ? N2 C53 C56 107.1(7) 2_546 . ? N2 C53 C54 108.2(7) 2_546 2_546 ? C56 C53 C54 111.6(8) . 2_546 ? N2 C53 C55 108.5(7) 2_546 . ? C56 C53 C55 111.3(8) . . ? C54 C53 C55 110.0(8) 2_546 . ? C53 C54 H54A 109.5 2_546 . ? C53 C54 H54B 109.5 2_546 . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 2_546 . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C63 C57 C58 134(4) . . ? C63 C57 C62 106(4) . . ? C58 C57 C62 120 . . ? C59 C58 C57 120 . . ? C59 C58 H58 120 . . ? C57 C58 H58 120 . . ? C58 C59 C60 120 . . ? C58 C59 H59 120 . . ? C60 C59 H59 120 . . ? C59 C60 C61 120 . . ? C59 C60 H60 120 . . ? C61 C60 H60 120 . . ? C62 C61 C60 120 . . ? C62 C61 H61 120 . . ? C60 C61 H61 120 . . ? C61 C62 C57 120 . . ? C61 C62 H62 120 . . ? C57 C62 H62 120 . . ? C57 C63 H63A 110 . . ? C57 C63 H63B 110.1 . . ? H63A C63 H63B 108.8 . . ? C57 C63 H63C 110.2 . . ? H63A C63 H63C 108.8 . . ? H63B C63 H63C 108.8 . . ?