#------------------------------------------------------------------------------ #$Date: 2020-09-03 04:45:51 +0300 (Thu, 03 Sep 2020) $ #$Revision: 255816 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705338.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_7705338 loop_ _publ_author_name 'Petrovskii, Stanislav' 'Paderina, Aleksandra V.' 'Sizova, Anastasia' 'Baranov, Andrey' 'Artem'ev, Alexander' 'Sizov, Vladimir' 'Grachova, Elena V.' _publ_section_title ; Luminescent behaviour of Au(I)-Cu(I) heterobimetallic coordination polymers based on alkynyl-tris(2-pyridyl)phosphine Au(I) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02583F _journal_year 2020 _chemical_formula_moiety 'C30 H23 Au N3 O P' _chemical_formula_sum 'C30 H23 Au N3 O P' _chemical_formula_weight 669.46 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc25k7gg _audit_creation_date 2020-04-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-06-27 deposited with the CCDC. 2020-09-02 downloaded from the CCDC. ; _cell_angle_alpha 109.897(4) _cell_angle_beta 111.317(4) _cell_angle_gamma 100.110(4) _cell_formula_units_Z 2 _cell_length_a 10.4121(5) _cell_length_b 11.9530(5) _cell_length_c 12.0119(5) _cell_measurement_reflns_used 5088 _cell_measurement_temperature 100(11) _cell_measurement_theta_max 30.7410 _cell_measurement_theta_min 3.2290 _cell_volume 1230.75(12) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _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 100(11) _diffrn_detector_area_resol_mean 16.2096 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.875 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -81.00 2.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - -22.4241 -77.0000 30.0000 83 #__ type_ start__ end____ width___ exp.time_ 2 omega 65.00 93.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 77.0000 -30.0000 28 #__ type_ start__ end____ width___ exp.time_ 3 omega -44.00 38.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 -57.0000 90.0000 82 #__ type_ start__ end____ width___ exp.time_ 4 omega -7.00 42.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 77.0000 -30.0000 49 #__ type_ start__ end____ width___ exp.time_ 5 omega -24.00 64.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 -99.0000 -150.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega 42.00 81.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 57.0000 -30.0000 39 #__ type_ start__ end____ width___ exp.time_ 7 omega 56.00 92.00 1.0000 5.3700 omega____ theta____ kappa____ phi______ frames - 23.3616 57.0000 -120.0000 36 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0592347000 _diffrn_orient_matrix_UB_12 -0.0054877000 _diffrn_orient_matrix_UB_13 -0.0571349000 _diffrn_orient_matrix_UB_21 0.0114836000 _diffrn_orient_matrix_UB_22 -0.0521741000 _diffrn_orient_matrix_UB_23 -0.0406646000 _diffrn_orient_matrix_UB_31 -0.0491254000 _diffrn_orient_matrix_UB_32 -0.0419120000 _diffrn_orient_matrix_UB_33 0.0082497000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0602 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.875 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11477 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.875 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.892 _diffrn_reflns_theta_min 2.860 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.071 _exptl_absorpt_correction_T_max 0.807 _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) 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 1.809 _exptl_crystal_description needle _exptl_crystal_F_000 654 _exptl_crystal_size_max 0.302 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.037 _refine_diff_density_max 1.753 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.169 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 6807 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0300 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+0.0265P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.0620 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6282 _reflns_number_total 6807 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02583f3.cif _cod_data_source_block ps-002 _cod_original_cell_volume 1230.74(11) _cod_database_code 7705338 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'P1 Au1 C32 O1 N3' _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 0.807 _shelx_estimated_absorpt_t_min 0.261 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.51 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C16) = Uanis(C17) 3.a Aromatic/amide H refined with riding coordinates: C1(H1A), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30) 3.b Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; ps-002.res created by SHELXL-2014/7 TITL ps-002_a.res in P-1 REM Old TITL PS-002 in P1 REM SHELXT solution in P-1 REM R1 0.056, Rweak 0.013, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C61 N10 O10 P2 Au2 CELL 0.71073 10.412089 11.952963 12.011922 109.8972 111.317 100.1098 ZERR 2 0.000467 0.000525 0.000546 0.0041 0.0042 0.0037 LATT 1 SFAC C H Au N O P UNIT 60 48 2 6 2 2 EADP C16 C17 L.S. 20 PLAN 20 SIZE 0.302 0.254 0.037 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.014100 0.026500 FVAR 3.52352 AU1 3 0.350276 0.274405 0.629892 11.00000 0.00910 0.01041 = 0.00945 0.00586 0.00319 0.00302 P1 6 0.394582 0.203874 0.787759 11.00000 0.00720 0.00803 = 0.00849 0.00395 0.00295 0.00213 O1 5 0.360304 0.464807 0.283702 11.00000 0.00619 0.01612 = 0.01125 0.00565 0.00387 0.00217 AFIX 147 H1 2 0.439989 0.510387 0.348244 11.00000 -1.50000 AFIX 0 N1 4 0.121478 0.064382 0.681453 11.00000 0.00856 0.01175 = 0.01504 0.00249 0.00347 0.00213 N2 4 0.561989 0.294904 1.054836 11.00000 0.01140 0.01356 = 0.00945 0.00441 0.00148 0.00106 N3 4 0.503579 0.043766 0.662799 11.00000 0.01015 0.01166 = 0.00977 0.00377 0.00359 0.00114 C1 1 -0.004647 0.004886 0.673914 11.00000 0.00969 0.01360 = 0.02122 0.00238 0.00460 0.00227 AFIX 43 H1A 2 -0.082134 -0.049837 0.590389 11.00000 -1.20000 AFIX 0 C2 1 -0.024983 0.021501 0.786492 11.00000 0.01229 0.01265 = 0.03551 0.01159 0.01459 0.00454 AFIX 43 H2 2 -0.113867 -0.022322 0.777881 11.00000 -1.20000 AFIX 0 C3 1 0.087816 0.103180 0.909485 11.00000 0.01666 0.01910 = 0.02061 0.01278 0.01529 0.01124 AFIX 43 H3 2 0.076517 0.116001 0.985714 11.00000 -1.20000 AFIX 0 C4 1 0.219884 0.166957 0.919187 11.00000 0.01061 0.01190 = 0.01324 0.00615 0.00618 0.00453 AFIX 43 H4 2 0.298247 0.223785 1.001357 11.00000 -1.20000 AFIX 0 C5 1 0.230339 0.142774 0.802301 11.00000 0.00935 0.00734 = 0.01350 0.00495 0.00639 0.00362 C6 1 0.671487 0.378718 1.172814 11.00000 0.01903 0.01982 = 0.00768 0.00589 0.00067 0.00334 AFIX 43 H6 2 0.687784 0.361095 1.245473 11.00000 -1.20000 AFIX 0 C7 1 0.763040 0.491555 1.193182 11.00000 0.01119 0.01495 = 0.01253 0.00255 0.00116 0.00111 AFIX 43 H7 2 0.839186 0.547163 1.277144 11.00000 -1.20000 AFIX 0 C8 1 0.738406 0.518919 1.086529 11.00000 0.01530 0.00862 = 0.02122 0.00454 0.00978 0.00435 AFIX 43 H8 2 0.798120 0.593310 1.097112 11.00000 -1.20000 AFIX 0 C9 1 0.622706 0.433657 0.962288 11.00000 0.01277 0.00857 = 0.01749 0.00634 0.00931 0.00433 AFIX 43 H9 2 0.602248 0.450260 0.888631 11.00000 -1.20000 AFIX 0 C10 1 0.538656 0.322662 0.952077 11.00000 0.00590 0.01078 = 0.01261 0.00537 0.00518 0.00493 C11 1 0.550880 -0.055283 0.638167 11.00000 0.01229 0.01386 = 0.01473 0.00035 0.00804 0.00350 AFIX 43 H11 2 0.582590 -0.074266 0.573084 11.00000 -1.20000 AFIX 0 C12 1 0.555138 -0.130344 0.703697 11.00000 0.01077 0.01206 = 0.01606 0.00360 0.00373 0.00521 AFIX 43 H12 2 0.588893 -0.197947 0.682955 11.00000 -1.20000 AFIX 0 C13 1 0.508292 -0.103586 0.801174 11.00000 0.01346 0.01316 = 0.01627 0.00983 0.00418 0.00389 AFIX 43 H13 2 0.511556 -0.151708 0.848186 11.00000 -1.20000 AFIX 0 C14 1 0.456243 -0.002669 0.826684 11.00000 0.01081 0.01215 = 0.01184 0.00614 0.00582 0.00410 AFIX 43 H14 2 0.421654 0.016780 0.889720 11.00000 -1.20000 AFIX 0 C15 1 0.456986 0.067596 0.756917 11.00000 0.00514 0.00576 = 0.00762 0.00070 0.00124 0.00063 C16 1 0.311551 0.344990 0.497187 11.00000 0.00606 0.00846 = 0.00866 0.00118 0.00028 -0.00039 C17 1 0.288219 0.392730 0.422119 11.00000 0.00606 0.00846 = 0.00866 0.00118 0.00028 -0.00039 C18 1 0.249947 0.449034 0.327647 11.00000 0.00583 0.01032 = 0.00828 0.00415 0.00232 0.00113 C19 1 0.227241 0.574791 0.389920 11.00000 0.00673 0.00850 = 0.00692 0.00110 0.00074 0.00097 C20 1 0.156654 0.587464 0.470440 11.00000 0.01294 0.01121 = 0.01041 0.00476 0.00333 0.00210 AFIX 43 H20 2 0.133762 0.523353 0.494539 11.00000 -1.20000 AFIX 0 C21 1 0.120399 0.695211 0.514786 11.00000 0.01594 0.01728 = 0.01411 0.00382 0.00842 0.00621 AFIX 43 H21 2 0.074503 0.703433 0.569190 11.00000 -1.20000 AFIX 0 C22 1 0.153050 0.791175 0.477460 11.00000 0.01637 0.01189 = 0.01431 0.00142 0.00294 0.00554 AFIX 43 H22 2 0.127349 0.862674 0.505379 11.00000 -1.20000 AFIX 0 C23 1 0.223601 0.778830 0.398991 11.00000 0.02158 0.01050 = 0.01612 0.00655 0.00790 0.00446 AFIX 43 H23 2 0.245629 0.842690 0.374326 11.00000 -1.20000 AFIX 0 C24 1 0.262392 0.672465 0.356090 11.00000 0.01291 0.01244 = 0.01054 0.00415 0.00533 0.00216 AFIX 43 H24 2 0.311871 0.666431 0.304738 11.00000 -1.20000 AFIX 0 C25 1 0.106911 0.363422 0.201389 11.00000 0.00656 0.00890 = 0.00801 0.00110 0.00156 0.00285 C26 1 0.069555 0.390013 0.092450 11.00000 0.01513 0.00961 = 0.01346 0.00323 0.00352 0.00508 AFIX 43 H26 2 0.134735 0.457121 0.096481 11.00000 -1.20000 AFIX 0 C27 1 -0.060999 0.320066 -0.021295 11.00000 0.01766 0.01732 = 0.00972 0.00312 0.00133 0.01031 AFIX 43 H27 2 -0.082794 0.338303 -0.094015 11.00000 -1.20000 AFIX 0 C28 1 -0.160016 0.221784 -0.026319 11.00000 0.00704 0.01526 = 0.01479 -0.00464 -0.00151 0.00340 AFIX 43 H28 2 -0.249208 0.174556 -0.102494 11.00000 -1.20000 AFIX 0 C29 1 -0.127123 0.193877 0.080400 11.00000 0.00863 0.01209 = 0.02488 0.00097 0.00846 0.00109 AFIX 43 H29 2 -0.193834 0.127841 0.076369 11.00000 -1.20000 AFIX 0 C30 1 0.006472 0.264653 0.194938 11.00000 0.01681 0.01191 = 0.01133 0.00316 0.01024 0.00579 AFIX 43 H30 2 0.028526 0.245784 0.267265 11.00000 -1.20000 AFIX 0 HKLF 4 REM ps-002_a.res in P-1 REM R1 = 0.0300 for 6282 Fo > 4sig(Fo) and 0.0341 for all 6807 data REM 320 parameters refined using 0 restraints END WGHT 0.0141 0.0265 REM Highest difference peak 1.753, deepest hole -1.375, 1-sigma level 0.169 Q1 1 0.2886 0.2410 0.5475 11.00000 0.05 1.75 Q2 1 0.3871 0.3392 0.6210 11.00000 0.05 1.51 Q3 1 0.4071 0.2942 0.7103 11.00000 0.05 1.51 Q4 1 0.3013 0.2143 0.6428 11.00000 0.05 1.34 Q5 1 0.3124 0.3263 0.6896 11.00000 0.05 1.03 Q6 1 0.3952 0.2193 0.5896 11.00000 0.05 0.98 Q7 1 0.2982 0.3071 0.5332 11.00000 0.05 0.94 Q8 1 0.4148 0.2468 0.7064 11.00000 0.05 0.92 Q9 1 0.3594 0.1628 0.7908 11.00000 0.05 0.86 Q10 1 0.1751 0.4152 0.2649 11.00000 0.05 0.78 Q11 1 0.5785 0.3762 0.9535 11.00000 0.05 0.73 Q12 1 0.2979 0.0578 0.6363 11.00000 0.05 0.72 Q13 1 0.1536 0.1301 0.9035 11.00000 0.05 0.72 Q14 1 0.4659 0.3382 0.5843 11.00000 0.05 0.71 Q15 1 0.8030 0.5614 1.1660 11.00000 0.05 0.71 Q16 1 0.2265 0.7848 0.4652 11.00000 0.05 0.70 Q17 1 0.4797 0.5410 0.4204 11.00000 0.05 0.70 Q18 1 0.4239 0.1203 0.7862 11.00000 0.05 0.68 Q19 1 0.1677 0.1146 0.7436 11.00000 0.05 0.66 Q20 1 0.1001 0.6237 0.4716 11.00000 0.05 0.65 ; _shelx_res_checksum 98061 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.35028(2) 0.27441(2) 0.62989(2) 0.00959(4) Uani 1 1 d . . . . . P1 P 0.39458(9) 0.20387(8) 0.78776(9) 0.00809(17) Uani 1 1 d . . . . . O1 O 0.3603(3) 0.4648(2) 0.2837(3) 0.0116(5) Uani 1 1 d . . . . . H1 H 0.4400 0.5104 0.3482 0.017 Uiso 1 1 calc GR . . . . N1 N 0.1215(3) 0.0644(3) 0.6815(3) 0.0137(6) Uani 1 1 d . . . . . N2 N 0.5620(3) 0.2949(3) 1.0548(3) 0.0132(6) Uani 1 1 d . . . . . N3 N 0.5036(3) 0.0438(3) 0.6628(3) 0.0115(6) Uani 1 1 d . . . . . C1 C -0.0046(4) 0.0049(3) 0.6739(4) 0.0175(8) Uani 1 1 d . . . . . H1A H -0.0821 -0.0498 0.5904 0.021 Uiso 1 1 calc R . . . . C2 C -0.0250(4) 0.0215(3) 0.7865(4) 0.0186(9) Uani 1 1 d . . . . . H2 H -0.1139 -0.0223 0.7779 0.022 Uiso 1 1 calc R . . . . C3 C 0.0878(4) 0.1032(3) 0.9095(4) 0.0145(7) Uani 1 1 d . . . . . H3 H 0.0765 0.1160 0.9857 0.017 Uiso 1 1 calc R . . . . C4 C 0.2199(4) 0.1670(3) 0.9192(4) 0.0114(7) Uani 1 1 d . . . . . H4 H 0.2982 0.2238 1.0014 0.014 Uiso 1 1 calc R . . . . C5 C 0.2303(4) 0.1428(3) 0.8023(4) 0.0095(7) Uani 1 1 d . . . . . C6 C 0.6715(4) 0.3787(3) 1.1728(4) 0.0179(8) Uani 1 1 d . . . . . H6 H 0.6878 0.3611 1.2455 0.021 Uiso 1 1 calc R . . . . C7 C 0.7630(4) 0.4916(3) 1.1932(4) 0.0159(8) Uani 1 1 d . . . . . H7 H 0.8392 0.5472 1.2771 0.019 Uiso 1 1 calc R . . . . C8 C 0.7384(4) 0.5189(3) 1.0865(4) 0.0152(8) Uani 1 1 d . . . . . H8 H 0.7981 0.5933 1.0971 0.018 Uiso 1 1 calc R . . . . C9 C 0.6227(4) 0.4337(3) 0.9623(4) 0.0119(7) Uani 1 1 d . . . . . H9 H 0.6022 0.4503 0.8886 0.014 Uiso 1 1 calc R . . . . C10 C 0.5387(3) 0.3227(3) 0.9521(4) 0.0091(7) Uani 1 1 d . . . . . C11 C 0.5509(4) -0.0553(3) 0.6382(4) 0.0150(8) Uani 1 1 d . . . . . H11 H 0.5826 -0.0743 0.5731 0.018 Uiso 1 1 calc R . . . . C12 C 0.5551(4) -0.1303(3) 0.7037(4) 0.0144(8) Uani 1 1 d . . . . . H12 H 0.5889 -0.1979 0.6830 0.017 Uiso 1 1 calc R . . . . C13 C 0.5083(4) -0.1036(3) 0.8012(4) 0.0142(7) Uani 1 1 d . . . . . H13 H 0.5116 -0.1517 0.8482 0.017 Uiso 1 1 calc R . . . . C14 C 0.4562(4) -0.0027(3) 0.8267(4) 0.0111(7) Uani 1 1 d . . . . . H14 H 0.4217 0.0168 0.8897 0.013 Uiso 1 1 calc R . . . . C15 C 0.4570(3) 0.0676(3) 0.7569(3) 0.0076(6) Uani 1 1 d . . . . . C16 C 0.3116(4) 0.3450(3) 0.4972(4) 0.0100(5) Uani 1 1 d . . . . . C17 C 0.2882(4) 0.3927(3) 0.4221(4) 0.0100(5) Uani 1 1 d . . . . . C18 C 0.2499(3) 0.4490(3) 0.3276(3) 0.0087(7) Uani 1 1 d . . . . . C19 C 0.2272(4) 0.5748(3) 0.3899(3) 0.0091(7) Uani 1 1 d . . . . . C20 C 0.1567(4) 0.5875(3) 0.4704(4) 0.0125(7) Uani 1 1 d . . . . . H20 H 0.1338 0.5234 0.4945 0.015 Uiso 1 1 calc R . . . . C21 C 0.1204(4) 0.6952(3) 0.5148(4) 0.0161(8) Uani 1 1 d . . . . . H21 H 0.0745 0.7034 0.5692 0.019 Uiso 1 1 calc R . . . . C22 C 0.1531(4) 0.7912(3) 0.4775(4) 0.0168(8) Uani 1 1 d . . . . . H22 H 0.1273 0.8627 0.5054 0.020 Uiso 1 1 calc R . . . . C23 C 0.2236(4) 0.7788(3) 0.3990(4) 0.0163(8) Uani 1 1 d . . . . . H23 H 0.2456 0.8427 0.3743 0.020 Uiso 1 1 calc R . . . . C24 C 0.2624(4) 0.6725(3) 0.3561(4) 0.0126(7) Uani 1 1 d . . . . . H24 H 0.3119 0.6664 0.3047 0.015 Uiso 1 1 calc R . . . . C25 C 0.1069(4) 0.3634(3) 0.2014(3) 0.0092(7) Uani 1 1 d . . . . . C26 C 0.0696(4) 0.3900(3) 0.0924(4) 0.0142(7) Uani 1 1 d . . . . . H26 H 0.1347 0.4571 0.0965 0.017 Uiso 1 1 calc R . . . . C27 C -0.0610(4) 0.3201(3) -0.0213(4) 0.0167(8) Uani 1 1 d . . . . . H27 H -0.0828 0.3383 -0.0940 0.020 Uiso 1 1 calc R . . . . C28 C -0.1600(4) 0.2218(3) -0.0263(4) 0.0180(8) Uani 1 1 d . . . . . H28 H -0.2492 0.1746 -0.1025 0.022 Uiso 1 1 calc R . . . . C29 C -0.1271(4) 0.1939(3) 0.0804(4) 0.0175(8) Uani 1 1 d . . . . . H29 H -0.1938 0.1278 0.0764 0.021 Uiso 1 1 calc R . . . . C30 C 0.0065(4) 0.2647(3) 0.1949(4) 0.0126(7) Uani 1 1 d . . . . . H30 H 0.0285 0.2458 0.2673 0.015 Uiso 1 1 calc R . . . . 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 Au1 0.00910(7) 0.01041(7) 0.00945(7) 0.00586(5) 0.00319(5) 0.00302(5) P1 0.0072(4) 0.0080(4) 0.0085(4) 0.0039(3) 0.0030(4) 0.0021(3) O1 0.0062(11) 0.0161(12) 0.0113(13) 0.0056(10) 0.0039(10) 0.0022(9) N1 0.0086(14) 0.0118(14) 0.0150(17) 0.0025(12) 0.0035(13) 0.0021(11) N2 0.0114(15) 0.0136(14) 0.0094(15) 0.0044(12) 0.0015(13) 0.0011(11) N3 0.0102(14) 0.0117(13) 0.0098(15) 0.0038(12) 0.0036(13) 0.0011(11) C1 0.0097(17) 0.0136(17) 0.021(2) 0.0024(15) 0.0046(16) 0.0023(14) C2 0.0123(18) 0.0127(17) 0.036(3) 0.0116(17) 0.0146(19) 0.0045(14) C3 0.0167(18) 0.0191(18) 0.021(2) 0.0128(16) 0.0153(17) 0.0112(14) C4 0.0106(17) 0.0119(16) 0.0132(18) 0.0061(14) 0.0062(15) 0.0045(13) C5 0.0094(16) 0.0073(15) 0.0135(18) 0.0050(13) 0.0064(15) 0.0036(12) C6 0.0190(19) 0.0198(18) 0.0077(18) 0.0059(15) 0.0007(16) 0.0033(15) C7 0.0112(17) 0.0149(17) 0.0125(19) 0.0025(15) 0.0012(15) 0.0011(14) C8 0.0153(18) 0.0086(16) 0.021(2) 0.0045(15) 0.0098(17) 0.0044(13) C9 0.0128(17) 0.0086(15) 0.0175(19) 0.0063(14) 0.0093(16) 0.0043(13) C10 0.0059(15) 0.0108(15) 0.0126(18) 0.0054(14) 0.0052(14) 0.0049(12) C11 0.0123(17) 0.0139(16) 0.0147(19) 0.0003(15) 0.0080(16) 0.0035(13) C12 0.0108(17) 0.0121(16) 0.016(2) 0.0036(15) 0.0037(16) 0.0052(13) C13 0.0135(18) 0.0132(16) 0.0163(19) 0.0098(15) 0.0042(16) 0.0039(13) C14 0.0108(16) 0.0121(16) 0.0118(18) 0.0061(14) 0.0058(15) 0.0041(13) C15 0.0051(15) 0.0058(14) 0.0076(16) 0.0007(12) 0.0012(13) 0.0006(11) C16 0.0061(11) 0.0085(11) 0.0087(12) 0.0012(9) 0.0003(10) -0.0004(9) C17 0.0061(11) 0.0085(11) 0.0087(12) 0.0012(9) 0.0003(10) -0.0004(9) C18 0.0058(15) 0.0103(15) 0.0083(17) 0.0042(13) 0.0023(14) 0.0011(12) C19 0.0067(15) 0.0085(15) 0.0069(16) 0.0011(13) 0.0007(13) 0.0010(12) C20 0.0129(17) 0.0112(16) 0.0104(18) 0.0048(14) 0.0033(15) 0.0021(13) C21 0.0159(19) 0.0173(18) 0.0141(19) 0.0038(15) 0.0084(16) 0.0062(14) C22 0.0164(19) 0.0119(16) 0.0143(19) 0.0014(15) 0.0029(16) 0.0055(14) C23 0.022(2) 0.0105(16) 0.016(2) 0.0065(15) 0.0079(17) 0.0045(14) C24 0.0129(17) 0.0124(16) 0.0105(18) 0.0042(14) 0.0053(15) 0.0022(13) C25 0.0066(15) 0.0089(15) 0.0080(17) 0.0011(13) 0.0016(14) 0.0028(12) C26 0.0151(18) 0.0096(16) 0.0135(19) 0.0032(14) 0.0035(16) 0.0051(13) C27 0.0177(19) 0.0173(18) 0.0097(18) 0.0031(15) 0.0013(16) 0.0103(15) C28 0.0070(17) 0.0153(17) 0.015(2) -0.0046(15) -0.0015(15) 0.0034(13) C29 0.0086(17) 0.0121(17) 0.025(2) 0.0010(16) 0.0085(17) 0.0011(13) C30 0.0168(18) 0.0119(16) 0.0113(18) 0.0032(14) 0.0102(16) 0.0058(13) 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 C16 Au1 P1 177.06(9) . . ? C5 P1 Au1 113.27(12) . . ? C5 P1 C10 109.16(16) . . ? C10 P1 Au1 113.19(11) . . ? C15 P1 Au1 115.15(12) . . ? C15 P1 C5 101.34(14) . . ? C15 P1 C10 103.69(15) . . ? C18 O1 H1 109.5 . . ? C5 N1 C1 117.4(3) . . ? C6 N2 C10 117.5(3) . . ? C11 N3 C15 116.4(3) . . ? N1 C1 H1A 118.7 . . ? N1 C1 C2 122.6(4) . . ? C2 C1 H1A 118.7 . . ? C1 C2 H2 120.5 . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3 120.4 . . ? C2 C3 C4 119.2(3) . . ? C4 C3 H3 120.4 . . ? C3 C4 H4 121.2 . . ? C5 C4 C3 117.6(3) . . ? C5 C4 H4 121.2 . . ? N1 C5 P1 109.3(3) . . ? N1 C5 C4 124.2(3) . . ? C4 C5 P1 126.4(3) . . ? N2 C6 H6 118.3 . . ? N2 C6 C7 123.4(4) . . ? C7 C6 H6 118.3 . . ? C6 C7 H7 120.7 . . ? C8 C7 C6 118.6(3) . . ? C8 C7 H7 120.7 . . ? C7 C8 H8 120.4 . . ? C7 C8 C9 119.1(3) . . ? C9 C8 H8 120.4 . . ? C8 C9 H9 121.1 . . ? C8 C9 C10 117.8(3) . . ? C10 C9 H9 121.1 . . ? N2 C10 P1 117.7(2) . . ? N2 C10 C9 123.6(3) . . ? C9 C10 P1 118.7(3) . . ? N3 C11 H11 118.1 . . ? N3 C11 C12 123.8(3) . . ? C12 C11 H11 118.1 . . ? C11 C12 H12 120.5 . . ? C11 C12 C13 119.0(3) . . ? C13 C12 H12 120.5 . . ? C12 C13 H13 120.9 . . ? C12 C13 C14 118.2(3) . . ? C14 C13 H13 120.9 . . ? C13 C14 H14 120.6 . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.6 . . ? N3 C15 P1 114.9(3) . . ? N3 C15 C14 123.9(3) . . ? C14 C15 P1 121.3(3) . . ? C17 C16 Au1 176.7(3) . . ? C16 C17 C18 176.5(4) . . ? O1 C18 C17 110.3(3) . . ? O1 C18 C19 111.6(3) . . ? O1 C18 C25 105.5(3) . . ? C17 C18 C19 110.9(3) . . ? C17 C18 C25 112.1(3) . . ? C25 C18 C19 106.3(3) . . ? C20 C19 C18 120.0(3) . . ? C24 C19 C18 120.7(3) . . ? C24 C19 C20 119.0(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.7 . . ? C20 C21 H21 120.0 . . ? C20 C21 C22 119.9(3) . . ? C22 C21 H21 120.0 . . ? C21 C22 H22 120.3 . . ? C23 C22 C21 119.4(3) . . ? C23 C22 H22 120.3 . . ? C22 C23 H23 119.5 . . ? C22 C23 C24 121.0(3) . . ? C24 C23 H23 119.5 . . ? C19 C24 H24 120.0 . . ? C23 C24 C19 120.1(3) . . ? C23 C24 H24 120.0 . . ? C26 C25 C18 119.3(3) . . ? C26 C25 C30 118.3(3) . . ? C30 C25 C18 122.2(3) . . ? C25 C26 H26 119.1 . . ? C27 C26 C25 121.9(3) . . ? C27 C26 H26 119.1 . . ? C26 C27 H27 120.4 . . ? C26 C27 C28 119.2(4) . . ? C28 C27 H27 120.4 . . ? C27 C28 H28 119.8 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.8 . . ? C28 C29 H29 120.0 . . ? C28 C29 C30 120.0(3) . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 120.3(4) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? 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 Au1 P1 2.2601(10) . ? Au1 C16 1.996(4) . ? P1 C5 1.831(3) . ? P1 C10 1.831(4) . ? P1 C15 1.830(3) . ? O1 H1 0.8200 . ? O1 C18 1.438(4) . ? N1 C1 1.334(4) . ? N1 C5 1.332(4) . ? N2 C6 1.330(4) . ? N2 C10 1.335(5) . ? N3 C11 1.343(4) . ? N3 C15 1.350(4) . ? C1 H1A 0.9300 . ? C1 C2 1.398(6) . ? C2 H2 0.9300 . ? C2 C3 1.367(5) . ? C3 H3 0.9300 . ? C3 C4 1.393(5) . ? C4 H4 0.9300 . ? C4 C5 1.383(5) . ? C6 H6 0.9300 . ? C6 C7 1.394(5) . ? C7 H7 0.9300 . ? C7 C8 1.375(5) . ? C8 H8 0.9300 . ? C8 C9 1.394(5) . ? C9 H9 0.9300 . ? C9 C10 1.395(4) . ? C11 H11 0.9300 . ? C11 C12 1.377(5) . ? C12 H12 0.9300 . ? C12 C13 1.388(5) . ? C13 H13 0.9300 . ? C13 C14 1.393(4) . ? C14 H14 0.9300 . ? C14 C15 1.375(5) . ? C16 C17 1.199(5) . ? C17 C18 1.478(5) . ? C18 C19 1.537(4) . ? C18 C25 1.527(5) . ? C19 C20 1.398(5) . ? C19 C24 1.394(5) . ? C20 H20 0.9300 . ? C20 C21 1.391(5) . ? C21 H21 0.9300 . ? C21 C22 1.399(5) . ? C22 H22 0.9300 . ? C22 C23 1.377(5) . ? C23 H23 0.9300 . ? C23 C24 1.390(5) . ? C24 H24 0.9300 . ? C25 C26 1.386(5) . ? C25 C30 1.392(4) . ? C26 H26 0.9300 . ? C26 C27 1.374(5) . ? C27 H27 0.9300 . ? C27 C28 1.388(5) . ? C28 H28 0.9300 . ? C28 C29 1.373(6) . ? C29 H29 0.9300 . ? C29 C30 1.395(5) . ? C30 H30 0.9300 . ?