Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Martyn Coles' 'Joanna Grundy' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Martyn Coles ' _publ_contact_author_address ; Dr Martyn Coles Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'M.P.COLES@SUSSEX.AC.UK ' _publ_section_title ; Synthesis and coordination chemistry of neutral phospha(III)guanidines. Formation of 1-aza-3-phospha-4-metallacyclobut-1-ene rings at group 6 metal centres ; data_mpc-1a(jul702) _database_code_CSD 205561 _audit_creation_date 2002-07-23T16:39:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Ph2PC(NHCy)(NCy)] _chemical_formula_moiety 'C25 H33 N2 P1' _chemical_formula_sum 'C25 H33 N2 P1' _chemical_formula_weight 392.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.0943(2) _cell_length_b 11.6147(2) _cell_length_c 21.0144(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2219.70(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6473 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_number 11636 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _reflns_number_total 3593 _reflns_number_gt 3315 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.6137P] 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 'H1 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 3593 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _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 -0.06(8) _refine_diff_density_max 0.195 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.035 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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 P P 0.47798(6) 0.05920(4) 0.83780(2) 0.02229(13) Uani 1 1 d . . . N1 N 0.2618(2) -0.09551(13) 0.80166(8) 0.0246(4) Uani 1 1 d . . . H1 H 0.322(3) -0.1072(18) 0.7710(11) 0.035(6) Uiso 1 1 d . . . N2 N 0.2132(2) -0.00246(14) 0.89606(7) 0.0243(4) Uani 1 1 d . . . C1 C 0.2992(2) -0.01944(14) 0.84839(8) 0.0209(4) Uani 1 1 d . . . C2 C 0.5266(3) 0.02287(15) 0.75558(8) 0.0240(4) Uani 1 1 d . . . C3 C 0.4703(3) 0.09429(17) 0.70825(9) 0.0330(5) Uani 1 1 d . . . H3 H 0.4086 0.157 0.7197 0.04 Uiso 1 1 calc R . . C4 C 0.5031(3) 0.07509(19) 0.64473(9) 0.0411(6) Uani 1 1 d . . . H4 H 0.462 0.1234 0.6129 0.049 Uiso 1 1 calc R . . C5 C 0.5947(3) -0.0137(2) 0.62776(10) 0.0415(6) Uani 1 1 d . . . H5 H 0.6184 -0.026 0.5843 0.05 Uiso 1 1 calc R . . C6 C 0.6521(3) -0.0846(2) 0.67369(10) 0.0452(6) Uani 1 1 d . . . H6 H 0.7155 -0.1459 0.6619 0.054 Uiso 1 1 calc R . . C7 C 0.6179(3) -0.06722(18) 0.73746(9) 0.0341(5) Uani 1 1 d . . . H7 H 0.6572 -0.1174 0.7689 0.041 Uiso 1 1 calc R . . C8 C 0.6000(2) -0.03235(15) 0.88517(8) 0.0215(4) Uani 1 1 d . . . C9 C 0.7504(3) -0.00734(17) 0.88540(9) 0.0275(5) Uani 1 1 d . . . H9 H 0.7872 0.0506 0.8577 0.033 Uiso 1 1 calc R . . C10 C 0.8469(2) -0.06520(19) 0.92510(10) 0.0327(5) Uani 1 1 d . . . H10 H 0.949 -0.0481 0.9239 0.039 Uiso 1 1 calc R . . C11 C 0.7941(3) -0.14799(19) 0.96656(10) 0.0355(6) Uani 1 1 d . . . H11 H 0.8594 -0.1857 0.995 0.043 Uiso 1 1 calc R . . C12 C 0.6466(3) -0.17563(19) 0.96647(10) 0.0339(5) Uani 1 1 d . . . H12 H 0.6107 -0.2337 0.9943 0.041 Uiso 1 1 calc R . . C13 C 0.5498(2) -0.11850(16) 0.92563(9) 0.0279(5) Uani 1 1 d . . . H13 H 0.4486 -0.1387 0.9255 0.033 Uiso 1 1 calc R . . C14 C 0.1300(2) -0.16768(15) 0.80269(8) 0.0212(4) Uani 1 1 d . . . H14 H 0.0428 -0.1176 0.8113 0.025 Uiso 1 1 calc R . . C15 C 0.1109(3) -0.22316(17) 0.73760(9) 0.0310(5) Uani 1 1 d . . . H15B H 0.2006 -0.2674 0.7268 0.037 Uiso 1 1 calc R . . H15A H 0.0983 -0.1623 0.7051 0.037 Uiso 1 1 calc R . . C16 C -0.0221(3) -0.30346(17) 0.73618(10) 0.0380(6) Uani 1 1 d . . . H16B H -0.1128 -0.2576 0.742 0.046 Uiso 1 1 calc R . . H16A H -0.0276 -0.3413 0.694 0.046 Uiso 1 1 calc R . . C17 C -0.0137(3) -0.39487(17) 0.78763(10) 0.0371(5) Uani 1 1 d . . . H17B H 0.0704 -0.4467 0.7791 0.045 Uiso 1 1 calc R . . H17A H -0.1048 -0.4416 0.7871 0.045 Uiso 1 1 calc R . . C18 C 0.0050(3) -0.33950(18) 0.85275(9) 0.0424(6) Uani 1 1 d . . . H18B H 0.017 -0.4004 0.8853 0.051 Uiso 1 1 calc R . . H18A H -0.0845 -0.2949 0.8634 0.051 Uiso 1 1 calc R . . C19 C 0.1381(3) -0.26001(17) 0.85406(9) 0.0316(5) Uani 1 1 d . . . H19B H 0.2285 -0.3062 0.8479 0.038 Uiso 1 1 calc R . . H19A H 0.1445 -0.2226 0.8963 0.038 Uiso 1 1 calc R . . C20 C 0.2575(2) 0.07745(16) 0.94665(8) 0.0249(4) Uani 1 1 d . . . H20 H 0.3627 0.0994 0.9401 0.03 Uiso 1 1 calc R . . C21 C 0.1635(3) 0.18575(17) 0.94561(9) 0.0297(5) Uani 1 1 d . . . H21B H 0.0587 0.1644 0.9502 0.036 Uiso 1 1 calc R . . H21A H 0.1757 0.2252 0.9042 0.036 Uiso 1 1 calc R . . C22 C 0.2068(3) 0.26790(17) 0.99942(10) 0.0343(5) Uani 1 1 d . . . H22B H 0.3088 0.295 0.9927 0.041 Uiso 1 1 calc R . . H22A H 0.1411 0.3359 0.9989 0.041 Uiso 1 1 calc R . . C23 C 0.1957(3) 0.20829(18) 1.06379(9) 0.0372(6) Uani 1 1 d . . . H23B H 0.2317 0.261 1.0974 0.045 Uiso 1 1 calc R . . H23A H 0.0913 0.1906 1.0729 0.045 Uiso 1 1 calc R . . C24 C 0.2846(3) 0.09763(17) 1.06550(9) 0.0348(6) Uani 1 1 d . . . H24B H 0.2676 0.058 1.1066 0.042 Uiso 1 1 calc R . . H24A H 0.3906 0.1163 1.0625 0.042 Uiso 1 1 calc R . . C25 C 0.2424(3) 0.01742(17) 1.01099(9) 0.0296(5) Uani 1 1 d . . . H25B H 0.1395 -0.0085 1.0167 0.035 Uiso 1 1 calc R . . H25A H 0.3065 -0.0514 1.0118 0.035 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 P 0.0221(3) 0.0217(2) 0.0230(2) -0.00097(19) 0.0025(2) -0.0016(2) N1 0.0247(11) 0.0279(9) 0.0213(9) -0.0055(7) 0.0043(8) -0.0067(8) N2 0.0202(11) 0.0310(9) 0.0217(8) -0.0060(7) -0.0003(7) -0.0021(8) C1 0.0228(12) 0.0202(9) 0.0197(9) 0.0003(7) -0.0017(9) 0.0016(8) C2 0.0230(12) 0.0247(9) 0.0245(9) -0.0011(7) 0.0043(9) -0.0062(9) C3 0.0361(14) 0.0322(11) 0.0306(11) 0.0025(8) -0.0003(10) -0.0003(10) C4 0.0526(18) 0.0435(12) 0.0274(11) 0.0059(9) -0.0054(11) -0.0084(13) C5 0.0507(18) 0.0512(14) 0.0227(11) -0.0068(10) 0.0056(11) -0.0125(13) C6 0.0501(18) 0.0494(14) 0.0359(13) -0.0125(11) 0.0056(12) 0.0084(12) C7 0.0402(15) 0.0339(11) 0.0283(11) -0.0021(9) 0.0015(10) 0.0060(11) C8 0.0199(12) 0.0249(10) 0.0197(10) -0.0051(7) 0.0008(8) -0.0021(8) C9 0.0230(13) 0.0285(10) 0.0311(11) -0.0028(9) 0.0039(9) -0.0044(9) C10 0.0164(13) 0.0423(12) 0.0393(11) -0.0130(10) -0.0007(9) -0.0006(10) C11 0.0288(16) 0.0459(13) 0.0318(11) -0.0016(10) -0.0064(10) 0.0086(11) C12 0.0256(15) 0.0432(13) 0.0331(12) 0.0082(10) -0.0010(10) 0.0019(10) C13 0.0181(13) 0.0343(11) 0.0313(11) 0.0034(9) 0.0003(9) -0.0014(9) C14 0.0182(13) 0.0236(10) 0.0219(10) -0.0022(8) -0.0016(8) -0.0017(8) C15 0.0410(15) 0.0295(10) 0.0224(10) -0.0021(8) -0.0031(10) -0.0020(10) C16 0.0381(15) 0.0364(11) 0.0395(12) -0.0097(9) -0.0110(12) -0.0048(11) C17 0.0325(15) 0.0291(10) 0.0497(13) -0.0066(9) 0.0003(11) -0.0080(11) C18 0.0514(19) 0.0368(11) 0.0388(12) -0.0004(9) 0.0082(12) -0.0190(12) C19 0.0356(15) 0.0330(11) 0.0263(11) 0.0026(8) -0.0030(10) -0.0077(10) C20 0.0192(12) 0.0318(10) 0.0237(9) -0.0059(8) 0.0028(8) -0.0025(9) C21 0.0325(15) 0.0295(11) 0.0271(10) -0.0006(8) -0.0003(10) -0.0009(10) C22 0.0419(16) 0.0258(11) 0.0352(11) -0.0039(9) -0.0015(11) -0.0006(10) C23 0.0474(17) 0.0353(12) 0.0288(11) -0.0102(9) 0.0043(11) -0.0044(11) C24 0.0429(16) 0.0385(12) 0.0232(10) -0.0025(9) -0.0034(10) -0.0018(11) C25 0.0323(14) 0.0299(10) 0.0265(10) -0.0027(8) -0.0020(9) 0.0017(10) #----------------------------------------------------------------------------# # 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 P C8 1.831(2) . ? P C2 1.8327(18) . ? P C1 1.878(2) . ? N1 C1 1.364(2) . ? N1 C14 1.463(3) . ? N2 C1 1.286(2) . ? N2 C20 1.468(2) . ? C2 C7 1.389(3) . ? C2 C3 1.393(3) . ? C3 C4 1.386(3) . ? C4 C5 1.373(3) . ? C5 C6 1.372(3) . ? C6 C7 1.390(3) . ? C8 C13 1.390(3) . ? C8 C9 1.398(3) . ? C9 C10 1.385(3) . ? C10 C11 1.383(3) . ? C11 C12 1.380(3) . ? C12 C13 1.397(3) . ? C14 C15 1.522(2) . ? C14 C19 1.524(3) . ? C15 C16 1.527(3) . ? C16 C17 1.517(3) . ? C17 C18 1.522(3) . ? C18 C19 1.523(3) . ? C20 C21 1.521(3) . ? C20 C25 1.527(3) . ? C21 C22 1.531(3) . ? C22 C23 1.523(3) . ? C23 C24 1.519(3) . ? C24 C25 1.525(3) . ? 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 C8 P C2 103.44(9) . . ? C8 P C1 100.25(9) . . ? C2 P C1 102.05(9) . . ? C1 N1 C14 124.39(17) . . ? C1 N2 C20 119.63(17) . . ? N2 C1 N1 120.56(19) . . ? N2 C1 P 122.97(14) . . ? N1 C1 P 116.46(14) . . ? C7 C2 C3 118.21(18) . . ? C7 C2 P 125.18(15) . . ? C3 C2 P 116.57(15) . . ? C4 C3 C2 120.9(2) . . ? C5 C4 C3 120.1(2) . . ? C6 C5 C4 119.9(2) . . ? C5 C6 C7 120.4(2) . . ? C2 C7 C6 120.5(2) . . ? C13 C8 C9 117.95(19) . . ? C13 C8 P 123.47(16) . . ? C9 C8 P 118.30(15) . . ? C10 C9 C8 121.40(19) . . ? C11 C10 C9 119.8(2) . . ? C12 C11 C10 119.9(2) . . ? C11 C12 C13 120.2(2) . . ? C8 C13 C12 120.7(2) . . ? N1 C14 C15 108.82(16) . . ? N1 C14 C19 111.97(17) . . ? C15 C14 C19 110.14(15) . . ? C14 C15 C16 111.49(18) . . ? C17 C16 C15 111.96(18) . . ? C16 C17 C18 110.53(16) . . ? C17 C18 C19 111.18(18) . . ? C18 C19 C14 112.04(18) . . ? N2 C20 C21 111.01(16) . . ? N2 C20 C25 109.14(16) . . ? C21 C20 C25 109.87(16) . . ? C20 C21 C22 111.13(18) . . ? C23 C22 C21 110.83(17) . . ? C24 C23 C22 111.75(18) . . ? C23 C24 C25 111.42(18) . . ? C24 C25 C20 111.31(17) . . ? #===END data_mpc-1b(jul1702) _database_code_CSD 205562 _audit_creation_date 2002-07-31T09:26:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [PPh2C(NiPr)(NHiPr)] _chemical_formula_moiety 'C19 H25 N2 P1' _chemical_formula_sum 'C19 H25 N2 P1' _chemical_formula_weight 312.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1) _symmetry_Int_Tables_number 76 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 12.1947(4) _cell_length_b 12.1947(4) _cell_length_c 12.6119(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1875.52(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13005 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.817 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_number 9328 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 23.82 _diffrn_reflns_theta_full 23.82 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 2815 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C5 C6 C7 iPr group is disordered; lower occupancy sites left isotropic. 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 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.4406P] 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 'H on N2 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 2815 _refine_ls_number_parameters 212 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.099 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 0.13(11) _refine_diff_density_max 0.116 _refine_diff_density_min -0.122 _refine_diff_density_rms 0.026 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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 P P 0.56937(5) 0.94491(5) 0.21392(5) 0.0482(2) Uani 1 1 d . . . N1 N 0.48121(16) 1.14856(17) 0.26985(18) 0.0486(5) Uani 1 1 d . . . N2 N 0.36862(19) 1.0017(2) 0.3003(2) 0.0571(6) Uani 1 1 d . . . H2A H 0.367(3) 0.935(3) 0.299(2) 0.063(9) Uiso 1 1 d . . . C1 C 0.4667(2) 1.0456(2) 0.2680(2) 0.0442(6) Uani 1 1 d . A . C2 C 0.5841(2) 1.1948(2) 0.2275(2) 0.0513(6) Uani 1 1 d . . . H2 H 0.6389 1.1343 0.2198 0.062 Uiso 1 1 calc R . . C3 C 0.5623(3) 1.2440(3) 0.1190(3) 0.0935(13) Uani 1 1 d . . . H3C H 0.5075 1.3025 0.1254 0.14 Uiso 1 1 calc R . . H3B H 0.5347 1.187 0.0713 0.14 Uiso 1 1 calc R . . H3A H 0.6305 1.2745 0.0904 0.14 Uiso 1 1 calc R . . C4 C 0.6286(3) 1.2783(3) 0.3040(3) 0.0872(12) Uani 1 1 d . . . H4C H 0.6975 1.3082 0.2764 0.131 Uiso 1 1 calc R . . H4B H 0.6419 1.2434 0.3728 0.131 Uiso 1 1 calc R . . H4A H 0.5753 1.3378 0.3127 0.131 Uiso 1 1 calc R . . C8 C 0.6639(2) 0.9366(2) 0.3268(2) 0.0511(6) Uani 1 1 d . . . C9 C 0.6397(3) 0.9679(3) 0.4291(3) 0.0685(9) Uani 1 1 d . . . H9 H 0.5694 0.9976 0.4445 0.082 Uiso 1 1 calc R . . C10 C 0.7161(3) 0.9571(3) 0.5103(3) 0.0821(10) Uani 1 1 d . . . H10 H 0.6978 0.9797 0.5801 0.098 Uiso 1 1 calc R . . C11 C 0.8177(3) 0.9138(3) 0.4900(3) 0.0775(10) Uani 1 1 d . . . H11 H 0.8694 0.9049 0.5457 0.093 Uiso 1 1 calc R . . C12 C 0.8440(3) 0.8837(3) 0.3891(3) 0.0767(10) Uani 1 1 d . . . H12 H 0.9149 0.8549 0.3747 0.092 Uiso 1 1 calc R . . C13 C 0.7686(2) 0.8946(2) 0.3065(3) 0.0671(8) Uani 1 1 d . . . H13 H 0.7883 0.8734 0.2365 0.08 Uiso 1 1 calc R . . C14 C 0.49447(19) 0.81491(18) 0.2253(2) 0.0436(6) Uani 1 1 d . . . C15 C 0.4347(2) 0.7820(2) 0.1361(2) 0.0486(6) Uani 1 1 d . . . H15 H 0.4352 0.8262 0.0741 0.058 Uiso 1 1 calc R . . C16 C 0.3749(2) 0.6855(2) 0.1375(2) 0.0535(7) Uani 1 1 d . . . H16 H 0.3336 0.6643 0.0769 0.064 Uiso 1 1 calc R . . C17 C 0.3751(2) 0.6208(2) 0.2259(2) 0.0596(7) Uani 1 1 d . . . H17 H 0.3345 0.5543 0.2262 0.072 Uiso 1 1 calc R . . C18 C 0.4337(3) 0.6509(2) 0.3145(2) 0.0632(8) Uani 1 1 d . . . H18 H 0.4329 0.6058 0.376 0.076 Uiso 1 1 calc R . . C19 C 0.4939(2) 0.7478(2) 0.3136(2) 0.0548(7) Uani 1 1 d . . . H19 H 0.5352 0.7681 0.3744 0.066 Uiso 1 1 calc R . . C5 C 0.2799(2) 1.0675(2) 0.3442(3) 0.0607(8) Uani 0.620(5) 1 d P A 1 H5 H 0.2807 1.1382 0.3041 0.073 Uiso 0.620(5) 1 calc PR A 1 C6 C 0.2893(4) 1.0957(4) 0.4517(4) 0.0690(15) Uani 0.620(5) 1 d P A 1 H6A H 0.3606 1.1304 0.4642 0.103 Uiso 0.620(5) 1 calc PR A 1 H6B H 0.2832 1.0294 0.4952 0.103 Uiso 0.620(5) 1 calc PR A 1 H6C H 0.2306 1.1469 0.4707 0.103 Uiso 0.620(5) 1 calc PR A 1 C7 C 0.1658(4) 1.0087(4) 0.3145(4) 0.0636(14) Uani 0.620(5) 1 d P A 1 H7A H 0.1654 0.9902 0.2388 0.095 Uiso 0.620(5) 1 calc PR A 1 H7B H 0.1048 1.0586 0.33 0.095 Uiso 0.620(5) 1 calc PR A 1 H7C H 0.1577 0.9416 0.3565 0.095 Uiso 0.620(5) 1 calc PR A 1 C5A C 0.2799(2) 1.0675(2) 0.3442(3) 0.0607(8) Uani 0.380(5) 1 d P A 2 H5A H 0.3175 1.1287 0.3824 0.073 Uiso 0.380(5) 1 calc PR A 2 C6A C 0.2317(6) 0.9902(6) 0.4367(6) 0.060(2) Uiso 0.380(5) 1 d P A 2 H6A1 H 0.2925 0.9594 0.4779 0.09 Uiso 0.380(5) 1 calc PR A 2 H6A2 H 0.189 0.9305 0.405 0.09 Uiso 0.380(5) 1 calc PR A 2 H6A3 H 0.1844 1.0336 0.4834 0.09 Uiso 0.380(5) 1 calc PR A 2 C7A C 0.2158(6) 1.1153(6) 0.2781(6) 0.057(2) Uiso 0.380(5) 1 d P A 2 H7A1 H 0.2593 1.1588 0.2281 0.086 Uiso 0.380(5) 1 calc PR A 2 H7A2 H 0.1653 1.1635 0.3166 0.086 Uiso 0.380(5) 1 calc PR A 2 H7A3 H 0.1737 1.06 0.239 0.086 Uiso 0.380(5) 1 calc PR A 2 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 P 0.0430(4) 0.0381(4) 0.0634(4) -0.0024(3) 0.0071(3) 0.0000(3) N1 0.0367(11) 0.0366(12) 0.0724(14) 0.0014(10) 0.0036(10) -0.0017(9) N2 0.0475(13) 0.0338(12) 0.0901(18) -0.0038(11) 0.0227(12) -0.0029(10) C1 0.0392(13) 0.0385(14) 0.0550(14) 0.0022(11) 0.0031(11) 0.0001(10) C2 0.0369(13) 0.0396(13) 0.0775(18) 0.0029(13) 0.0056(13) -0.0021(10) C3 0.062(2) 0.103(3) 0.115(3) 0.054(2) -0.005(2) -0.017(2) C4 0.0580(19) 0.080(2) 0.123(3) -0.034(2) 0.0236(19) -0.0300(17) C8 0.0400(14) 0.0350(13) 0.0782(18) -0.0044(12) -0.0010(13) -0.0013(11) C9 0.0526(17) 0.0641(18) 0.089(2) -0.0237(16) -0.0129(15) 0.0116(14) C10 0.077(2) 0.073(2) 0.096(2) -0.0268(18) -0.0329(19) 0.0149(17) C11 0.065(2) 0.0554(18) 0.112(3) -0.0082(18) -0.0328(19) 0.0003(15) C12 0.0443(16) 0.0612(19) 0.125(3) 0.007(2) -0.0114(19) 0.0048(14) C13 0.0455(16) 0.0581(18) 0.098(2) 0.0054(16) 0.0079(16) 0.0058(13) C14 0.0421(13) 0.0337(12) 0.0549(14) -0.0037(12) 0.0020(12) 0.0033(10) C15 0.0462(14) 0.0452(14) 0.0543(15) 0.0013(12) 0.0017(12) 0.0053(11) C16 0.0479(15) 0.0519(16) 0.0607(16) -0.0080(13) -0.0035(13) -0.0018(12) C17 0.0613(17) 0.0486(15) 0.0690(17) -0.0074(15) 0.0075(15) -0.0141(13) C18 0.077(2) 0.0483(16) 0.0639(17) 0.0048(14) 0.0024(15) -0.0132(14) C19 0.0606(17) 0.0449(15) 0.0589(16) -0.0031(12) -0.0060(13) -0.0041(13) C5 0.0517(16) 0.0401(14) 0.090(2) -0.0053(14) 0.0238(15) -0.0036(13) C6 0.064(3) 0.070(3) 0.072(3) 0.001(3) 0.000(3) -0.008(2) C7 0.041(2) 0.063(3) 0.087(3) -0.003(3) 0.008(2) -0.008(2) C5A 0.0517(16) 0.0401(14) 0.090(2) -0.0053(14) 0.0238(15) -0.0036(13) #----------------------------------------------------------------------------# # 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 P C8 1.835(3) . ? P C14 1.835(2) . ? P C1 1.882(3) . ? N1 C1 1.268(3) . ? N1 C2 1.476(3) . ? N2 C1 1.372(3) . ? N2 C5 1.456(4) . ? C2 C4 1.504(4) . ? C2 C3 1.517(5) . ? C8 C9 1.377(4) . ? C8 C13 1.400(4) . ? C9 C10 1.391(5) . ? C10 C11 1.372(5) . ? C11 C12 1.363(5) . ? C12 C13 1.396(5) . ? C14 C19 1.382(4) . ? C14 C15 1.399(4) . ? C15 C16 1.385(4) . ? C16 C17 1.366(4) . ? C17 C18 1.377(4) . ? C18 C19 1.392(4) . ? C5 C6 1.404(6) . ? C5 C7 1.609(5) . ? 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 C8 P C14 101.81(11) . . ? C8 P C1 99.92(12) . . ? C14 P C1 101.80(11) . . ? C1 N1 C2 119.4(2) . . ? C1 N2 C5 123.0(2) . . ? N1 C1 N2 120.2(2) . . ? N1 C1 P 124.07(19) . . ? N2 C1 P 115.63(18) . . ? N1 C2 C4 109.5(2) . . ? N1 C2 C3 109.2(2) . . ? C4 C2 C3 111.9(3) . . ? C9 C8 C13 118.0(3) . . ? C9 C8 P 125.3(2) . . ? C13 C8 P 116.8(2) . . ? C8 C9 C10 121.3(3) . . ? C11 C10 C9 120.3(4) . . ? C12 C11 C10 119.4(3) . . ? C11 C12 C13 121.1(3) . . ? C12 C13 C8 119.9(3) . . ? C19 C14 C15 118.4(2) . . ? C19 C14 P 125.2(2) . . ? C15 C14 P 116.38(19) . . ? C16 C15 C14 120.5(2) . . ? C17 C16 C15 120.0(3) . . ? C16 C17 C18 120.7(3) . . ? C17 C18 C19 119.6(3) . . ? C14 C19 C18 120.8(3) . . ? C6 C5 N2 116.2(3) . . ? C6 C5 C7 113.9(3) . . ? N2 C5 C7 108.0(3) . . ? #===END data_mpc-2a(aug3002) _database_code_CSD 205563 _audit_creation_date 2002-08-20T14:41:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Mo(CO)4{CyNHC(PPh2)NCy] _chemical_formula_moiety 'C29 H33 Mo1 N2 O4 P1' _chemical_formula_sum 'C29 H33 Mo1 N2 O4 P1' _chemical_formula_weight 600.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 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' '-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 32.0166(4) _cell_length_b 9.4980(2) _cell_length_c 21.3176(3) _cell_angle_alpha 90 _cell_angle_beta 118.448(1) _cell_angle_gamma 90 _cell_volume 5699.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8028 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.4 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8344 _exptl_absorpt_correction_T_max 0.9144 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_number 14946 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.912 _diffrn_measured_fraction_theta_max 0.912 _reflns_number_total 4577 _reflns_number_gt 4223 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+7.7314P] 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 'H on N2 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 4577 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.349 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # 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 0.149047(6) 0.851258(15) 0.017567(8) 0.01688(7) Uani 1 1 d . . . P P 0.128062(17) 0.76258(5) 0.10926(3) 0.01773(11) Uani 1 1 d . . . O1 O 0.25841(7) 0.84306(17) 0.13539(10) 0.0435(4) Uani 1 1 d . . . O2 O 0.18313(7) 0.9193(2) -0.09470(9) 0.0530(5) Uani 1 1 d . . . O3 O 0.04789(7) 0.86039(18) -0.11959(10) 0.0505(5) Uani 1 1 d . . . O4 O 0.13786(6) 1.17038(14) 0.03772(9) 0.0366(4) Uani 1 1 d . . . N1 N 0.14449(6) 0.60990(15) 0.02740(8) 0.0191(3) Uani 1 1 d . . . N2 N 0.11749(7) 0.46177(18) 0.09061(9) 0.0275(4) Uani 1 1 d . . . H2 H 0.1183(8) 0.394(3) 0.0701(12) 0.030(6) Uiso 1 1 d . . . C1 C 0.21912(9) 0.84584(19) 0.09442(12) 0.0251(5) Uani 1 1 d . . . C2 C 0.17091(8) 0.8899(2) -0.05367(11) 0.0293(5) Uani 1 1 d . . . C3 C 0.08317(9) 0.8537(2) -0.06754(13) 0.0276(5) Uani 1 1 d . . . C4 C 0.14363(7) 1.0513(2) 0.02926(10) 0.0229(4) Uani 1 1 d . . . C5 C 0.12963(7) 0.58571(18) 0.07367(10) 0.0185(4) Uani 1 1 d . . . C6 C 0.07285(7) 0.78629(19) 0.11320(11) 0.0217(4) Uani 1 1 d . . . C7 C 0.03226(8) 0.8177(2) 0.05026(12) 0.0323(5) Uani 1 1 d . . . H7 H 0.034 0.8269 0.0072 0.039 Uiso 1 1 calc R . . C8 C -0.01106(9) 0.8357(2) 0.04957(14) 0.0404(6) Uani 1 1 d . . . H8 H -0.0389 0.8552 0.006 0.048 Uiso 1 1 calc R . . C9 C -0.01351(9) 0.8252(2) 0.11212(14) 0.0407(6) Uani 1 1 d . . . H9 H -0.0431 0.8372 0.1118 0.049 Uiso 1 1 calc R . . C10 C 0.02679(9) 0.7972(3) 0.17504(14) 0.0424(6) Uani 1 1 d . . . H10 H 0.025 0.7913 0.2182 0.051 Uiso 1 1 calc R . . C11 C 0.07019(8) 0.7774(2) 0.17639(12) 0.0322(5) Uani 1 1 d . . . H11 H 0.0979 0.7578 0.2201 0.039 Uiso 1 1 calc R . . C12 C 0.17492(7) 0.76786(18) 0.20076(10) 0.0187(4) Uani 1 1 d . . . C13 C 0.18208(7) 0.8955(2) 0.23761(11) 0.0252(4) Uani 1 1 d . . . H13 H 0.1603 0.9708 0.2162 0.03 Uiso 1 1 calc R . . C14 C 0.22030(8) 0.9128(2) 0.30451(11) 0.0300(5) Uani 1 1 d . . . H14 H 0.2244 0.999 0.3293 0.036 Uiso 1 1 calc R . . C15 C 0.25271(8) 0.8051(2) 0.33566(11) 0.0306(5) Uani 1 1 d . . . H15 H 0.2792 0.8175 0.3817 0.037 Uiso 1 1 calc R . . C16 C 0.24646(8) 0.6792(2) 0.29967(11) 0.0291(5) Uani 1 1 d . . . H16 H 0.2689 0.6054 0.321 0.035 Uiso 1 1 calc R . . C17 C 0.20779(7) 0.65956(19) 0.23276(11) 0.0233(4) Uani 1 1 d . . . H17 H 0.2037 0.5724 0.2087 0.028 Uiso 1 1 calc R . . C18 C 0.15104(7) 0.49359(18) -0.01273(10) 0.0202(4) Uani 1 1 d . . . H18 H 0.1544 0.4043 0.0141 0.024 Uiso 1 1 calc R . . C19 C 0.10823(8) 0.4790(2) -0.08593(11) 0.0308(5) Uani 1 1 d . . . H19B H 0.1035 0.5675 -0.113 0.037 Uiso 1 1 calc R . . H19A H 0.0795 0.4622 -0.0808 0.037 Uiso 1 1 calc R . . C20 C 0.11504(8) 0.3565(2) -0.12711(12) 0.0365(5) Uani 1 1 d . . . H20B H 0.1157 0.2667 -0.1031 0.044 Uiso 1 1 calc R . . H20A H 0.0878 0.3533 -0.1759 0.044 Uiso 1 1 calc R . . C21 C 0.16098(9) 0.3716(2) -0.13155(12) 0.0335(5) Uani 1 1 d . . . H21B H 0.1657 0.2868 -0.1544 0.04 Uiso 1 1 calc R . . H21A H 0.1585 0.454 -0.1615 0.04 Uiso 1 1 calc R . . C22 C 0.20327(8) 0.3900(2) -0.05812(12) 0.0298(5) Uani 1 1 d . . . H22B H 0.2322 0.4056 -0.0628 0.036 Uiso 1 1 calc R . . H22A H 0.2079 0.303 -0.03 0.036 Uiso 1 1 calc R . . C23 C 0.19614(7) 0.5145(2) -0.01875(11) 0.0267(4) Uani 1 1 d . . . H23B H 0.2238 0.5225 0.0295 0.032 Uiso 1 1 calc R . . H23A H 0.1938 0.6028 -0.045 0.032 Uiso 1 1 calc R . . C24 C 0.10476(7) 0.43402(19) 0.14690(10) 0.0229(4) Uani 1 1 d . . . H24 H 0.1162 0.5147 0.1812 0.027 Uiso 1 1 calc R . . C25 C 0.05127(8) 0.4209(2) 0.11760(12) 0.0327(5) Uani 1 1 d . . . H25B H 0.0388 0.3458 0.081 0.039 Uiso 1 1 calc R . . H25A H 0.0358 0.5105 0.0945 0.039 Uiso 1 1 calc R . . C26 C 0.03921(9) 0.3863(3) 0.17717(15) 0.0455(6) Uani 1 1 d . . . H26B H 0.0497 0.4646 0.212 0.055 Uiso 1 1 calc R . . H26A H 0.0044 0.3763 0.1568 0.055 Uiso 1 1 calc R . . C27 C 0.06334(10) 0.2507(3) 0.21500(15) 0.0478(7) Uani 1 1 d . . . H27B H 0.0559 0.232 0.2543 0.057 Uiso 1 1 calc R . . H27A H 0.051 0.171 0.181 0.057 Uiso 1 1 calc R . . C28 C 0.11658(9) 0.2618(2) 0.24465(12) 0.0387(6) Uani 1 1 d . . . H28B H 0.1314 0.1706 0.2663 0.046 Uiso 1 1 calc R . . H28A H 0.1292 0.334 0.2827 0.046 Uiso 1 1 calc R . . C29 C 0.13009(8) 0.3007(2) 0.18715(12) 0.0301(5) Uani 1 1 d . . . H29B H 0.1218 0.2218 0.1529 0.036 Uiso 1 1 calc R . . H29A H 0.1649 0.3153 0.2096 0.036 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 0.02119(12) 0.01292(9) 0.01831(11) -0.00019(6) 0.01086(9) -0.00140(6) P 0.0215(3) 0.0144(2) 0.0200(3) -0.00070(18) 0.0120(2) 0.00007(18) O1 0.0257(12) 0.0525(11) 0.0446(10) 0.0040(8) 0.0105(10) -0.0005(7) O2 0.0547(12) 0.0809(13) 0.0352(9) -0.0016(9) 0.0309(10) -0.0208(10) O3 0.0377(12) 0.0515(11) 0.0414(11) -0.0034(8) 0.0019(12) 0.0045(8) O4 0.0487(11) 0.0146(7) 0.0461(9) -0.0029(6) 0.0222(9) 0.0000(6) N1 0.0239(9) 0.0148(7) 0.0210(8) -0.0012(6) 0.0126(8) -0.0004(6) N2 0.0466(12) 0.0145(8) 0.0319(10) -0.0051(7) 0.0272(10) -0.0057(8) C1 0.0301(15) 0.0214(10) 0.0287(12) 0.0005(8) 0.0179(13) -0.0013(8) C2 0.0270(13) 0.0318(11) 0.0260(11) -0.0040(9) 0.0101(11) -0.0068(9) C3 0.0299(15) 0.0214(11) 0.0308(13) -0.0022(8) 0.0139(14) -0.0004(8) C4 0.0237(11) 0.0235(11) 0.0193(10) 0.0026(8) 0.0086(10) -0.0029(8) C5 0.0195(11) 0.0161(9) 0.0185(9) -0.0013(7) 0.0080(9) 0.0001(7) C6 0.0232(11) 0.0159(9) 0.0286(11) -0.0008(8) 0.0145(10) 0.0006(7) C7 0.0280(13) 0.0377(12) 0.0325(12) -0.0008(9) 0.0155(12) 0.0026(9) C8 0.0227(13) 0.0472(14) 0.0454(15) -0.0002(11) 0.0114(13) 0.0049(10) C9 0.0330(15) 0.0364(13) 0.0659(18) 0.0065(11) 0.0342(15) 0.0070(10) C10 0.0447(16) 0.0500(15) 0.0500(15) 0.0117(12) 0.0368(15) 0.0114(11) C11 0.0327(13) 0.0366(12) 0.0341(12) 0.0086(9) 0.0215(12) 0.0092(9) C12 0.0215(11) 0.0189(9) 0.0204(10) -0.0014(7) 0.0137(9) -0.0027(7) C13 0.0312(13) 0.0209(10) 0.0273(11) -0.0025(8) 0.0170(11) 0.0002(8) C14 0.0366(14) 0.0300(11) 0.0290(12) -0.0112(9) 0.0200(12) -0.0097(9) C15 0.0256(13) 0.0428(13) 0.0214(11) -0.0045(9) 0.0097(11) -0.0101(10) C16 0.0228(12) 0.0326(11) 0.0300(12) 0.0048(9) 0.0110(11) 0.0014(9) C17 0.0241(12) 0.0200(10) 0.0271(11) -0.0014(8) 0.0132(11) -0.0015(8) C18 0.0266(12) 0.0143(9) 0.0227(10) -0.0007(7) 0.0140(10) 0.0008(7) C19 0.0265(13) 0.0367(12) 0.0285(11) -0.0097(9) 0.0125(11) 0.0032(9) C20 0.0317(14) 0.0437(14) 0.0291(12) -0.0178(10) 0.0105(12) -0.0002(10) C21 0.0443(15) 0.0326(11) 0.0296(12) -0.0039(9) 0.0225(12) 0.0086(10) C22 0.0335(13) 0.0260(10) 0.0390(12) 0.0015(9) 0.0249(12) 0.0074(9) C23 0.0247(12) 0.0260(10) 0.0311(11) -0.0036(8) 0.0148(11) -0.0001(8) C24 0.0297(12) 0.0187(9) 0.0250(10) -0.0019(8) 0.0170(10) -0.0039(8) C25 0.0303(13) 0.0253(11) 0.0407(13) 0.0007(9) 0.0154(12) -0.0044(9) C26 0.0445(16) 0.0382(13) 0.0714(18) 0.0040(12) 0.0419(16) -0.0048(11) C27 0.0630(18) 0.0376(13) 0.0624(17) 0.0090(12) 0.0459(16) -0.0077(12) C28 0.0586(17) 0.0278(12) 0.0348(12) 0.0069(9) 0.0263(13) 0.0004(10) C29 0.0351(13) 0.0238(10) 0.0342(12) 0.0034(9) 0.0187(11) 0.0014(9) #----------------------------------------------------------------------------# # 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 C4 1.9350(19) . ? Mo C2 1.986(2) . ? Mo C3 2.024(3) . ? Mo C1 2.054(3) . ? Mo N1 2.3129(15) . ? Mo P 2.4966(5) . ? P C12 1.8083(19) . ? P C6 1.8232(19) . ? P C5 1.8538(18) . ? O1 C1 1.140(3) . ? O2 C2 1.150(2) . ? O3 C3 1.148(3) . ? O4 C4 1.173(2) . ? N1 C5 1.304(2) . ? N1 C18 1.472(2) . ? N2 C5 1.342(2) . ? N2 C24 1.463(2) . ? C6 C7 1.384(3) . ? C6 C11 1.392(3) . ? C7 C8 1.390(3) . ? C8 C9 1.376(3) . ? C9 C10 1.373(4) . ? C10 C11 1.389(3) . ? C12 C17 1.395(3) . ? C12 C13 1.403(3) . ? C13 C14 1.377(3) . ? C14 C15 1.381(3) . ? C15 C16 1.383(3) . ? C16 C17 1.385(3) . ? C18 C19 1.515(3) . ? C18 C23 1.522(3) . ? C19 C20 1.534(3) . ? C20 C21 1.525(3) . ? C21 C22 1.515(3) . ? C22 C23 1.529(3) . ? C24 C25 1.523(3) . ? C24 C29 1.528(3) . ? C25 C26 1.529(3) . ? C26 C27 1.521(3) . ? C27 C28 1.513(4) . ? C28 C29 1.527(3) . ? 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 C4 Mo C2 90.15(8) . . ? C4 Mo C3 89.14(8) . . ? C2 Mo C3 84.77(8) . . ? C4 Mo C1 93.02(8) . . ? C2 Mo C1 88.03(8) . . ? C3 Mo C1 172.49(8) . . ? C4 Mo N1 161.49(7) . . ? C2 Mo N1 108.25(7) . . ? C3 Mo N1 90.50(7) . . ? C1 Mo N1 89.71(6) . . ? C4 Mo P 99.00(5) . . ? C2 Mo P 170.23(6) . . ? C3 Mo P 98.71(6) . . ? C1 Mo P 88.06(5) . . ? N1 Mo P 62.78(4) . . ? C12 P C6 105.74(9) . . ? C12 P C5 107.24(8) . . ? C6 P C5 110.28(8) . . ? C12 P Mo 116.16(6) . . ? C6 P Mo 128.52(7) . . ? C5 P Mo 85.15(6) . . ? C5 N1 C18 120.78(15) . . ? C5 N1 Mo 107.75(11) . . ? C18 N1 Mo 131.19(11) . . ? C5 N2 C24 127.45(16) . . ? O1 C1 Mo 177.81(17) . . ? O2 C2 Mo 176.58(19) . . ? O3 C3 Mo 173.18(19) . . ? O4 C4 Mo 175.15(16) . . ? N1 C5 N2 127.96(16) . . ? N1 C5 P 103.93(12) . . ? N2 C5 P 128.10(14) . . ? C7 C6 C11 119.28(18) . . ? C7 C6 P 117.71(14) . . ? C11 C6 P 122.99(16) . . ? C6 C7 C8 120.5(2) . . ? C9 C8 C7 119.9(2) . . ? C10 C9 C8 120.0(2) . . ? C9 C10 C11 120.8(2) . . ? C10 C11 C6 119.6(2) . . ? C17 C12 C13 118.64(18) . . ? C17 C12 P 123.49(14) . . ? C13 C12 P 117.28(15) . . ? C14 C13 C12 120.70(19) . . ? C13 C14 C15 120.23(19) . . ? C14 C15 C16 119.8(2) . . ? C15 C16 C17 120.6(2) . . ? C16 C17 C12 120.01(18) . . ? N1 C18 C19 110.98(15) . . ? N1 C18 C23 110.76(15) . . ? C19 C18 C23 110.74(16) . . ? C18 C19 C20 110.70(17) . . ? C21 C20 C19 111.62(18) . . ? C22 C21 C20 111.12(17) . . ? C21 C22 C23 111.28(17) . . ? C18 C23 C22 109.94(16) . . ? N2 C24 C25 112.11(17) . . ? N2 C24 C29 109.21(15) . . ? C25 C24 C29 110.79(16) . . ? C24 C25 C26 110.88(19) . . ? C27 C26 C25 110.92(19) . . ? C28 C27 C26 110.43(19) . . ? C27 C28 C29 112.0(2) . . ? C28 C29 C24 111.96(17) . . ? #===END data_mpc-3a(oct1602) _database_code_CSD 205564 _audit_creation_date 2002-10-19T11:20:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [W(CO)4{PPh2C(Ncy)(NHcy)}] _chemical_formula_moiety 'C29 H33 N2 O4 P1 W1' _chemical_formula_sum 'C29 H33 N2 O4 P1 W1' _chemical_formula_weight 688.39 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 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' '-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 32.0487(3) _cell_length_b 9.4740(1) _cell_length_c 21.3526(3) _cell_angle_alpha 90 _cell_angle_beta 118.084(1) _cell_angle_gamma 90 _cell_volume 5719.92(11) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17518 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3998 _exptl_absorpt_correction_T_max 0.6653 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.031 _diffrn_reflns_number 25963 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 6797 _reflns_number_gt 6127 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+9.5727P] 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 'H on N2 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 6797 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.636 _refine_diff_density_min -1.506 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # 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' 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' W W -0.849 6.8722 '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 W W 0.148956(3) 0.851330(9) 0.019179(5) 0.02158(4) Uani 1 1 d . . . P P 0.12834(2) 0.76216(6) 0.11092(3) 0.02083(12) Uani 1 1 d . . . O1 O 0.04829(9) 0.8578(3) -0.11630(15) 0.0630(8) Uani 1 1 d . . . O2 O 0.25759(8) 0.8438(2) 0.13507(14) 0.0523(6) Uani 1 1 d . . . O3 O 0.18350(9) 0.9158(3) -0.09280(13) 0.0649(7) Uani 1 1 d . . . O4 O 0.13765(8) 1.17185(19) 0.03951(12) 0.0453(5) Uani 1 1 d . . . N1 N 0.14453(7) 0.6108(2) 0.02876(10) 0.0220(4) Uani 1 1 d . . . N2 N 0.11877(8) 0.4602(2) 0.09289(12) 0.0316(5) Uani 1 1 d . . . H2 H 0.1203(11) 0.390(4) 0.0712(18) 0.042(9) Uiso 1 1 d . . . C1 C 0.08332(10) 0.8523(3) -0.06535(16) 0.0336(6) Uani 1 1 d . . . C2 C 0.21862(10) 0.8461(3) 0.09475(15) 0.0299(5) Uani 1 1 d . . . C3 C 0.17113(10) 0.8895(3) -0.05195(16) 0.0363(6) Uani 1 1 d . . . C4 C 0.14334(9) 1.0518(3) 0.03101(13) 0.0284(5) Uani 1 1 d . . . C5 C 0.13013(8) 0.5852(2) 0.07534(12) 0.0219(4) Uani 1 1 d . . . C6 C 0.17503(8) 0.7687(2) 0.20184(12) 0.0224(4) Uani 1 1 d . . . C7 C 0.18188(10) 0.8966(3) 0.23824(14) 0.0319(5) Uani 1 1 d . . . H7 H 0.1604 0.9711 0.2171 0.038 Uiso 1 1 calc R . . C8 C 0.21983(10) 0.9145(3) 0.30468(15) 0.0372(6) Uani 1 1 d . . . H8 H 0.2238 1.0002 0.329 0.045 Uiso 1 1 calc R . . C9 C 0.25204(10) 0.8067(3) 0.33553(15) 0.0384(6) Uani 1 1 d . . . H9 H 0.2779 0.8191 0.3809 0.046 Uiso 1 1 calc R . . C10 C 0.24633(9) 0.6805(3) 0.29994(16) 0.0364(6) Uani 1 1 d . . . H10 H 0.2687 0.6079 0.3208 0.044 Uiso 1 1 calc R . . C11 C 0.20782(9) 0.6606(3) 0.23358(15) 0.0298(5) Uani 1 1 d . . . H11 H 0.2038 0.574 0.2099 0.036 Uiso 1 1 calc R . . C12 C 0.07339(8) 0.7871(2) 0.11513(14) 0.0266(5) Uani 1 1 d . . . C13 C 0.03289(10) 0.8172(3) 0.05240(17) 0.0405(6) Uani 1 1 d . . . H13 H 0.0346 0.8253 0.0098 0.049 Uiso 1 1 calc R . . C14 C -0.01016(11) 0.8355(4) 0.0522(2) 0.0524(9) Uani 1 1 d . . . H14 H -0.0376 0.8541 0.0094 0.063 Uiso 1 1 calc R . . C15 C -0.01260(12) 0.8263(3) 0.1144(2) 0.0532(9) Uani 1 1 d . . . H15 H -0.0417 0.8388 0.1143 0.064 Uiso 1 1 calc R . . C16 C 0.02746(12) 0.7989(4) 0.1771(2) 0.0541(9) Uani 1 1 d . . . H16 H 0.0257 0.7937 0.2197 0.065 Uiso 1 1 calc R . . C17 C 0.07046(10) 0.7788(3) 0.17760(16) 0.0392(6) Uani 1 1 d . . . H17 H 0.0977 0.7594 0.2205 0.047 Uiso 1 1 calc R . . C18 C 0.15127(8) 0.4949(2) -0.01166(13) 0.0239(5) Uani 1 1 d . . . H18 H 0.1545 0.406 0.0146 0.029 Uiso 1 1 calc R . . C19 C 0.19605(9) 0.5154(3) -0.01784(15) 0.0324(6) Uani 1 1 d . . . H19A H 0.2232 0.5233 0.0296 0.039 Uiso 1 1 calc R . . H19B H 0.1938 0.603 -0.0437 0.039 Uiso 1 1 calc R . . C20 C 0.20323(10) 0.3903(3) -0.05722(16) 0.0364(6) Uani 1 1 d . . . H20A H 0.2318 0.4056 -0.062 0.044 Uiso 1 1 calc R . . H20B H 0.2077 0.3039 -0.0295 0.044 Uiso 1 1 calc R . . C21 C 0.16106(12) 0.3722(3) -0.13046(17) 0.0416(7) Uani 1 1 d . . . H21A H 0.1656 0.2878 -0.1531 0.05 Uiso 1 1 calc R . . H21B H 0.1588 0.4539 -0.16 0.05 Uiso 1 1 calc R . . C22 C 0.11539(11) 0.3579(3) -0.12521(18) 0.0460(8) Uani 1 1 d . . . H22A H 0.1161 0.2691 -0.1012 0.055 Uiso 1 1 calc R . . H22B H 0.0885 0.3543 -0.1731 0.055 Uiso 1 1 calc R . . C23 C 0.10849(9) 0.4807(3) -0.08442(15) 0.0378(6) Uani 1 1 d . . . H23A H 0.104 0.5685 -0.1111 0.045 Uiso 1 1 calc R . . H23B H 0.0801 0.4643 -0.0791 0.045 Uiso 1 1 calc R . . C24 C 0.10541(9) 0.4329(2) 0.14852(13) 0.0273(5) Uani 1 1 d . . . H24 H 0.1163 0.5134 0.182 0.033 Uiso 1 1 calc R . . C25 C 0.05203(10) 0.4180(3) 0.11898(17) 0.0404(7) Uani 1 1 d . . . H25A H 0.0365 0.5059 0.0953 0.049 Uiso 1 1 calc R . . H25B H 0.0404 0.3421 0.0837 0.049 Uiso 1 1 calc R . . C26 C 0.03939(13) 0.3853(4) 0.1777(2) 0.0556(9) Uani 1 1 d . . . H26A H 0.005 0.3746 0.1573 0.067 Uiso 1 1 calc R . . H26B H 0.0492 0.464 0.2114 0.067 Uiso 1 1 calc R . . C27 C 0.06358(14) 0.2506(4) 0.2166(2) 0.0606(10) Uani 1 1 d . . . H27A H 0.056 0.2336 0.2555 0.073 Uiso 1 1 calc R . . H27B H 0.0517 0.1704 0.1839 0.073 Uiso 1 1 calc R . . C28 C 0.11664(13) 0.2617(3) 0.24624(18) 0.0489(8) Uani 1 1 d . . . H28A H 0.1312 0.1714 0.2679 0.059 Uiso 1 1 calc R . . H28B H 0.1288 0.334 0.2835 0.059 Uiso 1 1 calc R . . C29 C 0.13056(11) 0.2996(3) 0.18919(16) 0.0371(6) Uani 1 1 d . . . H29A H 0.1226 0.2207 0.1558 0.045 Uiso 1 1 calc R . . H29B H 0.1648 0.3141 0.2114 0.045 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 W 0.02731(6) 0.01688(6) 0.02286(6) -0.00028(3) 0.01372(4) -0.00169(3) P 0.0249(3) 0.0172(3) 0.0234(3) -0.0006(2) 0.0138(2) 0.0007(2) O1 0.0448(14) 0.0650(17) 0.0482(16) -0.0047(11) -0.0037(12) 0.0064(11) O2 0.0322(11) 0.0643(16) 0.0522(15) 0.0054(11) 0.0132(11) -0.0022(9) O3 0.0697(16) 0.095(2) 0.0460(14) -0.0025(13) 0.0404(13) -0.0241(15) O4 0.0617(14) 0.0193(10) 0.0543(14) -0.0024(8) 0.0269(12) 0.0004(8) N1 0.0278(10) 0.0167(9) 0.0248(10) -0.0013(7) 0.0150(9) -0.0014(7) N2 0.0528(14) 0.0183(10) 0.0360(13) -0.0040(9) 0.0311(11) -0.0063(9) C1 0.0364(14) 0.0261(13) 0.0353(16) -0.0018(10) 0.0146(13) 0.0014(10) C2 0.0311(13) 0.0278(13) 0.0354(15) 0.0009(10) 0.0194(12) -0.0013(10) C3 0.0408(15) 0.0381(14) 0.0366(16) -0.0014(12) 0.0238(13) -0.0084(12) C4 0.0340(13) 0.0240(12) 0.0276(13) -0.0008(10) 0.0148(11) -0.0044(10) C5 0.0259(11) 0.0158(10) 0.0248(12) -0.0008(8) 0.0126(9) -0.0003(8) C6 0.0264(11) 0.0221(11) 0.0226(12) -0.0018(9) 0.0149(9) -0.0020(9) C7 0.0394(14) 0.0262(12) 0.0331(14) -0.0050(10) 0.0195(12) 0.0001(10) C8 0.0449(16) 0.0373(15) 0.0337(15) -0.0142(11) 0.0222(13) -0.0108(12) C9 0.0320(14) 0.0544(17) 0.0259(14) -0.0036(12) 0.0112(11) -0.0103(12) C10 0.0276(13) 0.0398(15) 0.0378(16) 0.0047(12) 0.0120(12) 0.0027(11) C11 0.0307(13) 0.0239(12) 0.0355(15) -0.0004(10) 0.0162(11) 0.0007(9) C12 0.0283(12) 0.0190(11) 0.0378(14) -0.0002(9) 0.0201(11) 0.0022(9) C13 0.0315(14) 0.0522(17) 0.0376(16) -0.0013(13) 0.0162(13) 0.0041(12) C14 0.0278(15) 0.063(2) 0.061(2) 0.0007(16) 0.0166(15) 0.0051(13) C15 0.0417(17) 0.0482(19) 0.086(3) 0.0088(17) 0.0435(19) 0.0096(14) C16 0.0535(19) 0.065(2) 0.066(2) 0.0176(18) 0.0462(19) 0.0169(17) C17 0.0395(15) 0.0450(17) 0.0439(17) 0.0101(13) 0.0286(13) 0.0101(12) C18 0.0312(12) 0.0176(10) 0.0283(12) 0.0002(9) 0.0184(10) 0.0018(9) C19 0.0302(13) 0.0297(13) 0.0411(16) -0.0049(11) 0.0199(12) 0.0005(10) C20 0.0389(15) 0.0360(14) 0.0442(17) -0.0009(12) 0.0276(13) 0.0088(12) C21 0.0567(19) 0.0404(16) 0.0377(17) -0.0054(12) 0.0305(15) 0.0097(13) C22 0.0413(16) 0.0535(19) 0.0405(18) -0.0229(13) 0.0169(14) 0.0005(13) C23 0.0304(13) 0.0455(16) 0.0342(15) -0.0128(12) 0.0125(11) 0.0040(11) C24 0.0368(13) 0.0203(11) 0.0308(13) -0.0015(9) 0.0209(11) -0.0043(10) C25 0.0364(15) 0.0329(15) 0.0517(19) 0.0007(12) 0.0204(13) -0.0067(11) C26 0.054(2) 0.0478(19) 0.087(3) 0.0054(18) 0.051(2) -0.0065(15) C27 0.078(2) 0.0456(19) 0.083(3) 0.0111(18) 0.058(2) -0.0110(17) C28 0.075(2) 0.0344(16) 0.0439(18) 0.0074(13) 0.0339(16) -0.0019(14) C29 0.0453(16) 0.0291(13) 0.0415(16) 0.0042(12) 0.0241(13) 0.0011(12) #----------------------------------------------------------------------------# # 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 W C4 1.936(3) . ? W C3 1.990(3) . ? W C1 2.027(3) . ? W C2 2.049(3) . ? W N1 2.299(2) . ? W P 2.4913(6) . ? P C6 1.810(2) . ? P C12 1.821(2) . ? P C5 1.853(2) . ? O1 C1 1.139(4) . ? O2 C2 1.135(3) . ? O3 C3 1.143(3) . ? O4 C4 1.179(3) . ? N1 C5 1.301(3) . ? N1 C18 1.474(3) . ? N2 C5 1.343(3) . ? N2 C24 1.463(3) . ? C6 C11 1.393(3) . ? C6 C7 1.400(3) . ? C7 C8 1.377(4) . ? C8 C9 1.379(4) . ? C9 C10 1.382(4) . ? C10 C11 1.386(4) . ? C12 C17 1.383(4) . ? C12 C13 1.387(4) . ? C13 C14 1.388(4) . ? C14 C15 1.370(5) . ? C15 C16 1.374(5) . ? C16 C17 1.386(4) . ? C18 C19 1.514(3) . ? C18 C23 1.519(3) . ? C19 C20 1.532(4) . ? C20 C21 1.520(4) . ? C21 C22 1.526(4) . ? C22 C23 1.531(4) . ? C24 C25 1.526(4) . ? C24 C29 1.530(4) . ? C25 C26 1.521(5) . ? C26 C27 1.521(5) . ? C27 C28 1.513(5) . ? C28 C29 1.524(4) . ? 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 C4 W C3 90.57(11) . . ? C4 W C1 89.46(10) . . ? C3 W C1 85.03(12) . . ? C4 W C2 93.14(10) . . ? C3 W C2 87.55(11) . . ? C1 W C2 172.16(11) . . ? C4 W N1 161.42(9) . . ? C3 W N1 107.89(10) . . ? C1 W N1 90.11(8) . . ? C2 W N1 89.77(8) . . ? C4 W P 98.90(8) . . ? C3 W P 169.77(9) . . ? C1 W P 98.82(9) . . ? C2 W P 88.09(8) . . ? N1 W P 62.84(5) . . ? C6 P C12 105.85(11) . . ? C6 P C5 107.52(10) . . ? C12 P C5 110.80(10) . . ? C6 P W 116.13(7) . . ? C12 P W 128.00(8) . . ? C5 P W 85.04(7) . . ? C5 N1 C18 120.75(19) . . ? C5 N1 W 108.17(15) . . ? C18 N1 W 130.86(15) . . ? C5 N2 C24 127.1(2) . . ? O1 C1 W 173.8(3) . . ? O2 C2 W 178.0(3) . . ? O3 C3 W 177.8(3) . . ? O4 C4 W 175.6(2) . . ? N1 C5 N2 128.2(2) . . ? N1 C5 P 103.61(16) . . ? N2 C5 P 128.22(18) . . ? C11 C6 C7 118.8(2) . . ? C11 C6 P 123.36(18) . . ? C7 C6 P 117.33(18) . . ? C8 C7 C6 120.6(3) . . ? C7 C8 C9 120.1(3) . . ? C8 C9 C10 120.1(3) . . ? C9 C10 C11 120.3(3) . . ? C10 C11 C6 120.1(2) . . ? C17 C12 C13 119.1(2) . . ? C17 C12 P 123.1(2) . . ? C13 C12 P 117.8(2) . . ? C12 C13 C14 120.4(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 120.2(3) . . ? C15 C16 C17 120.2(3) . . ? C12 C17 C16 120.2(3) . . ? N1 C18 C19 111.20(19) . . ? N1 C18 C23 110.76(19) . . ? C19 C18 C23 111.0(2) . . ? C18 C19 C20 110.0(2) . . ? C21 C20 C19 111.2(2) . . ? C20 C21 C22 110.7(2) . . ? C21 C22 C23 112.0(2) . . ? C18 C23 C22 110.3(2) . . ? N2 C24 C25 112.4(2) . . ? N2 C24 C29 109.2(2) . . ? C25 C24 C29 110.3(2) . . ? C26 C25 C24 111.1(3) . . ? C25 C26 C27 110.9(3) . . ? C28 C27 C26 110.7(3) . . ? C27 C28 C29 112.1(3) . . ? C28 C29 C24 111.9(2) . . ? #===END data_oct702 _database_code_CSD 205565 _audit_creation_date 2002-10-03T16:43:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common ; '[Mo(CO)4(NC5H10)2]' ; _chemical_formula_moiety 'C14 H20 Mo1 N2 O4' _chemical_formula_sum 'C14 H20 Mo1 N2 O4' _chemical_formula_weight 376.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 _symmetry_Int_Tables_number 96 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' '-y, -x, -z+1/2' _cell_length_a 12.0134(3) _cell_length_b 12.0134(3) _cell_length_c 11.2821(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1628.25(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9124 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8966 _exptl_absorpt_correction_T_max 0.9502 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_unetI/netI 0.029 _diffrn_reflns_number 9080 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 28.68 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _reflns_number_total 2002 _reflns_number_gt 1883 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.5934P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 2002 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.058 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _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 0.00(5) _refine_diff_density_max 0.426 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # 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' 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 0.714620(15) 0.714620(15) 1 0.02414(8) Uani 1 2 d S . . O1 O 0.63644(18) 0.53336(14) 0.82137(16) 0.0432(5) Uani 1 1 d . . . O2 O 0.52393(17) 0.8624(2) 0.8853(2) 0.0556(6) Uani 1 1 d . . . N N 0.85560(16) 0.77559(16) 0.87173(16) 0.0269(4) Uani 1 1 d . . . C1 C 0.6661(2) 0.6010(2) 0.8887(2) 0.0306(5) Uani 1 1 d . . . C2 C 0.5968(2) 0.8145(2) 0.9258(2) 0.0327(5) Uani 1 1 d . . . C3 C 0.9455(2) 0.6926(2) 0.8522(2) 0.0376(6) Uani 1 1 d . . . H3A H 0.9131 0.6251 0.8179 0.045 Uiso 1 1 calc R . . H3B H 0.9782 0.6726 0.9289 0.045 Uiso 1 1 calc R . . C4 C 1.0373(2) 0.7348(3) 0.7706(3) 0.0474(7) Uani 1 1 d . . . H4A H 1.0758 0.7971 0.8088 0.057 Uiso 1 1 calc R . . H4B H 1.0917 0.6753 0.7576 0.057 Uiso 1 1 calc R . . C5 C 0.9917(2) 0.7727(3) 0.6525(2) 0.0478(7) Uani 1 1 d . . . H5A H 0.9616 0.7087 0.6091 0.057 Uiso 1 1 calc R . . H5B H 1.0514 0.8057 0.605 0.057 Uiso 1 1 calc R . . C6 C 0.9006(3) 0.8578(3) 0.6730(3) 0.0512(8) Uani 1 1 d . . . H6A H 0.8668 0.8778 0.5969 0.061 Uiso 1 1 calc R . . H6B H 0.933 0.9253 0.7075 0.061 Uiso 1 1 calc R . . C7 C 0.8115(2) 0.8129(2) 0.7554(2) 0.0431(6) Uani 1 1 d . . . H7A H 0.7557 0.871 0.7688 0.052 Uiso 1 1 calc R . . H7B H 0.7742 0.75 0.7168 0.052 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 0.02561(9) 0.02561(9) 0.02120(13) -0.00006(8) 0.00006(8) -0.00250(10) O1 0.0582(12) 0.0367(10) 0.0347(10) -0.0093(8) -0.0017(9) -0.0098(9) O2 0.0448(11) 0.0667(14) 0.0552(13) 0.0088(12) -0.0118(10) 0.0106(11) N 0.0315(9) 0.0278(9) 0.0213(8) 0.0012(8) 0.0032(8) 0.0000(8) C1 0.0335(12) 0.0316(12) 0.0268(12) 0.0015(10) 0.0030(10) -0.0010(9) C2 0.0330(12) 0.0367(13) 0.0285(12) 0.0002(10) -0.0018(10) -0.0020(10) C3 0.0346(12) 0.0397(15) 0.0386(14) 0.0052(11) 0.0073(11) 0.0058(11) C4 0.0359(13) 0.0580(18) 0.0483(17) 0.0003(14) 0.0110(12) -0.0024(12) C5 0.0498(15) 0.0610(18) 0.0325(14) -0.0094(14) 0.0155(12) -0.0131(15) C6 0.0604(18) 0.0623(18) 0.0308(14) 0.0145(13) 0.0109(13) 0.0041(17) C7 0.0434(14) 0.0595(16) 0.0263(11) 0.0123(13) 0.0010(12) 0.0081(11) #----------------------------------------------------------------------------# # 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 C1 1.945(3) . ? Mo C1 1.945(3) 5_557 ? Mo C2 2.035(2) . ? Mo C2 2.035(2) 5_557 ? Mo N 2.3451(19) 5_557 ? Mo N 2.3451(19) . ? O1 C1 1.168(3) . ? O2 C2 1.143(3) . ? N C7 1.484(3) . ? N C3 1.486(3) . ? C3 C4 1.523(4) . ? C4 C5 1.510(4) . ? C5 C6 1.515(4) . ? C6 C7 1.517(4) . ? 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 C1 Mo C1 89.76(14) . 5_557 ? C1 Mo C2 86.55(10) . . ? C1 Mo C2 87.38(10) 5_557 . ? C1 Mo C2 87.38(10) . 5_557 ? C1 Mo C2 86.55(10) 5_557 5_557 ? C2 Mo C2 171.42(14) . 5_557 ? C1 Mo N 177.87(9) . 5_557 ? C1 Mo N 92.14(8) 5_557 5_557 ? C2 Mo N 92.59(8) . 5_557 ? C2 Mo N 93.69(8) 5_557 5_557 ? C1 Mo N 92.14(8) . . ? C1 Mo N 177.87(9) 5_557 . ? C2 Mo N 93.69(8) . . ? C2 Mo N 92.59(8) 5_557 . ? N Mo N 85.97(10) 5_557 . ? C7 N C3 109.3(2) . . ? C7 N Mo 112.46(14) . . ? C3 N Mo 114.02(14) . . ? O1 C1 Mo 179.5(2) . . ? O2 C2 Mo 173.6(2) . . ? N C3 C4 113.1(2) . . ? C5 C4 C3 111.8(2) . . ? C4 C5 C6 109.3(2) . . ? C5 C6 C7 111.3(2) . . ? N C7 C6 113.4(2) . . ? #===END