# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_11slbktl2 _database_code_depnum_ccdc_archive 'CCDC 900327' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-12 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(nitrato-O,O')-1,4,7,10,13-pentaoxacyclopentadecane-lead(II) ; # C10H20O5 # 15-crown-5 # 1,4,7,10,13-Pentaoxacyclopentadecane (chemspider) # 1,4,7,10,13-pentaoxacyclopentadecane (iLab defaults) # SMILES: C1OCCOCCOCCOCCOC1 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 N2 O11 Pb' _chemical_formula_sum 'C10 H20 N2 O11 Pb' _chemical_formula_structural '((C10 H20 O5) (N O3)2 Pb)' _chemical_formula_weight 551.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.307(4) _cell_length_b 8.303(2) _cell_length_c 13.152(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.815(4) _cell_angle_gamma 90.00 _cell_volume 1669.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4668 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 31.1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 10.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.708 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9241 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3811 _reflns_number_gt 3467 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3811 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.257395(10) 0.579480(18) 0.094054(11) 0.01328(7) Uani 1 1 d . . . O1 O 0.1974(2) 0.4085(3) -0.0686(3) 0.0237(8) Uani 1 1 d . . . O2 O 0.1017(2) 0.6764(4) 0.0075(2) 0.0202(7) Uani 1 1 d . . . O3 O 0.2100(2) 0.8898(4) 0.1239(3) 0.0195(7) Uani 1 1 d . . . O4 O 0.3483(2) 0.8160(4) 0.0046(3) 0.0207(7) Uani 1 1 d . . . O5 O 0.3780(2) 0.4935(4) -0.0406(2) 0.0222(7) Uani 1 1 d . . . O6 O 0.3896(2) 0.6257(4) 0.2193(3) 0.0286(8) Uani 1 1 d . . . O7 O 0.3501(2) 0.3742(4) 0.2020(3) 0.0248(7) Uani 1 1 d . . . O8 O 0.4523(3) 0.4409(4) 0.3150(3) 0.0359(9) Uani 1 1 d . . . O9 O 0.1746(2) 0.5747(3) 0.2608(3) 0.0262(8) Uani 1 1 d . . . O10 O 0.1430(2) 0.3673(4) 0.1644(2) 0.0207(7) Uani 1 1 d . . . O11 O 0.0716(3) 0.4106(4) 0.3002(3) 0.0342(10) Uani 1 1 d . . . N1 N 0.3980(3) 0.4793(5) 0.2472(3) 0.0224(9) Uani 1 1 d . . . N2 N 0.1293(3) 0.4487(5) 0.2424(3) 0.0200(8) Uani 1 1 d . . . C1 C 0.1063(4) 0.4412(6) -0.0938(5) 0.0289(12) Uani 1 1 d . . . H1A H 0.0702 0.3862 -0.0440 0.035 Uiso 1 1 calc R . . H1B H 0.0906 0.3960 -0.1619 0.035 Uiso 1 1 calc R . . C2 C 0.0856(3) 0.6155(6) -0.0941(4) 0.0257(11) Uani 1 1 d . . . H2A H 0.1227 0.6730 -0.1419 0.031 Uiso 1 1 calc R . . H2B H 0.0235 0.6326 -0.1163 0.031 Uiso 1 1 calc R . . C3 C 0.0785(3) 0.8436(5) 0.0158(4) 0.0199(10) Uani 1 1 d . . . H3A H 0.0140 0.8555 0.0130 0.024 Uiso 1 1 calc R . . H3B H 0.1018 0.9055 -0.0413 0.024 Uiso 1 1 calc R . . C4 C 0.1168(3) 0.9059(5) 0.1155(4) 0.0213(10) Uani 1 1 d . . . H4A H 0.1011 1.0209 0.1226 0.026 Uiso 1 1 calc R . . H4B H 0.0910 0.8460 0.1718 0.026 Uiso 1 1 calc R . . C5 C 0.2555(3) 1.0113(5) 0.0692(4) 0.0215(10) Uani 1 1 d . . . H5A H 0.2517 1.1164 0.1043 0.026 Uiso 1 1 calc R . . H5B H 0.2289 1.0228 -0.0006 0.026 Uiso 1 1 calc R . . C6 C 0.3492(3) 0.9602(6) 0.0652(4) 0.0246(11) Uani 1 1 d . . . H6A H 0.3842 1.0451 0.0335 0.029 Uiso 1 1 calc R . . H6B H 0.3745 0.9384 0.1345 0.029 Uiso 1 1 calc R . . C7 C 0.4350(3) 0.7593(6) -0.0140(4) 0.0271(11) Uani 1 1 d . . . H7A H 0.4650 0.7223 0.0502 0.033 Uiso 1 1 calc R . . H7B H 0.4701 0.8464 -0.0432 0.033 Uiso 1 1 calc R . . C8 C 0.4242(3) 0.6231(7) -0.0874(4) 0.0307(12) Uani 1 1 d . . . H8A H 0.3910 0.6596 -0.1496 0.037 Uiso 1 1 calc R . . H8B H 0.4823 0.5850 -0.1071 0.037 Uiso 1 1 calc R . . C9 C 0.3446(4) 0.3769(6) -0.1138(4) 0.0273(11) Uani 1 1 d . . . H9A H 0.3445 0.2689 -0.0818 0.033 Uiso 1 1 calc R . . H9B H 0.3834 0.3727 -0.1718 0.033 Uiso 1 1 calc R . . C10 C 0.2528(4) 0.4191(5) -0.1524(4) 0.0278(12) Uani 1 1 d . . . H10A H 0.2513 0.5295 -0.1808 0.033 Uiso 1 1 calc R . . H10B H 0.2328 0.3432 -0.2068 0.033 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 Pb1 0.00983(9) 0.01561(11) 0.01463(10) 0.00098(5) 0.00313(6) -0.00014(6) O1 0.0249(19) 0.0250(18) 0.0214(18) -0.0047(13) 0.0028(15) -0.0002(15) O2 0.0145(15) 0.0222(16) 0.0237(16) 0.0014(13) 0.0004(13) 0.0032(14) O3 0.0132(16) 0.0196(15) 0.0260(18) 0.0010(13) 0.0049(13) 0.0003(13) O4 0.0119(15) 0.0208(16) 0.0299(18) -0.0022(13) 0.0073(13) -0.0017(13) O5 0.0217(18) 0.0226(18) 0.0231(17) 0.0011(14) 0.0095(14) 0.0017(15) O6 0.033(2) 0.0241(17) 0.0286(19) 0.0063(15) -0.0042(16) -0.0085(17) O7 0.0203(18) 0.0201(15) 0.034(2) 0.0045(15) -0.0004(15) -0.0015(15) O8 0.023(2) 0.049(2) 0.034(2) 0.0122(17) -0.0112(17) -0.0001(18) O9 0.028(2) 0.027(2) 0.0246(19) -0.0064(13) 0.0100(16) -0.0081(15) O10 0.0157(16) 0.0236(16) 0.0234(17) -0.0033(14) 0.0057(13) -0.0023(14) O11 0.032(2) 0.038(2) 0.035(2) 0.0027(15) 0.0213(18) -0.0115(17) N1 0.0119(19) 0.035(2) 0.020(2) 0.0064(18) 0.0002(15) -0.0018(18) N2 0.019(2) 0.020(2) 0.021(2) 0.0048(16) 0.0093(16) 0.0007(17) C1 0.022(3) 0.032(3) 0.032(3) -0.005(2) -0.001(2) -0.007(2) C2 0.017(2) 0.034(3) 0.025(3) 0.002(2) -0.003(2) 0.000(2) C3 0.010(2) 0.020(2) 0.030(2) 0.0077(18) 0.0033(18) 0.0014(19) C4 0.016(2) 0.022(2) 0.027(3) 0.0017(18) 0.008(2) 0.0034(19) C5 0.019(2) 0.012(2) 0.033(3) 0.0040(18) 0.001(2) -0.0011(19) C6 0.016(2) 0.022(2) 0.036(3) 0.000(2) 0.004(2) -0.009(2) C7 0.012(2) 0.030(3) 0.040(3) 0.006(2) 0.013(2) 0.001(2) C8 0.025(3) 0.031(3) 0.037(3) 0.003(2) 0.022(2) 0.000(2) C9 0.032(3) 0.025(2) 0.026(3) -0.007(2) 0.012(2) 0.005(2) C10 0.036(3) 0.029(3) 0.019(2) -0.0051(18) 0.005(2) 0.001(2) _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 O6 2.574(4) . ? Pb1 O9 2.586(3) . ? Pb1 O7 2.596(3) . ? Pb1 O10 2.681(3) . ? Pb1 O1 2.691(3) . ? Pb1 O4 2.709(3) . ? Pb1 O2 2.712(3) . ? Pb1 O3 2.711(3) . ? Pb1 O5 2.716(3) . ? O1 C10 1.426(6) . ? O1 C1 1.443(6) . ? O2 C2 1.439(6) . ? O2 C3 1.439(5) . ? O3 C4 1.431(6) . ? O3 C5 1.439(5) . ? O4 C6 1.437(6) . ? O4 C7 1.441(5) . ? O5 C9 1.441(6) . ? O5 C8 1.442(6) . ? O6 N1 1.274(5) . ? O7 N1 1.268(5) . ? O8 N1 1.230(5) . ? O9 N2 1.272(5) . ? O10 N2 1.255(5) . ? O11 N2 1.234(5) . ? C1 C2 1.482(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.499(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.490(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.512(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 O6 Pb1 O9 82.07(12) . . ? O6 Pb1 O7 49.93(11) . . ? O9 Pb1 O7 78.69(11) . . ? O6 Pb1 O10 112.54(10) . . ? O9 Pb1 O10 48.84(9) . . ? O7 Pb1 O10 74.27(10) . . ? O6 Pb1 O1 144.50(11) . . ? O9 Pb1 O1 120.24(11) . . ? O7 Pb1 O1 104.15(11) . . ? O10 Pb1 O1 74.00(10) . . ? O6 Pb1 O4 76.46(11) . . ? O9 Pb1 O4 131.52(9) . . ? O7 Pb1 O4 115.78(10) . . ? O10 Pb1 O4 169.91(10) . . ? O1 Pb1 O4 101.51(10) . . ? O6 Pb1 O2 150.58(11) . . ? O9 Pb1 O2 84.45(11) . . ? O7 Pb1 O2 150.47(10) . . ? O10 Pb1 O2 76.37(10) . . ? O1 Pb1 O2 64.18(10) . . ? O4 Pb1 O2 93.55(9) . . ? O6 Pb1 O3 88.47(11) . . ? O9 Pb1 O3 75.27(10) . . ? O7 Pb1 O3 133.47(11) . . ? O10 Pb1 O3 112.99(9) . . ? O1 Pb1 O3 122.23(10) . . ? O4 Pb1 O3 61.36(9) . . ? O2 Pb1 O3 62.78(10) . . ? O6 Pb1 O5 85.33(12) . . ? O9 Pb1 O5 157.82(11) . . ? O7 Pb1 O5 79.23(11) . . ? O10 Pb1 O5 121.92(9) . . ? O1 Pb1 O5 63.84(11) . . ? O4 Pb1 O5 61.79(9) . . ? O2 Pb1 O5 114.56(10) . . ? O3 Pb1 O5 122.67(9) . . ? C10 O1 C1 114.5(4) . . ? C10 O1 Pb1 112.9(3) . . ? C1 O1 Pb1 111.8(3) . . ? C2 O2 C3 112.2(4) . . ? C2 O2 Pb1 113.1(3) . . ? C3 O2 Pb1 118.1(2) . . ? C4 O3 C5 113.7(3) . . ? C4 O3 Pb1 110.5(2) . . ? C5 O3 Pb1 117.0(2) . . ? C6 O4 C7 112.5(4) . . ? C6 O4 Pb1 110.7(3) . . ? C7 O4 Pb1 109.5(2) . . ? C9 O5 C8 112.4(4) . . ? C9 O5 Pb1 112.5(3) . . ? C8 O5 Pb1 116.4(3) . . ? N1 O6 Pb1 96.2(3) . . ? N1 O7 Pb1 95.3(3) . . ? N2 O9 Pb1 97.9(2) . . ? N2 O10 Pb1 93.8(2) . . ? O8 N1 O7 121.0(4) . . ? O8 N1 O6 120.7(4) . . ? O7 N1 O6 118.2(4) . . ? O11 N2 O10 121.2(4) . . ? O11 N2 O9 119.6(4) . . ? O10 N2 O9 119.1(4) . . ? O1 C1 C2 112.9(4) . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 108.3(4) . . ? O2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? O2 C3 C4 108.1(4) . . ? O2 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O3 C4 C3 112.3(4) . . ? O3 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? O3 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? O3 C5 C6 107.9(4) . . ? O3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O4 C6 C5 105.8(4) . . ? O4 C6 H6A 110.6 . . ? C5 C6 H6A 110.6 . . ? O4 C6 H6B 110.6 . . ? C5 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? O4 C7 C8 106.5(4) . . ? O4 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O4 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O5 C8 C7 109.4(4) . . ? O5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 111.2(4) . . ? O5 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? O5 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O1 C10 C9 107.7(4) . . ? O1 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O1 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 O1 C1 C2 -84.0(5) . . . . ? Pb1 O1 C1 C2 46.1(5) . . . . ? C3 O2 C2 C1 -176.6(4) . . . . ? Pb1 O2 C2 C1 46.8(4) . . . . ? O1 C1 C2 O2 -63.6(6) . . . . ? C2 O2 C3 C4 -166.7(4) . . . . ? Pb1 O2 C3 C4 -32.5(4) . . . . ? C5 O3 C4 C3 78.4(5) . . . . ? Pb1 O3 C4 C3 -55.5(4) . . . . ? O2 C3 C4 O3 59.1(4) . . . . ? C4 O3 C5 C6 -167.7(4) . . . . ? Pb1 O3 C5 C6 -37.0(5) . . . . ? C7 O4 C6 C5 174.9(4) . . . . ? Pb1 O4 C6 C5 -62.3(4) . . . . ? O3 C5 C6 O4 65.4(5) . . . . ? C6 O4 C7 C8 -173.2(4) . . . . ? Pb1 O4 C7 C8 63.2(4) . . . . ? C9 O5 C8 C7 164.4(4) . . . . ? Pb1 O5 C8 C7 32.6(5) . . . . ? O4 C7 C8 O5 -63.9(5) . . . . ? C8 O5 C9 C10 -90.9(5) . . . . ? Pb1 O5 C9 C10 42.9(5) . . . . ? C1 O1 C10 C9 -178.3(4) . . . . ? Pb1 O1 C10 C9 52.1(4) . . . . ? O5 C9 C10 O1 -64.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.471 _refine_diff_density_min -3.036 _refine_diff_density_rms 0.188 data_11pafktl3a _database_code_depnum_ccdc_archive 'CCDC 900328' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-14 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(aqua(1,4,7,10,13,16-hexaoxacyclooctadecane)- (\m~2~-tetrafluoroborate-F,F')lead(II)) tetrafluoroborate ; # C12H24O6 # 18-crown-6 # 1,4,7,10,13,16-hexaoxacyclooctadecane (chemspider) # 1,4,7,10,13,16-hexaoxacyclooctadecane (iLab defaults) # SMILES: C1OCCOCCOCCOCCOCCOC1 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H52 B2 F8 O14 Pb2 2+, 2(B F4 1-)' _chemical_formula_sum 'C24 H52 B4 F16 O14 Pb2' _chemical_formula_structural '((C12 H24 O6)(H2 O)(B F4)Pb)2 (B F4)2' _chemical_formula_weight 1326.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.818(4) _cell_length_b 10.661(3) _cell_length_c 15.298(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.66(2) _cell_angle_gamma 90.00 _cell_volume 2083.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9308 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 8.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.602 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11962 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4753 _reflns_number_gt 3344 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (C-H) difmap (O-H)' _refine_ls_hydrogen_treatment 'constr (C-H) refxyz (O-H)' # or mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4753 _refine_ls_number_parameters 277 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.20840(2) 0.08955(3) 0.897042(18) 0.01270(9) Uani 1 1 d . . . O1 O 0.2213(4) -0.1273(4) 0.8018(3) 0.0173(12) Uani 1 1 d U . . O2 O 0.1395(4) 0.0812(5) 0.7185(3) 0.0183(12) Uani 1 1 d . . . O3 O 0.1361(4) 0.3106(5) 0.8003(3) 0.0188(13) Uani 1 1 d . . . O4 O 0.2690(4) 0.3260(4) 0.9480(3) 0.0162(13) Uani 1 1 d . . . O5 O 0.3246(4) 0.1201(4) 1.0516(3) 0.0165(13) Uani 1 1 d . . . O6 O 0.3269(4) -0.1030(4) 0.9631(3) 0.0168(12) Uani 1 1 d U . . O7 O 0.3764(5) 0.1299(5) 0.8434(4) 0.0198(14) Uani 1 1 d D . . H7X H 0.395(6) 0.206(3) 0.842(5) 0.020 Uiso 1 1 d D . . H7Y H 0.385(6) 0.086(6) 0.798(3) 0.020 Uiso 1 1 d D . . C1 C 0.1964(7) -0.1289(7) 0.7095(5) 0.0197(19) Uani 1 1 d U . . H1A H 0.1759 -0.2147 0.6901 0.024 Uiso 1 1 calc R . . H1B H 0.2581 -0.1033 0.6789 0.024 Uiso 1 1 calc R . . C2 C 0.1092(7) -0.0413(6) 0.6881(5) 0.0189(19) Uani 1 1 d . . . H2A H 0.0916 -0.0396 0.6239 0.023 Uiso 1 1 calc R . . H2B H 0.0466 -0.0692 0.7166 0.023 Uiso 1 1 calc R . . C3 C 0.0645(7) 0.1739(7) 0.6886(5) 0.022(2) Uani 1 1 d . . . H3A H 0.0006 0.1666 0.7205 0.026 Uiso 1 1 calc R . . H3B H 0.0448 0.1636 0.6250 0.026 Uiso 1 1 calc R . . C4 C 0.1164(7) 0.2995(7) 0.7065(5) 0.021(2) Uani 1 1 d . . . H4A H 0.1829 0.3042 0.6780 0.025 Uiso 1 1 calc R . . H4B H 0.0700 0.3681 0.6833 0.025 Uiso 1 1 calc R . . C5 C 0.1847(6) 0.4267(6) 0.8243(5) 0.0171(18) Uani 1 1 d . . . H5A H 0.1389 0.4973 0.8038 0.021 Uiso 1 1 calc R . . H5B H 0.2519 0.4346 0.7972 0.021 Uiso 1 1 calc R . . C6 C 0.2031(7) 0.4292(7) 0.9209(5) 0.021(2) Uani 1 1 d . . . H6A H 0.2370 0.5091 0.9400 0.025 Uiso 1 1 calc R . . H6B H 0.1356 0.4228 0.9479 0.025 Uiso 1 1 calc R . . C7 C 0.3120(7) 0.3427(7) 1.0374(5) 0.0171(19) Uani 1 1 d . . . H7A H 0.2551 0.3453 1.0774 0.020 Uiso 1 1 calc R . . H7B H 0.3514 0.4225 1.0433 0.020 Uiso 1 1 calc R . . C8 C 0.3829(6) 0.2351(6) 1.0602(5) 0.0167(18) Uani 1 1 d . . . H8A H 0.4403 0.2337 1.0207 0.020 Uiso 1 1 calc R . . H8B H 0.4141 0.2442 1.1212 0.020 Uiso 1 1 calc R . . C9 C 0.3851(7) 0.0162(7) 1.0872(5) 0.021(2) Uani 1 1 d . . . H9A H 0.3910 0.0203 1.1521 0.025 Uiso 1 1 calc R . . H9B H 0.4565 0.0191 1.0670 0.025 Uiso 1 1 calc R . . C10 C 0.3317(7) -0.1028(6) 1.0571(5) 0.0187(18) Uani 1 1 d U . . H10A H 0.3716 -0.1763 1.0810 0.022 Uiso 1 1 calc R . . H10B H 0.2603 -0.1063 1.0774 0.022 Uiso 1 1 calc R . . C11 C 0.3034(7) -0.2254(6) 0.9280(5) 0.0164(17) Uani 1 1 d U . . H11A H 0.2345 -0.2541 0.9454 0.020 Uiso 1 1 calc R . . H11B H 0.3574 -0.2862 0.9505 0.020 Uiso 1 1 calc R . . C12 C 0.3015(7) -0.2156(6) 0.8287(5) 0.0157(16) Uani 1 1 d U . . H12A H 0.3701 -0.1863 0.8112 0.019 Uiso 1 1 calc R . . H12B H 0.2859 -0.2983 0.8012 0.019 Uiso 1 1 calc R . . B1 B -0.0324(8) 0.1739(8) 0.9745(6) 0.015(2) Uani 1 1 d . . . B2 B 0.4922(8) 0.4455(7) 0.8430(6) 0.016(2) Uani 1 1 d . . . F1 F -0.0757(4) 0.2937(4) 0.9786(3) 0.0258(12) Uani 1 1 d . . . F2 F -0.0398(4) 0.1285(4) 0.8898(3) 0.0286(13) Uani 1 1 d . . . F3 F 0.0741(4) 0.1819(4) 1.0058(3) 0.0218(11) Uani 1 1 d . . . F4 F -0.0836(4) 0.0944(4) 1.0309(3) 0.0225(11) Uani 1 1 d . . . F5 F 0.5722(4) 0.4992(4) 0.7972(3) 0.0299(12) Uani 1 1 d . . . F6 F 0.5370(4) 0.3837(4) 0.9151(3) 0.0295(13) Uani 1 1 d . . . F7 F 0.4256(4) 0.5364(4) 0.8637(3) 0.0353(14) Uani 1 1 d . . . F8 F 0.4401(4) 0.3571(4) 0.7863(3) 0.0237(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01009(15) 0.01417(14) 0.01424(14) -0.00065(15) 0.00353(10) -0.00050(15) O1 0.011(3) 0.021(3) 0.019(2) -0.001(2) -0.003(2) 0.003(2) O2 0.021(3) 0.015(3) 0.020(3) 0.002(2) 0.003(2) 0.005(3) O3 0.018(4) 0.021(3) 0.017(3) 0.002(2) 0.005(2) -0.004(3) O4 0.012(3) 0.018(3) 0.018(3) -0.002(2) 0.001(2) 0.003(2) O5 0.013(3) 0.013(3) 0.023(3) 0.001(2) 0.000(2) 0.000(2) O6 0.021(3) 0.012(2) 0.018(2) -0.003(2) 0.003(2) -0.001(2) O7 0.022(4) 0.012(3) 0.027(3) -0.004(2) 0.006(3) 0.004(3) C1 0.022(5) 0.021(4) 0.016(2) -0.005(3) 0.004(3) 0.005(3) C2 0.020(5) 0.015(4) 0.021(4) -0.006(4) -0.002(4) -0.004(4) C3 0.024(6) 0.025(4) 0.016(4) 0.010(4) -0.001(4) 0.007(4) C4 0.019(5) 0.022(4) 0.021(5) 0.004(4) 0.001(4) 0.007(4) C5 0.012(4) 0.007(4) 0.031(5) 0.008(3) -0.004(3) -0.001(3) C6 0.020(5) 0.011(4) 0.030(5) -0.002(3) 0.001(4) 0.003(4) C7 0.019(5) 0.019(4) 0.013(4) -0.003(3) 0.001(3) -0.008(4) C8 0.014(5) 0.019(4) 0.017(4) 0.000(3) -0.002(3) -0.010(4) C9 0.024(6) 0.021(4) 0.016(4) 0.003(4) -0.009(4) -0.001(4) C10 0.031(5) 0.008(4) 0.017(2) 0.003(3) 0.001(3) 0.005(4) C11 0.023(5) 0.005(3) 0.022(2) 0.000(2) 0.002(3) 0.009(3) C12 0.021(5) 0.005(3) 0.021(2) -0.005(2) 0.004(3) 0.005(3) B1 0.012(6) 0.014(4) 0.019(5) 0.004(4) -0.001(4) 0.000(4) B2 0.014(5) 0.004(4) 0.029(5) -0.003(4) 0.002(4) 0.003(3) F1 0.028(3) 0.016(2) 0.035(3) 0.003(2) 0.010(2) 0.006(2) F2 0.028(3) 0.031(3) 0.026(3) 0.001(2) -0.003(2) -0.001(2) F3 0.010(3) 0.029(3) 0.027(3) -0.006(2) 0.003(2) 0.001(2) F4 0.020(3) 0.018(2) 0.032(3) 0.012(2) 0.013(2) 0.004(2) F5 0.023(3) 0.036(3) 0.032(3) 0.002(2) 0.011(2) -0.008(2) F6 0.037(4) 0.031(3) 0.019(3) 0.005(2) -0.008(2) -0.001(2) F7 0.025(4) 0.024(3) 0.057(4) -0.012(2) 0.000(3) 0.008(2) F8 0.028(3) 0.024(2) 0.020(2) -0.001(2) 0.004(2) -0.007(2) _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 O7 2.406(6) . ? Pb1 F3 2.677(5) . ? Pb1 O6 2.701(5) . ? Pb1 O5 2.710(5) . ? Pb1 O4 2.732(5) . ? Pb1 O1 2.744(5) . ? Pb1 O2 2.803(5) . ? Pb1 O3 2.894(5) . ? O1 C1 1.423(8) . ? O1 C12 1.429(8) . ? O2 C3 1.428(8) . ? O2 C2 1.429(8) . ? O3 C5 1.420(8) . ? O3 C4 1.442(8) . ? O4 C6 1.428(8) . ? O4 C7 1.444(8) . ? O5 C9 1.435(8) . ? O5 C8 1.436(8) . ? O6 C11 1.433(8) . ? O6 C10 1.434(8) . ? O7 H7X 0.85(2) . ? O7 H7Y 0.85(2) . ? C1 C2 1.473(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.478(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.487(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.522(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? B1 F2 1.379(10) . ? B1 F1 1.396(9) . ? B1 F4 1.409(10) . ? B1 F3 1.412(10) . ? B2 F7 1.347(10) . ? B2 F6 1.369(9) . ? B2 F5 1.409(11) . ? B2 F8 1.411(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 O7 Pb1 F3 141.73(15) . . ? O7 Pb1 O6 76.82(17) . . ? F3 Pb1 O6 114.66(14) . . ? O7 Pb1 O5 80.34(18) . . ? F3 Pb1 O5 75.47(15) . . ? O6 Pb1 O5 60.80(14) . . ? O7 Pb1 O4 71.98(17) . . ? F3 Pb1 O4 70.46(15) . . ? O6 Pb1 O4 117.15(15) . . ? O5 Pb1 O4 61.11(14) . . ? O7 Pb1 O1 82.84(17) . . ? F3 Pb1 O1 135.18(15) . . ? O6 Pb1 O1 60.13(14) . . ? O5 Pb1 O1 120.77(14) . . ? O4 Pb1 O1 154.22(17) . . ? O7 Pb1 O2 83.87(17) . . ? F3 Pb1 O2 116.73(14) . . ? O6 Pb1 O2 117.62(14) . . ? O5 Pb1 O2 164.04(17) . . ? O4 Pb1 O2 111.54(14) . . ? O1 Pb1 O2 58.93(14) . . ? O7 Pb1 O3 86.46(17) . . ? F3 Pb1 O3 79.80(15) . . ? O6 Pb1 O3 163.17(17) . . ? O5 Pb1 O3 118.59(14) . . ? O4 Pb1 O3 57.75(14) . . ? O1 Pb1 O3 116.44(14) . . ? O2 Pb1 O3 57.69(14) . . ? C1 O1 C12 112.0(5) . . ? C1 O1 Pb1 121.2(4) . . ? C12 O1 Pb1 118.4(4) . . ? C3 O2 C2 111.7(6) . . ? C3 O2 Pb1 116.2(4) . . ? C2 O2 Pb1 113.7(4) . . ? C5 O3 C4 111.5(6) . . ? C5 O3 Pb1 117.5(4) . . ? C4 O3 Pb1 117.7(4) . . ? C6 O4 C7 110.6(5) . . ? C6 O4 Pb1 118.7(4) . . ? C7 O4 Pb1 117.5(4) . . ? C9 O5 C8 111.3(6) . . ? C9 O5 Pb1 118.7(4) . . ? C8 O5 Pb1 115.4(4) . . ? C11 O6 C10 111.6(5) . . ? C11 O6 Pb1 117.2(4) . . ? C10 O6 Pb1 110.5(4) . . ? Pb1 O7 H7X 116(6) . . ? Pb1 O7 H7Y 111(6) . . ? H7X O7 H7Y 117(7) . . ? O1 C1 C2 108.5(6) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? O2 C2 C1 109.1(6) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C4 106.3(6) . . ? O2 C3 H3A 110.5 . . ? C4 C3 H3A 110.5 . . ? O2 C3 H3B 110.5 . . ? C4 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? O3 C4 C3 107.0(6) . . ? O3 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O3 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.6 . . ? O3 C5 C6 107.8(6) . . ? O3 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? O3 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O4 C6 C5 108.6(6) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O4 C7 C8 107.9(6) . . ? O4 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O4 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O5 C8 C7 109.5(6) . . ? O5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 108.5(6) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O6 C10 C9 106.9(6) . . ? O6 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? O6 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? O6 C11 C12 107.3(6) . . ? O6 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O6 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? O1 C12 C11 106.5(6) . . ? O1 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? O1 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? F2 B1 F1 111.5(6) . . ? F2 B1 F4 111.4(6) . . ? F1 B1 F4 108.4(7) . . ? F2 B1 F3 109.3(7) . . ? F1 B1 F3 107.8(7) . . ? F4 B1 F3 108.3(6) . . ? F7 B2 F6 112.9(8) . . ? F7 B2 F5 109.0(6) . . ? F6 B2 F5 108.8(7) . . ? F7 B2 F8 110.3(7) . . ? F6 B2 F8 108.7(6) . . ? F5 B2 F8 107.0(7) . . ? B1 F3 Pb1 114.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 O1 C1 C2 176.6(6) . . . . ? Pb1 O1 C1 C2 -35.6(8) . . . . ? C3 O2 C2 C1 171.4(6) . . . . ? Pb1 O2 C2 C1 -54.7(8) . . . . ? O1 C1 C2 O2 58.3(9) . . . . ? C2 O2 C3 C4 -167.1(7) . . . . ? Pb1 O2 C3 C4 60.2(7) . . . . ? C5 O3 C4 C3 -179.7(6) . . . . ? Pb1 O3 C4 C3 40.2(8) . . . . ? O2 C3 C4 O3 -63.9(8) . . . . ? C4 O3 C5 C6 -179.3(6) . . . . ? Pb1 O3 C5 C6 -39.1(8) . . . . ? C7 O4 C6 C5 164.6(6) . . . . ? Pb1 O4 C6 C5 -55.3(8) . . . . ? O3 C5 C6 O4 59.6(8) . . . . ? C6 O4 C7 C8 -177.8(7) . . . . ? Pb1 O4 C7 C8 41.5(8) . . . . ? C9 O5 C8 C7 -170.0(6) . . . . ? Pb1 O5 C8 C7 50.9(7) . . . . ? O4 C7 C8 O5 -59.9(8) . . . . ? C8 O5 C9 C10 -166.3(7) . . . . ? Pb1 O5 C9 C10 -28.8(8) . . . . ? C11 O6 C10 C9 164.4(6) . . . . ? Pb1 O6 C10 C9 -63.3(7) . . . . ? O5 C9 C10 O6 60.2(9) . . . . ? C10 O6 C11 C12 -179.3(6) . . . . ? Pb1 O6 C11 C12 51.8(7) . . . . ? C1 O1 C12 C11 -167.6(6) . . . . ? Pb1 O1 C12 C11 43.6(7) . . . . ? O6 C11 C12 O1 -60.4(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7X F8 0.85(2) 1.93(4) 2.722(7) 154(7) . O7 H7Y F5 0.85(2) 1.85(3) 2.689(7) 170(8) 2_646 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pb1 F2 3.201(5) . . ? Pb1 F3 2.677(5) . . ? Pb1 F4 2.813(4) . 3_557 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.230 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.258 data_11paf053 _database_code_depnum_ccdc_archive 'CCDC 900329' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-16 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(aqua)-1,4,10,13-tetraoxo-7,16-dithia-cyclooctadecane- (tetrafluoroborate-F,F')-lead(II) tetrafluoroborate ; # C12H24O4S2 = [18]aneO4S2 # 1,4,10,13-tetraoxo-7,16-dithia-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-dithiacyclooctadecane (iLab defaults) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 B F4 O6 Pb S2 1+, B F4 1-' _chemical_formula_sum 'C12 H28 B2 F8 O6 Pb S2' _chemical_formula_structural '((C12 H24 O4 S2) (H2O)2 (B F4) Pb) (B F4)' _chemical_formula_weight 713.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.5374(15) _cell_length_b 15.5893(15) _cell_length_c 17.703(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4564.1(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8709 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 7.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.609 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11444 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5184 _reflns_number_gt 4191 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+4.8987P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (C-H) difmap (O-H)' _refine_ls_hydrogen_treatment 'constr (C-H) refxyz (O-H)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5184 _refine_ls_number_parameters 293 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.103413(6) 0.748834(6) 0.411439(5) 0.01244(4) Uani 1 1 d . . . S1 S 0.06605(4) 0.88490(4) 0.29554(4) 0.01658(14) Uani 1 1 d . . . S2 S 0.21546(4) 0.60717(4) 0.46209(4) 0.01638(14) Uani 1 1 d . . . O1 O -0.02142(11) 0.70576(12) 0.30386(12) 0.0195(4) Uani 1 1 d . . . O2 O 0.03644(12) 0.58105(12) 0.40609(11) 0.0174(4) Uani 1 1 d . . . O3 O 0.18440(11) 0.78062(12) 0.54258(11) 0.0169(4) Uani 1 1 d . . . O4 O 0.08996(11) 0.90950(11) 0.47160(11) 0.0159(4) Uani 1 1 d . . . O5 O 0.15638(13) 0.68578(14) 0.28746(12) 0.0239(5) Uani 1 1 d D . . H5X H 0.119(2) 0.668(3) 0.260(2) 0.064(7) Uiso 1 1 d D . . H5Y H 0.191(2) 0.649(2) 0.297(3) 0.064(7) Uiso 1 1 d D . . O6 O 0.23281(12) 0.82144(16) 0.38356(13) 0.0268(5) Uani 1 1 d D . . H6X H 0.242(3) 0.841(3) 0.3406(14) 0.064(7) Uiso 1 1 d D . . H6Y H 0.2748(17) 0.812(3) 0.408(2) 0.064(7) Uiso 1 1 d D . . C1 C -0.01971(17) 0.84336(18) 0.24319(17) 0.0201(6) Uani 1 1 d . . . H1A H -0.0549 0.8922 0.2291 0.024 Uiso 1 1 calc R . . H1B H 0.0006 0.8174 0.1958 0.024 Uiso 1 1 calc R . . C2 C -0.07067(17) 0.77763(19) 0.28358(18) 0.0210(6) Uani 1 1 d . . . H2A H -0.0946 0.8033 0.3296 0.025 Uiso 1 1 calc R . . H2B H -0.1153 0.7586 0.2503 0.025 Uiso 1 1 calc R . . C3 C -0.06989(18) 0.63483(18) 0.32831(18) 0.0216(6) Uani 1 1 d . . . H3A H -0.1093 0.6193 0.2885 0.026 Uiso 1 1 calc R . . H3B H -0.1003 0.6506 0.3745 0.026 Uiso 1 1 calc R . . C4 C -0.01539(18) 0.56035(18) 0.34434(16) 0.0187(6) Uani 1 1 d . . . H4A H -0.0481 0.5091 0.3569 0.022 Uiso 1 1 calc R . . H4B H 0.0174 0.5470 0.2991 0.022 Uiso 1 1 calc R . . C5 C 0.08307(18) 0.50841(18) 0.42997(18) 0.0196(6) Uani 1 1 d . . . H5A H 0.1170 0.4875 0.3878 0.023 Uiso 1 1 calc R . . H5B H 0.0467 0.4613 0.4459 0.023 Uiso 1 1 calc R . . C6 C 0.13580(17) 0.53587(18) 0.49520(17) 0.0179(6) Uani 1 1 d . . . H6A H 0.1602 0.4847 0.5193 0.022 Uiso 1 1 calc R . . H6B H 0.1025 0.5658 0.5335 0.022 Uiso 1 1 calc R . . C7 C 0.25593(17) 0.64829(18) 0.55010(17) 0.0189(6) Uani 1 1 d . . . H7A H 0.2679 0.5992 0.5837 0.023 Uiso 1 1 calc R . . H7B H 0.3077 0.6777 0.5393 0.023 Uiso 1 1 calc R . . C8 C 0.20097(17) 0.71014(19) 0.59196(16) 0.0178(6) Uani 1 1 d . . . H8A H 0.1500 0.6811 0.6063 0.021 Uiso 1 1 calc R . . H8B H 0.2278 0.7308 0.6385 0.021 Uiso 1 1 calc R . . C9 C 0.15209(19) 0.85275(18) 0.58265(16) 0.0191(6) Uani 1 1 d . . . H9A H 0.1872 0.8669 0.6262 0.023 Uiso 1 1 calc R . . H9B H 0.0974 0.8390 0.6020 0.023 Uiso 1 1 calc R . . C10 C 0.14787(17) 0.92737(18) 0.52964(17) 0.0182(6) Uani 1 1 d . . . H10A H 0.1318 0.9797 0.5576 0.022 Uiso 1 1 calc R . . H10B H 0.2017 0.9376 0.5068 0.022 Uiso 1 1 calc R . . C11 C 0.07801(18) 0.98233(18) 0.42305(17) 0.0195(6) Uani 1 1 d . . . H11A H 0.1300 0.9995 0.3998 0.023 Uiso 1 1 calc R . . H11B H 0.0570 1.0314 0.4526 0.023 Uiso 1 1 calc R . . C12 C 0.01809(17) 0.95767(18) 0.36229(17) 0.0196(6) Uani 1 1 d . . . H12A H -0.0008 1.0097 0.3356 0.024 Uiso 1 1 calc R . . H12B H -0.0294 0.9294 0.3855 0.024 Uiso 1 1 calc R . . B1 B -0.0606(2) 0.7432(2) 0.5409(2) 0.0212(7) Uani 1 1 d . . . F1 F 0.01194(9) 0.69949(10) 0.55379(10) 0.0227(4) Uani 1 1 d . . . F2 F -0.05498(9) 0.78448(12) 0.47092(10) 0.0266(4) Uani 1 1 d . . . F3 F -0.12438(10) 0.68385(12) 0.53769(12) 0.0311(5) Uani 1 1 d . . . F4 F -0.07432(13) 0.80197(12) 0.59751(12) 0.0399(5) Uani 1 1 d . . . B2 B 0.7720(2) 0.9859(2) 0.2698(2) 0.0205(7) Uani 1 1 d . . . F5 F 0.72343(11) 1.00317(11) 0.33082(10) 0.0265(4) Uani 1 1 d . . . F6 F 0.77090(11) 0.89853(11) 0.25305(11) 0.0299(4) Uani 1 1 d . . . F7 F 0.74553(12) 1.03349(14) 0.20825(11) 0.0386(5) Uani 1 1 d . . . F8 F 0.85162(10) 1.01019(12) 0.28524(12) 0.0328(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01367(6) 0.01251(6) 0.01114(6) 0.00170(4) 0.00074(4) 0.00026(4) S1 0.0169(3) 0.0177(3) 0.0151(3) 0.0035(3) -0.0019(3) -0.0007(3) S2 0.0169(3) 0.0172(3) 0.0150(3) 0.0029(3) 0.0008(3) 0.0016(3) O1 0.0167(9) 0.0149(10) 0.0268(12) 0.0053(9) -0.0049(9) -0.0026(8) O2 0.0215(10) 0.0127(9) 0.0179(11) -0.0004(8) -0.0053(8) 0.0002(8) O3 0.0229(10) 0.0138(9) 0.0139(10) 0.0001(8) -0.0024(8) 0.0018(8) O4 0.0208(9) 0.0117(9) 0.0152(10) 0.0004(8) -0.0039(8) -0.0025(8) O5 0.0282(12) 0.0258(11) 0.0176(12) -0.0024(9) 0.0034(10) 0.0004(10) O6 0.0181(10) 0.0428(14) 0.0195(12) 0.0152(11) -0.0029(9) -0.0080(10) C1 0.0231(14) 0.0204(14) 0.0168(15) 0.0034(12) -0.0071(12) 0.0016(12) C2 0.0176(14) 0.0218(14) 0.0237(17) 0.0050(12) -0.0057(12) 0.0018(12) C3 0.0195(14) 0.0203(15) 0.0251(16) 0.0050(12) -0.0059(13) -0.0079(12) C4 0.0231(14) 0.0162(14) 0.0168(15) -0.0005(11) -0.0036(12) -0.0071(12) C5 0.0230(14) 0.0112(13) 0.0245(16) 0.0019(12) -0.0022(13) 0.0011(12) C6 0.0193(13) 0.0142(13) 0.0203(16) 0.0039(11) -0.0008(12) 0.0013(11) C7 0.0179(13) 0.0198(14) 0.0189(15) 0.0056(12) -0.0035(12) 0.0004(12) C8 0.0204(14) 0.0197(15) 0.0133(14) 0.0043(11) -0.0033(11) -0.0012(12) C9 0.0281(15) 0.0161(14) 0.0131(14) -0.0021(11) -0.0034(12) -0.0008(12) C10 0.0227(15) 0.0156(13) 0.0163(15) -0.0018(12) -0.0060(12) -0.0014(11) C11 0.0259(15) 0.0142(14) 0.0185(15) 0.0035(11) -0.0019(12) 0.0015(12) C12 0.0229(14) 0.0163(14) 0.0197(15) 0.0019(12) -0.0026(12) 0.0049(12) B1 0.0186(15) 0.0211(17) 0.0238(18) 0.0072(14) 0.0054(14) 0.0033(14) F1 0.0195(8) 0.0246(9) 0.0239(10) 0.0034(8) -0.0028(7) 0.0041(7) F2 0.0180(8) 0.0343(10) 0.0275(10) 0.0154(8) 0.0021(8) 0.0016(8) F3 0.0170(8) 0.0297(10) 0.0467(13) 0.0135(9) 0.0075(8) -0.0019(8) F4 0.0557(13) 0.0291(11) 0.0350(12) -0.0040(9) 0.0145(10) 0.0138(10) B2 0.0241(16) 0.0204(16) 0.0170(17) 0.0018(13) -0.0053(14) -0.0003(14) F5 0.0293(9) 0.0268(10) 0.0232(10) 0.0000(8) 0.0032(8) 0.0058(8) F6 0.0367(10) 0.0251(9) 0.0278(10) -0.0094(8) -0.0019(8) -0.0023(8) F7 0.0412(11) 0.0479(12) 0.0265(11) 0.0177(10) -0.0076(9) -0.0046(9) F8 0.0184(9) 0.0349(10) 0.0451(13) -0.0153(9) -0.0048(8) -0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O6 2.471(2) . ? Pb1 O5 2.559(2) . ? Pb1 O3 2.726(2) . ? Pb1 O4 2.7307(18) . ? Pb1 O2 2.8421(19) . ? Pb1 F2 2.8773(17) . ? Pb1 O1 2.888(2) . ? Pb1 S1 3.0151(8) . ? Pb1 S2 3.0191(7) . ? Pb1 F1 3.0382(19) . ? S1 C1 1.814(3) . ? S1 C12 1.820(3) . ? S2 C7 1.813(3) . ? S2 C6 1.821(3) . ? O1 C2 1.431(3) . ? O1 C3 1.433(3) . ? O2 C4 1.426(3) . ? O2 C5 1.434(3) . ? O3 C8 1.431(3) . ? O3 C9 1.433(3) . ? O4 C10 1.432(3) . ? O4 C11 1.438(3) . ? O5 H5X 0.832(19) . ? O5 H5Y 0.829(19) . ? O6 H6X 0.833(19) . ? O6 H6Y 0.831(19) . ? C1 C2 1.507(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.497(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.518(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.512(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? B1 F4 1.377(4) . ? B1 F2 1.398(4) . ? B1 F1 1.399(4) . ? B1 F3 1.404(4) . ? B2 F5 1.373(4) . ? B2 F7 1.389(4) . ? B2 F6 1.394(4) . ? B2 F8 1.398(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Pb1 O5 73.03(8) . . ? O6 Pb1 O3 70.20(7) . . ? O5 Pb1 O3 129.20(7) . . ? O6 Pb1 O4 74.23(7) . . ? O5 Pb1 O4 135.61(6) . . ? O3 Pb1 O4 62.68(6) . . ? O6 Pb1 O2 138.81(7) . . ? O5 Pb1 O2 75.60(6) . . ? O3 Pb1 O2 112.78(6) . . ? O4 Pb1 O2 145.63(6) . . ? O6 Pb1 F2 140.64(7) . . ? O5 Pb1 F2 134.39(6) . . ? O3 Pb1 F2 95.77(6) . . ? O4 Pb1 F2 66.79(5) . . ? O2 Pb1 F2 80.51(5) . . ? O6 Pb1 O1 126.43(7) . . ? O5 Pb1 O1 65.78(6) . . ? O3 Pb1 O1 162.80(6) . . ? O4 Pb1 O1 114.35(5) . . ? O2 Pb1 O1 59.03(5) . . ? F2 Pb1 O1 68.62(6) . . ? O6 Pb1 S1 73.69(5) . . ? O5 Pb1 S1 75.92(6) . . ? O3 Pb1 S1 123.53(4) . . ? O4 Pb1 S1 66.64(5) . . ? O2 Pb1 S1 123.02(4) . . ? F2 Pb1 S1 85.79(4) . . ? O1 Pb1 S1 64.42(4) . . ? O6 Pb1 S2 82.12(5) . . ? O5 Pb1 S2 76.33(5) . . ? O3 Pb1 S2 65.07(4) . . ? O4 Pb1 S2 127.23(4) . . ? O2 Pb1 S2 64.91(4) . . ? F2 Pb1 S2 126.25(4) . . ? O1 Pb1 S2 117.68(4) . . ? S1 Pb1 S2 147.403(19) . . ? O6 Pb1 F1 135.48(6) . . ? O5 Pb1 F1 141.67(6) . . ? O3 Pb1 F1 65.43(6) . . ? O4 Pb1 F1 82.43(5) . . ? O2 Pb1 F1 66.46(5) . . ? F2 Pb1 F1 44.94(4) . . ? O1 Pb1 F1 97.60(5) . . ? S1 Pb1 F1 129.83(3) . . ? S2 Pb1 F1 82.76(3) . . ? C1 S1 C12 102.33(14) . . ? C1 S1 Pb1 104.88(9) . . ? C12 S1 Pb1 94.93(10) . . ? C7 S2 C6 101.90(13) . . ? C7 S2 Pb1 102.90(9) . . ? C6 S2 Pb1 95.63(9) . . ? C2 O1 C3 111.2(2) . . ? C2 O1 Pb1 112.97(16) . . ? C3 O1 Pb1 112.34(16) . . ? C4 O2 C5 111.7(2) . . ? C4 O2 Pb1 117.91(15) . . ? C5 O2 Pb1 120.50(15) . . ? C8 O3 C9 111.8(2) . . ? C8 O3 Pb1 118.36(16) . . ? C9 O3 Pb1 112.40(15) . . ? C10 O4 C11 111.5(2) . . ? C10 O4 Pb1 113.82(15) . . ? C11 O4 Pb1 120.16(16) . . ? Pb1 O5 H5X 112(3) . . ? Pb1 O5 H5Y 109(3) . . ? H5X O5 H5Y 114(4) . . ? Pb1 O6 H6X 120(3) . . ? Pb1 O6 H6Y 122(3) . . ? H6X O6 H6Y 113(4) . . ? C2 C1 S1 115.9(2) . . ? C2 C1 H1A 108.3 . . ? S1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? S1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? O1 C2 C1 109.5(2) . . ? O1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O1 C3 C4 108.6(2) . . ? O1 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O1 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 109.4(2) . . ? O2 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O2 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? O2 C5 C6 108.2(2) . . ? O2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? C5 C6 S2 110.2(2) . . ? C5 C6 H6A 109.6 . . ? S2 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? S2 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 S2 115.03(19) . . ? C8 C7 H7A 108.5 . . ? S2 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? S2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O3 C8 C7 107.7(2) . . ? O3 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O3 C9 C10 108.5(2) . . ? O3 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O4 C10 C9 109.3(2) . . ? O4 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? O4 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? O4 C11 C12 108.3(2) . . ? O4 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O4 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C11 C12 S1 109.6(2) . . ? C11 C12 H12A 109.8 . . ? S1 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? S1 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? F4 B1 F2 110.5(3) . . ? F4 B1 F1 110.2(3) . . ? F2 B1 F1 108.1(2) . . ? F4 B1 F3 110.1(3) . . ? F2 B1 F3 108.5(3) . . ? F1 B1 F3 109.2(2) . . ? B1 F1 Pb1 99.68(17) . . ? B1 F2 Pb1 107.23(16) . . ? F5 B2 F7 109.2(3) . . ? F5 B2 F6 110.6(3) . . ? F7 B2 F6 110.6(3) . . ? F5 B2 F8 110.1(3) . . ? F7 B2 F8 107.8(3) . . ? F6 B2 F8 108.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 S1 C1 C2 -75.4(2) . . . . ? Pb1 S1 C1 C2 23.2(2) . . . . ? C3 O1 C2 C1 -168.2(2) . . . . ? Pb1 O1 C2 C1 64.4(3) . . . . ? S1 C1 C2 O1 -58.8(3) . . . . ? C2 O1 C3 C4 176.8(2) . . . . ? Pb1 O1 C3 C4 -55.5(3) . . . . ? C5 O2 C4 C3 172.8(2) . . . . ? Pb1 O2 C4 C3 -41.1(3) . . . . ? O1 C3 C4 O2 64.5(3) . . . . ? C4 O2 C5 C6 -179.9(2) . . . . ? Pb1 O2 C5 C6 35.0(3) . . . . ? O2 C5 C6 S2 -70.6(3) . . . . ? C7 S2 C6 C5 168.6(2) . . . . ? Pb1 S2 C6 C5 64.08(19) . . . . ? C6 S2 C7 C8 -70.9(2) . . . . ? Pb1 S2 C7 C8 27.8(2) . . . . ? C9 O3 C8 C7 -164.0(2) . . . . ? Pb1 O3 C8 C7 62.9(2) . . . . ? S2 C7 C8 O3 -58.3(3) . . . . ? C8 O3 C9 C10 171.8(2) . . . . ? Pb1 O3 C9 C10 -52.3(2) . . . . ? C11 O4 C10 C9 174.6(2) . . . . ? Pb1 O4 C10 C9 -45.5(3) . . . . ? O3 C9 C10 O4 66.1(3) . . . . ? C10 O4 C11 C12 178.5(2) . . . . ? Pb1 O4 C11 C12 41.4(3) . . . . ? O4 C11 C12 S1 -72.5(3) . . . . ? C1 S1 C12 C11 166.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5X O1 0.832(19) 2.52(4) 2.971(3) 115(4) . O5 H5X F8 0.832(19) 2.64(4) 3.028(3) 110(3) 3_645 O5 H5Y F7 0.829(19) 2.08(2) 2.876(3) 160(4) 3_645 O5 H5Y S2 0.829(19) 3.02(4) 3.466(3) 116(4) . O6 H6X F6 0.833(19) 1.94(2) 2.773(3) 173(4) 6_556 O6 H6Y F3 0.831(19) 1.93(2) 2.744(3) 167(4) 4_566 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.612 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.103 data_11paf052 _database_code_depnum_ccdc_archive 'CCDC 900330' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-25 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(1,4,7-trioxa-10,13-dithiacyclopentadecane)lead(II) tetrafluoroborate dichloromethane solvate ; # C10H20O3S2 = [15]aneO3S2 # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab defaults) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (iLab selected options) # 1,4,7-trioxa-10,13-dithiacyclopentadecane (Chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 O6 Pb S4 2+, 2(B F4 1-), 1.22(C H2 Cl2)' _chemical_formula_sum 'C21.22 H42.44 B2 Cl2.44 F8 O6 Pb S4' _chemical_formula_weight 989.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 18.747(3) _cell_length_b 28.254(10) _cell_length_c 13.263(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7025(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13464 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3898 _exptl_absorpt_coefficient_mu 5.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17991 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7968 _reflns_number_gt 5920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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. The dichloromethane solvate was badly disordered. Only the C21 atom associated with Cl1 was identified and no H atoms were included in the model. All the Cl atoms and C21 were retained as isotropic. One BF~4~ was disordered (B2 centred). This was modelled using two orientations (A & B) and controlled using Shelxl DFIX commands ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+57.5977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7968 _refine_ls_number_parameters 394 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.555783(12) 0.889537(8) 0.238682(16) 0.01628(7) Uani 1 1 d . . . S1 S 0.39920(8) 0.88869(6) 0.18469(13) 0.0244(3) Uani 1 1 d . . . S2 S 0.49431(9) 0.98763(6) 0.20088(13) 0.0213(3) Uani 1 1 d . . . S3 S 0.49559(9) 0.80993(6) 0.37722(13) 0.0238(4) Uani 1 1 d . . . S4 S 0.52309(9) 0.92066(6) 0.45429(12) 0.0226(3) Uani 1 1 d . . . O1 O 0.5347(2) 0.90128(17) 0.0398(3) 0.0246(11) Uani 1 1 d . . . O2 O 0.6714(2) 0.91760(16) 0.1294(3) 0.0247(10) Uani 1 1 d . . . O3 O 0.6364(2) 0.97254(16) 0.2978(4) 0.0224(10) Uani 1 1 d . . . O4 O 0.5063(3) 0.79482(17) 0.1524(4) 0.0284(11) Uani 1 1 d . . . O5 O 0.6509(2) 0.82146(16) 0.1737(4) 0.0264(11) Uani 1 1 d . . . O6 O 0.6602(2) 0.86229(16) 0.3723(3) 0.0225(10) Uani 1 1 d . . . C1 C 0.4118(4) 0.8789(3) 0.0496(6) 0.0324(17) Uani 1 1 d . . . H1A H 0.4267 0.8456 0.0394 0.039 Uiso 1 1 calc R . . H1B H 0.3652 0.8830 0.0156 0.039 Uiso 1 1 calc R . . C2 C 0.4652(4) 0.9104(3) -0.0010(6) 0.0331(18) Uani 1 1 d . . . H2A H 0.4652 0.9043 -0.0745 0.040 Uiso 1 1 calc R . . H2B H 0.4522 0.9440 0.0102 0.040 Uiso 1 1 calc R . . C3 C 0.5883(4) 0.9301(3) -0.0083(5) 0.0276(16) Uani 1 1 d . . . H3A H 0.5825 0.9636 0.0120 0.033 Uiso 1 1 calc R . . H3B H 0.5834 0.9281 -0.0825 0.033 Uiso 1 1 calc R . . C4 C 0.6601(4) 0.9125(3) 0.0232(5) 0.0275(16) Uani 1 1 d . . . H4A H 0.6645 0.8786 0.0047 0.033 Uiso 1 1 calc R . . H4B H 0.6974 0.9302 -0.0136 0.033 Uiso 1 1 calc R . . C5 C 0.7138(4) 0.9578(2) 0.1554(6) 0.0266(16) Uani 1 1 d . . . H5A H 0.6958 0.9864 0.1208 0.032 Uiso 1 1 calc R . . H5B H 0.7640 0.9526 0.1352 0.032 Uiso 1 1 calc R . . C6 C 0.7086(3) 0.9637(2) 0.2676(6) 0.0280(16) Uani 1 1 d . . . H6A H 0.7262 0.9347 0.3012 0.034 Uiso 1 1 calc R . . H6B H 0.7391 0.9904 0.2891 0.034 Uiso 1 1 calc R . . C7 C 0.6163(4) 1.0208(2) 0.2824(5) 0.0261(15) Uani 1 1 d . . . H7A H 0.6302 1.0312 0.2139 0.031 Uiso 1 1 calc R . . H7B H 0.6405 1.0414 0.3321 0.031 Uiso 1 1 calc R . . C8 C 0.5360(4) 1.0242(2) 0.2951(5) 0.0265(16) Uani 1 1 d . . . H8A H 0.5204 1.0575 0.2870 0.032 Uiso 1 1 calc R . . H8B H 0.5221 1.0134 0.3633 0.032 Uiso 1 1 calc R . . C9 C 0.4050(4) 0.9827(2) 0.2502(6) 0.0280(16) Uani 1 1 d . . . H9A H 0.4070 0.9720 0.3211 0.034 Uiso 1 1 calc R . . H9B H 0.3817 1.0141 0.2487 0.034 Uiso 1 1 calc R . . C10 C 0.3617(4) 0.9479(3) 0.1884(6) 0.0290(16) Uani 1 1 d . . . H10A H 0.3577 0.9600 0.1186 0.035 Uiso 1 1 calc R . . H10B H 0.3129 0.9462 0.2168 0.035 Uiso 1 1 calc R . . C11 C 0.4374(4) 0.7753(2) 0.2970(6) 0.0273(15) Uani 1 1 d . . . H11A H 0.4164 0.7489 0.3360 0.033 Uiso 1 1 calc R . . H11B H 0.3979 0.7954 0.2717 0.033 Uiso 1 1 calc R . . C12 C 0.4793(4) 0.7564(3) 0.2106(6) 0.0363(18) Uani 1 1 d . . . H12A H 0.5193 0.7369 0.2360 0.044 Uiso 1 1 calc R . . H12B H 0.4485 0.7361 0.1681 0.044 Uiso 1 1 calc R . . C13 C 0.5610(4) 0.7810(3) 0.0842(6) 0.0339(18) Uani 1 1 d . . . H13A H 0.5649 0.8048 0.0297 0.041 Uiso 1 1 calc R . . H13B H 0.5482 0.7503 0.0531 0.041 Uiso 1 1 calc R . . C14 C 0.6316(4) 0.7764(3) 0.1363(7) 0.0370(19) Uani 1 1 d . . . H14A H 0.6279 0.7535 0.1925 0.044 Uiso 1 1 calc R . . H14B H 0.6681 0.7649 0.0884 0.044 Uiso 1 1 calc R . . C15 C 0.7135(3) 0.8215(2) 0.2347(6) 0.0282(16) Uani 1 1 d . . . H15A H 0.7413 0.8506 0.2208 0.034 Uiso 1 1 calc R . . H15B H 0.7435 0.7940 0.2168 0.034 Uiso 1 1 calc R . . C16 C 0.6956(4) 0.8195(3) 0.3455(6) 0.0291(16) Uani 1 1 d . . . H16A H 0.6643 0.7920 0.3593 0.035 Uiso 1 1 calc R . . H16B H 0.7397 0.8159 0.3857 0.035 Uiso 1 1 calc R . . C17 C 0.6466(4) 0.8648(3) 0.4784(5) 0.0265(16) Uani 1 1 d . . . H17A H 0.6920 0.8614 0.5159 0.032 Uiso 1 1 calc R . . H17B H 0.6147 0.8385 0.4985 0.032 Uiso 1 1 calc R . . C18 C 0.6124(4) 0.9111(3) 0.5044(5) 0.0253(15) Uani 1 1 d . . . H18A H 0.6437 0.9368 0.4797 0.030 Uiso 1 1 calc R . . H18B H 0.6102 0.9137 0.5788 0.030 Uiso 1 1 calc R . . C19 C 0.4706(4) 0.8768(3) 0.5222(5) 0.0269(16) Uani 1 1 d . . . H19A H 0.5025 0.8586 0.5674 0.032 Uiso 1 1 calc R . . H19B H 0.4350 0.8933 0.5647 0.032 Uiso 1 1 calc R . . C20 C 0.4320(4) 0.8424(3) 0.4526(5) 0.0269(16) Uani 1 1 d . . . H20A H 0.3992 0.8601 0.4079 0.032 Uiso 1 1 calc R . . H20B H 0.4032 0.8200 0.4932 0.032 Uiso 1 1 calc R . . B1 B 0.6048(4) 0.8540(3) 0.7734(6) 0.0254(17) Uani 1 1 d . . . F1 F 0.5344(2) 0.86784(18) 0.7858(4) 0.0480(13) Uani 1 1 d . . . F2 F 0.6253(2) 0.82390(17) 0.8488(3) 0.0423(12) Uani 1 1 d . . . F3 F 0.6480(2) 0.89382(15) 0.7713(3) 0.0374(11) Uani 1 1 d . . . F4 F 0.6107(2) 0.83056(14) 0.6811(3) 0.0347(10) Uani 1 1 d . . . B2 B 0.2233(5) 0.9379(3) -0.0175(6) 0.041(2) Uani 1 1 d D . . F5 F 0.2223(3) 0.9034(2) 0.0542(4) 0.0640(17) Uani 1 1 d D A . F6A F 0.2938(4) 0.9377(3) -0.0570(6) 0.041(3) Uiso 0.560(11) 1 d PD A 1 F7A F 0.2145(6) 0.9836(3) 0.0214(8) 0.064(3) Uiso 0.560(11) 1 d PD A 1 F8A F 0.1767(5) 0.9278(4) -0.0899(8) 0.073(4) Uiso 0.560(11) 1 d PD A 1 F6B F 0.2505(7) 0.9328(5) -0.1118(9) 0.071(5) Uiso 0.440(11) 1 d PD A 2 F7B F 0.2504(8) 0.9762(5) 0.0346(10) 0.071(5) Uiso 0.440(11) 1 d PD A 2 F8B F 0.1494(6) 0.9500(5) -0.0312(11) 0.069(5) Uiso 0.440(11) 1 d PD A 2 C21 C 0.2839(5) 0.8481(4) 0.7527(8) 0.072(3) Uiso 1 1 d D . . Cl1 Cl 0.37680(11) 0.85210(8) 0.76222(17) 0.0442(4) Uiso 1 1 d D . . Cl2A Cl 0.2507(4) 0.8101(3) 0.8412(6) 0.0442(4) Uiso 0.31 1 d PD . . Cl2B Cl 0.2694(5) 0.7938(4) 0.6673(8) 0.0442(4) Uiso 0.21 1 d PD . . Cl2C Cl 0.2572(5) 0.7942(3) 0.8109(7) 0.0442(4) Uiso 0.25 1 d P . . Cl2D Cl 0.2617(5) 0.8162(4) 0.8814(8) 0.0442(4) Uiso 0.23 1 d P . . Cl3A Cl 0.3258(5) 0.7408(3) 0.5719(7) 0.0442(4) Uiso 0.26 1 d P . . Cl3B Cl 0.3204(7) 0.7288(5) 0.5288(10) 0.0442(4) Uiso 0.18 1 d P . . 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 0.01551(11) 0.01664(11) 0.01670(11) 0.00037(9) -0.00038(9) 0.00216(10) S1 0.0170(7) 0.0248(8) 0.0315(9) 0.0010(8) -0.0028(7) 0.0019(7) S2 0.0237(8) 0.0197(8) 0.0206(8) 0.0004(6) 0.0028(7) 0.0039(7) S3 0.0231(8) 0.0206(8) 0.0277(9) 0.0048(7) -0.0028(7) -0.0027(7) S4 0.0265(8) 0.0229(8) 0.0183(8) -0.0006(7) 0.0015(7) -0.0005(7) O1 0.025(2) 0.030(3) 0.019(2) 0.002(2) 0.000(2) 0.006(2) O2 0.028(2) 0.022(2) 0.024(2) 0.003(2) 0.000(2) -0.005(2) O3 0.019(2) 0.016(2) 0.032(3) 0.001(2) 0.003(2) -0.0024(18) O4 0.027(3) 0.025(3) 0.034(3) -0.005(2) -0.001(2) -0.002(2) O5 0.025(2) 0.016(2) 0.038(3) -0.007(2) -0.003(2) 0.004(2) O6 0.021(2) 0.023(2) 0.022(2) 0.007(2) -0.001(2) 0.005(2) C1 0.029(4) 0.038(5) 0.030(4) -0.004(3) -0.010(3) 0.001(3) C2 0.028(4) 0.048(5) 0.023(4) 0.002(3) -0.007(3) 0.009(4) C3 0.032(4) 0.030(4) 0.020(3) 0.005(3) 0.009(3) 0.007(3) C4 0.031(4) 0.029(4) 0.022(3) 0.004(3) 0.009(3) 0.002(3) C5 0.025(3) 0.020(3) 0.034(4) -0.003(3) 0.008(3) -0.012(3) C6 0.019(3) 0.021(3) 0.043(4) -0.005(3) 0.003(3) -0.005(3) C7 0.034(4) 0.016(3) 0.028(4) -0.002(3) -0.001(3) -0.005(3) C8 0.038(4) 0.017(3) 0.025(3) -0.002(3) 0.000(3) 0.004(3) C9 0.027(4) 0.021(3) 0.036(4) 0.006(3) 0.004(3) 0.015(3) C10 0.017(3) 0.035(4) 0.035(4) 0.009(3) 0.002(3) 0.008(3) C11 0.028(4) 0.017(3) 0.036(4) 0.000(3) 0.001(3) -0.004(3) C12 0.041(4) 0.024(4) 0.044(5) -0.010(3) -0.003(4) -0.006(4) C13 0.039(4) 0.027(4) 0.036(4) -0.019(3) 0.005(4) -0.003(4) C14 0.030(4) 0.025(4) 0.056(5) -0.019(4) 0.009(4) 0.002(3) C15 0.016(3) 0.022(3) 0.046(4) -0.002(3) 0.005(3) 0.005(3) C16 0.020(3) 0.029(4) 0.038(4) 0.010(3) 0.000(3) 0.006(3) C17 0.019(3) 0.036(4) 0.025(4) 0.010(3) -0.007(3) -0.004(3) C18 0.024(3) 0.034(4) 0.018(3) 0.005(3) -0.002(3) -0.005(3) C19 0.030(4) 0.029(4) 0.022(3) -0.002(3) 0.005(3) -0.002(3) C20 0.022(3) 0.031(4) 0.028(4) 0.000(3) 0.004(3) -0.002(3) B1 0.026(4) 0.022(4) 0.028(4) 0.001(3) -0.003(3) -0.003(3) F1 0.023(2) 0.046(3) 0.075(4) -0.013(3) 0.000(2) 0.005(2) F2 0.044(3) 0.054(3) 0.029(2) 0.015(2) -0.006(2) 0.003(2) F3 0.038(2) 0.027(2) 0.047(3) -0.015(2) 0.011(2) -0.0105(19) F4 0.058(3) 0.020(2) 0.026(2) -0.0050(17) 0.002(2) -0.007(2) B2 0.035(5) 0.055(7) 0.032(5) 0.007(5) 0.003(4) -0.004(5) F5 0.054(3) 0.071(4) 0.067(4) 0.039(3) 0.005(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.688(5) . ? Pb1 O2 2.725(5) . ? Pb1 O6 2.750(4) . ? Pb1 S1 3.0216(16) . ? Pb1 S2 3.0430(18) . ? Pb1 S4 3.0540(17) . ? Pb1 S3 3.1158(18) . ? S1 C10 1.816(7) . ? S1 C1 1.828(8) . ? S2 C8 1.800(7) . ? S2 C9 1.802(7) . ? S3 C20 1.806(7) . ? S3 C11 1.811(7) . ? S4 C19 1.821(7) . ? S4 C18 1.822(7) . ? O1 C2 1.434(8) . ? O1 C3 1.442(8) . ? O2 C5 1.429(8) . ? O2 C4 1.431(8) . ? O3 C7 1.429(8) . ? O3 C6 1.433(8) . ? O4 C13 1.422(9) . ? O4 C12 1.425(9) . ? O5 C14 1.413(8) . ? O5 C15 1.425(8) . ? O6 C16 1.425(8) . ? O6 C17 1.432(8) . ? C1 C2 1.498(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.494(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.518(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.516(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.489(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.498(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.509(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.497(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.523(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? B1 F2 1.367(9) . ? B1 F1 1.386(9) . ? B1 F3 1.388(9) . ? B1 F4 1.396(9) . ? B2 F8A 1.329(11) . ? B2 F6B 1.358(12) . ? B2 F5 1.362(9) . ? B2 F7B 1.380(12) . ? B2 F7A 1.398(11) . ? B2 F6A 1.422(10) . ? B2 F8B 1.438(12) . ? C21 Cl2A 1.708(12) . ? C21 Cl1 1.750(10) . ? C21 Cl2C 1.779(14) . ? C21 Cl2B 1.925(13) . ? C21 Cl2D 1.974(15) . ? Cl2A Cl2D 0.597(10) . ? Cl2A Cl2C 0.616(10) . ? Cl2A Cl2B 2.379(13) . ? Cl2B Cl2C 1.919(14) . ? Cl2B Cl3A 2.230(13) . ? Cl2B Cl3A 2.396(13) 2_565 ? Cl2C Cl2D 1.127(13) . ? Cl3A Cl3B 0.671(13) . ? Cl3A Cl2B 2.396(13) 2_565 ? 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 # F8A B2 F6B 63.8(8) . . ? # F8A B2 F7B 140.6(11) . . ? # F6B B2 F7A 118.8(10) . . ? # F7B B2 F7A 30.3(7) . . ? # F6B B2 F6A 46.4(7) . . ? # F7B B2 F6A 81.2(8) . . ? # F8A B2 F8B 47.7(7) . . ? # F7A B2 F8B 73.4(8) . . ? # F6A B2 F8B 148.2(9) . . ? # Cl2A C21 Cl2C 20.2(3) . . ? # Cl2A C21 Cl2D 16.7(4) . . ? # Cl2C C21 Cl2D 34.4(5) . . ? # Cl2C Cl2A Cl2B 36.5(12) . . ? # Cl2C Cl2B Cl2A 11.0(4) . . ? # Cl2A Cl2C Cl2D 21.4(12) . . ? # Cl2A Cl2D Cl2C 22.2(13) . . ? O1 Pb1 O2 63.83(14) . . ? O1 Pb1 O6 140.51(14) . . ? O2 Pb1 O6 81.87(14) . . ? O1 Pb1 S1 68.00(11) . . ? O2 Pb1 S1 130.44(10) . . ? O6 Pb1 S1 147.33(10) . . ? O1 Pb1 S2 70.74(10) . . ? O2 Pb1 S2 87.05(10) . . ? O6 Pb1 S2 129.09(10) . . ? S1 Pb1 S2 66.44(5) . . ? O1 Pb1 S4 148.64(11) . . ? O2 Pb1 S4 125.03(10) . . ? O6 Pb1 S4 67.66(10) . . ? S1 Pb1 S4 91.67(5) . . ? S2 Pb1 S4 79.40(5) . . ? O1 Pb1 S3 127.92(11) . . ? O2 Pb1 S3 144.27(10) . . ? O6 Pb1 S3 71.07(10) . . ? S1 Pb1 S3 77.42(5) . . ? S2 Pb1 S3 128.13(5) . . ? S4 Pb1 S3 65.35(5) . . ? C10 S1 C1 102.5(4) . . ? C10 S1 Pb1 111.3(2) . . ? C1 S1 Pb1 96.2(2) . . ? C8 S2 C9 101.3(3) . . ? C8 S2 Pb1 104.2(2) . . ? C9 S2 Pb1 102.8(2) . . ? C20 S3 C11 101.6(3) . . ? C20 S3 Pb1 101.5(2) . . ? C11 S3 Pb1 105.2(2) . . ? C19 S4 C18 102.4(3) . . ? C19 S4 Pb1 112.0(2) . . ? C18 S4 Pb1 96.6(2) . . ? C2 O1 C3 111.4(5) . . ? C2 O1 Pb1 121.7(4) . . ? C3 O1 Pb1 113.6(4) . . ? C5 O2 C4 113.7(5) . . ? C5 O2 Pb1 123.0(4) . . ? C4 O2 Pb1 112.1(4) . . ? C7 O3 C6 112.1(5) . . ? C13 O4 C12 113.1(6) . . ? C14 O5 C15 114.3(5) . . ? C16 O6 C17 111.7(5) . . ? C16 O6 Pb1 114.1(4) . . ? C17 O6 Pb1 119.6(4) . . ? C2 C1 S1 115.8(5) . . ? C2 C1 H1A 108.3 . . ? S1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? S1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? O1 C2 C1 109.4(6) . . ? O1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? O1 C3 C4 108.4(6) . . ? O1 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O1 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? O2 C4 C3 112.0(6) . . ? O2 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? O2 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? O2 C5 C6 107.0(5) . . ? O2 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? O2 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? O3 C6 C5 111.0(6) . . ? O3 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? O3 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? O3 C7 C8 107.9(5) . . ? O3 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O3 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C7 C8 S2 108.5(5) . . ? C7 C8 H8A 110.0 . . ? S2 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? S2 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 S2 110.6(5) . . ? C10 C9 H9A 109.5 . . ? S2 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? S2 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 S1 113.9(5) . . ? C9 C10 H10A 108.8 . . ? S1 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? S1 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 S3 109.1(5) . . ? C12 C11 H11A 109.9 . . ? S3 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? S3 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O4 C12 C11 109.4(6) . . ? O4 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O4 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? O4 C13 C14 111.5(6) . . ? O4 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? O4 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? O5 C14 C13 108.1(6) . . ? O5 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O5 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O5 C15 C16 111.7(5) . . ? O5 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? O5 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O6 C16 C15 108.3(5) . . ? O6 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O6 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O6 C17 C18 110.2(5) . . ? O6 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O6 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C17 C18 S4 116.1(5) . . ? C17 C18 H18A 108.3 . . ? S4 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? S4 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C20 C19 S4 113.0(5) . . ? C20 C19 H19A 109.0 . . ? S4 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? S4 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 S3 110.2(5) . . ? C19 C20 H20A 109.6 . . ? S3 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? S3 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? F2 B1 F1 110.9(7) . . ? F2 B1 F3 110.8(6) . . ? F1 B1 F3 109.2(6) . . ? F2 B1 F4 109.0(6) . . ? F1 B1 F4 108.3(6) . . ? F3 B1 F4 108.7(6) . . ? F8A B2 F5 110.0(8) . . ? F6B B2 F5 124.9(10) . . ? F6B B2 F7B 114.0(10) . . ? F5 B2 F7B 102.5(9) . . ? F8A B2 F7A 112.8(9) . . ? F5 B2 F7A 113.6(8) . . ? F8A B2 F6A 110.0(8) . . ? F5 B2 F6A 105.5(7) . . ? F7A B2 F6A 104.5(8) . . ? F6B B2 F8B 105.7(9) . . ? F5 B2 F8B 104.1(8) . . ? F7B B2 F8B 103.5(10) . . ? Cl2A C21 Cl1 110.7(7) . . ? Cl1 C21 Cl2C 107.7(7) . . ? Cl2A C21 Cl2B 81.6(6) . . ? Cl1 C21 Cl2B 103.6(6) . . ? Cl2C C21 Cl2B 62.2(6) . . ? Cl1 C21 Cl2D 100.2(6) . . ? Cl2B C21 Cl2D 96.7(6) . . ? Cl2D Cl2A Cl2C 136(2) . . ? Cl2D Cl2A C21 107.9(16) . . ? Cl2C Cl2A C21 86.4(14) . . ? Cl2D Cl2A Cl2B 150.5(16) . . ? C21 Cl2A Cl2B 53.2(5) . . ? Cl2C Cl2B C21 55.1(5) . . ? Cl2C Cl2B Cl3A 128.6(7) . . ? C21 Cl2B Cl3A 143.3(7) . . ? C21 Cl2B Cl2A 45.2(4) . . ? Cl3A Cl2B Cl2A 138.7(6) . . ? Cl2C Cl2B Cl3A 116.0(6) . 2_565 ? C21 Cl2B Cl3A 137.8(6) . 2_565 ? Cl3A Cl2B Cl3A 77.3(5) . 2_565 ? Cl2A Cl2B Cl3A 118.8(5) . 2_565 ? Cl2A Cl2C C21 73.3(13) . . ? Cl2D Cl2C C21 82.3(8) . . ? Cl2A Cl2C Cl2B 132.5(15) . . ? Cl2D Cl2C Cl2B 144.9(9) . . ? C21 Cl2C Cl2B 62.6(5) . . ? Cl2A Cl2D C21 55.4(14) . . ? Cl2C Cl2D C21 63.2(8) . . ? Cl3B Cl3A Cl2B 138.5(17) . . ? Cl3B Cl3A Cl2B 97.5(16) . 2_565 ? Cl2B Cl3A Cl2B 67.7(5) . 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 S1 C1 C2 65.0(6) . . . . ? Pb1 S1 C1 C2 -48.4(6) . . . . ? C3 O1 C2 C1 178.7(6) . . . . ? Pb1 O1 C2 C1 -42.8(8) . . . . ? S1 C1 C2 O1 64.3(8) . . . . ? C2 O1 C3 C4 -169.4(6) . . . . ? Pb1 O1 C3 C4 48.6(6) . . . . ? C5 O2 C4 C3 -100.4(7) . . . . ? Pb1 O2 C4 C3 44.7(7) . . . . ? O1 C3 C4 O2 -63.5(7) . . . . ? C4 O2 C5 C6 169.0(6) . . . . ? Pb1 O2 C5 C6 28.2(7) . . . . ? C7 O3 C6 C5 -79.8(7) . . . . ? O2 C5 C6 O3 -61.6(7) . . . . ? C6 O3 C7 C8 168.1(6) . . . . ? O3 C7 C8 S2 -61.4(6) . . . . ? C9 S2 C8 C7 164.0(5) . . . . ? Pb1 S2 C8 C7 57.6(5) . . . . ? C8 S2 C9 C10 -173.1(5) . . . . ? Pb1 S2 C9 C10 -65.6(5) . . . . ? S2 C9 C10 S1 59.0(6) . . . . ? C1 S1 C10 C9 -121.9(6) . . . . ? Pb1 S1 C10 C9 -20.0(6) . . . . ? C20 S3 C11 C12 164.3(5) . . . . ? Pb1 S3 C11 C12 58.9(5) . . . . ? C13 O4 C12 C11 165.2(6) . . . . ? S3 C11 C12 O4 -62.2(7) . . . . ? C12 O4 C13 C14 -80.2(8) . . . . ? C15 O5 C14 C13 173.6(6) . . . . ? O4 C13 C14 O5 -63.1(8) . . . . ? C14 O5 C15 C16 -96.6(7) . . . . ? C17 O6 C16 C15 -175.2(5) . . . . ? Pb1 O6 C16 C15 45.4(6) . . . . ? O5 C15 C16 O6 -66.2(7) . . . . ? C16 O6 C17 C18 177.4(5) . . . . ? Pb1 O6 C17 C18 -45.7(6) . . . . ? O6 C17 C18 S4 66.3(7) . . . . ? C19 S4 C18 C17 66.9(6) . . . . ? Pb1 S4 C18 C17 -47.5(5) . . . . ? C18 S4 C19 C20 -122.2(5) . . . . ? Pb1 S4 C19 C20 -19.8(6) . . . . ? S4 C19 C20 S3 61.0(6) . . . . ? C11 S3 C20 C19 -176.4(5) . . . . ? Pb1 S3 C20 C19 -68.1(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pb1 O3 2.898(5) . . ? Pb1 O4 3.055(5) . . ? Pb1 O5 2.761(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.639 _refine_diff_density_min -1.780 _refine_diff_density_rms 0.176 data_12paf089ra _database_code_depnum_ccdc_archive 'CCDC 900331' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-06-30 _audit_author_name 'Farina, P. A.' _audit_update_record '2012-07-01 Moved C6 for better connectivity' _chemical_name_systematic ; (1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)lead(II) tetrafluoroborate ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxo-7,16-diselena-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 O4 Pb Se2 2+, 2(B F4 1-)' _chemical_formula_sum 'C12 H24 B2 F8 O4 Pb Se2' _chemical_formula_weight 771.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.953(5) _cell_length_b 12.060(5) _cell_length_c 15.530(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.693(6) _cell_angle_gamma 90.00 _cell_volume 2051.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5363 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 11.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6169 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2340 _reflns_number_gt 1930 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+24.4500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2340 _refine_ls_number_parameters 132 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.11258(3) 0.2500 0.01026(10) Uani 1 2 d S . . Se1 Se 0.22036(6) 0.16832(6) 0.28252(4) 0.01625(17) Uani 1 1 d U . . O1 O 0.3396(4) -0.0120(4) 0.1567(3) 0.0135(10) Uani 1 1 d U . . O2 O 0.5946(4) -0.0238(4) 0.1412(3) 0.0160(11) Uani 1 1 d . . . C1 C 0.1475(6) 0.0786(6) 0.1904(4) 0.0154(12) Uani 1 1 d U . . H1A H 0.1130 0.0105 0.2160 0.018 Uiso 1 1 calc R . . H1B H 0.0791 0.1207 0.1639 0.018 Uiso 1 1 calc R . . C2 C 0.2355(6) 0.0455(6) 0.1198(4) 0.0144(12) Uani 1 1 d U . . H2A H 0.1932 -0.0034 0.0778 0.017 Uiso 1 1 calc R . . H2B H 0.2634 0.1125 0.0890 0.017 Uiso 1 1 calc R . . C3 C 0.3977(6) -0.0783(6) 0.0914(4) 0.0155(14) Uani 1 1 d U . . H3A H 0.4089 -0.0335 0.0387 0.019 Uiso 1 1 calc R . . H3B H 0.3454 -0.1427 0.0766 0.019 Uiso 1 1 calc R . . C4 C 0.5183(6) -0.1175(6) 0.1243(4) 0.0131(13) Uani 1 1 d . . . H4A H 0.5073 -0.1608 0.1779 0.016 Uiso 1 1 calc R . . H4B H 0.5569 -0.1662 0.0811 0.016 Uiso 1 1 calc R . . C5 C 0.7245(6) -0.0473(6) 0.1387(5) 0.0158(15) Uani 1 1 d . . . H5A H 0.7419 -0.0999 0.0914 0.019 Uiso 1 1 calc R . . H5B H 0.7517 -0.0813 0.1937 0.019 Uiso 1 1 calc R . . C6 C 0.7914(6) 0.0604(6) 0.1242(4) 0.0167(15) Uani 1 1 d . . . H6A H 0.7592 0.0949 0.0707 0.020 Uiso 1 1 calc R . . H6B H 0.8788 0.0436 0.1150 0.020 Uiso 1 1 calc R . . F1 F 0.4703(4) 0.1864(3) 0.0865(3) 0.0259(10) Uani 1 1 d . . . F2 F 0.6327(4) 0.2926(4) 0.0528(3) 0.0315(11) Uani 1 1 d . . . F3 F 0.4409(4) 0.3452(4) 0.0116(3) 0.0297(11) Uani 1 1 d . . . F4 F 0.4972(4) 0.3496(4) 0.1542(3) 0.0362(13) Uani 1 1 d . . . B1 B 0.5105(8) 0.2965(6) 0.0751(5) 0.0160(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01020(18) 0.01135(18) 0.00926(17) 0.000 0.00142(12) 0.000 Se1 0.0139(4) 0.0173(4) 0.0175(4) -0.0018(3) 0.0005(3) 0.0024(3) O1 0.015(2) 0.014(2) 0.012(2) 0.0000(17) -0.0020(17) 0.0030(18) O2 0.008(2) 0.016(3) 0.024(3) -0.004(2) 0.000(2) -0.001(2) C1 0.008(3) 0.019(4) 0.018(3) 0.002(2) -0.0047(19) 0.001(2) C2 0.009(3) 0.024(4) 0.011(2) 0.001(2) -0.0076(19) -0.004(2) C3 0.016(3) 0.026(4) 0.004(3) -0.004(2) -0.003(2) -0.001(2) C4 0.011(3) 0.014(3) 0.014(3) 0.002(3) 0.004(3) -0.002(3) C5 0.009(3) 0.015(4) 0.023(4) -0.004(3) 0.004(3) 0.004(3) C6 0.011(3) 0.025(4) 0.014(4) -0.007(3) 0.001(3) 0.000(3) F1 0.033(3) 0.024(2) 0.021(2) 0.0079(18) -0.002(2) -0.010(2) F2 0.019(2) 0.041(3) 0.034(3) 0.002(2) 0.009(2) -0.003(2) F3 0.033(3) 0.032(3) 0.023(3) 0.0073(19) -0.003(2) 0.016(2) F4 0.035(3) 0.049(3) 0.025(3) -0.021(2) 0.004(2) 0.001(2) B1 0.023(5) 0.011(4) 0.014(4) -0.001(3) 0.001(3) 0.002(4) _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 O2 2.584(5) . ? Pb1 O2 2.584(5) 2_655 ? Pb1 F1 2.707(4) 2_655 ? Pb1 F1 2.707(4) . ? Pb1 O1 2.717(4) . ? Pb1 O1 2.717(4) 2_655 ? Pb1 Se1 3.1820(14) 2_655 ? Pb1 Se1 3.1820(14) . ? Se1 C6 1.953(7) 2_655 ? Se1 C1 1.957(7) . ? O1 C3 1.444(8) . ? O1 C2 1.447(7) . ? O2 C4 1.428(8) . ? O2 C5 1.451(8) . ? C1 C2 1.521(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.488(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 Se1 1.953(7) 2_655 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? F1 B1 1.410(9) . ? F2 B1 1.387(9) . ? F3 B1 1.371(9) . ? F4 B1 1.396(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 O2 Pb1 O2 100.9(2) . 2_655 ? O2 Pb1 F1 141.10(14) . 2_655 ? O2 Pb1 F1 68.93(14) 2_655 2_655 ? O2 Pb1 F1 68.93(14) . . ? O2 Pb1 F1 141.10(14) 2_655 . ? F1 Pb1 F1 141.60(18) 2_655 . ? O2 Pb1 O1 63.95(14) . . ? O2 Pb1 O1 74.62(14) 2_655 . ? F1 Pb1 O1 138.75(14) 2_655 . ? F1 Pb1 O1 67.17(13) . . ? O2 Pb1 O1 74.62(14) . 2_655 ? O2 Pb1 O1 63.95(14) 2_655 2_655 ? F1 Pb1 O1 67.17(13) 2_655 2_655 ? F1 Pb1 O1 138.75(14) . 2_655 ? O1 Pb1 O1 112.84(19) . 2_655 ? O2 Pb1 Se1 68.67(10) . 2_655 ? O2 Pb1 Se1 129.25(10) 2_655 2_655 ? F1 Pb1 Se1 88.54(10) 2_655 2_655 ? F1 Pb1 Se1 83.49(10) . 2_655 ? O1 Pb1 Se1 130.50(10) . 2_655 ? O1 Pb1 Se1 65.43(10) 2_655 2_655 ? O2 Pb1 Se1 129.25(10) . . ? O2 Pb1 Se1 68.67(10) 2_655 . ? F1 Pb1 Se1 83.49(10) 2_655 . ? F1 Pb1 Se1 88.54(10) . . ? O1 Pb1 Se1 65.43(10) . . ? O1 Pb1 Se1 130.50(10) 2_655 . ? Se1 Pb1 Se1 155.61(3) 2_655 . ? C6 Se1 C1 98.3(3) 2_655 . ? C6 Se1 Pb1 92.8(2) 2_655 . ? C1 Se1 Pb1 98.7(2) . . ? C3 O1 C2 109.8(5) . . ? C3 O1 Pb1 113.2(4) . . ? C2 O1 Pb1 116.6(4) . . ? C4 O2 C5 114.3(5) . . ? C4 O2 Pb1 112.7(4) . . ? C5 O2 Pb1 122.9(4) . . ? C2 C1 Se1 114.6(4) . . ? C2 C1 H1A 108.6 . . ? Se1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? Se1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? O1 C2 C1 110.1(5) . . ? O1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? O1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O1 C3 C4 109.3(5) . . ? O1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 109.1(6) . . ? O2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O2 C5 C6 108.3(5) . . ? O2 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O2 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C5 C6 Se1 115.2(5) . 2_655 ? C5 C6 H6A 108.5 . . ? Se1 C6 H6A 108.5 2_655 . ? C5 C6 H6B 108.5 . . ? Se1 C6 H6B 108.5 2_655 . ? H6A C6 H6B 107.5 . . ? B1 F1 Pb1 113.2(4) . . ? F3 B1 F2 111.4(6) . . ? F3 B1 F4 111.9(6) . . ? F2 B1 F4 110.3(6) . . ? F3 B1 F1 108.8(6) . . ? F2 B1 F1 107.7(6) . . ? F4 B1 F1 106.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Se1 C1 C2 -112.7(5) 2_655 . . . ? Pb1 Se1 C1 C2 -18.5(5) . . . . ? C3 O1 C2 C1 158.6(5) . . . . ? Pb1 O1 C2 C1 -71.1(6) . . . . ? Se1 C1 C2 O1 55.8(7) . . . . ? C2 O1 C3 C4 168.0(5) . . . . ? Pb1 O1 C3 C4 35.8(6) . . . . ? C5 O2 C4 C3 -155.6(5) . . . . ? Pb1 O2 C4 C3 57.8(6) . . . . ? O1 C3 C4 O2 -62.4(7) . . . . ? C4 O2 C5 C6 159.2(5) . . . . ? Pb1 O2 C5 C6 -58.1(6) . . . . ? O2 C5 C6 Se1 65.4(6) . . . 2_655 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pb1 F1 2.706(4) . . ? Pb1 F4 3.223(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.229 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.254 data_12paf090ra _database_code_depnum_ccdc_archive 'CCDC 900332' #TrackingRef 'Pb_all6_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-07-03 _audit_author_name 'Farina, P. A.' _audit_update_record ; 2012-07-02 Moved 4 ring atoms for better connectivity. mw ; _chemical_name_systematic ; (1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)lead(II) nitrate ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxo-7,16-diselena-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 O4 Pb Se2 2+, 2(N O3 1-)' _chemical_formula_sum 'C12 H24 N2 O10 Pb Se2' _chemical_formula_weight 721.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.969(4) _cell_length_b 11.735(5) _cell_length_c 15.385(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.382(6) _cell_angle_gamma 90.00 _cell_volume 1980.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6808 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block # small! _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 12.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.424 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9116 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.1040 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2271 _reflns_number_gt 1699 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+18.5409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2271 _refine_ls_number_parameters 141 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.0000 0.12100(5) 0.2500 0.0277(2) Uani 1 2 d S . . Se1 Se 0.28423(11) 0.15628(10) 0.22376(9) 0.0380(3) Uani 1 1 d . . . O1 O 0.0950(7) -0.0307(6) 0.1296(5) 0.0321(18) Uani 1 1 d . A . O2 O -0.1645(7) -0.0278(6) 0.1511(5) 0.0329(18) Uani 1 1 d . A . C1 C 0.2969(10) 0.0491(9) 0.1267(7) 0.032(3) Uani 1 1 d . . . H1A H 0.2708 0.0885 0.0728 0.039 Uiso 1 1 calc R A . H1B H 0.3836 0.0277 0.1199 0.039 Uiso 1 1 calc R . . C2 C 0.2235(10) -0.0572(9) 0.1359(8) 0.033(3) Uani 1 1 d . A . H2A H 0.2459 -0.1118 0.0897 0.039 Uiso 1 1 calc R . . H2B H 0.2412 -0.0930 0.1929 0.039 Uiso 1 1 calc R . . C3 C 0.0204(10) -0.1288(9) 0.1204(8) 0.032(2) Uani 1 1 d . . . H3A H 0.0107 -0.1668 0.1774 0.038 Uiso 1 1 calc R A . H3B H 0.0585 -0.1834 0.0797 0.038 Uiso 1 1 calc R . . C4 C -0.1011(11) -0.0919(9) 0.0860(8) 0.034(3) Uani 1 1 d . A . H4A H -0.0899 -0.0443 0.0335 0.041 Uiso 1 1 calc R . . H4B H -0.1498 -0.1596 0.0694 0.041 Uiso 1 1 calc R . . C5 C -0.2692(11) 0.0264(11) 0.1157(8) 0.042(3) Uani 1 1 d . . . H5A H -0.3111 -0.0263 0.0751 0.051 Uiso 1 1 calc R A . H5B H -0.2441 0.0947 0.0825 0.051 Uiso 1 1 calc R . . C6 C -0.3561(11) 0.0611(11) 0.1865(8) 0.039(3) Uani 1 1 d . . . H6A H -0.3891 -0.0085 0.2140 0.047 Uiso 1 1 calc R . . H6B H -0.4254 0.1027 0.1598 0.047 Uiso 1 1 calc R . . N1 N -0.0044(9) 0.2899(8) 0.0952(8) 0.041(3) Uani 1 1 d D . . O3 O -0.0095(10) 0.3561(7) 0.0314(8) 0.063(3) Uani 1 1 d . A . O4A O -0.029(3) 0.1903(14) 0.0899(14) 0.066(7) Uani 0.50 1 d PD A 1 O5A O -0.002(2) 0.3208(14) 0.1763(10) 0.055(5) Uani 0.50 1 d PD A 1 O4B O 0.0992(16) 0.258(2) 0.1105(18) 0.090(9) Uani 0.50 1 d PD A 2 O5B O -0.0893(17) 0.237(3) 0.119(2) 0.101(12) Uani 0.50 1 d PD A 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 0.0267(3) 0.0272(3) 0.0291(3) 0.000 0.0009(2) 0.000 Se1 0.0358(7) 0.0362(6) 0.0421(8) -0.0054(5) 0.0068(6) -0.0049(5) O1 0.028(4) 0.030(4) 0.038(5) -0.002(3) -0.003(4) -0.005(3) O2 0.027(4) 0.047(5) 0.025(4) -0.003(3) 0.007(3) 0.003(3) C1 0.025(6) 0.047(7) 0.025(6) 0.012(5) -0.004(5) -0.008(5) C2 0.034(6) 0.036(6) 0.028(7) -0.008(5) 0.003(5) 0.002(5) C3 0.029(6) 0.034(6) 0.033(7) 0.001(5) 0.005(5) -0.004(5) C4 0.038(7) 0.037(6) 0.028(6) -0.002(5) 0.003(5) -0.010(5) C5 0.035(7) 0.063(8) 0.029(7) 0.011(6) -0.007(6) -0.002(6) C6 0.031(7) 0.053(8) 0.033(7) -0.001(5) 0.007(6) 0.000(5) N1 0.034(6) 0.033(6) 0.056(8) -0.002(5) -0.002(6) 0.001(4) O3 0.071(8) 0.041(5) 0.078(8) 0.025(5) 0.019(6) 0.007(5) O4A 0.10(2) 0.063(15) 0.037(13) -0.016(10) -0.013(14) 0.013(14) O5A 0.090(17) 0.035(10) 0.041(12) -0.004(8) -0.007(11) 0.001(10) O4B 0.044(14) 0.091(17) 0.14(3) 0.055(16) -0.012(15) 0.024(12) O5B 0.032(13) 0.13(2) 0.14(3) 0.10(2) 0.026(15) 0.012(14) _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 O5A 2.605(17) 2 ? Pb1 O5A 2.605(17) . ? Pb1 O4A 2.61(2) . ? Pb1 O4A 2.61(2) 2 ? Pb1 O5B 2.62(2) 2 ? Pb1 O5B 2.62(2) . ? Pb1 O1 2.777(8) . ? Pb1 O4B 2.90(2) . ? Pb1 O2 2.929(8) . ? Pb1 Se1 3.1736(18) 2 ? Pb1 Se1 3.1736(18) . ? Se1 C6 1.939(12) 2 ? Se1 C1 1.957(12) . ? O1 C3 1.418(12) . ? O1 C2 1.446(13) . ? O2 C5 1.419(13) . ? O2 C4 1.436(13) . ? C1 C2 1.492(15) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.495(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.508(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 Se1 1.939(12) 2 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N1 O5B 1.176(16) . ? N1 O4A 1.202(16) . ? N1 O4B 1.218(15) . ? N1 O3 1.252(13) . ? N1 O5A 1.300(14) . ? 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 O5A Pb1 O5A 51.6(7) 2 . ? O5A Pb1 O4A 97.5(5) 2 . ? O5A Pb1 O4A 46.2(5) . . ? O5A Pb1 O4A 46.2(5) 2 2 ? O5A Pb1 O4A 97.5(5) . 2 ? O4A Pb1 O4A 143.7(7) . 2 ? O5A Pb1 O5B 36.3(8) 2 2 ? O5A Pb1 O5B 82.5(10) . 2 ? O4A Pb1 O5B 127.4(9) . 2 ? O4A Pb1 O5B 21.4(7) 2 2 ? O5A Pb1 O5B 82.5(10) 2 . ? O5A Pb1 O5B 36.3(8) . . ? O4A Pb1 O5B 21.4(7) . . ? O4A Pb1 O5B 127.4(9) 2 . ? O5B Pb1 O5B 117.3(17) 2 . ? O5A Pb1 O1 149.9(5) 2 . ? O5A Pb1 O1 106.8(4) . . ? O4A Pb1 O1 67.3(5) . . ? O4A Pb1 O1 141.8(5) 2 . ? O5B Pb1 O1 135.0(4) 2 . ? O5B Pb1 O1 87.7(9) . . ? O5A Pb1 O4B 79.6(7) 2 . ? O5A Pb1 O4B 34.9(6) . . ? O4A Pb1 O4B 34.2(7) . . ? O4A Pb1 O4B 118.7(7) 2 . ? O5B Pb1 O4B 98.1(10) 2 . ? O5B Pb1 O4B 44.0(5) . . ? O1 Pb1 O4B 73.7(6) . . ? O5A Pb1 O2 140.0(5) 2 . ? O5A Pb1 O2 107.9(4) . . ? O4A Pb1 O2 68.0(5) . . ? O4A Pb1 O2 138.2(6) 2 . ? O5B Pb1 O2 159.4(7) 2 . ? O5B Pb1 O2 71.6(7) . . ? O1 Pb1 O2 60.3(2) . . ? O4B Pb1 O2 100.4(6) . . ? O5A Pb1 Se1 80.3(5) 2 2 ? O5A Pb1 Se1 86.2(5) . 2 ? O4A Pb1 Se1 88.1(6) . 2 ? O4A Pb1 Se1 87.2(6) 2 2 ? O5B Pb1 Se1 101.3(4) 2 2 ? O5B Pb1 Se1 70.6(4) . 2 ? O1 Pb1 Se1 122.80(15) . 2 ? O4B Pb1 Se1 113.3(3) . 2 ? O2 Pb1 Se1 62.72(15) . 2 ? O5A Pb1 Se1 86.2(5) 2 . ? O5A Pb1 Se1 80.3(5) . . ? O4A Pb1 Se1 87.2(6) . . ? O4A Pb1 Se1 88.1(6) 2 . ? O5B Pb1 Se1 70.6(4) 2 . ? O5B Pb1 Se1 101.3(4) . . ? O1 Pb1 Se1 68.01(15) . . ? O4B Pb1 Se1 57.3(3) . . ? O2 Pb1 Se1 127.87(15) . . ? Se1 Pb1 Se1 165.01(5) 2 . ? C6 Se1 C1 98.2(5) 2 . ? C6 Se1 Pb1 103.3(4) 2 . ? C1 Se1 Pb1 95.0(3) . . ? C3 O1 C2 113.2(8) . . ? C3 O1 Pb1 111.6(6) . . ? C2 O1 Pb1 117.5(6) . . ? C5 O2 C4 111.2(9) . . ? C5 O2 Pb1 115.3(7) . . ? C4 O2 Pb1 112.0(6) . . ? C2 C1 Se1 115.1(8) . . ? C2 C1 H1A 108.5 . . ? Se1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? Se1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? O1 C2 C1 109.9(9) . . ? O1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O1 C3 C4 108.2(9) . . ? O1 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O1 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O2 C4 C3 109.9(9) . . ? O2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O2 C5 C6 111.0(10) . . ? O2 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O2 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 Se1 114.5(8) . 2 ? C5 C6 H6A 108.6 . . ? Se1 C6 H6A 108.6 2 . ? C5 C6 H6B 108.6 . . ? Se1 C6 H6B 108.6 2 . ? H6A C6 H6B 107.6 . . ? O5B N1 O4A 48.3(17) . . ? O5B N1 O4B 121.4(18) . . ? O4A N1 O4B 85.7(18) . . ? O5B N1 O3 122.3(16) . . ? O4A N1 O3 122.8(15) . . ? O4B N1 O3 112.1(15) . . ? O5B N1 O5A 82(2) . . ? O4A N1 O5A 109.9(15) . . ? O4B N1 O5A 83.4(17) . . ? O3 N1 O5A 125.4(12) . . ? N1 O4A Pb1 102.3(12) . . ? N1 O5A Pb1 99.6(10) . . ? N1 O4B Pb1 87.6(13) . . ? N1 O5B Pb1 102.5(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Se1 C1 C2 64.0(9) 2 . . . ? Pb1 Se1 C1 C2 -40.2(8) . . . . ? C3 O1 C2 C1 168.2(9) . . . . ? Pb1 O1 C2 C1 -59.4(10) . . . . ? Se1 C1 C2 O1 69.1(10) . . . . ? C2 O1 C3 C4 -161.8(9) . . . . ? Pb1 O1 C3 C4 62.9(10) . . . . ? C5 O2 C4 C3 169.0(9) . . . . ? Pb1 O2 C4 C3 38.4(10) . . . . ? O1 C3 C4 O2 -69.1(11) . . . . ? C4 O2 C5 C6 161.9(9) . . . . ? Pb1 O2 C5 C6 -69.3(11) . . . . ? O2 C5 C6 Se1 55.0(13) . . . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.023 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.278 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE ============================================================= data_12paf109ra _database_code_depnum_ccdc_archive 'CCDC 912764' #TrackingRef 'Pb_all2_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-11-22 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,4,7,10,13,16-hexaoxacyclooctadecane-nitrato-lead(II) hexafluorophosphate ; # C12H24O6 = 18-crown-6 # 1,4,7,10,13,16-hexaoxacyclooctadecane (Chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 N O9 Pb 1+, F6 P 1-' _chemical_formula_sum 'C12 H24 F6 N O9 P Pb' _chemical_formula_structural '((C12 H24 O6) (N O3) Pb) (P F6)' _chemical_formula_weight 678.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m n 21' _space_group_IT_number 31 _space_group_name_Hall 'P 2ac -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 12.958(5) _cell_length_b 8.475(3) _cell_length_c 9.296(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1020.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6273 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 8.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.536 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6653 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2334 _reflns_number_gt 2041 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' # WinGX (Farrugia) + SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(12) _chemical_absolute_configuration ad _refine_ls_number_reflns 2334 _refine_ls_number_parameters 148 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.13864(4) 0.49691(8) 0.02398(13) Uani 1 2 d S . . O1 O 0.5000 -0.1647(11) 0.4030(11) 0.029(2) Uani 1 2 d S . . O2 O 0.3159(4) 0.0077(7) 0.4162(7) 0.0260(14) Uani 1 1 d . . . O3 O 0.3149(5) 0.2892(8) 0.5746(7) 0.0304(15) Uani 1 1 d . . . O4 O 0.5000 0.4449(12) 0.6104(10) 0.029(2) Uani 1 2 d S . . C1 C 0.4111(6) -0.2098(12) 0.3231(11) 0.028(2) Uani 1 1 d . . . H1A H 0.4101 -0.3257 0.3097 0.033 Uiso 1 1 calc R . . H1B H 0.4122 -0.1593 0.2271 0.033 Uiso 1 1 calc R . . C2 C 0.3168(7) -0.1582(11) 0.4050(12) 0.030(2) Uani 1 1 d . . . H2A H 0.2539 -0.1945 0.3545 0.036 Uiso 1 1 calc R . . H2B H 0.3174 -0.2057 0.5023 0.036 Uiso 1 1 calc R . . C3 C 0.2260(6) 0.0640(10) 0.487(2) 0.030(2) Uani 1 1 d . . . H3A H 0.2240 0.0251 0.5872 0.036 Uiso 1 1 calc R . . H3B H 0.1634 0.0262 0.4365 0.036 Uiso 1 1 calc R . . C4 C 0.2299(6) 0.2392(10) 0.4850(19) 0.028(2) Uani 1 1 d . . . H4A H 0.2399 0.2775 0.3853 0.034 Uiso 1 1 calc R . . H4B H 0.1643 0.2832 0.5221 0.034 Uiso 1 1 calc R . . C5 C 0.3177(7) 0.4544(11) 0.5883(12) 0.031(2) Uani 1 1 d . . . H5A H 0.2529 0.4929 0.6324 0.038 Uiso 1 1 calc R . . H5B H 0.3252 0.5040 0.4925 0.038 Uiso 1 1 calc R . . C6 C 0.4090(7) 0.4973(13) 0.6828(13) 0.033(2) Uani 1 1 d . . . H6A H 0.4116 0.6128 0.6980 0.039 Uiso 1 1 calc R . . H6B H 0.4029 0.4450 0.7777 0.039 Uiso 1 1 calc R . . N1 N 0.5000 -0.0532(14) 0.7480(12) 0.025(3) Uani 1 2 d S . . O5 O 0.4167(5) -0.0088(10) 0.7025(9) 0.044(2) Uani 1 1 d . . . O6 O 0.5000 -0.1576(12) 0.8519(13) 0.042(3) Uani 1 2 d S . . P1 P 0.5000 0.3214(5) 0.1269(4) 0.0264(8) Uani 1 2 d S . . F1 F 0.5000 0.5013(10) 0.0800(10) 0.041(2) Uani 1 2 d S . . F2 F 0.5000 0.1401(9) 0.1769(10) 0.042(2) Uani 1 2 d S . . F3 F 0.4131(5) 0.2865(8) 0.0145(12) 0.066(2) Uani 1 1 d . . . F4 F 0.4141(6) 0.3581(8) 0.2475(9) 0.057(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02054(18) 0.0205(2) 0.0309(2) 0.0008(6) 0.000 0.000 O1 0.018(4) 0.038(6) 0.030(5) 0.005(5) 0.000 0.000 O2 0.023(3) 0.018(4) 0.036(4) -0.002(3) 0.005(3) 0.000(3) O3 0.025(4) 0.023(4) 0.043(4) 0.003(3) 0.004(3) 0.002(3) O4 0.026(5) 0.026(6) 0.036(5) -0.004(5) 0.000 0.000 C1 0.026(5) 0.023(5) 0.035(5) -0.008(5) -0.001(4) -0.006(4) C2 0.023(5) 0.026(6) 0.041(6) 0.001(5) -0.004(4) -0.004(4) C3 0.022(4) 0.026(4) 0.041(7) -0.003(8) 0.014(6) 0.007(3) C4 0.018(3) 0.030(4) 0.038(7) 0.002(7) -0.007(5) 0.002(3) C5 0.024(5) 0.017(5) 0.053(7) 0.002(5) 0.002(4) 0.005(4) C6 0.034(5) 0.027(6) 0.037(6) -0.005(5) 0.009(5) 0.011(4) N1 0.007(5) 0.037(7) 0.031(6) -0.014(6) 0.000 0.000 O5 0.030(4) 0.057(5) 0.044(5) 0.013(4) 0.008(3) 0.003(4) O6 0.038(6) 0.039(7) 0.050(7) 0.004(5) 0.000 0.000 P1 0.0214(16) 0.0211(19) 0.037(2) 0.0014(16) 0.000 0.000 F1 0.043(5) 0.028(5) 0.051(5) 0.006(4) 0.000 0.000 F2 0.054(6) 0.025(5) 0.046(6) -0.002(4) 0.000 0.000 F3 0.072(5) 0.058(4) 0.069(6) 0.014(6) -0.040(6) -0.026(3) F4 0.046(4) 0.058(5) 0.068(5) 0.012(4) 0.026(4) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.525(7) . ? Pb1 O5 2.525(7) 4_655 ? Pb1 O1 2.715(9) . ? Pb1 O2 2.736(6) . ? Pb1 O2 2.736(6) 4_655 ? Pb1 O4 2.801(10) . ? Pb1 O3 2.811(6) . ? O1 C1 1.423(10) . ? O1 C1 1.423(10) 4_655 ? O2 C2 1.410(10) . ? O2 C3 1.420(10) . ? O3 C5 1.406(12) . ? O3 C4 1.445(13) . ? O4 C6 1.429(10) 4_655 ? O4 C6 1.429(10) . ? C1 C2 1.504(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.486(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.517(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N1 O5 1.219(8) . ? N1 O5 1.219(8) 4_655 ? N1 O6 1.310(16) . ? P1 F3 1.564(9) . ? P1 F3 1.564(9) 4_655 ? P1 F1 1.586(9) . ? P1 F2 1.605(9) . ? P1 F4 1.610(7) 4_655 ? P1 F4 1.610(7) . ? 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 O5 Pb1 O5 50.6(3) . 4_655 ? O5 Pb1 O1 77.0(3) . . ? O5 Pb1 O1 77.0(3) 4_655 . ? O5 Pb1 O2 68.6(2) . . ? O5 Pb1 O2 112.3(2) 4_655 . ? O1 Pb1 O2 61.82(13) . . ? O5 Pb1 O2 112.3(2) . 4_655 ? O5 Pb1 O2 68.6(2) 4_655 4_655 ? O1 Pb1 O2 61.82(13) . 4_655 ? O2 Pb1 O2 121.4(3) . 4_655 ? O5 Pb1 O4 100.0(3) . . ? O5 Pb1 O4 100.0(3) 4_655 . ? O1 Pb1 O4 176.6(3) . . ? O2 Pb1 O4 118.62(13) . . ? O2 Pb1 O4 118.62(13) 4_655 . ? O5 Pb1 O3 70.5(2) . . ? O5 Pb1 O3 113.3(2) 4_655 . ? O1 Pb1 O3 120.82(15) . . ? O2 Pb1 O3 60.7(2) . . ? O2 Pb1 O3 176.87(19) 4_655 . ? O4 Pb1 O3 58.85(14) . . ? C1 O1 C1 108.2(10) . 4_655 ? C1 O1 Pb1 115.0(6) . . ? C1 O1 Pb1 115.0(6) 4_655 . ? C2 O2 C3 112.1(7) . . ? C2 O2 Pb1 114.7(5) . . ? C3 O2 Pb1 116.9(6) . . ? C5 O3 C4 111.4(7) . . ? C5 O3 Pb1 116.9(5) . . ? C4 O3 Pb1 111.7(6) . . ? C6 O4 C6 111.3(11) 4_655 . ? C6 O4 Pb1 117.7(6) 4_655 . ? C6 O4 Pb1 117.7(6) . . ? O1 C1 C2 108.4(8) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? O2 C2 C1 109.5(8) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 107.6(8) . . ? O2 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O2 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O3 C4 C3 108.2(8) . . ? O3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 108.1(8) . . ? O3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O4 C6 C5 107.2(9) . . ? O4 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O4 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? O5 N1 O5 124.6(13) . 4_655 ? O5 N1 O6 117.7(6) . . ? O5 N1 O6 117.7(6) 4_655 . ? N1 O5 Pb1 92.2(7) . . ? F3 P1 F3 92.1(8) . 4_655 ? F3 P1 F1 89.9(4) . . ? F3 P1 F1 89.9(4) 4_655 . ? F3 P1 F2 90.7(4) . . ? F3 P1 F2 90.7(4) 4_655 . ? F1 P1 F2 179.1(5) . . ? F3 P1 F4 177.7(5) . 4_655 ? F3 P1 F4 90.2(5) 4_655 4_655 ? F1 P1 F4 90.3(4) . 4_655 ? F2 P1 F4 89.0(4) . 4_655 ? F3 P1 F4 90.2(5) . . ? F3 P1 F4 177.7(5) 4_655 . ? F1 P1 F4 90.3(4) . . ? F2 P1 F4 89.0(4) . . ? F4 P1 F4 87.4(7) 4_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 C1 C2 -178.4(5) 4_655 . . . ? Pb1 O1 C1 C2 -48.4(10) . . . . ? C3 O2 C2 C1 177.3(10) . . . . ? Pb1 O2 C2 C1 -46.4(9) . . . . ? O1 C1 C2 O2 63.1(11) . . . . ? C2 O2 C3 C4 -176.7(9) . . . . ? Pb1 O2 C3 C4 48.0(13) . . . . ? C5 O3 C4 C3 -174.7(8) . . . . ? Pb1 O3 C4 C3 52.5(11) . . . . ? O2 C3 C4 O3 -66.9(14) . . . . ? C4 O3 C5 C6 -179.7(10) . . . . ? Pb1 O3 C5 C6 -49.6(9) . . . . ? C6 O4 C6 C5 172.8(6) 4_655 . . . ? Pb1 O4 C6 C5 -46.9(10) . . . . ? O3 C5 C6 O4 62.2(11) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pb1 F2 2.975(9) . . ? Pb1 F4 3.174(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.668 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.175 data_12paf125ra _database_code_depnum_ccdc_archive 'CCDC 912765' #TrackingRef 'Pb_all2_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-11-26 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bisaqua-1,4,7,10,13,16-hexaoxacyclooctadecane-lead(II) bis(hexafluorophosphate) hydrate ; # C12H24O6 = 18-crown-6 # 1,4,7,10,13,16-hexaoxacyclooctadecane (Chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H27.2 O7.6 Pb 2+ , 2(F6 P 1-), 0.6(H2 O)' _chemical_formula_sum 'C12 H28.40 F12 O8.20 P2 Pb' _chemical_formula_structural '((C12 H24 O6) (H2 O)1.6 Pb) (F6 P)2 (H2 O)0.6' _chemical_formula_weight 801.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.754(3) _cell_length_b 15.230(4) _cell_length_c 9.254(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.453(6) _cell_angle_gamma 90.00 _cell_volume 1233.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5148 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 7.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5846 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2908 _reflns_number_gt 2472 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+17.4072P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2908 _refine_ls_number_parameters 178 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.14071(6) 0.2500 0.34871(7) 0.0472(2) Uani 1 2 d S . . O1 O 0.3116(11) 0.2500 0.5963(11) 0.048(2) Uani 1 2 d S . . O2 O 0.2187(8) 0.0946(4) 0.4793(8) 0.0485(16) Uani 1 1 d . . . O3 O 0.0639(9) 0.0947(5) 0.2184(8) 0.0573(19) Uani 1 1 d . . . O4 O -0.0772(16) 0.2500 0.1319(12) 0.071(3) Uani 1 2 d S . . O5 O 0.428(2) 0.2500 0.312(2) 0.125(9) Uani 0.80 2 d SP . . O6 O 0.256(4) 0.2500 0.096(4) 0.24(2) Uani 0.80 2 d SP . . O7 O 0.530(3) 0.2500 0.025(3) 0.100(8) Uani 0.60 2 d SP . . C1 C 0.3112(15) 0.1721(7) 0.6827(13) 0.062(3) Uani 1 1 d . . . H1A H 0.2110 0.1647 0.7283 0.074 Uiso 1 1 calc R . . H1B H 0.3915 0.1756 0.7598 0.074 Uiso 1 1 calc R . . C2 C 0.3417(13) 0.0972(7) 0.5837(14) 0.062(3) Uani 1 1 d . . . H2A H 0.4401 0.1059 0.5352 0.074 Uiso 1 1 calc R . . H2B H 0.3469 0.0414 0.6386 0.074 Uiso 1 1 calc R . . C3 C 0.2342(15) 0.0233(6) 0.3836(15) 0.069(3) Uani 1 1 d . . . H3A H 0.2562 -0.0312 0.4384 0.082 Uiso 1 1 calc R . . H3B H 0.3196 0.0342 0.3178 0.082 Uiso 1 1 calc R . . C4 C 0.0905(15) 0.0143(7) 0.3002(14) 0.064(3) Uani 1 1 d . . . H4A H 0.0966 -0.0364 0.2335 0.077 Uiso 1 1 calc R . . H4B H 0.0051 0.0039 0.3663 0.077 Uiso 1 1 calc R . . C5 C -0.0791(18) 0.0946(10) 0.1442(15) 0.083(4) Uani 1 1 d . . . H5A H -0.1626 0.0977 0.2142 0.100 Uiso 1 1 calc R . . H5B H -0.0914 0.0398 0.0875 0.100 Uiso 1 1 calc R . . C6 C -0.086(2) 0.1723(11) 0.0455(15) 0.097(5) Uani 1 1 d . . . H6A H -0.0002 0.1706 -0.0219 0.116 Uiso 1 1 calc R . . H6B H -0.1831 0.1717 -0.0121 0.116 Uiso 1 1 calc R . . P1 P -0.2026(4) 0.2500 0.5860(4) 0.0350(7) Uani 1 2 d SD . . F1 F -0.0666(17) 0.2500 0.6797(19) 0.259(17) Uani 1 2 d SD . . F2 F -0.1228(14) 0.1803(5) 0.4895(13) 0.143(5) Uani 1 1 d . . . F3 F -0.2811(14) 0.1816(5) 0.6772(15) 0.162(6) Uani 1 1 d . . . F4 F -0.330(2) 0.2500 0.481(3) 0.33(2) Uani 1 2 d SD . . P2 P 0.5000 0.0000 1.0000 0.0567(10) Uani 1 2 d S . . F5 F 0.3435(8) 0.0530(5) 0.9830(8) 0.079(2) Uani 1 1 d . . . F6 F 0.5831(8) 0.0728(5) 0.9077(7) 0.0724(19) Uani 1 1 d . . . F7 F 0.5421(9) 0.0536(5) 1.1456(7) 0.076(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0460(3) 0.0277(3) 0.0675(4) 0.000 -0.0062(2) 0.000 O1 0.044(5) 0.036(5) 0.063(6) 0.000 -0.003(4) 0.000 O2 0.048(4) 0.025(3) 0.072(5) 0.002(3) 0.005(3) 0.003(3) O3 0.070(5) 0.036(4) 0.066(5) -0.014(3) 0.013(4) -0.007(3) O4 0.094(9) 0.073(8) 0.044(6) 0.000 -0.014(6) 0.000 O5 0.068(11) 0.23(3) 0.077(12) 0.000 0.020(9) 0.000 O6 0.14(2) 0.34(5) 0.24(4) 0.000 0.15(3) 0.000 O7 0.092(18) 0.065(14) 0.14(2) 0.000 0.024(16) 0.000 C1 0.071(7) 0.049(6) 0.065(7) 0.015(5) -0.020(6) 0.002(5) C2 0.054(6) 0.039(5) 0.092(9) 0.016(6) -0.006(6) 0.009(5) C3 0.080(8) 0.022(4) 0.105(10) 0.003(5) 0.013(7) 0.010(5) C4 0.089(9) 0.030(5) 0.074(8) -0.015(5) 0.008(6) -0.007(5) C5 0.097(10) 0.077(9) 0.074(9) -0.022(7) -0.026(8) -0.014(8) C6 0.139(14) 0.095(11) 0.054(7) -0.020(8) -0.035(8) -0.008(11) P1 0.0343(15) 0.0279(14) 0.0428(17) 0.000 0.0025(13) 0.000 F1 0.073(10) 0.58(6) 0.118(14) 0.000 -0.045(10) 0.000 F2 0.191(11) 0.043(4) 0.202(11) -0.021(6) 0.134(10) -0.015(6) F3 0.203(11) 0.037(4) 0.255(14) 0.010(6) 0.179(11) -0.001(5) F4 0.111(16) 0.70(8) 0.17(2) 0.000 -0.067(15) 0.000 P2 0.066(2) 0.067(3) 0.0375(19) 0.0072(18) -0.0003(17) -0.015(2) F5 0.072(5) 0.086(5) 0.078(5) 0.008(4) 0.000(4) -0.001(4) F6 0.085(5) 0.075(5) 0.058(4) 0.012(3) 0.009(3) -0.021(4) F7 0.085(5) 0.091(5) 0.054(4) -0.003(4) 0.000(3) -0.021(4) _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 O5 2.545(19) . ? Pb1 O6 2.57(3) . ? Pb1 O1 2.704(10) . ? Pb1 O3 2.731(7) . ? Pb1 O3 2.731(7) 4_565 ? Pb1 O4 2.733(11) . ? Pb1 O2 2.737(6) 4_565 ? Pb1 O2 2.737(6) . ? O1 C1 1.430(12) 4_565 ? O1 C1 1.430(12) . ? O2 C3 1.410(13) . ? O2 C2 1.429(13) . ? O3 C5 1.413(15) . ? O3 C4 1.456(14) . ? O4 C6 1.429(15) . ? O4 C6 1.429(15) 4_565 ? C1 C2 1.492(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.466(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.50(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? P1 F4 1.462(14) . ? P1 F1 1.455(12) . ? P1 F3 1.516(8) 4_565 ? P1 F3 1.516(8) . ? P1 F2 1.564(8) . ? P1 F2 1.564(8) 4_565 ? P2 F6 1.587(6) 3_657 ? P2 F6 1.587(6) . ? P2 F5 1.595(8) 3_657 ? P2 F5 1.595(8) . ? P2 F7 1.611(7) . ? P2 F7 1.611(7) 3_657 ? 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 O5 Pb1 O6 57.8(10) . . ? O5 Pb1 O1 65.5(5) . . ? O6 Pb1 O1 123.4(9) . . ? O5 Pb1 O3 100.0(3) . . ? O6 Pb1 O3 72.3(4) . . ? O1 Pb1 O3 119.92(17) . . ? O5 Pb1 O3 100.0(3) . 4_565 ? O6 Pb1 O3 72.3(4) . 4_565 ? O1 Pb1 O3 119.92(18) . 4_565 ? O3 Pb1 O3 120.0(3) . 4_565 ? O5 Pb1 O4 125.1(5) . . ? O6 Pb1 O4 67.3(9) . . ? O1 Pb1 O4 169.3(3) . . ? O3 Pb1 O4 61.08(18) . . ? O3 Pb1 O4 61.08(18) 4_565 . ? O5 Pb1 O2 79.8(3) . 4_565 ? O6 Pb1 O2 107.6(4) . 4_565 ? O1 Pb1 O2 59.96(15) . 4_565 ? O3 Pb1 O2 179.8(2) . 4_565 ? O3 Pb1 O2 60.1(2) 4_565 4_565 ? O4 Pb1 O2 119.07(15) . 4_565 ? O5 Pb1 O2 79.8(3) . . ? O6 Pb1 O2 107.6(4) . . ? O1 Pb1 O2 59.96(15) . . ? O3 Pb1 O2 60.1(2) . . ? O3 Pb1 O2 179.8(2) 4_565 . ? O4 Pb1 O2 119.07(15) . . ? O2 Pb1 O2 119.8(3) 4_565 . ? C1 O1 C1 112.0(12) 4_565 . ? C1 O1 Pb1 117.7(6) 4_565 . ? C1 O1 Pb1 117.7(6) . . ? C3 O2 C2 111.3(8) . . ? C3 O2 Pb1 114.5(6) . . ? C2 O2 Pb1 116.7(5) . . ? C5 O3 C4 112.3(10) . . ? C5 O3 Pb1 114.9(7) . . ? C4 O3 Pb1 117.7(6) . . ? C6 O4 C6 111.8(14) . 4_565 ? C6 O4 Pb1 116.0(8) . . ? C6 O4 Pb1 116.0(8) 4_565 . ? O1 C1 C2 106.7(9) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 107.0(8) . . ? O2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? O2 C3 C4 107.9(9) . . ? O2 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O3 C4 C3 108.5(9) . . ? O3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 108.6(12) . . ? O3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? O4 C6 C5 108.2(10) . . ? O4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? F4 P1 F1 174.9(14) . . ? F4 P1 F3 91.2(10) . 4_565 ? F1 P1 F3 92.5(9) . 4_565 ? F4 P1 F3 91.2(10) . . ? F1 P1 F3 92.5(9) . . ? F3 P1 F3 86.8(6) 4_565 . ? F4 P1 F2 88.0(10) . . ? F1 P1 F2 88.3(8) . . ? F3 P1 F2 179.0(8) 4_565 . ? F3 P1 F2 93.8(4) . . ? F4 P1 F2 88.0(10) . 4_565 ? F1 P1 F2 88.3(8) . 4_565 ? F3 P1 F2 93.8(4) 4_565 4_565 ? F3 P1 F2 179.0(8) . 4_565 ? F2 P1 F2 85.5(6) . 4_565 ? F6 P2 F6 180.0(4) 3_657 . ? F6 P2 F5 89.9(4) 3_657 3_657 ? F6 P2 F5 90.1(4) . 3_657 ? F6 P2 F5 90.1(4) 3_657 . ? F6 P2 F5 89.9(4) . . ? F5 P2 F5 180.000(2) 3_657 . ? F6 P2 F7 90.1(4) 3_657 . ? F6 P2 F7 89.9(4) . . ? F5 P2 F7 89.8(4) 3_657 . ? F5 P2 F7 90.2(4) . . ? F6 P2 F7 89.9(4) 3_657 3_657 ? F6 P2 F7 90.1(4) . 3_657 ? F5 P2 F7 90.2(4) 3_657 3_657 ? F5 P2 F7 89.8(4) . 3_657 ? F7 P2 F7 180.000(1) . 3_657 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 C1 C2 -169.4(7) 4_565 . . . ? Pb1 O1 C1 C2 49.5(11) . . . . ? C3 O2 C2 C1 -177.7(9) . . . . ? Pb1 O2 C2 C1 48.2(11) . . . . ? O1 C1 C2 O2 -62.2(12) . . . . ? C2 O2 C3 C4 168.6(10) . . . . ? Pb1 O2 C3 C4 -56.3(11) . . . . ? C5 O3 C4 C3 -175.0(11) . . . . ? Pb1 O3 C4 C3 -38.1(12) . . . . ? O2 C3 C4 O3 61.1(12) . . . . ? C4 O3 C5 C6 -171.1(11) . . . . ? Pb1 O3 C5 C6 50.7(13) . . . . ? C6 O4 C6 C5 -178.9(10) 4_565 . . . ? Pb1 O4 C6 C5 45.1(17) . . . . ? O3 C5 C6 O4 -63.0(17) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pb1 F2 2.881(9) . . ? O5 O7 2.825(34) . . ? O6 O7 2.506(36) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 5.488 _refine_diff_density_min -3.293 _refine_diff_density_rms 0.205 #===END OF CIF ============================================================== data_12paf127r _database_code_depnum_ccdc_archive 'CCDC 913970' #TrackingRef 'Pb_all1_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-12-03 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane-lead(II) bis-hexafluorophosphate ; # C12H24O4Se2 = [18]aneO4Se2 # 1,4,10,13-tetraoxa-7,16-diselena-cyclooctadecane # 1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane (iLab defaults) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 O4 Pb Se2 2+, 2(F6 P 1-) ' _chemical_formula_sum 'C12 H24 F12 O4 P2 Pb Se2' _chemical_formula_weight 887.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.012(4) _cell_length_b 12.949(5) _cell_length_c 16.105(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.402(7) _cell_angle_gamma 90.00 _cell_volume 2286.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8312 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 10.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.614 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9667 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2599 _reflns_number_gt 2435 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+8.2976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2599 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.0000 0.391388(17) 0.2500 0.01964(9) Uani 1 2 d S . . Se1 Se 0.27927(4) 0.34047(4) 0.23633(3) 0.02801(14) Uani 1 1 d . . . P1 P -0.00997(12) 0.19969(10) 0.42993(9) 0.0261(3) Uani 1 1 d . . . F1 F -0.0369(3) 0.3218(2) 0.4183(2) 0.0339(7) Uani 1 1 d . . . F2 F 0.1158(3) 0.2263(3) 0.4820(2) 0.0433(8) Uani 1 1 d . . . F3 F 0.0547(4) 0.2030(3) 0.3444(2) 0.0470(9) Uani 1 1 d . . . F4 F 0.0206(3) 0.0800(3) 0.4398(2) 0.0387(8) Uani 1 1 d . . . F5 F -0.1355(3) 0.1734(3) 0.3780(3) 0.0480(9) Uani 1 1 d . . . F6 F -0.0763(3) 0.1985(3) 0.5136(2) 0.0436(9) Uani 1 1 d . . . O1 O 0.1559(3) 0.4979(3) 0.3537(2) 0.0240(7) Uani 1 1 d . . . O2 O -0.0930(3) 0.5227(3) 0.3429(2) 0.0283(8) Uani 1 1 d . . . C1 C 0.3494(4) 0.4174(4) 0.3349(4) 0.0290(11) Uani 1 1 d . . . H1A H 0.4165 0.3762 0.3636 0.035 Uiso 1 1 calc R . . H1B H 0.3848 0.4827 0.3162 0.035 Uiso 1 1 calc R . . C2 C 0.2581(4) 0.4421(4) 0.3960(3) 0.0282(10) Uani 1 1 d . . . H2A H 0.2287 0.3774 0.4201 0.034 Uiso 1 1 calc R . . H2B H 0.2972 0.4847 0.4421 0.034 Uiso 1 1 calc R . . C3 C 0.1009(4) 0.5632(4) 0.4122(3) 0.0282(11) Uani 1 1 d . . . H3A H 0.1578 0.6193 0.4315 0.034 Uiso 1 1 calc R . . H3B H 0.0823 0.5223 0.4614 0.034 Uiso 1 1 calc R . . C4 C -0.0142(4) 0.6081(4) 0.3699(4) 0.0281(11) Uani 1 1 d . . . H4A H -0.0544 0.6527 0.4091 0.034 Uiso 1 1 calc R . . H4B H 0.0042 0.6503 0.3214 0.034 Uiso 1 1 calc R . . C5 C -0.2224(4) 0.5464(4) 0.3362(4) 0.0318(12) Uani 1 1 d . . . H5A H -0.2476 0.5765 0.2807 0.038 Uiso 1 1 calc R . . H5B H -0.2397 0.5974 0.3793 0.038 Uiso 1 1 calc R . . C6 C -0.2921(4) 0.4490(5) 0.3477(4) 0.0346(12) Uani 1 1 d . . . H6A H -0.3793 0.4670 0.3486 0.042 Uiso 1 1 calc R . . H6B H -0.2640 0.4199 0.4031 0.042 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 Pb1 0.01483(13) 0.01969(14) 0.02417(15) 0.000 0.00057(9) 0.000 Se1 0.0179(2) 0.0285(3) 0.0370(3) -0.0026(2) -0.0004(2) 0.00258(17) P1 0.0233(6) 0.0265(7) 0.0282(7) 0.0011(5) 0.0013(5) 0.0013(5) F1 0.0438(18) 0.0243(15) 0.0327(18) 0.0032(12) -0.0016(14) 0.0016(13) F2 0.0292(17) 0.047(2) 0.051(2) 0.0124(16) -0.0102(14) -0.0021(14) F3 0.060(2) 0.051(2) 0.032(2) 0.0093(16) 0.0166(17) 0.0216(17) F4 0.0408(18) 0.0312(17) 0.043(2) -0.0005(14) -0.0004(15) 0.0055(14) F5 0.0364(18) 0.0361(19) 0.068(3) 0.0046(17) -0.0160(17) -0.0039(14) F6 0.046(2) 0.0398(19) 0.048(2) 0.0064(16) 0.0183(17) 0.0062(15) O1 0.0176(15) 0.0290(18) 0.0247(18) -0.0020(14) -0.0006(13) 0.0009(13) O2 0.0150(15) 0.0276(18) 0.041(2) -0.0066(15) -0.0046(14) 0.0011(13) C1 0.017(2) 0.033(3) 0.035(3) 0.000(2) -0.006(2) 0.0013(19) C2 0.019(2) 0.037(3) 0.027(3) 0.003(2) -0.0051(19) -0.0011(19) C3 0.020(2) 0.035(3) 0.029(3) -0.007(2) -0.001(2) -0.0021(19) C4 0.020(2) 0.025(3) 0.039(3) -0.008(2) -0.001(2) -0.0009(17) C5 0.017(2) 0.034(3) 0.044(3) -0.012(2) 0.000(2) 0.0090(19) C6 0.018(2) 0.048(3) 0.039(3) -0.003(3) 0.006(2) -0.001(2) _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 O2 2.543(4) 2 ? Pb1 O2 2.543(4) . ? Pb1 O1 2.664(3) . ? Pb1 O1 2.664(3) 2 ? Pb1 Se1 3.1731(12) 2 ? Pb1 Se1 3.1731(12) . ? Se1 C6 1.966(6) 2 ? Se1 C1 1.969(5) . ? P1 F5 1.584(4) . ? P1 F2 1.588(3) . ? P1 F4 1.591(3) . ? P1 F6 1.593(4) . ? P1 F3 1.609(4) . ? P1 F1 1.617(3) . ? O1 C3 1.442(6) . ? O1 C2 1.452(6) . ? O2 C4 1.447(6) . ? O2 C5 1.452(5) . ? C1 C2 1.507(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.498(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.497(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 Se1 1.966(6) 2 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 O2 Pb1 O2 96.11(17) 2 . ? O2 Pb1 O1 75.60(11) 2 . ? O2 Pb1 O1 63.68(10) . . ? O2 Pb1 O1 63.68(10) 2 2 ? O2 Pb1 O1 75.60(11) . 2 ? O1 Pb1 O1 117.65(15) . 2 ? O2 Pb1 Se1 128.78(7) 2 2 ? O2 Pb1 Se1 69.60(7) . 2 ? O1 Pb1 Se1 129.48(7) . 2 ? O1 Pb1 Se1 65.13(7) 2 2 ? O2 Pb1 Se1 69.60(7) 2 . ? O2 Pb1 Se1 128.78(7) . . ? O1 Pb1 Se1 65.13(7) . . ? O1 Pb1 Se1 129.48(7) 2 . ? Se1 Pb1 Se1 156.02(2) 2 . ? C6 Se1 C1 98.4(2) 2 . ? C6 Se1 Pb1 91.86(14) 2 . ? C1 Se1 Pb1 98.52(14) . . ? F5 P1 F2 179.9(3) . . ? F5 P1 F4 90.52(19) . . ? F2 P1 F4 89.56(19) . . ? F5 P1 F6 89.9(2) . . ? F2 P1 F6 90.1(2) . . ? F4 P1 F6 90.87(19) . . ? F5 P1 F3 89.3(2) . . ? F2 P1 F3 90.7(2) . . ? F4 P1 F3 90.29(19) . . ? F6 P1 F3 178.6(2) . . ? F5 P1 F1 90.47(18) . . ? F2 P1 F1 89.45(19) . . ? F4 P1 F1 178.06(19) . . ? F6 P1 F1 90.81(18) . . ? F3 P1 F1 88.05(19) . . ? C3 O1 C2 109.8(4) . . ? C3 O1 Pb1 115.3(3) . . ? C2 O1 Pb1 117.5(3) . . ? C4 O2 C5 114.7(4) . . ? C4 O2 Pb1 115.1(3) . . ? C5 O2 Pb1 123.0(3) . . ? C2 C1 Se1 113.5(3) . . ? C2 C1 H1A 108.9 . . ? Se1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? Se1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O1 C2 C1 109.5(4) . . ? O1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O1 C3 C4 108.6(4) . . ? O1 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O1 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 107.3(4) . . ? O2 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O2 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O2 C5 C6 108.9(4) . . ? O2 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O2 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 C6 Se1 116.5(4) . 2 ? C5 C6 H6A 108.2 . . ? Se1 C6 H6A 108.2 2 . ? C5 C6 H6B 108.2 . . ? Se1 C6 H6B 108.2 2 . ? H6A C6 H6B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Se1 C1 C2 111.8(4) 2 . . . ? Pb1 Se1 C1 C2 18.6(4) . . . . ? C3 O1 C2 C1 -152.5(4) . . . . ? Pb1 O1 C2 C1 73.1(4) . . . . ? Se1 C1 C2 O1 -55.6(5) . . . . ? C2 O1 C3 C4 -172.1(4) . . . . ? Pb1 O1 C3 C4 -36.5(5) . . . . ? C5 O2 C4 C3 153.2(4) . . . . ? Pb1 O2 C4 C3 -55.6(5) . . . . ? O1 C3 C4 O2 59.2(5) . . . . ? C4 O2 C5 C6 -153.8(5) . . . . ? Pb1 O2 C5 C6 57.5(6) . . . . ? O2 C5 C6 Se1 -63.5(6) . . . 2 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F5 SE1 3.167(4) . 2 ? F1 O2 2.911(5) . . ? F3 Pb1 2.908(4) . . ? F1 Pb1 2.920(3) . . ? F4 F4 2.902(7) . 5_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.665 _refine_diff_density_min -1.455 _refine_diff_density_rms 0.167 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================