Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'J. Reglinski' _publ_contact_author_address ; Department of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email J.REGLINSKI@STRATH.AC.UK _publ_section_title ; The first bona-fide sodium complex of hydrotris(methimazolyl)borate: An example of sodium exhibiting a preference for sulfur over oxygen. ; _publ_requested_category FM loop_ _publ_author_name 'J Reglinski' 'Anne Biernat' 'Matthias Schwalbe' 'Mark Spicer' 'Dawn Wallace' data_ann2 _database_code_depnum_ccdc_archive 'CCDC 635366' _audit_creation_date 2006-08-04T10:56:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'NaTm from DMF/Et2O' _chemical_formula_moiety 'C27 H52 B2 N13 Na2 O7.50 S6' _chemical_formula_sum 'C27 H52 B2 N13 Na2 O7.50 S6' _chemical_formula_weight 938.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.664(5) _cell_length_b 14.087(5) _cell_length_c 15.255(5) _cell_angle_alpha 73.545(5) _cell_angle_beta 70.608(5) _cell_angle_gamma 78.101(5) _cell_volume 2250.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9542 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.38 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.88216E-2 _diffrn_orient_matrix_ub_12 -0.383294E-1 _diffrn_orient_matrix_ub_13 -0.484101E-1 _diffrn_orient_matrix_ub_21 -0.772605E-1 _diffrn_orient_matrix_ub_22 -0.291204E-1 _diffrn_orient_matrix_ub_23 0.403103E-1 _diffrn_orient_matrix_ub_31 -0.484101E-1 _diffrn_orient_matrix_ub_32 0.569869E-1 _diffrn_orient_matrix_ub_33 -0.337307E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_number 19385 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 10271 _reflns_number_gt 8037 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.5824P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10271 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.439 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.70684(13) 0.48077(11) 0.76319(10) 0.0216(3) Uani 1 1 d . . . C2 C 0.51229(15) 0.54815(12) 0.81035(11) 0.0288(3) Uani 1 1 d . . . H2 H 0.4253 0.5559 0.8310 0.035 Uiso 1 1 calc R . . C3 C 0.58343(16) 0.61912(13) 0.79362(12) 0.0339(4) Uani 1 1 d . . . H3 H 0.5561 0.6858 0.8003 0.041 Uiso 1 1 calc R . . C4 C 0.81093(17) 0.62955(14) 0.73569(14) 0.0403(4) Uani 1 1 d . . . H4A H 0.8826 0.5814 0.7435 0.060 Uiso 1 1 calc R . . H4B H 0.7961 0.6772 0.7755 0.060 Uiso 1 1 calc R . . H4C H 0.8260 0.6655 0.6685 0.060 Uiso 1 1 calc R . . C5 C 0.60952(13) 0.18630(11) 0.90158(10) 0.0220(3) Uani 1 1 d . . . C6 C 0.58080(14) 0.31168(12) 0.97152(11) 0.0252(3) Uani 1 1 d . . . H6 H 0.5626 0.3770 0.9825 0.030 Uiso 1 1 calc R . . C7 C 0.61345(14) 0.22768(12) 1.03176(11) 0.0257(3) Uani 1 1 d . . . H7 H 0.6225 0.2229 1.0926 0.031 Uiso 1 1 calc R . . C8 C 0.66735(17) 0.04560(12) 1.02841(12) 0.0357(4) Uani 1 1 d . . . H8A H 0.5986 0.0075 1.0449 0.054 Uiso 1 1 calc R . . H8B H 0.6904 0.0401 1.0860 0.054 Uiso 1 1 calc R . . H8C H 0.7373 0.0190 0.9813 0.054 Uiso 1 1 calc R . . C9 C 0.35584(13) 0.40651(11) 0.74511(11) 0.0222(3) Uani 1 1 d . . . C10 C 0.32112(14) 0.33502(12) 0.89951(11) 0.0292(4) Uani 1 1 d . . . H10 H 0.3337 0.3055 0.9604 0.035 Uiso 1 1 calc R . . C11 C 0.21378(14) 0.34974(13) 0.87936(12) 0.0326(4) Uani 1 1 d . . . H11 H 0.1371 0.3334 0.9233 0.039 Uiso 1 1 calc R . . C12 C 0.14550(15) 0.42084(14) 0.73072(13) 0.0354(4) Uani 1 1 d . . . H12A H 0.1464 0.4912 0.6969 0.053 Uiso 1 1 calc R . . H12B H 0.0639 0.4107 0.7754 0.053 Uiso 1 1 calc R . . H12C H 0.1654 0.3795 0.6844 0.053 Uiso 1 1 calc R . . C13 C 0.81760(13) 0.01065(11) 0.23595(10) 0.0226(3) Uani 1 1 d . . . C14 C 1.01563(14) -0.05025(12) 0.20141(11) 0.0281(3) Uani 1 1 d . . . H14 H 1.1021 -0.0543 0.1858 0.034 Uiso 1 1 calc R . . C15 C 0.95243(16) -0.12562(13) 0.21585(12) 0.0339(4) Uani 1 1 d . . . H15 H 0.9856 -0.1925 0.2127 0.041 Uiso 1 1 calc R . . C16 C 0.72819(18) -0.14333(14) 0.25532(14) 0.0407(4) Uani 1 1 d . . . H16A H 0.6503 -0.1005 0.2717 0.061 Uiso 1 1 calc R . . H16B H 0.7305 -0.2013 0.3088 0.061 Uiso 1 1 calc R . . H16C H 0.7357 -0.1659 0.1983 0.061 Uiso 1 1 calc R . . C17 C 0.90330(13) 0.30987(11) 0.09980(10) 0.0227(3) Uani 1 1 d . . . C18 C 0.93604(14) 0.18175(12) 0.03277(10) 0.0251(3) Uani 1 1 d . . . H18 H 0.9564 0.1159 0.0230 0.030 Uiso 1 1 calc R . . C19 C 0.90094(14) 0.26368(12) -0.02842(11) 0.0261(3) Uani 1 1 d . . . H19 H 0.8919 0.2663 -0.0887 0.031 Uiso 1 1 calc R . . C20 C 0.84072(16) 0.44607(13) -0.02792(12) 0.0345(4) Uani 1 1 d . . . H20A H 0.7707 0.4725 0.0193 0.052 Uiso 1 1 calc R . . H20B H 0.8166 0.4490 -0.0844 0.052 Uiso 1 1 calc R . . H20C H 0.9081 0.4861 -0.0464 0.052 Uiso 1 1 calc R . . C21 C 1.14698(13) 0.09934(11) 0.27149(10) 0.0221(3) Uani 1 1 d . . . C22 C 1.19211(14) 0.16252(12) 0.11482(11) 0.0265(3) Uani 1 1 d . . . H22 H 1.1836 0.1897 0.0524 0.032 Uiso 1 1 calc R . . C23 C 1.29725(14) 0.14522(12) 0.13845(11) 0.0289(4) Uani 1 1 d . . . H23 H 1.3762 0.1575 0.0961 0.035 Uiso 1 1 calc R . . C24 C 1.35587(15) 0.07530(14) 0.29119(13) 0.0367(4) Uani 1 1 d . . . H24A H 1.3460 0.1242 0.3286 0.055 Uiso 1 1 calc R . . H24B H 1.4394 0.0709 0.2479 0.055 Uiso 1 1 calc R . . H24C H 1.3408 0.0099 0.3344 0.055 Uiso 1 1 calc R . . C25 C 1.41009(16) 0.14378(15) 0.48600(14) 0.0439(5) Uani 1 1 d . . . H25A H 1.3748 0.0810 0.5053 0.066 Uiso 1 1 calc R . . H25B H 1.4566 0.1430 0.5293 0.066 Uiso 1 1 calc R . . H25C H 1.4648 0.1515 0.4205 0.066 Uiso 1 1 calc R . . C26 C 1.34706(18) 0.32701(15) 0.46456(14) 0.0439(5) Uani 1 1 d . . . H26A H 1.2798 0.3760 0.4486 0.066 Uiso 1 1 calc R . . H26B H 1.4203 0.3328 0.4092 0.066 Uiso 1 1 calc R . . H26C H 1.3644 0.3396 0.5186 0.066 Uiso 1 1 calc R . . C27 C 1.19514(16) 0.21327(17) 0.52307(14) 0.0437(5) Uani 1 1 d . . . H27 H 1.1754 0.1471 0.5392 0.052 Uiso 1 1 calc R . . B1 B 0.55061(15) 0.35933(12) 0.80109(12) 0.0203(3) Uani 1 1 d . . . B2 B 0.96113(15) 0.14029(13) 0.20533(12) 0.0208(3) Uani 1 1 d . . . N1 N 0.58800(11) 0.46185(9) 0.79218(8) 0.0213(3) Uani 1 1 d . . . N2 N 0.70393(12) 0.57692(10) 0.76485(9) 0.0279(3) Uani 1 1 d . . . N3 N 0.57838(11) 0.28617(9) 0.89054(8) 0.0210(3) Uani 1 1 d . . . N4 N 0.63115(11) 0.15005(10) 0.98823(9) 0.0248(3) Uani 1 1 d . . . N5 N 0.41014(11) 0.37045(9) 0.81584(8) 0.0217(3) Uani 1 1 d . . . N6 N 0.23601(11) 0.39271(10) 0.78345(10) 0.0263(3) Uani 1 1 d . . . N7 N 0.93290(11) 0.03467(9) 0.21323(9) 0.0217(3) Uani 1 1 d . . . N8 N 0.82931(12) -0.08731(10) 0.23631(9) 0.0289(3) Uani 1 1 d . . . N9 N 0.93731(11) 0.21008(9) 0.11268(8) 0.0216(3) Uani 1 1 d . . . N10 N 0.88065(11) 0.34285(10) 0.01345(9) 0.0244(3) Uani 1 1 d . . . N11 N 1.09867(11) 0.13388(9) 0.19717(8) 0.0216(3) Uani 1 1 d . . . N12 N 1.26871(11) 0.10635(10) 0.23561(9) 0.0254(3) Uani 1 1 d . . . N13 N 1.31228(12) 0.22672(11) 0.49033(10) 0.0341(3) Uani 1 1 d . . . O1 O 0.53503(10) 0.22291(9) 0.62910(8) 0.0311(3) Uani 1 1 d . . . O2 O 0.65271(13) 0.29308(12) 0.36076(11) 0.0496(4) Uani 1 1 d . . . O3 O 0.74623(12) 0.07417(9) 0.46409(10) 0.0413(3) Uani 1 1 d . . . O4 O 0.71816(10) 0.40204(9) 0.52375(8) 0.0311(3) Uani 1 1 d . . . O5 O 0.82913(10) 0.18461(9) 0.61665(8) 0.0321(3) Uani 1 1 d . . . O6 O 0.92350(10) 0.27838(9) 0.39763(8) 0.0303(3) Uani 1 1 d . . . O7 O 0.9864(4) 0.5035(3) 0.4698(2) 0.0748(13) Uani 0.50 1 d P . . O8 O 1.10967(12) 0.28172(13) 0.53398(11) 0.0586(4) Uani 1 1 d . . . Na1 Na 0.71637(6) 0.23153(5) 0.49917(4) 0.02871(15) Uani 1 1 d . . . Na2 Na 0.91295(6) 0.33811(5) 0.53841(5) 0.03515(16) Uani 1 1 d . . . S1 S 0.83469(3) 0.39893(3) 0.73395(3) 0.02771(10) Uani 1 1 d . . . S2 S 0.61834(4) 0.11418(3) 0.82650(3) 0.03122(10) Uani 1 1 d . . . S3 S 0.42423(4) 0.46042(3) 0.62898(3) 0.02948(10) Uani 1 1 d . . . S4 S 0.68371(3) 0.08723(3) 0.26132(3) 0.02915(10) Uani 1 1 d . . . S5 S 0.89150(4) 0.38443(3) 0.17320(3) 0.03481(11) Uani 1 1 d . . . S6 S 1.07109(4) 0.05479(3) 0.38853(3) 0.02910(10) Uani 1 1 d . . . H1 H 0.5976 0.3332 0.7355 0.020(4) Uiso 1 1 d . . . H2B H 0.9004 0.1706 0.2658 0.026(4) Uiso 1 1 d . . . H1WA H 0.4991 0.2828 0.6333 0.066(8) Uiso 1 1 d . . . H1WB H 0.5536 0.2021 0.6835 0.055(6) Uiso 1 1 d . . . H2WA H 0.6974 0.2884 0.3101 0.121(13) Uiso 1 1 d . . . H2WB H 0.6365 0.3602 0.3474 0.123(13) Uiso 1 1 d . . . H3WA H 0.7336 0.0798 0.4041 0.111(11) Uiso 1 1 d . . . H3WB H 0.8196 0.0548 0.4551 0.093(10) Uiso 1 1 d . . . H4WA H 0.7032 0.4494 0.4744 0.047(6) Uiso 1 1 d . . . H4WB H 0.6553 0.4132 0.5737 0.078(8) Uiso 1 1 d . . . H5WA H 0.8745 0.1201 0.6149 0.064(7) Uiso 1 1 d . . . H5WB H 0.7818 0.1723 0.6775 0.091(9) Uiso 1 1 d . . . H6WA H 0.9237 0.3038 0.3401 0.056(7) Uiso 1 1 d . . . H6WB H 0.9739 0.2230 0.3957 0.075(8) Uiso 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 0.0223(7) 0.0260(8) 0.0172(7) -0.0028(6) -0.0063(6) -0.0066(6) C2 0.0264(8) 0.0249(8) 0.0314(8) -0.0081(7) -0.0034(7) -0.0015(7) C3 0.0381(9) 0.0235(9) 0.0370(9) -0.0108(7) -0.0047(7) -0.0024(7) C4 0.0431(10) 0.0359(10) 0.0465(11) -0.0048(8) -0.0134(9) -0.0207(8) C5 0.0200(7) 0.0241(8) 0.0198(7) -0.0020(6) -0.0049(6) -0.0038(6) C6 0.0262(8) 0.0282(9) 0.0236(8) -0.0093(6) -0.0078(6) -0.0033(6) C7 0.0259(8) 0.0324(9) 0.0207(7) -0.0068(6) -0.0090(6) -0.0030(7) C8 0.0454(10) 0.0270(9) 0.0306(9) 0.0011(7) -0.0159(8) 0.0016(8) C9 0.0207(7) 0.0197(8) 0.0270(8) -0.0065(6) -0.0083(6) -0.0007(6) C10 0.0245(8) 0.0297(9) 0.0267(8) 0.0008(7) -0.0036(6) -0.0060(7) C11 0.0204(8) 0.0311(9) 0.0392(10) -0.0016(7) -0.0026(7) -0.0069(7) C12 0.0244(8) 0.0362(10) 0.0519(11) -0.0140(8) -0.0191(8) 0.0011(7) C13 0.0254(7) 0.0252(8) 0.0182(7) -0.0047(6) -0.0055(6) -0.0070(6) C14 0.0256(8) 0.0261(9) 0.0290(8) -0.0079(7) -0.0045(6) 0.0007(6) C15 0.0380(9) 0.0236(9) 0.0367(9) -0.0111(7) -0.0051(7) -0.0002(7) C16 0.0480(11) 0.0342(10) 0.0458(11) -0.0089(8) -0.0123(9) -0.0211(9) C17 0.0221(7) 0.0245(8) 0.0203(7) -0.0021(6) -0.0059(6) -0.0054(6) C18 0.0269(8) 0.0277(8) 0.0228(7) -0.0090(6) -0.0076(6) -0.0028(6) C19 0.0257(8) 0.0333(9) 0.0210(7) -0.0070(7) -0.0083(6) -0.0038(7) C20 0.0414(10) 0.0288(9) 0.0288(9) 0.0018(7) -0.0136(7) -0.0009(8) C21 0.0238(7) 0.0204(8) 0.0233(7) -0.0054(6) -0.0083(6) -0.0020(6) C22 0.0241(8) 0.0285(9) 0.0231(8) -0.0005(6) -0.0038(6) -0.0078(7) C23 0.0220(8) 0.0293(9) 0.0309(8) -0.0023(7) -0.0027(6) -0.0086(7) C24 0.0294(9) 0.0425(11) 0.0439(10) -0.0092(8) -0.0206(8) -0.0013(8) C25 0.0321(9) 0.0534(13) 0.0552(12) -0.0277(10) -0.0174(9) 0.0041(9) C26 0.0415(10) 0.0465(12) 0.0488(11) -0.0137(9) -0.0168(9) -0.0069(9) C27 0.0308(10) 0.0610(14) 0.0420(11) -0.0112(10) -0.0137(8) -0.0075(9) B1 0.0196(8) 0.0202(8) 0.0209(8) -0.0026(7) -0.0070(6) -0.0030(6) B2 0.0203(8) 0.0204(8) 0.0212(8) -0.0037(7) -0.0060(6) -0.0029(6) N1 0.0195(6) 0.0214(7) 0.0218(6) -0.0045(5) -0.0050(5) -0.0025(5) N2 0.0291(7) 0.0263(7) 0.0298(7) -0.0061(6) -0.0071(6) -0.0101(6) N3 0.0208(6) 0.0221(7) 0.0209(6) -0.0050(5) -0.0069(5) -0.0030(5) N4 0.0259(7) 0.0249(7) 0.0222(6) -0.0013(5) -0.0095(5) -0.0014(5) N5 0.0188(6) 0.0220(7) 0.0223(6) -0.0016(5) -0.0052(5) -0.0046(5) N6 0.0189(6) 0.0245(7) 0.0367(8) -0.0075(6) -0.0095(5) -0.0022(5) N7 0.0205(6) 0.0213(7) 0.0225(6) -0.0051(5) -0.0055(5) -0.0023(5) N8 0.0329(7) 0.0261(7) 0.0292(7) -0.0094(6) -0.0047(6) -0.0097(6) N9 0.0222(6) 0.0237(7) 0.0200(6) -0.0049(5) -0.0070(5) -0.0037(5) N10 0.0253(6) 0.0256(7) 0.0213(6) -0.0012(5) -0.0087(5) -0.0033(5) N11 0.0209(6) 0.0231(7) 0.0204(6) -0.0024(5) -0.0069(5) -0.0044(5) N12 0.0211(6) 0.0264(7) 0.0309(7) -0.0055(6) -0.0108(5) -0.0038(5) N13 0.0245(7) 0.0458(9) 0.0365(8) -0.0159(7) -0.0108(6) -0.0025(6) O1 0.0303(6) 0.0353(7) 0.0311(6) -0.0101(5) -0.0094(5) -0.0076(5) O2 0.0396(7) 0.0589(10) 0.0436(8) 0.0038(7) -0.0170(7) -0.0054(7) O3 0.0446(8) 0.0339(7) 0.0531(8) -0.0098(6) -0.0258(6) -0.0024(6) O4 0.0270(6) 0.0330(7) 0.0267(6) -0.0028(5) -0.0072(5) 0.0038(5) O5 0.0326(6) 0.0312(7) 0.0284(6) -0.0026(5) -0.0093(5) -0.0002(5) O6 0.0308(6) 0.0325(7) 0.0275(6) -0.0098(5) -0.0067(5) -0.0022(5) O7 0.094(3) 0.0350(16) 0.059(3) -0.002(2) 0.024(3) -0.0192(17) O8 0.0269(7) 0.0806(12) 0.0616(9) -0.0140(8) -0.0126(6) 0.0034(7) Na1 0.0279(3) 0.0314(4) 0.0273(3) -0.0085(3) -0.0066(3) -0.0047(3) Na2 0.0290(3) 0.0351(4) 0.0413(4) -0.0076(3) -0.0137(3) 0.0000(3) S1 0.01981(18) 0.0350(2) 0.0285(2) -0.00787(17) -0.00797(15) -0.00160(16) S2 0.0466(3) 0.0228(2) 0.0251(2) -0.00549(16) -0.01089(18) -0.00523(18) S3 0.0247(2) 0.0368(2) 0.02294(19) -0.00221(17) -0.00912(15) 0.00180(17) S4 0.02081(19) 0.0368(2) 0.0327(2) -0.01207(18) -0.00898(16) -0.00218(16) S5 0.0578(3) 0.0233(2) 0.0256(2) -0.00488(17) -0.01403(19) -0.00801(19) S6 0.0299(2) 0.0330(2) 0.01977(19) -0.00237(16) -0.00809(15) 0.00215(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 1.355(2) . ? C1 N1 1.3662(19) . ? C1 S1 1.7007(16) . ? C2 C3 1.345(2) . ? C2 N1 1.386(2) . ? C3 N2 1.384(2) . ? C4 N2 1.460(2) . ? C5 N3 1.355(2) . ? C5 N4 1.3630(19) . ? C5 S2 1.7007(16) . ? C6 C7 1.349(2) . ? C6 N3 1.3909(19) . ? C7 N4 1.381(2) . ? C8 N4 1.457(2) . ? C9 N5 1.3544(18) . ? C9 N6 1.3558(19) . ? C9 S3 1.7031(16) . ? C10 C11 1.348(2) . ? C10 N5 1.3889(19) . ? C11 N6 1.373(2) . ? C12 N6 1.459(2) . ? C13 N8 1.357(2) . ? C13 N7 1.3620(19) . ? C13 S4 1.7008(17) . ? C14 C15 1.342(2) . ? C14 N7 1.387(2) . ? C15 N8 1.389(2) . ? C16 N8 1.458(2) . ? C17 N9 1.355(2) . ? C17 N10 1.3617(19) . ? C17 S5 1.6972(16) . ? C18 C19 1.349(2) . ? C18 N9 1.3912(19) . ? C19 N10 1.379(2) . ? C20 N10 1.458(2) . ? C21 N12 1.3552(19) . ? C21 N11 1.3559(18) . ? C21 S6 1.7059(16) . ? C22 C23 1.347(2) . ? C22 N11 1.3834(19) . ? C23 N12 1.377(2) . ? C24 N12 1.4570(19) . ? C25 N13 1.454(2) . ? C26 N13 1.460(2) . ? C27 O8 1.239(2) . ? C27 N13 1.324(2) . ? B1 N3 1.545(2) . ? B1 N1 1.550(2) . ? B1 N5 1.558(2) . ? B2 N9 1.550(2) . ? B2 N7 1.553(2) . ? B2 N11 1.553(2) . ? O1 Na1 2.3671(14) . ? O2 Na1 2.3452(16) . ? O3 Na1 2.3562(16) . ? O4 Na2 2.3244(15) . ? O4 Na1 2.5390(16) . ? O5 Na2 2.3856(15) . ? O5 Na1 2.4320(14) . ? O6 Na2 2.4781(15) . ? O6 Na1 2.5031(15) . ? O7 O7 1.045(7) 2_766 ? O7 Na2 2.471(4) . ? O7 Na2 2.683(4) 2_766 ? O8 Na2 2.2531(17) . ? Na1 Na2 3.2726(13) . ? Na2 O7 2.683(4) 2_766 ? Na2 S1 3.1277(12) . ? 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 C1 N1 106.86(13) . . ? N2 C1 S1 126.18(11) . . ? N1 C1 S1 126.93(12) . . ? C3 C2 N1 108.11(14) . . ? C2 C3 N2 107.20(15) . . ? N3 C5 N4 107.12(13) . . ? N3 C5 S2 128.80(11) . . ? N4 C5 S2 124.06(12) . . ? C7 C6 N3 108.21(14) . . ? C6 C7 N4 106.94(13) . . ? N5 C9 N6 107.62(13) . . ? N5 C9 S3 126.63(11) . . ? N6 C9 S3 125.76(11) . . ? C11 C10 N5 108.13(14) . . ? C10 C11 N6 107.24(14) . . ? N8 C13 N7 106.84(13) . . ? N8 C13 S4 126.11(11) . . ? N7 C13 S4 127.04(12) . . ? C15 C14 N7 108.28(14) . . ? C14 C15 N8 107.00(15) . . ? N9 C17 N10 107.09(13) . . ? N9 C17 S5 128.56(11) . . ? N10 C17 S5 124.34(12) . . ? C19 C18 N9 108.34(14) . . ? C18 C19 N10 106.81(13) . . ? N12 C21 N11 107.08(13) . . ? N12 C21 S6 125.67(11) . . ? N11 C21 S6 127.25(11) . . ? C23 C22 N11 108.12(14) . . ? C22 C23 N12 107.04(13) . . ? O8 C27 N13 124.0(2) . . ? N3 B1 N1 108.19(12) . . ? N3 B1 N5 108.14(11) . . ? N1 B1 N5 109.34(12) . . ? N9 B2 N7 108.18(12) . . ? N9 B2 N11 108.61(11) . . ? N7 B2 N11 108.57(12) . . ? C1 N1 C2 108.41(13) . . ? C1 N1 B1 123.48(12) . . ? C2 N1 B1 128.11(13) . . ? C1 N2 C3 109.41(13) . . ? C1 N2 C4 125.34(14) . . ? C3 N2 C4 125.17(15) . . ? C5 N3 C6 108.35(12) . . ? C5 N3 B1 125.50(12) . . ? C6 N3 B1 126.10(13) . . ? C5 N4 C7 109.37(13) . . ? C5 N4 C8 125.17(14) . . ? C7 N4 C8 125.45(13) . . ? C9 N5 C10 107.86(12) . . ? C9 N5 B1 124.87(12) . . ? C10 N5 B1 126.85(12) . . ? C9 N6 C11 109.14(12) . . ? C9 N6 C12 124.98(14) . . ? C11 N6 C12 125.87(14) . . ? C13 N7 C14 108.50(13) . . ? C13 N7 B2 123.73(12) . . ? C14 N7 B2 127.76(13) . . ? C13 N8 C15 109.36(13) . . ? C13 N8 C16 125.16(14) . . ? C15 N8 C16 125.47(15) . . ? C17 N9 C18 108.20(12) . . ? C17 N9 B2 124.70(12) . . ? C18 N9 B2 126.88(13) . . ? C17 N10 C19 109.56(13) . . ? C17 N10 C20 125.03(14) . . ? C19 N10 C20 125.41(13) . . ? C21 N11 C22 108.37(12) . . ? C21 N11 B2 124.88(12) . . ? C22 N11 B2 126.75(12) . . ? C21 N12 C23 109.39(12) . . ? C21 N12 C24 125.10(14) . . ? C23 N12 C24 125.49(14) . . ? C27 N13 C25 122.29(17) . . ? C27 N13 C26 119.98(16) . . ? C25 N13 C26 117.54(15) . . ? Na2 O4 Na1 84.46(4) . . ? Na2 O5 Na1 85.57(4) . . ? Na2 O6 Na1 82.14(4) . . ? O7 O7 Na2 90.0(4) 2_766 . ? O7 O7 Na2 67.1(4) 2_766 2_766 ? Na2 O7 Na2 157.09(15) . 2_766 ? C27 O8 Na2 147.40(15) . . ? O2 Na1 O3 85.50(6) . . ? O2 Na1 O1 105.95(6) . . ? O3 Na1 O1 102.33(5) . . ? O2 Na1 O5 165.67(5) . . ? O3 Na1 O5 97.38(5) . . ? O1 Na1 O5 87.21(5) . . ? O2 Na1 O6 87.14(5) . . ? O3 Na1 O6 95.69(5) . . ? O1 Na1 O6 158.36(5) . . ? O5 Na1 O6 78.62(5) . . ? O2 Na1 O4 95.21(5) . . ? O3 Na1 O4 171.39(5) . . ? O1 Na1 O4 85.75(4) . . ? O5 Na1 O4 79.87(4) . . ? O6 Na1 O4 75.79(4) . . ? O2 Na1 Na2 121.33(5) . . ? O3 Na1 Na2 127.85(4) . . ? O1 Na1 Na2 109.98(4) . . ? O5 Na1 Na2 46.62(3) . . ? O6 Na1 Na2 48.60(4) . . ? O4 Na1 Na2 44.99(3) . . ? O8 Na2 O4 173.34(6) . . ? O8 Na2 O5 98.18(6) . . ? O4 Na2 O5 85.32(5) . . ? O8 Na2 O7 84.61(12) . . ? O4 Na2 O7 92.35(12) . . ? O5 Na2 O7 174.69(10) . . ? O8 Na2 O6 94.74(6) . . ? O4 Na2 O6 80.24(4) . . ? O5 Na2 O6 79.99(5) . . ? O7 Na2 O6 104.34(8) . . ? O8 Na2 O7 74.10(11) . 2_766 ? O4 Na2 O7 105.09(11) . 2_766 ? O5 Na2 O7 154.12(8) . 2_766 ? O7 Na2 O7 22.91(15) . 2_766 ? O6 Na2 O7 124.67(7) . 2_766 ? O8 Na2 S1 96.66(5) . . ? O4 Na2 S1 88.96(4) . . ? O5 Na2 S1 90.26(4) . . ? O7 Na2 S1 84.93(8) . . ? O6 Na2 S1 165.95(4) . . ? O7 Na2 S1 66.76(7) 2_766 . ? O8 Na2 Na1 128.64(6) . . ? O4 Na2 Na1 50.55(4) . . ? O5 Na2 Na1 47.81(3) . . ? O7 Na2 Na1 133.11(10) . . ? O6 Na2 Na1 49.26(3) . . ? O7 Na2 Na1 153.37(10) 2_766 . ? S1 Na2 Na1 116.74(3) . . ? C1 S1 Na2 120.12(5) . . ?