Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'F. Albert Cotton' _publ_contact_author_address ; Department of Chemistry and Laboratory for Molecular Structure and Bonding P.O. Box. 30012 Texas A&M University College Station TX 77842-3012 U.S.A. ; _publ_contact_author_phone 979-845-3646 _publ_contact_author_fax 979-845-9351 _publ_contact_author_email cotton@tamu.edu _publ_section_title ; Strong reducing agents containing dimolybdenum Mo24+ units and their oxidized cations with Mo25+/6+ cores stabilized by bicyclic guanidinate anions with a seven-membered ring ; loop_ _publ_author_name 'F. Albert Cotton' 'Carlos Murillo' 'Xiaoping Wang.' 'Chad C. Wilkinson' #========================================================================== data_2twoCH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 607802' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H52 Cl5 Mo2 N12' _chemical_formula_sum 'C30 H52 Cl5 Mo2 N12' _chemical_formula_weight 949.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8255(11) _cell_length_b 12.5118(12) _cell_length_c 16.3372(16) _cell_angle_alpha 98.855(2) _cell_angle_beta 104.043(2) _cell_angle_gamma 117.894(2) _cell_volume 1969.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5954 _cell_measurement_theta_min 2.4665 _cell_measurement_theta_max 27.5505 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7853 _exptl_absorpt_correction_T_max 0.8304 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11586 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6849 _reflns_number_gt 5275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0665P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6849 _refine_ls_number_parameters 452 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo2 Mo 1.00352(3) 0.99186(3) 0.06559(2) 0.02475(12) Uani 1 1 d . . . Mo1 Mo 0.98965(3) 0.98831(3) 0.43083(2) 0.02684(13) Uani 1 1 d . . . Cl1 Cl 0.99183(11) 0.98487(11) 0.24730(7) 0.0409(3) Uani 1 1 d . . . N10 N 0.8115(3) 0.9768(3) 0.0406(2) 0.0306(8) Uani 1 1 d . . . N8 N 0.8957(3) 0.7884(3) 0.0181(2) 0.0322(8) Uani 1 1 d . . . N6 N 0.5762(3) 0.8104(4) 0.4320(2) 0.0386(9) Uani 1 1 d . . . N5 N 0.7693(3) 0.8704(3) 0.3823(2) 0.0318(8) Uani 1 1 d . . . N12 N 0.6089(4) 0.9409(4) -0.0495(2) 0.0361(9) Uani 1 1 d . . . C3 C 0.9672(4) 1.2072(4) 0.5102(3) 0.0323(10) Uani 1 1 d . . . C10 C 0.7159(4) 0.8625(4) 0.4453(3) 0.0297(9) Uani 1 1 d . . . C24 C 0.7425(4) 0.9712(4) -0.0399(3) 0.0283(9) Uani 1 1 d . . . N3 N 0.9366(4) 1.3016(4) 0.5017(3) 0.0441(10) Uani 1 1 d . . . C17 C 0.8444(4) 0.7371(4) -0.0693(3) 0.0336(10) Uani 1 1 d . . . N9 N 0.7499(4) 0.6069(4) -0.1170(3) 0.0494(10) Uani 1 1 d . . . N1 N 0.9688(3) 1.1481(3) 0.4357(2) 0.0311(8) Uani 1 1 d . . . C22 C 0.7256(5) 0.9552(5) 0.0945(3) 0.0458(12) Uani 1 1 d . . . H22A H 0.7536 1.0354 0.1369 0.055 Uiso 1 1 calc R . . H22B H 0.7302 0.8969 0.1272 0.055 Uiso 1 1 calc R . . C14 C 0.6816(4) 0.7903(4) 0.2899(3) 0.0368(10) Uani 1 1 d . . . H14A H 0.6311 0.7016 0.2892 0.044 Uiso 1 1 calc R . . H14B H 0.7410 0.7964 0.2559 0.044 Uiso 1 1 calc R . . C13 C 0.5785(4) 0.8210(5) 0.2421(3) 0.0447(12) Uani 1 1 d . . . H13A H 0.5439 0.7778 0.1782 0.054 Uiso 1 1 calc R . . H13B H 0.6254 0.9129 0.2513 0.054 Uiso 1 1 calc R . . C7 C 1.0308(5) 1.2662(5) 0.6694(3) 0.0467(12) Uani 1 1 d . . . H7A H 1.1050 1.3508 0.6751 0.056 Uiso 1 1 calc R . . H7B H 1.0666 1.2388 0.7170 0.056 Uiso 1 1 calc R . . C8 C 0.7074(4) 0.8735(5) 0.5836(3) 0.0419(11) Uani 1 1 d . . . H8A H 0.7453 0.9477 0.6353 0.050 Uiso 1 1 calc R . . H8B H 0.6985 0.8014 0.6043 0.050 Uiso 1 1 calc R . . C21 C 0.8820(5) 0.7051(4) 0.0742(3) 0.0474(13) Uani 1 1 d . . . H21A H 0.9407 0.7589 0.1357 0.057 Uiso 1 1 calc R . . H21B H 0.9179 0.6525 0.0563 0.057 Uiso 1 1 calc R . . C1 C 0.9282(6) 1.1950(5) 0.3636(3) 0.0486(13) Uani 1 1 d . . . H1A H 0.8431 1.1262 0.3161 0.058 Uiso 1 1 calc R . . H1B H 1.0002 1.2303 0.3386 0.058 Uiso 1 1 calc R . . C27 C 0.6068(5) 0.9279(6) -0.2426(3) 0.0542(14) Uani 1 1 d . . . H27A H 0.6054 0.8485 -0.2591 0.065 Uiso 1 1 calc R . . H27B H 0.5927 0.9537 -0.2961 0.065 Uiso 1 1 calc R . . C28 C 0.7464(5) 1.0299(5) -0.1740(3) 0.0413(11) Uani 1 1 d . . . H28A H 0.8120 1.0570 -0.2046 0.050 Uiso 1 1 calc R . . H28B H 0.7409 1.1035 -0.1504 0.050 Uiso 1 1 calc R . . C20 C 0.7414(6) 0.6188(5) 0.0727(3) 0.0625(16) Uani 1 1 d . . . H20A H 0.6970 0.6674 0.0784 0.075 Uiso 1 1 calc R . . H20B H 0.7488 0.5876 0.1241 0.075 Uiso 1 1 calc R . . C9 C 0.5702(5) 0.8414(5) 0.5213(3) 0.0524(14) Uani 1 1 d . . . H9A H 0.4945 0.7685 0.5280 0.063 Uiso 1 1 calc R . . H9B H 0.5585 0.9142 0.5323 0.063 Uiso 1 1 calc R . . C12 C 0.4573(5) 0.7816(5) 0.2730(3) 0.0505(13) Uani 1 1 d . . . H12A H 0.3932 0.8001 0.2372 0.061 Uiso 1 1 calc R . . H12B H 0.4091 0.6895 0.2627 0.061 Uiso 1 1 calc R . . C23 C 0.5821(5) 0.8961(5) 0.0263(3) 0.0480(13) Uani 1 1 d . . . H23A H 0.5321 0.8030 0.0093 0.058 Uiso 1 1 calc R . . H23B H 0.5294 0.9261 0.0493 0.058 Uiso 1 1 calc R . . C15 C 0.8099(6) 0.7291(5) -0.2141(3) 0.0547(14) Uani 1 1 d . . . H15A H 0.8738 0.7318 -0.2434 0.066 Uiso 1 1 calc R . . H15B H 0.7541 0.7585 -0.2460 0.066 Uiso 1 1 calc R . . C6 C 0.9177(6) 1.2788(6) 0.6846(4) 0.0622(15) Uani 1 1 d . . . H6A H 0.9440 1.3173 0.7483 0.075 Uiso 1 1 calc R . . H6B H 0.8355 1.1937 0.6663 0.075 Uiso 1 1 calc R . . C18 C 0.6278(5) 0.5419(5) -0.0947(4) 0.0606(15) Uani 1 1 d . . . H18A H 0.5579 0.4646 -0.1442 0.073 Uiso 1 1 calc R . . H18B H 0.5912 0.5973 -0.0878 0.073 Uiso 1 1 calc R . . C5 C 0.8833(7) 1.3582(6) 0.6353(4) 0.0629(16) Uani 1 1 d . . . H5A H 0.9647 1.4443 0.6560 0.075 Uiso 1 1 calc R . . H5B H 0.8113 1.3648 0.6507 0.075 Uiso 1 1 calc R . . C4 C 0.8352(6) 1.3079(6) 0.5341(4) 0.0583(15) Uani 1 1 d . . . H4A H 0.7527 1.2225 0.5130 0.070 Uiso 1 1 calc R . . H4B H 0.8098 1.3629 0.5084 0.070 Uiso 1 1 calc R . . C16 C 0.7211(7) 0.5980(6) -0.2127(4) 0.083(2) Uani 1 1 d . . . H16A H 0.7432 0.5397 -0.2420 0.100 Uiso 1 1 calc R . . H16B H 0.6242 0.5670 -0.2432 0.100 Uiso 1 1 calc R . . C11 C 0.4983(5) 0.8480(5) 0.3694(3) 0.0489(13) Uani 1 1 d . . . H11A H 0.5544 0.9400 0.3806 0.059 Uiso 1 1 calc R . . H11B H 0.4153 0.8303 0.3818 0.059 Uiso 1 1 calc R . . C26 C 0.4897(5) 0.9036(6) -0.2103(3) 0.0685(18) Uani 1 1 d . . . H26A H 0.4924 0.9834 -0.1923 0.082 Uiso 1 1 calc R . . H26B H 0.4025 0.8431 -0.2594 0.082 Uiso 1 1 calc R . . C25 C 0.4953(5) 0.8520(6) -0.1341(3) 0.0586(15) Uani 1 1 d . . . H25A H 0.4086 0.8232 -0.1242 0.070 Uiso 1 1 calc R . . H25B H 0.5021 0.7771 -0.1507 0.070 Uiso 1 1 calc R . . C2 C 0.9078(8) 1.2957(6) 0.4060(4) 0.080(2) Uani 1 1 d . . . H2A H 0.8135 1.2741 0.3775 0.096 Uiso 1 1 calc R . . H2B H 0.9709 1.3779 0.4008 0.096 Uiso 1 1 calc R . . C19 C 0.6522(6) 0.5058(5) -0.0112(4) 0.0680(17) Uani 1 1 d . . . H19A H 0.6957 0.4561 -0.0159 0.082 Uiso 1 1 calc R . . H19B H 0.5635 0.4511 -0.0063 0.082 Uiso 1 1 calc R . . Cl2S Cl 0.3181(2) 0.4691(2) 0.44981(13) 0.0926(6) Uani 1 1 d . . . Cl1S Cl 0.3616(2) 0.5462(2) 0.63617(15) 0.1152(7) Uani 1 1 d . . . C1S C 0.3214(7) 0.4252(6) 0.5478(5) 0.080(2) Uani 1 1 d . . . H1SA H 0.2313 0.3515 0.5375 0.096 Uiso 1 1 calc R . . H1SB H 0.3890 0.4001 0.5619 0.096 Uiso 1 1 calc R . . N4 N 0.7940(3) 0.9011(3) 0.5301(2) 0.0325(8) Uani 1 1 d . . . N2 N 0.9974(4) 1.1789(3) 0.5846(2) 0.0324(8) Uani 1 1 d . . . N11 N 0.8029(3) 0.9976(3) -0.0989(2) 0.0306(8) Uani 1 1 d . . . N7 N 0.8842(3) 0.8084(3) -0.1217(2) 0.0323(8) Uani 1 1 d . . . C2S C 0.9371(18) 0.4003(18) 0.0545(8) 0.073(3) Uani 0.363(4) 1 d PD A 1 H2SA H 0.9950 0.4926 0.0678 0.088 Uiso 0.363(4) 1 calc PR A 1 H2SB H 0.9981 0.3674 0.0585 0.088 Uiso 0.363(4) 1 calc PR A 1 Cl4S Cl 0.8792(9) 0.3777(9) 0.1387(5) 0.1172(13) Uani 0.363(4) 1 d PD A 1 Cl3S Cl 0.8376(16) 0.3448(15) -0.0495(7) 0.168(3) Uani 0.363(4) 1 d PD A 1 C2SA C 0.8897(11) 0.2913(10) 0.0759(5) 0.073(3) Uani 0.637(4) 1 d PD A 2 H2SC H 0.9855 0.3304 0.0801 0.088 Uiso 0.637(4) 1 calc PR A 2 H2SD H 0.8501 0.1991 0.0591 0.088 Uiso 0.637(4) 1 calc PR A 2 Cl4A Cl 0.8909(5) 0.3401(5) 0.1836(3) 0.1172(13) Uani 0.637(4) 1 d PD A 2 Cl3A Cl 0.8135(8) 0.3190(7) -0.0027(4) 0.168(3) Uani 0.637(4) 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 Mo2 0.0206(2) 0.0316(2) 0.0235(2) 0.01112(16) 0.00774(16) 0.01412(17) Mo1 0.0232(2) 0.0402(2) 0.0241(2) 0.01424(17) 0.00961(16) 0.02009(18) Cl1 0.0385(6) 0.0590(8) 0.0315(6) 0.0202(5) 0.0129(5) 0.0285(6) N10 0.0279(19) 0.045(2) 0.0257(19) 0.0170(17) 0.0119(16) 0.0213(17) N8 0.0301(19) 0.035(2) 0.032(2) 0.0149(16) 0.0103(17) 0.0166(17) N6 0.0251(19) 0.057(3) 0.034(2) 0.0158(19) 0.0117(17) 0.0213(19) N5 0.0268(19) 0.043(2) 0.0259(19) 0.0122(16) 0.0066(16) 0.0197(17) N12 0.029(2) 0.060(3) 0.032(2) 0.0225(19) 0.0150(17) 0.0288(19) C3 0.024(2) 0.036(3) 0.041(3) 0.016(2) 0.012(2) 0.017(2) C10 0.026(2) 0.034(2) 0.032(2) 0.0125(19) 0.0111(19) 0.0176(19) C24 0.023(2) 0.033(2) 0.028(2) 0.0079(18) 0.0062(18) 0.0167(19) N3 0.051(2) 0.045(2) 0.051(3) 0.020(2) 0.020(2) 0.033(2) C17 0.031(2) 0.032(2) 0.042(3) 0.011(2) 0.014(2) 0.019(2) N9 0.050(3) 0.030(2) 0.054(3) 0.0083(19) 0.022(2) 0.011(2) N1 0.0283(19) 0.043(2) 0.030(2) 0.0183(17) 0.0090(16) 0.0227(17) C22 0.039(3) 0.079(4) 0.035(3) 0.025(3) 0.020(2) 0.037(3) C14 0.032(2) 0.047(3) 0.029(2) 0.013(2) 0.010(2) 0.019(2) C13 0.030(2) 0.062(3) 0.032(3) 0.020(2) 0.005(2) 0.018(2) C7 0.062(3) 0.055(3) 0.032(3) 0.017(2) 0.016(2) 0.038(3) C8 0.031(2) 0.062(3) 0.032(3) 0.017(2) 0.015(2) 0.021(2) C21 0.055(3) 0.040(3) 0.042(3) 0.024(2) 0.012(2) 0.020(2) C1 0.067(3) 0.064(3) 0.037(3) 0.025(3) 0.024(3) 0.046(3) C27 0.042(3) 0.104(5) 0.030(3) 0.024(3) 0.014(2) 0.048(3) C28 0.044(3) 0.068(3) 0.030(3) 0.024(2) 0.017(2) 0.039(3) C20 0.072(4) 0.060(4) 0.050(4) 0.028(3) 0.024(3) 0.026(3) C9 0.034(3) 0.085(4) 0.044(3) 0.023(3) 0.021(2) 0.031(3) C12 0.034(3) 0.071(4) 0.047(3) 0.026(3) 0.010(2) 0.029(3) C23 0.040(3) 0.082(4) 0.041(3) 0.031(3) 0.023(2) 0.038(3) C15 0.070(4) 0.045(3) 0.037(3) 0.009(2) 0.022(3) 0.021(3) C6 0.083(4) 0.068(4) 0.059(4) 0.025(3) 0.034(3) 0.052(4) C18 0.049(3) 0.040(3) 0.061(4) 0.008(3) 0.015(3) 0.004(3) C5 0.081(4) 0.067(4) 0.061(4) 0.022(3) 0.028(3) 0.053(4) C4 0.058(4) 0.060(4) 0.070(4) 0.017(3) 0.022(3) 0.042(3) C16 0.107(5) 0.056(4) 0.037(3) 0.008(3) 0.013(3) 0.015(4) C11 0.033(3) 0.072(4) 0.054(3) 0.027(3) 0.017(2) 0.034(3) C26 0.041(3) 0.127(6) 0.038(3) 0.025(3) 0.009(3) 0.048(4) C25 0.024(3) 0.093(4) 0.048(3) 0.025(3) 0.010(2) 0.023(3) C2 0.124(6) 0.094(5) 0.049(4) 0.034(4) 0.020(4) 0.078(5) C19 0.066(4) 0.052(4) 0.079(5) 0.023(3) 0.035(4) 0.021(3) Cl2S 0.0864(13) 0.1055(15) 0.0930(14) 0.0367(12) 0.0287(11) 0.0558(12) Cl1S 0.1261(19) 0.1014(16) 0.1059(17) 0.0260(13) 0.0381(14) 0.0546(14) C1S 0.062(4) 0.061(4) 0.108(6) 0.027(4) 0.029(4) 0.028(3) N4 0.0278(19) 0.046(2) 0.028(2) 0.0146(17) 0.0136(16) 0.0198(17) N2 0.036(2) 0.044(2) 0.027(2) 0.0129(16) 0.0105(16) 0.0277(18) N11 0.0282(19) 0.043(2) 0.029(2) 0.0163(17) 0.0134(16) 0.0217(17) N7 0.0309(19) 0.035(2) 0.0268(19) 0.0081(16) 0.0079(16) 0.0154(17) C2S 0.086(6) 0.075(6) 0.084(7) 0.021(5) 0.030(5) 0.064(6) Cl4S 0.106(2) 0.138(3) 0.081(3) 0.003(2) 0.018(2) 0.061(2) Cl3S 0.217(5) 0.188(5) 0.140(6) 0.025(5) 0.046(5) 0.154(4) C2SA 0.086(6) 0.075(6) 0.084(7) 0.021(5) 0.030(5) 0.064(6) Cl4A 0.106(2) 0.138(3) 0.081(3) 0.003(2) 0.018(2) 0.061(2) Cl3A 0.217(5) 0.188(5) 0.140(6) 0.025(5) 0.046(5) 0.154(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 Mo2 N7 2.109(3) 2_775 ? Mo2 N10 2.118(3) . ? Mo2 N8 2.141(3) . ? Mo2 N11 2.155(3) 2_775 ? Mo2 Mo2 2.1690(7) 2_775 ? Mo2 Cl1 3.0178(11) . ? Mo1 N1 2.118(3) . ? Mo1 N4 2.119(3) 2_776 ? Mo1 N2 2.149(3) 2_776 ? Mo1 N5 2.153(3) . ? Mo1 Mo1 2.1711(7) 2_776 ? Mo1 Cl1 2.9987(11) . ? N10 C24 1.341(5) . ? N10 C22 1.459(5) . ? N8 C17 1.324(5) . ? N8 C21 1.470(5) . ? N6 C10 1.406(5) . ? N6 C9 1.477(6) . ? N6 C11 1.487(5) . ? N5 C10 1.326(5) . ? N5 C14 1.469(5) . ? N12 C24 1.402(5) . ? N12 C25 1.477(6) . ? N12 C23 1.479(5) . ? C3 N2 1.331(5) . ? C3 N1 1.333(5) . ? C3 N3 1.403(5) . ? C10 N4 1.326(5) . ? C24 N11 1.327(5) . ? N3 C4 1.452(6) . ? N3 C2 1.500(6) . ? C17 N7 1.337(5) . ? C17 N9 1.412(6) . ? N9 C18 1.458(6) . ? N9 C16 1.491(6) . ? N1 C1 1.471(5) . ? C22 C23 1.524(6) . ? C14 C13 1.521(5) . ? C13 C12 1.523(6) . ? C7 N2 1.460(5) . ? C7 C6 1.491(7) . ? C8 N4 1.460(5) . ? C8 C9 1.515(6) . ? C21 C20 1.491(7) . ? C1 C2 1.491(7) . ? C27 C28 1.517(7) . ? C27 C26 1.516(6) . ? C28 N11 1.456(5) . ? C20 C19 1.515(8) . ? C12 C11 1.501(7) . ? C15 N7 1.453(5) . ? C15 C16 1.486(7) . ? C6 C5 1.505(7) . ? C18 C19 1.506(7) . ? C5 C4 1.530(7) . ? C26 C25 1.489(7) . ? Cl2S C1S 1.768(7) . ? Cl1S C1S 1.709(7) . ? N4 Mo1 2.119(3) 2_776 ? N2 Mo1 2.149(3) 2_776 ? N11 Mo2 2.155(3) 2_775 ? N7 Mo2 2.109(3) 2_775 ? C2S Cl3S 1.629(13) . ? C2S Cl4S 1.684(12) . ? C2SA Cl3A 1.564(8) . ? C2SA Cl4A 1.766(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 N7 Mo2 N10 93.45(13) 2_775 . ? N7 Mo2 N8 175.75(12) 2_775 . ? N10 Mo2 N8 88.23(13) . . ? N7 Mo2 N11 87.52(13) 2_775 2_775 ? N10 Mo2 N11 175.93(11) . 2_775 ? N8 Mo2 N11 90.53(13) . 2_775 ? N7 Mo2 Mo2 91.15(9) 2_775 2_775 ? N10 Mo2 Mo2 90.07(8) . 2_775 ? N8 Mo2 Mo2 92.75(9) . 2_775 ? N11 Mo2 Mo2 93.86(8) 2_775 2_775 ? N7 Mo2 Cl1 85.67(9) 2_775 . ? N10 Mo2 Cl1 83.55(9) . . ? N8 Mo2 Cl1 90.66(9) . . ? N11 Mo2 Cl1 92.59(9) 2_775 . ? Mo2 Mo2 Cl1 172.67(3) 2_775 . ? N1 Mo1 N4 93.47(13) . 2_776 ? N1 Mo1 N2 175.72(12) . 2_776 ? N4 Mo1 N2 88.33(13) 2_776 2_776 ? N1 Mo1 N5 87.95(13) . . ? N4 Mo1 N5 176.07(13) 2_776 . ? N2 Mo1 N5 90.00(13) 2_776 . ? N1 Mo1 Mo1 90.73(9) . 2_776 ? N4 Mo1 Mo1 89.81(9) 2_776 2_776 ? N2 Mo1 Mo1 93.15(9) 2_776 2_776 ? N5 Mo1 Mo1 93.84(9) . 2_776 ? N1 Mo1 Cl1 86.55(9) . . ? N4 Mo1 Cl1 84.34(9) 2_776 . ? N2 Mo1 Cl1 89.77(9) 2_776 . ? N5 Mo1 Cl1 92.09(9) . . ? Mo1 Mo1 Cl1 173.39(3) 2_776 . ? Mo1 Cl1 Mo2 177.78(5) . . ? C24 N10 C22 109.2(3) . . ? C24 N10 Mo2 119.7(3) . . ? C22 N10 Mo2 130.7(3) . . ? C17 N8 C21 119.1(4) . . ? C17 N8 Mo2 115.4(3) . . ? C21 N8 Mo2 125.4(3) . . ? C10 N6 C9 105.8(3) . . ? C10 N6 C11 117.8(3) . . ? C9 N6 C11 111.3(4) . . ? C10 N5 C14 120.2(4) . . ? C10 N5 Mo1 114.1(3) . . ? C14 N5 Mo1 125.2(3) . . ? C24 N12 C25 119.3(4) . . ? C24 N12 C23 106.0(3) . . ? C25 N12 C23 111.2(4) . . ? N2 C3 N1 120.9(4) . . ? N2 C3 N3 125.5(4) . . ? N1 C3 N3 113.5(4) . . ? N4 C10 N5 121.1(4) . . ? N4 C10 N6 112.9(4) . . ? N5 C10 N6 125.9(4) . . ? N11 C24 N10 120.6(4) . . ? N11 C24 N12 127.1(4) . . ? N10 C24 N12 112.2(3) . . ? C3 N3 C4 120.7(4) . . ? C3 N3 C2 105.6(4) . . ? C4 N3 C2 112.7(4) . . ? N8 C17 N7 120.9(4) . . ? N8 C17 N9 126.1(4) . . ? N7 C17 N9 113.0(4) . . ? C17 N9 C18 117.4(4) . . ? C17 N9 C16 105.7(4) . . ? C18 N9 C16 114.5(4) . . ? C3 N1 C1 109.6(3) . . ? C3 N1 Mo1 119.1(3) . . ? C1 N1 Mo1 130.1(3) . . ? N10 C22 C23 103.5(3) . . ? N5 C14 C13 116.6(4) . . ? C14 C13 C12 113.6(4) . . ? N2 C7 C6 117.2(4) . . ? N4 C8 C9 104.2(3) . . ? N8 C21 C20 117.1(4) . . ? N1 C1 C2 105.0(4) . . ? C28 C27 C26 113.2(4) . . ? N11 C28 C27 117.9(4) . . ? C21 C20 C19 113.2(5) . . ? N6 C9 C8 103.9(4) . . ? C11 C12 C13 113.3(4) . . ? N12 C23 C22 103.2(3) . . ? N7 C15 C16 106.0(4) . . ? C7 C6 C5 113.5(5) . . ? N9 C18 C19 114.2(5) . . ? C6 C5 C4 115.3(5) . . ? N3 C4 C5 114.2(4) . . ? C15 C16 N9 105.8(4) . . ? N6 C11 C12 114.5(4) . . ? C25 C26 C27 112.8(4) . . ? N12 C25 C26 115.8(5) . . ? C1 C2 N3 106.1(4) . . ? C18 C19 C20 113.8(5) . . ? Cl1S C1S Cl2S 112.3(4) . . ? C10 N4 C8 109.2(3) . . ? C10 N4 Mo1 119.7(3) . 2_776 ? C8 N4 Mo1 130.3(3) . 2_776 ? C3 N2 C7 119.4(4) . . ? C3 N2 Mo1 115.2(3) . 2_776 ? C7 N2 Mo1 125.1(3) . 2_776 ? C24 N11 C28 120.7(3) . . ? C24 N11 Mo2 114.6(2) . 2_775 ? C28 N11 Mo2 124.4(3) . 2_775 ? C17 N7 C15 109.4(4) . . ? C17 N7 Mo2 118.3(3) . 2_775 ? C15 N7 Mo2 130.3(3) . 2_775 ? Cl3S C2S Cl4S 123.9(12) . . ? Cl3A C2SA Cl4A 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.026 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.100 #===END of CIF for Compound 2.2CH2Cl2 ================= data_3 _database_code_depnum_ccdc_archive 'CCDC 607803' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H48 Cl2 Mo2 N12' _chemical_formula_sum 'C28 H48 Cl2 Mo2 N12' _chemical_formula_weight 815.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 10.0675(15) _cell_length_b 10.0675(15) _cell_length_c 15.797(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1601.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2213 _cell_measurement_theta_min 2.394 _cell_measurement_theta_max 27.306 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.9160 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4873 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.44 _reflns_number_total 944 _reflns_number_gt 804 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0247P)^2^+4.4565P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 944 _refine_ls_number_parameters 94 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.5000 0.5000 0.56982(3) 0.0335(2) Uani 1 4 d S . . Cl1 Cl 0.5000 0.5000 0.75019(12) 0.0586(6) Uani 1 4 d S . . N1 N 0.6010(18) 0.3131(15) 0.5750(6) 0.034(3) Uani 0.50 1 d PD . . N2 N 0.6233(19) 0.3367(15) 0.4280(6) 0.035(3) Uani 0.50 1 d PDU . . N3 N 0.7164(6) 0.1553(6) 0.5252(3) 0.0472(17) Uani 0.50 1 d PD . . C3 C 0.6467(5) 0.2672(5) 0.5000 0.0406(12) Uani 1 2 d SD . . C4 C 0.7312(10) 0.0417(8) 0.4690(5) 0.065(3) Uani 0.50 1 d PD A . H4A H 0.7359 -0.0395 0.5032 0.078 Uiso 0.50 1 calc PR . . H4B H 0.8151 0.0500 0.4381 0.078 Uiso 0.50 1 calc PR . . C5 C 0.6191(10) 0.0286(10) 0.4064(5) 0.079(3) Uani 0.50 1 d PD . . H5A H 0.6191 -0.0610 0.3821 0.095 Uiso 0.50 1 calc PR A . H5B H 0.5340 0.0422 0.4353 0.095 Uiso 0.50 1 calc PR . . C6 C 0.6345(13) 0.1294(9) 0.3368(5) 0.081(3) Uani 0.50 1 d PD A . H6A H 0.5468 0.1448 0.3117 0.097 Uiso 0.50 1 calc PR . . H6B H 0.6908 0.0905 0.2927 0.097 Uiso 0.50 1 calc PR . . C7 C 0.6929(16) 0.2634(12) 0.3610(10) 0.052(4) Uani 0.50 1 d PD A . H7A H 0.7849 0.2494 0.3792 0.062 Uiso 0.50 1 calc PR . . H7B H 0.6953 0.3192 0.3102 0.062 Uiso 0.50 1 calc PR . . C1 C 0.6526(18) 0.2535(13) 0.6530(10) 0.062(5) Uani 0.50 1 d PDU A 1 H1A H 0.5810 0.2288 0.6920 0.074 Uiso 0.50 1 calc PR A 1 H1B H 0.7151 0.3127 0.6819 0.074 Uiso 0.50 1 calc PR A 1 C2 C 0.7214(10) 0.1328(9) 0.6166(4) 0.057(2) Uani 0.50 1 d PDU A 1 H2A H 0.8134 0.1270 0.6365 0.069 Uiso 0.50 1 calc PR A 1 H2B H 0.6745 0.0511 0.6320 0.069 Uiso 0.50 1 calc PR A 1 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 0.0372(2) 0.0372(2) 0.0262(3) 0.000 0.000 0.000 Cl1 0.0720(9) 0.0720(9) 0.0318(8) 0.000 0.000 0.000 N1 0.037(7) 0.020(4) 0.046(5) 0.007(4) -0.013(4) -0.010(5) N2 0.032(5) 0.035(7) 0.037(4) -0.012(3) 0.009(3) -0.016(5) N3 0.049(4) 0.044(4) 0.048(4) 0.003(2) -0.009(3) 0.014(3) C3 0.029(3) 0.031(3) 0.062(3) 0.000 0.000 -0.002(2) C4 0.083(6) 0.040(5) 0.073(6) -0.003(4) -0.012(4) 0.017(4) C5 0.091(8) 0.072(7) 0.075(6) -0.013(5) 0.004(6) -0.023(6) C6 0.116(9) 0.082(8) 0.045(4) -0.018(5) 0.002(6) 0.044(7) C7 0.057(8) 0.062(8) 0.036(6) 0.006(5) 0.014(5) 0.008(5) C1 0.078(9) 0.063(7) 0.044(6) 0.007(5) -0.019(6) 0.026(6) C2 0.070(5) 0.053(5) 0.049(4) 0.011(4) -0.017(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 2.060(16) 11_566 ? Mo1 N2 2.060(16) 9_666 ? Mo1 N2 2.060(16) 10_556 ? Mo1 N2 2.060(16) 12_656 ? Mo1 N1 2.140(15) 4_565 ? Mo1 N1 2.140(15) 3_655 ? Mo1 N1 2.140(15) 2_665 ? Mo1 N1 2.140(14) . ? Mo1 Mo1 2.2058(13) 9_666 ? Mo1 Cl1 2.849(2) . ? N1 C3 1.353(7) . ? N1 C1 1.465(7) . ? N2 C3 1.357(7) . ? N2 C7 1.469(7) . ? N3 C3 1.385(6) . ? N3 C4 1.456(7) . ? N3 C2 1.462(7) . ? C4 C5 1.507(8) . ? C5 C6 1.504(8) . ? C6 C7 1.520(9) . ? C1 C2 1.513(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mo1 N2 89.984(10) 11_566 9_666 ? N2 Mo1 N2 89.984(11) 11_566 10_556 ? N2 Mo1 N2 178.1(5) 9_666 10_556 ? N2 Mo1 N2 178.1(5) 11_566 12_656 ? N2 Mo1 N2 89.982(10) 9_666 12_656 ? N2 Mo1 N2 89.985(10) 10_556 12_656 ? N2 Mo1 N1 8.8(10) 11_566 4_565 ? N2 Mo1 N1 81.3(10) 9_666 4_565 ? N2 Mo1 N1 98.6(10) 10_556 4_565 ? N2 Mo1 N1 170.8(9) 12_656 4_565 ? N2 Mo1 N1 170.8(9) 11_566 3_655 ? N2 Mo1 N1 98.6(10) 9_666 3_655 ? N2 Mo1 N1 81.3(10) 10_556 3_655 ? N2 Mo1 N1 8.8(10) 12_656 3_655 ? N1 Mo1 N1 175.6(5) 4_565 3_655 ? N2 Mo1 N1 98.6(10) 11_566 2_665 ? N2 Mo1 N1 8.8(10) 9_666 2_665 ? N2 Mo1 N1 170.8(9) 10_556 2_665 ? N2 Mo1 N1 81.3(10) 12_656 2_665 ? N1 Mo1 N1 89.92(2) 4_565 2_665 ? N1 Mo1 N1 89.92(2) 3_655 2_665 ? N2 Mo1 N1 81.3(10) 11_566 . ? N2 Mo1 N1 170.8(9) 9_666 . ? N2 Mo1 N1 8.8(10) 10_556 . ? N2 Mo1 N1 98.6(10) 12_656 . ? N1 Mo1 N1 89.91(2) 4_565 . ? N1 Mo1 N1 89.92(2) 3_655 . ? N1 Mo1 N1 175.6(5) 2_665 . ? N2 Mo1 Mo1 91.0(3) 11_566 9_666 ? N2 Mo1 Mo1 91.0(3) 9_666 9_666 ? N2 Mo1 Mo1 91.0(3) 10_556 9_666 ? N2 Mo1 Mo1 91.0(3) 12_656 9_666 ? N1 Mo1 Mo1 92.2(3) 4_565 9_666 ? N1 Mo1 Mo1 92.2(3) 3_655 9_666 ? N1 Mo1 Mo1 92.2(3) 2_665 9_666 ? N1 Mo1 Mo1 92.2(3) . 9_666 ? N2 Mo1 Cl1 89.0(3) 11_566 . ? N2 Mo1 Cl1 89.0(3) 9_666 . ? N2 Mo1 Cl1 89.0(3) 10_556 . ? N2 Mo1 Cl1 89.0(3) 12_656 . ? N1 Mo1 Cl1 87.8(3) 4_565 . ? N1 Mo1 Cl1 87.8(3) 3_655 . ? N1 Mo1 Cl1 87.8(3) 2_665 . ? N1 Mo1 Cl1 87.8(3) . . ? Mo1 Mo1 Cl1 180.0 9_666 . ? N2 N1 C3 84(2) 10_556 . ? N2 N1 C7 85(6) 10_556 10_556 ? C3 N1 C7 105.9(11) . 10_556 ? N2 N1 C1 100(5) 10_556 . ? C3 N1 C1 118.4(12) . . ? N2 N1 Mo1 72(5) 10_556 . ? C3 N1 Mo1 115.4(9) . . ? C7 N1 Mo1 129.0(8) 10_556 . ? C1 N1 Mo1 124.1(6) . . ? N1 N2 C3 82.4(19) 10_556 . ? N1 N2 C7 82(6) 10_556 . ? C3 N2 C7 105.1(12) . . ? N1 N2 C1 68(5) 10_556 10_556 ? C3 N2 C1 112.2(10) . 10_556 ? N1 N2 Mo1 100(5) 10_556 9_666 ? C3 N2 Mo1 120.2(10) . 9_666 ? C7 N2 Mo1 134.5(7) . 9_666 ? C1 N2 Mo1 123.9(6) 10_556 9_666 ? N3 N3 C4 94.5(5) 10_556 10_556 ? N3 N3 C3 73.3(2) 10_556 . ? C4 N3 C3 153.0(8) 10_556 . ? N3 N3 C4 52.5(4) 10_556 . ? C3 N3 C4 121.0(5) . . ? N3 N3 C2 170.9(4) 10_556 . ? C4 N3 C2 76.4(6) 10_556 . ? C3 N3 C2 115.3(5) . . ? C4 N3 C2 118.4(6) . . ? N3 N3 C5 123.9(3) 10_556 10_556 ? C4 N3 C5 51.0(5) 10_556 10_556 ? C3 N3 C5 116.0(5) . 10_556 ? C4 N3 C5 82.8(5) . 10_556 ? C2 N3 C5 50.6(5) . 10_556 ? N1 C3 N1 122.3(15) 10_556 . ? N1 C3 N2 119.9(4) 10_556 10_556 ? N1 C3 N2 119.9(4) . . ? N2 C3 N2 114.0(14) 10_556 . ? N1 C3 N3 101.5(7) 10_556 10_556 ? N1 C3 N3 134.6(7) . 10_556 ? N2 C3 N3 138.5(8) 10_556 10_556 ? N2 C3 N3 105.5(7) . 10_556 ? N1 C3 N3 134.6(7) 10_556 . ? N1 C3 N3 101.5(7) . . ? N2 C3 N3 105.5(7) 10_556 . ? N2 C3 N3 138.5(8) . . ? N3 C4 C5 113.1(7) . . ? C6 C5 C4 110.1(8) . . ? C5 C6 C7 117.0(9) . . ? N2 C7 C6 116.3(12) . . ? N1 C1 C2 99.9(11) . . ? N3 C2 C1 103.6(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.644 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.078 #===END of CIF for Compound 3 ================================= data_4 _database_code_depnum_ccdc_archive 'CCDC 607804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H56 Mo2 N12' _chemical_formula_sum 'C32 H56 Mo2 N12' _chemical_formula_weight 800.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.211(3) _cell_length_b 8.9627(14) _cell_length_c 19.641(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.168(3) _cell_angle_gamma 90.00 _cell_volume 3557.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4672 _cell_measurement_theta_min 2.486 _cell_measurement_theta_max 25.305 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8899 _exptl_absorpt_correction_T_max 0.9059 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Burker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10131 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3144 _reflns_number_gt 2593 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0640P)^2^+10.0600P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3144 _refine_ls_number_parameters 371 _refine_ls_number_restraints 475 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.73005(2) 0.35518(5) -0.00717(2) 0.0659(2) Uani 1 1 d D . . N1 N 0.8533(7) 0.2318(15) 0.0662(12) 0.076(6) Uani 0.598(7) 1 d PDU . 1 C1 C 0.9092(9) 0.1483(16) 0.0939(8) 0.107(5) Uani 0.598(7) 1 d PDU . 1 H1B H 0.9446 0.1475 0.0606 0.128 Uiso 0.598(7) 1 calc PR . 1 H1C H 0.8956 0.0448 0.1015 0.128 Uiso 0.598(7) 1 calc PR . 1 C2 C 0.9354(7) 0.2113(14) 0.1588(7) 0.116(5) Uani 0.598(7) 1 d PDU . 1 H2A H 0.9692 0.1456 0.1790 0.139 Uiso 0.598(7) 1 calc PR . 1 H2B H 0.8997 0.2239 0.1914 0.139 Uiso 0.598(7) 1 calc PR . 1 C3 C 0.9645(6) 0.3583(15) 0.1409(8) 0.103(3) Uani 0.598(7) 1 d PDU . 1 H3A H 0.9710 0.4178 0.1823 0.124 Uiso 0.598(7) 1 calc PR . 1 H3B H 1.0078 0.3429 0.1205 0.124 Uiso 0.598(7) 1 calc PR . 1 N3 N 0.9220(8) 0.4380(16) 0.0936(9) 0.101(6) Uani 0.598(7) 1 d PDU . 1 C5 C 0.9495(7) 0.5697(14) 0.0653(8) 0.103(3) Uani 0.598(7) 1 d PDU . 1 H5A H 0.9554 0.5503 0.0166 0.124 Uiso 0.598(7) 1 calc PR . 1 H5B H 0.9939 0.5813 0.0855 0.124 Uiso 0.598(7) 1 calc PR . 1 C6 C 0.9167(5) 0.7142(14) 0.0705(9) 0.112(4) Uani 0.598(7) 1 d PDU . 1 H6A H 0.9450 0.7893 0.0494 0.135 Uiso 0.598(7) 1 calc PR . 1 H6B H 0.9138 0.7395 0.1189 0.135 Uiso 0.598(7) 1 calc PR . 1 C7 C 0.8506(4) 0.7265(13) 0.0398(6) 0.081(3) Uani 0.598(7) 1 d PDU . 1 H7A H 0.8340 0.8281 0.0465 0.097 Uiso 0.598(7) 1 calc PR . 1 H7B H 0.8532 0.7089 -0.0093 0.097 Uiso 0.598(7) 1 calc PR . 1 C8 C 0.8044(6) 0.6211(13) 0.0686(7) 0.068(3) Uani 0.598(7) 1 d PDU . 1 H8A H 0.8097 0.6258 0.1183 0.081 Uiso 0.598(7) 1 calc PR . 1 H8B H 0.7595 0.6563 0.0574 0.081 Uiso 0.598(7) 1 calc PR . 1 N2 N 0.8080(8) 0.4657(14) 0.0489(11) 0.059(4) Uani 0.598(7) 1 d PDU . 1 C4 C 0.8635(8) 0.3833(16) 0.0649(15) 0.084(7) Uani 0.598(7) 1 d PDU . 1 N4 N 0.6713(9) 0.3420(16) 0.0827(7) 0.065(5) Uani 0.598(7) 1 d PDU . 1 C9 C 0.6238(8) 0.4581(16) 0.1008(7) 0.109(5) Uani 0.598(7) 1 d PDU . 1 H9A H 0.5794 0.4289 0.0849 0.131 Uiso 0.598(7) 1 calc PR . 1 H9B H 0.6354 0.5517 0.0782 0.131 Uiso 0.598(7) 1 calc PR . 1 C10 C 0.6238(9) 0.481(2) 0.1767(9) 0.150(7) Uani 0.598(7) 1 d PDU . 1 H10A H 0.5953 0.5652 0.1890 0.180 Uiso 0.598(7) 1 calc PR . 1 H10B H 0.6687 0.4995 0.1947 0.180 Uiso 0.598(7) 1 calc PR . 1 C11 C 0.5957(10) 0.330(2) 0.2033(9) 0.156(4) Uani 0.598(7) 1 d PDU . 1 H11A H 0.5977 0.3295 0.2532 0.187 Uiso 0.598(7) 1 calc PR . 1 H11B H 0.5492 0.3204 0.1888 0.187 Uiso 0.598(7) 1 calc PR . 1 N6 N 0.6328(8) 0.2068(17) 0.1777(7) 0.107(5) Uani 0.598(7) 1 d PDU . 1 C13 C 0.6221(8) 0.068(2) 0.2019(8) 0.156(4) Uani 0.598(7) 1 d PDU . 1 H13A H 0.6018 0.0121 0.1641 0.187 Uiso 0.598(7) 1 calc PR . 1 H13B H 0.5878 0.0788 0.2361 0.187 Uiso 0.598(7) 1 calc PR . 1 C14 C 0.6718(14) -0.029(3) 0.2319(11) 0.221(11) Uani 0.598(7) 1 d PDU . 1 H14A H 0.7012 0.0295 0.2619 0.265 Uiso 0.598(7) 1 calc PR . 1 H14B H 0.6501 -0.1047 0.2597 0.265 Uiso 0.598(7) 1 calc PR . 1 C15 C 0.7098(10) -0.1003(17) 0.1824(10) 0.119(6) Uani 0.598(7) 1 d PDU . 1 H15A H 0.7516 -0.1311 0.2044 0.143 Uiso 0.598(7) 1 calc PR . 1 H15D H 0.6864 -0.1916 0.1688 0.143 Uiso 0.598(7) 1 calc PR . 1 C16 C 0.7239(11) -0.031(2) 0.1288(9) 0.140(8) Uani 0.598(7) 1 d PDU . 1 H16A H 0.7048 -0.0959 0.0934 0.168 Uiso 0.598(7) 1 calc PR . 1 H16D H 0.7718 -0.0468 0.1265 0.168 Uiso 0.598(7) 1 calc PR . 1 N5 N 0.7164(13) 0.1130(19) 0.0988(8) 0.072(6) Uani 0.598(7) 1 d PDU . 1 C12 C 0.6754(8) 0.2204(16) 0.1204(6) 0.065(4) Uani 0.598(7) 1 d PDU . 1 N1A N 0.6827(14) 0.042(2) -0.0362(18) 0.071(9) Uani 0.402(7) 1 d PDU . 2 C1A C 0.6754(13) -0.117(2) -0.0528(18) 0.133(12) Uani 0.402(7) 1 d PDU . 2 H1AB H 0.7078 -0.1757 -0.0264 0.160 Uiso 0.402(7) 1 calc PR . 2 H1AC H 0.6833 -0.1332 -0.1013 0.160 Uiso 0.402(7) 1 calc PR . 2 C2A C 0.6063(13) -0.166(2) -0.0361(13) 0.139(9) Uani 0.402(7) 1 d PDU . 2 H2AA H 0.5957 -0.1402 0.0109 0.167 Uiso 0.402(7) 1 calc PR . 2 H2AB H 0.6014 -0.2745 -0.0419 0.167 Uiso 0.402(7) 1 calc PR . 2 C3A C 0.5612(11) -0.081(3) -0.0873(12) 0.103(3) Uani 0.402(7) 1 d PDU . 2 H3AA H 0.5492 -0.1476 -0.1252 0.124 Uiso 0.402(7) 1 calc PR . 2 H3AB H 0.5204 -0.0520 -0.0647 0.124 Uiso 0.402(7) 1 calc PR . 2 N3A N 0.5927(10) 0.049(2) -0.1134(11) 0.083(7) Uani 0.402(7) 1 d PDU . 2 C5A C 0.5566(10) 0.143(2) -0.1578(12) 0.103(3) Uani 0.402(7) 1 d PDU . 2 H5AA H 0.5265 0.0817 -0.1857 0.124 Uiso 0.402(7) 1 calc PR . 2 H5AB H 0.5876 0.1913 -0.1887 0.124 Uiso 0.402(7) 1 calc PR . 2 C6A C 0.5175(12) 0.260(3) -0.1251(17) 0.182(11) Uani 0.402(7) 1 d PDU . 2 H6AA H 0.4772 0.2802 -0.1522 0.218 Uiso 0.402(7) 1 calc PR . 2 H6AB H 0.5047 0.2277 -0.0797 0.218 Uiso 0.402(7) 1 calc PR . 2 C7A C 0.5574(13) 0.394(2) -0.1201(12) 0.142(9) Uani 0.402(7) 1 d PDU . 2 H7AA H 0.5913 0.3976 -0.1550 0.170 Uiso 0.402(7) 1 calc PR . 2 H7AB H 0.5304 0.4847 -0.1221 0.170 Uiso 0.402(7) 1 calc PR . 2 C8A C 0.5839(10) 0.370(2) -0.0565(11) 0.093(6) Uani 0.402(7) 1 d PDU . 2 H8AA H 0.5484 0.3325 -0.0277 0.112 Uiso 0.402(7) 1 calc PR . 2 H8AB H 0.5977 0.4666 -0.0380 0.112 Uiso 0.402(7) 1 calc PR . 2 N2A N 0.6394(9) 0.269(2) -0.0489(16) 0.066(7) Uani 0.402(7) 1 d PDU . 2 C4A C 0.6427(13) 0.128(3) -0.0747(18) 0.074(8) Uani 0.402(7) 1 d PDU . 2 N4A N 0.7691(19) 0.383(3) -0.1067(11) 0.074(9) Uani 0.402(7) 1 d PDU . 2 C9A C 0.7518(11) 0.498(3) -0.1556(11) 0.125(10) Uani 0.402(7) 1 d PDU . 2 H9AA H 0.7315 0.5826 -0.1322 0.150 Uiso 0.402(7) 1 calc PR . 2 H9AB H 0.7195 0.4590 -0.1890 0.150 Uiso 0.402(7) 1 calc PR . 2 C10A C 0.8123(14) 0.549(2) -0.1911(14) 0.137(11) Uani 0.402(7) 1 d PDU . 2 H10C H 0.8507 0.5604 -0.1603 0.165 Uiso 0.402(7) 1 calc PR . 2 H10D H 0.8051 0.6404 -0.2176 0.165 Uiso 0.402(7) 1 calc PR . 2 C11A C 0.8158(13) 0.406(3) -0.2363(11) 0.156(4) Uani 0.402(7) 1 d PDU . 2 H11C H 0.7722 0.3839 -0.2564 0.187 Uiso 0.402(7) 1 calc PR . 2 H11D H 0.8471 0.4212 -0.2731 0.187 Uiso 0.402(7) 1 calc PR . 2 N6A N 0.8372(8) 0.288(2) -0.1935(7) 0.073(5) Uani 0.402(7) 1 d PDU . 2 C13A C 0.8627(13) 0.164(3) -0.2253(11) 0.156(4) Uani 0.402(7) 1 d PDU . 2 H13C H 0.8782 0.1988 -0.2696 0.187 Uiso 0.402(7) 1 calc PR . 2 H13D H 0.8253 0.0977 -0.2347 0.187 Uiso 0.402(7) 1 calc PR . 2 C14A C 0.9152(13) 0.072(4) -0.1965(16) 0.177(11) Uani 0.402(7) 1 d PDU . 2 H14C H 0.9315 0.0055 -0.2320 0.212 Uiso 0.402(7) 1 calc PR . 2 H14D H 0.9520 0.1364 -0.1818 0.212 Uiso 0.402(7) 1 calc PR . 2 C15A C 0.8949(12) -0.016(3) -0.1400(16) 0.155(11) Uani 0.402(7) 1 d PDU . 2 H15B H 0.8990 -0.1219 -0.1509 0.185 Uiso 0.402(7) 1 calc PR . 2 H15C H 0.9235 0.0056 -0.1002 0.185 Uiso 0.402(7) 1 calc PR . 2 C16A C 0.8319(11) 0.017(2) -0.1258(13) 0.115(7) Uani 0.402(7) 1 d PDU . 2 H16C H 0.8156 -0.0675 -0.0990 0.138 Uiso 0.402(7) 1 calc PR . 2 H16B H 0.8075 0.0139 -0.1694 0.138 Uiso 0.402(7) 1 calc PR . 2 N5A N 0.8102(15) 0.149(3) -0.0915(12) 0.083(9) Uani 0.402(7) 1 d PDU . 2 C12A C 0.8038(11) 0.272(3) -0.1304(9) 0.076(8) Uani 0.402(7) 1 d PDU . 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 0.0810(4) 0.0489(3) 0.0678(3) 0.0055(2) 0.0004(2) 0.0114(2) N1 0.096(10) 0.057(8) 0.074(10) 0.007(5) -0.006(6) 0.029(7) C1 0.129(12) 0.080(9) 0.108(11) -0.016(8) -0.046(10) 0.044(8) C2 0.086(8) 0.109(10) 0.150(12) 0.029(10) -0.047(8) 0.009(8) C3 0.076(6) 0.118(5) 0.116(8) -0.024(5) 0.008(6) 0.008(5) N3 0.104(10) 0.070(8) 0.127(12) 0.010(8) -0.026(9) -0.012(8) C5 0.076(6) 0.118(5) 0.116(8) -0.024(5) 0.008(6) 0.008(5) C6 0.104(10) 0.084(9) 0.149(13) 0.005(9) 0.004(9) -0.002(8) C7 0.078(7) 0.064(7) 0.101(8) 0.003(6) 0.003(6) 0.003(6) C8 0.079(7) 0.047(7) 0.077(7) -0.005(5) -0.005(6) 0.011(5) N2 0.069(7) 0.054(7) 0.053(7) -0.004(5) -0.001(6) 0.015(5) C4 0.108(14) 0.056(10) 0.087(12) 0.019(8) -0.016(10) -0.014(9) N4 0.066(8) 0.054(7) 0.077(7) 0.004(6) 0.014(7) 0.015(6) C9 0.098(9) 0.091(9) 0.141(12) 0.028(8) 0.062(9) 0.046(8) C10 0.099(12) 0.165(17) 0.185(17) -0.060(14) 0.005(12) 0.058(12) C11 0.127(8) 0.229(10) 0.111(7) 0.064(8) 0.015(6) -0.014(9) N6 0.160(13) 0.084(8) 0.077(7) 0.005(6) -0.002(8) 0.014(9) C13 0.127(8) 0.229(10) 0.111(7) 0.064(8) 0.015(6) -0.014(9) C14 0.25(2) 0.23(2) 0.17(2) 0.03(2) 0.003(19) 0.03(2) C15 0.153(15) 0.072(9) 0.132(13) 0.008(9) -0.005(12) -0.007(10) C16 0.180(17) 0.148(15) 0.093(12) 0.062(11) 0.017(11) 0.062(13) N5 0.104(15) 0.050(7) 0.063(7) 0.007(5) 0.005(8) 0.014(7) C12 0.072(10) 0.071(8) 0.052(6) 0.000(5) 0.010(6) 0.007(7) N1A 0.092(14) 0.048(10) 0.074(16) -0.013(8) 0.006(11) -0.005(10) C1A 0.17(2) 0.055(15) 0.17(2) -0.024(14) -0.01(2) 0.020(16) C2A 0.18(2) 0.061(12) 0.18(2) -0.016(12) -0.028(19) -0.054(14) C3A 0.076(6) 0.118(5) 0.116(8) -0.024(5) 0.008(6) 0.008(5) N3A 0.083(11) 0.079(11) 0.087(11) -0.012(8) -0.016(9) 0.029(9) C5A 0.076(6) 0.118(5) 0.116(8) -0.024(5) 0.008(6) 0.008(5) C6A 0.14(2) 0.18(3) 0.22(2) 0.01(2) 0.00(2) 0.04(2) C7A 0.129(18) 0.144(19) 0.150(19) -0.032(17) -0.040(15) 0.061(16) C8A 0.089(12) 0.063(10) 0.126(17) -0.016(11) -0.037(12) 0.005(9) N2A 0.063(10) 0.065(12) 0.071(15) 0.002(7) -0.015(9) -0.008(8) C4A 0.080(14) 0.071(17) 0.072(13) -0.002(12) -0.006(11) 0.020(12) N4A 0.072(12) 0.082(15) 0.067(12) 0.027(11) -0.008(9) 0.002(9) C9A 0.135(17) 0.16(2) 0.076(13) 0.088(14) 0.011(12) 0.057(15) C10A 0.17(2) 0.110(19) 0.130(19) 0.075(16) 0.037(16) 0.050(16) C11A 0.127(8) 0.229(10) 0.111(7) 0.064(8) 0.015(6) -0.014(9) N6A 0.088(10) 0.075(9) 0.057(8) -0.019(7) 0.020(7) -0.018(9) C13A 0.127(8) 0.229(10) 0.111(7) 0.064(8) 0.015(6) -0.014(9) C14A 0.15(2) 0.17(2) 0.21(2) 0.056(19) 0.075(18) 0.098(18) C15A 0.16(2) 0.145(19) 0.17(2) 0.045(17) 0.052(17) 0.098(16) C16A 0.134(18) 0.089(13) 0.125(16) -0.010(12) 0.038(15) 0.003(14) N5A 0.096(19) 0.069(11) 0.083(12) -0.017(9) 0.001(11) -0.015(10) C12A 0.074(14) 0.078(12) 0.075(12) -0.003(10) -0.013(10) -0.035(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo1 2.0677(9) 7_655 ? Mo1 N5A 2.12(2) 7_655 ? Mo1 N5 2.138(12) 7_655 ? Mo1 N2A 2.137(10) . ? Mo1 N4A 2.138(11) . ? Mo1 N2 2.147(10) . ? Mo1 N1A 2.148(18) 7_655 ? Mo1 N4 2.150(9) . ? Mo1 N1 2.170(12) 7_655 ? N1 C4 1.374(9) . ? N1 C1 1.453(9) . ? N1 Mo1 2.170(12) 7_655 ? C1 C2 1.482(9) . ? C2 C3 1.488(9) . ? C3 N3 1.440(9) . ? N3 C4 1.389(8) . ? N3 C5 1.423(9) . ? C5 C6 1.459(9) . ? C6 C7 1.460(9) . ? C7 C8 1.451(9) . ? C8 N2 1.448(9) . ? N2 C4 1.374(9) . ? N4 C12 1.319(13) . ? N4 C9 1.465(14) . ? C9 C10 1.505(17) . ? C10 C11 1.563(18) . ? C11 N6 1.433(16) . ? N6 C13 1.348(16) . ? N6 C12 1.436(12) . ? C13 C14 1.448(17) . ? C14 C15 1.404(18) . ? C15 C16 1.260(16) . ? C16 N5 1.425(15) . ? N5 C12 1.345(13) . ? N5 Mo1 2.138(12) 7_655 ? N1A C4A 1.338(18) . ? N1A C1A 1.473(16) . ? N1A Mo1 2.148(18) 7_655 ? C1A C2A 1.507(19) . ? C2A C3A 1.544(19) . ? C3A N3A 1.432(17) . ? N3A C5A 1.407(17) . ? N3A C4A 1.437(14) . ? C5A C6A 1.467(19) . ? C6A C7A 1.445(19) . ? C7A C8A 1.366(18) . ? C8A N2A 1.448(16) . ? N2A C4A 1.360(17) . ? N4A C12A 1.309(17) . ? N4A C9A 1.448(17) . ? C9A C10A 1.491(19) . ? C10A C11A 1.56(2) . ? C11A N6A 1.418(18) . ? N6A C13A 1.374(18) . ? N6A C12A 1.430(14) . ? C13A C14A 1.451(19) . ? C14A C15A 1.427(19) . ? C15A C16A 1.341(18) . ? C16A N5A 1.439(18) . ? N5A C12A 1.342(17) . ? N5A Mo1 2.12(2) 7_655 ? 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 Mo1 Mo1 N5A 90.8(6) 7_655 7_655 ? Mo1 Mo1 N5 91.9(4) 7_655 7_655 ? N5A Mo1 N5 169.6(12) 7_655 7_655 ? Mo1 Mo1 N2A 92.9(6) 7_655 . ? N5A Mo1 N2A 90.1(13) 7_655 . ? N5 Mo1 N2A 99.8(12) 7_655 . ? Mo1 Mo1 N4A 94.6(6) 7_655 . ? N5A Mo1 N4A 174.3(7) 7_655 . ? N5 Mo1 N4A 8.8(19) 7_655 . ? N2A Mo1 N4A 91.2(16) . . ? Mo1 Mo1 N2 94.0(4) 7_655 . ? N5A Mo1 N2 80.3(11) 7_655 . ? N5 Mo1 N2 89.5(11) 7_655 . ? N2A Mo1 N2 168.2(11) . . ? N4A Mo1 N2 97.7(14) . . ? Mo1 Mo1 N1A 91.2(6) 7_655 7_655 ? N5A Mo1 N1A 88.4(14) 7_655 7_655 ? N5 Mo1 N1A 81.5(13) 7_655 7_655 ? N2A Mo1 N1A 175.7(7) . 7_655 ? N4A Mo1 N1A 89.9(17) . 7_655 ? N2 Mo1 N1A 8.6(17) . 7_655 ? Mo1 Mo1 N4 93.3(3) 7_655 . ? N5A Mo1 N4 11.1(13) 7_655 . ? N5 Mo1 N4 174.7(4) 7_655 . ? N2A Mo1 N4 79.2(11) . . ? N4A Mo1 N4 167.8(12) . . ? N2 Mo1 N4 90.9(9) . . ? N1A Mo1 N4 99.2(12) 7_655 . ? Mo1 Mo1 N1 92.4(3) 7_655 7_655 ? N5A Mo1 N1 100.0(11) 7_655 7_655 ? N5 Mo1 N1 89.9(11) 7_655 7_655 ? N2A Mo1 N1 9.9(15) . 7_655 ? N4A Mo1 N1 81.4(14) . 7_655 ? N2 Mo1 N1 173.6(4) . 7_655 ? N1A Mo1 N1 170.8(12) 7_655 7_655 ? N4 Mo1 N1 89.0(9) . 7_655 ? C4 N1 C1 113.5(12) . . ? C4 N1 Mo1 117.4(9) . 7_655 ? C1 N1 Mo1 127.2(10) . 7_655 ? N1 C1 C2 112.8(11) . . ? C1 C2 C3 105.6(12) . . ? N3 C3 C2 111.0(10) . . ? C4 N3 C5 118.0(13) . . ? C4 N3 C3 125.3(12) . . ? C5 N3 C3 115.6(10) . . ? N3 C5 C6 121.8(12) . . ? C5 C6 C7 116.8(13) . . ? C8 C7 C6 112.4(10) . . ? N2 C8 C7 119.0(13) . . ? C4 N2 C8 120.2(10) . . ? C4 N2 Mo1 117.2(9) . . ? C8 N2 Mo1 122.6(9) . . ? N2 C4 N1 114.4(10) . . ? N2 C4 N3 126.0(12) . . ? N1 C4 N3 118.0(12) . . ? C12 N4 C9 118.9(10) . . ? C12 N4 Mo1 118.5(8) . . ? C9 N4 Mo1 122.4(8) . . ? N4 C9 C10 110.6(12) . . ? C9 C10 C11 102.6(13) . . ? N6 C11 C10 110.8(12) . . ? C13 N6 C11 119.9(13) . . ? C13 N6 C12 117.2(13) . . ? C11 N6 C12 122.4(12) . . ? N6 C13 C14 125.6(19) . . ? C15 C14 C13 112.2(17) . . ? C16 C15 C14 119.3(17) . . ? C15 C16 N5 140.2(17) . . ? C12 N5 C16 125.3(12) . . ? C12 N5 Mo1 119.7(9) . 7_655 ? C16 N5 Mo1 114.7(10) . 7_655 ? N4 C12 N5 116.5(9) . . ? N4 C12 N6 118.6(11) . . ? N5 C12 N6 124.7(12) . . ? C4A N1A C1A 111.9(18) . . ? C4A N1A Mo1 117.5(15) . 7_655 ? C1A N1A Mo1 125.5(17) . 7_655 ? N1A C1A C2A 109.1(18) . . ? C1A C2A C3A 104.4(18) . . ? N3A C3A C2A 112.2(15) . . ? C5A N3A C3A 118.9(15) . . ? C5A N3A C4A 112.6(18) . . ? C3A N3A C4A 121.6(19) . . ? N3A C5A C6A 116(2) . . ? C7A C6A C5A 109(2) . . ? C8A C7A C6A 98.0(19) . . ? C7A C8A N2A 118.8(19) . . ? C4A N2A C8A 125.8(13) . . ? C4A N2A Mo1 115.6(13) . . ? C8A N2A Mo1 117.9(13) . . ? N1A C4A N2A 110.7(19) . . ? N1A C4A N3A 115.4(17) . . ? N2A C4A N3A 127.8(17) . . ? C12A N4A C9A 115.6(16) . . ? C12A N4A Mo1 116.5(12) . . ? C9A N4A Mo1 126.9(14) . . ? N4A C9A C10A 109.7(18) . . ? C9A C10A C11A 93.6(17) . . ? N6A C11A C10A 107.2(16) . . ? C13A N6A C11A 116.5(14) . . ? C13A N6A C12A 120.1(17) . . ? C11A N6A C12A 116.4(16) . . ? N6A C13A C14A 124(2) . . ? C15A C14A C13A 113.5(18) . . ? C16A C15A C14A 109.4(17) . . ? C15A C16A N5A 125(2) . . ? C12A N5A C16A 115.9(18) . . ? C12A N5A Mo1 120.1(13) . 7_655 ? C16A N5A Mo1 122.6(16) . 7_655 ? N4A C12A N5A 117.9(15) . . ? N4A C12A N6A 119.8(16) . . ? N5A C12A N6A 122.2(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.587 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.071 #===END of CIF for Compound 4 =========================== data_5 _database_code_depnum_ccdc_archive 'CCDC 607805' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H56 Cl Mo2 N12' _chemical_formula_sum 'C32 H56 Cl Mo2 N12' _chemical_formula_weight 836.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 14.1897(10) _cell_length_b 14.1897(10) _cell_length_c 17.504(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3524.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 988 _cell_measurement_theta_min 5.0535 _cell_measurement_theta_max 43.749 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 6.859 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5471 _exptl_absorpt_correction_T_max 0.9346 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker GADDS' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24701 _diffrn_reflns_av_R_equivalents 0.1694 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.41 _diffrn_reflns_theta_max 59.06 _reflns_number_total 1276 _reflns_number_gt 651 _reflns_threshold_expression >2sigma(I) _computing_data_collection FRAMBO _computing_cell_refinement FRAMBO _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0786P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1276 _refine_ls_number_parameters 131 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.2500 0.2500 1.11351(6) 0.0271(4) Uani 1 4 d S . . Mo2 Mo 0.2500 0.2500 0.99168(6) 0.0265(4) Uani 1 4 d S . . Cl3 Cl 0.2500 0.2500 0.7800(2) 0.0417(9) Uani 1 4 d S . . N1 N 0.1066(4) 0.2097(4) 0.9845(3) 0.0325(15) Uani 1 1 d D . . N2 N 0.1087(5) 0.1946(4) 1.1157(3) 0.0370(17) Uani 1 1 d D . . C4 C 0.0590(4) 0.1904(5) 1.0497(4) 0.036(2) Uani 1 1 d D A . N3 N -0.0340(4) 0.1652(5) 1.0475(4) 0.0449(19) Uani 0.622(9) 1 d PD A 1 C1 C 0.053(3) 0.2094(16) 0.9141(19) 0.046(6) Uani 0.622(9) 1 d PD A 1 H1A H 0.0968 0.2132 0.8701 0.055 Uiso 0.622(9) 1 calc PR A 1 H1B H 0.0114 0.2652 0.9126 0.055 Uiso 0.622(9) 1 calc PR A 1 C2 C -0.0055(9) 0.1211(11) 0.9077(7) 0.036(3) Uani 0.622(9) 1 d PD A 1 H2A H 0.0348 0.0644 0.9117 0.044 Uiso 0.622(9) 1 calc PR A 1 H2B H -0.0390 0.1194 0.8580 0.044 Uiso 0.622(9) 1 calc PR A 1 C3 C -0.0752(13) 0.1244(16) 0.9728(8) 0.042(5) Uani 0.622(9) 1 d PD A 1 H3A H -0.0984 0.0598 0.9829 0.051 Uiso 0.622(9) 1 calc PR A 1 H3B H -0.1299 0.1632 0.9572 0.051 Uiso 0.622(9) 1 calc PR A 1 C5 C -0.1004(19) 0.1723(16) 1.1042(13) 0.042(5) Uani 0.622(9) 1 d PD A 1 H5A H -0.1101 0.1096 1.1277 0.050 Uiso 0.622(9) 1 calc PR A 1 H5B H -0.1611 0.1926 1.0816 0.050 Uiso 0.622(9) 1 calc PR A 1 C6 C -0.0717(11) 0.2414(12) 1.1650(8) 0.050(4) Uani 0.622(9) 1 d PD A 1 H6A H -0.1286 0.2629 1.1926 0.060 Uiso 0.622(9) 1 calc PR A 1 H6B H -0.0426 0.2971 1.1404 0.060 Uiso 0.622(9) 1 calc PR A 1 C7 C -0.0029(10) 0.2001(10) 1.2216(7) 0.043(4) Uani 0.622(9) 1 d PD A 1 H7A H 0.0282 0.2513 1.2505 0.051 Uiso 0.622(9) 1 calc PR A 1 H7B H -0.0369 0.1594 1.2583 0.051 Uiso 0.622(9) 1 calc PR A 1 C8 C 0.0703(10) 0.1429(13) 1.1796(9) 0.033(4) Uani 0.622(9) 1 d PD A 1 H8A H 0.1218 0.1260 1.2152 0.039 Uiso 0.622(9) 1 calc PR A 1 H8B H 0.0414 0.0837 1.1610 0.039 Uiso 0.622(9) 1 calc PR A 1 C7A C 0.016(2) 0.1408(18) 0.8764(13) 0.043(4) Uani 0.378(9) 1 d PD A 2 H7AA H -0.0319 0.1562 0.8376 0.051 Uiso 0.378(9) 1 calc PR A 2 H7AB H 0.0690 0.1077 0.8507 0.051 Uiso 0.378(9) 1 calc PR A 2 C6A C -0.025(2) 0.0786(18) 0.9373(12) 0.050(4) Uani 0.378(9) 1 d PD A 2 H6AA H 0.0268 0.0466 0.9643 0.060 Uiso 0.378(9) 1 calc PR A 2 H6AB H -0.0633 0.0291 0.9117 0.060 Uiso 0.378(9) 1 calc PR A 2 N3A N -0.0340(4) 0.1652(5) 1.0475(4) 0.0449(19) Uani 0.378(9) 1 d PD A 2 C2A C -0.0443(18) 0.227(2) 1.1888(15) 0.036(3) Uani 0.378(9) 1 d PD A 2 H2AA H -0.0799 0.2155 1.2365 0.044 Uiso 0.378(9) 1 calc PR A 2 H2AB H -0.0329 0.2957 1.1840 0.044 Uiso 0.378(9) 1 calc PR A 2 C3A C -0.098(3) 0.191(3) 1.121(2) 0.042(5) Uani 0.378(9) 1 d PD A 2 H3AA H -0.1450 0.2395 1.1056 0.051 Uiso 0.378(9) 1 calc PR A 2 H3AB H -0.1339 0.1342 1.1364 0.051 Uiso 0.378(9) 1 calc PR A 2 C1A C 0.048(2) 0.174(2) 1.190(2) 0.046(6) Uani 0.378(9) 1 d PD A 2 H1AA H 0.0354 0.1057 1.1937 0.055 Uiso 0.378(9) 1 calc PR A 2 H1AB H 0.0846 0.1930 1.2358 0.055 Uiso 0.378(9) 1 calc PR A 2 C8A C 0.052(4) 0.230(3) 0.913(3) 0.033(4) Uani 0.378(9) 1 d PD A 2 H8AA H 0.0926 0.2642 0.8769 0.039 Uiso 0.378(9) 1 calc PR A 2 H8AB H -0.0022 0.2709 0.9261 0.039 Uiso 0.378(9) 1 calc PR A 2 C5A C -0.087(2) 0.126(3) 0.996(2) 0.042(5) Uani 0.378(9) 1 d PD A 2 H5AA H -0.1271 0.1741 0.9714 0.050 Uiso 0.378(9) 1 calc PR A 2 H5AB H -0.1286 0.0786 1.0206 0.050 Uiso 0.378(9) 1 calc PR 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 0.0292(4) 0.0292(4) 0.0230(7) 0.000 0.000 0.000 Mo2 0.0282(5) 0.0282(5) 0.0230(8) 0.000 0.000 0.000 Cl3 0.0490(13) 0.0490(13) 0.0271(19) 0.000 0.000 0.000 N1 0.038(4) 0.036(4) 0.023(4) 0.003(3) -0.003(4) 0.000(3) N2 0.046(4) 0.036(4) 0.030(4) 0.006(3) 0.000(3) 0.000(4) C4 0.049(5) 0.023(5) 0.035(5) 0.004(4) -0.007(5) 0.003(4) N3 0.023(4) 0.070(5) 0.041(5) 0.013(4) -0.004(4) -0.020(4) C1 0.048(10) 0.047(12) 0.043(11) 0.009(10) 0.005(8) -0.003(11) C2 0.034(9) 0.057(9) 0.019(9) 0.008(8) 0.001(6) -0.012(6) C3 0.042(11) 0.065(11) 0.020(10) -0.005(9) 0.001(8) -0.027(9) C5 0.038(10) 0.048(12) 0.040(14) 0.006(9) 0.003(9) -0.002(8) C6 0.049(8) 0.074(10) 0.027(8) -0.005(10) 0.000(6) -0.015(9) C7 0.025(8) 0.071(10) 0.032(8) -0.009(7) 0.011(6) -0.004(7) C8 0.029(8) 0.055(12) 0.014(8) 0.001(7) 0.000(6) -0.007(7) C7A 0.025(8) 0.071(10) 0.032(8) -0.009(7) 0.011(6) -0.004(7) C6A 0.049(8) 0.074(10) 0.027(8) -0.005(10) 0.000(6) -0.015(9) N3A 0.023(4) 0.070(5) 0.041(5) 0.013(4) -0.004(4) -0.020(4) C2A 0.034(9) 0.057(9) 0.019(9) 0.008(8) 0.001(6) -0.012(6) C3A 0.042(11) 0.065(11) 0.020(10) -0.005(9) 0.001(8) -0.027(9) C1A 0.048(10) 0.047(12) 0.043(11) 0.009(10) 0.005(8) -0.003(11) C8A 0.029(8) 0.055(12) 0.014(8) 0.001(7) 0.000(6) -0.007(7) C5A 0.038(10) 0.048(12) 0.040(14) 0.006(9) 0.003(9) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.1325(16) . ? Mo1 N2 2.154(7) . ? Mo1 N2 2.154(7) 4 ? Mo1 N2 2.154(7) 2 ? Mo1 N2 2.154(7) 3 ? Mo2 N1 2.117(6) 2 ? Mo2 N1 2.117(6) . ? Mo2 N1 2.117(6) 4 ? Mo2 N1 2.117(6) 3 ? N1 C4 1.354(6) . ? N1 C1 1.45(3) . ? N1 C8A 1.49(5) . ? N2 C4 1.355(6) . ? N2 C8 1.444(18) . ? N2 C1A 1.59(4) . ? C4 N3 1.369(6) . ? N3 C5 1.37(3) . ? N3 C3 1.54(2) . ? C1 C2 1.508(9) . ? C2 C3 1.510(9) . ? C5 C6 1.503(9) . ? C6 C7 1.510(9) . ? C7 C8 1.508(9) . ? C7A C6A 1.506(10) . ? C7A C8A 1.507(10) . ? C6A C5A 1.509(10) . ? C2A C3A 1.506(10) . ? C2A C1A 1.511(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 Mo2 Mo1 N2 91.03(16) . . ? Mo2 Mo1 N2 91.03(16) . 4 ? N2 Mo1 N2 89.982(7) . 4 ? Mo2 Mo1 N2 91.03(16) . 2 ? N2 Mo1 N2 177.9(3) . 2 ? N2 Mo1 N2 89.982(8) 4 2 ? Mo2 Mo1 N2 91.03(16) . 3 ? N2 Mo1 N2 89.981(7) . 3 ? N2 Mo1 N2 177.9(3) 4 3 ? N2 Mo1 N2 89.982(6) 2 3 ? N1 Mo2 N1 173.2(3) 2 . ? N1 Mo2 N1 89.80(2) 2 4 ? N1 Mo2 N1 89.80(2) . 4 ? N1 Mo2 N1 89.80(2) 2 3 ? N1 Mo2 N1 89.80(2) . 3 ? N1 Mo2 N1 173.2(3) 4 3 ? N1 Mo2 Mo1 93.38(16) 2 . ? N1 Mo2 Mo1 93.38(16) . . ? N1 Mo2 Mo1 93.38(16) 4 . ? N1 Mo2 Mo1 93.38(16) 3 . ? C4 N1 C1 117.1(14) . . ? C4 N1 C8A 119(2) . . ? C4 N1 Mo2 119.0(4) . . ? C1 N1 Mo2 123.7(13) . . ? C8A N1 Mo2 119.8(19) . . ? C4 N2 C8 116.2(9) . . ? C4 N2 C1A 114.2(13) . . ? C4 N2 Mo1 119.0(4) . . ? C8 N2 Mo1 123.4(8) . . ? C1A N2 Mo1 125.9(13) . . ? N1 C4 N2 116.8(6) . . ? N1 C4 N3 120.7(6) . . ? N2 C4 N3 122.5(7) . . ? C4 N3 C5 128.5(9) . . ? C4 N3 C3 119.1(8) . . ? C5 N3 C3 112.3(11) . . ? N1 C1 C2 110.8(19) . . ? C1 C2 C3 106.2(19) . . ? C2 C3 N3 113.8(14) . . ? N3 C5 C6 111.9(17) . . ? C5 C6 C7 112.8(16) . . ? C8 C7 C6 109.5(12) . . ? N2 C8 C7 111.3(13) . . ? C6A C7A C8A 109(3) . . ? C7A C6A C5A 117(2) . . ? C3A C2A C1A 107(3) . . ? C2A C1A N2 112(2) . . ? N1 C8A C7A 112(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 59.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.086 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.264 #===END of CIF for compound 5 ========================= data_SI _database_code_depnum_ccdc_archive 'CCDC 607806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H10 N2 S' _chemical_formula_sum 'C5 H10 N2 S' _chemical_formula_weight 130.21 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' S S 0.1246 0.1234 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 5.042(2) _cell_length_b 8.429(4) _cell_length_c 8.108(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.748(8) _cell_angle_gamma 90.00 _cell_volume 333.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1616 _cell_measurement_theta_min 2.5795 _cell_measurement_theta_max 27.4995 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 140 _exptl_absorpt_coefficient_mu 0.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9074 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2285 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.52 _reflns_number_total 817 _reflns_number_gt 738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0690P)^2^+0.0822P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 817 _refine_ls_number_parameters 67 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.207 _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 S1 S 0.48458(13) 0.2500 0.41208(7) 0.0399(3) Uani 1 2 d S . . C5 C 0.3249(4) 0.2500 0.5747(3) 0.0299(5) Uani 1 2 d SD . . N1 N 0.254(3) 0.3913(11) 0.623(2) 0.037(2) Uani 0.50 1 d PD . . H1A H 0.2785 0.4712 0.5610 0.044 Uiso 0.50 1 calc PR . . C1 C 0.142(3) 0.4303(15) 0.7650(13) 0.053(3) Uani 0.50 1 d PDU . . H2A H -0.0554 0.4449 0.7151 0.064 Uiso 0.50 1 calc PR . . H2C H 0.2144 0.5358 0.8023 0.064 Uiso 0.50 1 calc PR . . C2 C 0.1623(13) 0.3369(9) 0.9293(9) 0.0507(14) Uani 0.50 1 d PD . . H3A H -0.0212 0.3284 0.9488 0.061 Uiso 0.50 1 calc PR . . H3B H 0.2774 0.3964 1.0249 0.061 Uiso 0.50 1 calc PR . . C3 C 0.2823(12) 0.1684(8) 0.9284(7) 0.0477(13) Uani 0.50 1 d PD . . H4A H 0.2713 0.1089 1.0302 0.057 Uiso 0.50 1 calc PR . . H4B H 0.4739 0.1724 0.9224 0.057 Uiso 0.50 1 calc PR . . C4 C 0.095(2) 0.0928(13) 0.7634(11) 0.0412(18) Uani 0.50 1 d PD . . H5A H 0.0605 -0.0201 0.7785 0.049 Uiso 0.50 1 calc PR . . H5B H -0.0799 0.1491 0.7243 0.049 Uiso 0.50 1 calc PR . . N2 N 0.273(4) 0.1176(10) 0.651(2) 0.040(3) Uani 0.50 1 d PD . . H2B H 0.3587 0.0335 0.6307 0.048 Uiso 0.50 1 calc PR . . 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 S1 0.0650(5) 0.0213(3) 0.0412(4) 0.000 0.0278(3) 0.000 C5 0.0372(11) 0.0217(10) 0.0304(10) 0.000 0.0082(8) 0.000 N1 0.059(3) 0.022(3) 0.039(5) 0.004(2) 0.030(4) 0.006(2) C1 0.076(5) 0.037(4) 0.059(4) 0.005(2) 0.041(3) 0.000(3) C2 0.080(4) 0.034(2) 0.052(2) -0.0076(17) 0.042(3) -0.002(3) C3 0.075(4) 0.038(2) 0.036(2) 0.0040(16) 0.024(3) 0.005(3) C4 0.059(4) 0.019(3) 0.056(3) -0.003(2) 0.035(3) -0.013(3) N2 0.073(5) 0.013(2) 0.042(5) -0.003(2) 0.029(4) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C5 1.711(2) . ? C5 N1 1.332(6) . ? C5 N2 1.336(6) . ? N1 C1 1.441(7) . ? C1 C2 1.528(7) . ? C2 C3 1.544(5) . ? C3 C4 1.564(6) . ? C4 N2 1.444(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C5 N1 126.7(12) . 4_565 ? N1 C5 N2 120.6(3) 4_565 4_565 ? N1 C5 N2 120.6(3) . . ? N2 C5 N2 113.3(12) 4_565 . ? N1 C5 S1 116.3(6) . . ? N1 C5 S1 116.3(6) 4_565 . ? N2 C5 S1 123.1(6) 4_565 . ? N2 C5 S1 123.1(6) . . ? C5 N1 C1 129.1(13) . . ? N1 C1 C2 128.5(12) . . ? C1 C2 C3 114.2(7) . . ? C2 C3 C4 103.1(8) . . ? N2 C4 C3 98.2(10) . . ? C5 N2 C4 129.9(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.514 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.073 #===END of CIF for SI ==================================== data_SIIHI _database_code_depnum_ccdc_archive 'CCDC 607807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-methylmercapto-delta^2^-1,3-diazacycloheptane ; _chemical_name_common 2-methylmercapto-delta$2!-1,3-diazacycloheptane _chemical_melting_point ? _chemical_formula_moiety 'C6 H13 I N2 S' _chemical_formula_sum 'C6 H13 I N2 S' _chemical_formula_weight 272.14 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' 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' _cell_length_a 8.924(3) _cell_length_b 10.537(3) _cell_length_c 11.061(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1040.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6800 _cell_measurement_theta_min 2.282 _cell_measurement_theta_max 27.499 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3188 _exptl_absorpt_correction_T_max 0.4997 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7302 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2368 _reflns_number_gt 2336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0212P)^2^+0.1085P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 2368 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 I1 I 0.300415(15) 0.844712(15) 0.193810(14) 0.03708(6) Uani 1 1 d . . . S1 S 0.28303(7) 0.79527(6) -0.20380(6) 0.03986(13) Uani 1 1 d . . . C5 C 0.3008(3) 0.6529(2) -0.12361(19) 0.0322(4) Uani 1 1 d . . . N1 N 0.1734(2) 0.5897(2) -0.1102(2) 0.0365(4) Uani 1 1 d . . . H1A H 0.0918 0.6344 -0.1038 0.044 Uiso 1 1 calc R . . N2 N 0.4319(2) 0.6097(2) -0.08539(19) 0.0343(4) Uani 1 1 d . . . H2A H 0.5109 0.6343 -0.1251 0.041 Uiso 1 1 calc R . . C2 C 0.2252(3) 0.3868(3) 0.0042(3) 0.0480(7) Uani 1 1 d . . . H3A H 0.1924 0.2980 0.0061 0.058 Uiso 1 1 calc R . . H3B H 0.1877 0.4282 0.0775 0.058 Uiso 1 1 calc R . . C3 C 0.3956(3) 0.3908(3) 0.0048(2) 0.0410(6) Uani 1 1 d . . . H4A H 0.4328 0.3387 0.0718 0.049 Uiso 1 1 calc R . . H4B H 0.4331 0.3539 -0.0707 0.049 Uiso 1 1 calc R . . C1 C 0.1574(3) 0.4510(3) -0.1051(3) 0.0460(6) Uani 1 1 d . . . H2B H 0.2035 0.4149 -0.1777 0.055 Uiso 1 1 calc R . . H2C H 0.0504 0.4304 -0.1076 0.055 Uiso 1 1 calc R . . C4 C 0.4569(3) 0.5240(3) 0.0179(2) 0.0416(6) Uani 1 1 d . . . H5A H 0.4118 0.5625 0.0898 0.050 Uiso 1 1 calc R . . H5B H 0.5650 0.5182 0.0323 0.050 Uiso 1 1 calc R . . C6 C 0.4388(3) 0.8886(3) -0.1495(2) 0.0415(6) Uani 1 1 d . . . H6A H 0.4383 0.9708 -0.1889 0.062 Uiso 1 1 calc R . . H6B H 0.5319 0.8451 -0.1675 0.062 Uiso 1 1 calc R . . H6C H 0.4298 0.9000 -0.0627 0.062 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 I1 0.02347(8) 0.04035(9) 0.04740(9) 0.00032(7) 0.00172(6) 0.00079(6) S1 0.0384(3) 0.0418(3) 0.0394(3) 0.0041(2) -0.0086(3) 0.0014(3) C5 0.0298(10) 0.0354(11) 0.0315(9) -0.0027(8) 0.0002(8) 0.0051(13) N1 0.0225(10) 0.0380(11) 0.0490(12) -0.0021(8) -0.0018(8) 0.0050(8) N2 0.0236(9) 0.0399(10) 0.0394(10) 0.0046(9) 0.0020(8) 0.0025(8) C2 0.0396(16) 0.0434(15) 0.0609(17) 0.0088(12) 0.0015(13) -0.0008(12) C3 0.0397(14) 0.0368(13) 0.0465(14) 0.0038(10) -0.0024(12) 0.0077(11) C1 0.0376(13) 0.0387(14) 0.0616(17) -0.0021(12) -0.0107(12) -0.0053(11) C4 0.0354(13) 0.0427(14) 0.0467(13) 0.0059(11) -0.0088(10) -0.0002(11) C6 0.0373(13) 0.0390(13) 0.0482(14) 0.0062(11) -0.0034(11) -0.0016(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C5 1.750(3) . ? S1 C6 1.805(3) . ? C5 N2 1.325(3) . ? C5 N1 1.326(3) . ? N1 C1 1.469(3) . ? N2 C4 1.473(3) . ? C2 C1 1.511(4) . ? C2 C3 1.522(4) . ? C3 C4 1.513(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 S1 C6 103.20(12) . . ? N2 C5 N1 123.3(2) . . ? N2 C5 S1 122.45(18) . . ? N1 C5 S1 114.16(17) . . ? C5 N1 C1 125.9(2) . . ? C5 N2 C4 126.3(2) . . ? C1 C2 C3 113.0(3) . . ? C4 C3 C2 112.8(2) . . ? N1 C1 C2 115.9(2) . . ? N2 C4 C3 116.1(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.296 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.129 #===END of CIF for SII*HI ================================== data_SIIIHI _database_code_depnum_ccdc_archive 'CCDC 607808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 I N3 O' _chemical_formula_sum 'C8 H18 I N3 O' _chemical_formula_weight 299.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.4816(12) _cell_length_b 9.6131(13) _cell_length_c 14.5230(19) _cell_angle_alpha 98.683(2) _cell_angle_beta 91.420(2) _cell_angle_gamma 115.187(2) _cell_volume 1178.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7502 _cell_measurement_theta_min 2.3795 _cell_measurement_theta_max 27.5355 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4528 _exptl_absorpt_correction_T_max 0.5303 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4233 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4233 _reflns_number_gt 3767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0284P)^2^+1.0455P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4233 _refine_ls_number_parameters 267 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.095 _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 I1 I 0.19116(3) 0.96331(3) 0.197312(19) 0.03756(9) Uani 1 1 d . . . I2 I 0.57954(3) 0.59791(4) 0.31009(2) 0.04087(9) Uani 1 1 d . . . N3 N 0.1250(4) 0.6882(4) 0.3891(2) 0.0312(7) Uani 1 1 d . . . H3A H 0.2145 0.7037 0.4165 0.037 Uiso 1 1 calc R . . N1 N -0.0671(4) 0.5455(4) 0.2647(2) 0.0333(8) Uani 1 1 d . . . H1A H -0.1431 0.5321 0.3000 0.040 Uiso 1 1 calc R . . C6 C 0.0391(5) 0.7669(5) 0.4375(3) 0.0318(9) Uani 1 1 d . . . H6A H -0.0254 0.7849 0.3913 0.038 Uiso 1 1 calc R . . H6B H 0.1138 0.8688 0.4724 0.038 Uiso 1 1 calc R . . C5 C 0.0768(4) 0.5941(4) 0.3059(3) 0.0289(8) Uani 1 1 d . . . N2 N 0.1762(4) 0.5432(4) 0.2637(2) 0.0331(8) Uani 1 1 d . . . H2A H 0.2749 0.6079 0.2672 0.040 Uiso 1 1 calc R . . O1 O -0.0300(3) 0.8894(4) 0.62326(19) 0.0428(7) Uani 1 1 d . . . H1B H -0.0732 0.9378 0.6537 0.064 Uiso 1 1 calc R . . C2 C -0.1130(5) 0.3570(5) 0.1147(3) 0.0426(11) Uani 1 1 d . . . H3B H -0.1587 0.3343 0.0498 0.051 Uiso 1 1 calc R . . H3C H -0.1829 0.2747 0.1467 0.051 Uiso 1 1 calc R . . C8 C -0.1452(5) 0.7578(5) 0.5608(3) 0.0377(10) Uani 1 1 d . . . H8A H -0.2006 0.7929 0.5187 0.045 Uiso 1 1 calc R . . H8B H -0.2220 0.6877 0.5966 0.045 Uiso 1 1 calc R . . C4 C 0.1244(5) 0.3841(5) 0.2124(3) 0.0381(10) Uani 1 1 d . . . H5A H 0.0510 0.3116 0.2485 0.046 Uiso 1 1 calc R . . H5B H 0.2154 0.3609 0.2081 0.046 Uiso 1 1 calc R . . C7 C -0.0654(5) 0.6725(5) 0.5047(3) 0.0335(9) Uani 1 1 d . . . H7A H -0.1452 0.5740 0.4690 0.040 Uiso 1 1 calc R . . H7B H -0.0021 0.6472 0.5477 0.040 Uiso 1 1 calc R . . C1 C -0.1041(5) 0.5134(5) 0.1623(3) 0.0388(10) Uani 1 1 d . . . H2B H -0.0240 0.5969 0.1358 0.047 Uiso 1 1 calc R . . H2C H -0.2048 0.5155 0.1484 0.047 Uiso 1 1 calc R . . C3 C 0.0462(5) 0.3533(6) 0.1149(3) 0.0449(11) Uani 1 1 d . . . H4A H 0.0328 0.2508 0.0824 0.054 Uiso 1 1 calc R . . H4B H 0.1145 0.4321 0.0803 0.054 Uiso 1 1 calc R . . C5A C 0.3150(4) 1.0518(5) 0.8050(2) 0.0339(9) Uani 1 1 d D . . N1A N 0.4579(9) 1.0948(15) 0.8472(11) 0.036(2) Uani 0.853(4) 1 d PD A 1 H1AA H 0.4995 1.0296 0.8372 0.044 Uiso 0.853(4) 1 calc PR A 1 N2A N 0.2134(4) 1.0931(4) 0.8506(2) 0.0354(8) Uani 0.853(4) 1 d PD A 1 H2AC H 0.1470 1.1114 0.8179 0.043 Uiso 0.853(4) 1 calc PR A 1 N3A N 0.2728(6) 0.9759(5) 0.7164(2) 0.0305(11) Uani 0.853(4) 1 d PD A 1 H3AA H 0.1739 0.9359 0.6965 0.037 Uiso 0.853(4) 1 calc PR A 1 C1A C 0.5478(6) 1.2435(6) 0.9086(3) 0.0410(12) Uani 0.853(4) 1 d PD A 1 H2AB H 0.5401 1.3264 0.8800 0.049 Uiso 0.853(4) 1 calc PR A 1 H2AD H 0.6582 1.2632 0.9135 0.049 Uiso 0.853(4) 1 calc PR A 1 C2A C 0.4958(16) 1.2529(11) 1.0061(7) 0.0425(17) Uani 0.853(4) 1 d PD A 1 H3AB H 0.5733 1.3479 1.0462 0.051 Uiso 0.853(4) 1 calc PR A 1 H3AC H 0.4912 1.1631 1.0322 0.051 Uiso 0.853(4) 1 calc PR A 1 C3A C 0.3365(13) 1.2549(14) 1.0068(5) 0.0426(18) Uani 0.853(4) 1 d PD A 1 H4AA H 0.3106 1.2661 1.0716 0.051 Uiso 0.853(4) 1 calc PR A 1 H4AB H 0.3416 1.3458 0.9817 0.051 Uiso 0.853(4) 1 calc PR A 1 C4A C 0.2081(6) 1.1089(6) 0.9501(3) 0.0385(12) Uani 0.853(4) 1 d PD A 1 H5AA H 0.2132 1.0180 0.9700 0.046 Uiso 0.853(4) 1 calc PR A 1 H5AB H 0.1069 1.1068 0.9646 0.046 Uiso 0.853(4) 1 calc PR A 1 C6A C 0.3788(6) 0.9541(5) 0.6499(3) 0.0310(10) Uani 0.853(4) 1 d PD A 1 H6AA H 0.4846 1.0380 0.6682 0.037 Uiso 0.853(4) 1 calc PR A 1 H6AB H 0.3446 0.9623 0.5875 0.037 Uiso 0.853(4) 1 calc PR A 1 C7A C 0.3838(6) 0.7978(5) 0.6453(3) 0.0326(11) Uani 0.853(4) 1 d PD A 1 H7AA H 0.4238 0.7922 0.7068 0.039 Uiso 0.853(4) 1 calc PR A 1 H7AB H 0.2771 0.7142 0.6306 0.039 Uiso 0.853(4) 1 calc PR A 1 C8A C 0.4854(6) 0.7712(7) 0.5729(4) 0.0356(13) Uani 0.853(4) 1 d PD A 1 H8AA H 0.5897 0.8595 0.5834 0.043 Uiso 0.853(4) 1 calc PR A 1 H8AB H 0.4972 0.6764 0.5787 0.043 Uiso 0.853(4) 1 calc PR A 1 O1A O 0.4167(7) 0.7555(7) 0.4821(3) 0.0471(14) Uani 0.853(4) 1 d P A 1 H1AB H 0.4725 0.7396 0.4426 0.071 Uiso 0.853(4) 1 calc PR A 1 N1A' N 0.444(6) 1.066(11) 0.854(7) 0.036(2) Uani 0.147(4) 1 d PD A 2 H1AC H 0.5138 1.0525 0.8211 0.044 Uiso 0.147(4) 1 calc PR A 2 N2A' N 0.2134(4) 1.0931(4) 0.8506(2) 0.0354(8) Uani 0.147(4) 1 d PD A 2 H2AA H 0.1140 1.0307 0.8389 0.043 Uiso 0.147(4) 1 calc PR A 2 N3A' N 0.255(4) 0.928(2) 0.7356(15) 0.0305(11) Uani 0.147(4) 1 d PD A 2 H3AD H 0.1563 0.8937 0.7155 0.037 Uiso 0.147(4) 1 calc PR A 2 C1A' C 0.485(3) 1.107(4) 0.9706(19) 0.0410(12) Uani 0.147(4) 1 d PD A 2 H2AE H 0.4048 1.0232 0.9969 0.049 Uiso 0.147(4) 1 calc PR A 2 H2AF H 0.5853 1.1031 0.9844 0.049 Uiso 0.147(4) 1 calc PR A 2 C2A' C 0.497(10) 1.261(6) 1.021(6) 0.0425(17) Uani 0.147(4) 1 d PD A 2 H3AE H 0.5720 1.3453 0.9928 0.051 Uiso 0.147(4) 1 calc PR A 2 H3AF H 0.5382 1.2770 1.0866 0.051 Uiso 0.147(4) 1 calc PR A 2 C3A' C 0.343(9) 1.275(11) 1.021(3) 0.0426(18) Uani 0.147(4) 1 d PD A 2 H4AC H 0.2718 1.1984 1.0557 0.051 Uiso 0.147(4) 1 calc PR A 2 H4AD H 0.3626 1.3789 1.0532 0.051 Uiso 0.147(4) 1 calc PR A 2 C4A' C 0.264(3) 1.247(4) 0.9235(19) 0.0385(12) Uani 0.147(4) 1 d PD A 2 H5AC H 0.3338 1.3322 0.8932 0.046 Uiso 0.147(4) 1 calc PR A 2 H5AD H 0.1694 1.2634 0.9320 0.046 Uiso 0.147(4) 1 calc PR A 2 C6A' C 0.339(3) 0.850(3) 0.6925(19) 0.0310(10) Uani 0.147(4) 1 d P A 2 H6AC H 0.2655 0.7468 0.6588 0.037 Uiso 0.147(4) 1 calc PR A 2 H6AD H 0.4026 0.8349 0.7409 0.037 Uiso 0.147(4) 1 calc PR A 2 C7A' C 0.444(4) 0.938(3) 0.626(2) 0.0326(11) Uani 0.147(4) 1 d P A 2 H7AC H 0.5236 1.0382 0.6599 0.039 Uiso 0.147(4) 1 calc PR A 2 H7AD H 0.3828 0.9590 0.5793 0.039 Uiso 0.147(4) 1 calc PR A 2 C8A' C 0.522(4) 0.843(4) 0.578(3) 0.0356(13) Uani 0.147(4) 1 d P A 2 H8AC H 0.5587 0.7965 0.6232 0.043 Uiso 0.147(4) 1 calc PR A 2 H8AD H 0.6112 0.9080 0.5474 0.043 Uiso 0.147(4) 1 calc PR A 2 O1A' O 0.392(5) 0.713(5) 0.504(3) 0.0471(14) Uani 0.147(4) 1 d P A 2 H1AD H 0.4268 0.6536 0.4775 0.071 Uiso 0.147(4) 1 calc PR 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 I1 0.02956(15) 0.04727(17) 0.03859(16) 0.00186(12) 0.00312(11) 0.02116(13) I2 0.03453(17) 0.0589(2) 0.03987(17) 0.00806(14) 0.00480(12) 0.03059(15) N3 0.0275(18) 0.0427(19) 0.0252(17) -0.0027(15) -0.0013(13) 0.0200(15) N1 0.0237(17) 0.045(2) 0.0314(18) -0.0006(15) 0.0049(14) 0.0178(16) C6 0.037(2) 0.035(2) 0.028(2) 0.0003(17) 0.0033(17) 0.0219(19) C5 0.026(2) 0.035(2) 0.031(2) 0.0090(17) 0.0063(16) 0.0163(18) N2 0.0239(17) 0.045(2) 0.0322(18) 0.0009(15) 0.0061(14) 0.0184(16) O1 0.0399(17) 0.0570(19) 0.0342(16) -0.0103(14) -0.0006(13) 0.0298(16) C2 0.032(2) 0.048(3) 0.039(2) -0.014(2) -0.0040(19) 0.018(2) C8 0.033(2) 0.055(3) 0.031(2) 0.0018(19) 0.0033(18) 0.027(2) C4 0.034(2) 0.044(2) 0.044(2) 0.000(2) 0.0046(19) 0.026(2) C7 0.034(2) 0.036(2) 0.033(2) 0.0027(18) 0.0037(17) 0.0181(19) C1 0.033(2) 0.050(2) 0.035(2) -0.0033(19) -0.0057(18) 0.023(2) C3 0.036(2) 0.052(3) 0.047(3) -0.008(2) 0.004(2) 0.024(2) C5A 0.027(2) 0.037(2) 0.038(2) 0.0018(19) 0.0001(18) 0.0161(19) N1A 0.023(3) 0.045(6) 0.038(3) -0.009(4) -0.003(3) 0.017(3) N2A 0.0247(17) 0.050(2) 0.0321(19) -0.0020(16) -0.0002(14) 0.0203(16) N3A 0.026(2) 0.035(2) 0.029(2) -0.0018(18) 0.0019(18) 0.014(2) C1A 0.025(2) 0.061(3) 0.034(3) -0.002(2) 0.000(2) 0.018(2) C2A 0.032(2) 0.051(3) 0.036(5) -0.013(3) -0.007(3) 0.017(2) C3A 0.037(3) 0.054(5) 0.035(4) -0.008(3) 0.001(3) 0.025(3) C4A 0.032(3) 0.054(3) 0.028(2) 0.001(2) 0.009(2) 0.019(2) C6A 0.029(3) 0.039(3) 0.025(2) 0.0052(19) 0.0066(19) 0.014(2) C7A 0.033(3) 0.037(2) 0.030(2) 0.008(2) 0.006(2) 0.017(2) C8A 0.033(3) 0.044(3) 0.031(2) -0.004(3) -0.002(2) 0.021(3) O1A 0.038(3) 0.080(4) 0.029(3) -0.008(2) -0.0002(19) 0.037(3) N1A' 0.023(3) 0.045(6) 0.038(3) -0.009(4) -0.003(3) 0.017(3) N2A' 0.0247(17) 0.050(2) 0.0321(19) -0.0020(16) -0.0002(14) 0.0203(16) N3A' 0.026(2) 0.035(2) 0.029(2) -0.0018(18) 0.0019(18) 0.014(2) C1A' 0.025(2) 0.061(3) 0.034(3) -0.002(2) 0.000(2) 0.018(2) C2A' 0.032(2) 0.051(3) 0.036(5) -0.013(3) -0.007(3) 0.017(2) C3A' 0.037(3) 0.054(5) 0.035(4) -0.008(3) 0.001(3) 0.025(3) C4A' 0.032(3) 0.054(3) 0.028(2) 0.001(2) 0.009(2) 0.019(2) C6A' 0.029(3) 0.039(3) 0.025(2) 0.0052(19) 0.0066(19) 0.014(2) C7A' 0.033(3) 0.037(2) 0.030(2) 0.008(2) 0.006(2) 0.017(2) C8A' 0.033(3) 0.044(3) 0.031(2) -0.004(3) -0.002(2) 0.021(3) O1A' 0.038(3) 0.080(4) 0.029(3) -0.008(2) -0.0002(19) 0.037(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 N3 C5 1.333(5) . ? N3 C6 1.458(5) . ? N1 C5 1.330(5) . ? N1 C1 1.474(5) . ? C6 C7 1.519(5) . ? C5 N2 1.354(5) . ? N2 C4 1.461(5) . ? O1 C8 1.430(5) . ? C2 C1 1.523(6) . ? C2 C3 1.526(6) . ? C8 C7 1.505(5) . ? C4 C3 1.508(6) . ? C5A N3A' 1.336(8) . ? C5A N1A 1.336(5) . ? C5A N1A' 1.338(8) . ? C5A N3A 1.338(4) . ? C5A N2A 1.343(4) . ? N1A C1A 1.451(15) . ? N2A C4A 1.434(6) . ? N3A C6A 1.467(7) . ? C1A C2A 1.514(8) . ? C2A C3A 1.519(5) . ? C3A C4A 1.509(8) . ? C6A C7A 1.515(5) . ? C7A C8A 1.508(6) . ? C8A O1A 1.414(7) . ? N1A' C1A' 1.68(10) . ? N3A' C6A' 1.42(4) . ? C1A' C2A' 1.513(9) . ? C2A' C3A' 1.515(9) . ? C3A' C4A' 1.513(9) . ? C6A' C7A' 1.49(4) . ? C7A' C8A' 1.51(5) . ? C8A' O1A' 1.56(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N3 C6 124.8(3) . . ? C5 N1 C1 123.3(3) . . ? N3 C6 C7 112.1(3) . . ? N1 C5 N3 122.0(3) . . ? N1 C5 N2 119.3(4) . . ? N3 C5 N2 118.7(3) . . ? C5 N2 C4 122.6(3) . . ? C1 C2 C3 113.1(4) . . ? O1 C8 C7 109.1(3) . . ? N2 C4 C3 115.1(4) . . ? C8 C7 C6 112.7(3) . . ? N1 C1 C2 113.9(4) . . ? C4 C3 C2 112.7(4) . . ? N3A' C5A N1A 119.7(18) . . ? N3A' C5A N1A' 114(5) . . ? N1A C5A N3A 121.9(9) . . ? N1A' C5A N3A 122(5) . . ? N3A' C5A N2A 116.9(17) . . ? N1A C5A N2A 119.4(9) . . ? N1A' C5A N2A 119(5) . . ? N3A C5A N2A 118.7(4) . . ? C5A N1A C1A 124.1(11) . . ? C5A N2A C4A 123.7(4) . . ? C5A N3A C6A 125.7(4) . . ? N1A C1A C2A 114.2(8) . . ? C1A C2A C3A 112.3(11) . . ? C4A C3A C2A 112.7(10) . . ? N2A C4A C3A 115.3(5) . . ? N3A C6A C7A 112.6(4) . . ? C8A C7A C6A 112.7(4) . . ? O1A C8A C7A 109.9(4) . . ? C5A N1A' C1A' 128(8) . . ? C5A N3A' C6A' 124(3) . . ? C2A' C1A' N1A' 117(5) . . ? C1A' C2A' C3A' 115(7) . . ? C4A' C3A' C2A' 114(7) . . ? N3A' C6A' C7A' 112(3) . . ? C6A' C7A' C8A' 109(3) . . ? C7A' C8A' O1A' 105(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.531 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.103 #===END of CIF for SIII*HI ======================================= data_Htbu _database_code_depnum_ccdc_archive 'CCDC 607809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H15 N3' _chemical_formula_sum 'C8 H15 N3' _chemical_formula_weight 153.23 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 16.595(3) _cell_length_b 10.949(2) _cell_length_c 9.8457(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.995(3) _cell_angle_gamma 90.00 _cell_volume 1735.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4849 _cell_measurement_theta_min 2.24995 _cell_measurement_theta_max 27.50015 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9768 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11131 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3581 _reflns_number_gt 2866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0842P)^2^+0.3542P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3581 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 N2A N 0.45205(8) 0.92962(12) 0.13967(13) 0.0363(3) Uani 1 1 d . . . H2AA H 0.4332 0.9059 0.0535 0.044 Uiso 1 1 calc R . . N1A N 0.58920(8) 0.95331(14) 0.13832(14) 0.0406(3) Uani 1 1 d . . . N3A N 0.55228(8) 0.86144(13) 0.33281(15) 0.0422(4) Uani 1 1 d . . . C4A C 0.53524(9) 0.91552(14) 0.20360(15) 0.0331(3) Uani 1 1 d . . . C8AA C 0.39523(10) 0.98402(16) 0.21520(17) 0.0395(4) Uani 1 1 d . . . H8AA H 0.3498 1.0240 0.1476 0.047 Uiso 1 1 calc R . . H8AB H 0.4250 1.0472 0.2783 0.047 Uiso 1 1 calc R . . C3A C 0.63773(11) 0.84961(17) 0.41296(18) 0.0465(4) Uani 1 1 d . . . H3AA H 0.6565 0.7655 0.4062 0.056 Uiso 1 1 calc R . . H3AB H 0.6409 0.8671 0.5117 0.056 Uiso 1 1 calc R . . C7A C 0.35872(11) 0.89314(18) 0.29984(19) 0.0458(4) Uani 1 1 d . . . H7AA H 0.3164 0.9343 0.3375 0.055 Uiso 1 1 calc R . . H7AB H 0.3313 0.8276 0.2378 0.055 Uiso 1 1 calc R . . C2A C 0.69373(11) 0.93554(18) 0.36026(18) 0.0480(4) Uani 1 1 d . . . H2AB H 0.7519 0.9149 0.4019 0.058 Uiso 1 1 calc R . . H2AC H 0.6840 1.0195 0.3867 0.058 Uiso 1 1 calc R . . C1A C 0.67586(11) 0.9249(2) 0.20308(19) 0.0515(5) Uani 1 1 d . . . H1AB H 0.7119 0.9812 0.1676 0.062 Uiso 1 1 calc R . . H1AC H 0.6883 0.8417 0.1777 0.062 Uiso 1 1 calc R . . C5A C 0.49315(11) 0.77630(17) 0.3715(2) 0.0499(5) Uani 1 1 d . . . H5AA H 0.5234 0.7231 0.4467 0.060 Uiso 1 1 calc R . . H5AB H 0.4693 0.7245 0.2906 0.060 Uiso 1 1 calc R . . C6A C 0.42294(11) 0.83764(18) 0.41954(19) 0.0492(4) Uani 1 1 d . . . H6AA H 0.3959 0.7773 0.4673 0.059 Uiso 1 1 calc R . . H6AB H 0.4460 0.9019 0.4871 0.059 Uiso 1 1 calc R . . N2 N 0.06731(8) 0.86345(12) 0.99100(14) 0.0369(3) Uani 1 1 d . . . H2A H 0.0667 0.8888 1.0745 0.044 Uiso 1 1 calc R . . N1 N -0.06947(8) 0.89322(12) 0.87706(14) 0.0361(3) Uani 1 1 d . . . C4 C -0.00503(9) 0.82316(13) 0.90113(15) 0.0317(3) Uani 1 1 d . . . C1 C -0.14635(10) 0.84095(15) 0.79297(18) 0.0399(4) Uani 1 1 d . . . H1B H -0.1848 0.9068 0.7529 0.048 Uiso 1 1 calc R . . H1C H -0.1727 0.7911 0.8527 0.048 Uiso 1 1 calc R . . N3 N -0.00135(8) 0.70926(13) 0.84591(15) 0.0427(4) Uani 1 1 d . . . C3 C -0.07090(10) 0.66145(15) 0.74031(18) 0.0429(4) Uani 1 1 d . . . H3A H -0.1009 0.6013 0.7831 0.051 Uiso 1 1 calc R . . H3B H -0.0502 0.6201 0.6672 0.051 Uiso 1 1 calc R . . C2 C -0.12919(11) 0.76246(16) 0.67582(17) 0.0435(4) Uani 1 1 d . . . H2B H -0.1812 0.7280 0.6200 0.052 Uiso 1 1 calc R . . H2C H -0.1041 0.8121 0.6142 0.052 Uiso 1 1 calc R . . C8 C 0.14486(10) 0.86353(16) 0.9457(2) 0.0438(4) Uani 1 1 d . . . H8A H 0.1803 0.9296 0.9939 0.053 Uiso 1 1 calc R . . H8B H 0.1324 0.8807 0.8451 0.053 Uiso 1 1 calc R . . C5 C 0.06093(12) 0.61982(15) 0.9139(2) 0.0507(5) Uani 1 1 d . . . H5A H 0.0416 0.5382 0.8803 0.061 Uiso 1 1 calc R . . H5B H 0.0652 0.6219 1.0149 0.061 Uiso 1 1 calc R . . C6 C 0.14640(11) 0.63934(17) 0.8893(2) 0.0517(5) Uani 1 1 d . . . H6A H 0.1411 0.6552 0.7896 0.062 Uiso 1 1 calc R . . H6B H 0.1790 0.5645 0.9139 0.062 Uiso 1 1 calc R . . C7 C 0.19228(11) 0.74455(18) 0.9737(2) 0.0527(5) Uani 1 1 d . . . H7A H 0.2024 0.7250 1.0736 0.063 Uiso 1 1 calc R . . H7B H 0.2463 0.7545 0.9513 0.063 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 N2A 0.0329(7) 0.0462(8) 0.0291(6) -0.0001(5) 0.0062(5) 0.0006(5) N1A 0.0332(7) 0.0568(9) 0.0324(7) 0.0023(6) 0.0092(5) 0.0014(6) N3A 0.0371(7) 0.0501(8) 0.0387(7) 0.0131(6) 0.0079(6) 0.0048(6) C4A 0.0358(8) 0.0345(7) 0.0282(7) -0.0021(6) 0.0065(6) 0.0009(6) C8AA 0.0342(8) 0.0455(9) 0.0394(8) 0.0060(7) 0.0101(6) 0.0038(7) C3A 0.0451(10) 0.0525(10) 0.0376(9) 0.0011(7) 0.0014(7) 0.0100(8) C7A 0.0384(9) 0.0552(10) 0.0469(10) 0.0042(8) 0.0163(7) -0.0050(8) C2A 0.0369(9) 0.0576(11) 0.0446(10) -0.0061(8) 0.0007(7) 0.0040(8) C1A 0.0350(9) 0.0759(13) 0.0441(10) -0.0016(9) 0.0107(7) 0.0042(8) C5A 0.0517(10) 0.0452(10) 0.0542(11) 0.0186(8) 0.0154(8) 0.0028(8) C6A 0.0489(10) 0.0565(11) 0.0458(10) 0.0132(8) 0.0180(8) -0.0049(8) N2 0.0347(7) 0.0371(7) 0.0381(7) -0.0103(5) 0.0069(6) 0.0024(5) N1 0.0337(7) 0.0324(6) 0.0412(7) -0.0055(5) 0.0067(5) 0.0005(5) C4 0.0350(8) 0.0284(7) 0.0324(7) -0.0035(6) 0.0097(6) -0.0016(6) C1 0.0343(8) 0.0410(9) 0.0429(9) -0.0008(7) 0.0063(7) -0.0016(6) N3 0.0379(7) 0.0322(7) 0.0539(8) -0.0112(6) 0.0033(6) 0.0022(5) C3 0.0447(9) 0.0389(8) 0.0464(9) -0.0140(7) 0.0137(7) -0.0108(7) C2 0.0419(9) 0.0510(10) 0.0358(8) -0.0047(7) 0.0059(7) -0.0117(7) C8 0.0337(8) 0.0419(9) 0.0555(10) -0.0088(7) 0.0100(7) -0.0011(7) C5 0.0589(11) 0.0289(8) 0.0603(11) -0.0028(7) 0.0064(9) 0.0064(8) C6 0.0489(10) 0.0476(10) 0.0549(11) -0.0105(8) 0.0055(8) 0.0185(8) C7 0.0374(9) 0.0574(11) 0.0602(11) -0.0118(9) 0.0057(8) 0.0126(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N2A C4A 1.3804(19) . ? N2A C8AA 1.462(2) . ? N1A C4A 1.290(2) . ? N1A C1A 1.459(2) . ? N3A C4A 1.369(2) . ? N3A C3A 1.452(2) . ? N3A C5A 1.469(2) . ? C8AA C7A 1.515(2) . ? C3A C2A 1.500(3) . ? C7A C6A 1.512(3) . ? C2A C1A 1.508(3) . ? C5A C6A 1.516(3) . ? N2 C4 1.3802(19) . ? N2 C8 1.460(2) . ? N1 C4 1.291(2) . ? N1 C1 1.4594(19) . ? C4 N3 1.368(2) . ? C1 C2 1.519(2) . ? N3 C3 1.451(2) . ? N3 C5 1.463(2) . ? C3 C2 1.505(2) . ? C8 C7 1.512(2) . ? C5 C6 1.511(3) . ? C6 C7 1.514(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4A N2A C8AA 120.71(13) . . ? C4A N1A C1A 116.33(14) . . ? C4A N3A C3A 119.90(14) . . ? C4A N3A C5A 120.97(14) . . ? C3A N3A C5A 115.36(14) . . ? N1A C4A N3A 126.11(14) . . ? N1A C4A N2A 118.36(13) . . ? N3A C4A N2A 115.53(14) . . ? N2A C8AA C7A 113.90(14) . . ? N3A C3A C2A 111.17(14) . . ? C6A C7A C8AA 113.11(14) . . ? C3A C2A C1A 108.79(15) . . ? N1A C1A C2A 111.14(14) . . ? N3A C5A C6A 114.32(15) . . ? C7A C6A C5A 112.63(15) . . ? C4 N2 C8 119.90(13) . . ? C4 N1 C1 116.29(13) . . ? N1 C4 N3 125.70(14) . . ? N1 C4 N2 118.77(13) . . ? N3 C4 N2 115.52(13) . . ? N1 C1 C2 110.72(13) . . ? C4 N3 C3 120.63(13) . . ? C4 N3 C5 121.52(14) . . ? C3 N3 C5 115.96(14) . . ? N3 C3 C2 110.84(13) . . ? C3 C2 C1 108.34(13) . . ? N2 C8 C7 113.69(16) . . ? N3 C5 C6 114.75(16) . . ? C5 C6 C7 112.74(15) . . ? C8 C7 C6 112.63(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.590 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.043 #===END of CIF for Htbu ================================= data_Htbd _database_code_depnum_ccdc_archive 'CCDC 607810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H13 N3' _chemical_formula_sum 'C7 H13 N3' _chemical_formula_weight 139.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.937(3) _cell_length_b 8.520(5) _cell_length_c 8.671(5) _cell_angle_alpha 67.410(9) _cell_angle_beta 73.543(10) _cell_angle_gamma 71.570(9) _cell_volume 377.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1863 _cell_measurement_theta_min 2.589 _cell_measurement_theta_max 27.5225 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 152 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9672 _exptl_absorpt_correction_T_max 0.9933 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2203 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1310 _reflns_number_gt 1165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0960P)^2^+0.0934P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1310 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 N3 N 0.4769(2) 0.91856(18) 0.80105(17) 0.0330(4) Uani 1 1 d . . . N2 N 0.7000(3) 1.12330(18) 0.59852(19) 0.0371(4) Uani 1 1 d . . . H2A H 0.7611 1.1561 0.4905 0.044 Uiso 1 1 calc R . . C3 C 0.6810(3) 0.9553(2) 0.6792(2) 0.0322(4) Uani 1 1 d . . . C4 C 0.2391(3) 1.0409(2) 0.7858(2) 0.0369(5) Uani 1 1 d . . . H4A H 0.1132 0.9781 0.8562 0.044 Uiso 1 1 calc R . . H4B H 0.2180 1.0817 0.6675 0.044 Uiso 1 1 calc R . . N1 N 0.8449(3) 0.82256(19) 0.6502(2) 0.0400(4) Uani 1 1 d . . . C7 C 0.6201(3) 1.2500(2) 0.6892(3) 0.0406(5) Uani 1 1 d . . . H7A H 0.7043 1.3447 0.6264 0.049 Uiso 1 1 calc R . . H7B H 0.6674 1.1926 0.8010 0.049 Uiso 1 1 calc R . . C5 C 0.2049(3) 1.1976(2) 0.8387(2) 0.0394(5) Uani 1 1 d . . . H5A H 0.2517 1.1570 0.9498 0.047 Uiso 1 1 calc R . . H5B H 0.0332 1.2568 0.8516 0.047 Uiso 1 1 calc R . . C2 C 0.4861(4) 0.7366(2) 0.8266(3) 0.0435(5) Uani 1 1 d . . . H2B H 0.3814 0.7296 0.7612 0.052 Uiso 1 1 calc R . . H2C H 0.4389 0.6724 0.9470 0.052 Uiso 1 1 calc R . . C1 C 0.7534(4) 0.6669(2) 0.7599(3) 0.0467(5) Uani 1 1 d . . . H1B H 0.8415 0.6010 0.8541 0.056 Uiso 1 1 calc R . . H1C H 0.7704 0.5902 0.6951 0.056 Uiso 1 1 calc R . . C6 C 0.3497(3) 1.3287(2) 0.7140(3) 0.0453(5) Uani 1 1 d . . . H6A H 0.3152 1.4274 0.7555 0.054 Uiso 1 1 calc R . . H6B H 0.2981 1.3738 0.6040 0.054 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 N3 0.0281(8) 0.0348(8) 0.0324(8) -0.0094(6) 0.0017(6) -0.0107(6) N2 0.0318(8) 0.0385(8) 0.0342(8) -0.0084(6) 0.0037(6) -0.0123(6) C3 0.0288(9) 0.0398(9) 0.0279(9) -0.0110(7) -0.0011(7) -0.0116(7) C4 0.0245(9) 0.0463(10) 0.0368(10) -0.0107(8) 0.0000(7) -0.0126(7) N1 0.0342(8) 0.0398(8) 0.0415(9) -0.0150(7) 0.0045(6) -0.0106(6) C7 0.0348(10) 0.0354(9) 0.0492(11) -0.0115(8) -0.0004(8) -0.0142(7) C5 0.0261(9) 0.0414(10) 0.0428(10) -0.0120(8) -0.0016(7) -0.0039(7) C2 0.0458(11) 0.0377(10) 0.0448(11) -0.0119(8) 0.0023(8) -0.0181(8) C1 0.0487(12) 0.0376(10) 0.0490(12) -0.0175(9) 0.0055(9) -0.0120(8) C6 0.0372(10) 0.0350(10) 0.0538(12) -0.0105(8) -0.0032(9) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C3 1.394(2) . y N3 C2 1.465(2) . ? N3 C4 1.472(2) . ? N2 C3 1.356(2) . y N2 C7 1.458(2) . ? C3 N1 1.293(2) . y C4 C5 1.511(3) . ? N1 C1 1.467(2) . ? C7 C6 1.519(3) . ? C5 C6 1.519(3) . ? C2 C1 1.534(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N3 C2 104.92(14) . . y C3 N3 C4 120.69(14) . . y C2 N3 C4 115.71(14) . . ? C3 N2 C7 121.29(15) . . y N1 C3 N2 123.50(16) . . y N1 C3 N3 116.53(16) . . y N2 C3 N3 119.96(15) . . y N3 C4 C5 113.73(14) . . ? C3 N1 C1 106.34(15) . . y N2 C7 C6 114.30(16) . . ? C4 C5 C6 113.88(16) . . ? N3 C2 C1 102.23(14) . . ? N1 C1 C2 105.28(15) . . ? C5 C6 C7 112.67(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.448 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.052 #===END of CIF for Htbd =========================================