Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email MAKITA@RES.TITECH.AC.JP _publ_contact_author_name 'Prof Munetaka Akita' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 'Tue Sep 2 17:23:37 2003' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_contact_author_address ; Chemical Resources Laboratory Tokyo Institute of Technology 4259 Nagatsuta Midori-ku Yokohama 226-8503 JAPAN ; _publ_section_title ; A Peroxochromium Complex, TpiPr2Cr(O2)2, Obtained by Oxidative Dehydrative Condensation Between a Dihydroxochromium Complex and H2O2 [TpiPr2= hydrotris(3,5-diisopropylpyrazolyl)borato]. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name '' 'Munetaka Akita' 'Shiro Hikichi' 'Ken-ichiro Sugawara' #------------------------------------------------------------------------------ data_compound_3 _database_code_CSD 217496 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C64 H118 B2 Cr2 N12 O2 ' _chemical_formula_moiety 'C64 H118 B2 Cr2 N12 O2 ' _chemical_formula_weight 1213.33 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.813(1) _cell_length_b 22.974(1) _cell_length_c 13.0204(4) _cell_angle_alpha 101.495(4) _cell_angle_beta 114.731(2) _cell_angle_gamma 85.944(4) _cell_volume 3677.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6171 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.966 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 28733 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15071 _reflns_number_gt 7222 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0943 _refine_ls_wR_factor_ref 0.2356 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7222 _refine_ls_number_parameters 763 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0130 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.78 _refine_diff_density_min -1.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.98565(6) 0.04672(3) 0.91910(6) 0.0252(2) Uani 1.00 d . . . Cr(2) Cr 0.57991(7) 0.44993(4) 0.48555(7) 0.0428(3) Uani 1.00 d . . . O(1) O 0.9410(3) 0.0300(1) 1.0398(3) 0.0344(8) Uani 1.00 d . . . O(2) O 0.4220(3) 0.4678(2) 0.4330(3) 0.055(1) Uani 1.00 d . . . N(11A) N 0.8409(3) 0.0117(2) 0.7426(3) 0.0306(9) Uani 1.00 d . . . N(11B) N 0.6244(3) 0.4595(2) 0.3292(3) 0.036(1) Uani 1.00 d . . . N(12A) N 0.8097(3) 0.0502(2) 0.6660(3) 0.0294(9) Uani 1.00 d . . . N(12B) N 0.6759(3) 0.4111(2) 0.2955(4) 0.037(1) Uani 1.00 d . . . N(21A) N 1.0582(3) 0.0640(2) 0.8113(3) 0.0268(9) Uani 1.00 d . . . N(21B) N 0.7476(3) 0.4320(2) 0.5647(4) 0.038(1) Uani 1.00 d . . . N(22A) N 0.9949(3) 0.0874(2) 0.7134(3) 0.0273(9) Uani 1.00 d . . . N(22B) N 0.7906(3) 0.3952(2) 0.4968(4) 0.039(1) Uani 1.00 d . . . N(31A) N 0.9223(3) 0.1342(2) 0.9078(3) 0.0285(9) Uani 1.00 d . . . N(31B) N 0.5578(3) 0.3573(2) 0.4187(4) 0.037(1) Uani 1.00 d . . . N(32A) N 0.8797(3) 0.1503(2) 0.7992(3) 0.0285(9) Uani 1.00 d . . . N(32B) N 0.6264(3) 0.3291(2) 0.3724(4) 0.036(1) Uani 1.00 d . . . C(11A) C 0.7718(4) -0.0339(2) 0.6926(4) 0.033(1) Uani 1.00 d . . . C(11B) C 0.6108(5) 0.4963(2) 0.2569(4) 0.043(1) Uani 1.00 d . . . C(12A) C 0.6955(4) -0.0256(2) 0.5848(4) 0.038(1) Uani 1.00 d . . . C(12B) C 0.6493(5) 0.4726(2) 0.1755(5) 0.052(2) Uani 1.00 d . . . C(13A) C 0.7219(4) 0.0282(2) 0.5711(4) 0.032(1) Uani 1.00 d . . . C(13B) C 0.6907(5) 0.4183(2) 0.2019(5) 0.043(1) Uani 1.00 d . . . C(14A) C 0.7812(4) -0.0855(2) 0.7510(5) 0.045(1) Uani 1.00 d . . . C(14B) C 0.5581(6) 0.5552(3) 0.2708(5) 0.061(2) Uani 1.00 d . . . C(15A) C 0.6876(6) -0.0883(3) 0.7839(6) 0.075(2) Uani 1.00 d . . . C(15B) C 0.4399(7) 0.5500(4) 0.200(1) 0.164(5) Uani 1.00 d . . . C(16A) C 0.7877(7) -0.1432(2) 0.6746(6) 0.082(2) Uani 1.00 d . . . C(16B) C 0.6027(8) 0.6016(3) 0.2357(9) 0.121(4) Uani 1.00 d . . . C(17A) C 0.6648(4) 0.0613(2) 0.4732(4) 0.038(1) Uani 1.00 d . . . C(17B) C 0.7407(5) 0.3721(2) 0.1388(5) 0.049(2) Uani 1.00 d . . . C(18A) C 0.6000(4) 0.1127(2) 0.5084(5) 0.049(2) Uani 1.00 d . . . C(18B) C 0.6572(6) 0.3278(3) 0.0475(5) 0.066(2) Uani 1.00 d . . . C(19A) C 0.5926(4) 0.0194(3) 0.3637(5) 0.053(2) Uani 1.00 d . . . C(19B) C 0.8004(6) 0.4005(3) 0.0862(6) 0.080(2) Uani 1.00 d . . . C(21A) C 1.1533(4) 0.0545(2) 0.8065(4) 0.033(1) Uani 1.00 d . . . C(21B) C 0.8307(4) 0.4538(2) 0.6634(5) 0.042(1) Uani 1.00 d . . . C(22A) C 1.1524(4) 0.0709(2) 0.7087(5) 0.044(1) Uani 1.00 d . . . C(22B) C 0.9254(4) 0.4324(3) 0.6586(5) 0.050(2) Uani 1.00 d . . . C(23A) C 1.0508(4) 0.0914(2) 0.6522(4) 0.034(1) Uani 1.00 d . . . C(23B) C 0.8984(4) 0.3960(2) 0.5533(5) 0.044(1) Uani 1.00 d . . . C(24A) C 1.2450(4) 0.0283(2) 0.8982(5) 0.043(1) Uani 1.00 d . . . C(24B) C 0.8174(4) 0.4946(3) 0.7626(5) 0.052(2) Uani 1.00 d . . . C(25A) C 1.3464(5) 0.0662(3) 0.9460(6) 0.066(2) Uani 1.00 d . . . C(25B) C 0.8828(6) 0.5505(3) 0.8000(7) 0.078(2) Uani 1.00 d . . . C(26A) C 1.2661(5) -0.0346(3) 0.8488(6) 0.068(2) Uani 1.00 d . . . C(26B) C 0.8470(6) 0.4622(3) 0.8645(6) 0.078(2) Uani 1.00 d . . . C(27A) C 1.0057(4) 0.1123(3) 0.5376(5) 0.050(2) Uani 1.00 d . . . C(27B) C 0.9709(5) 0.3637(3) 0.5011(6) 0.061(2) Uani 1.00 d . . . C(28A) C 1.0244(8) 0.0717(3) 0.4471(6) 0.113(4) Uani 1.00 d . . . C(28B) C 0.9945(6) 0.4013(3) 0.4307(7) 0.091(3) Uani 1.00 d . . . C(29A) C 1.0463(9) 0.1716(3) 0.5498(7) 0.144(5) Uani 1.00 d . . . C(29B) C 1.0750(6) 0.3464(3) 0.5951(7) 0.102(3) Uani 1.00 d . . . C(31A) C 0.9147(4) 0.1822(2) 0.9808(4) 0.031(1) Uani 1.00 d . . . C(31B) C 0.4861(4) 0.3162(2) 0.4049(4) 0.039(1) Uani 1.00 d . . . C(32A) C 0.8686(4) 0.2287(2) 0.9230(5) 0.039(1) Uani 1.00 d . . . C(32B) C 0.5086(5) 0.2613(2) 0.3480(5) 0.046(1) Uani 1.00 d . . . C(33A) C 0.8467(4) 0.2078(2) 0.8089(4) 0.034(1) Uani 1.00 d . . . C(33B) C 0.5969(4) 0.2712(2) 0.3300(4) 0.037(1) Uani 1.00 d . . . C(34A) C 0.9551(5) 0.1834(2) 1.1088(5) 0.042(1) Uani 1.00 d . . . C(34B) C 0.3978(5) 0.3288(2) 0.4451(5) 0.051(2) Uani 1.00 d . . . C(35A) C 1.0149(6) 0.2413(3) 1.1781(6) 0.078(2) Uani 1.00 d . . . C(35B) C 0.2910(5) 0.3263(3) 0.3434(6) 0.083(2) Uani 1.00 d . . . C(36A) C 0.8602(6) 0.1779(3) 1.1398(6) 0.073(2) Uani 1.00 d . . . C(36B) C 0.3990(6) 0.2863(3) 0.5202(7) 0.084(2) Uani 1.00 d . . . C(37A) C 0.8015(5) 0.2414(2) 0.7096(5) 0.044(1) Uani 1.00 d . . . C(37B) C 0.6545(5) 0.2265(2) 0.2757(5) 0.046(1) Uani 1.00 d . . . C(38A) C 0.8862(6) 0.2821(3) 0.7146(7) 0.091(3) Uani 1.00 d . . . C(38B) C 0.5803(6) 0.1787(3) 0.1866(6) 0.084(2) Uani 1.00 d . . . C(39A) C 0.7063(6) 0.2772(3) 0.7122(6) 0.088(3) Uani 1.00 d . . . C(39B) C 0.7464(5) 0.2007(2) 0.3693(5) 0.058(2) Uani 1.00 d . . . C(40) C 0.3387(10) 0.2201(5) 0.730(1) 0.142(4) Uani 1.00 d . . . C(41) C 0.4496(9) 0.2129(5) 0.803(1) 0.143(4) Uani 1.00 d . . . C(42) C 0.4965(8) 0.1539(4) 0.7832(9) 0.119(3) Uani 1.00 d . . . C(43) C 0.5998(9) 0.1418(6) 0.8536(10) 0.150(5) Uani 1.00 d . . . C(44) C 0.6461(7) 0.0852(4) 0.8401(8) 0.101(3) Uani 1.00 d . . . C(45) C 0.8396(10) -0.2147(5) 1.050(1) 0.152(5) Uani 1.00 d . . . C(46) C 0.769(2) -0.256(1) 1.016(2) 0.26(1) Uani 1.00 d . . . C(47) C 0.750(2) -0.3091(6) 1.005(2) 0.24(1) Uani 1.00 d . . . C(48) C 0.620(1) -0.3807(10) 0.913(1) 0.224(9) Uani 1.00 d . . . C(49) C 0.683(2) -0.354(2) 0.980(2) 0.39(2) Uani 1.00 d . . . B(1) B 0.8785(5) 0.1059(2) 0.6920(5) 0.031(1) Uani 1.00 d . . . B(2) B 0.7185(5) 0.3641(3) 0.3727(5) 0.038(1) Uani 1.00 d . . . H(1) H 0.8889 0.0447 1.0717 0.0300 Uiso 1.00 calc . . . H(2) H 0.3714 0.4288 0.3609 0.0300 Uiso 1.00 calc . . . H(3) H 0.8496 0.1259 0.6266 0.0370 Uiso 1.00 calc . . . H(4) H 0.6369 -0.0520 0.5304 0.0470 Uiso 1.00 calc . . . H(5) H 0.8463 -0.0816 0.8206 0.0561 Uiso 1.00 calc . . . H(6) H 0.6834 -0.0514 0.8316 0.0752 Uiso 1.00 calc . . . H(7) H 0.6981 -0.1201 0.8252 0.0752 Uiso 1.00 calc . . . H(8) H 0.6225 -0.0952 0.7154 0.0752 Uiso 1.00 calc . . . H(9) H 0.7242 -0.1487 0.6041 0.0818 Uiso 1.00 calc . . . H(10) H 0.7941 -0.1757 0.7134 0.0818 Uiso 1.00 calc . . . H(11) H 0.8487 -0.1420 0.6576 0.0818 Uiso 1.00 calc . . . H(12) H 0.7189 0.0779 0.4570 0.0497 Uiso 1.00 calc . . . H(13) H 0.6468 0.1389 0.5758 0.0493 Uiso 1.00 calc . . . H(14) H 0.5465 0.0968 0.5246 0.0493 Uiso 1.00 calc . . . H(15) H 0.5663 0.1342 0.4466 0.0493 Uiso 1.00 calc . . . H(16) H 0.5370 0.0038 0.3767 0.0527 Uiso 1.00 calc . . . H(17) H 0.6340 -0.0126 0.3441 0.0527 Uiso 1.00 calc . . . H(18) H 0.5616 0.0410 0.3016 0.0527 Uiso 1.00 calc . . . H(19) H 1.2112 0.0689 0.6856 0.0543 Uiso 1.00 calc . . . H(20) H 1.2249 0.0269 0.9609 0.0512 Uiso 1.00 calc . . . H(21) H 1.4025 0.0487 1.0041 0.0657 Uiso 1.00 calc . . . H(22) H 1.3333 0.1055 0.9789 0.0657 Uiso 1.00 calc . . . H(23) H 1.3670 0.0681 0.8848 0.0657 Uiso 1.00 calc . . . H(24) H 1.2017 -0.0580 0.8172 0.0677 Uiso 1.00 calc . . . H(25) H 1.3204 -0.0519 0.9088 0.0677 Uiso 1.00 calc . . . H(26) H 1.2894 -0.0336 0.7894 0.0677 Uiso 1.00 calc . . . H(27) H 0.9283 0.1151 0.5122 0.0644 Uiso 1.00 calc . . . H(28) H 0.9996 0.0327 0.4408 0.1132 Uiso 1.00 calc . . . H(29) H 1.0994 0.0707 0.4652 0.1132 Uiso 1.00 calc . . . H(30) H 0.9867 0.0850 0.3753 0.1132 Uiso 1.00 calc . . . H(31) H 1.1211 0.1697 0.5676 0.1442 Uiso 1.00 calc . . . H(32) H 1.0351 0.1981 0.6107 0.1442 Uiso 1.00 calc . . . H(33) H 1.0092 0.1859 0.4790 0.1442 Uiso 1.00 calc . . . H(34) H 0.8543 0.2681 0.9556 0.0459 Uiso 1.00 calc . . . H(35) H 1.0007 0.1500 1.1267 0.0525 Uiso 1.00 calc . . . H(36) H 1.0412 0.2406 1.2588 0.0776 Uiso 1.00 calc . . . H(37) H 0.9675 0.2740 1.1604 0.0776 Uiso 1.00 calc . . . H(38) H 1.0736 0.2456 1.1590 0.0776 Uiso 1.00 calc . . . H(39) H 0.8136 0.2109 1.1212 0.0732 Uiso 1.00 calc . . . H(40) H 0.8862 0.1778 1.2206 0.0732 Uiso 1.00 calc . . . H(41) H 0.8217 0.1415 1.0968 0.0732 Uiso 1.00 calc . . . H(42) H 0.7787 0.2123 0.6368 0.0546 Uiso 1.00 calc . . . H(43) H 0.9461 0.2589 0.7122 0.0910 Uiso 1.00 calc . . . H(44) H 0.9089 0.3109 0.7848 0.0910 Uiso 1.00 calc . . . H(45) H 0.8572 0.3020 0.6501 0.0910 Uiso 1.00 calc . . . H(46) H 0.7274 0.3053 0.7832 0.0879 Uiso 1.00 calc . . . H(47) H 0.6522 0.2510 0.7061 0.0879 Uiso 1.00 calc . . . H(48) H 0.6786 0.2979 0.6488 0.0879 Uiso 1.00 calc . . . H(49) H 0.7611 0.3360 0.3438 0.0478 Uiso 1.00 calc . . . H(50) H 0.6470 0.4898 0.1123 0.0629 Uiso 1.00 calc . . . H(51) H 0.5684 0.5694 0.3506 0.0785 Uiso 1.00 calc . . . H(52) H 0.4073 0.5870 0.2160 0.1641 Uiso 1.00 calc . . . H(53) H 0.4112 0.5191 0.2195 0.1641 Uiso 1.00 calc . . . H(54) H 0.4257 0.5407 0.1199 0.1641 Uiso 1.00 calc . . . H(55) H 0.6779 0.6063 0.2826 0.1208 Uiso 1.00 calc . . . H(56) H 0.5681 0.6387 0.2457 0.1208 Uiso 1.00 calc . . . H(57) H 0.5908 0.5895 0.1564 0.1208 Uiso 1.00 calc . . . H(58) H 0.7911 0.3503 0.1958 0.0601 Uiso 1.00 calc . . . H(59) H 0.6074 0.3478 -0.0110 0.0663 Uiso 1.00 calc . . . H(60) H 0.6200 0.3106 0.0824 0.0663 Uiso 1.00 calc . . . H(61) H 0.6914 0.2970 0.0136 0.0663 Uiso 1.00 calc . . . H(62) H 0.8529 0.4280 0.1452 0.0801 Uiso 1.00 calc . . . H(63) H 0.7511 0.4212 0.0286 0.0801 Uiso 1.00 calc . . . H(64) H 0.8349 0.3703 0.0516 0.0801 Uiso 1.00 calc . . . H(65) H 0.9970 0.4408 0.7193 0.0612 Uiso 1.00 calc . . . H(66) H 0.7424 0.5050 0.7380 0.0658 Uiso 1.00 calc . . . H(67) H 0.9571 0.5412 0.8346 0.0781 Uiso 1.00 calc . . . H(68) H 0.8645 0.5778 0.8551 0.0781 Uiso 1.00 calc . . . H(69) H 0.8687 0.5682 0.7344 0.0781 Uiso 1.00 calc . . . H(70) H 0.8009 0.4282 0.8410 0.0782 Uiso 1.00 calc . . . H(71) H 0.8388 0.4887 0.9273 0.0782 Uiso 1.00 calc . . . H(72) H 0.9197 0.4496 0.8886 0.0782 Uiso 1.00 calc . . . H(73) H 0.9335 0.3276 0.4467 0.0796 Uiso 1.00 calc . . . H(74) H 1.0389 0.4346 0.4812 0.0907 Uiso 1.00 calc . . . H(75) H 0.9289 0.4153 0.3781 0.0907 Uiso 1.00 calc . . . H(76) H 1.0307 0.3777 0.3883 0.0907 Uiso 1.00 calc . . . H(77) H 1.0586 0.3246 0.6416 0.1018 Uiso 1.00 calc . . . H(78) H 1.1151 0.3816 0.6425 0.1018 Uiso 1.00 calc . . . H(79) H 1.1164 0.3221 0.5598 0.1018 Uiso 1.00 calc . . . H(80) H 0.4690 0.2238 0.3272 0.0574 Uiso 1.00 calc . . . H(81) H 0.4105 0.3683 0.4918 0.0641 Uiso 1.00 calc . . . H(82) H 0.2364 0.3385 0.3703 0.0826 Uiso 1.00 calc . . . H(83) H 0.2763 0.2864 0.3005 0.0826 Uiso 1.00 calc . . . H(84) H 0.2923 0.3523 0.2948 0.0826 Uiso 1.00 calc . . . H(85) H 0.3440 0.2967 0.5472 0.0840 Uiso 1.00 calc . . . H(86) H 0.4671 0.2887 0.5848 0.0840 Uiso 1.00 calc . . . H(87) H 0.3867 0.2466 0.4764 0.0840 Uiso 1.00 calc . . . H(88) H 0.6826 0.2471 0.2357 0.0598 Uiso 1.00 calc . . . H(89) H 0.5224 0.1964 0.1307 0.0842 Uiso 1.00 calc . . . H(90) H 0.5526 0.1560 0.2232 0.0842 Uiso 1.00 calc . . . H(91) H 0.6184 0.1529 0.1491 0.0842 Uiso 1.00 calc . . . H(92) H 0.7188 0.1817 0.4110 0.0585 Uiso 1.00 calc . . . H(93) H 0.7950 0.2321 0.4213 0.0585 Uiso 1.00 calc . . . H(94) H 0.7832 0.1721 0.3345 0.0585 Uiso 1.00 calc . . . H(95) H 0.3157 0.2597 0.7465 0.1550 Uiso 1.00 calc . . . H(96) H 0.3254 0.2104 0.6510 0.1550 Uiso 1.00 calc . . . H(97) H 0.2982 0.1936 0.7457 0.1550 Uiso 1.00 calc . . . H(98) H 0.4903 0.2420 0.7854 0.1634 Uiso 1.00 calc . . . H(99) H 0.4631 0.2254 0.8802 0.1634 Uiso 1.00 calc . . . H(100) H 0.4470 0.1262 0.7883 0.1472 Uiso 1.00 calc . . . H(101) H 0.4832 0.1444 0.7010 0.1472 Uiso 1.00 calc . . . H(102) H 0.6402 0.1691 0.8379 0.1793 Uiso 1.00 calc . . . H(103) H 0.6043 0.1526 0.9267 0.1793 Uiso 1.00 calc . . . H(104) H 0.6130 0.0559 0.8570 0.1207 Uiso 1.00 calc . . . H(105) H 0.6482 0.0723 0.7676 0.1207 Uiso 1.00 calc . . . H(106) H 0.7218 0.0877 0.8979 0.1207 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0267(4) 0.0263(4) 0.0283(4) 0.0037(3) 0.0154(4) 0.0096(3) Cr(2) 0.0341(5) 0.0470(5) 0.0393(6) 0.0093(4) 0.0139(4) -0.0038(4) O(1) 0.038(2) 0.038(2) 0.041(2) 0.011(2) 0.029(2) 0.011(2) O(2) 0.047(2) 0.048(2) 0.055(3) 0.010(2) 0.014(2) -0.003(2) N(11A) 0.031(2) 0.028(2) 0.032(2) -0.002(2) 0.010(2) 0.010(2) N(11B) 0.043(3) 0.036(2) 0.030(2) 0.008(2) 0.020(2) 0.004(2) N(12A) 0.033(2) 0.028(2) 0.029(2) 0.004(2) 0.012(2) 0.011(2) N(12B) 0.044(3) 0.039(2) 0.036(3) 0.011(2) 0.024(2) 0.008(2) N(21A) 0.024(2) 0.031(2) 0.027(2) 0.000(2) 0.012(2) 0.007(2) N(21B) 0.033(3) 0.044(2) 0.037(3) 0.007(2) 0.017(2) 0.005(2) N(22A) 0.024(2) 0.033(2) 0.029(2) 0.003(2) 0.015(2) 0.009(2) N(22B) 0.033(3) 0.048(3) 0.041(3) 0.012(2) 0.021(2) 0.009(2) N(31A) 0.037(2) 0.027(2) 0.025(2) 0.005(2) 0.016(2) 0.007(2) N(31B) 0.042(3) 0.034(2) 0.041(3) 0.010(2) 0.024(2) 0.004(2) N(32A) 0.033(2) 0.027(2) 0.032(2) 0.004(2) 0.019(2) 0.008(2) N(32B) 0.041(3) 0.033(2) 0.042(3) 0.008(2) 0.027(2) 0.006(2) C(11A) 0.029(3) 0.031(2) 0.038(3) -0.004(2) 0.012(2) 0.008(2) C(11B) 0.057(4) 0.044(3) 0.029(3) 0.011(3) 0.020(3) 0.009(3) C(12A) 0.034(3) 0.036(3) 0.038(3) -0.008(2) 0.009(3) 0.008(2) C(12B) 0.078(5) 0.044(3) 0.048(4) 0.019(3) 0.036(3) 0.021(3) C(13A) 0.024(3) 0.042(3) 0.028(3) 0.003(2) 0.009(2) 0.007(2) C(13B) 0.056(4) 0.041(3) 0.044(3) 0.006(3) 0.035(3) 0.008(3) C(14A) 0.033(3) 0.048(3) 0.046(4) -0.007(3) 0.003(3) 0.017(3) C(14B) 0.095(5) 0.044(3) 0.053(4) 0.031(4) 0.040(4) 0.018(3) C(15A) 0.089(6) 0.082(5) 0.079(5) 0.003(4) 0.046(4) 0.044(4) C(15B) 0.107(8) 0.086(6) 0.29(2) 0.051(6) 0.084(9) 0.015(8) C(16A) 0.127(7) 0.036(3) 0.099(6) 0.005(4) 0.060(5) 0.021(4) C(16B) 0.141(9) 0.051(4) 0.20(1) 0.029(5) 0.097(8) 0.032(6) C(17A) 0.030(3) 0.052(3) 0.034(3) -0.004(2) 0.010(2) 0.020(3) C(17B) 0.068(4) 0.048(3) 0.052(4) 0.021(3) 0.043(3) 0.023(3) C(18A) 0.038(3) 0.051(3) 0.059(4) 0.007(3) 0.015(3) 0.023(3) C(18B) 0.093(5) 0.050(4) 0.061(4) 0.019(4) 0.041(4) 0.006(3) C(19A) 0.039(3) 0.071(4) 0.041(4) 0.005(3) 0.009(3) 0.015(3) C(19B) 0.110(6) 0.077(5) 0.094(6) 0.026(4) 0.081(5) 0.026(4) C(21A) 0.028(3) 0.039(3) 0.039(3) 0.008(2) 0.020(2) 0.013(2) C(21B) 0.030(3) 0.056(3) 0.042(3) 0.003(3) 0.014(3) 0.011(3) C(22A) 0.034(3) 0.062(3) 0.051(4) 0.012(3) 0.028(3) 0.022(3) C(22B) 0.030(3) 0.063(4) 0.058(4) 0.004(3) 0.017(3) 0.017(3) C(23A) 0.036(3) 0.044(3) 0.037(3) 0.006(2) 0.027(3) 0.014(2) C(23B) 0.037(3) 0.047(3) 0.057(4) 0.008(3) 0.026(3) 0.019(3) C(24A) 0.029(3) 0.061(3) 0.047(3) 0.005(3) 0.019(3) 0.021(3) C(24B) 0.034(3) 0.076(4) 0.041(4) 0.005(3) 0.012(3) 0.007(3) C(25A) 0.041(4) 0.096(5) 0.062(5) 0.002(4) 0.016(3) 0.029(4) C(25B) 0.088(6) 0.060(4) 0.094(6) -0.006(4) 0.050(5) 0.001(4) C(26A) 0.074(5) 0.063(4) 0.081(5) 0.037(4) 0.043(4) 0.035(4) C(26B) 0.102(6) 0.085(5) 0.058(5) -0.004(4) 0.045(4) 0.008(4) C(27A) 0.042(3) 0.077(4) 0.054(4) 0.019(3) 0.033(3) 0.039(3) C(27B) 0.046(4) 0.064(4) 0.087(5) 0.015(3) 0.044(4) 0.013(4) C(28A) 0.21(1) 0.079(5) 0.049(5) -0.010(6) 0.046(6) 0.023(4) C(28B) 0.088(6) 0.112(6) 0.107(7) 0.024(5) 0.072(5) 0.034(5) C(29A) 0.29(1) 0.077(6) 0.060(6) 0.000(7) 0.055(7) 0.031(5) C(29B) 0.071(5) 0.106(6) 0.159(8) 0.046(5) 0.068(6) 0.060(6) C(31A) 0.037(3) 0.032(2) 0.030(3) 0.003(2) 0.021(2) 0.005(2) C(31B) 0.041(3) 0.037(3) 0.036(3) -0.001(2) 0.017(3) -0.003(2) C(32A) 0.050(3) 0.025(2) 0.048(3) 0.012(2) 0.028(3) 0.009(2) C(32B) 0.063(4) 0.031(3) 0.048(4) 0.005(3) 0.029(3) 0.003(3) C(33A) 0.039(3) 0.028(2) 0.042(3) 0.003(2) 0.024(3) 0.008(2) C(33B) 0.052(4) 0.032(3) 0.035(3) 0.011(3) 0.024(3) 0.009(2) C(34A) 0.052(4) 0.037(3) 0.038(3) 0.012(3) 0.023(3) 0.006(3) C(34B) 0.048(4) 0.044(3) 0.060(4) -0.005(3) 0.027(3) -0.003(3) C(35A) 0.103(6) 0.062(4) 0.052(4) 0.001(4) 0.022(4) -0.002(3) C(35B) 0.056(5) 0.085(5) 0.098(6) 0.009(4) 0.034(4) -0.002(4) C(36A) 0.088(5) 0.096(5) 0.056(4) 0.026(4) 0.048(4) 0.026(4) C(36B) 0.085(6) 0.103(6) 0.095(6) -0.005(5) 0.063(5) 0.025(5) C(37A) 0.062(4) 0.031(3) 0.046(3) 0.012(3) 0.028(3) 0.018(3) C(37B) 0.066(4) 0.030(3) 0.052(4) 0.011(3) 0.036(3) 0.007(3) C(38A) 0.107(6) 0.089(5) 0.102(6) 0.006(5) 0.050(5) 0.060(5) C(38B) 0.102(6) 0.060(4) 0.078(5) 0.018(4) 0.042(5) -0.017(4) C(39A) 0.088(6) 0.100(5) 0.101(6) 0.055(5) 0.049(5) 0.068(5) C(39B) 0.078(5) 0.051(3) 0.065(4) 0.030(3) 0.044(4) 0.027(3) C(40) 0.14(1) 0.143(9) 0.17(1) 0.029(8) 0.069(9) 0.085(8) C(41) 0.104(9) 0.150(10) 0.17(1) 0.020(8) 0.056(8) 0.040(9) C(42) 0.110(8) 0.111(7) 0.161(10) 0.020(6) 0.070(8) 0.056(7) C(43) 0.097(8) 0.19(1) 0.137(10) 0.033(8) 0.033(7) 0.008(8) C(44) 0.075(6) 0.093(6) 0.119(7) 0.005(5) 0.036(5) -0.004(5) C(45) 0.121(9) 0.100(7) 0.22(1) -0.025(7) 0.087(10) -0.036(8) C(46) 0.29(2) 0.27(2) 0.25(2) -0.13(2) 0.14(2) -0.03(2) C(47) 0.35(3) 0.110(10) 0.32(2) -0.10(1) 0.25(2) -0.08(1) C(48) 0.16(2) 0.33(2) 0.14(1) -0.08(1) 0.05(1) -0.06(1) C(49) 0.32(3) 0.54(5) 0.27(3) -0.26(3) 0.19(3) -0.21(3) B(1) 0.033(3) 0.034(3) 0.029(3) 0.003(3) 0.013(3) 0.016(3) B(2) 0.050(4) 0.032(3) 0.046(4) 0.013(3) 0.034(3) 0.010(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) Cr(1) 3.192(2) . 2_757 yes Cr(1) O(1) 2.020(4) . . yes Cr(1) O(1) 2.022(3) . 2_757 yes Cr(1) N(11A) 2.360(3) . . yes Cr(1) N(21A) 2.142(5) . . yes Cr(1) N(31A) 2.142(4) . . yes Cr(2) Cr(2) 3.153(2) . 2_666 yes Cr(2) O(2) 2.033(4) . . yes Cr(2) O(2) 1.979(4) . 2_666 yes Cr(2) N(11B) 2.412(5) . . yes Cr(2) N(21B) 2.152(4) . . yes Cr(2) N(31B) 2.124(4) . . yes N(11A) N(12A) 1.377(6) . . yes N(11A) C(11A) 1.336(6) . . yes N(11B) N(12B) 1.375(6) . . yes N(11B) C(11B) 1.335(8) . . yes N(12A) C(13A) 1.355(5) . . yes N(12A) B(1) 1.546(7) . . yes N(12B) C(13B) 1.360(9) . . yes N(12B) B(2) 1.540(8) . . yes N(21A) N(22A) 1.396(5) . . yes N(21A) C(21A) 1.342(7) . . yes N(21B) N(22B) 1.385(7) . . yes N(21B) C(21B) 1.346(6) . . yes N(22A) C(23A) 1.339(8) . . yes N(22A) B(1) 1.555(7) . . yes N(22B) C(23B) 1.357(7) . . yes N(22B) B(2) 1.552(6) . . yes N(31A) N(32A) 1.401(6) . . yes N(31A) C(31A) 1.333(6) . . yes N(31B) N(32B) 1.383(7) . . yes N(31B) C(31B) 1.349(8) . . yes N(32A) C(33A) 1.365(6) . . yes N(32A) B(1) 1.551(7) . . yes N(32B) C(33B) 1.355(6) . . yes N(32B) B(2) 1.549(9) . . yes C(11A) C(12A) 1.399(7) . . yes C(11A) C(14A) 1.501(8) . . yes C(11B) C(12B) 1.380(10) . . yes C(11B) C(14B) 1.505(8) . . yes C(12A) C(13A) 1.376(8) . . yes C(12B) C(13B) 1.379(8) . . yes C(13A) C(17A) 1.512(7) . . yes C(13B) C(17B) 1.518(9) . . yes C(14A) C(15A) 1.53(1) . . yes C(14A) C(16A) 1.513(8) . . yes C(14B) C(15B) 1.50(1) . . yes C(14B) C(16B) 1.50(1) . . yes C(17A) C(18A) 1.544(8) . . yes C(17A) C(19A) 1.533(6) . . yes C(17B) C(18B) 1.521(7) . . yes C(17B) C(19B) 1.52(1) . . yes C(21A) C(22A) 1.393(9) . . yes C(21A) C(24A) 1.519(7) . . yes C(21B) C(22B) 1.385(9) . . yes C(21B) C(24B) 1.507(9) . . yes C(22A) C(23A) 1.383(7) . . yes C(22B) C(23B) 1.370(8) . . yes C(23A) C(27A) 1.521(9) . . yes C(23B) C(27B) 1.51(1) . . yes C(24A) C(25A) 1.527(8) . . yes C(24A) C(26A) 1.521(8) . . yes C(24B) C(25B) 1.500(9) . . yes C(24B) C(26B) 1.54(1) . . yes C(27A) C(28A) 1.45(1) . . yes C(27A) C(29A) 1.46(1) . . yes C(27B) C(28B) 1.51(1) . . yes C(27B) C(29B) 1.538(9) . . yes C(31A) C(32A) 1.391(7) . . yes C(31A) C(34A) 1.515(8) . . yes C(31B) C(32B) 1.416(7) . . yes C(31B) C(34B) 1.51(1) . . yes C(32A) C(33A) 1.375(8) . . yes C(32B) C(33B) 1.38(1) . . yes C(33A) C(37A) 1.521(8) . . yes C(33B) C(37B) 1.501(9) . . yes C(34A) C(35A) 1.523(8) . . yes C(34A) C(36A) 1.54(1) . . yes C(34B) C(35B) 1.510(8) . . yes C(34B) C(36B) 1.51(1) . . yes C(37A) C(38A) 1.52(1) . . yes C(37A) C(39A) 1.51(1) . . yes C(37B) C(38B) 1.504(8) . . yes C(37B) C(39B) 1.528(7) . . yes C(40) C(41) 1.44(2) . . yes C(41) C(42) 1.48(2) . . yes C(42) C(43) 1.38(1) . . yes C(43) C(44) 1.42(2) . . yes C(45) C(46) 1.29(3) . . yes C(46) C(47) 1.22(3) . . yes C(47) C(49) 1.33(4) . . yes C(48) C(49) 1.07(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr(1) Cr(1) O(1) 37.88(9) 2_757 . . yes Cr(1) Cr(1) O(1) 37.8(1) 2_757 . 2_757 yes Cr(1) Cr(1) N(11A) 106.4(1) 2_757 . . yes Cr(1) Cr(1) N(21A) 136.6(1) 2_757 . . yes Cr(1) Cr(1) N(31A) 135.7(1) 2_757 . . yes O(1) Cr(1) O(1) 75.7(2) . . 2_757 yes O(1) Cr(1) N(11A) 104.4(2) . . . yes O(1) Cr(1) N(21A) 170.9(1) . . . yes O(1) Cr(1) N(31A) 98.4(2) . . . yes O(1) Cr(1) N(11A) 101.4(1) 2_757 . . yes O(1) Cr(1) N(21A) 99.3(2) 2_757 . . yes O(1) Cr(1) N(31A) 169.8(1) 2_757 . . yes N(11A) Cr(1) N(21A) 83.9(1) . . . yes N(11A) Cr(1) N(31A) 88.1(1) . . . yes N(21A) Cr(1) N(31A) 85.4(2) . . . yes Cr(2) Cr(2) O(2) 37.61(9) 2_666 . . yes Cr(2) Cr(2) O(2) 38.8(1) 2_666 . 2_666 yes Cr(2) Cr(2) N(11B) 110.1(1) 2_666 . . yes Cr(2) Cr(2) N(21B) 138.5(1) 2_666 . . yes Cr(2) Cr(2) N(31B) 131.8(1) 2_666 . . yes O(2) Cr(2) O(2) 76.4(1) . . 2_666 yes O(2) Cr(2) N(11B) 106.1(2) . . . yes O(2) Cr(2) N(21B) 172.0(2) . . . yes O(2) Cr(2) N(31B) 95.2(2) . . . yes O(2) Cr(2) N(11B) 105.2(2) 2_666 . . yes O(2) Cr(2) N(21B) 100.2(1) 2_666 . . yes O(2) Cr(2) N(31B) 165.7(2) 2_666 . . yes N(11B) Cr(2) N(21B) 81.7(2) . . . yes N(11B) Cr(2) N(31B) 88.2(2) . . . yes N(21B) Cr(2) N(31B) 86.6(2) . . . yes Cr(1) O(1) Cr(1) 104.3(2) . . 2_757 yes Cr(2) O(2) Cr(2) 103.6(1) . . 2_666 yes Cr(1) N(11A) N(12A) 114.4(2) . . . yes Cr(1) N(11A) C(11A) 139.6(3) . . . yes N(12A) N(11A) C(11A) 105.8(3) . . . yes Cr(2) N(11B) N(12B) 113.8(3) . . . yes Cr(2) N(11B) C(11B) 140.6(4) . . . yes N(12B) N(11B) C(11B) 105.6(5) . . . yes N(11A) N(12A) C(13A) 109.9(4) . . . yes N(11A) N(12A) B(1) 119.7(3) . . . yes C(13A) N(12A) B(1) 130.1(4) . . . yes N(11B) N(12B) C(13B) 109.7(4) . . . yes N(11B) N(12B) B(2) 118.6(5) . . . yes C(13B) N(12B) B(2) 131.1(5) . . . yes Cr(1) N(21A) N(22A) 118.2(3) . . . yes Cr(1) N(21A) C(21A) 136.4(3) . . . yes N(22A) N(21A) C(21A) 105.3(4) . . . yes Cr(2) N(21B) N(22B) 117.1(3) . . . yes Cr(2) N(21B) C(21B) 136.1(4) . . . yes N(22B) N(21B) C(21B) 106.0(4) . . . yes N(21A) N(22A) C(23A) 110.1(4) . . . yes N(21A) N(22A) B(1) 119.8(5) . . . yes C(23A) N(22A) B(1) 130.0(4) . . . yes N(21B) N(22B) C(23B) 109.4(4) . . . yes N(21B) N(22B) B(2) 121.0(4) . . . yes C(23B) N(22B) B(2) 129.5(5) . . . yes Cr(1) N(31A) N(32A) 117.4(3) . . . yes Cr(1) N(31A) C(31A) 136.6(3) . . . yes N(32A) N(31A) C(31A) 105.9(3) . . . yes Cr(2) N(31B) N(32B) 118.1(3) . . . yes Cr(2) N(31B) C(31B) 134.6(4) . . . yes N(32B) N(31B) C(31B) 107.3(4) . . . yes N(31A) N(32A) C(33A) 109.4(4) . . . yes N(31A) N(32A) B(1) 120.8(3) . . . yes C(33A) N(32A) B(1) 129.8(4) . . . yes N(31B) N(32B) C(33B) 109.4(5) . . . yes N(31B) N(32B) B(2) 120.7(4) . . . yes C(33B) N(32B) B(2) 129.9(5) . . . yes N(11A) C(11A) C(12A) 110.9(5) . . . yes N(11A) C(11A) C(14A) 121.2(4) . . . yes C(12A) C(11A) C(14A) 127.9(4) . . . yes N(11B) C(11B) C(12B) 111.6(5) . . . yes N(11B) C(11B) C(14B) 119.8(6) . . . yes C(12B) C(11B) C(14B) 128.6(6) . . . yes C(11A) C(12A) C(13A) 105.2(4) . . . yes C(11B) C(12B) C(13B) 105.3(6) . . . yes N(12A) C(13A) C(12A) 108.2(4) . . . yes N(12A) C(13A) C(17A) 122.9(4) . . . yes C(12A) C(13A) C(17A) 128.8(4) . . . yes N(12B) C(13B) C(12B) 107.8(5) . . . yes N(12B) C(13B) C(17B) 123.8(5) . . . yes C(12B) C(13B) C(17B) 128.4(6) . . . yes C(11A) C(14A) C(15A) 111.4(5) . . . yes C(11A) C(14A) C(16A) 110.6(6) . . . yes C(15A) C(14A) C(16A) 109.9(5) . . . yes C(11B) C(14B) C(15B) 110.9(5) . . . yes C(11B) C(14B) C(16B) 111.2(7) . . . yes C(15B) C(14B) C(16B) 108.9(7) . . . yes C(13A) C(17A) C(18A) 110.3(5) . . . yes C(13A) C(17A) C(19A) 111.4(4) . . . yes C(18A) C(17A) C(19A) 110.7(4) . . . yes C(13B) C(17B) C(18B) 111.0(6) . . . yes C(13B) C(17B) C(19B) 111.6(5) . . . yes C(18B) C(17B) C(19B) 110.8(6) . . . yes N(21A) C(21A) C(22A) 110.8(4) . . . yes N(21A) C(21A) C(24A) 121.6(5) . . . yes C(22A) C(21A) C(24A) 127.6(5) . . . yes N(21B) C(21B) C(22B) 110.1(5) . . . yes N(21B) C(21B) C(24B) 122.7(5) . . . yes C(22B) C(21B) C(24B) 127.2(4) . . . yes C(21A) C(22A) C(23A) 105.6(6) . . . yes C(21B) C(22B) C(23B) 106.5(4) . . . yes N(22A) C(23A) C(22A) 108.2(5) . . . yes N(22A) C(23A) C(27A) 124.5(5) . . . yes C(22A) C(23A) C(27A) 127.2(6) . . . yes N(22B) C(23B) C(22B) 107.9(5) . . . yes N(22B) C(23B) C(27B) 123.4(5) . . . yes C(22B) C(23B) C(27B) 128.6(5) . . . yes C(21A) C(24A) C(25A) 111.5(5) . . . yes C(21A) C(24A) C(26A) 110.0(4) . . . yes C(25A) C(24A) C(26A) 109.7(5) . . . yes C(21B) C(24B) C(25B) 111.7(6) . . . yes C(21B) C(24B) C(26B) 110.3(5) . . . yes C(25B) C(24B) C(26B) 110.3(5) . . . yes C(23A) C(27A) C(28A) 113.8(5) . . . yes C(23A) C(27A) C(29A) 111.3(5) . . . yes C(28A) C(27A) C(29A) 109.7(8) . . . yes C(23B) C(27B) C(28B) 110.8(6) . . . yes C(23B) C(27B) C(29B) 110.8(6) . . . yes C(28B) C(27B) C(29B) 110.5(6) . . . yes N(31A) C(31A) C(32A) 110.7(4) . . . yes N(31A) C(31A) C(34A) 122.3(4) . . . yes C(32A) C(31A) C(34A) 127.0(4) . . . yes N(31B) C(31B) C(32B) 108.8(6) . . . yes N(31B) C(31B) C(34B) 124.1(4) . . . yes C(32B) C(31B) C(34B) 127.2(5) . . . yes C(31A) C(32A) C(33A) 106.7(4) . . . yes C(31B) C(32B) C(33B) 106.2(5) . . . yes N(32A) C(33A) C(32A) 107.4(4) . . . yes N(32A) C(33A) C(37A) 124.2(5) . . . yes C(32A) C(33A) C(37A) 128.3(4) . . . yes N(32B) C(33B) C(32B) 108.3(5) . . . yes N(32B) C(33B) C(37B) 124.4(6) . . . yes C(32B) C(33B) C(37B) 127.2(4) . . . yes C(31A) C(34A) C(35A) 110.9(5) . . . yes C(31A) C(34A) C(36A) 109.8(4) . . . yes C(35A) C(34A) C(36A) 108.5(5) . . . yes C(31B) C(34B) C(35B) 110.4(6) . . . yes C(31B) C(34B) C(36B) 111.6(5) . . . yes C(35B) C(34B) C(36B) 110.4(6) . . . yes C(33A) C(37A) C(38A) 110.5(5) . . . yes C(33A) C(37A) C(39A) 110.6(6) . . . yes C(38A) C(37A) C(39A) 110.1(5) . . . yes C(33B) C(37B) C(38B) 111.7(6) . . . yes C(33B) C(37B) C(39B) 109.5(5) . . . yes C(38B) C(37B) C(39B) 111.7(4) . . . yes C(40) C(41) C(42) 117.1(9) . . . yes C(41) C(42) C(43) 121.1(9) . . . yes C(42) C(43) C(44) 122.6(9) . . . yes C(45) C(46) C(47) 147(2) . . . yes C(46) C(47) C(49) 151(2) . . . yes C(47) C(49) C(48) 145(3) . . . yes N(12A) B(1) N(22A) 109.8(4) . . . yes N(12A) B(1) N(32A) 111.5(5) . . . yes N(22A) B(1) N(32A) 108.9(3) . . . yes N(12B) B(2) N(22B) 109.0(4) . . . yes N(12B) B(2) N(32B) 111.5(4) . . . yes N(22B) B(2) N(32B) 110.7(6) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cr(1) Cr(1) 3.192(2) . 2_757 ? Cr(2) Cr(2) 3.153(2) . 2_666 ? #------------------------------------------------------------------------------ #===END data_compound_4 _database_code_CSD 217497 _audit_creation_date 'Tue May 27 23:55:12 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C67 H114 B2 Cr2 N16 O ' _chemical_formula_moiety 'C67 H114 B2 Cr2 N16 O ' _chemical_formula_weight 1285.36 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.7188(3) _cell_length_b 21.615(1) _cell_length_c 13.4270(8) _cell_angle_alpha 97.520(6) _cell_angle_beta 102.367(3) _cell_angle_gamma 108.213(4) _cell_volume 3872.4(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10131 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.968 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 26595 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15318 _reflns_number_gt 7631 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1999 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 7631 _refine_ls_number_parameters 767 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0120 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.52 _refine_diff_density_min -0.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.34825(5) 0.22318(3) 0.69040(5) 0.0337(2) Uani 1.00 d . . . Cr(2) Cr 0.16738(5) 0.24501(3) 0.49120(5) 0.0360(2) Uani 1.00 d . . . O(1) O 0.2041(2) 0.2058(2) 0.6174(3) 0.0444(8) Uani 1.00 d . . . N(11) N 0.3897(3) 0.2842(2) 0.8622(3) 0.0398(8) Uani 1.00 d . . . N(12) N 0.4738(3) 0.2792(2) 0.9237(3) 0.0383(8) Uani 1.00 d . . . N(21) N 0.4970(2) 0.2216(2) 0.7081(3) 0.0369(8) Uani 1.00 d . . . N(22) N 0.5487(2) 0.2191(2) 0.8058(3) 0.0370(8) Uani 1.00 d . . . N(31) N 0.3287(2) 0.1422(2) 0.7722(3) 0.0376(8) Uani 1.00 d . . . N(32) N 0.4017(2) 0.1538(2) 0.8635(3) 0.0369(8) Uani 1.00 d . . . N(41) N 0.1311(2) 0.1720(2) 0.3292(3) 0.0387(8) Uani 1.00 d . . . N(42) N 0.0663(2) 0.1832(2) 0.2490(3) 0.0376(8) Uani 1.00 d . . . N(51) N 0.1448(2) 0.3213(2) 0.4175(3) 0.0406(8) Uani 1.00 d . . . N(52) N 0.0817(3) 0.3041(2) 0.3177(3) 0.0436(9) Uani 1.00 d . . . N(61) N 0.0073(2) 0.2138(2) 0.4595(3) 0.0399(8) Uani 1.00 d . . . N(62) N -0.0439(2) 0.2082(2) 0.3567(3) 0.0389(8) Uani 1.00 d . . . N(71) N 0.3781(2) 0.3023(2) 0.6145(3) 0.0389(8) Uani 1.00 d . . . N(72) N 0.3210(2) 0.2854(2) 0.5103(3) 0.0395(8) Uani 1.00 d . . . N(81) N 0.893(1) 0.4226(7) 0.614(1) 0.28102(9) Uiso 1.00 d . . . N(82) N 0.6388(4) 0.0356(3) 0.4968(4) 0.09022(2) Uiso 1.00 d . . . C(11) C 0.3800(3) 0.3393(2) 0.9102(3) 0.044(1) Uani 1.00 d . . . C(12) C 0.4579(4) 0.3701(2) 1.0002(4) 0.051(1) Uani 1.00 d . . . C(13) C 0.5161(3) 0.3314(2) 1.0078(3) 0.045(1) Uani 1.00 d . . . C(14) C 0.2904(4) 0.3573(2) 0.8682(4) 0.057(1) Uani 1.00 d . . . C(15) C 0.3027(5) 0.4279(3) 0.9213(5) 0.080(2) Uani 1.00 d . . . C(16) C 0.1987(5) 0.3075(3) 0.8812(6) 0.103(2) Uani 1.00 d . . . C(17) C 0.6143(4) 0.3431(2) 1.0832(4) 0.056(1) Uani 1.00 d . . . C(18) C 0.6995(4) 0.3792(3) 1.0401(5) 0.087(2) Uani 1.00 d . . . C(19) C 0.6248(5) 0.3829(3) 1.1905(4) 0.086(2) Uani 1.00 d . . . C(21) C 0.5584(3) 0.2220(2) 0.6468(3) 0.042(1) Uani 1.00 d . . . C(22) C 0.6483(3) 0.2206(2) 0.7046(4) 0.051(1) Uani 1.00 d . . . C(23) C 0.6396(3) 0.2182(2) 0.8045(4) 0.045(1) Uani 1.00 d . . . C(24) C 0.5277(4) 0.2202(2) 0.5307(4) 0.050(1) Uani 1.00 d . . . C(25) C 0.6127(4) 0.2649(3) 0.4950(4) 0.073(2) Uani 1.00 d . . . C(26) C 0.4963(4) 0.1484(3) 0.4701(4) 0.068(1) Uani 1.00 d . . . C(27) C 0.7132(4) 0.2139(3) 0.8987(4) 0.058(1) Uani 1.00 d . . . C(28) C 0.8200(4) 0.2481(4) 0.8984(5) 0.095(2) Uani 1.00 d . . . C(29) C 0.6934(5) 0.1410(3) 0.9057(5) 0.085(2) Uani 1.00 d . . . C(31) C 0.2558(3) 0.0844(2) 0.7682(3) 0.042(1) Uani 1.00 d . . . C(32) C 0.2834(3) 0.0597(2) 0.8563(3) 0.047(1) Uani 1.00 d . . . C(33) C 0.3740(3) 0.1038(2) 0.9158(3) 0.0394(10) Uani 1.00 d . . . C(34) C 0.1603(3) 0.0567(2) 0.6839(4) 0.052(1) Uani 1.00 d . . . C(35) C 0.0777(4) 0.0692(3) 0.7255(5) 0.085(2) Uani 1.00 d . . . C(36) C 0.1321(4) -0.0174(2) 0.6393(4) 0.065(1) Uani 1.00 d . . . C(37) C 0.4343(3) 0.1038(2) 1.0222(3) 0.047(1) Uani 1.00 d . . . C(38) C 0.4259(4) 0.1557(3) 1.1057(4) 0.063(1) Uani 1.00 d . . . C(39) C 0.4003(4) 0.0345(3) 1.0467(4) 0.062(1) Uani 1.00 d . . . C(41) C 0.1616(3) 0.1255(2) 0.2860(3) 0.040(1) Uani 1.00 d . . . C(42) C 0.1170(4) 0.1062(2) 0.1786(4) 0.055(1) Uani 1.00 d . . . C(43) C 0.0564(4) 0.1432(2) 0.1572(3) 0.048(1) Uani 1.00 d . . . C(44) C 0.2325(3) 0.0990(2) 0.3507(3) 0.046(1) Uani 1.00 d . . . C(45) C 0.1909(5) 0.0686(3) 0.4319(5) 0.081(2) Uani 1.00 d . . . C(46) C 0.2606(5) 0.0496(3) 0.2839(4) 0.083(2) Uani 1.00 d . . . C(47) C -0.0104(4) 0.1414(3) 0.0528(4) 0.061(1) Uani 1.00 d . . . C(48) C -0.0880(6) 0.0754(3) 0.0076(7) 0.148(4) Uani 1.00 d . . . C(49) C 0.0512(8) 0.1602(7) -0.0190(7) 0.240(7) Uani 1.00 d . . . C(51) C 0.1842(3) 0.3883(2) 0.4434(3) 0.045(1) Uani 1.00 d . . . C(52) C 0.1477(4) 0.4144(2) 0.3595(4) 0.055(1) Uani 1.00 d . . . C(53) C 0.0840(4) 0.3604(2) 0.2811(4) 0.050(1) Uani 1.00 d . . . C(54) C 0.2533(4) 0.4247(2) 0.5500(4) 0.054(1) Uani 1.00 d . . . C(55) C 0.3237(4) 0.4928(3) 0.5488(4) 0.074(2) Uani 1.00 d . . . C(56) C 0.1924(5) 0.4316(3) 0.6275(4) 0.083(2) Uani 1.00 d . . . C(57) C 0.0303(4) 0.3597(3) 0.1719(4) 0.065(1) Uani 1.00 d . . . C(58) C 0.0968(7) 0.3627(7) 0.1033(6) 0.198(6) Uani 1.00 d . . . C(59) C -0.0081(7) 0.4173(4) 0.1701(6) 0.136(3) Uani 1.00 d . . . C(61) C -0.0628(3) 0.1953(2) 0.5104(3) 0.044(1) Uani 1.00 d . . . C(62) C -0.1574(3) 0.1769(2) 0.4423(4) 0.051(1) Uani 1.00 d . . . C(63) C -0.1433(3) 0.1854(2) 0.3458(3) 0.041(1) Uani 1.00 d . . . C(64) C -0.0377(3) 0.2007(3) 0.6268(4) 0.065(2) Uani 1.00 d . . . C(65) C -0.1135(4) 0.1425(3) 0.6546(4) 0.070(1) Uani 1.00 d . . . C(66) C -0.0392(5) 0.2674(3) 0.6813(5) 0.101(2) Uani 1.00 d . . . C(67) C -0.2216(3) 0.1714(2) 0.2434(4) 0.052(1) Uani 1.00 d . . . C(68) C -0.3161(4) 0.1143(3) 0.2390(4) 0.074(2) Uani 1.00 d . . . C(69) C -0.2447(4) 0.2323(3) 0.2244(4) 0.079(2) Uani 1.00 d . . . C(71) C 0.4634(3) 0.3535(2) 0.6237(3) 0.043(1) Uani 1.00 d . . . C(72) C 0.4628(3) 0.3691(2) 0.5258(4) 0.048(1) Uani 1.00 d . . . C(73) C 0.3740(3) 0.3252(2) 0.4565(3) 0.043(1) Uani 1.00 d . . . C(74) C 0.5359(3) 0.3889(2) 0.7287(4) 0.049(1) Uani 1.00 d . . . C(75) C 0.5160(4) 0.4502(3) 0.7716(4) 0.074(2) Uani 1.00 d . . . C(76) C 0.6441(4) 0.4070(3) 0.7267(5) 0.078(2) Uani 1.00 d . . . C(77) C 0.3395(3) 0.3169(2) 0.3399(4) 0.049(1) Uani 1.00 d . . . C(78) C 0.3711(4) 0.3827(3) 0.3050(4) 0.063(1) Uani 1.00 d . . . C(79) C 0.3776(4) 0.2683(3) 0.2835(4) 0.068(2) Uani 1.00 d . . . C(80) C 0.897(1) 0.4067(9) 0.534(2) 0.25641(9) Uiso 1.00 d . . . C(81) C 0.9144(8) 0.3723(5) 0.4534(9) 0.17290(5) Uiso 1.00 d . . . C(82) C 0.5909(4) 0.0016(3) 0.4193(5) 0.06780(2) Uiso 1.00 d . . . C(83) C 0.5271(5) -0.0426(3) 0.3230(5) 0.09402(2) Uiso 1.00 d . . . B(1) B 0.4982(3) 0.2159(2) 0.8964(4) 0.037(1) Uani 1.00 d . . . B(2) B 0.0119(4) 0.2301(2) 0.2743(4) 0.041(1) Uani 1.00 d . . . H(1) H 0.164(4) 0.188(3) 0.633(5) 0.0913(3) Uiso 1.00 calc . . . H(2) H 0.5441 0.2116 0.9576 0.0461 Uiso 1.00 calc . . . H(3) H 0.4661 0.4105 1.0496 0.0608 Uiso 1.00 calc . . . H(4) H 0.2824 0.3551 0.7943 0.0738 Uiso 1.00 calc . . . H(5) H 0.3056 0.4293 0.9938 0.0801 Uiso 1.00 calc . . . H(6) H 0.2474 0.4392 0.8883 0.0801 Uiso 1.00 calc . . . H(7) H 0.3632 0.4590 0.9154 0.0801 Uiso 1.00 calc . . . H(8) H 0.1419 0.3186 0.8526 0.1032 Uiso 1.00 calc . . . H(9) H 0.2055 0.3081 0.9542 0.1032 Uiso 1.00 calc . . . H(10) H 0.1905 0.2637 0.8456 0.1032 Uiso 1.00 calc . . . H(11) H 0.6190 0.2998 1.0925 0.0705 Uiso 1.00 calc . . . H(12) H 0.7617 0.3839 1.0862 0.0870 Uiso 1.00 calc . . . H(13) H 0.6977 0.4229 1.0342 0.0870 Uiso 1.00 calc . . . H(14) H 0.6922 0.3545 0.9723 0.0870 Uiso 1.00 calc . . . H(15) H 0.6882 0.3892 1.2364 0.0862 Uiso 1.00 calc . . . H(16) H 0.5729 0.3587 1.2186 0.0862 Uiso 1.00 calc . . . H(17) H 0.6196 0.4253 1.1838 0.0862 Uiso 1.00 calc . . . H(18) H 0.2456 0.0183 0.8716 0.0550 Uiso 1.00 calc . . . H(19) H 0.1676 0.0810 0.6278 0.0666 Uiso 1.00 calc . . . H(20) H 0.0991 0.1155 0.7595 0.0846 Uiso 1.00 calc . . . H(21) H 0.0627 0.0419 0.7748 0.0846 Uiso 1.00 calc . . . H(22) H 0.0194 0.0588 0.6688 0.0846 Uiso 1.00 calc . . . H(23) H 0.0740 -0.0319 0.5811 0.0649 Uiso 1.00 calc . . . H(24) H 0.1190 -0.0421 0.6919 0.0649 Uiso 1.00 calc . . . H(25) H 0.1861 -0.0247 0.6161 0.0649 Uiso 1.00 calc . . . H(26) H 0.5032 0.1168 1.0224 0.0581 Uiso 1.00 calc . . . H(27) H 0.4598 0.1528 1.1734 0.0631 Uiso 1.00 calc . . . H(28) H 0.3570 0.1472 1.1020 0.0631 Uiso 1.00 calc . . . H(29) H 0.4553 0.1994 1.0938 0.0631 Uiso 1.00 calc . . . H(30) H 0.3319 0.0218 1.0479 0.0619 Uiso 1.00 calc . . . H(31) H 0.4405 0.0349 1.1136 0.0619 Uiso 1.00 calc . . . H(32) H 0.4069 0.0028 0.9940 0.0619 Uiso 1.00 calc . . . H(33) H 0.7046 0.2193 0.6783 0.0631 Uiso 1.00 calc . . . H(34) H 0.4703 0.2345 0.5151 0.0666 Uiso 1.00 calc . . . H(35) H 0.6680 0.2498 0.5082 0.0732 Uiso 1.00 calc . . . H(36) H 0.6325 0.3100 0.5323 0.0732 Uiso 1.00 calc . . . H(37) H 0.5904 0.2627 0.4214 0.0732 Uiso 1.00 calc . . . H(38) H 0.4423 0.1203 0.4911 0.0684 Uiso 1.00 calc . . . H(39) H 0.5515 0.1331 0.4847 0.0684 Uiso 1.00 calc . . . H(40) H 0.4757 0.1468 0.3967 0.0684 Uiso 1.00 calc . . . H(41) H 0.7026 0.2366 0.9606 0.0756 Uiso 1.00 calc . . . H(42) H 0.8636 0.2468 0.9620 0.0955 Uiso 1.00 calc . . . H(43) H 0.8308 0.2932 0.8927 0.0955 Uiso 1.00 calc . . . H(44) H 0.8331 0.2248 0.8400 0.0955 Uiso 1.00 calc . . . H(45) H 0.6248 0.1194 0.9016 0.0851 Uiso 1.00 calc . . . H(46) H 0.7341 0.1388 0.9703 0.0851 Uiso 1.00 calc . . . H(47) H 0.7096 0.1187 0.8485 0.0851 Uiso 1.00 calc . . . H(48) H -0.0375 0.2278 0.2115 0.0533 Uiso 1.00 calc . . . H(49) H 0.1260 0.0725 0.1289 0.0650 Uiso 1.00 calc . . . H(50) H 0.2925 0.1357 0.3867 0.0591 Uiso 1.00 calc . . . H(51) H 0.1681 0.0989 0.4695 0.0810 Uiso 1.00 calc . . . H(52) H 0.2418 0.0596 0.4796 0.0810 Uiso 1.00 calc . . . H(53) H 0.1365 0.0278 0.3993 0.0810 Uiso 1.00 calc . . . H(54) H 0.2013 0.0138 0.2426 0.0822 Uiso 1.00 calc . . . H(55) H 0.3020 0.0318 0.3280 0.0822 Uiso 1.00 calc . . . H(56) H 0.2958 0.0716 0.2386 0.0822 Uiso 1.00 calc . . . H(57) H -0.0428 0.1736 0.0641 0.0747 Uiso 1.00 calc . . . H(58) H -0.1259 0.0627 0.0560 0.1489 Uiso 1.00 calc . . . H(59) H -0.0574 0.0432 -0.0076 0.1489 Uiso 1.00 calc . . . H(60) H -0.1310 0.0772 -0.0560 0.1489 Uiso 1.00 calc . . . H(61) H 0.0615 0.1220 -0.0514 0.2413 Uiso 1.00 calc . . . H(62) H 0.1136 0.1938 0.0194 0.2413 Uiso 1.00 calc . . . H(63) H 0.0174 0.1780 -0.0714 0.2413 Uiso 1.00 calc . . . H(64) H 0.1641 0.4610 0.3569 0.0667 Uiso 1.00 calc . . . H(65) H 0.2915 0.3976 0.5752 0.0699 Uiso 1.00 calc . . . H(66) H 0.3696 0.5124 0.6166 0.0739 Uiso 1.00 calc . . . H(67) H 0.2864 0.5209 0.5306 0.0739 Uiso 1.00 calc . . . H(68) H 0.3598 0.4881 0.4983 0.0739 Uiso 1.00 calc . . . H(69) H 0.2357 0.4484 0.6969 0.0832 Uiso 1.00 calc . . . H(70) H 0.1445 0.3886 0.6237 0.0832 Uiso 1.00 calc . . . H(71) H 0.1583 0.4616 0.6102 0.0832 Uiso 1.00 calc . . . H(72) H -0.0275 0.3180 0.1475 0.0852 Uiso 1.00 calc . . . H(73) H 0.1339 0.3345 0.1182 0.1991 Uiso 1.00 calc . . . H(74) H 0.1421 0.4084 0.1161 0.1991 Uiso 1.00 calc . . . H(75) H 0.0584 0.3496 0.0320 0.1991 Uiso 1.00 calc . . . H(76) H 0.0478 0.4591 0.1949 0.1361 Uiso 1.00 calc . . . H(77) H -0.0513 0.4152 0.2144 0.1361 Uiso 1.00 calc . . . H(78) H -0.0428 0.4156 0.1001 0.1361 Uiso 1.00 calc . . . H(79) H -0.2216 0.1611 0.4589 0.0620 Uiso 1.00 calc . . . H(80) H 0.0290 0.2001 0.6532 0.0830 Uiso 1.00 calc . . . H(81) H -0.1781 0.1460 0.6361 0.0698 Uiso 1.00 calc . . . H(82) H -0.0936 0.1441 0.7281 0.0698 Uiso 1.00 calc . . . H(83) H -0.1160 0.1008 0.6166 0.0698 Uiso 1.00 calc . . . H(84) H -0.0218 0.2713 0.7554 0.1006 Uiso 1.00 calc . . . H(85) H -0.1050 0.2691 0.6586 0.1006 Uiso 1.00 calc . . . H(86) H 0.0072 0.3036 0.6635 0.1006 Uiso 1.00 calc . . . H(87) H -0.1949 0.1572 0.1878 0.0656 Uiso 1.00 calc . . . H(88) H -0.3503 0.1294 0.2846 0.0742 Uiso 1.00 calc . . . H(89) H -0.2989 0.0779 0.2604 0.0742 Uiso 1.00 calc . . . H(90) H -0.3582 0.0999 0.1688 0.0742 Uiso 1.00 calc . . . H(91) H -0.1843 0.2684 0.2314 0.0792 Uiso 1.00 calc . . . H(92) H -0.2774 0.2445 0.2745 0.0792 Uiso 1.00 calc . . . H(93) H -0.2876 0.2232 0.1553 0.0792 Uiso 1.00 calc . . . H(94) H 0.5125 0.4043 0.5096 0.0587 Uiso 1.00 calc . . . H(95) H 0.5257 0.3580 0.7755 0.0621 Uiso 1.00 calc . . . H(96) H 0.5598 0.4706 0.8405 0.0742 Uiso 1.00 calc . . . H(97) H 0.4484 0.4377 0.7752 0.0742 Uiso 1.00 calc . . . H(98) H 0.5274 0.4815 0.7270 0.0742 Uiso 1.00 calc . . . H(99) H 0.6589 0.3671 0.7127 0.0785 Uiso 1.00 calc . . . H(100) H 0.6866 0.4341 0.7929 0.0785 Uiso 1.00 calc . . . H(101) H 0.6551 0.4315 0.6728 0.0785 Uiso 1.00 calc . . . H(102) H 0.2679 0.2979 0.3188 0.0631 Uiso 1.00 calc . . . H(103) H 0.4421 0.4034 0.3277 0.0629 Uiso 1.00 calc . . . H(104) H 0.3416 0.4119 0.3347 0.0629 Uiso 1.00 calc . . . H(105) H 0.3493 0.3748 0.2301 0.0629 Uiso 1.00 calc . . . H(106) H 0.3569 0.2265 0.3039 0.0677 Uiso 1.00 calc . . . H(107) H 0.4492 0.2864 0.3013 0.0677 Uiso 1.00 calc . . . H(108) H 0.3517 0.2620 0.2093 0.0677 Uiso 1.00 calc . . . H(109) H 0.8814 0.3235 0.4399 0.1939 Uiso 1.00 calc . . . H(110) H 0.8967 0.3838 0.3859 0.1939 Uiso 1.00 calc . . . H(111) H 0.9858 0.3782 0.4654 0.1939 Uiso 1.00 calc . . . H(112) H 0.4665 -0.0334 0.3002 0.1089 Uiso 1.00 calc . . . H(113) H 0.5588 -0.0390 0.2671 0.1089 Uiso 1.00 calc . . . H(114) H 0.5073 -0.0887 0.3287 0.1089 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0317(4) 0.0339(4) 0.0321(4) 0.0074(3) 0.0078(3) 0.0067(3) Cr(2) 0.0337(4) 0.0364(4) 0.0295(4) 0.0053(3) 0.0047(3) 0.0024(3) O(1) 0.033(2) 0.051(2) 0.044(2) 0.009(1) 0.005(2) 0.018(2) N(11) 0.043(2) 0.039(2) 0.037(2) 0.015(2) 0.010(2) 0.003(2) N(12) 0.041(2) 0.038(2) 0.032(2) 0.010(2) 0.009(2) 0.003(2) N(21) 0.036(2) 0.040(2) 0.033(2) 0.012(2) 0.008(2) 0.006(2) N(22) 0.036(2) 0.038(2) 0.034(2) 0.012(2) 0.007(2) 0.004(2) N(31) 0.035(2) 0.040(2) 0.034(2) 0.011(2) 0.005(2) 0.007(2) N(32) 0.041(2) 0.037(2) 0.032(2) 0.014(2) 0.010(2) 0.010(2) N(41) 0.035(2) 0.043(2) 0.032(2) 0.011(2) 0.004(2) 0.002(2) N(42) 0.037(2) 0.040(2) 0.032(2) 0.012(2) 0.008(2) 0.002(2) N(51) 0.039(2) 0.038(2) 0.035(2) 0.009(2) 0.003(2) 0.001(2) N(52) 0.043(2) 0.045(2) 0.035(2) 0.013(2) 0.000(2) 0.004(2) N(61) 0.037(2) 0.048(2) 0.027(2) 0.010(2) 0.005(2) 0.000(2) N(62) 0.035(2) 0.044(2) 0.028(2) 0.008(2) 0.003(2) 0.001(2) N(71) 0.033(2) 0.043(2) 0.035(2) 0.009(2) 0.005(2) 0.008(2) N(72) 0.038(2) 0.042(2) 0.034(2) 0.009(2) 0.009(2) 0.009(2) C(11) 0.047(3) 0.044(2) 0.036(3) 0.015(2) 0.010(2) 0.004(2) C(12) 0.064(3) 0.040(2) 0.050(3) 0.020(2) 0.019(3) -0.001(2) C(13) 0.048(3) 0.040(2) 0.038(3) 0.007(2) 0.008(2) 0.002(2) C(14) 0.068(3) 0.063(3) 0.046(3) 0.035(3) 0.012(3) 0.004(2) C(15) 0.094(4) 0.080(4) 0.074(4) 0.052(3) 0.012(3) 0.005(3) C(16) 0.060(4) 0.100(5) 0.150(7) 0.033(4) 0.033(4) 0.008(5) C(17) 0.057(3) 0.046(3) 0.048(3) 0.011(2) -0.004(2) -0.006(2) C(18) 0.049(3) 0.095(4) 0.093(5) 0.012(3) 0.007(3) -0.008(4) C(19) 0.082(4) 0.085(4) 0.053(4) 0.006(3) -0.005(3) -0.017(3) C(21) 0.046(3) 0.046(3) 0.039(3) 0.017(2) 0.019(2) 0.011(2) C(22) 0.043(3) 0.065(3) 0.051(3) 0.020(2) 0.017(2) 0.014(2) C(23) 0.038(3) 0.054(3) 0.046(3) 0.018(2) 0.014(2) 0.010(2) C(24) 0.056(3) 0.067(3) 0.041(3) 0.033(2) 0.021(2) 0.016(2) C(25) 0.077(4) 0.102(4) 0.063(4) 0.039(3) 0.041(3) 0.040(3) C(26) 0.076(4) 0.097(4) 0.043(3) 0.047(3) 0.014(3) 0.014(3) C(27) 0.044(3) 0.087(4) 0.048(3) 0.031(3) 0.014(2) 0.013(3) C(28) 0.043(3) 0.170(7) 0.068(4) 0.037(4) 0.008(3) 0.019(4) C(29) 0.089(5) 0.105(5) 0.071(4) 0.061(4) 0.004(3) 0.020(4) C(31) 0.045(3) 0.033(2) 0.042(3) 0.008(2) 0.011(2) 0.006(2) C(32) 0.052(3) 0.041(2) 0.043(3) 0.009(2) 0.011(2) 0.014(2) C(33) 0.042(2) 0.041(2) 0.035(2) 0.012(2) 0.012(2) 0.009(2) C(34) 0.048(3) 0.044(3) 0.049(3) 0.004(2) 0.001(2) 0.014(2) C(35) 0.051(3) 0.075(4) 0.108(5) 0.017(3) -0.001(3) -0.001(4) C(36) 0.064(3) 0.048(3) 0.058(3) 0.006(2) -0.007(3) 0.002(3) C(37) 0.051(3) 0.050(3) 0.036(3) 0.012(2) 0.011(2) 0.013(2) C(38) 0.070(4) 0.074(3) 0.039(3) 0.018(3) 0.014(3) 0.011(3) C(39) 0.070(3) 0.070(3) 0.047(3) 0.026(3) 0.008(3) 0.028(3) C(41) 0.045(3) 0.037(2) 0.029(2) 0.005(2) 0.012(2) 0.001(2) C(42) 0.079(4) 0.052(3) 0.037(3) 0.031(3) 0.015(3) 0.000(2) C(43) 0.061(3) 0.044(3) 0.029(2) 0.011(2) 0.010(2) -0.001(2) C(44) 0.050(3) 0.045(3) 0.040(3) 0.016(2) 0.011(2) 0.004(2) C(45) 0.096(4) 0.100(4) 0.084(4) 0.058(4) 0.048(4) 0.052(4) C(46) 0.118(5) 0.106(5) 0.052(4) 0.075(4) 0.027(4) 0.016(3) C(47) 0.083(4) 0.071(3) 0.027(3) 0.036(3) 0.006(3) 0.000(2) C(48) 0.130(7) 0.085(5) 0.137(7) 0.001(4) -0.089(6) 0.014(5) C(49) 0.154(9) 0.47(2) 0.073(6) 0.06(1) 0.003(6) 0.144(10) C(51) 0.048(3) 0.035(2) 0.042(3) 0.009(2) 0.005(2) 0.001(2) C(52) 0.063(3) 0.044(3) 0.051(3) 0.014(2) 0.007(3) 0.009(2) C(53) 0.063(3) 0.045(3) 0.042(3) 0.023(2) 0.009(2) 0.010(2) C(54) 0.060(3) 0.044(3) 0.047(3) 0.014(2) 0.008(2) 0.000(2) C(55) 0.076(4) 0.055(3) 0.059(4) -0.007(3) 0.009(3) -0.007(3) C(56) 0.092(4) 0.079(4) 0.052(4) 0.003(3) 0.016(3) -0.005(3) C(57) 0.072(4) 0.064(3) 0.048(3) 0.014(3) -0.001(3) 0.024(3) C(58) 0.183(9) 0.45(2) 0.071(5) 0.20(1) 0.069(6) 0.127(9) C(59) 0.168(8) 0.162(7) 0.090(6) 0.108(7) -0.021(5) 0.035(5) C(61) 0.036(2) 0.062(3) 0.032(2) 0.016(2) 0.009(2) 0.004(2) C(62) 0.040(3) 0.072(3) 0.038(3) 0.016(2) 0.013(2) 0.008(2) C(63) 0.036(2) 0.047(2) 0.037(3) 0.013(2) 0.006(2) 0.003(2) C(64) 0.041(3) 0.116(5) 0.042(3) 0.024(3) 0.020(2) 0.019(3) C(65) 0.079(4) 0.092(4) 0.043(3) 0.034(3) 0.015(3) 0.024(3) C(66) 0.095(5) 0.106(5) 0.055(4) -0.021(4) 0.029(4) -0.016(4) C(67) 0.041(3) 0.072(3) 0.044(3) 0.020(2) 0.011(2) 0.018(2) C(68) 0.052(3) 0.086(4) 0.066(4) 0.013(3) -0.005(3) 0.018(3) C(69) 0.072(4) 0.091(4) 0.068(4) 0.030(3) 0.001(3) 0.026(3) C(71) 0.033(2) 0.038(2) 0.047(3) 0.002(2) 0.006(2) 0.008(2) C(72) 0.043(3) 0.047(3) 0.047(3) 0.004(2) 0.013(2) 0.016(2) C(73) 0.042(3) 0.048(3) 0.039(3) 0.012(2) 0.015(2) 0.010(2) C(74) 0.042(3) 0.043(2) 0.045(3) -0.003(2) 0.004(2) 0.010(2) C(75) 0.087(4) 0.052(3) 0.063(4) 0.009(3) 0.007(3) 0.002(3) C(76) 0.042(3) 0.085(4) 0.077(4) -0.002(3) -0.005(3) 0.009(3) C(77) 0.045(3) 0.053(3) 0.042(3) 0.005(2) 0.016(2) 0.013(2) C(78) 0.078(4) 0.069(3) 0.052(3) 0.030(3) 0.026(3) 0.024(3) C(79) 0.091(4) 0.060(3) 0.055(3) 0.022(3) 0.031(3) 0.014(3) B(1) 0.034(3) 0.035(2) 0.038(3) 0.009(2) 0.009(2) 0.008(2) B(2) 0.042(3) 0.046(3) 0.023(3) 0.008(2) 0.000(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) O(1) 2.029(3) . . yes Cr(1) N(11) 2.353(3) . . yes Cr(1) N(21) 2.162(4) . . yes Cr(1) N(31) 2.162(4) . . yes Cr(1) N(71) 2.082(4) . . yes Cr(2) O(1) 2.038(4) . . yes Cr(2) N(41) 2.364(3) . . yes Cr(2) N(51) 2.106(4) . . yes Cr(2) N(61) 2.165(3) . . yes Cr(2) N(72) 2.097(3) . . yes N(11) N(12) 1.377(5) . . yes N(11) C(11) 1.340(6) . . yes N(12) C(13) 1.364(5) . . yes N(12) B(1) 1.540(7) . . yes N(21) N(22) 1.385(5) . . yes N(21) C(21) 1.345(6) . . yes N(22) C(23) 1.348(6) . . yes N(22) B(1) 1.553(7) . . yes N(31) N(32) 1.381(4) . . yes N(31) C(31) 1.355(5) . . yes N(32) C(33) 1.369(6) . . yes N(32) B(1) 1.548(5) . . yes N(41) N(42) 1.378(5) . . yes N(41) C(41) 1.337(6) . . yes N(42) C(43) 1.361(6) . . yes N(42) B(2) 1.523(7) . . yes N(51) N(52) 1.384(4) . . yes N(51) C(51) 1.346(5) . . yes N(52) C(53) 1.364(6) . . yes N(52) B(2) 1.557(5) . . yes N(61) N(62) 1.394(4) . . yes N(61) C(61) 1.345(6) . . yes N(62) C(63) 1.358(5) . . yes N(62) B(2) 1.551(7) . . yes N(71) N(72) 1.404(4) . . yes N(71) C(71) 1.358(5) . . yes N(72) C(73) 1.362(6) . . yes N(81) C(80) 1.12(3) . . yes N(82) C(82) 1.133(7) . . yes C(11) C(12) 1.392(6) . . yes C(11) C(14) 1.507(8) . . yes C(12) C(13) 1.370(8) . . yes C(13) C(17) 1.502(6) . . yes C(14) C(15) 1.534(8) . . yes C(14) C(16) 1.501(8) . . yes C(17) C(18) 1.529(8) . . yes C(17) C(19) 1.529(8) . . yes C(21) C(22) 1.395(7) . . yes C(21) C(24) 1.520(6) . . yes C(22) C(23) 1.380(7) . . yes C(23) C(27) 1.512(7) . . yes C(24) C(25) 1.533(8) . . yes C(24) C(26) 1.531(7) . . yes C(27) C(28) 1.515(8) . . yes C(27) C(29) 1.531(9) . . yes C(31) C(32) 1.393(7) . . yes C(31) C(34) 1.495(6) . . yes C(32) C(33) 1.370(5) . . yes C(33) C(37) 1.512(6) . . yes C(34) C(35) 1.522(9) . . yes C(34) C(36) 1.524(6) . . yes C(37) C(38) 1.531(7) . . yes C(37) C(39) 1.528(7) . . yes C(41) C(42) 1.397(6) . . yes C(41) C(44) 1.512(7) . . yes C(42) C(43) 1.384(8) . . yes C(43) C(47) 1.519(7) . . yes C(44) C(45) 1.490(8) . . yes C(44) C(46) 1.516(9) . . yes C(47) C(48) 1.472(7) . . yes C(47) C(49) 1.47(1) . . yes C(51) C(52) 1.405(7) . . yes C(51) C(54) 1.512(6) . . yes C(52) C(53) 1.386(5) . . yes C(53) C(57) 1.505(7) . . yes C(54) C(55) 1.517(7) . . yes C(54) C(56) 1.533(9) . . yes C(57) C(58) 1.47(1) . . yes C(57) C(59) 1.52(1) . . yes C(61) C(62) 1.395(6) . . yes C(61) C(64) 1.507(7) . . yes C(62) C(63) 1.381(7) . . yes C(63) C(67) 1.518(6) . . yes C(64) C(65) 1.546(8) . . yes C(64) C(66) 1.539(10) . . yes C(67) C(68) 1.528(7) . . yes C(67) C(69) 1.498(9) . . yes C(71) C(72) 1.398(7) . . yes C(71) C(74) 1.508(5) . . yes C(72) C(73) 1.395(5) . . yes C(73) C(77) 1.507(6) . . yes C(74) C(75) 1.513(8) . . yes C(74) C(76) 1.523(7) . . yes C(77) C(78) 1.521(7) . . yes C(77) C(79) 1.527(8) . . yes C(80) C(81) 1.34(2) . . yes C(82) C(83) 1.436(8) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cr(1) N(11) 110.2(1) . . . yes O(1) Cr(1) N(21) 157.5(1) . . . yes O(1) Cr(1) N(31) 99.6(1) . . . yes O(1) Cr(1) N(71) 84.5(1) . . . yes N(11) Cr(1) N(21) 92.3(1) . . . yes N(11) Cr(1) N(31) 80.5(1) . . . yes N(11) Cr(1) N(71) 98.9(1) . . . yes N(21) Cr(1) N(31) 84.5(1) . . . yes N(21) Cr(1) N(71) 91.4(1) . . . yes N(31) Cr(1) N(71) 175.8(1) . . . yes O(1) Cr(2) N(41) 114.0(1) . . . yes O(1) Cr(2) N(51) 154.1(1) . . . yes O(1) Cr(2) N(61) 102.1(1) . . . yes O(1) Cr(2) N(72) 85.3(1) . . . yes N(41) Cr(2) N(51) 91.9(1) . . . yes N(41) Cr(2) N(61) 83.9(1) . . . yes N(41) Cr(2) N(72) 95.7(1) . . . yes N(51) Cr(2) N(61) 81.0(1) . . . yes N(51) Cr(2) N(72) 91.1(1) . . . yes N(61) Cr(2) N(72) 172.1(1) . . . yes Cr(1) O(1) Cr(2) 121.0(2) . . . yes Cr(1) N(11) N(12) 111.7(3) . . . yes Cr(1) N(11) C(11) 137.3(3) . . . yes N(12) N(11) C(11) 105.9(3) . . . yes N(11) N(12) C(13) 110.2(4) . . . yes N(11) N(12) B(1) 118.5(3) . . . yes C(13) N(12) B(1) 131.0(4) . . . yes Cr(1) N(21) N(22) 117.4(3) . . . yes Cr(1) N(21) C(21) 136.8(3) . . . yes N(22) N(21) C(21) 105.8(3) . . . yes N(21) N(22) C(23) 110.5(4) . . . yes N(21) N(22) B(1) 119.8(3) . . . yes C(23) N(22) B(1) 129.7(4) . . . yes Cr(1) N(31) N(32) 115.3(2) . . . yes Cr(1) N(31) C(31) 137.3(3) . . . yes N(32) N(31) C(31) 106.5(3) . . . yes N(31) N(32) C(33) 109.9(3) . . . yes N(31) N(32) B(1) 122.2(3) . . . yes C(33) N(32) B(1) 128.0(3) . . . yes Cr(2) N(41) N(42) 113.9(3) . . . yes Cr(2) N(41) C(41) 139.4(3) . . . yes N(42) N(41) C(41) 106.4(3) . . . yes N(41) N(42) C(43) 110.0(4) . . . yes N(41) N(42) B(2) 119.2(3) . . . yes C(43) N(42) B(2) 130.5(4) . . . yes Cr(2) N(51) N(52) 119.0(2) . . . yes Cr(2) N(51) C(51) 133.8(3) . . . yes N(52) N(51) C(51) 107.1(4) . . . yes N(51) N(52) C(53) 109.6(3) . . . yes N(51) N(52) B(2) 118.4(4) . . . yes C(53) N(52) B(2) 131.2(3) . . . yes Cr(2) N(61) N(62) 115.6(3) . . . yes Cr(2) N(61) C(61) 138.7(3) . . . yes N(62) N(61) C(61) 105.6(3) . . . yes N(61) N(62) C(63) 110.0(3) . . . yes N(61) N(62) B(2) 121.3(3) . . . yes C(63) N(62) B(2) 128.6(3) . . . yes Cr(1) N(71) N(72) 113.0(2) . . . yes Cr(1) N(71) C(71) 131.6(3) . . . yes N(72) N(71) C(71) 108.1(3) . . . yes Cr(2) N(72) N(71) 114.0(3) . . . yes Cr(2) N(72) C(73) 130.9(3) . . . yes N(71) N(72) C(73) 107.7(3) . . . yes N(11) C(11) C(12) 110.2(4) . . . yes N(11) C(11) C(14) 120.2(3) . . . yes C(12) C(11) C(14) 129.4(4) . . . yes C(11) C(12) C(13) 106.6(4) . . . yes N(12) C(13) C(12) 107.0(4) . . . yes N(12) C(13) C(17) 122.4(5) . . . yes C(12) C(13) C(17) 130.3(4) . . . yes C(11) C(14) C(15) 111.9(4) . . . yes C(11) C(14) C(16) 110.2(5) . . . yes C(15) C(14) C(16) 110.1(5) . . . yes C(13) C(17) C(18) 110.2(4) . . . yes C(13) C(17) C(19) 111.9(5) . . . yes C(18) C(17) C(19) 109.8(4) . . . yes N(21) C(21) C(22) 109.9(4) . . . yes N(21) C(21) C(24) 122.8(4) . . . yes C(22) C(21) C(24) 127.1(5) . . . yes C(21) C(22) C(23) 106.5(5) . . . yes N(22) C(23) C(22) 107.3(4) . . . yes N(22) C(23) C(27) 123.3(4) . . . yes C(22) C(23) C(27) 129.4(5) . . . yes C(21) C(24) C(25) 111.8(3) . . . yes C(21) C(24) C(26) 109.0(4) . . . yes C(25) C(24) C(26) 109.1(5) . . . yes C(23) C(27) C(28) 112.5(5) . . . yes C(23) C(27) C(29) 110.1(4) . . . yes C(28) C(27) C(29) 110.8(6) . . . yes N(31) C(31) C(32) 109.0(3) . . . yes N(31) C(31) C(34) 122.9(4) . . . yes C(32) C(31) C(34) 128.0(4) . . . yes C(31) C(32) C(33) 107.7(4) . . . yes N(32) C(33) C(32) 106.9(4) . . . yes N(32) C(33) C(37) 123.2(3) . . . yes C(32) C(33) C(37) 129.7(4) . . . yes C(31) C(34) C(35) 109.7(4) . . . yes C(31) C(34) C(36) 112.5(4) . . . yes C(35) C(34) C(36) 110.3(4) . . . yes C(33) C(37) C(38) 110.2(4) . . . yes C(33) C(37) C(39) 110.6(3) . . . yes C(38) C(37) C(39) 110.8(4) . . . yes N(41) C(41) C(42) 110.3(4) . . . yes N(41) C(41) C(44) 121.8(3) . . . yes C(42) C(41) C(44) 127.9(5) . . . yes C(41) C(42) C(43) 106.0(4) . . . yes N(42) C(43) C(42) 107.3(4) . . . yes N(42) C(43) C(47) 124.5(5) . . . yes C(42) C(43) C(47) 128.3(4) . . . yes C(41) C(44) C(45) 111.2(5) . . . yes C(41) C(44) C(46) 112.1(4) . . . yes C(45) C(44) C(46) 110.5(5) . . . yes C(43) C(47) C(48) 112.1(5) . . . yes C(43) C(47) C(49) 108.7(6) . . . yes C(48) C(47) C(49) 110.2(6) . . . yes N(51) C(51) C(52) 109.3(3) . . . yes N(51) C(51) C(54) 121.5(4) . . . yes C(52) C(51) C(54) 129.2(4) . . . yes C(51) C(52) C(53) 106.6(4) . . . yes N(52) C(53) C(52) 107.4(4) . . . yes N(52) C(53) C(57) 123.6(4) . . . yes C(52) C(53) C(57) 128.9(5) . . . yes C(51) C(54) C(55) 112.5(4) . . . yes C(51) C(54) C(56) 109.7(4) . . . yes C(55) C(54) C(56) 110.0(4) . . . yes C(53) C(57) C(58) 110.1(6) . . . yes C(53) C(57) C(59) 111.1(5) . . . yes C(58) C(57) C(59) 110.2(7) . . . yes N(61) C(61) C(62) 110.5(4) . . . yes N(61) C(61) C(64) 122.4(4) . . . yes C(62) C(61) C(64) 126.8(4) . . . yes C(61) C(62) C(63) 106.2(4) . . . yes N(62) C(63) C(62) 107.6(3) . . . yes N(62) C(63) C(67) 124.2(4) . . . yes C(62) C(63) C(67) 128.1(4) . . . yes C(61) C(64) C(65) 110.3(3) . . . yes C(61) C(64) C(66) 109.7(5) . . . yes C(65) C(64) C(66) 109.5(5) . . . yes C(63) C(67) C(68) 111.1(4) . . . yes C(63) C(67) C(69) 111.9(4) . . . yes C(68) C(67) C(69) 110.6(5) . . . yes N(71) C(71) C(72) 108.7(3) . . . yes N(71) C(71) C(74) 121.4(4) . . . yes C(72) C(71) C(74) 129.6(4) . . . yes C(71) C(72) C(73) 106.6(4) . . . yes N(72) C(73) C(72) 108.9(4) . . . yes N(72) C(73) C(77) 122.5(3) . . . yes C(72) C(73) C(77) 128.5(4) . . . yes C(71) C(74) C(75) 110.4(4) . . . yes C(71) C(74) C(76) 113.2(4) . . . yes C(75) C(74) C(76) 110.6(4) . . . yes C(73) C(77) C(78) 112.5(3) . . . yes C(73) C(77) C(79) 111.1(4) . . . yes C(78) C(77) C(79) 109.3(4) . . . yes N(81) C(80) C(81) 159(2) . . . yes N(82) C(82) C(83) 177.7(7) . . . yes N(12) B(1) N(22) 111.2(4) . . . yes N(12) B(1) N(32) 109.8(4) . . . yes N(22) B(1) N(32) 108.9(3) . . . yes N(42) B(2) N(52) 113.5(4) . . . yes N(42) B(2) N(62) 110.3(4) . . . yes N(52) B(2) N(62) 107.6(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(38) C(79) 3.525(8) . 1_556 ? #------------------------------------------------------------------------------ #===END data_compound_5 _database_code_CSD 217498 _audit_creation_date 'Wed May 28 02:33:54 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H95 B2 Cl Cr2 N12 O3 ' _chemical_formula_moiety 'C54 H95 B2 Cl Cr2 N12 O3 ' _chemical_formula_weight 1121.49 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.621(1) _cell_length_b 20.116(2) _cell_length_c 12.0553(8) _cell_angle_alpha 97.853(6) _cell_angle_beta 97.743(5) _cell_angle_gamma 75.816(2) _cell_volume 3154.8(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9533 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 20489 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11787 _reflns_number_gt 8917 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1755 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 8917 _refine_ls_number_parameters 703 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.40 _refine_diff_density_min -0.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.14149(4) 0.18811(2) 0.76449(4) 0.0217(1) Uani 1.00 d . . . Cr(2) Cr 0.32981(4) 0.20969(2) 0.81127(4) 0.0216(1) Uani 1.00 d . . . Cl(1) Cl 0.46656(7) 0.11952(4) 0.85888(7) 0.0380(2) Uani 1.00 d . . . O(1) O 0.1968(2) 0.2682(1) 0.7745(2) 0.0253(5) Uani 1.00 d . . . O(2) O 0.2672(2) 0.1491(1) 0.6907(2) 0.0262(5) Uani 1.00 d . . . O(3) O 0.2389(2) 0.1796(1) 0.9028(2) 0.0276(5) Uani 1.00 d . . . N(11) N 0.1018(2) 0.0942(1) 0.7531(2) 0.0296(6) Uani 1.00 d . . . N(12) N 0.0012(2) 0.0931(1) 0.7179(2) 0.0288(6) Uani 1.00 d . . . N(21) N 0.0129(2) 0.2306(1) 0.8471(2) 0.0243(5) Uani 1.00 d . . . N(22) N -0.0768(2) 0.2114(1) 0.8021(2) 0.0260(6) Uani 1.00 d . . . N(31) N 0.0529(2) 0.2065(1) 0.6145(2) 0.0253(5) Uani 1.00 d . . . N(32) N -0.0422(2) 0.1921(1) 0.5999(2) 0.0277(6) Uani 1.00 d . . . N(41) N 0.1553(2) 0.4034(1) 0.7563(2) 0.0264(6) Uani 1.00 d . . . N(42) N 0.2421(2) 0.4251(1) 0.7535(2) 0.0238(5) Uani 1.00 d . . . N(51) N 0.3706(2) 0.2842(1) 0.9282(2) 0.0242(5) Uani 1.00 d . . . N(52) N 0.3533(2) 0.3519(1) 0.9033(2) 0.0223(5) Uani 1.00 d . . . N(61) N 0.4004(2) 0.2455(1) 0.6995(2) 0.0221(5) Uani 1.00 d . . . N(62) N 0.3827(2) 0.3157(1) 0.6915(2) 0.0225(5) Uani 1.00 d . . . C(11) C 0.1511(3) 0.0300(2) 0.7739(3) 0.0376(8) Uani 1.00 d . . . C(12) C 0.0815(3) -0.0122(2) 0.7528(4) 0.050(1) Uani 1.00 d . . . C(13) C -0.0115(3) 0.0284(2) 0.7191(3) 0.0414(9) Uani 1.00 d . . . C(14) C 0.2624(3) 0.0092(2) 0.8094(4) 0.0449(9) Uani 1.00 d . . . C(15) C 0.3202(4) -0.0362(3) 0.7147(5) 0.068(1) Uani 1.00 d . . . C(16) C 0.2837(5) -0.0256(3) 0.9156(5) 0.098(2) Uani 1.00 d . . . C(17) C -0.1109(3) 0.0080(2) 0.6849(4) 0.052(1) Uani 1.00 d . . . C(18) C -0.1191(4) -0.0214(3) 0.5623(4) 0.078(2) Uani 1.00 d . . . C(19) C -0.1254(5) -0.0428(3) 0.7587(5) 0.084(2) Uani 1.00 d . . . C(21) C -0.0079(3) 0.2725(2) 0.9419(3) 0.0282(7) Uani 1.00 d . . . C(22) C -0.1091(3) 0.2807(2) 0.9571(3) 0.0381(8) Uani 1.00 d . . . C(23) C -0.1517(3) 0.2418(2) 0.8698(3) 0.0309(7) Uani 1.00 d . . . C(24) C 0.0702(3) 0.3024(2) 1.0194(3) 0.0348(8) Uani 1.00 d . . . C(25) C 0.0562(4) 0.3782(2) 1.0147(4) 0.052(1) Uani 1.00 d . . . C(26) C 0.0670(4) 0.2880(2) 1.1404(3) 0.056(1) Uani 1.00 d . . . C(27) C -0.2543(3) 0.2263(2) 0.8518(3) 0.0421(9) Uani 1.00 d . . . C(28) C -0.3382(4) 0.2901(3) 0.8746(5) 0.080(2) Uani 1.00 d . . . C(29) C -0.2575(4) 0.1711(3) 0.9262(5) 0.074(2) Uani 1.00 d . . . C(31) C 0.0626(3) 0.2343(2) 0.5230(3) 0.0295(7) Uani 1.00 d . . . C(32) C -0.0263(3) 0.2376(2) 0.4488(3) 0.0362(8) Uani 1.00 d . . . C(33) C -0.0907(3) 0.2109(2) 0.5000(3) 0.0324(7) Uani 1.00 d . . . C(34) C 0.1563(3) 0.2546(2) 0.5019(3) 0.0382(8) Uani 1.00 d . . . C(35) C 0.1327(3) 0.3283(2) 0.4709(3) 0.0462(10) Uani 1.00 d . . . C(36) C 0.2075(3) 0.2039(2) 0.4101(3) 0.050(1) Uani 1.00 d . . . C(37) C -0.1981(3) 0.2067(2) 0.4617(4) 0.0471(10) Uani 1.00 d . . . C(38) C -0.2712(3) 0.2632(2) 0.5263(5) 0.068(1) Uani 1.00 d . . . C(39) C -0.2227(4) 0.2133(2) 0.3352(4) 0.069(1) Uani 1.00 d . . . C(41) C 0.0762(3) 0.4563(2) 0.7343(3) 0.0305(7) Uani 1.00 d . . . C(42) C 0.1135(3) 0.5125(2) 0.7164(3) 0.0345(8) Uani 1.00 d . . . C(43) C 0.2165(3) 0.4924(2) 0.7296(3) 0.0294(7) Uani 1.00 d . . . C(44) C -0.0322(3) 0.4539(2) 0.7377(3) 0.0355(8) Uani 1.00 d . . . C(45) C -0.1058(3) 0.5083(2) 0.6717(4) 0.053(1) Uani 1.00 d . . . C(46) C -0.0545(3) 0.3837(2) 0.7006(4) 0.0466(9) Uani 1.00 d . . . C(47) C 0.2901(3) 0.5369(2) 0.7203(3) 0.0338(8) Uani 1.00 d . . . C(48) C 0.2719(4) 0.5628(2) 0.6038(3) 0.049(1) Uani 1.00 d . . . C(49) C 0.2776(3) 0.5998(2) 0.8099(3) 0.0451(9) Uani 1.00 d . . . C(51) C 0.3874(3) 0.2855(2) 1.0411(3) 0.0273(7) Uani 1.00 d . . . C(52) C 0.3801(3) 0.3525(2) 1.0888(3) 0.0338(8) Uani 1.00 d . . . C(53) C 0.3589(3) 0.3932(2) 1.0019(3) 0.0278(7) Uani 1.00 d . . . C(54) C 0.4177(3) 0.2218(2) 1.1009(3) 0.0344(8) Uani 1.00 d . . . C(55) C 0.5248(4) 0.2157(3) 1.1589(4) 0.065(1) Uani 1.00 d . . . C(56) C 0.3443(4) 0.2231(2) 1.1859(4) 0.058(1) Uani 1.00 d . . . C(57) C 0.3426(3) 0.4699(2) 1.0110(3) 0.0329(8) Uani 1.00 d . . . C(58) C 0.4153(4) 0.4952(2) 1.1048(3) 0.051(1) Uani 1.00 d . . . C(59) C 0.2325(3) 0.5043(2) 1.0314(4) 0.0466(10) Uani 1.00 d . . . C(61) C 0.4444(2) 0.2113(2) 0.6090(3) 0.0253(6) Uani 1.00 d . . . C(62) C 0.4544(3) 0.2594(2) 0.5402(3) 0.0293(7) Uani 1.00 d . . . C(63) C 0.4165(2) 0.3237(2) 0.5937(3) 0.0262(7) Uani 1.00 d . . . C(64) C 0.4850(3) 0.1345(2) 0.5904(3) 0.0313(7) Uani 1.00 d . . . C(65) C 0.5983(3) 0.1165(2) 0.6290(4) 0.051(1) Uani 1.00 d . . . C(66) C 0.4661(4) 0.1062(2) 0.4676(3) 0.055(1) Uani 1.00 d . . . C(67) C 0.4143(3) 0.3926(2) 0.5571(3) 0.0334(8) Uani 1.00 d . . . C(68) C 0.5117(3) 0.4163(2) 0.6031(3) 0.0423(9) Uani 1.00 d . . . C(69) C 0.3998(3) 0.3903(2) 0.4285(3) 0.0419(9) Uani 1.00 d . . . B(1) B -0.0758(3) 0.1606(2) 0.6941(3) 0.0287(8) Uani 1.00 d . . . B(2) B 0.3488(3) 0.3765(2) 0.7844(3) 0.0240(7) Uani 1.00 d . . . H(1) H 0.172(3) 0.310(2) 0.776(3) 0.0543(2) Uiso 1.00 calc . . . H(2) H 0.287(5) 0.120(3) 0.703(5) 0.1051(3) Uiso 1.00 calc . . . H(3) H 0.258(3) 0.147(2) 0.916(3) 0.0351(2) Uiso 1.00 calc . . . H(4) H 0.0971 -0.0609 0.7619 0.0605 Uiso 1.00 calc . . . H(5) H 0.2882 0.0510 0.8278 0.0543 Uiso 1.00 calc . . . H(6) H 0.2984 -0.0788 0.6983 0.0685 Uiso 1.00 calc . . . H(7) H 0.3920 -0.0458 0.7382 0.0685 Uiso 1.00 calc . . . H(8) H 0.3063 -0.0125 0.6484 0.0685 Uiso 1.00 calc . . . H(9) H 0.2517 0.0054 0.9750 0.0977 Uiso 1.00 calc . . . H(10) H 0.3559 -0.0381 0.9362 0.0977 Uiso 1.00 calc . . . H(11) H 0.2571 -0.0663 0.9033 0.0977 Uiso 1.00 calc . . . H(12) H -0.1652 0.0492 0.6933 0.0634 Uiso 1.00 calc . . . H(13) H -0.1804 -0.0379 0.5444 0.0782 Uiso 1.00 calc . . . H(14) H -0.0614 -0.0588 0.5493 0.0782 Uiso 1.00 calc . . . H(15) H -0.1209 0.0139 0.5155 0.0782 Uiso 1.00 calc . . . H(16) H -0.1113 -0.0263 0.8364 0.0837 Uiso 1.00 calc . . . H(17) H -0.0798 -0.0867 0.7417 0.0837 Uiso 1.00 calc . . . H(18) H -0.1944 -0.0479 0.7450 0.0837 Uiso 1.00 calc . . . H(19) H -0.1426 0.1523 0.6712 0.0338 Uiso 1.00 calc . . . H(20) H -0.1436 0.3085 1.0177 0.0434 Uiso 1.00 calc . . . H(21) H 0.1362 0.2799 0.9969 0.0413 Uiso 1.00 calc . . . H(22) H 0.1041 0.3955 1.0702 0.0522 Uiso 1.00 calc . . . H(23) H -0.0118 0.4016 1.0298 0.0522 Uiso 1.00 calc . . . H(24) H 0.0674 0.3862 0.9412 0.0522 Uiso 1.00 calc . . . H(25) H 0.0011 0.3098 1.1641 0.0556 Uiso 1.00 calc . . . H(26) H 0.1182 0.3059 1.1895 0.0556 Uiso 1.00 calc . . . H(27) H 0.0796 0.2391 1.1433 0.0556 Uiso 1.00 calc . . . H(28) H -0.2656 0.2083 0.7743 0.0504 Uiso 1.00 calc . . . H(29) H -0.3243 0.3118 0.9492 0.0804 Uiso 1.00 calc . . . H(30) H -0.4023 0.2772 0.8683 0.0804 Uiso 1.00 calc . . . H(31) H -0.3412 0.3217 0.8207 0.0804 Uiso 1.00 calc . . . H(32) H -0.3213 0.1577 0.9085 0.0742 Uiso 1.00 calc . . . H(33) H -0.2506 0.1893 1.0039 0.0742 Uiso 1.00 calc . . . H(34) H -0.2026 0.1316 0.9127 0.0742 Uiso 1.00 calc . . . H(35) H -0.0396 0.2551 0.3766 0.0432 Uiso 1.00 calc . . . H(36) H 0.2029 0.2519 0.5710 0.0465 Uiso 1.00 calc . . . H(37) H 0.1942 0.3391 0.4561 0.0462 Uiso 1.00 calc . . . H(38) H 0.1045 0.3596 0.5322 0.0462 Uiso 1.00 calc . . . H(39) H 0.0845 0.3326 0.4049 0.0462 Uiso 1.00 calc . . . H(40) H 0.2239 0.1582 0.4328 0.0498 Uiso 1.00 calc . . . H(41) H 0.2687 0.2160 0.3978 0.0498 Uiso 1.00 calc . . . H(42) H 0.1622 0.2054 0.3418 0.0498 Uiso 1.00 calc . . . H(43) H -0.2069 0.1626 0.4752 0.0557 Uiso 1.00 calc . . . H(44) H -0.2602 0.2564 0.6047 0.0682 Uiso 1.00 calc . . . H(45) H -0.3400 0.2617 0.4978 0.0682 Uiso 1.00 calc . . . H(46) H -0.2597 0.3073 0.5173 0.0682 Uiso 1.00 calc . . . H(47) H -0.2250 0.2596 0.3215 0.0688 Uiso 1.00 calc . . . H(48) H -0.2875 0.2026 0.3097 0.0688 Uiso 1.00 calc . . . H(49) H -0.1709 0.1817 0.2952 0.0688 Uiso 1.00 calc . . . H(50) H 0.3976 0.4046 0.7910 0.0290 Uiso 1.00 calc . . . H(51) H 0.0733 0.5572 0.6984 0.0391 Uiso 1.00 calc . . . H(52) H -0.0459 0.4649 0.8155 0.0448 Uiso 1.00 calc . . . H(53) H -0.0957 0.5531 0.7015 0.0528 Uiso 1.00 calc . . . H(54) H -0.1745 0.5064 0.6782 0.0528 Uiso 1.00 calc . . . H(55) H -0.0936 0.4995 0.5939 0.0528 Uiso 1.00 calc . . . H(56) H -0.1218 0.3842 0.7168 0.0466 Uiso 1.00 calc . . . H(57) H -0.0057 0.3496 0.7403 0.0466 Uiso 1.00 calc . . . H(58) H -0.0501 0.3727 0.6211 0.0466 Uiso 1.00 calc . . . H(59) H 0.3590 0.5100 0.7310 0.0416 Uiso 1.00 calc . . . H(60) H 0.3228 0.5871 0.5968 0.0485 Uiso 1.00 calc . . . H(61) H 0.2057 0.5932 0.5950 0.0485 Uiso 1.00 calc . . . H(62) H 0.2759 0.5242 0.5467 0.0485 Uiso 1.00 calc . . . H(63) H 0.2894 0.5844 0.8835 0.0451 Uiso 1.00 calc . . . H(64) H 0.2098 0.6279 0.7991 0.0451 Uiso 1.00 calc . . . H(65) H 0.3259 0.6263 0.8030 0.0451 Uiso 1.00 calc . . . H(66) H 0.3886 0.3673 1.1678 0.0416 Uiso 1.00 calc . . . H(67) H 0.4171 0.1819 1.0471 0.0419 Uiso 1.00 calc . . . H(68) H 0.5433 0.1761 1.2003 0.0647 Uiso 1.00 calc . . . H(69) H 0.5277 0.2564 1.2097 0.0647 Uiso 1.00 calc . . . H(70) H 0.5713 0.2105 1.1035 0.0647 Uiso 1.00 calc . . . H(71) H 0.3453 0.2618 1.2419 0.0579 Uiso 1.00 calc . . . H(72) H 0.3645 0.1812 1.2215 0.0579 Uiso 1.00 calc . . . H(73) H 0.2768 0.2270 1.1482 0.0579 Uiso 1.00 calc . . . H(74) H 0.3562 0.4821 0.9412 0.0409 Uiso 1.00 calc . . . H(75) H 0.3986 0.4875 1.1761 0.0512 Uiso 1.00 calc . . . H(76) H 0.4094 0.5436 1.1031 0.0512 Uiso 1.00 calc . . . H(77) H 0.4838 0.4705 1.0943 0.0512 Uiso 1.00 calc . . . H(78) H 0.2234 0.5535 1.0389 0.0466 Uiso 1.00 calc . . . H(79) H 0.2174 0.4905 1.0991 0.0466 Uiso 1.00 calc . . . H(80) H 0.1875 0.4905 0.9689 0.0466 Uiso 1.00 calc . . . H(81) H 0.4806 0.2497 0.4683 0.0357 Uiso 1.00 calc . . . H(82) H 0.4502 0.1130 0.6337 0.0394 Uiso 1.00 calc . . . H(83) H 0.6225 0.0673 0.6233 0.0513 Uiso 1.00 calc . . . H(84) H 0.6099 0.1355 0.7058 0.0513 Uiso 1.00 calc . . . H(85) H 0.6340 0.1354 0.5823 0.0513 Uiso 1.00 calc . . . H(86) H 0.3941 0.1142 0.4456 0.0547 Uiso 1.00 calc . . . H(87) H 0.4957 0.0575 0.4588 0.0547 Uiso 1.00 calc . . . H(88) H 0.4966 0.1289 0.4211 0.0547 Uiso 1.00 calc . . . H(89) H 0.3577 0.4261 0.5866 0.0397 Uiso 1.00 calc . . . H(90) H 0.5688 0.3851 0.5711 0.0423 Uiso 1.00 calc . . . H(91) H 0.5214 0.4168 0.6836 0.0423 Uiso 1.00 calc . . . H(92) H 0.5062 0.4618 0.5835 0.0423 Uiso 1.00 calc . . . H(93) H 0.3914 0.4359 0.4076 0.0419 Uiso 1.00 calc . . . H(94) H 0.3404 0.3732 0.3995 0.0419 Uiso 1.00 calc . . . H(95) H 0.4585 0.3603 0.3978 0.0419 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0176(3) 0.0222(3) 0.0263(3) -0.0071(2) 0.0024(2) 0.0019(2) Cr(2) 0.0180(3) 0.0220(3) 0.0254(3) -0.0058(2) 0.0015(2) 0.0028(2) Cl(1) 0.0286(5) 0.0384(5) 0.0431(5) 0.0018(4) 0.0028(4) 0.0092(3) O(1) 0.021(1) 0.023(1) 0.032(1) -0.0079(9) -0.0012(9) 0.0027(9) O(2) 0.019(1) 0.027(1) 0.031(1) -0.0068(10) 0.0005(9) -0.0003(9) O(3) 0.026(1) 0.028(1) 0.031(1) -0.006(1) 0.0037(9) 0.0079(10) N(11) 0.024(2) 0.025(1) 0.041(2) -0.007(1) 0.006(1) 0.003(1) N(12) 0.026(2) 0.023(1) 0.041(2) -0.010(1) 0.008(1) 0.000(1) N(21) 0.020(1) 0.025(1) 0.028(1) -0.006(1) 0.003(1) 0.0013(10) N(22) 0.018(1) 0.026(1) 0.036(1) -0.009(1) 0.006(1) 0.001(1) N(31) 0.019(1) 0.031(1) 0.027(1) -0.012(1) -0.002(1) 0.0029(10) N(32) 0.018(1) 0.030(1) 0.036(1) -0.011(1) -0.002(1) 0.001(1) N(41) 0.020(1) 0.027(1) 0.031(1) -0.005(1) -0.001(1) 0.004(1) N(42) 0.023(2) 0.022(1) 0.027(1) -0.005(1) 0.002(1) 0.0034(9) N(51) 0.021(1) 0.025(1) 0.027(1) -0.008(1) -0.003(1) 0.0027(10) N(52) 0.020(1) 0.021(1) 0.026(1) -0.007(1) -0.002(1) 0.0029(9) N(61) 0.018(1) 0.023(1) 0.025(1) -0.006(1) 0.0008(10) 0.0014(9) N(62) 0.021(1) 0.022(1) 0.027(1) -0.009(1) 0.001(1) 0.0033(9) C(11) 0.031(2) 0.024(2) 0.059(2) -0.006(1) 0.010(2) 0.007(1) C(12) 0.034(2) 0.027(2) 0.092(3) -0.008(2) 0.012(2) 0.009(2) C(13) 0.039(2) 0.025(2) 0.064(2) -0.014(2) 0.012(2) 0.000(2) C(14) 0.030(2) 0.032(2) 0.073(3) -0.003(2) 0.004(2) 0.012(2) C(15) 0.046(3) 0.056(3) 0.097(4) -0.001(2) 0.020(3) -0.005(3) C(16) 0.065(4) 0.125(6) 0.110(5) -0.014(4) -0.008(3) 0.069(4) C(17) 0.037(2) 0.033(2) 0.092(3) -0.017(2) 0.015(2) -0.001(2) C(18) 0.060(4) 0.104(5) 0.081(4) -0.044(3) -0.006(3) 0.015(3) C(19) 0.082(4) 0.100(4) 0.093(4) -0.069(4) 0.013(3) 0.004(3) C(21) 0.026(2) 0.031(2) 0.027(2) -0.007(1) 0.002(1) 0.001(1) C(22) 0.032(2) 0.043(2) 0.039(2) -0.007(2) 0.012(2) -0.005(1) C(23) 0.022(2) 0.033(2) 0.039(2) -0.007(1) 0.009(1) 0.002(1) C(24) 0.026(2) 0.042(2) 0.033(2) -0.006(1) 0.004(1) -0.006(1) C(25) 0.061(3) 0.046(2) 0.053(2) -0.029(2) -0.009(2) 0.000(2) C(26) 0.060(3) 0.074(3) 0.034(2) -0.020(2) -0.004(2) 0.010(2) C(27) 0.032(2) 0.051(2) 0.047(2) -0.016(2) 0.016(2) -0.006(2) C(28) 0.027(3) 0.073(4) 0.129(5) -0.006(2) 0.012(3) -0.022(3) C(29) 0.063(4) 0.096(4) 0.084(4) -0.046(3) 0.012(3) 0.024(3) C(31) 0.028(2) 0.037(2) 0.025(2) -0.013(1) -0.001(1) 0.004(1) C(32) 0.033(2) 0.040(2) 0.036(2) -0.012(2) -0.006(2) 0.008(1) C(33) 0.025(2) 0.030(2) 0.041(2) -0.010(1) -0.006(1) 0.002(1) C(34) 0.033(2) 0.053(2) 0.034(2) -0.019(2) 0.000(2) 0.011(2) C(35) 0.053(3) 0.053(2) 0.040(2) -0.025(2) 0.007(2) 0.007(2) C(36) 0.041(3) 0.056(3) 0.054(2) -0.007(2) 0.015(2) 0.012(2) C(37) 0.029(2) 0.037(2) 0.077(3) -0.016(2) -0.017(2) 0.017(2) C(38) 0.030(3) 0.062(3) 0.119(4) -0.006(2) 0.007(3) 0.038(3) C(39) 0.059(3) 0.057(3) 0.085(3) -0.025(2) -0.045(3) 0.019(2) C(41) 0.029(2) 0.029(2) 0.031(2) -0.002(1) 0.000(1) 0.004(1) C(42) 0.036(2) 0.022(2) 0.043(2) -0.001(1) 0.000(2) 0.010(1) C(43) 0.035(2) 0.023(2) 0.031(2) -0.005(1) 0.005(1) 0.005(1) C(44) 0.024(2) 0.035(2) 0.045(2) -0.001(1) 0.001(1) 0.006(1) C(45) 0.033(2) 0.050(3) 0.073(3) -0.005(2) -0.008(2) 0.017(2) C(46) 0.028(2) 0.037(2) 0.073(3) -0.006(2) 0.004(2) 0.004(2) C(47) 0.036(2) 0.023(2) 0.043(2) -0.006(1) 0.005(2) 0.008(1) C(48) 0.061(3) 0.035(2) 0.054(2) -0.007(2) 0.016(2) 0.016(2) C(49) 0.056(3) 0.030(2) 0.053(2) -0.018(2) 0.006(2) 0.001(2) C(51) 0.026(2) 0.034(2) 0.023(2) -0.008(1) -0.001(1) 0.005(1) C(52) 0.043(2) 0.036(2) 0.021(2) -0.010(2) -0.001(1) 0.002(1) C(53) 0.031(2) 0.025(2) 0.027(2) -0.008(1) 0.004(1) -0.001(1) C(54) 0.038(2) 0.037(2) 0.028(2) -0.007(2) 0.002(1) 0.008(1) C(55) 0.044(3) 0.065(3) 0.083(3) -0.003(2) -0.015(2) 0.037(2) C(56) 0.052(3) 0.066(3) 0.062(3) -0.008(2) 0.014(2) 0.029(2) C(57) 0.041(2) 0.027(2) 0.031(2) -0.012(1) 0.004(1) -0.004(1) C(58) 0.066(3) 0.042(2) 0.045(2) -0.025(2) -0.008(2) -0.003(2) C(59) 0.051(3) 0.034(2) 0.055(2) -0.005(2) 0.018(2) -0.002(2) C(61) 0.022(2) 0.027(2) 0.027(2) -0.007(1) 0.008(1) -0.003(1) C(62) 0.030(2) 0.031(2) 0.030(2) -0.011(1) 0.011(1) -0.002(1) C(63) 0.021(2) 0.031(2) 0.028(2) -0.009(1) 0.003(1) 0.003(1) C(64) 0.030(2) 0.025(2) 0.039(2) -0.006(1) 0.010(1) 0.001(1) C(65) 0.031(2) 0.043(2) 0.077(3) -0.003(2) 0.007(2) 0.006(2) C(66) 0.068(3) 0.032(2) 0.050(2) 0.005(2) 0.003(2) -0.010(2) C(67) 0.043(2) 0.027(2) 0.035(2) -0.013(1) 0.009(2) 0.004(1) C(68) 0.049(3) 0.040(2) 0.046(2) -0.023(2) 0.010(2) 0.002(2) C(69) 0.057(3) 0.043(2) 0.030(2) -0.018(2) 0.004(2) 0.008(1) B(1) 0.014(2) 0.032(2) 0.042(2) -0.013(1) 0.003(1) -0.002(1) B(2) 0.021(2) 0.027(2) 0.026(2) -0.009(1) 0.005(1) 0.003(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) Cr(2) 2.6787(8) . . yes Cr(1) O(1) 1.923(3) . . yes Cr(1) O(2) 1.975(2) . . yes Cr(1) O(3) 1.985(2) . . yes Cr(1) N(11) 2.070(3) . . yes Cr(1) N(21) 2.072(3) . . yes Cr(1) N(31) 2.059(3) . . yes Cr(2) Cl(1) 2.3302(9) . . yes Cr(2) O(1) 1.936(2) . . yes Cr(2) O(2) 2.004(2) . . yes Cr(2) O(3) 2.008(3) . . yes Cr(2) N(51) 2.041(3) . . yes Cr(2) N(61) 2.053(3) . . yes N(11) N(12) 1.384(4) . . yes N(11) C(11) 1.343(4) . . yes N(12) C(13) 1.355(5) . . yes N(12) B(1) 1.535(4) . . yes N(21) N(22) 1.389(4) . . yes N(21) C(21) 1.342(4) . . yes N(22) C(23) 1.365(4) . . yes N(22) B(1) 1.541(4) . . yes N(31) N(32) 1.378(4) . . yes N(31) C(31) 1.339(4) . . yes N(32) C(33) 1.349(4) . . yes N(32) B(1) 1.542(5) . . yes N(41) N(42) 1.364(4) . . yes N(41) C(41) 1.342(4) . . yes N(42) C(43) 1.372(4) . . yes N(42) B(2) 1.570(4) . . yes N(51) N(52) 1.390(4) . . yes N(51) C(51) 1.347(4) . . yes N(52) C(53) 1.360(4) . . yes N(52) B(2) 1.569(4) . . yes N(61) N(62) 1.387(3) . . yes N(61) C(61) 1.339(4) . . yes N(62) C(63) 1.364(4) . . yes N(62) B(2) 1.566(4) . . yes C(11) C(12) 1.397(6) . . yes C(11) C(14) 1.490(5) . . yes C(12) C(13) 1.372(5) . . yes C(13) C(17) 1.500(6) . . yes C(14) C(15) 1.538(6) . . yes C(14) C(16) 1.502(8) . . yes C(17) C(18) 1.516(7) . . yes C(17) C(19) 1.508(8) . . yes C(21) C(22) 1.381(5) . . yes C(21) C(24) 1.504(5) . . yes C(22) C(23) 1.375(5) . . yes C(23) C(27) 1.486(6) . . yes C(24) C(25) 1.499(6) . . yes C(24) C(26) 1.534(6) . . yes C(27) C(28) 1.517(6) . . yes C(27) C(29) 1.531(8) . . yes C(31) C(32) 1.399(5) . . yes C(31) C(34) 1.493(6) . . yes C(32) C(33) 1.380(6) . . yes C(33) C(37) 1.492(6) . . yes C(34) C(35) 1.525(6) . . yes C(34) C(36) 1.518(5) . . yes C(37) C(38) 1.518(6) . . yes C(37) C(39) 1.534(7) . . yes C(41) C(42) 1.400(5) . . yes C(41) C(44) 1.497(5) . . yes C(42) C(43) 1.355(5) . . yes C(43) C(47) 1.521(6) . . yes C(44) C(45) 1.523(5) . . yes C(44) C(46) 1.512(6) . . yes C(47) C(48) 1.532(6) . . yes C(47) C(49) 1.539(5) . . yes C(51) C(52) 1.376(4) . . yes C(51) C(54) 1.499(5) . . yes C(52) C(53) 1.376(5) . . yes C(53) C(57) 1.495(5) . . yes C(54) C(55) 1.515(6) . . yes C(54) C(56) 1.518(6) . . yes C(57) C(58) 1.517(6) . . yes C(57) C(59) 1.527(6) . . yes C(61) C(62) 1.398(5) . . yes C(61) C(64) 1.504(4) . . yes C(62) C(63) 1.375(4) . . yes C(63) C(67) 1.504(5) . . yes C(64) C(65) 1.518(5) . . yes C(64) C(66) 1.524(5) . . yes C(67) C(68) 1.528(6) . . yes C(67) C(69) 1.533(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr(2) Cr(1) O(1) 46.24(6) . . . yes Cr(2) Cr(1) O(2) 48.14(7) . . . yes Cr(2) Cr(1) O(3) 48.24(8) . . . yes Cr(2) Cr(1) N(11) 126.33(7) . . . yes Cr(2) Cr(1) N(21) 129.68(8) . . . yes Cr(2) Cr(1) N(31) 123.65(9) . . . yes O(1) Cr(1) O(2) 79.0(1) . . . yes O(1) Cr(1) O(3) 76.9(1) . . . yes O(1) Cr(1) N(11) 172.32(10) . . . yes O(1) Cr(1) N(21) 99.6(1) . . . yes O(1) Cr(1) N(31) 95.0(1) . . . yes O(2) Cr(1) O(3) 82.24(10) . . . yes O(2) Cr(1) N(11) 94.0(1) . . . yes O(2) Cr(1) N(21) 177.8(1) . . . yes O(2) Cr(1) N(31) 93.37(10) . . . yes O(3) Cr(1) N(11) 99.0(1) . . . yes O(3) Cr(1) N(21) 95.78(10) . . . yes O(3) Cr(1) N(31) 171.4(1) . . . yes N(11) Cr(1) N(21) 87.3(1) . . . yes N(11) Cr(1) N(31) 88.7(1) . . . yes N(21) Cr(1) N(31) 88.5(1) . . . yes Cr(1) Cr(2) Cl(1) 120.18(3) . . . yes Cr(1) Cr(2) O(1) 45.83(8) . . . yes Cr(1) Cr(2) O(2) 47.24(7) . . . yes Cr(1) Cr(2) O(3) 47.51(6) . . . yes Cr(1) Cr(2) N(51) 125.12(8) . . . yes Cr(1) Cr(2) N(61) 122.96(7) . . . yes Cl(1) Cr(2) O(1) 165.84(9) . . . yes Cl(1) Cr(2) O(2) 92.74(7) . . . yes Cl(1) Cr(2) O(3) 91.97(7) . . . yes Cl(1) Cr(2) N(51) 97.28(7) . . . yes Cl(1) Cr(2) N(61) 96.18(7) . . . yes O(1) Cr(2) O(2) 78.04(9) . . . yes O(1) Cr(2) O(3) 76.1(1) . . . yes O(1) Cr(2) N(51) 91.91(9) . . . yes O(1) Cr(2) N(61) 95.04(10) . . . yes O(2) Cr(2) O(3) 81.0(1) . . . yes O(2) Cr(2) N(51) 169.92(9) . . . yes O(2) Cr(2) N(61) 93.1(1) . . . yes O(3) Cr(2) N(51) 97.5(1) . . . yes O(3) Cr(2) N(61) 170.17(9) . . . yes N(51) Cr(2) N(61) 87.0(1) . . . yes Cr(1) O(1) Cr(2) 87.94(10) . . . yes Cr(1) O(2) Cr(2) 84.63(9) . . . yes Cr(1) O(3) Cr(2) 84.25(10) . . . yes Cr(1) N(11) N(12) 117.3(2) . . . yes Cr(1) N(11) C(11) 135.3(2) . . . yes N(12) N(11) C(11) 107.4(3) . . . yes N(11) N(12) C(13) 109.1(3) . . . yes N(11) N(12) B(1) 119.4(3) . . . yes C(13) N(12) B(1) 131.3(3) . . . yes Cr(1) N(21) N(22) 117.5(2) . . . yes Cr(1) N(21) C(21) 135.8(2) . . . yes N(22) N(21) C(21) 106.6(3) . . . yes N(21) N(22) C(23) 109.5(2) . . . yes N(21) N(22) B(1) 118.8(3) . . . yes C(23) N(22) B(1) 131.7(3) . . . yes Cr(1) N(31) N(32) 118.1(2) . . . yes Cr(1) N(31) C(31) 134.6(2) . . . yes N(32) N(31) C(31) 107.2(2) . . . yes N(31) N(32) C(33) 109.5(3) . . . yes N(31) N(32) B(1) 118.9(2) . . . yes C(33) N(32) B(1) 131.6(3) . . . yes N(42) N(41) C(41) 107.4(3) . . . yes N(41) N(42) C(43) 109.1(2) . . . yes N(41) N(42) B(2) 120.0(3) . . . yes C(43) N(42) B(2) 130.7(3) . . . yes Cr(2) N(51) N(52) 120.7(2) . . . yes Cr(2) N(51) C(51) 129.3(2) . . . yes N(52) N(51) C(51) 107.2(2) . . . yes N(51) N(52) C(53) 108.1(2) . . . yes N(51) N(52) B(2) 127.0(2) . . . yes C(53) N(52) B(2) 124.0(3) . . . yes Cr(2) N(61) N(62) 120.5(2) . . . yes Cr(2) N(61) C(61) 128.9(2) . . . yes N(62) N(61) C(61) 108.5(3) . . . yes N(61) N(62) C(63) 107.7(2) . . . yes N(61) N(62) B(2) 127.8(3) . . . yes C(63) N(62) B(2) 123.7(3) . . . yes N(11) C(11) C(12) 108.5(3) . . . yes N(11) C(11) C(14) 123.9(4) . . . yes C(12) C(11) C(14) 127.5(3) . . . yes C(11) C(12) C(13) 107.3(3) . . . yes N(12) C(13) C(12) 107.6(4) . . . yes N(12) C(13) C(17) 123.8(3) . . . yes C(12) C(13) C(17) 128.5(4) . . . yes C(11) C(14) C(15) 111.6(3) . . . yes C(11) C(14) C(16) 111.7(4) . . . yes C(15) C(14) C(16) 111.2(4) . . . yes C(13) C(17) C(18) 111.2(4) . . . yes C(13) C(17) C(19) 111.4(4) . . . yes C(18) C(17) C(19) 110.3(4) . . . yes N(21) C(21) C(22) 109.4(3) . . . yes N(21) C(21) C(24) 123.7(3) . . . yes C(22) C(21) C(24) 126.8(3) . . . yes C(21) C(22) C(23) 107.8(3) . . . yes N(22) C(23) C(22) 106.7(3) . . . yes N(22) C(23) C(27) 123.0(3) . . . yes C(22) C(23) C(27) 130.0(3) . . . yes C(21) C(24) C(25) 112.8(3) . . . yes C(21) C(24) C(26) 109.6(4) . . . yes C(25) C(24) C(26) 110.1(3) . . . yes C(23) C(27) C(28) 112.2(4) . . . yes C(23) C(27) C(29) 109.8(3) . . . yes C(28) C(27) C(29) 110.4(4) . . . yes N(31) C(31) C(32) 109.1(3) . . . yes N(31) C(31) C(34) 124.8(3) . . . yes C(32) C(31) C(34) 126.0(3) . . . yes C(31) C(32) C(33) 106.4(3) . . . yes N(32) C(33) C(32) 107.8(3) . . . yes N(32) C(33) C(37) 123.1(4) . . . yes C(32) C(33) C(37) 128.9(3) . . . yes C(31) C(34) C(35) 111.8(3) . . . yes C(31) C(34) C(36) 109.2(3) . . . yes C(35) C(34) C(36) 111.0(3) . . . yes C(33) C(37) C(38) 110.3(3) . . . yes C(33) C(37) C(39) 110.8(4) . . . yes C(38) C(37) C(39) 109.5(3) . . . yes N(41) C(41) C(42) 108.8(3) . . . yes N(41) C(41) C(44) 123.2(3) . . . yes C(42) C(41) C(44) 127.8(3) . . . yes C(41) C(42) C(43) 106.9(3) . . . yes N(42) C(43) C(42) 107.7(3) . . . yes N(42) C(43) C(47) 126.4(3) . . . yes C(42) C(43) C(47) 125.8(3) . . . yes C(41) C(44) C(45) 111.8(3) . . . yes C(41) C(44) C(46) 114.3(3) . . . yes C(45) C(44) C(46) 110.3(3) . . . yes C(43) C(47) C(48) 110.5(3) . . . yes C(43) C(47) C(49) 111.4(3) . . . yes C(48) C(47) C(49) 108.4(3) . . . yes N(51) C(51) C(52) 109.4(3) . . . yes N(51) C(51) C(54) 123.4(3) . . . yes C(52) C(51) C(54) 127.0(3) . . . yes C(51) C(52) C(53) 107.0(3) . . . yes N(52) C(53) C(52) 108.2(3) . . . yes N(52) C(53) C(57) 124.6(3) . . . yes C(52) C(53) C(57) 127.2(3) . . . yes C(51) C(54) C(55) 109.2(4) . . . yes C(51) C(54) C(56) 111.3(3) . . . yes C(55) C(54) C(56) 110.3(3) . . . yes C(53) C(57) C(58) 110.9(3) . . . yes C(53) C(57) C(59) 110.2(3) . . . yes C(58) C(57) C(59) 110.3(3) . . . yes N(61) C(61) C(62) 108.5(3) . . . yes N(61) C(61) C(64) 125.4(3) . . . yes C(62) C(61) C(64) 125.9(3) . . . yes C(61) C(62) C(63) 106.9(3) . . . yes N(62) C(63) C(62) 108.4(3) . . . yes N(62) C(63) C(67) 123.8(3) . . . yes C(62) C(63) C(67) 127.8(3) . . . yes C(61) C(64) C(65) 109.8(3) . . . yes C(61) C(64) C(66) 112.1(3) . . . yes C(65) C(64) C(66) 109.8(3) . . . yes C(63) C(67) C(68) 111.1(3) . . . yes C(63) C(67) C(69) 111.2(3) . . . yes C(68) C(67) C(69) 109.6(3) . . . yes N(12) B(1) N(22) 108.3(3) . . . yes N(12) B(1) N(32) 109.5(3) . . . yes N(22) B(1) N(32) 108.7(3) . . . yes N(42) B(2) N(52) 110.2(3) . . . yes N(42) B(2) N(62) 114.3(2) . . . yes N(52) B(2) N(62) 113.0(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cr(1) Cr(2) 2.6787(8) . . ? C(36) C(56) 3.595(7) . 1_554 ? #------------------------------------------------------------------------------ #===END data_compound_7 _database_code_CSD 217499 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C69 H134 B2 Cr3 N12 O8 ' _chemical_formula_moiety 'C69 H134 B2 Cr3 N12 O8 ' _chemical_formula_weight 1437.50 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 16.588(2) _cell_length_b 18.845(2) _cell_length_c 13.537(2) _cell_angle_alpha 103.522(4) _cell_angle_beta 100.57(1) _cell_angle_gamma 90.225(6) _cell_volume 4039.7(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13330 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.956 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27075 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15556 _reflns_number_gt 11905 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2410 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11905 _refine_ls_number_parameters 898 _refine_ls_goodness_of_fit_ref 1.701 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0090 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.79 _refine_diff_density_min -1.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.56323(3) 0.22289(3) 0.21684(4) 0.0386(2) Uani 1.00 d . . . Cr(2) Cr 0.81930(3) 0.22006(3) 0.44736(4) 0.0402(2) Uani 1.00 d . . . Cr(3) Cr 0.76772(4) 0.27758(4) 0.21755(5) 0.0381(2) Uani 0.81 d P . . Cr(3A) Cr 0.6876(2) 0.0816(2) 0.2922(2) 0.0410(6) Uani 0.19 d P . . O(1) O 0.6664(2) 0.2607(2) 0.2035(2) 0.0564(7) Uani 1.00 d . . . O(2) O 0.6122(2) 0.1330(2) 0.2432(2) 0.0476(6) Uani 1.00 d . . . O(3) O 0.5872(1) 0.2634(2) 0.3694(2) 0.0473(6) Uani 1.00 d . . . O(4) O 0.8149(2) 0.2580(2) 0.3272(2) 0.0568(7) Uani 1.00 d . . . O(5) O 0.7431(1) 0.1369(2) 0.3665(2) 0.0471(6) Uani 1.00 d . . . O(6) O 0.7240(1) 0.2742(1) 0.4822(2) 0.0451(6) Uani 1.00 d . . . O(7) O 0.7994(2) 0.2291(2) 0.1199(3) 0.0614(9) Uani 0.81 d P . . O(7A) O 0.7333(8) 0.0413(8) 0.204(1) 0.056(4) Uani 0.19 d P . . O(8) O 0.7888(2) 0.3614(2) 0.2243(3) 0.0618(10) Uani 0.81 d P . . O(8A) O 0.6604(9) 0.0224(8) 0.350(1) 0.062(4) Uani 0.19 d P . . N(11) N 0.4468(2) 0.1841(2) 0.2248(2) 0.0386(6) Uani 1.00 d . . . N(12) N 0.3810(2) 0.1975(2) 0.1546(2) 0.0404(6) Uani 1.00 d . . . N(21) N 0.5088(2) 0.3192(2) 0.1931(2) 0.0446(7) Uani 1.00 d . . . N(22) N 0.4346(2) 0.3138(2) 0.1265(2) 0.0449(7) Uani 1.00 d . . . N(31) N 0.5285(2) 0.1762(2) 0.0581(2) 0.0402(6) Uani 1.00 d . . . N(32) N 0.4543(2) 0.1948(2) 0.0081(2) 0.0394(6) Uani 1.00 d . . . N(41) N 0.8300(2) 0.1777(2) 0.5785(2) 0.0430(7) Uani 1.00 d . . . N(42) N 0.9072(2) 0.1767(2) 0.6377(2) 0.0478(7) Uani 1.00 d . . . N(51) N 0.9025(2) 0.3035(2) 0.5397(3) 0.0498(8) Uani 1.00 d . . . N(52) N 0.9714(2) 0.2842(2) 0.5997(3) 0.0501(8) Uani 1.00 d . . . N(61) N 0.9205(2) 0.1585(2) 0.4132(2) 0.0497(8) Uani 1.00 d . . . N(62) N 0.9854(2) 0.1584(2) 0.4929(2) 0.0508(8) Uani 1.00 d . . . C(11) C 0.4178(2) 0.1453(2) 0.2832(3) 0.0427(8) Uani 1.00 d . . . C(12) C 0.3334(2) 0.1327(2) 0.2496(3) 0.0541(10) Uani 1.00 d . . . C(13) C 0.3120(2) 0.1657(2) 0.1690(3) 0.0493(9) Uani 1.00 d . . . C(14) C 0.4709(2) 0.1150(2) 0.3646(3) 0.0460(8) Uani 1.00 d . . . C(15) C 0.4342(3) 0.1264(3) 0.4627(3) 0.0563(10) Uani 1.00 d . . . C(16) C 0.4805(3) 0.0339(2) 0.3199(4) 0.062(1) Uani 1.00 d . . . C(17) C 0.2283(2) 0.1706(3) 0.1059(3) 0.062(1) Uani 1.00 d . . . C(18) C 0.1947(3) 0.2429(4) 0.1376(5) 0.105(2) Uani 1.00 d . . . C(19) C 0.1698(3) 0.1095(4) 0.1128(5) 0.101(2) Uani 1.00 d . . . C(21) C 0.5310(2) 0.3908(2) 0.2268(3) 0.0511(9) Uani 1.00 d . . . C(22) C 0.4711(3) 0.4313(2) 0.1818(4) 0.065(1) Uani 1.00 d . . . C(23) C 0.4120(3) 0.3821(2) 0.1178(3) 0.0557(10) Uani 1.00 d . . . C(24) C 0.6070(3) 0.4211(2) 0.3052(4) 0.060(1) Uani 1.00 d . . . C(25) C 0.5823(3) 0.4577(3) 0.4079(4) 0.078(1) Uani 1.00 d . . . C(26) C 0.6530(3) 0.4760(3) 0.2652(5) 0.080(1) Uani 1.00 d . . . C(27) C 0.3362(3) 0.3978(3) 0.0481(4) 0.066(1) Uani 1.00 d . . . C(28) C 0.2850(4) 0.4521(4) 0.1100(7) 0.130(3) Uani 1.00 d . . . C(29) C 0.3608(4) 0.4231(5) -0.0399(6) 0.121(3) Uani 1.00 d . . . C(31) C 0.5650(2) 0.1364(2) -0.0156(3) 0.0443(8) Uani 1.00 d . . . C(32) C 0.5153(2) 0.1301(2) -0.1115(3) 0.0499(9) Uani 1.00 d . . . C(33) C 0.4458(2) 0.1672(2) -0.0946(3) 0.0448(8) Uani 1.00 d . . . C(34) C 0.6435(2) 0.0994(2) 0.0077(3) 0.0517(9) Uani 1.00 d . . . C(35) C 0.6245(3) 0.0201(3) 0.0051(4) 0.069(1) Uani 1.00 d . . . C(36) C 0.6990(3) 0.1020(3) -0.0692(3) 0.064(1) Uani 1.00 d . . . C(37) C 0.3724(3) 0.1789(3) -0.1717(3) 0.061(1) Uani 1.00 d . . . C(38) C 0.3133(5) 0.1194(5) -0.1987(8) 0.195(6) Uani 1.00 d . . . C(39) C 0.3950(4) 0.1892(5) -0.2700(5) 0.117(3) Uani 1.00 d . . . C(41) C 0.7761(2) 0.1519(2) 0.6267(3) 0.0475(8) Uani 1.00 d . . . C(42) C 0.8184(3) 0.1349(3) 0.7169(3) 0.058(1) Uani 1.00 d . . . C(43) C 0.9003(2) 0.1505(3) 0.7215(3) 0.0517(9) Uani 1.00 d . . . C(44) C 0.6851(2) 0.1420(2) 0.5875(3) 0.0488(9) Uani 1.00 d . . . C(45) C 0.6394(3) 0.1802(3) 0.6704(4) 0.076(1) Uani 1.00 d . . . C(46) C 0.6609(3) 0.0618(3) 0.5539(5) 0.084(2) Uani 1.00 d . . . C(47) C 0.9722(3) 0.1449(3) 0.8040(3) 0.070(1) Uani 1.00 d . . . C(48) C 0.9983(4) 0.2203(4) 0.8760(5) 0.101(2) Uani 1.00 d . . . C(49) C 0.9508(4) 0.0917(4) 0.8657(4) 0.087(2) Uani 1.00 d . . . C(51) C 0.9074(3) 0.3762(3) 0.5556(4) 0.060(1) Uani 1.00 d . . . C(52) C 0.9788(3) 0.4048(3) 0.6248(4) 0.067(1) Uani 1.00 d . . . C(53) C 1.0179(3) 0.3461(3) 0.6521(3) 0.065(1) Uani 1.00 d . . . C(54) C 0.8433(3) 0.4191(3) 0.5060(5) 0.076(1) Uani 1.00 d . . . C(55) C 0.7999(4) 0.4651(4) 0.5863(7) 0.119(3) Uani 1.00 d . . . C(56) C 0.8813(4) 0.4674(4) 0.4496(6) 0.114(3) Uani 1.00 d . . . C(57) C 1.1007(3) 0.3448(3) 0.7218(4) 0.079(1) Uani 1.00 d . . . C(58) C 1.1166(4) 0.4145(5) 0.8063(6) 0.158(4) Uani 1.00 d . . . C(59) C 1.1687(3) 0.3367(4) 0.6607(6) 0.109(2) Uani 1.00 d . . . C(61) C 0.9401(2) 0.1169(3) 0.3267(3) 0.060(1) Uani 1.00 d . . . C(62) C 1.0182(2) 0.0908(3) 0.3512(4) 0.069(1) Uani 1.00 d . . . C(63) C 1.0449(2) 0.1177(3) 0.4556(3) 0.060(1) Uani 1.00 d . . . C(64) C 0.8842(3) 0.0997(3) 0.2230(3) 0.072(1) Uani 1.00 d . . . C(65) C 0.8456(4) 0.0189(3) 0.1968(4) 0.087(2) Uani 1.00 d . . . C(66) C 0.9294(4) 0.1034(4) 0.1391(5) 0.105(2) Uani 1.00 d . . . C(67) C 1.1242(2) 0.1040(3) 0.5207(3) 0.063(1) Uani 1.00 d . . . C(68) C 1.1212(4) 0.0268(4) 0.5380(6) 0.110(2) Uani 1.00 d . . . C(69) C 1.1959(3) 0.1154(5) 0.4689(5) 0.106(2) Uani 1.00 d . . . C(70) C 0.8234(5) 0.3542(5) 0.8109(9) 0.144(3) Uani 1.00 d . . . C(71) C 0.7899(6) 0.3437(5) 0.8997(8) 0.138(3) Uani 1.00 d . . . C(72) C 0.7064(3) 0.3463(2) 0.8835(3) 0.0548(9) Uani 1.00 d . . . C(73) C 0.6708(6) 0.3376(4) 0.9656(6) 0.115(2) Uani 1.00 d . . . C(74) C 0.5821(5) 0.3402(5) 0.9401(6) 0.119(3) Uani 1.00 d . . . C(75) C 0.5824(5) 0.3705(4) 0.6418(5) 0.102(2) Uani 1.00 d . . . C(76) C 0.4966(4) 0.3443(3) 0.6124(6) 0.093(2) Uani 1.00 d . . . C(77) C 0.4669(3) 0.3401(3) 0.5063(4) 0.0564(10) Uani 1.00 d . . . C(78) C 0.3819(4) 0.3373(4) 0.4788(7) 0.105(2) Uani 1.00 d . . . C(79) C 0.3539(4) 0.3501(5) 0.3763(6) 0.123(3) Uani 1.00 d . . . C(80) C 0.0700(6) 0.3083(6) 0.3781(8) 0.134(3) Uani 1.00 d . . . C(81) C 0.0175(6) 0.3155(8) 0.284(1) 0.184(5) Uani 1.00 d . . . C(82) C 0.0449(4) 0.3656(3) 0.2444(5) 0.080(2) Uani 1.00 d . . . C(83) C -0.0074(7) 0.3762(7) 0.1547(9) 0.160(4) Uani 1.00 d . . . C(84) C 0.0316(7) 0.4217(7) 0.1032(9) 0.163(4) Uani 1.00 d . . . B(1) B 0.3954(2) 0.2378(2) 0.0726(3) 0.0418(8) Uani 1.00 d . . . B(2) B 0.9819(2) 0.2045(3) 0.6027(3) 0.054(1) Uani 1.00 d . . . H(1) H 0.2971 0.1068 0.2773 0.0662 Uiso 1.00 calc . . . H(01) H 0.6459 0.2706 0.4263 0.0636 Uiso 1.00 calc . . . H(2) H 0.5235 0.1411 0.3834 0.0560 Uiso 1.00 calc . . . H(02) H 0.5451 0.2881 0.4051 0.0636 Uiso 1.00 calc . . . H(03) H 0.7355 0.2910 0.5430 0.0636 Uiso 1.00 calc . . . H(3) H 0.4323 0.1778 0.4922 0.0563 Uiso 1.00 calc . . . H(4) H 0.4677 0.1042 0.5119 0.0563 Uiso 1.00 calc . . . H(5) H 0.3796 0.1043 0.4456 0.0563 Uiso 1.00 calc . . . H(6) H 0.4273 0.0095 0.2943 0.0615 Uiso 1.00 calc . . . H(7) H 0.5101 0.0128 0.3730 0.0615 Uiso 1.00 calc . . . H(8) H 0.5103 0.0285 0.2643 0.0615 Uiso 1.00 calc . . . H(9) H 0.3437 0.2418 0.0286 0.0504 Uiso 1.00 calc . . . H(10) H 0.2342 0.1632 0.0357 0.0762 Uiso 1.00 calc . . . H(11) H 0.2334 0.2802 0.1356 0.1047 Uiso 1.00 calc . . . H(12) H 0.1844 0.2498 0.2067 0.1047 Uiso 1.00 calc . . . H(13) H 0.1442 0.2457 0.0911 0.1047 Uiso 1.00 calc . . . H(14) H 0.1583 0.1186 0.1815 0.1007 Uiso 1.00 calc . . . H(15) H 0.1949 0.0634 0.0971 0.1007 Uiso 1.00 calc . . . H(16) H 0.1195 0.1083 0.0641 0.1007 Uiso 1.00 calc . . . H(17) H 0.4715 0.4831 0.1939 0.0786 Uiso 1.00 calc . . . H(18) H 0.6417 0.3814 0.3155 0.0732 Uiso 1.00 calc . . . H(19) H 0.6302 0.4795 0.4572 0.0778 Uiso 1.00 calc . . . H(20) H 0.5566 0.4218 0.4335 0.0778 Uiso 1.00 calc . . . H(21) H 0.5444 0.4949 0.3973 0.0778 Uiso 1.00 calc . . . H(22) H 0.6974 0.5002 0.3187 0.0798 Uiso 1.00 calc . . . H(23) H 0.6160 0.5116 0.2458 0.0798 Uiso 1.00 calc . . . H(24) H 0.6745 0.4507 0.2061 0.0798 Uiso 1.00 calc . . . H(25) H 0.3030 0.3519 0.0214 0.0825 Uiso 1.00 calc . . . H(26) H 0.3199 0.4927 0.1525 0.1300 Uiso 1.00 calc . . . H(27) H 0.2599 0.4284 0.1530 0.1300 Uiso 1.00 calc . . . H(28) H 0.2432 0.4691 0.0632 0.1300 Uiso 1.00 calc . . . H(29) H 0.3830 0.3834 -0.0836 0.1206 Uiso 1.00 calc . . . H(30) H 0.4016 0.4626 -0.0129 0.1206 Uiso 1.00 calc . . . H(31) H 0.3136 0.4396 -0.0793 0.1206 Uiso 1.00 calc . . . H(32) H 0.5272 0.1041 -0.1772 0.0609 Uiso 1.00 calc . . . H(33) H 0.6722 0.1230 0.0763 0.0622 Uiso 1.00 calc . . . H(34) H 0.5871 0.0177 0.0507 0.0695 Uiso 1.00 calc . . . H(35) H 0.6744 -0.0022 0.0271 0.0695 Uiso 1.00 calc . . . H(36) H 0.6000 -0.0053 -0.0641 0.0695 Uiso 1.00 calc . . . H(37) H 0.7503 0.0814 -0.0482 0.0638 Uiso 1.00 calc . . . H(38) H 0.7088 0.1519 -0.0713 0.0638 Uiso 1.00 calc . . . H(39) H 0.6730 0.0745 -0.1367 0.0638 Uiso 1.00 calc . . . H(40) H 0.3487 0.2233 -0.1404 0.0740 Uiso 1.00 calc . . . H(41) H 0.3048 0.1059 -0.1371 0.1950 Uiso 1.00 calc . . . H(42) H 0.3328 0.0785 -0.2436 0.1950 Uiso 1.00 calc . . . H(43) H 0.2625 0.1335 -0.2337 0.1950 Uiso 1.00 calc . . . H(44) H 0.4058 0.1427 -0.3115 0.1168 Uiso 1.00 calc . . . H(45) H 0.4432 0.2212 -0.2538 0.1168 Uiso 1.00 calc . . . H(46) H 0.3505 0.2102 -0.3077 0.1168 Uiso 1.00 calc . . . H(47) H 1.0310 0.1998 0.6490 0.0645 Uiso 1.00 calc . . . H(48) H 0.7952 0.1174 0.7668 0.0690 Uiso 1.00 calc . . . H(49) H 0.6711 0.1634 0.5292 0.0590 Uiso 1.00 calc . . . H(50) H 0.6568 0.2310 0.6922 0.0759 Uiso 1.00 calc . . . H(51) H 0.6509 0.1583 0.7284 0.0759 Uiso 1.00 calc . . . H(52) H 0.5814 0.1755 0.6431 0.0759 Uiso 1.00 calc . . . H(53) H 0.6026 0.0554 0.5291 0.0839 Uiso 1.00 calc . . . H(54) H 0.6757 0.0399 0.6116 0.0839 Uiso 1.00 calc . . . H(55) H 0.6888 0.0389 0.4995 0.0839 Uiso 1.00 calc . . . H(56) H 1.0167 0.1272 0.7712 0.0869 Uiso 1.00 calc . . . H(57) H 1.0505 0.2179 0.9193 0.1011 Uiso 1.00 calc . . . H(58) H 0.9580 0.2352 0.9184 0.1011 Uiso 1.00 calc . . . H(59) H 1.0028 0.2552 0.8354 0.1011 Uiso 1.00 calc . . . H(60) H 0.9053 0.1089 0.8979 0.0869 Uiso 1.00 calc . . . H(61) H 0.9973 0.0884 0.9180 0.0869 Uiso 1.00 calc . . . H(62) H 0.9362 0.0444 0.8201 0.0869 Uiso 1.00 calc . . . H(63) H 0.9971 0.4554 0.6500 0.0834 Uiso 1.00 calc . . . H(64) H 0.8022 0.3859 0.4582 0.0965 Uiso 1.00 calc . . . H(65) H 0.8362 0.5051 0.6281 0.1185 Uiso 1.00 calc . . . H(66) H 0.7846 0.4356 0.6295 0.1185 Uiso 1.00 calc . . . H(67) H 0.7517 0.4838 0.5522 0.1185 Uiso 1.00 calc . . . H(68) H 0.9226 0.5002 0.4977 0.1142 Uiso 1.00 calc . . . H(69) H 0.8395 0.4951 0.4191 0.1142 Uiso 1.00 calc . . . H(70) H 0.9057 0.4374 0.3963 0.1142 Uiso 1.00 calc . . . H(71) H 1.0992 0.3027 0.7521 0.0965 Uiso 1.00 calc . . . H(72) H 1.1638 0.4098 0.8569 0.1582 Uiso 1.00 calc . . . H(73) H 1.0696 0.4234 0.8388 0.1582 Uiso 1.00 calc . . . H(74) H 1.1265 0.4546 0.7768 0.1582 Uiso 1.00 calc . . . H(75) H 1.1558 0.2953 0.6026 0.1088 Uiso 1.00 calc . . . H(76) H 1.2192 0.3296 0.7041 0.1088 Uiso 1.00 calc . . . H(77) H 1.1745 0.3801 0.6364 0.1088 Uiso 1.00 calc . . . H(78) H 1.0468 0.0579 0.3055 0.0795 Uiso 1.00 calc . . . H(79) H 0.8410 0.1324 0.2252 0.0861 Uiso 1.00 calc . . . H(80) H 0.8161 0.0136 0.2495 0.0874 Uiso 1.00 calc . . . H(81) H 0.8887 -0.0150 0.1938 0.0874 Uiso 1.00 calc . . . H(82) H 0.8088 0.0091 0.1311 0.0874 Uiso 1.00 calc . . . H(83) H 0.9702 0.0674 0.1361 0.1050 Uiso 1.00 calc . . . H(84) H 0.9556 0.1511 0.1529 0.1050 Uiso 1.00 calc . . . H(85) H 0.8916 0.0941 0.0741 0.1050 Uiso 1.00 calc . . . H(86) H 1.1315 0.1394 0.5865 0.0768 Uiso 1.00 calc . . . H(87) H 1.0761 0.0212 0.5714 0.1096 Uiso 1.00 calc . . . H(88) H 1.1717 0.0190 0.5810 0.1096 Uiso 1.00 calc . . . H(89) H 1.1141 -0.0082 0.4726 0.1096 Uiso 1.00 calc . . . H(90) H 1.2466 0.1121 0.5145 0.1063 Uiso 1.00 calc . . . H(91) H 1.1940 0.1627 0.4539 0.1063 Uiso 1.00 calc . . . H(92) H 1.1922 0.0784 0.4058 0.1063 Uiso 1.00 calc . . . H(93) H 0.8848 0.3527 0.8243 0.1799 Uiso 1.00 calc . . . H(94) H 0.8047 0.3180 0.7496 0.1799 Uiso 1.00 calc . . . H(95) H 0.8131 0.4016 0.7973 0.1799 Uiso 1.00 calc . . . H(96) H 0.8048 0.2971 0.9135 0.1757 Uiso 1.00 calc . . . H(97) H 0.8136 0.3806 0.9614 0.1757 Uiso 1.00 calc . . . H(98) H 0.6922 0.3939 0.8728 0.0656 Uiso 1.00 calc . . . H(99) H 0.6835 0.3106 0.8233 0.0656 Uiso 1.00 calc . . . H(100) H 0.6834 0.2887 0.9765 0.1413 Uiso 1.00 calc . . . H(101) H 0.6929 0.3720 1.0266 0.1413 Uiso 1.00 calc . . . H(102) H 0.5684 0.3885 0.9280 0.1451 Uiso 1.00 calc . . . H(103) H 0.5590 0.3054 0.8770 0.1451 Uiso 1.00 calc . . . H(104) H 0.5558 0.3333 0.9935 0.1451 Uiso 1.00 calc . . . H(105) H 0.6053 0.3757 0.7137 0.1225 Uiso 1.00 calc . . . H(106) H 0.6166 0.3405 0.6018 0.1225 Uiso 1.00 calc . . . H(107) H 0.5877 0.4197 0.6291 0.1225 Uiso 1.00 calc . . . H(108) H 0.4929 0.2961 0.6274 0.1148 Uiso 1.00 calc . . . H(109) H 0.4640 0.3752 0.6556 0.1148 Uiso 1.00 calc . . . H(110) H 0.4885 0.3824 0.4902 0.0719 Uiso 1.00 calc . . . H(111) H 0.4875 0.2978 0.4660 0.0719 Uiso 1.00 calc . . . H(112) H 0.3609 0.2898 0.4749 0.1314 Uiso 1.00 calc . . . H(113) H 0.3598 0.3727 0.5244 0.1314 Uiso 1.00 calc . . . H(114) H 0.3751 0.3977 0.3730 0.1370 Uiso 1.00 calc . . . H(115) H 0.3756 0.3147 0.3235 0.1370 Uiso 1.00 calc . . . H(116) H 0.2966 0.3482 0.3568 0.1370 Uiso 1.00 calc . . . H(117) H 0.0533 0.2719 0.4090 0.1564 Uiso 1.00 calc . . . H(118) H 0.1252 0.3010 0.3682 0.1564 Uiso 1.00 calc . . . H(119) H 0.0707 0.3554 0.4278 0.1564 Uiso 1.00 calc . . . H(120) H 0.0182 0.2633 0.2397 0.1779 Uiso 1.00 calc . . . H(121) H -0.0360 0.3181 0.2992 0.1779 Uiso 1.00 calc . . . H(122) H 0.0527 0.4094 0.2981 0.0988 Uiso 1.00 calc . . . H(123) H 0.0974 0.3525 0.2272 0.0988 Uiso 1.00 calc . . . H(124) H -0.0293 0.3323 0.1047 0.1965 Uiso 1.00 calc . . . H(125) H -0.0573 0.4030 0.1718 0.1965 Uiso 1.00 calc . . . H(126) H 0.0801 0.3956 0.0845 0.1965 Uiso 1.00 calc . . . H(127) H -0.0003 0.4304 0.0448 0.1965 Uiso 1.00 calc . . . H(128) H 0.0526 0.4662 0.1521 0.1965 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0290(3) 0.0589(4) 0.0261(3) -0.0003(2) 0.0014(2) 0.0096(2) Cr(2) 0.0286(3) 0.0622(4) 0.0313(3) -0.0003(2) 0.0007(2) 0.0182(2) Cr(3) 0.0306(3) 0.0558(4) 0.0320(4) -0.0016(3) 0.0044(2) 0.0196(3) Cr(3A) 0.041(2) 0.045(2) 0.037(2) 0.003(1) 0.005(1) 0.011(1) O(1) 0.040(1) 0.087(2) 0.042(2) -0.009(1) 0.005(1) 0.018(1) O(2) 0.040(1) 0.067(2) 0.039(1) 0.010(1) 0.006(1) 0.020(1) O(3) 0.040(1) 0.067(2) 0.030(1) 0.002(1) 0.0005(10) 0.006(1) O(4) 0.051(2) 0.085(2) 0.038(2) -0.010(1) 0.000(1) 0.027(1) O(5) 0.037(1) 0.065(2) 0.040(2) 0.006(1) 0.0028(10) 0.018(1) O(6) 0.038(1) 0.061(2) 0.034(1) 0.002(1) -0.0006(9) 0.012(1) O(7) 0.054(2) 0.097(3) 0.038(2) 0.018(2) 0.013(1) 0.022(2) O(7A) 0.033(7) 0.060(9) 0.07(1) -0.011(6) 0.008(6) 0.002(7) O(8) 0.044(2) 0.069(2) 0.080(3) -0.011(1) 0.003(2) 0.040(2) O(8A) 0.056(9) 0.055(9) 0.08(1) 0.002(7) 0.002(8) 0.030(8) N(11) 0.032(1) 0.054(2) 0.029(2) 0.000(1) 0.002(1) 0.013(1) N(12) 0.031(1) 0.056(2) 0.032(2) 0.000(1) 0.003(1) 0.009(1) N(21) 0.042(2) 0.053(2) 0.033(2) -0.001(1) -0.004(1) 0.009(1) N(22) 0.042(2) 0.055(2) 0.032(2) 0.004(1) -0.003(1) 0.010(1) N(31) 0.034(1) 0.057(2) 0.028(2) 0.003(1) 0.002(1) 0.010(1) N(32) 0.033(1) 0.054(2) 0.030(2) -0.001(1) 0.002(1) 0.010(1) N(41) 0.033(1) 0.068(2) 0.032(2) 0.005(1) 0.002(1) 0.022(1) N(42) 0.039(2) 0.079(2) 0.027(2) 0.012(1) 0.002(1) 0.020(1) N(51) 0.034(2) 0.072(2) 0.042(2) -0.007(1) -0.005(1) 0.020(2) N(52) 0.032(1) 0.080(2) 0.036(2) -0.005(1) -0.004(1) 0.018(2) N(61) 0.026(1) 0.091(2) 0.034(2) 0.010(1) 0.006(1) 0.018(2) N(62) 0.031(1) 0.089(2) 0.033(2) 0.011(1) 0.003(1) 0.018(2) C(11) 0.037(2) 0.057(2) 0.035(2) -0.003(1) 0.007(1) 0.013(2) C(12) 0.039(2) 0.080(3) 0.044(2) -0.012(2) 0.008(2) 0.017(2) C(13) 0.030(2) 0.081(3) 0.034(2) -0.003(2) 0.005(1) 0.009(2) C(14) 0.044(2) 0.059(2) 0.037(2) -0.004(1) 0.005(1) 0.016(2) C(15) 0.060(2) 0.068(3) 0.044(2) 0.003(2) 0.013(2) 0.017(2) C(16) 0.070(3) 0.068(3) 0.046(3) 0.004(2) 0.008(2) 0.013(2) C(17) 0.032(2) 0.109(4) 0.042(2) -0.004(2) 0.002(1) 0.015(2) C(18) 0.052(3) 0.158(6) 0.091(5) 0.030(3) -0.003(3) 0.016(4) C(19) 0.049(3) 0.168(6) 0.083(4) -0.032(3) -0.014(3) 0.047(4) C(21) 0.051(2) 0.053(2) 0.044(2) -0.006(2) -0.002(2) 0.010(2) C(22) 0.070(3) 0.046(2) 0.069(3) 0.004(2) -0.008(2) 0.014(2) C(23) 0.057(2) 0.057(2) 0.047(2) 0.009(2) -0.005(2) 0.013(2) C(24) 0.055(2) 0.061(3) 0.053(3) -0.010(2) -0.012(2) 0.009(2) C(25) 0.085(3) 0.075(3) 0.058(3) -0.005(2) -0.016(2) 0.009(2) C(26) 0.061(3) 0.083(4) 0.090(4) -0.015(2) 0.003(3) 0.020(3) C(27) 0.064(3) 0.057(3) 0.068(3) 0.009(2) -0.012(2) 0.016(2) C(28) 0.092(4) 0.128(6) 0.135(7) 0.056(4) -0.022(4) -0.006(5) C(29) 0.098(5) 0.170(7) 0.099(6) 0.004(4) -0.024(4) 0.077(5) C(31) 0.039(2) 0.060(2) 0.033(2) 0.002(1) 0.008(1) 0.009(2) C(32) 0.048(2) 0.070(3) 0.028(2) 0.006(2) 0.006(1) 0.006(2) C(33) 0.041(2) 0.063(2) 0.027(2) 0.000(1) 0.000(1) 0.009(2) C(34) 0.044(2) 0.076(3) 0.034(2) 0.011(2) 0.006(1) 0.012(2) C(35) 0.058(3) 0.086(3) 0.065(3) 0.018(2) 0.006(2) 0.023(3) C(36) 0.049(2) 0.094(3) 0.046(3) 0.004(2) 0.013(2) 0.010(2) C(37) 0.051(2) 0.094(3) 0.031(2) 0.007(2) -0.003(2) 0.008(2) C(38) 0.159(8) 0.198(9) 0.206(10) -0.118(7) -0.139(7) 0.140(8) C(39) 0.080(4) 0.206(8) 0.079(5) 0.003(4) -0.009(3) 0.080(5) C(41) 0.043(2) 0.066(2) 0.040(2) 0.011(2) 0.011(1) 0.025(2) C(42) 0.057(2) 0.090(3) 0.038(2) 0.019(2) 0.015(2) 0.031(2) C(43) 0.044(2) 0.083(3) 0.034(2) 0.015(2) 0.009(1) 0.025(2) C(44) 0.036(2) 0.071(3) 0.049(2) 0.007(2) 0.011(1) 0.030(2) C(45) 0.049(2) 0.115(4) 0.067(3) 0.020(2) 0.019(2) 0.023(3) C(46) 0.050(3) 0.081(4) 0.126(5) 0.001(2) 0.019(3) 0.035(3) C(47) 0.059(3) 0.123(4) 0.034(2) 0.029(3) 0.006(2) 0.031(2) C(48) 0.095(4) 0.139(6) 0.055(4) 0.004(4) -0.022(3) 0.024(3) C(49) 0.091(4) 0.131(5) 0.053(3) 0.045(3) 0.014(3) 0.049(3) C(51) 0.048(2) 0.072(3) 0.057(3) -0.014(2) -0.006(2) 0.024(2) C(52) 0.049(2) 0.084(3) 0.063(3) -0.019(2) -0.011(2) 0.023(2) C(53) 0.040(2) 0.102(4) 0.045(3) -0.017(2) -0.006(2) 0.016(2) C(54) 0.051(3) 0.072(3) 0.097(4) -0.015(2) -0.021(2) 0.033(3) C(55) 0.067(4) 0.114(5) 0.152(7) 0.008(3) -0.028(4) 0.024(5) C(56) 0.099(5) 0.099(4) 0.140(6) -0.039(3) -0.047(4) 0.075(4) C(57) 0.045(2) 0.114(4) 0.065(3) -0.012(2) -0.017(2) 0.019(3) C(58) 0.084(5) 0.220(10) 0.104(6) 0.005(5) -0.041(4) -0.047(6) C(59) 0.044(3) 0.148(6) 0.128(6) 0.002(3) -0.003(3) 0.034(5) C(61) 0.039(2) 0.103(3) 0.038(2) 0.012(2) 0.004(2) 0.015(2) C(62) 0.039(2) 0.119(4) 0.044(3) 0.021(2) 0.006(2) 0.007(2) C(63) 0.030(2) 0.103(3) 0.045(2) 0.010(2) 0.007(1) 0.012(2) C(64) 0.051(2) 0.127(4) 0.035(2) 0.024(2) 0.005(2) 0.017(2) C(65) 0.085(4) 0.106(4) 0.059(3) 0.006(3) -0.007(3) 0.012(3) C(66) 0.094(4) 0.172(7) 0.055(4) 0.045(4) 0.021(3) 0.034(4) C(67) 0.029(2) 0.102(4) 0.050(3) 0.009(2) -0.002(2) 0.009(2) C(68) 0.061(3) 0.142(6) 0.126(6) -0.002(3) -0.019(3) 0.061(5) C(69) 0.035(3) 0.186(7) 0.109(5) 0.016(3) 0.017(3) 0.054(5) C(70) 0.108(6) 0.136(7) 0.21(1) 0.025(5) 0.049(6) 0.065(7) C(71) 0.130(7) 0.147(7) 0.144(8) 0.045(6) 0.011(6) 0.059(6) C(72) 0.063(2) 0.056(2) 0.045(2) 0.006(2) 0.001(2) 0.018(2) C(73) 0.160(7) 0.115(5) 0.081(5) 0.034(5) 0.014(5) 0.047(4) C(74) 0.115(6) 0.144(7) 0.108(6) -0.014(5) 0.049(5) 0.030(5) C(75) 0.107(5) 0.138(6) 0.065(4) 0.025(4) 0.015(3) 0.029(4) C(76) 0.103(4) 0.077(4) 0.112(5) 0.020(3) 0.039(4) 0.032(3) C(77) 0.048(2) 0.069(3) 0.054(3) 0.007(2) 0.007(2) 0.021(2) C(78) 0.103(5) 0.082(4) 0.124(6) 0.005(3) 0.025(4) 0.010(4) C(79) 0.103(5) 0.147(7) 0.080(5) 0.026(4) -0.019(4) -0.022(4) C(80) 0.107(6) 0.175(8) 0.138(8) -0.023(5) 0.046(5) 0.053(6) C(81) 0.101(7) 0.25(1) 0.17(1) 0.004(8) 0.026(7) -0.012(10) C(82) 0.059(3) 0.098(4) 0.080(4) -0.022(3) 0.020(3) 0.009(3) C(83) 0.133(8) 0.19(1) 0.146(10) -0.008(7) 0.028(7) 0.015(8) C(84) 0.137(8) 0.22(1) 0.154(10) 0.022(7) 0.038(7) 0.083(9) B(1) 0.034(2) 0.055(2) 0.034(2) 0.004(2) -0.002(1) 0.013(2) B(2) 0.029(2) 0.098(4) 0.033(2) 0.007(2) -0.001(1) 0.017(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) O(1) 1.905(3) . . yes Cr(1) O(2) 1.961(3) . . yes Cr(1) O(3) 1.992(2) . . yes Cr(1) N(11) 2.092(3) . . yes Cr(1) N(21) 2.096(3) . . yes Cr(1) N(31) 2.093(3) . . yes Cr(2) O(4) 1.915(3) . . yes Cr(2) O(5) 1.982(2) . . yes Cr(2) O(6) 1.955(3) . . yes Cr(2) N(41) 2.091(3) . . yes Cr(2) N(51) 2.091(3) . . yes Cr(2) N(61) 2.105(3) . . yes Cr(3) O(1) 1.678(3) . . yes Cr(3) O(4) 1.668(3) . . yes Cr(3) O(7) 1.598(4) . . yes Cr(3) O(8) 1.594(4) . . yes Cr(3A) O(2) 1.716(4) . . yes Cr(3A) O(5) 1.452(3) . . yes Cr(3A) O(7A) 1.58(2) . . yes Cr(3A) O(8A) 1.61(2) . . yes N(11) N(12) 1.375(4) . . yes N(11) C(11) 1.342(5) . . yes N(12) C(13) 1.356(5) . . yes N(12) B(1) 1.536(6) . . yes N(21) N(22) 1.374(4) . . yes N(21) C(21) 1.346(5) . . yes N(22) C(23) 1.367(6) . . yes N(22) B(1) 1.528(5) . . yes N(31) N(32) 1.381(4) . . yes N(31) C(31) 1.341(5) . . yes N(32) C(33) 1.346(4) . . yes N(32) B(1) 1.536(5) . . yes N(41) N(42) 1.383(4) . . yes N(41) C(41) 1.349(6) . . yes N(42) C(43) 1.362(6) . . yes N(42) B(2) 1.535(6) . . yes N(51) N(52) 1.379(4) . . yes N(51) C(51) 1.337(6) . . yes N(52) C(53) 1.365(6) . . yes N(52) B(2) 1.522(7) . . yes N(61) N(62) 1.378(4) . . yes N(61) C(61) 1.343(5) . . yes N(62) C(63) 1.351(5) . . yes N(62) B(2) 1.547(5) . . yes C(11) C(12) 1.392(5) . . yes C(11) C(14) 1.502(5) . . yes C(12) C(13) 1.371(7) . . yes C(13) C(17) 1.505(5) . . yes C(14) C(15) 1.531(6) . . yes C(14) C(16) 1.528(6) . . yes C(17) C(18) 1.474(9) . . yes C(17) C(19) 1.533(9) . . yes C(21) C(22) 1.393(6) . . yes C(21) C(24) 1.505(5) . . yes C(22) C(23) 1.369(6) . . yes C(23) C(27) 1.503(6) . . yes C(24) C(25) 1.530(7) . . yes C(24) C(26) 1.534(8) . . yes C(27) C(28) 1.528(9) . . yes C(27) C(29) 1.50(1) . . yes C(31) C(32) 1.383(5) . . yes C(31) C(34) 1.496(5) . . yes C(32) C(33) 1.377(5) . . yes C(33) C(37) 1.505(5) . . yes C(34) C(35) 1.518(7) . . yes C(34) C(36) 1.520(7) . . yes C(37) C(38) 1.42(1) . . yes C(37) C(39) 1.500(9) . . yes C(41) C(42) 1.399(6) . . yes C(41) C(44) 1.501(5) . . yes C(42) C(43) 1.375(6) . . yes C(43) C(47) 1.499(6) . . yes C(44) C(45) 1.514(7) . . yes C(44) C(46) 1.503(7) . . yes C(47) C(48) 1.533(8) . . yes C(47) C(49) 1.526(9) . . yes C(51) C(52) 1.387(6) . . yes C(51) C(54) 1.494(7) . . yes C(52) C(53) 1.375(8) . . yes C(53) C(57) 1.520(6) . . yes C(54) C(55) 1.516(10) . . yes C(54) C(56) 1.52(1) . . yes C(57) C(58) 1.513(10) . . yes C(57) C(59) 1.505(9) . . yes C(61) C(62) 1.397(6) . . yes C(61) C(64) 1.498(6) . . yes C(62) C(63) 1.373(6) . . yes C(63) C(67) 1.503(6) . . yes C(64) C(65) 1.585(9) . . yes C(64) C(66) 1.485(9) . . yes C(67) C(68) 1.529(10) . . yes C(67) C(69) 1.524(8) . . yes C(70) C(71) 1.47(2) . . yes C(71) C(72) 1.36(1) . . yes C(72) C(73) 1.39(1) . . yes C(73) C(74) 1.45(1) . . yes C(75) C(76) 1.457(10) . . yes C(76) C(77) 1.414(9) . . yes C(77) C(78) 1.388(8) . . yes C(78) C(79) 1.46(1) . . yes C(80) C(81) 1.44(2) . . yes C(81) C(82) 1.31(2) . . yes C(82) C(83) 1.41(1) . . yes C(83) C(84) 1.44(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cr(1) O(2) 91.4(1) . . . yes O(1) Cr(1) O(3) 91.5(1) . . . yes O(1) Cr(1) N(11) 176.7(1) . . . yes O(1) Cr(1) N(21) 90.1(1) . . . yes O(1) Cr(1) N(31) 93.5(1) . . . yes O(2) Cr(1) O(3) 87.3(1) . . . yes O(2) Cr(1) N(11) 91.2(1) . . . yes O(2) Cr(1) N(21) 177.9(1) . . . yes O(2) Cr(1) N(31) 92.3(1) . . . yes O(3) Cr(1) N(11) 90.6(1) . . . yes O(3) Cr(1) N(21) 91.2(1) . . . yes O(3) Cr(1) N(31) 175.0(1) . . . yes N(11) Cr(1) N(21) 87.4(1) . . . yes N(11) Cr(1) N(31) 84.5(1) . . . yes N(21) Cr(1) N(31) 89.1(1) . . . yes O(4) Cr(2) O(5) 90.8(1) . . . yes O(4) Cr(2) O(6) 91.2(1) . . . yes O(4) Cr(2) N(41) 177.3(1) . . . yes O(4) Cr(2) N(51) 92.8(1) . . . yes O(4) Cr(2) N(61) 91.0(1) . . . yes O(5) Cr(2) O(6) 88.47(10) . . . yes O(5) Cr(2) N(41) 90.4(1) . . . yes O(5) Cr(2) N(51) 176.1(1) . . . yes O(5) Cr(2) N(61) 90.4(1) . . . yes O(6) Cr(2) N(41) 91.4(1) . . . yes O(6) Cr(2) N(51) 93.0(1) . . . yes O(6) Cr(2) N(61) 177.5(1) . . . yes N(41) Cr(2) N(51) 86.0(1) . . . yes N(41) Cr(2) N(61) 86.5(1) . . . yes N(51) Cr(2) N(61) 88.0(1) . . . yes O(1) Cr(3) O(4) 108.8(2) . . . yes O(1) Cr(3) O(7) 109.0(2) . . . yes O(1) Cr(3) O(8) 111.5(2) . . . yes O(4) Cr(3) O(7) 111.1(2) . . . yes O(4) Cr(3) O(8) 108.1(2) . . . yes O(7) Cr(3) O(8) 108.3(2) . . . yes O(2) Cr(3A) O(5) 102.3(2) . . . yes O(2) Cr(3A) O(7A) 110.1(6) . . . yes O(2) Cr(3A) O(8A) 117.2(6) . . . yes O(5) Cr(3A) O(7A) 109.4(5) . . . yes O(5) Cr(3A) O(8A) 108.9(6) . . . yes O(7A) Cr(3A) O(8A) 108.6(8) . . . yes Cr(1) O(1) Cr(3) 162.0(2) . . . yes Cr(1) O(2) Cr(3A) 155.6(2) . . . yes Cr(2) O(4) Cr(3) 154.0(2) . . . yes Cr(2) O(5) Cr(3A) 170.0(3) . . . yes Cr(1) N(11) N(12) 117.7(2) . . . yes Cr(1) N(11) C(11) 135.0(2) . . . yes N(12) N(11) C(11) 107.3(3) . . . yes N(11) N(12) C(13) 109.0(3) . . . yes N(11) N(12) B(1) 119.5(3) . . . yes C(13) N(12) B(1) 131.3(3) . . . yes Cr(1) N(21) N(22) 118.6(2) . . . yes Cr(1) N(21) C(21) 134.5(2) . . . yes N(22) N(21) C(21) 106.9(3) . . . yes N(21) N(22) C(23) 109.3(3) . . . yes N(21) N(22) B(1) 118.6(3) . . . yes C(23) N(22) B(1) 132.0(3) . . . yes Cr(1) N(31) N(32) 117.4(2) . . . yes Cr(1) N(31) C(31) 135.6(2) . . . yes N(32) N(31) C(31) 106.5(3) . . . yes N(31) N(32) C(33) 109.7(3) . . . yes N(31) N(32) B(1) 119.2(3) . . . yes C(33) N(32) B(1) 131.0(3) . . . yes Cr(2) N(41) N(42) 118.5(2) . . . yes Cr(2) N(41) C(41) 134.6(2) . . . yes N(42) N(41) C(41) 106.8(3) . . . yes N(41) N(42) C(43) 109.3(3) . . . yes N(41) N(42) B(2) 118.9(3) . . . yes C(43) N(42) B(2) 131.8(3) . . . yes Cr(2) N(51) N(52) 118.1(3) . . . yes Cr(2) N(51) C(51) 135.0(3) . . . yes N(52) N(51) C(51) 106.9(3) . . . yes N(51) N(52) C(53) 108.7(4) . . . yes N(51) N(52) B(2) 119.7(3) . . . yes C(53) N(52) B(2) 131.5(3) . . . yes Cr(2) N(61) N(62) 118.1(2) . . . yes Cr(2) N(61) C(61) 134.8(2) . . . yes N(62) N(61) C(61) 107.1(3) . . . yes N(61) N(62) C(63) 109.4(3) . . . yes N(61) N(62) B(2) 119.1(3) . . . yes C(63) N(62) B(2) 131.5(3) . . . yes N(11) C(11) C(12) 109.1(3) . . . yes N(11) C(11) C(14) 124.2(3) . . . yes C(12) C(11) C(14) 126.5(4) . . . yes C(11) C(12) C(13) 106.6(4) . . . yes N(12) C(13) C(12) 108.0(3) . . . yes N(12) C(13) C(17) 123.0(4) . . . yes C(12) C(13) C(17) 129.0(4) . . . yes C(11) C(14) C(15) 111.3(3) . . . yes C(11) C(14) C(16) 108.5(3) . . . yes C(15) C(14) C(16) 110.9(4) . . . yes C(13) C(17) C(18) 111.8(4) . . . yes C(13) C(17) C(19) 110.2(4) . . . yes C(18) C(17) C(19) 111.1(4) . . . yes N(21) C(21) C(22) 109.5(3) . . . yes N(21) C(21) C(24) 124.3(4) . . . yes C(22) C(21) C(24) 126.2(4) . . . yes C(21) C(22) C(23) 106.7(4) . . . yes N(22) C(23) C(22) 107.6(4) . . . yes N(22) C(23) C(27) 124.7(3) . . . yes C(22) C(23) C(27) 127.7(4) . . . yes C(21) C(24) C(25) 109.0(4) . . . yes C(21) C(24) C(26) 109.4(4) . . . yes C(25) C(24) C(26) 110.9(4) . . . yes C(23) C(27) C(28) 110.4(4) . . . yes C(23) C(27) C(29) 109.1(4) . . . yes C(28) C(27) C(29) 113.4(6) . . . yes N(31) C(31) C(32) 109.5(3) . . . yes N(31) C(31) C(34) 123.2(3) . . . yes C(32) C(31) C(34) 127.0(3) . . . yes C(31) C(32) C(33) 106.8(3) . . . yes N(32) C(33) C(32) 107.4(3) . . . yes N(32) C(33) C(37) 123.3(3) . . . yes C(32) C(33) C(37) 129.3(3) . . . yes C(31) C(34) C(35) 109.6(3) . . . yes C(31) C(34) C(36) 112.2(4) . . . yes C(35) C(34) C(36) 108.7(4) . . . yes C(33) C(37) C(38) 111.8(6) . . . yes C(33) C(37) C(39) 112.6(4) . . . yes C(38) C(37) C(39) 107.5(6) . . . yes N(41) C(41) C(42) 109.4(3) . . . yes N(41) C(41) C(44) 124.6(4) . . . yes C(42) C(41) C(44) 125.9(4) . . . yes C(41) C(42) C(43) 106.5(4) . . . yes N(42) C(43) C(42) 108.0(3) . . . yes N(42) C(43) C(47) 123.2(4) . . . yes C(42) C(43) C(47) 128.8(4) . . . yes C(41) C(44) C(45) 110.5(3) . . . yes C(41) C(44) C(46) 109.3(4) . . . yes C(45) C(44) C(46) 110.7(4) . . . yes C(43) C(47) C(48) 110.3(5) . . . yes C(43) C(47) C(49) 110.2(4) . . . yes C(48) C(47) C(49) 110.3(4) . . . yes N(51) C(51) C(52) 110.2(4) . . . yes N(51) C(51) C(54) 123.7(3) . . . yes C(52) C(51) C(54) 126.0(4) . . . yes C(51) C(52) C(53) 106.1(4) . . . yes N(52) C(53) C(52) 108.1(4) . . . yes N(52) C(53) C(57) 122.9(5) . . . yes C(52) C(53) C(57) 128.9(4) . . . yes C(51) C(54) C(55) 110.6(5) . . . yes C(51) C(54) C(56) 110.5(4) . . . yes C(55) C(54) C(56) 110.3(5) . . . yes C(53) C(57) C(58) 109.9(5) . . . yes C(53) C(57) C(59) 110.9(5) . . . yes C(58) C(57) C(59) 109.4(5) . . . yes N(61) C(61) C(62) 108.9(3) . . . yes N(61) C(61) C(64) 124.2(4) . . . yes C(62) C(61) C(64) 126.9(4) . . . yes C(61) C(62) C(63) 106.7(4) . . . yes N(62) C(63) C(62) 107.8(3) . . . yes N(62) C(63) C(67) 124.4(4) . . . yes C(62) C(63) C(67) 127.7(4) . . . yes C(61) C(64) C(65) 110.3(5) . . . yes C(61) C(64) C(66) 111.5(4) . . . yes C(65) C(64) C(66) 106.3(5) . . . yes C(63) C(67) C(68) 110.1(4) . . . yes C(63) C(67) C(69) 110.0(4) . . . yes C(68) C(67) C(69) 111.0(5) . . . yes C(70) C(71) C(72) 112.1(8) . . . yes C(71) C(72) C(73) 115.0(7) . . . yes C(72) C(73) C(74) 110.7(7) . . . yes C(75) C(76) C(77) 110.7(6) . . . yes C(76) C(77) C(78) 114.2(6) . . . yes C(77) C(78) C(79) 112.5(7) . . . yes C(80) C(81) C(82) 113.1(9) . . . yes C(81) C(82) C(83) 114.2(8) . . . yes C(82) C(83) C(84) 112.2(9) . . . yes N(12) B(1) N(22) 109.2(3) . . . yes N(12) B(1) N(32) 109.0(3) . . . yes N(22) B(1) N(32) 109.0(3) . . . yes N(42) B(2) N(52) 108.7(3) . . . yes N(42) B(2) N(62) 108.5(3) . . . yes N(52) B(2) N(62) 109.6(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(7A) C(38) 3.10(2) . 2_655 ? O(8A) C(38) 3.05(2) . 2_655 ? O(1) O(4) 2.721(4) . . ? O(1) O(2) 2.767(4) . . ? O(1) O(3) 2.793(4) . . ? O(2) O(3) 2.727(4) . . ? O(4) O(6) 2.764(4) . . ? O(4) O(5) 2.774(4) . . ? O(5) O(6) 2.746(4) . . ? #------------------------------------------------------------------------------ #===END data_compound_9 _database_code_CSD 217500 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C74 H144 B2 Cr6 N12 O16 ' _chemical_formula_moiety 'C74 H144 B2 Cr6 N12 O16 ' _chemical_formula_weight 1791.62 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.7618(4) _cell_length_b 16.9666(3) _cell_length_c 24.6837(4) _cell_angle_alpha 90 _cell_angle_beta 103.783(3) _cell_angle_gamma 90 _cell_volume 4784.0(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 23173 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.931 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 29001 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10442 _reflns_number_gt 4254 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2583 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4254 _refine_ls_number_parameters 458 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0590 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.11 _refine_diff_density_min -0.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.10751(9) 0.13949(6) 0.10674(4) 0.0388(3) Uani 1.00 d . . . Cr(2) Cr 0.1469(1) -0.10729(8) -0.00683(5) 0.0622(4) Uani 1.00 d . . . Cr(3) Cr 0.0744(1) -0.07284(6) 0.11231(5) 0.0535(3) Uani 1.00 d . . . O(1) O 0.1665(4) 0.1356(3) 0.0350(2) 0.050(1) Uani 1.00 d . . . O(2) O 0.0901(4) 0.0242(3) 0.1055(2) 0.051(1) Uani 1.00 d . . . O(3) O 0.0527(4) -0.1501(2) -0.0600(2) 0.046(1) Uani 1.00 d . . . O(4) O 0.1532(6) -0.0143(3) -0.0154(2) 0.081(2) Uani 1.00 d . . . O(5) O 0.2741(5) -0.1449(5) 0.0002(3) 0.123(3) Uani 1.00 d . . . O(6) O 0.1013(8) -0.1244(3) 0.0549(2) 0.114(3) Uani 1.00 d . . . O(7) O -0.0536(6) -0.0946(4) 0.1181(5) 0.157(4) Uani 1.00 d . . . O(8) O 0.1610(6) -0.1059(4) 0.1649(2) 0.098(2) Uani 1.00 d . . . N(11) N 0.0560(4) 0.1505(3) 0.1796(2) 0.042(1) Uani 1.00 d . . . N(12) N 0.1246(5) 0.1952(3) 0.2216(2) 0.041(1) Uani 1.00 d . . . N(21) N 0.1244(5) 0.2612(3) 0.1079(2) 0.045(1) Uani 1.00 d . . . N(22) N 0.1817(5) 0.2958(3) 0.1582(2) 0.043(1) Uani 1.00 d . . . N(31) N 0.2813(4) 0.1314(3) 0.1525(2) 0.039(1) Uani 1.00 d . . . N(32) N 0.3185(4) 0.1849(3) 0.1959(2) 0.041(1) Uani 1.00 d . . . C(11) C -0.0347(6) 0.1219(4) 0.1997(3) 0.047(2) Uani 1.00 d . . . C(12) C -0.0209(6) 0.1474(4) 0.2543(3) 0.051(2) Uani 1.00 d . . . C(13) C 0.0784(6) 0.1929(4) 0.2677(3) 0.047(2) Uani 1.00 d . . . C(14) C -0.1357(6) 0.0756(4) 0.1639(3) 0.059(2) Uani 1.00 d . . . C(15) C -0.2383(7) 0.1344(6) 0.1405(4) 0.084(3) Uani 1.00 d . . . C(16) C -0.1762(9) 0.0104(5) 0.1980(4) 0.097(3) Uani 1.00 d . . . C(17) C 0.1333(8) 0.2347(4) 0.3214(3) 0.061(2) Uani 1.00 d . . . C(18) C 0.0516(10) 0.2343(5) 0.3606(4) 0.099(4) Uani 1.00 d . . . C(19) C 0.2521(8) 0.1978(5) 0.3515(3) 0.083(3) Uani 1.00 d . . . C(21) C 0.0891(7) 0.3202(4) 0.0712(3) 0.054(2) Uani 1.00 d . . . C(22) C 0.1260(8) 0.3923(4) 0.0980(3) 0.072(2) Uani 1.00 d . . . C(23) C 0.1851(7) 0.3753(4) 0.1526(3) 0.057(2) Uani 1.00 d . . . C(24) C 0.0160(8) 0.3092(5) 0.0124(3) 0.068(2) Uani 1.00 d . . . C(25) C 0.0653(10) 0.3575(6) -0.0284(4) 0.105(4) Uani 1.00 d . . . C(26) C -0.1124(9) 0.3324(6) 0.0109(4) 0.099(3) Uani 1.00 d . . . C(27) C 0.245(1) 0.4306(5) 0.1981(4) 0.091(3) Uani 1.00 d . . . C(28) C 0.3538(10) 0.4651(7) 0.1828(7) 0.154(6) Uani 1.00 d . . . C(29) C 0.164(1) 0.4977(6) 0.2062(5) 0.127(5) Uani 1.00 d . . . C(31) C 0.3744(5) 0.0871(4) 0.1490(3) 0.040(1) Uani 1.00 d . . . C(32) C 0.4718(6) 0.1119(4) 0.1901(3) 0.051(2) Uani 1.00 d . . . C(33) C 0.4355(6) 0.1726(4) 0.2193(3) 0.046(2) Uani 1.00 d . . . C(34) C 0.3704(6) 0.0207(4) 0.1077(3) 0.051(2) Uani 1.00 d . . . C(35) C 0.4404(7) 0.0388(5) 0.0644(3) 0.073(2) Uani 1.00 d . . . C(36) C 0.4184(8) -0.0549(5) 0.1382(4) 0.082(3) Uani 1.00 d . . . C(37) C 0.5053(7) 0.2217(5) 0.2657(3) 0.064(2) Uani 1.00 d . . . C(38) C 0.5792(10) 0.2822(6) 0.2459(5) 0.113(4) Uani 1.00 d . . . C(39) C 0.586(1) 0.1709(7) 0.3086(4) 0.132(5) Uani 1.00 d . . . C(40) C 0.617(3) 0.532(2) 0.093(1) 0.3078(2) Uiso 1.00 d . . . C(41) C 0.711(2) 0.478(2) 0.103(1) 0.2473(1) Uiso 1.00 d . . . C(42) C 0.748(1) 0.4485(9) 0.1500(7) 0.13669(6) Uiso 1.00 d . . . C(43) C 0.822(3) 0.393(2) 0.155(1) 0.2816(2) Uiso 1.00 d . . . C(44) C 0.873(2) 0.364(1) 0.204(1) 0.2191(1) Uiso 1.00 d . . . C(45) C 0.312(1) 0.1602(8) -0.0753(6) 0.12788(5) Uiso 1.00 d . . . C(46) C 0.375(2) 0.218(1) -0.0363(9) 0.20658(10) Uiso 1.00 d . . . C(47) C 0.3311(7) 0.2272(4) 0.0101(3) 0.05551(2) Uiso 1.00 d . . . C(48) C 0.423(4) 0.260(3) 0.036(2) 0.4340(3) Uiso 1.00 d . . . C(49) C 0.429(2) 0.286(1) 0.0751(10) 0.2056(1) Uiso 1.00 d . . . B(1) B 0.2302(6) 0.2427(4) 0.2101(3) 0.039(2) Uani 1.00 d . . . H(3) H 0.2686 0.2838 0.2419 0.0686 Uiso 1.00 calc . . . H(4) H -0.0738 0.1355 0.2786 0.0611 Uiso 1.00 calc . . . H(5) H -0.1095 0.0510 0.1333 0.0729 Uiso 1.00 calc . . . H(6) H -0.2668 0.1557 0.1708 0.0843 Uiso 1.00 calc . . . H(7) H -0.3006 0.1070 0.1153 0.0843 Uiso 1.00 calc . . . H(8) H -0.2105 0.1765 0.1211 0.0843 Uiso 1.00 calc . . . H(9) H -0.1917 0.0327 0.2313 0.0966 Uiso 1.00 calc . . . H(10) H -0.1160 -0.0288 0.2079 0.0966 Uiso 1.00 calc . . . H(11) H -0.2462 -0.0134 0.1761 0.0966 Uiso 1.00 calc . . . H(12) H 0.1470 0.2889 0.3127 0.0755 Uiso 1.00 calc . . . H(13) H 0.0891 0.2597 0.3949 0.0991 Uiso 1.00 calc . . . H(14) H 0.0329 0.1808 0.3680 0.0991 Uiso 1.00 calc . . . H(15) H -0.0190 0.2620 0.3436 0.0991 Uiso 1.00 calc . . . H(16) H 0.2391 0.1462 0.3649 0.0829 Uiso 1.00 calc . . . H(17) H 0.2891 0.2306 0.3824 0.0829 Uiso 1.00 calc . . . H(18) H 0.3017 0.1938 0.3259 0.0829 Uiso 1.00 calc . . . H(19) H 0.1135 0.4439 0.0817 0.0866 Uiso 1.00 calc . . . H(20) H 0.0158 0.2539 0.0027 0.0850 Uiso 1.00 calc . . . H(21) H 0.1468 0.3453 -0.0239 0.1047 Uiso 1.00 calc . . . H(22) H 0.0569 0.4126 -0.0214 0.1047 Uiso 1.00 calc . . . H(23) H 0.0236 0.3453 -0.0659 0.1047 Uiso 1.00 calc . . . H(24) H -0.1173 0.3884 0.0155 0.0992 Uiso 1.00 calc . . . H(25) H -0.1371 0.3061 0.0406 0.0992 Uiso 1.00 calc . . . H(26) H -0.1623 0.3171 -0.0242 0.0992 Uiso 1.00 calc . . . H(27) H 0.2691 0.4028 0.2333 0.1066 Uiso 1.00 calc . . . H(28) H 0.4031 0.4230 0.1760 0.1543 Uiso 1.00 calc . . . H(29) H 0.3962 0.4971 0.2130 0.1543 Uiso 1.00 calc . . . H(30) H 0.3303 0.4968 0.1498 0.1543 Uiso 1.00 calc . . . H(31) H 0.2079 0.5353 0.2321 0.1267 Uiso 1.00 calc . . . H(32) H 0.1013 0.4771 0.2205 0.1267 Uiso 1.00 calc . . . H(33) H 0.1330 0.5231 0.1710 0.1267 Uiso 1.00 calc . . . H(34) H 0.5501 0.0895 0.1973 0.0621 Uiso 1.00 calc . . . H(35) H 0.2897 0.0115 0.0883 0.0626 Uiso 1.00 calc . . . H(36) H 0.5226 0.0362 0.0817 0.0734 Uiso 1.00 calc . . . H(37) H 0.4212 0.0908 0.0496 0.0734 Uiso 1.00 calc . . . H(38) H 0.4215 0.0010 0.0347 0.0734 Uiso 1.00 calc . . . H(39) H 0.3759 -0.0667 0.1659 0.0817 Uiso 1.00 calc . . . H(40) H 0.4998 -0.0480 0.1559 0.0817 Uiso 1.00 calc . . . H(41) H 0.4098 -0.0975 0.1120 0.0817 Uiso 1.00 calc . . . H(42) H 0.4521 0.2493 0.2837 0.0794 Uiso 1.00 calc . . . H(43) H 0.6161 0.3154 0.2765 0.1128 Uiso 1.00 calc . . . H(44) H 0.5307 0.3137 0.2171 0.1128 Uiso 1.00 calc . . . H(45) H 0.6381 0.2562 0.2313 0.1128 Uiso 1.00 calc . . . H(46) H 0.5399 0.1331 0.3232 0.1317 Uiso 1.00 calc . . . H(47) H 0.6279 0.2036 0.3385 0.1317 Uiso 1.00 calc . . . H(48) H 0.6397 0.1439 0.2916 0.1317 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0417(6) 0.0396(5) 0.0347(5) -0.0034(5) 0.0081(4) -0.0050(5) Cr(2) 0.0679(8) 0.0628(8) 0.0464(7) -0.0008(6) -0.0049(6) -0.0134(6) Cr(3) 0.0597(8) 0.0418(6) 0.0564(7) -0.0025(5) 0.0083(6) -0.0014(6) O(1) 0.058(3) 0.057(3) 0.038(2) -0.002(2) 0.014(2) -0.008(2) O(2) 0.048(3) 0.051(3) 0.055(3) -0.004(2) 0.012(2) -0.004(2) O(3) 0.044(3) 0.046(2) 0.047(3) 0.002(2) 0.007(2) -0.007(2) O(4) 0.113(5) 0.067(4) 0.055(3) -0.039(3) 0.005(3) -0.016(3) O(5) 0.060(4) 0.139(6) 0.138(6) 0.029(4) -0.039(4) -0.040(5) O(6) 0.250(9) 0.047(3) 0.044(3) -0.009(4) 0.033(5) -0.011(3) O(7) 0.086(5) 0.070(4) 0.34(1) -0.026(4) 0.092(7) -0.003(6) O(8) 0.150(6) 0.072(4) 0.053(4) 0.016(4) -0.014(4) 0.008(3) N(11) 0.045(3) 0.042(3) 0.035(3) -0.006(2) 0.004(2) -0.009(2) N(12) 0.048(3) 0.040(3) 0.034(3) 0.000(2) 0.010(2) -0.005(2) N(21) 0.060(3) 0.041(3) 0.031(3) -0.006(3) 0.004(3) -0.002(2) N(22) 0.057(3) 0.036(3) 0.033(3) -0.006(3) 0.008(2) -0.004(2) N(31) 0.041(3) 0.038(3) 0.035(3) -0.002(2) 0.002(2) -0.004(2) N(32) 0.040(3) 0.051(3) 0.031(3) -0.007(2) 0.005(2) -0.008(2) C(11) 0.040(4) 0.048(4) 0.057(4) -0.001(3) 0.018(3) 0.002(3) C(12) 0.061(4) 0.055(4) 0.042(4) -0.004(4) 0.024(3) -0.008(3) C(13) 0.061(4) 0.043(4) 0.042(4) 0.009(3) 0.021(3) -0.002(3) C(14) 0.056(5) 0.064(5) 0.060(5) -0.007(4) 0.021(4) 0.001(4) C(15) 0.053(5) 0.116(8) 0.083(6) 0.008(5) 0.014(4) -0.019(6) C(16) 0.098(7) 0.087(7) 0.110(8) -0.051(6) 0.036(6) -0.012(6) C(17) 0.096(6) 0.049(4) 0.046(4) -0.008(4) 0.031(4) -0.010(4) C(18) 0.17(1) 0.076(6) 0.076(6) -0.025(6) 0.084(7) -0.015(5) C(19) 0.116(8) 0.073(6) 0.044(5) -0.020(5) -0.012(5) 0.003(4) C(21) 0.079(5) 0.040(4) 0.037(4) -0.005(4) 0.002(4) 0.003(3) C(22) 0.115(7) 0.042(4) 0.049(5) 0.004(4) 0.003(5) 0.007(4) C(23) 0.081(5) 0.041(4) 0.043(4) -0.004(4) 0.002(4) 0.000(3) C(24) 0.097(6) 0.065(5) 0.032(4) 0.000(5) -0.004(4) 0.004(4) C(25) 0.16(1) 0.102(7) 0.047(5) -0.024(7) 0.011(6) 0.022(5) C(26) 0.114(8) 0.103(7) 0.065(6) 0.022(6) -0.012(6) 0.000(6) C(27) 0.157(10) 0.041(4) 0.053(5) -0.016(5) -0.014(6) 0.001(4) C(28) 0.104(9) 0.090(8) 0.25(2) -0.029(7) -0.004(10) -0.077(10) C(29) 0.20(1) 0.084(7) 0.119(9) -0.038(8) 0.086(9) -0.061(7) C(31) 0.038(3) 0.046(3) 0.041(3) -0.004(3) 0.016(3) -0.008(3) C(32) 0.036(4) 0.064(4) 0.054(4) 0.000(3) 0.010(3) -0.011(4) C(33) 0.040(4) 0.056(4) 0.039(4) -0.013(3) 0.007(3) -0.007(3) C(34) 0.046(4) 0.054(4) 0.055(4) 0.001(3) 0.016(3) -0.006(4) C(35) 0.069(5) 0.094(6) 0.066(5) -0.021(5) 0.032(4) -0.028(5) C(36) 0.090(7) 0.062(5) 0.089(7) 0.017(5) 0.015(5) -0.014(5) C(37) 0.052(4) 0.081(5) 0.051(4) -0.013(4) -0.002(4) -0.026(4) C(38) 0.132(9) 0.086(7) 0.113(9) -0.043(7) 0.016(7) -0.033(7) C(39) 0.15(1) 0.129(10) 0.079(7) -0.042(8) -0.054(7) -0.007(7) B(1) 0.047(4) 0.040(4) 0.031(4) -0.004(3) 0.008(3) -0.004(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) O(1) 2.050(5) . . yes Cr(1) O(2) 1.966(4) . . yes Cr(1) O(3) 1.969(4) . 3_555 yes Cr(1) N(11) 2.039(6) . . yes Cr(1) N(21) 2.075(5) . . yes Cr(1) N(31) 2.091(5) . . yes Cr(2) O(3) 1.669(4) . . yes Cr(2) O(4) 1.595(6) . . yes Cr(2) O(5) 1.598(7) . . yes Cr(2) O(6) 1.755(7) . . yes Cr(3) O(2) 1.670(4) . . yes Cr(3) O(6) 1.758(6) . . yes Cr(3) O(7) 1.590(8) . . yes Cr(3) O(8) 1.552(6) . . yes N(11) N(12) 1.378(7) . . yes N(11) C(11) 1.368(9) . . yes N(12) C(13) 1.374(10) . . yes N(12) B(1) 1.563(10) . . yes N(21) N(22) 1.393(7) . . yes N(21) C(21) 1.347(8) . . yes N(22) C(23) 1.358(8) . . yes N(22) B(1) 1.559(8) . . yes N(31) N(32) 1.393(7) . . yes N(31) C(31) 1.347(8) . . yes N(32) C(33) 1.375(8) . . yes N(32) B(1) 1.528(9) . . yes C(11) C(12) 1.39(1) . . yes C(11) C(14) 1.519(9) . . yes C(12) C(13) 1.373(10) . . yes C(13) C(17) 1.506(9) . . yes C(14) C(15) 1.57(1) . . yes C(14) C(16) 1.53(1) . . yes C(17) C(18) 1.52(1) . . yes C(17) C(19) 1.55(1) . . yes C(21) C(22) 1.408(10) . . yes C(21) C(24) 1.512(9) . . yes C(22) C(23) 1.39(1) . . yes C(23) C(27) 1.50(1) . . yes C(24) C(25) 1.52(1) . . yes C(24) C(26) 1.55(1) . . yes C(27) C(28) 1.54(2) . . yes C(27) C(29) 1.52(2) . . yes C(31) C(32) 1.400(8) . . yes C(31) C(34) 1.514(9) . . yes C(32) C(33) 1.38(1) . . yes C(33) C(37) 1.493(10) . . yes C(34) C(35) 1.53(1) . . yes C(34) C(36) 1.53(1) . . yes C(37) C(38) 1.50(1) . . yes C(37) C(39) 1.51(1) . . yes C(40) C(41) 1.42(4) . . yes C(41) C(42) 1.23(3) . . yes C(42) C(43) 1.27(3) . . yes C(43) C(44) 1.30(4) . . yes C(45) C(46) 1.45(2) . . yes C(46) C(47) 1.37(3) . . yes C(47) C(48) 1.26(4) . . yes C(48) C(49) 1.04(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cr(1) O(2) 90.6(2) . . . yes O(1) Cr(1) O(3) 88.3(2) . . 3_555 yes O(1) Cr(1) N(11) 175.8(2) . . . yes O(1) Cr(1) N(21) 89.6(2) . . . yes O(1) Cr(1) N(31) 88.6(2) . . . yes O(2) Cr(1) O(3) 90.0(2) . . 3_555 yes O(2) Cr(1) N(11) 93.1(2) . . . yes O(2) Cr(1) N(21) 179.5(2) . . . yes O(2) Cr(1) N(31) 91.6(2) . . . yes O(3) Cr(1) N(11) 93.7(2) 3_555 . . yes O(3) Cr(1) N(21) 89.6(2) 3_555 . . yes O(3) Cr(1) N(31) 176.6(2) 3_555 . . yes N(11) Cr(1) N(21) 86.8(2) . . . yes N(11) Cr(1) N(31) 89.2(2) . . . yes N(21) Cr(1) N(31) 88.8(2) . . . yes O(3) Cr(2) O(4) 111.7(2) . . . yes O(3) Cr(2) O(5) 109.9(3) . . . yes O(3) Cr(2) O(6) 109.1(3) . . . yes O(4) Cr(2) O(5) 109.7(4) . . . yes O(4) Cr(2) O(6) 108.2(3) . . . yes O(5) Cr(2) O(6) 108.1(4) . . . yes O(2) Cr(3) O(6) 111.4(3) . . . yes O(2) Cr(3) O(7) 111.6(3) . . . yes O(2) Cr(3) O(8) 112.0(3) . . . yes O(6) Cr(3) O(7) 108.3(5) . . . yes O(6) Cr(3) O(8) 106.7(3) . . . yes O(7) Cr(3) O(8) 106.7(5) . . . yes Cr(1) O(2) Cr(3) 173.2(3) . . . yes Cr(1) O(3) Cr(2) 141.7(3) 3_555 . . yes Cr(2) O(6) Cr(3) 140.2(4) . . . yes Cr(1) N(11) N(12) 118.0(4) . . . yes Cr(1) N(11) C(11) 135.0(4) . . . yes N(12) N(11) C(11) 106.9(5) . . . yes N(11) N(12) C(13) 109.3(5) . . . yes N(11) N(12) B(1) 119.7(5) . . . yes C(13) N(12) B(1) 130.9(5) . . . yes Cr(1) N(21) N(22) 117.1(4) . . . yes Cr(1) N(21) C(21) 135.8(4) . . . yes N(22) N(21) C(21) 107.0(5) . . . yes N(21) N(22) C(23) 110.3(5) . . . yes N(21) N(22) B(1) 119.6(5) . . . yes C(23) N(22) B(1) 130.1(5) . . . yes Cr(1) N(31) N(32) 117.4(4) . . . yes Cr(1) N(31) C(31) 135.0(4) . . . yes N(32) N(31) C(31) 107.5(4) . . . yes N(31) N(32) C(33) 108.9(5) . . . yes N(31) N(32) B(1) 119.2(4) . . . yes C(33) N(32) B(1) 131.9(5) . . . yes N(11) C(11) C(12) 108.6(6) . . . yes N(11) C(11) C(14) 122.9(6) . . . yes C(12) C(11) C(14) 128.3(7) . . . yes C(11) C(12) C(13) 107.8(7) . . . yes N(12) C(13) C(12) 107.3(6) . . . yes N(12) C(13) C(17) 123.0(6) . . . yes C(12) C(13) C(17) 129.7(7) . . . yes C(11) C(14) C(15) 108.2(6) . . . yes C(11) C(14) C(16) 110.9(6) . . . yes C(15) C(14) C(16) 110.4(7) . . . yes C(13) C(17) C(18) 110.8(7) . . . yes C(13) C(17) C(19) 112.4(6) . . . yes C(18) C(17) C(19) 109.2(7) . . . yes N(21) C(21) C(22) 108.5(6) . . . yes N(21) C(21) C(24) 124.6(6) . . . yes C(22) C(21) C(24) 126.8(6) . . . yes C(21) C(22) C(23) 107.6(6) . . . yes N(22) C(23) C(22) 106.5(6) . . . yes N(22) C(23) C(27) 124.3(6) . . . yes C(22) C(23) C(27) 129.2(6) . . . yes C(21) C(24) C(25) 110.6(7) . . . yes C(21) C(24) C(26) 108.6(7) . . . yes C(25) C(24) C(26) 111.7(7) . . . yes C(23) C(27) C(28) 108.8(9) . . . yes C(23) C(27) C(29) 111.8(8) . . . yes C(28) C(27) C(29) 109.2(8) . . . yes N(31) C(31) C(32) 108.9(6) . . . yes N(31) C(31) C(34) 124.2(5) . . . yes C(32) C(31) C(34) 126.8(6) . . . yes C(31) C(32) C(33) 107.4(6) . . . yes N(32) C(33) C(32) 107.3(5) . . . yes N(32) C(33) C(37) 123.3(6) . . . yes C(32) C(33) C(37) 129.3(6) . . . yes C(31) C(34) C(35) 112.8(6) . . . yes C(31) C(34) C(36) 110.1(6) . . . yes C(35) C(34) C(36) 108.5(7) . . . yes C(33) C(37) C(38) 112.8(7) . . . yes C(33) C(37) C(39) 111.0(7) . . . yes C(38) C(37) C(39) 107.8(8) . . . yes C(40) C(41) C(42) 120(2) . . . yes C(41) C(42) C(43) 118(2) . . . yes C(42) C(43) C(44) 122(2) . . . yes C(45) C(46) C(47) 113(1) . . . yes C(46) C(47) C(48) 91(2) . . . yes C(47) C(48) C(49) 121(4) . . . yes N(12) B(1) N(22) 107.2(5) . . . yes N(12) B(1) N(32) 108.9(5) . . . yes N(22) B(1) N(32) 108.6(5) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(8) C(27) 3.356(10) . 2_545 ? O(8) C(19) 3.54(1) . 2_545 ? O(8) C(17) 3.59(1) . 2_545 ? C(18) C(36) 3.59(1) . 2_555 ? O(1) O(3) 2.800(7) . 3_555 ? O(1) O(4) 2.820(7) . . ? O(1) O(2) 2.855(7) . . ? O(1) O(6) 3.398(8) . 3_555 ? O(2) O(8) 2.672(7) . . ? O(2) O(7) 2.696(9) . . ? O(2) O(3) 2.782(6) . 3_555 ? O(2) O(6) 2.832(7) . . ? O(2) O(4) 3.182(7) . 3_555 ? O(2) O(4) 3.307(8) . . ? O(3) O(5) 2.675(7) . . ? O(3) O(4) 2.701(7) . . ? O(3) O(6) 2.790(7) . . ? O(4) O(5) 2.612(9) . . ? O(4) O(6) 2.716(9) . . ? O(4) O(7) 3.13(1) . 3_555 ? O(5) O(6) 2.72(1) . . ? O(6) O(8) 2.658(8) . . ? O(6) O(7) 2.71(1) . . ? O(7) O(8) 2.521(10) . . ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(1) H(1) O(4) . . . 1.011 1.821 2.832(6) 179.852 no O(1*) H(1*) O(4*) . . . 1.011 1.821 2.832(6) 179.853 no O(4) O(1) 2.832(6) . . . 0.0388 0.0025 0.1579 179.853 no O(4) O(2) 3.307(7) . . . -0.0027 0.0211 0.1341 179.853 no O(4) O(2*) 3.181(6) . . . -0.0175 -0.0437 0.0768 179.853 no O(4) O(7*) 3.13(1) . . . 0.0204 -0.0482 0.1214 179.853 no O(7) O(4*) 3.13(1) . . . -0.0599 0.0855 -0.0853 179.853 no N(11) N(21) 2.826(7) . . . 0.1897 0.1543 0.0803 179.853 no N(11) N(22) 2.986(7) . . . 0.1992 0.1725 0.0982 179.853 no N(11) N(31) 2.900(7) . . . 0.1439 0.1703 0.1337 179.853 no N(11) N(32) 3.073(7) . . . 0.1617 0.1849 0.1415 179.853 no N(12) N(21) 3.023(7) . . . 0.2171 0.1840 0.1245 179.853 no N(12) N(31) 2.996(7) . . . 0.1739 0.1986 0.1769 179.853 no N(21) N(11) 2.826(7) . . . 0.2221 0.1333 0.1002 179.853 no N(21) N(12) 3.023(7) . . . 0.2394 0.1455 0.1245 179.853 no N(21) N(31) 2.916(6) . . . 0.2168 0.1232 0.1782 179.853 no N(21) N(32) 3.042(6) . . . 0.2362 0.1368 0.1883 179.853 no N(22) N(11) 2.986(7) . . . 0.2472 0.1654 0.1396 179.853 no N(22) N(31) 3.043(7) . . . 0.2418 0.1563 0.2144 179.853 no N(31) O(1) 2.890(6) . . . 0.1331 0.1119 0.2415 179.853 no N(31) N(12) 2.996(7) . . . 0.1527 0.1756 0.2290 179.853 no N(31) N(21) 2.916(6) . . . 0.1759 0.1372 0.2275 179.853 no N(31) N(22) 3.043(7) . . . 0.1855 0.1544 0.2485 179.853 no N(32) N(11) 3.073(7) . . . 0.1737 0.1906 0.2332 179.853 no N(32) N(21) 3.042(6) . . . 0.2100 0.1670 0.2548 179.853 no N(11*) N(21*) 2.826(7) . . . -0.1897 -0.1543 -0.0803 179.853 no N(11*) N(31*) 2.900(7) . . . -0.1439 -0.1703 -0.1337 179.853 no N(11*) N(22*) 2.986(7) . . . -0.1992 -0.1725 -0.0982 179.853 no N(11*) N(32*) 3.073(7) . . . -0.1617 -0.1849 -0.1415 179.853 no N(21*) N(11*) 2.826(7) . . . -0.2221 -0.1333 -0.1002 179.853 no N(21*) N(31*) 2.916(6) . . . -0.2168 -0.1232 -0.1782 179.853 no N(21*) N(12*) 3.023(7) . . . -0.2394 -0.1455 -0.1245 179.853 no N(21*) N(32*) 3.042(6) . . . -0.2362 -0.1368 -0.1883 179.853 no N(31*) O(1*) 2.890(6) . . . -0.1331 -0.1119 -0.2415 179.853 no N(31*) N(21*) 2.916(6) . . . -0.1759 -0.1372 -0.2275 179.853 no N(31*) N(12*) 2.996(7) . . . -0.1527 -0.1756 -0.2290 179.853 no N(31*) N(22*) 3.043(7) . . . -0.1855 -0.1544 -0.2485 179.853 no O(4*) O(2) 3.181(6) . . . 0.0175 0.0437 -0.0768 179.853 no O(4*) O(7) 3.13(1) . . . -0.0204 0.0482 -0.1214 179.853 no O(4*) O(1*) 2.832(6) . . . -0.0388 -0.0025 -0.1579 179.853 no O(4*) O(2*) 3.307(7) . . . 0.0027 -0.0211 -0.1341 179.853 no N(12*) N(21*) 3.023(7) . . . -0.2171 -0.1840 -0.1245 179.853 no N(12*) N(31*) 2.996(7) . . . -0.1739 -0.1986 -0.1769 179.853 no N(22*) N(11*) 2.986(7) . . . -0.2472 -0.1654 -0.1396 179.853 no N(22*) N(31*) 3.043(7) . . . -0.2418 -0.1563 -0.2144 179.853 no N(32*) N(11*) 3.073(7) . . . -0.1737 -0.1906 -0.2332 179.853 no N(32*) N(21*) 3.042(6) . . . -0.2100 -0.1670 -0.2548 179.853 no O(7*) O(4) 3.13(1) . . . 0.0599 -0.0855 0.0853 179.853 no O(1) H(1) O(4*) . . 3_555 1.011 1.821 2.832(6) 179.853 no O(1*) H(1*) O(4) . . 3_555 1.011 1.821 2.832(6) 179.855 no #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_compound_10 _database_code_CSD 217501 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C37 H74 B Cr N6 O3 ' _chemical_formula_moiety 'C37 H74 B Cr N6 O3 ' _chemical_formula_weight 713.84 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.1187(2) _cell_length_b 23.9459(8) _cell_length_c 13.5935(4) _cell_angle_alpha 90 _cell_angle_beta 92.537(1) _cell_angle_gamma 90 _cell_volume 4266.1(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 26914 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.970 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 31964 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8921 _reflns_number_gt 7759 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2409 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7759 _refine_ls_number_parameters 445 _refine_ls_goodness_of_fit_ref 1.885 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.23 _refine_diff_density_min -1.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.92710(2) 0.06608(1) 0.40105(3) 0.0272(2) Uani 1.00 d . . . O(1) O 0.9060(1) 0.03946(7) 0.5385(1) 0.0323(3) Uani 1.00 d . . . O(2) O 0.9347(1) -0.01109(7) 0.3589(1) 0.0344(4) Uani 1.00 d . . . O(3) O 1.0720(1) 0.06783(7) 0.4313(1) 0.0351(4) Uani 1.00 d . . . N(11) N 0.9442(1) 0.09570(8) 0.2601(1) 0.0314(4) Uani 1.00 d . . . N(12) N 0.8795(1) 0.13653(8) 0.2242(1) 0.0313(4) Uani 1.00 d . . . N(21) N 0.9115(1) 0.14970(8) 0.4442(2) 0.0319(4) Uani 1.00 d . . . N(22) N 0.8512(1) 0.18465(8) 0.3855(2) 0.0338(4) Uani 1.00 d . . . N(31) N 0.7686(1) 0.06697(7) 0.3702(2) 0.0280(4) Uani 1.00 d . . . N(32) N 0.7270(1) 0.11222(8) 0.3213(1) 0.0296(4) Uani 1.00 d . . . C(11) C 1.0072(2) 0.0826(1) 0.1885(2) 0.0376(5) Uani 1.00 d . . . C(12) C 0.9815(2) 0.1144(1) 0.1054(2) 0.0466(6) Uani 1.00 d . . . C(13) C 0.9017(2) 0.1483(1) 0.1300(2) 0.0402(5) Uani 1.00 d . . . C(14) C 1.0906(2) 0.0396(1) 0.2007(2) 0.0452(6) Uani 1.00 d . . . C(15) C 1.1946(2) 0.0660(2) 0.1847(4) 0.072(1) Uani 1.00 d . . . C(16) C 1.0720(3) -0.0097(2) 0.1304(3) 0.0656(9) Uani 1.00 d . . . C(17) C 0.8453(2) 0.1910(1) 0.0670(2) 0.0533(7) Uani 1.00 d . . . C(18) C 0.8872(4) 0.2482(2) 0.0874(6) 0.132(3) Uani 1.00 d . . . C(19) C 0.8642(7) 0.1829(4) -0.0381(4) 0.177(4) Uani 1.00 d . . . C(21) C 0.9503(2) 0.1804(1) 0.5193(2) 0.0399(5) Uani 1.00 d . . . C(22) C 0.9149(3) 0.2353(1) 0.5089(2) 0.0525(7) Uani 1.00 d . . . C(23) C 0.8529(2) 0.2364(1) 0.4243(2) 0.0449(6) Uani 1.00 d . . . C(24) C 1.0202(2) 0.1570(1) 0.6002(2) 0.0483(7) Uani 1.00 d . . . C(25) C 1.1143(3) 0.1939(2) 0.6166(3) 0.071(1) Uani 1.00 d . . . C(26) C 0.9661(3) 0.1493(2) 0.6954(3) 0.074(1) Uani 1.00 d . . . C(27) C 0.7972(3) 0.2861(1) 0.3772(3) 0.0660(9) Uani 1.00 d . . . C(28) C 0.8672(6) 0.3306(3) 0.3555(6) 0.157(3) Uani 1.00 d . . . C(29) C 0.7228(6) 0.3105(3) 0.4460(5) 0.141(3) Uani 1.00 d . . . C(31) C 0.6918(2) 0.0313(1) 0.3856(2) 0.0329(5) Uani 1.00 d . . . C(32) C 0.6010(2) 0.0536(1) 0.3462(2) 0.0406(6) Uani 1.00 d . . . C(33) C 0.6247(2) 0.1044(1) 0.3064(2) 0.0357(5) Uani 1.00 d . . . C(34) C 0.7064(2) -0.0234(1) 0.4394(2) 0.0399(6) Uani 1.00 d . . . C(35) C 0.6695(3) -0.0196(2) 0.5429(3) 0.077(1) Uani 1.00 d . . . C(36) C 0.6515(4) -0.0702(2) 0.3842(4) 0.099(2) Uani 1.00 d . . . C(37) C 0.5554(2) 0.1472(1) 0.2578(3) 0.0511(7) Uani 1.00 d . . . C(38) C 0.5214(5) 0.1890(3) 0.3326(5) 0.121(2) Uani 1.00 d . . . C(39) C 0.4624(3) 0.1202(2) 0.2085(5) 0.112(2) Uani 1.00 d . . . C(40) C 0.6292(6) 0.2826(4) 0.8188(6) 0.154(3) Uani 1.00 d . . . C(41) C 0.6708(8) 0.2519(7) 0.7385(7) 0.209(6) Uani 1.00 d . . . C(42) C 0.6344(4) 0.2103(2) 0.7020(4) 0.079(1) Uani 1.00 d . . . C(43) C 0.6797(6) 0.1838(5) 0.6333(9) 0.186(4) Uani 1.00 d . . . C(44) C 0.6522(9) 0.1384(4) 0.5907(7) 0.178(4) Uani 1.00 d . . . C(45) C 1.2434(4) 0.0018(3) -0.1191(4) 0.099(2) Uani 1.00 d . . . C(46) C 1.3093(9) -0.0326(8) -0.0738(8) 0.257(8) Uani 1.00 d . . . C(47) C 1.3350(3) -0.0323(2) 0.0224(3) 0.0616(8) Uani 1.00 d . . . C(48) C 1.394(1) -0.0682(7) 0.0770(9) 0.280(10) Uani 1.00 d . . . C(49) C 1.4172(8) -0.0609(4) 0.1714(6) 0.161(4) Uani 1.00 d . . . B(1) B 0.7974(2) 0.1604(1) 0.2921(2) 0.0312(5) Uani 1.00 d . . . H(1) H 0.9754 0.0338 0.5782 0.0674 Uiso 1.00 calc . . . H(2) H 0.8934 0.0013 0.5419 0.0450 Uiso 1.00 calc . . . H(3) H 0.8946 -0.0151 0.2848 0.0983 Uiso 1.00 calc . . . H(4) H 1.1093 0.0983 0.4135 0.0450 Uiso 1.00 calc . . . H(5) H 0.7592 0.1887 0.2582 0.0383 Uiso 1.00 calc . . . H(6) H 1.0149 0.1135 0.0446 0.0569 Uiso 1.00 calc . . . H(7) H 1.0910 0.0255 0.2671 0.0551 Uiso 1.00 calc . . . H(8) H 1.2469 0.0382 0.1933 0.0717 Uiso 1.00 calc . . . H(9) H 1.2068 0.0956 0.2315 0.0717 Uiso 1.00 calc . . . H(10) H 1.1955 0.0809 0.1191 0.0717 Uiso 1.00 calc . . . H(11) H 1.0100 -0.0283 0.1462 0.0656 Uiso 1.00 calc . . . H(12) H 1.1281 -0.0354 0.1373 0.0656 Uiso 1.00 calc . . . H(13) H 1.0662 0.0037 0.0639 0.0656 Uiso 1.00 calc . . . H(14) H 0.7738 0.1891 0.0774 0.0666 Uiso 1.00 calc . . . H(15) H 0.9590 0.2484 0.0767 0.1320 Uiso 1.00 calc . . . H(16) H 0.8762 0.2581 0.1545 0.1320 Uiso 1.00 calc . . . H(17) H 0.8533 0.2746 0.0442 0.1320 Uiso 1.00 calc . . . H(18) H 0.8429 0.1461 -0.0579 0.1766 Uiso 1.00 calc . . . H(19) H 0.9357 0.1872 -0.0482 0.1766 Uiso 1.00 calc . . . H(20) H 0.8263 0.2101 -0.0765 0.1766 Uiso 1.00 calc . . . H(21) H 0.9318 0.2664 0.5510 0.0631 Uiso 1.00 calc . . . H(22) H 1.0425 0.1208 0.5794 0.0596 Uiso 1.00 calc . . . H(23) H 1.1587 0.1779 0.6671 0.0707 Uiso 1.00 calc . . . H(24) H 1.0936 0.2306 0.6364 0.0707 Uiso 1.00 calc . . . H(25) H 1.1498 0.1966 0.5565 0.0707 Uiso 1.00 calc . . . H(26) H 0.9382 0.1844 0.7153 0.0737 Uiso 1.00 calc . . . H(27) H 1.0138 0.1360 0.7457 0.0737 Uiso 1.00 calc . . . H(28) H 0.9120 0.1226 0.6856 0.0737 Uiso 1.00 calc . . . H(29) H 0.7608 0.2738 0.3178 0.0794 Uiso 1.00 calc . . . H(30) H 0.9068 0.3403 0.4142 0.1568 Uiso 1.00 calc . . . H(31) H 0.8294 0.3627 0.3322 0.1568 Uiso 1.00 calc . . . H(32) H 0.9120 0.3184 0.3058 0.1568 Uiso 1.00 calc . . . H(33) H 0.7592 0.3253 0.5030 0.1411 Uiso 1.00 calc . . . H(34) H 0.6767 0.2820 0.4659 0.1411 Uiso 1.00 calc . . . H(35) H 0.6850 0.3399 0.4131 0.1411 Uiso 1.00 calc . . . H(36) H 0.5346 0.0367 0.3469 0.0491 Uiso 1.00 calc . . . H(37) H 0.7776 -0.0317 0.4433 0.0494 Uiso 1.00 calc . . . H(38) H 0.6952 0.0140 0.5736 0.0766 Uiso 1.00 calc . . . H(39) H 0.6937 -0.0514 0.5802 0.0766 Uiso 1.00 calc . . . H(40) H 0.5963 -0.0191 0.5408 0.0766 Uiso 1.00 calc . . . H(41) H 0.5794 -0.0631 0.3816 0.0987 Uiso 1.00 calc . . . H(42) H 0.6651 -0.1049 0.4175 0.0987 Uiso 1.00 calc . . . H(43) H 0.6751 -0.0723 0.3185 0.0987 Uiso 1.00 calc . . . H(44) H 0.5924 0.1668 0.2095 0.0616 Uiso 1.00 calc . . . H(45) H 0.5801 0.2040 0.3681 0.1205 Uiso 1.00 calc . . . H(46) H 0.4779 0.1709 0.3777 0.1205 Uiso 1.00 calc . . . H(47) H 0.4847 0.2188 0.2995 0.1205 Uiso 1.00 calc . . . H(48) H 0.4185 0.1485 0.1801 0.1115 Uiso 1.00 calc . . . H(49) H 0.4263 0.0995 0.2564 0.1115 Uiso 1.00 calc . . . H(50) H 0.4833 0.0954 0.1577 0.1115 Uiso 1.00 calc . . . H(51) H 0.6664 0.3177 0.8337 0.1835 Uiso 1.00 calc . . . H(52) H 0.5600 0.2921 0.8074 0.1835 Uiso 1.00 calc . . . H(53) H 0.6372 0.2600 0.8764 0.1835 Uiso 1.00 calc . . . H(54) H 0.6640 0.2825 0.6837 0.2357 Uiso 1.00 calc . . . H(55) H 0.7412 0.2505 0.7527 0.2357 Uiso 1.00 calc . . . H(56) H 0.6325 0.1849 0.7588 0.0945 Uiso 1.00 calc . . . H(57) H 0.5664 0.2166 0.6795 0.0945 Uiso 1.00 calc . . . H(58) H 0.6883 0.2121 0.5875 0.2369 Uiso 1.00 calc . . . H(59) H 0.7450 0.1752 0.6662 0.2369 Uiso 1.00 calc . . . H(60) H 0.5848 0.1453 0.5541 0.1950 Uiso 1.00 calc . . . H(61) H 0.6975 0.1281 0.5415 0.1950 Uiso 1.00 calc . . . H(62) H 0.6410 0.1084 0.6332 0.1950 Uiso 1.00 calc . . . H(63) H 1.2608 0.0413 -0.1068 0.1207 Uiso 1.00 calc . . . H(64) H 1.2407 -0.0036 -0.1877 0.1207 Uiso 1.00 calc . . . H(65) H 1.1769 -0.0035 -0.0943 0.1207 Uiso 1.00 calc . . . H(66) H 1.2931 -0.0686 -0.0877 0.3238 Uiso 1.00 calc . . . H(67) H 1.3770 -0.0239 -0.1005 0.3238 Uiso 1.00 calc . . . H(68) H 1.3584 0.0048 0.0377 0.0747 Uiso 1.00 calc . . . H(69) H 1.2694 -0.0367 0.0513 0.0747 Uiso 1.00 calc . . . H(70) H 1.3742 -0.1037 0.0667 0.3376 Uiso 1.00 calc . . . H(71) H 1.4642 -0.0633 0.0495 0.3376 Uiso 1.00 calc . . . H(72) H 1.4617 -0.0890 0.1976 0.1818 Uiso 1.00 calc . . . H(73) H 1.4423 -0.0253 0.1882 0.1818 Uiso 1.00 calc . . . H(74) H 1.3521 -0.0655 0.2053 0.1818 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0264(2) 0.0247(2) 0.0301(3) -0.0002(1) -0.0031(2) 0.0057(1) O(1) 0.0340(8) 0.0325(9) 0.0300(9) -0.0003(6) -0.0027(6) 0.0066(7) O(2) 0.0343(8) 0.0280(8) 0.0405(10) 0.0019(6) -0.0030(6) 0.0016(7) O(3) 0.0302(8) 0.0322(9) 0.042(1) -0.0031(5) -0.0042(7) 0.0090(7) N(11) 0.0286(9) 0.032(1) 0.033(1) 0.0020(7) 0.0002(7) 0.0059(8) N(12) 0.0307(9) 0.0313(10) 0.032(1) 0.0014(7) -0.0010(7) 0.0093(8) N(21) 0.0356(10) 0.0275(10) 0.032(1) -0.0005(7) -0.0049(7) 0.0050(8) N(22) 0.038(1) 0.0249(9) 0.038(1) 0.0012(7) -0.0027(8) 0.0054(8) N(31) 0.0297(10) 0.0249(10) 0.029(1) 0.0008(6) -0.0017(7) 0.0056(7) N(32) 0.0257(9) 0.0292(9) 0.034(1) 0.0022(6) -0.0024(6) 0.0058(8) C(11) 0.033(1) 0.044(1) 0.036(1) 0.0012(9) 0.0050(9) 0.005(1) C(12) 0.043(1) 0.059(2) 0.038(1) 0.004(1) 0.0101(10) 0.013(1) C(13) 0.039(1) 0.045(1) 0.036(1) -0.0011(10) 0.0029(9) 0.013(1) C(14) 0.039(1) 0.054(2) 0.043(1) 0.012(1) 0.0087(10) 0.007(1) C(15) 0.037(2) 0.084(3) 0.095(3) 0.008(1) 0.009(2) 0.006(2) C(16) 0.065(2) 0.066(2) 0.067(2) 0.018(2) 0.004(1) -0.010(2) C(17) 0.052(2) 0.061(2) 0.047(2) 0.009(1) 0.001(1) 0.025(1) C(18) 0.103(4) 0.085(4) 0.206(8) -0.001(3) -0.017(4) 0.085(4) C(19) 0.215(8) 0.245(9) 0.072(4) 0.146(7) 0.035(4) 0.072(5) C(21) 0.051(1) 0.030(1) 0.038(1) -0.0059(9) -0.007(1) -0.0017(10) C(22) 0.074(2) 0.031(1) 0.051(2) 0.000(1) -0.013(1) -0.005(1) C(23) 0.058(2) 0.027(1) 0.050(2) 0.003(1) -0.007(1) 0.000(1) C(24) 0.062(2) 0.040(1) 0.041(2) -0.003(1) -0.017(1) -0.002(1) C(25) 0.074(2) 0.060(2) 0.074(2) -0.013(2) -0.029(2) -0.011(2) C(26) 0.099(3) 0.074(3) 0.047(2) 0.004(2) -0.006(2) 0.002(2) C(27) 0.095(2) 0.029(1) 0.071(2) 0.015(1) -0.022(2) 0.001(1) C(28) 0.166(6) 0.079(4) 0.223(9) -0.001(4) -0.024(6) 0.088(5) C(29) 0.171(6) 0.110(5) 0.143(6) 0.095(4) 0.017(5) 0.019(4) C(31) 0.030(1) 0.033(1) 0.036(1) -0.0029(8) 0.0006(8) 0.0046(10) C(32) 0.028(1) 0.045(1) 0.049(2) -0.0036(9) 0.0017(9) 0.012(1) C(33) 0.028(1) 0.038(1) 0.041(1) 0.0010(8) -0.0010(8) 0.007(1) C(34) 0.034(1) 0.034(1) 0.051(2) -0.0058(9) -0.0026(9) 0.015(1) C(35) 0.081(2) 0.085(3) 0.066(2) 0.020(2) 0.028(2) 0.041(2) C(36) 0.128(4) 0.042(2) 0.119(4) -0.027(2) -0.066(3) 0.022(2) C(37) 0.031(1) 0.051(2) 0.071(2) 0.008(1) -0.001(1) 0.025(1) C(38) 0.140(4) 0.105(4) 0.117(4) 0.085(4) 0.012(3) 0.015(3) C(39) 0.069(2) 0.105(4) 0.156(5) 0.005(2) -0.052(3) 0.052(4) C(40) 0.153(6) 0.161(7) 0.149(7) 0.069(5) 0.000(5) -0.037(6) C(41) 0.151(8) 0.36(2) 0.121(7) 0.073(10) 0.046(6) 0.047(9) C(42) 0.085(3) 0.069(3) 0.085(3) -0.002(2) 0.015(2) -0.025(2) C(43) 0.121(6) 0.203(10) 0.24(1) -0.025(6) 0.057(7) -0.051(9) C(44) 0.29(1) 0.125(6) 0.126(6) -0.019(7) 0.077(7) -0.053(5) C(45) 0.118(4) 0.119(4) 0.059(3) -0.003(3) -0.001(2) 0.001(3) C(46) 0.182(9) 0.45(2) 0.139(8) 0.13(1) -0.052(7) -0.07(1) C(47) 0.060(2) 0.070(2) 0.055(2) 0.007(1) -0.001(1) -0.010(2) C(48) 0.24(1) 0.43(2) 0.165(10) 0.19(1) -0.095(9) -0.09(1) C(49) 0.190(8) 0.174(8) 0.115(6) 0.077(6) -0.032(6) 0.004(5) B(1) 0.032(1) 0.028(1) 0.033(1) 0.0025(9) -0.0014(9) 0.0078(10) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) O(1) 2.005(2) . . yes Cr(1) O(2) 1.939(2) . . yes Cr(1) O(3) 1.927(2) . . yes Cr(1) N(11) 2.065(2) . . yes Cr(1) N(21) 2.099(2) . . yes Cr(1) N(31) 2.103(2) . . yes O(1) O(2) 2.553(2) . 3_756 yes O(1) O(3) 2.616(2) . 3_756 yes N(11) N(12) 1.370(3) . . yes N(11) C(11) 1.342(3) . . yes N(12) C(13) 1.356(3) . . yes N(12) B(1) 1.558(3) . . yes N(21) N(22) 1.382(3) . . yes N(21) C(21) 1.340(3) . . yes N(22) C(23) 1.347(3) . . yes N(22) B(1) 1.538(3) . . yes N(31) N(32) 1.371(3) . . yes N(31) C(31) 1.345(3) . . yes N(32) C(33) 1.361(3) . . yes N(32) B(1) 1.541(3) . . yes C(11) C(12) 1.392(4) . . yes C(11) C(14) 1.506(4) . . yes C(12) C(13) 1.378(4) . . yes C(13) C(17) 1.507(4) . . yes C(14) C(15) 1.528(4) . . yes C(14) C(16) 1.531(5) . . yes C(17) C(18) 1.497(7) . . yes C(17) C(19) 1.473(7) . . yes C(21) C(22) 1.401(4) . . yes C(21) C(24) 1.508(4) . . yes C(22) C(23) 1.379(4) . . yes C(23) C(27) 1.522(4) . . yes C(24) C(25) 1.528(5) . . yes C(24) C(26) 1.514(5) . . yes C(27) C(28) 1.446(8) . . yes C(27) C(29) 1.500(8) . . yes C(31) C(32) 1.392(3) . . yes C(31) C(34) 1.506(4) . . yes C(32) C(33) 1.372(4) . . yes C(33) C(37) 1.504(4) . . yes C(34) C(35) 1.511(5) . . yes C(34) C(36) 1.514(5) . . yes C(37) C(38) 1.508(7) . . yes C(37) C(39) 1.511(6) . . yes C(40) C(41) 1.44(1) . . yes C(41) C(42) 1.20(2) . . yes C(42) C(43) 1.29(1) . . yes C(43) C(44) 1.28(2) . . yes C(45) C(46) 1.33(2) . . yes C(46) C(47) 1.34(1) . . yes C(47) C(48) 1.36(1) . . yes C(48) C(49) 1.32(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cr(1) O(2) 89.07(7) . . . yes O(1) Cr(1) O(3) 89.05(7) . . . yes O(1) Cr(1) N(11) 177.74(7) . . . yes O(1) Cr(1) N(21) 91.34(7) . . . yes O(1) Cr(1) N(31) 90.75(7) . . . yes O(2) Cr(1) O(3) 91.19(7) . . . yes O(2) Cr(1) N(11) 92.51(8) . . . yes O(2) Cr(1) N(21) 177.25(7) . . . yes O(2) Cr(1) N(31) 90.80(6) . . . yes O(3) Cr(1) N(11) 92.54(7) . . . yes O(3) Cr(1) N(21) 91.53(7) . . . yes O(3) Cr(1) N(31) 178.00(7) . . . yes N(11) Cr(1) N(21) 87.01(8) . . . yes N(11) Cr(1) N(31) 87.61(7) . . . yes N(21) Cr(1) N(31) 86.48(7) . . . yes Cr(1) O(1) O(2) 116.78(8) . . 3_756 yes Cr(1) O(1) O(3) 116.07(8) . . 3_756 yes O(2) O(1) O(3) 64.59(6) 3_756 . 3_756 yes Cr(1) O(2) O(1) 98.25(7) . . 3_756 yes Cr(1) O(3) O(1) 96.49(7) . . 3_756 yes Cr(1) N(11) N(12) 119.0(1) . . . yes Cr(1) N(11) C(11) 133.5(2) . . . yes N(12) N(11) C(11) 107.5(2) . . . yes N(11) N(12) C(13) 109.2(2) . . . yes N(11) N(12) B(1) 119.0(2) . . . yes C(13) N(12) B(1) 131.8(2) . . . yes Cr(1) N(21) N(22) 118.5(1) . . . yes Cr(1) N(21) C(21) 134.3(2) . . . yes N(22) N(21) C(21) 107.3(2) . . . yes N(21) N(22) C(23) 109.4(2) . . . yes N(21) N(22) B(1) 118.6(2) . . . yes C(23) N(22) B(1) 132.0(2) . . . yes Cr(1) N(31) N(32) 118.2(1) . . . yes Cr(1) N(31) C(31) 134.7(1) . . . yes N(32) N(31) C(31) 107.0(2) . . . yes N(31) N(32) C(33) 109.4(2) . . . yes N(31) N(32) B(1) 119.1(2) . . . yes C(33) N(32) B(1) 131.5(2) . . . yes N(11) C(11) C(12) 109.0(2) . . . yes N(11) C(11) C(14) 123.3(2) . . . yes C(12) C(11) C(14) 127.7(2) . . . yes C(11) C(12) C(13) 106.6(2) . . . yes N(12) C(13) C(12) 107.7(2) . . . yes N(12) C(13) C(17) 123.9(2) . . . yes C(12) C(13) C(17) 128.5(3) . . . yes C(11) C(14) C(15) 110.6(3) . . . yes C(11) C(14) C(16) 111.3(2) . . . yes C(15) C(14) C(16) 110.4(3) . . . yes C(13) C(17) C(18) 110.3(3) . . . yes C(13) C(17) C(19) 111.2(4) . . . yes C(18) C(17) C(19) 102.9(5) . . . yes N(21) C(21) C(22) 109.0(2) . . . yes N(21) C(21) C(24) 123.3(2) . . . yes C(22) C(21) C(24) 127.7(2) . . . yes C(21) C(22) C(23) 106.4(3) . . . yes N(22) C(23) C(22) 108.0(2) . . . yes N(22) C(23) C(27) 123.7(3) . . . yes C(22) C(23) C(27) 128.3(3) . . . yes C(21) C(24) C(25) 110.6(3) . . . yes C(21) C(24) C(26) 112.1(3) . . . yes C(25) C(24) C(26) 110.6(3) . . . yes C(23) C(27) C(28) 111.4(4) . . . yes C(23) C(27) C(29) 110.9(4) . . . yes C(28) C(27) C(29) 106.0(5) . . . yes N(31) C(31) C(32) 109.2(2) . . . yes N(31) C(31) C(34) 123.2(2) . . . yes C(32) C(31) C(34) 127.6(2) . . . yes C(31) C(32) C(33) 106.7(2) . . . yes N(32) C(33) C(32) 107.6(2) . . . yes N(32) C(33) C(37) 123.0(2) . . . yes C(32) C(33) C(37) 129.3(2) . . . yes C(31) C(34) C(35) 111.2(3) . . . yes C(31) C(34) C(36) 110.8(3) . . . yes C(35) C(34) C(36) 109.9(3) . . . yes C(33) C(37) C(38) 110.3(3) . . . yes C(33) C(37) C(39) 111.3(3) . . . yes C(38) C(37) C(39) 109.1(4) . . . yes C(40) C(41) C(42) 125.2(9) . . . yes C(41) C(42) C(43) 121.2(8) . . . yes C(42) C(43) C(44) 128.0(9) . . . yes C(45) C(46) C(47) 125(1) . . . yes C(46) C(47) C(48) 130.1(10) . . . yes C(47) C(48) C(49) 123(1) . . . yes N(12) B(1) N(22) 108.9(2) . . . yes N(12) B(1) N(32) 108.4(2) . . . yes N(22) B(1) N(32) 109.2(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 2.553(2) . 3_756 ? O(1) O(3) 2.616(2) . 3_756 ? O(1) O(2) 2.553(2) . 3_756 ? O(1) O(3) 2.616(2) . 3_756 ? O(1) O(3) 2.758(2) . . ? O(1) O(2) 2.767(2) . . ? O(1) O(1) 3.313(3) . 3_756 ? O(2) O(3) 2.762(2) . . ? O(2) O(3) 3.164(3) . 3_756 ? #------------------------------------------------------------------------------ #===END data_sug46 _database_code_CSD 217502 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C63 H112 B2 Cr2 N14 O4 ' _chemical_formula_moiety 'C63 H112 B2 Cr2 N14 O4 ' _chemical_formula_weight 1255.28 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.6053(9) _cell_length_b 16.611(1) _cell_length_c 14.3911(9) _cell_angle_alpha 99.328(2) _cell_angle_beta 97.619(3) _cell_angle_gamma 84.569(5) _cell_volume 3638.4(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9147 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.966 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27165 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 14755 _reflns_number_gt 9078 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1883 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9078 _refine_ls_number_parameters 801 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.52 _refine_diff_density_min -0.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr(1) Cr 0.70544(3) 0.32677(3) 0.22949(4) 0.0257(1) Uani 1.00 d . . . Cr(2) Cr 0.79626(3) 0.18217(3) 0.19733(4) 0.0269(1) Uani 1.00 d . . . O(1) O 0.8197(1) 0.2954(1) 0.1940(2) 0.0314(5) Uani 1.00 d . . . O(2) O 0.6799(1) 0.2266(1) 0.1381(2) 0.0307(5) Uani 1.00 d . . . O(3) O 0.7455(1) 0.2432(2) 0.3113(2) 0.0294(5) Uani 1.00 d . . . O(4) O 0.7575(2) 0.0788(2) 0.2139(2) 0.0378(6) Uani 1.00 d . . . N(11) N 0.5777(2) 0.3503(2) 0.2558(2) 0.0300(6) Uani 1.00 d . . . N(12) N 0.5452(2) 0.4315(2) 0.2682(2) 0.0308(7) Uani 1.00 d . . . N(21) N 0.7341(2) 0.4247(2) 0.3347(2) 0.0304(6) Uani 1.00 d . . . N(22) N 0.6850(2) 0.4974(2) 0.3291(2) 0.0312(6) Uani 1.00 d . . . N(31) N 0.6779(2) 0.4074(2) 0.1300(2) 0.0285(6) Uani 1.00 d . . . N(32) N 0.6314(2) 0.4805(2) 0.1557(2) 0.0279(6) Uani 1.00 d . . . N(41) N 0.9671(2) 0.3374(2) 0.1503(3) 0.0447(9) Uani 1.00 d . . . N(42) N 1.0118(2) 0.2726(2) 0.0999(2) 0.0355(7) Uani 1.00 d . . . N(51) N 0.9228(2) 0.1549(2) 0.2516(2) 0.0317(7) Uani 1.00 d . . . N(52) N 0.9923(2) 0.1692(2) 0.2074(2) 0.0324(7) Uani 1.00 d . . . N(61) N 0.8328(2) 0.1344(2) 0.0675(2) 0.0297(6) Uani 1.00 d . . . N(62) N 0.9088(2) 0.1527(2) 0.0366(2) 0.0283(6) Uani 1.00 d . . . N(71) N 0.6785(2) 0.1347(3) 0.4259(3) 0.0554(10) Uani 1.00 d . . . N(72) N 0.6744(2) 0.0668(2) 0.3589(3) 0.0494(9) Uani 1.00 d . . . C(11) C 0.5116(2) 0.3045(2) 0.2581(3) 0.0331(8) Uani 1.00 d . . . C(12) C 0.4365(2) 0.3552(3) 0.2716(3) 0.0414(9) Uani 1.00 d . . . C(13) C 0.4591(2) 0.4342(2) 0.2771(3) 0.0364(9) Uani 1.00 d . . . C(14) C 0.5199(2) 0.2122(3) 0.2467(3) 0.0402(9) Uani 1.00 d . . . C(15) C 0.4780(3) 0.1814(3) 0.3224(4) 0.059(1) Uani 1.00 d . . . C(16) C 0.4811(3) 0.1761(3) 0.1484(4) 0.059(1) Uani 1.00 d . . . C(17) C 0.4036(3) 0.5135(3) 0.2950(3) 0.044(1) Uani 1.00 d . . . C(18) C 0.4219(3) 0.5536(3) 0.3977(4) 0.071(2) Uani 1.00 d . . . C(19) C 0.3076(3) 0.4997(3) 0.2700(4) 0.058(1) Uani 1.00 d . . . C(21) C 0.7973(2) 0.4388(2) 0.4063(3) 0.0372(9) Uani 1.00 d . . . C(22) C 0.7905(3) 0.5206(3) 0.4456(3) 0.051(1) Uani 1.00 d . . . C(23) C 0.7191(3) 0.5568(3) 0.3956(3) 0.0427(9) Uani 1.00 d . . . C(24) C 0.8626(3) 0.3739(3) 0.4416(3) 0.0441(10) Uani 1.00 d . . . C(25) C 0.8637(5) 0.3801(4) 0.5479(4) 0.101(2) Uani 1.00 d . . . C(26) C 0.9531(3) 0.3808(4) 0.4180(5) 0.086(2) Uani 1.00 d . . . C(27) C 0.6843(3) 0.6444(3) 0.4112(3) 0.051(1) Uani 1.00 d . . . C(28) C 0.6494(3) 0.6665(3) 0.5076(4) 0.068(1) Uani 1.00 d . . . C(29) C 0.7549(4) 0.6996(3) 0.4056(4) 0.077(2) Uani 1.00 d . . . C(31) C 0.6953(2) 0.4069(2) 0.0406(3) 0.0361(9) Uani 1.00 d . . . C(32) C 0.6598(3) 0.4800(3) 0.0097(3) 0.0390(9) Uani 1.00 d . . . C(33) C 0.6194(2) 0.5248(2) 0.0834(3) 0.0305(8) Uani 1.00 d . . . C(34) C 0.7429(3) 0.3369(3) -0.0158(3) 0.047(1) Uani 1.00 d . . . C(35) C 0.6800(3) 0.2957(3) -0.0971(3) 0.063(1) Uani 1.00 d . . . C(36) C 0.8194(3) 0.3656(3) -0.0545(4) 0.067(1) Uani 1.00 d . . . C(37) C 0.5713(2) 0.6079(2) 0.0880(3) 0.0352(8) Uani 1.00 d . . . C(38) C 0.5421(3) 0.6295(3) -0.0110(3) 0.048(1) Uani 1.00 d . . . C(39) C 0.6256(3) 0.6744(3) 0.1457(3) 0.056(1) Uani 1.00 d . . . C(41) C 1.0050(3) 0.4048(3) 0.1445(4) 0.059(1) Uani 1.00 d . . . C(42) C 1.0732(3) 0.3858(3) 0.0899(4) 0.058(1) Uani 1.00 d . . . C(43) C 1.0770(2) 0.3025(3) 0.0624(3) 0.0405(9) Uani 1.00 d . . . C(44) C 0.9751(4) 0.4881(3) 0.1974(6) 0.103(3) Uani 1.00 d . . . C(45) C 1.0284(4) 0.5511(4) 0.1989(5) 0.090(2) Uani 1.00 d . . . C(46) C 0.8798(3) 0.5048(3) 0.1912(4) 0.064(1) Uani 1.00 d . . . C(47) C 1.1432(3) 0.2529(3) 0.0046(3) 0.045(1) Uani 1.00 d . . . C(48) C 1.2357(3) 0.2658(3) 0.0520(4) 0.061(1) Uani 1.00 d . . . C(49) C 1.1332(3) 0.2761(3) -0.0954(4) 0.064(1) Uani 1.00 d . . . C(51) C 0.9543(2) 0.1354(3) 0.3367(3) 0.0382(9) Uani 1.00 d . . . C(52) C 1.0436(3) 0.1364(3) 0.3487(3) 0.050(1) Uani 1.00 d . . . C(53) C 1.0664(2) 0.1578(3) 0.2679(3) 0.044(1) Uani 1.00 d . . . C(54) C 0.8993(3) 0.1123(3) 0.4042(3) 0.048(1) Uani 1.00 d . . . C(55) C 0.9283(4) 0.1501(3) 0.5059(3) 0.071(2) Uani 1.00 d . . . C(56) C 0.9014(3) 0.0197(3) 0.3980(4) 0.061(1) Uani 1.00 d . . . C(57) C 1.1545(3) 0.1751(4) 0.2492(3) 0.059(1) Uani 1.00 d . . . C(58) C 1.1714(3) 0.2648(4) 0.2899(4) 0.076(2) Uani 1.00 d . . . C(59) C 1.2250(3) 0.1176(4) 0.2922(4) 0.079(2) Uani 1.00 d . . . C(61) C 0.7859(2) 0.0934(2) -0.0071(3) 0.0349(8) Uani 1.00 d . . . C(62) C 0.8297(2) 0.0862(3) -0.0868(3) 0.0399(9) Uani 1.00 d . . . C(63) C 0.9059(2) 0.1222(2) -0.0571(3) 0.0347(8) Uani 1.00 d . . . C(64) C 0.7023(2) 0.0568(3) -0.0018(3) 0.0411(9) Uani 1.00 d . . . C(65) C 0.6313(3) 0.0769(3) -0.0797(4) 0.060(1) Uani 1.00 d . . . C(66) C 0.7171(3) -0.0359(3) -0.0065(4) 0.056(1) Uani 1.00 d . . . C(67) C 0.9777(2) 0.1278(3) -0.1157(3) 0.0394(9) Uani 1.00 d . . . C(68) C 0.9423(3) 0.1433(3) -0.2155(3) 0.061(1) Uani 1.00 d . . . C(69) C 1.0382(3) 0.0490(3) -0.1202(4) 0.057(1) Uani 1.00 d . . . C(71) C 0.6482(3) 0.1159(5) 0.5005(4) 0.079(2) Uani 1.00 d . . . C(72) C 0.6244(4) 0.0355(5) 0.4808(5) 0.093(2) Uani 1.00 d . . . C(73) C 0.6431(3) 0.0041(4) 0.3891(4) 0.065(1) Uani 1.00 d . . . C(74) C 0.6449(5) 0.1792(7) 0.5893(5) 0.141(4) Uani 1.00 d . . . C(75) C 0.5590(7) 0.2030(8) 0.6176(8) 0.182(5) Uani 1.00 d . . . C(76) C 0.7132(8) 0.2256(9) 0.625(1) 0.134(6) Uani 0.60 d P . . C(76A) C 0.689(1) 0.125(1) 0.6707(9) 0.125(8) Uani 0.40 d P . . C(77) C 0.6321(4) -0.0772(4) 0.3245(5) 0.083(2) Uani 1.00 d . . . C(78) C 0.5639(6) -0.0677(5) 0.2415(7) 0.149(4) Uani 1.00 d . . . C(79) C 0.7157(5) -0.1138(4) 0.2834(6) 0.113(3) Uani 1.00 d . . . B(1) B 0.6029(3) 0.4986(2) 0.2561(3) 0.0305(9) Uani 1.00 d . . . B(2) B 0.9922(3) 0.1838(3) 0.1024(3) 0.0327(9) Uani 1.00 d . . . H(01) H 0.8868 0.3204 0.1795 0.0399 Uiso 1.00 calc . . . H(02) H 0.6745 0.2290 0.0576 0.0399 Uiso 1.00 calc . . . H(03) H 0.7179 0.2177 0.3442 0.0399 Uiso 1.00 calc . . . H(04) H 0.6952 0.0707 0.3006 0.0561 Uiso 1.00 calc . . . H(4) H 0.3796 0.3387 0.2761 0.0491 Uiso 1.00 calc . . . H(5) H 0.5806 0.1943 0.2534 0.0494 Uiso 1.00 calc . . . H(05) H 0.7977 0.0425 0.1964 0.0399 Uiso 1.00 calc . . . H(6) H 0.5055 0.2029 0.3840 0.0595 Uiso 1.00 calc . . . H(7) H 0.4847 0.1227 0.3138 0.0595 Uiso 1.00 calc . . . H(8) H 0.4175 0.1992 0.3173 0.0595 Uiso 1.00 calc . . . H(9) H 0.4205 0.1933 0.1396 0.0594 Uiso 1.00 calc . . . H(10) H 0.4882 0.1175 0.1416 0.0594 Uiso 1.00 calc . . . H(11) H 0.5100 0.1946 0.1018 0.0594 Uiso 1.00 calc . . . H(12) H 0.4194 0.5504 0.2552 0.0527 Uiso 1.00 calc . . . H(13) H 0.4009 0.5214 0.4383 0.0707 Uiso 1.00 calc . . . H(14) H 0.3931 0.6075 0.4054 0.0707 Uiso 1.00 calc . . . H(15) H 0.4833 0.5572 0.4140 0.0707 Uiso 1.00 calc . . . H(16) H 0.2743 0.5515 0.2756 0.0583 Uiso 1.00 calc . . . H(17) H 0.2905 0.4670 0.3127 0.0583 Uiso 1.00 calc . . . H(18) H 0.2976 0.4719 0.2061 0.0583 Uiso 1.00 calc . . . H(19) H 0.5713 0.5511 0.2644 0.0362 Uiso 1.00 calc . . . H(20) H 0.8291 0.5474 0.4973 0.0601 Uiso 1.00 calc . . . H(21) H 0.8440 0.3205 0.4128 0.0550 Uiso 1.00 calc . . . H(22) H 0.9114 0.3457 0.5725 0.1009 Uiso 1.00 calc . . . H(23) H 0.8103 0.3629 0.5615 0.1009 Uiso 1.00 calc . . . H(24) H 0.8700 0.4358 0.5771 0.1009 Uiso 1.00 calc . . . H(25) H 0.9904 0.3350 0.4356 0.0859 Uiso 1.00 calc . . . H(26) H 0.9751 0.4306 0.4521 0.0859 Uiso 1.00 calc . . . H(27) H 0.9512 0.3811 0.3511 0.0859 Uiso 1.00 calc . . . H(28) H 0.6372 0.6527 0.3618 0.0645 Uiso 1.00 calc . . . H(29) H 0.6955 0.6588 0.5573 0.0678 Uiso 1.00 calc . . . H(30) H 0.6042 0.6318 0.5102 0.0678 Uiso 1.00 calc . . . H(31) H 0.6266 0.7226 0.5155 0.0678 Uiso 1.00 calc . . . H(32) H 0.8031 0.6901 0.4525 0.0767 Uiso 1.00 calc . . . H(33) H 0.7327 0.7557 0.4173 0.0767 Uiso 1.00 calc . . . H(34) H 0.7738 0.6879 0.3437 0.0767 Uiso 1.00 calc . . . H(35) H 0.6624 0.4959 -0.0512 0.0476 Uiso 1.00 calc . . . H(36) H 0.7656 0.2972 0.0255 0.0568 Uiso 1.00 calc . . . H(37) H 0.6308 0.2808 -0.0719 0.0631 Uiso 1.00 calc . . . H(38) H 0.7090 0.2474 -0.1288 0.0631 Uiso 1.00 calc . . . H(39) H 0.6610 0.3329 -0.1414 0.0631 Uiso 1.00 calc . . . H(40) H 0.8498 0.3196 -0.0885 0.0670 Uiso 1.00 calc . . . H(41) H 0.8580 0.3910 -0.0028 0.0670 Uiso 1.00 calc . . . H(42) H 0.7985 0.4044 -0.0965 0.0670 Uiso 1.00 calc . . . H(43) H 0.5201 0.6063 0.1189 0.0442 Uiso 1.00 calc . . . H(44) H 0.5079 0.6808 -0.0060 0.0475 Uiso 1.00 calc . . . H(45) H 0.5079 0.5875 -0.0474 0.0475 Uiso 1.00 calc . . . H(46) H 0.5920 0.6336 -0.0419 0.0475 Uiso 1.00 calc . . . H(47) H 0.6437 0.6610 0.2081 0.0562 Uiso 1.00 calc . . . H(48) H 0.5916 0.7258 0.1504 0.0562 Uiso 1.00 calc . . . H(49) H 0.6757 0.6782 0.1150 0.0562 Uiso 1.00 calc . . . H(50) H 1.0402 0.1499 0.0788 0.0403 Uiso 1.00 calc . . . H(51) H 1.1109 0.4233 0.0742 0.0712 Uiso 1.00 calc . . . H(52) H 0.9893 0.4790 0.2648 0.1355 Uiso 1.00 calc . . . H(53) H 1.0864 0.5348 0.2239 0.0903 Uiso 1.00 calc . . . H(54) H 1.0073 0.5992 0.2383 0.0903 Uiso 1.00 calc . . . H(55) H 1.0282 0.5626 0.1357 0.0903 Uiso 1.00 calc . . . H(56) H 0.8660 0.5556 0.2304 0.0638 Uiso 1.00 calc . . . H(57) H 0.8549 0.4614 0.2126 0.0638 Uiso 1.00 calc . . . H(58) H 0.8566 0.5081 0.1266 0.0638 Uiso 1.00 calc . . . H(59) H 1.1336 0.1957 -0.0012 0.0577 Uiso 1.00 calc . . . H(60) H 1.2428 0.2491 0.1136 0.0606 Uiso 1.00 calc . . . H(61) H 1.2460 0.3226 0.0584 0.0606 Uiso 1.00 calc . . . H(62) H 1.2762 0.2337 0.0137 0.0606 Uiso 1.00 calc . . . H(63) H 1.1516 0.3302 -0.0920 0.0640 Uiso 1.00 calc . . . H(64) H 1.0736 0.2748 -0.1222 0.0640 Uiso 1.00 calc . . . H(65) H 1.1683 0.2379 -0.1346 0.0640 Uiso 1.00 calc . . . H(66) H 1.0830 0.1247 0.4031 0.0588 Uiso 1.00 calc . . . H(67) H 0.8408 0.1335 0.3880 0.0599 Uiso 1.00 calc . . . H(68) H 0.9846 0.1260 0.5263 0.0705 Uiso 1.00 calc . . . H(69) H 0.8876 0.1401 0.5465 0.0705 Uiso 1.00 calc . . . H(70) H 0.9309 0.2080 0.5090 0.0705 Uiso 1.00 calc . . . H(71) H 0.8622 0.0064 0.4383 0.0608 Uiso 1.00 calc . . . H(72) H 0.9591 -0.0015 0.4180 0.0608 Uiso 1.00 calc . . . H(73) H 0.8842 -0.0043 0.3336 0.0608 Uiso 1.00 calc . . . H(74) H 1.1563 0.1682 0.1821 0.0720 Uiso 1.00 calc . . . H(75) H 1.2280 0.2756 0.2782 0.0760 Uiso 1.00 calc . . . H(76) H 1.1682 0.2737 0.3570 0.0760 Uiso 1.00 calc . . . H(77) H 1.1285 0.3007 0.2599 0.0760 Uiso 1.00 calc . . . H(78) H 1.2105 0.0620 0.2721 0.0790 Uiso 1.00 calc . . . H(79) H 1.2296 0.1297 0.3601 0.0790 Uiso 1.00 calc . . . H(80) H 1.2794 0.1247 0.2714 0.0790 Uiso 1.00 calc . . . H(81) H 0.8094 0.0604 -0.1495 0.0497 Uiso 1.00 calc . . . H(82) H 0.6826 0.0788 0.0585 0.0529 Uiso 1.00 calc . . . H(83) H 0.6204 0.1352 -0.0751 0.0599 Uiso 1.00 calc . . . H(84) H 0.5792 0.0532 -0.0725 0.0599 Uiso 1.00 calc . . . H(85) H 0.6494 0.0550 -0.1405 0.0599 Uiso 1.00 calc . . . H(86) H 0.6651 -0.0575 0.0046 0.0558 Uiso 1.00 calc . . . H(87) H 0.7635 -0.0486 0.0410 0.0558 Uiso 1.00 calc . . . H(88) H 0.7321 -0.0599 -0.0681 0.0558 Uiso 1.00 calc . . . H(89) H 1.0113 0.1734 -0.0859 0.0498 Uiso 1.00 calc . . . H(90) H 0.9044 0.1924 -0.2120 0.0608 Uiso 1.00 calc . . . H(91) H 0.9107 0.0980 -0.2476 0.0608 Uiso 1.00 calc . . . H(92) H 0.9895 0.1492 -0.2497 0.0608 Uiso 1.00 calc . . . H(93) H 1.0066 0.0036 -0.1521 0.0568 Uiso 1.00 calc . . . H(94) H 1.0602 0.0397 -0.0570 0.0568 Uiso 1.00 calc . . . H(95) H 1.0857 0.0545 -0.1542 0.0568 Uiso 1.00 calc . . . H(98) H 0.5978 0.0076 0.5219 0.1061 Uiso 1.00 calc . . . H(99) H 0.6143 -0.1156 0.3611 0.1024 Uiso 1.00 calc . . . H(100) H 0.5118 -0.0410 0.2643 0.1490 Uiso 1.00 calc . . . H(101) H 0.5521 -0.1207 0.2068 0.1490 Uiso 1.00 calc . . . H(102) H 0.5845 -0.0354 0.2007 0.1490 Uiso 1.00 calc . . . H(103) H 0.7072 -0.1679 0.2501 0.1131 Uiso 1.00 calc . . . H(104) H 0.7621 -0.1163 0.3340 0.1131 Uiso 1.00 calc . . . H(105) H 0.7301 -0.0800 0.2404 0.1131 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr(1) 0.0267(3) 0.0264(3) 0.0244(3) -0.0001(2) 0.0037(2) 0.0054(2) Cr(2) 0.0276(3) 0.0274(3) 0.0256(3) 0.0004(2) 0.0021(2) 0.0059(2) O(1) 0.032(1) 0.028(1) 0.035(1) 0.0021(10) 0.005(1) 0.006(1) O(2) 0.029(1) 0.029(1) 0.031(1) 0.0008(10) -0.0003(10) 0.002(1) O(3) 0.034(1) 0.032(1) 0.024(1) -0.0027(10) 0.0049(10) 0.008(1) O(4) 0.043(1) 0.033(1) 0.039(2) -0.001(1) 0.006(1) 0.009(1) N(11) 0.029(1) 0.028(2) 0.034(2) -0.002(1) 0.003(1) 0.008(1) N(12) 0.032(2) 0.030(2) 0.034(2) 0.002(1) 0.010(1) 0.010(1) N(21) 0.035(2) 0.029(2) 0.026(2) 0.002(1) 0.001(1) 0.004(1) N(22) 0.041(2) 0.025(2) 0.027(2) -0.003(1) 0.007(1) 0.001(1) N(31) 0.032(2) 0.028(2) 0.026(2) 0.003(1) 0.006(1) 0.005(1) N(32) 0.028(1) 0.028(2) 0.029(2) 0.002(1) 0.002(1) 0.010(1) N(41) 0.036(2) 0.032(2) 0.065(2) -0.006(1) 0.017(2) -0.004(2) N(42) 0.029(2) 0.033(2) 0.045(2) -0.005(1) 0.009(1) 0.003(1) N(51) 0.031(1) 0.031(2) 0.032(2) 0.001(1) 0.002(1) 0.008(1) N(52) 0.024(1) 0.040(2) 0.031(2) -0.003(1) 0.000(1) 0.003(1) N(61) 0.028(1) 0.029(2) 0.032(2) -0.002(1) 0.003(1) 0.005(1) N(62) 0.025(1) 0.034(2) 0.027(2) -0.001(1) 0.004(1) 0.006(1) N(71) 0.055(2) 0.069(3) 0.045(2) -0.015(2) 0.010(2) 0.009(2) N(72) 0.056(2) 0.051(2) 0.048(2) -0.013(2) 0.007(2) 0.020(2) C(11) 0.028(2) 0.032(2) 0.043(2) 0.001(1) 0.008(2) 0.013(2) C(12) 0.032(2) 0.045(2) 0.053(3) -0.001(2) 0.011(2) 0.020(2) C(13) 0.032(2) 0.043(2) 0.036(2) 0.005(2) 0.008(2) 0.012(2) C(14) 0.032(2) 0.037(2) 0.052(3) -0.005(2) 0.003(2) 0.010(2) C(15) 0.047(2) 0.051(3) 0.090(4) -0.003(2) 0.023(2) 0.026(3) C(16) 0.051(3) 0.042(3) 0.079(4) -0.005(2) -0.006(2) 0.002(2) C(17) 0.038(2) 0.041(2) 0.057(3) 0.009(2) 0.016(2) 0.018(2) C(18) 0.061(3) 0.063(4) 0.080(4) 0.014(2) 0.011(3) -0.007(3) C(19) 0.044(2) 0.066(3) 0.068(3) 0.014(2) 0.015(2) 0.025(3) C(21) 0.042(2) 0.035(2) 0.033(2) -0.003(2) 0.001(2) 0.004(2) C(22) 0.061(3) 0.041(3) 0.043(3) -0.007(2) -0.014(2) 0.000(2) C(23) 0.058(2) 0.037(2) 0.031(2) -0.001(2) 0.004(2) 0.003(2) C(24) 0.049(2) 0.040(2) 0.038(2) -0.001(2) -0.010(2) 0.005(2) C(25) 0.148(6) 0.096(5) 0.051(4) 0.057(4) 0.012(4) 0.027(3) C(26) 0.056(3) 0.079(4) 0.123(6) -0.001(3) -0.007(3) 0.032(4) C(27) 0.079(3) 0.033(2) 0.036(2) 0.000(2) -0.006(2) -0.002(2) C(28) 0.082(4) 0.054(3) 0.058(3) 0.003(3) 0.002(3) -0.011(3) C(29) 0.118(5) 0.042(3) 0.068(4) -0.012(3) 0.006(3) 0.006(3) C(31) 0.042(2) 0.038(2) 0.028(2) 0.006(2) 0.007(2) 0.008(2) C(32) 0.049(2) 0.043(2) 0.028(2) 0.003(2) 0.009(2) 0.015(2) C(33) 0.028(2) 0.034(2) 0.029(2) -0.002(1) 0.002(1) 0.008(2) C(34) 0.065(3) 0.045(3) 0.032(2) 0.020(2) 0.018(2) 0.014(2) C(35) 0.080(3) 0.054(3) 0.049(3) 0.008(2) 0.016(2) -0.007(2) C(36) 0.073(3) 0.080(4) 0.053(3) 0.016(3) 0.034(3) 0.015(3) C(37) 0.039(2) 0.030(2) 0.037(2) 0.000(2) 0.004(2) 0.011(2) C(38) 0.054(2) 0.043(3) 0.047(3) 0.001(2) -0.004(2) 0.021(2) C(39) 0.082(3) 0.038(3) 0.051(3) -0.009(2) 0.006(2) 0.011(2) C(41) 0.043(2) 0.038(3) 0.101(4) -0.004(2) 0.032(2) 0.005(2) C(42) 0.039(2) 0.040(3) 0.100(4) -0.008(2) 0.025(2) 0.014(2) C(43) 0.032(2) 0.041(2) 0.052(3) -0.004(2) 0.013(2) 0.013(2) C(44) 0.066(4) 0.037(3) 0.210(8) -0.015(3) 0.066(4) -0.015(4) C(45) 0.070(4) 0.064(4) 0.127(6) -0.016(3) 0.015(4) -0.027(4) C(46) 0.063(3) 0.041(3) 0.088(4) 0.000(2) 0.023(3) 0.002(3) C(47) 0.036(2) 0.052(3) 0.051(3) -0.002(2) 0.014(2) 0.013(2) C(48) 0.036(2) 0.067(3) 0.080(4) -0.004(2) 0.014(2) 0.008(3) C(49) 0.057(3) 0.072(4) 0.071(4) -0.005(2) 0.025(3) 0.022(3) C(51) 0.035(2) 0.045(2) 0.033(2) 0.006(2) -0.005(2) 0.013(2) C(52) 0.044(2) 0.068(3) 0.032(2) 0.003(2) -0.011(2) 0.011(2) C(53) 0.032(2) 0.057(3) 0.038(2) -0.006(2) -0.006(2) 0.000(2) C(54) 0.048(2) 0.059(3) 0.040(2) 0.013(2) 0.006(2) 0.025(2) C(55) 0.099(4) 0.070(4) 0.044(3) 0.022(3) 0.018(3) 0.020(3) C(56) 0.062(3) 0.071(4) 0.054(3) -0.003(2) 0.003(2) 0.027(3) C(57) 0.028(2) 0.103(4) 0.042(3) -0.011(2) -0.006(2) 0.002(3) C(58) 0.056(3) 0.106(5) 0.065(4) -0.035(3) -0.005(3) 0.002(3) C(59) 0.038(2) 0.113(5) 0.075(4) -0.001(3) -0.009(2) -0.003(3) C(61) 0.034(2) 0.034(2) 0.032(2) 0.000(2) -0.002(2) -0.002(2) C(62) 0.037(2) 0.051(3) 0.027(2) 0.000(2) -0.002(2) -0.002(2) C(63) 0.038(2) 0.039(2) 0.028(2) 0.000(2) 0.005(1) 0.006(2) C(64) 0.033(2) 0.046(2) 0.040(2) -0.006(2) -0.002(2) -0.003(2) C(65) 0.040(2) 0.075(4) 0.063(3) -0.015(2) -0.011(2) 0.012(3) C(66) 0.053(3) 0.042(3) 0.072(3) -0.012(2) 0.010(2) 0.000(2) C(67) 0.040(2) 0.049(3) 0.029(2) 0.001(2) 0.008(2) 0.005(2) C(68) 0.055(3) 0.088(4) 0.041(3) 0.009(2) 0.014(2) 0.018(3) C(69) 0.051(3) 0.061(3) 0.057(3) 0.008(2) 0.018(2) 0.003(2) C(71) 0.059(3) 0.128(6) 0.057(4) -0.024(3) 0.012(3) 0.024(4) C(72) 0.086(4) 0.149(7) 0.064(4) -0.043(4) 0.003(3) 0.060(4) C(73) 0.054(3) 0.071(4) 0.080(4) -0.016(2) -0.001(3) 0.044(3) C(74) 0.095(5) 0.26(1) 0.052(4) -0.037(6) 0.033(4) -0.044(6) C(75) 0.148(9) 0.21(1) 0.17(1) -0.005(8) 0.036(8) -0.025(9) C(76) 0.076(7) 0.14(1) 0.17(1) -0.029(7) 0.034(8) -0.08(1) C(76A) 0.20(2) 0.14(2) 0.009(6) 0.06(1) -0.025(8) -0.002(8) C(77) 0.066(3) 0.057(4) 0.134(6) -0.020(3) -0.005(4) 0.046(4) C(78) 0.168(8) 0.081(6) 0.172(9) -0.018(5) -0.079(7) 0.016(6) C(79) 0.135(6) 0.074(5) 0.137(7) -0.032(4) 0.022(5) 0.015(5) B(1) 0.034(2) 0.021(2) 0.036(2) 0.005(2) 0.007(2) 0.005(2) B(2) 0.031(2) 0.033(2) 0.033(2) -0.001(2) 0.005(2) 0.004(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr(1) Cr(2) 2.6761(7) . . yes Cr(1) O(1) 1.921(2) . . yes Cr(1) O(2) 1.984(2) . . yes Cr(1) O(3) 1.968(3) . . yes Cr(1) N(11) 2.067(3) . . yes Cr(1) N(21) 2.073(3) . . yes Cr(1) N(31) 2.092(3) . . yes Cr(2) O(1) 1.959(3) . . yes Cr(2) O(2) 2.027(2) . . yes Cr(2) O(3) 1.999(2) . . yes Cr(2) O(4) 1.933(3) . . yes Cr(2) N(51) 2.062(3) . . yes Cr(2) N(61) 2.041(3) . . yes N(11) N(12) 1.387(4) . . yes N(11) C(11) 1.345(5) . . yes N(12) C(13) 1.364(5) . . yes N(12) B(1) 1.542(5) . . yes N(21) N(22) 1.376(4) . . yes N(21) C(21) 1.336(4) . . yes N(22) C(23) 1.353(5) . . yes N(22) B(1) 1.546(5) . . yes N(31) N(32) 1.377(4) . . yes N(31) C(31) 1.348(5) . . yes N(32) C(33) 1.352(5) . . yes N(32) B(1) 1.542(5) . . yes N(41) N(42) 1.383(4) . . yes N(41) C(41) 1.334(6) . . yes N(42) C(43) 1.379(5) . . yes N(42) B(2) 1.541(6) . . yes N(51) N(52) 1.386(4) . . yes N(51) C(51) 1.336(5) . . yes N(52) C(53) 1.370(5) . . yes N(52) B(2) 1.568(6) . . yes N(61) N(62) 1.395(4) . . yes N(61) C(61) 1.341(4) . . yes N(62) C(63) 1.359(4) . . yes N(62) B(2) 1.581(5) . . yes N(71) N(72) 1.360(5) . . yes N(71) C(71) 1.321(8) . . yes N(72) C(73) 1.348(8) . . yes C(11) C(12) 1.393(5) . . yes C(11) C(14) 1.511(6) . . yes C(12) C(13) 1.377(6) . . yes C(13) C(17) 1.512(5) . . yes C(14) C(15) 1.519(8) . . yes C(14) C(16) 1.515(6) . . yes C(17) C(18) 1.521(7) . . yes C(17) C(19) 1.524(6) . . yes C(21) C(22) 1.384(6) . . yes C(21) C(24) 1.514(6) . . yes C(22) C(23) 1.387(6) . . yes C(23) C(27) 1.496(6) . . yes C(24) C(25) 1.514(7) . . yes C(24) C(26) 1.515(7) . . yes C(27) C(28) 1.534(7) . . yes C(27) C(29) 1.517(8) . . yes C(31) C(32) 1.402(6) . . yes C(31) C(34) 1.501(6) . . yes C(32) C(33) 1.382(5) . . yes C(33) C(37) 1.504(5) . . yes C(34) C(35) 1.537(6) . . yes C(34) C(36) 1.528(7) . . yes C(37) C(38) 1.526(6) . . yes C(37) C(39) 1.523(6) . . yes C(41) C(42) 1.388(7) . . yes C(41) C(44) 1.531(7) . . yes C(42) C(43) 1.373(6) . . yes C(43) C(47) 1.512(6) . . yes C(44) C(45) 1.392(9) . . yes C(44) C(46) 1.481(7) . . yes C(47) C(48) 1.531(6) . . yes C(47) C(49) 1.533(7) . . yes C(51) C(52) 1.383(5) . . yes C(51) C(54) 1.492(6) . . yes C(52) C(53) 1.369(7) . . yes C(53) C(57) 1.498(6) . . yes C(54) C(55) 1.524(6) . . yes C(54) C(56) 1.524(7) . . yes C(57) C(58) 1.542(8) . . yes C(57) C(59) 1.523(7) . . yes C(61) C(62) 1.394(6) . . yes C(61) C(64) 1.507(6) . . yes C(62) C(63) 1.368(5) . . yes C(63) C(67) 1.506(6) . . yes C(64) C(65) 1.523(6) . . yes C(64) C(66) 1.527(6) . . yes C(67) C(68) 1.522(6) . . yes C(67) C(69) 1.538(6) . . yes C(71) C(72) 1.39(1) . . yes C(71) C(74) 1.52(1) . . yes C(72) C(73) 1.396(9) . . yes C(73) C(77) 1.521(8) . . yes C(74) C(75) 1.45(1) . . yes C(74) C(76) 1.37(2) . . yes C(74) C(76A) 1.63(2) . . yes C(77) C(78) 1.51(1) . . yes C(77) C(79) 1.535(10) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr(2) Cr(1) O(1) 47.00(7) . . . yes Cr(2) Cr(1) O(2) 48.84(6) . . . yes Cr(2) Cr(1) O(3) 48.08(7) . . . yes Cr(2) Cr(1) N(11) 128.58(9) . . . yes Cr(2) Cr(1) N(21) 127.82(8) . . . yes Cr(2) Cr(1) N(31) 123.63(8) . . . yes O(1) Cr(1) O(2) 80.91(9) . . . yes O(1) Cr(1) O(3) 79.0(1) . . . yes O(1) Cr(1) N(11) 173.6(1) . . . yes O(1) Cr(1) N(21) 99.2(1) . . . yes O(1) Cr(1) N(31) 92.7(1) . . . yes O(2) Cr(1) O(3) 80.31(10) . . . yes O(2) Cr(1) N(11) 92.7(1) . . . yes O(2) Cr(1) N(21) 174.8(1) . . . yes O(2) Cr(1) N(31) 95.6(1) . . . yes O(3) Cr(1) N(11) 100.9(1) . . . yes O(3) Cr(1) N(21) 94.5(1) . . . yes O(3) Cr(1) N(31) 171.2(1) . . . yes N(11) Cr(1) N(21) 87.2(1) . . . yes N(11) Cr(1) N(31) 87.0(1) . . . yes N(21) Cr(1) N(31) 89.6(1) . . . yes Cr(1) Cr(2) O(1) 45.82(7) . . . yes Cr(1) Cr(2) O(2) 47.46(6) . . . yes Cr(1) Cr(2) O(3) 47.10(7) . . . yes Cr(1) Cr(2) O(4) 124.72(8) . . . yes Cr(1) Cr(2) N(51) 126.21(8) . . . yes Cr(1) Cr(2) N(61) 122.61(9) . . . yes O(1) Cr(2) O(2) 78.93(9) . . . yes O(1) Cr(2) O(3) 77.4(1) . . . yes O(1) Cr(2) O(4) 170.1(1) . . . yes O(1) Cr(2) N(51) 91.4(1) . . . yes O(1) Cr(2) N(61) 96.6(1) . . . yes O(2) Cr(2) O(3) 78.53(9) . . . yes O(2) Cr(2) O(4) 95.8(1) . . . yes O(2) Cr(2) N(51) 169.9(1) . . . yes O(2) Cr(2) N(61) 91.7(1) . . . yes O(3) Cr(2) O(4) 93.4(1) . . . yes O(3) Cr(2) N(51) 102.2(1) . . . yes O(3) Cr(2) N(61) 169.3(1) . . . yes O(4) Cr(2) N(51) 94.2(1) . . . yes O(4) Cr(2) N(61) 91.9(1) . . . yes N(51) Cr(2) N(61) 86.6(1) . . . yes Cr(1) O(1) Cr(2) 87.2(1) . . . yes Cr(1) O(2) Cr(2) 83.70(8) . . . yes Cr(1) O(3) Cr(2) 84.82(10) . . . yes Cr(1) N(11) N(12) 117.2(2) . . . yes Cr(1) N(11) C(11) 135.5(2) . . . yes N(12) N(11) C(11) 107.2(3) . . . yes N(11) N(12) C(13) 108.5(3) . . . yes N(11) N(12) B(1) 119.4(3) . . . yes C(13) N(12) B(1) 131.4(3) . . . yes Cr(1) N(21) N(22) 117.4(2) . . . yes Cr(1) N(21) C(21) 134.9(2) . . . yes N(22) N(21) C(21) 107.2(3) . . . yes N(21) N(22) C(23) 109.6(3) . . . yes N(21) N(22) B(1) 118.9(3) . . . yes C(23) N(22) B(1) 131.4(3) . . . yes Cr(1) N(31) N(32) 118.0(2) . . . yes Cr(1) N(31) C(31) 135.2(2) . . . yes N(32) N(31) C(31) 106.8(3) . . . yes N(31) N(32) C(33) 110.1(3) . . . yes N(31) N(32) B(1) 118.4(3) . . . yes C(33) N(32) B(1) 131.5(3) . . . yes N(42) N(41) C(41) 106.9(3) . . . yes N(41) N(42) C(43) 108.5(3) . . . yes N(41) N(42) B(2) 120.5(3) . . . yes C(43) N(42) B(2) 130.5(3) . . . yes Cr(2) N(51) N(52) 122.0(2) . . . yes Cr(2) N(51) C(51) 129.5(3) . . . yes N(52) N(51) C(51) 107.7(3) . . . yes N(51) N(52) C(53) 107.8(3) . . . yes N(51) N(52) B(2) 128.2(3) . . . yes C(53) N(52) B(2) 123.6(3) . . . yes Cr(2) N(61) N(62) 123.1(2) . . . yes Cr(2) N(61) C(61) 128.4(2) . . . yes N(62) N(61) C(61) 107.6(3) . . . yes N(61) N(62) C(63) 107.6(3) . . . yes N(61) N(62) B(2) 125.9(3) . . . yes C(63) N(62) B(2) 125.0(3) . . . yes N(72) N(71) C(71) 106.3(5) . . . yes N(71) N(72) C(73) 112.5(4) . . . yes N(11) C(11) C(12) 109.6(3) . . . yes N(11) C(11) C(14) 123.9(3) . . . yes C(12) C(11) C(14) 126.5(3) . . . yes C(11) C(12) C(13) 106.4(3) . . . yes N(12) C(13) C(12) 108.3(3) . . . yes N(12) C(13) C(17) 122.8(3) . . . yes C(12) C(13) C(17) 128.8(3) . . . yes C(11) C(14) C(15) 111.3(3) . . . yes C(11) C(14) C(16) 110.4(4) . . . yes C(15) C(14) C(16) 110.8(4) . . . yes C(13) C(17) C(18) 110.6(4) . . . yes C(13) C(17) C(19) 111.2(3) . . . yes C(18) C(17) C(19) 110.5(4) . . . yes N(21) C(21) C(22) 109.3(3) . . . yes N(21) C(21) C(24) 124.8(3) . . . yes C(22) C(21) C(24) 125.8(3) . . . yes C(21) C(22) C(23) 106.8(4) . . . yes N(22) C(23) C(22) 107.0(3) . . . yes N(22) C(23) C(27) 125.5(3) . . . yes C(22) C(23) C(27) 127.5(4) . . . yes C(21) C(24) C(25) 108.9(4) . . . yes C(21) C(24) C(26) 112.9(4) . . . yes C(25) C(24) C(26) 109.9(4) . . . yes C(23) C(27) C(28) 110.9(4) . . . yes C(23) C(27) C(29) 109.8(4) . . . yes C(28) C(27) C(29) 109.9(4) . . . yes N(31) C(31) C(32) 109.1(3) . . . yes N(31) C(31) C(34) 124.3(4) . . . yes C(32) C(31) C(34) 126.6(4) . . . yes C(31) C(32) C(33) 106.5(4) . . . yes N(32) C(33) C(32) 107.4(3) . . . yes N(32) C(33) C(37) 123.9(3) . . . yes C(32) C(33) C(37) 128.7(4) . . . yes C(31) C(34) C(35) 109.7(4) . . . yes C(31) C(34) C(36) 111.2(4) . . . yes C(35) C(34) C(36) 110.7(4) . . . yes C(33) C(37) C(38) 111.3(3) . . . yes C(33) C(37) C(39) 111.9(3) . . . yes C(38) C(37) C(39) 109.5(4) . . . yes N(41) C(41) C(42) 110.5(4) . . . yes N(41) C(41) C(44) 121.0(5) . . . yes C(42) C(41) C(44) 128.4(5) . . . yes C(41) C(42) C(43) 106.3(4) . . . yes N(42) C(43) C(42) 107.8(4) . . . yes N(42) C(43) C(47) 126.5(4) . . . yes C(42) C(43) C(47) 125.7(4) . . . yes C(41) C(44) C(45) 115.6(6) . . . yes C(41) C(44) C(46) 114.3(4) . . . yes C(45) C(44) C(46) 120.5(5) . . . yes C(43) C(47) C(48) 111.3(3) . . . yes C(43) C(47) C(49) 110.4(4) . . . yes C(48) C(47) C(49) 109.3(4) . . . yes N(51) C(51) C(52) 109.5(4) . . . yes N(51) C(51) C(54) 123.6(3) . . . yes C(52) C(51) C(54) 126.8(4) . . . yes C(51) C(52) C(53) 106.9(4) . . . yes N(52) C(53) C(52) 108.2(3) . . . yes N(52) C(53) C(57) 123.8(4) . . . yes C(52) C(53) C(57) 127.8(4) . . . yes C(51) C(54) C(55) 111.3(4) . . . yes C(51) C(54) C(56) 111.2(4) . . . yes C(55) C(54) C(56) 109.4(4) . . . yes C(53) C(57) C(58) 109.6(4) . . . yes C(53) C(57) C(59) 111.4(5) . . . yes C(58) C(57) C(59) 110.1(4) . . . yes N(61) C(61) C(62) 109.2(3) . . . yes N(61) C(61) C(64) 124.2(3) . . . yes C(62) C(61) C(64) 126.4(3) . . . yes C(61) C(62) C(63) 106.4(3) . . . yes N(62) C(63) C(62) 109.2(3) . . . yes N(62) C(63) C(67) 123.6(3) . . . yes C(62) C(63) C(67) 127.2(3) . . . yes C(61) C(64) C(65) 112.7(4) . . . yes C(61) C(64) C(66) 110.5(3) . . . yes C(65) C(64) C(66) 109.5(4) . . . yes C(63) C(67) C(68) 111.7(3) . . . yes C(63) C(67) C(69) 110.2(4) . . . yes C(68) C(67) C(69) 110.0(3) . . . yes N(71) C(71) C(72) 109.4(5) . . . yes N(71) C(71) C(74) 119.5(7) . . . yes C(72) C(71) C(74) 131.0(7) . . . yes C(71) C(72) C(73) 107.4(6) . . . yes N(72) C(73) C(72) 104.3(5) . . . yes N(72) C(73) C(77) 120.9(5) . . . yes C(72) C(73) C(77) 134.7(6) . . . yes C(71) C(74) C(75) 115.3(7) . . . yes C(71) C(74) C(76) 121.6(9) . . . yes C(71) C(74) C(76A) 100.8(9) . . . yes C(75) C(74) C(76) 120.9(10) . . . yes C(75) C(74) C(76A) 102(1) . . . yes C(76) C(74) C(76A) 81(1) . . . yes C(73) C(77) C(78) 110.9(5) . . . yes C(73) C(77) C(79) 113.1(5) . . . yes C(78) C(77) C(79) 107.0(6) . . . yes N(12) B(1) N(22) 109.5(3) . . . yes N(12) B(1) N(32) 108.9(3) . . . yes N(22) B(1) N(32) 108.3(3) . . . yes N(42) B(2) N(52) 110.4(3) . . . yes N(42) B(2) N(62) 116.0(3) . . . yes N(52) B(2) N(62) 112.0(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cr(1) Cr(2) 2.6761(7) . . ? C(65) C(78) 3.580(9) . 2_655 ? O(1) O(2) 2.534(3) . . ? O(1) N(41) 2.646(4) . . ? O(1) N(51) 2.879(4) . . ? O(1) N(31) 2.906(3) . . ? O(1) N(61) 2.988(4) . . ? O(2) O(3) 2.549(3) . . ? O(2) N(61) 2.919(4) . . ? O(2) N(11) 2.933(4) . . ? O(2) O(4) 2.940(4) . . ? O(3) O(4) 2.862(3) . . ? O(3) N(21) 2.970(4) . . ? O(3) N(71) 2.974(5) . . ? O(4) N(72) 2.642(5) . . ? O(4) N(61) 2.857(4) . . ? O(4) N(51) 2.927(4) . . ? N(11) N(21) 2.856(4) . . ? N(11) N(31) 2.865(4) . . ? N(12) N(32) 2.510(4) . . ? N(12) N(22) 2.521(4) . . ? N(12) N(21) 2.974(4) . . ? N(21) N(31) 2.936(4) . . ? N(22) N(32) 2.503(4) . . ? N(42) N(52) 2.553(5) . . ? N(42) N(62) 2.647(4) . . ? N(51) N(61) 2.815(4) . . ? N(52) N(62) 2.610(4) . . ? #------------------------------------------------------------------------------ #===END