Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #=============================================================================== _audit_creation_date 27-01-00 _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof P Braunstein' _publ_contact_author_address ; Prof P Braunstein Laboratoire de Chimie de Coordn. UMR 7513 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg cedex 67070 FRANCE ; _publ_requested_journal 'Dalton Trans.' _publ_contact_letter ; ? ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ;2-Boratanaphthalene Ligands in Heterometallic Complexes and Clusters ; # 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 'Pierre Braunstein' ;Laboratoire de Chimie de Coordination CNRS UMR 7513 4, rue Blaise Pascal 67070 Strasbourg Cedex France ; 'Elisabeth Cura' ;Laboratoire de Chimie de Coordination CNRS UMR 7513 4, rue Blaise Pascal 67070 Strasbourg Cedex France ; 'Gerhard E. Herberich' ;Institut fur Anorganische Chemie der Rheinisch-Westfalischen Technischen Hochschule Professor-Pirlet-Strasse 1 D-52056 Aachen Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st536 _database_code_CSD 153364 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C37 H38 Au B Mo N O3 P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C37 H38 Au B Mo N O3 P' _chemical_formula_weight 879.41 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Au ? -2.688 8.798 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 17.8519(8) _cell_length_b 10.3946(6) _cell_length_c 19.1659(8) _cell_angle_alpha 90 _cell_angle_beta 100.148(8) _cell_angle_gamma 90 _cell_volume 3500.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 8427 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 4.625 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 8427 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.8 deg 1 scans of 40 sec per frame. Data collection was divided into 4 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 101 frames Set 2 Theta = -1.10 Kappa = -130.00 Phi = 0.00 21 frames Set 3 Theta = -5.50 Kappa = -169.00 Phi = 0.00 23 frames Set 4 Theta = -6.40 Kappa = -86.00 Phi = 0.00 26 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8427 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8427 _reflns_number_gt 6860 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6860 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.030 _refine_ls_R_factor_gt 0.022 _refine_ls_wR_factor_all 6.000 _refine_ls_wR_factor_ref 0.031 _refine_ls_goodness_of_fit_all 9.870 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_shift/su_max 0.030 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.611 _refine_diff_density_min -0.143 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol AU 0.69087(1) -0.04606(1) 0.59237(1) 0.02602(5) Uani ? ? Au MO 0.79496(1) -0.20922(2) 0.55224(1) 0.01906(9) Uani ? ? Mo P 0.61215(4) 0.06595(6) 0.65149(4) 0.0245(3) Uani ? ? P C1 0.6001(1) 0.2369(3) 0.6334(1) 0.026(1) Uani ? ? C C2 0.5983(1) 0.2793(3) 0.5639(1) 0.030(1) Uani ? ? C C3 0.5828(2) 0.4074(3) 0.5468(2) 0.037(1) Uani ? ? C C4 0.5706(1) 0.4947(3) 0.5986(2) 0.035(1) Uani ? ? C C5 0.5746(2) 0.4543(2) 0.6674(2) 0.038(2) Uani ? ? C C6 0.5891(1) 0.3256(3) 0.6851(1) 0.033(1) Uani ? ? C C7 0.5154(1) 0.0018(3) 0.6368(1) 0.028(1) Uani ? ? C C8 0.5044(2) -0.1308(3) 0.6284(2) 0.043(2) Uani ? ? C C9 0.4325(2) -0.1846(3) 0.6202(2) 0.048(2) Uani ? ? C C10 0.3706(2) -0.1054(4) 0.6181(2) 0.050(2) Uani ? ? C C11 0.3796(2) 0.0252(4) 0.6255(2) 0.056(2) Uani ? ? C C12 0.4517(2) 0.0813(3) 0.6359(2) 0.044(2) Uani ? ? C C13 0.6458(1) 0.0532(2) 0.7468(1) 0.027(1) Uani ? ? C C14 0.7142(1) 0.1128(3) 0.7761(1) 0.038(2) Uani ? ? C C15 0.7434(2) 0.0988(3) 0.8483(2) 0.044(2) Uani ? ? C C16 0.7052(2) 0.0249(3) 0.8906(2) 0.039(2) Uani ? ? C C17 0.6376(2) -0.0341(3) 0.8618(2) 0.039(2) Uani ? ? C C18 0.6086(1) -0.0206(3) 0.7904(1) 0.032(1) Uani ? ? C C19 0.6854(1) -0.2480(2) 0.5223(1) 0.022(1) Uani ? ? C O1 0.62365(9) -0.2839(2) 0.5001(1) 0.0318(9) Uani ? ? O C20 0.7942(1) -0.2354(3) 0.4499(1) 0.027(1) Uani ? ? C O2 0.7933(1) -0.2477(2) 0.3899(1) 0.042(1) Uani ? ? O C21 0.8050(1) -0.0267(2) 0.5249(1) 0.027(1) Uani ? ? C O3 0.8163(1) 0.0764(2) 0.5056(1) 0.041(1) Uani ? ? O C22 0.8242(1) -0.4047(2) 0.6220(1) 0.024(1) Uani ? ? C C23 0.8837(1) -0.3830(2) 0.5810(1) 0.025(1) Uani ? ? C C24 0.9256(1) -0.2645(3) 0.5862(1) 0.026(1) Uani ? ? C B 0.9221(1) -0.1669(3) 0.6459(2) 0.026(1) Uani ? ? B C25 0.8493(1) -0.1913(2) 0.6791(1) 0.025(1) Uani ? ? C C26 0.8055(1) -0.3039(3) 0.6689(1) 0.025(1) Uani ? ? C C27 0.7401(1) -0.3230(3) 0.7089(1) 0.033(1) Uani ? ? C C28 0.8982(1) -0.4838(3) 0.5333(1) 0.032(1) Uani ? ? C C29 0.8615(2) -0.6009(3) 0.5320(2) 0.037(1) Uani ? ? C C30 0.8056(2) -0.6230(3) 0.5742(2) 0.036(1) Uani ? ? C C31 0.7859(1) -0.5278(2) 0.6165(2) 0.030(1) Uani ? ? C N 0.9743(1) -0.0643(2) 0.6652(1) 0.032(1) Uani ? ? N C32 1.0363(2) -0.0371(3) 0.6250(2) 0.038(2) Uani ? ? C C33 1.0280(2) 0.0912(4) 0.5874(2) 0.054(2) Uani ? ? C C34 1.1156(2) -0.0503(3) 0.6707(2) 0.057(2) Uani ? ? C C35 0.9693(2) 0.0282(3) 0.7234(2) 0.039(2) Uani ? ? C C36 0.9734(2) -0.0371(3) 0.7946(2) 0.051(2) Uani ? ? C C37 0.9015(2) 0.1198(3) 0.7051(2) 0.056(2) Uani ? ? C H1 0.6076 0.2205 0.5285 0.0404 Uiso calc C2 H H2 0.5806 0.4356 0.4993 0.0484 Uiso calc C3 H H3 0.5595 0.5821 0.5864 0.0463 Uiso calc C4 H H4 0.5675 0.5143 0.7031 0.0491 Uiso calc C5 H H5 0.5914 0.2982 0.7327 0.0422 Uiso calc C6 H H6 0.5472 -0.1851 0.6284 0.0557 Uiso calc C8 H H7 0.4261 -0.2751 0.6160 0.0630 Uiso calc C9 H H8 0.3209 -0.1415 0.6115 0.0701 Uiso calc C10 H H9 0.3360 0.0784 0.6236 0.0811 Uiso calc C11 H H10 0.4576 0.1716 0.6422 0.0602 Uiso calc C12 H H11 0.7409 0.1629 0.7470 0.0510 Uiso calc C14 H H12 0.7896 0.1402 0.8683 0.0606 Uiso calc C15 H H13 0.7254 0.0147 0.9395 0.0544 Uiso calc C16 H H14 0.6111 -0.0841 0.8910 0.0532 Uiso calc C17 H H15 0.5623 -0.0625 0.7709 0.0423 Uiso calc C18 H H16 0.9564 -0.2458 0.5518 0.0347 Uiso calc C24 H H17 0.8339 -0.1257 0.7081 0.0341 Uiso calc C25 H H18 0.7354 -0.2491 0.7369 0.0437 Uiso calc C27 H H19 0.6943 -0.3355 0.6760 0.0437 Uiso calc C27 H H20 0.7499 -0.3964 0.7387 0.0437 Uiso calc C27 H H21 0.9334 -0.4694 0.5023 0.0429 Uiso calc C28 H H22 0.8741 -0.6676 0.5023 0.0518 Uiso calc C29 H H23 0.7815 -0.7046 0.5731 0.0508 Uiso calc C30 H H24 0.7464 -0.5426 0.6429 0.0415 Uiso calc C31 H H25 1.0692 0.1031 0.5627 0.0706 Uiso calc C33 H H26 0.9814 0.0929 0.5547 0.0706 Uiso calc C33 H H27 1.0282 0.1581 0.6212 0.0706 Uiso calc C33 H H28 1.1533 -0.0320 0.6427 0.0790 Uiso calc C34 H H29 1.1204 0.0085 0.7092 0.0790 Uiso calc C34 H H30 1.1223 -0.1356 0.6885 0.0790 Uiso calc C34 H H31 0.9700 0.0259 0.8298 0.0699 Uiso calc C36 H H32 0.9324 -0.0961 0.7922 0.0699 Uiso calc C36 H H33 1.0203 -0.0819 0.8063 0.0699 Uiso calc C36 H H34 0.9005 0.1770 0.7436 0.0764 Uiso calc C37 H H35 0.9063 0.1678 0.6639 0.0764 Uiso calc C37 H H36 0.8556 0.0715 0.6965 0.0764 Uiso calc C37 H H37 1.0314 -0.1016 0.5894 0.0510 Uiso calc C32 H H38 1.0135 0.0807 0.7280 0.0508 Uiso calc C35 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol AU 0.02982(5) 0.02481(6) 0.02382(5) 0.00681(4) 0.00581(4) -0.00187(4) Au MO 0.01953(8) 0.0177(1) 0.0200(1) 0.00061(7) 0.00083(7) -0.00089(8) Mo P 0.0271(3) 0.0240(3) 0.0225(3) 0.0042(2) 0.0056(2) -0.0000(3) P C1 0.024(1) 0.027(1) 0.028(1) 0.002(1) 0.0071(9) -0.000(1) C C2 0.036(1) 0.032(1) 0.025(1) 0.003(1) 0.003(1) -0.000(1) C C3 0.041(1) 0.035(1) 0.035(1) 0.000(1) 0.006(1) 0.011(1) C C4 0.034(1) 0.025(1) 0.048(2) 0.004(1) 0.009(1) 0.009(1) C C5 0.041(1) 0.027(2) 0.048(2) -0.001(1) 0.015(1) -0.007(1) C C6 0.040(1) 0.031(1) 0.029(1) 0.002(1) 0.013(1) 0.001(1) C C7 0.032(1) 0.031(1) 0.021(1) -0.002(1) 0.004(1) 0.005(1) C C8 0.048(1) 0.041(2) 0.041(2) -0.006(1) 0.011(1) -0.010(1) C C9 0.058(2) 0.051(2) 0.038(2) -0.020(1) 0.010(1) -0.010(1) C C10 0.044(1) 0.075(2) 0.039(2) -0.023(1) -0.003(1) 0.022(2) C C11 0.029(1) 0.075(2) 0.079(2) 0.002(1) 0.000(2) 0.041(2) C C12 0.035(1) 0.042(2) 0.061(2) 0.005(1) 0.003(1) 0.020(2) C C13 0.030(1) 0.026(1) 0.026(1) 0.007(1) 0.003(1) -0.001(1) C C14 0.033(1) 0.051(2) 0.032(1) -0.003(1) 0.004(1) 0.000(1) C C15 0.037(1) 0.059(2) 0.038(2) 0.001(1) -0.010(1) -0.002(2) C C16 0.049(2) 0.046(2) 0.027(1) 0.016(1) -0.003(1) 0.005(1) C C17 0.054(2) 0.041(2) 0.027(1) 0.007(1) 0.004(1) 0.008(1) C C18 0.037(1) 0.032(1) 0.028(1) 0.003(1) 0.005(1) 0.003(1) C C19 0.028(1) 0.020(1) 0.019(1) 0.002(1) 0.0042(9) -0.000(1) C O1 0.0252(8) 0.036(1) 0.036(1) -0.0065(7) 0.0003(7) -0.0058(8) O C20 0.023(1) 0.027(1) 0.031(1) -0.003(1) 0.003(1) -0.000(1) C O2 0.054(1) 0.052(1) 0.0255(9) -0.011(1) 0.0092(8) -0.0040(9) O C21 0.028(1) 0.029(1) 0.025(1) -0.002(1) 0.004(1) -0.004(1) C O3 0.052(1) 0.0242(9) 0.056(1) -0.0056(9) 0.0171(9) 0.0055(9) O C22 0.024(1) 0.022(1) 0.028(1) 0.002(1) -0.006(1) 0.003(1) C C23 0.023(1) 0.024(1) 0.029(1) 0.006(1) -0.005(1) -0.001(1) C C24 0.020(1) 0.030(1) 0.029(1) 0.001(1) 0.0009(9) 0.001(1) C B 0.023(1) 0.027(1) 0.027(1) -0.001(1) -0.000(1) 0.002(1) B C25 0.026(1) 0.028(1) 0.023(1) -0.001(1) -0.001(1) -0.001(1) C C26 0.025(1) 0.028(1) 0.024(1) -0.001(1) -0.004(1) 0.004(1) C C27 0.035(1) 0.035(1) 0.031(1) -0.005(1) 0.004(1) 0.004(1) C C28 0.028(1) 0.033(1) 0.035(1) 0.010(1) -0.002(1) -0.004(1) C C29 0.040(1) 0.029(1) 0.044(2) 0.011(1) -0.008(1) -0.010(1) C C30 0.043(1) 0.022(1) 0.048(2) 0.002(1) -0.003(1) -0.001(1) C C31 0.029(1) 0.024(1) 0.039(2) -0.002(1) -0.003(1) 0.004(1) C N 0.029(1) 0.034(1) 0.032(1) -0.0080(9) 0.0020(9) -0.004(1) N C32 0.029(1) 0.045(2) 0.043(2) -0.011(1) 0.004(1) -0.004(1) C C33 0.043(2) 0.063(2) 0.057(2) -0.008(2) 0.009(1) 0.018(2) C C34 0.034(2) 0.077(3) 0.071(2) -0.006(1) 0.007(2) 0.018(2) C C35 0.036(1) 0.036(2) 0.045(2) -0.014(1) 0.005(1) -0.014(1) C C36 0.052(2) 0.072(2) 0.035(2) -0.018(1) 0.000(1) -0.016(2) C C37 0.062(2) 0.034(2) 0.084(2) -0.008(1) 0.023(2) -0.014(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag AU MO 2.7248(2) . . ? AU P 2.2750(7) . . ? AU C19 2.485(3) . . ? AU C21 2.607(3) . . ? MO C19 1.980(2) . . ? MO C20 1.979(3) . . ? MO C21 1.984(3) . . ? MO C22 2.438(3) . . ? MO C23 2.403(2) . . ? MO C24 2.379(2) . . ? MO B 2.670(3) . . ? MO C25 2.462(2) . . ? MO C26 2.419(3) . . ? MO C19 1.980(2) . . ? MO C20 1.979(3) . . ? MO C21 1.984(3) . . ? P C1 1.816(3) . . ? P C7 1.827(3) . . ? P C13 1.824(3) . . ? C1 C2 1.397(4) . . ? C1 C6 1.392(4) . . ? C2 C3 1.387(4) . . ? C3 C4 1.391(5) . . ? C4 C5 1.375(5) . . ? C5 C6 1.392(4) . . ? C7 C8 1.398(4) . . ? C7 C12 1.402(4) . . ? C8 C9 1.383(4) . . ? C9 C10 1.374(5) . . ? C10 C11 1.371(6) . . ? C11 C12 1.396(5) . . ? C13 C14 1.396(4) . . ? C13 C18 1.388(4) . . ? C14 C15 1.397(4) . . ? C15 C16 1.381(5) . . ? C16 C17 1.378(5) . . ? C17 C18 1.381(4) . . ? C19 O1 1.171(3) . . ? C20 O2 1.153(3) . . ? C21 O3 1.163(3) . . ? C22 C23 1.447(4) . . ? C22 C26 1.456(4) . . ? C22 C31 1.445(4) . . ? C23 C24 1.435(4) . . ? C23 C28 1.444(4) . . ? C24 B 1.538(4) . . ? B C25 1.566(4) . . ? B N 1.422(4) . . ? C25 C26 1.402(4) . . ? C26 C27 1.518(4) . . ? C28 C29 1.380(5) . . ? C29 C30 1.409(5) . . ? C30 C31 1.364(4) . . ? N C32 1.483(4) . . ? N C35 1.487(4) . . ? C32 C33 1.510(5) . . ? C32 C34 1.534(5) . . ? C35 C36 1.514(5) . . ? C35 C37 1.531(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MO AU P 166.16(2) . . . ? MO AU C19 44.38(5) . . . ? MO AU C21 43.63(6) . . . ? P AU C19 137.12(6) . . . ? P AU C21 144.41(6) . . . ? C19 AU C21 75.90(8) . . . ? AU MO C19 61.36(7) . . . ? AU MO C20 118.67(7) . . . ? AU MO C21 65.02(8) . . . ? AU MO C22 117.04(6) . . . ? AU MO C23 149.14(7) . . . ? AU MO C24 139.25(7) . . . ? AU MO B 104.43(7) . . . ? AU MO C25 81.02(6) . . . ? AU MO C26 86.47(6) . . . ? C19 MO C20 81.4(1) . . . ? C19 MO C21 104.4(1) . . . ? C19 MO C22 95.40(9) . . . ? C19 MO C23 119.4(1) . . . ? C19 MO C24 154.3(1) . . . ? C19 MO B 155.2(1) . . . ? C19 MO C25 119.94(9) . . . ? C19 MO C26 95.58(9) . . . ? C20 MO C21 81.6(1) . . . ? C20 MO C22 113.1(1) . . . ? C20 MO C23 90.7(1) . . . ? C20 MO C24 94.21(9) . . . ? C20 MO B 123.05(9) . . . ? C20 MO C25 157.33(9) . . . ? C20 MO C26 147.8(1) . . . ? C21 MO C22 157.1(1) . . . ? C21 MO C23 133.8(1) . . . ? C21 MO C24 100.0(1) . . . ? C21 MO B 85.1(1) . . . ? C21 MO C25 98.6(1) . . . ? C21 MO C26 129.6(1) . . . ? C22 MO C23 34.78(9) . . . ? C22 MO C24 62.86(8) . . . ? C22 MO B 72.20(9) . . . ? C22 MO C25 60.81(9) . . . ? C22 MO C26 34.89(9) . . . ? C23 MO C24 34.94(9) . . . ? C23 MO B 61.40(9) . . . ? C23 MO C25 72.60(9) . . . ? C23 MO C26 62.68(9) . . . ? C24 MO B 34.85(9) . . . ? C24 MO C25 63.31(9) . . . ? C24 MO C26 74.66(9) . . . ? B MO C25 35.23(9) . . . ? B MO C26 61.80(9) . . . ? C25 MO C26 33.38(8) . . . ? C19 MO C20 81.4(1) . . . ? C19 MO C21 104.4(1) . . . ? C20 MO C21 81.6(1) . . . ? C1 P C7 104.5(1) . . . ? C1 P C13 105.6(1) . . . ? C7 P C13 105.3(1) . . . ? P C1 C2 118.2(2) . . . ? P C1 C6 122.6(2) . . . ? C2 C1 C6 119.1(3) . . . ? C1 C2 C3 119.9(3) . . . ? C2 C3 C4 120.4(3) . . . ? C3 C4 C5 119.9(3) . . . ? C4 C5 C6 120.2(3) . . . ? C1 C6 C5 120.4(3) . . . ? P C7 C8 119.1(2) . . . ? P C7 C12 122.0(2) . . . ? C8 C7 C12 118.9(3) . . . ? C7 C8 C9 121.3(3) . . . ? C8 C9 C10 119.2(3) . . . ? C9 C10 C11 120.7(3) . . . ? C10 C11 C12 121.1(3) . . . ? C7 C12 C11 118.7(3) . . . ? P C13 C14 118.8(2) . . . ? P C13 C18 122.4(2) . . . ? C14 C13 C18 118.7(3) . . . ? C13 C14 C15 119.9(3) . . . ? C14 C15 C16 120.2(3) . . . ? C15 C16 C17 119.9(3) . . . ? C16 C17 C18 120.1(3) . . . ? C13 C18 C17 121.1(3) . . . ? MO C19 O1 171.5(2) . . . ? MO C20 O2 178.4(2) . . . ? MO C21 O3 173.6(2) . . . ? C23 C22 C26 119.5(2) . . . ? C23 C22 C31 118.8(3) . . . ? C26 C22 C31 121.7(2) . . . ? C22 C23 C24 121.3(2) . . . ? C22 C23 C28 117.5(2) . . . ? C24 C23 C28 121.2(3) . . . ? C23 C24 B 122.0(2) . . . ? C24 B C25 109.9(2) . . . ? C24 B N 125.4(2) . . . ? C25 B N 124.6(3) . . . ? B C25 C26 124.1(2) . . . ? C22 C26 C25 120.3(2) . . . ? C22 C26 C27 119.8(2) . . . ? C25 C26 C27 119.9(2) . . . ? C23 C28 C29 120.9(3) . . . ? C28 C29 C30 121.0(3) . . . ? C29 C30 C31 120.3(3) . . . ? C22 C31 C30 121.2(3) . . . ? B N C32 121.5(2) . . . ? B N C35 123.9(2) . . . ? C32 N C35 114.5(2) . . . ? N C32 C33 113.3(2) . . . ? N C32 C34 112.6(3) . . . ? C33 C32 C34 110.8(2) . . . ? N C35 C36 112.7(3) . . . ? N C35 C37 112.3(3) . . . ? C36 C35 C37 113.3(3) . . . ? data_st544 _database_code_CSD 153365 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H54 B2 Mo2 O6 P2 Pd2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H54 B2 Mo2 O6 P2 Pd2' _chemical_formula_weight 1119.12 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.8882(4) _cell_length_b 20.8012(8) _cell_length_c 11.9776(6) _cell_angle_alpha 90 _cell_angle_beta 103.372(5) _cell_angle_gamma 90 _cell_volume 2154.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description needle _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.73 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 8976 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.4 deg 1 scans of 150 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 129 frames Set 2 Theta = -6.40 Kappa = 0.00 Phi = 0.00 20 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8976 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5077 _reflns_number_gt 3678 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3678 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_all 0.677 _refine_ls_wR_factor_ref 0.043 _refine_ls_goodness_of_fit_all 9.99 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_shift/su_max 0.010 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.621 _refine_diff_density_min -0.266 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol MO 0.61344(3) 0.10486(1) 1.09233(2) 0.0218(1) Uani ? ? Mo PD 0.43554(3) 0.02969(1) 0.90578(2) 0.0211(1) Uani ? ? Pd P 0.3191(1) 0.07815(5) 0.72889(8) 0.0270(5) Uani ? ? P C1 0.1255(5) 0.1111(2) 0.7197(4) 0.040(2) Uani ? ? C C2 0.0173(5) 0.0642(2) 0.7563(5) 0.054(3) Uani ? ? C C3 0.4283(5) 0.1468(2) 0.6927(3) 0.039(2) Uani ? ? C C4 0.5924(5) 0.1289(2) 0.6886(4) 0.055(3) Uani ? ? C C5 0.2956(5) 0.0252(2) 0.6041(3) 0.039(2) Uani ? ? C C6 0.2258(7) 0.0546(2) 0.4858(4) 0.057(3) Uani ? ? C C7 0.7087(4) 0.0372(1) 1.0027(3) 0.026(2) Uani ? ? C O1 0.7983(3) 0.0134(1) 0.9579(2) 0.035(1) Uani ? ? O C8 0.5121(4) -0.0632(2) 0.8123(3) 0.029(2) Uani ? ? C O2 0.5936(3) -0.0510(1) 0.7499(2) 0.039(1) Uani ? ? O C9 0.4075(4) 0.1291(2) 0.9951(3) 0.030(2) Uani ? ? C O3 0.2908(3) 0.1578(1) 0.9646(2) 0.046(2) Uani ? ? O C10 0.8246(4) 0.1325(2) 1.2507(3) 0.029(2) Uani ? ? C C11 0.8809(4) 0.1414(2) 1.1519(3) 0.030(2) Uani ? ? C C12 0.8016(4) 0.1853(2) 1.0632(3) 0.029(2) Uani ? ? C C13 0.6623(5) 0.2171(2) 1.0757(3) 0.030(2) Uani ? ? C C14 0.6028(4) 0.2071(2) 1.1741(3) 0.030(2) Uani ? ? C B 0.6897(6) 0.1688(2) 1.2782(4) 0.034(2) Uani ? ? B C15 0.6427(5) 0.1638(2) 1.3970(3) 0.047(2) Uani ? ? C C16 1.0276(5) 0.1098(2) 1.1384(4) 0.043(2) Uani ? ? C C17 0.8643(5) 0.1980(2) 0.9638(3) 0.042(2) Uani ? ? C C18 0.7925(6) 0.2397(2) 0.8842(4) 0.058(3) Uani ? ? C C19 0.6536(6) 0.2698(2) 0.8916(4) 0.056(3) Uani ? ? C C20 0.5864(5) 0.2591(2) 0.9830(4) 0.040(2) Uani ? ? C H1 0.0827 0.1232 0.6424 0.0545 Uiso calc C1 H H2 0.1346 0.1479 0.7677 0.0545 Uiso calc C1 H H3 -0.0809 0.0838 0.7497 0.0824 Uiso calc C2 H H4 0.0062 0.0272 0.7085 0.0824 Uiso calc C2 H H5 0.0581 0.0519 0.8337 0.0824 Uiso calc C2 H H6 0.4321 0.1793 0.7490 0.0525 Uiso calc C3 H H7 0.3765 0.1628 0.6197 0.0525 Uiso calc C3 H H8 0.6443 0.1658 0.6696 0.0732 Uiso calc C4 H H9 0.6457 0.1131 0.7614 0.0732 Uiso calc C4 H H10 0.5900 0.0966 0.6321 0.0732 Uiso calc C4 H H11 0.2306 -0.0094 0.6151 0.0535 Uiso calc C5 H H12 0.3950 0.0090 0.6023 0.0535 Uiso calc C5 H H13 0.2195 0.0226 0.4283 0.0828 Uiso calc C6 H H14 0.1252 0.0705 0.4844 0.0828 Uiso calc C6 H H15 0.2895 0.0889 0.4716 0.0828 Uiso calc C6 H H16 0.8747 0.1013 1.3046 0.0394 Uiso calc C10 H H17 1.0472 0.1214 1.0664 0.0572 Uiso calc C16 H H18 1.1112 0.1236 1.1983 0.0572 Uiso calc C16 H H19 1.0171 0.0644 1.1420 0.0572 Uiso calc C16 H H20 0.5049 0.2250 1.1756 0.0410 Uiso calc C14 H H21 0.7148 0.1373 1.4476 0.0618 Uiso calc C15 H H22 0.6427 0.2055 1.4294 0.0618 Uiso calc C15 H H23 0.5422 0.1456 1.3857 0.0618 Uiso calc C15 H H24 0.9558 0.1769 0.9554 0.0553 Uiso calc C17 H H25 0.8365 0.2492 0.8209 0.0747 Uiso calc C18 H H26 0.6047 0.2982 0.8321 0.0772 Uiso calc C19 H H27 0.4911 0.2792 0.9852 0.0565 Uiso calc C20 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol MO 0.0227(1) 0.0193(1) 0.0236(1) 0.0008(1) 0.0037(1) -0.0013(1) Mo PD 0.0220(1) 0.0201(1) 0.0212(1) 0.0017(1) 0.0024(1) 0.0012(1) Pd P 0.0291(5) 0.0281(5) 0.0240(5) 0.0029(4) 0.0008(4) 0.0054(4) P C1 0.034(2) 0.047(2) 0.040(2) 0.013(2) -0.002(2) 0.010(2) C C2 0.024(2) 0.076(3) 0.086(3) 0.004(2) 0.005(2) 0.003(3) C C3 0.049(2) 0.035(2) 0.035(2) -0.006(2) 0.005(2) 0.010(2) C C4 0.045(3) 0.074(3) 0.049(3) -0.008(2) 0.011(2) 0.016(2) C C5 0.048(3) 0.044(2) 0.028(2) -0.003(2) 0.001(2) -0.004(2) C C6 0.081(4) 0.069(3) 0.033(2) 0.008(3) -0.004(3) -0.003(2) C C7 0.026(2) 0.023(2) 0.030(2) -0.004(1) 0.005(2) -0.004(1) C O1 0.028(1) 0.036(1) 0.042(1) -0.004(1) 0.013(1) -0.009(1) O C8 0.030(2) 0.026(2) 0.030(2) 0.003(2) 0.001(2) -0.005(2) C O2 0.034(1) 0.045(1) 0.039(1) 0.000(1) 0.019(1) -0.003(1) O C9 0.037(2) 0.025(2) 0.029(2) 0.000(2) -0.000(2) -0.005(2) C O3 0.042(2) 0.040(1) 0.056(2) 0.017(1) -0.008(1) -0.015(1) O C10 0.032(2) 0.026(2) 0.029(2) -0.002(2) -0.002(2) -0.005(2) C C11 0.030(2) 0.029(2) 0.029(2) -0.005(2) 0.005(2) -0.005(2) C C12 0.035(2) 0.023(2) 0.030(2) -0.010(2) 0.004(2) -0.005(2) C C13 0.042(2) 0.021(2) 0.030(2) -0.007(2) -0.001(2) -0.002(2) C C14 0.031(2) 0.024(2) 0.037(2) -0.001(2) 0.004(2) -0.008(2) C B 0.038(2) 0.027(2) 0.037(2) -0.005(2) 0.003(2) -0.009(2) B C15 0.059(3) 0.049(2) 0.036(2) 0.004(2) 0.014(2) -0.005(2) C C16 0.033(2) 0.048(2) 0.050(2) -0.008(2) 0.007(2) -0.008(2) C C17 0.053(2) 0.036(2) 0.039(2) -0.016(2) 0.011(2) 0.005(2) C C18 0.065(3) 0.060(3) 0.050(3) -0.016(2) 0.018(2) 0.004(2) C C19 0.065(3) 0.048(2) 0.058(3) -0.009(2) -0.001(3) 0.013(2) C C20 0.055(3) 0.028(2) 0.040(2) -0.006(2) -0.003(2) -0.002(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MO PD 2.8815(4) . . ? MO C7 2.066(4) . . ? MO C9 1.994(4) . . ? MO C10 2.409(4) . . ? MO C11 2.440(4) . . ? MO C12 2.446(4) . . ? MO C13 2.392(4) . . ? MO C14 2.353(4) . . ? MO B 2.547(5) . . ? PD P 2.358(1) . . ? PD C7 2.442(4) . . ? PD C8 2.409(4) . . ? PD C9 2.367(4) . . ? P C1 1.832(4) . . ? P C3 1.834(4) . . ? P C5 1.830(4) . . ? C1 C2 1.505(7) . . ? C3 C4 1.517(6) . . ? C5 C6 1.536(6) . . ? C7 O1 1.169(4) . . ? C8 O2 1.183(5) . . ? C9 O3 1.179(5) . . ? C10 C11 1.400(5) . . ? C10 B 1.517(6) . . ? C11 C12 1.453(5) . . ? C11 C16 1.502(6) . . ? C12 C13 1.442(6) . . ? C12 C17 1.451(6) . . ? C13 C14 1.414(6) . . ? C13 C20 1.450(6) . . ? C14 B 1.531(6) . . ? B C15 1.577(7) . . ? C17 C18 1.337(7) . . ? C18 C19 1.404(7) . . ? C19 C20 1.382(7) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag PD MO C7 56.3(1) . . . ? PD MO C9 54.5(1) . . . ? PD MO C10 158.08(9) . . . ? PD MO C11 135.95(9) . . . ? PD MO C12 122.07(9) . . . ? PD MO C13 122.9(1) . . . ? PD MO C14 138.2(1) . . . ? PD MO B 161.5(1) . . . ? C7 MO C9 107.4(2) . . . ? C7 MO C10 103.5(1) . . . ? C7 MO C11 82.9(1) . . . ? C7 MO C12 90.9(1) . . . ? C7 MO C13 121.1(1) . . . ? C7 MO C14 153.2(1) . . . ? C7 MO B 138.7(2) . . . ? C9 MO C10 147.4(1) . . . ? C9 MO C11 142.5(1) . . . ? C9 MO C12 108.0(1) . . . ? C9 MO C13 82.2(1) . . . ? C9 MO C14 84.0(1) . . . ? C9 MO B 113.7(2) . . . ? C10 MO C11 33.5(1) . . . ? C10 MO C12 61.0(1) . . . ? C10 MO C13 73.1(1) . . . ? C10 MO C14 63.6(1) . . . ? C10 MO B 35.5(1) . . . ? C11 MO C12 34.6(1) . . . ? C11 MO C13 62.4(1) . . . ? C11 MO C14 74.1(1) . . . ? C11 MO B 62.4(1) . . . ? C12 MO C13 34.7(1) . . . ? C12 MO C14 62.3(1) . . . ? C12 MO B 73.5(1) . . . ? C13 MO C14 34.7(1) . . . ? C13 MO B 63.0(1) . . . ? C14 MO B 36.1(1) . . . ? MO PD P 120.85(3) . . . ? MO PD C7 44.73(9) . . . ? MO PD C8 129.21(9) . . . ? MO PD C9 43.3(1) . . . ? P PD C7 125.52(9) . . . ? P PD C8 92.2(1) . . . ? P PD C9 87.8(1) . . . ? C7 PD C8 85.2(1) . . . ? C7 PD C9 85.8(1) . . . ? C8 PD C9 168.9(1) . . . ? C1 P C3 103.6(2) . . . ? C1 P C5 104.4(2) . . . ? C3 P C5 104.0(2) . . . ? P C1 C2 113.3(3) . . . ? P C3 C4 112.5(3) . . . ? P C5 C6 117.3(3) . . . ? C11 C10 B 124.9(4) . . . ? C10 C11 C12 119.6(4) . . . ? C10 C11 C16 121.5(4) . . . ? C12 C11 C16 118.8(4) . . . ? C11 C12 C13 119.7(4) . . . ? C11 C12 C17 120.1(4) . . . ? C13 C12 C17 120.2(4) . . . ? C12 C13 C14 121.0(3) . . . ? C12 C13 C20 117.1(4) . . . ? C14 C13 C20 121.9(4) . . . ? C13 C14 B 122.7(4) . . . ? C10 B C14 111.0(4) . . . ? C10 B C15 123.4(4) . . . ? C14 B C15 125.5(4) . . . ? C12 C17 C18 119.6(5) . . . ? C17 C18 C19 121.7(5) . . . ? C18 C19 C20 121.7(4) . . . ? C13 C20 C19 119.6(4) . . . ? data_st558 _database_code_CSD 153366 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C45 H55 Ag B2 Mo2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H55 Ag B2 Mo2 N2 O6' _chemical_formula_weight 1041.32 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Ag ? -1.085 1.101 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.0187(2) _cell_length_b 18.5098(6) _cell_length_c 20.4035(6) _cell_angle_alpha 90 _cell_angle_beta 98.989(5) _cell_angle_gamma 90 _cell_volume 4483.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.54 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 19098 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.7 deg 1 scans of 50 sec per frame. Data collection was divided into 4 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 107 frames Set 2 Theta = -1.70 Kappa = -170.00 Phi = 0.00 28 frames Set 3 Theta = -6.40 Kappa = 111.00 Phi = 0.00 20 frames Set 4 Theta = -6.40 Kappa = -144.00 Phi = 0.00 18 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19098 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10570 _reflns_number_gt 6353 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6353 _refine_ls_number_parameters 523 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_all 0.798 _refine_ls_wR_factor_ref 0.031 _refine_ls_goodness_of_fit_all 29.933 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_shift/su_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.429 _refine_diff_density_min -0.134 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol AG -0.65534(2) 0.35923(1) 0.13547(1) 0.0320(1) Uani ? ? Ag MO1 -0.76365(2) 0.25475(2) 0.04800(1) 0.0231(1) Uani ? ? Mo MO2 -0.55104(2) 0.47390(2) 0.21481(1) 0.0235(1) Uani ? ? Mo C1 -0.8358(2) 0.3477(2) 0.0582(1) 0.028(2) Uani ? ? C O1 -0.8939(2) 0.3992(1) 0.0598(1) 0.038(1) Uani ? ? O C2 -0.9236(2) 0.2296(2) 0.0411(2) 0.035(2) Uani ? ? C O2 -1.0203(2) 0.2183(2) 0.0362(1) 0.054(2) Uani ? ? O C3 -0.7462(2) 0.2200(2) 0.1402(2) 0.032(2) Uani ? ? C O3 -0.7345(2) 0.1932(1) 0.1926(1) 0.047(1) Uani ? ? O B1 -0.5708(2) 0.1793(2) 0.0490(2) 0.026(2) Uani ? ? B C4 -0.6804(2) 0.1427(2) 0.0149(1) 0.026(2) Uani ? ? C C5 -0.7498(2) 0.1716(2) -0.0411(1) 0.025(2) Uani ? ? C C6 -0.7296(2) 0.2423(2) -0.0652(1) 0.024(2) Uani ? ? C C7 -0.6399(2) 0.2866(2) -0.0296(1) 0.023(2) Uani ? ? C C8 -0.5699(2) 0.2600(2) 0.0284(1) 0.025(2) Uani ? ? C C9 -0.6238(2) 0.3577(2) -0.0552(1) 0.029(2) Uani ? ? C C10 -0.6845(2) 0.3808(2) -0.1144(2) 0.034(2) Uani ? ? C C11 -0.7691(2) 0.3356(2) -0.1503(2) 0.036(2) Uani ? ? C C12 -0.7924(2) 0.2709(2) -0.1256(2) 0.030(2) Uani ? ? C C13 -0.8453(2) 0.1258(2) -0.0772(2) 0.036(2) Uani ? ? C N1 -0.4872(2) 0.1428(1) 0.0955(1) 0.026(1) Uani ? ? N C14 -0.4973(2) 0.0652(2) 0.1113(2) 0.033(2) Uani ? ? C C15 -0.5013(3) 0.0519(2) 0.1844(2) 0.048(2) Uani ? ? C C16 -0.4075(3) 0.0192(2) 0.0856(2) 0.049(2) Uani ? ? C C17 -0.3804(2) 0.1759(2) 0.1277(2) 0.033(2) Uani ? ? C C18 -0.3040(2) 0.1956(2) 0.0770(2) 0.051(2) Uani ? ? C C19 -0.3975(3) 0.2379(2) 0.1739(2) 0.044(2) Uani ? ? C C20 -0.5498(2) 0.3758(2) 0.2546(1) 0.032(2) Uani ? ? C O4 -0.5453(2) 0.3224(1) 0.2851(1) 0.044(1) Uani ? ? O C21 -0.5010(2) 0.4532(2) 0.1299(2) 0.030(2) Uani ? ? C O5 -0.4619(2) 0.4481(1) 0.0807(1) 0.046(1) Uani ? ? O C22 -0.3885(2) 0.4720(2) 0.2459(2) 0.035(2) Uani ? ? C O6 -0.2918(2) 0.4737(1) 0.2640(1) 0.051(1) Uani ? ? O B2 -0.7132(2) 0.5518(2) 0.1661(2) 0.025(2) Uani ? ? B C23 -0.6075(2) 0.5971(2) 0.1827(1) 0.025(2) Uani ? ? C C24 -0.5467(2) 0.5994(2) 0.2468(2) 0.030(2) Uani ? ? C C25 -0.5854(2) 0.5591(2) 0.2994(1) 0.033(2) Uani ? ? C C26 -0.6836(2) 0.5134(2) 0.2869(1) 0.033(2) Uani ? ? C C27 -0.7434(2) 0.5058(2) 0.2203(2) 0.030(2) Uani ? ? C C28 -0.7169(3) 0.4750(2) 0.3415(2) 0.048(2) Uani ? ? C C29 -0.6587(3) 0.4863(2) 0.4054(2) 0.065(3) Uani ? ? C C30 -0.5653(3) 0.5332(3) 0.4159(2) 0.066(3) Uani ? ? C C31 -0.5279(3) 0.5662(2) 0.3666(2) 0.046(2) Uani ? ? C C32 -0.4447(3) 0.6482(2) 0.2630(2) 0.044(2) Uani ? ? C N2 -0.7893(2) 0.5533(1) 0.0962(1) 0.024(1) Uani ? ? N C33 -0.7271(2) 0.5658(2) 0.0364(1) 0.030(2) Uani ? ? C C34 -0.7074(2) 0.6442(2) 0.0214(2) 0.042(2) Uani ? ? C C35 -0.7914(3) 0.5286(2) -0.0243(2) 0.043(2) Uani ? ? C C36 -0.8965(2) 0.5998(2) 0.0951(1) 0.031(2) Uani ? ? C C37 -0.9832(2) 0.5566(2) 0.1251(2) 0.044(2) Uani ? ? C C38 -0.8737(2) 0.6711(2) 0.1313(2) 0.043(2) Uani ? ? C C39 0.4666(3) 0.1543(2) 0.7422(2) 0.052(2) Uani ? ? C C40 0.4304(3) 0.1548(2) 0.8037(2) 0.052(2) Uani ? ? C C41 0.5052(3) 0.1744(2) 0.8609(2) 0.057(2) Uani ? ? C C42 0.6130(3) 0.1931(2) 0.8568(2) 0.066(3) Uani ? ? C C43 0.6475(3) 0.1939(3) 0.7947(2) 0.070(3) Uani ? ? C C44 0.5764(3) 0.1750(2) 0.7386(2) 0.059(2) Uani ? ? C C45 0.3887(3) 0.1325(3) 0.6819(2) 0.078(3) Uani ? ? C H01 -0.8152 0.4998 0.0847 0.0336 Uiso ? ? H H1 -0.7022 0.0983 0.0326 0.0339 Uiso calc C4 H H2 -0.5214 0.2926 0.0552 0.0319 Uiso calc C8 H H3 -0.5704 0.3893 -0.0309 0.0378 Uiso calc C9 H H4 -0.6700 0.4271 -0.1314 0.0442 Uiso calc C10 H H5 -0.8091 0.3512 -0.1918 0.0475 Uiso calc C11 H H6 -0.8524 0.2430 -0.1488 0.0391 Uiso calc C12 H H7 -0.8474 0.0807 -0.0551 0.0472 Uiso calc C13 H H8 -0.9148 0.1503 -0.0776 0.0472 Uiso calc C13 H H9 -0.8331 0.1177 -0.1215 0.0472 Uiso calc C13 H H10 -0.5681 0.0499 0.0881 0.0453 Uiso calc C14 H H11 -0.5077 0.0015 0.1920 0.0620 Uiso calc C15 H H12 -0.4342 0.0696 0.2102 0.0620 Uiso calc C15 H H13 -0.5644 0.0762 0.1968 0.0620 Uiso calc C15 H H14 -0.4170 -0.0300 0.0968 0.0680 Uiso calc C16 H H15 -0.4150 0.0239 0.0388 0.0680 Uiso calc C16 H H16 -0.3348 0.0352 0.1053 0.0680 Uiso calc C16 H H17 -0.3420 0.1399 0.1558 0.0447 Uiso calc C17 H H18 -0.2364 0.2166 0.0993 0.0684 Uiso calc C18 H H19 -0.2865 0.1532 0.0544 0.0684 Uiso calc C18 H H20 -0.3416 0.2291 0.0459 0.0684 Uiso calc C18 H H21 -0.3263 0.2568 0.1930 0.0603 Uiso calc C19 H H22 -0.4407 0.2747 0.1496 0.0603 Uiso calc C19 H H23 -0.4360 0.2208 0.2081 0.0603 Uiso calc C19 H H24 -0.5819 0.6245 0.1487 0.0341 Uiso calc C23 H H25 -0.8023 0.4713 0.2111 0.0391 Uiso calc C27 H H26 -0.7783 0.4421 0.3343 0.0615 Uiso calc C28 H H27 -0.6822 0.4623 0.4421 0.0892 Uiso calc C29 H H28 -0.5282 0.5411 0.4599 0.0892 Uiso calc C30 H H29 -0.4620 0.5953 0.3754 0.0642 Uiso calc C31 H H30 -0.4137 0.6431 0.3085 0.0629 Uiso calc C32 H H31 -0.3898 0.6351 0.2363 0.0629 Uiso calc C32 H H32 -0.4667 0.6970 0.2543 0.0629 Uiso calc C32 H H33 -0.6542 0.5454 0.0481 0.0387 Uiso calc C33 H H34 -0.6690 0.6475 -0.0158 0.0545 Uiso calc C34 H H35 -0.7777 0.6685 0.0118 0.0545 Uiso calc C34 H H36 -0.6631 0.6661 0.0588 0.0545 Uiso calc C34 H H37 -0.7533 0.5362 -0.0612 0.0568 Uiso calc C35 H H38 -0.7957 0.4783 -0.0159 0.0568 Uiso calc C35 H H39 -0.8652 0.5481 -0.0337 0.0568 Uiso calc C35 H H40 -0.9240 0.6116 0.0502 0.0422 Uiso calc C36 H H41 -1.0494 0.5848 0.1246 0.0633 Uiso calc C37 H H42 -1.0012 0.5139 0.0998 0.0633 Uiso calc C37 H H43 -0.9535 0.5440 0.1695 0.0633 Uiso calc C37 H H44 -0.9421 0.6974 0.1291 0.0567 Uiso calc C38 H H45 -0.8433 0.6622 0.1764 0.0567 Uiso calc C38 H H46 -0.8214 0.6984 0.1111 0.0567 Uiso calc C38 H H47 0.3550 0.1418 0.8070 0.0682 Uiso calc C40 H H48 0.4800 0.1745 0.9028 0.0762 Uiso calc C41 H H49 0.6640 0.2056 0.8955 0.0868 Uiso calc C42 H H50 0.7225 0.2079 0.7914 0.0885 Uiso calc C43 H H51 0.6021 0.1759 0.6968 0.0754 Uiso calc C44 H H52 0.3177 0.1202 0.6936 0.1039 Uiso calc C45 H H53 0.3797 0.1713 0.6512 0.1039 Uiso calc C45 H H54 0.4189 0.0918 0.6623 0.1039 Uiso calc C45 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol AG 0.0328(1) 0.0294(1) 0.0340(1) -0.0044(1) -0.0000(1) -0.0072(1) Ag MO1 0.0234(1) 0.0209(2) 0.0252(1) -0.0016(1) 0.0060(1) -0.0014(1) Mo MO2 0.0246(1) 0.0218(2) 0.0244(1) 0.0040(1) 0.0012(1) -0.0028(1) Mo C1 0.025(1) 0.028(2) 0.029(2) -0.004(1) 0.000(1) -0.000(2) C O1 0.036(1) 0.028(1) 0.052(1) 0.006(1) 0.003(1) -0.001(1) O C2 0.037(1) 0.028(2) 0.041(2) -0.000(2) 0.011(1) -0.001(2) C O2 0.028(1) 0.064(2) 0.087(2) -0.009(1) 0.013(1) 0.002(2) O C3 0.031(1) 0.027(2) 0.039(2) 0.002(2) 0.009(1) -0.003(2) C O3 0.071(1) 0.042(2) 0.034(1) 0.003(1) 0.014(1) 0.010(1) O B1 0.026(1) 0.027(2) 0.024(2) 0.001(2) 0.008(1) -0.003(2) B C4 0.033(1) 0.019(2) 0.028(2) -0.001(1) 0.009(1) 0.001(2) C C5 0.024(1) 0.023(2) 0.029(2) -0.001(1) 0.006(1) -0.005(2) C C6 0.023(1) 0.024(2) 0.026(2) 0.002(1) 0.006(1) -0.004(2) C C7 0.024(1) 0.021(2) 0.024(2) 0.002(1) 0.009(1) -0.002(2) C C8 0.023(1) 0.024(2) 0.027(2) -0.004(1) 0.005(1) -0.005(2) C C9 0.032(1) 0.026(2) 0.030(2) 0.002(2) 0.008(1) -0.000(2) C C10 0.039(2) 0.026(2) 0.038(2) 0.004(2) 0.011(1) 0.006(2) C C11 0.038(2) 0.039(2) 0.031(2) 0.010(2) 0.001(1) 0.004(2) C C12 0.029(1) 0.030(2) 0.030(2) 0.005(1) 0.002(1) -0.005(2) C C13 0.042(2) 0.031(2) 0.035(2) -0.006(2) 0.003(1) -0.005(2) C N1 0.026(1) 0.022(1) 0.031(1) 0.003(1) 0.003(1) 0.004(1) N C14 0.034(1) 0.026(2) 0.042(2) -0.002(2) -0.001(1) 0.006(2) C C15 0.045(2) 0.045(2) 0.054(2) 0.004(2) 0.011(2) 0.019(2) C C16 0.068(2) 0.034(2) 0.052(2) 0.012(2) -0.001(2) -0.002(2) C C17 0.025(1) 0.031(2) 0.045(2) -0.003(2) -0.002(1) 0.006(2) C C18 0.036(2) 0.050(3) 0.074(3) -0.003(2) 0.015(2) 0.015(2) C C19 0.043(2) 0.043(2) 0.048(2) 0.003(2) -0.012(2) -0.007(2) C C20 0.036(1) 0.031(2) 0.028(2) 0.005(2) 0.005(1) -0.004(2) C O4 0.063(1) 0.032(1) 0.042(1) 0.004(1) 0.004(1) 0.007(1) O C21 0.030(1) 0.022(2) 0.041(2) -0.002(1) 0.004(1) -0.006(2) C O5 0.051(1) 0.048(2) 0.041(1) -0.011(1) 0.022(1) -0.014(1) O C22 0.038(2) 0.031(2) 0.035(2) 0.006(2) 0.002(1) 0.001(2) C O6 0.029(1) 0.066(2) 0.069(2) 0.008(1) -0.006(1) -0.002(2) O B2 0.025(1) 0.027(2) 0.023(2) 0.008(2) 0.005(1) -0.006(2) B C23 0.029(1) 0.019(2) 0.030(2) 0.007(1) 0.003(1) -0.001(2) C C24 0.034(1) 0.023(2) 0.036(2) 0.009(1) -0.000(1) -0.008(2) C C25 0.037(1) 0.033(2) 0.029(2) 0.021(2) -0.002(1) -0.010(2) C C26 0.044(2) 0.032(2) 0.025(2) 0.017(2) 0.013(1) 0.001(2) C C27 0.024(1) 0.032(2) 0.034(2) 0.006(1) 0.006(1) -0.003(2) C C28 0.057(2) 0.051(3) 0.037(2) 0.023(2) 0.018(2) 0.010(2) C C29 0.102(2) 0.073(3) 0.038(2) 0.042(2) 0.030(2) 0.019(2) C C30 0.071(2) 0.075(3) 0.053(2) 0.023(2) -0.008(2) -0.014(3) C C31 0.067(2) 0.053(3) 0.026(2) 0.024(2) 0.003(2) -0.003(2) C C32 0.046(2) 0.031(2) 0.061(2) 0.001(2) -0.014(2) -0.016(2) C N2 0.025(1) 0.024(1) 0.025(1) 0.004(1) 0.001(1) -0.001(1) N C33 0.030(1) 0.035(2) 0.024(2) 0.004(2) 0.006(1) 0.002(2) C C34 0.047(2) 0.040(2) 0.039(2) 0.001(2) 0.007(2) 0.010(2) C C35 0.051(2) 0.049(3) 0.031(2) 0.003(2) 0.005(2) 0.000(2) C C36 0.024(1) 0.037(2) 0.034(2) 0.012(1) -0.003(1) -0.005(2) C C37 0.025(1) 0.051(3) 0.068(2) 0.006(2) 0.002(2) -0.019(2) C C38 0.039(2) 0.037(2) 0.054(2) 0.013(2) 0.005(2) -0.008(2) C C39 0.073(2) 0.030(2) 0.064(3) 0.008(2) 0.020(2) 0.002(2) C C40 0.068(2) 0.029(2) 0.071(2) -0.003(2) 0.041(2) -0.004(2) C C41 0.076(2) 0.033(2) 0.077(3) -0.008(2) 0.040(2) -0.010(2) C C42 0.084(2) 0.047(3) 0.071(3) -0.007(2) 0.020(2) -0.020(2) C C43 0.070(2) 0.062(3) 0.081(3) -0.008(2) 0.039(2) -0.006(3) C C44 0.058(2) 0.046(3) 0.078(3) 0.000(2) 0.037(2) -0.001(2) C C45 0.094(3) 0.063(3) 0.081(3) 0.019(3) 0.007(3) 0.004(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag AG MO1 2.8097(4) . . ? AG MO2 2.8395(4) . . ? AG C1 2.484(3) . . ? AG C3 2.806(4) . . ? AG C20 2.577(3) . . ? AG C21 2.558(3) . . ? MO1 C1 1.953(4) . . ? MO1 C2 1.961(3) . . ? MO1 C3 1.969(4) . . ? MO1 B1 2.703(3) . . ? MO1 C4 2.443(3) . . ? MO1 C5 2.407(3) . . ? MO1 C6 2.418(3) . . ? MO1 C7 2.408(3) . . ? MO1 C8 2.425(3) . . ? MO2 C20 1.988(4) . . ? MO2 C21 1.959(4) . . ? MO2 C22 1.958(3) . . ? MO2 B2 2.502(3) . . ? MO2 C23 2.439(3) . . ? MO2 C24 2.411(3) . . ? MO2 C25 2.420(3) . . ? MO2 C26 2.443(3) . . ? MO2 C27 2.406(3) . . ? C1 O1 1.184(4) . . ? C2 O2 1.170(3) . . ? C3 O3 1.166(4) . . ? B1 C4 1.546(4) . . ? B1 C8 1.553(5) . . ? B1 N1 1.437(4) . . ? C4 C5 1.410(4) . . ? C5 C6 1.432(4) . . ? C5 C13 1.521(4) . . ? C6 C7 1.456(4) . . ? C6 C12 1.442(4) . . ? C7 C8 1.428(4) . . ? C7 C9 1.440(4) . . ? C9 C10 1.378(4) . . ? C10 C11 1.428(5) . . ? C11 C12 1.347(5) . . ? N1 C14 1.482(4) . . ? N1 C17 1.481(4) . . ? C14 C15 1.520(5) . . ? C14 C16 1.530(5) . . ? C17 C18 1.530(5) . . ? C17 C19 1.519(5) . . ? C20 O4 1.165(4) . . ? C21 O5 1.176(4) . . ? C22 O6 1.164(3) . . ? B2 C23 1.516(5) . . ? B2 C27 1.485(5) . . ? B2 N2 1.570(4) . . ? C23 C24 1.395(4) . . ? C24 C25 1.442(5) . . ? C24 C32 1.518(5) . . ? C25 C26 1.442(5) . . ? C25 C31 1.442(5) . . ? C26 C27 1.442(4) . . ? C26 C28 1.429(5) . . ? C28 C29 1.397(5) . . ? C29 C30 1.408(6) . . ? C30 C31 1.315(6) . . ? N2 C33 1.545(4) . . ? N2 C36 1.547(4) . . ? N2 H01 1.0536 . . ? C33 C34 1.511(5) . . ? C33 C35 1.517(5) . . ? C33 H01 1.9765 . . ? C36 C37 1.516(5) . . ? C36 C38 1.515(5) . . ? C39 C40 1.391(5) . . ? C39 C44 1.386(5) . . ? C39 C45 1.481(6) . . ? C40 C41 1.405(5) . . ? C41 C42 1.357(5) . . ? C42 C43 1.394(6) . . ? C43 C44 1.363(6) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MO1 AG MO2 174.95(1) . . . ? MO1 AG C1 42.75(8) . . . ? MO1 AG C3 41.04(8) . . . ? MO1 AG C20 142.34(9) . . . ? MO1 AG C21 134.98(8) . . . ? MO2 AG C1 133.63(8) . . . ? MO2 AG C3 143.72(8) . . . ? MO2 AG C20 42.71(9) . . . ? MO2 AG C21 42.15(8) . . . ? C1 AG C3 68.7(1) . . . ? C1 AG C20 149.4(1) . . . ? C1 AG C21 126.7(1) . . . ? C3 AG C20 102.3(1) . . . ? C3 AG C21 156.2(1) . . . ? C20 AG C21 73.0(1) . . . ? AG MO1 C1 59.69(8) . . . ? AG MO1 C2 124.1(1) . . . ? AG MO1 C3 69.4(1) . . . ? AG MO1 B1 92.26(8) . . . ? AG MO1 C4 126.22(7) . . . ? AG MO1 C5 147.14(7) . . . ? AG MO1 C6 122.77(8) . . . ? AG MO1 C7 88.64(7) . . . ? AG MO1 C8 73.47(7) . . . ? C1 MO1 C2 76.7(1) . . . ? C1 MO1 C3 99.7(1) . . . ? C1 MO1 B1 148.1(1) . . . ? C1 MO1 C4 170.2(1) . . . ? C1 MO1 C5 136.7(1) . . . ? C1 MO1 C6 109.3(1) . . . ? C1 MO1 C7 100.6(1) . . . ? C1 MO1 C8 115.9(1) . . . ? C2 MO1 C3 87.0(1) . . . ? C2 MO1 B1 135.0(1) . . . ? C2 MO1 C4 102.6(1) . . . ? C2 MO1 C5 88.7(1) . . . ? C2 MO1 C6 102.6(1) . . . ? C2 MO1 C7 135.2(1) . . . ? C2 MO1 C8 162.4(1) . . . ? C3 MO1 B1 82.0(1) . . . ? C3 MO1 C4 90.0(1) . . . ? C3 MO1 C5 120.2(1) . . . ? C3 MO1 C6 150.8(1) . . . ? C3 MO1 C7 136.4(1) . . . ? C3 MO1 C8 102.1(1) . . . ? B1 MO1 C4 34.5(1) . . . ? B1 MO1 C5 61.0(1) . . . ? B1 MO1 C6 71.6(1) . . . ? B1 MO1 C7 61.0(1) . . . ? B1 MO1 C8 34.7(1) . . . ? C4 MO1 C5 33.8(1) . . . ? C4 MO1 C6 61.2(1) . . . ? C4 MO1 C7 72.8(1) . . . ? C4 MO1 C8 62.8(1) . . . ? C5 MO1 C6 34.5(1) . . . ? C5 MO1 C7 62.5(1) . . . ? C5 MO1 C8 73.7(1) . . . ? C6 MO1 C7 35.1(1) . . . ? C6 MO1 C8 62.4(1) . . . ? C7 MO1 C8 34.4(1) . . . ? AG MO2 C20 61.59(9) . . . ? AG MO2 C21 61.23(9) . . . ? AG MO2 C22 120.1(1) . . . ? AG MO2 B2 87.55(9) . . . ? AG MO2 C23 117.80(7) . . . ? AG MO2 C24 149.71(7) . . . ? AG MO2 C25 141.64(8) . . . ? AG MO2 C26 107.19(9) . . . ? AG MO2 C27 82.43(8) . . . ? C20 MO2 C21 101.4(1) . . . ? C20 MO2 C22 84.7(1) . . . ? C20 MO2 B2 130.1(1) . . . ? C20 MO2 C23 161.3(1) . . . ? C20 MO2 C24 140.4(1) . . . ? C20 MO2 C25 107.2(1) . . . ? C20 MO2 C26 89.5(1) . . . ? C20 MO2 C27 98.7(1) . . . ? C21 MO2 C22 81.6(1) . . . ? C21 MO2 B2 95.1(1) . . . ? C21 MO2 C23 93.2(1) . . . ? C21 MO2 C24 115.6(1) . . . ? C21 MO2 C25 150.3(1) . . . ? C21 MO2 C26 155.6(1) . . . ? C21 MO2 C27 121.3(1) . . . ? C22 MO2 B2 144.6(1) . . . ? C22 MO2 C23 109.0(1) . . . ? C22 MO2 C24 87.2(1) . . . ? C22 MO2 C25 93.0(1) . . . ? C22 MO2 C26 121.4(1) . . . ? C22 MO2 C27 155.0(1) . . . ? B2 MO2 C23 35.7(1) . . . ? B2 MO2 C24 62.3(1) . . . ? B2 MO2 C25 72.5(1) . . . ? B2 MO2 C26 61.7(1) . . . ? B2 MO2 C27 35.1(1) . . . ? C23 MO2 C24 33.4(1) . . . ? C23 MO2 C25 60.7(1) . . . ? C23 MO2 C26 72.7(1) . . . ? C23 MO2 C27 63.5(1) . . . ? C24 MO2 C25 34.7(1) . . . ? C24 MO2 C26 62.4(1) . . . ? C24 MO2 C27 74.4(1) . . . ? C25 MO2 C26 34.5(1) . . . ? C25 MO2 C27 62.3(1) . . . ? C26 MO2 C27 34.6(1) . . . ? C4 B1 C8 110.0(3) . . . ? C4 B1 N1 123.3(3) . . . ? C8 B1 N1 126.6(3) . . . ? B1 C4 C5 123.5(3) . . . ? C4 C5 C6 120.9(3) . . . ? C4 C5 C13 119.1(3) . . . ? C6 C5 C13 119.9(3) . . . ? C5 C6 C7 119.7(3) . . . ? C5 C6 C12 122.3(3) . . . ? C7 C6 C12 117.9(3) . . . ? C6 C7 C8 120.9(3) . . . ? C6 C7 C9 117.7(3) . . . ? C8 C7 C9 121.4(3) . . . ? B1 C8 C7 121.8(3) . . . ? C7 C9 C10 121.3(3) . . . ? C9 C10 C11 120.3(3) . . . ? C10 C11 C12 120.2(3) . . . ? C6 C12 C11 122.3(3) . . . ? B1 N1 C14 121.8(3) . . . ? B1 N1 C17 124.5(3) . . . ? C14 N1 C17 113.5(2) . . . ? N1 C14 C15 112.8(3) . . . ? N1 C14 C16 112.3(3) . . . ? C15 C14 C16 112.2(3) . . . ? N1 C17 C18 111.6(3) . . . ? N1 C17 C19 113.4(2) . . . ? C18 C17 C19 113.2(3) . . . ? C23 B2 C27 116.4(3) . . . ? C23 B2 N2 122.8(3) . . . ? C27 B2 N2 120.8(3) . . . ? B2 C23 C24 121.6(3) . . . ? C23 C24 C25 119.9(3) . . . ? C23 C24 C32 120.6(3) . . . ? C25 C24 C32 119.3(3) . . . ? C24 C25 C26 121.5(3) . . . ? C24 C25 C31 119.8(3) . . . ? C26 C25 C31 118.7(3) . . . ? C25 C26 C27 119.8(3) . . . ? C25 C26 C28 118.4(3) . . . ? C27 C26 C28 121.8(3) . . . ? B2 C27 C26 120.2(3) . . . ? C26 C28 C29 119.5(4) . . . ? C28 C29 C30 120.3(4) . . . ? C29 C30 C31 122.1(4) . . . ? C25 C31 C30 120.9(4) . . . ? B2 N2 C33 115.8(2) . . . ? B2 N2 C36 112.8(2) . . . ? B2 N2 H01 107.19 . . . ? C33 N2 C36 114.2(2) . . . ? C33 N2 H01 97.25 . . . ? C36 N2 H01 107.72 . . . ? N2 C33 C34 114.4(3) . . . ? N2 C33 C35 109.3(3) . . . ? N2 C33 H01 31.92 . . . ? C34 C33 C35 110.3(3) . . . ? C34 C33 H01 143.89 . . . ? C35 C33 H01 83.29 . . . ? N2 C36 C37 108.9(3) . . . ? N2 C36 C38 113.0(2) . . . ? C37 C36 C38 110.3(3) . . . ? C40 C39 C44 118.8(4) . . . ? C40 C39 C45 120.3(4) . . . ? C44 C39 C45 121.0(4) . . . ? C39 C40 C41 120.1(3) . . . ? C40 C41 C42 120.5(4) . . . ? C41 C42 C43 118.8(4) . . . ? C42 C43 C44 121.6(4) . . . ? C39 C44 C43 120.2(4) . . . ? N2 H01 C33 50.82 . . . ? data_st639 _database_code_CSD 153367 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C38 H46 B2 Hg Mo2 N2 O6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H46 B2 Hg Mo2 N2 O6' _chemical_formula_weight 1040.89 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 Hg ? -3.084 9.223 International_Tables_Vol_IV_Table_2.3.1 Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 9.2428(6) _cell_length_b 9.7821(6) _cell_length_c 12.3798(5) _cell_angle_alpha 78.225(5) _cell_angle_beta 87.103(5) _cell_angle_gamma 67.449(5) _cell_volume 1011.5(1) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.71 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 4.440 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 6602 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 30 sec per frame. Data collection was divided into 3 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 91 frames Set 2 Theta = -3.30 Kappa = -169.00 Phi = 0.00 22 frames Set 3 Theta = -6.30 Kappa = -174.00 Phi = 0.00 23 frames Friedel pairs were averaged. Internal R = 0.06 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6602 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4590 _reflns_number_gt 3382 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3382 _refine_ls_number_parameters 250 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.063 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_all 0.633 _refine_ls_wR_factor_ref 0.058 _refine_ls_goodness_of_fit_all 11.963 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.045 _refine_diff_density_min -0.415 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol HG 1.0000 0.0000 1.0000 0.0314 0.500 Uani ? ? Hg MO 1.18001(5) -0.25823(5) 1.14359(4) 0.0256(2) 1.000 Uani ? ? Mo C1 1.0702(9) -0.0945(8) 1.2265(6) 0.045(3) 1.000 Uani ? ? C O1 1.0107(9) -0.0111(7) 1.2828(5) 0.082(4) 1.000 Uani ? ? O C2 1.3484(8) -0.2910(8) 1.2488(6) 0.045(3) 1.000 Uani ? ? C O2 1.4475(6) -0.3062(8) 1.3079(5) 0.074(3) 1.000 Uani ? ? O C3 1.3194(8) -0.1862(8) 1.0391(6) 0.046(3) 1.000 Uani ? ? C O3 1.4063(7) -0.1567(7) 0.9815(5) 0.076(3) 1.000 Uani ? ? O C4 1.2892(7) -0.5119(6) 1.1175(5) 0.031(3) 1.000 Uani ? ? C C5 1.1797(7) -0.4262(6) 1.0287(5) 0.030(2) 1.000 Uani ? ? C C6 1.0174(7) -0.3441(6) 1.0523(5) 0.031(2) 1.000 Uani ? ? C C7 0.9684(6) -0.3430(6) 1.1638(5) 0.028(2) 1.000 Uani ? ? C C8 1.0768(7) -0.4302(6) 1.2531(4) 0.029(2) 1.000 Uani ? ? C B 1.2411(8) -0.5461(7) 1.2379(5) 0.028(3) 1.000 Uani ? ? B N 1.3410(6) -0.6602(6) 1.3227(4) 0.034(3) 1.000 Uani ? ? N C9 1.500(1) -0.7605(9) 1.3008(6) 0.048(4) 1.000 Uani ? ? C C10 1.513(1) -0.924(1) 1.3157(8) 0.070(6) 1.000 Uani ? ? C C11 1.628(1) -0.749(1) 1.3680(9) 0.073(6) 1.000 Uani ? ? C C12 1.2936(8) -0.6872(8) 1.4388(5) 0.037(3) 1.000 Uani ? ? C C13 1.2705(9) -0.558(1) 1.4941(6) 0.046(4) 1.000 Uani ? ? C C14 1.154(1) -0.7324(9) 1.4499(6) 0.051(4) 1.000 Uani ? ? C C15 0.8066(7) -0.2505(7) 1.1856(6) 0.038(3) 1.000 Uani ? ? C C16 1.2269(9) -0.4170(7) 0.9127(5) 0.043(3) 1.000 Uani ? ? C C17 0.9021(7) -0.2652(6) 0.9623(5) 0.037(3) 1.000 Uani ? ? C C18 0.759(1) -0.193(1) 0.984(1) 0.035(5) 0.500 Uani ? ? C C19 0.709(1) -0.185(1) 1.097(1) 0.031(5) 0.500 Uani ? ? C C20 0.940(2) -0.266(1) 0.858(1) 0.048(6) 0.500 Uani ? ? C C21 1.106(2) -0.345(1) 0.833(1) 0.061(6) 0.500 Uani ? ? C H1 1.3975 -0.5499 1.1018 0.0435 1.000 Uiso calc C4 H H2 1.0461 -0.4162 1.3258 0.0409 1.000 Uiso calc C8 H H3 1.5183 -0.7265 1.2257 0.0858 1.000 Uiso calc C9 H H4 1.6170 -0.9868 1.3011 0.1292 1.000 Uiso calc C10 H H5 1.4892 -0.9582 1.3893 0.1292 1.000 Uiso calc C10 H H6 1.4416 -0.9298 1.2659 0.1292 1.000 Uiso calc C10 H H7 1.7274 -0.8158 1.3504 0.1187 1.000 Uiso calc C11 H H8 1.6236 -0.6482 1.3510 0.1187 1.000 Uiso calc C11 H H9 1.6110 -0.7752 1.4445 0.1187 1.000 Uiso calc C11 H H10 1.3790 -0.7711 1.4770 0.0593 1.000 Uiso calc C12 H H11 1.2404 -0.5802 1.5680 0.0702 1.000 Uiso calc C13 H H12 1.3658 -0.5419 1.4942 0.0702 1.000 Uiso calc C13 H H13 1.1909 -0.4689 1.4553 0.0702 1.000 Uiso calc C13 H H14 1.1280 -0.7485 1.5254 0.0767 1.000 Uiso calc C14 H H15 1.0676 -0.6543 1.4082 0.0767 1.000 Uiso calc C14 H H16 1.1789 -0.8229 1.4231 0.0767 1.000 Uiso calc C14 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol HG 0.0433 0.0184(1) 0.0388(1) -0.0125(1) -0.0120(1) 0.0061(1) Hg MO 0.0328(2) 0.0188(2) 0.0272(2) -0.0088(2) -0.0035(2) 0.0013(2) Mo C1 0.054(4) 0.037(3) 0.045(3) -0.008(3) -0.009(3) -0.007(3) C O1 0.099(5) 0.065(3) 0.087(3) -0.010(3) 0.002(3) -0.051(2) O C2 0.050(3) 0.043(3) 0.041(3) -0.018(2) -0.011(3) 0.002(3) C O2 0.062(3) 0.093(4) 0.069(3) -0.036(2) -0.030(2) 0.006(3) O C3 0.047(3) 0.041(3) 0.049(3) -0.020(2) -0.004(3) -0.001(3) C O3 0.075(3) 0.071(3) 0.082(3) -0.044(2) 0.032(3) -0.001(3) O C4 0.037(3) 0.024(2) 0.032(3) -0.006(2) 0.007(2) -0.004(2) C C5 0.048(3) 0.022(2) 0.026(2) -0.014(2) 0.006(2) -0.001(2) C C6 0.046(3) 0.020(2) 0.031(3) -0.017(2) -0.004(2) -0.001(2) C C7 0.036(2) 0.021(2) 0.030(3) -0.016(2) 0.002(2) 0.003(2) C C8 0.041(3) 0.023(2) 0.025(2) -0.009(2) 0.003(2) -0.001(2) C B 0.043(3) 0.019(2) 0.027(3) -0.010(2) 0.008(3) 0.000(2) B N 0.043(3) 0.029(2) 0.031(2) 0.004(2) 0.011(2) 0.002(2) N C9 0.059(4) 0.049(4) 0.039(3) 0.023(4) 0.013(3) 0.011(3) C C10 0.124(8) 0.042(5) 0.066(5) 0.034(5) 0.014(6) -0.002(4) C C11 0.052(5) 0.090(7) 0.083(6) 0.012(5) 0.007(5) 0.012(6) C C12 0.043(3) 0.034(3) 0.033(3) 0.007(3) 0.006(3) 0.006(3) C C13 0.051(4) 0.058(4) 0.033(3) -0.005(3) 0.002(3) 0.002(3) C C14 0.076(5) 0.043(4) 0.041(3) -0.013(3) 0.015(3) 0.007(3) C C15 0.038(3) 0.029(3) 0.050(3) -0.013(2) -0.000(3) 0.000(3) C C16 0.078(4) 0.034(3) 0.030(3) -0.023(3) 0.004(3) -0.003(2) C C17 0.057(3) 0.027(2) 0.032(3) -0.027(2) -0.009(2) 0.003(2) C C18 0.045(5) 0.023(4) 0.042(6) -0.016(4) -0.015(5) 0.000(4) C C19 0.025(5) 0.026(5) 0.047(6) -0.009(4) 0.010(5) -0.004(5) C C20 0.074(6) 0.040(5) 0.038(6) -0.042(4) -0.014(5) 0.005(5) C C21 0.095(7) 0.051(5) 0.046(7) -0.056(4) 0.000(6) -0.008(5) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag HG MO 2.7481 . . ? HG MO 2.7481 . 2_757 ? HG C1 2.7931 . . ? HG C1 2.7931 . 2_757 ? MO C1 1.992(8) . . ? MO C2 1.968(7) . . ? MO C3 1.996(8) . . ? MO C4 2.377(6) . . ? MO C5 2.383(6) . . ? MO C6 2.402(6) . . ? MO C7 2.385(6) . . ? MO C8 2.398(6) . . ? MO B 2.668(7) . . ? C1 O1 1.14(1) . . ? C2 O2 1.148(9) . . ? C3 O3 1.128(9) . . ? C4 C5 1.421(9) . . ? C4 B 1.541(9) . . ? C5 C6 1.452(9) . . ? C5 C16 1.475(9) . . ? C6 C7 1.433(9) . . ? C6 C17 1.453(9) . . ? C7 C8 1.423(8) . . ? C7 C15 1.466(9) . . ? C8 B 1.54(1) . . ? B N 1.425(9) . . ? N C9 1.471(9) . . ? N C12 1.482(8) . . ? C9 C10 1.54(2) . . ? C9 C11 1.53(2) . . ? C12 C13 1.50(1) . . ? C12 C14 1.51(1) . . ? C15 C19 1.34(1) . . ? C16 C21 1.40(2) . . ? C17 C18 1.28(2) . . ? C17 C20 1.32(2) . . ? C18 C19 1.46(2) . . ? C20 C21 1.48(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MO HG MO 180.00 . . 2_757 ? MO HG C1 42.12 . . . ? MO HG C1 137.88 . 2_757 . ? C1 HG C1 180.00 . . 2_757 ? HG MO C1 70.15 . . . ? HG MO C2 129.84 . . . ? HG MO C3 70.79 . . . ? HG MO C4 129.33 . . . ? HG MO C5 95.16 . . . ? HG MO C6 77.58 . . . ? HG MO C7 90.58 . . . ? HG MO C8 123.56 . . . ? HG MO B 149.38 . . . ? C1 MO C2 79.8(3) . . . ? C1 MO C3 106.5(3) . . . ? C1 MO C4 155.2(3) . . . ? C1 MO C5 151.9(3) . . . ? C1 MO C6 116.6(3) . . . ? C1 MO C7 92.0(3) . . . ? C1 MO C8 93.5(3) . . . ? C1 MO B 120.3(3) . . . ? C2 MO C3 81.1(3) . . . ? C2 MO C4 93.1(3) . . . ? C2 MO C5 126.1(3) . . . ? C2 MO C6 152.6(3) . . . ? C2 MO C7 130.6(3) . . . ? C2 MO C8 96.8(3) . . . ? C2 MO B 80.6(3) . . . ? C3 MO C4 95.6(3) . . . ? C3 MO C5 90.0(3) . . . ? C3 MO C6 112.1(3) . . . ? C3 MO C7 146.4(3) . . . ? C3 MO C8 159.0(3) . . . ? C3 MO B 125.0(3) . . . ? C4 MO C5 34.7(2) . . . ? C4 MO C6 62.5(2) . . . ? C4 MO C7 74.5(2) . . . ? C4 MO C8 63.5(2) . . . ? C4 MO B 35.0(2) . . . ? C5 MO C6 35.3(2) . . . ? C5 MO C7 63.4(2) . . . ? C5 MO C8 74.3(2) . . . ? C5 MO B 61.9(2) . . . ? C6 MO C7 34.8(2) . . . ? C6 MO C8 62.1(2) . . . ? C6 MO B 72.1(2) . . . ? C7 MO C8 34.6(2) . . . ? C7 MO B 61.8(2) . . . ? C8 MO B 34.8(2) . . . ? C5 C4 B 123.3(6) . . . ? C4 C5 C6 119.5(5) . . . ? C4 C5 C16 121.7(6) . . . ? C6 C5 C16 118.9(6) . . . ? C5 C6 C7 120.7(5) . . . ? C5 C6 C17 120.0(6) . . . ? C7 C6 C17 119.3(6) . . . ? C6 C7 C8 120.1(6) . . . ? C6 C7 C15 119.7(6) . . . ? C8 C7 C15 120.2(6) . . . ? C7 C8 B 123.2(5) . . . ? C4 B C8 109.5(5) . . . ? C4 B N 124.2(6) . . . ? C8 B N 126.1(5) . . . ? B N C9 121.9(5) . . . ? B N C12 123.1(5) . . . ? C9 N C12 115.0(5) . . . ? N C9 C10 111.1(9) . . . ? N C9 C11 113.3(8) . . . ? C10 C9 C11 111.5(8) . . . ? N C12 C13 112.6(6) . . . ? N C12 C14 112.4(7) . . . ? C13 C12 C14 112.2(6) . . . ? C7 C15 C19 115.9(8) . . . ? C5 C16 C21 116(1) . . . ? C6 C17 C18 119.3(8) . . . ? C6 C17 C20 121.7(9) . . . ? C18 C17 C20 118(1) . . . ? C17 C18 C19 121(1) . . . ? C15 C19 C18 123(1) . . . ? C17 C20 C21 118(1) . . . ? C16 C21 C20 123(1) . . . ?