data_c16_mo6 _audit_creation_method SHELXL-97 _publ_contact_author ; Takeru Ito Department of Chemistry, School of Science Tokai University 1117 Kitakaname, Hiratsuka 259-1292, Japan ; _publ_contact_author_email 'takeito@keyaki.cc.u-tokai.ac.jp' _publ_contact_author_fax '81-463-50-2094' _publ_contact_author_phone '81-463-58-1211 ex.3737' _publ_section_title ; Controllable Layered Structures in Polyoxomolybdate-Surfactant Hybrid Crystals ; loop_ _publ_author_name _publ_author_address 'ITO, Takeru' ; Chemical Resources Laboratory, Tokai University, 1117 Kitakaname, Hiratsuka 259-1292, Japan ; 'Yamase, Toshihiro' ; Chemical Resources Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta, Midori-ku, Yokohama 226-8503, Japan ; _journal_name_full ; Materials ; _chemical_name_systematic ; bis(hexadecyltrimethylammonium) hexamolybdate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H84 Mo6 N2 O19' _chemical_formula_weight 1448.71 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' 'O' 'O' 0.0106 0.0060 '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 9.911(8) _cell_length_b 22.34(3) _cell_length_c 25.58(3) _cell_angle_alpha 102.78(4) _cell_angle_beta 99.12(3) _cell_angle_gamma 91.19(4) _cell_volume 5444(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22012 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.7 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6776 _exptl_absorpt_correction_T_max 0.9724 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48956 _diffrn_reflns_av_R_equivalents 0.1260 _diffrn_reflns_av_sigmaI/netI 0.3418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 22835 _reflns_number_gt 5821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC)' _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. All the atoms except for Mo were refined isotropically utilizing suitable restraints of the N-C and C-C distances. ; _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^)+(0.0690P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22835 _refine_ls_number_parameters 594 _refine_ls_number_restraints 188 _refine_ls_R_factor_all 0.2455 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 0.724 _refine_ls_restrained_S_all 0.728 _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 0.91775(10) 0.86068(5) 0.04105(4) 0.0377(3) Uani 1 1 d . . . Mo2 Mo 0.59548(10) 0.84843(5) 0.05312(5) 0.0378(3) Uani 1 1 d . . . Mo3 Mo 0.82071(10) 0.77474(5) 0.11836(5) 0.0396(3) Uani 1 1 d . . . Mo4 Mo 1.00167(10) 0.90429(5) 0.17405(5) 0.0399(3) Uani 1 1 d . . . Mo5 Mo 0.77564(10) 0.97829(5) 0.10878(5) 0.0386(3) Uani 1 1 d . . . Mo6 Mo 0.68016(10) 0.89239(5) 0.18617(5) 0.0422(3) Uani 1 1 d . . . O1 O 0.7987(7) 0.8769(4) 0.1128(3) 0.0384(19) Uiso 1 1 d . . . O2 O 0.7268(6) 0.8426(3) 0.0062(3) 0.035(2) Uiso 1 1 d . . . O3 O 0.9113(7) 0.7823(4) 0.0581(3) 0.039(2) Uiso 1 1 d . . . O4 O 1.0573(6) 0.8871(3) 0.1018(3) 0.0341(19) Uiso 1 1 d . . . O5 O 0.8682(6) 0.9469(3) 0.0501(3) 0.0294(18) Uiso 1 1 d . . . O6 O 0.6528(7) 0.7721(4) 0.0703(3) 0.040(2) Uiso 1 1 d . . . O7 O 0.9846(7) 0.8171(4) 0.1644(3) 0.041(2) Uiso 1 1 d . . . O8 O 0.9449(6) 0.9809(3) 0.1558(3) 0.0299(18) Uiso 1 1 d . . . O9 O 0.6110(6) 0.9365(3) 0.0626(3) 0.037(2) Uiso 1 1 d . . . O10 O 0.5404(6) 0.8665(3) 0.1240(3) 0.037(2) Uiso 1 1 d . . . O11 O 0.7256(7) 0.8067(4) 0.1762(3) 0.042(2) Uiso 1 1 d . . . O12 O 0.8708(7) 0.9116(4) 0.2204(3) 0.041(2) Uiso 1 1 d . . . O13 O 0.6856(7) 0.9711(4) 0.1685(3) 0.041(2) Uiso 1 1 d . . . O14 O 1.0014(7) 0.8521(4) -0.0122(3) 0.043(2) Uiso 1 1 d . . . O15 O 0.4448(7) 0.8295(4) 0.0110(3) 0.043(2) Uiso 1 1 d . . . O16 O 0.8408(7) 0.7017(4) 0.1233(3) 0.052(2) Uiso 1 1 d . . . O17 O 1.1531(7) 0.9234(4) 0.2149(3) 0.043(2) Uiso 1 1 d . . . O18 O 0.7541(7) 1.0518(4) 0.1048(3) 0.045(2) Uiso 1 1 d . . . O19 O 0.5953(7) 0.9026(4) 0.2391(3) 0.054(2) Uiso 1 1 d . . . Mo7 Mo 0.13337(11) 0.40500(5) 0.17635(5) 0.0463(3) Uani 1 1 d . . . Mo8 Mo 0.46462(11) 0.39580(6) 0.19058(5) 0.0545(4) Uani 1 1 d . . . Mo9 Mo 0.31066(11) 0.47835(5) 0.11031(5) 0.0477(3) Uani 1 1 d . . . Mo10 Mo 0.10873(10) 0.35813(5) 0.04378(5) 0.0417(3) Uani 1 1 d . . . Mo11 Mo 0.26304(10) 0.27580(5) 0.12425(5) 0.0429(3) Uani 1 1 d . . . Mo12 Mo 0.43987(10) 0.34915(5) 0.05798(5) 0.0472(3) Uani 1 1 d . . . O20 O 0.2872(7) 0.3780(4) 0.1168(3) 0.044(2) Uiso 1 1 d . . . O21 O 0.2983(7) 0.4114(4) 0.2240(3) 0.042(2) Uiso 1 1 d . . . O22 O 0.1778(7) 0.4808(4) 0.1593(3) 0.046(2) Uiso 1 1 d . . . O23 O 0.0204(6) 0.3842(3) 0.1037(3) 0.037(2) Uiso 1 1 d . . . O24 O 0.1366(7) 0.3159(4) 0.1668(3) 0.043(2) Uiso 1 1 d . . . O25 O 0.4443(8) 0.4746(4) 0.1732(3) 0.056(2) Uiso 1 1 d . . . O26 O 0.1660(7) 0.4458(4) 0.0523(3) 0.045(2) Uiso 1 1 d . . . O27 O 0.1281(6) 0.2814(3) 0.0613(3) 0.0337(19) Uiso 1 1 d . . . O28 O 0.4077(7) 0.3089(4) 0.1804(3) 0.053(2) Uiso 1 1 d . . . O29 O 0.5547(7) 0.3707(4) 0.1302(3) 0.048(2) Uiso 1 1 d . . . O30 O 0.4360(7) 0.4393(4) 0.0675(3) 0.052(2) Uiso 1 1 d . . . O31 O 0.2716(6) 0.3435(3) 0.0114(3) 0.037(2) Uiso 1 1 d . . . O32 O 0.3958(7) 0.2743(4) 0.0756(3) 0.042(2) Uiso 1 1 d . . . O33 O 0.0165(8) 0.4235(4) 0.2171(3) 0.061(3) Uiso 1 1 d . . . O34 O 0.5937(8) 0.4082(4) 0.2441(4) 0.063(3) Uiso 1 1 d . . . O35 O 0.3288(8) 0.5520(4) 0.1060(3) 0.061(3) Uiso 1 1 d . . . O36 O -0.0180(7) 0.3484(4) -0.0099(3) 0.048(2) Uiso 1 1 d . . . O37 O 0.2449(7) 0.2018(4) 0.1285(3) 0.051(2) Uiso 1 1 d . . . O38 O 0.5617(8) 0.3322(4) 0.0180(3) 0.059(3) Uiso 1 1 d . . . N1 N 0.7919(8) 0.2320(4) 0.1400(4) 0.048(3) Uiso 1 1 d D . . C2 C 0.8963(10) 0.1911(5) 0.1590(4) 0.043(3) Uiso 1 1 d D . . H2A H 0.9871 0.2135 0.1677 0.052 Uiso 1 1 calc R . . H2B H 0.8998 0.1549 0.1289 0.052 Uiso 1 1 calc R . . C3 C 0.8693(10) 0.1687(6) 0.2083(4) 0.050(3) Uiso 1 1 d D . . H3A H 0.7817 0.1436 0.1987 0.060 Uiso 1 1 calc R . . H3B H 0.8586 0.2049 0.2375 0.060 Uiso 1 1 calc R . . C4 C 0.9825(10) 0.1303(5) 0.2308(5) 0.050(3) Uiso 1 1 d D . . H4A H 1.0056 0.0987 0.2002 0.060 Uiso 1 1 calc R . . H4B H 1.0656 0.1575 0.2471 0.060 Uiso 1 1 calc R . . C5 C 0.9422(11) 0.0995(6) 0.2724(5) 0.056(4) Uiso 1 1 d D . . H5A H 0.8627 0.0704 0.2552 0.067 Uiso 1 1 calc R . . H5B H 0.9122 0.1310 0.3013 0.067 Uiso 1 1 calc R . . C6 C 1.0534(11) 0.0649(6) 0.2983(5) 0.054(4) Uiso 1 1 d D . . H6A H 1.0885 0.0355 0.2692 0.065 Uiso 1 1 calc R . . H6B H 1.1301 0.0945 0.3181 0.065 Uiso 1 1 calc R . . C7 C 1.0064(10) 0.0303(5) 0.3371(5) 0.053(4) Uiso 1 1 d D . . H7A H 0.9281 0.0016 0.3173 0.064 Uiso 1 1 calc R . . H7B H 0.9731 0.0600 0.3664 0.064 Uiso 1 1 calc R . . C8 C 1.1165(11) -0.0064(6) 0.3630(5) 0.060(4) Uiso 1 1 d D . . H8A H 1.1446 -0.0385 0.3339 0.072 Uiso 1 1 calc R . . H8B H 1.1978 0.0216 0.3804 0.072 Uiso 1 1 calc R . . C9 C 1.0699(11) -0.0370(6) 0.4052(5) 0.057(4) Uiso 1 1 d D . . H9A H 1.0432 -0.0047 0.4344 0.068 Uiso 1 1 calc R . . H9B H 0.9874 -0.0642 0.3878 0.068 Uiso 1 1 calc R . . C10 C 1.1750(11) -0.0744(6) 0.4307(5) 0.055(4) Uiso 1 1 d D . . H10A H 1.2596 -0.0480 0.4463 0.066 Uiso 1 1 calc R . . H10B H 1.1975 -0.1084 0.4019 0.066 Uiso 1 1 calc R . . C11 C 1.1299(11) -0.1015(6) 0.4751(5) 0.055(4) Uiso 1 1 d D . . H11A H 1.1122 -0.0676 0.5050 0.066 Uiso 1 1 calc R . . H11B H 1.0430 -0.1265 0.4602 0.066 Uiso 1 1 calc R . . C12 C 1.2357(12) -0.1413(6) 0.4978(5) 0.073(4) Uiso 1 1 d D . . H12A H 1.2513 -0.1757 0.4679 0.088 Uiso 1 1 calc R . . H12B H 1.3233 -0.1165 0.5114 0.088 Uiso 1 1 calc R . . C13 C 1.1965(11) -0.1675(6) 0.5430(5) 0.055(4) Uiso 1 1 d D . . H13A H 1.1089 -0.1922 0.5293 0.066 Uiso 1 1 calc R . . H13B H 1.1808 -0.1331 0.5728 0.066 Uiso 1 1 calc R . . C14 C 1.3011(12) -0.2073(6) 0.5660(5) 0.070(4) Uiso 1 1 d D . . H14A H 1.3906 -0.1838 0.5769 0.084 Uiso 1 1 calc R . . H14B H 1.3111 -0.2436 0.5369 0.084 Uiso 1 1 calc R . . C15 C 1.2665(12) -0.2295(6) 0.6145(5) 0.068(4) Uiso 1 1 d D . . H15A H 1.1777 -0.2538 0.6037 0.082 Uiso 1 1 calc R . . H15B H 1.2560 -0.1934 0.6437 0.082 Uiso 1 1 calc R . . C16 C 1.3754(14) -0.2691(7) 0.6370(6) 0.090(5) Uiso 1 1 d D . . H16A H 1.3821 -0.3061 0.6081 0.108 Uiso 1 1 calc R . . H16B H 1.4649 -0.2456 0.6455 0.108 Uiso 1 1 calc R . . C17 C 1.3494(16) -0.2893(8) 0.6868(6) 0.116(6) Uiso 1 1 d D . . H17A H 1.4239 -0.3142 0.6984 0.174 Uiso 1 1 calc R . . H17B H 1.2624 -0.3139 0.6786 0.174 Uiso 1 1 calc R . . H17C H 1.3449 -0.2531 0.7161 0.174 Uiso 1 1 calc R . . C18 C 0.8223(11) 0.2435(6) 0.0875(4) 0.048(3) Uiso 1 1 d D . . H18A H 0.7551 0.2704 0.0740 0.073 Uiso 1 1 calc R . . H18B H 0.8173 0.2043 0.0606 0.073 Uiso 1 1 calc R . . H18C H 0.9144 0.2632 0.0933 0.073 Uiso 1 1 calc R . . C19 C 0.6490(9) 0.2032(6) 0.1314(5) 0.057(4) Uiso 1 1 d D . . H19A H 0.6286 0.1963 0.1659 0.085 Uiso 1 1 calc R . . H19B H 0.6420 0.1639 0.1047 0.085 Uiso 1 1 calc R . . H19C H 0.5835 0.2308 0.1179 0.085 Uiso 1 1 calc R . . C20 C 0.7965(12) 0.2923(6) 0.1814(5) 0.064(4) Uiso 1 1 d D . . H20A H 0.7754 0.2844 0.2156 0.097 Uiso 1 1 calc R . . H20B H 0.7289 0.3188 0.1676 0.097 Uiso 1 1 calc R . . H20C H 0.8881 0.3126 0.1880 0.097 Uiso 1 1 calc R . . N21 N 0.2898(8) 0.0233(4) 0.0874(4) 0.047(3) Uiso 1 1 d D . . C22 C 0.3456(13) 0.0107(6) 0.1399(4) 0.073(5) Uiso 1 1 d D . . H22A H 0.4314 -0.0106 0.1365 0.088 Uiso 1 1 calc R . . H22B H 0.2799 -0.0176 0.1492 0.088 Uiso 1 1 calc R . . C23 C 0.3754(16) 0.0678(7) 0.1863(5) 0.105(6) Uiso 1 1 d D . . H23A H 0.2909 0.0895 0.1918 0.127 Uiso 1 1 calc R . . H23B H 0.4438 0.0965 0.1791 0.127 Uiso 1 1 calc R . . C24 C 0.4332(17) 0.0418(8) 0.2372(6) 0.125(7) Uiso 1 1 d D . . H24A H 0.3597 0.0156 0.2444 0.150 Uiso 1 1 calc R . . H24B H 0.5082 0.0150 0.2277 0.150 Uiso 1 1 calc R . . C25 C 0.4842(17) 0.0863(7) 0.2865(6) 0.122(7) Uiso 1 1 d D . . H25A H 0.4077 0.1022 0.3052 0.147 Uiso 1 1 calc R . . H25B H 0.5341 0.1212 0.2786 0.147 Uiso 1 1 calc R . . C26 C 0.5800(13) 0.0534(7) 0.3219(6) 0.089(5) Uiso 1 1 d D . . H26A H 0.6334 0.0269 0.2973 0.107 Uiso 1 1 calc R . . H26B H 0.6457 0.0854 0.3463 0.107 Uiso 1 1 calc R . . C27 C 0.5324(12) 0.0146(6) 0.3567(5) 0.072(4) Uiso 1 1 d D . . H27A H 0.4690 -0.0190 0.3333 0.087 Uiso 1 1 calc R . . H27B H 0.4801 0.0401 0.3824 0.087 Uiso 1 1 calc R . . C28 C 0.6468(12) -0.0137(7) 0.3893(5) 0.078(5) Uiso 1 1 d D . . H28A H 0.6903 -0.0439 0.3635 0.093 Uiso 1 1 calc R . . H28B H 0.7174 0.0192 0.4085 0.093 Uiso 1 1 calc R . . C29 C 0.6012(12) -0.0453(6) 0.4304(5) 0.069(4) Uiso 1 1 d D . . H29A H 0.5692 -0.0140 0.4589 0.083 Uiso 1 1 calc R . . H29B H 0.5222 -0.0743 0.4120 0.083 Uiso 1 1 calc R . . C30 C 0.7098(12) -0.0801(6) 0.4572(5) 0.073(4) Uiso 1 1 d D . . H30A H 0.7894 -0.0513 0.4751 0.088 Uiso 1 1 calc R . . H30B H 0.7407 -0.1120 0.4287 0.088 Uiso 1 1 calc R . . C31 C 0.6633(12) -0.1107(6) 0.4989(5) 0.071(4) Uiso 1 1 d D . . H31A H 0.6364 -0.0785 0.5281 0.085 Uiso 1 1 calc R . . H31B H 0.5808 -0.1378 0.4813 0.085 Uiso 1 1 calc R . . C32 C 0.7677(12) -0.1481(6) 0.5242(5) 0.066(4) Uiso 1 1 d D . . H32A H 0.7958 -0.1798 0.4949 0.079 Uiso 1 1 calc R . . H32B H 0.8496 -0.1208 0.5424 0.079 Uiso 1 1 calc R . . C33 C 0.7208(12) -0.1793(6) 0.5648(5) 0.072(4) Uiso 1 1 d D . . H33A H 0.6391 -0.2067 0.5468 0.086 Uiso 1 1 calc R . . H33B H 0.6931 -0.1477 0.5943 0.086 Uiso 1 1 calc R . . C34 C 0.8282(12) -0.2167(6) 0.5897(5) 0.072(4) Uiso 1 1 d D . . H34A H 0.8528 -0.2496 0.5605 0.086 Uiso 1 1 calc R . . H34B H 0.9116 -0.1898 0.6063 0.086 Uiso 1 1 calc R . . C35 C 0.7823(12) -0.2457(6) 0.6325(5) 0.066(4) Uiso 1 1 d D . . H35A H 0.6974 -0.2717 0.6163 0.080 Uiso 1 1 calc R . . H35B H 0.7605 -0.2128 0.6623 0.080 Uiso 1 1 calc R . . C36 C 0.8892(13) -0.2850(7) 0.6563(6) 0.087(5) Uiso 1 1 d D . . H36A H 0.9090 -0.3187 0.6267 0.104 Uiso 1 1 calc R . . H36B H 0.9750 -0.2594 0.6716 0.104 Uiso 1 1 calc R . . C37 C 0.8453(15) -0.3120(8) 0.6995(6) 0.103(6) Uiso 1 1 d D . . H37A H 0.9178 -0.3366 0.7131 0.154 Uiso 1 1 calc R . . H37B H 0.7615 -0.3383 0.6845 0.154 Uiso 1 1 calc R . . H37C H 0.8277 -0.2789 0.7294 0.154 Uiso 1 1 calc R . . C38 C 0.2697(13) -0.0385(6) 0.0460(5) 0.079(5) Uiso 1 1 d D . . H38A H 0.2311 -0.0321 0.0101 0.119 Uiso 1 1 calc R . . H38B H 0.2070 -0.0660 0.0570 0.119 Uiso 1 1 calc R . . H38C H 0.3582 -0.0570 0.0444 0.119 Uiso 1 1 calc R . . C39 C 0.1508(9) 0.0479(6) 0.0858(5) 0.051(4) Uiso 1 1 d D . . H39A H 0.1185 0.0552 0.0496 0.077 Uiso 1 1 calc R . . H39B H 0.1551 0.0866 0.1131 0.077 Uiso 1 1 calc R . . H39C H 0.0874 0.0180 0.0935 0.077 Uiso 1 1 calc R . . C40 C 0.3821(11) 0.0630(6) 0.0674(5) 0.052(4) Uiso 1 1 d D . . H40A H 0.3379 0.0696 0.0322 0.077 Uiso 1 1 calc R . . H40B H 0.4679 0.0429 0.0632 0.077 Uiso 1 1 calc R . . H40C H 0.4014 0.1026 0.0936 0.077 Uiso 1 1 calc R . . N41 N 0.7815(9) 0.5234(5) 0.0887(4) 0.055(3) Uiso 1 1 d D . . C42 C 0.7669(13) 0.5147(6) 0.1428(5) 0.068(4) Uiso 1 1 d D . . H42A H 0.8341 0.4852 0.1528 0.081 Uiso 1 1 calc R . . H42B H 0.6744 0.4957 0.1406 0.081 Uiso 1 1 calc R . . C43 C 0.7866(16) 0.5716(7) 0.1870(5) 0.105(6) Uiso 1 1 d D . . H43A H 0.7388 0.6040 0.1718 0.126 Uiso 1 1 calc R . . H43B H 0.8855 0.5840 0.1943 0.126 Uiso 1 1 calc R . . C44 C 0.7429(18) 0.5742(9) 0.2428(6) 0.134(7) Uiso 1 1 d D . . H44A H 0.7531 0.6174 0.2639 0.161 Uiso 1 1 calc R . . H44B H 0.6449 0.5606 0.2369 0.161 Uiso 1 1 calc R . . C45 C 0.821(2) 0.5367(10) 0.2738(7) 0.172(10) Uiso 1 1 d D . . H45A H 0.9183 0.5519 0.2809 0.207 Uiso 1 1 calc R . . H45B H 0.8150 0.4942 0.2515 0.207 Uiso 1 1 calc R . . C46 C 0.7779(15) 0.5348(8) 0.3280(6) 0.105(6) Uiso 1 1 d D . . H46A H 0.7930 0.5761 0.3527 0.126 Uiso 1 1 calc R . . H46B H 0.6793 0.5221 0.3223 0.126 Uiso 1 1 calc R . . C47 C 0.8614(16) 0.4895(8) 0.3526(6) 0.113(6) Uiso 1 1 d D . . H47A H 0.9581 0.5056 0.3612 0.136 Uiso 1 1 calc R . . H47B H 0.8564 0.4507 0.3245 0.136 Uiso 1 1 calc R . . C48 C 0.8234(15) 0.4743(8) 0.4031(6) 0.107(6) Uiso 1 1 d D . . H48A H 0.8308 0.5126 0.4318 0.128 Uiso 1 1 calc R . . H48B H 0.7265 0.4584 0.3950 0.128 Uiso 1 1 calc R . . C49 C 0.9084(15) 0.4285(8) 0.4246(6) 0.108(6) Uiso 1 1 d D . . H49A H 1.0051 0.4445 0.4323 0.129 Uiso 1 1 calc R . . H49B H 0.9013 0.3905 0.3955 0.129 Uiso 1 1 calc R . . C50 C 0.8752(15) 0.4113(7) 0.4748(6) 0.102(6) Uiso 1 1 d D . . H50A H 0.8794 0.4494 0.5035 0.123 Uiso 1 1 calc R . . H50B H 0.7795 0.3939 0.4667 0.123 Uiso 1 1 calc R . . C51 C 0.9629(15) 0.3672(7) 0.4969(6) 0.102(6) Uiso 1 1 d D . . H51A H 1.0584 0.3849 0.5051 0.123 Uiso 1 1 calc R . . H51B H 0.9594 0.3293 0.4679 0.123 Uiso 1 1 calc R . . C52 C 0.9308(15) 0.3490(8) 0.5468(6) 0.105(6) Uiso 1 1 d D . . H52A H 0.9324 0.3868 0.5757 0.126 Uiso 1 1 calc R . . H52B H 0.8362 0.3302 0.5384 0.126 Uiso 1 1 calc R . . C53 C 1.0222(16) 0.3058(8) 0.5687(7) 0.112(6) Uiso 1 1 d D . . H53A H 1.1163 0.3252 0.5780 0.135 Uiso 1 1 calc R . . H53B H 1.0227 0.2686 0.5394 0.135 Uiso 1 1 calc R . . C54 C 0.9878(16) 0.2859(8) 0.6181(7) 0.117(7) Uiso 1 1 d D . . H54A H 0.9807 0.3233 0.6464 0.140 Uiso 1 1 calc R . . H54B H 0.8963 0.2640 0.6079 0.140 Uiso 1 1 calc R . . C55 C 1.0852(17) 0.2453(9) 0.6430(7) 0.141(8) Uiso 1 1 d D . . H55A H 1.1720 0.2702 0.6583 0.169 Uiso 1 1 calc R . . H55B H 1.1048 0.2122 0.6129 0.169 Uiso 1 1 calc R . . C56 C 1.050(2) 0.2145(9) 0.6872(9) 0.168(9) Uiso 1 1 d D . . H56A H 0.9690 0.1854 0.6719 0.201 Uiso 1 1 calc R . . H56B H 1.1273 0.1907 0.6988 0.201 Uiso 1 1 calc R . . C57 C 1.020(3) 0.2586(13) 0.7341(10) 0.238(14) Uiso 1 1 d D . . C58 C 0.6728(10) 0.5623(6) 0.0673(5) 0.054(4) Uiso 1 1 d D . . H58A H 0.6867 0.5671 0.0313 0.081 Uiso 1 1 calc R . . H58B H 0.6789 0.6028 0.0922 0.081 Uiso 1 1 calc R . . H58C H 0.5823 0.5422 0.0644 0.081 Uiso 1 1 calc R . . C59 C 0.9192(9) 0.5531(6) 0.0881(5) 0.051(4) Uiso 1 1 d D . . H59A H 0.9243 0.5579 0.0512 0.077 Uiso 1 1 calc R . . H59B H 0.9917 0.5272 0.0993 0.077 Uiso 1 1 calc R . . H59C H 0.9311 0.5936 0.1132 0.077 Uiso 1 1 calc R . . C60 C 0.7657(12) 0.4621(6) 0.0478(5) 0.068(4) Uiso 1 1 d D . . H60A H 0.7764 0.4686 0.0120 0.102 Uiso 1 1 calc R . . H60B H 0.6747 0.4428 0.0457 0.102 Uiso 1 1 calc R . . H60C H 0.8358 0.4353 0.0594 0.102 Uiso 1 1 calc R . . N61 N 0.3042(8) 0.7267(4) 0.1328(4) 0.044(3) Uiso 1 1 d D . . C62 C 0.326(2) 0.7842(9) 0.1813(7) 0.052(8) Uiso 0.535(18) 1 d PD A 1 C62' C 0.4251(17) 0.7292(10) 0.1769(7) 0.029(7) Uiso 0.465(18) 1 d PD A 2 C63 C 0.3814(15) 0.7640(8) 0.2319(6) 0.088(5) Uiso 1 1 d D . . C64 C 0.526(3) 0.7704(16) 0.2698(13) 0.280(17) Uiso 1 1 d D A . C65 C 0.489(3) 0.8118(15) 0.3235(14) 0.280(17) Uiso 1 1 d D . . C66 C 0.4437(19) 0.7719(10) 0.3593(8) 0.136(8) Uiso 1 1 d D A . H66A H 0.4065 0.7997 0.3888 0.163 Uiso 1 1 calc R . . H66B H 0.3658 0.7446 0.3371 0.163 Uiso 1 1 calc R . . C67 C 0.537(2) 0.7324(10) 0.3856(9) 0.158(9) Uiso 1 1 d D . . H67A H 0.6221 0.7573 0.4044 0.190 Uiso 1 1 calc R A . H67B H 0.5628 0.6991 0.3570 0.190 Uiso 1 1 calc R . . C68 C 0.4801(17) 0.7045(9) 0.4254(8) 0.125(7) Uiso 1 1 d D A . H68A H 0.4520 0.7381 0.4532 0.150 Uiso 1 1 calc R . . H68B H 0.3962 0.6792 0.4062 0.150 Uiso 1 1 calc R . . C69 C 0.5697(17) 0.6657(9) 0.4541(7) 0.121(7) Uiso 1 1 d D . . H69A H 0.5944 0.6318 0.4258 0.145 Uiso 1 1 calc R A . H69B H 0.6553 0.6909 0.4710 0.145 Uiso 1 1 calc R . . C70 C 0.5276(19) 0.6376(10) 0.4960(8) 0.150(8) Uiso 1 1 d D A . H70A H 0.4423 0.6121 0.4791 0.180 Uiso 1 1 calc R . . H70B H 0.5030 0.6714 0.5244 0.180 Uiso 1 1 calc R . . C71 C 0.6204(15) 0.5987(8) 0.5243(7) 0.101(6) Uiso 1 1 d D . . H71A H 0.6472 0.5655 0.4959 0.122 Uiso 1 1 calc R A . H71B H 0.7047 0.6245 0.5422 0.122 Uiso 1 1 calc R . . C72 C 0.5756(18) 0.5696(9) 0.5651(8) 0.137(8) Uiso 1 1 d D A . H72A H 0.4933 0.5427 0.5468 0.164 Uiso 1 1 calc R . . H72B H 0.5453 0.6027 0.5927 0.164 Uiso 1 1 calc R . . C73 C 0.6670(15) 0.5328(8) 0.5948(7) 0.096(5) Uiso 1 1 d D . . H73A H 0.7491 0.5596 0.6136 0.115 Uiso 1 1 calc R A . H73B H 0.6978 0.4997 0.5675 0.115 Uiso 1 1 calc R . . C74 C 0.6173(17) 0.5036(9) 0.6357(7) 0.127(7) Uiso 1 1 d D A . H74A H 0.5917 0.5369 0.6644 0.152 Uiso 1 1 calc R . . H74B H 0.5323 0.4785 0.6176 0.152 Uiso 1 1 calc R . . C75 C 0.7082(15) 0.4643(8) 0.6629(7) 0.093(5) Uiso 1 1 d D . . H75A H 0.7340 0.4313 0.6341 0.112 Uiso 1 1 calc R A . H75B H 0.7931 0.4896 0.6809 0.112 Uiso 1 1 calc R . . C76 C 0.6620(19) 0.4348(10) 0.7035(8) 0.158(9) Uiso 1 1 d D A . H76A H 0.5769 0.4101 0.6848 0.190 Uiso 1 1 calc R . . H76B H 0.6347 0.4684 0.7314 0.190 Uiso 1 1 calc R . . C77 C 0.7476(15) 0.3931(8) 0.7350(7) 0.104(6) Uiso 1 1 d D . . H77A H 0.6932 0.3787 0.7591 0.155 Uiso 1 1 calc R A . H77B H 0.8303 0.4164 0.7567 0.155 Uiso 1 1 calc R . . H77C H 0.7736 0.3576 0.7092 0.155 Uiso 1 1 calc R . . C78 C 0.1879(11) 0.6860(6) 0.1403(5) 0.048(3) Uiso 1 1 d D A . C79 C 0.4413(17) 0.7022(11) 0.1281(9) 0.047(8) Uiso 0.535(18) 1 d PD A 1 C80 C 0.2569(19) 0.7607(10) 0.0897(8) 0.038(7) Uiso 0.535(18) 1 d PD A 1 C79' C 0.346(2) 0.6909(11) 0.0803(8) 0.045(8) Uiso 0.465(18) 1 d PD A 2 C80' C 0.262(2) 0.7888(10) 0.1248(12) 0.047(8) Uiso 0.465(18) 1 d PD A 2 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 0.0442(6) 0.0286(7) 0.0428(8) 0.0102(6) 0.0123(5) -0.0032(5) Mo2 0.0394(6) 0.0269(7) 0.0470(8) 0.0102(6) 0.0051(5) -0.0064(5) Mo3 0.0472(6) 0.0227(7) 0.0515(8) 0.0135(6) 0.0095(6) -0.0020(5) Mo4 0.0425(6) 0.0293(7) 0.0471(8) 0.0127(6) 0.0011(6) -0.0057(5) Mo5 0.0445(6) 0.0197(7) 0.0528(8) 0.0111(6) 0.0087(6) -0.0041(5) Mo6 0.0494(7) 0.0344(8) 0.0457(8) 0.0093(6) 0.0172(6) -0.0037(5) Mo7 0.0555(7) 0.0292(8) 0.0548(8) 0.0089(7) 0.0128(6) 0.0009(6) Mo8 0.0512(7) 0.0319(8) 0.0724(10) 0.0119(7) -0.0129(7) -0.0041(6) Mo9 0.0510(7) 0.0210(7) 0.0727(9) 0.0143(7) 0.0104(6) -0.0008(5) Mo10 0.0428(6) 0.0330(8) 0.0491(8) 0.0116(6) 0.0039(6) -0.0009(5) Mo11 0.0478(7) 0.0211(7) 0.0592(8) 0.0124(6) 0.0035(6) -0.0029(5) Mo12 0.0455(7) 0.0252(7) 0.0726(9) 0.0111(7) 0.0152(6) -0.0009(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 Mo1 O14 1.683(8) . ? Mo1 O4 1.884(7) . ? Mo1 O3 1.898(8) . ? Mo1 O2 1.953(7) . ? Mo1 O5 1.971(7) . ? Mo1 O1 2.302(8) . ? Mo2 O15 1.683(7) . ? Mo2 O2 1.894(7) . ? Mo2 O6 1.927(8) . ? Mo2 O9 1.929(8) . ? Mo2 O10 1.937(8) . ? Mo2 O1 2.310(7) . ? Mo3 O16 1.677(9) . ? Mo3 O11 1.894(8) . ? Mo3 O6 1.898(7) . ? Mo3 O7 1.938(7) . ? Mo3 O3 1.939(8) . ? Mo3 O1 2.330(9) . ? Mo4 O17 1.675(7) . ? Mo4 O12 1.878(8) . ? Mo4 O7 1.909(8) . ? Mo4 O8 1.942(7) . ? Mo4 O4 1.972(8) . ? Mo4 O1 2.323(7) . ? Mo5 O18 1.684(8) . ? Mo5 O5 1.893(7) . ? Mo5 O8 1.894(6) . ? Mo5 O13 1.922(8) . ? Mo5 O9 1.940(7) . ? Mo5 O1 2.305(9) . ? Mo6 O19 1.680(8) . ? Mo6 O10 1.908(7) . ? Mo6 O13 1.911(8) . ? Mo6 O11 1.947(8) . ? Mo6 O12 1.949(7) . ? Mo6 O1 2.335(8) . ? Mo7 O33 1.677(9) . ? Mo7 O21 1.860(7) . ? Mo7 O22 1.900(9) . ? Mo7 O24 1.952(8) . ? Mo7 O23 1.965(7) . ? Mo7 O20 2.318(8) . ? Mo8 O34 1.687(8) . ? Mo8 O29 1.891(8) . ? Mo8 O25 1.916(9) . ? Mo8 O28 1.960(9) . ? Mo8 O21 1.977(7) . ? Mo8 O20 2.323(7) . ? Mo9 O35 1.682(9) . ? Mo9 O30 1.886(8) . ? Mo9 O26 1.894(7) . ? Mo9 O25 1.934(8) . ? Mo9 O22 1.951(8) . ? Mo9 O20 2.293(9) . ? Mo10 O36 1.680(7) . ? Mo10 O23 1.872(7) . ? Mo10 O27 1.873(8) . ? Mo10 O31 1.930(7) . ? Mo10 O26 1.983(8) . ? Mo10 O20 2.317(7) . ? Mo11 O37 1.689(9) . ? Mo11 O28 1.870(8) . ? Mo11 O24 1.899(8) . ? Mo11 O32 1.945(8) . ? Mo11 O27 1.951(7) . ? Mo11 O20 2.344(9) . ? Mo12 O38 1.699(8) . ? Mo12 O31 1.875(7) . ? Mo12 O32 1.886(8) . ? Mo12 O29 1.963(8) . ? Mo12 O30 1.976(9) . ? Mo12 O20 2.303(8) . ? N1 C2 1.488(9) . ? N1 C18 1.498(10) . ? N1 C19 1.505(10) . ? N1 C20 1.513(12) . ? C2 C3 1.515(10) . ? C3 C4 1.541(10) . ? C4 C5 1.488(11) . ? C5 C6 1.510(10) . ? C6 C7 1.508(11) . ? C7 C8 1.533(10) . ? C8 C9 1.524(11) . ? C9 C10 1.506(10) . ? C10 C11 1.519(11) . ? C11 C12 1.518(10) . ? C12 C13 1.504(11) . ? C13 C14 1.513(10) . ? C14 C15 1.519(11) . ? C15 C16 1.530(11) . ? C16 C17 1.501(12) . ? N21 C22 1.459(10) . ? N21 C40 1.482(12) . ? N21 C39 1.491(9) . ? N21 C38 1.531(10) . ? C22 C23 1.526(11) . ? C23 C24 1.571(11) . ? C24 C25 1.434(12) . ? C25 C26 1.520(11) . ? C26 C27 1.491(11) . ? C27 C28 1.531(10) . ? C28 C29 1.507(11) . ? C29 C30 1.507(10) . ? C30 C31 1.511(11) . ? C31 C32 1.500(10) . ? C32 C33 1.496(11) . ? C33 C34 1.515(10) . ? C34 C35 1.512(11) . ? C35 C36 1.528(10) . ? C36 C37 1.486(12) . ? N41 C42 1.470(10) . ? N41 C58 1.508(9) . ? N41 C59 1.509(10) . ? N41 C60 1.516(12) . ? C42 C43 1.488(11) . ? C43 C44 1.546(12) . ? C44 C45 1.435(12) . ? C45 C46 1.522(12) . ? C46 C47 1.501(11) . ? C47 C48 1.507(12) . ? C48 C49 1.482(11) . ? C49 C50 1.500(11) . ? C50 C51 1.474(11) . ? C51 C52 1.501(11) . ? C52 C53 1.475(11) . ? C53 C54 1.514(12) . ? C54 C55 1.502(11) . ? C55 C56 1.527(12) . ? C56 C57 1.449(13) . ? N61 C79 1.488(15) . ? N61 C80 1.496(15) . ? N61 C62 1.500(15) . ? N61 C80 1.506(17) . ? N61 C78 1.515(12) . ? N61 C79 1.525(16) . ? N61 C62 1.558(16) . ? C62 C63 1.490(16) . ? C62 C63 1.580(16) . ? C63 C64 1.579(17) . ? C64 C65 1.578(18) . ? C65 C66 1.521(18) . ? C66 C67 1.478(15) . ? C67 C68 1.483(16) . ? C68 C69 1.478(14) . ? C69 C70 1.464(15) . ? C70 C71 1.493(14) . ? C71 C72 1.464(15) . ? C72 C73 1.470(14) . ? C73 C74 1.488(15) . ? C74 C75 1.473(14) . ? C75 C76 1.471(15) . ? C76 C77 1.545(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 O14 Mo1 O4 103.7(3) . . ? O14 Mo1 O3 105.7(4) . . ? O4 Mo1 O3 88.8(3) . . ? O14 Mo1 O2 102.8(3) . . ? O4 Mo1 O2 153.3(3) . . ? O3 Mo1 O2 87.1(3) . . ? O14 Mo1 O5 101.7(3) . . ? O4 Mo1 O5 87.8(3) . . ? O3 Mo1 O5 152.5(3) . . ? O2 Mo1 O5 83.8(3) . . ? O14 Mo1 O1 177.1(3) . . ? O4 Mo1 O1 77.2(3) . . ? O3 Mo1 O1 77.1(3) . . ? O2 Mo1 O1 76.2(3) . . ? O5 Mo1 O1 75.5(3) . . ? O15 Mo2 O2 104.4(3) . . ? O15 Mo2 O6 104.5(3) . . ? O2 Mo2 O6 89.0(3) . . ? O15 Mo2 O9 102.2(3) . . ? O2 Mo2 O9 88.3(3) . . ? O6 Mo2 O9 153.0(3) . . ? O15 Mo2 O10 102.4(3) . . ? O2 Mo2 O10 153.1(3) . . ? O6 Mo2 O10 85.5(3) . . ? O9 Mo2 O10 84.9(3) . . ? O15 Mo2 O1 178.1(3) . . ? O2 Mo2 O1 77.1(3) . . ? O6 Mo2 O1 76.6(3) . . ? O9 Mo2 O1 76.6(3) . . ? O10 Mo2 O1 76.0(3) . . ? O16 Mo3 O11 103.0(4) . . ? O16 Mo3 O6 104.9(4) . . ? O11 Mo3 O6 87.6(3) . . ? O16 Mo3 O7 102.3(3) . . ? O11 Mo3 O7 87.2(3) . . ? O6 Mo3 O7 152.8(3) . . ? O16 Mo3 O3 104.1(4) . . ? O11 Mo3 O3 152.9(3) . . ? O6 Mo3 O3 87.0(3) . . ? O7 Mo3 O3 85.6(3) . . ? O16 Mo3 O1 178.5(3) . . ? O11 Mo3 O1 77.2(3) . . ? O6 Mo3 O1 76.6(3) . . ? O7 Mo3 O1 76.2(3) . . ? O3 Mo3 O1 75.7(3) . . ? O17 Mo4 O12 105.6(4) . . ? O17 Mo4 O7 103.0(3) . . ? O12 Mo4 O7 89.1(3) . . ? O17 Mo4 O8 104.2(3) . . ? O12 Mo4 O8 88.8(3) . . ? O7 Mo4 O8 152.3(3) . . ? O17 Mo4 O4 101.3(3) . . ? O12 Mo4 O4 153.0(3) . . ? O7 Mo4 O4 85.6(3) . . ? O8 Mo4 O4 83.9(3) . . ? O17 Mo4 O1 176.4(3) . . ? O12 Mo4 O1 77.9(3) . . ? O7 Mo4 O1 76.9(3) . . ? O8 Mo4 O1 75.6(3) . . ? O4 Mo4 O1 75.1(3) . . ? O18 Mo5 O5 103.3(3) . . ? O18 Mo5 O8 104.7(3) . . ? O5 Mo5 O8 87.7(3) . . ? O18 Mo5 O13 102.9(4) . . ? O5 Mo5 O13 153.7(3) . . ? O8 Mo5 O13 88.0(3) . . ? O18 Mo5 O9 101.8(3) . . ? O5 Mo5 O9 86.6(3) . . ? O8 Mo5 O9 153.4(3) . . ? O13 Mo5 O9 85.7(3) . . ? O18 Mo5 O1 178.3(3) . . ? O5 Mo5 O1 76.9(3) . . ? O8 Mo5 O1 76.9(3) . . ? O13 Mo5 O1 76.9(3) . . ? O9 Mo5 O1 76.5(3) . . ? O19 Mo6 O10 104.1(3) . . ? O19 Mo6 O13 104.4(4) . . ? O10 Mo6 O13 87.6(3) . . ? O19 Mo6 O11 103.1(4) . . ? O10 Mo6 O11 87.0(3) . . ? O13 Mo6 O11 152.4(3) . . ? O19 Mo6 O12 103.5(3) . . ? O10 Mo6 O12 152.3(3) . . ? O13 Mo6 O12 86.6(3) . . ? O11 Mo6 O12 85.6(3) . . ? O19 Mo6 O1 179.2(4) . . ? O10 Mo6 O1 75.9(3) . . ? O13 Mo6 O1 76.3(3) . . ? O11 Mo6 O1 76.1(3) . . ? O12 Mo6 O1 76.3(3) . . ? Mo1 O1 Mo5 91.0(3) . . ? Mo1 O1 Mo2 90.3(3) . . ? Mo5 O1 Mo2 90.7(3) . . ? Mo1 O1 Mo4 90.6(3) . . ? Mo5 O1 Mo4 90.1(3) . . ? Mo2 O1 Mo4 178.8(4) . . ? Mo1 O1 Mo3 90.0(3) . . ? Mo5 O1 Mo3 179.0(4) . . ? Mo2 O1 Mo3 89.5(3) . . ? Mo4 O1 Mo3 89.7(2) . . ? Mo1 O1 Mo6 179.2(4) . . ? Mo5 O1 Mo6 89.6(3) . . ? Mo2 O1 Mo6 90.2(3) . . ? Mo4 O1 Mo6 88.9(3) . . ? Mo3 O1 Mo6 89.4(3) . . ? Mo2 O2 Mo1 116.4(4) . . ? Mo1 O3 Mo3 117.2(4) . . ? Mo1 O4 Mo4 117.0(3) . . ? Mo5 O5 Mo1 116.5(4) . . ? Mo3 O6 Mo2 117.3(4) . . ? Mo4 O7 Mo3 117.1(3) . . ? Mo5 O8 Mo4 117.2(4) . . ? Mo2 O9 Mo5 116.1(3) . . ? Mo6 O10 Mo2 117.8(3) . . ? Mo3 O11 Mo6 117.3(4) . . ? Mo4 O12 Mo6 116.9(4) . . ? Mo6 O13 Mo5 117.1(4) . . ? O33 Mo7 O21 104.2(4) . . ? O33 Mo7 O22 103.2(4) . . ? O21 Mo7 O22 90.7(3) . . ? O33 Mo7 O24 102.9(4) . . ? O21 Mo7 O24 87.8(3) . . ? O22 Mo7 O24 153.4(3) . . ? O33 Mo7 O23 102.5(3) . . ? O21 Mo7 O23 153.2(3) . . ? O22 Mo7 O23 85.7(3) . . ? O24 Mo7 O23 83.8(3) . . ? O33 Mo7 O20 177.5(3) . . ? O21 Mo7 O20 78.3(3) . . ? O22 Mo7 O20 77.0(3) . . ? O24 Mo7 O20 76.6(3) . . ? O23 Mo7 O20 75.0(3) . . ? O34 Mo8 O29 103.3(4) . . ? O34 Mo8 O25 104.2(4) . . ? O29 Mo8 O25 89.3(4) . . ? O34 Mo8 O28 103.7(4) . . ? O29 Mo8 O28 86.6(4) . . ? O25 Mo8 O28 152.0(3) . . ? O34 Mo8 O21 104.1(4) . . ? O29 Mo8 O21 152.4(3) . . ? O25 Mo8 O21 86.4(3) . . ? O28 Mo8 O21 84.6(3) . . ? O34 Mo8 O20 179.6(4) . . ? O29 Mo8 O20 76.6(3) . . ? O25 Mo8 O20 76.1(3) . . ? O28 Mo8 O20 76.0(3) . . ? O21 Mo8 O20 76.0(3) . . ? O35 Mo9 O30 102.7(4) . . ? O35 Mo9 O26 102.7(4) . . ? O30 Mo9 O26 89.2(3) . . ? O35 Mo9 O25 103.0(4) . . ? O30 Mo9 O25 87.1(3) . . ? O26 Mo9 O25 154.2(4) . . ? O35 Mo9 O22 103.3(4) . . ? O30 Mo9 O22 153.9(4) . . ? O26 Mo9 O22 87.4(3) . . ? O25 Mo9 O22 84.8(3) . . ? O35 Mo9 O20 179.6(4) . . ? O30 Mo9 O20 77.3(3) . . ? O26 Mo9 O20 77.8(3) . . ? O25 Mo9 O20 76.5(3) . . ? O22 Mo9 O20 76.7(3) . . ? O36 Mo10 O23 103.9(3) . . ? O36 Mo10 O27 106.6(4) . . ? O23 Mo10 O27 89.6(3) . . ? O36 Mo10 O31 103.8(3) . . ? O23 Mo10 O31 151.9(3) . . ? O27 Mo10 O31 87.1(3) . . ? O36 Mo10 O26 100.6(4) . . ? O23 Mo10 O26 86.8(3) . . ? O27 Mo10 O26 152.7(3) . . ? O31 Mo10 O26 83.6(3) . . ? O36 Mo10 O20 176.1(4) . . ? O23 Mo10 O20 76.7(3) . . ? O27 Mo10 O20 77.2(3) . . ? O31 Mo10 O20 75.4(3) . . ? O26 Mo10 O20 75.6(3) . . ? O37 Mo11 O28 103.7(4) . . ? O37 Mo11 O24 103.5(4) . . ? O28 Mo11 O24 90.0(3) . . ? O37 Mo11 O32 103.8(4) . . ? O28 Mo11 O32 86.1(3) . . ? O24 Mo11 O32 152.6(3) . . ? O37 Mo11 O27 104.0(3) . . ? O28 Mo11 O27 152.1(3) . . ? O24 Mo11 O27 85.9(3) . . ? O32 Mo11 O27 85.0(3) . . ? O37 Mo11 O20 179.1(3) . . ? O28 Mo11 O20 77.1(3) . . ? O24 Mo11 O20 77.0(3) . . ? O32 Mo11 O20 75.7(3) . . ? O27 Mo11 O20 75.2(3) . . ? O38 Mo12 O31 106.9(4) . . ? O38 Mo12 O32 104.7(4) . . ? O31 Mo12 O32 90.8(3) . . ? O38 Mo12 O29 100.4(3) . . ? O31 Mo12 O29 152.3(3) . . ? O32 Mo12 O29 86.1(3) . . ? O38 Mo12 O30 101.8(4) . . ? O31 Mo12 O30 87.1(3) . . ? O32 Mo12 O30 152.9(3) . . ? O29 Mo12 O30 83.4(3) . . ? O38 Mo12 O20 175.4(4) . . ? O31 Mo12 O20 76.7(3) . . ? O32 Mo12 O20 77.8(3) . . ? O29 Mo12 O20 75.7(3) . . ? O30 Mo12 O20 75.4(3) . . ? Mo9 O20 Mo12 91.0(3) . . ? Mo9 O20 Mo10 90.9(3) . . ? Mo12 O20 Mo10 89.7(3) . . ? Mo9 O20 Mo7 90.2(3) . . ? Mo12 O20 Mo7 178.8(4) . . ? Mo10 O20 Mo7 90.4(3) . . ? Mo9 O20 Mo8 90.5(3) . . ? Mo12 O20 Mo8 90.6(3) . . ? Mo10 O20 Mo8 178.6(4) . . ? Mo7 O20 Mo8 89.3(3) . . ? Mo9 O20 Mo11 179.5(4) . . ? Mo12 O20 Mo11 89.4(3) . . ? Mo10 O20 Mo11 89.4(3) . . ? Mo7 O20 Mo11 89.4(3) . . ? Mo8 O20 Mo11 89.2(3) . . ? Mo7 O21 Mo8 116.4(4) . . ? Mo7 O22 Mo9 116.1(4) . . ? Mo10 O23 Mo7 117.9(3) . . ? Mo11 O24 Mo7 116.7(4) . . ? Mo8 O25 Mo9 116.7(4) . . ? Mo9 O26 Mo10 115.8(4) . . ? Mo10 O27 Mo11 118.1(4) . . ? Mo11 O28 Mo8 117.7(4) . . ? Mo8 O29 Mo12 117.1(4) . . ? Mo9 O30 Mo12 116.2(4) . . ? Mo12 O31 Mo10 117.9(4) . . ? Mo12 O32 Mo11 117.1(4) . . ? C2 N1 C18 107.7(8) . . ? C2 N1 C19 111.7(8) . . ? C18 N1 C19 109.5(8) . . ? C2 N1 C20 111.0(8) . . ? C18 N1 C20 109.9(9) . . ? C19 N1 C20 107.0(9) . . ? N1 C2 C3 114.0(8) . . ? C2 C3 C4 114.3(8) . . ? C5 C4 C3 113.1(8) . . ? C4 C5 C6 114.9(9) . . ? C7 C6 C5 113.6(9) . . ? C6 C7 C8 114.6(8) . . ? C9 C8 C7 113.7(9) . . ? C10 C9 C8 115.0(9) . . ? C9 C10 C11 114.3(9) . . ? C12 C11 C10 112.6(9) . . ? C13 C12 C11 114.1(9) . . ? C12 C13 C14 114.8(9) . . ? C13 C14 C15 114.7(10) . . ? C14 C15 C16 113.1(10) . . ? C17 C16 C15 115.0(11) . . ? C22 N21 C40 114.0(9) . . ? C22 N21 C39 113.2(9) . . ? C40 N21 C39 110.4(9) . . ? C22 N21 C38 106.9(9) . . ? C40 N21 C38 106.5(9) . . ? C39 N21 C38 105.1(8) . . ? N21 C22 C23 114.2(10) . . ? C22 C23 C24 104.0(11) . . ? C25 C24 C23 116.5(13) . . ? C24 C25 C26 106.6(12) . . ? C27 C26 C25 123.7(12) . . ? C26 C27 C28 114.8(10) . . ? C29 C28 C27 114.8(10) . . ? C30 C29 C28 114.7(10) . . ? C29 C30 C31 114.1(10) . . ? C32 C31 C30 115.0(10) . . ? C33 C32 C31 115.0(10) . . ? C32 C33 C34 113.9(10) . . ? C35 C34 C33 113.6(10) . . ? C34 C35 C36 113.5(10) . . ? C37 C36 C35 113.3(11) . . ? C42 N41 C58 112.3(9) . . ? C42 N41 C59 112.4(9) . . ? C58 N41 C59 107.8(8) . . ? C42 N41 C60 110.3(10) . . ? C58 N41 C60 106.1(9) . . ? C59 N41 C60 107.6(9) . . ? N41 C42 C43 115.3(11) . . ? C42 C43 C44 122.3(13) . . ? C45 C44 C43 113.2(13) . . ? C44 C45 C46 115.7(14) . . ? C47 C46 C45 108.6(12) . . ? C46 C47 C48 117.6(12) . . ? C49 C48 C47 114.7(12) . . ? C48 C49 C50 117.1(12) . . ? C51 C50 C49 116.8(12) . . ? C50 C51 C52 117.7(12) . . ? C53 C52 C51 116.5(12) . . ? C52 C53 C54 116.7(12) . . ? C55 C54 C53 117.3(13) . . ? C54 C55 C56 121.5(14) . . ? C57 C56 C55 112.4(17) . . ? C79 N61 C80 111.9(14) . . ? C62 N61 C80 114.1(15) . . ? C79 N61 C78 120.5(12) . . ? C80 N61 C78 110.5(10) . . ? C62 N61 C78 110.6(12) . . ? C80 N61 C78 113.6(12) . . ? C62 N61 C79 106.5(12) . . ? C80 N61 C79 108.4(16) . . ? C78 N61 C79 102.7(13) . . ? C79 N61 C62 106.7(13) . . ? C80 N61 C62 96.2(13) . . ? C78 N61 C62 108.1(11) . . ? C63 C62 N61 108.5(14) . . ? N61 C62 C63 106.9(12) . . ? C62 C63 C64 135(2) . . ? C64 C63 C62 98.5(16) . . ? C65 C64 C63 100(2) . . ? C66 C65 C64 110(3) . . ? C67 C66 C65 123(2) . . ? C66 C67 C68 114.6(17) . . ? C69 C68 C67 117.3(16) . . ? C70 C69 C68 122.6(16) . . ? C69 C70 C71 121.5(16) . . ? C72 C71 C70 120.9(15) . . ? C71 C72 C73 121.7(15) . . ? C72 C73 C74 120.1(14) . . ? C75 C74 C73 119.1(15) . . ? C76 C75 C74 120.4(14) . . ? C75 C76 C77 125.4(16) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.106 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.157 # start Validation Reply Form _vrf_PLAT026_c16_mo6 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 25 Perc. RESPONSE: ...This structure intrinsically exhibits many weak reflections at higher theta values. The submitted manuscript mainly reports the packing mode of the polymolybdate anions. The data obtained had insufficient quality, but was sufficient to elucidate the packing feature of the hexamolybdate anion. ; _vrf_PLAT029_c16_mo6 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.92 RESPONSE: ...This structure intrinsically exhibits many weak reflections at higher theta values. The data obtained had insufficient quality, but was sufficient to elucidate the packing feature of the hexamolybdate. ; _vrf_PLAT201_c16_mo6 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 118 RESPONSE: ...The data quality was not good, and significant disorder exists on surfactant cations. Therefore, atoms except for Mo were refined by using isotropic displacement parameters for the refinement. ; _vrf_PLAT220_c16_mo6 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.65 Ratio RESPONSE: ...The carbon atoms in the surfactant cations are flexible in this crystal lattice. Disorder of several carbon atoms also can affect the Ueq values. ; _vrf_PLAT241_c16_mo6 ; PROBLEM: Check High Ueq as Compared to Neighbors for C45 RESPONSE: ...The carbon atoms in the surfactant cations are flexible in this crystal lattice. Disorder of vicinal carbon atoms also can affect the Ueq values. ; _vrf_PLAT242_c16_mo6 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C66 RESPONSE: ...The carbon atoms in the surfactant cations are flexible in this crystal lattice. Disorder of vicinal carbon atoms also can affect the Ueq values. ; _vrf_PLAT701_c16_mo6 ; PROBLEM: Bond Calc 1.49(2), Rep 1.580(16), Dev.. 4.50 Sigma RESPONSE: ...Significant disorder of the carbon atom relevant to this chemical bond is considered to result in the bond length with a large deviation from normal values. ; _vrf_PLAT702_c16_mo6 ; PROBLEM: Angle Calc 96.1(12), Rep 114.1(15), Dev.. 15.00 Sigma RESPONSE: ...Significant disorder of the carbon atom relevant to this chemical bond is considered to result in the bond angle with a large deviation from normal values. ; # end Validation Reply Form