# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Andrews, C. D.' 'Burrows, A. D.' 'Lynam, J. M.' 'Mahon, M.' 'Palmer, M. T.' _publ_contact_author_name 'Dr A D Burrows' _publ_contact_author_address ; Dr A D Burrows School of Chemistry University of Bath Claverton Down BA2 7AY BATH ; _publ_contact_author_email 'A.D.BURROWS@BATH.AC.UK' data_L(00ab1) _database_code_CSD 161741 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 N O P' _chemical_formula_weight 293.29 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' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _cell_length_a 9.501(3) _cell_length_b 16.156(3) _cell_length_c 11.009(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.91(2) _cell_angle_gamma 90.00 _cell_volume 1556.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3326 _diffrn_reflns_av_R_equivalents 0.0085 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.96 _reflns_number_total 3036 _reflns_number_gt 2173 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0596P)^2^+0.1711P] 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 SHELXL _refine_ls_extinction_coef 0.0015(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3036 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.14522(5) 0.01228(3) 0.85452(4) 0.04407(15) Uani 1 1 d . . . N1 N 0.01554(15) 0.08779(8) 0.75842(14) 0.0469(3) Uani 1 1 d . . . O1 O 0.27174(18) 0.16795(9) 0.94411(15) 0.0749(4) Uani 1 1 d . . . C1 C 0.03586(17) -0.08056(10) 0.77915(15) 0.0428(4) Uani 1 1 d . . . C2 C -0.0615(2) -0.11137(12) 0.83571(19) 0.0580(5) Uani 1 1 d . . . H2 H -0.0705 -0.0835 0.9062 0.070 Uiso 1 1 calc R . . C3 C -0.1443(3) -0.18239(14) 0.7887(2) 0.0717(6) Uani 1 1 d . . . H3 H -0.2111 -0.2014 0.8258 0.086 Uiso 1 1 calc R . . C4 C -0.1286(3) -0.22523(13) 0.6875(2) 0.0709(6) Uani 1 1 d . . . H4 H -0.1823 -0.2742 0.6577 0.085 Uiso 1 1 calc R . . C5 C -0.0331(2) -0.19582(12) 0.6297(2) 0.0649(5) Uani 1 1 d . . . H5 H -0.0235 -0.2245 0.5601 0.078 Uiso 1 1 calc R . . C6 C 0.0480(2) -0.12380(11) 0.67529(18) 0.0534(4) Uani 1 1 d . . . H6 H 0.1117 -0.1040 0.6357 0.064 Uiso 1 1 calc R . . C7 C 0.28456(18) 0.01277(10) 0.77874(16) 0.0433(4) Uani 1 1 d . . . C8 C 0.4131(2) -0.03611(13) 0.8375(2) 0.0600(5) Uani 1 1 d . . . H8 H 0.4247 -0.0666 0.9125 0.072 Uiso 1 1 calc R . . C9 C 0.5236(2) -0.04002(16) 0.7863(2) 0.0753(6) Uani 1 1 d . . . H9 H 0.6088 -0.0736 0.8257 0.090 Uiso 1 1 calc R . . C10 C 0.5081(3) 0.00568(16) 0.6772(3) 0.0789(7) Uani 1 1 d . . . H10 H 0.5833 0.0033 0.6428 0.095 Uiso 1 1 calc R . . C11 C 0.3822(3) 0.05498(13) 0.6182(2) 0.0673(5) Uani 1 1 d . . . H11 H 0.3723 0.0860 0.5442 0.081 Uiso 1 1 calc R . . C12 C 0.2700(2) 0.05858(11) 0.66849(17) 0.0533(4) Uani 1 1 d . . . H12 H 0.1846 0.0919 0.6281 0.064 Uiso 1 1 calc R . . C13 C -0.1199(2) 0.07386(13) 0.65493(18) 0.0567(5) Uani 1 1 d . . . H13 H -0.1550 0.0224 0.6176 0.068 Uiso 1 1 calc R . . C14 C -0.1956(3) 0.14654(14) 0.6147(2) 0.0711(6) Uani 1 1 d . . . H14 H -0.2904 0.1537 0.5461 0.085 Uiso 1 1 calc R . . C15 C -0.1054(3) 0.20776(13) 0.6951(2) 0.0722(6) Uani 1 1 d . . . H15 H -0.1293 0.2638 0.6899 0.087 Uiso 1 1 calc R . . C16 C 0.0257(2) 0.17217(11) 0.78404(18) 0.0539(4) Uani 1 1 d . . . C17 C 0.1590(3) 0.20911(12) 0.8833(2) 0.0631(5) Uani 1 1 d . . . C18 C 0.1548(3) 0.30023(13) 0.9095(3) 0.0958(8) Uani 1 1 d . . . H18A H 0.2495 0.3165 0.9783 0.144 Uiso 1 1 calc R . . H18B H 0.0720 0.3117 0.9364 0.144 Uiso 1 1 calc R . . H18C H 0.1403 0.3307 0.8307 0.144 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 P1 0.0479(3) 0.0420(2) 0.0451(2) -0.00136(18) 0.02124(19) 0.00222(18) N1 0.0470(8) 0.0414(7) 0.0559(8) -0.0010(6) 0.0240(7) 0.0048(6) O1 0.0758(10) 0.0597(9) 0.0824(10) -0.0138(7) 0.0233(8) -0.0062(8) C1 0.0424(9) 0.0401(8) 0.0485(9) 0.0041(7) 0.0207(7) 0.0048(7) C2 0.0674(12) 0.0582(11) 0.0612(11) -0.0033(9) 0.0390(10) -0.0063(9) C3 0.0798(15) 0.0697(13) 0.0833(14) -0.0029(11) 0.0510(12) -0.0218(11) C4 0.0754(14) 0.0539(12) 0.0898(15) -0.0125(10) 0.0393(12) -0.0206(10) C5 0.0711(13) 0.0572(12) 0.0774(13) -0.0200(10) 0.0408(11) -0.0105(10) C6 0.0558(10) 0.0506(10) 0.0648(11) -0.0079(8) 0.0356(9) -0.0056(8) C7 0.0403(8) 0.0391(8) 0.0510(9) -0.0057(7) 0.0184(7) -0.0045(7) C8 0.0510(11) 0.0608(11) 0.0674(12) 0.0006(9) 0.0222(9) 0.0063(9) C9 0.0455(11) 0.0874(16) 0.0929(17) -0.0123(13) 0.0268(11) 0.0085(10) C10 0.0608(13) 0.0942(18) 0.0996(18) -0.0290(14) 0.0508(13) -0.0175(12) C11 0.0782(14) 0.0693(13) 0.0685(12) -0.0079(10) 0.0440(11) -0.0169(11) C12 0.0563(11) 0.0513(10) 0.0563(10) -0.0022(8) 0.0261(9) -0.0024(8) C13 0.0489(10) 0.0571(11) 0.0626(11) 0.0030(8) 0.0199(9) 0.0015(8) C14 0.0571(12) 0.0693(14) 0.0826(14) 0.0220(11) 0.0224(11) 0.0146(10) C15 0.0805(14) 0.0478(11) 0.0976(16) 0.0151(11) 0.0448(13) 0.0188(11) C16 0.0657(12) 0.0403(9) 0.0666(11) 0.0003(8) 0.0376(10) 0.0061(8) C17 0.0819(15) 0.0467(10) 0.0721(13) -0.0065(9) 0.0424(12) -0.0019(10) C18 0.131(2) 0.0481(13) 0.1079(19) -0.0182(13) 0.0467(17) -0.0079(13) _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 P1 N1 1.7637(14) . ? P1 C7 1.8190(18) . ? P1 C1 1.8293(17) . ? N1 C13 1.365(2) . ? N1 C16 1.388(2) . ? O1 C17 1.216(2) . ? C1 C6 1.382(2) . ? C1 C2 1.393(2) . ? C2 C3 1.373(3) . ? C3 C4 1.369(3) . ? C4 C5 1.380(3) . ? C5 C6 1.378(3) . ? C7 C12 1.382(2) . ? C7 C8 1.385(2) . ? C8 C9 1.373(3) . ? C9 C10 1.369(4) . ? C10 C11 1.372(3) . ? C11 C12 1.379(3) . ? C13 C14 1.358(3) . ? C14 C15 1.380(3) . ? C15 C16 1.375(3) . ? C16 C17 1.441(3) . ? C17 C18 1.504(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 N1 P1 C7 100.66(7) . . ? N1 P1 C1 98.87(7) . . ? C7 P1 C1 100.48(7) . . ? C13 N1 C16 107.45(15) . . ? C13 N1 P1 126.74(12) . . ? C16 N1 P1 125.48(12) . . ? C6 C1 C2 118.21(16) . . ? C6 C1 P1 125.03(13) . . ? C2 C1 P1 116.69(13) . . ? C3 C2 C1 120.88(17) . . ? C4 C3 C2 120.07(18) . . ? C3 C4 C5 120.09(19) . . ? C6 C5 C4 119.83(19) . . ? C5 C6 C1 120.90(17) . . ? C12 C7 C8 118.96(17) . . ? C12 C7 P1 124.31(13) . . ? C8 C7 P1 116.74(14) . . ? C9 C8 C7 120.7(2) . . ? C10 C9 C8 119.8(2) . . ? C9 C10 C11 120.3(2) . . ? C10 C11 C12 120.2(2) . . ? C11 C12 C7 120.07(18) . . ? C14 C13 N1 109.71(19) . . ? C13 C14 C15 107.01(19) . . ? C16 C15 C14 108.74(18) . . ? C15 C16 N1 107.09(17) . . ? C15 C16 C17 130.68(19) . . ? N1 C16 C17 122.14(17) . . ? O1 C17 C16 121.11(18) . . ? O1 C17 C18 120.8(2) . . ? C16 C17 C18 118.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.234 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.033 #===end data_1(00ab2) _database_code_CSD 161742 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.50 H22 Cl2 Mo N O3 P' _chemical_formula_weight 588.25 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.762(3) _cell_length_b 10.383(4) _cell_length_c 14.411(5) _cell_angle_alpha 110.50(3) _cell_angle_beta 93.69(3) _cell_angle_gamma 100.85(3) _cell_volume 1330.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Irregular _exptl_crystal_colour Dark Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4-circle diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5137 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4686 _reflns_number_gt 3577 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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 'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0025(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4686 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.20123(5) 0.85402(5) 0.31499(3) 0.01731(16) Uani 1 1 d . . . Cl1 Cl 0.01147(13) 0.82130(13) 0.17842(9) 0.0242(3) Uani 1 1 d . . . P1 P 0.33500(13) 0.90597(13) 0.18378(9) 0.0173(3) Uani 1 1 d . . . O1 O 0.0566(4) 1.0944(4) 0.4274(3) 0.0330(9) Uani 1 1 d . . . O2 O 0.4478(4) 1.1006(4) 0.4455(3) 0.0341(9) Uani 1 1 d . . . O3 O 0.5096(4) 0.7452(4) 0.2457(3) 0.0253(8) Uani 1 1 d . . . N1 N 0.5099(4) 1.0018(4) 0.2164(3) 0.0195(9) Uani 1 1 d . . . C1 C 0.0671(3) 0.6993(4) 0.3761(3) 0.0289(13) Uani 1 1 d G . . H1 H -0.0203 0.7145 0.3979 0.035 Uiso 1 1 calc R . . C2 C 0.2019(4) 0.7586(4) 0.43499(19) 0.0254(12) Uani 1 1 d G . . H2 H 0.2205 0.8205 0.5032 0.030 Uiso 1 1 calc R . . C3 C 0.3040(3) 0.7093(4) 0.3741(2) 0.0218(11) Uani 1 1 d G . . H3 H 0.4029 0.7323 0.3944 0.026 Uiso 1 1 calc R . . C4 C 0.2323(4) 0.6194(4) 0.2775(2) 0.0245(12) Uani 1 1 d G . . H4 H 0.2748 0.5718 0.2219 0.029 Uiso 1 1 calc R . . C5 C 0.0859(3) 0.6133(4) 0.2787(2) 0.0275(12) Uani 1 1 d G . . H5 H 0.0133 0.5608 0.2240 0.033 Uiso 1 1 calc R . . C6 C 0.1106(5) 1.0073(6) 0.3845(4) 0.0221(11) Uani 1 1 d . . . C7 C 0.3595(6) 1.0095(6) 0.3968(4) 0.0242(12) Uani 1 1 d . . . C8 C 0.5617(6) 1.1255(6) 0.2015(4) 0.0280(12) Uani 1 1 d . . . H8 H 0.5073 1.1722 0.1725 0.034 Uiso 1 1 calc R . . C9 C 0.7018(6) 1.1701(6) 0.2346(4) 0.0324(13) Uani 1 1 d . . . H9 H 0.7619 1.2520 0.2324 0.039 Uiso 1 1 calc R . . C10 C 0.7421(6) 1.0742(6) 0.2726(4) 0.0269(12) Uani 1 1 d . . . H10 H 0.8343 1.0800 0.3016 0.032 Uiso 1 1 calc R . . C11 C 0.6256(5) 0.9707(6) 0.2607(4) 0.0231(11) Uani 1 1 d . . . C12 C 0.6151(5) 0.8407(6) 0.2792(4) 0.0215(11) Uani 1 1 d . . . C13 C 0.7376(6) 0.8257(6) 0.3392(4) 0.0292(13) Uani 1 1 d . . . H13A H 0.7069 0.7497 0.3638 0.044 Uiso 1 1 calc R . . H13B H 0.7751 0.9145 0.3961 0.044 Uiso 1 1 calc R . . H13C H 0.8112 0.8031 0.2970 0.044 Uiso 1 1 calc R . . C14 C 0.3483(6) 0.7594(5) 0.0714(4) 0.0205(11) Uani 1 1 d . . . C15 C 0.2379(6) 0.6387(6) 0.0357(4) 0.0259(12) Uani 1 1 d . . . H15 H 0.1571 0.6352 0.0690 0.031 Uiso 1 1 calc R . . C16 C 0.2467(7) 0.5251(6) -0.0476(4) 0.0334(14) Uani 1 1 d . . . H16 H 0.1716 0.4436 -0.0719 0.040 Uiso 1 1 calc R . . C17 C 0.3652(7) 0.5293(6) -0.0962(4) 0.0372(15) Uani 1 1 d . . . H17 H 0.3712 0.4509 -0.1536 0.045 Uiso 1 1 calc R . . C18 C 0.4744(6) 0.6488(6) -0.0603(4) 0.0306(13) Uani 1 1 d . . . H18 H 0.5555 0.6522 -0.0932 0.037 Uiso 1 1 calc R . . C19 C 0.4656(6) 0.7624(6) 0.0228(4) 0.0247(11) Uani 1 1 d . . . H19 H 0.5410 0.8437 0.0470 0.030 Uiso 1 1 calc R . . C20 C 0.2598(5) 1.0228(5) 0.1367(4) 0.0195(10) Uani 1 1 d . . . C21 C 0.2322(6) 0.9960(5) 0.0348(4) 0.0230(11) Uani 1 1 d . . . H21 H 0.2551 0.9158 -0.0127 0.028 Uiso 1 1 calc R . . C22 C 0.1712(6) 1.0862(6) 0.0023(4) 0.0284(12) Uani 1 1 d . . . H22 H 0.1530 1.0673 -0.0673 0.034 Uiso 1 1 calc R . . C23 C 0.1368(6) 1.2028(6) 0.0701(5) 0.0327(14) Uani 1 1 d . . . H23 H 0.0942 1.2634 0.0474 0.039 Uiso 1 1 calc R . . C24 C 0.1649(6) 1.2309(6) 0.1716(4) 0.0308(13) Uani 1 1 d . . . H24 H 0.1426 1.3119 0.2186 0.037 Uiso 1 1 calc R . . C25 C 0.2257(6) 1.1409(6) 0.2051(4) 0.0288(13) Uani 1 1 d . . . H25 H 0.2438 1.1603 0.2748 0.035 Uiso 1 1 calc R . . C26 C 0.3646(16) 0.5637(16) 0.5561(11) 0.052(4) Uiso 0.50 1 d P . . Cl2 Cl 0.2388(5) 0.4253(6) 0.4815(4) 0.0548(12) Uiso 0.40 1 d P . . Cl3 Cl 0.4522(4) 0.5320(4) 0.6523(3) 0.0433(9) Uiso 0.40 1 d P . . Cl2A Cl 0.5000 0.5000 0.5000 0.089(10) Uiso 0.10 2 d SP . . Cl3A Cl 0.1972(18) 0.4715(18) 0.5112(13) 0.072(4) Uiso 0.15 1 d P . . 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 0.0207(3) 0.0170(2) 0.0142(2) 0.00601(17) -0.00139(16) 0.00500(17) Cl1 0.0220(6) 0.0274(7) 0.0230(7) 0.0117(5) -0.0038(5) 0.0024(5) P1 0.0199(7) 0.0151(6) 0.0148(6) 0.0047(5) -0.0025(5) 0.0027(5) O1 0.032(2) 0.030(2) 0.033(2) 0.0044(18) 0.0018(18) 0.0130(19) O2 0.033(2) 0.036(2) 0.024(2) 0.0042(19) -0.0048(18) 0.003(2) O3 0.025(2) 0.0232(19) 0.028(2) 0.0090(16) 0.0008(16) 0.0082(17) N1 0.020(2) 0.019(2) 0.017(2) 0.0048(18) -0.0026(17) 0.0030(17) C1 0.032(3) 0.032(3) 0.035(3) 0.022(3) 0.014(3) 0.012(3) C2 0.034(3) 0.029(3) 0.021(3) 0.017(2) 0.004(2) 0.012(2) C3 0.029(3) 0.019(3) 0.023(3) 0.013(2) 0.000(2) 0.009(2) C4 0.035(3) 0.016(3) 0.025(3) 0.009(2) 0.004(2) 0.010(2) C5 0.033(3) 0.019(3) 0.032(3) 0.013(2) 0.002(2) 0.004(2) C6 0.017(3) 0.027(3) 0.022(3) 0.010(2) -0.004(2) 0.004(2) C7 0.033(3) 0.026(3) 0.018(3) 0.010(2) 0.003(2) 0.014(3) C8 0.029(3) 0.024(3) 0.031(3) 0.015(2) -0.001(2) -0.002(2) C9 0.029(3) 0.030(3) 0.034(3) 0.015(3) 0.000(3) -0.006(2) C10 0.022(3) 0.034(3) 0.024(3) 0.011(2) -0.001(2) 0.006(2) C11 0.021(3) 0.026(3) 0.022(3) 0.009(2) -0.002(2) 0.005(2) C12 0.019(3) 0.030(3) 0.016(2) 0.006(2) 0.008(2) 0.011(2) C13 0.020(3) 0.044(3) 0.032(3) 0.022(3) 0.001(2) 0.011(2) C14 0.029(3) 0.018(2) 0.016(2) 0.008(2) -0.003(2) 0.006(2) C15 0.030(3) 0.022(3) 0.019(3) 0.003(2) -0.004(2) 0.003(2) C16 0.047(4) 0.023(3) 0.023(3) 0.004(2) -0.003(3) 0.004(3) C17 0.066(4) 0.023(3) 0.018(3) 0.001(2) -0.001(3) 0.015(3) C18 0.039(3) 0.037(3) 0.021(3) 0.012(3) 0.009(2) 0.018(3) C19 0.026(3) 0.028(3) 0.021(3) 0.009(2) 0.002(2) 0.009(2) C20 0.021(3) 0.019(3) 0.019(3) 0.010(2) -0.003(2) 0.003(2) C21 0.028(3) 0.021(3) 0.020(3) 0.007(2) 0.000(2) 0.007(2) C22 0.027(3) 0.036(3) 0.026(3) 0.019(3) -0.004(2) 0.005(2) C23 0.032(3) 0.034(3) 0.041(4) 0.024(3) 0.000(3) 0.009(3) C24 0.036(3) 0.027(3) 0.035(3) 0.016(3) 0.007(3) 0.010(3) C25 0.043(3) 0.022(3) 0.022(3) 0.010(2) 0.001(2) 0.006(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 C6 1.961(5) . ? Mo1 C7 1.969(6) . ? Mo1 C2 2.274(4) . ? Mo1 C3 2.312(3) . ? Mo1 C1 2.327(4) . ? Mo1 C4 2.386(3) . ? Mo1 C5 2.396(4) . ? Mo1 Cl1 2.4991(16) . ? Mo1 P1 2.5176(16) . ? P1 N1 1.748(4) . ? P1 C20 1.821(5) . ? P1 C14 1.825(5) . ? O1 C6 1.145(6) . ? O2 C7 1.131(7) . ? O3 C12 1.222(6) . ? N1 C8 1.383(7) . ? N1 C11 1.407(6) . ? C1 C5 1.4200 . ? C1 C2 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C8 C9 1.355(8) . ? C9 C10 1.395(8) . ? C10 C11 1.366(8) . ? C11 C12 1.451(7) . ? C12 C13 1.495(7) . ? C14 C19 1.381(7) . ? C14 C15 1.403(7) . ? C15 C16 1.378(8) . ? C16 C17 1.392(9) . ? C17 C18 1.387(9) . ? C18 C19 1.377(8) . ? C20 C25 1.393(7) . ? C20 C21 1.393(7) . ? C21 C22 1.389(7) . ? C22 C23 1.379(8) . ? C23 C24 1.384(8) . ? C24 C25 1.396(8) . ? C26 Cl2 1.677(16) . ? C26 Cl3A 1.69(2) . ? C26 Cl2A 1.712(15) . ? C26 Cl3 1.742(16) . ? Cl2 Cl3A 0.728(16) . ? Cl3 Cl2A 2.196(4) . ? Cl2A C26 1.712(15) 2_666 ? Cl2A Cl3 2.196(4) 2_666 ? 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 C6 Mo1 C7 76.0(2) . . ? C6 Mo1 C2 96.88(17) . . ? C7 Mo1 C2 90.09(17) . . ? C6 Mo1 C3 130.43(17) . . ? C7 Mo1 C3 87.02(17) . . ? C2 Mo1 C3 36.1 . . ? C6 Mo1 C1 92.32(17) . . ? C7 Mo1 C1 123.63(18) . . ? C2 Mo1 C1 35.93(5) . . ? C3 Mo1 C1 59.37(6) . . ? C6 Mo1 C4 150.59(17) . . ? C7 Mo1 C4 117.14(17) . . ? C2 Mo1 C4 59.02(6) . . ? C3 Mo1 C4 35.1 . . ? C1 Mo1 C4 58.33(6) . . ? C6 Mo1 C5 120.35(18) . . ? C7 Mo1 C5 144.87(17) . . ? C2 Mo1 C5 58.87(7) . . ? C3 Mo1 C5 58.40(6) . . ? C1 Mo1 C5 35.0 . . ? C4 Mo1 C5 34.5 . . ? C6 Mo1 Cl1 80.03(15) . . ? C7 Mo1 Cl1 134.99(15) . . ? C2 Mo1 Cl1 130.53(10) . . ? C3 Mo1 Cl1 136.48(9) . . ? C1 Mo1 Cl1 94.61(10) . . ? C4 Mo1 Cl1 102.30(9) . . ? C5 Mo1 Cl1 80.10(9) . . ? C6 Mo1 P1 111.62(16) . . ? C7 Mo1 P1 77.86(16) . . ? C2 Mo1 P1 144.83(9) . . ? C3 Mo1 P1 109.57(9) . . ? C1 Mo1 P1 152.05(9) . . ? C4 Mo1 P1 97.25(8) . . ? C5 Mo1 P1 117.14(10) . . ? Cl1 Mo1 P1 76.42(5) . . ? N1 P1 C20 98.7(2) . . ? N1 P1 C14 100.8(2) . . ? C20 P1 C14 104.4(2) . . ? N1 P1 Mo1 119.98(15) . . ? C20 P1 Mo1 111.17(17) . . ? C14 P1 Mo1 118.93(17) . . ? C8 N1 C11 106.1(4) . . ? C8 N1 P1 125.5(4) . . ? C11 N1 P1 128.3(3) . . ? C5 C1 C2 108.0 . . ? C5 C1 Mo1 75.16(14) . . ? C2 C1 Mo1 70.00(13) . . ? C1 C2 C3 108.0 . . ? C1 C2 Mo1 74.08(14) . . ? C3 C2 Mo1 73.41(14) . . ? C4 C3 C2 108.0 . . ? C4 C3 Mo1 75.31(14) . . ? C2 C3 Mo1 70.53(14) . . ? C3 C4 C5 108.0 . . ? C3 C4 Mo1 69.55(13) . . ? C5 C4 Mo1 73.09(13) . . ? C1 C5 C4 108.0 . . ? C1 C5 Mo1 69.89(13) . . ? C4 C5 Mo1 72.37(13) . . ? O1 C6 Mo1 177.6(5) . . ? O2 C7 Mo1 178.0(5) . . ? C9 C8 N1 109.7(5) . . ? C8 C9 C10 107.8(5) . . ? C11 C10 C9 107.9(5) . . ? C10 C11 N1 108.4(5) . . ? C10 C11 C12 129.1(5) . . ? N1 C11 C12 122.2(5) . . ? O3 C12 C11 121.0(5) . . ? O3 C12 C13 120.7(5) . . ? C11 C12 C13 118.2(5) . . ? C19 C14 C15 119.4(5) . . ? C19 C14 P1 121.9(4) . . ? C15 C14 P1 118.7(4) . . ? C16 C15 C14 119.9(5) . . ? C15 C16 C17 120.3(6) . . ? C18 C17 C16 119.5(5) . . ? C19 C18 C17 120.3(5) . . ? C18 C19 C14 120.6(5) . . ? C25 C20 C21 119.0(5) . . ? C25 C20 P1 118.6(4) . . ? C21 C20 P1 122.4(4) . . ? C22 C21 C20 120.3(5) . . ? C23 C22 C21 120.6(5) . . ? C22 C23 C24 119.6(5) . . ? C23 C24 C25 120.4(5) . . ? C20 C25 C24 120.1(5) . . ? Cl2 C26 Cl3A 25.0(6) . . ? Cl2 C26 Cl2A 94.5(8) . . ? Cl3A C26 Cl2A 119.4(11) . . ? Cl2 C26 Cl3 113.6(9) . . ? Cl3A C26 Cl3 117.4(10) . . ? Cl2A C26 Cl3 78.9(7) . . ? Cl3A Cl2 C26 78.3(15) . . ? C26 Cl3 Cl2A 49.9(5) . . ? C26 Cl2A C26 180.0(10) . 2_666 ? C26 Cl2A Cl3 51.1(5) . . ? C26 Cl2A Cl3 128.9(5) 2_666 . ? C26 Cl2A Cl3 128.9(5) . 2_666 ? C26 Cl2A Cl3 51.1(5) 2_666 2_666 ? Cl3 Cl2A Cl3 180.000(1) . 2_666 ? Cl2 Cl3A C26 76.7(15) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.406 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.120