# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_an_1368_av #TrackingRef 'an_1368_AV.cif' _audit_creation_date 2013-03-14 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C72 H128 Cu4 N16 O20 Si8), C12 H26 O5 Si2' _chemical_formula_sum 'C48 H90 Cu2 N8 O15 Si6' _chemical_formula_weight 1314.90 _chemical_melting_point ? _chemical_oxdiff_formula 'C15 H15 O5 Si2 N2 Cu Cl2' _chemical_oxdiff_usercomment AV_115_reluare 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' Cu Cu 0.3201 1.2651 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.423(5) _cell_length_b 10.0020(10) _cell_length_c 16.5770(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.896(10) _cell_angle_gamma 90.00 _cell_volume 7131.3(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3193 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.1834 _cell_measurement_theta_min 2.3928 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light blue' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2784 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_av_unetI/netI 0.1129 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 25327 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.40 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1593 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -21.00 11.25 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - -17.0127 -99.0000 120.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega -74.00 -36.50 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - -17.0127 -178.0000 120.0000 50 #__ type_ start__ end____ width___ exp.time_ 3 omega -25.00 3.50 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - -17.0127 -99.0000 60.0000 38 #__ type_ start__ end____ width___ exp.time_ 4 omega -6.00 76.50 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - 19.6690 38.0000 0.0000 110 #__ type_ start__ end____ width___ exp.time_ 5 omega 36.00 95.25 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - 19.6690 178.0000 -150.0000 79 #__ type_ start__ end____ width___ exp.time_ 6 omega -53.00 42.25 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - 19.6690 -38.0000 0.0000 127 #__ type_ start__ end____ width___ exp.time_ 7 omega -53.00 29.50 0.7500 60.0000 omega____ theta____ kappa____ phi______ frames - 19.6690 -19.0000 -120.0000 110 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0145998000 _diffrn_orient_matrix_UB_12 -0.0327741000 _diffrn_orient_matrix_UB_13 0.0070348000 _diffrn_orient_matrix_UB_21 0.0049693000 _diffrn_orient_matrix_UB_22 0.0357932000 _diffrn_orient_matrix_UB_23 -0.0328195000 _diffrn_orient_matrix_UB_31 0.0058186000 _diffrn_orient_matrix_UB_32 0.0517755000 _diffrn_orient_matrix_UB_33 0.0271769000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3358 _reflns_number_total 6251 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.658 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.088 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 341 _refine_ls_number_reflns 6251 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0951 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+3.3947P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2342 _refine_ls_wR_factor_ref 0.2736 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: {H8A,H8B} of C8, {H9A,H9B} of C9, {H10A,H10B} of C10, H2A of C2, H3 of C3, H4A of C4, H5 of C5, H6 of C6, H1 of C1, H2 of N2, {H15A,H15B} of C15, {H15C, H15D} of C15X, {H16A,H16B} of C16, {H16C,H16D} of C16X, {H17C,H17D,H17A,H17B} of C17, {H20A,H20B,H20C,H20D} of C20, {H21A,H21B} of C21, {H21C,H21D} of C21X, {H22A,H22B} of C22, {H22C,H22D} of C22X At 1.5 times of: {H11A,H11B,H11C} of C11, H4 of N4, H7 of O7, {H12A,H12B,H12C} of C12, {H12D, H12E,H12F} of C12X, {H13A,H13B,H13C} of C13, {H14A,H14B,H14C} of C14, {H14D, H14E,H14F} of C14X, {H23A,H23B,H23C} of C23, {H23D,H23E,H23F} of C23X, {H24A, H24B,H24C} of C24, {H24D,H24E,H24F} of C24X 2. Restrained distances Si3X-O8 = Si3-O8 1.7 with sigma of 0.02 Si3X-C22X = Si3-C22 1.85 with sigma of 0.01 C21-C20 = C21X-C20 = C21X-C22X = C21-C22 1.52 with sigma of 0.01 C16X-C17 = C16-C17 = C15-C16 = C15X-C16X 1.52 with sigma of 0.01 Si3-C24 = Si3X-C24X = Si3X-C23X = Si3-C23 1.54 with sigma of 0.01 Si3X-O8 with sigma of 0.001 Si3-O8 ~ Si3X_$1-O8 with sigma of 0.001 C21-C20 ~ C21X-C20 ~ C21X-C22X ~ C21-C22 with sigma of 0.001 Si3X-C22X ~ Si3-C22 with sigma of 0.001 C16-C17 ~ C16X-C17 ~ C15X-C16X ~ C15-C16 with sigma of 0.001 Si1-C11 ~ Si1-C12X ~ Si1-C12 ~ Si2-C13 ~ Si2-C14X with sigma of 0.001 Si3-C24 ~ Si3-C23 ~ Si3X-C24X ~ Si3X-C23X with sigma of 0.001 Si2-C15X_$2 ~ Si2-C15_$2 with sigma of 0.001 3. Uiso/Uaniso restraints and constraints Uanis(Si3X) ~ Ueq, Uanis(Si3) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uiso(C21X) = Uiso(C21) = Uiso(C22) = Uiso(C22X) Uanis(Si3) = Uanis(Si3X) Uiso(C15X) = Uiso(C15) = Uiso(C16) = Uiso(C16X) Uiso(C14) = Uiso(C14X) Uiso(C12X) = Uiso(C12) Uiso(C24X) = Uiso(C24) = Uiso(C23) = Uiso(C23X) 4. Others Fixed Sof: Si3X(0.5) Si3(0.5) O8(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C12X(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14X(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15(0.5) H15A(0.5) H15B(0.5) C15X(0.5) H15C(0.5) H15D(0.5) C16(0.5) H16A(0.5) H16B(0.5) C16X(0.5) H16C(0.5) H16D(0.5) H17C(0.5) H17D(0.5) H17A(0.5) H17B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) H20D(0.5) C21(0.5) H21A(0.5) H21B(0.5) C21X(0.5) H21C(0.5) H21D(0.5) C22(0.5) H22A(0.5) H22B(0.5) C22X(0.5) H22C(0.5) H22D(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C23X(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C24X(0.5) H24D(0.5) H24E(0.5) H24F(0.5) 5.a Riding coordinates: O7(H7), N4(H4), C12(H12A,H12B,H12C), C12X(H12D,H12E,H12F), C13(H13A,H13B, H13C), C14(H14A,H14B,H14C), C14X(H14D,H14E,H14F), C23(H23A,H23B,H23C), C23X(H23D,H23E,H23F), C24(H24A,H24B,H24C), C24X(H24D,H24E,H24F) 5.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B), C15X(H15C,H15D), C16(H16A,H16B), C16X(H16C,H16D), C17(H17C,H17D), C17(H17A,H17B), C20(H20A, H20B), C20(H20C,H20D), C21(H21A,H21B), C21X(H21C,H21D), C22(H22A,H22B), C22X(H22C,H22D) 5.c Aromatic/amide H refined with riding coordinates: N2(H2), C1(H1), C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6) 5.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cu1 Cu 0.234559(19) 0.35334(7) 0.55274(4) 0.0487(3) Uani 1 1 d . . . Si1 Si 0.41917(7) 0.1382(4) 0.6698(2) 0.1251(13) Uani 1 1 d D . . Si2 Si 0.39668(11) -0.1301(4) 0.7479(3) 0.1550(17) Uani 1 1 d D . . Si3X Si 0.4766(3) 0.5708(12) 0.5339(8) 0.174(3) Uani 0.50 1 d PDU . 2 Si3 Si 0.4767(3) 0.6303(12) 0.5134(8) 0.174(3) Uani 0.50 1 d PDU A 1 O1 O 0.27971(11) 0.3729(4) 0.5968(3) 0.0592(13) Uani 1 1 d . . . O2 O 0.30121(10) 0.2272(5) 0.5198(3) 0.0572(12) Uani 1 1 d . . . O3 O 0.28229(12) 0.0075(5) 0.8699(3) 0.0705(15) Uani 1 1 d . . . O4 O 0.30546(12) 0.1990(5) 0.8518(3) 0.0787(16) Uani 1 1 d . . . O5 O 0.4052(2) 0.0020(11) 0.7018(6) 0.189(4) Uani 1 1 d . B . O6 O 0.3461(2) 0.5899(10) 0.4767(6) 0.160(3) Uani 1 1 d . . . O7 O 0.35250(16) 0.6442(6) 0.3571(5) 0.106(2) Uani 1 1 d . . . H7 H 0.3379 0.7012 0.3565 0.159 Uiso 1 1 d R . . O8 O 0.4945(5) 0.528(2) 0.4630(13) 0.250(12) Uiso 0.50 1 d PD . . N1 N 0.22956(14) 0.2201(5) 0.6373(3) 0.0546(14) Uani 1 1 d . . . N2 N 0.23838(18) 0.0961(6) 0.7466(3) 0.0684(17) Uani 1 1 d . . . H2 H 0.2480 0.0595 0.7898 0.082 Uiso 1 1 calc R . . N3 N 0.23769(13) 0.4972(5) 0.4729(3) 0.0521(14) Uani 1 1 d . . . N4 N 0.25430(18) 0.6598(6) 0.4034(4) 0.0763(19) Uani 1 1 d . . . H4 H 0.2671 0.7278 0.3884 0.114 Uiso 1 1 d R . . C1 C 0.20338(19) 0.1519(7) 0.6478(5) 0.069(2) Uani 1 1 d . . . H1 H 0.1846 0.1568 0.6136 0.083 Uiso 1 1 calc R . . C2 C 0.2089(3) 0.0758(8) 0.7158(5) 0.085(3) Uani 1 1 d . . . H2A H 0.1948 0.0202 0.7368 0.102 Uiso 1 1 calc R . . C3 C 0.25046(18) 0.1835(7) 0.6986(4) 0.0581(18) Uani 1 1 d . . . H3 H 0.2708 0.2144 0.7073 0.070 Uiso 1 1 calc R . . C4 C 0.21321(19) 0.5498(8) 0.4208(5) 0.076(2) Uani 1 1 d . . . H4A H 0.1926 0.5212 0.4155 0.091 Uiso 1 1 calc R . . C5 C 0.2243(2) 0.6494(8) 0.3791(6) 0.088(3) Uani 1 1 d . . . H5 H 0.2128 0.7021 0.3397 0.106 Uiso 1 1 calc R . . C6 C 0.26199(17) 0.5671(7) 0.4615(4) 0.0565(18) Uani 1 1 d . . . H6 H 0.2819 0.5548 0.4895 0.068 Uiso 1 1 calc R . . C7 C 0.30249(16) 0.3110(7) 0.5763(4) 0.0492(16) Uani 1 1 d . . . C8 C 0.33393(16) 0.3421(8) 0.6234(5) 0.069(2) Uani 1 1 d . B . H8A H 0.3407 0.4281 0.6052 0.082 Uiso 1 1 calc R . . H8B H 0.3315 0.3510 0.6805 0.082 Uiso 1 1 calc R . . C9 C 0.35884(17) 0.2434(9) 0.6165(5) 0.076(2) Uani 1 1 d . . . H9A H 0.3619 0.2374 0.5598 0.092 Uiso 1 1 calc R B . H9B H 0.3518 0.1566 0.6325 0.092 Uiso 1 1 calc R . . C10 C 0.3896(2) 0.2720(11) 0.6660(6) 0.112(3) Uani 1 1 d . B . H10A H 0.3861 0.2916 0.7213 0.135 Uiso 1 1 calc R . . H10B H 0.3981 0.3520 0.6444 0.135 Uiso 1 1 calc R . . C11 C 0.4276(3) 0.1013(15) 0.5644(6) 0.185(6) Uani 1 1 d D B . H11A H 0.4096 0.0626 0.5332 0.277 Uiso 1 1 calc R . . H11B H 0.4447 0.0397 0.5670 0.277 Uiso 1 1 calc R . . H11C H 0.4329 0.1827 0.5390 0.277 Uiso 1 1 calc R . . C12 C 0.4535(6) 0.145(3) 0.7512(16) 0.189(9) Uiso 0.50 1 d PD B 2 H12A H 0.4578 0.2368 0.7666 0.283 Uiso 0.50 1 d PR B 2 H12B H 0.4714 0.1073 0.7315 0.283 Uiso 0.50 1 d PR B 2 H12C H 0.4490 0.0957 0.7978 0.283 Uiso 0.50 1 d PR B 2 C12X C 0.4552(5) 0.216(3) 0.7253(18) 0.189(9) Uiso 0.50 1 d PD B 1 H12D H 0.4604 0.2944 0.6965 0.283 Uiso 0.50 1 d PR B 1 H12E H 0.4719 0.1527 0.7280 0.283 Uiso 0.50 1 d PR B 1 H12F H 0.4518 0.2405 0.7794 0.283 Uiso 0.50 1 d PR B 1 C13 C 0.4340(3) -0.1974(18) 0.8026(11) 0.254(10) Uani 1 1 d D B . H13A H 0.4381 -0.2832 0.7804 0.382 Uiso 1 1 d R . . H13B H 0.4324 -0.2067 0.8595 0.382 Uiso 1 1 d R . . H13C H 0.4507 -0.1373 0.7958 0.382 Uiso 1 1 d R . . C14 C 0.3720(9) -0.228(3) 0.658(2) 0.206(11) Uiso 0.50 1 d P B 1 H14A H 0.3565 -0.1690 0.6299 0.309 Uiso 0.50 1 d PR B 1 H14B H 0.3620 -0.3034 0.6785 0.309 Uiso 0.50 1 d PR B 1 H14C H 0.3855 -0.2577 0.6202 0.309 Uiso 0.50 1 d PR B 1 C14X C 0.3765(8) -0.279(2) 0.697(2) 0.206(11) Uiso 0.50 1 d PD B 2 H14D H 0.3569 -0.2527 0.6677 0.309 Uiso 0.50 1 d PR B 2 H14E H 0.3733 -0.3444 0.7374 0.309 Uiso 0.50 1 d PR B 2 H14F H 0.3892 -0.3172 0.6596 0.309 Uiso 0.50 1 d PR B 2 C15 C 0.3778(4) -0.123(2) 0.8244(19) 0.154(5) Uiso 0.50 1 d PD B 1 H15A H 0.3661 -0.2062 0.8249 0.185 Uiso 0.50 1 calc PR B 1 H15B H 0.3930 -0.1232 0.8731 0.185 Uiso 0.50 1 calc PR B 1 C15X C 0.3833(3) -0.064(3) 0.8481(18) 0.154(5) Uiso 0.50 1 d PD B 2 H15C H 0.3879 -0.1288 0.8916 0.185 Uiso 0.50 1 calc PR B 2 H15D H 0.3939 0.0191 0.8649 0.185 Uiso 0.50 1 calc PR B 2 C16 C 0.3552(5) -0.009(3) 0.8328(10) 0.154(5) Uiso 0.50 1 d PD B 1 H16A H 0.3666 0.0717 0.8249 0.185 Uiso 0.50 1 calc PR B 1 H16B H 0.3393 -0.0167 0.7857 0.185 Uiso 0.50 1 calc PR B 1 C16X C 0.3484(4) -0.041(3) 0.8288(8) 0.154(5) Uiso 0.50 1 d PD B 2 H16C H 0.3378 -0.1251 0.8154 0.185 Uiso 0.50 1 calc PR B 2 H16D H 0.3439 0.0189 0.7827 0.185 Uiso 0.50 1 calc PR B 2 C17 C 0.3375(2) 0.0203(9) 0.9042(5) 0.087(3) Uani 1 1 d D . . H17C H 0.3359 -0.0476 0.9452 0.105 Uiso 0.50 1 calc PR B 2 H17D H 0.3519 0.0888 0.9273 0.105 Uiso 0.50 1 calc PR B 2 H17A H 0.3349 -0.0618 0.9337 0.105 Uiso 0.50 1 calc PR B 1 H17B H 0.3495 0.0821 0.9412 0.105 Uiso 0.50 1 calc PR B 1 C18 C 0.30611(19) 0.0799(8) 0.8751(4) 0.064(2) Uani 1 1 d . B . C19 C 0.3604(3) 0.5792(12) 0.4206(8) 0.103(3) Uani 1 1 d . . . C20 C 0.3861(3) 0.4856(11) 0.4214(10) 0.166(6) Uani 1 1 d D . . H20A H 0.3917 0.4764 0.3670 0.200 Uiso 0.50 1 calc PR C 1 H20B H 0.3801 0.3984 0.4396 0.200 Uiso 0.50 1 calc PR C 1 H20C H 0.3815 0.4272 0.3746 0.200 Uiso 0.50 1 calc PR C 2 H20D H 0.3867 0.4303 0.4696 0.200 Uiso 0.50 1 calc PR C 2 C21 C 0.4135(5) 0.539(4) 0.4790(18) 0.225(9) Uiso 0.50 1 d PD A 1 H21A H 0.4114 0.6357 0.4794 0.270 Uiso 0.50 1 calc PR A 1 H21B H 0.4110 0.5083 0.5331 0.270 Uiso 0.50 1 calc PR A 1 C21X C 0.4185(5) 0.542(4) 0.420(2) 0.225(9) Uiso 0.50 1 d PD A 2 H21C H 0.4316 0.4691 0.4070 0.270 Uiso 0.50 1 calc PR A 2 H21D H 0.4172 0.6051 0.3754 0.270 Uiso 0.50 1 calc PR A 2 C22 C 0.4469(5) 0.509(3) 0.467(2) 0.225(9) Uiso 0.50 1 d PD A 1 H22A H 0.4479 0.5051 0.4090 0.270 Uiso 0.50 1 calc PR A 1 H22B H 0.4523 0.4214 0.4894 0.270 Uiso 0.50 1 calc PR A 1 C22X C 0.4354(4) 0.612(3) 0.495(2) 0.225(9) Uiso 0.50 1 d PD A 2 H22C H 0.4234 0.5971 0.5390 0.270 Uiso 0.50 1 calc PR A 2 H22D H 0.4346 0.7071 0.4833 0.270 Uiso 0.50 1 calc PR A 2 C23 C 0.4818(10) 0.671(4) 0.6050(10) 0.261(10) Uiso 0.50 1 d PD A 1 H23A H 0.4966 0.7426 0.6133 0.391 Uiso 0.50 1 d PR A 1 H23B H 0.4896 0.5950 0.6367 0.391 Uiso 0.50 1 d PR A 1 H23C H 0.4624 0.6992 0.6216 0.391 Uiso 0.50 1 d PR A 1 C23X C 0.4768(9) 0.551(4) 0.6272(9) 0.261(10) Uiso 0.50 1 d PD D 2 H23D H 0.4678 0.6284 0.6493 0.391 Uiso 0.50 1 d PR D 2 H23E H 0.4976 0.5382 0.6541 0.391 Uiso 0.50 1 d PR D 2 H23F H 0.4644 0.4738 0.6353 0.391 Uiso 0.50 1 d PR D 2 C24 C 0.4828(12) 0.770(3) 0.478(3) 0.261(10) Uiso 0.50 1 d PD A 1 H24A H 0.4634 0.8118 0.4569 0.391 Uiso 0.50 1 d PR A 1 H24B H 0.4952 0.7602 0.4343 0.391 Uiso 0.50 1 d PR A 1 H24C H 0.4937 0.8249 0.5198 0.391 Uiso 0.50 1 d PR A 1 C24X C 0.4855(14) 0.714(3) 0.509(3) 0.261(10) Uiso 0.50 1 d PD E 2 H24D H 0.4781 0.7289 0.4527 0.391 Uiso 0.50 1 d PR E 2 H24E H 0.5077 0.7241 0.5186 0.391 Uiso 0.50 1 d PR E 2 H24F H 0.4762 0.7789 0.5415 0.391 Uiso 0.50 1 d PR E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0499(6) 0.0532(5) 0.0423(5) -0.0027(4) 0.0042(3) -0.0003(4) Si1 0.057(2) 0.211(4) 0.106(2) 0.022(2) 0.0087(16) 0.034(2) Si2 0.177(4) 0.165(4) 0.138(3) 0.029(3) 0.077(3) 0.055(3) Si3X 0.171(4) 0.198(7) 0.153(5) -0.005(5) 0.018(4) -0.064(5) Si3 0.171(4) 0.198(7) 0.153(5) -0.005(5) 0.018(4) -0.064(5) O1 0.049(3) 0.066(3) 0.060(3) -0.005(2) -0.004(2) -0.001(2) O2 0.048(3) 0.069(3) 0.052(3) -0.004(2) -0.004(2) 0.001(2) O3 0.074(4) 0.074(3) 0.063(3) 0.015(3) 0.008(3) -0.028(3) O4 0.066(4) 0.060(3) 0.108(4) 0.006(3) 0.009(3) -0.005(3) O5 0.134(8) 0.237(10) 0.215(10) 0.102(9) 0.093(7) 0.064(7) O6 0.161(9) 0.183(8) 0.135(8) 0.026(7) 0.012(7) 0.032(7) O7 0.103(6) 0.112(5) 0.105(5) 0.004(4) 0.024(4) 0.026(4) N1 0.057(4) 0.054(3) 0.053(3) -0.006(3) 0.007(3) -0.003(3) N2 0.091(6) 0.069(4) 0.044(3) 0.003(3) 0.007(3) 0.005(4) N3 0.050(4) 0.055(3) 0.052(3) -0.001(3) 0.009(3) -0.003(3) N4 0.095(6) 0.057(4) 0.076(5) 0.011(3) 0.009(4) -0.012(4) C1 0.064(6) 0.073(5) 0.067(5) 0.000(4) 0.000(4) -0.006(4) C2 0.116(9) 0.073(6) 0.069(6) 0.000(5) 0.028(5) -0.020(5) C3 0.062(5) 0.056(4) 0.055(4) -0.001(4) 0.003(4) 0.000(4) C4 0.065(6) 0.082(6) 0.077(5) 0.015(5) 0.001(4) -0.009(4) C5 0.078(7) 0.088(6) 0.096(7) 0.036(5) 0.005(5) -0.004(5) C6 0.059(5) 0.063(5) 0.048(4) -0.001(3) 0.008(3) -0.001(4) C7 0.046(5) 0.061(4) 0.041(4) 0.007(3) 0.010(3) -0.003(3) C8 0.041(5) 0.099(6) 0.062(5) -0.007(4) -0.006(3) -0.001(4) C9 0.039(5) 0.117(7) 0.071(5) -0.008(5) -0.002(4) 0.001(4) C10 0.061(7) 0.177(10) 0.093(7) -0.006(7) -0.012(5) -0.024(6) C11 0.176(14) 0.246(16) 0.149(12) 0.039(11) 0.083(10) 0.079(12) C13 0.28(3) 0.240(18) 0.23(2) 0.115(16) -0.009(17) 0.064(17) C17 0.085(7) 0.086(6) 0.097(6) 0.019(5) 0.035(5) -0.003(5) C18 0.068(6) 0.070(5) 0.059(5) 0.008(4) 0.026(4) 0.013(5) C19 0.100(9) 0.112(8) 0.095(9) 0.004(7) 0.009(7) 0.011(7) C20 0.118(11) 0.098(8) 0.273(18) -0.004(10) -0.011(11) 0.025(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 2.005(5) . ? Cu1 O2 1.999(4) 7_556 ? Cu1 O3 2.194(5) 4_556 ? Cu1 N1 1.967(6) . ? Cu1 N3 1.972(5) . ? Si1 O5 1.611(10) . ? Si1 C10 1.850(11) . ? Si1 C11 1.871(8) . ? Si1 C12 1.871(8) . ? Si1 C12X 1.871(8) . ? Si2 O5 1.595(10) . ? Si2 C13 1.871(8) . ? Si2 C14 1.98(3) . ? Si2 C14X 1.871(8) . ? Si2 C15 1.60(3) . ? Si2 C15X 1.95(3) . ? Si3X O8 1.591(9) 5_666 ? Si3X C22X 1.861(7) . ? Si3X C23X 1.557(5) . ? Si3X C24X 1.557(5) . ? Si3 O8 1.591(9) . ? Si3 C22 1.861(7) . ? Si3 C23 1.557(5) . ? Si3 C24 1.557(5) . ? O1 C7 1.253(8) . ? O2 Cu1 1.999(4) 7_556 ? O2 C7 1.253(7) . ? O3 Cu1 2.194(5) 4_546 ? O3 C18 1.256(9) . ? O4 C18 1.251(9) . ? O6 C19 1.189(12) . ? O7 C19 1.244(12) . ? O8 Si3X 1.591(9) 5_666 ? O8 Si3 2.02(3) 5_666 ? N1 C1 1.357(9) . ? N1 C3 1.318(8) . ? N2 C2 1.327(10) . ? N2 C3 1.337(9) . ? N3 C4 1.379(9) . ? N3 C6 1.302(8) . ? N4 C5 1.313(10) . ? N4 C6 1.345(9) . ? C1 C2 1.354(10) . ? C4 C5 1.340(10) . ? C7 C8 1.508(9) . ? C8 C9 1.480(10) . ? C9 C10 1.495(10) . ? C15 C16 1.524(5) . ? C15X C16X 1.524(5) . ? C16 C17 1.524(5) . ? C16X C17 1.524(5) . ? C17 C18 1.506(10) . ? C19 C20 1.457(14) . ? C20 C21 1.517(5) . ? C20 C21X 1.517(5) . ? C21 C22 1.517(5) . ? C21X C22X 1.517(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O3 96.11(19) . 4_556 ? O2 Cu1 O1 153.97(19) 7_556 . ? O2 Cu1 O3 109.9(2) 7_556 4_556 ? N1 Cu1 O1 90.3(2) . . ? N1 Cu1 O2 90.2(2) . 7_556 ? N1 Cu1 O3 88.9(2) . 4_556 ? N1 Cu1 N3 175.3(2) . . ? N3 Cu1 O1 91.1(2) . . ? N3 Cu1 O2 90.6(2) . 7_556 ? N3 Cu1 O3 86.5(2) . 4_556 ? O5 Si1 C10 109.4(5) . . ? O5 Si1 C11 105.8(7) . . ? O5 Si1 C12 95.4(11) . . ? O5 Si1 C12X 121.2(11) . . ? C10 Si1 C11 109.5(5) . . ? C10 Si1 C12 118.6(11) . . ? C10 Si1 C12X 104.2(11) . . ? C11 Si1 C12X 106.5(12) . . ? C12 Si1 C11 116.2(12) . . ? C12 Si1 C12X 25.8(14) . . ? O5 Si2 C13 106.7(7) . . ? O5 Si2 C14 100.6(11) . . ? O5 Si2 C14X 124.6(12) . . ? O5 Si2 C15 121.4(9) . . ? O5 Si2 C15X 104.0(10) . . ? C13 Si2 C14 122.2(13) . . ? C13 Si2 C14X 104.6(13) . . ? C13 Si2 C15X 92.8(8) . . ? C14X Si2 C14 24.8(16) . . ? C14X Si2 C15X 118.8(15) . . ? C15 Si2 C13 97.8(10) . . ? C15 Si2 C14 109.7(15) . . ? C15 Si2 C14X 97.6(15) . . ? C15 Si2 C15X 21.2(11) . . ? C15X Si2 C14 128.3(14) . . ? O8 Si3X C22X 149.7(17) 5_666 . ? C23X Si3X O8 89.7(17) . 5_666 ? C23X Si3X C22X 104(2) . . ? C24X Si3X O8 111(3) . 5_666 ? C24X Si3X C22X 88(3) . . ? C24X Si3X C23X 114(3) . . ? O8 Si3 C22 73.9(13) . . ? C23 Si3 O8 132(2) . . ? C23 Si3 C22 125(2) . . ? C23 Si3 C24 97(3) . . ? C24 Si3 O8 105(3) . . ? C24 Si3 C22 125(2) . . ? C7 O1 Cu1 128.5(4) . . ? C7 O2 Cu1 132.1(5) . 7_556 ? C18 O3 Cu1 134.7(5) . 4_546 ? Si2 O5 Si1 168.8(8) . . ? Si3X O8 Si3 17.2(7) 5_666 5_666 ? Si3X O8 Si3 145.3(19) 5_666 . ? Si3 O8 Si3 137.5(14) . 5_666 ? C1 N1 Cu1 127.5(5) . . ? C3 N1 Cu1 127.3(5) . . ? C3 N1 C1 105.2(6) . . ? C2 N2 C3 107.9(6) . . ? C4 N3 Cu1 125.5(5) . . ? C6 N3 Cu1 128.5(5) . . ? C6 N3 C4 105.9(6) . . ? C5 N4 C6 107.7(7) . . ? C2 C1 N1 109.5(7) . . ? N2 C2 C1 106.6(7) . . ? N1 C3 N2 110.8(7) . . ? C5 C4 N3 107.8(7) . . ? N4 C5 C4 108.2(8) . . ? N3 C6 N4 110.4(7) . . ? O1 C7 C8 116.8(6) . . ? O2 C7 O1 125.3(6) . . ? O2 C7 C8 118.0(6) . . ? C9 C8 C7 116.2(6) . . ? C8 C9 C10 116.0(7) . . ? C9 C10 Si1 116.4(7) . . ? C16 C15 Si2 120.6(18) . . ? C16X C15X Si2 106.0(14) . . ? C17 C16 C15 127.9(19) . . ? C15X C16X C17 107.4(13) . . ? C16 C17 C16X 16.3(19) . . ? C18 C17 C16 111.0(10) . . ? C18 C17 C16X 105.4(8) . . ? O3 C18 C17 119.7(7) . . ? O4 C18 O3 123.0(7) . . ? O4 C18 C17 117.2(7) . . ? O6 C19 O7 120.1(12) . . ? O6 C19 C20 122.1(13) . . ? O7 C19 C20 117.7(12) . . ? C19 C20 C21 108.2(15) . . ? C19 C20 C21X 118.1(18) . . ? C21X C20 C21 39.5(17) . . ? C22 C21 C20 121.9(18) . . ? C22X C21X C20 121(2) . . ? C21 C22 Si3 116.1(16) . . ? C21X C22X Si3X 121(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O4 0.85 1.72 2.567(8) 173.1 6_565 N2 H2 O3 0.86 1.93 2.744(8) 158.6 . N4 H4 O4 0.93 1.99 2.861(9) 154.7 6_565 _database_code_depnum_ccdc_archive 'CCDC 919581'