# Electronic Supplementary Material (ESI) for Chemical Communications # 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_9 _audit_creation_date 2013-06-18T13:47:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C51 H49 I6 N11 O7' _chemical_formula_sum 'C17 H12 I2 N2 O2' _chemical_formula_weight 530.09 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.385(4) _cell_length_b 4.1207(6) _cell_length_c 15.706(2) _cell_angle_alpha 90 _cell_angle_beta 98.230(4) _cell_angle_gamma 90 _cell_volume 1626.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5604 _cell_measurement_theta_min 2.8483 _cell_measurement_theta_max 70.4757 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.647 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.035 _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 0.753 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed x-ray tube' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'APEX-II CCD' _diffrn_orient_matrix_type 'x-axis to radiation source' _diffrn_orient_matrix_ub_11 0.60934E-2 _diffrn_orient_matrix_ub_12 0.720867E-1 _diffrn_orient_matrix_ub_13 -0.188379E-1 _diffrn_orient_matrix_ub_21 0.378169E-1 _diffrn_orient_matrix_ub_22 0.336257E-1 _diffrn_orient_matrix_ub_23 0.609903E-1 _diffrn_orient_matrix_ub_31 0.763203E-1 _diffrn_orient_matrix_ub_32 -0.513865E-2 _diffrn_orient_matrix_ub_33 -0.895358E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method '\f or \w oscillation scans' _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.027 _diffrn_reflns_number 10563 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.2 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 2602 _reflns_number_gt 2395 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 software' _computing_cell_refinement 'SAINT V8.27B integration software' _computing_data_reduction 'SORTAV (Blessing, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0115P)^2^+6.2846P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2602 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.026 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0456 _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 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_diff_density_max 0.848 _refine_diff_density_min -0.631 _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' I I -0.4742 1.8119 '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' 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 C1 C 0.52481(19) 0.3628(11) 0.2481(3) 0.0209(12) Uani 1 1 d . . . C2 C 0.57201(19) 0.5371(13) 0.2498(3) 0.0194(11) Uani 1 1 d . . . H2 H 0.5815 0.6228 0.1994 0.023 Uiso 1 1 calc R . . C3 C 0.6048(2) 0.5811(13) 0.3283(3) 0.0216(11) Uani 1 1 d . . . H3 H 0.6364 0.6972 0.3308 0.026 Uiso 1 1 calc R . . C4 C 0.58985(19) 0.4512(13) 0.4020(3) 0.0197(11) Uani 1 1 d . . . C5 C 0.54221(16) 0.286(2) 0.4001(3) 0.0236(10) Uani 1 1 d . . . H5 H 0.5322 0.2053 0.4507 0.028 Uiso 1 1 calc R . . C6 C 0.50940(17) 0.240(2) 0.3222(3) 0.0247(12) Uani 1 1 d . . . H6 H 0.4774 0.1283 0.3202 0.03 Uiso 1 1 calc R . . C7 C 0.71302(19) 0.5325(12) 0.7668(3) 0.0170(10) Uani 1 1 d . . . C8 C 0.76361(19) 0.6180(12) 0.7488(3) 0.0187(10) Uani 1 1 d . . . H8 H 0.7673 0.7224 0.6975 0.022 Uiso 1 1 calc R . . C9 C 0.8086(2) 0.5463(12) 0.8082(3) 0.0188(11) Uani 1 1 d . . . H9 H 0.8423 0.6029 0.7963 0.023 Uiso 1 1 calc R . . C10 C 0.80314(19) 0.3910(12) 0.8847(3) 0.0174(10) Uani 1 1 d . . . C11 C 0.75258(18) 0.305(2) 0.9026(3) 0.0203(13) Uani 1 1 d . . . H11 H 0.7489 0.2001 0.9538 0.024 Uiso 1 1 calc R . . C12 C 0.7082(2) 0.3769(12) 0.8441(3) 0.0197(11) Uani 1 1 d . . . H12 H 0.6746 0.3208 0.8565 0.024 Uiso 1 1 calc R . . C13 C 0.67514(16) 0.295(2) 0.4938(3) 0.0233(12) Uani 1 1 d . . . C14 C 0.69715(18) 0.3355(11) 0.5838(3) 0.0167(13) Uani 1 1 d . . . H14 H 0.7296 0.2525 0.6097 0.02 Uiso 1 1 calc R . . C16 C 0.61555(19) 0.6030(13) 0.5572(3) 0.0201(11) Uani 1 1 d . . . C17 C 0.62224(15) 0.763(3) 0.7420(2) 0.0216(9) Uani 1 1 d . . . H17A H 0.6162 0.9746 0.7172 0.032 Uiso 1 1 calc R . . H17B H 0.6306 0.7817 0.8034 0.032 Uiso 1 1 calc R . . H17C H 0.5908 0.6329 0.728 0.032 Uiso 1 1 calc R . . I1 I 0.478452(11) 0.26610(10) 0.128465(16) 0.02740(9) Uani 1 1 d . . . I2 I 0.870075(11) 0.27635(13) 0.974289(16) 0.02728(9) Uani 1 1 d . . . N1 N 0.66682(15) 0.6078(10) 0.7076(2) 0.0184(9) Uani 1 1 d . . . N2 N 0.62590(15) 0.4683(10) 0.4816(2) 0.0185(9) Uani 1 1 d . . . O1 O 0.57709(11) 0.7633(18) 0.56768(16) 0.0276(7) Uani 1 1 d . . . O2 O 0.69256(13) 0.1542(10) 0.4368(2) 0.0325(11) Uani 1 1 d . . . C15 C 0.66325(18) 0.5127(13) 0.6243(3) 0.0170(10) Uani 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 C1 0.023(2) 0.025(3) 0.014(2) -0.0037(18) -0.0012(19) 0.004(2) C2 0.021(2) 0.025(3) 0.011(2) 0.002(2) -0.0003(19) -0.001(2) C3 0.019(2) 0.029(3) 0.018(2) 0.003(2) 0.003(2) -0.003(2) C4 0.018(2) 0.027(3) 0.013(2) 0.000(2) -0.0019(19) 0.004(2) C5 0.020(2) 0.036(3) 0.0150(18) 0.004(4) 0.0034(16) -0.009(4) C6 0.017(2) 0.030(3) 0.026(2) 0.007(4) 0.0014(17) 0.002(3) C7 0.020(2) 0.017(2) 0.013(2) -0.0024(19) -0.0003(19) 0.002(2) C8 0.026(3) 0.018(2) 0.012(2) 0.0016(19) 0.0031(19) -0.002(2) C9 0.019(2) 0.021(3) 0.017(2) -0.003(2) 0.0027(19) -0.001(2) C10 0.018(2) 0.019(2) 0.014(2) -0.0005(18) -0.0004(19) -0.0008(19) C11 0.027(2) 0.022(4) 0.0103(17) -0.001(3) -0.0006(16) -0.001(3) C12 0.021(2) 0.022(3) 0.016(2) -0.0025(18) 0.0042(19) -0.0025(19) C13 0.0155(19) 0.036(3) 0.0179(19) -0.001(4) 0.0020(16) -0.008(4) C14 0.017(2) 0.018(4) 0.0142(19) -0.0019(19) 0.0003(17) 0.001(2) C16 0.021(3) 0.025(3) 0.014(2) 0.003(2) 0.001(2) -0.001(2) C17 0.0183(19) 0.029(2) 0.0183(18) -0.006(4) 0.0036(15) 0.003(4) I1 0.03449(17) 0.02402(16) 0.01964(14) -0.0036(3) -0.00995(11) 0.0021(3) I2 0.02736(16) 0.03178(18) 0.02016(14) -0.0006(3) -0.00531(11) 0.0041(3) N1 0.017(2) 0.026(2) 0.0127(19) -0.0009(17) 0.0033(16) 0.0038(18) N2 0.016(2) 0.028(3) 0.0104(19) -0.0014(17) -0.0007(16) 0.0015(19) O1 0.0207(15) 0.043(2) 0.0185(13) 0.000(3) 0.0000(12) 0.012(3) O2 0.0235(18) 0.054(3) 0.0187(17) -0.0107(17) 0.0000(15) 0.0112(18) C15 0.014(2) 0.024(3) 0.013(2) 0.001(2) 0.0019(19) -0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C6 1.376(7) . ? C1 C2 1.394(7) . ? C1 I1 2.108(4) . ? C2 C3 1.396(7) . ? C3 C4 1.377(7) . ? C4 C5 1.385(8) . ? C4 N2 1.440(6) . ? C5 C6 1.391(6) . ? C7 C12 1.394(7) . ? C7 C8 1.399(7) . ? C7 N1 1.422(6) . ? C8 C9 1.398(7) . ? C9 C10 1.386(7) . ? C10 C11 1.398(7) . ? C10 I2 2.099(5) . ? C11 C12 1.380(6) . ? C13 O2 1.202(7) . ? C13 N2 1.429(7) . ? C13 C14 1.454(6) . ? C14 C15 1.355(7) . ? C16 O1 1.209(6) . ? C16 N2 1.370(6) . ? C16 C15 1.532(6) . ? C17 N1 1.468(7) . ? N1 C15 1.357(6) . ? 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 C6 C1 C2 121.4(4) . . ? C6 C1 I1 119.7(4) . . ? C2 C1 I1 118.9(3) . . ? C1 C2 C3 119.0(4) . . ? C4 C3 C2 119.4(5) . . ? C3 C4 C5 121.1(4) . . ? C3 C4 N2 119.5(4) . . ? C5 C4 N2 119.2(4) . . ? C4 C5 C6 119.8(5) . . ? C1 C6 C5 119.2(6) . . ? C12 C7 C8 119.3(4) . . ? C12 C7 N1 120.2(4) . . ? C8 C7 N1 120.5(4) . . ? C9 C8 C7 119.9(4) . . ? C10 C9 C8 120.1(5) . . ? C9 C10 C11 120.0(4) . . ? C9 C10 I2 120.9(4) . . ? C11 C10 I2 119.1(3) . . ? C12 C11 C10 119.8(5) . . ? C11 C12 C7 120.9(5) . . ? O2 C13 N2 123.3(4) . . ? O2 C13 C14 130.5(5) . . ? N2 C13 C14 106.2(5) . . ? C15 C14 C13 109.7(4) . . ? O1 C16 N2 126.7(4) . . ? O1 C16 C15 127.8(4) . . ? N2 C16 C15 105.5(4) . . ? C15 N1 C7 120.2(4) . . ? C15 N1 C17 122.1(4) . . ? C7 N1 C17 117.5(3) . . ? C16 N2 C13 111.0(4) . . ? C16 N2 C4 126.5(4) . . ? C13 N2 C4 121.8(4) . . ? C14 C15 N1 130.5(4) . . ? C14 C15 C16 107.5(4) . . ? N1 C15 C16 122.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.5(8) . . . . ? I1 C1 C2 C3 -175.3(4) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C2 C3 C4 C5 -1.9(9) . . . . ? C2 C3 C4 N2 173.9(5) . . . . ? C3 C4 C5 C6 2.0(11) . . . . ? N2 C4 C5 C6 -173.8(7) . . . . ? C2 C1 C6 C5 -1.4(11) . . . . ? I1 C1 C6 C5 175.4(6) . . . . ? C4 C5 C6 C1 -0.4(13) . . . . ? C12 C7 C8 C9 0.2(7) . . . . ? N1 C7 C8 C9 179.1(4) . . . . ? C7 C8 C9 C10 0.0(7) . . . . ? C8 C9 C10 C11 0.1(8) . . . . ? C8 C9 C10 I2 179.4(4) . . . . ? C9 C10 C11 C12 -0.3(9) . . . . ? I2 C10 C11 C12 -179.6(5) . . . . ? C10 C11 C12 C7 0.4(9) . . . . ? C8 C7 C12 C11 -0.4(8) . . . . ? N1 C7 C12 C11 -179.3(5) . . . . ? O2 C13 C14 C15 -179.8(8) . . . . ? N2 C13 C14 C15 1.6(7) . . . . ? C12 C7 N1 C15 -127.3(5) . . . . ? C8 C7 N1 C15 53.7(7) . . . . ? C12 C7 N1 C17 47.2(7) . . . . ? C8 C7 N1 C17 -131.7(6) . . . . ? O1 C16 N2 C13 -179.9(6) . . . . ? C15 C16 N2 C13 1.1(6) . . . . ? O1 C16 N2 C4 -9.4(9) . . . . ? C15 C16 N2 C4 171.7(4) . . . . ? O2 C13 N2 C16 179.6(7) . . . . ? C14 C13 N2 C16 -1.7(7) . . . . ? O2 C13 N2 C4 8.6(10) . . . . ? C14 C13 N2 C4 -172.8(5) . . . . ? C3 C4 N2 C16 123.7(6) . . . . ? C5 C4 N2 C16 -60.4(8) . . . . ? C3 C4 N2 C13 -66.7(7) . . . . ? C5 C4 N2 C13 109.2(7) . . . . ? C13 C14 C15 N1 179.3(6) . . . . ? C13 C14 C15 C16 -1.0(6) . . . . ? C7 N1 C15 C14 2.9(8) . . . . ? C17 N1 C15 C14 -171.4(6) . . . . ? C7 N1 C15 C16 -176.8(4) . . . . ? C17 N1 C15 C16 8.9(8) . . . . ? O1 C16 C15 C14 -179.0(6) . . . . ? N2 C16 C15 C14 -0.1(5) . . . . ? O1 C16 C15 N1 0.8(9) . . . . ? N2 C16 C15 N1 179.7(4) . . . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 957501' ####################################################################### # # 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_5 _audit_creation_date 2013-03-07T09:28:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H34 N2 O2 Si2' _chemical_formula_sum 'C30 H34 N2 O2 Si2' _chemical_formula_weight 510.77 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.4957(5) _cell_length_b 22.4434(8) _cell_length_c 11.2136(4) _cell_angle_alpha 90 _cell_angle_beta 113.2100(10) _cell_angle_gamma 90 _cell_volume 2890.29(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 1.54186 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.33 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.5115 _exptl_absorpt_correction_T_max 0.7534 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_unetI/netI 0.0329 _diffrn_reflns_number 35203 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 70.85 _diffrn_reflns_theta_full 67.5 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 5446 _reflns_number_gt 4553 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0890P)^2^+2.8058P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0010(2) _refine_ls_number_reflns 5446 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.715 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # 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 0.0181 0.0091 '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 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 C1 C 0.5661(3) -0.14060(15) 0.6891(3) 0.0518(9) Uani 1 1 d . . . H1A H 0.5084 -0.1095 0.6802 0.078 Uiso 1 1 calc R . . H1B H 0.5465 -0.1766 0.7258 0.078 Uiso 1 1 calc R . . H1C H 0.566 -0.1498 0.6036 0.078 Uiso 1 1 calc R . . C2 C 0.7597(2) -0.16378(11) 0.8539(2) 0.0285(6) Uani 1 1 d . . . C3 C 0.8602(2) -0.17865(12) 0.8370(3) 0.0311(6) Uani 1 1 d . . . H3 H 0.8774 -0.1596 0.7709 0.037 Uiso 1 1 calc R . . C4 C 0.9362(2) -0.22099(12) 0.9154(3) 0.0319(6) Uani 1 1 d . . . H4 H 1.0052 -0.2306 0.9032 0.038 Uiso 1 1 calc R . . C5 C 0.9117(3) -0.24969(13) 1.0124(3) 0.0383(2) Uani 1 1 d . . . C6 C 0.8077(2) -0.23621(13) 1.0259(3) 0.0349(6) Uani 1 1 d . . . H6 H 0.7886 -0.2564 1.0894 0.042 Uiso 1 1 calc R . . C7 C 0.7326(2) -0.19376(12) 0.9476(3) 0.0342(6) Uani 1 1 d . . . H7 H 0.6622 -0.1849 0.9575 0.041 Uiso 1 1 calc R . . C8 C 0.9920(3) -0.29354(13) 1.0966(3) 0.0383(2) Uani 1 1 d . . . C9 C 1.0561(3) -0.33080(13) 1.1623(3) 0.0383(2) Uani 1 1 d . . . C10 C 1.0746(4) -0.46218(18) 1.1651(4) 0.0693(11) Uani 1 1 d . . . H10A H 1.1141 -0.4974 1.2147 0.104 Uiso 1 1 calc R . . H10B H 1.0781 -0.463 1.0793 0.104 Uiso 1 1 calc R . . H10C H 0.9931 -0.4622 1.155 0.104 Uiso 1 1 calc R . . C11 C 1.1559(3) -0.39429(17) 1.4200(3) 0.0549(9) Uani 1 1 d . . . H11A H 1.1922 -0.3573 1.4637 0.082 Uiso 1 1 calc R . . H11B H 1.2026 -0.4284 1.4668 0.082 Uiso 1 1 calc R . . H11C H 1.0772 -0.3975 1.4187 0.082 Uiso 1 1 calc R . . C12 C 1.2958(3) -0.38691(16) 1.2542(3) 0.0482(8) Uani 1 1 d . . . H12A H 1.3249 -0.3463 1.2796 0.072 Uiso 1 1 calc R . . H12B H 1.2931 -0.3954 1.1673 0.072 Uiso 1 1 calc R . . H12C H 1.3479 -0.4154 1.3163 0.072 Uiso 1 1 calc R . . C13 C 0.9646(3) 0.12269(14) 0.7737(3) 0.0436(8) Uani 1 1 d . . . H13A H 0.972 0.1328 0.8616 0.065 Uiso 1 1 calc R . . H13B H 0.9851 0.1575 0.7341 0.065 Uiso 1 1 calc R . . H13C H 1.0173 0.0897 0.7778 0.065 Uiso 1 1 calc R . . C14 C 0.7667(2) 0.15277(11) 0.6361(2) 0.0296(6) Uani 1 1 d . . . C15 C 0.6771(2) 0.16757(12) 0.6744(3) 0.0327(6) Uani 1 1 d . . . H15 H 0.6666 0.1455 0.7413 0.039 Uiso 1 1 calc R . . C16 C 0.6030(2) 0.21445(12) 0.6153(3) 0.0345(6) Uani 1 1 d . . . H16 H 0.5415 0.2243 0.6413 0.041 Uiso 1 1 calc R . . C17 C 0.6186(3) 0.24750(14) 0.5170(3) 0.0405(2) Uani 1 1 d . . . C18 C 0.7111(2) 0.23351(12) 0.4827(3) 0.0339(6) Uani 1 1 d . . . H18 H 0.724 0.2564 0.4183 0.041 Uiso 1 1 calc R . . C19 C 0.7846(2) 0.18651(12) 0.5415(3) 0.0326(6) Uani 1 1 d . . . H19 H 0.8474 0.1772 0.5172 0.039 Uiso 1 1 calc R . . C20 C 0.5399(3) 0.29620(13) 0.4510(3) 0.0405(2) Uani 1 1 d . . . C21 C 0.4790(3) 0.33573(13) 0.3962(3) 0.0405(2) Uani 1 1 d . . . C22 C 0.2528(4) 0.3744(2) 0.1856(5) 0.0903(17) Uani 1 1 d . . . H22A H 0.2711 0.3497 0.124 0.135 Uiso 1 1 calc R . . H22B H 0.2056 0.4085 0.1398 0.135 Uiso 1 1 calc R . . H22C H 0.2091 0.3506 0.2246 0.135 Uiso 1 1 calc R . . C23 C 0.3593(4) 0.44528(16) 0.4371(4) 0.0584(10) Uani 1 1 d . . . H23A H 0.3268 0.484 0.4002 0.088 Uiso 1 1 calc R . . H23B H 0.4319 0.4513 0.5133 0.088 Uiso 1 1 calc R . . H23C H 0.3034 0.4239 0.4626 0.088 Uiso 1 1 calc R . . C24 C 0.4748(4) 0.44541(17) 0.2447(4) 0.0602(10) Uani 1 1 d . . . H24A H 0.4885 0.4218 0.1785 0.09 Uiso 1 1 calc R . . H24B H 0.5497 0.4563 0.3135 0.09 Uiso 1 1 calc R . . H24C H 0.4318 0.4816 0.205 0.09 Uiso 1 1 calc R . . C25 C 0.8258(2) -0.03866(12) 0.8525(2) 0.0279(6) Uani 1 1 d . . . C26 C 0.7186(2) -0.06544(12) 0.7496(2) 0.0276(5) Uani 1 1 d . . . C27 C 0.6581(2) -0.03206(12) 0.6432(3) 0.0314(6) Uani 1 1 d . . . H27 H 0.5873 -0.0476 0.5813 0.038 Uiso 1 1 calc R . . C28 C 0.6962(2) 0.02576(12) 0.6199(2) 0.0294(6) Uani 1 1 d . . . C29 C 0.8071(2) 0.05099(11) 0.7210(2) 0.0279(6) Uani 1 1 d . . . C30 C 0.8689(2) 0.01719(12) 0.8253(2) 0.0306(6) Uani 1 1 d . . . H30 H 0.9434 0.0307 0.8829 0.037 Uiso 1 1 calc R . . N1 N 0.68171(18) -0.11963(10) 0.7750(2) 0.0312(5) Uani 1 1 d . . . N2 N 0.84511(19) 0.10504(9) 0.6958(2) 0.0304(5) Uani 1 1 d . . . O1 O 0.86987(16) -0.06174(9) 0.96059(17) 0.0366(5) Uani 1 1 d . . . O2 O 0.64475(17) 0.05259(9) 0.51747(18) 0.0398(5) Uani 1 1 d . . . Si1 Si 0.38947(7) 0.40123(4) 0.31435(8) 0.0405(2) Uani 1 1 d . . . Si2 Si 1.14774(7) -0.39373(4) 1.25288(8) 0.0383(2) Uani 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 C1 0.0335(16) 0.0406(18) 0.060(2) 0.0124(15) -0.0037(15) -0.0117(13) C2 0.0269(13) 0.0240(13) 0.0304(13) -0.0009(10) 0.0066(10) -0.0002(10) C3 0.0334(14) 0.0271(13) 0.0325(13) 0.0032(10) 0.0125(11) 0.0000(11) C4 0.0312(13) 0.0303(14) 0.0361(14) 0.0041(11) 0.0153(11) 0.0041(11) C5 0.0385(4) 0.0353(4) 0.0416(4) 0.0083(3) 0.0163(3) 0.0079(3) C6 0.0359(15) 0.0330(15) 0.0378(15) 0.0080(12) 0.0167(12) 0.0038(12) C7 0.0306(14) 0.0320(14) 0.0401(15) 0.0017(11) 0.0140(12) 0.0010(11) C8 0.0385(4) 0.0353(4) 0.0416(4) 0.0083(3) 0.0163(3) 0.0079(3) C9 0.0385(4) 0.0353(4) 0.0416(4) 0.0083(3) 0.0163(3) 0.0079(3) C10 0.068(3) 0.046(2) 0.084(3) -0.001(2) 0.020(2) -0.0017(19) C11 0.054(2) 0.062(2) 0.053(2) 0.0199(17) 0.0259(17) 0.0162(17) C12 0.0399(17) 0.056(2) 0.0483(18) 0.0117(15) 0.0163(14) 0.0126(15) C13 0.0323(15) 0.0347(16) 0.0489(17) 0.0076(13) 0.0000(13) -0.0081(12) C14 0.0310(13) 0.0245(13) 0.0280(13) 0.0001(10) 0.0059(11) -0.0018(10) C15 0.0381(15) 0.0285(14) 0.0315(13) 0.0011(11) 0.0136(12) -0.0042(11) C16 0.0361(15) 0.0307(14) 0.0380(15) -0.0019(11) 0.0159(12) 0.0013(11) C17 0.0404(4) 0.0334(4) 0.0464(5) 0.0049(3) 0.0157(3) 0.0070(3) C18 0.0393(15) 0.0273(14) 0.0342(14) 0.0048(11) 0.0135(12) 0.0008(11) C19 0.0326(14) 0.0310(14) 0.0342(14) 0.0029(11) 0.0131(11) 0.0015(11) C20 0.0404(4) 0.0334(4) 0.0464(5) 0.0049(3) 0.0157(3) 0.0070(3) C21 0.0404(4) 0.0334(4) 0.0464(5) 0.0049(3) 0.0157(3) 0.0070(3) C22 0.062(3) 0.069(3) 0.100(4) -0.020(3) -0.012(2) 0.016(2) C23 0.072(2) 0.0397(19) 0.080(3) 0.0090(17) 0.048(2) 0.0129(17) C24 0.073(3) 0.055(2) 0.066(2) 0.0196(18) 0.041(2) 0.0180(19) C25 0.0228(12) 0.0267(13) 0.0285(13) 0.0002(10) 0.0040(10) 0.0015(10) C26 0.0236(12) 0.0259(13) 0.0299(13) -0.0018(10) 0.0070(10) -0.0008(10) C27 0.0255(13) 0.0287(14) 0.0307(13) 0.0025(10) 0.0012(11) -0.0006(10) C28 0.0257(13) 0.0268(13) 0.0287(13) 0.0009(10) 0.0033(10) 0.0008(10) C29 0.0248(12) 0.0249(13) 0.0308(13) -0.0005(10) 0.0076(10) -0.0004(10) C30 0.0251(13) 0.0295(14) 0.0292(13) -0.0002(10) 0.0021(10) -0.0034(10) N1 0.0234(11) 0.0266(11) 0.0351(12) 0.0045(9) 0.0024(9) -0.0022(9) N2 0.0267(11) 0.0245(11) 0.0341(12) 0.0029(9) 0.0054(9) -0.0027(9) O1 0.0354(10) 0.0327(10) 0.0307(10) 0.0058(8) 0.0011(8) -0.0020(8) O2 0.0401(11) 0.0330(11) 0.0318(10) 0.0069(8) -0.0012(9) -0.0022(9) Si1 0.0404(4) 0.0334(4) 0.0464(5) 0.0049(3) 0.0157(3) 0.0070(3) Si2 0.0385(4) 0.0353(4) 0.0416(4) 0.0083(3) 0.0163(3) 0.0079(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.463(3) . ? C2 C3 1.383(4) . ? C2 C7 1.397(4) . ? C2 N1 1.426(3) . ? C3 C4 1.385(4) . ? C4 C5 1.397(4) . ? C5 C6 1.399(4) . ? C5 C8 1.456(4) . ? C6 C7 1.382(4) . ? C8 C9 1.191(4) . ? C9 Si2 1.849(3) . ? C10 Si2 1.859(4) . ? C11 Si2 1.837(4) . ? C12 Si2 1.851(3) . ? C13 N2 1.457(3) . ? C14 C15 1.389(4) . ? C14 C19 1.391(4) . ? C14 N2 1.428(3) . ? C15 C16 1.386(4) . ? C16 C17 1.404(4) . ? C17 C18 1.390(4) . ? C17 C20 1.461(4) . ? C18 C19 1.383(4) . ? C20 C21 1.173(4) . ? C21 Si1 1.856(3) . ? C22 Si1 1.850(4) . ? C23 Si1 1.850(4) . ? C24 Si1 1.841(4) . ? C25 O1 1.230(3) . ? C25 C30 1.443(4) . ? C25 C26 1.507(3) . ? C26 C27 1.358(4) . ? C26 N1 1.370(3) . ? C27 C28 1.441(4) . ? C28 O2 1.230(3) . ? C28 C29 1.513(3) . ? C29 C30 1.352(4) . ? C29 N2 1.372(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C7 119.3(2) . . ? C3 C2 N1 121.2(2) . . ? C7 C2 N1 119.5(2) . . ? C2 C3 C4 120.7(3) . . ? C3 C4 C5 120.3(3) . . ? C4 C5 C6 118.8(3) . . ? C4 C5 C8 120.7(3) . . ? C6 C5 C8 120.5(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C2 120.3(3) . . ? C9 C8 C5 177.8(3) . . ? C8 C9 Si2 174.7(3) . . ? C15 C14 C19 119.8(2) . . ? C15 C14 N2 121.4(2) . . ? C19 C14 N2 118.7(2) . . ? C16 C15 C14 120.1(3) . . ? C15 C16 C17 120.2(3) . . ? C18 C17 C16 119.0(3) . . ? C18 C17 C20 119.7(3) . . ? C16 C17 C20 121.2(3) . . ? C19 C18 C17 120.5(3) . . ? C18 C19 C14 120.2(3) . . ? C21 C20 C17 178.0(4) . . ? C20 C21 Si1 176.8(3) . . ? O1 C25 C30 121.0(2) . . ? O1 C25 C26 120.3(2) . . ? C30 C25 C26 118.5(2) . . ? C27 C26 N1 123.8(2) . . ? C27 C26 C25 118.2(2) . . ? N1 C26 C25 117.7(2) . . ? C26 C27 C28 123.2(2) . . ? O2 C28 C27 121.5(2) . . ? O2 C28 C29 120.3(2) . . ? C27 C28 C29 118.1(2) . . ? C30 C29 N2 123.3(2) . . ? C30 C29 C28 118.7(2) . . ? N2 C29 C28 117.8(2) . . ? C29 C30 C25 122.5(2) . . ? C26 N1 C2 122.8(2) . . ? C26 N1 C1 118.3(2) . . ? C2 N1 C1 116.2(2) . . ? C29 N2 C14 122.1(2) . . ? C29 N2 C13 118.2(2) . . ? C14 N2 C13 115.4(2) . . ? C24 Si1 C23 110.47(18) . . ? C24 Si1 C22 110.8(2) . . ? C23 Si1 C22 111.0(2) . . ? C24 Si1 C21 107.43(16) . . ? C23 Si1 C21 108.36(16) . . ? C22 Si1 C21 108.60(18) . . ? C11 Si2 C9 109.80(15) . . ? C11 Si2 C12 109.84(17) . . ? C9 Si2 C12 110.00(15) . . ? C11 Si2 C10 110.7(2) . . ? C9 Si2 C10 105.76(17) . . ? C12 Si2 C10 110.70(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C2 C3 C4 -2.7(4) . . . . ? N1 C2 C3 C4 179.1(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 1.9(4) . . . . ? C3 C4 C5 C8 -179.0(3) . . . . ? C4 C5 C6 C7 -2.2(4) . . . . ? C8 C5 C6 C7 178.8(3) . . . . ? C5 C6 C7 C2 0.0(4) . . . . ? C3 C2 C7 C6 2.5(4) . . . . ? N1 C2 C7 C6 -179.3(2) . . . . ? C4 C5 C8 C9 -83(9) . . . . ? C6 C5 C8 C9 96(9) . . . . ? C5 C8 C9 Si2 -7(11) . . . . ? C19 C14 C15 C16 2.4(4) . . . . ? N2 C14 C15 C16 179.5(2) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C18 -1.7(4) . . . . ? C15 C16 C17 C20 178.5(3) . . . . ? C16 C17 C18 C19 2.0(4) . . . . ? C20 C17 C18 C19 -178.2(3) . . . . ? C17 C18 C19 C14 -0.2(4) . . . . ? C15 C14 C19 C18 -2.1(4) . . . . ? N2 C14 C19 C18 -179.3(2) . . . . ? C18 C17 C20 C21 -8(10) . . . . ? C16 C17 C20 C21 17E1(10) . . . . ? C17 C20 C21 Si1 -62(13) . . . . ? O1 C25 C26 C27 165.5(3) . . . . ? C30 C25 C26 C27 -8.9(4) . . . . ? O1 C25 C26 N1 -8.1(4) . . . . ? C30 C25 C26 N1 177.4(2) . . . . ? N1 C26 C27 C28 177.9(3) . . . . ? C25 C26 C27 C28 4.7(4) . . . . ? C26 C27 C28 O2 173.7(3) . . . . ? C26 C27 C28 C29 -1.8(4) . . . . ? O2 C28 C29 C30 -172.2(3) . . . . ? C27 C28 C29 C30 3.4(4) . . . . ? O2 C28 C29 N2 2.1(4) . . . . ? C27 C28 C29 N2 177.6(2) . . . . ? N2 C29 C30 C25 177.9(3) . . . . ? C28 C29 C30 C25 -8.2(4) . . . . ? O1 C25 C30 C29 -163.4(3) . . . . ? C26 C25 C30 C29 11.0(4) . . . . ? C27 C26 N1 C2 155.2(3) . . . . ? C25 C26 N1 C2 -31.5(4) . . . . ? C27 C26 N1 C1 -5.5(4) . . . . ? C25 C26 N1 C1 167.8(3) . . . . ? C3 C2 N1 C26 -46.6(4) . . . . ? C7 C2 N1 C26 135.1(3) . . . . ? C3 C2 N1 C1 114.5(3) . . . . ? C7 C2 N1 C1 -63.8(4) . . . . ? C30 C29 N2 C14 -146.1(3) . . . . ? C28 C29 N2 C14 39.9(4) . . . . ? C30 C29 N2 C13 9.6(4) . . . . ? C28 C29 N2 C13 -164.4(3) . . . . ? C15 C14 N2 C29 44.5(4) . . . . ? C19 C14 N2 C29 -138.4(3) . . . . ? C15 C14 N2 C13 -111.9(3) . . . . ? C19 C14 N2 C13 65.3(3) . . . . ? C20 C21 Si1 C24 50(5) . . . . ? C20 C21 Si1 C23 -69(5) . . . . ? C20 C21 Si1 C22 170(5) . . . . ? C8 C9 Si2 C11 -127(3) . . . . ? C8 C9 Si2 C12 112(3) . . . . ? C8 C9 Si2 C10 -8(3) . . . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 957502'