# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Lewis, Andrew' 'Nakamaru-Ogiso, Eiko' 'Kikkawa, James M' 'Carroll, Patrick' 'Schelter, Eric J' _publ_contact_author_name 'Mr Andrew Lewis, ' _publ_contact_author_email schelter@sas.upenn.edu _publ_section_title ; Pentavalent Uranium Trans-Dihalides and -Pseudohalides ; # Attachment '- U(V)X2.cif' data_UP4100(Cmpd1) _database_code_depnum_ccdc_archive 'CCDC 870190' #TrackingRef '- U(V)X2.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 F2 N3 Si6 U' _chemical_formula_weight 757.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.7891(7) _cell_length_b 12.4396(8) _cell_length_c 22.9328(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3363.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 5.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.4061 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 82945 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.63 _reflns_number_total 7771 _reflns_number_gt 7570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0169P)^2^+2.1650P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.366(3) _refine_ls_number_reflns 7771 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0188 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0427 _refine_ls_wR_factor_gt 0.0422 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.716746(8) 0.556258(8) 0.622738(4) 0.02451(3) Uani 1 1 d . . . Si1 Si 0.62061(10) 0.48294(8) 0.48791(4) 0.0387(2) Uani 1 1 d . . . Si2 Si 0.65630(8) 0.30084(6) 0.57342(4) 0.03037(18) Uani 1 1 d . . . Si3 Si 0.67943(8) 0.82803(7) 0.63963(4) 0.0375(2) Uani 1 1 d . . . Si4 Si 0.46961(8) 0.68776(8) 0.65375(5) 0.0409(2) Uani 1 1 d . . . Si5 Si 1.00129(6) 0.50116(6) 0.62807(4) 0.03123(17) Uani 1 1 d . . . Si6 Si 0.88147(8) 0.53401(6) 0.74439(4) 0.03163(19) Uani 1 1 d . . . F1 F 0.63529(17) 0.47110(14) 0.68717(8) 0.0384(5) Uani 1 1 d . . . F2 F 0.80327(17) 0.64185(15) 0.55907(8) 0.0381(4) Uani 1 1 d . . . N1 N 0.6602(2) 0.4391(2) 0.55765(10) 0.0278(5) Uani 1 1 d . . . N2 N 0.6162(2) 0.70059(19) 0.64029(11) 0.0297(5) Uani 1 1 d . . . N3 N 0.8776(2) 0.52823(17) 0.66776(11) 0.0256(5) Uani 1 1 d . . . C1 C 0.4887(4) 0.4142(4) 0.46165(19) 0.0629(13) Uani 1 1 d . . . H1a H 0.5029 0.3386 0.4575 0.094 Uiso 1 1 calc R . . H1b H 0.4668 0.4437 0.4246 0.094 Uiso 1 1 calc R . . H1c H 0.4287 0.4252 0.4894 0.094 Uiso 1 1 calc R . . C2 C 0.5849(5) 0.6293(3) 0.48750(18) 0.0619(13) Uani 1 1 d . . . H2a H 0.5232 0.6424 0.5139 0.093 Uiso 1 1 calc R . . H2b H 0.5633 0.6506 0.4488 0.093 Uiso 1 1 calc R . . H2c H 0.6500 0.6700 0.4996 0.093 Uiso 1 1 calc R . . C3 C 0.7364(4) 0.4620(3) 0.43424(15) 0.0599(12) Uani 1 1 d . . . H3a H 0.8049 0.4944 0.4485 0.090 Uiso 1 1 calc R . . H3b H 0.7158 0.4943 0.3977 0.090 Uiso 1 1 calc R . . H3c H 0.7484 0.3863 0.4287 0.090 Uiso 1 1 calc R . . C4 C 0.5122(3) 0.2564(3) 0.59509(19) 0.0513(10) Uani 1 1 d . . . H4a H 0.4885 0.2954 0.6291 0.077 Uiso 1 1 calc R . . H4b H 0.5134 0.1809 0.6037 0.077 Uiso 1 1 calc R . . H4c H 0.4601 0.2698 0.5638 0.077 Uiso 1 1 calc R . . C5 C 0.7558(3) 0.2662(2) 0.63431(14) 0.0375(7) Uani 1 1 d . . . H5a H 0.8315 0.2871 0.6238 0.056 Uiso 1 1 calc R . . H5b H 0.7536 0.1901 0.6413 0.056 Uiso 1 1 calc R . . H5c H 0.7333 0.3037 0.6690 0.056 Uiso 1 1 calc R . . C6 C 0.7063(4) 0.2206(3) 0.50945(15) 0.0460(9) Uani 1 1 d . . . H6a H 0.6578 0.2342 0.4766 0.069 Uiso 1 1 calc R . . H6b H 0.7041 0.1455 0.5189 0.069 Uiso 1 1 calc R . . H6c H 0.7826 0.2410 0.4999 0.069 Uiso 1 1 calc R . . C7 C 0.6257(5) 0.9146(3) 0.7000(3) 0.0796(17) Uani 1 1 d . . . H7a H 0.5451 0.9234 0.6961 0.119 Uiso 1 1 calc R . . H7b H 0.6619 0.9837 0.6982 0.119 Uiso 1 1 calc R . . H7c H 0.6424 0.8813 0.7368 0.119 Uiso 1 1 calc R . . C8 C 0.6604(5) 0.8964(4) 0.5681(2) 0.0728(15) Uani 1 1 d . . . H8a H 0.6878 0.8506 0.5374 0.109 Uiso 1 1 calc R . . H8b H 0.7023 0.9626 0.5679 0.109 Uiso 1 1 calc R . . H8c H 0.5814 0.9112 0.5619 0.109 Uiso 1 1 calc R . . C9 C 0.8354(3) 0.8187(3) 0.65196(19) 0.0490(9) Uani 1 1 d . . . H9a H 0.8496 0.7834 0.6885 0.074 Uiso 1 1 calc R . . H9b H 0.8674 0.8896 0.6528 0.074 Uiso 1 1 calc R . . H9c H 0.8695 0.7782 0.6209 0.074 Uiso 1 1 calc R . . C10 C 0.4176(3) 0.5534(3) 0.6289(2) 0.0573(10) Uani 1 1 d . . . H10a H 0.4245 0.5483 0.5873 0.086 Uiso 1 1 calc R . . H10b H 0.3394 0.5449 0.6397 0.086 Uiso 1 1 calc R . . H10c H 0.4620 0.4978 0.6468 0.086 Uiso 1 1 calc R . . C11 C 0.4360(4) 0.6979(4) 0.7325(2) 0.0668(13) Uani 1 1 d . . . H11a H 0.4812 0.6472 0.7538 0.100 Uiso 1 1 calc R . . H11b H 0.3571 0.6825 0.7385 0.100 Uiso 1 1 calc R . . H11Cc H 0.4523 0.7693 0.7460 0.100 Uiso 1 1 calc R . . C12 C 0.3867(3) 0.7912(3) 0.6122(2) 0.0637(13) Uani 1 1 d . . . H12a H 0.4088 0.8618 0.6247 0.096 Uiso 1 1 calc R . . H12b H 0.3072 0.7812 0.6193 0.096 Uiso 1 1 calc R . . H12c H 0.4017 0.7836 0.5712 0.096 Uiso 1 1 calc R . . C13 C 1.0899(3) 0.6240(3) 0.6197(2) 0.0551(10) Uani 1 1 d . . . H13a H 1.0456 0.6800 0.6021 0.083 Uiso 1 1 calc R . . H13b H 1.1541 0.6082 0.5954 0.083 Uiso 1 1 calc R . . H13c H 1.1158 0.6472 0.6574 0.083 Uiso 1 1 calc R . . C14 C 1.0882(3) 0.3915(3) 0.66144(19) 0.0487(9) Uani 1 1 d . . . H14a H 1.1145 0.4139 0.6991 0.073 Uiso 1 1 calc R . . H14b H 1.1521 0.3763 0.6368 0.073 Uiso 1 1 calc R . . H14c H 1.0426 0.3280 0.6655 0.073 Uiso 1 1 calc R . . C15 C 0.9656(3) 0.4526(4) 0.55287(15) 0.0504(9) Uani 1 1 d . . . H15a H 0.9140 0.3931 0.5555 0.076 Uiso 1 1 calc R . . H15b H 1.0337 0.4300 0.5335 0.076 Uiso 1 1 calc R . . H15c H 0.9309 0.5098 0.5312 0.076 Uiso 1 1 calc R . . C16 C 0.7634(4) 0.6200(3) 0.77230(14) 0.0524(11) Uani 1 1 d . . . H16a H 0.7614 0.6862 0.7508 0.079 Uiso 1 1 calc R . . H16b H 0.7756 0.6352 0.8129 0.079 Uiso 1 1 calc R . . H16c H 0.6927 0.5829 0.7676 0.079 Uiso 1 1 calc R . . C17 C 1.0166(4) 0.5956(3) 0.77108(18) 0.0535(11) Uani 1 1 d . . . H17a H 1.0798 0.5534 0.7579 0.080 Uiso 1 1 calc R . . H17b H 1.0162 0.5976 0.8129 0.080 Uiso 1 1 calc R . . H17c H 1.0232 0.6674 0.7561 0.080 Uiso 1 1 calc R . . C18 C 0.8673(4) 0.3972(3) 0.77679(14) 0.0407(8) Uani 1 1 d . . . H18a H 0.7931 0.3693 0.7685 0.061 Uiso 1 1 calc R . . H18b H 0.8778 0.4014 0.8182 0.061 Uiso 1 1 calc R . . H18c H 0.9236 0.3505 0.7603 0.061 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 U1 0.02528(5) 0.02171(4) 0.02654(5) -0.00065(4) -0.00298(4) 0.00269(4) Si1 0.0565(6) 0.0319(4) 0.0278(5) 0.0060(4) -0.0130(4) -0.0063(4) Si2 0.0364(5) 0.0230(4) 0.0317(4) 0.0029(3) -0.0070(4) -0.0056(3) Si3 0.0438(5) 0.0217(4) 0.0471(5) 0.0024(4) -0.0021(4) 0.0030(3) Si4 0.0319(5) 0.0334(5) 0.0573(6) 0.0063(4) 0.0098(4) 0.0109(4) Si5 0.0237(4) 0.0304(4) 0.0396(5) 0.0097(4) 0.0001(4) 0.0016(3) Si6 0.0463(5) 0.0240(4) 0.0246(4) 0.0025(3) -0.0087(3) 0.0028(3) F1 0.0391(11) 0.0348(10) 0.0412(10) 0.0043(8) 0.0046(8) 0.0021(8) F2 0.0432(12) 0.0364(10) 0.0346(10) 0.0073(8) 0.0021(8) -0.0035(8) N1 0.0324(13) 0.0249(11) 0.0261(11) 0.0063(11) -0.0035(10) -0.0013(12) N2 0.0306(13) 0.0254(11) 0.0331(14) 0.0036(10) 0.0054(10) 0.0030(10) N3 0.0277(13) 0.0179(11) 0.0312(13) 0.0042(9) -0.0017(10) 0.0008(8) C1 0.071(3) 0.065(3) 0.053(2) 0.012(2) -0.035(2) -0.013(2) C2 0.105(4) 0.037(2) 0.044(2) 0.0110(17) -0.022(2) 0.007(2) C3 0.095(3) 0.060(3) 0.0249(16) 0.0072(16) -0.0016(18) -0.010(2) C4 0.042(2) 0.047(2) 0.065(3) 0.0185(19) -0.0069(18) -0.0109(17) C5 0.0461(19) 0.0276(14) 0.0389(18) 0.0075(13) -0.0091(14) -0.0009(12) C6 0.069(3) 0.0279(15) 0.0413(18) -0.0069(13) -0.0047(19) -0.0028(17) C7 0.077(3) 0.042(2) 0.120(5) -0.035(3) 0.020(3) 0.001(2) C8 0.086(4) 0.050(2) 0.083(3) 0.037(2) -0.028(3) -0.020(2) C9 0.045(2) 0.0368(18) 0.066(2) 0.0000(17) -0.0111(18) -0.0080(16) C10 0.0312(16) 0.0488(19) 0.092(3) -0.005(3) 0.003(2) -0.0014(16) C11 0.068(3) 0.060(3) 0.073(3) 0.004(2) 0.034(2) 0.008(2) C12 0.038(2) 0.051(2) 0.102(4) 0.019(2) -0.003(2) 0.0178(17) C13 0.0311(17) 0.0451(19) 0.089(3) 0.019(2) 0.006(2) -0.0048(14) C14 0.038(2) 0.044(2) 0.064(3) 0.0104(18) 0.0015(18) 0.0146(16) C15 0.045(2) 0.070(3) 0.0369(18) -0.005(2) 0.0138(15) 0.008(2) C16 0.082(3) 0.050(2) 0.0254(16) -0.0021(14) -0.0009(18) 0.026(2) C17 0.076(3) 0.0369(18) 0.048(2) 0.0020(16) -0.027(2) -0.0143(19) C18 0.064(2) 0.0306(16) 0.0278(16) 0.0073(13) 0.0000(16) -0.0031(16) 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 U1 F1 2.0562(19) . ? U1 F2 2.0751(18) . ? U1 N2 2.189(2) . ? U1 N3 2.187(2) . ? U1 N1 2.190(3) . ? U1 Si6 3.4104(9) . ? U1 Si4 3.4162(9) . ? U1 Si1 3.4171(10) . ? U1 Si5 3.4260(8) . ? U1 Si3 3.4312(9) . ? U1 Si2 3.4470(8) . ? Si1 N1 1.753(2) . ? Si1 C3 1.856(5) . ? Si1 C2 1.868(4) . ? Si1 C1 1.874(4) . ? Si2 N1 1.758(3) . ? Si2 C4 1.854(4) . ? Si2 C6 1.869(3) . ? Si2 C5 1.874(3) . ? Si3 N2 1.752(3) . ? Si3 C8 1.862(4) . ? Si3 C9 1.864(4) . ? Si3 C7 1.865(4) . ? Si4 N2 1.762(3) . ? Si4 C11 1.853(5) . ? Si4 C10 1.870(4) . ? Si4 C12 1.877(4) . ? Si5 N3 1.751(3) . ? Si5 C13 1.861(4) . ? Si5 C14 1.870(4) . ? Si5 C15 1.875(4) . ? Si6 N3 1.759(3) . ? Si6 C18 1.865(3) . ? Si6 C16 1.868(4) . ? Si6 C17 1.871(4) . ? 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 F1 U1 F2 178.35(8) . . ? F1 U1 N2 92.15(8) . . ? F2 U1 N2 88.56(8) . . ? F1 U1 N3 89.06(8) . . ? F2 U1 N3 89.29(8) . . ? N2 U1 N3 120.90(9) . . ? F1 U1 N1 90.28(8) . . ? F2 U1 N1 90.66(8) . . ? N2 U1 N1 120.41(10) . . ? N3 U1 N1 118.67(9) . . ? F1 U1 Si6 68.67(6) . . ? F2 U1 Si6 109.71(6) . . ? N2 U1 Si6 102.98(7) . . ? N3 U1 Si6 26.77(7) . . ? N1 U1 Si6 132.61(7) . . ? F1 U1 Si4 72.47(5) . . ? F2 U1 Si4 108.67(6) . . ? N2 U1 Si4 26.74(7) . . ? N3 U1 Si4 135.85(7) . . ? N1 U1 Si4 101.59(7) . . ? Si6 U1 Si4 110.74(3) . . ? F1 U1 Si1 110.97(6) . . ? F2 U1 Si1 70.32(6) . . ? N2 U1 Si1 101.87(7) . . ? N3 U1 Si1 132.23(7) . . ? N1 U1 Si1 26.45(7) . . ? Si6 U1 Si1 155.15(2) . . ? Si4 U1 Si1 91.91(3) . . ? F1 U1 Si5 109.18(6) . . ? F2 U1 Si5 69.29(6) . . ? N2 U1 Si5 133.46(7) . . ? N3 U1 Si5 26.14(7) . . ? N1 U1 Si5 100.92(7) . . ? Si6 U1 Si5 52.92(2) . . ? Si4 U1 Si5 157.43(2) . . ? Si1 U1 Si5 107.68(3) . . ? F1 U1 Si3 111.51(5) . . ? F2 U1 Si3 68.71(5) . . ? N2 U1 Si3 26.06(7) . . ? N3 U1 Si3 102.41(6) . . ? N1 U1 Si3 133.91(7) . . ? Si6 U1 Si3 93.47(2) . . ? Si4 U1 Si3 52.80(2) . . ? Si1 U1 Si3 108.82(2) . . ? Si5 U1 Si3 108.58(2) . . ? F1 U1 Si2 70.39(5) . . ? F2 U1 Si2 110.10(5) . . ? N2 U1 Si2 134.78(7) . . ? N3 U1 Si2 100.79(6) . . ? N1 U1 Si2 25.86(6) . . ? Si6 U1 Si2 108.14(2) . . ? Si4 U1 Si2 109.47(2) . . ? Si1 U1 Si2 52.31(2) . . ? Si5 U1 Si2 91.70(2) . . ? Si3 U1 Si2 156.74(2) . . ? N1 Si1 C3 111.44(16) . . ? N1 Si1 C2 111.56(17) . . ? C3 Si1 C2 107.4(2) . . ? N1 Si1 C1 111.85(17) . . ? C3 Si1 C1 109.5(2) . . ? C2 Si1 C1 104.8(2) . . ? N1 Si1 U1 33.81(9) . . ? C3 Si1 U1 113.18(14) . . ? C2 Si1 U1 79.58(13) . . ? C1 Si1 U1 133.44(16) . . ? N1 Si2 C4 111.76(16) . . ? N1 Si2 C6 110.64(14) . . ? C4 Si2 C6 109.9(2) . . ? N1 Si2 C5 111.22(13) . . ? C4 Si2 C5 107.77(16) . . ? C6 Si2 C5 105.36(17) . . ? N1 Si2 U1 32.90(8) . . ? C4 Si2 U1 112.11(14) . . ? C6 Si2 U1 133.18(12) . . ? C5 Si2 U1 80.68(10) . . ? N2 Si3 C8 111.68(18) . . ? N2 Si3 C9 111.24(15) . . ? C8 Si3 C9 106.3(2) . . ? N2 Si3 C7 111.80(19) . . ? C8 Si3 C7 110.5(3) . . ? C9 Si3 C7 105.0(2) . . ? N2 Si3 U1 33.28(8) . . ? C8 Si3 U1 111.45(17) . . ? C9 Si3 U1 80.17(12) . . ? C7 Si3 U1 134.14(17) . . ? N2 Si4 C11 112.0(2) . . ? N2 Si4 C10 110.43(15) . . ? C11 Si4 C10 106.7(2) . . ? N2 Si4 C12 111.07(16) . . ? C11 Si4 C12 109.7(2) . . ? C10 Si4 C12 106.7(2) . . ? N2 Si4 U1 33.98(8) . . ? C11 Si4 U1 114.70(16) . . ? C10 Si4 U1 77.77(11) . . ? C12 Si4 U1 131.82(16) . . ? N3 Si5 C13 111.27(16) . . ? N3 Si5 C14 112.56(15) . . ? C13 Si5 C14 109.48(18) . . ? N3 Si5 C15 110.68(14) . . ? C13 Si5 C15 107.2(2) . . ? C14 Si5 C15 105.3(2) . . ? N3 Si5 U1 33.39(8) . . ? C13 Si5 U1 112.44(12) . . ? C14 Si5 U1 134.19(13) . . ? C15 Si5 U1 79.16(12) . . ? N3 Si6 C18 111.00(13) . . ? N3 Si6 C16 110.27(14) . . ? C18 Si6 C16 108.63(19) . . ? N3 Si6 C17 111.44(17) . . ? C18 Si6 C17 108.67(17) . . ? C16 Si6 C17 106.7(2) . . ? N3 Si6 U1 34.06(8) . . ? C18 Si6 U1 110.41(12) . . ? C16 Si6 U1 79.03(11) . . ? C17 Si6 U1 136.00(13) . . ? Si1 N1 Si2 119.01(15) . . ? Si1 N1 U1 119.74(14) . . ? Si2 N1 U1 121.24(12) . . ? Si3 N2 Si4 120.05(14) . . ? Si3 N2 U1 120.66(13) . . ? Si4 N2 U1 119.28(13) . . ? Si5 N3 Si6 120.36(15) . . ? Si5 N3 U1 120.47(13) . . ? Si6 N3 U1 119.17(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.643 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.065 #===END data_UP4069(Cmpd2) _database_code_depnum_ccdc_archive 'CCDC 870191' #TrackingRef '- U(V)X2.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Cl2 N3 Si6 U' _chemical_formula_weight 790.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.9533(4) _cell_length_b 12.5081(4) _cell_length_c 22.8740(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3420.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 5.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.6029 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 65838 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.58 _reflns_number_total 7776 _reflns_number_gt 7599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0005(18) _refine_ls_number_reflns 7776 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0116 _refine_ls_R_factor_gt 0.0110 _refine_ls_wR_factor_ref 0.0281 _refine_ls_wR_factor_gt 0.0280 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.718576(6) 0.436960(5) 0.118391(3) 0.01546(2) Uani 1 1 d . . . N1 N 0.87624(13) 0.47172(12) 0.16128(7) 0.0180(3) Uani 1 1 d . . . N2 N 0.66175(13) 0.55518(14) 0.05588(6) 0.0174(3) Uani 1 1 d . . . N4 N 0.62917(13) 0.29343(13) 0.14260(7) 0.0198(3) Uani 1 1 d . . . Si1 Si 0.48285(5) 0.30188(5) 0.15680(3) 0.02596(13) Uani 1 1 d . . . Si2 Si 0.69535(5) 0.16736(4) 0.14814(3) 0.02418(13) Uani 1 1 d . . . Si3 Si 0.66133(5) 0.69513(4) 0.06958(2) 0.01972(11) Uani 1 1 d . . . Si4 Si 0.61046(5) 0.51036(5) -0.01250(3) 0.02366(12) Uani 1 1 d . . . Si5 Si 0.99663(4) 0.50865(4) 0.12060(3) 0.02198(11) Uani 1 1 d . . . Si6 Si 0.88883(5) 0.46455(4) 0.23844(2) 0.02306(12) Uani 1 1 d . . . C1 C 0.42028(18) 0.42030(19) 0.11897(11) 0.0370(5) Uani 1 1 d . . . H1A H 0.4773 0.4728 0.1121 0.055 Uiso 1 1 calc R . . H1B H 0.3627 0.4506 0.1431 0.055 Uiso 1 1 calc R . . H1C H 0.3887 0.3982 0.0823 0.055 Uiso 1 1 calc R . . C2 C 0.40635(19) 0.1841(2) 0.12652(11) 0.0406(6) Uani 1 1 d . . . H2A H 0.4214 0.1781 0.0854 0.061 Uiso 1 1 calc R . . H2B H 0.3275 0.1933 0.1325 0.061 Uiso 1 1 calc R . . H2C H 0.4309 0.1203 0.1460 0.061 Uiso 1 1 calc R . . C3 C 0.4556(2) 0.31039(18) 0.23675(10) 0.0344(5) Uani 1 1 d . . . H3A H 0.4799 0.2456 0.2553 0.052 Uiso 1 1 calc R . . H3B H 0.3769 0.3200 0.2433 0.052 Uiso 1 1 calc R . . H3C H 0.4958 0.3699 0.2528 0.052 Uiso 1 1 calc R . . C4 C 0.6696(2) 0.08553(18) 0.08139(11) 0.0407(6) Uani 1 1 d . . . H4A H 0.5913 0.0695 0.0784 0.061 Uiso 1 1 calc R . . H4B H 0.7114 0.0201 0.0839 0.061 Uiso 1 1 calc R . . H4C H 0.6929 0.1248 0.0475 0.061 Uiso 1 1 calc R . . C5 C 0.6459(2) 0.09301(18) 0.21398(11) 0.0390(6) Uani 1 1 d . . . H5A H 0.6616 0.1342 0.2484 0.059 Uiso 1 1 calc R . . H5B H 0.6840 0.0255 0.2163 0.059 Uiso 1 1 calc R . . H5C H 0.5668 0.0811 0.2111 0.059 Uiso 1 1 calc R . . C6 C 0.85031(19) 0.17993(18) 0.15845(9) 0.0289(5) Uani 1 1 d . . . H6A H 0.8854 0.1922 0.1213 0.043 Uiso 1 1 calc R . . H6B H 0.8790 0.1152 0.1753 0.043 Uiso 1 1 calc R . . H6C H 0.8659 0.2389 0.1841 0.043 Uiso 1 1 calc R . . C7 C 0.51960(18) 0.74083(18) 0.09185(10) 0.0296(5) Uani 1 1 d . . . H7A H 0.4680 0.7295 0.0603 0.044 Uiso 1 1 calc R . . H7B H 0.5220 0.8156 0.1013 0.044 Uiso 1 1 calc R . . H7C H 0.4955 0.7011 0.1255 0.044 Uiso 1 1 calc R . . C8 C 0.70715(19) 0.76902(17) 0.00281(9) 0.0276(5) Uani 1 1 d . . . H8A H 0.7819 0.7479 -0.0073 0.041 Uiso 1 1 calc R . . H8B H 0.7055 0.8445 0.0104 0.041 Uiso 1 1 calc R . . H8C H 0.6576 0.7527 -0.0290 0.041 Uiso 1 1 calc R . . C9 C 0.76355(18) 0.73541(16) 0.12778(9) 0.0250(4) Uani 1 1 d . . . H9A H 0.7254 0.7415 0.1645 0.038 Uiso 1 1 calc R . . H9B H 0.7964 0.8030 0.1178 0.038 Uiso 1 1 calc R . . H9C H 0.8213 0.6823 0.1308 0.038 Uiso 1 1 calc R . . C10 C 0.5663(2) 0.36587(18) -0.00911(11) 0.0351(6) Uani 1 1 d . . . H10A H 0.5789 0.3387 0.0296 0.053 Uiso 1 1 calc R . . H10B H 0.6093 0.3250 -0.0366 0.053 Uiso 1 1 calc R . . H10C H 0.4883 0.3602 -0.0186 0.053 Uiso 1 1 calc R . . C11 C 0.4807(2) 0.58354(19) -0.03474(11) 0.0389(6) Uani 1 1 d . . . H11A H 0.4247 0.5754 -0.0050 0.058 Uiso 1 1 calc R . . H11B H 0.4533 0.5548 -0.0709 0.058 Uiso 1 1 calc R . . H11C H 0.4975 0.6580 -0.0397 0.058 Uiso 1 1 calc R . . C12 C 0.7179(2) 0.52609(18) -0.07037(9) 0.0334(5) Uani 1 1 d . . . H12A H 0.7321 0.6007 -0.0767 0.050 Uiso 1 1 calc R . . H12B H 0.6915 0.4942 -0.1060 0.050 Uiso 1 1 calc R . . H12C H 0.7858 0.4914 -0.0584 0.050 Uiso 1 1 calc R . . C13 C 0.95870(18) 0.5641(2) 0.04711(8) 0.0291(4) Uani 1 1 d . . . H13A H 0.8790 0.5614 0.0421 0.044 Uiso 1 1 calc R . . H13B H 0.9941 0.5224 0.0171 0.044 Uiso 1 1 calc R . . H13C H 0.9836 0.6369 0.0444 0.044 Uiso 1 1 calc R . . C14 C 1.0770(2) 0.61911(18) 0.15711(10) 0.0317(5) Uani 1 1 d . . . H14A H 1.0302 0.6811 0.1606 0.048 Uiso 1 1 calc R . . H14B H 1.1417 0.6364 0.1341 0.048 Uiso 1 1 calc R . . H14C H 1.1003 0.5962 0.1953 0.048 Uiso 1 1 calc R . . C15 C 1.09037(18) 0.39181(18) 0.10998(11) 0.0341(5) Uani 1 1 d . . . H15A H 1.1170 0.3674 0.1473 0.051 Uiso 1 1 calc R . . H15B H 1.1528 0.4123 0.0861 0.051 Uiso 1 1 calc R . . H15C H 1.0498 0.3353 0.0911 0.051 Uiso 1 1 calc R . . C16 C 0.8743(2) 0.60090(17) 0.27123(9) 0.0294(5) Uani 1 1 d . . . H16A H 0.9254 0.6491 0.2524 0.044 Uiso 1 1 calc R . . H16B H 0.8910 0.5976 0.3122 0.044 Uiso 1 1 calc R . . H16C H 0.7991 0.6260 0.2659 0.044 Uiso 1 1 calc R . . C17 C 1.0266(2) 0.40716(17) 0.26089(10) 0.0348(6) Uani 1 1 d . . . H17A H 1.0350 0.3371 0.2443 0.052 Uiso 1 1 calc R . . H17B H 1.0298 0.4023 0.3027 0.052 Uiso 1 1 calc R . . H17C H 1.0859 0.4525 0.2472 0.052 Uiso 1 1 calc R . . C18 C 0.7821(2) 0.37264(17) 0.27116(9) 0.0312(5) Uani 1 1 d . . . H18A H 0.7399 0.3392 0.2405 0.047 Uiso 1 1 calc R . . H18B H 0.7325 0.4128 0.2958 0.047 Uiso 1 1 calc R . . H18C H 0.8192 0.3188 0.2940 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.61650(4) 0.54223(4) 0.19882(2) 0.02394(10) Uani 1 1 d . . . Cl2 Cl 0.82237(4) 0.33099(4) 0.03825(2) 0.02386(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 U1 0.01736(3) 0.01353(3) 0.01549(3) 0.00003(3) 0.00160(3) 0.00018(3) N1 0.0214(8) 0.0149(7) 0.0177(8) -0.0018(6) -0.0008(6) 0.0001(6) N2 0.0183(7) 0.0185(8) 0.0155(7) -0.0021(7) -0.0017(6) 0.0017(8) N4 0.0225(8) 0.0174(8) 0.0194(8) -0.0017(7) 0.0011(7) -0.0039(7) Si1 0.0214(3) 0.0260(3) 0.0305(3) 0.0011(3) 0.0033(2) -0.0065(3) Si2 0.0299(3) 0.0155(2) 0.0272(3) -0.0001(2) 0.0006(2) -0.0026(2) Si3 0.0216(3) 0.0163(3) 0.0212(3) 0.0007(2) -0.0009(2) 0.0014(2) Si4 0.0287(3) 0.0215(3) 0.0208(3) -0.0016(2) -0.0079(2) 0.0025(3) Si5 0.0186(2) 0.0212(3) 0.0261(3) -0.0034(3) 0.0002(3) -0.0020(2) Si6 0.0324(3) 0.0181(3) 0.0186(3) -0.0007(2) -0.0054(2) -0.0031(2) C1 0.0208(10) 0.0417(13) 0.0484(13) 0.0058(14) -0.0019(11) -0.0019(10) C2 0.0310(12) 0.0414(13) 0.0494(16) -0.0022(12) -0.0019(11) -0.0168(11) C3 0.0370(13) 0.0284(12) 0.0379(13) 0.0022(10) 0.0158(10) -0.0053(11) C4 0.0488(14) 0.0282(13) 0.0450(14) -0.0146(11) -0.0013(12) -0.0042(11) C5 0.0446(14) 0.0245(11) 0.0480(14) 0.0134(10) 0.0079(12) -0.0031(11) C6 0.0330(12) 0.0243(11) 0.0293(11) 0.0031(9) -0.0013(9) 0.0010(10) C7 0.0286(11) 0.0265(11) 0.0336(12) -0.0019(10) 0.0000(10) 0.0071(9) C8 0.0300(12) 0.0242(10) 0.0287(11) 0.0048(9) -0.0020(10) 0.0006(10) C9 0.0301(11) 0.0177(9) 0.0274(11) -0.0010(8) 0.0007(9) -0.0027(8) C10 0.0413(14) 0.0292(12) 0.0349(13) -0.0041(10) -0.0123(11) -0.0049(11) C11 0.0400(13) 0.0347(14) 0.0422(13) 0.0005(11) -0.0222(11) 0.0051(11) C12 0.0521(14) 0.0298(11) 0.0183(10) -0.0001(8) -0.0025(11) 0.0062(12) C13 0.0294(11) 0.0313(11) 0.0266(10) 0.0027(11) 0.0055(8) -0.0066(11) C14 0.0279(12) 0.0287(12) 0.0385(13) -0.0013(10) -0.0019(10) -0.0090(10) C15 0.0205(10) 0.0369(12) 0.0450(15) -0.0077(11) 0.0014(10) 0.0028(9) C16 0.0414(13) 0.0258(11) 0.0211(10) -0.0036(8) -0.0010(9) -0.0057(10) C17 0.0451(14) 0.0232(11) 0.0361(13) 0.0027(9) -0.0182(11) -0.0011(10) C18 0.0483(13) 0.0275(10) 0.0178(10) 0.0036(8) -0.0046(11) -0.0061(12) Cl1 0.0280(2) 0.0198(2) 0.0241(2) -0.00187(19) 0.0084(2) 0.0024(2) Cl2 0.0275(2) 0.0238(2) 0.0203(2) -0.00275(19) 0.00288(19) 0.0041(2) 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 U1 N4 2.1614(16) . ? U1 N2 2.1663(15) . ? U1 N1 2.1687(16) . ? U1 Cl1 2.5704(5) . ? U1 Cl2 2.5801(5) . ? U1 Si4 3.3877(6) . ? U1 Si1 3.4009(6) . ? U1 Si6 3.4352(6) . ? U1 Si5 3.4429(5) . ? U1 Si2 3.4514(6) . ? N1 Si6 1.7736(16) . ? N1 Si5 1.7749(17) . ? N2 Si4 1.7710(16) . ? N2 Si3 1.7783(18) . ? N4 Si2 1.7689(17) . ? N4 Si1 1.7821(17) . ? Si1 C3 1.861(2) . ? Si1 C2 1.867(2) . ? Si1 C1 1.871(2) . ? Si2 C4 1.864(2) . ? Si2 C5 1.866(2) . ? Si2 C6 1.874(2) . ? Si3 C7 1.859(2) . ? Si3 C8 1.867(2) . ? Si3 C9 1.876(2) . ? Si4 C12 1.855(2) . ? Si4 C11 1.871(2) . ? Si4 C10 1.884(2) . ? Si5 C15 1.858(2) . ? Si5 C13 1.874(2) . ? Si5 C14 1.879(2) . ? Si6 C17 1.869(2) . ? Si6 C16 1.871(2) . ? Si6 C18 1.873(2) . ? 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 N4 U1 N2 125.52(6) . . ? N4 U1 N1 118.71(6) . . ? N2 U1 N1 115.74(6) . . ? N4 U1 Cl1 90.42(4) . . ? N2 U1 Cl1 88.51(4) . . ? N1 U1 Cl1 89.20(4) . . ? N4 U1 Cl2 89.60(4) . . ? N2 U1 Cl2 91.86(4) . . ? N1 U1 Cl2 90.37(4) . . ? Cl1 U1 Cl2 179.529(17) . . ? N4 U1 Si4 105.24(4) . . ? N2 U1 Si4 27.38(4) . . ? N1 U1 Si4 132.61(4) . . ? Cl1 U1 Si4 108.217(15) . . ? Cl2 U1 Si4 72.227(15) . . ? N4 U1 Si1 27.32(4) . . ? N2 U1 Si1 104.47(4) . . ? N1 U1 Si1 134.65(4) . . ? Cl1 U1 Si1 71.112(15) . . ? Cl2 U1 Si1 109.070(16) . . ? Si4 U1 Si1 92.686(15) . . ? N4 U1 Si6 99.88(4) . . ? N2 U1 Si6 130.15(4) . . ? N1 U1 Si6 26.29(4) . . ? Cl1 U1 Si6 69.979(16) . . ? Cl2 U1 Si6 109.555(16) . . ? Si4 U1 Si6 154.851(14) . . ? Si1 U1 Si6 109.525(15) . . ? N4 U1 Si5 133.62(4) . . ? N2 U1 Si5 97.74(4) . . ? N1 U1 Si5 26.13(4) . . ? Cl1 U1 Si5 108.320(15) . . ? Cl2 U1 Si5 71.340(15) . . ? Si4 U1 Si5 108.099(16) . . ? Si1 U1 Si5 157.735(15) . . ? Si6 U1 Si5 52.425(15) . . ? N4 U1 Si2 25.60(4) . . ? N2 U1 Si2 140.53(4) . . ? N1 U1 Si2 100.17(4) . . ? Cl1 U1 Si2 108.734(15) . . ? Cl2 U1 Si2 71.144(15) . . ? Si4 U1 Si2 114.103(14) . . ? Si1 U1 Si2 52.916(14) . . ? Si6 U1 Si2 89.322(14) . . ? Si5 U1 Si2 109.223(13) . . ? Si6 N1 Si5 117.78(9) . . ? Si6 N1 U1 120.91(8) . . ? Si5 N1 U1 121.31(8) . . ? Si4 N2 Si3 117.79(9) . . ? Si4 N2 U1 118.38(9) . . ? Si3 N2 U1 123.81(8) . . ? Si2 N4 Si1 118.60(9) . . ? Si2 N4 U1 122.53(9) . . ? Si1 N4 U1 118.86(9) . . ? N4 Si1 C3 110.76(10) . . ? N4 Si1 C2 111.48(10) . . ? C3 Si1 C2 108.90(11) . . ? N4 Si1 C1 110.79(9) . . ? C3 Si1 C1 109.83(11) . . ? C2 Si1 C1 104.91(11) . . ? N4 Si1 U1 33.82(5) . . ? C3 Si1 U1 111.76(8) . . ? C2 Si1 U1 134.58(8) . . ? C1 Si1 U1 79.54(7) . . ? N4 Si2 C4 110.91(10) . . ? N4 Si2 C5 111.14(10) . . ? C4 Si2 C5 109.59(11) . . ? N4 Si2 C6 112.11(9) . . ? C4 Si2 C6 108.20(12) . . ? C5 Si2 C6 104.66(11) . . ? N4 Si2 U1 31.87(5) . . ? C4 Si2 U1 112.85(8) . . ? C5 Si2 U1 132.19(8) . . ? C6 Si2 U1 82.14(7) . . ? N2 Si3 C7 110.70(9) . . ? N2 Si3 C8 110.02(8) . . ? C7 Si3 C8 109.82(10) . . ? N2 Si3 C9 112.81(8) . . ? C7 Si3 C9 108.45(10) . . ? C8 Si3 C9 104.86(10) . . ? N2 Si4 C12 110.91(9) . . ? N2 Si4 C11 111.85(10) . . ? C12 Si4 C11 109.14(11) . . ? N2 Si4 C10 111.36(10) . . ? C12 Si4 C10 108.97(11) . . ? C11 Si4 C10 104.37(11) . . ? N2 Si4 U1 34.23(6) . . ? C12 Si4 U1 113.29(8) . . ? C11 Si4 U1 133.55(9) . . ? C10 Si4 U1 79.08(8) . . ? N1 Si5 C15 110.66(9) . . ? N1 Si5 C13 111.74(9) . . ? C15 Si5 C13 108.66(11) . . ? N1 Si5 C14 111.91(9) . . ? C15 Si5 C14 109.15(11) . . ? C13 Si5 C14 104.49(11) . . ? N1 Si5 U1 32.56(5) . . ? C15 Si5 U1 112.05(7) . . ? C13 Si5 U1 81.35(7) . . ? C14 Si5 U1 133.78(8) . . ? N1 Si6 C17 111.57(10) . . ? N1 Si6 C16 110.18(9) . . ? C17 Si6 C16 108.77(10) . . ? N1 Si6 C18 111.77(9) . . ? C17 Si6 C18 104.75(11) . . ? C16 Si6 C18 109.63(10) . . ? N1 Si6 U1 32.79(5) . . ? C17 Si6 U1 134.69(8) . . ? C16 Si6 U1 110.92(7) . . ? C18 Si6 U1 81.63(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.467 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.048 #===END data_UP4095(Cmpd3) _database_code_depnum_ccdc_archive 'CCDC 870192' #TrackingRef '- U(V)X2.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Br2 N3 Si6 U' _chemical_formula_weight 879.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _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 12.5472(12) _cell_length_b 15.7287(15) _cell_length_c 36.278(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.963(2) _cell_angle_gamma 90.00 _cell_volume 7072.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 7.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.4893 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 42607 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15933 _reflns_number_gt 12847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0215P)^2^+18.7501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15933 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.479406(14) 0.868707(11) 0.146916(5) 0.02199(5) Uani 1 1 d . . . Br1 Br 0.37214(5) 0.99380(3) 0.103615(16) 0.03936(13) Uani 1 1 d . . . Br2 Br 0.58182(4) 0.74136(3) 0.190986(15) 0.03530(12) Uani 1 1 d . . . Si1 Si 0.46224(12) 0.91840(9) 0.23937(4) 0.0282(3) Uani 1 1 d . . . Si2 Si 0.53830(11) 1.05775(8) 0.19173(4) 0.0269(3) Uani 1 1 d . . . Si3 Si 0.34797(12) 0.68236(9) 0.12039(4) 0.0311(3) Uani 1 1 d . . . Si4 Si 0.20418(12) 0.82820(11) 0.13633(4) 0.0381(4) Uani 1 1 d . . . Si5 Si 0.74220(12) 0.85640(10) 0.13042(5) 0.0362(4) Uani 1 1 d . . . Si6 Si 0.57258(13) 0.87263(10) 0.06172(4) 0.0372(3) Uani 1 1 d . . . N1 N 0.4933(3) 0.9511(2) 0.19527(10) 0.0231(8) Uani 1 1 d . . . N2 N 0.3365(3) 0.7901(3) 0.13466(11) 0.0253(9) Uani 1 1 d . . . N3 N 0.6026(3) 0.8657(3) 0.11123(11) 0.0257(9) Uani 1 1 d . . . C1 C 0.3860(5) 1.0029(4) 0.26070(16) 0.0403(13) Uani 1 1 d . . . H1a H 0.4283 1.0540 0.2638 0.060 Uiso 1 1 calc R . . H1b H 0.3714 0.9839 0.2846 0.060 Uiso 1 1 calc R . . H1c H 0.3191 1.0141 0.2446 0.060 Uiso 1 1 calc R . . C2 C 0.3764(4) 0.8211(4) 0.23591(15) 0.0377(13) Uani 1 1 d . . . H2a H 0.3683 0.7992 0.2109 0.057 Uiso 1 1 calc R . . H2b H 0.3067 0.8352 0.2420 0.057 Uiso 1 1 calc R . . H2c H 0.4099 0.7790 0.2530 0.057 Uiso 1 1 calc R . . C3 C 0.5875(5) 0.8937(4) 0.27245(16) 0.0474(15) Uani 1 1 d . . . H3a H 0.6310 0.8546 0.2609 0.071 Uiso 1 1 calc R . . H3b H 0.5687 0.8686 0.2947 0.071 Uiso 1 1 calc R . . H3c H 0.6274 0.9451 0.2787 0.071 Uiso 1 1 calc R . . C4 C 0.4247(4) 1.1356(3) 0.18795(17) 0.0399(13) Uani 1 1 d . . . H4a H 0.3646 1.1144 0.1707 0.060 Uiso 1 1 calc R . . H4b H 0.4476 1.1891 0.1792 0.060 Uiso 1 1 calc R . . H4c H 0.4033 1.1432 0.2120 0.060 Uiso 1 1 calc R . . C5 C 0.6056(5) 1.0719(4) 0.14962(15) 0.0394(13) Uani 1 1 d . . . H5a H 0.5983 1.0208 0.1350 0.059 Uiso 1 1 calc R . . H5b H 0.6808 1.0841 0.1573 0.059 Uiso 1 1 calc R . . H5c H 0.5724 1.1183 0.1349 0.059 Uiso 1 1 calc R . . C6 C 0.6412(5) 1.0866(4) 0.23298(16) 0.0395(13) Uani 1 1 d . . . H6a H 0.6072 1.0898 0.2549 0.059 Uiso 1 1 calc R . . H6b H 0.6725 1.1407 0.2287 0.059 Uiso 1 1 calc R . . H6c H 0.6968 1.0440 0.2365 0.059 Uiso 1 1 calc R . . C7 C 0.2406(5) 0.6537(4) 0.08088(16) 0.0439(15) Uani 1 1 d . . . H7a H 0.1711 0.6654 0.0877 0.066 Uiso 1 1 calc R . . H7b H 0.2458 0.5944 0.0753 0.066 Uiso 1 1 calc R . . H7c H 0.2496 0.6867 0.0593 0.066 Uiso 1 1 calc R . . C8 C 0.3409(5) 0.6071(4) 0.15941(16) 0.0489(16) Uani 1 1 d . . . H8a H 0.3836 0.6284 0.1817 0.073 Uiso 1 1 calc R . . H8b H 0.3681 0.5526 0.1534 0.073 Uiso 1 1 calc R . . H8c H 0.2673 0.6013 0.1633 0.073 Uiso 1 1 calc R . . C9 C 0.4783(5) 0.6635(4) 0.10248(16) 0.0405(14) Uani 1 1 d . . . H9a H 0.5172 0.7161 0.1025 0.061 Uiso 1 1 calc R . . H9b H 0.4636 0.6417 0.0775 0.061 Uiso 1 1 calc R . . H9c H 0.5209 0.6231 0.1182 0.061 Uiso 1 1 calc R . . C10 C 0.2026(5) 0.9283(4) 0.16437(18) 0.0504(16) Uani 1 1 d . . . H10a H 0.1649 0.9183 0.1851 0.076 Uiso 1 1 calc R . . H10b H 0.1667 0.9725 0.1489 0.076 Uiso 1 1 calc R . . H10c H 0.2753 0.9455 0.1735 0.076 Uiso 1 1 calc R . . C11 C 0.1334(5) 0.8517(5) 0.08844(17) 0.0523(17) Uani 1 1 d . . . H11a H 0.1780 0.8874 0.0758 0.078 Uiso 1 1 calc R . . H11b H 0.0666 0.8802 0.0900 0.078 Uiso 1 1 calc R . . H11c H 0.1190 0.7994 0.0749 0.078 Uiso 1 1 calc R . . C12 C 0.1246(5) 0.7484(5) 0.1590(2) 0.0597(19) Uani 1 1 d . . . H12a H 0.1121 0.6990 0.1433 0.090 Uiso 1 1 calc R . . H12b H 0.0568 0.7729 0.1624 0.090 Uiso 1 1 calc R . . H12c H 0.1642 0.7324 0.1828 0.090 Uiso 1 1 calc R . . C13 C 0.7886(4) 0.7433(4) 0.12978(19) 0.0458(15) Uani 1 1 d . . . H13a H 0.7359 0.7068 0.1381 0.069 Uiso 1 1 calc R . . H13b H 0.8562 0.7372 0.1460 0.069 Uiso 1 1 calc R . . H13c H 0.7974 0.7279 0.1048 0.069 Uiso 1 1 calc R . . C14 C 0.8320(5) 0.9221(4) 0.1053(2) 0.0559(18) Uani 1 1 d . . . H14a H 0.8309 0.9000 0.0806 0.084 Uiso 1 1 calc R . . H14b H 0.9044 0.9202 0.1186 0.084 Uiso 1 1 calc R . . H14c H 0.8069 0.9798 0.1039 0.084 Uiso 1 1 calc R . . C15 C 0.7709(5) 0.8995(4) 0.17939(17) 0.0467(15) Uani 1 1 d . . . H15a H 0.7942 0.9575 0.1787 0.070 Uiso 1 1 calc R . . H15b H 0.8265 0.8662 0.1938 0.070 Uiso 1 1 calc R . . H15c H 0.7065 0.8967 0.1906 0.070 Uiso 1 1 calc R . . C16 C 0.4300(5) 0.8416(4) 0.04340(16) 0.0501(16) Uani 1 1 d . . . H16a H 0.3976 0.8167 0.0631 0.075 Uiso 1 1 calc R . . H16b H 0.4295 0.8010 0.0236 0.075 Uiso 1 1 calc R . . H16c H 0.3898 0.8911 0.0341 0.075 Uiso 1 1 calc R . . C17 C 0.6545(6) 0.7959(5) 0.0384(2) 0.064(2) Uani 1 1 d . . . H17a H 0.7298 0.8060 0.0468 0.096 Uiso 1 1 calc R . . H17b H 0.6389 0.8034 0.0119 0.096 Uiso 1 1 calc R . . H17c H 0.6367 0.7388 0.0447 0.096 Uiso 1 1 calc R . . C18 C 0.5997(6) 0.9836(4) 0.04632(18) 0.0549(17) Uani 1 1 d . . . H18a H 0.5416 1.0203 0.0505 0.082 Uiso 1 1 calc R . . H18b H 0.6054 0.9833 0.0202 0.082 Uiso 1 1 calc R . . H18c H 0.6660 1.0039 0.0604 0.082 Uiso 1 1 calc R . . U1' U 0.934677(14) 0.172244(11) 0.608599(5) 0.02373(5) Uani 1 1 d . . . Br1' Br 1.02542(5) 0.01374(3) 0.605519(16) 0.03856(13) Uani 1 1 d . . . Br2' Br 0.84307(4) 0.32959(3) 0.611528(16) 0.03641(12) Uani 1 1 d . . . Si1' Si 1.03091(13) 0.26670(12) 0.69309(5) 0.0428(4) Uani 1 1 d . . . Si2' Si 0.96285(14) 0.08115(12) 0.69611(5) 0.0441(4) Uani 1 1 d . . . Si3' Si 1.00468(13) 0.29415(11) 0.53738(4) 0.0376(4) Uani 1 1 d . . . Si4' Si 1.18772(11) 0.19767(10) 0.58426(4) 0.0317(3) Uani 1 1 d . . . Si5' Si 0.65668(12) 0.15343(10) 0.60176(5) 0.0357(3) Uani 1 1 d . . . Si6' Si 0.76311(13) 0.05557(10) 0.54530(4) 0.0352(3) Uani 1 1 d . . . N1' N 0.9774(3) 0.1739(3) 0.66881(12) 0.0333(10) Uani 1 1 d . . . N2' N 1.0471(3) 0.2237(2) 0.57511(11) 0.0254(9) Uani 1 1 d . . . N3' N 0.7778(3) 0.1243(2) 0.58478(11) 0.0275(9) Uani 1 1 d . . . C1' C 1.1436(5) 0.2411(5) 0.73127(19) 0.067(2) Uani 1 1 d . . . H1a' H 1.1197 0.1999 0.7477 0.100 Uiso 1 1 calc R . . H1b' H 1.1659 0.2919 0.7450 0.100 Uiso 1 1 calc R . . H1c' H 1.2032 0.2185 0.7208 0.100 Uiso 1 1 calc R . . C2' C 1.0930(5) 0.3416(4) 0.66272(19) 0.0542(17) Uani 1 1 d . . . H2a' H 1.1631 0.3583 0.6751 0.081 Uiso 1 1 calc R . . H2b' H 1.0481 0.3910 0.6578 0.081 Uiso 1 1 calc R . . H2c' H 1.0998 0.3141 0.6396 0.081 Uiso 1 1 calc R . . C3' C 0.9246(6) 0.3251(5) 0.71368(19) 0.063(2) Uani 1 1 d . . . H3a' H 0.8646 0.3369 0.6945 0.094 Uiso 1 1 calc R . . H3b' H 0.9538 0.3776 0.7244 0.094 Uiso 1 1 calc R . . H3c' H 0.9007 0.2908 0.7327 0.094 Uiso 1 1 calc R . . C4' C 1.0931(6) 0.0251(5) 0.70857(19) 0.062(2) Uani 1 1 d . . . H4a' H 1.1256 0.0170 0.6866 0.093 Uiso 1 1 calc R . . H4b' H 1.0810 -0.0292 0.7193 0.093 Uiso 1 1 calc R . . H4c' H 1.1403 0.0583 0.7263 0.093 Uiso 1 1 calc R . . C5' C 0.8594(6) 0.0050(4) 0.67198(19) 0.0584(19) Uani 1 1 d . . . H5a' H 0.8253 0.0294 0.6489 0.088 Uiso 1 1 calc R . . H5b' H 0.8060 -0.0059 0.6877 0.088 Uiso 1 1 calc R . . H5c' H 0.8940 -0.0474 0.6671 0.088 Uiso 1 1 calc R . . C6' C 0.9124(6) 0.1094(6) 0.74060(18) 0.069(2) Uani 1 1 d . . . H6a' H 0.9676 0.1397 0.7567 0.103 Uiso 1 1 calc R . . H6b' H 0.8946 0.0583 0.7528 0.103 Uiso 1 1 calc R . . H6c' H 0.8494 0.1445 0.7351 0.103 Uiso 1 1 calc R . . C7' C 1.0705(5) 0.2645(5) 0.49636(18) 0.065(2) Uani 1 1 d . . . H7a' H 1.1473 0.2616 0.5039 0.098 Uiso 1 1 calc R . . H7b' H 1.0540 0.3065 0.4771 0.098 Uiso 1 1 calc R . . H7c' H 1.0442 0.2101 0.4870 0.098 Uiso 1 1 calc R . . C8' C 1.0359(5) 0.4069(4) 0.5505(2) 0.0556(18) Uani 1 1 d . . . H8a' H 0.9933 0.4437 0.5329 0.083 Uiso 1 1 calc R . . H8b' H 1.1111 0.4176 0.5502 0.083 Uiso 1 1 calc R . . H8c' H 1.0193 0.4174 0.5750 0.083 Uiso 1 1 calc R . . C9' C 0.8555(5) 0.2860(4) 0.52022(16) 0.0457(15) Uani 1 1 d . . . H9a' H 0.8437 0.2557 0.4970 0.069 Uiso 1 1 calc R . . H9b' H 0.8252 0.3420 0.5167 0.069 Uiso 1 1 calc R . . H9c' H 0.8214 0.2560 0.5383 0.069 Uiso 1 1 calc R . . C10' C 1.2308(5) 0.1608(4) 0.63370(16) 0.0464(15) Uani 1 1 d . . . H10a' H 1.1702 0.1627 0.6469 0.070 Uiso 1 1 calc R . . H10b' H 1.2868 0.1973 0.6458 0.070 Uiso 1 1 calc R . . H10c' H 1.2573 0.1036 0.6336 0.070 Uiso 1 1 calc R . . C11' C 1.2220(5) 0.1125(4) 0.55192(17) 0.0452(15) Uani 1 1 d . . . H11a' H 1.1657 0.0706 0.5486 0.068 Uiso 1 1 calc R . . H11b' H 1.2889 0.0861 0.5624 0.068 Uiso 1 1 calc R . . H11c' H 1.2290 0.1372 0.5282 0.068 Uiso 1 1 calc R . . C12' C 1.2725(5) 0.2935(4) 0.57906(19) 0.0496(16) Uani 1 1 d . . . H12a' H 1.2558 0.3149 0.5540 0.074 Uiso 1 1 calc R . . H12b' H 1.3474 0.2782 0.5841 0.074 Uiso 1 1 calc R . . H12c' H 1.2579 0.3366 0.5963 0.074 Uiso 1 1 calc R . . C13' C 0.5849(4) 0.2404(4) 0.57219(18) 0.0469(15) Uani 1 1 d . . . H13a' H 0.6369 0.2786 0.5646 0.070 Uiso 1 1 calc R . . H13b' H 0.5389 0.2710 0.5864 0.070 Uiso 1 1 calc R . . H13c' H 0.5421 0.2160 0.5505 0.070 Uiso 1 1 calc R . . C14' C 0.5618(5) 0.0615(4) 0.6017(2) 0.0563(18) Uani 1 1 d . . . H14a' H 0.5403 0.0419 0.5765 0.084 Uiso 1 1 calc R . . H14b' H 0.4992 0.0792 0.6119 0.084 Uiso 1 1 calc R . . H14c' H 0.5972 0.0162 0.6165 0.084 Uiso 1 1 calc R . . C15' C 0.6816(5) 0.1869(4) 0.65214(16) 0.0444(15) Uani 1 1 d . . . H15a' H 0.6773 0.1381 0.6677 0.067 Uiso 1 1 calc R . . H15b' H 0.6281 0.2278 0.6565 0.067 Uiso 1 1 calc R . . H15c' H 0.7520 0.2119 0.6579 0.067 Uiso 1 1 calc R . . C16' C 0.8817(5) 0.0646(4) 0.51999(15) 0.0393(13) Uani 1 1 d . . . H16a' H 0.9330 0.1039 0.5329 0.059 Uiso 1 1 calc R . . H16b' H 0.8580 0.0846 0.4951 0.059 Uiso 1 1 calc R . . H16c' H 0.9150 0.0098 0.5191 0.059 Uiso 1 1 calc R . . C17' C 0.6436(5) 0.0849(4) 0.50976(17) 0.0514(16) Uani 1 1 d . . . H17a' H 0.5791 0.0814 0.5209 0.077 Uiso 1 1 calc R . . H17b' H 0.6384 0.0464 0.4890 0.077 Uiso 1 1 calc R . . H17c' H 0.6523 0.1419 0.5012 0.077 Uiso 1 1 calc R . . C18' C 0.7473(6) -0.0563(4) 0.55944(19) 0.0540(17) Uani 1 1 d . . . H18a' H 0.8101 -0.0735 0.5764 0.081 Uiso 1 1 calc R . . H18b' H 0.7389 -0.0921 0.5378 0.081 Uiso 1 1 calc R . . H18c' H 0.6847 -0.0612 0.5715 0.081 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 U1 0.02472(9) 0.01825(8) 0.02277(9) -0.00028(7) 0.00295(7) 0.00239(7) Br1 0.0483(3) 0.0286(3) 0.0387(3) 0.0054(2) -0.0011(2) 0.0126(2) Br2 0.0416(3) 0.0276(3) 0.0347(3) 0.0060(2) -0.0003(2) 0.0074(2) Si1 0.0362(8) 0.0266(7) 0.0229(7) -0.0014(6) 0.0082(6) -0.0040(6) Si2 0.0304(7) 0.0182(6) 0.0328(7) -0.0026(6) 0.0066(6) -0.0009(5) Si3 0.0422(8) 0.0237(7) 0.0273(7) -0.0001(6) 0.0050(6) -0.0065(6) Si4 0.0270(7) 0.0495(10) 0.0373(8) -0.0092(8) 0.0032(6) -0.0015(7) Si5 0.0281(7) 0.0291(8) 0.0525(10) -0.0023(7) 0.0105(7) 0.0025(6) Si6 0.0469(9) 0.0371(9) 0.0305(8) 0.0017(7) 0.0151(7) -0.0023(7) N1 0.028(2) 0.020(2) 0.023(2) 0.0008(16) 0.0064(16) -0.0012(16) N2 0.028(2) 0.025(2) 0.023(2) -0.0016(17) 0.0035(17) -0.0026(17) N3 0.025(2) 0.023(2) 0.028(2) -0.0009(18) 0.0021(17) -0.0011(17) C1 0.040(3) 0.043(3) 0.039(3) -0.010(3) 0.013(3) -0.003(3) C2 0.041(3) 0.040(3) 0.033(3) 0.002(3) 0.011(2) -0.009(3) C3 0.058(4) 0.048(4) 0.033(3) 0.002(3) -0.005(3) -0.001(3) C4 0.039(3) 0.027(3) 0.054(4) 0.001(3) 0.006(3) 0.004(2) C5 0.049(3) 0.030(3) 0.041(3) 0.004(2) 0.014(3) -0.011(3) C6 0.045(3) 0.030(3) 0.042(3) -0.007(3) 0.002(3) -0.009(2) C7 0.056(4) 0.039(3) 0.034(3) -0.006(3) -0.002(3) -0.017(3) C8 0.065(4) 0.043(4) 0.038(3) 0.012(3) 0.005(3) -0.019(3) C9 0.056(4) 0.027(3) 0.041(3) -0.006(2) 0.016(3) 0.004(3) C10 0.046(4) 0.056(4) 0.050(4) -0.018(3) 0.009(3) 0.011(3) C11 0.036(3) 0.072(5) 0.044(4) -0.015(3) -0.007(3) 0.017(3) C12 0.043(4) 0.077(5) 0.063(4) -0.016(4) 0.020(3) -0.023(3) C13 0.031(3) 0.034(3) 0.072(4) -0.004(3) 0.008(3) 0.005(2) C14 0.049(4) 0.049(4) 0.075(5) -0.010(4) 0.028(4) -0.011(3) C15 0.043(3) 0.045(4) 0.049(4) -0.007(3) -0.002(3) 0.008(3) C16 0.074(5) 0.044(4) 0.030(3) 0.001(3) 0.004(3) -0.004(3) C17 0.069(5) 0.073(5) 0.058(4) -0.019(4) 0.033(4) -0.001(4) C18 0.061(4) 0.058(4) 0.046(4) 0.019(3) 0.011(3) -0.013(3) U1' 0.02474(9) 0.01971(9) 0.02781(10) 0.00065(8) 0.00744(7) 0.00313(7) Br1' 0.0464(3) 0.0247(3) 0.0466(3) 0.0027(2) 0.0136(3) 0.0115(2) Br2' 0.0366(3) 0.0237(2) 0.0497(3) -0.0019(2) 0.0092(2) 0.0073(2) Si1' 0.0373(9) 0.0537(11) 0.0362(9) -0.0134(8) 0.0021(7) 0.0094(8) Si2' 0.0445(9) 0.0553(11) 0.0359(9) 0.0151(8) 0.0165(7) 0.0159(8) Si3' 0.0358(8) 0.0424(9) 0.0346(8) 0.0120(7) 0.0056(7) -0.0056(7) Si4' 0.0248(7) 0.0354(8) 0.0358(8) -0.0073(7) 0.0075(6) -0.0013(6) Si5' 0.0293(7) 0.0309(8) 0.0486(9) -0.0016(7) 0.0117(7) -0.0027(6) Si6' 0.0424(9) 0.0271(8) 0.0366(8) -0.0050(7) 0.0081(7) -0.0072(6) N1' 0.035(2) 0.038(3) 0.029(2) -0.001(2) 0.0101(19) 0.012(2) N2' 0.027(2) 0.021(2) 0.029(2) -0.0020(17) 0.0046(17) -0.0028(16) N3' 0.032(2) 0.021(2) 0.031(2) 0.0015(18) 0.0098(18) 0.0001(17) C1' 0.049(4) 0.100(6) 0.047(4) -0.005(4) -0.009(3) 0.006(4) C2' 0.050(4) 0.044(4) 0.067(4) -0.019(3) 0.006(3) -0.003(3) C3' 0.062(4) 0.075(5) 0.052(4) -0.027(4) 0.013(3) 0.017(4) C4' 0.066(5) 0.070(5) 0.053(4) 0.027(4) 0.015(3) 0.025(4) C5' 0.083(5) 0.040(4) 0.060(4) 0.014(3) 0.034(4) 0.007(3) C6' 0.057(4) 0.109(7) 0.045(4) 0.019(4) 0.023(3) 0.015(4) C7' 0.049(4) 0.110(7) 0.040(4) 0.021(4) 0.019(3) 0.000(4) C8' 0.048(4) 0.039(4) 0.078(5) 0.023(3) 0.002(3) -0.008(3) C9' 0.046(3) 0.052(4) 0.038(3) 0.013(3) 0.000(3) -0.006(3) C10' 0.034(3) 0.060(4) 0.044(3) -0.009(3) 0.000(3) 0.011(3) C11' 0.039(3) 0.054(4) 0.045(3) -0.014(3) 0.013(3) 0.002(3) C12' 0.040(3) 0.051(4) 0.060(4) -0.004(3) 0.015(3) -0.014(3) C13' 0.030(3) 0.048(4) 0.062(4) -0.005(3) 0.005(3) 0.008(3) C14' 0.045(4) 0.048(4) 0.083(5) -0.005(4) 0.029(4) -0.018(3) C15' 0.042(3) 0.045(4) 0.051(4) 0.004(3) 0.023(3) 0.007(3) C16' 0.045(3) 0.041(3) 0.033(3) -0.007(3) 0.010(3) -0.004(3) C17' 0.057(4) 0.055(4) 0.040(3) -0.003(3) -0.001(3) -0.012(3) C18' 0.078(5) 0.027(3) 0.060(4) -0.008(3) 0.023(4) -0.010(3) 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 U1 N1 2.166(4) . ? U1 N3 2.166(4) . ? U1 N2 2.167(4) . ? U1 Br1 2.7371(6) . ? U1 Br2 2.7530(6) . ? U1 Si2 3.4141(14) . ? U1 Si3 3.4267(14) . ? U1 Si5 3.4471(15) . ? Si1 N1 1.780(4) . ? Si1 C2 1.864(5) . ? Si1 C3 1.864(6) . ? Si1 C1 1.874(6) . ? Si2 N1 1.782(4) . ? Si2 C4 1.868(5) . ? Si2 C5 1.871(6) . ? Si2 C6 1.874(5) . ? Si3 N2 1.784(4) . ? Si3 C8 1.858(6) . ? Si3 C7 1.863(5) . ? Si3 C9 1.875(6) . ? Si4 N2 1.775(4) . ? Si4 C11 1.861(6) . ? Si4 C12 1.871(7) . ? Si4 C10 1.877(6) . ? Si5 N3 1.787(4) . ? Si5 C14 1.866(6) . ? Si5 C13 1.873(6) . ? Si5 C15 1.883(6) . ? Si6 N3 1.780(4) . ? Si6 C17 1.870(7) . ? Si6 C16 1.874(7) . ? Si6 C18 1.880(6) . ? U1' N2' 2.158(4) . ? U1' N3' 2.159(4) . ? U1' N1' 2.167(4) . ? U1' Br2' 2.7378(6) . ? U1' Br1' 2.7502(6) . ? U1' Si6' 3.4256(15) . ? U1' Si3' 3.4396(15) . ? U1' Si4' 3.4487(15) . ? U1' Si2' 3.4505(16) . ? U1' Si1' 3.4506(16) . ? Si1' N1' 1.782(5) . ? Si1' C1' 1.862(6) . ? Si1' C2' 1.865(7) . ? Si1' C3' 1.869(6) . ? Si2' N1' 1.788(5) . ? Si2' C4' 1.850(7) . ? Si2' C6' 1.876(7) . ? Si2' C5' 1.879(7) . ? Si3' N2' 1.776(4) . ? Si3' C8' 1.861(7) . ? Si3' C7' 1.870(7) . ? Si3' C9' 1.883(6) . ? Si4' N2' 1.792(4) . ? Si4' C12' 1.872(6) . ? Si4' C11' 1.874(6) . ? Si4' C10' 1.882(6) . ? Si5' N3' 1.786(4) . ? Si5' C14' 1.873(6) . ? Si5' C13' 1.880(6) . ? Si5' C15' 1.881(6) . ? Si6' N3' 1.781(4) . ? Si6' C18' 1.852(6) . ? Si6' C16' 1.871(6) . ? Si6' C17' 1.876(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 N1 U1 N3 121.50(15) . . ? N1 U1 N2 117.84(14) . . ? N3 U1 N2 120.65(15) . . ? N1 U1 Br1 90.29(10) . . ? N3 U1 Br1 90.32(11) . . ? N2 U1 Br1 88.58(11) . . ? N1 U1 Br2 89.63(10) . . ? N3 U1 Br2 91.09(11) . . ? N2 U1 Br2 90.02(11) . . ? Br1 U1 Br2 178.382(19) . . ? N1 U1 Si2 27.03(10) . . ? N3 U1 Si2 100.48(11) . . ? N2 U1 Si2 134.89(11) . . ? Br1 U1 Si2 72.41(3) . . ? Br2 U1 Si2 108.08(3) . . ? N1 U1 Si3 135.52(10) . . ? N3 U1 Si3 99.82(11) . . ? N2 U1 Si3 26.80(11) . . ? Br1 U1 Si3 106.35(3) . . ? Br2 U1 Si3 72.63(3) . . ? Si2 U1 Si3 159.67(4) . . ? N1 U1 Si5 102.47(11) . . ? N3 U1 Si5 26.35(11) . . ? N2 U1 Si5 135.71(11) . . ? Br1 U1 Si5 109.81(3) . . ? Br2 U1 Si5 71.78(3) . . ? Si2 U1 Si5 89.40(4) . . ? Si3 U1 Si5 109.56(4) . . ? N1 Si1 C2 112.4(2) . . ? N1 Si1 C3 111.0(2) . . ? C2 Si1 C3 107.0(3) . . ? N1 Si1 C1 111.3(2) . . ? C2 Si1 C1 106.4(3) . . ? C3 Si1 C1 108.4(3) . . ? N1 Si2 C4 112.0(2) . . ? N1 Si2 C5 111.1(2) . . ? C4 Si2 C5 107.4(3) . . ? N1 Si2 C6 110.9(2) . . ? C4 Si2 C6 108.9(3) . . ? C5 Si2 C6 106.3(3) . . ? N1 Si2 U1 33.55(12) . . ? C4 Si2 U1 115.45(19) . . ? C5 Si2 U1 78.87(18) . . ? C6 Si2 U1 131.46(19) . . ? N2 Si3 C8 111.6(3) . . ? N2 Si3 C7 111.8(2) . . ? C8 Si3 C7 108.5(3) . . ? N2 Si3 C9 111.4(2) . . ? C8 Si3 C9 108.1(3) . . ? C7 Si3 C9 105.1(3) . . ? N2 Si3 U1 33.21(13) . . ? C8 Si3 U1 114.1(2) . . ? C7 Si3 U1 132.96(19) . . ? C9 Si3 U1 79.92(18) . . ? N2 Si4 C11 110.4(2) . . ? N2 Si4 C12 110.7(3) . . ? C11 Si4 C12 109.5(3) . . ? N2 Si4 C10 113.0(2) . . ? C11 Si4 C10 107.2(3) . . ? C12 Si4 C10 105.9(3) . . ? N3 Si5 C14 113.2(3) . . ? N3 Si5 C13 111.1(2) . . ? C14 Si5 C13 107.9(3) . . ? N3 Si5 C15 111.7(2) . . ? C14 Si5 C15 102.7(3) . . ? C13 Si5 C15 109.8(3) . . ? N3 Si5 U1 32.55(13) . . ? C14 Si5 U1 136.1(2) . . ? C13 Si5 U1 111.28(19) . . ? C15 Si5 U1 82.2(2) . . ? N3 Si6 C17 111.8(3) . . ? N3 Si6 C16 112.5(2) . . ? C17 Si6 C16 103.5(3) . . ? N3 Si6 C18 109.7(3) . . ? C17 Si6 C18 109.1(3) . . ? C16 Si6 C18 110.1(3) . . ? Si1 N1 Si2 116.9(2) . . ? Si1 N1 U1 123.6(2) . . ? Si2 N1 U1 119.42(19) . . ? Si4 N2 Si3 116.7(2) . . ? Si4 N2 U1 123.3(2) . . ? Si3 N2 U1 120.0(2) . . ? Si6 N3 Si5 116.0(2) . . ? Si6 N3 U1 122.9(2) . . ? Si5 N3 U1 121.1(2) . . ? N2' U1' N3' 122.76(15) . . ? N2' U1' N1' 118.86(16) . . ? N3' U1' N1' 118.32(16) . . ? N2' U1' Br2' 89.87(10) . . ? N3' U1' Br2' 88.23(11) . . ? N1' U1' Br2' 89.41(11) . . ? N2' U1' Br1' 90.36(10) . . ? N3' U1' Br1' 91.41(11) . . ? N1' U1' Br1' 90.72(11) . . ? Br2' U1' Br1' 179.63(2) . . ? N2' U1' Si6' 102.78(11) . . ? N3' U1' Si6' 26.62(11) . . ? N1' U1' Si6' 135.48(13) . . ? Br2' U1' Si6' 106.65(3) . . ? Br1' U1' Si6' 73.02(3) . . ? N2' U1' Si3' 26.09(11) . . ? N3' U1' Si3' 102.58(11) . . ? N1' U1' Si3' 134.33(13) . . ? Br2' U1' Si3' 71.53(3) . . ? Br1' U1' Si3' 108.60(3) . . ? Si6' U1' Si3' 90.14(4) . . ? N2' U1' Si4' 26.32(11) . . ? N3' U1' Si4' 139.16(11) . . ? N1' U1' Si4' 99.43(12) . . ? Br2' U1' Si4' 108.30(3) . . ? Br1' U1' Si4' 72.02(3) . . ? Si6' U1' Si4' 113.45(4) . . ? Si3' U1' Si4' 52.41(4) . . ? N2' U1' Si2' 133.77(11) . . ? N3' U1' Si2' 100.34(11) . . ? N1' U1' Si2' 26.30(13) . . ? Br2' U1' Si2' 108.85(3) . . ? Br1' U1' Si2' 71.17(3) . . ? Si6' U1' Si2' 110.97(4) . . ? Si3' U1' Si2' 157.08(4) . . ? Si4' U1' Si2' 108.50(4) . . ? N2' U1' Si1' 99.77(11) . . ? N3' U1' Si1' 132.61(11) . . ? N1' U1' Si1' 26.12(13) . . ? Br2' U1' Si1' 70.56(3) . . ? Br1' U1' Si1' 109.67(3) . . ? Si6' U1' Si1' 157.29(4) . . ? Si3' U1' Si1' 109.41(4) . . ? Si4' U1' Si1' 88.21(4) . . ? Si2' U1' Si1' 52.41(5) . . ? N1' Si1' C1' 112.0(3) . . ? N1' Si1' C2' 112.7(3) . . ? C1' Si1' C2' 103.7(3) . . ? N1' Si1' C3' 111.3(3) . . ? C1' Si1' C3' 108.4(3) . . ? C2' Si1' C3' 108.4(3) . . ? N1' Si1' U1' 32.36(14) . . ? C1' Si1' U1' 133.4(3) . . ? C2' Si1' U1' 82.4(2) . . ? C3' Si1' U1' 113.2(2) . . ? N1' Si2' C4' 111.2(3) . . ? N1' Si2' C6' 111.1(3) . . ? C4' Si2' C6' 107.8(3) . . ? N1' Si2' C5' 112.6(3) . . ? C4' Si2' C5' 109.2(3) . . ? C6' Si2' C5' 104.5(3) . . ? N1' Si2' U1' 32.48(15) . . ? C4' Si2' U1' 112.5(2) . . ? C6' Si2' U1' 133.9(2) . . ? C5' Si2' U1' 82.6(2) . . ? N2' Si3' C8' 111.8(3) . . ? N2' Si3' C7' 109.9(3) . . ? C8' Si3' C7' 109.8(3) . . ? N2' Si3' C9' 112.0(2) . . ? C8' Si3' C9' 107.9(3) . . ? C7' Si3' C9' 105.1(3) . . ? N2' Si3' U1' 32.28(13) . . ? C8' Si3' U1' 114.1(2) . . ? C7' Si3' U1' 130.9(3) . . ? C9' Si3' U1' 81.55(18) . . ? N2' Si4' C12' 110.8(3) . . ? N2' Si4' C11' 111.3(2) . . ? C12' Si4' C11' 108.9(3) . . ? N2' Si4' C10' 112.0(2) . . ? C12' Si4' C10' 105.1(3) . . ? C11' Si4' C10' 108.5(3) . . ? N2' Si4' U1' 32.28(13) . . ? C12' Si4' U1' 132.8(2) . . ? C11' Si4' U1' 112.8(2) . . ? C10' Si4' U1' 81.92(19) . . ? N3' Si5' C14' 112.1(3) . . ? N3' Si5' C13' 110.4(2) . . ? C14' Si5' C13' 108.2(3) . . ? N3' Si5' C15' 112.7(2) . . ? C14' Si5' C15' 103.1(3) . . ? C13' Si5' C15' 110.1(3) . . ? N3' Si6' C18' 110.8(3) . . ? N3' Si6' C16' 111.0(2) . . ? C18' Si6' C16' 109.6(3) . . ? N3' Si6' C17' 112.0(3) . . ? C18' Si6' C17' 108.4(3) . . ? C16' Si6' C17' 104.8(3) . . ? N3' Si6' U1' 32.90(13) . . ? C18' Si6' U1' 114.0(2) . . ? C16' Si6' U1' 79.85(18) . . ? C17' Si6' U1' 132.9(2) . . ? Si1' N1' Si2' 117.2(2) . . ? Si1' N1' U1' 121.5(2) . . ? Si2' N1' U1' 121.2(2) . . ? Si3' N2' Si4' 117.0(2) . . ? Si3' N2' U1' 121.6(2) . . ? Si4' N2' U1' 121.4(2) . . ? Si6' N3' Si5' 116.5(2) . . ? Si6' N3' U1' 120.5(2) . . ? Si5' N3' U1' 123.0(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.000 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.127 #===END data_UP4083(Cmpd5) _database_code_depnum_ccdc_archive 'CCDC 870193' #TrackingRef '- U(V)X2.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Cl F N3 Si6 U' _chemical_formula_weight 773.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.8481(6) _cell_length_b 12.5048(5) _cell_length_c 22.9076(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3393.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 5.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.5499 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 119534 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7818 _reflns_number_gt 7218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0160P)^2^+0.5566P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(3) _refine_ls_number_reflns 7818 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0394 _refine_ls_wR_factor_gt 0.0379 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.778917(9) 0.557773(8) 0.620743(5) 0.02277(3) Uani 1 1 d . A . F1 F 0.6941(19) 0.6421(19) 0.5538(12) 0.069(2) Uani 0.598(6) 1 d P A 1 Cl1 Cl 0.88416(18) 0.45574(16) 0.69954(10) 0.0430(6) Uani 0.598(6) 1 d P A 1 Cl1' Cl 0.6786(13) 0.6572(13) 0.5482(9) 0.069(2) Uani 0.402(6) 1 d P A 2 F1' F 0.8549(7) 0.4765(6) 0.6831(4) 0.0430(6) Uani 0.402(6) 1 d P A 2 Si1 Si 1.02505(9) 0.68780(8) 0.65186(6) 0.0472(3) Uani 1 1 d . A . Si2 Si 0.81547(8) 0.82750(7) 0.63998(5) 0.0392(2) Uani 1 1 d . A . Si3 Si 0.83670(8) 0.30166(7) 0.57202(4) 0.0314(2) Uani 1 1 d . . . Si4 Si 0.87576(10) 0.48287(8) 0.48650(5) 0.0403(3) Uani 1 1 d . A . Si5 Si 0.49663(7) 0.49858(7) 0.62639(5) 0.0314(2) Uani 1 1 d . A . Si6 Si 0.61386(9) 0.53704(7) 0.74295(4) 0.0339(2) Uani 1 1 d . A . N1 N 0.8785(2) 0.7006(2) 0.63882(12) 0.0311(6) Uani 1 1 d . A . N2 N 0.8340(2) 0.4403(2) 0.55684(10) 0.0274(5) Uani 1 1 d . A . N3 N 0.6208(2) 0.52944(18) 0.66622(11) 0.0254(6) Uani 1 1 d . A . C1 C 1.0807(3) 0.5597(3) 0.6205(2) 0.0675(12) Uani 1 1 d . . . H1A H 1.0292 0.5026 0.6291 0.101 Uiso 1 1 calc R A . H1B H 1.1530 0.5441 0.6373 0.101 Uiso 1 1 calc R . . H1C H 1.0883 0.5669 0.5789 0.101 Uiso 1 1 calc R . . C2 C 1.1056(3) 0.7970(3) 0.6146(3) 0.0764(15) Uani 1 1 d . . . H2A H 1.0911 0.7944 0.5734 0.115 Uiso 1 1 calc R A . H2B H 1.1848 0.7875 0.6216 0.115 Uiso 1 1 calc R . . H2C H 1.0820 0.8650 0.6298 0.115 Uiso 1 1 calc R . . C3 C 1.0571(4) 0.6886(4) 0.7311(2) 0.0740(15) Uani 1 1 d . . . H3A H 1.0365 0.7565 0.7474 0.111 Uiso 1 1 calc R A . H3B H 1.1364 0.6767 0.7368 0.111 Uiso 1 1 calc R . . H3C H 1.0151 0.6329 0.7500 0.111 Uiso 1 1 calc R . . C4 C 0.8382(4) 0.8992(3) 0.5698(2) 0.0721(15) Uani 1 1 d . . . H4A H 0.9167 0.9166 0.5657 0.108 Uiso 1 1 calc R A . H4B H 0.7943 0.9638 0.5695 0.108 Uiso 1 1 calc R . . H4C H 0.8152 0.8543 0.5380 0.108 Uiso 1 1 calc R . . C5 C 0.8692(4) 0.9095(3) 0.7023(2) 0.0767(16) Uani 1 1 d . . . H5A H 0.8577 0.8714 0.7382 0.115 Uiso 1 1 calc R A . H5B H 0.8292 0.9763 0.7037 0.115 Uiso 1 1 calc R . . H5C H 0.9483 0.9231 0.6971 0.115 Uiso 1 1 calc R . . C6 C 0.6591(3) 0.8195(3) 0.65180(18) 0.0495(10) Uani 1 1 d . . . H6A H 0.6254 0.7782 0.6211 0.074 Uiso 1 1 calc R A . H6B H 0.6277 0.8903 0.6517 0.074 Uiso 1 1 calc R . . H6C H 0.6441 0.7860 0.6887 0.074 Uiso 1 1 calc R . . C7 C 0.9812(3) 0.2573(3) 0.59345(19) 0.0505(10) Uani 1 1 d . A . H7A H 1.0319 0.2674 0.5612 0.076 Uiso 1 1 calc R . . H7B H 0.9794 0.1830 0.6039 0.076 Uiso 1 1 calc R . . H7C H 1.0066 0.2987 0.6262 0.076 Uiso 1 1 calc R . . C8 C 0.7878(3) 0.2233(3) 0.50724(15) 0.0435(9) Uani 1 1 d . A . H8A H 0.7121 0.2441 0.4974 0.065 Uiso 1 1 calc R . . H8B H 0.7894 0.1484 0.5163 0.065 Uiso 1 1 calc R . . H8C H 0.8367 0.2373 0.4747 0.065 Uiso 1 1 calc R . . C9 C 0.7369(3) 0.2654(3) 0.63256(14) 0.0388(8) Uani 1 1 d . A . H9A H 0.7662 0.2913 0.6690 0.058 Uiso 1 1 calc R . . H9B H 0.7289 0.1891 0.6343 0.058 Uiso 1 1 calc R . . H9C H 0.6646 0.2974 0.6253 0.058 Uiso 1 1 calc R . . C10 C 0.9142(4) 0.6277(3) 0.48574(19) 0.0613(14) Uani 1 1 d . . . H10A H 0.9681 0.6418 0.5161 0.092 Uiso 1 1 calc R A . H10B H 0.8478 0.6700 0.4922 0.092 Uiso 1 1 calc R . . H10C H 0.9465 0.6457 0.4486 0.092 Uiso 1 1 calc R . . C11 C 1.0066(4) 0.4126(3) 0.4615(2) 0.0640(13) Uani 1 1 d . . . H11A H 1.0659 0.4240 0.4893 0.096 Uiso 1 1 calc R A . H11B H 1.0291 0.4404 0.4242 0.096 Uiso 1 1 calc R . . H11C H 0.9918 0.3374 0.4581 0.096 Uiso 1 1 calc R . . C12 C 0.7607(4) 0.4636(3) 0.43253(15) 0.0589(12) Uani 1 1 d . . . H12A H 0.7492 0.3885 0.4261 0.088 Uiso 1 1 calc R A . H12B H 0.7811 0.4974 0.3964 0.088 Uiso 1 1 calc R . . H12C H 0.6924 0.4950 0.4472 0.088 Uiso 1 1 calc R . . C13 C 0.5321(3) 0.4468(4) 0.55213(15) 0.0475(9) Uani 1 1 d . . . H13A H 0.5652 0.5030 0.5293 0.071 Uiso 1 1 calc R A . H13B H 0.4645 0.4220 0.5333 0.071 Uiso 1 1 calc R . . H13C H 0.5846 0.3887 0.5556 0.071 Uiso 1 1 calc R . . C14 C 0.4117(3) 0.3904(3) 0.66178(18) 0.0492(10) Uani 1 1 d . . . H14A H 0.4546 0.3252 0.6622 0.074 Uiso 1 1 calc R A . H14B H 0.3432 0.3796 0.6402 0.074 Uiso 1 1 calc R . . H14C H 0.3938 0.4107 0.7011 0.074 Uiso 1 1 calc R . . C15 C 0.4080(3) 0.6198(3) 0.6167(2) 0.0522(10) Uani 1 1 d . . . H15A H 0.3862 0.6469 0.6543 0.078 Uiso 1 1 calc R A . H15B H 0.3417 0.6018 0.5947 0.078 Uiso 1 1 calc R . . H15C H 0.4503 0.6734 0.5962 0.078 Uiso 1 1 calc R . . C16 C 0.6278(3) 0.4014(3) 0.77644(15) 0.0405(9) Uani 1 1 d . . . H16A H 0.5733 0.3540 0.7593 0.061 Uiso 1 1 calc R A . H16B H 0.6149 0.4062 0.8177 0.061 Uiso 1 1 calc R . . H16C H 0.7024 0.3743 0.7695 0.061 Uiso 1 1 calc R . . C17 C 0.4776(4) 0.5976(3) 0.76810(19) 0.0565(12) Uani 1 1 d . . . H17A H 0.4680 0.6664 0.7502 0.085 Uiso 1 1 calc R A . H17B H 0.4790 0.6056 0.8098 0.085 Uiso 1 1 calc R . . H17C H 0.4161 0.5518 0.7572 0.085 Uiso 1 1 calc R . . C18 C 0.7269(4) 0.6267(3) 0.77155(15) 0.0528(10) Uani 1 1 d . . . H18A H 0.7960 0.5871 0.7752 0.079 Uiso 1 1 calc R A . H18B H 0.7050 0.6538 0.8091 0.079 Uiso 1 1 calc R . . H18C H 0.7378 0.6853 0.7450 0.079 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 U1 0.02392(5) 0.02102(5) 0.02337(5) 0.00201(5) 0.00044(5) -0.00054(5) F1 0.058(4) 0.067(4) 0.083(3) -0.032(3) 0.024(3) -0.011(3) Cl1 0.0451(12) 0.0388(10) 0.0450(12) 0.0036(8) -0.0114(7) -0.0006(8) Cl1' 0.058(4) 0.067(4) 0.083(3) -0.032(3) 0.024(3) -0.011(3) F1' 0.0451(12) 0.0388(10) 0.0450(12) 0.0036(8) -0.0114(7) -0.0006(8) Si1 0.0324(6) 0.0357(5) 0.0734(8) 0.0053(5) -0.0125(5) -0.0089(4) Si2 0.0458(6) 0.0227(4) 0.0492(6) 0.0047(4) 0.0002(4) -0.0026(4) Si3 0.0356(5) 0.0239(4) 0.0346(5) 0.0033(4) 0.0069(4) 0.0057(4) Si4 0.0551(7) 0.0338(5) 0.0320(6) 0.0060(4) 0.0185(5) 0.0080(5) Si5 0.0246(4) 0.0294(4) 0.0403(6) 0.0073(4) 0.0007(4) -0.0017(3) Si6 0.0518(6) 0.0254(5) 0.0244(5) 0.0022(4) 0.0109(4) -0.0025(4) N1 0.0312(14) 0.0252(13) 0.0368(16) 0.0062(11) -0.0025(12) -0.0055(11) N2 0.0308(13) 0.0248(12) 0.0267(13) 0.0065(13) 0.0053(10) 0.0035(13) N3 0.0295(14) 0.0213(13) 0.0255(14) 0.0025(10) 0.0028(11) 0.0008(10) C1 0.0242(17) 0.061(2) 0.118(4) -0.010(4) 0.001(2) 0.0012(19) C2 0.045(2) 0.057(3) 0.127(4) 0.005(3) 0.001(3) -0.020(2) C3 0.072(3) 0.056(3) 0.093(4) -0.001(3) -0.050(3) -0.003(2) C4 0.087(4) 0.046(2) 0.083(4) 0.037(2) 0.024(3) 0.014(2) C5 0.082(4) 0.041(3) 0.107(4) -0.028(3) -0.022(3) -0.004(2) C6 0.054(2) 0.034(2) 0.061(3) -0.0023(19) 0.009(2) 0.0059(19) C7 0.043(2) 0.042(2) 0.066(3) 0.0140(19) 0.008(2) 0.0150(17) C8 0.049(2) 0.0316(17) 0.049(2) -0.0052(15) 0.007(2) 0.0043(18) C9 0.043(2) 0.0299(16) 0.043(2) 0.0052(14) 0.0090(17) -0.0001(14) C10 0.092(4) 0.040(2) 0.052(3) 0.011(2) 0.029(3) -0.003(2) C11 0.074(3) 0.056(3) 0.062(3) 0.011(2) 0.043(2) 0.014(2) C12 0.094(3) 0.055(3) 0.0276(18) 0.0050(16) 0.0069(19) 0.016(2) C13 0.044(2) 0.058(2) 0.041(2) -0.001(2) -0.0123(16) -0.012(2) C14 0.043(2) 0.045(2) 0.059(3) 0.0106(19) 0.0042(19) -0.0136(18) C15 0.0304(19) 0.050(2) 0.077(3) 0.016(2) -0.004(2) 0.0051(16) C16 0.063(3) 0.0335(18) 0.0251(18) 0.0068(14) 0.0049(17) 0.0002(17) C17 0.079(3) 0.038(2) 0.052(3) 0.0006(18) 0.037(2) 0.010(2) C18 0.084(3) 0.044(2) 0.0304(19) -0.0014(15) 0.002(2) -0.015(2) 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 U1 F1' 1.971(8) . ? U1 F1 2.11(3) . ? U1 N3 2.173(2) . ? U1 N2 2.174(3) . ? U1 N1 2.180(2) . ? U1 Cl1' 2.391(19) . ? U1 Cl1 2.538(2) . ? U1 Si4 3.4134(10) . ? U1 Si1 3.4141(10) . ? U1 Si6 3.4248(9) . ? U1 Si5 3.4279(8) . ? U1 Si2 3.4291(10) . ? Si1 N1 1.769(3) . ? Si1 C3 1.853(5) . ? Si1 C2 1.871(4) . ? Si1 C1 1.875(4) . ? Si2 N1 1.754(3) . ? Si2 C4 1.861(4) . ? Si2 C5 1.870(4) . ? Si2 C6 1.875(4) . ? Si3 N2 1.768(3) . ? Si3 C7 1.865(4) . ? Si3 C8 1.870(4) . ? Si3 C9 1.878(3) . ? Si4 N2 1.768(2) . ? Si4 C12 1.856(4) . ? Si4 C10 1.867(4) . ? Si4 C11 1.871(4) . ? Si5 N3 1.773(3) . ? Si5 C15 1.858(3) . ? Si5 C13 1.868(4) . ? Si5 C14 1.871(4) . ? Si6 N3 1.762(3) . ? Si6 C18 1.865(4) . ? Si6 C16 1.869(3) . ? Si6 C17 1.874(4) . ? 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 F1' U1 F1 178.5(7) . . ? F1' U1 N3 87.9(2) . . ? F1 U1 N3 91.1(6) . . ? F1' U1 N2 90.1(2) . . ? F1 U1 N2 89.5(6) . . ? N3 U1 N2 118.14(9) . . ? F1' U1 N1 92.2(2) . . ? F1 U1 N1 89.2(7) . . ? N3 U1 N1 120.60(9) . . ? N2 U1 N1 121.26(10) . . ? F1' U1 Cl1' 177.1(4) . . ? F1 U1 Cl1' 2.5(10) . . ? N3 U1 Cl1' 89.4(4) . . ? N2 U1 Cl1' 91.9(4) . . ? N1 U1 Cl1' 88.6(4) . . ? F1' U1 Cl1 2.2(3) . . ? F1 U1 Cl1 178.8(6) . . ? N3 U1 Cl1 90.04(8) . . ? N2 U1 Cl1 89.52(8) . . ? N1 U1 Cl1 90.63(8) . . ? Cl1' U1 Cl1 178.6(4) . . ? F1' U1 Si4 111.0(2) . . ? F1 U1 Si4 69.1(6) . . ? N3 U1 Si4 132.62(7) . . ? N2 U1 Si4 26.76(7) . . ? N1 U1 Si4 102.36(7) . . ? Cl1' U1 Si4 71.6(4) . . ? Cl1 U1 Si4 109.74(5) . . ? F1' U1 Si1 72.8(2) . . ? F1 U1 Si1 108.7(7) . . ? N3 U1 Si1 135.57(7) . . ? N2 U1 Si1 101.87(7) . . ? N1 U1 Si1 26.88(7) . . ? Cl1' U1 Si1 108.8(4) . . ? Cl1 U1 Si1 70.81(5) . . ? Si4 U1 Si1 91.82(3) . . ? F1' U1 Si6 68.3(2) . . ? F1 U1 Si6 111.0(6) . . ? N3 U1 Si6 26.28(7) . . ? N2 U1 Si6 132.12(7) . . ? N1 U1 Si6 102.46(7) . . ? Cl1' U1 Si6 108.9(4) . . ? Cl1 U1 Si6 70.19(5) . . ? Si4 U1 Si6 155.18(3) . . ? Si1 U1 Si6 110.68(3) . . ? F1' U1 Si5 107.9(2) . . ? F1 U1 Si5 70.8(7) . . ? N3 U1 Si5 26.54(7) . . ? N2 U1 Si5 99.94(7) . . ? N1 U1 Si5 134.24(7) . . ? Cl1' U1 Si5 69.7(4) . . ? Cl1 U1 Si5 110.12(5) . . ? Si4 U1 Si5 107.62(3) . . ? Si1 U1 Si5 158.18(3) . . ? Si6 U1 Si5 52.82(3) . . ? F1' U1 Si2 110.9(2) . . ? F1 U1 Si2 70.3(6) . . ? N3 U1 Si2 101.98(6) . . ? N2 U1 Si2 135.50(7) . . ? N1 U1 Si2 26.03(7) . . ? Cl1' U1 Si2 68.9(4) . . ? Cl1 U1 Si2 109.94(5) . . ? Si4 U1 Si2 110.08(2) . . ? Si1 U1 Si2 52.90(3) . . ? Si6 U1 Si2 92.38(2) . . ? Si5 U1 Si2 109.32(2) . . ? N1 Si1 C3 111.46(19) . . ? N1 Si1 C2 110.92(17) . . ? C3 Si1 C2 109.8(2) . . ? N1 Si1 C1 110.97(15) . . ? C3 Si1 C1 107.9(2) . . ? C2 Si1 C1 105.6(2) . . ? N1 Si1 U1 33.86(8) . . ? C3 Si1 U1 112.45(16) . . ? C2 Si1 U1 133.44(17) . . ? C1 Si1 U1 79.26(11) . . ? N1 Si2 C4 111.19(18) . . ? N1 Si2 C5 111.28(18) . . ? C4 Si2 C5 110.3(2) . . ? N1 Si2 C6 112.00(16) . . ? C4 Si2 C6 107.1(2) . . ? C5 Si2 C6 104.8(2) . . ? N1 Si2 U1 33.06(9) . . ? C4 Si2 U1 112.41(16) . . ? C5 Si2 U1 132.91(16) . . ? C6 Si2 U1 80.86(12) . . ? N2 Si3 C7 111.07(16) . . ? N2 Si3 C8 110.60(14) . . ? C7 Si3 C8 109.73(18) . . ? N2 Si3 C9 111.75(13) . . ? C7 Si3 C9 108.17(17) . . ? C8 Si3 C9 105.34(16) . . ? N2 Si3 U1 32.06(8) . . ? C7 Si3 U1 111.83(14) . . ? C8 Si3 U1 132.80(12) . . ? C9 Si3 U1 81.98(10) . . ? N2 Si4 C12 111.28(16) . . ? N2 Si4 C10 111.65(17) . . ? C12 Si4 C10 107.4(2) . . ? N2 Si4 C11 111.68(17) . . ? C12 Si4 C11 110.1(2) . . ? C10 Si4 C11 104.5(2) . . ? N2 Si4 U1 33.63(9) . . ? C12 Si4 U1 112.89(13) . . ? C10 Si4 U1 79.88(13) . . ? C11 Si4 U1 133.10(16) . . ? N3 Si5 C15 110.64(16) . . ? N3 Si5 C13 110.95(14) . . ? C15 Si5 C13 107.6(2) . . ? N3 Si5 C14 112.37(16) . . ? C15 Si5 C14 109.75(18) . . ? C13 Si5 C14 105.35(19) . . ? N3 Si5 U1 33.19(8) . . ? C15 Si5 U1 111.76(12) . . ? C13 Si5 U1 79.70(11) . . ? C14 Si5 U1 134.20(13) . . ? N3 Si6 C18 110.45(15) . . ? N3 Si6 C16 110.87(14) . . ? C18 Si6 C16 109.74(18) . . ? N3 Si6 C17 111.63(18) . . ? C18 Si6 C17 105.5(2) . . ? C16 Si6 C17 108.47(17) . . ? N3 Si6 U1 33.08(8) . . ? C18 Si6 U1 80.31(12) . . ? C16 Si6 U1 110.71(12) . . ? C17 Si6 U1 135.45(14) . . ? Si2 N1 Si1 119.82(15) . . ? Si2 N1 U1 120.91(14) . . ? Si1 N1 U1 119.26(14) . . ? Si4 N2 Si3 118.01(15) . . ? Si4 N2 U1 119.61(15) . . ? Si3 N2 U1 122.37(12) . . ? Si6 N3 Si5 119.10(15) . . ? Si6 N3 U1 120.64(13) . . ? Si5 N3 U1 120.27(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.622 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.071 #===END data_UP4166(Cmpd7) _database_code_depnum_ccdc_archive 'CCDC 870194' #TrackingRef '- U(V)X2.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H54 N5 S2 Si6 U' _chemical_formula_weight 835.37 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1020(3) _cell_length_b 15.1440(4) _cell_length_c 20.9071(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.1240(10) _cell_angle_gamma 90.00 _cell_volume 3831.69(17) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 4.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.5665 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 72576 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8785 _reflns_number_gt 7500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0944P)^2^+48.8851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8785 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.75198(2) 0.25990(2) 0.083697(14) 0.02764(12) Uani 1 1 d . . . S1 S 0.7324(3) 0.5937(2) 0.0687(2) 0.0729(10) Uani 1 1 d . . . S2 S 0.7693(4) -0.0726(2) 0.0934(2) 0.0800(11) Uani 1 1 d . . . Si1 Si 0.8754(3) 0.2075(2) 0.22672(14) 0.0508(7) Uani 1 1 d . . . Si2 Si 0.9785(2) 0.3596(2) 0.15054(14) 0.0476(7) Uani 1 1 d . . . Si3 Si 0.9122(3) 0.1904(2) -0.04139(14) 0.0502(7) Uani 1 1 d . . . Si4 Si 0.7293(2) 0.3214(2) -0.07317(13) 0.0430(6) Uani 1 1 d . . . Si5 Si 0.4942(3) 0.1686(2) 0.07469(15) 0.0524(7) Uani 1 1 d . . . Si6 Si 0.5225(2) 0.3268(2) 0.16354(14) 0.0513(7) Uani 1 1 d . . . N1 N 0.8751(6) 0.2722(6) 0.1580(4) 0.0352(16) Uani 1 1 d . . . N2 N 0.7997(7) 0.2555(5) -0.0151(4) 0.0339(16) Uani 1 1 d . . . N3 N 0.5795(7) 0.2498(5) 0.1081(4) 0.0369(18) Uani 1 1 d . . . N4 N 0.7367(7) 0.4120(6) 0.0788(4) 0.045(2) Uani 1 1 d . . . N5 N 0.7675(8) 0.1075(6) 0.0899(4) 0.049(2) Uani 1 1 d . . . C1 C 0.7332(11) 0.1559(11) 0.2392(7) 0.077(4) Uani 1 1 d . . . H1A H 0.6797 0.2017 0.2462 0.116 Uiso 1 1 calc R . . H1B H 0.7354 0.1175 0.2757 0.116 Uiso 1 1 calc R . . H1C H 0.7129 0.1226 0.2019 0.116 Uiso 1 1 calc R . . C2 C 0.9045(10) 0.2726(10) 0.3002(5) 0.057(3) Uani 1 1 d . . . H2A H 0.9736 0.3030 0.2955 0.086 Uiso 1 1 calc R . . H2B H 0.9086 0.2336 0.3363 0.086 Uiso 1 1 calc R . . H2C H 0.8465 0.3148 0.3068 0.086 Uiso 1 1 calc R . . C3 C 0.9785(11) 0.1156(11) 0.2172(7) 0.077(4) Uani 1 1 d . . . H3A H 0.9647 0.0850 0.1778 0.116 Uiso 1 1 calc R . . H3B H 0.9717 0.0751 0.2523 0.116 Uiso 1 1 calc R . . H3C H 1.0519 0.1397 0.2167 0.116 Uiso 1 1 calc R . . C4 C 1.1160(9) 0.3166(11) 0.1763(6) 0.069(4) Uani 1 1 d . . . H4A H 1.1195 0.3153 0.2221 0.104 Uiso 1 1 calc R . . H4B H 1.1731 0.3544 0.1601 0.104 Uiso 1 1 calc R . . H4C H 1.1260 0.2580 0.1598 0.104 Uiso 1 1 calc R . . C5 C 0.9939(10) 0.3933(9) 0.0643(6) 0.059(3) Uani 1 1 d . . . H5A H 0.9409 0.3619 0.0386 0.088 Uiso 1 1 calc R . . H5B H 1.0671 0.3795 0.0499 0.088 Uiso 1 1 calc R . . H5C H 0.9814 0.4557 0.0603 0.088 Uiso 1 1 calc R . . C6 C 0.9423(11) 0.4573(9) 0.1993(6) 0.068(3) Uani 1 1 d . . . H6A H 0.8747 0.4824 0.1837 0.101 Uiso 1 1 calc R . . H6B H 1.0004 0.5002 0.1964 0.101 Uiso 1 1 calc R . . H6C H 0.9331 0.4398 0.2431 0.101 Uiso 1 1 calc R . . C7 C 0.8595(13) 0.0837(9) -0.0770(6) 0.070(4) Uani 1 1 d . . . H7A H 0.8406 0.0435 -0.0432 0.105 Uiso 1 1 calc R . . H7B H 0.9160 0.0579 -0.1032 0.105 Uiso 1 1 calc R . . H7C H 0.7952 0.0954 -0.1026 0.105 Uiso 1 1 calc R . . C8 C 1.0059(10) 0.1621(10) 0.0290(6) 0.070(4) Uani 1 1 d . . . H8A H 1.0164 0.2136 0.0551 0.104 Uiso 1 1 calc R . . H8B H 1.0761 0.1422 0.0133 0.104 Uiso 1 1 calc R . . H8C H 0.9725 0.1163 0.0541 0.104 Uiso 1 1 calc R . . C9 C 1.0002(10) 0.2520(9) -0.1004(6) 0.061(4) Uani 1 1 d . . . H9A H 0.9561 0.2685 -0.1367 0.091 Uiso 1 1 calc R . . H9B H 1.0599 0.2148 -0.1142 0.091 Uiso 1 1 calc R . . H9C H 1.0296 0.3041 -0.0805 0.091 Uiso 1 1 calc R . . C10 C 0.7072(12) 0.2555(10) -0.1487(6) 0.069(4) Uani 1 1 d . . . H10A H 0.7728 0.2576 -0.1744 0.103 Uiso 1 1 calc R . . H10B H 0.6463 0.2800 -0.1723 0.103 Uiso 1 1 calc R . . H10C H 0.6911 0.1952 -0.1378 0.103 Uiso 1 1 calc R . . C11 C 0.8088(10) 0.4232(8) -0.0908(6) 0.057(3) Uani 1 1 d . . . H11A H 0.8101 0.4602 -0.0535 0.085 Uiso 1 1 calc R . . H11B H 0.7744 0.4542 -0.1255 0.085 Uiso 1 1 calc R . . H11C H 0.8830 0.4077 -0.1024 0.085 Uiso 1 1 calc R . . C12 C 0.5875(10) 0.3533(9) -0.0446(6) 0.062(3) Uani 1 1 d . . . H12A H 0.5504 0.3020 -0.0283 0.093 Uiso 1 1 calc R . . H12B H 0.5459 0.3775 -0.0796 0.093 Uiso 1 1 calc R . . H12C H 0.5940 0.3967 -0.0113 0.093 Uiso 1 1 calc R . . C13 C 0.5541(10) 0.1231(9) -0.0017(6) 0.062(3) Uani 1 1 d . . . H13A H 0.6106 0.1622 -0.0170 0.092 Uiso 1 1 calc R . . H13B H 0.4968 0.1182 -0.0333 0.092 Uiso 1 1 calc R . . H13C H 0.5853 0.0659 0.0064 0.092 Uiso 1 1 calc R . . C14 C 0.3571(9) 0.2165(10) 0.0525(6) 0.060(3) Uani 1 1 d . . . H14A H 0.3139 0.2254 0.0904 0.089 Uiso 1 1 calc R . . H14B H 0.3190 0.1766 0.0243 0.089 Uiso 1 1 calc R . . H14C H 0.3678 0.2720 0.0312 0.089 Uiso 1 1 calc R . . C15 C 0.4774(11) 0.0715(9) 0.1316(6) 0.065(3) Uani 1 1 d . . . H15A H 0.5466 0.0410 0.1358 0.097 Uiso 1 1 calc R . . H15B H 0.4226 0.0317 0.1150 0.097 Uiso 1 1 calc R . . H15C H 0.4544 0.0927 0.1728 0.097 Uiso 1 1 calc R . . C16 C 0.4227(11) 0.2685(11) 0.2191(7) 0.073(4) Uani 1 1 d . . . H16A H 0.3555 0.2556 0.1965 0.109 Uiso 1 1 calc R . . H16B H 0.4067 0.3059 0.2550 0.109 Uiso 1 1 calc R . . H16C H 0.4553 0.2145 0.2340 0.109 Uiso 1 1 calc R . . C17 C 0.4475(11) 0.4159(9) 0.1215(7) 0.066(4) Uani 1 1 d . . . H17A H 0.4993 0.4524 0.0990 0.099 Uiso 1 1 calc R . . H17B H 0.4079 0.4510 0.1520 0.099 Uiso 1 1 calc R . . H17C H 0.3963 0.3905 0.0916 0.099 Uiso 1 1 calc R . . C18 C 0.6311(11) 0.3782(10) 0.2165(6) 0.070(4) Uani 1 1 d . . . H18A H 0.6740 0.3325 0.2365 0.104 Uiso 1 1 calc R . . H18B H 0.5960 0.4134 0.2488 0.104 Uiso 1 1 calc R . . H18C H 0.6787 0.4149 0.1912 0.104 Uiso 1 1 calc R . . C19 C 0.7347(8) 0.4892(7) 0.0747(5) 0.045(2) Uani 1 1 d . . . C20 C 0.7690(10) 0.0312(8) 0.0906(5) 0.050(3) 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 U1 0.02302(17) 0.03793(19) 0.02197(17) 0.00105(11) -0.00054(11) 0.00382(11) S1 0.079(2) 0.0432(16) 0.096(3) -0.0036(16) -0.001(2) 0.0052(15) S2 0.107(3) 0.0424(16) 0.090(3) 0.0082(16) 0.012(2) 0.0071(17) Si1 0.0433(15) 0.070(2) 0.0395(15) 0.0138(14) -0.0024(12) 0.0090(14) Si2 0.0373(14) 0.0676(19) 0.0378(14) -0.0016(13) -0.0018(11) -0.0059(13) Si3 0.0464(16) 0.0653(19) 0.0389(15) -0.0079(13) 0.0033(12) 0.0130(14) Si4 0.0371(13) 0.0586(17) 0.0334(13) 0.0074(11) 0.0005(10) 0.0002(12) Si5 0.0443(16) 0.067(2) 0.0463(16) 0.0045(14) 0.0036(13) -0.0135(14) Si6 0.0385(14) 0.075(2) 0.0403(15) -0.0006(14) 0.0056(11) 0.0134(14) N1 0.026(3) 0.057(5) 0.023(3) 0.003(3) -0.001(3) 0.006(3) N2 0.027(4) 0.049(4) 0.025(4) -0.002(3) -0.003(3) 0.003(3) N3 0.025(4) 0.060(5) 0.025(4) 0.001(3) 0.002(3) 0.000(3) N4 0.034(4) 0.057(6) 0.045(5) -0.008(4) -0.004(4) -0.003(4) N5 0.054(5) 0.046(5) 0.047(5) 0.004(4) -0.001(4) -0.003(4) C1 0.067(8) 0.104(11) 0.062(8) 0.038(8) -0.006(6) -0.029(8) C2 0.041(6) 0.111(10) 0.020(4) 0.002(5) -0.008(4) -0.002(6) C3 0.064(8) 0.102(11) 0.065(8) 0.037(8) -0.005(6) 0.030(8) C4 0.031(5) 0.121(12) 0.056(7) 0.006(7) -0.002(5) -0.002(6) C5 0.052(6) 0.072(8) 0.053(7) 0.003(6) 0.010(5) -0.019(6) C6 0.068(8) 0.080(9) 0.055(7) -0.019(6) -0.006(6) -0.020(7) C7 0.091(10) 0.065(8) 0.053(7) -0.024(6) 0.001(7) 0.016(7) C8 0.053(7) 0.092(10) 0.063(8) -0.012(7) -0.004(6) 0.038(7) C9 0.032(5) 0.120(12) 0.031(5) 0.003(5) 0.005(4) 0.007(5) C10 0.049(7) 0.131(14) 0.026(5) -0.009(6) -0.008(5) -0.004(7) C11 0.057(7) 0.062(7) 0.050(6) 0.021(5) 0.006(5) -0.013(5) C12 0.055(7) 0.074(8) 0.056(7) 0.018(6) 0.002(5) 0.017(6) C13 0.056(7) 0.069(8) 0.060(7) -0.017(6) 0.007(6) -0.011(6) C14 0.035(5) 0.091(9) 0.052(7) 0.004(6) 0.003(5) -0.010(6) C15 0.058(7) 0.074(8) 0.063(8) 0.025(6) 0.003(6) -0.015(6) C16 0.040(6) 0.132(13) 0.046(7) 0.009(7) 0.015(5) 0.008(7) C17 0.056(7) 0.075(8) 0.068(8) -0.003(6) 0.005(6) 0.034(6) C18 0.069(8) 0.087(10) 0.053(7) -0.032(7) 0.004(6) 0.016(7) C19 0.042(5) 0.047(6) 0.047(6) -0.004(4) -0.003(4) 0.003(4) C20 0.058(6) 0.045(6) 0.047(6) 0.001(4) 0.005(5) -0.001(5) 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 U1 N2 2.148(8) . ? U1 N3 2.156(8) . ? U1 N1 2.158(7) . ? U1 N4 2.313(10) . ? U1 N5 2.319(9) . ? U1 Si6 3.398(3) . ? U1 Si5 3.417(3) . ? U1 Si4 3.420(3) . ? U1 Si3 3.425(3) . ? U1 Si2 3.425(3) . ? U1 Si1 3.432(3) . ? S1 C19 1.589(11) . ? S2 C20 1.573(12) . ? Si1 N1 1.739(8) . ? Si1 C2 1.858(12) . ? Si1 C3 1.881(14) . ? Si1 C1 1.909(13) . ? Si2 N1 1.829(9) . ? Si2 C6 1.848(13) . ? Si2 C4 1.865(12) . ? Si2 C5 1.884(12) . ? Si3 N2 1.769(8) . ? Si3 C9 1.880(12) . ? Si3 C7 1.889(13) . ? Si3 C8 1.905(13) . ? Si4 N2 1.785(8) . ? Si4 C11 1.854(11) . ? Si4 C12 1.881(12) . ? Si4 C10 1.887(12) . ? Si5 N3 1.749(9) . ? Si5 C14 1.869(13) . ? Si5 C13 1.885(12) . ? Si5 C15 1.903(12) . ? Si6 N3 1.784(9) . ? Si6 C17 1.847(13) . ? Si6 C18 1.885(13) . ? Si6 C16 1.897(13) . ? N4 C19 1.172(14) . ? N5 C20 1.156(15) . ? 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 N2 U1 N3 119.2(3) . . ? N2 U1 N1 120.6(3) . . ? N3 U1 N1 120.2(3) . . ? N2 U1 N4 90.5(3) . . ? N3 U1 N4 90.2(3) . . ? N1 U1 N4 90.1(3) . . ? N2 U1 N5 90.1(3) . . ? N3 U1 N5 89.7(3) . . ? N1 U1 N5 89.4(3) . . ? N4 U1 N5 179.3(3) . . ? N2 U1 Si6 134.7(2) . . ? N3 U1 Si6 27.4(2) . . ? N1 U1 Si6 100.6(2) . . ? N4 U1 Si6 70.1(2) . . ? N5 U1 Si6 109.6(2) . . ? N2 U1 Si5 100.5(2) . . ? N3 U1 Si5 25.8(2) . . ? N1 U1 Si5 134.7(2) . . ? N4 U1 Si5 109.1(2) . . ? N5 U1 Si5 71.0(2) . . ? Si6 U1 Si5 53.18(9) . . ? N2 U1 Si4 26.7(2) . . ? N3 U1 Si4 99.8(2) . . ? N1 U1 Si4 136.1(2) . . ? N4 U1 Si4 71.3(2) . . ? N5 U1 Si4 109.3(2) . . ? Si6 U1 Si4 109.03(7) . . ? Si5 U1 Si4 89.19(7) . . ? N2 U1 Si3 26.1(2) . . ? N3 U1 Si3 135.2(2) . . ? N1 U1 Si3 100.7(2) . . ? N4 U1 Si3 108.5(2) . . ? N5 U1 Si3 72.0(2) . . ? Si6 U1 Si3 158.66(8) . . ? Si5 U1 Si3 110.59(8) . . ? Si4 U1 Si3 52.82(7) . . ? N2 U1 Si2 100.9(2) . . ? N3 U1 Si2 135.2(2) . . ? N1 U1 Si2 28.1(2) . . ? N4 U1 Si2 69.1(2) . . ? N5 U1 Si2 110.6(2) . . ? Si6 U1 Si2 108.80(8) . . ? Si5 U1 Si2 158.54(7) . . ? Si4 U1 Si2 109.50(7) . . ? Si3 U1 Si2 89.62(7) . . ? N2 U1 Si1 135.5(2) . . ? N3 U1 Si1 101.4(2) . . ? N1 U1 Si1 25.1(2) . . ? N4 U1 Si1 107.7(2) . . ? N5 U1 Si1 71.7(2) . . ? Si6 U1 Si1 89.73(7) . . ? Si5 U1 Si1 110.48(8) . . ? Si4 U1 Si1 158.79(7) . . ? Si3 U1 Si1 110.39(8) . . ? Si2 U1 Si1 53.14(8) . . ? N1 Si1 C2 112.6(5) . . ? N1 Si1 C3 109.3(5) . . ? C2 Si1 C3 110.8(6) . . ? N1 Si1 C1 110.1(5) . . ? C2 Si1 C1 105.9(6) . . ? C3 Si1 C1 108.1(8) . . ? N1 Si1 U1 31.8(3) . . ? C2 Si1 U1 132.8(4) . . ? C3 Si1 U1 111.5(5) . . ? C1 Si1 U1 79.8(4) . . ? N1 Si2 C6 111.7(5) . . ? N1 Si2 C4 109.4(6) . . ? C6 Si2 C4 109.4(7) . . ? N1 Si2 C5 110.3(5) . . ? C6 Si2 C5 109.6(6) . . ? C4 Si2 C5 106.3(6) . . ? N1 Si2 U1 33.7(2) . . ? C6 Si2 U1 112.8(4) . . ? C4 Si2 U1 132.6(5) . . ? C5 Si2 U1 79.0(4) . . ? N2 Si3 C9 111.4(5) . . ? N2 Si3 C7 109.9(5) . . ? C9 Si3 C7 110.9(6) . . ? N2 Si3 C8 110.1(5) . . ? C9 Si3 C8 106.3(6) . . ? C7 Si3 C8 108.2(7) . . ? N2 Si3 U1 32.3(3) . . ? C9 Si3 U1 132.2(4) . . ? C7 Si3 U1 111.9(5) . . ? C8 Si3 U1 79.4(4) . . ? N2 Si4 C11 110.6(5) . . ? N2 Si4 C12 111.2(5) . . ? C11 Si4 C12 108.9(6) . . ? N2 Si4 C10 109.9(5) . . ? C11 Si4 C10 110.3(6) . . ? C12 Si4 C10 105.9(6) . . ? N2 Si4 U1 32.8(3) . . ? C11 Si4 U1 112.1(4) . . ? C12 Si4 U1 80.6(4) . . ? C10 Si4 U1 132.0(5) . . ? N3 Si5 C14 110.5(5) . . ? N3 Si5 C13 111.6(5) . . ? C14 Si5 C13 105.9(6) . . ? N3 Si5 C15 110.9(5) . . ? C14 Si5 C15 111.0(6) . . ? C13 Si5 C15 106.8(7) . . ? N3 Si5 U1 32.5(3) . . ? C14 Si5 U1 131.8(4) . . ? C13 Si5 U1 80.9(4) . . ? C15 Si5 U1 112.2(4) . . ? N3 Si6 C17 111.0(5) . . ? N3 Si6 C18 112.4(5) . . ? C17 Si6 C18 108.6(7) . . ? N3 Si6 C16 109.9(6) . . ? C17 Si6 C16 108.6(6) . . ? C18 Si6 C16 106.1(7) . . ? N3 Si6 U1 33.7(3) . . ? C17 Si6 U1 112.7(4) . . ? C18 Si6 U1 80.9(4) . . ? C16 Si6 U1 133.2(5) . . ? Si1 N1 Si2 118.5(4) . . ? Si1 N1 U1 123.1(4) . . ? Si2 N1 U1 118.2(4) . . ? Si3 N2 Si4 117.8(5) . . ? Si3 N2 U1 121.6(4) . . ? Si4 N2 U1 120.5(4) . . ? Si5 N3 Si6 119.4(5) . . ? Si5 N3 U1 121.7(4) . . ? Si6 N3 U1 118.9(4) . . ? C19 N4 U1 176.3(8) . . ? C20 N5 U1 175.5(10) . . ? N4 C19 S1 179.5(11) . . ? N5 C20 S2 178.4(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.541 _refine_diff_density_min -2.138 _refine_diff_density_rms 0.231