Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Charles Winter' _publ_contact_author_address ; Department of Chemistry Wayne State University 5101 Cass Avenue Detroit MI 48202 UNITED STATES OF AMERICA ; _publ_contact_author_email CHW@CHEM.WAYNE.EDU _publ_section_title ; Film growth precursor development for metal nitrides. Synthesis, structure, and volatility of molybdenum(VI) and tungsten(VI) complexes containing bis(imido)metal fragments and various nitrogen donor ligands ; loop_ _publ_author_name 'Charles Winter' 'Oussama M. El-Kadri' 'Mary J. Heeg' # Attachment 'Samk (1b).txt' data_samk_(1b) _database_code_depnum_ccdc_archive 'CCDC 287641' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H59 N14 W2' _chemical_formula_weight 1031.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 10.368(8) _cell_length_b 16.603(14) _cell_length_c 13.099(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.82(2) _cell_angle_gamma 90.00 _cell_volume 2228(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.3 _exptl_crystal_description brick _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 5.197 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2303 _exptl_absorpt_correction_T_max 0.2563 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15976 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.52 _reflns_number_total 5309 _reflns_number_gt 3897 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^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 0.00012(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5309 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.103 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.297111(16) 0.239639(10) 0.098077(12) 0.05535(8) Uani 1 1 d . . . N1 N 0.1820(3) 0.1955(2) 0.0026(3) 0.0640(9) Uani 1 1 d . . . N2 N 0.4484(4) 0.2057(2) 0.0721(3) 0.0695(9) Uani 1 1 d . . . N3 N 0.2753(3) 0.1438(2) 0.2047(2) 0.0590(8) Uani 1 1 d . . . N4 N 0.3994(3) 0.3023(2) 0.2397(2) 0.0575(8) Uani 1 1 d . . . N5 N 0.1321(3) 0.3031(2) 0.1629(2) 0.0590(8) Uani 1 1 d . . . N6 N 0.3082(4) 0.3497(2) 0.0155(3) 0.0676(9) Uani 1 1 d . . . N7 N 0.3162(5) 0.4239(3) 0.0528(4) 0.1066(16) Uani 1 1 d . . . H7 H 0.3120 0.4375 0.1155 0.128 Uiso 0.50 1 calc PR . . C1 C 0.0854(5) 0.1532(3) -0.0686(4) 0.0825(14) Uani 1 1 d . . . C2 C 0.1473(7) 0.0859(5) -0.1184(5) 0.134(3) Uani 1 1 d . . . H2A H 0.2122 0.1070 -0.1561 0.161 Uiso 1 1 calc R . . H2B H 0.0819 0.0578 -0.1650 0.161 Uiso 1 1 calc R . . H2C H 0.1877 0.0493 -0.0663 0.161 Uiso 1 1 calc R . . C3 C -0.0146(6) 0.1195(5) -0.0014(6) 0.143(3) Uani 1 1 d . . . H3A H 0.0310 0.0893 0.0555 0.171 Uiso 1 1 calc R . . H3B H -0.0758 0.0849 -0.0429 0.171 Uiso 1 1 calc R . . H3C H -0.0604 0.1634 0.0245 0.171 Uiso 1 1 calc R . . C4 C 0.0209(9) 0.2122(5) -0.1463(6) 0.153(3) Uani 1 1 d . . . H4A H -0.0250 0.2517 -0.1123 0.184 Uiso 1 1 calc R . . H4B H -0.0397 0.1843 -0.1971 0.184 Uiso 1 1 calc R . . H4C H 0.0858 0.2383 -0.1796 0.184 Uiso 1 1 calc R . . C5 C 0.5621(5) 0.1750(4) 0.0387(5) 0.0913(16) Uani 1 1 d . . . C6 C 0.6404(9) 0.2444(4) 0.0063(10) 0.178(6) Uani 1 1 d . . . H6A H 0.5879 0.2923 0.0003 0.214 Uiso 1 1 calc R . . H6B H 0.6668 0.2325 -0.0592 0.214 Uiso 1 1 calc R . . H6C H 0.7163 0.2527 0.0572 0.214 Uiso 1 1 calc R . . C7 C 0.6376(8) 0.1258(6) 0.1222(6) 0.181(4) Uani 1 1 d . . . H7A H 0.6742 0.1603 0.1780 0.218 Uiso 1 1 calc R . . H7B H 0.7065 0.0980 0.0955 0.218 Uiso 1 1 calc R . . H7C H 0.5807 0.0872 0.1469 0.218 Uiso 1 1 calc R . . C8 C 0.5257(8) 0.1207(6) -0.0528(5) 0.172(4) Uani 1 1 d . . . H8A H 0.4641 0.0812 -0.0370 0.206 Uiso 1 1 calc R . . H8B H 0.6024 0.0942 -0.0687 0.206 Uiso 1 1 calc R . . H8C H 0.4872 0.1520 -0.1112 0.206 Uiso 1 1 calc R . . C9 C 0.2907(5) 0.0669(3) 0.1776(4) 0.0770(13) Uani 1 1 d . . . H9 H 0.3237 0.0501 0.1190 0.092 Uiso 1 1 calc R . . C10 C 0.2500 0.0167(4) 0.2500 0.086(2) Uani 1 2 d S . . H10 H 0.2500 -0.0394 0.2500 0.103 Uiso 1 2 calc SR . . C11 C 0.3316(8) 0.4738(5) -0.0240(6) 0.137(3) Uani 1 1 d . . . H11 H 0.3412 0.5293 -0.0179 0.164 Uiso 1 1 calc R . . C12 C 0.3314(6) 0.4312(5) -0.1122(6) 0.121(2) Uani 1 1 d . . . H12 H 0.3387 0.4510 -0.1776 0.146 Uiso 1 1 calc R . . C13 C 0.3184(6) 0.3550(4) -0.0847(4) 0.1041(19) Uani 1 1 d . . . H13 H 0.3165 0.3112 -0.1292 0.125 Uiso 1 1 calc R . . C14 C 0.5089(5) 0.3445(3) 0.2422(4) 0.0792(13) Uani 1 1 d . . . H14 H 0.5510 0.3533 0.1855 0.095 Uiso 1 1 calc R . . C15 C 0.0380(5) 0.3446(3) 0.1024(4) 0.0769(13) Uani 1 1 d . . . H15 H 0.0344 0.3527 0.0318 0.092 Uiso 1 1 calc R . . C16 C -0.0514(5) 0.3731(3) 0.1602(4) 0.0890(16) Uani 1 1 d . . . H16 H -0.1245 0.4047 0.1383 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.06142(12) 0.05685(12) 0.04699(11) -0.00113(7) 0.00576(8) 0.00186(7) N1 0.070(2) 0.066(2) 0.055(2) -0.0048(16) 0.0054(17) -0.0009(17) N2 0.073(2) 0.072(2) 0.064(2) 0.0029(19) 0.0123(18) 0.0124(19) N3 0.065(2) 0.0522(18) 0.059(2) -0.0004(15) 0.0076(16) 0.0024(14) N4 0.058(2) 0.061(2) 0.0513(19) 0.0029(15) 0.0010(15) -0.0062(15) N5 0.065(2) 0.060(2) 0.0478(19) -0.0007(15) -0.0046(16) 0.0096(16) N6 0.075(2) 0.075(2) 0.053(2) 0.0076(18) 0.0064(18) -0.0023(18) N7 0.160(5) 0.077(3) 0.076(3) 0.022(3) -0.001(3) -0.014(3) C1 0.080(3) 0.088(4) 0.074(3) -0.023(3) -0.006(3) 0.004(3) C2 0.127(5) 0.150(7) 0.115(5) -0.071(5) -0.012(4) 0.012(5) C3 0.090(5) 0.167(7) 0.169(7) -0.028(6) 0.013(5) -0.040(4) C4 0.171(8) 0.143(7) 0.118(6) -0.022(5) -0.064(5) 0.019(6) C5 0.065(3) 0.112(4) 0.100(4) 0.000(3) 0.023(3) 0.018(3) C6 0.115(7) 0.136(7) 0.311(18) 0.009(7) 0.120(10) 0.008(4) C7 0.136(6) 0.253(12) 0.145(7) 0.009(7) -0.010(5) 0.108(7) C8 0.182(8) 0.210(10) 0.136(7) -0.056(7) 0.066(6) 0.050(7) C9 0.105(4) 0.057(3) 0.071(3) -0.006(2) 0.019(3) 0.009(2) C10 0.111(6) 0.045(3) 0.095(5) 0.000 -0.002(4) 0.000 C11 0.184(7) 0.111(6) 0.103(5) 0.055(5) -0.016(5) -0.031(5) C12 0.120(5) 0.145(6) 0.095(5) 0.062(5) 0.005(4) -0.014(4) C13 0.140(5) 0.113(5) 0.065(3) 0.012(3) 0.032(3) -0.003(4) C14 0.073(3) 0.086(3) 0.078(3) 0.006(3) 0.011(3) -0.025(2) C15 0.078(3) 0.088(3) 0.057(3) 0.003(2) -0.011(2) 0.023(3) C16 0.078(3) 0.103(4) 0.083(4) 0.003(3) -0.001(3) 0.034(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 N2 1.749(4) . ? W1 N1 1.752(4) . ? W1 N6 2.136(4) . ? W1 N3 2.151(3) . ? W1 N4 2.247(4) . ? W1 N5 2.281(3) . ? N1 C1 1.441(6) . ? N2 C5 1.413(6) . ? N3 C9 1.342(5) . ? N3 N3 1.369(6) 2 ? N4 C14 1.330(5) . ? N4 N5 1.364(4) 2 ? N5 C15 1.347(5) . ? N5 N4 1.364(4) 2 ? N6 N7 1.323(6) . ? N6 C13 1.335(6) . ? N7 C11 1.331(7) . ? C1 C2 1.489(7) . ? C1 C4 1.494(9) . ? C1 C3 1.564(8) . ? C5 C6 1.508(9) . ? C5 C7 1.488(8) . ? C5 C8 1.501(9) . ? C9 C10 1.377(6) . ? C10 C9 1.377(6) 2 ? C11 C12 1.355(9) . ? C12 C13 1.329(8) . ? C14 C16 1.371(6) 2 ? C15 C16 1.368(6) . ? C16 C14 1.371(6) 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 N2 W1 N1 105.03(17) . . ? N2 W1 N6 93.30(16) . . ? N1 W1 N6 94.61(16) . . ? N2 W1 N3 94.28(15) . . ? N1 W1 N3 91.49(16) . . ? N6 W1 N3 168.70(13) . . ? N2 W1 N4 89.21(16) . . ? N1 W1 N4 165.29(14) . . ? N6 W1 N4 88.11(14) . . ? N3 W1 N4 83.64(13) . . ? N2 W1 N5 165.39(15) . . ? N1 W1 N5 89.51(15) . . ? N6 W1 N5 83.96(14) . . ? N3 W1 N5 86.60(13) . . ? N4 W1 N5 76.38(12) . . ? C1 N1 W1 174.4(4) . . ? C5 N2 W1 172.7(4) . . ? C9 N3 N3 107.8(3) . 2 ? C9 N3 W1 120.2(3) . . ? N3 N3 W1 130.92(11) 2 . ? C14 N4 N5 107.3(3) . 2 ? C14 N4 W1 123.9(3) . . ? N5 N4 W1 128.8(2) 2 . ? C15 N5 N4 107.4(3) . 2 ? C15 N5 W1 122.3(3) . . ? N4 N5 W1 130.1(2) 2 . ? N7 N6 C13 107.0(4) . . ? N7 N6 W1 127.9(3) . . ? C13 N6 W1 124.9(4) . . ? N6 N7 C11 107.9(5) . . ? N1 C1 C2 110.2(5) . . ? N1 C1 C4 108.5(5) . . ? C2 C1 C4 111.8(6) . . ? N1 C1 C3 105.4(4) . . ? C2 C1 C3 110.2(6) . . ? C4 C1 C3 110.6(6) . . ? N2 C5 C6 108.8(5) . . ? N2 C5 C7 109.9(5) . . ? C6 C5 C7 112.4(7) . . ? N2 C5 C8 110.1(5) . . ? C6 C5 C8 108.4(7) . . ? C7 C5 C8 107.2(6) . . ? N3 C9 C10 109.5(4) . . ? C9 C10 C9 105.4(6) . 2 ? N7 C11 C12 109.6(7) . . ? C13 C12 C11 104.6(6) . . ? C12 C13 N6 110.8(6) . . ? N4 C14 C16 110.9(4) . 2 ? N5 C15 C16 110.0(4) . . ? C15 C16 C14 104.4(4) . 2 ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.102 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.100 # Attachment 'Revised Lybd1 (2a).cif' data_lybd _database_code_depnum_ccdc_archive 'CCDC 287642' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 Mo N10' _chemical_formula_weight 620.70 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.7510(11) _cell_length_b 9.8157(10) _cell_length_c 17.518(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.306(2) _cell_angle_gamma 90.00 _cell_volume 1649.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1004 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.5 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8640 _exptl_absorpt_correction_T_max 0.9189 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11650 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6661 _reflns_number_gt 5245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^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 0.10(3) _refine_ls_number_reflns 6661 _refine_ls_number_parameters 372 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.017 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.74752(3) 0.76843(2) 0.75128(3) 0.03772(8) Uani 1 1 d . . . N1 N 0.8384(3) 0.9126(3) 0.6816(2) 0.0432(9) Uani 1 1 d . . . N2 N 0.9347(3) 1.0024(3) 0.72115(19) 0.0453(8) Uani 1 1 d . . . C1 C 0.8337(4) 0.9285(4) 0.6049(2) 0.0515(10) Uani 1 1 d . . . C2 C 0.9315(5) 1.0268(4) 0.5948(3) 0.0577(11) Uani 1 1 d . . . H2 H 0.9531 1.0573 0.5481 0.069 Uiso 1 1 calc R . . C3 C 0.9893(4) 1.0692(4) 0.6675(3) 0.0529(11) Uani 1 1 d . . . C4 C 0.7377(5) 0.8510(5) 0.5450(2) 0.0697(13) Uani 1 1 d . . . H4A H 0.7147 0.7657 0.5663 0.084 Uiso 1 1 calc R . . H4B H 0.7823 0.8344 0.5012 0.084 Uiso 1 1 calc R . . H4C H 0.6541 0.9028 0.5286 0.084 Uiso 1 1 calc R . . C5 C 1.1037(5) 1.1719(4) 0.6929(3) 0.0690(13) Uani 1 1 d . . . H5A H 1.0979 1.2038 0.7440 0.100 Uiso 1 1 d . . . H5B H 1.0926 1.2473 0.6574 0.100 Uiso 1 1 d . . . H5C H 1.1927 1.1299 0.6934 0.100 Uiso 1 1 d . . . N3 N 0.6194(3) 0.6617(3) 0.82131(17) 0.0438(8) Uani 1 1 d . . . N4 N 0.5203(3) 0.5739(3) 0.78246(19) 0.0490(8) Uani 1 1 d . . . C6 C 0.6273(4) 0.6426(4) 0.8985(2) 0.0509(10) Uani 1 1 d . . . C7 C 0.5331(5) 0.5438(4) 0.9095(3) 0.0569(11) Uani 1 1 d . . . H7 H 0.5152 0.5108 0.9565 0.068 Uiso 1 1 calc R . . C8 C 0.4698(4) 0.5035(4) 0.8352(3) 0.0509(10) Uani 1 1 d . . . C9 C 0.7218(5) 0.7231(5) 0.9598(2) 0.0694(13) Uani 1 1 d . . . H9A H 0.7920 0.7679 0.9369 0.083 Uiso 1 1 calc R . . H9B H 0.7655 0.6627 1.0000 0.083 Uiso 1 1 calc R . . H9C H 0.6681 0.7900 0.9815 0.083 Uiso 1 1 calc R . . C10 C 0.3607(5) 0.3963(4) 0.8119(3) 0.0743(14) Uani 1 1 d . . . H10A H 0.3049 0.4202 0.7628 0.089 Uiso 1 1 calc R . . H10B H 0.3024 0.3900 0.8504 0.089 Uiso 1 1 calc R . . H10C H 0.4050 0.3101 0.8073 0.089 Uiso 1 1 calc R . . N5 N 0.5318(3) 0.8455(3) 0.67886(18) 0.0468(7) Uani 1 1 d . . . N6 N 0.4304(5) 0.7460(4) 0.6615(3) 0.0492(13) Uani 1 1 d . . . C11 C 0.4702(4) 0.9572(4) 0.6423(2) 0.0510(10) Uani 1 1 d . . . C12 C 0.3363(4) 0.9233(4) 0.6037(2) 0.0551(11) Uani 1 1 d . . . H12 H 0.2727 0.9822 0.5746 0.066 Uiso 1 1 calc R . . C13 C 0.3162(4) 0.7922(4) 0.6160(2) 0.0511(10) Uani 1 1 d . . . C14 C 0.5411(5) 1.0917(4) 0.6478(3) 0.0709(13) Uani 1 1 d . . . H14A H 0.6316 1.0836 0.6798 0.085 Uiso 1 1 calc R . . H14B H 0.4866 1.1569 0.6703 0.085 Uiso 1 1 calc R . . H14C H 0.5509 1.1215 0.5969 0.085 Uiso 1 1 calc R . . C15 C 0.1952(4) 0.6968(5) 0.5916(3) 0.0695(13) Uani 1 1 d . . . H15A H 0.1918 0.6701 0.5386 0.083 Uiso 1 1 calc R . . H15B H 0.1099 0.7421 0.5965 0.083 Uiso 1 1 calc R . . H15C H 0.2066 0.6175 0.6242 0.083 Uiso 1 1 calc R . . N7 N 0.9039(3) 0.7565(3) 0.81543(16) 0.0436(7) Uani 1 1 d . . . C16 C 1.0463(6) 0.7224(5) 0.8503(4) 0.0437(13) Uani 1 1 d . . . C17 C 1.1345(4) 0.7250(5) 0.7852(3) 0.0680(12) Uani 1 1 d . . . H17A H 1.1067 0.6512 0.7499 0.082 Uiso 1 1 calc R . . H17B H 1.2313 0.7156 0.8076 0.082 Uiso 1 1 calc R . . H17C H 1.1201 0.8100 0.7578 0.082 Uiso 1 1 calc R . . C18 C 1.0508(5) 0.5855(4) 0.8892(3) 0.0745(14) Uani 1 1 d . . . H18A H 0.9848 0.5838 0.9238 0.089 Uiso 1 1 calc R . . H18B H 1.1427 0.5694 0.9180 0.089 Uiso 1 1 calc R . . H18C H 1.0276 0.5158 0.8506 0.089 Uiso 1 1 calc R . . C19 C 1.1028(5) 0.8335(6) 0.9104(3) 0.0789(15) Uani 1 1 d . . . H19A H 1.1009 0.9202 0.8849 0.095 Uiso 1 1 calc R . . H19B H 1.1969 0.8119 0.9340 0.095 Uiso 1 1 calc R . . H19C H 1.0456 0.8373 0.9497 0.095 Uiso 1 1 calc R . . N8 N 0.7413(3) 0.6289(3) 0.68969(17) 0.0426(7) Uani 1 1 d . . . C20 C 0.7533(4) 0.4954(4) 0.6551(2) 0.0460(10) Uani 1 1 d . . . C21 C 0.7834(5) 0.3917(4) 0.7194(2) 0.0677(13) Uani 1 1 d . . . H21A H 0.8665 0.4173 0.7547 0.081 Uiso 1 1 calc R . . H21B H 0.7965 0.3038 0.6977 0.081 Uiso 1 1 calc R . . H21C H 0.7065 0.3880 0.7468 0.081 Uiso 1 1 calc R . . C22 C 0.6156(5) 0.4611(4) 0.6026(3) 0.0729(14) Uani 1 1 d . . . H22A H 0.5419 0.4627 0.6323 0.087 Uiso 1 1 calc R . . H22B H 0.6214 0.3720 0.5808 0.087 Uiso 1 1 calc R . . H22C H 0.5968 0.5270 0.5616 0.087 Uiso 1 1 calc R . . C23 C 0.8687(5) 0.4974(5) 0.6078(3) 0.0880(17) Uani 1 1 d . . . H23A H 0.8434 0.5574 0.5643 0.106 Uiso 1 1 calc R . . H23B H 0.8825 0.4071 0.5895 0.106 Uiso 1 1 calc R . . H23C H 0.9533 0.5290 0.6395 0.106 Uiso 1 1 calc R . . N9 N 0.7973(3) 1.0497(3) 0.84197(19) 0.0443(8) Uani 1 1 d . . . N10 N 0.6898(4) 0.9621(4) 0.8203(2) 0.0467(10) Uani 1 1 d . . . C24 C 0.7637(4) 1.1510(4) 0.8857(2) 0.0496(10) Uani 1 1 d . . . C25 C 0.6283(4) 1.1278(4) 0.8941(2) 0.0543(10) Uani 1 1 d . . . H25 H 0.5756 1.1811 0.9220 0.065 Uiso 1 1 calc R . . C26 C 0.5856(4) 1.0109(4) 0.8535(3) 0.0511(10) Uani 1 1 d . . . C27 C 0.8664(5) 1.2605(4) 0.9154(3) 0.0673(12) Uani 1 1 d . . . H27A H 0.9096 1.2401 0.9677 0.081 Uiso 1 1 calc R . . H27B H 0.8190 1.3464 0.9141 0.081 Uiso 1 1 calc R . . H27C H 0.9364 1.2653 0.8833 0.081 Uiso 1 1 calc R . . C28 C 0.4460(5) 0.9458(5) 0.8452(3) 0.0703(13) Uani 1 1 d . . . H28A H 0.4386 0.8742 0.8072 0.100 Uiso 1 1 d . . . H28B H 0.3751 1.0127 0.8287 0.100 Uiso 1 1 d . . . H28C H 0.4339 0.9082 0.8941 0.100 Uiso 1 1 d . . . H1N6 H 0.445(4) 0.665(4) 0.697(2) 0.063(12) Uiso 1 1 d . . . H1N9 H 0.876(5) 1.036(5) 0.815(3) 0.101(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03822(15) 0.03660(13) 0.03855(14) -0.0027(3) 0.00740(10) -0.0074(3) N1 0.037(2) 0.046(2) 0.048(2) 0.0026(16) 0.0099(17) -0.0067(15) N2 0.042(2) 0.0396(16) 0.056(2) -0.0025(15) 0.0121(16) -0.0111(14) C1 0.052(3) 0.054(2) 0.047(3) 0.0073(19) 0.006(2) -0.005(2) C2 0.056(3) 0.064(3) 0.057(3) 0.012(2) 0.020(2) -0.005(2) C3 0.046(3) 0.049(2) 0.066(3) 0.006(2) 0.018(2) -0.002(2) C4 0.089(4) 0.078(3) 0.040(3) 0.005(2) 0.007(2) -0.011(3) C5 0.054(3) 0.056(2) 0.099(4) 0.000(2) 0.020(3) -0.012(2) N3 0.042(2) 0.0484(17) 0.0408(19) -0.0001(14) 0.0077(15) -0.0102(14) N4 0.0393(19) 0.0499(18) 0.060(2) 0.0019(16) 0.0150(17) -0.0062(15) C6 0.050(3) 0.062(2) 0.043(2) -0.0010(19) 0.015(2) 0.003(2) C7 0.056(3) 0.065(3) 0.054(3) 0.016(2) 0.021(2) -0.001(2) C8 0.038(2) 0.048(2) 0.069(3) 0.009(2) 0.018(2) 0.0012(18) C9 0.067(3) 0.095(3) 0.047(3) -0.008(2) 0.015(2) -0.011(3) C10 0.056(3) 0.060(3) 0.109(4) 0.019(3) 0.021(3) -0.011(2) N5 0.0447(19) 0.0455(18) 0.0477(19) -0.0046(15) 0.0014(15) -0.0074(15) N6 0.050(3) 0.043(2) 0.052(3) -0.0018(18) -0.001(2) -0.0074(18) C11 0.049(3) 0.048(2) 0.056(3) 0.0041(18) 0.009(2) 0.0013(18) C12 0.051(3) 0.061(3) 0.050(2) 0.009(2) 0.000(2) 0.008(2) C13 0.039(2) 0.066(3) 0.047(2) -0.003(2) 0.004(2) -0.005(2) C14 0.078(3) 0.050(2) 0.082(3) 0.007(2) 0.006(3) 0.000(2) C15 0.045(3) 0.100(3) 0.060(3) 0.002(2) 0.000(2) -0.017(2) N7 0.0440(18) 0.053(2) 0.0344(16) 0.0021(14) 0.0088(14) -0.0115(15) C16 0.027(2) 0.061(3) 0.043(3) -0.001(2) 0.007(2) -0.004(2) C17 0.048(3) 0.080(3) 0.085(3) -0.015(3) 0.034(2) -0.004(2) C18 0.072(3) 0.077(3) 0.068(3) 0.018(2) -0.007(3) -0.007(2) C19 0.048(3) 0.109(4) 0.075(3) -0.022(3) -0.002(3) -0.019(3) N8 0.048(2) 0.0454(16) 0.0368(17) -0.0024(13) 0.0134(15) -0.0100(14) C20 0.052(3) 0.042(2) 0.045(2) -0.0084(16) 0.010(2) -0.0100(17) C21 0.086(4) 0.047(2) 0.069(3) -0.003(2) 0.010(3) 0.004(2) C22 0.083(4) 0.068(3) 0.061(3) -0.019(2) -0.006(3) -0.014(2) C23 0.096(4) 0.075(3) 0.110(4) -0.027(3) 0.066(4) -0.011(3) N9 0.041(2) 0.0459(17) 0.049(2) -0.0092(15) 0.0172(17) -0.0089(15) N10 0.038(2) 0.047(2) 0.054(2) -0.0113(17) 0.0063(17) -0.0170(16) C24 0.056(3) 0.048(2) 0.044(2) -0.0002(18) 0.005(2) -0.0080(19) C25 0.052(3) 0.057(2) 0.056(3) -0.009(2) 0.016(2) 0.006(2) C26 0.042(3) 0.063(3) 0.048(3) -0.008(2) 0.008(2) -0.001(2) C27 0.078(3) 0.062(3) 0.062(3) -0.016(2) 0.013(2) -0.023(2) C28 0.043(3) 0.091(3) 0.079(3) -0.016(3) 0.018(2) -0.010(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 N7 1.729(3) . ? Mo1 N8 1.738(3) . ? Mo1 N1 2.160(4) . ? Mo1 N3 2.171(3) . ? Mo1 N10 2.374(4) . ? Mo1 N5 2.378(3) . ? N1 C1 1.345(5) . ? N1 N2 1.381(4) . ? N2 C3 1.332(5) . ? C1 C2 1.390(5) . ? C1 C4 1.484(6) . ? C2 C3 1.363(6) . ? C3 C5 1.511(6) . ? N3 C6 1.354(4) . ? N3 N4 1.380(4) . ? N4 C8 1.318(5) . ? C6 C7 1.373(5) . ? C6 C9 1.507(5) . ? C7 C8 1.393(6) . ? C8 C10 1.501(5) . ? N5 C11 1.354(5) . ? N5 N6 1.385(5) . ? N6 C13 1.327(6) . ? C11 C12 1.399(5) . ? C11 C14 1.485(5) . ? C12 C13 1.326(5) . ? C13 C15 1.507(5) . ? N7 C16 1.453(7) . ? C16 C18 1.504(6) . ? C16 C17 1.545(7) . ? C16 C19 1.547(7) . ? N8 C20 1.457(4) . ? C20 C21 1.507(5) . ? C20 C23 1.512(6) . ? C20 C22 1.523(5) . ? N9 C24 1.331(5) . ? N9 N10 1.356(4) . ? N10 C26 1.346(5) . ? C24 C25 1.374(5) . ? C24 C27 1.497(5) . ? C25 C26 1.376(5) . ? C26 C28 1.487(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 N7 Mo1 N8 106.20(14) . . ? N7 Mo1 N1 90.49(13) . . ? N8 Mo1 N1 97.92(14) . . ? N7 Mo1 N3 97.47(12) . . ? N8 Mo1 N3 90.62(12) . . ? N1 Mo1 N3 166.26(12) . . ? N7 Mo1 N10 89.14(13) . . ? N8 Mo1 N10 164.18(13) . . ? N1 Mo1 N10 85.52(13) . . ? N3 Mo1 N10 83.43(11) . . ? N7 Mo1 N5 164.11(13) . . ? N8 Mo1 N5 89.44(13) . . ? N1 Mo1 N5 84.44(12) . . ? N3 Mo1 N5 84.91(11) . . ? N10 Mo1 N5 75.48(11) . . ? C1 N1 N2 109.0(3) . . ? C1 N1 Mo1 134.1(3) . . ? N2 N1 Mo1 116.5(3) . . ? C3 N2 N1 106.4(3) . . ? N1 C1 C2 107.8(4) . . ? N1 C1 C4 123.5(4) . . ? C2 C1 C4 128.7(4) . . ? C3 C2 C1 105.8(4) . . ? N2 C3 C2 111.0(4) . . ? N2 C3 C5 119.2(4) . . ? C2 C3 C5 129.7(4) . . ? C6 N3 N4 108.4(3) . . ? C6 N3 Mo1 134.1(3) . . ? N4 N3 Mo1 116.5(2) . . ? C8 N4 N3 107.3(3) . . ? N3 C6 C7 108.5(4) . . ? N3 C6 C9 123.9(4) . . ? C7 C6 C9 127.6(4) . . ? C6 C7 C8 105.4(4) . . ? N4 C8 C7 110.4(4) . . ? N4 C8 C10 120.7(4) . . ? C7 C8 C10 128.9(4) . . ? C11 N5 N6 103.2(4) . . ? C11 N5 Mo1 141.7(3) . . ? N6 N5 Mo1 114.9(3) . . ? C13 N6 N5 112.3(4) . . ? N5 C11 C12 109.4(3) . . ? N5 C11 C14 121.8(4) . . ? C12 C11 C14 128.8(4) . . ? C13 C12 C11 107.7(4) . . ? N6 C13 C12 107.3(4) . . ? N6 C13 C15 119.2(4) . . ? C12 C13 C15 133.5(4) . . ? C16 N7 Mo1 162.7(3) . . ? N7 C16 C18 110.1(4) . . ? N7 C16 C17 107.6(4) . . ? C18 C16 C17 112.0(4) . . ? N7 C16 C19 108.7(4) . . ? C18 C16 C19 110.1(5) . . ? C17 C16 C19 108.3(4) . . ? C20 N8 Mo1 166.0(3) . . ? N8 C20 C21 108.4(3) . . ? N8 C20 C23 109.8(3) . . ? C21 C20 C23 110.7(4) . . ? N8 C20 C22 108.8(3) . . ? C21 C20 C22 109.6(3) . . ? C23 C20 C22 109.5(4) . . ? C24 N9 N10 112.2(3) . . ? C26 N10 N9 105.0(3) . . ? C26 N10 Mo1 140.4(3) . . ? N9 N10 Mo1 114.1(3) . . ? N9 C24 C25 106.1(3) . . ? N9 C24 C27 121.2(4) . . ? C25 C24 C27 132.6(4) . . ? C24 C25 C26 106.9(4) . . ? N10 C26 C25 109.8(4) . . ? N10 C26 C28 123.6(4) . . ? C25 C26 C28 126.6(4) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.391 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.054 # Attachment 'Ussa (2b).txt' data_ussa_(2b) _database_code_depnum_ccdc_archive 'CCDC 287643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 N10 W' _chemical_formula_weight 708.61 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.742(2) _cell_length_b 9.821(2) _cell_length_c 17.521(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.240(5) _cell_angle_gamma 90.00 _cell_volume 1649.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 939 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27. _exptl_crystal_description chunks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 3.534 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4378 _exptl_absorpt_correction_T_max 0.5383 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11684 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4919 _reflns_number_gt 4521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^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 0.00030(14) _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 0.044(8) _refine_ls_number_reflns 4919 _refine_ls_number_parameters 375 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.24788(4) 0.231101(15) 0.24987(3) 0.03636(7) Uani 1 1 d . . . N1 N 0.0898(6) 0.2434(5) 0.1849(3) 0.0439(11) Uani 1 1 d . . . C1 C -0.0526(19) 0.2762(10) 0.1532(9) 0.051(3) Uani 1 1 d . . . C2 C -0.0568(8) 0.4143(7) 0.1121(4) 0.073(2) Uani 1 1 d . . . H2A H -0.0249 0.4841 0.1495 0.088 Uiso 1 1 calc R . . H2B H -0.1507 0.4338 0.0873 0.088 Uiso 1 1 calc R . . H2C H 0.0026 0.4115 0.0739 0.088 Uiso 1 1 calc R . . C3 C -0.1093(8) 0.1664(10) 0.0895(5) 0.078(2) Uani 1 1 d . . . H3A H -0.0564 0.1709 0.0483 0.094 Uiso 1 1 calc R . . H3B H -0.2057 0.1842 0.0692 0.094 Uiso 1 1 calc R . . H3C H -0.1001 0.0772 0.1124 0.094 Uiso 1 1 calc R . . C4 C -0.1411(8) 0.2777(7) 0.2134(5) 0.0648(18) Uani 1 1 d . . . H4A H -0.1394 0.1895 0.2371 0.078 Uiso 1 1 calc R . . H4B H -0.2352 0.3002 0.1901 0.078 Uiso 1 1 calc R . . H4C H -0.1064 0.3444 0.2520 0.078 Uiso 1 1 calc R . . N2 N 0.2539(5) 0.3708(4) 0.3133(2) 0.0420(10) Uani 1 1 d . . . C5 C 0.2430(6) 0.5043(5) 0.3477(3) 0.0467(14) Uani 1 1 d . . . C6 C 0.2104(9) 0.6086(6) 0.2839(4) 0.0679(18) Uani 1 1 d . . . H6A H 0.2770 0.6011 0.2497 0.081 Uiso 1 1 calc R . . H6B H 0.2152 0.6982 0.3061 0.081 Uiso 1 1 calc R . . H6C H 0.1183 0.5929 0.2552 0.081 Uiso 1 1 calc R . . C7 C 0.3802(8) 0.5376(7) 0.3995(4) 0.074(2) Uani 1 1 d . . . H7A H 0.4036 0.4668 0.4373 0.089 Uiso 1 1 calc R . . H7B H 0.3720 0.6226 0.4254 0.089 Uiso 1 1 calc R . . H7C H 0.4521 0.5448 0.3687 0.089 Uiso 1 1 calc R . . C8 C 0.1253(9) 0.5027(8) 0.3945(5) 0.084(2) Uani 1 1 d . . . H8A H 0.0390 0.4811 0.3609 0.100 Uiso 1 1 calc R . . H8B H 0.1181 0.5907 0.4173 0.100 Uiso 1 1 calc R . . H8C H 0.1447 0.4354 0.4347 0.100 Uiso 1 1 calc R . . N3 N 0.3752(4) 0.3352(5) 0.1801(3) 0.0410(10) Uani 1 1 d . . . N4 N 0.4746(4) 0.4248(4) 0.2190(3) 0.0433(11) Uani 1 1 d . . . C9 C 0.3668(6) 0.3536(6) 0.1028(3) 0.0472(13) Uani 1 1 d . . . C10 C 0.4589(7) 0.4522(6) 0.0917(4) 0.0546(15) Uani 1 1 d . . . H10 H 0.4749 0.4858 0.0444 0.066 Uiso 1 1 calc R . . C11 C 0.5243(6) 0.4926(6) 0.1648(4) 0.0502(15) Uani 1 1 d . . . C12 C 0.2715(9) 0.2735(7) 0.0425(4) 0.068(2) Uani 1 1 d . . . H12A H 0.3194 0.1941 0.0289 0.082 Uiso 1 1 calc R . . H12B H 0.2436 0.3288 -0.0027 0.082 Uiso 1 1 calc R . . H12C H 0.1904 0.2461 0.0628 0.082 Uiso 1 1 calc R . . C13 C 0.6366(7) 0.6002(7) 0.1884(5) 0.074(2) Uani 1 1 d . . . H13A H 0.5939 0.6884 0.1878 0.089 Uiso 1 1 calc R . . H13B H 0.7006 0.5992 0.1525 0.089 Uiso 1 1 calc R . . H13C H 0.6862 0.5809 0.2396 0.089 Uiso 1 1 calc R . . N5 N 0.4619(5) 0.1543(5) 0.3219(3) 0.0438(10) Uani 1 1 d . . . N6 N 0.5599(15) 0.2539(8) 0.3425(8) 0.049(3) Uani 1 1 d . . . C14 C 0.5230(6) 0.0415(6) 0.3581(4) 0.0510(14) Uani 1 1 d . . . C15 C 0.6560(6) 0.0743(7) 0.3966(4) 0.0562(16) Uani 1 1 d . . . H15 H 0.7194 0.0151 0.4256 0.067 Uiso 1 1 calc R . . C16 C 0.6766(7) 0.2085(7) 0.3842(4) 0.0489(14) Uani 1 1 d . . . C17 C 0.4547(8) -0.0929(6) 0.3516(4) 0.0676(19) Uani 1 1 d . . . H17A H 0.3565 -0.0816 0.3504 0.081 Uiso 1 1 calc R . . H17B H 0.4936 -0.1478 0.3955 0.081 Uiso 1 1 calc R . . H17C H 0.4696 -0.1368 0.3048 0.081 Uiso 1 1 calc R . . C18 C 0.7976(7) 0.3002(8) 0.4094(4) 0.0685(19) Uani 1 1 d . . . H18A H 0.7907 0.3779 0.3757 0.082 Uiso 1 1 calc R . . H18B H 0.8826 0.2521 0.4073 0.082 Uiso 1 1 calc R . . H18C H 0.7976 0.3299 0.4617 0.082 Uiso 1 1 calc R . . N7 N 0.1610(5) 0.0857(6) 0.3195(3) 0.0412(14) Uani 1 1 d . . . N8 N 0.0625(5) -0.0039(4) 0.2806(3) 0.0448(11) Uani 1 1 d . . . C19 C 0.1648(7) 0.0714(6) 0.3962(4) 0.0521(15) Uani 1 1 d . . . C20 C 0.0665(7) -0.0263(6) 0.4076(4) 0.0567(16) Uani 1 1 d . . . H20 H 0.0451 -0.0556 0.4546 0.068 Uiso 1 1 calc R . . C21 C 0.0081(7) -0.0697(6) 0.3346(4) 0.0518(15) Uani 1 1 d . . . C22 C 0.2613(8) 0.1479(8) 0.4567(4) 0.0682(19) Uani 1 1 d . . . H22A H 0.3477 0.0991 0.4697 0.082 Uiso 1 1 calc R . . H22B H 0.2197 0.1575 0.5021 0.082 Uiso 1 1 calc R . . H22C H 0.2787 0.2364 0.4372 0.082 Uiso 1 1 calc R . . C23 C -0.1065(7) -0.1719(7) 0.3108(4) 0.0678(19) Uani 1 1 d . . . H23A H -0.1954 -0.1283 0.3085 0.081 Uiso 1 1 calc R . . H23B H -0.0974 -0.2446 0.3479 0.081 Uiso 1 1 calc R . . H23C H -0.0999 -0.2080 0.2606 0.081 Uiso 1 1 calc R . . N9 N 0.3053(6) 0.0386(6) 0.1810(3) 0.0452(15) Uani 1 1 d . . . N10 N 0.1989(5) -0.0488(5) 0.1597(3) 0.0457(11) Uani 1 1 d . . . C24 C 0.4091(6) -0.0115(7) 0.1480(4) 0.0520(15) Uani 1 1 d . . . C25 C 0.3666(6) -0.1288(6) 0.1072(3) 0.0542(15) Uani 1 1 d . . . H25 H 0.4194 -0.1823 0.0795 0.065 Uiso 1 1 calc R . . C26 C 0.2300(6) -0.1511(6) 0.1157(3) 0.0481(13) Uani 1 1 d . . . C27 C 0.5521(6) 0.0558(7) 0.1574(4) 0.0670(19) Uani 1 1 d . . . H27A H 0.5461 0.1361 0.1258 0.080 Uiso 1 1 calc R . . H27B H 0.6176 -0.0066 0.1416 0.080 Uiso 1 1 calc R . . H27C H 0.5828 0.0803 0.2108 0.080 Uiso 1 1 calc R . . C28 C 0.1288(9) -0.2598(6) 0.0868(4) 0.0594(17) Uani 1 1 d . . . H28A H 0.0603 -0.2662 0.1198 0.071 Uiso 1 1 calc R . . H28B H 0.1770 -0.3451 0.0869 0.071 Uiso 1 1 calc R . . H28C H 0.0836 -0.2386 0.0349 0.071 Uiso 1 1 calc R . . H1N6 H 0.554(7) 0.316(7) 0.308(4) 0.06(2) Uiso 1 1 d . . . H1N H 0.129(5) -0.049(5) 0.187(3) 0.021(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03705(9) 0.03314(10) 0.03836(10) -0.0040(3) 0.00525(7) -0.0060(3) N1 0.047(3) 0.041(3) 0.045(3) -0.002(2) 0.010(2) -0.009(2) C1 0.045(6) 0.060(6) 0.048(6) -0.010(5) 0.009(5) -0.004(5) C2 0.063(4) 0.069(5) 0.078(5) 0.018(4) -0.012(4) -0.003(4) C3 0.061(5) 0.090(6) 0.077(6) -0.026(5) -0.005(4) -0.017(5) C4 0.047(4) 0.079(5) 0.071(5) 0.007(4) 0.015(3) 0.004(3) N2 0.051(3) 0.045(3) 0.031(2) -0.0024(19) 0.008(2) -0.012(2) C5 0.056(3) 0.038(3) 0.048(3) -0.006(2) 0.012(3) -0.005(3) C6 0.092(5) 0.043(3) 0.068(4) -0.001(3) 0.012(4) 0.001(3) C7 0.091(5) 0.058(4) 0.065(4) -0.011(3) -0.008(4) -0.013(4) C8 0.101(7) 0.064(5) 0.100(6) -0.017(4) 0.057(5) -0.008(4) N3 0.039(2) 0.040(2) 0.046(3) 0.000(2) 0.011(2) -0.007(2) N4 0.035(2) 0.040(2) 0.054(3) 0.002(2) 0.005(2) -0.0096(19) C9 0.042(3) 0.055(4) 0.045(3) 0.001(3) 0.010(3) 0.000(3) C10 0.055(4) 0.061(4) 0.052(4) 0.016(3) 0.019(3) 0.002(3) C11 0.041(3) 0.042(3) 0.069(4) 0.012(3) 0.015(3) 0.001(2) C12 0.075(5) 0.092(6) 0.037(3) 0.001(3) 0.009(3) -0.015(4) C13 0.055(4) 0.053(4) 0.114(6) 0.018(4) 0.013(4) -0.014(3) N5 0.042(2) 0.038(3) 0.049(3) -0.001(2) 0.004(2) -0.007(2) N6 0.042(6) 0.037(4) 0.061(6) 0.004(3) -0.009(4) -0.007(3) C14 0.054(3) 0.041(3) 0.056(4) 0.002(3) 0.004(3) 0.004(3) C15 0.050(3) 0.059(4) 0.057(4) 0.009(3) 0.002(3) 0.006(3) C16 0.047(3) 0.057(4) 0.041(3) 0.002(3) 0.002(3) -0.002(3) C17 0.077(5) 0.042(3) 0.082(5) 0.005(3) 0.007(4) -0.008(3) C18 0.054(4) 0.089(5) 0.058(4) 0.009(4) -0.004(3) -0.020(4) N7 0.039(3) 0.042(3) 0.042(3) 0.003(2) 0.006(2) -0.011(2) N8 0.040(2) 0.036(2) 0.059(3) 0.000(2) 0.012(2) -0.0074(19) C19 0.055(4) 0.045(3) 0.057(4) 0.010(3) 0.011(3) -0.001(3) C20 0.062(4) 0.052(4) 0.058(4) 0.015(3) 0.014(3) -0.004(3) C21 0.049(4) 0.036(3) 0.073(4) 0.004(3) 0.016(3) 0.000(3) C22 0.087(5) 0.072(5) 0.043(4) 0.003(3) 0.003(4) -0.011(4) C23 0.051(4) 0.055(4) 0.102(6) -0.001(4) 0.027(4) -0.017(3) N9 0.043(3) 0.044(4) 0.049(3) -0.007(2) 0.009(2) -0.010(2) N10 0.042(3) 0.044(3) 0.052(3) -0.009(2) 0.012(2) -0.011(2) C24 0.043(3) 0.055(4) 0.059(4) -0.009(3) 0.011(3) -0.002(3) C25 0.056(4) 0.055(4) 0.051(4) -0.013(3) 0.009(3) 0.009(3) C26 0.059(3) 0.043(3) 0.043(3) -0.008(2) 0.011(3) -0.008(3) C27 0.039(3) 0.081(5) 0.083(5) -0.018(4) 0.016(3) -0.006(3) C28 0.075(5) 0.052(4) 0.052(4) -0.011(3) 0.012(3) -0.014(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 N1 1.749(5) . ? W1 N2 1.760(4) . ? W1 N7 2.147(5) . ? W1 N3 2.149(4) . ? W1 N5 2.360(5) . ? W1 N9 2.363(6) . ? N1 C1 1.437(18) . ? C1 C4 1.475(17) . ? C1 C2 1.533(13) . ? C1 C3 1.579(15) . ? N2 C5 1.455(7) . ? C5 C6 1.508(8) . ? C5 C7 1.512(8) . ? C5 C8 1.524(9) . ? N3 C9 1.354(7) . ? N3 N4 1.394(6) . ? N4 C11 1.320(7) . ? C9 C10 1.357(8) . ? C9 C12 1.499(9) . ? C10 C11 1.384(9) . ? C11 C13 1.525(8) . ? N5 C14 1.361(7) . ? N5 N6 1.370(12) . ? N6 C16 1.315(15) . ? C14 C15 1.388(8) . ? C14 C17 1.474(8) . ? C15 C16 1.356(9) . ? C16 C18 1.487(9) . ? N7 C19 1.346(8) . ? N7 N8 1.389(6) . ? N8 C21 1.332(7) . ? C19 C20 1.394(8) . ? C19 C22 1.488(9) . ? C20 C21 1.372(9) . ? C21 C23 1.504(8) . ? N9 C24 1.344(8) . ? N9 N10 1.347(7) . ? N10 C26 1.334(7) . ? C24 C25 1.380(8) . ? C24 C27 1.524(8) . ? C25 C26 1.382(8) . ? C26 C28 1.480(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W1 N2 106.5(2) . . ? N1 W1 N7 91.5(2) . . ? N2 W1 N7 97.6(2) . . ? N1 W1 N3 97.3(2) . . ? N2 W1 N3 91.76(19) . . ? N7 W1 N3 164.9(2) . . ? N1 W1 N5 164.1(2) . . ? N2 W1 N5 89.11(19) . . ? N7 W1 N5 83.34(18) . . ? N3 W1 N5 84.94(17) . . ? N1 W1 N9 89.1(2) . . ? N2 W1 N9 164.1(2) . . ? N7 W1 N9 84.9(2) . . ? N3 W1 N9 82.95(17) . . ? N5 W1 N9 75.54(18) . . ? C1 N1 W1 160.9(7) . . ? N1 C1 C4 111.9(11) . . ? N1 C1 C2 108.8(11) . . ? C4 C1 C2 110.9(9) . . ? N1 C1 C3 108.2(9) . . ? C4 C1 C3 109.7(11) . . ? C2 C1 C3 107.2(11) . . ? C5 N2 W1 165.3(4) . . ? N2 C5 C6 109.0(5) . . ? N2 C5 C7 108.8(5) . . ? C6 C5 C7 110.2(5) . . ? N2 C5 C8 109.3(5) . . ? C6 C5 C8 109.1(6) . . ? C7 C5 C8 110.4(6) . . ? C9 N3 N4 108.5(4) . . ? C9 N3 W1 134.0(4) . . ? N4 N3 W1 116.3(3) . . ? C11 N4 N3 106.2(5) . . ? N3 C9 C10 108.4(5) . . ? N3 C9 C12 123.6(5) . . ? C10 C9 C12 128.0(6) . . ? C9 C10 C11 106.2(5) . . ? N4 C11 C10 110.7(5) . . ? N4 C11 C13 119.5(6) . . ? C10 C11 C13 129.8(6) . . ? C14 N5 N6 103.4(6) . . ? C14 N5 W1 141.4(4) . . ? N6 N5 W1 114.9(6) . . ? C16 N6 N5 113.4(7) . . ? N5 C14 C15 109.4(5) . . ? N5 C14 C17 122.6(6) . . ? C15 C14 C17 127.9(6) . . ? C16 C15 C14 107.4(6) . . ? N6 C16 C15 106.3(7) . . ? N6 C16 C18 121.4(7) . . ? C15 C16 C18 132.3(6) . . ? C19 N7 N8 108.5(5) . . ? C19 N7 W1 133.9(4) . . ? N8 N7 W1 116.8(4) . . ? C21 N8 N7 106.7(5) . . ? N7 C19 C20 108.5(6) . . ? N7 C19 C22 124.0(6) . . ? C20 C19 C22 127.5(6) . . ? C21 C20 C19 105.2(6) . . ? N8 C21 C20 111.1(6) . . ? N8 C21 C23 119.7(6) . . ? C20 C21 C23 129.1(6) . . ? C24 N9 N10 104.4(5) . . ? C24 N9 W1 141.0(4) . . ? N10 N9 W1 114.3(4) . . ? C26 N10 N9 113.4(5) . . ? N9 C24 C25 110.5(6) . . ? N9 C24 C27 122.5(6) . . ? C25 C24 C27 127.0(6) . . ? C24 C25 C26 106.4(5) . . ? N10 C26 C25 105.4(5) . . ? N10 C26 C28 122.4(6) . . ? C25 C26 C28 132.3(6) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.876 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.078 # Attachment 'Moka (3a).txt' data_moka_(3a) _database_code_depnum_ccdc_archive 'CCDC 287644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 Mo N6' _chemical_formula_weight 596.75 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.211(2) _cell_length_b 10.9777(11) _cell_length_c 19.579(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.467(2) _cell_angle_gamma 90.00 _cell_volume 3590.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 21.5 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9089 _exptl_absorpt_correction_T_max 0.9261 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25925 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8538 _reflns_number_gt 3228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^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 0.00016(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8538 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.30030(2) 0.41738(3) 0.76988(2) 0.06261(17) Uani 1 1 d . . . N1 N 0.3994(2) 0.4045(3) 0.78253(19) 0.0668(10) Uani 1 1 d . . . C1 C 0.4818(3) 0.4380(4) 0.7980(3) 0.0821(15) Uani 1 1 d . . . C2 C 0.5012(4) 0.5560(8) 0.8347(7) 0.256(6) Uani 1 1 d . . . H2A H 0.4656 0.6166 0.8035 0.307 Uiso 1 1 calc R . . H2B H 0.5554 0.5770 0.8437 0.307 Uiso 1 1 calc R . . H2C H 0.4953 0.5521 0.8813 0.307 Uiso 1 1 calc R . . C3 C 0.5365(4) 0.3431(9) 0.8421(6) 0.230(5) Uani 1 1 d . . . H3A H 0.5389 0.3445 0.8920 0.276 Uiso 1 1 calc R . . H3B H 0.5890 0.3575 0.8432 0.276 Uiso 1 1 calc R . . H3C H 0.5176 0.2650 0.8201 0.276 Uiso 1 1 calc R . . C4 C 0.4892(5) 0.4454(9) 0.7261(5) 0.212(5) Uani 1 1 d . . . H4A H 0.4752 0.3683 0.7011 0.254 Uiso 1 1 calc R . . H4B H 0.5433 0.4656 0.7342 0.254 Uiso 1 1 calc R . . H4C H 0.4538 0.5073 0.6959 0.254 Uiso 1 1 calc R . . N2 N 0.2874(2) 0.5544(3) 0.8064(2) 0.0682(10) Uani 1 1 d . . . C5 C 0.2866(3) 0.6656(5) 0.8457(3) 0.0807(14) Uani 1 1 d . . . C6 C 0.3431(4) 0.6531(6) 0.9239(3) 0.158(3) Uani 1 1 d . . . H6A H 0.3277 0.5849 0.9460 0.189 Uiso 1 1 calc R . . H6B H 0.3423 0.7260 0.9506 0.189 Uiso 1 1 calc R . . H6C H 0.3960 0.6401 0.9260 0.189 Uiso 1 1 calc R . . C7 C 0.2051(4) 0.6822(10) 0.8438(5) 0.231(5) Uani 1 1 d . . . H7A H 0.1723 0.7236 0.7987 0.277 Uiso 1 1 calc R . . H7B H 0.2080 0.7296 0.8859 0.277 Uiso 1 1 calc R . . H7C H 0.1822 0.6040 0.8453 0.277 Uiso 1 1 calc R . . C8 C 0.3116(7) 0.7697(6) 0.8122(4) 0.240(6) Uani 1 1 d . . . H8A H 0.3567 0.7464 0.8015 0.288 Uiso 1 1 calc R . . H8B H 0.3263 0.8369 0.8465 0.288 Uiso 1 1 calc R . . H8C H 0.2681 0.7936 0.7670 0.288 Uiso 1 1 calc R . . N3 N 0.2410(2) 0.4281(3) 0.6561(2) 0.0730(11) Uani 1 1 d . . . N4 N 0.2466(2) 0.3031(3) 0.6623(2) 0.0723(11) Uani 1 1 d . . . C9 C 0.1876(2) 0.4594(4) 0.5882(2) 0.0569(11) Uani 1 1 d . . . C10 C 0.1605(3) 0.3524(4) 0.5506(3) 0.0677(14) Uani 1 1 d . . . C11 C 0.1975(2) 0.2573(4) 0.5983(2) 0.0609(11) Uani 1 1 d . . . C12 C 0.1674(3) 0.5913(4) 0.5671(2) 0.0697(13) Uani 1 1 d . . . C13 C 0.2441(3) 0.6662(4) 0.5901(3) 0.1003(18) Uani 1 1 d . . . H13A H 0.2731 0.6614 0.6431 0.120 Uiso 1 1 calc R . . H13B H 0.2308 0.7496 0.5759 0.120 Uiso 1 1 calc R . . H13C H 0.2767 0.6347 0.5659 0.120 Uiso 1 1 calc R . . C14 C 0.1180(3) 0.6394(5) 0.6072(3) 0.1084(19) Uani 1 1 d . . . H14A H 0.0685 0.5954 0.5913 0.130 Uiso 1 1 calc R . . H14B H 0.1072 0.7243 0.5960 0.130 Uiso 1 1 calc R . . H14C H 0.1470 0.6293 0.6599 0.130 Uiso 1 1 calc R . . C15 C 0.1215(4) 0.6011(4) 0.4832(3) 0.125(2) Uani 1 1 d . . . H15A H 0.1531 0.5673 0.4586 0.150 Uiso 1 1 calc R . . H15B H 0.1104 0.6852 0.4696 0.150 Uiso 1 1 calc R . . H15C H 0.0720 0.5570 0.4686 0.150 Uiso 1 1 calc R . . C16 C 0.1900(3) 0.1206(4) 0.5859(3) 0.0771(14) Uani 1 1 d . . . C17 C 0.2305(4) 0.0858(5) 0.5348(4) 0.137(3) Uani 1 1 d . . . H17A H 0.2260 -0.0005 0.5264 0.164 Uiso 1 1 calc R . . H17B H 0.2860 0.1082 0.5574 0.164 Uiso 1 1 calc R . . H17C H 0.2052 0.1277 0.4882 0.164 Uiso 1 1 calc R . . C18 C 0.1027(4) 0.0860(5) 0.5483(4) 0.130(2) Uani 1 1 d . . . H18A H 0.0760 0.1055 0.5804 0.156 Uiso 1 1 calc R . . H18B H 0.0982 0.0001 0.5381 0.156 Uiso 1 1 calc R . . H18C H 0.0783 0.1302 0.5025 0.156 Uiso 1 1 calc R . . C19 C 0.2296(4) 0.0539(5) 0.6594(3) 0.144(3) Uani 1 1 d . . . H19A H 0.2041 0.0765 0.6921 0.173 Uiso 1 1 calc R . . H19B H 0.2853 0.0754 0.6819 0.173 Uiso 1 1 calc R . . H19C H 0.2245 -0.0324 0.6508 0.173 Uiso 1 1 calc R . . N5 N 0.2808(2) 0.2950(3) 0.8398(2) 0.0750(11) Uani 1 1 d . . . N6 N 0.2015(2) 0.3151(3) 0.7948(2) 0.0737(11) Uani 1 1 d . . . C20 C 0.2866(3) 0.2019(4) 0.8865(2) 0.0599(11) Uani 1 1 d . . . C21 C 0.2101(3) 0.1639(4) 0.8712(3) 0.0666(14) Uani 1 1 d . . . C22 C 0.1586(2) 0.2354(4) 0.8133(2) 0.0597(11) Uani 1 1 d . . . C23 C 0.3670(3) 0.1561(4) 0.9412(3) 0.0746(13) Uani 1 1 d . . . C24 C 0.3543(3) 0.0620(5) 0.9917(3) 0.120(2) Uani 1 1 d . . . H24A H 0.4049 0.0268 1.0229 0.144 Uiso 1 1 calc R . . H24B H 0.3193 -0.0008 0.9622 0.144 Uiso 1 1 calc R . . H24C H 0.3307 0.1000 1.0222 0.144 Uiso 1 1 calc R . . C25 C 0.4109(3) 0.0999(5) 0.8976(3) 0.113(2) Uani 1 1 d . . . H25A H 0.4177 0.1599 0.8650 0.136 Uiso 1 1 calc R . . H25B H 0.3804 0.0327 0.8688 0.136 Uiso 1 1 calc R . . H25C H 0.4624 0.0715 0.9315 0.136 Uiso 1 1 calc R . . C26 C 0.4167(3) 0.2624(5) 0.9855(3) 0.122(2) Uani 1 1 d . . . H26A H 0.4287 0.3163 0.9527 0.146 Uiso 1 1 calc R . . H26B H 0.4657 0.2323 1.0230 0.146 Uiso 1 1 calc R . . H26C H 0.3871 0.3057 1.0088 0.146 Uiso 1 1 calc R . . C27 C 0.0697(3) 0.2350(4) 0.7758(3) 0.0755(14) Uani 1 1 d . . . C28 C 0.0407(3) 0.3079(5) 0.7044(3) 0.1016(18) Uani 1 1 d . . . H28A H 0.0577 0.3910 0.7154 0.122 Uiso 1 1 calc R . . H28B H -0.0167 0.3049 0.6812 0.122 Uiso 1 1 calc R . . H28C H 0.0626 0.2742 0.6713 0.122 Uiso 1 1 calc R . . C29 C 0.0352(3) 0.2967(6) 0.8272(3) 0.129(2) Uani 1 1 d . . . H29A H 0.0482 0.2489 0.8715 0.155 Uiso 1 1 calc R . . H29B H -0.0219 0.3031 0.8018 0.155 Uiso 1 1 calc R . . H29C H 0.0579 0.3766 0.8403 0.155 Uiso 1 1 calc R . . C30 C 0.0398(3) 0.1069(5) 0.7617(5) 0.190(4) Uani 1 1 d . . . H30A H 0.0581 0.0692 0.7270 0.229 Uiso 1 1 calc R . . H30B H -0.0176 0.1068 0.7413 0.229 Uiso 1 1 calc R . . H30C H 0.0598 0.0622 0.8076 0.229 Uiso 1 1 calc R . . H10 H 0.128(2) 0.346(3) 0.510(2) 0.054(13) Uiso 1 1 d . . . H21 H 0.196(3) 0.109(4) 0.896(2) 0.082(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0579(3) 0.0578(2) 0.0559(3) 0.0057(2) 0.00540(17) -0.0160(2) N1 0.051(2) 0.077(2) 0.062(2) -0.0013(19) 0.0120(18) -0.0166(18) C1 0.072(4) 0.076(3) 0.105(4) -0.004(3) 0.043(3) -0.004(3) C2 0.113(6) 0.216(9) 0.471(17) -0.200(10) 0.151(9) -0.097(6) C3 0.090(6) 0.273(11) 0.331(13) 0.155(10) 0.087(7) 0.032(6) C4 0.156(8) 0.363(14) 0.151(8) 0.009(8) 0.097(7) -0.039(8) N2 0.074(3) 0.063(2) 0.059(2) -0.0002(18) 0.0180(19) -0.0158(18) C5 0.073(4) 0.097(4) 0.065(3) -0.019(3) 0.020(3) 0.002(3) C6 0.150(6) 0.176(7) 0.104(5) -0.069(5) 0.004(5) 0.009(5) C7 0.107(6) 0.347(14) 0.220(10) -0.123(9) 0.046(6) 0.055(7) C8 0.526(18) 0.077(5) 0.186(8) -0.053(5) 0.214(10) -0.077(8) N3 0.081(3) 0.051(2) 0.064(2) -0.0002(18) 0.005(2) -0.0121(18) N4 0.076(3) 0.048(2) 0.068(3) 0.0030(18) 0.001(2) -0.0092(17) C9 0.060(3) 0.058(3) 0.047(3) 0.001(2) 0.014(2) 0.001(2) C10 0.069(3) 0.069(3) 0.046(3) -0.004(3) 0.002(3) -0.001(3) C11 0.065(3) 0.054(3) 0.057(3) -0.003(2) 0.016(2) -0.005(2) C12 0.090(4) 0.065(3) 0.050(3) 0.004(2) 0.024(2) 0.015(3) C13 0.121(5) 0.064(3) 0.125(5) 0.007(3) 0.058(4) -0.001(3) C14 0.121(5) 0.094(4) 0.117(5) 0.008(4) 0.055(4) 0.036(4) C15 0.185(7) 0.093(4) 0.072(4) 0.016(3) 0.024(4) 0.040(4) C16 0.089(4) 0.052(3) 0.085(4) -0.010(3) 0.029(3) -0.013(2) C17 0.181(7) 0.074(4) 0.181(7) -0.023(4) 0.098(6) -0.002(4) C18 0.133(6) 0.090(4) 0.158(6) -0.036(4) 0.049(5) -0.047(4) C19 0.218(8) 0.067(4) 0.104(5) 0.013(3) 0.017(5) -0.006(4) N5 0.047(2) 0.080(3) 0.078(3) 0.023(2) 0.0032(19) -0.0139(18) N6 0.045(2) 0.078(3) 0.078(3) 0.028(2) 0.003(2) -0.0105(18) C20 0.056(3) 0.063(3) 0.052(3) 0.007(2) 0.012(2) 0.000(2) C21 0.052(3) 0.069(3) 0.073(3) 0.026(3) 0.019(3) -0.002(2) C22 0.049(3) 0.064(3) 0.060(3) 0.009(2) 0.015(2) -0.007(2) C23 0.056(3) 0.087(3) 0.075(3) 0.016(3) 0.019(3) 0.012(3) C24 0.075(4) 0.159(6) 0.109(5) 0.074(4) 0.017(3) 0.027(3) C25 0.092(4) 0.112(5) 0.137(5) 0.024(4) 0.046(4) 0.036(3) C26 0.080(4) 0.146(5) 0.089(4) -0.015(4) -0.020(3) 0.007(4) C27 0.046(3) 0.091(4) 0.076(3) 0.025(3) 0.009(3) -0.008(2) C28 0.064(3) 0.149(5) 0.069(4) 0.021(3) 0.002(3) 0.010(3) C29 0.069(4) 0.220(8) 0.097(5) 0.035(5) 0.033(4) 0.011(4) C30 0.071(4) 0.119(5) 0.279(10) 0.061(6) -0.038(5) -0.043(4) _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 N2 1.721(4) . ? Mo1 N1 1.728(3) . ? Mo1 N5 2.047(4) . ? Mo1 N3 2.056(4) . ? Mo1 N4 2.308(4) . ? Mo1 N6 2.331(4) . ? N1 C1 1.455(6) . ? C1 C2 1.454(7) . ? C1 C3 1.462(8) . ? C1 C4 1.470(8) . ? N2 C5 1.448(6) . ? C5 C6 1.471(7) . ? C5 C7 1.479(8) . ? C5 C8 1.477(8) . ? N3 C9 1.341(5) . ? N3 N4 1.378(4) . ? N4 C11 1.315(5) . ? C9 C10 1.370(6) . ? C9 C12 1.511(5) . ? C10 C11 1.384(6) . ? C11 C16 1.518(6) . ? C12 C14 1.505(6) . ? C12 C15 1.522(6) . ? C12 C13 1.527(6) . ? C16 C18 1.511(7) . ? C16 C17 1.509(7) . ? C16 C19 1.516(7) . ? N5 C20 1.348(5) . ? N5 N6 1.378(4) . ? N6 C22 1.317(5) . ? C20 C21 1.369(6) . ? C20 C23 1.514(5) . ? C21 C22 1.390(6) . ? C22 C27 1.488(5) . ? C23 C24 1.511(6) . ? C23 C26 1.519(6) . ? C23 C25 1.513(6) . ? C27 C30 1.494(7) . ? C27 C28 1.512(6) . ? C27 C29 1.539(7) . ? 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 N2 Mo1 N1 108.66(16) . . ? N2 Mo1 N5 101.98(17) . . ? N1 Mo1 N5 107.44(15) . . ? N2 Mo1 N3 107.45(15) . . ? N1 Mo1 N3 103.20(16) . . ? N5 Mo1 N3 127.29(13) . . ? N2 Mo1 N4 140.87(14) . . ? N1 Mo1 N4 97.17(15) . . ? N5 Mo1 N4 97.48(13) . . ? N3 Mo1 N4 36.24(11) . . ? N2 Mo1 N6 95.14(15) . . ? N1 Mo1 N6 141.27(14) . . ? N5 Mo1 N6 35.95(11) . . ? N3 Mo1 N6 97.93(13) . . ? N4 Mo1 N6 81.23(13) . . ? C1 N1 Mo1 160.2(3) . . ? C2 C1 N1 110.8(5) . . ? C2 C1 C3 111.7(7) . . ? N1 C1 C3 110.2(5) . . ? C2 C1 C4 109.1(7) . . ? N1 C1 C4 107.1(5) . . ? C3 C1 C4 107.7(7) . . ? C5 N2 Mo1 172.1(3) . . ? N2 C5 C6 108.9(4) . . ? N2 C5 C7 108.2(5) . . ? C6 C5 C7 108.5(6) . . ? N2 C5 C8 110.2(4) . . ? C6 C5 C8 108.8(6) . . ? C7 C5 C8 112.2(7) . . ? C9 N3 N4 110.0(3) . . ? C9 N3 Mo1 161.6(3) . . ? N4 N3 Mo1 81.9(2) . . ? C11 N4 N3 107.3(3) . . ? C11 N4 Mo1 163.2(3) . . ? N3 N4 Mo1 61.90(19) . . ? N3 C9 C10 106.1(4) . . ? N3 C9 C12 121.2(4) . . ? C10 C9 C12 132.7(4) . . ? C9 C10 C11 108.0(4) . . ? N4 C11 C10 108.6(4) . . ? N4 C11 C16 121.0(4) . . ? C10 C11 C16 130.4(4) . . ? C14 C12 C9 109.0(4) . . ? C14 C12 C15 110.6(4) . . ? C9 C12 C15 109.4(4) . . ? C14 C12 C13 108.9(4) . . ? C9 C12 C13 109.9(4) . . ? C15 C12 C13 109.0(4) . . ? C18 C16 C17 108.1(5) . . ? C18 C16 C19 110.6(5) . . ? C17 C16 C19 109.5(5) . . ? C18 C16 C11 109.7(4) . . ? C17 C16 C11 108.6(4) . . ? C19 C16 C11 110.3(4) . . ? C20 N5 N6 109.5(3) . . ? C20 N5 Mo1 164.6(3) . . ? N6 N5 Mo1 83.3(2) . . ? C22 N6 N5 107.7(3) . . ? C22 N6 Mo1 165.9(3) . . ? N5 N6 Mo1 60.7(2) . . ? N5 C20 C21 106.5(4) . . ? N5 C20 C23 121.6(4) . . ? C21 C20 C23 131.9(4) . . ? C20 C21 C22 107.7(4) . . ? N6 C22 C21 108.5(4) . . ? N6 C22 C27 120.9(4) . . ? C21 C22 C27 130.5(4) . . ? C24 C23 C20 109.4(4) . . ? C24 C23 C26 111.2(5) . . ? C20 C23 C26 109.7(4) . . ? C24 C23 C25 110.1(4) . . ? C20 C23 C25 108.5(4) . . ? C26 C23 C25 107.9(5) . . ? C30 C27 C22 109.8(4) . . ? C30 C27 C28 111.1(5) . . ? C22 C27 C28 111.5(4) . . ? C30 C27 C29 108.8(6) . . ? C22 C27 C29 108.8(4) . . ? C28 C27 C29 106.8(4) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.437 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.054 # Attachment 'Elss (3b).txt' data_elss_(3b) _database_code_depnum_ccdc_archive 'CCDC 287645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 N6 W' _chemical_formula_weight 684.66 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.253(5) _cell_length_b 11.006(3) _cell_length_c 19.533(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.752(7) _cell_angle_gamma 90.00 _cell_volume 3591.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description chunks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 3.241 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3572 _exptl_absorpt_correction_T_max 0.5634 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25563 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8469 _reflns_number_gt 5882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^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 0.00026(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8469 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.201371(8) 0.583062(13) 0.228839(7) 0.06161(7) Uani 1 1 d . . . N1 N 0.2612(2) 0.5744(3) 0.34225(16) 0.0743(9) Uani 1 1 d . . . N2 N 0.25500(18) 0.6987(3) 0.33673(16) 0.0750(9) Uani 1 1 d . . . C1 C 0.3133(2) 0.5422(3) 0.41099(18) 0.0600(8) Uani 1 1 d . . . C2 C 0.3405(2) 0.6483(3) 0.44958(18) 0.0692(9) Uani 1 1 d . . . H2 H 0.3771 0.6552 0.4990 0.083 Uiso 1 1 calc R . . C3 C 0.3033(2) 0.7437(3) 0.40154(19) 0.0644(9) Uani 1 1 d . . . C4 C 0.3334(3) 0.4108(3) 0.4317(2) 0.0740(11) Uani 1 1 d . . . C5 C 0.3824(3) 0.3607(5) 0.3917(3) 0.1054(15) Uani 1 1 d . . . H5A H 0.3529 0.3689 0.3386 0.126 Uiso 1 1 calc R . . H5B H 0.3936 0.2764 0.4041 0.126 Uiso 1 1 calc R . . H5C H 0.4317 0.4050 0.4068 0.126 Uiso 1 1 calc R . . C6 C 0.2553(3) 0.3379(4) 0.4078(3) 0.1008(14) Uani 1 1 d . . . H6A H 0.2236 0.3693 0.4327 0.121 Uiso 1 1 calc R . . H6B H 0.2676 0.2540 0.4209 0.121 Uiso 1 1 calc R . . H6C H 0.2260 0.3447 0.3546 0.121 Uiso 1 1 calc R . . C7 C 0.3795(4) 0.3994(4) 0.5153(2) 0.125(2) Uani 1 1 d . . . H7A H 0.4281 0.4456 0.5305 0.150 Uiso 1 1 calc R . . H7B H 0.3922 0.3155 0.5282 0.150 Uiso 1 1 calc R . . H7C H 0.3475 0.4297 0.5404 0.150 Uiso 1 1 calc R . . C8 C 0.3099(3) 0.8793(4) 0.4150(2) 0.0780(11) Uani 1 1 d . . . C9 C 0.3983(3) 0.9162(4) 0.4513(4) 0.127(2) Uani 1 1 d . . . H9A H 0.4255 0.8671 0.4949 0.152 Uiso 1 1 calc R . . H9B H 0.4023 1.0002 0.4655 0.152 Uiso 1 1 calc R . . H9C H 0.4223 0.9042 0.4162 0.152 Uiso 1 1 calc R . . C10 C 0.2693(4) 0.9141(4) 0.4656(4) 0.134(2) Uani 1 1 d . . . H10A H 0.2924 0.8691 0.5115 0.160 Uiso 1 1 calc R . . H10B H 0.2132 0.8961 0.4414 0.160 Uiso 1 1 calc R . . H10C H 0.2764 0.9995 0.4763 0.160 Uiso 1 1 calc R . . C11 C 0.2682(4) 0.9477(4) 0.3417(3) 0.142(3) Uani 1 1 d . . . H11A H 0.2694 1.0333 0.3516 0.170 Uiso 1 1 calc R . . H11B H 0.2136 0.9210 0.3179 0.170 Uiso 1 1 calc R . . H11C H 0.2952 0.9319 0.3094 0.170 Uiso 1 1 calc R . . N3 N 0.22035(16) 0.7064(3) 0.15946(16) 0.0749(9) Uani 1 1 d . . . N4 N 0.30009(16) 0.6864(3) 0.20524(16) 0.0744(9) Uani 1 1 d . . . C12 C 0.21357(19) 0.7990(3) 0.11418(18) 0.0598(8) Uani 1 1 d . . . C13 C 0.2903(2) 0.8398(3) 0.1297(2) 0.0698(10) Uani 1 1 d . . . H13 H 0.3047 0.9032 0.1061 0.084 Uiso 1 1 calc R . . C14 C 0.34180(18) 0.7671(3) 0.18743(18) 0.0620(8) Uani 1 1 d . . . C15 C 0.1333(2) 0.8451(4) 0.0595(2) 0.0759(11) Uani 1 1 d . . . C16 C 0.0909(3) 0.9024(4) 0.1029(3) 0.1098(17) Uani 1 1 d . . . H16A H 0.0861 0.8444 0.1376 0.132 Uiso 1 1 calc R . . H16B H 0.0385 0.9281 0.0691 0.132 Uiso 1 1 calc R . . H16C H 0.1208 0.9715 0.1299 0.132 Uiso 1 1 calc R . . C17 C 0.0848(3) 0.7403(5) 0.0144(2) 0.1119(17) Uani 1 1 d . . . H17A H 0.0850 0.6756 0.0475 0.134 Uiso 1 1 calc R . . H17B H 0.1077 0.7119 -0.0191 0.134 Uiso 1 1 calc R . . H17C H 0.0308 0.7664 -0.0139 0.134 Uiso 1 1 calc R . . C18 C 0.1469(3) 0.9407(5) 0.0092(3) 0.121(2) Uani 1 1 d . . . H18A H 0.0972 0.9803 -0.0199 0.145 Uiso 1 1 calc R . . H18B H 0.1673 0.9022 -0.0237 0.145 Uiso 1 1 calc R . . H18C H 0.1849 0.9997 0.0395 0.145 Uiso 1 1 calc R . . C19 C 0.4320(2) 0.7694(4) 0.2264(2) 0.0764(11) Uani 1 1 d . . . C20 C 0.4608(2) 0.6965(5) 0.2973(2) 0.1010(15) Uani 1 1 d . . . H20A H 0.4395 0.7303 0.3308 0.121 Uiso 1 1 calc R . . H20B H 0.5182 0.6987 0.3205 0.121 Uiso 1 1 calc R . . H20C H 0.4432 0.6139 0.2860 0.121 Uiso 1 1 calc R . . C21 C 0.4658(3) 0.7103(6) 0.1745(3) 0.128(2) Uani 1 1 d . . . H21A H 0.4404 0.6332 0.1577 0.154 Uiso 1 1 calc R . . H21B H 0.5224 0.6986 0.2011 0.154 Uiso 1 1 calc R . . H21C H 0.4559 0.7621 0.1321 0.154 Uiso 1 1 calc R . . C22 C 0.4604(3) 0.8973(5) 0.2402(4) 0.171(3) Uani 1 1 d . . . H22A H 0.4339 0.9443 0.1956 0.205 Uiso 1 1 calc R . . H22B H 0.5171 0.8995 0.2541 0.205 Uiso 1 1 calc R . . H22C H 0.4484 0.9307 0.2800 0.205 Uiso 1 1 calc R . . N5 N 0.10115(18) 0.5954(3) 0.21557(17) 0.0717(8) Uani 1 1 d . . . C23 C 0.0195(2) 0.5679(4) 0.2019(3) 0.0848(12) Uani 1 1 d . . . C24 C -0.0045(4) 0.4557(8) 0.1601(7) 0.279(7) Uani 1 1 d . . . H24A H -0.0074 0.4678 0.1104 0.334 Uiso 1 1 calc R . . H24B H -0.0560 0.4313 0.1576 0.334 Uiso 1 1 calc R . . H24C H 0.0341 0.3935 0.1845 0.334 Uiso 1 1 calc R . . C25 C 0.0130(6) 0.5552(10) 0.2735(4) 0.232(5) Uani 1 1 d . . . H25A H 0.0531 0.4995 0.3047 0.278 Uiso 1 1 calc R . . H25B H -0.0391 0.5246 0.2654 0.278 Uiso 1 1 calc R . . H25C H 0.0208 0.6329 0.2977 0.278 Uiso 1 1 calc R . . C26 C -0.0335(4) 0.6647(8) 0.1590(5) 0.219(4) Uani 1 1 d . . . H26A H -0.0282 0.7335 0.1908 0.263 Uiso 1 1 calc R . . H26B H -0.0878 0.6365 0.1393 0.263 Uiso 1 1 calc R . . H26C H -0.0193 0.6879 0.1185 0.263 Uiso 1 1 calc R . . N6 N 0.21497(19) 0.4444(3) 0.19279(16) 0.0703(8) Uani 1 1 d . . . C27 C 0.2122(2) 0.3327(4) 0.1534(2) 0.0792(11) Uani 1 1 d . . . C28 C 0.1554(4) 0.3474(7) 0.0744(3) 0.157(3) Uani 1 1 d . . . H28A H 0.1642 0.4245 0.0560 0.189 Uiso 1 1 calc R . . H28B H 0.1015 0.3438 0.0712 0.189 Uiso 1 1 calc R . . H28C H 0.1635 0.2834 0.0449 0.189 Uiso 1 1 calc R . . C29 C 0.1867(6) 0.2325(5) 0.1880(5) 0.235(5) Uani 1 1 d . . . H29A H 0.1920 0.1571 0.1658 0.282 Uiso 1 1 calc R . . H29B H 0.1318 0.2441 0.1803 0.282 Uiso 1 1 calc R . . H29C H 0.2196 0.2306 0.2407 0.282 Uiso 1 1 calc R . . C30 C 0.2924(4) 0.3058(9) 0.1560(5) 0.245(5) Uani 1 1 d . . . H30A H 0.3128 0.3762 0.1404 0.294 Uiso 1 1 calc R . . H30B H 0.2890 0.2392 0.1232 0.294 Uiso 1 1 calc R . . H30C H 0.3277 0.2846 0.2062 0.294 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05581(10) 0.05462(9) 0.05689(9) 0.00554(6) 0.00449(6) -0.01478(6) N1 0.085(2) 0.0527(18) 0.0604(17) -0.0049(13) 0.0028(15) -0.0104(14) N2 0.080(2) 0.0496(17) 0.0704(18) 0.0017(14) 0.0046(15) -0.0052(14) C1 0.067(2) 0.0561(19) 0.0525(18) 0.0020(15) 0.0198(16) 0.0004(16) C2 0.077(2) 0.063(2) 0.0530(18) -0.0066(16) 0.0108(17) 0.0003(18) C3 0.066(2) 0.057(2) 0.064(2) -0.0074(17) 0.0188(16) -0.0080(17) C4 0.099(3) 0.060(2) 0.0554(19) 0.0027(16) 0.024(2) 0.0118(19) C5 0.118(4) 0.095(3) 0.113(4) 0.008(3) 0.057(3) 0.030(3) C6 0.126(4) 0.057(3) 0.122(4) 0.005(2) 0.053(3) -0.006(3) C7 0.194(6) 0.079(3) 0.067(3) 0.018(2) 0.015(3) 0.031(3) C8 0.090(3) 0.052(2) 0.082(3) -0.0079(19) 0.025(2) -0.0090(19) C9 0.113(4) 0.081(3) 0.167(5) -0.033(3) 0.035(4) -0.039(3) C10 0.171(6) 0.078(4) 0.167(6) -0.023(3) 0.085(5) 0.000(3) C11 0.222(7) 0.062(3) 0.106(4) 0.004(3) 0.029(4) -0.005(4) N3 0.0482(15) 0.079(2) 0.0772(19) 0.0261(16) 0.0041(14) -0.0107(14) N4 0.0496(16) 0.074(2) 0.0787(19) 0.0278(16) 0.0040(14) -0.0119(14) C12 0.0518(18) 0.063(2) 0.0562(18) 0.0073(15) 0.0127(14) 0.0009(15) C13 0.057(2) 0.068(2) 0.077(2) 0.0227(19) 0.0194(17) -0.0054(17) C14 0.0485(17) 0.067(2) 0.0617(19) 0.0105(16) 0.0133(14) -0.0033(15) C15 0.058(2) 0.079(3) 0.079(2) 0.018(2) 0.0159(18) 0.0112(19) C16 0.079(3) 0.114(4) 0.135(4) 0.020(3) 0.042(3) 0.033(3) C17 0.072(3) 0.135(4) 0.090(3) -0.010(3) -0.008(2) 0.002(3) C18 0.084(3) 0.148(5) 0.110(4) 0.074(3) 0.017(3) 0.029(3) C19 0.0468(18) 0.088(3) 0.081(2) 0.018(2) 0.0124(17) -0.0117(18) C20 0.063(2) 0.147(4) 0.074(3) 0.026(3) 0.008(2) 0.012(3) C21 0.072(3) 0.220(7) 0.090(3) 0.038(4) 0.030(3) 0.014(3) C22 0.077(3) 0.114(5) 0.243(8) 0.042(4) -0.017(4) -0.041(3) N5 0.0664(19) 0.071(2) 0.0688(18) -0.0019(14) 0.0178(15) -0.0154(14) C23 0.058(2) 0.091(3) 0.106(3) -0.003(2) 0.034(2) -0.004(2) C24 0.114(6) 0.237(9) 0.517(19) -0.222(11) 0.161(9) -0.111(6) C25 0.176(8) 0.389(16) 0.163(8) 0.011(8) 0.102(7) -0.046(8) C26 0.086(4) 0.238(10) 0.313(11) 0.117(9) 0.060(6) 0.019(5) N6 0.074(2) 0.070(2) 0.0569(16) 0.0011(14) 0.0157(14) -0.0164(15) C27 0.077(3) 0.083(3) 0.070(2) -0.016(2) 0.023(2) 0.001(2) C28 0.142(5) 0.167(6) 0.109(4) -0.054(4) -0.006(4) 0.012(5) C29 0.485(16) 0.088(5) 0.209(7) -0.065(5) 0.220(9) -0.099(7) C30 0.117(6) 0.345(13) 0.232(9) -0.137(9) 0.029(5) 0.070(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 W1 N6 1.740(3) . ? W1 N5 1.746(3) . ? W1 N1 2.040(3) . ? W1 N3 2.044(3) . ? W1 N2 2.315(3) . ? W1 N4 2.329(3) . ? N1 C1 1.344(4) . ? N1 N2 1.373(4) . ? N2 C3 1.314(4) . ? C1 C2 1.369(5) . ? C1 C4 1.507(5) . ? C2 C3 1.389(5) . ? C3 C8 1.512(5) . ? C4 C5 1.509(6) . ? C4 C7 1.511(5) . ? C4 C6 1.535(6) . ? C8 C10 1.504(7) . ? C8 C11 1.523(6) . ? C8 C9 1.532(6) . ? N3 C12 1.323(4) . ? N3 N4 1.385(4) . ? N4 C14 1.304(4) . ? C12 C13 1.383(5) . ? C12 C15 1.511(5) . ? C13 C14 1.393(4) . ? C14 C19 1.510(4) . ? C15 C16 1.500(6) . ? C15 C17 1.504(6) . ? C15 C18 1.526(6) . ? C19 C22 1.487(6) . ? C19 C20 1.501(5) . ? C19 C21 1.529(6) . ? N5 C23 1.437(5) . ? C23 C24 1.447(7) . ? C23 C25 1.457(8) . ? C23 C26 1.456(8) . ? N6 C27 1.440(5) . ? C27 C29 1.464(7) . ? C27 C30 1.475(7) . ? C27 C28 1.480(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 N6 W1 N5 108.66(14) . . ? N6 W1 N1 107.32(13) . . ? N5 W1 N1 103.60(15) . . ? N6 W1 N3 102.95(14) . . ? N5 W1 N3 107.28(12) . . ? N1 W1 N3 126.28(11) . . ? N6 W1 N2 140.71(12) . . ? N5 W1 N2 97.23(13) . . ? N1 W1 N2 36.07(10) . . ? N3 W1 N2 96.67(12) . . ? N6 W1 N4 95.76(14) . . ? N5 W1 N4 141.29(12) . . ? N1 W1 N4 96.87(12) . . ? N3 W1 N4 36.19(9) . . ? N2 W1 N4 80.47(12) . . ? C1 N1 N2 110.1(3) . . ? C1 N1 W1 162.1(3) . . ? N2 N1 W1 82.95(19) . . ? C3 N2 N1 107.3(3) . . ? C3 N2 W1 163.4(3) . . ? N1 N2 W1 60.98(16) . . ? N1 C1 C2 106.2(3) . . ? N1 C1 C4 121.3(3) . . ? C2 C1 C4 132.5(3) . . ? C1 C2 C3 107.6(3) . . ? N2 C3 C2 108.8(3) . . ? N2 C3 C8 121.0(3) . . ? C2 C3 C8 130.2(3) . . ? C5 C4 C7 110.0(4) . . ? C5 C4 C1 110.0(4) . . ? C7 C4 C1 109.8(3) . . ? C5 C4 C6 108.8(4) . . ? C7 C4 C6 109.3(4) . . ? C1 C4 C6 108.9(3) . . ? C3 C8 C10 109.9(4) . . ? C3 C8 C11 110.4(4) . . ? C10 C8 C11 107.4(5) . . ? C3 C8 C9 109.7(4) . . ? C10 C8 C9 109.5(5) . . ? C11 C8 C9 109.8(5) . . ? C12 N3 N4 110.2(3) . . ? C12 N3 W1 163.8(3) . . ? N4 N3 W1 83.19(17) . . ? C14 N4 N3 107.1(3) . . ? C14 N4 W1 165.1(3) . . ? N3 N4 W1 60.61(16) . . ? N3 C12 C13 106.8(3) . . ? N3 C12 C15 122.3(3) . . ? C13 C12 C15 130.8(3) . . ? C12 C13 C14 106.5(3) . . ? N4 C14 C13 109.3(3) . . ? N4 C14 C19 120.8(3) . . ? C13 C14 C19 129.8(3) . . ? C16 C15 C12 108.4(4) . . ? C16 C15 C17 109.7(4) . . ? C12 C15 C17 109.3(3) . . ? C16 C15 C18 109.2(4) . . ? C12 C15 C18 108.9(3) . . ? C17 C15 C18 111.2(4) . . ? C22 C19 C20 111.8(4) . . ? C22 C19 C14 109.7(4) . . ? C20 C19 C14 111.2(3) . . ? C22 C19 C21 108.6(5) . . ? C20 C19 C21 107.4(4) . . ? C14 C19 C21 108.0(3) . . ? C23 N5 W1 163.2(3) . . ? N5 C23 C24 109.8(4) . . ? N5 C23 C25 108.7(5) . . ? C24 C23 C25 109.7(7) . . ? N5 C23 C26 110.5(4) . . ? C24 C23 C26 108.6(7) . . ? C25 C23 C26 109.4(7) . . ? C27 N6 W1 170.0(3) . . ? N6 C27 C29 110.2(4) . . ? N6 C27 C30 109.3(4) . . ? C29 C27 C30 109.2(7) . . ? N6 C27 C28 108.8(4) . . ? C29 C27 C28 110.1(5) . . ? C30 C27 C28 109.1(5) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.703 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.058 # Attachment 'Revised Emon1 (4a).cif' data_emon _database_code_depnum_ccdc_archive 'CCDC 287646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H50 Cl2 Mo2 N8' _chemical_formula_weight 737.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.276(2) _cell_length_b 10.7343(14) _cell_length_c 17.974(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.598(2) _cell_angle_gamma 90.00 _cell_volume 3486.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 22.5 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8405 _exptl_absorpt_correction_T_max 0.9154 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50139 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_av_sigmaI/netI 0.1721 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.27 _reflns_number_total 8259 _reflns_number_gt 3704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1242P)^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 0.0081(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8259 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1791 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2393 _refine_ls_wR_factor_gt 0.2038 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.008 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.32749(5) 0.60530(8) 0.27073(4) 0.0347(3) Uani 1 1 d . . . Mo2 Mo 0.19223(5) 0.35222(8) 0.19908(5) 0.0366(3) Uani 1 1 d . . . Cl1 Cl 0.27788(16) 0.7743(2) 0.19140(15) 0.0561(7) Uani 1 1 d . . . Cl2 Cl 0.13848(17) 0.3014(3) 0.30929(16) 0.0707(9) Uani 1 1 d . . . N1 N 0.4165(5) 0.6638(7) 0.2907(4) 0.045(2) Uani 1 1 d . . . C1 C 0.4727(6) 0.7550(11) 0.3251(6) 0.057(3) Uani 1 1 d . . . C2 C 0.4561(8) 0.8003(13) 0.4007(6) 0.086(5) Uani 1 1 d . . . H2A H 0.4069 0.8341 0.3949 0.103 Uiso 1 1 calc R . . H2B H 0.4911 0.8637 0.4196 0.103 Uiso 1 1 calc R . . H2C H 0.4598 0.7319 0.4354 0.103 Uiso 1 1 calc R . . C3 C 0.4685(8) 0.8625(11) 0.2711(7) 0.078(4) Uani 1 1 d . . . H3A H 0.4788 0.8336 0.2232 0.093 Uiso 1 1 calc R . . H3B H 0.5042 0.9245 0.2904 0.093 Uiso 1 1 calc R . . H3C H 0.4198 0.8981 0.2653 0.093 Uiso 1 1 calc R . . C4 C 0.5494(6) 0.6947(11) 0.3290(7) 0.070(4) Uani 1 1 d . . . H4A H 0.5547 0.6299 0.3662 0.084 Uiso 1 1 calc R . . H4B H 0.5870 0.7566 0.3423 0.084 Uiso 1 1 calc R . . H4C H 0.5544 0.6599 0.2808 0.084 Uiso 1 1 calc R . . N2 N 0.2790(5) 0.6443(8) 0.3441(5) 0.050(2) Uani 1 1 d . . . C5 C 0.2411(7) 0.6785(10) 0.4057(6) 0.057(3) Uani 1 1 d . . . C6 C 0.1695(9) 0.6045(17) 0.4002(8) 0.122(7) Uani 1 1 d . . . H6A H 0.1442 0.6073 0.3494 0.147 Uiso 1 1 calc R . . H6B H 0.1386 0.6400 0.4333 0.147 Uiso 1 1 calc R . . H6C H 0.1806 0.5196 0.4143 0.147 Uiso 1 1 calc R . . C7 C 0.2897(10) 0.646(2) 0.4773(7) 0.155(9) Uani 1 1 d . . . H7A H 0.3004 0.5585 0.4780 0.186 Uiso 1 1 calc R . . H7B H 0.2650 0.6667 0.5191 0.186 Uiso 1 1 calc R . . H7C H 0.3351 0.6923 0.4807 0.186 Uiso 1 1 calc R . . C8 C 0.2278(13) 0.8132(16) 0.4004(11) 0.184(11) Uani 1 1 d . . . H8A H 0.2742 0.8562 0.4037 0.221 Uiso 1 1 calc R . . H8B H 0.2025 0.8394 0.4408 0.221 Uiso 1 1 calc R . . H8C H 0.1980 0.8322 0.3532 0.221 Uiso 1 1 calc R . . N3 N 0.3431(4) 0.4139(7) 0.3095(4) 0.0348(17) Uani 1 1 d . . . N4 N 0.2967(4) 0.3214(7) 0.2770(4) 0.0390(19) Uani 1 1 d . . . C9 C 0.3928(6) 0.3623(10) 0.3643(5) 0.048(3) Uani 1 1 d . . . C10 C 0.4478(7) 0.4350(11) 0.4119(7) 0.071(4) Uani 1 1 d . . . H10A H 0.4801 0.4744 0.3815 0.086 Uiso 1 1 calc R . . H10B H 0.4761 0.3814 0.4480 0.086 Uiso 1 1 calc R . . H10C H 0.4236 0.4975 0.4377 0.086 Uiso 1 1 calc R . . C11 C 0.3784(6) 0.2373(10) 0.3649(6) 0.052(3) Uani 1 1 d . . . H11 H 0.4042 0.1791 0.3970 0.063 Uiso 1 1 calc R . . C12 C 0.3194(6) 0.2123(10) 0.3105(6) 0.051(3) Uani 1 1 d . . . C13 C 0.2824(7) 0.0930(11) 0.2874(8) 0.077(4) Uani 1 1 d . . . H13A H 0.2305 0.0997 0.2906 0.092 Uiso 1 1 calc R . . H13B H 0.3038 0.0277 0.3201 0.092 Uiso 1 1 calc R . . H13C H 0.2887 0.0743 0.2365 0.092 Uiso 1 1 calc R . . N5 N 0.3223(4) 0.5054(7) 0.1592(4) 0.0347(18) Uani 1 1 d . . . N6 N 0.2748(4) 0.4091(7) 0.1329(4) 0.0382(19) Uani 1 1 d . . . C14 C 0.3630(5) 0.5358(9) 0.1041(5) 0.041(2) Uani 1 1 d . . . C15 C 0.4200(6) 0.6331(10) 0.1113(6) 0.054(3) Uani 1 1 d . . . H15A H 0.3973 0.7130 0.1151 0.065 Uiso 1 1 calc R . . H15B H 0.4449 0.6317 0.0680 0.065 Uiso 1 1 calc R . . H15C H 0.4552 0.6181 0.1557 0.065 Uiso 1 1 calc R . . C16 C 0.3422(6) 0.4551(10) 0.0441(6) 0.053(3) Uani 1 1 d . . . H16 H 0.3614 0.4528 -0.0010 0.063 Uiso 1 1 calc R . . C17 C 0.2880(6) 0.3799(10) 0.0639(5) 0.049(3) Uani 1 1 d . . . C18 C 0.2503(8) 0.2781(14) 0.0175(7) 0.100(6) Uani 1 1 d . . . H18A H 0.2451 0.2073 0.0489 0.120 Uiso 1 1 calc R . . H18B H 0.2791 0.2553 -0.0209 0.120 Uiso 1 1 calc R . . H18C H 0.2023 0.3058 -0.0055 0.120 Uiso 1 1 calc R . . N7 N 0.1421(5) 0.4875(8) 0.1799(5) 0.047(2) Uani 1 1 d . . . C19 C 0.0855(6) 0.5698(11) 0.1420(6) 0.056(3) Uani 1 1 d . . . C20 C 0.0801(7) 0.6848(12) 0.1901(7) 0.081(4) Uani 1 1 d . . . H20A H 0.0488 0.7453 0.1618 0.097 Uiso 1 1 calc R . . H20B H 0.1285 0.7194 0.2046 0.097 Uiso 1 1 calc R . . H20C H 0.0595 0.6622 0.2343 0.097 Uiso 1 1 calc R . . C21 C 0.1094(8) 0.6058(14) 0.0676(7) 0.095(5) Uani 1 1 d . . . H21A H 0.1135 0.5322 0.0381 0.114 Uiso 1 1 calc R . . H21B H 0.1565 0.6470 0.0768 0.114 Uiso 1 1 calc R . . H21C H 0.0734 0.6608 0.0407 0.114 Uiso 1 1 calc R . . C22 C 0.0137(8) 0.5067(13) 0.1287(8) 0.095(5) Uani 1 1 d . . . H22A H 0.0172 0.4342 0.0981 0.114 Uiso 1 1 calc R . . H22B H -0.0229 0.5624 0.1032 0.114 Uiso 1 1 calc R . . H22C H -0.0004 0.4822 0.1759 0.114 Uiso 1 1 calc R . . N8 N 0.1516(5) 0.2315(8) 0.1452(5) 0.054(2) Uani 1 1 d . . . C23 C 0.0999(7) 0.1346(11) 0.1103(7) 0.062(3) Uani 1 1 d . . . C24 C 0.1417(8) 0.0191(11) 0.0992(8) 0.093(5) Uani 1 1 d . . . H24A H 0.1791 0.0372 0.0686 0.111 Uiso 1 1 calc R . . H24B H 0.1084 -0.0426 0.0748 0.111 Uiso 1 1 calc R . . H24C H 0.1646 -0.0119 0.1472 0.111 Uiso 1 1 calc R . . C25 C 0.0635(9) 0.1800(15) 0.0325(9) 0.121(7) Uani 1 1 d . . . H25A H 0.0444 0.2626 0.0367 0.145 Uiso 1 1 calc R . . H25B H 0.0237 0.1250 0.0133 0.145 Uiso 1 1 calc R . . H25C H 0.0995 0.1807 -0.0013 0.145 Uiso 1 1 calc R . . C26 C 0.0450(10) 0.1137(18) 0.1615(11) 0.172(11) Uani 1 1 d . . . H26A H 0.0701 0.0884 0.2100 0.206 Uiso 1 1 calc R . . H26B H 0.0111 0.0497 0.1413 0.206 Uiso 1 1 calc R . . H26C H 0.0183 0.1895 0.1666 0.206 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0385(5) 0.0381(5) 0.0276(4) -0.0027(3) 0.0051(3) -0.0033(4) Mo2 0.0326(5) 0.0404(5) 0.0361(5) -0.0021(4) 0.0031(3) -0.0014(4) Cl1 0.0632(19) 0.0488(16) 0.0561(17) 0.0088(12) 0.0078(14) 0.0092(14) Cl2 0.060(2) 0.099(2) 0.0575(18) 0.0114(16) 0.0249(15) -0.0082(17) N1 0.052(5) 0.048(5) 0.034(4) -0.002(4) 0.008(4) -0.010(4) C1 0.047(7) 0.061(8) 0.062(7) -0.019(6) 0.003(6) -0.018(6) C2 0.097(11) 0.109(12) 0.055(8) -0.023(7) 0.022(7) -0.047(9) C3 0.087(10) 0.059(8) 0.088(10) -0.009(7) 0.012(8) -0.037(7) C4 0.053(8) 0.067(8) 0.090(9) -0.005(7) 0.016(7) -0.022(6) N2 0.061(6) 0.046(5) 0.043(5) -0.005(4) 0.010(4) 0.003(4) C5 0.068(8) 0.053(7) 0.057(7) -0.013(5) 0.028(6) -0.012(6) C6 0.108(13) 0.21(2) 0.063(9) -0.032(10) 0.057(9) -0.055(13) C7 0.137(17) 0.29(3) 0.033(8) -0.016(12) 0.010(9) -0.066(17) C8 0.30(3) 0.093(15) 0.19(2) -0.027(14) 0.17(2) 0.022(17) N3 0.031(4) 0.046(5) 0.027(4) 0.003(3) 0.003(3) -0.006(4) N4 0.034(5) 0.044(5) 0.039(4) 0.006(3) 0.006(4) -0.008(4) C9 0.062(7) 0.057(7) 0.023(5) 0.009(4) -0.003(5) 0.000(6) C10 0.071(9) 0.064(8) 0.068(8) 0.018(6) -0.024(7) -0.022(7) C11 0.044(7) 0.062(8) 0.051(6) 0.026(5) 0.006(5) 0.011(6) C12 0.046(7) 0.056(7) 0.053(7) 0.016(5) 0.010(5) -0.004(5) C13 0.061(8) 0.060(8) 0.103(11) 0.020(7) -0.008(8) -0.008(7) N5 0.043(5) 0.042(5) 0.021(4) -0.002(3) 0.010(3) -0.006(4) N6 0.039(5) 0.049(5) 0.025(4) -0.003(3) -0.001(3) 0.002(4) C14 0.038(6) 0.061(7) 0.023(5) 0.002(4) 0.005(4) -0.001(5) C15 0.063(8) 0.054(7) 0.048(6) 0.005(5) 0.015(6) -0.009(6) C16 0.053(7) 0.070(8) 0.036(6) -0.002(5) 0.012(5) -0.002(6) C17 0.054(7) 0.068(8) 0.026(5) -0.009(4) 0.011(5) -0.007(6) C18 0.109(12) 0.147(14) 0.053(8) -0.048(8) 0.041(8) -0.070(11) N7 0.040(5) 0.052(5) 0.050(5) 0.004(4) 0.010(4) 0.014(4) C19 0.044(7) 0.065(8) 0.058(7) 0.003(6) 0.003(6) 0.016(6) C20 0.075(10) 0.071(9) 0.098(10) 0.005(7) 0.015(8) 0.036(7) C21 0.080(11) 0.126(13) 0.074(10) 0.022(9) -0.004(8) 0.026(9) C22 0.076(11) 0.090(11) 0.108(12) -0.024(9) -0.024(9) 0.011(9) N8 0.051(6) 0.058(6) 0.059(6) -0.013(4) 0.025(5) -0.012(5) C23 0.049(7) 0.059(8) 0.075(8) -0.016(6) 0.005(6) -0.022(6) C24 0.107(12) 0.048(8) 0.123(13) -0.024(8) 0.017(10) -0.011(8) C25 0.130(16) 0.076(11) 0.132(15) 0.000(9) -0.061(13) -0.017(10) C26 0.124(16) 0.21(2) 0.20(2) -0.150(18) 0.093(15) -0.113(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.730(8) . ? Mo1 N2 1.747(8) . ? Mo1 N3 2.174(7) . ? Mo1 N5 2.263(7) . ? Mo1 Cl1 2.400(3) . ? Mo2 N8 1.718(8) . ? Mo2 N7 1.724(8) . ? Mo2 N6 2.146(8) . ? Mo2 N4 2.217(8) . ? Mo2 Cl2 2.402(3) . ? N1 C1 1.485(12) . ? C1 C3 1.502(16) . ? C1 C2 1.516(15) . ? C1 C4 1.536(16) . ? N2 C5 1.438(13) . ? C5 C8 1.467(19) . ? C5 C7 1.491(18) . ? C5 C6 1.521(17) . ? N3 C9 1.355(12) . ? N3 N4 1.378(10) . ? N4 C12 1.354(12) . ? C9 C11 1.367(14) . ? C9 C10 1.447(14) . ? C11 C12 1.369(14) . ? C12 C13 1.479(16) . ? N5 C14 1.365(11) . ? N5 N6 1.386(10) . ? N6 C17 1.336(11) . ? C14 C16 1.392(13) . ? C14 C15 1.466(13) . ? C16 C17 1.364(14) . ? C17 C18 1.480(14) . ? N7 C19 1.449(13) . ? C19 C22 1.465(16) . ? C19 C21 1.519(17) . ? C19 C20 1.518(16) . ? N8 C23 1.480(13) . ? C23 C26 1.476(19) . ? C23 C24 1.486(16) . ? C23 C25 1.536(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 N2 108.9(4) . . ? N1 Mo1 N3 101.7(3) . . ? N2 Mo1 N3 92.4(3) . . ? N1 Mo1 N5 105.7(3) . . ? N2 Mo1 N5 145.4(3) . . ? N3 Mo1 N5 79.8(3) . . ? N1 Mo1 Cl1 96.3(3) . . ? N2 Mo1 Cl1 94.5(3) . . ? N3 Mo1 Cl1 157.6(2) . . ? N5 Mo1 Cl1 82.5(2) . . ? N8 Mo2 N7 110.5(4) . . ? N8 Mo2 N6 100.5(3) . . ? N7 Mo2 N6 92.7(3) . . ? N8 Mo2 N4 120.1(4) . . ? N7 Mo2 N4 129.3(4) . . ? N6 Mo2 N4 77.4(3) . . ? N8 Mo2 Cl2 95.6(3) . . ? N7 Mo2 Cl2 94.9(3) . . ? N6 Mo2 Cl2 158.5(2) . . ? N4 Mo2 Cl2 82.3(2) . . ? C1 N1 Mo1 153.6(7) . . ? N1 C1 C3 105.8(9) . . ? N1 C1 C2 111.5(9) . . ? C3 C1 C2 109.6(10) . . ? N1 C1 C4 108.1(9) . . ? C3 C1 C4 108.1(10) . . ? C2 C1 C4 113.5(10) . . ? C5 N2 Mo1 178.1(8) . . ? N2 C5 C8 107.2(11) . . ? N2 C5 C7 108.1(11) . . ? C8 C5 C7 111.0(14) . . ? N2 C5 C6 108.9(9) . . ? C8 C5 C6 112.2(15) . . ? C7 C5 C6 109.3(12) . . ? C9 N3 N4 108.5(8) . . ? C9 N3 Mo1 131.4(7) . . ? N4 N3 Mo1 120.1(5) . . ? C12 N4 N3 107.8(8) . . ? C12 N4 Mo2 126.0(7) . . ? N3 N4 Mo2 125.3(6) . . ? N3 C9 C11 107.3(9) . . ? N3 C9 C10 122.7(10) . . ? C11 C9 C10 130.0(10) . . ? C9 C11 C12 108.6(9) . . ? N4 C12 C11 107.8(9) . . ? N4 C12 C13 121.8(10) . . ? C11 C12 C13 130.4(10) . . ? C14 N5 N6 108.2(7) . . ? C14 N5 Mo1 125.0(6) . . ? N6 N5 Mo1 126.7(5) . . ? C17 N6 N5 107.5(8) . . ? C17 N6 Mo2 133.5(7) . . ? N5 N6 Mo2 118.6(5) . . ? N5 C14 C16 107.3(9) . . ? N5 C14 C15 124.3(8) . . ? C16 C14 C15 128.4(9) . . ? C17 C16 C14 107.0(9) . . ? N6 C17 C16 110.0(9) . . ? N6 C17 C18 124.2(10) . . ? C16 C17 C18 125.8(9) . . ? C19 N7 Mo2 158.0(8) . . ? N7 C19 C22 110.8(10) . . ? N7 C19 C21 106.8(9) . . ? C22 C19 C21 110.0(11) . . ? N7 C19 C20 109.3(9) . . ? C22 C19 C20 109.6(11) . . ? C21 C19 C20 110.3(11) . . ? C23 N8 Mo2 164.4(8) . . ? C26 C23 N8 107.0(10) . . ? C26 C23 C24 111.6(13) . . ? N8 C23 C24 109.5(10) . . ? C26 C23 C25 112.0(14) . . ? N8 C23 C25 109.0(10) . . ? C24 C23 C25 107.7(12) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.315 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.203 # Attachment 'Revised Kalu1 (4b).cif' data_kalu _database_code_depnum_ccdc_archive 'CCDC 287647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H50 Cl2 N8 W2' _chemical_formula_weight 913.34 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' Cl Cl 0.1484 0.1585 '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' _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 18.373(3) _cell_length_b 10.7499(15) _cell_length_c 18.014(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.798(2) _cell_angle_gamma 90.00 _cell_volume 3516.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 26.5 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 6.717 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2378 _exptl_absorpt_correction_T_max 0.4323 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25289 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.26 _reflns_number_total 8284 _reflns_number_gt 5143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^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_number_reflns 8284 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.816 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.326901(10) 0.605428(16) 0.270969(10) 0.03705(6) Uani 1 1 d . . . W2 W 0.191977(10) 0.353752(16) 0.199632(10) 0.03902(6) Uani 1 1 d . . . Cl1 Cl 0.27842(7) 0.77123(10) 0.19091(7) 0.0568(3) Uani 1 1 d . . . N1 N 0.34211(19) 0.4156(3) 0.30772(19) 0.0407(9) Uani 1 1 d . . . N2 N 0.29678(18) 0.3221(3) 0.27596(18) 0.0394(9) Uani 1 1 d . . . C1 C 0.3917(3) 0.3626(4) 0.3628(2) 0.0493(12) Uani 1 1 d . . . C2 C 0.3779(3) 0.2370(4) 0.3646(3) 0.0511(13) Uani 1 1 d . . . H2 H 0.4038 0.1786 0.3964 0.061 Uiso 1 1 calc R . . C3 C 0.3192(3) 0.2148(4) 0.3109(3) 0.0474(12) Uani 1 1 d . . . C4 C 0.4495(3) 0.4345(5) 0.4118(3) 0.0825(19) Uani 1 1 d . . . H4A H 0.4807 0.4756 0.3813 0.099 Uiso 1 1 calc R . . H4B H 0.4785 0.3789 0.4461 0.099 Uiso 1 1 calc R . . H4C H 0.4266 0.4953 0.4397 0.099 Uiso 1 1 calc R . . C5 C 0.2830(3) 0.0953(4) 0.2883(3) 0.0834(19) Uani 1 1 d . . . H5A H 0.2367 0.0909 0.3067 0.100 Uiso 1 1 calc R . . H5B H 0.3140 0.0280 0.3091 0.100 Uiso 1 1 calc R . . H5C H 0.2748 0.0891 0.2345 0.100 Uiso 1 1 calc R . . N3 N 0.32161(19) 0.5067(3) 0.16056(18) 0.0363(9) Uani 1 1 d . . . N4 N 0.27435(19) 0.4109(3) 0.13374(19) 0.0384(9) Uani 1 1 d . . . C6 C 0.3621(2) 0.5336(4) 0.1059(2) 0.0397(11) Uani 1 1 d . . . C7 C 0.3420(3) 0.4567(4) 0.0457(2) 0.0516(13) Uani 1 1 d . . . H7 H 0.3613 0.4559 0.0009 0.062 Uiso 1 1 calc R . . C8 C 0.2875(3) 0.3810(4) 0.0648(2) 0.0509(13) Uani 1 1 d . . . C9 C 0.4192(2) 0.6323(4) 0.1115(2) 0.0518(13) Uani 1 1 d . . . H9A H 0.3966 0.7119 0.1163 0.062 Uiso 1 1 calc R . . H9B H 0.4422 0.6316 0.0671 0.062 Uiso 1 1 calc R . . H9C H 0.4556 0.6174 0.1548 0.062 Uiso 1 1 calc R . . C10 C 0.2472(3) 0.2799(5) 0.0175(3) 0.099(2) Uani 1 1 d . . . H10A H 0.2514 0.2032 0.0451 0.119 Uiso 1 1 calc R . . H10B H 0.2682 0.2699 -0.0277 0.119 Uiso 1 1 calc R . . H10C H 0.1961 0.3020 0.0049 0.119 Uiso 1 1 calc R . . N5 N 0.2769(2) 0.6430(3) 0.3424(2) 0.0482(10) Uani 1 1 d . . . C11 C 0.2411(3) 0.6775(4) 0.4058(3) 0.0621(15) Uani 1 1 d . . . C12 C 0.1681(3) 0.6151(6) 0.4023(3) 0.109(2) Uani 1 1 d . . . H12A H 0.1368 0.6389 0.3568 0.131 Uiso 1 1 calc R . . H12B H 0.1458 0.6398 0.4448 0.131 Uiso 1 1 calc R . . H12C H 0.1748 0.5265 0.4029 0.131 Uiso 1 1 calc R . . C13 C 0.2895(4) 0.6421(8) 0.4770(3) 0.157(4) Uani 1 1 d . . . H13A H 0.2958 0.5534 0.4787 0.188 Uiso 1 1 calc R . . H13B H 0.2672 0.6686 0.5191 0.188 Uiso 1 1 calc R . . H13C H 0.3366 0.6815 0.4789 0.188 Uiso 1 1 calc R . . C14 C 0.2301(5) 0.8157(5) 0.4018(5) 0.206(5) Uani 1 1 d . . . H14A H 0.2771 0.8564 0.4079 0.247 Uiso 1 1 calc R . . H14B H 0.2035 0.8416 0.4411 0.247 Uiso 1 1 calc R . . H14C H 0.2025 0.8375 0.3540 0.247 Uiso 1 1 calc R . . N6 N 0.41542(19) 0.6636(3) 0.29271(18) 0.0441(9) Uani 1 1 d . . . C15 C 0.4736(3) 0.7516(4) 0.3256(3) 0.0543(13) Uani 1 1 d . . . C16 C 0.4600(3) 0.7947(5) 0.4034(3) 0.090(2) Uani 1 1 d . . . H16A H 0.4122 0.8321 0.3994 0.109 Uiso 1 1 calc R . . H16B H 0.4969 0.8545 0.4228 0.109 Uiso 1 1 calc R . . H16C H 0.4627 0.7245 0.4366 0.109 Uiso 1 1 calc R . . C17 C 0.5483(3) 0.6893(5) 0.3295(3) 0.0805(18) Uani 1 1 d . . . H17A H 0.5523 0.6231 0.3657 0.097 Uiso 1 1 calc R . . H17B H 0.5865 0.7493 0.3443 0.097 Uiso 1 1 calc R . . H17C H 0.5533 0.6561 0.2811 0.097 Uiso 1 1 calc R . . C18 C 0.4695(3) 0.8611(4) 0.2716(3) 0.0802(18) Uani 1 1 d . . . H18A H 0.4775 0.8322 0.2231 0.096 Uiso 1 1 calc R . . H18B H 0.5066 0.9210 0.2901 0.096 Uiso 1 1 calc R . . H18C H 0.4218 0.8991 0.2675 0.096 Uiso 1 1 calc R . . Cl2 Cl 0.14244(8) 0.30604(13) 0.31122(7) 0.0709(4) Uani 1 1 d . . . N7 N 0.1403(2) 0.4879(3) 0.1779(2) 0.0483(10) Uani 1 1 d . . . C19 C 0.0849(3) 0.5726(4) 0.1416(3) 0.0587(14) Uani 1 1 d . . . C20 C 0.0801(3) 0.6868(4) 0.1906(3) 0.0754(17) Uani 1 1 d . . . H20A H 0.0664 0.6618 0.2377 0.090 Uiso 1 1 calc R . . H20B H 0.0438 0.7431 0.1656 0.090 Uiso 1 1 calc R . . H20C H 0.1272 0.7275 0.1994 0.090 Uiso 1 1 calc R . . C21 C 0.0108(3) 0.5082(5) 0.1282(4) 0.100(2) Uani 1 1 d . . . H21A H 0.0122 0.4415 0.0930 0.120 Uiso 1 1 calc R . . H21B H -0.0265 0.5668 0.1083 0.120 Uiso 1 1 calc R . . H21C H -0.0002 0.4754 0.1748 0.120 Uiso 1 1 calc R . . C22 C 0.1096(3) 0.6126(5) 0.0674(3) 0.097(2) Uani 1 1 d . . . H22A H 0.1594 0.6422 0.0772 0.116 Uiso 1 1 calc R . . H22B H 0.0780 0.6779 0.0449 0.116 Uiso 1 1 calc R . . H22C H 0.1067 0.5428 0.0339 0.116 Uiso 1 1 calc R . . N8 N 0.1528(2) 0.2274(3) 0.1474(2) 0.0516(10) Uani 1 1 d . . . C23 C 0.1005(3) 0.1341(5) 0.1123(3) 0.0660(15) Uani 1 1 d . . . C24 C 0.1417(3) 0.0185(4) 0.0987(3) 0.097(2) Uani 1 1 d . . . H24A H 0.1740 0.0354 0.0627 0.117 Uiso 1 1 calc R . . H24B H 0.1075 -0.0456 0.0797 0.117 Uiso 1 1 calc R . . H24C H 0.1702 -0.0087 0.1450 0.117 Uiso 1 1 calc R . . C25 C 0.0475(4) 0.1096(7) 0.1643(4) 0.164(4) Uani 1 1 d . . . H25A H 0.0736 0.0825 0.2118 0.197 Uiso 1 1 calc R . . H25B H 0.0137 0.0458 0.1437 0.197 Uiso 1 1 calc R . . H25C H 0.0208 0.1843 0.1712 0.197 Uiso 1 1 calc R . . C26 C 0.0618(4) 0.1781(6) 0.0365(4) 0.136(3) Uani 1 1 d . . . H26A H 0.0448 0.2618 0.0408 0.163 Uiso 1 1 calc R . . H26B H 0.0206 0.1248 0.0199 0.163 Uiso 1 1 calc R . . H26C H 0.0955 0.1755 0.0007 0.163 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.04165(12) 0.04048(10) 0.02925(10) -0.00228(8) 0.00613(9) -0.00316(9) W2 0.03601(12) 0.04294(10) 0.03758(12) -0.00184(9) 0.00392(9) -0.00153(9) Cl1 0.0658(9) 0.0475(6) 0.0567(8) 0.0089(6) 0.0080(7) 0.0077(6) N1 0.044(2) 0.042(2) 0.034(2) 0.0038(17) 0.0016(18) -0.0031(18) N2 0.038(2) 0.041(2) 0.040(2) 0.0070(17) 0.0080(19) -0.0016(17) C1 0.050(3) 0.062(3) 0.034(3) 0.005(2) -0.001(2) -0.003(3) C2 0.050(3) 0.053(3) 0.048(3) 0.016(2) 0.001(3) 0.003(2) C3 0.048(3) 0.042(3) 0.051(3) 0.008(2) 0.004(3) -0.002(2) C4 0.092(5) 0.081(4) 0.062(4) 0.015(3) -0.030(3) 0.000(3) C5 0.084(4) 0.052(3) 0.107(5) 0.020(3) -0.008(4) -0.004(3) N3 0.036(2) 0.0411(19) 0.032(2) 0.0011(16) 0.0068(18) 0.0020(17) N4 0.040(2) 0.043(2) 0.032(2) 0.0047(17) 0.0058(18) -0.0017(17) C6 0.039(3) 0.049(3) 0.032(3) 0.003(2) 0.006(2) 0.003(2) C7 0.061(4) 0.063(3) 0.031(3) -0.001(2) 0.006(3) -0.002(3) C8 0.062(4) 0.060(3) 0.031(3) -0.010(2) 0.009(3) -0.004(3) C9 0.055(3) 0.060(3) 0.043(3) 0.009(2) 0.016(3) -0.007(3) C10 0.114(6) 0.128(5) 0.064(4) -0.044(4) 0.043(4) -0.054(4) N5 0.054(3) 0.049(2) 0.045(2) -0.0034(19) 0.018(2) 0.0028(19) C11 0.079(4) 0.066(3) 0.049(3) -0.011(3) 0.032(3) -0.015(3) C12 0.078(5) 0.183(7) 0.074(4) -0.040(5) 0.038(4) -0.036(5) C13 0.107(6) 0.325(12) 0.043(4) -0.008(6) 0.030(4) -0.024(7) C14 0.367(14) 0.074(5) 0.240(10) -0.024(5) 0.247(11) 0.007(6) N6 0.047(2) 0.049(2) 0.036(2) 0.0015(17) 0.0061(19) -0.0027(19) C15 0.045(3) 0.063(3) 0.054(3) -0.009(3) 0.004(3) -0.018(3) C16 0.105(5) 0.110(5) 0.059(4) -0.039(3) 0.024(4) -0.044(4) C17 0.048(4) 0.104(4) 0.087(5) -0.023(4) 0.002(3) -0.023(3) C18 0.088(5) 0.071(4) 0.081(4) -0.013(3) 0.013(4) -0.037(3) Cl2 0.0661(10) 0.0924(9) 0.0593(9) 0.0133(7) 0.0253(8) -0.0052(8) N7 0.051(3) 0.056(2) 0.041(2) 0.0021(19) 0.019(2) 0.008(2) C19 0.050(4) 0.060(3) 0.063(4) -0.001(3) 0.003(3) 0.012(3) C20 0.062(4) 0.063(3) 0.102(5) -0.002(3) 0.016(4) 0.013(3) C21 0.072(5) 0.087(4) 0.137(6) -0.021(4) 0.002(4) 0.012(4) C22 0.112(5) 0.121(5) 0.056(4) 0.030(4) 0.008(4) 0.036(4) N8 0.042(3) 0.057(2) 0.059(3) -0.013(2) 0.017(2) -0.0073(19) C23 0.056(4) 0.059(3) 0.081(4) -0.021(3) 0.005(3) -0.015(3) C24 0.103(5) 0.060(4) 0.123(6) -0.032(4) 0.000(4) -0.009(3) C25 0.136(7) 0.185(8) 0.197(9) -0.114(7) 0.109(7) -0.120(6) C26 0.113(6) 0.092(5) 0.174(8) -0.011(5) -0.072(6) -0.029(4) _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 N6 1.730(3) . ? W1 N5 1.739(4) . ? W1 N1 2.151(3) . ? W1 N3 2.243(3) . ? W1 Cl1 2.3786(11) . ? W2 N7 1.738(3) . ? W2 N8 1.744(3) . ? W2 N4 2.151(3) . ? W2 N2 2.215(3) . ? W2 Cl2 2.3858(13) . ? N1 C1 1.365(5) . ? N1 N2 1.373(4) . ? N2 C3 1.347(5) . ? C1 C2 1.375(6) . ? C1 C4 1.490(6) . ? C2 C3 1.356(6) . ? C3 C5 1.475(6) . ? N3 C6 1.354(5) . ? N3 N4 1.386(4) . ? N4 C8 1.340(5) . ? C6 C7 1.368(5) . ? C6 C9 1.484(5) . ? C7 C8 1.375(6) . ? C8 C10 1.504(6) . ? N5 C11 1.450(5) . ? C11 C13 1.494(7) . ? C11 C12 1.492(7) . ? C11 C14 1.499(7) . ? N6 C15 1.481(5) . ? C15 C18 1.522(6) . ? C15 C17 1.520(6) . ? C15 C16 1.531(6) . ? N7 C19 1.445(5) . ? C19 C21 1.514(7) . ? C19 C22 1.536(7) . ? C19 C20 1.522(6) . ? N8 C23 1.464(5) . ? C23 C25 1.475(7) . ? C23 C24 1.495(6) . ? C23 C26 1.516(7) . ? 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 N6 W1 N5 109.42(16) . . ? N6 W1 N1 101.53(14) . . ? N5 W1 N1 92.93(14) . . ? N6 W1 N3 106.46(14) . . ? N5 W1 N3 144.11(15) . . ? N1 W1 N3 79.04(12) . . ? N6 W1 Cl1 96.79(11) . . ? N5 W1 Cl1 94.80(12) . . ? N1 W1 Cl1 156.46(10) . . ? N3 W1 Cl1 81.69(8) . . ? N7 W2 N8 110.97(17) . . ? N7 W2 N4 92.58(14) . . ? N8 W2 N4 101.08(14) . . ? N7 W2 N2 131.37(15) . . ? N8 W2 N2 117.61(15) . . ? N4 W2 N2 76.60(12) . . ? N7 W2 Cl2 95.89(11) . . ? N8 W2 Cl2 96.19(12) . . ? N4 W2 Cl2 156.59(10) . . ? N2 W2 Cl2 81.45(9) . . ? C1 N1 N2 107.0(3) . . ? C1 N1 W1 131.4(3) . . ? N2 N1 W1 121.6(3) . . ? C3 N2 N1 108.0(3) . . ? C3 N2 W2 126.6(3) . . ? N1 N2 W2 124.1(2) . . ? N1 C1 C2 108.8(4) . . ? N1 C1 C4 123.4(4) . . ? C2 C1 C4 127.8(4) . . ? C3 C2 C1 106.6(4) . . ? N2 C3 C2 109.6(4) . . ? N2 C3 C5 121.7(4) . . ? C2 C3 C5 128.7(4) . . ? C6 N3 N4 106.9(3) . . ? C6 N3 W1 126.2(3) . . ? N4 N3 W1 126.9(3) . . ? C8 N4 N3 108.0(3) . . ? C8 N4 W2 133.2(3) . . ? N3 N4 W2 118.4(3) . . ? N3 C6 C7 109.6(4) . . ? N3 C6 C9 124.3(4) . . ? C7 C6 C9 126.1(4) . . ? C6 C7 C8 106.2(4) . . ? N4 C8 C7 109.3(4) . . ? N4 C8 C10 123.7(4) . . ? C7 C8 C10 126.9(4) . . ? C11 N5 W1 175.2(3) . . ? N5 C11 C13 109.2(5) . . ? N5 C11 C12 111.4(4) . . ? C13 C11 C12 109.6(5) . . ? N5 C11 C14 106.9(4) . . ? C13 C11 C14 110.6(6) . . ? C12 C11 C14 109.2(6) . . ? C15 N6 W1 156.4(3) . . ? N6 C15 C18 106.0(4) . . ? N6 C15 C17 109.1(4) . . ? C18 C15 C17 109.0(4) . . ? N6 C15 C16 110.6(4) . . ? C18 C15 C16 110.6(4) . . ? C17 C15 C16 111.3(5) . . ? C19 N7 W2 161.4(3) . . ? N7 C19 C21 109.7(4) . . ? N7 C19 C22 106.8(4) . . ? C21 C19 C22 111.5(5) . . ? N7 C19 C20 110.2(4) . . ? C21 C19 C20 109.3(4) . . ? C22 C19 C20 109.3(4) . . ? C23 N8 W2 163.0(3) . . ? N8 C23 C25 107.5(4) . . ? N8 C23 C24 109.0(4) . . ? C25 C23 C24 110.8(5) . . ? N8 C23 C26 111.2(4) . . ? C25 C23 C26 111.3(6) . . ? C24 C23 C26 107.0(5) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.618 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.101 # Attachment 'Revised Wush1 (5b).cif' data_wush _database_code_depnum_ccdc_archive 'CCDC 287648' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H56 N10 W' _chemical_formula_weight 788.74 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' W W -0.8490 6.8722 '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 14.5205(11) _cell_length_b 13.8974(11) _cell_length_c 19.5636(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.661(2) _cell_angle_gamma 90.00 _cell_volume 3928.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 923 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26.0 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.975 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4689 _exptl_absorpt_correction_T_max 0.6475 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28344 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9067 _reflns_number_gt 5840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^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_number_reflns 9067 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.229639(10) 0.153260(10) 0.229380(6) 0.03660(5) Uani 1 1 d . . . N1 N 0.16152(18) 0.14049(18) 0.15063(12) 0.0395(7) Uani 1 1 d . . . C1 C 0.0935(3) 0.1099(3) 0.09574(18) 0.0547(10) Uani 1 1 d . . . C2 C 0.0163(3) 0.1826(3) 0.0855(2) 0.0852(15) Uani 1 1 d . . . H2A H -0.0100 0.1922 0.1281 0.102 Uiso 1 1 calc R . . H2B H -0.0306 0.1593 0.0515 0.102 Uiso 1 1 calc R . . H2C H 0.0403 0.2425 0.0705 0.102 Uiso 1 1 calc R . . C3 C 0.1422(3) 0.0996(4) 0.03005(18) 0.0999(17) Uani 1 1 d . . . H3A H 0.1724 0.1589 0.0208 0.120 Uiso 1 1 calc R . . H3B H 0.0974 0.0843 -0.0078 0.120 Uiso 1 1 calc R . . H3C H 0.1873 0.0490 0.0360 0.120 Uiso 1 1 calc R . . C4 C 0.0566(3) 0.0136(3) 0.1162(2) 0.0898(15) Uani 1 1 d . . . H4A H 0.1065 -0.0318 0.1226 0.108 Uiso 1 1 calc R . . H4B H 0.0113 -0.0090 0.0808 0.108 Uiso 1 1 calc R . . H4C H 0.0284 0.0204 0.1584 0.108 Uiso 1 1 calc R . . N2 N 0.15220(17) 0.16273(19) 0.29205(12) 0.0412(7) Uani 1 1 d . . . C5 C 0.0679(3) 0.1866(3) 0.32357(18) 0.0558(10) Uani 1 1 d . . . C6 C 0.0817(3) 0.1667(4) 0.39902(19) 0.125(2) Uani 1 1 d . . . H6A H 0.0987 0.1004 0.4064 0.149 Uiso 1 1 calc R . . H6B H 0.0253 0.1795 0.4191 0.149 Uiso 1 1 calc R . . H6C H 0.1300 0.2073 0.4200 0.149 Uiso 1 1 calc R . . C7 C -0.0113(3) 0.1272(4) 0.2908(3) 0.119(2) Uani 1 1 d . . . H7A H -0.0275 0.1490 0.2446 0.143 Uiso 1 1 calc R . . H7B H -0.0637 0.1340 0.3167 0.143 Uiso 1 1 calc R . . H7C H 0.0068 0.0608 0.2902 0.143 Uiso 1 1 calc R . . C8 C 0.0484(3) 0.2913(3) 0.3100(3) 0.120(2) Uani 1 1 d . . . H8A H 0.0990 0.3291 0.3307 0.144 Uiso 1 1 calc R . . H8B H -0.0074 0.3091 0.3292 0.144 Uiso 1 1 calc R . . H8C H 0.0413 0.3025 0.2613 0.144 Uiso 1 1 calc R . . N3 N 0.25283(18) 0.30512(19) 0.23127(13) 0.0414(7) Uani 1 1 d . . . N4 N 0.28346(18) 0.3444(2) 0.29480(12) 0.0466(7) Uani 1 1 d . . . N5 N 0.2748(2) 0.4613(2) 0.21456(13) 0.0537(8) Uani 1 1 d . . . C9 C 0.2952(2) 0.4360(3) 0.28146(16) 0.0472(9) Uani 1 1 d . . . C10 C 0.3232(3) 0.5094(3) 0.33648(18) 0.0620(11) Uani 1 1 d . . . H10 H 0.3758 0.5458 0.3223 0.074 Uiso 1 1 calc R . . C11 C 0.3530(3) 0.4622(3) 0.40400(18) 0.0983(16) Uani 1 1 d . . . H11A H 0.3025 0.4255 0.4187 0.118 Uiso 1 1 calc R . . H11B H 0.3712 0.5106 0.4376 0.118 Uiso 1 1 calc R . . H11C H 0.4044 0.4202 0.3988 0.118 Uiso 1 1 calc R . . C12 C 0.2456(4) 0.5787(3) 0.3437(2) 0.120(2) Uani 1 1 d . . . H12A H 0.2301 0.6112 0.3008 0.144 Uiso 1 1 calc R . . H12B H 0.2645 0.6250 0.3787 0.144 Uiso 1 1 calc R . . H12C H 0.1924 0.5442 0.3562 0.144 Uiso 1 1 calc R . . C13 C 0.2493(2) 0.3780(2) 0.18553(16) 0.0418(9) Uani 1 1 d . . . C14 C 0.2152(2) 0.3696(2) 0.11108(15) 0.0476(9) Uani 1 1 d . . . H14 H 0.1972 0.3027 0.1015 0.057 Uiso 1 1 calc R . . C15 C 0.2911(3) 0.3965(3) 0.06605(17) 0.0757(13) Uani 1 1 d . . . H15A H 0.3072 0.4630 0.0730 0.091 Uiso 1 1 calc R . . H15B H 0.2693 0.3861 0.0187 0.091 Uiso 1 1 calc R . . H15C H 0.3447 0.3572 0.0781 0.091 Uiso 1 1 calc R . . C16 C 0.1310(3) 0.4332(3) 0.09436(18) 0.0770(13) Uani 1 1 d . . . H16A H 0.0844 0.4168 0.1239 0.092 Uiso 1 1 calc R . . H16B H 0.1070 0.4235 0.0474 0.092 Uiso 1 1 calc R . . H16C H 0.1483 0.4994 0.1012 0.092 Uiso 1 1 calc R . . N6 N 0.25636(17) 0.00222(18) 0.23215(13) 0.0404(7) Uani 1 1 d . . . N7 N 0.28752(19) -0.0391(2) 0.17410(13) 0.0473(7) Uani 1 1 d . . . N8 N 0.2813(2) -0.1529(2) 0.25488(13) 0.0535(8) Uani 1 1 d . . . C17 C 0.3006(3) -0.1300(3) 0.19087(18) 0.0503(10) Uani 1 1 d . . . C18 C 0.3323(3) -0.2032(3) 0.1411(2) 0.0713(13) Uani 1 1 d . . . H18 H 0.3868 -0.2359 0.1637 0.086 Uiso 1 1 calc R . . C19 C 0.3596(4) -0.1588(3) 0.0772(2) 0.138(2) Uani 1 1 d . . . H19A H 0.3078 -0.1246 0.0546 0.165 Uiso 1 1 calc R . . H19B H 0.3787 -0.2081 0.0474 0.165 Uiso 1 1 calc R . . H19C H 0.4098 -0.1148 0.0884 0.165 Uiso 1 1 calc R . . C20 C 0.2583(4) -0.2776(4) 0.1253(3) 0.134(2) Uani 1 1 d . . . H20A H 0.2424 -0.3059 0.1673 0.161 Uiso 1 1 calc R . . H20B H 0.2807 -0.3267 0.0966 0.161 Uiso 1 1 calc R . . H20C H 0.2045 -0.2478 0.1018 0.161 Uiso 1 1 calc R . . C21 C 0.2543(2) -0.0690(3) 0.27925(16) 0.0440(9) Uani 1 1 d . . . C22 C 0.2202(2) -0.0585(3) 0.34857(16) 0.0501(9) Uani 1 1 d . . . H22 H 0.2069 0.0097 0.3560 0.060 Uiso 1 1 calc R . . C23 C 0.2929(3) -0.0915(3) 0.40528(17) 0.0720(13) Uani 1 1 d . . . H23A H 0.3048 -0.1589 0.3999 0.086 Uiso 1 1 calc R . . H23B H 0.2706 -0.0805 0.4492 0.086 Uiso 1 1 calc R . . H23C H 0.3490 -0.0559 0.4024 0.086 Uiso 1 1 calc R . . C24 C 0.1317(3) -0.1155(3) 0.3522(2) 0.0833(14) Uani 1 1 d . . . H24A H 0.0848 -0.0916 0.3184 0.100 Uiso 1 1 calc R . . H24B H 0.1111 -0.1087 0.3971 0.100 Uiso 1 1 calc R . . H24C H 0.1431 -0.1822 0.3434 0.100 Uiso 1 1 calc R . . N9 N 0.36155(19) 0.13239(19) 0.31479(13) 0.0409(7) Uani 1 1 d . . . C25 C 0.3625(2) 0.1735(2) 0.37725(16) 0.0478(9) Uani 1 1 d . . . H25 H 0.3138 0.2136 0.3863 0.057 Uiso 1 1 calc R . . C26 C 0.4344(3) 0.1577(3) 0.42859(16) 0.0603(10) Uani 1 1 d . . . H26 H 0.4332 0.1858 0.4716 0.072 Uiso 1 1 calc R . . C27 C 0.5065(3) 0.1004(3) 0.4148(2) 0.0674(12) Uani 1 1 d . . . H27 H 0.5554 0.0895 0.4483 0.081 Uiso 1 1 calc R . . C28 C 0.5066(2) 0.0589(3) 0.35143(18) 0.0587(10) Uani 1 1 d . . . H28 H 0.5554 0.0200 0.3410 0.070 Uiso 1 1 calc R . . C29 C 0.4328(2) 0.0762(3) 0.30357(17) 0.0479(9) Uani 1 1 d . . . H29 H 0.4326 0.0470 0.2608 0.057 Uiso 1 1 calc R . . N10 N 0.36876(19) 0.17679(18) 0.16974(12) 0.0398(7) Uani 1 1 d . . . C30 C 0.3791(2) 0.1324(2) 0.11011(15) 0.0478(9) Uani 1 1 d . . . H30 H 0.3334 0.0896 0.0926 0.057 Uiso 1 1 calc R . . C31 C 0.4545(3) 0.1471(3) 0.07339(17) 0.0575(10) Uani 1 1 d . . . H31 H 0.4589 0.1157 0.0319 0.069 Uiso 1 1 calc R . . C32 C 0.5220(3) 0.2085(3) 0.09928(18) 0.0617(11) Uani 1 1 d . . . H32 H 0.5737 0.2191 0.0757 0.074 Uiso 1 1 calc R . . C33 C 0.5137(3) 0.2550(3) 0.16047(17) 0.0567(10) Uani 1 1 d . . . H33 H 0.5593 0.2970 0.1791 0.068 Uiso 1 1 calc R . . C34 C 0.4361(2) 0.2375(3) 0.19307(16) 0.0476(9) Uani 1 1 d . . . H34 H 0.4299 0.2699 0.2340 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03898(8) 0.03522(8) 0.03524(6) -0.00278(8) 0.00191(5) -0.00226(9) N1 0.0428(17) 0.0345(17) 0.0400(13) -0.0026(13) -0.0016(12) -0.0042(14) C1 0.051(3) 0.057(3) 0.053(2) -0.0112(19) -0.013(2) -0.009(2) C2 0.065(3) 0.093(4) 0.090(3) -0.007(3) -0.028(3) -0.001(3) C3 0.087(4) 0.153(5) 0.057(3) -0.040(3) -0.009(2) -0.018(3) C4 0.086(3) 0.072(3) 0.105(3) -0.013(3) -0.028(3) -0.027(3) N2 0.0408(16) 0.0381(17) 0.0450(14) -0.0025(14) 0.0060(13) 0.0024(14) C5 0.055(3) 0.060(3) 0.054(2) -0.0012(19) 0.014(2) 0.010(2) C6 0.111(4) 0.209(7) 0.060(3) 0.009(3) 0.043(3) 0.063(4) C7 0.060(3) 0.156(6) 0.149(5) -0.040(4) 0.043(3) -0.022(3) C8 0.109(4) 0.081(4) 0.181(5) 0.025(4) 0.078(4) 0.047(3) N3 0.051(2) 0.0366(16) 0.0370(14) -0.0048(14) 0.0061(14) -0.0061(14) N4 0.059(2) 0.0382(17) 0.0420(14) -0.0038(15) 0.0007(13) -0.0073(17) N5 0.075(2) 0.0391(18) 0.0456(16) -0.0004(16) 0.0012(15) -0.0074(17) C9 0.055(3) 0.039(2) 0.047(2) -0.0031(18) 0.0003(18) -0.0060(18) C10 0.083(3) 0.044(3) 0.056(2) -0.0090(19) -0.008(2) -0.011(2) C11 0.154(5) 0.072(3) 0.062(3) -0.012(3) -0.026(3) -0.019(3) C12 0.159(5) 0.086(4) 0.108(4) -0.052(3) -0.027(4) 0.037(4) C13 0.045(2) 0.040(2) 0.0405(18) -0.0017(16) 0.0061(17) -0.0026(17) C14 0.058(2) 0.043(2) 0.0421(18) 0.0016(16) 0.0030(17) -0.0071(19) C15 0.078(3) 0.104(4) 0.046(2) 0.010(2) 0.009(2) 0.001(3) C16 0.074(3) 0.096(4) 0.059(2) -0.006(2) -0.006(2) 0.012(3) N6 0.0433(19) 0.0342(17) 0.0439(15) -0.0060(14) 0.0051(14) -0.0005(13) N7 0.058(2) 0.0368(18) 0.0486(16) -0.0070(15) 0.0111(15) -0.0007(16) N8 0.067(2) 0.0392(17) 0.0557(18) 0.0053(17) 0.0143(16) 0.0092(19) C17 0.055(2) 0.040(3) 0.057(2) -0.0016(18) 0.0103(19) 0.0043(19) C18 0.095(4) 0.052(3) 0.070(3) -0.010(2) 0.025(3) 0.017(3) C19 0.235(7) 0.082(4) 0.115(4) -0.009(3) 0.112(4) 0.030(4) C20 0.169(6) 0.095(4) 0.149(5) -0.064(4) 0.058(4) -0.029(4) C21 0.039(2) 0.043(2) 0.049(2) -0.0034(18) -0.0004(17) -0.0030(18) C22 0.058(3) 0.043(2) 0.051(2) -0.0003(18) 0.0129(19) 0.005(2) C23 0.085(3) 0.078(3) 0.053(2) 0.010(2) 0.013(2) 0.005(3) C24 0.069(3) 0.099(4) 0.086(3) -0.001(3) 0.028(3) -0.015(3) N9 0.0378(17) 0.0389(19) 0.0456(15) 0.0016(13) 0.0026(13) 0.0008(14) C25 0.054(2) 0.040(2) 0.050(2) -0.0025(17) 0.0061(18) -0.0065(18) C26 0.066(3) 0.075(3) 0.0371(18) -0.004(2) -0.0067(19) -0.014(3) C27 0.054(3) 0.086(3) 0.059(3) 0.008(2) -0.011(2) -0.006(2) C28 0.042(2) 0.072(3) 0.061(2) 0.005(2) 0.001(2) 0.008(2) C29 0.045(2) 0.054(2) 0.0446(19) -0.0002(18) 0.0040(18) 0.0003(19) N10 0.0449(18) 0.0390(19) 0.0350(14) -0.0025(12) 0.0019(13) -0.0031(14) C30 0.051(2) 0.048(3) 0.0432(19) -0.0028(17) -0.0016(17) -0.0034(18) C31 0.064(3) 0.065(3) 0.0457(19) -0.004(2) 0.0162(19) 0.001(2) C32 0.052(3) 0.078(3) 0.057(2) 0.003(2) 0.017(2) -0.005(2) C33 0.048(3) 0.065(3) 0.056(2) 0.004(2) 0.0029(19) -0.012(2) C34 0.050(2) 0.052(2) 0.0404(18) 0.0001(17) 0.0020(18) -0.007(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 W1 N2 1.748(2) . ? W1 N1 1.756(2) . ? W1 N6 2.134(3) . ? W1 N3 2.137(3) . ? W1 N9 2.432(3) . ? W1 N10 2.452(3) . ? N1 C1 1.449(4) . ? C1 C2 1.507(5) . ? C1 C4 1.511(5) . ? C1 C3 1.534(5) . ? N2 C5 1.462(4) . ? C5 C6 1.496(5) . ? C5 C8 1.500(5) . ? C5 C7 1.507(5) . ? N3 C13 1.349(4) . ? N3 N4 1.390(3) . ? N4 C9 1.314(4) . ? N5 C13 1.326(4) . ? N5 C9 1.359(4) . ? C9 C10 1.509(4) . ? C10 C11 1.500(5) . ? C10 C12 1.499(5) . ? C13 C14 1.496(4) . ? C14 C16 1.518(5) . ? C14 C15 1.523(4) . ? N6 C21 1.355(4) . ? N6 N7 1.388(3) . ? N7 C17 1.314(4) . ? N8 C21 1.333(4) . ? N8 C17 1.348(4) . ? C17 C18 1.512(5) . ? C18 C19 1.481(5) . ? C18 C20 1.501(6) . ? C21 C22 1.496(4) . ? C22 C23 1.524(4) . ? C22 C24 1.518(5) . ? N9 C29 1.332(4) . ? N9 C25 1.348(4) . ? C25 C26 1.393(4) . ? C26 C27 1.364(5) . ? C27 C28 1.367(5) . ? C28 C29 1.372(4) . ? N10 C34 1.338(4) . ? N10 C30 1.341(4) . ? C30 C31 1.383(4) . ? C31 C32 1.360(5) . ? C32 C33 1.376(5) . ? C33 C34 1.370(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 W1 N1 106.10(11) . . ? N2 W1 N6 100.61(11) . . ? N1 W1 N6 90.47(11) . . ? N2 W1 N3 91.41(11) . . ? N1 W1 N3 100.90(11) . . ? N6 W1 N3 160.55(9) . . ? N2 W1 N9 92.56(10) . . ? N1 W1 N9 158.16(10) . . ? N6 W1 N9 74.72(9) . . ? N3 W1 N9 89.64(9) . . ? N2 W1 N10 160.14(10) . . ? N1 W1 N10 90.87(10) . . ? N6 W1 N10 89.25(9) . . ? N3 W1 N10 74.98(9) . . ? N9 W1 N10 73.31(8) . . ? C1 N1 W1 164.5(2) . . ? N1 C1 C2 110.2(3) . . ? N1 C1 C4 107.3(3) . . ? C2 C1 C4 110.5(3) . . ? N1 C1 C3 108.2(3) . . ? C2 C1 C3 110.5(3) . . ? C4 C1 C3 110.1(3) . . ? C5 N2 W1 159.4(2) . . ? N2 C5 C6 109.7(3) . . ? N2 C5 C8 107.2(3) . . ? C6 C5 C8 111.0(4) . . ? N2 C5 C7 109.4(3) . . ? C6 C5 C7 109.9(4) . . ? C8 C5 C7 109.5(4) . . ? C13 N3 N4 106.6(3) . . ? C13 N3 W1 137.2(2) . . ? N4 N3 W1 116.1(2) . . ? C9 N4 N3 103.9(2) . . ? C13 N5 C9 102.2(3) . . ? N4 C9 N5 114.9(3) . . ? N4 C9 C10 122.9(3) . . ? N5 C9 C10 122.0(3) . . ? C11 C10 C12 110.7(4) . . ? C11 C10 C9 111.5(3) . . ? C12 C10 C9 110.4(3) . . ? N5 C13 N3 112.4(3) . . ? N5 C13 C14 122.4(3) . . ? N3 C13 C14 125.1(3) . . ? C13 C14 C16 110.3(3) . . ? C13 C14 C15 110.8(3) . . ? C16 C14 C15 110.3(3) . . ? C21 N6 N7 106.6(3) . . ? C21 N6 W1 136.0(2) . . ? N7 N6 W1 117.4(2) . . ? C17 N7 N6 104.1(3) . . ? C21 N8 C17 102.7(3) . . ? N7 C17 N8 114.9(3) . . ? N7 C17 C18 122.1(3) . . ? N8 C17 C18 123.0(3) . . ? C19 C18 C17 112.7(3) . . ? C19 C18 C20 111.0(4) . . ? C17 C18 C20 109.8(4) . . ? N8 C21 N6 111.6(3) . . ? N8 C21 C22 123.0(3) . . ? N6 C21 C22 125.2(3) . . ? C21 C22 C23 111.3(3) . . ? C21 C22 C24 110.4(3) . . ? C23 C22 C24 109.7(3) . . ? C29 N9 C25 117.4(3) . . ? C29 N9 W1 121.9(2) . . ? C25 N9 W1 120.6(2) . . ? N9 C25 C26 121.8(3) . . ? C27 C26 C25 119.0(3) . . ? C26 C27 C28 119.6(4) . . ? C29 C28 C27 118.3(4) . . ? N9 C29 C28 123.8(3) . . ? C34 N10 C30 116.5(3) . . ? C34 N10 W1 122.0(2) . . ? C30 N10 W1 121.3(2) . . ? N10 C30 C31 123.1(3) . . ? C32 C31 C30 118.6(3) . . ? C31 C32 C33 119.7(4) . . ? C34 C33 C32 118.0(4) . . ? N10 C34 C33 124.1(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.372 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.078 # Attachment 'Revised Wfle1 (6b).cif' data_wfle _database_code_depnum_ccdc_archive 'CCDC 287649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 F6 N12 W' _chemical_formula_weight 758.41 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0230(12) _cell_length_b 12.6800(19) _cell_length_c 13.964(2) _cell_angle_alpha 95.403(2) _cell_angle_beta 90.521(3) _cell_angle_gamma 102.089(3) _cell_volume 1554.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 934 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 21.0 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 3.784 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5182 _exptl_absorpt_correction_T_max 0.7034 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11030 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.1758 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7105 _reflns_number_gt 3209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^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_number_reflns 7105 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1390 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.819 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.17813(4) 0.27253(3) 0.23765(3) 0.05021(15) Uani 1 1 d . . . N1 N 0.2770(7) 0.1858(5) 0.1727(5) 0.0519(19) Uani 1 1 d . . . C1 C 0.3377(11) 0.1006(8) 0.1218(8) 0.072(3) Uani 1 1 d . . . C2 C 0.3972(16) 0.0390(11) 0.1953(11) 0.153(6) Uani 1 1 d . . . H2A H 0.4730 0.0877 0.2359 0.184 Uiso 1 1 calc R . . H2B H 0.4410 -0.0169 0.1631 0.184 Uiso 1 1 calc R . . H2C H 0.3154 0.0069 0.2338 0.184 Uiso 1 1 calc R . . C3 C 0.2077(15) 0.0228(10) 0.0676(10) 0.122(5) Uani 1 1 d . . . H3A H 0.1593 -0.0291 0.1102 0.150 Uiso 1 1 d . . . H3B H 0.2448 -0.0146 0.0135 0.150 Uiso 1 1 d . . . H3C H 0.1349 0.0616 0.0465 0.150 Uiso 1 1 d . . . C4 C 0.4583(16) 0.1467(10) 0.0591(12) 0.185(9) Uani 1 1 d . . . H4A H 0.4165 0.1811 0.0100 0.223 Uiso 1 1 calc R . . H4B H 0.5034 0.0900 0.0296 0.223 Uiso 1 1 calc R . . H4C H 0.5342 0.1992 0.0964 0.223 Uiso 1 1 calc R . . N2 N 0.0269(7) 0.1852(6) 0.2869(5) 0.059(2) Uani 1 1 d . . . C5 C -0.0780(10) 0.0944(8) 0.3156(7) 0.065(3) Uani 1 1 d . . . C6 C 0.0122(13) 0.0164(9) 0.3552(9) 0.109(4) Uani 1 1 d . . . H6A H 0.0796 -0.0034 0.3072 0.131 Uiso 1 1 calc R . . H6B H -0.0568 -0.0475 0.3714 0.131 Uiso 1 1 calc R . . H6C H 0.0700 0.0516 0.4117 0.131 Uiso 1 1 calc R . . C7 C -0.1734(13) 0.0398(10) 0.2298(9) 0.120(5) Uani 1 1 d . . . H7A H -0.2344 0.0873 0.2088 0.143 Uiso 1 1 calc R . . H7B H -0.2379 -0.0257 0.2466 0.143 Uiso 1 1 calc R . . H7C H -0.1090 0.0228 0.1788 0.143 Uiso 1 1 calc R . . C8 C -0.1732(17) 0.1343(11) 0.3955(11) 0.190(9) Uani 1 1 d . . . H8A H -0.1076 0.1723 0.4478 0.228 Uiso 1 1 calc R . . H8B H -0.2413 0.0735 0.4180 0.228 Uiso 1 1 calc R . . H8C H -0.2305 0.1822 0.3710 0.228 Uiso 1 1 calc R . . N3 N 0.0998(8) 0.2851(6) 0.0252(6) 0.065(2) Uani 1 1 d . . . N4 N 0.0480(7) 0.2926(6) 0.1129(5) 0.0539(19) Uani 1 1 d . . . N5 N -0.0948(8) 0.3008(8) 0.1106(6) 0.085(3) Uani 1 1 d . . . N6 N -0.1364(9) 0.3018(8) 0.0199(6) 0.085(3) Uani 1 1 d . . . C9 C -0.0176(10) 0.2922(8) -0.0298(7) 0.059(3) Uani 1 1 d . . . C10 C -0.0124(10) 0.2853(9) -0.1333(6) 0.054(2) Uani 1 1 d . . . F1 F 0.0815(8) 0.2383(7) -0.1746(4) 0.129(3) Uani 1 1 d . . . F2 F -0.1498(7) 0.2465(6) -0.1766(4) 0.116(2) Uani 1 1 d . . . F3 F 0.0181(8) 0.3874(6) -0.1637(5) 0.124(2) Uani 1 1 d . . . N7 N 0.2730(9) 0.2704(7) 0.4506(6) 0.076(2) Uani 1 1 d . . . N8 N 0.3198(8) 0.2966(6) 0.3666(5) 0.055(2) Uani 1 1 d . . . N9 N 0.4658(10) 0.3248(11) 0.3696(7) 0.136(5) Uani 1 1 d . . . N10 N 0.5177(10) 0.3222(11) 0.4591(7) 0.134(5) Uani 1 1 d . . . C11 C 0.3943(12) 0.2840(9) 0.5041(8) 0.067(3) Uani 1 1 d . . . C12 C 0.3923(13) 0.2689(12) 0.5988(11) 0.090(4) Uani 1 1 d . . . F4 F 0.2730(10) 0.2385(10) 0.6422(5) 0.196(5) Uani 1 1 d . . . F5 F 0.4541(18) 0.3455(13) 0.6597(7) 0.287(10) Uani 1 1 d . . . F6 F 0.475(2) 0.2072(15) 0.6249(8) 0.291(10) Uani 1 1 d . . . N11 N 0.3508(7) 0.4233(6) 0.1814(5) 0.0544(19) Uani 1 1 d . . . C13 C 0.3094(10) 0.5071(8) 0.1477(7) 0.061(3) Uani 1 1 d . . . H13 H 0.2080 0.5115 0.1511 0.073 Uiso 1 1 calc R . . C14 C 0.4120(12) 0.5911(8) 0.1065(7) 0.072(3) Uani 1 1 d . . . H14 H 0.3811 0.6495 0.0830 0.086 Uiso 1 1 calc R . . C15 C 0.5604(11) 0.5791(9) 0.1042(7) 0.076(3) Uani 1 1 d . . . H15 H 0.6318 0.6309 0.0770 0.092 Uiso 1 1 calc R . . C16 C 0.6048(11) 0.4981(9) 0.1385(7) 0.070(3) Uani 1 1 d . . . H16 H 0.7064 0.4937 0.1376 0.084 Uiso 1 1 calc R . . C17 C 0.5003(8) 0.4208(7) 0.1754(6) 0.055(2) Uani 1 1 d . . . H17 H 0.5327 0.3625 0.1979 0.066 Uiso 1 1 calc R . . N12 N 0.0947(7) 0.4237(6) 0.3153(5) 0.0529(19) Uani 1 1 d . . . C18 C 0.1850(10) 0.5106(8) 0.3607(7) 0.065(3) Uani 1 1 d . . . H18 H 0.2890 0.5147 0.3595 0.078 Uiso 1 1 calc R . . C19 C 0.1343(11) 0.5947(8) 0.4093(7) 0.069(3) Uani 1 1 d . . . H19 H 0.2028 0.6534 0.4403 0.082 Uiso 1 1 calc R . . C20 C -0.0174(13) 0.5914(9) 0.4117(7) 0.074(3) Uani 1 1 d . . . H20 H -0.0544 0.6483 0.4428 0.088 Uiso 1 1 calc R . . C21 C -0.1148(11) 0.5014(9) 0.3668(7) 0.074(3) Uani 1 1 d . . . H21 H -0.2193 0.4957 0.3677 0.088 Uiso 1 1 calc R . . C22 C -0.0546(10) 0.4211(8) 0.3211(6) 0.059(2) Uani 1 1 d . . . H22 H -0.1213 0.3604 0.2919 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03836(18) 0.0589(3) 0.0520(2) 0.00458(17) 0.00359(15) 0.00741(15) N1 0.052(4) 0.046(4) 0.054(5) -0.009(4) -0.007(4) 0.008(4) C1 0.060(6) 0.063(7) 0.094(8) -0.013(6) -0.001(6) 0.022(6) C2 0.148(13) 0.119(12) 0.211(17) -0.001(12) -0.050(12) 0.084(11) C3 0.117(10) 0.098(10) 0.143(12) -0.047(9) -0.007(9) 0.033(8) C4 0.179(14) 0.087(10) 0.27(2) -0.024(11) 0.179(15) 0.001(9) N2 0.049(4) 0.057(5) 0.062(5) 0.008(4) 0.001(4) -0.009(4) C5 0.053(5) 0.059(7) 0.077(7) 0.011(6) 0.011(5) -0.005(5) C6 0.109(9) 0.094(9) 0.115(10) 0.043(8) -0.006(8) -0.014(8) C7 0.104(9) 0.115(11) 0.113(11) 0.023(9) -0.024(8) -0.042(8) C8 0.200(16) 0.118(12) 0.229(18) -0.014(12) 0.172(15) -0.009(11) N3 0.049(4) 0.075(6) 0.069(6) -0.006(5) 0.013(4) 0.012(4) N4 0.046(4) 0.067(5) 0.051(5) -0.005(4) 0.004(4) 0.022(4) N5 0.053(5) 0.133(8) 0.074(7) 0.020(6) 0.015(5) 0.031(5) N6 0.063(5) 0.154(9) 0.045(5) 0.010(6) -0.006(4) 0.036(5) C9 0.046(5) 0.079(7) 0.053(7) 0.012(5) 0.005(5) 0.014(5) C10 0.052(5) 0.072(7) 0.036(6) 0.011(5) 0.009(5) 0.002(5) F1 0.142(6) 0.210(8) 0.055(4) 0.008(5) 0.017(4) 0.086(6) F2 0.095(5) 0.165(7) 0.073(4) 0.000(4) -0.018(4) 0.002(4) F3 0.133(6) 0.139(7) 0.101(5) 0.057(5) 0.003(4) 0.015(5) N7 0.053(5) 0.110(7) 0.059(6) 0.007(5) -0.008(5) 0.001(5) N8 0.046(4) 0.072(6) 0.047(5) 0.011(4) 0.010(4) 0.012(4) N9 0.057(6) 0.255(14) 0.084(8) 0.073(9) -0.006(5) -0.019(7) N10 0.059(6) 0.257(14) 0.081(8) 0.075(9) -0.016(6) -0.006(7) C11 0.064(7) 0.086(8) 0.049(7) -0.005(6) -0.004(6) 0.013(6) C12 0.056(6) 0.105(10) 0.098(12) 0.010(9) 0.018(7) -0.008(7) F4 0.133(7) 0.339(14) 0.082(6) 0.074(7) 0.018(5) -0.048(8) F5 0.330(19) 0.340(18) 0.078(7) -0.022(9) -0.014(8) -0.167(16) F6 0.40(2) 0.49(2) 0.116(9) 0.164(13) 0.086(10) 0.34(2) N11 0.043(4) 0.055(5) 0.063(5) 0.003(4) 0.010(4) 0.005(4) C13 0.060(6) 0.058(7) 0.067(7) -0.001(5) 0.010(5) 0.019(5) C14 0.083(7) 0.068(7) 0.065(7) 0.022(6) 0.019(6) 0.012(6) C15 0.060(6) 0.094(9) 0.066(7) 0.017(6) 0.005(5) -0.009(6) C16 0.056(6) 0.085(8) 0.069(7) 0.016(6) 0.010(5) 0.012(6) C17 0.035(4) 0.059(6) 0.069(7) 0.012(5) 0.005(4) 0.004(4) N12 0.042(4) 0.051(5) 0.061(5) 0.004(4) 0.005(4) 0.001(4) C18 0.052(5) 0.081(8) 0.064(7) 0.019(6) 0.020(5) 0.017(6) C19 0.074(7) 0.073(7) 0.058(7) 0.004(6) 0.013(5) 0.012(6) C20 0.095(8) 0.073(8) 0.059(7) 0.002(6) 0.008(6) 0.035(7) C21 0.054(6) 0.090(8) 0.077(8) 0.013(7) 0.019(6) 0.014(6) C22 0.054(5) 0.073(7) 0.048(6) 0.006(5) -0.006(5) 0.009(5) _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 N2 1.757(6) . ? W1 N1 1.751(7) . ? W1 N4 2.156(7) . ? W1 N8 2.160(7) . ? W1 N12 2.376(7) . ? W1 N11 2.399(7) . ? N1 C1 1.442(11) . ? C1 C4 1.463(14) . ? C1 C2 1.506(15) . ? C1 C3 1.510(14) . ? N2 C5 1.421(10) . ? C5 C7 1.494(13) . ? C5 C8 1.527(14) . ? C5 C6 1.542(13) . ? N3 N4 1.317(9) . ? N3 C9 1.327(10) . ? N4 N5 1.315(9) . ? N5 N6 1.320(10) . ? N6 C9 1.303(10) . ? C9 C10 1.441(12) . ? C10 F1 1.249(10) . ? C10 F2 1.349(10) . ? C10 F3 1.374(10) . ? N7 C11 1.291(11) . ? N7 N8 1.299(9) . ? N8 N9 1.290(10) . ? N9 N10 1.337(11) . ? N10 C11 1.309(12) . ? C11 C12 1.354(15) . ? C12 F4 1.248(12) . ? C12 F6 1.264(14) . ? C12 F5 1.259(14) . ? N11 C13 1.321(10) . ? N11 C17 1.359(9) . ? C13 C14 1.426(12) . ? C14 C15 1.379(13) . ? C15 C16 1.307(12) . ? C16 C17 1.354(11) . ? N12 C18 1.327(11) . ? N12 C22 1.344(10) . ? C18 C19 1.372(12) . ? C19 C20 1.361(13) . ? C20 C21 1.380(13) . ? C21 C22 1.362(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 N2 W1 N1 104.5(3) . . ? N2 W1 N4 94.4(3) . . ? N1 W1 N4 93.3(3) . . ? N2 W1 N8 94.2(3) . . ? N1 W1 N8 95.8(3) . . ? N4 W1 N8 165.5(3) . . ? N2 W1 N12 89.6(3) . . ? N1 W1 N12 165.8(3) . . ? N4 W1 N12 86.8(2) . . ? N8 W1 N12 81.5(3) . . ? N2 W1 N11 166.5(3) . . ? N1 W1 N11 88.6(3) . . ? N4 W1 N11 81.5(3) . . ? N8 W1 N11 87.4(3) . . ? N12 W1 N11 77.4(2) . . ? C1 N1 W1 170.7(6) . . ? N1 C1 C4 110.2(9) . . ? N1 C1 C2 108.0(9) . . ? C4 C1 C2 110.9(11) . . ? N1 C1 C3 107.7(8) . . ? C4 C1 C3 113.0(11) . . ? C2 C1 C3 106.9(10) . . ? C5 N2 W1 165.8(7) . . ? N2 C5 C7 108.5(8) . . ? N2 C5 C8 108.4(9) . . ? C7 C5 C8 112.0(10) . . ? N2 C5 C6 108.3(8) . . ? C7 C5 C6 110.3(9) . . ? C8 C5 C6 109.2(11) . . ? N4 N3 C9 103.3(7) . . ? N5 N4 N3 110.6(7) . . ? N5 N4 W1 126.6(6) . . ? N3 N4 W1 122.3(5) . . ? N4 N5 N6 108.0(7) . . ? C9 N6 N5 105.4(7) . . ? N6 C9 N3 112.6(8) . . ? N6 C9 C10 125.0(9) . . ? N3 C9 C10 122.4(8) . . ? F1 C10 F2 108.6(9) . . ? F1 C10 F3 104.7(8) . . ? F2 C10 F3 99.5(8) . . ? F1 C10 C9 119.0(9) . . ? F2 C10 C9 112.8(8) . . ? F3 C10 C9 110.2(8) . . ? C11 N7 N8 105.3(8) . . ? N9 N8 N7 109.4(8) . . ? N9 N8 W1 125.2(7) . . ? N7 N8 W1 124.8(6) . . ? N8 N9 N10 109.5(8) . . ? C11 N10 N9 102.8(9) . . ? N7 C11 N10 112.9(10) . . ? N7 C11 C12 123.3(11) . . ? N10 C11 C12 123.6(10) . . ? F4 C12 F6 102.5(14) . . ? F4 C12 F5 97.9(13) . . ? F6 C12 F5 92.6(14) . . ? F4 C12 C11 123.0(12) . . ? F6 C12 C11 115.6(12) . . ? F5 C12 C11 119.7(13) . . ? C13 N11 C17 116.0(8) . . ? C13 N11 W1 124.4(6) . . ? C17 N11 W1 119.4(6) . . ? N11 C13 C14 123.5(9) . . ? C15 C14 C13 115.0(9) . . ? C16 C15 C14 122.8(10) . . ? C15 C16 C17 118.8(10) . . ? C16 C17 N11 123.9(9) . . ? C18 N12 C22 115.4(8) . . ? C18 N12 W1 124.9(6) . . ? C22 N12 W1 119.6(6) . . ? N12 C18 C19 124.1(9) . . ? C20 C19 C18 119.3(10) . . ? C19 C20 C21 118.2(10) . . ? C22 C21 C20 118.5(9) . . ? N12 C22 C21 124.5(9) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.789 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.130 # Attachment 'Revised Somo1 (7a).cif' data_somo _database_code_depnum_ccdc_archive 'CCDC 287650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Mo N8' _chemical_formula_weight 630.64 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.952(6) _cell_length_b 10.658(4) _cell_length_c 19.851(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.311(8) _cell_angle_gamma 90.00 _cell_volume 3294(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1010 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 25.5 _exptl_crystal_description rhomboid _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8134 _exptl_absorpt_correction_T_max 0.8465 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18681 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7040 _reflns_number_gt 4532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.5940P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7040 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.229505(16) 0.91947(3) 0.292096(13) 0.04969(11) Uani 1 1 d . . . N1 N 0.12013(16) 0.9259(3) 0.27467(14) 0.0557(7) Uani 1 1 d . . . C1 C 0.0452(2) 0.9615(4) 0.28804(19) 0.0668(10) Uani 1 1 d . . . C2 C -0.0331(2) 0.9627(5) 0.2153(2) 0.0892(13) Uani 1 1 d . . . H2A H -0.0234 1.0203 0.1822 0.107 Uiso 1 1 calc R . . H2B H -0.0827 0.9884 0.2236 0.107 Uiso 1 1 calc R . . H2C H -0.0422 0.8800 0.1944 0.107 Uiso 1 1 calc R . . C3 C 0.0352(3) 0.8596(6) 0.3380(2) 0.1142(19) Uani 1 1 d . . . H3A H 0.0278 0.7797 0.3139 0.137 Uiso 1 1 calc R . . H3B H -0.0141 0.8775 0.3488 0.137 Uiso 1 1 calc R . . H3C H 0.0856 0.8574 0.3829 0.137 Uiso 1 1 calc R . . C4 C 0.0577(3) 1.0867(5) 0.3242(3) 0.117(2) Uani 1 1 d . . . H4A H 0.1059 1.0834 0.3706 0.141 Uiso 1 1 calc R . . H4B H 0.0070 1.1092 0.3318 0.141 Uiso 1 1 calc R . . H4C H 0.0683 1.1483 0.2935 0.141 Uiso 1 1 calc R . . N2 N 0.28168(17) 1.0402(3) 0.35095(14) 0.0606(7) Uani 1 1 d . . . C5 C 0.3282(3) 1.1459(4) 0.3943(2) 0.0802(12) Uani 1 1 d . . . C6 C 0.4169(3) 1.1009(6) 0.4448(3) 0.131(2) Uani 1 1 d . . . H6A H 0.4117 1.0385 0.4776 0.157 Uiso 1 1 calc R . . H6B H 0.4498 1.1705 0.4726 0.157 Uiso 1 1 calc R . . H6C H 0.4454 1.0652 0.4160 0.157 Uiso 1 1 calc R . . C7 C 0.3365(6) 1.2395(6) 0.3401(4) 0.214(5) Uani 1 1 d . . . H7A H 0.3554 1.1970 0.3065 0.256 Uiso 1 1 calc R . . H7B H 0.3776 1.3028 0.3661 0.256 Uiso 1 1 calc R . . H7C H 0.2817 1.2780 0.3134 0.256 Uiso 1 1 calc R . . C8 C 0.2841(4) 1.1977(7) 0.4398(4) 0.185(4) Uani 1 1 d . . . H8A H 0.2312 1.2367 0.4085 0.222 Uiso 1 1 calc R . . H8B H 0.3205 1.2589 0.4733 0.222 Uiso 1 1 calc R . . H8C H 0.2723 1.1311 0.4669 0.222 Uiso 1 1 calc R . . N3 N 0.23762(16) 0.9874(3) 0.19486(13) 0.0530(7) Uani 1 1 d . . . N4 N 0.31772(16) 0.9609(3) 0.20325(14) 0.0566(7) Uani 1 1 d . . . N5 N 0.35205(16) 0.8991(3) 0.26373(14) 0.0569(7) Uani 1 1 d . . . C9 C 0.18433(19) 1.0394(3) 0.12586(16) 0.0519(8) Uani 1 1 d . . . C10 C 0.1077(2) 1.0926(3) 0.11884(19) 0.0651(10) Uani 1 1 d . . . H10 H 0.0926 1.0960 0.1590 0.078 Uiso 1 1 calc R . . C11 C 0.0529(2) 1.1411(4) 0.0518(2) 0.0796(11) Uani 1 1 d . . . H11 H 0.0007 1.1762 0.0472 0.095 Uiso 1 1 calc R . . C12 C 0.0745(3) 1.1380(4) -0.0072(2) 0.0818(12) Uani 1 1 d . . . H12 H 0.0379 1.1719 -0.0518 0.098 Uiso 1 1 calc R . . C13 C 0.1505(3) 1.0847(5) -0.0004(2) 0.0928(15) Uani 1 1 d . . . H13 H 0.1651 1.0821 -0.0409 0.111 Uiso 1 1 calc R . . C14 C 0.2063(2) 1.0344(5) 0.06571(19) 0.0793(12) Uani 1 1 d . . . H14 H 0.2577 0.9978 0.0696 0.095 Uiso 1 1 calc R . . C15 C 0.44092(19) 0.8735(4) 0.28740(17) 0.0573(9) Uani 1 1 d . . . C16 C 0.4718(2) 0.7693(4) 0.3310(2) 0.0782(11) Uani 1 1 d . . . H16 H 0.4352 0.7193 0.3440 0.094 Uiso 1 1 calc R . . C17 C 0.5584(3) 0.7399(5) 0.3552(2) 0.0951(14) Uani 1 1 d . . . H17 H 0.5796 0.6689 0.3839 0.114 Uiso 1 1 calc R . . C18 C 0.6121(3) 0.8133(6) 0.3373(3) 0.1012(17) Uani 1 1 d . . . H18 H 0.6700 0.7926 0.3537 0.121 Uiso 1 1 calc R . . C19 C 0.5821(3) 0.9169(5) 0.2957(3) 0.0988(16) Uani 1 1 d . . . H19 H 0.6197 0.9671 0.2839 0.119 Uiso 1 1 calc R . . C20 C 0.4955(2) 0.9496(4) 0.2704(2) 0.0777(11) Uani 1 1 d . . . H20 H 0.4752 1.0217 0.2424 0.093 Uiso 1 1 calc R . . N6 N 0.26908(17) 0.7619(3) 0.36218(14) 0.0600(7) Uani 1 1 d . . . N7 N 0.25429(17) 0.6676(3) 0.31540(16) 0.0599(7) Uani 1 1 d . . . N8 N 0.22039(15) 0.7164(3) 0.25051(14) 0.0546(7) Uani 1 1 d . . . C21 C 0.3140(2) 0.7330(4) 0.43750(19) 0.0731(11) Uani 1 1 d . . . C22 C 0.3658(3) 0.6287(5) 0.4601(2) 0.0968(15) Uani 1 1 d . . . H22 H 0.3712 0.5734 0.4259 0.116 Uiso 1 1 calc R . . C23 C 0.4099(4) 0.6076(8) 0.5348(4) 0.138(3) Uani 1 1 d . . . H23 H 0.4447 0.5371 0.5506 0.166 Uiso 1 1 calc R . . C24 C 0.4030(4) 0.6886(9) 0.5850(3) 0.153(4) Uani 1 1 d . . . H24 H 0.4334 0.6737 0.6348 0.183 Uiso 1 1 calc R . . C25 C 0.3519(4) 0.7915(8) 0.5625(3) 0.134(3) Uani 1 1 d . . . H25 H 0.3472 0.8468 0.5970 0.161 Uiso 1 1 calc R . . C26 C 0.3064(3) 0.8143(5) 0.4879(2) 0.0963(15) Uani 1 1 d . . . H26 H 0.2711 0.8843 0.4725 0.116 Uiso 1 1 calc R . . C27 C 0.19300(18) 0.6341(4) 0.18992(18) 0.0547(8) Uani 1 1 d . . . C28 C 0.2032(2) 0.5055(4) 0.1966(2) 0.0692(10) Uani 1 1 d . . . H28 H 0.2300 0.4688 0.2426 0.083 Uiso 1 1 calc R . . C29 C 0.1730(3) 0.4321(4) 0.1341(3) 0.0834(13) Uani 1 1 d . . . H29 H 0.1796 0.3454 0.1386 0.100 Uiso 1 1 calc R . . C30 C 0.1341(3) 0.4833(6) 0.0664(3) 0.0905(13) Uani 1 1 d . . . H30 H 0.1146 0.4328 0.0248 0.109 Uiso 1 1 calc R . . C31 C 0.1241(3) 0.6092(5) 0.0604(2) 0.0989(15) Uani 1 1 d . . . H31 H 0.0972 0.6450 0.0142 0.119 Uiso 1 1 calc R . . C32 C 0.1530(3) 0.6858(4) 0.1214(2) 0.0784(12) Uani 1 1 d . . . H32 H 0.1454 0.7722 0.1161 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.04891(15) 0.0574(2) 0.04348(15) 0.00332(13) 0.01906(11) 0.00675(12) N1 0.0534(14) 0.067(2) 0.0507(14) 0.0093(13) 0.0252(11) 0.0083(12) C1 0.0505(18) 0.089(3) 0.066(2) -0.003(2) 0.0293(16) 0.0022(17) C2 0.056(2) 0.123(4) 0.083(3) 0.011(3) 0.0220(19) 0.003(2) C3 0.080(3) 0.188(6) 0.089(3) 0.033(4) 0.048(2) 0.004(3) C4 0.082(3) 0.136(5) 0.137(4) -0.050(4) 0.047(3) 0.017(3) N2 0.0675(17) 0.062(2) 0.0522(15) 0.0035(13) 0.0238(13) 0.0058(14) C5 0.072(2) 0.081(3) 0.075(2) -0.019(2) 0.0149(19) -0.004(2) C6 0.077(3) 0.142(5) 0.135(5) -0.019(4) 0.002(3) -0.012(3) C7 0.331(11) 0.089(5) 0.122(5) 0.017(4) -0.017(6) -0.088(6) C8 0.113(4) 0.212(8) 0.218(7) -0.160(7) 0.052(4) -0.028(5) N3 0.0499(13) 0.062(2) 0.0495(14) 0.0064(13) 0.0225(11) 0.0026(12) N4 0.0478(14) 0.071(2) 0.0524(15) -0.0037(13) 0.0209(12) -0.0015(12) N5 0.0469(14) 0.072(2) 0.0503(14) 0.0013(13) 0.0177(11) 0.0062(12) C9 0.0545(17) 0.046(2) 0.0517(17) 0.0051(14) 0.0177(14) -0.0059(13) C10 0.068(2) 0.067(3) 0.0587(19) 0.0077(17) 0.0229(16) 0.0094(17) C11 0.070(2) 0.082(3) 0.073(3) 0.011(2) 0.0140(19) 0.015(2) C12 0.083(3) 0.082(3) 0.060(2) 0.015(2) 0.0062(19) -0.003(2) C13 0.088(3) 0.133(5) 0.055(2) 0.017(2) 0.026(2) -0.014(3) C14 0.060(2) 0.120(4) 0.059(2) 0.012(2) 0.0248(17) -0.001(2) C15 0.0430(16) 0.079(3) 0.0498(17) -0.0111(16) 0.0181(13) 0.0033(15) C16 0.0532(19) 0.097(3) 0.081(2) 0.007(2) 0.0227(18) 0.010(2) C17 0.058(2) 0.119(4) 0.093(3) 0.012(3) 0.014(2) 0.023(2) C18 0.048(2) 0.144(5) 0.100(3) -0.012(3) 0.017(2) 0.019(3) C19 0.052(2) 0.141(5) 0.103(3) -0.014(3) 0.031(2) -0.016(3) C20 0.0533(19) 0.099(3) 0.078(2) -0.001(2) 0.0236(18) -0.0037(19) N6 0.0608(15) 0.067(2) 0.0505(14) 0.0103(14) 0.0203(12) 0.0058(14) N7 0.0529(14) 0.060(2) 0.0655(17) 0.0126(16) 0.0224(13) 0.0042(13) N8 0.0527(14) 0.055(2) 0.0567(15) 0.0060(13) 0.0219(12) 0.0043(12) C21 0.062(2) 0.096(3) 0.055(2) 0.024(2) 0.0164(16) -0.011(2) C22 0.080(3) 0.109(4) 0.087(3) 0.046(3) 0.018(2) 0.004(3) C23 0.092(4) 0.181(7) 0.111(4) 0.093(5) 0.007(3) -0.011(4) C24 0.109(5) 0.253(10) 0.067(3) 0.071(5) 0.003(3) -0.067(5) C25 0.133(5) 0.207(8) 0.051(3) 0.011(3) 0.024(3) -0.056(5) C26 0.096(3) 0.134(5) 0.052(2) 0.008(2) 0.022(2) -0.009(3) C27 0.0445(16) 0.055(2) 0.069(2) -0.0074(17) 0.0279(15) -0.0007(14) C28 0.0526(19) 0.059(3) 0.097(3) -0.001(2) 0.0308(19) 0.0022(16) C29 0.074(2) 0.050(3) 0.135(4) -0.017(3) 0.051(3) -0.0023(19) C30 0.088(3) 0.083(4) 0.100(3) -0.032(3) 0.037(3) -0.005(2) C31 0.116(4) 0.100(5) 0.071(3) -0.013(3) 0.027(3) -0.005(3) C32 0.091(3) 0.073(3) 0.064(2) -0.007(2) 0.022(2) 0.003(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 N2 1.728(3) . ? Mo1 N1 1.748(3) . ? Mo1 N6 2.113(3) . ? Mo1 N3 2.116(3) . ? Mo1 N8 2.300(3) . ? Mo1 N5 2.368(3) . ? N1 C1 1.447(4) . ? C1 C4 1.490(6) . ? C1 C2 1.526(5) . ? C1 C3 1.526(6) . ? N2 C5 1.447(5) . ? C5 C8 1.486(7) . ? C5 C7 1.514(8) . ? C5 C6 1.518(6) . ? N3 N4 1.331(3) . ? N3 C9 1.421(4) . ? N4 N5 1.289(4) . ? N5 C15 1.416(4) . ? C9 C10 1.373(5) . ? C9 C14 1.385(5) . ? C10 C11 1.386(5) . ? C11 C12 1.361(6) . ? C12 C13 1.364(6) . ? C13 C14 1.387(5) . ? C15 C20 1.370(5) . ? C15 C16 1.378(5) . ? C16 C17 1.387(5) . ? C17 C18 1.350(7) . ? C18 C19 1.351(7) . ? C19 C20 1.395(6) . ? N6 N7 1.324(4) . ? N6 C21 1.417(4) . ? N7 N8 1.294(4) . ? N8 C27 1.410(4) . ? C21 C26 1.367(6) . ? C21 C22 1.377(6) . ? C22 C23 1.390(7) . ? C23 C24 1.358(10) . ? C24 C25 1.359(10) . ? C25 C26 1.394(6) . ? C27 C32 1.372(5) . ? C27 C28 1.381(5) . ? C28 C29 1.383(6) . ? C29 C30 1.356(6) . ? C30 C31 1.352(7) . ? C31 C32 1.379(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 N2 Mo1 N1 108.89(13) . . ? N2 Mo1 N6 101.69(13) . . ? N1 Mo1 N6 101.35(11) . . ? N2 Mo1 N3 99.29(12) . . ? N1 Mo1 N3 104.65(11) . . ? N6 Mo1 N3 138.93(11) . . ? N2 Mo1 N8 152.55(11) . . ? N1 Mo1 N8 92.89(11) . . ? N6 Mo1 N8 56.45(10) . . ? N3 Mo1 N8 90.79(11) . . ? N2 Mo1 N5 88.10(12) . . ? N1 Mo1 N5 156.70(11) . . ? N6 Mo1 N5 90.22(10) . . ? N3 Mo1 N5 55.57(9) . . ? N8 Mo1 N5 76.63(10) . . ? C1 N1 Mo1 155.9(2) . . ? N1 C1 C4 110.9(3) . . ? N1 C1 C2 109.0(3) . . ? C4 C1 C2 110.7(4) . . ? N1 C1 C3 105.3(3) . . ? C4 C1 C3 110.8(4) . . ? C2 C1 C3 110.0(4) . . ? C5 N2 Mo1 174.0(3) . . ? N2 C5 C8 111.4(4) . . ? N2 C5 C7 105.8(4) . . ? C8 C5 C7 113.4(6) . . ? N2 C5 C6 108.1(4) . . ? C8 C5 C6 108.7(5) . . ? C7 C5 C6 109.3(5) . . ? N4 N3 C9 115.5(2) . . ? N4 N3 Mo1 104.16(18) . . ? C9 N3 Mo1 140.0(2) . . ? N5 N4 N3 106.7(2) . . ? N4 N5 C15 115.9(3) . . ? N4 N5 Mo1 93.41(17) . . ? C15 N5 Mo1 149.0(2) . . ? C10 C9 C14 119.6(3) . . ? C10 C9 N3 118.3(3) . . ? C14 C9 N3 122.1(3) . . ? C9 C10 C11 120.0(4) . . ? C12 C11 C10 120.7(4) . . ? C11 C12 C13 119.4(4) . . ? C12 C13 C14 121.2(4) . . ? C9 C14 C13 119.1(4) . . ? C20 C15 C16 120.4(3) . . ? C20 C15 N5 122.6(3) . . ? C16 C15 N5 117.0(3) . . ? C15 C16 C17 119.1(4) . . ? C18 C17 C16 120.6(5) . . ? C17 C18 C19 120.3(4) . . ? C18 C19 C20 120.8(4) . . ? C15 C20 C19 118.7(4) . . ? N7 N6 C21 116.6(3) . . ? N7 N6 Mo1 102.65(18) . . ? C21 N6 Mo1 139.9(3) . . ? N8 N7 N6 106.2(3) . . ? N7 N8 C27 117.8(3) . . ? N7 N8 Mo1 94.6(2) . . ? C27 N8 Mo1 147.6(2) . . ? C26 C21 C22 120.4(4) . . ? C26 C21 N6 117.9(4) . . ? C22 C21 N6 121.7(4) . . ? C21 C22 C23 118.8(6) . . ? C24 C23 C22 120.9(7) . . ? C23 C24 C25 120.1(5) . . ? C24 C25 C26 120.1(7) . . ? C21 C26 C25 119.6(6) . . ? C32 C27 C28 119.2(4) . . ? C32 C27 N8 117.6(3) . . ? C28 C27 N8 123.3(3) . . ? C27 C28 C29 119.2(4) . . ? C30 C29 C28 121.6(4) . . ? C31 C30 C29 118.8(4) . . ? C30 C31 C32 121.4(5) . . ? C27 C32 C31 119.8(4) . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.571 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.066 # Attachment 'Revised Orrg1 (7b).cif' data_orrg _database_code_depnum_ccdc_archive 'CCDC 287651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 N8 W' _chemical_formula_weight 718.55 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' W W -0.8490 6.8722 '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 8.674(5) _cell_length_b 10.011(5) _cell_length_c 19.666(11) _cell_angle_alpha 90.598(10) _cell_angle_beta 92.544(9) _cell_angle_gamma 103.321(11) _cell_volume 1659.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 926 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 24.5 _exptl_crystal_description rods _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 3.513 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4738 _exptl_absorpt_correction_T_max 0.5401 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11506 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7521 _reflns_number_gt 5462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^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_number_reflns 7521 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.010 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.36465(3) 0.09153(2) 0.228427(12) 0.05143(10) Uani 1 1 d . . . N1 N 0.5820(6) 0.1366(5) 0.3040(2) 0.0549(12) Uani 1 1 d . . . N2 N 0.6602(6) 0.2380(5) 0.2699(3) 0.0574(12) Uani 1 1 d . . . N3 N 0.5715(6) 0.2450(5) 0.2138(2) 0.0577(12) Uani 1 1 d . . . C1 C 0.6489(7) 0.1084(6) 0.3674(3) 0.0519(13) Uani 1 1 d . . . C2 C 0.5854(8) -0.0123(7) 0.3967(4) 0.0683(17) Uani 1 1 d . . . H2 H 0.5007 -0.0737 0.3746 0.082 Uiso 1 1 calc R . . C3 C 0.6446(9) -0.0451(8) 0.4585(4) 0.078(2) Uani 1 1 d . . . H3 H 0.6003 -0.1285 0.4781 0.094 Uiso 1 1 calc R . . C4 C 0.7675(9) 0.0437(8) 0.4909(4) 0.0756(19) Uani 1 1 d . . . H4 H 0.8080 0.0211 0.5327 0.091 Uiso 1 1 calc R . . C5 C 0.8323(10) 0.1664(8) 0.4627(4) 0.086(2) Uani 1 1 d . . . H5 H 0.9164 0.2272 0.4855 0.103 Uiso 1 1 calc R . . C6 C 0.7747(9) 0.2011(7) 0.4008(4) 0.078(2) Uani 1 1 d . . . H6 H 0.8189 0.2849 0.3815 0.094 Uiso 1 1 calc R . . C7 C 0.6331(7) 0.3507(6) 0.1683(3) 0.0560(14) Uani 1 1 d . . . C8 C 0.5841(10) 0.3328(8) 0.1009(3) 0.077(2) Uani 1 1 d . . . H8 H 0.5095 0.2544 0.0859 0.092 Uiso 1 1 calc R . . C9 C 0.6473(13) 0.4334(10) 0.0552(4) 0.104(3) Uani 1 1 d . . . H9 H 0.6147 0.4232 0.0094 0.125 Uiso 1 1 calc R . . C10 C 0.7571(14) 0.5470(10) 0.0777(6) 0.112(3) Uani 1 1 d . . . H10 H 0.7989 0.6138 0.0468 0.134 Uiso 1 1 calc R . . C11 C 0.8062(11) 0.5647(9) 0.1430(6) 0.102(3) Uani 1 1 d . . . H11 H 0.8826 0.6422 0.1576 0.122 Uiso 1 1 calc R . . C12 C 0.7411(9) 0.4655(7) 0.1890(4) 0.078(2) Uani 1 1 d . . . H12 H 0.7725 0.4783 0.2349 0.094 Uiso 1 1 calc R . . N4 N 0.2153(6) 0.0041(5) 0.3055(2) 0.0550(12) Uani 1 1 d . . . N5 N 0.2086(6) 0.1100(5) 0.3468(3) 0.0557(12) Uani 1 1 d . . . N6 N 0.3015(6) 0.2159(5) 0.3217(2) 0.0549(12) Uani 1 1 d . . . C13 C 0.1118(7) -0.1212(5) 0.3211(3) 0.0521(13) Uani 1 1 d . . . C14 C -0.0279(8) -0.1272(7) 0.3543(4) 0.0724(18) Uani 1 1 d . . . H14 H -0.0588 -0.0469 0.3653 0.087 Uiso 1 1 calc R . . C15 C -0.1188(9) -0.2513(8) 0.3704(4) 0.083(2) Uani 1 1 d . . . H15 H -0.2123 -0.2539 0.3922 0.100 Uiso 1 1 calc R . . C16 C -0.0806(11) -0.3684(9) 0.3565(4) 0.090(2) Uani 1 1 d . . . H16 H -0.1452 -0.4509 0.3695 0.108 Uiso 1 1 calc R . . C17 C 0.0549(10) -0.3686(7) 0.3227(4) 0.082(2) Uani 1 1 d . . . H17 H 0.0825 -0.4504 0.3118 0.098 Uiso 1 1 calc R . . C18 C 0.1497(9) -0.2420(7) 0.3052(4) 0.0718(18) Uani 1 1 d . . . H18 H 0.2413 -0.2403 0.2821 0.086 Uiso 1 1 calc R . . C19 C 0.3246(8) 0.3400(6) 0.3609(3) 0.0578(15) Uani 1 1 d . . . C20 C 0.4161(8) 0.4563(6) 0.3337(4) 0.0734(19) Uani 1 1 d . . . H20 H 0.4617 0.4512 0.2921 0.088 Uiso 1 1 calc R . . C21 C 0.4400(9) 0.5811(7) 0.3686(5) 0.089(2) Uani 1 1 d . . . H21 H 0.5010 0.6599 0.3501 0.107 Uiso 1 1 calc R . . C22 C 0.3752(11) 0.5889(8) 0.4294(5) 0.096(3) Uani 1 1 d . . . H22 H 0.3946 0.6725 0.4531 0.115 Uiso 1 1 calc R . . C23 C 0.2808(13) 0.4743(8) 0.4563(4) 0.104(3) Uani 1 1 d . . . H23 H 0.2323 0.4814 0.4969 0.125 Uiso 1 1 calc R . . C24 C 0.2575(10) 0.3475(7) 0.4227(4) 0.080(2) Uani 1 1 d . . . H24 H 0.1976 0.2689 0.4418 0.096 Uiso 1 1 calc R . . N7 N 0.2264(6) 0.1491(5) 0.1757(3) 0.0613(13) Uani 1 1 d . . . C25 C 0.1052(10) 0.1960(9) 0.1365(4) 0.087(2) Uani 1 1 d . . . C26 C 0.0975(17) 0.1401(14) 0.0655(6) 0.167(6) Uani 1 1 d . . . H26A H 0.2020 0.1597 0.0483 0.200 Uiso 1 1 calc R . . H26B H 0.0297 0.1822 0.0372 0.200 Uiso 1 1 calc R . . H26C H 0.0556 0.0426 0.0652 0.200 Uiso 1 1 calc R . . C27 C 0.1451(15) 0.3511(10) 0.1377(7) 0.158(5) Uani 1 1 d . . . H27A H 0.1438 0.3844 0.1835 0.189 Uiso 1 1 calc R . . H27B H 0.0681 0.3829 0.1095 0.189 Uiso 1 1 calc R . . H27C H 0.2486 0.3844 0.1206 0.189 Uiso 1 1 calc R . . C28 C -0.0459(12) 0.1446(15) 0.1702(8) 0.173(6) Uani 1 1 d . . . H28A H -0.0624 0.0473 0.1761 0.207 Uiso 1 1 calc R . . H28B H -0.1319 0.1635 0.1424 0.207 Uiso 1 1 calc R . . H28C H -0.0412 0.1896 0.2138 0.207 Uiso 1 1 calc R . . N8 N 0.4081(6) -0.0544(5) 0.1900(3) 0.0596(13) Uani 1 1 d . . . C29 C 0.4074(10) -0.1589(8) 0.1385(4) 0.078(2) Uani 1 1 d . . . C30 C 0.5212(18) -0.0950(11) 0.0878(6) 0.178(7) Uani 1 1 d . . . H30A H 0.4926 -0.0139 0.0709 0.213 Uiso 1 1 calc R . . H30B H 0.5188 -0.1588 0.0508 0.213 Uiso 1 1 calc R . . H30C H 0.6261 -0.0707 0.1089 0.213 Uiso 1 1 calc R . . C31 C 0.2479(15) -0.2041(16) 0.1051(8) 0.239(11) Uani 1 1 d . . . H31A H 0.2102 -0.1252 0.0911 0.287 Uiso 1 1 calc R . . H31B H 0.1768 -0.2555 0.1365 0.287 Uiso 1 1 calc R . . H31C H 0.2529 -0.2608 0.0660 0.287 Uiso 1 1 calc R . . C32 C 0.465(2) -0.2735(12) 0.1699(7) 0.186(7) Uani 1 1 d . . . H32A H 0.5606 -0.2371 0.1972 0.223 Uiso 1 1 calc R . . H32B H 0.4872 -0.3328 0.1347 0.223 Uiso 1 1 calc R . . H32C H 0.3858 -0.3246 0.1980 0.223 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05658(16) 0.05090(14) 0.04395(15) -0.00359(9) 0.00196(10) 0.00683(10) N1 0.063(3) 0.047(3) 0.051(3) 0.001(2) -0.003(2) 0.004(2) N2 0.059(3) 0.060(3) 0.052(3) 0.001(2) 0.006(2) 0.012(2) N3 0.067(3) 0.061(3) 0.041(3) 0.001(2) 0.002(2) 0.005(2) C1 0.057(3) 0.052(3) 0.047(3) -0.001(3) -0.001(3) 0.014(3) C2 0.071(4) 0.068(4) 0.063(4) 0.005(3) -0.004(3) 0.012(3) C3 0.085(5) 0.080(5) 0.066(5) 0.011(4) 0.003(4) 0.014(4) C4 0.083(5) 0.096(5) 0.048(4) 0.005(4) -0.004(3) 0.022(4) C5 0.105(6) 0.087(5) 0.054(4) -0.013(4) -0.021(4) 0.006(4) C6 0.091(5) 0.062(4) 0.073(5) -0.001(3) -0.011(4) 0.003(4) C7 0.060(4) 0.056(3) 0.054(4) 0.007(3) 0.011(3) 0.016(3) C8 0.103(6) 0.075(4) 0.050(4) 0.007(3) 0.007(4) 0.016(4) C9 0.160(9) 0.092(6) 0.065(5) 0.024(5) 0.023(6) 0.035(6) C10 0.142(9) 0.088(6) 0.110(8) 0.053(6) 0.044(7) 0.027(6) C11 0.090(6) 0.095(6) 0.114(8) 0.036(6) 0.017(6) 0.005(5) C12 0.069(5) 0.073(4) 0.085(5) 0.016(4) 0.001(4) 0.002(4) N4 0.064(3) 0.049(3) 0.049(3) -0.006(2) 0.004(2) 0.007(2) N5 0.062(3) 0.048(3) 0.055(3) -0.001(2) 0.007(2) 0.007(2) N6 0.065(3) 0.044(2) 0.052(3) -0.007(2) 0.005(2) 0.007(2) C13 0.056(3) 0.047(3) 0.048(3) -0.006(2) -0.004(3) 0.003(3) C14 0.066(4) 0.064(4) 0.084(5) -0.011(3) 0.012(4) 0.005(3) C15 0.060(4) 0.069(4) 0.105(6) -0.018(4) 0.011(4) -0.017(4) C16 0.097(6) 0.082(5) 0.075(5) -0.011(4) 0.013(5) -0.016(4) C17 0.086(5) 0.054(4) 0.102(6) -0.004(4) 0.005(5) 0.009(4) C18 0.072(4) 0.058(4) 0.084(5) -0.004(3) 0.015(4) 0.010(3) C19 0.066(4) 0.051(3) 0.056(4) -0.007(3) -0.008(3) 0.016(3) C20 0.063(4) 0.050(3) 0.103(6) -0.008(3) 0.009(4) 0.002(3) C21 0.076(5) 0.055(4) 0.130(8) -0.014(4) 0.009(5) 0.003(3) C22 0.117(7) 0.063(5) 0.101(7) -0.023(4) -0.009(6) 0.011(5) C23 0.160(9) 0.077(5) 0.074(5) -0.018(4) 0.024(6) 0.023(6) C24 0.117(6) 0.058(4) 0.061(4) -0.004(3) 0.013(4) 0.009(4) N7 0.055(3) 0.072(3) 0.054(3) 0.001(3) 0.001(2) 0.008(3) C25 0.084(6) 0.093(6) 0.085(6) 0.001(4) -0.017(4) 0.027(4) C26 0.196(13) 0.188(13) 0.120(10) -0.011(9) -0.075(9) 0.070(11) C27 0.180(12) 0.099(7) 0.206(14) 0.010(8) -0.050(10) 0.068(8) C28 0.076(7) 0.241(15) 0.209(15) 0.086(12) 0.003(8) 0.049(8) N8 0.064(3) 0.056(3) 0.058(3) -0.010(2) 0.011(3) 0.012(2) C29 0.093(5) 0.070(4) 0.071(5) -0.019(4) 0.019(4) 0.016(4) C30 0.276(17) 0.116(8) 0.117(9) -0.052(7) 0.116(11) -0.022(9) C31 0.138(11) 0.273(18) 0.29(2) -0.240(18) -0.061(12) 0.047(11) C32 0.32(2) 0.127(9) 0.152(12) 0.009(8) 0.092(13) 0.121(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N7 1.751(5) . ? W1 N8 1.761(5) . ? W1 N4 2.103(5) . ? W1 N3 2.109(5) . ? W1 N1 2.304(5) . ? W1 N6 2.360(5) . ? N1 N2 1.295(6) . ? N1 C1 1.412(7) . ? N2 N3 1.328(7) . ? N3 C7 1.417(7) . ? C1 C2 1.352(9) . ? C1 C6 1.392(9) . ? C2 C3 1.371(10) . ? C3 C4 1.350(10) . ? C4 C5 1.362(10) . ? C5 C6 1.374(10) . ? C7 C12 1.351(9) . ? C7 C8 1.371(9) . ? C8 C9 1.389(10) . ? C9 C10 1.359(13) . ? C10 C11 1.332(14) . ? C11 C12 1.389(11) . ? N4 N5 1.341(6) . ? N4 C13 1.410(7) . ? N5 N6 1.293(6) . ? N6 C19 1.424(7) . ? C13 C18 1.361(8) . ? C13 C14 1.390(9) . ? C14 C15 1.358(9) . ? C15 C16 1.319(11) . ? C16 C17 1.375(11) . ? C17 C18 1.398(9) . ? C19 C20 1.377(9) . ? C19 C24 1.380(9) . ? C20 C21 1.388(10) . ? C21 C22 1.353(12) . ? C22 C23 1.373(12) . ? C23 C24 1.393(10) . ? N7 C25 1.442(9) . ? C25 C28 1.481(13) . ? C25 C26 1.493(14) . ? C25 C27 1.510(12) . ? N8 C29 1.448(8) . ? C29 C31 1.475(13) . ? C29 C32 1.484(13) . ? C29 C30 1.479(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 N7 W1 N8 108.9(3) . . ? N7 W1 N4 99.2(2) . . ? N8 W1 N4 102.0(2) . . ? N7 W1 N3 100.9(2) . . ? N8 W1 N3 102.6(2) . . ? N4 W1 N3 141.03(19) . . ? N7 W1 N1 150.3(2) . . ? N8 W1 N1 95.8(2) . . ? N4 W1 N1 91.23(19) . . ? N3 W1 N1 56.54(18) . . ? N7 W1 N6 90.5(2) . . ? N8 W1 N6 153.4(2) . . ? N4 W1 N6 55.65(17) . . ? N3 W1 N6 91.10(18) . . ? N1 W1 N6 72.64(18) . . ? N2 N1 C1 117.9(5) . . ? N2 N1 W1 94.4(3) . . ? C1 N1 W1 147.3(4) . . ? N1 N2 N3 106.2(5) . . ? N2 N3 C7 116.5(5) . . ? N2 N3 W1 102.7(3) . . ? C7 N3 W1 140.6(4) . . ? C2 C1 C6 119.7(6) . . ? C2 C1 N1 118.1(6) . . ? C6 C1 N1 122.2(6) . . ? C1 C2 C3 120.8(7) . . ? C4 C3 C2 119.9(7) . . ? C3 C4 C5 120.3(7) . . ? C4 C5 C6 120.6(7) . . ? C5 C6 C1 118.7(7) . . ? C12 C7 C8 119.5(6) . . ? C12 C7 N3 122.0(6) . . ? C8 C7 N3 118.4(6) . . ? C7 C8 C9 119.1(8) . . ? C10 C9 C8 119.8(9) . . ? C11 C10 C9 121.5(8) . . ? C10 C11 C12 118.8(9) . . ? C7 C12 C11 121.2(8) . . ? N5 N4 C13 114.5(5) . . ? N5 N4 W1 104.9(3) . . ? C13 N4 W1 140.0(4) . . ? N6 N5 N4 105.4(4) . . ? N5 N6 C19 115.5(5) . . ? N5 N6 W1 94.0(3) . . ? C19 N6 W1 150.3(4) . . ? C18 C13 C14 117.7(6) . . ? C18 C13 N4 119.8(6) . . ? C14 C13 N4 122.5(5) . . ? C15 C14 C13 119.4(7) . . ? C16 C15 C14 123.1(8) . . ? C15 C16 C17 120.0(8) . . ? C16 C17 C18 117.9(7) . . ? C13 C18 C17 121.9(7) . . ? C20 C19 C24 120.1(6) . . ? C20 C19 N6 116.9(6) . . ? C24 C19 N6 123.0(6) . . ? C19 C20 C21 119.7(7) . . ? C22 C21 C20 120.4(8) . . ? C21 C22 C23 120.4(7) . . ? C22 C23 C24 120.1(8) . . ? C19 C24 C23 119.2(7) . . ? C25 N7 W1 175.8(5) . . ? N7 C25 C28 106.9(7) . . ? N7 C25 C26 108.7(8) . . ? C28 C25 C26 111.4(10) . . ? N7 C25 C27 109.1(7) . . ? C28 C25 C27 109.5(9) . . ? C26 C25 C27 111.0(9) . . ? C29 N8 W1 158.6(5) . . ? N8 C29 C31 110.2(7) . . ? N8 C29 C32 109.3(8) . . ? C31 C29 C32 112.8(11) . . ? N8 C29 C30 106.6(6) . . ? C31 C29 C30 109.5(11) . . ? C32 C29 C30 108.2(9) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 2.219 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.116