Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Sonia M.P.R.M Cunha' 'M Fatima C Guedes da Silva' 'Armando J. L. Pombeiro' _publ_contact_author_name 'Prof Armando J. L. Pombeiro' _publ_contact_author_address ; Centro de Química Estrutural, Complexo I Instituto Superior Técnico Av. Rovisco Pais, 1049-001 Lisboa Lisboa 1049-001 PORTUGAL ; _publ_contact_author_email 'POMBEIRO@IST.UTL.PT' _publ_section_title ; Activation of cyanamide by a molybdenum(0) diphosphinic centre. Formation of cyanoimide and its reactivity with electrophiles ; data_pmb01 _database_code_CSD 171672 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H48 B Cl2 F4 Mo N4 P4' _chemical_formula_weight 1142.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 22.450(4) _cell_length_b 12.196(2) _cell_length_c 39.540(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.93(3) _cell_angle_gamma 90.00 _cell_volume 10695(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 24.2 _cell_measurement_theta_max 35.7 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4664 _exptl_absorpt_coefficient_mu 4.511 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3447 _exptl_absorpt_correction_T_max 0.4811 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator filter _diffrn_measurement_device_type Nicolet_P3 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 4006 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 50.06 _reflns_number_total 4004 _reflns_number_gt 3931 _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^)+(0.1336P)^2^+104.6649P] 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 0.000013(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4004 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1938 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.234 _refine_ls_shift/su_mean 0.034 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.0000 0.35817(9) 0.2500 0.0588(5) Uani 1 2 d S . . P1 P 0.02800(13) 0.2250(2) 0.29958(7) 0.0574(8) Uani 1 1 d . . . P2 P 0.03498(12) 0.4921(2) 0.29858(7) 0.0563(8) Uani 1 1 d . . . N1 N -0.0799(4) 0.3582(6) 0.2607(2) 0.057(2) Uani 1 1 d . . . N2A N -0.1774(9) 0.3557(14) 0.2772(5) 0.110(6) Uiso 0.75 1 d P . . N2B N -0.1920(16) 0.358(3) 0.2568(11) 0.061(10) Uiso 0.25 1 d P . . C1 C -0.0247(5) 0.1160(9) 0.3054(3) 0.062(3) Uani 1 1 d . . . C2 C -0.0791(5) 0.1403(10) 0.3181(3) 0.071(3) Uani 1 1 d . . . C3 C -0.1211(6) 0.0598(14) 0.3200(3) 0.088(4) Uani 1 1 d . . . C4 C -0.1108(8) -0.0444(13) 0.3096(4) 0.102(5) Uani 1 1 d . . . C5 C -0.0572(7) -0.0705(11) 0.2979(4) 0.093(4) Uani 1 1 d . . . C6 C -0.0164(6) 0.0099(10) 0.2957(3) 0.078(3) Uani 1 1 d . . . C7 C 0.1009(5) 0.1561(9) 0.3048(3) 0.066(3) Uani 1 1 d . . . C8 C 0.1263(6) 0.1248(9) 0.2768(3) 0.074(3) Uani 1 1 d . . . C9 C 0.1812(6) 0.0713(11) 0.2802(4) 0.085(4) Uani 1 1 d . . . C10 C 0.2111(6) 0.0485(11) 0.3115(5) 0.097(4) Uani 1 1 d . . . C11 C 0.1869(8) 0.0778(15) 0.3405(4) 0.116(5) Uani 1 1 d . . . C12 C 0.1326(6) 0.1305(12) 0.3369(4) 0.094(4) Uani 1 1 d . . . C13 C 0.0910(5) 0.5953(9) 0.2930(3) 0.061(3) Uani 1 1 d . . . C14 C 0.1501(6) 0.5634(11) 0.2912(3) 0.082(4) Uani 1 1 d . . . C15 C 0.1911(6) 0.6460(17) 0.2847(4) 0.111(5) Uani 1 1 d . . . C16 C 0.1736(9) 0.7544(13) 0.2807(4) 0.107(5) Uani 1 1 d . . . C17 C 0.1174(7) 0.7830(11) 0.2828(4) 0.096(4) Uani 1 1 d . . . C18 C 0.0767(6) 0.7036(11) 0.2882(3) 0.080(4) Uani 1 1 d . . . C19 C -0.0213(5) 0.5671(8) 0.3178(3) 0.058(3) Uani 1 1 d . . . C20 C -0.0098(6) 0.6027(12) 0.3511(3) 0.088(4) Uani 1 1 d . . . C21 C -0.0537(9) 0.6588(12) 0.3650(4) 0.107(5) Uani 1 1 d . . . C22 C -0.1082(8) 0.6816(11) 0.3466(4) 0.089(4) Uani 1 1 d . . . C23 C -0.1208(5) 0.6493(10) 0.3134(4) 0.078(3) Uani 1 1 d . . . C24 C -0.0764(6) 0.5911(9) 0.2992(3) 0.069(3) Uani 1 1 d . . . C25 C 0.0312(5) 0.3105(9) 0.3378(2) 0.063(3) Uani 1 1 d . . . C26 C 0.0715(5) 0.4088(9) 0.3341(3) 0.067(3) Uani 1 1 d . . . C27 C -0.1298(7) 0.3576(10) 0.2673(4) 0.099(5) Uani 1 1 d . . . Mo1' Mo 0.0000 0.0000 0.5000 0.0605(5) Uani 1 2 d S . . P1' P 0.01638(13) 0.0643(2) 0.44139(7) 0.0612(8) Uani 1 1 d . . . P2' P -0.09223(12) -0.0838(2) 0.46327(7) 0.0601(8) Uani 1 1 d . . . N1' N -0.0447(4) 0.1314(7) 0.5028(2) 0.060(2) Uani 1 1 d . . . N2'A N -0.0985(10) 0.301(2) 0.5028(6) 0.145(8) Uiso 0.75 1 d P . . N2'B N -0.0897(14) 0.310(3) 0.5222(9) 0.048(9) Uiso 0.25 1 d P . . C1' C 0.0440(6) 0.2033(10) 0.4352(3) 0.067(3) Uani 1 1 d . . . C2' C 0.0047(6) 0.2916(12) 0.4325(3) 0.088(4) Uani 1 1 d . . . C3' C 0.0282(9) 0.3975(12) 0.4305(4) 0.103(5) Uani 1 1 d . . . C4' C 0.0875(11) 0.4140(13) 0.4309(4) 0.111(5) Uani 1 1 d . . . C5' C 0.1258(7) 0.3295(15) 0.4327(4) 0.103(5) Uani 1 1 d . . . C6' C 0.1054(6) 0.2214(11) 0.4346(3) 0.085(4) Uani 1 1 d . . . C7' C 0.0621(6) -0.0249(10) 0.4187(3) 0.073(3) Uani 1 1 d . . . C8' C 0.1179(7) -0.0589(12) 0.4358(3) 0.091(4) Uani 1 1 d . . . C9' C 0.1565(7) -0.1214(14) 0.4185(5) 0.123(6) Uani 1 1 d . . . C10' C 0.1334(11) -0.1527(16) 0.3846(5) 0.144(7) Uani 1 1 d . . . C11' C 0.0793(9) -0.1196(17) 0.3692(4) 0.128(6) Uani 1 1 d . . . C12' C 0.0438(6) -0.0560(11) 0.3858(3) 0.088(4) Uani 1 1 d . . . C13' C -0.1044(5) -0.2318(10) 0.4586(3) 0.065(3) Uani 1 1 d . . . C14' C -0.1494(6) -0.2699(11) 0.4331(3) 0.078(3) Uani 1 1 d . . . C15' C -0.1580(6) -0.3807(13) 0.4281(3) 0.087(4) Uani 1 1 d . . . C16' C -0.1236(7) -0.4529(11) 0.4488(4) 0.090(4) Uani 1 1 d . . . C17' C -0.0813(7) -0.4168(12) 0.4741(4) 0.090(4) Uani 1 1 d . . . C18' C -0.0707(5) -0.3054(10) 0.4794(3) 0.072(3) Uani 1 1 d . . . C19' C -0.1647(5) -0.0340(10) 0.4725(3) 0.068(3) Uani 1 1 d . . . C20' C -0.1993(6) -0.1005(10) 0.4907(3) 0.079(3) Uani 1 1 d . . . C21' C -0.2516(6) -0.0614(13) 0.5003(4) 0.098(4) Uani 1 1 d . . . C22' C -0.2701(6) 0.0417(15) 0.4919(4) 0.104(5) Uani 1 1 d . . . C23' C -0.2375(7) 0.1091(13) 0.4742(4) 0.108(5) Uani 1 1 d . . . C24' C -0.1846(6) 0.0699(11) 0.4642(4) 0.087(4) Uani 1 1 d . . . C25' C -0.0592(5) 0.0668(10) 0.4155(3) 0.071(3) Uani 1 1 d . . . C26' C -0.0907(5) -0.0423(10) 0.4185(3) 0.072(3) Uani 1 1 d . . . C27' C -0.0687(6) 0.2149(14) 0.5070(5) 0.112(6) Uani 1 1 d . . . B B -0.1729(13) 0.313(2) 0.3780(10) 0.148(11) Uani 1 1 d . . . F1 F -0.1205(7) 0.3436(15) 0.3716(5) 0.249(8) Uani 1 1 d . . . F2 F -0.1702(10) 0.2781(17) 0.4094(6) 0.314(13) Uani 1 1 d . . . F3 F -0.1983(10) 0.255(2) 0.3559(6) 0.367(17) Uani 1 1 d . . . F4 F -0.2073(6) 0.3968(12) 0.3817(4) 0.233(7) Uani 1 1 d . . . Cl1 Cl 0.2461(3) 0.4108(9) 0.3625(3) 0.278(5) Uani 1 1 d . . . Cl2 Cl 0.1806(4) 0.5783(9) 0.3889(3) 0.276(4) Uani 1 1 d . . . C1D C 0.2454(10) 0.542(3) 0.3780(12) 0.33(3) Uani 1 1 d . . . H2A H -0.0860 0.2137 0.3258 0.080 Uiso 1 1 d . . . H3A H -0.1582 0.0775 0.3274 0.080 Uiso 1 1 d . . . H4A H -0.1412 -0.0996 0.3108 0.080 Uiso 1 1 d . . . H5A H -0.0491 -0.1442 0.2910 0.080 Uiso 1 1 d . . . H6A H 0.0178 -0.0074 0.2867 0.080 Uiso 1 1 d . . . H8A H 0.1064 0.1414 0.2552 0.080 Uiso 1 1 d . . . H9A H 0.1982 0.0499 0.2605 0.080 Uiso 1 1 d . . . H10A H 0.2486 0.0100 0.3135 0.080 Uiso 1 1 d . . . H11A H 0.2089 0.0612 0.3628 0.080 Uiso 1 1 d . . . H12A H 0.1162 0.1497 0.3563 0.080 Uiso 1 1 d . . . H14A H 0.1629 0.4875 0.2941 0.080 Uiso 1 1 d . . . H15A H 0.2318 0.6278 0.2838 0.080 Uiso 1 1 d . . . H16A H 0.2034 0.8092 0.2764 0.080 Uiso 1 1 d . . . H17A H 0.1054 0.8577 0.2805 0.080 Uiso 1 1 d . . . H18A H 0.0363 0.7245 0.2885 0.080 Uiso 1 1 d . . . H20A H 0.0296 0.5906 0.3648 0.080 Uiso 1 1 d . . . H21A H -0.0458 0.6818 0.3882 0.080 Uiso 1 1 d . . . H22A H -0.1385 0.7204 0.3570 0.080 Uiso 1 1 d . . . H23A H -0.1590 0.6650 0.2998 0.080 Uiso 1 1 d . . . H24A H -0.0854 0.5682 0.2758 0.080 Uiso 1 1 d . . . H25A H 0.0468 0.2701 0.3572 0.080 Uiso 1 1 d . . . H25B H -0.0096 0.3337 0.3395 0.080 Uiso 1 1 d . . . H26A H 0.0732 0.4521 0.3547 0.080 Uiso 1 1 d . . . H26B H 0.1085 0.3872 0.3303 0.080 Uiso 1 1 d . . . H2'A H -0.0375 0.2798 0.4321 0.080 Uiso 1 1 d . . . H3'A H 0.0007 0.4596 0.4289 0.080 Uiso 1 1 d . . . H4'A H 0.1014 0.4882 0.4293 0.080 Uiso 1 1 d . . . H5'A H 0.1682 0.3437 0.4330 0.080 Uiso 1 1 d . . . H6'A H 0.1327 0.1606 0.4355 0.080 Uiso 1 1 d . . . H8'A H 0.1298 -0.0393 0.4592 0.080 Uiso 1 1 d . . . H9'A H 0.1969 -0.1430 0.4299 0.080 Uiso 1 1 d . . . H10B H 0.1583 -0.1982 0.3729 0.080 Uiso 1 1 d . . . H11B H 0.0671 -0.1407 0.3462 0.080 Uiso 1 1 d . . . H12B H 0.0055 -0.0319 0.3739 0.080 Uiso 1 1 d . . . H14B H -0.1743 -0.2182 0.4186 0.080 Uiso 1 1 d . . . H15B H -0.1882 -0.4064 0.4102 0.080 Uiso 1 1 d . . . H16B H -0.1287 -0.5298 0.4454 0.080 Uiso 1 1 d . . . H17B H -0.0579 -0.4688 0.4890 0.080 Uiso 1 1 d . . . H18B H -0.0397 -0.2804 0.4976 0.080 Uiso 1 1 d . . . H20B H -0.1863 -0.1732 0.4961 0.080 Uiso 1 1 d . . . H21B H -0.2751 -0.1077 0.5130 0.080 Uiso 1 1 d . . . H22B H -0.3069 0.0690 0.4982 0.080 Uiso 1 1 d . . . H23B H -0.2519 0.1821 0.4687 0.080 Uiso 1 1 d . . . H24B H -0.1619 0.1167 0.4519 0.080 Uiso 1 1 d . . . H25C H -0.0557 0.0811 0.3921 0.080 Uiso 1 1 d . . . H25D H -0.0824 0.1251 0.4234 0.080 Uiso 1 1 d . . . H26C H -0.1313 -0.0366 0.4066 0.080 Uiso 1 1 d . . . H26D H -0.0705 -0.0975 0.4073 0.080 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0856(10) 0.0375(8) 0.0551(8) 0.000 0.0167(7) 0.000 P1 0.0728(19) 0.0437(16) 0.0586(17) 0.0045(13) 0.0195(14) 0.0008(14) P2 0.0663(18) 0.0434(16) 0.0615(17) -0.0036(13) 0.0169(14) -0.0027(14) N1 0.057(6) 0.033(5) 0.079(6) -0.003(4) 0.011(5) 0.000(4) C1 0.074(8) 0.046(7) 0.064(7) 0.018(5) 0.005(6) 0.000(6) C2 0.069(8) 0.075(9) 0.072(8) 0.000(6) 0.017(6) 0.005(7) C3 0.080(9) 0.098(12) 0.091(10) 0.022(8) 0.029(7) -0.017(9) C4 0.106(12) 0.075(11) 0.123(12) 0.030(9) 0.012(10) -0.025(9) C5 0.105(11) 0.058(9) 0.114(11) -0.010(8) 0.012(9) -0.010(9) C6 0.088(9) 0.058(9) 0.087(9) 0.010(7) 0.013(7) 0.004(8) C7 0.070(7) 0.063(7) 0.063(8) 0.010(6) 0.004(7) -0.007(6) C8 0.084(9) 0.056(8) 0.084(9) 0.015(6) 0.019(7) 0.011(7) C9 0.081(10) 0.075(9) 0.105(11) 0.015(8) 0.030(8) 0.009(8) C10 0.074(10) 0.076(9) 0.141(15) 0.007(10) 0.022(10) 0.015(7) C11 0.103(13) 0.125(14) 0.110(13) 0.031(11) -0.013(10) 0.022(11) C12 0.086(10) 0.114(12) 0.085(10) 0.011(8) 0.016(8) 0.029(9) C13 0.060(8) 0.057(8) 0.064(7) 0.000(6) 0.008(6) -0.008(6) C14 0.065(9) 0.084(9) 0.099(10) 0.007(7) 0.013(7) -0.007(8) C15 0.047(8) 0.158(17) 0.130(13) 0.005(11) 0.022(8) -0.021(10) C16 0.135(15) 0.071(11) 0.122(12) -0.001(9) 0.037(11) -0.036(10) C17 0.101(11) 0.060(9) 0.138(13) -0.014(8) 0.054(10) -0.010(9) C18 0.091(9) 0.065(9) 0.093(9) -0.002(7) 0.044(7) -0.016(8) C19 0.069(8) 0.046(7) 0.061(7) -0.009(6) 0.022(6) -0.007(6) C20 0.089(9) 0.096(10) 0.083(10) -0.020(8) 0.023(7) 0.015(8) C21 0.157(15) 0.094(11) 0.078(10) -0.020(8) 0.041(11) 0.027(11) C22 0.112(12) 0.069(9) 0.095(11) 0.010(8) 0.044(9) 0.020(8) C23 0.068(8) 0.068(8) 0.102(11) -0.001(8) 0.022(7) 0.008(7) C24 0.091(10) 0.054(7) 0.067(7) -0.007(6) 0.032(7) 0.001(7) C25 0.089(8) 0.053(7) 0.049(6) 0.007(5) 0.015(6) 0.001(6) C26 0.074(8) 0.054(7) 0.070(7) -0.015(6) 0.005(6) -0.006(6) C27 0.075(10) 0.052(8) 0.178(15) -0.014(8) 0.042(11) -0.008(7) Mo1' 0.0581(8) 0.0701(10) 0.0557(8) 0.0053(7) 0.0160(6) 0.0035(7) P1' 0.0685(19) 0.0616(19) 0.0558(17) 0.0047(14) 0.0172(14) 0.0072(15) P2' 0.0608(18) 0.0597(19) 0.0616(18) 0.0000(14) 0.0149(14) 0.0034(15) N1' 0.066(6) 0.041(5) 0.074(6) 0.001(5) 0.016(5) 0.015(5) C1' 0.075(9) 0.062(8) 0.066(7) 0.012(6) 0.012(6) 0.004(7) C2' 0.117(11) 0.072(10) 0.079(9) 0.005(7) 0.027(8) 0.002(9) C3' 0.143(15) 0.065(10) 0.107(11) 0.011(8) 0.035(11) 0.021(10) C4' 0.158(17) 0.067(11) 0.104(12) 0.010(9) 0.009(12) -0.026(12) C5' 0.101(11) 0.101(13) 0.106(11) 0.014(9) 0.014(9) -0.029(10) C6' 0.089(10) 0.076(10) 0.085(9) 0.012(7) 0.003(7) -0.004(8) C7' 0.084(9) 0.077(9) 0.067(9) 0.002(7) 0.037(7) 0.008(7) C8' 0.091(10) 0.098(10) 0.088(9) -0.001(8) 0.024(8) 0.019(8) C9' 0.119(13) 0.139(15) 0.119(14) 0.014(11) 0.049(11) 0.065(11) C10' 0.20(2) 0.148(16) 0.102(14) -0.021(12) 0.071(14) 0.071(15) C11' 0.148(16) 0.158(17) 0.085(11) -0.031(11) 0.042(11) 0.043(13) C12' 0.110(11) 0.095(10) 0.064(9) -0.005(7) 0.027(8) 0.013(8) C13' 0.069(8) 0.080(9) 0.051(7) -0.013(7) 0.025(6) -0.005(7) C14' 0.081(9) 0.075(10) 0.081(9) -0.008(7) 0.017(7) 0.001(7) C15' 0.092(10) 0.089(11) 0.082(9) -0.019(8) 0.026(8) -0.026(9) C16' 0.103(11) 0.064(9) 0.114(12) -0.010(9) 0.046(10) -0.007(9) C17' 0.095(11) 0.073(10) 0.105(11) 0.004(9) 0.028(9) 0.011(8) C18' 0.072(8) 0.063(9) 0.087(9) 0.005(7) 0.033(7) 0.006(7) C19' 0.067(8) 0.072(9) 0.066(7) -0.008(6) 0.014(6) 0.011(7) C20' 0.074(9) 0.074(8) 0.095(9) -0.008(7) 0.033(7) 0.004(7) C21' 0.080(10) 0.094(11) 0.129(12) 0.011(9) 0.041(8) 0.009(8) C22' 0.071(10) 0.118(13) 0.127(13) -0.012(10) 0.033(9) 0.040(10) C23' 0.091(11) 0.094(11) 0.140(14) 0.023(10) 0.024(10) 0.030(9) C24' 0.082(10) 0.074(10) 0.110(10) 0.008(8) 0.026(8) 0.006(8) C25' 0.083(8) 0.083(9) 0.048(7) 0.006(6) 0.010(6) 0.007(7) C26' 0.067(8) 0.085(9) 0.063(7) 0.001(6) 0.005(6) -0.007(7) C27' 0.077(10) 0.082(11) 0.186(17) 0.059(11) 0.044(10) 0.018(9) B 0.106(18) 0.11(2) 0.24(4) -0.05(2) 0.06(2) -0.024(16) F1 0.180(13) 0.29(2) 0.283(19) -0.091(15) 0.064(12) -0.026(13) F2 0.38(3) 0.26(2) 0.29(2) 0.174(19) 0.019(19) -0.021(18) F3 0.32(2) 0.37(3) 0.42(3) -0.28(3) 0.07(2) -0.12(2) F4 0.183(12) 0.186(12) 0.310(18) -0.052(13) -0.023(11) 0.093(11) Cl1 0.158(6) 0.289(11) 0.358(12) 0.050(10) -0.048(7) 0.006(7) Cl2 0.224(8) 0.302(11) 0.291(10) -0.024(9) 0.011(7) -0.094(8) C1D 0.085(16) 0.28(4) 0.63(8) -0.24(5) 0.07(3) -0.04(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.907(9) . ? Mo1 N1 1.907(9) 2 ? Mo1 P1 2.549(3) 2 ? Mo1 P1 2.549(3) . ? Mo1 P2 2.551(3) . ? Mo1 P2 2.551(3) 2 ? P1 C1 1.818(11) . ? P1 C7 1.823(12) . ? P1 C25 1.829(10) . ? P2 C13 1.816(11) . ? P2 C26 1.821(12) . ? P2 C19 1.819(11) . ? N1 C27 1.189(15) . ? N2A N2B 0.82(4) . ? N2A C27 1.19(2) . ? N2B C27 1.39(4) . ? C1 C6 1.371(15) . ? C1 C2 1.422(15) . ? C2 C3 1.371(17) . ? C3 C4 1.37(2) . ? C4 C5 1.39(2) . ? C5 C6 1.354(17) . ? C7 C8 1.375(16) . ? C7 C12 1.393(16) . ? C8 C9 1.383(16) . ? C9 C10 1.343(19) . ? C10 C11 1.39(2) . ? C11 C12 1.368(19) . ? C13 C18 1.366(16) . ? C13 C14 1.396(15) . ? C14 C15 1.414(19) . ? C15 C16 1.38(2) . ? C16 C17 1.32(2) . ? C17 C18 1.373(17) . ? C19 C24 1.367(15) . ? C19 C20 1.375(15) . ? C20 C21 1.382(18) . ? C21 C22 1.353(19) . ? C22 C23 1.357(18) . ? C23 C24 1.408(16) . ? C25 C26 1.523(15) . ? Mo1' N1' 1.904(9) . ? Mo1' N1' 1.904(9) 5_556 ? Mo1' P1' 2.527(3) 5_556 ? Mo1' P1' 2.527(3) . ? Mo1' P2' 2.551(3) . ? Mo1' P2' 2.551(3) 5_556 ? P1' C7' 1.823(12) . ? P1' C1' 1.834(12) . ? P1' C25' 1.841(12) . ? P2' C19' 1.826(11) . ? P2' C13' 1.832(12) . ? P2' C26' 1.848(11) . ? N1' C27' 1.176(17) . ? N2'A N2'B 0.77(3) . ? N2'A C27' 1.24(2) . ? N2'B C27' 1.42(4) . ? C1' C2' 1.386(17) . ? C1' C6' 1.400(16) . ? C2' C3' 1.40(2) . ? C3' C4' 1.34(2) . ? C4' C5' 1.34(2) . ? C5' C6' 1.401(19) . ? C7' C12' 1.358(16) . ? C7' C8' 1.390(17) . ? C8' C9' 1.409(18) . ? C9' C10' 1.41(2) . ? C10' C11' 1.33(2) . ? C11' C12' 1.353(19) . ? C13' C18' 1.365(15) . ? C13' C14' 1.392(15) . ? C14' C15' 1.376(18) . ? C15' C16' 1.360(19) . ? C16' C17' 1.340(19) . ? C17' C18' 1.389(18) . ? C19' C24' 1.367(16) . ? C19' C20' 1.398(16) . ? C20' C21' 1.373(17) . ? C21' C22' 1.35(2) . ? C22' C23' 1.36(2) . ? C23' C24' 1.394(18) . ? C25' C26' 1.520(16) . ? B F3 1.20(3) . ? B F1 1.30(2) . ? B F2 1.30(4) . ? B F4 1.31(3) . ? Cl1 C1D 1.71(3) . ? Cl2 C1D 1.64(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 N1 180.0(6) . 2 ? N1 Mo1 P1 92.4(3) . 2 ? N1 Mo1 P1 87.5(3) 2 2 ? N1 Mo1 P1 87.5(3) . . ? N1 Mo1 P1 92.4(3) 2 . ? P1 Mo1 P1 100.80(13) 2 . ? N1 Mo1 P2 91.3(2) . . ? N1 Mo1 P2 88.7(3) 2 . ? P1 Mo1 P2 176.23(9) 2 . ? P1 Mo1 P2 79.55(9) . . ? N1 Mo1 P2 88.7(3) . 2 ? N1 Mo1 P2 91.3(2) 2 2 ? P1 Mo1 P2 79.55(9) 2 2 ? P1 Mo1 P2 176.23(9) . 2 ? P2 Mo1 P2 100.35(13) . 2 ? C1 P1 C7 103.9(5) . . ? C1 P1 C25 104.8(5) . . ? C7 P1 C25 104.5(5) . . ? C1 P1 Mo1 118.4(3) . . ? C7 P1 Mo1 119.3(4) . . ? C25 P1 Mo1 104.2(3) . . ? C13 P2 C26 104.0(5) . . ? C13 P2 C19 104.0(5) . . ? C26 P2 C19 102.6(5) . . ? C13 P2 Mo1 119.4(4) . . ? C26 P2 Mo1 105.8(3) . . ? C19 P2 Mo1 118.9(4) . . ? C27 N1 Mo1 179.6(11) . . ? N2B N2A C27 85(3) . . ? N2A N2B C27 59(3) . . ? C6 C1 C2 117.2(11) . . ? C6 C1 P1 122.4(10) . . ? C2 C1 P1 120.3(9) . . ? C3 C2 C1 120.4(11) . . ? C4 C3 C2 119.9(12) . . ? C3 C4 C5 120.6(12) . . ? C6 C5 C4 119.0(12) . . ? C5 C6 C1 122.9(12) . . ? C8 C7 C12 117.1(11) . . ? C8 C7 P1 121.0(9) . . ? C12 C7 P1 121.9(10) . . ? C7 C8 C9 121.8(12) . . ? C10 C9 C8 119.8(13) . . ? C9 C10 C11 120.3(13) . . ? C12 C11 C10 119.6(13) . . ? C11 C12 C7 121.3(13) . . ? C18 C13 C14 117.9(10) . . ? C18 C13 P2 122.3(9) . . ? C14 C13 P2 119.7(9) . . ? C13 C14 C15 117.5(12) . . ? C16 C15 C14 121.4(13) . . ? C17 C16 C15 120.2(13) . . ? C16 C17 C18 119.2(13) . . ? C13 C18 C17 123.8(12) . . ? C24 C19 C20 117.8(10) . . ? C24 C19 P2 120.9(8) . . ? C20 C19 P2 121.3(9) . . ? C19 C20 C21 119.8(13) . . ? C22 C21 C20 122.0(13) . . ? C21 C22 C23 119.8(12) . . ? C22 C23 C24 118.5(12) . . ? C19 C24 C23 122.1(11) . . ? C26 C25 P1 108.4(7) . . ? C25 C26 P2 108.2(7) . . ? N1 C27 N2A 174(2) . . ? N1 C27 N2B 150(2) . . ? N2A C27 N2B 36.1(15) . . ? N1' Mo1' N1' 180.0(5) . 5_556 ? N1' Mo1' P1' 93.1(3) . 5_556 ? N1' Mo1' P1' 86.9(3) 5_556 5_556 ? N1' Mo1' P1' 86.9(3) . . ? N1' Mo1' P1' 93.1(3) 5_556 . ? P1' Mo1' P1' 180.000(1) 5_556 . ? N1' Mo1' P2' 88.9(3) . . ? N1' Mo1' P2' 91.1(3) 5_556 . ? P1' Mo1' P2' 100.19(9) 5_556 . ? P1' Mo1' P2' 79.81(9) . . ? N1' Mo1' P2' 91.1(3) . 5_556 ? N1' Mo1' P2' 88.9(3) 5_556 5_556 ? P1' Mo1' P2' 79.81(9) 5_556 5_556 ? P1' Mo1' P2' 100.19(9) . 5_556 ? P2' Mo1' P2' 180.00(11) . 5_556 ? C7' P1' C1' 105.0(5) . . ? C7' P1' C25' 106.0(6) . . ? C1' P1' C25' 102.2(5) . . ? C7' P1' Mo1' 116.0(4) . . ? C1' P1' Mo1' 120.7(4) . . ? C25' P1' Mo1' 105.2(4) . . ? C19' P2' C13' 103.0(5) . . ? C19' P2' C26' 104.5(5) . . ? C13' P2' C26' 101.4(5) . . ? C19' P2' Mo1' 115.0(4) . . ? C13' P2' Mo1' 123.2(4) . . ? C26' P2' Mo1' 107.6(4) . . ? C27' N1' Mo1' 174.2(12) . . ? N2'B N2'A C27' 86(4) . . ? N2'A N2'B C27' 61(3) . . ? C2' C1' C6' 119.4(12) . . ? C2' C1' P1' 120.3(10) . . ? C6' C1' P1' 120.2(9) . . ? C1' C2' C3' 118.7(13) . . ? C4' C3' C2' 121.2(14) . . ? C5' C4' C3' 120.9(15) . . ? C4' C5' C6' 121.0(14) . . ? C1' C6' C5' 118.7(13) . . ? C12' C7' C8' 119.8(11) . . ? C12' C7' P1' 121.9(11) . . ? C8' C7' P1' 118.3(10) . . ? C7' C8' C9' 120.2(13) . . ? C10' C9' C8' 116.4(14) . . ? C11' C10' C9' 121.7(14) . . ? C10' C11' C12' 121.0(15) . . ? C11' C12' C7' 120.9(14) . . ? C18' C13' C14' 119.4(11) . . ? C18' C13' P2' 121.8(9) . . ? C14' C13' P2' 118.8(10) . . ? C15' C14' C13' 120.1(12) . . ? C16' C15' C14' 119.7(13) . . ? C17' C16' C15' 120.5(13) . . ? C16' C17' C18' 121.2(13) . . ? C13' C18' C17' 119.1(12) . . ? C24' C19' C20' 118.3(11) . . ? C24' C19' P2' 121.8(10) . . ? C20' C19' P2' 119.7(9) . . ? C21' C20' C19' 120.6(12) . . ? C22' C21' C20' 119.9(13) . . ? C21' C22' C23' 121.3(12) . . ? C22' C23' C24' 119.2(13) . . ? C19' C24' C23' 120.7(12) . . ? C26' C25' P1' 110.0(8) . . ? C25' C26' P2' 113.1(8) . . ? N1' C27' N2'A 164(2) . . ? N1' C27' N2'B 163(2) . . ? N2'A C27' N2'B 32.8(15) . . ? F3 B F1 112(3) . . ? F3 B F2 117(3) . . ? F1 B F2 112(3) . . ? F3 B F4 109(3) . . ? F1 B F4 111(2) . . ? F2 B F4 95(2) . . ? Cl2 C1D Cl1 113.9(17) . . ? _diffrn_measured_fraction_theta_max 0.727 _diffrn_reflns_theta_full 50.06 _diffrn_measured_fraction_theta_full 0.727 _refine_diff_density_max 0.969 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.096 #===END data_pmb03 _database_code_CSD 171673 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H53 B F4 Mo N4 O P4' _chemical_formula_weight 1104.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.778(2) _cell_length_b 21.290(4) _cell_length_c 22.115(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.85(3) _cell_angle_gamma 90.00 _cell_volume 5544.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.2 _cell_measurement_theta_max 12.8 _exptl_crystal_description prism _exptl_crystal_colour dark_brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8673 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator filter _diffrn_measurement_device_type CAD4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 100 _diffrn_standards_decay_% 2 _diffrn_reflns_number 7930 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.46 _reflns_number_total 2003 _reflns_number_gt 2003 _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^)+(0.1112P)^2^+7.0505P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2003 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.773 _refine_ls_shift/su_mean 0.086 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 0.23399(11) 0.12955(6) 0.33598(7) 0.0439(5) Uani 1 1 d . . . P1 P 0.0814(3) 0.09947(19) 0.4133(2) 0.0486(12) Uani 1 1 d . . . P2 P 0.1735(3) 0.02196(19) 0.2963(2) 0.0486(12) Uani 1 1 d . . . P3 P 0.3902(3) 0.1579(2) 0.2615(2) 0.0506(12) Uani 1 1 d . . . P4 P 0.2633(4) 0.24502(19) 0.3610(2) 0.0497(13) Uani 1 1 d . . . N1 N 0.1129(13) 0.1602(7) 0.2753(9) 0.052(5) Uani 1 1 d . . . N2 N -0.020(2) 0.1970(12) 0.2070(13) 0.175(11) Uani 1 1 d . . . N3 N 0.3449(10) 0.1047(6) 0.3876(6) 0.055(4) Uani 1 1 d . . . N4 N 0.5030(13) 0.0749(10) 0.4580(10) 0.128(8) Uani 1 1 d . . . C1 C 0.1337(13) 0.0947(8) 0.4917(8) 0.049(4) Uani 1 1 d . . . C2 C 0.2180(13) 0.0507(8) 0.5060(9) 0.056(5) Uani 1 1 d . . . C3 C 0.2640(14) 0.0485(10) 0.5612(13) 0.074(6) Uani 1 1 d . . . C4 C 0.2288(17) 0.0847(12) 0.6062(10) 0.077(6) Uani 1 1 d . . . C5 C 0.1453(16) 0.1305(10) 0.5932(10) 0.078(5) Uani 1 1 d . . . C6 C 0.0993(13) 0.1345(8) 0.5367(9) 0.061(5) Uani 1 1 d . . . C7 C -0.0555(12) 0.1405(8) 0.4204(7) 0.053(5) Uani 1 1 d . . . C8 C -0.0816(13) 0.1924(8) 0.3861(9) 0.061(5) Uani 1 1 d . . . C9 C -0.1867(17) 0.2223(9) 0.3929(10) 0.081(6) Uani 1 1 d . . . C10 C -0.2647(14) 0.1969(10) 0.4338(11) 0.072(6) Uani 1 1 d . . . C11 C -0.2404(15) 0.1469(10) 0.4668(10) 0.075(6) Uani 1 1 d . . . C12 C -0.1363(14) 0.1155(7) 0.4600(8) 0.067(5) Uani 1 1 d . . . C13 C 0.1571(16) 0.0067(8) 0.2176(9) 0.061(5) Uani 1 1 d . . . C14 C 0.0650(19) 0.0253(11) 0.1862(11) 0.091(7) Uani 1 1 d . . . C15 C 0.050(2) 0.0186(16) 0.1237(17) 0.130(11) Uani 1 1 d . . . C16 C 0.131(4) -0.0137(15) 0.0941(13) 0.151(14) Uani 1 1 d . . . C17 C 0.231(3) -0.0334(11) 0.1260(17) 0.119(9) Uani 1 1 d . . . C18 C 0.240(2) -0.0230(11) 0.1870(14) 0.103(7) Uani 1 1 d . . . C19 C 0.2540(13) -0.0467(7) 0.3233(8) 0.060(5) Uani 1 1 d . . . C20 C 0.2009(14) -0.1035(9) 0.3321(8) 0.066(5) Uani 1 1 d . . . C21 C 0.267(2) -0.1535(8) 0.3545(10) 0.090(7) Uani 1 1 d . . . C22 C 0.380(3) -0.1471(11) 0.3652(13) 0.126(10) Uani 1 1 d . . . C23 C 0.4274(19) -0.0904(12) 0.3595(14) 0.143(12) Uani 1 1 d . . . C24 C 0.3685(15) -0.0413(8) 0.3363(11) 0.094(8) Uani 1 1 d . . . C25 C 0.0380(12) 0.0192(7) 0.3959(9) 0.059(5) Uani 1 1 d . . . C26 C 0.0328(12) 0.0107(7) 0.3260(9) 0.060(5) Uani 1 1 d . . . C27 C 0.3629(15) 0.1697(8) 0.1810(9) 0.060(5) Uani 1 1 d . . . C28 C 0.2667(16) 0.1467(8) 0.1530(10) 0.068(6) Uani 1 1 d . . . C29 C 0.2512(18) 0.1531(11) 0.0907(12) 0.093(7) Uani 1 1 d . . . C30 C 0.327(3) 0.1860(13) 0.0568(11) 0.105(8) Uani 1 1 d . . . C31 C 0.424(2) 0.2060(11) 0.0859(15) 0.109(9) Uani 1 1 d . . . C32 C 0.4450(19) 0.1993(9) 0.1477(11) 0.081(6) Uani 1 1 d . . . C33 C 0.5153(12) 0.1077(7) 0.2647(8) 0.052(5) Uani 1 1 d . . . C34 C 0.5274(17) 0.0603(10) 0.2220(11) 0.093(7) Uani 1 1 d . . . C35 C 0.622(2) 0.0209(9) 0.2230(12) 0.108(8) Uani 1 1 d . . . C36 C 0.7037(17) 0.0290(9) 0.2682(11) 0.081(6) Uani 1 1 d . . . C37 C 0.6935(15) 0.0739(11) 0.3072(10) 0.084(6) Uani 1 1 d . . . C38 C 0.5994(15) 0.1133(9) 0.3074(8) 0.078(6) Uani 1 1 d . . . C39 C 0.3499(12) 0.2608(8) 0.4298(8) 0.050(5) Uani 1 1 d . . . C40 C 0.3363(16) 0.2240(9) 0.4789(10) 0.078(6) Uani 1 1 d . . . C41 C 0.397(2) 0.2354(11) 0.5328(11) 0.106(8) Uani 1 1 d . . . C42 C 0.4714(18) 0.2871(12) 0.5350(12) 0.097(7) Uani 1 1 d . . . C43 C 0.4850(18) 0.3201(10) 0.4848(12) 0.091(8) Uani 1 1 d . . . C44 C 0.4255(16) 0.3111(9) 0.4311(10) 0.079(6) Uani 1 1 d . . . C45 C 0.1423(13) 0.2987(7) 0.3682(10) 0.053(5) Uani 1 1 d . . . C46 C 0.1065(17) 0.3181(10) 0.4236(10) 0.078(6) Uani 1 1 d . . . C47 C 0.011(2) 0.3551(9) 0.4277(11) 0.085(7) Uani 1 1 d . . . C48 C -0.0449(18) 0.3750(10) 0.3765(16) 0.103(8) Uani 1 1 d . . . C49 C -0.0113(17) 0.3555(9) 0.3212(11) 0.083(6) Uani 1 1 d . . . C50 C 0.0846(16) 0.3178(9) 0.3159(10) 0.078(6) Uani 1 1 d . . . C51 C 0.4456(13) 0.2354(8) 0.2854(9) 0.069(6) Uani 1 1 d . . . C52 C 0.3462(15) 0.2784(8) 0.3000(8) 0.067(5) Uani 1 1 d . . . C53 C 0.058(2) 0.1773(9) 0.2518(13) 0.072(8) Uani 1 1 d . . . C54 C 0.4269(17) 0.0897(10) 0.4243(9) 0.078(6) Uani 1 1 d . . . C55 C -0.132(3) 0.2340(18) 0.2096(17) 0.235(14) Uiso 1 1 d . . . C56 C -0.220(3) 0.1961(18) 0.1846(19) 0.276(16) Uiso 1 1 d . . . O1W O 0.245(3) 0.4034(17) 0.5617(16) 0.211(13) Uiso 0.70 1 d P . . O1W' O 0.084(4) 0.469(2) 0.551(2) 0.129(18) Uiso 0.30 1 d P . . B B -0.354(3) 0.367(2) 0.290(2) 0.149(12) Uiso 1 1 d . . . F1 F -0.4391(18) 0.3678(11) 0.2408(12) 0.121(8) Uiso 0.63(3) 1 d P . . F2 F -0.3747(19) 0.3371(11) 0.3407(12) 0.117(8) Uiso 0.63(3) 1 d P . . F3 F -0.255(2) 0.3699(13) 0.2526(11) 0.132(10) Uiso 0.63(3) 1 d P . . F4 F -0.330(2) 0.4257(13) 0.3266(14) 0.172(13) Uiso 0.63(3) 1 d P . . F1' F -0.340(2) 0.3131(14) 0.3127(16) 0.068(10) Uiso 0.37(3) 1 d P . . F2' F -0.285(5) 0.407(3) 0.276(3) 0.20(2) Uiso 0.37(3) 1 d P . . F3' F -0.458(2) 0.3891(13) 0.2751(15) 0.073(11) Uiso 0.37(3) 1 d P . . F4' F -0.322(4) 0.308(3) 0.245(3) 0.19(2) Uiso 0.37(3) 1 d P . . H2A H 0.2435 0.0233 0.4743 0.120 Uiso 1 1 d . . . H3A H 0.3218 0.0173 0.5710 0.120 Uiso 1 1 d . . . H4A H 0.2597 0.0847 0.6460 0.120 Uiso 1 1 d . . . H5A H 0.1193 0.1581 0.6243 0.120 Uiso 1 1 d . . . H6A H 0.0410 0.1641 0.5276 0.120 Uiso 1 1 d . . . H8A H -0.0277 0.2078 0.3592 0.120 Uiso 1 1 d . . . H9A H -0.2019 0.2574 0.3688 0.120 Uiso 1 1 d . . . H10A H -0.3340 0.2187 0.4361 0.120 Uiso 1 1 d . . . H11A H -0.2920 0.1304 0.4937 0.120 Uiso 1 1 d . . . H12A H -0.1178 0.0808 0.4840 0.120 Uiso 1 1 d . . . H14A H 0.0042 0.0479 0.2072 0.120 Uiso 1 1 d . . . H15A H -0.0151 0.0316 0.1038 0.120 Uiso 1 1 d . . . H16A H 0.1269 -0.0197 0.0515 0.120 Uiso 1 1 d . . . H17A H 0.2882 -0.0547 0.1027 0.120 Uiso 1 1 d . . . H18A H 0.3075 -0.0385 0.2061 0.120 Uiso 1 1 d . . . H20A H 0.1239 -0.1091 0.3231 0.120 Uiso 1 1 d . . . H21A H 0.2279 -0.1938 0.3598 0.120 Uiso 1 1 d . . . H22A H 0.4200 -0.1824 0.3818 0.120 Uiso 1 1 d . . . H23A H 0.5081 -0.0862 0.3671 0.120 Uiso 1 1 d . . . H24A H 0.4041 -0.0015 0.3304 0.120 Uiso 1 1 d . . . H25A H -0.0347 0.0105 0.4129 0.120 Uiso 1 1 d . . . H25B H 0.0921 -0.0101 0.4131 0.120 Uiso 1 1 d . . . H26A H 0.0049 -0.0304 0.3165 0.120 Uiso 1 1 d . . . H26B H -0.0191 0.0411 0.3091 0.120 Uiso 1 1 d . . . H28A H 0.2105 0.1251 0.1771 0.120 Uiso 1 1 d . . . H29A H 0.1828 0.1376 0.0737 0.120 Uiso 1 1 d . . . H30A H 0.3186 0.1889 0.0169 0.120 Uiso 1 1 d . . . H31A H 0.4820 0.2275 0.0635 0.120 Uiso 1 1 d . . . H32A H 0.5096 0.2149 0.1669 0.120 Uiso 1 1 d . . . H34A H 0.4729 0.0548 0.1904 0.120 Uiso 1 1 d . . . H35A H 0.6303 -0.0107 0.1935 0.120 Uiso 1 1 d . . . H36A H 0.7680 0.0022 0.2686 0.120 Uiso 1 1 d . . . H37A H 0.7482 0.0805 0.3406 0.120 Uiso 1 1 d . . . H38A H 0.5908 0.1460 0.3375 0.120 Uiso 1 1 d . . . H40A H 0.2841 0.1895 0.4779 0.120 Uiso 1 1 d . . . H41A H 0.3850 0.2098 0.5666 0.120 Uiso 1 1 d . . . H42A H 0.5119 0.2931 0.5710 0.120 Uiso 1 1 d . . . H43A H 0.5378 0.3561 0.4867 0.120 Uiso 1 1 d . . . H44A H 0.4369 0.3357 0.3980 0.120 Uiso 1 1 d . . . H46A H 0.1447 0.3050 0.4584 0.120 Uiso 1 1 d . . . H47A H -0.0147 0.3684 0.4658 0.120 Uiso 1 1 d . . . H48A H -0.1117 0.4000 0.3789 0.120 Uiso 1 1 d . . . H49A H -0.0492 0.3683 0.2847 0.120 Uiso 1 1 d . . . H50A H 0.1103 0.3050 0.2774 0.120 Uiso 1 1 d . . . H51A H 0.4881 0.2533 0.2518 0.120 Uiso 1 1 d . . . H51B H 0.4950 0.2311 0.3189 0.120 Uiso 1 1 d . . . H52A H 0.3726 0.3194 0.3114 0.120 Uiso 1 1 d . . . H52B H 0.2965 0.2839 0.2646 0.120 Uiso 1 1 d . . . H55A H -0.1171 0.2705 0.1873 0.120 Uiso 1 1 d . . . H55B H -0.1433 0.2421 0.2498 0.120 Uiso 1 1 d . . . H56A H -0.2906 0.2320 0.1880 0.120 Uiso 1 1 d . . . H56B H -0.2170 0.1943 0.1420 0.120 Uiso 1 1 d . . . H56C H -0.2436 0.1655 0.2055 0.120 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0329(8) 0.0361(8) 0.0627(11) 0.0021(9) -0.0031(6) -0.0040(8) P1 0.036(3) 0.039(2) 0.071(4) 0.003(2) 0.005(2) -0.003(2) P2 0.034(2) 0.041(3) 0.070(4) -0.005(2) -0.005(2) -0.004(2) P3 0.039(3) 0.049(3) 0.064(3) 0.005(3) 0.002(2) -0.007(2) P4 0.047(3) 0.037(3) 0.065(4) 0.008(2) -0.001(2) -0.005(2) N1 0.035(10) 0.034(10) 0.087(14) 0.003(9) -0.009(9) 0.028(7) N2 0.15(2) 0.20(3) 0.17(3) -0.01(2) -0.002(19) 0.10(2) N3 0.044(8) 0.049(8) 0.072(11) 0.014(8) -0.023(8) 0.001(6) N4 0.043(11) 0.17(2) 0.17(2) 0.045(16) -0.039(12) 0.005(11) C1 0.054(11) 0.041(9) 0.051(13) 0.007(10) -0.008(9) -0.009(9) C2 0.038(10) 0.075(13) 0.054(13) 0.036(11) 0.003(9) -0.017(9) C3 0.042(11) 0.089(15) 0.093(19) 0.027(15) 0.019(13) 0.002(10) C4 0.045(12) 0.118(18) 0.066(16) 0.051(15) -0.009(11) -0.024(12) C5 0.068(13) 0.093(15) 0.073(16) -0.015(14) 0.002(11) -0.034(14) C6 0.064(11) 0.057(11) 0.061(14) 0.002(12) -0.024(11) -0.016(10) C7 0.042(9) 0.064(12) 0.052(12) 0.016(10) 0.002(9) -0.005(9) C8 0.040(10) 0.068(12) 0.076(15) 0.007(11) -0.008(9) 0.020(9) C9 0.065(14) 0.069(13) 0.110(19) 0.007(13) -0.013(13) 0.025(11) C10 0.034(11) 0.085(16) 0.097(19) -0.037(14) -0.006(12) 0.017(11) C11 0.042(11) 0.095(17) 0.090(17) -0.025(14) 0.013(11) -0.005(11) C12 0.060(12) 0.059(13) 0.080(14) -0.003(11) 0.013(11) -0.002(9) C13 0.044(12) 0.049(11) 0.090(16) 0.016(11) -0.017(11) 0.004(9) C14 0.077(16) 0.123(19) 0.072(17) -0.040(16) 0.010(14) -0.010(14) C15 0.11(2) 0.16(3) 0.13(3) -0.03(2) -0.03(2) -0.022(18) C16 0.28(5) 0.10(2) 0.07(2) -0.018(17) -0.05(3) -0.04(3) C17 0.17(3) 0.072(17) 0.12(3) -0.024(18) 0.03(2) 0.007(17) C18 0.13(2) 0.082(16) 0.10(2) -0.004(16) -0.009(18) 0.013(15) C19 0.045(11) 0.046(12) 0.088(15) 0.011(10) -0.006(10) 0.004(9) C20 0.068(12) 0.047(11) 0.083(15) 0.007(11) -0.010(11) -0.009(9) C21 0.16(2) 0.027(11) 0.079(17) -0.006(11) 0.004(16) -0.012(14) C22 0.13(2) 0.060(16) 0.18(3) 0.030(16) -0.08(2) 0.017(15) C23 0.102(19) 0.072(17) 0.25(4) -0.01(2) -0.07(2) 0.039(17) C24 0.055(13) 0.044(12) 0.18(2) 0.003(13) -0.030(14) 0.006(10) C25 0.048(11) 0.028(9) 0.101(16) 0.009(10) 0.027(10) -0.011(8) C26 0.040(10) 0.045(10) 0.096(17) -0.014(11) 0.006(10) -0.010(8) C27 0.047(12) 0.058(12) 0.076(16) 0.014(11) 0.020(12) 0.018(9) C28 0.051(12) 0.075(14) 0.079(17) -0.018(12) -0.006(11) 0.011(10) C29 0.079(16) 0.12(2) 0.079(18) 0.007(16) -0.020(14) 0.016(13) C30 0.11(2) 0.12(2) 0.08(2) 0.034(17) -0.003(18) 0.026(17) C31 0.10(2) 0.099(19) 0.13(3) 0.014(18) 0.030(19) -0.012(15) C32 0.123(19) 0.080(15) 0.042(15) 0.012(12) 0.002(14) -0.008(13) C33 0.023(9) 0.052(12) 0.080(14) 0.002(10) 0.008(9) 0.003(7) C34 0.075(14) 0.060(13) 0.14(2) -0.014(15) -0.038(14) 0.001(12) C35 0.098(17) 0.056(13) 0.17(3) -0.026(14) -0.032(18) 0.012(12) C36 0.075(15) 0.055(13) 0.114(19) -0.016(14) 0.002(14) 0.008(11) C37 0.049(12) 0.105(18) 0.097(17) -0.008(14) -0.012(11) 0.020(12) C38 0.050(11) 0.116(18) 0.067(13) -0.021(13) -0.006(10) -0.005(12) C39 0.042(10) 0.041(10) 0.067(14) 0.011(10) 0.000(9) -0.004(8) C40 0.083(14) 0.079(15) 0.071(16) 0.000(13) -0.008(13) -0.033(11) C41 0.122(19) 0.103(18) 0.092(19) 0.013(15) -0.021(16) -0.043(15) C42 0.088(17) 0.12(2) 0.08(2) -0.012(17) -0.028(15) -0.020(14) C43 0.102(17) 0.084(16) 0.09(2) 0.019(14) -0.031(16) -0.044(13) C44 0.072(13) 0.082(14) 0.082(17) 0.002(12) -0.036(12) -0.016(11) C45 0.043(11) 0.046(11) 0.072(16) 0.009(10) 0.010(11) 0.000(8) C46 0.072(14) 0.071(14) 0.091(19) 0.004(13) 0.022(13) -0.005(11) C47 0.100(18) 0.054(14) 0.10(2) -0.003(13) 0.034(15) 0.007(12) C48 0.084(15) 0.063(14) 0.16(3) 0.005(17) 0.043(18) 0.043(12) C49 0.072(14) 0.061(14) 0.11(2) 0.006(13) 0.008(13) 0.023(11) C50 0.065(13) 0.070(13) 0.097(19) 0.002(13) -0.030(13) 0.003(11) C51 0.046(11) 0.052(11) 0.109(17) -0.031(11) 0.027(11) -0.013(9) C52 0.090(14) 0.045(11) 0.066(14) 0.012(10) -0.008(12) -0.022(10) C53 0.08(2) 0.030(13) 0.11(3) -0.017(14) 0.035(18) 0.014(12) C54 0.052(13) 0.109(16) 0.075(15) 0.047(13) 0.027(12) -0.029(12) _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 N3 1.801(12) . ? Mo N1 2.050(16) . ? Mo P4 2.542(4) . ? Mo P2 2.550(4) . ? Mo P3 2.560(5) . ? Mo P1 2.579(5) . ? P1 C25 1.823(15) . ? P1 C1 1.835(17) . ? P1 C7 1.843(16) . ? P2 C13 1.78(2) . ? P2 C26 1.807(16) . ? P2 C19 1.837(16) . ? P3 C27 1.82(2) . ? P3 C33 1.820(15) . ? P3 C51 1.849(16) . ? P4 C52 1.822(18) . ? P4 C45 1.836(17) . ? P4 C39 1.850(17) . ? N1 C53 0.90(3) . ? N2 C53 1.41(3) . ? N2 C55 1.54(4) . ? N3 C54 1.29(2) . ? N4 C54 1.20(2) . ? C1 C6 1.37(2) . ? C1 C2 1.40(2) . ? C2 C3 1.33(2) . ? C3 C4 1.33(3) . ? C4 C5 1.41(3) . ? C5 C6 1.36(2) . ? C7 C8 1.37(2) . ? C7 C12 1.41(2) . ? C8 C9 1.40(2) . ? C9 C10 1.41(3) . ? C10 C11 1.32(2) . ? C11 C12 1.41(2) . ? C13 C18 1.35(3) . ? C13 C14 1.34(2) . ? C14 C15 1.40(3) . ? C15 C16 1.36(4) . ? C16 C17 1.43(4) . ? C17 C18 1.37(3) . ? C19 C24 1.38(2) . ? C19 C20 1.38(2) . ? C20 C21 1.40(2) . ? C21 C22 1.36(3) . ? C22 C23 1.34(3) . ? C23 C24 1.35(3) . ? C25 C26 1.56(2) . ? C27 C32 1.38(2) . ? C27 C28 1.37(2) . ? C28 C29 1.39(3) . ? C29 C30 1.37(3) . ? C30 C31 1.36(3) . ? C31 C32 1.39(3) . ? C33 C38 1.36(2) . ? C33 C34 1.39(2) . ? C34 C35 1.39(3) . ? C35 C36 1.39(3) . ? C36 C37 1.29(2) . ? C37 C38 1.39(2) . ? C39 C40 1.35(2) . ? C39 C44 1.39(2) . ? C40 C41 1.40(3) . ? C41 C42 1.41(3) . ? C42 C43 1.33(3) . ? C43 C44 1.38(3) . ? C45 C46 1.37(3) . ? C45 C50 1.39(2) . ? C46 C47 1.38(3) . ? C47 C48 1.37(3) . ? C48 C49 1.36(3) . ? C49 C50 1.39(2) . ? C51 C52 1.52(2) . ? C55 C56 1.42(4) . ? B F2' 1.22(6) . ? B F1' 1.26(5) . ? B F2 1.31(4) . ? B F3' 1.35(4) . ? B F3 1.44(5) . ? B F1 1.47(4) . ? B F4 1.51(5) . ? B F4' 1.64(6) . ? F1 F3' 0.91(3) . ? F2 F1' 0.90(3) . ? F3 F2' 1.00(6) . ? F3 F4' 1.54(5) . ? F4 F2' 1.32(6) . ? 1' F4' 1.51(6) . ? 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 N3 Mo N1 177.5(7) . . ? N3 Mo P4 92.9(4) . . ? N1 Mo P4 85.8(5) . . ? N3 Mo P2 98.7(4) . . ? N1 Mo P2 82.7(5) . . ? P4 Mo P2 168.42(15) . . ? N3 Mo P3 87.5(4) . . ? N1 Mo P3 90.2(5) . . ? P4 Mo P3 79.37(15) . . ? P2 Mo P3 100.98(15) . . ? N3 Mo P1 90.7(4) . . ? N1 Mo P1 91.6(5) . . ? P4 Mo P1 100.92(15) . . ? P2 Mo P1 79.10(14) . . ? P3 Mo P1 178.19(16) . . ? C25 P1 C1 103.7(8) . . ? C25 P1 C7 102.7(7) . . ? C1 P1 C7 103.1(8) . . ? C25 P1 Mo 106.8(6) . . ? C1 P1 Mo 114.4(5) . . ? C7 P1 Mo 123.9(5) . . ? C13 P2 C26 104.1(9) . . ? C13 P2 C19 102.7(9) . . ? C26 P2 C19 104.4(8) . . ? C13 P2 Mo 121.8(6) . . ? C26 P2 Mo 104.3(5) . . ? C19 P2 Mo 117.6(6) . . ? C27 P3 C33 104.5(8) . . ? C27 P3 C51 102.3(9) . . ? C33 P3 C51 103.3(7) . . ? C27 P3 Mo 122.9(6) . . ? C33 P3 Mo 115.2(5) . . ? C51 P3 Mo 106.3(6) . . ? C52 P4 C45 104.3(9) . . ? C52 P4 C39 104.1(8) . . ? C45 P4 C39 103.6(9) . . ? C52 P4 Mo 106.7(6) . . ? C45 P4 Mo 121.2(5) . . ? C39 P4 Mo 115.2(5) . . ? C53 N1 Mo 173(3) . . ? C53 N2 C55 133(3) . . ? C54 N3 Mo 177.0(13) . . ? C6 C1 C2 117.8(15) . . ? C6 C1 P1 123.5(14) . . ? C2 C1 P1 118.6(14) . . ? C3 C2 C1 120.6(18) . . ? C2 C3 C4 122.7(19) . . ? C3 C4 C5 118.2(18) . . ? C6 C5 C4 119.8(19) . . ? C5 C6 C1 120.7(17) . . ? C8 C7 C12 120.0(15) . . ? C8 C7 P1 121.6(12) . . ? C12 C7 P1 118.4(13) . . ? C7 C8 C9 119.8(17) . . ? C8 C9 C10 118.7(17) . . ? C11 C10 C9 121.9(16) . . ? C10 C11 C12 120.4(18) . . ? C11 C12 C7 119.1(17) . . ? C18 C13 C14 118(2) . . ? C18 C13 P2 120.4(17) . . ? C14 C13 P2 121.9(18) . . ? C13 C14 C15 125(2) . . ? C16 C15 C14 117(3) . . ? C15 C16 C17 120(3) . . ? C18 C17 C16 119(3) . . ? C13 C18 C17 121(2) . . ? C24 C19 C20 119.3(15) . . ? C24 C19 P2 119.9(13) . . ? C20 C19 P2 120.8(13) . . ? C19 C20 C21 117.7(16) . . ? C22 C21 C20 121.5(17) . . ? C23 C22 C21 119.0(18) . . ? C22 C23 C24 121(2) . . ? C23 C24 C19 120.6(18) . . ? C26 C25 P1 109.0(11) . . ? C25 C26 P2 108.8(10) . . ? C32 C27 C28 120.3(19) . . ? C32 C27 P3 118.0(17) . . ? C28 C27 P3 121.6(16) . . ? C27 C28 C29 120(2) . . ? C30 C29 C28 121(2) . . ? C31 C30 C29 117(2) . . ? C30 C31 C32 125(2) . . ? C27 C32 C31 117(2) . . ? C38 C33 C34 116.9(15) . . ? C38 C33 P3 123.7(14) . . ? C34 C33 P3 119.4(14) . . ? C35 C34 C33 121.0(18) . . ? C34 C35 C36 119(2) . . ? C37 C36 C35 120.2(19) . . ? C36 C37 C38 122.0(19) . . ? C33 C38 C37 121.1(17) . . ? C40 C39 C44 120.8(16) . . ? C40 C39 P4 119.1(13) . . ? C44 C39 P4 120.0(14) . . ? C39 C40 C41 121.2(17) . . ? C42 C41 C40 118(2) . . ? C43 C42 C41 118(2) . . ? C42 C43 C44 125.4(19) . . ? C39 C44 C43 116.1(17) . . ? C46 C45 C50 120.2(17) . . ? C46 C45 P4 121.1(17) . . ? C50 C45 P4 118.7(16) . . ? C47 C46 C45 120(2) . . ? C48 C47 C46 120(2) . . ? C49 C48 C47 120.5(18) . . ? C48 C49 C50 120(2) . . ? C45 C50 C49 119(2) . . ? C52 C51 P3 109.1(11) . . ? C51 C52 P4 110.2(12) . . ? N1 C53 N2 170(3) . . ? N4 C54 N3 179(3) . . ? C56 C55 N2 108(3) . . ? F2' B F1' 131(5) . . ? F2' B F2 134(5) . . ? F1' B F2 41(2) . . ? F2' B F3' 107(5) . . ? F1' B F3' 121(4) . . ? F2 B F3' 101(3) . . ? F2' B F3 43(3) . . ? F1' B F3 100(4) . . ? F2 B F3 133(4) . . ? F3' B F3 125(4) . . ? F2' B F1 104(4) . . ? F1' B F1 113(4) . . ? F2 B F1 120(3) . . ? F3' B F1 37.4(16) . . ? F3 B F1 97(3) . . ? F2' B F4 57(4) . . ? F1' B F4 121(4) . . ? F2 B F4 89(3) . . ? F3' B F4 90(3) . . ? F3 B F4 98(3) . . ? F1 B F4 120(3) . . ? F2' B F4' 103(5) . . ? F1' B F4' 61(3) . . ? F2 B F4' 101(4) . . ? F3' B F4' 109(4) . . ? F3 B F4' 60(3) . . ? F1 B F4' 74(3) . . ? F4 B F4' 156(4) . . ? F3' F1 B 64(3) . . ? F1' F2 B 66(3) . . ? F2' F3 B 56(4) . . ? F2' F3 F4' 122(5) . . ? B F3 F4' 67(3) . . ? F2' F4 B 50(3) . . ? F2 F1' B 73(3) . . ? F2 F1' F4' 142(4) . . ? B F1' F4' 72(3) . . ? F3 F2' B 80(5) . . ? F3 F2' F4 145(7) . . ? B F2' F4 73(5) . . ? F1 F3' B 79(3) . . ? F1' F4' F3 85(3) . . ? F1' F4' B 47(2) . . ? F3 F4' B 54(3) . . ? _diffrn_measured_fraction_theta_max 0.278 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.278 _refine_diff_density_max 0.543 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.074