# 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_x1268fin _database_code_depnum_ccdc_archive 'CCDC 904635' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2012-08-15T14:54:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C61.50 H69.50 N4.50 O24.50 Zn4' _chemical_formula_weight 1525.2 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.6899(4) _cell_length_b 23.6899(4) _cell_length_c 30.8058(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 14972.3(5) _cell_formula_units_Z 6 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 21046 _cell_measurement_theta_min 2.9351 _cell_measurement_theta_max 28.855 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4716 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.95757 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0232381 _diffrn_orient_matrix_ub_12 -0.0170265 _diffrn_orient_matrix_ub_13 0.0165374 _diffrn_orient_matrix_ub_21 -0.0029711 _diffrn_orient_matrix_ub_22 -0.0297594 _diffrn_orient_matrix_ub_23 -0.007325 _diffrn_orient_matrix_ub_31 0.0254424 _diffrn_orient_matrix_ub_32 0.0044402 _diffrn_orient_matrix_ub_33 0.014222 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_number 62800 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6809 _reflns_number_gt 5693 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+19.3668P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6809 _refine_ls_number_parameters 339 _refine_ls_number_restraints 200 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.14 _refine_ls_wR_factor_gt 0.135 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.511 _refine_diff_density_min -0.64 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn1 Zn 0 0 0.246531(16) 0.03925(16) Uani 1 3 d S . . Zn2 Zn -0.043495(13) -0.087015(13) 0.159241(8) 0.02725(11) Uani 1 1 d D . . O1 O -0.0255(5) -0.0926(4) 0.2558(3) 0.120(5) Uani 0.493(6) 1 d PD A 1 O2 O -0.0744(18) -0.1580(7) 0.2008(4) 0.044(3) Uani 0.493(6) 1 d PD A 1 O3 O -0.2000(11) -0.3833(7) 0.2690(8) 0.068(4) Uani 0.493(6) 1 d PD A 1 O4 O -0.3259(4) -0.5480(5) 0.4572(3) 0.0355(12) Uani 0.493(6) 1 d PD . 1 O5 O -0.2285(8) -0.5413(6) 0.4620(4) 0.0505(16) Uani 0.493(6) 1 d PD A 1 O6 O -0.2681(4) -0.3479(3) 0.3694(2) 0.111(3) Uani 0.493(6) 1 d PD A 1 C1 C -0.0616(5) -0.1472(5) 0.2399(4) 0.057(3) Uani 0.493(6) 1 d PD A 1 C2 C -0.0932(6) -0.2049(5) 0.2698(4) 0.073(3) Uani 0.493(6) 1 d PD A 1 C3 C -0.1322(8) -0.2672(6) 0.2537(4) 0.0561(9) Uani 0.493(6) 1 d PD A 1 H3 H -0.1395 -0.2739 0.2233 0.067 Uiso 0.493(6) 1 calc PR A 1 C4 C -0.1607(7) -0.3196(6) 0.2817(4) 0.0540(8) Uani 0.493(6) 1 d PD A 1 C5 C -0.1497(6) -0.3098(5) 0.3261(4) 0.0789(17) Uani 0.493(6) 1 d PD A 1 C6 C -0.1110(7) -0.2478(6) 0.3411(3) 0.136(7) Uani 0.493(6) 1 d PD A 1 H6 H -0.1039 -0.2405 0.3715 0.164 Uiso 0.493(6) 1 calc PR A 1 C7 C -0.0821(8) -0.1956(6) 0.3131(4) 0.120(7) Uani 0.493(6) 1 d PD A 1 H7 H -0.0544 -0.153 0.3241 0.143 Uiso 0.493(6) 1 calc PR A 1 C8 C -0.198(5) -0.395(2) 0.2229(11) 0.111(3) Uani 0.493(6) 1 d PD A 1 H8A H -0.2235 -0.4421 0.2172 0.166 Uiso 0.493(6) 1 calc PR A 1 H8B H -0.1532 -0.378 0.2136 0.166 Uiso 0.493(6) 1 calc PR A 1 H8C H -0.2176 -0.3732 0.2067 0.166 Uiso 0.493(6) 1 calc PR A 1 C9 C -0.2667(6) -0.5246(5) 0.4471(4) 0.0446(13) Uani 0.493(6) 1 d PD A 1 C10 C -0.2354(6) -0.4687(5) 0.4161(4) 0.0602(9) Uani 0.493(6) 1 d PD A 1 C11 C -0.2653(6) -0.4332(6) 0.4074(4) 0.072(4) Uani 0.493(6) 1 d PD A 1 H11 H -0.3051 -0.4439 0.4214 0.087 Uiso 0.493(6) 1 calc PR A 1 C12 C -0.2378(6) -0.3816(5) 0.3781(3) 0.081(5) Uani 0.493(6) 1 d PD A 1 C13 C -0.1801(5) -0.3660(5) 0.3574(4) 0.0798(14) Uani 0.493(6) 1 d PD A 1 C14 C -0.1492(6) -0.4003(5) 0.3676(4) 0.088(5) Uani 0.493(6) 1 d PD A 1 H14 H -0.1084 -0.3885 0.3546 0.105 Uiso 0.493(6) 1 calc PR A 1 C15 C -0.1763(6) -0.4514(6) 0.3964(4) 0.081(5) Uani 0.493(6) 1 d PD A 1 H15 H -0.1545 -0.4749 0.4029 0.097 Uiso 0.493(6) 1 calc PR A 1 C16 C -0.3273(7) -0.3629(7) 0.3931(5) 0.136(6) Uani 0.493(6) 1 d PD A 1 H16A H -0.3442 -0.3352 0.3824 0.204 Uiso 0.493(6) 1 calc PR A 1 H16B H -0.3174 -0.3548 0.4241 0.204 Uiso 0.493(6) 1 calc PR A 1 H16C H -0.3601 -0.4088 0.3886 0.204 Uiso 0.493(6) 1 calc PR A 1 O1F O -0.0666(6) -0.0919(4) 0.2560(3) 0.125(5) Uani 0.507(6) 1 d PD A 2 O2F O -0.0830(17) -0.1569(7) 0.2020(4) 0.044(3) Uani 0.507(6) 1 d PD A 2 O3F O -0.1830(10) -0.3820(7) 0.2700(8) 0.068(4) Uani 0.507(6) 1 d PD A 2 O4F O -0.2223(7) -0.5481(4) 0.4572(3) 0.0355(12) Uani 0.507(6) 1 d PD A 2 O5F O -0.3130(4) -0.5417(6) 0.4619(4) 0.0505(16) Uani 0.507(6) 1 d PD . 2 O6F O -0.0797(3) -0.3484(3) 0.3694(2) 0.111(3) Uani 0.507(6) 1 d PD A 2 C1F C -0.0843(5) -0.1462(5) 0.2414(4) 0.057(3) Uani 0.507(6) 1 d PD A 2 C2F C -0.1107(6) -0.2036(5) 0.2715(4) 0.073(3) Uani 0.507(6) 1 d PD A 2 C3F C -0.1340(7) -0.2657(6) 0.2551(4) 0.0561(9) Uani 0.507(6) 1 d PD A 2 H3F H -0.1333 -0.272 0.2247 0.067 Uiso 0.507(6) 1 calc PR A 2 C4F C -0.1584(6) -0.3184(5) 0.2828(4) 0.0540(8) Uani 0.507(6) 1 d PD A 2 C5F C -0.1595(6) -0.3090(5) 0.3273(3) 0.0789(17) Uani 0.507(6) 1 d PD A 2 C6F C -0.1357(7) -0.2472(6) 0.3429(4) 0.143(8) Uani 0.507(6) 1 d PD A 2 H6F H -0.1354 -0.2404 0.3733 0.172 Uiso 0.507(6) 1 calc PR A 2 C7F C -0.1120(8) -0.1946(6) 0.3151(4) 0.125(8) Uani 0.507(6) 1 d PD A 2 H7F H -0.0966 -0.152 0.3264 0.15 Uiso 0.507(6) 1 calc PR A 2 C8F C -0.196(5) -0.394(2) 0.2240(10) 0.111(3) Uani 0.507(6) 1 d PD A 2 H8F1 H -0.2077 -0.4396 0.2176 0.166 Uiso 0.507(6) 1 calc PR A 2 H8F2 H -0.1566 -0.3648 0.2075 0.166 Uiso 0.507(6) 1 calc PR A 2 H8F3 H -0.2317 -0.3874 0.2156 0.166 Uiso 0.507(6) 1 calc PR A 2 C9F C -0.2579(6) -0.5245(5) 0.4471(4) 0.0446(13) Uani 0.507(6) 1 d PD A 2 C10F C -0.2332(6) -0.4685(5) 0.4163(4) 0.0602(9) Uani 0.507(6) 1 d PD A 2 C11F C -0.1681(6) -0.4334(5) 0.4075(4) 0.069(4) Uani 0.507(6) 1 d PD A 2 H11F H -0.1391 -0.4445 0.4213 0.083 Uiso 0.507(6) 1 calc PR A 2 C12F C -0.1438(6) -0.3817(4) 0.3784(3) 0.077(4) Uani 0.507(6) 1 d PD A 2 C13F C -0.1855(5) -0.3654(5) 0.3581(3) 0.0798(14) Uani 0.507(6) 1 d PD A 2 C14F C -0.2507(6) -0.3989(5) 0.3683(4) 0.094(5) Uani 0.507(6) 1 d PD A 2 H14F H -0.2793 -0.3864 0.3555 0.113 Uiso 0.507(6) 1 calc PR A 2 C15F C -0.2749(6) -0.4504(6) 0.3971(4) 0.086(5) Uani 0.507(6) 1 d PD A 2 H15F H -0.3201 -0.4735 0.4039 0.103 Uiso 0.507(6) 1 calc PR A 2 C16F C -0.0355(5) -0.3637(7) 0.3930(5) 0.144(6) Uani 0.507(6) 1 d PD A 2 H16D H 0.009 -0.3363 0.3823 0.217 Uiso 0.507(6) 1 calc PR A 2 H16E H -0.0489 -0.4097 0.3886 0.217 Uiso 0.507(6) 1 calc PR A 2 H16F H -0.0371 -0.3555 0.4241 0.217 Uiso 0.507(6) 1 calc PR A 2 O7 O 0 0 0.18190(8) 0.0236(5) Uani 1 3 d S . . O8 O 0 0 0.3171(2) 0.150(3) Uani 1 3 d S A . H8X H 0.0231 -0.022 0.3277 0.224 Uiso 0.22 1 calc PR . . H8Y H -0.045 -0.0231 0.3277 0.224 Uiso 0.22 1 calc PR . . H8Z H 0.022 0.045 0.3277 0.224 Uiso 0.22 1 calc 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 Zn1 0.0456(2) 0.0456(2) 0.0265(3) 0 0 0.02282(11) Zn2 0.03092(17) 0.02663(17) 0.02282(16) 0.00094(10) 0.00042(10) 0.01334(12) O1 0.169(9) 0.041(4) 0.071(5) 0.021(3) -0.073(6) -0.008(5) O2 0.056(7) 0.0379(11) 0.0334(11) 0.0128(9) 0.0086(15) 0.0204(16) O3 0.074(10) 0.0382(14) 0.077(2) 0.0114(13) 0.003(5) 0.016(3) O4 0.036(3) 0.032(2) 0.038(2) 0.0138(17) 0.0063(16) 0.0166(17) O5 0.046(3) 0.054(3) 0.054(3) 0.022(3) 0.012(2) 0.027(2) O6 0.146(7) 0.092(5) 0.119(6) 0.063(4) 0.026(5) 0.079(5) C1 0.077(7) 0.0364(18) 0.045(2) 0.0137(15) 0.013(4) 0.019(3) C2 0.122(7) 0.0388(19) 0.0344(19) 0.0132(15) 0.011(3) 0.022(3) C3 0.077(2) 0.0394(17) 0.0412(17) 0.0123(13) 0.0078(16) 0.0216(16) C4 0.066(2) 0.0341(16) 0.0528(19) 0.0140(13) 0.0072(15) 0.0185(15) C5 0.113(4) 0.045(2) 0.056(2) 0.0232(17) 0.013(3) 0.022(2) C6 0.27(2) 0.055(8) 0.032(6) 0.020(5) -0.011(8) 0.039(10) C7 0.187(17) 0.044(6) 0.062(8) 0.007(5) 0.002(8) 0.008(7) C8 0.158(8) 0.051(3) 0.088(4) -0.012(2) -0.005(4) 0.026(3) C9 0.046(3) 0.0440(16) 0.0430(16) 0.0175(13) 0.0084(17) 0.0219(18) C10 0.069(2) 0.0492(19) 0.057(2) 0.0265(15) 0.0138(17) 0.0248(17) C11 0.099(10) 0.059(7) 0.065(6) 0.023(5) 0.033(6) 0.044(7) C12 0.124(13) 0.052(7) 0.074(6) 0.022(5) 0.026(7) 0.048(8) C13 0.104(4) 0.056(2) 0.064(2) 0.0320(19) 0.016(2) 0.029(2) C14 0.103(10) 0.050(7) 0.113(11) 0.047(7) 0.057(8) 0.040(7) C15 0.071(8) 0.061(8) 0.109(11) 0.046(7) 0.040(8) 0.031(7) C16 0.130(11) 0.132(11) 0.183(14) 0.086(10) 0.040(10) 0.092(9) O1F 0.242(12) 0.044(4) 0.072(5) 0.023(3) 0.097(7) 0.058(6) O2F 0.056(7) 0.0379(11) 0.0334(11) 0.0128(9) 0.0086(15) 0.0204(16) O3F 0.074(10) 0.0382(14) 0.077(2) 0.0114(13) 0.003(5) 0.016(3) O4F 0.036(3) 0.032(2) 0.038(2) 0.0138(17) 0.0063(16) 0.0166(17) O5F 0.046(3) 0.054(3) 0.054(3) 0.022(3) 0.012(2) 0.027(2) O6F 0.089(5) 0.093(5) 0.115(5) 0.062(4) 0.040(4) 0.019(4) C1F 0.077(7) 0.0364(18) 0.045(2) 0.0137(15) 0.013(4) 0.019(3) C2F 0.122(7) 0.0388(19) 0.0344(19) 0.0132(15) 0.011(3) 0.022(3) C3F 0.077(2) 0.0394(17) 0.0412(17) 0.0123(13) 0.0078(16) 0.0216(16) C4F 0.066(2) 0.0341(16) 0.0528(19) 0.0140(13) 0.0072(15) 0.0185(15) C5F 0.113(4) 0.045(2) 0.056(2) 0.0232(17) 0.013(3) 0.022(2) C6F 0.250(19) 0.045(7) 0.055(8) 0.014(6) 0.051(10) 0.014(9) C7F 0.24(2) 0.047(6) 0.041(6) 0.010(4) 0.026(8) 0.041(9) C8F 0.158(8) 0.051(3) 0.088(4) -0.012(2) -0.005(4) 0.026(3) C9F 0.046(3) 0.0440(16) 0.0430(16) 0.0175(13) 0.0084(17) 0.0219(18) C10F 0.069(2) 0.0492(19) 0.057(2) 0.0265(15) 0.0138(17) 0.0248(17) C11F 0.066(6) 0.049(6) 0.068(6) 0.022(5) -0.012(5) 0.010(5) C12F 0.075(7) 0.046(6) 0.067(6) 0.023(5) 0.000(5) -0.002(5) C13F 0.104(4) 0.056(2) 0.064(2) 0.0320(19) 0.016(2) 0.029(2) C14F 0.081(7) 0.052(7) 0.116(10) 0.054(7) -0.013(7) 0.009(5) C15F 0.074(7) 0.062(7) 0.118(11) 0.055(8) 0.011(7) 0.031(5) C16F 0.075(7) 0.142(11) 0.202(15) 0.098(11) 0.045(8) 0.044(7) O7 0.0258(8) 0.0258(8) 0.0193(12) 0 0 0.0129(4) O8 0.195(5) 0.195(5) 0.059(4) 0 0 0.097(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1F 1.969(8) 2 ? Zn1 O1F 1.969(8) 3 ? Zn1 O1F 1.969(8) . ? Zn1 O1 1.983(8) 2 ? Zn1 O1 1.983(8) 3 ? Zn1 O1 1.983(8) . ? Zn1 O7 1.991(3) . ? Zn1 O8 2.175(6) . ? Zn2 O4F 1.914(7) 9_544 ? Zn2 O4 1.915(7) 8_444 ? Zn2 O7 1.9168(9) . ? Zn2 O2 1.942(10) . ? Zn2 O2F 1.949(10) . ? Zn2 O5F 1.998(8) 8_444 ? Zn2 O5 2.001(8) 9_544 ? Zn2 Zn2 3.0921(5) 2 ? Zn2 Zn2 3.0921(5) 3 ? O1 C1 1.241(10) . ? O2 C1 1.237(11) . ? O3 C4 1.376(10) . ? O3 C8 1.450(17) . ? O4 C9 1.263(9) . ? O4 Zn2 1.915(7) 6_445 ? O5 C9 1.244(10) . ? O5 Zn2 2.001(8) 5_445 ? O6 C12 1.340(13) . ? O6 C16 1.460(12) . ? C1 C2 1.501(9) . ? C2 C7 1.356(9) . ? C2 C3 1.383(9) . ? C3 C4 1.379(8) . ? C4 C5 1.392(8) . ? C5 C6 1.366(9) . ? C5 C13 1.502(9) . ? C6 C7 1.377(9) . ? C9 C10 1.493(9) . ? C10 C11 1.369(11) . ? C10 C15 1.386(11) . ? C11 C12 1.391(10) . ? C12 C13 1.380(11) . ? C13 C14 1.377(11) . ? C14 C15 1.374(10) . ? O1F C1F 1.223(9) . ? O2F C1F 1.243(11) . ? O3F C4F 1.375(10) . ? O3F C8F 1.448(17) . ? O4F C9F 1.262(9) . ? O4F Zn2 1.914(7) 5_445 ? O5F C9F 1.243(9) . ? O5F Zn2 1.998(8) 6_445 ? O6F C12F 1.346(13) . ? O6F C16F 1.462(12) . ? C1F C2F 1.501(9) . ? C2F C7F 1.362(9) . ? C2F C3F 1.382(8) . ? C3F C4F 1.378(8) . ? C4F C5F 1.390(8) . ? C5F C6F 1.367(9) . ? C5F C13F 1.498(9) . ? C6F C7F 1.380(9) . ? C9F C10F 1.492(9) . ? C10F C11F 1.364(11) . ? C10F C15F 1.391(11) . ? C11F C12F 1.388(10) . ? C12F C13F 1.377(11) . ? C13F C14F 1.376(11) . ? C14F C15F 1.382(10) . ? O7 Zn2 1.9168(9) 2 ? O7 Zn2 1.9168(9) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1F Zn1 O1F 117.84(12) 2 3 ? O1F Zn1 O1F 117.84(12) 2 . ? O1F Zn1 O1F 117.84(12) 3 . ? O1F Zn1 O1 28.8(4) 2 2 ? O1F Zn1 O1 89.7(4) 3 2 ? O1F Zn1 O1 144.9(4) . 2 ? O1F Zn1 O1 144.9(4) 2 3 ? O1F Zn1 O1 28.8(4) 3 3 ? O1F Zn1 O1 89.7(4) . 3 ? O1 Zn1 O1 117.97(12) 2 3 ? O1F Zn1 O1 89.7(4) 2 . ? O1F Zn1 O1 144.9(4) 3 . ? O1F Zn1 O1 28.8(4) . . ? O1 Zn1 O1 117.97(12) 2 . ? O1 Zn1 O1 117.97(12) 3 . ? O1F Zn1 O7 98.5(2) 2 . ? O1F Zn1 O7 98.5(2) 3 . ? O1F Zn1 O7 98.5(2) . . ? O1 Zn1 O7 98.3(2) 2 . ? O1 Zn1 O7 98.3(2) 3 . ? O1 Zn1 O7 98.3(2) . . ? O1F Zn1 O8 81.5(2) 2 . ? O1F Zn1 O8 81.5(2) 3 . ? O1F Zn1 O8 81.5(2) . . ? O1 Zn1 O8 81.7(2) 2 . ? O1 Zn1 O8 81.7(2) 3 . ? O1 Zn1 O8 81.7(2) . . ? O7 Zn1 O8 180.0000(10) . . ? O4F Zn2 O4 102.6(3) 9_544 8_444 ? O4F Zn2 O7 116.6(4) 9_544 . ? O4 Zn2 O7 116.7(4) 8_444 . ? O4F Zn2 O2 97.9(11) 9_544 . ? O4 Zn2 O2 103.0(11) 8_444 . ? O7 Zn2 O2 117.3(5) . . ? O4F Zn2 O2F 103.8(10) 9_544 . ? O4 Zn2 O2F 98.7(11) 8_444 . ? O7 Zn2 O2F 116.0(4) . . ? O2 Zn2 O2F 7(2) . . ? O4F Zn2 O5F 110.9(3) 9_544 8_444 ? O4 Zn2 O5F 8.5(3) 8_444 8_444 ? O7 Zn2 O5F 109.9(4) . 8_444 ? O2 Zn2 O5F 103.0(12) . 8_444 ? O2F Zn2 O5F 98.0(11) . 8_444 ? O4F Zn2 O5 8.5(3) 9_544 9_544 ? O4 Zn2 O5 110.9(3) 8_444 9_544 ? O7 Zn2 O5 110.0(4) . 9_544 ? O2 Zn2 O5 97.1(12) . 9_544 ? O2F Zn2 O5 103.4(12) . 9_544 ? O5F Zn2 O5 119.2(4) 8_444 9_544 ? O4F Zn2 Zn2 80.4(4) 9_544 2 ? O4 Zn2 Zn2 127.9(5) 8_444 2 ? O7 Zn2 Zn2 36.24(4) . 2 ? O2 Zn2 Zn2 128.4(9) . 2 ? O2F Zn2 Zn2 131.6(8) . 2 ? O5F Zn2 Zn2 126.0(5) 8_444 2 ? O5 Zn2 Zn2 74.2(4) 9_544 2 ? O4F Zn2 Zn2 127.9(5) 9_544 3 ? O4 Zn2 Zn2 80.5(4) 8_444 3 ? O7 Zn2 Zn2 36.24(4) . 3 ? O2 Zn2 Zn2 132.7(8) . 3 ? O2F Zn2 Zn2 127.5(8) . 3 ? O5F Zn2 Zn2 74.1(4) 8_444 3 ? O5 Zn2 Zn2 126.2(5) 9_544 3 ? Zn2 Zn2 Zn2 60 2 3 ? C1 O1 Zn1 140.0(7) . . ? C1 O2 Zn2 121.0(11) . . ? C4 O3 C8 114.9(19) . . ? C9 O4 Zn2 126.4(7) . 6_445 ? C9 O5 Zn2 130.4(10) . 5_445 ? C12 O6 C16 119.4(8) . . ? O2 C1 O1 124.7(12) . . ? O2 C1 C2 116.8(9) . . ? O1 C1 C2 118.5(8) . . ? C7 C2 C3 119.8(7) . . ? C7 C2 C1 119.2(7) . . ? C3 C2 C1 120.9(7) . . ? C4 C3 C2 120.1(7) . . ? O3 C4 C3 124.6(12) . . ? O3 C4 C5 115.5(12) . . ? C3 C4 C5 119.9(7) . . ? C6 C5 C4 118.8(6) . . ? C6 C5 C13 120.2(7) . . ? C4 C5 C13 121.0(7) . . ? C5 C6 C7 121.2(7) . . ? C2 C7 C6 120.2(8) . . ? O5 C9 O4 126.5(9) . . ? O5 C9 C10 113.6(8) . . ? O4 C9 C10 119.8(8) . . ? C11 C10 C15 119.2(7) . . ? C11 C10 C9 119.4(7) . . ? C15 C10 C9 121.5(7) . . ? C10 C11 C12 120.6(8) . . ? O6 C12 C13 120.0(9) . . ? O6 C12 C11 119.9(10) . . ? C13 C12 C11 120.1(8) . . ? C14 C13 C12 118.9(7) . . ? C14 C13 C5 120.6(8) . . ? C12 C13 C5 120.4(8) . . ? C15 C14 C13 121.1(8) . . ? C14 C15 C10 120.1(8) . . ? C1F O1F Zn1 140.6(7) . . ? C1F O2F Zn2 122.5(11) . . ? C4F O3F C8F 115.8(19) . . ? C9F O4F Zn2 126.7(7) . 5_445 ? C9F O5F Zn2 130.8(9) . 6_445 ? C12F O6F C16F 119.3(7) . . ? O1F C1F O2F 122.9(11) . . ? O1F C1F C2F 119.6(8) . . ? O2F C1F C2F 117.5(8) . . ? C7F C2F C3F 120.0(7) . . ? C7F C2F C1F 120.0(7) . . ? C3F C2F C1F 120.0(7) . . ? C4F C3F C2F 120.1(7) . . ? O3F C4F C3F 124.9(11) . . ? O3F C4F C5F 115.3(11) . . ? C3F C4F C5F 119.9(7) . . ? C6F C5F C4F 119.2(7) . . ? C6F C5F C13F 119.8(7) . . ? C4F C5F C13F 120.9(7) . . ? C5F C6F C7F 120.8(8) . . ? C2F C7F C6F 120.1(8) . . ? O5F C9F O4F 126.2(9) . . ? O5F C9F C10F 113.9(7) . . ? O4F C9F C10F 119.9(7) . . ? C11F C10F C15F 119.3(7) . . ? C11F C10F C9F 119.3(7) . . ? C15F C10F C9F 121.3(7) . . ? C10F C11F C12F 120.6(8) . . ? O6F C12F C13F 119.9(8) . . ? O6F C12F C11F 119.9(10) . . ? C13F C12F C11F 120.2(8) . . ? C14F C13F C12F 119.3(6) . . ? C14F C13F C5F 120.0(8) . . ? C12F C13F C5F 120.5(8) . . ? C13F C14F C15F 120.5(8) . . ? C14F C15F C10F 120.0(8) . . ? Zn2 O7 Zn2 107.53(7) . 2 ? Zn2 O7 Zn2 107.53(7) . 3 ? Zn2 O7 Zn2 107.53(7) 2 3 ? Zn2 O7 Zn1 111.35(7) . . ? Zn2 O7 Zn1 111.35(7) 2 . ? Zn2 O7 Zn1 111.35(7) 3 . ? # 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 0.000 202 41 ' 1 dmf ' 2 -0.014 0.466 -0.008 7314 973 ' 24 dmf ' 3 0.333 0.667 0.667 201 41 ' 1 dmf ' 4 0.667 0.333 0.333 201 41 ' 1 dmf ' _platon_squeeze_details ; The crystals were grown from dmf (undried). The SQUEEZE analysis reveal approximately 27 molecules of dmf for the unit cell, i.e. 4.5 molecules of dmf for the asymmetric unit. However, small amounts of water may be expected as well, because the solvent was taken undried. For this structure determination dmf was only taken into account. ; data_x0748fin _database_code_depnum_ccdc_archive 'CCDC 904636' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2010-07-08T16:33:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C200 H240 Cd7 Cl2 N16 O68' _chemical_formula_weight 4813.78 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' '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+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 22.3139(2) _cell_length_b 22.3139(2) _cell_length_c 43.2016(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 21510.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 11596 _cell_measurement_theta_min 2.5771 _cell_measurement_theta_max 28.8177 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9864 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.8897 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_ub_11 -0.0216926169 _diffrn_orient_matrix_ub_12 0.0148207752 _diffrn_orient_matrix_ub_13 -0.0092309013 _diffrn_orient_matrix_ub_21 0.018802106 _diffrn_orient_matrix_ub_22 0.0255890969 _diffrn_orient_matrix_ub_23 -0.0008320795 _diffrn_orient_matrix_ub_31 0.0136696252 _diffrn_orient_matrix_ub_32 -0.011693879 _diffrn_orient_matrix_ub_33 -0.0135503967 _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_unetI/netI 0.1712 _diffrn_reflns_number 78757 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 10987 _reflns_number_gt 5182 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^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_number_reflns 10987 _refine_ls_number_parameters 576 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_diff_density_max 0.54 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.5 0 0.75 0.0600(4) Uani 1 4 d S . . Cd2 Cd 0.86572(3) 0.86809(3) 0.676095(11) 0.03529(15) Uani 1 1 d . . . Cd3 Cd 0.86336(4) 0.75 0.625 0.0366(2) Uani 1 2 d S . . Cl1 Cl 0.8289(11) 0.8134(10) 0.7685(6) 0.404(12) Uiso 0.5 1 d P . . O1 O 0.5881(3) -0.0292(4) 0.77351(16) 0.084(2) Uani 1 1 d . . . O2 O 0.5502(4) 0.0512(4) 0.79492(15) 0.072(2) Uani 1 1 d . . . O3 O 0.7599(4) -0.0822(3) 0.84416(18) 0.091(2) Uani 1 1 d . . . O4 O 0.8249(3) 0.9113(3) 0.72291(14) 0.0571(18) Uani 1 1 d . . . O5 O 0.9040(3) 0.9475(3) 0.70275(15) 0.0557(18) Uani 1 1 d . . . O6 O 0.9168(3) 1.2819(3) 0.89998(14) 0.065(2) Uani 1 1 d . . . O7 O 0.8208(3) 1.2954(2) 0.89322(13) 0.0397(16) Uani 1 1 d . . . O8 O 0.9575(3) 1.1256(3) 0.77114(17) 0.089(2) Uani 1 1 d . . . O9 O 0.7708(3) 1.1601(3) 0.80131(14) 0.0617(19) Uani 1 1 d . . . O10 O 0.8835(3) 0.7847(3) 0.70428(13) 0.0547(18) Uani 1 1 d . . . O11 O 0.8558(3) 0.7134(2) 0.67116(12) 0.0486(16) Uani 1 1 d . . . O12 O 0.9164(3) 0.4147(3) 0.88151(16) 0.079(2) Uani 1 1 d . . . O13 O 0.8214(3) 0.4318(3) 0.88900(12) 0.0407(16) Uani 1 1 d . . . O14 O 0.8027(4) 0.5368(4) 0.73557(19) 0.107(3) Uani 1 1 d . . . O15 O 0.7622(4) 0.5692(3) 0.80088(19) 0.095(3) Uani 1 1 d . . . O101 O 0.0981(10) 0.3029(9) 0.9408(5) 0.375(7) Uiso 1 1 d D . . O102 O 0.4368(6) 0.1470(8) 0.8482(4) 0.261(7) Uiso 1 1 d D . . N1 N 0.4772(6) 0.1583(6) 0.7860(3) 0.161(5) Uiso 1 1 d D . . H1A H 0.4627 0.152 0.8057 0.193 Uiso 1 1 calc R . . H1B H 0.4895 0.1219 0.7783 0.193 Uiso 1 1 calc R . . N2 N 0.0374(7) 0.3627(7) 0.8957(4) 0.196(6) Uiso 1 1 d D . . H2A H 0.053 0.3394 0.9113 0.235 Uiso 1 1 calc R . . H2B H -0.0037 0.3602 0.8969 0.235 Uiso 1 1 calc R . . N101 N 0.2049(10) 0.2915(7) 0.9469(6) 0.375(7) Uiso 1 1 d D . . N102 N 0.4223(6) 0.1006(8) 0.8916(4) 0.239(8) Uiso 1 1 d D . . C1 C 0.5891(5) 0.0122(6) 0.7938(3) 0.066(3) Uani 1 1 d . . . C2 C 0.6384(5) 0.0109(5) 0.8186(2) 0.056(3) Uani 1 1 d . . . C3 C 0.6753(5) -0.0378(5) 0.8198(2) 0.066(3) Uani 1 1 d . . . H3 H 0.6721 -0.07 0.8055 0.079 Uiso 1 1 calc R . . C4 C 0.7198(5) -0.0372(6) 0.8444(3) 0.083(4) Uani 1 1 d . . . C5 C 0.7265(4) 0.0112(5) 0.86396(18) 0.047(2) Uani 1 1 d . . . C6 C 0.6889(5) 0.0559(5) 0.8614(2) 0.054(3) Uani 1 1 d . . . H6 H 0.6925 0.0888 0.8752 0.065 Uiso 1 1 calc R . . C7 C 0.6443(5) 0.0570(5) 0.8395(2) 0.062(3) Uani 1 1 d . . . H7 H 0.6174 0.0899 0.8388 0.075 Uiso 1 1 calc R . . C8 C 0.7438(7) -0.1365(6) 0.8301(5) 0.193(9) Uani 1 1 d . . . H8A H 0.7775 -0.1645 0.8312 0.289 Uiso 1 1 calc R . . H8B H 0.7333 -0.1293 0.8084 0.289 Uiso 1 1 calc R . . H8C H 0.7092 -0.1537 0.8409 0.289 Uiso 1 1 calc R . . C9 C 0.8667(5) 0.9480(4) 0.7224(2) 0.048(2) Uani 1 1 d . . . C10 C 0.8651(5) 0.9931(4) 0.7475(2) 0.053(2) Uani 1 1 d . . . C11 C 0.9110(5) 1.0342(5) 0.7476(2) 0.064(3) Uani 1 1 d . . . H11 H 0.9422 1.0312 0.7327 0.077 Uiso 1 1 calc R . . C12 C 0.9121(5) 1.0811(5) 0.7697(2) 0.062(3) Uani 1 1 d . . . C13 C 0.8690(4) 1.0848(4) 0.79227(17) 0.041(2) Uani 1 1 d . . . C14 C 0.8248(5) 1.0428(4) 0.7918(2) 0.067(3) Uani 1 1 d . . . H14 H 0.7943 1.0442 0.8071 0.08 Uiso 1 1 calc R . . C15 C 0.8229(4) 0.9973(4) 0.7692(2) 0.052(3) Uani 1 1 d . . . H15 H 0.791 0.9692 0.7695 0.063 Uiso 1 1 calc R . . C16 C 0.8697(4) 1.1326(4) 0.81664(15) 0.0438(18) Uani 1 1 d . . . C17 C 0.8186(5) 1.1695(4) 0.8213(2) 0.056(3) Uani 1 1 d . . . C18 C 0.8185(4) 1.2122(4) 0.84436(17) 0.042(2) Uani 1 1 d . . . H18 H 0.7836 1.2356 0.8479 0.051 Uiso 1 1 calc R . . C19 C 0.8700(5) 1.2213(4) 0.86263(17) 0.041(2) Uani 1 1 d . . . C20 C 0.9182(4) 1.1848(4) 0.8583(2) 0.050(3) Uani 1 1 d . . . H20 H 0.9529 1.1899 0.8708 0.06 Uiso 1 1 calc R . . C21 C 0.9172(4) 1.1404(4) 0.8361(2) 0.052(2) Uani 1 1 d . . . H21 H 0.9507 1.1145 0.8342 0.063 Uiso 1 1 calc R . . C22 C 0.8693(5) 1.2694(4) 0.88639(16) 0.040(2) Uani 1 1 d . . . C23 C 1.0084(5) 1.1231(5) 0.7504(3) 0.115(5) Uani 1 1 d . . . H23A H 1.0347 1.1574 0.7543 0.173 Uiso 1 1 calc R . . H23B H 0.9943 1.1244 0.7289 0.173 Uiso 1 1 calc R . . H23C H 1.0306 1.0858 0.7539 0.173 Uiso 1 1 calc R . . C24 C 0.7197(4) 1.1961(4) 0.8046(2) 0.064(3) Uani 1 1 d . . . H24A H 0.6904 1.1854 0.7886 0.096 Uiso 1 1 calc R . . H24B H 0.7309 1.2383 0.8024 0.096 Uiso 1 1 calc R . . H24C H 0.7021 1.1896 0.8251 0.096 Uiso 1 1 calc R . . C25 C 0.8700(4) 0.7316(4) 0.6970(2) 0.042(2) Uani 1 1 d . . . C26 C 0.8697(4) 0.6851(4) 0.72214(17) 0.051(2) Uani 1 1 d D . . C27 C 0.8393(4) 0.6326(4) 0.71771(18) 0.062(3) Uani 1 1 d D . . H27 H 0.8191 0.6257 0.6987 0.075 Uiso 1 1 calc R . . C28 C 0.8376(5) 0.5900(4) 0.7403(2) 0.072(3) Uani 1 1 d D . . C29 C 0.8681(4) 0.5975(4) 0.7672(2) 0.065(3) Uani 1 1 d D . . C30 C 0.9026(6) 0.6473(5) 0.7707(2) 0.129(6) Uani 1 1 d D . . H30 H 0.9281 0.6506 0.7882 0.155 Uiso 1 1 calc R . . C31 C 0.9012(5) 0.6934(5) 0.7490(2) 0.092(4) Uani 1 1 d D . . H31 H 0.9218 0.7299 0.7528 0.11 Uiso 1 1 calc R . . C32 C 0.8664(5) 0.5532(4) 0.79440(19) 0.080(3) Uani 1 1 d D . . C33 C 0.8143(4) 0.5424(4) 0.8112(2) 0.071(4) Uani 1 1 d D . . C34 C 0.8152(4) 0.5039(4) 0.83599(18) 0.054(3) Uani 1 1 d D . . H34 H 0.7791 0.4959 0.847 0.065 Uiso 1 1 calc R . . C35 C 0.8672(4) 0.4771(4) 0.84504(17) 0.054(2) Uani 1 1 d D . . C36 C 0.9188(4) 0.4848(4) 0.8271(2) 0.075(4) Uani 1 1 d D . . H36 H 0.9544 0.4635 0.832 0.09 Uiso 1 1 calc R . . C37 C 0.9177(4) 0.5233(4) 0.8022(2) 0.073(3) Uani 1 1 d D . . H37 H 0.9531 0.5292 0.7903 0.087 Uiso 1 1 calc R . . C38 C 0.8662(5) 0.4381(4) 0.8740(2) 0.051(2) Uani 1 1 d . . . C39 C 0.7679(7) 0.5331(7) 0.7090(3) 0.150(7) Uani 1 1 d . . . H39A H 0.7476 0.4942 0.7084 0.226 Uiso 1 1 calc R . . H39B H 0.7937 0.5372 0.6907 0.226 Uiso 1 1 calc R . . H39C H 0.738 0.5653 0.709 0.226 Uiso 1 1 calc R . . C40 C 0.7049(5) 0.5535(7) 0.8142(4) 0.142(7) Uani 1 1 d . . . H40A H 0.673 0.5754 0.8034 0.213 Uiso 1 1 calc R . . H40B H 0.7046 0.5642 0.8362 0.213 Uiso 1 1 calc R . . H40C H 0.6982 0.5103 0.812 0.213 Uiso 1 1 calc R . . C41 C 0.5269(7) 0.1968(9) 0.7877(5) 0.232(10) Uiso 1 1 d D . . H41A H 0.5586 0.178 0.8 0.348 Uiso 1 1 calc R . . H41B H 0.5149 0.2346 0.7974 0.348 Uiso 1 1 calc R . . H41C H 0.5418 0.2049 0.7667 0.348 Uiso 1 1 calc R . . C42 C 0.4266(6) 0.1823(6) 0.7657(3) 0.127(5) Uiso 1 1 d D . . H42A H 0.3914 0.1563 0.7677 0.19 Uiso 1 1 calc R . . H42B H 0.4397 0.1831 0.7441 0.19 Uiso 1 1 calc R . . H42C H 0.4162 0.223 0.7724 0.19 Uiso 1 1 calc R . . C43 C 0.0555(9) 0.4266(8) 0.9013(4) 0.217(10) Uiso 1 1 d D . . H43A H 0.0452 0.438 0.9226 0.325 Uiso 1 1 calc R . . H43B H 0.0343 0.4528 0.8868 0.325 Uiso 1 1 calc R . . H43C H 0.0988 0.4307 0.8982 0.325 Uiso 1 1 calc R . . C44 C 0.0567(12) 0.3375(9) 0.8656(5) 0.308(15) Uiso 1 1 d D . . H44A H 0.0426 0.296 0.8639 0.462 Uiso 1 1 calc R . . H44B H 0.1006 0.3383 0.8644 0.462 Uiso 1 1 calc R . . H44C H 0.0398 0.3614 0.8487 0.462 Uiso 1 1 calc R . . C101 C 0.2111(12) 0.2899(13) 0.9799(5) 0.375(7) Uiso 1 1 d D . . H10A H 0.2534 0.2848 0.9853 0.563 Uiso 1 1 calc R . . H10B H 0.1879 0.2563 0.9882 0.563 Uiso 1 1 calc R . . H10C H 0.1962 0.3275 0.9887 0.563 Uiso 1 1 calc R . . C102 C 0.2664(11) 0.2858(12) 0.9318(6) 0.375(7) Uiso 1 1 d D . . H10D H 0.2971 0.2827 0.948 0.563 Uiso 1 1 calc R . . H10E H 0.2742 0.3213 0.9191 0.563 Uiso 1 1 calc R . . H10F H 0.2674 0.2499 0.9188 0.563 Uiso 1 1 calc R . . C103 C 0.1515(11) 0.2969(8) 0.9285(6) 0.375(7) Uiso 1 1 d D . . H103 H 0.1551 0.296 0.9066 0.45 Uiso 1 1 calc R . . C104 C 0.4091(13) 0.1610(9) 0.9047(5) 0.341(16) Uiso 1 1 d D . . H10G H 0.3989 0.1571 0.9266 0.511 Uiso 1 1 calc R . . H10H H 0.3752 0.1788 0.8935 0.511 Uiso 1 1 calc R . . H10I H 0.4443 0.1868 0.9024 0.511 Uiso 1 1 calc R . . C105 C 0.4172(9) 0.0506(8) 0.9139(4) 0.243(10) Uiso 1 1 d D . . H10J H 0.4056 0.0664 0.9342 0.364 Uiso 1 1 calc R . . H10K H 0.456 0.0302 0.9157 0.364 Uiso 1 1 calc R . . H10L H 0.3868 0.0222 0.9067 0.364 Uiso 1 1 calc R . . C106 C 0.4392(8) 0.0942(10) 0.8616(4) 0.328(16) Uiso 1 1 d D . . H106 H 0.4507 0.0578 0.8519 0.394 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 Cd1 0.0715(6) 0.0715(6) 0.0369(8) 0 0 0 Cd2 0.0402(4) 0.0405(4) 0.0252(2) -0.0043(3) 0.0011(3) -0.0024(3) Cd3 0.0439(5) 0.0374(5) 0.0286(4) 0.0002(4) 0 0 O1 0.082(6) 0.107(7) 0.063(5) -0.022(5) -0.028(4) -0.016(5) O2 0.087(6) 0.071(6) 0.058(5) 0.000(4) -0.030(4) -0.020(5) O3 0.080(6) 0.062(5) 0.130(7) -0.038(5) -0.027(5) 0.012(5) O4 0.068(5) 0.061(5) 0.043(4) -0.006(3) -0.002(4) 0.006(4) O5 0.054(4) 0.061(5) 0.052(4) -0.016(3) 0.012(4) 0.002(4) O6 0.070(5) 0.077(5) 0.047(4) -0.030(4) -0.011(4) 0.022(4) O7 0.043(4) 0.038(4) 0.037(3) -0.012(3) 0.004(3) 0.014(3) O8 0.094(6) 0.079(6) 0.093(5) -0.045(5) 0.030(5) -0.020(5) O9 0.051(4) 0.083(5) 0.051(4) -0.026(4) -0.004(3) 0.003(4) O10 0.072(5) 0.053(4) 0.039(4) 0.006(3) -0.001(3) 0.001(4) O11 0.058(4) 0.052(4) 0.036(4) 0.003(3) -0.001(3) -0.011(3) O12 0.058(5) 0.112(6) 0.068(5) 0.055(4) -0.018(4) -0.010(5) O13 0.044(4) 0.055(4) 0.023(3) 0.012(3) 0.000(3) -0.011(3) O14 0.153(8) 0.080(6) 0.088(6) 0.028(5) -0.012(6) -0.009(6) O15 0.079(6) 0.083(6) 0.124(7) 0.045(5) 0.010(5) 0.019(5) C1 0.076(9) 0.060(8) 0.061(8) 0.022(7) -0.020(7) -0.022(7) C2 0.053(6) 0.064(7) 0.052(6) 0.002(5) 0.012(6) -0.018(7) C3 0.060(7) 0.076(8) 0.063(7) -0.033(6) 0.006(6) -0.005(7) C4 0.043(7) 0.081(9) 0.126(11) 0.013(8) -0.018(7) 0.015(7) C5 0.054(7) 0.051(6) 0.036(5) -0.015(5) 0.001(4) -0.006(5) C6 0.069(7) 0.061(7) 0.033(5) 0.000(5) -0.009(5) 0.012(6) C7 0.066(8) 0.067(7) 0.054(6) -0.010(6) 0.023(6) 0.001(6) C8 0.167(16) 0.082(10) 0.33(2) -0.068(15) -0.095(17) 0.056(13) C9 0.064(7) 0.039(5) 0.042(6) -0.002(5) -0.003(6) -0.013(6) C10 0.050(6) 0.057(6) 0.050(6) -0.014(5) -0.019(6) 0.010(6) C11 0.060(7) 0.088(8) 0.046(6) -0.038(6) -0.015(5) 0.029(7) C12 0.062(7) 0.050(7) 0.073(7) -0.019(6) 0.022(6) 0.013(6) C13 0.044(5) 0.049(5) 0.030(4) -0.006(4) 0.005(5) 0.010(6) C14 0.093(9) 0.048(7) 0.059(7) -0.004(6) 0.017(6) 0.014(7) C15 0.065(7) 0.045(6) 0.047(6) -0.018(5) 0.009(5) -0.015(5) C16 0.057(6) 0.040(5) 0.034(4) 0.001(5) 0.006(5) 0.003(6) C17 0.087(8) 0.047(6) 0.035(5) -0.015(5) -0.006(6) -0.002(6) C18 0.055(6) 0.045(6) 0.027(5) -0.009(4) 0.003(5) 0.013(5) C19 0.055(6) 0.037(5) 0.032(4) 0.002(4) -0.006(5) 0.014(5) C20 0.039(6) 0.075(8) 0.037(5) -0.009(5) 0.002(5) -0.005(6) C21 0.053(6) 0.053(6) 0.050(6) -0.004(6) 0.003(5) 0.014(6) C22 0.052(6) 0.047(6) 0.021(4) 0.011(4) -0.007(5) 0.008(6) C23 0.087(9) 0.104(10) 0.156(11) -0.068(9) 0.081(9) -0.015(8) C24 0.042(6) 0.068(7) 0.082(8) -0.031(6) -0.005(6) 0.007(6) C25 0.032(5) 0.049(6) 0.047(5) 0.008(4) -0.002(5) -0.001(5) C26 0.049(6) 0.067(7) 0.037(5) 0.023(5) 0.006(5) -0.012(6) C27 0.095(8) 0.049(6) 0.042(5) 0.005(6) 0.000(5) -0.011(7) C28 0.117(10) 0.046(7) 0.052(7) -0.007(6) 0.013(7) -0.025(7) C29 0.047(6) 0.084(8) 0.064(7) 0.044(6) 0.005(6) -0.011(7) C30 0.187(15) 0.130(13) 0.072(8) 0.055(9) -0.069(9) -0.086(12) C31 0.124(11) 0.096(10) 0.056(7) 0.032(7) -0.001(7) -0.056(8) C32 0.080(8) 0.100(9) 0.059(6) 0.060(6) -0.011(7) -0.022(9) C33 0.032(6) 0.073(8) 0.109(9) 0.057(7) -0.010(6) 0.002(6) C34 0.040(6) 0.063(7) 0.060(6) 0.041(6) 0.018(5) 0.014(5) C35 0.051(6) 0.059(6) 0.052(6) 0.018(5) 0.004(6) -0.019(6) C36 0.034(6) 0.119(10) 0.071(7) 0.058(7) 0.000(5) 0.014(6) C37 0.035(6) 0.110(10) 0.073(8) 0.039(7) 0.004(6) 0.009(6) C38 0.052(6) 0.052(6) 0.049(5) 0.017(5) -0.021(7) 0.002(6) C39 0.178(16) 0.185(16) 0.088(10) 0.054(10) -0.087(11) -0.050(12) C40 0.054(8) 0.174(16) 0.198(17) 0.086(13) 0.046(10) 0.018(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.307(7) 11_556 ? Cd1 O1 2.307(7) . ? Cd1 O1 2.307(7) 2_655 ? Cd1 O1 2.307(7) 12_546 ? Cd1 O2 2.515(6) 11_556 ? Cd1 O2 2.515(6) . ? Cd1 O2 2.515(6) 2_655 ? Cd1 O2 2.515(6) 12_546 ? Cd1 C1 2.758(11) 11_556 ? Cd1 C1 2.758(11) . ? Cd1 C1 2.758(11) 2_655 ? Cd1 C1 2.758(11) 12_546 ? Cd2 O10 2.258(6) . ? Cd2 O5 2.280(6) . ? Cd2 O7 2.365(5) 8_454 ? Cd2 O13 2.414(5) 8_554 ? Cd2 O4 2.419(6) . ? Cd2 O6 2.441(6) 8_454 ? Cd2 O12 2.463(6) 8_554 ? Cd2 C9 2.679(9) . ? Cd2 C22 2.750(8) 8_454 ? Cd2 Cd3 3.4379(6) . ? Cd3 O11 2.161(5) . ? Cd3 O11 2.161(5) 14_465 ? Cd3 O13 2.288(6) 11_566 ? Cd3 O13 2.288(6) 8_554 ? Cd3 O7 2.326(6) 11_466 ? Cd3 O7 2.326(6) 8_454 ? Cd3 Cd2 3.4379(6) 14_465 ? O1 C1 1.272(13) . ? O2 C1 1.232(12) . ? O3 C4 1.343(12) . ? O3 C8 1.404(14) . ? O4 C9 1.243(10) . ? O5 C9 1.189(11) . ? O6 C22 1.243(10) . ? O6 Cd2 2.441(6) 16_454 ? O7 C22 1.264(10) . ? O7 Cd3 2.326(6) 12_656 ? O7 Cd2 2.365(5) 16_454 ? O8 C12 1.418(12) . ? O8 C23 1.448(11) . ? O9 C17 1.388(11) . ? O9 C24 1.401(10) . ? O10 C25 1.264(9) . ? O11 C25 1.228(9) . ? O12 C38 1.278(10) . ? O12 Cd2 2.463(6) 16_444 ? O13 C38 1.198(11) . ? O13 Cd3 2.288(6) 12_646 ? O13 Cd2 2.414(5) 16_444 ? O14 C39 1.390(12) . ? O14 C28 1.433(11) . ? O15 C33 1.381(10) . ? O15 C40 1.444(12) . ? O101 C103 1.312(17) . ? O102 C106 1.314(16) . ? N1 C41 1.405(14) . ? N1 C42 1.527(12) . ? N2 C44 1.481(15) . ? N2 C43 1.501(14) . ? N101 C101 1.434(16) . ? N101 C103 1.435(15) . ? N101 C102 1.523(16) . ? N102 C106 1.356(15) . ? N102 C105 1.480(14) . ? N102 C104 1.491(15) . ? C1 C2 1.534(13) . ? C2 C3 1.365(13) . ? C2 C7 1.376(12) . ? C3 C4 1.454(14) . ? C4 C5 1.382(14) . ? C5 C6 1.308(12) . ? C5 C5 1.419(17) 5_656 ? C6 C7 1.373(13) . ? C9 C10 1.481(12) . ? C10 C15 1.332(12) . ? C10 C11 1.376(13) . ? C11 C12 1.418(12) . ? C12 C13 1.372(12) . ? C13 C14 1.362(13) . ? C13 C16 1.499(11) . ? C14 C15 1.407(12) . ? C16 C21 1.363(11) . ? C16 C17 1.420(12) . ? C17 C18 1.379(11) . ? C18 C19 1.409(11) . ? C19 C20 1.363(11) . ? C19 C22 1.485(10) . ? C20 C21 1.380(12) . ? C22 Cd2 2.750(8) 16_454 ? C25 C26 1.503(10) . ? C26 C27 1.368(9) . ? C26 C31 1.371(9) . ? C27 C28 1.362(9) . ? C28 C29 1.358(9) . ? C29 C30 1.361(10) . ? C29 C32 1.536(10) . ? C30 C31 1.391(10) . ? C32 C37 1.368(9) . ? C32 C33 1.392(9) . ? C33 C34 1.372(9) . ? C34 C35 1.364(9) . ? C35 C36 1.399(9) . ? C35 C38 1.527(11) . ? C36 C37 1.376(9) . ? 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 Cd1 O1 101.18(15) 11_556 . ? O1 Cd1 O1 101.18(15) 11_556 2_655 ? O1 Cd1 O1 127.8(4) . 2_655 ? O1 Cd1 O1 127.8(4) 11_556 12_546 ? O1 Cd1 O1 101.18(15) . 12_546 ? O1 Cd1 O1 101.18(15) 2_655 12_546 ? O1 Cd1 O2 53.8(3) 11_556 11_556 ? O1 Cd1 O2 80.0(2) . 11_556 ? O1 Cd1 O2 148.5(3) 2_655 11_556 ? O1 Cd1 O2 84.9(3) 12_546 11_556 ? O1 Cd1 O2 148.5(3) 11_556 . ? O1 Cd1 O2 53.8(3) . . ? O1 Cd1 O2 84.9(3) 2_655 . ? O1 Cd1 O2 80.0(2) 12_546 . ? O2 Cd1 O2 126.6(2) 11_556 . ? O1 Cd1 O2 80.0(2) 11_556 2_655 ? O1 Cd1 O2 84.9(3) . 2_655 ? O1 Cd1 O2 53.8(3) 2_655 2_655 ? O1 Cd1 O2 148.5(3) 12_546 2_655 ? O2 Cd1 O2 126.6(2) 11_556 2_655 ? O2 Cd1 O2 79.0(3) . 2_655 ? O1 Cd1 O2 84.9(3) 11_556 12_546 ? O1 Cd1 O2 148.5(3) . 12_546 ? O1 Cd1 O2 80.0(2) 2_655 12_546 ? O1 Cd1 O2 53.8(3) 12_546 12_546 ? O2 Cd1 O2 79.0(3) 11_556 12_546 ? O2 Cd1 O2 126.6(2) . 12_546 ? O2 Cd1 O2 126.6(2) 2_655 12_546 ? O1 Cd1 C1 27.3(3) 11_556 11_556 ? O1 Cd1 C1 90.8(3) . 11_556 ? O1 Cd1 C1 126.1(3) 2_655 11_556 ? O1 Cd1 C1 106.6(4) 12_546 11_556 ? O2 Cd1 C1 26.5(3) 11_556 11_556 ? O2 Cd1 C1 144.4(2) . 11_556 ? O2 Cd1 C1 104.2(3) 2_655 11_556 ? O2 Cd1 C1 80.6(3) 12_546 11_556 ? O1 Cd1 C1 126.1(3) 11_556 . ? O1 Cd1 C1 27.3(3) . . ? O1 Cd1 C1 106.6(4) 2_655 . ? O1 Cd1 C1 90.8(3) 12_546 . ? O2 Cd1 C1 104.2(3) 11_556 . ? O2 Cd1 C1 26.5(3) . . ? O2 Cd1 C1 80.6(3) 2_655 . ? O2 Cd1 C1 144.4(3) 12_546 . ? C1 Cd1 C1 118.0(3) 11_556 . ? O1 Cd1 C1 90.8(3) 11_556 2_655 ? O1 Cd1 C1 106.6(4) . 2_655 ? O1 Cd1 C1 27.3(3) 2_655 2_655 ? O1 Cd1 C1 126.1(3) 12_546 2_655 ? O2 Cd1 C1 144.4(2) 11_556 2_655 ? O2 Cd1 C1 80.6(3) . 2_655 ? O2 Cd1 C1 26.5(3) 2_655 2_655 ? O2 Cd1 C1 104.2(3) 12_546 2_655 ? C1 Cd1 C1 118.0(3) 11_556 2_655 ? C1 Cd1 C1 93.4(5) . 2_655 ? O1 Cd1 C1 106.6(4) 11_556 12_546 ? O1 Cd1 C1 126.1(3) . 12_546 ? O1 Cd1 C1 90.8(3) 2_655 12_546 ? O1 Cd1 C1 27.3(3) 12_546 12_546 ? O2 Cd1 C1 80.6(3) 11_556 12_546 ? O2 Cd1 C1 104.2(3) . 12_546 ? O2 Cd1 C1 144.4(2) 2_655 12_546 ? O2 Cd1 C1 26.5(3) 12_546 12_546 ? C1 Cd1 C1 93.4(5) 11_556 12_546 ? C1 Cd1 C1 118.0(3) . 12_546 ? C1 Cd1 C1 118.0(3) 2_655 12_546 ? O10 Cd2 O5 107.6(2) . . ? O10 Cd2 O7 94.2(2) . 8_454 ? O5 Cd2 O7 154.0(2) . 8_454 ? O10 Cd2 O13 84.0(2) . 8_554 ? O5 Cd2 O13 116.2(2) . 8_554 ? O7 Cd2 O13 79.26(17) 8_454 8_554 ? O10 Cd2 O4 86.8(2) . . ? O5 Cd2 O4 53.8(2) . . ? O7 Cd2 O4 115.5(2) 8_454 . ? O13 Cd2 O4 163.2(2) 8_554 . ? O10 Cd2 O6 138.7(2) . 8_454 ? O5 Cd2 O6 100.0(2) . 8_454 ? O7 Cd2 O6 54.04(19) 8_454 8_454 ? O13 Cd2 O6 110.7(2) 8_554 8_454 ? O4 Cd2 O6 85.4(2) . 8_454 ? O10 Cd2 O12 134.8(2) . 8_554 ? O5 Cd2 O12 83.6(2) . 8_554 ? O7 Cd2 O12 91.1(2) 8_454 8_554 ? O13 Cd2 O12 53.1(2) 8_554 8_554 ? O4 Cd2 O12 130.3(2) . 8_554 ? O6 Cd2 O12 77.5(3) 8_454 8_554 ? O10 Cd2 C9 98.3(2) . . ? O5 Cd2 C9 26.2(3) . . ? O7 Cd2 C9 138.7(3) 8_454 . ? O13 Cd2 C9 141.0(3) 8_554 . ? O4 Cd2 C9 27.6(2) . . ? O6 Cd2 C9 93.2(3) 8_454 . ? O12 Cd2 C9 106.8(3) 8_554 . ? O10 Cd2 C22 118.8(3) . 8_454 ? O5 Cd2 C22 126.9(3) . 8_454 ? O7 Cd2 C22 27.3(2) 8_454 8_454 ? O13 Cd2 C22 93.9(2) 8_554 8_454 ? O4 Cd2 C22 102.9(2) . 8_454 ? O6 Cd2 C22 26.9(2) 8_454 8_454 ? O12 Cd2 C22 81.6(2) 8_554 8_454 ? C9 Cd2 C22 117.8(3) . 8_454 ? O10 Cd2 Cd3 73.60(15) . . ? O5 Cd2 Cd3 157.80(17) . . ? O7 Cd2 Cd3 42.44(14) 8_454 . ? O13 Cd2 Cd3 41.61(14) 8_554 . ? O4 Cd2 Cd3 146.77(18) . . ? O6 Cd2 Cd3 91.89(17) 8_454 . ? O12 Cd2 Cd3 80.81(16) 8_554 . ? C9 Cd2 Cd3 171.64(19) . . ? C22 Cd2 Cd3 66.1(2) 8_454 . ? O11 Cd3 O11 171.0(3) . 14_465 ? O11 Cd3 O13 91.9(2) . 11_566 ? O11 Cd3 O13 94.1(2) 14_465 11_566 ? O11 Cd3 O13 94.1(2) . 8_554 ? O11 Cd3 O13 91.9(2) 14_465 8_554 ? O13 Cd3 O13 96.3(3) 11_566 8_554 ? O11 Cd3 O7 90.3(2) . 11_466 ? O11 Cd3 O7 83.9(2) 14_465 11_466 ? O13 Cd3 O7 82.69(19) 11_566 11_466 ? O13 Cd3 O7 175.6(2) 8_554 11_466 ? O11 Cd3 O7 83.9(2) . 8_454 ? O11 Cd3 O7 90.3(2) 14_465 8_454 ? O13 Cd3 O7 175.6(2) 11_566 8_454 ? O13 Cd3 O7 82.69(19) 8_554 8_454 ? O7 Cd3 O7 98.7(3) 11_466 8_454 ? O11 Cd3 Cd2 72.44(15) . . ? O11 Cd3 Cd2 107.70(15) 14_465 . ? O13 Cd3 Cd2 133.87(14) 11_566 . ? O13 Cd3 Cd2 44.48(14) 8_554 . ? O7 Cd3 Cd2 138.39(14) 11_466 . ? O7 Cd3 Cd2 43.31(13) 8_454 . ? O11 Cd3 Cd2 107.70(15) . 14_465 ? O11 Cd3 Cd2 72.44(15) 14_465 14_465 ? O13 Cd3 Cd2 44.48(14) 11_566 14_465 ? O13 Cd3 Cd2 133.87(14) 8_554 14_465 ? O7 Cd3 Cd2 43.31(13) 11_466 14_465 ? O7 Cd3 Cd2 138.39(14) 8_454 14_465 ? Cd2 Cd3 Cd2 178.24(4) . 14_465 ? C1 O1 Cd1 96.5(7) . . ? C1 O2 Cd1 87.8(7) . . ? C4 O3 C8 118.5(10) . . ? C9 O4 Cd2 87.9(6) . . ? C9 O5 Cd2 96.0(6) . . ? C22 O6 Cd2 90.6(5) . 16_454 ? C22 O7 Cd3 143.4(5) . 12_656 ? C22 O7 Cd2 93.6(5) . 16_454 ? Cd3 O7 Cd2 94.3(2) 12_656 16_454 ? C12 O8 C23 120.4(8) . . ? C17 O9 C24 118.4(7) . . ? C25 O10 Cd2 126.6(5) . . ? C25 O11 Cd3 133.8(5) . . ? C38 O12 Cd2 89.7(6) . 16_444 ? C38 O13 Cd3 121.1(6) . 12_646 ? C38 O13 Cd2 94.0(5) . 16_444 ? Cd3 O13 Cd2 93.9(2) 12_646 16_444 ? C39 O14 C28 118.1(9) . . ? C33 O15 C40 120.7(8) . . ? C41 N1 C42 113.4(12) . . ? C44 N2 C43 115.1(14) . . ? C101 N101 C103 129.1(16) . . ? C101 N101 C102 109.6(14) . . ? C103 N101 C102 121.3(15) . . ? C106 N102 C105 124.4(14) . . ? C106 N102 C104 120.8(13) . . ? C105 N102 C104 114.7(13) . . ? O2 C1 O1 121.9(10) . . ? O2 C1 C2 119.4(11) . . ? O1 C1 C2 118.7(11) . . ? O2 C1 Cd1 65.7(6) . . ? O1 C1 Cd1 56.2(6) . . ? C2 C1 Cd1 173.2(8) . . ? C3 C2 C7 120.7(10) . . ? C3 C2 C1 118.3(10) . . ? C7 C2 C1 120.9(11) . . ? C2 C3 C4 115.7(10) . . ? O3 C4 C5 121.1(11) . . ? O3 C4 C3 116.3(11) . . ? C5 C4 C3 121.9(10) . . ? C6 C5 C4 118.4(9) . . ? C6 C5 C5 122.1(7) . 5_656 ? C4 C5 C5 119.4(8) . 5_656 ? C5 C6 C7 122.4(10) . . ? C6 C7 C2 120.7(10) . . ? O5 C9 O4 122.3(9) . . ? O5 C9 C10 123.1(10) . . ? O4 C9 C10 114.6(10) . . ? O5 C9 Cd2 57.8(5) . . ? O4 C9 Cd2 64.5(5) . . ? C10 C9 Cd2 177.8(8) . . ? C15 C10 C11 118.6(9) . . ? C15 C10 C9 125.6(10) . . ? C11 C10 C9 115.9(10) . . ? C10 C11 C12 120.5(10) . . ? C13 C12 C11 120.7(10) . . ? C13 C12 O8 115.2(9) . . ? C11 C12 O8 124.0(9) . . ? C14 C13 C12 117.1(9) . . ? C14 C13 C16 120.6(8) . . ? C12 C13 C16 122.3(9) . . ? C13 C14 C15 122.0(10) . . ? C10 C15 C14 121.1(10) . . ? C21 C16 C17 117.6(8) . . ? C21 C16 C13 122.1(9) . . ? C17 C16 C13 120.2(8) . . ? C18 C17 O9 123.5(9) . . ? C18 C17 C16 120.3(9) . . ? O9 C17 C16 116.2(8) . . ? C17 C18 C19 120.1(9) . . ? C20 C19 C18 118.9(8) . . ? C20 C19 C22 122.3(9) . . ? C18 C19 C22 118.8(8) . . ? C19 C20 C21 120.7(9) . . ? C16 C21 C20 122.3(9) . . ? O6 C22 O7 121.2(8) . . ? O6 C22 C19 118.6(9) . . ? O7 C22 C19 120.2(9) . . ? O6 C22 Cd2 62.6(4) . 16_454 ? O7 C22 Cd2 59.1(4) . 16_454 ? C19 C22 Cd2 174.9(5) . 16_454 ? O11 C25 O10 126.8(8) . . ? O11 C25 C26 115.3(8) . . ? O10 C25 C26 117.9(8) . . ? C27 C26 C31 119.2(6) . . ? C27 C26 C25 119.5(8) . . ? C31 C26 C25 121.2(8) . . ? C28 C27 C26 120.8(7) . . ? C29 C28 C27 120.9(7) . . ? C29 C28 O14 119.7(8) . . ? C27 C28 O14 119.4(8) . . ? C28 C29 C30 118.7(7) . . ? C28 C29 C32 124.3(8) . . ? C30 C29 C32 117.0(8) . . ? C29 C30 C31 121.0(7) . . ? C26 C31 C30 118.9(7) . . ? C37 C32 C33 119.1(6) . . ? C37 C32 C29 118.8(8) . . ? C33 C32 C29 122.1(8) . . ? C34 C33 O15 122.4(8) . . ? C34 C33 C32 120.2(7) . . ? O15 C33 C32 117.3(8) . . ? C35 C34 C33 120.7(7) . . ? C34 C35 C36 119.2(6) . . ? C34 C35 C38 118.2(8) . . ? C36 C35 C38 122.5(8) . . ? C37 C36 C35 119.7(7) . . ? C32 C37 C36 120.8(7) . . ? O13 C38 O12 123.2(8) . . ? O13 C38 C35 121.5(9) . . ? O12 C38 C35 115.3(10) . . ? O101 C103 N101 123(2) . . ? O102 C106 N102 108.4(15) . . ? 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 N1 H1B O2 0.92 2.2 2.916(15) 134.3 . N1 H1A O102 0.92 1.93 2.85(2) 173.5 . N2 H2B O12 0.92 2.26 3.001(17) 137.5 1_455 N2 H2A O101 0.92 1.82 2.72(3) 167.7 . data_x0932fin _database_code_depnum_ccdc_archive 'CCDC 904637' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2010-01-18T13:13:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C68 H60 O28 Pb6' _chemical_formula_weight 2568.3 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 29.5046(5) _cell_length_b 14.3407(2) _cell_length_c 18.4708(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7815.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 22072 _cell_measurement_theta_min 2.8361 _cell_measurement_theta_max 32.3071 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.28554 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_ub_11 -0.0110683863 _diffrn_orient_matrix_ub_12 0.0003862251 _diffrn_orient_matrix_ub_13 0.0234729546 _diffrn_orient_matrix_ub_21 0.0479251901 _diffrn_orient_matrix_ub_22 0.0047284449 _diffrn_orient_matrix_ub_23 0.0053152445 _diffrn_orient_matrix_ub_31 -0.0058432506 _diffrn_orient_matrix_ub_32 0.0382017752 _diffrn_orient_matrix_ub_33 -0.0009191818 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_unetI/netI 0.0941 _diffrn_reflns_number 111713 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 11939 _reflns_number_gt 7063 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11939 _refine_ls_number_parameters 558 _refine_ls_number_restraints 2458 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.03 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.82 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.968 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.185 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pb1 Pb 0.913423(7) 0.987930(15) 0.890903(12) 0.02016(5) Uani 1 1 d . . . Pb2 Pb 0.982215(7) 1.118436(14) 1.018519(11) 0.01824(5) Uani 1 1 d . . . Pb3 Pb 1.034889(7) 1.054726(15) 0.833164(11) 0.01970(5) Uani 1 1 d . . . O1 O 0.91101(12) 1.0118(3) 1.0353(2) 0.0252(9) Uani 1 1 d . A . O2 O 0.88495(13) 0.9578(3) 1.1403(2) 0.0323(10) Uani 1 1 d . . . O4 O 0.56344(12) 1.3335(3) 0.9612(2) 0.0260(10) Uani 1 1 d . . . O5 O 0.54806(13) 1.3088(3) 1.0762(2) 0.0279(10) Uani 1 1 d . . . O7 O 0.91176(13) 1.1616(3) 0.9136(2) 0.0263(9) Uani 1 1 d . B . O8 O 0.93750(14) 1.1236(3) 0.8050(2) 0.0322(10) Uani 1 1 d . B . O10 O 0.95284(13) 1.9229(3) 0.7806(2) 0.0271(10) Uani 1 1 d . . . O11 O 0.94721(13) 1.8885(3) 0.6644(2) 0.0267(9) Uani 1 1 d . . . O13 O 0.98578(11) 1.0092(2) 0.92676(18) 0.0181(8) Uani 1 1 d . . . C1 C 0.87976(19) 1.0010(4) 1.0800(3) 0.0253(13) Uani 1 1 d D . . O3 O 0.71363(15) 0.9959(4) 1.1079(3) 0.053(2) Uani 0.767(8) 1 d PD A 1 C2 C 0.83350(13) 1.0398(3) 1.0661(2) 0.0275(14) Uani 0.767(8) 1 d PD A 1 C3 C 0.79525(16) 0.9949(5) 1.0924(5) 0.0340(19) Uani 0.767(8) 1 d PD A 1 H3 H 0.7979 0.9363 1.116 0.041 Uiso 0.767(8) 1 calc PR A 1 C4 C 0.75286(16) 1.0363(4) 1.0840(4) 0.041(2) Uani 0.767(8) 1 d PD A 1 C5 C 0.74862(14) 1.1219(3) 1.0496(3) 0.0405(18) Uani 0.767(8) 1 d PD A 1 C6 C 0.78709(18) 1.1653(4) 1.0224(4) 0.046(2) Uani 0.767(8) 1 d PD A 1 H6 H 0.7846 1.2245 0.9996 0.055 Uiso 0.767(8) 1 calc PR A 1 C7 C 0.82938(18) 1.1227(5) 1.0282(5) 0.0357(18) Uani 0.767(8) 1 d PD A 1 H7 H 0.8552 1.1504 1.0062 0.043 Uiso 0.767(8) 1 calc PR A 1 C8 C 0.7164(3) 0.9094(7) 1.1478(8) 0.110(6) Uani 0.767(8) 1 d PD A 1 H8A H 0.6859 0.8888 1.1611 0.165 Uiso 0.767(8) 1 calc PR A 1 H8B H 0.7344 0.9191 1.1918 0.165 Uiso 0.767(8) 1 calc PR A 1 H8C H 0.7309 0.8617 1.1177 0.165 Uiso 0.767(8) 1 calc PR A 1 O3F O 0.7780(5) 1.2344(13) 0.9705(13) 0.114(12) Uiso 0.233(8) 1 d PD A 2 C2F C 0.83350(13) 1.0398(3) 1.0661(2) 0.0275(14) Uani 0.233(8) 1 d PD A 2 C3F C 0.8282(3) 1.1161(11) 1.0206(11) 0.0357(18) Uani 0.233(8) 1 d PD A 2 H3F H 0.8535 1.1397 0.9944 0.043 Uiso 0.233(8) 1 calc PR A 2 C4F C 0.7860(2) 1.1580(8) 1.0133(8) 0.046(2) Uani 0.233(8) 1 d PD A 2 C5F C 0.74862(14) 1.1219(3) 1.0496(3) 0.0405(18) Uani 0.233(8) 1 d PD A 2 C6F C 0.7538(3) 1.0449(9) 1.0947(9) 0.041(2) Uani 0.233(8) 1 d PD A 2 H6F H 0.7285 1.0205 1.12 0.05 Uiso 0.233(8) 1 calc PR A 2 C7F C 0.7962(3) 1.0038(11) 1.1027(11) 0.0340(19) Uani 0.233(8) 1 d PD A 2 H7F H 0.7997 0.9509 1.1332 0.041 Uiso 0.233(8) 1 calc PR A 2 C8F C 0.8145(10) 1.296(2) 0.951(2) 0.15(2) Uiso 0.233(8) 1 d PD A 2 H8F1 H 0.8024 1.3492 0.9235 0.218 Uiso 0.233(8) 1 calc PR A 2 H8F2 H 0.8367 1.2627 0.9213 0.218 Uiso 0.233(8) 1 calc PR A 2 H8F3 H 0.8293 1.3194 0.995 0.218 Uiso 0.233(8) 1 calc PR A 2 C9 C 0.57400(19) 1.3033(4) 1.0239(3) 0.0251(13) Uani 1 1 d D . . O6 O 0.70323(18) 1.1873(5) 1.1687(3) 0.063(3) Uani 0.744(8) 1 d PD A 1 C10 C 0.61900(14) 1.2566(3) 1.0316(2) 0.0311(15) Uani 0.744(8) 1 d PD A 1 C11 C 0.6382(2) 1.2414(7) 1.0994(3) 0.0350(17) Uani 0.744(8) 1 d PD A 1 H11 H 0.6224 1.2598 1.142 0.042 Uiso 0.744(8) 1 calc PR A 1 C12 C 0.68041(19) 1.1993(5) 1.1046(3) 0.0397(18) Uani 0.744(8) 1 d PD A 1 C13 C 0.70295(16) 1.1690(4) 1.0425(2) 0.0445(19) Uani 0.744(8) 1 d PD A 1 C14 C 0.6839(2) 1.1846(6) 0.9758(3) 0.050(2) Uani 0.744(8) 1 d PD A 1 H14 H 0.699 1.1637 0.9334 0.06 Uiso 0.744(8) 1 calc PR A 1 C15 C 0.6426(2) 1.2306(7) 0.9698(3) 0.0431(19) Uani 0.744(8) 1 d PD A 1 H15 H 0.6305 1.2444 0.9233 0.052 Uiso 0.744(8) 1 calc PR A 1 C16 C 0.6801(4) 1.2047(11) 1.2363(4) 0.113(6) Uani 0.744(8) 1 d PD A 1 H16A H 0.7008 1.1924 1.2767 0.169 Uiso 0.744(8) 1 calc PR A 1 H16B H 0.6537 1.1637 1.2401 0.169 Uiso 0.744(8) 1 calc PR A 1 H16C H 0.6703 1.2699 1.238 0.169 Uiso 0.744(8) 1 calc PR A 1 O6F O 0.7102(4) 1.1652(11) 0.9156(4) 0.036(5) Uiso 0.256(8) 1 d PD A 2 C10F C 0.61900(14) 1.2566(3) 1.0316(2) 0.0311(15) Uani 0.256(8) 1 d PD A 2 C11F C 0.6435(4) 1.2357(14) 0.9697(3) 0.0431(19) Uani 0.256(8) 1 d PD A 2 H11F H 0.6318 1.2521 0.9235 0.052 Uiso 0.256(8) 1 calc PR A 2 C12F C 0.6852(3) 1.1909(8) 0.9748(3) 0.050(2) Uani 0.256(8) 1 d PD A 2 C13F C 0.70295(16) 1.1690(4) 1.0425(2) 0.0445(19) Uani 0.256(8) 1 d PD A 2 C14F C 0.6786(3) 1.1912(10) 1.1045(3) 0.0397(18) Uani 0.256(8) 1 d PD A 2 H14F H 0.6907 1.1766 1.1508 0.048 Uiso 0.256(8) 1 calc PR A 2 C15F C 0.6367(4) 1.2347(15) 1.0994(4) 0.0350(17) Uani 0.256(8) 1 d PD A 2 H15F H 0.6201 1.2495 1.1419 0.042 Uiso 0.256(8) 1 calc PR A 2 C16F C 0.6937(9) 1.185(2) 0.8429(5) 0.078(12) Uiso 0.256(8) 1 d PD A 2 H16D H 0.7153 1.1611 0.8071 0.117 Uiso 0.256(8) 1 calc PR A 2 H16E H 0.6905 1.2529 0.8367 0.117 Uiso 0.256(8) 1 calc PR A 2 H16F H 0.6642 1.1554 0.8358 0.117 Uiso 0.256(8) 1 calc PR A 2 C17 C 0.92334(18) 1.1837(4) 0.8495(3) 0.0252(14) Uani 1 1 d D . . O9 O 0.8846(4) 1.5064(5) 0.9057(4) 0.097(5) Uani 0.566(7) 1 d PD B 1 C18 C 0.92246(15) 1.2839(3) 0.8280(2) 0.0287(14) Uani 0.566(7) 1 d PD B 1 C19 C 0.9044(5) 1.3471(4) 0.8772(5) 0.052(2) Uani 0.566(7) 1 d PD B 1 H19 H 0.8924 1.3257 0.9219 0.062 Uiso 0.566(7) 1 calc PR B 1 C20 C 0.9040(3) 1.4418(4) 0.8607(4) 0.054(2) Uani 0.566(7) 1 d PD B 1 C21 C 0.92219(19) 1.4736(3) 0.7960(2) 0.0374(17) Uani 0.566(7) 1 d PD B 1 C22 C 0.9411(3) 1.4097(4) 0.7476(4) 0.0318(15) Uani 0.566(7) 1 d PD B 1 H22 H 0.9543 1.4311 0.7037 0.038 Uiso 0.566(7) 1 calc PR B 1 C23 C 0.9407(5) 1.3148(4) 0.7632(5) 0.0278(14) Uani 0.566(7) 1 d PD B 1 H23 H 0.9528 1.2714 0.7296 0.033 Uiso 0.566(7) 1 calc PR B 1 C24 C 0.8680(10) 1.4765(10) 0.9761(8) 0.193(16) Uani 0.566(7) 1 d PD B 1 H24A H 0.8552 1.5301 1.0019 0.289 Uiso 0.566(7) 1 calc PR B 1 H24B H 0.8931 1.4503 1.0042 0.289 Uiso 0.566(7) 1 calc PR B 1 H24C H 0.8445 1.4289 0.9696 0.289 Uiso 0.566(7) 1 calc PR B 1 O9F O 0.9577(4) 1.4507(5) 0.6851(4) 0.049(4) Uani 0.434(7) 1 d PD B 2 C18F C 0.92246(15) 1.2839(3) 0.8280(2) 0.0287(14) Uani 0.434(7) 1 d PD B 2 C19F C 0.9399(6) 1.3158(4) 0.7621(5) 0.0278(14) Uani 0.434(7) 1 d PD B 2 H19F H 0.9514 1.2725 0.7278 0.033 Uiso 0.434(7) 1 calc PR B 2 C20F C 0.9404(3) 1.4102(4) 0.7467(4) 0.0318(15) Uani 0.434(7) 1 d PD B 2 C21F C 0.92219(19) 1.4736(3) 0.7960(2) 0.0374(17) Uani 0.434(7) 1 d PD B 2 C22F C 0.9058(4) 1.4425(4) 0.8621(4) 0.054(2) Uani 0.434(7) 1 d PD B 2 H22F H 0.8946 1.486 0.8965 0.065 Uiso 0.434(7) 1 calc PR B 2 C23F C 0.9056(6) 1.3479(5) 0.8780(5) 0.052(2) Uani 0.434(7) 1 d PD B 2 H23F H 0.894 1.3267 0.923 0.062 Uiso 0.434(7) 1 calc PR B 2 C24F C 0.9683(5) 1.3939(8) 0.6229(5) 0.038(4) Uani 0.434(7) 1 d PD B 2 H24D H 0.9796 1.4336 0.5837 0.057 Uiso 0.434(7) 1 calc PR B 2 H24E H 0.9408 1.3614 0.6067 0.057 Uiso 0.434(7) 1 calc PR B 2 H24F H 0.9915 1.3481 0.6359 0.057 Uiso 0.434(7) 1 calc PR B 2 C25 C 0.94553(19) 1.8658(4) 0.7309(3) 0.0264(14) Uani 1 1 d D . . O12 O 0.9695(3) 1.5870(4) 0.8843(4) 0.051(3) Uani 0.552(7) 1 d PD B 1 C26 C 0.93750(16) 1.7648(3) 0.7478(2) 0.0284(14) Uani 0.552(7) 1 d PD B 1 C27 C 0.9564(5) 1.7258(4) 0.8100(5) 0.0331(19) Uani 0.552(7) 1 d PD B 1 H27 H 0.9729 1.7642 0.8427 0.04 Uiso 0.552(7) 1 calc PR B 1 C28 C 0.9515(3) 1.6316(4) 0.8246(3) 0.0378(18) Uani 0.552(7) 1 d PD B 1 C29 C 0.92586(18) 1.5759(3) 0.7778(2) 0.0356(16) Uani 0.552(7) 1 d PD B 1 C30 C 0.9072(3) 1.6145(4) 0.7161(4) 0.0444(19) Uani 0.552(7) 1 d PD B 1 H30 H 0.8904 1.5763 0.6837 0.053 Uiso 0.552(7) 1 calc PR B 1 C31 C 0.9127(5) 1.7089(5) 0.7008(5) 0.0377(19) Uani 0.552(7) 1 d PD B 1 H31 H 0.8995 1.735 0.6584 0.045 Uiso 0.552(7) 1 calc PR B 1 C32 C 0.9995(4) 1.6365(7) 0.9325(5) 0.045(4) Uani 0.552(7) 1 d PD B 1 H32A H 1.0091 1.5948 0.9717 0.067 Uiso 0.552(7) 1 calc PR B 1 H32B H 0.9836 1.6904 0.9531 0.067 Uiso 0.552(7) 1 calc PR B 1 H32C H 1.0262 1.6579 0.9056 0.067 Uiso 0.552(7) 1 calc PR B 1 O12F O 0.8912(4) 1.5528(6) 0.6643(5) 0.077(5) Uani 0.448(7) 1 d PD B 2 C26F C 0.93750(16) 1.7648(3) 0.7478(2) 0.0284(14) Uani 0.448(7) 1 d PD B 2 C27F C 0.9169(6) 1.7074(5) 0.6973(5) 0.0377(19) Uani 0.448(7) 1 d PD B 2 H27F H 0.9065 1.7324 0.6527 0.045 Uiso 0.448(7) 1 calc PR B 2 C28F C 0.9115(3) 1.6127(4) 0.7121(4) 0.0444(19) Uani 0.448(7) 1 d PD B 2 C29F C 0.92586(18) 1.5759(3) 0.7778(2) 0.0356(16) Uani 0.448(7) 1 d PD B 2 C30F C 0.9471(4) 1.6341(5) 0.8278(4) 0.0378(18) Uani 0.448(7) 1 d PD B 2 H30F H 0.9582 1.609 0.8719 0.045 Uiso 0.448(7) 1 calc PR B 2 C31F C 0.9521(6) 1.7286(5) 0.8134(5) 0.0331(19) Uani 0.448(7) 1 d PD B 2 H31F H 0.9655 1.7684 0.8485 0.04 Uiso 0.448(7) 1 calc PR B 2 C32F C 0.8816(10) 1.5840(14) 0.5910(8) 0.176(17) Uani 0.448(7) 1 d PD B 2 H32D H 0.867 1.5335 0.5639 0.263 Uiso 0.448(7) 1 calc PR B 2 H32E H 0.91 1.6015 0.567 0.263 Uiso 0.448(7) 1 calc PR B 2 H32F H 0.8613 1.6381 0.5926 0.263 Uiso 0.448(7) 1 calc PR B 2 O14 O 0.8343(3) 0.9744(8) 1.2787(5) 0.068(3) Uiso 0.537(7) 1 d PD C 1 H14A H 0.8215 1.0134 1.2516 0.103 Uiso 0.537(7) 1 calc PR C 1 C33 C 0.8024(5) 0.9424(10) 1.3341(8) 0.068(3) Uiso 0.537(7) 1 d PD C 1 H33A H 0.8178 0.8938 1.3631 0.082 Uiso 0.537(7) 1 calc PR C 1 H33B H 0.7767 0.9119 1.3089 0.082 Uiso 0.537(7) 1 calc PR C 1 C34 C 0.7832(5) 1.0118(11) 1.3850(8) 0.068(3) Uiso 0.537(7) 1 d PD C 1 H34A H 0.7633 0.9802 1.4197 0.103 Uiso 0.537(7) 1 calc PR C 1 H34B H 0.7657 1.0583 1.3579 0.103 Uiso 0.537(7) 1 calc PR C 1 H34C H 0.8079 1.0428 1.4111 0.103 Uiso 0.537(7) 1 calc PR C 1 O14F O 0.8272(5) 1.0630(11) 1.2661(7) 0.093(4) Uiso 0.463(7) 1 d PD C 2 H14B H 0.8466 1.0409 1.2946 0.14 Uiso 0.463(7) 1 calc PR C 2 C33F C 0.8047(7) 1.1370(13) 1.2995(10) 0.093(4) Uiso 0.463(7) 1 d PD C 2 H33C H 0.7813 1.1629 1.2667 0.112 Uiso 0.463(7) 1 calc PR C 2 H33D H 0.8264 1.1873 1.3116 0.112 Uiso 0.463(7) 1 calc PR C 2 C34F C 0.7819(7) 1.0987(15) 1.3704(9) 0.093(4) Uiso 0.463(7) 1 d PD C 2 H34D H 0.766 1.1495 1.3952 0.14 Uiso 0.463(7) 1 calc PR C 2 H34E H 0.8053 1.073 1.4024 0.14 Uiso 0.463(7) 1 calc PR C 2 H34F H 0.7602 1.0495 1.3578 0.14 Uiso 0.463(7) 1 calc PR C 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 Pb1 0.01201(10) 0.02494(11) 0.02352(10) -0.00062(9) -0.00061(9) -0.00043(9) Pb2 0.01410(10) 0.01928(10) 0.02134(10) -0.00031(9) 0.00110(9) 0.00020(9) Pb3 0.01524(10) 0.02482(11) 0.01904(10) 0.00379(9) 0.00175(9) 0.00377(9) O1 0.013(2) 0.033(2) 0.029(2) -0.0069(18) 0.0016(17) -0.0015(19) O2 0.013(2) 0.033(3) 0.050(3) 0.011(2) -0.0006(19) 0.0055(19) O4 0.017(2) 0.029(2) 0.033(3) 0.0024(19) -0.0032(18) 0.0071(18) O5 0.016(2) 0.029(2) 0.038(3) -0.009(2) 0.0006(18) 0.0029(18) O7 0.031(3) 0.019(2) 0.029(2) 0.0008(18) 0.0033(19) 0.0061(19) O8 0.042(3) 0.023(2) 0.031(2) -0.005(2) 0.002(2) 0.009(2) O10 0.026(2) 0.024(2) 0.031(2) -0.0075(19) 0.0032(18) 0.0019(18) O11 0.031(2) 0.022(2) 0.027(2) 0.0038(19) -0.0005(19) -0.0019(18) O13 0.016(2) 0.023(2) 0.0158(18) 0.0033(16) 0.0003(15) 0.0032(17) C1 0.015(3) 0.019(3) 0.042(4) -0.001(3) -0.006(3) 0.004(3) O3 0.007(3) 0.067(5) 0.085(5) 0.037(4) -0.001(3) 0.000(3) C2 0.011(3) 0.038(4) 0.034(3) 0.001(3) 0.000(3) 0.007(3) C3 0.016(3) 0.037(4) 0.050(5) 0.011(4) 0.000(3) 0.001(3) C4 0.021(4) 0.065(5) 0.038(5) 0.017(4) 0.002(3) 0.005(4) C5 0.023(4) 0.057(5) 0.041(4) 0.017(4) 0.003(3) 0.019(3) C6 0.027(4) 0.054(5) 0.055(5) 0.027(4) 0.011(4) 0.016(4) C7 0.024(4) 0.037(4) 0.047(5) 0.017(4) 0.009(3) 0.010(3) C8 0.020(6) 0.107(11) 0.203(17) 0.103(11) 0.022(7) 0.003(6) C2F 0.011(3) 0.038(4) 0.034(3) 0.001(3) 0.000(3) 0.007(3) C3F 0.024(4) 0.037(4) 0.047(5) 0.017(4) 0.009(3) 0.010(3) C4F 0.027(4) 0.054(5) 0.055(5) 0.027(4) 0.011(4) 0.016(4) C5F 0.023(4) 0.057(5) 0.041(4) 0.017(4) 0.003(3) 0.019(3) C6F 0.021(4) 0.065(5) 0.038(5) 0.017(4) 0.002(3) 0.005(4) C7F 0.016(3) 0.037(4) 0.050(5) 0.011(4) 0.000(3) 0.001(3) C9 0.018(3) 0.026(3) 0.032(4) -0.004(3) -0.002(3) 0.005(3) O6 0.022(4) 0.125(7) 0.040(4) 0.011(4) -0.004(3) 0.023(4) C10 0.017(3) 0.045(4) 0.032(4) 0.007(3) 0.002(3) 0.010(3) C11 0.026(4) 0.048(4) 0.032(4) 0.005(3) 0.009(3) 0.009(3) C12 0.023(4) 0.064(5) 0.032(4) 0.008(4) -0.007(3) 0.018(3) C13 0.022(4) 0.062(5) 0.049(5) 0.017(4) 0.009(3) 0.019(4) C14 0.029(4) 0.087(6) 0.033(4) 0.009(4) 0.008(3) 0.028(4) C15 0.034(4) 0.064(5) 0.030(4) 0.000(3) 0.001(3) 0.024(4) C16 0.067(10) 0.216(19) 0.055(9) 0.023(10) 0.006(7) 0.052(11) C10F 0.017(3) 0.045(4) 0.032(4) 0.007(3) 0.002(3) 0.010(3) C11F 0.034(4) 0.064(5) 0.030(4) 0.000(3) 0.001(3) 0.024(4) C12F 0.029(4) 0.087(6) 0.033(4) 0.009(4) 0.008(3) 0.028(4) C13F 0.022(4) 0.062(5) 0.049(5) 0.017(4) 0.009(3) 0.019(4) C14F 0.023(4) 0.064(5) 0.032(4) 0.008(4) -0.007(3) 0.018(3) C15F 0.026(4) 0.048(4) 0.032(4) 0.005(3) 0.009(3) 0.009(3) C17 0.018(3) 0.025(3) 0.032(4) -0.008(3) -0.007(3) 0.008(3) O9 0.174(12) 0.025(5) 0.092(8) 0.015(5) 0.087(8) 0.039(6) C18 0.030(4) 0.022(3) 0.034(4) 0.003(3) 0.003(3) 0.007(3) C19 0.069(6) 0.028(4) 0.057(5) 0.004(4) 0.023(4) 0.012(4) C20 0.077(6) 0.026(4) 0.060(5) -0.005(4) 0.026(4) 0.009(4) C21 0.048(5) 0.024(4) 0.040(4) 0.001(3) 0.008(3) 0.007(3) C22 0.036(4) 0.029(4) 0.030(4) 0.000(3) 0.006(3) 0.002(3) C23 0.029(4) 0.025(3) 0.030(4) -0.008(3) 0.001(3) 0.001(3) C24 0.42(4) 0.039(10) 0.117(16) 0.028(10) 0.20(2) 0.075(17) O9F 0.082(10) 0.018(6) 0.047(7) -0.002(5) 0.025(6) -0.003(6) C18F 0.030(4) 0.022(3) 0.034(4) 0.003(3) 0.003(3) 0.007(3) C19F 0.029(4) 0.025(3) 0.030(4) -0.008(3) 0.001(3) 0.001(3) C20F 0.036(4) 0.029(4) 0.030(4) 0.000(3) 0.006(3) 0.002(3) C21F 0.048(5) 0.024(4) 0.040(4) 0.001(3) 0.008(3) 0.007(3) C22F 0.077(6) 0.026(4) 0.060(5) -0.005(4) 0.026(4) 0.009(4) C23F 0.069(6) 0.028(4) 0.057(5) 0.004(4) 0.023(4) 0.012(4) C24F 0.066(12) 0.017(8) 0.031(8) -0.007(6) -0.002(8) 0.001(7) C25 0.019(3) 0.024(3) 0.036(4) 0.001(3) -0.004(3) 0.001(3) O12 0.090(8) 0.018(4) 0.045(5) 0.008(4) -0.021(5) 0.009(5) C26 0.035(4) 0.022(3) 0.028(3) -0.006(3) 0.003(3) 0.000(3) C27 0.049(5) 0.027(4) 0.023(3) -0.007(3) 0.006(3) -0.001(3) C28 0.057(5) 0.029(4) 0.027(4) -0.002(3) 0.005(3) 0.007(3) C29 0.041(4) 0.026(4) 0.040(4) -0.001(3) 0.008(3) 0.000(3) C30 0.046(5) 0.034(4) 0.054(5) -0.003(4) -0.010(4) -0.013(4) C31 0.041(5) 0.026(4) 0.046(4) 0.004(3) -0.011(4) -0.003(3) C32 0.073(10) 0.027(7) 0.035(7) -0.006(6) -0.014(7) 0.013(6) O12F 0.110(12) 0.040(7) 0.082(10) 0.011(7) -0.042(9) -0.034(8) C26F 0.035(4) 0.022(3) 0.028(3) -0.006(3) 0.003(3) 0.000(3) C27F 0.041(5) 0.026(4) 0.046(4) 0.004(3) -0.011(4) -0.003(3) C28F 0.046(5) 0.034(4) 0.054(5) -0.003(4) -0.010(4) -0.013(4) C29F 0.041(4) 0.026(4) 0.040(4) -0.001(3) 0.008(3) 0.000(3) C30F 0.057(5) 0.029(4) 0.027(4) -0.002(3) 0.005(3) 0.007(3) C31F 0.049(5) 0.027(4) 0.023(3) -0.007(3) 0.006(3) -0.001(3) C32F 0.23(4) 0.09(2) 0.21(4) 0.05(2) -0.13(3) -0.10(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O13 2.256(3) . ? Pb1 O10 2.524(4) 1_545 ? Pb1 O7 2.526(4) . ? Pb1 O8 2.610(4) . ? Pb1 O4 2.656(4) 8_755 ? Pb1 O1 2.690(4) . ? Pb1 Pb2 3.6302(3) . ? Pb2 O13 2.294(3) 5_777 ? Pb2 O13 2.310(3) . ? Pb2 O4 2.522(4) 4_577 ? Pb2 O1 2.617(4) . ? Pb2 Pb2 3.6206(4) 5_777 ? Pb3 O13 2.348(3) . ? Pb3 O2 2.422(4) 5_777 ? Pb3 O11 2.442(4) 3_746 ? Pb3 O5 2.604(4) 4_577 ? Pb3 Pb3 3.6983(4) 3_756 ? O1 C1 1.247(6) . ? O2 C1 1.283(7) . ? O2 Pb3 2.422(4) 5_777 ? O4 C9 1.275(7) . ? O4 Pb2 2.522(4) 4_477 ? O4 Pb1 2.656(4) 8_765 ? O5 C9 1.235(7) . ? O5 Pb3 2.604(4) 4_477 ? O7 C17 1.272(7) . ? O8 C17 1.262(6) . ? O10 C25 1.250(7) . ? O10 Pb1 2.524(4) 1_565 ? O11 C25 1.271(7) . ? O11 Pb3 2.442(4) 3_766 ? O13 Pb2 2.294(3) 5_777 ? C1 C2 1.496(6) . ? O3 C4 1.367(5) . ? O3 C8 1.446(7) . ? C2 C7 1.386(5) . ? C2 C3 1.387(5) . ? C3 C4 1.393(5) . ? C4 C5 1.389(5) . ? C5 C6 1.389(5) . ? C5 C13 1.513(6) . ? C6 C7 1.393(5) . ? O3F C4F 1.371(7) . ? O3F C8F 1.442(9) . ? C3F C4F 1.390(6) . ? C6F C7F 1.390(6) . ? C9 C10 1.494(7) . ? O6 C12 1.373(5) . ? O6 C16 1.443(7) . ? C10 C15 1.388(5) . ? C10 C11 1.391(5) . ? C11 C12 1.389(5) . ? C12 C13 1.396(5) . ? C13 C14 1.373(5) . ? C14 C15 1.390(5) . ? O6F C12F 1.370(6) . ? O6F C16F 1.458(9) . ? C11F C12F 1.390(6) . ? C14F C15F 1.389(6) . ? C17 C18 1.491(7) . ? O9 C20 1.371(6) . ? O9 C24 1.453(8) . ? C18 C23 1.385(5) . ? C18 C19 1.389(5) . ? C19 C20 1.391(5) . ? C20 C21 1.388(5) . ? C21 C22 1.396(5) . ? C21 C29 1.509(6) . ? C22 C23 1.391(5) . ? O9F C20F 1.377(6) . ? O9F C24F 1.443(8) . ? C19F C20F 1.384(5) . ? C22F C23F 1.387(6) . ? C25 C26 1.501(7) . ? O12 C28 1.382(6) . ? O12 C32 1.443(8) . ? C26 C31 1.390(6) . ? C26 C27 1.395(5) . ? C27 C28 1.386(5) . ? C28 C29 1.398(5) . ? C29 C30 1.383(5) . ? C30 C31 1.392(6) . ? O12F C28F 1.370(6) . ? O12F C32F 1.454(9) . ? C27F C28F 1.394(5) . ? C30F C31F 1.388(6) . ? O14 C33 1.465(13) . ? C33 C34 1.481(13) . ? O14F C33F 1.398(15) . ? C33F C34F 1.571(16) . ? 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 O13 Pb1 O10 81.42(12) . 1_545 ? O13 Pb1 O7 80.58(13) . . ? O10 Pb1 O7 120.46(12) 1_545 . ? O13 Pb1 O8 79.63(12) . . ? O10 Pb1 O8 70.09(12) 1_545 . ? O7 Pb1 O8 51.00(12) . . ? O13 Pb1 O4 74.10(12) . 8_755 ? O10 Pb1 O4 88.15(12) 1_545 8_755 ? O7 Pb1 O4 138.25(12) . 8_755 ? O8 Pb1 O4 148.10(12) . 8_755 ? O13 Pb1 O1 73.55(11) . . ? O10 Pb1 O1 149.23(12) 1_545 . ? O7 Pb1 O1 73.14(12) . . ? O8 Pb1 O1 121.02(12) . . ? O4 Pb1 O1 68.18(12) 8_755 . ? O13 Pb1 Pb2 37.87(9) . . ? O10 Pb1 Pb2 117.18(9) 1_545 . ? O7 Pb1 Pb2 52.77(9) . . ? O8 Pb1 Pb2 81.84(9) . . ? O4 Pb1 Pb2 88.22(8) 8_755 . ? O1 Pb1 Pb2 46.01(8) . . ? O13 Pb2 O13 76.32(13) 5_777 . ? O13 Pb2 O4 76.19(13) 5_777 4_577 ? O13 Pb2 O4 104.55(12) . 4_577 ? O13 Pb2 O1 79.15(12) 5_777 . ? O13 Pb2 O1 74.18(12) . . ? O4 Pb2 O1 154.81(12) 4_577 . ? O13 Pb2 Pb2 38.32(8) 5_777 5_777 ? O13 Pb2 Pb2 38.00(8) . 5_777 ? O4 Pb2 Pb2 90.52(9) 4_577 5_777 ? O1 Pb2 Pb2 72.95(8) . 5_777 ? O13 Pb2 Pb1 96.02(9) 5_777 . ? O13 Pb2 Pb1 36.83(8) . . ? O4 Pb2 Pb1 140.25(9) 4_577 . ? O1 Pb2 Pb1 47.69(8) . . ? Pb2 Pb2 Pb1 63.620(7) 5_777 . ? O13 Pb3 O2 115.63(13) . 5_777 ? O13 Pb3 O11 81.28(13) . 3_746 ? O2 Pb3 O11 73.29(13) 5_777 3_746 ? O13 Pb3 O5 80.08(12) . 4_577 ? O2 Pb3 O5 77.28(13) 5_777 4_577 ? O11 Pb3 O5 133.57(13) 3_746 4_577 ? O13 Pb3 Pb3 105.55(8) . 3_756 ? O2 Pb3 Pb3 135.40(10) 5_777 3_756 ? O11 Pb3 Pb3 97.81(9) 3_746 3_756 ? O5 Pb3 Pb3 128.10(9) 4_577 3_756 ? C1 O1 Pb2 138.1(3) . . ? C1 O1 Pb1 131.3(3) . . ? Pb2 O1 Pb1 86.29(11) . . ? C1 O2 Pb3 109.2(3) . 5_777 ? C9 O4 Pb2 100.9(3) . 4_477 ? C9 O4 Pb1 131.6(3) . 8_765 ? Pb2 O4 Pb1 95.12(12) 4_477 8_765 ? C9 O5 Pb3 130.0(4) . 4_477 ? C17 O7 Pb1 94.9(3) . . ? C17 O8 Pb1 91.3(4) . . ? C25 O10 Pb1 139.1(4) . 1_565 ? C25 O11 Pb3 103.9(3) . 3_766 ? Pb1 O13 Pb2 114.26(15) . 5_777 ? Pb1 O13 Pb2 105.30(13) . . ? Pb2 O13 Pb2 103.68(13) 5_777 . ? Pb1 O13 Pb3 113.92(14) . . ? Pb2 O13 Pb3 106.99(13) 5_777 . ? Pb2 O13 Pb3 112.32(14) . . ? O1 C1 O2 123.0(5) . . ? O1 C1 C2 121.1(5) . . ? O2 C1 C2 115.9(5) . . ? C4 O3 C8 118.7(5) . . ? C7 C2 C3 120.3(4) . . ? C7 C2 C1 119.1(4) . . ? C3 C2 C1 120.7(4) . . ? C2 C3 C4 119.6(4) . . ? O3 C4 C5 116.5(4) . . ? O3 C4 C3 122.9(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 119.2(4) . . ? C4 C5 C13 121.0(4) . . ? C6 C5 C13 119.8(4) . . ? C5 C6 C7 120.5(4) . . ? C2 C7 C6 119.6(4) . . ? C4F O3F C8F 120.6(9) . . ? O3F C4F C3F 123.7(6) . . ? O5 C9 O4 122.5(5) . . ? O5 C9 C10 120.3(5) . . ? O4 C9 C10 117.1(5) . . ? C12 O6 C16 119.5(6) . . ? C15 C10 C11 119.7(4) . . ? C15 C10 C9 119.2(4) . . ? C11 C10 C9 121.2(4) . . ? C12 C11 C10 119.7(4) . . ? O6 C12 C11 123.6(4) . . ? O6 C12 C13 115.9(4) . . ? C11 C12 C13 120.4(4) . . ? C14 C13 C12 119.5(4) . . ? C14 C13 C5 121.1(4) . . ? C12 C13 C5 119.4(4) . . ? C13 C14 C15 120.5(4) . . ? C10 C15 C14 120.1(4) . . ? C12F O6F C16F 120.1(8) . . ? O6F C12F C11F 123.2(5) . . ? O8 C17 O7 121.6(5) . . ? O8 C17 C18 119.4(5) . . ? O7 C17 C18 118.9(5) . . ? C20 O9 C24 118.9(6) . . ? C23 C18 C19 120.4(4) . . ? C23 C18 C17 122.1(4) . . ? C19 C18 C17 117.5(4) . . ? C18 C19 C20 119.8(4) . . ? O9 C20 C21 117.5(5) . . ? O9 C20 C19 122.1(5) . . ? C21 C20 C19 120.4(4) . . ? C20 C21 C22 119.3(4) . . ? C20 C21 C29 122.6(4) . . ? C22 C21 C29 117.9(4) . . ? C23 C22 C21 120.4(4) . . ? C18 C23 C22 119.7(4) . . ? C20F O9F C24F 120.0(6) . . ? O9F C20F C19F 125.9(5) . . ? O10 C25 O11 122.4(5) . . ? O10 C25 C26 120.4(5) . . ? O11 C25 C26 117.0(5) . . ? C28 O12 C32 120.1(6) . . ? C31 C26 C27 119.7(4) . . ? C31 C26 C25 120.6(4) . . ? C27 C26 C25 119.7(4) . . ? C28 C27 C26 120.5(4) . . ? O12 C28 C27 124.5(5) . . ? O12 C28 C29 115.9(4) . . ? C27 C28 C29 119.6(4) . . ? C30 C29 C28 119.7(4) . . ? C30 C29 C21 123.0(4) . . ? C28 C29 C21 117.2(4) . . ? C29 C30 C31 120.7(4) . . ? C26 C31 C30 119.7(4) . . ? C28F O12F C32F 119.5(7) . . ? O12F C28F C27F 122.3(5) . . ? O14 C33 C34 118.6(12) . . ? O14F C33F C34F 107.8(13) . . ? #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------# data_x0443fin _database_code_depnum_ccdc_archive 'CCDC 911251' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2012-11-16T14:20:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C16 H18 O2' _chemical_formula_weight 242.3 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 15.1458(6) _cell_length_b 20.2514(9) _cell_length_c 8.6838(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2663.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2073 _cell_measurement_theta_min 2.6735 _cell_measurement_theta_max 32.1816 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.99175 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0327008003 _diffrn_orient_matrix_ub_12 -0.0415742728 _diffrn_orient_matrix_ub_13 0.0075215942 _diffrn_orient_matrix_ub_21 0.0158030317 _diffrn_orient_matrix_ub_22 0.0145941784 _diffrn_orient_matrix_ub_23 0.0324874936 _diffrn_orient_matrix_ub_31 -0.0728411554 _diffrn_orient_matrix_ub_32 -0.0155216185 _diffrn_orient_matrix_ub_33 0.0103862555 _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_number 3551 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 1073 _reflns_number_gt 936 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1073 _refine_ls_number_parameters 107 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_diff_density_max 0.283 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.042 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 O 0.02104(8) 0.06996(7) 0.64697(15) 0.0293(3) Uani 1 1 d . . . C1 C 0.07952(10) 0.05216(8) 0.5357(2) 0.0204(3) Uani 1 1 d . . . C2 C 0.16689(10) 0.07342(8) 0.5325(2) 0.0218(3) Uani 1 1 d . . . C3 C 0.22221(10) 0.05638(8) 0.4108(2) 0.0224(3) Uani 1 1 d . . . C4 C 0.18863(10) 0.01855(8) 0.2913(2) 0.0253(4) Uani 1 1 d . . . C5 C 0.10170(10) -0.00313(8) 0.2956(2) 0.0235(3) Uani 1 1 d . . . C6 C 0.04627(9) 0.01208(7) 0.4178(2) 0.0196(3) Uani 1 1 d . . . C7 C 0.31670(11) 0.07878(10) 0.4097(2) 0.0326(4) Uani 1 1 d . . . H7A H 0.3199 0.1242 0.3709 0.049 Uiso 1 1 calc R . . H7B H 0.3514 0.0497 0.3428 0.049 Uiso 1 1 calc R . . H7C H 0.3404 0.0771 0.5146 0.049 Uiso 1 1 calc R . . C8 C 0.05397(13) 0.10403(11) 0.7779(3) 0.0345(4) Uani 1 1 d . . . H2 H 0.1887(14) 0.0970(12) 0.613(3) 0.031(6) Uiso 1 1 d . . . H4 H 0.2255(13) 0.0094(12) 0.203(3) 0.026(6) Uiso 1 1 d . . . H5 H 0.0762(15) -0.0310(12) 0.207(3) 0.030(6) Uiso 1 1 d . . . H8A H 0.0998(18) 0.0758(12) 0.829(3) 0.039(7) Uiso 1 1 d . . . H8B H 0.0787(15) 0.1469(12) 0.753(3) 0.035(6) Uiso 1 1 d . . . H8C H 0.0012(18) 0.1087(13) 0.843(4) 0.052(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0225(6) 0.0383(7) 0.0271(7) -0.0127(6) 0.0050(5) -0.0047(5) C1 0.0203(7) 0.0207(7) 0.0203(7) 0.0008(6) 0.0006(7) 0.0008(5) C2 0.0192(7) 0.0234(7) 0.0227(8) 0.0003(7) -0.0017(6) -0.0017(5) C3 0.0189(6) 0.0226(7) 0.0258(8) 0.0042(7) -0.0006(7) 0.0005(6) C4 0.0229(7) 0.0263(8) 0.0267(8) -0.0002(8) 0.0055(7) -0.0001(6) C5 0.0244(7) 0.0226(7) 0.0234(8) -0.0015(7) 0.0024(7) -0.0032(6) C6 0.0178(6) 0.0192(7) 0.0217(8) 0.0020(6) 0.0002(6) -0.0007(5) C7 0.0198(7) 0.0457(10) 0.0323(10) 0.0042(9) 0.0009(8) -0.0064(7) C8 0.0332(9) 0.0439(11) 0.0265(10) -0.0129(9) 0.0046(8) -0.0098(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.359(2) . ? O1 C8 1.420(2) . ? C1 C2 1.392(2) . ? C1 C6 1.400(2) . ? C2 C3 1.392(2) . ? C2 H2 0.91(2) . ? C3 C4 1.386(3) . ? C3 C7 1.501(2) . ? C4 C5 1.388(2) . ? C4 H4 0.97(2) . ? C5 C6 1.388(2) . ? C5 H5 1.03(3) . ? C6 C6 1.485(3) 2 ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 1.00(3) . ? C8 H8B 0.97(3) . ? C8 H8C 0.99(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C8 117.96(14) . . ? O1 C1 C2 123.49(15) . . ? O1 C1 C6 116.04(13) . . ? C2 C1 C6 120.43(15) . . ? C1 C2 C3 120.72(15) . . ? C1 C2 H2 119.4(14) . . ? C3 C2 H2 119.8(14) . . ? C4 C3 C2 118.96(14) . . ? C4 C3 C7 120.79(16) . . ? C2 C3 C7 120.25(16) . . ? C3 C4 C5 120.18(17) . . ? C3 C4 H4 119.3(13) . . ? C5 C4 H4 120.5(13) . . ? C6 C5 C4 121.59(17) . . ? C6 C5 H5 117.9(13) . . ? C4 C5 H5 120.5(13) . . ? C5 C6 C1 118.05(13) . . ? C5 C6 C6 119.86(11) . 2 ? C1 C6 C6 122.05(11) . 2 ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 H8A 108.8(15) . . ? O1 C8 H8B 113.3(16) . . ? H8A C8 H8B 110(2) . . ? O1 C8 H8C 102.9(17) . . ? H8A C8 H8C 111(2) . . ? H8B C8 H8C 111(2) . . ? # END of CIF #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#