# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1509 data_global _publ_contact_author m.g.b.drew _publ_contact_author_email m.g.b.drew@reading.ac.uk _publ_contact_author_fax '0118 931 6310' _publ_contact_author_phone '0118 931 8789' data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Mo(CO)(NCMe)(MeCCMe)I2(P(OPh)3) _chemical_formula_sum 'C25 H24 I2 Mo N O4 P' _chemical_formula_weight 783.16 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.738(16) _cell_length_b 13.392(15) _cell_length_c 14.581(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.069(10) _cell_angle_gamma 90.00 _cell_volume 2876(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 2.687 _exptl_absorpt_correction_type 'DIFABS (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 1.00 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9497 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.01 _reflns_number_total 9360 _reflns_number_gt 6709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. two molecules in the asymmetric unit. Alternative structures were refined with reversed coordinates and the structure with the lowest R value is reported here. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^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 0.00031(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.34(3) _refine_ls_number_reflns 9360 _refine_ls_number_parameters 620 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1A Mo 0.49890(7) 0.37460(8) 0.18321(7) 0.0400(2) Uani 1 d . . . I2A I 0.62469(7) 0.42650(8) 0.32860(6) 0.0683(3) Uani 1 d . . . I3A I 0.53435(6) 0.17089(7) 0.21715(6) 0.0568(2) Uani 1 d . . . P4A P 0.4935(2) 0.5594(2) 0.1787(2) 0.0391(7) Uani 1 d . . . O51A O 0.5790(6) 0.6267(6) 0.1638(6) 0.049(2) Uani 1 d . . . C52A C 0.6460(8) 0.6145(8) 0.0969(8) 0.040(3) Uani 1 d . . . C53A C 0.6196(10) 0.5993(9) 0.0064(9) 0.050(3) Uani 1 d . . . H53A H 0.5585 0.5937 -0.0111 0.060 Uiso 1 calc R . . C54A C 0.6872(11) 0.5926(11) -0.0586(10) 0.059(4) Uani 1 d . . . H54A H 0.6710 0.5842 -0.1204 0.071 Uiso 1 calc R . . C55A C 0.7765(10) 0.5984(12) -0.0319(12) 0.068(4) Uani 1 d . . . H55A H 0.8210 0.5897 -0.0749 0.082 Uiso 1 calc R . . C56A C 0.8012(10) 0.6171(13) 0.0579(12) 0.071(4) Uani 1 d . . . H56A H 0.8621 0.6252 0.0755 0.085 Uiso 1 calc R . . C57A C 0.7331(10) 0.6239(11) 0.1239(11) 0.062(4) Uani 1 d . . . H57A H 0.7489 0.6348 0.1854 0.074 Uiso 1 calc R . . O61A O 0.4613(6) 0.6085(6) 0.2714(5) 0.044(2) Uani 1 d . . . C62A C 0.4725(9) 0.7068(9) 0.3003(9) 0.052(3) Uani 1 d . . . C63A C 0.4472(14) 0.7890(11) 0.2482(12) 0.084(6) Uani 1 d . . . H63A H 0.4231 0.7799 0.1889 0.100 Uiso 1 calc R . . C64A C 0.4573(15) 0.8867(14) 0.2836(15) 0.103(7) Uani 1 d . . . H64A H 0.4415 0.9415 0.2473 0.124 Uiso 1 calc R . . C65A C 0.4882(14) 0.8994(15) 0.3656(19) 0.107(9) Uani 1 d . . . H65A H 0.4944 0.9641 0.3882 0.128 Uiso 1 calc R . . C66A C 0.5135(11) 0.8175(19) 0.4240(19) 0.125(11) Uani 1 d . . . H66A H 0.5358 0.8296 0.4834 0.150 Uiso 1 calc R . . C67A C 0.5049(9) 0.7187(13) 0.3919(10) 0.067(4) Uani 1 d . . . H67A H 0.5197 0.6643 0.4291 0.080 Uiso 1 calc R . . O71A O 0.4282(5) 0.6106(6) 0.0990(6) 0.047(2) Uani 1 d . . . C72A C 0.3353(9) 0.5989(9) 0.0858(10) 0.050(3) Uani 1 d . . . C73A C 0.2742(9) 0.6149(11) 0.1575(10) 0.059(4) Uani 1 d . . . H73A H 0.2954 0.6293 0.2169 0.071 Uiso 1 calc R . . C74A C 0.1809(11) 0.6082(14) 0.1357(12) 0.076(5) Uani 1 d . . . H74A H 0.1393 0.6215 0.1806 0.091 Uiso 1 calc R . . C75A C 0.1501(12) 0.5818(13) 0.0476(13) 0.077(5) Uani 1 d . . . H75A H 0.0880 0.5760 0.0353 0.092 Uiso 1 calc R . . C76A C 0.2074(11) 0.5646(11) -0.0199(11) 0.065(4) Uani 1 d . . . H76A H 0.1853 0.5461 -0.0780 0.078 Uiso 1 calc R . . C77A C 0.3011(11) 0.5748(11) -0.0021(10) 0.062(4) Uani 1 d . . . H77A H 0.3410 0.5654 -0.0494 0.075 Uiso 1 calc R . . C22A C 0.4501(12) 0.3683(14) -0.0398(9) 0.075(4) Uani 1 d . . . H22A H 0.4032 0.3303 -0.0709 0.090 Uiso 1 calc R . . H22B H 0.5080 0.3380 -0.0496 0.090 Uiso 1 calc R . . H22C H 0.4499 0.4353 -0.0634 0.090 Uiso 1 calc R . . C21A C 0.4338(8) 0.3707(9) 0.0591(8) 0.046(3) Uani 1 d . . . C11A C 0.3699(9) 0.3635(8) 0.1224(10) 0.053(3) Uani 1 d . . . C12A C 0.2729(9) 0.3467(11) 0.1301(14) 0.073(5) Uani 1 d . . . H12A H 0.2451 0.3392 0.0700 0.088 Uiso 1 calc R . . H12B H 0.2463 0.4027 0.1603 0.088 Uiso 1 calc R . . H12C H 0.2633 0.2872 0.1652 0.088 Uiso 1 calc R . . C10A C 0.4098(10) 0.3696(9) 0.2814(10) 0.057(3) Uani 1 d . . . O10A O 0.3565(8) 0.3641(9) 0.3373(8) 0.084(3) Uani 1 d . . . N30A N 0.6216(7) 0.3656(8) 0.0999(7) 0.047(2) Uani 1 d . . . C31A C 0.6828(9) 0.3556(9) 0.0591(9) 0.050(3) Uani 1 d . . . C32A C 0.7647(10) 0.3362(12) 0.0056(11) 0.066(4) Uani 1 d . . . H32A H 0.8180 0.3433 0.0449 0.080 Uiso 1 calc R . . H32B H 0.7670 0.3832 -0.0440 0.080 Uiso 1 calc R . . H32C H 0.7620 0.2696 -0.0187 0.080 Uiso 1 calc R . . I3B I 0.95919(6) -0.32982(7) 0.28366(6) 0.0554(2) Uani 1 d . . . Mo1B Mo 0.94911(6) -0.12288(8) 0.31784(7) 0.0404(2) Uani 1 d . . . I2B I 1.02768(7) -0.08241(8) 0.14573(6) 0.0673(3) Uani 1 d . . . P4B P 0.9540(2) 0.0616(2) 0.3208(2) 0.0391(7) Uani 1 d . . . O51B O 0.9181(6) 0.1176(6) 0.4113(6) 0.0455(19) Uani 1 d . . . C52B C 0.8348(8) 0.0978(8) 0.4499(8) 0.040(3) Uani 1 d . . . C53B C 0.8364(10) 0.0753(10) 0.5416(9) 0.053(3) Uani 1 d . . . H53B H 0.8923 0.0711 0.5732 0.064 Uiso 1 calc R . . C54B C 0.7580(11) 0.0584(11) 0.5891(11) 0.065(4) Uani 1 d . . . H54B H 0.7600 0.0415 0.6511 0.078 Uiso 1 calc R . . C55B C 0.6742(12) 0.0682(11) 0.5382(11) 0.069(4) Uani 1 d . . . H55B H 0.6198 0.0573 0.5669 0.082 Uiso 1 calc R . . C56B C 0.6734(10) 0.0932(11) 0.4490(11) 0.064(4) Uani 1 d . . . H56B H 0.6178 0.0994 0.4172 0.077 Uiso 1 calc R . . C57B C 0.7527(9) 0.1101(10) 0.4024(10) 0.053(3) Uani 1 d . . . H57B H 0.7505 0.1291 0.3410 0.064 Uiso 1 calc R . . O61B O 0.9008(5) 0.1146(6) 0.2379(6) 0.0442(19) Uani 1 d . . . C62B C 0.9192(9) 0.2138(10) 0.2107(8) 0.048(3) Uani 1 d . . . C63B C 0.8928(12) 0.3888(13) 0.2170(12) 0.082(5) Uani 1 d . . . H63B H 0.8611 0.4424 0.2408 0.098 Uiso 1 calc R . . C64B C 0.8717(10) 0.2907(10) 0.2462(11) 0.062(4) Uani 1 d . . . H64B H 0.8268 0.2794 0.2881 0.074 Uiso 1 calc R . . C65B C 0.9579(11) 0.4067(14) 0.1555(14) 0.090(6) Uani 1 d . . . H65B H 0.9730 0.4716 0.1394 0.108 Uiso 1 calc R . . C66B C 1.0005(11) 0.3266(14) 0.1181(12) 0.075(5) Uani 1 d . . . H66B H 1.0425 0.3377 0.0731 0.090 Uiso 1 calc R . . C67B C 0.9830(9) 0.2282(11) 0.1453(10) 0.058(4) Uani 1 d . . . H67B H 1.0134 0.1746 0.1201 0.070 Uiso 1 calc R . . O71B O 1.0462(6) 0.1219(7) 0.3162(6) 0.054(2) Uani 1 d . . . C72B C 1.1294(9) 0.1071(8) 0.3650(9) 0.049(3) Uani 1 d . . . C73B C 1.2083(9) 0.1125(11) 0.3174(10) 0.058(4) Uani 1 d . . . H73B H 1.2063 0.1203 0.2540 0.070 Uiso 1 calc R . . C74B C 1.2895(10) 0.1063(14) 0.3654(15) 0.085(5) Uani 1 d . . . H74B H 1.3430 0.1124 0.3339 0.102 Uiso 1 calc R . . C75B C 1.2947(12) 0.0912(13) 0.4595(14) 0.078(5) Uani 1 d . . . H75B H 1.3502 0.0841 0.4913 0.094 Uiso 1 calc R . . C76B C 1.2128(11) 0.0873(12) 0.5040(11) 0.067(4) Uani 1 d . . . H76B H 1.2145 0.0789 0.5674 0.081 Uiso 1 calc R . . C77B C 1.1308(9) 0.0953(9) 0.4597(9) 0.048(3) Uani 1 d . . . H77B H 1.0773 0.0929 0.4915 0.057 Uiso 1 calc R . . C10B C 0.8287(9) -0.1159(10) 0.2467(9) 0.052(3) Uani 1 d . . . O10B O 0.7627(7) -0.1149(10) 0.2049(8) 0.091(4) Uani 1 d . . . N30B N 1.0912(7) -0.1365(7) 0.3657(7) 0.047(2) Uani 1 d . . . C31B C 1.1626(11) -0.1532(10) 0.3904(10) 0.058(4) Uani 1 d . . . C32B C 1.2558(10) -0.1693(12) 0.4237(13) 0.081(5) Uani 1 d . . . H32D H 1.2968 -0.1450 0.3792 0.097 Uiso 1 calc R . . H32E H 1.2659 -0.2393 0.4335 0.097 Uiso 1 calc R . . H32F H 1.2661 -0.1341 0.4805 0.097 Uiso 1 calc R . . C22B C 0.9779(12) -0.1399(11) 0.5436(11) 0.076(5) Uani 1 d . . . H22D H 0.9492 -0.0983 0.5876 0.091 Uiso 1 calc R . . H22E H 1.0399 -0.1195 0.5381 0.091 Uiso 1 calc R . . H22F H 0.9761 -0.2082 0.5635 0.091 Uiso 1 calc R . . C21B C 0.9297(8) -0.1305(9) 0.4544(7) 0.043(3) Uani 1 d . . . C11B C 0.8516(10) -0.1356(9) 0.4122(9) 0.055(3) Uani 1 d . . . C12B C 0.7510(11) -0.1550(11) 0.4227(13) 0.077(5) Uani 1 d . . . H12D H 0.7393 -0.1657 0.4863 0.092 Uiso 1 calc R . . H12E H 0.7333 -0.2132 0.3880 0.092 Uiso 1 calc R . . H12F H 0.7168 -0.0984 0.4005 0.092 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1A 0.0443(6) 0.0356(5) 0.0404(6) -0.0034(4) 0.0050(4) 0.0011(4) I2A 0.0715(7) 0.0701(6) 0.0615(6) -0.0080(5) -0.0218(5) 0.0010(5) I3A 0.0672(6) 0.0409(4) 0.0620(5) 0.0047(4) 0.0011(4) 0.0054(4) P4A 0.0430(18) 0.0323(16) 0.0426(17) 0.0005(12) 0.0104(13) 0.0023(11) O51A 0.053(5) 0.049(5) 0.046(5) -0.013(4) 0.010(4) -0.014(4) C52A 0.045(7) 0.030(6) 0.044(7) 0.010(5) -0.002(5) -0.003(5) C53A 0.060(9) 0.044(7) 0.046(8) 0.004(5) 0.001(6) -0.002(5) C54A 0.075(11) 0.059(9) 0.046(8) 0.011(6) 0.031(7) 0.009(7) C55A 0.051(10) 0.062(10) 0.093(13) 0.021(8) 0.025(8) 0.003(6) C56A 0.038(8) 0.094(12) 0.081(12) 0.003(9) 0.004(7) -0.009(7) C57A 0.060(10) 0.056(9) 0.069(10) 0.010(7) -0.001(7) -0.010(6) O61A 0.056(5) 0.039(5) 0.037(5) -0.011(3) 0.009(4) -0.008(3) C62A 0.052(8) 0.043(7) 0.062(9) -0.015(6) 0.034(6) -0.014(5) C63A 0.142(18) 0.037(9) 0.075(12) -0.001(7) 0.044(11) -0.011(8) C64A 0.156(19) 0.052(11) 0.105(15) -0.023(10) 0.072(14) -0.032(11) C65A 0.087(14) 0.068(15) 0.17(2) -0.072(14) 0.059(14) -0.038(10) C66A 0.035(9) 0.15(2) 0.19(3) -0.12(2) -0.011(12) -0.004(11) C67A 0.042(8) 0.101(12) 0.057(9) -0.037(8) -0.009(6) -0.013(7) O71A 0.043(5) 0.045(5) 0.054(5) 0.005(4) 0.005(4) 0.005(3) C72A 0.043(8) 0.038(7) 0.070(9) 0.008(6) 0.016(6) 0.009(5) C73A 0.052(9) 0.074(10) 0.050(8) 0.013(7) -0.011(6) 0.004(7) C74A 0.053(10) 0.099(13) 0.077(11) 0.007(9) 0.016(8) 0.019(8) C75A 0.061(11) 0.084(12) 0.085(13) 0.019(9) -0.007(9) -0.011(8) C76A 0.068(11) 0.072(10) 0.053(9) 0.007(7) -0.035(8) 0.008(7) C77A 0.078(11) 0.058(9) 0.050(8) -0.010(6) -0.001(7) 0.001(7) C22A 0.098(12) 0.091(11) 0.036(7) -0.014(8) -0.001(7) -0.020(10) C21A 0.066(8) 0.025(6) 0.045(7) -0.006(5) 0.002(6) 0.008(5) C11A 0.074(9) 0.010(6) 0.075(9) 0.002(5) -0.016(7) -0.003(5) C12A 0.040(8) 0.054(10) 0.125(15) 0.009(8) 0.001(8) -0.006(6) C10A 0.077(9) 0.025(6) 0.068(9) -0.007(6) 0.007(7) 0.001(6) O10A 0.086(8) 0.082(8) 0.089(8) -0.001(6) 0.061(6) 0.004(6) N30A 0.050(6) 0.046(6) 0.044(6) 0.002(5) -0.003(5) -0.002(5) C31A 0.047(8) 0.052(8) 0.053(8) -0.004(6) 0.011(6) 0.012(6) C32A 0.054(9) 0.074(10) 0.070(10) -0.003(8) -0.011(7) 0.003(7) I3B 0.0585(5) 0.0417(4) 0.0659(6) -0.0075(4) 0.0009(4) 0.0054(4) Mo1B 0.0392(5) 0.0378(5) 0.0444(6) 0.0016(4) 0.0058(4) 0.0024(4) I2B 0.0782(7) 0.0705(6) 0.0548(5) 0.0033(5) 0.0249(4) 0.0084(5) P4B 0.0335(17) 0.0365(17) 0.0475(18) 0.0044(13) 0.0057(12) -0.0026(11) O51B 0.045(5) 0.044(5) 0.048(5) -0.006(4) 0.013(4) 0.001(3) C52B 0.048(8) 0.034(6) 0.038(7) 0.002(4) -0.003(5) -0.001(5) C53B 0.057(9) 0.049(8) 0.053(8) -0.008(6) -0.007(6) -0.009(6) C54B 0.076(11) 0.051(9) 0.068(10) 0.014(7) 0.016(8) -0.006(7) C55B 0.067(11) 0.064(10) 0.077(11) -0.017(8) 0.030(8) -0.013(7) C56B 0.054(9) 0.067(10) 0.072(10) 0.021(7) -0.003(7) -0.007(7) C57B 0.059(9) 0.049(8) 0.052(8) -0.001(6) 0.014(6) 0.004(6) O61B 0.036(5) 0.038(5) 0.058(5) 0.007(4) -0.007(4) 0.004(3) C62B 0.044(7) 0.056(8) 0.042(7) 0.007(5) -0.010(5) -0.012(6) C63B 0.092(12) 0.068(12) 0.085(12) -0.009(8) -0.011(9) 0.003(9) C64B 0.068(10) 0.033(8) 0.085(11) 0.001(6) 0.028(8) 0.005(6) C65B 0.053(10) 0.088(14) 0.131(16) 0.044(12) 0.023(10) -0.019(9) C66B 0.067(11) 0.093(13) 0.065(11) 0.030(9) 0.019(8) -0.010(9) C67B 0.044(8) 0.064(9) 0.068(10) 0.021(7) 0.015(6) -0.001(6) O71B 0.048(5) 0.060(6) 0.053(5) 0.015(4) -0.007(4) -0.011(4) C72B 0.066(9) 0.020(6) 0.059(8) -0.002(5) -0.001(6) -0.009(5) C73B 0.040(8) 0.068(9) 0.065(9) 0.013(7) -0.005(6) -0.006(6) C74B 0.037(9) 0.098(14) 0.121(16) 0.011(11) 0.017(9) 0.002(8) C75B 0.060(11) 0.067(10) 0.107(15) -0.009(9) -0.013(10) 0.016(7) C76B 0.076(12) 0.063(10) 0.062(10) -0.012(7) -0.003(8) -0.005(7) C77B 0.052(8) 0.038(7) 0.052(8) -0.006(5) -0.003(6) 0.008(5) C10B 0.051(8) 0.037(7) 0.070(9) 0.003(6) 0.018(6) -0.007(6) O10B 0.059(6) 0.120(11) 0.092(8) 0.011(7) -0.040(6) -0.022(7) N30B 0.047(6) 0.030(6) 0.064(7) -0.005(4) 0.009(5) 0.003(4) C31B 0.054(9) 0.058(9) 0.064(9) 0.006(6) 0.011(7) 0.009(6) C32B 0.054(10) 0.067(11) 0.120(16) 0.004(9) -0.022(10) -0.022(7) C22B 0.113(13) 0.045(9) 0.073(11) 0.003(7) 0.032(9) 0.028(8) C21B 0.059(8) 0.037(6) 0.033(6) 0.007(5) 0.002(5) -0.006(6) C11B 0.077(10) 0.027(7) 0.063(8) -0.011(5) 0.032(7) -0.002(6) C12B 0.065(10) 0.053(10) 0.115(15) -0.021(8) 0.041(9) -0.018(7) _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 Mo1A C10A 1.977(15) . ? Mo1A C21A 2.019(12) . ? Mo1A C11A 2.074(13) . ? Mo1A N30A 2.217(11) . ? Mo1A P4A 2.477(4) . ? Mo1A I3A 2.818(3) . ? Mo1A I2A 2.851(3) . ? P4A O51A 1.570(9) . ? P4A O61A 1.590(8) . ? P4A O71A 1.633(9) . ? O51A C52A 1.423(15) . ? C52A C57A 1.335(18) . ? C52A C53A 1.377(17) . ? C53A C54A 1.404(19) . ? C54A C55A 1.36(2) . ? C55A C56A 1.37(2) . ? C56A C57A 1.42(2) . ? O61A C62A 1.391(14) . ? C62A C63A 1.38(2) . ? C62A C67A 1.412(19) . ? C63A C64A 1.41(2) . ? C64A C65A 1.27(3) . ? C65A C66A 1.43(4) . ? C66A C67A 1.41(3) . ? O71A C72A 1.385(16) . ? C72A C77A 1.40(2) . ? C72A C73A 1.42(2) . ? C73A C74A 1.40(2) . ? C74A C75A 1.39(2) . ? C75A C76A 1.34(3) . ? C76A C77A 1.40(2) . ? C22A C21A 1.470(17) . ? C21A C11A 1.346(18) . ? C11A C12A 1.46(2) . ? C10A O10A 1.154(16) . ? N30A C31A 1.106(15) . ? C31A C32A 1.48(2) . ? I3B Mo1B 2.821(3) . ? Mo1B C21B 2.026(11) . ? Mo1B C10B 2.025(14) . ? Mo1B C11B 2.034(12) . ? Mo1B N30B 2.191(11) . ? Mo1B P4B 2.472(4) . ? Mo1B I2B 2.853(3) . ? P4B O61B 1.584(8) . ? P4B O71B 1.585(9) . ? P4B O51B 1.624(8) . ? O51B C52B 1.394(15) . ? C52B C53B 1.369(18) . ? C52B C57B 1.383(19) . ? C53B C54B 1.39(2) . ? C54B C55B 1.42(2) . ? C55B C56B 1.34(2) . ? C56B C57B 1.39(2) . ? O61B C62B 1.416(14) . ? C62B C64B 1.357(19) . ? C62B C67B 1.376(18) . ? C63B C65B 1.36(2) . ? C63B C64B 1.42(2) . ? C65B C66B 1.37(3) . ? C66B C67B 1.40(2) . ? O71B C72B 1.410(16) . ? C72B C73B 1.38(2) . ? C72B C77B 1.388(18) . ? C73B C74B 1.37(2) . ? C74B C75B 1.39(3) . ? C75B C76B 1.39(2) . ? C76B C77B 1.35(2) . ? C10B O10B 1.129(16) . ? N30B C31B 1.123(17) . ? C31B C32B 1.46(2) . ? C22B C21B 1.46(2) . ? C21B C11B 1.288(18) . ? C11B C12B 1.52(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 C10A Mo1A C21A 109.9(6) . . ? C10A Mo1A C11A 71.6(6) . . ? C21A Mo1A C11A 38.4(5) . . ? C10A Mo1A N30A 165.9(5) . . ? C21A Mo1A N30A 83.1(4) . . ? C11A Mo1A N30A 121.1(5) . . ? C10A Mo1A P4A 91.8(4) . . ? C21A Mo1A P4A 89.3(3) . . ? C11A Mo1A P4A 91.8(3) . . ? N30A Mo1A P4A 93.8(3) . . ? C10A Mo1A I3A 88.0(4) . . ? C21A Mo1A I3A 102.2(3) . . ? C11A Mo1A I3A 99.7(3) . . ? N30A Mo1A I3A 83.9(3) . . ? P4A Mo1A I3A 167.85(9) . . ? C10A Mo1A I2A 84.3(4) . . ? C21A Mo1A I2A 161.5(4) . . ? C11A Mo1A I2A 153.7(4) . . ? N30A Mo1A I2A 84.2(3) . . ? P4A Mo1A I2A 78.24(9) . . ? I3A Mo1A I2A 89.65(6) . . ? O51A P4A O61A 98.4(4) . . ? O51A P4A O71A 96.7(5) . . ? O61A P4A O71A 104.2(5) . . ? O51A P4A Mo1A 123.5(4) . . ? O61A P4A Mo1A 113.6(3) . . ? O71A P4A Mo1A 117.1(3) . . ? C52A O51A P4A 127.6(7) . . ? C57A C52A C53A 122.2(13) . . ? C57A C52A O51A 118.1(11) . . ? C53A C52A O51A 119.6(11) . . ? C52A C53A C54A 118.2(13) . . ? C55A C54A C53A 120.4(15) . . ? C54A C55A C56A 120.3(14) . . ? C55A C56A C57A 119.4(14) . . ? C52A C57A C56A 119.3(14) . . ? C62A O61A P4A 127.8(8) . . ? C63A C62A O61A 124.1(13) . . ? C63A C62A C67A 120.4(13) . . ? O61A C62A C67A 115.2(13) . . ? C62A C63A C64A 120.9(18) . . ? C65A C64A C63A 120(2) . . ? C64A C65A C66A 122.1(16) . . ? C67A C66A C65A 120(2) . . ? C66A C67A C62A 116.4(19) . . ? C72A O71A P4A 127.3(8) . . ? O71A C72A C77A 118.3(12) . . ? O71A C72A C73A 122.0(12) . . ? C77A C72A C73A 119.6(13) . . ? C74A C73A C72A 117.7(13) . . ? C75A C74A C73A 120.7(15) . . ? C76A C75A C74A 121.9(15) . . ? C75A C76A C77A 119.3(14) . . ? C72A C77A C76A 120.7(14) . . ? C11A C21A C22A 144.5(13) . . ? C11A C21A Mo1A 73.0(8) . . ? C22A C21A Mo1A 142.2(10) . . ? C21A C11A C12A 141.0(14) . . ? C21A C11A Mo1A 68.6(7) . . ? C12A C11A Mo1A 150.0(12) . . ? O10A C10A Mo1A 177.7(12) . . ? C31A N30A Mo1A 176.1(11) . . ? N30A C31A C32A 176.9(14) . . ? C21B Mo1B C10B 110.7(5) . . ? C21B Mo1B C11B 37.0(5) . . ? C10B Mo1B C11B 73.9(6) . . ? C21B Mo1B N30B 81.3(4) . . ? C10B Mo1B N30B 167.7(4) . . ? C11B Mo1B N30B 117.9(5) . . ? C21B Mo1B P4B 92.3(4) . . ? C10B Mo1B P4B 89.2(4) . . ? C11B Mo1B P4B 95.4(3) . . ? N30B Mo1B P4B 93.0(3) . . ? C21B Mo1B I3B 97.7(4) . . ? C10B Mo1B I3B 90.4(4) . . ? C11B Mo1B I3B 94.6(3) . . ? N30B Mo1B I3B 85.3(3) . . ? P4B Mo1B I3B 169.51(9) . . ? C21B Mo1B I2B 162.0(3) . . ? C10B Mo1B I2B 85.3(3) . . ? C11B Mo1B I2B 158.5(4) . . ? N30B Mo1B I2B 83.3(3) . . ? P4B Mo1B I2B 79.20(9) . . ? I3B Mo1B I2B 90.32(5) . . ? O61B P4B O71B 98.1(5) . . ? O61B P4B O51B 104.2(5) . . ? O71B P4B O51B 96.0(5) . . ? O61B P4B Mo1B 115.0(3) . . ? O71B P4B Mo1B 122.2(4) . . ? O51B P4B Mo1B 117.8(3) . . ? C52B O51B P4B 123.9(7) . . ? C53B C52B C57B 120.0(12) . . ? C53B C52B O51B 116.9(11) . . ? C57B C52B O51B 122.8(11) . . ? C52B C53B C54B 122.5(14) . . ? C53B C54B C55B 116.5(15) . . ? C56B C55B C54B 120.4(15) . . ? C55B C56B C57B 122.3(15) . . ? C52B C57B C56B 118.2(14) . . ? C62B O61B P4B 122.7(7) . . ? C64B C62B C67B 122.1(12) . . ? C64B C62B O61B 119.9(12) . . ? C67B C62B O61B 117.9(12) . . ? C65B C63B C64B 121.9(17) . . ? C62B C64B C63B 117.8(14) . . ? C63B C65B C66B 118.1(15) . . ? C65B C66B C67B 122.2(14) . . ? C62B C67B C66B 117.7(15) . . ? C72B O71B P4B 129.7(8) . . ? C73B C72B C77B 121.6(13) . . ? C73B C72B O71B 118.2(12) . . ? C77B C72B O71B 120.0(12) . . ? C74B C73B C72B 118.6(15) . . ? C73B C74B C75B 122.1(16) . . ? C74B C75B C76B 116.7(16) . . ? C77B C76B C75B 123.2(17) . . ? C76B C77B C72B 117.7(14) . . ? O10B C10B Mo1B 177.3(13) . . ? C31B N30B Mo1B 173.3(10) . . ? N30B C31B C32B 177.0(15) . . ? C11B C21B C22B 144.7(13) . . ? C11B C21B Mo1B 71.8(8) . . ? C22B C21B Mo1B 142.8(11) . . ? C21B C11B C12B 145.1(14) . . ? C21B C11B Mo1B 71.2(8) . . ? C12B C11B Mo1B 143.1(12) . . ? _refine_diff_density_max 0.823 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.135 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Mo(CO)(NCMe)(PhCCPh)(P(OPh)3)I2 _chemical_formula_sum 'C35 H28 I2 Mo N O4 P' _chemical_formula_weight 907.13 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.439(12) _cell_length_b 11.186(14) _cell_length_c 16.110(17) _cell_angle_alpha 89.763(10) _cell_angle_beta 73.927(10) _cell_angle_gamma 77.097(10) _cell_volume 1759(4) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 2.211 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_T_max 1.00 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5681 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.88 _reflns_number_total 5681 _reflns_number_gt 4356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+22.9080P] 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 0.0000(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5681 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2417 _refine_ls_wR_factor_gt 0.2223 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.139 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.14753(10) 0.19459(9) 0.23726(6) 0.0438(3) Uani 1 d . . . I2 I 0.17491(11) 0.17580(11) 0.40848(6) 0.0763(4) Uani 1 d . . . I3 I 0.36351(10) -0.01124(9) 0.17766(7) 0.0735(4) Uani 1 d . . . P4 P -0.0336(3) 0.3685(3) 0.31963(17) 0.0473(7) Uani 1 d . . . O41 O -0.1115(9) 0.4496(7) 0.2579(5) 0.056(2) Uani 1 d . . . C42 C -0.2017(13) 0.5660(11) 0.2766(8) 0.055(3) Uani 1 d . . . C43 C -0.2151(15) 0.6320(13) 0.2069(9) 0.067(4) Uani 1 d . . . H43 H -0.1631 0.6012 0.1514 0.080 Uiso 1 calc R . . C44 C -0.307(2) 0.7459(16) 0.2198(13) 0.094(5) Uani 1 d . . . H44 H -0.3200 0.7886 0.1720 0.113 Uiso 1 calc R . . C45 C -0.377(2) 0.7945(16) 0.2976(14) 0.097(6) Uani 1 d . . . H45 H -0.4320 0.8737 0.3045 0.116 Uiso 1 calc R . . C46 C -0.3692(19) 0.7285(18) 0.3689(12) 0.093(5) Uani 1 d . . . H46 H -0.4239 0.7611 0.4235 0.112 Uiso 1 calc R . . C47 C -0.2774(19) 0.6101(16) 0.3599(10) 0.089(5) Uani 1 d . . . H47 H -0.2692 0.5651 0.4076 0.107 Uiso 1 calc R . . O51 O 0.0027(9) 0.4702(8) 0.3734(5) 0.057(2) Uani 1 d . . . C52 C 0.1149(16) 0.5274(12) 0.3392(8) 0.063(3) Uani 1 d . . . C53 C 0.191(2) 0.5372(19) 0.3945(10) 0.094(6) Uani 1 d . . . H53 H 0.1711 0.5061 0.4490 0.112 Uiso 1 calc R . . C54 C 0.297(2) 0.595(2) 0.3666(13) 0.111(7) Uani 1 d . . . H54 H 0.3497 0.6029 0.4033 0.134 Uiso 1 calc R . . C55 C 0.328(2) 0.640(2) 0.2855(14) 0.115(8) Uani 1 d . . . H55 H 0.4028 0.6749 0.2663 0.138 Uiso 1 calc R . . C56 C 0.2416(18) 0.6330(16) 0.2319(12) 0.088(5) Uani 1 d . . . H56 H 0.2532 0.6713 0.1798 0.105 Uiso 1 calc R . . C57 C 0.1408(18) 0.5685(12) 0.2581(10) 0.074(4) Uani 1 d . . . H57 H 0.0914 0.5533 0.2209 0.089 Uiso 1 calc R . . O31 O -0.1554(9) 0.3484(8) 0.4026(5) 0.059(2) Uani 1 d . . . C62 C -0.2445(12) 0.2698(11) 0.4027(7) 0.049(3) Uani 1 d . . . C63 C -0.2362(13) 0.1745(15) 0.4536(9) 0.069(4) Uani 1 d . . . H63 H -0.1714 0.1598 0.4844 0.083 Uiso 1 calc R . . C64 C -0.3277(17) 0.0972(14) 0.4593(11) 0.078(4) Uani 1 d . . . H64 H -0.3239 0.0303 0.4937 0.093 Uiso 1 calc R . . C65 C -0.4200(18) 0.1218(16) 0.4146(11) 0.083(5) Uani 1 d . . . H65 H -0.4789 0.0697 0.4171 0.100 Uiso 1 calc R . . C66 C -0.4302(18) 0.2216(19) 0.3650(10) 0.090(5) Uani 1 d . . . H66 H -0.4967 0.2382 0.3356 0.108 Uiso 1 calc R . . C67 C -0.3406(16) 0.2971(16) 0.3595(9) 0.075(4) Uani 1 d . . . H67 H -0.3461 0.3656 0.3266 0.090 Uiso 1 calc R . . C21 C 0.0581(11) 0.2188(10) 0.1384(6) 0.042(2) Uani 1 d . . . C11 C 0.1601(12) 0.2751(10) 0.1214(6) 0.046(3) Uani 1 d . . . C12 C 0.2406(12) 0.3416(11) 0.0560(7) 0.048(2) Uani 1 d . . . C13 C 0.3791(15) 0.2925(15) 0.0164(9) 0.073(4) Uani 1 d . . . H13 H 0.4218 0.2178 0.0330 0.088 Uiso 1 calc R . . C14 C 0.4535(18) 0.3525(18) -0.0465(10) 0.089(5) Uani 1 d . . . H14 H 0.5446 0.3165 -0.0748 0.107 Uiso 1 calc R . . C15 C 0.393(2) 0.4657(17) -0.0676(11) 0.088(5) Uani 1 d . . . H15 H 0.4451 0.5085 -0.1081 0.106 Uiso 1 calc R . . C16 C 0.262(2) 0.5143(14) -0.0307(10) 0.084(5) Uani 1 d . . . H16 H 0.2236 0.5908 -0.0468 0.100 Uiso 1 calc R . . C17 C 0.1774(16) 0.4544(12) 0.0328(8) 0.065(3) Uani 1 d . . . H17 H 0.0847 0.4891 0.0573 0.078 Uiso 1 calc R . . O100 O 0.3905(9) 0.3286(9) 0.2106(6) 0.064(2) Uani 1 d . . . C100 C 0.2947(13) 0.2855(11) 0.2238(7) 0.051(3) Uani 1 d . . . C22 C -0.0389(14) 0.1875(11) 0.0984(8) 0.056(3) Uani 1 d . . . C23 C -0.0083(19) 0.1810(15) 0.0086(9) 0.082(5) Uani 1 d . . . H23 H 0.0721 0.1996 -0.0249 0.098 Uiso 1 calc R . . C24 C -0.096(2) 0.1473(18) -0.0301(12) 0.096(6) Uani 1 d . . . H24 H -0.0744 0.1435 -0.0902 0.115 Uiso 1 calc R . . C25 C -0.213(3) 0.119(2) 0.0151(19) 0.136(11) Uani 1 d . . . H25 H -0.2704 0.0933 -0.0128 0.163 Uiso 1 calc R . . C26 C -0.2463(19) 0.130(2) 0.1025(16) 0.109(7) Uani 1 d . . . H26 H -0.3304 0.1173 0.1346 0.131 Uiso 1 calc R . . C27 C -0.1587(15) 0.1599(14) 0.1458(11) 0.074(4) Uani 1 d . . . H27 H -0.1808 0.1611 0.2058 0.089 Uiso 1 calc R . . N200 N 0.0262(11) 0.0567(9) 0.2772(7) 0.057(2) Uani 1 d . . . C201 C -0.0178(15) -0.0261(13) 0.2987(8) 0.062(3) Uani 1 d . . . C202 C -0.063(2) -0.1349(17) 0.3302(13) 0.104(6) Uani 1 d . . . H20A H -0.0420 -0.1534 0.3839 0.124 Uiso 1 calc R . . H20B H -0.0174 -0.2027 0.2884 0.124 Uiso 1 calc R . . H20C H -0.1604 -0.1209 0.3394 0.124 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0517(6) 0.0438(5) 0.0402(5) 0.0053(4) -0.0151(4) -0.0175(4) I2 0.0830(7) 0.1066(8) 0.0538(5) 0.0240(5) -0.0325(4) -0.0356(6) I3 0.0702(6) 0.0536(5) 0.0928(7) 0.0028(4) -0.0248(5) -0.0039(4) P4 0.0557(17) 0.0523(17) 0.0364(13) -0.0022(11) -0.0095(12) -0.0221(14) O41 0.071(5) 0.047(4) 0.046(4) -0.003(3) -0.008(4) -0.017(4) C42 0.051(7) 0.047(7) 0.064(7) -0.008(5) -0.014(5) -0.008(6) C43 0.074(9) 0.061(8) 0.060(7) -0.008(6) -0.028(6) 0.004(7) C44 0.113(14) 0.068(10) 0.103(13) 0.002(9) -0.052(11) 0.001(10) C45 0.104(14) 0.056(9) 0.129(16) -0.020(10) -0.033(12) -0.014(10) C46 0.086(12) 0.090(12) 0.082(11) -0.030(9) 0.005(9) -0.010(10) C47 0.105(13) 0.075(10) 0.061(9) -0.008(7) 0.007(8) -0.004(10) O51 0.068(5) 0.064(5) 0.043(4) -0.011(4) -0.008(4) -0.033(5) C52 0.090(10) 0.052(7) 0.058(7) -0.006(5) -0.017(7) -0.041(8) C53 0.108(13) 0.115(15) 0.065(9) -0.010(9) -0.010(8) -0.058(12) C54 0.123(16) 0.133(18) 0.093(12) -0.028(11) -0.010(11) -0.087(15) C55 0.094(13) 0.123(17) 0.108(14) -0.040(12) 0.030(11) -0.058(13) C56 0.084(11) 0.068(10) 0.111(13) -0.006(9) -0.001(9) -0.047(9) C57 0.099(11) 0.041(7) 0.079(9) -0.003(6) -0.006(8) -0.034(8) O31 0.061(5) 0.071(6) 0.045(4) -0.003(4) -0.005(4) -0.031(5) C62 0.054(6) 0.054(7) 0.040(5) -0.001(5) -0.006(5) -0.022(6) C63 0.042(6) 0.090(10) 0.068(8) 0.009(7) -0.011(6) -0.005(7) C64 0.071(9) 0.053(8) 0.096(11) 0.010(7) 0.004(8) -0.022(8) C65 0.072(10) 0.082(11) 0.086(10) -0.017(8) 0.012(8) -0.039(9) C66 0.087(11) 0.127(16) 0.077(10) 0.027(10) -0.033(8) -0.054(11) C67 0.087(10) 0.094(11) 0.061(8) 0.023(7) -0.027(7) -0.049(9) C21 0.050(6) 0.037(5) 0.042(5) -0.007(4) -0.017(4) -0.008(5) C11 0.056(6) 0.034(5) 0.040(5) -0.010(4) -0.008(5) 0.000(5) C12 0.056(6) 0.049(6) 0.041(5) 0.002(4) -0.011(5) -0.023(6) C13 0.062(8) 0.076(10) 0.071(8) 0.009(7) 0.000(7) -0.019(7) C14 0.070(10) 0.104(13) 0.079(10) 0.019(9) 0.002(8) -0.019(10) C15 0.099(13) 0.089(12) 0.074(10) 0.008(9) -0.002(9) -0.045(11) C16 0.130(15) 0.057(8) 0.069(9) 0.021(7) -0.026(9) -0.034(10) C17 0.084(9) 0.055(7) 0.050(7) 0.002(5) -0.019(6) -0.004(7) O100 0.060(5) 0.067(6) 0.075(6) 0.005(4) -0.023(4) -0.030(5) C100 0.068(8) 0.050(7) 0.039(5) 0.000(4) -0.015(5) -0.021(6) C22 0.071(8) 0.042(6) 0.052(6) -0.012(5) -0.024(6) 0.002(6) C23 0.105(12) 0.085(11) 0.055(8) -0.012(7) -0.032(8) -0.010(10) C24 0.114(15) 0.092(13) 0.084(11) -0.027(9) -0.058(11) 0.011(12) C25 0.14(2) 0.122(19) 0.17(2) -0.067(18) -0.11(2) 0.015(17) C26 0.070(11) 0.107(16) 0.17(2) -0.011(14) -0.055(12) -0.029(11) C27 0.064(9) 0.068(9) 0.091(10) -0.005(7) -0.029(8) -0.007(8) N200 0.063(6) 0.044(6) 0.068(6) 0.005(5) -0.019(5) -0.023(5) C201 0.074(8) 0.055(8) 0.061(7) -0.005(6) -0.014(6) -0.031(7) C202 0.104(14) 0.079(11) 0.114(14) 0.009(10) 0.008(11) -0.043(11) _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 C100 1.988(13) . ? Mo1 C21 2.046(10) . ? Mo1 C11 2.052(11) . ? Mo1 N200 2.193(10) . ? Mo1 P4 2.471(4) . ? Mo1 I3 2.794(3) . ? Mo1 I2 2.853(3) . ? P4 O51 1.603(8) . ? P4 O41 1.608(9) . ? P4 O31 1.624(8) . ? O41 C42 1.404(14) . ? C42 C43 1.362(18) . ? C42 C47 1.383(18) . ? C43 C44 1.39(2) . ? C44 C45 1.31(3) . ? C45 C46 1.37(3) . ? C46 C47 1.43(2) . ? O51 C52 1.435(15) . ? C52 C57 1.359(19) . ? C52 C53 1.36(2) . ? C53 C54 1.37(2) . ? C54 C55 1.38(3) . ? C55 C56 1.42(3) . ? C56 C57 1.38(2) . ? O31 C62 1.415(14) . ? C62 C63 1.344(18) . ? C62 C67 1.354(19) . ? C63 C64 1.41(2) . ? C64 C65 1.34(2) . ? C65 C66 1.37(2) . ? C66 C67 1.38(2) . ? C21 C11 1.319(16) . ? C21 C22 1.445(16) . ? C11 C12 1.468(15) . ? C12 C17 1.389(17) . ? C12 C13 1.391(18) . ? C13 C14 1.37(2) . ? C14 C15 1.37(2) . ? C15 C16 1.32(2) . ? C16 C17 1.43(2) . ? O100 C100 1.172(14) . ? C22 C27 1.37(2) . ? C22 C23 1.391(18) . ? C23 C24 1.36(2) . ? C24 C25 1.34(3) . ? C25 C26 1.35(3) . ? C26 C27 1.39(2) . ? N200 C201 1.135(16) . ? C201 C202 1.44(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 C100 Mo1 C21 112.6(4) . . ? C100 Mo1 C11 75.1(5) . . ? C21 Mo1 C11 37.6(4) . . ? C100 Mo1 N200 160.7(4) . . ? C21 Mo1 N200 85.0(4) . . ? C11 Mo1 N200 121.7(4) . . ? C100 Mo1 P4 93.4(4) . . ? C21 Mo1 P4 88.4(3) . . ? C11 Mo1 P4 93.2(3) . . ? N200 Mo1 P4 94.8(3) . . ? C100 Mo1 I3 84.8(4) . . ? C21 Mo1 I3 103.3(3) . . ? C11 Mo1 I3 97.9(3) . . ? N200 Mo1 I3 83.5(3) . . ? P4 Mo1 I3 167.92(8) . . ? C100 Mo1 I2 82.0(3) . . ? C21 Mo1 I2 160.1(3) . . ? C11 Mo1 I2 154.5(3) . . ? N200 Mo1 I2 83.0(3) . . ? P4 Mo1 I2 76.83(9) . . ? I3 Mo1 I2 91.10(6) . . ? O51 P4 O41 102.7(5) . . ? O51 P4 O31 91.8(4) . . ? O41 P4 O31 104.6(5) . . ? O51 P4 Mo1 120.8(4) . . ? O41 P4 Mo1 111.6(3) . . ? O31 P4 Mo1 122.0(4) . . ? C42 O41 P4 128.6(7) . . ? C43 C42 C47 121.4(13) . . ? C43 C42 O41 115.9(11) . . ? C47 C42 O41 122.7(12) . . ? C42 C43 C44 119.4(14) . . ? C45 C44 C43 121.7(17) . . ? C44 C45 C46 120.1(17) . . ? C45 C46 C47 120.6(15) . . ? C42 C47 C46 116.5(15) . . ? C52 O51 P4 123.5(7) . . ? C57 C52 C53 123.8(15) . . ? C57 C52 O51 121.5(12) . . ? C53 C52 O51 114.7(12) . . ? C52 C53 C54 117.6(17) . . ? C53 C54 C55 121.7(19) . . ? C54 C55 C56 118.6(18) . . ? C57 C56 C55 119.0(18) . . ? C52 C57 C56 118.8(16) . . ? C62 O31 P4 125.4(7) . . ? C63 C62 C67 122.6(13) . . ? C63 C62 O31 116.5(11) . . ? C67 C62 O31 120.7(12) . . ? C62 C63 C64 118.6(14) . . ? C65 C64 C63 119.0(15) . . ? C64 C65 C66 121.8(16) . . ? C65 C66 C67 119.2(16) . . ? C62 C67 C66 118.8(14) . . ? C11 C21 C22 140.1(10) . . ? C11 C21 Mo1 71.5(6) . . ? C22 C21 Mo1 147.9(9) . . ? C21 C11 C12 144.1(10) . . ? C21 C11 Mo1 71.0(6) . . ? C12 C11 Mo1 144.6(9) . . ? C17 C12 C13 119.7(12) . . ? C17 C12 C11 119.5(11) . . ? C13 C12 C11 120.8(11) . . ? C14 C13 C12 120.9(15) . . ? C15 C14 C13 119.8(16) . . ? C16 C15 C14 120.3(15) . . ? C15 C16 C17 122.8(15) . . ? C12 C17 C16 116.4(14) . . ? O100 C100 Mo1 172.9(10) . . ? C27 C22 C23 118.6(14) . . ? C27 C22 C21 122.3(11) . . ? C23 C22 C21 119.1(13) . . ? C24 C23 C22 119.8(18) . . ? C25 C24 C23 122.5(18) . . ? C24 C25 C26 117.9(17) . . ? C25 C26 C27 122(2) . . ? C22 C27 C26 118.8(17) . . ? C201 N200 Mo1 169.3(11) . . ? N200 C201 C202 174.3(17) . . ? _refine_diff_density_max 1.474 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.174 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Mo(NCMe)(CO)(MeCCPh)I2(P(OPh)3),0.5(CH3)2CO, H2O' _chemical_formula_sum 'C31.50 H34 I2 Mo N O5.50 P' _chemical_formula_weight 895.31 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 12.121(13) _cell_length_b 15.702(17) _cell_length_c 20.38(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.265(10) _cell_angle_gamma 90.00 _cell_volume 3723(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11072 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6779 _reflns_number_gt 4283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1861P)^2^+8.1347P] 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 0.0006(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6779 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.2996 _refine_ls_wR_factor_gt 0.2658 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.117 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.45850(9) 0.65084(6) 0.17017(5) 0.0476(3) Uani 1 d . . . I2 I 0.32378(9) 0.78922(7) 0.10171(5) 0.0744(4) Uani 1 d . . . I3 I 0.26503(9) 0.54847(7) 0.16242(7) 0.0846(4) Uani 1 d . . . P4 P 0.6084(3) 0.75756(19) 0.17018(14) 0.0494(7) Uani 1 d . . . O41 O 0.7359(7) 0.7171(5) 0.2037(4) 0.0555(19) Uani 1 d . . . C42 C 0.8432(11) 0.7494(8) 0.2041(6) 0.058(3) Uani 1 d . . . C43 C 0.8682(12) 0.8361(9) 0.2042(8) 0.071(4) Uani 1 d . . . H43 H 0.8119 0.8767 0.2033 0.086 Uiso 1 calc R . . C44 C 0.9741(13) 0.8592(12) 0.2058(9) 0.086(5) Uani 1 d . . . H44 H 0.9910 0.9168 0.2039 0.103 Uiso 1 calc R . . C45 C 1.0596(14) 0.8001(13) 0.2103(9) 0.088(5) Uani 1 d . . . H45 H 1.1339 0.8178 0.2128 0.105 Uiso 1 calc R . . C46 C 1.0369(17) 0.7206(16) 0.2112(12) 0.110(7) Uani 1 d . . . H46 H 1.0949 0.6810 0.2133 0.132 Uiso 1 calc R . . C47 C 0.9244(13) 0.6915(9) 0.2088(8) 0.076(4) Uani 1 d . . . H47 H 0.9086 0.6337 0.2105 0.091 Uiso 1 calc R . . O51 O 0.6098(8) 0.8471(5) 0.2088(4) 0.060(2) Uani 1 d . . . C52 C 0.6155(10) 0.8574(7) 0.2778(6) 0.053(3) Uani 1 d . . . C53 C 0.6798(13) 0.8097(8) 0.3297(6) 0.063(3) Uani 1 d . . . H53 H 0.7194 0.7626 0.3203 0.076 Uiso 1 calc R . . C54 C 0.6870(17) 0.8306(13) 0.3968(8) 0.088(5) Uani 1 d . . . H54 H 0.7339 0.7997 0.4329 0.106 Uiso 1 calc R . . C55 C 0.620(2) 0.9019(13) 0.4095(10) 0.101(6) Uani 1 d . . . H55 H 0.6204 0.9163 0.4540 0.121 Uiso 1 calc R . . C56 C 0.5587(17) 0.9451(13) 0.3584(9) 0.096(6) Uani 1 d . . . H56 H 0.5160 0.9907 0.3672 0.116 Uiso 1 calc R . . C57 C 0.5533(11) 0.9274(9) 0.2916(8) 0.069(3) Uani 1 d . . . H57 H 0.5095 0.9610 0.2563 0.083 Uiso 1 calc R . . O61 O 0.6192(8) 0.8011(6) 0.1009(4) 0.061(2) Uani 1 d . . . C62 C 0.6103(12) 0.7553(10) 0.0402(6) 0.065(3) Uani 1 d . . . C63 C 0.6791(16) 0.6868(12) 0.0389(8) 0.083(4) Uani 1 d . . . H63 H 0.7315 0.6668 0.0784 0.100 Uiso 1 calc R . . C64 C 0.667(2) 0.6476(14) -0.0251(10) 0.109(7) Uani 1 d . . . H64 H 0.7109 0.6000 -0.0288 0.131 Uiso 1 calc R . . C65 C 0.586(2) 0.683(2) -0.0843(9) 0.121(9) Uani 1 d . . . H65 H 0.5804 0.6589 -0.1268 0.146 Uiso 1 calc R . . C66 C 0.518(2) 0.7511(18) -0.0809(11) 0.119(7) Uani 1 d . . . H66 H 0.4635 0.7719 -0.1194 0.143 Uiso 1 calc R . . C67 C 0.5330(17) 0.7861(14) -0.0189(7) 0.095(6) Uani 1 d . . . H67 H 0.4893 0.8337 -0.0154 0.115 Uiso 1 calc R . . C100 C 0.4422(11) 0.6127(8) 0.0751(6) 0.058(3) Uani 1 d . . . O100 O 0.4287(10) 0.5861(7) 0.0206(5) 0.084(3) Uani 1 d . . . N200 N 0.4194(9) 0.7110(6) 0.2599(5) 0.056(2) Uani 1 d . . . C201 C 0.3862(11) 0.7472(9) 0.2975(6) 0.057(3) Uani 1 d . . . C202 C 0.3309(16) 0.7985(10) 0.3404(8) 0.080(4) Uani 1 d . . . H20A H 0.3034 0.8510 0.3175 0.096 Uiso 1 calc R . . H20B H 0.3859 0.8106 0.3834 0.096 Uiso 1 calc R . . H20C H 0.2676 0.7673 0.3481 0.096 Uiso 1 calc R . . C12 C 0.6316(14) 0.4941(10) 0.1412(7) 0.078(4) Uani 1 d . . . H22A H 0.7111 0.5085 0.1487 0.093 Uiso 1 calc R . . H22B H 0.5943 0.4924 0.0929 0.093 Uiso 1 calc R . . H22C H 0.6257 0.4393 0.1608 0.093 Uiso 1 calc R . . C11 C 0.5745(11) 0.5600(7) 0.1741(6) 0.054(3) Uani 1 d . . . C21 C 0.5870(10) 0.5883(7) 0.2382(6) 0.054(3) Uani 1 d . . . C22 C 0.6593(11) 0.5732(7) 0.3079(5) 0.053(3) Uani 1 d . . . C23 C 0.7688(13) 0.5419(9) 0.3167(7) 0.070(4) Uani 1 d . . . H23 H 0.7935 0.5301 0.2784 0.084 Uiso 1 calc R . . C24 C 0.8429(17) 0.5275(13) 0.3810(8) 0.098(6) Uani 1 d . . . H24 H 0.9161 0.5052 0.3867 0.117 Uiso 1 calc R . . C25 C 0.803(2) 0.5482(15) 0.4374(8) 0.107(7) Uani 1 d . . . H25 H 0.8509 0.5415 0.4814 0.129 Uiso 1 calc R . . C26 C 0.698(2) 0.5768(13) 0.4286(8) 0.102(6) Uani 1 d . . . H26 H 0.6732 0.5881 0.4669 0.123 Uiso 1 calc R . . C27 C 0.6213(16) 0.5913(10) 0.3629(7) 0.077(4) Uani 1 d . . . H27 H 0.5477 0.6124 0.3577 0.093 Uiso 1 calc R . . C400 C 0.294(5) 0.560(3) 0.405(3) 0.122(14) Uiso 0.50 d P . . C401 C 0.375(3) 0.628(2) 0.4399(18) 0.086(9) Uiso 0.50 d P . . H40A H 0.4428 0.6263 0.4240 0.103 Uiso 0.50 calc PR . . H40B H 0.3968 0.6185 0.4884 0.103 Uiso 0.50 calc PR . . H40C H 0.3392 0.6826 0.4298 0.103 Uiso 0.50 calc PR . . C402 C 0.195(6) 0.558(4) 0.372(3) 0.15(2) Uiso 0.50 d P . . H40D H 0.1786 0.6073 0.3423 0.185 Uiso 0.50 calc PR . . H40E H 0.1466 0.5589 0.4018 0.185 Uiso 0.50 calc PR . . H40F H 0.1812 0.5075 0.3447 0.185 Uiso 0.50 calc PR . . O403 O 0.325(5) 0.537(4) 0.365(3) 0.21(2) Uiso 0.50 d P . . O500 O 0.462(3) 0.6998(18) 0.5198(16) 0.218(11) Uiso 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 0.0551(6) 0.0474(5) 0.0406(5) -0.0055(4) 0.0140(4) 0.0009(4) I2 0.0724(6) 0.0791(7) 0.0693(6) 0.0126(5) 0.0158(4) 0.0202(4) I3 0.0735(7) 0.0736(7) 0.1149(9) -0.0221(6) 0.0395(6) -0.0171(5) P4 0.0610(17) 0.0461(15) 0.0404(14) -0.0033(12) 0.0128(12) -0.0009(12) O41 0.058(5) 0.052(4) 0.056(5) 0.002(4) 0.015(4) 0.005(4) C42 0.064(8) 0.061(7) 0.050(6) -0.005(6) 0.016(6) 0.006(6) C43 0.060(8) 0.057(7) 0.099(11) -0.003(7) 0.026(7) 0.002(6) C44 0.060(9) 0.090(11) 0.096(11) 0.010(9) 0.005(8) -0.008(8) C45 0.063(9) 0.109(14) 0.086(11) -0.015(10) 0.010(8) -0.005(9) C46 0.080(12) 0.126(18) 0.113(15) -0.016(13) 0.008(10) 0.033(12) C47 0.078(10) 0.055(7) 0.087(10) -0.004(7) 0.011(8) 0.013(7) O51 0.089(6) 0.041(4) 0.051(4) -0.008(3) 0.023(4) 0.006(4) C52 0.060(7) 0.042(6) 0.054(6) 0.004(5) 0.013(5) -0.011(5) C53 0.083(9) 0.053(7) 0.049(6) -0.009(6) 0.010(6) -0.009(6) C54 0.105(12) 0.097(12) 0.061(8) 0.003(8) 0.019(8) -0.008(10) C55 0.136(16) 0.102(13) 0.082(11) -0.031(11) 0.061(12) -0.028(12) C56 0.102(13) 0.106(13) 0.072(10) -0.033(10) 0.009(9) 0.023(10) C57 0.055(7) 0.066(8) 0.086(9) -0.010(7) 0.020(7) 0.004(6) O61 0.071(5) 0.062(5) 0.053(5) 0.000(4) 0.021(4) 0.004(4) C62 0.069(8) 0.079(9) 0.047(6) 0.006(6) 0.016(6) -0.016(7) C63 0.096(11) 0.096(11) 0.062(8) -0.021(8) 0.028(8) -0.013(9) C64 0.141(17) 0.131(16) 0.081(11) -0.060(12) 0.073(12) -0.046(14) C65 0.137(18) 0.19(3) 0.050(9) -0.029(12) 0.050(11) -0.058(18) C66 0.14(2) 0.15(2) 0.073(12) 0.001(13) 0.038(12) -0.015(17) C67 0.111(13) 0.136(16) 0.040(7) 0.006(8) 0.021(8) -0.001(11) C100 0.072(8) 0.048(6) 0.052(7) 0.000(5) 0.014(6) -0.002(5) O100 0.104(8) 0.097(8) 0.044(5) -0.023(5) 0.009(5) -0.005(6) N200 0.057(6) 0.054(6) 0.062(6) 0.007(5) 0.025(5) 0.002(4) C201 0.060(7) 0.070(7) 0.042(6) -0.007(6) 0.019(5) 0.008(6) C202 0.104(12) 0.081(10) 0.067(8) -0.018(7) 0.044(8) -0.004(8) C12 0.094(10) 0.078(9) 0.056(7) -0.027(7) 0.011(7) 0.026(8) C11 0.068(7) 0.042(6) 0.052(6) -0.010(5) 0.018(5) 0.000(5) C21 0.058(6) 0.049(6) 0.054(6) -0.015(5) 0.014(5) -0.011(5) C22 0.078(8) 0.045(6) 0.032(5) -0.005(5) 0.007(5) -0.004(5) C23 0.075(9) 0.077(9) 0.053(7) 0.008(7) 0.009(6) -0.003(7) C24 0.100(12) 0.113(14) 0.060(9) -0.002(9) -0.010(8) -0.007(10) C25 0.111(15) 0.134(17) 0.048(9) 0.020(10) -0.023(9) -0.019(13) C26 0.16(2) 0.105(13) 0.037(7) -0.007(8) 0.022(10) -0.012(13) C27 0.109(12) 0.071(9) 0.045(7) 0.006(6) 0.009(7) 0.011(8) _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 C100 1.983(13) . ? Mo1 C11 1.989(12) . ? Mo1 C21 2.026(13) . ? Mo1 N200 2.223(11) . ? Mo1 P4 2.471(4) . ? Mo1 I3 2.811(3) . ? Mo1 I2 2.839(2) . ? P4 O61 1.607(9) . ? P4 O51 1.609(8) . ? P4 O41 1.633(9) . ? O41 C42 1.394(16) . ? C42 C47 1.323(19) . ? C42 C43 1.395(19) . ? C43 C44 1.33(2) . ? C44 C45 1.38(3) . ? C45 C46 1.28(3) . ? C46 C47 1.43(3) . ? O51 C52 1.398(14) . ? C52 C53 1.351(18) . ? C52 C57 1.404(18) . ? C53 C54 1.39(2) . ? C54 C55 1.45(3) . ? C55 C56 1.29(3) . ? C56 C57 1.37(2) . ? O61 C62 1.407(17) . ? C62 C63 1.37(2) . ? C62 C67 1.39(2) . ? C63 C64 1.41(2) . ? C64 C65 1.44(4) . ? C65 C66 1.37(4) . ? C66 C67 1.34(3) . ? C100 O100 1.155(15) . ? N200 C201 1.116(15) . ? C201 C202 1.480(19) . ? C12 C11 1.503(17) . ? C11 C21 1.348(17) . ? C21 C22 1.464(16) . ? C22 C27 1.35(2) . ? C22 C23 1.38(2) . ? C23 C24 1.38(2) . ? C24 C25 1.41(3) . ? C25 C26 1.31(3) . ? C26 C27 1.42(2) . ? C400 O403 1.06(7) . ? C400 C402 1.20(7) . ? C400 C401 1.49(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 C100 Mo1 C11 72.5(5) . . ? C100 Mo1 C21 111.7(5) . . ? C11 Mo1 C21 39.2(5) . . ? C100 Mo1 N200 160.9(5) . . ? C11 Mo1 N200 125.6(4) . . ? C21 Mo1 N200 86.7(4) . . ? C100 Mo1 P4 94.4(4) . . ? C11 Mo1 P4 88.6(4) . . ? C21 Mo1 P4 84.5(3) . . ? N200 Mo1 P4 92.2(3) . . ? C100 Mo1 I3 85.4(4) . . ? C11 Mo1 I3 99.3(4) . . ? C21 Mo1 I3 103.3(3) . . ? N200 Mo1 I3 85.6(3) . . ? P4 Mo1 I3 171.66(8) . . ? C100 Mo1 I2 82.2(4) . . ? C11 Mo1 I2 150.7(4) . . ? C21 Mo1 I2 159.0(3) . . ? N200 Mo1 I2 81.6(3) . . ? P4 Mo1 I2 78.62(11) . . ? I3 Mo1 I2 93.10(9) . . ? O61 P4 O51 93.8(5) . . ? O61 P4 O41 103.4(5) . . ? O51 P4 O41 104.9(5) . . ? O61 P4 Mo1 121.9(4) . . ? O51 P4 Mo1 120.0(4) . . ? O41 P4 Mo1 110.2(3) . . ? C42 O41 P4 129.3(8) . . ? C47 C42 O41 115.1(12) . . ? C47 C42 C43 120.9(14) . . ? O41 C42 C43 123.8(11) . . ? C44 C43 C42 118.4(14) . . ? C43 C44 C45 121.6(17) . . ? C46 C45 C44 119.9(18) . . ? C45 C46 C47 121.3(17) . . ? C42 C47 C46 117.8(16) . . ? C52 O51 P4 125.7(7) . . ? C53 C52 O51 125.3(12) . . ? C53 C52 C57 120.1(13) . . ? O51 C52 C57 114.5(11) . . ? C52 C53 C54 120.3(15) . . ? C53 C54 C55 118.4(17) . . ? C56 C55 C54 119.0(16) . . ? C55 C56 C57 123.6(17) . . ? C56 C57 C52 118.6(15) . . ? C62 O61 P4 123.4(8) . . ? C63 C62 C67 121.5(15) . . ? C63 C62 O61 121.5(12) . . ? C67 C62 O61 116.9(15) . . ? C62 C63 C64 117.3(18) . . ? C63 C64 C65 118(2) . . ? C66 C65 C64 122.9(17) . . ? C67 C66 C65 116(2) . . ? C66 C67 C62 124(2) . . ? O100 C100 Mo1 175.6(12) . . ? C201 N200 Mo1 169.1(10) . . ? N200 C201 C202 173.2(14) . . ? C21 C11 C12 136.0(12) . . ? C21 C11 Mo1 71.9(7) . . ? C12 C11 Mo1 152.1(10) . . ? C11 C21 C22 139.6(12) . . ? C11 C21 Mo1 68.9(7) . . ? C22 C21 Mo1 151.5(9) . . ? C27 C22 C23 120.3(12) . . ? C27 C22 C21 121.2(13) . . ? C23 C22 C21 118.5(11) . . ? C22 C23 C24 121.9(15) . . ? C23 C24 C25 116.9(18) . . ? C26 C25 C24 120.8(14) . . ? C25 C26 C27 122.6(18) . . ? C22 C27 C26 117.5(17) . . ? O403 C400 C402 94(6) . . ? O403 C400 C401 107(6) . . ? C402 C400 C401 135(6) . . ? _refine_diff_density_max 1.618 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.226 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Mo(CO)(MeCCPh)I2(P(OPh)3)2 _chemical_formula_sum 'C46 H35 I2 Mo O7 P2' _chemical_formula_weight 1111.42 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.08(2) _cell_length_b 11.581(17) _cell_length_c 23.65(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.475(10) _cell_angle_gamma 90.00 _cell_volume 4575(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2180 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker,1983)' _exptl_absorpt_correction_T_min 0.183 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5649 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3702 _reflns_number_gt 1695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. The structure was disordered. All atoms apart from the carbonyl and the phenylacetlene were consistent with a non-crystallographic twofold axis. It was possible that these two groups were disordered over two sites but no satisfactory model could be found. The phenyl group was however necessarily refined as a rigid group as was one of the phenyl rings in a phosphite. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1656P)^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 0.0011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(7) _refine_ls_number_reflns 3702 _refine_ls_number_parameters 446 _refine_ls_number_restraints 219 _refine_ls_R_factor_all 0.1771 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2693 _refine_ls_wR_factor_gt 0.2125 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.03395(13) 0.6253(3) 0.32103(10) 0.0799(8) Uani 1 d . . . I2 I 0.14309(12) 0.4597(3) 0.30857(9) 0.1170(11) Uani 1 d . . . I3 I 0.15510(12) 0.7896(3) 0.33351(10) 0.1182(11) Uani 1 d . . . C21 C -0.040(2) 0.499(3) 0.2965(17) 0.119(11) Uiso 1 d D . . C22 C -0.0670(19) 0.383(3) 0.2760(13) 0.091(8) Uiso 1 d . . . H22A H -0.1129 0.3654 0.2853 0.109 Uiso 1 calc R . . H22B H -0.0248 0.3295 0.2964 0.109 Uiso 1 calc R . . H22C H -0.0810 0.3784 0.2326 0.109 Uiso 1 calc R . . O100 O -0.0228(16) 0.868(2) 0.3643(12) 0.122(8) Uiso 1 d . . . C100 C -0.0080(17) 0.767(3) 0.3429(13) 0.087(8) Uiso 1 d . . . C11 C -0.069(3) 0.596(4) 0.315(2) 0.144(15) Uiso 1 d D . . C12 C -0.1512(11) 0.620(2) 0.3222(10) 0.086(8) Uiso 1 d G . . C13 C -0.1670(14) 0.685(2) 0.3657(10) 0.127(12) Uiso 1 d G . . H13 H -0.1263 0.7276 0.3946 0.152 Uiso 1 calc R . . C14 C -0.2437(16) 0.687(2) 0.3662(11) 0.133(13) Uiso 1 d G . . H14 H -0.2542 0.7305 0.3953 0.159 Uiso 1 calc R . . C15 C -0.3045(12) 0.624(3) 0.3231(13) 0.19(2) Uiso 1 d G . . H15 H -0.3558 0.6248 0.3234 0.222 Uiso 1 calc R . . C16 C -0.2888(12) 0.559(2) 0.2795(11) 0.116(11) Uiso 1 d G . . H16 H -0.3295 0.5163 0.2507 0.139 Uiso 1 calc R . . C17 C -0.2121(14) 0.557(2) 0.2791(9) 0.122(12) Uiso 1 d G . . H17 H -0.2015 0.5134 0.2499 0.146 Uiso 1 calc R . . P4 P 0.0982(4) 0.5801(9) 0.4330(3) 0.087(3) Uani 1 d . . . O41 O 0.0533(13) 0.661(2) 0.4676(9) 0.108(7) Uani 1 d . . . C42 C 0.0812(18) 0.675(4) 0.5310(12) 0.097(9) Uani 1 d U . . C43 C 0.112(2) 0.790(4) 0.5505(15) 0.119(10) Uani 1 d U . . H43 H 0.1147 0.8443 0.5226 0.143 Uiso 1 calc R . . C44 C 0.137(3) 0.816(5) 0.6126(15) 0.141(12) Uani 1 d U . . H44 H 0.1599 0.8866 0.6286 0.169 Uiso 1 calc R . . C45 C 0.125(2) 0.723(4) 0.6513(13) 0.126(11) Uani 1 d U . . H45 H 0.1384 0.7367 0.6928 0.151 Uiso 1 calc R . . C46 C 0.098(3) 0.627(4) 0.6285(17) 0.129(12) Uani 1 d U . . H46 H 0.0930 0.5697 0.6545 0.154 Uiso 1 calc R . . C47 C 0.076(2) 0.602(4) 0.5698(13) 0.104(9) Uani 1 d U . . H47 H 0.0565 0.5284 0.5562 0.125 Uiso 1 calc R . . O51 O 0.1912(14) 0.614(2) 0.4711(10) 0.104(7) Uani 1 d . . . C52 C 0.2577(18) 0.538(3) 0.4943(12) 0.093(9) Uani 1 d U . . C53 C 0.263(2) 0.474(4) 0.5472(16) 0.127(11) Uani 1 d U . . H53 H 0.2246 0.4719 0.5642 0.152 Uiso 1 calc R . . C54 C 0.336(2) 0.416(4) 0.5694(16) 0.130(12) Uani 1 d U . . H54 H 0.3505 0.3825 0.6081 0.156 Uiso 1 calc R . . C55 C 0.387(2) 0.401(5) 0.542(2) 0.137(12) Uani 1 d U . . H55 H 0.4295 0.3501 0.5578 0.165 Uiso 1 calc R . . C56 C 0.377(2) 0.463(5) 0.489(2) 0.136(11) Uani 1 d U . . H56 H 0.4148 0.4595 0.4716 0.164 Uiso 1 calc R . . C57 C 0.3075(18) 0.530(4) 0.4640(14) 0.105(9) Uani 1 d U . . H57 H 0.2959 0.5682 0.4271 0.126 Uiso 1 calc R . . O61 O 0.0963(12) 0.4523(18) 0.4591(8) 0.085(6) Uani 1 d . . . C62 C 0.040(2) 0.356(4) 0.4334(14) 0.105(10) Uani 1 d U . . C63 C -0.031(2) 0.389(3) 0.4331(15) 0.114(10) Uani 1 d U . . H63 H -0.0446 0.4604 0.4446 0.137 Uiso 1 calc R . . C64 C -0.090(3) 0.277(5) 0.4083(19) 0.135(11) Uani 1 d U . . H64 H -0.1430 0.2795 0.4043 0.162 Uiso 1 calc R . . C65 C 0.005(3) 0.161(5) 0.3980(19) 0.141(12) Uani 1 d U . . H65 H 0.0188 0.0871 0.3897 0.169 Uiso 1 calc R . . C66 C -0.061(3) 0.188(4) 0.3948(16) 0.123(11) Uani 1 d U . . H66 H -0.0989 0.1294 0.3789 0.148 Uiso 1 calc R . . C67 C 0.062(3) 0.261(4) 0.4170(16) 0.118(10) Uani 1 d U . . H67 H 0.1135 0.2544 0.4169 0.141 Uiso 1 calc R . . P7 P -0.0143(5) 0.6697(10) 0.2082(3) 0.094(3) Uani 1 d . . . O71 O -0.0391(15) 0.7982(17) 0.1818(9) 0.094(6) Uani 1 d . . . C72 C -0.0719(13) 0.880(2) 0.2063(10) 0.112(11) Uani 1 d GU . . C73 C -0.1453(12) 0.8637(19) 0.2113(9) 0.097(9) Uani 1 d GU . . H73 H -0.1710 0.7927 0.2013 0.116 Uiso 1 calc R . . C74 C -0.1803(13) 0.954(3) 0.2313(11) 0.129(11) Uani 1 d GU . . H74 H -0.2294 0.9426 0.2347 0.155 Uiso 1 calc R . . C75 C -0.1419(19) 1.060(2) 0.2463(13) 0.137(13) Uani 1 d GU . . H75 H -0.1653 1.1197 0.2597 0.164 Uiso 1 calc R . . C76 C -0.0685(19) 1.0759(19) 0.2412(13) 0.157(15) Uani 1 d GU . . H76 H -0.0428 1.1469 0.2513 0.188 Uiso 1 calc R . . C77 C -0.0335(13) 0.986(3) 0.2212(11) 0.126(12) Uani 1 d GU . . H77 H 0.0156 0.9970 0.2178 0.151 Uiso 1 calc R . . O81 O -0.0923(12) 0.590(2) 0.1752(8) 0.095(6) Uani 1 d . . . C82 C -0.1292(18) 0.569(4) 0.1091(12) 0.096(9) Uani 1 d U . . C83 C -0.1748(19) 0.651(4) 0.0698(15) 0.113(11) Uani 1 d U . . H83 H -0.1785 0.7241 0.0843 0.136 Uiso 1 calc R . . C84 C -0.216(2) 0.626(4) 0.0088(14) 0.113(10) Uani 1 d U . . H84 H -0.2487 0.6795 -0.0188 0.135 Uiso 1 calc R . . C85 C -0.203(2) 0.515(4) -0.0084(11) 0.106(10) Uani 1 d U . . H85 H -0.2305 0.4954 -0.0493 0.127 Uiso 1 calc R . . C86 C -0.154(2) 0.432(4) 0.0300(13) 0.114(10) Uani 1 d U . . H86 H -0.1457 0.3599 0.0160 0.137 Uiso 1 calc R . . C87 C -0.1202(19) 0.464(4) 0.0902(14) 0.101(9) Uani 1 d U . . H87 H -0.0894 0.4106 0.1188 0.121 Uiso 1 calc R . . O91 O 0.0393(11) 0.6366(19) 0.1701(9) 0.094(6) Uani 1 d . . . C92 C 0.084(2) 0.710(4) 0.1466(14) 0.117(10) Uani 1 d U . . C93 C 0.038(2) 0.773(4) 0.0938(16) 0.120(10) Uani 1 d U . . H93 H -0.0171 0.7707 0.0758 0.144 Uiso 1 calc R . . C94 C 0.082(3) 0.835(5) 0.0726(17) 0.141(13) Uani 1 d U . . H94 H 0.0562 0.8741 0.0361 0.169 Uiso 1 calc R . . C95 C 0.162(3) 0.846(5) 0.0997(19) 0.139(12) Uani 1 d U . . H95 H 0.1889 0.8972 0.0838 0.167 Uiso 1 calc R . . C96 C 0.203(2) 0.783(5) 0.150(2) 0.142(12) Uani 1 d U . . H96 H 0.2589 0.7888 0.1675 0.170 Uiso 1 calc R . . C97 C 0.164(2) 0.707(5) 0.1772(17) 0.139(12) Uani 1 d U . . H97 H 0.1899 0.6613 0.2116 0.167 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0806(14) 0.084(2) 0.0745(13) 0.0012(12) 0.0295(11) 0.0029(14) I2 0.1278(19) 0.129(3) 0.1038(14) 0.0164(14) 0.0550(13) 0.0397(16) I3 0.1040(15) 0.134(3) 0.1029(14) 0.0197(14) 0.0235(11) -0.0284(15) P4 0.067(4) 0.109(8) 0.075(4) 0.008(4) 0.015(3) -0.012(4) O41 0.097(14) 0.14(2) 0.082(12) 0.001(13) 0.031(11) 0.011(13) C42 0.088(16) 0.15(3) 0.068(15) -0.043(16) 0.049(12) -0.023(17) C43 0.13(2) 0.15(3) 0.083(16) -0.018(18) 0.053(15) -0.02(2) C44 0.16(2) 0.17(3) 0.077(17) -0.032(19) 0.019(17) -0.03(2) C45 0.17(3) 0.15(3) 0.047(13) -0.018(16) 0.033(15) -0.02(2) C46 0.16(2) 0.13(3) 0.085(18) -0.006(19) 0.035(17) -0.04(2) C47 0.113(19) 0.15(2) 0.079(16) -0.046(15) 0.073(14) -0.056(17) O51 0.102(15) 0.11(2) 0.104(14) -0.006(13) 0.043(12) -0.006(13) C52 0.087(16) 0.10(2) 0.071(14) -0.006(15) 0.006(13) 0.002(17) C53 0.108(18) 0.17(3) 0.081(16) 0.027(19) 0.008(15) 0.02(2) C54 0.091(19) 0.19(3) 0.087(18) 0.02(2) 0.012(16) 0.01(2) C55 0.064(15) 0.20(3) 0.14(2) 0.01(2) 0.019(17) 0.010(19) C56 0.089(17) 0.19(3) 0.15(2) 0.02(2) 0.069(18) -0.01(2) C57 0.077(15) 0.15(3) 0.095(16) 0.021(17) 0.045(13) -0.007(18) O61 0.101(13) 0.069(16) 0.071(10) 0.008(10) 0.019(9) -0.009(11) C62 0.13(2) 0.10(3) 0.089(16) -0.032(16) 0.050(15) -0.06(2) C63 0.109(18) 0.13(3) 0.131(19) -0.075(18) 0.082(16) -0.057(18) C64 0.12(2) 0.18(3) 0.13(2) -0.03(2) 0.062(17) -0.03(2) C65 0.16(3) 0.16(3) 0.12(2) -0.02(2) 0.07(2) -0.03(3) C66 0.13(2) 0.14(3) 0.106(19) -0.056(19) 0.052(18) -0.02(2) C67 0.14(2) 0.13(3) 0.102(18) 0.016(19) 0.074(16) 0.00(2) P7 0.089(5) 0.126(9) 0.070(4) -0.004(4) 0.036(4) 0.007(5) O71 0.16(2) 0.033(14) 0.093(12) -0.006(10) 0.051(13) 0.015(13) C72 0.14(2) 0.10(2) 0.076(15) -0.017(16) 0.015(16) 0.05(2) C73 0.055(12) 0.13(2) 0.093(16) -0.037(16) 0.015(12) 0.017(15) C74 0.12(2) 0.15(3) 0.114(19) -0.01(2) 0.048(17) 0.04(2) C75 0.15(2) 0.10(2) 0.13(2) -0.02(2) 0.03(2) 0.07(2) C76 0.19(3) 0.09(3) 0.13(2) -0.03(2) -0.01(2) 0.03(2) C77 0.15(2) 0.08(2) 0.100(18) 0.006(18) 0.003(18) 0.04(2) O81 0.088(12) 0.12(2) 0.074(11) -0.020(11) 0.030(9) -0.013(12) C82 0.081(15) 0.14(3) 0.064(14) -0.011(16) 0.024(12) -0.005(18) C83 0.094(19) 0.13(2) 0.090(17) -0.022(17) 0.003(15) 0.033(18) C84 0.14(2) 0.12(3) 0.071(15) -0.007(16) 0.026(15) -0.02(2) C85 0.13(2) 0.12(3) 0.045(12) -0.024(15) 0.012(13) -0.005(19) C86 0.13(2) 0.13(2) 0.064(14) -0.022(16) 0.012(14) 0.002(19) C87 0.089(16) 0.11(2) 0.090(16) -0.015(17) 0.021(13) 0.006(18) O91 0.070(10) 0.105(18) 0.100(13) 0.027(12) 0.026(10) 0.024(11) C92 0.14(2) 0.16(3) 0.074(15) -0.017(17) 0.066(15) 0.00(2) C93 0.105(19) 0.16(3) 0.098(18) 0.031(19) 0.044(15) -0.01(2) C94 0.13(2) 0.19(3) 0.10(2) 0.04(2) 0.037(18) 0.04(2) C95 0.12(2) 0.20(3) 0.13(2) 0.05(2) 0.084(18) 0.02(2) C96 0.078(17) 0.22(3) 0.14(2) 0.03(2) 0.051(17) 0.02(2) C97 0.11(2) 0.21(3) 0.095(19) 0.04(2) 0.034(16) 0.02(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 C11 1.85(5) . ? Mo1 C21 1.92(4) . ? Mo1 C100 1.96(3) . ? Mo1 P4 2.505(8) . ? Mo1 P7 2.523(8) . ? Mo1 I2 2.833(5) . ? Mo1 I3 2.844(4) . ? C21 C11 1.39(2) . ? C21 C22 1.44(4) . ? O100 C100 1.34(4) . ? C11 C12 1.57(5) . ? C12 C13 1.3900 . ? C12 C17 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? P4 O61 1.61(2) . ? P4 O51 1.62(2) . ? P4 O41 1.65(2) . ? O41 C42 1.40(3) . ? C42 C47 1.27(5) . ? C42 C43 1.45(5) . ? C43 C44 1.39(5) . ? C44 C45 1.47(6) . ? C45 C46 1.26(5) . ? C46 C47 1.32(5) . ? O51 C52 1.42(4) . ? C52 C57 1.35(4) . ? C52 C53 1.42(5) . ? C53 C54 1.39(6) . ? C54 C55 1.33(6) . ? C55 C56 1.38(6) . ? C56 C57 1.40(6) . ? O61 C62 1.48(4) . ? C62 C67 1.28(5) . ? C62 C63 1.34(5) . ? C63 C64 1.64(6) . ? C64 C66 1.25(6) . ? C65 C66 1.21(6) . ? C65 C67 1.51(6) . ? P7 O91 1.60(2) . ? P7 O71 1.61(2) . ? P7 O81 1.62(2) . ? O71 C72 1.36(3) . ? C72 C73 1.3900 . ? C72 C77 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? O81 C82 1.47(3) . ? C82 C87 1.33(5) . ? C82 C83 1.36(5) . ? C83 C84 1.38(4) . ? C84 C85 1.39(5) . ? C85 C86 1.39(5) . ? C86 C87 1.37(4) . ? O91 C92 1.42(4) . ? C92 C97 1.35(5) . ? C92 C93 1.41(5) . ? C93 C94 1.30(6) . ? C94 C95 1.34(6) . ? C95 C96 1.35(6) . ? C96 C97 1.44(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 C11 Mo1 C21 43.0(9) . . ? C11 Mo1 C100 72.2(15) . . ? C21 Mo1 C100 115.0(14) . . ? C11 Mo1 P4 94.9(15) . . ? C21 Mo1 P4 98.5(12) . . ? C100 Mo1 P4 88.1(9) . . ? C11 Mo1 P7 91.7(15) . . ? C21 Mo1 P7 85.2(12) . . ? C100 Mo1 P7 95.5(9) . . ? P4 Mo1 P7 173.2(3) . . ? C11 Mo1 I2 148.2(13) . . ? C21 Mo1 I2 165.5(11) . . ? C100 Mo1 I2 76.7(9) . . ? P4 Mo1 I2 90.2(2) . . ? P7 Mo1 I2 85.1(2) . . ? C11 Mo1 I3 126.0(13) . . ? C21 Mo1 I3 83.5(11) . . ? C100 Mo1 I3 160.9(8) . . ? P4 Mo1 I3 84.8(2) . . ? P7 Mo1 I3 90.0(2) . . ? I22 Mo1 I3 85.65(15) . . ? C11 C21 C22 138(4) . . ? C11 C21 Mo1 66(3) . . ? C22 C21 Mo1 156(3) . . ? O100 C100 Mo1 170(2) . . ? C21 C11 C12 132(4) . . ? C21 C11 Mo1 71(3) . . ? C12 C11 Mo1 157(3) . . ? C13 C12 C17 120.0 . . ? C13 C12 C11 130(2) . . ? C17 C12 C11 110(2) . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C12 120.0 . . ? O61 P4 O51 100.2(12) . . ? O61 P4 O41 104.3(12) . . ? O51 P4 O41 100.9(12) . . ? O61 P4 Mo1 121.9(8) . . ? O51 P4 Mo1 120.0(9) . . ? O41 P4 Mo1 106.8(8) . . ? C42 O41 P4 123(2) . . ? C47 C42 O41 127(3) . . ? C47 C42 C43 120(3) . . ? O41 C42 C43 112(3) . . ? C44 C43 C42 118(4) . . ? C43 C44 C45 115(4) . . ? C46 C45 C44 120(3) . . ? C45 C46 C47 124(4) . . ? C42 C47 C46 122(4) . . ? C52 O51 P4 128(2) . . ? C57 C52 C53 127(3) . . ? C57 C52 O51 118(3) . . ? C53 C52 O51 115(3) . . ? C54 C53 C52 109(4) . . ? C55 C54 C53 127(4) . . ? C54 C55 C56 120(4) . . ? C55 C56 C57 117(3) . . ? C52 C57 C56 119(3) . . ? C62 O61 P4 131(2) . . ? C67 C62 C63 131(4) . . ? C67 C62 O61 121(4) . . ? C63 C62 O61 107(3) . . ? C62 C63 C64 105(3) . . ? C66 C64 C63 118(4) . . ? C66 C65 C67 112(5) . . ? C65 C66 C64 134(5) . . ? C62 C67 C65 119(4) . . ? O91 P7 O71 98.1(12) . . ? O91 P7 O81 101.3(11) . . ? O71 P7 O81 106.3(13) . . ? O91 P7 Mo1 120.5(8) . . ? O71 P7 Mo1 122.1(8) . . ? O81 P7 Mo1 106.1(8) . . ? C72 O71 P7 125.5(18) . . ? O71 C72 C73 122(2) . . ? O71 C72 C77 118(2) . . ? C73 C72 C77 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C76 C75 C74 120.0 . . ? C77 C76 C75 120.0 . . ? C76 C77 C72 120.0 . . ? C82 O81 P7 124.3(19) . . ? C87 C82 C83 122(3) . . ? C87 C82 O81 116(3) . . ? C83 C82 O81 122(4) . . ? C82 C83 C84 121(4) . . ? C83 C84 C85 115(4) . . ? C84 C85 C86 126(3) . . ? C87 C86 C85 114(4) . . ? C82 C87 C86 122(4) . . ? C92 O91 P7 129(2) . . ? C97 C92 C93 129(4) . . ? C97 C92 O91 115(4) . . ? C93 C92 O91 116(3) . . ? C94 C93 C92 113(4) . . ? C93 C94 C95 125(4) . . ? C94 C95 C96 120(4) . . ? C95 C96 C97 122(3) . . ? C92 C97 C96 111(4) . . ? _refine_diff_density_max 1.077 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.157 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Mo(MeCCMe)(CO)I2(P(OMe)3)2 _chemical_formula_sum 'C11 H24 I2 Mo O7 P2' _chemical_formula_weight 679.98 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 20.52(2) _cell_length_b 15.400(17) _cell_length_c 14.286(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4514(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 3.482 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.265 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12203 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4198 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+11.3521P] 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 0.00052(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4198 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.163 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.35064(3) 0.24433(4) 0.51703(6) 0.0484(3) Uani 1 d . . . C22 C 0.3715(7) 0.1297(8) 0.3157(8) 0.085(3) Uani 1 d . . . H1A H 0.3855 0.0728 0.3342 0.102 Uiso 1 calc R . . H1B H 0.4083 0.1623 0.2938 0.102 Uiso 1 calc R . . H1C H 0.3398 0.1249 0.2664 0.102 Uiso 1 calc R . . C21 C 0.3419(5) 0.1750(5) 0.3975(6) 0.061(2) Uani 1 d . . . C11 C 0.2829(5) 0.1944(6) 0.4286(7) 0.073(3) Uani 1 d . . . C12 C 0.2146(6) 0.1835(8) 0.3984(11) 0.107(4) Uani 1 d . . . H4A H 0.1964 0.2392 0.3833 0.128 Uiso 1 calc R . . H4B H 0.1900 0.1574 0.4480 0.128 Uiso 1 calc R . . H4C H 0.2130 0.1467 0.3441 0.128 Uiso 1 calc R . . C100 C 0.2634(5) 0.2683(7) 0.5753(8) 0.076(3) Uani 1 d . . . O100 O 0.2137(4) 0.2767(7) 0.6076(8) 0.116(3) Uani 1 d . . . I2 I 0.36321(3) 0.11586(4) 0.65688(5) 0.0668(3) Uani 1 d . . . I3 I 0.39214(4) 0.37167(4) 0.64904(5) 0.0782(3) Uani 1 d . . . P4 P 0.34974(10) 0.37848(13) 0.42237(18) 0.0552(6) Uani 1 d . . . O41 O 0.3273(4) 0.3547(4) 0.3198(5) 0.0752(18) Uani 1 d . . . C42 C 0.3194(6) 0.4185(8) 0.2460(8) 0.087(3) Uani 1 d . . . H12A H 0.2744 0.4351 0.2416 0.104 Uiso 1 calc R . . H12B H 0.3332 0.3939 0.1875 0.104 Uiso 1 calc R . . H12C H 0.3454 0.4686 0.2600 0.104 Uiso 1 calc R . . O51 O 0.4167(3) 0.4274(4) 0.4097(5) 0.0746(18) Uani 1 d . . . C52 C 0.4296(6) 0.5165(7) 0.4134(10) 0.099(4) Uani 1 d . . . H22A H 0.3998 0.5467 0.3730 0.119 Uiso 1 calc R . . H22B H 0.4735 0.5271 0.3932 0.119 Uiso 1 calc R . . H22C H 0.4243 0.5368 0.4765 0.119 Uiso 1 calc R . . O61 O 0.3051(3) 0.4585(4) 0.4496(6) 0.081(2) Uani 1 d . . . C62 C 0.2378(6) 0.4515(9) 0.4630(14) 0.148(8) Uani 1 d . . . H32A H 0.2160 0.4967 0.4288 0.178 Uiso 1 calc R . . H32B H 0.2281 0.4570 0.5284 0.178 Uiso 1 calc R . . H32C H 0.2231 0.3960 0.4409 0.178 Uiso 1 calc R . . P7 P 0.46839(11) 0.21974(15) 0.47609(16) 0.0546(5) Uani 1 d . . . O71 O 0.4825(4) 0.1197(4) 0.4664(5) 0.079(2) Uani 1 d . . . C72 C 0.5436(7) 0.0845(9) 0.4321(12) 0.125(6) Uani 1 d . . . H42A H 0.5465 0.0938 0.3658 0.150 Uiso 1 calc R . . H42B H 0.5453 0.0234 0.4450 0.150 Uiso 1 calc R . . H42C H 0.5793 0.1130 0.4628 0.150 Uiso 1 calc R . . O81 O 0.4889(3) 0.2590(4) 0.3782(5) 0.0634(15) Uani 1 d . . . C82 C 0.5469(5) 0.3096(8) 0.3582(7) 0.082(3) Uani 1 d . . . H52A H 0.5459 0.3283 0.2941 0.098 Uiso 1 calc R . . H52B H 0.5849 0.2746 0.3687 0.098 Uiso 1 calc R . . H52C H 0.5482 0.3594 0.3985 0.098 Uiso 1 calc R . . O91 O 0.5270(3) 0.2554(4) 0.5376(5) 0.0748(19) Uani 1 d . . . C92 C 0.5403(6) 0.2235(10) 0.6324(7) 0.099(4) Uani 1 d . . . H62A H 0.5845 0.2370 0.6493 0.119 Uiso 1 calc R . . H62B H 0.5340 0.1618 0.6343 0.119 Uiso 1 calc R . . H62C H 0.5111 0.2510 0.6757 0.119 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0424(4) 0.0423(4) 0.0605(5) 0.0010(3) 0.0027(3) -0.0007(3) C22 0.097(8) 0.087(8) 0.070(7) -0.015(5) 0.013(6) -0.005(6) C21 0.077(6) 0.044(4) 0.061(5) -0.007(4) -0.014(4) -0.014(4) C11 0.081(6) 0.059(5) 0.079(7) 0.012(5) -0.021(5) -0.015(5) C12 0.076(7) 0.090(9) 0.154(13) 0.008(8) -0.036(8) -0.016(6) C100 0.052(5) 0.078(6) 0.098(8) 0.025(6) 0.012(5) 0.007(5) O100 0.062(5) 0.145(8) 0.140(8) 0.034(7) 0.038(5) 0.027(5) I2 0.0685(5) 0.0619(4) 0.0700(5) 0.0117(3) 0.0065(3) 0.0027(3) I3 0.0979(6) 0.0640(5) 0.0727(5) -0.0175(3) 0.0062(3) -0.0093(3) P4 0.0473(11) 0.0445(11) 0.0737(16) 0.0048(9) 0.0030(10) 0.0027(8) O41 0.097(5) 0.052(4) 0.076(4) 0.012(3) -0.001(4) -0.007(4) C42 0.090(7) 0.087(8) 0.083(7) 0.015(6) -0.019(6) -0.001(6) O51 0.058(3) 0.048(3) 0.117(6) 0.018(3) 0.006(3) -0.007(3) C52 0.087(8) 0.064(7) 0.146(12) 0.016(7) -0.027(7) -0.026(6) O61 0.076(4) 0.058(4) 0.110(6) 0.011(4) 0.011(4) 0.011(3) C62 0.067(8) 0.093(9) 0.28(2) 0.059(12) 0.065(11) 0.034(7) P7 0.0455(11) 0.0594(12) 0.0589(13) 0.0037(10) 0.0038(9) 0.0049(10) O71 0.076(5) 0.060(4) 0.103(6) 0.012(3) 0.026(4) 0.025(3) C72 0.110(10) 0.088(9) 0.177(15) 0.018(9) 0.074(10) 0.038(8) O81 0.056(3) 0.078(4) 0.056(4) 0.010(3) -0.001(3) -0.006(3) C82 0.064(6) 0.100(8) 0.082(7) 0.006(6) 0.009(5) -0.020(6) O91 0.053(4) 0.109(6) 0.062(4) 0.011(3) -0.004(3) -0.013(3) C92 0.073(7) 0.169(13) 0.056(6) 0.017(7) -0.020(5) -0.013(8) _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 C100 2.010(10) . ? Mo1 C21 2.022(9) . ? Mo1 C11 2.027(10) . ? Mo1 P4 2.469(3) . ? Mo1 P7 2.516(3) . ? Mo1 I2 2.823(2) . ? Mo1 I3 2.849(2) . ? C22 C21 1.491(14) . ? C21 C11 1.324(15) . ? C11 C12 1.476(14) . ? C100 O100 1.127(12) . ? P4 O41 1.578(8) . ? P4 O51 1.578(6) . ? P4 O61 1.584(7) . ? O41 C42 1.450(12) . ? O51 C52 1.398(11) . ? O61 C62 1.400(14) . ? P7 O71 1.573(6) . ? P7 O81 1.581(7) . ? P7 O91 1.586(7) . ? O71 C72 1.452(12) . ? O81 C82 1.451(12) . ? O91 C92 1.466(12) . ? 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 C100 Mo1 C21 111.7(5) . . ? C100 Mo1 C11 73.6(5) . . ? C21 Mo1 C11 38.2(4) . . ? C100 Mo1 P4 93.9(3) . . ? C21 Mo1 P4 88.8(3) . . ? C11 Mo1 P4 88.4(3) . . ? C100 Mo1 P7 168.7(4) . . ? C21 Mo1 P7 78.9(3) . . ? C11 Mo1 P7 117.1(4) . . ? P4 Mo1 P7 90.27(8) . . ? C100 Mo1 I2 85.2(3) . . ? C21 Mo1 I2 103.6(3) . . ? C11 Mo1 I2 103.7(3) . . ? P4 Mo1 I2 167.03(7) . . ? P7 Mo1 I2 88.43(6) . . ? C100 Mo1 I3 82.2(4) . . ? C21 Mo1 I3 161.5(3) . . ? C11 Mo1 I3 151.2(3) . . ? P4 Mo1 I3 77.79(10) . . ? P7 Mo1 I3 88.40(8) . . ? I2 Mo1 I3 89.27(9) . . ? C11 C21 C22 138.0(10) . . ? C11 C21 Mo1 71.1(6) . . ? C22 C21 Mo1 150.8(8) . . ? C21 C11 C12 138.1(11) . . ? C21 C11 Mo1 70.7(6) . . ? C12 C11 Mo1 151.0(10) . . ? O100 C100 Mo1 175.9(11) . . ? O41 P4 O51 104.9(4) . . ? O41 P4 O61 104.0(4) . . ? O51 P4 O61 99.2(4) . . ? O41 P4 Mo1 108.4(3) . . ? O51 P4 Mo1 117.2(3) . . ? O61 P4 Mo1 121.3(3) . . ? C42 O41 P4 123.3(7) . . ? C52 O51 P4 129.0(7) . . ? C62 O61 P4 123.0(8) . . ? O71 P7 O81 104.3(4) . . ? O71 P7 O91 104.3(4) . . ? O81 P7 O91 98.9(4) . . ? O71 P7 Mo1 110.2(3) . . ? O81 P7 Mo1 113.9(3) . . ? O91 P7 Mo1 123.1(3) . . ? C72 O71 P7 123.7(7) . . ? C82 O81 P7 126.8(6) . . ? C92 O91 P7 122.4(7) . . ? _refine_diff_density_max 1.344 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.169 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety W(CO)(MeCCMe)I2(P(OEt)3)2 _chemical_formula_sum 'C17 H36 I2 O7 P2 W' _chemical_formula_weight 852.05 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.133(12) _cell_length_b 40.22(5) _cell_length_c 19.49(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.806(10) _cell_angle_gamma 90.00 _cell_volume 8710(17) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4848 _exptl_absorpt_coefficient_mu 6.245 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.327 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14473 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.92 _reflns_number_total 8573 _reflns_number_gt 4972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. there were 3 molecules in the asymmetric unit. The structure was close to C2/c with one molecule in an 8-fold general position and one in a 4-fold position with an imposed 2-fold axis but attempts to refine in this spacegroup proved unsuccessful. A solution in Cc was thus sought with three independent molecules in the asymmetric unit. Each molecule was consistent with 2-fold symmetry apart from the carbonyl and dimethylacetylene moieties which were disordered over two sites. This was treated by refining two disordered overlapping positions for each moiety. Each group was given 50% occupancy in each of two positions and constraining the distances in each coordinate group. The refined models each had approximate two-fold symmetry. Only the W, I and P atoms were refined anisotropically. Atoms are named accordingly. The three molecules are called A, B and C and atoms named D, E or F are disordered atoms in molecules A, B and C respectively. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 8573 _refine_ls_number_parameters 493 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.3847 _refine_ls_wR_factor_gt 0.3344 _refine_ls_goodness_of_fit_ref 1.300 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.216 _refine_ls_shift/su_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1A W 0.00665(11) 0.30350(3) 0.24540(7) 0.0529(5) Uani 1 d D . . I3A I 0.1592(3) 0.25135(9) 0.19891(18) 0.0837(11) Uani 1 d . . . I2A I -0.1432(3) 0.25225(9) 0.29091(19) 0.0863(11) Uani 1 d . . . P4A P -0.1190(9) 0.30197(15) 0.1344(6) 0.043(2) Uani 1 d . . . C10A C -0.119(4) 0.3253(11) 0.301(3) 0.047(3) Uiso 0.50 d PD A 1 O10A O -0.175(3) 0.3455(8) 0.3229(19) 0.047(3) Uiso 0.50 d PD A 1 C22A C 0.171(4) 0.3492(12) 0.141(2) 0.047(3) Uiso 0.50 d PD A 1 H22A H 0.2224 0.3670 0.1580 0.056 Uiso 0.50 calc PR A 1 H22B H 0.1221 0.3568 0.1017 0.056 Uiso 0.50 calc PR A 1 H22C H 0.2199 0.3309 0.1278 0.056 Uiso 0.50 calc PR A 1 C21A C 0.093(4) 0.3383(6) 0.196(2) 0.047(3) Uiso 0.50 d PD A 1 C11A C 0.021(4) 0.3534(5) 0.236(2) 0.047(3) Uiso 0.50 d PD A 1 C12A C -0.014(4) 0.3898(7) 0.238(3) 0.047(3) Uiso 0.50 d PD A 1 H12A H 0.0568 0.4033 0.2446 0.056 Uiso 0.50 calc PR A 1 H12B H -0.0660 0.3936 0.2742 0.056 Uiso 0.50 calc PR A 1 H12C H -0.0559 0.3957 0.1945 0.056 Uiso 0.50 calc PR A 1 C10D C 0.128(4) 0.3304(10) 0.201(3) 0.047(3) Uiso 0.50 d PD A 2 O10D O 0.187(3) 0.3514(7) 0.1899(19) 0.047(3) Uiso 0.50 d PD A 2 C22D C -0.193(4) 0.3388(12) 0.342(3) 0.047(3) Uiso 0.50 d PD A 2 H22A H -0.1768 0.3564 0.3750 0.056 Uiso 0.50 calc PR A 2 H22B H -0.2091 0.3186 0.3664 0.056 Uiso 0.50 calc PR A 2 H22C H -0.2610 0.3445 0.3121 0.056 Uiso 0.50 calc PR A 2 C21D C -0.087(4) 0.3339(6) 0.302(2) 0.047(3) Uiso 0.50 d PD A 2 C11D C -0.018(4) 0.3520(5) 0.265(2) 0.047(3) Uiso 0.50 d PD A 2 C12D C 0.033(4) 0.3864(8) 0.273(3) 0.047(3) Uiso 0.50 d PD A 2 H12A H -0.0275 0.4009 0.2899 0.056 Uiso 0.50 calc PR A 2 H12B H 0.0562 0.3943 0.2298 0.056 Uiso 0.50 calc PR A 2 H12C H 0.1015 0.3861 0.3058 0.056 Uiso 0.50 calc PR A 2 O41A O -0.261(2) 0.2954(7) 0.1342(15) 0.062(6) Uiso 1 d . . . C42A C -0.324(3) 0.3195(9) 0.180(2) 0.063(9) Uiso 1 d . . . H42A H -0.2926 0.3418 0.1745 0.076 Uiso 1 calc R . . H42B H -0.3104 0.3130 0.2278 0.076 Uiso 1 calc R . . C43A C -0.456(4) 0.3184(11) 0.158(2) 0.081(11) Uiso 1 d . . . H43A H -0.4780 0.2961 0.1451 0.098 Uiso 1 calc R . . H43B H -0.4722 0.3330 0.1199 0.098 Uiso 1 calc R . . H43C H -0.5013 0.3253 0.1959 0.098 Uiso 1 calc R . . O51A O -0.084(2) 0.2744(6) 0.0759(16) 0.066(7) Uiso 1 d . . . C52A C -0.119(4) 0.2385(11) 0.086(3) 0.083(13) Uiso 1 d . . . H52A H -0.0821 0.2302 0.1287 0.100 Uiso 1 calc R . . H52B H -0.2057 0.2369 0.0873 0.100 Uiso 1 calc R . . C53A C -0.081(3) 0.2194(9) 0.031(2) 0.067(8) Uiso 1 d . . . H53A H -0.1351 0.2229 -0.0091 0.080 Uiso 1 calc R . . H53B H -0.0813 0.1963 0.0432 0.080 Uiso 1 calc R . . H53C H -0.0013 0.2260 0.0208 0.080 Uiso 1 calc R . . O61A O -0.090(2) 0.3344(6) 0.0866(14) 0.064(6) Uiso 1 d . . . C62A C -0.166(4) 0.3477(9) 0.036(2) 0.076(10) Uiso 1 d . . . H62A H -0.1685 0.3317 -0.0015 0.091 Uiso 1 calc R . . H62B H -0.2455 0.3473 0.0536 0.091 Uiso 1 calc R . . C63A C -0.158(5) 0.3741(14) 0.010(3) 0.115(17) Uiso 1 d . . . H63A H -0.0901 0.3858 0.0310 0.138 Uiso 1 calc R . . H63B H -0.2300 0.3866 0.0149 0.138 Uiso 1 calc R . . H63C H -0.1464 0.3712 -0.0385 0.138 Uiso 1 calc R . . P7A P 0.1342(8) 0.3007(2) 0.3601(5) 0.048(2) Uani 1 d . . . O71A O 0.114(2) 0.2741(6) 0.4121(15) 0.061(6) Uiso 1 d . . . C72A C 0.142(3) 0.2406(9) 0.414(2) 0.071(10) Uiso 1 d D . . H72A H 0.2241 0.2374 0.4324 0.086 Uiso 1 calc R . . H72B H 0.1330 0.2311 0.3685 0.086 Uiso 1 calc R . . C73A C 0.055(4) 0.2232(10) 0.461(2) 0.083(11) Uiso 1 d D . . H73A H 0.0743 0.2295 0.5083 0.100 Uiso 1 calc R . . H73B H 0.0624 0.1995 0.4569 0.100 Uiso 1 calc R . . H73C H -0.0265 0.2297 0.4482 0.100 Uiso 1 calc R . . O81A O 0.277(3) 0.2958(7) 0.3612(16) 0.071(7) Uiso 1 d . . . C82A C 0.367(3) 0.3122(8) 0.3223(19) 0.059(8) Uiso 1 d . . . H82A H 0.3578 0.3042 0.2754 0.070 Uiso 1 calc R . . H82B H 0.3491 0.3358 0.3212 0.070 Uiso 1 calc R . . C83A C 0.491(5) 0.3087(12) 0.345(3) 0.097(15) Uiso 1 d . . . H83A H 0.5022 0.3152 0.3924 0.116 Uiso 1 calc R . . H83B H 0.5392 0.3225 0.3177 0.116 Uiso 1 calc R . . H83C H 0.5147 0.2859 0.3403 0.116 Uiso 1 calc R . . O91A O 0.130(3) 0.3373(8) 0.3891(17) 0.088(9) Uiso 1 d . . . C92A C 0.170(4) 0.3390(9) 0.472(2) 0.082(11) Uiso 1 d D . . H92A H 0.1179 0.3265 0.5000 0.098 Uiso 1 calc R . . H92B H 0.2539 0.3330 0.4824 0.098 Uiso 1 calc R . . C93A C 0.148(7) 0.3768(10) 0.474(4) 0.15(3) Uiso 1 d D . . H93A H 0.2240 0.3882 0.4787 0.181 Uiso 1 calc R . . H93B H 0.1017 0.3820 0.5121 0.181 Uiso 1 calc R . . H93C H 0.1051 0.3836 0.4319 0.181 Uiso 1 calc R . . W1B W 0.51710(10) 0.13694(3) 0.23467(7) 0.0568(6) Uani 1 d D . . I2B I 0.3623(3) 0.08775(9) 0.2852(2) 0.0886(11) Uani 1 d . . . I3B I 0.6641(3) 0.08282(9) 0.19296(18) 0.0841(11) Uani 1 d . . . P4B P 0.3930(9) 0.13513(17) 0.1234(6) 0.048(3) Uani 1 d . . . C10B C 0.647(3) 0.1599(12) 0.185(2) 0.047(3) Uiso 0.50 d PD B 1 O10B O 0.694(3) 0.1755(8) 0.1474(18) 0.047(3) Uiso 0.50 d PD B 1 C22B C 0.348(4) 0.1847(12) 0.334(2) 0.047(3) Uiso 0.50 d PD B 1 H22D H 0.3945 0.2001 0.3625 0.056 Uiso 0.50 calc PR B 1 H22E H 0.3260 0.1660 0.3614 0.056 Uiso 0.50 calc PR B 1 H22F H 0.2763 0.1955 0.3151 0.056 Uiso 0.50 calc PR B 1 C21B C 0.421(3) 0.1729(6) 0.277(2) 0.047(3) Uiso 0.50 d PD B 1 C11B C 0.504(4) 0.1869(5) 0.243(3) 0.047(3) Uiso 0.50 d PD B 1 C12B C 0.514(4) 0.2207(8) 0.210(3) 0.047(3) Uiso 0.50 d PD B 1 H12D H 0.4823 0.2373 0.2394 0.056 Uiso 0.50 calc PR B 1 H12E H 0.4680 0.2209 0.1663 0.056 Uiso 0.50 calc PR B 1 H12F H 0.5964 0.2255 0.2031 0.056 Uiso 0.50 calc PR B 1 C10E C 0.400(4) 0.1572(12) 0.297(2) 0.047(3) Uiso 0.50 d PD C 2 O10E O 0.326(3) 0.1725(8) 0.3170(18) 0.047(3) Uiso 0.50 d PD C 2 C22E C 0.703(3) 0.1868(13) 0.174(3) 0.047(3) Uiso 0.50 d PD B 2 H22D H 0.7494 0.1900 0.2171 0.056 Uiso 0.50 calc PR B 2 H22E H 0.7015 0.2072 0.1485 0.056 Uiso 0.50 calc PR B 2 H22F H 0.7401 0.1697 0.1483 0.056 Uiso 0.50 calc PR B 2 C21E C 0.580(3) 0.1769(7) 0.1874(17) 0.047(3) Uiso 0.50 d PD B 2 C11E C 0.499(3) 0.1864(5) 0.230(2) 0.047(3) Uiso 0.50 d PD B 2 C12E C 0.493(4) 0.1825(12) 0.3063(18) 0.047(3) Uiso 0.50 d PD B 2 H12D H 0.4281 0.1678 0.3155 0.056 Uiso 0.50 calc PR B 2 H12E H 0.4792 0.2038 0.3265 0.056 Uiso 0.50 calc PR B 2 H12F H 0.5674 0.1735 0.3255 0.056 Uiso 0.50 calc PR B 2 O41B O 0.251(2) 0.1281(7) 0.1221(15) 0.063(6) Uiso 1 d . . . C42B C 0.195(4) 0.1518(12) 0.167(3) 0.094(14) Uiso 1 d . . . H42C H 0.2245 0.1741 0.1588 0.113 Uiso 1 calc R . . H42D H 0.2126 0.1461 0.2146 0.113 Uiso 1 calc R . . C43B C 0.055(5) 0.1495(13) 0.147(3) 0.101(15) Uiso 1 d . . . H43D H 0.0347 0.1639 0.1085 0.121 Uiso 1 calc R . . H43E H 0.0115 0.1561 0.1853 0.121 Uiso 1 calc R . . H43F H 0.0346 0.1270 0.1342 0.121 Uiso 1 calc R . . O51B O 0.432(2) 0.1073(6) 0.0640(14) 0.057(6) Uiso 1 d . . . C52B C 0.393(5) 0.0698(11) 0.071(3) 0.095(14) Uiso 1 d . . . H52C H 0.4263 0.0611 0.1144 0.114 Uiso 1 calc R . . H52D H 0.3056 0.0687 0.0712 0.114 Uiso 1 calc R . . C53B C 0.426(4) 0.0515(11) 0.022(3) 0.093(12) Uiso 1 d . . . H53D H 0.4315 0.0288 0.0376 0.112 Uiso 1 calc R . . H53E H 0.5041 0.0587 0.0097 0.112 Uiso 1 calc R . . H53F H 0.3694 0.0532 -0.0166 0.112 Uiso 1 calc R . . O61B O 0.4210(17) 0.1675(5) 0.0780(11) 0.044(4) Uiso 1 d . . . C62B C 0.347(5) 0.1779(12) 0.024(3) 0.098(14) Uiso 1 d . . . H62C H 0.3783 0.1686 -0.0170 0.118 Uiso 1 calc R . . H62D H 0.2695 0.1673 0.0291 0.118 Uiso 1 calc R . . C63B C 0.325(5) 0.2090(12) 0.011(3) 0.097(13) Uiso 1 d . . . H63D H 0.2411 0.2135 0.0163 0.116 Uiso 1 calc R . . H63E H 0.3435 0.2140 -0.0351 0.116 Uiso 1 calc R . . H63F H 0.3731 0.2226 0.0426 0.116 Uiso 1 calc R . . P7B P 0.6472(8) 0.1351(3) 0.3470(6) 0.057(3) Uani 1 d . . . O81B O 0.794(2) 0.1305(7) 0.3471(15) 0.061(6) Uiso 1 d . . . C82B C 0.871(3) 0.1448(9) 0.312(2) 0.068(9) Uiso 1 d . . . H82C H 0.8452 0.1676 0.3041 0.082 Uiso 1 calc R . . H82D H 0.8687 0.1341 0.2670 0.082 Uiso 1 calc R . . C83B C 1.001(5) 0.1455(13) 0.340(3) 0.104(16) Uiso 1 d . . . H83D H 1.0071 0.1588 0.3810 0.125 Uiso 1 calc R . . H83E H 1.0498 0.1550 0.3064 0.125 Uiso 1 calc R . . H83F H 1.0270 0.1233 0.3506 0.125 Uiso 1 calc R . . O91B O 0.626(2) 0.1081(7) 0.4019(16) 0.066(7) Uiso 1 d . . . C92B C 0.651(3) 0.0745(9) 0.399(2) 0.067(10) Uiso 1 d . . . H92C H 0.7357 0.0703 0.4118 0.081 Uiso 1 calc R . . H92D H 0.6313 0.0657 0.3538 0.081 Uiso 1 calc R . . C93B C 0.566(4) 0.0580(11) 0.455(2) 0.085(11) Uiso 1 d . . . H93D H 0.5771 0.0699 0.4981 0.102 Uiso 1 calc R . . H93E H 0.5883 0.0351 0.4626 0.102 Uiso 1 calc R . . H93F H 0.4834 0.0593 0.4385 0.102 Uiso 1 calc R . . O71B O 0.6411(19) 0.1704(5) 0.3761(12) 0.055(5) Uiso 1 d . . . C72B C 0.675(4) 0.1726(10) 0.459(3) 0.092(13) Uiso 1 d . . . H72C H 0.6262 0.1574 0.4846 0.110 Uiso 1 calc R . . H72D H 0.7594 0.1680 0.4707 0.110 Uiso 1 calc R . . C73B C 0.642(6) 0.2114(13) 0.475(4) 0.14(2) Uiso 1 d . . . H73D H 0.7114 0.2226 0.4949 0.162 Uiso 1 calc R . . H73E H 0.5781 0.2123 0.5055 0.162 Uiso 1 calc R . . H73F H 0.6158 0.2222 0.4321 0.162 Uiso 1 calc R . . W1C W 0.51626(18) 0.47023(5) 0.23645(11) 0.0803(8) Uani 1 d D . . I2C I 0.3716(4) 0.41761(11) 0.2818(2) 0.1069(15) Uani 1 d . . . I3C I 0.6710(4) 0.41859(10) 0.1889(2) 0.1051(14) Uani 1 d . . . P4C P 0.3888(14) 0.4673(2) 0.1263(9) 0.094(5) Uani 1 d . . . C10C C 0.627(7) 0.4992(16) 0.184(4) 0.094(7) Uiso 0.50 d PD D 1 O10C O 0.681(5) 0.5096(13) 0.143(2) 0.094(7) Uiso 0.50 d PD D 1 C22C C 0.331(7) 0.507(2) 0.340(4) 0.094(7) Uiso 0.50 d PD D 1 H22G H 0.3665 0.5249 0.3683 0.113 Uiso 0.50 calc PR D 1 H22H H 0.3257 0.4876 0.3674 0.113 Uiso 0.50 calc PR D 1 H22I H 0.2515 0.5140 0.3232 0.113 Uiso 0.50 calc PR D 1 C21C C 0.406(6) 0.5009(9) 0.282(4) 0.094(7) Uiso 0.50 d PD D 1 C11C C 0.480(6) 0.5186(6) 0.246(4) 0.094(7) Uiso 0.50 d PD D 1 C12C C 0.491(7) 0.5555(8) 0.236(4) 0.094(7) Uiso 0.50 d PD D 1 H12G H 0.4987 0.5603 0.1886 0.113 Uiso 0.50 calc PR D 1 H12H H 0.5612 0.5634 0.2628 0.113 Uiso 0.50 calc PR D 1 H12I H 0.4209 0.5663 0.2516 0.113 Uiso 0.50 calc PR D 1 C10F C 0.393(6) 0.4892(19) 0.297(4) 0.094(7) Uiso 0.50 d PD E 2 O10F O 0.321(4) 0.5043(15) 0.318(3) 0.094(7) Uiso 0.50 d PD E 2 C22F C 0.703(6) 0.5247(16) 0.164(4) 0.094(7) Uiso 0.50 d PD D 2 H22G H 0.7262 0.5448 0.1877 0.113 Uiso 0.50 calc PR D 2 H22H H 0.6801 0.5298 0.1165 0.113 Uiso 0.50 calc PR D 2 H22I H 0.7693 0.5094 0.1659 0.113 Uiso 0.50 calc PR D 2 C21F C 0.599(6) 0.5093(9) 0.196(4) 0.094(7) Uiso 0.50 d PD D 2 C11F C 0.516(5) 0.5200(5) 0.235(3) 0.094(7) Uiso 0.50 d PD D 2 C12F C 0.480(7) 0.5123(19) 0.306(3) 0.094(7) Uiso 0.50 d PD D 2 H12G H 0.4206 0.5280 0.3185 0.113 Uiso 0.50 calc PR D 2 H12H H 0.5496 0.5138 0.3375 0.113 Uiso 0.50 calc PR D 2 H12I H 0.4475 0.4902 0.3067 0.113 Uiso 0.50 calc PR D 2 O41C O 0.247(3) 0.4598(9) 0.1250(19) 0.088(9) Uiso 1 d . . . C42C C 0.196(5) 0.4842(13) 0.164(3) 0.104(16) Uiso 1 d . . . H42E H 0.2237 0.5060 0.1505 0.125 Uiso 1 calc R . . H42F H 0.2177 0.4808 0.2121 0.125 Uiso 1 calc R . . C43C C 0.053(5) 0.4810(15) 0.148(3) 0.12(2) Uiso 1 d . . . H43G H 0.0277 0.4958 0.1115 0.147 Uiso 1 calc R . . H43H H 0.0135 0.4866 0.1887 0.147 Uiso 1 calc R . . H43I H 0.0337 0.4585 0.1349 0.147 Uiso 1 calc R . . O51C O 0.434(3) 0.4401(7) 0.0633(17) 0.077(8) Uiso 1 d . . . C52C C 0.389(5) 0.4056(11) 0.076(3) 0.088(14) Uiso 1 d . . . H52E H 0.4218 0.3975 0.1202 0.106 Uiso 1 calc R . . H52F H 0.3018 0.4055 0.0759 0.106 Uiso 1 calc R . . C53C C 0.428(4) 0.3857(11) 0.022(3) 0.094(12) Uiso 1 d . . . H53G H 0.3967 0.3635 0.0268 0.113 Uiso 1 calc R . . H53H H 0.5140 0.3850 0.0249 0.113 Uiso 1 calc R . . H53I H 0.3985 0.3948 -0.0210 0.113 Uiso 1 calc R . . O61C O 0.419(2) 0.4988(6) 0.0797(15) 0.074(7) Uiso 1 d . . . C62C C 0.341(5) 0.5120(12) 0.031(3) 0.096(13) Uiso 1 d . . . H62E H 0.3461 0.4977 -0.0091 0.115 Uiso 1 calc R . . H62F H 0.2618 0.5082 0.0471 0.115 Uiso 1 calc R . . C63C C 0.338(6) 0.5413(15) 0.007(3) 0.126(19) Uiso 1 d . . . H63G H 0.2931 0.5552 0.0360 0.151 Uiso 1 calc R . . H63H H 0.3002 0.5412 -0.0387 0.151 Uiso 1 calc R . . H63I H 0.4187 0.5496 0.0059 0.151 Uiso 1 calc R . . P7C P 0.6500(14) 0.4673(4) 0.3474(9) 0.101(5) Uani 1 d . . . O71C O 0.796(3) 0.4642(8) 0.3462(19) 0.088(9) Uiso 1 d . . . C72C C 0.879(5) 0.4835(13) 0.320(3) 0.115(18) Uiso 1 d . . . H72C H 0.8575 0.5065 0.3272 0.138 Uiso 1 calc R . . H72D H 0.8745 0.4800 0.2702 0.138 Uiso 1 calc R . . C73C C 0.998(6) 0.4794(15) 0.343(3) 0.13(2) Uiso 1 d . . . H73D H 1.0182 0.4954 0.3791 0.150 Uiso 1 calc R . . H73E H 1.0496 0.4827 0.3064 0.150 Uiso 1 calc R . . H73F H 1.0095 0.4574 0.3616 0.150 Uiso 1 calc R . . O81C O 0.631(3) 0.4406(8) 0.4023(18) 0.082(8) Uiso 1 d . . . C82C C 0.663(4) 0.4081(9) 0.397(2) 0.071(10) Uiso 1 d . . . H82E H 0.7461 0.4044 0.4123 0.085 Uiso 1 calc R . . H82F H 0.6474 0.3997 0.3506 0.085 Uiso 1 calc R . . C83C C 0.564(5) 0.3908(13) 0.454(3) 0.118(17) Uiso 1 d . . . H83G H 0.5583 0.4053 0.4926 0.142 Uiso 1 calc R . . H83H H 0.5936 0.3695 0.4691 0.142 Uiso 1 calc R . . H83I H 0.4856 0.3882 0.4306 0.142 Uiso 1 calc R . . O91C O 0.639(3) 0.5026(7) 0.3766(17) 0.088(8) Uiso 1 d . . . C92C C 0.667(5) 0.5071(10) 0.463(3) 0.097(14) Uiso 1 d D . . H92E H 0.6124 0.4939 0.4882 0.117 Uiso 1 calc R . . H92F H 0.7495 0.5009 0.4768 0.117 Uiso 1 calc R . . C93C C 0.647(7) 0.5447(11) 0.473(4) 0.15(3) Uiso 1 d D . . H93G H 0.7160 0.5543 0.4971 0.181 Uiso 1 calc R . . H93H H 0.5773 0.5479 0.4989 0.181 Uiso 1 calc R . . H93I H 0.6334 0.5552 0.4288 0.181 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1A 0.0456(7) 0.0508(8) 0.0622(12) 0.0002(8) 0.0032(6) 0.0052(7) I3A 0.0683(16) 0.105(2) 0.077(2) -0.0246(18) -0.0021(16) 0.0472(16) I2A 0.0742(18) 0.114(2) 0.070(2) 0.0286(19) 0.0012(16) -0.0305(17) P4A 0.050(5) 0.024(3) 0.055(6) 0.003(3) 0.008(5) 0.008(3) P7A 0.029(4) 0.079(6) 0.037(5) 0.004(4) 0.015(4) 0.002(3) W1B 0.0520(9) 0.0450(7) 0.0718(14) 0.0029(7) -0.0069(8) 0.0064(6) I2B 0.0736(18) 0.105(2) 0.086(3) 0.027(2) -0.0024(17) -0.0273(17) I3B 0.0837(19) 0.0853(18) 0.081(2) -0.0220(17) -0.0102(17) 0.0398(16) P4B 0.056(5) 0.026(3) 0.063(7) 0.001(3) 0.012(5) 0.009(3) P7B 0.033(4) 0.089(7) 0.048(6) -0.001(5) 0.002(4) 0.011(4) W1C 0.0799(12) 0.0589(9) 0.0987(19) 0.0050(10) -0.0190(12) 0.0050(9) I2C 0.109(3) 0.119(3) 0.091(3) 0.020(2) -0.007(2) -0.035(2) I3C 0.113(3) 0.108(2) 0.092(3) -0.008(2) -0.007(2) 0.042(2) P4C 0.113(10) 0.037(5) 0.125(12) 0.005(6) -0.038(9) 0.007(5) P7C 0.094(10) 0.089(9) 0.113(13) 0.009(8) -0.035(9) 0.007(7) _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 W1A C21D 1.986(18) . ? W1A C21A 1.987(18) . ? W1A C11D 2.011(18) . ? W1A C10D 1.982(17) . ? W1A C11A 2.021(18) . ? W1A C10A 2.027(17) . ? W1A P4A 2.497(11) . ? W1A P7A 2.570(11) . ? W1A I2A 2.831(4) . ? W1A I3A 2.883(4) . ? P4A O41A 1.61(3) . ? P4A O61A 1.65(3) . ? P4A O51A 1.66(3) . ? C10A O10A 1.123(17) . ? C22A C21A 1.488(18) . ? C21A C11A 1.310(17) . ? C11A C12A 1.520(18) . ? C10D O10D 1.092(17) . ? C22D C21D 1.473(18) . ? C21D C11D 1.306(18) . ? C11D C12D 1.498(18) . ? O41A C42A 1.52(5) . ? C42A C43A 1.50(5) . ? O51A C52A 1.51(5) . ? C52A C53A 1.40(6) . ? O61A C62A 1.37(4) . ? C62A C63A 1.19(6) . ? P7A O71A 1.50(3) . ? P7A O91A 1.58(3) . ? P7A O81A 1.61(3) . ? O71A C72A 1.38(5) . ? C72A C73A 1.543(19) . ? O81A C82A 1.45(5) . ? C82A C83A 1.42(6) . ? O91A C92A 1.65(5) . ? C92A C93A 1.54(2) . ? W1B C21B 2.009(18) . ? W1B C11E 2.001(19) . ? W1B C21E 2.003(18) . ? W1B C11B 2.023(18) . ? W1B C10B 2.018(17) . ? W1B P4B 2.495(12) . ? W1B P7B 2.545(11) . ? W1B I2B 2.842(4) . ? W1B I3B 2.873(4) . ? P4B O41B 1.61(3) . ? P4B O61B 1.62(2) . ? P4B O51B 1.69(3) . ? C10B O10B 1.120(17) . ? C22B C21B 1.500(18) . ? C21B C11B 1.306(18) . ? C11B C12B 1.507(18) . ? C10E O10E 1.119(17) . ? C22E C21E 1.471(18) . ? C21E C11E 1.328(17) . ? C11E C12E 1.495(19) . ? O41B C42B 1.45(6) . ? C42B C43B 1.58(7) . ? O51B C52B 1.58(5) . ? C52B C53B 1.27(6) . ? O61B C62B 1.36(5) . ? C62B C63B 1.30(7) . ? P7B O91B 1.55(3) . ? P7B O71B 1.53(2) . ? P7B O81B 1.64(3) . ? O81B C82B 1.28(5) . ? C82B C83B 1.51(6) . ? O91B C92B 1.38(5) . ? C92B C93B 1.63(6) . ? O71B C72B 1.64(5) . ? C72B C73B 1.64(6) . ? W1C C21C 1.99(2) . ? W1C C11C 1.999(19) . ? W1C C21F 2.005(19) . ? W1C C11F 2.00(2) . ? W1C C10C 2.019(19) . ? W1C P4C 2.496(15) . ? W1C P7C 2.545(16) . ? W1C I2C 2.836(5) . ? W1C I3C 2.891(5) . ? P4C O41C 1.60(4) . ? P4C O61C 1.61(3) . ? P4C O51C 1.74(3) . ? P4C C42C 2.41(6) . ? C10C O10C 1.115(19) . ? C22C C21C 1.487(19) . ? C21C C11C 1.317(19) . ? C11C C12C 1.502(19) . ? C10F O10F 1.111(19) . ? C22F C21F 1.493(19) . ? C21F C11F 1.298(19) . ? C11F C12F 1.50(2) . ? O41C C42C 1.38(6) . ? C42C C43C 1.60(7) . ? O51C C52C 1.50(5) . ? C52C C53C 1.41(6) . ? O61C C62C 1.36(5) . ? C62C C63C 1.26(7) . ? P7C O81C 1.54(4) . ? P7C O91C 1.54(3) . ? P7C O71C 1.63(4) . ? O71C C72C 1.35(6) . ? C72C C73C 1.39(8) . ? O81C C82C 1.36(5) . ? C82C C83C 1.75(7) . ? O91C C92C 1.70(6) . ? C92C C93C 1.54(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 C21D W1A C21A 97.2(12) . . ? C21D W1A C11D 38.1(6) . . ? C21A W1A C11D 59.1(12) . . ? C21D W1A C10D 107.9(17) . . ? C21A W1A C10D 14.8(17) . . ? C11D W1A C10D 70.1(16) . . ? C21D W1A C11A 59.1(12) . . ? C21A W1A C11A 38.1(6) . . ? C11D W1A C11A 21.0(12) . . ? C10D W1A C11A 50.1(16) . . ? C21D W1A C10A 14.2(16) . . ? C21A W1A C10A 109.2(16) . . ? C11D W1A C10A 50.9(16) . . ? C10D W1A C10A 121.1(19) . . ? C11A W1A C10A 71.3(16) . . ? C21D W1A P4A 102.3(16) . . ? C21A W1A P4A 81.7(16) . . ? C11D W1A P4A 96.7(14) . . ? C10D W1A P4A 89.5(16) . . ? C11A W1A P4A 89.6(16) . . ? C10A W1A P4A 96.2(16) . . ? C21D W1A P7A 79.7(16) . . ? C21A W1A P7A 101.4(16) . . ? C11D W1A P7A 87.0(14) . . ? C10D W1A P7A 93.0(16) . . ? C11A W1A P7A 94.4(16) . . ? C10A W1A P7A 85.0(16) . . ? P4A W1A P7A 176.1(2) . . ? C21D W1A I2A 86.1(9) . . ? C21A W1A I2A 168.5(15) . . ? C11D W1A I2A 123.8(9) . . ? C10D W1A I2A 166.0(14) . . ? C11A W1A I2A 143.3(10) . . ? C10A W1A I2A 72.9(14) . . ? P4A W1A I2A 86.9(2) . . ? P7A W1A I2A 89.9(2) . . ? C21D W1A I3A 164.4(14) . . ? C21A W1A I3A 92.6(9) . . ? C11D W1A I3A 148.9(10) . . ? C10D W1A I3A 79.9(14) . . ? C11A W1A I3A 130.0(9) . . ? C10A W1A I3A 157.7(14) . . ? P4A W1A I3A 91.0(2) . . ? P7A W1A I3A 86.5(2) . . ? I2A W1A I3A 86.58(14) . . ? O41A P4A O61A 111.0(14) . . ? O41A P4A O51A 99.6(15) . . ? O61A P4A O51A 94.3(16) . . ? O41A P4A W1A 120.2(13) . . ? O61A P4A W1A 110.6(10) . . ? O51A P4A W1A 117.9(10) . . ? O10A C10A W1A 159(4) . . ? C11A C21A C22A 135(2) . . ? C11A C21A W1A 72.3(11) . . ? C22A C21A W1A 152(2) . . ? C21A C11A C12A 129(2) . . ? C21A C11A W1A 69.5(11) . . ? C12A C11A W1A 159(3) . . ? O10D C10D W1A 160(4) . . ? C11D C21D C22D 138(3) . . ? C11D C21D W1A 71.9(11) . . ? C22D C21D W1A 148(3) . . ? C21D C11D C12D 133(3) . . ? C21D C11D W1A 69.9(11) . . ? C12D C11D W1A 150(3) . . ? C42A O41A P4A 113(2) . . ? O41A C42A C43A 107(3) . . ? C52A O51A P4A 119(3) . . ? C53A C52A O51A 110(4) . . ? C62A O61A P4A 126(2) . . ? C63A C62A O61A 127(4) . . ? O71A P7A O91A 114.5(18) . . ? O71A P7A O81A 95.5(15) . . ? O91A P7A O81A 99.5(16) . . ? O71A P7A W1A 121.3(11) . . ? O91A P7A W1A 104.1(12) . . ? O81A P7A W1A 120.5(12) . . ? C72A O71A P7A 133(3) . . ? O71A C72A C73A 108(3) . . ? C82A O81A P7A 131(2) . . ? C83A C82A O81A 118(4) . . ? P7A O91A C92A 112(2) . . ? C93A C92A O91A 92(4) . . ? C21B W1B C11E 41.0(14) . . ? C21B W1B C21E 79.7(14) . . ? C11E W1B C21E 38.7(6) . . ? C21B W1B C11B 37.8(6) . . ? C11E W1B C11B 7(2) . . ? C21E W1B C11B 42.7(14) . . ? C21B W1B C10B 106.6(18) . . ? C11E W1B C10B 66.3(17) . . ? C21E W1B C10B 29.2(17) . . ? C11B W1B C10B 68.8(18) . . ? C21B W1B P4B 95.7(14) . . ? C11E W1B P4B 86.7(12) . . ? C21E W1B P4B 79.3(12) . . ? C11B W1B P4B 93.2(17) . . ? C10B W1B P4B 88.1(15) . . ? C21B W1B P7B 87.5(14) . . ? C11E W1B P7B 96.7(13) . . ? C21E W1B P7B 102.9(12) . . ? C11B W1B P7B 90.2(17) . . ? C10B W1B P7B 92.5(15) . . ? P4B W1B P7B 176.5(3) . . ? C21B W1B I2B 90.4(9) . . ? C11E W1B I2B 130.1(10) . . ? C21E W1B I2B 163.1(12) . . ? C11B W1B I2B 128.1(9) . . ? C10B W1B I2B 162.9(15) . . ? P4B W1B I2B 88.1(2) . . ? P7B W1B I2B 90.3(3) . . ? C21B W1B I3B 172.2(13) . . ? C11E W1B I3B 143.1(10) . . ? C21E W1B I3B 104.8(10) . . ? C11B W1B I3B 145.1(10) . . ? C10B W1B I3B 76.8(15) . . ? P4B W1B I3B 91.4(2) . . ? P7B W1B I3B 85.4(2) . . ? I2B W1B I3B 86.60(14) . . ? O41B P4B O61B 111.1(13) . . ? O41B P4B O51B 99.8(14) . . ? O61B P4B O51B 95.3(14) . . ? O41B P4B W1B 120.4(12) . . ? O61B P4B W1B 109.6(8) . . ? O51B P4B W1B 117.6(9) . . ? O10B C10B W1B 163(4) . . ? C11B C21B C22B 133(3) . . ? C11B C21B W1B 71.7(11) . . ? C22B C21B W1B 150(3) . . ? C21B C11B C12B 133(3) . . ? C21B C11B W1B 70.5(11) . . ? C12B C11B W1B 149(3) . . ? C11E C21E C22E 136(3) . . ? C11E C21E W1B 70.6(11) . . ? C22E C21E W1B 131(3) . . ? C21E C11E C12E 132(2) . . ? C21E C11E W1B 70.7(11) . . ? C12E C11E W1B 82(2) . . ? C42B O41B P4B 109(3) . . ? O41B C42B C43B 105(4) . . ? C52B O51B P4B 119(3) . . ? C53B C52B O51B 113(4) . . ? C62B O61B P4B 123(2) . . ? C63B C62B O61B 123(4) . . ? O91B P7B O71B 112.3(16) . . ? O91B P7B O81B 96.7(15) . . ? O71B P7B O81B 99.9(14) . . ? O91B P7B W1B 120.6(11) . . ? O71B P7B W1B 104.9(10) . . ? O81B P7B W1B 120.9(12) . . ? C82B O81B P7B 131(3) . . ? O81B C82B C83B 118(4) . . ? C92B O91B P7B 128(3) . . ? O91B C92B C93B 104(3) . . ? P7B O71B C72B 114(2) . . ? C73B C72B O71B 101(3) . . ? C21C W1C C11C 38.6(7) . . ? C21C W1C C21F 89.9(19) . . ? C11C W1C C21F 51(2) . . ? C21C W1C C11F 52.1(18) . . ? C11C W1C C11F 14(2) . . ? C21F W1C C11F 37.8(6) . . ? C21C W1C C10C 106(3) . . ? C11C W1C C10C 68(3) . . ? C21F W1C C10C 16(3) . . ? C11F W1C C10C 54(3) . . ? C21C W1C P4C 94(3) . . ? C11C W1C P4C 91(2) . . ? C21F W1C P4C 87(3) . . ? C11F W1C P4C 92(2) . . ? C10C W1C P4C 86(3) . . ? C21C W1C P7C 90(3) . . ? C11C W1C P7C 94(2) . . ? C21F W1C P7C 96(3) . . ? C11F W1C P7C 94(2) . . ? C10C W1C P7C 96(3) . . ? P4C W1C P7C 174.5(4) . . ? C21C W1C I2C 86.9(13) . . ? C11C W1C I2C 125.0(14) . . ? C21F W1C I2C 172(2) . . ? C11F W1C I2C 138.7(14) . . ? C10C W1C I2C 165(2) . . ? P4C W1C I2C 86.0(4) . . ? P7C W1C I2C 90.7(4) . . ? C21C W1C I3C 170.9(18) . . ? C11C W1C I3C 149.2(14) . . ? C21F W1C I3C 98.0(16) . . ? C11F W1C I3C 135.5(14) . . ? C10C W1C I3C 82(2) . . ? P4C W1C I3C 90.4(3) . . ? P7C W1C I3C 84.9(4) . . ? I2C W1C I3C 85.79(16) . . ? O41C P4C O61C 112.5(17) . . ? O41C P4C O51C 101.4(18) . . ? O61C P4C O51C 90.8(18) . . ? O41C P4C C42C 33.2(18) . . ? O61C P4C C42C 100.0(18) . . ? O51C P4C C42C 133.8(18) . . ? O41C P4C W1C 121.7(17) . . ? O61C P4C W1C 108.7(11) . . ? O51C P4C W1C 117.5(11) . . ? C42C P4C W1C 101.2(16) . . ? O10C C10C W1C 163(7) . . ? C11C C21C C22C 135(3) . . ? C11C C21C W1C 71.3(12) . . ? C22C C21C W1C 148(5) . . ? C21C C11C C12C 131(3) . . ? C21C C11C W1C 70.1(11) . . ? C12C C11C W1C 159(3) . . ? C11F C21F C22F 135(3) . . ? C11F C21F W1C 71.0(11) . . ? C22F C21F W1C 152(4) . . ? C21F C11F C12F 135(3) . . ? C21F C11F W1C 71.2(12) . . ? C12F C11F W1C 77(3) . . ? C42C O41C P4C 107(3) . . ? O41C C42C C43C 106(4) . . ? O41C C42C P4C 39(2) . . ? C43C C42C P4C 144(4) . . ? C52C O51C P4C 110(3) . . ? C53C C52C O51C 106(4) . . ? C62C O61C P4C 124(3) . . ? C63C C62C O61C 128(5) . . ? O81C P7C O91C 112(2) . . ? O81C P7C O71C 98.1(19) . . ? O91C P7C O71C 100.5(19) . . ? O81C P7C W1C 121.5(14) . . ? O91C P7C W1C 102.3(13) . . ? O71C P7C W1C 121.2(17) . . ? C72C O71C P7C 133(4) . . ? O71C C72C C73C 118(5) . . ? C82C O81C P7C 125(3) . . ? O81C C82C C83C 99(3) . . ? P7C O91C C92C 117(2) . . ? C93C C92C O91C 102(4) . . ? _refine_diff_density_max 5.831 _refine_diff_density_min -4.509 _refine_diff_density_rms 0.288 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Mo(CO)(MeCCMe)I2(P(OPr)3)2? _chemical_formula_sum 'C23 H48 I2 Mo O7 P2' _chemical_formula_weight 848.29 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 14.116(15) _cell_length_b 14.142(15) _cell_length_c 9.143(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1825(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.354 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4922 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.84 _reflns_number_total 3299 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. The dimethylacetylene and the carbonyl group were disordered over two positions but the metal occupied a crystallographic 2-fold axis and the dimethylacetylene and carbonyl group occupied equivalent positions relative to the two-fold axis. The superimposed carbonyl and dimethylacetylene were each refined with 50% occupancy with constrained dimensions and thermal parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+8.4740P] 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 0.0098(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_number_reflns 3299 _refine_ls_number_parameters 166 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1898 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.820 _refine_ls_shift/su_max 0.321 _refine_ls_shift/su_mean 0.047 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.0000 0.5000 0.32871(14) 0.0641(5) Uani 1 d SD . . I2 I -0.1026(2) 0.39723(17) 0.55139(11) 0.0956(5) Uani 1 d . . . P4 P 0.1272(7) 0.3729(5) 0.3439(4) 0.0773(11) Uani 1 d . . . C100 C 0.088(4) 0.592(3) 0.224(2) 0.052(4) Uiso 0.50 d PD . . O100 O 0.127(2) 0.652(2) 0.177(3) 0.090(10) Uiso 0.50 d PD . . C12 C -0.001(3) 0.536(2) -0.039(3) 0.106(14) Uiso 0.50 d PD . . H22A H -0.0334 0.4964 -0.1085 0.127 Uiso 0.50 calc PR . . H22B H 0.0655 0.5376 -0.0637 0.127 Uiso 0.50 calc PR . . H22C H -0.0263 0.5985 -0.0427 0.127 Uiso 0.50 calc PR . . C11 C -0.013(4) 0.496(4) 0.1119(17) 0.079(6) Uiso 0.50 d PD . . C21 C -0.0808(16) 0.4485(17) 0.177(2) 0.064(7) Uiso 0.50 d PD . . C22 C -0.139(7) 0.364(6) 0.133(6) 0.106(16) Uiso 0.50 d PD . . H22A H -0.2048 0.3801 0.1379 0.128 Uiso 0.50 calc PR . . H22B H -0.1256 0.3126 0.1976 0.128 Uiso 0.50 calc PR . . H22C H -0.1230 0.3465 0.0343 0.128 Uiso 0.50 calc PR . . O41 O 0.106(2) 0.2858(15) 0.246(3) 0.142(10) Uani 1 d DU . . C42 C 0.053(2) 0.2026(17) 0.269(3) 0.173(12) Uani 1 d DU . . H42 H -0.0037 0.2160 0.3270 0.207 Uiso 1 calc R . . C43 C 0.117(4) 0.132(2) 0.347(6) 0.28(3) Uani 1 d DU . . H43A H 0.1818 0.1448 0.3211 0.339 Uiso 1 calc R . . H43B H 0.1005 0.0693 0.3179 0.339 Uiso 1 calc R . . H43C H 0.1092 0.1389 0.4506 0.339 Uiso 1 calc R . . C44 C 0.026(4) 0.166(3) 0.117(4) 0.25(2) Uani 1 d DU . . H44A H 0.0807 0.1409 0.0693 0.296 Uiso 1 calc R . . H44B H 0.0004 0.2172 0.0598 0.296 Uiso 1 calc R . . H44C H -0.0213 0.1174 0.1266 0.296 Uiso 1 calc R . . O51 O 0.2185(11) 0.4094(14) 0.270(3) 0.119(9) Uani 1 d DU . . C52 C 0.3093(11) 0.3707(14) 0.265(2) 0.090(5) Uani 1 d DU . . H52 H 0.3121 0.3183 0.3347 0.108 Uiso 1 calc R . . C53 C 0.3803(17) 0.444(3) 0.311(4) 0.188(17) Uani 1 d DU . . H53A H 0.3749 0.4984 0.2491 0.226 Uiso 1 calc R . . H53B H 0.4430 0.4183 0.3036 0.226 Uiso 1 calc R . . H53C H 0.3682 0.4620 0.4107 0.226 Uiso 1 calc R . . C54 C 0.327(2) 0.331(3) 0.114(3) 0.171(15) Uani 1 d DU . . H54A H 0.3903 0.3080 0.1080 0.205 Uiso 1 calc R . . H54B H 0.3175 0.3804 0.0429 0.205 Uiso 1 calc R . . H54C H 0.2829 0.2808 0.0956 0.205 Uiso 1 calc R . . O61 O 0.1532(15) 0.3197(13) 0.4878(13) 0.111(8) Uani 1 d DU . . C62 C 0.1476(19) 0.3459(16) 0.6361(14) 0.107(6) Uani 1 d DU . . H62 H 0.1055 0.4004 0.6489 0.129 Uiso 1 calc R . . C63 C 0.110(4) 0.260(3) 0.720(4) 0.22(3) Uani 1 d DU . . H63A H 0.1090 0.2060 0.6562 0.266 Uiso 1 calc R . . H63B H 0.0475 0.2728 0.7548 0.266 Uiso 1 calc R . . H63C H 0.1513 0.2471 0.8015 0.266 Uiso 1 calc R . . C64 C 0.248(3) 0.370(3) 0.685(4) 0.157(15) Uani 1 d DU . . H64A H 0.2468 0.3971 0.7808 0.189 Uiso 1 calc R . . H64B H 0.2758 0.4141 0.6174 0.189 Uiso 1 calc R . . H64C H 0.2859 0.3132 0.6865 0.189 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.081(2) 0.0564(15) 0.0550(6) 0.000 0.000 0.0096(6) I2 0.105(2) 0.0800(13) 0.1016(7) 0.0137(13) 0.0149(17) -0.0172(5) P4 0.093(6) 0.062(4) 0.0767(18) 0.004(4) -0.010(5) 0.0136(15) O41 0.19(3) 0.106(15) 0.136(17) -0.035(13) -0.044(18) 0.004(14) C42 0.25(3) 0.114(18) 0.16(2) -0.045(18) -0.01(3) -0.01(2) C43 0.31(6) 0.14(3) 0.40(6) -0.02(4) -0.07(5) 0.13(4) C44 0.33(6) 0.21(4) 0.20(4) -0.08(3) -0.02(4) -0.12(4) O51 0.060(11) 0.116(13) 0.18(2) 0.059(13) 0.007(12) 0.033(9) C52 0.061(11) 0.113(13) 0.097(13) -0.001(10) 0.005(9) 0.031(10) C53 0.078(19) 0.31(5) 0.18(3) 0.04(3) 0.01(2) 0.00(3) C54 0.14(3) 0.26(4) 0.12(2) -0.06(2) 0.008(19) 0.06(3) O61 0.16(2) 0.089(9) 0.084(7) 0.016(7) -0.034(9) 0.029(12) C62 0.13(2) 0.120(18) 0.068(9) 0.052(14) -0.009(15) 0.015(11) C63 0.23(5) 0.19(4) 0.25(4) 0.15(3) 0.05(4) -0.05(3) C64 0.16(4) 0.13(2) 0.18(3) 0.03(2) -0.04(3) 0.00(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 C21 1.941(19) . ? Mo1 C11 1.991(16) . ? Mo1 C100 2.030(13) . ? Mo1 P4 2.545(4) 2_565 ? Mo1 P4 2.545(4) . ? Mo1 I2 2.891(2) . ? Mo1 I2 2.891(2) 2_565 ? P4 O41 1.55(2) . ? P4 O51 1.54(2) . ? P4 O61 1.560(12) . ? C100 O100 1.107(15) . ? C12 C11 1.504(18) . ? C11 C21 1.310(18) . ? C21 C22 1.499(18) . ? O41 C42 1.412(15) . ? C42 C44 1.528(13) . ? C42 C43 1.522(14) . ? O51 C52 1.394(17) . ? C52 C53 1.502(17) . ? C52 C54 1.504(16) . ? O61 C62 1.408(16) . ? C62 C64 1.528(16) . ? C62 C63 1.530(15) . ? 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 C21 Mo1 C11 38.9(7) . . ? C21 Mo1 C100 105.1(11) . . ? C11 Mo1 C100 66.9(10) . . ? C21 Mo1 P4 83.7(8) . 2_565 ? C11 Mo1 P4 91(2) . 2_565 ? C100 Mo1 P4 90(2) . 2_565 ? C21 Mo1 P4 100.8(8) . . ? C11 Mo1 P4 96(2) . . ? C100 Mo1 P4 93(2) . . ? P4 Mo1 P4 173.75(17) 2_565 . ? C21 Mo1 I2 91.2(6) . . ? C11 Mo1 I2 129.8(7) . . ? C100 Mo1 I2 163.2(6) . . ? P4 Mo1 I2 87.9(2) 2_565 . ? P4 Mo1 I2 87.7(2) . . ? C21 Mo1 I2 171.1(8) . 2_565 ? C11 Mo1 I2 139.6(7) . 2_565 ? C100 Mo1 I2 72.8(6) . 2_565 ? P4 Mo1 I2 87.7(2) 2_565 2_565 ? P4 Mo1 I2 87.9(2) . 2_565 ? I2 Mo1 I2 90.45(9) . 2_565 ? O41 P4 O51 99.9(13) . . ? O41 P4 O61 98.7(14) . . ? O51 P4 O61 109.5(12) . . ? O41 P4 Mo1 113.2(13) . . ? O51 P4 Mo1 109.2(7) . . ? O61 P4 Mo1 123.6(6) . . ? O100 C100 Mo1 170(5) . . ? C12 C11 C21 104(4) ? . ? C21 C11 C12 134(3) . . ? C12 C11 Mo1 144(7) ? . ? C21 C11 Mo1 68.5(8) . . ? C11 C21 C22 133(3) . . ? C11 C21 Mo1 72.6(8) . . ? C22 C21 Mo1 144(4) . . ? C42 O41 P4 133(2) . . ? O41 C42 C44 106.4(14) . . ? O41 C42 C43 107.2(15) . . ? C44 C42 C43 111(2) . . ? C52 O51 P4 130.6(16) . . ? O51 C52 C53 109.4(14) . . ? O51 C52 C54 109.0(14) . . ? C53 C52 C54 114(2) . . ? C62 O61 P4 132.3(11) . . ? O61 C62 C64 106.6(14) . . ? O61 C62 C63 107.0(14) . . ? C64 C62 C63 110.4(17) . . ? _refine_diff_density_max 0.672 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.115 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety W(CO)(MeCCMe)I2(P(OPr)3)2 _chemical_formula_sum 'C23 H48 I2 O7 P2 W' _chemical_formula_weight 936.20 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 14.079(15) _cell_length_b 14.072(15) _cell_length_c 9.146(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1812(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 5.011 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5550 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.88 _reflns_number_total 3335 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+8.4740P] 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 0.0096(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(7) _refine_ls_number_reflns 3335 _refine_ls_number_parameters 166 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 0.710 _refine_ls_restrained_S_all 0.711 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.0000 0.5000 0.32785(5) 0.0541(2) Uani 1 d SD . . I2 I -0.1019(2) 0.39882(19) 0.55130(10) 0.0821(3) Uani 1 d . . . P4 P 0.1265(6) 0.3729(6) 0.3429(3) 0.0638(6) Uani 1 d . . . C100 C 0.0840(18) 0.6023(18) 0.227(2) 0.052(5) Uiso 0.50 d PD . . O100 O 0.1334(14) 0.6589(14) 0.190(3) 0.070(6) Uiso 0.50 d PD . . C12 C 0.002(5) 0.527(3) -0.038(2) 0.113(15) Uiso 0.50 d PD . . H22A H 0.0181 0.4735 -0.0987 0.135 Uiso 0.50 calc PR . . H22B H 0.0532 0.5717 -0.0386 0.135 Uiso 0.50 calc PR . . H22C H -0.0544 0.5567 -0.0761 0.135 Uiso 0.50 calc PR . . C11 C -0.016(3) 0.494(3) 0.1153(13) 0.054(5) Uiso 0.50 d PD . . C21 C -0.072(4) 0.435(3) 0.178(2) 0.068(6) Uiso 0.50 d PD . . C22 C -0.133(3) 0.354(2) 0.133(3) 0.065(7) Uiso 0.50 d PD . . H22A H -0.1983 0.3709 0.1442 0.079 Uiso 0.50 calc PR . . H22B H -0.1188 0.2998 0.1937 0.079 Uiso 0.50 calc PR . . H22C H -0.1201 0.3382 0.0328 0.079 Uiso 0.50 calc PR . . O41 O 0.1050(19) 0.2845(11) 0.245(3) 0.117(7) Uani 1 d DU . . C42 C 0.0507(19) 0.2007(15) 0.259(3) 0.151(11) Uani 1 d DU . . H42 H -0.0042 0.2088 0.3240 0.181 Uiso 1 calc R . . C43 C 0.118(3) 0.1250(18) 0.312(6) 0.20(2) Uani 1 d DU . . H43A H 0.1766 0.1288 0.2583 0.240 Uiso 1 calc R . . H43B H 0.0903 0.0635 0.2984 0.240 Uiso 1 calc R . . H43C H 0.1312 0.1344 0.4145 0.240 Uiso 1 calc R . . C44 C 0.023(4) 0.175(3) 0.104(4) 0.22(2) Uani 1 d DU . . H44A H 0.0027 0.2316 0.0535 0.263 Uiso 1 calc R . . H44B H -0.0284 0.1303 0.1061 0.263 Uiso 1 calc R . . H44C H 0.0763 0.1479 0.0545 0.263 Uiso 1 calc R . . O51 O 0.2193(10) 0.4108(13) 0.276(3) 0.111(7) Uani 1 d DU . . C52 C 0.3113(10) 0.3725(14) 0.266(2) 0.096(6) Uani 1 d DU . . H52 H 0.3179 0.3168 0.3294 0.115 Uiso 1 calc R . . C53 C 0.3798(14) 0.448(2) 0.309(5) 0.160(14) Uani 1 d DU . . H53A H 0.3669 0.5049 0.2540 0.192 Uiso 1 calc R . . H53B H 0.4434 0.4273 0.2891 0.192 Uiso 1 calc R . . H53C H 0.3733 0.4614 0.4115 0.192 Uiso 1 calc R . . C54 C 0.326(2) 0.346(3) 0.109(3) 0.169(14) Uani 1 d DU . . H54A H 0.3863 0.3684 0.0767 0.202 Uiso 1 calc R . . H54B H 0.2763 0.3738 0.0508 0.202 Uiso 1 calc R . . H54C H 0.3231 0.2779 0.0996 0.202 Uiso 1 calc R . . O61 O 0.161(2) 0.322(2) 0.4866(12) 0.119(7) Uani 1 d DU . . C62 C 0.1458(15) 0.3415(18) 0.6370(15) 0.099(6) Uani 1 d DU . . H62 H 0.0961 0.3889 0.6545 0.119 Uiso 1 calc R . . C63 C 0.122(3) 0.244(3) 0.700(4) 0.158(17) Uani 1 d DU . . H63A H 0.1075 0.2009 0.6216 0.190 Uiso 1 calc R . . H63B H 0.0686 0.2491 0.7640 0.190 Uiso 1 calc R . . H63C H 0.1759 0.2203 0.7535 0.190 Uiso 1 calc R . . C64 C 0.241(3) 0.370(4) 0.696(5) 0.19(2) Uani 1 d DU . . H64A H 0.2471 0.3490 0.7951 0.231 Uiso 1 calc R . . H64B H 0.2469 0.4383 0.6926 0.231 Uiso 1 calc R . . H64C H 0.2903 0.3421 0.6375 0.231 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0566(13) 0.0554(13) 0.0504(3) 0.000 0.000 0.0119(2) I2 0.0759(18) 0.0702(16) 0.1000(6) 0.0103(14) 0.0170(14) -0.0150(4) P4 0.054(4) 0.062(4) 0.0749(15) 0.002(4) -0.005(4) 0.0136(10) O41 0.18(2) 0.059(9) 0.114(12) -0.013(9) -0.028(13) 0.027(11) C42 0.20(3) 0.107(17) 0.14(2) -0.045(16) -0.04(2) 0.029(19) C43 0.22(4) 0.12(3) 0.26(5) 0.00(3) -0.11(4) 0.04(3) C44 0.25(5) 0.22(4) 0.19(4) -0.09(3) -0.07(3) -0.03(4) O51 0.060(9) 0.096(10) 0.18(2) 0.057(12) 0.010(10) 0.012(7) C52 0.046(8) 0.104(13) 0.137(16) -0.008(11) -0.006(9) 0.030(8) C53 0.065(13) 0.16(3) 0.26(4) -0.02(3) -0.01(2) -0.004(16) C54 0.15(3) 0.23(4) 0.12(2) -0.03(3) 0.04(2) -0.02(3) O61 0.129(16) 0.140(18) 0.087(7) -0.003(12) -0.032(11) 0.074(11) C62 0.068(11) 0.15(2) 0.082(9) 0.018(13) -0.038(10) 0.007(10) C63 0.105(19) 0.15(3) 0.22(4) 0.10(3) -0.01(2) -0.002(19) C64 0.13(3) 0.26(5) 0.20(4) -0.07(4) -0.09(3) 0.00(3) _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 W1 C21 1.929(16) . ? W1 C11 1.959(12) . ? W1 C100 2.079(13) . ? W1 P4 2.528(3) 2_565 ? W1 P4 2.528(3) . ? W1 I2 2.875(2) . ? W1 I2 2.875(2) 2_565 ? P4 O41 1.563(19) . ? P4 O51 1.537(18) . ? P4 O61 1.571(12) . ? C100 O100 1.109(15) . ? C12 C11 1.503(16) . ? C11 C21 1.270(15) . ? C21 C22 1.490(16) . ? O41 C42 1.411(15) . ? C42 C43 1.509(14) . ? C42 C44 1.517(14) . ? O51 C52 1.405(17) . ? C52 C53 1.491(17) . ? C52 C54 1.495(17) . ? O61 C62 1.418(16) . ? C62 C64 1.502(16) . ? C62 C63 1.526(16) . ? 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 C21 W1 C11 38.1(5) . . ? C21 W1 C100 108.0(9) . . ? C11 W1 C100 69.9(8) . . ? C21 W1 P4 90(2) . 2_565 ? C11 W1 P4 90.3(15) . 2_565 ? C100 W1 P4 86.3(9) . 2_565 ? C21 W1 P4 94(2) . . ? C11 W1 P4 95.9(15) . . ? C100 W1 P4 96.5(9) . . ? P4 W1 P4 173.75(14) 2_565 . ? C21 W1 I2 90.6(5) . . ? C11 W1 I2 128.7(5) . . ? C100 W1 I2 160.5(6) . . ? P4 W1 I2 87.7(2) 2_565 . ? P4 W1 I2 87.9(2) . . ? C21 W1 I2 178(2) . 2_565 ? C11 W1 I2 141.8(5) . 2_565 ? C100 W1 I2 71.9(6) . 2_565 ? P4 W1 I2 87.9(2) 2_565 2_565 ? P4 W1 I2 87.7(2) . 2_565 ? I2 W1 I2 89.38(8) . 2_565 ? O41 P4 O51 102.4(11) . . ? O41 P4 O61 100.3(15) . . ? O51 P4 O61 103.1(15) . . ? O41 P4 W1 113.2(9) . . ? O51 P4 W1 109.4(8) . . ? O61 P4 W1 125.7(5) . . ? O100 C100 W1 171(2) . . ? C12 C11 C21 111(5) ? . ? C12 C11 C12 40(5) ? . ? C21 C11 C12 136.6(19) . . ? C12 C11 W1 148(6) ? . ? C21 C11 W1 69.7(7) . . ? C11 C21 C22 137(2) . . ? C11 C21 W1 72.2(7) . . ? C22 C21 W1 149(2) . . ? C42 O41 P4 136(2) . . ? O41 C42 C43 106.2(14) . . ? O41 C42 C44 104.5(14) . . ? C43 C42 C44 107(2) . . ? C52 O51 P4 132.6(16) . . ? O51 C52 C53 107.7(13) . . ? O51 C52 C54 106.6(14) . . ? C53 C52 C54 110(2) . . ? C62 O61 P4 132.7(11) . . ? O61 C62 C64 105.5(13) . . ? O61 C62 C63 103.0(13) . . ? C64 C62 C63 107.6(18) . . ? _refine_diff_density_max 1.107 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.125 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety W(CO)(MeCCPh)I2(P(OPr)3)2 _chemical_formula_sum 'C28 H44 I2 O7 P2 W' _chemical_formula_weight 992.22 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 12.498(14) _cell_length_b 16.916(17) _cell_length_c 18.95(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.944(10) _cell_angle_gamma 90.00 _cell_volume 3969(8) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 4.581 _exptl_absorpt_correction_type 'DIFABS(Stuart and Walker, 1983)' _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 1.000 _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10013 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.91 _reflns_number_total 6190 _reflns_number_gt 3391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1296P)^2^+1.3317P] 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 0.00000(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6190 _refine_ls_number_parameters 200 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1761 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2621 _refine_ls_wR_factor_gt 0.2215 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.341 _refine_ls_shift/su_mean 0.028 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.42128(7) 0.28255(4) 0.12839(4) 0.0515(3) Uani 1 d . . . I2 I 0.32709(13) 0.13340(8) 0.08745(8) 0.0729(5) Uani 1 d . . . I3 I 0.40103(17) 0.31909(9) -0.02181(7) 0.0909(6) Uani 1 d . . . P7 P 0.6018(5) 0.2185(3) 0.1099(3) 0.0608(14) Uani 1 d . . . P4 P 0.2302(5) 0.3209(3) 0.1392(3) 0.0656(16) Uani 1 d . . . C100 C 0.4400(18) 0.2297(10) 0.2196(10) 0.058(5) Uiso 1 d . . . O100 O 0.4513(15) 0.1985(10) 0.2741(10) 0.093(5) Uiso 1 d . . . O71 O 0.6979(15) 0.2691(9) 0.0886(9) 0.090(5) Uiso 1 d . . . C72 C 0.706(3) 0.3550(19) 0.0948(19) 0.131(11) Uiso 1 d . . . H72 H 0.6423 0.3755 0.1121 0.157 Uiso 1 calc R . . C74 C 0.806(5) 0.369(4) 0.152(3) 0.29(3) Uiso 1 d . . . H74A H 0.7902 0.3516 0.1971 0.347 Uiso 1 calc R . . H74B H 0.8213 0.4250 0.1537 0.347 Uiso 1 calc R . . H74C H 0.8669 0.3411 0.1390 0.347 Uiso 1 calc R . . C73 C 0.719(4) 0.391(3) 0.028(3) 0.23(2) Uiso 1 d . . . H73A H 0.7549 0.4411 0.0373 0.273 Uiso 1 calc R . . H73B H 0.6488 0.3999 0.0014 0.273 Uiso 1 calc R . . H73C H 0.7606 0.3579 0.0016 0.273 Uiso 1 calc R . . C82 C 0.736(2) 0.1184(16) 0.1954(16) 0.105(8) Uiso 1 d . . . H82 H 0.7798 0.1205 0.1564 0.126 Uiso 1 calc R . . C83 C 0.801(3) 0.148(2) 0.265(2) 0.159(14) Uiso 1 d . . . H83A H 0.7951 0.1104 0.3022 0.190 Uiso 1 calc R . . H83B H 0.7728 0.1980 0.2775 0.190 Uiso 1 calc R . . H83C H 0.8753 0.1538 0.2585 0.190 Uiso 1 calc R . . C84 C 0.684(4) 0.040(2) 0.198(2) 0.188(18) Uiso 1 d . . . H84A H 0.6316 0.0417 0.2303 0.226 Uiso 1 calc R . . H84B H 0.7381 0.0011 0.2138 0.226 Uiso 1 calc R . . H84C H 0.6492 0.0261 0.1512 0.226 Uiso 1 calc R . . O81 O 0.6447(13) 0.1751(8) 0.1824(8) 0.077(4) Uiso 1 d . . . C93 C 0.730(3) 0.1162(18) -0.0250(16) 0.122(10) Uiso 1 d . . . H93A H 0.7831 0.1476 0.0038 0.146 Uiso 1 calc R . . H93B H 0.7418 0.1190 -0.0739 0.146 Uiso 1 calc R . . H93C H 0.7357 0.0622 -0.0092 0.146 Uiso 1 calc R . . C94 C 0.532(2) 0.1026(16) -0.0603(15) 0.110(9) Uiso 1 d . . . H94A H 0.5276 0.1169 -0.1097 0.131 Uiso 1 calc R . . H94B H 0.4657 0.1161 -0.0432 0.131 Uiso 1 calc R . . H94C H 0.5442 0.0467 -0.0552 0.131 Uiso 1 calc R . . C92 C 0.623(2) 0.1459(14) -0.0184(13) 0.086(7) Uiso 1 d . . . H92 H 0.6197 0.2007 -0.0355 0.103 Uiso 1 calc R . . O91 O 0.6033(14) 0.1473(9) 0.0540(9) 0.091(5) Uiso 1 d . . . O41 O 0.2310(13) 0.4076(8) 0.1662(8) 0.081(4) Uiso 1 d . . . C42 C 0.131(3) 0.452(2) 0.1780(19) 0.134(11) Uiso 1 d . . . H42 H 0.0682 0.4166 0.1725 0.161 Uiso 1 calc R . . C43 C 0.154(3) 0.4839(18) 0.2550(18) 0.136(12) Uiso 1 d . . . H43A H 0.1675 0.5397 0.2538 0.163 Uiso 1 calc R . . H43B H 0.2159 0.4576 0.2800 0.163 Uiso 1 calc R . . H43C H 0.0923 0.4744 0.2790 0.163 Uiso 1 calc R . . C44 C 0.117(3) 0.513(2) 0.127(2) 0.161(14) Uiso 1 d . . . H44A H 0.0637 0.5498 0.1397 0.193 Uiso 1 calc R . . H44B H 0.0939 0.4918 0.0810 0.193 Uiso 1 calc R . . H44C H 0.1845 0.5408 0.1272 0.193 Uiso 1 calc R . . O51 O 0.163(2) 0.2729(13) 0.1885(12) 0.144(8) Uiso 1 d D . . C52 C 0.190(2) 0.2150(17) 0.2432(17) 0.154(14) Uiso 1 d D . . H52 H 0.2544 0.1828 0.2420 0.184 Uiso 1 calc R . . C53 C 0.181(5) 0.264(3) 0.3088(14) 0.39(5) Uiso 1 d D . . H53A H 0.1516 0.2321 0.3434 0.472 Uiso 1 calc R . . H53B H 0.1347 0.3084 0.2962 0.472 Uiso 1 calc R . . H53C H 0.2516 0.2822 0.3285 0.472 Uiso 1 calc R . . C54 C 0.082(4) 0.173(3) 0.240(3) 0.31(3) Uiso 1 d D . . H54A H 0.0501 0.1863 0.2823 0.367 Uiso 1 calc R . . H54B H 0.0925 0.1173 0.2384 0.367 Uiso 1 calc R . . H54C H 0.0346 0.1903 0.1989 0.367 Uiso 1 calc R . . O61 O 0.133(2) 0.3234(17) 0.0749(17) 0.179(11) Uiso 1 d . . . C62 C 0.102(3) 0.2811(17) 0.0098(17) 0.112(9) Uiso 1 d . . . H62 H 0.1648 0.2501 0.0003 0.134 Uiso 1 calc R . . C64 C 0.086(4) 0.351(3) -0.048(3) 0.24(3) Uiso 1 d . . . H64A H 0.1205 0.3981 -0.0274 0.292 Uiso 1 calc R . . H64B H 0.0104 0.3608 -0.0612 0.292 Uiso 1 calc R . . H64C H 0.1180 0.3360 -0.0890 0.292 Uiso 1 calc R . . C63 C 0.016(5) 0.226(3) 0.019(3) 0.24(3) Uiso 1 d . . . H63A H 0.0372 0.1943 0.0603 0.290 Uiso 1 calc R . . H63B H 0.0037 0.1921 -0.0225 0.290 Uiso 1 calc R . . H63C H -0.0484 0.2545 0.0236 0.290 Uiso 1 calc R . . C11 C 0.4868(17) 0.3638(10) 0.2057(10) 0.058(5) Uiso 1 d . . . C12 C 0.5250(19) 0.3848(12) 0.2766(11) 0.069(5) Uiso 1 d . . . C13 C 0.615(2) 0.3408(14) 0.3114(13) 0.081(6) Uiso 1 d . . . H13 H 0.6431 0.2972 0.2901 0.097 Uiso 1 calc R . . C16 C 0.520(3) 0.473(2) 0.380(2) 0.141(12) Uiso 1 d . . . H16 H 0.4862 0.5115 0.4041 0.170 Uiso 1 calc R . . C17 C 0.483(2) 0.4478(13) 0.3078(13) 0.084(7) Uiso 1 d . . . H17 H 0.4281 0.4761 0.2812 0.101 Uiso 1 calc R . . C14 C 0.660(3) 0.3662(16) 0.3789(16) 0.110(9) Uiso 1 d . . . H14 H 0.7189 0.3393 0.4032 0.132 Uiso 1 calc R . . C15 C 0.620(2) 0.4293(14) 0.4094(14) 0.091(7) Uiso 1 d . . . H15 H 0.6568 0.4470 0.4524 0.109 Uiso 1 calc R . . C21 C 0.4542(17) 0.3956(11) 0.1411(10) 0.061(5) Uiso 1 d . . . C22 C 0.454(2) 0.4787(15) 0.1089(15) 0.105(8) Uiso 1 d . . . H22A H 0.4657 0.5171 0.1465 0.126 Uiso 1 calc R . . H22B H 0.3849 0.4884 0.0808 0.126 Uiso 1 calc R . . H22C H 0.5098 0.4826 0.0793 0.126 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0509(7) 0.0509(4) 0.0526(4) 0.0027(3) 0.0068(4) 0.0035(4) I2 0.0725(13) 0.0596(8) 0.0856(10) -0.0155(6) 0.0079(8) -0.0016(7) I3 0.1248(17) 0.0856(10) 0.0594(9) 0.0107(7) 0.0022(9) 0.0085(10) P7 0.051(4) 0.067(3) 0.068(3) 0.005(2) 0.019(3) 0.002(3) P4 0.049(4) 0.063(3) 0.085(4) -0.020(3) 0.008(3) 0.005(3) _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 W1 C21 1.961(19) . ? W1 C100 1.932(19) . ? W1 C11 2.091(18) . ? W1 P4 2.511(7) . ? W1 P7 2.569(6) . ? W1 I2 2.847(3) . ? W1 I3 2.890(4) . ? P7 O71 1.551(18) . ? P7 O81 1.585(15) . ? P7 O91 1.603(17) . ? P4 O61 1.60(3) . ? P4 O41 1.548(15) . ? P4 O51 1.57(2) . ? C100 O100 1.13(2) . ? O71 C72 1.45(3) . ? C72 C73 1.44(5) . ? C72 C74 1.54(6) . ? C82 C84 1.48(4) . ? C82 O81 1.48(3) . ? C82 C83 1.53(4) . ? C93 C92 1.45(3) . ? C94 C92 1.49(3) . ? C92 O91 1.43(3) . ? O41 C42 1.50(4) . ? C42 C44 1.41(4) . ? C42 C43 1.55(4) . ? O51 C52 1.432(18) . ? C52 C53 1.508(19) . ? C52 C54 1.513(19) . ? O61 C62 1.43(4) . ? C62 C63 1.45(5) . ? C62 C64 1.60(5) . ? C11 C21 1.36(3) . ? C11 C12 1.39(3) . ? C12 C17 1.38(3) . ? C12 C13 1.42(3) . ? C13 C14 1.39(3) . ? C16 C17 1.44(4) . ? C16 C15 1.49(4) . ? C14 C15 1.35(3) . ? C21 C22 1.53(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 C21 W1 C100 110.1(8) . . ? C21 W1 C11 38.7(7) . . ? C100 W1 C11 71.9(7) . . ? C21 W1 P4 85.4(7) . . ? C100 W1 P4 92.6(7) . . ? C11 W1 P4 93.3(6) . . ? C21 W1 P7 105.0(7) . . ? C100 W1 P7 85.8(7) . . ? C11 W1 P7 96.1(6) . . ? P4 W1 P7 169.43(18) . . ? C21 W1 I2 165.3(6) . . ? C100 W1 I2 80.1(5) . . ? C11 W1 I2 151.7(5) . . ? P4 W1 I2 83.61(14) . . ? P7 W1 I2 85.82(14) . . ? C21 W1 I3 84.4(6) . . ? C100 W1 I3 164.6(5) . . ? C11 W1 I3 121.5(5) . . ? P4 W1 I3 94.03(15) . . ? P7 W1 I3 85.12(13) . . ? I2 W1 I3 86.74(6) . . ? O71 P7 O81 107.4(9) . . ? O71 P7 O91 99.6(10) . . ? O81 P7 O91 101.0(8) . . ? O71 P7 W1 120.8(7) . . ? O81 P7 W1 106.0(6) . . ? O91 P7 W1 119.9(7) . . ? O61 P4 O41 101.6(12) . . ? O61 P4 O51 93.2(15) . . ? O41 P4 O51 106.1(11) . . ? O61 P4 W1 124.9(12) . . ? O41 P4 W1 107.8(7) . . ? O51 P4 W1 120.5(10) . . ? O100 C100 W1 177.1(19) . . ? C72 O71 P7 127(2) . . ? C73 C72 O71 113(3) . . ? C73 C72 C74 111(4) . . ? O71 C72 C74 106(3) . . ? C84 C82 O81 105(3) . . ? C84 C82 C83 116(3) . . ? O81 C82 C83 104(2) . . ? C82 O81 P7 127.2(16) . . ? C93 C92 O91 112(2) . . ? C93 C92 C94 115(2) . . ? O91 C92 C94 108(2) . . ? C92 O91 P7 131.8(15) . . ? C42 O41 P4 123.4(18) . . ? C44 C42 O41 107(3) . . ? C44 C42 C43 112(3) . . ? O41 C42 C43 106(3) . . ? C52 O51 P4 134(2) . . ? O51 C52 C53 100.7(16) . . ? O51 C52 C54 100.1(16) . . ? C53 C52 C54 96.9(16) . . ? C62 O61 P4 137(3) . . ? C63 C62 O61 110(3) . . ? C63 C62 C64 122(4) . . ? O61 C62 C64 102(3) . . ? C21 C11 C12 142.5(19) . . ? C21 C11 W1 65.4(11) . . ? C12 C11 W1 152.1(15) . . ? C17 C12 C11 119(2) . . ? C17 C12 C13 121(2) . . ? C11 C12 C13 120(2) . . ? C14 C13 C12 118(2) . . ? C17 C16 C15 110(3) . . ? C16 C17 C12 124(3) . . ? C15 C14 C13 121(3) . . ? C14 C15 C16 125(3) . . ? C11 C21 C22 135.5(19) . . ? C11 C21 W1 75.7(11) . . ? C22 C21 W1 148.7(16) . . ? _refine_diff_density_max 2.717 _refine_diff_density_min -1.647 _refine_diff_density_rms 0.231 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_19 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24' _chemical_formula_weight 348.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.631(14) _cell_length_b 11.290(14) _cell_length_c 15.645(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.636(10) _cell_angle_gamma 90.00 _cell_volume 2025(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6329 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3623 _reflns_number_gt 1761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^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 0.004(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3623 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1713 _refine_ls_R_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.3101 _refine_ls_wR_factor_gt 0.2526 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3633(3) 0.7671(3) 0.0037(2) 0.0526(9) Uani 1 d . . . C2 C 0.2475(3) 0.7990(3) 0.0080(2) 0.0540(9) Uani 1 d . . . C3 C 0.2211(3) 0.8688(3) 0.0759(2) 0.0525(9) Uani 1 d . . . C4 C 0.3118(3) 0.9120(3) 0.1394(2) 0.0544(9) Uani 1 d . . . C5 C 0.4280(3) 0.8838(3) 0.1335(2) 0.0495(9) Uani 1 d . . . C6 C 0.4529(3) 0.8105(3) 0.0674(2) 0.0505(9) Uani 1 d . . . C11 C 0.3901(3) 0.6860(4) -0.0669(3) 0.0700(12) Uani 1 d . . . H11A H 0.3773 0.6053 -0.0515 0.084 Uiso 1 calc R . . H11B H 0.4701 0.6960 -0.0737 0.084 Uiso 1 calc R . . H11C H 0.3401 0.7050 -0.1203 0.084 Uiso 1 calc R . . C21 C 0.1512(3) 0.7607(3) -0.0639(3) 0.0614(10) Uani 1 d . . . C22 C 0.0941(4) 0.6523(4) -0.0610(3) 0.0798(13) Uani 1 d . . . H22 H 0.1163 0.6017 -0.0143 0.096 Uiso 1 calc R . . C23 C 0.0050(4) 0.6191(5) -0.1266(4) 0.0997(17) Uani 1 d . . . H23 H -0.0318 0.5465 -0.1231 0.120 Uiso 1 calc R . . C24 C -0.0296(4) 0.6896(6) -0.1954(4) 0.1010(17) Uani 1 d . . . H24 H -0.0895 0.6662 -0.2392 0.121 Uiso 1 calc R . . C25 C 0.0262(5) 0.7988(6) -0.1998(4) 0.1046(17) Uani 1 d . . . H25 H 0.0024 0.8492 -0.2464 0.126 Uiso 1 calc R . . C26 C 0.1161(4) 0.8321(4) -0.1355(3) 0.0850(14) Uani 1 d . . . H26 H 0.1538 0.9038 -0.1402 0.102 Uiso 1 calc R . . C31 C 0.0948(3) 0.8978(4) 0.0825(3) 0.0722(12) Uani 1 d . . . H31A H 0.0444 0.8692 0.0318 0.087 Uiso 1 calc R . . H31B H 0.0859 0.9820 0.0869 0.087 Uiso 1 calc R . . H31C H 0.0745 0.8603 0.1330 0.087 Uiso 1 calc R . . C41 C 0.2809(4) 0.9845(4) 0.2128(3) 0.0788(13) Uani 1 d . . . H41A H 0.3464 0.9873 0.2591 0.095 Uiso 1 calc R . . H41B H 0.2156 0.9491 0.2333 0.095 Uiso 1 calc R . . H41C H 0.2609 1.0634 0.1928 0.095 Uiso 1 calc R . . C51 C 0.5237(3) 0.9302(3) 0.2007(2) 0.0561(10) Uani 1 d . . . C52 C 0.5812(3) 0.8575(4) 0.2650(3) 0.0749(12) Uani 1 d . . . H52 H 0.5631 0.7773 0.2646 0.090 Uiso 1 calc R . . C53 C 0.6651(4) 0.9026(6) 0.3298(4) 0.1012(16) Uani 1 d . . . H53 H 0.7018 0.8533 0.3737 0.121 Uiso 1 calc R . . C54 C 0.6946(4) 1.0223(6) 0.3292(4) 0.1033(19) Uani 1 d . . . H54 H 0.7503 1.0533 0.3731 0.124 Uiso 1 calc R . . C55 C 0.6422(4) 1.0923(5) 0.2651(4) 0.0990(17) Uani 1 d . . . H55 H 0.6642 1.1714 0.2638 0.119 Uiso 1 calc R . . C56 C 0.5567(4) 1.0496(4) 0.2012(3) 0.0798(13) Uani 1 d . . . H56 H 0.5204 1.1002 0.1581 0.096 Uiso 1 calc R . . C61 C 0.5784(3) 0.7801(3) 0.0635(2) 0.0513(9) Uani 1 d . . . C62 C 0.6219(3) 0.6696(3) 0.0883(3) 0.0661(11) Uani 1 d . . . H62 H 0.5729 0.6133 0.1067 0.079 Uiso 1 calc R . . C63 C 0.7371(3) 0.6408(3) 0.0865(3) 0.0699(11) Uani 1 d . . . H63 H 0.7648 0.5660 0.1042 0.084 Uiso 1 calc R . . C64 C 0.8105(4) 0.7216(4) 0.0591(3) 0.0758(13) Uani 1 d . . . H64 H 0.8879 0.7021 0.0580 0.091 Uiso 1 calc R . . C65 C 0.7679(4) 0.8332(4) 0.0326(3) 0.0767(13) Uani 1 d . . . H65 H 0.8166 0.8886 0.0130 0.092 Uiso 1 calc R . . C66 C 0.6529(3) 0.8614(3) 0.0356(3) 0.0661(11) Uani 1 d . . . H66 H 0.6252 0.9364 0.0184 0.079 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(2) 0.0515(18) 0.057(2) 0.0019(15) 0.0061(17) 0.0017(14) C2 0.044(2) 0.0544(19) 0.062(2) 0.0041(16) 0.0031(17) -0.0018(14) C3 0.0404(19) 0.0544(18) 0.062(2) 0.0030(17) 0.0063(17) 0.0038(14) C4 0.047(2) 0.0576(19) 0.058(2) -0.0008(16) 0.0080(17) 0.0004(15) C5 0.0413(19) 0.0477(17) 0.058(2) 0.0022(15) 0.0045(16) 0.0038(13) C6 0.044(2) 0.0477(17) 0.060(2) 0.0053(15) 0.0093(17) 0.0024(14) C11 0.056(2) 0.070(2) 0.082(3) -0.014(2) 0.005(2) 0.0014(18) C21 0.042(2) 0.070(2) 0.070(3) -0.0089(19) 0.0047(18) 0.0022(16) C22 0.061(3) 0.084(3) 0.090(3) -0.006(2) 0.000(2) -0.018(2) C23 0.063(3) 0.119(4) 0.114(5) -0.022(3) 0.004(3) -0.029(3) C24 0.066(3) 0.148(5) 0.081(4) -0.030(4) -0.009(3) -0.011(3) C25 0.089(4) 0.136(5) 0.078(4) 0.009(3) -0.018(3) 0.010(3) C26 0.080(3) 0.089(3) 0.078(3) 0.004(2) -0.009(3) -0.002(2) C31 0.049(2) 0.084(3) 0.083(3) 0.002(2) 0.011(2) 0.0041(19) C41 0.071(3) 0.091(3) 0.074(3) -0.021(2) 0.013(2) 0.010(2) C51 0.045(2) 0.066(2) 0.056(2) -0.0070(17) 0.0041(17) 0.0007(15) C52 0.058(2) 0.086(3) 0.076(3) 0.007(2) 0.000(2) -0.005(2) C53 0.067(3) 0.145(5) 0.081(4) 0.011(3) -0.015(3) 0.005(3) C54 0.053(3) 0.132(4) 0.116(5) -0.054(4) -0.011(3) -0.004(3) C55 0.074(3) 0.079(3) 0.132(5) -0.027(3) -0.017(3) -0.002(2) C56 0.075(3) 0.063(2) 0.095(4) -0.011(2) -0.004(3) 0.002(2) C61 0.0425(19) 0.0532(19) 0.057(2) -0.0010(15) 0.0060(16) 0.0009(14) C62 0.057(2) 0.055(2) 0.088(3) 0.0096(18) 0.017(2) 0.0062(16) C63 0.058(2) 0.063(2) 0.089(3) 0.005(2) 0.013(2) 0.0118(18) C64 0.050(2) 0.077(3) 0.101(4) -0.007(2) 0.013(2) 0.0062(19) C65 0.052(2) 0.074(3) 0.107(4) 0.012(2) 0.021(2) -0.0068(18) C66 0.050(2) 0.055(2) 0.091(3) 0.0075(19) 0.009(2) 0.0018(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.405(5) . ? C1 C2 1.407(5) . ? C1 C11 1.506(5) . ? C2 C3 1.397(5) . ? C2 C21 1.511(5) . ? C3 C4 1.410(5) . ? C3 C31 1.525(5) . ? C4 C5 1.408(5) . ? C4 C41 1.501(6) . ? C5 C6 1.391(5) . ? C5 C51 1.492(5) . ? C6 C61 1.511(5) . ? C21 C26 1.385(6) . ? C21 C22 1.397(5) . ? C22 C23 1.383(7) . ? C23 C24 1.344(8) . ? C24 C25 1.401(8) . ? C25 C26 1.376(7) . ? C51 C52 1.381(5) . ? C51 C56 1.400(6) . ? C52 C53 1.382(6) . ? C53 C54 1.394(8) . ? C54 C55 1.341(8) . ? C55 C56 1.374(6) . ? C61 C66 1.382(5) . ? C61 C62 1.378(5) . ? C62 C63 1.384(5) . ? C63 C64 1.366(6) . ? C64 C65 1.391(6) . ? C65 C66 1.383(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 C6 C1 C2 118.6(3) . . ? C6 C1 C11 120.9(3) . . ? C2 C1 C11 120.6(3) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 C21 119.8(3) . . ? C1 C2 C21 119.1(3) . . ? C2 C3 C4 119.8(3) . . ? C2 C3 C31 120.6(3) . . ? C4 C3 C31 119.6(3) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 C41 122.0(3) . . ? C3 C4 C41 118.7(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 C51 120.6(3) . . ? C4 C5 C51 119.0(3) . . ? C5 C6 C1 120.9(3) . . ? C5 C6 C61 119.2(3) . . ? C1 C6 C61 119.9(3) . . ? C26 C21 C22 117.2(4) . . ? C26 C21 C2 121.1(4) . . ? C22 C21 C2 121.6(4) . . ? C23 C22 C21 121.0(5) . . ? C24 C23 C22 121.3(5) . . ? C23 C24 C25 118.8(5) . . ? C26 C25 C24 120.4(5) . . ? C25 C26 C21 121.2(5) . . ? C52 C51 C56 117.9(4) . . ? C52 C51 C5 121.2(3) . . ? C56 C51 C5 120.9(3) . . ? C53 C52 C51 120.8(4) . . ? C52 C53 C54 119.8(5) . . ? C55 C54 C53 119.6(4) . . ? C54 C55 C56 121.3(5) . . ? C55 C56 C51 120.4(4) . . ? C66 C61 C62 118.1(3) . . ? C66 C61 C6 121.5(3) . . ? C62 C61 C6 120.4(3) . . ? C61 C62 C63 121.2(4) . . ? C64 C63 C62 120.5(4) . . ? C63 C64 C65 119.2(4) . . ? C66 C65 C64 119.8(4) . . ? C61 C66 C65 121.2(3) . . ? _refine_diff_density_max 0.375 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.056 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END