# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2138 data_1 _audit_creation_date 98-08-01 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd16 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name ' Graham McCann ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Group 6 Transition Metal Carbonyl Complexes with Chalcogen-bridged Diarsenic(III) Ligands' # Title of paper ; # 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 'Doerrer, Linda H.' #<--'Last name, first name' ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address for author 1 ; 'Green, Jennifer C.' # Author 2 ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address 2 ; 'Green, Malcolm L. H.' # Author 3 ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address 3 ; 'Haiduc, I.' # Author 4 ; 'Department of Chemistry Babes-Bolyai University Cluj-Napoca Cluj-Napoca RO-3400 Romania' ; # Address 4 'Jardine, C. N.' # Author 5 ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' ; # Address 5 'Pascu, S. I.' # Author 6 ; 'Inorganic Chemistry Laboratory' South Parks Road Oxford OX1 3QR UK' ; # Address 6 'Silaghi-Dumitrescu, L.' # Author 7 ; 'Department of Chemistry Babes-Bolyai University Cluj-Napoca Cluj-Napoca RO-3400 Romania' # Address 7 ; 'Watkin, D.J.' # Author 8 ; 'Chemical Crystallography Laboratory 9 Parks Road OXFORD OX1 3PD UK' # Address 8 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software ,Xpress, MAC Science, 1989' _computing_data_reduction ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # 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 #**************************************************************************** _cell_length_a 10.831(4) _cell_angle_alpha 86.080(2) _cell_length_b 13.264(4) _cell_angle_beta 87.157(2) _cell_length_c 17.913(6) _cell_angle_gamma 65.773(2) _cell_volume 2340.6(1) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 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 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' 'As ' -0.0300 2.0070 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972 2.5310 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 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' 'C ' 0.0020 0.0020 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 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C52 H40 As4 Mo1 O6 ' _chemical_formula_moiety ' C52 H40 As4 Mo1 O6 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1156.52 _cell_measurement_reflns_used 15259 _cell_measurement_theta_min 0 _cell_measurement_theta_max 26.57 _cell_measurement_temperature 125 _cell_formula_units_Z 2 _exptl_crystal_description ' irregular ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.35 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1144.23 _exptl_absorpt_coefficient_mu 3.12 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.336 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 125 _diffrn_reflns_number 9009 _reflns_number_total 9009 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 9009 # Number of reflections without Friedels Law is 0 _reflns_number_gt 7246 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _reflns_threshold_expression >3.00\s(I) _refine_diff_density_min -0.94 _refine_diff_density_max 0.86 _refine_ls_number_reflns 7246 _refine_ls_number_parameters 568 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0307 _refine_ls_goodness_of_fit_ref 1.0375 _refine_ls_shift/su_max 0.041964 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2.42 -0.243 1.80 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Mo1 0.423768(19) -0.053479(16) 1.302141(11) 0.0122 1.0000 Uani As1 0.19265(2) 0.000984(19) 1.237868(13) 0.0122 1.0000 Uani As2 0.29744(3) -0.21978(2) 1.151789(14) 0.0169 1.0000 Uani As3 0.42497(2) -0.239000(19) 1.360931(12) 0.0107 1.0000 Uani As4 0.69063(2) -0.38067(2) 1.271202(13) 0.0156 1.0000 Uani O1 0.16145(18) -0.09721(15) 1.1862(1) 0.0189 1.0000 Uani O2 0.54163(17) -0.36875(14) 1.32746(9) 0.0157 1.0000 Uani O3 0.3033(2) 0.04783(19) 1.45934(11) 0.0353 1.0000 Uani O4 0.4132(3) 0.17930(18) 1.24617(12) 0.0360 1.0000 Uani O5 0.7116(2) -0.1225(2) 1.36777(14) 0.0425 1.0000 Uani O6 0.5894(2) -0.13390(17) 1.14996(11) 0.0283 1.0000 Uani C1 0.3413(3) 0.0105(2) 1.40237(15) 0.0206 1.0000 Uani C2 0.4160(3) 0.0947(2) 1.26618(14) 0.0212 1.0000 Uani C3 0.6055(3) -0.0958(2) 1.34409(15) 0.0239 1.0000 Uani C4 0.5259(3) -0.1103(2) 1.20393(15) 0.0196 1.0000 Uani C10 0.0236(2) 0.0549(2) 1.29471(14) 0.0176 1.0000 Uani C11 -0.0854(3) 0.0342(2) 1.27428(16) 0.0250 1.0000 Uani C12 -0.2070(3) 0.0764(3) 1.31410(18) 0.0306 1.0000 Uani C13 -0.2189(3) 0.1387(3) 1.37544(18) 0.0338 1.0000 Uani C14 -0.1119(3) 0.1614(3) 1.39523(18) 0.0394 1.0000 Uani C15 0.0095(3) 0.1190(3) 1.35492(17) 0.0289 1.0000 Uani C20 0.1513(3) 0.1185(2) 1.15973(14) 0.0184 1.0000 Uani C21 0.0358(3) 0.2166(2) 1.16334(16) 0.0253 1.0000 Uani C22 0.0087(3) 0.2985(2) 1.10625(19) 0.0320 1.0000 Uani C23 0.0975(4) 0.2823(3) 1.04548(17) 0.0355 1.0000 Uani C24 0.2134(4) 0.1842(3) 1.04101(17) 0.0371 1.0000 Uani C25 0.2403(3) 0.1031(2) 1.09870(16) 0.0276 1.0000 Uani C30 0.2916(3) -0.1672(2) 1.04619(14) 0.0212 1.0000 Uani C31 0.1717(3) -0.1247(2) 1.00670(16) 0.0262 1.0000 Uani C32 0.1710(3) -0.0828(3) 0.93317(17) 0.0321 1.0000 Uani C33 0.2896(4) -0.0826(3) 0.89930(17) 0.0344 1.0000 Uani C34 0.4091(3) -0.1258(3) 0.93805(17) 0.0359 1.0000 Uani C35 0.4100(3) -0.1685(3) 1.01183(16) 0.0287 1.0000 Uani C40 0.1855(3) -0.3021(2) 1.14441(14) 0.0226 1.0000 Uani C41 0.0458(3) -0.2550(3) 1.15209(16) 0.0294 1.0000 Uani C42 -0.0276(4) -0.3194(3) 1.14760(17) 0.0375 1.0000 Uani C43 0.0379(4) -0.4297(3) 1.13545(17) 0.0395 1.0000 Uani C44 0.1757(5) -0.4781(3) 1.12842(18) 0.0444 1.0000 Uani C45 0.2515(3) -0.4144(3) 1.13323(17) 0.0325 1.0000 Uani C50 0.2633(2) -0.2678(2) 1.36002(13) 0.0162 1.0000 Uani C51 0.2630(3) -0.3588(2) 1.32643(14) 0.0203 1.0000 Uani C52 0.1429(3) -0.3747(3) 1.32646(15) 0.0275 1.0000 Uani C53 0.0271(3) -0.3000(3) 1.35969(16) 0.0291 1.0000 Uani C54 0.0277(3) -0.2095(2) 1.39318(16) 0.0272 1.0000 Uani C55 0.1461(3) -0.1932(2) 1.39333(15) 0.0225 1.0000 Uani C60 0.4681(2) -0.27398(19) 1.46698(12) 0.0139 1.0000 Uani C61 0.5433(2) -0.2279(2) 1.50153(14) 0.0178 1.0000 Uani C62 0.5875(3) -0.2636(2) 1.57398(14) 0.0211 1.0000 Uani C63 0.5579(3) -0.3460(2) 1.61202(14) 0.0240 1.0000 Uani C64 0.4816(3) -0.3917(2) 1.57821(14) 0.0232 1.0000 Uani C65 0.4365(3) -0.3556(2) 1.50540(14) 0.0190 1.0000 Uani C70 0.8233(3) -0.4915(2) 1.33719(14) 0.0182 1.0000 Uani C71 0.9486(3) -0.5593(2) 1.30751(15) 0.0241 1.0000 Uani C72 1.0509(3) -0.6297(3) 1.35447(18) 0.0307 1.0000 Uani C73 1.0271(3) -0.6317(3) 1.43111(18) 0.0350 1.0000 Uani C74 0.9023(3) -0.5655(3) 1.46053(16) 0.0343 1.0000 Uani C75 0.7998(3) -0.4937(2) 1.41400(15) 0.0257 1.0000 Uani C80 0.6740(3) -0.4787(2) 1.20007(15) 0.0232 1.0000 Uani C81 0.6604(3) -0.4432(3) 1.12466(16) 0.0320 1.0000 Uani C82 0.6411(4) -0.5093(3) 1.07206(18) 0.0439 1.0000 Uani C83 0.6362(4) -0.6071(3) 1.0941(2) 0.0472 1.0000 Uani C84 0.6488(4) -0.6430(3) 1.1689(2) 0.0429 1.0000 Uani C85 0.6689(3) -0.5799(3) 1.22180(17) 0.0310 1.0000 Uani H111 -0.0793 0.0022 1.2470 0.0229 1.0000 Uiso H121 -0.2809 0.0618 1.2954 0.0378 1.0000 Uiso H131 -0.3071 0.1690 1.4026 0.0528 1.0000 Uiso H141 -0.1258 0.2110 1.4276 0.0566 1.0000 Uiso H151 0.0633 0.1483 1.3671 0.0362 1.0000 Uiso H211 -0.0278 0.2245 1.1982 0.0322 1.0000 Uiso H221 -0.0779 0.3765 1.1228 0.0604 1.0000 Uiso H231 0.0850 0.3524 1.0174 0.1120 1.0000 Uiso H241 0.2937 0.1636 1.0028 0.0507 1.0000 Uiso H251 0.3344 0.0357 1.0987 0.0313 1.0000 Uiso H311 0.0923 -0.1339 1.0272 0.0185 1.0000 Uiso H321 0.0891 -0.0750 0.9024 0.0560 1.0000 Uiso H331 0.2840 -0.0485 0.8437 0.1175 1.0000 Uiso H341 0.5047 -0.1342 0.9167 0.0334 1.0000 Uiso H351 0.5051 -0.2024 1.0380 0.0335 1.0000 Uiso H411 0.0052 -0.1762 1.1579 0.0438 1.0000 Uiso H421 -0.1119 -0.2859 1.1546 0.0363 1.0000 Uiso H431 -0.0220 -0.4690 1.1325 0.0386 1.0000 Uiso H441 0.2421 -0.5418 1.1283 0.0663 1.0000 Uiso H451 0.3322 -0.4425 1.1350 0.0001 1.0000 Uiso H511 0.3401 -0.4086 1.3083 0.0020 1.0000 Uiso H521 0.1532 -0.4425 1.3042 0.0310 1.0000 Uiso H531 -0.0561 -0.3160 1.3606 0.0643 1.0000 Uiso H541 -0.0515 -0.1601 1.4112 0.0384 1.0000 Uiso H551 0.1546 -0.1451 1.4129 0.0090 1.0000 Uiso H611 0.5667 -0.1820 1.4779 0.0407 1.0000 Uiso H621 0.6417 -0.2306 1.5948 0.0108 1.0000 Uiso H631 0.5807 -0.3696 1.6634 0.0765 1.0000 Uiso H641 0.4535 -0.4516 1.6074 0.0148 1.0000 Uiso H651 0.3710 -0.3829 1.4842 0.0103 1.0000 Uiso H711 0.9678 -0.5689 1.2489 0.0378 1.0000 Uiso H721 1.1306 -0.6595 1.3264 0.0918 1.0000 Uiso H731 1.1027 -0.6731 1.4671 0.0787 1.0000 Uiso H741 0.8810 -0.5657 1.5191 0.0830 1.0000 Uiso H751 0.7060 -0.4390 1.4346 0.0171 1.0000 Uiso H811 0.6783 -0.3918 1.1134 0.0139 1.0000 Uiso H821 0.6616 -0.4783 1.0514 0.0206 1.0000 Uiso H831 0.6135 -0.6649 1.0671 0.0717 1.0000 Uiso H841 0.6231 -0.7019 1.1895 0.0853 1.0000 Uiso H851 0.6533 -0.5953 1.2818 0.0529 1.0000 Uiso 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 Mo1 0.0116(1) 0.0118(1) 0.0128(1) -0.00109(8) -0.00008(7) -0.00447(8 As1 0.01091(11) 0.01158(11) 0.01152(11) -0.00259(9) 0.00048(9) -0.00186(9 As2 0.01818(12) 0.01529(12) 0.01427(12) -0.0040(1) 0.0013(1) -0.0036(1) As3 0.01028(11) 0.01109(11) 0.00989(11) -0.00171(9) 0.00040(8) -0.00338(9 As4 0.01603(12) 0.01415(12) 0.01270(12) -0.00112(9) 0.00265(9) -0.0025(1) O1 0.0182(8) 0.0177(9) 0.0195(8) -0.0068(7) 0.0001(7) -0.0053(7) O2 0.0174(8) 0.0122(8) 0.0147(8) -0.0036(7) 0.0037(7) -0.0031(7) O3 0.0467(13) 0.0327(12) 0.022(1) -0.0136(9) 0.0055(9) -0.0101(11 O4 0.0590(15) 0.0246(11) 0.0315(11) 0.0032(9) -0.0023(11) -0.0249(11 O5 0.022(1) 0.0618(16) 0.0489(14) 0.0114(12) -0.013(1) -0.0228(11 O6 0.026(1) 0.0317(11) 0.021(1) -0.0019(9) 0.0093(8) -0.0071(9) C1 0.0230(12) 0.0161(12) 0.0222(13) -0.002(1) -0.002(1) -0.0072(11 C2 0.0256(13) 0.0219(13) 0.0171(12) -0.005(1) 0.002(1) -0.0102(11 C3 0.0230(13) 0.0277(14) 0.0247(13) 0.0024(11) -0.0001(11) -0.0147(12 C4 0.0158(11) 0.0173(12) 0.0231(13) 0.001(1) -0.002(1) -0.004(1) C10 0.0149(11) 0.0165(11) 0.0174(11) -0.000(1) 0.0017(9) -0.003(1) C11 0.0216(13) 0.0271(14) 0.0269(13) -0.0074(12) 0.0022(11) -0.0100(12 C12 0.0171(12) 0.0316(15) 0.0413(17) 0.0002(14) 0.0059(12) -0.0091(12 C13 0.0222(13) 0.0351(17) 0.0322(15) -0.0038(14) 0.0131(12) -0.0009(13 C14 0.0327(16) 0.0442(19) 0.0308(16) -0.0209(15) 0.0114(13) -0.0035(15 C15 0.0212(13) 0.0321(15) 0.0306(15) -0.0131(13) 0.0011(12) -0.0064(12 C20 0.0198(12) 0.0185(12) 0.0170(11) 0.000(1) -0.004(1) -0.008(1) C21 0.0215(13) 0.0195(13) 0.0308(14) 0.0026(11) -0.0005(11) -0.0047(11 C22 0.0320(15) 0.0158(13) 0.0395(16) 0.0006(13) -0.0075(13) -0.0005(12 C23 0.0503(19) 0.0285(15) 0.0240(14) 0.0088(13) -0.0090(14) -0.0130(15 C24 0.0480(19) 0.0360(17) 0.0214(14) 0.0035(13) 0.0042(13) -0.0126(16 C25 0.0305(14) 0.0249(14) 0.0213(13) 0.0006(12) 0.0040(12) -0.0059(12 C30 0.0278(13) 0.0227(13) 0.0129(11) -0.005(1) 0.002(1) -0.0098(11 C31 0.0247(13) 0.0280(14) 0.0230(13) -0.0030(12) 0.0003(11) -0.0078(12 C32 0.0329(15) 0.0343(16) 0.0269(14) -0.0003(13) -0.0028(12) -0.0114(14 C33 0.0437(18) 0.0408(18) 0.0215(14) -0.0000(13) 0.0010(13) -0.0205(15 C34 0.0398(17) 0.053(2) 0.0222(14) -0.0012(14) 0.0034(13) -0.0264(16 C35 0.0292(14) 0.0355(16) 0.0216(13) -0.0052(12) 0.0020(11) -0.0132(13 C40 0.0366(15) 0.0204(13) 0.0146(11) -0.003(1) 0.0012(11) -0.0155(12 C41 0.0359(16) 0.0320(15) 0.0241(13) -0.0007(12) -0.0018(12) -0.0176(14 C42 0.0440(18) 0.053(2) 0.0281(15) 0.0031(14) -0.0047(14) -0.0325(17 C43 0.065(2) 0.047(2) 0.0223(14) -0.0014(13) -0.0006(15) -0.0384(19 C44 0.085(3) 0.0264(16) 0.0271(16) -0.0079(13) 0.0045(17) -0.0285(19 C45 0.0432(17) 0.0267(15) 0.0282(14) -0.0067(12) 0.0069(13) -0.0151(14 C50 0.0155(11) 0.0208(12) 0.013(1) 0.003(1) -0.0013(9) -0.008(1) C51 0.0234(12) 0.0242(13) 0.0162(11) -0.000(1) -0.001(1) -0.0127(11 C52 0.0353(15) 0.0365(16) 0.0199(13) 0.0044(12) -0.0088(12) -0.0241(14 C53 0.0237(13) 0.0454(18) 0.0261(13) 0.0099(13) -0.0069(11) -0.0234(13 C54 0.0144(12) 0.0323(15) 0.0298(14) 0.0070(12) -0.0014(11) -0.0057(11 C55 0.0209(12) 0.0222(13) 0.0243(13) 0.0015(11) -0.003(1) -0.0088(11 C60 0.014(1) 0.0141(11) 0.010(1) -0.0033(9) 0.0018(9) -0.0015(9) C61 0.0156(11) 0.0195(12) 0.0182(11) -0.003(1) 0.0013(9) -0.007(1) C62 0.0202(12) 0.0237(13) 0.0179(12) -0.003(1) -0.004(1) -0.0069(11 C63 0.0306(14) 0.0225(13) 0.0138(11) -0.002(1) -0.0033(11) -0.0050(12 C64 0.0317(14) 0.0197(13) 0.0162(12) -0.001(1) 0.0004(11) -0.0086(12 C65 0.0231(12) 0.0171(12) 0.0145(11) -0.005(1) 0.003(1) -0.0055(11 C70 0.0180(11) 0.0158(11) 0.0198(12) -0.002(1) -0.001(1) -0.006(1) C71 0.0206(12) 0.0251(14) 0.0238(13) 0.0009(11) 0.0004(11) -0.0070(11 C72 0.0174(12) 0.0324(16) 0.0345(15) -0.0013(13) 0.0001(12) -0.0023(12 C73 0.0256(14) 0.0359(17) 0.0355(16) 0.0031(14) -0.0117(13) -0.0039(13 C74 0.0339(16) 0.0398(17) 0.0218(14) 0.0013(13) -0.0077(12) -0.0071(14 C75 0.0222(13) 0.0284(14) 0.0195(13) -0.0017(11) -0.0009(11) -0.0032(12 C80 0.0178(12) 0.0247(13) 0.0174(12) -0.0097(11) 0.001(1) 0.0022(11 C81 0.0299(15) 0.0339(16) 0.0201(13) -0.0036(12) -0.0000(12) -0.0003(13 C82 0.0361(17) 0.054(2) 0.0219(14) -0.0127(15) -0.0060(13) 0.0041(17 C83 0.0388(18) 0.046(2) 0.044(2) -0.0305(18) -0.0087(16) 0.0004(17 C84 0.0414(19) 0.0372(18) 0.049(2) -0.0222(16) -0.0016(16) -0.0114(16 C85 0.0322(15) 0.0290(15) 0.0301(15) -0.0114(13) 0.0017(12) -0.0094(13 _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 Mo1 . As1 . 2.6080(3) yes Mo1 . As3 . 2.6048(3) yes Mo1 . C1 . 2.042(3) yes Mo1 . C2 . 1.996(3) yes Mo1 . C3 . 1.984(3) yes Mo1 . C4 . 2.047(3) yes As1 . O1 . 1.7952(17) yes As1 . C10 . 1.934(2) yes As1 . C20 . 1.945(2) yes As2 . O1 . 1.8098(18) yes As2 . C30 . 1.966(2) yes As2 . C40 . 1.951(3) yes As3 . O2 . 1.7886(17) yes As3 . C50 . 1.941(2) yes As3 . C60 . 1.957(2) yes As4 . O2 . 1.8155(17) yes As4 . C70 . 1.955(2) yes As4 . C80 . 1.947(3) yes O3 . C1 . 1.147(3) yes O4 . C2 . 1.143(3) yes O5 . C3 . 1.149(3) yes O6 . C4 . 1.142(3) yes C10 . C11 . 1.387(4) yes C10 . C15 . 1.383(4) yes C11 . C12 . 1.383(4) yes C11 . H111 . 0.653(3) no C12 . C13 . 1.389(5) yes C12 . H121 . 0.976(3) no C13 . C14 . 1.379(5) yes C13 . H131 . 0.988(3) no C14 . C15 . 1.386(4) yes C14 . H141 . 0.867(3) no C15 . H151 . 0.865(3) no C20 . C21 . 1.389(4) yes C20 . C25 . 1.390(4) yes C21 . C22 . 1.389(4) yes C21 . H211 . 0.884(3) no C22 . C23 . 1.383(5) yes C22 . H221 . 1.120(3) no C23 . C24 . 1.392(5) yes C23 . H231 . 0.988(3) no C24 . C25 . 1.389(4) yes C24 . H241 . 1.035(3) no C25 . H251 . 1.045(3) no C30 . C31 . 1.393(4) yes C30 . C35 . 1.389(4) yes C31 . C32 . 1.393(4) yes C31 . H311 . 0.969(3) no C32 . C33 . 1.395(5) yes C32 . H321 . 1.033(3) no C33 . C34 . 1.382(5) yes C33 . H331 . 1.059(3) no C34 . C35 . 1.401(4) yes C34 . H341 . 1.049(3) no C35 . H351 . 1.059(3) no C40 . C41 . 1.383(4) yes C40 . C45 . 1.386(4) yes C41 . C42 . 1.393(4) yes C41 . H411 . 0.964(3) no C42 . C43 . 1.367(5) yes C42 . H421 . 0.842(4) no C43 . C44 . 1.364(6) yes C43 . H431 . 0.989(3) no C44 . C45 . 1.408(5) yes C44 . H441 . 0.856(4) no C45 . H451 . 0.798(3) no C50 . C51 . 1.386(4) yes C50 . C55 . 1.386(4) yes C51 . C52 . 1.401(4) yes C51 . H511 . 0.888(3) no C52 . C53 . 1.377(5) yes C52 . H521 . 0.971(3) no C53 . C54 . 1.381(5) yes C53 . H531 . 1.006(3) no C54 . C55 . 1.386(4) yes C54 . H541 . 0.900(3) no C55 . H551 . 0.788(3) no C60 . C61 . 1.390(3) yes C60 . C65 . 1.393(3) yes C61 . C62 . 1.389(3) yes C61 . H611 . 0.833(2) no C62 . C63 . 1.387(4) yes C62 . H621 . 0.965(3) no C63 . C64 . 1.388(4) yes C63 . H631 . 0.962(2) no C64 . C65 . 1.398(4) yes C64 . H641 . 1.060(3) no C65 . H651 . 1.017(3) no C70 . C71 . 1.387(4) yes C70 . C75 . 1.387(4) yes C71 . C72 . 1.394(4) yes C71 . H711 . 1.065(3) no C72 . C73 . 1.385(5) yes C72 . H721 . 0.926(3) no C73 . C74 . 1.376(5) yes C73 . H731 . 1.011(3) no C74 . C75 . 1.396(4) yes C74 . H741 . 1.064(3) no C75 . H751 . 1.044(3) no C80 . C81 . 1.394(4) yes C80 . C85 . 1.394(4) yes C81 . C82 . 1.408(5) yes C81 . H811 . 0.794(3) no C82 . C83 . 1.351(6) yes C82 . H821 . 0.633(4) no C83 . C84 . 1.384(6) yes C83 . H831 . 1.048(3) no C84 . C85 . 1.387(4) yes C84 . H841 . 0.977(4) no C85 . H851 . 1.098(3) 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 As1 . Mo1 . As3 . 93.182(9) yes As1 . Mo1 . C1 . 95.45(7) yes As3 . Mo1 . C1 . 85.58(7) yes As1 . Mo1 . C2 . 87.51(8) yes As3 . Mo1 . C2 . 174.69(8) yes C1 . Mo1 . C2 . 89.1(1) yes As1 . Mo1 . C3 . 176.07(8) yes As3 . Mo1 . C3 . 88.39(8) yes C1 . Mo1 . C3 . 88.25(11) yes C2 . Mo1 . C3 . 91.26(11) yes As1 . Mo1 . C4 . 90.61(7) yes As3 . Mo1 . C4 . 98.69(7) yes C1 . Mo1 . C4 . 172.4(1) yes C2 . Mo1 . C4 . 86.6(1) yes C3 . Mo1 . C4 . 85.59(11) yes Mo1 . As1 . O1 . 120.82(6) yes Mo1 . As1 . C10 . 121.33(7) yes O1 . As1 . C10 . 97.3(1) yes Mo1 . As1 . C20 . 114.86(7) yes O1 . As1 . C20 . 98.10(9) yes C10 . As1 . C20 . 99.9(1) yes O1 . As2 . C30 . 97.2(1) yes O1 . As2 . C40 . 95.0(1) yes C30 . As2 . C40 . 97.6(1) yes Mo1 . As3 . O2 . 120.68(5) yes Mo1 . As3 . C50 . 120.30(7) yes O2 . As3 . C50 . 97.25(9) yes Mo1 . As3 . C60 . 117.41(7) yes O2 . As3 . C60 . 96.89(9) yes C50 . As3 . C60 . 99.5(1) yes O2 . As4 . C70 . 96.56(9) yes O2 . As4 . C80 . 95.8(1) yes C70 . As4 . C80 . 98.93(11) yes As1 . O1 . As2 . 122.2(1) yes As3 . O2 . As4 . 121.73(9) yes Mo1 . C1 . O3 . 175.0(2) yes Mo1 . C2 . O4 . 179.0(2) yes Mo1 . C3 . O5 . 178.5(3) yes Mo1 . C4 . O6 . 172.3(2) yes As1 . C10 . C11 . 121.2(2) yes As1 . C10 . C15 . 119.28(19) yes C11 . C10 . C15 . 119.5(2) yes C10 . C11 . C12 . 120.4(3) yes C10 . C11 . H111 . 120.8(3) no C12 . C11 . H111 . 118.7(3) no C11 . C12 . C13 . 119.5(3) yes C11 . C12 . H121 . 116.3(3) no C13 . C12 . H121 . 124.1(3) no C12 . C13 . C14 . 120.4(3) yes C12 . C13 . H131 . 118.2(3) no C14 . C13 . H131 . 121.4(3) no C13 . C14 . C15 . 119.7(3) yes C13 . C14 . H141 . 119.1(3) no C15 . C14 . H141 . 120.4(4) no C10 . C15 . C14 . 120.5(3) yes C10 . C15 . H151 . 127.5(3) no C14 . C15 . H151 . 111.0(3) no As1 . C20 . C21 . 121.87(19) yes As1 . C20 . C25 . 118.63(19) yes C21 . C20 . C25 . 119.5(2) yes C20 . C21 . C22 . 120.4(3) yes C20 . C21 . H211 . 121.0(3) no C22 . C21 . H211 . 118.0(3) no C21 . C22 . C23 . 119.7(3) yes C21 . C22 . H221 . 110.5(3) no C23 . C22 . H221 . 128.9(3) no C22 . C23 . C24 . 120.5(3) yes C22 . C23 . H231 . 112.3(3) no C24 . C23 . H231 . 124.5(3) no C23 . C24 . C25 . 119.4(3) yes C23 . C24 . H241 . 129.3(3) no C25 . C24 . H241 . 110.8(3) no C20 . C25 . C24 . 120.5(3) yes C20 . C25 . H251 . 120.5(2) no C24 . C25 . H251 . 118.5(3) no As2 . C30 . C31 . 121.8(2) yes As2 . C30 . C35 . 118.3(2) yes C31 . C30 . C35 . 119.8(2) yes C30 . C31 . C32 . 119.8(3) yes C30 . C31 . H311 . 120.4(3) no C32 . C31 . H311 . 119.2(3) no C31 . C32 . C33 . 120.2(3) yes C31 . C32 . H321 . 115.3(3) no C33 . C32 . H321 . 122.1(3) no C32 . C33 . C34 . 120.2(3) yes C32 . C33 . H331 . 117.6(3) no C34 . C33 . H331 . 122.2(3) no C33 . C34 . C35 . 119.6(3) yes C33 . C34 . H341 . 126.2(3) no C35 . C34 . H341 . 114.1(3) no C30 . C35 . C34 . 120.4(3) yes C30 . C35 . H351 . 123.5(3) no C34 . C35 . H351 . 116.1(3) no As2 . C40 . C41 . 123.4(2) yes As2 . C40 . C45 . 117.3(2) yes C41 . C40 . C45 . 119.2(3) yes C40 . C41 . C42 . 120.4(3) yes C40 . C41 . H411 . 115.5(3) no C42 . C41 . H411 . 124.0(3) no C41 . C42 . C43 . 120.2(3) yes C41 . C42 . H421 . 115.3(4) no C43 . C42 . H421 . 124.5(3) no C42 . C43 . C44 . 120.4(3) yes C42 . C43 . H431 . 114.9(4) no C44 . C43 . H431 . 124.7(4) no C43 . C44 . C45 . 120.1(3) yes C43 . C44 . H441 . 141.3(4) no C45 . C44 . H441 . 97.7(4) no C40 . C45 . C44 . 119.7(3) yes C40 . C45 . H451 . 118.3(3) no C44 . C45 . H451 . 121.5(4) no As3 . C50 . C51 . 121.68(19) yes As3 . C50 . C55 . 117.78(19) yes C51 . C50 . C55 . 120.5(2) yes C50 . C51 . C52 . 119.3(3) yes C50 . C51 . H511 . 119.5(2) no C52 . C51 . H511 . 121.1(3) no C51 . C52 . C53 . 119.7(3) yes C51 . C52 . H521 . 113.6(3) no C53 . C52 . H521 . 126.6(3) no C52 . C53 . C54 . 120.9(2) yes C52 . C53 . H531 . 117.4(3) no C54 . C53 . H531 . 121.7(3) no C53 . C54 . C55 . 119.8(3) yes C53 . C54 . H541 . 117.9(3) no C55 . C54 . H541 . 122.2(3) no C50 . C55 . C54 . 119.9(3) yes C50 . C55 . H551 . 114.9(3) no C54 . C55 . H551 . 125.2(3) no As3 . C60 . C61 . 120.61(17) yes As3 . C60 . C65 . 119.17(18) yes C61 . C60 . C65 . 119.8(2) yes C60 . C61 . C62 . 120.0(2) yes C60 . C61 . H611 . 120.2(3) no C62 . C61 . H611 . 119.6(3) no C61 . C62 . C63 . 120.4(2) yes C61 . C62 . H621 . 116.7(2) no C63 . C62 . H621 . 122.9(2) no C62 . C63 . C64 . 120.0(2) yes C62 . C63 . H631 . 123.2(3) no C64 . C63 . H631 . 116.5(3) no C63 . C64 . C65 . 119.8(2) yes C63 . C64 . H641 . 121.2(2) no C65 . C64 . H641 . 119.0(2) no C60 . C65 . C64 . 120.0(2) yes C60 . C65 . H651 . 121.1(2) no C64 . C65 . H651 . 118.4(2) no As4 . C70 . C71 . 119.05(19) yes As4 . C70 . C75 . 120.7(2) yes C71 . C70 . C75 . 119.8(2) yes C70 . C71 . C72 . 120.3(3) yes C70 . C71 . H711 . 122.8(2) no C72 . C71 . H711 . 116.4(3) no C71 . C72 . C73 . 119.7(3) yes C71 . C72 . H721 . 108.6(3) no C73 . C72 . H721 . 130.9(3) no C72 . C73 . C74 . 120.0(3) yes C72 . C73 . H731 . 121.6(3) no C74 . C73 . H731 . 118.0(3) no C73 . C74 . C75 . 120.7(3) yes C73 . C74 . H741 . 121.6(3) no C75 . C74 . H741 . 117.7(3) no C70 . C75 . C74 . 119.5(3) yes C70 . C75 . H751 . 117.8(2) no C74 . C75 . H751 . 122.7(3) no As4 . C80 . C81 . 118.1(2) yes As4 . C80 . C85 . 122.8(2) yes C81 . C80 . C85 . 119.0(3) yes C80 . C81 . C82 . 119.8(3) yes C80 . C81 . H811 . 115.7(3) no C82 . C81 . H811 . 123.5(3) no C81 . C82 . C83 . 120.5(3) yes C81 . C82 . H821 . 78.0(4) no C83 . C82 . H821 . 154.0(5) no C82 . C83 . C84 . 120.3(3) yes C82 . C83 . H831 . 134.0(4) no C84 . C83 . H831 . 105.3(4) no C83 . C84 . C85 . 120.4(3) yes C83 . C84 . H841 . 123.2(3) no C85 . C84 . H841 . 114.8(4) no C80 . C85 . C84 . 120.0(3) yes C80 . C85 . H851 . 116.7(3) no C84 . C85 . H851 . 121.2(3) no #END data_2 _audit_creation_date 99-06-17 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd18 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name 'Graham McCann ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Group 6 Transition Metal Carbonyl Complexes with Chalcogen-bridged Diarsenic(III) Ligands' # Title of paper ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software, Xpress, MAC Science, 1989' _computing_data_reduction ; DIP2000 software 'DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; DIP2000 software 'DENZO Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # 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 #**************************************************************************** _cell_length_a 9.939(2) _cell_angle_alpha 106.770(2) _cell_length_b 11.591(5) _cell_angle_beta 95.130(2) _cell_length_c 13.010(5) _cell_angle_gamma 112.790(2) _cell_volume 1288.2(2) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 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 'Cr ' 0.2840 0.6240 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International_Tables_Vol_IV_Table_2.2B' 'As ' -0.0300 2.0070 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972 2.5310 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 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' 'C ' 0.0020 0.0020 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 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C28 H20 As2 Cr1 O5 ' _chemical_formula_moiety ' C28 H20 As2 Cr1 O5 ' _chemical_compound_source ; ? ; _chemical_formula_weight 638.30 _cell_measurement_reflns_used 7268 _cell_measurement_theta_min 0 _cell_measurement_theta_max 26.57 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' rhombus ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 636.57 _exptl_absorpt_coefficient_mu 3.01 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 4872 _reflns_number_total 4872 _diffrn_reflns_av_R_equivalents 0.034 # Number of reflections with Friedels Law is 4872 # Number of reflections without Friedels Law is 0 _reflns_number_gt 4266 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _reflns_threshold_expression >3.00\s(I) _refine_diff_density_min -0.72 _refine_diff_density_max 0.54 _refine_ls_number_reflns 4266 _refine_ls_number_parameters 345 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0327 _refine_ls_goodness_of_fit_ref 1.0458 _refine_ls_shift/su_max 0.020528 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 1.39 0.250 0.863 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type As1 -6.36200(3) -0.15988(2) -0.269749(17) 0.0154 1.0000 Uani As2 -6.29413(3) 0.10994(2) -0.182275(17) 0.0147 1.0000 Uani Cr1 -6.15437(4) 0.01959(3) -0.29806(3) 0.0150 1.0000 Uani O1 -6.42888(19) -0.04926(15) -0.18319(13) 0.0208 1.0000 Uani O2 -6.3459(2) -0.0037(2) -0.50544(15) 0.0365 1.0000 Uani O3 -5.9382(2) 0.0474(2) -0.10166(16) 0.0373 1.0000 Uani O4 -5.9430(2) 0.28145(17) -0.31118(16) 0.0315 1.0000 Uani O5 -6.0084(3) -0.1340(2) -0.4344(2) 0.0479 1.0000 Uani C1 -6.2779(3) 0.0022(2) -0.42732(19) 0.0226 1.0000 Uani C2 -6.0226(3) 0.0379(2) -0.17310(19) 0.0213 1.0000 Uani C3 -6.0215(3) 0.1812(2) -0.30420(19) 0.0208 1.0000 Uani C4 -6.0672(3) -0.0775(2) -0.3841(2) 0.0250 1.0000 Uani C10 -6.5504(3) -0.2891(2) -0.37145(17) 0.0185 1.0000 Uani C11 -6.5886(3) -0.4247(2) -0.4040(2) 0.0258 1.0000 Uani C12 -6.7220(3) -0.5166(3) -0.4789(2) 0.0330 1.0000 Uani C13 -6.8190(3) -0.4735(3) -0.5202(2) 0.0337 1.0000 Uani C14 -6.7821(3) -0.3373(3) -0.4869(2) 0.0316 1.0000 Uani C15 -6.6479(3) -0.2449(3) -0.4136(2) 0.0242 1.0000 Uani C20 -6.3357(3) -0.2543(2) -0.17527(18) 0.0198 1.0000 Uani C21 -6.4374(3) -0.2884(3) -0.1098(2) 0.0268 1.0000 Uani C22 -6.4137(3) -0.3511(3) -0.0383(2) 0.0310 1.0000 Uani C23 -6.2911(3) -0.3810(3) -0.0338(2) 0.0320 1.0000 Uani C24 -6.1919(3) -0.3488(3) -0.0999(2) 0.0307 1.0000 Uani C25 -6.2136(3) -0.2848(2) -0.1715(2) 0.0239 1.0000 Uani C30 -6.2362(3) 0.2101(2) -0.02551(18) 0.0202 1.0000 Uani C31 -6.1915(3) 0.3475(2) 0.0102(2) 0.0274 1.0000 Uani C32 -6.1496(3) 0.4209(3) 0.1229(2) 0.0350 1.0000 Uani C33 -6.1538(3) 0.3581(3) 0.1987(2) 0.0357 1.0000 Uani C34 -6.1957(3) 0.2212(3) 0.1623(2) 0.0357 1.0000 Uani C35 -6.2365(3) 0.1469(3) 0.0502(2) 0.0283 1.0000 Uani C40 -6.4217(3) 0.1827(2) -0.23135(18) 0.0186 1.0000 Uani C41 -6.3671(3) 0.2725(3) -0.2857(2) 0.0251 1.0000 Uani C42 -6.4569(3) 0.3282(3) -0.3195(2) 0.0303 1.0000 Uani C43 -6.5985(3) 0.2940(3) -0.2993(2) 0.0295 1.0000 Uani C44 -6.6536(3) 0.2019(3) -0.2469(2) 0.0332 1.0000 Uani C45 -6.5648(3) 0.1470(3) -0.2120(2) 0.0278 1.0000 Uani H111 -6.5194 -0.4564 -0.3732 0.0245 1.0000 Uiso H121 -6.7480 -0.6142 -0.5030 0.0291 1.0000 Uiso H131 -6.9157 -0.5399 -0.5738 0.0282 1.0000 Uiso H141 -6.8530 -0.3063 -0.5163 0.0321 1.0000 Uiso H151 -6.6208 -0.1471 -0.3909 0.0257 1.0000 Uiso H211 -6.5263 -0.2680 -0.1142 0.0297 1.0000 Uiso H221 -6.4850 -0.3748 0.0100 0.0334 1.0000 Uiso H231 -6.2747 -0.4262 0.0178 0.0336 1.0000 Uiso H241 -6.1045 -0.3713 -0.0967 0.0317 1.0000 Uiso H251 -6.1420 -0.2612 -0.2195 0.0246 1.0000 Uiso H311 -6.1896 0.3932 -0.0446 0.0271 1.0000 Uiso H321 -6.1162 0.5198 0.1489 0.0327 1.0000 Uiso H331 -6.1268 0.4108 0.2794 0.0310 1.0000 Uiso H341 -6.1965 0.1759 0.2172 0.0339 1.0000 Uiso H351 -6.2659 0.0486 0.0244 0.0301 1.0000 Uiso H411 -6.2644 0.2970 -0.3004 0.0282 1.0000 Uiso H421 -6.4185 0.3930 -0.3586 0.0344 1.0000 Uiso H431 -6.6617 0.3355 -0.3223 0.0338 1.0000 Uiso H441 -6.7575 0.1753 -0.2344 0.0372 1.0000 Uiso H451 -6.6035 0.0821 -0.1731 0.0319 1.0000 Uiso 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 As1 0.01598(14) 0.01369(11) 0.01848(12) 0.00740(8) 0.00447(9) 0.00702(9 As2 0.01686(14) 0.01438(11) 0.01564(12) 0.00643(8) 0.00508(9) 0.00852(9 Cr1 0.0158(2) 0.01413(17) 0.01591(17) 0.00567(13) 0.00450(14) 0.00694(1 O1 0.0208(9) 0.0178(7) 0.0269(8) 0.0101(6) 0.0103(7) 0.0089(7) O2 0.0435(13) 0.0393(11) 0.0244(9) 0.0123(8) -0.0022(8) 0.0170(9) O3 0.0347(12) 0.0386(11) 0.0362(11) 0.0169(9) -0.0048(8) 0.0136(9) O4 0.0319(11) 0.0182(8) 0.041(1) 0.0121(7) 0.0112(8) 0.0061(8) O5 0.0517(15) 0.0396(11) 0.0553(14) 0.005(1) 0.0284(12) 0.0278(11 C1 0.0249(14) 0.0188(11) 0.0234(11) 0.0079(9) 0.008(1) 0.0078(9) C2 0.0193(13) 0.019(1) 0.0265(11) 0.0087(9) 0.0046(9) 0.0084(9) C3 0.0223(13) 0.0226(11) 0.021(1) 0.0052(9) 0.0064(9) 0.014(1) C4 0.0263(14) 0.0183(11) 0.0281(12) 0.0073(9) 0.008(1) 0.008(1) C10 0.0174(12) 0.0212(11) 0.017(1) 0.0078(8) 0.0042(8) 0.0077(9) C11 0.0243(14) 0.0202(11) 0.0302(12) 0.0092(9) 0.003(1) 0.007(1) C12 0.0295(16) 0.0239(12) 0.0350(14) 0.007(1) 0.0031(11) 0.0043(11 C13 0.0208(15) 0.0397(15) 0.0273(13) 0.0096(11) 0.002(1) 0.0021(11 C14 0.0231(15) 0.0490(16) 0.0294(13) 0.0197(12) 0.006(1) 0.0180(12 C15 0.0229(14) 0.0312(12) 0.0237(11) 0.014(1) 0.0074(9) 0.014(1) C20 0.0200(13) 0.017(1) 0.022(1) 0.0078(8) 0.0014(9) 0.0079(9) C21 0.0259(15) 0.0286(12) 0.0357(13) 0.0194(11) 0.0112(11) 0.0147(11 C22 0.0378(17) 0.0296(13) 0.0331(13) 0.0189(11) 0.0132(11) 0.0154(12 C23 0.0387(17) 0.0272(12) 0.0360(14) 0.0185(11) 0.0026(11) 0.0159(12 C24 0.0260(15) 0.0292(13) 0.0418(15) 0.0154(11) 0.0006(11) 0.0164(11 C25 0.0206(14) 0.0225(11) 0.0321(12) 0.012(1) 0.007(1) 0.011(1) C30 0.0190(13) 0.0242(11) 0.019(1) 0.0062(9) 0.0040(9) 0.0117(9) C31 0.0319(15) 0.0251(12) 0.0247(12) 0.005(1) 0.000(1) 0.0160(11 C32 0.0358(17) 0.0349(14) 0.0279(13) -0.0035(11) -0.0028(11) 0.0215(13 C33 0.0285(16) 0.0533(17) 0.0196(12) 0.0007(11) 0.001(1) 0.0215(13 C34 0.0321(17) 0.0541(17) 0.0224(12) 0.0176(12) 0.0067(11) 0.0171(13 C35 0.0326(15) 0.0336(13) 0.0249(12) 0.016(1) 0.009(1) 0.0157(11 C40 0.0198(12) 0.019(1) 0.018(1) 0.0063(8) 0.0032(8) 0.0095(9) C41 0.0240(14) 0.0290(12) 0.0323(12) 0.019(1) 0.011(1) 0.015(1) C42 0.0324(16) 0.0310(13) 0.0406(14) 0.0241(11) 0.0118(11) 0.0179(12 C43 0.0309(16) 0.0358(14) 0.0351(13) 0.0199(11) 0.0095(11) 0.0218(12 C44 0.0252(16) 0.0480(16) 0.0426(15) 0.0283(13) 0.0155(12) 0.0215(13 C45 0.0265(15) 0.0367(13) 0.0333(13) 0.0232(11) 0.0131(11) 0.0178(11 _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 As1 . Cr1 . 2.4442(4) yes As1 . O1 . 1.8207(15) yes As1 . C10 . 1.934(2) yes As1 . C20 . 1.928(2) yes As2 . Cr1 . 2.4262(4) yes As2 . O1 . 1.8080(15) yes As2 . C30 . 1.935(2) yes As2 . C40 . 1.928(2) yes Cr1 . C1 . 1.903(2) yes Cr1 . C2 . 1.900(2) yes Cr1 . C3 . 1.857(2) yes Cr1 . C4 . 1.863(2) yes O2 . C1 . 1.138(3) yes O3 . C2 . 1.144(3) yes O4 . C3 . 1.157(3) yes O5 . C4 . 1.148(3) yes C10 . C11 . 1.385(3) yes C10 . C15 . 1.398(3) yes C11 . C12 . 1.385(4) yes C11 . H111 . 1.000(3) no C12 . C13 . 1.380(4) yes C12 . H121 . 1.000(3) no C13 . C14 . 1.394(4) yes C13 . H131 . 1.000(3) no C14 . C15 . 1.383(4) yes C14 . H141 . 1.000(3) no C15 . H151 . 1.000(2) no C20 . C21 . 1.393(3) yes C20 . C25 . 1.390(3) yes C21 . C22 . 1.391(3) yes C21 . H211 . 1.000(3) no C22 . C23 . 1.391(4) yes C22 . H221 . 1.000(3) no C23 . C24 . 1.380(4) yes C23 . H231 . 1.000(2) no C24 . C25 . 1.396(3) yes C24 . H241 . 1.000(3) no C25 . H251 . 1.000(2) no C30 . C31 . 1.392(3) yes C30 . C35 . 1.387(3) yes C31 . C32 . 1.394(4) yes C31 . H311 . 1.000(2) no C32 . C33 . 1.380(4) yes C32 . H321 . 1.000(3) no C33 . C34 . 1.391(4) yes C33 . H331 . 1.000(3) no C34 . C35 . 1.390(4) yes C34 . H341 . 1.000(3) no C35 . H351 . 1.000(3) no C40 . C41 . 1.391(3) yes C40 . C45 . 1.388(3) yes C41 . C42 . 1.395(3) yes C41 . H411 . 1.000(3) no C42 . C43 . 1.379(4) yes C42 . H421 . 1.000(2) no C43 . C44 . 1.393(4) yes C43 . H431 . 1.000(2) no C44 . C45 . 1.386(4) yes C44 . H441 . 1.000(3) no C45 . H451 . 1.000(2) 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 Cr1 . As1 . O1 . 94.87(5) yes Cr1 . As1 . C10 . 128.90(6) yes O1 . As1 . C10 . 98.75(9) yes Cr1 . As1 . C20 . 123.46(7) yes O1 . As1 . C20 . 100.77(9) yes C10 . As1 . C20 . 101.90(9) yes Cr1 . As2 . O1 . 95.82(5) yes Cr1 . As2 . C30 . 128.68(7) yes O1 . As2 . C30 . 99.70(9) yes Cr1 . As2 . C40 . 123.29(7) yes O1 . As2 . C40 . 102.15(9) yes C30 . As2 . C40 . 100.65(9) yes As1 . Cr1 . As2 . 69.493(12) yes As1 . Cr1 . C1 . 90.92(7) yes As2 . Cr1 . C1 . 91.20(7) yes As1 . Cr1 . C2 . 91.37(7) yes As2 . Cr1 . C2 . 91.53(7) yes C1 . Cr1 . C2 . 176.9(1) yes As1 . Cr1 . C3 . 165.57(7) yes As2 . Cr1 . C3 . 96.37(7) yes C1 . Cr1 . C3 . 86.4(1) yes C2 . Cr1 . C3 . 91.9(1) yes As1 . Cr1 . C4 . 100.74(7) yes As2 . Cr1 . C4 . 170.12(7) yes C1 . Cr1 . C4 . 90.42(11) yes C2 . Cr1 . C4 . 87.13(11) yes C3 . Cr1 . C4 . 93.5(1) yes As1 . O1 . As2 . 99.81(8) yes Cr1 . C1 . O2 . 176.7(2) yes Cr1 . C2 . O3 . 176.1(2) yes Cr1 . C3 . O4 . 177.3(2) yes Cr1 . C4 . O5 . 177.4(3) yes As1 . C10 . C11 . 120.64(18) yes As1 . C10 . C15 . 119.56(17) yes C11 . C10 . C15 . 119.8(2) yes C10 . C11 . C12 . 120.4(2) yes C10 . C11 . H111 . 119.8(2) no C12 . C11 . H111 . 119.8(2) no C11 . C12 . C13 . 120.0(2) yes C11 . C12 . H121 . 120.0(3) no C13 . C12 . H121 . 120.0(3) no C12 . C13 . C14 . 119.9(2) yes C12 . C13 . H131 . 120.1(3) no C14 . C13 . H131 . 120.1(3) no C13 . C14 . C15 . 120.4(2) yes C13 . C14 . H141 . 119.8(3) no C15 . C14 . H141 . 119.8(3) no C10 . C15 . C14 . 119.5(2) yes C10 . C15 . H151 . 120.2(2) no C14 . C15 . H151 . 120.2(2) no As1 . C20 . C21 . 119.60(18) yes As1 . C20 . C25 . 119.55(17) yes C21 . C20 . C25 . 120.8(2) yes C20 . C21 . C22 . 119.1(2) yes C20 . C21 . H211 . 120.4(2) no C22 . C21 . H211 . 120.4(2) no C21 . C22 . C23 . 120.1(2) yes C21 . C22 . H221 . 119.9(3) no C23 . C22 . H221 . 119.9(2) no C22 . C23 . C24 . 120.5(2) yes C22 . C23 . H231 . 119.8(3) no C24 . C23 . H231 . 119.8(3) no C23 . C24 . C25 . 120.0(2) yes C23 . C24 . H241 . 120.0(2) no C25 . C24 . H241 . 120.0(3) no C20 . C25 . C24 . 119.4(2) yes C20 . C25 . H251 . 120.3(2) no C24 . C25 . H251 . 120.3(2) no As2 . C30 . C31 . 118.84(17) yes As2 . C30 . C35 . 120.75(18) yes C31 . C30 . C35 . 120.4(2) yes C30 . C31 . C32 . 119.5(2) yes C30 . C31 . H311 . 120.3(2) no C32 . C31 . H311 . 120.3(2) no C31 . C32 . C33 . 120.5(3) yes C31 . C32 . H321 . 119.8(3) no C33 . C32 . H321 . 119.8(3) no C32 . C33 . C34 . 119.7(2) yes C32 . C33 . H331 . 120.2(3) no C34 . C33 . H331 . 120.2(3) no C33 . C34 . C35 . 120.5(2) yes C33 . C34 . H341 . 119.7(3) no C35 . C34 . H341 . 119.7(3) no C30 . C35 . C34 . 119.5(2) yes C30 . C35 . H351 . 120.3(2) no C34 . C35 . H351 . 120.3(2) no As2 . C40 . C41 . 118.76(18) yes As2 . C40 . C45 . 120.65(17) yes C41 . C40 . C45 . 120.6(2) yes C40 . C41 . C42 . 119.4(2) yes C40 . C41 . H411 . 120.3(2) no C42 . C41 . H411 . 120.3(2) no C41 . C42 . C43 . 120.1(2) yes C41 . C42 . H421 . 119.9(3) no C43 . C42 . H421 . 119.9(2) no C42 . C43 . C44 . 120.2(2) yes C42 . C43 . H431 . 119.9(2) no C44 . C43 . H431 . 119.9(3) no C43 . C44 . C45 . 120.2(2) yes C43 . C44 . H441 . 119.9(3) no C45 . C44 . H441 . 119.9(3) no C40 . C45 . C44 . 119.5(2) yes C40 . C45 . H451 . 120.2(2) no C44 . C45 . H451 . 120.2(2) no #END data_3 _audit_creation_date 99-06-17 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd38 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name ' Graham McCann ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Group 6 Transition Metal Carbonyl Complexes with Chalcogen-bridged Diarsenic(III) Ligands' # Title of paper ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software, Xpress, MAC Science, 1989' _computing_data_reduction ; DIP2000 software 'DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; DIP2000 software 'DENZO Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # 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 #**************************************************************************** _cell_length_a 10.6640(3) _cell_angle_alpha 90. _cell_length_b 9.6160(3) _cell_angle_beta 92.816(2) _cell_length_c 26.2380(5) _cell_angle_gamma 90. _cell_volume 2687.3(3) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' 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 'Cr ' 0.2840 0.6240 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International_Tables_Vol_IV_Table_2.2B' 'As ' -0.0300 2.0070 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972 2.5310 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 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' 'C ' 0.0020 0.0020 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 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H20 As2 Cr1 O6 ' _chemical_formula_moiety ' C29 H20 As2 Cr1 O6 ' _chemical_compound_source ; ? ; _chemical_formula_weight 666.31 _cell_measurement_reflns_used 18543 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 125 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.35 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1329.18 _exptl_absorpt_coefficient_mu 2.89 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.31 # Sheldrick geometric definitions 0.31 0.31 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 125 _diffrn_reflns_number 5582 _reflns_number_total 5582 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 5582 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5613 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_gt 4550 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _reflns_threshold_expression >3.00\s(I) _refine_diff_density_min -0.68 _refine_diff_density_max 0.61 _refine_ls_number_reflns 4550 _refine_ls_number_parameters 343 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0325 _refine_ls_goodness_of_fit_ref 1.0608 _refine_ls_shift/su_max 0.002177 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 1.67 0.780 1.23 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \wA # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type As1 0.795562(17) -0.060595(19) 0.633537(7) 0.0234 1.0000 Uani As2 0.609539(18) 0.06555(2) 0.547616(7) 0.0265 1.0000 Uani Cr1 0.97465(3) 0.02513(3) 0.685190(11) 0.0237 1.0000 Uani O1 1.19736(13) 0.13571(15) 0.74791(5) 0.0344 1.0000 Uani O2 0.85005(14) 0.30758(15) 0.69616(6) 0.0355 1.0000 Uani O3 1.11022(14) -0.25365(15) 0.68375(6) 0.0360 1.0000 Uani O4 0.86458(15) -0.06239(15) 0.78514(6) 0.0365 1.0000 Uani O5 1.07850(15) 0.10908(18) 0.58333(6) 0.0422 1.0000 Uani O6 0.76062(12) 0.06309(13) 0.58447(5) 0.0288 1.0000 Uani C1 1.11331(18) 0.0945(2) 0.72349(7) 0.0285 1.0000 Uani C2 0.89503(17) 0.2007(2) 0.69085(7) 0.0272 1.0000 Uani C3 1.05770(17) -0.1503(2) 0.68284(7) 0.0282 1.0000 Uani C4 0.90330(18) -0.0309(2) 0.74700(8) 0.0284 1.0000 Uani C5 1.04043(19) 0.0781(2) 0.62152(8) 0.0321 1.0000 Uani C11 0.81685(17) -0.2299(2) 0.59464(7) 0.0277 1.0000 Uani C12 0.84565(19) -0.3531(2) 0.62077(8) 0.0316 1.0000 Uani C13 0.8707(2) -0.4727(2) 0.59377(9) 0.0353 1.0000 Uani C14 0.8677(2) -0.4716(2) 0.54108(9) 0.0379 1.0000 Uani C15 0.8392(2) -0.3486(2) 0.51487(8) 0.0394 1.0000 Uani C16 0.81558(19) -0.2277(2) 0.54146(8) 0.0332 1.0000 Uani C21 0.63537(17) -0.0864(2) 0.66440(7) 0.0278 1.0000 Uani C22 0.55584(19) -0.1969(2) 0.65188(8) 0.0326 1.0000 Uani C23 0.44079(19) -0.2069(2) 0.67483(9) 0.0381 1.0000 Uani C24 0.40525(19) -0.1071(2) 0.70906(8) 0.0350 1.0000 Uani C25 0.48411(19) 0.0052(2) 0.72091(8) 0.0327 1.0000 Uani C26 0.59950(18) 0.0148(2) 0.69896(7) 0.0298 1.0000 Uani C31 0.67116(18) 0.1987(2) 0.49841(7) 0.0295 1.0000 Uani C32 0.59697(19) 0.3099(2) 0.48133(8) 0.0342 1.0000 Uani C33 0.6395(2) 0.3995(2) 0.44428(8) 0.0381 1.0000 Uani C34 0.7558(2) 0.3775(2) 0.42378(8) 0.0363 1.0000 Uani C35 0.8294(2) 0.2660(2) 0.44049(8) 0.0354 1.0000 Uani C36 0.78803(18) 0.1767(2) 0.47762(8) 0.0318 1.0000 Uani C41 0.52439(17) 0.1964(2) 0.59093(7) 0.0290 1.0000 Uani C42 0.39898(19) 0.1757(2) 0.60137(8) 0.0337 1.0000 Uani C43 0.34257(19) 0.2625(2) 0.63629(8) 0.0365 1.0000 Uani C44 0.4115(2) 0.3674(2) 0.66096(8) 0.0359 1.0000 Uani C45 0.5368(2) 0.3885(2) 0.65022(8) 0.0347 1.0000 Uani C46 0.59218(18) 0.3043(2) 0.61489(8) 0.0312 1.0000 Uani H121 0.8466 -0.3537 0.6594 0.0295 1.0000 Uiso H131 0.8927 -0.5620 0.6128 0.0330 1.0000 Uiso H141 0.8842 -0.5593 0.5215 0.0359 1.0000 Uiso H151 0.8364 -0.3477 0.4765 0.0371 1.0000 Uiso H161 0.7974 -0.1381 0.5223 0.0312 1.0000 Uiso H221 0.5812 -0.2689 0.6264 0.0306 1.0000 Uiso H231 0.3826 -0.2876 0.6665 0.0353 1.0000 Uiso H241 0.3225 -0.1139 0.7256 0.0335 1.0000 Uiso H251 0.4581 0.0789 0.7455 0.0306 1.0000 Uiso H261 0.6579 0.0937 0.7080 0.0291 1.0000 Uiso H321 0.5117 0.3248 0.4961 0.0312 1.0000 Uiso H331 0.5852 0.4801 0.4320 0.0361 1.0000 Uiso H341 0.7872 0.4435 0.3972 0.0344 1.0000 Uiso H351 0.9130 0.2494 0.4256 0.0333 1.0000 Uiso H361 0.8424 0.0963 0.4899 0.0302 1.0000 Uiso H421 0.3492 0.0984 0.5840 0.0321 1.0000 Uiso H431 0.2516 0.2485 0.6435 0.0348 1.0000 Uiso H441 0.3707 0.4279 0.6872 0.0334 1.0000 Uiso H451 0.5873 0.4646 0.6678 0.0328 1.0000 Uiso H461 0.6818 0.3218 0.6063 0.0288 1.0000 Uiso 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 As1 0.02096(11) 0.02783(11) 0.02110(12) -0.00117(6) -0.00115(8) -0.00083(6 As2 0.02294(11) 0.03122(12) 0.02493(12) 0.00062(7) -0.00287(8) -0.00127(7 Cr1 0.02155(14) 0.02797(15) 0.02136(15) -0.00014(11) -0.00099(11) -0.00106(1 O1 0.0290(7) 0.0413(8) 0.0324(7) -0.0031(6) -0.0045(6) -0.0038(6) O2 0.0389(8) 0.0324(8) 0.0348(8) -0.0007(6) -0.0024(6) 0.0028(6) O3 0.0368(7) 0.0356(8) 0.0355(8) 0.0001(6) 0.0015(6) 0.0071(6) O4 0.0401(8) 0.0402(8) 0.0299(8) 0.0030(6) 0.0078(7) -0.0019(6) O5 0.0412(8) 0.056(1) 0.0304(8) 0.0043(7) 0.0074(7) -0.0086(7) O6 0.0234(6) 0.0346(7) 0.0281(7) 0.0023(5) -0.0028(5) -0.0014(5) C1 0.0288(9) 0.0289(9) 0.028(1) 0.0020(7) 0.0021(8) 0.0020(7) C2 0.0270(9) 0.034(1) 0.0201(9) 0.0007(7) -0.0034(7) -0.0046(8) C3 0.0252(9) 0.037(1) 0.0222(9) -0.0015(7) 0.0003(7) -0.0033(8) C4 0.0258(9) 0.0303(9) 0.029(1) -0.0030(7) -0.0009(8) 0.0024(7) C5 0.0272(9) 0.037(1) 0.0319(11) -0.0006(8) -0.0022(8) -0.0024(8) C11 0.0234(8) 0.0308(9) 0.029(1) -0.0052(7) 0.0004(7) -0.0035(7) C12 0.033(1) 0.035(1) 0.0273(9) 0.0007(8) 0.0035(8) -0.0042(8) C13 0.0385(11) 0.0304(9) 0.0371(11) 0.0018(8) 0.0035(9) -0.0038(8) C14 0.0422(12) 0.033(1) 0.0384(12) -0.0087(9) 0.005(1) -0.0047(9) C15 0.0478(12) 0.0424(11) 0.028(1) -0.0042(8) 0.0021(9) 0.000(1) C16 0.037(1) 0.035(1) 0.027(1) -0.0012(8) 0.0008(8) -0.0002(8) C21 0.0224(8) 0.035(1) 0.0255(9) 0.0012(7) -0.0008(7) -0.0005(7) C22 0.0290(9) 0.036(1) 0.032(1) -0.0025(8) -0.0012(8) -0.0033(8) C23 0.0278(9) 0.0460(12) 0.0404(12) -0.0017(9) -0.0003(9) -0.0073(9) C24 0.0251(9) 0.0458(11) 0.0342(11) 0.0035(9) 0.0021(8) -0.0017(8) C25 0.0298(9) 0.0407(11) 0.027(1) -0.0006(8) 0.0004(8) 0.0040(8) C26 0.0280(9) 0.034(1) 0.027(1) -0.0002(7) -0.0008(8) -0.0032(8) C31 0.0288(9) 0.035(1) 0.0245(9) -0.0006(7) -0.0029(7) -0.0028(7) C32 0.031(1) 0.0428(11) 0.029(1) 0.0017(8) -0.0005(8) 0.0020(8) C33 0.0428(12) 0.0409(11) 0.0302(11) 0.0036(9) -0.0032(9) 0.0040(9) C34 0.0436(12) 0.0400(11) 0.025(1) 0.0020(8) 0.0011(9) -0.0038(9) C35 0.034(1) 0.0440(11) 0.028(1) -0.0042(8) 0.0034(8) -0.0023(9) C36 0.0300(9) 0.036(1) 0.029(1) -0.0014(8) -0.0002(8) 0.0011(8) C41 0.0256(9) 0.035(1) 0.027(1) 0.0041(7) 0.0012(7) 0.0017(7) C42 0.0270(9) 0.0432(11) 0.031(1) 0.0023(8) -0.0020(8) -0.0004(8) C43 0.028(1) 0.0495(12) 0.0322(11) 0.0043(9) 0.0030(8) 0.0007(9) C44 0.033(1) 0.0451(12) 0.030(1) 0.0022(8) 0.0046(8) 0.0065(9) C45 0.0347(11) 0.0384(11) 0.031(1) 0.0022(8) -0.0013(8) 0.0006(8) C46 0.0272(9) 0.036(1) 0.030(1) 0.0027(8) 0.0009(8) 0.0012(8) _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 As1 . Cr1 . 2.4309(3) yes As1 . O6 . 1.7787(13) yes As1 . C11 . 1.9409(19) yes As1 . C21 . 1.9421(19) yes As2 . O6 . 1.8380(13) yes As2 . C31 . 1.955(2) yes As2 . C41 . 1.949(2) yes Cr1 . C1 . 1.869(2) yes Cr1 . C2 . 1.899(2) yes Cr1 . C3 . 1.907(2) yes Cr1 . C4 . 1.903(2) yes Cr1 . C5 . 1.912(2) yes O1 . C1 . 1.147(2) yes O2 . C2 . 1.145(2) yes O3 . C3 . 1.141(2) yes O4 . C4 . 1.142(3) yes O5 . C5 . 1.139(3) yes C11 . C12 . 1.395(3) yes C11 . C16 . 1.395(3) yes C12 . C13 . 1.384(3) yes C12 . H121 . 1.012(2) no C13 . C14 . 1.381(3) yes C13 . H131 . 1.015(2) no C14 . C15 . 1.394(3) yes C14 . H141 . 1.007(2) no C15 . C16 . 1.385(3) yes C15 . H151 . 1.006(2) no C16 . H161 . 1.012(2) no C21 . C22 . 1.389(3) yes C21 . C26 . 1.397(3) yes C22 . C23 . 1.396(3) yes C22 . H221 . 1.008(2) no C23 . C24 . 1.380(3) yes C23 . H231 . 1.011(2) no C24 . C25 . 1.394(3) yes C24 . H241 . 1.005(2) no C25 . C26 . 1.387(3) yes C25 . H251 . 1.007(2) no C26 . H261 . 1.0030(19) no C31 . C32 . 1.391(3) yes C31 . C36 . 1.401(3) yes C32 . C33 . 1.392(3) yes C32 . H321 . 1.016(2) no C33 . C34 . 1.392(3) yes C33 . H331 . 1.011(2) no C34 . C35 . 1.387(3) yes C34 . H341 . 1.012(2) no C35 . C36 . 1.387(3) yes C35 . H351 . 1.003(2) no C36 . H361 . 1.009(2) no C41 . C42 . 1.393(3) yes C41 . C46 . 1.396(3) yes C42 . C43 . 1.398(3) yes C42 . H421 . 1.009(2) no C43 . C44 . 1.389(3) yes C43 . H431 . 1.007(2) no C44 . C45 . 1.393(3) yes C44 . H441 . 1.015(2) no C45 . C46 . 1.385(3) yes C45 . H451 . 1.008(2) no C46 . H461 . 1.007(2) 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 Cr1 . As1 . O6 . 107.92(4) yes Cr1 . As1 . C11 . 117.95(5) yes O6 . As1 . C11 . 101.89(7) yes Cr1 . As1 . C21 . 119.60(6) yes O6 . As1 . C21 . 103.30(7) yes C11 . As1 . C21 . 103.89(8) yes O6 . As2 . C31 . 92.38(7) yes O6 . As2 . C41 . 97.06(7) yes C31 . As2 . C41 . 98.27(9) yes As1 . Cr1 . C1 . 178.44(6) yes As1 . Cr1 . C2 . 90.18(5) yes C1 . Cr1 . C2 . 89.18(8) yes As1 . Cr1 . C3 . 92.03(6) yes C1 . Cr1 . C3 . 88.65(8) yes C2 . Cr1 . C3 . 177.22(8) yes As1 . Cr1 . C4 . 92.47(6) yes C1 . Cr1 . C4 . 88.95(8) yes C2 . Cr1 . C4 . 89.19(8) yes C3 . Cr1 . C4 . 89.03(8) yes As1 . Cr1 . C5 . 85.13(6) yes C1 . Cr1 . C5 . 93.45(9) yes C2 . Cr1 . C5 . 90.93(8) yes C3 . Cr1 . C5 . 90.94(8) yes C4 . Cr1 . C5 . 177.59(8) yes As1 . O6 . As2 . 122.44(7) yes Cr1 . C1 . O1 . 178.51(17) yes Cr1 . C2 . O2 . 177.07(16) yes Cr1 . C3 . O3 . 176.58(16) yes Cr1 . C4 . O4 . 177.27(17) yes Cr1 . C5 . O5 . 179.28(18) yes As1 . C11 . C12 . 118.84(15) yes As1 . C11 . C16 . 121.17(15) yes C12 . C11 . C16 . 119.71(18) yes C11 . C12 . C13 . 119.83(19) yes C11 . C12 . H121 . 119.21(19) no C13 . C12 . H121 . 121.0(2) no C12 . C13 . C14 . 120.7(2) yes C12 . C13 . H131 . 119.8(2) no C14 . C13 . H131 . 119.5(2) no C13 . C14 . C15 . 119.6(2) yes C13 . C14 . H141 . 120.6(2) no C15 . C14 . H141 . 119.8(2) no C14 . C15 . C16 . 120.3(2) yes C14 . C15 . H151 . 119.7(2) no C16 . C15 . H151 . 120.0(2) no C11 . C16 . C15 . 119.86(19) yes C11 . C16 . H161 . 120.21(19) no C15 . C16 . H161 . 119.9(2) no As1 . C21 . C22 . 122.59(15) yes As1 . C21 . C26 . 117.14(14) yes C22 . C21 . C26 . 120.23(18) yes C21 . C22 . C23 . 119.33(19) yes C21 . C22 . H221 . 120.07(19) no C23 . C22 . H221 . 120.60(19) no C22 . C23 . C24 . 120.53(19) yes C22 . C23 . H231 . 120.2(2) no C24 . C23 . H231 . 119.3(2) no C23 . C24 . C25 . 120.12(19) yes C23 . C24 . H241 . 120.7(2) no C25 . C24 . H241 . 119.1(2) no C24 . C25 . C26 . 119.78(19) yes C24 . C25 . H251 . 120.4(2) no C26 . C25 . H251 . 119.9(2) no C21 . C26 . C25 . 120.00(18) yes C21 . C26 . H261 . 119.65(18) no C25 . C26 . H261 . 120.35(19) no As2 . C31 . C32 . 120.78(15) yes As2 . C31 . C36 . 119.54(15) yes C32 . C31 . C36 . 119.55(18) yes C31 . C32 . C33 . 120.08(19) yes C31 . C32 . H321 . 119.4(2) no C33 . C32 . H321 . 120.5(2) no C32 . C33 . C34 . 120.2(2) yes C32 . C33 . H331 . 119.8(2) no C34 . C33 . H331 . 120.0(2) no C33 . C34 . C35 . 119.77(19) yes C33 . C34 . H341 . 120.1(2) no C35 . C34 . H341 . 120.1(2) no C34 . C35 . C36 . 120.37(19) yes C34 . C35 . H351 . 120.0(2) no C36 . C35 . H351 . 119.6(2) no C31 . C36 . C35 . 120.03(19) yes C31 . C36 . H361 . 119.97(19) no C35 . C36 . H361 . 120.00(19) no As2 . C41 . C42 . 120.12(15) yes As2 . C41 . C46 . 119.75(14) yes C42 . C41 . C46 . 119.92(19) yes C41 . C42 . C43 . 119.5(2) yes C41 . C42 . H421 . 120.3(2) no C43 . C42 . H421 . 120.21(19) no C42 . C43 . C44 . 120.28(19) yes C42 . C43 . H431 . 119.5(2) no C44 . C43 . H431 . 120.2(2) no C43 . C44 . C45 . 120.2(2) yes C43 . C44 . H441 . 119.8(2) no C45 . C44 . H441 . 120.0(2) no C44 . C45 . C46 . 119.7(2) yes C44 . C45 . H451 . 120.7(2) no C46 . C45 . H451 . 119.7(2) no C41 . C46 . C45 . 120.48(18) yes C41 . C46 . H461 . 120.0(2) no C45 . C46 . H461 . 119.5(2) no #END data_4 _audit_creation_date 99-06-17 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd41 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name 'Graham McCann ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Group 6 Transition Metal Carbonyl Complexes with Chalcogen-bridged Diarsenic(III) Ligands' # Title of paper ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software, Xpress, MAC Science, 1989' _computing_data_reduction ; DIP2000 software 'DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; DIP2000 software 'DENZO Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # 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 #**************************************************************************** _cell_length_a 10.790(6) _cell_angle_alpha 79.572(3) _cell_length_b 13.288(7) _cell_angle_beta 85.858(3) _cell_length_c 19.831(6) _cell_angle_gamma 82.035(3) _cell_volume 2766.1(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' 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 'As ' -0.0300 2.0070 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972 2.5310 'International_Tables_Vol_IV_Table_2.2B' 'Cr ' 0.2840 0.6240 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 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' 'O ' 0.0080 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' 'C ' 0.0020 0.0020 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 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C56 H40 As4 Cr2 O8 S2 ' _chemical_formula_moiety ' C56 H40 As4 Cr2 O8 S2 s' _chemical_compound_source ; ? ; _chemical_formula_weight 1308.73 _cell_measurement_reflns_used 13010 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 298 _cell_formula_units_Z 2 _exptl_crystal_description ' irregular ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1305.56 _exptl_absorpt_coefficient_mu 2.88 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.42 # Sheldrick geometric definitions 0.42 0.42 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 298 _diffrn_reflns_number 10569 _reflns_number_total 10569 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 10569 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11555 _diffrn_measured_fraction_theta_max 0.915 _reflns_number_gt 6333 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _reflns_threshold_expression >3.00\s(I) _refine_diff_density_min -0.58 _refine_diff_density_max 1.05 _refine_ls_number_reflns 6333 _refine_ls_number_parameters 649 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0489 _refine_ls_goodness_of_fit_ref 1.0959 _refine_ls_shift/su_max 0.001419 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 1.11 0.412 0.773 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \wA # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type As1 2.67728(5) -0.17577(4) 0.10182(3) 0.0335 1.0000 Uani As2 2.42235(5) -0.24565(4) 0.12175(3) 0.0332 1.0000 Uani As3 2.17086(6) 0.29491(5) 0.36250(3) 0.0455 1.0000 Uani As4 1.92610(6) 0.21472(4) 0.41113(3) 0.0407 1.0000 Uani Cr1 2.58590(8) -0.27856(6) 0.20457(4) 0.0332 1.0000 Uani Cr2 1.95759(9) 0.37375(7) 0.33144(5) 0.0422 1.0000 Uani S1 2.50337(14) -0.12918(11) 0.04028(8) 0.0445 1.0000 Uani S2 2.12592(16) 0.13870(13) 0.4153(1) 0.0589 1.0000 Uani O1 2.7950(5) -0.2961(4) 0.2991(3) 0.0746 1.0000 Uani O2 2.4639(5) -0.0919(4) 0.2636(3) 0.0632 1.0000 Uani O3 2.7063(5) -0.4781(4) 0.1598(3) 0.0718 1.0000 Uani O4 2.4333(5) -0.4048(4) 0.3114(3) 0.0821 1.0000 Uani O5 1.6827(6) 0.4359(5) 0.3179(3) 0.0911 1.0000 Uani O6 1.9388(6) 0.5251(5) 0.4311(3) 0.0890 1.0000 Uani O7 1.9557(7) 0.2540(5) 0.2164(3) 0.1009 1.0000 Uani O8 2.0283(7) 0.5467(5) 0.2224(4) 0.1132 1.0000 Uani C1 2.7171(6) -0.2891(5) 0.2625(3) 0.0478 1.0000 Uani C2 2.5100(5) -0.1601(5) 0.2394(3) 0.0435 1.0000 Uani C3 2.6603(6) -0.4017(5) 0.1748(3) 0.0461 1.0000 Uani C4 2.4926(6) -0.3570(4) 0.2711(3) 0.0485 1.0000 Uani C5 1.7879(7) 0.4133(5) 0.3222(4) 0.0577 1.0000 Uani C6 1.9478(7) 0.4642(5) 0.3963(4) 0.0580 1.0000 Uani C7 1.9590(7) 0.2969(5) 0.2612(3) 0.0565 1.0000 Uani C8 2.0028(7) 0.4802(6) 0.2652(4) 0.0675 1.0000 Uani C11 2.7443(5) -0.0459(4) 0.0970(3) 0.0378 1.0000 Uani C12 2.8128(7) -0.0039(5) 0.0405(3) 0.0551 1.0000 Uani C13 2.8610(7) 0.0882(5) 0.0396(4) 0.0660 1.0000 Uani C14 2.8414(6) 0.1365(5) 0.0957(4) 0.0613 1.0000 Uani C15 2.7744(6) 0.0940(5) 0.1526(4) 0.0600 1.0000 Uani C16 2.7248(6) 0.0042(4) 0.1530(3) 0.0489 1.0000 Uani C21 2.7958(5) -0.2441(4) 0.0406(3) 0.0384 1.0000 Uani C22 2.7783(6) -0.2345(5) -0.0295(3) 0.0536 1.0000 Uani C23 2.8669(8) -0.2869(6) -0.0695(3) 0.0647 1.0000 Uani C24 2.9683(7) -0.3484(6) -0.0399(4) 0.0665 1.0000 Uani C25 2.9851(7) -0.3581(6) 0.0292(4) 0.0680 1.0000 Uani C26 2.8982(6) -0.3057(5) 0.0694(3) 0.0527 1.0000 Uani C31 2.3798(5) -0.3481(4) 0.0724(3) 0.0382 1.0000 Uani C32 2.3670(6) -0.4459(5) 0.1102(3) 0.0546 1.0000 Uani C33 2.3340(7) -0.5208(5) 0.0764(4) 0.0666 1.0000 Uani C34 2.3172(6) -0.5013(5) 0.0081(4) 0.0572 1.0000 Uani C35 2.3305(6) -0.4042(5) -0.0288(3) 0.0560 1.0000 Uani C36 2.3617(6) -0.3282(5) 0.0032(3) 0.0471 1.0000 Uani C41 2.2592(5) -0.1747(4) 0.1456(3) 0.0389 1.0000 Uani C42 2.2449(6) -0.0701(5) 0.1458(4) 0.0561 1.0000 Uani C43 2.1346(8) -0.0222(6) 0.1724(4) 0.0733 1.0000 Uani C44 2.0397(7) -0.0802(7) 0.1981(4) 0.0787 1.0000 Uani C45 2.0533(7) -0.1835(7) 0.1960(4) 0.0747 1.0000 Uani C46 2.1642(6) -0.2318(5) 0.1693(3) 0.0539 1.0000 Uani C51 2.3021(6) 0.2625(5) 0.2949(3) 0.0494 1.0000 Uani C52 2.2956(8) 0.1856(6) 0.2577(4) 0.0685 1.0000 Uani C53 2.3840(9) 0.1697(6) 0.2050(4) 0.0754 1.0000 Uani C54 2.4776(8) 0.2318(7) 0.1888(4) 0.0739 1.0000 Uani C55 2.4854(8) 0.3077(6) 0.2266(4) 0.0748 1.0000 Uani C56 2.3983(7) 0.3220(5) 0.2800(4) 0.0643 1.0000 Uani C61 2.2646(7) 0.3374(6) 0.4304(3) 0.0628 1.0000 Uani C62 2.3288(12) 0.2686(9) 0.4777(6) 0.1236 1.0000 Uani C63 2.3921(16) 0.3060(14) 0.5269(7) 0.1656 1.0000 Uani C64 2.3863(14) 0.4086(15) 0.5247(6) 0.1337 1.0000 Uani C65 2.326(1) 0.478(1) 0.4764(7) 0.1066 1.0000 Uani C66 2.2619(8) 0.4438(7) 0.4284(4) 0.0799 1.0000 Uani C71 1.8712(6) 0.2067(5) 0.5073(3) 0.0486 1.0000 Uani C72 1.9246(8) 0.2649(6) 0.5460(4) 0.0684 1.0000 Uani C73 1.885(1) 0.2624(7) 0.6149(4) 0.0844 1.0000 Uani C74 1.7946(9) 0.2017(7) 0.6436(4) 0.0787 1.0000 Uani C75 1.7456(8) 0.1429(7) 0.6059(4) 0.0807 1.0000 Uani C76 1.7840(7) 0.1437(6) 0.5370(4) 0.0664 1.0000 Uani C81 1.8363(6) 0.1121(5) 0.3848(3) 0.0487 1.0000 Uani C82 1.8889(7) 0.0092(5) 0.3897(4) 0.0680 1.0000 Uani C83 1.816(1) -0.0618(6) 0.3741(5) 0.0891 1.0000 Uani C84 1.697(1) -0.0318(7) 0.3538(4) 0.0876 1.0000 Uani C85 1.6490(8) 0.0683(8) 0.3474(5) 0.0912 1.0000 Uani C86 1.7183(7) 0.1412(6) 0.3633(4) 0.0718 1.0000 Uani H121 2.8274 -0.0405 -0.0012 0.0509 1.0000 Uiso H131 2.9119 0.1212 -0.0028 0.0609 1.0000 Uiso H141 2.8757 0.2037 0.0963 0.0598 1.0000 Uiso H151 2.7597 0.1304 0.1946 0.0564 1.0000 Uiso H161 2.6719 -0.0260 0.1946 0.0471 1.0000 Uiso H221 2.7013 -0.1899 -0.0503 0.0508 1.0000 Uiso H231 2.8563 -0.2797 -0.1207 0.0606 1.0000 Uiso H241 3.0311 -0.3869 -0.0696 0.0603 1.0000 Uiso H251 3.0613 -0.4045 0.0502 0.0662 1.0000 Uiso H261 2.9097 -0.3120 0.1203 0.0545 1.0000 Uiso H321 2.3808 -0.4614 0.1622 0.0527 1.0000 Uiso H331 2.3195 -0.5910 0.1031 0.0632 1.0000 Uiso H341 2.2988 -0.5580 -0.0158 0.0574 1.0000 Uiso H351 2.3166 -0.3885 -0.0804 0.0517 1.0000 Uiso H361 2.3718 -0.2571 -0.0242 0.0465 1.0000 Uiso H421 2.3152 -0.0276 0.1267 0.0548 1.0000 Uiso H431 2.1234 0.0539 0.1733 0.0744 1.0000 Uiso H441 1.9585 -0.0453 0.2176 0.0750 1.0000 Uiso H451 1.9823 -0.2248 0.2156 0.0701 1.0000 Uiso H461 2.1732 -0.3090 0.1678 0.0539 1.0000 Uiso H521 2.2233 0.1421 0.2674 0.0678 1.0000 Uiso H531 2.3822 0.1111 0.1782 0.0726 1.0000 Uiso H541 2.5396 0.2225 0.1485 0.0711 1.0000 Uiso H551 2.5564 0.3519 0.2147 0.0738 1.0000 Uiso H561 2.4053 0.3777 0.3085 0.0630 1.0000 Uiso H621 2.3331 0.1887 0.4782 0.1114 1.0000 Uiso H631 2.4528 0.2625 0.5647 0.1359 1.0000 Uiso H641 2.4199 0.4390 0.5606 0.1167 1.0000 Uiso H651 2.3273 0.5569 0.4747 0.1031 1.0000 Uiso H661 2.2134 0.4951 0.3915 0.0761 1.0000 Uiso H721 1.9943 0.3072 0.5246 0.0643 1.0000 Uiso H731 1.9230 0.3053 0.6443 0.0798 1.0000 Uiso H741 1.7632 0.2024 0.6928 0.0728 1.0000 Uiso H751 1.6791 0.0976 0.6285 0.0799 1.0000 Uiso H761 1.7474 0.0982 0.5086 0.0661 1.0000 Uiso H821 1.9803 -0.0134 0.4032 0.0643 1.0000 Uiso H831 1.8519 -0.1389 0.3782 0.0808 1.0000 Uiso H841 1.6449 -0.0847 0.3440 0.0798 1.0000 Uiso H851 1.5587 0.0896 0.3315 0.0826 1.0000 Uiso H861 1.6810 0.2174 0.3600 0.0688 1.0000 Uiso 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 As1 0.0379(3) 0.0307(3) 0.0335(3) -0.0039(2) 0.0008(2) -0.0141(2) As2 0.0381(3) 0.0281(3) 0.0348(3) -0.0021(2) -0.0033(2) -0.0129(2) As3 0.0513(4) 0.0438(3) 0.0430(3) -0.0048(3) -0.0016(3) -0.0155(3) As4 0.0499(4) 0.0373(3) 0.0350(3) -0.0007(2) -0.0026(2) -0.0126(3) Cr1 0.0390(5) 0.0317(4) 0.0296(4) -0.0021(3) -0.0015(3) -0.0115(3) Cr2 0.0560(6) 0.0363(5) 0.0345(5) -0.0011(4) -0.0026(4) -0.0129(4) S1 0.0469(8) 0.0418(7) 0.0429(8) 0.0091(6) -0.0069(6) -0.0186(6) S2 0.056(1) 0.0467(9) 0.0683(11) 0.0086(8) -0.0052(8) -0.0089(7) O1 0.063(3) 0.095(4) 0.069(3) -0.014(3) -0.023(3) -0.013(3) O2 0.071(3) 0.054(3) 0.070(3) -0.030(2) 0.013(2) -0.011(2) O3 0.105(4) 0.047(3) 0.065(3) -0.020(2) -0.002(3) -0.000(3) O4 0.086(4) 0.068(3) 0.082(4) 0.013(3) 0.022(3) -0.024(3) O5 0.081(4) 0.082(4) 0.100(5) 0.010(3) -0.019(3) 0.003(3) O6 0.109(5) 0.080(4) 0.091(4) -0.047(3) -0.002(3) -0.013(3) O7 0.134(5) 0.133(5) 0.056(3) -0.046(4) 0.014(3) -0.060(4) O8 0.145(6) 0.086(4) 0.096(5) 0.037(4) 0.002(4) -0.042(4) C1 0.045(3) 0.056(4) 0.045(4) -0.009(3) -0.008(3) -0.012(3) C2 0.044(3) 0.050(3) 0.038(3) -0.005(3) -0.001(2) -0.016(3) C3 0.059(4) 0.046(3) 0.033(3) 0.001(3) -0.006(3) -0.013(3) C4 0.052(4) 0.043(3) 0.048(4) 0.004(3) 0.009(3) -0.018(3) C5 0.054(4) 0.061(4) 0.054(4) 0.003(3) -0.011(3) -0.005(3) C6 0.072(5) 0.050(4) 0.053(4) -0.006(3) -0.002(3) -0.012(3) C7 0.075(5) 0.065(4) 0.033(3) -0.005(3) 0.007(3) -0.028(3) C8 0.074(5) 0.056(4) 0.069(5) 0.007(4) -0.006(4) -0.017(4) C11 0.040(3) 0.031(3) 0.046(3) -0.004(2) -0.003(2) -0.016(2) C12 0.074(4) 0.049(3) 0.047(4) -0.006(3) 0.005(3) -0.030(3) C13 0.072(5) 0.055(4) 0.072(5) 0.006(3) 0.004(4) -0.039(4) C14 0.057(4) 0.036(3) 0.094(6) -0.009(3) -0.019(4) -0.013(3) C15 0.056(4) 0.047(4) 0.084(5) -0.026(3) -0.006(3) -0.012(3) C16 0.049(3) 0.042(3) 0.062(4) -0.017(3) 0.004(3) -0.015(3) C21 0.044(3) 0.030(3) 0.045(3) -0.007(2) 0.005(2) -0.020(2) C22 0.064(4) 0.056(4) 0.042(4) -0.008(3) 0.003(3) -0.017(3) C23 0.092(6) 0.064(4) 0.043(4) -0.017(3) 0.018(4) -0.030(4) C24 0.068(5) 0.057(4) 0.079(5) -0.026(4) 0.028(4) -0.021(4) C25 0.057(4) 0.061(4) 0.085(6) -0.015(4) 0.010(4) -0.006(3) C26 0.049(4) 0.058(4) 0.051(4) -0.013(3) 0.002(3) -0.003(3) C31 0.037(3) 0.031(3) 0.049(3) -0.008(2) -0.010(2) -0.006(2) C32 0.073(4) 0.040(3) 0.056(4) -0.002(3) -0.020(3) -0.022(3) C33 0.085(5) 0.036(3) 0.084(6) -0.007(3) -0.026(4) -0.021(3) C34 0.060(4) 0.043(3) 0.077(5) -0.029(3) -0.005(3) -0.008(3) C35 0.060(4) 0.067(4) 0.050(4) -0.025(3) -0.001(3) -0.021(3) C36 0.054(4) 0.044(3) 0.045(3) -0.010(3) 0.001(3) -0.009(3) C41 0.037(3) 0.043(3) 0.040(3) -0.011(2) -0.004(2) -0.011(2) C42 0.057(4) 0.042(3) 0.068(4) -0.005(3) -0.011(3) -0.004(3) C43 0.074(5) 0.057(4) 0.087(6) -0.020(4) -0.012(4) 0.014(4) C44 0.055(5) 0.100(7) 0.079(6) -0.031(5) -0.016(4) 0.023(4) C45 0.054(4) 0.105(7) 0.072(5) -0.024(5) -0.002(4) -0.023(4) C46 0.042(3) 0.056(4) 0.066(4) -0.013(3) 0.005(3) -0.018(3) C51 0.051(4) 0.048(3) 0.049(4) -0.008(3) 0.000(3) -0.007(3) C52 0.078(5) 0.069(5) 0.064(5) -0.021(4) -0.001(4) -0.017(4) C53 0.099(6) 0.069(5) 0.060(5) -0.026(4) -0.008(4) 0.007(4) C54 0.068(5) 0.076(5) 0.064(5) 0.001(4) 0.009(4) 0.014(4) C55 0.068(5) 0.072(5) 0.075(5) 0.004(4) 0.012(4) -0.010(4) C56 0.066(4) 0.057(4) 0.068(5) -0.009(3) 0.011(4) -0.013(3) C61 0.061(4) 0.086(5) 0.046(4) -0.007(4) -0.005(3) -0.031(4) C62 0.14(1) 0.111(8) 0.12(1) 0.023(7) -0.073(8) -0.059(7) C63 0.213(16) 0.191(15) 0.10(1) 0.04(1) -0.09(1) -0.098(13) C64 0.147(11) 0.210(15) 0.070(7) -0.034(9) -0.007(7) -0.100(11) C65 0.099(7) 0.137(9) 0.107(8) -0.054(7) 0.010(6) -0.058(7) C66 0.079(5) 0.094(6) 0.082(6) -0.037(5) 0.002(4) -0.037(5) C71 0.062(4) 0.048(3) 0.034(3) -0.005(3) -0.002(3) -0.004(3) C72 0.100(6) 0.066(4) 0.042(4) -0.001(3) -0.006(4) -0.025(4) C73 0.128(8) 0.082(6) 0.048(5) -0.017(4) -0.014(5) -0.017(5) C74 0.101(6) 0.090(6) 0.043(4) -0.017(4) 0.011(4) -0.005(5) C75 0.084(6) 0.097(6) 0.059(5) -0.008(4) 0.018(4) -0.022(5) C76 0.075(5) 0.075(5) 0.053(4) -0.011(4) 0.005(3) -0.027(4) C81 0.057(4) 0.056(4) 0.035(3) -0.003(3) -0.001(3) -0.024(3) C82 0.075(5) 0.054(4) 0.081(5) -0.017(4) -0.015(4) -0.017(4) C83 0.109(7) 0.061(5) 0.109(7) -0.028(5) -0.019(6) -0.026(5) C84 0.126(8) 0.080(6) 0.070(6) -0.005(4) -0.036(5) -0.055(6) C85 0.084(6) 0.095(7) 0.099(7) 0.007(5) -0.048(5) -0.039(5) C86 0.071(5) 0.058(4) 0.090(6) -0.007(4) -0.026(4) -0.018(4) _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 As1 . Cr1 . 2.4629(9) yes As1 . S1 . 2.2647(15) yes As1 . C11 . 1.946(5) yes As1 . C21 . 1.945(5) yes As2 . Cr1 . 2.439(1) yes As2 . S1 . 2.2440(14) yes As2 . C31 . 1.934(5) yes As2 . C41 . 1.947(5) yes As3 . Cr2 . 2.4648(12) yes As3 . S2 . 2.2495(17) yes As3 . C51 . 1.938(6) yes As3 . C61 . 1.945(7) yes As4 . Cr2 . 2.448(1) yes As4 . S2 . 2.2512(19) yes As4 . C71 . 1.943(6) yes As4 . C81 . 1.941(6) yes Cr1 . C1 . 1.862(6) yes Cr1 . C2 . 1.893(6) yes Cr1 . C3 . 1.894(7) yes Cr1 . C4 . 1.855(5) yes Cr2 . C5 . 1.847(7) yes Cr2 . C6 . 1.902(7) yes Cr2 . C7 . 1.868(6) yes Cr2 . C8 . 1.841(7) yes O1 . C1 . 1.133(7) yes O2 . C2 . 1.138(7) yes O3 . C3 . 1.146(7) yes O4 . C4 . 1.143(7) yes O5 . C5 . 1.139(8) yes O6 . C6 . 1.145(8) yes O7 . C7 . 1.144(8) yes O8 . C8 . 1.157(8) yes C11 . C12 . 1.371(8) yes C11 . C16 . 1.384(8) yes C12 . C13 . 1.392(8) yes C12 . H121 . 1.025(6) no C13 . C14 . 1.37(1) yes C13 . H131 . 1.034(7) no C14 . C15 . 1.37(1) yes C14 . H141 . 1.015(6) no C15 . C16 . 1.373(8) yes C15 . H151 . 1.030(7) no C16 . H161 . 1.020(6) no C21 . C22 . 1.398(8) yes C21 . C26 . 1.374(9) yes C22 . C23 . 1.390(9) yes C22 . H221 . 1.018(7) no C23 . C24 . 1.371(11) yes C23 . H231 . 1.015(7) no C24 . C25 . 1.375(11) yes C24 . H241 . 1.012(7) no C25 . C26 . 1.38(1) yes C25 . H251 . 1.023(8) no C26 . H261 . 1.015(6) no C31 . C32 . 1.397(8) yes C31 . C36 . 1.373(8) yes C32 . C33 . 1.393(8) yes C32 . H321 . 1.032(6) no C33 . C34 . 1.35(1) yes C33 . H331 . 1.012(7) no C34 . C35 . 1.38(1) yes C34 . H341 . 1.008(6) no C35 . C36 . 1.376(8) yes C35 . H351 . 1.024(6) no C36 . H361 . 1.017(6) no C41 . C42 . 1.378(8) yes C41 . C46 . 1.364(8) yes C42 . C43 . 1.39(1) yes C42 . H421 . 1.018(7) no C43 . C44 . 1.379(12) yes C43 . H431 . 1.006(7) no C44 . C45 . 1.369(12) yes C44 . H441 . 1.017(7) no C45 . C46 . 1.39(1) yes C45 . H451 . 1.017(8) no C46 . H461 . 1.023(6) no C51 . C52 . 1.375(9) yes C51 . C56 . 1.375(9) yes C52 . C53 . 1.389(11) yes C52 . H521 . 1.022(8) no C53 . C54 . 1.375(12) yes C53 . H531 . 1.023(7) no C54 . C55 . 1.376(12) yes C54 . H541 . 1.018(8) no C55 . C56 . 1.39(1) yes C55 . H551 . 1.018(8) no C56 . H561 . 1.022(7) no C61 . C62 . 1.344(12) yes C61 . C66 . 1.404(11) yes C62 . C63 . 1.426(16) yes C62 . H621 . 1.054(11) no C63 . C64 . 1.35(2) yes C63 . H631 . 1.065(13) no C64 . C65 . 1.342(18) yes C64 . H641 . 0.992(11) no C65 . C66 . 1.393(12) yes C65 . H651 . 1.038(12) no C66 . H661 . 1.03(1) no C71 . C72 . 1.387(9) yes C71 . C76 . 1.375(9) yes C72 . C73 . 1.40(1) yes C72 . H721 . 1.022(7) no C73 . C74 . 1.378(12) yes C73 . H731 . 1.026(8) no C74 . C75 . 1.352(12) yes C74 . H741 . 1.013(7) no C75 . C76 . 1.40(1) yes C75 . H751 . 1.026(8) no C76 . H761 . 1.031(7) no C81 . C82 . 1.39(1) yes C81 . C86 . 1.35(1) yes C82 . C83 . 1.40(1) yes C82 . H821 . 1.031(8) no C83 . C84 . 1.355(13) yes C83 . H831 . 1.035(9) no C84 . C85 . 1.347(13) yes C84 . H841 . 1.013(7) no C85 . C86 . 1.39(1) yes C85 . H851 . 1.032(8) no C86 . H861 . 1.029(8) 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 Cr1 . As1 . S1 . 98.98(4) yes Cr1 . As1 . C11 . 126.71(16) yes S1 . As1 . C11 . 103.13(16) yes Cr1 . As1 . C21 . 119.67(15) yes S1 . As1 . C21 . 103.37(17) yes C11 . As1 . C21 . 101.4(2) yes Cr1 . As2 . S1 . 100.28(4) yes Cr1 . As2 . C31 . 123.92(16) yes S1 . As2 . C31 . 104.33(17) yes Cr1 . As2 . C41 . 119.13(16) yes S1 . As2 . C41 . 103.45(17) yes C31 . As2 . C41 . 102.9(2) yes Cr2 . As3 . S2 . 98.66(5) yes Cr2 . As3 . C51 . 122.79(19) yes S2 . As3 . C51 . 103.27(19) yes Cr2 . As3 . C61 . 123.9(2) yes S2 . As3 . C61 . 102.5(2) yes C51 . As3 . C61 . 101.8(3) yes Cr2 . As4 . S2 . 99.12(5) yes Cr2 . As4 . C71 . 125.23(18) yes S2 . As4 . C71 . 103.42(19) yes Cr2 . As4 . C81 . 120.95(18) yes S2 . As4 . C81 . 103.8(2) yes C71 . As4 . C81 . 101.0(2) yes As1 . Cr1 . As2 . 75.49(3) yes As1 . Cr1 . C1 . 98.53(19) yes As2 . Cr1 . C1 . 173.23(19) yes As1 . Cr1 . C2 . 93.04(17) yes As2 . Cr1 . C2 . 88.01(18) yes C1 . Cr1 . C2 . 89.2(3) yes As1 . Cr1 . C3 . 90.19(17) yes As2 . Cr1 . C3 . 93.68(18) yes C1 . Cr1 . C3 . 89.5(3) yes C2 . Cr1 . C3 . 176.6(2) yes As1 . Cr1 . C4 . 169.0(2) yes As2 . Cr1 . C4 . 93.6(2) yes C1 . Cr1 . C4 . 92.4(3) yes C2 . Cr1 . C4 . 88.1(3) yes C3 . Cr1 . C4 . 88.9(3) yes As3 . Cr2 . As4 . 75.67(3) yes As3 . Cr2 . C5 . 168.7(2) yes As4 . Cr2 . C5 . 93.2(2) yes As3 . Cr2 . C6 . 92.6(2) yes As4 . Cr2 . C6 . 98.5(2) yes C5 . Cr2 . C6 . 86.9(3) yes As3 . Cr2 . C7 . 92.0(2) yes As4 . Cr2 . C7 . 86.60(19) yes C5 . Cr2 . C7 . 89.4(3) yes C6 . Cr2 . C7 . 173.8(3) yes As3 . Cr2 . C8 . 97.3(2) yes As4 . Cr2 . C8 . 170.5(3) yes C5 . Cr2 . C8 . 94.0(3) yes C6 . Cr2 . C8 . 88.1(3) yes C7 . Cr2 . C8 . 87.3(3) yes As1 . S1 . As2 . 83.44(5) yes As3 . S2 . As4 . 84.06(6) yes Cr1 . C1 . O1 . 178.3(6) yes Cr1 . C2 . O2 . 176.5(5) yes Cr1 . C3 . O3 . 176.9(5) yes Cr1 . C4 . O4 . 178.8(6) yes Cr2 . C5 . O5 . 178.3(6) yes Cr2 . C6 . O6 . 174.3(7) yes Cr2 . C7 . O7 . 176.4(7) yes Cr2 . C8 . O8 . 177.9(8) yes As1 . C11 . C12 . 122.0(4) yes As1 . C11 . C16 . 118.9(4) yes C12 . C11 . C16 . 119.1(5) yes C11 . C12 . C13 . 120.2(6) yes C11 . C12 . H121 . 119.5(5) no C13 . C12 . H121 . 120.3(6) no C12 . C13 . C14 . 119.9(6) yes C12 . C13 . H131 . 121.0(7) no C14 . C13 . H131 . 119.1(6) no C13 . C14 . C15 . 120.0(6) yes C13 . C14 . H141 . 121.5(7) no C15 . C14 . H141 . 118.5(7) no C14 . C15 . C16 . 120.1(6) yes C14 . C15 . H151 . 120.0(6) no C16 . C15 . H151 . 120.0(7) no C11 . C16 . C15 . 120.6(6) yes C11 . C16 . H161 . 119.2(5) no C15 . C16 . H161 . 120.2(6) no As1 . C21 . C22 . 122.7(5) yes As1 . C21 . C26 . 117.2(4) yes C22 . C21 . C26 . 120.1(6) yes C21 . C22 . C23 . 119.0(7) yes C21 . C22 . H221 . 119.7(6) no C23 . C22 . H221 . 121.3(6) no C22 . C23 . C24 . 120.0(7) yes C22 . C23 . H231 . 120.0(8) no C24 . C23 . H231 . 120.0(7) no C23 . C24 . C25 . 120.9(7) yes C23 . C24 . H241 . 119.0(8) no C25 . C24 . H241 . 120.0(8) no C24 . C25 . C26 . 119.5(7) yes C24 . C25 . H251 . 119.6(7) no C26 . C25 . H251 . 120.9(8) no C21 . C26 . C25 . 120.4(6) yes C21 . C26 . H261 . 119.3(6) no C25 . C26 . H261 . 120.3(7) no As2 . C31 . C32 . 117.3(4) yes As2 . C31 . C36 . 123.0(4) yes C32 . C31 . C36 . 119.8(5) yes C31 . C32 . C33 . 118.7(6) yes C31 . C32 . H321 . 120.2(5) no C33 . C32 . H321 . 121.1(6) no C32 . C33 . C34 . 121.4(6) yes C32 . C33 . H331 . 120.2(7) no C34 . C33 . H331 . 118.4(6) no C33 . C34 . C35 . 119.4(5) yes C33 . C34 . H341 . 120.0(7) no C35 . C34 . H341 . 120.5(7) no C34 . C35 . C36 . 120.6(6) yes C34 . C35 . H351 . 119.8(6) no C36 . C35 . H351 . 119.6(6) no C31 . C36 . C35 . 120.2(6) yes C31 . C36 . H361 . 119.5(5) no C35 . C36 . H361 . 120.4(6) no As2 . C41 . C42 . 119.9(4) yes As2 . C41 . C46 . 118.9(4) yes C42 . C41 . C46 . 120.8(6) yes C41 . C42 . C43 . 120.0(6) yes C41 . C42 . H421 . 120.4(6) no C43 . C42 . H421 . 119.7(6) no C42 . C43 . C44 . 119.4(7) yes C42 . C43 . H431 . 120.7(8) no C44 . C43 . H431 . 119.9(8) no C43 . C44 . C45 . 120.3(7) yes C43 . C44 . H441 . 119.6(9) no C45 . C44 . H441 . 120.1(9) no C44 . C45 . C46 . 120.4(7) yes C44 . C45 . H451 . 118.9(8) no C46 . C45 . H451 . 120.7(8) no C41 . C46 . C45 . 119.1(6) yes C41 . C46 . H461 . 121.2(6) no C45 . C46 . H461 . 119.6(6) no As3 . C51 . C52 . 120.9(5) yes As3 . C51 . C56 . 119.7(5) yes C52 . C51 . C56 . 119.2(6) yes C51 . C52 . C53 . 120.3(7) yes C51 . C52 . H521 . 120.0(7) no C53 . C52 . H521 . 119.6(7) no C52 . C53 . C54 . 120.3(7) yes C52 . C53 . H531 . 121.0(9) no C54 . C53 . H531 . 118.7(8) no C53 . C54 . C55 . 119.5(7) yes C53 . C54 . H541 . 120.2(9) no C55 . C54 . H541 . 120.3(9) no C54 . C55 . C56 . 120.0(7) yes C54 . C55 . H551 . 118.6(8) no C56 . C55 . H551 . 121.4(8) no C51 . C56 . C55 . 120.7(7) yes C51 . C56 . H561 . 119.6(7) no C55 . C56 . H561 . 119.7(7) no As3 . C61 . C62 . 122.0(7) yes As3 . C61 . C66 . 117.2(6) yes C62 . C61 . C66 . 120.8(7) yes C61 . C62 . C63 . 118.5(11) yes C61 . C62 . H621 . 120.8(9) no C63 . C62 . H621 . 120.7(11) no C62 . C63 . C64 . 119.5(12) yes C62 . C63 . H631 . 127.7(17) no C64 . C63 . H631 . 112.5(13) no C63 . C64 . C65 . 122.8(10) yes C63 . C64 . H641 . 123.0(17) no C65 . C64 . H641 . 113.9(17) no C64 . C65 . C66 . 118.7(11) yes C64 . C65 . H651 . 120.8(12) no C66 . C65 . H651 . 120.5(13) no C61 . C66 . C65 . 119.6(10) yes C61 . C66 . H661 . 119.7(7) no C65 . C66 . H661 . 120.7(9) no As4 . C71 . C72 . 118.1(5) yes As4 . C71 . C76 . 121.6(5) yes C72 . C71 . C76 . 120.4(6) yes C71 . C72 . C73 . 119.3(7) yes C71 . C72 . H721 . 120.1(7) no C73 . C72 . H721 . 120.6(7) no C72 . C73 . C74 . 119.8(7) yes C72 . C73 . H731 . 120.4(9) no C74 . C73 . H731 . 119.7(8) no C73 . C74 . C75 . 120.5(7) yes C73 . C74 . H741 . 119.7(8) no C75 . C74 . H741 . 119.8(9) no C74 . C75 . C76 . 120.8(7) yes C74 . C75 . H751 . 119.3(8) no C76 . C75 . H751 . 119.9(8) no C71 . C76 . C75 . 119.2(7) yes C71 . C76 . H761 . 120.2(6) no C75 . C76 . H761 . 120.7(7) no As4 . C81 . C82 . 121.5(5) yes As4 . C81 . C86 . 118.7(5) yes C82 . C81 . C86 . 119.7(6) yes C81 . C82 . C83 . 118.5(7) yes C81 . C82 . H821 . 120.7(6) no C83 . C82 . H821 . 120.8(7) no C82 . C83 . C84 . 121.1(8) yes C82 . C83 . H831 . 120.2(9) no C84 . C83 . H831 . 118.7(8) no C83 . C84 . C85 . 119.7(7) yes C83 . C84 . H841 . 120.1(10) no C85 . C84 . H841 . 120.2(10) no C84 . C85 . C86 . 120.8(8) yes C84 . C85 . H851 . 118.5(8) no C86 . C85 . H851 . 120.7(9) no C81 . C86 . C85 . 120.2(7) yes C81 . C86 . H861 . 118.6(6) no C85 . C86 . H861 . 121.2(7) no #END data_5 _audit_creation_date 99-06-21 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd62 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' malcolm.green@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category FA _publ_requested_coeditor_name 'Graham McCann ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Group 6 Transition Metal Carbonyl Complexes with Chalcogen-bridged Diarsenic(III) Ligands' # Title of paper ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software, Xpress, MAC Science, 1989' _computing_data_reduction ; DIP2000 software 'DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; DIP2000 software 'DENZO Otwinowski & Minor, 1996' ; # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # 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 #**************************************************************************** _cell_length_a 10.456(2) _cell_angle_alpha 90. _cell_length_b 26.817(5) _cell_angle_beta 96.14(3) _cell_length_c 17.543(4) _cell_angle_gamma 90. _cell_volume 4890.7(5) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' 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 ' 0.0020 0.0020 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 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 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 ' 0.1100 0.1240 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' 'As ' -0.0300 2.0070 16.6723 2.6345 6.0701 0.2647 3.4313 12.9479 4.2779 47.7972 2.5310 'International_Tables_Vol_IV_Table_2.2B' 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C26 H20 As2 Mo0.50 O2 S1 ' _chemical_formula_moiety ' C26 H20 As2 Mo0.50 O2 S1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 594.32 _cell_measurement_reflns_used 12945 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' irregular block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2353.28 _exptl_absorpt_coefficient_mu 3.07 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 0.541 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 4703 _reflns_number_total 4703 _diffrn_reflns_av_R_equivalents 0.06 # Number of reflections with Friedels Law is 4703 # Number of reflections without Friedels Law is 0 _reflns_number_gt 3835 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _reflns_threshold_expression >3.00\s(I) _refine_diff_density_min -0.65 _refine_diff_density_max 0.62 _refine_ls_number_reflns 3835 _refine_ls_number_parameters 285 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0373 _refine_ls_goodness_of_fit_ref 1.0636 _refine_ls_shift/su_max 0.001350 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 0.439 0.267 0.283 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Mo1 1.0000 0.227452(14) 0.7500 0.0272 1.0000 Uani As1 0.94616(3) 0.159978(12) 0.643093(19) 0.0247 1.0000 Uani As2 1.06436(3) 0.050860(13) 0.550056(18) 0.0256 1.0000 Uani S1 1.10348(8) 0.10265(3) 0.65358(4) 0.0270 1.0000 Uani O1 1.0722(3) 0.31322(14) 0.8697(3) 0.0909 1.0000 Uani O2 0.7086(3) 0.22941(12) 0.79077(18) 0.0485 1.0000 Uani C1 1.0454(4) 0.28092(15) 0.8276(3) 0.0552 1.0000 Uani C2 0.8130(4) 0.22784(13) 0.7762(2) 0.0333 1.0000 Uani C11 0.7826(3) 0.12398(14) 0.64076(19) 0.0306 1.0000 Uani C12 0.7718(4) 0.07280(14) 0.6541(2) 0.0349 1.0000 Uani C13 0.6526(4) 0.05080(17) 0.6586(2) 0.0456 1.0000 Uani C14 0.5430(4) 0.0806(2) 0.6503(2) 0.0513 1.0000 Uani C15 0.5515(4) 0.1320(2) 0.6372(3) 0.0534 1.0000 Uani C16 0.6717(4) 0.15342(16) 0.6317(2) 0.0427 1.0000 Uani C21 0.9479(3) 0.18188(15) 0.5364(2) 0.0348 1.0000 Uani C22 1.0416(4) 0.21650(19) 0.5204(3) 0.0525 1.0000 Uani C23 1.0522(5) 0.2315(2) 0.4458(3) 0.0652 1.0000 Uani C24 0.9693(5) 0.2134(2) 0.3869(3) 0.0600 1.0000 Uani C25 0.8742(5) 0.1788(2) 0.4013(2) 0.0606 1.0000 Uani C26 0.8631(4) 0.16266(18) 0.4769(2) 0.0464 1.0000 Uani C31 1.2104(3) 0.00647(13) 0.5860(2) 0.0289 1.0000 Uani C32 1.2255(4) -0.01132(14) 0.6609(2) 0.0360 1.0000 Uani C33 1.3241(4) -0.04529(15) 0.6843(2) 0.0426 1.0000 Uani C34 1.4065(4) -0.06176(15) 0.6325(3) 0.0450 1.0000 Uani C35 1.3912(4) -0.04451(16) 0.5572(3) 0.0462 1.0000 Uani C36 1.2935(4) -0.01061(16) 0.5337(2) 0.0397 1.0000 Uani C41 1.1493(3) 0.08698(13) 0.4712(2) 0.0313 1.0000 Uani C42 1.2597(4) 0.11556(17) 0.4886(2) 0.0470 1.0000 Uani C43 1.3173(4) 0.13940(18) 0.4303(3) 0.0512 1.0000 Uani C44 1.2653(4) 0.13486(16) 0.3545(2) 0.0465 1.0000 Uani C45 1.1566(4) 0.10579(19) 0.3368(2) 0.0500 1.0000 Uani C46 1.0966(4) 0.08208(16) 0.3952(2) 0.0410 1.0000 Uani H121 0.8511 0.0516 0.6600 0.0336 1.0000 Uiso H131 0.6461 0.0135 0.6674 0.0423 1.0000 Uiso H141 0.4578 0.0649 0.6556 0.0480 1.0000 Uiso H151 0.4722 0.1527 0.6313 0.0478 1.0000 Uiso H161 0.6782 0.1898 0.6212 0.0385 1.0000 Uiso H221 1.1003 0.2308 0.5632 0.0488 1.0000 Uiso H231 1.1223 0.2555 0.4355 0.0623 1.0000 Uiso H241 0.9742 0.2246 0.3332 0.0564 1.0000 Uiso H251 0.8152 0.1652 0.3582 0.0528 1.0000 Uiso H261 0.7948 0.1375 0.4869 0.0439 1.0000 Uiso H321 1.1661 0.0003 0.6986 0.0330 1.0000 Uiso H331 1.3346 -0.0579 0.7381 0.0421 1.0000 Uiso H341 1.4760 -0.0858 0.6494 0.0402 1.0000 Uiso H351 1.4498 -0.0568 0.5201 0.0434 1.0000 Uiso H361 1.2825 0.0021 0.4795 0.0376 1.0000 Uiso H421 1.2994 0.1188 0.5431 0.0461 1.0000 Uiso H431 1.3949 0.1607 0.4431 0.0504 1.0000 Uiso H441 1.3067 0.1519 0.3128 0.0449 1.0000 Uiso H451 1.1198 0.1015 0.2824 0.0451 1.0000 Uiso H461 1.0174 0.0623 0.3827 0.0374 1.0000 Uiso 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 Mo1 0.0241(2) 0.01445(18) 0.0453(2) 0.0000 0.01424(17) 0.0000 As1 0.02301(17) 0.02568(17) 0.02598(17) 0.00465(13) 0.00552(13) 0.00424(1 As2 0.02197(17) 0.03056(18) 0.02411(17) -0.00397(13) 0.00160(13) 0.00011(1 S1 0.0283(4) 0.0280(4) 0.0242(4) -0.0031(3) -0.0002(3) 0.0077(3) O1 0.054(2) 0.059(2) 0.166(4) -0.072(3) 0.038(3) -0.0194(17 O2 0.0304(15) 0.0596(19) 0.0577(18) -0.0109(14) 0.0153(13) 0.0009(13 C1 0.031(2) 0.034(2) 0.105(4) -0.025(2) 0.028(2) -0.0055(16 C2 0.031(2) 0.0255(17) 0.045(2) -0.0063(15) 0.0103(16) -0.0021(13 C11 0.0287(17) 0.0371(18) 0.0262(16) 0.0001(14) 0.0042(13) 0.0005(14 C12 0.0373(19) 0.0377(19) 0.0299(17) 0.0021(15) 0.0042(15) -0.0052(15 C13 0.051(3) 0.054(3) 0.0310(19) 0.0050(17) 0.0020(17) -0.010(2) C14 0.035(2) 0.076(3) 0.043(2) -0.008(2) 0.0049(18) -0.018(2) C15 0.026(2) 0.075(3) 0.058(3) -0.021(2) 0.0028(19) 0.0013(19 C16 0.0290(19) 0.047(2) 0.051(2) -0.0128(18) -0.0002(17) 0.0038(16 C21 0.0303(18) 0.045(2) 0.0294(17) 0.0171(15) 0.0070(15) 0.0137(15 C22 0.043(2) 0.067(3) 0.049(2) 0.029(2) 0.012(2) 0.006(2) C23 0.064(3) 0.087(4) 0.048(3) 0.037(3) 0.019(2) 0.018(3) C24 0.050(3) 0.092(4) 0.041(2) 0.031(2) 0.018(2) 0.037(3) C25 0.054(3) 0.094(4) 0.033(2) 0.008(2) 0.003(2) 0.031(3) C26 0.040(2) 0.065(3) 0.034(2) 0.0062(19) 0.0045(17) 0.0160(19 C31 0.0270(17) 0.0280(17) 0.0315(17) -0.0034(13) 0.0021(14) -0.0002(13 C32 0.038(2) 0.0345(19) 0.0365(19) -0.0015(15) 0.0071(16) 0.0025(15 C33 0.048(2) 0.036(2) 0.042(2) 0.0028(16) -0.0049(18) 0.0053(16 C34 0.036(2) 0.037(2) 0.061(3) -0.0063(18) -0.0026(19) 0.0094(16 C35 0.041(2) 0.044(2) 0.054(2) -0.0127(19) 0.0050(19) 0.0174(18 C36 0.034(2) 0.049(2) 0.0359(19) -0.0062(17) 0.0040(16) 0.0077(17 C41 0.0278(17) 0.0352(18) 0.0321(17) -0.0026(14) 0.0090(14) 0.0031(14 C42 0.043(2) 0.062(3) 0.037(2) -0.0064(19) 0.0086(18) -0.017(2) C43 0.048(3) 0.057(3) 0.051(3) -0.008(2) 0.018(2) -0.014(2) C44 0.051(3) 0.046(2) 0.046(2) 0.0053(18) 0.022(2) 0.0024(19 C45 0.045(2) 0.077(3) 0.0281(19) 0.0093(19) 0.0059(17) 0.010(2) C46 0.035(2) 0.056(2) 0.0312(19) 0.0015(17) 0.0009(16) -0.0026(17 _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 Mo1 . As1 . 2.6234(4) yes Mo1 . As1 5_756 2.6234(4) yes Mo1 . C1 . 1.999(4) yes Mo1 . C1 5_756 1.999(4) yes Mo1 . C2 . 2.056(4) yes Mo1 . C2 5_756 2.056(4) yes As1 . S1 . 2.2446(8) yes As1 . C11 . 1.961(4) yes As1 . C21 . 1.963(3) yes As2 . S1 . 2.2882(8) yes As2 . C31 . 1.985(3) yes As2 . C41 . 1.975(4) yes O1 . C1 . 1.153(5) yes O2 . C2 . 1.149(4) yes C11 . C12 . 1.399(5) yes C11 . C16 . 1.398(5) yes C12 . C13 . 1.389(6) yes C12 . H121 . 1.001(4) no C13 . C14 . 1.392(7) yes C13 . H131 . 1.015(4) no C14 . C15 . 1.402(7) yes C14 . H141 . 0.999(4) no C15 . C16 . 1.394(6) yes C15 . H151 . 0.993(4) no C16 . H161 . 0.996(4) no C21 . C22 . 1.400(6) yes C21 . C26 . 1.394(6) yes C22 . C23 . 1.384(6) yes C22 . H221 . 0.995(5) no C23 . C24 . 1.366(8) yes C23 . H231 . 1.005(6) no C24 . C25 . 1.402(8) yes C24 . H241 . 0.996(4) no C25 . C26 . 1.412(6) yes C25 . H251 . 0.992(5) no C26 . H261 . 1.011(5) no C31 . C32 . 1.391(5) yes C31 . C36 . 1.406(5) yes C32 . C33 . 1.404(5) yes C32 . H321 . 1.004(4) no C33 . C34 . 1.389(6) yes C33 . H331 . 0.998(4) no C34 . C35 . 1.392(6) yes C34 . H341 . 0.993(4) no C35 . C36 . 1.396(5) yes C35 . H351 . 0.997(4) no C36 . H361 . 1.006(4) no C41 . C42 . 1.391(5) yes C41 . C46 . 1.394(5) yes C42 . C43 . 1.396(6) yes C42 . H421 . 1.005(4) no C43 . C44 . 1.388(6) yes C43 . H431 . 0.997(4) no C44 . C45 . 1.386(7) yes C44 . H441 . 1.000(4) no C45 . C46 . 1.409(6) yes C45 . H451 . 0.997(4) no C46 . H461 . 0.989(4) 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 As1 . Mo1 . As1 5_756 92.786(18) yes As1 . Mo1 . C1 . 177.07(15) yes As1 5_756 Mo1 . C1 . 89.48(16) yes As1 . Mo1 . C1 5_756 89.48(16) yes As1 5_756 Mo1 . C1 5_756 177.07(15) yes C1 . Mo1 . C1 5_756 88.3(3) yes As1 . Mo1 . C2 . 91.6(1) yes As1 5_756 Mo1 . C2 . 88.85(11) yes C1 . Mo1 . C2 . 90.36(15) yes C1 5_756 Mo1 . C2 . 89.23(15) yes As1 . Mo1 . C2 5_756 88.85(11) yes As1 5_756 Mo1 . C2 5_756 91.6(1) yes C1 . Mo1 . C2 5_756 89.23(15) yes C1 5_756 Mo1 . C2 5_756 90.36(15) yes C2 . Mo1 . C2 5_756 179.42(19) yes Mo1 . As1 . S1 . 108.33(2) yes Mo1 . As1 . C11 . 118.3(1) yes S1 . As1 . C11 . 107.13(11) yes Mo1 . As1 . C21 . 116.87(12) yes S1 . As1 . C21 . 101.6(1) yes C11 . As1 . C21 . 102.97(15) yes S1 . As2 . C31 . 92.6(1) yes S1 . As2 . C41 . 101.68(11) yes C31 . As2 . C41 . 97.36(14) yes As1 . S1 . As2 . 106.47(3) yes Mo1 . C1 . O1 . 176.9(5) yes Mo1 . C2 . O2 . 178.2(3) yes As1 . C11 . C12 . 124.4(3) yes As1 . C11 . C16 . 115.8(3) yes C12 . C11 . C16 . 119.5(3) yes C11 . C12 . C13 . 121.0(4) yes C11 . C12 . H121 . 119.6(3) no C13 . C12 . H121 . 119.4(4) no C12 . C13 . C14 . 118.9(4) yes C12 . C13 . H131 . 120.2(4) no C14 . C13 . H131 . 120.9(4) no C13 . C14 . C15 . 121.1(4) yes C13 . C14 . H141 . 118.6(5) no C15 . C14 . H141 . 120.3(5) no C14 . C15 . C16 . 119.3(4) yes C14 . C15 . H151 . 119.9(4) no C16 . C15 . H151 . 120.8(5) no C11 . C16 . C15 . 120.2(4) yes C11 . C16 . H161 . 120.1(4) no C15 . C16 . H161 . 119.7(4) no As1 . C21 . C22 . 117.9(3) yes As1 . C21 . C26 . 122.2(3) yes C22 . C21 . C26 . 119.8(4) yes C21 . C22 . C23 . 120.8(5) yes C21 . C22 . H221 . 119.5(4) no C23 . C22 . H221 . 119.7(5) no C22 . C23 . C24 . 120.2(5) yes C22 . C23 . H231 . 119.4(6) no C24 . C23 . H231 . 120.4(4) no C23 . C24 . C25 . 120.3(4) yes C23 . C24 . H241 . 121.0(6) no C25 . C24 . H241 . 118.6(5) no C24 . C25 . C26 . 120.2(5) yes C24 . C25 . H251 . 120.0(5) no C26 . C25 . H251 . 119.8(6) no C21 . C26 . C25 . 118.7(4) yes C21 . C26 . H261 . 121.4(4) no C25 . C26 . H261 . 119.9(4) no As2 . C31 . C32 . 120.8(3) yes As2 . C31 . C36 . 119.8(3) yes C32 . C31 . C36 . 119.3(3) yes C31 . C32 . C33 . 120.3(3) yes C31 . C32 . H321 . 120.0(4) no C33 . C32 . H321 . 119.7(4) no C32 . C33 . C34 . 120.2(4) yes C32 . C33 . H331 . 120.0(4) no C34 . C33 . H331 . 119.9(4) no C33 . C34 . C35 . 119.9(4) yes C33 . C34 . H341 . 119.8(4) no C35 . C34 . H341 . 120.3(4) no C34 . C35 . C36 . 120.2(4) yes C34 . C35 . H351 . 119.5(4) no C36 . C35 . H351 . 120.4(4) no C31 . C36 . C35 . 120.2(4) yes C31 . C36 . H361 . 119.4(4) no C35 . C36 . H361 . 120.3(4) no As2 . C41 . C42 . 122.8(3) yes As2 . C41 . C46 . 117.5(3) yes C42 . C41 . C46 . 119.7(3) yes C41 . C42 . C43 . 120.4(4) yes C41 . C42 . H421 . 120.3(4) no C43 . C42 . H421 . 119.4(4) no C42 . C43 . C44 . 120.4(4) yes C42 . C43 . H431 . 120.2(4) no C44 . C43 . H431 . 119.4(4) no C43 . C44 . C45 . 119.5(4) yes C43 . C44 . H441 . 120.4(4) no C45 . C44 . H441 . 120.1(4) no C44 . C45 . C46 . 120.6(4) yes C44 . C45 . H451 . 120.2(4) no C46 . C45 . H451 . 119.2(5) no C41 . C46 . C45 . 119.5(4) yes C41 . C46 . H461 . 119.9(4) no C45 . C46 . H461 . 120.6(4) no #END