#------------------------------------------------------------------------------ #$Date: 2020-09-03 04:44:59 +0300 (Thu, 03 Sep 2020) $ #$Revision: 255815 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705334.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_7705334 loop_ _publ_author_name 'Li, Zili' 'Mackie , Emily R. R.' 'Ramkissoon , Pria' 'Mather , Joel' 'Wiratpruk, Nuchareenat' 'Soares da Costa, Tatiana P.' 'Barnard, Peter' _publ_section_title ; Synthesis, Conformational Analysis and Antibacterial Activity of Au(I)-Ag(I) and Au(I)-Hg(II) Heterobimetallic N-Heterocyclic Carbene Complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02225J _journal_year 2020 _chemical_formula_moiety '2(B F4), C20 H26 Ag Au N8' _chemical_formula_sum 'C20 H26 Ag Au B2 F8 N8' _chemical_formula_weight 856.94 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-11-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-06-21 deposited with the CCDC. 2020-09-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.4520(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.49130(10) _cell_length_b 14.38060(10) _cell_length_c 17.91910(10) _cell_measurement_reflns_used 26541 _cell_measurement_temperature 149.99(10) _cell_measurement_theta_max 71.0800 _cell_measurement_theta_min 3.6310 _cell_volume 3334.20(4) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 149.99(10) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0094 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 33825 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.256 _diffrn_reflns_theta_min 4.008 _exptl_absorpt_coefficient_mu 13.480 _exptl_absorpt_correction_T_max 0.96899 _exptl_absorpt_correction_T_min 0.96899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.707 _exptl_crystal_description block _exptl_crystal_F_000 1640 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.618 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 201 _refine_ls_number_reflns 3241 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.106 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0217 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+7.0971P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.0595 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3185 _reflns_number_total 3241 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; pjbsn090.res created by SHELXL-2014/7 TITL pjbsn090_a.res in I2/a REM Old TITL PJBSN090 in I2/a REM SHELXT solution in I2/a REM R1 0.112, Rweak 0.014, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C26 B2 N7 F4 Ag2 CELL 1.54184 13.4913 14.3806 17.9191 90 106.452 90 ZERR 4 0.0001 0.0001 0.0001 0 0.001 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Ag Au B F N UNIT 80 104 4 4 8 32 32 DFIX 1.5 C11 C10 C9 C8 L.S. 4 PLAN 10 SIZE 0.04 0.04 0.02 TEMP -123.16(10) list 4 ABIN fmap 2 53 ACTA REM REM REM WGHT 0.031300 7.097100 FVAR 0.17897 B1 5 0.611680 0.438731 0.288248 11.00000 0.04231 0.05045 = 0.05088 0.01150 0.00770 -0.00861 F1 6 0.597879 0.440092 0.211144 11.00000 0.25393 0.08119 = 0.05746 0.00964 0.03449 -0.02027 F2 6 0.520247 0.468337 0.301656 11.00000 0.05804 0.12549 = 0.16645 0.05528 0.03898 0.01661 F3 6 0.633837 0.349598 0.318884 11.00000 0.06301 0.04621 = 0.06466 0.00758 0.01169 -0.01238 F4 6 0.686398 0.498543 0.324707 11.00000 0.06946 0.05124 = 0.11801 0.00633 -0.01985 -0.01683 C1 1 0.723135 0.749759 0.623921 11.00000 0.03458 0.04212 = 0.04644 -0.00365 0.00615 -0.00180 N1 7 0.637378 0.702189 0.624915 11.00000 0.03527 0.03890 = 0.04200 -0.00418 0.00650 -0.00264 PART 1 AG1 3 0.842931 0.705961 0.577153 10.50000 0.02659 0.05004 = 0.04869 -0.00690 0.00589 -0.00339 PART 0 PART 2 AU1 4 0.839932 0.706090 0.582491 10.50000 0.03078 0.03632 = 0.04503 -0.00230 0.00872 0.00081 PART 0 C2 1 0.577725 0.752300 0.662108 11.00000 0.04132 0.05045 = 0.05435 -0.00559 0.01536 -0.00334 AFIX 43 H2 2 0.513551 0.733934 0.669547 11.00000 -1.20000 AFIX 0 N2 7 0.717684 0.829217 0.662356 11.00000 0.04266 0.04181 = 0.06189 -0.01197 0.01445 -0.00771 C3 1 0.628656 0.831969 0.685538 11.00000 0.04921 0.04888 = 0.06360 -0.01467 0.02173 -0.00438 AFIX 43 H3 2 0.607379 0.881077 0.712961 11.00000 -1.20000 AFIX 0 N3 7 0.522630 0.624706 0.516493 11.00000 0.03134 0.03650 = 0.04716 -0.00513 0.00718 -0.00220 C4 1 0.530405 0.662418 0.449653 11.00000 0.03333 0.03906 = 0.05176 -0.00245 0.00617 -0.00117 N4 7 0.432579 0.665662 0.403056 11.00000 0.03292 0.05841 = 0.05134 0.00130 0.00353 -0.00427 C5 1 0.420655 0.604141 0.512106 11.00000 0.03623 0.05071 = 0.05676 -0.00747 0.01217 -0.00964 AFIX 43 H5 2 0.395575 0.577492 0.551762 11.00000 -1.20000 AFIX 0 C6 1 0.364767 0.629439 0.440710 11.00000 0.03327 0.06440 = 0.05986 -0.00632 0.00881 -0.00794 AFIX 43 H6 2 0.292019 0.623600 0.419777 11.00000 -1.20000 AFIX 0 C7 1 0.608667 0.613191 0.586573 11.00000 0.03662 0.03487 = 0.04915 -0.00100 0.00521 -0.00240 AFIX 23 H7A 2 0.588631 0.569617 0.622552 11.00000 -1.20000 H7B 2 0.668635 0.586368 0.572639 11.00000 -1.20000 AFIX 0 C8 1 0.794548 0.903586 0.676200 11.00000 0.05807 0.05041 = 0.09698 -0.02382 0.03037 -0.02023 AFIX 23 H8A 2 0.792136 0.937226 0.723857 11.00000 -1.20000 H8B 2 0.863717 0.874563 0.687024 11.00000 -1.20000 AFIX 0 C9 1 0.785779 0.965581 0.620021 10.50000 0.09656 0.08852 = 0.06628 0.00842 0.00723 -0.04161 AFIX 137 H9A 2 0.785919 0.933639 0.571741 10.50000 -1.50000 H9B 2 0.844048 1.009030 0.634670 10.50000 -1.50000 H9C 2 0.720883 0.999938 0.612092 10.50000 -1.50000 AFIX 0 C10 1 0.402054 0.702444 0.323376 11.00000 0.04176 0.11500 = 0.05595 0.01860 -0.00062 -0.00900 AFIX 23 H10A 2 0.341210 0.743065 0.318111 11.00000 -1.20000 H10B 2 0.458955 0.742594 0.317454 11.00000 -1.20000 AFIX 0 C11 1 0.378669 0.642455 0.263373 10.50000 0.05606 0.05044 = 0.05777 -0.00232 0.02181 -0.00496 AFIX 137 H11A 2 0.362697 0.677107 0.214310 10.50000 -1.50000 H11B 2 0.318539 0.605228 0.265159 10.50000 -1.50000 H11C 2 0.437725 0.601302 0.266916 10.50000 -1.50000 AFIX 0 HKLF 4 REM pjbsn090_a.res in I2/a REM R1 = 0.0217 for 3185 Fo > 4sig(Fo) and 0.0220 for all 3241 data REM 201 parameters refined using 2 restraints END WGHT 0.0313 7.0980 REM Highest difference peak 0.618, deepest hole -0.539, 1-sigma level 0.072 Q1 1 0.5273 0.4411 0.2459 11.00000 0.05 0.62 Q2 1 0.6843 0.4331 0.2434 11.00000 0.05 0.60 Q3 1 0.5880 0.4943 0.3435 11.00000 0.05 0.42 Q4 1 0.8535 0.7007 0.6362 11.00000 0.05 0.35 Q5 1 0.8137 0.7002 0.6270 11.00000 0.05 0.34 Q6 1 0.8175 0.7154 0.5242 11.00000 0.05 0.27 Q7 1 0.8471 0.7950 0.5772 11.00000 0.05 0.24 Q8 1 0.8709 0.7831 0.5846 11.00000 0.05 0.23 Q9 1 0.8151 0.9202 0.6251 11.00000 0.05 0.23 Q10 1 0.8559 0.7043 0.5372 11.00000 0.05 0.22 REM The information below was added by Olex2. REM REM R1 = 0.0217 for 3185 Fo > 4sig(Fo) and 0.0220 for all 34622 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.62, deepest hole -0.54 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0220 REM R1_gt = 0.0217 REM wR_ref = 0.0595 REM GOOF = 1.084 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 34622 REM Reflections_gt = 3185 REM Parameters = n/a REM Hole = -0.54 REM Peak = 0.62 REM Flack = n/a ; _cod_data_source_file d0dt02225j2.cif _cod_data_source_block 5b _cod_database_code 7705334 _shelx_shelxl_version_number 2014/7 _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 0.774 _shelx_estimated_absorpt_t_min 0.615 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C11-C10 = C9-C8 1.5 with sigma of 0.02 3. Others Fixed Sof: Ag1(0.5) Au1(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) 4.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6) 4.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C11(H11A,H11B,H11C) ; _shelx_fab_file ; 0 0 -20 -1.2655 3.6187 0 0 -18 -1.2483 6.1316 0 0 -16 -0.4558 3.7901 0 0 -14 1.0497 -4.3151 0 0 -12 4.5616 -11.2372 0 0 -10 11.7483 -7.4158 0 0 -8 23.6394 5.8404 0 0 -6 43.8413 14.4711 0 0 -4 76.6514 10.3138 0 0 -2 113.4433 2.4000 0 1 -21 0.4988 -0.6128 0 1 -19 0.7277 -3.0472 0 1 -17 0.5068 -4.2800 0 1 -15 -0.6614 -1.1226 0 1 -13 -3.1606 5.2245 0 1 -11 -7.6286 7.8528 0 1 -9 -15.3488 2.0235 0 1 -7 -28.6684 -7.0093 0 1 -5 -50.2940 -9.8584 0 1 -3 -77.7825 -5.6641 0 1 -1 -98.5871 -1.2429 0 2 -20 0.2948 -0.6508 0 2 -18 0.1694 0.6652 0 2 -16 0.6319 1.7036 0 2 -14 2.6761 0.6005 0 2 -12 5.3408 -1.7509 0 2 -10 8.3220 -2.6826 0 2 -8 14.3462 -1.1234 0 2 -6 24.5045 1.7622 0 2 -4 34.0825 3.6360 0 2 -2 38.4194 2.3392 0 2 0 39.0547 -1.4457 0 3 -19 -0.4397 1.0772 0 3 -17 -0.6067 0.4889 0 3 -15 -1.6995 -0.1306 0 3 -13 -3.4586 -0.5166 0 3 -11 -4.3775 -0.5577 0 3 -9 -5.3657 0.3036 0 3 -7 -8.3502 1.3581 0 3 -5 -9.1330 0.7954 0 3 -3 -1.4968 -0.3930 0 3 -1 8.8919 0.6910 0 4 -20 0.0947 -0.4783 0 4 -18 0.4245 -0.4627 0 4 -16 1.0146 -0.5218 0 4 -14 1.8875 -0.2713 0 4 -12 2.5611 0.4611 0 4 -10 2.5238 0.7801 0 4 -8 2.4236 0.0766 0 4 -6 1.3089 -0.7214 0 4 -4 -5.0507 -0.6241 0 4 -2 -16.1971 -0.2736 0 4 0 -22.1976 -0.4689 0 5 -19 -0.2686 -0.0996 0 5 -17 -0.5861 -0.0437 0 5 -15 -1.0855 0.0117 0 5 -13 -1.7678 -0.1395 0 5 -11 -2.2450 -0.1218 0 5 -9 -2.2189 0.1508 0 5 -7 -1.5536 0.1018 0 5 -5 0.3575 -0.2616 0 5 -3 3.7103 -0.3993 0 5 -1 6.6594 -0.2869 0 6 -18 0.2446 0.2448 0 6 -16 0.3921 0.0162 0 6 -14 0.9579 -0.0074 0 6 -12 1.4141 0.1102 0 6 -10 1.6578 0.0495 0 6 -8 1.9102 -0.0184 0 6 -6 2.2622 0.2192 0 6 -4 3.7702 0.3693 0 6 -2 6.8231 0.1520 0 6 0 8.5975 -0.0707 0 7 -19 -0.0623 -0.4856 0 7 -17 -0.0588 0.0165 0 7 -15 -0.1816 0.3070 0 7 -13 -0.0121 0.1784 0 7 -11 0.3028 -0.2550 0 7 -9 -0.0068 -0.4870 0 7 -7 -0.8124 -0.2479 0 7 -5 -2.5122 0.1446 0 7 -3 -6.5235 0.2383 0 7 -1 -10.8989 -0.1298 0 8 -18 0.2182 -0.1919 0 8 -16 0.2682 -0.5913 0 8 -14 -0.3518 -0.2519 0 8 -12 -1.1596 0.1579 0 8 -10 -1.3827 0.2578 0 8 -8 -1.1459 0.1419 0 8 -6 -0.5781 -0.1784 0 8 -4 1.1449 -0.4447 0 8 -2 3.8954 -0.1198 0 8 0 5.3450 0.6785 0 9 -17 -0.5289 1.2820 0 9 -15 -0.1584 0.9468 0 9 -13 0.1872 -0.1019 0 9 -11 0.3211 -0.4502 0 9 -9 0.9817 -0.2470 0 9 -7 1.6416 -0.0110 0 9 -5 1.3973 0.4322 0 9 -3 1.2822 0.8119 0 9 -1 1.8998 0.4498 0 10 -16 0.1551 -1.1018 0 10 -14 0.4373 -0.4108 0 10 -12 1.2122 0.3618 0 10 -10 0.7254 0.6914 0 10 -8 -0.8888 0.5842 0 10 -6 -1.5172 -0.0251 0 10 -4 -1.9681 -0.7977 0 10 -2 -4.1974 -0.9112 0 10 0 -5.8127 -0.2035 0 11 -15 -0.1428 -0.2133 0 11 -13 -0.9056 -0.1398 0 11 -11 -1.1485 -0.2906 0 11 -9 -0.2287 -0.5494 0 11 -7 0.7057 -0.3195 0 11 -5 1.3536 0.2180 0 11 -3 2.9509 0.3229 0 11 -1 4.9361 -0.1062 0 12 -14 0.2551 0.3805 0 12 -12 -0.0675 0.0996 0 12 -10 -0.2680 0.1761 0 12 -8 -0.0742 0.2264 0 12 -6 -0.4408 -0.0325 0 12 -4 -1.5983 -0.2012 0 12 -2 -2.3960 -0.0272 0 12 0 -2.5380 0.2444 0 13 -13 0.2822 0.0112 0 13 -11 1.1137 -0.1855 0 13 -9 0.7804 -0.3513 0 13 -7 0.1788 -0.1403 0 13 -5 0.6255 0.3328 0 13 -3 1.0659 0.4363 0 13 -1 0.6934 0.0880 0 14 -12 -0.4115 0.0381 0 14 -10 -0.8943 0.2807 0 14 -8 -0.7678 0.3731 0 14 -6 -0.5786 0.0097 0 14 -4 -0.6039 -0.1599 0 14 -2 -0.5646 0.3868 0 14 0 -0.4902 0.6666 0 15 -11 0.0124 -0.0845 0 15 -9 0.3168 -0.0761 0 15 -7 0.6463 -0.1734 0 15 -5 0.6844 -0.2861 0 15 -3 0.7145 -0.5337 0 15 -1 0.9555 -0.5889 0 16 -8 0.1558 -0.5124 0 16 -6 -0.3042 0.3006 0 16 -4 -0.6869 0.6107 0 16 -2 -0.9411 -0.4897 0 16 0 -1.0605 -1.4938 0 17 -5 0.1347 -0.9383 0 17 -3 0.6473 -0.1418 0 17 -1 0.8418 2.0492 1 1 -20 -0.5398 0.8423 1 1 -18 -0.8300 0.7937 1 1 -16 -1.4195 -0.7622 1 1 -14 -2.1399 -2.7922 1 1 -12 -2.5041 -2.7931 1 1 -10 -2.8664 0.7611 1 1 -8 -2.8489 5.0237 1 1 -6 1.8385 4.4120 1 1 -4 15.8349 -1.2634 1 1 -2 33.7235 -4.5424 1 1 0 40.9592 -1.0472 1 1 2 31.9938 3.3352 1 1 4 18.0185 1.9673 1 1 6 10.0586 -2.5045 1 1 8 6.5634 -3.7210 1 1 10 3.1327 -1.0030 1 1 12 0.8792 1.8552 1 1 14 0.7269 2.3896 1 1 16 0.5148 0.8524 1 1 18 -0.3371 -1.1156 1 1 20 -0.4853 -1.8025 1 2 -21 0.4273 -0.0190 1 2 -19 0.9145 -0.3512 1 2 -17 1.6800 -0.2714 1 2 -15 2.4765 0.5067 1 2 -13 2.8206 1.4886 1 2 -11 3.0872 1.1830 1 2 -9 3.6800 -1.1380 1 2 -7 1.7159 -2.9970 1 2 -5 -9.1341 -1.1236 1 2 -3 -29.5329 2.5161 1 2 -1 -46.8241 2.3461 1 2 1 -47.0396 -1.5257 1 2 3 -33.3173 -2.8700 1 2 5 -20.0305 0.3048 1 2 7 -12.7835 3.1015 1 2 9 -7.6939 2.2040 1 2 11 -3.6191 -0.4059 1 2 13 -2.1144 -1.8996 1 2 15 -1.7384 -1.4818 1 2 17 -0.7963 0.0820 1 2 19 -0.1353 1.2137 1 3 -20 -0.6503 -0.3158 1 3 -18 -1.2776 -0.3550 1 3 -16 -1.9709 0.2035 1 3 -14 -2.1697 0.7561 1 3 -12 -1.9993 0.5703 1 3 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10 -10 0.8476 0.8589 12 10 -8 0.7109 1.9060 12 10 -6 0.1785 1.1360 12 10 -4 0.0296 -0.9891 12 10 -2 0.3573 -1.8275 12 10 0 0.4130 -1.3788 12 10 2 -0.0959 -1.8420 12 11 -9 -0.6393 -0.8298 12 11 -7 -0.8102 -1.8036 12 11 -5 -1.4497 -0.9975 12 11 -3 -2.0788 0.5781 12 11 -1 -1.7785 1.1949 12 11 1 -0.7678 1.0947 12 12 -6 1.3623 0.7628 12 12 -4 2.0263 1.3195 12 12 -2 1.9566 0.9793 13 1 -16 -0.3089 -0.9049 13 1 -14 -0.4546 -3.0546 13 1 -12 -0.4521 -1.4235 13 1 -10 -0.4207 2.7836 13 1 -8 -0.3488 4.4247 13 1 -6 -0.3244 1.4641 13 1 -4 -0.6615 -2.7170 13 1 -2 -0.9931 -4.1563 13 1 0 -0.5901 -2.0684 13 1 2 0.1027 1.4651 13 1 4 0.1862 3.3387 13 1 6 -0.0557 2.2688 13 1 8 -0.0558 0.2119 13 2 -17 0.0353 1.1216 13 2 -15 0.0176 2.8154 13 2 -13 0.0443 2.4887 13 2 -11 0.3394 -0.0838 13 2 -9 0.7714 -2.4561 13 2 -7 0.8791 -2.1751 13 2 -5 0.7619 0.3554 13 2 -3 0.8436 2.3009 13 2 -1 0.8080 1.8454 13 2 1 0.2870 0.1375 13 2 3 -0.2065 -0.9742 13 2 5 -0.2687 -1.2808 13 2 7 -0.1626 -1.1876 13 3 -16 0.5279 -0.8244 13 3 -14 0.7031 -0.4509 13 3 -12 0.4031 -0.1506 13 3 -10 -0.2219 -0.1026 13 3 -8 -0.8107 0.2446 13 3 -6 -1.0404 0.5901 13 3 -4 -0.7395 0.2865 13 3 -2 -0.1548 -0.0907 13 3 0 0.2272 -0.1658 13 3 2 0.3347 -0.6135 13 3 4 0.4426 -0.9056 13 3 6 0.5062 0.1190 13 4 -17 -0.4817 -0.2400 13 4 -15 -0.6743 -0.4056 13 4 -13 -0.4332 -0.6088 13 4 -11 -0.2519 -0.6416 13 4 -9 -0.2903 -0.7182 13 4 -7 0.2010 -0.7636 13 4 -5 0.9603 -0.0300 13 4 -3 0.6182 1.1729 13 4 -1 -0.6346 1.1758 13 4 1 -1.2247 -0.1543 13 4 3 -0.8798 -0.9180 13 4 5 -0.4787 -0.4844 13 4 7 -0.2829 -0.0933 13 5 -16 0.2308 0.1972 13 5 -14 -0.0536 0.2107 13 5 -12 -0.2557 0.6606 13 5 -10 0.3205 0.9455 13 5 -8 0.8363 0.5042 13 5 -6 0.1106 -0.4098 13 5 -4 -0.8228 -1.2608 13 5 -2 -0.3176 -1.3667 13 5 0 0.9096 -0.0037 13 5 2 1.1887 1.9201 13 5 4 0.5548 2.0056 13 5 6 0.0279 0.0657 13 6 -15 -0.0008 0.5474 13 6 -13 0.2018 -0.1108 13 6 -11 0.2203 -0.1403 13 6 -9 -0.2072 0.8636 13 6 -7 -0.6613 1.5490 13 6 -5 -0.5890 0.6752 13 6 -3 -0.1735 -0.6875 13 6 -1 0.0002 -0.9293 13 6 1 -0.1122 -0.6253 13 6 3 -0.1347 -0.8073 13 6 5 0.0015 -0.6806 13 7 -14 0.5313 -0.4353 13 7 -12 0.3633 0.1060 13 7 -10 -0.1543 -0.7379 13 7 -8 -0.1240 -1.7407 13 7 -6 0.9095 -1.1714 13 7 -4 1.6682 0.6702 13 7 -2 0.9685 1.4956 13 7 0 -0.3056 0.2673 13 7 2 -0.7504 -0.8930 13 7 4 -0.3948 -0.0473 13 8 -13 -0.8487 -0.6857 13 8 -11 -0.5090 -0.5903 13 8 -9 -0.0143 0.2170 13 8 -7 -0.3080 0.7991 13 8 -5 -1.2559 0.6652 13 8 -3 -1.4868 0.0003 13 8 -1 -0.5785 -0.2273 13 8 1 0.3602 0.5078 13 8 3 0.5554 0.8711 13 9 -12 0.5141 1.5477 13 9 -10 0.5778 1.3098 13 9 -8 0.6051 0.7971 13 9 -6 0.5016 -0.2592 13 9 -4 0.3306 -1.2314 13 9 -2 0.2748 -0.9949 13 9 0 0.2785 -0.1768 13 9 2 0.1295 -0.4429 13 10 -9 -0.7090 -1.9747 13 10 -7 -0.5972 -1.7087 13 10 -5 0.0519 0.3681 13 10 -3 0.3671 2.3788 13 10 -1 0.0031 2.0662 14 0 -16 0.1530 2.3725 14 0 -14 0.4067 1.3671 14 0 -12 -0.0883 -2.2022 14 0 -10 -1.0370 -5.0171 14 0 -8 -1.3665 -3.2153 14 0 -6 -0.6454 2.2981 14 0 -4 0.2875 5.9698 14 0 -2 0.4054 3.6615 14 0 0 0.0949 -2.4140 14 0 2 0.4435 -5.9838 14 0 4 1.0008 -4.1564 14 1 -15 0.1109 0.1853 14 1 -13 0.1239 1.8296 14 1 -11 0.5687 2.5170 14 1 -9 1.0400 1.5143 14 1 -7 0.9192 -0.7117 14 1 -5 0.2989 -3.0258 14 1 -3 -0.0654 -3.0458 14 1 -1 0.1016 0.2265 14 1 1 0.1581 3.0846 14 1 3 -0.1914 1.8510 14 1 5 -0.2716 -0.9786 14 2 -16 -0.5662 -1.9186 14 2 -14 -0.5825 -2.4692 14 2 -12 -0.4215 -0.7166 14 2 -10 -0.4628 1.8037 14 2 -8 -0.5680 1.9046 14 2 -6 -0.4687 -0.1498 14 2 -4 -0.4151 -1.3534 14 2 -2 -0.5894 -1.0393 14 2 0 -0.7316 -0.3554 14 2 2 -0.7530 0.7083 14 2 4 -0.7556 1.7080 14 3 -15 0.1575 1.0216 14 3 -13 -0.0432 -0.1770 14 3 -11 0.0026 -1.4556 14 3 -9 0.3324 -1.3683 14 3 -7 0.3203 0.4343 14 3 -5 0.1219 2.1446 14 3 -3 0.3802 1.7005 14 3 -1 0.7991 -0.2500 14 3 1 0.8841 -1.1093 14 3 3 0.8693 -0.0497 14 3 5 0.7955 1.0940 14 4 -14 0.7620 1.6058 14 4 -12 0.6294 1.1937 14 4 -10 -0.0127 -0.0843 14 4 -8 -0.4360 -0.7392 14 4 -6 -0.2022 -0.9135 14 4 -4 0.0050 -1.1375 14 4 -2 -0.2273 -0.4867 14 4 0 -0.4026 0.7164 14 4 2 -0.3473 0.2037 14 4 4 -0.3583 -1.6994 14 5 -13 -0.6010 -0.7184 14 5 -11 -0.3424 0.1565 14 5 -9 0.0681 0.3356 14 5 -7 0.4715 -0.1953 14 5 -5 0.6336 0.0691 14 5 -3 0.4044 1.0185 14 5 -1 0.0050 0.5711 14 5 1 -0.1362 -1.0625 14 5 3 0.0893 -1.2950 14 6 -12 0.0594 -0.8771 14 6 -10 0.3334 -0.1844 14 6 -8 0.0644 0.5509 14 6 -6 -0.8019 0.8535 14 6 -4 -1.1507 0.4304 14 6 -2 -0.5067 -0.2476 14 6 0 0.1066 0.2444 14 6 2 -0.0320 1.8701 14 7 -11 -0.2893 0.5035 14 7 -9 -0.4192 -0.2118 14 7 -7 0.1043 -0.2277 14 7 -5 0.6986 -0.4704 14 7 -3 0.6260 -0.6446 14 7 -1 0.2283 0.0241 14 7 1 0.1766 0.2700 14 8 -10 0.3901 0.4368 14 8 -8 0.0896 -0.3126 14 8 -6 -0.0654 -1.5361 14 8 -4 0.0557 -1.5664 14 8 -2 0.1062 -0.8845 14 8 0 -0.0835 -1.0058 14 9 -7 0.1129 1.6720 14 9 -5 -0.0356 3.3554 14 9 -3 -0.3074 2.7613 15 1 -14 0.2677 2.5704 15 1 -12 0.0050 -0.5670 15 1 -10 -0.4370 -3.0666 15 1 -8 -0.7088 -1.6497 15 1 -6 -0.5628 1.6945 15 1 -4 -0.2105 2.9921 15 1 -2 -0.0676 2.0069 15 1 0 -0.0316 0.4289 15 1 2 0.2326 -1.1620 15 2 -13 0.2009 1.5039 15 2 -11 0.4760 2.7604 15 2 -9 0.8592 2.4280 15 2 -7 1.1920 0.5005 15 2 -5 1.0445 -1.7878 15 2 -3 0.5176 -2.0744 15 2 -1 0.2104 0.5372 15 2 1 0.1711 3.2173 15 3 -12 -0.6492 -0.8856 15 3 -10 -0.5977 0.1851 15 3 -8 -0.8138 -0.4482 15 3 -6 -1.2295 -1.0964 15 3 -4 -1.1267 0.0016 15 3 -2 -0.4875 0.2587 15 3 0 -0.1343 -1.8917 15 3 2 -0.3008 -3.0409 15 4 -13 0.5148 -0.2492 15 4 -11 0.6636 -1.3464 15 4 -9 0.3965 -1.3885 15 4 -7 0.2795 -0.2187 15 4 -5 0.5545 0.2125 15 4 -3 0.5625 -0.4847 15 4 -1 0.0058 -0.3647 15 4 1 -0.3712 0.8316 15 5 -12 -0.6127 0.4495 15 5 -10 -0.7622 0.5015 15 5 -8 -0.1132 1.2532 15 5 -6 0.3339 1.5371 15 5 -4 0.0257 0.7431 15 5 -2 -0.1027 0.3533 15 5 0 0.4649 1.0085 15 6 -11 0.8632 1.7555 15 6 -9 0.7117 0.7468 15 6 -7 0.0533 -1.3647 15 6 -5 -0.1345 -1.6656 15 6 -3 0.1716 -0.2336 15 6 -1 0.1198 -0.2295 15 7 -8 -0.4933 -0.4251 15 7 -6 -0.3666 1.6284 15 7 -4 -0.3735 1.7301 16 0 -10 -0.4428 -0.3314 16 0 -8 -0.5165 -2.9079 16 0 -6 -0.3138 -4.5352 16 0 -4 -0.1777 -2.5849 16 0 -2 -0.2859 0.0102 16 1 -11 0.2811 0.0854 16 1 -9 0.5614 -0.1640 16 1 -7 0.4021 -1.1180 16 1 -5 0.1125 -0.9471 16 1 -3 0.1103 -0.0365 16 1 -1 0.2458 -0.4017 16 2 -10 -0.5360 -1.3965 16 2 -8 -0.6955 1.4585 16 2 -6 -0.3174 3.6931 16 2 -4 -0.0205 1.7470 16 2 -2 -0.0765 -0.7889 16 3 -9 0.7521 1.8018 16 3 -7 0.9225 1.0361 16 3 -5 0.5383 0.8836 16 3 -3 0.2028 1.6261 16 4 -8 -0.7281 -3.5420 16 4 -6 -1.0109 -5.0834 16 4 -4 -0.6731 -3.5176 0 0 0 0.0 0.0 ; _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop in perfluoroether oil' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.6117(3) 0.4387(3) 0.2882(2) 0.0490(8) Uani 1 1 d . . . . . F1 F 0.5979(4) 0.4401(2) 0.21114(16) 0.1328(15) Uani 1 1 d . . . . . F2 F 0.5202(2) 0.4683(2) 0.3017(2) 0.1152(12) Uani 1 1 d . . . . . F3 F 0.63384(16) 0.34960(13) 0.31888(12) 0.0593(5) Uani 1 1 d . . . . . F4 F 0.68640(19) 0.49854(16) 0.32471(17) 0.0891(8) Uani 1 1 d . . . . . C1 C 0.7231(2) 0.7498(2) 0.62392(17) 0.0421(6) Uani 1 1 d . . . . . N1 N 0.63738(19) 0.70219(15) 0.62491(15) 0.0396(5) Uani 1 1 d . . . . . Ag1 Ag 0.8429(4) 0.7060(3) 0.5772(4) 0.0428(10) Uani 0.5 1 d . . P A 1 Au1 Au 0.8399(2) 0.70609(13) 0.5825(2) 0.0378(3) Uani 0.5 1 d . . P A 2 C2 C 0.5777(2) 0.7523(2) 0.66211(19) 0.0483(7) Uani 1 1 d . . . . . H2 H 0.5136 0.7339 0.6695 0.058 Uiso 1 1 calc R . . . . N2 N 0.7177(2) 0.82922(19) 0.66236(17) 0.0489(6) Uani 1 1 d . . . . . C3 C 0.6287(3) 0.8320(2) 0.6855(2) 0.0527(8) Uani 1 1 d . . . . . H3 H 0.6074 0.8811 0.7130 0.063 Uiso 1 1 calc R . . . . N3 N 0.52263(17) 0.62471(16) 0.51649(14) 0.0391(5) Uani 1 1 d . . . . . C4 C 0.5304(2) 0.6624(2) 0.44965(18) 0.0426(6) Uani 1 1 d . . . . . N4 N 0.43258(19) 0.6657(2) 0.40306(16) 0.0493(6) Uani 1 1 d . . . . . C5 C 0.4207(2) 0.6041(2) 0.51211(19) 0.0481(7) Uani 1 1 d . . . . . H5 H 0.3956 0.5775 0.5518 0.058 Uiso 1 1 calc R . . . . C6 C 0.3648(2) 0.6294(3) 0.4407(2) 0.0534(8) Uani 1 1 d . . . . . H6 H 0.2920 0.6236 0.4198 0.064 Uiso 1 1 calc R . . . . C7 C 0.6087(2) 0.61319(19) 0.58657(17) 0.0416(6) Uani 1 1 d . . . . . H7A H 0.5886 0.5696 0.6226 0.050 Uiso 1 1 calc R . . . . H7B H 0.6686 0.5864 0.5726 0.050 Uiso 1 1 calc R . . . . C8 C 0.7945(3) 0.9036(3) 0.6762(3) 0.0668(10) Uani 1 1 d D . . . . H8A H 0.7921 0.9372 0.7239 0.080 Uiso 1 1 calc R . . . . H8B H 0.8637 0.8746 0.6870 0.080 Uiso 1 1 calc R . . . . C9 C 0.7858(8) 0.9656(7) 0.6200(5) 0.087(3) Uani 0.5 1 d D . P . . H9A H 0.7859 0.9336 0.5717 0.131 Uiso 0.5 1 calc GR . P . . H9B H 0.8440 1.0090 0.6347 0.131 Uiso 0.5 1 calc GR . P . . H9C H 0.7209 0.9999 0.6121 0.131 Uiso 0.5 1 calc GR . P . . C10 C 0.4021(3) 0.7024(3) 0.3234(2) 0.0739(13) Uani 1 1 d D . . . . H10A H 0.3412 0.7431 0.3181 0.089 Uiso 1 1 calc R . . . . H10B H 0.4590 0.7426 0.3175 0.089 Uiso 1 1 calc R . . . . C11 C 0.3787(5) 0.6425(5) 0.2634(4) 0.0536(15) Uani 0.5 1 d D . P . . H11A H 0.3627 0.6771 0.2143 0.080 Uiso 0.5 1 calc GR . P . . H11B H 0.3185 0.6052 0.2652 0.080 Uiso 0.5 1 calc GR . P . . H11C H 0.4377 0.6013 0.2669 0.080 Uiso 0.5 1 calc GR . P . . 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 B1 0.0423(17) 0.0505(19) 0.0509(19) 0.0115(15) 0.0077(15) -0.0086(15) F1 0.254(5) 0.0812(19) 0.0575(15) 0.0096(13) 0.034(2) -0.020(2) F2 0.0580(15) 0.125(3) 0.166(3) 0.055(2) 0.0390(17) 0.0166(16) F3 0.0630(12) 0.0462(10) 0.0647(11) 0.0076(9) 0.0117(9) -0.0124(9) F4 0.0695(15) 0.0512(12) 0.118(2) 0.0063(13) -0.0199(14) -0.0168(11) C1 0.0346(14) 0.0421(15) 0.0464(15) -0.0036(12) 0.0062(11) -0.0018(12) N1 0.0353(12) 0.0389(13) 0.0420(13) -0.0042(9) 0.0065(10) -0.0026(9) Ag1 0.0266(7) 0.0500(15) 0.0487(13) -0.0069(6) 0.0059(7) -0.0034(6) Au1 0.0308(5) 0.0363(6) 0.0450(4) -0.0023(3) 0.0087(3) 0.0008(3) C2 0.0413(16) 0.0505(17) 0.0543(17) -0.0056(14) 0.0154(13) -0.0033(13) N2 0.0427(13) 0.0418(13) 0.0619(16) -0.0120(12) 0.0144(12) -0.0077(11) C3 0.0492(17) 0.0489(17) 0.064(2) -0.0147(15) 0.0217(15) -0.0044(14) N3 0.0313(11) 0.0365(11) 0.0472(13) -0.0051(10) 0.0072(9) -0.0022(9) C4 0.0333(14) 0.0391(14) 0.0518(16) -0.0024(12) 0.0062(12) -0.0012(11) N4 0.0329(12) 0.0584(16) 0.0513(14) 0.0013(12) 0.0035(10) -0.0043(11) C5 0.0362(14) 0.0507(17) 0.0568(17) -0.0075(14) 0.0122(13) -0.0096(13) C6 0.0333(14) 0.064(2) 0.0599(19) -0.0063(16) 0.0088(13) -0.0079(14) C7 0.0366(14) 0.0349(13) 0.0492(15) -0.0010(12) 0.0052(12) -0.0024(11) C8 0.058(2) 0.0504(19) 0.097(3) -0.0238(19) 0.030(2) -0.0202(16) C9 0.097(7) 0.089(6) 0.066(5) 0.008(5) 0.007(5) -0.042(5) C10 0.0418(19) 0.115(4) 0.056(2) 0.019(2) -0.0006(16) -0.0090(19) C11 0.056(4) 0.050(4) 0.058(4) -0.002(3) 0.022(3) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 B1 F2 107.6(4) . . ? F1 B1 F3 111.8(3) . . ? F1 B1 F4 110.9(3) . . ? F2 B1 F3 108.4(3) . . ? F4 B1 F2 107.5(4) . . ? F4 B1 F3 110.4(3) . . ? N1 C1 Ag1 127.5(2) . . ? N1 C1 Au1 127.4(2) . . ? N2 C1 N1 104.6(3) . . ? N2 C1 Ag1 127.8(2) . . ? N2 C1 Au1 127.7(2) . . ? C1 N1 C2 111.1(2) . . ? C1 N1 C7 123.8(3) . . ? C2 N1 C7 125.0(3) . . ? C1 Ag1 Ag1 80.8(2) . 2_656 ? C4 Ag1 C1 171.0(3) 2_656 . ? C4 Ag1 Ag1 108.0(4) 2_656 2_656 ? C1 Au1 Au1 82.84(14) . 2_656 ? C1 Au1 C4 174.6(2) . 2_656 ? C4 Au1 Au1 102.5(2) 2_656 2_656 ? C3 C2 N1 106.2(3) . . ? C1 N2 C3 110.9(3) . . ? C1 N2 C8 124.7(3) . . ? C3 N2 C8 124.4(3) . . ? C2 C3 N2 107.1(3) . . ? C4 N3 C5 111.2(2) . . ? C4 N3 C7 124.7(2) . . ? C5 N3 C7 124.0(3) . . ? N3 C4 Ag1 128.8(3) . 2_656 ? N3 C4 Au1 130.5(2) . 2_656 ? N3 C4 N4 104.8(2) . . ? N4 C4 Ag1 126.4(3) . 2_656 ? N4 C4 Au1 124.7(2) . 2_656 ? C4 N4 C6 110.6(3) . . ? C4 N4 C10 124.8(3) . . ? C6 N4 C10 124.6(3) . . ? C6 C5 N3 106.1(3) . . ? C5 C6 N4 107.3(3) . . ? N1 C7 N3 110.4(2) . . ? C9 C8 N2 117.2(5) . . ? C11 C10 N4 119.0(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 F1 1.341(5) . ? B1 F2 1.389(5) . ? B1 F3 1.393(4) . ? B1 F4 1.345(4) . ? C1 N1 1.349(4) . ? C1 Ag1 2.116(8) . ? C1 Au1 2.023(5) . ? C1 N2 1.347(4) . ? N1 C2 1.384(4) . ? N1 C7 1.452(3) . ? Ag1 Ag1 3.163(9) 2_656 ? Ag1 C4 2.002(7) 2_656 ? Au1 Au1 3.250(6) 2_656 ? Au1 C4 2.087(5) 2_656 ? C2 C3 1.341(5) . ? N2 C3 1.378(4) . ? N2 C8 1.461(4) . ? N3 C4 1.346(4) . ? N3 C5 1.387(4) . ? N3 C7 1.458(4) . ? C4 Ag1 2.002(7) 2_656 ? C4 Au1 2.087(5) 2_656 ? C4 N4 1.348(4) . ? N4 C6 1.383(4) . ? N4 C10 1.468(5) . ? C5 C6 1.338(5) . ? C8 C9 1.325(9) . ? C10 C11 1.344(7) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.368 0.000 0.500 318.6 81.1 ? 2 -0.869 0.500 0.000 318.6 81.1 ?