# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- p1-2.cif' _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dfsun@sdu.edu.cn _publ_contact_author_name 'Daofeng Sun' _publ_section_title ; Solvent-modulated two luminescent Cd(II) metal-organic frameworks constructed from tetrapodal silicon-based linker ; loop_ _publ_author_name 'Di Sun' 'Daofeng Sun' data_p1 #TrackingRef '- p1-2.cif' _database_code_depnum_ccdc_archive 'CCDC 836455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H52 Cd4 N2 O26 Si2' _chemical_formula_weight 1770.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 15.64840(10) _cell_length_b 15.64840(10) _cell_length_c 36.3862(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8909.98(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8273 _cell_measurement_theta_min 4.984 _cell_measurement_theta_max 49.511 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8949 _exptl_absorpt_correction_T_max 0.9220 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32774 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12795 _reflns_number_gt 10950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 12795 _refine_ls_number_parameters 883 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.002 _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 Cd1 Cd 0.61733(3) 1.00365(3) 0.117760(14) 0.02890(13) Uani 1 1 d . . . Cd2 Cd 0.10461(3) 0.51353(3) 0.111209(14) 0.02766(13) Uani 1 1 d . . . Cd3 Cd 0.00877(3) -0.40102(3) 0.216342(17) 0.03952(15) Uani 1 1 d . . . Cd4 Cd 0.99629(4) 0.55481(4) -0.004037(18) 0.04570(16) Uani 1 1 d . . . Si1 Si 0.60763(10) 0.50662(10) 0.11431(7) 0.0242(4) Uani 1 1 d . . . Si2 Si 0.11038(10) 0.00855(10) 0.11392(7) 0.0230(4) Uani 1 1 d . . . C1 C 0.6985(4) 0.4756(4) 0.0834(2) 0.0284(16) Uani 1 1 d . . . C2 C 0.6862(4) 0.4208(4) 0.05335(19) 0.0354(17) Uani 1 1 d . . . H2A H 0.6312 0.4025 0.0477 0.042 Uiso 1 1 calc R . . C3 C 0.7526(4) 0.3939(5) 0.0323(2) 0.047(2) Uani 1 1 d . . . H3A H 0.7418 0.3573 0.0127 0.056 Uiso 1 1 calc R . . C4 C 0.8325(5) 0.4184(5) 0.0388(2) 0.047(2) Uani 1 1 d . . . H4A H 0.8765 0.4010 0.0233 0.056 Uiso 1 1 calc R . . C5 C 0.8499(4) 0.4710(4) 0.06945(19) 0.0276(15) Uani 1 1 d . . . C6 C 0.7826(4) 0.5004(4) 0.09148(19) 0.0253(14) Uani 1 1 d . . . H6A H 0.7937 0.5362 0.1113 0.030 Uiso 1 1 calc R . . C7 C 0.9405(4) 0.4963(4) 0.0785(2) 0.0313(17) Uani 1 1 d . . . C8 C 0.6412(3) 0.5980(4) 0.14436(19) 0.0226(14) Uani 1 1 d . . . C9 C 0.6884(4) 0.5840(4) 0.1766(2) 0.0355(18) Uani 1 1 d . . . H9A H 0.7026 0.5286 0.1835 0.043 Uiso 1 1 calc R . . C10 C 0.7142(5) 0.6530(5) 0.1982(2) 0.0407(18) Uani 1 1 d . . . H10A H 0.7450 0.6435 0.2196 0.049 Uiso 1 1 calc R . . C11 C 0.6940(4) 0.7345(4) 0.1878(2) 0.0326(17) Uani 1 1 d . . . H11A H 0.7105 0.7801 0.2026 0.039 Uiso 1 1 calc R . . C12 C 0.6489(4) 0.7503(4) 0.1552(2) 0.0283(16) Uani 1 1 d . . . C13 C 0.6235(4) 0.6818(4) 0.13445(19) 0.0241(14) Uani 1 1 d . . . H13A H 0.5933 0.6919 0.1129 0.029 Uiso 1 1 calc R . . C14 C 0.6309(4) 0.8412(4) 0.1436(2) 0.0336(17) Uani 1 1 d . . . C15 C 0.5140(4) 0.5384(4) 0.0846(2) 0.0300(16) Uani 1 1 d . . . C16 C 0.5255(4) 0.5749(4) 0.0498(2) 0.0328(17) Uani 1 1 d . . . H16A H 0.5803 0.5811 0.0403 0.039 Uiso 1 1 calc R . . C17 C 0.4560(5) 0.6015(5) 0.0296(2) 0.044(2) Uani 1 1 d . . . H17A H 0.4649 0.6306 0.0077 0.053 Uiso 1 1 calc R . . C18 C 0.3754(4) 0.5866(5) 0.0409(2) 0.0383(18) Uani 1 1 d . . . H18A H 0.3298 0.6005 0.0257 0.046 Uiso 1 1 calc R . . C19 C 0.3602(4) 0.5508(4) 0.0749(2) 0.0286(16) Uani 1 1 d . . . C20 C 0.4293(4) 0.5277(4) 0.0974(2) 0.0303(16) Uani 1 1 d . . . H20A H 0.4195 0.5054 0.1207 0.036 Uiso 1 1 calc R . . C21 C 0.2710(4) 0.5364(4) 0.0893(2) 0.0327(17) Uani 1 1 d . . . C22 C 0.5798(4) 0.4122(4) 0.14374(19) 0.0251(15) Uani 1 1 d . . . C23 C 0.5413(5) 0.4234(4) 0.1783(2) 0.0445(19) Uani 1 1 d . . . H23A H 0.5300 0.4782 0.1869 0.053 Uiso 1 1 calc R . . C24 C 0.5203(6) 0.3529(5) 0.1997(3) 0.055(2) Uani 1 1 d . . . H24A H 0.4946 0.3612 0.2225 0.067 Uiso 1 1 calc R . . C25 C 0.5366(5) 0.2704(5) 0.1878(2) 0.042(2) Uani 1 1 d . . . H25A H 0.5211 0.2239 0.2023 0.051 Uiso 1 1 calc R . . C26 C 0.5762(4) 0.2582(4) 0.1546(2) 0.0305(16) Uani 1 1 d . . . C27 C 0.5960(4) 0.3299(4) 0.1322(2) 0.0277(15) Uani 1 1 d . . . H27A H 0.6205 0.3212 0.1092 0.033 Uiso 1 1 calc R . . C28 C 0.5948(4) 0.1708(4) 0.1407(2) 0.0340(18) Uani 1 1 d . . . C29 C 0.0837(4) 0.1042(4) 0.14247(18) 0.0223(14) Uani 1 1 d . . . C30 C 0.0952(4) 0.1871(4) 0.1288(2) 0.0283(16) Uani 1 1 d . . . H30A H 0.1149 0.1948 0.1050 0.034 Uiso 1 1 calc R . . C31 C 0.0774(4) 0.2591(4) 0.1508(2) 0.0324(17) Uani 1 1 d . . . C32 C 0.0464(5) 0.2479(4) 0.1860(2) 0.043(2) Uani 1 1 d . . . H32A H 0.0353 0.2952 0.2007 0.051 Uiso 1 1 calc R . . C33 C 0.0316(5) 0.1651(4) 0.1997(2) 0.0398(19) Uani 1 1 d . . . H33A H 0.0086 0.1571 0.2230 0.048 Uiso 1 1 calc R . . C34 C 0.0519(4) 0.0966(4) 0.1778(2) 0.0306(16) Uani 1 1 d . . . H34A H 0.0438 0.0420 0.1873 0.037 Uiso 1 1 calc R . . C35 C 0.0930(5) 0.3465(4) 0.1346(2) 0.0390(19) Uani 1 1 d . . . C36 C 0.2079(4) 0.0310(4) 0.0851(2) 0.0295(16) Uani 1 1 d . . . C37 C 0.2011(4) 0.0699(5) 0.0504(2) 0.0396(19) Uani 1 1 d . . . H37A H 0.1482 0.0868 0.0414 0.048 Uiso 1 1 calc R . . C38 C 0.2754(4) 0.0828(5) 0.0297(2) 0.047(2) Uani 1 1 d . . . H38A H 0.2711 0.1061 0.0063 0.057 Uiso 1 1 calc R . . C39 C 0.3531(4) 0.0622(4) 0.0430(2) 0.0368(17) Uani 1 1 d . . . H39A H 0.4014 0.0714 0.0286 0.044 Uiso 1 1 calc R . . C40 C 0.3618(4) 0.0279(4) 0.0774(2) 0.0280(16) Uani 1 1 d . . . C41 C 0.2864(4) 0.0107(4) 0.09764(19) 0.0269(15) Uani 1 1 d . . . H41A H 0.2913 -0.0156 0.1205 0.032 Uiso 1 1 calc R . . C42 C 0.4486(4) 0.0084(4) 0.0936(2) 0.0312(17) Uani 1 1 d . . . C43 C 0.0189(4) -0.0193(4) 0.08306(19) 0.0264(15) Uani 1 1 d . . . C44 C 0.0316(4) -0.0604(4) 0.0492(2) 0.0342(17) Uani 1 1 d . . . H44A H 0.0869 -0.0725 0.0414 0.041 Uiso 1 1 calc R . . C45 C -0.0382(4) -0.0836(5) 0.0267(2) 0.0412(19) Uani 1 1 d . . . H45A H -0.0295 -0.1120 0.0046 0.049 Uiso 1 1 calc R . . C46 C -0.1217(4) -0.0626(4) 0.0386(2) 0.0391(18) Uani 1 1 d . . . H46A H -0.1683 -0.0741 0.0236 0.047 Uiso 1 1 calc R . . C47 C -0.1342(4) -0.0247(4) 0.0729(2) 0.0276(16) Uani 1 1 d . . . C48 C -0.0658(4) -0.0053(4) 0.0945(2) 0.0269(15) Uani 1 1 d . . . H48A H -0.0754 0.0179 0.1177 0.032 Uiso 1 1 calc R . . C49 C -0.2242(4) -0.0083(4) 0.0860(2) 0.0304(16) Uani 1 1 d . . . C50 C 0.1332(4) -0.0844(3) 0.14464(17) 0.0190(13) Uani 1 1 d . . . C51 C 0.1804(4) -0.0745(4) 0.17719(19) 0.0273(15) Uani 1 1 d . . . H51A H 0.2003 -0.0207 0.1838 0.033 Uiso 1 1 calc R . . C52 C 0.1983(4) -0.1467(4) 0.2003(2) 0.0325(16) Uani 1 1 d . . . H52A H 0.2272 -0.1396 0.2224 0.039 Uiso 1 1 calc R . . C53 C 0.1726(4) -0.2247(4) 0.18940(19) 0.0284(15) Uani 1 1 d . . . H53A H 0.1854 -0.2714 0.2042 0.034 Uiso 1 1 calc R . . C54 C 0.1286(4) -0.2385(3) 0.1575(2) 0.0264(15) Uani 1 1 d . . . C55 C 0.1080(4) -0.1661(4) 0.1345(2) 0.0282(16) Uani 1 1 d . . . H55A H 0.0778 -0.1742 0.1128 0.034 Uiso 1 1 calc R . . C56 C 0.1050(4) -0.3270(4) 0.1437(2) 0.0262(15) Uani 1 1 d . . . C57 C 0.8181(10) 0.5581(11) -0.0528(5) 0.136(6) Uani 1 1 d DU . . H57A H 0.8178 0.5407 -0.0784 0.163 Uiso 1 1 calc R . . H57B H 0.8386 0.6165 -0.0524 0.163 Uiso 1 1 calc R . . C58 C 0.7241(11) 0.5617(9) -0.0408(5) 0.188(9) Uani 1 1 d D . . H58A H 0.6940 0.6024 -0.0557 0.282 Uiso 1 1 calc R . . H58B H 0.7208 0.5786 -0.0155 0.282 Uiso 1 1 calc R . . H58C H 0.6986 0.5063 -0.0437 0.282 Uiso 1 1 calc R . . C59 C -0.0867(5) -0.2296(5) 0.2319(3) 0.052(2) Uani 1 1 d . . . H59A H -0.0960 -0.2575 0.2541 0.063 Uiso 1 1 calc R . . C60 C -0.1102(9) -0.0983(9) 0.1948(4) 0.123(5) Uani 1 1 d . . . H60A H -0.0799 -0.1298 0.1763 0.185 Uiso 1 1 calc R . . H60B H -0.0792 -0.0472 0.2007 0.185 Uiso 1 1 calc R . . H60C H -0.1659 -0.0834 0.1858 0.185 Uiso 1 1 calc R . . C61 C -0.1656(7) -0.1128(7) 0.2599(3) 0.091(4) Uani 1 1 d . . . H61A H -0.1668 -0.1530 0.2799 0.137 Uiso 1 1 calc R . . H61B H -0.2230 -0.0993 0.2527 0.137 Uiso 1 1 calc R . . H61C H -0.1369 -0.0617 0.2677 0.137 Uiso 1 1 calc R . . C62 C 0.9233(6) 0.6883(5) 0.0529(2) 0.050(2) Uani 1 1 d . . . H62A H 0.9770 0.6844 0.0638 0.060 Uiso 1 1 calc R . . C63 C 0.7747(5) 0.7277(6) 0.0571(3) 0.067(3) Uani 1 1 d . . . H63A H 0.7747 0.7093 0.0319 0.100 Uiso 1 1 calc R . . H63B H 0.7578 0.7866 0.0583 0.100 Uiso 1 1 calc R . . H63C H 0.7353 0.6935 0.0710 0.100 Uiso 1 1 calc R . . C64 C 0.8702(5) 0.7436(5) 0.1112(3) 0.059(2) Uani 1 1 d . . . H64A H 0.9287 0.7361 0.1186 0.089 Uiso 1 1 calc R . . H64B H 0.8340 0.7087 0.1263 0.089 Uiso 1 1 calc R . . H64C H 0.8544 0.8025 0.1140 0.089 Uiso 1 1 calc R . . N1 N -0.1189(5) -0.1512(5) 0.2280(2) 0.067(2) Uani 1 1 d . . . N2 N 0.8605(4) 0.7182(4) 0.0724(2) 0.0438(16) Uani 1 1 d . . . O1 O 0.9971(3) 0.4984(3) 0.05426(13) 0.0282(10) Uani 1 1 d . . . O1W O 0.1021(4) -0.3539(4) 0.26082(18) 0.075(2) Uani 1 1 d . . . O2 O 0.9567(3) 0.5098(3) 0.11131(15) 0.0378(12) Uani 1 1 d . . . O2W O 0.0624(5) -0.5354(4) 0.22385(18) 0.079(2) Uani 1 1 d . . . O3 O 0.6172(3) 0.8535(3) 0.11038(18) 0.0509(14) Uani 1 1 d . . . O3W O -0.0948(3) -0.4625(3) 0.18108(15) 0.0461(14) Uani 1 1 d . . . O4 O 0.6323(3) 0.9003(3) 0.16690(16) 0.0464(14) Uani 1 1 d . . . O4W O -0.0859(4) -0.4250(4) 0.26251(16) 0.0600(16) Uani 1 1 d . . . O5 O 0.2104(3) 0.5336(3) 0.06609(14) 0.0362(12) Uani 1 1 d . . . O5W O 1.0536(8) 0.4328(6) -0.0193(2) 0.148(5) Uani 1 1 d . . . O6 O 0.2562(3) 0.5270(4) 0.12287(16) 0.0457(14) Uani 1 1 d . . . O6W O 1.1174(5) 0.6239(7) 0.0146(3) 0.139(4) Uani 1 1 d . . . O7 O 0.6181(4) 0.1605(3) 0.10761(17) 0.0562(16) Uani 1 1 d . . . O7W O 1.0294(4) 0.6241(4) -0.05814(17) 0.0694(18) Uani 1 1 d . . . O8 O 0.5903(3) 0.1087(3) 0.16191(16) 0.0438(13) Uani 1 1 d . . . O9 O 0.1046(3) 0.3580(3) 0.10112(16) 0.0453(14) Uani 1 1 d . . . O10 O 0.0929(4) 0.4098(3) 0.15692(16) 0.0539(15) Uani 1 1 d . . . O11 O 0.5126(3) 0.0145(4) 0.07322(16) 0.0477(14) Uani 1 1 d . . . O12 O 0.4533(3) -0.0123(4) 0.12690(17) 0.0517(15) Uani 1 1 d . . . O13 O -0.2844(3) -0.0097(3) 0.06486(15) 0.0424(13) Uani 1 1 d . . . O14 O -0.2332(3) 0.0054(3) 0.11988(16) 0.0412(13) Uani 1 1 d . . . O15 O 0.0979(3) -0.3858(3) 0.16694(15) 0.0377(12) Uani 1 1 d . . . O16 O 0.0988(3) -0.3378(3) 0.11019(14) 0.0324(11) Uani 1 1 d . . . O17 O 0.9151(4) 0.6645(4) 0.02025(17) 0.072(2) Uani 1 1 d . . . O18 O 0.8800(6) 0.5099(6) -0.0360(3) 0.127(4) Uani 1 1 d . . . H18B H 0.8734 0.4510 -0.0379 0.153 Uiso 1 1 calc R . . O22 O -0.0458(4) -0.2674(3) 0.20830(18) 0.0608(17) 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 Cd1 0.0261(2) 0.0266(2) 0.0340(3) -0.0010(2) 0.0021(2) 0.00085(17) Cd2 0.0242(2) 0.0190(2) 0.0398(4) -0.0002(2) -0.0017(2) -0.00006(17) Cd3 0.0451(3) 0.0360(3) 0.0374(4) -0.0027(3) 0.0034(3) -0.0039(2) Cd4 0.0438(3) 0.0645(4) 0.0288(3) -0.0004(3) 0.0019(3) -0.0001(3) Si1 0.0203(8) 0.0230(9) 0.0293(10) -0.0022(8) 0.0013(8) 0.0007(7) Si2 0.0191(8) 0.0198(8) 0.0299(10) -0.0011(8) 0.0012(8) -0.0022(6) C1 0.032(4) 0.020(3) 0.032(4) 0.000(3) -0.004(3) -0.004(2) C2 0.033(4) 0.048(4) 0.025(4) -0.012(3) 0.003(3) -0.012(3) C3 0.030(4) 0.069(5) 0.041(5) -0.024(4) 0.007(4) -0.022(3) C4 0.045(5) 0.065(5) 0.031(5) -0.018(4) 0.014(4) -0.015(4) C5 0.028(3) 0.027(3) 0.027(4) -0.006(3) 0.000(3) -0.003(3) C6 0.030(4) 0.024(3) 0.021(4) 0.006(3) -0.003(3) 0.001(3) C7 0.027(4) 0.026(3) 0.041(5) -0.006(3) -0.009(4) 0.006(3) C8 0.012(3) 0.021(3) 0.035(4) -0.002(3) 0.000(3) -0.003(2) C9 0.035(4) 0.030(4) 0.042(5) 0.001(3) 0.001(3) 0.002(3) C10 0.058(5) 0.048(5) 0.016(4) -0.008(3) -0.010(4) -0.008(4) C11 0.024(3) 0.037(4) 0.037(5) -0.013(3) 0.006(3) -0.005(3) C12 0.025(3) 0.022(3) 0.038(5) -0.005(3) 0.006(3) 0.005(2) C13 0.020(3) 0.029(3) 0.024(4) -0.004(3) -0.004(3) 0.005(2) C14 0.036(4) 0.029(4) 0.036(5) 0.000(4) 0.007(4) 0.000(3) C15 0.025(3) 0.028(3) 0.037(5) 0.001(3) -0.002(3) 0.000(3) C16 0.024(3) 0.037(4) 0.038(5) 0.003(3) 0.001(3) -0.011(3) C17 0.055(5) 0.046(5) 0.032(5) 0.010(4) -0.014(4) -0.015(4) C18 0.029(4) 0.049(4) 0.037(5) -0.004(4) -0.011(3) -0.003(3) C19 0.029(4) 0.024(3) 0.032(4) -0.011(3) -0.004(3) 0.006(3) C20 0.023(3) 0.043(4) 0.025(4) -0.005(3) 0.001(3) 0.009(3) C21 0.024(4) 0.029(4) 0.045(5) -0.004(3) -0.009(4) 0.006(3) C22 0.021(3) 0.026(3) 0.028(4) 0.003(3) 0.001(3) 0.004(2) C23 0.059(5) 0.022(4) 0.052(5) -0.001(4) 0.016(4) 0.000(3) C24 0.079(6) 0.039(5) 0.049(6) 0.007(4) 0.030(5) 0.003(4) C25 0.048(4) 0.030(4) 0.049(6) 0.012(4) 0.007(4) -0.007(3) C26 0.027(3) 0.027(3) 0.037(5) 0.001(3) -0.003(3) 0.005(3) C27 0.033(4) 0.024(3) 0.026(4) 0.000(3) 0.007(3) 0.001(3) C28 0.028(4) 0.026(4) 0.048(5) 0.004(4) -0.009(4) 0.009(3) C29 0.017(3) 0.021(3) 0.029(4) -0.002(3) 0.009(3) 0.001(2) C30 0.026(3) 0.023(3) 0.035(4) -0.010(3) -0.002(3) 0.001(2) C31 0.042(4) 0.013(3) 0.042(5) 0.009(3) -0.009(4) 0.000(3) C32 0.054(5) 0.022(4) 0.052(6) -0.001(4) -0.001(4) -0.002(3) C33 0.049(4) 0.031(4) 0.039(5) 0.001(3) 0.019(4) 0.005(3) C34 0.035(4) 0.019(3) 0.038(5) 0.001(3) 0.007(3) 0.004(3) C35 0.045(4) 0.017(4) 0.055(6) 0.005(4) -0.007(4) -0.003(3) C36 0.021(3) 0.035(4) 0.033(4) 0.002(3) 0.007(3) -0.005(3) C37 0.024(4) 0.054(5) 0.041(5) 0.009(4) -0.005(3) -0.005(3) C38 0.027(4) 0.078(6) 0.036(5) 0.033(4) -0.002(3) -0.012(4) C39 0.029(4) 0.038(4) 0.043(5) 0.005(4) 0.011(4) -0.003(3) C40 0.023(3) 0.021(3) 0.040(5) -0.003(3) 0.004(3) -0.006(2) C41 0.032(4) 0.027(3) 0.022(4) 0.001(3) 0.004(3) -0.002(3) C42 0.031(4) 0.034(4) 0.029(5) -0.005(3) -0.001(3) 0.012(3) C43 0.023(3) 0.023(3) 0.032(4) 0.009(3) -0.001(3) 0.003(2) C44 0.025(4) 0.047(4) 0.030(5) -0.009(4) 0.006(3) -0.003(3) C45 0.028(4) 0.065(5) 0.031(5) -0.015(4) 0.010(3) -0.008(3) C46 0.031(4) 0.049(4) 0.037(5) -0.008(4) -0.008(3) -0.013(3) C47 0.026(3) 0.025(3) 0.032(4) 0.000(3) 0.001(3) 0.004(2) C48 0.031(4) 0.021(3) 0.028(4) 0.001(3) 0.011(3) 0.004(3) C49 0.020(3) 0.029(4) 0.042(5) 0.003(3) 0.002(3) -0.001(3) C50 0.023(3) 0.015(3) 0.019(4) 0.001(3) 0.005(3) 0.003(2) C51 0.030(3) 0.024(3) 0.029(4) -0.005(3) -0.002(3) -0.003(3) C52 0.027(4) 0.043(4) 0.028(4) 0.002(3) -0.006(3) 0.002(3) C53 0.031(3) 0.022(3) 0.033(4) 0.009(3) -0.010(3) -0.006(3) C54 0.029(3) 0.013(3) 0.037(4) 0.001(3) 0.006(3) -0.002(2) C55 0.022(3) 0.024(3) 0.039(5) 0.000(3) 0.003(3) -0.010(2) C56 0.029(3) 0.015(3) 0.034(5) -0.003(3) 0.000(3) 0.002(2) C57 0.137(7) 0.131(7) 0.140(7) 0.003(5) -0.006(5) 0.008(5) C58 0.24(2) 0.100(11) 0.22(2) -0.072(13) -0.081(19) 0.057(13) C59 0.040(4) 0.053(5) 0.064(6) -0.019(5) 0.000(4) 0.002(4) C60 0.130(12) 0.102(10) 0.138(13) 0.043(9) 0.047(10) -0.011(8) C61 0.077(7) 0.082(8) 0.115(10) -0.043(7) 0.021(7) 0.017(6) C62 0.064(6) 0.052(5) 0.035(5) 0.007(4) 0.003(4) 0.012(4) C63 0.057(6) 0.064(6) 0.079(8) 0.012(5) -0.005(5) 0.007(4) C64 0.062(5) 0.051(5) 0.065(7) 0.000(5) 0.013(5) 0.001(4) N1 0.066(5) 0.049(4) 0.087(7) -0.019(4) 0.014(4) 0.000(3) N2 0.045(4) 0.036(3) 0.050(5) 0.009(3) 0.000(3) 0.005(3) O1 0.021(2) 0.033(2) 0.031(3) -0.002(2) 0.005(2) 0.0005(17) O1W 0.069(4) 0.099(5) 0.058(4) -0.032(4) 0.017(3) -0.026(4) O2 0.030(3) 0.050(3) 0.033(3) -0.010(3) -0.004(2) -0.003(2) O2W 0.147(7) 0.037(3) 0.052(5) -0.004(3) -0.014(4) 0.026(4) O3 0.059(3) 0.032(3) 0.061(4) 0.003(3) -0.013(3) 0.003(2) O3W 0.036(3) 0.060(3) 0.043(4) -0.017(3) -0.006(2) -0.007(2) O4 0.048(3) 0.032(3) 0.059(4) -0.008(3) 0.015(3) 0.002(2) O4W 0.077(4) 0.060(4) 0.043(4) 0.012(3) 0.004(3) -0.009(3) O5 0.031(3) 0.044(3) 0.034(3) -0.007(2) -0.007(2) 0.007(2) O5W 0.250(12) 0.126(7) 0.069(6) 0.038(5) 0.071(7) 0.120(8) O6 0.027(3) 0.074(4) 0.036(4) 0.007(3) -0.005(2) 0.007(2) O6W 0.092(6) 0.215(10) 0.110(7) 0.092(7) -0.056(5) -0.084(6) O7 0.098(5) 0.024(3) 0.046(4) -0.002(3) 0.005(4) 0.012(3) O7W 0.086(5) 0.084(5) 0.038(4) 0.002(3) 0.002(3) -0.003(4) O8 0.054(3) 0.031(3) 0.046(3) 0.002(3) 0.007(3) -0.008(2) O9 0.062(3) 0.034(3) 0.041(4) 0.011(3) 0.009(3) 0.001(2) O10 0.077(4) 0.026(3) 0.058(4) 0.009(3) -0.006(3) -0.001(2) O11 0.024(3) 0.069(4) 0.050(4) 0.005(3) 0.008(3) 0.006(2) O12 0.022(3) 0.077(4) 0.056(4) -0.004(3) -0.001(3) 0.015(2) O13 0.023(3) 0.057(3) 0.047(4) 0.000(3) -0.005(2) 0.003(2) O14 0.025(2) 0.054(3) 0.045(4) -0.010(3) 0.007(2) -0.005(2) O15 0.041(3) 0.023(2) 0.049(3) -0.002(2) 0.014(2) -0.001(2) O16 0.042(3) 0.023(2) 0.032(3) -0.004(2) 0.000(2) -0.0031(18) O17 0.095(5) 0.086(5) 0.036(4) 0.010(3) 0.004(3) 0.054(4) O18 0.134(8) 0.132(7) 0.116(8) 0.047(6) -0.074(7) -0.040(6) O22 0.062(4) 0.043(3) 0.078(5) 0.000(3) 0.021(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O11 2.312(5) 1_565 ? Cd1 O8 2.337(5) 1_565 ? Cd1 O14 2.340(4) 1_665 ? Cd1 O3 2.365(5) . ? Cd1 O4 2.422(6) . ? Cd1 O13 2.472(5) 1_665 ? Cd1 O7 2.482(5) 1_565 ? Cd1 O12 2.600(5) 1_565 ? Cd2 O2 2.315(4) 1_455 ? Cd2 O16 2.328(4) 1_565 ? Cd2 O10 2.332(5) . ? Cd2 O5 2.352(5) . ? Cd2 O6 2.419(5) . ? Cd2 O9 2.462(5) . ? Cd2 O15 2.570(5) 1_565 ? Cd3 O4W 2.271(6) . ? Cd3 O22 2.278(5) . ? Cd3 O3W 2.279(5) . ? Cd3 O2W 2.280(5) . ? Cd3 O15 2.287(5) . ? Cd3 O1W 2.301(6) . ? Cd4 O5W 2.181(8) . ? Cd4 O18 2.271(8) . ? Cd4 O6W 2.284(7) . ? Cd4 O1 2.298(5) . ? Cd4 O7W 2.306(6) . ? Cd4 O17 2.312(6) . ? Si1 C8 1.875(6) . ? Si1 C22 1.877(7) . ? Si1 C1 1.877(7) . ? Si1 C15 1.887(7) . ? Si2 C50 1.869(6) . ? Si2 C29 1.869(6) . ? Si2 C43 1.871(7) . ? Si2 C36 1.884(6) . ? C1 C2 1.403(9) . ? C1 C6 1.403(9) . ? C2 C3 1.357(9) . ? C2 H2A 0.9300 . ? C3 C4 1.330(10) . ? C3 H3A 0.9300 . ? C4 C5 1.412(10) . ? C4 H4A 0.9300 . ? C5 C6 1.400(9) . ? C5 C7 1.508(9) . ? C6 H6A 0.9300 . ? C7 O2 1.239(9) . ? C7 O1 1.250(8) . ? C8 C13 1.388(8) . ? C8 C9 1.403(9) . ? C9 C10 1.394(10) . ? C9 H9A 0.9300 . ? C10 C11 1.368(10) . ? C10 H10A 0.9300 . ? C11 C12 1.402(10) . ? C11 H11A 0.9300 . ? C12 C13 1.370(9) . ? C12 C14 1.511(9) . ? C13 H13A 0.9300 . ? C14 O3 1.241(9) . ? C14 O4 1.256(9) . ? C15 C16 1.400(10) . ? C15 C20 1.415(9) . ? C16 C17 1.377(10) . ? C16 H16A 0.9300 . ? C17 C18 1.346(10) . ? C17 H17A 0.9300 . ? C18 C19 1.379(10) . ? C18 H18A 0.9300 . ? C19 C20 1.405(9) . ? C19 C21 1.507(9) . ? C20 H20A 0.9300 . ? C21 O6 1.251(9) . ? C21 O5 1.272(8) . ? C22 C27 1.378(9) . ? C22 C23 1.405(10) . ? C23 C24 1.390(11) . ? C23 H23A 0.9300 . ? C24 C25 1.384(11) . ? C24 H24A 0.9300 . ? C25 C26 1.374(10) . ? C25 H25A 0.9300 . ? C26 C27 1.421(9) . ? C26 C28 1.487(9) . ? C27 H27A 0.9300 . ? C28 O8 1.244(8) . ? C28 O7 1.268(9) . ? C29 C34 1.385(9) . ? C29 C30 1.401(9) . ? C30 C31 1.408(9) . ? C30 H30A 0.9300 . ? C31 C32 1.381(11) . ? C31 C35 1.510(9) . ? C32 C33 1.406(10) . ? C32 H32A 0.9300 . ? C33 C34 1.372(9) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 O9 1.243(9) . ? C35 O10 1.281(9) . ? C36 C41 1.348(9) . ? C36 C37 1.407(10) . ? C37 C38 1.400(10) . ? C37 H37A 0.9300 . ? C38 C39 1.346(10) . ? C38 H38A 0.9300 . ? C39 C40 1.371(10) . ? C39 H39A 0.9300 . ? C40 C41 1.416(9) . ? C40 C42 1.510(9) . ? C41 H41A 0.9300 . ? C42 O11 1.249(9) . ? C42 O12 1.258(9) . ? C43 C44 1.406(10) . ? C43 C48 1.406(8) . ? C44 C45 1.410(10) . ? C44 H44A 0.9300 . ? C45 C46 1.415(9) . ? C45 H45A 0.9300 . ? C46 C47 1.394(10) . ? C46 H46A 0.9300 . ? C47 C48 1.364(9) . ? C47 C49 1.508(9) . ? C48 H48A 0.9300 . ? C49 O13 1.216(8) . ? C49 O14 1.260(9) . ? C49 Cd1 2.742(7) 1_445 ? C50 C55 1.387(8) . ? C50 C51 1.405(9) . ? C51 C52 1.435(9) . ? C51 H51A 0.9300 . ? C52 C53 1.345(9) . ? C52 H52A 0.9300 . ? C53 C54 1.367(9) . ? C53 H53A 0.9300 . ? C54 C55 1.445(9) . ? C54 C56 1.518(8) . ? C55 H55A 0.9300 . ? C56 O16 1.235(8) . ? C56 O15 1.255(8) . ? C57 O18 1.371(17) . ? C57 C58 1.535(9) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O22 1.224(9) . ? C59 N1 1.334(11) . ? C59 H59A 0.9300 . ? C60 N1 1.470(14) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 N1 1.498(12) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 O17 1.252(10) . ? C62 N2 1.299(10) . ? C62 H62A 0.9300 . ? C63 N2 1.459(10) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 N2 1.476(11) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? O2 Cd2 2.315(4) 1_655 ? O7 Cd1 2.482(5) 1_545 ? O8 Cd1 2.337(5) 1_545 ? O11 Cd1 2.312(5) 1_545 ? O12 Cd1 2.600(5) 1_545 ? O13 Cd1 2.472(5) 1_445 ? O14 Cd1 2.340(4) 1_445 ? O15 Cd2 2.570(5) 1_545 ? O16 Cd2 2.328(4) 1_545 ? O18 H18B 0.9300 . ? 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 O11 Cd1 O8 107.57(19) 1_565 1_565 ? O11 Cd1 O14 136.98(19) 1_565 1_665 ? O8 Cd1 O14 98.60(18) 1_565 1_665 ? O11 Cd1 O3 89.6(2) 1_565 . ? O8 Cd1 O3 141.0(2) 1_565 . ? O14 Cd1 O3 90.94(17) 1_665 . ? O11 Cd1 O4 129.43(19) 1_565 . ? O8 Cd1 O4 88.83(18) 1_565 . ? O14 Cd1 O4 83.52(18) 1_665 . ? O3 Cd1 O4 54.6(2) . . ? O11 Cd1 O13 84.34(17) 1_565 1_665 ? O8 Cd1 O13 135.00(17) 1_565 1_665 ? O14 Cd1 O13 53.51(18) 1_665 1_665 ? O3 Cd1 O13 80.11(19) . 1_665 ? O4 Cd1 O13 117.28(16) . 1_665 ? O11 Cd1 O7 80.0(2) 1_565 1_565 ? O8 Cd1 O7 53.68(19) 1_565 1_565 ? O14 Cd1 O7 89.31(19) 1_665 1_565 ? O3 Cd1 O7 164.9(2) . 1_565 ? O4 Cd1 O7 140.32(19) . 1_565 ? O13 Cd1 O7 87.97(19) 1_665 1_565 ? O11 Cd1 O12 52.89(19) 1_565 1_565 ? O8 Cd1 O12 78.53(18) 1_565 1_565 ? O14 Cd1 O12 169.6(2) 1_665 1_565 ? O3 Cd1 O12 85.32(18) . 1_565 ? O4 Cd1 O12 86.37(18) . 1_565 ? O13 Cd1 O12 134.86(18) 1_665 1_565 ? O7 Cd1 O12 96.84(19) 1_565 1_565 ? O2 Cd2 O16 89.24(16) 1_455 1_565 ? O2 Cd2 O10 84.4(2) 1_455 . ? O16 Cd2 O10 134.76(19) 1_565 . ? O2 Cd2 O5 135.06(18) 1_455 . ? O16 Cd2 O5 83.26(16) 1_565 . ? O10 Cd2 O5 130.24(18) . . ? O2 Cd2 O6 169.18(19) 1_455 . ? O16 Cd2 O6 87.33(17) 1_565 . ? O10 Cd2 O6 90.73(19) . . ? O5 Cd2 O6 54.60(18) . . ? O2 Cd2 O9 88.57(17) 1_455 . ? O16 Cd2 O9 170.26(19) 1_565 . ? O10 Cd2 O9 54.39(19) . . ? O5 Cd2 O9 91.61(17) . . ? O6 Cd2 O9 96.47(18) . . ? O2 Cd2 O15 88.48(17) 1_455 1_565 ? O16 Cd2 O15 53.04(17) 1_565 1_565 ? O10 Cd2 O15 81.99(18) . 1_565 ? O5 Cd2 O15 119.85(16) . 1_565 ? O6 Cd2 O15 81.27(17) . 1_565 ? O9 Cd2 O15 136.35(18) . 1_565 ? O4W Cd3 O22 90.1(2) . . ? O4W Cd3 O3W 83.3(2) . . ? O22 Cd3 O3W 92.8(2) . . ? O4W Cd3 O2W 89.9(2) . . ? O22 Cd3 O2W 179.4(3) . . ? O3W Cd3 O2W 86.6(2) . . ? O4W Cd3 O15 174.9(2) . . ? O22 Cd3 O15 91.84(19) . . ? O3W Cd3 O15 91.99(19) . . ? O2W Cd3 O15 88.0(2) . . ? O4W Cd3 O1W 86.9(2) . . ? O22 Cd3 O1W 91.9(2) . . ? O3W Cd3 O1W 169.1(2) . . ? O2W Cd3 O1W 88.7(3) . . ? O15 Cd3 O1W 97.6(2) . . ? O5W Cd4 O18 85.9(5) . . ? O5W Cd4 O6W 98.6(5) . . ? O18 Cd4 O6W 164.4(3) . . ? O5W Cd4 O1 84.1(2) . . ? O18 Cd4 O1 111.0(3) . . ? O6W Cd4 O1 84.5(2) . . ? O5W Cd4 O7W 95.8(3) . . ? O18 Cd4 O7W 83.6(3) . . ? O6W Cd4 O7W 81.0(3) . . ? O1 Cd4 O7W 165.4(2) . . ? O5W Cd4 O17 166.8(3) . . ? O18 Cd4 O17 89.1(4) . . ? O6W Cd4 O17 89.5(4) . . ? O1 Cd4 O17 86.29(18) . . ? O7W Cd4 O17 95.8(2) . . ? C8 Si1 C22 109.5(3) . . ? C8 Si1 C1 109.5(3) . . ? C22 Si1 C1 108.3(3) . . ? C8 Si1 C15 110.5(3) . . ? C22 Si1 C15 110.7(3) . . ? C1 Si1 C15 108.3(3) . . ? C50 Si2 C29 109.5(3) . . ? C50 Si2 C43 108.9(3) . . ? C29 Si2 C43 110.4(3) . . ? C50 Si2 C36 108.8(3) . . ? C29 Si2 C36 109.9(3) . . ? C43 Si2 C36 109.3(3) . . ? C2 C1 C6 117.5(6) . . ? C2 C1 Si1 121.4(5) . . ? C6 C1 Si1 120.9(5) . . ? C3 C2 C1 121.6(6) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C4 C3 C2 122.0(7) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 119.3(7) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 120.0(6) . . ? C6 C5 C7 119.7(6) . . ? C4 C5 C7 120.4(6) . . ? C5 C6 C1 119.6(6) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? O2 C7 O1 122.0(6) . . ? O2 C7 C5 116.6(7) . . ? O1 C7 C5 121.3(7) . . ? C13 C8 C9 118.0(6) . . ? C13 C8 Si1 120.9(5) . . ? C9 C8 Si1 121.0(5) . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.0(7) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C13 C12 C11 118.4(6) . . ? C13 C12 C14 121.8(7) . . ? C11 C12 C14 119.8(6) . . ? C12 C13 C8 122.5(6) . . ? C12 C13 H13A 118.7 . . ? C8 C13 H13A 118.7 . . ? O3 C14 O4 123.2(7) . . ? O3 C14 C12 116.8(7) . . ? O4 C14 C12 120.0(7) . . ? O3 C14 Cd1 60.4(4) . . ? O4 C14 Cd1 63.0(4) . . ? C12 C14 Cd1 172.8(5) . . ? C16 C15 C20 117.8(6) . . ? C16 C15 Si1 121.7(5) . . ? C20 C15 Si1 120.5(5) . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 121.6(7) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 120.4(7) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C20 119.6(6) . . ? C18 C19 C21 122.2(6) . . ? C20 C19 C21 118.2(6) . . ? C19 C20 C15 119.9(7) . . ? C19 C20 H20A 120.0 . . ? C15 C20 H20A 120.0 . . ? O6 C21 O5 120.4(6) . . ? O6 C21 C19 121.9(6) . . ? O5 C21 C19 117.7(7) . . ? O6 C21 Cd2 61.7(4) . . ? O5 C21 Cd2 58.7(3) . . ? C19 C21 Cd2 176.3(5) . . ? C27 C22 C23 118.0(6) . . ? C27 C22 Si1 121.2(5) . . ? C23 C22 Si1 120.8(5) . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C25 C24 C23 121.5(8) . . ? C25 C24 H24A 119.3 . . ? C23 C24 H24A 119.3 . . ? C26 C25 C24 119.2(7) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C27 119.6(6) . . ? C25 C26 C28 121.0(6) . . ? C27 C26 C28 119.3(7) . . ? C22 C27 C26 121.5(6) . . ? C22 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? O8 C28 O7 120.4(6) . . ? O8 C28 C26 119.8(7) . . ? O7 C28 C26 119.7(7) . . ? C34 C29 C30 117.1(6) . . ? C34 C29 Si2 121.8(5) . . ? C30 C29 Si2 121.1(5) . . ? C29 C30 C31 120.9(6) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C32 C31 C30 119.6(6) . . ? C32 C31 C35 122.3(6) . . ? C30 C31 C35 118.0(7) . . ? C31 C32 C33 120.2(7) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 118.5(7) . . ? C34 C33 H33A 120.7 . . ? C32 C33 H33A 120.7 . . ? C33 C34 C29 123.6(6) . . ? C33 C34 H34A 118.2 . . ? C29 C34 H34A 118.2 . . ? O9 C35 O10 120.7(7) . . ? O9 C35 C31 122.5(7) . . ? O10 C35 C31 116.8(7) . . ? O9 C35 Cd2 63.4(4) . . ? O10 C35 Cd2 57.5(4) . . ? C31 C35 Cd2 172.3(6) . . ? C41 C36 C37 118.3(6) . . ? C41 C36 Si2 120.5(5) . . ? C37 C36 Si2 121.2(5) . . ? C38 C37 C36 118.8(6) . . ? C38 C37 H37A 120.6 . . ? C36 C37 H37A 120.6 . . ? C39 C38 C37 121.6(7) . . ? C39 C38 H38A 119.2 . . ? C37 C38 H38A 119.2 . . ? C38 C39 C40 120.7(7) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C39 C40 C41 117.8(6) . . ? C39 C40 C42 121.6(6) . . ? C41 C40 C42 120.6(7) . . ? C36 C41 C40 122.7(7) . . ? C36 C41 H41A 118.7 . . ? C40 C41 H41A 118.7 . . ? O11 C42 O12 123.0(7) . . ? O11 C42 C40 118.3(7) . . ? O12 C42 C40 118.7(7) . . ? C44 C43 C48 117.7(6) . . ? C44 C43 Si2 121.7(5) . . ? C48 C43 Si2 120.5(5) . . ? C43 C44 C45 121.1(6) . . ? C43 C44 H44A 119.5 . . ? C45 C44 H44A 119.5 . . ? C44 C45 C46 118.5(7) . . ? C44 C45 H45A 120.7 . . ? C46 C45 H45A 120.7 . . ? C47 C46 C45 120.2(6) . . ? C47 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C48 C47 C46 120.0(6) . . ? C48 C47 C49 120.9(6) . . ? C46 C47 C49 119.1(6) . . ? C47 C48 C43 122.3(6) . . ? C47 C48 H48A 118.8 . . ? C43 C48 H48A 118.8 . . ? O13 C49 O14 122.3(6) . . ? O13 C49 C47 121.4(7) . . ? O14 C49 C47 116.3(6) . . ? O13 C49 Cd1 64.3(4) . 1_445 ? O14 C49 Cd1 58.3(3) . 1_445 ? C47 C49 Cd1 171.4(5) . 1_445 ? C55 C50 C51 118.3(6) . . ? C55 C50 Si2 120.3(5) . . ? C51 C50 Si2 121.3(4) . . ? C50 C51 C52 120.7(6) . . ? C50 C51 H51A 119.7 . . ? C52 C51 H51A 119.7 . . ? C53 C52 C51 118.9(6) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C52 C53 C54 122.9(6) . . ? C52 C53 H53A 118.5 . . ? C54 C53 H53A 118.5 . . ? C53 C54 C55 118.7(5) . . ? C53 C54 C56 123.2(6) . . ? C55 C54 C56 118.0(6) . . ? C50 C55 C54 120.4(6) . . ? C50 C55 H55A 119.8 . . ? C54 C55 H55A 119.8 . . ? O16 C56 O15 123.9(6) . . ? O16 C56 C54 118.1(6) . . ? O15 C56 C54 117.9(6) . . ? O18 C57 C58 124.8(14) . . ? O18 C57 H57A 106.1 . . ? C58 C57 H57A 106.1 . . ? O18 C57 H57B 106.1 . . ? C58 C57 H57B 106.1 . . ? H57A C57 H57B 106.3 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O22 C59 N1 124.5(9) . . ? O22 C59 H59A 117.7 . . ? N1 C59 H59A 117.7 . . ? N1 C60 H60A 109.5 . . ? N1 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N1 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N1 C61 H61A 109.5 . . ? N1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O17 C62 N2 123.1(8) . . ? O17 C62 H62A 118.4 . . ? N2 C62 H62A 118.4 . . ? N2 C63 H63A 109.5 . . ? N2 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N2 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N2 C64 H64A 109.5 . . ? N2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C59 N1 C60 124.8(9) . . ? C59 N1 C61 118.1(9) . . ? C60 N1 C61 117.1(9) . . ? C62 N2 C63 121.7(8) . . ? C62 N2 C64 122.7(7) . . ? C63 N2 C64 115.6(7) . . ? C7 O1 Cd4 131.1(4) . . ? C7 O2 Cd2 102.0(4) . 1_655 ? C14 O3 Cd1 92.5(4) . . ? C14 O4 Cd1 89.5(5) . . ? C21 O5 Cd2 93.8(4) . . ? C21 O6 Cd2 91.2(4) . . ? C28 O7 Cd1 89.0(4) . 1_545 ? C28 O8 Cd1 96.5(5) . 1_545 ? C35 O9 Cd2 89.8(4) . . ? C35 O10 Cd2 94.9(5) . . ? C42 O11 Cd1 98.5(5) . 1_545 ? C42 O12 Cd1 84.8(4) . 1_545 ? C49 O13 Cd1 89.3(4) . 1_445 ? C49 O14 Cd1 94.4(4) . 1_445 ? C56 O15 Cd3 131.3(4) . . ? C56 O15 Cd2 85.1(4) . 1_545 ? Cd3 O15 Cd2 125.56(19) . 1_545 ? C56 O16 Cd2 96.8(4) . 1_545 ? C62 O17 Cd4 121.8(5) . . ? C57 O18 Cd4 128.7(10) . . ? C57 O18 H18B 115.7 . . ? Cd4 O18 H18B 115.7 . . ? C59 O22 Cd3 123.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.928 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.227 2696 686 ' ' _platon_squeeze_details ; Disordered, independent solvent molecules were eliminated from the refinement using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13]. ; # start Validation Reply Form _vrf_PLAT602_p1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The large voids are ocuppied by disordered solvent molecules (mainly DMF molecules), The disordered solvents are excluded in the refinement by PLATON/SQUEEZE. ; # end Validation Reply Form data_p2 #TrackingRef '- p1-2.cif' _database_code_depnum_ccdc_archive 'CCDC 836456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cd2 N2 O10 Si' _chemical_formula_weight 879.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 12.9879(15) _cell_length_b 12.9879(15) _cell_length_c 25.025(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4221.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6266 _cell_measurement_theta_min 4.953 _cell_measurement_theta_max 50.012 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8809 _exptl_absorpt_correction_T_max 0.9183 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10549 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1922 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+8.2213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1922 _refine_ls_number_parameters 116 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.102 _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 Cd1 Cd 0.17497(3) 0.88411(3) 0.5000 0.0440(2) Uani 1 2 d S . . Si1 Si 0.5000 1.0000 0.7500 0.0338(4) Uani 1 4 d S . . C1 C 0.4062(3) 1.0691(3) 0.70602(14) 0.0409(8) Uani 1 1 d . . . C2 C 0.3758(4) 1.1702(4) 0.7154(2) 0.0685(14) Uani 1 1 d . . . H2A H 0.4058 1.2067 0.7434 0.082 Uiso 1 1 calc R . . C3 C 0.3011(5) 1.2179(4) 0.6838(2) 0.088(2) Uani 1 1 d . . . H3A H 0.2796 1.2845 0.6916 0.106 Uiso 1 1 calc R . . C4 C 0.2593(4) 1.1658(4) 0.6408(2) 0.0709(14) Uani 1 1 d . . . H4A H 0.2100 1.1979 0.6196 0.085 Uiso 1 1 calc R . . C5 C 0.2900(3) 1.0671(3) 0.62920(16) 0.0477(10) Uani 1 1 d . . . C6 C 0.3636(3) 1.0198(3) 0.66105(14) 0.0407(8) Uani 1 1 d . . . H6A H 0.3854 0.9536 0.6525 0.049 Uiso 1 1 calc R . . C7 C 0.2451(3) 1.0102(4) 0.58165(15) 0.0488(10) Uani 1 1 d . . . O1 O 0.2848(2) 0.9255(2) 0.56846(12) 0.0558(8) Uani 1 1 d . . . O2 O 0.1672(3) 1.0461(3) 0.55801(13) 0.0636(9) Uani 1 1 d . . . O3 O 0.2303(6) 0.7176(5) 0.5000 0.104(2) Uani 1 2 d S . . N1 N 0.2167(11) 0.5547(11) 0.5310(6) 0.127(5) Uiso 0.50 1 d PD . . C10 C 0.1227(16) 0.5125(18) 0.5000 0.271(13) Uiso 1 2 d SD . . H10A H 0.1048 0.5529 0.4693 0.406 Uiso 0.50 1 d PR . . H10B H 0.1398 0.4438 0.4890 0.406 Uiso 0.50 1 d PR . . H10C H 0.0654 0.5103 0.5242 0.406 Uiso 0.50 1 d PR . . C8 C 0.2360(16) 0.6539(11) 0.5251(8) 0.142(8) Uani 0.50 1 d P . . H8A H 0.2816 0.6736 0.5536 0.170 Uiso 0.50 1 d PR . . C9 C 0.243(2) 0.488(2) 0.5771(12) 0.197(11) Uiso 0.50 1 d P . . H9A H 0.2949 0.5100 0.6021 0.295 Uiso 0.50 1 d PR . . H9B H 0.2619 0.4224 0.5625 0.295 Uiso 0.50 1 d PR . . H9C H 0.1781 0.4823 0.5951 0.295 Uiso 0.50 1 d PR . . 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 Cd1 0.0504(3) 0.0474(3) 0.0341(3) 0.000 0.000 -0.00867(17) Si1 0.0408(6) 0.0408(6) 0.0198(9) 0.000 0.000 0.000 C1 0.050(2) 0.048(2) 0.0242(17) 0.0020(16) -0.0027(15) 0.0028(17) C2 0.095(4) 0.062(3) 0.048(3) -0.016(2) -0.026(3) 0.020(3) C3 0.126(5) 0.060(3) 0.077(4) -0.017(3) -0.033(4) 0.039(3) C4 0.088(4) 0.072(3) 0.053(3) -0.007(2) -0.028(3) 0.027(3) C5 0.054(2) 0.056(2) 0.033(2) 0.0036(18) -0.0061(18) 0.0013(18) C6 0.048(2) 0.042(2) 0.0322(19) 0.0016(16) -0.0034(17) 0.0005(16) C7 0.055(2) 0.060(3) 0.032(2) 0.0089(19) -0.0077(18) -0.009(2) O1 0.0615(19) 0.0612(19) 0.0447(17) -0.0050(14) -0.0096(14) -0.0030(15) O2 0.0666(19) 0.076(2) 0.0488(18) 0.0142(16) -0.0161(16) 0.0026(17) O3 0.147(6) 0.045(3) 0.119(6) 0.000 0.000 0.019(4) C8 0.215(19) 0.062(8) 0.149(16) -0.018(9) 0.102(14) -0.009(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.278(6) . ? Cd1 O1 2.293(3) . ? Cd1 O1 2.293(3) 10_556 ? Cd1 O2 2.314(3) 11_466 ? Cd1 O2 2.314(3) 4_465 ? Cd1 O2 2.558(4) . ? Cd1 O2 2.558(4) 10_556 ? Si1 C1 1.871(4) 15_466 ? Si1 C1 1.871(4) 2_675 ? Si1 C1 1.871(4) . ? Si1 C1 1.871(4) 16_656 ? C1 C2 1.391(6) . ? C1 C6 1.408(5) . ? C2 C3 1.398(7) . ? C2 H2A 0.9300 . ? C3 C4 1.381(7) . ? C3 H3A 0.9300 . ? C4 C5 1.375(6) . ? C4 H4A 0.9300 . ? C5 C6 1.388(6) . ? C5 C7 1.517(6) . ? C6 H6A 0.9300 . ? C7 O1 1.259(5) . ? C7 O2 1.261(5) . ? O2 Cd1 2.314(3) 3_665 ? O3 C8 1.042(17) 10_556 ? O3 C8 1.042(17) . ? N1 C8 1.320(17) . ? N1 C9 1.48(3) . ? N1 C10 1.547(9) . ? N1 N1 1.55(3) 10_556 ? N1 C8 1.92(2) 10_556 ? C10 N1 1.547(9) 10_556 ? C10 H10A 0.9600 . ? C10 H10B 0.9601 . ? C10 H10C 0.9600 . ? C8 C8 1.26(4) 10_556 ? C8 N1 1.92(2) 10_556 ? C8 H8A 0.9602 . ? C9 H9A 0.9600 . ? C9 H9B 0.9601 . ? C9 H9C 0.9599 . ? 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 O3 Cd1 O1 91.50(16) . . ? O3 Cd1 O1 91.50(16) . 10_556 ? O1 Cd1 O1 96.67(16) . 10_556 ? O3 Cd1 O2 87.42(19) . 11_466 ? O1 Cd1 O2 170.49(12) . 11_466 ? O1 Cd1 O2 92.80(12) 10_556 11_466 ? O3 Cd1 O2 87.42(19) . 4_465 ? O1 Cd1 O2 92.80(12) . 4_465 ? O1 Cd1 O2 170.49(12) 10_556 4_465 ? O2 Cd1 O2 77.72(18) 11_466 4_465 ? O3 Cd1 O2 142.45(10) . . ? O1 Cd1 O2 53.68(11) . . ? O1 Cd1 O2 104.81(12) 10_556 . ? O2 Cd1 O2 124.36(15) 11_466 . ? O2 Cd1 O2 81.50(16) 4_465 . ? O3 Cd1 O2 142.45(10) . 10_556 ? O1 Cd1 O2 104.81(12) . 10_556 ? O1 Cd1 O2 53.68(11) 10_556 10_556 ? O2 Cd1 O2 81.50(16) 11_466 10_556 ? O2 Cd1 O2 124.36(15) 4_465 10_556 ? O2 Cd1 O2 69.16(14) . 10_556 ? C1 Si1 C1 110.24(12) 15_466 2_675 ? C1 Si1 C1 110.24(11) 15_466 . ? C1 Si1 C1 107.9(2) 2_675 . ? C1 Si1 C1 107.9(2) 15_466 16_656 ? C1 Si1 C1 110.24(11) 2_675 16_656 ? C1 Si1 C1 110.24(11) . 16_656 ? C2 C1 C6 116.9(4) . . ? C2 C1 Si1 122.5(3) . . ? C6 C1 Si1 120.5(3) . . ? C1 C2 C3 121.3(4) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 C7 120.6(4) . . ? C6 C5 C7 120.0(4) . . ? C5 C6 C1 121.9(4) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O1 C7 O2 121.9(4) . . ? O1 C7 C5 118.2(4) . . ? O2 C7 C5 119.8(4) . . ? C7 O1 Cd1 98.4(2) . . ? C7 O2 Cd1 142.4(3) . 3_665 ? C7 O2 Cd1 86.0(3) . . ? Cd1 O2 Cd1 104.49(13) 3_665 . ? C8 O3 C8 74.2(18) 10_556 . ? C8 O3 Cd1 140.9(8) 10_556 . ? C8 O3 Cd1 140.9(8) . . ? C8 N1 C9 127.8(19) . . ? C8 N1 C10 116.1(18) . . ? C9 N1 C10 111.5(16) . . ? C8 N1 N1 83.6(11) . 10_556 ? C9 N1 N1 141.1(12) . 10_556 ? C10 N1 N1 59.9(7) . 10_556 ? C8 N1 C8 40.5(13) . 10_556 ? C9 N1 C8 158.4(16) . 10_556 ? C10 N1 C8 88.5(12) . 10_556 ? N1 N1 C8 43.0(6) 10_556 10_556 ? N1 C10 N1 60.3(14) . 10_556 ? N1 C10 H10A 113.6 . . ? N1 C10 H10A 66.1 10_556 . ? N1 C10 H10B 107.0 . . ? N1 C10 H10B 90.2 10_556 . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 107.8 . . ? N1 C10 H10C 159.9 10_556 . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C8 C8 52.9(9) . 10_556 ? O3 C8 N1 146(2) . . ? C8 C8 N1 96.4(11) 10_556 . ? O3 C8 N1 94.7(14) . 10_556 ? C8 C8 N1 43.0(6) 10_556 10_556 ? N1 C8 N1 53.4(12) . 10_556 ? O3 C8 H8A 106.2 . . ? C8 C8 H8A 137.8 10_556 . ? N1 C8 H8A 107.1 . . ? N1 C8 H8A 143.2 10_556 . ? N1 C9 H9A 119.7 . . ? N1 C9 H9B 106.3 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 101.9 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.025 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 412 83 ' ' 2 0.500 0.500 0.500 412 83 ' ' _platon_squeeze_details ; Disordered, independent solvent molecules were eliminated from the refinement using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13]. ; # start Validation Reply Form _vrf_PLAT602_p1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The large voids are ocuppied by disordered solvent molecules (mainly WATER molecules), The disordered solvents are excluded in the refinement by PLATON/SQUEEZE. ; # end Validation Reply Form