data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hung Kay Lee' _publ_contact_author_email HKLEE@CUHK.EDU.HK _publ_section_title ; New Dioxo-Molybdenum(VI) and -Tungsten(VI) Complexes with N-capped Tripodal N2O2 Tetradentate Ligands: Synthesis, Structures and Catalytic Activities towards Olefin Epoxidation ; loop_ _publ_author_name 'Hung Kay Lee.' 'Jonathan Dilworth' 'Dennis Ng' 'Lok Tong.' 'Yee-Lok Wong.' # Attachment 'Wong_et_al.cif' data_Ylwmo1 _database_code_depnum_ccdc_archive 'CCDC 759487' #TrackingRef 'Wong_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Mo N2 O4' _chemical_formula_weight 558.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5617(17) _cell_length_b 14.180(3) _cell_length_c 25.984(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00 _cell_volume 3154.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 1.426 _exptl_absorpt_process_details 'ABSCOR program, Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IIC imaging plate' _diffrn_measurement_method 'phi oscillation method' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6273 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4078 _reflns_number_gt 3218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS-IIC Rigaku' _computing_cell_refinement 'BioteX software MSC 1995' _computing_data_reduction 'BioteX software MSC 1995' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL Vers. 6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+13.4749P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0112(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4078 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2454 _refine_ls_wR_factor_gt 0.2327 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.003 _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 -0.00442(9) 0.81116(7) 0.23690(4) 0.0750(5) Uani 1 1 d . . . N1 N 0.0350(9) 0.9616(6) 0.2713(3) 0.080(2) Uani 1 1 d . . . N2 N -0.2500(9) 0.8838(6) 0.2542(3) 0.073(2) Uani 1 1 d . . . O1 O -0.0490(7) 0.7837(5) 0.3092(3) 0.0726(18) Uani 1 1 d . . . O2 O -0.0258(7) 0.8802(5) 0.1713(3) 0.081(2) Uani 1 1 d . . . O3 O -0.0788(8) 0.7087(5) 0.2142(3) 0.087(2) Uani 1 1 d . . . O4 O 0.1929(7) 0.8025(5) 0.2368(3) 0.084(2) Uani 1 1 d . . . C1 C -0.1705(11) 0.7315(8) 0.3300(4) 0.075(3) Uani 1 1 d . . . C2 C -0.3224(11) 0.7428(8) 0.3104(4) 0.076(3) Uani 1 1 d . . . C3 C -0.4416(12) 0.6905(10) 0.3319(5) 0.102(4) Uani 1 1 d . . . H3B H -0.5435 0.7001 0.3208 0.122 Uiso 1 1 calc R . . C4 C -0.4130(15) 0.6241(11) 0.3697(6) 0.109(4) Uani 1 1 d . . . H4B H -0.4916 0.5834 0.3805 0.131 Uiso 1 1 calc R . . C5 C -0.2675(12) 0.6194(9) 0.3907(5) 0.091(3) Uani 1 1 d . . . H5A H -0.2518 0.5799 0.4188 0.109 Uiso 1 1 calc R . . C6 C -0.1407(11) 0.6712(8) 0.3720(4) 0.077(3) Uani 1 1 d . . . C7 C 0.0212(12) 0.6629(8) 0.3951(5) 0.085(3) Uani 1 1 d . . . C8 C 0.1348(13) 0.6228(11) 0.3536(6) 0.118(5) Uani 1 1 d . . . H8A H 0.1383 0.6649 0.3247 0.178 Uiso 1 1 calc R . . H8B H 0.0987 0.5620 0.3425 0.178 Uiso 1 1 calc R . . H8C H 0.2375 0.6169 0.3681 0.178 Uiso 1 1 calc R . . C9 C 0.0782(19) 0.7597(10) 0.4127(6) 0.141(6) Uani 1 1 d . . . H9A H 0.0752 0.8029 0.3843 0.211 Uiso 1 1 calc R . . H9B H 0.1834 0.7545 0.4252 0.211 Uiso 1 1 calc R . . H9C H 0.0119 0.7824 0.4398 0.211 Uiso 1 1 calc R . . C10 C 0.0234(15) 0.5917(11) 0.4415(5) 0.116(5) Uani 1 1 d . . . H10A H -0.0447 0.6142 0.4682 0.175 Uiso 1 1 calc R . . H10B H 0.1278 0.5867 0.4547 0.175 Uiso 1 1 calc R . . H10C H -0.0114 0.5309 0.4300 0.175 Uiso 1 1 calc R . . C11 C -0.1510(12) 0.8619(8) 0.1389(5) 0.081(3) Uani 1 1 d . . . C12 C -0.1288(12) 0.8247(8) 0.0898(5) 0.085(3) Uani 1 1 d . . . C13 C -0.2654(15) 0.8037(10) 0.0639(5) 0.104(4) Uani 1 1 d . . . H13A H -0.2582 0.7761 0.0315 0.125 Uiso 1 1 calc R . . C14 C -0.4139(15) 0.8219(10) 0.0840(7) 0.111(4) Uani 1 1 d . . . H14A H -0.5021 0.8058 0.0650 0.133 Uiso 1 1 calc R . . C15 C -0.4308(12) 0.8632(9) 0.1312(5) 0.092(3) Uani 1 1 d . . . H15A H -0.5294 0.8752 0.1448 0.110 Uiso 1 1 calc R . . C16 C -0.2957(12) 0.8870(9) 0.1587(5) 0.084(3) Uani 1 1 d . . . C17 C 0.0341(13) 0.8046(9) 0.0656(5) 0.092(3) Uani 1 1 d . . . C18 C 0.1261(15) 0.7358(10) 0.0961(6) 0.116(4) Uani 1 1 d . . . H18A H 0.0732 0.6761 0.0964 0.173 Uiso 1 1 calc R . . H18B H 0.1371 0.7585 0.1307 0.173 Uiso 1 1 calc R . . H18C H 0.2276 0.7284 0.0809 0.173 Uiso 1 1 calc R . . C19 C 0.0258(17) 0.7732(12) 0.0098(6) 0.133(5) Uani 1 1 d . . . H19A H -0.0245 0.7128 0.0078 0.199 Uiso 1 1 calc R . . H19B H 0.1295 0.7685 -0.0040 0.199 Uiso 1 1 calc R . . H19C H -0.0329 0.8184 -0.0098 0.199 Uiso 1 1 calc R . . C20 C 0.1217(15) 0.9030(10) 0.0646(6) 0.122(5) Uani 1 1 d . . . H20A H 0.2238 0.8950 0.0499 0.183 Uiso 1 1 calc R . . H20B H 0.1314 0.9266 0.0991 0.183 Uiso 1 1 calc R . . H20C H 0.0631 0.9470 0.0442 0.183 Uiso 1 1 calc R . . C21 C -0.0849(12) 1.0068(8) 0.2953(5) 0.080(3) Uani 1 1 d . . . C22 C -0.0704(14) 1.0939(10) 0.3189(5) 0.104(4) Uani 1 1 d . . . H22A H -0.1542 1.1227 0.3354 0.125 Uiso 1 1 calc R . . C23 C 0.0762(15) 1.1361(11) 0.3167(6) 0.111(4) Uani 1 1 d . . . H23A H 0.0925 1.1946 0.3319 0.134 Uiso 1 1 calc R . . C24 C 0.1983(14) 1.0903(9) 0.2917(5) 0.101(4) Uani 1 1 d . . . H24A H 0.2971 1.1175 0.2910 0.121 Uiso 1 1 calc R . . C25 C 0.1732(12) 1.0071(7) 0.2688(5) 0.081(3) Uani 1 1 d . . . H25A H 0.2544 0.9795 0.2504 0.097 Uiso 1 1 calc R . . C26 C -0.3628(11) 0.8074(8) 0.2660(5) 0.086(3) Uani 1 1 d . . . H26A H -0.3752 0.7691 0.2354 0.103 Uiso 1 1 calc R . . H26B H -0.4633 0.8362 0.2732 0.103 Uiso 1 1 calc R . . C27 C -0.3053(11) 0.9387(9) 0.2083(5) 0.090(3) Uani 1 1 d . . . H27A H -0.4130 0.9572 0.2140 0.108 Uiso 1 1 calc R . . H27B H -0.2436 0.9958 0.2056 0.108 Uiso 1 1 calc R . . C28 C -0.2362(13) 0.9519(9) 0.2978(5) 0.097(4) Uani 1 1 d . . . H28A H -0.2409 0.9177 0.3301 0.116 Uiso 1 1 calc R . . H28B H -0.3234 0.9955 0.2969 0.116 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 0.0504(5) 0.0785(7) 0.0961(8) 0.0013(6) -0.0012(4) -0.0009(4) N1 0.064(5) 0.083(6) 0.093(7) -0.005(5) 0.000(4) -0.001(4) N2 0.055(4) 0.090(6) 0.075(6) 0.004(5) -0.001(4) -0.003(4) O1 0.058(4) 0.078(4) 0.082(5) 0.010(4) 0.001(3) -0.012(3) O2 0.054(4) 0.085(5) 0.103(6) 0.007(4) -0.005(3) -0.005(3) O3 0.067(4) 0.081(5) 0.114(6) -0.007(4) -0.004(4) -0.017(4) O4 0.056(4) 0.102(5) 0.093(5) 0.003(4) -0.006(3) 0.020(4) C1 0.052(5) 0.082(7) 0.091(8) 0.005(6) 0.003(5) 0.006(5) C2 0.056(6) 0.077(7) 0.094(8) -0.009(6) 0.002(5) 0.006(5) C3 0.057(6) 0.129(11) 0.119(11) 0.001(9) 0.002(6) 0.006(7) C4 0.083(8) 0.123(11) 0.122(11) 0.030(9) 0.019(7) -0.029(7) C5 0.065(7) 0.102(9) 0.106(9) 0.008(7) 0.010(6) 0.004(6) C6 0.057(6) 0.080(7) 0.094(8) -0.006(6) 0.000(5) -0.007(5) C7 0.073(7) 0.080(8) 0.103(9) -0.004(6) -0.013(6) 0.002(5) C8 0.073(7) 0.132(12) 0.150(13) 0.051(10) 0.006(8) 0.006(7) C9 0.159(14) 0.113(11) 0.150(14) -0.007(10) -0.079(12) -0.017(10) C10 0.110(10) 0.141(12) 0.098(10) 0.027(9) -0.017(7) 0.013(9) C11 0.065(6) 0.084(8) 0.093(9) 0.005(6) -0.011(6) -0.005(5) C12 0.074(7) 0.091(8) 0.088(8) 0.005(7) -0.009(6) -0.009(6) C13 0.091(9) 0.124(11) 0.097(9) 0.000(8) -0.012(7) -0.006(8) C14 0.080(8) 0.126(11) 0.128(13) 0.015(10) -0.025(8) -0.004(8) C15 0.064(7) 0.114(10) 0.098(10) 0.019(8) -0.009(6) -0.001(6) C16 0.062(6) 0.101(8) 0.090(8) 0.008(7) -0.002(6) -0.004(6) C17 0.081(7) 0.104(9) 0.091(9) -0.003(7) 0.003(6) -0.007(7) C18 0.096(9) 0.115(11) 0.136(12) 0.004(9) 0.006(8) 0.026(8) C19 0.119(11) 0.168(15) 0.111(12) -0.013(11) 0.025(9) 0.004(10) C20 0.106(10) 0.122(12) 0.138(13) 0.003(10) 0.018(8) -0.008(9) C21 0.067(6) 0.073(7) 0.101(9) 0.005(6) -0.001(6) 0.000(6) C22 0.083(8) 0.126(12) 0.104(10) 0.006(9) -0.003(7) 0.024(8) C23 0.084(9) 0.102(10) 0.148(13) -0.013(9) -0.022(8) -0.009(8) C24 0.079(8) 0.088(9) 0.137(12) -0.003(8) -0.022(7) 0.002(7) C25 0.066(6) 0.062(6) 0.113(9) -0.002(6) 0.003(6) -0.009(5) C26 0.051(5) 0.089(8) 0.117(9) 0.013(7) -0.008(5) -0.016(5) C27 0.057(6) 0.095(8) 0.117(10) 0.018(8) -0.005(6) 0.005(5) C28 0.072(7) 0.122(10) 0.097(9) -0.002(8) 0.008(6) 0.016(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 Mo1 O3 1.693(7) . ? Mo1 O4 1.694(6) . ? Mo1 O1 1.956(7) . ? Mo1 O2 1.974(7) . ? Mo1 N1 2.337(9) . ? Mo1 N2 2.384(8) . ? N1 C25 1.349(12) . ? N1 C21 1.361(13) . ? N2 C26 1.483(12) . ? N2 C28 1.495(14) . ? N2 C27 1.500(13) . ? O1 C1 1.386(12) . ? O2 C11 1.387(12) . ? C1 C2 1.406(13) . ? C1 C6 1.409(15) . ? C2 C3 1.380(16) . ? C2 C26 1.513(15) . ? C3 C4 1.380(17) . ? C4 C5 1.362(15) . ? C5 C6 1.398(14) . ? C6 C7 1.514(14) . ? C7 C9 1.527(17) . ? C7 C8 1.559(18) . ? C7 C10 1.573(16) . ? C11 C16 1.388(15) . ? C11 C12 1.393(16) . ? C12 C13 1.382(15) . ? C12 C17 1.557(16) . ? C13 C14 1.399(18) . ? C14 C15 1.368(18) . ? C15 C16 1.401(15) . ? C16 C27 1.485(16) . ? C17 C18 1.484(16) . ? C17 C19 1.519(18) . ? C17 C20 1.584(17) . ? C21 C22 1.386(17) . ? C21 C28 1.513(15) . ? C22 C23 1.391(17) . ? C23 C24 1.391(17) . ? C24 C25 1.339(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo1 O4 108.2(4) . . ? O3 Mo1 O1 95.2(3) . . ? O4 Mo1 O1 100.5(3) . . ? O3 Mo1 O2 95.1(3) . . ? O4 Mo1 O2 97.3(3) . . ? O1 Mo1 O2 155.5(3) . . ? O3 Mo1 N1 166.2(3) . . ? O4 Mo1 N1 85.6(3) . . ? O1 Mo1 N1 80.9(3) . . ? O2 Mo1 N1 83.8(3) . . ? O3 Mo1 N2 96.0(3) . . ? O4 Mo1 N2 155.7(3) . . ? O1 Mo1 N2 74.5(3) . . ? O2 Mo1 N2 82.3(3) . . ? N1 Mo1 N2 70.2(3) . . ? C25 N1 C21 117.3(10) . . ? C25 N1 Mo1 123.0(7) . . ? C21 N1 Mo1 119.7(7) . . ? C26 N2 C28 111.4(9) . . ? C26 N2 C27 109.8(8) . . ? C28 N2 C27 107.1(9) . . ? C26 N2 Mo1 107.3(6) . . ? C28 N2 Mo1 110.6(6) . . ? C27 N2 Mo1 110.7(6) . . ? C1 O1 Mo1 128.8(6) . . ? C11 O2 Mo1 120.2(6) . . ? O1 C1 C2 119.5(10) . . ? O1 C1 C6 119.4(8) . . ? C2 C1 C6 121.1(10) . . ? C3 C2 C1 118.4(11) . . ? C3 C2 C26 117.8(9) . . ? C1 C2 C26 123.8(9) . . ? C2 C3 C4 121.6(10) . . ? C5 C4 C3 118.7(11) . . ? C4 C5 C6 123.0(12) . . ? C5 C6 C1 116.6(10) . . ? C5 C6 C7 122.1(11) . . ? C1 C6 C7 121.3(9) . . ? C6 C7 C9 110.0(10) . . ? C6 C7 C8 109.0(10) . . ? C9 C7 C8 109.6(11) . . ? C6 C7 C10 111.4(10) . . ? C9 C7 C10 110.0(11) . . ? C8 C7 C10 106.8(10) . . ? O2 C11 C16 114.6(11) . . ? O2 C11 C12 121.4(10) . . ? C16 C11 C12 123.9(10) . . ? C13 C12 C11 114.4(11) . . ? C13 C12 C17 121.4(12) . . ? C11 C12 C17 124.2(10) . . ? C12 C13 C14 123.1(14) . . ? C15 C14 C13 120.7(12) . . ? C14 C15 C16 118.2(12) . . ? C11 C16 C15 119.1(12) . . ? C11 C16 C27 119.9(10) . . ? C15 C16 C27 121.0(11) . . ? C18 C17 C19 110.0(12) . . ? C18 C17 C12 112.3(11) . . ? C19 C17 C12 113.5(10) . . ? C18 C17 C20 109.6(11) . . ? C19 C17 C20 105.4(12) . . ? C12 C17 C20 105.7(10) . . ? N1 C21 C22 123.7(10) . . ? N1 C21 C28 115.1(10) . . ? C22 C21 C28 121.1(11) . . ? C21 C22 C23 116.4(12) . . ? C22 C23 C24 119.8(13) . . ? C25 C24 C23 119.9(12) . . ? C24 C25 N1 122.7(11) . . ? N2 C26 C2 116.9(8) . . ? C16 C27 N2 114.6(10) . . ? N2 C28 C21 111.5(9) . . ? _diffrn_measured_fraction_theta_max 0.735 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.735 _refine_diff_density_max 0.620 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.092 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.020 0.000 0.500 341.1 7.4 2 -0.025 0.500 0.000 341.1 6.4 _platon_squeeze_details ; ; #===END data_YLWW01 _database_code_depnum_ccdc_archive 'CCDC 759488' #TrackingRef 'Wong_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 N2 O4 W' _chemical_formula_weight 646.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.257(4) _cell_length_b 12.703(3) _cell_length_c 20.780(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5347.2(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 4.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 1.194 _exptl_absorpt_process_details 'ABSCOR program, Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IIC imaging plate' _diffrn_measurement_method 'phi oscillation method' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12458 _diffrn_reflns_av_R_equivalents 0.1555 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4113 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS-IIC RIGAKU' _computing_cell_refinement 'BioteX software MSC 1995' _computing_data_reduction 'BioteX software MSC 1995' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL Vers. 6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1678P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4113 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.2514 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 -0.003106(17) 0.60631(3) 0.82331(2) 0.0536(3) Uani 1 1 d . . . N1 N -0.0363(4) 0.7087(5) 0.9109(3) 0.0583(17) Uani 1 1 d . . . N2 N -0.0089(3) 0.7834(6) 0.7896(4) 0.0522(18) Uani 1 1 d . . . O1 O -0.0954(3) 0.6188(5) 0.8008(3) 0.0674(17) Uani 1 1 d . . . O2 O 0.0815(3) 0.6531(4) 0.8566(3) 0.0606(15) Uani 1 1 d . . . O3 O 0.0245(4) 0.5649(5) 0.7491(3) 0.0694(17) Uani 1 1 d . . . O4 O -0.0101(3) 0.4954(6) 0.8705(4) 0.0685(19) Uani 1 1 d . . . C1 C -0.1346(4) 0.6717(7) 0.7595(4) 0.057(2) Uani 1 1 d . . . C2 C -0.2020(5) 0.6464(8) 0.7575(4) 0.064(2) Uani 1 1 d . . . C3 C -0.2413(6) 0.6981(11) 0.7136(6) 0.090(3) Uani 1 1 d . . . H3B H -0.2860 0.6816 0.7116 0.107 Uiso 1 1 calc R . . C4 C -0.2165(6) 0.7734(10) 0.6728(5) 0.086(3) Uani 1 1 d . . . H4B H -0.2437 0.8050 0.6423 0.104 Uiso 1 1 calc R . . C5 C -0.1499(6) 0.8022(9) 0.6777(4) 0.074(3) Uani 1 1 d . . . H5A H -0.1334 0.8568 0.6526 0.088 Uiso 1 1 calc R . . C6 C -0.1088(5) 0.7490(7) 0.7199(4) 0.065(2) Uani 1 1 d . . . C7 C -0.2335(5) 0.5677(8) 0.8058(5) 0.075(3) Uani 1 1 d . . . C8 C -0.2013(6) 0.4573(9) 0.7997(6) 0.092(3) Uani 1 1 d . . . H8A H -0.2215 0.4100 0.8300 0.139 Uiso 1 1 calc R . . H8B H -0.1549 0.4624 0.8086 0.139 Uiso 1 1 calc R . . H8C H -0.2077 0.4310 0.7569 0.139 Uiso 1 1 calc R . . C9 C -0.3065(6) 0.5518(11) 0.7945(8) 0.119(5) Uani 1 1 d . . . H9A H -0.3234 0.5024 0.8254 0.178 Uiso 1 1 calc R . . H9B H -0.3134 0.5251 0.7519 0.178 Uiso 1 1 calc R . . H9C H -0.3291 0.6178 0.7992 0.178 Uiso 1 1 calc R . . C10 C -0.2236(7) 0.6088(9) 0.8725(5) 0.092(4) Uani 1 1 d . . . H10A H -0.2427 0.5606 0.9029 0.138 Uiso 1 1 calc R . . H10B H -0.2447 0.6762 0.8765 0.138 Uiso 1 1 calc R . . H10C H -0.1773 0.6160 0.8809 0.138 Uiso 1 1 calc R . . C11 C 0.1072(4) 0.7431(7) 0.8807(4) 0.056(2) Uani 1 1 d . . . C12 C 0.1435(5) 0.7435(7) 0.9380(4) 0.061(2) Uani 1 1 d . . . C13 C 0.1631(6) 0.8419(9) 0.9605(5) 0.084(3) Uani 1 1 d . . . H13A H 0.1859 0.8458 0.9992 0.101 Uiso 1 1 calc R . . C14 C 0.1502(5) 0.9335(9) 0.9277(6) 0.083(3) Uani 1 1 d . . . H14A H 0.1639 0.9973 0.9451 0.100 Uiso 1 1 calc R . . C15 C 0.1176(5) 0.9328(7) 0.8701(6) 0.073(3) Uani 1 1 d . . . H15A H 0.1108 0.9949 0.8474 0.088 Uiso 1 1 calc R . . C16 C 0.0947(4) 0.8366(7) 0.8462(4) 0.055(2) Uani 1 1 d . . . C17 C 0.1658(6) 0.6464(10) 0.9763(5) 0.082(3) Uani 1 1 d . . . C18 C 0.1252(11) 0.6382(19) 1.0379(11) 0.248(15) Uani 1 1 d . . . H18A H 0.1284 0.7030 1.0615 0.372 Uiso 1 1 calc R . . H18B H 0.1417 0.5815 1.0638 0.372 Uiso 1 1 calc R . . H18C H 0.0798 0.6251 1.0272 0.372 Uiso 1 1 calc R . . C19 C 0.1581(12) 0.5457(11) 0.9406(10) 0.216(13) Uani 1 1 d . . . H19A H 0.1834 0.5486 0.9015 0.324 Uiso 1 1 calc R . . H19B H 0.1124 0.5350 0.9304 0.324 Uiso 1 1 calc R . . H19C H 0.1737 0.4886 0.9667 0.324 Uiso 1 1 calc R . . C20 C 0.2366(6) 0.6572(10) 0.9970(7) 0.107(4) Uani 1 1 d . . . H20A H 0.2646 0.6587 0.9597 0.160 Uiso 1 1 calc R . . H20B H 0.2485 0.5986 1.0237 0.160 Uiso 1 1 calc R . . H20C H 0.2420 0.7214 1.0208 0.160 Uiso 1 1 calc R . . C21 C -0.0469(5) 0.8124(7) 0.9016(4) 0.060(2) Uani 1 1 d . . . C22 C -0.0578(7) 0.8764(9) 0.9538(6) 0.090(3) Uani 1 1 d . . . H22A H -0.0648 0.9480 0.9476 0.108 Uiso 1 1 calc R . . C23 C -0.0587(7) 0.8363(12) 1.0144(6) 0.107(4) Uani 1 1 d . . . H23A H -0.0650 0.8806 1.0495 0.128 Uiso 1 1 calc R . . C24 C -0.0501(6) 0.7288(11) 1.0237(6) 0.094(4) Uani 1 1 d . . . H24A H -0.0523 0.6986 1.0645 0.112 Uiso 1 1 calc R . . C25 C -0.0383(6) 0.6698(9) 0.9700(5) 0.078(3) Uani 1 1 d . . . H25A H -0.0313 0.5979 0.9752 0.093 Uiso 1 1 calc R . . C26 C -0.0374(5) 0.7830(7) 0.7238(4) 0.062(2) Uani 1 1 d . . . H26A H -0.0112 0.7364 0.6970 0.075 Uiso 1 1 calc R . . H26B H -0.0336 0.8533 0.7060 0.075 Uiso 1 1 calc R . . C27 C 0.0600(4) 0.8281(7) 0.7839(5) 0.067(3) Uani 1 1 d . . . H27A H 0.0857 0.7836 0.7554 0.081 Uiso 1 1 calc R . . H27B H 0.0574 0.8974 0.7645 0.081 Uiso 1 1 calc R . . C28 C -0.0476(5) 0.8499(7) 0.8341(5) 0.063(2) Uani 1 1 d . . . H28A H -0.0929 0.8525 0.8192 0.075 Uiso 1 1 calc R . . H28B H -0.0302 0.9210 0.8328 0.075 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 0.0414(4) 0.0488(5) 0.0706(5) -0.00130(13) -0.00178(14) 0.00110(12) N1 0.051(4) 0.058(4) 0.066(4) -0.001(3) 0.006(4) -0.003(3) N2 0.045(4) 0.042(4) 0.069(5) 0.003(3) 0.003(3) 0.003(3) O1 0.048(4) 0.072(4) 0.082(4) 0.018(3) -0.006(3) -0.001(3) O2 0.046(4) 0.058(4) 0.078(4) -0.008(3) -0.004(3) 0.005(3) O3 0.058(4) 0.066(4) 0.085(4) -0.020(3) 0.006(4) -0.002(3) O4 0.053(4) 0.065(4) 0.088(5) 0.004(4) -0.007(3) 0.000(3) C1 0.046(5) 0.056(5) 0.069(5) 0.002(4) -0.005(4) 0.007(4) C2 0.040(5) 0.082(7) 0.069(6) 0.003(5) -0.002(4) 0.004(4) C3 0.055(6) 0.127(10) 0.087(8) 0.000(7) -0.010(6) 0.014(6) C4 0.068(7) 0.117(9) 0.074(7) 0.010(6) -0.017(6) 0.021(7) C5 0.068(7) 0.088(7) 0.065(6) 0.010(4) -0.008(5) 0.005(5) C6 0.055(5) 0.070(6) 0.071(6) 0.007(4) -0.010(5) 0.002(4) C7 0.045(6) 0.093(8) 0.086(7) -0.010(6) 0.005(5) -0.002(5) C8 0.075(8) 0.089(8) 0.113(8) -0.008(7) 0.007(7) -0.014(6) C9 0.047(7) 0.137(11) 0.172(13) 0.023(10) 0.008(9) -0.021(7) C10 0.080(9) 0.107(9) 0.089(8) -0.001(6) 0.025(7) -0.002(6) C11 0.036(4) 0.063(5) 0.070(5) -0.013(4) 0.009(4) -0.002(4) C12 0.048(5) 0.071(6) 0.065(5) -0.002(4) 0.005(4) -0.012(4) C13 0.066(7) 0.095(9) 0.093(8) -0.018(6) -0.012(6) -0.002(6) C14 0.058(7) 0.084(8) 0.108(8) -0.036(6) -0.002(6) -0.006(5) C15 0.053(6) 0.043(5) 0.123(8) 0.005(5) 0.005(6) -0.003(4) C16 0.036(4) 0.053(5) 0.077(6) 0.000(4) 0.004(4) 0.002(4) C17 0.054(6) 0.111(8) 0.082(7) 0.010(6) -0.019(5) -0.007(6) C18 0.130(19) 0.34(3) 0.28(3) 0.22(2) 0.084(19) 0.081(19) C19 0.33(3) 0.073(10) 0.25(2) 0.008(11) -0.22(2) 0.006(13) C20 0.064(8) 0.111(9) 0.146(11) -0.017(8) -0.042(8) 0.008(7) C21 0.047(5) 0.056(6) 0.077(6) -0.007(4) 0.006(4) 0.002(4) C22 0.088(9) 0.072(8) 0.110(9) -0.020(6) 0.010(7) 0.014(5) C23 0.117(12) 0.137(12) 0.067(7) -0.032(7) 0.013(7) 0.029(9) C24 0.081(9) 0.118(10) 0.082(7) -0.013(7) 0.021(6) 0.004(7) C25 0.070(7) 0.093(8) 0.071(7) 0.013(5) 0.000(5) -0.001(6) C26 0.052(5) 0.065(5) 0.070(6) 0.008(4) 0.004(4) 0.000(4) C27 0.043(5) 0.071(6) 0.087(7) 0.022(5) 0.008(5) -0.002(4) C28 0.044(5) 0.051(5) 0.094(7) -0.007(4) 0.004(5) 0.003(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 O4 1.723(8) . ? W1 O3 1.723(6) . ? W1 O1 1.933(7) . ? W1 O2 1.941(6) . ? W1 N1 2.336(7) . ? W1 N2 2.359(8) . ? N1 C25 1.324(11) . ? N1 C21 1.349(11) . ? N2 C28 1.478(12) . ? N2 C26 1.485(12) . ? N2 C27 1.512(10) . ? O1 C1 1.349(10) . ? O2 C11 1.353(9) . ? C1 C6 1.384(12) . ? C1 C2 1.402(12) . ? C2 C3 1.378(14) . ? C2 C7 1.555(14) . ? C3 C4 1.373(16) . ? C4 C5 1.402(15) . ? C5 C6 1.386(13) . ? C6 C26 1.512(13) . ? C7 C10 1.493(15) . ? C7 C9 1.511(15) . ? C7 C8 1.552(14) . ? C11 C12 1.400(12) . ? C11 C16 1.411(12) . ? C12 C13 1.392(13) . ? C12 C17 1.535(14) . ? C13 C14 1.373(15) . ? C14 C15 1.367(15) . ? C15 C16 1.398(12) . ? C16 C27 1.477(13) . ? C17 C19 1.487(18) . ? C17 C20 1.504(15) . ? C17 C18 1.53(2) . ? C21 C22 1.373(14) . ? C21 C28 1.482(13) . ? C22 C23 1.359(17) . ? C23 C24 1.391(16) . ? C24 C25 1.366(14) . ? 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 O4 W1 O3 106.7(3) . . ? O4 W1 O1 97.2(3) . . ? O3 W1 O1 97.0(3) . . ? O4 W1 O2 96.9(3) . . ? O3 W1 O2 97.3(3) . . ? O1 W1 O2 156.1(2) . . ? O4 W1 N1 89.3(3) . . ? O3 W1 N1 163.9(3) . . ? O1 W1 N1 82.2(3) . . ? O2 W1 N1 78.8(3) . . ? O4 W1 N2 160.9(3) . . ? O3 W1 N2 92.4(3) . . ? O1 W1 N2 78.6(2) . . ? O2 W1 N2 81.8(2) . . ? N1 W1 N2 71.7(3) . . ? C25 N1 C21 119.5(8) . . ? C25 N1 W1 121.6(7) . . ? C21 N1 W1 118.6(5) . . ? C28 N2 C26 111.9(7) . . ? C28 N2 C27 108.9(7) . . ? C26 N2 C27 106.7(7) . . ? C28 N2 W1 112.7(6) . . ? C26 N2 W1 106.9(5) . . ? C27 N2 W1 109.6(5) . . ? C1 O1 W1 139.9(6) . . ? C11 O2 W1 137.0(5) . . ? O1 C1 C6 120.6(8) . . ? O1 C1 C2 118.6(8) . . ? C6 C1 C2 120.8(8) . . ? C3 C2 C1 118.3(9) . . ? C3 C2 C7 119.8(9) . . ? C1 C2 C7 121.8(8) . . ? C4 C3 C2 121.9(11) . . ? C3 C4 C5 119.3(10) . . ? C6 C5 C4 119.8(10) . . ? C1 C6 C5 119.7(9) . . ? C1 C6 C26 122.2(8) . . ? C5 C6 C26 118.0(9) . . ? C10 C7 C9 108.7(10) . . ? C10 C7 C8 109.6(10) . . ? C9 C7 C8 106.1(10) . . ? C10 C7 C2 108.7(9) . . ? C9 C7 C2 112.8(10) . . ? C8 C7 C2 110.9(9) . . ? O2 C11 C12 121.4(8) . . ? O2 C11 C16 117.0(8) . . ? C12 C11 C16 121.6(8) . . ? C13 C12 C11 116.0(9) . . ? C13 C12 C17 117.6(9) . . ? C11 C12 C17 126.3(8) . . ? C14 C13 C12 122.7(10) . . ? C15 C14 C13 121.4(9) . . ? C14 C15 C16 118.5(9) . . ? C15 C16 C11 119.7(9) . . ? C15 C16 C27 122.3(8) . . ? C11 C16 C27 118.0(7) . . ? C19 C17 C20 108.8(12) . . ? C19 C17 C18 107.7(15) . . ? C20 C17 C18 106.3(13) . . ? C19 C17 C12 113.7(9) . . ? C20 C17 C12 110.8(10) . . ? C18 C17 C12 109.3(11) . . ? N1 C21 C22 119.4(9) . . ? N1 C21 C28 116.8(7) . . ? C22 C21 C28 123.7(9) . . ? C23 C22 C21 120.8(11) . . ? C22 C23 C24 119.7(11) . . ? C25 C24 C23 116.6(11) . . ? N1 C25 C24 124.0(11) . . ? N2 C26 C6 114.9(7) . . ? C16 C27 N2 113.5(7) . . ? N2 C28 C21 113.8(8) . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.874 _refine_diff_density_max 6.206 _refine_diff_density_min -3.756 _refine_diff_density_rms 0.385 #===END data_YLWMO4 _database_code_depnum_ccdc_archive 'CCDC 759489' #TrackingRef 'Wong_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H51 Mo N3 O4' _chemical_formula_weight 709.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 16.327(3) _cell_length_b 10.457(2) _cell_length_c 25.688(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.18(3) _cell_angle_gamma 90.00 _cell_volume 4000.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 1.198 _exptl_absorpt_process_details 'ABSCOR program, Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IIC imaging plate' _diffrn_measurement_method 'phi oscillation method' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9524 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5511 _reflns_number_gt 4510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS-IIC RIGAKU' _computing_cell_refinement 'BioteX software MSC 1995' _computing_data_reduction 'BioteX software MSC 1995' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL Vers. 6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1001P)^2^+0.9314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5511 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1977 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Mo1 Mo 0.52050(3) 0.61219(5) 0.86436(2) 0.0590(2) Uani 1 1 d . . . O1 O 0.3964(2) 0.6505(4) 0.84591(17) 0.0677(11) Uani 1 1 d . . . O2 O 0.6458(3) 0.6393(4) 0.88366(17) 0.0701(11) Uani 1 1 d . . . O3 O 0.5023(3) 0.5315(5) 0.80299(17) 0.0775(12) Uani 1 1 d . . . O4 O 0.5334(3) 0.4997(4) 0.91573(17) 0.0721(11) Uani 1 1 d . . . N1 N 0.5442(3) 0.7827(5) 0.92461(19) 0.0593(12) Uani 1 1 d . . . N2 N 0.5793(4) 0.9862(5) 0.9484(2) 0.0757(14) Uani 1 1 d . . . H2A H 0.5879 1.0662 0.9447 0.091 Uiso 1 1 calc R . . N3 N 0.5076(3) 0.8069(5) 0.81113(18) 0.0602(12) Uani 1 1 d . . . C1 C 0.3359(4) 0.7439(6) 0.8237(2) 0.0617(14) Uani 1 1 d . . . C2 C 0.3431(4) 0.8265(7) 0.7821(2) 0.0633(15) Uani 1 1 d . . . C3 C 0.2775(4) 0.9216(7) 0.7560(3) 0.0723(17) Uani 1 1 d . . . H3B H 0.2825 0.9743 0.7283 0.087 Uiso 1 1 calc R . . C4 C 0.2058(4) 0.9376(8) 0.7710(3) 0.0770(19) Uani 1 1 d . . . C5 C 0.2017(4) 0.8549(7) 0.8126(3) 0.0745(18) Uani 1 1 d . . . H5A H 0.1532 0.8642 0.8225 0.089 Uiso 1 1 calc R . . C6 C 0.2641(4) 0.7595(7) 0.8406(2) 0.0677(16) Uani 1 1 d . . . C7 C 0.2502(4) 0.6669(7) 0.8823(3) 0.0693(16) Uani 1 1 d . . . C8 C 0.2268(5) 0.5364(9) 0.8551(3) 0.096(2) Uani 1 1 d . . . H8A H 0.2751 0.5059 0.8463 0.144 Uiso 1 1 calc R . . H8B H 0.1730 0.5421 0.8207 0.144 Uiso 1 1 calc R . . H8C H 0.2174 0.4783 0.8811 0.144 Uiso 1 1 calc R . . C9 C 0.1708(5) 0.7106(9) 0.8964(3) 0.105(3) Uani 1 1 d . . . H9A H 0.1170 0.7148 0.8619 0.158 Uiso 1 1 calc R . . H9B H 0.1836 0.7936 0.9140 0.158 Uiso 1 1 calc R . . H9C H 0.1627 0.6505 0.9222 0.158 Uiso 1 1 calc R . . C10 C 0.3345(5) 0.6548(8) 0.9381(3) 0.089(2) Uani 1 1 d . . . H10A H 0.3836 0.6247 0.9301 0.134 Uiso 1 1 calc R . . H10B H 0.3233 0.5953 0.9630 0.134 Uiso 1 1 calc R . . H10C H 0.3493 0.7368 0.9564 0.134 Uiso 1 1 calc R . . C11 C 0.1363(5) 1.0404(10) 0.7430(3) 0.107(3) Uani 1 1 d . . . C12 C 0.1635(11) 1.1395(17) 0.7173(9) 0.306(15) Uani 1 1 d . . . H12A H 0.2198 1.1733 0.7440 0.458 Uiso 1 1 calc R . . H12B H 0.1191 1.2059 0.7060 0.458 Uiso 1 1 calc R . . H12C H 0.1706 1.1075 0.6844 0.458 Uiso 1 1 calc R . . C13 C 0.0546(13) 0.970(2) 0.7022(9) 0.40(2) Uani 1 1 d . . . H13A H 0.0694 0.9249 0.6746 0.596 Uiso 1 1 calc R . . H13B H 0.0073 1.0297 0.6830 0.596 Uiso 1 1 calc R . . H13C H 0.0352 0.9097 0.7231 0.596 Uiso 1 1 calc R . . C14 C 0.0971(13) 1.0911(18) 0.7787(7) 0.265(12) Uani 1 1 d . . . H14A H 0.1372 1.1525 0.8044 0.398 Uiso 1 1 calc R . . H14B H 0.0863 1.0231 0.8003 0.398 Uiso 1 1 calc R . . H14C H 0.0413 1.1320 0.7557 0.398 Uiso 1 1 calc R . . C15 C 0.7028(4) 0.7298(6) 0.8792(2) 0.0623(15) Uani 1 1 d . . . C16 C 0.6712(4) 0.8120(7) 0.8320(2) 0.0637(15) Uani 1 1 d . . . C17 C 0.7265(4) 0.9083(7) 0.8263(3) 0.0729(18) Uani 1 1 d . . . H17A H 0.7044 0.9633 0.7952 0.088 Uiso 1 1 calc R . . C18 C 0.8143(4) 0.9225(7) 0.8668(3) 0.0716(17) Uani 1 1 d . . . C19 C 0.8443(4) 0.8351(8) 0.9121(3) 0.0803(19) Uani 1 1 d . . . H19A H 0.9037 0.8420 0.9383 0.096 Uiso 1 1 calc R . . C20 C 0.7927(4) 0.7384(7) 0.9211(2) 0.0685(16) Uani 1 1 d . . . C21 C 0.8318(4) 0.6471(8) 0.9703(3) 0.082(2) Uani 1 1 d . . . C22 C 0.9294(6) 0.6698(12) 1.0053(4) 0.143(4) Uani 1 1 d . . . H22A H 0.9508 0.6099 1.0364 0.214 Uiso 1 1 calc R . . H22B H 0.9380 0.7553 1.0201 0.214 Uiso 1 1 calc R . . H22C H 0.9621 0.6586 0.9820 0.214 Uiso 1 1 calc R . . C23 C 0.7813(7) 0.6527(13) 1.0072(4) 0.151(5) Uani 1 1 d . . . H23A H 0.8064 0.5923 1.0379 0.226 Uiso 1 1 calc R . . H23B H 0.7194 0.6322 0.9850 0.226 Uiso 1 1 calc R . . H23C H 0.7856 0.7373 1.0227 0.226 Uiso 1 1 calc R . . C24 C 0.8216(7) 0.5083(11) 0.9488(4) 0.143(4) Uani 1 1 d . . . H24A H 0.8450 0.4512 0.9808 0.215 Uiso 1 1 calc R . . H24B H 0.8541 0.4972 0.9253 0.215 Uiso 1 1 calc R . . H24C H 0.7592 0.4899 0.9268 0.215 Uiso 1 1 calc R . . C25 C 0.8757(5) 1.0295(9) 0.8614(3) 0.093(2) Uani 1 1 d . . . C26 C 0.8510(9) 1.0642(15) 0.7993(5) 0.221(9) Uani 1 1 d . . . H26A H 0.8893 1.1320 0.7973 0.332 Uiso 1 1 calc R . . H26B H 0.7896 1.0916 0.7820 0.332 Uiso 1 1 calc R . . H26C H 0.8587 0.9907 0.7793 0.332 Uiso 1 1 calc R . . C27 C 0.9737(6) 0.9906(14) 0.8876(5) 0.172(5) Uani 1 1 d . . . H27A H 1.0097 1.0592 0.8835 0.257 Uiso 1 1 calc R . . H27B H 0.9818 0.9159 0.8686 0.257 Uiso 1 1 calc R . . H27C H 0.9917 0.9722 0.9274 0.257 Uiso 1 1 calc R . . C28 C 0.8728(13) 1.1381(15) 0.8966(10) 0.267(11) Uani 1 1 d . . . H28A H 0.9098 1.2059 0.8930 0.400 Uiso 1 1 calc R . . H28B H 0.8946 1.1120 0.9357 0.400 Uiso 1 1 calc R . . H28C H 0.8120 1.1678 0.8840 0.400 Uiso 1 1 calc R . . C29 C 0.5716(4) 0.7955(6) 0.9836(2) 0.0619(15) Uani 1 1 d . . . C30 C 0.5771(4) 0.7037(7) 1.0243(2) 0.0700(16) Uani 1 1 d . . . H30A H 0.5595 0.6194 1.0144 0.084 Uiso 1 1 calc R . . C31 C 0.6111(4) 0.7463(8) 1.0813(3) 0.081(2) Uani 1 1 d . . . H31A H 0.6181 0.6873 1.1099 0.097 Uiso 1 1 calc R . . C32 C 0.6345(5) 0.8734(8) 1.0965(3) 0.088(2) Uani 1 1 d . . . H32A H 0.6557 0.8975 1.1346 0.105 Uiso 1 1 calc R . . C33 C 0.6267(5) 0.9649(8) 1.0550(3) 0.091(2) Uani 1 1 d . . . H33A H 0.6426 1.0499 1.0646 0.109 Uiso 1 1 calc R . . C34 C 0.5941(5) 0.9228(7) 0.9988(3) 0.0726(17) Uani 1 1 d . . . C35 C 0.5489(4) 0.8991(6) 0.9062(2) 0.0637(15) Uani 1 1 d . . . C36 C 0.4165(3) 0.8065(6) 0.7622(2) 0.0636(15) Uani 1 1 d . . . H36A H 0.4139 0.8737 0.7356 0.076 Uiso 1 1 calc R . . H36B H 0.4073 0.7254 0.7423 0.076 Uiso 1 1 calc R . . C37 C 0.5779(4) 0.7979(7) 0.7869(2) 0.0661(15) Uani 1 1 d . . . H37A H 0.5724 0.7159 0.7681 0.079 Uiso 1 1 calc R . . H37B H 0.5669 0.8642 0.7584 0.079 Uiso 1 1 calc R . . C38 C 0.5207(4) 0.9314(7) 0.8443(2) 0.0645(15) Uani 1 1 d . . . H38A H 0.5665 0.9830 0.8394 0.077 Uiso 1 1 calc R . . H38B H 0.4652 0.9797 0.8304 0.077 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 0.0647(3) 0.0496(4) 0.0616(3) 0.0009(2) 0.0248(2) -0.0004(2) O1 0.060(2) 0.066(3) 0.071(2) 0.016(2) 0.0208(18) -0.005(2) O2 0.069(3) 0.061(3) 0.079(3) 0.017(2) 0.028(2) 0.0111(19) O3 0.097(3) 0.061(3) 0.074(3) -0.009(2) 0.035(2) -0.001(2) O4 0.075(2) 0.054(3) 0.087(3) 0.012(2) 0.033(2) -0.002(2) N1 0.065(3) 0.050(3) 0.060(3) 0.004(2) 0.022(2) -0.002(2) N2 0.103(4) 0.046(3) 0.075(3) -0.004(3) 0.033(3) -0.006(3) N3 0.058(3) 0.068(4) 0.053(3) 0.006(2) 0.0213(19) 0.001(2) C1 0.067(3) 0.055(4) 0.059(3) 0.008(3) 0.022(3) 0.001(3) C2 0.064(3) 0.065(4) 0.061(3) 0.006(3) 0.025(3) 0.001(3) C3 0.067(4) 0.078(5) 0.075(4) 0.025(3) 0.032(3) 0.007(3) C4 0.070(4) 0.089(6) 0.074(4) 0.022(4) 0.032(3) 0.016(3) C5 0.069(4) 0.073(5) 0.087(4) 0.013(3) 0.037(3) 0.006(3) C6 0.065(3) 0.077(5) 0.059(3) 0.011(3) 0.023(3) 0.000(3) C7 0.077(4) 0.071(5) 0.065(4) 0.008(3) 0.034(3) -0.001(3) C8 0.092(5) 0.101(7) 0.093(5) 0.010(5) 0.035(4) -0.015(4) C9 0.105(5) 0.138(9) 0.094(5) 0.039(5) 0.063(4) 0.017(5) C10 0.088(5) 0.103(6) 0.073(4) 0.018(4) 0.028(3) -0.010(4) C11 0.098(5) 0.124(8) 0.103(6) 0.051(5) 0.047(5) 0.049(5) C12 0.247(17) 0.27(2) 0.53(3) 0.31(2) 0.29(2) 0.202(17) C13 0.24(2) 0.24(2) 0.42(3) -0.07(2) -0.16(2) 0.157(19) C14 0.33(2) 0.28(2) 0.278(19) 0.156(18) 0.223(18) 0.22(2) C15 0.058(3) 0.069(5) 0.064(3) -0.001(3) 0.028(2) 0.000(3) C16 0.057(3) 0.076(5) 0.062(3) 0.010(3) 0.028(2) 0.009(3) C17 0.075(4) 0.080(5) 0.067(4) 0.013(3) 0.033(3) 0.001(3) C18 0.065(4) 0.072(5) 0.078(4) 0.004(3) 0.029(3) -0.008(3) C19 0.073(4) 0.093(6) 0.071(4) 0.006(4) 0.026(3) -0.010(4) C20 0.067(4) 0.069(5) 0.065(3) 0.009(3) 0.024(3) -0.001(3) C21 0.071(4) 0.090(6) 0.081(4) 0.025(4) 0.025(3) 0.008(4) C22 0.093(6) 0.161(10) 0.130(7) 0.068(7) 0.001(5) -0.011(6) C23 0.132(8) 0.226(13) 0.115(7) 0.093(8) 0.070(6) 0.067(8) C24 0.151(8) 0.091(8) 0.144(8) 0.038(6) 0.016(6) 0.014(6) C25 0.092(5) 0.089(7) 0.097(5) 0.010(4) 0.040(4) -0.023(4) C26 0.225(14) 0.276(19) 0.128(9) 0.070(10) 0.036(8) -0.142(14) C27 0.091(7) 0.156(12) 0.261(13) 0.070(10) 0.066(7) -0.011(6) C28 0.32(2) 0.144(13) 0.49(3) -0.109(16) 0.32(2) -0.108(13) C29 0.069(3) 0.054(4) 0.060(3) 0.007(3) 0.024(3) 0.003(3) C30 0.075(4) 0.058(4) 0.070(4) 0.007(3) 0.023(3) -0.003(3) C31 0.089(4) 0.091(6) 0.065(4) 0.013(4) 0.034(3) 0.011(4) C32 0.108(5) 0.082(6) 0.069(4) -0.015(4) 0.031(4) 0.003(4) C33 0.124(6) 0.084(6) 0.066(4) -0.014(4) 0.040(4) -0.009(5) C34 0.097(4) 0.054(4) 0.062(4) 0.000(3) 0.028(3) 0.004(3) C35 0.072(3) 0.057(4) 0.062(3) 0.008(3) 0.026(3) 0.004(3) C36 0.063(3) 0.063(4) 0.063(3) 0.006(3) 0.023(2) -0.006(3) C37 0.069(3) 0.071(5) 0.060(3) 0.009(3) 0.028(3) 0.007(3) C38 0.066(3) 0.066(4) 0.062(3) 0.001(3) 0.027(3) -0.001(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 Mo1 O3 1.703(4) . ? Mo1 O4 1.715(4) . ? Mo1 O2 1.918(4) . ? Mo1 O1 1.924(4) . ? Mo1 N1 2.288(5) . ? Mo1 N3 2.414(5) . ? O1 C1 1.338(7) . ? O2 C15 1.366(7) . ? N1 C35 1.320(7) . ? N1 C29 1.400(7) . ? N2 C35 1.345(8) . ? N2 C34 1.385(8) . ? N3 C36 1.503(7) . ? N3 C37 1.516(7) . ? N3 C38 1.522(8) . ? C1 C6 1.416(8) . ? C1 C2 1.417(8) . ? C2 C3 1.413(8) . ? C2 C36 1.497(8) . ? C3 C4 1.385(8) . ? C4 C5 1.395(9) . ? C4 C11 1.514(9) . ? C5 C6 1.397(9) . ? C6 C7 1.529(9) . ? C7 C8 1.509(11) . ? C7 C10 1.533(8) . ? C7 C9 1.552(9) . ? C11 C12 1.394(15) . ? C11 C14 1.421(14) . ? C11 C13 1.51(2) . ? C15 C16 1.401(8) . ? C15 C20 1.423(8) . ? C16 C17 1.399(9) . ? C16 C37 1.497(8) . ? C17 C18 1.392(8) . ? C18 C19 1.400(9) . ? C18 C25 1.547(9) . ? C19 C20 1.395(9) . ? C20 C21 1.501(9) . ? C21 C23 1.492(11) . ? C21 C22 1.494(10) . ? C21 C24 1.537(13) . ? C25 C28 1.463(16) . ? C25 C27 1.515(12) . ? C25 C26 1.522(11) . ? C29 C34 1.394(9) . ? C29 C30 1.395(8) . ? C30 C31 1.408(9) . ? C31 C32 1.394(10) . ? C32 C33 1.398(10) . ? C33 C34 1.391(8) . ? C35 C38 1.502(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 O3 Mo1 O4 107.0(2) . . ? O3 Mo1 O2 94.3(2) . . ? O4 Mo1 O2 96.93(18) . . ? O3 Mo1 O1 96.2(2) . . ? O4 Mo1 O1 96.73(18) . . ? O2 Mo1 O1 159.5(2) . . ? O3 Mo1 N1 158.3(2) . . ? O4 Mo1 N1 94.6(2) . . ? O2 Mo1 N1 80.98(18) . . ? O1 Mo1 N1 82.73(17) . . ? O3 Mo1 N3 87.24(19) . . ? O4 Mo1 N3 165.76(19) . . ? O2 Mo1 N3 81.84(16) . . ? O1 Mo1 N3 81.15(16) . . ? N1 Mo1 N3 71.15(17) . . ? C1 O1 Mo1 140.8(4) . . ? C15 O2 Mo1 140.6(4) . . ? C35 N1 C29 105.1(5) . . ? C35 N1 Mo1 119.7(4) . . ? C29 N1 Mo1 134.2(4) . . ? C35 N2 C34 107.1(5) . . ? C36 N3 C37 108.2(4) . . ? C36 N3 C38 109.5(4) . . ? C37 N3 C38 109.1(5) . . ? C36 N3 Mo1 107.3(3) . . ? C37 N3 Mo1 106.0(4) . . ? C38 N3 Mo1 116.4(3) . . ? O1 C1 C6 120.9(5) . . ? O1 C1 C2 119.4(5) . . ? C6 C1 C2 119.7(5) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C36 119.6(5) . . ? C1 C2 C36 119.8(5) . . ? C4 C3 C2 121.0(6) . . ? C3 C4 C5 116.7(6) . . ? C3 C4 C11 120.4(6) . . ? C5 C4 C11 122.9(6) . . ? C4 C5 C6 125.6(6) . . ? C5 C6 C1 116.5(5) . . ? C5 C6 C7 121.8(5) . . ? C1 C6 C7 121.4(6) . . ? C8 C7 C6 109.3(5) . . ? C8 C7 C10 108.5(6) . . ? C6 C7 C10 112.0(5) . . ? C8 C7 C9 107.3(6) . . ? C6 C7 C9 110.9(6) . . ? C10 C7 C9 108.7(6) . . ? C12 C11 C14 110.0(13) . . ? C12 C11 C13 113.5(14) . . ? C14 C11 C13 97.3(14) . . ? C12 C11 C4 115.6(8) . . ? C14 C11 C4 113.9(8) . . ? C13 C11 C4 105.0(10) . . ? O2 C15 C16 118.4(5) . . ? O2 C15 C20 120.5(5) . . ? C16 C15 C20 121.1(6) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 C37 119.1(5) . . ? C15 C16 C37 120.5(6) . . ? C18 C17 C16 120.6(6) . . ? C17 C18 C19 117.1(6) . . ? C17 C18 C25 121.1(6) . . ? C19 C18 C25 121.8(6) . . ? C20 C19 C18 125.5(6) . . ? C19 C20 C15 115.2(6) . . ? C19 C20 C21 121.5(6) . . ? C15 C20 C21 123.2(6) . . ? C23 C21 C22 109.9(8) . . ? C23 C21 C20 110.8(6) . . ? C22 C21 C20 112.8(7) . . ? C23 C21 C24 105.0(9) . . ? C22 C21 C24 107.4(8) . . ? C20 C21 C24 110.6(6) . . ? C28 C25 C27 103.3(11) . . ? C28 C25 C26 113.6(13) . . ? C27 C25 C26 107.9(9) . . ? C28 C25 C18 108.7(7) . . ? C27 C25 C18 111.8(7) . . ? C26 C25 C18 111.3(7) . . ? C34 C29 C30 121.3(6) . . ? C34 C29 N1 108.9(5) . . ? C30 C29 N1 129.8(6) . . ? C29 C30 C31 116.0(7) . . ? C32 C31 C30 122.6(7) . . ? C31 C32 C33 120.8(6) . . ? C34 C33 C32 116.8(7) . . ? N2 C34 C33 131.7(7) . . ? N2 C34 C29 105.7(5) . . ? C33 C34 C29 122.5(6) . . ? N1 C35 N2 113.1(5) . . ? N1 C35 C38 123.3(6) . . ? N2 C35 C38 123.6(6) . . ? C2 C36 N3 111.8(4) . . ? C16 C37 N3 112.2(4) . . ? C35 C38 N3 108.2(5) . . ? _diffrn_measured_fraction_theta_max 0.781 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.781 _refine_diff_density_max 0.443 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.076 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.286 -0.166 1.051 104.8 13.2 2 0.714 0.166 0.949 104.7 13.4 3 0.007 0.145 0.603 11.2 0.4 4 0.714 0.334 0.449 104.7 13.3 5 0.082 0.229 0.373 10.3 0.6 6 0.082 0.271 0.873 10.3 0.6 7 0.007 0.355 0.103 11.3 0.2 8 0.286 0.666 0.551 104.8 13.4 9 -0.007 0.645 0.897 11.1 0.2 10 0.918 0.729 0.127 10.3 1.0 11 0.918 0.771 0.627 10.4 0.9 12 0.993 0.855 0.397 11.2 0.2 _platon_squeeze_details ; ;