# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_NaTTC_120K _audit_creation_date 2013-06-13 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H16 N6 Na2 O6 S6' _chemical_formula_sum 'C6 H16 N6 Na2 O6 S6' _chemical_formula_weight 506.59 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Na1 C3 H8 O3 N3 S3' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 10.3697(4) _cell_length_b 12.6801(3) _cell_length_c 7.7756(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.059(4) _cell_angle_gamma 90.00 _cell_volume 966.37(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6298 _cell_measurement_temperature 120 _cell_measurement_theta_max 71.2560 _cell_measurement_theta_min 4.4830 _exptl_absorpt_coefficient_mu 7.350 _exptl_absorpt_correction_T_max 0.703 _exptl_absorpt_correction_T_min 0.273 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.3399 _exptl_crystal_size_mid 0.0971 _exptl_crystal_size_min 0.0512 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 10524 _diffrn_reflns_theta_full 70.9317 _diffrn_reflns_theta_max 71.22 _diffrn_reflns_theta_min 4.51 _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_measured_fraction_theta_max 0.9897 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 62.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega 35.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 120.0000 35 #__ type_ start__ end____ width___ exp.time_ 3 omega 0.00 39.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 0.0000 39 #__ type_ start__ end____ width___ exp.time_ 4 omega -15.00 12.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - -54.7500 77.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 5 omega -117.00 -25.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -180.0000 92 #__ type_ start__ end____ width___ exp.time_ 6 omega -78.00 -19.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - -54.7500 77.0000 -60.0000 59 #__ type_ start__ end____ width___ exp.time_ 7 omega 76.00 103.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 8 omega 93.00 121.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 9 omega 82.00 125.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - 54.7500 37.0000 -150.0000 43 #__ type_ start__ end____ width___ exp.time_ 10 omega 37.00 63.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 11 omega 38.00 112.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 0.0000 90.0000 74 #__ type_ start__ end____ width___ exp.time_ 12 omega 59.00 86.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 13 omega 45.00 80.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 150.0000 35 #__ type_ start__ end____ width___ exp.time_ 14 omega 38.00 66.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -180.0000 28 #__ type_ start__ end____ width___ exp.time_ 15 omega 38.00 72.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -150.0000 34 #__ type_ start__ end____ width___ exp.time_ 16 omega 82.00 153.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 -90.0000 71 #__ type_ start__ end____ width___ exp.time_ 17 omega 53.00 83.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -30.0000 30 #__ type_ start__ end____ width___ exp.time_ 18 omega 69.00 134.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 30.0000 65 #__ type_ start__ end____ width___ exp.time_ 19 omega 65.00 104.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -150.0000 39 #__ type_ start__ end____ width___ exp.time_ 20 omega 39.00 69.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 0.0000 30 #__ type_ start__ end____ width___ exp.time_ 21 omega 112.00 140.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 22 omega 150.00 178.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 23 omega 40.00 91.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 150.0000 51 #__ type_ start__ end____ width___ exp.time_ 24 omega 114.00 139.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 25 omega 41.00 68.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 26 omega 124.00 162.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 0.0000 90.0000 38 #__ type_ start__ end____ width___ exp.time_ 27 omega 37.00 64.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 28 omega -30.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 29 omega -21.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 30.0000 90 #__ type_ start__ end____ width___ exp.time_ 30 omega -127.00 -29.00 1.0000 1.3700 omega____ theta____ kappa____ phi______ frames - -54.7500 -37.0000 -90.0000 98 #__ type_ start__ end____ width___ exp.time_ 31 omega -125.00 -34.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 30.0000 91 #__ type_ start__ end____ width___ exp.time_ 32 omega 90.00 123.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -30.0000 33 #__ type_ start__ end____ width___ exp.time_ 33 omega 93.00 119.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 105.0000 -80.0000 26 #__ type_ start__ end____ width___ exp.time_ 34 omega -137.00 -99.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -150.0000 38 #__ type_ start__ end____ width___ exp.time_ 35 omega -100.00 -74.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 36 omega -83.00 -57.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 37 omega 41.00 67.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 38 omega 96.00 131.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 0.0000 35 #__ type_ start__ end____ width___ exp.time_ 39 omega 97.00 127.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -92.0000 -132.4267 30 #__ type_ start__ end____ width___ exp.time_ 40 omega 65.00 91.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 41 omega 38.00 64.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 42 omega 41.00 66.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 43 omega 53.00 79.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 44 omega 88.00 114.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 45 omega 131.00 166.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -60.0000 35 #__ type_ start__ end____ width___ exp.time_ 46 omega 142.00 167.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 47 omega 36.00 91.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 -90.0000 55 #__ type_ start__ end____ width___ exp.time_ 48 omega 120.00 147.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 49 omega 101.00 126.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 90.0000 25 #__ type_ start__ end____ width___ exp.time_ 50 omega 84.00 113.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 96.1262 29 #__ type_ start__ end____ width___ exp.time_ 51 omega 103.00 129.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 -61.4574 26 #__ type_ start__ end____ width___ exp.time_ 52 omega 109.00 134.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 53 omega 42.00 139.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 0.0000 97 #__ type_ start__ end____ width___ exp.time_ 54 omega 44.00 70.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 55 omega 40.00 68.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 56 omega 37.00 62.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 57 omega 109.00 134.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 30.0000 25 #__ type_ start__ end____ width___ exp.time_ 58 omega 93.00 119.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 59 omega 127.00 162.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -120.0000 35 #__ type_ start__ end____ width___ exp.time_ 60 omega 85.00 111.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 61 omega 55.00 81.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 62 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 90.0000 45 #__ type_ start__ end____ width___ exp.time_ 63 omega -30.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 150.0000 100 #__ type_ start__ end____ width___ exp.time_ 64 omega -69.00 21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -60.0000 90 #__ type_ start__ end____ width___ exp.time_ 65 omega -73.00 15.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -19.0000 -90.0000 88 #__ type_ start__ end____ width___ exp.time_ 66 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 30.0000 45 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1064159000 _diffrn_orient_matrix_UB_12 -0.0770176000 _diffrn_orient_matrix_UB_13 -0.1202899000 _diffrn_orient_matrix_UB_21 0.1075368000 _diffrn_orient_matrix_UB_22 -0.0885970000 _diffrn_orient_matrix_UB_23 0.0462866000 _diffrn_orient_matrix_UB_31 -0.0425377000 _diffrn_orient_matrix_UB_32 -0.0313049000 _diffrn_orient_matrix_UB_33 0.1653141000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3531 _reflns_number_total 3723 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.374 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(2) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3723 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0290 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.3656P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.0931 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2. Restrained distances O6-H6A 0.958 with sigma of 0.02 H6B-O6 = O6-H6A 0.958 with sigma of 0.02 H1A-O1 = O1-H1B 0.958 with sigma of 0.02 H5B-O5 = O5-H5A 0.958 with sigma of 0.02 H2B-O2 = O2-H2A 0.958 with sigma of 0.02 H3B-O3 = O3-H3A 0.958 with sigma of 0.02 H4B-O4 = O4-H4A 0.958 with sigma of 0.02 H6B-H6A 1.515 with sigma of 0.04 H1A-H1B 1.515 with sigma of 0.04 H5B-H5A 1.515 with sigma of 0.04 H2B-H2A 1.515 with sigma of 0.04 H3B-H3A 1.515 with sigma of 0.04 H4B-H4A 1.515 with sigma of 0.04 3.a Aromatic/amide H refined with riding coordinates: N11(H11), N12(H12), N9(H9), N10(H10) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H1A H 0.876(3) 0.665(3) 0.123(6) 0.024(10) Uiso 1 1 d D . . H1B H 0.995(6) 0.659(4) 0.055(9) 0.11(3) Uiso 1 1 d D . . H2A H 1.180(2) 0.792(3) 0.552(4) 0.019(9) Uiso 1 1 d D . . H2B H 1.092(4) 0.839(3) 0.374(5) 0.053(15) Uiso 1 1 d D . . H3A H 0.845(5) 0.545(5) 0.518(9) 0.13(3) Uiso 1 1 d D . . H3B H 0.888(4) 0.640(3) 0.645(5) 0.027(11) Uiso 1 1 d D . . H4A H 1.015(5) 0.493(2) -0.218(6) 0.051(14) Uiso 1 1 d D . . H4B H 1.121(2) 0.423(4) -0.099(7) 0.054(15) Uiso 1 1 d D . . H5A H 1.015(4) 0.378(3) 0.444(5) 0.048(14) Uiso 1 1 d D . . H5B H 1.138(3) 0.399(4) 0.383(7) 0.062(18) Uiso 1 1 d D . . H6A H 0.814(3) 0.244(4) -0.066(3) 0.032(12) Uiso 1 1 d D . . H6B H 0.872(6) 0.211(5) 0.130(6) 0.11(3) Uiso 1 1 d D . . O1 O 0.9455(2) 0.6217(2) 0.1158(3) 0.0217(5) Uani 1 1 d D . . O2 O 1.0954(2) 0.7913(2) 0.4663(3) 0.0222(5) Uani 1 1 d D . . O3 O 0.9205(2) 0.5871(2) 0.5831(3) 0.0260(5) Uani 1 1 d D . . O4 O 1.0236(3) 0.4301(2) -0.1487(3) 0.0298(5) Uani 1 1 d D . . O5 O 1.0521(3) 0.4221(2) 0.3752(3) 0.0206(5) Uani 1 1 d D . . O6 O 0.8932(2) 0.2468(2) 0.0371(3) 0.0230(5) Uani 1 1 d D . . Na1 Na 0.91268(13) 0.43720(11) 0.06624(18) 0.0236(3) Uani 1 1 d . . . Na2 Na 1.08278(12) 0.60578(11) 0.42812(17) 0.0217(3) Uani 1 1 d . . . C16 C 0.3915(3) 0.6990(3) -0.1589(4) 0.0175(6) Uani 1 1 d . . . C17 C 0.5829(3) 0.7878(3) 0.0556(4) 0.0179(7) Uani 1 1 d . . . C18 C 0.3988(3) 0.8823(3) -0.1585(4) 0.0172(6) Uani 1 1 d . . . N5 N 0.3367(3) 0.7919(2) -0.2329(3) 0.0183(6) Uani 1 1 d . . . N11 N 0.5210(3) 0.8787(2) -0.0187(4) 0.0182(6) Uani 1 1 d . . . H11 H 0.5602 0.9373 0.0239 0.022 Uiso 1 1 calc R . . N12 N 0.5125(3) 0.6990(2) -0.0173(4) 0.0172(6) Uani 1 1 d . . . H12 H 0.5460 0.6392 0.0281 0.021 Uiso 1 1 calc R . . S4 S 0.31341(8) 0.58333(6) -0.22984(10) 0.0200(2) Uani 1 1 d . . . S5 S 0.73099(8) 0.78508(6) 0.22493(10) 0.0186(2) Uani 1 1 d . . . S6 S 0.32829(8) 1.00102(6) -0.22940(10) 0.0195(2) Uani 1 1 d . . . C13 C 0.3977(3) 0.8527(3) 0.3439(4) 0.0162(6) Uani 1 1 d . . . C14 C 0.5838(3) 0.7622(3) 0.5602(4) 0.0158(6) Uani 1 1 d . . . C15 C 0.3945(3) 0.6698(3) 0.3504(4) 0.0168(6) Uani 1 1 d . . . N3 N 0.3376(3) 0.7617(2) 0.2754(4) 0.0176(6) Uani 1 1 d . . . N9 N 0.5187(3) 0.8519(2) 0.4863(4) 0.0177(6) Uani 1 1 d . . . H9 H 0.5546 0.9113 0.5304 0.021 Uiso 1 1 calc R . . N10 N 0.5172(3) 0.6723(2) 0.4899(4) 0.0177(6) Uani 1 1 d . . . H10 H 0.5537 0.6132 0.5348 0.021 Uiso 1 1 calc R . . S1 S 0.31905(8) 0.55348(6) 0.27864(10) 0.0195(2) Uani 1 1 d . . . S2 S 0.73403(8) 0.76292(6) 0.72885(10) 0.0184(2) Uani 1 1 d . . . S3 S 0.32932(8) 0.97037(6) 0.25999(10) 0.01944(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0239(11) 0.0188(13) 0.0221(12) 0.0019(10) 0.0072(10) 0.0024(10) O2 0.0227(12) 0.0198(12) 0.0227(11) 0.0000(9) 0.0054(10) 0.0001(9) O3 0.0251(12) 0.0260(12) 0.0278(12) 0.0008(10) 0.0098(10) 0.0014(10) O4 0.0286(12) 0.0311(13) 0.0312(13) 0.0031(11) 0.0116(11) 0.0052(11) O5 0.0222(11) 0.0159(12) 0.0232(11) 0.0007(10) 0.0067(10) 0.0029(10) O6 0.0223(11) 0.0235(13) 0.0222(11) -0.0012(10) 0.0059(10) 0.0000(10) Na1 0.0299(7) 0.0194(7) 0.0201(6) -0.0021(5) 0.0064(5) -0.0006(6) Na2 0.0250(6) 0.0184(7) 0.0211(6) -0.0012(5) 0.0066(5) -0.0018(5) C16 0.0184(14) 0.0185(17) 0.0174(15) 0.0022(12) 0.0082(12) 0.0013(13) C17 0.0190(15) 0.0198(18) 0.0166(14) 0.0025(14) 0.0082(12) 0.0024(13) C18 0.0172(14) 0.0191(16) 0.0165(15) 0.0005(13) 0.0070(13) -0.0013(12) N5 0.0205(13) 0.0170(15) 0.0175(13) 0.0011(11) 0.0062(11) -0.0002(11) N11 0.0192(14) 0.0125(14) 0.0220(13) -0.0015(11) 0.0055(11) 0.0003(10) N12 0.0194(12) 0.0135(15) 0.0171(13) 0.0014(11) 0.0039(11) 0.0013(11) S4 0.0224(4) 0.0146(4) 0.0200(4) -0.0002(3) 0.0030(3) -0.0023(3) S5 0.0184(4) 0.0177(5) 0.0174(4) -0.0004(3) 0.0025(3) 0.0002(3) S6 0.0215(4) 0.0141(4) 0.0202(4) 0.0000(3) 0.0031(3) 0.0011(3) C13 0.0175(13) 0.0170(16) 0.0145(15) 0.0008(12) 0.0059(12) 0.0008(12) C14 0.0173(14) 0.0154(16) 0.0148(14) 0.0033(12) 0.0055(12) 0.0033(13) C15 0.0193(14) 0.0139(15) 0.0186(15) -0.0002(13) 0.0081(12) -0.0002(13) N3 0.0188(12) 0.0150(15) 0.0182(13) 0.0009(10) 0.0051(11) -0.0007(11) N9 0.0212(14) 0.0119(14) 0.0211(13) -0.0006(11) 0.0082(11) -0.0009(11) N10 0.0204(13) 0.0142(14) 0.0176(12) 0.0029(11) 0.0049(11) 0.0009(11) S1 0.0216(4) 0.0142(5) 0.0208(4) -0.0011(3) 0.0044(3) -0.0014(3) S2 0.0186(4) 0.0168(5) 0.0178(4) 0.0007(3) 0.0031(3) -0.0003(3) S3 0.0220(4) 0.0137(4) 0.0197(4) 0.0007(3) 0.0028(3) 0.0023(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 O1 Na1 2.377(3) . ? O1 Na2 2.389(3) . ? O2 Na2 2.369(3) . ? O3 Na2 2.380(3) . ? O4 Na1 2.319(3) . ? O5 Na1 2.373(3) . ? O5 Na2 2.368(3) . ? O6 Na1 2.427(3) . ? Na1 Na2 3.5152(14) . ? Na1 S6 3.2525(15) 2_645 ? Na1 S3 2.9583(16) 2_645 ? Na2 S4 2.9530(15) 1_656 ? Na2 S1 3.1069(14) 1_655 ? C16 N5 1.353(4) . ? C16 N12 1.373(4) . ? C16 S4 1.679(3) . ? C17 N11 1.353(5) . ? C17 N12 1.361(5) . ? C17 S5 1.665(3) . ? C18 N5 1.349(5) . ? C18 N11 1.375(5) . ? C18 S6 1.685(4) . ? S4 Na2 2.9530(15) 1_454 ? S6 Na1 3.2525(15) 2_655 ? C13 N3 1.337(4) . ? C13 N9 1.376(4) . ? C13 S3 1.689(3) . ? C14 N9 1.352(4) . ? C14 N10 1.352(5) . ? C14 S2 1.677(3) . ? C15 N3 1.349(5) . ? C15 N10 1.377(4) . ? C15 S1 1.678(3) . ? S1 Na2 3.1069(14) 1_455 ? S3 Na1 2.9583(16) 2_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 Na1 O1 Na2 95.06(10) . . ? Na2 O5 Na1 95.72(10) . . ? O1 Na1 O6 175.66(11) . . ? O1 Na1 Na2 42.60(7) . . ? O1 Na1 S6 77.27(7) . 2_645 ? O1 Na1 S3 92.04(8) . 2_645 ? O4 Na1 O1 94.38(10) . . ? O4 Na1 O5 116.42(10) . . ? O4 Na1 O6 86.56(10) . . ? O4 Na1 Na2 111.28(8) . . ? O4 Na1 S6 156.29(9) . 2_645 ? O4 Na1 S3 82.48(8) . 2_645 ? O5 Na1 O1 84.68(10) . . ? O5 Na1 O6 91.10(10) . . ? O5 Na1 Na2 42.09(7) . . ? O5 Na1 S6 85.23(7) . 2_645 ? O5 Na1 S3 160.98(8) . 2_645 ? O6 Na1 Na2 133.19(8) . . ? O6 Na1 S6 103.46(7) . 2_645 ? O6 Na1 S3 92.28(8) . 2_645 ? S6 Na1 Na2 77.59(3) 2_645 . ? S3 Na1 Na2 131.55(5) 2_645 . ? S3 Na1 S6 75.79(4) 2_645 2_645 ? O1 Na2 Na1 42.34(7) . . ? O1 Na2 S4 164.19(8) . 1_656 ? O1 Na2 S1 85.33(7) . 1_655 ? O2 Na2 O1 91.94(10) . . ? O2 Na2 O3 93.14(10) . . ? O2 Na2 Na1 134.17(7) . . ? O2 Na2 S4 89.29(7) . 1_656 ? O2 Na2 S1 103.93(7) . 1_655 ? O3 Na2 O1 103.77(9) . . ? O3 Na2 Na1 95.26(7) . . ? O3 Na2 S4 91.89(7) . 1_656 ? O3 Na2 S1 160.47(9) . 1_655 ? O5 Na2 O1 84.53(9) . . ? O5 Na2 O2 175.49(11) . . ? O5 Na2 O3 85.00(10) . . ? O5 Na2 Na1 42.20(7) . . ? O5 Na2 S4 94.88(8) . 1_656 ? O5 Na2 S1 78.62(7) . 1_655 ? S4 Na2 Na1 135.19(5) 1_656 . ? S4 Na2 S1 79.09(4) 1_656 1_655 ? S1 Na2 Na1 79.73(4) 1_655 . ? N5 C16 N12 119.2(3) . . ? N5 C16 S4 122.0(3) . . ? N12 C16 S4 118.7(3) . . ? N11 C17 N12 114.3(3) . . ? N11 C17 S5 122.8(3) . . ? N12 C17 S5 122.9(3) . . ? N5 C18 N11 119.9(3) . . ? N5 C18 S6 121.5(3) . . ? N11 C18 S6 118.6(3) . . ? C18 N5 C16 118.8(3) . . ? C17 N11 C18 123.5(3) . . ? C17 N12 C16 124.0(3) . . ? C16 S4 Na2 111.94(12) . 1_454 ? C18 S6 Na1 87.51(11) . 2_655 ? N3 C13 N9 119.9(3) . . ? N3 C13 S3 121.8(2) . . ? N9 C13 S3 118.3(3) . . ? N9 C14 N10 114.8(3) . . ? N9 C14 S2 122.3(3) . . ? N10 C14 S2 122.8(3) . . ? N3 C15 N10 118.8(3) . . ? N3 C15 S1 121.6(3) . . ? N10 C15 S1 119.5(3) . . ? C13 N3 C15 119.5(3) . . ? C14 N9 C13 123.1(3) . . ? C14 N10 C15 123.8(3) . . ? C15 S1 Na2 91.55(11) . 1_455 ? C13 S3 Na1 109.71(12) . 2_655 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 -8 0 0.0501 0.0022 -8.0023 0.0114 0.6147 0.7097 0.2523 0 8 0 0.0471 -0.0022 8.0023 -0.0114 -0.6147 -0.7097 -0.2523 -6 0 0 0.0276 -5.9974 0.0017 0.0118 0.6367 -0.6446 0.2570 6 0 0 0.0236 5.9974 -0.0017 -0.0118 -0.6367 0.6446 -0.2570 -2 -2 5 0.1654 -1.9839 -1.9960 4.9951 -0.2360 0.1947 0.9726 2 2 -5 0.1624 1.9839 1.9960 -4.9951 0.2360 -0.1947 -0.9726 4 -3 -5 0.1496 3.9844 -3.0061 -4.9919 0.4080 0.4637 -0.9006 -4 3 5 0.1496 -3.9844 3.0061 4.9919 -0.4080 -0.4637 0.9006 _database_code_depnum_ccdc_archive 'CCDC 944676' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_NaTTC_RT _audit_creation_date 2013-06-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C3 H8 N3 Na O3 S3' _chemical_formula_sum 'C3 H8 N3 Na O3 S3' _chemical_formula_weight 253.29 _chemical_melting_point ? _chemical_oxdiff_formula 'Na C3 H8 O3 N3 S3' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 10.4530(2) _cell_length_b 12.7369(2) _cell_length_c 7.86207(17) _cell_angle_alpha 90.00 _cell_angle_beta 109.644(2) _cell_angle_gamma 90.00 _cell_volume 985.83(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10603 _cell_measurement_temperature 298 _cell_measurement_theta_max 71.1740 _cell_measurement_theta_min 3.4450 _exptl_absorpt_coefficient_mu 7.204 _exptl_absorpt_correction_T_max 0.711 _exptl_absorpt_correction_T_min 0.312 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.2605 _exptl_crystal_size_mid 0.0934 _exptl_crystal_size_min 0.0504 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0096 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 17362 _diffrn_reflns_theta_full 70.9317 _diffrn_reflns_theta_max 71.35 _diffrn_reflns_theta_min 4.49 _diffrn_ambient_temperature 298 _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_measured_fraction_theta_max 0.9754 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 43.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega 33.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 120.0000 44 #__ type_ start__ end____ width___ exp.time_ 3 omega -5.00 21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega 32.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -180.0000 37 #__ type_ start__ end____ width___ exp.time_ 5 omega 33.00 74.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -30.0000 41 #__ type_ start__ end____ width___ exp.time_ 6 omega -65.00 -39.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega -124.00 -85.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 -60.0000 39 #__ type_ start__ end____ width___ exp.time_ 8 omega 76.00 123.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 30.0000 47 #__ type_ start__ end____ width___ exp.time_ 9 omega 79.00 126.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -180.0000 47 #__ type_ start__ end____ width___ exp.time_ 10 omega 42.00 113.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 120.0000 71 #__ type_ start__ end____ width___ exp.time_ 11 omega -17.00 70.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 -37.0000 120.0000 87 #__ type_ start__ end____ width___ exp.time_ 12 omega -85.00 -24.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 63.0000 30.0000 61 #__ type_ start__ end____ width___ exp.time_ 13 omega -80.00 -40.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -75.0000 -52.8755 40 #__ type_ start__ end____ width___ exp.time_ 14 omega -110.00 -43.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 -120.0000 67 #__ type_ start__ end____ width___ exp.time_ 15 omega -66.00 -36.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 -90.0000 30 #__ type_ start__ end____ width___ exp.time_ 16 omega 41.00 67.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 17 omega 122.00 148.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 18 omega 56.00 82.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 54.00 90.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 120.0000 36 #__ type_ start__ end____ width___ exp.time_ 20 omega 44.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 60.0000 31 #__ type_ start__ end____ width___ exp.time_ 22 omega 134.00 171.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -90.0000 37 #__ type_ start__ end____ width___ exp.time_ 23 omega 145.00 171.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 24 omega 79.00 112.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -90.0000 33 #__ type_ start__ end____ width___ exp.time_ 25 omega 88.00 134.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -180.0000 46 #__ type_ start__ end____ width___ exp.time_ 26 omega 91.00 117.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 27 omega 84.00 142.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -60.0000 58 #__ type_ start__ end____ width___ exp.time_ 28 omega 49.00 75.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 29 omega 37.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -120.0000 35 #__ type_ start__ end____ width___ exp.time_ 30 omega 82.00 108.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 31 omega 37.00 63.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 32 omega 122.00 148.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 33 omega 53.00 79.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 34 omega 38.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 150.0000 33 #__ type_ start__ end____ width___ exp.time_ 35 omega 39.00 75.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -90.0000 36 #__ type_ start__ end____ width___ exp.time_ 36 omega 118.00 165.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 120.0000 47 #__ type_ start__ end____ width___ exp.time_ 37 omega 83.00 109.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 38 omega 43.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 39 omega 79.00 106.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 40 omega 92.00 118.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 41 omega 140.00 169.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -60.0000 29 #__ type_ start__ end____ width___ exp.time_ 42 omega 87.00 122.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -30.0000 35 #__ type_ start__ end____ width___ exp.time_ 43 omega 79.00 105.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 44 omega 75.00 101.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 45 omega 107.00 132.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 46 omega 37.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 30.0000 32 #__ type_ start__ end____ width___ exp.time_ 47 omega 134.00 164.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -120.0000 30 #__ type_ start__ end____ width___ exp.time_ 48 omega 87.00 135.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -60.0000 48 #__ type_ start__ end____ width___ exp.time_ 49 omega 83.00 127.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 150.0000 44 #__ type_ start__ end____ width___ exp.time_ 50 omega 87.00 146.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -120.0000 59 #__ type_ start__ end____ width___ exp.time_ 51 omega 79.00 118.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -60.0000 39 #__ type_ start__ end____ width___ exp.time_ 52 omega 91.00 116.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 53 omega 40.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 54 omega 89.00 117.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 55 omega 45.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 56 omega 85.00 112.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 57 omega 85.00 110.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 58 omega 88.00 115.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 59 omega 89.00 153.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 60.0000 64 #__ type_ start__ end____ width___ exp.time_ 60 omega -25.00 42.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 150.0000 67 #__ type_ start__ end____ width___ exp.time_ 61 omega -21.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -30.0000 90 #__ type_ start__ end____ width___ exp.time_ 62 omega -69.00 21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 0.0000 90 #__ type_ start__ end____ width___ exp.time_ 63 omega -69.00 21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 -120.0000 90 #__ type_ start__ end____ width___ exp.time_ 64 omega -125.00 -25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -180.0000 100 #__ type_ start__ end____ width___ exp.time_ 65 omega -112.00 -18.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 125.0000 60.0000 94 #__ type_ start__ end____ width___ exp.time_ 66 omega -75.00 14.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 57.0000 90.0000 89 #__ type_ start__ end____ width___ exp.time_ 67 omega -125.00 -25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 68 omega -125.00 -25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 69 omega -124.00 -33.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 30.0000 91 #__ type_ start__ end____ width___ exp.time_ 70 omega -125.00 -25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 120.0000 100 #__ type_ start__ end____ width___ exp.time_ 71 omega -3.00 96.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 -125.0000 -90.0000 99 #__ type_ start__ end____ width___ exp.time_ 72 omega 37.00 90.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 30.0000 53 #__ type_ start__ end____ width___ exp.time_ 73 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 -30.0000 99 #__ type_ start__ end____ width___ exp.time_ 74 omega 39.00 83.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -30.0000 44 #__ type_ start__ end____ width___ exp.time_ 75 omega 38.00 147.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -60.0000 109 #__ type_ start__ end____ width___ exp.time_ 76 omega 87.00 177.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 77 omega 37.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 30.0000 34 #__ type_ start__ end____ width___ exp.time_ 78 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 150.0000 99 #__ type_ start__ end____ width___ exp.time_ 79 omega 38.00 147.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 150.0000 109 #__ type_ start__ end____ width___ exp.time_ 80 omega 87.00 177.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 90.0000 90 #__ type_ start__ end____ width___ exp.time_ 81 omega 79.00 158.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 0.0000 79 #__ type_ start__ end____ width___ exp.time_ 82 omega 37.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 0.0000 34 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1550068000 _diffrn_orient_matrix_UB_12 0.0163065000 _diffrn_orient_matrix_UB_13 0.0684848000 _diffrn_orient_matrix_UB_21 0.0099508000 _diffrn_orient_matrix_UB_22 -0.0596473000 _diffrn_orient_matrix_UB_23 -0.1656073000 _diffrn_orient_matrix_UB_31 -0.0186288000 _diffrn_orient_matrix_UB_32 0.1039601000 _diffrn_orient_matrix_UB_33 -0.1057714000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_special_details ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1827 _reflns_number_total 1918 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.419 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.051 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 1918 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0254 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.4136P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.0716 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2. Restrained distances H3A-O3 = O3-H3B 0.958 with sigma of 0.02 H1A-O1 = O1-H1B 0.958 with sigma of 0.02 H2A-O2 0.958 with sigma of 0.02 H2A-O2 = O2-H2B 0.958 with sigma of 0.02 H3A-H3B 1.515 with sigma of 0.04 H1A-H1B 1.515 with sigma of 0.04 H2A-H2B 1.515 with sigma of 0.04 3.a Aromatic/amide H refined with riding coordinates: N5(H5), N6(H6) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C7 C 0.39342(15) 0.67327(12) 0.0957(2) 0.0273(3) Uani 1 1 d . . . C8 C 0.39540(15) 0.85554(12) 0.0992(2) 0.0276(3) Uani 1 1 d . . . C9 C 0.58185(16) 0.76246(11) 0.3105(2) 0.0267(3) Uani 1 1 d . . . N2 N 0.33585(14) 0.76519(10) 0.02546(18) 0.0304(3) Uani 1 1 d . . . N5 N 0.51757(13) 0.85247(10) 0.23832(17) 0.0301(3) Uani 1 1 d . . . H5 H 0.5553 0.9111 0.2819 0.036 Uiso 1 1 calc R . . N6 N 0.51446(13) 0.67407(10) 0.23692(17) 0.0292(3) Uani 1 1 d . . . H6 H 0.5494 0.6147 0.2811 0.035 Uiso 1 1 calc R . . S1 S 0.32083(4) 0.55732(3) 0.01817(5) 0.03594(13) Uani 1 1 d . . . S2 S 0.32341(4) 0.97253(3) 0.02756(5) 0.03534(13) Uani 1 1 d . . . S3 S 0.73059(4) 0.76086(3) 0.47827(6) 0.03338(13) Uani 1 1 d . . . H3A H 1.181(2) 0.774(2) 0.812(3) 0.063(7) Uiso 1 1 d D . . H1A H 1.008(2) 0.362(2) 0.687(4) 0.081(9) Uiso 1 1 d D . . H1B H 1.134(2) 0.364(2) 0.640(4) 0.078(8) Uiso 1 1 d D . . H2A H 0.865(2) 0.613(2) 0.855(5) 0.110(12) Uiso 1 1 d D . . H2B H 0.989(4) 0.551(3) 0.958(4) 0.142(17) Uiso 1 1 d D . . H3B H 1.117(3) 0.819(2) 0.637(3) 0.100(11) Uiso 1 1 d D . . O1 O 1.05455(13) 0.40020(10) 0.62937(18) 0.0400(3) Uani 1 1 d D . . O2 O 0.9397(3) 0.57495(18) 0.8534(4) 0.0929(7) Uani 1 1 d D . . O3 O 1.10150(14) 0.77289(11) 0.71566(19) 0.0432(3) Uani 1 1 d D . . Na1 Na 1.08406(8) 0.58499(6) 0.68175(9) 0.04411(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C7 0.0266(7) 0.0266(7) 0.0285(7) -0.0002(6) 0.0091(6) -0.0008(6) C8 0.0266(7) 0.0273(7) 0.0281(7) 0.0004(6) 0.0082(6) 0.0014(6) C9 0.0259(7) 0.0267(7) 0.0275(7) -0.0004(5) 0.0089(6) 0.0007(5) N2 0.0281(7) 0.0268(7) 0.0312(7) 0.0000(5) 0.0032(6) -0.0004(5) N5 0.0278(6) 0.0225(6) 0.0341(7) -0.0025(5) 0.0028(5) -0.0002(5) N6 0.0269(6) 0.0236(6) 0.0325(7) 0.0013(5) 0.0037(5) 0.0006(5) S1 0.0361(2) 0.0253(2) 0.0373(2) -0.00069(15) 0.00026(17) -0.00546(15) S2 0.0346(2) 0.0253(2) 0.0385(2) 0.00158(15) 0.00221(17) 0.00437(14) S3 0.0282(2) 0.0317(2) 0.0326(2) -0.00199(14) 0.00006(17) 0.00083(14) O1 0.0374(6) 0.0363(6) 0.0440(7) 0.0036(5) 0.0109(5) 0.0032(5) O2 0.1078(16) 0.0844(14) 0.1194(18) 0.0448(13) 0.0815(15) 0.0468(12) O3 0.0408(7) 0.0429(7) 0.0409(7) -0.0031(6) 0.0072(6) 0.0003(5) Na1 0.0509(4) 0.0391(4) 0.0375(4) -0.0042(3) 0.0085(3) -0.0035(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 C7 N2 1.347(2) . ? C7 N6 1.3744(19) . ? C7 S1 1.6785(15) . ? C8 N2 1.344(2) . ? C8 N5 1.375(2) . ? C8 S2 1.6791(15) . ? C9 N5 1.3533(19) . ? C9 N6 1.3506(19) . ? C9 S3 1.6669(16) . ? S1 Na1 2.9739(8) 1_454 ? S2 Na1 3.2102(9) 4_475 ? O1 Na1 2.3949(14) 3_766 ? O1 Na1 2.3914(14) . ? O2 Na1 2.3415(19) . ? O3 Na1 2.4082(15) . ? Na1 S1 2.9739(8) 1_656 ? Na1 S2 3.2101(9) 4_676 ? Na1 O1 2.3949(15) 3_766 ? Na1 Na1 3.5450(14) 3_766 ? 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 C7 N6 119.20(13) . . ? N2 C7 S1 122.06(12) . . ? N6 C7 S1 118.74(11) . . ? N2 C8 N5 119.39(13) . . ? N2 C8 S2 121.66(12) . . ? N5 C8 S2 118.95(11) . . ? N5 C9 S3 122.79(11) . . ? N6 C9 N5 114.37(14) . . ? N6 C9 S3 122.83(11) . . ? C8 N2 C7 119.28(14) . . ? C9 N5 C8 123.73(13) . . ? C9 N6 C7 123.92(13) . . ? C7 S1 Na1 110.99(6) . 1_454 ? C8 S2 Na1 89.37(5) . 4_475 ? Na1 O1 Na1 95.57(5) . 3_766 ? S1 Na1 S2 77.74(2) 1_656 4_676 ? S1 Na1 Na1 133.11(4) 1_656 3_766 ? S2 Na1 Na1 78.13(3) 4_676 3_766 ? O1 Na1 S1 162.67(5) 3_766 1_656 ? O1 Na1 S1 93.27(4) . 1_656 ? O1 Na1 S2 77.42(4) . 4_676 ? O1 Na1 S2 85.01(4) 3_766 4_676 ? O1 Na1 O1 84.43(5) . 3_766 ? O1 Na1 O3 176.15(6) . . ? O1 Na1 O3 91.84(5) 3_766 . ? O1 Na1 Na1 42.18(3) 3_766 3_766 ? O1 Na1 Na1 42.25(3) . 3_766 ? O2 Na1 S1 89.19(7) . 1_656 ? O2 Na1 S2 160.08(6) . 4_676 ? O2 Na1 O1 107.88(8) . 3_766 ? O2 Na1 O1 88.55(7) . . ? O2 Na1 O3 91.72(7) . . ? O2 Na1 Na1 100.97(8) . 3_766 ? O3 Na1 S1 90.57(4) . 1_656 ? O3 Na1 S2 103.24(4) . 4_676 ? O3 Na1 Na1 134.01(5) . 3_766 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 6 1 0 0.0332 5.9988 1.0046 0.0020 0.9464 -0.0006 -0.0075 -6 -1 0 0.0172 -5.9988 -1.0046 -0.0020 -0.9464 0.0006 0.0075 -1 8 0 0.0537 -1.0027 7.9987 -0.0007 -0.0250 -0.4870 0.8503 1 -8 0 0.0397 1.0027 -7.9987 0.0007 0.0250 0.4870 -0.8503 -3 -2 5 0.1136 -2.9997 -1.9987 4.9998 -0.1552 -0.7386 -0.6807 3 2 -5 0.1092 2.9997 1.9987 -4.9998 0.1552 0.7386 0.6807 _database_code_depnum_ccdc_archive 'CCDC 944677' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_KTTC _audit_creation_date 2013-06-13 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 K2 N6 O2 S6' _chemical_formula_sum 'C6 H8 K2 N6 O2 S6' _chemical_formula_weight 466.74 _chemical_melting_point ? _chemical_oxdiff_formula 'S3 N3 C3 H4 O1 K1' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.3438(4) _cell_length_b 10.3247(4) _cell_length_c 11.6813(5) _cell_angle_alpha 76.285(3) _cell_angle_beta 80.914(4) _cell_angle_gamma 87.551(4) _cell_volume 849.64(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5620 _cell_measurement_temperature 298.6(2) _cell_measurement_theta_max 71.1960 _cell_measurement_theta_min 3.9250 _exptl_absorpt_coefficient_mu 11.961 _exptl_absorpt_correction_T_max 0.498 _exptl_absorpt_correction_T_min 0.098 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rhombohedral _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.5209 _exptl_crystal_size_mid 0.1775 _exptl_crystal_size_min 0.0688 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10459 _diffrn_reflns_theta_full 71.9829 _diffrn_reflns_theta_max 71.22 _diffrn_reflns_theta_min 3.94 _diffrn_ambient_temperature 298.6(2) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9755 _diffrn_measured_fraction_theta_max 0.9918 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -22.00 33.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 -120.0000 55 #__ type_ start__ end____ width___ exp.time_ 2 omega 41.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 120.0000 28 #__ type_ start__ end____ width___ exp.time_ 3 omega -2.00 25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -37.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 4 omega -50.00 -18.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -37.0000 -30.0000 32 #__ type_ start__ end____ width___ exp.time_ 5 omega -70.00 -4.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 57.0000 -60.0000 66 #__ type_ start__ end____ width___ exp.time_ 6 omega -90.00 -29.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 138.0000 -67.0000 61 #__ type_ start__ end____ width___ exp.time_ 7 omega -126.00 -32.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -37.0000 120.0000 94 #__ type_ start__ end____ width___ exp.time_ 8 omega 95.00 124.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 9 omega 87.00 125.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 90.0000 38 #__ type_ start__ end____ width___ exp.time_ 10 omega 83.00 122.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -180.0000 39 #__ type_ start__ end____ width___ exp.time_ 11 omega -72.00 -20.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 25.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 12 omega -17.00 9.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 25.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 13 omega -139.00 -63.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 0.0000 76 #__ type_ start__ end____ width___ exp.time_ 14 omega 47.00 73.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 15 omega 104.00 139.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 -120.0000 35 #__ type_ start__ end____ width___ exp.time_ 16 omega 37.00 62.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 17 omega 40.00 65.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 18 omega 95.00 137.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -150.0000 42 #__ type_ start__ end____ width___ exp.time_ 19 omega 43.00 71.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 120.0000 28 #__ type_ start__ end____ width___ exp.time_ 20 omega 94.00 130.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 36 #__ type_ start__ end____ width___ exp.time_ 21 omega 93.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -60.0000 85 #__ type_ start__ end____ width___ exp.time_ 22 omega 37.00 62.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 23 omega 62.00 88.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -15.0000 114.6601 26 #__ type_ start__ end____ width___ exp.time_ 24 omega 67.00 142.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 120.0000 75 #__ type_ start__ end____ width___ exp.time_ 25 omega 48.00 117.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 120.0000 69 #__ type_ start__ end____ width___ exp.time_ 26 omega 48.00 94.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 -120.0000 46 #__ type_ start__ end____ width___ exp.time_ 27 omega 67.00 147.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -60.0000 80 #__ type_ start__ end____ width___ exp.time_ 28 omega 90.00 132.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 120.0000 42 #__ type_ start__ end____ width___ exp.time_ 29 omega 151.00 177.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 30 omega 37.00 63.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 31 omega 139.00 174.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 35 #__ type_ start__ end____ width___ exp.time_ 32 omega 132.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -120.0000 46 #__ type_ start__ end____ width___ exp.time_ 33 omega 104.00 129.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 34 omega 71.00 122.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 30.0000 51 #__ type_ start__ end____ width___ exp.time_ 35 omega 37.00 62.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 36 omega 80.00 121.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 -30.0000 41 #__ type_ start__ end____ width___ exp.time_ 37 omega 42.00 71.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 38 omega 47.00 83.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -60.0000 36 #__ type_ start__ end____ width___ exp.time_ 39 omega 75.00 117.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 90.0000 42 #__ type_ start__ end____ width___ exp.time_ 40 omega 88.00 120.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 41 omega 42.00 71.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 42 omega 129.00 163.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -15.0000 114.6601 34 #__ type_ start__ end____ width___ exp.time_ 43 omega 99.00 133.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 120.0000 34 #__ type_ start__ end____ width___ exp.time_ 44 omega 64.00 90.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 45 omega 87.00 113.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 -175.2424 26 #__ type_ start__ end____ width___ exp.time_ 46 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -120.0000 45 #__ type_ start__ end____ width___ exp.time_ 47 omega -69.00 21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -57.0000 150.0000 90 #__ type_ start__ end____ width___ exp.time_ 48 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -150.0000 45 #__ type_ start__ end____ width___ exp.time_ 49 omega -125.00 -25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 50 omega -125.00 -25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 51 omega -125.00 -25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 52 omega -125.00 -25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 30.0000 100 #__ type_ start__ end____ width___ exp.time_ 53 omega -124.00 -33.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 -90.0000 91 #__ type_ start__ end____ width___ exp.time_ 54 omega 73.00 126.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -90.0000 53 #__ type_ start__ end____ width___ exp.time_ 55 omega -134.00 -75.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 150.0000 59 #__ type_ start__ end____ width___ exp.time_ 56 omega 84.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 30.0000 94 #__ type_ start__ end____ width___ exp.time_ 57 omega 79.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -30.0000 99 #__ type_ start__ end____ width___ exp.time_ 58 omega 88.00 123.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 90.0000 35 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0059621000 _diffrn_orient_matrix_UB_12 0.1526770000 _diffrn_orient_matrix_UB_13 -0.0189048000 _diffrn_orient_matrix_UB_21 0.0267706000 _diffrn_orient_matrix_UB_22 0.0151647000 _diffrn_orient_matrix_UB_23 -0.1360086000 _diffrn_orient_matrix_UB_31 -0.2106692000 _diffrn_orient_matrix_UB_32 0.0071019000 _diffrn_orient_matrix_UB_33 0.0032729000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2968 _reflns_number_total 3266 _reflns_odcompleteness_completeness 97.55 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.361 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 3266 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0372 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0613P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1028 _refine_ls_wR_factor_ref 0.1066 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2. Restrained distances H2B-O2 = O2-H2A 0.958 with sigma of 0.02 H1B-O1 = O1-H1A 0.958 with sigma of 0.02 H2B-H2A 1.515 with sigma of 0.04 H1B-H1A 1.515 with sigma of 0.04 3.a Aromatic/amide H refined with riding coordinates: N3(H3), N4(H4), N10(H10), N14(H14) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap 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 H1A H -0.005(6) -0.328(2) 0.317(4) 0.111(15) Uiso 1 1 d D . . H1B H -0.042(5) -0.464(3) 0.292(3) 0.085(12) Uiso 1 1 d D . . H2A H 0.424(7) -0.675(3) 0.192(5) 0.15(2) Uiso 1 1 d D . . H2B H 0.582(3) -0.583(5) 0.189(5) 0.16(3) Uiso 1 1 d D . . C3 C -0.2752(3) 0.0249(2) 0.02084(18) 0.0343(4) Uani 1 1 d . . . C5 C -0.0967(3) 0.02513(19) -0.16048(17) 0.0340(4) Uani 1 1 d . . . C8 C -0.1660(3) -0.1849(2) -0.02003(18) 0.0365(4) Uani 1 1 d . . . C16 C 0.4247(3) -0.2329(2) 0.39817(18) 0.0348(4) Uani 1 1 d . . . C18 C 0.2448(3) -0.23534(19) 0.57947(18) 0.0354(4) Uani 1 1 d . . . C19 C 0.3116(3) -0.02475(19) 0.43984(18) 0.0349(4) Uani 1 1 d . . . N1 N -0.1916(3) 0.09293(16) -0.08616(15) 0.0366(4) Uani 1 1 d . . . N3 N -0.2552(3) -0.11202(16) 0.05271(14) 0.0365(4) Uani 1 1 d . . . H3 H -0.3027 -0.1531 0.1235 0.044 Uiso 1 1 calc R . . N4 N -0.0890(3) -0.11250(17) -0.12754(15) 0.0377(4) Uani 1 1 d . . . H4 H -0.0320 -0.1543 -0.1783 0.045 Uiso 1 1 calc R . . N10 N 0.2290(3) -0.09928(17) 0.54602(16) 0.0377(4) Uani 1 1 d . . . H10 H 0.1634 -0.0589 0.5948 0.045 Uiso 1 1 calc R . . N13 N 0.3416(3) -0.30274(17) 0.50441(15) 0.0390(4) Uani 1 1 d . . . N14 N 0.4124(3) -0.09611(16) 0.36902(15) 0.0364(4) Uani 1 1 d . . . H14 H 0.4721 -0.0537 0.3022 0.044 Uiso 1 1 calc R . . O1 O 0.0249(3) -0.4184(2) 0.3290(2) 0.0701(6) Uani 1 1 d D . . O2 O 0.4544(4) -0.5896(2) 0.1940(3) 0.0866(8) Uani 1 1 d D . . S1 S 0.28767(9) 0.13937(5) 0.39848(5) 0.04552(17) Uani 1 1 d . . . S2 S -0.15064(10) -0.35131(5) 0.02006(5) 0.05097(18) Uani 1 1 d . . . S3 S 0.54659(8) -0.31142(5) 0.29911(5) 0.04145(16) Uani 1 1 d . . . S4 S -0.39971(8) 0.10147(5) 0.11941(5) 0.04124(16) Uani 1 1 d . . . S5 S 0.02003(8) 0.10104(5) -0.29410(4) 0.04015(16) Uani 1 1 d . . . S6 S 0.13869(9) -0.31374(5) 0.71580(5) 0.04555(17) Uani 1 1 d . . . K1 K 0.27654(8) -0.56072(5) 0.45153(5) 0.05403(17) Uani 1 1 d . . . K2 K 0.28763(11) -0.36797(6) 0.08889(6) 0.0655(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C3 0.0367(11) 0.0325(9) 0.0343(9) -0.0097(7) -0.0053(8) 0.0023(7) C5 0.0375(11) 0.0325(9) 0.0322(9) -0.0086(7) -0.0046(8) 0.0008(7) C8 0.0418(11) 0.0334(9) 0.0342(10) -0.0093(8) -0.0038(8) 0.0010(8) C16 0.0383(11) 0.0303(9) 0.0353(9) -0.0085(7) -0.0033(8) 0.0022(7) C18 0.0417(11) 0.0301(9) 0.0328(9) -0.0068(7) -0.0024(8) 0.0011(7) C19 0.0380(11) 0.0311(9) 0.0349(9) -0.0081(7) -0.0029(8) 0.0008(7) N1 0.0426(10) 0.0308(8) 0.0355(8) -0.0081(7) -0.0033(7) 0.0022(7) N3 0.0443(10) 0.0317(8) 0.0306(8) -0.0053(6) -0.0009(7) 0.0022(7) N4 0.0454(10) 0.0323(8) 0.0337(8) -0.0097(7) 0.0018(7) 0.0020(7) N10 0.0449(10) 0.0306(8) 0.0357(8) -0.0091(7) 0.0010(7) 0.0029(7) N13 0.0487(11) 0.0315(8) 0.0345(9) -0.0078(7) 0.0000(8) 0.0029(7) N14 0.0447(10) 0.0292(8) 0.0318(8) -0.0058(6) 0.0026(7) 0.0000(7) O1 0.0741(15) 0.0448(9) 0.0992(17) -0.0190(10) -0.0348(13) 0.0064(9) O2 0.0930(19) 0.0406(10) 0.130(2) -0.0108(12) -0.0429(17) 0.0047(10) S1 0.0611(4) 0.0280(3) 0.0442(3) -0.0075(2) -0.0005(3) 0.0024(2) S2 0.0721(4) 0.0297(3) 0.0461(3) -0.0074(2) 0.0030(3) 0.0020(2) S3 0.0507(3) 0.0343(3) 0.0363(3) -0.0104(2) 0.0045(2) 0.0041(2) S4 0.0484(3) 0.0361(3) 0.0366(3) -0.0109(2) 0.0031(2) 0.0057(2) S5 0.0497(3) 0.0346(3) 0.0329(3) -0.0069(2) 0.0020(2) -0.0007(2) S6 0.0598(4) 0.0345(3) 0.0359(3) -0.0057(2) 0.0078(2) 0.0009(2) K1 0.0606(4) 0.0405(3) 0.0604(3) -0.0100(2) -0.0119(3) 0.0045(2) K2 0.0848(5) 0.0443(3) 0.0626(4) -0.0045(2) -0.0125(3) 0.0118(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 C3 N1 1.346(3) . ? C3 N3 1.381(3) . ? C3 S4 1.681(2) . ? C3 K2 3.472(2) 2 ? C5 N1 1.336(3) . ? C5 N4 1.382(2) . ? C5 S5 1.685(2) . ? C8 N3 1.342(3) . ? C8 N4 1.350(3) . ? C8 S2 1.674(2) . ? C16 N13 1.344(3) . ? C16 N14 1.374(2) . ? C16 S3 1.689(2) . ? C16 K1 3.388(2) 2_646 ? C16 K1 3.483(2) . ? C18 N10 1.371(3) . ? C18 N13 1.345(3) . ? C18 S6 1.688(2) . ? C19 N10 1.359(3) . ? C19 N14 1.351(3) . ? C19 S1 1.658(2) . ? N1 K2 2.8906(17) 2 ? N13 K1 2.9472(18) . ? N13 K1 3.145(2) 2_646 ? O1 K1 2.689(2) . ? O1 K1 3.083(3) 2_546 ? O1 K2 3.089(3) . ? O2 K1 3.162(4) . ? O2 K2 2.674(2) . ? S1 K1 3.2942(7) 1_565 ? S2 K2 3.4263(11) . ? S2 K2 3.6653(9) 2_545 ? S3 K1 3.2979(8) . ? S3 K1 3.3375(8) 2_646 ? S3 K2 3.4983(10) . ? S4 K2 3.2489(8) 2 ? K1 C16 3.388(2) 2_646 ? K1 N13 3.145(2) 2_646 ? K1 O1 3.083(3) 2_546 ? K1 S1 3.2942(7) 1_545 ? K1 S3 3.3375(8) 2_646 ? K1 K1 3.9780(12) 2_646 ? K1 K2 4.2213(8) . ? K2 C3 3.472(2) 2 ? K2 N1 2.8906(17) 2 ? K2 S2 3.6653(9) 2_545 ? K2 S4 3.2488(8) 2 ? K2 K2 4.6246(13) 2_645 ? 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 C3 N3 119.40(18) . . ? N1 C3 S4 122.11(15) . . ? N1 C3 K2 53.86(10) . 2 ? N3 C3 S4 118.47(15) . . ? N3 C3 K2 173.21(14) . 2 ? S4 C3 K2 68.25(7) . 2 ? N1 C5 N4 119.85(18) . . ? N1 C5 S5 122.51(15) . . ? N4 C5 S5 117.63(15) . . ? N3 C8 N4 114.31(18) . . ? N3 C8 S2 122.66(16) . . ? N4 C8 S2 123.03(16) . . ? N13 C16 N14 120.28(18) . . ? N13 C16 S3 120.64(15) . . ? N13 C16 K1 68.10(12) . 2_646 ? N13 C16 K1 55.89(10) . . ? N14 C16 S3 119.08(15) . . ? N14 C16 K1 130.88(14) . 2_646 ? N14 C16 K1 157.27(15) . . ? S3 C16 K1 69.57(7) . . ? S3 C16 K1 73.79(7) . 2_646 ? K1 C16 K1 70.74(4) 2_646 . ? N10 C18 S6 118.03(16) . . ? N13 C18 N10 120.16(18) . . ? N13 C18 S6 121.80(15) . . ? N10 C19 S1 123.28(16) . . ? N14 C19 N10 114.27(17) . . ? N14 C19 S1 122.44(15) . . ? C3 N1 K2 104.05(12) . 2 ? C5 N1 C3 118.76(17) . . ? C5 N1 K2 137.16(13) . 2 ? C8 N3 C3 123.97(17) . . ? C8 N4 C5 123.53(18) . . ? C19 N10 C18 123.52(18) . . ? C16 N13 C18 118.21(17) . . ? C16 N13 K1 101.93(12) . . ? C16 N13 K1 88.54(13) . 2_646 ? C18 N13 K1 122.54(14) . 2_646 ? C18 N13 K1 131.78(14) . . ? K1 N13 K1 81.46(5) . 2_646 ? C19 N14 C16 123.46(17) . . ? K1 O1 K1 94.84(8) . 2_546 ? K1 O1 K2 171.47(8) 2_546 . ? K1 O1 K2 93.60(7) . . ? K2 O2 K1 92.28(9) . . ? C19 S1 K1 151.86(8) . 1_565 ? C8 S2 K2 97.06(8) . . ? C8 S2 K2 136.21(8) . 2_545 ? K2 S2 K2 115.61(2) . 2_545 ? C16 S3 K1 81.74(7) . . ? C16 S3 K1 77.13(7) . 2_646 ? C16 S3 K2 112.78(8) . . ? K1 S3 K1 73.67(2) . 2_646 ? K1 S3 K2 146.99(2) 2_646 . ? K1 S3 K2 76.74(2) . . ? C3 S4 K2 83.04(7) . 2 ? C16 K1 C16 109.26(4) 2_646 . ? C16 K1 K1 53.52(4) . 2_646 ? C16 K1 K1 55.74(4) 2_646 2_646 ? C16 K1 K2 69.54(4) . . ? C16 K1 K2 133.23(4) 2_646 . ? N13 K1 C16 102.69(5) . 2_646 ? N13 K1 C16 23.36(5) 2_646 2_646 ? N13 K1 C16 96.65(5) 2_646 . ? N13 K1 C16 22.18(5) . . ? N13 K1 N13 98.54(5) . 2_646 ? N13 K1 O1 82.03(5) . 2_546 ? N13 K1 O2 77.43(6) 2_646 . ? N13 K1 O2 114.94(6) . . ? N13 K1 S1 168.96(5) . 1_545 ? N13 K1 S1 70.48(4) 2_646 1_545 ? N13 K1 S3 47.97(3) 2_646 2_646 ? N13 K1 S3 49.65(4) . . ? N13 K1 S3 81.75(4) 2_646 . ? N13 K1 S3 84.07(4) . 2_646 ? N13 K1 K1 51.43(4) . 2_646 ? N13 K1 K1 47.11(4) 2_646 2_646 ? N13 K1 K2 89.64(4) . . ? N13 K1 K2 110.89(4) 2_646 . ? O1 K1 C16 102.47(5) 2_546 . ? O1 K1 C16 76.25(6) . . ? O1 K1 C16 174.38(6) . 2_646 ? O1 K1 C16 94.53(5) 2_546 2_646 ? O1 K1 N13 117.01(5) 2_546 2_646 ? O1 K1 N13 82.83(6) . . ? O1 K1 N13 157.81(7) . 2_646 ? O1 K1 O1 85.16(8) . 2_546 ? O1 K1 O2 81.92(7) . . ? O1 K1 O2 156.97(7) 2_546 . ? O1 K1 S1 106.84(5) . 1_545 ? O1 K1 S1 103.73(4) 2_546 1_545 ? O1 K1 S3 153.13(6) . 2_646 ? O1 K1 S3 69.84(4) 2_546 2_646 ? O1 K1 S3 131.15(4) 2_546 . ? O1 K1 S3 82.46(5) . . ? O1 K1 K1 129.76(5) . 2_646 ? O1 K1 K1 104.85(5) 2_546 2_646 ? O1 K1 K2 132.06(4) 2_546 . ? O1 K1 K2 46.92(6) . . ? O2 K1 C16 96.48(6) . 2_646 ? O2 K1 C16 92.89(6) . . ? O2 K1 S1 62.51(4) . 1_545 ? O2 K1 S3 124.93(5) . 2_646 ? O2 K1 S3 65.78(5) . . ? O2 K1 K1 98.07(6) . 2_646 ? O2 K1 K2 39.26(4) . . ? S1 K1 C16 67.76(4) 1_545 2_646 ? S1 K1 C16 153.78(4) 1_545 . ? S1 K1 S3 125.10(2) 1_545 . ? S1 K1 S3 89.071(19) 1_545 2_646 ? S1 K1 K1 117.58(3) 1_545 2_646 ? S1 K1 K2 93.212(18) 1_545 . ? S3 K1 C16 101.85(4) . 2_646 ? S3 K1 C16 28.69(4) . . ? S3 K1 C16 29.08(4) 2_646 2_646 ? S3 K1 C16 99.10(4) 2_646 . ? S3 K1 S3 106.33(2) . 2_646 ? S3 K1 K1 53.623(17) . 2_646 ? S3 K1 K1 52.709(16) 2_646 2_646 ? S3 K1 K2 53.766(17) . . ? S3 K1 K2 156.15(2) 2_646 . ? K1 K1 K2 106.10(2) 2_646 . ? C3 K2 S2 132.83(4) 2 2_545 ? C3 K2 S3 87.65(4) 2 . ? C3 K2 K1 124.77(4) 2 . ? C3 K2 K2 121.18(4) 2 2_645 ? N1 K2 C3 22.08(5) 2 2 ? N1 K2 O1 82.51(5) 2 . ? N1 K2 S2 140.74(5) 2 2_545 ? N1 K2 S2 78.64(4) 2 . ? N1 K2 S3 79.65(4) 2 . ? N1 K2 S4 50.80(4) 2 2 ? N1 K2 K1 105.61(4) 2 . ? N1 K2 K2 142.30(5) 2 2_645 ? O1 K2 C3 104.52(5) . 2 ? O1 K2 S2 98.56(4) . 2_545 ? O1 K2 S2 73.78(5) . . ? O1 K2 S3 73.87(4) . . ? O1 K2 S4 133.07(4) . 2 ? O1 K2 K1 39.47(4) . . ? O1 K2 K2 133.36(4) . 2_645 ? O2 K2 C3 151.22(8) . 2 ? O2 K2 N1 147.02(8) . 2 ? O2 K2 O1 83.55(9) . . ? O2 K2 S2 71.00(6) . 2_545 ? O2 K2 S2 125.29(7) . . ? O2 K2 S3 67.80(6) . . ? O2 K2 S4 137.48(8) . 2 ? O2 K2 K1 48.46(8) . . ? O2 K2 K2 52.08(8) . 2_645 ? S2 K2 C3 83.34(4) . 2 ? S2 K2 S2 64.39(2) . 2_545 ? S2 K2 S3 142.92(3) . . ? S2 K2 K1 109.40(2) . . ? S2 K2 K1 98.971(18) 2_545 . ? S2 K2 K2 57.571(18) 2_545 2_645 ? S2 K2 K2 117.62(3) . 2_645 ? S3 K2 S2 138.66(2) . 2_545 ? S3 K2 K1 49.499(14) . . ? S3 K2 K2 97.79(3) . 2_645 ? S4 K2 C3 28.72(3) 2 2 ? S4 K2 S2 114.11(2) 2 2_545 ? S4 K2 S2 90.43(2) 2 . ? S4 K2 S3 98.63(2) 2 . ? S4 K2 K1 146.50(2) 2 . ? S4 K2 K2 93.28(2) 2 2_645 ? K1 K2 K2 100.407(19) . 2_645 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 7 1 0.0524 -0.0013 7.0048 1.0092 1.0504 -0.0311 0.0533 0 -7 -1 0.0164 0.0013 -7.0048 -1.0092 -1.0504 0.0311 -0.0533 0 1 -7 0.0846 0.0019 1.0029 -6.9947 0.2854 0.9666 -0.0162 0 -1 7 0.0696 -0.0019 -1.0029 6.9947 -0.2854 -0.9666 0.0162 -4 0 -4 0.2026 -3.9977 0.0028 -4.0007 0.0522 0.4371 0.8291 4 0 4 0.1906 3.9977 -0.0028 4.0007 -0.0522 -0.4371 -0.8291 _database_code_depnum_ccdc_archive 'CCDC 944678' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RbTTC1 _audit_creation_date 2013-06-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 N6 O2 Rb2 S6' _chemical_formula_sum 'C6 H8 N6 O2 Rb2 S6' _chemical_formula_weight 559.48 _chemical_melting_point ? _chemical_oxdiff_formula 'S3 N3 C3 H4 O1 Rb1' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.3545(3) _cell_length_b 10.5336(4) _cell_length_c 11.7338(5) _cell_angle_alpha 76.921(4) _cell_angle_beta 80.641(4) _cell_angle_gamma 88.730(4) _cell_volume 873.54(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7334 _cell_measurement_temperature 298.6(8) _cell_measurement_theta_max 71.0580 _cell_measurement_theta_min 4.3040 _exptl_absorpt_coefficient_mu 14.106 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.127 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rhombohedral _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.1217 _exptl_crystal_size_mid 0.1042 _exptl_crystal_size_min 0.0739 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 15054 _diffrn_reflns_theta_full 70.9317 _diffrn_reflns_theta_max 71.21 _diffrn_reflns_theta_min 3.92 _diffrn_ambient_temperature 298.6(8) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9938 _diffrn_measured_fraction_theta_max 0.9900 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 47.00 74.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 90.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega 32.00 57.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 3 omega 38.00 65.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 4 omega 40.00 73.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -150.0000 33 #__ type_ start__ end____ width___ exp.time_ 5 omega -4.00 24.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 6 omega -112.00 -21.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 125.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 7 omega 6.00 127.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 0.0000 -120.0000 121 #__ type_ start__ end____ width___ exp.time_ 8 omega 48.00 124.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 -120.0000 76 #__ type_ start__ end____ width___ exp.time_ 9 omega -12.00 34.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 -57.0000 90.0000 46 #__ type_ start__ end____ width___ exp.time_ 10 omega -4.00 73.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 -57.0000 -90.0000 77 #__ type_ start__ end____ width___ exp.time_ 11 omega -140.00 -63.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 60.0000 77 #__ type_ start__ end____ width___ exp.time_ 12 omega 42.00 75.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 -120.0000 33 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 30.0000 33 #__ type_ start__ end____ width___ exp.time_ 14 omega 90.00 122.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 -120.0000 32 #__ type_ start__ end____ width___ exp.time_ 15 omega 38.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -60.0000 34 #__ type_ start__ end____ width___ exp.time_ 16 omega 40.00 68.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 17 omega 150.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 18 omega 40.00 66.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 78.00 105.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 20 omega 38.00 66.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 63.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 22 omega 84.00 141.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -150.0000 57 #__ type_ start__ end____ width___ exp.time_ 23 omega 97.00 154.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 120.0000 57 #__ type_ start__ end____ width___ exp.time_ 24 omega 37.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -180.0000 32 #__ type_ start__ end____ width___ exp.time_ 25 omega 120.00 147.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 0.0000 27 #__ type_ start__ end____ width___ exp.time_ 26 omega 39.00 144.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 0.0000 105 #__ type_ start__ end____ width___ exp.time_ 27 omega 89.00 116.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 28 omega 51.00 114.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 63 #__ type_ start__ end____ width___ exp.time_ 29 omega 41.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -30.0000 30 #__ type_ start__ end____ width___ exp.time_ 30 omega 40.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -180.0000 31 #__ type_ start__ end____ width___ exp.time_ 31 omega 42.00 67.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 32 omega 147.00 177.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 0.0000 30 #__ type_ start__ end____ width___ exp.time_ 33 omega 84.00 123.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 0.0000 39 #__ type_ start__ end____ width___ exp.time_ 34 omega 47.00 78.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 90.0000 31 #__ type_ start__ end____ width___ exp.time_ 35 omega 61.00 111.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -90.0000 50 #__ type_ start__ end____ width___ exp.time_ 36 omega 51.00 141.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 37 omega 47.00 74.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 38 omega 90.00 177.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -30.0000 87 #__ type_ start__ end____ width___ exp.time_ 39 omega 46.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 40 omega 68.00 132.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 90.0000 64 #__ type_ start__ end____ width___ exp.time_ 41 omega 121.00 171.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 60.0000 50 #__ type_ start__ end____ width___ exp.time_ 42 omega 106.00 133.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 43 omega 92.00 129.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 49.7917 37 #__ type_ start__ end____ width___ exp.time_ 44 omega 90.00 117.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 45 omega 57.00 94.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -92.0000 -139.6621 37 #__ type_ start__ end____ width___ exp.time_ 46 omega -70.00 30.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 47 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 0.0000 45 #__ type_ start__ end____ width___ exp.time_ 48 omega -30.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 49 omega -125.00 -25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 150.0000 100 #__ type_ start__ end____ width___ exp.time_ 50 omega -125.00 -25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 51 omega -125.00 -25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 52 omega -124.00 -33.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 60.0000 91 #__ type_ start__ end____ width___ exp.time_ 53 omega 73.00 126.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 54 omega 73.00 126.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 60.0000 53 #__ type_ start__ end____ width___ exp.time_ 55 omega 33.00 124.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 -30.0000 91 #__ type_ start__ end____ width___ exp.time_ 56 omega 73.00 126.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -60.0000 53 #__ type_ start__ end____ width___ exp.time_ 57 omega 25.00 125.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 58 omega -134.00 -44.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 59 omega -134.00 -34.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 60 omega 84.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 90.0000 94 #__ type_ start__ end____ width___ exp.time_ 61 omega 37.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -90.0000 35 #__ type_ start__ end____ width___ exp.time_ 62 omega 83.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 35.0000 -73.0000 95 #__ type_ start__ end____ width___ exp.time_ 63 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 120.0000 99 #__ type_ start__ end____ width___ exp.time_ 64 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 30.0000 99 #__ type_ start__ end____ width___ exp.time_ 65 omega 37.00 90.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 90.0000 53 #__ type_ start__ end____ width___ exp.time_ 66 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -60.0000 99 #__ type_ start__ end____ width___ exp.time_ 67 omega 79.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 150.0000 99 #__ type_ start__ end____ width___ exp.time_ 68 omega 79.00 129.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 0.0000 50 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0856111000 _diffrn_orient_matrix_UB_12 -0.1299126000 _diffrn_orient_matrix_UB_13 0.0543643000 _diffrn_orient_matrix_UB_21 0.1576957000 _diffrn_orient_matrix_UB_22 0.0752793000 _diffrn_orient_matrix_UB_23 0.0285417000 _diffrn_orient_matrix_UB_31 -0.1135056000 _diffrn_orient_matrix_UB_32 0.0023239000 _diffrn_orient_matrix_UB_33 0.1220109000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2997 _reflns_number_total 3358 _reflns_odcompleteness_completeness 99.38 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.794 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 3358 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0325 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.2841P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.0928 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2. Restrained distances H2B-O2 = O2-H2A 0.957 with sigma of 0.02 H3A-O3 0.958 with sigma of 0.02 O3-H3B 0.958 with sigma of 0.02 H3A-O3 = O3-H3B 0.958 with sigma of 0.02 H2B-H2A 1.513 with sigma of 0.04 H3A-H3B 1.515 with sigma of 0.04 3.a Aromatic/amide H refined with riding coordinates: N3(H3), N4(H4), N5(H5), N10(H10) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H2A H 0.564(6) 0.446(4) 0.213(5) 0.10(2) Uiso 1 1 d D . . H2B H 0.499(8) 0.315(2) 0.196(5) 0.11(2) Uiso 1 1 d D . . H3A H 0.075(8) 0.685(3) 0.305(7) 0.14(3) Uiso 1 1 d D . . H3B H -0.090(4) 0.614(5) 0.283(5) 0.090(18) Uiso 1 1 d D . . C4 C 0.3291(4) -0.1852(3) 0.4794(3) 0.0362(6) Uani 1 1 d . . . C6 C 0.4036(4) 0.0203(3) 0.3415(3) 0.0356(6) Uani 1 1 d . . . C7 C 0.2260(4) 0.0194(3) 0.5228(3) 0.0349(6) Uani 1 1 d . . . C8 C 0.0807(4) 0.2344(3) 0.1017(3) 0.0361(6) Uani 1 1 d . . . C9 C 0.1884(4) 0.0309(3) 0.0594(3) 0.0365(6) Uani 1 1 d . . . C12 C 0.2644(4) 0.2365(3) -0.0782(3) 0.0372(6) Uani 1 1 d . . . N1 N 0.1670(4) 0.3017(2) -0.0035(2) 0.0399(6) Uani 1 1 d . . . N2 N 0.3105(4) 0.0861(2) 0.4171(2) 0.0366(5) Uani 1 1 d . . . N3 N 0.2417(3) -0.1148(2) 0.5537(2) 0.0366(5) Uani 1 1 d . . . H3 H 0.1931 -0.1552 0.6239 0.044 Uiso 1 1 calc R . . N4 N 0.2753(4) 0.1029(2) -0.0447(2) 0.0385(5) Uani 1 1 d . . . H4 H 0.3413 0.0630 -0.0929 0.046 Uiso 1 1 calc R . . N5 N 0.4072(4) -0.1148(2) 0.3734(2) 0.0390(5) Uani 1 1 d . . . H5 H 0.4626 -0.1556 0.3223 0.047 Uiso 1 1 calc R . . N10 N 0.0887(4) 0.1012(2) 0.1303(2) 0.0378(5) Uani 1 1 d . . . H10 H 0.0273 0.0601 0.1966 0.045 Uiso 1 1 calc R . . O2 O 0.4800(4) 0.4040(2) 0.1824(3) 0.0601(7) Uani 1 1 d D . . O3 O 0.0259(5) 0.6019(3) 0.3078(3) 0.0693(9) Uani 1 1 d D . . S1 S 0.33871(13) -0.34822(7) 0.51878(8) 0.0487(2) Uani 1 1 d . . . S2 S -0.04312(11) 0.31067(7) 0.20032(7) 0.04153(18) Uani 1 1 d . . . S3 S 0.20487(12) -0.12986(7) 0.09902(8) 0.0467(2) Uani 1 1 d . . . S5 S 0.10185(11) 0.09255(7) 0.62316(7) 0.04177(18) Uani 1 1 d . . . S6 S 0.52130(11) 0.09416(7) 0.20874(7) 0.04085(18) Uani 1 1 d . . . S8 S 0.37770(12) 0.31301(7) -0.21211(7) 0.0465(2) Uani 1 1 d . . . Rb1 Rb 0.23506(5) 0.56971(3) 0.05206(3) 0.05110(13) Uani 1 1 d . . . Rb2 Rb 0.20331(5) 0.37046(3) 0.41882(3) 0.05506(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C4 0.0383(15) 0.0307(13) 0.0412(16) -0.0105(12) -0.0081(12) 0.0014(11) C6 0.0388(15) 0.0295(13) 0.0408(16) -0.0103(11) -0.0094(12) 0.0003(11) C7 0.0394(15) 0.0301(13) 0.0373(15) -0.0108(11) -0.0086(12) 0.0035(11) C8 0.0406(15) 0.0294(13) 0.0398(16) -0.0114(11) -0.0070(12) 0.0044(11) C9 0.0436(15) 0.0265(12) 0.0418(16) -0.0114(11) -0.0088(12) 0.0015(11) C12 0.0436(16) 0.0283(13) 0.0395(16) -0.0089(11) -0.0049(12) 0.0007(11) N1 0.0526(15) 0.0256(11) 0.0407(14) -0.0087(10) -0.0032(11) 0.0026(10) N2 0.0445(13) 0.0276(11) 0.0390(13) -0.0108(10) -0.0062(10) 0.0017(9) N3 0.0453(13) 0.0283(11) 0.0354(13) -0.0087(10) -0.0019(10) 0.0003(9) N4 0.0482(14) 0.0272(11) 0.0403(14) -0.0119(10) -0.0017(11) 0.0031(10) N5 0.0473(14) 0.0283(11) 0.0417(14) -0.0128(10) -0.0016(11) 0.0035(10) N10 0.0472(14) 0.0283(11) 0.0365(13) -0.0073(10) -0.0026(10) -0.0004(10) O2 0.0635(17) 0.0410(14) 0.079(2) -0.0145(14) -0.0204(15) 0.0057(12) O3 0.082(2) 0.0408(15) 0.088(2) -0.0120(15) -0.0281(18) 0.0069(14) S1 0.0657(5) 0.0264(3) 0.0521(5) -0.0105(3) -0.0019(4) 0.0012(3) S2 0.0522(4) 0.0306(3) 0.0408(4) -0.0124(3) 0.0009(3) 0.0035(3) S3 0.0644(5) 0.0241(3) 0.0500(5) -0.0094(3) -0.0031(4) 0.0028(3) S5 0.0510(4) 0.0314(3) 0.0417(4) -0.0118(3) 0.0004(3) 0.0053(3) S6 0.0514(4) 0.0315(3) 0.0383(4) -0.0087(3) -0.0019(3) -0.0004(3) S8 0.0613(5) 0.0306(3) 0.0426(4) -0.0071(3) 0.0048(3) 0.0010(3) Rb1 0.0620(2) 0.03398(18) 0.0574(2) -0.01084(14) -0.00974(16) 0.00479(14) Rb2 0.0704(3) 0.03859(19) 0.0549(2) -0.00852(15) -0.00997(17) 0.00741(15) _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 C4 N3 1.346(4) . ? C4 N5 1.340(4) . ? C4 S1 1.678(3) . ? C6 N2 1.340(4) . ? C6 N5 1.388(4) . ? C6 S6 1.681(3) . ? C7 N2 1.339(4) . ? C7 N3 1.385(4) . ? C7 S5 1.686(3) . ? C7 Rb2 3.631(3) . ? C8 N1 1.341(4) . ? C8 N10 1.368(4) . ? C8 S2 1.691(3) . ? C8 Rb1 3.518(3) 2_565 ? C8 Rb1 3.624(3) . ? C9 N4 1.351(4) . ? C9 N10 1.354(4) . ? C9 S3 1.659(3) . ? C12 N1 1.341(4) . ? C12 N4 1.377(4) . ? C12 S8 1.686(3) . ? N1 Rb1 3.305(3) 2_565 ? N1 Rb1 3.106(2) . ? N2 Rb2 3.084(2) . ? O2 Rb1 3.137(3) 2_665 ? O2 Rb1 2.860(3) . ? O2 Rb2 3.117(3) . ? O3 Rb1 3.228(4) . ? O3 Rb2 3.444(4) 2_566 ? O3 Rb2 2.884(3) . ? S1 Rb2 3.9365(10) 2_556 ? S1 Rb2 3.6376(9) 1_545 ? S1 Rb2 3.5533(10) 2_656 ? S2 Rb1 3.4558(9) 2_565 ? S2 Rb1 3.4057(9) . ? S2 Rb2 3.5422(9) . ? S3 Rb1 3.3295(8) 1_545 ? S5 Rb2 3.3487(8) . ? Rb1 C8 3.518(3) 2_565 ? Rb1 N1 3.305(3) 2_565 ? Rb1 O2 3.137(3) 2_665 ? Rb1 S2 3.4558(9) 2_565 ? Rb1 S3 3.3295(8) 1_565 ? Rb1 Rb1 4.2445(7) 2_565 ? Rb1 Rb1 4.2244(7) 2_665 ? Rb2 O3 3.444(4) 2_566 ? Rb2 S1 3.9365(10) 2_556 ? Rb2 S1 3.6377(9) 1_565 ? Rb2 S1 3.5532(10) 2_656 ? Rb2 Rb2 4.4898(7) 2_566 ? 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 N3 C4 S1 121.8(2) . . ? N5 C4 N3 114.8(3) . . ? N5 C4 S1 123.4(2) . . ? N2 C6 N5 119.5(3) . . ? N2 C6 S6 122.9(2) . . ? N5 C6 S6 117.6(2) . . ? N2 C7 N3 119.8(3) . . ? N2 C7 S5 122.6(2) . . ? N2 C7 Rb2 55.78(14) . . ? N3 C7 S5 117.6(2) . . ? N3 C7 Rb2 175.5(2) . . ? S5 C7 Rb2 66.85(9) . . ? N1 C8 N10 120.1(3) . . ? N1 C8 S2 121.2(2) . . ? N1 C8 Rb1 57.05(15) . . ? N1 C8 Rb1 69.86(16) . 2_565 ? N10 C8 S2 118.6(2) . . ? N10 C8 Rb1 158.2(2) . . ? N10 C8 Rb1 128.17(19) . 2_565 ? S2 C8 Rb1 68.98(9) . . ? S2 C8 Rb1 73.94(10) . 2_565 ? Rb1 C8 Rb1 72.91(5) 2_565 . ? N4 C9 N10 114.4(2) . . ? N4 C9 S3 123.1(2) . . ? N10 C9 S3 122.5(2) . . ? N1 C12 N4 119.5(3) . . ? N1 C12 S8 122.2(2) . . ? N4 C12 S8 118.4(2) . . ? C8 N1 C12 118.9(2) . . ? C8 N1 Rb1 87.75(18) . 2_565 ? C8 N1 Rb1 101.71(18) . . ? C12 N1 Rb1 121.3(2) . 2_565 ? C12 N1 Rb1 131.7(2) . . ? Rb1 N1 Rb1 82.85(6) . 2_565 ? C6 N2 Rb2 137.86(19) . . ? C7 N2 C6 118.9(2) . . ? C7 N2 Rb2 103.18(17) . . ? C4 N3 C7 123.3(3) . . ? C9 N4 C12 123.7(3) . . ? C4 N5 C6 123.6(3) . . ? C9 N10 C8 123.4(3) . . ? Rb1 O2 Rb1 89.43(8) . 2_665 ? Rb1 O2 Rb2 92.22(8) . . ? Rb2 O2 Rb1 178.26(9) . 2_665 ? Rb1 O3 Rb2 178.64(10) . 2_566 ? Rb2 O3 Rb1 89.53(8) . . ? Rb2 O3 Rb2 89.95(9) . 2_566 ? C4 S1 Rb2 90.09(11) . 2_556 ? C4 S1 Rb2 138.48(11) . 1_545 ? C4 S1 Rb2 97.73(10) . 2_656 ? Rb2 S1 Rb2 72.588(19) 1_545 2_556 ? Rb2 S1 Rb2 158.16(3) 2_656 2_556 ? Rb2 S1 Rb2 112.40(2) 2_656 1_545 ? C8 S2 Rb1 78.01(10) . 2_565 ? C8 S2 Rb1 83.41(11) . . ? C8 S2 Rb2 113.97(10) . . ? Rb1 S2 Rb1 76.423(19) . 2_565 ? Rb1 S2 Rb2 148.88(2) 2_565 . ? Rb1 S2 Rb2 76.677(19) . . ? C9 S3 Rb1 154.80(11) . 1_545 ? C7 S5 Rb2 85.57(11) . . ? C8 Rb1 C8 107.09(5) 2_565 . ? C8 Rb1 Rb1 85.65(5) . 2_665 ? C8 Rb1 Rb1 54.70(5) 2_565 2_565 ? C8 Rb1 Rb1 52.39(5) . 2_565 ? C8 Rb1 Rb1 133.75(5) 2_565 2_665 ? N1 Rb1 C8 22.39(7) 2_565 2_565 ? N1 Rb1 C8 101.21(7) . 2_565 ? N1 Rb1 C8 95.29(6) 2_565 . ? N1 Rb1 C8 21.24(7) . . ? N1 Rb1 N1 97.15(6) . 2_565 ? N1 Rb1 O2 80.86(7) . 2_665 ? N1 Rb1 O3 114.12(7) . . ? N1 Rb1 S2 81.23(5) 2_565 . ? N1 Rb1 S2 47.70(5) . . ? N1 Rb1 S2 83.31(5) . 2_565 ? N1 Rb1 S2 46.04(5) 2_565 2_565 ? N1 Rb1 S3 166.21(5) . 1_565 ? N1 Rb1 S3 69.07(5) 2_565 1_565 ? N1 Rb1 Rb1 50.59(5) . 2_565 ? N1 Rb1 Rb1 154.11(5) 2_565 2_665 ? N1 Rb1 Rb1 46.56(4) 2_565 2_565 ? N1 Rb1 Rb1 74.77(5) . 2_665 ? O2 Rb1 C8 91.15(7) 2_665 2_565 ? O2 Rb1 C8 177.76(8) . 2_565 ? O2 Rb1 C8 101.09(7) 2_665 . ? O2 Rb1 C8 71.15(7) . . ? O2 Rb1 N1 77.65(7) . . ? O2 Rb1 N1 155.52(8) . 2_565 ? O2 Rb1 N1 112.43(7) 2_665 2_565 ? O2 Rb1 O2 90.57(8) . 2_665 ? O2 Rb1 O3 163.12(7) 2_665 . ? O2 Rb1 O3 85.48(8) . . ? O2 Rb1 S2 66.97(5) 2_665 2_565 ? O2 Rb1 S2 152.66(6) . 2_565 ? O2 Rb1 S2 77.69(6) . . ? O2 Rb1 S2 128.50(5) 2_665 . ? O2 Rb1 S3 104.46(5) 2_665 1_565 ? O2 Rb1 S3 114.58(6) . 1_565 ? O2 Rb1 Rb1 100.43(5) 2_665 2_565 ? O2 Rb1 Rb1 123.52(5) . 2_565 ? O2 Rb1 Rb1 42.61(5) 2_665 2_665 ? O2 Rb1 Rb1 47.96(6) . 2_665 ? O3 Rb1 C8 93.28(7) . 2_565 ? O3 Rb1 C8 93.15(7) . . ? O3 Rb1 N1 74.76(7) . 2_565 ? O3 Rb1 S2 120.49(5) . 2_565 ? O3 Rb1 S2 66.59(5) . . ? O3 Rb1 S3 62.86(5) . 1_565 ? O3 Rb1 Rb1 131.09(5) . 2_665 ? O3 Rb1 Rb1 95.41(6) . 2_565 ? S2 Rb1 C8 28.05(5) 2_565 2_565 ? S2 Rb1 C8 27.61(5) . . ? S2 Rb1 C8 97.10(5) 2_565 . ? S2 Rb1 C8 100.10(5) . 2_565 ? S2 Rb1 S2 103.578(19) . 2_565 ? S2 Rb1 Rb1 108.541(17) . 2_665 ? S2 Rb1 Rb1 51.257(15) 2_565 2_565 ? S2 Rb1 Rb1 108.114(19) 2_565 2_665 ? S2 Rb1 Rb1 52.320(16) . 2_565 ? S3 Rb1 C8 66.34(5) 1_565 2_565 ? S3 Rb1 C8 153.65(5) 1_565 . ? S3 Rb1 S2 87.11(2) 1_565 2_565 ? S3 Rb1 S2 126.17(2) 1_565 . ? S3 Rb1 Rb1 117.85(2) 1_565 2_665 ? S3 Rb1 Rb1 115.63(2) 1_565 2_565 ? Rb1 Rb1 Rb1 120.550(16) 2_665 2_565 ? C7 Rb2 S1 135.15(5) . 1_565 ? C7 Rb2 S1 90.11(5) . 2_556 ? C7 Rb2 Rb1 124.53(5) . . ? C7 Rb2 Rb2 125.17(5) . 2_566 ? N2 Rb2 C7 21.04(7) . . ? N2 Rb2 O2 78.06(7) . . ? N2 Rb2 O3 111.59(7) . 2_566 ? N2 Rb2 S1 141.59(5) . 1_565 ? N2 Rb2 S1 75.72(5) . 2_656 ? N2 Rb2 S1 102.28(5) . 2_556 ? N2 Rb2 S2 79.26(5) . . ? N2 Rb2 S5 48.61(5) . . ? N2 Rb2 Rb1 105.89(5) . . ? N2 Rb2 Rb2 145.22(5) . 2_566 ? O2 Rb2 C7 99.00(7) . . ? O2 Rb2 O3 164.25(7) . 2_566 ? O2 Rb2 S1 99.47(5) . 1_565 ? O2 Rb2 S1 130.84(5) . 2_556 ? O2 Rb2 S1 70.56(5) . 2_656 ? O2 Rb2 S2 72.52(5) . . ? O2 Rb2 S5 126.33(5) . . ? O2 Rb2 Rb1 41.53(5) . . ? O2 Rb2 Rb2 134.96(5) . 2_566 ? O3 Rb2 C7 90.72(6) 2_566 . ? O3 Rb2 C7 151.87(8) . . ? O3 Rb2 N2 147.08(8) . . ? O3 Rb2 O2 87.18(9) . . ? O3 Rb2 O3 90.05(9) . 2_566 ? O3 Rb2 S1 65.12(5) 2_566 1_565 ? O3 Rb2 S1 99.08(5) 2_566 2_656 ? O3 Rb2 S1 65.92(7) . 2_556 ? O3 Rb2 S1 60.96(5) 2_566 2_556 ? O3 Rb2 S1 69.48(6) . 1_565 ? O3 Rb2 S1 126.73(7) . 2_656 ? O3 Rb2 S2 68.22(6) . . ? O3 Rb2 S2 120.61(5) 2_566 . ? O3 Rb2 S5 140.08(7) . . ? O3 Rb2 Rb1 138.52(4) 2_566 . ? O3 Rb2 Rb1 48.49(7) . . ? O3 Rb2 Rb2 39.96(4) 2_566 2_566 ? O3 Rb2 Rb2 50.08(7) . 2_566 ? S1 Rb2 C7 80.83(5) 2_656 . ? S1 Rb2 S1 107.411(19) 1_565 2_556 ? S1 Rb2 S1 158.16(3) 2_656 2_556 ? S1 Rb2 S1 67.60(2) 2_656 1_565 ? S1 Rb2 Rb1 94.619(16) 2_556 . ? S1 Rb2 Rb1 106.905(18) 2_656 . ? S1 Rb2 Rb1 95.544(17) 1_565 . ? S1 Rb2 Rb2 56.781(17) 1_565 2_566 ? S1 Rb2 Rb2 120.342(19) 2_656 2_566 ? S1 Rb2 Rb2 50.631(14) 2_556 2_566 ? S2 Rb2 C7 87.39(5) . . ? S2 Rb2 S1 138.73(2) . 2_656 ? S2 Rb2 S1 137.23(2) . 1_565 ? S2 Rb2 S1 59.69(2) . 2_556 ? S2 Rb2 Rb1 50.239(14) . . ? S2 Rb2 Rb2 98.754(17) . 2_566 ? S5 Rb2 C7 27.58(5) . . ? S5 Rb2 O3 63.27(5) . 2_566 ? S5 Rb2 S1 88.43(2) . 2_656 ? S5 Rb2 S1 117.59(2) . 1_565 ? S5 Rb2 S1 74.95(2) . 2_556 ? S5 Rb2 S2 99.03(2) . . ? S5 Rb2 Rb1 146.827(18) . . ? S5 Rb2 Rb2 98.486(18) . 2_566 ? Rb1 Rb2 Rb2 98.563(12) . 2_566 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 2 8 0.0521 0.0000 2.0000 8.0000 0.1751 0.3789 0.9807 0 -2 -8 0.0521 -0.0000 -2.0000 -8.0000 -0.1751 -0.3789 -0.9807 1 -6 1 0.0509 1.0000 -6.0000 1.0000 0.9195 -0.2654 -0.0054 -1 6 -1 0.0229 -1.0000 6.0000 -1.0000 -0.9195 0.2654 0.0054 0 0 7 0.0440 0.0000 -0.0000 7.0000 0.3806 0.1998 0.8541 -3 -4 1 0.0447 -3.0000 -4.0000 1.0000 0.3172 -0.7457 0.4532 3 4 -1 0.0447 3.0000 4.0000 -1.0000 -0.3172 0.7457 -0.4532 3 5 3 0.0639 3.0000 5.0000 3.0000 -0.2296 0.9351 0.0371 -3 -5 -3 0.0329 -3.0000 -5.0000 -3.0000 0.2296 -0.9351 -0.0371 4 -3 0 0.0273 4.0000 -3.0000 0.0000 0.7322 0.4049 -0.4610 _database_code_depnum_ccdc_archive 'CCDC 944679' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RbTTC2 _audit_creation_date 2013-06-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H10.5 N6 O3 Rb1.5 S6' _chemical_formula_sum 'C6 H10.50 N6 O3 Rb1.50 S6' _chemical_formula_weight 535.27 _chemical_melting_point ? _chemical_oxdiff_formula 'S6 N6 C6 H9 O2.5 Rb1.5' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.5673(3) _cell_length_b 11.2806(6) _cell_length_c 11.4428(4) _cell_angle_alpha 107.984(4) _cell_angle_beta 94.103(3) _cell_angle_gamma 102.469(4) _cell_volume 897.06(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7535 _cell_measurement_temperature 298.9(8) _cell_measurement_theta_max 71.1390 _cell_measurement_theta_min 4.1040 _exptl_absorpt_coefficient_mu 12.154 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_correction_T_min 0.123 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.5026 _exptl_crystal_size_mid 0.0751 _exptl_crystal_size_min 0.0386 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_unetI/netI 0.0192 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12265 _diffrn_reflns_theta_full 71.9829 _diffrn_reflns_theta_max 71.15 _diffrn_reflns_theta_min 4.11 _diffrn_ambient_temperature 298.9(8) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9763 _diffrn_measured_fraction_theta_max 0.9920 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 4.00 30.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega 32.00 64.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 3 omega -65.00 -31.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -90.0000 34 #__ type_ start__ end____ width___ exp.time_ 4 omega -2.00 24.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega -66.00 -21.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - -54.7500 125.0000 -60.0000 45 #__ type_ start__ end____ width___ exp.time_ 6 omega 79.00 126.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 90.0000 47 #__ type_ start__ end____ width___ exp.time_ 7 omega 33.00 124.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 60.0000 91 #__ type_ start__ end____ width___ exp.time_ 8 omega 75.00 113.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 0.0000 38 #__ type_ start__ end____ width___ exp.time_ 9 omega 29.00 124.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 37.0000 -180.0000 95 #__ type_ start__ end____ width___ exp.time_ 10 omega -17.00 8.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 37.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 11 omega -69.00 -41.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 37.0000 120.0000 28 #__ type_ start__ end____ width___ exp.time_ 12 omega -110.00 -20.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 111.0000 -150.0000 90 #__ type_ start__ end____ width___ exp.time_ 13 omega 37.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -60.0000 33 #__ type_ start__ end____ width___ exp.time_ 14 omega 38.00 68.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 90.0000 30 #__ type_ start__ end____ width___ exp.time_ 15 omega 89.00 154.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 30.0000 65 #__ type_ start__ end____ width___ exp.time_ 16 omega 37.00 62.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 17 omega 43.00 72.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 18 omega 97.00 136.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -70.0000 127.9469 39 #__ type_ start__ end____ width___ exp.time_ 19 omega 44.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 139.8682 26 #__ type_ start__ end____ width___ exp.time_ 20 omega 71.00 101.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 0.0000 30 #__ type_ start__ end____ width___ exp.time_ 21 omega 122.00 177.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 -30.0000 55 #__ type_ start__ end____ width___ exp.time_ 22 omega 39.00 64.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 23 omega 84.00 126.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -60.0000 42 #__ type_ start__ end____ width___ exp.time_ 24 omega 41.00 71.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 150.0000 30 #__ type_ start__ end____ width___ exp.time_ 25 omega 42.00 67.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 26 omega 77.00 117.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 27 omega 136.00 173.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 0.0000 37 #__ type_ start__ end____ width___ exp.time_ 28 omega 108.00 133.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 29 omega 38.00 64.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 30 omega 38.00 72.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -30.0000 34 #__ type_ start__ end____ width___ exp.time_ 31 omega 49.00 80.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -70.0000 127.9469 31 #__ type_ start__ end____ width___ exp.time_ 32 omega 47.00 73.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 33 omega 95.00 140.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 -90.0000 45 #__ type_ start__ end____ width___ exp.time_ 34 omega 48.00 81.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -120.0000 33 #__ type_ start__ end____ width___ exp.time_ 35 omega 53.00 80.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 36 omega 119.00 145.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 37 omega 148.00 173.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 38 omega 53.00 82.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -30.0000 29 #__ type_ start__ end____ width___ exp.time_ 39 omega 38.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 150.0000 32 #__ type_ start__ end____ width___ exp.time_ 40 omega 135.00 175.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -120.0000 40 #__ type_ start__ end____ width___ exp.time_ 41 omega 79.00 120.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 42 omega 92.00 117.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 43 omega 89.00 116.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 44 omega 46.00 71.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 45 omega 74.00 145.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 139.8682 71 #__ type_ start__ end____ width___ exp.time_ 46 omega 89.00 116.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 90.0000 27 #__ type_ start__ end____ width___ exp.time_ 47 omega 68.00 134.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -92.0000 5.3638 66 #__ type_ start__ end____ width___ exp.time_ 48 omega 106.00 133.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 90.0000 27 #__ type_ start__ end____ width___ exp.time_ 49 omega 88.00 114.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 50 omega 101.00 128.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 51 omega 41.00 106.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -92.0000 -81.3666 65 #__ type_ start__ end____ width___ exp.time_ 52 omega -30.00 70.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 53 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -150.0000 45 #__ type_ start__ end____ width___ exp.time_ 54 omega -125.00 -25.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 120.0000 100 #__ type_ start__ end____ width___ exp.time_ 55 omega -124.00 -33.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 -150.0000 91 #__ type_ start__ end____ width___ exp.time_ 56 omega -15.00 85.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 -77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 57 omega 25.00 125.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 58 omega 25.00 125.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 59 omega 25.00 125.00 1.0000 1.1400 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 60 omega 88.00 178.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 0.0000 90 #__ type_ start__ end____ width___ exp.time_ 61 omega 84.00 178.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -120.0000 94 #__ type_ start__ end____ width___ exp.time_ 62 omega 37.00 72.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -90.0000 35 #__ type_ start__ end____ width___ exp.time_ 63 omega 84.00 178.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 90.0000 94 #__ type_ start__ end____ width___ exp.time_ 64 omega 37.00 72.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -150.0000 35 #__ type_ start__ end____ width___ exp.time_ 65 omega 79.00 118.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 120.0000 39 #__ type_ start__ end____ width___ exp.time_ 66 omega 88.00 119.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -180.0000 31 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1919855000 _diffrn_orient_matrix_UB_12 -0.0672477000 _diffrn_orient_matrix_UB_13 0.0164816000 _diffrn_orient_matrix_UB_21 -0.0533812000 _diffrn_orient_matrix_UB_22 -0.0582943000 _diffrn_orient_matrix_UB_23 -0.1421856000 _diffrn_orient_matrix_UB_31 0.0689107000 _diffrn_orient_matrix_UB_32 -0.1186580000 _diffrn_orient_matrix_UB_33 0.0009512000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3368 _reflns_number_total 3453 _reflns_odcompleteness_completeness 97.63 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.354 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 229 _refine_ls_number_reflns 3453 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0295 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.8496P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.0750 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2. Restrained distances H1B-O1 = O1-H1A 0.957 with sigma of 0.02 H2B-O2 = O2-H2A 0.957 with sigma of 0.02 H3A-O3 0.957 with sigma of 0.02 H3B-O3 0.957 with sigma of 0.02 H2A-O2 = O2-H2B 0.958 with sigma of 0.02 H1A-O1 = O1-H1B 0.958 with sigma of 0.02 H3A-O3 0.958 with sigma of 0.02 H3B-O3 0.958 with sigma of 0.02 H1B-H1A 1.513 with sigma of 0.04 H2B-H2A 1.513 with sigma of 0.04 H2A-H2B 1.515 with sigma of 0.04 H1A-H1B 1.515 with sigma of 0.04 3. Others Fixed Sof: H3B(0.5) 4.a Aromatic/amide H refined with riding coordinates: N1(H1), N2(H2), N4(H4), N5(H5), N6(H6) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H1A H -0.277(3) -0.509(6) 0.142(5) 0.11(2) Uiso 1 1 d D . . H1B H -0.097(8) -0.519(8) 0.198(5) 0.17(3) Uiso 1 1 d D . . H3A H -0.205(5) -0.148(4) -0.021(3) 0.075(14) Uiso 1 1 d D . . H2A H 0.507(5) -0.288(3) 0.022(3) 0.061(12) Uiso 1 1 d D . . H2B H 0.540(6) -0.215(5) 0.159(2) 0.097(18) Uiso 1 1 d D . . H3B H -0.040(14) -0.013(6) 0.030(10) 0.08(3) Uiso 0.50 1 d PD . . C1 C 0.2056(4) 0.0230(3) 0.6334(2) 0.0297(5) Uani 1 1 d . . . C2 C 0.3348(4) 0.3681(3) 0.2224(2) 0.0305(5) Uani 1 1 d . . . C4 C 0.2761(4) 0.3963(2) 0.4321(2) 0.0283(5) Uani 1 1 d . . . C7 C 0.3214(4) 0.1976(2) 0.2959(2) 0.0289(5) Uani 1 1 d . . . C9 C 0.2527(4) -0.1731(3) 0.4940(2) 0.0300(5) Uani 1 1 d . . . C10 C 0.1771(4) -0.1599(3) 0.6978(2) 0.0283(5) Uani 1 1 d . . . N1 N 0.2479(3) -0.0480(2) 0.5230(2) 0.0311(5) Uani 1 1 d . . . H1 H 0.2729 -0.0108 0.4689 0.037 Uiso 1 1 calc R . . N2 N 0.1770(3) -0.0345(2) 0.7206(2) 0.0313(5) Uani 1 1 d . . . H2 H 0.1583 0.0097 0.7925 0.038 Uiso 1 1 calc R . . N3 N 0.3441(3) 0.2465(2) 0.2030(2) 0.0316(5) Uani 1 1 d . . . N4 N 0.3001(3) 0.4398(2) 0.3358(2) 0.0315(5) Uani 1 1 d . . . H4 H 0.2933 0.5173 0.3457 0.038 Uiso 1 1 calc R . . N5 N 0.2080(3) -0.2262(2) 0.5821(2) 0.0316(5) Uani 1 1 d . . . H5 H 0.1981 -0.3074 0.5643 0.038 Uiso 1 1 calc R . . N6 N 0.2898(3) 0.2732(2) 0.4086(2) 0.0317(5) Uani 1 1 d . . . H6 H 0.2780 0.2407 0.4672 0.038 Uiso 1 1 calc R . . O1 O -0.1520(4) -0.4998(3) 0.1319(3) 0.0625(7) Uani 1 1 d D . . O2 O 0.4693(3) -0.2241(2) 0.0834(2) 0.0497(5) Uani 1 1 d D . . O3 O -0.1100(4) -0.0884(2) 0.0401(2) 0.0491(5) Uani 1 1 d D . . S1 S 0.23323(12) 0.48371(7) 0.56797(6) 0.03944(17) Uani 1 1 d . . . S2 S 0.14183(11) -0.23452(7) 0.80116(6) 0.03896(17) Uani 1 1 d . . . S3 S 0.33006(11) 0.04584(6) 0.28033(6) 0.03659(16) Uani 1 1 d . . . S4 S 0.36163(12) 0.43985(7) 0.11365(7) 0.04366(18) Uani 1 1 d . . . S5 S 0.31180(13) -0.25466(7) 0.36174(7) 0.04391(19) Uani 1 1 d . . . S6 S 0.19297(11) 0.17431(7) 0.65755(7) 0.03869(17) Uani 1 1 d . . . Rb1 Rb 0.5000 0.0000 0.0000 0.04479(12) Uani 1 2 d S . . Rb2 Rb 0.06933(5) -0.28183(3) 0.08622(3) 0.05119(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0316(13) 0.0287(13) 0.0282(12) 0.0084(10) 0.0065(10) 0.0072(10) C2 0.0347(13) 0.0316(13) 0.0251(12) 0.0102(10) 0.0044(10) 0.0072(11) C4 0.0345(13) 0.0246(12) 0.0258(12) 0.0082(10) 0.0035(10) 0.0075(10) C7 0.0331(13) 0.0264(13) 0.0244(12) 0.0051(10) 0.0037(10) 0.0068(10) C9 0.0373(13) 0.0276(13) 0.0264(12) 0.0092(10) 0.0060(10) 0.0102(11) C10 0.0312(12) 0.0278(13) 0.0265(12) 0.0102(10) 0.0065(10) 0.0064(10) N1 0.0452(13) 0.0266(11) 0.0263(10) 0.0122(9) 0.0109(9) 0.0120(10) N2 0.0405(12) 0.0273(11) 0.0277(11) 0.0085(9) 0.0108(9) 0.0108(9) N3 0.0404(12) 0.0304(11) 0.0263(10) 0.0106(9) 0.0083(9) 0.0110(10) N4 0.0444(13) 0.0240(11) 0.0271(11) 0.0085(9) 0.0071(9) 0.0103(9) N5 0.0455(13) 0.0240(11) 0.0268(11) 0.0085(9) 0.0111(9) 0.0101(9) N6 0.0483(13) 0.0274(11) 0.0239(10) 0.0111(9) 0.0095(9) 0.0134(10) O1 0.0788(19) 0.0662(17) 0.0554(15) 0.0360(14) 0.0192(14) 0.0185(15) O2 0.0571(14) 0.0479(13) 0.0459(13) 0.0154(11) 0.0123(11) 0.0156(11) O3 0.0627(15) 0.0401(12) 0.0344(11) 0.0062(9) 0.0103(10) 0.0000(11) S1 0.0639(5) 0.0318(3) 0.0269(3) 0.0094(3) 0.0152(3) 0.0185(3) S2 0.0581(4) 0.0327(3) 0.0301(3) 0.0159(3) 0.0146(3) 0.0091(3) S3 0.0557(4) 0.0261(3) 0.0320(3) 0.0108(3) 0.0135(3) 0.0146(3) S4 0.0692(5) 0.0391(4) 0.0310(3) 0.0194(3) 0.0149(3) 0.0171(4) S5 0.0766(5) 0.0371(4) 0.0293(3) 0.0145(3) 0.0239(3) 0.0275(4) S6 0.0576(4) 0.0276(3) 0.0367(3) 0.0126(3) 0.0156(3) 0.0173(3) Rb1 0.0492(2) 0.0463(2) 0.0406(2) 0.01958(18) 0.00884(17) 0.00711(18) Rb2 0.05228(19) 0.0528(2) 0.04698(18) 0.01737(15) 0.00983(14) 0.00805(15) _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 C1 N1 1.372(3) . ? C1 N2 1.354(3) . ? C1 S6 1.667(3) . ? C2 N3 1.338(4) . ? C2 N4 1.378(3) . ? C2 S4 1.683(3) . ? C4 N4 1.346(3) . ? C4 N6 1.359(3) . ? C4 S1 1.661(3) . ? C7 N3 1.346(3) . ? C7 N6 1.378(3) . ? C7 S3 1.681(3) . ? C9 N1 1.356(3) . ? C9 N5 1.351(3) . ? C9 S5 1.658(3) . ? C10 N2 1.357(3) . ? C10 N5 1.369(3) . ? C10 S2 1.656(3) . ? N3 Rb1 3.513(2) . ? O1 Rb2 3.127(3) 2_545 ? O1 Rb2 2.875(3) . ? O2 Rb1 2.937(3) . ? O2 Rb2 2.960(3) . ? O3 Rb1 3.358(3) 1_455 ? O3 Rb2 2.961(3) . ? S2 Rb1 3.4389(8) 1_556 ? S2 Rb2 3.5256(7) 1_556 ? S3 Rb1 3.4733(7) . ? S3 Rb2 3.6937(8) . ? S4 Rb2 3.5985(10) 2 ? S5 Rb2 3.4253(9) . ? S6 Rb2 3.6993(8) 2_556 ? Rb1 N3 3.513(2) 2_655 ? Rb1 O2 2.937(3) 2_655 ? Rb1 O3 3.358(3) 1_655 ? Rb1 O3 3.358(3) 2 ? Rb1 S2 3.4389(8) 1_554 ? Rb1 S2 3.4389(8) 2_656 ? Rb1 S3 3.4733(7) 2_655 ? Rb1 Rb2 4.4299(4) . ? Rb1 Rb2 4.4299(4) 2_655 ? Rb2 O1 3.127(3) 2_545 ? Rb2 S2 3.5255(7) 1_554 ? Rb2 S4 3.5984(10) 2 ? Rb2 S6 3.6993(8) 2_556 ? Rb2 Rb2 4.5496(8) 2_545 ? 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 C1 S6 120.5(2) . . ? N2 C1 N1 117.2(2) . . ? N2 C1 S6 122.2(2) . . ? N3 C2 N4 119.6(2) . . ? N3 C2 S4 123.2(2) . . ? N4 C2 S4 117.1(2) . . ? N4 C4 N6 114.0(2) . . ? N4 C4 S1 123.7(2) . . ? N6 C4 S1 122.4(2) . . ? N3 C7 N6 119.6(2) . . ? N3 C7 S3 122.4(2) . . ? N6 C7 S3 118.0(2) . . ? N1 C9 S5 122.9(2) . . ? N5 C9 N1 114.7(2) . . ? N5 C9 S5 122.4(2) . . ? N2 C10 N5 116.9(2) . . ? N2 C10 S2 123.6(2) . . ? N5 C10 S2 119.5(2) . . ? C9 N1 C1 124.2(2) . . ? C1 N2 C10 121.9(2) . . ? C2 N3 C7 118.9(2) . . ? C2 N3 Rb1 141.13(17) . . ? C7 N3 Rb1 98.54(16) . . ? C4 N4 C2 124.2(2) . . ? C9 N5 C10 124.7(2) . . ? C4 N6 C7 123.7(2) . . ? Rb2 O1 Rb2 98.49(8) . 2_545 ? Rb1 O2 Rb2 97.39(7) . . ? Rb2 O3 Rb1 147.89(8) . 1_455 ? C10 S2 Rb1 88.25(9) . 1_556 ? C10 S2 Rb2 159.69(10) . 1_556 ? Rb1 S2 Rb2 78.989(16) 1_556 1_556 ? C7 S3 Rb1 93.27(9) . . ? C7 S3 Rb2 136.77(9) . . ? Rb1 S3 Rb2 76.286(15) . . ? C2 S4 Rb2 99.68(10) . 2 ? C9 S5 Rb2 119.08(10) . . ? C1 S6 Rb2 111.26(10) . 2_556 ? N3 Rb1 N3 180.0 . 2_655 ? N3 Rb1 Rb2 88.15(4) 2_655 2_655 ? N3 Rb1 Rb2 91.85(4) . 2_655 ? N3 Rb1 Rb2 91.85(4) 2_655 . ? N3 Rb1 Rb2 88.15(4) . . ? O2 Rb1 N3 112.39(6) . . ? O2 Rb1 N3 67.61(6) 2_655 . ? O2 Rb1 N3 112.39(6) 2_655 2_655 ? O2 Rb1 N3 67.60(6) . 2_655 ? O2 Rb1 O2 180.0 2_655 . ? O2 Rb1 O3 115.81(6) 2_655 1_655 ? O2 Rb1 O3 115.81(6) . 2 ? O2 Rb1 O3 64.19(6) 2_655 2 ? O2 Rb1 O3 64.19(6) . 1_655 ? O2 Rb1 S2 74.58(5) . 1_554 ? O2 Rb1 S2 105.42(5) 2_655 1_554 ? O2 Rb1 S2 74.58(5) 2_655 2_656 ? O2 Rb1 S2 105.42(5) . 2_656 ? O2 Rb1 S3 67.71(5) . . ? O2 Rb1 S3 112.29(5) 2_655 . ? O2 Rb1 S3 112.29(5) . 2_655 ? O2 Rb1 S3 67.71(5) 2_655 2_655 ? O2 Rb1 Rb2 41.50(5) . . ? O2 Rb1 Rb2 138.50(5) 2_655 . ? O2 Rb1 Rb2 41.50(5) 2_655 2_655 ? O2 Rb1 Rb2 138.50(5) . 2_655 ? O3 Rb1 N3 51.48(5) 2 . ? O3 Rb1 N3 128.52(5) 1_655 . ? O3 Rb1 N3 128.52(5) 2 2_655 ? O3 Rb1 N3 51.48(5) 1_655 2_655 ? O3 Rb1 O3 180.0 2 1_655 ? O3 Rb1 S2 64.02(4) 1_655 2_656 ? O3 Rb1 S2 64.02(4) 2 1_554 ? O3 Rb1 S2 115.98(4) 1_655 1_554 ? O3 Rb1 S2 115.98(4) 2 2_656 ? O3 Rb1 S3 105.75(4) 2 2_655 ? O3 Rb1 S3 74.25(4) 1_655 2_655 ? O3 Rb1 S3 105.75(4) 1_655 . ? O3 Rb1 S3 74.25(4) 2 . ? O3 Rb1 Rb2 74.33(4) 2 . ? O3 Rb1 Rb2 105.67(4) 1_655 . ? O3 Rb1 Rb2 74.33(4) 1_655 2_655 ? O3 Rb1 Rb2 105.67(4) 2 2_655 ? S2 Rb1 N3 111.27(4) 2_656 2_655 ? S2 Rb1 N3 68.73(4) 2_656 . ? S2 Rb1 N3 111.27(4) 1_554 . ? S2 Rb1 N3 68.73(4) 1_554 2_655 ? S2 Rb1 S2 179.998(1) 2_656 1_554 ? S2 Rb1 S3 100.696(17) 2_656 2_655 ? S2 Rb1 S3 100.697(18) 1_554 . ? S2 Rb1 S3 79.304(17) 2_656 . ? S2 Rb1 S3 79.303(17) 1_554 2_655 ? S2 Rb1 Rb2 51.370(12) 1_554 . ? S2 Rb1 Rb2 51.371(12) 2_656 2_655 ? S2 Rb1 Rb2 128.629(12) 2_656 . ? S2 Rb1 Rb2 128.630(12) 1_554 2_655 ? S3 Rb1 N3 44.71(4) 2_655 2_655 ? S3 Rb1 N3 135.29(4) . 2_655 ? S3 Rb1 N3 135.29(4) 2_655 . ? S3 Rb1 N3 44.71(4) . . ? S3 Rb1 S3 180.0 2_655 . ? S3 Rb1 Rb2 125.901(13) . 2_655 ? S3 Rb1 Rb2 54.099(13) 2_655 2_655 ? S3 Rb1 Rb2 125.900(13) 2_655 . ? S3 Rb1 Rb2 54.099(13) . . ? Rb2 Rb1 Rb2 180.0 2_655 . ? O1 Rb2 O1 81.51(8) . 2_545 ? O1 Rb2 O2 126.74(8) . . ? O1 Rb2 O3 118.53(8) . . ? O1 Rb2 S2 59.69(5) 2_545 1_554 ? O1 Rb2 S2 129.34(6) . 1_554 ? O1 Rb2 S3 134.35(6) 2_545 . ? O1 Rb2 S3 135.44(6) . . ? O1 Rb2 S4 63.15(6) . 2 ? O1 Rb2 S4 74.68(6) 2_545 2 ? O1 Rb2 S5 110.33(6) 2_545 . ? O1 Rb2 S5 80.89(6) . . ? O1 Rb2 S6 69.56(6) . 2_556 ? O1 Rb2 S6 150.68(6) 2_545 2_556 ? O1 Rb2 Rb1 88.77(5) 2_545 . ? O1 Rb2 Rb1 167.08(7) . . ? O1 Rb2 Rb2 42.83(6) . 2_545 ? O1 Rb2 Rb2 38.68(5) 2_545 2_545 ? O2 Rb2 O1 71.68(8) . 2_545 ? O2 Rb2 O3 114.73(7) . . ? O2 Rb2 S2 72.97(5) . 1_554 ? O2 Rb2 S3 64.38(5) . . ? O2 Rb2 S4 142.09(5) . 2 ? O2 Rb2 S5 67.48(5) . . ? O2 Rb2 S6 130.03(5) . 2_556 ? O2 Rb2 Rb1 41.10(5) . . ? O2 Rb2 Rb2 99.32(5) . 2_545 ? O3 Rb2 O1 121.66(7) . 2_545 ? O3 Rb2 S2 67.31(5) . 1_554 ? O3 Rb2 S3 69.87(5) . . ? O3 Rb2 S4 69.89(5) . 2 ? O3 Rb2 S5 125.98(5) . . ? O3 Rb2 S6 71.28(5) . 2_556 ? O3 Rb2 Rb1 73.89(5) . . ? O3 Rb2 Rb2 131.50(5) . 2_545 ? S2 Rb2 S3 94.958(18) 1_554 . ? S2 Rb2 S4 75.314(19) 1_554 2 ? S2 Rb2 S6 138.45(2) 1_554 2_556 ? S2 Rb2 Rb1 49.640(13) 1_554 . ? S2 Rb2 Rb2 93.081(16) 1_554 2_545 ? S3 Rb2 S6 73.545(18) . 2_556 ? S3 Rb2 Rb1 49.614(12) . . ? S3 Rb2 Rb2 158.546(18) . 2_545 ? S4 Rb2 S3 139.24(2) 2 . ? S4 Rb2 S6 87.74(2) 2 2_556 ? S4 Rb2 Rb1 122.400(15) 2 . ? S4 Rb2 Rb2 62.159(15) 2 2_545 ? S5 Rb2 S2 140.12(2) . 1_554 ? S5 Rb2 S3 63.648(18) . . ? S5 Rb2 S4 142.90(2) . 2 ? S5 Rb2 S6 70.502(19) . 2_556 ? S5 Rb2 Rb1 94.681(17) . . ? S5 Rb2 Rb2 97.973(17) . 2_545 ? S6 Rb2 Rb1 120.547(15) 2_556 . ? S6 Rb2 Rb2 112.248(16) 2_556 2_545 ? Rb1 Rb2 Rb2 126.949(13) . 2_545 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 -7 3 0.0540 0.0000 -7.0000 3.0000 0.5202 -0.0185 0.8335 0 7 -3 0.0210 -0.0000 7.0000 -3.0000 -0.5202 0.0185 -0.8335 5 -2 -1 0.2443 5.0000 -2.0000 -1.0000 -0.8419 -0.0081 0.5809 -5 2 1 0.2483 -5.0000 2.0000 1.0000 0.8419 0.0081 -0.5809 0 0 -7 0.0103 -0.0000 0.0000 -7.0000 -0.1154 0.9953 -0.0067 0 0 7 0.0283 0.0000 -0.0000 7.0000 0.1154 -0.9953 0.0067 _database_code_depnum_ccdc_archive 'CCDC 944680' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CsTTC1 _audit_creation_date 2013-05-30 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C3 H2 Cs N3 S3' _chemical_formula_sum 'C3 H2 Cs N3 S3' _chemical_formula_weight 309.17 _chemical_melting_point ? _chemical_oxdiff_formula 'Cs C3 N3 S3 H2' 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.7457 7.9052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 5.1031(3) _cell_length_b 7.9838(6) _cell_length_c 10.9408(6) _cell_angle_alpha 96.431(5) _cell_angle_beta 103.270(5) _cell_angle_gamma 104.265(5) _cell_volume 413.70(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2771 _cell_measurement_temperature 300.00(14) _cell_measurement_theta_max 71.1650 _cell_measurement_theta_min 4.2150 _exptl_absorpt_coefficient_mu 41.431 _exptl_absorpt_correction_T_max 0.293 _exptl_absorpt_correction_T_min 0.034 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_density_diffrn 2.482 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.1963 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.0449 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3826 _diffrn_reflns_theta_full 71.06 _diffrn_reflns_theta_max 71.06 _diffrn_reflns_theta_min 4.22 _diffrn_ambient_temperature 300.00(14) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.9794 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 32.00 57.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 -37.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega 2.00 28.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega -123.00 -90.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - -54.7500 -158.0000 -10.0000 33 #__ type_ start__ end____ width___ exp.time_ 5 omega -123.00 -28.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 -180.0000 95 #__ type_ start__ end____ width___ exp.time_ 6 omega -12.00 43.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 -57.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 7 omega -5.00 70.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 -37.0000 -180.0000 75 #__ type_ start__ end____ width___ exp.time_ 8 omega 73.00 113.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 -120.0000 40 #__ type_ start__ end____ width___ exp.time_ 9 omega 0.00 94.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 -125.0000 -30.0000 94 #__ type_ start__ end____ width___ exp.time_ 10 omega -74.00 -47.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -50.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 11 omega 42.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -90.0000 29 #__ type_ start__ end____ width___ exp.time_ 12 omega 79.00 138.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -150.0000 59 #__ type_ start__ end____ width___ exp.time_ 13 omega 85.00 122.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 14 omega 39.00 66.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 15 omega 43.00 69.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 16 omega 38.00 67.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 17 omega 37.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -120.0000 34 #__ type_ start__ end____ width___ exp.time_ 18 omega 37.00 62.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 90.0000 25 #__ type_ start__ end____ width___ exp.time_ 19 omega 39.00 111.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 0.0000 72 #__ type_ start__ end____ width___ exp.time_ 20 omega 94.00 121.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 21 omega 87.00 176.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -180.0000 89 #__ type_ start__ end____ width___ exp.time_ 22 omega 42.00 68.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 23 omega 44.00 90.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 120.0000 46 #__ type_ start__ end____ width___ exp.time_ 24 omega 53.00 103.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -60.0000 50 #__ type_ start__ end____ width___ exp.time_ 25 omega 91.00 122.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 30.0000 31 #__ type_ start__ end____ width___ exp.time_ 26 omega 153.00 178.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 30.0000 25 #__ type_ start__ end____ width___ exp.time_ 27 omega 43.00 70.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 28 omega 147.00 173.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 29 omega 76.00 126.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 12.0000 150.0000 50 #__ type_ start__ end____ width___ exp.time_ 30 omega 82.00 111.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 31 omega 43.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 12.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 32 omega 37.00 71.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 30.0000 34 #__ type_ start__ end____ width___ exp.time_ 33 omega 140.00 169.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 111.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 34 omega 46.00 95.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 150.0000 49 #__ type_ start__ end____ width___ exp.time_ 35 omega 110.00 140.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 150.0000 30 #__ type_ start__ end____ width___ exp.time_ 36 omega 47.00 88.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 90.0000 41 #__ type_ start__ end____ width___ exp.time_ 37 omega 120.00 164.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -60.0000 44 #__ type_ start__ end____ width___ exp.time_ 38 omega 107.00 133.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 39 omega 73.00 119.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 178.0000 -30.0000 46 #__ type_ start__ end____ width___ exp.time_ 40 omega 78.00 123.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -85.0000 -7.4306 45 #__ type_ start__ end____ width___ exp.time_ 41 omega -70.00 30.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 42 omega 32.00 77.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 150.0000 45 #__ type_ start__ end____ width___ exp.time_ 43 omega -124.00 -33.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - -54.7500 -57.0000 -120.0000 91 #__ type_ start__ end____ width___ exp.time_ 44 omega -125.00 -25.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - -54.7500 -77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 45 omega 25.00 50.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 46 omega 33.00 124.00 1.0000 2.1700 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 -30.0000 91 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1139233000 _diffrn_orient_matrix_UB_12 -0.0738053000 _diffrn_orient_matrix_UB_13 -0.1441089000 _diffrn_orient_matrix_UB_21 -0.0944874000 _diffrn_orient_matrix_UB_22 0.1658948000 _diffrn_orient_matrix_UB_23 -0.0213044000 _diffrn_orient_matrix_UB_31 0.2873498000 _diffrn_orient_matrix_UB_32 0.0893325000 _diffrn_orient_matrix_UB_33 -0.0199781000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1527 _reflns_number_total 1568 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.938 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.115 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0301 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.1938P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.0857 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2.a Aromatic/amide H refined with riding coordinates: N1(H1), N3(H3) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cs1 Cs 0.35823(6) 0.21684(4) 0.42123(3) 0.05360(15) Uani 1 1 d . . . S2 S 0.0363(3) 0.42020(17) 0.62874(11) 0.0505(3) Uani 1 1 d . . . N1 N 0.1162(8) 0.3623(5) 0.8640(3) 0.0403(7) Uani 1 1 d . . . H1 H 0.2749 0.4396 0.8762 0.048 Uiso 1 1 calc R . . N2 N -0.3104(8) 0.1938(5) 0.7200(3) 0.0428(8) Uani 1 1 d . . . C5 C -0.0641(10) 0.3164(6) 0.7432(4) 0.0389(8) Uani 1 1 d . . . N3 N -0.2032(8) 0.1767(5) 0.9391(4) 0.0420(8) Uani 1 1 d . . . H3 H -0.2566 0.1337 1.0009 0.050 Uiso 1 1 calc R . . C2 C -0.3849(9) 0.1258(6) 0.8179(4) 0.0397(8) Uani 1 1 d . . . C3 C 0.0556(10) 0.2915(5) 0.9648(4) 0.0388(8) Uani 1 1 d . . . S1 S -0.6938(2) -0.02491(15) 0.79807(11) 0.0459(3) Uani 1 1 d . . . S3 S 0.2821(2) 0.34134(16) 1.10875(10) 0.0490(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cs1 0.0461(2) 0.0635(2) 0.0428(2) 0.00197(13) 0.00473(13) 0.01017(14) S2 0.0467(6) 0.0650(7) 0.0341(5) 0.0168(5) 0.0090(4) 0.0034(5) N1 0.0354(18) 0.0464(18) 0.0333(16) 0.0100(14) 0.0062(14) 0.0025(15) N2 0.040(2) 0.0489(19) 0.0340(17) 0.0087(14) 0.0056(15) 0.0053(16) C5 0.037(2) 0.046(2) 0.0299(18) 0.0070(15) 0.0054(16) 0.0077(17) N3 0.0385(19) 0.0498(19) 0.0332(17) 0.0107(14) 0.0081(15) 0.0043(16) C2 0.035(2) 0.043(2) 0.038(2) 0.0064(16) 0.0071(16) 0.0084(17) C3 0.040(2) 0.0412(19) 0.0335(19) 0.0084(15) 0.0082(16) 0.0091(17) S1 0.0356(5) 0.0511(6) 0.0408(5) 0.0071(4) 0.0047(4) -0.0003(4) S3 0.0408(6) 0.0610(6) 0.0336(5) 0.0137(4) 0.0019(4) -0.0016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs1 Cs1 4.4036(7) 2_666 ? Cs1 S2 3.8680(13) 2_666 ? Cs1 S2 3.5625(14) . ? Cs1 S2 3.5443(13) 1_655 ? Cs1 S2 3.9336(14) 2_566 ? Cs1 N2 3.390(4) 2_556 ? Cs1 N2 3.365(4) 1_655 ? Cs1 C5 3.897(4) 1_655 ? Cs1 C2 3.618(4) 2_556 ? Cs1 S1 3.6599(13) 2_556 ? Cs1 S1 3.5329(12) 2_456 ? Cs1 S3 3.6288(11) 1_554 ? S2 Cs1 3.8680(12) 2_666 ? S2 Cs1 3.9336(14) 2_566 ? S2 Cs1 3.5442(13) 1_455 ? S2 C5 1.684(4) . ? N1 C5 1.377(5) . ? N1 C3 1.357(5) . ? N2 Cs1 3.390(4) 2_556 ? N2 Cs1 3.365(4) 1_455 ? N2 C5 1.339(6) . ? N2 C2 1.343(6) . ? C5 Cs1 3.897(4) 1_455 ? N3 C2 1.383(6) . ? N3 C3 1.356(6) . ? C2 Cs1 3.618(4) 2_556 ? C2 S1 1.682(5) . ? C3 S3 1.665(4) . ? S1 Cs1 3.6599(13) 2_556 ? S1 Cs1 3.5330(12) 2_456 ? S3 Cs1 3.6289(11) 1_556 ? 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 S2 Cs1 Cs1 49.93(2) 2_566 2_666 ? S2 Cs1 Cs1 56.93(2) . 2_666 ? S2 Cs1 Cs1 50.51(2) 2_666 2_666 ? S2 Cs1 Cs1 58.13(2) 1_655 2_666 ? S2 Cs1 S2 91.79(3) 1_655 . ? S2 Cs1 S2 50.96(3) 1_655 2_666 ? S2 Cs1 S2 108.06(2) 1_655 2_566 ? S2 Cs1 S2 50.28(3) . 2_566 ? S2 Cs1 S2 81.70(2) 2_666 2_566 ? S2 Cs1 S2 107.44(2) . 2_666 ? S2 Cs1 C5 79.47(7) . 1_655 ? S2 Cs1 C5 25.60(7) 1_655 1_655 ? S2 Cs1 C5 76.37(7) 2_666 1_655 ? S2 Cs1 C2 154.70(8) . 2_556 ? S2 Cs1 C2 110.32(7) 1_655 2_556 ? S2 Cs1 S1 88.01(3) 1_655 2_556 ? S2 Cs1 S1 177.54(3) . 2_556 ? S2 Cs1 S3 116.01(3) . 1_554 ? S2 Cs1 S3 112.39(3) 1_655 1_554 ? N2 Cs1 Cs1 82.02(7) 1_655 2_666 ? N2 Cs1 Cs1 164.32(7) 2_556 2_666 ? N2 Cs1 S2 138.17(7) 2_556 . ? N2 Cs1 S2 138.97(7) 2_556 2_566 ? N2 Cs1 S2 73.54(7) 1_655 . ? N2 Cs1 S2 114.20(7) 2_556 2_666 ? N2 Cs1 S2 118.77(7) 1_655 2_566 ? N2 Cs1 S2 45.04(7) 1_655 1_655 ? N2 Cs1 S2 95.90(7) 1_655 2_666 ? N2 Cs1 S2 111.04(7) 2_556 1_655 ? N2 Cs1 N2 97.82(8) 1_655 2_556 ? N2 Cs1 C5 19.54(10) 1_655 1_655 ? N2 Cs1 C5 106.10(9) 2_556 1_655 ? N2 Cs1 C2 113.28(10) 1_655 2_556 ? N2 Cs1 C2 21.79(9) 2_556 2_556 ? N2 Cs1 S1 107.92(7) 1_655 2_556 ? N2 Cs1 S1 69.25(7) 2_556 2_456 ? N2 Cs1 S1 43.97(7) 2_556 2_556 ? N2 Cs1 S1 137.91(7) 1_655 2_456 ? N2 Cs1 S3 157.23(7) 1_655 1_554 ? N2 Cs1 S3 87.90(6) 2_556 1_554 ? C5 Cs1 Cs1 69.22(6) 1_655 2_666 ? C5 Cs1 S2 114.54(7) 1_655 2_566 ? C2 Cs1 Cs1 145.87(7) 2_556 2_666 ? C2 Cs1 S2 127.86(7) 2_556 2_566 ? C2 Cs1 S2 96.30(7) 2_556 2_666 ? C2 Cs1 C5 115.44(9) 2_556 1_655 ? C2 Cs1 S1 26.72(7) 2_556 2_556 ? C2 Cs1 S3 67.64(7) 2_556 1_554 ? S1 Cs1 Cs1 120.93(2) 2_456 2_666 ? S1 Cs1 Cs1 121.07(2) 2_556 2_666 ? S1 Cs1 S2 127.52(3) 2_556 2_566 ? S1 Cs1 S2 126.12(3) 2_456 2_666 ? S1 Cs1 S2 177.04(2) 2_456 1_655 ? S1 Cs1 S2 89.73(3) 2_456 . ? S1 Cs1 S2 70.57(3) 2_556 2_666 ? S1 Cs1 S2 71.07(3) 2_456 2_566 ? S1 Cs1 C5 101.27(7) 2_556 1_655 ? S1 Cs1 C5 157.35(7) 2_456 1_655 ? S1 Cs1 C2 68.77(7) 2_456 2_556 ? S1 Cs1 S1 90.37(3) 2_456 2_556 ? S1 Cs1 S3 64.66(3) 2_456 1_554 ? S3 Cs1 Cs1 86.60(2) 1_554 2_666 ? S3 Cs1 S2 65.83(3) 1_554 2_566 ? S3 Cs1 S2 61.88(3) 1_554 2_666 ? S3 Cs1 C5 137.99(7) 1_554 1_655 ? S3 Cs1 S1 61.89(3) 1_554 2_556 ? Cs1 S2 Cs1 71.94(2) 1_455 2_566 ? Cs1 S2 Cs1 129.04(3) 1_455 2_666 ? Cs1 S2 Cs1 72.56(2) . 2_666 ? Cs1 S2 Cs1 81.70(2) 2_666 2_566 ? Cs1 S2 Cs1 129.72(3) . 2_566 ? Cs1 S2 Cs1 91.79(3) 1_455 . ? C5 S2 Cs1 107.98(16) . 2_566 ? C5 S2 Cs1 88.97(16) . 1_455 ? C5 S2 Cs1 119.24(16) . . ? C5 S2 Cs1 141.28(17) . 2_666 ? C3 N1 C5 123.1(4) . . ? Cs1 N2 Cs1 82.18(8) 1_455 2_556 ? C5 N2 Cs1 103.2(2) . 1_455 ? C5 N2 Cs1 117.7(3) . 2_556 ? C5 N2 C2 118.8(4) . . ? C2 N2 Cs1 88.7(3) . 2_556 ? C2 N2 Cs1 136.1(3) . 1_455 ? S2 C5 Cs1 65.43(14) . 1_455 ? N1 C5 Cs1 172.1(3) . 1_455 ? N1 C5 S2 117.7(3) . . ? N2 C5 Cs1 57.2(2) . 1_455 ? N2 C5 S2 122.2(3) . . ? N2 C5 N1 120.2(4) . . ? C3 N3 C2 122.9(4) . . ? N2 C2 Cs1 69.5(2) . 2_556 ? N2 C2 N3 120.0(4) . . ? N2 C2 S1 122.0(3) . . ? N3 C2 Cs1 124.1(3) . 2_556 ? N3 C2 S1 118.0(3) . . ? S1 C2 Cs1 78.03(15) . 2_556 ? N1 C3 S3 122.6(4) . . ? N3 C3 N1 114.8(4) . . ? N3 C3 S3 122.6(3) . . ? Cs1 S1 Cs1 90.37(3) 2_456 2_556 ? C2 S1 Cs1 75.26(15) . 2_556 ? C2 S1 Cs1 142.44(15) . 2_456 ? C3 S3 Cs1 140.46(16) . 1_556 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 5 -1 0.0271 -0.0025 4.9971 -1.0003 -0.2244 0.8505 0.4657 0 -5 1 0.0228 0.0025 -4.9971 1.0003 0.2244 -0.8505 -0.4657 0 0 -7 0.0114 0.0021 -0.0021 -6.9952 1.0080 0.1485 0.1402 0 0 7 0.0334 -0.0021 0.0021 6.9952 -1.0080 -0.1485 -0.1402 -3 4 1 0.0696 -3.0002 3.9964 1.0009 -0.0974 0.9251 -0.5251 3 -4 -1 0.0696 3.0002 -3.9964 -1.0009 0.0974 -0.9251 0.5251 _database_code_depnum_ccdc_archive 'CCDC 944681' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CsTTC2 _audit_creation_date 2013-06-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H4 Cs2 N6 S6' _chemical_formula_sum 'C6 H4 Cs2 N6 S6' _chemical_formula_weight 618.33 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Cs2 S6 C6 N6 H4' 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.7457 7.9052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x, -y, z+1/2' 3 'x+1/2, y+1/2, z' 4 'x+1/2, -y+1/2, z+1/2' _cell_length_a 5.41409(8) _cell_length_b 21.2829(3) _cell_length_c 14.9761(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.3402(13) _cell_angle_gamma 90.00 _cell_volume 1724.22(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10388 _cell_measurement_temperature 300.00(14) _cell_measurement_theta_max 71.1550 _cell_measurement_theta_min 4.1590 _exptl_absorpt_coefficient_mu 39.763 _exptl_absorpt_correction_T_max 0.470 _exptl_absorpt_correction_T_min 0.018 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear light orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.3237 _exptl_crystal_size_mid 0.1699 _exptl_crystal_size_min 0.0214 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13137 _diffrn_reflns_theta_full 69.9455 _diffrn_reflns_theta_max 71.15 _diffrn_reflns_theta_min 4.15 _diffrn_ambient_temperature 300.00(14) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.9994 _diffrn_measured_fraction_theta_max 0.8386 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 13.00 41.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 2 omega -25.00 6.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 0.0000 31 #__ type_ start__ end____ width___ exp.time_ 3 omega 8.00 62.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 60.0000 54 #__ type_ start__ end____ width___ exp.time_ 4 omega 36.00 62.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega 27.00 123.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -30.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega 33.00 112.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 150.0000 79 #__ type_ start__ end____ width___ exp.time_ 7 omega 75.00 121.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 54.7500 125.0000 60.0000 46 #__ type_ start__ end____ width___ exp.time_ 8 omega 57.00 96.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 54.7500 57.0000 90.0000 39 #__ type_ start__ end____ width___ exp.time_ 9 omega -46.00 3.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 37.0000 60.0000 49 #__ type_ start__ end____ width___ exp.time_ 10 omega -85.00 -3.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 63.0000 -120.0000 82 #__ type_ start__ end____ width___ exp.time_ 11 omega -141.00 -72.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -150.0000 69 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 68.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 13 omega 39.00 72.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 120.0000 33 #__ type_ start__ end____ width___ exp.time_ 14 omega 39.00 72.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -60.0000 33 #__ type_ start__ end____ width___ exp.time_ 15 omega 80.00 124.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 90.0000 44 #__ type_ start__ end____ width___ exp.time_ 16 omega 40.00 67.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 17 omega 40.00 71.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -90.0000 31 #__ type_ start__ end____ width___ exp.time_ 18 omega 41.00 81.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -30.0000 40 #__ type_ start__ end____ width___ exp.time_ 19 omega 84.00 110.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 20 omega 41.00 107.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 150.0000 66 #__ type_ start__ end____ width___ exp.time_ 21 omega 42.00 78.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -120.0000 36 #__ type_ start__ end____ width___ exp.time_ 22 omega 79.00 107.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 23 omega 43.00 69.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 24 omega 39.00 64.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 25 omega 45.00 143.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -150.0000 98 #__ type_ start__ end____ width___ exp.time_ 26 omega 39.00 72.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 90.0000 33 #__ type_ start__ end____ width___ exp.time_ 27 omega 150.00 176.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 28 omega 38.00 71.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 60.0000 33 #__ type_ start__ end____ width___ exp.time_ 29 omega 63.00 99.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -12.0000 -60.0000 36 #__ type_ start__ end____ width___ exp.time_ 30 omega 134.00 177.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -12.0000 -60.0000 43 #__ type_ start__ end____ width___ exp.time_ 31 omega 42.00 68.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 32 omega 88.00 114.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 25.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 33 omega 109.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 0.0000 69 #__ type_ start__ end____ width___ exp.time_ 34 omega 50.00 75.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 35 omega 52.00 77.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 36 omega 102.00 129.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 37 omega 88.00 115.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 38 omega 146.00 172.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 39 omega 50.00 95.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 -30.0000 45 #__ type_ start__ end____ width___ exp.time_ 40 omega 100.00 138.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 -30.0000 38 #__ type_ start__ end____ width___ exp.time_ 41 omega 42.00 71.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -120.0000 29 #__ type_ start__ end____ width___ exp.time_ 42 omega 101.00 146.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -120.0000 45 #__ type_ start__ end____ width___ exp.time_ 43 omega 42.00 71.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 -180.0000 29 #__ type_ start__ end____ width___ exp.time_ 44 omega 39.00 70.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 0.0000 31 #__ type_ start__ end____ width___ exp.time_ 45 omega 39.00 64.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 46 omega 50.00 108.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 60.0000 58 #__ type_ start__ end____ width___ exp.time_ 47 omega 69.00 95.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 108.2968 26 #__ type_ start__ end____ width___ exp.time_ 48 omega -26.00 72.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 37.0000 -60.0000 98 #__ type_ start__ end____ width___ exp.time_ 49 omega -25.00 42.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 120.0000 67 #__ type_ start__ end____ width___ exp.time_ 50 omega -25.00 42.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 -150.0000 67 #__ type_ start__ end____ width___ exp.time_ 51 omega -112.00 -18.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -54.7500 125.0000 0.0000 94 #__ type_ start__ end____ width___ exp.time_ 52 omega 25.00 125.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -180.0000 100 #__ type_ start__ end____ width___ exp.time_ 53 omega 75.00 126.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 121.0000 -122.0000 51 #__ type_ start__ end____ width___ exp.time_ 54 omega 25.00 125.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 30.0000 100 #__ type_ start__ end____ width___ exp.time_ 55 omega 25.00 125.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 56 omega 25.00 125.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 77.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 57 omega 84.00 109.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 58 omega 88.00 178.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 90.0000 90 #__ type_ start__ end____ width___ exp.time_ 59 omega 84.00 178.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 37.0000 30.0000 94 #__ type_ start__ end____ width___ exp.time_ 60 omega 38.00 178.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 12.0000 -120.0000 140 #__ type_ start__ end____ width___ exp.time_ 61 omega 32.00 57.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 62 omega 100.00 125.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 54.7500 155.0000 37.0000 25 #__ type_ start__ end____ width___ exp.time_ 63 omega 91.00 117.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 64 omega 37.00 62.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -25.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 65 omega 39.00 64.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -50.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 66 omega 43.00 68.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -37.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 67 omega 45.00 71.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 68 omega 47.00 73.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -111.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 69 omega 39.00 65.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 0.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 70 omega 113.00 149.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 0.0000 -180.0000 36 #__ type_ start__ end____ width___ exp.time_ 71 omega 153.00 178.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 77.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 72 omega 66.00 116.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -63.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 73 omega 56.00 95.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -30.0000 39 #__ type_ start__ end____ width___ exp.time_ 74 omega 106.00 141.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 -134.8294 35 #__ type_ start__ end____ width___ exp.time_ 75 omega 109.00 142.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -60.0000 33 #__ type_ start__ end____ width___ exp.time_ 76 omega 152.00 177.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 63.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 77 omega 91.00 126.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 50.0000 -30.0000 35 #__ type_ start__ end____ width___ exp.time_ 78 omega 54.00 80.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 155.0000 37.0000 26 #__ type_ start__ end____ width___ exp.time_ 79 omega 78.00 104.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -91.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 80 omega 96.00 141.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 109.5000 -93.0000 13.8441 45 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0432566000 _diffrn_orient_matrix_UB_12 -0.0678753000 _diffrn_orient_matrix_UB_13 0.0328178000 _diffrn_orient_matrix_UB_21 -0.2005517000 _diffrn_orient_matrix_UB_22 -0.0235008000 _diffrn_orient_matrix_UB_23 -0.0679250000 _diffrn_orient_matrix_UB_31 0.1975404000 _diffrn_orient_matrix_UB_32 -0.0089928000 _diffrn_orient_matrix_UB_33 -0.0700435000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2796 _reflns_number_total 2824 _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 69.95 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.633 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.205 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(5) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2824 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0460 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1207 _refine_ls_wR_factor_ref 0.1236 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups 2.a Aromatic/amide H refined with riding coordinates: N6(H6), N7(H7), N8(H8), N9(H9) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C1 C 1.7343(17) -0.2685(4) -0.3049(5) 0.0528(17) Uani 1 1 d . . . C6 C 0.9070(14) -0.4561(3) -0.0077(4) 0.0450(13) Uani 1 1 d . . . C7 C 1.1797(15) -0.4042(3) -0.0952(5) 0.0479(14) Uani 1 1 d . . . C8 C 1.7465(13) -0.1558(3) -0.3012(5) 0.0462(14) Uani 1 1 d . . . C9 C 1.4804(15) -0.2061(4) -0.2120(6) 0.0513(15) Uani 1 1 d . . . C14 C 0.9029(16) -0.3429(3) -0.0098(5) 0.0505(15) Uani 1 1 d . . . N3 N 1.5792(13) -0.1534(3) -0.2393(4) 0.0514(13) Uani 1 1 d . . . N6 N 0.8157(12) -0.3992(3) 0.0186(4) 0.0457(11) Uani 1 1 d . . . H6 H 0.6970 -0.3990 0.0550 0.055 Uiso 1 1 calc R . . N7 N 1.5553(16) -0.2633(3) -0.2454(5) 0.0584(15) Uani 1 1 d . . . H7 H 1.4848 -0.2969 -0.2274 0.070 Uiso 1 1 calc R . . N8 N 1.0895(14) -0.3474(3) -0.0663(5) 0.0513(13) Uani 1 1 d . . . H8 H 1.1553 -0.3134 -0.0851 0.062 Uiso 1 1 calc R . . N9 N 1.8253(13) -0.2120(3) -0.3327(5) 0.0515(13) Uani 1 1 d . . . H9 H 1.9373 -0.2121 -0.3718 0.062 Uiso 1 1 calc R . . N10 N 1.0919(13) -0.4581(3) -0.0641(4) 0.0487(12) Uani 1 1 d . . . S1 S 1.8636(4) -0.08899(8) -0.34535(14) 0.0531(4) Uani 1 1 d . . . S2 S 1.4001(4) -0.40269(9) -0.17249(16) 0.0597(4) Uani 1 1 d . . . S3 S 1.2575(4) -0.20699(9) -0.13576(15) 0.0578(4) Uani 1 1 d . . . S4 S 0.7788(4) -0.52200(8) 0.03093(16) 0.0575(4) Uani 1 1 d . . . S5 S 1.8299(6) -0.33710(10) -0.3448(2) 0.0779(7) Uani 1 1 d . . . S11 S 0.7824(5) -0.27566(9) 0.02312(17) 0.0643(5) Uani 1 1 d . . . Cs1 Cs 0.86302(7) -0.51206(2) -0.24038(4) 0.06049(18) Uani 1 1 d . . . Cs2 Cs 0.77855(9) -0.11470(2) -0.02780(5) 0.06626(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.065(5) 0.044(3) 0.051(3) 0.004(3) 0.021(3) 0.002(3) C6 0.051(3) 0.043(3) 0.042(3) 0.002(2) 0.004(2) 0.006(3) C7 0.055(4) 0.045(3) 0.044(3) -0.001(3) 0.007(3) 0.008(3) C8 0.050(4) 0.040(3) 0.049(3) -0.002(2) 0.006(3) -0.001(2) C9 0.055(4) 0.045(3) 0.056(4) -0.002(3) 0.016(3) 0.002(3) C14 0.057(4) 0.038(3) 0.057(4) 0.001(3) 0.010(3) 0.004(3) N3 0.058(4) 0.037(2) 0.060(3) -0.004(2) 0.014(3) 0.004(2) N6 0.049(3) 0.037(2) 0.051(3) 0.003(2) 0.011(2) 0.003(2) N7 0.075(5) 0.036(2) 0.065(4) 0.001(2) 0.028(3) -0.001(3) N8 0.061(4) 0.038(3) 0.056(3) 0.000(2) 0.012(3) -0.002(2) N9 0.053(3) 0.044(3) 0.058(3) 0.000(2) 0.017(3) -0.003(2) N10 0.057(3) 0.039(2) 0.051(3) -0.009(2) 0.009(2) -0.001(2) S1 0.0539(10) 0.0415(8) 0.0651(10) -0.0003(7) 0.0173(8) -0.0022(6) S2 0.0664(12) 0.0482(8) 0.0664(10) -0.0006(8) 0.0274(9) 0.0040(8) S3 0.0620(11) 0.0479(8) 0.0656(10) -0.0010(8) 0.0276(8) 0.0026(7) S4 0.0642(11) 0.0386(7) 0.0707(11) 0.0006(7) 0.0153(9) -0.0057(7) S5 0.104(2) 0.0422(8) 0.0916(15) -0.0056(9) 0.0510(14) 0.0054(10) S11 0.0762(13) 0.0384(8) 0.0809(12) 0.0021(8) 0.0362(10) 0.0078(8) Cs1 0.0608(3) 0.0615(3) 0.0592(3) -0.0133(2) 0.0022(2) 0.0076(2) Cs2 0.0587(3) 0.0510(2) 0.0897(4) -0.0065(2) 0.0103(2) 0.00009(19) _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 C1 N7 1.348(12) . ? C1 N9 1.370(10) . ? C1 S5 1.668(8) . ? C6 N6 1.373(9) . ? C6 N10 1.336(11) . ? C6 S4 1.678(7) . ? C6 Cs1 3.681(7) . ? C7 N8 1.380(10) . ? C7 N10 1.334(10) . ? C7 S2 1.696(8) . ? C7 Cs1 3.554(7) . ? C8 N3 1.323(11) . ? C8 N9 1.361(10) . ? C8 S1 1.702(7) . ? C8 Cs1 3.828(7) 3 ? C9 N3 1.315(10) . ? C9 N7 1.382(10) . ? C9 S3 1.695(8) . ? C9 Cs2 3.693(8) 1_655 ? C14 N6 1.362(9) . ? C14 N8 1.348(12) . ? C14 S11 1.655(7) . ? N3 Cs1 3.228(6) 3 ? N3 Cs2 3.406(7) 1_655 ? N10 Cs1 3.091(6) . ? N10 Cs2 3.518(6) 3_545 ? S1 Cs1 3.584(2) 3 ? S1 Cs1 3.481(2) 3_655 ? S2 Cs1 3.830(2) . ? S2 Cs1 3.597(2) 1_655 ? S3 Cs2 3.749(2) 1_655 ? S3 Cs2 3.679(2) . ? S4 Cs1 3.512(2) 2_545 ? S4 Cs1 4.113(2) . ? S4 Cs2 3.436(2) 3_445 ? S4 Cs2 3.490(2) 3_545 ? S5 Cs1 4.040(2) 1_655 ? S5 Cs2 4.099(4) 4_544 ? S5 Cs2 3.874(3) 4_644 ? S11 Cs2 3.509(2) . ? Cs1 C8 3.828(7) 3_445 ? Cs1 N3 3.228(6) 3_445 ? Cs1 S1 3.584(2) 3_445 ? Cs1 S1 3.481(2) 3_345 ? Cs1 S2 3.597(2) 1_455 ? Cs1 S4 3.512(2) 2_544 ? Cs1 S5 4.040(2) 1_455 ? Cs2 C9 3.693(8) 1_455 ? Cs2 N3 3.406(7) 1_455 ? Cs2 N10 3.518(6) 3_455 ? Cs2 S3 3.749(2) 1_455 ? Cs2 S4 3.436(2) 3 ? Cs2 S4 3.490(2) 3_455 ? Cs2 S5 4.099(4) 4_445 ? Cs2 S5 3.874(3) 4_345 ? Cs2 Cs1 5.0738(9) 3 ? Cs2 Cs1 4.4027(8) 3_455 ? 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 C1 N9 113.9(7) . . ? N7 C1 S5 123.5(6) . . ? N9 C1 S5 122.5(6) . . ? N6 C6 S4 118.7(6) . . ? N6 C6 Cs1 123.2(4) . . ? N10 C6 N6 119.8(6) . . ? N10 C6 S4 121.5(5) . . ? N10 C6 Cs1 54.0(3) . . ? S4 C6 Cs1 92.5(3) . . ? N8 C7 S2 117.7(6) . . ? N8 C7 Cs1 126.1(5) . . ? N10 C7 N8 120.6(7) . . ? N10 C7 S2 121.7(6) . . ? N10 C7 Cs1 59.2(4) . . ? S2 C7 Cs1 86.0(3) . . ? N3 C8 N9 120.6(7) . . ? N3 C8 S1 121.1(5) . . ? N3 C8 Cs1 53.8(4) . 3 ? N9 C8 S1 118.2(6) . . ? N9 C8 Cs1 165.0(5) . 3 ? S1 C8 Cs1 68.8(2) . 3 ? N3 C9 N7 120.6(7) . . ? N3 C9 S3 121.9(6) . . ? N3 C9 Cs2 67.2(4) . 1_655 ? N7 C9 S3 117.5(6) . . ? N7 C9 Cs2 127.4(6) . 1_655 ? S3 C9 Cs2 78.7(3) . 1_655 ? N6 C14 S11 121.4(6) . . ? N8 C14 N6 114.3(6) . . ? N8 C14 S11 124.3(6) . . ? C8 N3 Cs1 106.9(5) . 3 ? C8 N3 Cs2 117.4(5) . 1_655 ? C9 N3 C8 119.0(6) . . ? C9 N3 Cs1 130.1(5) . 3 ? C9 N3 Cs2 92.0(5) . 1_655 ? Cs1 N3 Cs2 83.11(14) 3 1_655 ? C14 N6 C6 123.6(7) . . ? C1 N7 C9 122.8(7) . . ? C14 N8 C7 122.9(7) . . ? C8 N9 C1 123.0(7) . . ? C6 N10 Cs1 105.5(4) . . ? C6 N10 Cs2 98.7(4) . 3_545 ? C7 N10 C6 118.7(6) . . ? C7 N10 Cs1 99.1(4) . . ? C7 N10 Cs2 139.9(5) . 3_545 ? Cs1 N10 Cs2 83.28(13) . 3_545 ? C8 S1 Cs1 84.9(3) . 3 ? C8 S1 Cs1 120.8(2) . 3_655 ? Cs1 S1 Cs1 100.04(5) 3_655 3 ? C7 S2 Cs1 67.8(3) . . ? C7 S2 Cs1 134.3(3) . 1_655 ? Cs1 S2 Cs1 93.55(5) 1_655 . ? C9 S3 Cs2 145.5(3) . . ? C9 S3 Cs2 75.0(3) . 1_655 ? Cs2 S3 Cs2 93.57(5) . 1_655 ? C6 S4 Cs1 63.4(2) . . ? C6 S4 Cs1 97.2(2) . 2_545 ? C6 S4 Cs2 136.4(2) . 3_445 ? C6 S4 Cs2 92.8(3) . 3_545 ? Cs1 S4 Cs1 159.65(6) 2_545 . ? Cs2 S4 Cs1 83.95(5) 3_445 . ? Cs2 S4 Cs1 70.23(4) 3_545 . ? Cs2 S4 Cs1 106.94(6) 3_545 2_545 ? Cs2 S4 Cs1 115.95(7) 3_445 2_545 ? Cs2 S4 Cs2 102.83(5) 3_445 3_545 ? C1 S5 Cs1 132.6(3) . 1_655 ? C1 S5 Cs2 103.3(3) . 4_544 ? C1 S5 Cs2 134.3(3) . 4_644 ? Cs1 S5 Cs2 92.74(6) 1_655 4_544 ? Cs2 S5 Cs1 90.61(5) 4_644 1_655 ? Cs2 S5 Cs2 85.50(6) 4_644 4_544 ? C14 S11 Cs2 141.0(3) . . ? C6 Cs1 C8 117.97(14) . 3_445 ? C6 Cs1 S2 62.16(13) . . ? C6 Cs1 S4 24.05(11) . . ? C6 Cs1 S5 93.94(11) . 1_455 ? C7 Cs1 C6 36.97(18) . . ? C7 Cs1 C8 114.14(15) . 3_445 ? C7 Cs1 S1 102.06(13) . 3_445 ? C7 Cs1 S2 74.54(13) . 1_455 ? C7 Cs1 S2 26.23(14) . . ? C7 Cs1 S4 59.93(13) . . ? C7 Cs1 S5 69.78(13) . 1_455 ? C8 Cs1 S2 97.79(11) 3_445 . ? C8 Cs1 S4 106.08(11) 3_445 . ? C8 Cs1 S5 131.33(12) 3_445 1_455 ? N3 Cs1 C6 106.70(15) 3_445 . ? N3 Cs1 C7 115.67(17) 3_445 . ? N3 Cs1 C8 19.31(18) 3_445 3_445 ? N3 Cs1 S1 45.24(14) 3_445 3_445 ? N3 Cs1 S1 80.71(13) 3_445 3_345 ? N3 Cs1 S2 107.09(14) 3_445 . ? N3 Cs1 S2 149.13(14) 3_445 1_455 ? N3 Cs1 S4 103.28(12) 3_445 2_544 ? N3 Cs1 S4 90.11(13) 3_445 . ? N3 Cs1 S5 150.61(14) 3_445 1_455 ? N10 Cs1 C6 20.47(18) . . ? N10 Cs1 C7 21.75(17) . . ? N10 Cs1 C8 107.31(16) . 3_445 ? N10 Cs1 N3 102.07(17) . 3_445 ? N10 Cs1 S1 105.09(13) . 3_445 ? N10 Cs1 S1 146.85(14) . 3_345 ? N10 Cs1 S2 43.46(14) . . ? N10 Cs1 S2 77.17(13) . 1_455 ? N10 Cs1 S4 141.98(13) . 2_544 ? N10 Cs1 S4 39.82(13) . . ? N10 Cs1 S5 89.91(12) . 1_455 ? S1 Cs1 C6 126.78(13) 3_345 . ? S1 Cs1 C6 122.83(12) 3_445 . ? S1 Cs1 C7 157.90(13) 3_345 . ? S1 Cs1 C8 86.30(11) 3_345 3_445 ? S1 Cs1 C8 26.28(11) 3_445 3_445 ? S1 Cs1 S1 100.04(5) 3_345 3_445 ? S1 Cs1 S2 83.96(5) 3_345 1_455 ? S1 Cs1 S2 79.31(5) 3_445 . ? S1 Cs1 S2 165.38(5) 3_445 1_455 ? S1 Cs1 S2 166.71(5) 3_345 . ? S1 Cs1 S4 65.74(5) 3_345 2_544 ? S1 Cs1 S4 107.86(5) 3_345 . ? S1 Cs1 S4 121.74(5) 3_445 . ? S1 Cs1 S5 105.88(5) 3_445 1_455 ? S1 Cs1 S5 103.73(6) 3_345 1_455 ? S2 Cs1 C6 62.75(11) 1_455 . ? S2 Cs1 C8 167.22(12) 1_455 3_445 ? S2 Cs1 S2 93.55(5) 1_455 . ? S2 Cs1 S4 83.26(5) . . ? S2 Cs1 S4 69.36(5) 1_455 . ? S2 Cs1 S5 59.51(5) 1_455 1_455 ? S2 Cs1 S5 64.14(6) . 1_455 ? S4 Cs1 C6 149.01(11) 2_544 . ? S4 Cs1 C7 120.23(13) 2_544 . ? S4 Cs1 C8 89.02(11) 2_544 3_445 ? S4 Cs1 S1 74.75(5) 2_544 3_445 ? S4 Cs1 S2 101.56(5) 2_544 . ? S4 Cs1 S2 94.47(5) 2_544 1_455 ? S4 Cs1 S4 163.50(6) 2_544 . ? S4 Cs1 S5 55.27(6) 2_544 1_455 ? S5 Cs1 S4 115.15(5) 1_455 . ? C9 Cs2 S3 26.31(13) 1_455 1_455 ? C9 Cs2 S5 130.67(12) 1_455 4_445 ? C9 Cs2 S5 96.96(14) 1_455 4_345 ? C9 Cs2 Cs1 91.31(13) 1_455 3 ? C9 Cs2 Cs1 61.73(12) 1_455 3_455 ? N3 Cs2 C9 20.85(17) 1_455 1_455 ? N3 Cs2 N10 90.42(14) 1_455 3_455 ? N3 Cs2 S3 70.39(12) 1_455 . ? N3 Cs2 S3 42.93(13) 1_455 1_455 ? N3 Cs2 S4 98.73(12) 1_455 3_455 ? N3 Cs2 S4 126.41(13) 1_455 3 ? N3 Cs2 S5 139.08(11) 1_455 4_445 ? N3 Cs2 S5 114.19(14) 1_455 4_345 ? N3 Cs2 S11 87.98(12) 1_455 . ? N3 Cs2 Cs1 46.71(10) 1_455 3_455 ? N3 Cs2 Cs1 72.70(13) 1_455 3 ? N10 Cs2 C9 105.63(15) 3_455 1_455 ? N10 Cs2 S3 102.89(11) 3_455 1_455 ? N10 Cs2 S3 129.86(12) 3_455 . ? N10 Cs2 S5 122.49(10) 3_455 4_445 ? N10 Cs2 S5 100.11(12) 3_455 4_345 ? N10 Cs2 Cs1 71.21(12) 3_455 3 ? N10 Cs2 Cs1 44.21(10) 3_455 3_455 ? S3 Cs2 C9 71.63(13) . 1_455 ? S3 Cs2 S3 93.57(5) . 1_455 ? S3 Cs2 S5 71.56(6) 1_455 4_345 ? S3 Cs2 S5 130.02(5) . 4_345 ? S3 Cs2 S5 69.70(5) . 4_445 ? S3 Cs2 S5 132.20(5) 1_455 4_445 ? S3 Cs2 Cs1 59.03(3) . 3 ? S3 Cs2 Cs1 107.19(4) . 3_455 ? S3 Cs2 Cs1 66.10(3) 1_455 3_455 ? S3 Cs2 Cs1 115.63(4) 1_455 3 ? S4 Cs2 C9 144.06(13) 3 1_455 ? S4 Cs2 C9 99.58(13) 3_455 1_455 ? S4 Cs2 N10 44.17(12) 3_455 3_455 ? S4 Cs2 N10 73.39(11) 3 3_455 ? S4 Cs2 S3 80.06(5) 3_455 1_455 ? S4 Cs2 S3 169.26(6) 3 1_455 ? S4 Cs2 S3 81.76(5) 3 . ? S4 Cs2 S3 168.52(6) 3_455 . ? S4 Cs2 S4 102.82(5) 3 3_455 ? S4 Cs2 S5 55.09(5) 3 4_445 ? S4 Cs2 S5 57.07(6) 3_455 4_345 ? S4 Cs2 S5 118.79(7) 3 4_345 ? S4 Cs2 S5 121.59(6) 3_455 4_445 ? S4 Cs2 S11 119.66(5) 3_455 . ? S4 Cs2 S11 120.48(6) 3 . ? S4 Cs2 Cs1 53.71(4) 3 3 ? S4 Cs2 Cs1 115.12(4) 3_455 3 ? S4 Cs2 Cs1 105.92(4) 3 3_455 ? S4 Cs2 Cs1 61.53(4) 3_455 3_455 ? S5 Cs2 S5 85.50(6) 4_345 4_445 ? S5 Cs2 Cs1 169.44(4) 4_345 3 ? S5 Cs2 Cs1 94.09(4) 4_445 3 ? S5 Cs2 Cs1 109.04(6) 4_345 3_455 ? S5 Cs2 Cs1 160.77(3) 4_445 3_455 ? S11 Cs2 C9 69.31(13) . 1_455 ? S11 Cs2 N10 163.20(12) . 3_455 ? S11 Cs2 S3 65.17(6) . 1_455 ? S11 Cs2 S3 64.94(5) . . ? S11 Cs2 S5 67.21(6) . 4_445 ? S11 Cs2 S5 65.55(5) . 4_345 ? S11 Cs2 Cs1 123.94(4) . 3 ? S11 Cs2 Cs1 129.78(5) . 3_455 ? Cs1 Cs2 Cs1 69.268(12) 3_455 3 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 -14 1 0.0204 0.0041 -13.9985 1.0071 0.9834 0.2598 0.0562 3 -1 1 0.1211 3.0002 -0.9874 1.0025 0.2297 -0.6466 0.5313 3 -2 -7 0.1263 2.9985 -1.9980 -6.9965 0.0357 -0.0792 1.1003 -1 -1 -9 0.0852 -1.0018 -1.0156 -8.9995 -0.2697 0.8361 0.4416 -2 -1 -7 0.0706 -2.0012 -1.0167 -7.0004 -0.2473 0.9007 0.1041 2 1 7 0.1056 2.0012 1.0167 7.0004 0.2473 -0.9007 -0.1041 0 2 10 0.0581 0.0019 2.0132 9.9983 0.1916 -0.7268 -0.7180 0 14 -1 0.0010 -0.0041 13.9985 -1.0071 -0.9834 -0.2598 -0.0562 _database_code_depnum_ccdc_archive 'CCDC 944682'