# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Manfred Scheer' _publ_contact_author_email MANFRED.SCHEER@CHEMIE.UNI-REGENSBURG.DE _publ_section_title ; 1,2,3-Triphosphole derivatives as reactive intermediates ; loop_ _publ_author_name 'Manfred Scheer' 'Gabor Balazs' 'Christian Kuntz' 'Markus Stubenhofer' 'Manfred Zabel' # Attachment 'ms11-final.cif' # CIF-file generated for Scheer/Stubenhofer R = 0.04 #============================================================================== data_ms11 _database_code_depnum_ccdc_archive 'CCDC 714100' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H10 As2 O20 P4 W4, C7 H8' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C39 H18 As2 O20 P4 W4' _chemical_formula_iupac ? _chemical_formula_weight 1815.61 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.2685(5) _cell_length_b 12.4386(5) _cell_length_c 18.7689(7) _cell_angle_alpha 96.500(3) _cell_angle_beta 102.035(4) _cell_angle_gamma 115.791(4) _cell_volume 2453.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 7899 _cell_measurement_theta_min 2.4681 _cell_measurement_theta_max 62.0395 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.214 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.196 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.458 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 20.288 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.019 _exptl_absorpt_correction_T_max 0.033 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Analytical absorption correction using crystal faces, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -29.00 25.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -1.2571 45.0000 90.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega -29.00 25.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -1.2571 45.0000 210.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 3 omega 24.00 77.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 2.5071 45.0000 270.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 4 omega 25.00 77.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 2.5071 45.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 5 omega -158.00 -105.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 -45.0000 0.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 6 omega -117.00 -61.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 115.0000 254.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 7 omega -109.00 -56.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 -45.0000 330.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 8 omega -111.00 -57.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 45.0000 30.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 9 omega -111.00 -8.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 45.0000 150.0000 0.0000 0.0000 103 #__ type_ start__ end____ width___ exp.time_ 10 omega -114.00 -59.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 108.0000 19.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 11 omega -55.00 -6.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 0.0000 180.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 12 omega -117.00 -4.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 77.0000 240.0000 0.0000 0.0000 113 #__ type_ start__ end____ width___ exp.time_ 13 omega 106.00 159.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 45.0000 60.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 14 omega 74.00 111.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -77.0000 240.0000 0.0000 0.0000 37 #__ type_ start__ end____ width___ exp.time_ 15 omega 57.00 135.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 45.0000 210.0000 0.0000 0.0000 78 #__ type_ start__ end____ width___ exp.time_ 16 omega 64.00 113.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -77.0000 0.0000 0.0000 0.0000 49 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 13743 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 62.18 _diffrn_reflns_theta_full 62.18 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 7523 # number of observed reflections (> n sig(I)) _reflns_number_gt 6360 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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 cavity in the crystal structure is slightly larger than necessary for a toluene molecule which causes the slight spinning of the solvent molecule. This leads to the somewhat lager e.s.d.s. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 7523 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.834 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.203 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags W1 W Uani 0.20769(4) -0.24296(3) 0.64053(2) 1.000 0.0260(1) . . W2 W Uani 0.66023(4) 0.32444(3) 0.97620(2) 1.000 0.0273(1) . . W3 W Uani 0.83552(3) 0.35000(3) 0.73204(2) 1.000 0.0239(1) . . W4 W Uani 0.29064(3) 0.21184(3) 0.49886(2) 1.000 0.0256(1) . . As1 As Uani 0.36612(9) 0.06849(10) 0.80715(5) 1.000 0.0385(3) . . As2 As Uani 0.48275(8) 0.10045(8) 0.64750(4) 1.000 0.0234(3) . . P1 P Uani 0.39465(19) -0.04776(18) 0.71455(10) 1.000 0.0232(6) . . P3 P Uani 0.5836(2) 0.18637(18) 0.84911(10) 1.000 0.0242(6) . . P4 P Uani 0.61927(19) 0.26683(18) 0.74871(10) 1.000 0.0229(6) . . P6 P Uani 0.3335(2) 0.17086(19) 0.62517(11) 1.000 0.0259(6) . . O1 O Uani 0.0307(7) -0.1206(7) 0.6446(4) 1.000 0.057(3) . . O2 O Uani 0.2048(8) -0.3028(7) 0.8009(4) 1.000 0.060(3) . . O3 O Uani 0.3389(7) -0.4039(6) 0.5991(4) 1.000 0.053(3) . . O4 O Uani 0.2280(7) -0.1599(6) 0.4874(3) 1.000 0.042(2) . . O5 O Uani -0.0486(7) -0.4846(6) 0.5638(4) 1.000 0.053(2) . . O6 O Uani 0.8672(7) 0.5539(6) 0.9363(4) 1.000 0.053(2) . . O7 O Uani 0.8735(7) 0.2559(7) 1.0491(4) 1.000 0.055(3) . . O8 O Uani 0.4732(8) 0.1068(7) 1.0350(5) 1.000 0.061(3) . . O9 O Uani 0.4469(6) 0.4036(6) 0.9249(3) 1.000 0.044(2) . . O10 O Uani 0.7486(7) 0.4991(6) 1.1345(3) 1.000 0.044(2) . . O11 O Uani 0.7884(6) 0.0759(6) 0.6796(3) 1.000 0.038(2) . . O12 O Uani 0.9803(6) 0.3726(6) 0.8992(3) 1.000 0.047(2) . . O13 O Uani 0.9094(7) 0.6328(6) 0.7765(4) 1.000 0.053(3) . . O14 O Uani 0.6935(6) 0.3484(6) 0.5685(3) 1.000 0.044(2) . . O15 O Uani 1.0915(6) 0.4220(6) 0.6908(3) 1.000 0.0378(19) . . O16 O Uani 0.4701(6) 0.1214(6) 0.4447(4) 1.000 0.047(2) . . O17 O Uani 0.5227(7) 0.4765(6) 0.5773(3) 1.000 0.047(2) . . O18 O Uani 0.1037(7) 0.3117(6) 0.5312(4) 1.000 0.047(2) . . O19 O Uani 0.0517(6) -0.0519(6) 0.4325(4) 1.000 0.045(2) . . O20 O Uani 0.2457(7) 0.2775(6) 0.3419(3) 1.000 0.049(2) . . C1 C Uani 0.5437(8) -0.0378(7) 0.7679(4) 1.000 0.025(2) . . C2 C Uani 0.6251(7) 0.0657(7) 0.8268(4) 1.000 0.025(2) . . C3 C Uani 0.7418(7) 0.0761(8) 0.8659(4) 1.000 0.026(3) . . C4 C Uani 0.7741(8) -0.0136(8) 0.8468(4) 1.000 0.029(3) . . C5 C Uani 0.6938(9) -0.1169(8) 0.7896(5) 1.000 0.035(3) . . C6 C Uani 0.5778(8) -0.1283(7) 0.7504(4) 1.000 0.027(3) . . C7 C Uani 0.4092(8) 0.3090(7) 0.7016(4) 1.000 0.029(3) . . C8 C Uani 0.5348(8) 0.3573(7) 0.7455(4) 1.000 0.026(3) . . C9 C Uani 0.5950(9) 0.4761(8) 0.7901(4) 1.000 0.032(3) . . C10 C Uani 0.5319(9) 0.5444(8) 0.7941(5) 1.000 0.035(3) . . C11 C Uani 0.4068(9) 0.4941(8) 0.7537(5) 1.000 0.035(3) . . C12 C Uani 0.3459(9) 0.3780(8) 0.7070(4) 1.000 0.033(3) . . C13 C Uani 0.0956(9) -0.1619(8) 0.6465(5) 1.000 0.036(3) . . C14 C Uani 0.2066(9) -0.2832(8) 0.7426(5) 1.000 0.039(3) . . C15 C Uani 0.2991(10) -0.3430(8) 0.6169(5) 1.000 0.038(3) . . C16 C Uani 0.2204(9) -0.1910(8) 0.5422(5) 1.000 0.035(3) . . C17 C Uani 0.0468(9) -0.3981(9) 0.5906(5) 1.000 0.036(3) . . C18 C Uani 0.7915(9) 0.4707(9) 0.9488(5) 1.000 0.039(3) . . C19 C Uani 0.7965(9) 0.2780(8) 1.0207(5) 1.000 0.036(3) . . C20 C Uani 0.5377(9) 0.1831(9) 1.0117(5) 1.000 0.037(3) . . C21 C Uani 0.5208(9) 0.3725(8) 0.9421(5) 1.000 0.034(3) . . C22 C Uani 0.7127(9) 0.4356(8) 1.0786(5) 1.000 0.033(3) . . C23 C Uani 0.8033(7) 0.1724(8) 0.6987(4) 1.000 0.030(3) . . C24 C Uani 0.9253(9) 0.3617(8) 0.8388(5) 1.000 0.035(3) . . C25 C Uani 0.8812(9) 0.5307(9) 0.7623(5) 1.000 0.035(3) . . C26 C Uani 0.7477(8) 0.3486(7) 0.6273(5) 1.000 0.033(3) . . C27 C Uani 0.9991(8) 0.3984(7) 0.7063(4) 1.000 0.027(2) . . C28 C Uani 0.4078(8) 0.1526(8) 0.4657(4) 1.000 0.029(3) . . C29 C Uani 0.4421(9) 0.3824(8) 0.5476(5) 1.000 0.034(3) . . C30 C Uani 0.1708(9) 0.2756(8) 0.5215(5) 1.000 0.032(3) . . C31 C Uani 0.1386(9) 0.0418(8) 0.4558(5) 1.000 0.031(3) . . C32 C Uani 0.2621(9) 0.2535(8) 0.3989(5) 1.000 0.034(3) . . C33 C Uani 0.1663(12) 0.1467(9) 0.9406(7) 1.000 0.054(4) . . C34 C Uani 0.1387(14) 0.1914(18) 0.8823(11) 1.000 0.096(8) . . C35 C Uani 0.0802(17) 0.126(3) 0.8122(11) 1.000 0.144(14) . . C36 C Uani 0.0365(18) -0.002(3) 0.8009(12) 1.000 0.183(14) . . C37 C Uani 0.0587(14) -0.0499(16) 0.8609(14) 1.000 0.122(8) . . C38 C Uani 0.1206(15) 0.0189(12) 0.9297(10) 1.000 0.089(6) . . C39 C Uani 0.2358(16) 0.2267(16) 1.0164(9) 1.000 0.101(7) . . H1 H Uiso 0.31090 0.00100 0.86050 1.000 0.0310 . . H2 H Uiso 0.256(8) 0.112(8) 0.655(5) 1.000 0.0310 . . H3 H Uiso 0.52150 -0.19880 0.71130 1.000 0.0330 calc R H4 H Uiso 0.71700 -0.17860 0.77740 1.000 0.0410 calc R H5 H Uiso 0.85360 -0.00460 0.87340 1.000 0.0340 calc R H6 H Uiso 0.79840 0.14550 0.90570 1.000 0.0310 calc R H7 H Uiso 0.26020 0.34500 0.67820 1.000 0.0400 calc R H8 H Uiso 0.36210 0.53940 0.75800 1.000 0.0420 calc R H9 H Uiso 0.57460 0.62540 0.82450 1.000 0.0420 calc R H10 H Uiso 0.68120 0.51080 0.81830 1.000 0.0380 calc R H34 H Uiso 0.16270 0.27640 0.89140 1.000 0.1150 calc R H35 H Uiso 0.06840 0.16280 0.77180 1.000 0.1720 calc R H36 H Uiso -0.00780 -0.05370 0.75210 1.000 0.2220 calc R H37 H Uiso 0.02840 -0.13600 0.85290 1.000 0.1470 calc R H38 H Uiso 0.13400 -0.01690 0.97060 1.000 0.1080 calc R H39A H Uiso 0.32460 0.24500 1.02780 1.000 0.1520 calc R H39B H Uiso 0.19830 0.18490 1.05300 1.000 0.1520 calc R H39C H Uiso 0.23050 0.30340 1.01860 1.000 0.1520 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 W1 0.0224(2) 0.0241(2) 0.0215(2) 0.0061(2) 0.0011(2) 0.0043(2) W2 0.0286(2) 0.0289(2) 0.0208(2) 0.0056(2) 0.0028(2) 0.0123(2) W3 0.0181(2) 0.0241(2) 0.0219(2) 0.0054(2) 0.0019(2) 0.0051(2) W4 0.0216(2) 0.0248(2) 0.0234(2) 0.0067(2) -0.0009(2) 0.0077(2) As1 0.0219(5) 0.0416(6) 0.0388(5) -0.0048(4) 0.0072(4) 0.0075(5) As2 0.0215(5) 0.0230(4) 0.0213(4) 0.0069(3) 0.0019(4) 0.0081(4) P1 0.0193(10) 0.0227(10) 0.0216(9) 0.0069(8) 0.0016(8) 0.0062(9) P3 0.0226(11) 0.0256(10) 0.0209(9) 0.0069(8) 0.0016(8) 0.0100(9) P4 0.0197(10) 0.0235(10) 0.0211(9) 0.0071(8) 0.0018(8) 0.0077(9) P6 0.0197(10) 0.0288(11) 0.0254(9) 0.0096(8) 0.0022(9) 0.0093(9) O1 0.031(4) 0.079(5) 0.055(4) -0.006(4) -0.003(3) 0.033(4) O2 0.073(6) 0.059(5) 0.028(3) 0.016(3) 0.009(4) 0.015(4) O3 0.072(5) 0.045(4) 0.046(4) 0.002(3) 0.000(4) 0.041(4) O4 0.053(4) 0.047(4) 0.036(3) 0.017(3) 0.013(3) 0.030(4) O5 0.036(4) 0.045(4) 0.039(3) 0.007(3) 0.000(3) -0.010(4) O6 0.057(5) 0.037(4) 0.032(3) 0.008(3) 0.006(3) -0.003(4) O7 0.054(5) 0.069(5) 0.040(4) 0.001(3) -0.006(4) 0.038(4) O8 0.067(5) 0.046(4) 0.072(5) 0.031(4) 0.036(5) 0.018(4) O9 0.043(4) 0.057(4) 0.038(3) 0.014(3) 0.008(3) 0.031(4) O10 0.052(4) 0.048(4) 0.024(3) -0.002(3) 0.004(3) 0.023(4) O11 0.042(4) 0.032(4) 0.039(3) 0.008(3) 0.013(3) 0.017(3) O12 0.029(4) 0.067(5) 0.022(3) 0.008(3) -0.008(3) 0.011(3) O13 0.054(5) 0.026(4) 0.060(4) 0.001(3) 0.011(4) 0.008(3) O14 0.032(4) 0.056(4) 0.030(3) 0.017(3) -0.004(3) 0.014(3) O15 0.023(3) 0.046(4) 0.038(3) 0.013(3) 0.009(3) 0.010(3) O16 0.036(4) 0.056(4) 0.043(4) 0.005(3) 0.009(3) 0.019(4) O17 0.043(4) 0.036(4) 0.034(3) 0.007(3) -0.003(3) 0.001(3) O18 0.045(4) 0.052(4) 0.047(4) 0.004(3) 0.002(3) 0.032(4) O19 0.040(4) 0.034(4) 0.045(4) -0.002(3) 0.008(3) 0.009(3) O20 0.054(5) 0.047(4) 0.031(3) 0.014(3) 0.003(3) 0.015(4) C1 0.024(4) 0.030(4) 0.025(4) 0.015(3) 0.008(3) 0.014(4) C2 0.017(4) 0.026(4) 0.023(4) 0.011(3) 0.002(3) 0.004(3) C3 0.017(4) 0.033(5) 0.022(4) 0.006(3) 0.002(3) 0.008(4) C4 0.026(5) 0.039(5) 0.023(4) 0.014(4) 0.007(4) 0.016(4) C5 0.039(5) 0.035(5) 0.031(4) 0.015(4) 0.011(4) 0.016(4) C6 0.026(5) 0.027(4) 0.027(4) 0.010(3) 0.005(4) 0.012(4) C7 0.026(5) 0.028(4) 0.028(4) 0.004(3) 0.004(4) 0.010(4) C8 0.028(5) 0.027(4) 0.023(4) 0.009(3) 0.008(4) 0.012(4) C9 0.037(5) 0.036(5) 0.023(4) 0.008(4) 0.008(4) 0.017(4) C10 0.047(6) 0.029(5) 0.028(4) 0.008(4) 0.007(4) 0.018(5) C11 0.053(6) 0.042(5) 0.029(4) 0.016(4) 0.015(4) 0.035(5) C12 0.042(5) 0.045(5) 0.024(4) 0.012(4) 0.010(4) 0.030(5) C13 0.025(5) 0.037(5) 0.025(4) -0.008(4) -0.006(4) 0.006(4) C14 0.035(5) 0.028(5) 0.037(5) -0.005(4) 0.002(4) 0.006(4) C15 0.046(6) 0.027(5) 0.029(4) 0.008(4) -0.001(4) 0.012(5) C16 0.045(6) 0.036(5) 0.027(4) 0.005(4) 0.003(4) 0.025(5) C17 0.032(5) 0.039(5) 0.028(4) 0.012(4) 0.006(4) 0.008(5) C18 0.034(6) 0.041(6) 0.023(4) 0.003(4) -0.005(4) 0.008(5) C19 0.038(5) 0.045(5) 0.022(4) 0.002(4) -0.005(4) 0.024(5) C20 0.037(5) 0.033(5) 0.031(4) 0.006(4) 0.006(4) 0.010(5) C21 0.033(5) 0.037(5) 0.025(4) 0.007(4) 0.001(4) 0.013(4) C22 0.042(6) 0.037(5) 0.025(4) 0.013(4) 0.013(4) 0.021(5) C23 0.012(4) 0.038(5) 0.028(4) 0.005(4) -0.003(3) 0.007(4) C24 0.033(5) 0.024(4) 0.039(5) 0.008(4) 0.009(5) 0.005(4) C25 0.034(5) 0.035(5) 0.031(4) 0.005(4) 0.003(4) 0.015(4) C26 0.027(5) 0.020(4) 0.035(5) 0.008(4) 0.008(4) -0.003(4) C27 0.015(4) 0.027(4) 0.022(4) 0.009(3) -0.003(4) -0.001(4) C28 0.020(4) 0.046(5) 0.025(4) 0.007(4) 0.005(4) 0.019(4) C29 0.036(5) 0.034(5) 0.026(4) 0.007(4) -0.002(4) 0.017(5) C30 0.030(5) 0.031(5) 0.031(4) 0.004(4) 0.002(4) 0.014(4) C31 0.029(5) 0.027(5) 0.034(4) 0.003(4) 0.004(4) 0.014(4) C32 0.034(5) 0.037(5) 0.028(4) 0.002(4) 0.008(4) 0.015(4) C33 0.062(8) 0.030(5) 0.064(7) 0.001(5) 0.022(6) 0.016(5) C34 0.053(9) 0.134(14) 0.138(16) 0.078(13) 0.049(11) 0.057(10) C35 0.047(11) 0.32(4) 0.067(12) 0.037(17) 0.012(10) 0.091(18) C36 0.036(10) 0.34(4) 0.077(12) -0.12(2) -0.016(10) 0.060(18) C37 0.042(9) 0.094(12) 0.175(19) -0.083(14) 0.017(11) 0.017(8) C38 0.091(11) 0.045(7) 0.123(13) 0.007(8) 0.018(10) 0.033(8) C39 0.093(12) 0.105(12) 0.085(10) -0.012(9) 0.033(9) 0.033(10) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 P1 2.479(2) . . yes W1 C13 2.041(12) . . yes W1 C14 2.035(9) . . yes W1 C15 2.074(12) . . yes W1 C16 2.037(9) . . yes W1 C17 2.001(10) . . yes W2 P3 2.5011(19) . . yes W2 C18 2.043(11) . . yes W2 C19 2.048(11) . . yes W2 C20 2.044(11) . . yes W2 C21 2.053(12) . . yes W2 C22 2.032(9) . . yes W3 P4 2.498(3) . . yes W3 C23 2.062(9) . . yes W3 C24 2.031(9) . . yes W3 C25 2.042(10) . . yes W3 C26 2.029(9) . . yes W3 C27 2.011(10) . . yes W4 P6 2.479(2) . . yes W4 C28 2.046(10) . . yes W4 C29 2.052(10) . . yes W4 C30 2.042(12) . . yes W4 C31 2.039(10) . . yes W4 C32 2.004(9) . . yes As1 P1 2.315(2) . . yes As1 P3 2.312(3) . . yes As2 P1 2.347(2) . . yes As2 P4 2.337(2) . . yes As2 P6 2.335(3) . . yes As1 H1 1.4600 . . no P1 C1 1.837(10) . . yes P3 P4 2.266(3) . . yes P3 C2 1.816(9) . . yes P4 C8 1.830(10) . . yes P6 C7 1.836(8) . . yes P6 H2 1.21(10) . . no O1 C13 1.117(15) . . yes O2 C14 1.150(12) . . yes O3 C15 1.121(15) . . yes O4 C16 1.147(11) . . yes O5 C17 1.148(13) . . yes O6 C18 1.139(13) . . yes O7 C19 1.141(14) . . yes O8 C20 1.142(14) . . yes O9 C21 1.135(14) . . yes O10 C22 1.112(11) . . yes O11 C23 1.135(11) . . yes O12 C24 1.151(11) . . yes O13 C25 1.143(13) . . yes O14 C26 1.163(11) . . yes O15 C27 1.150(13) . . yes O16 C28 1.113(13) . . yes O17 C29 1.129(12) . . yes O18 C30 1.131(15) . . yes O19 C31 1.138(12) . . yes O20 C32 1.144(11) . . yes C1 C6 1.391(13) . . no C1 C2 1.406(11) . . no C2 C3 1.409(13) . . no C3 C4 1.373(14) . . no C4 C5 1.385(12) . . no C5 C6 1.397(15) . . no C7 C12 1.394(15) . . no C7 C8 1.403(13) . . no C8 C9 1.394(12) . . no C9 C10 1.382(16) . . no C10 C11 1.376(16) . . no C11 C12 1.383(12) . . no C3 H6 0.9500 . . no C4 H5 0.9500 . . no C5 H4 0.9500 . . no C6 H3 0.9500 . . no C9 H10 0.9500 . . no C10 H9 0.9500 . . no C11 H8 0.9500 . . no C12 H7 0.9500 . . no C33 C34 1.33(2) . . no C33 C38 1.409(18) . . no C33 C39 1.48(2) . . no C34 C35 1.33(3) . . no C35 C36 1.41(5) . . no C36 C37 1.37(4) . . no C37 C38 1.32(3) . . no C34 H34 0.9500 . . no C35 H35 0.9500 . . no C36 H36 0.9500 . . no C37 H37 0.9500 . . no C38 H38 0.9500 . . no C39 H39A 0.9800 . . no C39 H39B 0.9800 . . no C39 H39C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 W1 C13 89.4(3) . . . yes P1 W1 C14 83.5(3) . . . yes P1 W1 C15 99.0(3) . . . yes P1 W1 C16 92.3(3) . . . yes P1 W1 C17 172.9(3) . . . yes C13 W1 C14 93.2(4) . . . yes C13 W1 C15 170.2(4) . . . yes C13 W1 C16 87.0(4) . . . yes C13 W1 C17 86.0(4) . . . yes C14 W1 C15 92.8(4) . . . yes C14 W1 C16 175.8(4) . . . yes C14 W1 C17 91.3(4) . . . yes C15 W1 C16 87.6(4) . . . yes C15 W1 C17 86.1(4) . . . yes C16 W1 C17 92.9(4) . . . yes P3 W2 C18 94.2(3) . . . yes P3 W2 C19 96.3(3) . . . yes P3 W2 C20 89.6(3) . . . yes P3 W2 C21 88.5(3) . . . yes P3 W2 C22 176.8(3) . . . yes C18 W2 C19 90.2(4) . . . yes C18 W2 C20 175.7(4) . . . yes C18 W2 C21 92.8(4) . . . yes C18 W2 C22 87.3(4) . . . yes C19 W2 C20 87.3(4) . . . yes C19 W2 C21 174.2(4) . . . yes C19 W2 C22 86.5(4) . . . yes C20 W2 C21 89.4(4) . . . yes C20 W2 C22 89.0(4) . . . yes C21 W2 C22 88.7(4) . . . yes P4 W3 C23 88.9(3) . . . yes P4 W3 C24 95.8(3) . . . yes P4 W3 C25 95.9(3) . . . yes P4 W3 C26 84.2(3) . . . yes P4 W3 C27 172.3(2) . . . yes C23 W3 C24 91.5(3) . . . yes C23 W3 C25 175.1(4) . . . yes C23 W3 C26 91.9(3) . . . yes C23 W3 C27 85.1(4) . . . yes C24 W3 C25 88.8(4) . . . yes C24 W3 C26 176.6(4) . . . yes C24 W3 C27 89.2(4) . . . yes C25 W3 C26 87.8(4) . . . yes C25 W3 C27 90.0(4) . . . yes C26 W3 C27 91.1(4) . . . yes P6 W4 C28 93.8(2) . . . yes P6 W4 C29 84.9(3) . . . yes P6 W4 C30 92.1(3) . . . yes P6 W4 C31 92.5(3) . . . yes P6 W4 C32 177.2(3) . . . yes C28 W4 C29 90.0(4) . . . yes C28 W4 C30 174.1(3) . . . yes C28 W4 C31 91.5(4) . . . yes C28 W4 C32 86.6(4) . . . yes C29 W4 C30 90.2(4) . . . yes C29 W4 C31 177.0(4) . . . yes C29 W4 C32 92.4(4) . . . yes C30 W4 C31 88.6(4) . . . yes C30 W4 C32 87.5(4) . . . yes C31 W4 C32 90.3(4) . . . yes P1 As1 P3 87.57(9) . . . yes P1 As2 P4 98.68(7) . . . yes P1 As2 P6 101.00(9) . . . yes P4 As2 P6 92.71(9) . . . yes P3 As1 H1 114.00 . . . no P1 As1 H1 114.00 . . . no W1 P1 C1 123.7(3) . . . yes As1 P1 As2 99.96(9) . . . yes As1 P1 C1 98.5(3) . . . yes As2 P1 C1 96.9(3) . . . yes W1 P1 As1 117.09(11) . . . yes W1 P1 As2 116.21(8) . . . yes W2 P3 P4 120.23(10) . . . yes W2 P3 As1 113.23(10) . . . yes As1 P3 C2 98.2(3) . . . yes P4 P3 C2 96.4(3) . . . yes W2 P3 C2 124.1(3) . . . yes As1 P3 P4 100.00(10) . . . yes W3 P4 C8 121.5(3) . . . yes W3 P4 As2 107.51(9) . . . yes W3 P4 P3 119.20(11) . . . yes P3 P4 C8 102.1(3) . . . yes As2 P4 C8 100.7(3) . . . yes As2 P4 P3 102.96(10) . . . yes W4 P6 C7 113.7(3) . . . yes W4 P6 As2 113.60(10) . . . yes As2 P6 C7 100.6(3) . . . yes W4 P6 H2 127(5) . . . no C7 P6 H2 94(4) . . . no As2 P6 H2 104(5) . . . no P1 C1 C6 121.6(6) . . . yes P1 C1 C2 118.3(7) . . . yes C2 C1 C6 120.1(9) . . . no P3 C2 C1 120.6(7) . . . yes P3 C2 C3 120.8(6) . . . yes C1 C2 C3 118.5(8) . . . no C2 C3 C4 120.4(8) . . . no C3 C4 C5 121.7(9) . . . no C4 C5 C6 118.5(9) . . . no C1 C6 C5 120.9(8) . . . no C8 C7 C12 119.3(7) . . . no P6 C7 C8 122.2(7) . . . yes P6 C7 C12 117.6(7) . . . yes C7 C8 C9 118.8(9) . . . no P4 C8 C7 121.9(6) . . . yes P4 C8 C9 119.2(8) . . . yes C8 C9 C10 121.4(10) . . . no C9 C10 C11 119.5(9) . . . no C10 C11 C12 120.4(10) . . . no C7 C12 C11 120.6(10) . . . no W1 C13 O1 175.2(8) . . . yes W1 C14 O2 177.6(10) . . . yes W1 C15 O3 173.8(9) . . . yes W1 C16 O4 178.9(9) . . . yes W1 C17 O5 176.5(10) . . . yes W2 C18 O6 177.4(8) . . . yes W2 C19 O7 176.3(8) . . . yes W2 C20 O8 176.6(8) . . . yes W2 C21 O9 177.3(7) . . . yes W2 C22 O10 175.9(10) . . . yes W3 C23 O11 178.1(8) . . . yes W3 C24 O12 177.2(8) . . . yes W3 C25 O13 176.7(9) . . . yes W3 C26 O14 177.1(9) . . . yes W3 C27 O15 177.7(7) . . . yes W4 C28 O16 177.0(7) . . . yes W4 C29 O17 176.5(9) . . . yes W4 C30 O18 177.2(8) . . . yes W4 C31 O19 178.1(10) . . . yes W4 C32 O20 179.8(14) . . . yes C2 C3 H6 120.00 . . . no C4 C3 H6 120.00 . . . no C3 C4 H5 119.00 . . . no C5 C4 H5 119.00 . . . no C4 C5 H4 121.00 . . . no C6 C5 H4 121.00 . . . no C1 C6 H3 120.00 . . . no C5 C6 H3 120.00 . . . no C8 C9 H10 119.00 . . . no C10 C9 H10 119.00 . . . no C9 C10 H9 120.00 . . . no C11 C10 H9 120.00 . . . no C10 C11 H8 120.00 . . . no C12 C11 H8 120.00 . . . no C7 C12 H7 120.00 . . . no C11 C12 H7 120.00 . . . no C34 C33 C38 118.5(14) . . . no C34 C33 C39 121.4(14) . . . no C38 C33 C39 119.9(13) . . . no C33 C34 C35 125(2) . . . no C34 C35 C36 116(2) . . . no C35 C36 C37 119(2) . . . no C36 C37 C38 123(2) . . . no C33 C38 C37 118.2(16) . . . no C33 C34 H34 118.00 . . . no C35 C34 H34 118.00 . . . no C34 C35 H35 122.00 . . . no C36 C35 H35 122.00 . . . no C35 C36 H36 120.00 . . . no C37 C36 H36 121.00 . . . no C36 C37 H37 119.00 . . . no C38 C37 H37 119.00 . . . no C33 C38 H38 121.00 . . . no C37 C38 H38 121.00 . . . no C33 C39 H39A 109.00 . . . no C33 C39 H39B 109.00 . . . no C33 C39 H39C 109.00 . . . no H39A C39 H39B 110.00 . . . no H39A C39 H39C 110.00 . . . no H39B C39 H39C 109.00 . . . no 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 C13 W1 P1 As1 35.6(3) . . . . no C14 W1 P1 As1 -57.7(3) . . . . no C15 W1 P1 As1 -149.5(3) . . . . no C16 W1 P1 As1 122.6(3) . . . . no C13 W1 P1 As2 -82.3(3) . . . . no C14 W1 P1 As2 -175.6(3) . . . . no C15 W1 P1 As2 92.6(3) . . . . no C16 W1 P1 As2 4.6(3) . . . . no C13 W1 P1 C1 158.4(4) . . . . no C14 W1 P1 C1 65.1(5) . . . . no C15 W1 P1 C1 -26.7(4) . . . . no C16 W1 P1 C1 -114.7(5) . . . . no C20 W2 P3 P4 161.9(4) . . . . no C21 W2 P3 P4 72.5(3) . . . . no C18 W2 P3 C2 103.2(5) . . . . no C19 W2 P3 C2 12.6(5) . . . . no C20 W2 P3 C2 -74.6(5) . . . . no C21 W2 P3 C2 -164.1(4) . . . . no C18 W2 P3 P4 -20.3(4) . . . . no C19 W2 P3 P4 -110.9(3) . . . . no C20 W2 P3 As1 43.9(3) . . . . no C18 W2 P3 As1 -138.2(3) . . . . no C19 W2 P3 As1 131.1(3) . . . . no C21 W2 P3 As1 -45.5(3) . . . . no C25 W3 P4 P3 -106.0(3) . . . . no C23 W3 P4 P3 74.8(2) . . . . no C24 W3 P4 P3 -16.6(3) . . . . no C26 W3 P4 C8 -64.6(4) . . . . no C25 W3 P4 As2 137.6(3) . . . . no C23 W3 P4 As2 -41.7(2) . . . . no C24 W3 P4 As2 -133.0(3) . . . . no C26 W3 P4 P3 166.8(3) . . . . no C26 W3 P4 As2 50.4(3) . . . . no C25 W3 P4 C8 22.6(4) . . . . no C23 W3 P4 C8 -156.6(3) . . . . no C24 W3 P4 C8 112.0(4) . . . . no C31 W4 P6 As2 94.7(3) . . . . no C30 W4 P6 As2 -176.7(3) . . . . no C28 W4 P6 As2 3.0(3) . . . . no C28 W4 P6 C7 117.2(5) . . . . no C29 W4 P6 As2 -86.7(3) . . . . no C31 W4 P6 C7 -151.1(5) . . . . no C29 W4 P6 C7 27.6(5) . . . . no C30 W4 P6 C7 -62.4(5) . . . . no P3 As1 P1 As2 -64.57(9) . . . . no P1 As1 P3 W2 -166.64(9) . . . . no P1 As1 P3 P4 64.15(10) . . . . no P1 As1 P3 C2 -33.9(2) . . . . no P3 As1 P1 W1 169.03(10) . . . . no P3 As1 P1 C1 34.0(3) . . . . no P4 As2 P6 C7 -2.1(3) . . . . no P1 As2 P4 P3 -0.46(13) . . . . no P1 As2 P6 C7 97.3(3) . . . . no P4 As2 P1 W1 168.86(11) . . . . no P6 As2 P1 W1 74.36(11) . . . . no P1 As2 P6 W4 -140.81(9) . . . . no P4 As2 P6 W4 119.80(9) . . . . no P1 As2 P4 W3 126.24(9) . . . . no P6 As2 P4 W3 -132.20(9) . . . . no P6 As2 P1 C1 -152.6(3) . . . . no P6 As2 P4 P3 101.11(12) . . . . no P1 As2 P4 C8 -105.7(3) . . . . no P6 As2 P4 C8 -4.1(3) . . . . no P4 As2 P1 As1 41.86(11) . . . . no P6 As2 P1 As1 -52.64(10) . . . . no P4 As2 P1 C1 -58.1(3) . . . . no W1 P1 C1 C2 -158.3(5) . . . . no As2 P1 C1 C2 73.7(7) . . . . no W1 P1 C1 C6 22.9(8) . . . . no As1 P1 C1 C2 -27.5(7) . . . . no As2 P1 C1 C6 -105.1(7) . . . . no As1 P1 C1 C6 153.7(7) . . . . no W2 P3 P4 As2 -165.62(11) . . . . no W2 P3 P4 W3 75.54(16) . . . . no C2 P3 P4 As2 58.4(3) . . . . no C2 P3 P4 C8 162.5(4) . . . . no W2 P3 P4 C8 -61.5(3) . . . . no As1 P3 P4 W3 -159.97(9) . . . . no As1 P3 P4 As2 -41.13(12) . . . . no As1 P3 P4 C8 63.0(3) . . . . no C2 P3 P4 W3 -60.5(3) . . . . no As1 P3 C2 C1 27.7(7) . . . . no P4 P3 C2 C1 -73.4(7) . . . . no W2 P3 C2 C3 -29.7(8) . . . . no As1 P3 C2 C3 -155.0(6) . . . . no P4 P3 C2 C3 103.9(7) . . . . no W2 P3 C2 C1 153.1(5) . . . . no W3 P4 C8 C7 131.1(6) . . . . no As2 P4 C8 C9 -169.8(6) . . . . no P3 P4 C8 C9 84.3(7) . . . . no W3 P4 C8 C9 -51.4(7) . . . . no As2 P4 C8 C7 12.7(7) . . . . no P3 P4 C8 C7 -93.2(7) . . . . no W4 P6 C7 C8 -110.7(6) . . . . no As2 P6 C7 C8 11.1(7) . . . . no W4 P6 C7 C12 58.4(8) . . . . no As2 P6 C7 C12 -179.9(6) . . . . no P1 C1 C2 P3 -0.2(9) . . . . no C6 C1 C2 P3 178.7(6) . . . . no C6 C1 C2 C3 1.4(12) . . . . no P1 C1 C6 C5 177.4(7) . . . . no C2 C1 C6 C5 -1.4(13) . . . . no P1 C1 C2 C3 -177.5(6) . . . . no C1 C2 C3 C4 -0.4(12) . . . . no P3 C2 C3 C4 -177.7(7) . . . . no C2 C3 C4 C5 -0.6(13) . . . . no C3 C4 C5 C6 0.6(14) . . . . no C4 C5 C6 C1 0.4(13) . . . . no C8 C7 C12 C11 1.6(12) . . . . no P6 C7 C8 P4 -17.4(10) . . . . no P6 C7 C8 C9 165.2(6) . . . . no C12 C7 C8 P4 173.8(6) . . . . no C12 C7 C8 C9 -3.7(12) . . . . no P6 C7 C12 C11 -167.8(7) . . . . no P4 C8 C9 C10 -174.8(7) . . . . no C7 C8 C9 C10 2.7(12) . . . . no C8 C9 C10 C11 0.5(13) . . . . no C9 C10 C11 C12 -2.7(14) . . . . no C10 C11 C12 C7 1.7(14) . . . . no C38 C33 C34 C35 -6(3) . . . . no C39 C33 C34 C35 178(2) . . . . no C34 C33 C38 C37 4(3) . . . . no C39 C33 C38 C37 -180.0(18) . . . . no C33 C34 C35 C36 5(4) . . . . no C34 C35 C36 C37 -1(4) . . . . no C35 C36 C37 C38 -1(4) . . . . no C36 C37 C38 C33 -1(3) . . . . no 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 W4 O1 3.882(9) . 2_556 no As1 C7 3.682(8) . . no As1 C36 3.72(3) . . no As2 O16 3.416(8) . 2_656 no As1 H2 3.11(9) . . no P1 C13 3.195(12) . . no P1 C14 3.025(10) . . no P1 C15 3.472(10) . . no P1 C16 3.272(9) . . no P3 C18 3.343(10) . . no P3 C19 3.401(10) . . no P3 C20 3.218(10) . . no P3 C21 3.193(11) . . no P4 C23 3.209(10) . . no P4 C24 3.375(12) . . no P4 C25 3.385(11) . . no P4 C26 3.056(10) . . no P6 C28 3.317(9) . . no P6 C29 3.073(9) . . no P6 C30 3.269(11) . . no P6 C31 3.276(10) . . no O1 C36 3.10(2) . . no O1 O20 3.175(12) . 2_556 no O1 W4 3.882(9) . 2_556 no O1 O19 3.115(11) . 2_556 no O1 C32 3.100(15) . 2_556 no O1 C30 3.290(12) . 2_556 no O1 C31 3.063(14) . 2_556 no O2 O7 3.230(12) . 2_657 no O2 C22 3.196(13) . 2_657 no O2 O10 3.059(11) . 2_657 no O2 C19 3.332(12) . 2_657 no O3 C11 3.387(12) . 1_545 no O4 O14 3.059(11) . 2_656 no O4 O19 3.075(12) . . no O4 C31 3.211(13) . . no O4 C23 3.411(9) . 2_656 no O4 C26 3.157(12) . 2_656 no O5 C26 3.043(12) . 1_445 no O5 O18 3.145(10) . 2_556 no O5 O14 2.962(11) . 1_445 no O5 C27 3.253(10) . 1_445 no O5 O5 2.947(11) . 2_546 no O5 C17 3.102(12) . 2_546 no O6 C25 3.293(12) . . no O6 O12 3.055(9) . 2_767 no O6 O12 3.204(11) . . no O6 C24 3.257(13) . . no O6 O7 2.955(12) . 2_767 no O7 O6 2.955(12) . 2_767 no O7 O2 3.230(12) . 2_657 no O8 O8 3.211(13) . 2_657 no O9 C21 3.346(12) . 2_667 no O9 C9 3.395(11) . . no O9 C10 3.261(11) . . no O9 C22 3.350(14) . 2_667 no O9 O10 3.190(11) . 2_667 no O9 C34 3.39(2) . . no O9 O9 3.101(8) . 2_667 no O10 O12 3.240(12) . 2_767 no O10 C11 3.133(13) . 2_667 no O10 O9 3.190(11) . 2_667 no O10 O2 3.059(11) . 2_657 no O10 O15 3.237(8) . 2_767 no O11 C6 3.373(11) . . no O11 O16 3.220(10) . 2_656 no O11 C31 3.264(12) . 2_656 no O11 C28 3.296(10) . 2_656 no O11 C5 3.326(11) . . no O11 O19 3.233(11) . 2_656 no O12 O6 3.204(11) . . no O12 O10 3.240(12) . 2_767 no O12 C18 3.231(12) . 2_767 no O12 C18 3.290(14) . . no O12 C22 3.369(13) . 2_767 no O12 O6 3.055(9) . 2_767 no O13 O20 3.233(11) . 2_666 no O14 C16 3.326(13) . 2_656 no O14 O17 3.154(12) . . no O14 C28 3.260(12) . . no O14 O4 3.059(11) . 2_656 no O14 C29 3.243(14) . . no O14 O16 3.164(10) . . no O14 O5 2.962(11) . 1_665 no O15 O18 3.211(10) . 1_655 no O15 O10 3.237(8) . 2_767 no O15 C17 3.230(12) . 1_665 no O15 C12 3.356(14) . 1_655 no O15 C14 3.240(11) . 1_665 no O16 As2 3.416(8) . 2_656 no O16 O14 3.164(10) . . no O16 O11 3.220(10) . 2_656 no O17 O14 3.154(12) . . no O17 C7 3.414(10) . . no O17 C32 3.147(12) . 2_666 no O17 O20 3.053(10) . 2_666 no O17 C29 3.075(11) . 2_666 no O17 O17 3.011(8) . 2_666 no O18 C17 3.211(13) . 2_556 no O18 O19 3.197(10) . 2_556 no O18 O5 3.145(10) . 2_556 no O18 O15 3.211(10) . 1_455 no O19 O1 3.115(11) . 2_556 no O19 O11 3.233(11) . 2_656 no O19 O4 3.075(12) . . no O19 O18 3.197(10) . 2_556 no O19 C30 3.295(12) . 2_556 no O20 O13 3.233(11) . 2_666 no O20 C5 3.402(13) . 2_656 no O20 O17 3.053(10) . 2_666 no O20 O1 3.175(12) . 2_556 no O1 H36 2.3100 . . no O3 H3 2.7900 . . no O6 H10 2.6400 . . no O6 H39C 2.6900 . 2_667 no O7 H38 2.9100 . 2_657 no O7 H37 2.8800 . 2_657 no O7 H6 2.6500 . . no O10 H8 2.6300 . 2_667 no O10 H34 2.6600 . 2_667 no O12 H6 2.7700 . . no O13 H37 2.6500 . 1_665 no O13 H10 2.8700 . . no O15 H8 2.8900 . 1_655 no O15 H7 2.6700 . 1_655 no O18 H7 2.8800 . . no O20 H4 2.6500 . 2_656 no C2 C23 3.565(12) . . no C3 C19 3.357(12) . . no C3 C23 3.592(11) . . no C3 C24 3.446(13) . . no C4 C36 3.45(3) . 1_655 no C5 O11 3.326(11) . . no C5 O20 3.402(13) . 2_656 no C6 O11 3.373(11) . . no C6 C15 3.474(13) . . no C7 O17 3.414(10) . . no C7 As1 3.682(8) . . no C9 O9 3.395(11) . . no C9 C25 3.440(17) . . no C9 C18 3.447(13) . . no C9 C21 3.395(12) . . no C10 O9 3.261(11) . . no C11 O10 3.133(13) . 2_667 no C11 O3 3.387(12) . 1_565 no C12 C29 3.435(13) . . no C12 O15 3.356(14) . 1_455 no C12 C30 3.443(12) . . no C13 P1 3.195(12) . . no C13 As1 3.730(10) . . no C13 C17 2.757(14) . . no C13 C14 2.960(14) . . no C13 C16 2.807(15) . . no C14 C27 3.539(12) . 1_445 no C14 O15 3.240(11) . 1_445 no C14 C13 2.960(14) . . no C14 P1 3.025(10) . . no C14 C17 2.886(13) . . no C14 C15 2.977(15) . . no C15 P1 3.472(10) . . no C15 C6 3.474(13) . . no C15 C14 2.977(15) . . no C15 C16 2.846(14) . . no C15 C17 2.781(18) . . no C16 P1 3.272(9) . . no C16 C13 2.807(15) . . no C16 C17 2.926(14) . . no C16 O14 3.326(13) . 2_656 no C16 As2 3.603(10) . . no C16 C15 2.846(14) . . no C17 C16 2.926(14) . . no C17 O15 3.230(12) . 1_445 no C17 C14 2.886(13) . . no C17 C15 2.781(18) . . no C17 O18 3.211(13) . 2_556 no C17 C13 2.757(14) . . no C17 C27 3.457(13) . 1_445 no C17 O5 3.102(12) . 2_546 no C18 P3 3.343(10) . . no C18 C19 2.898(14) . . no C18 C21 2.966(17) . . no C18 C9 3.447(13) . . no C18 C24 3.393(16) . . no C18 O12 3.290(14) . . no C18 C22 2.814(14) . . no C18 O12 3.231(12) . 2_767 no C19 O2 3.332(12) . 2_657 no C19 C3 3.357(12) . . no C19 P3 3.401(10) . . no C19 C22 2.796(15) . . no C19 C20 2.824(17) . . no C19 C18 2.898(14) . . no C20 P3 3.218(10) . . no C20 C19 2.824(17) . . no C20 C21 2.882(14) . . no C20 C22 2.858(14) . . no C20 As1 3.739(9) . . no C21 P3 3.193(11) . . no C21 O9 3.346(12) . 2_667 no C21 As1 3.728(9) . . no C21 C9 3.395(12) . . no C21 C18 2.966(17) . . no C21 C22 2.854(14) . . no C21 C20 2.882(14) . . no C22 C18 2.814(14) . . no C22 C19 2.796(15) . . no C22 C21 2.854(14) . . no C22 O9 3.350(14) . 2_667 no C22 O12 3.369(13) . 2_767 no C22 O2 3.196(13) . 2_657 no C22 C20 2.858(14) . . no C23 P4 3.209(10) . . no C23 C3 3.592(11) . . no C23 O4 3.411(9) . 2_656 no C23 As2 3.515(10) . . no C23 C27 2.754(13) . . no C23 C26 2.941(13) . . no C23 C2 3.565(12) . . no C23 C24 2.931(12) . . no C24 C18 3.393(16) . . no C24 C3 3.446(13) . . no C24 O6 3.257(13) . . no C24 C27 2.837(13) . . no C24 P4 3.375(12) . . no C24 C25 2.850(14) . . no C24 C23 2.931(12) . . no C25 C27 2.867(15) . . no C25 O6 3.293(12) . . no C25 P4 3.385(11) . . no C25 C9 3.440(17) . . no C25 C26 2.824(13) . . no C25 C24 2.850(14) . . no C26 C23 2.941(13) . . no C26 P4 3.056(10) . . no C26 C27 2.884(14) . . no C26 O5 3.043(12) . 1_665 no C26 O4 3.157(12) . 2_656 no C26 C25 2.824(13) . . no C26 As2 3.505(9) . . no C27 C23 2.754(13) . . no C27 C26 2.884(14) . . no C27 C25 2.867(15) . . no C27 C14 3.539(12) . 1_665 no C27 O5 3.253(10) . 1_665 no C27 C24 2.837(13) . . no C27 C17 3.457(13) . 1_665 no C28 C31 2.927(16) . . no C28 As2 3.553(8) . . no C28 C32 2.778(15) . . no C28 O14 3.260(12) . . no C28 C29 2.898(13) . . no C28 O11 3.296(10) . 2_656 no C28 P6 3.317(9) . . no C29 O14 3.243(14) . . no C29 C32 2.928(13) . . no C29 C12 3.435(13) . . no C29 C29 3.521(13) . 2_666 no C29 C28 2.898(13) . . no C29 C7 3.180(12) . . no C29 P6 3.073(9) . . no C29 O17 3.075(11) . 2_666 no C29 C30 2.900(16) . . no C30 C29 2.900(16) . . no C30 C31 2.849(14) . . no C30 P6 3.269(11) . . no C30 C32 2.797(14) . . no C30 C12 3.443(12) . . no C30 O19 3.295(12) . 2_556 no C30 O1 3.290(12) . 2_556 no C31 O1 3.063(14) . 2_556 no C31 C30 2.849(14) . . no C31 P6 3.276(10) . . no C31 O4 3.211(13) . . no C31 O11 3.264(12) . 2_656 no C31 C32 2.865(13) . . no C31 C28 2.927(16) . . no C32 C31 2.865(13) . . no C32 C29 2.928(13) . . no C32 O1 3.100(15) . 2_556 no C32 O17 3.147(12) . 2_666 no C32 C28 2.778(15) . . no C32 C30 2.797(14) . . no C34 O9 3.39(2) . . no C36 O1 3.10(2) . . no C36 C4 3.45(3) . 1_455 no C36 As1 3.72(3) . . no C4 H39B 3.0800 . 2_657 no C13 H36 3.0500 . . no C13 H2 3.07(9) . . no C15 H3 2.6100 . . no C18 H39C 2.9500 . 2_667 no C18 H10 2.7500 . . no C19 H6 2.5700 . . no C20 H39A 3.0900 . . no C24 H6 3.0300 . . no C25 H10 2.7900 . . no C30 H7 2.8000 . . no C35 H5 3.0800 . 1_455 no C36 H5 2.8500 . 1_455 no C37 H1 2.8800 . . no C37 H5 2.8600 . 1_455 no C38 H1 2.9700 . . no C38 H5 3.1000 . 1_455 no H1 C38 2.9700 . . no H1 C37 2.8800 . . no H2 As1 3.11(9) . . no H2 C13 3.07(9) . . no H3 C15 2.6100 . . no H3 O3 2.7900 . . no H4 O20 2.6500 . 2_656 no H5 C35 3.0800 . 1_655 no H5 C36 2.8500 . 1_655 no H5 C38 3.1000 . 1_655 no H5 C37 2.8600 . 1_655 no H6 O12 2.7700 . . no H6 O7 2.6500 . . no H6 C19 2.5700 . . no H6 C24 3.0300 . . no H7 O15 2.6700 . 1_455 no H7 C30 2.8000 . . no H7 O18 2.8800 . . no H8 O15 2.8900 . 1_455 no H8 O10 2.6300 . 2_667 no H10 O6 2.6400 . . no H10 O13 2.8700 . . no H10 C18 2.7500 . . no H10 C25 2.7900 . . no H34 H39C 2.2900 . . no H34 O10 2.6600 . 2_667 no H36 O1 2.3100 . . no H36 C13 3.0500 . . no H37 O13 2.6500 . 1_445 no H37 O7 2.8800 . 2_657 no H38 H39B 2.4900 . . no H38 O7 2.9100 . 2_657 no H39A C20 3.0900 . . no H39B H38 2.4900 . . no H39B C4 3.0800 . 2_657 no H39C H34 2.2900 . . no H39C O6 2.6900 . 2_667 no H39C C18 2.9500 . 2_667 no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C36 H36 O1 0.9500 2.3100 3.10(2) 140.00 . yes _vrf_PLAT027_ms11 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 62.18 Deg. RESPONSE: Theta is technically limited at the Oxford Diffraction Gemini Ultra. ; #===END # Attachment 'pw2ph.cif' # CIF-file generated for pw2ph R = 0.03 #============================================================================== data_pw2ph _database_code_depnum_ccdc_archive 'CCDC 714101' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H10 O20 P6 W4, C H2 Cl2' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C33 H12 Cl2 O20 P6 W4' _chemical_formula_iupac ? _chemical_formula_weight 1720.51 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.547(3) _cell_length_b 14.237(3) _cell_length_c 17.070(7) _cell_angle_alpha 111.295(6) _cell_angle_beta 104.846(7) _cell_angle_gamma 99.201(18) _cell_volume 2425.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 6178 _cell_measurement_theta_min 2.9566 _cell_measurement_theta_max 62.1439 _cell_special_details ; Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0. ; _exptl_crystal_description 'flat prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.356 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 20.615 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.29287 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -27.00 22.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -1.2571 45.0000 120.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 2 omega -21.00 26.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 2.5071 45.0000 240.0000 0.0000 0.0000 47 #__ type_ start__ end____ width___ exp.time_ 3 phi -177.00 -119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 40.0000 2.5071 0.0000 - 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 4 omega -113.00 -57.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 106.0000 227.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 5 phi -31.00 31.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames -40.0000 -83.1433 0.0000 - 0.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 6 omega -115.00 -59.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 75.0000 0.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 7 omega -107.00 -50.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 -79.0000 314.0000 0.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 8 omega -107.00 -56.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 -45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 9 omega -115.00 -61.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -83.1433 112.0000 60.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 10 omega 54.00 82.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -121.0000 217.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 11 omega 81.00 109.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -45.0000 120.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 12 omega 58.00 109.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 45.0000 0.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 13 omega 11.00 61.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -45.0000 120.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 14 omega 60.00 100.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 -45.0000 0.0000 0.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 15 omega 105.00 133.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 84.3933 64.0000 -48.0000 0.0000 0.0000 28 ; _diffrn_detector_area_resol_mean 10.5431 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10270 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 62.12 _diffrn_reflns_theta_full 62.12 _diffrn_measured_fraction_theta_max 0.790 _diffrn_measured_fraction_theta_full 0.790 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 6061 # number of observed reflections (> n sig(I)) _reflns_number_gt 4743 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 6061 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.270 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.156 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.317 0.278 0.190 7 1 ' ' 2 0.500 1.000 0.500 96 38 CH2Cl2 3 0.683 0.722 0.809 7 1 ' ' _platon_squeeze_details ; With the aid of PLATON two solvent accessible areas were found, but it was impossible to refine any reasonable molecule from difference Fourier peaks. Therefore the midpoint, the size and the number of electrons in these voids were refined and the contribution to the calculated structure factors of the disordered solvent is taken into account by back-Fourier transformation with the program SQUEEZE (Sluis and Spek, 1990). The void were found at (0.500, 1.000, 0.500 ) the sizes is 96\%A^3^, 38 e^-^. This electron number corresponds to one dichlormethane molecule. ; #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags W1 W Uani 1.34550(3) 0.55287(3) 0.35362(3) 1.000 0.0177(1) . . W2 W Uani 0.83916(3) 0.14429(3) -0.07864(3) 1.000 0.0154(1) . . W3 W Uani 0.64869(3) 0.24012(3) 0.19262(3) 1.000 0.0158(1) . . W4 W Uani 0.92938(3) 0.74587(3) 0.38444(3) 1.000 0.0194(1) . . P1 P Uani 1.13710(17) 0.42692(15) 0.25896(14) 1.000 0.0139(6) . . P2 P Uani 1.0764(2) 0.39471(17) 0.11680(15) 1.000 0.0242(7) . . P3 P Uani 0.92661(18) 0.25654(15) 0.08449(14) 1.000 0.0137(6) . . P4 P Uani 0.81503(17) 0.34153(14) 0.16244(15) 1.000 0.0134(6) . . P5 P Uani 0.96611(18) 0.45596(15) 0.29072(15) 1.000 0.0149(6) . . P6 P Uani 0.95622(18) 0.59696(15) 0.26533(15) 1.000 0.0164(6) . . O1 O Uani 1.4566(6) 0.3784(5) 0.3929(5) 1.000 0.037(2) . . O2 O Uani 1.4186(6) 0.4762(5) 0.1777(5) 1.000 0.033(2) . . O3 O Uani 1.2831(6) 0.7490(5) 0.3212(4) 1.000 0.037(2) . . O4 O Uani 1.2593(6) 0.6182(5) 0.5251(5) 1.000 0.038(3) . . O5 O Uani 1.6206(6) 0.6973(5) 0.4687(5) 1.000 0.045(2) . . O6 O Uani 0.8443(6) 0.3479(5) -0.1148(4) 1.000 0.034(2) . . O7 O Uani 0.5552(6) 0.1012(5) -0.0912(4) 1.000 0.031(3) . . O8 O Uani 0.8243(6) -0.0769(4) -0.0685(4) 1.000 0.032(2) . . O9 O Uani 1.1197(5) 0.1701(4) -0.0732(4) 1.000 0.0252(19) . . O10 O Uani 0.7460(6) 0.0189(5) -0.2888(4) 1.000 0.030(2) . . O11 O Uani 0.6462(5) 0.0163(5) 0.0542(5) 1.000 0.032(2) . . O12 O Uani 0.8563(6) 0.2256(5) 0.3487(5) 1.000 0.037(3) . . O13 O Uani 0.6546(5) 0.4675(5) 0.3240(4) 1.000 0.0284(19) . . O14 O Uani 0.4215(6) 0.2454(5) 0.0428(5) 1.000 0.035(2) . . O15 O Uani 0.4436(7) 0.1317(5) 0.2491(5) 1.000 0.049(3) . . O16 O Uani 0.8853(6) 0.6098(5) 0.4936(4) 1.000 0.038(2) . . O17 O Uani 1.2156(7) 0.8299(6) 0.5055(5) 1.000 0.051(3) . . O18 O Uani 0.9987(6) 0.8802(5) 0.2804(5) 1.000 0.037(3) . . O19 O Uani 0.6405(6) 0.6658(5) 0.2686(5) 1.000 0.046(3) . . O20 O Uani 0.8744(9) 0.9379(5) 0.5211(6) 1.000 0.063(4) . . C1 C Uani 1.0986(7) 0.2920(5) 0.2478(5) 1.000 0.012(3) . . C2 C Uani 1.0031(7) 0.2159(6) 0.1693(6) 1.000 0.015(3) . . C3 C Uani 0.9610(7) 0.1139(6) 0.1620(6) 1.000 0.015(3) . . C4 C Uani 1.0141(7) 0.0903(6) 0.2324(6) 1.000 0.018(3) . . C5 C Uani 1.1072(7) 0.1632(6) 0.3072(6) 1.000 0.019(3) . . C6 C Uani 1.1494(7) 0.2654(6) 0.3172(6) 1.000 0.018(3) . . C7 C Uani 0.8362(7) 0.5366(6) 0.1540(6) 1.000 0.017(3) . . C8 C Uani 0.7741(7) 0.4307(6) 0.1118(6) 1.000 0.016(3) . . C9 C Uani 0.6779(7) 0.3900(6) 0.0294(6) 1.000 0.021(3) . . C10 C Uani 0.6454(8) 0.4548(7) -0.0111(6) 1.000 0.026(3) . . C11 C Uani 0.7064(8) 0.5623(7) 0.0309(7) 1.000 0.030(3) . . C12 C Uani 0.7997(8) 0.6031(6) 0.1130(6) 1.000 0.025(3) . . C13 C Uani 1.4124(7) 0.4394(7) 0.3783(6) 1.000 0.021(3) . . C14 C Uani 1.3934(7) 0.5061(7) 0.2402(7) 1.000 0.023(3) . . C15 C Uani 1.2999(7) 0.6781(7) 0.3322(6) 1.000 0.021(3) . . C16 C Uani 1.2918(8) 0.5949(7) 0.4641(8) 1.000 0.029(3) . . C17 C Uani 1.5201(8) 0.6481(7) 0.4272(6) 1.000 0.027(3) . . C18 C Uani 0.8408(7) 0.2782(6) -0.0985(6) 1.000 0.019(3) . . C19 C Uani 0.6573(8) 0.1194(6) -0.0854(6) 1.000 0.022(3) . . C20 C Uani 0.8306(8) 0.0023(7) -0.0703(6) 1.000 0.020(3) . . C21 C Uani 1.0202(8) 0.1606(6) -0.0756(6) 1.000 0.026(3) . . C22 C Uani 0.7795(7) 0.0625(6) -0.2152(6) 1.000 0.016(3) . . C23 C Uani 0.6479(7) 0.0957(6) 0.1028(6) 1.000 0.020(3) . . C24 C Uani 0.7839(8) 0.2313(6) 0.2933(7) 1.000 0.023(3) . . C25 C Uani 0.6520(7) 0.3856(7) 0.2785(6) 1.000 0.018(3) . . C26 C Uani 0.5057(8) 0.2442(6) 0.0951(6) 1.000 0.022(3) . . C27 C Uani 0.5173(8) 0.1709(6) 0.2282(7) 1.000 0.028(3) . . C28 C Uani 0.8988(8) 0.6571(6) 0.4540(6) 1.000 0.026(3) . . C29 C Uani 1.1148(8) 0.7970(7) 0.4608(6) 1.000 0.028(3) . . C30 C Uani 0.9714(8) 0.8321(7) 0.3160(7) 1.000 0.026(3) . . C31 C Uani 0.7422(8) 0.6959(6) 0.3101(6) 1.000 0.023(3) . . C32 C Uani 0.8960(10) 0.8685(7) 0.4732(6) 1.000 0.031(3) . . Cl1 Cl Uani 0.5027(4) 0.8502(4) 0.2721(3) 1.000 0.096(2) . . Cl2 Cl Uani 0.7192(4) 0.9183(7) 0.2354(6) 1.000 0.229(5) . . C40 C Uani 0.6294(19) 0.9550(13) 0.3017(11) 1.000 0.124(9) . . H1 H Uiso 1.15570 0.34960 0.10200 1.000 0.0360 . . H2 H Uiso 1.04420 0.61390 0.23920 1.000 0.0250 . . H22 H Uiso 0.89710 0.06180 0.10940 1.000 0.0180 calc R H23 H Uiso 0.98480 0.02190 0.22830 1.000 0.0220 calc R H24 H Uiso 1.14420 0.14410 0.35350 1.000 0.0230 calc R H25 H Uiso 1.21230 0.31650 0.37090 1.000 0.0210 calc R H28 H Uiso 0.63460 0.31720 0.00090 1.000 0.0250 calc R H29 H Uiso 0.58110 0.42610 -0.06780 1.000 0.0320 calc R H30 H Uiso 0.68390 0.60680 0.00310 1.000 0.0360 calc R H31 H Uiso 0.84010 0.67640 0.14260 1.000 0.0300 calc R H40A H Uiso 0.59960 1.01390 0.29460 1.000 0.1490 calc R H40B H Uiso 0.68060 0.97940 0.36530 1.000 0.1490 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 W1 0.0132(2) 0.0204(2) 0.0124(2) 0.0041(2) 0.0003(2) -0.0006(2) W2 0.0164(2) 0.0118(2) 0.0121(2) 0.0023(2) 0.0022(2) -0.0002(1) W3 0.0143(2) 0.0128(2) 0.0166(3) 0.0048(2) 0.0035(2) 0.0003(1) W4 0.0263(2) 0.0100(2) 0.0186(3) 0.0038(2) 0.0081(2) 0.0014(2) P1 0.0120(9) 0.0139(9) 0.0115(13) 0.0027(9) 0.0017(9) 0.0026(8) P2 0.0249(11) 0.0228(11) 0.0117(14) 0.0066(10) -0.0029(10) -0.0107(9) P3 0.0145(10) 0.0125(9) 0.0108(13) 0.0041(9) 0.0026(9) 0.0004(8) P4 0.0122(9) 0.0114(9) 0.0127(13) 0.0032(9) 0.0014(9) 0.0023(8) P5 0.0145(10) 0.0112(9) 0.0144(13) 0.0041(9) 0.0009(9) 0.0018(8) P6 0.0184(10) 0.0098(9) 0.0169(13) 0.0057(9) 0.0010(10) 0.0013(8) O1 0.029(3) 0.052(4) 0.044(5) 0.030(4) 0.015(3) 0.021(3) O2 0.029(4) 0.047(4) 0.014(4) 0.005(4) 0.007(3) 0.005(3) O3 0.038(4) 0.022(3) 0.037(5) 0.011(3) -0.001(3) -0.001(3) O4 0.038(4) 0.051(4) 0.034(5) 0.019(4) 0.020(4) 0.023(3) O5 0.021(3) 0.058(4) 0.038(5) 0.016(4) 0.000(3) -0.005(3) O6 0.063(4) 0.022(3) 0.021(4) 0.015(3) 0.015(4) 0.011(3) O7 0.022(4) 0.036(4) 0.030(5) 0.012(3) 0.007(3) 0.002(3) O8 0.053(4) 0.018(3) 0.029(4) 0.010(3) 0.022(4) 0.011(3) O9 0.020(3) 0.029(3) 0.023(4) 0.007(3) 0.010(3) 0.003(3) O10 0.036(4) 0.035(3) 0.010(4) 0.000(3) 0.008(3) 0.013(3) O11 0.030(3) 0.019(3) 0.034(5) 0.005(3) 0.005(3) -0.001(3) O12 0.040(4) 0.051(4) 0.031(5) 0.026(4) 0.013(4) 0.021(3) O13 0.027(3) 0.023(3) 0.030(4) 0.002(3) 0.014(3) 0.009(3) O14 0.028(3) 0.032(3) 0.035(5) 0.011(3) -0.002(3) 0.008(3) O15 0.047(4) 0.040(4) 0.061(6) 0.020(4) 0.032(4) -0.002(3) O16 0.061(4) 0.027(3) 0.022(4) 0.010(3) 0.013(4) 0.005(3) O17 0.045(5) 0.060(5) 0.031(5) 0.017(4) 0.000(4) -0.006(4) O18 0.046(4) 0.031(4) 0.039(5) 0.024(4) 0.014(4) 0.002(3) O19 0.023(4) 0.048(4) 0.068(6) 0.030(4) 0.011(4) 0.006(3) O20 0.111(7) 0.025(4) 0.066(7) 0.007(4) 0.066(6) 0.021(4) C1 0.017(4) 0.008(4) 0.011(5) 0.000(3) 0.007(4) 0.008(3) C2 0.015(4) 0.012(4) 0.015(5) 0.005(4) 0.003(4) 0.005(3) C3 0.015(4) 0.016(4) 0.014(5) 0.005(4) 0.007(4) 0.002(3) C4 0.023(4) 0.017(4) 0.012(5) 0.003(4) 0.008(4) 0.007(3) C5 0.029(5) 0.028(5) 0.008(5) 0.011(4) 0.007(4) 0.018(4) C6 0.018(4) 0.020(4) 0.012(5) 0.005(4) 0.002(4) 0.008(3) C7 0.017(4) 0.018(4) 0.008(5) 0.001(4) 0.002(4) 0.000(3) C8 0.014(4) 0.019(4) 0.019(5) 0.014(4) 0.003(4) 0.008(3) C9 0.020(4) 0.017(4) 0.021(6) 0.003(4) 0.005(4) 0.009(3) C10 0.019(4) 0.029(5) 0.019(6) 0.006(4) -0.006(4) 0.006(4) C11 0.037(5) 0.021(5) 0.031(6) 0.015(5) 0.002(5) 0.010(4) C12 0.035(5) 0.018(4) 0.020(6) 0.009(4) 0.004(5) 0.007(4) C13 0.010(4) 0.039(5) 0.022(6) 0.020(5) 0.009(4) 0.008(4) C14 0.012(4) 0.022(4) 0.024(7) 0.009(5) -0.005(5) -0.003(4) C15 0.021(4) 0.024(5) 0.010(5) 0.004(4) 0.001(4) 0.003(4) C16 0.016(4) 0.027(5) 0.037(7) 0.019(5) -0.006(5) 0.001(4) C17 0.015(5) 0.037(5) 0.011(6) -0.001(4) 0.000(4) -0.007(4) C18 0.025(4) 0.014(4) 0.012(5) -0.001(4) 0.008(4) 0.001(3) C19 0.016(5) 0.018(4) 0.023(6) 0.004(4) -0.001(4) 0.006(3) C20 0.025(4) 0.023(4) 0.016(5) 0.0050 0.017(4) 0.009(3) C21 0.018(5) 0.019(4) 0.026(6) 0.006(4) -0.008(4) 0.000(4) C22 0.016(4) 0.022(4) 0.007(6) 0.003(4) 0.008(4) 0.002(3) C23 0.019(4) 0.016(4) 0.017(6) 0.006(4) 0.000(4) -0.001(3) C24 0.023(4) 0.017(4) 0.034(6) 0.013(4) 0.014(5) 0.003(4) C25 0.016(4) 0.024(5) 0.011(5) 0.006(4) 0.004(4) 0.002(4) C26 0.021(5) 0.019(4) 0.019(6) 0.003(4) 0.006(4) 0.002(4) C27 0.026(5) 0.017(4) 0.033(6) 0.009(4) 0.006(5) -0.003(4) C28 0.029(5) 0.016(4) 0.025(6) 0.010(4) 0.000(4) 0.000(4) C29 0.027(5) 0.030(5) 0.015(6) 0.009(4) -0.001(5) -0.005(4) C30 0.025(5) 0.023(5) 0.029(6) 0.011(5) 0.009(5) 0.008(4) C31 0.030(5) 0.021(4) 0.030(6) 0.014(4) 0.021(5) 0.012(4) C32 0.069(7) 0.015(5) 0.017(6) 0.005(4) 0.029(6) 0.013(5) Cl1 0.089(3) 0.138(4) 0.141(4) 0.110(4) 0.069(3) 0.066(3) Cl2 0.079(3) 0.376(10) 0.466(12) 0.381(10) 0.133(5) 0.117(5) C40 0.157(19) 0.087(12) 0.067(13) -0.009(10) 0.000(13) 0.038(12) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 P1 2.478(2) . . yes W1 C13 2.028(10) . . yes W1 C14 2.056(10) . . yes W1 C15 2.065(10) . . yes W1 C16 2.049(11) . . yes W1 C17 2.018(10) . . yes W2 P3 2.478(2) . . yes W2 C18 2.052(9) . . yes W2 C19 2.039(10) . . yes W2 C20 2.066(11) . . yes W2 C21 2.051(10) . . yes W2 C22 2.053(9) . . yes W3 P4 2.490(2) . . yes W3 C23 2.068(9) . . yes W3 C24 2.062(10) . . yes W3 C25 2.045(10) . . yes W3 C26 2.048(9) . . yes W3 C27 2.018(10) . . yes W4 P6 2.475(3) . . yes W4 C28 2.072(9) . . yes W4 C29 2.048(10) . . yes W4 C30 2.061(11) . . yes W4 C31 2.058(10) . . yes W4 C32 2.021(10) . . yes Cl1 C40 1.73(2) . . yes Cl2 C40 1.73(2) . . yes P1 P5 2.238(3) . . yes P1 C1 1.828(8) . . yes P1 P2 2.193(3) . . yes P2 P3 2.191(4) . . yes P3 C2 1.824(9) . . yes P3 P4 2.259(3) . . yes P4 C8 1.834(10) . . yes P4 P5 2.244(3) . . yes P5 P6 2.216(3) . . yes P6 C7 1.831(9) . . yes P2 H1 1.2300 . . no P6 H2 1.2300 . . no O1 C13 1.145(13) . . yes O2 C14 1.128(12) . . yes O3 C15 1.129(13) . . yes O4 C16 1.151(14) . . yes O5 C17 1.139(12) . . yes O6 C18 1.121(12) . . yes O7 C19 1.136(12) . . yes O8 C20 1.130(12) . . yes O9 C21 1.124(11) . . yes O10 C22 1.105(11) . . yes O11 C23 1.127(12) . . yes O12 C24 1.128(13) . . yes O13 C25 1.133(12) . . yes O14 C26 1.146(12) . . yes O15 C27 1.145(13) . . yes O16 C28 1.134(12) . . yes O17 C29 1.126(13) . . yes O18 C30 1.127(13) . . yes O19 C31 1.121(12) . . yes O20 C32 1.142(14) . . yes C1 C2 1.411(12) . . no C1 C6 1.390(12) . . no C2 C3 1.404(13) . . no C3 C4 1.384(13) . . no C4 C5 1.357(13) . . no C5 C6 1.391(13) . . no C7 C8 1.381(13) . . no C7 C12 1.422(13) . . no C8 C9 1.396(13) . . no C9 C10 1.382(14) . . no C10 C11 1.397(15) . . no C11 C12 1.377(14) . . no C3 H22 0.9500 . . no C4 H23 0.9500 . . no C5 H24 0.9500 . . no C6 H25 0.9500 . . no C9 H28 0.9500 . . no C10 H29 0.9500 . . no C11 H30 0.9500 . . no C12 H31 0.9500 . . no C40 H40A 0.9900 . . no C40 H40B 0.9900 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 W1 C13 91.6(3) . . . yes P1 W1 C14 86.9(3) . . . yes P1 W1 C15 94.9(3) . . . yes P1 W1 C16 91.0(3) . . . yes P1 W1 C17 176.3(3) . . . yes C13 W1 C14 87.2(4) . . . yes C13 W1 C15 173.0(4) . . . yes C13 W1 C16 92.4(4) . . . yes C13 W1 C17 85.6(4) . . . yes C14 W1 C15 90.4(4) . . . yes C14 W1 C16 177.9(4) . . . yes C14 W1 C17 90.6(4) . . . yes C15 W1 C16 90.2(4) . . . yes C15 W1 C17 87.8(4) . . . yes C16 W1 C17 91.5(4) . . . yes P3 W2 C18 88.3(3) . . . yes P3 W2 C19 95.2(3) . . . yes P3 W2 C20 96.6(3) . . . yes P3 W2 C21 86.8(3) . . . yes P3 W2 C22 174.1(3) . . . yes C18 W2 C19 92.5(4) . . . yes C18 W2 C20 175.1(4) . . . yes C18 W2 C21 90.0(4) . . . yes C18 W2 C22 87.4(4) . . . yes C19 W2 C20 86.9(4) . . . yes C19 W2 C21 176.9(4) . . . yes C19 W2 C22 89.0(3) . . . yes C20 W2 C21 90.5(4) . . . yes C20 W2 C22 87.8(4) . . . yes C21 W2 C22 89.2(3) . . . yes P4 W3 C23 94.3(3) . . . yes P4 W3 C24 89.5(3) . . . yes P4 W3 C25 83.6(3) . . . yes P4 W3 C26 94.3(3) . . . yes P4 W3 C27 174.3(3) . . . yes C23 W3 C24 90.6(4) . . . yes C23 W3 C25 177.7(4) . . . yes C23 W3 C26 89.4(4) . . . yes C23 W3 C27 91.1(4) . . . yes C24 W3 C25 90.4(4) . . . yes C24 W3 C26 176.2(4) . . . yes C24 W3 C27 88.9(4) . . . yes C25 W3 C26 89.7(4) . . . yes C25 W3 C27 91.0(4) . . . yes C26 W3 C27 87.3(4) . . . yes P6 W4 C28 92.2(3) . . . yes P6 W4 C29 93.3(3) . . . yes P6 W4 C30 85.7(3) . . . yes P6 W4 C31 87.8(3) . . . yes P6 W4 C32 175.0(3) . . . yes C28 W4 C29 88.7(4) . . . yes C28 W4 C30 176.1(4) . . . yes C28 W4 C31 90.7(4) . . . yes C28 W4 C32 90.7(4) . . . yes C29 W4 C30 88.1(4) . . . yes C29 W4 C31 178.8(4) . . . yes C29 W4 C32 90.9(4) . . . yes C30 W4 C31 92.5(4) . . . yes C30 W4 C32 91.5(4) . . . yes C31 W4 C32 88.1(4) . . . yes W1 P1 P2 116.41(11) . . . yes W1 P1 P5 120.79(11) . . . yes W1 P1 C1 122.0(3) . . . yes P2 P1 P5 100.51(12) . . . yes P2 P1 C1 99.0(3) . . . yes P5 P1 C1 93.2(3) . . . yes P1 P2 P3 91.26(12) . . . yes W2 P3 P2 111.40(11) . . . yes W2 P3 P4 123.03(11) . . . yes W2 P3 C2 125.2(3) . . . yes P2 P3 P4 97.48(12) . . . yes P2 P3 C2 98.9(3) . . . yes P4 P3 C2 95.3(3) . . . yes W3 P4 P3 119.67(11) . . . yes W3 P4 P5 110.77(11) . . . yes W3 P4 C8 118.0(3) . . . yes P3 P4 P5 101.54(12) . . . yes P3 P4 C8 103.8(3) . . . yes P5 P4 C8 100.2(3) . . . yes P1 P5 P4 101.12(12) . . . yes P1 P5 P6 100.79(12) . . . yes P4 P5 P6 95.88(12) . . . yes W4 P6 P5 116.24(11) . . . yes W4 P6 C7 118.5(3) . . . yes P5 P6 C7 100.3(3) . . . yes P3 P2 H1 98.00 . . . no P1 P2 H1 94.00 . . . no W4 P6 H2 118.00 . . . no C7 P6 H2 95.00 . . . no P5 P6 H2 105.00 . . . no P1 C1 C6 122.3(6) . . . yes P1 C1 C2 117.6(6) . . . yes C2 C1 C6 119.7(8) . . . no P3 C2 C1 118.7(7) . . . yes P3 C2 C3 121.4(7) . . . yes C1 C2 C3 119.6(8) . . . no C2 C3 C4 119.1(8) . . . no C3 C4 C5 121.2(9) . . . no C4 C5 C6 121.1(9) . . . no C1 C6 C5 119.3(8) . . . no C8 C7 C12 119.1(8) . . . no P6 C7 C8 122.4(7) . . . yes P6 C7 C12 118.3(7) . . . yes C7 C8 C9 120.0(9) . . . no P4 C8 C7 121.1(7) . . . yes P4 C8 C9 118.9(7) . . . yes C8 C9 C10 120.4(9) . . . no C9 C10 C11 120.4(9) . . . no C10 C11 C12 119.3(9) . . . no C7 C12 C11 120.7(9) . . . no W1 C13 O1 176.2(8) . . . yes W1 C14 O2 177.1(10) . . . yes W1 C15 O3 175.4(8) . . . yes W1 C16 O4 178.7(9) . . . yes W1 C17 O5 176.4(9) . . . yes W2 C18 O6 174.8(8) . . . yes W2 C19 O7 177.2(9) . . . yes W2 C20 O8 177.9(8) . . . yes W2 C21 O9 179.4(9) . . . yes W2 C22 O10 179.1(8) . . . yes W3 C23 O11 179.0(8) . . . yes W3 C24 O12 178.8(9) . . . yes W3 C25 O13 177.6(8) . . . yes W3 C26 O14 176.4(8) . . . yes W3 C27 O15 179.4(12) . . . yes W4 C28 O16 178.2(7) . . . yes W4 C29 O17 176.3(9) . . . yes W4 C30 O18 177.6(8) . . . yes W4 C31 O19 178.0(9) . . . yes W4 C32 O20 177.8(9) . . . yes C2 C3 H22 120.00 . . . no C4 C3 H22 120.00 . . . no C3 C4 H23 119.00 . . . no C5 C4 H23 119.00 . . . no C4 C5 H24 119.00 . . . no C6 C5 H24 119.00 . . . no C1 C6 H25 120.00 . . . no C5 C6 H25 120.00 . . . no C8 C9 H28 120.00 . . . no C10 C9 H28 120.00 . . . no C9 C10 H29 120.00 . . . no C11 C10 H29 120.00 . . . no C10 C11 H30 120.00 . . . no C12 C11 H30 120.00 . . . no C7 C12 H31 120.00 . . . no C11 C12 H31 120.00 . . . no Cl1 C40 Cl2 110.4(11) . . . yes Cl1 C40 H40A 110.00 . . . no Cl1 C40 H40B 110.00 . . . no Cl2 C40 H40A 110.00 . . . no Cl2 C40 H40B 110.00 . . . no H40A C40 H40B 108.00 . . . no 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 C13 W1 P1 P2 -115.1(3) . . . . no C14 W1 P1 P2 -28.0(3) . . . . no C15 W1 P1 P2 62.1(3) . . . . no C16 W1 P1 P2 152.4(3) . . . . no C13 W1 P1 P5 122.6(3) . . . . no C14 W1 P1 P5 -150.2(3) . . . . no C15 W1 P1 P5 -60.1(3) . . . . no C16 W1 P1 P5 30.2(3) . . . . no C13 W1 P1 C1 6.0(4) . . . . no C14 W1 P1 C1 93.1(4) . . . . no C15 W1 P1 C1 -176.7(4) . . . . no C16 W1 P1 C1 -86.5(4) . . . . no C21 W2 P3 P2 46.3(3) . . . . no C18 W2 P3 P4 71.2(3) . . . . no C19 W2 P3 P4 -21.2(3) . . . . no C20 W2 P3 P4 -108.6(3) . . . . no C21 W2 P3 P4 161.3(3) . . . . no C18 W2 P3 C2 -162.4(4) . . . . no C19 W2 P3 C2 105.3(4) . . . . no C20 W2 P3 C2 17.9(5) . . . . no C21 W2 P3 C2 -72.3(4) . . . . no C18 W2 P3 P2 -43.8(3) . . . . no C19 W2 P3 P2 -136.1(3) . . . . no C20 W2 P3 P2 136.5(3) . . . . no C26 W3 P4 P5 140.1(3) . . . . no C23 W3 P4 C8 115.3(4) . . . . no C24 W3 P4 C8 -154.1(4) . . . . no C24 W3 P4 P5 -39.6(3) . . . . no C25 W3 P4 P5 50.9(3) . . . . no C23 W3 P4 P3 -12.6(3) . . . . no C24 W3 P4 P3 78.0(3) . . . . no C25 W3 P4 P3 168.4(3) . . . . no C26 W3 P4 P3 -102.4(3) . . . . no C23 W3 P4 P5 -130.2(3) . . . . no C26 W3 P4 C8 25.5(4) . . . . no C25 W3 P4 C8 -63.7(4) . . . . no C30 W4 P6 C7 -72.4(4) . . . . no C28 W4 P6 P5 -8.7(3) . . . . no C30 W4 P6 P5 168.0(3) . . . . no C31 W4 P6 P5 -99.3(3) . . . . no C29 W4 P6 P5 80.2(3) . . . . no C31 W4 P6 C7 20.3(4) . . . . no C29 W4 P6 C7 -160.2(4) . . . . no C28 W4 P6 C7 110.9(4) . . . . no W1 P1 P2 P3 165.44(11) . . . . no W1 P1 C1 C2 -154.9(6) . . . . no W1 P1 P5 P4 165.01(11) . . . . no W1 P1 P5 P6 66.74(15) . . . . no C1 P1 P2 P3 32.7(3) . . . . no P5 P1 P2 P3 -62.22(13) . . . . no C1 P1 P5 P4 -64.4(3) . . . . no C1 P1 P5 P6 -162.6(3) . . . . no P2 P1 P5 P4 35.42(15) . . . . no P2 P1 P5 P6 -62.85(14) . . . . no P2 P1 C1 C2 -25.8(7) . . . . no P5 P1 C1 C6 -97.1(7) . . . . no P5 P1 C1 C2 75.4(7) . . . . no P2 P1 C1 C6 161.7(7) . . . . no W1 P1 C1 C6 32.6(8) . . . . no P1 P2 P3 W2 -165.75(11) . . . . no P1 P2 P3 P4 64.31(13) . . . . no P1 P2 P3 C2 -32.3(3) . . . . no W2 P3 C2 C3 -37.4(9) . . . . no P2 P3 C2 C3 -161.6(7) . . . . no P2 P3 C2 C1 24.7(7) . . . . no P4 P3 C2 C1 -73.8(7) . . . . no C2 P3 P4 W3 -66.3(3) . . . . no W2 P3 P4 W3 72.46(16) . . . . no W2 P3 P4 P5 -165.35(12) . . . . no W2 P3 P4 C8 -61.7(3) . . . . no P2 P3 P4 W3 -165.93(11) . . . . no P2 P3 P4 P5 -43.73(14) . . . . no P2 P3 P4 C8 59.9(3) . . . . no W2 P3 C2 C1 148.9(6) . . . . no C2 P3 P4 P5 55.9(3) . . . . no C2 P3 P4 C8 159.6(4) . . . . no P4 P3 C2 C3 100.0(7) . . . . no C8 P4 P5 P6 0.8(3) . . . . no W3 P4 C8 C7 121.7(7) . . . . no P3 P4 C8 C7 -103.2(7) . . . . no P3 P4 C8 C9 77.1(7) . . . . no W3 P4 C8 C9 -58.0(8) . . . . no P5 P4 C8 C9 -178.2(7) . . . . no P3 P4 P5 P1 5.04(15) . . . . no P3 P4 P5 P6 107.28(12) . . . . no C8 P4 P5 P1 -101.5(3) . . . . no W3 P4 P5 P6 -124.58(11) . . . . no P5 P4 C8 C7 1.5(8) . . . . no W3 P4 P5 P1 133.18(11) . . . . no P1 P5 P6 W4 -130.51(11) . . . . no P4 P5 P6 C7 -2.1(3) . . . . no P1 P5 P6 C7 100.5(3) . . . . no P4 P5 P6 W4 126.95(11) . . . . no W4 P6 C7 C8 -123.9(7) . . . . no P5 P6 C7 C8 3.7(8) . . . . no W4 P6 C7 C12 51.3(8) . . . . no P5 P6 C7 C12 178.9(7) . . . . no P1 C1 C2 P3 0.8(10) . . . . no C6 C1 C2 P3 173.5(7) . . . . no C6 C1 C2 C3 -0.4(13) . . . . no P1 C1 C6 C5 173.9(7) . . . . no C2 C1 C6 C5 1.5(13) . . . . no P1 C1 C2 C3 -173.1(7) . . . . no C1 C2 C3 C4 0.2(13) . . . . no P3 C2 C3 C4 -173.5(7) . . . . no C2 C3 C4 C5 -1.2(13) . . . . no C3 C4 C5 C6 2.4(14) . . . . no C4 C5 C6 C1 -2.6(13) . . . . no C8 C7 C12 C11 -2.1(14) . . . . no P6 C7 C8 P4 -3.7(11) . . . . no P6 C7 C8 C9 175.9(7) . . . . no C12 C7 C8 P4 -178.8(7) . . . . no C12 C7 C8 C9 0.8(13) . . . . no P6 C7 C12 C11 -177.4(7) . . . . no P4 C8 C9 C10 -179.4(7) . . . . no C7 C8 C9 C10 1.0(13) . . . . no C8 C9 C10 C11 -1.5(14) . . . . no C9 C10 C11 C12 0.3(15) . . . . no C10 C11 C12 C7 1.6(14) . . . . no 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 Cl1 O3 3.163(9) . 1_455 no Cl1 O19 3.271(10) . . no Cl1 O7 3.332(8) . 2_665 no Cl1 C19 3.464(11) . 2_665 no Cl2 O18 3.300(10) . . no Cl2 C30 3.492(13) . . no Cl2 O7 3.377(10) . 2_665 no P1 C13 3.244(9) . . no P1 C14 3.133(10) . . no P1 C15 3.359(11) . . no P1 C16 3.243(12) . . no P3 C18 3.169(9) . . no P3 C19 3.349(10) . . no P3 C20 3.403(10) . . no P3 C21 3.127(10) . . no P4 C24 3.219(10) . . no P4 C23 3.355(10) . . no P4 C25 3.041(9) . . no P4 C26 3.340(10) . . no P6 C29 3.301(10) . . no P6 C15 3.693(9) . . no P6 C28 3.289(10) . . no P6 C30 3.101(11) . . no P6 C31 3.158(10) . . no O1 O13 3.123(10) . 1_655 no O1 C6 3.340(12) . . no O1 C25 3.353(12) . 1_655 no O1 C17 3.177(12) . 2_866 no O1 O4 3.205(11) . 2_866 no O1 C16 3.144(13) . 2_866 no O1 O5 3.187(11) . 2_866 no O2 O19 2.995(11) . 1_655 no O2 C11 3.280(13) . 2_765 no O2 C10 3.284(12) . 2_765 no O3 Cl1 3.163(9) . 1_655 no O3 O6 3.106(9) . 2_765 no O3 C29 3.397(12) . . no O4 O13 3.236(10) . 2_766 no O4 O12 3.211(11) . 2_766 no O4 C25 3.268(12) . 2_766 no O4 C24 3.280(13) . 2_766 no O4 O1 3.205(11) . 2_866 no O5 O1 3.187(11) . 2_866 no O5 C28 3.407(12) . 1_655 no O5 C31 3.350(12) . 1_655 no O6 O3 3.106(9) . 2_765 no O7 C26 3.345(11) . . no O7 O11 3.158(10) . . no O7 C23 3.243(11) . . no O7 C23 3.264(12) . 2_655 no O7 Cl2 3.377(10) . 2_665 no O7 O11 2.980(10) . 2_655 no O7 C40 3.397(18) . 2_665 no O7 Cl1 3.332(8) . 2_665 no O8 C21 3.353(11) . 2_755 no O8 O9 3.136(9) . 2_755 no O8 C2 3.376(11) . 2_755 no O8 C3 3.287(11) . 2_755 no O9 O8 3.136(9) . 2_755 no O9 O18 3.203(10) . 2_765 no O10 O15 3.188(11) . 2_655 no O10 C5 3.283(12) . 2_755 no O10 O18 3.009(11) . 2_765 no O11 C20 3.352(12) . . no O11 C19 3.238(12) . . no O11 O7 3.158(10) . . no O11 O7 2.980(10) . 2_655 no O11 C3 3.410(11) . . no O12 O4 3.211(11) . 2_766 no O12 C29 3.321(12) . 2_766 no O12 O17 3.128(11) . 2_766 no O12 C28 3.414(12) . 2_766 no O12 C5 3.332(11) . . no O12 C4 3.342(12) . . no O13 O1 3.123(10) . 1_455 no O13 O4 3.236(10) . 2_766 no O13 C28 3.189(11) . . no O13 C31 3.359(12) . . no O13 C13 3.175(11) . 1_455 no O13 O16 3.106(9) . . no O13 C17 3.394(12) . 1_455 no O13 C14 3.215(11) . 1_455 no O15 C22 3.227(12) . 2_655 no O15 C19 3.419(12) . 2_655 no O15 O10 3.188(11) . 2_655 no O16 C6 3.236(11) . 2_766 no O16 O13 3.106(9) . . no O17 C40 3.365(19) . 2_776 no O17 O12 3.128(11) . 2_766 no O18 O9 3.203(10) . 2_765 no O18 C22 3.149(12) . 2_765 no O18 Cl2 3.300(10) . . no O18 C4 3.367(12) . 1_565 no O18 O10 3.009(11) . 2_765 no O18 O20 3.194(12) . 2_776 no O18 C21 3.271(12) . 2_765 no O19 C17 3.412(12) . 1_455 no O19 C14 3.156(12) . 1_455 no O19 O2 2.995(11) . 1_455 no O19 Cl1 3.271(10) . . no O20 C30 3.257(14) . 2_776 no O20 O18 3.194(12) . 2_776 no O1 H25 2.7000 . . no O2 H30 2.7100 . 2_765 no O2 H29 2.7100 . 2_765 no O3 H2 2.7600 . . no O6 H2 2.9100 . 2_765 no O7 H28 2.7600 . . no O8 H22 2.7600 . . no O9 H23 2.8300 . 2_755 no O9 H31 2.8700 . 2_765 no O10 H24 2.8300 . 2_755 no O11 H22 2.6900 . . no O14 H30 2.8400 . 2_665 no O14 H28 2.8700 . . no O15 H40A 2.8000 . 1_545 no O16 H25 2.7700 . 2_766 no O17 H40B 2.6300 . 2_776 no O18 H23 2.4900 . 1_565 no O18 H31 2.9100 . . no O20 H24 2.8200 . 2_766 no C2 O8 3.376(11) . 2_755 no C3 O11 3.410(11) . . no C3 C20 3.481(13) . . no C3 C23 3.435(12) . . no C3 C24 3.567(13) . . no C3 O8 3.287(11) . 2_755 no C3 C20 3.507(13) . 2_755 no C4 C22 3.472(13) . 2_755 no C4 C21 3.484(13) . 2_755 no C4 O12 3.342(12) . . no C4 O18 3.367(12) . 1_545 no C5 O12 3.332(11) . . no C5 O10 3.283(12) . 2_755 no C6 O1 3.340(12) . . no C6 C13 3.247(13) . . no C6 O16 3.236(11) . 2_766 no C9 C18 3.373(12) . . no C9 C19 3.567(13) . . no C9 C26 3.322(13) . . no C10 O2 3.284(12) . 2_765 no C11 O2 3.280(13) . 2_765 no C12 C30 3.574(14) . . no C12 C31 3.421(13) . . no C13 C16 2.943(14) . . no C13 P1 3.244(9) . . no C13 O13 3.175(11) . 1_655 no C13 C1 3.540(12) . . no C13 C6 3.247(13) . . no C13 C14 2.817(15) . . no C13 C17 2.749(15) . . no C14 O13 3.215(11) . 1_655 no C14 P1 3.133(10) . . no C14 P2 3.481(10) . . no C14 C17 2.897(14) . . no C14 O19 3.156(12) . 1_655 no C14 C13 2.817(15) . . no C14 C15 2.924(14) . . no C15 C16 2.914(15) . . no C15 C14 2.924(14) . . no C15 C17 2.831(13) . . no C15 P1 3.359(11) . . no C15 P6 3.693(9) . . no C16 P1 3.243(12) . . no C16 C15 2.914(15) . . no C16 C17 2.912(14) . . no C16 C13 2.943(14) . . no C16 O1 3.144(13) . 2_866 no C17 O19 3.412(12) . 1_655 no C17 C15 2.831(13) . . no C17 C14 2.897(14) . . no C17 O13 3.394(12) . 1_655 no C17 O1 3.177(12) . 2_866 no C17 C13 2.749(15) . . no C17 C16 2.912(14) . . no C18 P3 3.169(9) . . no C18 C21 2.901(13) . . no C18 C22 2.835(13) . . no C18 C9 3.373(12) . . no C18 P2 3.559(9) . . no C18 C19 2.955(13) . . no C19 O15 3.419(12) . 2_655 no C19 O11 3.238(12) . . no C19 C20 2.822(14) . . no C19 P3 3.349(10) . . no C19 Cl1 3.464(11) . 2_665 no C19 C9 3.567(13) . . no C19 C18 2.955(13) . . no C19 C23 3.377(13) . . no C19 C22 2.867(13) . . no C20 P3 3.403(10) . . no C20 C19 2.822(14) . . no C20 C22 2.856(13) . . no C20 O11 3.352(12) . . no C20 C21 2.924(14) . . no C20 C3 3.507(13) . 2_755 no C20 C3 3.481(13) . . no C21 C18 2.901(13) . . no C21 P2 3.547(10) . . no C21 C22 2.881(13) . . no C21 P3 3.127(10) . . no C21 C20 2.924(14) . . no C21 O18 3.271(12) . 2_765 no C21 O8 3.353(11) . 2_755 no C21 C4 3.484(13) . 2_755 no C22 C18 2.835(13) . . no C22 C21 2.881(13) . . no C22 O18 3.149(12) . 2_765 no C22 C20 2.856(13) . . no C22 C19 2.867(13) . . no C22 O15 3.227(12) . 2_655 no C22 C4 3.472(13) . 2_755 no C23 C3 3.435(12) . . no C23 C19 3.377(13) . . no C23 C26 2.896(13) . . no C23 P4 3.355(10) . . no C23 O7 3.243(11) . . no C23 O7 3.264(12) . 2_655 no C23 C27 2.917(13) . . no C23 C24 2.936(14) . . no C24 C23 2.936(14) . . no C24 P5 3.558(10) . . no C24 P4 3.219(10) . . no C24 C3 3.567(13) . . no C24 O4 3.280(13) . 2_766 no C24 C27 2.856(14) . . no C24 C25 2.913(14) . . no C25 P5 3.536(9) . . no C25 O1 3.353(12) . 1_455 no C25 P4 3.041(9) . . no C25 C24 2.913(14) . . no C25 O4 3.268(12) . 2_766 no C25 C27 2.896(14) . . no C25 C26 2.887(13) . . no C26 C23 2.896(13) . . no C26 P4 3.340(10) . . no C26 O7 3.345(11) . . no C26 C25 2.887(13) . . no C26 C27 2.807(14) . . no C26 C9 3.322(13) . . no C27 C23 2.917(13) . . no C27 C26 2.807(14) . . no C27 C24 2.856(14) . . no C27 C25 2.896(14) . . no C28 O12 3.414(12) . 2_766 no C28 C32 2.913(14) . . no C28 O13 3.189(11) . . no C28 P6 3.289(10) . . no C28 C31 2.939(13) . . no C28 O5 3.407(12) . 1_455 no C28 P5 3.549(10) . . no C28 C29 2.880(14) . . no C29 P6 3.301(10) . . no C29 O12 3.321(12) . 2_766 no C29 O3 3.397(12) . . no C29 C30 2.858(14) . . no C29 C32 2.899(15) . . no C29 C28 2.880(14) . . no C30 P6 3.101(11) . . no C30 C31 2.976(14) . . no C30 C12 3.574(14) . . no C30 Cl2 3.492(13) . . no C30 C29 2.858(14) . . no C30 C32 2.926(14) . . no C30 O20 3.257(14) . 2_776 no C31 O5 3.350(12) . 1_455 no C31 C7 3.362(13) . . no C31 C12 3.421(13) . . no C31 O13 3.359(12) . . no C31 P6 3.158(10) . . no C31 C32 2.836(13) . . no C31 C28 2.939(13) . . no C31 C30 2.976(14) . . no C32 C30 2.926(14) . . no C32 C28 2.913(14) . . no C32 C29 2.899(15) . . no C32 C31 2.836(13) . . no C40 O7 3.397(18) . 2_665 no C40 O17 3.365(19) . 2_776 no C13 H25 2.6100 . . no C14 H1 3.0000 . . no C15 H2 2.7800 . . no C19 H28 2.7500 . . no C20 H22 2.7200 . . no C21 H1 3.0300 . . no C21 H23 2.9200 . 2_755 no C23 H22 2.9700 . . no C26 H28 2.8000 . . no C27 H40A 3.0300 . 1_545 no C30 H31 2.8000 . . no H1 C14 3.0000 . . no H1 C21 3.0300 . . no H2 O3 2.7600 . . no H2 O6 2.9100 . 2_765 no H2 C15 2.7800 . . no H22 C20 2.7200 . . no H22 C23 2.9700 . . no H22 O11 2.6900 . . no H22 O8 2.7600 . . no H23 C21 2.9200 . 2_755 no H23 O18 2.4900 . 1_545 no H23 O9 2.8300 . 2_755 no H24 O20 2.8200 . 2_766 no H24 O10 2.8300 . 2_755 no H25 O1 2.7000 . . no H25 C13 2.6100 . . no H25 O16 2.7700 . 2_766 no H28 O7 2.7600 . . no H28 O14 2.8700 . . no H28 C26 2.8000 . . no H28 C19 2.7500 . . no H29 O2 2.7100 . 2_765 no H30 O14 2.8400 . 2_665 no H30 O2 2.7100 . 2_765 no H31 O9 2.8700 . 2_765 no H31 O18 2.9100 . . no H31 C30 2.8000 . . no H40A O15 2.8000 . 1_565 no H40A C27 3.0300 . 1_565 no H40B O17 2.6300 . 2_776 no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C4 H23 O18 0.9500 2.4900 3.367(12) 153.00 1_545 yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; _vrf_REFLT03_pw2ph ; PROBLEM: Reflection count < 85% complete (theta max?) RESPONSE: All crystals were intergrown small rods. A treatment of the data to enable the refinements with the shelxl hklf5 option was not possible, therefore only the uninfluenced reflections were used for structural calculations. ; _vrf_PLAT022_pw2ph ; PROBLEM: Ratio Unique / Expected Reflections too Low .... 0.79 RESPONSE: All crystals were intergrown small rods. A treatment of the data to enable the refinements with the shelxl hklf5 option was not possible, therefore only the uninfluenced reflections were used for structural calculations. ; _vrf_PLAT029_pw2ph ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.79 RESPONSE: All crystals were intergrown small rods. A treatment of the data to enable the refinements with the shelxl hklf5 option was not possible, therefore only the uninfluenced reflections were used for structural calculations. ; # end Validation Reply Form #===END