#------------------------------------------------------------------------------ #$Date: 2015-11-25 18:35:01 +0200 (Wed, 25 Nov 2015) $ #$Revision: 170533 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/80/7118072.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7118072 loop_ _publ_author_name 'Savi\'c, Nada D' 'Gli\ 2\s(I)' _iucr_refine_instructions_details ; co_bg18.res created by SHELXL-2014/7 TITL co_bg18 - #2331 - in P-1 - superflip - smart CELL 0.71073 7.5443 8.1087 11.1747 110.4953 99.2196 98.0356 ZERR 1 0.0032 0.0035 0.0047 0.0115 0.0092 0.0111 LATT 1 SFAC C H Ag B F N UNIT 20 18 2 2 8 6 L.S. 10 PLAN 25 SIZE 0.12 0.15 0.33 TEMP -173 BOND $H CONF HTAB MORE -1 fmap 2 acta REM REM REM WGHT 0.020900 0.350000 FVAR 0.15480 AG 3 1.015120 0.837950 0.859196 11.00000 0.02128 0.00883 = 0.01625 0.00268 0.00529 0.00031 N1 6 0.871535 0.751487 1.002739 11.00000 0.01454 0.00991 = 0.01221 0.00152 0.00225 0.00096 N2 6 0.846023 0.885429 1.111751 11.00000 0.01685 0.00964 = 0.01364 0.00157 0.00271 0.00109 N3 6 0.949609 0.565763 0.695561 11.00000 0.02445 0.01413 = 0.01858 0.00348 0.00481 0.00262 C1 1 0.765997 0.841914 1.195181 11.00000 0.01633 0.01205 = 0.01525 0.00236 0.00337 0.00156 H1 2 0.748416 0.943894 1.269964 11.00000 -1.20000 C2 1 0.703677 0.662068 1.183103 11.00000 0.01225 0.01264 = 0.01463 0.00404 0.00221 0.00142 C3 1 0.618199 0.617334 1.274411 11.00000 0.01793 0.01962 = 0.01983 0.00757 0.00768 0.00375 H3 2 0.600321 0.717028 1.352116 11.00000 -1.20000 C4 1 0.561142 0.438468 1.252276 11.00000 0.01780 0.02130 = 0.02390 0.01168 0.00799 0.00216 H4 2 0.506503 0.405278 1.312590 11.00000 -1.20000 C5 1 0.586931 0.301369 1.140913 11.00000 0.01615 0.01493 = 0.02454 0.00992 0.00451 0.00089 H5 2 0.545030 0.183252 1.130518 11.00000 -1.20000 C6 1 0.669478 0.342944 1.050750 11.00000 0.01371 0.01218 = 0.01996 0.00616 0.00289 0.00137 H6 2 0.688097 0.246284 0.973411 11.00000 -1.20000 C7 1 0.728827 0.525671 1.071769 11.00000 0.01057 0.01055 = 0.01447 0.00391 0.00082 0.00071 C8 1 0.813757 0.582362 0.984316 11.00000 0.01219 0.01059 = 0.01303 0.00308 0.00211 0.00176 H8 2 0.831453 0.493805 0.905885 11.00000 -1.20000 C9 1 0.926669 0.424612 0.618245 11.00000 0.01923 0.01508 = 0.01601 0.00518 0.00534 0.00203 C10 1 0.898325 0.245515 0.517224 11.00000 0.03171 0.01477 = 0.02103 -0.00161 0.01127 -0.00012 AFIX 138 H10A 2 0.786560 0.218559 0.462442 11.00000 -1.50000 H10B 2 0.903635 0.163605 0.555246 11.00000 -1.50000 H10C 2 0.987108 0.242719 0.471001 11.00000 -1.50000 AFIX 0 F1 5 0.285125 0.030110 0.177173 11.00000 0.02730 0.02286 = 0.03068 0.01630 0.01272 0.00722 F2 5 0.253536 -0.190395 0.256532 11.00000 0.07063 0.01410 = 0.02885 0.00984 0.02543 0.01066 F3 5 0.205708 0.084480 0.373025 11.00000 0.03586 0.02318 = 0.03226 0.00810 0.01951 0.01428 F4 5 0.493968 0.049087 0.352814 11.00000 0.02066 0.07031 = 0.04228 0.01057 -0.00131 0.01045 B 4 0.310206 -0.006618 0.291302 11.00000 0.01867 0.01465 = 0.02212 0.00529 0.00718 0.00546 HKLF 4 REM co_bg18 - #2331 - in P-1 - superflip - smart REM R1 = 0.0196 for 3860 Fo > 4sig(Fo) and 0.0222 for all 4134 data REM 192 parameters refined using 0 restraints END WGHT 0.0210 0.3494 REM Instructions for potential hydrogen bonds EQIV $1 x, y+1, z+1 HTAB C1 F4_$1 EQIV $2 -x+1, -y, -z+1 HTAB C8 F2_$2 HTAB C10 F4 HTAB C10 F2_$2 HTAB C10 F3_$2 EQIV $3 x+1, y, z HTAB C10 F3_$3 REM Highest difference peak 0.640, deepest hole -0.294, 1-sigma level 0.085 Q1 1 1.0455 0.5207 0.5778 11.00000 0.05 0.64 Q2 1 1.1242 0.8171 0.8501 11.00000 0.05 0.62 Q3 1 0.9233 0.8533 0.8652 11.00000 0.05 0.62 Q4 1 1.0152 0.8344 0.7942 11.00000 0.05 0.62 Q5 1 0.6649 0.6354 1.2255 11.00000 0.05 0.58 Q6 1 1.0645 0.8563 0.9377 11.00000 0.05 0.57 Q7 1 0.7473 0.5522 1.0142 11.00000 0.05 0.53 Q8 1 0.7966 0.8549 1.1478 11.00000 0.05 0.52 Q9 1 0.6964 0.4389 1.0675 11.00000 0.05 0.52 Q10 1 0.7134 0.5941 1.1317 11.00000 0.05 0.51 Q11 1 0.7233 0.7546 1.1903 11.00000 0.05 0.48 Q12 1 0.6210 0.3368 1.0961 11.00000 0.05 0.47 Q13 1 0.5799 0.3804 1.1958 11.00000 0.05 0.47 Q14 1 0.9168 0.7848 0.9685 11.00000 0.05 0.43 Q15 1 0.4862 0.0120 0.3914 11.00000 0.05 0.42 Q16 1 0.6036 0.5268 1.2503 11.00000 0.05 0.40 Q17 1 0.6487 0.2952 0.9973 11.00000 0.05 0.38 Q18 1 0.8404 0.8246 1.0594 11.00000 0.05 0.37 Q19 1 0.2590 0.0452 0.3318 11.00000 0.05 0.37 Q20 1 0.8155 0.6627 0.9863 11.00000 0.05 0.37 Q21 1 0.2741 0.1022 0.4294 11.00000 0.05 0.37 Q22 1 0.9748 0.5146 0.6458 11.00000 0.05 0.35 Q23 1 0.3415 -0.1282 0.2944 11.00000 0.05 0.34 Q24 1 0.8806 0.9767 1.1264 11.00000 0.05 0.33 Q25 1 0.3978 0.0735 0.3773 11.00000 0.05 0.33 ; _cod_data_source_file c5md00494b2.cif _cod_data_source_block co_bg18 _cod_database_code 7118072 _audit_block_refno 2331 _audit_block_usercomment BG79 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.825 _shelx_estimated_absorpt_t_min 0.609 _shelxl_version_number 2014/7 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Idealised Me refined as rotating group with stretchable bonds: C10(H10A,H10B,H10C) ; _shelx_res_checksum 88404 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Ag Ag 1.01512(2) 0.83795(2) 0.85920(2) 0.01622(4) Uani 1 1 d . N1 N 0.87154(16) 0.75149(15) 1.00274(11) 0.0132(2) Uani 1 1 d . N2 N 0.84602(16) 0.88543(15) 1.11175(12) 0.0144(2) Uani 1 1 d . N3 N 0.94961(19) 0.56576(17) 0.69556(13) 0.0200(2) Uani 1 1 d . C1 C 0.76600(19) 0.84191(18) 1.19518(14) 0.0155(2) Uani 1 1 d . H1 H 0.748(3) 0.944(3) 1.270(2) 0.019 Uiso 1 1 d R C2 C 0.70368(18) 0.66207(18) 1.18310(13) 0.0137(2) Uani 1 1 d . C3 C 0.6182(2) 0.6173(2) 1.27441(15) 0.0187(3) Uani 1 1 d . H3 H 0.600(3) 0.717(3) 1.352(2) 0.022 Uiso 1 1 d R C4 C 0.5611(2) 0.4385(2) 1.25228(16) 0.0200(3) Uani 1 1 d . H4 H 0.507(3) 0.405(3) 1.313(2) 0.024 Uiso 1 1 d R C5 C 0.5869(2) 0.3014(2) 1.14091(15) 0.0181(3) Uani 1 1 d . H5 H 0.545(3) 0.183(3) 1.131(2) 0.022 Uiso 1 1 d R C6 C 0.66948(19) 0.34294(18) 1.05075(15) 0.0155(2) Uani 1 1 d . H6 H 0.688(3) 0.246(3) 0.973(2) 0.019 Uiso 1 1 d R C7 C 0.72883(17) 0.52567(17) 1.07177(13) 0.0125(2) Uani 1 1 d . C8 C 0.81376(18) 0.58236(17) 0.98432(13) 0.0125(2) Uani 1 1 d . H8 H 0.831(3) 0.494(3) 0.9059(19) 0.015 Uiso 1 1 d R C9 C 0.9267(2) 0.42461(19) 0.61825(14) 0.0170(3) Uani 1 1 d . C10 C 0.8983(2) 0.2455(2) 0.51722(16) 0.0247(3) Uani 1 1 d . H10A H 0.7866(18) 0.2186(9) 0.4624(12) 0.037 Uiso 1 1 calc GR H10B H 0.9036(19) 0.1636(12) 0.5552(6) 0.037 Uiso 1 1 calc GR H10C H 0.9871(17) 0.2427(6) 0.4710(11) 0.037 Uiso 1 1 calc GR F1 F 0.28512(14) 0.03011(13) 0.17717(10) 0.02429(19) Uani 1 1 d . F2 F 0.25354(19) -0.19039(13) 0.25653(11) 0.0355(3) Uani 1 1 d . F3 F 0.20571(15) 0.08448(14) 0.37302(11) 0.0288(2) Uani 1 1 d . F4 F 0.49397(16) 0.0491(2) 0.35281(13) 0.0484(3) Uani 1 1 d . B B 0.3102(2) -0.0066(2) 0.29130(17) 0.0184(3) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02128(6) 0.00883(5) 0.01625(6) 0.00268(4) 0.00529(4) 0.00031(4) N1 0.0145(5) 0.0099(5) 0.0122(5) 0.0015(4) 0.0023(4) 0.0010(4) N2 0.0169(5) 0.0096(5) 0.0136(5) 0.0016(4) 0.0027(4) 0.0011(4) N3 0.0245(6) 0.0141(5) 0.0186(6) 0.0035(5) 0.0048(5) 0.0026(5) C1 0.0163(6) 0.0121(6) 0.0152(6) 0.0024(5) 0.0034(5) 0.0016(5) C2 0.0123(5) 0.0126(5) 0.0146(6) 0.0040(5) 0.0022(4) 0.0014(4) C3 0.0179(6) 0.0196(7) 0.0198(7) 0.0076(5) 0.0077(5) 0.0038(5) C4 0.0178(6) 0.0213(7) 0.0239(7) 0.0117(6) 0.0080(5) 0.0022(5) C5 0.0161(6) 0.0149(6) 0.0245(7) 0.0099(5) 0.0045(5) 0.0009(5) C6 0.0137(6) 0.0122(6) 0.0200(7) 0.0062(5) 0.0029(5) 0.0014(4) C7 0.0106(5) 0.0105(5) 0.0145(6) 0.0039(5) 0.0008(4) 0.0007(4) C8 0.0122(5) 0.0106(5) 0.0130(6) 0.0031(5) 0.0021(4) 0.0018(4) C9 0.0192(6) 0.0151(6) 0.0160(6) 0.0052(5) 0.0053(5) 0.0020(5) C10 0.0317(8) 0.0148(6) 0.0210(7) -0.0016(6) 0.0113(6) -0.0001(6) F1 0.0273(5) 0.0229(4) 0.0307(5) 0.0163(4) 0.0127(4) 0.0072(4) F2 0.0706(8) 0.0141(4) 0.0289(5) 0.0098(4) 0.0254(5) 0.0107(5) F3 0.0359(5) 0.0232(5) 0.0323(5) 0.0081(4) 0.0195(4) 0.0143(4) F4 0.0207(5) 0.0703(9) 0.0423(7) 0.0106(7) -0.0013(5) 0.0104(6) B 0.0187(7) 0.0147(7) 0.0221(8) 0.0053(6) 0.0072(6) 0.0055(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N2 Ag N1 127.44(4) 2_777 . N2 Ag N3 135.49(5) 2_777 . N3 Ag N1 96.99(5) . . N2 N1 Ag 117.88(8) . . C8 N1 Ag 122.87(9) . . C8 N1 N2 119.26(12) . . N1 N2 Ag 114.12(9) . 2_777 C1 N2 Ag 125.67(9) . 2_777 C1 N2 N1 119.65(12) . . C9 N3 Ag 174.77(13) . . N2 C1 H1 115.8(12) . . N2 C1 C2 124.18(13) . . C2 C1 H1 120.0(12) . . C3 C2 C1 123.48(13) . . C7 C2 C1 116.16(12) . . C7 C2 C3 120.35(13) . . C2 C3 H3 118.7(12) . . C4 C3 C2 118.64(14) . . C4 C3 H3 122.6(12) . . C3 C4 H4 120.3(13) . . C3 C4 C5 121.11(14) . . C5 C4 H4 118.6(13) . . C4 C5 H5 117.5(13) . . C6 C5 C4 120.90(13) . . C6 C5 H5 121.6(13) . . C5 C6 H6 120.5(12) . . C5 C6 C7 118.80(13) . . C7 C6 H6 120.7(12) . . C2 C7 C6 120.20(13) . . C2 C7 C8 116.68(12) . . C6 C7 C8 123.12(13) . . N1 C8 C7 124.05(12) . . N1 C8 H8 116.3(11) . . C7 C8 H8 119.6(11) . . N3 C9 C10 178.76(16) . . C9 C10 H10A 109.5 . . C9 C10 H10B 109.5 . . C9 C10 H10C 109.5 . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . F2 B F1 108.46(13) . . F2 B F3 109.73(13) . . F3 B F1 109.34(13) . . F4 B F1 108.64(13) . . F4 B F2 110.34(15) . . F4 B F3 110.30(14) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ag N1 2.3173(13) . Ag N2 2.2267(15) 2_777 Ag N3 2.2447(15) . N1 N2 1.3812(16) . N1 C8 1.3113(18) . N2 Ag 2.2267(14) 2_777 N2 C1 1.3074(19) . N3 C9 1.1361(19) . C1 H1 0.99(2) . C1 C2 1.420(2) . C2 C3 1.412(2) . C2 C7 1.4064(19) . C3 H3 1.00(2) . C3 C4 1.375(2) . C4 H4 0.94(2) . C4 C5 1.411(2) . C5 H5 0.93(2) . C5 C6 1.377(2) . C6 H6 0.99(2) . C6 C7 1.4100(19) . C7 C8 1.4177(19) . C8 H8 0.96(2) . C9 C10 1.455(2) . C10 H10A 0.907(13) . C10 H10B 0.907(13) . C10 H10C 0.907(13) . F1 B 1.398(2) . F2 B 1.385(2) . F3 B 1.3865(19) . F4 B 1.379(2) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Ag N1 N2 Ag -7.93(12) . 2_777 Ag N1 N2 C1 -179.81(10) . . Ag N1 C8 C7 178.70(10) . . Ag N2 C1 C2 -169.88(10) 2_777 . N1 N2 C1 C2 1.0(2) . . N2 N1 C8 C7 -1.6(2) . . N2 C1 C2 C3 179.71(14) . . N2 C1 C2 C7 -1.3(2) . . C1 C2 C3 C4 179.23(14) . . C1 C2 C7 C6 -179.34(13) . . C1 C2 C7 C8 0.17(18) . . C2 C3 C4 C5 0.0(2) . . C2 C7 C8 N1 1.2(2) . . C3 C2 C7 C6 -0.3(2) . . C3 C2 C7 C8 179.24(13) . . C3 C4 C5 C6 -0.3(2) . . C4 C5 C6 C7 0.2(2) . . C5 C6 C7 C2 0.0(2) . . C5 C6 C7 C8 -179.45(13) . . C6 C7 C8 N1 -179.29(13) . . C7 C2 C3 C4 0.2(2) . . C8 N1 N2 Ag 172.31(10) . 2_777 C8 N1 N2 C1 0.44(19) . .