Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Anthony C. Willis' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_email willis@rsc.anu.edu.au _publ_section_title ; A Mercury Bis(tricarbido) Complex: [Hg{CCCW(CO)2Tp}2(dmso)4](dmso)2 (Tp = hydrotrispyrazolylborate) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address A.C.Willis ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; R.D.Dewhurst ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; A.F.Hill ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [(C~9~H~10~BN~6~)W(CO)~2~C~3~HgC~3~W(CO)~2~(C~9~H~10~BN~6~)].6(Me~2~SO) is reported. ; _publ_section_comment #Text of the paper ; The unit cell contains one [(C~9~H~10~BN~6~)W(CO)~2~C~3~HgC~3~W(CO)~2~(C~9~H~10~BN~6~)] molecule and six dimethylsulphoxide molecules of solvation. The [(C~9~H~10~BN~6~)W(CO)~2~C~3~HgC~3~W(CO)~2~(C~9~H~10~BN~6~)] molecule is centred on a crystallographic inversion. There are additional longer contacts between the Hg atom and O atoms of four adjacent dimethylsulphoxide molecules, so the molecule could, alternatively, be regarded as [(C~9~H~10~BN~6~)W(CO)~2~C~3~Hg(OSMe~2~)~4~C~3~W(CO)~2~(C~9~H~10~BN~6~)]. All three unique dimethylsulphoxide molecules have some degree of disorder. In each case there are two orientations for the molecule with the C and O atoms in common (or very close to it) and the S atom having alternative sites on either side of this plane. In molecules 1 and 3 the relative occupancies are about 0.93:0.07 so the predominant S site has been refined with anisotropic displacement parameters and the minor one has been assigned an isotropic displacement parameter set equal to U~equiv~ of the major. In molecule 2 the relative occupancies are more equal (0.62:0.38) so the S sites were refined with a common isotropic displacement parameter. One of the C atoms was best regarded as being on two sites also and was treated in a similar manner. Restraints were imposed on the bond lengths within the dimethylsulphoxide molecules to aid sensible refinement of the low-occupancy sites. Peaks in the final difference electron density map are generally all of similar height and are located within disordered regions of the structure or near the W atom. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms were included at idealized positions and ride on the atom to which they are attached. ; _publ_section_exptl_prep ; The compound was prepared by RDD and recrystallized from dimethylsulphoxide. The sample ID was RD-3,138. ; #========================================================================== data_rian18 _database_code_depnum_ccdc_archive 'CCDC 245028' _audit_creation_date 04-10-05 _audit_creation_method CRYSTALS_ver_12-03-99 # 5100958 rian18 _audit_update_record ; 2004-05-10 - Report on C40 H56 B2 Hg1 N12 O10 S6 W2 by Anthony C. Willis for Anthony F. Hill and Rian Dewhurst 2004-05-11- passes checkcif tests with minor warnings ; _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 9.3324(2) _cell_angle_alpha 66.7946(8) _cell_length_b 12.4640(2) _cell_angle_beta 84.4796(7) _cell_length_c 13.5127(2) _cell_angle_gamma 86.4672(8) _cell_volume 1437.44(4) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Hg ' -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246 12.6089 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C40 H56 B2 Hg1 N12 O10 S6 W2 ' _chemical_formula_moiety ' C28 H20 B2 Hg N12 O4 W2, 6(C2 H6 O S) ' _chemical_compound_source ; ? ; _chemical_formula_weight 1647.27 _cell_measurement_reflns_used 21365 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.13 _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 6.933 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 2.0 deg at rate 800 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 95 percent of data collected with 2-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.050 -1 0 0 0.080 0 1 0 0.010 0 -1 0 0.040 0 0 1 0.010 0 0 -1 0.010 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; # Sheldrick geometric definitions 0.71 0.87 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 31300 _reflns_number_total 6594 _diffrn_reflns_av_R_equivalents 0.06 # Number of reflections with Friedels Law is 6594 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6600 _diffrn_reflns_theta_min 2.637 _diffrn_reflns_theta_max 27.494 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.494 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -14 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -0.90 _refine_diff_density_max 0.90 _refine_ls_number_reflns 4582 _refine_ls_number_restraints 18 _refine_ls_number_parameters 337 #_refine_ls_R_factor_ref 0.0262 _refine_ls_wR_factor_ref 0.0288 _refine_ls_goodness_of_fit_ref 1.1270 #_reflns_number_all 6575 _refine_ls_R_factor_all 0.0446 _refine_ls_wR_factor_all 0.0433 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4582 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_gt 0.0288 _refine_ls_shift/su_max 0.001463 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.368 0.107 0.105 ; _refine_ls_extinction_coef 36(2) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Larson, A.C. (1970). The Inclusion of Secondary Extinction in Least-Squares Refinement in Crystal Structures. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 291-294 Altomare, A., Cascarano, G., Giacovazzo C., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Hg1 Hg 0.5000 0.5000 0.5000 0.0457 1.0000 Uani S . . . . . W1 W 0.21511(2) 0.766056(18) 0.047307(15) 0.0290 1.0000 Uani . . . . . . S10 S 0.17498(18) 0.55105(14) 0.70527(13) 0.0452 0.929(3) Uani D . P . . . S11 S 0.3090(19) 0.5498(13) 0.7127(11) 0.0452 0.071(3) Uiso D . P . . . S20 S 0.8258(3) 0.7400(3) 0.4495(2) 0.0578(6) 0.623(3) Uiso D . P . . . S21 S 0.8127(5) 0.6355(4) 0.5090(4) 0.0578(6) 0.377(3) Uiso D . P . . . S30 S 0.74118(17) 0.10458(14) 0.52012(12) 0.0431 0.929(3) Uani D . P . . . S31 S 0.6549(18) 0.0629(13) 0.5908(13) 0.0431 0.071(3) Uiso D . P . . . O1 O 0.2618(5) 0.5975(4) 0.5999(3) 0.0589 1.0000 Uani D . . . . . O2 O 0.6907(6) 0.7056(6) 0.4222(5) 0.0820 1.0000 Uani D . . . . . O3 O 0.7345(5) -0.0266(4) 0.5634(4) 0.0541 1.0000 Uani D . . . . . O5 O -0.0411(5) 0.8374(5) 0.1803(4) 0.0622 1.0000 Uani . . . . . . O6 O 0.0915(5) 0.5193(4) 0.0980(4) 0.0573 1.0000 Uani . . . . . . N11 N 0.1111(4) 0.8365(4) -0.1117(3) 0.0322 1.0000 Uani . . . . . . N12 N 0.1870(4) 0.9064(3) -0.2048(3) 0.0304 1.0000 Uani . . . . . . N21 N 0.3997(4) 0.7440(3) -0.0590(3) 0.0305 1.0000 Uani . . . . . . N22 N 0.4357(4) 0.8295(4) -0.1579(3) 0.0323 1.0000 Uani . . . . . . N31 N 0.2918(4) 0.9462(4) -0.0175(3) 0.0328 1.0000 Uani . . . . . . N32 N 0.3402(4) 1.0033(3) -0.1237(3) 0.0312 1.0000 Uani . . . . . . C1 C 0.2985(5) 0.6939(4) 0.1770(4) 0.0325 1.0000 Uani . . . . . . C2 C 0.3528(6) 0.6322(5) 0.2744(4) 0.0384 1.0000 Uani . . . . . . C3 C 0.4049(6) 0.5795(5) 0.3601(4) 0.0443 1.0000 Uani . . . . . . C5 C 0.0483(6) 0.8106(5) 0.1303(4) 0.0382 1.0000 Uani . . . . . . C6 C 0.1358(6) 0.6106(5) 0.0803(4) 0.0384 1.0000 Uani . . . . . . C13 C 0.1033(6) 0.9351(5) -0.2889(4) 0.0406 1.0000 Uani . . . . . . C14 C -0.0268(6) 0.8823(5) -0.2505(5) 0.0434 1.0000 Uani . . . . . . C15 C -0.0176(6) 0.8217(5) -0.1401(4) 0.0391 1.0000 Uani . . . . . . C23 C 0.5596(6) 0.7976(5) -0.2006(4) 0.0382 1.0000 Uani . . . . . . C24 C 0.6048(6) 0.6899(5) -0.1293(5) 0.0437 1.0000 Uani . . . . . . C25 C 0.5013(6) 0.6602(4) -0.0429(4) 0.0369 1.0000 Uani . . . . . . C33 C 0.3776(5) 1.1120(4) -0.1408(5) 0.0381 1.0000 Uani . . . . . . C34 C 0.3559(6) 1.1266(5) -0.0447(5) 0.0436 1.0000 Uani . . . . . . C35 C 0.3024(6) 1.0213(5) 0.0297(5) 0.0396 1.0000 Uani . . . . . . C101 C 0.2288(9) 0.6214(7) 0.7863(6) 0.0701 1.0000 Uani D . . . . . C102 C 0.2439(8) 0.4096(5) 0.7809(5) 0.0588 1.0000 Uani D . . . . . C201 C 0.7917(10) 0.6962(9) 0.5992(7) 0.0919 1.0000 Uani D . . . . . C202 C 0.9460(14) 0.6231(11) 0.4538(12) 0.079(3) 0.623(3) Uiso D . P . . . C212 C 0.961(2) 0.7243(19) 0.4486(18) 0.079(3) 0.377(3) Uiso D . P . . . C301 C 0.5695(7) 0.1577(6) 0.4757(6) 0.0648 1.0000 Uani D . . . . . C302 C 0.7303(11) 0.1438(7) 0.6340(6) 0.0774 1.0000 Uani D . . . . . B1 B 0.3413(6) 0.9414(5) -0.2018(4) 0.0331 1.0000 Uani . . . . . . H1 H 0.3792(6) 0.9939(5) -0.2759(4) 0.0381 1.0000 Uiso R . . . . . H131 H 0.1316(6) 0.9861(5) -0.3657(4) 0.0500 1.0000 Uiso R . . . . . H141 H -0.1104(6) 0.8865(5) -0.2930(5) 0.0529 1.0000 Uiso R . . . . . H151 H -0.0960(6) 0.7738(5) -0.0890(4) 0.0470 1.0000 Uiso R . . . . . H231 H 0.6101(6) 0.8445(5) -0.2721(4) 0.0465 1.0000 Uiso R . . . . . H241 H 0.6928(6) 0.6434(5) -0.1380(5) 0.0548 1.0000 Uiso R . . . . . H251 H 0.5027(6) 0.5858(4) 0.0228(4) 0.0445 1.0000 Uiso R . . . . . H331 H 0.4149(5) 1.1722(4) -0.2116(5) 0.0443 1.0000 Uiso R . . . . . H341 H 0.3747(6) 1.1977(5) -0.0313(5) 0.0544 1.0000 Uiso R . . . . . H351 H 0.2754(6) 1.0041(5) 0.1078(5) 0.0498 1.0000 Uiso R . . . . . H1011 H 0.1717(9) 0.5916(7) 0.8579(6) 0.0878 0.9000 Uiso R . . . . . H1012 H 0.2113(9) 0.7076(7) 0.7495(6) 0.0878 0.9000 Uiso R . . . . . H1013 H 0.3336(9) 0.6049(7) 0.7972(6) 0.0878 0.9000 Uiso R . . . . . H1014 H 0.2630(9) 0.5872(7) 0.8606(6) 0.0878 0.1000 Uiso R . . . . . H1015 H 0.2535(9) 0.7058(7) 0.7512(6) 0.0878 0.1000 Uiso R . . . . . H1016 H 0.1220(9) 0.6140(7) 0.7909(6) 0.0878 0.1000 Uiso R . . . . . H1021 H 0.1871(8) 0.3763(5) 0.8525(5) 0.0665 0.9000 Uiso R . . . . . H1022 H 0.3472(8) 0.4145(5) 0.7924(5) 0.0665 0.9000 Uiso R . . . . . H1023 H 0.2363(8) 0.3582(5) 0.7407(5) 0.0665 0.9000 Uiso R . . . . . H1024 H 0.2747(8) 0.3768(5) 0.8563(5) 0.0665 0.1000 Uiso R . . . . . H1025 H 0.1363(8) 0.4127(5) 0.7832(5) 0.0665 0.1000 Uiso R . . . . . H1026 H 0.2832(8) 0.3588(5) 0.7425(5) 0.0665 0.1000 Uiso R . . . . . H2011 H 0.8770(10) 0.7153(9) 0.6282(7) 0.1232 0.6000 Uiso R . . . . . H2012 H 0.7046(10) 0.7397(9) 0.6147(7) 0.1232 0.6000 Uiso R . . . . . H2013 H 0.7752(10) 0.6104(9) 0.6346(7) 0.1232 0.6000 Uiso R . . . . . H2014 H 0.8616(10) 0.6591(9) 0.6556(7) 0.1232 0.4000 Uiso R . . . . . H2015 H 0.8097(10) 0.7817(9) 0.5623(7) 0.1232 0.4000 Uiso R . . . . . H2016 H 0.6912(10) 0.6843(9) 0.6340(7) 0.1232 0.4000 Uiso R . . . . . H2021 H 1.0425(14) 0.6376(11) 0.4719(12) 0.0946 0.6000 Uiso R . . . . . H2022 H 0.9080(14) 0.5486(11) 0.5101(12) 0.0946 0.6000 Uiso R . . . . . H2023 H 0.9555(14) 0.6172(11) 0.3818(12) 0.0946 0.6000 Uiso R . . . . . H2121 H 1.045(2) 0.6922(19) 0.4929(18) 0.0946 0.4000 Uiso R . . . . . H2122 H 0.937(2) 0.8053(19) 0.4441(18) 0.0946 0.4000 Uiso R . . . . . H2123 H 0.985(2) 0.7261(19) 0.3743(18) 0.0946 0.4000 Uiso R . . . . . H3011 H 0.5674(7) 0.2450(6) 0.4458(6) 0.0710 0.9000 Uiso R . . . . . H3012 H 0.4951(7) 0.1277(6) 0.5378(6) 0.0710 0.9000 Uiso R . . . . . H3013 H 0.5487(7) 0.1306(6) 0.4181(6) 0.0710 0.9000 Uiso R . . . . . H3014 H 0.5139(7) 0.2203(6) 0.4928(6) 0.0710 0.1000 Uiso R . . . . . H3015 H 0.6440(7) 0.1941(6) 0.4148(6) 0.0710 0.1000 Uiso R . . . . . H3016 H 0.5025(7) 0.1124(6) 0.4543(6) 0.0710 0.1000 Uiso R . . . . . H3021 H 0.7343(11) 0.2306(7) 0.6087(6) 0.0969 0.9000 Uiso R . . . . . H3022 H 0.8128(11) 0.1065(7) 0.6788(6) 0.0969 0.9000 Uiso R . . . . . H3023 H 0.6375(11) 0.1164(7) 0.6784(6) 0.0969 0.9000 Uiso R . . . . . H3024 H 0.6572(11) 0.1994(7) 0.6480(6) 0.0969 0.1000 Uiso R . . . . . H3025 H 0.7745(11) 0.0946(7) 0.7026(6) 0.0969 0.1000 Uiso R . . . . . H3026 H 0.8069(11) 0.1888(7) 0.5788(6) 0.0969 0.1000 Uiso 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 Hg1 0.0558(2) 0.05049(19) 0.02544(15) -0.00897(13) -0.01602(13) 0.01771(14) W1 0.03136(11) 0.03063(11) 0.02181(10) -0.00597(7) -0.00780(7) 0.00169(7) S10 0.0470(9) 0.0464(9) 0.0408(8) -0.0153(7) -0.0075(7) 0.0039(7) S30 0.0487(9) 0.0444(8) 0.0372(8) -0.0168(7) -0.0049(6) -0.0003(7) O1 0.077(3) 0.049(3) 0.042(2) -0.011(2) 0.003(2) 0.005(2) O2 0.069(3) 0.111(5) 0.086(4) -0.056(4) -0.021(3) -0.002(3) O3 0.071(3) 0.041(2) 0.053(3) -0.018(2) -0.025(2) 0.006(2) O5 0.045(2) 0.087(4) 0.061(3) -0.040(3) 0.005(2) 0.009(2) O6 0.062(3) 0.042(2) 0.067(3) -0.020(2) 0.003(2) -0.014(2) N11 0.031(2) 0.036(2) 0.027(2) -0.0080(17) -0.0096(16) 0.0022(17) N12 0.037(2) 0.029(2) 0.0238(19) -0.0083(16) -0.0099(16) 0.0073(16) N21 0.033(2) 0.028(2) 0.030(2) -0.0093(17) -0.0071(16) 0.0032(16) N22 0.032(2) 0.033(2) 0.028(2) -0.0081(17) -0.0030(16) 0.0028(17) N31 0.035(2) 0.037(2) 0.028(2) -0.0129(17) -0.0090(16) 0.0023(17) N32 0.030(2) 0.030(2) 0.031(2) -0.0073(17) -0.0072(16) 0.0019(16) C1 0.036(3) 0.032(2) 0.029(2) -0.010(2) -0.006(2) 0.003(2) C2 0.041(3) 0.042(3) 0.030(2) -0.012(2) -0.006(2) 0.004(2) C3 0.051(3) 0.052(3) 0.024(3) -0.008(2) -0.009(2) 0.008(3) C5 0.040(3) 0.039(3) 0.030(3) -0.006(2) -0.010(2) -0.001(2) C6 0.036(3) 0.047(3) 0.027(2) -0.011(2) -0.002(2) 0.005(2) C13 0.052(3) 0.042(3) 0.031(3) -0.016(2) -0.017(2) 0.011(2) C14 0.042(3) 0.048(3) 0.042(3) -0.016(3) -0.025(2) 0.009(2) C15 0.032(3) 0.044(3) 0.041(3) -0.015(2) -0.012(2) 0.000(2) C23 0.033(3) 0.043(3) 0.040(3) -0.020(2) 0.002(2) 0.002(2) C24 0.039(3) 0.046(3) 0.052(3) -0.026(3) -0.007(2) 0.010(2) C25 0.041(3) 0.029(3) 0.041(3) -0.013(2) -0.014(2) 0.008(2) C33 0.034(3) 0.028(2) 0.049(3) -0.010(2) -0.007(2) -0.002(2) C34 0.043(3) 0.034(3) 0.059(4) -0.022(3) -0.017(3) 0.004(2) C35 0.042(3) 0.041(3) 0.041(3) -0.021(2) -0.015(2) 0.009(2) C101 0.097(6) 0.060(4) 0.062(4) -0.033(4) -0.002(4) -0.012(4) C102 0.073(5) 0.044(3) 0.050(4) -0.009(3) 0.003(3) -0.001(3) C201 0.101(7) 0.106(7) 0.101(7) -0.072(6) -0.048(6) 0.039(6) C301 0.058(4) 0.056(4) 0.064(4) -0.001(3) -0.022(3) -0.002(3) C302 0.123(7) 0.060(5) 0.059(4) -0.033(4) -0.024(5) 0.019(5) B1 0.035(3) 0.033(3) 0.027(3) -0.008(2) -0.002(2) -0.002(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 . O1 2_666 2.937(4) no Hg1 . O2 2_666 2.986(6) no Hg1 . C3 2_666 2.020(5) no Hg1 . S11 2_666 3.480(15) no Hg1 . S21 2_666 3.495(5) no Hg1 . S11 . 3.480(15) no Hg1 . S21 . 3.495(5) no Hg1 . O1 . 2.937(4) yes Hg1 . O2 . 2.986(6) yes Hg1 . C3 . 2.020(5) yes W1 . N11 . 2.267(4) yes W1 . N21 . 2.210(4) yes W1 . N31 . 2.202(4) yes W1 . C1 . 1.849(5) yes W1 . C5 . 2.009(6) yes W1 . C6 . 1.984(6) yes S10 . O1 . 1.485(4) yes S10 . C101 . 1.771(7) yes S10 . C102 . 1.770(6) yes S11 . O1 . 1.501(14) yes S11 . C101 . 1.680(15) yes S11 . C102 . 1.740(15) yes S20 . O2 . 1.480(6) yes S20 . C201 . 1.876(9) yes S20 . C202 . 1.768(12) yes S21 . O2 . 1.662(7) yes S21 . C201 . 1.662(8) yes S21 . C212 . 1.750(15) yes S30 . O3 . 1.507(4) yes S30 . C301 . 1.763(6) yes S30 . C302 . 1.782(7) yes S31 . O3 . 1.451(14) yes S31 . C301 . 1.768(15) yes S31 . C302 . 1.576(14) yes O5 . C5 . 1.140(7) yes O6 . C6 . 1.160(7) yes N11 . N12 . 1.372(6) yes N11 . C15 . 1.340(6) yes N12 . C13 . 1.359(6) yes N12 . B1 . 1.539(7) yes N21 . N22 . 1.367(6) yes N21 . C25 . 1.333(6) yes N22 . C23 . 1.350(6) yes N22 . B1 . 1.539(7) yes N31 . N32 . 1.371(6) yes N31 . C35 . 1.337(7) yes N32 . C33 . 1.344(6) yes N32 . B1 . 1.533(7) yes C1 . C2 . 1.365(7) yes C2 . C3 . 1.216(7) yes C13 . C14 . 1.372(8) yes C13 . H131 . 1.000 no C14 . C15 . 1.391(8) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C23 . C24 . 1.378(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.385(8) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C33 . C34 . 1.376(8) yes C33 . H331 . 1.000 no C34 . C35 . 1.388(8) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C101 . H1011 . 1.000 no C101 . H1012 . 1.000 no C101 . H1013 . 1.000 no C101 . H1014 . 1.000 no C101 . H1015 . 1.000 no C101 . H1016 . 1.000 no C102 . H1021 . 1.000 no C102 . H1022 . 1.000 no C102 . H1023 . 1.000 no C102 . H1024 . 1.000 no C102 . H1025 . 1.000 no C102 . H1026 . 1.000 no C201 . H2011 . 1.000 no C201 . H2012 . 1.000 no C201 . H2013 . 1.000 no C201 . H2014 . 1.000 no C201 . H2015 . 1.000 no C201 . H2016 . 1.000 no C202 . H2021 . 1.000 no C202 . H2022 . 1.000 no C202 . H2023 . 1.000 no C212 . H2121 . 1.000 no C212 . H2122 . 1.000 no C212 . H2123 . 1.000 no C301 . H3011 . 1.000 no C301 . H3012 . 1.000 no C301 . H3013 . 1.000 no C301 . H3014 . 1.000 no C301 . H3015 . 1.000 no C301 . H3016 . 1.000 no C302 . H3021 . 1.000 no C302 . H3022 . 1.000 no C302 . H3023 . 1.000 no C302 . H3024 . 1.000 no C302 . H3025 . 1.000 no C302 . H3026 . 1.000 no B1 . H1 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 2_666 Hg1 . O2 2_666 97.61(15) no O1 2_666 Hg1 . C3 2_666 86.77(19) no O2 2_666 Hg1 . C3 2_666 86.5(2) no O1 2_666 Hg1 . S11 2_666 25.3(3) no O2 2_666 Hg1 . S11 2_666 98.3(3) no C3 2_666 Hg1 . S11 2_666 112.1(3) no O1 2_666 Hg1 . S21 2_666 106.84(13) no O2 2_666 Hg1 . S21 2_666 28.35(13) no C3 2_666 Hg1 . S21 2_666 113.46(19) no S11 2_666 Hg1 . S21 2_666 95.4(3) no O1 2_666 Hg1 . S11 . 154.7(3) no O2 2_666 Hg1 . S11 . 81.7(3) no C3 2_666 Hg1 . S11 . 67.9(3) no S11 2_666 Hg1 . S11 . 179.997 no S21 2_666 Hg1 . S11 . 84.6(3) no O1 2_666 Hg1 . S21 . 73.16(13) no O2 2_666 Hg1 . S21 . 151.65(13) no C3 2_666 Hg1 . S21 . 66.54(19) no S11 2_666 Hg1 . S21 . 84.6(3) no S21 2_666 Hg1 . S21 . 179.997 no O1 2_666 Hg1 . O1 . 180.0 yes O2 2_666 Hg1 . O1 . 82.39(15) no C3 2_666 Hg1 . O1 . 93.23(19) no S11 2_666 Hg1 . O1 . 154.7(3) no S21 2_666 Hg1 . O1 . 73.16(13) no O1 2_666 Hg1 . O2 . 82.39(15) yes O2 2_666 Hg1 . O2 . 180.0 no C3 2_666 Hg1 . O2 . 93.5(2) no S11 2_666 Hg1 . O2 . 81.7(3) no S21 2_666 Hg1 . O2 . 151.65(13) no O1 2_666 Hg1 . C3 . 93.23(19) yes O2 2_666 Hg1 . C3 . 93.5(2) yes C3 2_666 Hg1 . C3 . 180.0 yes S11 2_666 Hg1 . C3 . 67.9(3) no S21 2_666 Hg1 . C3 . 66.54(19) no S11 . Hg1 . S21 . 95.4(3) no S11 . Hg1 . O1 . 25.3(3) no S21 . Hg1 . O1 . 106.84(13) no S11 . Hg1 . O2 . 98.3(3) no S21 . Hg1 . O2 . 28.35(13) no O1 . Hg1 . O2 . 97.61(15) yes S11 . Hg1 . C3 . 112.1(3) no S21 . Hg1 . C3 . 113.46(19) no O1 . Hg1 . C3 . 86.77(19) yes O2 . Hg1 . C3 . 86.5(2) yes N11 . W1 . N21 . 80.85(15) yes N11 . W1 . N31 . 80.86(15) yes N21 . W1 . N31 . 81.97(15) yes N11 . W1 . C1 . 174.28(19) yes N21 . W1 . C1 . 97.55(18) yes N31 . W1 . C1 . 104.42(19) yes N11 . W1 . C5 . 94.96(18) yes N21 . W1 . C5 . 171.78(18) yes N31 . W1 . C5 . 90.41(19) yes C1 . W1 . C5 . 87.3(2) yes N11 . W1 . C6 . 89.47(18) yes N21 . W1 . C6 . 94.59(18) yes N31 . W1 . C6 . 170.12(18) yes C1 . W1 . C6 . 85.2(2) yes C5 . W1 . C6 . 92.4(2) yes O1 . S10 . C101 . 107.9(3) yes O1 . S10 . C102 . 107.9(3) yes C101 . S10 . C102 . 97.6(4) yes Hg1 . S11 . O1 . 56.7(5) no Hg1 . S11 . C101 . 160.2(8) no O1 . S11 . C101 . 111.9(10) no Hg1 . S11 . C102 . 97.0(6) no O1 . S11 . C102 . 108.7(9) no C101 . S11 . C102 . 102.4(9) no O2 . S20 . C201 . 101.6(4) yes O2 . S20 . C202 . 102.7(6) yes C201 . S20 . C202 . 97.1(6) yes Hg1 . S21 . O2 . 58.6(3) no Hg1 . S21 . C201 . 111.8(4) no O2 . S21 . C201 . 103.6(4) no Hg1 . S21 . C202 . 122.8(6) no Hg1 . S21 . C212 . 152.9(8) no O2 . S21 . C212 . 100.1(9) no C201 . S21 . C212 . 88.2(9) no O3 . S30 . C301 . 105.8(3) yes O3 . S30 . C302 . 106.9(3) yes C301 . S30 . C302 . 98.0(4) yes O3 . S31 . C301 . 108.1(9) yes S30 . S31 . C302 . 79.7(10) yes O3 . S31 . C302 . 121.9(11) yes C301 . S31 . C302 . 106.1(9) yes Hg1 . O1 . S11 . 98.0(7) no Hg1 . O1 . S10 . 133.5(2) yes S21 . O2 . Hg1 . 93.1(3) no S20 . O2 . Hg1 . 138.9(4) yes W1 . N11 . N12 . 120.2(3) yes W1 . N11 . C15 . 133.2(4) yes N12 . N11 . C15 . 106.5(4) yes N11 . N12 . C13 . 109.2(4) yes N11 . N12 . B1 . 120.5(4) yes C13 . N12 . B1 . 130.3(4) yes W1 . N21 . N22 . 121.7(3) yes W1 . N21 . C25 . 131.6(4) yes N22 . N21 . C25 . 106.5(4) yes N21 . N22 . C23 . 109.1(4) yes N21 . N22 . B1 . 120.4(4) yes C23 . N22 . B1 . 130.5(4) yes W1 . N31 . N32 . 122.4(3) yes W1 . N31 . C35 . 131.4(4) yes N32 . N31 . C35 . 106.2(4) yes N31 . N32 . C33 . 109.6(4) yes N31 . N32 . B1 . 119.7(4) yes C33 . N32 . B1 . 130.7(4) yes W1 . C1 . C2 . 174.9(4) yes C1 . C2 . C3 . 178.0(6) yes C2 . C3 . Hg1 . 176.5(5) yes W1 . C5 . O5 . 176.3(5) yes W1 . C6 . O6 . 178.6(5) yes N12 . C13 . C14 . 108.4(5) yes N12 . C13 . H131 . 125.777 no C14 . C13 . H131 . 125.778 no C13 . C14 . C15 . 105.5(4) yes C13 . C14 . H141 . 127.272 no C15 . C14 . H141 . 127.275 no C14 . C15 . N11 . 110.4(5) yes C14 . C15 . H151 . 124.782 no N11 . C15 . H151 . 124.784 no N22 . C23 . C24 . 108.8(5) yes N22 . C23 . H231 . 125.623 no C24 . C23 . H231 . 125.623 no C23 . C24 . C25 . 104.7(5) yes C23 . C24 . H241 . 127.668 no C25 . C24 . H241 . 127.671 no C24 . C25 . N21 . 111.0(5) yes C24 . C25 . H251 . 124.502 no N21 . C25 . H251 . 124.506 no N32 . C33 . C34 . 108.5(5) yes N32 . C33 . H331 . 125.750 no C34 . C33 . H331 . 125.752 no C33 . C34 . C35 . 105.1(5) yes C33 . C34 . H341 . 127.445 no C35 . C34 . H341 . 127.443 no C34 . C35 . N31 . 110.6(5) yes C34 . C35 . H351 . 124.687 no N31 . C35 . H351 . 124.685 no S10 . C101 . H1011 . 109.467 no S10 . C101 . H1012 . 109.464 no H1011 . C101 . H1012 . 109.475 no S10 . C101 . H1013 . 109.469 no H1011 . C101 . H1013 . 109.476 no H1012 . C101 . H1013 . 109.476 no S11 . C101 . H1014 . 109.467 no S11 . C101 . H1015 . 109.467 no H1011 . C101 . H1015 . 119.795 no S11 . C101 . H1016 . 109.467 no H1014 . C101 . H1015 . 109.475 no H1014 . C101 . H1016 . 109.475 no H1015 . C101 . H1016 . 109.476 no S10 . C102 . H1021 . 109.466 no S10 . C102 . H1022 . 109.467 no H1021 . C102 . H1022 . 109.476 no S10 . C102 . H1023 . 109.466 no H1021 . C102 . H1023 . 109.476 no H1022 . C102 . H1023 . 109.476 no S11 . C102 . H1024 . 109.466 no S11 . C102 . H1025 . 109.467 no S11 . C102 . H1026 . 109.468 no H1024 . C102 . H1025 . 109.476 no H1024 . C102 . H1026 . 109.476 no H1025 . C102 . H1026 . 109.476 no S20 . C201 . H2011 . 109.461 no S20 . C201 . H2012 . 109.471 no H2011 . C201 . H2012 . 109.475 no S20 . C201 . H2013 . 109.469 no H2011 . C201 . H2013 . 109.476 no H2012 . C201 . H2013 . 109.476 no S21 . C201 . H2014 . 109.465 no S21 . C201 . H2015 . 109.460 no S21 . C201 . H2016 . 109.476 no H2014 . C201 . H2015 . 109.476 no H2014 . C201 . H2016 . 109.476 no H2015 . C201 . H2016 . 109.476 no S20 . C202 . H2021 . 109.476 no S20 . C202 . H2022 . 109.462 no H2021 . C202 . H2022 . 109.476 no S20 . C202 . H2023 . 109.461 no H2021 . C202 . H2023 . 109.476 no H2022 . C202 . H2023 . 109.476 no S21 . C212 . H2121 . 109.478 no S21 . C212 . H2122 . 109.450 no H2121 . C212 . H2122 . 109.476 no S21 . C212 . H2123 . 109.472 no H2121 . C212 . H2123 . 109.476 no H2122 . C212 . H2123 . 109.476 no S30 . C301 . H3011 . 109.467 no S30 . C301 . H3012 . 109.468 no H3011 . C301 . H3012 . 109.476 no S30 . C301 . H3013 . 109.465 no H3011 . C301 . H3013 . 109.476 no H3012 . C301 . H3013 . 109.476 no S31 . C301 . H3014 . 109.468 no S31 . C301 . H3015 . 109.454 no S31 . C301 . H3016 . 109.477 no H3014 . C301 . H3015 . 109.476 no H3014 . C301 . H3016 . 109.476 no H3015 . C301 . H3016 . 109.476 no S30 . C302 . H3021 . 109.467 no S30 . C302 . H3022 . 109.464 no H3021 . C302 . H3022 . 109.476 no S30 . C302 . H3023 . 109.469 no H3021 . C302 . H3023 . 109.476 no H3022 . C302 . H3023 . 109.476 no S31 . C302 . H3024 . 109.479 no S31 . C302 . H3025 . 109.464 no S31 . C302 . H3026 . 109.456 no H3024 . C302 . H3025 . 109.476 no H3024 . C302 . H3026 . 109.476 no H3025 . C302 . H3026 . 109.477 no N12 . B1 . N22 . 108.5(4) yes N12 . B1 . N32 . 109.1(4) yes N22 . B1 . N32 . 107.9(4) yes N12 . B1 . H1 . 109.885 no N22 . B1 . H1 . 111.002 no N32 . B1 . H1 . 110.422 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 S10 O6 3.344(5) . 2_566 no S11 C3 3.30(2) . 2_666 no S20 O5 3.476(5) . 1_655 no S21 C3 3.268(7) . 2_666 no S30 O1 3.416(5) . 2_666 no S30 C13 3.517(6) . 2_665 no S31 C23 3.49(1) . 1_546 no O1 C301 3.265(9) . 2_666 no O1 C3 3.469(7) . . no O1 C302 3.514(7) . 2_666 no O1 C212 3.55(2) . 1_455 no O2 C301 3.38(1) . 2_666 no O2 C3 3.50(1) . . no O2 C102 3.56(1) . 2_666 no O3 C201 3.31(1) . 1_545 no O3 C14 3.330(8) . 1_646 no O3 C23 3.401(6) . 1_546 no O3 C301 3.541(9) . 2_656 no O5 C33 3.218(7) . 2_575 no O5 N32 3.294(6) . 2_575 no O5 C212 3.33(2) . 1_455 no O5 N12 3.517(7) . 2_575 no O5 C34 3.523(8) . 2_575 no O5 C102 3.548(9) . 2_566 no O6 C101 3.470(9) . 2_566 no O6 O6 3.48(1) . 2_565 no N11 C101 3.54(1) . 1_554 no N12 C101 3.60(1) . 1_554 no N21 C34 3.552(8) . 2_675 no N21 C101 3.56(1) . 1_554 no N31 C34 3.450(7) . 2_675 no C2 C302 3.49(1) . 2_666 no C33 C35 3.495(7) . 2_675 no C34 C102 3.544(7) . 1_564 no C34 C35 3.566(8) . 2_675 no C202 C202 2.97(2) . 2_766 no C212 C302 3.28(2) . 2_766 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag W1 N11 N12 C13 . . . . 178.7(4) no W1 N11 N12 B1 . . . . -2.2(6) no W1 N11 C15 C14 . . . . -178.0(4) no W1 N21 N22 C23 . . . . 174.3(4) no W1 N21 N22 B1 . . . . -4.3(7) no W1 N21 C25 C24 . . . . -173.5(4) no W1 N31 N32 C33 . . . . 178.9(3) no W1 N31 N32 B1 . . . . 0.3(5) no W1 N31 C35 C34 . . . . -179.3(3) no N11 W1 N21 N22 . . . . 44.2(4) no N11 W1 N21 C25 . . . . -142.3(5) no N11 W1 N31 N32 . . . . -41.9(3) no N11 W1 N31 C35 . . . . 137.9(5) no N11 N12 C13 C14 . . . . -0.8(7) no N11 N12 B1 N22 . . . . 60.1(6) no N11 N12 B1 N32 . . . . -57.3(5) no N11 C15 C14 C13 . . . . 0.2(8) no N12 N11 W1 N21 . . . . -40.7(4) no N12 N11 W1 N31 . . . . 42.6(4) no N12 N11 W1 C5 . . . . 132.2(4) no N12 N11 W1 C6 . . . . -135.4(4) no N12 N11 C15 C14 . . . . -0.7(7) no N12 C13 C14 C15 . . . . 0.4(7) no N12 B1 N22 N21 . . . . -57.0(6) no N12 B1 N22 C23 . . . . 124.8(6) no N12 B1 N32 N31 . . . . 59.1(5) no N12 B1 N32 C33 . . . . -119.2(5) no N21 W1 N11 C15 . . . . 136.4(6) no N21 W1 N31 N32 . . . . 40.1(3) no N21 W1 N31 C35 . . . . -140.2(5) no N21 N22 C23 C24 . . . . 0.3(7) no N21 N22 B1 N32 . . . . 61.1(6) no N21 C25 C24 C23 . . . . -0.5(8) no N22 N21 W1 N31 . . . . -37.8(4) no N22 N21 W1 C1 . . . . -141.4(4) no N22 N21 W1 C6 . . . . 132.9(4) no N22 N21 C25 C24 . . . . 0.7(7) no N22 C23 C24 C25 . . . . 0.1(8) no N22 B1 N12 C13 . . . . -121.0(6) no N22 B1 N32 N31 . . . . -58.6(5) no N22 B1 N32 C33 . . . . 123.1(5) no N31 W1 N11 C15 . . . . -140.4(6) no N31 W1 N21 C25 . . . . 135.7(5) no N31 N32 C33 C34 . . . . 0.9(5) no N31 C35 C34 C33 . . . . 0.0(6) no N32 N31 W1 C1 . . . . 135.9(3) no N32 N31 W1 C5 . . . . -136.8(3) no N32 N31 C35 C34 . . . . 0.5(6) no N32 C33 C34 C35 . . . . -0.6(6) no N32 B1 N12 C13 . . . . 121.6(6) no N32 B1 N22 C23 . . . . -117.1(6) no C1 W1 N21 C25 . . . . 32.1(5) no C1 W1 N31 C35 . . . . -44.4(5) no C5 W1 N11 C15 . . . . -50.8(6) no C5 W1 N31 C35 . . . . 42.9(5) no C6 W1 N11 C15 . . . . 41.6(6) no C6 W1 N21 C25 . . . . -53.6(5) no C13 N12 N11 C15 . . . . 0.9(6) no C14 C13 N12 B1 . . . . -179.8(5) no C15 N11 N12 B1 . . . . -180.0(5) no C23 N22 N21 C25 . . . . -0.6(6) no C24 C23 N22 B1 . . . . 178.7(6) no C25 N21 N22 B1 . . . . -179.2(5) no C33 N32 N31 C35 . . . . -0.9(5) no C34 C33 N32 B1 . . . . 179.4(5) no C35 N31 N32 B1 . . . . -179.5(4) no #------------------------------------------------------------------------------ # start Validation Reply Form #_vrf_PLAT305_rian18 #; #PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) >H2021 #RESPONSE: ... #Platon/checkcif has been confused by the disorder. #These atoms ARE bonded to the rest of the molecule. #; # end Validation Reply Form #===END data_rian12 _database_code_depnum_ccdc_archive 'CCDC 245029' _audit_creation_date 04-14-07 _audit_creation_method CRYSTALS_ver_12-03-99 # 7131615 rian12 _audit_update_record ; 2004-07-14 - Report on C17 H19 B N6 O2 Si W by Anthony C. Willis for Anthony F. Hill and Rian Dewhurst 2004-07-14- passes checkcif tests with minor warnings ; _publ_section_abstract #Text of the abstract ; The crystal structure of [(C~9~H~10~BN~6~)W(CO)~2~C~3~Si(CH~3~)~3~] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit contains one [(C~9~H~10~BN~6~)W(CO)~2~C~3~Si(CH~3~)~3~] molecule. When refined with anisotropic displacement parameters, the atoms of the Si(CH~3~)~3~ unit exhibited very elongated ellipsoids, suggesting that these atoms were disordered. Each atom was therefore split over two sites with isotropic displacement parameters which were constrained to be equal for the carbon atoms and identical anisotropic displacement parameters for the silicon sites. A connectivity of sites was established corresponding to two orientations of the Si(CH~3~)~3~ unit. Restraints were imposed upon bonded Si---C distances and C---Si---C angles. The relative populations of these two orientation were refined. A difference electron density map at this stage revealed a column of electon density extending along (0,0,z) which would appear to be disordered solvate molecules. Local maxima were 2.6 - 2.8\%A apart. The compound was recrystallised from dichloromethane/petroleum ether with water possibly also present. Attempts were made to model the observed electron density with partially-occupied water molecules, but refinement was very unstable and the results not very convincing particularly as water should not have been present to any large extent. Therefore the computer program SQUEEZE within PLATON [Sluis, P. van der and Spek, A.L. (1990) Acta Crystallogr., Sect. A, 46, 194-201.] was used instead to account for this unassigned electron density. The program identified solvent accessible voids totalling 712.8\%A^3^ in the cell and 32 electrons per unit cell were recovered. The formula weight, density etc. listed in the Tables do not include any correction for the missing solvate. The largest peak in the final difference electron density map was near the W atom. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms were included at idealized positions and ride on the atom to which they are attached. ; _publ_section_exptl_prep ; The compound was prepared by RDD and recrystallized from dichloromethane/petroleum spirit. The sample ID was RD-3,129. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 38.1017(5) _cell_angle_alpha 90 _cell_length_b 38.1017(5) _cell_angle_beta 90 _cell_length_c 8.18960(10) _cell_angle_gamma 120 _cell_volume 10296.3(2) _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 18 _chemical_formula_sum ' C17 H19 B N6 O2 Si W ' _chemical_formula_moiety ' C17 H19 B N6 O2 Si W ' _chemical_compound_source ; ? ; _chemical_formula_weight 562.12 _cell_measurement_reflns_used 27412 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4896.00 _exptl_absorpt_coefficient_mu 5.123 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 1.8 deg at rate 36 sec/frame, crystal-detector distance 40mm, multiple scan sets so over 95 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.050 -1 0 0 0.080 0 1 0 0.010 0 -1 0 0.040 0 0 1 0.010 0 0 -1 0.010 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; # Sheldrick geometric definitions 0.26 0.28 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 5264 _reflns_number_total 5264 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 5264 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5244 _diffrn_reflns_theta_min 2.562 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.477 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min -49 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 49 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _refine_diff_density_min -0.94 _refine_diff_density_max 1.33 _refine_ls_number_reflns 2881 _refine_ls_number_restraints 18 _refine_ls_number_parameters 251 #_refine_ls_R_factor_ref 0.0269 _refine_ls_wR_factor_ref 0.0282 _refine_ls_goodness_of_fit_ref 1.1247 #_reflns_number_all 3581 _refine_ls_R_factor_all 0.0347 _refine_ls_wR_factor_all 0.0332 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2881 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_gt 0.0282 _refine_ls_shift/su_max 0.003068 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.621 0.0333 0.440 0.00494 0.126 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Spek, A.L. (2001) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Sluis, P. van der & Spek, A.L. (1990) Acta Crystallogr., Sect. A, 46, 194-201. Altomare, A., Cascarano, G., Giacovazzo C., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens W1 W 0.204192(7) 0.122291(7) 0.27770(3) 0.0385 1.0000 Uani . . . . . . Si40 Si 0.3147(4) 0.2550(4) 0.7905(15) 0.0629 0.591(11) Uani D . P . . . Si41 Si 0.3203(6) 0.2586(6) 0.760(2) 0.0629 0.409(11) Uani D . P . . . O5 O 0.13315(17) 0.11278(19) 0.4991(6) 0.0807 1.0000 Uani . . . . . . O6 O 0.21025(19) 0.05841(17) 0.4989(6) 0.0801 1.0000 Uani . . . . . . N11 N 0.15963(13) 0.07374(13) 0.1060(5) 0.0337 1.0000 Uani . . . . . . N12 N 0.16377(13) 0.07898(13) -0.0586(5) 0.0347 1.0000 Uani . . . . . . N21 N 0.24713(13) 0.12421(13) 0.0930(5) 0.0337 1.0000 Uani . . . . . . N22 N 0.23914(13) 0.12173(13) -0.0691(5) 0.0358 1.0000 Uani . . . . . . N31 N 0.19734(14) 0.16095(13) 0.0975(5) 0.0354 1.0000 Uani . . . . . . N32 N 0.19647(13) 0.15436(13) -0.0656(5) 0.0344 1.0000 Uani . . . . . . C1 C 0.23919(18) 0.16203(18) 0.4194(7) 0.0426 1.0000 Uani . . . . . . C2 C 0.26321(19) 0.19045(19) 0.5318(8) 0.0494 1.0000 Uani . . . . . . C3 C 0.2852(2) 0.2168(2) 0.6310(9) 0.0637 1.0000 Uani D . . . . . C5 C 0.1590(2) 0.1162(2) 0.4157(7) 0.0517 1.0000 Uani . . . . . . C6 C 0.2080(2) 0.0815(2) 0.4155(7) 0.0478 1.0000 Uani . . . . . . C13 C 0.13367(18) 0.04627(18) -0.1335(8) 0.0443 1.0000 Uani . . . . . . C14 C 0.10962(18) 0.01939(18) -0.0174(8) 0.0464 1.0000 Uani . . . . . . C15 C 0.12663(18) 0.03719(17) 0.1299(8) 0.0432 1.0000 Uani . . . . . . C23 C 0.26991(18) 0.12263(17) -0.1526(8) 0.0444 1.0000 Uani . . . . . . C24 C 0.29869(18) 0.12555(19) -0.0444(9) 0.0523 1.0000 Uani . . . . . . C25 C 0.28338(17) 0.12662(17) 0.1074(8) 0.0447 1.0000 Uani . . . . . . C33 C 0.19216(17) 0.18259(18) -0.1475(8) 0.0454 1.0000 Uani . . . . . . C34 C 0.19018(18) 0.20842(19) -0.0347(9) 0.0497 1.0000 Uani . . . . . . C35 C 0.19331(18) 0.19393(17) 0.1143(8) 0.0455 1.0000 Uani . . . . . . C410 C 0.2937(6) 0.2888(6) 0.803(2) 0.080(3) 0.591(11) Uiso D . P . . . C411 C 0.2934(9) 0.2841(9) 0.842(3) 0.080(3) 0.409(11) Uiso D . P . . . C420 C 0.3080(4) 0.2299(4) 0.9912(15) 0.073(3) 0.591(11) Uiso D . P . . . C421 C 0.3341(6) 0.2350(6) 0.924(2) 0.073(3) 0.409(11) Uiso D . P . . . C430 C 0.3674(4) 0.2829(5) 0.720(2) 0.087(4) 0.591(11) Uiso D . P . . . C431 C 0.3653(6) 0.2949(6) 0.639(3) 0.087(4) 0.409(11) Uiso D . P . . . B1 B 0.19935(19) 0.11812(19) -0.1307(7) 0.0355 1.0000 Uani . . . . . . H1 H 0.19842(19) 0.11751(19) -0.2528(7) 0.0431 1.0000 Uiso R . . . . . H131 H 0.12965(18) 0.04238(18) -0.2542(8) 0.0530 1.0000 Uiso R . . . . . H141 H 0.08483(18) -0.00760(18) -0.0353(8) 0.0545 1.0000 Uiso R . . . . . H151 H 0.11594(18) 0.02470(17) 0.2393(8) 0.0533 1.0000 Uiso R . . . . . H231 H 0.27155(18) 0.12137(17) -0.2741(8) 0.0540 1.0000 Uiso R . . . . . H241 H 0.32490(18) 0.12666(19) -0.0697(9) 0.0639 1.0000 Uiso R . . . . . H251 H 0.29739(17) 0.12888(17) 0.2134(8) 0.0544 1.0000 Uiso R . . . . . H331 H 0.19065(17) 0.18450(18) -0.2689(8) 0.0561 1.0000 Uiso R . . . . . H341 H 0.18711(18) 0.23256(19) -0.0570(9) 0.0621 1.0000 Uiso R . . . . . H351 H 0.19268(18) 0.20620(17) 0.2214(8) 0.0555 1.0000 Uiso R . . . . . H4101 H 0.3087(6) 0.3100(6) 0.888(2) 0.0964 0.5906 Uiso R . . . . . H4102 H 0.2965(6) 0.3021(6) 0.695(2) 0.0964 0.5906 Uiso R . . . . . H4103 H 0.2643(6) 0.2728(6) 0.833(2) 0.0964 0.5906 Uiso R . . . . . H4111 H 0.3122(9) 0.3072(9) 0.913(3) 0.0964 0.4094 Uiso R . . . . . H4112 H 0.2841(9) 0.2945(9) 0.750(3) 0.0964 0.4094 Uiso R . . . . . H4113 H 0.2695(9) 0.2643(9) 0.907(3) 0.0964 0.4094 Uiso R . . . . . H4201 H 0.3240(4) 0.2507(4) 1.0759(15) 0.0876 0.5906 Uiso R . . . . . H4202 H 0.3178(4) 0.2099(4) 0.9840(15) 0.0876 0.5906 Uiso R . . . . . H4203 H 0.2787(4) 0.2154(4) 1.0219(15) 0.0876 0.5906 Uiso R . . . . . H4211 H 0.3536(6) 0.2564(6) 1.000(2) 0.0876 0.4094 Uiso R . . . . . H4212 H 0.3471(6) 0.2201(6) 0.876(2) 0.0876 0.4094 Uiso R . . . . . H4213 H 0.3092(6) 0.2155(6) 0.985(2) 0.0876 0.4094 Uiso R . . . . . H4301 H 0.3845(4) 0.3039(5) 0.802(2) 0.1041 0.5906 Uiso R . . . . . H4302 H 0.3778(4) 0.2636(5) 0.705(2) 0.1041 0.5906 Uiso R . . . . . H4303 H 0.3688(4) 0.2964(5) 0.613(2) 0.1041 0.5906 Uiso R . . . . . H4311 H 0.3844(6) 0.3178(6) 0.711(3) 0.1041 0.4094 Uiso R . . . . . H4312 H 0.3792(6) 0.2807(6) 0.594(3) 0.1041 0.4094 Uiso R . . . . . H4313 H 0.3563(6) 0.3059(6) 0.547(3) 0.1041 0.4094 Uiso 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 0.04295(14) 0.04189(14) 0.03173(10) -0.00524(10) -0.00530(10) 0.02195(12) Si40 0.056(3) 0.051(2) 0.073(4) -0.020(2) -0.020(3) 0.021(3) Si41 0.056(3) 0.051(2) 0.073(4) -0.020(2) -0.020(3) 0.021(3) O5 0.066(3) 0.119(5) 0.059(3) -0.002(3) 0.009(3) 0.048(3) O6 0.114(5) 0.072(4) 0.064(3) 0.005(3) -0.019(3) 0.054(4) N11 0.035(2) 0.034(2) 0.034(2) -0.0017(19) -0.0020(19) 0.018(2) N12 0.035(2) 0.035(2) 0.034(2) -0.0022(19) -0.0057(19) 0.018(2) N21 0.030(2) 0.035(2) 0.038(2) -0.0023(19) 0.0000(19) 0.017(2) N22 0.036(3) 0.038(2) 0.037(2) -0.0032(19) 0.0018(19) 0.021(2) N31 0.037(2) 0.032(2) 0.037(2) -0.0011(19) 0.001(2) 0.017(2) N32 0.034(2) 0.039(3) 0.033(2) 0.0025(19) -0.0011(18) 0.020(2) C1 0.044(3) 0.044(3) 0.040(3) -0.005(3) -0.001(3) 0.022(3) C2 0.045(3) 0.046(4) 0.051(4) -0.008(3) -0.003(3) 0.018(3) C3 0.060(4) 0.059(4) 0.064(5) -0.014(4) -0.010(4) 0.023(4) C5 0.053(4) 0.066(4) 0.037(3) -0.006(3) -0.001(3) 0.030(4) C6 0.059(4) 0.054(4) 0.032(3) -0.002(3) -0.009(3) 0.029(3) C13 0.040(3) 0.040(3) 0.053(4) -0.014(3) -0.012(3) 0.020(3) C14 0.038(3) 0.031(3) 0.067(4) -0.011(3) -0.013(3) 0.015(3) C15 0.040(3) 0.034(3) 0.059(4) 0.007(3) 0.000(3) 0.021(3) C23 0.043(3) 0.043(3) 0.049(3) -0.004(3) 0.010(3) 0.023(3) C24 0.031(3) 0.048(4) 0.081(5) -0.005(3) 0.007(3) 0.022(3) C25 0.033(3) 0.038(3) 0.065(4) -0.008(3) -0.011(3) 0.019(3) C33 0.038(3) 0.049(4) 0.053(4) 0.016(3) 0.001(3) 0.025(3) C34 0.043(3) 0.039(3) 0.074(4) 0.011(3) 0.005(3) 0.025(3) C35 0.039(3) 0.036(3) 0.064(4) -0.008(3) 0.006(3) 0.020(3) B1 0.038(3) 0.038(3) 0.031(3) -0.003(3) -0.001(3) 0.020(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . N11 . 2.268(4) yes W1 . N21 . 2.202(4) yes W1 . N31 . 2.191(4) yes W1 . C1 . 1.844(6) yes W1 . C5 . 1.975(7) yes W1 . C6 . 1.986(6) yes Si40 . C3 . 1.858(17) yes Si40 . C410 . 1.830(13) yes Si40 . C420 . 1.854(13) yes Si40 . C430 . 1.836(14) yes Si41 . C3 . 1.82(2) yes Si41 . C411 . 1.856(17) yes Si41 . C421 . 1.832(16) yes Si41 . C431 . 1.860(16) yes O5 . C5 . 1.150(8) yes O6 . C6 . 1.149(7) yes N11 . N12 . 1.360(6) yes N11 . C15 . 1.345(7) yes N12 . C13 . 1.348(7) yes N12 . B1 . 1.546(8) yes N21 . N22 . 1.355(6) yes N21 . C25 . 1.343(7) yes N22 . C23 . 1.343(7) yes N22 . B1 . 1.537(8) yes N31 . N32 . 1.356(6) yes N31 . C35 . 1.347(7) yes N32 . C33 . 1.346(7) yes N32 . B1 . 1.535(8) yes C1 . C2 . 1.366(8) yes C2 . C3 . 1.236(9) yes C13 . C14 . 1.362(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.377(8) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C23 . C24 . 1.370(9) yes C23 . H231 . 1.000 no C24 . C25 . 1.383(9) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C33 . C34 . 1.379(9) yes C33 . H331 . 1.000 no C34 . C35 . 1.369(9) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C410 . H4101 . 1.000 no C410 . H4102 . 1.000 no C410 . H4103 . 1.000 no C411 . H4111 . 1.000 no C411 . H4112 . 1.000 no C411 . H4113 . 1.000 no C420 . H4201 . 1.000 no C420 . H4202 . 1.000 no C420 . H4203 . 1.000 no C421 . H4211 . 1.000 no C421 . H4212 . 1.000 no C421 . H4213 . 1.000 no C430 . H4301 . 1.000 no C430 . H4302 . 1.000 no C430 . H4303 . 1.000 no C431 . H4311 . 1.000 no C431 . H4312 . 1.000 no C431 . H4313 . 1.000 no B1 . H1 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N11 . W1 . N21 . 80.91(16) yes N11 . W1 . N31 . 80.70(16) yes N21 . W1 . N31 . 81.44(16) yes N11 . W1 . C1 . 178.3(2) yes N21 . W1 . C1 . 100.7(2) yes N31 . W1 . C1 . 98.8(2) yes N11 . W1 . C5 . 90.3(2) yes N21 . W1 . C5 . 170.7(2) yes N31 . W1 . C5 . 94.2(2) yes C1 . W1 . C5 . 88.1(3) yes N11 . W1 . C6 . 91.8(2) yes N21 . W1 . C6 . 94.1(2) yes N31 . W1 . C6 . 171.8(2) yes C1 . W1 . C6 . 88.8(3) yes C5 . W1 . C6 . 89.1(3) yes C3 . Si40 . C410 . 106.5(8) yes C3 . Si40 . C420 . 110.2(8) yes C410 . Si40 . C420 . 108.7(8) yes C3 . Si40 . C430 . 106.8(8) yes C410 . Si40 . C430 . 110.3(9) yes C420 . Si40 . C430 . 114.0(9) yes C3 . Si41 . C411 . 108.1(11) yes C3 . Si41 . C421 . 105.2(11) yes C411 . Si41 . C421 . 111.2(12) yes C3 . Si41 . C431 . 110.1(11) yes C411 . Si41 . C431 . 110.2(12) yes C421 . Si41 . C431 . 111.9(12) yes W1 . N11 . N12 . 120.7(3) yes W1 . N11 . C15 . 133.3(4) yes N12 . N11 . C15 . 106.1(4) yes N11 . N12 . C13 . 109.4(5) yes N11 . N12 . B1 . 120.1(4) yes C13 . N12 . B1 . 130.4(5) yes W1 . N21 . N22 . 122.2(3) yes W1 . N21 . C25 . 131.6(4) yes N22 . N21 . C25 . 106.2(5) yes N21 . N22 . C23 . 109.5(5) yes N21 . N22 . B1 . 120.3(4) yes C23 . N22 . B1 . 130.1(5) yes W1 . N31 . N32 . 122.6(3) yes W1 . N31 . C35 . 131.7(4) yes N32 . N31 . C35 . 105.6(5) yes N31 . N32 . C33 . 110.2(5) yes N31 . N32 . B1 . 120.2(4) yes C33 . N32 . B1 . 129.6(5) yes W1 . C1 . C2 . 176.4(5) yes C1 . C2 . C3 . 178.6(7) yes W1 . C5 . O5 . 178.5(6) yes W1 . C6 . O6 . 178.2(6) yes N12 . C13 . C14 . 108.6(5) yes N12 . C13 . H131 . 125.687 no C14 . C13 . H131 . 125.686 no C13 . C14 . C15 . 105.5(5) yes C13 . C14 . H141 . 127.247 no C15 . C14 . H141 . 127.244 no C14 . C15 . N11 . 110.4(6) yes C14 . C15 . H151 . 124.807 no N11 . C15 . H151 . 124.808 no N22 . C23 . C24 . 109.0(5) yes N22 . C23 . H231 . 125.492 no C24 . C23 . H231 . 125.491 no C23 . C24 . C25 . 104.6(5) yes C23 . C24 . H241 . 127.712 no C25 . C24 . H241 . 127.713 no C24 . C25 . N21 . 110.7(5) yes C24 . C25 . H251 . 124.648 no N21 . C25 . H251 . 124.650 no N32 . C33 . C34 . 108.0(5) yes N32 . C33 . H331 . 126.023 no C34 . C33 . H331 . 126.024 no C33 . C34 . C35 . 105.2(5) yes C33 . C34 . H341 . 127.394 no C35 . C34 . H341 . 127.394 no C34 . C35 . N31 . 111.0(6) yes C34 . C35 . H351 . 124.488 no N31 . C35 . H351 . 124.488 no Si40 . C410 . H4101 . 109.466 no Si40 . C410 . H4102 . 109.451 no H4101 . C410 . H4102 . 109.476 no Si40 . C410 . H4103 . 109.483 no H4101 . C410 . H4103 . 109.476 no H4102 . C410 . H4103 . 109.476 no Si41 . C411 . H4111 . 109.470 no Si41 . C411 . H4112 . 109.476 no Si40 . C411 . H4112 . 116.469 no H4111 . C411 . H4112 . 109.475 no Si41 . C411 . H4113 . 109.454 no H4111 . C411 . H4113 . 109.476 no H4112 . C411 . H4113 . 109.476 no Si40 . C420 . H4201 . 109.452 no Si40 . C420 . H4202 . 109.457 no H4201 . C420 . H4202 . 109.476 no Si40 . C420 . H4203 . 109.491 no H4201 . C420 . H4203 . 109.476 no H4202 . C420 . H4203 . 109.476 no Si41 . C421 . H4211 . 109.483 no Si41 . C421 . H4212 . 109.430 no H4211 . C421 . H4212 . 109.476 no Si41 . C421 . H4213 . 109.487 no H4211 . C421 . H4213 . 109.476 no H4212 . C421 . H4213 . 109.476 no Si40 . C430 . H4301 . 109.452 no Si40 . C430 . H4302 . 109.459 no H4301 . C430 . H4302 . 109.476 no Si40 . C430 . H4303 . 109.489 no H4301 . C430 . H4303 . 109.476 no H4302 . C430 . H4303 . 109.476 no Si41 . C431 . H4311 . 109.458 no Si41 . C431 . H4312 . 109.461 no H4311 . C431 . H4312 . 109.476 no Si41 . C431 . H4313 . 109.480 no H4311 . C431 . H4313 . 109.476 no H4312 . C431 . H4313 . 109.476 no N12 . B1 . N22 . 108.1(4) yes N12 . B1 . N32 . 108.2(4) yes N22 . B1 . N32 . 108.4(4) yes N12 . B1 . H1 . 110.856 no N22 . B1 . H1 . 110.621 no N32 . B1 . H1 . 110.540 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 O5 O6 3.414(9) . 14_556 no N11 C34 3.493(9) . 8 no N12 C34 3.574(9) . 8 no N12 C14 3.588(9) . 14 no N21 C34 3.57(1) . 8 no N21 C420 3.60(1) . 1_554 no N31 C14 3.60(1) . 14 no N32 C14 3.585(9) . 14 no C3 C33 3.60(1) . 1_556 no C13 C35 3.51(1) . 8 no C15 C33 3.40(1) . 8 no C25 C421 3.58(2) . 6_556 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag W1 N11 N12 C13 . . . . -179.6(5) no W1 N11 N12 B1 . . . . 0.6(8) no W1 N11 C15 C14 . . . . 179.4(5) no W1 N21 N22 C23 . . . . -178.4(4) no W1 N21 N22 B1 . . . . 1.0(6) no W1 N21 C25 C24 . . . . 178.0(4) no W1 N31 N32 C33 . . . . -179.8(3) no W1 N31 N32 B1 . . . . 1.4(6) no W1 N31 C35 C34 . . . . 179.6(4) no N11 W1 N21 N22 . . . . 41.0(4) no N11 W1 N21 C25 . . . . -137.0(5) no N11 W1 N31 N32 . . . . -42.4(4) no N11 W1 N31 C35 . . . . 137.6(5) no N11 N12 C13 C14 . . . . 0.0(9) no N11 N12 B1 N22 . . . . 58.4(8) no N11 N12 B1 N32 . . . . -58.9(8) no N11 C15 C14 C13 . . . . 1(1) no N12 N11 W1 N21 . . . . -41.6(5) no N12 N11 W1 N31 . . . . 41.1(5) no N12 N11 W1 C5 . . . . 135.4(5) no N12 N11 W1 C6 . . . . -135.6(5) no N12 N11 C15 C14 . . . . -0.5(9) no N12 C13 C14 C15 . . . . -0.3(9) no N12 B1 N22 N21 . . . . -60.3(6) no N12 B1 N22 C23 . . . . 119.0(6) no N12 B1 N32 N31 . . . . 58.7(6) no N12 B1 N32 C33 . . . . -119.8(5) no N21 W1 N11 C15 . . . . 138.4(7) no N21 W1 N31 N32 . . . . 39.7(4) no N21 W1 N31 C35 . . . . -140.3(5) no N21 N22 C23 C24 . . . . 0.3(6) no N21 N22 B1 N32 . . . . 56.8(6) no N21 C25 C24 C23 . . . . 0.4(7) no N22 N21 W1 N31 . . . . -40.9(4) no N22 N21 W1 C1 . . . . -138.3(4) no N22 N21 W1 C6 . . . . 132.1(4) no N22 N21 C25 C24 . . . . -0.2(6) no N22 C23 C24 C25 . . . . -0.4(7) no N22 B1 N12 C13 . . . . -121.3(7) no N22 B1 N32 N31 . . . . -58.3(5) no N22 B1 N32 C33 . . . . 123.1(5) no N31 W1 N11 C15 . . . . -138.9(7) no N31 W1 N21 C25 . . . . 141.1(5) no N31 N32 C33 C34 . . . . 0.0(6) no N31 C35 C34 C33 . . . . 0.4(6) no N32 N31 W1 C1 . . . . 139.2(4) no N32 N31 W1 C5 . . . . -132.1(4) no N32 N31 C35 C34 . . . . -0.4(6) no N32 C33 C34 C35 . . . . -0.3(6) no N32 B1 N12 C13 . . . . 121.4(7) no N32 B1 N22 C23 . . . . -123.9(6) no C1 W1 N21 C25 . . . . 43.8(6) no C1 W1 N31 C35 . . . . -40.7(5) no C5 W1 N11 C15 . . . . -44.6(7) no C5 W1 N31 C35 . . . . 48.0(5) no C6 W1 N11 C15 . . . . 44.5(7) no C6 W1 N21 C25 . . . . -45.8(5) no C13 N12 N11 C15 . . . . 0.3(8) no C14 C13 N12 B1 . . . . 179.7(7) no C15 N11 N12 B1 . . . . -179.4(7) no C23 N22 N21 C25 . . . . 0.0(6) no C24 C23 N22 B1 . . . . -179.1(5) no C25 N21 N22 B1 . . . . 179.4(5) no C33 N32 N31 C35 . . . . 0.2(5) no C34 C33 N32 B1 . . . . 178.7(5) no C35 N31 N32 B1 . . . . -178.6(4) no #------------------------------------------------------------------------------ # start Validation Reply Form #_vrf_PLAT601_rian12 #; #PROBLEM: Structure Contains Solvent Accessible VOIDS of . 237.00 A**3 #RESPONSE: ... #Yes, there is a featureless column of electron density running along #(0,0,z) [and equivalent lines] which was removed using SQUEEZE. #It presumably arises from disordered solvate molecules. #There is therefore a solvent accessible void in the final structure. #; # end Validation Reply Form #===END