Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _publ_contact_author_name 'Malcolm L.H.Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; _publ_contact_author_phone '(01865) 272649' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chemistry.ox.ac.uk' _journal_coden_Cambridge 186 _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? loop_ _publ_author_name 'N.G.Jones' 'M.L.H.Green' 'I.C.Vei' 'L.H.Rees' 'S.Pascu' 'D.Watkin' 'X.Morise' 'P.Braunstein' #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of eta6-arene complexes of Molybdenum containing beta-ketophosphine and related P,O mixed donor ligands. ; ## -----------------REFERENCES ----------------------## _publ_section_references ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Chebychev Weights # Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 # Denzo # Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' data_1b _database_code_CSD 168488 #============= Material Relevant to Compound(1b)===================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #************************************************************************** _cell_length_a 25.516(2) _cell_angle_alpha 90 _cell_length_b 9.196(4) _cell_angle_beta 112.973(2) _cell_length_c 23.678(2) _cell_angle_gamma 90 _cell_volume 5115.3 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C30 H30 Cl1 Mo1 O1 P1 ' _chemical_formula_moiety ' C30 H30 Cl1 Mo1 O1 P1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 568.93 _cell_measurement_reflns_used 20774 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2323.172 _exptl_absorpt_coefficient_mu 0.701 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.93 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 20774 _reflns_number_total 4959 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 4959 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5291 _diffrn_measured_fraction_theta_max 0.937 _reflns_number_gt 4721 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.48 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -31 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _refine_diff_density_min -0.90 _refine_diff_density_max 0.72 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4721 _refine_ls_number_parameters 307 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0374 _refine_ls_goodness_of_fit_ref 0.9985 _refine_ls_shift/su_max 0.000786 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 1.99 -.223 1.62 0.812E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Mo1 0.883857(9) 0.56386(2) 0.08210(1) 0.0185 1.0000 Uani Cl1 0.78601(3) 0.46080(7) 0.02738(3) 0.0262 1.0000 Uani P1 0.90786(3) 0.29814(7) 0.07672(3) 0.0183 1.0000 Uani O1 0.92731(8) 0.3204(2) -0.0397(1) 0.0311 1.0000 Uani C1 0.86687(11) 0.2089(3) 0.00275(12) 0.0213 1.0000 Uani C2 0.88171(11) 0.2622(3) -0.04917(13) 0.0223 1.0000 Uani C11 0.83955(12) 0.2425(3) -0.11330(13) 0.0251 1.0000 Uani C12 0.85018(14) 0.3095(3) -0.16048(14) 0.0346 1.0000 Uani C13 0.81328(17) 0.2960(4) -0.22032(16) 0.0458 1.0000 Uani C14 0.76463(15) 0.2118(5) -0.23466(15) 0.0477 1.0000 Uani C15 0.75359(14) 0.1432(4) -0.18896(15) 0.0422 1.0000 Uani C16 0.79056(12) 0.1590(3) -0.12797(13) 0.0303 1.0000 Uani C21 0.88929(11) 0.1795(3) 0.12851(12) 0.0210 1.0000 Uani C22 0.83278(11) 0.1397(3) 0.11409(12) 0.0246 1.0000 Uani C23 0.81823(13) 0.0612(3) 0.15596(14) 0.0318 1.0000 Uani C24 0.85919(15) 0.0230(3) 0.21232(14) 0.0340 1.0000 Uani C25 0.91533(14) 0.0631(4) 0.22698(14) 0.0359 1.0000 Uani C26 0.93012(12) 0.1405(3) 0.18521(13) 0.0287 1.0000 Uani C31 0.98153(11) 0.2408(3) 0.09489(13) 0.0242 1.0000 Uani C32 0.99343(13) 0.1023(3) 0.07805(15) 0.0343 1.0000 Uani C33 1.04914(15) 0.0564(4) 0.09464(17) 0.0436 1.0000 Uani C34 1.09349(14) 0.1460(4) 0.12827(18) 0.0442 1.0000 Uani C35 1.08258(13) 0.2809(4) 0.14558(18) 0.0444 1.0000 Uani C36 1.02680(12) 0.3296(3) 0.12866(15) 0.0340 1.0000 Uani C41 0.94935(14) 0.6193(3) 0.03965(19) 0.0422 1.0000 Uani C42 0.89442(15) 0.6197(3) -0.00660(15) 0.0347 1.0000 Uani C43 0.85387(14) 0.7232(3) -0.00486(15) 0.0336 1.0000 Uani C44 0.79859(17) 0.7373(4) -0.05814(19) 0.0517 1.0000 Uani C45 0.86416(15) 0.8012(3) 0.04779(16) 0.0364 1.0000 Uani C46 0.91852(15) 0.7876(3) 0.09824(16) 0.0401 1.0000 Uani C47 0.96185(15) 0.7080(4) 0.0898(2) 0.0498 1.0000 Uani C51 0.84382(13) 0.6317(3) 0.14766(14) 0.0318 1.0000 Uani C52 0.87666(13) 0.5045(3) 0.16818(13) 0.0295 1.0000 Uani C53 0.93568(14) 0.5213(3) 0.18229(14) 0.0357 1.0000 Uani H11 0.8744 0.1019 0.0076 0.0261 1.0000 Uiso H12 0.8255 0.2273 -0.0079 0.0261 1.0000 Uiso H121 0.8856 0.3687 -0.1504 0.0444 1.0000 Uiso H131 0.8213 0.3464 -0.2535 0.0583 1.0000 Uiso H141 0.7376 0.2010 -0.2784 0.0575 1.0000 Uiso H151 0.7188 0.0815 -0.1996 0.0504 1.0000 Uiso H161 0.7820 0.1104 -0.0948 0.0377 1.0000 Uiso H221 0.8027 0.1677 0.0736 0.0295 1.0000 Uiso H231 0.7777 0.0320 0.1452 0.0398 1.0000 Uiso H241 0.8484 -0.0332 0.2423 0.0439 1.0000 Uiso H251 0.9452 0.0361 0.2678 0.0426 1.0000 Uiso H261 0.9707 0.1686 0.1961 0.0346 1.0000 Uiso H321 0.9614 0.0362 0.0539 0.0420 1.0000 Uiso H331 1.0571 -0.0422 0.0821 0.0559 1.0000 Uiso H341 1.1337 0.1126 0.1401 0.0565 1.0000 Uiso H351 1.1150 0.3451 0.1706 0.0522 1.0000 Uiso H361 1.0194 0.4290 0.1410 0.0400 1.0000 Uiso H411 0.9794 0.5544 0.0361 0.0562 1.0000 Uiso H421 0.8839 0.5473 -0.0407 0.0470 1.0000 Uiso H441 0.7752 0.8145 -0.0495 0.0609 1.0000 Uiso H442 0.8056 0.7643 -0.0955 0.0609 1.0000 Uiso H443 0.7778 0.6425 -0.0653 0.0609 1.0000 Uiso H451 0.8342 0.8668 0.0511 0.0493 1.0000 Uiso H461 0.9253 0.8342 0.1387 0.0496 1.0000 Uiso H471 1.0020 0.7160 0.1204 0.0596 1.0000 Uiso H511 0.8625 0.7247 0.1440 0.0411 1.0000 Uiso H512 0.8018 0.6288 0.1368 0.0411 1.0000 Uiso H521 0.8596 0.4094 0.1725 0.0364 1.0000 Uiso H531 0.9511 0.6183 0.1774 0.0390 1.0000 Uiso H532 0.9619 0.4361 0.1971 0.0390 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01955(11) 0.01460(11) 0.02258(11) -0.00306(9) 0.00947(8) -0.00157(8) Cl1 0.0208(3) 0.0264(3) 0.0302(3) -0.0011(2) 0.0088(2) -0.0018(2) P1 0.0175(3) 0.0170(3) 0.0217(3) -0.0026(2) 0.0090(3) -0.0010(2) O1 0.030(1) 0.033(1) 0.0372(11) -0.0028(9) 0.0199(9) -0.0052(8) C1 0.0267(12) 0.0175(11) 0.0212(12) -0.0039(9) 0.0110(11) -0.0033(9) C2 0.0283(13) 0.0146(11) 0.0291(14) -0.0012(9) 0.0167(12) 0.0025(9) C11 0.0324(14) 0.0203(12) 0.0288(14) 0.000(1) 0.0189(12) 0.007(1) C12 0.0456(17) 0.0317(15) 0.0337(15) 0.0075(12) 0.0234(14) 0.0039(13) C13 0.063(2) 0.050(2) 0.0330(17) 0.0137(15) 0.0277(17) 0.0160(17) C14 0.0464(19) 0.072(3) 0.0255(16) -0.0006(15) 0.0148(15) 0.0200(18) C15 0.0336(15) 0.062(2) 0.0303(16) -0.0108(15) 0.0118(14) -0.0003(15) C16 0.0306(13) 0.0388(16) 0.0248(14) -0.0029(12) 0.0142(12) -0.0021(12) C21 0.0271(12) 0.0134(11) 0.0239(12) -0.0025(9) 0.0115(11) -0.0005(9) C22 0.0277(13) 0.0213(13) 0.0247(13) -0.005(1) 0.0100(11) -0.006(1) C23 0.0368(14) 0.0262(13) 0.0364(15) -0.0063(12) 0.0186(13) -0.0103(12) C24 0.0512(18) 0.0291(15) 0.0294(15) -0.0012(11) 0.0240(14) -0.0088(13) C25 0.0422(16) 0.0356(16) 0.0286(14) 0.0027(13) 0.0125(13) -0.0039(14) C26 0.0327(14) 0.0256(14) 0.0281(14) -0.0026(11) 0.0123(12) -0.0047(11) C31 0.0242(12) 0.0257(13) 0.0260(13) 0.004(1) 0.0132(11) 0.005(1) C32 0.0349(15) 0.0324(15) 0.0376(16) 0.0020(12) 0.0164(14) 0.0095(12) C33 0.0487(19) 0.0411(18) 0.0500(19) 0.0081(16) 0.0291(16) 0.0205(16) C34 0.0350(16) 0.050(2) 0.057(2) 0.0250(17) 0.0274(16) 0.0212(15) C35 0.0236(14) 0.0469(19) 0.060(2) 0.0171(16) 0.0132(15) 0.0042(13) C36 0.0262(13) 0.0269(14) 0.0468(18) 0.0059(13) 0.0121(13) 0.0025(11) C41 0.0346(16) 0.0287(15) 0.077(3) 0.0108(16) 0.0371(18) 0.0018(13) C42 0.0554(19) 0.0212(13) 0.0408(17) 0.0077(12) 0.0333(16) 0.0052(13) C43 0.0424(16) 0.0217(13) 0.0421(17) 0.0117(12) 0.0225(15) 0.0003(12) C44 0.051(2) 0.046(2) 0.055(2) 0.0196(17) 0.0175(19) 0.0071(16) C45 0.0560(19) 0.0149(13) 0.0525(19) 0.0079(12) 0.0363(17) 0.0076(12) C46 0.055(2) 0.0221(14) 0.0468(19) -0.0092(13) 0.0240(17) -0.0177(13) C47 0.0373(17) 0.0359(18) 0.076(3) 0.0075(17) 0.0215(18) -0.0157(14) C51 0.0425(16) 0.0310(15) 0.0292(14) -0.0040(12) 0.0221(14) 0.0035(12) C52 0.0432(16) 0.0290(14) 0.0188(12) -0.0030(11) 0.0148(13) 0.0021(12) C53 0.0394(16) 0.0292(15) 0.0288(15) -0.0067(11) 0.0029(13) 0.0000(12) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . Cl1 . 2.5070(6) yes Mo1 . P1 . 2.5344(6) yes Mo1 . C41 . 2.318(3) yes Mo1 . C42 . 2.278(3) yes Mo1 . C43 . 2.396(3) yes Mo1 . C45 . 2.315(3) yes Mo1 . C46 . 2.213(3) yes Mo1 . C47 . 2.338(3) yes Mo1 . C51 . 2.254(3) yes Mo1 . C52 . 2.186(3) yes Mo1 . C53 . 2.254(3) yes P1 . C1 . 1.846(3) yes P1 . C21 . 1.837(3) yes P1 . C31 . 1.835(3) yes O1 . C2 . 1.220(3) yes C1 . C2 . 1.503(4) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C11 . 1.490(4) yes C11 . C12 . 1.392(4) yes C11 . C16 . 1.391(4) yes C12 . C13 . 1.367(5) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.373(5) yes C14 . H141 . 1.000 no C15 . C16 . 1.390(4) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C21 . C22 . 1.395(4) yes C21 . C26 . 1.387(4) yes C22 . C23 . 1.389(4) yes C22 . H221 . 1.000 no C23 . C24 . 1.381(4) yes C23 . H231 . 1.000 no C24 . C25 . 1.386(5) yes C24 . H241 . 1.000 no C25 . C26 . 1.385(4) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C31 . C32 . 1.403(4) yes C31 . C36 . 1.386(4) yes C32 . C33 . 1.384(4) yes C32 . H321 . 1.000 no C33 . C34 . 1.375(5) yes C33 . H331 . 1.000 no C34 . C35 . 1.369(5) yes C34 . H341 . 1.000 no C35 . C36 . 1.394(4) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no C41 . C42 . 1.402(5) yes C41 . C47 . 1.371(6) yes C41 . H411 . 1.000 no C42 . C43 . 1.418(4) yes C42 . H421 . 1.000 no C43 . C44 . 1.486(5) yes C43 . C45 . 1.372(5) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C45 . C46 . 1.440(5) yes C45 . H451 . 1.000 no C46 . C47 . 1.404(5) yes C46 . H461 . 1.000 no C47 . H471 . 1.000 no C51 . C52 . 1.410(4) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . C53 . 1.418(5) yes C52 . H521 . 1.000 no C53 . H531 . 1.000 no C53 . H532 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Mo1 . P1 . 79.69(2) yes Cl1 . Mo1 . C41 . 126.9(1) yes P1 . Mo1 . C41 . 87.76(8) yes Cl1 . Mo1 . C42 . 93.50(9) yes P1 . Mo1 . C42 . 93.05(7) yes C41 . Mo1 . C42 . 35.51(13) yes Cl1 . Mo1 . C43 . 82.38(8) yes P1 . Mo1 . C43 . 123.28(8) yes C41 . Mo1 . C43 . 62.32(11) yes C42 . Mo1 . C43 . 35.20(11) yes Cl1 . Mo1 . C45 . 97.99(9) yes P1 . Mo1 . C45 . 156.23(8) yes C41 . Mo1 . C45 . 74.64(11) yes C42 . Mo1 . C45 . 63.35(11) yes C43 . Mo1 . C45 . 33.81(11) yes Cl1 . Mo1 . C46 . 133.7(1) yes P1 . Mo1 . C46 . 144.8(1) yes C41 . Mo1 . C46 . 64.11(13) yes C42 . Mo1 . C46 . 76.50(12) yes C43 . Mo1 . C46 . 63.39(12) yes Cl1 . Mo1 . C47 . 154.2(1) yes P1 . Mo1 . C47 . 109.6(1) yes C41 . Mo1 . C47 . 34.25(14) yes C42 . Mo1 . C47 . 62.65(14) yes C43 . Mo1 . C47 . 72.36(12) yes Cl1 . Mo1 . C51 . 80.38(8) yes P1 . Mo1 . C51 . 119.00(8) yes C41 . Mo1 . C51 . 146.62(12) yes C42 . Mo1 . C51 . 145.20(11) yes C43 . Mo1 . C51 . 110.13(11) yes Cl1 . Mo1 . C52 . 87.61(8) yes P1 . Mo1 . C52 . 85.18(8) yes C41 . Mo1 . C52 . 142.78(13) yes C42 . Mo1 . C52 . 177.71(11) yes C43 . Mo1 . C52 . 147.04(11) yes Cl1 . Mo1 . C53 . 122.34(9) yes P1 . Mo1 . C53 . 80.29(8) yes C41 . Mo1 . C53 . 105.57(13) yes C42 . Mo1 . C53 . 141.04(13) yes C43 . Mo1 . C53 . 150.46(11) yes C45 . Mo1 . C46 . 37.00(13) yes C45 . Mo1 . C47 . 63.55(13) yes C46 . Mo1 . C47 . 35.81(13) yes C45 . Mo1 . C51 . 83.46(11) yes C46 . Mo1 . C51 . 83.21(12) yes C47 . Mo1 . C51 . 112.98(14) yes C45 . Mo1 . C52 . 118.49(11) yes C46 . Mo1 . C52 . 104.15(12) yes C47 . Mo1 . C52 . 116.60(14) yes C51 . Mo1 . C52 . 36.99(11) yes C45 . Mo1 . C53 . 119.41(12) yes C46 . Mo1 . C53 . 87.08(12) yes C47 . Mo1 . C53 . 83.38(14) yes C51 . Mo1 . C53 . 63.94(12) yes C52 . Mo1 . C53 . 37.21(12) yes Mo1 . P1 . C1 . 114.71(8) yes Mo1 . P1 . C21 . 114.14(8) yes C1 . P1 . C21 . 99.84(11) yes Mo1 . P1 . C31 . 120.74(9) yes C1 . P1 . C31 . 104.12(12) yes C21 . P1 . C31 . 100.38(12) yes P1 . C1 . C2 . 113.62(17) yes P1 . C1 . H11 . 108.43 no C2 . C1 . H11 . 108.4 no P1 . C1 . H12 . 108.43 no C2 . C1 . H12 . 108.4 no H11 . C1 . H12 . 109.5 no O1 . C2 . C1 . 121.4(2) yes O1 . C2 . C11 . 119.8(3) yes C1 . C2 . C11 . 118.8(2) yes C2 . C11 . C12 . 118.3(3) yes C2 . C11 . C16 . 122.9(3) yes C12 . C11 . C16 . 118.8(3) yes C11 . C12 . C13 . 121.4(3) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.3 no C12 . C13 . C14 . 119.5(3) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 120.2 no C13 . C14 . C15 . 120.2(3) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 119.9 no C14 . C15 . C16 . 120.4(3) yes C14 . C15 . H151 . 119.8 no C16 . C15 . H151 . 119.8 no C11 . C16 . C15 . 119.8(3) yes C11 . C16 . H161 . 120.1 no C15 . C16 . H161 . 120.1 no P1 . C21 . C22 . 120.3(2) yes P1 . C21 . C26 . 120.5(2) yes C22 . C21 . C26 . 118.9(2) yes C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 120.0 no C22 . C23 . C24 . 120.6(3) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 119.5(3) yes C23 . C24 . H241 . 120.2 no C25 . C24 . H241 . 120.2 no C24 . C25 . C26 . 120.1(3) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.0 no C21 . C26 . C25 . 120.9(3) yes C21 . C26 . H261 . 119.6 no C25 . C26 . H261 . 119.6 no P1 . C31 . C32 . 120.7(2) yes P1 . C31 . C36 . 120.9(2) yes C32 . C31 . C36 . 118.4(3) yes C31 . C32 . C33 . 120.5(3) yes C31 . C32 . H321 . 119.7 no C33 . C32 . H321 . 119.7 no C32 . C33 . C34 . 120.3(3) yes C32 . C33 . H331 . 119.9 no C34 . C33 . H331 . 119.9 no C33 . C34 . C35 . 119.9(3) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 120.0 no C34 . C35 . C36 . 120.6(3) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 119.7 no C31 . C36 . C35 . 120.3(3) yes C31 . C36 . H361 . 119.9 no C35 . C36 . H361 . 119.9 no Mo1 . C41 . C42 . 70.69(17) yes Mo1 . C41 . C47 . 73.7(2) yes C42 . C41 . C47 . 119.9(3) yes Mo1 . C41 . H411 . 127.6 no C42 . C41 . H411 . 120.1 no C47 . C41 . H411 . 120.1 no Mo1 . C42 . C41 . 73.80(19) yes Mo1 . C42 . C43 . 76.95(18) yes C41 . C42 . C43 . 119.8(3) yes Mo1 . C42 . H421 . 120.2 no C41 . C42 . H421 . 120.1 no C43 . C42 . H421 . 120.1 no Mo1 . C43 . C42 . 67.85(16) yes Mo1 . C43 . C44 . 131.4(2) yes C42 . C43 . C44 . 119.7(3) yes Mo1 . C43 . C45 . 69.84(17) yes C42 . C43 . C45 . 119.6(3) yes C44 . C43 . C45 . 120.5(3) yes C43 . C44 . H441 . 109.5 no C43 . C44 . H442 . 109.5 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 109.5 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no Mo1 . C45 . C43 . 76.35(16) yes Mo1 . C45 . C46 . 67.67(15) yes C43 . C45 . C46 . 119.3(3) yes Mo1 . C45 . H451 . 127.5 no C43 . C45 . H451 . 120.4 no C46 . C45 . H451 . 120.4 no Mo1 . C46 . C45 . 75.33(18) yes Mo1 . C46 . C47 . 76.95(18) yes C45 . C46 . C47 . 119.0(3) yes Mo1 . C46 . H461 . 118.1 no C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 120.5 no Mo1 . C47 . C41 . 72.07(18) yes Mo1 . C47 . C46 . 67.24(17) yes C41 . C47 . C46 . 120.2(3) yes Mo1 . C47 . H471 . 134.2 no C41 . C47 . H471 . 119.9 no C46 . C47 . H471 . 119.9 no Mo1 . C51 . C52 . 68.89(16) yes Mo1 . C51 . H511 . 79.44(17) no C52 . C51 . H511 . 120.0 no Mo1 . C51 . H512 . 122.9 no C52 . C51 . H512 . 120.0 no H511 . C51 . H512 . 120.0 no Mo1 . C52 . C51 . 74.12(17) yes Mo1 . C52 . C53 . 74.00(18) yes C51 . C52 . C53 . 115.1(3) yes Mo1 . C52 . H521 . 120.8 no C51 . C52 . H521 . 122.4 no C53 . C52 . H521 . 122.4 no Mo1 . C53 . C52 . 68.79(17) yes Mo1 . C53 . H531 . 79.55 no C52 . C53 . H531 . 120.0 no Mo1 . C53 . H532 . 122.9 no C52 . C53 . H532 . 120.0 no H531 . C53 . H532 . 120.0 no #==END data_3a _database_code_CSD 168490 #============= Material Relevant to Compound(3a)===================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 12.0880(3) _cell_angle_alpha 90 _cell_length_b 14.8310(4) _cell_angle_beta 95.400(2) _cell_length_c 20.3990(5) _cell_angle_gamma 90 _cell_volume 3640.8 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C23 H19 Mo0.50 O1 P1 ' _chemical_formula_moiety ' C23 H19 Mo0.50 O1 P1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 390.35 _cell_measurement_reflns_used 10555 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 190 _cell_formula_units_Z 8 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1601.516 _exptl_absorpt_coefficient_mu 0.488 # Sheldrick geometric definitions 0.64 0.61 _diffrn_measurement_device_type ; Unknown ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DATA COLLECTION ; _computing_data_reduction ; SPARE ; _computing_cell_refinement ; SPARE ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 190 _diffrn_reflns_number 10555 _reflns_number_total 3708 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 3708 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3727 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_gt 3522 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.48 _refine_diff_density_max 0.48 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3522 _refine_ls_number_parameters 232 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0309 _refine_ls_goodness_of_fit_ref 1.0572 _refine_ls_shift/su_max 0.000657 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 2.46 0.454 2.00 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Spare Spare Spare Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Mo1 0.5000 0.091051(9) 0.7500 0.0182 1.0000 Uani P1 0.61523(3) 0.19774(2) 0.817205(15) 0.0210 1.0000 Uani O1 0.61663(8) 0.13615(6) 0.68628(4) 0.0231 1.0000 Uani C1 0.57103(12) 0.31328(9) 0.83335(6) 0.0252 1.0000 Uani C2 0.62237(13) 0.38554(11) 0.80449(8) 0.0322 1.0000 Uani C3 0.58972(16) 0.47342(11) 0.81494(9) 0.0407 1.0000 Uani C4 0.50452(17) 0.49040(11) 0.85369(9) 0.0444 1.0000 Uani C5 0.45015(17) 0.41932(12) 0.88095(9) 0.0423 1.0000 Uani C6 0.48291(14) 0.33086(11) 0.87082(7) 0.0329 1.0000 Uani C7 0.66331(12) 0.15665(9) 0.89957(6) 0.0251 1.0000 Uani C8 0.58524(14) 0.12961(12) 0.94165(8) 0.0357 1.0000 Uani C9 0.61912(18) 0.09504(12) 1.00357(9) 0.0428 1.0000 Uani C10 0.73127(19) 0.08571(12) 1.02350(9) 0.0468 1.0000 Uani C11 0.80904(17) 0.11062(16) 0.98145(11) 0.0545 1.0000 Uani C12 0.77534(14) 0.14652(13) 0.91983(9) 0.0412 1.0000 Uani C13 0.73038(11) 0.2082(1) 0.77019(7) 0.0272 1.0000 Uani C14 0.70950(11) 0.17803(9) 0.70731(7) 0.0227 1.0000 Uani C15 0.78690(11) 0.19166(9) 0.65518(7) 0.0249 1.0000 Uani C16 0.88462(13) 0.2417(1) 0.66622(8) 0.0332 1.0000 Uani C17 0.95338(14) 0.25431(11) 0.61622(9) 0.0399 1.0000 Uani C18 0.92591(15) 0.21774(13) 0.55465(9) 0.0407 1.0000 Uani C19 0.82973(15) 0.16750(14) 0.54312(8) 0.0432 1.0000 Uani C20 0.76068(13) 0.15426(12) 0.59300(8) 0.0346 1.0000 Uani C21 0.58375(14) -0.0381(1) 0.70799(9) 0.0355 1.0000 Uani C22 0.61340(13) -0.0294(1) 0.77585(9) 0.0360 1.0000 Uani C23 0.52637(15) -0.0286(1) 0.81919(8) 0.0349 1.0000 Uani H21 0.6836 0.3736 0.7759 0.0383 1.0000 Uiso H31 0.6279 0.5246 0.7944 0.0482 1.0000 Uiso H41 0.4820 0.5539 0.8621 0.0527 1.0000 Uiso H51 0.3870 0.4317 0.9080 0.0512 1.0000 Uiso H61 0.4432 0.2799 0.8905 0.0398 1.0000 Uiso H81 0.5042 0.1351 0.9272 0.0431 1.0000 Uiso H91 0.5625 0.0769 1.0338 0.0517 1.0000 Uiso H101 0.7558 0.0611 1.0681 0.0549 1.0000 Uiso H111 0.8900 0.1028 0.9954 0.0638 1.0000 Uiso H121 0.8323 0.1651 0.8899 0.0488 1.0000 Uiso H131 0.8036 0.2337 0.7881 0.0328 1.0000 Uiso H161 0.9053 0.2687 0.7106 0.0408 1.0000 Uiso H171 1.0233 0.2902 0.6249 0.0493 1.0000 Uiso H181 0.9753 0.2275 0.5186 0.0502 1.0000 Uiso H191 0.8098 0.1405 0.4986 0.0525 1.0000 Uiso H201 0.6915 0.1175 0.5842 0.0418 1.0000 Uiso H211 0.6428 -0.0515 0.6782 0.0437 1.0000 Uiso H221 0.6931 -0.0238 0.7936 0.0432 1.0000 Uiso H231 0.5441 -0.0213 0.8678 0.0420 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0199(1) 0.0170(1) 0.0181(1) 0.0000 0.00324(6) 0.0000 P1 0.02168(17) 0.02406(18) 0.01724(16) -0.00039(11) 0.00226(12) -0.00199(12) O1 0.0242(4) 0.0253(5) 0.0204(4) -0.0006(3) 0.0056(4) -0.0017(4) C1 0.0303(7) 0.0251(6) 0.0195(6) -0.0024(5) -0.0019(5) -0.0027(5) C2 0.0350(7) 0.0288(7) 0.0319(7) 0.0006(6) -0.0013(6) -0.0079(6) C3 0.052(1) 0.0272(8) 0.0417(9) 0.0009(6) -0.0044(7) -0.0081(7) C4 0.0643(11) 0.0262(7) 0.0413(9) -0.0057(6) -0.0023(8) 0.0043(7) C5 0.0547(11) 0.0384(9) 0.0349(9) -0.0062(7) 0.0098(8) 0.0094(7) C6 0.0410(8) 0.0314(8) 0.0270(7) -0.0012(5) 0.0065(6) 0.0010(6) C7 0.0281(7) 0.0267(7) 0.0199(6) -0.0011(5) 0.0001(5) -0.0001(5) C8 0.0348(8) 0.0465(9) 0.0265(7) 0.0058(6) 0.0061(6) 0.0050(7) C9 0.0543(11) 0.049(1) 0.0260(8) 0.0065(6) 0.0081(7) 0.0051(7) C10 0.0626(12) 0.048(1) 0.0267(8) 0.0079(7) -0.0117(8) -0.0018(8) C11 0.040(1) 0.0686(12) 0.0509(11) 0.021(1) -0.0171(8) -0.0055(9) C12 0.0294(8) 0.052(1) 0.0409(9) 0.0131(7) -0.0040(7) -0.0042(7) C13 0.0234(6) 0.0335(7) 0.0250(7) -0.0008(5) 0.0043(5) -0.0038(5) C14 0.0211(6) 0.0226(6) 0.0249(6) 0.0021(5) 0.0050(5) 0.0015(5) C15 0.0267(6) 0.0230(6) 0.0259(7) 0.0037(5) 0.0073(5) 0.0045(5) C16 0.0352(8) 0.0280(7) 0.0387(8) -0.0050(6) 0.0153(6) -0.0044(6) C17 0.0386(8) 0.0319(8) 0.053(1) -0.0012(7) 0.0229(8) -0.0054(6) C18 0.0407(9) 0.0451(9) 0.0397(9) 0.0100(7) 0.0216(7) 0.0074(7) C19 0.0413(9) 0.0640(11) 0.0260(7) -0.0005(7) 0.0117(7) 0.0052(8) C20 0.0298(7) 0.0474(9) 0.0273(7) -0.0007(6) 0.0067(6) 0.0016(6) C21 0.0431(8) 0.0201(6) 0.0461(9) -0.0031(6) 0.0191(7) 0.0051(6) C22 0.0332(7) 0.0248(7) 0.0500(9) 0.0032(6) 0.0044(7) 0.0108(6) C23 0.0499(9) 0.0222(7) 0.0330(7) 0.0081(6) 0.0057(7) 0.0023(6) _refine_ls_extinction_coef 83.6(110) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . P1 . 2.4421(3) yes Mo1 . P1 5_656 2.4421(3) yes Mo1 . O1 . 2.1140(9) yes Mo1 . O1 5_656 2.1140(9) yes Mo1 . C21 . 2.3645(14) yes Mo1 . C21 5_656 2.3645(14) yes Mo1 . C22 . 2.2825(14) yes Mo1 . C22 5_656 2.2825(14) yes Mo1 . C23 . 2.2707(14) yes Mo1 . C23 5_656 2.2707(14) yes P1 . C1 . 1.8339(14) yes P1 . C7 . 1.8298(14) yes P1 . C13 . 1.7699(14) yes O1 . C14 . 1.3189(17) yes C1 . C2 . 1.396(2) yes C1 . C6 . 1.393(2) yes C2 . C3 . 1.384(2) yes C2 . H21 . 1.0000 no C3 . C4 . 1.379(3) yes C3 . H31 . 1.0000 no C4 . C5 . 1.386(3) yes C4 . H41 . 1.0000 no C5 . C6 . 1.392(2) yes C5 . H51 . 1.0000 no C6 . H61 . 1.0000 no C7 . C8 . 1.393(2) yes C7 . C12 . 1.386(2) yes C8 . C9 . 1.389(2) yes C8 . H81 . 1.0000 no C9 . C10 . 1.385(3) yes C9 . H91 . 1.0000 no C10 . C11 . 1.381(3) yes C10 . H101 . 1.0000 no C11 . C12 . 1.390(3) yes C11 . H111 . 1.0000 no C12 . H121 . 1.0000 no C13 . C14 . 1.359(2) yes C13 . H131 . 1.0000 no C14 . C15 . 1.4947(18) yes C15 . C16 . 1.395(2) yes C15 . C20 . 1.393(2) yes C16 . C17 . 1.388(2) yes C16 . H161 . 1.0000 no C17 . C18 . 1.380(3) yes C17 . H171 . 1.0000 no C18 . C19 . 1.382(3) yes C18 . H181 . 1.0000 no C19 . C20 . 1.389(2) yes C19 . H191 . 1.0000 no C20 . H201 . 1.0000 no C21 . C22 . 1.403(3) yes C21 . C23 5_656 1.400(2) yes C21 . H211 . 1.0000 no C22 . C23 . 1.437(2) yes C22 . H221 . 1.0000 no C23 . H231 . 1.0000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Mo1 . P1 5_656 99.228(16) yes P1 . Mo1 . O1 . 76.23(3) yes P1 5_656 Mo1 . O1 . 80.09(3) yes P1 . Mo1 . O1 5_656 80.09(3) yes P1 5_656 Mo1 . O1 5_656 76.23(3) yes O1 . Mo1 . O1 5_656 143.11(5) yes P1 . Mo1 . C21 . 119.16(4) yes P1 5_656 Mo1 . C21 . 124.22(4) yes O1 . Mo1 . C21 . 72.57(5) yes O1 5_656 Mo1 . C21 . 144.31(5) yes P1 . Mo1 . C21 5_656 124.22(4) yes P1 5_656 Mo1 . C21 5_656 119.16(4) yes O1 . Mo1 . C21 5_656 144.31(5) yes O1 5_656 Mo1 . C21 5_656 72.57(5) yes C21 . Mo1 . C21 5_656 71.81(8) yes P1 . Mo1 . C22 . 94.52(4) yes P1 5_656 Mo1 . C22 . 159.23(5) yes O1 . Mo1 . C22 . 88.21(5) yes O1 5_656 Mo1 . C22 . 121.75(5) yes C21 . Mo1 . C22 . 35.09(6) yes P1 . Mo1 . C22 5_656 159.23(5) yes P1 5_656 Mo1 . C22 5_656 94.52(4) yes O1 . Mo1 . C22 5_656 121.75(5) yes O1 5_656 Mo1 . C22 5_656 88.21(5) yes C21 . Mo1 . C22 5_656 63.31(6) yes P1 . Mo1 . C23 . 96.77(4) yes P1 5_656 Mo1 . C23 . 153.44(4) yes O1 . Mo1 . C23 . 124.51(5) yes O1 5_656 Mo1 . C23 . 85.86(5) yes C21 . Mo1 . C23 . 63.42(6) yes P1 . Mo1 . C23 5_656 153.44(4) yes P1 5_656 Mo1 . C23 5_656 96.77(4) yes O1 . Mo1 . C23 5_656 85.86(5) yes O1 5_656 Mo1 . C23 5_656 124.51(5) yes C21 . Mo1 . C23 5_656 35.09(6) yes C21 5_656 Mo1 . C22 . 63.31(6) yes C21 5_656 Mo1 . C22 5_656 35.09(6) yes C22 . Mo1 . C22 5_656 77.05(9) yes C21 5_656 Mo1 . C23 . 35.09(6) yes C22 . Mo1 . C23 . 36.78(6) yes C22 5_656 Mo1 . C23 . 65.07(6) yes C21 5_656 Mo1 . C23 5_656 63.42(6) yes C22 . Mo1 . C23 5_656 65.07(6) yes C22 5_656 Mo1 . C23 5_656 36.78(6) yes C23 . Mo1 . C23 5_656 77.25(8) yes Mo1 . P1 . C1 . 123.08(4) yes Mo1 . P1 . C7 . 114.50(5) yes C1 . P1 . C7 . 102.65(6) yes Mo1 . P1 . C13 . 100.87(5) yes C1 . P1 . C13 . 105.83(7) yes C7 . P1 . C13 . 109.18(7) yes Mo1 . O1 . C14 . 123.06(8) yes P1 . C1 . C2 . 119.54(12) yes P1 . C1 . C6 . 121.61(11) yes C2 . C1 . C6 . 118.75(14) yes C1 . C2 . C3 . 120.89(16) yes C1 . C2 . H21 . 119.55 no C3 . C2 . H21 . 119.55 no C2 . C3 . C4 . 119.96(16) yes C2 . C3 . H31 . 120.02 no C4 . C3 . H31 . 120.02 no C3 . C4 . C5 . 119.93(16) yes C3 . C4 . H41 . 120.03 no C5 . C4 . H41 . 120.03 no C4 . C5 . C6 . 120.34(17) yes C4 . C5 . H51 . 119.83 no C6 . C5 . H51 . 119.83 no C1 . C6 . C5 . 120.07(15) yes C1 . C6 . H61 . 119.97 no C5 . C6 . H61 . 119.96 no P1 . C7 . C8 . 119.12(11) yes P1 . C7 . C12 . 121.79(12) yes C8 . C7 . C12 . 118.98(14) yes C7 . C8 . C9 . 120.51(16) yes C7 . C8 . H81 . 119.74 no C9 . C8 . H81 . 119.74 no C8 . C9 . C10 . 120.04(17) yes C8 . C9 . H91 . 119.98 no C10 . C9 . H91 . 119.98 no C9 . C10 . C11 . 119.70(16) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 120.35(18) yes C10 . C11 . H111 . 119.82 no C12 . C11 . H111 . 119.8 no C7 . C12 . C11 . 120.39(17) yes C7 . C12 . H121 . 119.81 no C11 . C12 . H121 . 119.81 no P1 . C13 . C14 . 113.4(1) yes P1 . C13 . H131 . 123.31 no C14 . C13 . H131 . 123.31 no O1 . C14 . C13 . 122.59(12) yes O1 . C14 . C15 . 113.76(12) yes C13 . C14 . C15 . 123.62(13) yes C14 . C15 . C16 . 122.30(13) yes C14 . C15 . C20 . 119.33(13) yes C16 . C15 . C20 . 118.37(13) yes C15 . C16 . C17 . 120.66(15) yes C15 . C16 . H161 . 119.67 no C17 . C16 . H161 . 119.67 no C16 . C17 . C18 . 120.43(16) yes C16 . C17 . H171 . 119.79 no C18 . C17 . H171 . 119.79 no C17 . C18 . C19 . 119.56(15) yes C17 . C18 . H181 . 120.22 no C19 . C18 . H181 . 120.22 no C18 . C19 . C20 . 120.35(16) yes C18 . C19 . H191 . 119.83 no C20 . C19 . H191 . 119.83 no C15 . C20 . C19 . 120.63(16) yes C15 . C20 . H201 . 119.68 no C19 . C20 . H201 . 119.68 no Mo1 . C21 . C22 . 69.26(8) yes Mo1 . C21 . C23 5_656 68.79(8) yes C22 . C21 . C23 5_656 121.77(15) yes Mo1 . C21 . H211 . 137.36 no C22 . C21 . H211 . 119.11 no C23 5_656 C21 . H211 . 119.11 no Mo1 . C22 . C21 . 75.65(9) yes Mo1 . C22 . C23 . 71.16(8) yes C21 . C22 . C23 . 118.30(15) yes Mo1 . C22 . H221 . 123.81 no C21 . C22 . H221 . 120.85 no C23 . C22 . H221 . 120.85 no Mo1 . C23 . C21 5_656 76.12(9) yes Mo1 . C23 . C22 . 72.06(8) yes C21 5_656 C23 . C22 . 118.65(15) yes Mo1 . C23 . H231 . 122.48 no C21 5_656 C23 . H231 . 120.67 no C22 . C23 . H231 . 120.67 no #==END data_3b _database_code_CSD 168491 #============= Material Relevant to Compound(3b)===================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 12.5120(3) _cell_angle_alpha 90 _cell_length_b 14.7700(3) _cell_angle_beta 95.413(1) _cell_length_c 20.2580(3) _cell_angle_gamma 90 _cell_volume 3727.0 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C47 H39 Mo1 O2 P2 ' _chemical_formula_moiety ' C47 H39 Mo1 O2 P2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 793.71 _cell_measurement_reflns_used 29614 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 190 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' navye ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1629.521 _exptl_absorpt_coefficient_mu 0.478 # Sheldrick geometric definitions 0.83 0.91 _diffrn_measurement_device_type ; Unknown ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DATA COLLECTION ; _computing_data_reduction ; SPARE ; _computing_cell_refinement ; SPARE ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.91 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 190 _diffrn_reflns_number 29614 _reflns_number_total 7628 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 7628 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7685 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_gt 6718 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.53 _refine_diff_density_max 0.64 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6718 _refine_ls_number_parameters 479 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0320 _refine_ls_goodness_of_fit_ref 1.0579 _refine_ls_shift/su_max 0.005722 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 1.49 0.189 1.38 0.187E-010.288 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Spare Spare Spare Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Mo1 0.505013(14) 0.402875(11) 0.245890(8) 0.0175 1.0000 Uani P2 0.39820(4) 0.29560(4) 0.17446(2) 0.0199 1.0000 Uani C3 0.34584(17) 0.33932(14) 0.09304(9) 0.0227 1.0000 Uani C4 0.41665(19) 0.37219(18) 0.05010(11) 0.0348 1.0000 Uani C5 0.3784(2) 0.4083(2) -0.01103(12) 0.0451 1.0000 Uani C6 0.2691(2) 0.41397(19) -0.02901(11) 0.0423 1.0000 Uani C7 0.1983(2) 0.38259(19) 0.01383(13) 0.0423 1.0000 Uani C8 0.23583(18) 0.34484(17) 0.07434(11) 0.0315 1.0000 Uani C9 0.44755(18) 0.18350(15) 0.1524(1) 0.0271 1.0000 Uani C10 0.5340(2) 0.17366(17) 0.11458(12) 0.0372 1.0000 Uani C11 0.5703(3) 0.0876(2) 0.09942(16) 0.0561 1.0000 Uani C12 0.5204(3) 0.0117(2) 0.12040(18) 0.0600 1.0000 Uani C13 0.4364(3) 0.02024(18) 0.15883(17) 0.0540 1.0000 Uani C14 0.3998(2) 0.10568(17) 0.17516(13) 0.0396 1.0000 Uani C15 0.28749(16) 0.27679(15) 0.2209(1) 0.0253 1.0000 Uani C16 0.30109(16) 0.31095(14) 0.28341(9) 0.0225 1.0000 Uani O17 0.38772(11) 0.3559(1) 0.30659(6) 0.0228 1.0000 Uani C18 0.21953(17) 0.29936(14) 0.3322(1) 0.0250 1.0000 Uani C19 0.1163(2) 0.26723(18) 0.31338(14) 0.0414 1.0000 Uani C20 0.0434(2) 0.2550(2) 0.36024(17) 0.0510 1.0000 Uani C21 0.0711(2) 0.2757(2) 0.42583(15) 0.0502 1.0000 Uani C22 0.1716(2) 0.3074(3) 0.44447(14) 0.0647 1.0000 Uani C23 0.2457(2) 0.3200(2) 0.39835(12) 0.0500 1.0000 Uani P24 0.61333(4) 0.29392(4) 0.31401(2) 0.0193 1.0000 Uani C25 0.57121(17) 0.17764(15) 0.3294(1) 0.0249 1.0000 Uani C26 0.4941(2) 0.15834(17) 0.37239(11) 0.0332 1.0000 Uani C27 0.4642(2) 0.0692(2) 0.38242(13) 0.0449 1.0000 Uani C28 0.5077(2) -0.00093(18) 0.34901(14) 0.0455 1.0000 Uani C29 0.5824(2) 0.01726(17) 0.30491(13) 0.0425 1.0000 Uani C30 0.61367(19) 0.10616(16) 0.29499(11) 0.0333 1.0000 Uani C31 0.72711(16) 0.28330(16) 0.2682(1) 0.0262 1.0000 Uani C32 0.71036(16) 0.31703(14) 0.2058(1) 0.0219 1.0000 Uani O33 0.62232(11) 0.3605(1) 0.18375(6) 0.0222 1.0000 Uani C34 0.78920(17) 0.30540(14) 0.1550(1) 0.0237 1.0000 Uani C35 0.76807(18) 0.34566(18) 0.09284(11) 0.0326 1.0000 Uani C36 0.8383(2) 0.3351(2) 0.04405(11) 0.0411 1.0000 Uani C37 0.9304(2) 0.28326(18) 0.05673(12) 0.0393 1.0000 Uani C38 0.9522(2) 0.24332(17) 0.11774(13) 0.0388 1.0000 Uani C39 0.88249(19) 0.25439(16) 0.16705(12) 0.0325 1.0000 Uani C40 0.65580(17) 0.33401(14) 0.39796(9) 0.0229 1.0000 Uani C41 0.57831(18) 0.36612(16) 0.4371(1) 0.0292 1.0000 Uani C42 0.6076(2) 0.40084(18) 0.49988(11) 0.0363 1.0000 Uani C43 0.7147(2) 0.4047(2) 0.52418(11) 0.0431 1.0000 Uani C44 0.7924(2) 0.3726(2) 0.48580(12) 0.0426 1.0000 Uani C45 0.76346(18) 0.33700(18) 0.42308(11) 0.0329 1.0000 Uani C46 0.5206(2) 0.52051(16) 0.31779(11) 0.0387 1.0000 Uani C47 0.4178(2) 0.53212(16) 0.28495(13) 0.0386 1.0000 Uani C48 0.39859(19) 0.52766(15) 0.21590(13) 0.0332 1.0000 Uani C49 0.4901(2) 0.52583(15) 0.17847(11) 0.0325 1.0000 Uani C50 0.5939(2) 0.53390(16) 0.21137(13) 0.0352 1.0000 Uani C51 0.6118(2) 0.52404(16) 0.28111(13) 0.0385 1.0000 Uani C52 0.2889(3) 0.5377(2) 0.1842(2) 0.0439 0.772(5) Uani C152 0.7064(9) 0.5262(7) 0.3145(5) 0.0391 0.228(5) Uani H41 0.4957 0.3700 0.0632 0.0420 1.0000 Uiso H51 0.4302 0.4302 -0.0422 0.0543 1.0000 Uiso H61 0.2417 0.4406 -0.0727 0.0497 1.0000 Uiso H71 0.1192 0.3870 0.0012 0.0493 1.0000 Uiso H81 0.1837 0.3214 0.1047 0.0374 1.0000 Uiso H101 0.5702 0.2285 0.0982 0.0447 1.0000 Uiso H111 0.6334 0.0812 0.0730 0.0676 1.0000 Uiso H121 0.5452 -0.0497 0.1078 0.0712 1.0000 Uiso H131 0.4012 -0.0351 0.1752 0.0633 1.0000 Uiso H141 0.3388 0.1112 0.2034 0.0469 1.0000 Uiso H151 0.2211 0.2441 0.2029 0.0303 1.0000 Uiso H191 0.0946 0.2529 0.2658 0.0505 1.0000 Uiso H201 -0.0299 0.2308 0.3462 0.0631 1.0000 Uiso H211 0.0181 0.2676 0.4594 0.0621 1.0000 Uiso H221 0.1924 0.3219 0.4922 0.0784 1.0000 Uiso H231 0.3186 0.3443 0.4131 0.0602 1.0000 Uiso H261 0.4602 0.2086 0.3961 0.0398 1.0000 Uiso H271 0.4101 0.0558 0.4144 0.0540 1.0000 Uiso H281 0.4853 -0.0647 0.3567 0.0535 1.0000 Uiso H291 0.6139 -0.0332 0.2802 0.0502 1.0000 Uiso H301 0.6675 0.1192 0.2627 0.0398 1.0000 Uiso H311 0.7964 0.2553 0.2866 0.0316 1.0000 Uiso H351 0.7015 0.3826 0.0832 0.0393 1.0000 Uiso H361 0.8224 0.3649 -0.0001 0.0499 1.0000 Uiso H371 0.9806 0.2750 0.0216 0.0486 1.0000 Uiso H381 1.0186 0.2060 0.1269 0.0482 1.0000 Uiso H391 0.8998 0.2254 0.2114 0.0399 1.0000 Uiso H411 0.5008 0.3642 0.4198 0.0352 1.0000 Uiso H421 0.5511 0.4231 0.5277 0.0440 1.0000 Uiso H431 0.7358 0.4305 0.5692 0.0508 1.0000 Uiso H441 0.8699 0.3750 0.5033 0.0497 1.0000 Uiso H451 0.8201 0.3135 0.3959 0.0391 1.0000 Uiso H461 0.5296 0.5098 0.3667 0.0462 1.0000 Uiso H471 0.3561 0.5440 0.3118 0.0475 1.0000 Uiso H491 0.4803 0.5189 0.1292 0.0391 1.0000 Uiso H501 0.6559 0.5468 0.1851 0.0425 1.0000 Uiso H521 0.2895 0.5328 0.1350 0.0518 0.7721 Uiso H522 0.2599 0.5982 0.1957 0.0518 0.7721 Uiso H523 0.2424 0.4889 0.2004 0.0518 0.7721 Uiso H1521 0.7632 0.5285 0.2830 0.0460 0.2279 Uiso H1522 0.7120 0.5810 0.3436 0.0460 0.2279 Uiso H1523 0.7164 0.4705 0.3426 0.0460 0.2279 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02004(8) 0.01728(8) 0.01492(8) 0.00127(7) 0.00058(5) 0.00012(8) P2 0.0213(2) 0.0207(3) 0.0172(2) 0.00114(19) -0.00038(19) 0.0001(2) C3 0.026(1) 0.023(1) 0.0178(9) -0.0013(8) -0.0014(8) 0.0010(8) C4 0.0323(12) 0.0455(15) 0.0272(11) 0.005(1) 0.0061(9) 0.002(1) C5 0.0547(16) 0.0545(17) 0.0265(11) 0.0095(11) 0.0067(11) -0.0031(14) C6 0.0593(16) 0.0406(15) 0.024(1) 0.009(1) -0.010(1) -0.0021(13) C7 0.0383(13) 0.0456(16) 0.0395(13) 0.0111(11) -0.0142(11) -0.0028(12) C8 0.0302(12) 0.0339(13) 0.0294(11) 0.0061(9) -0.0030(9) -0.002(1) C9 0.0307(11) 0.0227(11) 0.026(1) -0.0030(8) -0.0089(9) 0.0018(9) C10 0.0395(13) 0.0317(13) 0.0405(13) -0.008(1) 0.0046(11) 0.004(1) C11 0.0571(18) 0.0466(18) 0.0655(18) -0.0175(15) 0.0101(15) 0.0145(14) C12 0.063(2) 0.0333(16) 0.082(2) -0.0140(15) -0.0036(17) 0.0137(14) C13 0.0586(19) 0.0226(13) 0.077(2) 0.0025(13) -0.0136(16) -0.0025(12) C14 0.0410(13) 0.0263(12) 0.0499(14) 0.0053(11) -0.0046(11) -0.0003(11) C15 0.022(1) 0.0296(11) 0.024(1) 0.0035(8) 0.0016(8) -0.0040(9) C16 0.021(1) 0.023(1) 0.0232(9) 0.0062(8) 0.0008(8) 0.0035(8) O17 0.0225(7) 0.0266(8) 0.0195(6) 0.0001(6) 0.0027(5) 0.0016(6) C18 0.023(1) 0.0232(11) 0.029(1) 0.0076(8) 0.0069(8) 0.0052(8) C19 0.0327(13) 0.0393(15) 0.0542(15) -0.0181(12) 0.0148(12) -0.0063(11) C20 0.0352(14) 0.0413(15) 0.081(2) -0.0149(15) 0.0299(14) -0.0088(12) C21 0.0385(14) 0.0557(18) 0.0611(17) 0.0215(14) 0.0299(13) 0.0146(13) C22 0.0367(15) 0.127(3) 0.0322(13) 0.0247(17) 0.0128(12) 0.0196(17) C23 0.0248(12) 0.099(3) 0.0266(11) 0.0115(13) 0.005(1) 0.0095(14) P24 0.0186(2) 0.0234(3) 0.0159(2) 0.00285(19) 0.00108(18) 0.0018(2) C25 0.025(1) 0.0272(11) 0.0206(9) 0.0046(8) -0.0050(8) 0.0013(9) C26 0.0373(12) 0.0346(13) 0.028(1) 0.0029(9) 0.0032(9) -0.008(1) C27 0.0502(15) 0.0470(16) 0.0378(13) 0.0055(11) 0.0058(12) -0.0156(13) C28 0.0574(17) 0.0302(14) 0.0461(14) 0.0105(11) -0.0088(13) -0.0074(13) C29 0.0523(16) 0.0275(13) 0.0457(14) 0.0031(11) -0.0061(12) 0.0085(11) C30 0.0350(12) 0.0277(12) 0.0369(11) 0.005(1) 0.0009(9) 0.007(1) C31 0.022(1) 0.0338(12) 0.0231(9) 0.0013(8) 0.0038(8) 0.0030(9) C32 0.022(1) 0.020(1) 0.0233(9) -0.0022(8) 0.0028(8) -0.0045(8) O33 0.0225(7) 0.0258(7) 0.0185(6) 0.0025(6) 0.0032(5) -0.0016(6) C34 0.026(1) 0.023(1) 0.0229(9) -0.0037(8) 0.0066(8) -0.0068(8) C35 0.0296(11) 0.0437(14) 0.025(1) -0.0004(9) 0.0050(9) -0.002(1) C36 0.0418(14) 0.0602(17) 0.023(1) 0.0021(11) 0.010(1) -0.0056(13) C37 0.0442(14) 0.0404(14) 0.0368(12) -0.0085(11) 0.0216(11) -0.0092(11) C38 0.0396(13) 0.0293(12) 0.0516(14) -0.0008(11) 0.0249(12) 0.001(1) C39 0.0343(12) 0.0268(11) 0.0388(12) 0.0044(9) 0.016(1) 0.0018(9) C40 0.027(1) 0.0240(11) 0.0172(9) 0.0047(8) 0.0001(8) -0.0008(8) C41 0.0305(11) 0.0343(12) 0.023(1) -0.0001(9) 0.0045(8) -0.0006(9) C42 0.0482(14) 0.0389(13) 0.023(1) -0.001(1) 0.0083(9) 0.0017(12) C43 0.0595(16) 0.0465(15) 0.021(1) -0.0031(11) -0.008(1) -0.0016(14) C44 0.0339(13) 0.0574(18) 0.0331(12) -0.0038(11) -0.015(1) -0.0001(12) C45 0.0252(11) 0.0427(14) 0.0299(11) -0.000(1) -0.0031(9) 0.002(1) C46 0.0664(18) 0.0215(12) 0.0276(11) -0.0051(9) 0.0004(11) 0.0033(11) C47 0.0554(16) 0.0193(11) 0.0441(13) -0.001(1) 0.0204(12) 0.0074(11) C48 0.0331(12) 0.0183(11) 0.0476(13) 0.0025(9) 0.001(1) 0.0069(9) C49 0.0462(14) 0.0236(11) 0.028(1) 0.0051(9) 0.004(1) -0.002(1) C50 0.0380(13) 0.0230(12) 0.0452(13) 0.000(1) 0.0074(11) -0.008(1) C51 0.0443(14) 0.0209(11) 0.0480(13) 0.003(1) -0.0079(11) -0.007(1) C52 0.0320(17) 0.0283(17) 0.069(2) -0.0077(15) -0.0065(16) 0.0097(13) C152 0.0443(17) 0.0215(15) 0.0491(16) 0.0042(13) -0.0074(14) -0.0074(14) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . P2 . 2.4548(6) yes Mo1 . O17 . 2.1182(13) yes Mo1 . P24 . 2.4450(5) yes Mo1 . O33 . 2.1163(13) yes Mo1 . C46 . 2.264(2) yes Mo1 . C47 . 2.372(2) yes Mo1 . C48 . 2.321(2) yes Mo1 . C49 . 2.269(2) yes Mo1 . C50 . 2.370(2) yes Mo1 . C51 . 2.306(2) yes P2 . C3 . 1.834(2) yes P2 . C9 . 1.837(2) yes P2 . C15 . 1.768(2) yes C3 . C4 . 1.387(3) yes C3 . C8 . 1.395(3) yes C4 . C5 . 1.391(3) yes C4 . H41 . 1.000(2) no C5 . C6 . 1.385(4) yes C5 . H51 . 1.000(2) no C6 . C7 . 1.378(4) yes C6 . H61 . 1.000(2) no C7 . C8 . 1.388(3) yes C7 . H71 . 1.000(3) no C8 . H81 . 1.000(2) no C9 . C10 . 1.391(3) yes C9 . C14 . 1.394(3) yes C10 . C11 . 1.393(4) yes C10 . H101 . 1.000(3) no C11 . C12 . 1.370(5) yes C11 . H111 . 1.000(3) no C12 . C13 . 1.372(5) yes C12 . H121 . 1.000(3) no C13 . C14 . 1.393(4) yes C13 . H131 . 1.000(3) no C14 . H141 . 1.000(3) no C15 . C16 . 1.359(3) yes C15 . H151 . 1.000(2) no C16 . O17 . 1.319(3) yes C16 . C18 . 1.496(3) yes C18 . C19 . 1.395(3) yes C18 . C23 . 1.383(3) yes C19 . C20 . 1.389(4) yes C19 . H191 . 1.000(3) no C20 . C21 . 1.376(5) yes C20 . H201 . 1.000(3) no C21 . C22 . 1.362(5) yes C21 . H211 . 1.000(2) no C22 . C23 . 1.389(3) yes C22 . H221 . 1.000(3) no C23 . H231 . 1.000(3) no P24 . C25 . 1.832(2) yes P24 . C31 . 1.777(2) yes P24 . C40 . 1.832(2) yes C25 . C26 . 1.389(3) yes C25 . C30 . 1.397(3) yes C26 . C27 . 1.389(4) yes C26 . H261 . 1.000(2) no C27 . C28 . 1.378(4) yes C27 . H271 . 1.000(3) no C28 . C29 . 1.379(4) yes C28 . H281 . 1.000(3) no C29 . C30 . 1.390(4) yes C29 . H291 . 1.000(3) no C30 . H301 . 1.000(2) no C31 . C32 . 1.358(3) yes C31 . H311 . 1.000(2) no C32 . O33 . 1.316(3) yes C32 . C34 . 1.500(3) yes C34 . C35 . 1.396(3) yes C34 . C39 . 1.391(3) yes C35 . C36 . 1.392(3) yes C35 . H351 . 1.000(2) no C36 . C37 . 1.386(4) yes C36 . H361 . 1.000(2) no C37 . C38 . 1.373(4) yes C37 . H371 . 1.000(2) no C38 . C39 . 1.396(3) yes C38 . H381 . 1.000(3) no C39 . H391 . 1.000(2) no C40 . C41 . 1.392(3) yes C40 . C45 . 1.395(3) yes C41 . C42 . 1.389(3) yes C41 . H411 . 1.000(2) no C42 . C43 . 1.384(4) yes C42 . H421 . 1.000(2) no C43 . C44 . 1.385(4) yes C43 . H431 . 1.000(2) no C44 . C45 . 1.391(3) yes C44 . H441 . 1.000(2) no C45 . H451 . 1.000(2) no C46 . C47 . 1.402(4) yes C46 . C51 . 1.421(4) yes C46 . H461 . 1.000(2) no C47 . C48 . 1.398(4) yes C47 . H471 . 1.000(2) no C48 . C49 . 1.432(3) yes C48 . C52 . 1.467(4) yes C49 . C50 . 1.408(4) yes C49 . H491 . 1.000(2) no C50 . C51 . 1.417(4) yes C50 . H501 . 1.000(2) no C51 . C152 . 1.308(12) yes C52 . H521 . 1.000(4) no C52 . H522 . 1.000(3) no C52 . H523 . 1.000(4) no C152 . H1521 . 1.00(1) no C152 . H1522 . 1.000(9) no C152 . H1523 . 1.000(11) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P2 . Mo1 . O17 . 76.26(4) yes P2 . Mo1 . P24 . 98.616(17) yes O17 . Mo1 . P24 . 80.47(4) yes P2 . Mo1 . O33 . 80.11(4) yes O17 . Mo1 . O33 . 143.71(5) yes P24 . Mo1 . O33 . 76.27(4) yes P2 . Mo1 . C46 . 152.09(8) yes O17 . Mo1 . C46 . 84.25(8) yes P24 . Mo1 . C46 . 97.62(7) yes O33 . Mo1 . C46 . 125.95(8) yes P2 . Mo1 . C47 . 118.30(7) yes O17 . Mo1 . C47 . 72.77(7) yes P24 . Mo1 . C47 . 126.13(7) yes O33 . Mo1 . C47 . 143.43(7) yes C46 . Mo1 . C47 . 35.1(1) yes P2 . Mo1 . C48 . 95.24(6) yes O17 . Mo1 . C48 . 90.00(7) yes P24 . Mo1 . C48 . 160.77(6) yes O33 . Mo1 . C48 . 119.46(7) yes C46 . Mo1 . C48 . 64.62(9) yes P2 . Mo1 . C49 . 98.77(6) yes O17 . Mo1 . C49 . 126.09(7) yes P24 . Mo1 . C49 . 151.19(7) yes O33 . Mo1 . C49 . 84.31(7) yes C46 . Mo1 . C49 . 76.72(8) yes P2 . Mo1 . C50 . 126.70(6) yes O17 . Mo1 . C50 . 143.95(7) yes P24 . Mo1 . C50 . 116.97(7) yes O33 . Mo1 . C50 . 72.22(7) yes C46 . Mo1 . C50 . 63.18(9) yes P2 . Mo1 . C51 . 161.94(7) yes O17 . Mo1 . C51 . 119.17(8) yes P24 . Mo1 . C51 . 93.56(7) yes O33 . Mo1 . C51 . 89.95(8) yes C46 . Mo1 . C51 . 36.2(1) yes C47 . Mo1 . C48 . 34.65(9) yes C47 . Mo1 . C49 . 62.76(8) yes C48 . Mo1 . C49 . 36.32(8) yes C47 . Mo1 . C50 . 71.62(8) yes C48 . Mo1 . C50 . 63.12(9) yes C49 . Mo1 . C50 . 35.25(9) yes C47 . Mo1 . C51 . 62.8(1) yes C48 . Mo1 . C51 . 76.47(8) yes C49 . Mo1 . C51 . 65.01(9) yes C50 . Mo1 . C51 . 35.24(9) yes Mo1 . P2 . C3 . 115.55(7) yes Mo1 . P2 . C9 . 123.26(7) yes C3 . P2 . C9 . 101.45(9) yes Mo1 . P2 . C15 . 101.41(7) yes C3 . P2 . C15 . 107.6(1) yes C9 . P2 . C15 . 106.62(11) yes P2 . C3 . C4 . 119.50(17) yes P2 . C3 . C8 . 121.63(16) yes C4 . C3 . C8 . 118.8(2) yes C3 . C4 . C5 . 120.4(2) yes C3 . C4 . H41 . 119.8(2) no C5 . C4 . H41 . 119.8(2) no C4 . C5 . C6 . 120.4(2) yes C4 . C5 . H51 . 119.8(3) no C6 . C5 . H51 . 119.8(2) no C5 . C6 . C7 . 119.5(2) yes C5 . C6 . H61 . 120.3(3) no C7 . C6 . H61 . 120.3(3) no C6 . C7 . C8 . 120.5(2) yes C6 . C7 . H71 . 119.8(2) no C8 . C7 . H71 . 119.8(2) no C3 . C8 . C7 . 120.4(2) yes C3 . C8 . H81 . 119.8(2) no C7 . C8 . H81 . 119.8(2) no P2 . C9 . C10 . 121.66(18) yes P2 . C9 . C14 . 119.90(18) yes C10 . C9 . C14 . 118.4(2) yes C9 . C10 . C11 . 120.2(3) yes C9 . C10 . H101 . 119.9(2) no C11 . C10 . H101 . 119.9(2) no C10 . C11 . C12 . 120.7(3) yes C10 . C11 . H111 . 119.7(3) no C12 . C11 . H111 . 119.7(3) no C11 . C12 . C13 . 119.8(3) yes C11 . C12 . H121 . 120.1(3) no C13 . C12 . H121 . 120.1(3) no C12 . C13 . C14 . 120.3(3) yes C12 . C13 . H131 . 119.9(3) no C14 . C13 . H131 . 119.9(3) no C9 . C14 . C13 . 120.5(2) yes C9 . C14 . H141 . 119.7(2) no C13 . C14 . H141 . 119.7(3) no P2 . C15 . C16 . 113.70(16) yes P2 . C15 . H151 . 123.15(16) no C16 . C15 . H151 . 123.15(19) no C15 . C16 . O17 . 123.04(17) yes C15 . C16 . C18 . 122.67(19) yes O17 . C16 . C18 . 114.28(17) yes Mo1 . O17 . C16 . 123.30(12) yes C16 . C18 . C19 . 122.0(2) yes C16 . C18 . C23 . 120.1(2) yes C19 . C18 . C23 . 117.9(2) yes C18 . C19 . C20 . 120.6(3) yes C18 . C19 . H191 . 119.7(2) no C20 . C19 . H191 . 119.7(3) no C19 . C20 . C21 . 120.6(3) yes C19 . C20 . H201 . 119.7(3) no C21 . C20 . H201 . 119.7(3) no C20 . C21 . C22 . 119.1(2) yes C20 . C21 . H211 . 120.5(3) no C22 . C21 . H211 . 120.5(3) no C21 . C22 . C23 . 121.1(3) yes C21 . C22 . H221 . 119.4(3) no C23 . C22 . H221 . 119.4(3) no C18 . C23 . C22 . 120.7(3) yes C18 . C23 . H231 . 119.7(2) no C22 . C23 . H231 . 119.7(3) no Mo1 . P24 . C25 . 124.05(7) yes Mo1 . P24 . C31 . 101.09(7) yes C25 . P24 . C31 . 105.3(1) yes Mo1 . P24 . C40 . 114.08(7) yes C25 . P24 . C40 . 102.02(9) yes C31 . P24 . C40 . 109.7(1) yes P24 . C25 . C26 . 121.80(17) yes P24 . C25 . C30 . 119.66(16) yes C26 . C25 . C30 . 118.5(2) yes C25 . C26 . C27 . 120.0(2) yes C25 . C26 . H261 . 120.0(2) no C27 . C26 . H261 . 120.0(2) no C26 . C27 . C28 . 121.1(2) yes C26 . C27 . H271 . 119.5(3) no C28 . C27 . H271 . 119.5(3) no C27 . C28 . C29 . 119.7(2) yes C27 . C28 . H281 . 120.1(3) no C29 . C28 . H281 . 120.1(3) no C28 . C29 . C30 . 119.7(2) yes C28 . C29 . H291 . 120.2(3) no C30 . C29 . H291 . 120.2(3) no C25 . C30 . C29 . 121.1(2) yes C25 . C30 . H301 . 119.5(2) no C29 . C30 . H301 . 119.5(2) no P24 . C31 . C32 . 113.14(16) yes P24 . C31 . H311 . 123.43(16) no C32 . C31 . H311 . 123.43(19) no C31 . C32 . O33 . 123.07(18) yes C31 . C32 . C34 . 122.88(19) yes O33 . C32 . C34 . 114.03(17) yes Mo1 . O33 . C32 . 123.22(12) yes C32 . C34 . C35 . 119.3(2) yes C32 . C34 . C39 . 122.51(19) yes C35 . C34 . C39 . 118.21(19) yes C34 . C35 . C36 . 121.0(2) yes C34 . C35 . H351 . 119.5(2) no C36 . C35 . H351 . 119.5(2) no C35 . C36 . C37 . 120.0(2) yes C35 . C36 . H361 . 120.0(3) no C37 . C36 . H361 . 120.0(2) no C36 . C37 . C38 . 119.7(2) yes C36 . C37 . H371 . 120.2(3) no C38 . C37 . H371 . 120.2(3) no C37 . C38 . C39 . 120.6(2) yes C37 . C38 . H381 . 119.7(2) no C39 . C38 . H381 . 119.7(3) no C34 . C39 . C38 . 120.6(2) yes C34 . C39 . H391 . 119.71(19) no C38 . C39 . H391 . 119.7(2) no P24 . C40 . C41 . 118.82(16) yes P24 . C40 . C45 . 122.31(16) yes C41 . C40 . C45 . 118.81(19) yes C40 . C41 . C42 . 120.6(2) yes C40 . C41 . H411 . 119.7(2) no C42 . C41 . H411 . 119.7(2) no C41 . C42 . C43 . 120.3(2) yes C41 . C42 . H421 . 119.9(2) no C43 . C42 . H421 . 119.9(2) no C42 . C43 . C44 . 119.6(2) yes C42 . C43 . H431 . 120.2(3) no C44 . C43 . H431 . 120.2(3) no C43 . C44 . C45 . 120.4(2) yes C43 . C44 . H441 . 119.8(2) no C45 . C44 . H441 . 119.8(3) no C40 . C45 . C44 . 120.3(2) yes C40 . C45 . H451 . 119.8(2) no C44 . C45 . H451 . 119.8(2) no Mo1 . C46 . C47 . 76.66(14) yes Mo1 . C46 . C51 . 73.51(13) yes C47 . C46 . C51 . 119.6(2) yes Mo1 . C46 . H461 . 120.77(18) no C47 . C46 . H461 . 120.2(3) no C51 . C46 . H461 . 120.2(3) no Mo1 . C47 . C46 . 68.23(13) yes Mo1 . C47 . C48 . 70.68(13) yes C46 . C47 . C48 . 122.1(2) yes Mo1 . C47 . H471 . 136.49(18) no C46 . C47 . H471 . 118.9(2) no C48 . C47 . H471 . 118.9(3) no Mo1 . C48 . C47 . 74.67(14) yes Mo1 . C48 . C49 . 69.88(13) yes C47 . C48 . C49 . 117.4(2) yes Mo1 . C48 . C52 . 133.22(19) yes C47 . C48 . C52 . 119.9(3) yes C49 . C48 . C52 . 122.2(3) yes Mo1 . C49 . C48 . 73.79(13) yes Mo1 . C49 . C50 . 76.28(14) yes C48 . C49 . C50 . 119.7(2) yes Mo1 . C49 . H491 . 120.93(17) no C48 . C49 . H491 . 120.1(2) no C50 . C49 . H491 . 120.1(2) no Mo1 . C50 . C49 . 68.47(13) yes Mo1 . C50 . C51 . 69.90(13) yes C49 . C50 . C51 . 121.0(2) yes Mo1 . C50 . H501 . 136.21(19) no C49 . C50 . H501 . 119.5(2) no C51 . C50 . H501 . 119.5(3) no Mo1 . C51 . C46 . 70.29(14) yes Mo1 . C51 . C50 . 74.86(14) yes C46 . C51 . C50 . 117.8(2) yes Mo1 . C51 . C152 . 130.4(5) yes C46 . C51 . C152 . 117.6(4) yes C50 . C51 . C152 . 124.4(5) yes C48 . C52 . H521 . 109.5(3) no C48 . C52 . H522 . 109.5(3) no H521 . C52 . H522 . 109.5(3) no C48 . C52 . H523 . 109.5(3) no H521 . C52 . H523 . 109.5(3) no H522 . C52 . H523 . 109.5(3) no C51 . C152 . H1521 . 109.5(8) no C51 . C152 . H1522 . 109.5(8) no H1521 . C152 . H1522 . 109.5(10) no C51 . C152 . H1523 . 109.5(9) no H1521 . C152 . H1523 . 109.5(9) no H1522 . C152 . H1523 . 109.5(9) no #==END data_6 _database_code_CSD 168492 #============= Material Relevant to Compound(6)===================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** #============================================================= _cell_length_a 11.0924(2) _cell_angle_alpha 90 _cell_length_b 21.8354(4) _cell_angle_beta 102.7274(8) _cell_length_c 14.7699(3) _cell_angle_gamma 90 _cell_volume 3489.5 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C36.50 H37 Cl1 F6 Mo1 N1 O1 P2 ' _chemical_formula_moiety ' C36.50 H37 Cl1 F6 Mo1 N1 O1 P2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 813.03 _cell_measurement_reflns_used 7494 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1650.286 _exptl_absorpt_coefficient_mu 0.608 # Sheldrick geometric definitions 0.93 0.98 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.98 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 14831 _reflns_number_total 7947 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 7947 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8006 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_gt 5979 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -0.76 _refine_diff_density_max 1.10 _reflns_threshold_expression >2.00\s(I) _refine_ls_number_reflns 5979 _refine_ls_number_parameters 451 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0516 _refine_ls_goodness_of_fit_ref 1.1201 _refine_ls_shift/su_max 0.000934 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.966 0.447 0.689 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Mo1 0.87390(2) 0.150651(11) 0.897696(17) 0.0209 1.0000 Uani N1 0.6165(2) 0.29089(12) 0.94900(19) 0.0271 1.0000 Uani O1 0.78036(19) 0.23124(9) 0.94302(15) 0.0247 1.0000 Uani P1 0.65927(6) 0.14485(3) 0.80784(5) 0.0198 1.0000 Uani P2 0.80116(9) 0.37958(4) 0.72477(6) 0.0337 1.0000 Uani F1 0.6877(3) 0.33754(17) 0.6813(3) 0.0874 1.0000 Uani F2 0.8195(3) 0.33827(12) 0.81567(18) 0.0595 1.0000 Uani F3 0.8884(4) 0.33608(16) 0.6841(3) 0.0874 1.0000 Uani F4 0.9162(4) 0.42061(17) 0.7695(3) 0.0995 1.0000 Uani F5 0.7151(4) 0.42323(16) 0.7659(3) 0.0999 1.0000 Uani F6 0.7806(3) 0.42003(11) 0.63339(16) 0.0513 1.0000 Uani C1 0.6742(3) 0.24974(13) 0.9055(2) 0.0234 1.0000 Uani C2 0.6099(3) 0.22528(13) 0.8124(2) 0.0234 1.0000 Uani C3 0.6726(3) 0.31089(15) 1.0424(2) 0.0291 1.0000 Uani C4 0.6874(3) 0.27074(19) 1.1153(3) 0.0397 1.0000 Uani C5 0.7309(4) 0.2927(2) 1.2063(3) 0.0503 1.0000 Uani C6 0.7583(4) 0.3538(2) 1.2204(3) 0.0517 1.0000 Uani C7 0.7453(4) 0.3933(2) 1.1463(3) 0.0539 1.0000 Uani C8 0.7026(3) 0.37211(18) 1.0568(3) 0.0417 1.0000 Uani C9 0.4942(3) 0.31528(14) 0.9094(2) 0.0280 1.0000 Uani C10 0.4018(3) 0.30607(18) 0.9584(3) 0.0398 1.0000 Uani C11 0.2851(4) 0.3296(2) 0.9243(3) 0.0508 1.0000 Uani C12 0.2608(4) 0.3628(2) 0.8417(3) 0.0513 1.0000 Uani C13 0.3535(4) 0.37200(19) 0.7940(3) 0.0472 1.0000 Uani C14 0.4721(3) 0.34845(16) 0.8282(3) 0.0375 1.0000 Uani C15 0.6169(3) 0.12693(14) 0.6848(2) 0.0258 1.0000 Uani C16 0.6580(3) 0.07145(15) 0.6544(2) 0.0316 1.0000 Uani C17 0.6191(4) 0.05379(19) 0.5627(3) 0.0435 1.0000 Uani C18 0.5383(4) 0.0907(2) 0.5000(3) 0.0437 1.0000 Uani C19 0.4981(3) 0.14554(19) 0.5291(2) 0.0394 1.0000 Uani C20 0.5366(3) 0.16373(16) 0.6205(2) 0.0315 1.0000 Uani C21 0.5433(3) 0.10303(14) 0.8544(2) 0.0231 1.0000 Uani C22 0.5060(3) 0.04450(14) 0.8242(2) 0.0297 1.0000 Uani C23 0.4216(3) 0.01281(15) 0.8643(3) 0.0358 1.0000 Uani C24 0.3743(3) 0.03933(18) 0.9337(3) 0.0382 1.0000 Uani C25 0.4110(3) 0.09756(17) 0.9648(2) 0.0342 1.0000 Uani C26 0.4958(3) 0.12935(16) 0.9257(2) 0.0293 1.0000 Uani C27 0.8352(3) 0.05618(15) 0.9447(2) 0.0307 1.0000 Uani C28 0.8091(3) 0.10149(15) 1.0081(2) 0.0296 1.0000 Uani C29 0.9105(3) 0.13712(17) 1.0532(2) 0.0338 1.0000 Uani C30 0.9410(3) 0.13161(16) 0.7641(2) 0.0307 1.0000 Uani C31 0.9301(3) 0.19685(15) 0.7751(2) 0.0321 1.0000 Uani C32 1.0051(3) 0.22466(15) 0.8527(3) 0.0342 1.0000 Uani C33 1.0717(3) 0.18965(18) 0.9262(3) 0.0382 1.0000 Uani C34 1.0741(3) 0.12394(17) 0.9168(3) 0.0341 1.0000 Uani C35 1.0206(3) 0.09642(16) 0.8317(3) 0.0349 1.0000 Uani C36 1.0390(4) 0.0293(2) 0.8155(4) 0.0528 1.0000 Uani C100 0.5403(9) 0.5162(5) 0.0235(6) 0.0766 0.5000 Uani Cl1 0.4157(4) 0.47296(18) 0.0412(3) 0.0821 0.5000 Uani Cl2 0.5641(4) 0.50282(18) -0.0876(3) 0.0865 0.5000 Uani H21 0.6346 0.2496 0.7621 0.0287 1.0000 Uiso H22 0.5185 0.2276 0.8056 0.0287 1.0000 Uiso H41 0.6678 0.2261 1.1034 0.0480 1.0000 Uiso H51 0.7411 0.2634 1.2606 0.0587 1.0000 Uiso H61 0.7888 0.3699 1.2852 0.0609 1.0000 Uiso H71 0.7666 0.4379 1.1564 0.0611 1.0000 Uiso H81 0.6945 0.4008 1.0026 0.0484 1.0000 Uiso H101 0.4201 0.2823 1.0179 0.0483 1.0000 Uiso H111 0.2175 0.3229 0.9582 0.0611 1.0000 Uiso H121 0.1764 0.3801 0.8175 0.0606 1.0000 Uiso H131 0.3361 0.3961 0.7345 0.0538 1.0000 Uiso H141 0.5405 0.3561 0.7950 0.0445 1.0000 Uiso H161 0.7162 0.0445 0.6993 0.0389 1.0000 Uiso H171 0.6498 0.0141 0.5408 0.0528 1.0000 Uiso H181 0.5096 0.0778 0.4336 0.0531 1.0000 Uiso H191 0.4396 0.1720 0.4836 0.0475 1.0000 Uiso H201 0.5067 0.2037 0.6412 0.0386 1.0000 Uiso H221 0.5397 0.0248 0.7732 0.0348 1.0000 Uiso H231 0.3952 -0.0296 0.8428 0.0423 1.0000 Uiso H241 0.3123 0.0166 0.9613 0.0450 1.0000 Uiso H251 0.3767 0.1167 1.0149 0.0414 1.0000 Uiso H261 0.5228 0.1715 0.9484 0.0364 1.0000 Uiso H271 0.9208 0.0514 0.9347 0.0368 1.0000 Uiso H272 0.7672 0.0290 0.9106 0.0368 1.0000 Uiso H281 0.7244 0.1075 1.0200 0.0352 1.0000 Uiso H291 0.8995 0.1698 1.0981 0.0409 1.0000 Uiso H292 0.9941 0.1301 1.0396 0.0409 1.0000 Uiso H301 0.8911 0.1110 0.7072 0.0373 1.0000 Uiso H311 0.8697 0.2219 0.7281 0.0402 1.0000 Uiso H321 1.0127 0.2704 0.8561 0.0425 1.0000 Uiso H331 1.1164 0.2102 0.9852 0.0443 1.0000 Uiso H341 1.1140 0.0978 0.9709 0.0411 1.0000 Uiso H361 1.0979 0.0111 0.8699 0.0690 1.0000 Uiso H362 1.0734 0.0239 0.7584 0.0690 1.0000 Uiso H363 0.9578 0.0072 0.8060 0.0690 1.0000 Uiso H1001 0.5259 0.5611 0.0318 0.1422 1.0000 Uiso H1002 0.6187 0.5044 0.0713 0.1422 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01645(13) 0.02100(13) 0.02517(14) 0.0005(1) 0.00409(8) -0.00003(9) N1 0.0210(12) 0.0278(12) 0.0315(13) -0.005(1) 0.004(1) 0.004(1) O1 0.021(1) 0.025(1) 0.028(1) -0.0040(8) 0.0050(8) -0.0002(8) P1 0.0186(3) 0.0203(3) 0.0208(3) -0.0009(3) 0.0045(2) -0.0009(2) P2 0.0368(5) 0.0312(4) 0.0332(4) 0.0106(3) 0.0077(3) 0.0012(3) F1 0.078(2) 0.091(2) 0.076(2) 0.0326(18) -0.0207(17) -0.0395(18) F2 0.0738(18) 0.0535(14) 0.0451(13) 0.0257(11) -0.0000(12) -0.0089(12) F3 0.099(2) 0.0735(19) 0.107(3) 0.0395(19) 0.061(2) 0.0447(18) F4 0.114(3) 0.093(2) 0.073(2) 0.0301(19) -0.0207(19) -0.060(2) F5 0.146(3) 0.070(2) 0.113(3) 0.0333(19) 0.091(3) 0.047(2) F6 0.0708(16) 0.0450(12) 0.0404(12) 0.018(1) 0.0171(11) 0.0103(11) C1 0.0235(14) 0.0219(13) 0.0246(13) 0.0007(11) 0.0048(11) -0.0019(11) C2 0.0233(13) 0.0223(13) 0.0241(13) -0.0015(11) 0.0038(11) -0.0005(11) C3 0.0191(13) 0.0373(16) 0.0308(16) -0.0111(13) 0.0054(11) -0.0000(12) C4 0.0362(19) 0.048(2) 0.0348(17) -0.0068(15) 0.0088(14) 0.0018(15) C5 0.039(2) 0.079(3) 0.0323(19) -0.0053(19) 0.0075(15) 0.005(2) C6 0.0307(18) 0.079(3) 0.042(2) -0.031(2) 0.0009(15) 0.0060(19) C7 0.038(2) 0.054(2) 0.062(3) -0.030(2) -0.0060(18) 0.0046(17) C8 0.0301(17) 0.0376(18) 0.053(2) -0.0159(17) -0.0015(15) 0.0037(14) C9 0.0243(14) 0.0260(14) 0.0318(16) -0.0086(12) 0.0022(12) 0.0047(12) C10 0.0310(17) 0.0439(19) 0.046(2) -0.0066(16) 0.0124(15) 0.0067(15) C11 0.035(2) 0.060(2) 0.060(3) -0.011(2) 0.0145(18) 0.0078(18) C12 0.0342(19) 0.053(2) 0.061(3) -0.013(2) -0.0017(18) 0.0176(17) C13 0.045(2) 0.043(2) 0.048(2) -0.0004(17) -0.0012(17) 0.0187(17) C14 0.0344(17) 0.0322(16) 0.0445(19) -0.0033(15) 0.0056(14) 0.0071(14) C15 0.0240(14) 0.0302(14) 0.0244(14) -0.0056(12) 0.0082(11) -0.0077(12) C16 0.0320(16) 0.0281(15) 0.0355(17) -0.0065(13) 0.0090(13) -0.0046(12) C17 0.044(2) 0.044(2) 0.046(2) -0.0183(17) 0.0184(16) -0.0135(16) C18 0.042(2) 0.060(2) 0.0291(17) -0.0087(16) 0.0085(15) -0.0225(18) C19 0.0330(17) 0.057(2) 0.0269(16) 0.0043(15) 0.0044(13) -0.0124(16) C20 0.0277(15) 0.0407(17) 0.0268(15) 0.0033(13) 0.0074(12) -0.0014(13) C21 0.0171(12) 0.0273(14) 0.0235(13) 0.0043(11) 0.001(1) 0.0010(11) C22 0.0282(15) 0.0260(14) 0.0341(16) 0.0039(12) 0.0050(12) -0.0012(12) C23 0.0289(16) 0.0280(16) 0.049(2) 0.0125(14) 0.0049(14) -0.0045(12) C24 0.0254(15) 0.047(2) 0.0416(18) 0.0188(16) 0.0069(13) 0.0002(14) C25 0.0275(15) 0.0447(19) 0.0324(16) 0.0097(14) 0.0114(13) 0.0028(14) C26 0.0244(14) 0.0370(16) 0.0268(14) 0.0023(13) 0.0061(11) -0.0016(12) C27 0.0274(15) 0.0273(15) 0.0372(17) 0.0113(13) 0.0063(12) 0.0005(12) C28 0.0270(15) 0.0341(16) 0.0277(15) 0.0119(13) 0.0060(12) 0.0030(12) C29 0.0275(16) 0.0440(19) 0.0283(15) 0.0061(13) 0.0023(12) 0.0026(13) C30 0.0270(15) 0.0339(15) 0.0336(16) -0.0020(13) 0.0116(13) 0.0018(12) C31 0.0299(15) 0.0320(16) 0.0377(17) 0.0063(13) 0.0144(13) 0.0007(13) C32 0.0302(16) 0.0269(15) 0.050(2) -0.0019(14) 0.0195(15) -0.0079(12) C33 0.0268(16) 0.0442(19) 0.044(2) -0.0048(16) 0.0090(14) -0.0143(14) C34 0.0208(15) 0.0411(18) 0.0400(18) 0.0083(15) 0.0062(13) 0.0056(13) C35 0.0300(16) 0.0316(16) 0.047(2) 0.0027(14) 0.0174(14) 0.0027(13) C36 0.052(2) 0.041(2) 0.072(3) 0.004(2) 0.028(2) 0.0115(18) C100 0.074(5) 0.053(5) 0.101(6) 0.008(5) 0.014(5) -0.002(4) Cl1 0.080(2) 0.070(2) 0.103(3) 0.0208(18) 0.036(2) 0.0029(17) Cl2 0.100(3) 0.067(2) 0.095(3) 0.0254(18) 0.027(2) -0.0071(19) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . O1 . 2.220(2) yes Mo1 . P1 . 2.4603(7) yes Mo1 . C27 . 2.248(3) yes Mo1 . C28 . 2.201(3) yes Mo1 . C29 . 2.263(3) yes Mo1 . C30 . 2.295(3) yes Mo1 . C31 . 2.276(3) yes Mo1 . C32 . 2.366(3) yes Mo1 . C33 . 2.304(3) yes Mo1 . C34 . 2.253(3) yes Mo1 . C35 . 2.388(3) yes N1 . C1 . 1.346(4) yes N1 . C3 . 1.451(4) yes N1 . C9 . 1.455(4) yes O1 . C1 . 1.253(4) yes P1 . C2 . 1.845(3) yes P1 . C15 . 1.817(3) yes P1 . C21 . 1.830(3) yes P2 . F1 . 1.576(3) yes P2 . F2 . 1.593(2) yes P2 . F3 . 1.567(3) yes P2 . F4 . 1.580(3) yes P2 . F5 . 1.563(3) yes P2 . F6 . 1.587(2) yes C1 . C2 . 1.501(4) yes C2 . H21 . 0.999 no C2 . H22 . 0.998 no C3 . C4 . 1.370(5) yes C3 . C8 . 1.383(5) yes C4 . C5 . 1.407(5) yes C4 . H41 . 1.006 no C5 . C6 . 1.374(7) yes C5 . H51 . 1.012 no C6 . C7 . 1.375(7) yes C6 . H61 . 1.007 no C7 . C8 . 1.382(6) yes C7 . H71 . 1.006 no C8 . H81 . 1.006 no C9 . C10 . 1.392(5) yes C9 . C14 . 1.377(5) yes C10 . C11 . 1.381(6) yes C10 . H101 . 1.003 no C11 . C12 . 1.394(7) yes C11 . H111 . 0.999 no C12 . C13 . 1.383(7) yes C12 . H121 . 1.000 no C13 . C14 . 1.399(5) yes C13 . H131 . 1.006 no C14 . H141 . 1.004 no C15 . C16 . 1.403(4) yes C15 . C20 . 1.402(5) yes C16 . C17 . 1.383(5) yes C16 . H161 . 1.007 no C17 . C18 . 1.395(6) yes C17 . H171 . 1.009 no C18 . C19 . 1.379(6) yes C18 . H181 . 1.002 no C19 . C20 . 1.383(5) yes C19 . H191 . 1.008 no C20 . H201 . 1.005 no C21 . C22 . 1.387(4) yes C21 . C26 . 1.400(4) yes C22 . C23 . 1.396(5) yes C22 . H221 . 1.007 no C23 . C24 . 1.379(6) yes C23 . H231 . 1.002 no C24 . C25 . 1.382(6) yes C24 . H241 . 1.003 no C25 . C26 . 1.393(4) yes C25 . H251 . 0.995 no C26 . H261 . 1.003 no C27 . C28 . 1.435(5) yes C27 . H271 . 0.998 no C27 . H272 . 1.003 no C28 . C29 . 1.409(5) yes C28 . H281 . 1.002 no C29 . H291 . 0.999 no C29 . H292 . 1.004 no C30 . C31 . 1.442(5) yes C30 . C35 . 1.406(5) yes C30 . H301 . 1.006 no C31 . C32 . 1.397(5) yes C31 . H311 . 1.013 no C32 . C33 . 1.399(5) yes C32 . H321 . 1.003 no C33 . C34 . 1.442(5) yes C33 . H331 . 1.008 no C34 . C35 . 1.401(5) yes C34 . H341 . 1.003 no C35 . C36 . 1.506(5) yes C36 . H361 . 1.000 no C36 . H362 . 1.006 no C36 . H363 . 1.004 no C100 . C100 2_665 1.226(17) yes C100 . Cl1 . 1.740(8) yes C100 . Cl1 2_665 1.189(9) yes C100 . Cl2 . 1.742(8) yes C100 . Cl2 2_665 1.70(1) yes C100 . H1001 . 1.01 no C100 . H1002 . 1.025 no Cl1 . Cl2 2_665 0.856(5) yes Cl1 . H1001 2_665 1.563 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Mo1 . P1 . 75.07(6) yes O1 . Mo1 . C27 . 120.0(1) yes P1 . Mo1 . C27 . 83.75(8) yes O1 . Mo1 . C28 . 85.0(1) yes P1 . Mo1 . C28 . 86.53(8) yes C27 . Mo1 . C28 . 37.63(13) yes O1 . Mo1 . C29 . 77.79(11) yes P1 . Mo1 . C29 . 118.48(9) yes C27 . Mo1 . C29 . 64.57(13) yes C28 . Mo1 . C29 . 36.76(12) yes O1 . Mo1 . C30 . 131.7(1) yes P1 . Mo1 . C30 . 89.18(9) yes C27 . Mo1 . C30 . 102.67(13) yes C28 . Mo1 . C30 . 140.30(13) yes C29 . Mo1 . C30 . 146.06(12) yes O1 . Mo1 . C31 . 96.7(1) yes P1 . Mo1 . C31 . 89.76(9) yes C27 . Mo1 . C31 . 139.18(13) yes C28 . Mo1 . C31 . 175.40(13) yes C29 . Mo1 . C31 . 147.80(13) yes O1 . Mo1 . C32 . 84.3(1) yes P1 . Mo1 . C32 . 117.75(9) yes C27 . Mo1 . C32 . 152.24(12) yes C28 . Mo1 . C32 . 149.63(13) yes C29 . Mo1 . C32 . 112.99(13) yes O1 . Mo1 . C33 . 98.14(11) yes P1 . Mo1 . C33 . 152.5(1) yes C27 . Mo1 . C33 . 121.46(13) yes C28 . Mo1 . C33 . 119.88(13) yes C29 . Mo1 . C33 . 84.96(13) yes O1 . Mo1 . C34 . 132.91(11) yes P1 . Mo1 . C34 . 149.8(1) yes C27 . Mo1 . C34 . 88.52(12) yes C28 . Mo1 . C34 . 104.77(12) yes C29 . Mo1 . C34 . 83.56(13) yes O1 . Mo1 . C35 . 157.3(1) yes P1 . Mo1 . C35 . 114.82(9) yes C27 . Mo1 . C35 . 82.23(12) yes C28 . Mo1 . C35 . 115.08(12) yes C29 . Mo1 . C35 . 111.34(13) yes C30 . Mo1 . C31 . 36.78(12) yes C30 . Mo1 . C32 . 63.01(12) yes C31 . Mo1 . C32 . 34.98(13) yes C30 . Mo1 . C33 . 75.39(13) yes C31 . Mo1 . C33 . 64.21(13) yes C32 . Mo1 . C33 . 34.82(13) yes C30 . Mo1 . C34 . 64.09(12) yes C31 . Mo1 . C34 . 77.24(12) yes C32 . Mo1 . C34 . 64.00(13) yes C33 . Mo1 . C34 . 36.88(14) yes C30 . Mo1 . C35 . 34.88(12) yes C31 . Mo1 . C35 . 64.18(12) yes C32 . Mo1 . C35 . 72.98(12) yes C33 . Mo1 . C35 . 63.29(13) yes C34 . Mo1 . C35 . 35.00(13) yes C1 . N1 . C3 . 120.4(2) yes C1 . N1 . C9 . 123.5(3) yes C3 . N1 . C9 . 116.0(2) yes Mo1 . O1 . C1 . 125.34(19) yes Mo1 . P1 . C2 . 101.03(9) yes Mo1 . P1 . C15 . 123.8(1) yes C2 . P1 . C15 . 103.18(14) yes Mo1 . P1 . C21 . 119.97(9) yes C2 . P1 . C21 . 102.83(13) yes C15 . P1 . C21 . 102.71(13) yes F1 . P2 . F2 . 87.45(16) yes F1 . P2 . F3 . 89.8(3) yes F2 . P2 . F3 . 90.28(17) yes F1 . P2 . F4 . 178.9(2) yes F2 . P2 . F4 . 91.57(16) yes F3 . P2 . F4 . 89.6(3) yes F1 . P2 . F5 . 90.7(3) yes F2 . P2 . F5 . 89.59(18) yes F3 . P2 . F5 . 179.5(3) yes F4 . P2 . F5 . 89.9(3) yes F1 . P2 . F6 . 91.47(16) yes F2 . P2 . F6 . 178.92(16) yes F3 . P2 . F6 . 89.80(16) yes F4 . P2 . F6 . 89.51(16) yes F5 . P2 . F6 . 90.33(16) yes N1 . C1 . O1 . 120.2(3) yes N1 . C1 . C2 . 119.6(3) yes O1 . C1 . C2 . 120.1(3) yes P1 . C2 . C1 . 106.7(2) yes P1 . C2 . H21 . 110.2 no C1 . C2 . H21 . 109.8 no P1 . C2 . H22 . 110.4 no C1 . C2 . H22 . 110.0 no H21 . C2 . H22 . 109.7 no N1 . C3 . C4 . 120.5(3) yes N1 . C3 . C8 . 118.4(3) yes C4 . C3 . C8 . 121.0(3) yes C3 . C4 . C5 . 119.3(4) yes C3 . C4 . H41 . 119.9 no C5 . C4 . H41 . 120.8 no C4 . C5 . C6 . 119.5(4) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 120.5(4) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 119.5 no C6 . C7 . C8 . 120.3(4) yes C6 . C7 . H71 . 120.6 no C8 . C7 . H71 . 119.1 no C3 . C8 . C7 . 119.3(4) yes C3 . C8 . H81 . 120.3 no C7 . C8 . H81 . 120.3 no N1 . C9 . C10 . 117.8(3) yes N1 . C9 . C14 . 120.9(3) yes C10 . C9 . C14 . 121.2(3) yes C9 . C10 . C11 . 119.7(4) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 120.2 no C10 . C11 . C12 . 119.8(4) yes C10 . C11 . H111 . 120.7 no C12 . C11 . H111 . 119.5 no C11 . C12 . C13 . 120.0(4) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 120.6(4) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 119.4 no C9 . C14 . C13 . 118.7(4) yes C9 . C14 . H141 . 120.4 no C13 . C14 . H141 . 120.9 no P1 . C15 . C16 . 118.4(2) yes P1 . C15 . C20 . 122.6(2) yes C16 . C15 . C20 . 118.8(3) yes C15 . C16 . C17 . 120.0(3) yes C15 . C16 . H161 . 120.1 no C17 . C16 . H161 . 119.9 no C16 . C17 . C18 . 120.4(4) yes C16 . C17 . H171 . 119.9 no C18 . C17 . H171 . 119.7 no C17 . C18 . C19 . 120.0(3) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.6 no C18 . C19 . C20 . 120.2(4) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 120.1 no C15 . C20 . C19 . 120.7(3) yes C15 . C20 . H201 . 119.7 no C19 . C20 . H201 . 119.7 no P1 . C21 . C22 . 121.6(2) yes P1 . C21 . C26 . 119.3(2) yes C22 . C21 . C26 . 119.0(3) yes C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 119.9 no C22 . C23 . C24 . 120.5(3) yes C22 . C23 . H231 . 120.1 no C24 . C23 . H231 . 119.4 no C23 . C24 . C25 . 120.1(3) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 119.8 no C24 . C25 . C26 . 119.8(3) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.2 no C21 . C26 . C25 . 120.5(3) yes C21 . C26 . H261 . 119.6 no C25 . C26 . H261 . 119.9 no Mo1 . C27 . C28 . 69.43(17) yes Mo1 . C27 . H271 . 78.32 no C28 . C27 . H271 . 120.2 no Mo1 . C27 . H272 . 124.1 no C28 . C27 . H272 . 119.9 no H271 . C27 . H272 . 119.9 no Mo1 . C28 . C27 . 72.95(17) yes Mo1 . C28 . C29 . 73.99(19) yes C27 . C28 . C29 . 115.8(3) yes Mo1 . C28 . H281 . 122.6 no C27 . C28 . H281 . 122.4 no C29 . C28 . H281 . 121.8 no Mo1 . C29 . C28 . 69.25(18) yes Mo1 . C29 . H291 . 124.0 no C28 . C29 . H291 . 120.4 no Mo1 . C29 . H292 . 77.44 no C28 . C29 . H292 . 119.9 no H291 . C29 . H292 . 119.7 no Mo1 . C30 . C31 . 70.90(18) yes Mo1 . C30 . C35 . 76.2(2) yes C31 . C30 . C35 . 121.0(3) yes Mo1 . C30 . H301 . 125.2 no C31 . C30 . H301 . 119.5 no C35 . C30 . H301 . 119.5 no Mo1 . C31 . C30 . 72.32(18) yes Mo1 . C31 . C32 . 76.03(19) yes C30 . C31 . C32 . 118.2(3) yes Mo1 . C31 . H311 . 122.0 no C30 . C31 . H311 . 121.0 no C32 . C31 . H311 . 120.8 no Mo1 . C32 . C31 . 69.00(18) yes Mo1 . C32 . C33 . 70.19(18) yes C31 . C32 . C33 . 121.1(3) yes Mo1 . C32 . H321 . 135.8 no C31 . C32 . H321 . 120.1 no C33 . C32 . H321 . 118.8 no Mo1 . C33 . C32 . 74.99(19) yes Mo1 . C33 . C34 . 69.62(18) yes C32 . C33 . C34 . 119.1(3) yes Mo1 . C33 . H331 . 126.2 no C32 . C33 . H331 . 120.2 no C34 . C33 . H331 . 120.7 no Mo1 . C34 . C33 . 73.50(19) yes Mo1 . C34 . C35 . 77.76(19) yes C33 . C34 . C35 . 120.0(3) yes Mo1 . C34 . H341 . 119.8 no C33 . C34 . H341 . 120.3 no C35 . C34 . H341 . 119.7 no Mo1 . C35 . C30 . 68.95(18) yes Mo1 . C35 . C34 . 67.24(18) yes C30 . C35 . C34 . 118.5(3) yes Mo1 . C35 . C36 . 132.5(3) yes C30 . C35 . C36 . 120.3(4) yes C34 . C35 . C36 . 121.0(4) yes C35 . C36 . H361 . 110.3 no C35 . C36 . H362 . 109.7 no H361 . C36 . H362 . 109.0 no C35 . C36 . H363 . 110.0 no H361 . C36 . H363 . 109.1 no H362 . C36 . H363 . 108.7 no C100 2_665 C100 . Cl1 . 43.0(6) yes C100 2_665 C100 . Cl1 2_665 92.2(9) yes Cl1 . C100 . Cl1 2_665 135.2(7) yes C100 2_665 C100 . Cl2 . 67.3(8) yes Cl1 . C100 . Cl2 . 109.9(5) yes Cl1 2_665 C100 . Cl2 . 26.2(3) yes C100 2_665 C100 . Cl2 2_665 71.0(7) yes Cl1 . C100 . Cl2 2_665 28.8(2) yes Cl1 2_665 C100 . Cl2 2_665 161.3(9) yes Cl2 . C100 . Cl2 2_665 138.3(5) yes C100 2_665 C100 . H1001 . 121.0 no Cl1 . C100 . H1001 . 111.0 no Cl1 2_665 C100 . H1001 . 90.4 no Cl2 . C100 . H1001 . 109.8 no Cl2 2_665 C100 . H1001 . 91.4 no C100 2_665 C100 . H1002 . 130.3 no Cl1 . C100 . H1002 . 110.0 no Cl1 2_665 C100 . H1002 . 99.6 no Cl2 . C100 . H1002 . 109.0 no Cl2 2_665 C100 . H1002 . 97.7 no H1001 . C100 . H1002 . 107.0 no C100 . Cl1 . C100 2_665 44.8(7) yes C100 . Cl1 . Cl2 2_665 73.0(5) yes C100 2_665 Cl1 . Cl2 2_665 116.0(7) yes C100 . Cl1 . H1001 2_665 72.0 no C100 2_665 Cl1 . H1001 2_665 40.1 no Cl2 2_665 Cl1 . H1001 2_665 140.5 no C100 . Cl2 . C100 2_665 41.7(5) yes C100 . Cl2 . Cl1 2_665 37.8(5) yes C100 2_665 Cl2 . Cl1 2_665 78.2(5) yes C100 . H1001 . Cl1 2_665 49.5 no