# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address M.Koberl ; Department Chemie, Department Chemie, Molekulare Katalyse, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; M.Cokoja ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; B.Bechlars ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; E.Herdtweck ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; F.Kuhn ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_name 'Prof. Fritz Kuhn' _publ_contact_author_email fritz.kuehn@ch.tum.de _publ_section_title ; Dicarboxylate-bridged (Mo2)n (n = 2, 3, 4) paddle-wheel complexes: Potential intermediate building blocks for metal-organic frameworks ; _publ_contact_author_address ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_fax '+49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13073' _publ_contact_letter # Include date of submission ; Date of submission: June 2011 ; # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? # Attachment '- compound_2.cif' # CIF-file generated for KOEB 6081-123 # Compound_2 #=================================================================== #TrackingRef '- compound_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 830421' _audit_creation_date 9-Jun-11 _audit_creation_method 'PLATON option' _audit_update_record ; 9-Jun-11 Updated by the Author E.H. Text writing by E.H. Checkcif OK 9-Jun-11 Updated by the Author E.H. ; _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C34 H48 Mo4 N16 O4, 6(B F4), 8(C2 H3 N)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H72 B6 F24 Mo4 N24 O4' _chemical_formula_weight 1977.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 14.9896(4) _cell_length_b 18.3686(5) _cell_length_c 15.5071(4) _cell_angle_alpha 90 _cell_angle_beta 92.7229(14) _cell_angle_gamma 90 _cell_volume 4264.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 9252 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.46 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method none _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6608 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 10 s per frame dx 45 3202 frames measured in 8 data sets phi-scan with delta_phi = 0.50 omega-scans with delta_omega = 0.50 ; _publ_section_exptl_prep ; The crystal was fixed on the top of a glass fiber with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Solution and refinements with the program WinGX; Farrugia (1999). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 82672 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0094 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.46 _reflns_number_total 7880 _reflns_number_gt 7572 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+5.3086P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 7880 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.759 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.055 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Mo1 Mo Uani 0.05042(1) -0.01650(1) 0.22787(1) 1.000 0.0136(1) . . Mo2 Mo Uani 0.14157(1) 0.06399(1) 0.17863(1) 1.000 0.0142(1) . . O1 O Uani -0.00679(8) -0.03394(6) 0.10515(7) 1.000 0.0149(3) . . O2 O Uani 0.08338(8) 0.05121(6) 0.05496(7) 1.000 0.0152(3) . . N1 N Uani 0.06526(10) 0.16111(8) 0.19643(10) 1.000 0.0197(5) . . N2 N Uani 0.21918(10) 0.09173(8) 0.29419(10) 1.000 0.0201(5) . . N3 N Uani 0.24898(10) -0.00541(9) 0.14392(10) 1.000 0.0197(5) . . N4 N Uani -0.06007(10) 0.05310(8) 0.25256(9) 1.000 0.0185(4) . . N5 N Uani 0.08863(10) -0.01568(8) 0.36303(10) 1.000 0.0197(5) . . N6 N Uani 0.13319(10) -0.11038(8) 0.22110(10) 1.000 0.0193(4) . . N7 N Uani 0.23521(12) 0.15669(10) 0.09259(11) 1.000 0.0306(5) . . N8 N Uani 0.06302(12) 0.11255(10) 0.71990(12) 1.000 0.0325(6) . . C1 C Uani 0.02140(11) 0.00477(9) 0.04487(11) 1.000 0.0142(5) . . C2 C Uani 0.03014(13) 0.21475(10) 0.20789(12) 1.000 0.0218(5) . . C3 C Uani -0.01501(14) 0.28346(11) 0.22346(15) 1.000 0.0303(6) . . C4 C Uani 0.25839(13) 0.10863(10) 0.35535(12) 1.000 0.0233(6) . . C5 C Uani 0.30815(16) 0.13246(13) 0.43354(14) 1.000 0.0373(7) . . C6 C Uani 0.30798(12) -0.03957(10) 0.12426(12) 1.000 0.0213(5) . . C7 C Uani 0.38340(14) -0.08334(13) 0.09964(15) 1.000 0.0323(7) . . C8 C Uani -0.12096(13) 0.08772(10) 0.26439(11) 1.000 0.0207(5) . . C9 C Uani -0.19833(14) 0.13279(13) 0.28001(14) 1.000 0.0322(6) . . C10 C Uani 0.10741(13) -0.02077(10) 0.43462(12) 1.000 0.0219(6) . . C11 C Uani 0.13124(16) -0.02827(13) 0.52625(13) 1.000 0.0338(7) . . C12 C Uani 0.17922(13) -0.15947(10) 0.22587(12) 1.000 0.0207(5) . . C13 C Uani 0.23860(15) -0.22173(11) 0.23242(14) 1.000 0.0302(6) . . C14 C Uani 0.27856(14) 0.19697(12) 0.05957(14) 1.000 0.0307(6) . . C15 C Uani 0.3360(2) 0.24767(18) 0.0165(2) 1.000 0.0643(11) . . C16 C Uani 0.11533(14) 0.15049(11) 0.69437(13) 1.000 0.0283(6) . . C17 C Uani 0.18399(17) 0.19878(15) 0.66339(16) 1.000 0.0445(8) . . F9 F Uani 0.16366(13) 0.46985(10) 0.06025(12) 1.000 0.0684(7) . . F10 F Uani 0.13526(12) 0.41672(10) 0.18688(10) 1.000 0.0589(6) . . F11 F Uani 0.0787(3) 0.3707(2) 0.06196(19) 0.729(7) 0.0625(13) . . F12 F Uani 0.2283(2) 0.36540(16) 0.08879(16) 0.729(7) 0.0651(10) . . B3 B Uani 0.1462(2) 0.40562(16) 0.09948(19) 1.000 0.0472(10) . . F11A F Uani 0.0396(6) 0.4009(6) 0.0611(6) 0.271(7) 0.065(3) . . F12A F Uani 0.1537(8) 0.3324(4) 0.0970(5) 0.271(7) 0.083(4) . . N9 N Uani 0.66163(19) 0.23705(17) 0.36723(17) 1.000 0.0698(10) . . C18 C Uani 0.60135(17) 0.25466(14) 0.40305(16) 1.000 0.0399(8) . . C19 C Uani 0.52467(16) 0.27827(13) 0.44869(16) 1.000 0.0398(8) . . N10 N Uani 0.6923(2) -0.0362(2) 0.3276(2) 1.000 0.0836(14) . . C20 C Uani 0.6288(2) -0.01005(17) 0.34746(17) 1.000 0.0508(9) . . C21 C Uani 0.5491(2) 0.0268(2) 0.3746(2) 1.000 0.0780(14) . . N11 N Uani 0.44266(19) 0.1744(2) 0.2505(2) 1.000 0.0791(13) . . C22 C Uani 0.47902(17) 0.14772(16) 0.19633(18) 1.000 0.0468(8) . . C23 C Uani 0.5258(2) 0.11236(17) 0.1280(2) 1.000 0.0591(11) . . N12 N Uani 0.10554(16) 0.55983(16) 0.5639(2) 1.000 0.0701(10) . . C24 C Uani 0.17892(16) 0.55728(14) 0.58637(17) 1.000 0.0398(8) . . C25 C Uani 0.27253(15) 0.55232(14) 0.61227(15) 1.000 0.0361(7) . . F1 F Uani 0.38115(10) 0.39630(8) 0.53986(11) 1.000 0.0494(5) . . F2 F Uani 0.23939(8) 0.37178(8) 0.57527(9) 1.000 0.0420(5) . . F3 F Uani 0.34766(10) 0.28673(9) 0.59436(10) 1.000 0.0554(5) . . F4 F Uani 0.29804(10) 0.31746(9) 0.45943(9) 1.000 0.0487(5) . . B1 B Uani 0.31662(15) 0.34309(13) 0.54189(14) 1.000 0.0241(6) . . F5 F Uani 0.11023(10) 0.22642(10) 0.38778(10) 1.000 0.0542(5) . . F6 F Uani -0.02775(9) 0.18025(8) 0.40167(9) 1.000 0.0440(5) . . F7 F Uani 0.09177(14) 0.13416(9) 0.48007(11) 1.000 0.0675(7) . . F8 F Uani 0.04084(10) 0.24692(10) 0.51018(11) 1.000 0.0608(6) . . B2 B Uani 0.05294(16) 0.19626(13) 0.44621(16) 1.000 0.0286(7) . . H31 H Uiso -0.06970 0.28650 0.18640 1.000 0.0450 calc R H32 H Uiso 0.02460 0.32400 0.21030 1.000 0.0450 calc R H33 H Uiso -0.03030 0.28610 0.28410 1.000 0.0450 calc R H51 H Uiso 0.29490 0.18380 0.44450 1.000 0.0560 calc R H52 H Uiso 0.37230 0.12670 0.42600 1.000 0.0560 calc R H53 H Uiso 0.29070 0.10290 0.48260 1.000 0.0560 calc R H71 H Uiso 0.41800 -0.05620 0.05830 1.000 0.0480 calc R H72 H Uiso 0.36160 -0.12870 0.07300 1.000 0.0480 calc R H73 H Uiso 0.42150 -0.09460 0.15100 1.000 0.0480 calc R H91 H Uiso -0.24200 0.10430 0.31080 1.000 0.0480 calc R H92 H Uiso -0.22550 0.14940 0.22480 1.000 0.0480 calc R H93 H Uiso -0.17960 0.17500 0.31500 1.000 0.0480 calc R H111 H Uiso 0.09630 -0.06780 0.55050 1.000 0.0510 calc R H112 H Uiso 0.11840 0.01740 0.55590 1.000 0.0510 calc R H113 H Uiso 0.19500 -0.03950 0.53410 1.000 0.0510 calc R H131 H Uiso 0.28110 -0.21520 0.28180 1.000 0.0450 calc R H132 H Uiso 0.27130 -0.22600 0.17940 1.000 0.0450 calc R H133 H Uiso 0.20360 -0.26600 0.24050 1.000 0.0450 calc R H151 H Uiso 0.36950 0.22150 -0.02650 1.000 0.0960 calc R H152 H Uiso 0.37780 0.27010 0.05910 1.000 0.0960 calc R H153 H Uiso 0.29940 0.28560 -0.01220 1.000 0.0960 calc R H171 H Uiso 0.19990 0.23500 0.70790 1.000 0.0670 calc R H172 H Uiso 0.16120 0.22360 0.61090 1.000 0.0670 calc R H173 H Uiso 0.23700 0.17020 0.65050 1.000 0.0670 calc R H191 H Uiso 0.53650 0.32640 0.47400 1.000 0.0600 calc R H192 H Uiso 0.51310 0.24340 0.49470 1.000 0.0600 calc R H193 H Uiso 0.47240 0.28100 0.40840 1.000 0.0600 calc R H211 H Uiso 0.55920 0.07950 0.37480 1.000 0.1170 calc R H212 H Uiso 0.53570 0.01070 0.43280 1.000 0.1170 calc R H213 H Uiso 0.49870 0.01510 0.33450 1.000 0.1170 calc R H231 H Uiso 0.57790 0.14160 0.11410 1.000 0.0890 calc R H232 H Uiso 0.48560 0.10770 0.07660 1.000 0.0890 calc R H233 H Uiso 0.54550 0.06390 0.14730 1.000 0.0890 calc R H251 H Uiso 0.30500 0.59240 0.58620 1.000 0.0540 calc R H252 H Uiso 0.29640 0.50570 0.59290 1.000 0.0540 calc R H253 H Uiso 0.27970 0.55550 0.67530 1.000 0.0540 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 Mo1 0.0148(1) 0.0139(1) 0.0121(1) 0.0005(1) 0.0004(1) 0.0002(1) Mo2 0.0145(1) 0.0142(1) 0.0138(1) -0.0003(1) -0.0005(1) -0.0012(1) O1 0.0160(6) 0.0149(6) 0.0137(6) 0.0006(5) 0.0006(5) 0.0000(5) O2 0.0156(6) 0.0155(6) 0.0144(6) 0.0002(5) 0.0002(5) -0.0010(5) N1 0.0214(8) 0.0170(8) 0.0206(8) -0.0005(6) -0.0006(6) -0.0015(6) N2 0.0210(8) 0.0191(8) 0.0199(8) 0.0001(6) -0.0009(6) -0.0025(6) N3 0.0178(8) 0.0209(8) 0.0203(8) 0.0012(6) 0.0008(6) -0.0019(6) N4 0.0195(8) 0.0199(8) 0.0161(7) 0.0001(6) 0.0021(6) 0.0000(6) N5 0.0214(8) 0.0200(8) 0.0176(8) 0.0006(6) 0.0012(6) -0.0015(6) N6 0.0211(8) 0.0184(8) 0.0184(7) 0.0013(6) 0.0000(6) 0.0001(7) N7 0.0352(10) 0.0265(9) 0.0305(9) -0.0001(7) 0.0061(8) -0.0080(8) N8 0.0308(10) 0.0295(10) 0.0374(10) 0.0058(8) 0.0025(8) -0.0067(8) C1 0.0136(8) 0.0134(8) 0.0155(9) -0.0005(6) 0.0010(7) 0.0036(6) C2 0.0219(9) 0.0205(10) 0.0227(9) 0.0001(7) -0.0006(7) -0.0044(8) C3 0.0303(11) 0.0196(10) 0.0409(12) -0.0031(9) 0.0009(9) 0.0037(8) C4 0.0254(10) 0.0202(9) 0.0240(10) 0.0016(8) -0.0013(8) -0.0036(8) C5 0.0435(13) 0.0391(13) 0.0279(11) -0.0045(9) -0.0130(10) -0.0078(10) C6 0.0196(9) 0.0224(9) 0.0218(9) 0.0025(7) 0.0005(7) -0.0028(8) C7 0.0232(10) 0.0357(12) 0.0385(12) 0.0005(10) 0.0060(9) 0.0090(9) C8 0.0224(10) 0.0226(9) 0.0171(9) 0.0012(7) 0.0016(7) -0.0002(8) C9 0.0261(10) 0.0392(12) 0.0316(11) 0.0022(9) 0.0058(8) 0.0136(9) C10 0.0227(9) 0.0225(10) 0.0204(10) 0.0006(7) 0.0017(7) -0.0032(7) C11 0.0415(13) 0.0424(13) 0.0169(10) 0.0038(9) -0.0035(9) -0.0068(10) C12 0.0236(9) 0.0188(9) 0.0196(9) 0.0017(7) 0.0005(7) -0.0018(8) C13 0.0341(11) 0.0215(10) 0.0347(11) 0.0019(8) 0.0001(9) 0.0101(9) C14 0.0259(10) 0.0317(11) 0.0348(11) 0.0035(9) 0.0037(9) -0.0026(9) C15 0.0422(15) 0.066(2) 0.086(2) 0.0287(17) 0.0157(15) -0.0187(14) C16 0.0302(11) 0.0279(11) 0.0264(10) 0.0023(8) -0.0016(8) -0.0060(9) C17 0.0462(14) 0.0496(15) 0.0376(13) 0.0046(11) 0.0020(11) -0.0278(12) F9 0.0706(12) 0.0688(12) 0.0650(11) 0.0205(9) -0.0058(9) -0.0257(10) F10 0.0708(11) 0.0663(11) 0.0398(8) -0.0105(8) 0.0051(8) -0.0183(9) F11 0.077(3) 0.063(2) 0.0473(14) -0.0090(15) 0.0013(16) -0.0397(19) F12 0.078(2) 0.0627(18) 0.0557(15) 0.0091(12) 0.0155(13) 0.0266(16) B3 0.073(2) 0.0306(14) 0.0379(15) 0.0008(12) 0.0005(14) -0.0013(14) F11A 0.046(5) 0.081(7) 0.067(5) -0.004(5) -0.001(4) -0.005(4) F12A 0.135(11) 0.046(4) 0.066(5) 0.000(3) -0.013(5) 0.041(5) N9 0.0655(17) 0.093(2) 0.0524(15) 0.0050(14) 0.0173(13) 0.0393(16) C18 0.0446(14) 0.0388(13) 0.0363(12) 0.0013(10) 0.0020(11) 0.0125(11) C19 0.0374(13) 0.0360(13) 0.0466(14) -0.0034(11) 0.0076(10) 0.0053(10) N10 0.076(2) 0.107(3) 0.0685(19) -0.0129(18) 0.0106(16) 0.0123(19) C20 0.0551(17) 0.0594(18) 0.0375(14) 0.0038(12) -0.0022(12) -0.0057(14) C21 0.059(2) 0.110(3) 0.064(2) -0.006(2) -0.0088(16) 0.018(2) N11 0.0581(17) 0.111(3) 0.0681(18) -0.0206(18) 0.0021(14) 0.0252(17) C22 0.0368(13) 0.0529(16) 0.0507(15) -0.0005(13) 0.0011(11) 0.0048(12) C23 0.069(2) 0.0519(17) 0.0583(18) 0.0025(14) 0.0224(15) 0.0055(15) N12 0.0308(13) 0.0763(19) 0.103(2) 0.0267(16) 0.0000(13) -0.0011(12) C24 0.0294(13) 0.0393(13) 0.0512(14) 0.0109(11) 0.0059(10) -0.0008(10) C25 0.0268(11) 0.0423(13) 0.0390(12) 0.0013(10) 0.0004(9) 0.0006(9) F1 0.0395(8) 0.0381(8) 0.0720(10) -0.0114(7) 0.0166(7) -0.0178(6) F2 0.0277(7) 0.0566(9) 0.0423(8) -0.0043(7) 0.0069(6) 0.0037(6) F3 0.0484(9) 0.0610(10) 0.0571(9) 0.0324(8) 0.0070(7) 0.0108(8) F4 0.0516(9) 0.0578(9) 0.0357(7) -0.0174(7) -0.0067(6) 0.0026(7) B1 0.0221(11) 0.0270(11) 0.0233(11) 0.0013(9) 0.0012(8) -0.0041(9) F5 0.0411(8) 0.0705(11) 0.0515(9) 0.0040(8) 0.0085(7) -0.0172(8) F6 0.0316(7) 0.0560(9) 0.0448(8) -0.0166(7) 0.0069(6) -0.0129(6) F7 0.1067(15) 0.0381(9) 0.0558(10) 0.0023(7) -0.0160(10) 0.0102(9) F8 0.0450(9) 0.0708(11) 0.0661(10) -0.0436(9) -0.0022(7) 0.0084(8) B2 0.0306(12) 0.0257(12) 0.0300(12) -0.0072(9) 0.0055(9) -0.0014(9) #================================================================== # 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 Mo1 Mo2 2.1760(2) . . yes Mo1 O1 2.0747(11) . . yes Mo1 N4 2.1411(15) . . yes Mo1 N5 2.1464(16) . . yes Mo1 N6 2.1299(15) . . yes Mo1 N8 2.6060(18) . 3_556 yes Mo2 O2 2.0820(11) . . yes Mo2 N1 2.1441(15) . . yes Mo2 N2 2.1509(15) . . yes Mo2 N3 2.1423(16) . . yes Mo2 N7 2.6130(18) . . yes F9 B3 1.359(3) . . yes F10 B3 1.388(3) . . yes F11 B3 1.311(5) . . yes F11A B3 1.681(10) . . yes F12 B3 1.452(4) . . yes F12A B3 1.350(8) . . yes O1 C1 1.263(2) . . yes O2 C1 1.266(2) . . yes F1 B1 1.377(3) . . yes F2 B1 1.394(3) . . yes F3 B1 1.384(3) . . yes F4 B1 1.379(3) . . yes F5 B2 1.393(3) . . yes F6 B2 1.395(3) . . yes F7 B2 1.374(3) . . yes F8 B2 1.378(3) . . yes N1 C2 1.135(2) . . yes N2 C4 1.135(2) . . yes N3 C6 1.138(2) . . yes N4 C8 1.135(2) . . yes N5 C10 1.136(2) . . yes N6 C12 1.136(2) . . yes N7 C14 1.124(3) . . yes N8 C16 1.134(3) . . yes N9 C18 1.130(4) . . yes N10 C20 1.122(4) . . yes N11 C22 1.134(4) . . yes C1 C1 1.515(2) . 3_555 no C2 C3 1.458(3) . . no C4 C5 1.460(3) . . no C6 C7 1.453(3) . . no C8 C9 1.455(3) . . no C10 C11 1.455(3) . . no C12 C13 1.450(3) . . no N12 C24 1.139(3) . . yes C14 C15 1.452(4) . . no C16 C17 1.457(3) . . no C3 H33 0.9800 . . no C3 H32 0.9800 . . no C3 H31 0.9800 . . no C5 H52 0.9800 . . no C5 H51 0.9800 . . no C5 H53 0.9800 . . no C7 H73 0.9800 . . no C7 H71 0.9800 . . no C7 H72 0.9800 . . no C9 H92 0.9800 . . no C9 H93 0.9800 . . no C9 H91 0.9800 . . no C11 H111 0.9800 . . no C11 H113 0.9800 . . no C11 H112 0.9800 . . no C13 H131 0.9800 . . no C13 H133 0.9800 . . no C13 H132 0.9800 . . no C15 H151 0.9800 . . no C15 H152 0.9800 . . no C15 H153 0.9800 . . no C17 H173 0.9800 . . no C17 H171 0.9800 . . no C17 H172 0.9800 . . no C18 C19 1.445(4) . . no C19 H192 0.9800 . . no C19 H191 0.9800 . . no C19 H193 0.9800 . . no C20 C21 1.453(4) . . no C21 H212 0.9800 . . no C21 H213 0.9800 . . no C21 H211 0.9800 . . no C22 C23 1.452(4) . . no C23 H232 0.9800 . . no C23 H233 0.9800 . . no C23 H231 0.9800 . . no C24 C25 1.444(3) . . no C25 H252 0.9800 . . no C25 H253 0.9800 . . no C25 H251 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mo2 Mo1 O1 91.27(3) . . . yes Mo2 Mo1 N4 99.26(4) . . . yes Mo2 Mo1 N5 101.25(4) . . . yes Mo2 Mo1 N6 98.97(4) . . . yes Mo2 Mo1 N8 177.36(4) . . 3_556 yes O1 Mo1 N4 88.09(5) . . . yes O1 Mo1 N5 167.49(5) . . . yes O1 Mo1 N6 92.64(5) . . . yes O1 Mo1 N8 86.17(5) . . 3_556 yes N4 Mo1 N5 89.66(5) . . . yes N4 Mo1 N6 161.73(6) . . . yes N4 Mo1 N8 80.04(6) . . 3_556 yes N5 Mo1 N6 85.69(6) . . . yes N5 Mo1 N8 81.32(6) . . 3_556 yes N6 Mo1 N8 81.80(6) . . 3_556 yes Mo1 Mo2 O2 90.23(3) . . . yes Mo1 Mo2 N1 99.93(4) . . . yes Mo1 Mo2 N2 101.09(4) . . . yes Mo1 Mo2 N3 100.12(4) . . . yes Mo1 Mo2 N7 169.56(4) . . . yes O2 Mo2 N1 90.55(5) . . . yes O2 Mo2 N2 168.66(5) . . . yes O2 Mo2 N3 89.34(5) . . . yes O2 Mo2 N7 79.33(5) . . . yes N1 Mo2 N2 88.07(6) . . . yes N1 Mo2 N3 159.95(6) . . . yes N1 Mo2 N7 80.00(6) . . . yes N2 Mo2 N3 88.12(6) . . . yes N2 Mo2 N7 89.35(6) . . . yes N3 Mo2 N7 80.28(6) . . . yes Mo1 O1 C1 116.98(10) . . . yes Mo2 O2 C1 117.57(10) . . . yes Mo2 N1 C2 175.29(15) . . . yes Mo2 N2 C4 177.51(15) . . . yes Mo2 N3 C6 176.92(15) . . . yes Mo1 N4 C8 177.11(15) . . . yes Mo1 N5 C10 174.77(15) . . . yes Mo1 N6 C12 173.29(15) . . . yes Mo2 N7 C14 176.14(17) . . . yes Mo1 N8 C16 175.20(17) 3_556 . . yes O1 C1 O2 123.88(15) . . . yes O1 C1 C1 118.22(14) . . 3_555 yes O2 C1 C1 117.91(14) . . 3_555 yes N1 C2 C3 179.5(2) . . . yes N2 C4 C5 178.4(2) . . . yes N3 C6 C7 179.7(2) . . . yes N4 C8 C9 179.3(2) . . . yes N5 C10 C11 179.3(2) . . . yes N6 C12 C13 179.46(19) . . . yes N7 C14 C15 178.7(3) . . . yes N8 C16 C17 178.6(2) . . . yes C2 C3 H31 110.00 . . . no C2 C3 H32 109.00 . . . no C2 C3 H33 109.00 . . . no H31 C3 H32 109.00 . . . no H31 C3 H33 109.00 . . . no H32 C3 H33 110.00 . . . no C4 C5 H51 109.00 . . . no C4 C5 H52 110.00 . . . no C4 C5 H53 109.00 . . . no H51 C5 H52 109.00 . . . no H51 C5 H53 110.00 . . . no H52 C5 H53 109.00 . . . no C6 C7 H71 109.00 . . . no C6 C7 H72 109.00 . . . no C6 C7 H73 110.00 . . . no H71 C7 H72 109.00 . . . no H71 C7 H73 109.00 . . . no H72 C7 H73 109.00 . . . no C8 C9 H91 109.00 . . . no C8 C9 H92 109.00 . . . no C8 C9 H93 109.00 . . . no H91 C9 H92 109.00 . . . no H91 C9 H93 109.00 . . . no H92 C9 H93 110.00 . . . no C10 C11 H111 109.00 . . . no C10 C11 H112 109.00 . . . no C10 C11 H113 110.00 . . . no H111 C11 H112 109.00 . . . no H111 C11 H113 109.00 . . . no H112 C11 H113 110.00 . . . no C12 C13 H131 109.00 . . . no C12 C13 H132 110.00 . . . no C12 C13 H133 109.00 . . . no H131 C13 H132 109.00 . . . no H131 C13 H133 110.00 . . . no H132 C13 H133 109.00 . . . no C14 C15 H151 109.00 . . . no C14 C15 H152 109.00 . . . no C14 C15 H153 109.00 . . . no H151 C15 H152 109.00 . . . no H151 C15 H153 109.00 . . . no H152 C15 H153 109.00 . . . no C16 C17 H171 109.00 . . . no C16 C17 H172 109.00 . . . no C16 C17 H173 109.00 . . . no H171 C17 H172 109.00 . . . no H171 C17 H173 110.00 . . . no H172 C17 H173 109.00 . . . no N9 C18 C19 179.2(3) . . . yes H191 C19 H192 109.00 . . . no H192 C19 H193 109.00 . . . no C18 C19 H192 109.00 . . . no H191 C19 H193 109.00 . . . no C18 C19 H191 110.00 . . . no C18 C19 H193 109.00 . . . no N10 C20 C21 177.3(4) . . . yes H211 C21 H213 109.00 . . . no H212 C21 H213 109.00 . . . no C20 C21 H213 110.00 . . . no C20 C21 H211 109.00 . . . no C20 C21 H212 109.00 . . . no H211 C21 H212 109.00 . . . no N11 C22 C23 178.9(3) . . . yes H232 C23 H233 109.00 . . . no H231 C23 H233 109.00 . . . no C22 C23 H232 109.00 . . . no C22 C23 H233 109.00 . . . no C22 C23 H231 109.00 . . . no H231 C23 H232 110.00 . . . no N12 C24 C25 177.9(3) . . . yes C24 C25 H252 109.00 . . . no C24 C25 H251 109.00 . . . no H251 C25 H252 110.00 . . . no H251 C25 H253 109.00 . . . no C24 C25 H253 109.00 . . . no H252 C25 H253 109.00 . . . no F11 B3 F12 109.9(3) . . . yes F11A B3 F12A 91.0(6) . . . yes F10 B3 F12A 100.8(4) . . . yes F9 B3 F10 110.1(2) . . . yes F9 B3 F11 112.8(3) . . . yes F9 B3 F12 102.0(2) . . . yes F9 B3 F11A 95.0(4) . . . yes F9 B3 F12A 146.5(5) . . . yes F10 B3 F11 112.4(3) . . . yes F10 B3 F12 109.1(2) . . . yes F10 B3 F11A 101.5(4) . . . yes F1 B1 F2 109.69(18) . . . yes F1 B1 F3 109.13(18) . . . yes F1 B1 F4 109.42(18) . . . yes F2 B1 F3 109.06(17) . . . yes F2 B1 F4 109.81(17) . . . yes F3 B1 F4 109.72(19) . . . yes F5 B2 F6 107.98(19) . . . yes F5 B2 F7 108.42(19) . . . yes F5 B2 F8 107.82(19) . . . yes F6 B2 F7 110.84(19) . . . yes F6 B2 F8 110.97(18) . . . yes F7 B2 F8 110.7(2) . . . yes # End of Crystallographic Information File # Attachment '- compound_4.cif' # CIF-file generated for KoMa13 # Compound 4 #=================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 830422' #TrackingRef '- compound_4.cif' #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 26-Apr-11 _audit_update_record ; 26-Apr-11 Updated by the Author B.B. Text writing by B.B. Checkcif OK ; #=================================================================== # 4. TEXT #=================================================================== _publ_section_abstract ; 'The treatment of the dimeric paddle-wheel (PW) compound ...' ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). WinGX (Version 1.70.01 January 2005), J. Appl. Cryst. 32, 837-838. Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen, Germany. Spek, A. L. (2008). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Stoe (2004). X-AREA, Version 1.26, Stoe & Cie GmbH, Darmstadt, Germany. ; #=================================================================== # 5. CHEMICAL DATA #=================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Mo4 N12 O8, 4(B F4), 2(C2 H3 N)' _chemical_formula_sum 'C40 H54 B4 F16 Mo4 N14 O8' _chemical_formula_weight 1589.97 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' N N 0.0061 0.0033 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6698(4) _cell_length_b 10.7944(5) _cell_length_c 15.1873(6) _cell_angle_alpha 89.095(2) _cell_angle_beta 86.007(2) _cell_angle_gamma 64.711(2) _cell_volume 1577.52(11) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.01 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6625 _exptl_absorpt_correction_T_max 0.8577 _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_special_details ; Diffractometer operator B. Bechlars scanspeed 15 s per frame dx 50 3143 frames measured in 12 data sets phi-scan with delta_phi = 0.5 omega-scans with delta_omega = 0.5 ; _publ_section_exptl_prep ; The crystal was fixed on the top of a glass capillary with perflorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Solution and refinements with the program: WinGX; Farrugia(1999). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi-and omega-rotation' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean '16 #8 for binned mode' _diffrn_standards_decay_% 0 _diffrn_reflns_number 27873 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6159 _reflns_number_gt 5979 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEXII Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker 2008b)' _computing_data_reduction 'SAINT (Bruker 2008b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2005)' _computing_publication_material 'DIAMOND (Brandenburg, 2005)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _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^ > 2\s(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^)+(0.0262P)^2^+1.8880P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6159 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.900 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.078 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== 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 Mo1 Mo 0.417464(17) 0.343617(16) 0.668373(11) 0.01558(6) Uani 1 1 d . . . Mo2 Mo 0.422297(17) 0.528494(16) 0.715467(10) 0.01544(6) Uani 1 1 d . . . O1 O 0.60356(14) 0.29469(14) 0.59162(9) 0.0178(3) Uani 1 1 d . . . O2 O 0.60675(14) 0.48673(14) 0.64038(9) 0.0180(3) Uani 1 1 d . . . O3 O 0.30800(14) 0.44560(14) 0.56116(9) 0.0178(3) Uani 1 1 d . . . O4 O 0.31247(14) 0.63713(14) 0.60952(9) 0.0176(3) Uani 1 1 d . . . N1 N 0.22861(18) 0.35578(17) 0.73734(12) 0.0212(4) Uani 1 1 d . . . N2 N 0.23571(18) 0.61599(17) 0.80129(11) 0.0201(3) Uani 1 1 d . . . N3 N 0.52695(19) 0.19877(18) 0.76613(12) 0.0233(4) Uani 1 1 d . . . N4 N 0.54112(18) 0.45441(18) 0.82963(12) 0.0222(4) Uani 1 1 d . . . N5 N 0.5765(2) 0.2347(2) 0.24306(15) 0.0359(5) Uani 1 1 d . . . N6 N 0.5886(2) 0.8829(2) 0.40016(15) 0.0337(5) Uani 1 1 d . . . C1 C 0.6585(2) 0.3789(2) 0.59273(12) 0.0169(4) Uani 1 1 d . . . C2 C 0.2159(2) 0.6440(2) 0.46990(13) 0.0181(4) Uani 1 1 d . . . C3 C 0.1084(2) 0.6001(2) 0.43334(15) 0.0262(5) Uani 1 1 d . . . H3A H 0.1296 0.5693 0.3708 0.031 Uiso 1 1 calc R . . H3B H 0.0901 0.5325 0.4704 0.031 Uiso 1 1 calc R . . C4 C -0.0037(2) 0.7475(3) 0.44669(17) 0.0357(6) Uani 1 1 d . . . H4A H -0.0797 0.7560 0.4910 0.043 Uiso 1 1 calc R . . H4B H -0.0416 0.7923 0.3910 0.043 Uiso 1 1 calc R . . C5 C 0.1023(2) 0.7937(2) 0.48216(15) 0.0249(4) Uani 1 1 d . . . H5A H 0.0808 0.8260 0.5444 0.030 Uiso 1 1 calc R . . H5B H 0.1204 0.8604 0.4441 0.030 Uiso 1 1 calc R . . C6 C 0.28002(19) 0.5721(2) 0.55317(13) 0.0166(4) Uani 1 1 d . . . C7 C 0.1295(2) 0.3661(2) 0.77599(14) 0.0223(4) Uani 1 1 d . . . C8 C 0.0023(3) 0.3807(3) 0.82641(17) 0.0334(5) Uani 1 1 d . . . H8A H 0.0231 0.3516 0.8872 0.050 Uiso 1 1 calc R . . H8B H -0.0357 0.3236 0.7993 0.050 Uiso 1 1 calc R . . H8C H -0.0659 0.4769 0.8266 0.050 Uiso 1 1 calc R . . C9 C 0.1350(2) 0.6688(2) 0.84418(13) 0.0207(4) Uani 1 1 d . . . C10 C 0.0069(2) 0.7344(2) 0.89972(16) 0.0302(5) Uani 1 1 d . . . H10A H 0.0054 0.6728 0.9475 0.045 Uiso 1 1 calc R . . H10B H -0.0727 0.7550 0.8642 0.045 Uiso 1 1 calc R . . H10C H 0.0015 0.8196 0.9250 0.045 Uiso 1 1 calc R . . C11 C 0.5793(2) 0.1224(2) 0.81910(17) 0.0313(5) Uani 1 1 d . . . C12 C 0.6421(3) 0.0258(3) 0.8890(2) 0.0554(8) Uani 1 1 d . . . H12A H 0.5786 0.0514 0.9423 0.083 Uiso 1 1 calc R . . H12B H 0.7298 0.0279 0.9020 0.083 Uiso 1 1 calc R . . H12C H 0.6599 -0.0669 0.8698 0.083 Uiso 1 1 calc R . . C13 C 0.6081(2) 0.4087(2) 0.88727(14) 0.0225(4) Uani 1 1 d . . . C14 C 0.6944(2) 0.3473(2) 0.96058(15) 0.0303(5) Uani 1 1 d . . . H14A H 0.6397 0.3259 1.0078 0.045 Uiso 1 1 calc R . . H14B H 0.7275 0.4119 0.9831 0.045 Uiso 1 1 calc R . . H14C H 0.7742 0.2629 0.9402 0.045 Uiso 1 1 calc R . . C15 C 0.6272(3) 0.1393(3) 0.20047(17) 0.0339(5) Uani 1 1 d . . . C16 C 0.6911(4) 0.0152(4) 0.1463(3) 0.0755(12) Uani 1 1 d . . . H16A H 0.6976 -0.0636 0.1819 0.113 Uiso 1 1 calc R . . H16B H 0.7845 0.0020 0.1239 0.113 Uiso 1 1 calc R . . H16C H 0.6344 0.0235 0.0965 0.113 Uiso 1 1 calc R . . C17 C 0.6285(2) 0.9621(2) 0.41542(15) 0.0265(5) Uani 1 1 d . . . C18 C 0.6796(3) 1.0633(3) 0.43599(18) 0.0390(6) Uani 1 1 d . . . H18A H 0.7594 1.0511 0.3952 0.058 Uiso 1 1 calc R . . H18B H 0.7080 1.0511 0.4967 0.058 Uiso 1 1 calc R . . H18C H 0.6056 1.1557 0.4299 0.058 Uiso 1 1 calc R . . B1 B 0.0622(4) 0.9299(3) 0.2273(2) 0.0506(9) Uani 1 1 d . . . F1 F 0.1137(3) 1.0202(2) 0.25296(16) 0.0912(8) Uani 1 1 d . . . F2 F 0.15409(17) 0.79852(17) 0.24664(13) 0.0518(4) Uani 1 1 d . . . F3 F 0.0501(2) 0.9376(2) 0.13477(13) 0.0643(5) Uani 1 1 d . . . F4 F -0.0668(2) 0.9576(3) 0.26761(15) 0.0875(8) Uani 1 1 d . . . B2 B 0.7064(3) -0.3126(3) -0.01503(18) 0.0299(5) Uani 1 1 d . . . F5 F 0.7188(2) -0.20327(15) 0.02236(10) 0.0498(4) Uani 1 1 d . . . F6 F 0.72371(17) -0.30847(18) -0.10633(10) 0.0471(4) Uani 1 1 d . . . F7 F 0.57947(19) -0.3133(2) 0.00714(14) 0.0644(5) Uani 1 1 d . . . F8 F 0.81293(19) -0.43308(16) 0.01264(13) 0.0541(4) Uani 1 1 d . . . N7 N 0.0237(4) 0.3520(3) 0.3232(2) 0.0733(10) Uani 1 1 d . . . C19 C 0.1387(4) 0.2933(3) 0.3318(2) 0.0482(7) Uani 1 1 d . . . C20 C 0.2841(4) 0.2208(5) 0.3469(4) 0.1026(18) Uani 1 1 d . . . H20A H 0.3031 0.2562 0.4009 0.154 Uiso 1 1 calc R . . H20B H 0.3400 0.2339 0.2967 0.154 Uiso 1 1 calc R . . H20C H 0.3082 0.1229 0.3532 0.154 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 Mo1 0.01592(9) 0.01460(9) 0.01664(9) 0.00094(6) 0.00157(6) -0.00733(7) Mo2 0.01631(9) 0.01562(9) 0.01457(9) -0.00029(6) 0.00086(6) -0.00726(7) O1 0.0178(7) 0.0172(7) 0.0194(7) -0.0007(5) 0.0014(5) -0.0088(6) O2 0.0181(7) 0.0188(7) 0.0187(7) -0.0008(5) 0.0007(5) -0.0097(6) O3 0.0181(7) 0.0176(7) 0.0187(7) 0.0004(5) -0.0005(5) -0.0087(6) O4 0.0183(7) 0.0170(7) 0.0177(7) 0.0010(5) -0.0004(5) -0.0079(6) N1 0.0224(9) 0.0184(8) 0.0228(9) 0.0009(7) 0.0018(7) -0.0094(7) N2 0.0203(9) 0.0204(8) 0.0195(8) 0.0001(7) -0.0010(7) -0.0085(7) N3 0.0233(9) 0.0198(8) 0.0267(9) 0.0039(7) -0.0002(7) -0.0094(7) N4 0.0223(9) 0.0240(9) 0.0202(9) -0.0008(7) 0.0005(7) -0.0100(7) N5 0.0379(12) 0.0273(11) 0.0443(12) -0.0062(9) 0.0021(10) -0.0161(9) N6 0.0332(11) 0.0284(10) 0.0415(12) -0.0083(9) 0.0027(9) -0.0157(9) C1 0.0160(9) 0.0190(9) 0.0157(9) 0.0042(7) -0.0026(7) -0.0074(8) C2 0.0146(9) 0.0210(10) 0.0180(9) 0.0008(7) -0.0004(7) -0.0071(8) C3 0.0200(10) 0.0374(12) 0.0259(11) 0.0046(9) -0.0058(9) -0.0163(9) C4 0.0168(10) 0.0462(15) 0.0390(14) 0.0079(11) -0.0034(10) -0.0087(10) C5 0.0152(10) 0.0241(11) 0.0274(11) 0.0042(8) 0.0013(8) -0.0015(8) C6 0.0122(8) 0.0199(9) 0.0175(9) 0.0005(7) 0.0033(7) -0.0073(7) C7 0.0240(11) 0.0191(10) 0.0244(10) -0.0012(8) 0.0019(9) -0.0102(8) C8 0.0290(12) 0.0409(13) 0.0358(13) -0.0032(10) 0.0101(10) -0.0217(11) C9 0.0226(11) 0.0194(9) 0.0208(10) 0.0019(8) -0.0034(8) -0.0093(8) C10 0.0215(11) 0.0314(12) 0.0302(12) -0.0030(9) 0.0061(9) -0.0053(9) C11 0.0282(12) 0.0269(11) 0.0373(13) 0.0087(10) -0.0023(10) -0.0107(10) C12 0.0485(17) 0.0467(17) 0.0586(19) 0.0324(15) -0.0093(14) -0.0089(14) C13 0.0225(10) 0.0225(10) 0.0223(11) -0.0015(8) 0.0014(9) -0.0098(8) C14 0.0309(12) 0.0317(12) 0.0266(11) 0.0036(9) -0.0097(9) -0.0107(10) C15 0.0340(13) 0.0321(13) 0.0415(14) -0.0027(11) -0.0040(11) -0.0193(11) C16 0.079(3) 0.059(2) 0.083(3) -0.043(2) 0.008(2) -0.026(2) C17 0.0270(11) 0.0229(10) 0.0272(11) -0.0032(9) 0.0046(9) -0.0093(9) C18 0.0514(16) 0.0328(13) 0.0423(14) -0.0090(11) 0.0081(12) -0.0284(12) B1 0.056(2) 0.0348(16) 0.053(2) -0.0019(14) 0.0196(16) -0.0156(15) F1 0.153(2) 0.0538(12) 0.0820(16) -0.0185(11) 0.0191(16) -0.0625(15) F2 0.0389(9) 0.0385(9) 0.0770(12) -0.0064(8) -0.0023(8) -0.0155(7) F3 0.0773(14) 0.0559(11) 0.0529(11) 0.0011(9) 0.0181(10) -0.0253(10) F4 0.0454(11) 0.0996(17) 0.0696(14) 0.0310(12) 0.0227(10) 0.0100(11) B2 0.0300(13) 0.0276(13) 0.0331(14) 0.0040(10) 0.0006(11) -0.0138(11) F5 0.0832(13) 0.0299(8) 0.0370(8) -0.0043(6) -0.0033(8) -0.0248(8) F6 0.0497(9) 0.0625(11) 0.0347(8) -0.0088(7) 0.0022(7) -0.0297(8) F7 0.0396(10) 0.0832(14) 0.0718(13) 0.0056(11) 0.0136(9) -0.0304(10) F8 0.0540(10) 0.0324(8) 0.0745(12) 0.0111(8) -0.0186(9) -0.0154(8) N7 0.084(2) 0.0383(14) 0.099(2) 0.0052(15) -0.058(2) -0.0198(15) C19 0.063(2) 0.0383(15) 0.0408(15) 0.0038(12) -0.0083(14) -0.0187(14) C20 0.042(2) 0.111(4) 0.126(4) 0.026(3) 0.025(2) -0.010(2) #=================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mo1 O3 2.0825(14) . ? Mo1 O1 2.0932(14) . ? Mo1 N3 2.1497(18) . ? Mo1 Mo2 2.1529(2) . ? Mo1 N1 2.1585(18) . ? Mo2 O2 2.0790(14) . ? Mo2 O4 2.0895(14) . ? Mo2 N2 2.1507(18) . ? Mo2 N4 2.1562(18) . ? O1 C1 1.276(2) . ? O2 C1 1.267(2) . ? O3 C6 1.272(2) . ? O4 C6 1.270(2) . ? N1 C7 1.136(3) . ? N2 C9 1.138(3) . ? N3 C11 1.135(3) . ? N4 C13 1.137(3) . ? N5 C15 1.126(3) . ? N6 C17 1.139(3) . ? C1 C2 1.519(3) 2_666 ? C2 C6 1.518(3) . ? C2 C1 1.519(3) 2_666 ? C2 C3 1.553(3) . ? C2 C5 1.556(3) . ? C3 C4 1.535(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.548(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C8 1.459(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.454(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.460(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.458(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.454(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.460(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? B1 F4 1.377(4) . ? B1 F2 1.378(4) . ? B1 F1 1.379(4) . ? B1 F3 1.417(4) . ? B2 F7 1.376(3) . ? B2 F5 1.378(3) . ? B2 F6 1.389(3) . ? B2 F8 1.395(3) . ? N7 C19 1.131(4) . ? C19 C20 1.442(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 O3 Mo1 O1 89.24(5) . . ? O3 Mo1 N3 166.92(6) . . ? O1 Mo1 N3 90.61(6) . . ? O3 Mo1 Mo2 91.31(4) . . ? O1 Mo1 Mo2 90.66(4) . . ? N3 Mo1 Mo2 101.77(5) . . ? O3 Mo1 N1 90.80(6) . . ? O1 Mo1 N1 168.54(6) . . ? N3 Mo1 N1 86.77(7) . . ? Mo2 Mo1 N1 100.79(5) . . ? O2 Mo2 O4 89.02(5) . . ? O2 Mo2 N2 166.20(6) . . ? O4 Mo2 N2 90.13(6) . . ? O2 Mo2 Mo1 91.37(4) . . ? O4 Mo2 Mo1 90.69(4) . . ? N2 Mo2 Mo1 102.41(5) . . ? O2 Mo2 N4 88.71(6) . . ? O4 Mo2 N4 168.12(6) . . ? N2 Mo2 N4 89.30(6) . . ? Mo1 Mo2 N4 101.03(5) . . ? C1 O1 Mo1 117.70(12) . . ? C1 O2 Mo2 117.96(12) . . ? C6 O3 Mo1 117.76(12) . . ? C6 O4 Mo2 118.04(12) . . ? C7 N1 Mo1 177.13(17) . . ? C9 N2 Mo2 176.23(17) . . ? C11 N3 Mo1 176.95(18) . . ? C13 N4 Mo2 176.15(17) . . ? O2 C1 O1 122.27(18) . . ? O2 C1 C2 118.12(17) . 2_666 ? O1 C1 C2 119.45(17) . 2_666 ? C6 C2 C1 103.35(15) . 2_666 ? C6 C2 C3 115.27(16) . . ? C1 C2 C3 115.32(17) 2_666 . ? C6 C2 C5 116.17(16) . . ? C1 C2 C5 117.03(17) 2_666 . ? C3 C2 C5 90.21(16) . . ? C4 C3 C2 89.58(17) . . ? C4 C3 H3A 113.7 . . ? C2 C3 H3A 113.7 . . ? C4 C3 H3B 113.7 . . ? C2 C3 H3B 113.7 . . ? H3A C3 H3B 111.0 . . ? C3 C4 C5 91.20(16) . . ? C3 C4 H4A 113.4 . . ? C5 C4 H4A 113.4 . . ? C3 C4 H4B 113.4 . . ? C5 C4 H4B 113.4 . . ? H4A C4 H4B 110.7 . . ? C4 C5 C2 89.01(17) . . ? C4 C5 H5A 113.8 . . ? C2 C5 H5A 113.8 . . ? C4 C5 H5B 113.8 . . ? C2 C5 H5B 113.8 . . ? H5A C5 H5B 111.0 . . ? O4 C6 O3 122.16(18) . . ? O4 C6 C2 119.13(17) . . ? O3 C6 C2 118.54(17) . . ? N1 C7 C8 179.2(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 179.1(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 178.0(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 178.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C16 179.0(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C18 179.4(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? F4 B1 F2 109.4(3) . . ? F4 B1 F1 112.7(3) . . ? F2 B1 F1 109.0(3) . . ? F4 B1 F3 107.9(3) . . ? F2 B1 F3 108.2(3) . . ? F1 B1 F3 109.5(3) . . ? F7 B2 F5 112.5(2) . . ? F7 B2 F6 108.6(2) . . ? F5 B2 F6 109.7(2) . . ? F7 B2 F8 110.1(2) . . ? F5 B2 F8 108.2(2) . . ? F6 B2 F8 107.7(2) . . ? N7 C19 C20 177.4(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? # End of Crystallographic Information File