Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Neale G. Jones' 'Malcolm L.H. Green' 'Ino Vei' 'Pierre Braunstein' 'Xavier Morise' _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' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of molybdenum arene complexes containing amide derived heterodifunctional P,O ligands. ; data_Compound2a _database_code_CSD 169296 _audit_creation_date 01-28-09 _audit_creation_method CRYSTALS_ver_12-03-99 # ino6 # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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 # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #************************************************************************** _cell_length_a 10.8978(2) _cell_angle_alpha 90 _cell_length_b 18.1501(3) _cell_angle_beta 104.2295(6) _cell_length_c 14.0945(3) _cell_angle_gamma 90 _cell_volume 2702.3 _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' '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' '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' _chemical_formula_sum ' C25 H31 F6 Mo1 N1 O2 P2 ' _chemical_formula_moiety ' C25 H31 F6 Mo1 N1 O2 P2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 649.40 _cell_measurement_reflns_used 24477 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1313.732 _exptl_absorpt_coefficient_mu 0.669 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.82 _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 24477 _reflns_number_total 6343 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections with Friedels Law is 6343 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6198 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 5053 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -0.61 _refine_diff_density_max 0.84 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5053 _refine_ls_number_parameters 335 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0392 _refine_ls_goodness_of_fit_ref 1.0104 _refine_ls_shift/su_max 0.006412 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.06 0.469 0.735 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; large adps and short C-C distance of the ethanol suggest it may be disordered. This could not be resolved and was ignored during refinement All H atoms were positioned geometrically following each cycle of refinement ; # 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 0.247328(15) 0.119930(9) -0.025130(11) 0.0214 1.0000 Uani C2 0.5146(2) 0.16584(11) -0.03580(15) 0.0255 1.0000 Uani C3 0.6257(2) 0.17264(13) -0.07959(17) 0.0316 1.0000 Uani C4 0.36944(19) 0.28281(11) 0.12654(15) 0.0246 1.0000 Uani C5 0.4129(2) 0.33663(13) 0.07168(16) 0.0301 1.0000 Uani C6 0.3859(2) 0.41048(13) 0.08284(18) 0.0353 1.0000 Uani C7 0.3154(2) 0.43174(13) 0.14743(19) 0.0353 1.0000 Uani C8 0.2715(3) 0.37908(14) 0.2008(2) 0.0393 1.0000 Uani C9 0.2981(2) 0.30466(13) 0.19102(18) 0.0337 1.0000 Uani C10 0.46078(19) 0.14524(11) 0.22453(14) 0.0224 1.0000 Uani C11 0.5844(2) 0.11857(11) 0.25275(16) 0.0252 1.0000 Uani C12 0.6290(2) 0.08492(13) 0.34370(17) 0.0320 1.0000 Uani C13 0.5498(2) 0.07736(13) 0.40657(16) 0.0330 1.0000 Uani C14 0.4254(2) 0.10250(13) 0.37821(17) 0.0324 1.0000 Uani C15 0.3810(2) 0.13598(13) 0.28795(16) 0.0285 1.0000 Uani C16 0.2949(2) 0.00461(13) -0.06373(19) 0.0361 1.0000 Uani C17 0.3431(2) 0.01847(12) 0.03791(18) 0.0325 1.0000 Uani C18 0.2477(2) 0.03231(12) 0.08855(17) 0.0317 1.0000 Uani C19 0.0307(2) 0.12347(16) -0.0258(2) 0.0410 1.0000 Uani C20 0.0905(2) 0.19201(16) 0.00147(19) 0.0411 1.0000 Uani C21 0.1466(3) 0.23047(14) -0.0660(2) 0.0470 1.0000 Uani C22 0.1475(3) 0.19780(17) -0.1560(2) 0.0458 1.0000 Uani C23 0.1080(3) 0.12493(17) -0.17448(18) 0.0439 1.0000 Uani C24 0.0463(2) 0.08773(16) -0.1090(2) 0.0422 1.0000 Uani C25 0.3991(5) 0.1304(3) -0.3453(4) 0.0854 1.0000 Uani C26 0.2924(4) 0.1680(3) -0.4021(4) 0.0945 1.0000 Uani F1 0.37780(18) 0.36421(11) -0.31824(15) 0.0656 1.0000 Uani F2 0.55664(19) 0.30100(9) -0.25763(14) 0.0555 1.0000 Uani F3 0.41383(17) 0.3138(1) -0.16817(13) 0.0532 1.0000 Uani F4 0.6013(2) 0.37374(13) -0.12497(14) 0.0710 1.0000 Uani F5 0.4219(2) 0.43789(11) -0.1861(2) 0.0773 1.0000 Uani F6 0.56467(15) 0.42376(9) -0.27506(12) 0.0477 1.0000 Uani N1 0.52614(16) 0.1908(1) 0.05548(13) 0.0254 1.0000 Uani P1 0.39666(5) 0.18526(3) 0.10405(3) 0.0207 1.0000 Uani P2 0.48982(6) 0.36975(3) -0.22036(4) 0.0300 1.0000 Uani O1 0.41415(15) 0.13697(9) -0.08340(11) 0.0284 1.0000 Uani O2 0.24685(17) 0.22898(11) -0.35954(14) 0.0452 1.0000 Uani H31 0.6973 0.1969 -0.0316 0.0402 1.0000 Uiso H32 0.6018 0.2031 -0.1405 0.0402 1.0000 Uiso H33 0.6525 0.1225 -0.0960 0.0402 1.0000 Uiso H51 0.4634 0.3219 0.0243 0.0361 1.0000 Uiso H61 0.4179 0.4487 0.0437 0.0413 1.0000 Uiso H71 0.2966 0.4850 0.1552 0.0406 1.0000 Uiso H81 0.2200 0.3942 0.2473 0.0486 1.0000 Uiso H91 0.2657 0.2669 0.2305 0.0422 1.0000 Uiso H111 0.6416 0.1236 0.2074 0.0303 1.0000 Uiso H121 0.7180 0.0662 0.3636 0.0371 1.0000 Uiso H131 0.5820 0.0539 0.4722 0.0382 1.0000 Uiso H141 0.3679 0.0964 0.4231 0.0396 1.0000 Uiso H151 0.2915 0.1537 0.2679 0.0347 1.0000 Uiso H161 0.3544 -0.0058 -0.1060 0.0428 1.0000 Uiso H162 0.2015 0.0052 -0.0930 0.0428 1.0000 Uiso H171 0.4355 0.0185 0.0707 0.0377 1.0000 Uiso H181 0.2719 0.0427 0.1604 0.0371 1.0000 Uiso H182 0.1565 0.0317 0.0523 0.0371 1.0000 Uiso H191 -0.0227 0.1008 0.0149 0.0488 1.0000 Uiso H201 0.0936 0.2135 0.0673 0.0474 1.0000 Uiso H211 0.1849 0.2803 -0.0491 0.0508 1.0000 Uiso H221 0.1764 0.2267 -0.2069 0.0523 1.0000 Uiso H231 0.1226 0.0987 -0.2331 0.0503 1.0000 Uiso H241 0.0147 0.0362 -0.1234 0.0485 1.0000 Uiso H251 0.4213 0.0885 -0.3841 0.0972 1.0000 Uiso H252 0.4723 0.1651 -0.3273 0.0972 1.0000 Uiso H253 0.3791 0.1109 -0.2845 0.0972 1.0000 Uiso H261 0.3149 0.1857 -0.4628 0.1086 1.0000 Uiso H262 0.2217 0.1315 -0.4200 0.1086 1.0000 Uiso H271 0.6078 0.2120 0.0942 0.0313 1.0000 Uiso H281 0.2932 0.2768 -0.3449 0.0518 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 0.02170(11) 0.02205(11) 0.0192(1) -0.00254(6) 0.00261(6) -0.00189(6) C2 0.029(1) 0.0234(9) 0.0264(9) 0.0015(7) 0.0113(8) 0.0008(8) C3 0.0337(11) 0.0339(11) 0.0329(11) 0.0021(9) 0.0187(9) 0.0014(9) C4 0.0232(9) 0.0243(9) 0.0246(9) -0.0035(7) 0.0029(7) -0.0030(7) C5 0.0337(11) 0.029(1) 0.027(1) 0.0015(8) 0.0073(8) -0.0023(9) C6 0.0397(12) 0.0268(11) 0.0367(12) 0.0052(9) 0.005(1) -0.0042(9) C7 0.0334(11) 0.026(1) 0.0419(12) -0.0051(9) 0.001(1) 0.0007(9) C8 0.0422(13) 0.0336(12) 0.0457(13) -0.009(1) 0.0175(11) 0.004(1) C9 0.0355(11) 0.0295(11) 0.0404(12) -0.0048(9) 0.018(1) -0.0021(9) C10 0.0229(9) 0.0241(9) 0.0197(8) -0.0029(7) 0.0044(7) -0.0047(7) C11 0.0222(9) 0.0236(9) 0.030(1) -0.0021(8) 0.0069(8) -0.0012(7) C12 0.0291(11) 0.0286(11) 0.0350(11) 0.0032(9) 0.0017(9) 0.0013(8) C13 0.0402(12) 0.0288(11) 0.026(1) 0.0031(8) 0.0018(9) -0.0025(9) C14 0.0358(12) 0.0349(11) 0.028(1) 0.0013(9) 0.0114(9) -0.0033(9) C15 0.025(1) 0.0350(11) 0.027(1) 0.0001(8) 0.0087(8) -0.0021(8) C16 0.0399(12) 0.0257(11) 0.0414(12) -0.0099(9) 0.007(1) 0.0015(9) C17 0.0371(11) 0.0179(9) 0.0392(12) -0.0012(8) 0.0030(9) 0.0001(8) C18 0.0347(11) 0.025(1) 0.0325(11) 0.0044(8) 0.0036(9) -0.0070(9) C19 0.0242(11) 0.0578(16) 0.0401(13) 0.0059(11) 0.0061(9) 0.003(1) C20 0.0295(11) 0.0509(15) 0.0381(12) -0.0120(11) -0.0008(9) 0.0129(11) C21 0.0419(14) 0.0280(12) 0.0571(16) 0.0049(11) -0.0146(12) 0.008(1) C22 0.0363(13) 0.0556(16) 0.0389(13) 0.0218(12) -0.004(1) 0.0043(12) C23 0.0405(14) 0.0598(17) 0.0255(11) -0.004(1) -0.003(1) 0.0094(12) C24 0.0290(11) 0.0436(14) 0.0486(14) -0.0114(11) -0.001(1) -0.004(1) C25 0.092(3) 0.075(3) 0.077(3) -0.021(2) -0.005(2) 0.034(2) C26 0.075(3) 0.106(4) 0.090(3) -0.051(3) -0.003(2) 0.040(3) F1 0.0533(11) 0.0614(11) 0.0656(12) 0.0245(9) -0.0171(9) -0.0118(9) F2 0.0708(11) 0.0382(9) 0.0682(11) 0.0073(8) 0.0373(9) 0.0170(8) F3 0.056(1) 0.053(1) 0.058(1) 0.0099(8) 0.0297(8) -0.0096(8) F4 0.0618(12) 0.1006(17) 0.0408(9) 0.0073(9) -0.0062(9) -0.0225(11) F5 0.0773(14) 0.046(1) 0.130(2) -0.0177(11) 0.0674(14) 0.0027(9) F6 0.0495(9) 0.0424(8) 0.0567(9) 0.0084(7) 0.0233(8) -0.0069(7) N1 0.0242(8) 0.0302(9) 0.0238(8) -0.0013(7) 0.0097(6) -0.0036(7) P1 0.0202(2) 0.0231(2) 0.0192(2) -0.00238(17) 0.00580(17) -0.00304(18) P2 0.0269(3) 0.0302(3) 0.0342(3) 0.0028(2) 0.0101(2) 0.0008(2) O1 0.0314(8) 0.0315(7) 0.0238(7) -0.0032(6) 0.0098(6) -0.0016(6) O2 0.0348(9) 0.045(1) 0.0500(11) -0.0126(8) -0.0011(8) 0.0078(8) _refine_ls_extinction_coef 156.6(306) _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 . C16 . 2.255(2) yes Mo1 . C17 . 2.194(2) yes Mo1 . C18 . 2.257(2) yes Mo1 . C19 . 2.359(2) yes Mo1 . C20 . 2.256(2) yes Mo1 . C21 . 2.292(2) yes Mo1 . C22 . 2.366(2) yes Mo1 . C23 . 2.275(2) yes Mo1 . C24 . 2.295(2) yes Mo1 . P1 . 2.4316(5) yes Mo1 . O1 . 2.1930(15) yes C2 . C3 . 1.494(3) yes C2 . N1 . 1.340(3) yes C2 . O1 . 1.250(3) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . C5 . 1.398(3) yes C4 . C9 . 1.392(3) yes C4 . P1 . 1.836(2) yes C5 . C6 . 1.389(3) yes C5 . H51 . 1.000 no C6 . C7 . 1.383(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.374(4) yes C7 . H71 . 1.000 no C8 . C9 . 1.395(3) yes C8 . H81 . 1.000 no C9 . H91 . 1.000 no C10 . C11 . 1.395(3) yes C10 . C15 . 1.402(3) yes C10 . P1 . 1.821(2) yes C11 . C12 . 1.395(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.388(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.393(3) yes C13 . H131 . 1.000 no C14 . C15 . 1.385(3) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.422(3) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . C18 . 1.420(3) yes C17 . H171 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C19 . C20 . 1.413(4) yes C19 . C24 . 1.387(4) yes C19 . H191 . 1.000 no C20 . C21 . 1.433(4) yes C20 . H201 . 1.000 no C21 . C22 . 1.402(4) yes C21 . H211 . 1.000 no C22 . C23 . 1.395(4) yes C22 . H221 . 1.000 no C23 . C24 . 1.437(4) yes C23 . H231 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.414(6) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . O2 . 1.406(4) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no F1 . P2 . 1.6049(19) yes F2 . P2 . 1.5973(17) yes F3 . P2 . 1.5997(16) yes F4 . P2 . 1.5768(19) yes F5 . P2 . 1.5772(18) yes F6 . P2 . 1.5907(15) yes N1 . P1 . 1.7160(17) yes N1 . H271 . 1.0000 no O2 . H281 . 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 C16 . Mo1 . C17 . 37.24(9) yes C16 . Mo1 . C18 . 63.69(9) yes C17 . Mo1 . C18 . 37.18(9) yes C16 . Mo1 . C19 . 108.3(1) yes C17 . Mo1 . C19 . 113.59(9) yes C18 . Mo1 . C19 . 81.33(9) yes C16 . Mo1 . C20 . 143.8(1) yes C17 . Mo1 . C20 . 136.4(1) yes C18 . Mo1 . C20 . 99.2(1) yes C19 . Mo1 . C20 . 35.6(1) yes C16 . Mo1 . C21 . 151.2(1) yes C17 . Mo1 . C21 . 170.9(1) yes C18 . Mo1 . C21 . 135.47(11) yes C19 . Mo1 . C21 . 63.8(1) yes C20 . Mo1 . C21 . 36.72(11) yes C16 . Mo1 . C22 . 117.08(11) yes C17 . Mo1 . C22 . 154.0(1) yes C18 . Mo1 . C22 . 153.49(9) yes C19 . Mo1 . C22 . 73.3(1) yes C20 . Mo1 . C22 . 64.0(1) yes C16 . Mo1 . C23 . 87.4(1) yes C17 . Mo1 . C23 . 123.4(1) yes C18 . Mo1 . C23 . 124.7(1) yes C19 . Mo1 . C23 . 63.6(1) yes C20 . Mo1 . C23 . 76.7(1) yes C16 . Mo1 . C24 . 83.47(9) yes C17 . Mo1 . C24 . 107.07(9) yes C18 . Mo1 . C24 . 91.2(1) yes C19 . Mo1 . C24 . 34.6(1) yes C20 . Mo1 . C24 . 64.33(9) yes C16 . Mo1 . P1 . 118.82(6) yes C17 . Mo1 . P1 . 86.67(6) yes C18 . Mo1 . P1 . 85.86(6) yes C19 . Mo1 . P1 . 118.32(7) yes C20 . Mo1 . P1 . 89.30(6) yes C16 . Mo1 . O1 . 77.27(8) yes C17 . Mo1 . O1 . 85.10(8) yes C18 . Mo1 . O1 . 120.54(7) yes C19 . Mo1 . O1 . 156.28(8) yes C20 . Mo1 . O1 . 135.42(9) yes C21 . Mo1 . C22 . 35.00(11) yes C21 . Mo1 . C23 . 64.1(1) yes C22 . Mo1 . C23 . 34.93(11) yes C21 . Mo1 . C24 . 75.9(1) yes C22 . Mo1 . C24 . 63.4(1) yes C23 . Mo1 . C24 . 36.66(11) yes C21 . Mo1 . P1 . 87.28(7) yes C22 . Mo1 . P1 . 112.79(8) yes C23 . Mo1 . P1 . 147.69(8) yes C24 . Mo1 . P1 . 152.68(7) yes C21 . Mo1 . O1 . 99.91(9) yes C22 . Mo1 . O1 . 83.59(8) yes C23 . Mo1 . O1 . 94.25(9) yes C24 . Mo1 . O1 . 128.13(8) yes P1 . Mo1 . O1 . 75.39(4) yes C3 . C2 . N1 . 118.31(19) yes C3 . C2 . O1 . 120.34(19) yes N1 . C2 . O1 . 121.36(19) yes C2 . C3 . H31 . 109.47 no C2 . C3 . H32 . 109.5 no H31 . C3 . H32 . 109.5 no C2 . C3 . H33 . 109.5 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no C5 . C4 . C9 . 118.8(2) yes C5 . C4 . P1 . 119.16(16) yes C9 . C4 . P1 . 121.86(16) yes C4 . C5 . C6 . 120.1(2) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 119.9 no C5 . C6 . C7 . 120.7(2) yes C5 . C6 . H61 . 119.6 no C7 . C6 . H61 . 119.6 no C6 . C7 . C8 . 119.4(2) yes C6 . C7 . H71 . 120.3 no C8 . C7 . H71 . 120.3 no C7 . C8 . C9 . 120.7(2) yes C7 . C8 . H81 . 119.6 no C9 . C8 . H81 . 119.6 no C4 . C9 . C8 . 120.2(2) yes C4 . C9 . H91 . 119.9 no C8 . C9 . H91 . 119.9 no C11 . C10 . C15 . 118.92(19) yes C11 . C10 . P1 . 121.79(15) yes C15 . C10 . P1 . 119.12(16) yes C10 . C11 . C12 . 120.52(19) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 119.7 no C11 . C12 . C13 . 120.0(2) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 119.9(2) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 120.2(2) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 119.9 no C10 . C15 . C14 . 120.5(2) yes C10 . C15 . H151 . 119.8 no C14 . C15 . H151 . 119.8 no Mo1 . C16 . C17 . 69.06(12) yes Mo1 . C16 . H161 . 122.66 no C17 . C16 . H161 . 120.0 no Mo1 . C16 . H162 . 79.51 no C17 . C16 . H162 . 120.0 no H161 . C16 . H162 . 120.0 no Mo1 . C17 . C16 . 73.70(13) yes Mo1 . C17 . C18 . 73.81(13) yes C16 . C17 . C18 . 113.8(2) yes Mo1 . C17 . H171 . 120.80 no C16 . C17 . H171 . 123.1 no C18 . C17 . H171 . 123.1 no Mo1 . C18 . C17 . 69.01(12) yes Mo1 . C18 . H181 . 122.73 no C17 . C18 . H181 . 120.0 no Mo1 . C18 . H182 . 79.49 no C17 . C18 . H182 . 120.0 no H181 . C18 . H182 . 120.0 no Mo1 . C19 . C20 . 68.22(14) yes Mo1 . C19 . C24 . 70.12(14) yes C20 . C19 . C24 . 119.8(2) yes Mo1 . C19 . H191 . 135.18 no C20 . C19 . H191 . 120.1 no C24 . C19 . H191 . 120.1 no Mo1 . C20 . C19 . 76.22(15) yes Mo1 . C20 . C21 . 72.99(14) yes C19 . C20 . C21 . 119.5(2) yes Mo1 . C20 . H201 . 121.77 no C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 120.3 no Mo1 . C21 . C20 . 70.28(14) yes Mo1 . C21 . C22 . 75.41(15) yes C20 . C21 . C22 . 119.6(2) yes Mo1 . C21 . H211 . 125.84 no C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 120.2 no Mo1 . C22 . C21 . 69.59(14) yes Mo1 . C22 . C23 . 68.94(14) yes C21 . C22 . C23 . 119.9(3) yes Mo1 . C22 . H221 . 135.0 no C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 120.0 no Mo1 . C23 . C22 . 76.13(15) yes Mo1 . C23 . C24 . 72.43(14) yes C22 . C23 . C24 . 119.8(3) yes Mo1 . C23 . H231 . 122.7 no C22 . C23 . H231 . 120.1 no C24 . C23 . H231 . 120.1 no Mo1 . C24 . C19 . 75.24(15) yes Mo1 . C24 . C23 . 70.91(14) yes C19 . C24 . C23 . 119.8(3) yes Mo1 . C24 . H241 . 125.5 no C19 . C24 . H241 . 120.1 no C23 . C24 . H241 . 120.1 no C26 . C25 . H251 . 109.5 no C26 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C26 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C25 . C26 . O2 . 117.8(4) yes C25 . C26 . H261 . 107.4 no O2 . C26 . H261 . 107.4 no C25 . C26 . H262 . 107.4 no O2 . C26 . H262 . 107.4 no H261 . C26 . H262 . 109.5 no C2 . N1 . P1 . 118.07(15) yes C2 . N1 . H271 . 120.97 no P1 . N1 . H271 . 120.97 no Mo1 . P1 . C4 . 119.53(7) yes Mo1 . P1 . C10 . 122.44(7) yes C4 . P1 . C10 . 105.36(9) yes Mo1 . P1 . N1 . 101.22(6) yes C4 . P1 . N1 . 101.30(9) yes C10 . P1 . N1 . 103.34(9) yes F1 . P2 . F2 . 88.87(12) yes F1 . P2 . F3 . 89.1(1) yes F2 . P2 . F3 . 89.1(1) yes F1 . P2 . F4 . 178.76(14) yes F2 . P2 . F4 . 89.89(12) yes F3 . P2 . F4 . 90.85(11) yes F1 . P2 . F5 . 89.84(14) yes F2 . P2 . F5 . 178.65(14) yes F3 . P2 . F5 . 91.27(11) yes F4 . P2 . F5 . 91.40(14) yes F1 . P2 . F6 . 89.7(1) yes F2 . P2 . F6 . 89.57(9) yes F3 . P2 . F6 . 178.2(1) yes F4 . P2 . F6 . 90.3(1) yes F5 . P2 . F6 . 90.0(1) yes Mo1 . O1 . C2 . 123.74(13) yes C26 . O2 . H281 . 123.9 no #===END data_Compound3a _database_code_CSD 169297 _audit_creation_date 01-28-09 _audit_creation_method CRYSTALS_ver_12-03-99 # ino9 # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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 11.4697(5) _cell_angle_alpha 90 _cell_length_b 13.7585(8) _cell_angle_beta 105.4(1) _cell_length_c 16.5254(9) _cell_angle_gamma 90 _cell_volume 2513.8 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-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' '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' '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' _chemical_formula_sum ' C24 H27 F6 Mo1 N1 O1 P2 ' _chemical_formula_moiety ' C24 H27 F6 Mo1 N1 O1 P2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 617.36 _cell_measurement_reflns_used 16660 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1241.698 _exptl_absorpt_coefficient_mu 0.712 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.87 _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 16660 _reflns_number_total 5979 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 3076 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.60 _refine_diff_density_max 0.63 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3076 _refine_ls_number_parameters 345 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0471 _refine_ls_goodness_of_fit_ref 1.0325 _refine_ls_shift/su_max 0.000437 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.688 0.249 0.403 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; Initial structure solution showed two 6-membered rings bonded to Mo with unfeasibly short C-C contacts. These were interpreted as an allyl and phenyl group disordered by interchange such that the allyl C atoms overlapped with three phenyl C atoms. Attempts to split the overlapping sites lead to a model that could not successfully be refined. Accordingly the occupancies of the overlapping C atoms were set to 1 while those of the other C atoms were refined. C-C bond lengths were restrained to be 1.4(01) A and vibrational restraints were aplied to directly-bonded atoms. refinement of the PF6 anion lead to unreasonably large adps, suggesting the ion to be disordered, but it was not possible to resolve this. Examination of the structure shows a considerable void to lie adjacent to the PF6 anion. Difference Fourier maps show no significant electron density to be present in this region, suggesting it to be genuinely vacant. All H atoms were positioned geometrically following each cycle of refinement ; # 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 0.72395(4) 0.37299(3) 0.14284(2) 0.0275 1.0000 Uani C1 0.9126(4) 0.4389(3) 0.3013(3) 0.0300 1.0000 Uani C2 1.0190(5) 0.4967(4) 0.3485(3) 0.0426 1.0000 Uani C3 0.8809(5) 0.3863(4) 0.4362(3) 0.0398 1.0000 Uani C4 0.6077(5) 0.3450(4) 0.3299(3) 0.0358 1.0000 Uani C5 0.6025(5) 0.4358(4) 0.3656(4) 0.0428 1.0000 Uani C6 0.5079(6) 0.4626(5) 0.3973(4) 0.0529 1.0000 Uani C7 0.4141(6) 0.3980(5) 0.3927(5) 0.0604 1.0000 Uani C8 0.4149(6) 0.3092(5) 0.3569(5) 0.0639 1.0000 Uani C9 0.5112(5) 0.2822(4) 0.3257(4) 0.0534 1.0000 Uani C10 0.7797(5) 0.1936(4) 0.3144(3) 0.0356 1.0000 Uani C11 0.8989(6) 0.1745(4) 0.3570(4) 0.0461 1.0000 Uani C12 0.9371(6) 0.0789(5) 0.3768(4) 0.0553 1.0000 Uani C13 0.8565(7) 0.0032(4) 0.3536(5) 0.0599 1.0000 Uani C14 0.7399(6) 0.0199(4) 0.3091(4) 0.0537 1.0000 Uani C15 0.6996(6) 0.1147(4) 0.2890(4) 0.0469 1.0000 Uani C202 0.5302(5) 0.4146(4) 0.1288(4) 0.0505 1.0000 Uani C101 0.6208(14) 0.271(1) 0.0397(8) 0.0692 0.404(9) Uani C102 0.7081(7) 0.2156(4) 0.1015(4) 0.0615 1.0000 Uani C103 0.8300(6) 0.2425(4) 0.1266(4) 0.0603 1.0000 Uani C104 0.8665(6) 0.3149(5) 0.0808(4) 0.0558 1.0000 Uani C105 0.7835(12) 0.3735(11) 0.0259(8) 0.0594 0.404(9) Uani C106 0.6596(15) 0.3529(12) 0.0028(9) 0.0640 0.404(9) Uani C201 0.5348(7) 0.3742(7) 0.0480(5) 0.0463 0.596(9) Uani C203 0.6054(5) 0.4946(4) 0.1633(3) 0.0420 1.0000 Uani C204 0.6751(5) 0.5352(4) 0.1137(3) 0.0436 1.0000 Uani C205 0.6926(8) 0.4906(6) 0.0414(5) 0.0423 0.596(9) Uani C206 0.6231(8) 0.4074(7) 0.0093(5) 0.0420 0.596(9) Uani N1 0.8488(4) 0.3858(3) 0.3432(2) 0.0301 1.0000 Uani O1 0.8833(3) 0.4408(2) 0.22281(19) 0.0336 1.0000 Uani P1 0.73041(12) 0.31748(9) 0.28243(7) 0.0308 1.0000 Uani P2 0.75590(15) 0.70811(11) 0.41551(13) 0.0595 1.0000 Uani F1 0.8918(3) 0.7359(4) 0.4390(4) 0.1286 1.0000 Uani F2 0.7349(6) 0.7757(4) 0.4863(4) 0.1413 1.0000 Uani F3 0.7830(4) 0.6180(3) 0.4776(3) 0.0920 1.0000 Uani F4 0.6179(3) 0.6791(3) 0.3927(4) 0.1136 1.0000 Uani F5 0.7732(6) 0.6368(4) 0.3451(4) 0.1255 1.0000 Uani F6 0.7261(4) 0.7947(3) 0.3524(4) 0.1073 1.0000 Uani H21 1.0553 0.5314 0.3079 0.0502 1.0000 Uiso H22 1.0805 0.4522 0.3842 0.0502 1.0000 Uiso H23 0.9925 0.5452 0.3850 0.0502 1.0000 Uiso H31 0.8240 0.3430 0.4560 0.0468 1.0000 Uiso H32 0.9655 0.3621 0.4587 0.0468 1.0000 Uiso H33 0.8746 0.4540 0.4566 0.0468 1.0000 Uiso H51 0.6697 0.4831 0.3683 0.0507 1.0000 Uiso H61 0.5070 0.5281 0.4234 0.0647 1.0000 Uiso H71 0.3452 0.4168 0.4159 0.0744 1.0000 Uiso H81 0.3461 0.2632 0.3531 0.0791 1.0000 Uiso H91 0.5111 0.2166 0.2996 0.0645 1.0000 Uiso H111 0.9577 0.2293 0.3737 0.0547 1.0000 Uiso H121 1.0231 0.0655 0.4078 0.0673 1.0000 Uiso H131 0.8839 -0.0648 0.3697 0.0774 1.0000 Uiso H141 0.6832 -0.0360 0.2909 0.0689 1.0000 Uiso H151 0.6139 0.1268 0.2565 0.0594 1.0000 Uiso H1011 0.5337 0.2516 0.0233 0.0827 0.4038 Uiso H1021 0.6518 0.2484 0.0524 0.0757 0.5962 Uiso H1022 0.6773 0.1636 0.1327 0.0757 1.0000 Uiso H1031 0.8881 0.2108 0.1755 0.0725 1.0000 Uiso H1041 0.9528 0.3367 0.0962 0.0692 1.0000 Uiso H1042 0.8067 0.3454 0.0322 0.0692 0.5962 Uiso H1051 0.8131 0.4325 0.0020 0.0758 0.4038 Uiso H1061 0.6010 0.3946 -0.0384 0.0755 0.4038 Uiso H2011 0.4755 0.3231 0.0202 0.0521 0.5962 Uiso H2021 0.5286 0.3897 0.0717 0.0589 0.4038 Uiso H2022 0.4788 0.3831 0.1617 0.0589 1.0000 Uiso H2031 0.6086 0.5207 0.2203 0.0504 1.0000 Uiso H2041 0.7295 0.5916 0.1351 0.0516 1.0000 Uiso H2042 0.6704 0.5077 0.0568 0.0516 0.4038 Uiso H2051 0.7530 0.5170 0.0132 0.0512 0.5962 Uiso H2061 0.6366 0.3724 -0.0405 0.0477 0.5962 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 0.0342(2) 0.0257(2) 0.02097(18) -0.00020(19) 0.00438(13) -0.0042(2) C1 0.031(3) 0.027(2) 0.029(2) -0.0011(19) 0.003(2) -0.003(2) C2 0.040(3) 0.048(3) 0.038(3) -0.008(2) 0.007(2) -0.012(3) C3 0.049(3) 0.050(3) 0.018(2) 0.003(2) 0.005(2) -0.005(3) C4 0.041(3) 0.031(3) 0.034(3) 0.012(2) 0.008(2) -0.000(2) C5 0.039(3) 0.046(3) 0.041(3) 0.004(2) 0.008(2) -0.005(3) C6 0.050(4) 0.059(4) 0.053(4) 0.006(3) 0.019(3) 0.004(3) C7 0.048(4) 0.067(5) 0.071(4) 0.021(3) 0.024(3) 0.010(3) C8 0.040(4) 0.054(4) 0.104(6) 0.023(4) 0.030(4) -0.006(3) C9 0.040(3) 0.041(3) 0.081(5) 0.015(3) 0.018(3) -0.005(3) C10 0.048(3) 0.030(2) 0.032(3) 0.001(2) 0.017(2) -0.006(2) C11 0.050(4) 0.041(3) 0.046(3) 0.005(3) 0.010(3) -0.004(3) C12 0.065(4) 0.042(3) 0.062(4) 0.006(3) 0.021(3) 0.014(3) C13 0.082(5) 0.031(3) 0.080(5) 0.010(3) 0.045(4) 0.011(3) C14 0.070(5) 0.031(3) 0.071(4) -0.006(3) 0.038(4) -0.010(3) C15 0.058(4) 0.036(3) 0.055(3) -0.005(3) 0.029(3) -0.011(3) C202 0.038(3) 0.060(3) 0.049(3) 0.017(3) 0.004(2) 0.005(3) C101 0.096(7) 0.063(6) 0.048(6) -0.027(5) 0.018(5) -0.023(6) C102 0.118(5) 0.036(3) 0.035(3) -0.014(2) 0.029(3) -0.020(3) C103 0.090(4) 0.044(3) 0.046(3) -0.012(3) 0.019(3) 0.019(3) C104 0.058(3) 0.062(4) 0.053(3) -0.025(3) 0.024(3) -0.002(3) C105 0.087(6) 0.056(6) 0.047(5) -0.012(5) 0.038(5) -0.000(6) C106 0.095(7) 0.061(7) 0.033(5) -0.018(5) 0.011(6) -0.002(6) C201 0.039(4) 0.051(4) 0.041(4) 0.008(4) -0.005(3) 0.001(4) C203 0.047(3) 0.041(3) 0.038(3) 0.010(2) 0.011(2) 0.016(2) C204 0.057(3) 0.033(3) 0.039(3) 0.007(2) 0.009(2) 0.007(2) C205 0.046(5) 0.042(4) 0.039(4) 0.012(3) 0.013(4) 0.006(4) C206 0.043(4) 0.056(5) 0.021(3) 0.005(3) -0.004(3) 0.004(4) N1 0.035(2) 0.029(2) 0.0243(18) -0.0024(16) 0.0053(16) -0.0078(17) O1 0.042(2) 0.0340(18) 0.0252(16) -0.0013(14) 0.0099(15) -0.0147(16) P1 0.0347(7) 0.0292(6) 0.0260(6) 0.0043(5) 0.0036(5) -0.0094(5) P2 0.0408(9) 0.0358(8) 0.1024(15) 0.0244(9) 0.0199(9) 0.0111(7) F1 0.039(2) 0.110(4) 0.220(7) 0.082(4) 0.005(3) -0.006(3) F2 0.187(7) 0.089(4) 0.168(6) -0.031(4) 0.082(6) -0.003(4) F3 0.088(3) 0.065(3) 0.118(4) 0.043(3) 0.019(3) 0.010(2) F4 0.052(3) 0.071(3) 0.215(7) 0.042(4) 0.030(3) 0.001(2) F5 0.187(6) 0.072(3) 0.152(5) 0.006(3) 0.106(5) 0.004(4) F6 0.085(3) 0.061(3) 0.158(5) 0.061(3) 0.002(3) -0.002(2) _refine_ls_extinction_coef 145.7(241) _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 . C202 . 2.247(6) yes Mo1 . C101 . 2.280(14) yes Mo1 . C102 . 2.263(6) yes Mo1 . C103 . 2.225(6) yes Mo1 . C104 . 2.293(6) yes Mo1 . C105 . 2.215(13) yes Mo1 . C106 . 2.252(15) yes Mo1 . C201 . 2.314(8) yes Mo1 . C203 . 2.238(5) yes Mo1 . C204 . 2.320(5) yes Mo1 . C205 . 2.289(8) yes Mo1 . C206 . 2.253(8) yes Mo1 . O1 . 2.161(3) yes Mo1 . P1 . 2.4123(12) yes C1 . C2 . 1.491(7) yes C1 . N1 . 1.347(6) yes C1 . O1 . 1.251(6) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . N1 . 1.482(6) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C3 . H33 . 1.000 no C4 . C5 . 1.389(8) yes C4 . C9 . 1.392(8) yes C4 . P1 . 1.824(6) yes C5 . C6 . 1.375(8) yes C5 . H51 . 1.000 no C6 . C7 . 1.382(9) yes C6 . H61 . 1.000 no C7 . C8 . 1.36(1) yes C7 . H71 . 1.000 no C8 . C9 . 1.388(9) yes C8 . H81 . 1.000 no C9 . H91 . 1.000 no C10 . C11 . 1.387(8) yes C10 . C15 . 1.412(7) yes C10 . P1 . 1.828(5) yes C11 . C12 . 1.397(8) yes C11 . H111 . 1.000 no C12 . C13 . 1.38(1) yes C12 . H121 . 1.000 no C13 . C14 . 1.36(1) yes C13 . H131 . 1.000 no C14 . C15 . 1.394(8) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C202 . C201 . 1.461(8) yes C202 . C203 . 1.421(6) yes C202 . H2021 . 1.000 no C202 . H2022 . 1.000 no C101 . C102 . 1.444(9) yes C101 . C106 . 1.408(9) yes C101 . H1011 . 1.000 no C102 . C103 . 1.398(7) yes C102 . H1021 . 1.000 no C102 . H1022 . 1.000 no C103 . C104 . 1.382(7) yes C103 . H1031 . 1.000 no C104 . C105 . 1.386(9) yes C104 . H1041 . 1.000 no C104 . H1042 . 1.000 no C105 . C106 . 1.399(9) yes C105 . H1051 . 1.000 no C106 . C206 . 0.879(17) yes C106 . H1061 . 1.000 no C201 . C206 . 1.411(8) yes C201 . H2011 . 1.000 no C203 . C204 . 1.406(6) yes C203 . H2031 . 1.000 no C204 . C205 . 1.404(7) yes C204 . H2041 . 1.000 no C204 . H2042 . 1.000 no C205 . C206 . 1.415(8) yes C205 . H2051 . 1.000 no C206 . H2061 . 1.000 no N1 . P1 . 1.735(4) yes P2 . F1 . 1.551(4) yes P2 . F2 . 1.562(5) yes P2 . F3 . 1.587(4) yes P2 . F4 . 1.578(4) yes P2 . F5 . 1.574(5) yes P2 . F6 . 1.560(4) yes H1061 . H2061 . 0.518 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 C202 . Mo1 . C101 . 77.1(4) yes C202 . Mo1 . C102 . 102.4(2) yes C101 . Mo1 . C102 . 37.1(3) yes C202 . Mo1 . C103 . 138.7(2) yes C101 . Mo1 . C103 . 66.7(4) yes C102 . Mo1 . C103 . 36.3(2) yes C202 . Mo1 . C104 . 147.8(2) yes C101 . Mo1 . C104 . 75.0(5) yes C102 . Mo1 . C104 . 62.7(2) yes C103 . Mo1 . C104 . 35.59(19) yes C202 . Mo1 . C105 . 115.8(3) yes C101 . Mo1 . C105 . 64.5(6) yes C102 . Mo1 . C105 . 76.0(4) yes C103 . Mo1 . C105 . 65.9(3) yes C104 . Mo1 . C105 . 35.8(2) yes C202 . Mo1 . C106 . 83.2(5) yes C101 . Mo1 . C106 . 36.2(3) yes C102 . Mo1 . C106 . 66.1(5) yes C103 . Mo1 . C106 . 79.5(5) yes C104 . Mo1 . C106 . 64.9(5) yes C202 . Mo1 . C201 . 37.3(2) yes C101 . Mo1 . C201 . 44.9(4) yes C102 . Mo1 . C201 . 79.4(3) yes C103 . Mo1 . C201 . 111.6(3) yes C104 . Mo1 . C201 . 110.6(3) yes C202 . Mo1 . C203 . 36.94(17) yes C101 . Mo1 . C203 . 110.9(4) yes C102 . Mo1 . C203 . 139.3(2) yes C103 . Mo1 . C203 . 174.5(2) yes C104 . Mo1 . C203 . 149.6(2) yes C202 . Mo1 . C204 . 63.7(2) yes C101 . Mo1 . C204 . 112.8(3) yes C102 . Mo1 . C204 . 149.6(2) yes C103 . Mo1 . C204 . 149.4(2) yes C104 . Mo1 . C204 . 113.8(2) yes C202 . Mo1 . C205 . 77.7(3) yes C101 . Mo1 . C205 . 86.4(3) yes C102 . Mo1 . C205 . 118.1(2) yes C103 . Mo1 . C205 . 117.8(3) yes C104 . Mo1 . C205 . 84.9(3) yes C202 . Mo1 . C206 . 67.0(3) yes C101 . Mo1 . C206 . 50.8(4) yes C102 . Mo1 . C206 . 85.8(3) yes C103 . Mo1 . C206 . 101.9(3) yes C104 . Mo1 . C206 . 82.9(3) yes C202 . Mo1 . O1 . 127.26(18) yes C101 . Mo1 . O1 . 155.3(4) yes C102 . Mo1 . O1 . 125.7(2) yes C103 . Mo1 . O1 . 91.2(2) yes C104 . Mo1 . O1 . 80.59(18) yes C202 . Mo1 . P1 . 87.53(15) yes C101 . Mo1 . P1 . 113.4(4) yes C102 . Mo1 . P1 . 88.00(16) yes C103 . Mo1 . P1 . 88.92(16) yes C104 . Mo1 . P1 . 118.24(18) yes C105 . Mo1 . C106 . 36.5(3) yes C105 . Mo1 . C201 . 82.0(4) yes C106 . Mo1 . C201 . 46.6(5) yes C105 . Mo1 . C203 . 118.1(3) yes C106 . Mo1 . C203 . 101.6(5) yes C201 . Mo1 . C203 . 66.4(3) yes C105 . Mo1 . C204 . 85.9(4) yes C106 . Mo1 . C204 . 84.8(5) yes C201 . Mo1 . C204 . 73.8(3) yes C203 . Mo1 . C204 . 35.87(16) yes C105 . Mo1 . C205 . 51.9(4) yes C106 . Mo1 . C205 . 52.3(4) yes C201 . Mo1 . C205 . 64.1(3) yes C203 . Mo1 . C205 . 66.4(2) yes C204 . Mo1 . C205 . 35.47(19) yes C105 . Mo1 . C206 . 48.8(4) yes C106 . Mo1 . C206 . 22.5(4) yes C201 . Mo1 . C206 . 36.0(2) yes C203 . Mo1 . C206 . 79.5(3) yes C204 . Mo1 . C206 . 64.0(3) yes C105 . Mo1 . O1 . 97.2(4) yes C106 . Mo1 . O1 . 132.4(4) yes C201 . Mo1 . O1 . 154.0(3) yes C203 . Mo1 . O1 . 91.95(17) yes C204 . Mo1 . O1 . 80.21(17) yes C105 . Mo1 . P1 . 153.8(3) yes C106 . Mo1 . P1 . 149.6(4) yes C201 . Mo1 . P1 . 115.8(2) yes C203 . Mo1 . P1 . 87.55(13) yes C204 . Mo1 . P1 . 116.59(13) yes C205 . Mo1 . C206 . 36.3(2) yes C205 . Mo1 . O1 . 94.9(2) yes C206 . Mo1 . O1 . 129.7(2) yes C205 . Mo1 . P1 . 152.05(19) yes C206 . Mo1 . P1 . 151.7(2) yes O1 . Mo1 . P1 . 75.29(9) yes C2 . C1 . N1 . 120.1(4) yes C2 . C1 . O1 . 119.2(4) yes N1 . C1 . O1 . 120.7(4) yes C1 . C2 . H21 . 109.5 no C1 . C2 . H22 . 109.5 no H21 . C2 . H22 . 109.5 no C1 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N1 . C3 . H31 . 109.5 no N1 . C3 . H32 . 109.5 no H31 . C3 . H32 . 109.5 no N1 . C3 . H33 . 109.5 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no C5 . C4 . C9 . 117.1(5) yes C5 . C4 . P1 . 119.7(4) yes C9 . C4 . P1 . 122.9(4) yes C4 . C5 . C6 . 122.0(5) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 119.0 no C5 . C6 . C7 . 119.2(6) yes C5 . C6 . H61 . 120.4 no C7 . C6 . H61 . 120.4 no C6 . C7 . C8 . 120.5(6) yes C6 . C7 . H71 . 119.8 no C8 . C7 . H71 . 119.8 no C7 . C8 . C9 . 120.0(6) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.0 no C4 . C9 . C8 . 121.1(6) yes C4 . C9 . H91 . 119.5 no C8 . C9 . H91 . 119.5 no C11 . C10 . C15 . 118.7(5) yes C11 . C10 . P1 . 120.7(4) yes C15 . C10 . P1 . 120.3(4) yes C10 . C11 . C12 . 120.2(5) yes C10 . C11 . H111 . 119.9 no C12 . C11 . H111 . 119.9 no C11 . C12 . C13 . 120.1(6) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 120.8(6) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 119.6 no C13 . C14 . C15 . 120.2(6) yes C13 . C14 . H141 . 119.9 no C15 . C14 . H141 . 119.9 no C10 . C15 . C14 . 120.0(6) yes C10 . C15 . H151 . 120.0 no C14 . C15 . H151 . 120.0 no Mo1 . C202 . C201 . 73.8(4) yes Mo1 . C202 . C203 . 71.2(3) yes C201 . C202 . C203 . 119.7(6) yes Mo1 . C202 . H2021 . 77.2 no C203 . C202 . H2021 . 120.0 no Mo1 . C202 . H2022 . 122.9 no C201 . C202 . H2022 . 120.1 no C203 . C202 . H2022 . 120.0 no H2021 . C202 . H2022 . 120.0 no Mo1 . C101 . C102 . 70.8(6) yes Mo1 . C101 . C106 . 70.8(8) yes C102 . C101 . C106 . 119.3(14) yes Mo1 . C101 . H1011 . 130.5 no C102 . C101 . H1011 . 120.3 no C106 . C101 . H1011 . 120.4 no Mo1 . C102 . C101 . 72.1(6) yes Mo1 . C102 . C103 . 70.4(3) yes C101 . C102 . C103 . 121.4(8) yes Mo1 . C102 . H1021 . 78.2 no C103 . C102 . H1021 . 120.0 no Mo1 . C102 . H1022 . 122.7 no C101 . C102 . H1022 . 117.9 no C103 . C102 . H1022 . 120.0 no H1021 . C102 . H1022 . 120.0 no Mo1 . C103 . C102 . 73.4(4) yes Mo1 . C103 . C104 . 74.9(4) yes C102 . C103 . C104 . 117.0(6) yes Mo1 . C103 . H1031 . 121.5 no C102 . C103 . H1031 . 121.5 no C104 . C103 . H1031 . 121.5 no Mo1 . C104 . C103 . 69.5(3) yes Mo1 . C104 . C105 . 69.0(6) yes C103 . C104 . C105 . 121.5(9) yes Mo1 . C104 . H1041 . 123.8 no C103 . C104 . H1041 . 120.0 no C105 . C104 . H1041 . 117.0 no Mo1 . C104 . H1042 . 78.1 no C103 . C104 . H1042 . 120.0 no H1041 . C104 . H1042 . 120.0 no Mo1 . C105 . C104 . 75.2(6) yes Mo1 . C105 . C106 . 73.2(8) yes C104 . C105 . C106 . 122.1(14) yes Mo1 . C105 . H1051 . 124.2 no C104 . C105 . H1051 . 119.0 no C106 . C105 . H1051 . 118.9 no Mo1 . C106 . C101 . 73.0(8) yes Mo1 . C106 . C105 . 70.3(8) yes C101 . C106 . C105 . 117.3(16) yes Mo1 . C106 . C206 . 78.8(12) yes C101 . C106 . C206 . 114.4(16) yes C105 . C106 . C206 . 106.0(14) yes Mo1 . C106 . H1061 . 127.3 no C101 . C106 . H1061 . 121.3 no C105 . C106 . H1061 . 121.3 no C206 . C106 . H1061 . 48.6 no Mo1 . C201 . C202 . 68.8(4) yes Mo1 . C201 . C206 . 69.6(5) yes C202 . C201 . C206 . 119.8(7) yes Mo1 . C201 . H2011 . 135.0 no C202 . C201 . H2011 . 120.1 no C206 . C201 . H2011 . 120.1 no Mo1 . C203 . C202 . 71.9(3) yes Mo1 . C203 . C204 . 75.3(3) yes C202 . C203 . C204 . 117.0(5) yes Mo1 . C203 . H2031 . 122.7 no C202 . C203 . H2031 . 121.5 no C204 . C203 . H2031 . 121.5 no Mo1 . C204 . C203 . 68.8(3) yes Mo1 . C204 . C205 . 71.0(4) yes C203 . C204 . C205 . 123.7(6) yes Mo1 . C204 . H2041 . 125.4 no C203 . C204 . H2041 . 120.0 no C205 . C204 . H2041 . 115.1 no Mo1 . C204 . H2042 . 77.4 no C203 . C204 . H2042 . 120.0 no H2041 . C204 . H2042 . 120.0 no Mo1 . C205 . C204 . 73.5(4) yes Mo1 . C205 . C206 . 70.5(5) yes C204 . C205 . C206 . 118.6(7) yes Mo1 . C205 . H2051 . 127.3 no C204 . C205 . H2051 . 120.7 no C206 . C205 . H2051 . 120.7 no Mo1 . C206 . C106 . 78.7(12) yes Mo1 . C206 . C201 . 74.4(5) yes C106 . C206 . C201 . 101.6(12) yes Mo1 . C206 . C205 . 73.2(5) yes C106 . C206 . C205 . 119.8(13) yes C201 . C206 . C205 . 119.6(8) yes Mo1 . C206 . H2061 . 123.6 no C201 . C206 . H2061 . 120.2 no C205 . C206 . H2061 . 120.2 no C1 . N1 . C3 . 120.7(4) yes C1 . N1 . P1 . 116.4(3) yes C3 . N1 . P1 . 122.8(3) yes Mo1 . O1 . C1 . 125.1(3) yes Mo1 . P1 . C4 . 120.97(16) yes Mo1 . P1 . C10 . 119.99(16) yes C4 . P1 . C10 . 106.5(2) yes Mo1 . P1 . N1 . 101.64(13) yes C4 . P1 . N1 . 102.3(2) yes C10 . P1 . N1 . 101.8(2) yes F1 . P2 . F2 . 90.6(3) yes F1 . P2 . F3 . 91.1(3) yes F2 . P2 . F3 . 91.3(4) yes F1 . P2 . F4 . 179.3(3) yes F2 . P2 . F4 . 89.1(3) yes F3 . P2 . F4 . 88.2(2) yes F1 . P2 . F5 . 91.3(3) yes F2 . P2 . F5 . 177.5(3) yes F3 . P2 . F5 . 87.1(3) yes F4 . P2 . F5 . 88.9(3) yes F1 . P2 . F6 . 90.4(2) yes F2 . P2 . F6 . 89.8(4) yes F3 . P2 . F6 . 178.1(3) yes F4 . P2 . F6 . 90.3(2) yes F5 . P2 . F6 . 91.8(4) yes C101 . H1021 . C102 . 153.7 no C104 . H1042 . C105 . 139.4 no C106 . H1061 . C206 . 57.6 no C106 . H1061 . H2061 . 46.3 no C206 . H1061 . H2061 . 98.7 no C202 . H2021 . C201 . 167.9 no C204 . H2042 . C205 . 143.0 no C106 . H2061 . C206 . 58.4 no C106 . H2061 . H1061 . 103.4 no C206 . H2061 . H1061 . 50.5 no #===END data_Compound4a _database_code_CSD 169298 _audit_creation_date 01-02-10 _audit_creation_method CRYSTALS_ver_12-03-99 # 9281505 Compound X # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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 14.8887(8) _cell_angle_alpha 90 _cell_length_b 16.5295(8) _cell_angle_beta 90 _cell_length_c 16.1773(9) _cell_angle_gamma 90 _cell_volume 3981.3 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'C m c a ' 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' 'x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' 'x+1/2,-y,z+1/2' '-x+1/2,y,-z+1/2' '-x,-y+1/2,z+1/2' 'x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 'x+1/2,y,-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' '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' '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 H24 Mo1 N1 O1 P1 ' _chemical_formula_moiety ' C23 H24 Mo1 N1 O1 P1 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 457.36 _cell_measurement_reflns_used 2391 _cell_measurement_theta_min 3 _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 0.08 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1854.035 _exptl_absorpt_coefficient_mu 0.752 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.94 _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 4476 _reflns_number_total 2362 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections with Friedels Law is 2362 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2280 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 1511 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.58 _refine_diff_density_max 0.64 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1511 _refine_ls_number_parameters 145 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0387 _refine_ls_goodness_of_fit_ref 1.0575 _refine_ls_shift/su_max 0.002028 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.507 0.919E-01 0.212 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; the phenyl and allyl groups are disordered by symmetry, such that three of the C atoms overlap. The overlapping positions could not be resolved. Attempts to refine the structure in the subgroup C 2 c b lead to unstable refinement. All H atoms were positioned geometrically following each cycle of refinement ; # 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 1.0000 -0.00422(3) 0.81119(3) 0.0241 1.0000 Uani N1 1.0000 0.1931(3) 0.7836(3) 0.0317 1.0000 Uani P1 1.0000 0.11341(8) 0.71934(8) 0.0257 1.0000 Uani O1 1.0000 0.1005(2) 0.8902(2) 0.0413 1.0000 Uani C1 0.9222(6) -0.1240(5) 0.7713(5) 0.0406 1.0000 Uani C2 0.9569(5) -0.1316(4) 0.8509(5) 0.0337 1.0000 Uani C3 0.9294(6) -0.0757(4) 0.9137(5) 0.0340 1.0000 Uani C4 0.8691(3) -0.0247(3) 0.8839(3) 0.0541 0.5000 Uani C5 0.8504(3) -0.0020(2) 0.8026(3) 0.0430 0.5000 Uani C6 0.8833(4) -0.0538(3) 0.7391(3) 0.0527 0.5000 Uani C7 1.0000 0.1733(3) 0.8612(3) 0.0302 1.0000 Uani C8 1.0000 0.2386(3) 0.9264(4) 0.0385 1.0000 Uani C9 0.9044(3) 0.1343(2) 0.6511(2) 0.0284 1.0000 Uani C10 0.8424(3) 0.1918(3) 0.6724(3) 0.0558 1.0000 Uani C11 0.7671(4) 0.2064(3) 0.6237(4) 0.0682 1.0000 Uani C12 0.7528(3) 0.1636(3) 0.5532(3) 0.0446 1.0000 Uani C13 0.8140(4) 0.1069(4) 0.5306(3) 0.0619 1.0000 Uani C14 0.8887(3) 0.0914(3) 0.5795(3) 0.0622 1.0000 Uani H11 0.9254 -0.1725 0.7345 0.0487 0.5000 Uiso H21 0.9998 -0.1757 0.8641 0.0404 0.5000 Uiso H31 0.9525 -0.0753 0.9718 0.0409 0.5000 Uiso H41 0.9040 -0.0752 0.8952 0.0649 0.5000 Uiso H42 0.8475 0.0096 0.9308 0.0649 1.0000 Uiso H51 0.8157 0.0482 0.7896 0.0516 1.0000 Uiso H61 0.9179 -0.1037 0.7538 0.0633 0.5000 Uiso H62 0.8718 -0.0404 0.6797 0.0633 1.0000 Uiso H81 1.0000 0.2132 0.9825 0.0462 1.0000 Uiso H82 1.0548 0.2730 0.9199 0.0462 1.0000 Uiso H101 0.8513 0.2239 0.7242 0.0670 1.0000 Uiso H111 0.7230 0.2488 0.6407 0.0818 1.0000 Uiso H121 0.6982 0.1736 0.5186 0.0535 1.0000 Uiso H131 0.8052 0.0758 0.4782 0.0742 1.0000 Uiso H141 0.9319 0.0483 0.5624 0.0746 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 0.0273(2) 0.02102(19) 0.02389(19) -0.0006(2) 0.0000 0.0000 N1 0.035(2) 0.023(2) 0.037(2) -0.0001(18) 0.0000 0.0000 P1 0.0290(6) 0.0224(6) 0.0257(6) 0.0000(5) 0.0000 0.0000 O1 0.077(3) 0.0229(18) 0.0246(18) -0.0016(16) 0.0000 0.0000 C1 0.045(5) 0.024(3) 0.053(5) -0.008(3) 0.015(4) -0.015(3) C2 0.034(4) 0.025(3) 0.042(4) 0.004(3) 0.001(3) -0.000(3) C3 0.038(4) 0.033(4) 0.032(4) 0.003(3) 0.003(3) 0.004(3) C4 0.031(2) 0.070(3) 0.062(3) 0.032(2) 0.002(2) -0.005(2) C5 0.0316(17) 0.0316(17) 0.066(3) 0.009(2) -0.0138(19) -0.0055(18) C6 0.064(3) 0.0332(19) 0.061(3) -0.002(2) -0.030(3) -0.006(2) C7 0.036(3) 0.021(2) 0.033(3) -0.006(2) 0.0000 0.0000 C8 0.046(3) 0.035(3) 0.034(3) -0.004(2) 0.0000 0.0000 C9 0.0317(18) 0.0249(16) 0.0285(18) 0.0061(14) -0.0023(16) -0.0039(14) C10 0.048(3) 0.060(3) 0.059(3) -0.021(2) -0.021(2) 0.022(2) C11 0.059(3) 0.063(3) 0.082(4) -0.020(3) -0.031(3) 0.025(3) C12 0.036(2) 0.045(2) 0.052(2) 0.019(2) -0.013(2) -0.0097(19) C13 0.055(3) 0.086(4) 0.045(2) -0.016(3) -0.017(2) 0.006(3) C14 0.050(3) 0.081(4) 0.056(3) -0.030(3) -0.025(2) 0.024(3) _refine_ls_extinction_coef 146.486 _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 . 2.4471(14) yes Mo1 . O1 . 2.152(4) yes Mo1 . C1 . 2.383(7) yes Mo1 . C1 5_755 2.383(7) yes Mo1 . C2 . 2.294(7) yes Mo1 . C2 5_755 2.294(7) yes Mo1 . C3 . 2.292(7) yes Mo1 . C3 5_755 2.292(7) yes Mo1 . C4 . 2.302(5) yes Mo1 . C4 5_755 2.302(5) yes Mo1 . C5 . 2.231(4) yes Mo1 . C5 5_755 2.231(4) yes Mo1 . C6 . 2.248(4) yes Mo1 . C6 5_755 2.248(4) yes N1 . P1 . 1.679(4) yes N1 . C7 . 1.298(7) yes P1 . C9 . 1.834(4) yes P1 . C9 5_755 1.834(4) yes O1 . C7 . 1.291(6) yes C1 . C2 . 1.393(12) yes C1 . C6 . 1.40(1) yes C1 . H11 . 1.000 no C2 . C3 . 1.433(11) yes C2 . H21 . 1.000 no C3 . C4 . 1.324(9) yes C3 . H31 . 1.000 no C4 . C5 . 1.395(6) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . C6 . 1.425(7) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . C8 . 1.508(7) yes C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H82 5_755 1.000 no C9 . C10 . 1.369(6) yes C9 . C14 . 1.377(6) yes C10 . C11 . 1.391(7) yes C10 . H101 . 1.000 no C11 . C12 . 1.359(6) yes C11 . H111 . 1.000 no C12 . C13 . 1.357(7) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(7) yes C13 . H131 . 1.000 no C14 . H141 . 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 P1 . Mo1 . O1 . 73.8(1) yes P1 . Mo1 . C1 . 119.7(2) yes O1 . Mo1 . C1 . 146.0(2) yes P1 . Mo1 . C1 5_755 119.7(2) yes O1 . Mo1 . C1 5_755 146.0(2) yes C1 . Mo1 . C1 5_755 58.2(4) yes P1 . Mo1 . C2 . 154.1(2) yes O1 . Mo1 . C2 . 124.9(2) yes C1 . Mo1 . C2 . 34.6(3) yes C1 5_755 Mo1 . C2 . 56.5(3) yes P1 . Mo1 . C2 5_755 154.1(2) yes O1 . Mo1 . C2 5_755 124.9(2) yes C1 . Mo1 . C2 5_755 56.5(3) yes C1 5_755 Mo1 . C2 5_755 34.6(3) yes C2 . Mo1 . C2 5_755 32.5(4) yes P1 . Mo1 . C3 . 148.12(19) yes O1 . Mo1 . C3 . 89.1(2) yes C1 . Mo1 . C3 . 62.9(3) yes C1 5_755 Mo1 . C3 . 89.4(3) yes C2 . Mo1 . C3 . 36.4(3) yes P1 . Mo1 . C3 5_755 148.12(19) yes O1 . Mo1 . C3 5_755 89.1(2) yes C1 . Mo1 . C3 5_755 89.4(3) yes C1 5_755 Mo1 . C3 5_755 62.9(3) yes C2 . Mo1 . C3 5_755 56.8(3) yes P1 . Mo1 . C4 . 115.27(12) yes O1 . Mo1 . C4 . 79.32(15) yes C1 . Mo1 . C4 . 66.7(2) yes C1 5_755 Mo1 . C4 . 115.3(3) yes C2 . Mo1 . C4 . 59.0(2) yes P1 . Mo1 . C4 5_755 115.27(12) yes O1 . Mo1 . C4 5_755 79.32(15) yes C1 . Mo1 . C4 5_755 115.3(3) yes C1 5_755 Mo1 . C4 5_755 66.7(2) yes C2 . Mo1 . C4 5_755 87.6(2) yes P1 . Mo1 . C5 . 87.1(1) yes O1 . Mo1 . C5 . 91.37(11) yes C1 . Mo1 . C5 . 60.8(2) yes C1 5_755 Mo1 . C5 . 118.8(2) yes C2 . Mo1 . C5 . 75.7(2) yes P1 . Mo1 . C5 5_755 87.1(1) yes O1 . Mo1 . C5 5_755 91.37(11) yes C1 . Mo1 . C5 5_755 118.8(2) yes C1 5_755 Mo1 . C5 5_755 60.8(2) yes C2 . Mo1 . C5 5_755 108.2(2) yes P1 . Mo1 . C6 . 88.55(12) yes O1 . Mo1 . C6 . 127.00(13) yes C1 . Mo1 . C6 . 35.0(2) yes C1 5_755 Mo1 . C6 . 86.1(2) yes C2 . Mo1 . C6 . 66.1(2) yes P1 . Mo1 . C6 5_755 88.55(12) yes O1 . Mo1 . C6 5_755 127.00(13) yes C1 . Mo1 . C6 5_755 86.1(2) yes C1 5_755 Mo1 . C6 5_755 35.0(2) yes C2 . Mo1 . C6 5_755 91.5(2) yes C2 5_755 Mo1 . C3 . 56.8(3) yes C2 5_755 Mo1 . C3 5_755 36.4(3) yes C3 . Mo1 . C3 5_755 54.6(4) yes C2 5_755 Mo1 . C4 . 87.6(2) yes C3 . Mo1 . C4 . 33.5(2) yes C3 5_755 Mo1 . C4 . 86.7(2) yes C2 5_755 Mo1 . C4 5_755 59.0(2) yes C3 . Mo1 . C4 5_755 86.7(2) yes C3 5_755 Mo1 . C4 5_755 33.5(2) yes C4 . Mo1 . C4 5_755 115.8(2) yes C2 5_755 Mo1 . C5 . 108.2(2) yes C3 . Mo1 . C5 . 66.2(2) yes C3 5_755 Mo1 . C5 . 120.7(2) yes C4 . Mo1 . C5 . 35.80(16) yes C4 5_755 Mo1 . C5 . 151.57(17) yes C2 5_755 Mo1 . C5 5_755 75.7(2) yes C3 . Mo1 . C5 5_755 120.7(2) yes C3 5_755 Mo1 . C5 5_755 66.2(2) yes C4 . Mo1 . C5 5_755 151.57(17) yes C4 5_755 Mo1 . C5 5_755 35.80(16) yes C2 5_755 Mo1 . C6 . 91.5(2) yes C3 . Mo1 . C6 . 80.4(2) yes C3 5_755 Mo1 . C6 . 122.8(2) yes C4 . Mo1 . C6 . 63.7(2) yes C4 5_755 Mo1 . C6 . 150.03(19) yes C2 5_755 Mo1 . C6 5_755 66.1(2) yes C3 . Mo1 . C6 5_755 122.8(2) yes C3 5_755 Mo1 . C6 5_755 80.4(2) yes C4 . Mo1 . C6 5_755 150.03(19) yes C4 5_755 Mo1 . C6 5_755 63.7(2) yes C5 . Mo1 . C5 5_755 172.6(2) yes C5 . Mo1 . C6 . 37.09(17) yes C5 5_755 Mo1 . C6 . 138.16(19) yes C5 . Mo1 . C6 5_755 138.16(19) yes C5 5_755 Mo1 . C6 5_755 37.09(17) yes C6 . Mo1 . C6 5_755 101.2(3) yes P1 . N1 . C7 . 113.6(3) yes Mo1 . P1 . N1 . 104.33(16) yes Mo1 . P1 . C9 . 121.02(11) yes N1 . P1 . C9 . 103.01(15) yes Mo1 . P1 . C9 5_755 121.02(11) yes N1 . P1 . C9 5_755 103.01(15) yes C9 . P1 . C9 5_755 101.7(2) yes Mo1 . O1 . C7 . 122.3(3) yes Mo1 . C1 . C2 . 69.2(4) yes Mo1 . C1 . C6 . 67.2(3) yes C2 . C1 . C6 . 125.0(7) yes Mo1 . C1 . H11 . 143.5 no C2 . C1 . H11 . 117.5 no C6 . C1 . H11 . 117.5 no Mo1 . C2 . C1 . 76.2(4) yes Mo1 . C2 . C2 5_755 73.75(19) yes Mo1 . C2 . C3 . 71.7(4) yes C1 . C2 . C3 . 119.4(7) yes Mo1 . C2 . H21 . 123.5 no C1 . C2 . H21 . 120.3 no C3 . C2 . H21 . 120.3 no Mo1 . C3 . C2 . 71.8(4) yes Mo1 . C3 . C4 . 73.6(4) yes C2 . C3 . C4 . 110.2(7) yes Mo1 . C3 . H31 . 121.2 no C2 . C3 . H31 . 124.9 no C4 . C3 . H31 . 124.9 no Mo1 . C4 . C3 . 72.9(4) yes Mo1 . C4 . C5 . 69.3(2) yes C3 . C4 . C5 . 130.5(6) yes Mo1 . C4 . H41 . 77.1 no C5 . C4 . H41 . 120.0 no Mo1 . C4 . H42 . 125.2 no C3 . C4 . H42 . 107.5 no C5 . C4 . H42 . 120.0 no H41 . C4 . H42 . 120.0 no Mo1 . C5 . C4 . 74.9(2) yes Mo1 . C5 . C6 . 72.1(2) yes C4 . C5 . C6 . 116.8(4) yes Mo1 . C5 . H51 . 122.9 no C4 . C5 . H51 . 121.6 no C6 . C5 . H51 . 121.6 no Mo1 . C6 . C1 . 77.8(4) yes Mo1 . C6 . C5 . 70.8(2) yes C1 . C6 . C5 . 111.8(5) yes Mo1 . C6 . H61 . 77.2 no C5 . C6 . H61 . 120.0 no Mo1 . C6 . H62 . 123.3 no C1 . C6 . H62 . 127.9 no C5 . C6 . H62 . 120.0 no H61 . C6 . H62 . 120.0 no N1 . C7 . O1 . 125.9(5) yes N1 . C7 . C8 . 119.7(5) yes O1 . C7 . C8 . 114.4(5) yes C7 . C8 . H81 . 109.5 no C7 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no C7 . C8 . H82 5_755 109.5 no H81 . C8 . H82 5_755 109.5 no H82 . C8 . H82 5_755 109.5 no P1 . C9 . C10 . 120.1(3) yes P1 . C9 . C14 . 122.8(3) yes C10 . C9 . C14 . 117.0(4) yes C9 . C10 . C11 . 121.4(4) yes C9 . C10 . H101 . 119.3 no C11 . C10 . H101 . 119.3 no C10 . C11 . C12 . 120.8(5) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 118.7(4) yes C11 . C12 . H121 . 120.7 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 120.8(4) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 119.6 no C9 . C14 . C13 . 121.4(4) yes C9 . C14 . H141 . 119.3 no C13 . C14 . H141 . 119.3 no C2 . H21 . C2 5_755 80.4 no C3 . H41 . C4 . 122.5 no C1 . H61 . C6 . 148.1 no