# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1688 # CIF-file generated for WAND 4022-143 # =================================================================== data_global # =================================================================== # 0. AUDIT DETAILS _audit_creation_date 17-Jan-99 _audit_creation_method 'PLATON option' _audit_update_record ; 25-May-99 Updated by the Author E.H. ; # =================================================================== # 1. SUBMISSION DETAILS # =================================================================== # Name and address of author for X-ray correspondence _publ_contact_author ; Dr. Eberhardt Herdtweck Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; _publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de' _publ_contact_author_fax ' 089 289 13473' _publ_contact_author_phone '089 289 13143' _publ_requested_journal ' J. Chem.Soc., Dalton Trans. ' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission: June 1999 Dear Debbie Middleton, the original manuscript was sent to ' J. Chem.Soc., Dalton Trans. ' Paper ref. 9/04742E Please deposit and send deposit number. Sincerely Eberhardt Herdtweck ; # =================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) # =================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # =================================================================== # 3. TITLE AND AUTHOR LIST # =================================================================== _publ_section_title ; Dimolybdenum(II) Complexes Linked by Axial Cyano Bridges to Organic and Organometallic Ligands: Syntheses, Structures, and Characterization ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Xue, W.-M.' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; 'K\"uhn, F.' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; 'Zhang, G.' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; 'Herdtweck, E.' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; 'Raudaschl-Sieber, G.' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstrasse 4 D-85747 Garching bei M\"unchen ; # ======================================================================= # 4. TEXT # ======================================================================= _publ_section_abstract ; none ; # Insert blank lines between paragraphs _publ_section_comment ; none ; _publ_section_experimental ; none ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Spek, A.L. (1990). Acta Cryst. A46, C34 ; _publ_section_figure_captions ; none ; _publ_section_acknowledgements ; none ; _publ_section_table_legends ; none ; # =================================================================== data_WAND-4022-143 # =================================================================== _chemical_name_systematic ; not known ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H62 Mo2 N4 O4 P4, 2(B F4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C72 H62 B2 F8 Mo2 N4 O4 P4' _chemical_formula_weight 1536.64 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' 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' 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 13.3057(3) _cell_length_b 16.4102(3) _cell_length_c 16.3923(4) _cell_angle_alpha 90 _cell_angle_beta 103.550(1) _cell_angle_gamma 90 _cell_volume 3479.62(13) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _cell_measurement_reflns_used 13911 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.11 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8843 _exptl_absorpt_correction_T_max 0.9396 _exptl_absorpt_process_details ; Otwinowski, Z.; and Minor, W. "Processing of X-ray Diffraction Data Collected in Oscillation Mode", Metthods in Enzymology 276, 1996. Carter W. C.; Sweet, Jr. & R. M.; Eds., Academic Press, (USA). ; _exptl_special_details ; Diffractometer operator Herdtweck, E. ; _publ_section_exptl_prep ; the crystals were handled in air, fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward. ; # =================================================================== # 7. EXPERIMENTAL DATA # =================================================================== _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kappa CCD (Nonius)' _diffrn_measurement_method ' rotation ' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 14627 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.11 _reflns_number_total 7325 _reflns_number_gt 6134 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Nonius- CCD-Software. ; _computing_data_collection 'Kappa CCD (Nonius)' _computing_cell_refinement 'Denzo and HKL' _computing_data_reduction 'Denzo and HKL' _computing_structure_solution 'SIR92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek, 1999)' _computing_publication_material 'PLATON (Spek, 1999)' # =================================================================== # 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+2.5525P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_number_reflns 7325 _refine_ls_number_parameters 557 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.481 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.065 # =================================================================== # 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 Mo Mo Uani 0.06978(1) 0.53445(1) 0.51562(1) 1.000 0.0152(1) P1 P Uani 0.16201(4) 0.46564(3) 0.41257(3) 1.000 0.0166(2) P2 P Uani -0.03752(4) 0.38626(3) 0.35673(3) 1.000 0.0178(2) O1 O Uani 0.14159(11) 0.44864(9) 0.60506(9) 1.000 0.0196(4) O2 O Uani -0.00415(11) 0.37672(9) 0.57329(9) 1.000 0.0199(5) N2 N Uani 0.23532(17) 0.62232(15) 0.55126(14) 1.000 0.0432(8) N1 N Uani 0.08207(14) 0.40589(11) 0.34146(11) 1.000 0.0215(6) C1 C Uani 0.1351(2) 0.32411(18) 0.68022(19) 1.000 0.0350(9) C2 C Uani 0.08831(17) 0.38695(14) 0.61603(14) 1.000 0.0219(7) C3 C Uani 0.1194(2) 0.36594(18) 0.27328(18) 1.000 0.0318(8) C11 C Uani 0.22903(16) 0.53187(13) 0.35355(13) 1.000 0.0179(6) C12 C Uani 0.30662(17) 0.50131(15) 0.31713(14) 1.000 0.0216(7) C13 C Uani 0.35687(18) 0.55311(15) 0.27264(15) 1.000 0.0263(7) C14 C Uani 0.33306(18) 0.63493(15) 0.26659(15) 1.000 0.0269(7) C15 C Uani 0.25807(18) 0.66614(15) 0.30368(14) 1.000 0.0246(7) C16 C Uani 0.20481(17) 0.61484(14) 0.34637(13) 1.000 0.0209(7) C21 C Uani 0.26395(17) 0.39822(14) 0.46756(14) 1.000 0.0234(7) C22 C Uani 0.2445(2) 0.31615(16) 0.47824(18) 1.000 0.0348(9) C23 C Uani 0.3217(3) 0.26646(19) 0.5261(2) 1.000 0.0470(11) C24 C Uani 0.4169(3) 0.2986(2) 0.56231(18) 1.000 0.0481(10) C25 C Uani 0.4370(2) 0.3798(2) 0.55267(17) 1.000 0.0448(10) C26 C Uani 0.3609(2) 0.42940(18) 0.50638(16) 1.000 0.0329(9) C31 C Uani -0.12474(17) 0.41729(14) 0.25878(14) 1.000 0.0224(7) C32 C Uani -0.0945(2) 0.47450(17) 0.20695(17) 1.000 0.0370(9) C33 C Uani -0.1629(3) 0.4984(2) 0.13314(19) 1.000 0.0503(11) C34 C Uani -0.2612(2) 0.46710(19) 0.11124(18) 1.000 0.0435(10) C35 C Uani -0.2931(2) 0.41205(18) 0.16319(17) 1.000 0.0378(9) C36 C Uani -0.22561(18) 0.38713(16) 0.23665(16) 1.000 0.0282(8) C41 C Uani -0.04999(16) 0.27569(13) 0.35603(14) 1.000 0.0204(7) C42 C Uani -0.07668(17) 0.23086(14) 0.28142(15) 1.000 0.0237(7) C43 C Uani -0.07713(19) 0.14654(15) 0.28322(17) 1.000 0.0302(8) C44 C Uani -0.0500(2) 0.10577(17) 0.35887(18) 1.000 0.0354(9) C45 C Uani -0.0259(2) 0.14896(16) 0.43333(18) 1.000 0.0389(10) C46 C Uani -0.0269(2) 0.23364(15) 0.43227(16) 1.000 0.0300(8) C50 C Uani 0.29552(19) 0.67256(17) 0.55451(16) 1.000 0.0350(8) C51 C Uani 0.37324(18) 0.73439(16) 0.56035(16) 1.000 0.0318(8) C52 C Uani 0.3627(2) 0.79520(17) 0.50043(17) 1.000 0.0345(8) C53 C Uani 0.4390(2) 0.85353(17) 0.50673(18) 1.000 0.0348(8) C54 C Uani 0.52571(19) 0.85172(16) 0.57399(16) 1.000 0.0327(8) C55 C Uani 0.5351(2) 0.79004(18) 0.63373(18) 1.000 0.0407(9) C56 C Uani 0.4599(2) 0.73132(19) 0.62693(18) 1.000 0.0400(9) C57 C Uani 0.6052(2) 0.91259(17) 0.58177(17) 1.000 0.0392(9) C58 C Uani 0.6732(3) 0.96041(19) 0.5893(2) 1.000 0.0480(10) F1 F Uani 0.30624(14) 0.36352(11) 0.17975(13) 1.000 0.0651(7) F2 F Uani 0.41039(16) 0.29636(10) 0.11360(12) 1.000 0.0639(7) F3 F Uani 0.37883(16) 0.43119(11) 0.09000(11) 1.000 0.0628(7) F4 F Uani 0.47573(15) 0.39173(14) 0.21283(14) 1.000 0.0766(8) B B Uani 0.3935(2) 0.36933(18) 0.14881(19) 1.000 0.0311(9) H11 H Uiso 0.163(3) 0.348(2) 0.733(2) 1.000 0.079(12) H12 H Uiso 0.086(3) 0.292(2) 0.689(2) 1.000 0.070(11) H13 H Uiso 0.189(3) 0.300(2) 0.664(2) 1.000 0.080(12) H31 H Uiso 0.141(2) 0.4060(17) 0.2393(17) 1.000 0.035(7) H32 H Uiso 0.177(2) 0.3345(18) 0.2952(18) 1.000 0.048(9) H33 H Uiso 0.066(2) 0.3351(18) 0.2402(18) 1.000 0.046(8) H121 H Uiso 0.3240(17) 0.4458(14) 0.3223(13) 1.000 0.015(6) H131 H Uiso 0.4041(19) 0.5314(14) 0.2463(15) 1.000 0.023(6) H141 H Uiso 0.3669(18) 0.6690(15) 0.2363(15) 1.000 0.025(6) H151 H Uiso 0.2416(19) 0.7201(16) 0.2988(15) 1.000 0.026(7) H161 H Uiso 0.1526(17) 0.6365(13) 0.3717(14) 1.000 0.017(6) H221 H Uiso 0.181(2) 0.2947(15) 0.4545(15) 1.000 0.026(7) H231 H Uiso 0.304(2) 0.2120(19) 0.5300(19) 1.000 0.049(9) H241 H Uiso 0.469(2) 0.2654(18) 0.5941(19) 1.000 0.052(9) H251 H Uiso 0.504(3) 0.4020(19) 0.577(2) 1.000 0.062(10) H261 H Uiso 0.3741(19) 0.4845(16) 0.5012(16) 1.000 0.030(7) H321 H Uiso -0.028(2) 0.4960(19) 0.2198(19) 1.000 0.052(9) H331 H Uiso -0.141(3) 0.536(2) 0.099(2) 1.000 0.065(10) H341 H Uiso -0.306(2) 0.4830(17) 0.0603(19) 1.000 0.047(8) H351 H Uiso -0.360(2) 0.3926(17) 0.1463(18) 1.000 0.044(8) H361 H Uiso -0.246(2) 0.3503(16) 0.2743(17) 1.000 0.035(7) H421 H Uiso -0.0976(18) 0.2588(15) 0.2284(16) 1.000 0.024(6) H431 H Uiso -0.098(2) 0.1166(16) 0.2335(17) 1.000 0.032(7) H441 H Uiso -0.051(2) 0.0503(17) 0.3615(16) 1.000 0.031(7) H451 H Uiso -0.009(2) 0.1226(16) 0.4835(18) 1.000 0.039(8) H461 H Uiso -0.012(2) 0.2631(15) 0.4851(17) 1.000 0.033(7) H521 H Uiso 0.303(2) 0.7968(16) 0.4549(17) 1.000 0.040(8) H531 H Uiso 0.430(2) 0.8984(19) 0.4666(19) 1.000 0.051(9) H551 H Uiso 0.594(2) 0.7888(16) 0.6784(18) 1.000 0.041(8) H561 H Uiso 0.469(2) 0.6916(18) 0.6669(18) 1.000 0.045(8) H581 H Uiso 0.727(3) 0.998(2) 0.595(2) 1.000 0.061(10) 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 Mo 0.0146(1) 0.0152(1) 0.0168(1) -0.0020(1) 0.0057(1) -0.0023(1) P1 0.0170(3) 0.0166(3) 0.0177(3) -0.0021(2) 0.0071(2) -0.0018(2) P2 0.0189(3) 0.0172(3) 0.0191(3) -0.0032(2) 0.0079(2) -0.0033(2) O1 0.0174(7) 0.0210(8) 0.0206(8) -0.0011(6) 0.0048(6) -0.0004(6) O2 0.0208(8) 0.0179(8) 0.0219(8) 0.0006(6) 0.0066(6) -0.0020(6) N2 0.0346(12) 0.0601(16) 0.0371(13) -0.0146(12) 0.0130(10) -0.0232(12) N1 0.0223(9) 0.0223(10) 0.0233(10) -0.0081(8) 0.0119(8) -0.0063(8) C1 0.0324(15) 0.0330(16) 0.0378(16) 0.0129(13) 0.0043(12) 0.0039(12) C2 0.0237(11) 0.0221(12) 0.0212(11) -0.0009(9) 0.0077(9) 0.0027(9) C3 0.0308(14) 0.0377(16) 0.0326(14) -0.0190(13) 0.0190(12) -0.0123(12) C11 0.0164(10) 0.0197(12) 0.0180(10) -0.0011(9) 0.0047(8) -0.0045(8) C12 0.0224(11) 0.0209(13) 0.0224(11) -0.0046(10) 0.0072(9) -0.0034(9) C13 0.0218(11) 0.0338(14) 0.0264(12) -0.0027(10) 0.0122(10) -0.0039(10) C14 0.0243(12) 0.0314(14) 0.0269(12) 0.0043(10) 0.0101(10) -0.0081(10) C15 0.0254(12) 0.0223(13) 0.0253(12) 0.0014(10) 0.0044(9) -0.0039(10) C16 0.0195(11) 0.0242(12) 0.0197(11) -0.0018(9) 0.0060(9) -0.0008(9) C21 0.0282(12) 0.0252(13) 0.0199(11) 0.0001(9) 0.0117(9) 0.0060(9) C22 0.0369(15) 0.0273(14) 0.0453(16) 0.0058(12) 0.0199(12) 0.0061(12) C23 0.067(2) 0.0321(17) 0.0513(19) 0.0145(14) 0.0328(17) 0.0204(15) C24 0.0501(19) 0.067(2) 0.0287(15) 0.0138(15) 0.0125(13) 0.0319(17) C25 0.0387(16) 0.063(2) 0.0290(14) 0.0016(14) 0.0004(12) 0.0153(15) C26 0.0315(14) 0.0379(17) 0.0272(13) -0.0022(12) 0.0024(10) 0.0037(12) C31 0.0279(12) 0.0211(12) 0.0198(11) -0.0044(9) 0.0091(9) 0.0009(9) C32 0.0389(15) 0.0429(17) 0.0290(14) 0.0069(12) 0.0077(11) -0.0104(13) C33 0.059(2) 0.058(2) 0.0335(16) 0.0184(15) 0.0098(14) -0.0042(16) C34 0.0454(17) 0.0523(19) 0.0295(14) 0.0062(13) 0.0024(13) 0.0117(14) C35 0.0262(13) 0.0473(18) 0.0371(15) -0.0004(13) 0.0019(11) 0.0083(12) C36 0.0255(12) 0.0307(14) 0.0292(13) 0.0002(11) 0.0083(10) 0.0027(10) C41 0.0183(10) 0.0182(12) 0.0273(12) -0.0027(9) 0.0105(9) -0.0036(8) C42 0.0221(11) 0.0225(13) 0.0277(13) -0.0059(10) 0.0083(9) -0.0017(9) C43 0.0288(13) 0.0247(14) 0.0406(15) -0.0137(12) 0.0149(11) -0.0046(10) C44 0.0428(15) 0.0179(14) 0.0527(18) -0.0063(12) 0.0256(13) -0.0067(11) C45 0.0611(19) 0.0250(15) 0.0371(16) 0.0038(12) 0.0244(14) -0.0030(13) C46 0.0422(15) 0.0225(14) 0.0286(13) -0.0053(11) 0.0149(11) -0.0072(11) C50 0.0290(13) 0.0483(17) 0.0295(13) -0.0143(12) 0.0102(11) -0.0115(12) C51 0.0258(12) 0.0393(16) 0.0318(13) -0.0129(12) 0.0098(10) -0.0109(11) C52 0.0264(13) 0.0396(16) 0.0347(15) -0.0105(12) 0.0014(11) 0.0002(11) C53 0.0359(14) 0.0296(15) 0.0367(15) -0.0047(12) 0.0041(12) -0.0013(11) C54 0.0308(13) 0.0317(15) 0.0355(14) -0.0077(11) 0.0073(11) -0.0079(11) C55 0.0321(14) 0.0516(18) 0.0329(15) 0.0000(13) -0.0037(12) -0.0192(13) C56 0.0402(16) 0.0469(18) 0.0310(15) 0.0009(13) 0.0048(12) -0.0155(13) C57 0.0393(15) 0.0341(15) 0.0402(15) -0.0014(12) 0.0015(12) -0.0074(12) C58 0.0478(18) 0.0406(18) 0.0492(18) 0.0078(14) -0.0014(14) -0.0167(15) F1 0.0656(12) 0.0502(11) 0.1003(15) -0.0345(11) 0.0611(12) -0.0220(9) F2 0.0975(15) 0.0335(10) 0.0771(13) -0.0007(9) 0.0535(12) 0.0232(9) F3 0.0983(15) 0.0445(11) 0.0512(11) 0.0148(9) 0.0288(10) 0.0286(10) F4 0.0484(11) 0.0841(15) 0.0820(15) 0.0053(12) -0.0153(10) 0.0044(10) B 0.0321(15) 0.0308(16) 0.0338(15) 0.0015(13) 0.0148(12) 0.0057(12) # =================================================================== # 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 P1 2.5703(5) . . yes Mo O1 2.0950(15) . . yes Mo N2 2.582(2) . . yes Mo C2 2.905(2) . . yes Mo Mo 2.1315(3) . 3_566 yes Mo P2 2.5839(5) . 3_566 yes Mo O2 2.1012(15) . 3_566 yes Mo C2 2.936(2) . 3_566 yes P1 N1 1.6943(19) . . yes P1 C11 1.821(2) . . yes P1 C21 1.818(2) . . yes P2 N1 1.699(2) . . yes P2 C31 1.820(2) . . yes P2 C41 1.822(2) . . yes F1 B 1.375(3) . . yes F2 B 1.371(3) . . yes F3 B 1.382(3) . . yes F4 B 1.377(4) . . yes O1 C2 1.273(3) . . yes O2 C2 1.276(3) . . yes N2 C50 1.142(4) . . yes N1 C3 1.478(3) . . yes C1 C2 1.500(4) . . no C11 C12 1.401(3) . . no C11 C16 1.398(3) . . no C12 C13 1.389(3) . . no C13 C14 1.378(3) . . no C14 C15 1.383(3) . . no C15 C16 1.390(3) . . no C21 C26 1.395(4) . . no C21 C22 1.390(4) . . no C22 C23 1.399(4) . . no C23 C24 1.372(5) . . no C24 C25 1.375(5) . . no C25 C26 1.380(4) . . no C31 C32 1.388(4) . . no C31 C36 1.396(3) . . no C32 C33 1.389(4) . . no C33 C34 1.372(5) . . no C34 C35 1.375(4) . . no C35 C36 1.385(4) . . no C41 C42 1.400(3) . . no C41 C46 1.397(3) . . no C42 C43 1.384(3) . . no C43 C44 1.381(4) . . no C44 C45 1.383(4) . . no C45 C46 1.390(4) . . no C50 C51 1.436(4) . . no C51 C52 1.384(4) . . no C51 C56 1.391(4) . . no C52 C53 1.381(4) . . no C53 C54 1.397(4) . . no C54 C57 1.439(4) . . no C54 C55 1.393(4) . . no C55 C56 1.375(4) . . no C57 C58 1.182(5) . . no C1 H13 0.91(4) . . no C1 H11 0.94(3) . . no C1 H12 0.88(4) . . no C3 H33 0.94(3) . . no C3 H32 0.92(3) . . no C3 H31 0.95(3) . . no C12 H121 0.94(2) . . no C13 H131 0.91(3) . . no C14 H141 0.93(2) . . no C15 H151 0.91(3) . . no C16 H161 0.96(2) . . no C22 H221 0.91(3) . . no C23 H231 0.93(3) . . no C24 H241 0.94(3) . . no C25 H251 0.96(4) . . no C26 H261 0.93(3) . . no C32 H321 0.93(3) . . no C33 H331 0.92(3) . . no C34 H341 0.94(3) . . no C35 H351 0.92(3) . . no C36 H361 0.95(3) . . no C42 H421 0.96(3) . . no C43 H431 0.94(3) . . no C44 H441 0.91(3) . . no C45 H451 0.91(3) . . no C46 H461 0.97(3) . . no C52 H521 0.95(3) . . no C53 H531 0.98(3) . . no C55 H551 0.94(3) . . no C56 H561 0.91(3) . . no C58 H581 0.93(4) . . 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 P1 Mo O1 87.42(4) . . . yes P1 Mo N2 83.15(5) . . . yes P1 Mo C2 90.92(5) . . . yes Mo Mo P1 97.60(1) 3_566 . . yes P1 Mo P2 161.61(2) . . 3_566 yes P1 Mo O2 91.93(4) . . 3_566 yes P1 Mo C2 94.59(5) . . 3_566 yes O1 Mo N2 89.54(7) . . . yes O1 Mo C2 22.95(6) . . . yes Mo Mo O1 92.31(4) 3_566 . . yes P2 Mo O1 84.65(4) 3_566 . . yes O1 Mo O2 177.42(6) . . 3_566 yes O1 Mo C2 160.14(6) . . 3_566 yes N2 Mo C2 112.48(7) . . . yes Mo Mo N2 178.03(6) 3_566 . . yes P2 Mo N2 80.23(5) 3_566 . . yes O2 Mo N2 87.90(7) 3_566 . . yes N2 Mo C2 110.32(7) . . 3_566 yes Mo Mo C2 69.37(5) 3_566 . . yes P2 Mo C2 88.22(5) 3_566 . . yes O2 Mo C2 159.61(6) 3_566 . . yes C2 Mo C2 137.20(6) . . 3_566 yes Mo Mo P2 99.27(1) 3_566 . 3_566 yes Mo Mo O2 90.25(4) 3_566 . 3_566 yes Mo Mo C2 67.83(5) 3_566 . 3_566 yes P2 Mo O2 95.25(4) 3_566 . 3_566 yes P2 Mo C2 98.49(5) 3_566 . 3_566 yes O2 Mo C2 22.42(6) 3_566 . 3_566 yes Mo P1 N1 112.77(7) . . . yes Mo P1 C11 117.10(7) . . . yes Mo P1 C21 110.93(7) . . . yes N1 P1 C11 106.65(9) . . . yes N1 P1 C21 105.32(10) . . . yes C11 P1 C21 103.02(10) . . . yes N1 P2 C31 104.05(10) . . . yes N1 P2 C41 105.96(10) . . . yes Mo P2 N1 111.28(6) 3_566 . . yes C31 P2 C41 103.58(10) . . . yes Mo P2 C31 112.40(8) 3_566 . . yes Mo P2 C41 118.32(7) 3_566 . . yes Mo O1 C2 117.11(14) . . . yes Mo O2 C2 118.69(14) 3_566 . . yes Mo N2 C50 164.9(2) . . . yes P1 N1 P2 117.85(11) . . . yes P1 N1 C3 120.58(16) . . . yes P2 N1 C3 121.30(16) . . . yes Mo C2 O1 39.94(10) . . . yes Mo C2 O2 81.70(12) . . . yes Mo C2 C1 159.43(17) . . . yes Mo C2 Mo 42.80(3) . . 3_566 yes O1 C2 O2 121.6(2) . . . yes O1 C2 C1 119.5(2) . . . yes Mo C2 O1 82.74(13) 3_566 . . yes O2 C2 C1 118.9(2) . . . yes Mo C2 O2 38.89(10) 3_566 . . yes Mo C2 C1 157.76(17) 3_566 . . yes P1 C11 C12 120.94(17) . . . yes P1 C11 C16 119.61(16) . . . yes C12 C11 C16 119.4(2) . . . no C11 C12 C13 119.9(2) . . . no C12 C13 C14 120.2(2) . . . no C13 C14 C15 120.4(2) . . . no C14 C15 C16 120.2(2) . . . no C11 C16 C15 119.8(2) . . . no P1 C21 C22 120.85(19) . . . yes P1 C21 C26 120.39(19) . . . yes C22 C21 C26 118.5(2) . . . no C21 C22 C23 120.1(3) . . . no C22 C23 C24 120.0(3) . . . no C23 C24 C25 120.5(3) . . . no C24 C25 C26 119.8(3) . . . no C21 C26 C25 121.0(3) . . . no P2 C31 C32 120.87(19) . . . yes P2 C31 C36 120.37(18) . . . yes C32 C31 C36 118.7(2) . . . no C31 C32 C33 120.0(3) . . . no C32 C33 C34 120.8(3) . . . no C33 C34 C35 119.8(3) . . . no C34 C35 C36 120.1(3) . . . no C31 C36 C35 120.6(2) . . . no P2 C41 C42 122.21(17) . . . yes P2 C41 C46 119.05(17) . . . yes C42 C41 C46 118.7(2) . . . no C41 C42 C43 120.5(2) . . . no C42 C43 C44 120.1(2) . . . no C43 C44 C45 120.2(3) . . . no C44 C45 C46 120.1(3) . . . no C41 C46 C45 120.3(2) . . . no N2 C50 C51 178.4(3) . . . yes C50 C51 C52 120.7(2) . . . no C50 C51 C56 118.6(2) . . . no C52 C51 C56 120.7(2) . . . no C51 C52 C53 119.7(3) . . . no C52 C53 C54 120.1(3) . . . no C53 C54 C55 119.4(2) . . . no C53 C54 C57 120.6(2) . . . no C55 C54 C57 119.9(2) . . . no C54 C55 C56 120.6(3) . . . no C51 C56 C55 119.5(3) . . . no C54 C57 C58 177.5(3) . . . no C2 C1 H11 112(2) . . . no C2 C1 H12 109(2) . . . no C2 C1 H13 109(2) . . . no H11 C1 H12 104(3) . . . no H11 C1 H13 106(3) . . . no H12 C1 H13 117(3) . . . no N1 C3 H31 109.8(17) . . . no N1 C3 H32 110.4(18) . . . no N1 C3 H33 109.5(17) . . . no H31 C3 H32 106(2) . . . no H31 C3 H33 109(2) . . . no H32 C3 H33 112(3) . . . no C11 C12 H121 120.0(14) . . . no C13 C12 H121 120.2(14) . . . no C12 C13 H131 118.6(15) . . . no C14 C13 H131 121.2(15) . . . no C13 C14 H141 119.5(15) . . . no C15 C14 H141 120.1(15) . . . no C14 C15 H151 120.3(16) . . . no C16 C15 H151 119.5(16) . . . no C11 C16 H161 120.1(13) . . . no C15 C16 H161 120.0(13) . . . no C21 C22 H221 120.0(16) . . . no C23 C22 H221 119.9(16) . . . no C22 C23 H231 115.7(18) . . . no C24 C23 H231 124.2(18) . . . no C23 C24 H241 120.3(18) . . . no C25 C24 H241 119.2(18) . . . no C24 C25 H251 120.5(19) . . . no C26 C25 H251 119.7(19) . . . no C21 C26 H261 119.3(16) . . . no C25 C26 H261 119.6(16) . . . no C31 C32 H321 121.0(19) . . . no C33 C32 H321 119.0(19) . . . no C32 C33 H331 119(2) . . . no C34 C33 H331 120(2) . . . no C33 C34 H341 119.6(17) . . . no C35 C34 H341 120.5(17) . . . no C34 C35 H351 117.2(18) . . . no C36 C35 H351 122.8(18) . . . no C31 C36 H361 117.5(17) . . . no C35 C36 H361 121.9(17) . . . no C41 C42 H421 119.9(15) . . . no C43 C42 H421 119.5(15) . . . no C42 C43 H431 120.5(16) . . . no C44 C43 H431 119.3(16) . . . no C43 C44 H441 121.5(16) . . . no C45 C44 H441 118.2(16) . . . no C44 C45 H451 120.8(17) . . . no C46 C45 H451 119.1(17) . . . no C41 C46 H461 120.5(15) . . . no C45 C46 H461 119.2(15) . . . no C51 C52 H521 120.1(16) . . . no C53 C52 H521 120.1(16) . . . no C52 C53 H531 120.0(17) . . . no C54 C53 H531 119.8(17) . . . no C54 C55 H551 119.0(17) . . . no C56 C55 H551 120.4(17) . . . no C51 C56 H561 122.4(18) . . . no C55 C56 H561 118.1(18) . . . no C57 C58 H581 180(2) . . . no F1 B F2 109.3(2) . . . yes F1 B F3 108.3(2) . . . yes F1 B F4 109.0(2) . . . yes F2 B F3 111.0(2) . . . yes F2 B F4 112.0(2) . . . yes F3 B F4 107.0(2) . . . yes data_1 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' 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 12.570(5) _cell_length_b 24.135(5) _cell_length_c 22.969(9) _cell_angle_alpha 90 _cell_angle_beta 93.75(2) _cell_angle_gamma 90 _cell_volume 6953(4) _cell_formula_units_Z 4 _cell_measurement_temperature 163(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.1 _cell_measurement_theta_max 46.8 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.48 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 4.451 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1330 _exptl_absorpt_correction_T_max 0.2239 _exptl_absorpt_process_details ; none ; _exptl_special_details ; Diffractometer operator Herdtweck, E. ; _publ_section_exptl_prep ; the crystals were handled in air, fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 163(1) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 (Nonius)' _diffrn_measurement_method 'theta/2theta' _diffrn_standards_interval_time 1 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 12.5 _diffrn_reflns_number 13023 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 68.46 _reflns_number_total 12451 _reflns_number_gt 11390 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; MoleN-Software. ; _computing_data_collection 'CAD4 (Nonius)' _computing_cell_refinement 'CAD4 (Nonius) SET4 / CELLDIM' _computing_data_reduction 'MoleN (Nonius)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON PLUTON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=================================================================== # 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+26.2688P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_number_reflns 12451 _refine_ls_number_parameters 847 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 68.46 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.068 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.100 #=================================================================== # 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 Mo11 Mo Uani 0.47599(2) -0.04101(1) 0.50850(1) 1.000 0.0108(1) P11 P Uani 0.27841(7) -0.03098(4) 0.47574(4) 1.000 0.0136(2) P12 P Uani 0.35030(7) 0.07651(4) 0.44013(4) 1.000 0.0126(2) O11 O Uani 0.43304(19) -0.02003(10) 0.59237(10) 1.000 0.0156(7) O12 O Uani 0.48250(19) 0.06570(10) 0.57445(10) 1.000 0.0160(7) N11 N Uani 0.2494(2) 0.03157(13) 0.44591(14) 1.000 0.0173(9) N12 N Uani 0.4142(3) -0.14498(16) 0.52094(18) 1.000 0.0336(12) C11 C Uani 0.4189(3) 0.04741(18) 0.66806(17) 1.000 0.0265(11) C12 C Uani 0.4462(3) 0.02963(16) 0.60848(15) 1.000 0.0166(10) C13 C Uani 0.1394(3) 0.04455(17) 0.42419(19) 1.000 0.0246(11) C14 C Uani 0.3894(3) -0.18418(18) 0.49684(19) 1.000 0.0266(12) C15 C Uani 0.3578(5) -0.2340(2) 0.4647(2) 1.000 0.0421(17) C111 C Uani 0.2167(3) -0.08151(15) 0.42592(17) 1.000 0.0204(11) C112 C Uani 0.1082(3) -0.09347(18) 0.4255(2) 1.000 0.0291(12) C113 C Uani 0.0638(4) -0.13164(19) 0.3864(2) 1.000 0.0383(17) C114 C Uani 0.1260(4) -0.1584(2) 0.3484(2) 1.000 0.0423(16) C115 C Uani 0.2326(4) -0.14708(19) 0.34818(18) 1.000 0.0341(14) C116 C Uani 0.2785(4) -0.10853(17) 0.38678(17) 1.000 0.0257(11) C121 C Uani 0.2018(3) -0.03443(17) 0.53979(16) 1.000 0.0205(11) C122 C Uani 0.1799(3) 0.0136(2) 0.56987(18) 1.000 0.0285(14) C123 C Uani 0.1331(4) 0.0100(3) 0.6229(2) 1.000 0.0418(16) C124 C Uani 0.1107(4) -0.0402(3) 0.6463(2) 1.000 0.0466(19) C125 C Uani 0.1320(4) -0.0876(3) 0.6173(2) 1.000 0.0453(18) C126 C Uani 0.1776(3) -0.0856(2) 0.5634(2) 1.000 0.0312(14) C131 C Uani 0.3635(3) 0.08514(16) 0.36223(15) 1.000 0.0173(10) C132 C Uani 0.3296(3) 0.04474(18) 0.32297(17) 1.000 0.0233(11) C133 C Uani 0.3478(4) 0.0508(2) 0.26395(19) 1.000 0.0362(16) C134 C Uani 0.4003(4) 0.0964(2) 0.24526(19) 1.000 0.0406(18) C135 C Uani 0.4342(4) 0.1372(2) 0.28409(19) 1.000 0.0367(16) C136 C Uani 0.4168(3) 0.13174(18) 0.34261(18) 1.000 0.0270(12) C141 C Uani 0.3011(3) 0.14273(15) 0.46291(16) 1.000 0.0163(10) C142 C Uani 0.2289(3) 0.17330(16) 0.42673(17) 1.000 0.0221(12) C143 C Uani 0.1895(4) 0.22269(18) 0.4461(2) 1.000 0.0309(12) C144 C Uani 0.2229(4) 0.24264(18) 0.5008(2) 1.000 0.0321(14) C145 C Uani 0.2952(4) 0.21358(19) 0.53615(19) 1.000 0.0328(14) C146 C Uani 0.3330(3) 0.16306(17) 0.51776(17) 1.000 0.0236(11) Mo21 Mo Uani 0.02460(2) 0.48071(1) 0.54035(1) 1.000 0.0091(1) P21 P Uani 0.22144(7) 0.51051(4) 0.54433(4) 1.000 0.0123(3) P22 P Uani 0.14360(7) 0.57709(4) 0.44562(4) 1.000 0.0125(2) O21 O Uani 0.07829(18) 0.41111(10) 0.49772(10) 1.000 0.0131(7) O22 O Uani 0.02802(18) 0.45076(10) 0.41338(10) 1.000 0.0130(7) N21 N Uani 0.2458(2) 0.55707(13) 0.49183(13) 1.000 0.0174(9) N22 N Uani 0.0853(3) 0.43621(18) 0.64211(16) 1.000 0.0360(12) C21 C Uani 0.1076(3) 0.36127(17) 0.41097(18) 1.000 0.0257(12) C22 C Uani 0.0696(3) 0.41021(14) 0.44250(15) 1.000 0.0134(10) C23 C Uani 0.3518(3) 0.58253(19) 0.48982(18) 1.000 0.0256(11) C24 C Uani 0.0844(4) 0.41457(19) 0.68541(19) 1.000 0.0321(12) C25 C Uani 0.0848(7) 0.3868(3) 0.7414(3) 1.000 0.070(3) C211 C Uani 0.2833(3) 0.54021(16) 0.61099(15) 1.000 0.0171(10) C212 C Uani 0.3916(3) 0.53474(18) 0.62628(17) 1.000 0.0236(11) C213 C Uani 0.4378(3) 0.56377(19) 0.67337(18) 1.000 0.0291(14) C214 C Uani 0.3774(4) 0.59789(19) 0.70542(18) 1.000 0.0314(12) C215 C Uani 0.2688(4) 0.60284(19) 0.69139(18) 1.000 0.0304(12) C216 C Uani 0.2222(3) 0.57375(17) 0.64488(17) 1.000 0.0234(11) C221 C Uani 0.3033(3) 0.45143(16) 0.52939(16) 1.000 0.0180(11) C222 C Uani 0.3364(3) 0.44216(18) 0.47320(17) 1.000 0.0231(11) C223 C Uani 0.3908(3) 0.39393(19) 0.4614(2) 1.000 0.0315(15) C224 C Uani 0.4113(3) 0.3553(2) 0.5044(2) 1.000 0.0352(14) C225 C Uani 0.3788(4) 0.36411(19) 0.5599(2) 1.000 0.0359(14) C226 C Uani 0.3249(3) 0.41203(17) 0.57239(18) 1.000 0.0250(12) C231 C Uani 0.1189(3) 0.64877(15) 0.46330(17) 1.000 0.0184(11) C232 C Uani 0.1452(4) 0.66811(18) 0.51942(19) 1.000 0.0285(12) C233 C Uani 0.1148(4) 0.7211(2) 0.5351(2) 1.000 0.0404(17) C234 C Uani 0.0595(4) 0.7545(2) 0.4954(3) 1.000 0.0458(18) C235 C Uani 0.0330(4) 0.7353(2) 0.4400(3) 1.000 0.0452(19) C236 C Uani 0.0620(3) 0.68260(18) 0.4236(2) 1.000 0.0305(14) C241 C Uani 0.1992(3) 0.57834(16) 0.37466(16) 1.000 0.0179(11) C242 C Uani 0.2469(4) 0.62514(18) 0.35250(19) 1.000 0.0302(14) C243 C Uani 0.2955(4) 0.6222(2) 0.3001(2) 1.000 0.0431(16) C244 C Uani 0.2965(4) 0.5736(2) 0.2695(2) 1.000 0.0406(16) C245 C Uani 0.2497(4) 0.5270(2) 0.29095(19) 1.000 0.0329(16) C246 C Uani 0.2007(3) 0.52942(17) 0.34326(17) 1.000 0.0236(11) N1 N Uani -0.0981(4) 0.4833(2) 0.2177(2) 1.000 0.0512(17) C1 C Uani -0.0429(4) 0.4507(2) 0.23784(18) 1.000 0.0314(14) C2 C Uani 0.0285(4) 0.4099(2) 0.2644(2) 1.000 0.0417(16) N2 N Uani 0.5842(5) 0.2921(3) 0.4046(2) 1.000 0.073(2) C3 C Uani 0.6267(5) 0.2667(3) 0.3728(3) 1.000 0.0511(19) C4 C Uani 0.6812(5) 0.2335(4) 0.3321(3) 1.000 0.072(3) N3 N Uani 0.2998(4) 0.3885(3) 0.2989(3) 1.000 0.073(2) C5 C Uani 0.3144(4) 0.3441(3) 0.3097(3) 1.000 0.054(2) C6 C Uani 0.3318(6) 0.2867(3) 0.3254(4) 1.000 0.081(3) N4 N Uani 0.1941(7) 0.3462(5) 0.1595(5) 1.000 0.137(5) C7 C Uani 0.1979(9) 0.2981(7) 0.1698(4) 1.000 0.110(5) C8 C Uani 0.2032(11) 0.2401(6) 0.1798(6) 1.000 0.164(8) F11 F Uani 0.9237(3) 0.29185(14) 0.31082(19) 1.000 0.0698(14) F12 F Uani 1.0852(3) 0.2566(3) 0.3067(2) 1.000 0.126(3) F13 F Uani 0.9611(4) 0.23213(19) 0.24002(19) 1.000 0.1013(19) F14 F Uani 0.9564(5) 0.20465(19) 0.3311(3) 1.000 0.128(3) B11 B Uani 0.9798(4) 0.2457(2) 0.2960(2) 1.000 0.0350(17) F21 F Uani 0.4425(8) 0.2305(3) 0.1631(3) 1.000 0.202(4) F22 F Uani 0.5042(5) 0.2803(3) 0.2334(2) 1.000 0.131(3) F23 F Uani 0.5029(4) 0.31115(18) 0.1437(2) 1.000 0.1002(19) F24 F Uani 0.6132(5) 0.2443(2) 0.1772(3) 1.000 0.143(3) B21 B Uani 0.5119(6) 0.2667(3) 0.1784(3) 1.000 0.0465(19) H11A H Uiso 0.43400 0.08700 0.67310 1.000 0.0340 H11B H Uiso 0.46180 0.02630 0.69750 1.000 0.0340 H11C H Uiso 0.34310 0.04060 0.67270 1.000 0.0340 H13A H Uiso 0.09290 0.01310 0.43170 1.000 0.0320 H13B H Uiso 0.13760 0.05170 0.38210 1.000 0.0320 H13C H Uiso 0.11470 0.07750 0.44430 1.000 0.0320 H15A H Uiso 0.34670 -0.26420 0.49220 1.000 0.0550 H15B H Uiso 0.41400 -0.24450 0.43920 1.000 0.0550 H15C H Uiso 0.29140 -0.22700 0.44110 1.000 0.0550 H112 H Uiso 0.06500 -0.07540 0.45210 1.000 0.0380 H113 H Uiso -0.01040 -0.13940 0.38570 1.000 0.0500 H114 H Uiso 0.09480 -0.18510 0.32210 1.000 0.0550 H115 H Uiso 0.27510 -0.16560 0.32160 1.000 0.0440 H116 H Uiso 0.35240 -0.10050 0.38650 1.000 0.0330 H122 H Uiso 0.19680 0.04880 0.55430 1.000 0.0370 H123 H Uiso 0.11650 0.04300 0.64310 1.000 0.0540 H124 H Uiso 0.08000 -0.04210 0.68300 1.000 0.0610 H125 H Uiso 0.11580 -0.12240 0.63380 1.000 0.0590 H126 H Uiso 0.19180 -0.11890 0.54320 1.000 0.0400 H132 H Uiso 0.29400 0.01280 0.33600 1.000 0.0300 H133 H Uiso 0.32360 0.02320 0.23680 1.000 0.0470 H134 H Uiso 0.41340 0.10000 0.20520 1.000 0.0530 H135 H Uiso 0.46970 0.16900 0.27070 1.000 0.0480 H136 H Uiso 0.44110 0.15960 0.36950 1.000 0.0350 H142 H Uiso 0.20730 0.16000 0.38890 1.000 0.0290 H143 H Uiso 0.13930 0.24310 0.42200 1.000 0.0400 H144 H Uiso 0.19560 0.27680 0.51390 1.000 0.0420 H145 H Uiso 0.31920 0.22810 0.57320 1.000 0.0420 H146 H Uiso 0.38110 0.14230 0.54280 1.000 0.0300 H21A H Uiso 0.09530 0.36710 0.36880 1.000 0.0330 H21B H Uiso 0.06880 0.32830 0.42250 1.000 0.0330 H21C H Uiso 0.18410 0.35610 0.42070 1.000 0.0330 H23A H Uiso 0.40080 0.56570 0.51980 1.000 0.0330 H23B H Uiso 0.34660 0.62240 0.49710 1.000 0.0330 H23C H Uiso 0.37890 0.57640 0.45130 1.000 0.0330 H25A H Uiso 0.01380 0.37160 0.74670 1.000 0.0900 H25B H Uiso 0.10350 0.41350 0.77260 1.000 0.0900 H25C H Uiso 0.13730 0.35680 0.74280 1.000 0.0900 H212 H Uiso 0.43400 0.51100 0.60430 1.000 0.0310 H213 H Uiso 0.51200 0.56000 0.68350 1.000 0.0380 H214 H Uiso 0.40980 0.61820 0.73730 1.000 0.0410 H215 H Uiso 0.22660 0.62630 0.71380 1.000 0.0400 H216 H Uiso 0.14750 0.57660 0.63590 1.000 0.0310 H222 H Uiso 0.32170 0.46880 0.44330 1.000 0.0300 H223 H Uiso 0.41380 0.38760 0.42340 1.000 0.0410 H224 H Uiso 0.44820 0.32220 0.49590 1.000 0.0460 H225 H Uiso 0.39350 0.33720 0.58960 1.000 0.0470 H226 H Uiso 0.30240 0.41800 0.61060 1.000 0.0330 H232 H Uiso 0.18370 0.64510 0.54700 1.000 0.0370 H233 H Uiso 0.13250 0.73430 0.57350 1.000 0.0530 H234 H Uiso 0.03960 0.79090 0.50620 1.000 0.0590 H235 H Uiso -0.00570 0.75840 0.41270 1.000 0.0590 H236 H Uiso 0.04300 0.66960 0.38530 1.000 0.0400 H242 H Uiso 0.24610 0.65920 0.37330 1.000 0.0400 H243 H Uiso 0.32840 0.65430 0.28540 1.000 0.0560 H244 H Uiso 0.32950 0.57210 0.23350 1.000 0.0530 H245 H Uiso 0.25090 0.49310 0.26990 1.000 0.0430 H246 H Uiso 0.16790 0.49720 0.35770 1.000 0.0310 H2A H Uiso 0.07970 0.39840 0.23630 1.000 0.0540 H2B H Uiso -0.01250 0.37770 0.27600 1.000 0.0540 H2C H Uiso 0.06700 0.42590 0.29880 1.000 0.0540 H4A H Uiso 0.75840 0.23680 0.34050 1.000 0.0940 H4B H Uiso 0.66250 0.24640 0.29230 1.000 0.0940 H4C H Uiso 0.66000 0.19460 0.33570 1.000 0.0940 H6A H Uiso 0.37760 0.26940 0.29760 1.000 0.1050 H6B H Uiso 0.26330 0.26730 0.32440 1.000 0.1050 H6C H Uiso 0.36650 0.28460 0.36480 1.000 0.1050 H8A H Uiso 0.14340 0.22870 0.20240 1.000 0.2130 H8B H Uiso 0.27050 0.23100 0.20170 1.000 0.2130 H8C H Uiso 0.19950 0.22050 0.14240 1.000 0.2130 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 Mo11 0.0113(1) 0.0101(1) 0.0109(1) 0.0004(1) 0.0007(1) 0.0010(1) P11 0.0121(4) 0.0132(4) 0.0154(4) 0.0009(3) 0.0000(3) 0.0000(3) P12 0.0134(4) 0.0110(4) 0.0134(4) 0.0002(3) 0.0000(3) 0.0022(3) O11 0.0144(12) 0.0182(14) 0.0145(12) 0.0022(10) 0.0025(9) 0.0024(10) O12 0.0176(12) 0.0156(13) 0.0150(12) -0.0017(10) 0.0018(10) 0.0029(10) N11 0.0132(15) 0.0143(16) 0.0240(16) 0.0033(12) -0.0011(12) 0.0033(12) N12 0.036(2) 0.022(2) 0.042(2) 0.0042(17) -0.0032(17) -0.0007(16) C11 0.030(2) 0.033(2) 0.0169(19) -0.0050(16) 0.0050(16) 0.0018(18) C12 0.0130(17) 0.022(2) 0.0145(17) -0.0016(15) -0.0004(13) 0.0055(14) C13 0.0158(19) 0.021(2) 0.036(2) 0.0059(17) -0.0054(16) 0.0033(15) C14 0.023(2) 0.027(2) 0.030(2) 0.0112(19) 0.0025(17) -0.0002(17) C15 0.059(3) 0.032(3) 0.035(3) 0.004(2) 0.001(2) -0.009(2) C111 0.024(2) 0.0137(19) 0.0226(19) 0.0045(15) -0.0064(15) -0.0018(15) C112 0.027(2) 0.024(2) 0.035(2) 0.0034(18) -0.0069(18) -0.0044(17) C113 0.036(3) 0.028(3) 0.048(3) 0.007(2) -0.020(2) -0.012(2) C114 0.063(3) 0.023(2) 0.037(3) 0.000(2) -0.026(2) -0.013(2) C115 0.056(3) 0.025(2) 0.020(2) -0.0033(17) -0.0085(19) 0.001(2) C116 0.035(2) 0.021(2) 0.0201(19) 0.0014(16) -0.0048(16) 0.0004(17) C121 0.0124(17) 0.030(2) 0.0190(18) 0.0034(16) -0.0002(14) 0.0007(15) C122 0.0187(19) 0.042(3) 0.025(2) -0.0040(18) 0.0040(16) 0.0046(18) C123 0.029(2) 0.070(4) 0.027(2) -0.006(2) 0.0064(19) 0.015(2) C124 0.021(2) 0.093(5) 0.027(2) 0.011(3) 0.0114(19) 0.014(3) C125 0.027(2) 0.070(4) 0.040(3) 0.030(3) 0.010(2) 0.002(2) C126 0.020(2) 0.041(3) 0.033(2) 0.014(2) 0.0052(17) 0.0019(18) C131 0.0135(17) 0.023(2) 0.0151(17) -0.0005(14) -0.0003(13) 0.0042(14) C132 0.023(2) 0.026(2) 0.0207(19) -0.0035(16) -0.0006(15) 0.0035(16) C133 0.040(3) 0.049(3) 0.019(2) -0.011(2) -0.0024(18) 0.008(2) C134 0.039(3) 0.067(4) 0.016(2) 0.003(2) 0.0039(18) 0.004(2) C135 0.038(3) 0.048(3) 0.025(2) 0.011(2) 0.0087(19) -0.006(2) C136 0.031(2) 0.029(2) 0.021(2) 0.0019(17) 0.0013(16) -0.0054(17) C141 0.0172(18) 0.0116(18) 0.0205(18) 0.0004(14) 0.0042(14) 0.0029(14) C142 0.025(2) 0.018(2) 0.023(2) -0.0018(15) -0.0012(16) 0.0053(16) C143 0.035(2) 0.020(2) 0.037(2) -0.0008(18) -0.0030(19) 0.0137(18) C144 0.040(3) 0.020(2) 0.036(2) -0.0069(18) 0.000(2) 0.0138(18) C145 0.045(3) 0.026(2) 0.027(2) -0.0081(18) -0.0007(19) 0.0098(19) C146 0.029(2) 0.022(2) 0.0197(19) -0.0027(16) 0.0013(16) 0.0074(16) Mo21 0.0088(1) 0.0089(1) 0.0095(1) 0.0014(1) 0.0009(1) -0.0004(1) P21 0.0094(4) 0.0155(5) 0.0121(4) 0.0011(3) 0.0010(3) -0.0016(3) P22 0.0125(4) 0.0126(4) 0.0124(4) 0.0015(3) 0.0017(3) -0.0030(3) O21 0.0117(11) 0.0113(12) 0.0164(12) 0.0020(9) 0.0009(9) 0.0007(9) O22 0.0134(12) 0.0120(12) 0.0135(11) -0.0007(9) 0.0011(9) -0.0008(9) N21 0.0109(14) 0.0233(17) 0.0181(15) 0.0046(13) 0.0022(12) -0.0049(12) N22 0.035(2) 0.047(2) 0.025(2) 0.0099(18) -0.0055(16) -0.0041(18) C21 0.032(2) 0.019(2) 0.026(2) -0.0022(16) 0.0013(17) 0.0088(17) C22 0.0152(17) 0.0101(18) 0.0150(17) -0.0013(13) 0.0011(13) -0.0020(13) C23 0.0128(18) 0.036(2) 0.028(2) 0.0107(18) 0.0007(15) -0.0112(16) C24 0.037(2) 0.031(2) 0.028(2) 0.0031(19) -0.0009(18) -0.0099(19) C25 0.121(6) 0.052(4) 0.036(3) 0.018(3) 0.007(3) -0.027(4) C211 0.0168(18) 0.022(2) 0.0125(16) 0.0007(14) 0.0017(13) -0.0065(14) C212 0.0191(19) 0.031(2) 0.0204(19) 0.0032(16) -0.0018(15) -0.0052(16) C213 0.022(2) 0.038(3) 0.026(2) 0.0056(18) -0.0090(16) -0.0083(18) C214 0.039(2) 0.033(2) 0.021(2) -0.0016(18) -0.0081(18) -0.013(2) C215 0.037(2) 0.032(2) 0.022(2) -0.0052(18) 0.0009(18) -0.0024(19) C216 0.022(2) 0.028(2) 0.0199(19) -0.0008(16) -0.0001(15) -0.0035(16) C221 0.0099(16) 0.022(2) 0.0218(19) -0.0017(15) -0.0014(14) -0.0006(14) C222 0.0134(18) 0.032(2) 0.024(2) -0.0041(17) 0.0019(15) -0.0025(16) C223 0.0153(19) 0.038(3) 0.042(3) -0.013(2) 0.0079(17) -0.0016(17) C224 0.016(2) 0.029(2) 0.061(3) -0.015(2) 0.006(2) 0.0031(17) C225 0.026(2) 0.026(2) 0.055(3) 0.006(2) -0.003(2) 0.0060(18) C226 0.021(2) 0.026(2) 0.028(2) 0.0041(17) 0.0026(16) 0.0027(16) C231 0.0158(18) 0.0141(19) 0.026(2) -0.0003(15) 0.0070(15) -0.0059(14) C232 0.035(2) 0.022(2) 0.029(2) -0.0031(17) 0.0062(18) -0.0091(17) C233 0.048(3) 0.030(3) 0.045(3) -0.019(2) 0.017(2) -0.012(2) C234 0.043(3) 0.016(2) 0.080(4) -0.012(2) 0.017(3) -0.002(2) C235 0.035(3) 0.020(3) 0.080(4) 0.006(2) 0.000(3) 0.004(2) C236 0.030(2) 0.019(2) 0.042(3) 0.0031(18) -0.0012(19) -0.0004(17) C241 0.0188(18) 0.019(2) 0.0161(17) 0.0017(14) 0.0036(14) -0.0044(15) C242 0.043(3) 0.024(2) 0.025(2) -0.0009(17) 0.0120(19) -0.0134(19) C243 0.062(3) 0.040(3) 0.030(2) 0.006(2) 0.024(2) -0.026(2) C244 0.056(3) 0.047(3) 0.021(2) -0.002(2) 0.020(2) -0.014(2) C245 0.042(3) 0.034(3) 0.024(2) -0.0078(18) 0.0119(19) -0.007(2) C246 0.029(2) 0.022(2) 0.0206(19) 0.0013(16) 0.0087(16) -0.0075(16) N1 0.053(3) 0.048(3) 0.053(3) 0.004(2) 0.007(2) 0.008(2) C1 0.035(2) 0.039(3) 0.021(2) -0.0009(19) 0.0071(18) -0.004(2) C2 0.047(3) 0.048(3) 0.029(2) 0.005(2) -0.007(2) -0.001(2) N2 0.083(4) 0.090(4) 0.046(3) 0.010(3) 0.013(3) 0.028(3) C3 0.042(3) 0.068(4) 0.043(3) 0.012(3) 0.000(2) -0.003(3) C4 0.045(3) 0.110(6) 0.061(4) -0.025(4) -0.002(3) -0.001(4) N3 0.044(3) 0.054(4) 0.120(5) 0.016(3) 0.004(3) 0.001(2) C5 0.032(3) 0.062(4) 0.070(4) 0.001(3) 0.014(3) -0.004(3) C6 0.063(4) 0.053(4) 0.129(7) 0.010(4) 0.018(4) 0.005(3) N4 0.085(6) 0.183(11) 0.140(9) -0.064(8) -0.015(5) 0.050(7) C7 0.089(7) 0.176(12) 0.066(6) -0.034(7) 0.009(5) 0.042(8) C8 0.169(13) 0.198(15) 0.133(11) 0.064(10) 0.071(9) 0.077(12) F11 0.072(2) 0.042(2) 0.098(3) -0.0085(19) 0.025(2) 0.0060(17) F12 0.047(2) 0.219(7) 0.112(4) -0.053(4) 0.008(2) -0.006(3) F13 0.141(4) 0.089(3) 0.067(3) -0.025(2) -0.046(3) 0.057(3) F14 0.197(6) 0.056(3) 0.139(5) 0.048(3) 0.077(4) 0.024(3) B11 0.036(3) 0.034(3) 0.035(3) 0.003(2) 0.003(2) 0.004(2) F21 0.327(11) 0.101(4) 0.157(6) 0.033(4) -0.150(7) -0.120(6) F22 0.154(5) 0.180(6) 0.055(3) -0.044(3) -0.013(3) 0.016(4) F23 0.090(3) 0.075(3) 0.141(4) 0.064(3) 0.048(3) 0.034(2) F24 0.138(5) 0.115(4) 0.186(6) 0.094(4) 0.083(5) 0.077(4) B21 0.069(4) 0.036(3) 0.036(3) 0.004(2) 0.014(3) -0.007(3) #=================================================================== # 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 Mo11 P11 2.5590(14) . . yes Mo11 O11 2.097(2) . . yes Mo11 N12 2.648(4) . . yes Mo11 Mo11 2.1133(9) . 3_656 yes Mo11 P12 2.5607(14) . 3_656 yes Mo11 O12 2.095(2) . 3_656 yes Mo21 O22 2.096(3) . 3_566 yes Mo21 N22 2.639(4) . . yes Mo21 P21 2.5725(14) . . yes Mo21 O21 2.079(3) . . yes Mo21 Mo21 2.1295(9) . 3_566 yes Mo21 P22 2.5709(14) . 3_566 yes P11 C111 1.812(4) . . yes P11 N11 1.688(3) . . yes P11 C121 1.812(4) . . yes P12 C141 1.804(4) . . yes P12 N11 1.681(3) . . yes P12 C131 1.820(4) . . yes P21 C211 1.819(4) . . yes P21 C221 1.804(4) . . yes P21 N21 1.691(3) . . yes P22 N21 1.683(3) . . yes P22 C231 1.809(4) . . yes P22 C241 1.815(4) . . yes O11 C12 1.262(5) . . yes O12 C12 1.274(4) . . yes F11 B11 1.373(6) . . yes F12 B11 1.357(6) . . yes F13 B11 1.333(6) . . yes F14 B11 1.323(7) . . yes O21 C22 1.266(4) . . yes O22 C22 1.278(4) . . yes F21 B21 1.268(11) . . yes F22 B21 1.315(8) . . yes F23 B21 1.337(8) . . yes F24 B21 1.385(10) . . yes N11 C13 1.473(5) . . yes N12 C14 1.130(6) . . yes N21 C23 1.471(5) . . yes N22 C24 1.124(6) . . yes N1 C1 1.128(7) . . yes N2 C3 1.116(9) . . yes N3 C5 1.112(10) . . yes N4 C7 1.19(2) . . yes C11 C12 1.495(5) . . no C14 C15 1.453(7) . . no C11 H11A 0.9796 . . no C11 H11B 0.9798 . . no C111 C116 1.389(6) . . no C11 H11C 0.9795 . . no C111 C112 1.393(5) . . no C112 C113 1.379(6) . . no C13 H13C 0.9803 . . no C13 H13B 0.9808 . . no C13 H13A 0.9802 . . no C113 C114 1.371(7) . . no C114 C115 1.368(7) . . no C15 H15C 0.9797 . . no C15 H15A 0.9804 . . no C115 C116 1.385(6) . . no C15 H15B 0.9800 . . no C121 C126 1.390(6) . . no C121 C122 1.386(6) . . no C122 C123 1.390(6) . . no C123 C124 1.362(10) . . no C124 C125 1.359(9) . . no C125 C126 1.399(6) . . no C131 C132 1.377(6) . . no C131 C136 1.399(6) . . no C132 C133 1.397(6) . . no C133 C134 1.367(7) . . no C134 C135 1.377(7) . . no C135 C136 1.382(6) . . no C141 C146 1.387(5) . . no C141 C142 1.400(5) . . no C142 C143 1.376(6) . . no C143 C144 1.385(7) . . no C144 C145 1.371(7) . . no C145 C146 1.385(6) . . no C112 H112 0.9496 . . no C113 H113 0.9504 . . no C114 H114 0.9503 . . no C115 H115 0.9490 . . no C116 H116 0.9494 . . no C21 C22 1.481(5) . . no C122 H122 0.9512 . . no C123 H123 0.9517 . . no C124 H124 0.9509 . . no C24 C25 1.450(8) . . no C125 H125 0.9490 . . no C126 H126 0.9507 . . no C132 H132 0.9495 . . no C133 H133 0.9489 . . no C134 H134 0.9493 . . no C135 H135 0.9491 . . no C136 H136 0.9499 . . no C142 H142 0.9492 . . no C143 H143 0.9495 . . no C144 H144 0.9495 . . no C145 H145 0.9510 . . no C146 H146 0.9497 . . no C21 H21A 0.9810 . . no C21 H21C 0.9809 . . no C21 H21B 0.9788 . . no C23 H23C 0.9799 . . no C23 H23A 0.9814 . . no C23 H23B 0.9796 . . no C25 H25A 0.9799 . . no C25 H25B 0.9808 . . no C25 H25C 0.9788 . . no C1 C2 1.441(7) . . no C211 C216 1.389(5) . . no C211 C212 1.390(5) . . no C212 C213 1.384(6) . . no C213 C214 1.367(6) . . no C214 C215 1.387(7) . . no C215 C216 1.377(6) . . no C221 C222 1.400(5) . . no C221 C226 1.385(6) . . no C222 C223 1.386(6) . . no C223 C224 1.370(7) . . no C224 C225 1.380(6) . . no C225 C226 1.380(6) . . no C231 C232 1.390(6) . . no C231 C236 1.387(6) . . no C232 C233 1.389(7) . . no C233 C234 1.372(8) . . no C234 C235 1.375(9) . . no C235 C236 1.382(7) . . no C241 C242 1.391(6) . . no C241 C246 1.384(6) . . no C242 C243 1.387(7) . . no C243 C244 1.368(7) . . no C244 C245 1.375(7) . . no C245 C246 1.387(6) . . no C2 H2C 0.9786 . . no C2 H2A 0.9809 . . no C2 H2B 0.9790 . . no C212 H212 0.9500 . . no C213 H213 0.9508 . . no C214 H214 0.9504 . . no C215 H215 0.9501 . . no C216 H216 0.9506 . . no C222 H222 0.9500 . . no C223 H223 0.9496 . . no C224 H224 0.9504 . . no C225 H225 0.9512 . . no C226 H226 0.9505 . . no C232 H232 0.9507 . . no C233 H233 0.9504 . . no C234 H234 0.9508 . . no C235 H235 0.9491 . . no C236 H236 0.9497 . . no C242 H242 0.9512 . . no C243 H243 0.9505 . . no C244 H244 0.9497 . . no C245 H245 0.9510 . . no C246 H246 0.9500 . . no C3 C4 1.438(10) . . no C4 H4B 0.9797 . . no C4 H4C 0.9809 . . no C4 H4A 0.9802 . . no C5 C6 1.445(10) . . no C6 H6B 0.9791 . . no C6 H6C 0.9799 . . no C6 H6A 0.9806 . . no C7 C8 1.42(2) . . no C8 H8B 0.9804 . . no C8 H8C 0.9791 . . no C8 H8A 0.9804 . . 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 P11 Mo11 O11 86.79(7) . . . yes P11 Mo11 N12 80.53(9) . . . yes Mo11 Mo11 P11 98.08(3) 3_656 . . yes P11 Mo11 P12 161.63(4) . . 3_656 yes P11 Mo11 O12 93.11(7) . . 3_656 yes O11 Mo11 N12 91.99(11) . . . yes Mo11 Mo11 O11 92.14(7) 3_656 . . yes P12 Mo11 O11 85.44(7) 3_656 . . yes O11 Mo11 O12 177.43(10) . . 3_656 yes Mo11 Mo11 N12 175.56(9) 3_656 . . yes P12 Mo11 N12 83.14(9) 3_656 . . yes O12 Mo11 N12 85.46(11) 3_656 . . yes Mo11 Mo11 P12 98.82(3) 3_656 . 3_656 yes Mo11 Mo11 O12 90.42(7) 3_656 . 3_656 yes P12 Mo11 O12 93.92(7) 3_656 . 3_656 yes P22 Mo21 O22 94.31(7) 3_566 . 3_566 yes Mo21 Mo21 O22 90.75(7) 3_566 . 3_566 yes Mo21 Mo21 O21 91.61(7) 3_566 . . yes P21 Mo21 O21 84.35(7) . . . yes P21 Mo21 N22 81.99(9) . . . yes Mo21 Mo21 P21 97.62(3) 3_566 . . yes P21 Mo21 P22 160.77(4) . . 3_566 yes P21 Mo21 O22 95.51(7) . . 3_566 yes O21 Mo21 N22 90.25(11) . . . yes Mo21 Mo21 N22 178.06(10) 3_566 . . yes P22 Mo21 O21 85.15(7) 3_566 . . yes O21 Mo21 O22 177.64(9) . . 3_566 yes Mo21 Mo21 P22 98.74(3) 3_566 . 3_566 yes P22 Mo21 N22 81.99(9) 3_566 . . yes O22 Mo21 N22 87.40(11) 3_566 . . yes Mo11 P11 C121 108.30(13) . . . yes Mo11 P11 C111 119.29(13) . . . yes Mo11 P11 N11 112.56(10) . . . yes N11 P11 C111 105.87(17) . . . yes N11 P11 C121 104.98(17) . . . yes C111 P11 C121 104.69(18) . . . yes N11 P12 C131 105.63(17) . . . yes N11 P12 C141 105.91(16) . . . yes Mo11 P12 N11 111.89(11) 3_656 . . yes C131 P12 C141 103.82(18) . . . yes Mo11 P12 C131 111.20(13) 3_656 . . yes Mo11 P12 C141 117.45(13) 3_656 . . yes Mo21 P21 C211 119.83(13) . . . yes Mo21 P21 C221 109.36(13) . . . yes N21 P21 C211 104.54(16) . . . yes N21 P21 C221 104.92(16) . . . yes C211 P21 C221 104.71(18) . . . yes Mo21 P21 N21 112.27(10) . . . yes N21 P22 C231 105.56(17) . . . yes Mo21 P22 C241 119.32(13) 3_566 . . yes Mo21 P22 C231 109.65(13) 3_566 . . yes C231 P22 C241 105.52(18) . . . yes N21 P22 C241 104.37(16) . . . yes Mo21 P22 N21 111.42(11) 3_566 . . yes Mo11 O11 C12 117.5(2) . . . yes Mo11 O12 C12 119.0(2) 3_656 . . yes Mo21 O21 C22 118.4(2) . . . yes Mo21 O22 C22 118.1(2) 3_566 . . yes P11 N11 P12 117.72(16) . . . yes P12 N11 C13 122.2(3) . . . yes P11 N11 C13 120.1(2) . . . yes Mo11 N12 C14 144.5(4) . . . yes P21 N21 P22 118.31(16) . . . yes P21 N21 C23 120.4(2) . . . yes P22 N21 C23 121.1(3) . . . yes Mo21 N22 C24 162.5(4) . . . yes O12 C12 C11 118.6(3) . . . yes O11 C12 O12 121.0(3) . . . yes O11 C12 C11 120.5(3) . . . yes N12 C14 C15 178.8(5) . . . yes P11 C111 C116 119.4(3) . . . yes P11 C111 C112 121.5(3) . . . yes C12 C11 H11C 109.54 . . . no C112 C111 C116 119.1(4) . . . no C12 C11 H11B 109.48 . . . no H11B C11 H11C 109.45 . . . no C12 C11 H11A 109.50 . . . no H11A C11 H11B 109.39 . . . no H11A C11 H11C 109.46 . . . no C111 C112 C113 119.8(4) . . . no N11 C13 H13A 109.46 . . . no N11 C13 H13B 109.39 . . . no H13B C13 H13C 109.52 . . . no H13A C13 H13B 109.52 . . . no N11 C13 H13C 109.41 . . . no C112 C113 C114 120.4(4) . . . no H13A C13 H13C 109.54 . . . no C113 C114 C115 120.5(4) . . . no C14 C15 H15C 109.46 . . . no H15A C15 H15B 109.35 . . . no C114 C115 C116 119.9(4) . . . no H15A C15 H15C 109.43 . . . no C14 C15 H15B 109.51 . . . no C14 C15 H15A 109.49 . . . no H15B C15 H15C 109.59 . . . no C111 C116 C115 120.2(4) . . . no P11 C121 C122 120.0(3) . . . yes C122 C121 C126 119.5(4) . . . no P11 C121 C126 119.9(3) . . . yes C121 C122 C123 119.6(5) . . . no C122 C123 C124 120.8(6) . . . no C123 C124 C125 120.2(5) . . . no C124 C125 C126 120.7(6) . . . no C121 C126 C125 119.3(5) . . . no P12 C131 C132 121.3(3) . . . yes P12 C131 C136 119.0(3) . . . yes C132 C131 C136 119.5(3) . . . no C131 C132 C133 119.9(4) . . . no C132 C133 C134 120.1(4) . . . no C133 C134 C135 120.5(4) . . . no C134 C135 C136 120.0(4) . . . no C131 C136 C135 120.0(4) . . . no P12 C141 C142 121.1(3) . . . yes C142 C141 C146 119.4(3) . . . no P12 C141 C146 119.5(3) . . . yes C141 C142 C143 119.9(4) . . . no C142 C143 C144 120.0(4) . . . no C143 C144 C145 120.6(4) . . . no C144 C145 C146 119.8(4) . . . no C141 C146 C145 120.3(4) . . . no C111 C112 H112 120.07 . . . no C113 C112 H112 120.12 . . . no C114 C113 H113 119.76 . . . no C112 C113 H113 119.84 . . . no C113 C114 H114 119.69 . . . no C115 C114 H114 119.79 . . . no C114 C115 H115 120.07 . . . no C116 C115 H115 119.99 . . . no C115 C116 H116 119.98 . . . no C111 C116 H116 119.84 . . . no O22 C22 C21 119.3(3) . . . yes O21 C22 C21 119.6(3) . . . yes O21 C22 O22 121.1(3) . . . yes C123 C122 H122 120.21 . . . no C121 C122 H122 120.20 . . . no C122 C123 H123 119.60 . . . no C124 C123 H123 119.63 . . . no N22 C24 C25 179.2(6) . . . yes C125 C124 H124 119.88 . . . no C123 C124 H124 119.93 . . . no C126 C125 H125 119.67 . . . no C124 C125 H125 119.66 . . . no C121 C126 H126 120.51 . . . no C125 C126 H126 120.24 . . . no C131 C132 H132 120.04 . . . no C133 C132 H132 120.08 . . . no C134 C133 H133 119.97 . . . no C132 C133 H133 119.89 . . . no C133 C134 H134 119.74 . . . no C135 C134 H134 119.76 . . . no C134 C135 H135 120.03 . . . no C136 C135 H135 119.99 . . . no C135 C136 H136 120.02 . . . no C131 C136 H136 120.01 . . . no C141 C142 H142 120.05 . . . no C143 C142 H142 120.10 . . . no C142 C143 H143 120.03 . . . no C144 C143 H143 119.94 . . . no C145 C144 H144 119.72 . . . no C143 C144 H144 119.67 . . . no C144 C145 H145 120.03 . . . no C146 C145 H145 120.16 . . . no C145 C146 H146 119.83 . . . no C141 C146 H146 119.89 . . . no C22 C21 H21C 109.44 . . . no C22 C21 H21A 109.48 . . . no C22 C21 H21B 109.50 . . . no H21B C21 H21C 109.47 . . . no H21A C21 H21B 109.55 . . . no H21A C21 H21C 109.40 . . . no N21 C23 H23A 109.47 . . . no H23A C23 H23B 109.43 . . . no N21 C23 H23B 109.53 . . . no N21 C23 H23C 109.54 . . . no H23A C23 H23C 109.38 . . . no H23B C23 H23C 109.48 . . . no C24 C25 H25C 109.53 . . . no C24 C25 H25A 109.45 . . . no C24 C25 H25B 109.34 . . . no H25B C25 H25C 109.46 . . . no H25A C25 H25B 109.38 . . . no H25A C25 H25C 109.67 . . . no N1 C1 C2 178.8(5) . . . yes P21 C211 C212 122.2(3) . . . yes C212 C211 C216 118.8(3) . . . no P21 C211 C216 118.7(3) . . . yes C211 C212 C213 120.2(4) . . . no C212 C213 C214 120.4(4) . . . no C213 C214 C215 120.0(4) . . . no C214 C215 C216 119.9(4) . . . no C211 C216 C215 120.6(4) . . . no P21 C221 C222 120.6(3) . . . yes P21 C221 C226 119.6(3) . . . yes C222 C221 C226 119.4(4) . . . no C221 C222 C223 119.7(4) . . . no C222 C223 C224 120.2(4) . . . no C223 C224 C225 120.5(4) . . . no C224 C225 C226 120.0(4) . . . no C221 C226 C225 120.2(4) . . . no C232 C231 C236 119.5(4) . . . no P22 C231 C232 119.7(3) . . . yes P22 C231 C236 120.3(3) . . . yes C231 C232 C233 119.8(4) . . . no C232 C233 C234 120.3(5) . . . no C233 C234 C235 119.9(5) . . . no C234 C235 C236 120.7(5) . . . no C231 C236 C235 119.8(5) . . . no P22 C241 C242 122.9(3) . . . yes P22 C241 C246 118.2(3) . . . yes C242 C241 C246 118.8(4) . . . no C241 C242 C243 120.1(4) . . . no C242 C243 C244 120.6(4) . . . no C243 C244 C245 119.9(4) . . . no C244 C245 C246 120.0(4) . . . no C241 C246 C245 120.6(4) . . . no H2B C2 H2C 109.56 . . . no C1 C2 H2B 109.47 . . . no C1 C2 H2A 109.40 . . . no H2A C2 H2C 109.38 . . . no C1 C2 H2C 109.49 . . . no H2A C2 H2B 109.52 . . . no C213 C212 H212 119.95 . . . no C211 C212 H212 119.82 . . . no C212 C213 H213 119.84 . . . no C214 C213 H213 119.75 . . . no C213 C214 H214 120.02 . . . no C215 C214 H214 120.01 . . . no C214 C215 H215 120.09 . . . no C216 C215 H215 120.00 . . . no C211 C216 H216 119.68 . . . no C215 C216 H216 119.71 . . . no C221 C222 H222 120.19 . . . no C223 C222 H222 120.15 . . . no C224 C223 H223 119.92 . . . no C222 C223 H223 119.91 . . . no C223 C224 H224 119.68 . . . no C225 C224 H224 119.81 . . . no C226 C225 H225 119.88 . . . no C224 C225 H225 120.12 . . . no C221 C226 H226 119.87 . . . no C225 C226 H226 119.92 . . . no C231 C232 H232 120.10 . . . no C233 C232 H232 120.12 . . . no C232 C233 H233 119.84 . . . no C234 C233 H233 119.84 . . . no C233 C234 H234 120.01 . . . no C235 C234 H234 120.07 . . . no C236 C235 H235 119.57 . . . no C234 C235 H235 119.76 . . . no C231 C236 H236 120.14 . . . no C235 C236 H236 120.11 . . . no C243 C242 H242 119.99 . . . no C241 C242 H242 119.94 . . . no C242 C243 H243 119.55 . . . no C244 C243 H243 119.84 . . . no C243 C244 H244 119.95 . . . no C245 C244 H244 120.14 . . . no C244 C245 H245 120.00 . . . no C246 C245 H245 119.96 . . . no C241 C246 H246 119.68 . . . no C245 C246 H246 119.70 . . . no N2 C3 C4 179.5(8) . . . yes C3 C4 H4A 109.53 . . . no C3 C4 H4B 109.51 . . . no C3 C4 H4C 109.56 . . . no H4A C4 H4B 109.38 . . . no H4A C4 H4C 109.40 . . . no H4B C4 H4C 109.45 . . . no N3 C5 C6 178.2(8) . . . yes C5 C6 H6A 109.36 . . . no C5 C6 H6B 109.52 . . . no C5 C6 H6C 109.34 . . . no H6A C6 H6B 109.51 . . . no H6A C6 H6C 109.54 . . . no H6B C6 H6C 109.55 . . . no N4 C7 C8 177.7(12) . . . yes C7 C8 H8A 109.45 . . . no C7 C8 H8B 109.50 . . . no C7 C8 H8C 109.60 . . . no H8A C8 H8B 109.34 . . . no H8A C8 H8C 109.57 . . . no H8B C8 H8C 109.38 . . . no F11 B11 F12 108.0(5) . . . yes F11 B11 F13 112.2(4) . . . yes F11 B11 F14 108.6(5) . . . yes F12 B11 F13 109.3(4) . . . yes F12 B11 F14 106.7(5) . . . yes F13 B11 F14 111.8(5) . . . yes F21 B21 F22 110.2(7) . . . yes F21 B21 F23 111.0(7) . . . yes F21 B21 F24 110.0(7) . . . yes F22 B21 F23 111.3(6) . . . yes F22 B21 F24 104.0(6) . . . yes F23 B21 F24 110.1(6) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Mo11 P11 N11 97.27(14) . . . . no O11 Mo11 P11 C111 -137.79(16) . . . . no O11 Mo11 P11 C121 -18.34(16) . . . . no N12 Mo11 P11 N11 -170.17(16) . . . . no N12 Mo11 P11 C111 -45.24(17) . . . . no N12 Mo11 P11 C121 74.22(17) . . . . no Mo11 Mo11 P11 N11 5.57(13) 3_656 . . . no Mo11 Mo11 P11 C111 130.50(15) 3_656 . . . no Mo11 Mo11 P11 C121 -110.05(14) 3_656 . . . no O12 Mo11 P11 N11 -85.30(14) 3_656 . . . no O12 Mo11 P11 C111 39.63(16) 3_656 . . . no O12 Mo11 P11 C121 159.09(16) 3_656 . . . no P11 Mo11 O11 C12 -98.3(2) . . . . no N12 Mo11 O11 C12 -178.7(3) . . . . no Mo11 Mo11 O11 C12 -0.4(2) 3_656 . . . no P12 Mo11 O11 C12 98.3(2) 3_656 . . . no P11 Mo11 N12 C14 73.5(6) . . . . no O11 Mo11 N12 C14 159.9(6) . . . . no P12 Mo11 N12 C14 -114.9(6) 3_656 . . . no O12 Mo11 N12 C14 -20.4(6) 3_656 . . . no P11 Mo11 Mo11 P12 -7.23(4) . . 3_656 . no P11 Mo11 Mo11 O12 86.80(7) . . 3_656 . no P11 Mo11 Mo11 P11 -180.00(4) . . 3_656 3_656 no P11 Mo11 Mo11 O11 -92.94(7) . . 3_656 3_656 no O11 Mo11 Mo11 P12 -94.29(7) . . 3_656 . no O11 Mo11 Mo11 O12 -0.26(10) . . 3_656 . no O11 Mo11 Mo11 P11 92.94(7) . . 3_656 3_656 no O11 Mo11 Mo11 O11 -180.00(9) . . 3_656 3_656 no P12 Mo11 Mo11 P12 180.00(11) 3_656 . 3_656 . no P12 Mo11 Mo11 O12 -85.97(7) 3_656 . 3_656 . no O12 Mo11 Mo11 P12 85.97(7) 3_656 . 3_656 . no O12 Mo11 Mo11 O12 -179.97(9) 3_656 . 3_656 . no O11 Mo11 P12 N11 -101.69(14) . . 3_656 3_656 no O11 Mo11 P12 C131 16.16(15) . . 3_656 3_656 no O11 Mo11 P12 C141 135.52(16) . . 3_656 3_656 no N12 Mo11 P12 N11 165.75(15) . . 3_656 3_656 no N12 Mo11 P12 C131 -76.40(16) . . 3_656 3_656 no N12 Mo11 P12 C141 42.95(17) . . 3_656 3_656 no P11 Mo11 O12 C12 97.1(3) . . 3_656 3_656 no N12 Mo11 O12 C12 177.4(3) . . 3_656 3_656 no O22 Mo21 P21 C211 40.77(16) 3_566 . . . no O22 Mo21 P21 C221 161.54(15) 3_566 . . . no P21 Mo21 O21 C22 -97.0(2) . . . . no N22 Mo21 O21 C22 -179.0(3) . . . . no Mo21 Mo21 O21 C22 0.5(3) 3_566 . . . no P22 Mo21 O21 C22 99.1(2) 3_566 . . . no P21 Mo21 Mo21 P22 -10.14(4) . . 3_566 . no P21 Mo21 Mo21 O22 84.34(7) . . 3_566 . no P21 Mo21 Mo21 P21 180.0(3) . . 3_566 3_566 no P21 Mo21 Mo21 O21 -95.49(7) . . 3_566 3_566 no O21 Mo21 Mo21 P22 -94.66(7) . . 3_566 . no O21 Mo21 Mo21 O22 -0.18(9) . . 3_566 . no O21 Mo21 Mo21 P21 95.49(7) . . 3_566 3_566 no O21 Mo21 Mo21 O21 -180.00(9) . . 3_566 3_566 no P22 Mo21 Mo21 P22 180.0(6) 3_566 . 3_566 . no P22 Mo21 Mo21 O22 -85.52(7) 3_566 . 3_566 . no O22 Mo21 Mo21 P22 85.52(7) 3_566 . 3_566 . no O22 Mo21 Mo21 O22 -179.98(10) 3_566 . 3_566 . no O21 Mo21 P22 N21 -103.96(14) . . 3_566 3_566 no O21 Mo21 P22 C231 12.53(15) . . 3_566 3_566 no O21 Mo21 P22 C241 134.29(16) . . 3_566 3_566 no O21 Mo21 P21 N21 99.94(14) . . . . no O21 Mo21 P21 C211 -136.86(16) . . . . no O21 Mo21 P21 C221 -16.09(15) . . . . no N22 Mo21 P21 N21 -169.01(15) . . . . no N22 Mo21 P21 C211 -45.81(17) . . . . no N22 Mo21 P21 C221 74.96(16) . . . . no Mo21 Mo21 P21 N21 9.07(12) 3_566 . . . no Mo21 Mo21 P21 C211 132.27(15) 3_566 . . . no Mo21 Mo21 P21 C221 -106.96(13) 3_566 . . . no O22 Mo21 P21 N21 -82.43(14) 3_566 . . . no N22 Mo21 P22 C231 -78.40(16) . . 3_566 3_566 no N22 Mo21 P22 C241 43.36(17) . . 3_566 3_566 no P21 Mo21 O22 C22 97.8(2) . . 3_566 3_566 no N22 Mo21 O22 C22 179.5(3) . . 3_566 3_566 no N22 Mo21 P22 N21 165.11(15) . . 3_566 3_566 no C121 P11 N11 P12 119.2(2) . . . . no C121 P11 N11 C13 -62.8(3) . . . . no Mo11 P11 N11 P12 1.6(2) . . . . no Mo11 P11 N11 C13 179.6(3) . . . . no C111 P11 N11 P12 -130.4(2) . . . . no C111 P11 N11 C13 47.6(3) . . . . no C121 P11 C111 C116 -149.9(3) . . . . no Mo11 P11 C121 C122 89.7(3) . . . . no Mo11 P11 C121 C126 -81.4(3) . . . . no N11 P11 C121 C122 -30.7(4) . . . . no N11 P11 C121 C126 158.1(3) . . . . no C111 P11 C121 C122 -142.0(3) . . . . no C111 P11 C121 C126 46.8(4) . . . . no C121 P11 C111 C112 30.9(4) . . . . no Mo11 P11 C111 C116 -28.6(4) . . . . no N11 P11 C111 C112 -79.8(4) . . . . no Mo11 P11 C111 C112 152.1(3) . . . . no N11 P11 C111 C116 99.5(3) . . . . no C131 P12 N11 C13 -64.0(3) . . . . no C141 P12 N11 P11 -136.4(2) . . . . no C131 P12 N11 P11 113.9(2) . . . . no N11 P12 C131 C132 -24.7(4) . . . . no N11 P12 C131 C136 160.5(3) . . . . no C141 P12 C131 C132 -135.9(3) . . . . no C141 P12 C131 C136 49.2(3) . . . . no Mo11 P12 C131 C132 96.9(3) 3_656 . . . no Mo11 P12 C131 C136 -78.0(3) 3_656 . . . no N11 P12 C141 C142 -74.7(3) . . . . no N11 P12 C141 C146 103.6(3) . . . . no C131 P12 C141 C142 36.3(4) . . . . no C131 P12 C141 C146 -145.4(3) . . . . no Mo11 P12 C141 C142 159.5(3) 3_656 . . . no Mo11 P12 C141 C146 -22.2(4) 3_656 . . . no Mo11 P12 N11 C13 174.8(3) 3_656 . . . no C141 P12 N11 C13 45.7(3) . . . . no Mo11 P12 N11 P11 -7.3(2) 3_656 . . . no Mo21 P21 C221 C222 96.9(3) . . . . no C211 P21 C221 C222 -133.6(3) . . . . no C211 P21 C221 C226 52.8(4) . . . . no C211 P21 N21 P22 -131.6(2) . . . . no C211 P21 N21 C23 43.6(3) . . . . no C221 P21 N21 P22 118.5(2) . . . . no C221 P21 N21 C23 -66.3(3) . . . . no Mo21 P21 C211 C212 150.9(3) . . . . no Mo21 P21 C211 C216 -35.2(4) . . . . no N21 P21 C211 C212 -82.2(4) . . . . no N21 P21 C211 C216 91.6(3) . . . . no C221 P21 C211 C212 27.8(4) . . . . no C221 P21 C211 C216 -158.3(3) . . . . no Mo21 P21 C221 C226 -76.8(3) . . . . no N21 P21 C221 C222 -23.8(4) . . . . no N21 P21 C221 C226 162.6(3) . . . . no Mo21 P21 N21 P22 -0.2(2) . . . . no Mo21 P21 N21 C23 175.1(3) . . . . no C231 P22 N21 P21 111.2(2) . . . . no C231 P22 N21 C23 -64.0(3) . . . . no C241 P22 N21 P21 -137.8(2) . . . . no C241 P22 N21 C23 47.0(3) . . . . no Mo21 P22 N21 P21 -7.8(2) 3_566 . . . no Mo21 P22 N21 C23 177.0(3) 3_566 . . . no N21 P22 C231 C232 -26.8(4) . . . . no N21 P22 C231 C236 161.3(3) . . . . no C241 P22 C231 C232 -137.0(3) . . . . no C241 P22 C231 C236 51.1(4) . . . . no C231 P22 C241 C246 -163.7(3) . . . . no Mo21 P22 C241 C242 144.8(3) 3_566 . . . no Mo21 P22 C231 C232 93.3(3) 3_566 . . . no Mo21 P22 C231 C236 -78.6(3) 3_566 . . . no N21 P22 C241 C242 -90.0(4) . . . . no N21 P22 C241 C246 85.3(3) . . . . no C231 P22 C241 C242 21.0(4) . . . . no Mo21 P22 C241 C246 -39.9(3) 3_566 . . . no Mo11 O11 C12 O12 1.2(5) . . . . no Mo11 O11 C12 C11 -179.1(3) . . . . no Mo11 O12 C12 O11 -1.5(5) 3_656 . . . no Mo11 O12 C12 C11 178.8(2) 3_656 . . . no Mo21 O21 C22 C21 179.7(2) . . . . no Mo21 O21 C22 O22 -0.6(4) . . . . no Mo21 O22 C22 C21 -179.9(3) 3_566 . . . no Mo21 O22 C22 O21 0.4(4) 3_566 . . . no P11 C111 C116 H116 0.27 . . . . no C116 C111 C112 H112 179.80 . . . . no C112 C111 C116 H116 179.55 . . . . no P11 C111 C112 H112 -0.94 . . . . no C111 C112 C113 H113 -179.05 . . . . no H112 C112 C113 H113 1.01 . . . . no H112 C112 C113 C114 -179.15 . . . . no C112 C113 C114 H114 178.91 . . . . no H113 C113 C114 H114 -1.24 . . . . no H113 C113 C114 C115 178.95 . . . . no C113 C114 C115 H115 -179.63 . . . . no H114 C114 C115 C116 -179.46 . . . . no H114 C114 C115 H115 0.56 . . . . no C114 C115 C116 H116 -179.64 . . . . no H115 C115 C116 C111 -179.72 . . . . no H115 C115 C116 H116 0.33 . . . . no C122 C121 C126 H126 179.67 . . . . no P11 C121 C122 H122 8.15 . . . . no C126 C121 C122 H122 179.36 . . . . no P11 C121 C126 H126 -9.11 . . . . no H122 C122 C123 H123 1.49 . . . . no C121 C122 C123 H123 -178.50 . . . . no H122 C122 C123 C124 -178.52 . . . . no C122 C123 C124 H124 178.72 . . . . no H123 C123 C124 H124 -1.29 . . . . no H123 C123 C124 C125 178.64 . . . . no H124 C124 C125 H125 0.27 . . . . no C123 C124 C125 H125 -179.66 . . . . no H124 C124 C125 C126 -179.70 . . . . no C124 C125 C126 H126 -179.52 . . . . no H125 C125 C126 C121 -179.51 . . . . no H125 C125 C126 H126 0.51 . . . . no C132 C131 C136 H136 -179.33 . . . . no P12 C131 C136 H136 -4.40 . . . . no P12 C131 C132 H132 4.55 . . . . no C136 C131 C132 H132 179.36 . . . . no H132 C132 C133 C134 -179.12 . . . . no C131 C132 C133 H133 -179.16 . . . . no H132 C132 C133 H133 0.92 . . . . no H133 C133 C134 C135 178.88 . . . . no C132 C133 C134 H134 179.02 . . . . no H133 C133 C134 H134 -1.02 . . . . no H134 C134 C135 C136 -178.99 . . . . no H134 C134 C135 H135 0.81 . . . . no C133 C134 C135 H135 -179.09 . . . . no C134 C135 C136 H136 179.06 . . . . no H135 C135 C136 H136 -0.74 . . . . no H135 C135 C136 C131 179.34 . . . . no C146 C141 C142 H142 179.14 . . . . no P12 C141 C146 H146 0.75 . . . . no P12 C141 C142 H142 -2.61 . . . . no C142 C141 C146 H146 179.03 . . . . no H142 C142 C143 H143 1.53 . . . . no C141 C142 C143 H143 -178.58 . . . . no H142 C142 C143 C144 -178.57 . . . . no C142 C143 C144 H144 179.82 . . . . no H143 C143 C144 C145 179.87 . . . . no H143 C143 C144 H144 -0.28 . . . . no C143 C144 C145 H145 178.24 . . . . no H144 C144 C145 C146 178.32 . . . . no H144 C144 C145 H145 -1.61 . . . . no C144 C145 C146 H146 -177.74 . . . . no H145 C145 C146 H146 2.19 . . . . no H145 C145 C146 C141 -177.67 . . . . no P21 C211 C212 C213 171.8(3) . . . . no C212 C211 C216 C215 2.6(6) . . . . no C216 C211 C212 C213 -2.1(6) . . . . no P21 C211 C216 C215 -171.5(3) . . . . no C211 C212 C213 C214 0.3(6) . . . . no C212 C213 C214 C215 1.1(7) . . . . no C213 C214 C215 C216 -0.6(7) . . . . no C214 C215 C216 C211 -1.3(6) . . . . no C222 C221 C226 C225 0.1(6) . . . . no P21 C221 C222 C223 -174.0(3) . . . . no C226 C221 C222 C223 -0.4(6) . . . . no P21 C221 C226 C225 173.9(3) . . . . no C221 C222 C223 C224 0.5(6) . . . . no C222 C223 C224 C225 -0.5(6) . . . . no C223 C224 C225 C226 0.2(7) . . . . no C224 C225 C226 C221 0.0(7) . . . . no P22 C231 C232 C233 -172.3(4) . . . . no C236 C231 C232 C233 -0.3(7) . . . . no P22 C231 C236 C235 172.6(3) . . . . no C232 C231 C236 C235 0.7(6) . . . . no C231 C232 C233 C234 -0.3(7) . . . . no C232 C233 C234 C235 0.7(8) . . . . no C233 C234 C235 C236 -0.3(8) . . . . no C234 C235 C236 C231 -0.3(7) . . . . no P22 C241 C242 C243 174.8(4) . . . . no C246 C241 C242 C243 -0.5(6) . . . . no P22 C241 C246 C245 -174.9(3) . . . . no C242 C241 C246 C245 0.6(6) . . . . no C241 C242 C243 C244 0.5(8) . . . . no C242 C243 C244 C245 -0.5(7) . . . . no C243 C244 C245 C246 0.6(7) . . . . no C244 C245 C246 C241 -0.6(7) . . . . no data_GUOA-4018-163 # =================================================================== _chemical_name_systematic ; not known ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H62 Mo2 N4 O4 P4, 2(B F4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68 H62 B2 F8 Mo2 N4 O4 P4' _chemical_formula_weight 1488.60 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' 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' 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 13.7189(4) _cell_length_b 16.1930(5) _cell_length_c 15.4451(5) _cell_angle_alpha 90 _cell_angle_beta 105.437(1) _cell_angle_gamma 90 _cell_volume 3307.35(18) _cell_formula_units_Z 2 _cell_measurement_temperature 163(1) _cell_measurement_reflns_used 33992 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.36 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8748 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details ; Otwinowski, Z.; and Minor, W. "Processing of X-ray Diffraction Data Collected in Oscillation Mode", Metthods in Enzymology 276, 1996. Carter W. C.; Sweet, Jr. & R. M.; Eds., Academic Press, (USA). ; _exptl_special_details ; Diffractometer operator Herdtweck, E. ; _publ_section_exptl_prep ; the crystals were handled in air, fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward. ; # =================================================================== # 7. EXPERIMENTAL DATA # =================================================================== _diffrn_ambient_temperature 163(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kappa CCD (Nonius)' _diffrn_measurement_method ' rotation ' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 20864 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.36 _reflns_number_total 6727 _reflns_number_gt 5671 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Nonius- CCD-Software. ; _computing_data_collection 'Kappa CCD (Nonius)' _computing_cell_refinement 'Denzo and HKL' _computing_data_reduction 'Denzo and HKL' _computing_structure_solution 'SIR-92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON PLUTON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' # =================================================================== # 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+7.1596P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_number_reflns 6727 _refine_ls_number_parameters 519 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.871 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.081 # =================================================================== # 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 Mo Mo Uani 0.06185(2) 0.54179(2) 0.50854(2) 1.000 0.0213(1) P1 P Uani 0.15971(6) 0.46656(5) 0.41124(6) 1.000 0.0239(3) P2 P Uani -0.02286(6) 0.36727(5) 0.36839(6) 1.000 0.0228(3) O1 O Uani 0.15111(16) 0.47281(13) 0.61463(16) 1.000 0.0255(7) O2 O Uani 0.02282(16) 0.38526(13) 0.59731(16) 1.000 0.0259(7) N2 N Uani 0.2129(3) 0.6424(2) 0.5308(3) 1.000 0.0499(14) N1 N Uani 0.09255(19) 0.38684(17) 0.3529(2) 1.000 0.0268(8) C1 C Uani 0.1733(3) 0.3572(3) 0.7146(3) 1.000 0.0424(14) C2 C Uani 0.1127(2) 0.4080(2) 0.6380(2) 1.000 0.0269(10) C3 C Uani 0.1326(3) 0.3386(3) 0.2887(3) 1.000 0.0348(14) C11 C Uani 0.2026(2) 0.5287(2) 0.3298(2) 1.000 0.0280(10) C12 C Uani 0.2860(3) 0.5058(3) 0.3001(3) 1.000 0.0366(11) C13 C Uani 0.3149(3) 0.5527(3) 0.2358(3) 1.000 0.0471(14) C14 C Uani 0.2603(3) 0.6223(3) 0.2008(3) 1.000 0.0485(16) C15 C Uani 0.1792(4) 0.6466(3) 0.2313(3) 1.000 0.0482(16) C16 C Uani 0.1493(3) 0.6003(2) 0.2951(3) 1.000 0.0380(11) C21 C Uani 0.2745(2) 0.4186(2) 0.4792(2) 1.000 0.0300(10) C22 C Uani 0.2778(3) 0.3340(3) 0.4986(3) 1.000 0.0385(12) C23 C Uani 0.3655(4) 0.2992(3) 0.5518(3) 1.000 0.0538(17) C24 C Uani 0.4495(3) 0.3468(4) 0.5866(3) 1.000 0.0562(18) C25 C Uani 0.4462(3) 0.4308(4) 0.5709(3) 1.000 0.0541(18) C26 C Uani 0.3585(3) 0.4668(3) 0.5177(3) 1.000 0.0423(15) C31 C Uani -0.1113(2) 0.3874(2) 0.2598(2) 1.000 0.0265(10) C32 C Uani -0.0858(3) 0.4412(3) 0.1989(3) 1.000 0.0411(12) C33 C Uani -0.1565(4) 0.4600(3) 0.1186(3) 1.000 0.0556(17) C34 C Uani -0.2523(3) 0.4270(3) 0.0993(3) 1.000 0.0527(14) C35 C Uani -0.2789(3) 0.3747(3) 0.1598(3) 1.000 0.0446(14) C36 C Uani -0.2091(3) 0.3558(2) 0.2401(3) 1.000 0.0343(11) C41 C Uani -0.0303(2) 0.25580(19) 0.3821(2) 1.000 0.0244(9) C42 C Uani -0.0499(3) 0.2025(2) 0.3082(3) 1.000 0.0295(10) C43 C Uani -0.0535(3) 0.1175(2) 0.3204(3) 1.000 0.0335(11) C44 C Uani -0.0394(3) 0.0859(2) 0.4059(3) 1.000 0.0361(11) C45 C Uani -0.0217(3) 0.1379(2) 0.4791(3) 1.000 0.0386(11) C46 C Uani -0.0166(3) 0.2231(2) 0.4673(3) 1.000 0.0321(11) C50 C Uani 0.2572(4) 0.6989(3) 0.5163(4) 1.000 0.0595(17) C51 C Uani 0.3105(4) 0.7719(3) 0.4935(4) 1.000 0.0557(16) C52 C Uani 0.4139(4) 0.7835(3) 0.5342(4) 1.000 0.0612(17) C53 C Uani 0.4665(5) 0.8558(5) 0.5076(4) 1.000 0.075(2) C54 C Uani 0.4233(9) 0.9021(4) 0.4584(6) 1.000 0.117(4) C55 C Uani 0.3072(7) 0.8956(4) 0.4146(5) 1.000 0.099(3) C56 C Uani 0.2607(4) 0.8245(4) 0.4370(4) 1.000 0.0664(19) F1 F Uani 0.5793(3) 0.65774(19) 0.6985(3) 1.000 0.0926(15) F2 F Uani 0.5137(4) 0.7142(2) 0.8004(4) 1.000 0.129(2) F3 F Uani 0.4152(3) 0.6549(5) 0.6900(4) 1.000 0.184(3) F4 F Uani 0.5206(3) 0.5801(2) 0.7968(3) 1.000 0.0965(16) B B Uani 0.5086(4) 0.6481(3) 0.7447(5) 1.000 0.060(2) H11 H Uiso 0.135(4) 0.324(3) 0.738(4) 1.000 0.068(16) H12 H Uiso 0.205(3) 0.393(3) 0.764(3) 1.000 0.053(13) H13 H Uiso 0.220(5) 0.325(4) 0.687(4) 1.000 0.10(2) H31 H Uiso 0.202(4) 0.346(3) 0.298(3) 1.000 0.062(14) H32 H Uiso 0.101(4) 0.356(3) 0.228(3) 1.000 0.056(14) H33 H Uiso 0.122(4) 0.287(4) 0.295(4) 1.000 0.073(17) H121 H Uiso 0.321(3) 0.460(3) 0.321(3) 1.000 0.042(12) H131 H Uiso 0.364(4) 0.531(3) 0.213(4) 1.000 0.069(16) H141 H Uiso 0.276(3) 0.651(3) 0.152(3) 1.000 0.052(13) H151 H Uiso 0.147(4) 0.691(3) 0.209(4) 1.000 0.071(17) H161 H Uiso 0.092(3) 0.615(2) 0.312(3) 1.000 0.038(11) H221 H Uiso 0.225(3) 0.303(3) 0.476(3) 1.000 0.037(11) H231 H Uiso 0.363(4) 0.246(3) 0.563(3) 1.000 0.057(15) H241 H Uiso 0.512(4) 0.326(3) 0.624(3) 1.000 0.066(15) H251 H Uiso 0.497(4) 0.467(3) 0.595(3) 1.000 0.052(13) H261 H Uiso 0.356(3) 0.517(3) 0.504(3) 1.000 0.051(14) H321 H Uiso -0.023(4) 0.467(3) 0.212(3) 1.000 0.050(13) H331 H Uiso -0.138(4) 0.493(3) 0.074(3) 1.000 0.061(14) H341 H Uiso -0.298(4) 0.438(3) 0.040(4) 1.000 0.071(16) H351 H Uiso -0.346(3) 0.352(3) 0.147(3) 1.000 0.049(12) H361 H Uiso -0.226(3) 0.324(2) 0.282(3) 1.000 0.027(10) H421 H Uiso -0.060(3) 0.225(2) 0.247(2) 1.000 0.024(9) H431 H Uiso -0.068(3) 0.087(2) 0.270(3) 1.000 0.033(10) H441 H Uiso -0.045(3) 0.031(3) 0.415(3) 1.000 0.046(12) H451 H Uiso -0.014(3) 0.120(2) 0.536(3) 1.000 0.032(10) H461 H Uiso -0.007(3) 0.255(2) 0.516(2) 1.000 0.019(9) H521 H Uiso 0.45000 0.74570 0.57810 1.000 0.0730 H531 H Uiso 0.53720 0.86270 0.53260 1.000 0.0890 H541 H Uiso 0.45890 0.94750 0.44250 1.000 0.1400 H551 H Uiso 0.27060 0.93680 0.37550 1.000 0.1200 H561 H Uiso 0.19090 0.81530 0.40970 1.000 0.0800 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 Mo 0.0152(1) 0.0166(1) 0.0324(2) 0.0013(1) 0.0066(1) -0.0015(1) P1 0.0161(4) 0.0205(4) 0.0362(5) 0.0022(4) 0.0087(3) -0.0004(3) P2 0.0184(4) 0.0171(4) 0.0331(5) 0.0017(3) 0.0074(3) -0.0011(3) O1 0.0177(10) 0.0219(11) 0.0356(13) 0.0015(10) 0.0047(9) 0.0014(9) O2 0.0227(11) 0.0201(11) 0.0351(13) 0.0029(10) 0.0081(10) 0.0000(9) N2 0.0401(19) 0.046(2) 0.069(3) -0.0141(18) 0.0242(18) -0.0253(17) N1 0.0209(13) 0.0205(13) 0.0422(17) -0.0019(12) 0.0142(12) -0.0020(11) C1 0.035(2) 0.037(2) 0.049(3) 0.015(2) 0.0002(19) 0.0052(18) C2 0.0233(16) 0.0223(16) 0.0362(19) 0.0019(14) 0.0096(14) 0.0045(13) C3 0.031(2) 0.030(2) 0.048(3) -0.0055(18) 0.0188(18) -0.0013(16) C11 0.0226(15) 0.0239(17) 0.0379(19) 0.0013(15) 0.0090(14) -0.0042(13) C12 0.0272(18) 0.035(2) 0.051(2) 0.0043(18) 0.0162(17) 0.0002(16) C13 0.040(2) 0.047(2) 0.063(3) 0.003(2) 0.029(2) -0.0054(19) C14 0.056(3) 0.039(2) 0.059(3) 0.011(2) 0.030(2) -0.010(2) C15 0.055(3) 0.035(2) 0.059(3) 0.015(2) 0.023(2) 0.005(2) C16 0.0326(19) 0.036(2) 0.049(2) 0.0090(18) 0.0173(18) 0.0020(16) C21 0.0194(15) 0.0362(19) 0.037(2) 0.0074(16) 0.0122(14) 0.0067(14) C22 0.034(2) 0.038(2) 0.045(2) 0.0100(19) 0.0131(18) 0.0053(18) C23 0.053(3) 0.057(3) 0.054(3) 0.024(2) 0.019(2) 0.024(2) C24 0.032(2) 0.090(4) 0.047(3) 0.030(3) 0.0113(19) 0.024(2) C25 0.0214(19) 0.086(4) 0.052(3) 0.017(3) 0.0045(18) -0.002(2) C26 0.0239(18) 0.049(3) 0.052(3) 0.010(2) 0.0067(17) 0.0002(18) C31 0.0247(16) 0.0226(16) 0.0318(18) 0.0020(14) 0.0070(13) 0.0035(13) C32 0.032(2) 0.042(2) 0.049(2) 0.0179(19) 0.0105(17) 0.0015(17) C33 0.050(3) 0.065(3) 0.052(3) 0.032(2) 0.014(2) 0.008(2) C34 0.042(2) 0.071(3) 0.041(2) 0.010(2) 0.004(2) 0.015(2) C35 0.0276(19) 0.059(3) 0.044(2) 0.000(2) 0.0039(17) 0.0014(19) C36 0.0285(18) 0.039(2) 0.035(2) 0.0011(17) 0.0078(16) -0.0030(16) C41 0.0185(14) 0.0185(15) 0.0359(19) 0.0027(14) 0.0069(13) 0.0001(12) C42 0.0304(17) 0.0239(17) 0.037(2) -0.0015(15) 0.0136(15) -0.0005(14) C43 0.0299(18) 0.0232(17) 0.047(2) -0.0073(17) 0.0096(16) -0.0001(14) C44 0.0344(19) 0.0168(17) 0.054(2) 0.0041(17) 0.0065(17) 0.0007(14) C45 0.044(2) 0.0232(18) 0.043(2) 0.0088(17) 0.0016(18) 0.0016(16) C46 0.0334(19) 0.0217(17) 0.038(2) -0.0016(16) 0.0039(16) 0.0005(14) C50 0.050(3) 0.067(3) 0.062(3) -0.012(3) 0.016(2) -0.005(2) C51 0.045(2) 0.056(3) 0.069(3) -0.010(3) 0.020(2) -0.011(2) C52 0.047(3) 0.068(3) 0.069(3) 0.008(3) 0.016(2) -0.014(2) C53 0.062(3) 0.092(5) 0.063(4) -0.025(3) 0.005(3) 0.021(3) C54 0.240(11) 0.052(4) 0.107(6) -0.040(4) 0.131(7) -0.073(5) C55 0.170(8) 0.066(4) 0.074(4) 0.019(3) 0.053(5) 0.023(5) C56 0.069(3) 0.076(4) 0.054(3) 0.013(3) 0.016(3) -0.010(3) F1 0.105(3) 0.0549(18) 0.151(3) 0.006(2) 0.092(3) 0.0141(18) F2 0.181(5) 0.061(2) 0.187(5) -0.016(3) 0.120(4) 0.011(3) F3 0.080(3) 0.327(9) 0.135(4) 0.091(5) 0.013(3) -0.040(4) F4 0.125(3) 0.058(2) 0.131(3) 0.024(2) 0.077(3) 0.017(2) B 0.049(3) 0.042(3) 0.098(5) 0.002(3) 0.033(3) 0.004(2) # =================================================================== # 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 P1 2.5727(9) . . yes Mo O1 2.089(2) . . yes Mo N2 2.586(4) . . yes Mo Mo 2.1313(4) . 3_566 yes Mo P2 2.5709(9) . 3_566 yes Mo O2 2.099(2) . 3_566 yes P1 N1 1.699(3) . . yes P1 C11 1.826(3) . . yes P1 C21 1.818(3) . . yes P2 N1 1.693(3) . . yes P2 C31 1.819(3) . . yes P2 C41 1.823(3) . . yes F1 B 1.357(8) . . yes F2 B 1.363(7) . . yes F3 B 1.338(8) . . yes F4 B 1.348(7) . . yes O1 C2 1.269(4) . . yes O2 C2 1.280(4) . . yes N2 C50 1.153(6) . . yes N1 C3 1.478(5) . . yes C1 C2 1.498(5) . . no C11 C12 1.392(5) . . no C11 C16 1.399(5) . . no C12 C13 1.389(6) . . no C13 C14 1.381(7) . . no C14 C15 1.376(7) . . no C15 C16 1.384(6) . . no C21 C26 1.388(5) . . no C21 C22 1.400(6) . . no C22 C23 1.383(7) . . no C23 C24 1.372(7) . . no C24 C25 1.380(9) . . no C25 C26 1.391(7) . . no C31 C36 1.392(5) . . no C31 C32 1.393(6) . . no C32 C33 1.390(7) . . no C33 C34 1.376(7) . . no C34 C35 1.380(6) . . no C35 C36 1.384(6) . . no C41 C46 1.384(5) . . no C41 C42 1.399(5) . . no C42 C43 1.392(5) . . no C43 C44 1.381(6) . . no C44 C45 1.378(6) . . no C45 C46 1.396(5) . . no C50 C51 1.481(7) . . no C51 C52 1.403(8) . . no C51 C56 1.279(8) . . no C52 C53 1.489(9) . . no C53 C54 1.118(11) . . no C54 C55 1.559(15) . . no C55 C56 1.403(10) . . no C1 H13 1.00(7) . . no C1 H11 0.89(5) . . no C1 H12 0.96(5) . . no C3 H33 0.86(6) . . no C3 H32 0.96(5) . . no C3 H31 0.93(6) . . no C12 H121 0.90(5) . . no C13 H131 0.91(6) . . no C14 H141 0.96(5) . . no C15 H151 0.87(5) . . no C16 H161 0.92(4) . . no C22 H221 0.87(5) . . no C23 H231 0.88(5) . . no C24 H241 0.96(5) . . no C25 H251 0.91(5) . . no C26 H261 0.84(5) . . no C32 H321 0.93(5) . . no C33 H331 0.96(5) . . no C34 H341 0.98(6) . . no C35 H351 0.96(4) . . no C36 H361 0.90(4) . . no C42 H421 0.99(3) . . no C43 H431 0.90(4) . . no C44 H441 0.91(5) . . no C45 H451 0.90(4) . . no C46 H461 0.89(3) . . no C52 H521 0.9492 . . no C53 H531 0.9502 . . no C54 H541 0.9503 . . no C55 H551 0.9489 . . no C56 H561 0.9497 . . 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 P1 Mo O1 85.23(7) . . . yes P1 Mo N2 81.47(9) . . . yes Mo Mo P1 98.58(2) 3_566 . . yes P1 Mo P2 161.22(3) . . 3_566 yes P1 Mo O2 94.48(7) . . 3_566 yes O1 Mo N2 87.18(11) . . . yes Mo Mo O1 92.22(6) 3_566 . . yes P2 Mo O1 85.42(7) 3_566 . . yes O1 Mo O2 177.57(9) . . 3_566 yes Mo Mo N2 179.40(9) 3_566 . . yes P2 Mo N2 81.83(9) 3_566 . . yes O2 Mo N2 90.38(11) 3_566 . . yes Mo Mo P2 98.03(2) 3_566 . 3_566 yes Mo Mo O2 90.21(6) 3_566 . 3_566 yes P2 Mo O2 94.16(7) 3_566 . 3_566 yes Mo P1 N1 112.09(10) . . . yes Mo P1 C11 117.09(10) . . . yes Mo P1 C21 111.81(10) . . . yes N1 P1 C11 106.38(15) . . . yes N1 P1 C21 104.23(14) . . . yes C11 P1 C21 104.16(14) . . . yes N1 P2 C31 104.81(14) . . . yes N1 P2 C41 106.56(14) . . . yes Mo P2 N1 112.56(11) 3_566 . . yes C31 P2 C41 103.90(14) . . . yes Mo P2 C31 111.11(10) 3_566 . . yes Mo P2 C41 116.88(10) 3_566 . . yes Mo O1 C2 117.7(2) . . . yes Mo O2 C2 118.8(2) 3_566 . . yes Mo N2 C50 156.8(4) . . . yes P1 N1 P2 117.58(17) . . . yes P1 N1 C3 120.8(2) . . . yes P2 N1 C3 121.6(3) . . . yes O1 C2 O2 121.1(3) . . . yes O1 C2 C1 119.6(3) . . . yes O2 C2 C1 119.3(3) . . . yes P1 C11 C12 121.6(3) . . . yes P1 C11 C16 119.3(3) . . . yes C12 C11 C16 119.1(3) . . . no C11 C12 C13 120.4(4) . . . no C12 C13 C14 119.8(4) . . . no C13 C14 C15 120.2(4) . . . no C14 C15 C16 120.6(4) . . . no C11 C16 C15 119.9(4) . . . no P1 C21 C22 121.0(3) . . . yes P1 C21 C26 120.0(3) . . . yes C22 C21 C26 118.9(3) . . . no C21 C22 C23 119.9(4) . . . no C22 C23 C24 120.7(5) . . . no C23 C24 C25 120.0(4) . . . no C24 C25 C26 120.0(5) . . . no C21 C26 C25 120.4(4) . . . no P2 C31 C32 120.6(3) . . . yes P2 C31 C36 120.2(3) . . . yes C32 C31 C36 118.9(3) . . . no C31 C32 C33 119.9(4) . . . no C32 C33 C34 120.5(4) . . . no C33 C34 C35 120.1(4) . . . no C34 C35 C36 119.8(4) . . . no C31 C36 C35 120.7(4) . . . no P2 C41 C42 121.4(2) . . . yes P2 C41 C46 119.4(2) . . . yes C42 C41 C46 119.2(3) . . . no C41 C42 C43 120.4(4) . . . no C42 C43 C44 119.7(4) . . . no C43 C44 C45 120.5(3) . . . no C44 C45 C46 120.0(4) . . . no C41 C46 C45 120.2(4) . . . no N2 C50 C51 177.3(6) . . . yes C50 C51 C52 120.3(5) . . . no C50 C51 C56 119.1(5) . . . no C52 C51 C56 120.6(5) . . . no C51 C52 C53 119.2(5) . . . no C52 C53 C54 120.4(8) . . . no C53 C54 C55 123.0(9) . . . no C54 C55 C56 115.3(6) . . . no C51 C56 C55 121.3(6) . . . no C2 C1 H11 113(4) . . . no C2 C1 H12 109(3) . . . no C2 C1 H13 103(3) . . . no H11 C1 H12 103(5) . . . no H11 C1 H13 112(5) . . . no H12 C1 H13 116(5) . . . no N1 C3 H31 112(3) . . . no N1 C3 H32 110(3) . . . no N1 C3 H33 110(4) . . . no H31 C3 H32 107(4) . . . no H31 C3 H33 108(5) . . . no H32 C3 H33 110(5) . . . no C11 C12 H121 121(3) . . . no C13 C12 H121 119(3) . . . no C12 C13 H131 117(3) . . . no C14 C13 H131 123(3) . . . no C13 C14 H141 119(3) . . . no C15 C14 H141 120(3) . . . no C14 C15 H151 118(4) . . . no C16 C15 H151 121(4) . . . no C11 C16 H161 120(2) . . . no C15 C16 H161 120(2) . . . no C21 C22 H221 120(3) . . . no C23 C22 H221 120(3) . . . no C22 C23 H231 116(3) . . . no C24 C23 H231 123(3) . . . no C23 C24 H241 124(3) . . . no C25 C24 H241 116(3) . . . no C24 C25 H251 125(3) . . . no C26 C25 H251 115(3) . . . no C21 C26 H261 118(3) . . . no C25 C26 H261 122(3) . . . no C31 C32 H321 121(3) . . . no C33 C32 H321 119(3) . . . no C32 C33 H331 121(3) . . . no C34 C33 H331 119(3) . . . no C33 C34 H341 118(3) . . . no C35 C34 H341 122(3) . . . no C34 C35 H351 120(3) . . . no C36 C35 H351 120(3) . . . no C31 C36 H361 118(3) . . . no C35 C36 H361 121(3) . . . no C41 C42 H421 120.1(19) . . . no C43 C42 H421 119.6(19) . . . no C42 C43 H431 116(2) . . . no C44 C43 H431 125(2) . . . no C43 C44 H441 121(3) . . . no C45 C44 H441 118(3) . . . no C44 C45 H451 123(2) . . . no C46 C45 H451 117(2) . . . no C41 C46 H461 122(2) . . . no C45 C46 H461 118(2) . . . no C51 C52 H521 120.45 . . . no C53 C52 H521 120.33 . . . no C52 C53 H531 119.83 . . . no C54 C53 H531 119.75 . . . no C53 C54 H541 118.57 . . . no C55 C54 H541 118.42 . . . no C54 C55 H551 122.34 . . . no C56 C55 H551 122.37 . . . no C51 C56 H561 119.39 . . . no C55 C56 H561 119.34 . . . no F1 B F2 108.5(5) . . . yes F1 B F3 110.9(6) . . . yes F1 B F4 114.6(5) . . . yes F2 B F3 102.3(5) . . . yes F2 B F4 106.7(6) . . . yes F3 B F4 112.9(5) . . . yes # End of Crystallographic Information File #=================================================================== data_GUOB-3068-163 #=================================================================== _chemical_name_systematic ; not known ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H52 B2 F8 Mo2 N2 O4 P4, C54 H52 Mo2 N2 O4 P4, 4(C H2 Cl2), 2(B F4)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C112 H112 B4 Cl8 F16 Mo4 N4 O8 P8' _chemical_formula_weight 2904.42 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.711(1) _cell_length_b 14.003(1) _cell_length_c 17.822(2) _cell_angle_alpha 68.73(1) _cell_angle_beta 77.20(1) _cell_angle_gamma 89.44(1) _cell_volume 3100.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 163(1) _cell_measurement_reflns_used 4827 _cell_measurement_theta_min 10.8 _cell_measurement_theta_max 25.8 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5995 _exptl_absorpt_correction_T_max 0.8175 _exptl_absorpt_process_details ; IPDS Operating System Version 2.8. Stoe&Cie. GmbH, Darmstadt, Deutschland, (1997). Programm DECAY: SF=3 ; _exptl_special_details ; Diffractometer operator Herdtweck, E. ; _publ_section_exptl_prep ; the crystals were handled in air, fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 163(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'IPDS (STOE)' _diffrn_measurement_method ' rotation ' _diffrn_standards_interval_time ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 30270 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.64 _reflns_number_total 10855 _reflns_number_gt 9103 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; MoleN-Software. ; _computing_data_collection 'IPDS (STOE)' _computing_cell_refinement 'IPDS (STOE)' _computing_data_reduction 'IPDS (STOE)' _computing_structure_solution 'SIR92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'PLATON (Spek, 1999)' #=================================================================== # 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+4.9451P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_number_reflns 10855 _refine_ls_number_parameters 739 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 2.277 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.108 #=================================================================== # 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 Mo11 Mo Uani -0.01049(2) 0.56573(2) 0.45012(2) 1.000 0.0160(1) P11 P Uani 0.01291(7) 0.69812(7) 0.51542(6) 1.000 0.0178(3) P12 P Uani 0.07704(7) 0.52223(8) 0.63559(6) 1.000 0.0182(3) F11 F Uani -0.0283(5) 0.7235(3) 0.3308(3) 1.000 0.107(2) F12 F Uani -0.0760(2) 0.7897(3) 0.21170(16) 1.000 0.0454(9) F13 F Uani 0.0720(2) 0.8480(4) 0.2209(3) 1.000 0.0841(18) F14 F Uani -0.0679(3) 0.8847(3) 0.2901(2) 1.000 0.0642(12) O11 O Uani -0.16179(19) 0.5631(2) 0.50507(16) 1.000 0.0213(8) O12 O Uani -0.14139(19) 0.4261(2) 0.61130(16) 1.000 0.0223(8) N11 N Uani 0.0662(2) 0.6500(3) 0.5974(2) 1.000 0.0227(10) C11 C Uani -0.3034(3) 0.4916(4) 0.6182(3) 1.000 0.0394(16) C12 C Uani -0.1962(3) 0.4940(3) 0.5754(2) 1.000 0.0232(11) C13 C Uani 0.0980(4) 0.7185(3) 0.6360(3) 1.000 0.0332(14) C111 C Uani 0.0887(3) 0.8151(3) 0.4481(2) 1.000 0.0211(11) C112 C Uani 0.0715(4) 0.9097(4) 0.4564(3) 1.000 0.0390(17) C113 C Uani 0.1347(4) 0.9951(4) 0.4064(3) 1.000 0.0460(17) C114 C Uani 0.2157(3) 0.9896(4) 0.3472(3) 1.000 0.0332(12) C115 C Uani 0.2330(3) 0.8972(3) 0.3383(3) 1.000 0.0305(14) C116 C Uani 0.1705(3) 0.8108(3) 0.3874(2) 1.000 0.0254(12) C121 C Uani -0.1072(3) 0.7376(3) 0.5572(2) 1.000 0.0209(11) C122 C Uani -0.1482(3) 0.7006(3) 0.6420(2) 1.000 0.0264(11) C123 C Uani -0.2426(3) 0.7263(4) 0.6730(3) 1.000 0.0314(14) C124 C Uani -0.2971(3) 0.7873(4) 0.6192(3) 1.000 0.0342(16) C125 C Uani -0.2572(3) 0.8230(4) 0.5356(3) 1.000 0.0359(16) C126 C Uani -0.1621(3) 0.7991(3) 0.5035(3) 1.000 0.0279(11) C131 C Uani 0.2112(3) 0.5116(3) 0.6246(2) 1.000 0.0204(11) C132 C Uani 0.2782(3) 0.5905(4) 0.5665(3) 1.000 0.0296(14) C133 C Uani 0.3805(3) 0.5791(4) 0.5535(3) 1.000 0.0396(14) C134 C Uani 0.4153(3) 0.4882(4) 0.5994(3) 1.000 0.0397(16) C135 C Uani 0.3495(3) 0.4093(4) 0.6563(3) 1.000 0.0327(14) C136 C Uani 0.2463(3) 0.4192(3) 0.6696(3) 1.000 0.0272(12) C141 C Uani 0.0251(3) 0.4807(3) 0.7465(2) 1.000 0.0241(11) C142 C Uani 0.0820(3) 0.4881(4) 0.8003(3) 1.000 0.0365(14) C143 C Uani 0.0376(4) 0.4609(4) 0.8840(3) 1.000 0.0438(18) C144 C Uani -0.0627(4) 0.4280(4) 0.9137(3) 1.000 0.0416(16) C145 C Uani -0.1189(4) 0.4197(4) 0.8613(3) 1.000 0.0397(14) C146 C Uani -0.0755(3) 0.4459(4) 0.7774(3) 1.000 0.0324(14) B11 B Uani -0.0245(4) 0.8122(4) 0.2623(3) 1.000 0.0322(14) Mo21 Mo Uani 0.50129(2) 0.96548(3) -0.04389(2) 1.000 0.0196(1) P21 P Uani 0.62544(8) 0.83030(9) 0.00546(6) 1.000 0.0252(3) P22 P Uani 0.64539(7) 0.94838(8) 0.10688(6) 1.000 0.0219(3) O21 O Uani 0.3910(2) 0.8514(2) 0.03726(16) 1.000 0.0254(9) O22 O Uani 0.38680(19) 0.9217(2) 0.13054(15) 1.000 0.0240(8) N23 N Uani 0.6851(3) 0.8545(3) 0.0715(2) 1.000 0.0307(11) C21 C Uani 0.2847(4) 0.7668(4) 0.1707(3) 1.000 0.0377(14) C22 C Uani 0.3576(3) 0.8515(3) 0.1096(2) 1.000 0.0255(11) C23 C Uani 0.7702(3) 0.7944(4) 0.0971(3) 1.000 0.0407(14) C211 C Uani 0.7292(3) 0.8112(4) -0.0704(2) 1.000 0.0288(14) C212 C Uani 0.7560(4) 0.7140(4) -0.0672(3) 1.000 0.0413(17) C213 C Uani 0.8435(4) 0.7055(5) -0.1213(3) 1.000 0.0509(19) C214 C Uani 0.9030(4) 0.7906(5) -0.1758(3) 1.000 0.0488(19) C215 C Uani 0.8760(4) 0.8877(5) -0.1801(3) 1.000 0.0450(18) C216 C Uani 0.7887(3) 0.8981(4) -0.1282(3) 1.000 0.0356(14) C221 C Uani 0.5587(3) 0.7048(4) 0.0633(3) 1.000 0.0321(14) C222 C Uani 0.5494(4) 0.6579(4) 0.1483(3) 1.000 0.0401(16) C223 C Uani 0.4943(4) 0.5649(5) 0.1928(3) 1.000 0.0523(19) C224 C Uani 0.4458(4) 0.5182(5) 0.1546(4) 1.000 0.0556(19) C225 C Uani 0.4527(4) 0.5652(5) 0.0697(4) 1.000 0.055(2) C226 C Uani 0.5090(4) 0.6575(4) 0.0245(3) 1.000 0.0408(16) C231 C Uani 0.7576(3) 1.0368(4) 0.0778(3) 1.000 0.0325(14) C232 C Uani 0.8295(4) 1.0484(5) 0.0061(3) 1.000 0.0469(16) C233 C Uani 0.9152(4) 1.1174(5) -0.0174(3) 1.000 0.0524(16) C234 C Uani 0.9291(4) 1.1676(5) 0.0332(4) 1.000 0.053(2) C235 C Uani 0.8568(4) 1.1567(5) 0.1045(4) 1.000 0.053(2) C236 C Uani 0.7706(4) 1.0917(4) 0.1262(3) 1.000 0.0401(16) C241 C Uani 0.6223(3) 0.8909(3) 0.2192(2) 1.000 0.0203(11) C242 C Uani 0.7004(3) 0.8727(3) 0.2599(2) 1.000 0.0258(11) C243 C Uani 0.6798(3) 0.8303(4) 0.3453(3) 1.000 0.0309(14) C244 C Uani 0.5821(3) 0.8071(4) 0.3912(2) 1.000 0.0332(13) C245 C Uani 0.5036(3) 0.8246(4) 0.3514(2) 1.000 0.0316(14) C246 C Uani 0.5239(3) 0.8659(3) 0.2656(2) 1.000 0.0256(11) Cl1 Cl Uani 0.65738(16) 0.35885(15) 0.26412(12) 1.000 0.0796(7) Cl2 Cl Uani 0.72414(14) 0.44464(19) 0.08338(13) 1.000 0.0914(8) C1 C Uani 0.6512(5) 0.3481(6) 0.1707(4) 1.000 0.069(3) Cl3 Cl Uani 0.7700(2) 0.07598(19) 0.34263(13) 1.000 0.1055(9) Cl4 Cl Uani 0.6313(2) 0.0897(2) 0.48631(15) 1.000 0.1202(13) C2 C Uani 0.6404(7) 0.0793(6) 0.3902(4) 1.000 0.080(3) F21 F Uani 0.4357(2) 0.2382(2) 0.19012(19) 1.000 0.0515(10) F22 F Uani 0.4146(4) 0.0756(3) 0.1969(4) 1.000 0.102(2) F23 F Uani 0.5496(3) 0.1586(4) 0.1290(2) 1.000 0.0884(16) F24 F Uani 0.5123(6) 0.1156(4) 0.2669(3) 1.000 0.151(3) B21 B Uani 0.4787(4) 0.1468(4) 0.2008(3) 1.000 0.0347(17) H11A H Uiso -0.31850 0.43370 0.67150 1.000 0.0590 H11B H Uiso -0.34690 0.48360 0.58370 1.000 0.0590 H11C H Uiso -0.31520 0.55600 0.62750 1.000 0.0590 H13A H Uiso 0.08590 0.78950 0.60510 1.000 0.0500 H13B H Uiso 0.16970 0.71380 0.63480 1.000 0.0500 H13C H Uiso 0.05950 0.69720 0.69350 1.000 0.0500 H112 H Uiso 0.01580 0.91480 0.49700 1.000 0.0470 H113 H Uiso 0.12240 1.05900 0.41270 1.000 0.0550 H114 H Uiso 0.25910 1.04910 0.31290 1.000 0.0400 H115 H Uiso 0.28900 0.89300 0.29760 1.000 0.0360 H116 H Uiso 0.18310 0.74760 0.38000 1.000 0.0300 H122 H Uiso -0.11150 0.65760 0.67900 1.000 0.0310 H123 H Uiso -0.26980 0.70200 0.73110 1.000 0.0380 H124 H Uiso -0.36210 0.80430 0.64020 1.000 0.0420 H125 H Uiso -0.29480 0.86470 0.49890 1.000 0.0430 H126 H Uiso -0.13490 0.82470 0.44540 1.000 0.0330 H132 H Uiso 0.25430 0.65280 0.53520 1.000 0.0360 H133 H Uiso 0.42650 0.63340 0.51340 1.000 0.0480 H134 H Uiso 0.48540 0.48070 0.59110 1.000 0.0470 H135 H Uiso 0.37420 0.34710 0.68710 1.000 0.0390 H136 H Uiso 0.20060 0.36400 0.70880 1.000 0.0330 H142 H Uiso 0.15100 0.51180 0.77980 1.000 0.0440 H143 H Uiso 0.07650 0.46490 0.92090 1.000 0.0520 H144 H Uiso -0.09310 0.41100 0.97080 1.000 0.0500 H145 H Uiso -0.18780 0.39600 0.88230 1.000 0.0470 H146 H Uiso -0.11470 0.43990 0.74130 1.000 0.0390 H21A H Uiso 0.28480 0.76260 0.22680 1.000 0.0570 H21B H Uiso 0.30360 0.70180 0.16490 1.000 0.0570 H21C H Uiso 0.21740 0.78020 0.16090 1.000 0.0570 H23A H Uiso 0.78220 0.74380 0.07060 1.000 0.0610 H23B H Uiso 0.75360 0.75880 0.15740 1.000 0.0610 H23C H Uiso 0.83060 0.84100 0.08030 1.000 0.0610 H212 H Uiso 0.71530 0.65420 -0.02880 1.000 0.0490 H213 H Uiso 0.86180 0.63950 -0.12000 1.000 0.0610 H214 H Uiso 0.96320 0.78330 -0.21110 1.000 0.0580 H215 H Uiso 0.91740 0.94700 -0.21850 1.000 0.0540 H216 H Uiso 0.76920 0.96470 -0.13200 1.000 0.0430 H222 H Uiso 0.58150 0.69020 0.17590 1.000 0.0480 H223 H Uiso 0.49000 0.53300 0.25060 1.000 0.0630 H224 H Uiso 0.40770 0.45430 0.18560 1.000 0.0660 H225 H Uiso 0.41850 0.53350 0.04290 1.000 0.0660 H226 H Uiso 0.51380 0.68890 -0.03340 1.000 0.0490 H232 H Uiso 0.82120 1.01040 -0.02690 1.000 0.0560 H233 H Uiso 0.96290 1.12890 -0.06800 1.000 0.0630 H234 H Uiso 0.98890 1.21020 0.01930 1.000 0.0640 H235 H Uiso 0.86600 1.19340 0.13830 1.000 0.0640 H236 H Uiso 0.72040 1.08500 0.17440 1.000 0.0480 H242 H Uiso 0.76800 0.88950 0.22880 1.000 0.0310 H243 H Uiso 0.73340 0.81700 0.37270 1.000 0.0370 H244 H Uiso 0.56850 0.77920 0.44990 1.000 0.0400 H245 H Uiso 0.43620 0.80830 0.38290 1.000 0.0380 H246 H Uiso 0.47020 0.87720 0.23840 1.000 0.0310 H1A H Uiso 0.58040 0.35010 0.16630 1.000 0.0820 H1B H Uiso 0.67360 0.28040 0.17130 1.000 0.0820 H2A H Uiso 0.61160 0.13860 0.35400 1.000 0.0960 H2B H Uiso 0.60190 0.01570 0.39760 1.000 0.0960 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 Mo11 0.0147(2) 0.0186(2) 0.0166(2) -0.0077(1) -0.0057(1) 0.0053(1) P11 0.0178(4) 0.0196(5) 0.0186(4) -0.0089(4) -0.0062(4) 0.0057(4) P12 0.0170(4) 0.0216(5) 0.0176(4) -0.0076(4) -0.0066(4) 0.0043(4) F11 0.220(6) 0.0355(19) 0.076(3) 0.0080(18) -0.105(3) 0.000(3) F12 0.0341(14) 0.069(2) 0.0329(14) -0.0148(14) -0.0146(12) 0.0032(14) F13 0.0306(17) 0.152(4) 0.087(3) -0.069(3) -0.0053(17) -0.005(2) F14 0.063(2) 0.063(2) 0.077(2) -0.0361(19) -0.0199(18) 0.0195(19) O11 0.0170(12) 0.0262(15) 0.0253(14) -0.0128(12) -0.0087(11) 0.0079(12) O12 0.0188(13) 0.0256(15) 0.0232(13) -0.0111(12) -0.0029(11) 0.0022(12) N11 0.0262(17) 0.0223(18) 0.0263(16) -0.0124(14) -0.0140(14) 0.0067(15) C11 0.020(2) 0.053(3) 0.046(3) -0.023(2) -0.0017(19) 0.006(2) C12 0.0184(18) 0.028(2) 0.029(2) -0.0179(18) -0.0046(16) 0.0035(17) C13 0.046(3) 0.030(2) 0.038(2) -0.021(2) -0.024(2) 0.009(2) C111 0.0229(19) 0.021(2) 0.0219(18) -0.0098(16) -0.0072(15) 0.0035(17) C112 0.041(3) 0.026(3) 0.046(3) -0.021(2) 0.011(2) -0.003(2) C113 0.051(3) 0.025(3) 0.057(3) -0.023(2) 0.011(3) -0.005(3) C114 0.034(2) 0.028(2) 0.034(2) -0.010(2) -0.0028(19) -0.007(2) C115 0.026(2) 0.032(3) 0.031(2) -0.012(2) -0.0011(18) 0.001(2) C116 0.026(2) 0.023(2) 0.028(2) -0.0117(18) -0.0043(17) 0.0045(18) C121 0.0209(18) 0.021(2) 0.0254(19) -0.0132(16) -0.0069(15) 0.0065(17) C122 0.029(2) 0.024(2) 0.0249(19) -0.0094(17) -0.0033(17) 0.0057(18) C123 0.031(2) 0.032(3) 0.029(2) -0.0143(19) 0.0027(18) 0.000(2) C124 0.023(2) 0.044(3) 0.046(3) -0.030(2) -0.0063(19) 0.011(2) C125 0.032(2) 0.047(3) 0.043(3) -0.027(2) -0.020(2) 0.020(2) C126 0.030(2) 0.036(2) 0.0242(19) -0.0159(18) -0.0116(17) 0.012(2) C131 0.0174(18) 0.027(2) 0.0195(17) -0.0100(16) -0.0075(15) 0.0045(17) C132 0.027(2) 0.033(3) 0.026(2) -0.0060(19) -0.0089(17) 0.003(2) C133 0.023(2) 0.051(3) 0.035(2) -0.006(2) -0.0041(18) -0.006(2) C134 0.021(2) 0.064(4) 0.041(2) -0.025(3) -0.0116(19) 0.013(2) C135 0.028(2) 0.042(3) 0.037(2) -0.019(2) -0.0185(19) 0.017(2) C136 0.028(2) 0.029(2) 0.027(2) -0.0094(18) -0.0131(17) 0.0080(19) C141 0.027(2) 0.026(2) 0.0195(18) -0.0087(16) -0.0053(16) 0.0029(18) C142 0.032(2) 0.055(3) 0.025(2) -0.017(2) -0.0080(18) 0.000(2) C143 0.050(3) 0.061(4) 0.024(2) -0.018(2) -0.012(2) 0.000(3) C144 0.056(3) 0.043(3) 0.020(2) -0.011(2) 0.002(2) -0.006(3) C145 0.037(2) 0.044(3) 0.030(2) -0.012(2) 0.0060(19) -0.011(2) C146 0.031(2) 0.040(3) 0.028(2) -0.015(2) -0.0063(18) -0.001(2) B11 0.027(2) 0.043(3) 0.025(2) -0.008(2) -0.0111(19) 0.009(2) Mo21 0.0185(2) 0.0286(2) 0.0144(2) -0.0090(1) -0.0078(1) 0.0106(1) P21 0.0252(5) 0.0357(6) 0.0177(5) -0.0110(4) -0.0095(4) 0.0160(5) P22 0.0178(5) 0.0317(6) 0.0151(4) -0.0058(4) -0.0067(4) 0.0091(4) O21 0.0234(14) 0.0337(17) 0.0225(13) -0.0116(12) -0.0102(11) 0.0111(13) O22 0.0206(13) 0.0348(17) 0.0176(12) -0.0097(12) -0.0069(11) 0.0088(13) N23 0.0297(18) 0.046(2) 0.0256(17) -0.0190(17) -0.0157(15) 0.0242(18) C21 0.035(2) 0.044(3) 0.030(2) -0.013(2) 0.0000(19) -0.005(2) C22 0.0208(19) 0.035(2) 0.0227(19) -0.0106(18) -0.0096(16) 0.0125(18) C23 0.035(2) 0.064(3) 0.037(2) -0.027(2) -0.023(2) 0.034(2) C211 0.027(2) 0.043(3) 0.0217(19) -0.0158(19) -0.0101(17) 0.017(2) C212 0.042(3) 0.044(3) 0.042(3) -0.022(2) -0.008(2) 0.016(2) C213 0.053(3) 0.056(4) 0.056(3) -0.037(3) -0.010(3) 0.027(3) C214 0.040(3) 0.072(4) 0.039(3) -0.030(3) -0.003(2) 0.020(3) C215 0.042(3) 0.061(4) 0.028(2) -0.016(2) -0.001(2) 0.010(3) C216 0.038(2) 0.045(3) 0.024(2) -0.013(2) -0.0080(19) 0.016(2) C221 0.031(2) 0.039(3) 0.027(2) -0.0125(19) -0.0083(18) 0.017(2) C222 0.043(3) 0.042(3) 0.029(2) -0.009(2) -0.003(2) 0.010(2) C223 0.050(3) 0.052(4) 0.039(3) -0.005(3) 0.001(2) 0.009(3) C224 0.041(3) 0.045(3) 0.062(4) -0.008(3) 0.005(3) 0.002(3) C225 0.045(3) 0.057(4) 0.069(4) -0.030(3) -0.015(3) 0.006(3) C226 0.042(3) 0.038(3) 0.037(2) -0.007(2) -0.010(2) 0.002(2) C231 0.0179(19) 0.044(3) 0.025(2) 0.0015(19) -0.0088(16) 0.007(2) C232 0.033(2) 0.072(4) 0.025(2) -0.005(2) -0.0076(19) 0.004(3) C233 0.023(2) 0.081(4) 0.033(2) 0.000(3) -0.002(2) -0.001(3) C234 0.034(3) 0.047(4) 0.064(4) -0.002(3) -0.012(3) -0.010(3) C235 0.042(3) 0.053(4) 0.066(4) -0.022(3) -0.014(3) -0.006(3) C236 0.031(2) 0.043(3) 0.046(3) -0.016(2) -0.009(2) 0.001(2) C241 0.0215(18) 0.023(2) 0.0162(17) -0.0061(15) -0.0060(14) 0.0052(17) C242 0.024(2) 0.032(2) 0.0246(19) -0.0110(18) -0.0111(16) 0.0081(18) C243 0.034(2) 0.041(3) 0.023(2) -0.0120(19) -0.0171(18) 0.009(2) C244 0.042(2) 0.040(3) 0.0161(18) -0.0060(18) -0.0113(18) 0.007(2) C245 0.026(2) 0.043(3) 0.0199(19) -0.0068(19) -0.0018(16) 0.003(2) C246 0.0219(19) 0.032(2) 0.0216(19) -0.0065(17) -0.0083(16) 0.0047(18) Cl1 0.0950(13) 0.0730(12) 0.0776(11) -0.0234(10) -0.0411(10) 0.0023(11) Cl2 0.0620(11) 0.1068(17) 0.0782(12) -0.0054(11) -0.0109(9) -0.0054(11) C1 0.064(4) 0.071(5) 0.077(4) -0.033(4) -0.019(3) 0.000(4) Cl3 0.155(2) 0.0914(15) 0.0763(12) -0.0507(12) -0.0036(14) -0.0401(16) Cl4 0.169(3) 0.146(2) 0.0896(15) -0.0802(16) -0.0574(16) 0.070(2) C2 0.127(7) 0.060(4) 0.060(4) -0.016(3) -0.047(4) 0.008(5) F21 0.0568(19) 0.0455(18) 0.0527(17) -0.0257(15) -0.0016(15) 0.0147(16) F22 0.094(3) 0.061(3) 0.176(5) -0.047(3) -0.077(3) 0.014(3) F23 0.098(3) 0.093(3) 0.061(2) -0.029(2) 0.007(2) 0.042(3) F24 0.303(8) 0.133(4) 0.116(4) -0.095(4) -0.167(5) 0.144(5) B21 0.031(3) 0.036(3) 0.040(3) -0.021(2) -0.002(2) 0.002(2) #=================================================================== # 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 Mo11 P11 2.5761(11) . . yes Mo11 F11 2.505(5) . . yes Mo11 O11 2.083(3) . . yes Mo11 Mo11 2.1152(5) . 2_566 yes Mo11 P12 2.5860(12) . 2_566 yes Mo11 O12 2.110(3) . 2_566 yes Mo21 Mo21 2.1109(6) . 2_675 yes Mo21 P21 2.5781(13) . . yes Mo21 O21 2.081(3) . . yes Mo21 P22 2.5943(11) . 2_675 yes Mo21 O22 2.112(3) . 2_675 yes Cl1 C1 1.745(7) . . yes Cl2 C1 1.749(7) . . yes Cl3 C2 1.799(10) . . yes Cl4 C2 1.748(7) . . yes P11 C111 1.805(4) . . yes P11 N11 1.695(3) . . yes P11 C121 1.819(4) . . yes P12 C131 1.817(4) . . yes P12 N11 1.686(4) . . yes P12 C141 1.817(3) . . yes P21 N23 1.700(4) . . yes P21 C211 1.824(4) . . yes P21 C221 1.813(6) . . yes P22 C241 1.819(3) . . yes P22 C231 1.840(5) . . yes P22 N23 1.690(4) . . yes F11 B11 1.382(7) . . yes F12 B11 1.380(6) . . yes F13 B11 1.363(7) . . yes F14 B11 1.361(7) . . yes F21 B21 1.371(7) . . yes F22 B21 1.366(8) . . yes F23 B21 1.381(6) . . yes F24 B21 1.286(8) . . yes O11 C12 1.264(4) . . yes O12 C12 1.279(5) . . yes O21 C22 1.269(4) . . yes O22 C22 1.267(5) . . yes N11 C13 1.484(6) . . yes N23 C23 1.489(6) . . yes C11 C12 1.493(6) . . no C11 H11B 0.9798 . . no C11 H11C 0.9801 . . no C11 H11A 0.9798 . . no C111 C112 1.397(7) . . no C111 C116 1.393(5) . . no C112 C113 1.371(8) . . no C13 H13C 0.9795 . . no C113 C114 1.375(7) . . no C13 H13A 0.9794 . . no C13 H13B 0.9806 . . no C114 C115 1.372(7) . . no C115 C116 1.372(6) . . no C121 C122 1.389(5) . . no C121 C126 1.390(6) . . no C122 C123 1.389(6) . . no C123 C124 1.385(7) . . no C124 C125 1.369(7) . . no C125 C126 1.393(6) . . no C131 C132 1.380(6) . . no C131 C136 1.398(6) . . no C132 C133 1.387(6) . . no C133 C134 1.387(8) . . no C134 C135 1.365(7) . . no C135 C136 1.396(6) . . no C141 C146 1.387(6) . . no C141 C142 1.394(6) . . no C142 C143 1.390(7) . . no C143 C144 1.377(8) . . no C144 C145 1.371(8) . . no C145 C146 1.392(7) . . no C112 H112 0.9505 . . no C113 H113 0.9504 . . no C114 H114 0.9492 . . no C115 H115 0.9500 . . no C116 H116 0.9498 . . no C21 C22 1.482(7) . . no C122 H122 0.9506 . . no C123 H123 0.9502 . . no C124 H124 0.9506 . . no C125 H125 0.9492 . . no C126 H126 0.9497 . . no C132 H132 0.9497 . . no C133 H133 0.9498 . . no C134 H134 0.9503 . . no C135 H135 0.9510 . . no C136 H136 0.9497 . . no C142 H142 0.9506 . . no C143 H143 0.9502 . . no C144 H144 0.9509 . . no C145 H145 0.9497 . . no C146 H146 0.9504 . . no C21 H21C 0.9805 . . no C21 H21B 0.9788 . . no C21 H21A 0.9803 . . no C23 H23C 0.9799 . . no C23 H23A 0.9789 . . no C23 H23B 0.9800 . . no C211 C216 1.395(7) . . no C211 C212 1.391(8) . . no C212 C213 1.397(8) . . no C213 C214 1.363(9) . . no C214 C215 1.385(10) . . no C215 C216 1.383(7) . . no C221 C222 1.392(7) . . no C221 C226 1.390(8) . . no C222 C223 1.378(8) . . no C223 C224 1.366(9) . . no C224 C225 1.395(9) . . no C225 C226 1.380(9) . . no C231 C232 1.388(7) . . no C231 C236 1.385(8) . . no C232 C233 1.414(9) . . no C233 C234 1.372(9) . . no C234 C235 1.387(9) . . no C235 C236 1.392(8) . . no C241 C242 1.394(6) . . no C241 C246 1.390(6) . . no C242 C243 1.381(6) . . no C243 C244 1.378(6) . . no C244 C245 1.389(6) . . no C245 C246 1.387(5) . . no C1 H1B 0.9907 . . no C1 H1A 0.9904 . . no C212 H212 0.9514 . . no C213 H213 0.9488 . . no C214 H214 0.9500 . . no C215 H215 0.9512 . . no C216 H216 0.9503 . . no C222 H222 0.9495 . . no C223 H223 0.9507 . . no C224 H224 0.9494 . . no C225 H225 0.9498 . . no C226 H226 0.9507 . . no C232 H232 0.9486 . . no C233 H233 0.9499 . . no C234 H234 0.9496 . . no C235 H235 0.9500 . . no C236 H236 0.9494 . . no C242 H242 0.9506 . . no C243 H243 0.9506 . . no C244 H244 0.9488 . . no C245 H245 0.9500 . . no C246 H246 0.9499 . . no C2 H2A 0.9897 . . no C2 H2B 0.9911 . . 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 P11 Mo11 F11 82.58(11) . . . yes P11 Mo11 O11 84.16(8) . . . yes Mo11 Mo11 P11 96.67(3) 2_566 . . yes P11 Mo11 P12 160.13(4) . . 2_566 yes P11 Mo11 O12 96.17(8) . . 2_566 yes F11 Mo11 O11 89.61(17) . . . yes Mo11 Mo11 F11 177.79(15) 2_566 . . yes P12 Mo11 F11 81.37(12) 2_566 . . yes F11 Mo11 O12 87.51(17) . . 2_566 yes Mo11 Mo11 O11 92.38(8) 2_566 . . yes P12 Mo11 O11 84.09(8) 2_566 . . yes O11 Mo11 O12 177.04(10) . . 2_566 yes Mo11 Mo11 P12 99.78(3) 2_566 . 2_566 yes Mo11 Mo11 O12 90.51(8) 2_566 . 2_566 yes P12 Mo11 O12 94.76(8) 2_566 . 2_566 yes P22 Mo21 O21 84.48(8) 2_675 . . yes O21 Mo21 O22 177.31(11) . . 2_675 yes P21 Mo21 O21 84.96(8) . . . yes Mo21 Mo21 P21 97.18(3) 2_675 . . yes P21 Mo21 P22 160.28(4) . . 2_675 yes P21 Mo21 O22 94.82(8) . . 2_675 yes Mo21 Mo21 O21 92.31(8) 2_675 . . yes Mo21 Mo21 O22 90.39(8) 2_675 . 2_675 yes P22 Mo21 O22 94.94(8) 2_675 . 2_675 yes Mo21 Mo21 P22 99.84(3) 2_675 . 2_675 yes Mo11 P11 N11 112.73(16) . . . yes Mo11 P11 C111 116.37(13) . . . yes N11 P11 C121 104.55(16) . . . yes C111 P11 C121 106.07(19) . . . yes Mo11 P11 C121 111.23(14) . . . yes N11 P11 C111 104.95(18) . . . yes Mo11 P12 N11 110.71(12) 2_566 . . yes N11 P12 C131 103.89(17) . . . yes N11 P12 C141 105.58(19) . . . yes Mo11 P12 C141 120.13(15) 2_566 . . yes C131 P12 C141 104.90(17) . . . yes Mo11 P12 C131 110.30(14) 2_566 . . yes Mo21 P21 C211 119.54(14) . . . yes N23 P21 C221 105.5(2) . . . yes Mo21 P21 C221 110.08(15) . . . yes N23 P21 C211 102.5(2) . . . yes Mo21 P21 N23 112.53(16) . . . yes C211 P21 C221 105.6(2) . . . yes N23 P22 C241 106.27(19) . . . yes Mo21 P22 N23 110.50(14) 2_675 . . yes Mo21 P22 C231 113.55(17) 2_675 . . yes Mo21 P22 C241 117.49(14) 2_675 . . yes C231 P22 C241 103.3(2) . . . yes N23 P22 C231 104.7(2) . . . yes Mo11 F11 B11 172.5(5) . . . yes Mo11 O11 C12 117.7(3) . . . yes Mo11 O12 C12 117.7(2) 2_566 . . yes Mo21 O21 C22 117.9(3) . . . yes Mo21 O22 C22 118.2(2) 2_675 . . yes P11 N11 C13 120.4(3) . . . yes P11 N11 P12 117.9(2) . . . yes P12 N11 C13 121.6(3) . . . yes P21 N23 C23 120.6(3) . . . yes P22 N23 C23 121.1(3) . . . yes P21 N23 P22 118.3(2) . . . yes O12 C12 C11 118.9(3) . . . yes O11 C12 O12 121.7(4) . . . yes O11 C12 C11 119.4(4) . . . yes C12 C11 H11A 109.47 . . . no C12 C11 H11B 109.53 . . . no C12 C11 H11C 109.45 . . . no H11B C11 H11C 109.42 . . . no P11 C111 C112 122.8(3) . . . yes P11 C111 C116 119.0(3) . . . yes C112 C111 C116 118.2(4) . . . no H11A C11 H11B 109.46 . . . no H11A C11 H11C 109.49 . . . no C111 C112 C113 120.3(5) . . . no N11 C13 H13C 109.41 . . . no N11 C13 H13A 109.41 . . . no N11 C13 H13B 109.41 . . . no H13B C13 H13C 109.47 . . . no H13A C13 H13B 109.51 . . . no C112 C113 C114 120.9(5) . . . no H13A C13 H13C 109.61 . . . no C113 C114 C115 119.2(5) . . . no C114 C115 C116 120.9(4) . . . no C111 C116 C115 120.5(4) . . . no P11 C121 C126 119.6(3) . . . yes C122 C121 C126 119.5(4) . . . no P11 C121 C122 120.7(3) . . . yes C121 C122 C123 120.3(4) . . . no C122 C123 C124 120.0(4) . . . no C123 C124 C125 119.8(4) . . . no C124 C125 C126 121.0(4) . . . no C121 C126 C125 119.5(4) . . . no P12 C131 C132 120.2(3) . . . yes C132 C131 C136 120.0(4) . . . no P12 C131 C136 119.5(3) . . . yes C131 C132 C133 120.2(5) . . . no C132 C133 C134 119.7(5) . . . no C133 C134 C135 120.4(4) . . . no C134 C135 C136 120.5(5) . . . no C131 C136 C135 119.1(4) . . . no P12 C141 C142 121.8(3) . . . yes P12 C141 C146 118.6(3) . . . yes C142 C141 C146 119.4(4) . . . no C141 C142 C143 119.9(4) . . . no C142 C143 C144 120.2(5) . . . no C143 C144 C145 120.3(5) . . . no C144 C145 C146 120.3(5) . . . no C141 C146 C145 119.9(4) . . . no C113 C112 H112 119.87 . . . no C111 C112 H112 119.81 . . . no C114 C113 H113 119.50 . . . no C112 C113 H113 119.61 . . . no C113 C114 H114 120.32 . . . no C115 C114 H114 120.43 . . . no C114 C115 H115 119.52 . . . no C116 C115 H115 119.59 . . . no C111 C116 H116 119.72 . . . no C115 C116 H116 119.81 . . . no O22 C22 C21 119.8(3) . . . yes O21 C22 O22 121.1(3) . . . yes O21 C22 C21 119.1(4) . . . yes C121 C122 H122 119.92 . . . no C123 C122 H122 119.82 . . . no C122 C123 H123 120.00 . . . no C124 C123 H123 120.02 . . . no C123 C124 H124 120.18 . . . no C125 C124 H124 120.00 . . . no C126 C125 H125 119.44 . . . no C124 C125 H125 119.60 . . . no C121 C126 H126 120.25 . . . no C125 C126 H126 120.28 . . . no C133 C132 H132 119.79 . . . no C131 C132 H132 119.98 . . . no C132 C133 H133 120.12 . . . no C134 C133 H133 120.15 . . . no C135 C134 H134 119.78 . . . no C133 C134 H134 119.78 . . . no C134 C135 H135 119.70 . . . no C136 C135 H135 119.76 . . . no C131 C136 H136 120.48 . . . no C135 C136 H136 120.44 . . . no C143 C142 H142 120.02 . . . no C141 C142 H142 120.12 . . . no C142 C143 H143 119.98 . . . no C144 C143 H143 119.85 . . . no C143 C144 H144 119.85 . . . no C145 C144 H144 119.86 . . . no C146 C145 H145 119.80 . . . no C144 C145 H145 119.89 . . . no C145 C146 H146 120.04 . . . no C141 C146 H146 120.02 . . . no C22 C21 H21A 109.43 . . . no C22 C21 H21B 109.50 . . . no H21B C21 H21C 109.57 . . . no H21A C21 H21C 109.39 . . . no C22 C21 H21C 109.45 . . . no H21A C21 H21B 109.49 . . . no H23A C23 H23C 109.60 . . . no H23A C23 H23B 109.41 . . . no N23 C23 H23C 109.50 . . . no N23 C23 H23A 109.43 . . . no H23B C23 H23C 109.48 . . . no N23 C23 H23B 109.40 . . . no Cl1 C1 Cl2 113.7(5) . . . yes C212 C211 C216 119.7(4) . . . no P21 C211 C212 122.4(3) . . . yes P21 C211 C216 117.6(4) . . . yes C211 C212 C213 119.0(5) . . . no C212 C213 C214 121.0(6) . . . no C213 C214 C215 120.3(5) . . . no C214 C215 C216 119.7(5) . . . no C211 C216 C215 120.2(5) . . . no C222 C221 C226 118.7(5) . . . no P21 C221 C226 120.3(4) . . . yes P21 C221 C222 120.8(4) . . . yes C221 C222 C223 120.7(5) . . . no C222 C223 C224 120.6(5) . . . no C223 C224 C225 119.5(6) . . . no C224 C225 C226 120.3(6) . . . no C221 C226 C225 120.2(5) . . . no P22 C231 C236 120.9(4) . . . yes P22 C231 C232 119.1(4) . . . yes C232 C231 C236 120.0(5) . . . no C231 C232 C233 119.5(6) . . . no C232 C233 C234 119.7(5) . . . no C233 C234 C235 120.7(6) . . . no C234 C235 C236 119.6(6) . . . no C231 C236 C235 120.4(5) . . . no P22 C241 C242 121.8(3) . . . yes C242 C241 C246 119.2(3) . . . no P22 C241 C246 118.9(3) . . . yes C241 C242 C243 120.1(4) . . . no C242 C243 C244 120.5(4) . . . no C243 C244 C245 119.9(3) . . . no C244 C245 C246 119.8(4) . . . no C241 C246 C245 120.4(4) . . . no Cl2 C1 H1A 108.87 . . . no Cl1 C1 H1B 108.82 . . . no Cl2 C1 H1B 108.83 . . . no H1A C1 H1B 107.62 . . . no Cl1 C1 H1A 108.79 . . . no C211 C212 H212 120.50 . . . no C213 C212 H212 120.50 . . . no C214 C213 H213 119.55 . . . no C212 C213 H213 119.49 . . . no C213 C214 H214 119.84 . . . no C215 C214 H214 119.85 . . . no C216 C215 H215 120.11 . . . no C214 C215 H215 120.15 . . . no C215 C216 H216 119.86 . . . no C211 C216 H216 119.92 . . . no C221 C222 H222 119.66 . . . no C223 C222 H222 119.66 . . . no C224 C223 H223 119.71 . . . no C222 C223 H223 119.70 . . . no C225 C224 H224 120.32 . . . no C223 C224 H224 120.23 . . . no C224 C225 H225 119.85 . . . no C226 C225 H225 119.86 . . . no C221 C226 H226 119.85 . . . no C225 C226 H226 119.90 . . . no C231 C232 H232 120.26 . . . no C233 C232 H232 120.28 . . . no C232 C233 H233 120.10 . . . no C234 C233 H233 120.19 . . . no C233 C234 H234 119.64 . . . no C235 C234 H234 119.65 . . . no C236 C235 H235 120.17 . . . no C234 C235 H235 120.23 . . . no C235 C236 H236 119.84 . . . no C231 C236 H236 119.79 . . . no C241 C242 H242 119.94 . . . no C243 C242 H242 119.92 . . . no C244 C243 H243 119.69 . . . no C242 C243 H243 119.78 . . . no C243 C244 H244 120.04 . . . no C245 C244 H244 120.06 . . . no C244 C245 H245 120.05 . . . no C246 C245 H245 120.14 . . . no C245 C246 H246 119.77 . . . no C241 C246 H246 119.82 . . . no Cl3 C2 Cl4 109.6(5) . . . yes Cl3 C2 H2B 109.69 . . . no Cl4 C2 H2A 109.82 . . . no Cl4 C2 H2B 109.84 . . . no H2A C2 H2B 108.11 . . . no Cl3 C2 H2A 109.79 . . . no F12 B11 F14 111.9(5) . . . yes F13 B11 F14 108.0(5) . . . yes F11 B11 F12 107.6(5) . . . yes F11 B11 F13 111.4(5) . . . yes F11 B11 F14 107.3(4) . . . yes F12 B11 F13 110.6(4) . . . yes F21 B21 F22 110.9(5) . . . yes F21 B21 F23 108.0(4) . . . yes F21 B21 F24 111.4(5) . . . yes F22 B21 F23 97.6(5) . . . yes F22 B21 F24 113.6(6) . . . yes F23 B21 F24 114.6(5) . . . yes # End of Crystallographic Information File # =================================================================== data_WANE-4025-143 # =================================================================== _chemical_name_systematic ; not known ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C54 H52 B2 F8 Mo2 N2 O4 P4), C4 H10 O, C6 H14' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C118 H128 B4 F16 Mo4 N4 O9 P8' _chemical_formula_weight 2725.01 _chemical_compound_source 'see text' 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' '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' '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' 'P' 'P' 0.1023 0.0942 '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' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.8037(3) _cell_length_b 19.1309(3) _cell_length_c 22.2622(4) _cell_angle_alpha 77.758(1) _cell_angle_beta 69.838(1) _cell_angle_gamma 77.453(1) _cell_volume 6097.90(19) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _cell_measurement_reflns_used 87573 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 26.43 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8161 _exptl_absorpt_correction_T_max 0.9117 _exptl_absorpt_process_details ; Otwinowski, Z.; and Minor, W. "Processing of X-ray Diffraction Data Collected in Oscillation Mode", Metthods in Enzymology 276, 1996. Carter W. C.; Sweet, Jr. & R. M.; Eds., Academic Press, (USA). ; _exptl_special_details ; Diffractometer operator Herdtweck, E. ; _publ_section_exptl_prep ; the crystals were handled in air, fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward. ; # =================================================================== # 7. EXPERIMENTAL DATA # =================================================================== _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kappa CCD (Nonius)' _diffrn_measurement_method ' rotation ' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 45149 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.43 _reflns_number_total 24833 _reflns_number_gt 20239 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Nonius- CCD-Software. ; _computing_data_collection 'Kappa CCD (Nonius)' _computing_cell_refinement 'Denzo and HKL' _computing_data_reduction 'Denzo and HKL' _computing_structure_solution 'SIR-92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON PLUTON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' # =================================================================== # 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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+8.3017P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_number_reflns 24833 _refine_ls_number_parameters 1477 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.943 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.075 # =================================================================== # 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 Mo11 Mo Uani 0.23319(2) 0.20851(1) 0.75800(1) 1.000 0.0157(1) Mo12 Mo Uani 0.21124(2) 0.31118(1) 0.70253(1) 1.000 0.0159(1) P11 P Uani 0.39685(5) 0.21662(4) 0.75216(4) 1.000 0.0186(2) P12 P Uani 0.35364(5) 0.36546(4) 0.69284(4) 1.000 0.0188(2) P13 P Uani 0.05048(5) 0.30376(4) 0.70544(4) 1.000 0.0188(2) P14 P Uani 0.09324(5) 0.15491(4) 0.76169(4) 1.000 0.0182(2) O11 O Uani 0.29743(13) 0.15811(10) 0.67601(10) 1.000 0.0202(6) O12 O Uani 0.27344(13) 0.26540(10) 0.61651(10) 1.000 0.0211(6) O13 O Uani 0.14989(13) 0.36161(10) 0.78497(10) 1.000 0.0201(6) O14 O Uani 0.16928(13) 0.25384(10) 0.84446(10) 1.000 0.0202(6) N11 N Uani 0.41910(16) 0.30277(13) 0.73129(13) 1.000 0.0222(8) N12 N Uani 0.02783(16) 0.21787(13) 0.72288(12) 1.000 0.0207(8) C11 C Uani 0.3598(2) 0.16594(18) 0.56141(16) 1.000 0.0327(11) C12 C Uani 0.3072(2) 0.19784(16) 0.62103(15) 1.000 0.0227(9) C13 C Uani 0.5025(2) 0.31887(18) 0.73818(19) 1.000 0.0342(11) C14 C Uani 0.0950(2) 0.35593(18) 0.89993(16) 1.000 0.0327(11) C15 C Uani 0.14059(19) 0.32180(16) 0.83991(15) 1.000 0.0210(9) C16 C Uani -0.0561(2) 0.20195(18) 0.71611(17) 1.000 0.0298(10) C111 C Uani 0.4263(2) 0.18773(16) 0.82661(15) 1.000 0.0222(9) C112 C Uani 0.5097(2) 0.14699(16) 0.82920(17) 1.000 0.0270(10) C113 C Uani 0.5306(3) 0.13346(19) 0.88643(19) 1.000 0.0370(11) C114 C Uani 0.4702(3) 0.16107(19) 0.94077(18) 1.000 0.0377(12) C115 C Uani 0.3877(2) 0.20336(19) 0.93814(17) 1.000 0.0339(11) C116 C Uani 0.3650(2) 0.21530(17) 0.88157(16) 1.000 0.0272(10) C121 C Uani 0.48344(19) 0.16703(16) 0.69121(15) 1.000 0.0231(9) C122 C Uani 0.5304(2) 0.20491(18) 0.63273(16) 1.000 0.0293(10) C123 C Uani 0.5912(2) 0.16781(19) 0.58295(17) 1.000 0.0347(11) C124 C Uani 0.6056(2) 0.0933(2) 0.59220(18) 1.000 0.0360(11) C125 C Uani 0.5603(2) 0.05518(18) 0.65043(18) 1.000 0.0337(11) C126 C Uani 0.4986(2) 0.09129(17) 0.69962(17) 1.000 0.0280(10) C131 C Uani 0.3296(2) 0.44117(16) 0.73680(16) 1.000 0.0248(9) C132 C Uani 0.3145(2) 0.42818(18) 0.80319(17) 1.000 0.0316(11) C133 C Uani 0.2938(3) 0.4845(2) 0.8382(2) 1.000 0.0430(12) C134 C Uani 0.2880(3) 0.5550(2) 0.8073(2) 1.000 0.0491(14) C135 C Uani 0.3019(3) 0.5690(2) 0.7420(2) 1.000 0.0512(15) C136 C Uani 0.3220(2) 0.51258(18) 0.70586(18) 1.000 0.0355(11) C141 C Uani 0.4302(2) 0.39279(15) 0.61233(15) 1.000 0.0220(9) C142 C Uani 0.5043(2) 0.42793(17) 0.60326(17) 1.000 0.0291(10) C143 C Uani 0.5704(2) 0.43557(19) 0.54326(18) 1.000 0.0360(11) C144 C Uani 0.5642(2) 0.40985(19) 0.49200(18) 1.000 0.0380(11) C145 C Uani 0.4893(2) 0.37844(19) 0.49946(17) 1.000 0.0358(11) C146 C Uani 0.4226(2) 0.37039(17) 0.55930(16) 1.000 0.0281(10) C151 C Uani 0.0274(2) 0.33813(16) 0.62906(15) 1.000 0.0228(9) C152 C Uani -0.0372(2) 0.39855(17) 0.62008(16) 1.000 0.0285(10) C153 C Uani -0.0486(2) 0.42233(19) 0.55918(18) 1.000 0.0360(11) C154 C Uani 0.0023(2) 0.3857(2) 0.50814(18) 1.000 0.0381(12) C155 C Uani 0.0665(2) 0.32587(19) 0.51639(16) 1.000 0.0328(11) C156 C Uani 0.0799(2) 0.30305(18) 0.57640(16) 1.000 0.0283(10) C161 C Uani -0.0370(2) 0.35214(17) 0.76663(15) 1.000 0.0238(9) C162 C Uani -0.0919(2) 0.31432(18) 0.82132(16) 1.000 0.0277(10) C163 C Uani -0.1547(2) 0.3505(2) 0.87041(17) 1.000 0.0352(11) C164 C Uani -0.1633(2) 0.4246(2) 0.86517(18) 1.000 0.0364(11) C165 C Uani -0.1088(2) 0.46303(19) 0.81119(18) 1.000 0.0332(11) C166 C Uani -0.0452(2) 0.42750(17) 0.76252(17) 1.000 0.0285(10) C171 C Uani 0.12610(19) 0.07923(16) 0.71692(15) 1.000 0.0224(9) C172 C Uani 0.1280(2) 0.08933(19) 0.65267(16) 1.000 0.0317(11) C173 C Uani 0.1520(2) 0.0302(2) 0.61965(17) 1.000 0.0392(11) C174 C Uani 0.1752(2) -0.0385(2) 0.6504(2) 1.000 0.0401(14) C175 C Uani 0.1767(2) -0.04876(19) 0.71336(19) 1.000 0.0364(11) C176 C Uani 0.1520(2) 0.00973(17) 0.74701(17) 1.000 0.0289(10) C181 C Uani 0.01687(19) 0.11801(15) 0.83859(14) 1.000 0.0201(9) C182 C Uani -0.0385(2) 0.06839(17) 0.84177(16) 1.000 0.0279(10) C183 C Uani -0.0932(2) 0.03881(18) 0.90052(17) 1.000 0.0325(11) C184 C Uani -0.0943(2) 0.05734(18) 0.95743(17) 1.000 0.0330(11) C185 C Uani -0.0396(2) 0.10669(18) 0.95490(16) 1.000 0.0323(11) C186 C Uani 0.0151(2) 0.13676(17) 0.89621(15) 1.000 0.0260(10) Mo21 Mo Uani 0.28880(2) 0.19254(1) 0.27946(1) 1.000 0.0150(1) Mo22 Mo Uani 0.29457(1) 0.25458(1) 0.18772(1) 1.000 0.0146(1) P21 P Uani 0.42268(5) 0.23667(4) 0.29307(4) 1.000 0.0178(2) P22 P Uani 0.45238(5) 0.29460(4) 0.15777(4) 1.000 0.0180(2) P23 P Uani 0.14202(5) 0.23122(4) 0.18363(4) 1.000 0.0166(2) P24 P Uani 0.15266(5) 0.12759(4) 0.29798(4) 1.000 0.0173(2) O21 O Uani 0.20639(13) 0.27864(10) 0.32718(9) 1.000 0.0185(6) O22 O Uani 0.22033(13) 0.34655(10) 0.23097(10) 1.000 0.0192(6) O23 O Uani 0.37186(13) 0.16687(10) 0.14045(10) 1.000 0.0193(6) O24 O Uani 0.37362(13) 0.10378(10) 0.23662(10) 1.000 0.0204(6) N21 N Uani 0.49502(16) 0.26710(13) 0.22073(12) 1.000 0.0226(8) N22 N Uani 0.09632(16) 0.16672(13) 0.24409(12) 1.000 0.0210(8) C21 C Uani 0.1425(2) 0.40398(17) 0.32561(16) 1.000 0.0298(10) C22 C Uani 0.19254(18) 0.33979(15) 0.29248(14) 1.000 0.0191(9) C23 C Uani 0.5850(2) 0.2825(2) 0.21672(17) 1.000 0.0343(11) C24 C Uani 0.4516(2) 0.04546(17) 0.14290(17) 1.000 0.0325(11) C25 C Uani 0.39657(19) 0.10897(15) 0.17508(15) 1.000 0.0211(9) C26 C Uani 0.0100(2) 0.14475(19) 0.24824(17) 1.000 0.0317(11) C211 C Uani 0.49501(19) 0.16931(16) 0.33201(15) 1.000 0.0232(9) C212 C Uani 0.5039(2) 0.1742(2) 0.39072(17) 1.000 0.0387(11) C213 C Uani 0.5544(3) 0.1178(2) 0.42085(19) 1.000 0.0500(14) C214 C Uani 0.5970(2) 0.0574(2) 0.39188(19) 1.000 0.0419(11) C215 C Uani 0.5916(2) 0.05256(19) 0.3325(2) 1.000 0.0401(13) C216 C Uani 0.5393(2) 0.10784(17) 0.30315(17) 1.000 0.0299(10) C221 C Uani 0.3839(2) 0.31149(16) 0.33988(15) 1.000 0.0229(9) C222 C Uani 0.4054(2) 0.38060(18) 0.31062(18) 1.000 0.0357(11) C223 C Uani 0.3713(3) 0.4380(2) 0.3457(2) 1.000 0.0461(15) C224 C Uani 0.3164(3) 0.4280(2) 0.4091(2) 1.000 0.0430(14) C225 C Uani 0.2949(2) 0.3593(2) 0.43843(18) 1.000 0.0341(11) C226 C Uani 0.3274(2) 0.30212(17) 0.40349(16) 1.000 0.0274(10) C231 C Uani 0.53700(19) 0.25196(16) 0.09167(15) 1.000 0.0224(9) C232 C Uani 0.5959(2) 0.18919(17) 0.10241(17) 1.000 0.0313(10) C233 C Uani 0.6592(2) 0.1581(2) 0.05000(19) 1.000 0.0396(11) C234 C Uani 0.6631(3) 0.1892(2) -0.01188(18) 1.000 0.0401(12) C235 C Uani 0.6018(3) 0.2506(2) -0.02266(19) 1.000 0.0466(12) C236 C Uani 0.5391(2) 0.28158(19) 0.02874(17) 1.000 0.0345(11) C241 C Uani 0.4621(2) 0.39003(16) 0.13148(15) 1.000 0.0222(9) C242 C Uani 0.5456(2) 0.41268(17) 0.09405(17) 1.000 0.0299(10) C243 C Uani 0.5521(2) 0.48566(19) 0.07810(19) 1.000 0.0386(11) C244 C Uani 0.4769(2) 0.53662(19) 0.0994(2) 1.000 0.0408(13) C245 C Uani 0.3935(2) 0.51472(18) 0.1354(2) 1.000 0.0419(13) C246 C Uani 0.3855(2) 0.44154(17) 0.15124(17) 1.000 0.0304(10) C251 C Uani 0.14199(19) 0.20172(15) 0.11136(14) 1.000 0.0190(8) C252 C Uani 0.0706(2) 0.22429(16) 0.08451(16) 1.000 0.0247(9) C253 C Uani 0.0738(2) 0.19645(18) 0.03121(16) 1.000 0.0303(11) C254 C Uani 0.1466(2) 0.14576(17) 0.00386(16) 1.000 0.0282(10) C255 C Uani 0.2172(2) 0.12263(17) 0.03010(15) 1.000 0.0272(10) C256 C Uani 0.2157(2) 0.15087(16) 0.08300(15) 1.000 0.0240(9) C261 C Uani 0.05639(19) 0.31194(16) 0.19512(15) 1.000 0.0225(9) C262 C Uani -0.0016(2) 0.32093(19) 0.25735(17) 1.000 0.0313(11) C263 C Uani -0.0625(2) 0.3850(2) 0.2678(2) 1.000 0.0416(13) C264 C Uani -0.0655(2) 0.4395(2) 0.2171(2) 1.000 0.0443(14) C265 C Uani -0.0079(2) 0.43131(18) 0.1560(2) 1.000 0.0404(13) C266 C Uani 0.0538(2) 0.36790(16) 0.14416(17) 1.000 0.0286(10) C271 C Uani 0.18748(19) 0.03292(15) 0.28568(15) 1.000 0.0208(9) C272 C Uani 0.1934(2) 0.01195(17) 0.22772(15) 1.000 0.0253(10) C273 C Uani 0.2234(2) -0.05972(18) 0.21830(18) 1.000 0.0329(11) C274 C Uani 0.2481(2) -0.11074(18) 0.26610(19) 1.000 0.0355(13) C275 C Uani 0.2443(2) -0.08993(17) 0.32276(18) 1.000 0.0322(10) C276 C Uani 0.2145(2) -0.01832(16) 0.33275(16) 1.000 0.0263(10) C281 C Uani 0.0669(2) 0.12375(16) 0.37750(14) 1.000 0.0225(9) C282 C Uani 0.0107(2) 0.07065(17) 0.40164(16) 1.000 0.0260(10) C283 C Uani -0.0540(2) 0.06967(19) 0.46203(17) 1.000 0.0366(11) C284 C Uani -0.0617(3) 0.1203(2) 0.5000(2) 1.000 0.0567(16) C285 C Uani -0.0060(3) 0.1729(2) 0.4770(2) 1.000 0.0621(17) C286 C Uani 0.0580(2) 0.17533(19) 0.41599(17) 1.000 0.0396(12) O33 O Uani 0.85769(18) 0.31058(17) 0.07933(14) 0.500 0.0367(10) C31 C Uani 0.9013(3) 0.4259(3) 0.0313(2) 1.000 0.0591(17) C32 C Uani 0.8516(3) 0.3691(3) 0.0297(2) 1.000 0.0576(16) C33 C Uani 0.85769(18) 0.31058(17) 0.07933(14) 0.500 0.0367(10) C34 C Uani 0.8166(3) 0.2544(2) 0.0754(2) 1.000 0.0536(15) C35 C Uani 0.8252(3) 0.1940(3) 0.1312(3) 1.000 0.070(2) C36 C Uani 0.8195(10) 0.2413(13) 0.1917(10) 0.500 0.253(12) O43 O Uani 0.2656(2) 0.69637(17) 0.30844(16) 0.500 0.0423(10) C41 C Uani 0.3082(2) 0.70372(18) 0.19680(16) 1.000 0.0290(10) C42 C Uani 0.2847(3) 0.6538(3) 0.2589(2) 1.000 0.0581(16) C43 C Uani 0.2656(2) 0.69637(17) 0.30844(16) 0.500 0.0423(10) C44 C Uani 0.2585(3) 0.6498(3) 0.3625(3) 1.000 0.082(2) C45 C Uani 0.2260(5) 0.7034(4) 0.4185(3) 1.000 0.099(3) C46 C Uani 0.2277(8) 0.7194(7) 0.4778(11) 0.500 0.179(11) F1 F Uani 0.26087(19) 0.08930(12) 0.82796(13) 1.000 0.0667(10) F2 F Uani 0.20438(17) -0.01070(16) 0.88453(12) 1.000 0.0685(10) F3 F Uani 0.30859(19) 0.02778(13) 0.91184(12) 1.000 0.0611(10) F4 F Uani 0.34923(17) -0.01863(14) 0.82006(12) 1.000 0.0641(9) B1 B Uani 0.2811(3) 0.0212(2) 0.86184(18) 1.000 0.0285(11) F5 F Uani 0.1857(2) 0.43887(14) 0.63848(16) 1.000 0.0840(13) F6 F Uani 0.22682(18) 0.54505(16) 0.58868(16) 1.000 0.0817(13) F7 F Uani 0.08180(14) 0.52909(12) 0.61564(11) 1.000 0.0486(8) F8 F Uani 0.1858(3) 0.4769(2) 0.53641(16) 1.000 0.1198(18) B2 B Uani 0.1706(3) 0.4977(2) 0.5938(2) 1.000 0.0319(12) F9 F Uani 0.29523(15) 0.11696(12) 0.38610(10) 1.000 0.0486(8) F10 F Uani 0.20586(15) 0.04413(12) 0.46308(10) 1.000 0.0453(8) F11 F Uani 0.33783(15) 0.06030(11) 0.47319(10) 1.000 0.0437(8) F12 F Uani 0.21856(15) 0.15255(11) 0.48311(12) 1.000 0.0485(8) B3 B Uani 0.2647(3) 0.0931(2) 0.45226(19) 1.000 0.0341(12) F13 F Uani 0.36700(14) 0.36855(11) -0.02546(11) 1.000 0.0480(8) F14 F Uani 0.22031(16) 0.35495(15) -0.00046(12) 1.000 0.0628(10) F15 F Uani 0.28821(17) 0.32798(13) 0.07682(11) 1.000 0.0577(9) F16 F Uani 0.25496(17) 0.44447(12) 0.03375(13) 1.000 0.0636(9) B4 B Uani 0.2825(3) 0.3747(2) 0.02061(19) 1.000 0.0307(12) H11A H Uiso 0.38010 0.11420 0.57290 1.000 0.0490 H11B H Uiso 0.41300 0.19020 0.53790 1.000 0.0490 H11C H Uiso 0.32100 0.17230 0.53390 1.000 0.0490 H13A H Uiso 0.53060 0.27630 0.76180 1.000 0.0510 H13B H Uiso 0.48630 0.35990 0.76210 1.000 0.0510 H13C H Uiso 0.54560 0.33110 0.69520 1.000 0.0510 H14A H Uiso 0.07720 0.40810 0.88810 1.000 0.0490 H14B H Uiso 0.13730 0.34800 0.92500 1.000 0.0490 H14C H Uiso 0.04050 0.33410 0.92600 1.000 0.0490 H16A H Uiso -0.05810 0.14990 0.72840 1.000 0.0450 H16B H Uiso -0.05560 0.21680 0.67110 1.000 0.0450 H16C H Uiso -0.10990 0.22870 0.74440 1.000 0.0450 H112 H Uiso 0.55210 0.12860 0.79180 1.000 0.0320 H113 H Uiso 0.58700 0.10480 0.88840 1.000 0.0440 H114 H Uiso 0.48510 0.15120 0.97990 1.000 0.0450 H115 H Uiso 0.34710 0.22400 0.97490 1.000 0.0410 H116 H Uiso 0.30750 0.24230 0.88020 1.000 0.0330 H122 H Uiso 0.52100 0.25640 0.62660 1.000 0.0350 H123 H Uiso 0.62250 0.19400 0.54290 1.000 0.0420 H124 H Uiso 0.64690 0.06800 0.55850 1.000 0.0430 H125 H Uiso 0.57150 0.00370 0.65680 1.000 0.0400 H126 H Uiso 0.46660 0.06460 0.73910 1.000 0.0340 H132 H Uiso 0.31850 0.37970 0.82480 1.000 0.0380 H133 H Uiso 0.28360 0.47460 0.88360 1.000 0.0520 H134 H Uiso 0.27440 0.59380 0.83130 1.000 0.0590 H135 H Uiso 0.29780 0.61770 0.72090 1.000 0.0620 H136 H Uiso 0.33050 0.52280 0.66070 1.000 0.0430 H142 H Uiso 0.50900 0.44630 0.63820 1.000 0.0350 H143 H Uiso 0.62050 0.45890 0.53740 1.000 0.0430 H144 H Uiso 0.61120 0.41360 0.45150 1.000 0.0460 H145 H Uiso 0.48370 0.36240 0.46360 1.000 0.0430 H146 H Uiso 0.37100 0.34930 0.56400 1.000 0.0340 H152 H Uiso -0.07340 0.42350 0.65540 1.000 0.0340 H153 H Uiso -0.09180 0.46400 0.55300 1.000 0.0430 H154 H Uiso -0.00670 0.40160 0.46710 1.000 0.0460 H155 H Uiso 0.10140 0.30050 0.48120 1.000 0.0400 H156 H Uiso 0.12550 0.26290 0.58160 1.000 0.0340 H162 H Uiso -0.08640 0.26320 0.82520 1.000 0.0330 H163 H Uiso -0.19170 0.32400 0.90760 1.000 0.0420 H164 H Uiso -0.20650 0.44920 0.89860 1.000 0.0430 H165 H Uiso -0.11520 0.51420 0.80750 1.000 0.0400 H166 H Uiso -0.00690 0.45410 0.72620 1.000 0.0340 H172 H Uiso 0.11280 0.13660 0.63140 1.000 0.0380 H173 H Uiso 0.15240 0.03710 0.57600 1.000 0.0470 H174 H Uiso 0.19030 -0.07890 0.62810 1.000 0.0480 H175 H Uiso 0.19450 -0.09590 0.73370 1.000 0.0440 H176 H Uiso 0.15270 0.00260 0.79040 1.000 0.0350 H182 H Uiso -0.03830 0.05500 0.80300 1.000 0.0340 H183 H Uiso -0.13060 0.00540 0.90190 1.000 0.0390 H184 H Uiso -0.13190 0.03670 0.99790 1.000 0.0400 H185 H Uiso -0.03990 0.11970 0.99390 1.000 0.0390 H186 H Uiso 0.05180 0.17060 0.89510 1.000 0.0310 H21A H Uiso 0.12610 0.38930 0.37260 1.000 0.0450 H21B H Uiso 0.08690 0.42330 0.31350 1.000 0.0450 H21C H Uiso 0.18170 0.44140 0.31240 1.000 0.0450 H23A H Uiso 0.59750 0.26240 0.25770 1.000 0.0510 H23B H Uiso 0.58430 0.33500 0.20840 1.000 0.0510 H23C H Uiso 0.63270 0.26030 0.18140 1.000 0.0510 H24A H Uiso 0.46510 0.00550 0.17560 1.000 0.0490 H24B H Uiso 0.50880 0.05900 0.11170 1.000 0.0490 H24C H Uiso 0.41690 0.03020 0.12030 1.000 0.0490 H26A H Uiso -0.01220 0.17330 0.21300 1.000 0.0470 H26B H Uiso -0.03580 0.15320 0.28990 1.000 0.0470 H26C H Uiso 0.02070 0.09320 0.24460 1.000 0.0470 H212 H Uiso 0.47540 0.21640 0.41050 1.000 0.0470 H213 H Uiso 0.55920 0.12110 0.46150 1.000 0.0600 H214 H Uiso 0.63050 0.01860 0.41290 1.000 0.0510 H215 H Uiso 0.62350 0.01160 0.31170 1.000 0.0480 H216 H Uiso 0.53370 0.10370 0.26300 1.000 0.0360 H222 H Uiso 0.44320 0.38810 0.26690 1.000 0.0420 H223 H Uiso 0.38590 0.48470 0.32580 1.000 0.0550 H224 H Uiso 0.29330 0.46770 0.43280 1.000 0.0510 H225 H Uiso 0.25790 0.35190 0.48240 1.000 0.0410 H226 H Uiso 0.31080 0.25580 0.42320 1.000 0.0330 H232 H Uiso 0.59340 0.16730 0.14540 1.000 0.0380 H233 H Uiso 0.69970 0.11510 0.05740 1.000 0.0480 H234 H Uiso 0.70770 0.16880 -0.04740 1.000 0.0480 H235 H Uiso 0.60320 0.27140 -0.06560 1.000 0.0560 H236 H Uiso 0.49710 0.32350 0.02110 1.000 0.0410 H242 H Uiso 0.59790 0.37780 0.07950 1.000 0.0360 H243 H Uiso 0.60880 0.50070 0.05230 1.000 0.0460 H244 H Uiso 0.48200 0.58660 0.08940 1.000 0.0490 H245 H Uiso 0.34140 0.55000 0.14950 1.000 0.0500 H246 H Uiso 0.32800 0.42690 0.17540 1.000 0.0370 H252 H Uiso 0.01990 0.25870 0.10300 1.000 0.0300 H253 H Uiso 0.02540 0.21230 0.01300 1.000 0.0360 H254 H Uiso 0.14800 0.12700 -0.03280 1.000 0.0340 H255 H Uiso 0.26680 0.08730 0.01190 1.000 0.0330 H256 H Uiso 0.26520 0.13560 0.10020 1.000 0.0290 H262 H Uiso 0.00040 0.28330 0.29260 1.000 0.0380 H263 H Uiso -0.10200 0.39100 0.31020 1.000 0.0500 H264 H Uiso -0.10760 0.48290 0.22430 1.000 0.0530 H265 H Uiso -0.01010 0.46950 0.12120 1.000 0.0480 H266 H Uiso 0.09380 0.36290 0.10170 1.000 0.0340 H272 H Uiso 0.17700 0.04690 0.19470 1.000 0.0300 H273 H Uiso 0.22690 -0.07390 0.17900 1.000 0.0390 H274 H Uiso 0.26770 -0.16000 0.25990 1.000 0.0430 H275 H Uiso 0.26220 -0.12490 0.35520 1.000 0.0390 H276 H Uiso 0.21250 -0.00430 0.37170 1.000 0.0320 H282 H Uiso 0.01700 0.03470 0.37620 1.000 0.0310 H283 H Uiso -0.09320 0.03410 0.47740 1.000 0.0440 H284 H Uiso -0.10530 0.11910 0.54200 1.000 0.0680 H285 H Uiso -0.01160 0.20780 0.50340 1.000 0.0750 H286 H Uiso 0.09570 0.21200 0.40040 1.000 0.0480 H31A H Uiso 0.89710 0.46600 -0.00380 1.000 0.0890 H31B H Uiso 0.96550 0.40550 0.02560 1.000 0.0890 H31C H Uiso 0.87400 0.44390 0.07300 1.000 0.0890 H32A H Uiso 0.78670 0.38970 0.03540 1.000 0.0690 H32B H Uiso 0.87810 0.35180 -0.01280 1.000 0.0690 H33A H Uiso 0.92270 0.29240 0.07560 0.500 0.0440 H33B H Uiso 0.82710 0.32720 0.12190 0.500 0.0440 H34A H Uiso 0.84770 0.23640 0.03340 1.000 0.0650 H34B H Uiso 0.75150 0.27190 0.07910 1.000 0.0650 H35A H Uiso 0.88400 0.16110 0.11880 0.500 0.0840 H35B H Uiso 0.77460 0.16550 0.14520 0.500 0.0840 H35C H Uiso 0.79520 0.15440 0.13090 0.500 0.1050 H35D H Uiso 0.79610 0.21300 0.17230 0.500 0.1050 H35E H Uiso 0.88990 0.17590 0.12610 0.500 0.1050 H36A H Uiso 0.82430 0.20690 0.23030 0.500 0.3820 H36B H Uiso 0.76120 0.27400 0.20250 0.500 0.3820 H36C H Uiso 0.86980 0.26940 0.17640 0.500 0.3820 H41A H Uiso 0.32240 0.67680 0.16080 1.000 0.0440 H41B H Uiso 0.36140 0.72490 0.19270 1.000 0.0440 H41C H Uiso 0.25630 0.74240 0.19600 1.000 0.0440 H42A H Uiso 0.23070 0.63210 0.26400 1.000 0.0700 H42B H Uiso 0.33640 0.61430 0.26050 1.000 0.0700 H43A H Uiso 0.31550 0.72440 0.29950 0.500 0.0510 H43B H Uiso 0.20790 0.73060 0.31170 0.500 0.0510 H44A H Uiso 0.31780 0.61890 0.36160 1.000 0.0990 H44B H Uiso 0.21230 0.61860 0.36990 1.000 0.0990 H45A H Uiso 0.24250 0.74900 0.39020 0.500 0.1190 H45B H Uiso 0.15910 0.70900 0.42810 0.500 0.1190 H45C H Uiso 0.21980 0.67380 0.46110 0.500 0.1490 H45D H Uiso 0.16720 0.73320 0.41850 0.500 0.1490 H45E H Uiso 0.27180 0.73480 0.40920 0.500 0.1490 H46A H Uiso 0.18960 0.76630 0.48630 0.500 0.2680 H46B H Uiso 0.29050 0.72150 0.47450 0.500 0.2680 H46C H Uiso 0.20400 0.68150 0.51320 0.500 0.2680 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 Mo11 0.0144(1) 0.0148(1) 0.0186(1) 0.0011(1) -0.0072(1) -0.0041(1) Mo12 0.0145(1) 0.0152(1) 0.0185(1) 0.0012(1) -0.0072(1) -0.0037(1) P11 0.0162(4) 0.0180(4) 0.0226(4) 0.0014(3) -0.0087(3) -0.0047(3) P12 0.0164(4) 0.0176(4) 0.0223(4) 0.0019(3) -0.0075(3) -0.0051(3) P13 0.0170(4) 0.0199(4) 0.0215(4) 0.0018(3) -0.0098(3) -0.0053(3) P14 0.0179(4) 0.0193(4) 0.0190(4) 0.0019(3) -0.0078(3) -0.0075(3) O11 0.0205(10) 0.0189(10) 0.0225(11) -0.0018(8) -0.0085(9) -0.0042(8) O12 0.0220(11) 0.0219(11) 0.0205(11) -0.0003(8) -0.0083(9) -0.0055(8) O13 0.0178(10) 0.0187(10) 0.0251(12) -0.0019(8) -0.0091(9) -0.0031(8) O14 0.0185(10) 0.0200(11) 0.0224(11) -0.0016(8) -0.0071(9) -0.0039(8) N11 0.0195(12) 0.0201(13) 0.0300(15) 0.0044(10) -0.0143(11) -0.0067(10) N12 0.0204(12) 0.0204(13) 0.0253(14) 0.0034(10) -0.0132(11) -0.0081(10) C11 0.0395(19) 0.0340(19) 0.0231(18) -0.0092(14) -0.0067(15) -0.0032(15) C12 0.0213(15) 0.0264(16) 0.0244(17) -0.0038(13) -0.0099(13) -0.0074(13) C13 0.0281(17) 0.0295(18) 0.053(2) 0.0078(16) -0.0250(17) -0.0141(14) C14 0.0373(19) 0.0314(18) 0.0268(19) -0.0083(14) -0.0054(15) -0.0037(15) C15 0.0157(14) 0.0241(16) 0.0260(17) -0.0055(13) -0.0091(12) -0.0028(12) C16 0.0245(16) 0.0336(18) 0.038(2) 0.0017(15) -0.0180(15) -0.0117(14) C111 0.0233(15) 0.0208(15) 0.0260(17) 0.0030(12) -0.0130(13) -0.0086(12) C112 0.0274(17) 0.0230(16) 0.0341(19) -0.0033(13) -0.0166(14) -0.0006(13) C113 0.039(2) 0.0327(19) 0.048(2) -0.0022(16) -0.0301(18) -0.0003(16) C114 0.053(2) 0.037(2) 0.033(2) 0.0046(16) -0.0267(18) -0.0150(17) C115 0.040(2) 0.039(2) 0.0259(19) -0.0001(15) -0.0104(15) -0.0173(16) C116 0.0241(16) 0.0289(17) 0.0276(18) 0.0030(13) -0.0094(14) -0.0070(13) C121 0.0162(14) 0.0264(16) 0.0281(17) -0.0050(13) -0.0101(13) 0.0002(12) C122 0.0248(16) 0.0269(17) 0.0326(19) 0.0003(14) -0.0110(14) 0.0020(13) C123 0.0297(18) 0.043(2) 0.0241(19) 0.0000(15) -0.0058(14) 0.0002(15) C124 0.0264(18) 0.045(2) 0.038(2) -0.0172(17) -0.0108(16) 0.0036(15) C125 0.0301(18) 0.0265(17) 0.048(2) -0.0116(16) -0.0151(17) -0.0010(14) C126 0.0253(16) 0.0264(17) 0.035(2) -0.0038(14) -0.0125(14) -0.0051(13) C131 0.0220(15) 0.0233(16) 0.0304(18) -0.0022(13) -0.0076(13) -0.0087(12) C132 0.0339(18) 0.0306(18) 0.033(2) -0.0042(14) -0.0112(15) -0.0099(14) C133 0.050(2) 0.050(2) 0.037(2) -0.0123(18) -0.0146(18) -0.0170(19) C134 0.053(2) 0.042(2) 0.058(3) -0.025(2) -0.007(2) -0.0191(19) C135 0.057(3) 0.0221(19) 0.069(3) -0.0090(18) -0.008(2) -0.0119(17) C136 0.040(2) 0.0251(17) 0.035(2) 0.0010(15) -0.0056(16) -0.0075(15) C141 0.0206(15) 0.0172(14) 0.0252(17) 0.0035(12) -0.0068(13) -0.0042(12) C142 0.0241(16) 0.0291(17) 0.0336(19) 0.0040(14) -0.0105(14) -0.0089(13) C143 0.0218(17) 0.038(2) 0.043(2) 0.0096(16) -0.0083(15) -0.0120(14) C144 0.0275(18) 0.038(2) 0.032(2) 0.0074(16) 0.0029(15) -0.0038(15) C145 0.038(2) 0.0349(19) 0.0283(19) 0.0026(15) -0.0060(16) -0.0072(16) C146 0.0261(16) 0.0262(17) 0.0287(18) 0.0027(13) -0.0070(14) -0.0068(13) C151 0.0242(15) 0.0253(16) 0.0228(17) 0.0065(12) -0.0146(13) -0.0098(13) C152 0.0273(17) 0.0303(17) 0.0286(18) 0.0023(14) -0.0132(14) -0.0049(14) C153 0.0319(18) 0.0340(19) 0.045(2) 0.0124(16) -0.0258(17) -0.0060(15) C154 0.036(2) 0.052(2) 0.031(2) 0.0103(17) -0.0194(16) -0.0182(17) C155 0.0335(18) 0.045(2) 0.0231(18) 0.0013(15) -0.0116(15) -0.0145(16) C156 0.0274(17) 0.0313(17) 0.0300(19) 0.0002(14) -0.0141(14) -0.0087(14) C161 0.0185(15) 0.0290(17) 0.0272(17) -0.0011(13) -0.0134(13) -0.0030(12) C162 0.0214(16) 0.0338(18) 0.0296(19) -0.0033(14) -0.0108(14) -0.0044(13) C163 0.0270(18) 0.050(2) 0.0266(19) -0.0035(16) -0.0054(14) -0.0091(16) C164 0.0266(18) 0.051(2) 0.034(2) -0.0173(17) -0.0105(15) 0.0010(16) C165 0.0314(18) 0.0310(18) 0.043(2) -0.0106(16) -0.0185(16) -0.0004(14) C166 0.0237(16) 0.0292(17) 0.035(2) -0.0048(14) -0.0136(14) -0.0016(13) C171 0.0194(15) 0.0260(16) 0.0232(17) -0.0039(12) -0.0039(12) -0.0111(12) C172 0.0335(18) 0.0347(19) 0.0291(19) -0.0022(14) -0.0071(15) -0.0170(15) C173 0.040(2) 0.058(2) 0.0246(19) -0.0156(17) -0.0007(15) -0.0246(18) C174 0.0303(19) 0.040(2) 0.052(3) -0.0226(18) -0.0016(17) -0.0128(16) C175 0.0297(18) 0.0290(18) 0.050(2) -0.0109(16) -0.0100(17) -0.0028(14) C176 0.0251(16) 0.0299(17) 0.0317(19) -0.0054(14) -0.0082(14) -0.0048(13) C181 0.0167(14) 0.0204(15) 0.0216(16) 0.0030(12) -0.0066(12) -0.0044(11) C182 0.0246(16) 0.0319(18) 0.0288(18) 0.0000(14) -0.0075(14) -0.0134(14) C183 0.0304(18) 0.0357(19) 0.033(2) 0.0039(15) -0.0082(15) -0.0202(15) C184 0.0295(18) 0.0386(19) 0.0250(18) 0.0062(15) -0.0030(14) -0.0128(15) C185 0.0381(19) 0.0370(19) 0.0228(18) -0.0031(14) -0.0086(15) -0.0111(15) C186 0.0285(17) 0.0274(16) 0.0230(17) -0.0010(13) -0.0077(13) -0.0094(13) Mo21 0.0141(1) 0.0141(1) 0.0160(1) -0.0001(1) -0.0040(1) -0.0041(1) Mo22 0.0128(1) 0.0146(1) 0.0156(1) -0.0003(1) -0.0038(1) -0.0032(1) P21 0.0155(4) 0.0198(4) 0.0181(4) 0.0000(3) -0.0050(3) -0.0057(3) P22 0.0143(3) 0.0187(4) 0.0196(4) 0.0006(3) -0.0041(3) -0.0053(3) P23 0.0145(3) 0.0181(4) 0.0172(4) -0.0017(3) -0.0051(3) -0.0030(3) P24 0.0165(4) 0.0180(4) 0.0170(4) -0.0007(3) -0.0038(3) -0.0064(3) O21 0.0155(10) 0.0191(10) 0.0185(11) -0.0008(8) -0.0026(8) -0.0041(8) O22 0.0189(10) 0.0167(10) 0.0209(11) -0.0009(8) -0.0061(8) -0.0028(8) O23 0.0171(10) 0.0196(10) 0.0212(11) -0.0037(8) -0.0058(8) -0.0027(8) O24 0.0199(10) 0.0181(10) 0.0228(12) -0.0017(8) -0.0078(9) -0.0019(8) N21 0.0178(12) 0.0275(14) 0.0220(14) 0.0030(11) -0.0060(10) -0.0097(10) N22 0.0166(12) 0.0261(13) 0.0206(14) 0.0028(10) -0.0059(10) -0.0098(10) C21 0.0340(18) 0.0237(16) 0.0267(18) -0.0071(13) -0.0053(14) 0.0018(14) C22 0.0141(13) 0.0197(15) 0.0233(17) -0.0028(12) -0.0050(12) -0.0040(11) C23 0.0202(16) 0.051(2) 0.034(2) 0.0053(16) -0.0108(14) -0.0180(15) C24 0.0335(18) 0.0267(17) 0.034(2) -0.0099(15) -0.0098(15) 0.0060(14) C25 0.0161(14) 0.0199(15) 0.0278(18) -0.0039(12) -0.0069(12) -0.0036(11) C26 0.0194(16) 0.0396(19) 0.039(2) 0.0067(15) -0.0133(14) -0.0158(14) C211 0.0143(14) 0.0297(17) 0.0235(17) 0.0029(13) -0.0051(12) -0.0073(12) C212 0.0275(18) 0.056(2) 0.0260(19) -0.0074(17) -0.0077(15) 0.0071(16) C213 0.032(2) 0.081(3) 0.029(2) -0.001(2) -0.0159(17) 0.011(2) C214 0.0234(18) 0.047(2) 0.046(2) 0.0142(18) -0.0143(17) -0.0012(16) C215 0.0290(19) 0.0324(19) 0.059(3) 0.0015(17) -0.0206(18) -0.0022(15) C216 0.0266(17) 0.0274(17) 0.039(2) -0.0027(14) -0.0157(15) -0.0042(14) C221 0.0208(15) 0.0262(16) 0.0257(17) -0.0027(13) -0.0116(13) -0.0060(12) C222 0.045(2) 0.0293(18) 0.034(2) -0.0036(15) -0.0093(16) -0.0144(16) C223 0.068(3) 0.0293(19) 0.048(3) -0.0089(17) -0.020(2) -0.0161(18) C224 0.046(2) 0.041(2) 0.052(3) -0.0237(19) -0.0188(19) -0.0053(17) C225 0.0258(17) 0.047(2) 0.035(2) -0.0174(16) -0.0097(15) -0.0056(15) C226 0.0230(16) 0.0283(17) 0.0339(19) -0.0063(14) -0.0098(14) -0.0072(13) C231 0.0166(14) 0.0243(16) 0.0252(17) -0.0018(12) -0.0042(12) -0.0068(12) C232 0.0266(17) 0.0289(17) 0.0290(19) 0.0007(14) -0.0001(14) -0.0044(14) C233 0.0314(19) 0.0323(19) 0.044(2) -0.0063(16) -0.0002(17) -0.0005(15) C234 0.039(2) 0.042(2) 0.033(2) -0.0161(17) 0.0020(16) -0.0051(17) C235 0.055(2) 0.052(2) 0.027(2) -0.0079(17) -0.0071(18) -0.004(2) C236 0.0332(19) 0.038(2) 0.0286(19) -0.0063(15) -0.0096(15) 0.0029(15) C241 0.0227(15) 0.0205(15) 0.0237(17) 0.0026(12) -0.0089(13) -0.0072(12) C242 0.0222(16) 0.0263(17) 0.036(2) 0.0017(14) -0.0048(14) -0.0064(13) C243 0.0304(19) 0.0328(19) 0.046(2) 0.0103(16) -0.0053(16) -0.0181(15) C244 0.037(2) 0.0240(18) 0.060(3) 0.0054(17) -0.0164(19) -0.0115(15) C245 0.0324(19) 0.0197(17) 0.068(3) -0.0016(17) -0.0125(19) -0.0028(14) C246 0.0200(16) 0.0265(17) 0.042(2) -0.0012(15) -0.0065(14) -0.0070(13) C251 0.0187(14) 0.0212(15) 0.0181(15) -0.0010(11) -0.0058(12) -0.0073(12) C252 0.0228(15) 0.0234(16) 0.0312(18) -0.0039(13) -0.0139(14) -0.0019(12) C253 0.0355(18) 0.0344(18) 0.0293(19) -0.0034(14) -0.0190(15) -0.0095(15) C254 0.0369(18) 0.0307(17) 0.0210(17) -0.0027(13) -0.0098(14) -0.0137(14) C255 0.0274(17) 0.0306(17) 0.0234(17) -0.0069(13) -0.0045(13) -0.0068(13) C256 0.0218(15) 0.0275(16) 0.0245(17) -0.0035(13) -0.0087(13) -0.0053(13) C261 0.0149(14) 0.0247(16) 0.0306(18) -0.0074(13) -0.0094(13) -0.0017(12) C262 0.0223(16) 0.0384(19) 0.034(2) -0.0138(15) -0.0060(14) -0.0029(14) C263 0.0234(18) 0.048(2) 0.053(3) -0.029(2) -0.0029(17) 0.0013(16) C264 0.0278(19) 0.030(2) 0.079(3) -0.023(2) -0.019(2) 0.0056(15) C265 0.034(2) 0.0236(18) 0.067(3) -0.0054(17) -0.026(2) 0.0042(15) C266 0.0243(16) 0.0237(16) 0.040(2) -0.0054(14) -0.0142(15) -0.0007(13) C271 0.0183(14) 0.0198(15) 0.0253(17) -0.0030(12) -0.0056(12) -0.0075(12) C272 0.0245(16) 0.0298(17) 0.0236(17) -0.0042(13) -0.0069(13) -0.0094(13) C273 0.0283(17) 0.039(2) 0.038(2) -0.0194(16) -0.0110(15) -0.0047(15) C274 0.0270(17) 0.0249(17) 0.059(3) -0.0176(17) -0.0148(17) 0.0000(14) C275 0.0318(18) 0.0220(16) 0.047(2) -0.0012(15) -0.0203(16) -0.0037(14) C276 0.0286(17) 0.0254(16) 0.0288(18) -0.0048(13) -0.0129(14) -0.0053(13) C281 0.0211(15) 0.0251(16) 0.0183(16) -0.0003(12) -0.0007(12) -0.0096(12) C282 0.0260(16) 0.0255(16) 0.0267(18) -0.0017(13) -0.0050(13) -0.0122(13) C283 0.0367(19) 0.040(2) 0.031(2) -0.0046(16) 0.0022(15) -0.0238(16) C284 0.058(3) 0.066(3) 0.035(2) -0.018(2) 0.0225(19) -0.038(2) C285 0.068(3) 0.062(3) 0.050(3) -0.037(2) 0.025(2) -0.041(2) C286 0.043(2) 0.038(2) 0.031(2) -0.0121(16) 0.0127(16) -0.0256(17) O33 0.0254(14) 0.0532(19) 0.0282(16) -0.0053(13) -0.0105(12) 0.0031(13) C31 0.055(3) 0.072(3) 0.048(3) -0.010(2) -0.017(2) -0.003(2) C32 0.042(2) 0.088(3) 0.039(3) -0.006(2) -0.013(2) -0.005(2) C33 0.0254(14) 0.0532(19) 0.0282(16) -0.0053(13) -0.0105(12) 0.0031(13) C34 0.0211(19) 0.074(3) 0.063(3) -0.014(2) -0.0121(19) 0.0000(19) C35 0.035(2) 0.080(4) 0.087(4) 0.000(3) -0.015(3) -0.009(2) C36 0.069(10) 0.35(3) 0.17(2) 0.12(2) 0.007(11) 0.092(15) O43 0.0336(16) 0.0461(18) 0.046(2) -0.0073(15) -0.0128(14) -0.0031(14) C41 0.0207(16) 0.0388(19) 0.0301(19) -0.0100(15) -0.0044(13) -0.0109(14) C42 0.044(2) 0.062(3) 0.074(3) -0.021(3) -0.023(2) -0.002(2) C43 0.0336(16) 0.0461(18) 0.046(2) -0.0073(15) -0.0128(14) -0.0031(14) C44 0.027(2) 0.066(3) 0.137(5) 0.054(3) -0.033(3) -0.027(2) C45 0.101(5) 0.133(6) 0.063(4) -0.043(4) -0.006(4) -0.021(4) C46 0.043(7) 0.074(9) 0.33(3) 0.038(14) -0.013(12) 0.032(6) F1 0.0865(19) 0.0353(13) 0.0773(19) 0.0250(12) -0.0451(16) -0.0079(12) F2 0.0510(15) 0.097(2) 0.0521(16) 0.0253(14) -0.0173(13) -0.0344(14) F3 0.096(2) 0.0479(14) 0.0540(16) -0.0183(12) -0.0451(15) 0.0046(13) F4 0.0598(16) 0.0755(18) 0.0439(15) -0.0275(13) -0.0061(12) 0.0175(13) B1 0.033(2) 0.0251(19) 0.024(2) -0.0015(15) -0.0089(16) 0.0004(16) F5 0.084(2) 0.0476(15) 0.119(3) 0.0445(16) -0.0611(19) -0.0149(14) F6 0.0502(16) 0.0790(19) 0.109(3) 0.0255(17) -0.0239(16) -0.0361(14) F7 0.0318(11) 0.0582(14) 0.0555(15) -0.0194(12) -0.0161(11) 0.0081(10) F8 0.116(3) 0.172(4) 0.061(2) -0.072(2) -0.018(2) 0.036(3) B2 0.031(2) 0.029(2) 0.029(2) 0.0018(16) -0.0082(17) 0.0009(16) F9 0.0472(13) 0.0644(15) 0.0337(13) 0.0228(10) -0.0194(10) -0.0258(11) F10 0.0593(14) 0.0518(13) 0.0310(12) -0.0077(10) -0.0052(10) -0.0350(11) F11 0.0603(14) 0.0380(12) 0.0409(13) -0.0032(9) -0.0301(11) -0.0033(10) F12 0.0546(14) 0.0353(12) 0.0644(16) -0.0116(11) -0.0274(12) -0.0065(10) B3 0.048(2) 0.034(2) 0.023(2) 0.0014(16) -0.0103(18) -0.0186(18) F13 0.0376(12) 0.0410(12) 0.0522(15) 0.0016(10) 0.0005(10) -0.0114(10) F14 0.0490(14) 0.099(2) 0.0528(16) -0.0097(14) -0.0217(12) -0.0291(14) F15 0.0626(15) 0.0689(16) 0.0373(14) 0.0221(11) -0.0254(12) -0.0146(13) F16 0.0626(16) 0.0376(13) 0.0776(19) -0.0132(12) -0.0058(14) -0.0032(11) B4 0.032(2) 0.031(2) 0.025(2) 0.0058(16) -0.0067(16) -0.0097(16) # =================================================================== # 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 Mo11 Mo12 2.1151(3) . . yes Mo11 P11 2.5817(9) . . yes Mo11 P14 2.6027(9) . . yes Mo11 O11 2.082(2) . . yes Mo11 O14 2.113(2) . . yes Mo12 P12 2.6028(9) . . yes Mo12 P13 2.5532(9) . . yes Mo12 O12 2.107(2) . . yes Mo12 O13 2.087(2) . . yes Mo21 O24 2.099(2) . . yes Mo21 Mo22 2.1161(3) . . yes Mo21 P21 2.5705(9) . . yes Mo21 P24 2.5838(9) . . yes Mo21 O21 2.0962(19) . . yes Mo22 P23 2.5802(9) . . yes Mo22 P22 2.5918(9) . . yes Mo22 O23 2.095(2) . . yes Mo22 O22 2.108(2) . . yes P11 C111 1.817(3) . . yes P11 C121 1.821(3) . . yes P11 N11 1.694(3) . . yes P12 C141 1.825(3) . . yes P12 N11 1.696(3) . . yes P12 C131 1.818(3) . . yes P13 C151 1.818(3) . . yes P13 N12 1.694(3) . . yes P13 C161 1.818(3) . . yes P14 C171 1.813(3) . . yes P14 N12 1.703(3) . . yes P14 C181 1.822(3) . . yes P21 C211 1.813(3) . . yes P21 C221 1.823(3) . . yes P21 N21 1.692(3) . . yes P22 C231 1.816(3) . . yes P22 C241 1.818(3) . . yes P22 N21 1.697(3) . . yes P23 C261 1.817(3) . . yes P23 C251 1.815(3) . . yes P23 N22 1.694(3) . . yes P24 N22 1.691(3) . . yes P24 C271 1.825(3) . . yes P24 C281 1.819(3) . . yes F1 B1 1.392(5) . . yes F2 B1 1.366(6) . . yes F3 B1 1.364(5) . . yes F4 B1 1.363(5) . . yes F5 B2 1.373(5) . . yes F6 B2 1.363(6) . . yes F7 B2 1.362(5) . . yes F8 B2 1.346(5) . . yes O11 C12 1.275(4) . . yes O12 C12 1.284(4) . . yes O13 C15 1.276(4) . . yes O14 C15 1.275(4) . . yes F9 B3 1.390(4) . . yes F10 B3 1.389(5) . . yes F11 B3 1.371(5) . . yes F12 B3 1.387(4) . . yes O21 C22 1.279(3) . . yes O22 C22 1.273(4) . . yes O23 C25 1.277(4) . . yes O24 C25 1.278(4) . . yes F13 B4 1.374(5) . . yes F14 B4 1.372(6) . . yes F15 B4 1.393(5) . . yes F16 B4 1.372(4) . . yes O33 C32 1.409(6) . . yes O33 C34 1.402(5) . . yes O33 H33A 0.9908 . . no O33 H33B 0.9890 . . no O43 C42 1.420(6) . . yes O43 C44 1.323(7) . . yes O43 H43A 0.9896 . . no O43 H43B 0.9903 . . no N11 C13 1.480(5) . . yes N12 C16 1.486(4) . . yes N21 C23 1.483(4) . . yes N22 C26 1.481(4) . . yes C11 C12 1.479(5) . . no C14 C15 1.494(5) . . no C11 H11A 0.9795 . . no C11 H11C 0.9802 . . no C111 C116 1.396(5) . . no C111 C112 1.391(5) . . no C11 H11B 0.9795 . . no C112 C113 1.383(5) . . no C13 H13C 0.9794 . . no C13 H13A 0.9794 . . no C113 C114 1.382(5) . . no C13 H13B 0.9804 . . no C14 H14B 0.9791 . . no C14 H14C 0.9808 . . no C114 C115 1.390(6) . . no C14 H14A 0.9809 . . no C115 C116 1.386(5) . . no C16 H16B 0.9796 . . no C16 H16C 0.9798 . . no C16 H16A 0.9796 . . no C121 C126 1.399(4) . . no C121 C122 1.392(5) . . no C122 C123 1.399(5) . . no C123 C124 1.376(5) . . no C124 C125 1.382(5) . . no C125 C126 1.385(5) . . no C131 C136 1.394(5) . . no C131 C132 1.389(5) . . no C132 C133 1.379(5) . . no C133 C134 1.377(5) . . no C134 C135 1.369(6) . . no C135 C136 1.399(5) . . no C141 C146 1.388(5) . . no C141 C142 1.409(5) . . no C142 C143 1.385(5) . . no C143 C144 1.375(5) . . no C144 C145 1.386(5) . . no C145 C146 1.387(5) . . no C151 C156 1.391(5) . . no C151 C152 1.396(5) . . no C152 C153 1.396(5) . . no C153 C154 1.375(5) . . no C154 C155 1.381(5) . . no C155 C156 1.388(5) . . no C161 C166 1.405(5) . . no C161 C162 1.389(5) . . no C162 C163 1.390(5) . . no C163 C164 1.378(5) . . no C164 C165 1.383(5) . . no C165 C166 1.382(5) . . no C171 C176 1.400(4) . . no C171 C172 1.393(5) . . no C172 C173 1.392(5) . . no C173 C174 1.383(5) . . no C174 C175 1.381(6) . . no C175 C176 1.389(5) . . no C181 C186 1.393(4) . . no C181 C182 1.401(5) . . no C182 C183 1.377(5) . . no C183 C184 1.380(5) . . no C184 C185 1.393(5) . . no C185 C186 1.380(5) . . no C112 H112 0.9504 . . no C113 H113 0.9494 . . no C114 H114 0.9499 . . no C115 H115 0.9499 . . no C116 H116 0.9497 . . no C21 C22 1.496(4) . . no C122 H122 0.9510 . . no C123 H123 0.9513 . . no C24 C25 1.492(4) . . no C124 H124 0.9499 . . no C125 H125 0.9506 . . no C126 H126 0.9510 . . no C132 H132 0.9497 . . no C133 H133 0.9503 . . no C134 H134 0.9499 . . no C135 H135 0.9497 . . no C136 H136 0.9497 . . no C142 H142 0.9493 . . no C143 H143 0.9491 . . no C144 H144 0.9507 . . no C145 H145 0.9506 . . no C146 H146 0.9513 . . no C152 H152 0.9507 . . no C153 H153 0.9499 . . no C154 H154 0.9489 . . no C155 H155 0.9490 . . no C156 H156 0.9497 . . no C162 H162 0.9507 . . no C163 H163 0.9495 . . no C164 H164 0.9488 . . no C165 H165 0.9507 . . no C166 H166 0.9492 . . no C172 H172 0.9498 . . no C173 H173 0.9505 . . no C174 H174 0.9496 . . no C175 H175 0.9497 . . no C176 H176 0.9501 . . no C182 H182 0.9498 . . no C183 H183 0.9498 . . no C184 H184 0.9501 . . no C185 H185 0.9508 . . no C186 H186 0.9500 . . no C21 H21B 0.9805 . . no C21 H21C 0.9801 . . no C21 H21A 0.9801 . . no C23 H23A 0.9806 . . no C23 H23B 0.9802 . . no C23 H23C 0.9802 . . no C24 H24B 0.9794 . . no C24 H24A 0.9798 . . no C24 H24C 0.9804 . . no C26 H26C 0.9797 . . no C26 H26A 0.9806 . . no C26 H26B 0.9799 . . no C211 C216 1.392(4) . . no C211 C212 1.386(5) . . no C212 C213 1.392(6) . . no C213 C214 1.372(5) . . no C214 C215 1.377(6) . . no C215 C216 1.389(5) . . no C221 C226 1.387(5) . . no C221 C222 1.402(5) . . no C222 C223 1.387(5) . . no C223 C224 1.377(6) . . no C224 C225 1.395(5) . . no C225 C226 1.381(5) . . no C231 C232 1.383(5) . . no C231 C236 1.387(5) . . no C31 C32 1.485(8) . . no C32 C33 1.409(6) . . no C232 C233 1.395(5) . . no C33 C34 1.402(5) . . no C233 C234 1.366(5) . . no C34 C35 1.528(7) . . no C234 C235 1.386(6) . . no C235 C236 1.376(5) . . no C35 C36 1.74(2) . . no C241 C242 1.400(5) . . no C241 C246 1.389(5) . . no C242 C243 1.383(5) . . no C243 C244 1.375(5) . . no C244 C245 1.387(5) . . no C245 C246 1.392(5) . . no C251 C252 1.400(5) . . no C251 C256 1.401(4) . . no C252 C253 1.382(5) . . no C253 C254 1.385(5) . . no C254 C255 1.381(5) . . no C255 C256 1.387(4) . . no C261 C262 1.395(5) . . no C261 C266 1.390(5) . . no C262 C263 1.392(5) . . no C263 C264 1.371(6) . . no C264 C265 1.370(6) . . no C265 C266 1.392(5) . . no C271 C276 1.390(4) . . no C271 C272 1.398(4) . . no C272 C273 1.386(5) . . no C273 C274 1.385(5) . . no C274 C275 1.380(5) . . no C275 C276 1.387(4) . . no C281 C286 1.394(5) . . no C281 C282 1.393(5) . . no C282 C283 1.380(5) . . no C283 C284 1.376(5) . . no C284 C285 1.380(6) . . no C285 C286 1.384(6) . . no C212 H212 0.9511 . . no C213 H213 0.9499 . . no C214 H214 0.9503 . . no C215 H215 0.9507 . . no C216 H216 0.9490 . . no C222 H222 0.9497 . . no C223 H223 0.9481 . . no C224 H224 0.9514 . . no C225 H225 0.9501 . . no C226 H226 0.9505 . . no C31 H31B 0.9788 . . no C31 H31A 0.9813 . . no C31 H31C 0.9805 . . no C232 H232 0.9508 . . no C32 H32A 0.9896 . . no C32 H32B 0.9897 . . no C33 H33A 0.9908 . . no C33 H33B 0.9890 . . no C233 H233 0.9487 . . no C34 H34B 0.9904 . . no C234 H234 0.9495 . . no C34 H34A 0.9903 . . no C35 H35E 0.9804 . . no C35 H35D 0.9794 . . no C35 H35A 0.9892 . . no C35 H35B 0.9897 . . no C35 H35C 0.9794 . . no C235 H235 0.9490 . . no C36 H36A 0.9802 . . no C36 H35D 0.9553 . . no C236 H236 0.9494 . . no C36 H36B 0.9791 . . no C36 H36C 0.9789 . . no C242 H242 0.9491 . . no C243 H243 0.9501 . . no C244 H244 0.9493 . . no C245 H245 0.9499 . . no C246 H246 0.9504 . . no C252 H252 0.9504 . . no C253 H253 0.9499 . . no C254 H254 0.9506 . . no C255 H255 0.9500 . . no C256 H256 0.9506 . . no C262 H262 0.9501 . . no C263 H263 0.9500 . . no C264 H264 0.9490 . . no C265 H265 0.9501 . . no C266 H266 0.9500 . . no C272 H272 0.9498 . . no C273 H273 0.9502 . . no C274 H274 0.9497 . . no C275 H275 0.9502 . . no C276 H276 0.9491 . . no C282 H282 0.9488 . . no C283 H283 0.9499 . . no C284 H284 0.9504 . . no C285 H285 0.9507 . . no C286 H286 0.9505 . . no C41 C42 1.484(6) . . no C42 C43 1.420(6) . . no C43 C44 1.323(7) . . no C44 C45 1.656(9) . . no C45 C46 1.43(2) . . no C41 H41A 0.9791 . . no C41 H41B 0.9792 . . no C41 H41C 0.9805 . . no C42 H42B 0.9901 . . no C42 H42A 0.9903 . . no C43 H43B 0.9903 . . no C43 H43A 0.9896 . . no C44 H44A 0.9897 . . no C44 H44B 0.9906 . . no C45 H45A 0.9892 . . no C45 H45B 0.9898 . . no C45 H45D 0.9790 . . no C45 H45E 0.9800 . . no C45 H45C 0.9808 . . no C46 H45C 1.0638 . . no C46 H46B 0.9787 . . no C46 H46C 0.9794 . . no C46 H46A 0.9809 . . 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 Mo12 Mo11 P11 95.46(2) . . . yes Mo12 Mo11 P14 100.27(2) . . . yes Mo12 Mo11 O11 92.71(6) . . . yes Mo12 Mo11 O14 90.58(5) . . . yes P11 Mo11 P14 160.60(3) . . . yes P11 Mo11 O11 84.66(6) . . . yes P11 Mo11 O14 94.98(6) . . . yes P14 Mo11 O11 83.32(6) . . . yes P14 Mo11 O14 96.14(6) . . . yes O11 Mo11 O14 176.72(8) . . . yes Mo11 Mo12 P12 101.68(2) . . . yes Mo11 Mo12 P13 96.23(2) . . . yes Mo11 Mo12 O12 90.40(5) . . . yes Mo11 Mo12 O13 92.39(6) . . . yes P12 Mo12 P13 160.43(3) . . . yes P12 Mo12 O12 94.50(6) . . . yes P12 Mo12 O13 84.38(6) . . . yes P13 Mo12 O12 93.19(6) . . . yes P13 Mo12 O13 87.08(6) . . . yes O12 Mo12 O13 177.16(8) . . . yes P21 Mo21 P24 163.62(3) . . . yes P21 Mo21 O21 85.64(6) . . . yes P21 Mo21 O24 92.72(6) . . . yes Mo22 Mo21 P21 96.66(2) . . . yes Mo22 Mo21 P24 99.72(2) . . . yes Mo22 Mo21 O21 91.71(5) . . . yes Mo22 Mo21 O24 91.44(6) . . . yes P24 Mo21 O21 93.53(6) . . . yes P24 Mo21 O24 87.20(6) . . . yes O21 Mo21 O24 176.60(8) . . . yes Mo21 Mo22 O23 91.55(6) . . . yes P22 Mo22 P23 163.53(3) . . . yes P22 Mo22 O22 94.81(6) . . . yes Mo21 Mo22 P22 99.24(2) . . . yes Mo21 Mo22 P23 97.05(2) . . . yes Mo21 Mo22 O22 91.08(6) . . . yes P23 Mo22 O22 87.27(6) . . . yes P23 Mo22 O23 93.93(6) . . . yes P22 Mo22 O23 83.25(6) . . . yes O22 Mo22 O23 176.95(8) . . . yes Mo11 P11 N11 112.49(10) . . . yes Mo11 P11 C111 117.07(11) . . . yes C111 P11 C121 106.84(15) . . . yes Mo11 P11 C121 112.41(11) . . . yes N11 P11 C111 101.87(14) . . . yes N11 P11 C121 105.01(14) . . . yes Mo12 P12 C141 118.71(11) . . . yes N11 P12 C131 101.54(14) . . . yes N11 P12 C141 105.72(14) . . . yes Mo12 P12 C131 114.96(12) . . . yes Mo12 P12 N11 108.15(10) . . . yes C131 P12 C141 106.06(14) . . . yes N12 P13 C161 105.58(14) . . . yes C151 P13 C161 107.23(15) . . . yes Mo12 P13 N12 113.20(10) . . . yes Mo12 P13 C151 114.33(11) . . . yes Mo12 P13 C161 112.14(11) . . . yes N12 P13 C151 103.59(14) . . . yes N12 P14 C171 104.01(14) . . . yes N12 P14 C181 107.31(14) . . . yes C171 P14 C181 101.64(14) . . . yes Mo11 P14 C171 112.42(11) . . . yes Mo11 P14 C181 120.66(11) . . . yes Mo11 P14 N12 109.37(10) . . . yes N21 P21 C211 104.36(14) . . . yes N21 P21 C221 106.53(14) . . . yes Mo21 P21 N21 111.50(10) . . . yes Mo21 P21 C211 115.88(11) . . . yes Mo21 P21 C221 111.90(11) . . . yes C211 P21 C221 105.96(15) . . . yes C231 P22 C241 102.87(14) . . . yes Mo22 P22 N21 110.25(10) . . . yes Mo22 P22 C231 112.18(11) . . . yes Mo22 P22 C241 119.14(11) . . . yes N21 P22 C231 104.63(14) . . . yes N21 P22 C241 106.60(14) . . . yes C251 P23 C261 106.27(14) . . . yes Mo22 P23 C251 117.97(11) . . . yes Mo22 P23 C261 110.57(11) . . . yes Mo22 P23 N22 112.71(10) . . . yes N22 P23 C261 104.70(14) . . . yes N22 P23 C251 103.55(13) . . . yes Mo21 P24 C281 117.34(11) . . . yes Mo21 P24 C271 113.05(11) . . . yes Mo21 P24 N22 110.45(10) . . . yes C271 P24 C281 103.67(14) . . . yes N22 P24 C271 105.10(14) . . . yes N22 P24 C281 106.26(14) . . . yes Mo11 O11 C12 117.45(18) . . . yes Mo12 O12 C12 118.11(19) . . . yes Mo12 O13 C15 117.61(18) . . . yes Mo11 O14 C15 118.03(19) . . . yes Mo21 O21 C22 117.61(17) . . . yes Mo22 O22 C22 117.92(18) . . . yes Mo22 O23 C25 117.70(19) . . . yes Mo21 O24 C25 117.53(18) . . . yes C32 O33 C34 110.7(3) . . . yes C32 O33 H33B 109.52 . . . no C32 O33 H33A 109.50 . . . no C34 O33 H33B 109.46 . . . no H33A O33 H33B 108.11 . . . no C34 O33 H33A 109.51 . . . no C42 O43 C44 105.6(4) . . . yes C44 O43 H43B 110.60 . . . no C42 O43 H43B 110.65 . . . no C42 O43 H43A 110.63 . . . no C44 O43 H43A 110.67 . . . no H43A O43 H43B 108.66 . . . no P12 N11 C13 121.5(2) . . . yes P11 N11 C13 119.3(2) . . . yes P11 N11 P12 118.62(16) . . . yes P13 N12 P14 116.81(16) . . . yes P14 N12 C16 121.5(2) . . . yes P13 N12 C16 120.6(2) . . . yes P22 N21 C23 121.7(2) . . . yes P21 N21 C23 120.1(2) . . . yes P21 N21 P22 117.10(16) . . . yes P23 N22 P24 118.38(16) . . . yes P23 N22 C26 120.2(2) . . . yes P24 N22 C26 121.4(2) . . . yes O11 C12 O12 121.1(3) . . . yes O11 C12 C11 119.5(3) . . . yes O12 C12 C11 119.3(3) . . . yes O13 C15 O14 121.4(3) . . . yes O13 C15 C14 119.0(3) . . . yes O14 C15 C14 119.7(3) . . . yes C112 C111 C116 119.7(3) . . . no P11 C111 C116 116.7(2) . . . yes C12 C11 H11C 109.43 . . . no H11A C11 H11B 109.53 . . . no C12 C11 H11A 109.43 . . . no C12 C11 H11B 109.57 . . . no H11A C11 H11C 109.48 . . . no H11B C11 H11C 109.39 . . . no P11 C111 C112 123.2(2) . . . yes C111 C112 C113 119.7(3) . . . no H13A C13 H13B 109.55 . . . no N11 C13 H13A 109.41 . . . no N11 C13 H13C 109.42 . . . no N11 C13 H13B 109.41 . . . no H13B C13 H13C 109.50 . . . no C112 C113 C114 120.7(4) . . . no H13A C13 H13C 109.54 . . . no C15 C14 H14A 109.47 . . . no H14B C14 H14C 109.52 . . . no C15 C14 H14C 109.44 . . . no C15 C14 H14B 109.45 . . . no H14A C14 H14B 109.49 . . . no H14A C14 H14C 109.46 . . . no C113 C114 C115 120.0(4) . . . no C114 C115 C116 119.6(3) . . . no N12 C16 H16B 109.46 . . . no H16B C16 H16C 109.44 . . . no C111 C116 C115 120.2(3) . . . no H16A C16 H16C 109.50 . . . no N12 C16 H16C 109.46 . . . no H16A C16 H16B 109.56 . . . no N12 C16 H16A 109.41 . . . no P11 C121 C122 119.5(2) . . . yes P11 C121 C126 121.3(2) . . . yes C122 C121 C126 118.9(3) . . . no C121 C122 C123 120.5(3) . . . no C122 C123 C124 119.7(3) . . . no C123 C124 C125 120.2(3) . . . no C124 C125 C126 120.6(3) . . . no C121 C126 C125 120.0(3) . . . no P12 C131 C136 121.4(3) . . . yes C132 C131 C136 118.8(3) . . . no P12 C131 C132 119.7(2) . . . yes C131 C132 C133 121.1(3) . . . no C132 C133 C134 119.9(4) . . . no C133 C134 C135 119.9(4) . . . no C134 C135 C136 120.9(4) . . . no C131 C136 C135 119.3(3) . . . no C142 C141 C146 118.6(3) . . . no P12 C141 C146 119.1(2) . . . yes P12 C141 C142 121.8(2) . . . yes C141 C142 C143 119.9(3) . . . no C142 C143 C144 120.7(3) . . . no C143 C144 C145 119.9(3) . . . no C144 C145 C146 119.9(3) . . . no C141 C146 C145 120.8(3) . . . no P13 C151 C152 123.9(2) . . . yes P13 C151 C156 117.3(2) . . . yes C152 C151 C156 118.8(3) . . . no C151 C152 C153 119.9(3) . . . no C152 C153 C154 120.4(3) . . . no C153 C154 C155 120.2(3) . . . no C154 C155 C156 119.7(3) . . . no C151 C156 C155 120.9(3) . . . no P13 C161 C162 120.3(2) . . . yes C162 C161 C166 118.6(3) . . . no P13 C161 C166 120.9(2) . . . yes C161 C162 C163 120.6(3) . . . no C162 C163 C164 120.2(3) . . . no C163 C164 C165 119.9(3) . . . no C164 C165 C166 120.4(3) . . . no C161 C166 C165 120.2(3) . . . no P14 C171 C176 119.4(2) . . . yes P14 C171 C172 121.1(2) . . . yes C172 C171 C176 119.4(3) . . . no C171 C172 C173 120.1(3) . . . no C172 C173 C174 120.0(3) . . . no C173 C174 C175 120.4(3) . . . no C174 C175 C176 120.1(3) . . . no C171 C176 C175 119.9(3) . . . no P14 C181 C186 120.2(2) . . . yes P14 C181 C182 121.4(2) . . . yes C182 C181 C186 118.4(3) . . . no C181 C182 C183 120.7(3) . . . no C182 C183 C184 120.6(3) . . . no C183 C184 C185 119.2(3) . . . no C184 C185 C186 120.5(3) . . . no C181 C186 C185 120.6(3) . . . no C113 C112 H112 120.20 . . . no C111 C112 H112 120.13 . . . no C114 C113 H113 119.69 . . . no C112 C113 H113 119.60 . . . no C115 C114 H114 120.01 . . . no C113 C114 H114 119.99 . . . no C114 C115 H115 120.20 . . . no C116 C115 H115 120.16 . . . no C115 C116 H116 119.89 . . . no C111 C116 H116 119.87 . . . no O21 C22 O22 121.2(3) . . . yes O21 C22 C21 118.7(3) . . . yes C121 C122 H122 119.68 . . . no O22 C22 C21 120.1(3) . . . yes C123 C122 H122 119.81 . . . no C124 C123 H123 120.14 . . . no C122 C123 H123 120.13 . . . no C123 C124 H124 119.88 . . . no C125 C124 H124 119.93 . . . no O23 C25 C24 119.0(3) . . . yes C126 C125 H125 119.64 . . . no O23 C25 O24 121.5(3) . . . yes O24 C25 C24 119.4(3) . . . yes C124 C125 H125 119.74 . . . no C121 C126 H126 120.01 . . . no C125 C126 H126 120.01 . . . no C133 C132 H132 119.49 . . . no C131 C132 H132 119.40 . . . no C134 C133 H133 120.10 . . . no C132 C133 H133 119.95 . . . no C135 C134 H134 120.12 . . . no C133 C134 H134 120.00 . . . no C136 C135 H135 119.48 . . . no C134 C135 H135 119.59 . . . no C135 C136 H136 120.39 . . . no C131 C136 H136 120.32 . . . no C141 C142 H142 120.11 . . . no C143 C142 H142 120.00 . . . no C142 C143 H143 119.69 . . . no C144 C143 H143 119.57 . . . no C143 C144 H144 120.07 . . . no C145 C144 H144 120.04 . . . no C144 C145 H145 119.99 . . . no C146 C145 H145 120.07 . . . no C141 C146 H146 119.63 . . . no C145 C146 H146 119.55 . . . no C151 C152 H152 120.04 . . . no C153 C152 H152 120.02 . . . no C154 C153 H153 119.87 . . . no C152 C153 H153 119.78 . . . no C155 C154 H154 119.87 . . . no C153 C154 H154 119.88 . . . no C156 C155 H155 120.10 . . . no C154 C155 H155 120.20 . . . no C155 C156 H156 119.58 . . . no C151 C156 H156 119.51 . . . no C161 C162 H162 119.63 . . . no C163 C162 H162 119.73 . . . no C164 C163 H163 120.03 . . . no C162 C163 H163 119.81 . . . no C165 C164 H164 120.07 . . . no C163 C164 H164 120.00 . . . no C164 C165 H165 119.80 . . . no C166 C165 H165 119.80 . . . no C161 C166 H166 119.87 . . . no C165 C166 H166 119.88 . . . no C173 C172 H172 119.99 . . . no C171 C172 H172 119.95 . . . no C172 C173 H173 119.95 . . . no C174 C173 H173 120.09 . . . no C173 C174 H174 119.84 . . . no C175 C174 H174 119.73 . . . no C174 C175 H175 119.93 . . . no C176 C175 H175 119.97 . . . no C171 C176 H176 119.99 . . . no C175 C176 H176 120.07 . . . no C181 C182 H182 119.63 . . . no C183 C182 H182 119.68 . . . no C182 C183 H183 119.74 . . . no C184 C183 H183 119.64 . . . no C183 C184 H184 120.45 . . . no C185 C184 H184 120.32 . . . no C184 C185 H185 119.76 . . . no C186 C185 H185 119.77 . . . no C185 C186 H186 119.68 . . . no C181 C186 H186 119.73 . . . no C22 C21 H21A 109.45 . . . no H21A C21 H21B 109.45 . . . no H21B C21 H21C 109.44 . . . no C22 C21 H21C 109.43 . . . no H21A C21 H21C 109.55 . . . no C22 C21 H21B 109.51 . . . no N21 C23 H23A 109.49 . . . no H23B C23 H23C 109.43 . . . no H23A C23 H23B 109.45 . . . no N21 C23 H23C 109.46 . . . no H23A C23 H23C 109.50 . . . no N21 C23 H23B 109.49 . . . no C25 C24 H24A 109.43 . . . no C25 C24 H24C 109.42 . . . no H24A C24 H24B 109.52 . . . no H24B C24 H24C 109.48 . . . no C25 C24 H24B 109.49 . . . no H24A C24 H24C 109.50 . . . no N22 C26 H26B 109.52 . . . no N22 C26 H26A 109.52 . . . no H26A C26 H26C 109.48 . . . no N22 C26 H26C 109.52 . . . no H26B C26 H26C 109.37 . . . no H26A C26 H26B 109.42 . . . no P21 C211 C216 118.0(2) . . . yes C212 C211 C216 118.7(3) . . . no P21 C211 C212 123.1(3) . . . yes C211 C212 C213 120.4(3) . . . no C212 C213 C214 120.0(4) . . . no C213 C214 C215 120.5(4) . . . no C214 C215 C216 119.6(3) . . . no C211 C216 C215 120.7(3) . . . no P21 C221 C226 120.5(2) . . . yes P21 C221 C222 120.3(2) . . . yes C222 C221 C226 119.1(3) . . . no C221 C222 C223 119.8(3) . . . no C222 C223 C224 120.8(4) . . . no C223 C224 C225 119.6(4) . . . no C224 C225 C226 119.9(3) . . . no C221 C226 C225 120.8(3) . . . no P22 C231 C236 118.6(2) . . . yes P22 C231 C232 122.0(2) . . . yes C232 C231 C236 119.3(3) . . . no O33 C32 C31 110.2(4) . . . yes C231 C232 C233 119.9(3) . . . no C31 C32 C33 110.2(4) . . . no C32 C33 C34 110.7(3) . . . no C232 C233 C234 120.4(3) . . . no O33 C34 C35 107.2(4) . . . yes C33 C34 C35 107.2(4) . . . no C233 C234 C235 119.8(4) . . . no C234 C235 C236 120.2(4) . . . no C34 C35 C36 103.0(8) . . . no C231 C236 C235 120.4(3) . . . no P22 C241 C242 121.6(2) . . . yes C242 C241 C246 119.4(3) . . . no P22 C241 C246 119.0(3) . . . yes C241 C242 C243 120.3(3) . . . no C242 C243 C244 120.3(3) . . . no C243 C244 C245 119.8(3) . . . no C244 C245 C246 120.6(3) . . . no C241 C246 C245 119.6(3) . . . no P23 C251 C252 123.6(2) . . . yes C252 C251 C256 118.6(3) . . . no P23 C251 C256 117.7(2) . . . yes C251 C252 C253 120.0(3) . . . no C252 C253 C254 121.0(3) . . . no C253 C254 C255 119.6(3) . . . no C254 C255 C256 120.1(3) . . . no C251 C256 C255 120.7(3) . . . no P23 C261 C262 119.2(2) . . . yes C262 C261 C266 119.4(3) . . . no P23 C261 C266 121.0(2) . . . yes C261 C262 C263 120.0(3) . . . no C262 C263 C264 120.2(4) . . . no C263 C264 C265 120.1(4) . . . no C264 C265 C266 121.0(4) . . . no C261 C266 C265 119.3(3) . . . no P24 C271 C276 119.5(2) . . . yes C272 C271 C276 119.4(3) . . . no P24 C271 C272 120.9(2) . . . yes C271 C272 C273 120.1(3) . . . no C272 C273 C274 120.1(3) . . . no C273 C274 C275 119.9(3) . . . no C274 C275 C276 120.5(3) . . . no C271 C276 C275 120.0(3) . . . no P24 C281 C282 122.5(2) . . . yes C282 C281 C286 118.8(3) . . . no P24 C281 C286 118.7(2) . . . yes C281 C282 C283 120.9(3) . . . no C282 C283 C284 119.9(3) . . . no C283 C284 C285 119.9(4) . . . no C284 C285 C286 120.8(4) . . . no C281 C286 C285 119.7(3) . . . no C211 C212 H212 119.75 . . . no C213 C212 H212 119.82 . . . no C214 C213 H213 120.04 . . . no C212 C213 H213 119.98 . . . no C213 C214 H214 119.83 . . . no C215 C214 H214 119.68 . . . no C214 C215 H215 120.20 . . . no C216 C215 H215 120.16 . . . no C211 C216 H216 119.65 . . . no C215 C216 H216 119.68 . . . no C221 C222 H222 120.12 . . . no C223 C222 H222 120.08 . . . no C222 C223 H223 119.65 . . . no C224 C223 H223 119.58 . . . no C223 C224 H224 120.19 . . . no C225 C224 H224 120.18 . . . no C224 C225 H225 119.99 . . . no C226 C225 H225 120.07 . . . no C225 C226 H226 119.64 . . . no C221 C226 H226 119.57 . . . no H31A C31 H31C 109.46 . . . no C32 C31 H31A 109.33 . . . no C32 C31 H31B 109.58 . . . no H31A C31 H31B 109.41 . . . no H31B C31 H31C 109.48 . . . no C32 C31 H31C 109.57 . . . no O33 C32 H32A 109.53 . . . no C31 C32 H32B 109.62 . . . no C33 C32 H32A 109.53 . . . no C33 C32 H32B 109.62 . . . no H32A C32 H32B 108.18 . . . no C31 C32 H32A 109.63 . . . no C233 C232 H232 120.04 . . . no O33 C32 H32B 109.62 . . . no C231 C232 H232 120.11 . . . no C32 C33 H33A 109.50 . . . no C32 C33 H33B 109.52 . . . no C234 C233 H233 119.83 . . . no C232 C233 H233 119.81 . . . no C34 C33 H33B 109.46 . . . no H33A C33 H33B 108.11 . . . no C34 C33 H33A 109.51 . . . no C235 C234 H234 120.13 . . . no C33 C34 H34A 110.24 . . . no O33 C34 H34A 110.24 . . . no C233 C234 H234 120.04 . . . no C35 C34 H34A 110.31 . . . no C35 C34 H34B 110.29 . . . no C33 C34 H34B 110.29 . . . no O33 C34 H34B 110.29 . . . no H34A C34 H34B 108.56 . . . no C34 C35 H35E 109.50 . . . no H35A C35 H35B 109.11 . . . no H35C C35 H35D 109.56 . . . no H35C C35 H35E 109.43 . . . no H35D C35 H35E 109.48 . . . no C234 C235 H235 119.92 . . . no C36 C35 H35A 111.17 . . . no C36 C35 H35B 111.24 . . . no C36 C35 H35C 133.16 . . . no C36 C35 H35D 25.37 . . . no C36 C35 H35E 89.77 . . . no H35A C35 H35C 87.74 . . . no H35A C35 H35D 126.70 . . . no H35A C35 H35E 23.18 . . . no H35B C35 H35C 24.85 . . . no H35B C35 H35D 86.29 . . . no H35B C35 H35E 127.74 . . . no C34 C35 H35B 111.13 . . . no C34 C35 H35C 109.43 . . . no C34 C35 H35D 109.42 . . . no C236 C235 H235 119.91 . . . no C34 C35 H35A 111.15 . . . no C35 C36 H35D 26.05 . . . no C35 C36 H36C 109.50 . . . no C35 C36 H36A 109.43 . . . no C35 C36 H36B 109.48 . . . no C235 C236 H236 119.83 . . . no H36A C36 H36C 109.41 . . . no H35D C36 H36C 134.86 . . . no H36A C36 H36B 109.42 . . . no C231 C236 H236 119.81 . . . no H36B C36 H36C 109.59 . . . no H35D C36 H36B 91.35 . . . no H35D C36 H36A 99.72 . . . no C243 C242 H242 119.89 . . . no C241 C242 H242 119.85 . . . no C244 C243 H243 119.79 . . . no C242 C243 H243 119.86 . . . no C245 C244 H244 120.11 . . . no C243 C244 H244 120.14 . . . no C246 C245 H245 119.69 . . . no C244 C245 H245 119.68 . . . no C245 C246 H246 120.24 . . . no C241 C246 H246 120.20 . . . no C253 C252 H252 120.02 . . . no C251 C252 H252 119.98 . . . no C254 C253 H253 119.43 . . . no C252 C253 H253 119.58 . . . no C253 C254 H254 120.19 . . . no C255 C254 H254 120.16 . . . no C256 C255 H255 120.01 . . . no C254 C255 H255 119.91 . . . no C251 C256 H256 119.61 . . . no C255 C256 H256 119.69 . . . no C261 C262 H262 120.03 . . . no C263 C262 H262 119.98 . . . no C262 C263 H263 119.88 . . . no C264 C263 H263 119.94 . . . no C263 C264 H264 119.97 . . . no C265 C264 H264 119.96 . . . no C264 C265 H265 119.52 . . . no C266 C265 H265 119.49 . . . no C261 C266 H266 120.31 . . . no C265 C266 H266 120.36 . . . no C273 C272 H272 119.94 . . . no C271 C272 H272 119.97 . . . no C272 C273 H273 119.92 . . . no C274 C273 H273 119.95 . . . no C273 C274 H274 120.08 . . . no C275 C274 H274 119.99 . . . no C276 C275 H275 119.73 . . . no C274 C275 H275 119.77 . . . no C275 C276 H276 120.06 . . . no C271 C276 H276 119.99 . . . no C283 C282 H282 119.57 . . . no C281 C282 H282 119.55 . . . no C282 C283 H283 120.08 . . . no C284 C283 H283 120.00 . . . no C285 C284 H284 120.01 . . . no C283 C284 H284 120.09 . . . no C286 C285 H285 119.65 . . . no C284 C285 H285 119.60 . . . no C281 C286 H286 120.13 . . . no C285 C286 H286 120.18 . . . no O43 C42 C41 106.2(4) . . . yes C41 C42 C43 106.2(4) . . . no C42 C43 C44 105.6(4) . . . no C43 C44 C45 102.8(4) . . . no O43 C44 C45 102.8(4) . . . yes C44 C45 C46 150.8(8) . . . no C42 C41 H41A 109.45 . . . no C42 C41 H41B 109.41 . . . no C42 C41 H41C 109.44 . . . no H41A C41 H41B 109.46 . . . no H41A C41 H41C 109.57 . . . no H41B C41 H41C 109.49 . . . no O43 C42 H42A 110.52 . . . no O43 C42 H42B 110.50 . . . no C41 C42 H42A 110.52 . . . no C41 C42 H42B 110.52 . . . no C43 C42 H42A 110.52 . . . no C43 C42 H42B 110.50 . . . no H42A C42 H42B 108.61 . . . no C42 C43 H43A 110.63 . . . no C42 C43 H43B 110.65 . . . no C44 C43 H43A 110.67 . . . no C44 C43 H43B 110.60 . . . no H43A C43 H43B 108.66 . . . no O43 C44 H44A 111.17 . . . no O43 C44 H44B 111.26 . . . no C43 C44 H44A 111.17 . . . no C43 C44 H44B 111.26 . . . no C45 C44 H44A 111.18 . . . no C45 C44 H44B 111.18 . . . no H44A C44 H44B 109.19 . . . no C44 C45 H45A 98.89 . . . no C44 C45 H45B 98.93 . . . no C44 C45 H45C 109.42 . . . no C44 C45 H45D 109.56 . . . no C44 C45 H45E 109.50 . . . no C46 C45 H45A 98.93 . . . no C46 C45 H45B 98.89 . . . no C46 C45 H45C 48.17 . . . no C46 C45 H45D 97.08 . . . no C46 C45 H45E 70.63 . . . no H45A C45 H45B 104.02 . . . no H45A C45 H45C 146.62 . . . no H45A C45 H45D 75.84 . . . no H45A C45 H45E 42.03 . . . no H45B C45 H45C 89.03 . . . no H45B C45 H45D 28.89 . . . no H45B C45 H45E 137.48 . . . no H45C C45 H45D 109.39 . . . no H45C C45 H45E 109.45 . . . no H45D C45 H45E 109.51 . . . no C45 C46 H45C 43.39 . . . no C45 C46 H46A 109.39 . . . no C45 C46 H46B 109.47 . . . no C45 C46 H46C 109.40 . . . no H45C C46 H46A 134.00 . . . no H45C C46 H46B 114.66 . . . no H45C C46 H46C 67.28 . . . no H46A C46 H46B 109.45 . . . no H46A C46 H46C 109.53 . . . no H46B C46 H46C 109.58 . . . no F1 B1 F2 108.2(4) . . . yes F1 B1 F3 110.0(3) . . . yes F1 B1 F4 108.1(3) . . . yes F2 B1 F3 110.5(3) . . . yes F2 B1 F4 110.0(3) . . . yes F3 B1 F4 110.0(4) . . . yes F5 B2 F6 108.0(4) . . . yes F5 B2 F7 108.2(3) . . . yes F5 B2 F8 110.5(3) . . . yes F6 B2 F7 110.0(3) . . . yes F6 B2 F8 111.3(4) . . . yes F7 B2 F8 108.8(4) . . . yes F9 B3 F10 107.9(3) . . . yes F9 B3 F11 109.5(3) . . . yes F9 B3 F12 108.2(3) . . . yes F10 B3 F11 110.3(3) . . . yes F10 B3 F12 110.1(3) . . . yes F11 B3 F12 110.8(3) . . . yes F13 B4 F14 110.0(3) . . . yes F13 B4 F15 108.6(3) . . . yes F13 B4 F16 110.1(3) . . . yes F14 B4 F15 108.4(3) . . . yes F14 B4 F16 110.1(4) . . . yes F15 B4 F16 109.4(3) . . . yes # End of Crystallographic Information File