# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1755 data_sy110 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 As2 Co2 O5' _chemical_formula_weight 806.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.766(7) _cell_length_b 9.446(2) _cell_length_c 21.693(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.02(4) _cell_angle_gamma 90.00 _cell_volume 3420.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 2.930 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.7043 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.6 _diffrn_reflns_number 12436 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6022 _reflns_number_gt 3371 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6022 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.231 _refine_ls_shift/su_mean 0.014 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.36765(3) 0.38450(6) 0.14522(3) 0.04881(18) Uani 1 1 d . . . As2 As 0.53712(3) 0.51086(6) 0.17702(3) 0.04554(17) Uani 1 1 d . . . Co1 Co 0.39175(5) 0.45065(9) 0.25240(4) 0.0570(2) Uani 1 1 d . . . Co2 Co 0.51688(4) 0.58788(9) 0.27116(4) 0.0504(2) Uani 1 1 d . . . O1 O 0.4522(2) 0.4238(4) 0.11990(16) 0.0514(10) Uani 1 1 d . . . O3 O 0.2346(3) 0.4313(8) 0.2654(3) 0.166(3) Uani 1 1 d . . . O4 O 0.5854(3) 0.8716(6) 0.2846(3) 0.1077(19) Uani 1 1 d . . . O5 O 0.4681(4) 0.2011(6) 0.3284(3) 0.139(2) Uani 1 1 d . . . O6 O 0.6326(3) 0.4482(7) 0.3846(2) 0.121(2) Uani 1 1 d . . . C1 C 0.4056(3) 0.6518(6) 0.2391(3) 0.0568(16) Uani 1 1 d . . . H1 H 0.3747 0.7265 0.2100 0.068 Uiso 1 1 calc R . . C2 C 0.4271(3) 0.6203(6) 0.3031(3) 0.0530(16) Uani 1 1 d . . . C3 C 0.2956(4) 0.4376(9) 0.2585(3) 0.098(3) Uani 1 1 d . . . C4 C 0.5611(4) 0.7584(8) 0.2791(3) 0.071(2) Uani 1 1 d . . . C5 C 0.4371(5) 0.2982(8) 0.2980(3) 0.086(2) Uani 1 1 d . . . C6 C 0.5878(4) 0.5002(8) 0.3390(3) 0.0737(19) Uani 1 1 d . . . C22 C 0.4329(4) 0.8246(8) 0.3761(3) 0.076(2) Uani 1 1 d . . . H22 H 0.4334 0.8856 0.3426 0.091 Uiso 1 1 calc R . . C23 C 0.4366(4) 0.8783(10) 0.4367(4) 0.104(3) Uani 1 1 d . . . H23 H 0.4401 0.9756 0.4435 0.125 Uiso 1 1 calc R . . C24 C 0.4352(4) 0.7906(13) 0.4869(4) 0.108(4) Uani 1 1 d . . . H24 H 0.4379 0.8279 0.5273 0.130 Uiso 1 1 calc R . . C25 C 0.4300(4) 0.6477(11) 0.4764(4) 0.096(3) Uani 1 1 d . . . H25 H 0.4283 0.5878 0.5100 0.116 Uiso 1 1 calc R . . C26 C 0.4271(3) 0.5902(8) 0.4169(3) 0.075(2) Uani 1 1 d . . . H26 H 0.4244 0.4926 0.4110 0.090 Uiso 1 1 calc R . . C21 C 0.4282(3) 0.6791(7) 0.3658(3) 0.0576(17) Uani 1 1 d . . . C32 C 0.2362(3) 0.5784(5) 0.0880(2) 0.0708(19) Uani 1 1 d G . . H32 H 0.2429 0.5994 0.1315 0.085 Uiso 1 1 calc R . . C33 C 0.1775(2) 0.6475(4) 0.0375(3) 0.091(3) Uani 1 1 d G . . H33 H 0.1449 0.7147 0.0471 0.109 Uiso 1 1 calc R . . C34 C 0.1676(2) 0.6162(5) -0.0274(3) 0.105(3) Uani 1 1 d G . . H34 H 0.1283 0.6624 -0.0612 0.126 Uiso 1 1 calc R . . C35 C 0.2163(3) 0.5158(6) -0.04182(17) 0.100(3) Uani 1 1 d G . . H35 H 0.2097 0.4948 -0.0853 0.120 Uiso 1 1 calc R . . C36 C 0.2750(2) 0.4467(4) 0.0087(2) 0.075(2) Uani 1 1 d G . . H36 H 0.3076 0.3795 -0.0009 0.090 Uiso 1 1 calc R . . C31 C 0.2850(2) 0.4780(4) 0.0736(2) 0.0552(16) Uani 1 1 d G . . C42 C 0.5037(2) 0.6585(4) 0.05209(19) 0.0583(16) Uani 1 1 d G . . H42 H 0.4587 0.6007 0.0370 0.070 Uiso 1 1 calc R . . C43 C 0.5182(3) 0.7589(5) 0.01064(14) 0.082(2) Uani 1 1 d G . . H43 H 0.4829 0.7682 -0.0322 0.098 Uiso 1 1 calc R . . C44 C 0.5854(3) 0.8453(4) 0.0332(2) 0.083(2) Uani 1 1 d G . . H44 H 0.5951 0.9125 0.0055 0.100 Uiso 1 1 calc R . . C45 C 0.6382(2) 0.8314(4) 0.0972(2) 0.086(2) Uani 1 1 d G . . H45 H 0.6831 0.8892 0.1123 0.103 Uiso 1 1 calc R . . C46 C 0.6237(2) 0.7310(4) 0.13865(15) 0.0678(19) Uani 1 1 d G . . H46 H 0.6590 0.7216 0.1815 0.081 Uiso 1 1 calc R . . C41 C 0.5564(2) 0.6446(4) 0.11609(17) 0.0474(14) Uani 1 1 d G . . C52 C 0.2836(2) 0.1309(5) 0.0810(2) 0.076(2) Uani 1 1 d G . . H52 H 0.2381 0.1878 0.0676 0.091 Uiso 1 1 calc R . . C53 C 0.2780(2) -0.0112(5) 0.0634(2) 0.095(2) Uani 1 1 d G . . H53 H 0.2288 -0.0495 0.0383 0.113 Uiso 1 1 calc R . . C54 C 0.3460(3) -0.0962(3) 0.0833(2) 0.075(2) Uani 1 1 d G . . H54 H 0.3423 -0.1913 0.0715 0.091 Uiso 1 1 calc R . . C55 C 0.4195(3) -0.0390(4) 0.1208(2) 0.074(2) Uani 1 1 d G . . H55 H 0.4650 -0.0958 0.1341 0.089 Uiso 1 1 calc R . . C56 C 0.4251(2) 0.1032(5) 0.13838(17) 0.0673(18) Uani 1 1 d G . . H56 H 0.4743 0.1414 0.1635 0.081 Uiso 1 1 calc R . . C51 C 0.3571(3) 0.1881(3) 0.11847(19) 0.0488(15) Uani 1 1 d G . . C62 C 0.6288(2) 0.2622(5) 0.23133(17) 0.0634(17) Uani 1 1 d G . . H62 H 0.6015 0.2689 0.2610 0.076 Uiso 1 1 calc R . . C63 C 0.6819(3) 0.1513(4) 0.23615(19) 0.0724(19) Uani 1 1 d G . . H63 H 0.6903 0.0839 0.2690 0.087 Uiso 1 1 calc R . . C64 C 0.7226(2) 0.1413(4) 0.1918(2) 0.076(2) Uani 1 1 d G . . H64 H 0.7582 0.0671 0.1950 0.092 Uiso 1 1 calc R . . C65 C 0.7101(2) 0.2422(5) 0.1427(2) 0.076(2) Uani 1 1 d G . . H65 H 0.7373 0.2355 0.1130 0.091 Uiso 1 1 calc R . . C66 C 0.6569(2) 0.3531(4) 0.13783(16) 0.0625(17) Uani 1 1 d G . . H66 H 0.6486 0.4205 0.1049 0.075 Uiso 1 1 calc R . . C61 C 0.61627(19) 0.3631(4) 0.18216(19) 0.0467(14) Uani 1 1 d G . . 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 0.0459(4) 0.0522(4) 0.0497(4) -0.0026(3) 0.0181(3) -0.0062(3) As2 0.0428(3) 0.0556(4) 0.0400(3) 0.0003(3) 0.0164(3) -0.0037(3) Co1 0.0589(5) 0.0652(6) 0.0541(5) -0.0073(4) 0.0288(4) -0.0133(4) Co2 0.0471(5) 0.0634(6) 0.0429(5) -0.0041(4) 0.0181(4) -0.0050(4) O1 0.048(2) 0.060(2) 0.049(2) -0.005(2) 0.0211(18) -0.010(2) O3 0.097(4) 0.274(9) 0.158(6) -0.065(6) 0.082(4) -0.069(5) O4 0.118(4) 0.090(4) 0.122(5) -0.032(4) 0.049(4) -0.047(4) O5 0.204(7) 0.092(5) 0.102(5) 0.037(4) 0.029(4) 0.007(4) O6 0.103(4) 0.179(6) 0.070(3) 0.034(4) 0.017(3) 0.031(4) C1 0.052(4) 0.069(4) 0.051(4) -0.002(3) 0.019(3) -0.001(3) C2 0.040(3) 0.063(4) 0.056(4) -0.013(3) 0.017(3) -0.003(3) C3 0.081(5) 0.144(7) 0.085(5) -0.033(5) 0.050(5) -0.036(5) C4 0.055(4) 0.093(6) 0.068(5) -0.019(4) 0.026(4) -0.017(4) C5 0.114(7) 0.084(6) 0.058(5) 0.002(4) 0.026(5) -0.015(5) C6 0.068(5) 0.099(6) 0.063(4) 0.006(4) 0.034(4) 0.009(4) C22 0.077(5) 0.081(5) 0.066(5) -0.020(4) 0.021(4) 0.013(4) C23 0.076(5) 0.123(8) 0.098(6) -0.052(6) 0.009(5) 0.017(5) C24 0.065(5) 0.188(11) 0.069(6) -0.049(7) 0.019(5) 0.029(7) C25 0.080(5) 0.155(8) 0.063(5) -0.010(6) 0.036(4) 0.027(6) C26 0.071(5) 0.097(6) 0.064(5) -0.016(4) 0.033(4) 0.005(4) C21 0.042(4) 0.067(5) 0.062(4) -0.013(4) 0.016(3) 0.012(3) C32 0.043(4) 0.068(5) 0.096(5) -0.002(4) 0.018(4) -0.010(4) C33 0.047(5) 0.075(5) 0.142(7) 0.028(6) 0.021(5) 0.001(4) C34 0.056(5) 0.117(8) 0.125(8) 0.061(6) 0.008(5) -0.004(5) C35 0.069(5) 0.133(8) 0.086(6) 0.040(5) 0.013(5) -0.002(5) C36 0.056(4) 0.089(5) 0.071(5) 0.011(4) 0.011(4) -0.001(4) C31 0.043(4) 0.053(4) 0.065(4) 0.011(3) 0.012(3) -0.007(3) C42 0.064(4) 0.063(4) 0.045(4) -0.003(3) 0.015(3) -0.007(3) C43 0.113(6) 0.081(5) 0.048(4) 0.018(4) 0.023(4) -0.003(5) C44 0.134(7) 0.063(5) 0.066(5) 0.000(4) 0.051(5) -0.024(5) C45 0.094(6) 0.098(6) 0.070(5) -0.005(4) 0.031(5) -0.036(5) C46 0.078(5) 0.075(5) 0.051(4) 0.007(4) 0.022(4) -0.023(4) C41 0.057(4) 0.044(4) 0.045(3) -0.001(3) 0.021(3) -0.002(3) C52 0.063(5) 0.053(4) 0.105(6) -0.010(4) 0.021(4) -0.013(4) C53 0.078(5) 0.064(5) 0.133(7) -0.014(5) 0.025(5) -0.023(5) C54 0.105(6) 0.046(4) 0.084(5) -0.003(4) 0.043(5) -0.016(5) C55 0.084(5) 0.061(5) 0.074(5) 0.006(4) 0.023(4) 0.010(4) C56 0.069(5) 0.058(4) 0.064(4) -0.001(4) 0.010(3) 0.003(4) C51 0.056(4) 0.046(4) 0.048(4) -0.003(3) 0.022(3) -0.007(3) C62 0.054(4) 0.068(5) 0.066(4) 0.003(4) 0.018(3) 0.002(4) C63 0.053(4) 0.076(5) 0.077(5) 0.018(4) 0.007(4) 0.003(4) C64 0.059(4) 0.065(5) 0.094(6) -0.006(4) 0.013(4) 0.006(4) C65 0.066(5) 0.086(5) 0.084(5) -0.008(4) 0.036(4) 0.010(4) C66 0.059(4) 0.070(5) 0.062(4) 0.007(4) 0.026(3) 0.005(4) C61 0.039(3) 0.053(4) 0.044(3) -0.004(3) 0.008(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O1 1.806(3) . ? As1 C51 1.934(3) . ? As1 C31 1.946(3) . ? As1 Co1 2.3018(12) . ? As2 O1 1.791(3) . ? As2 C41 1.942(3) . ? As2 C61 1.957(3) . ? As2 Co2 2.3092(11) . ? Co1 C5 1.776(8) . ? Co1 C3 1.761(7) . ? Co1 C2 1.923(6) . ? Co1 C1 1.950(6) . ? Co1 Co2 2.4837(13) . ? Co2 C6 1.780(7) . ? Co2 C4 1.774(7) . ? Co2 C2 1.967(5) . ? Co2 C1 1.954(5) . ? O3 C3 1.145(7) . ? O4 C4 1.144(7) . ? O5 C5 1.153(8) . ? O6 C6 1.146(7) . ? C1 C2 1.339(7) . ? C2 C21 1.464(7) . ? C22 C21 1.390(8) . ? C22 C23 1.391(9) . ? C23 C24 1.374(11) . ? C24 C25 1.366(11) . ? C25 C26 1.385(8) . ? C26 C21 1.396(8) . ? C32 C33 1.3900 . ? C32 C31 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C31 1.3900 . ? C42 C43 1.3900 . ? C42 C41 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C41 1.3900 . ? C52 C53 1.3900 . ? C52 C51 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C51 1.3900 . ? C62 C63 1.3900 . ? C62 C61 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C61 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 As1 C51 96.38(16) . . ? O1 As1 C31 98.24(16) . . ? C51 As1 C31 103.11(18) . . ? O1 As1 Co1 111.42(11) . . ? C51 As1 Co1 121.94(12) . . ? C31 As1 Co1 120.75(15) . . ? O1 As2 C41 97.53(16) . . ? O1 As2 C61 97.49(16) . . ? C41 As2 C61 102.22(17) . . ? O1 As2 Co2 114.04(11) . . ? C41 As2 Co2 120.96(12) . . ? C61 As2 Co2 120.04(13) . . ? C5 Co1 C3 99.7(4) . . ? C5 Co1 C2 111.1(3) . . ? C3 Co1 C2 98.7(3) . . ? C5 Co1 C1 144.7(3) . . ? C3 Co1 C1 104.7(3) . . ? C2 Co1 C1 40.5(2) . . ? C5 Co1 As1 103.6(2) . . ? C3 Co1 As1 101.9(2) . . ? C2 Co1 As1 135.62(18) . . ? C1 Co1 As1 96.00(17) . . ? C5 Co1 Co2 97.0(2) . . ? C3 Co1 Co2 149.4(3) . . ? C2 Co1 Co2 51.11(16) . . ? C1 Co1 Co2 50.56(16) . . ? As1 Co1 Co2 98.83(5) . . ? C6 Co2 C4 100.3(3) . . ? C6 Co2 C2 102.2(3) . . ? C4 Co2 C2 102.1(3) . . ? C6 Co2 C1 141.4(3) . . ? C4 Co2 C1 96.6(3) . . ? C2 Co2 C1 40.0(2) . . ? C6 Co2 As2 107.7(2) . . ? C4 Co2 As2 100.0(2) . . ? C2 Co2 As2 138.63(17) . . ? C1 Co2 As2 103.18(17) . . ? C6 Co2 Co1 103.5(2) . . ? C4 Co2 Co1 146.2(2) . . ? C2 Co2 Co1 49.54(16) . . ? C1 Co2 Co1 50.42(17) . . ? As2 Co2 Co1 95.30(4) . . ? As2 O1 As1 118.37(18) . . ? C2 C1 Co1 68.7(4) . . ? C2 C1 Co2 70.6(3) . . ? Co1 C1 Co2 79.0(2) . . ? C1 C2 C21 141.8(6) . . ? C1 C2 Co1 70.8(4) . . ? C21 C2 Co1 138.1(5) . . ? C1 C2 Co2 69.5(3) . . ? C21 C2 Co2 129.2(4) . . ? Co1 C2 Co2 79.3(2) . . ? O3 C3 Co1 176.8(7) . . ? O4 C4 Co2 175.9(6) . . ? O5 C5 Co1 178.4(8) . . ? O6 C6 Co2 176.8(7) . . ? C21 C22 C23 119.5(7) . . ? C24 C23 C22 121.4(9) . . ? C25 C24 C23 118.8(8) . . ? C24 C25 C26 121.4(9) . . ? C21 C26 C25 119.9(7) . . ? C26 C21 C22 118.9(6) . . ? C26 C21 C2 120.8(6) . . ? C22 C21 C2 120.3(6) . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C31 C36 C35 120.0 . . ? C36 C31 C32 120.0 . . ? C36 C31 As1 120.7(3) . . ? C32 C31 As1 119.2(3) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C46 C41 C42 120.0 . . ? C46 C41 As2 118.2(2) . . ? C42 C41 As2 121.7(2) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C51 C56 C55 120.0 . . ? C56 C51 C52 120.0 . . ? C56 C51 As1 118.4(3) . . ? C52 C51 As1 121.6(3) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C61 C66 C65 120.0 . . ? C66 C61 C62 120.0 . . ? C66 C61 As2 122.9(3) . . ? C62 C61 As2 117.1(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.304 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.080 data_ab115 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H20 As2 Cl Co3 O8' _chemical_formula_weight 894.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.843(4) _cell_length_b 11.199(3) _cell_length_c 19.844(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.873(15) _cell_angle_gamma 90.00 _cell_volume 3497.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 3.407 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.148 _exptl_absorpt_correction_T_max 0.620 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens p4' _diffrn_measurement_method THETA/2THETA _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.9 _diffrn_reflns_number 12717 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6162 _reflns_number_gt 3110 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6162 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1613 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.47541(8) 1.57837(12) 0.34105(8) 0.0546(4) Uani 1 1 d . . . Co3 Co 0.33928(9) 1.66302(13) 0.25985(9) 0.0665(5) Uani 1 1 d . . . Co2 Co 0.45154(9) 1.61104(12) 0.21055(8) 0.0622(4) Uani 1 1 d . . . As1 As 0.59080(6) 1.45493(9) 0.36487(6) 0.0498(3) Uani 1 1 d . . . As2 As 0.54425(7) 1..46987(9) 0.19945(6) 0.0572(3) Uani 1 1 d . . . O1 O 0.5945(4) 1.3725(8) 0.2812(3) 0.074(2) Uani 1 1 d . . . C1 C 0.3970(6) 1.5156(9) 0.2572(5) 0.054(3) Uani 1 1 d . . . Cl1 Cl 0.34917(17) 1.3744(2) 0.23528(16) 0.0680(8) Uani 1 1 d . . . O3 O 0.4111(6) 1.4669(10) 0.4437(5) 0.116(4) Uani 1 1 d . . . C3 C 0.4386(8) 1.5103(11) 0.4064(7) 0.076(4) Uani 1 1 d . . . O4 O 0.3361(7) 1.5821(10) 0.0622(5) 0.137(4) Uani 1 1 d . . . C4 C 0.3850(9) 1.5971(12) 0.1197(7) 0.093(4) Uani 1 1 d . . . O5 O 0.5611(6) 1.8024(9) 0.4076(6) 0.133(4) Uani 1 1 d . . . C5 C 0.5290(8) 1.7146(12) 0.3831(7) 0.084(4) Uani 1 1 d . . . O6 O 0.5337(8) 1.8451(9) 0.2206(8) 0.166(5) Uani 1 1 d . . . C6 C 0.5042(9) 1.7523(12) 0.2161(9) 0.109(5) Uani 1 1 d . . . O7 O 0.2352(6) 1.5891(10) 0.3429(6) 0.128(4) Uani 1 1 d . . . C7 C 0.2744(7) 1.6190(11) 0.3100(7) 0.084(4) Uani 1 1 d . . . C8 C 0.2552(9) 1.6707(14) 0.1781(9) 0.103(5) Uani 1 1 d . . . O8 O 0.1951(7) 1.6716(11) 0.1241(6) 0.141(4) Uani 1 1 d . . . O9 O 0.3813(6) 1.9176(9) 0.2945(7) 0.133(4) Uani 1 1 d . . . C9 C 0.3630(8) 1.8182(12) 0.2808(8) 0.096(4) Uani 1 1 d . . . C31 C 0.6011(4) 1.3113(5) 0.4214(4) 0.049(2) Uani 1 1 d G . . C32 C 0.5326(4) 1.2330(7) 0.4020(4) 0.082(4) Uani 1 1 d G . . H32 H 0.4833 1.2509 0.3633 0.098 Uiso 1 1 calc R . . C33 C 0.5377(5) 1.1278(6) 0.4405(5) 0.112(5) Uani 1 1 d G . . H33 H 0.4919 1.0754 0.4276 0.134 Uiso 1 1 calc R . . C34 C 0.6114(6) 1.1010(6) 0.4984(5) 0.105(5) Uani 1 1 d G . . H34 H 0.6148 1.0306 0.5242 0.126 Uiso 1 1 calc R . . C35 C 0.6799(5) 1.1793(7) 0.5177(4) 0.089(4) Uani 1 1 d G . . H35 H 0.7291 1.1613 0.5565 0.107 Uiso 1 1 calc R . . C36 C 0.6747(4) 1.2845(6) 0.4792(4) 0.065(3) Uani 1 1 d G . . H36 H 0.7205 1.3369 0.4922 0.078 Uiso 1 1 calc R . . C41 C 0.4944(5) 1.3402(8) 0.1361(7) 0.086(4) Uani 1 1 d G . . C42 C 0.4849(6) 1.2280(10) 0.1622(6) 0.132(7) Uani 1 1 d G . . H42 H 0.5062 1.2134 0.2116 0.159 Uiso 1 1 calc R . . C43 C 0.4435(7) 1.1378(7) 0.1146(9) 0.180(11) Uani 1 1 d G . . H43 H 0.4371 1.0627 0.1321 0.216 Uiso 1 1 calc R . . C44 C 0.4116(6) 1.1596(12) 0.0408(8) 0.181(12) Uani 1 1 d G . . H44 H 0.3839 1.0992 0.0090 0.217 Uiso 1 1 calc R . . C45 C 0.4211(7) 1.2717(15) 0.0147(5) 0.217(14) Uani 1 1 d G . . H45 H 0.3998 1.2864 -0.0347 0.260 Uiso 1 1 calc R . . C46 C 0.4626(7) 1.3620(10) 0.0623(7) 0.123(6) Uani 1 1 d G . . H46 H 0.4690 1.4370 0.0448 0.147 Uiso 1 1 calc R . . C51 C 0.7026(3) 1.5246(6) 0.4029(4) 0.064(3) Uani 1 1 d G . . C52 C 0.7250(6) 1.5913(8) 0.4660(5) 0.094(4) Uani 1 1 d G . . H52 H 0.6865 1.6007 0.4895 0.113 Uiso 1 1 calc R . . C53 C 0.8049(7) 1.6438(8) 0.4940(5) 0.145(7) Uani 1 1 d G . . H53 H 0.8198 1.6884 0.5362 0.175 Uiso 1 1 calc R . . C54 C 0.8624(4) 1.6297(8) 0.4588(6) 0.143(8) Uani 1 1 d G . . H54 H 0.9158 1.6648 0.4775 0.171 Uiso 1 1 calc R . . C55 C 0.8400(4) 1.5630(9) 0.3957(6) 0.124(7) Uani 1 1 d G . . H55 H 0.8785 1.5535 0.3722 0.149 Uiso 1 1 calc R . . C56 C 0.7601(5) 1.5105(7) 0.3677(4) 0.082(4) Uani 1 1 d G . . H56 H 0.7452 1.4658 0.3255 0.099 Uiso 1 1 calc R . . C61 C 0.6434(4) 1.5084(7) 0.1763(4) 0.066(3) Uani 1 1 d G . . C62 C 0.6824(5) 1.4202(6) 0.1497(5) 0.089(4) Uani 1 1 d G . . H62 H 0.6578 1.3449 0.1388 0.107 Uiso 1 1 calc R . . C63 C 0.7581(5) 1.4444(9) 0.1393(5) 0.119(6) Uani 1 1 d G . . H63 H 0.7842 1.3854 0.1215 0.143 Uiso 1 1 calc R . . C64 C 0.7949(4) 1.5569(11) 0.1555(5) 0.137(7) Uani 1 1 d G . . H64 H 0.8456 1.5731 0.1485 0.165 Uiso 1 1 calc R . . C65 C 0.7560(6) 1.6451(7) 0.1821(5) 0.129(6) Uani 1 1 d G . . H65 H 0.7806 1.7204 0.1929 0.155 Uiso 1 1 calc R . . C66 C 0.6802(6) 1.6209(6) 0.1925(5) 0.097(4) Uani 1 1 d G . . H66 H 0.6542 1.6799 0.2103 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0474(8) 0.0605(8) 0.0541(10) -0.0079(7) 0.0157(7) 0.0040(6) Co3 0.0537(9) 0.0680(9) 0.0705(12) -0.0053(8) 0.0131(9) 0..0136(7) Co2 0.0737(11) 0.0525(8) 0.0644(11) 0.0097(8) 0.0297(9) 0.0066(7) As1 0.0444(6) 0.0545(6) 0.0514(7) 0.0035(5) 0.0181(5) 0.0015(5) As2 0.0638(7) 0.0552(6) 0.0605(8) 0.0040(6) 0.0316(6) -0.0010(5) O1 0.054(4) 0.146(7) 0.025(4) 0.038(4) 0.020(4) 0.032(4) C1 0.050(6) 0.069(6) 0.043(7) -0.009(5) 0.016(5) 0.010(5) Cl1 0.0659(18) 0.0618(16) 0.077(2) -0.0104(15) 0.0256(16) -0.0150(13) O3 0.097(7) 0.192(11) 0.078(7) 0.020(7) 0.052(6) 0.001(7) C3 0.067(8) 0.103(10) 0.061(9) -0.009(7) 0.027(7) 0.009(7) O4 0.161(11) 0.157(10) 0.057(7) 0.021(7) -0.007(7) 0.069(8) C4 0.112(11) 0.103(10) 0.058(10) 0.042(9) 0.025(9) 0.053(9) O5 0.106(8) 0.086(7) 0.167(11) -0.051(7) -0.001(7) -0.005(6) C5 0.069(9) 0.084(9) 0.079(10) -0.013(8) 0.003(8) 0.012(7) O6 0.184(12) 0.063(6) 0.279(16) 0.007(8) 0.118(12) -0.027(7) C6 0.112(12) 0.068(9) 0.155(15) -0.005(9) 0.057(11) -0.006(8) O7 0.100(8) 0.174(10) 0.141(10) 0.004(8) 0.080(7) 0.027(7) C7 0.060(8) 0.095(9) 0.100(11) -0.028(8) 0.030(8) 0.007(7) C8 0.067(9) 0.118(11) 0.110(13) 0.017(10) 0.014(9) 0.037(9) O8 0.116(9) 0.162(10) 0.116(10) -0.009(8) 0.005(8) 0.040(8) O9 0.106(8) 0.076(6) 0.202(12) -0.008(8) 0.036(8) 0.018(6) C9 0.071(9) 0.075(9) 0.136(14) -0.003(9) 0.031(9) 0.016(7) C31 0.043(6) 0.063(6) 0.037(7) 0.003(5) 0.009(5) 0.003(5) C32 0.072(8) 0.080(8) 0.091(10) 0.020(7) 0.026(8) -0.007(7) C33 0.110(12) 0.091(10) 0.145(15) 0.036(10) 0.059(11) -0.021(9) C34 0.116(12) 0.076(9) 0.134(14) 0.044(9) 0.057(11) 0.018(9) C35 0.095(10) 0.088(9) 0.073(9) 0.034(8) 0.016(8) 0.022(8) C36 0.068(8) 0.053(6) 0.073(9) 0.011(6) 0.025(7) 0.000(5) C41 0.052(7) 0.085(9) 0.121(13) -0.033(9) 0.031(8) -0.008(6) C42 0.146(14) 0.083(10) 0.24(2) -0.060(12) 0.151(15) -0.034(9) C43 0.116(15) 0.143(16) 0.32(3) -0.148(19) 0.127(19) -0.067(12) C44 0.063(11) 0.22(2) 0.24(3) -0.17(2) 0.024(15) -0.009(13) C45 0.120(17) 0.24(3) 0.25(3) -0.17(2) 0.011(17) 0.028(18) C46 0.096(12) 0.154(16) 0.109(14) -0.054(13) 0.025(11) 0.016(11) C51 0.040(6) 0.058(6) 0.092(10) 0.022(7) 0.021(6) 0.001(5) C52 0.055(8) 0.078(8) 0.136(13) -0.033(9) 0.018(8) -0.008(7) C53 0.095(12) 0.091(11) 0.23(2) -0.047(12) 0.030(14) -0.020(10) C54 0.073(11) 0.085(11) 0.25(2) 0.038(13) 0.028(14) -0.022(9) C55 0.054(9) 0.162(16) 0.144(16) 0.083(13) 0.021(10) 0.004(10) C56 0.039(7) 0.123(10) 0.080(10) 0.044(8) 0.015(7) 0.013(6) C61 0.072(8) 0.085(8) 0.045(8) -0.004(6) 0.028(6) -0.009(6) C62 0.090(9) 0.101(9) 0.092(10) -0.032(8) 0.052(9) -0.023(8) C63 0.095(11) 0.175(16) 0.111(13) -0.030(12) 0.064(10) -0.006(11) C64 0.110(13) 0.183(18) 0.159(17) 0.035(15) 0.097(13) -0.016(13) C65 0.122(14) 0.123(13) 0.162(17) 0.042(12) 0.076(13) -0.023(11) C66 0.106(11) 0.088(9) 0.102(11) 0.018(8) 0.041(9) -0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C3 1.795(14) . ? Co1 C5 1.818(14) . ? Co1 C1 1.855(10) . ? Co1 As1 2.2928(17) . ? Co1 Co3 2.474(2) . ? Co1 Co2 2.502(2) . ? Co3 C8 1.734(15) . ? Co3 C7 1.790(14) . ? Co3 C9 1.798(14) . ? Co3 C1 1.927(9) . ? Co3 Co2 2.488(2) . ? Co2 C4 1.758(14) . ? Co2 C6 1.798(14) . ? Co2 C1 1.856(10) . ? Co2 As2 2.2872(18) . ? As1 O1 1.921(7) . ? As1 C51 1.927(6) . ? As1 C31 1.933(5) . ? As2 O1 1.886(6) . ? As2 C41 1.909(7) . ? As2 C61 1.933(6) . ? C1 Cl1 1.758(10) . ? O3 C3 1.114(13) . ? O4 C4 1.157(14) . ? O5 C5 1.143(13) . ? O6 C6 1.141(14) . ? O7 C7 1.131(14) . ? C8 O8 1.184(14) . ? O9 C9 1.162(14) .. ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co1 C5 105.5(6) . . ? C3 Co1 C1 99.7(5) . . ? C5 Co1 C1 144.0(5) . . ? C3 Co1 As1 94.6(4) . . ? C5 Co1 As1 99.5(4) . . ? C1 Co1 As1 103.7(3) . . ? C3 Co1 Co3 98.9(4) . . ? C5 Co1 Co3 99.9(4) . . ? C1 Co1 Co3 50.4(3) . . ? As1 Co1 Co3 152.40(8) . . ? C3 Co1 Co2 147.2(4) . . ? C5 Co1 Co2 102.9(4) . . ? C1 Co1 Co2 47.6(3) . . ? As1 Co1 Co2 96.51(6) . . ? Co3 Co1 Co2 59.99(6) . . ? C8 Co3 C7 94.4(6) . . ? C8 Co3 C9 102.0(7) . . ? C7 Co3 C9 105.5(6) . . ? C8 Co3 C1 105.6(6) . . ? C7 Co3 C1 101.2(5) . . ? C9 Co3 C1 139.6(5) . . ? C8 Co3 Co1 152.5(5) . . ? C7 Co3 Co1 98.0(4) . . ? C9 Co3 Co1 98.1(4) . . ? C1 Co3 Co1 47.9(3) . . ? C8 Co3 Co2 97.2(5) . . ? C7 Co3 Co2 148.7(4) . . ? C9 Co3 Co2 100.4(4) . . ? C1 Co3 Co2 47.7(3) . . ? Co1 Co3 Co2 60.57(6) . . ? C4 Co2 C6 105.1(7) . . ? C4 Co2 C1 102.2(6) . . ? C6 Co2 C1 142.9(6) . . ? C4 Co2 As2 92.7(4) . . ? C6 Co2 As2 106.0(5) . . ? C1 Co2 As2 97.2(3) . . ? C4 Co2 Co3 97.3(4) . . ? C6 Co2 Co3 101.4(5) . . ? C1 Co2 Co3 50.1(3) . . ? As2 Co2 Co3 147.16(8) . . ? C4 Co2 Co1 149.0(5) . . ? C6 Co2 Co1 99.9(5) . . ? C1 Co2 Co1 47.6(3) . . ? As2 Co2 Co1 97.77(7) . . ? Co3 Co2 Co1 59.44(6) . . ? O1 As1 C51 101.8(3) . . ? O1 As1 C31 94.5(3) . . ? C51 As1 C31 103.7(3) . . ? O1 As1 Co1 113.4(2) . . ? C51 As1 Co1 118.4(2) . . ? C31 As1 Co1 121.0(2) . . ? O1 As2 C41 94.8(5) . . ? O1 As2 C61 99.9(3) . . ? C41 As2 C61 103.1(4) . . ? O1 As2 Co2 115.4(2) . . ? C41 As2 Co2 115.8(3) . . ? C61 As2 Co2 123.1(2) . . ? As2 O1 As1 108.8(4) . . ? Cl1 C1 Co2 131.3(6) . . ? Cl1 C1 Co1 132.8(6) . . ? Co2 C1 Co1 84.8(4) . . ? Cl1 C1 Co3 125.9(5) . . ? Co2 C1 Co3 82.2(4) . . ? Co1 C1 Co3 81.7(4) . . ? O3 C3 Co1 175.8(12) . . ? O4 C4 Co2 173.7(14) . . ? O5 C5 Co1 177.7(13) . . ? O6 C6 Co2 175.8(14) . . ? O7 C7 Co3 178.0(13) . . ? O8 C8 Co3 176.1(15) . . ? O9 C9 Co3 177.5(12) . . ? C32 C31 C36 120.0 . . ? C32 C31 As1 118.1(4) . . ? C36 C31 As1 121.9(4) . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 As2 121.6(8) . . ? C46 C41 As2 118.3(8) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 As1 118.9(5) . . ? C56 C51 As1 121.1(5) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 As2 119.8(5) . . ? C66 C61 As2 120.0(5) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.574 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.132 data_sB060 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 As4 Co2 O4' _chemical_formula_weight 804.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.387(3) _cell_length_b 18.918(4) _cell_length_c 19.785(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.142(7) _cell_angle_gamma 90.00 _cell_volume 6069.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 5.447 _exptl_absorpt_correction_type 'semi-empirical using psi-scans' _exptl_absorpt_correction_T_min 0.4055 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 8960 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 22.00 _reflns_number_total 7420 _reflns_number_gt 4113 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7420 _refine_ls_number_parameters 541 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.09673(10) 0.01415(9) 0.22567(8) 0.0445(5) Uani 1 1 d D . . As2 As -0.08102(11) -0.01006(9) 0.12164(8) 0.0458(5) Uani 1 1 d D . . As3 As 0.05162(10) 0.04231(9) 0.38971(7) 0.0395(4) Uani 1 1 d D . . As4 As -0.10337(11) -0.03632(9) 0.29538(8) 0.0448(5) Uani 1 1 d D . . Co1 Co 0.03374(12) 0.09084(10) 0.27935(9) 0.0333(5) Uani 1 1 d D . . Co2 Co -0.10861(12) 0.04827(11) 0.21178(9) 0.0357(6) Uani 1 1 d D . . O1 O 0.0272(5) -0.0280(6) 0.1437(5) 0.061(3) Uani 1 1 d D . . O2 O -0.0299(6) -0.0191(6) 0.3842(4) 0.059(3) Uani 1 1 d D . . O3 O 0.1491(8) 0.2067(6) 0.3222(7) 0.087(4) Uani 1 1 d D . . O4 O -0.2841(7) 0.0732(8) 0.1420(7) 0.096(5) Uani 1 1 d D . . C1 C -0.0554(8) 0.1377(6) 0.2052(6) 0.031(4) Uani 1 1 d D . . C2 C -0.0740(8) 0.1335(7) 0.2663(6) 0.034(4) Uani 1 1 d D . . C3 C 0.1065(9) 0.1593(7) 0.3042(8) 0.044(4) Uani 1 1 d D . . C4 C -0.2163(8) 0.0616(10) 0.1706(8) 0.059(5) Uani 1 1 d D . . C11 C -0.0660(7) 0.1922(4) 0.1490(4) 0.037(4) Uani 1 1 d G . . C12 C -0.0072(6) 0.2021(5) 0.1175(6) 0.051(5) Uani 1 1 d G . . H12 H 0.0396 0.1736 0.1311 0.061 Uiso 1 1 calc R . . C13 C -0.0182(7) 0.2545(6) 0.0656(5) 0.063(6) Uani 1 1 d G . . H13 H 0.0212 0.2612 0.0446 0.075 Uiso 1 1 calc R . . C14 C -0.0880(9) 0.2971(5) 0.0453(4) 0.072(7) Uani 1 1 d G . . H14 H -0.0954 0.3322 0.0106 0.086 Uiso 1 1 calc R . . C15 C -0.1469(6) 0.2872(5) 0.0768(6) 0.069(6) Uani 1 1 d G . . H15 H -0.1936 0.3156 0.0632 0.082 Uiso 1 1 calc R . . C16 C -0.1359(6) 0.2347(6) 0.1287(5) 0.048(5) Uani 1 1 d G . . H16 H -0.1753 0.2281 0.1498 0.057 Uiso 1 1 calc R . . C21 C -0.1039(6) 0.1857(5) 0.3090(4) 0.031(4) Uani 1 1 d G . . C22 C -0.0662(5) 0.2513(6) 0.3273(5) 0.052(5) Uani 1 1 d G . . H22 H -0.0224 0.2633 0.3131 0.062 Uiso 1 1 calc R . . C23 C -0.0939(7) 0.2991(4) 0.3668(5) 0.050(5) Uani 1 1 d G . . H23 H -0.0686 0.3430 0.3791 0.060 Uiso 1 1 calc R . . C24 C -0.1593(7) 0.2812(5) 0.3881(5) 0.057(5) Uani 1 1 d G . . H24 H -0.1779 0.3132 0.4146 0.068 Uiso 1 1 calc R . . C25 C -0.1971(5) 0.2156(6) 0.3698(5) 0.046(4) Uani 1 1 d G . . H25 H -0.2409 0.2036 0.3841 0.056 Uiso 1 1 calc R . . C26 C -0.1694(6) 0.1678(4) 0.3303(5) 0.045(4) Uani 1 1 d G . . H26 H -0.1946 0.1239 0.3181 0.054 Uiso 1 1 calc R . . C31 C 0.1547(10) -0.0702(7) 0.2735(8) 0.068(6) Uani 1 1 d D . . H31A H 0.1226 -0.0941 0.2970 0.102 Uiso 1 1 calc R . . H31B H 0.2071 -0.0571 0.3088 0.102 Uiso 1 1 calc R . . H31C H 0.1631 -0.1010 0.2382 0.102 Uiso 1 1 calc R . . C32 C 0.1771(9) 0.0428(9) 0.1843(8) 0.065(5) Uani 1 1 d D . . H32A H 0.1598 0.0863 0.1581 0.098 Uiso 1 1 calc R . . H32B H 0.1818 0.0068 0.1518 0.098 Uiso 1 1 calc R . . H32C H 0.2296 0.0496 0.2223 0.098 Uiso 1 1 calc R . . C41 C -0.1214(11) -0.1029(7) 0.0831(8) 0.071(6) Uani 1 1 d D . . H41A H -0.1146 -0.1350 0.1224 0.107 Uiso 1 1 calc R . . H41B H -0.0908 -0.1198 0.0546 0.107 Uiso 1 1 calc R . . H41C H -0.1788 -0.0997 0.0534 0.107 Uiso 1 1 calc R . . C42 C -0.1010(12) 0.0412(8) 0.0319(6) 0.074(6) Uani 1 1 d D . . H42A H -0.0833 0.0893 0.0427 0.110 Uiso 1 1 calc R . . H42B H -0.1588 0.0402 0.0033 0.110 Uiso 1 1 calc R . . H42C H -0.0708 0.0193 0.0053 0.110 Uiso 1 1 calc R . . C51 C 0.1432(8) -0.0151(8) 0.4525(7) 0.056(5) Uani 1 1 d D . . H51A H 0.1559 -0.0514 0.4243 0.084 Uiso 1 1 calc R . . H51B H 0.1278 -0.0364 0.4899 0.084 Uiso 1 1 calc R . . H51C H 0.1907 0.0144 0.4742 0.084 Uiso 1 1 calc R . . C52 C 0.0399(11) 0.1071(8) 0.4611(7) 0.075(6) Uani 1 1 d D . . H52A H -0.0036 0.1401 0.4379 0.112 Uiso 1 1 calc R . . H52B H 0.0906 0.1323 0.4838 0.112 Uiso 1 1 calc R . . H52C H 0.0267 0.0810 0.4972 0.112 Uiso 1 1 calc R . . C61 C -0.1950(9) -0.0520(9) 0.3284(8) 0.064(5) Uani 1 1 d D . . H61A H -0.2165 -0.0072 0.3363 0.096 Uiso 1 1 calc R . . H61B H -0.1761 -0.0783 0.3729 0.096 Uiso 1 1 calc R . . H61C H -0.2377 -0.0781 0.2923 0.096 Uiso 1 1 calc R . . C62 C -0.0731(11) -0.1331(6) 0.2841(8) 0.074(6) Uani 1 1 d D . . H62A H -0.0273 -0.1333 0.2679 0.111 Uiso 1 1 calc R . . H62B H -0.1191 -0.1568 0.2490 0.111 Uiso 1 1 calc R . . H62C H -0.0579 -0.1572 0.3297 0.111 Uiso 1 1 calc R . . Co1X Co 0.46672(13) 0.79313(10) 0.71214(10) 0.0354(5) Uani 1 1 d D . . Co2X Co 0.61062(13) 0.74877(11) 0.76932(9) 0.0357(5) Uani 1 1 d D . . As1X As 0.41191(10) 0.71368(9) 0.77041(8) 0.0420(5) Uani 1 1 d D . . As2X As 0.59287(11) 0.68480(9) 0.86059(8) 0.0424(5) Uani 1 1 d D . . As3X As 0.44025(11) 0.74999(9) 0.59731(8) 0.0439(5) Uani 1 1 d D . . As4X As 0.60096(10) 0.67149(9) 0.67675(8) 0.0430(5) Uani 1 1 d D . . O1X O 0.4862(5) 0.6801(6) 0.8530(4) 0.053(3) Uani 1 1 d D . . O2X O 0.5239(5) 0.6971(6) 0.5917(4) 0.058(3) Uani 1 1 d D . . O3X O 0.3547(8) 0.9113(6) 0.6893(8) 0.087(4) Uani 1 1 d D . . O4X O 0.7889(7) 0.7676(8) 0.8341(7) 0.094(5) Uani 1 1 d D . . C1X C 0.5595(8) 0.8367(7) 0.7862(7) 0.040(4) Uani 1 1 d D . . C2X C 0.5700(8) 0.8372(7) 0.7209(7) 0.049(5) Uani 1 1 d D . . C3X C 0.3976(10) 0.8636(7) 0.6966(9) 0.053(5) Uani 1 1 d D . . C4X C 0.7196(8) 0.7597(10) 0.8083(8) 0.062(5) Uani 1 1 d D . . C11X C 0.5741(7) 0.8864(5) 0.8487(4) 0.043(4) Uani 1 1 d G . . C12X C 0.5241(6) 0.8827(5) 0.8897(6) 0.054(5) Uani 1 1 d G . . H12X H 0.4795 0.8518 0.8764 0.065 Uiso 1 1 calc R . . C13X C 0.5405(7) 0.9253(6) 0.9505(5) 0.077(7) Uani 1 1 d G . . H13X H 0.5070 0.9228 0.9780 0.092 Uiso 1 1 calc R . . C14X C 0.6071(8) 0.9716(5) 0.9704(4) 0.057(5) Uani 1 1 d G . . H14X H 0.6181 1.0001 1.0111 0.068 Uiso 1 1 calc R . . C15X C 0.6572(6) 0.9753(5) 0.9293(6) 0.073(6) Uani 1 1 d G . . H15X H 0.7017 1.0062 0.9426 0.087 Uiso 1 1 calc R . . C16X C 0.6407(6) 0.9327(6) 0.8685(6) 0.063(5) Uani 1 1 d G . . H16X H 0.6742 0.9352 0.8410 0.076 Uiso 1 1 calc R . . C21X C 0.5976(3) 0.8904(2) 0.6765(2) 0.033(4) Uani 1 1 d G . . C22X C 0.5577(4) 0.9553(2) 0.6598(3) 0.056(5) Uani 1 1 d G . . H22X H 0.5178 0.9672 0.6789 0.067 Uiso 1 1 calc R . . C23X C 0.5775(4) 1.0023(3) 0.6147(3) 0.064(5) Uani 1 1 d G . . H23X H 0.5509 1.0458 0.6035 0.077 Uiso 1 1 calc R . . C24X C 0.6372(4) 0.9845(3) 0.5861(3) 0.057(5) Uani 1 1 d G . . H24X H 0.6505 1.0160 0.5559 0.068 Uiso 1 1 calc R . . C25X C 0.6771(4) 0.9196(3) 0.6028(3) 0.058(5) Uani 1 1 d G . . H25X H 0.7171 0.9076 0.5837 0.070 Uiso 1 1 calc R . . C26X C 0.6573(3) 0.8725(3) 0.6480(3) 0.043(4) Uani 1 1 d G . . H26X H 0.6840 0.8291 0.6592 0.052 Uiso 1 1 calc R . . C31X C 0.3618(4) 0.6262(3) 0.7274(4) 0.068(6) Uani 1 1 d G . . H31D H 0.3946 0..6046 0.7031 0.102 Uiso 1 1 calc R . . H31E H 0.3074 0.6352 0.6931 0.102 Uiso 1 1 calc R . . H31F H 0.3584 0.5950 0.7646 0.102 Uiso 1 1 calc R . . C32X C 0.3303(4) 0.7408(4) 0.8129(4) 0.055(5) Uani 1 1 d G . . H32D H 0.3457 0.7852 0.8376 0.082 Uiso 1 1 calc R . . H32E H 0.3280 0.7052 0.8467 0.082 Uiso 1 1 calc R . . H32F H 0.2771 0.7452 0.7752 0.082 Uiso 1 1 calc R . . C41X C 0.6238(5) 0.5875(3) 0.8829(3) 0.065(6) Uani 1 1 d G . . H41D H 0.6037 0.5598 0.8393 0.098 Uiso 1 1 calc R . . H41E H 0.6005 0.5701 0.9168 0.098 Uiso 1 1 calc R . . H41F H 0.6828 0.5838 0.9036 0.098 Uiso 1 1 calc R . . C42X C 0.6421(5) 0.7232(4) 0.9581(2) 0.077(6) Uani 1 1 d G . . H42D H 0.6321 0.7732 0.9569 0.115 Uiso 1 1 calc R . . H42E H 0.7005 0.7147 0.9761 0.115 Uiso 1 1 calc R . . H42F H 0.6181 0.7008 0.9893 0.115 Uiso 1 1 calc R . . C51X C 0.3489(4) 0.6870(4) 0.5395(3) 0.059(5) Uani 1 1 d G . . H51D H 0.3441 0.6483 0.5691 0.089 Uiso 1 1 calc R . . H51E H 0.3603 0.6690 0.4987 0.089 Uiso 1 1 calc R . . H51F H 0.2982 0.7132 0.5227 0.089 Uiso 1 1 calc R . . C52X C 0.4298(3) 0.8185(3) 0.5214(2) 0.086(7) Uani 1 1 d G . . H52D H 0.4705 0.8549 0.5399 0.128 Uiso 1 1 calc R . . H52E H 0.3757 0.8391 0.5054 0.128 Uiso 1 1 calc R . . H52F H 0.4380 0.7954 0.4813 0.128 Uiso 1 1 calc R . . C62X C 0.5672(4) 0.5729(2) 0.6748(4) 0.076(6) Uani 1 1 d G . . H62D H 0.5236 0.5694 0.6937 0.115 Uiso 1 1 calc R . . H62E H 0.6133 0.5450 0.7040 0.115 Uiso 1 1 calc R . . H62F H 0.5480 0.5558 0.6258 0.115 Uiso 1 1 calc R . . C61X C 0.6873(4) 0.6620(3) 0.6362(4) 0.060(5) Uani 1 1 d G . . H61D H 0.7102 0.7077 0.6337 0.090 Uiso 1 1 calc R . . H61E H 0.6644 0.6422 0.5885 0.090 Uiso 1 1 calc R . . H61F H 0.7299 0.6315 0.6666 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0340(11) 0.0536(12) 0.0471(10) -0.0106(9) 0.0160(9) 0.0020(10) As2 0.0382(11) 0.0538(12) 0.0416(10) -0.0089(9) 0.0097(9) -0.0018(10) As3 0.0377(11) 0.0434(10) 0.0349(9) 0.0001(8) 0.0100(8) -0.0031(9) As4 0.0392(11) 0.0453(11) 0.0452(10) 0.0071(8) 0.0093(9) -0.0087(10) Co1 0.0300(13) 0.0338(13) 0.0372(11) 0.0001(9) 0.0134(10) -0.0004(11) Co2 0.0293(14) 0.0397(13) 0.0356(11) 0.0012(10) 0.0087(10) -0.0011(12) O1 0.041(8) 0.077(9) 0.061(7) -0.033(6) 0.015(6) 0.011(7) O2 0.040(7) 0.087(9) 0.041(6) 0.014(6) 0.004(6) -0.037(7) O3 0.076(11) 0.055(9) 0.121(11) -0.008(8) 0.026(9) -0.016(9) O4 0.042(9) 0.129(14) 0.097(11) -0.019(9) -0.001(8) -0.007(10) C1 0.032(10) 0.034(9) 0.030(8) 0.006(7) 0.015(8) 0.005(8) C2 0.023(9) 0.040(10) 0.040(9) 0.011(8) 0.010(8) 0.001(8) C3 0.038(12) 0.024(10) 0.076(12) -0.004(9) 0.029(10) -0.007(9) C4 0.040(13) 0.073(14) 0.049(11) 0.007(10) -0.003(10) 0.005(12) C11 0.049(12) 0.023(9) 0.037(9) 0.004(7) 0.013(9) 0.000(9) C12 0.048(12) 0.056(12) 0.049(10) -0.011(9) 0.016(9) -0.018(10) C13 0.107(18) 0.051(12) 0.045(10) -0.006(10) 0.044(12) -0.033(13) C14 0.13(2) 0.036(12) 0.036(10) 0.008(9) 0.009(12) -0.004(13) C15 0.080(16) 0.061(14) 0.049(11) 0.001(10) 0.004(11) 0.017(12) C16 0.053(13) 0.050(11) 0.030(9) 0.011(8) 0.003(9) -0.003(10) C21 0.020(9) 0.045(11) 0.020(7) 0.020(7) -0.002(7) 0.013(8) C22 0.061(13) 0.050(12) 0.053(10) 0.013(9) 0.031(10) -0.019(11) C23 0.072(14) 0.030(10) 0.042(10) 0.015(8) 0.015(10) 0.013(10) C24 0.056(14) 0.062(14) 0.046(10) -0.013(9) 0.011(10) 0.012(11) C25 0.033(11) 0.061(13) 0.047(10) -0.006(9) 0.016(9) 0.004(10) C26 0.026(10) 0.064(12) 0.036(9) -0.009(9) 0.000(8) -0.015(10) C31 0.072(15) 0.054(12) 0.078(12) -0.012(10) 0.028(12) 0.014(11) C32 0.037(12) 0.089(15) 0.065(11) -0.005(11) 0.013(10) -0.019(11) C41 0.063(14) 0.050(12) 0.088(13) -0.028(10) 0.013(12) -0.015(11) C42 0.099(17) 0.081(14) 0.040(10) -0.012(10) 0.023(11) 0.004(13) C51 0.050(12) 0.048(11) 0.049(10) 0.005(8) -0.008(9) 0.006(10) C52 0.094(17) 0.079(15) 0.056(11) -0.018(10) 0.032(12) -0.012(13) C61 0.066(14) 0.066(13) 0.069(12) 0.019(10) 0.037(11) -0.004(11) C62 0.066(15) 0.054(13) 0.080(13) 0.023(10) 0.001(11) -0.001(11) Co1X 0.0312(14) 0.0387(13) 0.0351(11) 0.0022(10) 0.0107(10) 0.0008(12) Co2X 0.0313(14) 0.0402(13) 0.0335(11) -0.0013(10) 0.0092(10) -0.0013(12) As1X 0.0322(11) 0.0493(12) 0.0450(10) 0.0070(8) 0.0147(9) 0.0005(9) As2X 0.0357(11) 0.0505(11) 0.0389(9) 0.0063(8) 0.0107(8) 0.0054(9) As3X 0.0381(11) 0.0551(12) 0.0347(9) -0.0019(8) 0.0084(8) 0.0042(10) As4X 0.0361(11) 0.0479(11) 0.0413(9) -0.0054(8) 0.0094(8) 0.0066(9) O1X 0.025(7) 0.090(9) 0.051(6) 0.029(6) 0.023(5) 0.007(6) O2X 0.039(7) 0.095(9) 0.029(6) -0.008(6) 0.001(5) 0.012(7) O3X 0.072(11) 0.043(9) 0.155(13) 0.010(9) 0.051(10) 0.015(8) O4X 0.035(9) 0.110(13) 0.123(12) 0.009(10) 0.011(9) -0.016(9) C1X 0.038(11) 0.047(11) 0.041(9) -0.005(8) 0.022(8) 0.003(9) C2X 0.043(12) 0.046(11) 0.059(10) 0.000(9) 0.021(9) 0.004(9) C3X 0.061(14) 0.033(11) 0.077(12) -0.008(10) 0.038(11) -0.007(11) C4X 0.039(13) 0.085(15) 0.050(11) -0.004(10) 0.001(10) -0.001(12) C11X 0.063(13) 0.030(10) 0.032(9) 0.019(7) 0.013(9) 0.009(10) C12X 0.070(14) 0.038(10) 0.069(12) -0.005(9) 0.043(11) 0.008(10) C13X 0.099(19) 0.088(16) 0.051(12) 0.004(11) 0.036(12) 0.040(15) C14X 0.071(15) 0.048(12) 0.042(10) -0.001(9) 0.008(11) 0.012(11) C15X 0.075(15) 0.072(14) 0.065(12) -0.050(11) 0.017(12) -0.040(12) C16X 0.044(13) 0.053(13) 0.095(14) -0.010(11) 0.029(11) -0.016(11) C21X 0.035(10) 0.023(9) 0.045(9) -0.002(7) 0.019(8) -0.007(8) C22X 0.035(11) 0.047(12) 0.085(12) 0.008(10) 0.022(10) 0.013(10) C23X 0.071(15) 0.056(12) 0.086(13) 0.024(11) 0.054(12) 0.016(11) C24X 0.060(14) 0.054(12) 0.049(10) 0.014(9) 0.010(10) 0.001(11) C25X 0.058(13) 0.076(14) 0.060(11) 0.000(10) 0.045(11) -0.003(11) C26X 0.045(12) 0.035(10) 0.047(9) 0.005(8) 0.014(9) 0.010(9) C31X 0.060(14) 0.054(12) 0.084(13) 0.013(10) 0.020(11) 0.000(11) C32X 0.036(11) 0.074(13) 0.052(10) 0.006(9) 0.012(9) -0.010(10) C41X 0.071(15) 0.067(13) 0.079(13) -0.002(10) 0.053(12) 0.002(12) C42X 0.073(15) 0.108(17) 0.044(10) -0.001(11) 0.014(10) -0.034(13) C51X 0.032(11) 0.055(12) 0.066(11) -0.012(9) -0.013(9) 0.007(10) C52X 0.113(19) 0.094(16) 0.039(10) 0.024(10) 0.015(11) 0.032(15) C62X 0.081(16) 0.077(14) 0.074(12) -0.023(11) 0.032(12) -0.027(13) C61X 0.045(12) 0.078(14) 0.050(10) -0.030(10) 0.010(9) -0.001(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O1 1.820(8) . ? As1 C32 1..935(11) . ? As1 C31 1.941(11) . ? As1 Co1 2.296(2) . ? As2 O1 1.804(8) . ? As2 C42 1.941(11) . ? As2 C41 1.942(11) . ? As2 Co2 2.290(2) . ? As3 O2 1.805(8) . ? As3 C52 1.936(11) . ? As3 C51 1.957(11) . ? As3 Co1 2.284(2) . ? As4 O2 1.791(8) . ? As4 C62 1.941(12) . ? As4 C61 1.951(11) . ? As4 Co2 2.280(2) . ? Co1 C3 1.752(12) . ? Co1 C1 1.924(12) . ? Co1 C2 1.970(12) . ? Co1 Co2 2.485(3) . ? Co2 C4 1.770(13) . ? Co2 C2 1.912(13) . ? Co2 C1 1.955(12) . ? O3 C3 1.137(12) . ? O4 C4 1.130(13) . ? C1 C2 1.360(14) . ? C1 C11 1.478(12) . ? C2 C21 1.509(13) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? Co1X C3X 1.746(13) . ? Co1X C2X 1.931(13) . ? Co1X C1X 1.930(13) . ? Co1X As1X 2.300(2) . ? Co1X As3X 2.299(2) . ? Co1X Co2X 2.490(3) . ? Co2X C4X 1.782(13) . ? Co2X C2X 1.931(13) . ? Co2X C1X 1.971(12) . ? Co2X As2X 2.285(2) . ? Co2X As4X 2.302(2) . ? As1X O1X 1.794(8) . ? As1X C31X 1.920(6) . ? As1X C32X 1.961(5) . ? As2X O1X 1.807(8) . ? As2X C41X 1.925(6) . ? As2X C42X 1.947(6) . ? As3X O2X 1.802(8) . ? As3X C52X 1.943(5) . ? As3X C51X 1.985(5) . ? As4X O2X 1.799(8) . ? As4X C61X 1.949(5) . ? As4X C62X 1.952(5) . ? O3X C3X 1.145(13) . ? O4X C4X 1.135(13) . ? C1X C2X 1.371(14) . ? C1X C11X 1.499(13) . ? C2X C21X 1.522(13) . ? C11X C12X 1.3900 . ? C11X C16X 1.3900 . ? C12X C13X 1.3900 . ? C13X C14X 1.3900 . ? C14X C15X 1.3900 . ? C15X C16X 1.3900 . ? C21X C22X 1.3900 . ? C21X C26X 1.3900 . ? C22X C23X 1.3900 . ? C23X C24X 1.3900 . ? C24X C25X 1.3900 . ? C25X C26X 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 As1 C32 95.4(5) . . ? O1 As1 C31 97.8(6) . . ? C32 As1 C31 96.3(7) . . ? O1 As1 Co1 114.5(3) . . ? C32 As1 Co1 123.8(5) . . ? C31 As1 Co1 123.0(4) . . ? O1 As2 C42 98.2(6) . . ? O1 As2 C41 97.1(6) . . ? C42 As2 C41 99.9(7) . . ? O1 As2 Co2 113.3(3) . . ? C42 As2 Co2 116.9(5) . . ? C41 As2 Co2 126.4(5) . . ? O2 As3 C52 99.4(6) . . ? O2 As3 C51 97.0(6) . . ? C52 As3 C51 99.4(7) . . ? O2 As3 Co1 111.6(3) . . ? C52 As3 Co1 115.4(5) . . ? C51 As3 Co1 129.0(4) . . ? O2 As4 C62 99.1(6) . . ? O2 As4 C61 94.5(5) . . ? C62 As4 C61 100.6(7) . . ? O2 As4 Co2 114.3(3) . . ? C62 As4 Co2 121.4(5) . . ? C61 As4 Co2 121.7(5) . . ? C3 Co1 C1 100.1(6) . . ? C3 Co1 C2 106.9(6) . . ? C1 Co1 C2 40.9(4) . . ? C3 Co1 As3 101.1(5) . . ? C1 Co1 As3 135.1(4) . . ? C2 Co1 As3 94.9(4) . . ? C3 Co1 As1 100.4(5) . . ? C1 Co1 As1 109.0(4) . . ? C2 Co1 As1 142.0(4) . . ? As3 Co1 As1 105.37(10) . . ? C3 Co1 Co2 150.3(5) . . ? C1 Co1 Co2 50.7(4) . . ? C2 Co1 Co2 49.2(4) .. . ? As3 Co1 Co2 98.61(9) . . ? As1 Co1 Co2 95.45(9) . . ? C4 Co2 C2 101.8(7) . . ? C4 Co2 C1 107.0(7) . . ? C2 Co2 C1 41.2(4) . . ? C4 Co2 As4 101.1(6) . . ? C2 Co2 As4 105.1(4) . . ? C1 Co2 As4 139.4(4) . . ? C4 Co2 As2 101.2(6) . . ? C2 Co2 As2 137.2(4) . . ? C1 Co2 As2 97.4(4) . . ? As4 Co2 As2 105.19(10) . . ? C4 Co2 Co1 152.2(6) . . ? C2 Co2 Co1 51.2(4) . . ? C1 Co2 Co1 49.6(4) . . ? As4 Co2 Co1 93.77(9) . . ? As2 Co2 Co1 97.32(9) . . ? As2 O1 As1 115.6(5) . . ? As4 O2 As3 116.3(4) . . ? C2 C1 C11 134.7(12) . . ? C2 C1 Co1 71.4(7) . . ? C11 C1 Co1 137.9(9) . . ? C2 C1 Co2 67.7(7) . . ? C11 C1 Co2 136.0(8) . . ? Co1 C1 Co2 79.7(4) . . ? C1 C2 C21 134.4(11) . . ? C1 C2 Co2 71.1(7) . . ? C21 C2 Co2 140.0(9) . . ? C1 C2 Co1 67.7(7) . . ? C21 C2 Co1 134.3(8) . . ? Co2 C2 Co1 79.6(5) . . ? O3 C3 Co1 174.2(15) . . ? O4 C4 Co2 176.0(19) . . ? C12 C11 C16 120.0 . . ? C12 C11 C1 121.3(9) . . ? C16 C11 C1 118.7(9) . . ? C11 C12 C13 120.0 . .. ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 C2 120.3(9) . . ? C26 C21 C2 119.7(9) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C3X Co1X C2X 104.2(7) . . ? C3X Co1X C1X 98.1(7) . . ? C2X Co1X C1X 41.6(5) . . ? C3X Co1X As1X 101.7(5) . . ? C2X Co1X As1X 141.1(4) . . ? C1X Co1X As1X 106.4(4) . . ? C3X Co1X As3X 102.6(5) . . ? C2X Co1X As3X 95.2(4) . . ? C1X Co1X As3X 135.8(4) . . ? As1X Co1X As3X 106.97(10) . . ? C3X Co1X Co2X 148.5(6) . . ? C2X Co1X Co2X 49.8(4) . . ? C1X Co1X Co2X 51.1(4) . . ? As1X Co1X Co2X 94.72(9) . . ? As3X Co1X Co2X 98.02(9) . . ? C4X Co2X C2X 104.8(7) . . ? C4X Co2X C1X 107.6(7) . . ? C2X Co2X C1X 41.1(4) . . ? C4X Co2X As2X 98.3(6) . . ? C2X Co2X As2X 136.2(4) . . ? C1X Co2X As2X 96.6(4) . . ? C4X Co2X As4X 100.3(6) . . ? C2X Co2X As4X 104.3(4) . . ? C1X Co2X As4X 139.8(4) . . ? As2X Co2X As4X 107.48(10) . . ? C4X Co2X Co1X 153.5(6) . . ? C2X Co2X Co1X 49.8(4) . . ? C1X Co2X Co1X 49.6(4) . . ? As2X Co2X Co1X 97.90(10) . . ? As4X Co2X Co1X 94.57(9) . . ? O1X As1X C31X 99.2(4) . . ? O1X As1X C32X 95.6(4) . . ? C31X As1X C32X 97.6(2) . . ? O1X As1X Co1X 113.3(3) . . ? C31X As1X Co1X 123.0(2) . . ? C32X As1X Co1X 122.6(2) . . ? O1X As2X C41X 99.5(4) . . ? O1X As2X C42X 99.9(4) . . ? C41X As2X C42X 98.3(2) . . ? O1X As2X Co2X 112.8(3) . . ? C41X As2X Co2X 125.5(2) . . ? C42X As2X Co2X 116.6(2) . . ? O2X As3X C52X 100.1(4) . . ? O2X As3X C51X 97.3(4) . . ? C52X As3X C51X 97.1(2) . . ? O2X As3X Co1X 112.3(3) . . ? C52X As3X Co1X 117.2(2) . . ? C51X As3X Co1X 128.0(2) . . ? O2X As4X C61X 93.7(4) . . ? O2X As4X C62X 97.0(4) . . ? C61X As4X C62X 100.1(2) . . ? O2X As4X Co2X 112.9(3) . . ? C61X As4X Co2X 122.7(2) . . ? C62X As4X Co2X 123.9(2) . . ? As1X O1X As2X 116.0(4) . . ? As4X O2X As3X 115.9(4) . . ? C2X C1X C11X 137.1(13) . . ? C2X C1X Co1X 69.2(8) . . ? C11X C1X Co1X 137.8(9) . . ? C2X C1X Co2X 67.9(7) . . ? C11X C1X Co2X 135.7(9) . . ? Co1X C1X Co2X 79.3(5) . . ? C1X C2X C21X 136.6(12) . . ? C1X C2X Co2X 71.0(8) . . ? C21X C2X Co2X 136.4(9) . . ? C1X C2X Co1X 69.2(8) . . ? C21X C2X Co1X 135.3(9) . . ? Co2X C2X Co1X 80.3(5) . . ? O3X C3X Co1X 176.8(18) . . ? O4X C4X Co2X 178.7(19) . . ? C12X C11X C16X 120.0 . . ? C12X C11X C1X 119.6(9) . . ? C16X C11X C1X 120.3(9) . . ? C11X C12X C13X 120.0 . . ? C12X C13X C14X 120.0 . . ? C15X C14X C13X 120.0 . . ? C16X C15X C14X 120.0 . . ? C15X C16X C11X 120.0 . . ? C22X C21X C26X 120.0 . . ? C22X C21X C2X 119.1(5) . . ? C26X C21X C2X 120.7(5) . . ? C23X C22X C21X 120.0 . . ? C22X C23X C24X 120.0 . . ? C25X C24X C23X 120.0 . . ? C26X C25X C24X 120.0 . . ? C25X C26X C21X 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.048 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.173 data_sy109 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 As Co Mo O9' _chemical_formula_weight 720.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.938(4) _cell_length_b 14.533(3) _cell_length_c 16.455(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.94(2) _cell_angle_gamma 90.00 _cell_volume 2812.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.254 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.7723 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method theta\2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.4 _diffrn_reflns_number 17092 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8202 _reflns_number_gt 4317 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8202 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1330 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 1.524 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.02233(6) -0.18040(5) 0.16579(4) 0.03542(18) Uani 1 1 d . . . Mo1 Mo 0.23125(4) -0.25731(3) 0.20218(3) 0.03454(13) Uani 1 1 d . . . As1 As -0.15996(5) -0.18083(4) 0.09037(4) 0.03832(16) Uani 1 1 d . . . O1 O -0.1683(4) -0.1806(3) -0.0181(2) 0.0538(11) Uani 1 1 d . . . O3 O 0.0824(5) 0.0113(4) 0.1420(4) 0.0971(19) Uani 1 1 d . . . O4 O 0.1487(4) -0.3804(3) 0.3386(3) 0.0683(13) Uani 1 1 d . . . O5 O -0.0254(5) -0.1813(4) 0.3348(3) 0.0896(17) Uani 1 1 d . . . O6 O 0.3102(4) -0.4428(3) 0.1316(3) 0.0683(14) Uani 1 1 d . . . C3 C 0.0577(6) -0.0628(5) 0.1518(4) 0.0545(17) Uani 1 1 d . . . C4 C 0.1775(5) -0.3355(4) 0.2897(4) 0.0453(14) Uani 1 1 d . . . C5 C -0.0096(5) -0.1811(4) 0.2685(4) 0.0519(16) Uani 1 1 d . . . C6 C 0.2806(5) -0.3750(4) 0.1565(4) 0.0473(15) Uani 1 1 d . . . C1 C 0.0701(4) -0.3037(4) 0.1377(3) 0.0326(12) Uani 1 1 d . . . C2 C 0.1121(4) -0.2375(4) 0.0906(3) 0.0341(12) Uani 1 1 d . . . O11 O 0.0145(4) -0.4572(3) 0.1622(3) 0.0618(12) Uani 1 1 d . . . O12 O -0.0616(3) -0.3849(3) 0.0452(2) 0.0500(10) Uani 1 1 d . . . C11 C 0.0070(5) -0.3901(4) 0.1188(4) 0.0398(13) Uani 1 1 d . . . C12 C -0.1353(6) -0.4631(5) 0.0212(4) 0.068(2) Uani 1 1 d . . . H12A H -0.1812 -0.4515 -0.0316 0.102 Uiso 1 1 calc R . . H12B H -0.1836 -0.4726 0.0615 0.102 Uiso 1 1 calc R . . H12C H -0.0899 -0.5171 0.0180 0.102 Uiso 1 1 calc R . . O22 O 0.1932(4) -0.2944(3) -0.0186(3) 0.0583(12) Uani 1 1 d . . . O21 O 0.0527(4) -0.1909(3) -0.0502(3) 0.0604(12) Uani 1 1 d . . . C21 C 0.1151(5) -0.2366(4) 0.0013(4) 0.0428(14) Uani 1 1 d . . . C22 C 0.1977(7) -0.3037(6) -0.1055(5) 0.084(2) Uani 1 1 d . . . H22A H 0.2560 -0.3470 -0.1125 0.126 Uiso 1 1 calc R . . H22B H 0.2146 -0.2451 -0.1273 0.126 Uiso 1 1 calc R . . H22C H 0.1256 -0.3253 -0.1342 0.126 Uiso 1 1 calc R . . C31 C -0.25765(18) -0.07543(19) 0.09832(18) 0.0448(14) Uani 1 1 d G . . C32 C -0.2578(2) -0.0015(3) 0.04468(18) 0.076(2) Uani 1 1 d G . . H32 H -0.2106 -0.0022 0.0053 0.091 Uiso 1 1 calc R . . C33 C -0.3287(2) 0.0734(2) 0.0499(2) 0.092(3) Uani 1 1 d G . . H33 H -0.3288 0.1228 0.0140 0.111 Uiso 1 1 calc R . . C34 C -0.3993(2) 0.0743(2) 0.1088(2) 0.078(2) Uani 1 1 d G . . H34 H -0.4467 0.1245 0.1123 0.093 Uiso 1 1 calc R . . C35 C -0.3991(2) 0.0004(3) 0.1624(2) 0.0680(19) Uani 1 1 d G . . H35 H -0.4464 0.0011 0.2018 0.082 Uiso 1 1 calc R . . C36 C -0.32831(18) -0.0744(2) 0.1572(2) 0.0613(18) Uani 1 1 d G . . H36 H -0.3282 -0.1239 0.1931 0.074 Uiso 1 1 calc R . . C41 C 0.30247(18) -0.1141(2) 0.25690(19) 0.0559(17) Uani 1 1 d G . . C42 C 0.3531(2) -0.1859(3) 0.30866(19) 0.0584(17) Uani 1 1 d G . . C43 C 0.4195(2) -0.2477(2) 0.2687(2) 0.0599(17) Uani 1 1 d G . . C44 C 0.41218(19) -0.2061(3) 0.1830(2) 0.0583(17) Uani 1 1 d G . . C45 C 0.33996(18) -0.1251(2) 0.1783(2) 0.0569(17) Uani 1 1 d G . . C51 C -0.2670(3) -0.2793(3) 0.1022(3) 0.0447(14) Uani 1 1 d G . . C52 C -0.2544(3) -0.3298(3) 0.1750(2) 0.0591(17) Uani 1 1 d G . . H52 H -0.1951 -0.3165 0.2179 0.071 Uiso 1 1 calc R . . C53 C -0.3306(4) -0.3999(3) 0.1837(3) 0.075(2) Uani 1 1 d G . . H53 H -0.3222 -0.4337 0.2324 0.090 Uiso 1 1 calc R . . C54 C -0.4193(4) -0.4197(3) 0.1195(3) 0.080(2) Uani 1 1 d G . . H54 H -0.4703 -0.4667 0.1253 0.097 Uiso 1 1 calc R . . C55 C -0.4319(3) -0.3693(4) 0.0467(3) 0.079(2) Uani 1 1 d G . . H55 H -0.4912 -0.3825 0.0038 0.095 Uiso 1 1 calc R . . C56 C -0.3557(4) -0.2991(3) 0.0381(2) 0.0631(19) Uani 1 1 d G . . H56 H -0.3641 -0.2654 -0.0106 0.076 Uiso 1 1 calc R . . Q1 H -0.0944 -0.1704 -0.0273 0.07(2) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0336(4) 0.0361(4) 0.0356(4) -0.0035(3) 0.0032(3) 0.0004(3) Mo1 0.0300(2) 0.0348(3) 0.0370(2) 0.0001(2) 0.00057(18) -0.0038(2) As1 0.0328(3) 0.0441(3) 0.0374(3) -0.0028(3) 0.0041(2) 0.0038(3) O1 0.042(3) 0.081(3) 0.037(2) -0.004(2) 0.003(2) 0.010(2) O3 0.110(5) 0.041(4) 0.133(5) 0.019(3) -0.001(4) -0.009(3) O4 0.070(3) 0.078(3) 0.054(3) 0.018(3) 0.004(3) -0.024(3) O5 0.105(4) 0.127(4) 0.042(3) -0.013(3) 0.026(3) 0.010(4) O6 0.051(3) 0.052(3) 0.101(4) -0.021(3) 0.011(3) 0.004(3) C3 0.050(4) 0.043(4) 0.067(4) 0.005(3) 0.002(3) 0.007(3) C4 0.037(3) 0.050(4) 0.045(4) 0.003(3) -0.004(3) -0.010(3) C5 0.049(4) 0.055(4) 0.050(4) -0.013(3) 0.004(3) 0.001(3) C6 0.032(3) 0.047(4) 0.061(4) 0.000(3) 0.004(3) -0.004(3) C1 0.030(3) 0.033(3) 0.035(3) 0.000(2) 0.006(2) 0.002(2) C2 0.031(3) 0.034(3) 0.037(3) 0.003(2) 0.003(2) 0.002(2) O11 0.072(3) 0.040(3) 0.070(3) 0.009(2) 0.005(2) -0.014(2) O12 0.045(2) 0.043(2) 0.057(3) -0.014(2) -0.004(2) -0.010(2) C11 0.034(3) 0.040(3) 0.047(3) -0.009(3) 0.012(3) -0.004(3) C12 0.053(5) 0.063(5) 0.085(5) -0.030(4) 0.006(4) -0.013(4) O22 0.060(3) 0.076(3) 0.041(3) 0.003(2) 0.015(2) 0.024(2) O21 0.059(3) 0.083(3) 0.041(3) 0.015(2) 0.013(2) 0.020(3) C21 0.033(3) 0.049(3) 0.047(3) 0.002(3) 0.009(3) 0.002(3) C22 0.086(6) 0.127(7) 0.046(5) -0.003(5) 0.031(4) 0.028(5) C31 0.038(3) 0.049(4) 0.048(4) -0.006(3) 0.011(3) 0.005(3) C32 0.090(6) 0.061(5) 0.083(5) 0.019(4) 0.036(4) 0.027(4) C33 0.122(7) 0.068(6) 0.092(6) 0.026(5) 0.035(5) 0.040(5) C34 0.070(5) 0.064(5) 0.103(6) -0.015(4) 0.025(5) 0.020(4) C35 0.061(5) 0.061(5) 0.092(5) -0.016(4) 0.041(4) -0.002(4) C36 0.061(4) 0.054(4) 0.074(5) -0.001(4) 0.026(4) 0.003(4) C41 0.052(4) 0.045(4) 0.065(4) -0.007(3) -0.007(3) -0.018(3) C42 0.053(4) 0.055(4) 0.061(4) -0.007(4) -0.005(3) -0.020(4) C43 0.038(4) 0.064(4) 0.072(4) -0.006(4) -0.009(3) -0.016(4) C44 0.033(4) 0.055(4) 0.085(5) -0.007(3) 0.007(3) -0.019(3) C45 0.046(4) 0.051(4) 0.070(4) 0.002(3) 0.001(3) -0.022(3) C51 0.032(3) 0.040(3) 0.062(4) -0.004(3) 0.009(3) 0.001(3) C52 0.044(4) 0.066(4) 0.066(4) 0.003(4) 0.006(3) 0.000(3) C53 0.064(5) 0.066(5) 0.100(6) 0.018(4) 0.029(4) -0.009(4) C54 0.046(5) 0.060(5) 0.141(7) -0.008(5) 0.030(5) -0.016(4) C55 0.045(5) 0.081(6) 0.104(6) -0.013(5) -0.001(4) -0.017(4) C56 0.047(4) 0.069(5) 0.067(5) -0.003(4) -0.006(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C3 1.785(7) . ? Co1 C5 1.796(7) . ? Co1 C1 1.960(5) . ? Co1 C2 1.956(5) . ? Co1 As1 2.3115(11) . ? Co1 Mo1 2.7041(11) . ? Mo1 C6 1.997(7) . ? Mo1 C4 2.024(7) . ? Mo1 C1 2.138(5) . ? Mo1 C2 2.140(5) . ? Mo1 C42 2.320(3) . ? Mo1 C43 2.328(2) . ? Mo1 C44 2.357(3) . ? Mo1 C41 2.366(3) . ? Mo1 C45 2.389(3) . ? As1 O1 1.770(4) . ? As1 C31 1.943(3) . ? As1 C51 1.951(3) . ? O3 C3 1.135(7) . ? O4 C4 1.135(7) . ? O5 C5 1.139(7) . ? O6 C6 1.147(7) . ? C1 C2 1.383(7) . ? C1 C11 1.470(7) . ? C2 C21 1.475(7) . ? O11 C11 1.203(7) . ? O12 C11 1.342(6) . ? O12 C12 1.450(7) . ? O22 C21 1.337(7) . ? O22 C22 1.447(8) . ? O21 C21 1.222(7) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.4144 . ? C41 C45 1.4486 . ? C42 C43 1.4316 . ? C43 C44 1.5234 . ? C44 C45 1.4529 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co1 C5 102.7(3) . . ? C3 Co1 C1 139.4(3) . . ? C5 Co1 C1 109.5(3) . . ? C3 Co1 C2 99.0(3) . . ? C5 Co1 C2 145.3(3) . . ? C1 Co1 C2 41.4(2) . . ? C3 Co1 As1 98.9(2) . . ? C5 Co1 As1 99.9(2) . . ? C1 Co1 As1 99.01(15) . . ? C2 Co1 As1 103.10(15) . . ? C3 Co1 Mo1 101.2(2) . . ? C5 Co1 Mo1 97.3(2) . . ? C1 Co1 Mo1 51.62(15) . . ? C2 Co1 Mo1 51.68(15) . . ? As1 Co1 Mo1 149.83(4) . . ? C6 Mo1 C4 86.4(2) . . ? C6 Mo1 C1 80.9(2) . . ? C4 Mo1 C1 78.9(2) . . ? C6 Mo1 C2 89.3(2) . . ? C4 Mo1 C2 116.2(2) . . ? C1 Mo1 C2 37.73(19) . . ? C6 Mo1 C42 118.69(19) . . ? C4 Mo1 C42 87.04(19) . . ? C1 Mo1 C42 155.28(16) . . ? C2 Mo1 C42 145.60(17) . . ? C6 Mo1 C43 84.52(19) . . ? C4 Mo1 C43 95.63(19) . . ? C1 Mo1 C43 164.71(16) . . ? C2 Mo1 C43 147.17(17) . . ? C42 Mo1 C43 35.9 . . ? C6 Mo1 C44 83.30(19) . . ? C4 Mo1 C44 133.11(19) . . ? C1 Mo1 C44 143.08(17) . .. ? C2 Mo1 C44 109.33(17) . . ? C42 Mo1 C44 59.37(6) . . ? C43 Mo1 C44 37.9 . . ? C6 Mo1 C41 141.83(18) . . ? C4 Mo1 C41 111.12(19) . . ? C1 Mo1 C41 134.36(15) . . ? C2 Mo1 C41 110.49(16) . . ? C42 Mo1 C41 35.1 . . ? C43 Mo1 C41 60.93(6) . . ? C44 Mo1 C41 59.73(6) . . ? C6 Mo1 C45 115.01(19) . . ? C4 Mo1 C45 144.76(19) . . ? C1 Mo1 C45 129.76(15) . . ? C2 Mo1 C45 92.86(16) . . ? C42 Mo1 C45 58.45(6) . . ? C43 Mo1 C45 61.40(6) . . ? C44 Mo1 C45 35.6 . . ? C41 Mo1 C45 35.5 . . ? C6 Mo1 Co1 126.25(17) . . ? C4 Mo1 Co1 89.78(17) . . ? C1 Mo1 Co1 45.93(14) . . ? C2 Mo1 Co1 45.82(14) . . ? C42 Mo1 Co1 114.60(8) . . ? C43 Mo1 Co1 149.10(9) . . ? C44 Mo1 Co1 132.16(9) . . ? C41 Mo1 Co1 88.73(6) . . ? C45 Mo1 Co1 97.91(6) . . ? O1 As1 C31 97.83(17) . . ? O1 As1 C51 100.24(19) . . ? C31 As1 C51 99.25(15) . . ? O1 As1 Co1 115.18(14) . . ? C31 As1 Co1 118.82(7) . . ? C51 As1 Co1 121.37(13) . . ? O3 C3 Co1 178.4(7) . . ? O4 C4 Mo1 178.8(6) . . ? O5 C5 Co1 177.3(6) . . ? O6 C6 Mo1 178.8(6) . . ? C2 C1 C11 134.2(5) . . ? C2 C1 Co1 69.2(3) . . ? C11 C1 Co1 132.2(4) . . ? C2 C1 Mo1 71.2(3) . . ? C11 C1 Mo1 139.3(4) . . ? Co1 C1 Mo1 82.45(19) . . ? C1 C2 C21 129.7(5) . . ? C1 C2 Co1 69.5(3) . . ? C21 C2 Co1 137.4(4) . . ? C1 C2 Mo1 71.1(3) . . ? C21 C2 Mo1 136.8(4) . . ? Co1 C2 Mo1 82.50(19) . . ? C11 O12 C12 116.6(5) . . ? O11 C11 O12 123.6(5) . . ? O11 C11 C1 125.7(5) . . ? O12 C11 C1 110.7(5) . . ? C21 O22 C22 116.6(5) . . ? O21 C21 O22 122.6(5) . . ? O21 C21 C2 125.3(5) . . ? O22 C21 C2 112.1(5) . . ? C32 C31 C36 120.0 . . ? C32 C31 As1 120.10(14) . . ? C36 C31 As1 119.89(14) . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C45 106.9 . . ? C42 C41 Mo1 70.67(8) . . ? C45 C41 Mo1 73.11(10) . . ? C41 C42 C43 113.5 . . ? C41 C42 Mo1 74.22(7) . . ? C43 C42 Mo1 72.35(7) . . ? C42 C43 C44 103.2 . . ? C42 C43 Mo1 71.78(8) . . ? C44 C43 Mo1 72.06(10) . . ? C45 C44 C43 108.0 . . ? C45 C44 Mo1 73.37(6) . . ? C43 C44 Mo1 69.99(9) . . ? C41 C45 C44 108.3 . . ? C41 C45 Mo1 71.42(10) . . ? C44 C45 Mo1 70.98(6) . . ? C52 C51 C56 120.0 . . ? C52 C51 As1 119.8(2) . . ? C56 C51 As1 120.2(2) . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.618 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.104 data_ab105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 As2 Cl0 Co3 O8' _chemical_formula_weight 874.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0810(17) _cell_length_b 12.489(2) _cell_length_c 13.650(3) _cell_angle_alpha 68.551(18) _cell_angle_beta 70.462(13) _cell_angle_gamma 64.379(12) _cell_volume 1689.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 3.447 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 0.7094 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens P4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 11808 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5904 _reflns_number_gt 4394 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5904 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.28068(5) 0.63939(5) 0.15683(4) 0.03404(14) Uani 1 1 d . . . Co2 Co 0.07698(5) 0.62741(5) 0.27506(4) 0.03560(14) Uani 1 1 d . . . Co3 Co 0.16932(6) 0.53601(5) 0.12043(5) 0.04483(16) Uani 1 1 d . . . As1 As 0.27102(4) 0.80277(4) 0.20250(3) 0.03499(11) Uani 1 1 d . . . As2 As 0.01940(4) 0.79100(3) 0.34247(3) 0.03383(11) Uani 1 1 d . . . O1 O 0.1145(2) 0.8849(2) 0.2669(2) 0.0379(6) Uani 1 1 d . . . C1 C 0.1190(4) 0.7043(4) 0.1256(3) 0.0369(9) Uani 1 1 d . . . C2 C 0.0483(4) 0.8215(4) 0.0541(3) 0.0528(12) Uani 1 1 d . . . H2A H 0.0309 0.8897 0.0807 0.079 Uiso 1 1 calc R . . H2B H -0.0293 0.8177 0.0538 0.079 Uiso 1 1 calc R . . H2C H 0.0980 0.8320 -0.0178 0.079 Uiso 1 1 calc R . . O3 O 0.4554(3) 0.6678(3) -0.0508(3) 0.0699(10) Uani 1 1 d . . . C3 C 0.3864(4) 0.6583(4) 0.0299(3) 0.0449(10) Uani 1 1 d . . . O4 O -0.1810(3) 0.6554(3) 0.2929(3) 0.0759(11) Uani 1 1 d . . . C4 C -0.0799(5) 0.6429(4) 0.2881(4) 0.0492(11) Uani 1 1 d . . . O5 O 0.4454(4) 0.4187(3) 0.2860(3) 0.0791(11) Uani 1 1 d . . . C5 C 0.3822(4) 0.5072(4) 0.2375(4) 0.0470(11) Uani 1 1 d . . . O6 O 0.1673(4) 0.4067(3) 0.4473(3) 0.0789(11) Uani 1 1 d . . . C6 C 0.1322(4) 0.4939(4) 0.3828(3) 0.0490(11) Uani 1 1 d . . . O7 O -0.0679(4) 0.5489(5) 0.0963(4) 0.1131(18) Uani 1 1 d . . . C7 C 0.0248(5) 0.5418(6) 0.1059(4) 0.0721(16) Uani 1 1 d . . . O8 O 0.2877(4) 0.2794(3) 0.2437(3) 0.0916(13) Uani 1 1 d . . . C8 C 0.2417(5) 0.3777(5) 0.1954(4) 0.0607(13) Uani 1 1 d . . . O9 O 0.3034(4) 0.5329(4) -0.1014(3) 0.0944(14) Uani 1 1 d . . . C9 C 0.2525(5) 0.5355(5) -0.0155(4) 0.0574(13) Uani 1 1 d . . . C31 C 0.3011(3) 0.9459(2) 0.09419(19) 0.0414(10) Uani 1 1 d G . . C32 C 0.2879(3) 0.9679(3) -0.0095(2) 0.0538(12) Uani 1 1 d G . . H32 H 0.2682 0.9133 -0.0261 0.065 Uiso 1 1 calc R . . C33 C 0.3042(3) 1.0716(3) -0.08824(18) 0.0658(14) Uani 1 1 d G . . H33 H 0.2953 1.0863 -0.1576 0.079 Uiso 1 1 calc R . . C34 C 0.3337(3) 1.1533(2) -0.0634(2) 0.0692(15) Uani 1 1 d G . . H34 H 0.3446 1.2227 -0.1161 0.083 Uiso 1 1 calc R . . C35 C 0.3469(3) 1.1313(3) 0.0403(3) 0.0806(18) Uani 1 1 d G . . H35 H 0.3666 1.1860 0.0570 0.097 Uiso 1 1 calc R . . C36 C 0.3306(3) 1.0276(3) 0.1191(2) 0.0665(14) Uani 1 1 d G . . H36 H 0.3394 1.0129 0.1884 0.080 Uiso 1 1 calc R . . C41 C -0.14349(18) 0.9202(2) 0.3289(2) 0.0359(9) Uani 1 1 d G . . C42 C -0.1527(2) 1.0366(2) 0.2606(2) 0.0461(11) Uani 1 1 d G . . H42 H -0.0804 1.0551 0.2238 0.055 Uiso 1 1 calc R . . C43 C -0.2698(3) 1.12511(19) 0.2471(2) 0.0572(12) Uani 1 1 d G . . H43 H -0.2760 1.2029 0.2014 0.069 Uiso 1 1 calc R . . C44 C -0.3779(2) 1.0973(2) 0.3021(2) 0.0603(14) Uani 1 1 d G . . H44 H -0.4563 1.1566 0.2931 0.072 Uiso 1 1 calc R . . C45 C -0.36868(19) 0.9810(3) 0.3704(2) 0.0567(12) Uani 1 1 d G . . H45 H -0.4409 0.9624 0.4072 0.068 Uiso 1 1 calc R . . C46 C -0.2515(2) 0.8925(2) 0.3839(2) 0.0477(11) Uani 1 1 d G . . H46 H -0.2454 0.8146 0.4296 0.057 Uiso 1 1 calc R . . C51 C 0.3597(3) 0.7727(3) 0.3108(2) 0.0439(10) Uani 1 1 d G . . C52 C 0.4749(3) 0.6774(3) 0.3170(3) 0.0606(13) Uani 1 1 d G . . H52 H 0.5109 0.6299 0.2678 0.073 Uiso 1 1 calc R . . C53 C 0.5363(3) 0.6532(3) 0.3968(3) 0.0823(18) Uani 1 1 d G . . H53 H 0.6133 0.5895 0.4010 0.099 Uiso 1 1 calc R . . C54 C 0.4825(4) 0.7242(4) 0.4703(3) 0.090(2) Uani 1 1 d G . . H54 H 0.5235 0.7079 0.5237 0.108 Uiso 1 1 calc R . . C55 C 0.3673(4) 0.8194(4) 0.4641(2) 0.0882(19) Uani 1 1 d G . . H55 H 0.3313 0.8669 0.5133 0.106 Uiso 1 1 calc R . . C56 C 0.3059(3) 0.8436(3) 0.3843(3) 0.0670(15) Uani 1 1 d G . . H56 H 0.2288 0.9074 0.3802 0.080 Uiso 1 1 calc R . . C61 C 0.0297(3) 0.7700(3) 0.48816(18) 0.0400(10) Uani 1 1 d G . . C62 C 0.1209(3) 0.6659(2) 0.5345(2) 0.0681(16) Uani 1 1 d G . . H62 H 0.1724 0.6059 0.4976 0.082 Uiso 1 1 calc R . . C63 C 0.1353(3) 0.6515(2) 0.6360(2) 0.0815(19) Uani 1 1 d G . . H63 H 0.1964 0.5819 0.6670 0.098 Uiso 1 1 calc R . . C64 C 0.0583(4) 0.7412(3) 0.6911(2) 0.0710(16) Uani 1 1 d G . . H64 H 0.0679 0.7315 0.7590 0.085 Uiso 1 1 calc R . . C65 C -0.0329(3) 0.8453(3) 0.6447(2) 0.094(2) Uani 1 1 d G . . H65 H -0.0844 0.9052 0.6816 0.113 Uiso 1 1 calc R . . C66 C -0.0473(3) 0.8597(2) 0.5433(2) 0.0718(16) Uani 1 1 d G . . H66 H -0.1084 0.9293 0.5122 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0329(3) 0.0337(3) 0.0317(3) -0.0104(2) -0.0073(2) -0.0065(2) Co2 0.0392(3) 0.0322(3) 0.0312(3) -0.0091(2) -0.0036(2) -0.0110(2) Co3 0.0475(4) 0.0512(4) 0.0424(3) -0.0228(3) -0.0050(3) -0.0179(3) As1 0.0336(2) 0.0354(2) 0.0342(2) -0.01023(18) -0.00767(17) -0.00928(18) As2 0.0344(2) 0.0301(2) 0.0315(2) -0.00906(17) -0.00636(17) -0.00610(17) O1 0.0345(15) 0.0353(15) 0.0398(15) -0.0101(12) -0.0052(12) -0.0105(12) C1 0.032(2) 0.045(2) 0.031(2) -0.0091(18) -0.0060(17) -0.0126(18) C2 0.044(3) 0.062(3) 0.043(3) 0.000(2) -0.015(2) -0.016(2) O3 0.058(2) 0.087(3) 0.046(2) -0.0183(18) 0.0096(17) -0.0225(19) C3 0.042(3) 0.049(3) 0.040(3) -0.014(2) -0.011(2) -0.008(2) O4 0.051(2) 0.091(3) 0.099(3) -0.043(2) -0.002(2) -0.031(2) C4 0.052(3) 0.051(3) 0.048(3) -0.017(2) -0.001(2) -0.024(2) O5 0.080(3) 0.055(2) 0.083(3) 0.004(2) -0.044(2) -0.004(2) C5 0.051(3) 0.043(3) 0.047(3) -0.011(2) -0.013(2) -0.014(2) O6 0.108(3) 0.048(2) 0.050(2) 0.0079(17) -0.018(2) -0.017(2) C6 0.062(3) 0.039(3) 0.039(2) -0.012(2) 0.000(2) -0.017(2) O7 0.071(3) 0.205(5) 0.116(4) -0.100(4) -0.004(3) -0.059(3) C7 0.069(4) 0.114(5) 0.061(3) -0.054(3) 0.001(3) -0.043(4) O8 0.118(4) 0.049(2) 0.096(3) -0.016(2) -0.027(3) -0.019(2) C8 0.071(4) 0.057(3) 0.059(3) -0.027(3) -0.004(3) -0.025(3) O9 0.100(3) 0.144(4) 0.056(2) -0.049(3) 0.014(2) -0.062(3) C9 0.063(3) 0.069(3) 0.053(3) -0.027(3) -0.010(3) -0.028(3) C31 0.035(2) 0.042(2) 0.044(2) -0.0107(19) -0.0049(19) -0.0145(19) C32 0.058(3) 0.052(3) 0.050(3) -0.006(2) -0.016(2) -0.021(2) C33 0.073(4) 0.062(3) 0.050(3) 0.004(3) -0.015(3) -0.027(3) C34 0.074(4) 0.057(3) 0.062(3) 0.004(3) -0.003(3) -0.034(3) C35 0.108(5) 0.063(4) 0.079(4) -0.022(3) 0.006(4) -0.053(3) C36 0.092(4) 0.063(3) 0.052(3) -0.020(3) -0.002(3) -0.040(3) C41 0.034(2) 0.034(2) 0.036(2) -0.0112(18) -0.0098(18) -0.0053(18) C42 0.043(3) 0.042(2) 0.047(3) -0.007(2) -0.013(2) -0.011(2) C43 0.058(3) 0.045(3) 0.056(3) -0.004(2) -0.023(2) -0.006(2) C44 0.048(3) 0.058(3) 0.069(3) -0.027(3) -0.029(3) 0.007(2) C45 0.035(3) 0.060(3) 0.071(3) -0.026(3) -0.006(2) -0.009(2) C46 0.042(3) 0.039(2) 0.052(3) -0.010(2) -0.006(2) -0.008(2) C51 0.043(3) 0.052(3) 0.040(2) -0.008(2) -0.014(2) -0.019(2) C52 0.047(3) 0.062(3) 0.069(3) -0.009(3) -0.019(3) -0.017(2) C53 0.059(4) 0.082(4) 0.099(5) 0.007(4) -0.045(3) -0.023(3) C54 0.110(5) 0.116(5) 0.071(4) 0.007(4) -0.053(4) -0.064(5) C55 0.103(5) 0.124(6) 0.069(4) -0.028(4) -0.031(4) -0.057(5) C56 0.063(3) 0.090(4) 0.061(3) -0.036(3) -0.024(3) -0.018(3) C61 0.047(2) 0.038(2) 0.033(2) -0.0085(18) -0.0067(19) -0.016(2) C62 0.092(4) 0.043(3) 0.062(3) -0.020(2) -0.041(3) 0.006(3) C63 0.127(5) 0.050(3) 0.074(4) -0.012(3) -0.064(4) -0.008(3) C64 0.113(5) 0.066(3) 0.047(3) -0.018(3) -0.027(3) -0.033(3) C65 0.108(5) 0.091(4) 0.072(4) -0.054(3) -0.040(4) 0.018(4) C66 0.082(4) 0.064(3) 0.057(3) -0.032(3) -0.028(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C3 1.780(4) . ? Co1 C5 1.807(5) . ? Co1 C1 1.895(4) . ? Co1 As1 2.2895(8) . ? Co1 Co3 2.4784(8) . ? Co1 Co2 2.4836(9) . ? Co2 C4 1.773(5) . ? Co2 C6 1.814(5) . ? Co2 C1 1.908(4) . ? Co2 As2 2.2853(8) . ? Co2 Co3 2.4675(9) . ? Co3 C7 1.789(6) . ? Co3 C9 1.792(5) . ? Co3 C8 1.828(6) . ? Co3 C1 1.941(4) . ? As1 O1 1.808(3) . ? As1 C31 1.945(2) . ? As1 C51 1.944(2) . ? As2 O1 1.802(3) . ? As2 C41 1.9467(19) . ? As2 C61 1.948(2) . ? C1 C2 1.502(5) . ? O3 C3 1.139(5) . ? O4 C4 1.144(5) . ? O5 C5 1.147(5) . ? O6 C6 1.136(5) . ? O7 C7 1.133(6) . ? O8 C8 1.147(6) . ? O9 C9 1.132(5) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co1 C5 101.1(2) . . ? C3 Co1 C1 105.79(18) . . ? C5 Co1 C1 141.79(19) . . ? C3 Co1 As1 97.56(14) . . ? C5 Co1 As1 104.01(14) . . ? C1 Co1 As1 98.90(12) . . ? C3 Co1 Co3 98.75(14) . . ? C5 Co1 Co3 99.12(14) . . ? C1 Co1 Co3 50.58(12) . . ? As1 Co1 Co3 148.45(3) . . ? C3 Co1 Co2 153.56(14) . . ? C5 Co1 Co2 97.62(15) . . ? C1 Co1 Co2 49.44(11) . . ? As1 Co1 Co2 95.87(3) . . ? Co3 Co1 Co2 59.64(3) . . ? C4 Co2 C6 104.4(2) . . ? C4 Co2 C1 100.94(19) . . ? C6 Co2 C1 143.96(18) . . ? C4 Co2 As2 94.00(14) . . ? C6 Co2 As2 104.34(13) . . ? C1 Co2 As2 98.95(12) . . ? C4 Co2 Co3 96.57(14) . . ? C6 Co2 Co3 100.80(13) . . ? C1 Co2 Co3 50.73(12) . . ? As2 Co2 Co3 149.29(3) . . ? C4 Co2 Co1 148.99(15) . . ? C6 Co2 Co1 100.20(15) . . ? C1 Co2 Co1 49.00(12) . . ? As2 Co2 Co1 97.95(3) . . ? Co3 Co2 Co1 60.07(2) . . ? C7 Co3 C9 96.9(2) . . ? C7 Co3 C8 104.8(3) . . ? C9 Co3 C8 102.8(2) . . ? C7 Co3 C1 99.2(2) . . ? C9 Co3 C1 104.42(19) . . ? C8 Co3 C1 140.86(19) . . ? C7 Co3 Co2 96.10(15) . . ? C9 Co3 Co2 152.59(16) . . ? C8 Co3 Co2 97.01(15) . . ? C1 Co3 Co2 49.53(11) . . ? C7 Co3 Co1 147.59(18) . . ? C9 Co3 Co1 97.33(15) . . ? C8 Co3 Co1 100.18(16) . . ? C1 Co3 Co1 48.94(11) . . ? Co2 Co3 Co1 60.28(2) . . ? O1 As1 C31 96.40(12) . . ? O1 As1 C51 98.44(12) . . ? C31 As1 C51 103.45(12) . . ? O1 As1 Co1 112.76(9) . . ? C31 As1 Co1 121.89(9) . . ? C51 As1 Co1 119.28(9) . . ? O1 As2 C41 97.43(11) . . ? O1 As2 C61 100.02(13) . . ? C41 As2 C61 102.94(11) . . ? O1 As2 Co2 111.76(8) . . ? C41 As2 Co2 118.39(8) . . ? C61 As2 Co2 122.16(8) . . ? As2 O1 As1 114.40(13) . . ? C2 C1 Co1 134.0(3) . . ? C2 C1 Co2 131.9(3) . . ? Co1 C1 Co2 81.56(15) . . ? C2 C1 Co3 128.9(3) . . ? Co1 C1 Co3 80.49(15) . . ? Co2 C1 Co3 79.75(15) . . ? O3 C3 Co1 178.5(4) . . ? O4 C4 Co2 177.6(5) . . ? O5 C5 Co1 175.6(4) . . ? O6 C6 Co2 176.6(4) . . ? O7 C7 Co3 178.1(6) . . ? O8 C8 Co3 178.5(5) . . ? O9 C9 Co3 177.9(5) . . ? C32 C31 C36 120.0 . . ? C32 C31 As1 118.21(16) . . ? C36 C31 As1 121.75(16) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 As2 121.01(14) . . ? C46 C41 As2 118.88(14) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 As1 119.98(17) . . ? C56 C51 As1 119.98(17) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 As2 118.57(15) . . ? C66 C61 As2 121.33(15) . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C65 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.332 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.090