data_c16_mo8 _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 ; tetra(hexadecyltrimethylammonium) octamolybdate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 4(C19 H42 N), Mo8 O26 ; _chemical_formula_sum 'C76 H168 Mo8 N4 O26' _chemical_formula_weight 2321.66 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' '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 9.958(8) _cell_length_b 11.149(3) _cell_length_c 24.95(2) _cell_angle_alpha 98.06(4) _cell_angle_beta 94.828(7) _cell_angle_gamma 115.66(4) _cell_volume 2439(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12441 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.062 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9012 _exptl_absorpt_correction_T_max 0.9791 _exptl_absorpt_process_details ; Higashi, T. (1999). Numabs - Numerical 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 21313 _diffrn_reflns_av_R_equivalents 0.1257 _diffrn_reflns_av_sigmaI/netI 0.3289 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10383 _reflns_number_gt 3745 _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. ; _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^)+(0.0269P)^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 10383 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1779 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 0.713 _refine_ls_restrained_S_all 0.713 _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 0.35295(6) 0.17244(7) 0.49359(3) 0.02063(18) Uani 1 1 d . . . Mo2 Mo 0.50179(7) 0.38048(7) 0.61487(3) 0.02204(18) Uani 1 1 d . . . Mo3 Mo 0.68054(6) 0.49554(7) 0.49460(3) 0.01865(18) Uani 1 1 d . . . Mo4 Mo 0.65568(7) 0.72968(7) 0.63057(3) 0.0301(2) Uani 1 1 d . . . O1 O 0.3859(5) 0.0435(5) 0.46352(18) 0.0273(13) Uani 1 1 d . . . O2 O 0.1924(4) 0.0939(5) 0.52044(19) 0.0278(13) Uani 1 1 d . . . O3 O 0.2600(5) 0.2046(4) 0.42914(18) 0.0267(13) Uani 1 1 d . . . O4 O 0.5005(4) 0.2434(4) 0.55910(18) 0.0214(12) Uani 1 1 d . . . O5 O 0.3382(5) 0.2899(5) 0.63829(18) 0.0257(13) Uani 1 1 d . . . O6 O 0.6407(4) 0.3944(5) 0.66350(18) 0.0258(13) Uani 1 1 d . . . O7 O 0.5064(5) 0.5571(4) 0.63165(17) 0.0244(12) Uani 1 1 d . . . O8 O 0.5885(5) 0.8362(5) 0.65836(19) 0.0333(14) Uani 1 1 d . . . O9 O 0.8084(5) 0.7547(5) 0.6745(2) 0.0414(15) Uani 1 1 d . . . O10 O 0.6891(5) 0.5161(5) 0.56651(18) 0.0298(13) Uani 1 1 d . . . O11 O 0.6313(5) 0.6159(5) 0.46914(19) 0.0372(14) Uani 1 1 d . . . O12 O 0.8552(5) 0.5236(5) 0.47995(19) 0.0322(14) Uani 1 1 d . . . O13 O 0.5519(5) 0.3290(5) 0.46093(19) 0.0331(14) Uani 1 1 d . . . N1 N 0.2069(5) -0.1453(6) 0.6131(2) 0.0188(14) Uani 1 1 d . . . N2 N -0.0528(5) 0.2635(6) 0.6196(2) 0.0226(15) Uani 1 1 d . . . C1 C 0.3324(7) -0.1016(7) 0.5811(3) 0.028(2) Uani 1 1 d . . . H1A H 0.3424 -0.0198 0.5679 0.033 Uiso 1 1 calc R . . H1B H 0.3113 -0.1742 0.5497 0.033 Uiso 1 1 calc R . . H1C H 0.4266 -0.0818 0.6044 0.033 Uiso 1 1 calc R . . C2 C 0.0625(7) -0.1812(8) 0.5766(3) 0.040(2) Uani 1 1 d . . . H2A H -0.0210 -0.2102 0.5976 0.048 Uiso 1 1 calc R . . H2B H 0.0439 -0.2552 0.5461 0.048 Uiso 1 1 calc R . . H2C H 0.0700 -0.1016 0.5620 0.048 Uiso 1 1 calc R . . C3 C 0.1940(8) -0.2706(8) 0.6321(3) 0.045(2) Uani 1 1 d . . . H3A H 0.1121 -0.3009 0.6538 0.054 Uiso 1 1 calc R . . H3B H 0.2893 -0.2508 0.6547 0.054 Uiso 1 1 calc R . . H3C H 0.1722 -0.3422 0.6002 0.054 Uiso 1 1 calc R . . C4 C 0.2316(7) -0.0344(8) 0.6609(3) 0.031(2) Uani 1 1 d . . . H4A H 0.2246 0.0409 0.6461 0.037 Uiso 1 1 calc R . . H4B H 0.1480 -0.0705 0.6822 0.037 Uiso 1 1 calc R . . C5 C 0.3765(7) 0.0225(7) 0.6994(3) 0.033(2) Uani 1 1 d . . . H5A H 0.4618 0.0607 0.6791 0.040 Uiso 1 1 calc R . . H5B H 0.3846 -0.0509 0.7154 0.040 Uiso 1 1 calc R . . C6 C 0.3863(8) 0.1324(8) 0.7449(3) 0.040(2) Uani 1 1 d . . . H6A H 0.3066 0.0918 0.7673 0.048 Uiso 1 1 calc R . . H6B H 0.3672 0.2006 0.7286 0.048 Uiso 1 1 calc R . . C7 C 0.5383(8) 0.2024(8) 0.7817(3) 0.038(2) Uani 1 1 d . . . H7A H 0.6179 0.2376 0.7588 0.045 Uiso 1 1 calc R . . H7B H 0.5544 0.1345 0.7994 0.045 Uiso 1 1 calc R . . C8 C 0.5562(7) 0.3194(7) 0.8264(3) 0.031(2) Uani 1 1 d . . . H8A H 0.4797 0.2834 0.8504 0.037 Uiso 1 1 calc R . . H8B H 0.5353 0.3853 0.8088 0.037 Uiso 1 1 calc R . . C9 C 0.7118(8) 0.3939(8) 0.8617(3) 0.040(2) Uani 1 1 d . . . H9A H 0.7321 0.3278 0.8792 0.048 Uiso 1 1 calc R . . H9B H 0.7880 0.4287 0.8375 0.048 Uiso 1 1 calc R . . C10 C 0.7333(8) 0.5105(8) 0.9058(3) 0.032(2) Uani 1 1 d . . . H10A H 0.6607 0.4756 0.9313 0.038 Uiso 1 1 calc R . . H10B H 0.7098 0.5755 0.8887 0.038 Uiso 1 1 calc R . . C11 C 0.8923(7) 0.5850(8) 0.9385(3) 0.030(2) Uani 1 1 d . . . H11A H 0.9651 0.6162 0.9128 0.036 Uiso 1 1 calc R . . H11B H 0.9139 0.5209 0.9569 0.036 Uiso 1 1 calc R . . C12 C 0.9164(7) 0.7080(7) 0.9819(3) 0.030(2) Uani 1 1 d . . . H12A H 0.8944 0.7720 0.9634 0.036 Uiso 1 1 calc R . . H12B H 0.8433 0.6766 1.0075 0.036 Uiso 1 1 calc R . . C13 C 1.0730(7) 0.7825(8) 1.0144(3) 0.032(2) Uani 1 1 d . . . H13A H 1.1464 0.8145 0.9889 0.039 Uiso 1 1 calc R . . H13B H 1.0954 0.7188 1.0330 0.039 Uiso 1 1 calc R . . C14 C 1.0941(7) 0.9025(7) 1.0569(3) 0.028(2) Uani 1 1 d . . . H14A H 1.0201 0.8701 1.0821 0.034 Uiso 1 1 calc R . . H14B H 1.0714 0.9658 1.0382 0.034 Uiso 1 1 calc R . . C15 C 1.2513(8) 0.9798(8) 1.0906(3) 0.031(2) Uani 1 1 d . . . H15A H 1.3252 1.0137 1.0655 0.037 Uiso 1 1 calc R . . H15B H 1.2747 0.9162 1.1088 0.037 Uiso 1 1 calc R . . C16 C 1.2708(7) 1.0995(7) 1.1341(3) 0.029(2) Uani 1 1 d . . . H16A H 1.1943 1.0655 1.1583 0.034 Uiso 1 1 calc R . . H16B H 1.2498 1.1638 1.1155 0.034 Uiso 1 1 calc R . . C17 C 1.4268(7) 1.1769(7) 1.1698(3) 0.032(2) Uani 1 1 d . . . H17A H 1.4453 1.1146 1.1906 0.039 Uiso 1 1 calc R . . H17B H 1.5044 1.2064 1.1457 0.039 Uiso 1 1 calc R . . C18 C 1.4445(7) 1.3004(8) 1.2100(3) 0.036(2) Uani 1 1 d . . . H18A H 1.4243 1.3623 1.1895 0.044 Uiso 1 1 calc R . . H18B H 1.3691 1.2712 1.2349 0.044 Uiso 1 1 calc R . . C19 C 1.6015(7) 1.3765(8) 1.2438(3) 0.045(2) Uani 1 1 d . . . H19A H 1.6083 1.4551 1.2691 0.054 Uiso 1 1 calc R . . H19B H 1.6764 1.4072 1.2193 0.054 Uiso 1 1 calc R . . H19C H 1.6213 1.3161 1.2647 0.054 Uiso 1 1 calc R . . C20 C -0.0017(7) 0.1835(7) 0.5799(3) 0.0244(19) Uani 1 1 d . . . H20A H -0.0890 0.0988 0.5613 0.029 Uiso 1 1 calc R . . H20B H 0.0718 0.1624 0.5999 0.029 Uiso 1 1 calc R . . H20C H 0.0452 0.2370 0.5527 0.029 Uiso 1 1 calc R . . C21 C 0.0805(7) 0.3897(7) 0.6478(3) 0.034(2) Uani 1 1 d . . . H21A H 0.1500 0.3670 0.6694 0.041 Uiso 1 1 calc R . . H21B H 0.0481 0.4454 0.6722 0.041 Uiso 1 1 calc R . . H21C H 0.1317 0.4405 0.6205 0.041 Uiso 1 1 calc R . . C22 C -0.1546(8) 0.3032(8) 0.5875(3) 0.040(2) Uani 1 1 d . . . H22A H -0.2450 0.2215 0.5686 0.048 Uiso 1 1 calc R . . H22B H -0.1017 0.3536 0.5604 0.048 Uiso 1 1 calc R . . H22C H -0.1840 0.3606 0.6123 0.048 Uiso 1 1 calc R . . C23 C -0.1318(8) 0.1831(8) 0.6605(3) 0.031(2) Uani 1 1 d . . . H23A H -0.2272 0.1057 0.6410 0.037 Uiso 1 1 calc R . . H23B H -0.1582 0.2412 0.6869 0.037 Uiso 1 1 calc R . . C24 C -0.0400(7) 0.1282(7) 0.6926(3) 0.0254(19) Uani 1 1 d . . . H24A H 0.0667 0.1978 0.7021 0.030 Uiso 1 1 calc R . . H24B H -0.0435 0.0470 0.6693 0.030 Uiso 1 1 calc R . . C25 C -0.1023(8) 0.0907(8) 0.7451(3) 0.038(2) Uani 1 1 d . . . H25A H -0.0633 0.0305 0.7586 0.046 Uiso 1 1 calc R . . H25B H -0.2136 0.0390 0.7363 0.046 Uiso 1 1 calc R . . C26 C -0.0607(7) 0.2139(8) 0.7913(3) 0.036(2) Uani 1 1 d . . . H26A H -0.0880 0.2795 0.7763 0.043 Uiso 1 1 calc R . . H26B H -0.1226 0.1831 0.8203 0.043 Uiso 1 1 calc R . . C27 C 0.1060(7) 0.2879(8) 0.8178(3) 0.032(2) Uani 1 1 d . . . H27A H 0.1350 0.2237 0.8331 0.038 Uiso 1 1 calc R . . H27B H 0.1692 0.3217 0.7895 0.038 Uiso 1 1 calc R . . C28 C 0.1345(7) 0.4061(8) 0.8630(3) 0.033(2) Uani 1 1 d . . . H28A H 0.0633 0.3722 0.8890 0.040 Uiso 1 1 calc R . . H28B H 0.1117 0.4724 0.8466 0.040 Uiso 1 1 calc R . . C29 C 0.2931(8) 0.4790(8) 0.8948(3) 0.032(2) Uani 1 1 d . . . H29A H 0.3648 0.5120 0.8689 0.039 Uiso 1 1 calc R . . H29B H 0.3156 0.4136 0.9120 0.039 Uiso 1 1 calc R . . C30 C 0.3187(7) 0.5994(7) 0.9395(3) 0.029(2) Uani 1 1 d . . . H30A H 0.2950 0.6639 0.9220 0.035 Uiso 1 1 calc R . . H30B H 0.2463 0.5657 0.9651 0.035 Uiso 1 1 calc R . . C31 C 0.4754(8) 0.6756(8) 0.9723(3) 0.034(2) Uani 1 1 d . . . H31A H 0.5482 0.7087 0.9467 0.041 Uiso 1 1 calc R . . H31B H 0.4988 0.6117 0.9902 0.041 Uiso 1 1 calc R . . C32 C 0.4986(8) 0.7953(8) 1.0158(3) 0.035(2) Uani 1 1 d . . . H32A H 0.4248 0.7625 1.0410 0.042 Uiso 1 1 calc R . . H32B H 0.4772 0.8602 0.9978 0.042 Uiso 1 1 calc R . . C33 C 0.6575(7) 0.8703(8) 1.0495(3) 0.033(2) Uani 1 1 d . . . H33A H 0.6799 0.8058 1.0675 0.039 Uiso 1 1 calc R . . H33B H 0.7319 0.9048 1.0246 0.039 Uiso 1 1 calc R . . C34 C 0.6749(7) 0.9881(8) 1.0929(3) 0.031(2) Uani 1 1 d . . . H34A H 0.6534 1.0528 1.0748 0.037 Uiso 1 1 calc R . . H34B H 0.5993 0.9534 1.1174 0.037 Uiso 1 1 calc R . . C35 C 0.8304(7) 1.0624(8) 1.1272(3) 0.030(2) Uani 1 1 d . . . H35A H 0.9059 1.0919 1.1023 0.035 Uiso 1 1 calc R . . H35B H 0.8491 0.9984 1.1467 0.035 Uiso 1 1 calc R . . C36 C 0.8548(7) 1.1863(8) 1.1692(3) 0.036(2) Uani 1 1 d . . . H36A H 0.8340 1.2494 1.1498 0.043 Uiso 1 1 calc R . . H36B H 0.7803 1.1564 1.1945 0.043 Uiso 1 1 calc R . . C37 C 1.0108(8) 1.2628(8) 1.2030(3) 0.049(2) Uani 1 1 d . . . H37A H 1.0860 1.2906 1.1779 0.058 Uiso 1 1 calc R . . H37B H 1.0306 1.2012 1.2238 0.058 Uiso 1 1 calc R . . C38 C 1.0318(9) 1.3876(8) 1.2428(3) 0.054(3) Uani 1 1 d . . . H38A H 1.1349 1.4328 1.2633 0.065 Uiso 1 1 calc R . . H38B H 0.9596 1.3607 1.2684 0.065 Uiso 1 1 calc R . . H38C H 1.0144 1.4500 1.2225 0.065 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 0.0210(4) 0.0132(4) 0.0268(5) 0.0032(3) 0.0032(3) 0.0072(3) Mo2 0.0224(4) 0.0182(4) 0.0251(5) 0.0039(4) 0.0010(3) 0.0095(3) Mo3 0.0168(4) 0.0155(4) 0.0248(4) 0.0040(3) 0.0030(3) 0.0083(3) Mo4 0.0237(4) 0.0277(5) 0.0422(5) 0.0147(4) 0.0068(4) 0.0122(4) O1 0.037(3) 0.025(3) 0.034(3) 0.011(3) 0.011(3) 0.024(3) O2 0.018(3) 0.033(4) 0.031(3) 0.003(3) 0.011(2) 0.009(2) O3 0.031(3) 0.016(3) 0.033(3) 0.006(3) -0.001(2) 0.011(2) O4 0.016(3) 0.016(3) 0.029(3) 0.000(2) 0.002(2) 0.005(2) O5 0.025(3) 0.019(3) 0.033(3) 0.002(3) 0.010(2) 0.010(2) O6 0.016(3) 0.033(4) 0.029(3) 0.004(3) -0.001(2) 0.012(2) O7 0.043(3) 0.021(3) 0.017(3) 0.002(3) 0.002(2) 0.023(3) O8 0.038(3) 0.023(3) 0.044(4) 0.006(3) 0.004(3) 0.018(3) O9 0.045(3) 0.054(4) 0.039(4) 0.022(3) 0.008(3) 0.031(3) O10 0.034(3) 0.023(3) 0.017(3) 0.000(3) -0.002(2) 0.000(2) O11 0.069(4) 0.032(4) 0.019(3) -0.007(3) -0.017(3) 0.039(3) O12 0.019(3) 0.040(4) 0.043(4) 0.007(3) 0.017(2) 0.016(3) O13 0.029(3) 0.018(3) 0.041(4) 0.003(3) 0.019(3) -0.001(2) N1 0.016(3) 0.014(4) 0.025(4) 0.001(3) 0.007(3) 0.005(3) N2 0.007(3) 0.025(4) 0.031(4) 0.002(3) 0.005(3) 0.003(3) C1 0.027(4) 0.037(6) 0.025(5) 0.009(4) 0.001(4) 0.019(4) C2 0.020(4) 0.046(6) 0.047(6) -0.001(5) 0.003(4) 0.010(4) C3 0.052(6) 0.017(5) 0.054(7) 0.007(5) 0.013(5) 0.005(4) C4 0.033(5) 0.029(5) 0.027(5) -0.002(4) 0.010(4) 0.012(4) C5 0.032(5) 0.022(5) 0.044(6) -0.009(4) -0.001(4) 0.015(4) C6 0.047(5) 0.032(6) 0.039(6) -0.005(5) 0.011(5) 0.020(5) C7 0.054(6) 0.040(6) 0.023(5) 0.000(5) 0.000(4) 0.028(5) C8 0.038(5) 0.026(5) 0.015(5) -0.008(4) -0.005(4) 0.008(4) C9 0.041(5) 0.051(7) 0.034(6) 0.003(5) 0.005(4) 0.028(5) C10 0.046(5) 0.027(5) 0.028(5) 0.004(4) 0.006(4) 0.022(4) C11 0.016(4) 0.038(6) 0.025(5) -0.004(4) -0.003(3) 0.005(4) C12 0.035(5) 0.024(5) 0.024(5) 0.001(4) -0.001(4) 0.007(4) C13 0.040(5) 0.029(6) 0.023(5) 0.000(4) 0.000(4) 0.014(4) C14 0.035(4) 0.023(5) 0.023(5) 0.002(4) 0.000(4) 0.011(4) C15 0.048(5) 0.039(6) 0.019(5) 0.008(4) 0.011(4) 0.029(5) C16 0.035(5) 0.027(5) 0.024(5) 0.011(4) 0.007(4) 0.013(4) C17 0.037(5) 0.026(5) 0.035(6) 0.009(4) 0.001(4) 0.016(4) C18 0.026(4) 0.043(6) 0.027(5) -0.008(5) 0.003(4) 0.009(4) C19 0.030(5) 0.053(7) 0.037(6) 0.004(5) -0.001(4) 0.007(4) C20 0.021(4) 0.018(5) 0.032(5) 0.000(4) 0.007(4) 0.007(4) C21 0.032(5) 0.028(6) 0.041(6) -0.002(4) 0.001(4) 0.015(4) C22 0.039(5) 0.061(7) 0.044(6) 0.015(5) 0.008(4) 0.043(5) C23 0.042(5) 0.037(6) 0.021(5) 0.007(4) 0.009(4) 0.023(4) C24 0.019(4) 0.013(5) 0.036(5) -0.001(4) 0.002(4) 0.001(4) C25 0.042(5) 0.026(6) 0.038(6) 0.010(5) 0.007(4) 0.008(4) C26 0.037(5) 0.030(6) 0.033(6) 0.001(5) 0.003(4) 0.010(4) C27 0.028(4) 0.032(6) 0.030(5) -0.004(4) -0.003(4) 0.013(4) C28 0.029(5) 0.030(6) 0.045(6) 0.018(5) 0.017(4) 0.012(4) C29 0.045(5) 0.035(6) 0.021(5) 0.006(4) 0.006(4) 0.022(4) C30 0.029(4) 0.029(5) 0.028(5) 0.004(4) 0.002(4) 0.011(4) C31 0.044(5) 0.023(5) 0.033(5) 0.000(4) 0.004(4) 0.013(4) C32 0.041(5) 0.034(6) 0.032(6) 0.011(5) 0.007(4) 0.017(4) C33 0.025(4) 0.030(6) 0.042(6) 0.007(5) 0.006(4) 0.011(4) C34 0.029(4) 0.032(6) 0.037(6) 0.010(4) 0.015(4) 0.015(4) C35 0.034(5) 0.034(6) 0.020(5) 0.004(4) 0.003(4) 0.015(4) C36 0.031(5) 0.032(6) 0.042(6) 0.004(5) 0.004(4) 0.013(4) C37 0.060(6) 0.044(7) 0.035(6) -0.007(5) -0.022(5) 0.027(5) C38 0.088(7) 0.042(7) 0.034(6) 0.007(5) -0.004(5) 0.033(6) _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 O1 1.698(4) . ? Mo1 O2 1.704(4) . ? Mo1 O4 1.919(4) . ? Mo1 O3 1.942(4) . ? Mo1 O13 2.305(5) . ? Mo1 O11 2.345(5) 2_666 ? Mo2 O6 1.700(4) . ? Mo2 O5 1.708(4) . ? Mo2 O4 1.912(4) . ? Mo2 O7 1.935(4) . ? Mo2 O10 2.381(5) . ? Mo2 O11 2.399(5) 2_666 ? Mo3 O12 1.711(4) . ? Mo3 O13 1.765(5) . ? Mo3 O10 1.766(5) . ? Mo3 O11 1.788(4) . ? Mo4 O9 1.690(5) . ? Mo4 O8 1.696(4) . ? Mo4 O3 1.856(5) 2_666 ? Mo4 O7 1.859(5) . ? O3 Mo4 1.856(5) 2_666 ? O11 Mo1 2.345(5) 2_666 ? O11 Mo2 2.399(5) 2_666 ? N1 C1 1.480(7) . ? N1 C3 1.493(8) . ? N1 C2 1.496(7) . ? N1 C4 1.512(8) . ? N2 C21 1.478(8) . ? N2 C22 1.488(8) . ? N2 C23 1.497(8) . ? N2 C20 1.506(7) . ? C4 C5 1.486(9) . ? C5 C6 1.513(9) . ? C6 C7 1.512(9) . ? C7 C8 1.527(9) . ? C8 C9 1.523(9) . ? C9 C10 1.505(9) . ? C10 C11 1.521(9) . ? C11 C12 1.538(9) . ? C12 C13 1.503(9) . ? C13 C14 1.511(9) . ? C14 C15 1.518(9) . ? C15 C16 1.527(9) . ? C16 C17 1.531(9) . ? C17 C18 1.519(9) . ? C18 C19 1.518(8) . ? C23 C24 1.533(8) . ? C24 C25 1.531(9) . ? C25 C26 1.540(9) . ? C26 C27 1.532(8) . ? C27 C28 1.515(9) . ? C28 C29 1.510(9) . ? C29 C30 1.532(9) . ? C30 C31 1.506(9) . ? C31 C32 1.516(9) . ? C32 C33 1.531(9) . ? C33 C34 1.517(9) . ? C34 C35 1.511(9) . ? C35 C36 1.526(9) . ? C36 C37 1.510(9) . ? C37 C38 1.514(10) . ? 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 O1 Mo1 O2 104.3(2) . . ? O1 Mo1 O4 101.0(2) . . ? O2 Mo1 O4 100.2(2) . . ? O1 Mo1 O3 99.4(2) . . ? O2 Mo1 O3 97.1(2) . . ? O4 Mo1 O3 148.98(19) . . ? O1 Mo1 O13 91.38(19) . . ? O2 Mo1 O13 163.62(19) . . ? O4 Mo1 O13 81.03(19) . . ? O3 Mo1 O13 75.34(19) . . ? O1 Mo1 O11 165.5(2) . 2_666 ? O2 Mo1 O11 89.9(2) . 2_666 ? O4 Mo1 O11 73.43(17) . 2_666 ? O3 Mo1 O11 81.07(18) . 2_666 ? O13 Mo1 O11 74.70(17) . 2_666 ? O6 Mo2 O5 104.6(2) . . ? O6 Mo2 O4 100.2(2) . . ? O5 Mo2 O4 100.5(2) . . ? O6 Mo2 O7 102.3(2) . . ? O5 Mo2 O7 98.0(2) . . ? O4 Mo2 O7 146.13(19) . . ? O6 Mo2 O10 89.44(19) . . ? O5 Mo2 O10 165.72(19) . . ? O4 Mo2 O10 79.36(17) . . ? O7 Mo2 O10 75.91(17) . . ? O6 Mo2 O11 162.45(19) . 2_666 ? O5 Mo2 O11 92.5(2) . 2_666 ? O4 Mo2 O11 72.27(17) . 2_666 ? O7 Mo2 O11 78.79(18) . 2_666 ? O10 Mo2 O11 73.74(17) . 2_666 ? O12 Mo3 O13 107.4(2) . . ? O12 Mo3 O10 108.3(2) . . ? O13 Mo3 O10 111.7(2) . . ? O12 Mo3 O11 108.5(2) . . ? O13 Mo3 O11 110.2(2) . . ? O10 Mo3 O11 110.6(2) . . ? O9 Mo4 O8 107.5(2) . . ? O9 Mo4 O3 102.4(2) . 2_666 ? O8 Mo4 O3 106.6(2) . 2_666 ? O9 Mo4 O7 106.5(2) . . ? O8 Mo4 O7 104.6(2) . . ? O3 Mo4 O7 127.9(2) 2_666 . ? Mo4 O3 Mo1 129.3(2) 2_666 . ? Mo2 O4 Mo1 120.3(2) . . ? Mo4 O7 Mo2 131.5(2) . . ? Mo3 O10 Mo2 126.7(2) . . ? Mo3 O11 Mo1 135.5(2) . 2_666 ? Mo3 O11 Mo2 135.4(2) . 2_666 ? Mo1 O11 Mo2 88.87(16) 2_666 2_666 ? Mo3 O13 Mo1 127.7(2) . . ? C1 N1 C3 108.0(5) . . ? C1 N1 C2 109.1(5) . . ? C3 N1 C2 107.9(5) . . ? C1 N1 C4 111.4(5) . . ? C3 N1 C4 111.4(6) . . ? C2 N1 C4 109.0(5) . . ? C21 N2 C22 107.5(6) . . ? C21 N2 C23 110.5(6) . . ? C22 N2 C23 110.8(5) . . ? C21 N2 C20 108.6(5) . . ? C22 N2 C20 108.0(5) . . ? C23 N2 C20 111.4(5) . . ? C5 C4 N1 116.6(5) . . ? C4 C5 C6 110.9(6) . . ? C5 C6 C7 112.5(6) . . ? C6 C7 C8 114.3(6) . . ? C7 C8 C9 114.2(6) . . ? C10 C9 C8 115.4(6) . . ? C9 C10 C11 113.4(6) . . ? C10 C11 C12 113.5(5) . . ? C13 C12 C11 114.0(6) . . ? C12 C13 C14 113.1(6) . . ? C13 C14 C15 114.3(6) . . ? C14 C15 C16 114.0(5) . . ? C15 C16 C17 115.2(6) . . ? C18 C17 C16 113.5(6) . . ? C19 C18 C17 112.0(6) . . ? N2 C23 C24 114.6(5) . . ? C23 C24 C25 111.0(6) . . ? C24 C25 C26 113.8(6) . . ? C27 C26 C25 115.1(6) . . ? C28 C27 C26 110.9(6) . . ? C27 C28 C29 115.1(6) . . ? C28 C29 C30 113.7(6) . . ? C31 C30 C29 115.6(6) . . ? C30 C31 C32 114.7(6) . . ? C31 C32 C33 114.2(6) . . ? C34 C33 C32 112.3(6) . . ? C35 C34 C33 113.2(5) . . ? C34 C35 C36 114.7(6) . . ? C37 C36 C35 115.1(6) . . ? C36 C37 C38 113.4(6) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.076 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.166