Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_yin198 _database_code_depnum_ccdc_archive 'CCDC 281546' # CIF produced by WinGX routine CIF_UPDATE # Created on 2003-08-25 at 14:03:36 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : yin198 #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of crystallographer #Blacque, Olivier #Anorganisch-Chemisches Institut der #Universit\"at Z\"urich #Winterthurerstrasee 190 #CH-8057 Z\"urich #----------------------------------------------------------------------------# _audit_creation_date 2003-08-25T14:03:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; trans-hydrido-nitrosyl-tetrakis(trimethylphosphine)molybdenum(0) ; _chemical_formula_moiety 'C12 H37 Mo N O P4' _chemical_formula_sum 'C12 H37 Mo N O P4' _chemical_formula_weight 431.25 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.5261(7) _cell_length_b 15.6484(15) _cell_length_c 14.6607(11) _cell_angle_alpha 90 _cell_angle_beta 98.876(9) _cell_angle_gamma 90 _cell_volume 2159.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8001 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 30.2 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.968 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '\f oscillation scan' _diffrn_standards_number 200 _diffrn_standards_interval_count image _diffrn_standards_interval_time 7 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_unetI/netI 0.0667 _diffrn_reflns_number 16665 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 30.29 _diffrn_reflns_theta_full 30.29 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _reflns_number_total 6197 _reflns_number_gt 5035 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'IPDS software (Stoe & Cie, 1999)' _computing_cell_refinement 'IPDS software (Stoe & Cie, 1999)' _computing_data_reduction 'IPDS software (Stoe & Cie, 1999)' _computing_structure_solution ; Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565. ; _computing_publication_material ; Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6197 _refine_ls_number_parameters 188 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_diff_density_max 0.46 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo -1.02298(2) -0.356683(16) -0.25514(2) 0.01929(6) Uani 1 1 d . . . H H -1.006(4) -0.466(2) -0.175(2) 0.021(10) Uiso 1 1 d . . . P1 P -0.85826(10) -0.41312(6) -0.35380(6) 0.02270(19) Uani 1 1 d . . . P2 P -1.20839(10) -0.45891(6) -0.32007(7) 0.02478(19) Uani 1 1 d . . . P3 P -1.19178(10) -0.27713(6) -0.17616(6) 0.0241(2) Uani 1 1 d . . . P4 P -0.82846(10) -0.32218(6) -0.13224(6) 0.02308(19) Uani 1 1 d . . . N N -1.0284(4) -0.2637(2) -0.3310(2) 0.0285(7) Uani 1 1 d . . . O O -1.0242(4) -0.2005(2) -0.3790(3) 0.0600(10) Uani 1 1 d . . . C1 C -0.9333(5) -0.4232(3) -0.4765(3) 0.0343(9) Uani 1 1 d . . . H1A H -1.0066 -0.4659 -0.4837 0.045 Uiso 1 1 calc R . . H1B H -0.8598 -0.4396 -0.511 0.045 Uiso 1 1 calc R . . H1C H -0.9728 -0.3693 -0.499 0.045 Uiso 1 1 calc R . . C2 C -0.7606(5) -0.5132(3) -0.3328(3) 0.0348(9) Uani 1 1 d . . . H2A H -0.7055 -0.5229 -0.3814 0.045 Uiso 1 1 calc R . . H2B H -0.8264 -0.5594 -0.3312 0.045 Uiso 1 1 calc R . . H2C H -0.6985 -0.51 -0.2747 0.045 Uiso 1 1 calc R . . C3 C -0.7131(5) -0.3391(3) -0.3659(3) 0.0367(10) Uani 1 1 d . . . H3A H -0.6572 -0.3619 -0.4093 0.048 Uiso 1 1 calc R . . H3B H -0.6543 -0.3319 -0.307 0.048 Uiso 1 1 calc R . . H3C H -0.7519 -0.2849 -0.3875 0.048 Uiso 1 1 calc R . . C4 C -1.3420(5) -0.4894(3) -0.2491(3) 0.0389(10) Uani 1 1 d . . . H4A H -1.2957 -0.507 -0.1892 0.051 Uiso 1 1 calc R . . H4B H -1.3979 -0.5359 -0.2781 0.051 Uiso 1 1 calc R . . H4C H -1.4026 -0.4415 -0.2428 0.051 Uiso 1 1 calc R . . C5 C -1.1474(5) -0.5670(2) -0.3435(3) 0.0390(10) Uani 1 1 d . . . H5A H -1.0865 -0.5642 -0.3899 0.051 Uiso 1 1 calc R . . H5B H -1.228 -0.6024 -0.3651 0.051 Uiso 1 1 calc R . . H5C H -1.0959 -0.5908 -0.2879 0.051 Uiso 1 1 calc R . . C6 C -1.3234(5) -0.4347(3) -0.4292(3) 0.0433(11) Uani 1 1 d . . . H6A H -1.3849 -0.4824 -0.447 0.056 Uiso 1 1 calc R . . H6B H -1.2659 -0.424 -0.4763 0.056 Uiso 1 1 calc R . . H6C H -1.3796 -0.3851 -0.4215 0.056 Uiso 1 1 calc R . . C7 C -1.2612(5) -0.3159(3) -0.0746(3) 0.0402(10) Uani 1 1 d . . . H7A H -1.3279 -0.2752 -0.0573 0.052 Uiso 1 1 calc R . . H7C H -1.308 -0.3697 -0.0885 0.052 Uiso 1 1 calc R . . C8 C -1.3565(4) -0.2477(3) -0.2517(3) 0.0370(10) Uani 1 1 d . . . H8A H -1.334 -0.2158 -0.3035 0.048 Uiso 1 1 calc R . . H8B H -1.4143 -0.2134 -0.2179 0.048 Uiso 1 1 calc R . . H8C H -1.4075 -0.2985 -0.2734 0.048 Uiso 1 1 calc R . . C9 C -1.1327(5) -0.1694(3) -0.1400(3) 0.0348(9) Uani 1 1 d . . . H9A H -1.2115 -0.1375 -0.124 0.045 Uiso 1 1 calc R . . H9B H -1.0964 -0.1413 -0.1897 0.045 Uiso 1 1 calc R . . H9C H -1.0593 -0.173 -0.0873 0.045 Uiso 1 1 calc R . . C10 C -0.6755(5) -0.3947(3) -0.1114(3) 0.0365(9) Uani 1 1 d . . . H10A H -0.6139 -0.3776 -0.0564 0.047 Uiso 1 1 calc R . . H10B H -0.6244 -0.3925 -0.1629 0.047 Uiso 1 1 calc R . . H10C H -0.7081 -0.452 -0.1041 0.047 Uiso 1 1 calc R . . C11 C -0.8676(5) -0.3184(3) -0.0131(2) 0.0352(9) Uani 1 1 d . . . H11A H -0.928 -0.2704 -0.0064 0.046 Uiso 1 1 calc R . . H11B H -0.7805 -0.3127 0.0292 0.046 Uiso 1 1 calc R . . H11C H -0.9148 -0.3701 0.0001 0.046 Uiso 1 1 calc R . . C12 C -0.7367(5) -0.2203(3) -0.1388(3) 0.0424(11) Uani 1 1 d . . . H12A H -0.6596 -0.2162 -0.0884 0.055 Uiso 1 1 calc R . . H12B H -0.8021 -0.1742 -0.1352 0.055 Uiso 1 1 calc R . . H12C H -0.7003 -0.217 -0.1962 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.01845(13) 0.02002(12) 0.01973(11) -0.00002(16) 0.00399(8) 0.00077(16) P1 0.0223(5) 0.0219(4) 0.0252(4) 0.0016(3) 0.0077(4) 0.0025(4) P2 0.0227(5) 0.0213(4) 0.0310(5) -0.0005(4) 0.0062(4) -0.0015(4) P3 0.0252(5) 0.0235(4) 0.0249(4) -0.0003(4) 0.0076(4) 0.0036(4) P4 0.0241(5) 0.0215(4) 0.0232(4) 0.0008(3) 0.0021(4) -0.0031(4) N 0.0339(19) 0.0243(16) 0.0279(16) 0.0053(12) 0.0064(13) 0.0030(13) O 0.069(3) 0.048(2) 0.064(2) 0.0372(17) 0.0118(19) 0.0092(18) C1 0.035(2) 0.040(2) 0.0294(19) 0.0015(16) 0.0082(16) 0.0032(18) C2 0.030(2) 0.032(2) 0.042(2) -0.0011(17) 0.0055(17) 0.0099(17) C3 0.030(2) 0.044(3) 0.040(2) 0.0045(17) 0.0152(18) -0.0066(17) C4 0.035(3) 0.033(2) 0.052(3) -0.0030(19) 0.016(2) -0.0097(18) C5 0.045(3) 0.0201(17) 0.055(3) -0.0073(17) 0.016(2) -0.0050(17) C6 0.042(3) 0.046(3) 0.039(2) 0.002(2) -0.004(2) -0.005(2) C7 0.049(3) 0.042(2) 0.033(2) 0.0022(18) 0.0190(19) 0.004(2) C8 0.025(2) 0.041(2) 0.044(2) -0.0014(18) 0.0028(18) 0.0115(18) C9 0.037(3) 0.0293(19) 0.039(2) -0.0049(16) 0.0063(18) 0.0043(17) C10 0.026(2) 0.041(2) 0.039(2) 0.0021(18) -0.0052(18) 0.0049(18) C11 0.033(2) 0.045(2) 0.0266(19) 0.0031(16) 0.0018(16) 0.0009(18) C12 0.047(3) 0.032(2) 0.049(3) -0.0040(19) 0.010(2) -0.017(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N 1.827(3) . ? Mo P4 2.4375(10) . ? Mo P1 2.4566(10) . ? Mo P3 2.4597(10) . ? Mo P2 2.4629(10) . ? Mo H 2.06(4) . ? P1 C2 1.823(4) . ? P1 C3 1.832(4) . ? P1 C1 1.838(4) . ? P2 C4 1.827(4) . ? P2 C6 1.834(4) . ? P2 C5 1.838(4) . ? P3 C7 1.824(4) . ? P3 C9 1.829(4) . ? P3 C8 1.834(4) . ? P4 C12 1.828(4) . ? P4 C10 1.835(4) . ? P4 C11 1.843(4) . ? N O 1.218(4) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Mo P4 102.73(11) . . ? N Mo P1 83.61(11) . . ? P4 Mo P1 91.89(3) . . ? N Mo P3 85.66(11) . . ? P4 Mo P3 91.01(3) . . ? P1 Mo P3 169.25(3) . . ? N Mo P2 109.31(11) . . ? P4 Mo P2 147.96(3) . . ? P1 Mo P2 91.38(3) . . ? P3 Mo P2 91.65(3) . . ? N Mo H 175.7(11) . . ? P4 Mo H 77.2(11) . . ? P1 Mo H 92.1(11) . . ? P3 Mo H 98.6(11) . . ? P2 Mo H 70.8(11) . . ? C2 P1 C3 100.7(2) . . ? C2 P1 C1 101.7(2) . . ? C3 P1 C1 98.3(2) . . ? C2 P1 Mo 124.40(15) . . ? C3 P1 Mo 112.93(14) . . ? C1 P1 Mo 114.84(14) . . ? C4 P2 C6 100.1(2) . . ? C4 P2 C5 97.7(2) . . ? C6 P2 C5 101.0(2) . . ? C4 P2 Mo 118.09(15) . . ? C6 P2 Mo 119.96(16) . . ? C5 P2 Mo 116.20(15) . . ? C7 P3 C9 101.8(2) . . ? C7 P3 C8 101.1(2) . . ? C9 P3 C8 98.0(2) . . ? C7 P3 Mo 124.19(16) . . ? C9 P3 Mo 114.11(15) . . ? C8 P3 Mo 113.77(14) . . ? C12 P4 C10 100.0(2) . . ? C12 P4 C11 101.0(2) . . ? C10 P4 C11 97.7(2) . . ? C12 P4 Mo 118.00(16) . . ? C10 P4 Mo 118.65(14) . . ? C11 P4 Mo 117.76(14) . . ? O N Mo 176.2(3) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? data_yin157 _database_code_depnum_ccdc_archive 'CCDC 281547' # CIF produced by WinGX routine CIF_UPDATE # Created on 2003-07-24 at 11:20:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : yin157 _audit_creation_date 2003-07-24T11:20:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; trans-diphenylmethoxy-nitrosyl-tetrakis(trimethylphosphine)molybdenum(0) ; _chemical_formula_moiety 'C25 H47 Mo N O2 P4' _chemical_formula_sum 'C25 H47 Mo N O2 P4' _chemical_formula_weight 613.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0261(9) _cell_length_b 16.7255(10) _cell_length_c 18.7690(18) _cell_angle_alpha 90 _cell_angle_beta 94.046(11) _cell_angle_gamma 90 _cell_volume 3139.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 30.25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'block cut from very large crystal' _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.8 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '\f rotation scan' _diffrn_standards_number 218 _diffrn_standards_interval_count image _diffrn_standards_interval_time 1 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_number 44839 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 30.34 _diffrn_reflns_theta_full 30.34 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 9353 _reflns_number_gt 7336 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'IPDS software (Stoe & Cie, 1999)' _computing_cell_refinement 'IPDS software (Stoe & Cie, 1999)' _computing_data_reduction 'IPDS software (Stoe & Cie, 1999)' _computing_structure_solution ; Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565. ; _computing_publication_material ; Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9353 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1 _refine_ls_restrained_S_all 1 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.322 _refine_diff_density_min -0.65 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.377476(14) 0.871589(8) 0.755022(7) 0.01981(4) Uani 1 1 d . . . P1 P 0.42420(5) 0.92837(3) 0.63562(2) 0.02837(10) Uani 1 1 d . . . P2 P 0.20185(5) 0.77963(3) 0.70108(3) 0.03094(10) Uani 1 1 d . . . P3 P 0.30638(7) 0.84140(3) 0.87627(3) 0.03753(13) Uani 1 1 d . . . P4 P 0.58591(5) 0.93369(3) 0.80938(3) 0.03552(11) Uani 1 1 d . . . N1 N 0.47923(16) 0.78492(10) 0.74919(8) 0.0310(3) Uani 1 1 d . . . O1 O 0.5442(2) 0.72299(11) 0.74649(11) 0.0591(5) Uani 1 1 d . . . O2 O 0.23721(16) 0.96323(9) 0.76688(9) 0.0414(3) Uani 1 1 d . . . C1 C 0.2375(2) 1.04535(12) 0.76310(11) 0.0324(4) Uani 1 1 d . . . H1 H 0.3295 1.0635 0.7586 0.042 Uiso 1 1 calc R . . C2 C 0.1869(2) 1.08093(13) 0.83168(10) 0.0362(4) Uani 1 1 d . . . C3 C 0.0732(2) 1.05113(14) 0.86152(13) 0.0416(5) Uani 1 1 d . . . H3 H 0.0233 1.0107 0.8384 0.054 Uiso 1 1 calc R . . C4 C 0.0342(2) 1.08197(16) 0.92618(13) 0.0446(5) Uani 1 1 d . . . H4 H -0.0408 1.0617 0.9464 0.058 Uiso 1 1 calc R . . C5 C 0.1067(3) 1.14176(16) 0.95928(12) 0.0468(6) Uani 1 1 d . . . H5 H 0.0813 1.1622 1.0023 0.061 Uiso 1 1 calc R . . C6 C 0.2165(3) 1.17180(17) 0.92972(13) 0.0491(6) Uani 1 1 d . . . H6 H 0.2649 1.2128 0.9528 0.064 Uiso 1 1 calc R . . C7 C 0.2567(2) 1.14216(15) 0.86600(12) 0.0423(5) Uani 1 1 d . . . H7 H 0.3313 1.1637 0.8462 0.055 Uiso 1 1 calc R . . C8 C 0.1500(2) 1.07424(13) 0.69727(11) 0.0362(4) Uani 1 1 d . . . C9 C 0.0386(3) 1.03228(15) 0.67024(14) 0.0463(5) Uani 1 1 d . . . H9 H 0.0115 0.9867 0.6936 0.06 Uiso 1 1 calc R . . C10 C -0.0336(3) 1.05819(18) 0.60776(16) 0.0565(7) Uani 1 1 d . . . H10 H -0.1091 1.0303 0.5901 0.073 Uiso 1 1 calc R . . C11 C 0.0078(3) 1.12498(19) 0.57278(15) 0.0589(7) Uani 1 1 d . . . H11 H -0.0374 1.1415 0.5304 0.077 Uiso 1 1 calc R . . C12 C 0.1160(3) 1.16674(18) 0.60111(15) 0.0583(7) Uani 1 1 d . . . H12 H 0.1429 1.2127 0.5782 0.076 Uiso 1 1 calc R . . C13 C 0.1862(3) 1.14196(15) 0.66329(13) 0.0455(5) Uani 1 1 d . . . H13 H 0.2587 1.1718 0.682 0.059 Uiso 1 1 calc R . . C14 C 0.5440(2) 0.86928(16) 0.58845(12) 0.0448(5) Uani 1 1 d . . . H14A H 0.5101 0.816 0.5811 0.058 Uiso 1 1 calc R . . H14B H 0.6278 0.8673 0.6164 0.058 Uiso 1 1 calc R . . H14C H 0.5567 0.8936 0.5431 0.058 Uiso 1 1 calc R . . C15 C 0.2891(2) 0.94220(15) 0.56553(11) 0.0433(5) Uani 1 1 d . . . H15A H 0.3259 0.9612 0.5228 0.056 Uiso 1 1 calc R . . H15B H 0.2261 0.9805 0.5812 0.056 Uiso 1 1 calc R . . H15C H 0.2447 0.8921 0.5559 0.056 Uiso 1 1 calc R . . C16 C 0.4955(3) 1.02970(15) 0.63162(13) 0.0464(5) Uani 1 1 d . . . H16A H 0.5764 1.0324 0.6621 0.06 Uiso 1 1 calc R . . H16B H 0.4323 1.0679 0.6473 0.06 Uiso 1 1 calc R . . H16C H 0.5149 1.0416 0.5834 0.06 Uiso 1 1 calc R . . C17 C 0.0272(3) 0.80720(19) 0.6808(2) 0.0686(9) Uani 1 1 d . . . H17A H 0.0214 0.8463 0.6432 0.089 Uiso 1 1 calc R . . H17B H -0.0084 0.8292 0.7227 0.089 Uiso 1 1 calc R . . H17C H -0.0231 0.7606 0.6657 0.089 Uiso 1 1 calc R . . C18 C 0.2440(3) 0.73538(14) 0.61600(13) 0.0467(5) Uani 1 1 d . . . H18A H 0.1827 0.6928 0.6032 0.061 Uiso 1 1 calc R . . H18B H 0.3335 0.7146 0.6209 0.061 Uiso 1 1 calc R . . H18C H 0.238 0.7756 0.5794 0.061 Uiso 1 1 calc R . . C19 C 0.1859(3) 0.68543(14) 0.74981(15) 0.0522(6) Uani 1 1 d . . . H19A H 0.1444 0.6955 0.7935 0.068 Uiso 1 1 calc R . . H19B H 0.273 0.6628 0.7605 0.068 Uiso 1 1 calc R . . H19C H 0.132 0.6487 0.7209 0.068 Uiso 1 1 calc R . . C20 C 0.1272(3) 0.83214(17) 0.88612(17) 0.0625(8) Uani 1 1 d . . . H20A H 0.0913 0.7899 0.8559 0.081 Uiso 1 1 calc R . . H20B H 0.0836 0.8816 0.8727 0.081 Uiso 1 1 calc R . . H20C H 0.1125 0.8201 0.9349 0.081 Uiso 1 1 calc R . . C21 C 0.3724(4) 0.74924(17) 0.91827(14) 0.0666(9) Uani 1 1 d . . . H21A H 0.4682 0.7492 0.9185 0.087 Uiso 1 1 calc R . . H21B H 0.3371 0.7039 0.8919 0.087 Uiso 1 1 calc R . . H21C H 0.3465 0.7464 0.9665 0.087 Uiso 1 1 calc R . . C22 C 0.3410(3) 0.91511(16) 0.94752(12) 0.0551(7) Uani 1 1 d . . . H22A H 0.2986 0.8987 0.9894 0.072 Uiso 1 1 calc R . . H22B H 0.3068 0.9663 0.932 0.072 Uiso 1 1 calc R . . H22C H 0.4358 0.9189 0.9584 0.072 Uiso 1 1 calc R . . C23 C 0.6668(3) 0.8746(2) 0.88242(18) 0.0673(8) Uani 1 1 d . . . H23A H 0.7513 0.8982 0.8975 0.087 Uiso 1 1 calc R . . H23B H 0.6807 0.821 0.8662 0.087 Uiso 1 1 calc R . . H23C H 0.6107 0.8735 0.9218 0.087 Uiso 1 1 calc R . . C24 C 0.5931(3) 1.03445(16) 0.84685(15) 0.0516(6) Uani 1 1 d . . . H24A H 0.5294 1.0391 0.8825 0.067 Uiso 1 1 calc R . . H24B H 0.5723 1.0727 0.8096 0.067 Uiso 1 1 calc R . . H24C H 0.6813 1.0445 0.8682 0.067 Uiso 1 1 calc R . . C25 C 0.7300(3) 0.9343(3) 0.75461(18) 0.0753(11) Uani 1 1 d . . . H25A H 0.7141 0.9713 0.7159 0.098 Uiso 1 1 calc R . . H25B H 0.743 0.8817 0.7359 0.098 Uiso 1 1 calc R . . H25C H 0.8085 0.9502 0.7834 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02242(7) 0.02065(7) 0.01644(6) 0.00015(5) 0.00199(4) 0.00172(5) P1 0.0311(2) 0.0347(2) 0.01985(19) 0.00255(17) 0.00538(16) -0.00077(18) P2 0.0297(2) 0.0270(2) 0.0366(2) -0.00810(19) 0.00574(19) -0.00454(18) P3 0.0617(4) 0.0302(2) 0.0224(2) 0.00461(18) 0.0153(2) 0.0071(2) P4 0.0287(2) 0.0429(3) 0.0335(2) -0.0054(2) -0.00861(19) 0.0001(2) N1 0.0311(8) 0.0325(8) 0.0293(7) -0.0028(6) 0.0018(6) 0.0095(6) O1 0.0611(12) 0.0498(10) 0.0654(12) -0.0109(9) -0.0033(9) 0.0346(9) O2 0.0475(9) 0.0293(7) 0.0472(9) -0.0002(6) 0.0025(7) 0.0147(6) C1 0.0295(9) 0.0323(9) 0.0355(9) 0.0003(8) 0.0035(7) 0.0032(7) C2 0.0388(10) 0.0422(11) 0.0279(9) 0.0060(8) 0.0053(7) 0.0208(9) C3 0.0393(11) 0.0393(11) 0.0453(12) 0.0021(9) -0.0025(9) 0.0064(9) C4 0.0337(10) 0.0577(14) 0.0436(11) 0.0155(10) 0.0121(9) 0.0107(10) C5 0.0484(13) 0.0648(16) 0.0274(9) -0.0012(9) 0.0047(9) 0.0173(11) C6 0.0488(13) 0.0584(15) 0.0392(11) -0.0036(11) -0.0040(10) 0.0001(11) C7 0.0359(10) 0.0565(14) 0.0350(10) 0.0068(9) 0.0060(8) 0.0058(10) C8 0.0396(10) 0.0379(10) 0.0308(9) -0.0050(8) -0.0002(8) 0.0168(8) C9 0.0475(13) 0.0403(12) 0.0523(13) -0.0065(10) 0.0108(10) 0.0025(10) C10 0.0380(12) 0.0643(17) 0.0650(17) -0.0258(14) -0.0114(11) 0.0042(11) C11 0.0639(17) 0.0656(18) 0.0436(13) -0.0032(12) -0.0224(12) 0.0216(14) C12 0.0726(19) 0.0503(15) 0.0506(14) 0.0102(12) -0.0058(13) 0.0021(13) C13 0.0440(12) 0.0482(13) 0.0426(12) -0.0031(10) -0.0087(9) 0.0016(10) C14 0.0455(12) 0.0572(14) 0.0332(10) -0.0011(10) 0.0138(9) 0.0094(11) C15 0.0479(12) 0.0533(13) 0.0277(9) 0.0055(9) -0.0034(8) 0.0056(10) C16 0.0543(14) 0.0417(12) 0.0448(12) 0.0084(10) 0.0143(10) -0.0109(10) C17 0.0307(12) 0.0600(17) 0.113(3) -0.0348(18) -0.0072(14) -0.0027(11) C18 0.0638(15) 0.0376(11) 0.0389(11) -0.0144(9) 0.0057(10) -0.0086(11) C19 0.0731(17) 0.0309(11) 0.0553(14) -0.0063(10) 0.0233(13) -0.0153(11) C20 0.0770(19) 0.0478(14) 0.0691(17) -0.0042(13) 0.0494(16) -0.0064(13) C21 0.119(3) 0.0452(14) 0.0375(12) 0.0180(11) 0.0197(14) 0.0229(16) C22 0.089(2) 0.0521(15) 0.0251(9) -0.0043(9) 0.0095(11) 0.0102(14) C23 0.0617(17) 0.0694(19) 0.0656(17) 0.0052(15) -0.0319(14) 0.0158(15) C24 0.0482(13) 0.0466(13) 0.0573(15) -0.0088(11) -0.0147(11) -0.0103(11) C25 0.0275(11) 0.132(3) 0.0660(18) -0.023(2) 0.0013(11) -0.0052(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.7803(16) . ? Mo1 O2 2.1025(14) . ? Mo1 P3 2.4840(5) . ? Mo1 P4 2.4872(6) . ? Mo1 P2 2.4979(5) . ? Mo1 P1 2.5083(5) . ? P1 C14 1.831(2) . ? P1 C15 1.835(2) . ? P1 C16 1.843(2) . ? P2 C17 1.824(3) . ? P2 C19 1.834(2) . ? P2 C18 1.836(2) . ? P3 C20 1.825(3) . ? P3 C21 1.834(3) . ? P3 C22 1.834(3) . ? P4 C24 1.826(3) . ? P4 C25 1.831(3) . ? P4 C23 1.832(3) . ? N1 O1 1.227(2) . ? O2 C1 1.375(2) . ? C1 C2 1.536(3) . ? C1 C8 1.542(3) . ? C1 H1 0.98 . ? C2 C7 1.375(3) . ? C2 C3 1.397(3) . ? C3 C4 1.400(3) . ? C3 H3 0.93 . ? C4 C5 1.360(4) . ? C4 H4 0.93 . ? C5 C6 1.362(4) . ? C5 H5 0.93 . ? C6 C7 1.381(3) . ? C6 H6 0.93 . ? C7 H7 0.93 . ? C8 C13 1.362(3) . ? C8 C9 1.385(3) . ? C9 C10 1.403(4) . ? C9 H9 0.93 . ? C10 C11 1.375(4) . ? C10 H10 0.93 . ? C11 C12 1.366(4) . ? C11 H11 0.93 . ? C12 C13 1.383(4) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O2 172.09(7) . . ? N1 Mo1 P3 95.37(5) . . ? O2 Mo1 P3 79.27(5) . . ? N1 Mo1 P4 84.07(6) . . ? O2 Mo1 P4 101.60(5) . . ? P3 Mo1 P4 89.78(2) . . ? N1 Mo1 P2 82.20(6) . . ? O2 Mo1 P2 91.96(5) . . ? P3 Mo1 P2 90.37(2) . . ? P4 Mo1 P2 166.229(19) . . ? N1 Mo1 P1 96.28(5) . . ? O2 Mo1 P1 89.25(5) . . ? P3 Mo1 P1 168.288(18) . . ? P4 Mo1 P1 90.22(2) . . ? P2 Mo1 P1 92.396(19) . . ? C14 P1 C15 101.38(11) . . ? C14 P1 C16 101.96(12) . . ? C15 P1 C16 97.09(12) . . ? C14 P1 Mo1 113.44(8) . . ? C15 P1 Mo1 120.89(8) . . ? C16 P1 Mo1 118.82(8) . . ? C17 P2 C19 101.85(15) . . ? C17 P2 C18 101.34(14) . . ? C19 P2 C18 96.95(11) . . ? C17 P2 Mo1 124.58(9) . . ? C19 P2 Mo1 114.24(10) . . ? C18 P2 Mo1 113.68(9) . . ? C20 P3 C21 102.30(16) . . ? C20 P3 C22 96.91(14) . . ? C21 P3 C22 101.97(13) . . ? C20 P3 Mo1 117.26(11) . . ? C21 P3 Mo1 116.52(9) . . ? C22 P3 Mo1 118.66(9) . . ? C24 P4 C25 101.53(16) . . ? C24 P4 C23 101.93(14) . . ? C25 P4 C23 95.62(17) . . ? C24 P4 Mo1 123.55(9) . . ? C25 P4 Mo1 116.45(10) . . ? C23 P4 Mo1 113.34(11) . . ? O1 N1 Mo1 176.75(18) . . ? C1 O2 Mo1 135.93(14) . . ? O2 C1 C2 109.96(17) . . ? O2 C1 C8 110.54(17) . . ? C2 C1 C8 110.30(15) . . ? O2 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? C8 C1 H1 108.7 . . ? C7 C2 C3 118.74(19) . . ? C7 C2 C1 119.58(19) . . ? C3 C2 C1 121.7(2) . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 120.9(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.2(2) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C13 C8 C9 119.0(2) . . ? C13 C8 C1 118.7(2) . . ? C9 C8 C1 122.2(2) . . ? C8 C9 C10 120.3(2) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 119.2(2) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 121.2(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C8 C13 C12 120.5(2) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P2 C19 H19A 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P3 C20 H20A 109.5 . . ? P3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P3 C22 H22A 109.5 . . ? P3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P4 C23 H23A 109.5 . . ? P4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P4 C24 H24A 109.5 . . ? P4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P4 C25 H25A 109.5 . . ? P4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? data_8 _database_code_depnum_ccdc_archive 'CCDC 281548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitrosyl-penta(trimethylphosphine)molybdenum tetrakis[bis(3,5-trifluoromethyl)phenyl]borane ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H57 B F24 Mo N O P5' _chemical_formula_weight 1369.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 13.1223(18) _cell_length_b 13.2643(12) _cell_length_c 18.473(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.728(15) _cell_angle_gamma 90.00 _cell_volume 3045.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.10 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.8552 _exptl_absorpt_correction_T_max 0.9668 _exptl_special_details ; Some of the F-atoms had to be refined isotropically because of rotational disorder. Thus EADP and PART instructions of SHELXL-97 were applied. Positions of H-atoms were calculated after each refinement cycle (riding model). According to the thin plate crystal the diffracting power was low. As a consequence the displacement parameters are relatively large. ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 5.0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33425 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0923 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.09 _reflns_number_total 14600 _reflns_number_gt 8827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 14600 _refine_ls_number_parameters 697 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.73575(4) 1.00133(4) 0.49262(3) 0.03324(11) Uani 1 d . . . P1 P 0.60475(16) 1.07346(15) 0.55496(11) 0.0509(4) Uani 1 d . . . P2 P 0.7560(3) 1.17241(19) 0.44223(16) 0.0809(8) Uani 1 d . . . P3 P 0.88950(17) 0.9275(2) 0.45640(14) 0.0757(8) Uani 1 d . . . P4 P 0.59377(15) 0.96328(17) 0.35440(11) 0.0512(5) Uani 1 d . . . P5 P 0.7028(3) 0.83038(19) 0.53836(16) 0.0778(7) Uani 1 d . . . N1 N 0.8330(5) 1.0343(5) 0.5813(3) 0.0595(17) Uani 1 d . . . O1 O 0.8976(6) 1.0561(7) 0.6407(4) 0.103(3) Uani 1 d . . . C1 C 0.4580(8) 1.0654(12) 0.5132(6) 0.106(4) Uani 1 d . . . H1A H 0.4251 1.0727 0.5536 0.159 Uiso 1 calc R . . H1B H 0.4383 0.9998 0.4882 0.159 Uiso 1 calc R . . H1C H 0.4322 1.1192 0.4754 0.159 Uiso 1 calc R . . C2 C 0.6158(9) 1.0162(7) 0.6493(5) 0.081(3) Uani 1 d . . . H2A H 0.5599 1.0442 0.6680 0.121 Uiso 1 calc R . . H2B H 0.6869 1.0312 0.6858 0.121 Uiso 1 calc R . . H2C H 0.6066 0.9430 0.6435 0.121 Uiso 1 calc R . . C3 C 0.6340(13) 1.2007(8) 0.5957(7) 0.124(5) Uani 1 d . . . H3A H 0.6405 1.2475 0.5563 0.186 Uiso 1 calc R . . H3B H 0.7018 1.1997 0.6383 0.186 Uiso 1 calc R . . H3C H 0.5756 1.2228 0.6142 0.186 Uiso 1 calc R . . C4 C 0.8187(12) 1.2016(10) 0.3680(7) 0.117(5) Uani 1 d . . . H4A H 0.8026 1.2716 0.3511 0.176 Uiso 1 calc R . . H4B H 0.7897 1.1562 0.3244 0.176 Uiso 1 calc R . . H4C H 0.8968 1.1926 0.3893 0.176 Uiso 1 calc R . . C5 C 0.8370(14) 1.2556(10) 0.5145(7) 0.138(6) Uani 1 d . . . H5A H 0.9116 1.2317 0.5317 0.207 Uiso 1 calc R . . H5B H 0.8094 1.2568 0.5579 0.207 Uiso 1 calc R . . H5C H 0.8341 1.3237 0.4935 0.207 Uiso 1 calc R . . C6 C 0.6281(13) 1.2462(8) 0.4014(8) 0.128(5) Uani 1 d . . . H6A H 0.5762 1.2259 0.4267 0.192 Uiso 1 calc R . . H6B H 0.5980 1.2329 0.3464 0.192 Uiso 1 calc R . . H6C H 0.6435 1.3184 0.4097 0.192 Uiso 1 calc R . . C7 C 0.8775(9) 0.8433(11) 0.3795(6) 0.114(5) Uani 1 d . . . H7A H 0.8491 0.8797 0.3309 0.172 Uiso 1 calc R . . H7B H 0.8283 0.7884 0.3811 0.172 Uiso 1 calc R . . H7C H 0.9484 0.8154 0.3839 0.172 Uiso 1 calc R . . C8 C 0.9851(10) 1.0254(13) 0.4333(11) 0.160(7) Uani 1 d . . . H8A H 1.0581 0.9976 0.4477 0.239 Uiso 1 calc R . . H8B H 0.9856 1.0875 0.4621 0.239 Uiso 1 calc R . . H8C H 0.9598 1.0403 0.3784 0.239 Uiso 1 calc R . . C9 C 0.9874(8) 0.8719(12) 0.5360(6) 0.123(5) Uani 1 d . . . H9A H 0.9594 0.8084 0.5491 0.184 Uiso 1 calc R . . H9B H 1.0038 0.9180 0.5797 0.184 Uiso 1 calc R . . H9C H 1.0530 0.8587 0.5232 0.184 Uiso 1 calc R . . C10 C 0.4555(6) 1.0093(8) 0.3326(5) 0.071(2) Uani 1 d . . . H10A H 0.4151 0.9947 0.2791 0.106 Uiso 1 calc R . . H10B H 0.4565 1.0822 0.3413 0.106 Uiso 1 calc R . . H10C H 0.4211 0.9755 0.3659 0.106 Uiso 1 calc R . . C11 C 0.5659(7) 0.8339(8) 0.3210(6) 0.082(3) Uani 1 d . . . H11A H 0.5304 0.7983 0.3528 0.123 Uiso 1 calc R . . H11B H 0.6336 0.7998 0.3245 0.123 Uiso 1 calc R . . H11C H 0.5188 0.8340 0.2677 0.123 Uiso 1 calc R . . C12 C 0.6289(8) 1.0174(8) 0.2735(5) 0.084(3) Uani 1 d . . . H12A H 0.5928 0.9792 0.2269 0.126 Uiso 1 calc R . . H12B H 0.7070 1.0140 0.2843 0.126 Uiso 1 calc R . . H12C H 0.6056 1.0880 0.2663 0.126 Uiso 1 calc R . . C13 C 0.7410(12) 0.7158(6) 0.4947(8) 0.103(3) Uani 1 d . . . H13A H 0.7383 0.6567 0.5259 0.154 Uiso 1 calc R . . H13B H 0.8142 0.7239 0.4924 0.154 Uiso 1 calc R . . H13C H 0.6907 0.7066 0.4430 0.154 Uiso 1 calc R . . C14 C 0.7832(13) 0.8064(10) 0.6365(7) 0.133(5) Uani 1 d . . . H14A H 0.8248 0.8669 0.6581 0.199 Uiso 1 calc R . . H14B H 0.8324 0.7502 0.6383 0.199 Uiso 1 calc R . . H14C H 0.7359 0.7891 0.6663 0.199 Uiso 1 calc R . . C15 C 0.5674(10) 0.7912(7) 0.5346(7) 0.106(4) Uani 1 d . . . H15A H 0.5722 0.7460 0.5775 0.159 Uiso 1 calc R . . H15B H 0.5327 0.7558 0.4864 0.159 Uiso 1 calc R . . H15C H 0.5249 0.8507 0.5378 0.159 Uiso 1 calc R . . B1 B 0.9941(6) 0.5059(5) 0.2375(5) 0.0303(13) Uani 1 d . . . C16 C 1.0383(4) 0.5193(4) 0.1642(3) 0.0289(11) Uani 1 d . . . C17 C 0.9708(4) 0.5167(4) 0.0891(3) 0.0309(11) Uani 1 d . . . H17 H 0.8952 0.5145 0.0796 0.037 Uiso 1 calc R . . C18 C 1.0094(4) 0.5173(4) 0.0268(3) 0.0334(12) Uani 1 d . . . C181 C 0.9349(5) 0.5104(5) -0.0507(3) 0.0374(13) Uani 1 d . . . F181 F 0.9598(4) 0.5680(5) -0.1026(3) 0.0958(19) Uani 1 d . . . F182 F 0.8297(4) 0.5320(6) -0.0594(3) 0.099(2) Uani 1 d . . . F183 F 0.9274(7) 0.4193(5) -0.0807(3) 0.125(3) Uani 1 d . . . C19 C 1.1188(5) 0.5197(4) 0.0394(4) 0.0381(13) Uani 1 d . . . H19 H 1.1460 0.5206 -0.0024 0.046 Uiso 1 calc R . . C20 C 1.1877(4) 0.5207(4) 0.1127(4) 0.0359(13) Uani 1 d . . . C201 C 1.3098(6) 0.5207(6) 0.1316(5) 0.056(2) Uani 1 d . . . F201 F 1.3543(3) 0.4462(4) 0.1769(4) 0.0887(18) Uani 1 d . . . F202 F 1.3387(4) 0.5129(4) 0.0686(4) 0.0887(16) Uani 1 d . . . F203 F 1.3533(3) 0.6071(4) 0.1654(3) 0.0659(12) Uani 1 d . . . C21 C 1.1492(4) 0.5205(4) 0.1745(4) 0.0368(13) Uani 1 d . . . H21 H 1.1989 0.5212 0.2249 0.044 Uiso 1 calc R . . C22 C 0.9983(5) 0.3840(4) 0.2511(3) 0.0302(11) Uani 1 d . . . C23 C 0.9172(4) 0.3205(4) 0.2092(3) 0.0297(11) Uani 1 d . . . H23 H 0.8525 0.3490 0.1761 0.036 Uiso 1 calc R . . C24 C 0.9277(5) 0.2149(4) 0.2141(3) 0.0317(12) Uani 1 d . . . C241 C 0.8397(6) 0.1504(5) 0.1658(4) 0.0476(16) Uani 1 d . . . F241 F 0.7424(3) 0.1842(4) 0.1623(3) 0.0788(15) Uani 1 d . . . F242 F 0.8369(5) 0.1444(5) 0.0939(3) 0.0933(18) Uani 1 d . . . F243 F 0.8428(5) 0.0571(3) 0.1915(3) 0.0859(16) Uani 1 d . . . C25 C 1.0213(5) 0.1712(5) 0.2607(3) 0.0379(14) Uani 1 d . . . H25 H 1.0289 0.0999 0.2634 0.045 Uiso 1 calc R . . C26 C 1.1039(5) 0.2330(5) 0.3034(3) 0.0394(13) Uani 1 d . . . C261 C 1.2054(6) 0.1854(6) 0.3549(4) 0.0523(18) Uani 1 d . . . F261 F 1.1920(9) 0.1130(9) 0.4021(6) 0.0800(12) Uiso 0.465(3) d P A 1 F262 F 1.2857(10) 0.2039(10) 0.3181(7) 0.0800(12) Uiso 0.465(3) d P A 1 F263 F 1.2642(10) 0.2494(9) 0.4152(7) 0.0800(12) Uiso 0.465(3) d P A 1 F264 F 1.2195(8) 0.0949(8) 0.3378(5) 0.0800(12) Uiso 0.535(3) d P A 2 F265 F 1.2941(9) 0.2360(8) 0.3453(6) 0.0800(12) Uiso 0.535(3) d P A 2 F266 F 1.2241(9) 0.2091(8) 0.4219(6) 0.0800(12) Uiso 0.535(3) d P A 2 C27 C 1.0936(5) 0.3368(5) 0.2985(3) 0.0331(13) Uiso 1 d . . . H27 H 1.1518 0.3776 0.3276 0.040 Uiso 1 calc R . . C28 C 0.8736(4) 0.5536(4) 0.2209(3) 0.0289(11) Uani 1 d . . . C29 C 0.8026(4) 0.5160(4) 0.2572(3) 0.0291(11) Uani 1 d . . . H29 H 0.8217 0.4561 0.2867 0.035 Uiso 1 calc R . . C30 C 0.7054(4) 0.5625(4) 0.2518(3) 0.0347(12) Uani 1 d . . . C301 C 0.6366(5) 0.5182(6) 0.2929(4) 0.0476(17) Uani 1 d . . . F301 F 0.5940(4) 0.4291(4) 0.2656(3) 0.0721(13) Uani 1 d . . . F302 F 0.6922(4) 0.4995(4) 0.3663(3) 0.0735(16) Uani 1 d . . . F303 F 0.5541(4) 0.5763(4) 0.2927(3) 0.0732(13) Uani 1 d . . . C31 C 0.6734(4) 0.6471(4) 0.2075(3) 0.0360(12) Uani 1 d . . . H31 H 0.6058 0.6775 0.2020 0.043 Uiso 1 calc R . . C32 C 0.7416(5) 0.6877(4) 0.1709(3) 0.0368(12) Uani 1 d . . . F321 F 0.7004(11) 0.7659(10) 0.0532(7) 0.0834(12) Uiso 0.465(3) d P A 1 F322 F 0.6835(11) 0.8551(9) 0.1620(7) 0.0834(12) Uiso 0.465(3) d P A 1 F323 F 0.7995(11) 0.8441(10) 0.1362(8) 0.0834(12) Uiso 0.465(3) d P A 1 F324 F 0.6294(9) 0.7600(8) 0.0542(6) 0.0834(12) Uiso 0.535(3) d P A 2 F325 F 0.6262(9) 0.8263(8) 0.1313(6) 0.0834(12) Uiso 0.535(3) d P A 2 F326 F 0.7771(9) 0.8166(8) 0.0905(7) 0.0834(12) Uiso 0.535(3) d P A 2 C321 C 0.7086(7) 0.7811(6) 0.1230(5) 0.062(2) Uani 1 d . . . C33 C 0.8422(5) 0.6409(4) 0.1790(3) 0.0337(13) Uani 1 d . . . H33 H 0.8889 0.6705 0.1549 0.040 Uiso 1 calc R . . C34 C 1.0637(4) 0.5686(4) 0.3125(3) 0.0291(11) Uani 1 d . . . C35 C 1.1179(5) 0.6593(5) 0.3089(4) 0.0362(14) Uani 1 d . . . H35 H 1.1199 0.6822 0.2607 0.043 Uiso 1 calc R . . C36 C 1.1684(5) 0.7163(4) 0.3737(3) 0.0381(13) Uani 1 d . . . C361 C 1.2196(7) 0.8118(6) 0.3655(4) 0.055(2) Uani 1 d . . . F361 F 1.2830(8) 0.8010(7) 0.3231(6) 0.166(4) Uani 1 d . . . F362 F 1.1536(8) 0.8746(5) 0.3200(5) 0.150(4) Uani 1 d . . . F363 F 1.2731(8) 0.8557(6) 0.4262(3) 0.181(5) Uani 1 d . . . C37 C 1.1644(5) 0.6862(5) 0.4446(3) 0.0394(13) Uani 1 d . . . H37 H 1.1977 0.7255 0.4889 0.047 Uiso 1 calc R . . C38 C 1.1111(4) 0.5982(4) 0.4496(3) 0.0358(12) Uani 1 d . . . C381 C 1.1038(5) 0.5651(5) 0.5236(4) 0.0450(15) Uiso 1 d . . . F381 F 1.0131(9) 0.5528(10) 0.5248(7) 0.0776(12) Uiso 0.465(3) d P A 1 F382 F 1.1545(9) 0.6280(9) 0.5826(6) 0.0776(12) Uiso 0.465(3) d P A 1 F383 F 1.1337(11) 0.4703(9) 0.5367(7) 0.0776(12) Uiso 0.465(3) d P A 1 F384 F 1.0312(8) 0.6200(8) 0.5459(6) 0.0776(12) Uiso 0.535(3) d P A 2 F385 F 1.1953(8) 0.5684(8) 0.5808(5) 0.0776(12) Uiso 0.535(3) d P A 2 F386 F 1.0551(10) 0.4758(8) 0.5249(6) 0.0776(12) Uiso 0.535(3) d P A 2 C39 C 1.0629(4) 0.5404(4) 0.3852(3) 0.0310(11) Uiso 1 d . . . H39 H 1.0281 0.4794 0.3906 0.037 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03165(18) 0.03457(19) 0.03233(18) 0.0010(2) 0.00865(13) 0.0046(2) P1 0.0549(11) 0.0530(11) 0.0521(10) 0.0000(9) 0.0276(9) 0.0073(9) P2 0.139(2) 0.0502(13) 0.0779(16) -0.0079(12) 0.0689(17) -0.0230(15) P3 0.0406(10) 0.112(2) 0.0714(14) -0.0176(14) 0.0140(10) 0.0277(11) P4 0.0386(9) 0.0708(12) 0.0446(10) -0.0062(9) 0.0137(8) 0.0081(8) P5 0.118(2) 0.0441(13) 0.0814(17) 0.0175(12) 0.0457(16) 0.0030(13) N1 0.046(3) 0.095(5) 0.029(3) -0.012(3) 0.000(2) 0.004(3) O1 0.070(4) 0.162(8) 0.070(4) -0.033(5) 0.011(3) -0.010(5) C1 0.059(5) 0.193(14) 0.070(6) 0.000(7) 0.026(5) 0.037(7) C2 0.127(8) 0.082(6) 0.052(4) -0.007(4) 0.054(5) -0.024(6) C3 0.242(16) 0.060(6) 0.139(10) -0.006(6) 0.159(12) 0.009(8) C4 0.181(13) 0.095(9) 0.108(9) -0.018(7) 0.093(9) -0.059(8) C5 0.230(16) 0.114(10) 0.102(8) -0.054(7) 0.097(10) -0.118(11) C6 0.222(15) 0.060(6) 0.134(10) 0.044(7) 0.102(11) 0.056(8) C7 0.077(6) 0.162(12) 0.101(8) -0.044(8) 0.026(6) 0.046(7) C8 0.078(8) 0.210(17) 0.228(19) 0.039(14) 0.102(11) 0.019(9) C9 0.056(5) 0.209(14) 0.082(7) -0.007(8) -0.009(5) 0.072(7) C10 0.046(4) 0.110(7) 0.055(4) -0.007(5) 0.014(3) 0.015(4) C11 0.067(5) 0.097(7) 0.080(6) -0.042(5) 0.020(5) -0.006(5) C12 0.077(6) 0.125(9) 0.048(4) -0.002(5) 0.018(4) 0.001(6) C13 0.160(10) 0.036(4) 0.123(8) 0.000(6) 0.060(8) -0.011(7) C14 0.208(16) 0.102(9) 0.106(9) 0.053(8) 0.076(10) 0.050(10) C15 0.146(10) 0.062(6) 0.153(10) -0.023(6) 0.109(9) -0.046(6) B1 0.023(3) 0.034(3) 0.033(3) -0.005(3) 0.008(2) -0.004(3) C16 0.024(2) 0.024(3) 0.038(3) 0.004(2) 0.010(2) 0.0015(18) C17 0.029(2) 0.033(3) 0.033(2) 0.001(2) 0.012(2) 0.005(2) C18 0.037(3) 0.027(3) 0.038(3) -0.003(2) 0.015(2) -0.002(2) C181 0.037(3) 0.045(4) 0.039(3) -0.004(3) 0.025(2) -0.010(3) F181 0.081(3) 0.145(5) 0.051(3) 0.029(3) 0.006(2) -0.039(3) F182 0.076(3) 0.181(6) 0.036(2) 0.022(3) 0.013(2) 0.049(4) F183 0.170(7) 0.089(4) 0.067(3) -0.013(3) -0.032(4) 0.007(4) C19 0.040(3) 0.031(3) 0.054(3) -0.004(2) 0.030(3) -0.004(2) C20 0.026(2) 0.027(3) 0.058(3) -0.001(2) 0.017(2) -0.0004(19) C201 0.033(3) 0.061(5) 0.081(6) 0.012(4) 0.029(4) 0.008(3) F201 0.029(2) 0.081(4) 0.147(5) 0.035(4) 0.014(3) 0.023(2) F202 0.058(3) 0.107(4) 0.126(4) -0.023(3) 0.065(3) -0.009(3) F203 0.036(2) 0.069(3) 0.091(3) -0.009(2) 0.018(2) -0.018(2) C21 0.028(3) 0.035(3) 0.046(3) -0.004(2) 0.011(2) 0.001(2) C22 0.030(3) 0.032(2) 0.030(3) -0.002(2) 0.012(2) 0.004(2) C23 0.025(2) 0.037(3) 0.026(3) 0.003(2) 0.006(2) 0.003(2) C24 0.035(3) 0.034(3) 0.027(3) -0.003(2) 0.012(2) -0.006(2) C241 0.056(4) 0.049(4) 0.033(3) -0.003(3) 0.008(3) -0.020(3) F241 0.041(2) 0.084(3) 0.101(4) -0.037(3) 0.009(2) 0.000(2) F242 0.120(4) 0.115(4) 0.055(3) -0.037(3) 0.041(3) -0.053(4) F243 0.096(4) 0.036(2) 0.099(4) 0.009(2) -0.005(3) -0.021(2) C25 0.044(3) 0.028(3) 0.048(4) -0.005(3) 0.023(3) 0.000(2) C26 0.034(3) 0.038(3) 0.042(3) 0.003(3) 0.008(3) 0.012(3) C261 0.055(4) 0.042(4) 0.056(4) 0.011(3) 0.013(4) 0.016(3) C28 0.033(3) 0.028(3) 0.023(2) -0.002(2) 0.006(2) -0.001(2) C29 0.029(2) 0.032(3) 0.025(2) 0.006(2) 0.0055(19) -0.001(2) C30 0.034(3) 0.036(3) 0.033(3) 0.000(2) 0.009(2) 0.002(2) C301 0.036(3) 0.071(5) 0.040(3) 0.000(3) 0.018(3) 0.004(3) F301 0.067(3) 0.064(3) 0.093(3) -0.001(3) 0.035(3) -0.029(2) F302 0.055(3) 0.124(5) 0.047(2) 0.022(3) 0.025(2) 0.000(3) F303 0.053(2) 0.083(3) 0.104(4) 0.025(3) 0.053(3) 0.019(2) C31 0.033(3) 0.039(3) 0.035(3) -0.008(2) 0.010(2) 0.008(2) C32 0.044(3) 0.038(3) 0.030(3) 0.000(2) 0.015(2) 0.012(2) C321 0.084(6) 0.050(4) 0.076(5) 0.022(4) 0.059(5) 0.033(4) C33 0.046(3) 0.025(3) 0.035(3) -0.003(2) 0.019(3) -0.003(3) C34 0.019(2) 0.031(3) 0.034(3) 0.002(2) 0.003(2) 0.000(2) C35 0.040(3) 0.029(3) 0.036(3) 0.002(3) 0.009(3) -0.007(3) C36 0.037(3) 0.033(3) 0.039(3) 0.000(2) 0.005(2) -0.003(2) C361 0.057(4) 0.063(5) 0.042(4) -0.001(4) 0.012(3) -0.032(4) F361 0.197(8) 0.124(6) 0.246(10) -0.063(6) 0.168(8) -0.096(6) F362 0.199(8) 0.067(4) 0.141(6) 0.037(4) -0.005(6) -0.064(5) F363 0.282(11) 0.159(7) 0.066(4) 0.000(4) 0.006(5) -0.180(8) C37 0.036(3) 0.043(3) 0.036(3) -0.004(3) 0.006(2) 0.001(2) C38 0.029(3) 0.039(3) 0.038(3) 0.002(2) 0.008(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.778(6) . yes Mo1 P2 2.499(3) . yes Mo1 P5 2.506(3) . yes Mo1 P3 2.519(2) . yes Mo1 P1 2.543(2) . yes Mo1 P4 2.682(2) . yes P1 C1 1.833(10) . yes P1 C3 1.838(11) . yes P1 C2 1.863(8) . yes P2 C5 1.794(10) . yes P2 C4 1.852(10) . yes P2 C6 1.880(13) . yes P3 C9 1.773(9) . yes P3 C7 1.774(11) . yes P3 C8 1.946(14) . yes P4 C11 1.820(10) . yes P4 C10 1.832(7) . yes P4 C12 1.845(9) . yes P5 C14 1.809(13) . yes P5 C15 1.830(10) . yes P5 C13 1.863(10) . yes N1 O1 1.187(8) . yes C1 H1A 0.9800 . yes C1 H1B 0.9800 . yes C1 H1C 0.9800 . yes C2 H2A 0.9800 . yes C2 H2B 0.9800 . yes C2 H2C 0.9800 . yes C3 H3A 0.9800 . yes C3 H3B 0.9800 . yes C3 H3C 0.9800 . yes C4 H4A 0.9800 . yes C4 H4B 0.9800 . yes C4 H4C 0.9800 . yes C5 H5A 0.9800 . yes C5 H5B 0.9800 . yes C5 H5C 0.9800 . yes C6 H6A 0.9800 . yes C6 H6B 0.9800 . yes C6 H6C 0.9800 . yes C7 H7A 0.9800 . yes C7 H7B 0.9800 . yes C7 H7C 0.9800 . yes C8 H8A 0.9800 . yes C8 H8B 0.9800 . yes C8 H8C 0.9800 . yes C9 H9A 0.9800 . yes C9 H9B 0.9800 . yes C9 H9C 0.9800 . yes C10 H10A 0.9800 . yes C10 H10B 0.9800 . yes C10 H10C 0.9800 . yes C11 H11A 0.9800 . yes C11 H11B 0.9800 . yes C11 H11C 0.9800 . yes C12 H12A 0.9800 . yes C12 H12B 0.9800 . yes C12 H12C 0.9800 . yes C13 H13A 0.9800 . yes C13 H13B 0.9800 . yes C13 H13C 0.9800 . yes C14 H14A 0.9800 . yes C14 H14B 0.9800 . yes C14 H14C 0.9800 . yes C15 H15A 0.9800 . yes C15 H15B 0.9800 . yes C15 H15C 0.9800 . yes B1 C34 1.622(10) . yes B1 C22 1.634(9) . yes B1 C28 1.638(9) . yes B1 C16 1.646(9) . yes C16 C17 1.386(7) . yes C16 C21 1.405(7) . yes C17 C18 1.400(8) . yes C17 H17 0.9500 . yes C18 C19 1.379(8) . yes C18 C181 1.454(8) . yes C181 F183 1.319(8) . yes C181 F181 1.345(7) . yes C181 F182 1.368(8) . yes C19 C20 1.366(9) . yes C19 H19 0.9500 . yes C20 C21 1.389(9) . yes C20 C201 1.527(9) . yes C201 F201 1.306(9) . yes C201 F202 1.338(10) . yes C201 F203 1.342(10) . yes C21 H21 0.9500 . yes C22 C23 1.383(8) . yes C22 C27 1.422(8) . yes C23 C24 1.408(8) . yes C23 H23 0.9500 . yes C24 C25 1.380(8) . yes C24 C241 1.484(8) . yes C241 F242 1.320(8) . yes C241 F243 1.322(8) . yes C241 F241 1.334(9) . yes C25 C26 1.386(8) . yes C25 H25 0.9500 . yes C26 C27 1.383(8) . yes C26 C261 1.505(9) . yes C261 F266 1.222(12) . yes C261 F264 1.269(12) . yes C261 F261 1.345(14) . yes C261 F265 1.402(13) . yes C261 F263 1.416(14) . yes C261 F262 1.447(15) . yes C27 H27 0.9500 . yes C28 C33 1.380(8) . yes C28 C29 1.402(7) . yes C29 C30 1.392(8) . yes C29 H29 0.9500 . yes C30 C31 1.372(8) . yes C30 C301 1.474(9) . yes C301 F303 1.328(8) . yes C301 F301 1.335(8) . yes C301 F302 1.341(8) . yes C31 C32 1.392(8) . yes C31 H31 0.9500 . yes C32 C33 1.422(9) . yes C32 C321 1.503(9) . yes F321 C321 1.274(14) . yes F322 C321 1.319(14) . yes F322 F323 1.739(18) . yes F323 C321 1.412(15) . yes F324 C321 1.388(14) . yes F324 F325 1.685(16) . yes F325 C321 1.287(13) . yes F326 C321 1.317(13) . yes C33 H33 0.9500 . yes C34 C39 1.396(8) . yes C34 C35 1.410(8) . yes C35 C36 1.390(8) . yes C35 H35 0.9500 . yes C36 C37 1.387(8) . yes C36 C361 1.464(9) . yes C361 F363 1.258(9) . yes C361 F362 1.298(11) . yes C361 F361 1.321(10) . yes C37 C38 1.380(8) . yes C37 H37 0.9500 . yes C38 C39 1.386(8) . yes C38 C381 1.468(9) . yes C381 F381 1.208(13) . yes C381 F383 1.317(14) . yes C381 F385 1.320(11) . yes C381 F386 1.350(13) . yes C381 F382 1.363(13) . yes C381 F384 1.363(12) . yes C39 H39 0.9500 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 P2 89.4(2) . . yes N1 Mo1 P5 93.6(2) . . yes P2 Mo1 P5 176.31(13) . . yes N1 Mo1 P3 86.6(2) . . yes P2 Mo1 P3 93.66(11) . . yes P5 Mo1 P3 88.72(10) . . yes N1 Mo1 P1 83.1(2) . . yes P2 Mo1 P1 89.73(8) . . yes P5 Mo1 P1 88.43(9) . . yes P3 Mo1 P1 169.14(7) . . yes N1 Mo1 P4 175.8(2) . . yes P2 Mo1 P4 86.60(9) . . yes P5 Mo1 P4 90.48(9) . . yes P3 Mo1 P4 92.57(7) . . yes P1 Mo1 P4 97.93(7) . . yes C1 P1 C3 106.2(7) . . yes C1 P1 C2 97.2(5) . . yes C3 P1 C2 92.8(4) . . yes C1 P1 Mo1 124.0(4) . . yes C3 P1 Mo1 116.6(4) . . yes C2 P1 Mo1 114.1(3) . . yes C5 P2 C4 97.2(5) . . yes C5 P2 C6 102.5(8) . . yes C4 P2 C6 98.3(6) . . yes C5 P2 Mo1 112.9(5) . . yes C4 P2 Mo1 126.3(4) . . yes C6 P2 Mo1 115.8(4) . . yes C9 P3 C7 104.9(6) . . yes C9 P3 C8 96.5(7) . . yes C7 P3 C8 98.2(8) . . yes C9 P3 Mo1 111.7(4) . . yes C7 P3 Mo1 125.8(4) . . yes C8 P3 Mo1 115.3(5) . . yes C11 P4 C10 99.4(4) . . yes C11 P4 C12 99.6(5) . . yes C10 P4 C12 100.4(4) . . yes C11 P4 Mo1 120.2(3) . . yes C10 P4 Mo1 118.9(3) . . yes C12 P4 Mo1 114.8(3) . . yes C14 P5 C15 103.6(6) . . yes C14 P5 C13 98.0(6) . . yes C15 P5 C13 98.3(6) . . yes C14 P5 Mo1 112.9(5) . . yes C15 P5 Mo1 121.0(4) . . yes C13 P5 Mo1 119.5(4) . . yes O1 N1 Mo1 179.7(7) . . yes P1 C1 H1A 109.5 . . yes P1 C1 H1B 109.5 . . yes H1A C1 H1B 109.5 . . yes P1 C1 H1C 109.5 . . yes H1A C1 H1C 109.5 . . yes H1B C1 H1C 109.5 . . yes P1 C2 H2A 109.5 . . yes P1 C2 H2B 109.5 . . yes H2A C2 H2B 109.5 . . yes P1 C2 H2C 109.5 . . yes H2A C2 H2C 109.5 . . yes H2B C2 H2C 109.5 . . yes P1 C3 H3A 109.5 . . yes P1 C3 H3B 109.5 . . yes H3A C3 H3B 109.5 . . yes P1 C3 H3C 109.5 . . yes H3A C3 H3C 109.5 . . yes H3B C3 H3C 109.5 . . yes P2 C4 H4A 109.5 . . yes P2 C4 H4B 109.5 . . yes H4A C4 H4B 109.5 . . yes P2 C4 H4C 109.5 . . yes H4A C4 H4C 109.5 . . yes H4B C4 H4C 109.5 . . yes P2 C5 H5A 109.5 . . yes P2 C5 H5B 109.5 . . yes H5A C5 H5B 109.5 . . yes P2 C5 H5C 109.5 . . yes H5A C5 H5C 109.5 . . yes H5B C5 H5C 109.5 . . yes P2 C6 H6A 109.5 . . yes P2 C6 H6B 109.5 . . yes H6A C6 H6B 109.5 . . yes P2 C6 H6C 109.5 . . yes H6A C6 H6C 109.5 . . yes H6B C6 H6C 109.5 . . yes P3 C7 H7A 109.5 . . yes P3 C7 H7B 109.5 . . yes H7A C7 H7B 109.5 . . yes P3 C7 H7C 109.5 . . yes H7A C7 H7C 109.5 . . yes H7B C7 H7C 109.5 . . yes P3 C8 H8A 109.5 . . yes P3 C8 H8B 109.5 . . yes H8A C8 H8B 109.5 . . yes P3 C8 H8C 109.5 . . yes H8A C8 H8C 109.5 . . yes H8B C8 H8C 109.5 . . yes P3 C9 H9A 109.5 . . yes P3 C9 H9B 109.5 . . yes H9A C9 H9B 109.5 . . yes P3 C9 H9C 109.5 . . yes H9A C9 H9C 109.5 . . yes H9B C9 H9C 109.5 . . yes P4 C10 H10A 109.5 . . yes P4 C10 H10B 109.5 . . yes H10A C10 H10B 109.5 . . yes P4 C10 H10C 109.5 . . yes H10A C10 H10C 109.5 . . yes H10B C10 H10C 109.5 . . yes P4 C11 H11A 109.5 . . yes P4 C11 H11B 109.5 . . yes H11A C11 H11B 109.5 . . yes P4 C11 H11C 109.5 . . yes H11A C11 H11C 109.5 . . yes H11B C11 H11C 109.5 . . yes P4 C12 H12A 109.5 . . yes P4 C12 H12B 109.5 . . yes H12A C12 H12B 109.5 . . yes P4 C12 H12C 109.5 . . yes H12A C12 H12C 109.5 . . yes H12B C12 H12C 109.5 . . yes P5 C13 H13A 109.5 . . yes P5 C13 H13B 109.5 . . yes H13A C13 H13B 109.5 . . yes P5 C13 H13C 109.5 . . yes H13A C13 H13C 109.5 . . yes H13B C13 H13C 109.5 . . yes P5 C14 H14A 109.5 . . yes P5 C14 H14B 109.5 . . yes H14A C14 H14B 109.5 . . yes P5 C14 H14C 109.5 . . yes H14A C14 H14C 109.5 . . yes H14B C14 H14C 109.5 . . yes P5 C15 H15A 109.5 . . yes P5 C15 H15B 109.5 . . yes H15A C15 H15B 109.5 . . yes P5 C15 H15C 109.5 . . yes H15A C15 H15C 109.5 . . yes H15B C15 H15C 109.5 . . yes C34 B1 C22 113.2(6) . . yes C34 B1 C28 101.9(5) . . yes C22 B1 C28 113.2(5) . . yes C34 B1 C16 113.4(5) . . yes C22 B1 C16 103.3(5) . . yes C28 B1 C16 112.2(6) . . yes C17 C16 C21 116.0(5) . . yes C17 C16 B1 122.7(5) . . yes C21 C16 B1 120.8(5) . . yes C16 C17 C18 122.6(5) . . yes C16 C17 H17 118.7 . . yes C18 C17 H17 118.7 . . yes C19 C18 C17 119.5(5) . . yes C19 C18 C181 120.2(5) . . yes C17 C18 C181 120.2(5) . . yes F183 C181 F181 102.9(6) . . yes F183 C181 F182 102.0(6) . . yes F181 C181 F182 105.3(6) . . yes F183 C181 C18 114.1(6) . . yes F181 C181 C18 115.1(5) . . yes F182 C181 C18 115.8(5) . . yes C20 C19 C18 119.4(5) . . yes C20 C19 H19 120.3 . . yes C18 C19 H19 120.3 . . yes C19 C20 C21 121.0(5) . . yes C19 C20 C201 122.6(6) . . yes C21 C20 C201 116.4(6) . . yes F201 C201 F202 107.8(7) . . yes F201 C201 F203 108.2(7) . . yes F202 C201 F203 105.9(6) . . yes F201 C201 C20 111.5(6) . . yes F202 C201 C20 111.8(7) . . yes F203 C201 C20 111.3(6) . . yes C20 C21 C16 121.5(5) . . yes C20 C21 H21 119.2 . . yes C16 C21 H21 119.2 . . yes C23 C22 C27 116.3(5) . . yes C23 C22 B1 122.3(6) . . yes C27 C22 B1 120.7(6) . . yes C22 C23 C24 121.9(5) . . yes C22 C23 H23 119.1 . . yes C24 C23 H23 119.1 . . yes C25 C24 C23 120.5(5) . . yes C25 C24 C241 119.9(5) . . yes C23 C24 C241 119.6(5) . . yes F242 C241 F243 107.0(6) . . yes F242 C241 F241 104.7(6) . . yes F243 C241 F241 104.6(6) . . yes F242 C241 C24 113.9(6) . . yes F243 C241 C24 113.3(6) . . yes F241 C241 C24 112.6(6) . . yes C24 C25 C26 118.9(5) . . yes C24 C25 H25 120.6 . . yes C26 C25 H25 120.6 . . yes C27 C26 C25 120.6(5) . . yes C27 C26 C261 120.5(6) . . yes C25 C26 C261 118.9(6) . . yes F266 C261 F264 119.8(9) . . yes F266 C261 F261 63.5(8) . . yes F264 C261 F261 63.0(7) . . yes F266 C261 F265 95.7(8) . . yes F264 C261 F265 103.2(8) . . yes F261 C261 F265 135.2(9) . . yes F266 C261 F263 33.7(6) . . yes F264 C261 F263 132.6(9) . . yes F261 C261 F263 94.1(8) . . yes F265 C261 F263 63.1(7) . . yes F266 C261 F262 119.5(9) . . yes F264 C261 F262 81.8(8) . . yes F261 C261 F262 133.8(9) . . yes F265 C261 F262 26.0(6) . . yes F263 C261 F262 88.5(8) . . yes F266 C261 C26 112.4(8) . . yes F264 C261 C26 114.1(8) . . yes F261 C261 C26 115.8(8) . . yes F265 C261 C26 108.7(7) . . yes F263 C261 C26 113.2(7) . . yes F262 C261 C26 105.2(7) . . yes C26 C27 C22 121.8(6) . . yes C26 C27 H27 119.1 . . yes C22 C27 H27 119.1 . . yes C33 C28 C29 116.2(5) . . yes C33 C28 B1 121.7(5) . . yes C29 C28 B1 121.5(5) . . yes C30 C29 C28 122.8(5) . . yes C30 C29 H29 118.6 . . yes C28 C29 H29 118.6 . . yes C31 C30 C29 120.2(5) . . yes C31 C30 C301 120.8(5) . . yes C29 C30 C301 119.0(5) . . yes F303 C301 F301 105.6(5) . . yes F303 C301 F302 106.7(6) . . yes F301 C301 F302 104.1(6) . . yes F303 C301 C30 113.6(6) . . yes F301 C301 C30 114.2(5) . . yes F302 C301 C30 111.8(5) . . yes C30 C31 C32 119.0(5) . . yes C30 C31 H31 120.5 . . yes C32 C31 H31 120.5 . . yes C31 C32 C33 120.0(5) . . yes C31 C32 C321 119.7(5) . . yes C33 C32 C321 120.3(6) . . yes C321 F322 F323 52.8(7) . . yes C321 F323 F322 48.1(7) . . yes C321 F324 F325 48.4(6) . . yes C321 F325 F324 53.6(7) . . yes F321 C321 F325 113.1(10) . . yes F321 C321 F326 56.3(8) . . yes F325 C321 F326 127.5(9) . . yes F321 C321 F322 135.6(10) . . yes F325 C321 F322 39.0(6) . . yes F326 C321 F322 108.0(10) . . yes F321 C321 F324 41.1(7) . . yes F325 C321 F324 78.0(9) . . yes F326 C321 F324 94.3(8) . . yes F322 C321 F324 113.9(9) . . yes F321 C321 F323 93.5(9) . . yes F325 C321 F323 113.5(10) . . yes F326 C321 F323 37.4(6) . . yes F322 C321 F323 79.0(10) . . yes F324 C321 F323 128.4(9) . . yes F321 C321 C32 112.3(8) . . yes F325 C321 C32 114.1(7) . . yes F326 C321 C32 116.9(7) . . yes F322 C321 C32 111.5(8) . . yes F324 C321 C32 111.3(8) . . yes F323 C321 C32 108.5(8) . . yes C28 C33 C32 121.7(6) . . yes C28 C33 H33 119.2 . . yes C32 C33 H33 119.2 . . yes C39 C34 C35 115.7(5) . . yes C39 C34 B1 120.5(5) . . yes C35 C34 B1 123.5(5) . . yes C36 C35 C34 122.2(6) . . yes C36 C35 H35 118.9 . . yes C34 C35 H35 118.9 . . yes C37 C36 C35 120.3(5) . . yes C37 C36 C361 120.3(6) . . yes C35 C36 C361 119.3(6) . . yes F363 C361 F362 110.2(9) . . yes F363 C361 F361 107.5(8) . . yes F362 C361 F361 95.8(8) . . yes F363 C361 C36 116.8(6) . . yes F362 C361 C36 112.9(6) . . yes F361 C361 C36 111.4(7) . . yes C38 C37 C36 118.7(5) . . yes C38 C37 H37 120.6 . . yes C36 C37 H37 120.6 . . yes C37 C38 C39 120.8(5) . . yes C37 C38 C381 120.1(5) . . yes C39 C38 C381 119.1(5) . . yes F381 C381 F383 96.0(9) . . yes F381 C381 F385 129.7(9) . . yes F383 C381 F385 75.1(8) . . yes F381 C381 F386 53.6(7) . . yes F383 C381 F386 43.4(6) . . yes F385 C381 F386 109.2(8) . . yes F381 C381 F382 107.5(9) . . yes F383 C381 F382 113.4(9) . . yes F385 C381 F382 42.0(6) . . yes F386 C381 F382 129.5(8) . . yes F381 C381 F384 43.9(7) . . yes F383 C381 F384 130.7(9) . . yes F385 C381 F384 106.6(8) . . yes F386 C381 F384 94.8(8) . . yes F382 C381 F384 69.0(7) . . yes F381 C381 C38 114.6(8) . . yes F383 C381 C38 110.5(7) . . yes F385 C381 C38 114.8(7) . . yes F386 C381 C38 116.8(7) . . yes F382 C381 C38 113.5(7) . . yes F384 C381 C38 112.5(6) . . yes C38 C39 C34 122.3(5) . . yes C38 C39 H39 118.8 . . yes C34 C39 H39 118.8 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mo1 P1 C1 -172.1(6) . . . . yes P2 Mo1 P1 C1 98.5(6) . . . . yes P5 Mo1 P1 C1 -78.3(6) . . . . yes P3 Mo1 P1 C1 -153.2(7) . . . . yes P4 Mo1 P1 C1 11.9(6) . . . . yes N1 Mo1 P1 C3 52.2(6) . . . . yes P2 Mo1 P1 C3 -37.1(5) . . . . yes P5 Mo1 P1 C3 146.1(5) . . . . yes P3 Mo1 P1 C3 71.2(8) . . . . yes P4 Mo1 P1 C3 -123.7(5) . . . . yes N1 Mo1 P1 C2 -54.2(4) . . . . yes P2 Mo1 P1 C2 -143.6(3) . . . . yes P5 Mo1 P1 C2 39.6(4) . . . . yes P3 Mo1 P1 C2 -35.3(7) . . . . yes P4 Mo1 P1 C2 129.8(3) . . . . yes N1 Mo1 P2 C5 -8.3(6) . . . . yes P5 Mo1 P2 C5 134.9(17) . . . . yes P3 Mo1 P2 C5 -94.9(6) . . . . yes P1 Mo1 P2 C5 74.8(6) . . . . yes P4 Mo1 P2 C5 172.7(6) . . . . yes N1 Mo1 P2 C4 110.3(6) . . . . yes P5 Mo1 P2 C4 -106.4(17) . . . . yes P3 Mo1 P2 C4 23.7(6) . . . . yes P1 Mo1 P2 C4 -166.6(6) . . . . yes P4 Mo1 P2 C4 -68.7(6) . . . . yes N1 Mo1 P2 C6 -126.1(5) . . . . yes P5 Mo1 P2 C6 17.2(18) . . . . yes P3 Mo1 P2 C6 147.3(5) . . . . yes P1 Mo1 P2 C6 -43.0(5) . . . . yes P4 Mo1 P2 C6 54.9(5) . . . . yes N1 Mo1 P3 C9 35.5(6) . . . . yes P2 Mo1 P3 C9 124.7(6) . . . . yes P5 Mo1 P3 C9 -58.1(6) . . . . yes P1 Mo1 P3 C9 16.7(8) . . . . yes P4 Mo1 P3 C9 -148.6(6) . . . . yes N1 Mo1 P3 C7 164.5(7) . . . . yes P2 Mo1 P3 C7 -106.4(7) . . . . yes P5 Mo1 P3 C7 70.8(6) . . . . yes P1 Mo1 P3 C7 145.6(7) . . . . yes P4 Mo1 P3 C7 -19.6(6) . . . . yes N1 Mo1 P3 C8 -73.3(7) . . . . yes P2 Mo1 P3 C8 15.9(7) . . . . yes P5 Mo1 P3 C8 -167.0(6) . . . . yes P1 Mo1 P3 C8 -92.1(8) . . . . yes P4 Mo1 P3 C8 102.6(6) . . . . yes N1 Mo1 P4 C11 142(3) . . . . yes P2 Mo1 P4 C11 156.8(4) . . . . yes P5 Mo1 P4 C11 -25.5(4) . . . . yes P3 Mo1 P4 C11 63.3(4) . . . . yes P1 Mo1 P4 C11 -113.9(4) . . . . yes N1 Mo1 P4 C10 -95(3) . . . . yes P2 Mo1 P4 C10 -80.8(4) . . . . yes P5 Mo1 P4 C10 96.9(4) . . . . yes P3 Mo1 P4 C10 -174.4(4) . . . . yes P1 Mo1 P4 C10 8.4(4) . . . . yes N1 Mo1 P4 C12 23(3) . . . . yes P2 Mo1 P4 C12 37.9(4) . . . . yes P5 Mo1 P4 C12 -144.3(4) . . . . yes P3 Mo1 P4 C12 -55.6(4) . . . . yes P1 Mo1 P4 C12 127.2(4) . . . . yes N1 Mo1 P5 C14 0.2(5) . . . . yes P2 Mo1 P5 C14 -143.0(17) . . . . yes P3 Mo1 P5 C14 86.7(5) . . . . yes P1 Mo1 P5 C14 -82.8(5) . . . . yes P4 Mo1 P5 C14 179.3(5) . . . . yes N1 Mo1 P5 C15 123.6(5) . . . . yes P2 Mo1 P5 C15 -19.6(18) . . . . yes P3 Mo1 P5 C15 -149.9(5) . . . . yes P1 Mo1 P5 C15 40.6(5) . . . . yes P4 Mo1 P5 C15 -57.3(5) . . . . yes N1 Mo1 P5 C13 -114.1(6) . . . . yes P2 Mo1 P5 C13 102.7(18) . . . . yes P3 Mo1 P5 C13 -27.6(6) . . . . yes P1 Mo1 P5 C13 162.9(6) . . . . yes P4 Mo1 P5 C13 65.0(6) . . . . yes P2 Mo1 N1 O1 137(100) . . . . yes P5 Mo1 N1 O1 -41(100) . . . . yes P3 Mo1 N1 O1 -130(100) . . . . yes P1 Mo1 N1 O1 47(100) . . . . yes P4 Mo1 N1 O1 151(100) . . . . yes C34 B1 C16 C17 -148.1(5) . . . . yes C22 B1 C16 C17 88.9(6) . . . . yes C28 B1 C16 C17 -33.3(7) . . . . yes C34 B1 C16 C21 40.4(7) . . . . yes C22 B1 C16 C21 -82.5(6) . . . . yes C28 B1 C16 C21 155.3(5) . . . . yes C21 C16 C17 C18 -1.2(7) . . . . yes B1 C16 C17 C18 -173.0(5) . . . . yes C16 C17 C18 C19 0.5(8) . . . . yes C16 C17 C18 C181 177.5(5) . . . . yes C19 C18 C181 F183 76.8(8) . . . . yes C17 C18 C181 F183 -100.1(7) . . . . yes C19 C18 C181 F181 -41.8(8) . . . . yes C17 C18 C181 F181 141.3(6) . . . . yes C19 C18 C181 F182 -165.3(6) . . . . yes C17 C18 C181 F182 17.8(8) . . . . yes C17 C18 C19 C20 0.4(8) . . . . yes C181 C18 C19 C20 -176.5(5) . . . . yes C18 C19 C20 C21 -0.7(8) . . . . yes C18 C19 C20 C201 178.4(5) . . . . yes C19 C20 C201 F201 -124.9(7) . . . . yes C21 C20 C201 F201 54.2(9) . . . . yes C19 C20 C201 F202 -4.1(9) . . . . yes C21 C20 C201 F202 175.1(6) . . . . yes C19 C20 C201 F203 114.2(7) . . . . yes C21 C20 C201 F203 -66.7(8) . . . . yes C19 C20 C21 C16 0.0(8) . . . . yes C201 C20 C21 C16 -179.2(5) . . . . yes C17 C16 C21 C20 0.9(7) . . . . yes B1 C16 C21 C20 172.9(5) . . . . yes C34 B1 C22 C23 154.4(5) . . . . yes C28 B1 C22 C23 39.0(9) . . . . yes C16 B1 C22 C23 -82.5(7) . . . . yes C34 B1 C22 C27 -35.5(8) . . . . yes C28 B1 C22 C27 -150.9(6) . . . . yes C16 B1 C22 C27 87.6(7) . . . . yes C27 C22 C23 C24 1.0(9) . . . . yes B1 C22 C23 C24 171.5(6) . . . . yes C22 C23 C24 C25 -1.0(8) . . . . yes C22 C23 C24 C241 -177.9(6) . . . . yes C25 C24 C241 F242 -99.6(7) . . . . yes C23 C24 C241 F242 77.3(8) . . . . yes C25 C24 C241 F243 23.0(9) . . . . yes C23 C24 C241 F243 -160.1(6) . . . . yes C25 C24 C241 F241 141.4(6) . . . . yes C23 C24 C241 F241 -41.7(8) . . . . yes C23 C24 C25 C26 1.0(8) . . . . yes C241 C24 C25 C26 177.9(6) . . . . yes C24 C25 C26 C27 -1.1(9) . . . . yes C24 C25 C26 C261 179.3(6) . . . . yes C27 C26 C261 F266 59.9(11) . . . . yes C25 C26 C261 F266 -120.4(9) . . . . yes C27 C26 C261 F264 -159.3(8) . . . . yes C25 C26 C261 F264 20.3(11) . . . . yes C27 C26 C261 F261 130.3(8) . . . . yes C25 C26 C261 F261 -50.1(10) . . . . yes C27 C26 C261 F265 -44.8(10) . . . . yes C25 C26 C261 F265 134.9(8) . . . . yes C27 C26 C261 F263 23.3(11) . . . . yes C25 C26 C261 F263 -157.1(8) . . . . yes C27 C26 C261 F262 -71.7(9) . . . . yes C25 C26 C261 F262 108.0(8) . . . . yes C25 C26 C27 C22 1.1(9) . . . . yes C261 C26 C27 C22 -179.2(6) . . . . yes C23 C22 C27 C26 -1.1(9) . . . . yes B1 C22 C27 C26 -171.8(6) . . . . yes C34 B1 C28 C33 84.8(6) . . . . yes C22 B1 C28 C33 -153.2(6) . . . . yes C16 B1 C28 C33 -36.9(7) . . . . yes C34 B1 C28 C29 -86.2(6) . . . . yes C22 B1 C28 C29 35.8(8) . . . . yes C16 B1 C28 C29 152.1(5) . . . . yes C33 C28 C29 C30 0.2(8) . . . . yes B1 C28 C29 C30 171.7(5) . . . . yes C28 C29 C30 C31 2.2(8) . . . . yes C28 C29 C30 C301 -179.1(5) . . . . yes C31 C30 C301 F303 -10.5(9) . . . . yes C29 C30 C301 F303 170.8(5) . . . . yes C31 C30 C301 F301 110.8(7) . . . . yes C29 C30 C301 F301 -67.9(7) . . . . yes C31 C30 C301 F302 -131.3(6) . . . . yes C29 C30 C301 F302 50.0(8) . . . . yes C29 C30 C31 C32 -2.6(8) . . . . yes C301 C30 C31 C32 178.7(5) . . . . yes C30 C31 C32 C33 0.7(8) . . . . yes C30 C31 C32 C321 -179.2(6) . . . . yes F324 F325 C321 F321 21.9(9) . . . . yes F324 F325 C321 F326 86.2(12) . . . . yes F324 F325 C321 F322 156.9(13) . . . . yes F324 F325 C321 F323 126.8(10) . . . . yes F324 F325 C321 C32 -108.2(10) . . . . yes F323 F322 C321 F321 -83.7(15) . . . . yes F323 F322 C321 F325 -152.1(13) . . . . yes F323 F322 C321 F326 -24.0(8) . . . . yes F323 F322 C321 F324 -127.3(10) . . . . yes F323 F322 C321 C32 105.7(10) . . . . yes F325 F324 C321 F321 -148.6(13) . . . . yes F325 F324 C321 F326 -127.5(9) . . . . yes F325 F324 C321 F322 -15.7(9) . . . . yes F325 F324 C321 F323 -110.6(12) . . . . yes F325 F324 C321 C32 111.4(8) . . . . yes F322 F323 C321 F321 135.9(10) . . . . yes F322 F323 C321 F325 18.8(9) . . . . yes F322 F323 C321 F326 140.4(13) . . . . yes F322 F323 C321 F324 111.9(12) . . . . yes F322 F323 C321 C32 -109.2(9) . . . . yes C31 C32 C321 F321 -118.5(9) . . . . yes C33 C32 C321 F321 61.6(12) . . . . yes C31 C32 C321 F325 11.9(12) . . . . yes C33 C32 C321 F325 -168.0(8) . . . . yes C31 C32 C321 F326 179.2(8) . . . . yes C33 C32 C321 F326 -0.7(12) . . . . yes C31 C32 C321 F322 54.3(12) . . . . yes C33 C32 C321 F322 -125.6(9) . . . . yes C31 C32 C321 F324 -74.1(9) . . . . yes C33 C32 C321 F324 106.0(8) . . . . yes C31 C32 C321 F323 139.5(8) . . . . yes C33 C32 C321 F323 -40.4(10) . . . . yes C29 C28 C33 C32 -2.2(8) . . . . yes B1 C28 C33 C32 -173.7(6) . . . . yes C31 C32 C33 C28 1.8(9) . . . . yes C321 C32 C33 C28 -178.2(6) . . . . yes C22 B1 C34 C39 -40.4(8) . . . . yes C28 B1 C34 C39 81.5(6) . . . . yes C16 B1 C34 C39 -157.7(5) . . . . yes C22 B1 C34 C35 146.8(6) . . . . yes C28 B1 C34 C35 -91.3(6) . . . . yes C16 B1 C34 C35 29.5(8) . . . . yes C39 C34 C35 C36 0.7(9) . . . . yes B1 C34 C35 C36 173.8(6) . . . . yes C34 C35 C36 C37 -1.7(9) . . . . yes C34 C35 C36 C361 -177.6(6) . . . . yes C37 C36 C361 F363 10.7(13) . . . . yes C35 C36 C361 F363 -173.3(9) . . . . yes C37 C36 C361 F362 -118.6(8) . . . . yes C35 C36 C361 F362 57.3(11) . . . . yes C37 C36 C361 F361 134.9(8) . . . . yes C35 C36 C361 F361 -49.2(11) . . . . yes C35 C36 C37 C38 1.1(9) . . . . yes C361 C36 C37 C38 177.0(6) . . . . yes C36 C37 C38 C39 0.3(8) . . . . yes C36 C37 C38 C381 -178.9(6) . . . . yes C37 C38 C381 F381 123.2(9) . . . . yes C39 C38 C381 F381 -56.1(11) . . . . yes C37 C38 C381 F383 -129.7(8) . . . . yes C39 C38 C381 F383 51.1(9) . . . . yes C37 C38 C381 F385 -47.0(9) . . . . yes C39 C38 C381 F385 133.7(8) . . . . yes C37 C38 C381 F386 -176.9(8) . . . . yes C39 C38 C381 F386 3.9(10) . . . . yes C37 C38 C381 F382 -0.9(10) . . . . yes C39 C38 C381 F382 179.9(7) . . . . yes C37 C38 C381 F384 75.1(8) . . . . yes C39 C38 C381 F384 -104.2(8) . . . . yes C37 C38 C39 C34 -1.3(8) . . . . yes C381 C38 C39 C34 178.0(5) . . . . yes C35 C34 C39 C38 0.8(8) . . . . yes B1 C34 C39 C38 -172.6(5) . . . . yes _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.110 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.096 data_12 _database_code_depnum_ccdc_archive 'CCDC 281549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitrosyl-tris(trimethylphosphine)-N-benzylidene-1-naphthylamine- molybdenum ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H41 Mo N2 O P3' _chemical_formula_weight 586.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.1601(7) _cell_length_b 13.9020(9) _cell_length_c 10.9422(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.548(8) _cell_angle_gamma 90.00 _cell_volume 1473.62(18) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 30.4 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.8121 _exptl_absorpt_correction_T_max 0.9635 _exptl_special_details ; see text ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 5.20 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23862 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.1547 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30.41 _reflns_number_total 8795 _reflns_number_gt 4993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 8795 _refine_ls_number_parameters 306 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 0.671 _refine_ls_restrained_S_all 0.671 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.69735(3) 0.94275(3) 0.82887(3) 0.02430(7) Uani 1 d . . . P1 P 0.76832(11) 1.11592(7) 0.84339(10) 0.0318(2) Uani 1 d . . . P2 P 0.73243(10) 0.92331(7) 0.62173(9) 0.0360(3) Uani 1 d . . . P3 P 0.63673(11) 0.76964(7) 0.84503(10) 0.0336(2) Uani 1 d . . . N1 N 0.8689(3) 0.9047(2) 0.9109(3) 0.0326(7) Uani 1 d . . . O1 O 0.9819(3) 0.8718(2) 0.9729(3) 0.0554(8) Uani 1 d . . . C1 C 0.9444(5) 1.1368(3) 0.8396(5) 0.0597(13) Uani 1 d . . . H1A H 0.9701 1.2039 0.8622 0.090 Uiso 1 calc R . . H1B H 0.9499 1.1236 0.7533 0.090 Uiso 1 calc R . . H1C H 1.0078 1.0940 0.9013 0.090 Uiso 1 calc R . . C2 C 0.6660(5) 1.2055(3) 0.7315(5) 0.0597(13) Uani 1 d . . . H2A H 0.6748 1.1943 0.6459 0.090 Uiso 1 calc R . . H2B H 0.6996 1.2701 0.7607 0.090 Uiso 1 calc R . . H2C H 0.5688 1.1999 0.7282 0.090 Uiso 1 calc R . . C3 C 0.7780(5) 1.1763(3) 0.9942(4) 0.0543(13) Uani 1 d . . . H3A H 0.8358 1.1385 1.0660 0.081 Uiso 1 calc R . . H3B H 0.6850 1.1824 1.0026 0.081 Uiso 1 calc R . . H3C H 0.8183 1.2404 0.9950 0.081 Uiso 1 calc R . . C4 C 0.9109(4) 0.8972(3) 0.6303(4) 0.0513(12) Uani 1 d . . . H4A H 0.9184 0.8916 0.5433 0.077 Uiso 1 calc R . . H4B H 0.9395 0.8366 0.6763 0.077 Uiso 1 calc R . . H4C H 0.9707 0.9494 0.6757 0.077 Uiso 1 calc R . . C5 C 0.6371(5) 0.8309(3) 0.5094(4) 0.0472(12) Uani 1 d . . . H5A H 0.6589 0.8364 0.4284 0.071 Uiso 1 calc R . . H5B H 0.5377 0.8401 0.4937 0.071 Uiso 1 calc R . . H5C H 0.6638 0.7670 0.5464 0.071 Uiso 1 calc R . . C6 C 0.6938(6) 1.0244(4) 0.5104(4) 0.0590(15) Uani 1 d . . . H6A H 0.7110 1.0057 0.4302 0.088 Uiso 1 calc R . . H6B H 0.7529 1.0790 0.5484 0.088 Uiso 1 calc R . . H6C H 0.5967 1.0427 0.4927 0.088 Uiso 1 calc R . . C7 C 0.7602(5) 0.6840(3) 0.8157(5) 0.0533(12) Uani 1 d . . . H7A H 0.7436 0.6202 0.8460 0.080 Uiso 1 calc R . . H7B H 0.8543 0.7048 0.8618 0.080 Uiso 1 calc R . . H7C H 0.7490 0.6813 0.7236 0.080 Uiso 1 calc R . . C8 C 0.4705(4) 0.7190(3) 0.7536(5) 0.0491(12) Uani 1 d . . . H8A H 0.4684 0.6503 0.7731 0.074 Uiso 1 calc R . . H8B H 0.4574 0.7274 0.6618 0.074 Uiso 1 calc R . . H8C H 0.3963 0.7522 0.7769 0.074 Uiso 1 calc R . . C9 C 0.6442(5) 0.7324(3) 1.0057(4) 0.0544(12) Uani 1 d . . . H9A H 0.5710 0.7648 1.0314 0.082 Uiso 1 calc R . . H9B H 0.7342 0.7497 1.0654 0.082 Uiso 1 calc R . . H9C H 0.6314 0.6626 1.0073 0.082 Uiso 1 calc R . . N2 N 0.4791(3) 0.9845(2) 0.7705(3) 0.0335(8) Uani 1 d . . . C10 C 0.4480(3) 0.9717(2) 0.8843(3) 0.0303(9) Uani 1 d . . . C11 C 0.3170(3) 0.9501(4) 0.9002(3) 0.0370(8) Uani 1 d . . . H11 H 0.2380 0.9443 0.8272 0.044 Uiso 1 calc R . . C12 C 0.3049(3) 0.9376(4) 1.0224(4) 0.0429(8) Uani 1 d . . . H12 H 0.2160 0.9262 1.0313 0.051 Uiso 1 calc R . . C13 C 0.4174(4) 0.9410(4) 1.1313(3) 0.0425(8) Uani 1 d . . . H13 H 0.4064 0.9305 1.2135 0.051 Uiso 1 calc R . . C14 C 0.5454(4) 0.9598(3) 1.1187(3) 0.0338(10) Uani 1 d . . . H14 H 0.6240 0.9614 1.1925 0.041 Uiso 1 calc R . . C15 C 0.5603(4) 0.9763(2) 0.9986(3) 0.0297(9) Uani 1 d . . . H15 H 0.6493 0.9914 0.9926 0.036 Uiso 1 calc R . . C161 C 0.3645(19) 0.9545(18) 0.663(2) 0.0303(12) Uiso 0.36(6) d P A 1 H16A H 0.3140 0.9023 0.6907 0.036 Uiso 0.36(6) calc PR A 1 H16B H 0.4013 0.9279 0.5955 0.036 Uiso 0.36(6) calc PR A 1 C162 C 0.3766(10) 0.9699(12) 0.6463(11) 0.0303(12) Uiso 0.64(6) d P A 2 H16C H 0.3371 0.9048 0.6468 0.036 Uiso 0.64(6) calc PR A 2 H16D H 0.4260 0.9693 0.5810 0.036 Uiso 0.64(6) calc PR A 2 C17 C 0.2593(4) 1.0382(3) 0.6018(3) 0.0306(8) Uani 1 d . . . C18 C 0.2514(4) 1.1206(3) 0.6689(3) 0.0347(9) Uani 1 d . . . H18 H 0.3214 1.1333 0.7472 0.042 Uiso 1 calc R . . C19 C 0.1421(4) 1.1866(3) 0.6244(4) 0.0390(10) Uani 1 d . . . H19 H 0.1386 1.2429 0.6725 0.047 Uiso 1 calc R . . C20 C 0.0418(4) 1.1692(3) 0.5124(4) 0.0394(10) Uani 1 d . . . H20 H -0.0321 1.2137 0.4837 0.047 Uiso 1 calc R . . C21 C -0.0579(4) 1.0689(3) 0.3197(4) 0.0474(11) Uani 1 d . . . H21 H -0.1330 1.1123 0.2901 0.057 Uiso 1 calc R . . C22 C -0.0514(4) 0.9907(3) 0.2474(4) 0.0546(12) Uani 1 d . . . H22 H -0.1210 0.9801 0.1682 0.065 Uiso 1 calc R . . C23 C 0.0584(4) 0.9256(4) 0.2901(4) 0.0516(14) Uani 1 d . . . H23 H 0.0638 0.8712 0.2394 0.062 Uiso 1 calc R . . C24 C 0.1572(3) 0.9404(5) 0.4040(3) 0.0420(8) Uani 1 d . . . H24 H 0.2299 0.8949 0.4321 0.050 Uiso 1 calc R . . C25 C 0.1557(4) 1.0208(3) 0.4820(3) 0.0309(8) Uani 1 d . . . C26 C 0.0440(4) 1.0877(3) 0.4380(4) 0.0323(9) Uani 1 d . . . 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 0.02190(12) 0.02531(13) 0.02470(13) 0.0009(2) 0.00553(10) 0.00044(18) P1 0.0368(6) 0.0266(6) 0.0315(6) 0.0018(4) 0.0097(4) -0.0002(4) P2 0.0381(5) 0.0408(8) 0.0313(5) -0.0052(4) 0.0139(4) -0.0028(5) P3 0.0337(6) 0.0266(6) 0.0386(6) 0.0012(4) 0.0082(5) -0.0035(4) N1 0.0367(18) 0.0302(17) 0.0312(17) -0.0005(13) 0.0106(14) -0.0056(13) O1 0.0250(16) 0.058(2) 0.072(2) -0.0005(17) -0.0028(14) 0.0132(13) C1 0.051(3) 0.049(3) 0.083(4) -0.002(3) 0.027(3) -0.016(2) C2 0.075(4) 0.046(3) 0.056(3) 0.003(2) 0.016(3) 0.005(3) C3 0.082(4) 0.035(3) 0.050(3) -0.004(2) 0.026(3) -0.013(2) C4 0.043(2) 0.069(3) 0.050(3) -0.020(2) 0.027(2) -0.010(2) C5 0.046(3) 0.059(3) 0.039(3) -0.013(2) 0.016(2) -0.001(2) C6 0.079(4) 0.065(3) 0.036(3) -0.010(2) 0.022(3) -0.011(3) C7 0.052(3) 0.036(3) 0.072(3) 0.007(2) 0.018(3) -0.001(2) C8 0.046(3) 0.036(3) 0.060(3) 0.007(2) 0.009(2) -0.008(2) C9 0.074(3) 0.034(3) 0.056(3) 0.009(2) 0.021(3) -0.004(2) N2 0.0275(17) 0.0395(18) 0.0292(17) -0.0072(13) 0.0018(14) 0.0037(13) C10 0.0255(18) 0.027(2) 0.037(2) -0.0047(15) 0.0079(15) -0.0017(14) C11 0.0244(15) 0.029(2) 0.056(2) 0.001(3) 0.0092(14) -0.002(2) C12 0.0379(18) 0.031(2) 0.067(2) 0.004(3) 0.0278(18) -0.004(3) C13 0.055(2) 0.0342(19) 0.047(2) 0.008(3) 0.0282(18) -0.005(3) C14 0.0370(19) 0.031(3) 0.0327(18) -0.0015(17) 0.0089(15) -0.0030(17) C15 0.0240(18) 0.034(2) 0.033(2) -0.0027(15) 0.0117(16) -0.0015(14) C17 0.024(2) 0.035(2) 0.034(2) 0.0010(17) 0.0093(17) -0.0015(15) C18 0.035(2) 0.038(2) 0.030(2) 0.0011(17) 0.0085(17) -0.0069(17) C19 0.043(3) 0.035(2) 0.043(3) 0.0056(19) 0.020(2) 0.0011(19) C20 0.033(2) 0.048(3) 0.041(2) 0.018(2) 0.017(2) 0.0103(18) C21 0.034(2) 0.063(3) 0.040(2) 0.012(2) 0.0042(19) 0.013(2) C22 0.040(3) 0.075(3) 0.037(2) 0.000(2) -0.007(2) -0.003(2) C23 0.050(2) 0.065(4) 0.034(2) -0.008(2) 0.0022(18) -0.001(2) C24 0.0358(18) 0.049(2) 0.0361(18) -0.001(3) 0.0036(15) 0.002(3) C25 0.025(2) 0.039(2) 0.028(2) 0.0045(17) 0.0081(17) -0.0014(15) C26 0.028(2) 0.040(2) 0.030(2) 0.0089(17) 0.0093(17) -0.0004(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.783(3) . yes Mo1 N2 2.193(3) . yes Mo1 P2 2.4134(10) . yes Mo1 P3 2.5036(11) . yes Mo1 P1 2.5044(11) . yes P1 C1 1.825(4) . yes P1 C3 1.828(4) . yes P1 C2 1.834(5) . yes P2 C6 1.823(5) . yes P2 C4 1.824(4) . yes P2 C5 1.839(4) . yes P3 C9 1.813(4) . yes P3 C8 1.825(4) . yes P3 C7 1.827(4) . yes N1 O1 1.232(4) . yes C1 H1A 0.9800 . yes C1 H1B 0.9800 . yes C1 H1C 0.9800 . yes C2 H2A 0.9800 . yes C2 H2B 0.9800 . yes C2 H2C 0.9800 . yes C3 H3A 0.9800 . yes C3 H3B 0.9800 . yes C3 H3C 0.9800 . yes C4 H4A 0.9800 . yes C4 H4B 0.9800 . yes C4 H4C 0.9800 . yes C5 H5A 0.9800 . yes C5 H5B 0.9800 . yes C5 H5C 0.9800 . yes C6 H6A 0.9800 . yes C6 H6B 0.9800 . yes C6 H6C 0.9800 . yes C7 H7A 0.9800 . yes C7 H7B 0.9800 . yes C7 H7C 0.9800 . yes C8 H8A 0.9800 . yes C8 H8B 0.9800 . yes C8 H8C 0.9800 . yes C9 H9A 0.9800 . yes C9 H9B 0.9800 . yes C9 H9C 0.9800 . yes N2 C10 1.386(5) . yes N2 C161 1.448(14) . yes N2 C162 1.456(9) . yes C10 C15 1.417(5) . yes C10 C11 1.425(4) . yes C11 C12 1.390(5) . yes C11 H11 0.9500 . yes C12 C13 1.381(5) . yes C12 H12 0.9500 . yes C13 C14 1.374(5) . yes C13 H13 0.9500 . yes C14 C15 1.386(5) . yes C14 H14 0.9500 . yes C15 H15 0.9500 . yes C161 C17 1.585(19) . yes C161 H16A 0.9900 . yes C161 H16B 0.9900 . yes C162 C17 1.487(11) . yes C162 H16C 0.9900 . yes C162 H16D 0.9900 . yes C17 C18 1.376(5) . yes C17 C25 1.433(5) . yes C18 C19 1.409(5) . yes C18 H18 0.9500 . yes C19 C20 1.359(6) . yes C19 H19 0.9500 . yes C20 C26 1.399(6) . yes C20 H20 0.9500 . yes C21 C22 1.358(6) . yes C21 C26 1.417(5) . yes C21 H21 0.9500 . yes C22 C23 1.403(6) . yes C22 H22 0.9500 . yes C23 C24 1.360(5) . yes C23 H23 0.9500 . yes C24 C25 1.409(6) . yes C24 H24 0.9500 . yes C25 C26 1.434(5) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 N2 166.98(12) . . yes N1 Mo1 P2 92.33(10) . . yes N2 Mo1 P2 100.31(8) . . yes N1 Mo1 P3 84.45(10) . . yes N2 Mo1 P3 91.51(8) . . yes P2 Mo1 P3 93.89(4) . . yes N1 Mo1 P1 91.95(10) . . yes N2 Mo1 P1 90.60(8) . . yes P2 Mo1 P1 92.64(4) . . yes P3 Mo1 P1 172.67(4) . . yes C1 P1 C3 99.3(2) . . yes C1 P1 C2 103.9(2) . . yes C3 P1 C2 99.0(2) . . yes C1 P1 Mo1 114.62(16) . . yes C3 P1 Mo1 115.78(15) . . yes C2 P1 Mo1 121.06(17) . . yes C6 P2 C4 101.4(2) . . yes C6 P2 C5 97.35(19) . . yes C4 P2 C5 102.2(2) . . yes C6 P2 Mo1 118.58(16) . . yes C4 P2 Mo1 113.60(14) . . yes C5 P2 Mo1 120.57(16) . . yes C9 P3 C8 100.5(2) . . yes C9 P3 C7 98.9(2) . . yes C8 P3 C7 102.9(2) . . yes C9 P3 Mo1 113.83(15) . . yes C8 P3 Mo1 122.59(15) . . yes C7 P3 Mo1 114.65(15) . . yes O1 N1 Mo1 173.9(3) . . yes P1 C1 H1A 109.5 . . yes P1 C1 H1B 109.5 . . yes H1A C1 H1B 109.5 . . yes P1 C1 H1C 109.5 . . yes H1A C1 H1C 109.5 . . yes H1B C1 H1C 109.5 . . yes P1 C2 H2A 109.5 . . yes P1 C2 H2B 109.5 . . yes H2A C2 H2B 109.5 . . yes P1 C2 H2C 109.5 . . yes H2A C2 H2C 109.5 . . yes H2B C2 H2C 109.5 . . yes P1 C3 H3A 109.5 . . yes P1 C3 H3B 109.5 . . yes H3A C3 H3B 109.5 . . yes P1 C3 H3C 109.5 . . yes H3A C3 H3C 109.5 . . yes H3B C3 H3C 109.5 . . yes P2 C4 H4A 109.5 . . yes P2 C4 H4B 109.5 . . yes H4A C4 H4B 109.5 . . yes P2 C4 H4C 109.5 . . yes H4A C4 H4C 109.5 . . yes H4B C4 H4C 109.5 . . yes P2 C5 H5A 109.5 . . yes P2 C5 H5B 109.5 . . yes H5A C5 H5B 109.5 . . yes P2 C5 H5C 109.5 . . yes H5A C5 H5C 109.5 . . yes H5B C5 H5C 109.5 . . yes P2 C6 H6A 109.5 . . yes P2 C6 H6B 109.5 . . yes H6A C6 H6B 109.5 . . yes P2 C6 H6C 109.5 . . yes H6A C6 H6C 109.5 . . yes H6B C6 H6C 109.5 . . yes P3 C7 H7A 109.5 . . yes P3 C7 H7B 109.5 . . yes H7A C7 H7B 109.5 . . yes P3 C7 H7C 109.5 . . yes H7A C7 H7C 109.5 . . yes H7B C7 H7C 109.5 . . yes P3 C8 H8A 109.5 . . yes P3 C8 H8B 109.5 . . yes H8A C8 H8B 109.5 . . yes P3 C8 H8C 109.5 . . yes H8A C8 H8C 109.5 . . yes H8B C8 H8C 109.5 . . yes P3 C9 H9A 109.5 . . yes P3 C9 H9B 109.5 . . yes H9A C9 H9B 109.5 . . yes P3 C9 H9C 109.5 . . yes H9A C9 H9C 109.5 . . yes H9B C9 H9C 109.5 . . yes C10 N2 C161 110.6(14) . . yes C10 N2 C162 121.9(7) . . yes C161 N2 C162 12.8(9) . . yes C10 N2 Mo1 100.9(2) . . yes C161 N2 Mo1 130.9(7) . . yes C162 N2 Mo1 127.6(4) . . yes N2 C10 C15 116.5(3) . . yes N2 C10 C11 127.6(3) . . yes C15 C10 C11 115.8(3) . . yes C12 C11 C10 120.0(3) . . yes C12 C11 H11 120.0 . . yes C10 C11 H11 120.0 . . yes C13 C12 C11 122.3(3) . . yes C13 C12 H12 118.8 . . yes C11 C12 H12 118.8 . . yes C14 C13 C12 118.8(3) . . yes C14 C13 H13 120.6 . . yes C12 C13 H13 120.6 . . yes C13 C14 C15 120.3(3) . . yes C13 C14 H14 119.9 . . yes C15 C14 H14 119.9 . . yes C14 C15 C10 122.7(3) . . yes C14 C15 H15 118.7 . . yes C10 C15 H15 118.7 . . yes N2 C161 C17 113.9(13) . . yes N2 C161 H16A 108.8 . . yes C17 C161 H16A 108.8 . . yes N2 C161 H16B 108.8 . . yes C17 C161 H16B 108.8 . . yes H16A C161 H16B 107.7 . . yes N2 C162 C17 119.6(6) . . yes N2 C162 H16C 107.4 . . yes C17 C162 H16C 107.4 . . yes N2 C162 H16D 107.4 . . yes C17 C162 H16D 107.4 . . yes H16C C162 H16D 107.0 . . yes C18 C17 C25 119.0(3) . . yes C18 C17 C162 121.8(4) . . yes C25 C17 C162 119.1(4) . . yes C18 C17 C161 121.9(6) . . yes C25 C17 C161 118.4(6) . . yes C162 C17 C161 11.6(8) . . yes C17 C18 C19 121.6(4) . . yes C17 C18 H18 119.2 . . yes C19 C18 H18 119.2 . . yes C20 C19 C18 119.7(4) . . yes C20 C19 H19 120.2 . . yes C18 C19 H19 120.2 . . yes C19 C20 C26 121.9(4) . . yes C19 C20 H20 119.0 . . yes C26 C20 H20 119.0 . . yes C22 C21 C26 122.0(4) . . yes C22 C21 H21 119.0 . . yes C26 C21 H21 119.0 . . yes C21 C22 C23 119.7(4) . . yes C21 C22 H22 120.2 . . yes C23 C22 H22 120.2 . . yes C24 C23 C22 120.1(5) . . yes C24 C23 H23 120.0 . . yes C22 C23 H23 120.0 . . yes C23 C24 C25 122.4(5) . . yes C23 C24 H24 118.8 . . yes C25 C24 H24 118.8 . . yes C24 C25 C17 123.3(3) . . yes C24 C25 C26 117.6(3) . . yes C17 C25 C26 119.1(3) . . yes C20 C26 C21 123.0(4) . . yes C20 C26 C25 118.7(3) . . yes C21 C26 C25 118.2(4) . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mo1 P1 C1 31.8(2) . . . . yes N2 Mo1 P1 C1 -160.9(2) . . . . yes P2 Mo1 P1 C1 -60.59(19) . . . . yes P3 Mo1 P1 C1 92.3(4) . . . . yes N1 Mo1 P1 C3 -82.9(2) . . . . yes N2 Mo1 P1 C3 84.3(2) . . . . yes P2 Mo1 P1 C3 -175.32(19) . . . . yes P3 Mo1 P1 C3 -22.4(4) . . . . yes N1 Mo1 P1 C2 157.5(2) . . . . yes N2 Mo1 P1 C2 -35.2(2) . . . . yes P2 Mo1 P1 C2 65.13(19) . . . . yes P3 Mo1 P1 C2 -142.0(3) . . . . yes N1 Mo1 P2 C6 -126.8(2) . . . . yes N2 Mo1 P2 C6 56.3(2) . . . . yes P3 Mo1 P2 C6 148.6(2) . . . . yes P1 Mo1 P2 C6 -34.8(2) . . . . yes N1 Mo1 P2 C4 -7.89(19) . . . . yes N2 Mo1 P2 C4 175.26(19) . . . . yes P3 Mo1 P2 C4 -92.49(17) . . . . yes P1 Mo1 P2 C4 84.17(17) . . . . yes N1 Mo1 P2 C5 113.8(2) . . . . yes N2 Mo1 P2 C5 -63.1(2) . . . . yes P3 Mo1 P2 C5 29.17(19) . . . . yes P1 Mo1 P2 C5 -154.17(19) . . . . yes N1 Mo1 P3 C9 71.9(2) . . . . yes N2 Mo1 P3 C9 -95.7(2) . . . . yes P2 Mo1 P3 C9 163.89(18) . . . . yes P1 Mo1 P3 C9 11.0(4) . . . . yes N1 Mo1 P3 C8 -166.8(2) . . . . yes N2 Mo1 P3 C8 25.6(2) . . . . yes P2 Mo1 P3 C8 -74.82(19) . . . . yes P1 Mo1 P3 C8 132.3(3) . . . . yes N1 Mo1 P3 C7 -40.9(2) . . . . yes N2 Mo1 P3 C7 151.5(2) . . . . yes P2 Mo1 P3 C7 51.05(18) . . . . yes P1 Mo1 P3 C7 -101.8(4) . . . . yes N2 Mo1 N1 O1 42(3) . . . . yes P2 Mo1 N1 O1 -124(3) . . . . yes P3 Mo1 N1 O1 -30(3) . . . . yes P1 Mo1 N1 O1 144(3) . . . . yes N1 Mo1 N2 C10 -0.6(7) . . . . yes P2 Mo1 N2 C10 165.23(19) . . . . yes P3 Mo1 N2 C10 71.0(2) . . . . yes P1 Mo1 N2 C10 -102.0(2) . . . . yes N1 Mo1 N2 C161 -130.4(19) . . . . yes P2 Mo1 N2 C161 35.4(19) . . . . yes P3 Mo1 N2 C161 -58.8(19) . . . . yes P1 Mo1 N2 C161 128.2(19) . . . . yes N1 Mo1 N2 C162 -146.5(11) . . . . yes P2 Mo1 N2 C162 19.3(10) . . . . yes P3 Mo1 N2 C162 -74.9(10) . . . . yes P1 Mo1 N2 C162 112.1(10) . . . . yes C161 N2 C10 C15 165.6(9) . . . . yes C162 N2 C10 C15 172.4(7) . . . . yes Mo1 N2 C10 C15 23.9(3) . . . . yes C161 N2 C10 C11 -11.4(10) . . . . yes C162 N2 C10 C11 -4.6(8) . . . . yes Mo1 N2 C10 C11 -153.0(4) . . . . yes N2 C10 C11 C12 178.6(4) . . . . yes C15 C10 C11 C12 1.7(7) . . . . yes C10 C11 C12 C13 -2.9(8) . . . . yes C11 C12 C13 C14 1.6(9) . . . . yes C12 C13 C14 C15 0.9(7) . . . . yes C13 C14 C15 C10 -2.2(6) . . . . yes N2 C10 C15 C14 -176.5(3) . . . . yes C11 C10 C15 C14 0.8(5) . . . . yes C10 N2 C161 C17 91(2) . . . . yes C162 N2 C161 C17 -62(4) . . . . yes Mo1 N2 C161 C17 -142.3(9) . . . . yes C10 N2 C162 C17 69.2(16) . . . . yes C161 N2 C162 C17 99(4) . . . . yes Mo1 N2 C162 C17 -151.2(8) . . . . yes N2 C162 C17 C18 6.4(18) . . . . yes N2 C162 C17 C25 -177.3(9) . . . . yes N2 C162 C17 C161 -88(4) . . . . yes N2 C161 C17 C18 -20(3) . . . . yes N2 C161 C17 C25 169.5(13) . . . . yes N2 C161 C17 C162 73(4) . . . . yes C25 C17 C18 C19 1.8(5) . . . . yes C162 C17 C18 C19 178.1(9) . . . . yes C161 C17 C18 C19 -168.2(15) . . . . yes C17 C18 C19 C20 -0.2(6) . . . . yes C18 C19 C20 C26 -0.8(6) . . . . yes C26 C21 C22 C23 0.3(7) . . . . yes C21 C22 C23 C24 0.6(7) . . . . yes C22 C23 C24 C25 -1.2(7) . . . . yes C23 C24 C25 C17 -179.5(4) . . . . yes C23 C24 C25 C26 0.7(6) . . . . yes C18 C17 C25 C24 177.7(4) . . . . yes C162 C17 C25 C24 1.3(10) . . . . yes C161 C17 C25 C24 -11.9(15) . . . . yes C18 C17 C25 C26 -2.4(5) . . . . yes C162 C17 C25 C26 -178.8(9) . . . . yes C161 C17 C25 C26 168.0(14) . . . . yes C19 C20 C26 C21 -178.7(4) . . . . yes C19 C20 C26 C25 0.1(6) . . . . yes C22 C21 C26 C20 178.1(4) . . . . yes C22 C21 C26 C25 -0.7(6) . . . . yes C24 C25 C26 C20 -178.6(4) . . . . yes C17 C25 C26 C20 1.5(5) . . . . yes C24 C25 C26 C21 0.2(5) . . . . yes C17 C25 C26 C21 -179.6(3) . . . . yes _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.41 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.868 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.076 data_15 _database_code_depnum_ccdc_archive 'CCDC 281550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitrosyl-tris(trimethylphosphine)-N-benzylidene-1-naphthylamine- molybdenum ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H41 Mo N2 O P3' _chemical_formula_weight 586.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.4047(9) _cell_length_b 14.3370(13) _cell_length_c 30.111(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5786.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.10 _exptl_crystal_description block _exptl_crystal_colour green-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.8116 _exptl_absorpt_correction_T_max 0.9150 _exptl_special_details ; see text ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 44150 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.09 _reflns_number_total 6985 _reflns_number_gt 5146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6985 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.521897(12) 0.156340(11) 0.341575(5) 0.01819(6) Uani 1 d . . . P1 P 0.53081(5) -0.01361(4) 0.32613(2) 0.02914(13) Uani 1 d . . . P2 P 0.33226(4) 0.17964(4) 0.33709(2) 0.02699(12) Uani 1 d . . . P3 P 0.54613(5) 0.32425(4) 0.36040(2) 0.02846(13) Uani 1 d . . . N1 N 0.53706(13) 0.18045(13) 0.28392(6) 0.0245(4) Uani 1 d . . . O1 O 0.55344(14) 0.19536(14) 0.24456(5) 0.0403(4) Uani 1 d . . . N2 N 0.53497(13) 0.12052(12) 0.41427(6) 0.0220(4) Uani 1 d . . . H2 H 0.5365 0.0572 0.4076 0.026 Uiso 1 calc R . . C1 C 0.70673(16) 0.13087(14) 0.39976(7) 0.0240(4) Uani 1 d . . . C2 C 0.67617(15) 0.14669(14) 0.35499(7) 0.0221(4) Uani 1 d . . . C3 C 0.75542(17) 0.15930(16) 0.32369(8) 0.0298(5) Uani 1 d . . . H3 H 0.7388 0.1681 0.2933 0.036 Uiso 1 calc R . . C4 C 0.85345(17) 0.15921(16) 0.33539(9) 0.0334(5) Uani 1 d . . . H4 H 0.9028 0.1684 0.3132 0.040 Uiso 1 calc R . . C5 C 0.98547(19) 0.14785(18) 0.39273(11) 0.0417(6) Uani 1 d . . . H5 H 1.0346 0.1604 0.3708 0.050 Uiso 1 calc R . . C6 C 1.0145(2) 0.13238(19) 0.43554(12) 0.0469(7) Uani 1 d . . . H6 H 1.0832 0.1336 0.4432 0.056 Uiso 1 calc R . . C7 C 0.9429(2) 0.11478(18) 0.46793(10) 0.0439(7) Uani 1 d . . . H7 H 0.9632 0.1028 0.4976 0.053 Uiso 1 calc R . . C8 C 0.84256(19) 0.11452(16) 0.45740(9) 0.0346(5) Uani 1 d . . . H8 H 0.7947 0.1040 0.4801 0.041 Uiso 1 calc R . . C9 C 0.81000(16) 0.12972(14) 0.41327(8) 0.0260(4) Uani 1 d . . . C10 C 0.88381(17) 0.14556(15) 0.38039(9) 0.0301(5) Uani 1 d . . . C11 C 0.62668(16) 0.11648(14) 0.42968(7) 0.0243(4) Uani 1 d . . . H11A H 0.6358 0.0544 0.4435 0.029 Uiso 1 calc R . . H11B H 0.6327 0.1633 0.4537 0.029 Uiso 1 calc R . . C12 C 0.45477(17) 0.10620(15) 0.44429(7) 0.0259(4) Uani 1 d . . . C13 C 0.37957(18) 0.04439(17) 0.43292(8) 0.0320(5) Uani 1 d . . . H13 H 0.3838 0.0105 0.4059 0.038 Uiso 1 calc R . . C14 C 0.2980(2) 0.0316(2) 0.46073(9) 0.0409(6) Uani 1 d . . . H14 H 0.2472 -0.0117 0.4528 0.049 Uiso 1 calc R . . C15 C 0.2905(2) 0.08170(19) 0.49995(10) 0.0441(7) Uani 1 d . . . H15 H 0.2341 0.0739 0.5187 0.053 Uiso 1 calc R . . C16 C 0.3653(2) 0.14293(18) 0.51152(9) 0.0432(6) Uani 1 d . . . H16 H 0.3607 0.1769 0.5385 0.052 Uiso 1 calc R . . C17 C 0.4475(2) 0.15542(17) 0.48405(8) 0.0353(5) Uani 1 d . . . H17 H 0.4989 0.1976 0.4924 0.042 Uiso 1 calc R . . C18 C 0.4257(3) -0.0884(2) 0.31115(12) 0.0560(8) Uani 1 d . . . H18A H 0.3923 -0.0630 0.2849 0.084 Uiso 1 calc R . . H18B H 0.3784 -0.0911 0.3359 0.084 Uiso 1 calc R . . H18C H 0.4501 -0.1514 0.3046 0.084 Uiso 1 calc R . . C19 C 0.5880(3) -0.08410(19) 0.36967(10) 0.0517(8) Uani 1 d . . . H19A H 0.6019 -0.1467 0.3582 0.077 Uiso 1 calc R . . H19B H 0.5423 -0.0886 0.3950 0.077 Uiso 1 calc R . . H19C H 0.6504 -0.0548 0.3793 0.077 Uiso 1 calc R . . C20 C 0.6136(3) -0.0340(2) 0.27921(10) 0.0530(8) Uani 1 d . . . H20A H 0.6210 -0.1013 0.2745 0.079 Uiso 1 calc R . . H20B H 0.6790 -0.0064 0.2854 0.079 Uiso 1 calc R . . H20C H 0.5853 -0.0052 0.2525 0.079 Uiso 1 calc R . . C21 C 0.3036(2) 0.25822(19) 0.29103(8) 0.0383(6) Uani 1 d . . . H21A H 0.3410 0.2389 0.2646 0.057 Uiso 1 calc R . . H21B H 0.3225 0.3220 0.2991 0.057 Uiso 1 calc R . . H21C H 0.2319 0.2559 0.2847 0.057 Uiso 1 calc R . . C22 C 0.2465(2) 0.0841(2) 0.32378(13) 0.0544(8) Uani 1 d . . . H22A H 0.1789 0.1089 0.3201 0.082 Uiso 1 calc R . . H22B H 0.2470 0.0384 0.3480 0.082 Uiso 1 calc R . . H22C H 0.2678 0.0539 0.2962 0.082 Uiso 1 calc R . . C23 C 0.2626(2) 0.2340(2) 0.38283(10) 0.0475(7) Uani 1 d . . . H23A H 0.2964 0.2915 0.3920 0.071 Uiso 1 calc R . . H23B H 0.2596 0.1908 0.4080 0.071 Uiso 1 calc R . . H23C H 0.1948 0.2487 0.3729 0.071 Uiso 1 calc R . . C24 C 0.6175(4) 0.3515(2) 0.40915(13) 0.0814(14) Uani 1 d . . . H24A H 0.6816 0.3187 0.4080 0.122 Uiso 1 calc R . . H24B H 0.5807 0.3317 0.4356 0.122 Uiso 1 calc R . . H24C H 0.6293 0.4189 0.4105 0.122 Uiso 1 calc R . . C25 C 0.6192(5) 0.3807(3) 0.31819(15) 0.113(2) Uani 1 d . . . H25A H 0.6244 0.4474 0.3249 0.169 Uiso 1 calc R . . H25B H 0.5870 0.3723 0.2892 0.169 Uiso 1 calc R . . H25C H 0.6861 0.3532 0.3174 0.169 Uiso 1 calc R . . C26 C 0.4481(4) 0.4096(3) 0.3668(3) 0.182(4) Uani 1 d . . . H26A H 0.4776 0.4715 0.3712 0.272 Uiso 1 calc R . . H26B H 0.4070 0.3935 0.3926 0.272 Uiso 1 calc R . . H26C H 0.4064 0.4103 0.3400 0.272 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01721(8) 0.01888(8) 0.01849(8) -0.00038(6) 0.00059(6) -0.00188(6) P1 0.0365(3) 0.0211(2) 0.0298(3) -0.0053(2) 0.0037(3) -0.0007(2) P2 0.0193(2) 0.0314(3) 0.0303(3) 0.0017(2) -0.0011(2) -0.0031(2) P3 0.0292(3) 0.0204(2) 0.0358(3) -0.0022(2) -0.0080(2) -0.0020(2) N1 0.0208(9) 0.0269(9) 0.0259(9) 0.0010(7) 0.0009(7) -0.0015(7) O1 0.0425(10) 0.0577(11) 0.0207(8) 0.0082(8) 0.0046(7) -0.0017(9) N2 0.0250(9) 0.0199(8) 0.0210(8) 0.0008(6) 0.0024(7) -0.0004(7) C1 0.0215(10) 0.0228(9) 0.0277(11) 0.0002(8) -0.0028(8) 0.0004(8) C2 0.0188(9) 0.0216(9) 0.0258(10) 0.0009(8) 0.0001(8) 0.0002(8) C3 0.0242(10) 0.0339(11) 0.0313(11) 0.0024(10) 0.0041(9) -0.0015(9) C4 0.0212(10) 0.0334(11) 0.0457(14) 0.0014(10) 0.0089(10) -0.0013(9) C5 0.0207(11) 0.0371(13) 0.0673(19) -0.0077(12) -0.0012(12) 0.0008(10) C6 0.0267(12) 0.0402(14) 0.074(2) -0.0119(14) -0.0167(14) 0.0050(11) C7 0.0419(15) 0.0336(13) 0.0561(17) -0.0050(12) -0.0240(14) 0.0059(11) C8 0.0344(13) 0.0277(11) 0.0417(14) -0.0006(10) -0.0113(11) 0.0000(10) C9 0.0230(10) 0.0185(9) 0.0366(12) -0.0010(8) -0.0052(9) 0.0008(8) C10 0.0203(10) 0.0226(10) 0.0475(14) -0.0020(10) -0.0012(9) 0.0007(8) C11 0.0268(10) 0.0198(9) 0.0262(11) 0.0001(8) -0.0028(9) 0.0005(8) C12 0.0275(11) 0.0265(10) 0.0238(10) 0.0066(8) 0.0049(8) 0.0039(8) C13 0.0331(12) 0.0376(12) 0.0253(11) 0.0033(9) 0.0063(9) -0.0041(10) C14 0.0348(13) 0.0460(14) 0.0419(14) 0.0089(12) 0.0110(11) -0.0080(12) C15 0.0472(16) 0.0412(14) 0.0438(15) 0.0109(11) 0.0242(13) 0.0065(12) C16 0.0610(18) 0.0354(13) 0.0331(13) -0.0002(11) 0.0208(13) 0.0056(12) C17 0.0458(14) 0.0308(11) 0.0294(12) -0.0010(9) 0.0104(10) -0.0001(11) C18 0.058(2) 0.0349(14) 0.075(2) -0.0249(14) 0.0015(17) -0.0111(13) C19 0.077(2) 0.0270(12) 0.0510(17) 0.0014(11) -0.0067(16) 0.0126(13) C20 0.067(2) 0.0421(15) 0.0493(17) -0.0147(13) 0.0204(15) 0.0074(14) C21 0.0340(13) 0.0478(14) 0.0330(13) 0.0048(11) -0.0085(10) 0.0012(11) C22 0.0297(13) 0.0440(15) 0.089(2) -0.0007(15) -0.0134(16) -0.0085(12) C23 0.0344(14) 0.0640(18) 0.0442(15) 0.0069(14) 0.0104(12) 0.0126(13) C24 0.150(4) 0.0345(15) 0.060(2) -0.0042(15) -0.047(3) -0.018(2) C25 0.219(6) 0.046(2) 0.074(3) 0.0013(19) 0.040(3) -0.059(3) C26 0.066(3) 0.050(2) 0.429(13) -0.099(5) -0.071(5) 0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.7819(18) . yes Mo1 C2 2.112(2) . yes Mo1 N2 2.2551(17) . yes Mo1 P1 2.4835(6) . yes Mo1 P3 2.4945(6) . yes Mo1 P2 2.5674(6) . yes P1 C20 1.820(3) . yes P1 C19 1.824(3) . yes P1 C18 1.827(3) . yes P2 C21 1.828(3) . yes P2 C22 1.832(3) . yes P2 C23 1.837(3) . yes P3 C24 1.795(3) . yes P3 C25 1.797(4) . yes P3 C26 1.807(4) . yes N1 O1 1.224(2) . yes N2 C11 1.315(3) . yes N2 C12 1.420(3) . yes N2 H2 0.9300 . yes C1 C11 1.416(3) . yes C1 C2 1.427(3) . yes C1 C9 1.443(3) . yes C2 C3 1.432(3) . yes C3 C4 1.361(3) . yes C3 H3 0.9500 . yes C4 C10 1.428(4) . yes C4 H4 0.9500 . yes C5 C6 1.365(5) . yes C5 C10 1.413(3) . yes C5 H5 0.9500 . yes C6 C7 1.392(5) . yes C6 H6 0.9500 . yes C7 C8 1.382(4) . yes C7 H7 0.9500 . yes C8 C9 1.415(3) . yes C8 H8 0.9500 . yes C9 C10 1.418(3) . yes C11 H11A 0.9900 . yes C11 H11B 0.9900 . yes C12 C13 1.385(3) . yes C12 C17 1.393(3) . yes C13 C14 1.390(3) . yes C13 H13 0.9500 . yes C14 C15 1.386(4) . yes C14 H14 0.9500 . yes C15 C16 1.378(4) . yes C15 H15 0.9500 . yes C16 C17 1.390(4) . yes C16 H16 0.9500 . yes C17 H17 0.9500 . yes C18 H18A 0.9800 . yes C18 H18B 0.9800 . yes C18 H18C 0.9800 . yes C19 H19A 0.9800 . yes C19 H19B 0.9800 . yes C19 H19C 0.9800 . yes C20 H20A 0.9800 . yes C20 H20B 0.9800 . yes C20 H20C 0.9800 . yes C21 H21A 0.9800 . yes C21 H21B 0.9800 . yes C21 H21C 0.9800 . yes C22 H22A 0.9800 . yes C22 H22B 0.9800 . yes C22 H22C 0.9800 . yes C23 H23A 0.9800 . yes C23 H23B 0.9800 . yes C23 H23C 0.9800 . yes C24 H24A 0.9800 . yes C24 H24B 0.9800 . yes C24 H24C 0.9800 . yes C25 H25A 0.9800 . yes C25 H25B 0.9800 . yes C25 H25C 0.9800 . yes C26 H26A 0.9800 . yes C26 H26B 0.9800 . yes C26 H26C 0.9800 . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 C2 95.02(8) . . yes N1 Mo1 N2 168.82(7) . . yes C2 Mo1 N2 73.94(7) . . yes N1 Mo1 P1 90.13(6) . . yes C2 Mo1 P1 85.67(6) . . yes N2 Mo1 P1 87.40(5) . . yes N1 Mo1 P3 91.11(6) . . yes C2 Mo1 P3 83.81(6) . . yes N2 Mo1 P3 89.37(5) . . yes P1 Mo1 P3 169.48(2) . . yes N1 Mo1 P2 92.09(6) . . yes C2 Mo1 P2 171.20(6) . . yes N2 Mo1 P2 99.07(5) . . yes P1 Mo1 P2 99.52(2) . . yes P3 Mo1 P2 90.88(2) . . yes C20 P1 C19 102.29(16) . . yes C20 P1 C18 100.62(16) . . yes C19 P1 C18 100.14(17) . . yes C20 P1 Mo1 109.40(10) . . yes C19 P1 Mo1 115.41(10) . . yes C18 P1 Mo1 125.82(11) . . yes C21 P2 C22 99.37(14) . . yes C21 P2 C23 101.56(13) . . yes C22 P2 C23 99.35(16) . . yes C21 P2 Mo1 109.17(9) . . yes C22 P2 Mo1 122.36(10) . . yes C23 P2 Mo1 121.25(10) . . yes C24 P3 C25 100.9(3) . . yes C24 P3 C26 98.8(3) . . yes C25 P3 C26 99.6(4) . . yes C24 P3 Mo1 117.70(11) . . yes C25 P3 Mo1 110.18(14) . . yes C26 P3 Mo1 125.69(15) . . yes O1 N1 Mo1 176.07(17) . . yes C11 N2 C12 118.46(19) . . yes C11 N2 Mo1 115.16(14) . . yes C12 N2 Mo1 126.32(14) . . yes C11 N2 H2 90.8 . . yes C12 N2 H2 90.8 . . yes Mo1 N2 H2 90.8 . . yes C11 C1 C2 113.99(19) . . yes C11 C1 C9 123.1(2) . . yes C2 C1 C9 122.9(2) . . yes C1 C2 C3 115.40(19) . . yes C1 C2 Mo1 118.18(15) . . yes C3 C2 Mo1 126.33(16) . . yes C4 C3 C2 123.1(2) . . yes C4 C3 H3 118.5 . . yes C2 C3 H3 118.5 . . yes C3 C4 C10 121.4(2) . . yes C3 C4 H4 119.3 . . yes C10 C4 H4 119.3 . . yes C6 C5 C10 121.3(3) . . yes C6 C5 H5 119.3 . . yes C10 C5 H5 119.3 . . yes C5 C6 C7 119.7(2) . . yes C5 C6 H6 120.2 . . yes C7 C6 H6 120.2 . . yes C8 C7 C6 120.7(3) . . yes C8 C7 H7 119.6 . . yes C6 C7 H7 119.6 . . yes C7 C8 C9 121.0(3) . . yes C7 C8 H8 119.5 . . yes C9 C8 H8 119.5 . . yes C8 C9 C10 117.7(2) . . yes C8 C9 C1 124.2(2) . . yes C10 C9 C1 118.1(2) . . yes C5 C10 C9 119.5(2) . . yes C5 C10 C4 121.4(2) . . yes C9 C10 C4 119.1(2) . . yes N2 C11 C1 118.5(2) . . yes N2 C11 H11A 107.7 . . yes C1 C11 H11A 107.7 . . yes N2 C11 H11B 107.7 . . yes C1 C11 H11B 107.7 . . yes H11A C11 H11B 107.1 . . yes C13 C12 C17 119.1(2) . . yes C13 C12 N2 119.1(2) . . yes C17 C12 N2 121.8(2) . . yes C12 C13 C14 120.6(2) . . yes C12 C13 H13 119.7 . . yes C14 C13 H13 119.7 . . yes C15 C14 C13 120.1(3) . . yes C15 C14 H14 119.9 . . yes C13 C14 H14 119.9 . . yes C16 C15 C14 119.5(2) . . yes C16 C15 H15 120.2 . . yes C14 C15 H15 120.2 . . yes C15 C16 C17 120.6(2) . . yes C15 C16 H16 119.7 . . yes C17 C16 H16 119.7 . . yes C16 C17 C12 120.1(2) . . yes C16 C17 H17 120.0 . . yes C12 C17 H17 120.0 . . yes P1 C18 H18A 109.5 . . yes P1 C18 H18B 109.5 . . yes H18A C18 H18B 109.5 . . yes P1 C18 H18C 109.5 . . yes H18A C18 H18C 109.5 . . yes H18B C18 H18C 109.5 . . yes P1 C19 H19A 109.5 . . yes P1 C19 H19B 109.5 . . yes H19A C19 H19B 109.5 . . yes P1 C19 H19C 109.5 . . yes H19A C19 H19C 109.5 . . yes H19B C19 H19C 109.5 . . yes P1 C20 H20A 109.5 . . yes P1 C20 H20B 109.5 . . yes H20A C20 H20B 109.5 . . yes P1 C20 H20C 109.5 . . yes H20A C20 H20C 109.5 . . yes H20B C20 H20C 109.5 . . yes P2 C21 H21A 109.5 . . yes P2 C21 H21B 109.5 . . yes H21A C21 H21B 109.5 . . yes P2 C21 H21C 109.5 . . yes H21A C21 H21C 109.5 . . yes H21B C21 H21C 109.5 . . yes P2 C22 H22A 109.5 . . yes P2 C22 H22B 109.5 . . yes H22A C22 H22B 109.5 . . yes P2 C22 H22C 109.5 . . yes H22A C22 H22C 109.5 . . yes H22B C22 H22C 109.5 . . yes P2 C23 H23A 109.5 . . yes P2 C23 H23B 109.5 . . yes H23A C23 H23B 109.5 . . yes P2 C23 H23C 109.5 . . yes H23A C23 H23C 109.5 . . yes H23B C23 H23C 109.5 . . yes P3 C24 H24A 109.5 . . yes P3 C24 H24B 109.5 . . yes H24A C24 H24B 109.5 . . yes P3 C24 H24C 109.5 . . yes H24A C24 H24C 109.5 . . yes H24B C24 H24C 109.5 . . yes P3 C25 H25A 109.5 . . yes P3 C25 H25B 109.5 . . yes H25A C25 H25B 109.5 . . yes P3 C25 H25C 109.5 . . yes H25A C25 H25C 109.5 . . yes H25B C25 H25C 109.5 . . yes P3 C26 H26A 109.5 . . yes P3 C26 H26B 109.5 . . yes H26A C26 H26B 109.5 . . yes P3 C26 H26C 109.5 . . yes H26A C26 H26C 109.5 . . yes H26B C26 H26C 109.5 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mo1 P1 C20 32.50(14) . . . . yes C2 Mo1 P1 C20 -62.52(14) . . . . yes N2 Mo1 P1 C20 -136.59(14) . . . . yes P3 Mo1 P1 C20 -64.30(18) . . . . yes P2 Mo1 P1 C20 124.64(13) . . . . yes N1 Mo1 P1 C19 147.16(14) . . . . yes C2 Mo1 P1 C19 52.14(15) . . . . yes N2 Mo1 P1 C19 -21.94(14) . . . . yes P3 Mo1 P1 C19 50.36(19) . . . . yes P2 Mo1 P1 C19 -120.70(13) . . . . yes N1 Mo1 P1 C18 -87.17(16) . . . . yes C2 Mo1 P1 C18 177.81(16) . . . . yes N2 Mo1 P1 C18 103.73(16) . . . . yes P3 Mo1 P1 C18 176.03(18) . . . . yes P2 Mo1 P1 C18 4.97(15) . . . . yes N1 Mo1 P2 C21 -26.20(11) . . . . yes C2 Mo1 P2 C21 117.7(4) . . . . yes N2 Mo1 P2 C21 154.45(11) . . . . yes P1 Mo1 P2 C21 -116.69(10) . . . . yes P3 Mo1 P2 C21 64.94(10) . . . . yes N1 Mo1 P2 C22 88.91(16) . . . . yes C2 Mo1 P2 C22 -127.2(4) . . . . yes N2 Mo1 P2 C22 -90.44(15) . . . . yes P1 Mo1 P2 C22 -1.58(15) . . . . yes P3 Mo1 P2 C22 -179.95(15) . . . . yes N1 Mo1 P2 C23 -143.54(13) . . . . yes C2 Mo1 P2 C23 0.3(4) . . . . yes N2 Mo1 P2 C23 37.11(13) . . . . yes P1 Mo1 P2 C23 125.98(12) . . . . yes P3 Mo1 P2 C23 -52.39(12) . . . . yes N1 Mo1 P3 C24 -140.7(2) . . . . yes C2 Mo1 P3 C24 -45.8(2) . . . . yes N2 Mo1 P3 C24 28.2(2) . . . . yes P1 Mo1 P3 C24 -44.0(2) . . . . yes P2 Mo1 P3 C24 127.2(2) . . . . yes N1 Mo1 P3 C25 -25.8(2) . . . . yes C2 Mo1 P3 C25 69.2(3) . . . . yes N2 Mo1 P3 C25 143.1(2) . . . . yes P1 Mo1 P3 C25 70.9(3) . . . . yes P2 Mo1 P3 C25 -117.9(2) . . . . yes N1 Mo1 P3 C26 93.1(4) . . . . yes C2 Mo1 P3 C26 -172.0(4) . . . . yes N2 Mo1 P3 C26 -98.1(4) . . . . yes P1 Mo1 P3 C26 -170.2(4) . . . . yes P2 Mo1 P3 C26 1.0(4) . . . . yes C2 Mo1 N1 O1 13(2) . . . . yes N2 Mo1 N1 O1 5(3) . . . . yes P1 Mo1 N1 O1 -72(2) . . . . yes P3 Mo1 N1 O1 97(2) . . . . yes P2 Mo1 N1 O1 -172(2) . . . . yes N1 Mo1 N2 C11 12.4(4) . . . . yes C2 Mo1 N2 C11 3.58(14) . . . . yes P1 Mo1 N2 C11 89.82(14) . . . . yes P3 Mo1 N2 C11 -80.16(14) . . . . yes P2 Mo1 N2 C11 -170.95(14) . . . . yes N1 Mo1 N2 C12 -170.3(3) . . . . yes C2 Mo1 N2 C12 -179.13(18) . . . . yes P1 Mo1 N2 C12 -92.90(16) . . . . yes P3 Mo1 N2 C12 97.12(16) . . . . yes P2 Mo1 N2 C12 6.34(17) . . . . yes C11 C1 C2 C3 -178.58(19) . . . . yes C9 C1 C2 C3 1.5(3) . . . . yes C11 C1 C2 Mo1 4.5(2) . . . . yes C9 C1 C2 Mo1 -175.43(15) . . . . yes N1 Mo1 C2 C1 177.45(16) . . . . yes N2 Mo1 C2 C1 -4.26(15) . . . . yes P1 Mo1 C2 C1 -92.80(15) . . . . yes P3 Mo1 C2 C1 86.88(15) . . . . yes P2 Mo1 C2 C1 33.7(5) . . . . yes N1 Mo1 C2 C3 0.94(19) . . . . yes N2 Mo1 C2 C3 179.2(2) . . . . yes P1 Mo1 C2 C3 90.69(18) . . . . yes P3 Mo1 C2 C3 -89.64(18) . . . . yes P2 Mo1 C2 C3 -142.8(3) . . . . yes C1 C2 C3 C4 -1.9(3) . . . . yes Mo1 C2 C3 C4 174.71(18) . . . . yes C2 C3 C4 C10 0.5(4) . . . . yes C10 C5 C6 C7 -0.6(4) . . . . yes C5 C6 C7 C8 -1.2(4) . . . . yes C6 C7 C8 C9 1.6(4) . . . . yes C7 C8 C9 C10 -0.3(3) . . . . yes C7 C8 C9 C1 -179.7(2) . . . . yes C11 C1 C9 C8 -0.2(3) . . . . yes C2 C1 C9 C8 179.8(2) . . . . yes C11 C1 C9 C10 -179.63(19) . . . . yes C2 C1 C9 C10 0.3(3) . . . . yes C6 C5 C10 C9 2.0(4) . . . . yes C6 C5 C10 C4 -178.3(2) . . . . yes C8 C9 C10 C5 -1.5(3) . . . . yes C1 C9 C10 C5 178.0(2) . . . . yes C8 C9 C10 C4 178.7(2) . . . . yes C1 C9 C10 C4 -1.8(3) . . . . yes C3 C4 C10 C5 -178.4(2) . . . . yes C3 C4 C10 C9 1.4(3) . . . . yes C12 N2 C11 C1 -179.93(18) . . . . yes Mo1 N2 C11 C1 -2.4(2) . . . . yes C2 C1 C11 N2 -1.2(3) . . . . yes C9 C1 C11 N2 178.78(19) . . . . yes C11 N2 C12 C13 -131.3(2) . . . . yes Mo1 N2 C12 C13 51.4(3) . . . . yes C11 N2 C12 C17 51.3(3) . . . . yes Mo1 N2 C12 C17 -125.9(2) . . . . yes C17 C12 C13 C14 0.0(4) . . . . yes N2 C12 C13 C14 -177.4(2) . . . . yes C12 C13 C14 C15 0.9(4) . . . . yes C13 C14 C15 C16 -1.2(4) . . . . yes C14 C15 C16 C17 0.6(4) . . . . yes C15 C16 C17 C12 0.3(4) . . . . yes C13 C12 C17 C16 -0.6(4) . . . . yes N2 C12 C17 C16 176.7(2) . . . . yes _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.685 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.073 #======================================END=============================