#------------------------------------------------------------------------------ #$Date: 2020-02-05 04:13:59 +0200 (Wed, 05 Feb 2020) $ #$Revision: 247875 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557235.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_1557235 loop_ _publ_author_name 'Navarro, Miquel' 'Toledo, Alberto' 'Ladeira, Sonia' 'Sosa Carrizo, E. Daiann' 'Miqueu, Karinne' 'Bourissou, Didier' _publ_section_title ; Versatility and Adaptative Behaviour of the P^N Chelating Ligand MeDalphos within Gold(I) pi Complexes: ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC06398F _journal_year 2020 _chemical_formula_moiety 'C33 H48 Au N O P, F6 Sb, C H2 Cl2' _chemical_formula_sum 'C34 H50 Au Cl2 F6 N O P Sb' _chemical_formula_weight 1023.35 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_update_record ; 2019-11-25 deposited with the CCDC. 2020-01-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.904(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9121(11) _cell_length_b 17.7644(18) _cell_length_c 19.509(2) _cell_measurement_reflns_used 9147 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 39.84 _cell_measurement_theta_min 3.15 _cell_volume 3654.5(6) _computing_cell_refinement 'APEX2 and SAINT' _computing_data_collection APEX2 _computing_data_reduction SAINT _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator triumph _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_unetI/netI 0.0156 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 152131 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.728 _diffrn_reflns_theta_min 2.999 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.999 _exptl_absorpt_correction_T_max 0.7481 _exptl_absorpt_correction_T_min 0.5851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.86 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2008 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 3.222 _refine_diff_density_min -1.849 _refine_diff_density_rms 0.121 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 434 _refine_ls_number_reflns 14574 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0302 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+6.5282P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.079 _reflns_Friedel_coverage 0 _reflns_number_gt 12480 _reflns_number_total 14574 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06398f2.cif _cod_data_source_block ATP092 _cod_original_cell_volume 3654.6(6) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557235 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL ATP092_a.res in P2(1)/c CELL 0.71073 10.9121 17.7644 19.5091 90.000 104.904 90.000 ZERR 4.00 0.0011 0.0018 0.0020 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H AU N O P SB F CL UNIT 136 200 4 4 4 4 4 24 8 MERG 2 OMIT -2 4 1 OMIT -1 6 4 OMIT -1 0 4 SHEL 40 0.64 FMAP 2 PLAN 20 SIZE 0.100 0.100 0.260 ACTA BOND $H L.S. 4 TEMP -80.16 WGHT 0.039100 6.528200 FVAR 0.06908 C1 1 0.773793 0.272421 0.458423 11.00000 0.01831 0.02076 = 0.01946 0.00134 0.00369 -0.00184 C2 1 0.906181 0.275485 0.469064 11.00000 0.01900 0.02888 = 0.03253 0.00311 0.00700 -0.00219 AFIX 43 H2 2 0.955734 0.232522 0.487300 11.00000 -1.20000 AFIX 0 C3 1 0.966000 0.339676 0.453579 11.00000 0.02528 0.03597 = 0.04482 0.00364 0.01335 -0.00896 AFIX 43 H3 2 1.055551 0.340648 0.461217 11.00000 -1.20000 AFIX 0 C4 1 0.894280 0.402330 0.426911 11.00000 0.03881 0.03150 = 0.04858 0.00664 0.01764 -0.00998 AFIX 43 H4 2 0.934615 0.446538 0.416115 11.00000 -1.20000 AFIX 0 C5 1 0.764320 0.400751 0.415961 11.00000 0.03525 0.02262 = 0.03811 0.00906 0.01305 -0.00263 AFIX 43 H5 2 0.716053 0.444154 0.397676 11.00000 -1.20000 AFIX 0 C6 1 0.702355 0.336633 0.431221 11.00000 0.02503 0.02052 = 0.01870 0.00292 0.00585 -0.00028 C7 1 0.528437 0.395715 0.465731 11.00000 0.03625 0.02799 = 0.04007 -0.00111 0.01472 0.00705 AFIX 137 H7A 2 0.572819 0.385893 0.515335 11.00000 -1.50000 H7B 2 0.436673 0.393011 0.460090 11.00000 -1.50000 H7C 2 0.550889 0.445998 0.452238 11.00000 -1.50000 AFIX 0 C8 1 0.502733 0.353093 0.344397 11.00000 0.03091 0.04352 = 0.02527 0.01109 0.00417 0.00605 AFIX 137 H8A 2 0.532389 0.401139 0.329891 11.00000 -1.50000 H8B 2 0.410765 0.355258 0.338119 11.00000 -1.50000 H8C 2 0.523008 0.312429 0.315187 11.00000 -1.50000 AFIX 0 C9 1 0.756397 0.178519 0.580468 11.00000 0.01697 0.01886 = 0.01640 0.00024 0.00236 0.00085 C10 1 0.714561 0.251294 0.610563 11.00000 0.06040 0.03023 = 0.02008 -0.00082 0.00627 0.01886 AFIX 23 H10A 2 0.757019 0.295042 0.595186 11.00000 -1.20000 H10B 2 0.621811 0.257854 0.592109 11.00000 -1.20000 AFIX 0 C11 1 0.749050 0.247718 0.691994 11.00000 0.08057 0.04086 = 0.02204 -0.00672 0.00956 0.02241 AFIX 13 H11 2 0.720550 0.295166 0.710774 11.00000 -1.20000 AFIX 0 C12 1 0.692362 0.110889 0.605535 11.00000 0.04353 0.04098 = 0.02015 0.00763 0.00073 -0.01843 AFIX 23 H12A 2 0.721034 0.063770 0.587433 11.00000 -1.20000 H12B 2 0.599244 0.114631 0.586643 11.00000 -1.20000 AFIX 0 C13 1 0.933915 0.167645 0.691995 11.00000 0.02277 0.06547 = 0.02248 0.00191 -0.00215 0.00308 AFIX 13 H13 2 1.027856 0.162558 0.710769 11.00000 -1.20000 AFIX 0 C14 1 0.869719 0.100407 0.715459 11.00000 0.05361 0.03733 = 0.02234 0.00368 -0.00052 0.01392 AFIX 23 H14A 2 0.892789 0.097393 0.767891 11.00000 -1.20000 H14B 2 0.897985 0.053498 0.696782 11.00000 -1.20000 AFIX 0 C15 1 0.726414 0.109074 0.687425 11.00000 0.04649 0.05158 = 0.01989 0.00931 0.00342 -0.01821 AFIX 13 H15 2 0.683102 0.065384 0.703478 11.00000 -1.20000 AFIX 0 C16 1 0.684033 0.181846 0.715769 11.00000 0.03521 0.09588 = 0.02326 0.00979 0.01281 0.02016 AFIX 23 H16A 2 0.590969 0.187414 0.698016 11.00000 -1.20000 H16B 2 0.705416 0.180216 0.768235 11.00000 -1.20000 AFIX 0 C17 1 0.900656 0.171618 0.610020 11.00000 0.01992 0.06669 = 0.02094 0.00379 0.00218 0.00450 AFIX 23 H17A 2 0.943031 0.215640 0.595051 11.00000 -1.20000 H17B 2 0.931308 0.125655 0.590999 11.00000 -1.20000 AFIX 0 C18 1 0.890435 0.239878 0.720651 11.00000 0.06773 0.04827 = 0.02214 -0.00544 -0.00328 -0.01579 AFIX 23 H18A 2 0.912469 0.238282 0.773128 11.00000 -1.20000 H18B 2 0.933745 0.283696 0.706021 11.00000 -1.20000 AFIX 0 C19 1 0.731344 0.108756 0.426969 11.00000 0.01747 0.02092 = 0.01312 0.00051 0.00211 0.00151 C20 1 0.620542 0.003178 0.309650 11.00000 0.03506 0.03429 = 0.03287 -0.01181 -0.00302 -0.00081 AFIX 23 H20A 2 0.628991 -0.037843 0.276820 11.00000 -1.20000 H20B 2 0.529982 0.017554 0.299400 11.00000 -1.20000 AFIX 0 C21 1 0.883999 0.020748 0.390218 11.00000 0.02557 0.03618 = 0.03304 -0.00859 0.00766 0.00533 AFIX 13 H21 2 0.975206 0.005767 0.400031 11.00000 -1.20000 AFIX 0 C22 1 0.838900 0.048038 0.313849 11.00000 0.04722 0.03906 = 0.03303 -0.00830 0.02270 -0.00443 AFIX 23 H22A 2 0.848975 0.007400 0.281003 11.00000 -1.20000 H22B 2 0.890533 0.091629 0.306419 11.00000 -1.20000 AFIX 0 C23 1 0.699632 0.070892 0.298695 11.00000 0.04836 0.03355 = 0.01420 -0.00079 0.00206 0.00265 AFIX 13 H23 2 0.669735 0.088605 0.248501 11.00000 -1.20000 AFIX 0 C24 1 0.870550 0.084421 0.441449 11.00000 0.01875 0.03611 = 0.02866 -0.00905 0.00239 0.00446 AFIX 23 H24A 2 0.900924 0.066688 0.491039 11.00000 -1.20000 H24B 2 0.923239 0.127930 0.435084 11.00000 -1.20000 AFIX 0 C25 1 0.666749 -0.024004 0.386499 11.00000 0.03649 0.01971 = 0.03269 -0.00445 0.01065 -0.00176 AFIX 13 H25 2 0.614995 -0.068354 0.393684 11.00000 -1.20000 AFIX 0 C26 1 0.651537 0.039564 0.437214 11.00000 0.03099 0.02042 = 0.02964 -0.00002 0.01286 -0.00204 AFIX 23 H26A 2 0.679784 0.021726 0.486864 11.00000 -1.20000 H26B 2 0.561088 0.054010 0.427653 11.00000 -1.20000 AFIX 0 C27 1 0.685246 0.134951 0.348998 11.00000 0.03712 0.02621 = 0.01359 0.00285 0.00007 0.00283 AFIX 23 H27A 2 0.595175 0.150375 0.338808 11.00000 -1.20000 H27B 2 0.735558 0.179018 0.341221 11.00000 -1.20000 AFIX 0 C28 1 0.805978 -0.047090 0.401912 11.00000 0.04246 0.02635 = 0.03162 -0.00202 0.00704 0.01162 AFIX 23 H28A 2 0.836015 -0.064848 0.451510 11.00000 -1.20000 H28B 2 0.815866 -0.088709 0.370012 11.00000 -1.20000 AFIX 0 C29 1 0.276941 0.233253 0.421471 11.00000 0.01722 0.03753 = 0.03434 -0.00193 0.00221 0.00093 H29 2 0.269607 0.271407 0.446873 11.00000 0.04900 C30 1 0.293918 0.164065 0.455302 11.00000 0.03251 0.05123 = 0.03576 0.00968 0.00473 -0.01343 H30 2 0.305621 0.163149 0.509321 11.00000 0.04267 C31 1 0.258404 0.100274 0.347282 11.00000 0.07383 0.03845 = 0.05977 -0.00742 -0.01208 -0.00743 AFIX 23 H31A 2 0.229949 0.050873 0.325439 11.00000 -1.20000 H31B 2 0.341435 0.112128 0.338146 11.00000 -1.20000 AFIX 0 C32 1 0.164169 0.159463 0.314732 11.00000 0.03677 0.05483 = 0.04805 -0.00330 -0.00959 -0.00875 AFIX 23 H32A 2 0.082719 0.149856 0.326687 11.00000 -1.20000 H32B 2 0.148731 0.158358 0.262466 11.00000 -1.20000 AFIX 0 C33 1 0.216152 0.236579 0.343185 11.00000 0.03039 0.04637 = 0.04487 0.00980 -0.00755 0.00422 AFIX 23 H33A 2 0.279443 0.253477 0.318113 11.00000 -1.20000 H33B 2 0.146149 0.273707 0.333781 11.00000 -1.20000 AFIX 0 C34 1 0.801187 0.479377 0.604859 11.00000 0.05731 0.06764 = 0.06344 -0.02060 0.00691 -0.02122 AFIX 23 H34A 2 0.732860 0.452237 0.619533 11.00000 -1.20000 H34B 2 0.775031 0.485006 0.552630 11.00000 -1.20000 AFIX 0 AU1 3 0.482745 0.215490 0.450916 11.00000 0.01453 0.02720 = 0.02079 -0.00017 0.00196 0.00155 N1 4 0.566073 0.338710 0.419730 11.00000 0.02365 0.02187 = 0.02139 0.00525 0.00493 0.00438 O1 5 0.271874 0.096442 0.422499 11.00000 0.07422 0.04083 = 0.06491 0.01542 -0.00677 -0.02539 P1 6 0.696387 0.188536 0.481873 11.00000 0.01371 0.01735 = 0.01593 0.00240 0.00233 0.00045 SB1 7 0.338553 0.144934 0.136083 11.00000 0.03743 0.05587 = 0.02585 0.00538 0.00234 -0.00804 F1 8 0.492848 0.101071 0.134232 11.00000 0.05630 0.15830 = 0.04666 0.00472 0.00449 0.03257 F2 8 0.415144 0.188212 0.224012 11.00000 0.07487 0.07474 = 0.04045 -0.00732 -0.00476 -0.01833 F3 8 0.184825 0.189464 0.136638 11.00000 0.04883 0.09285 = 0.07884 -0.00553 0.01196 0.00624 F4 8 0.265328 0.100955 0.047774 11.00000 0.06412 0.11453 = 0.03750 -0.01930 -0.00530 0.00064 F5 8 0.381118 0.228418 0.089431 11.00000 0.08365 0.10980 = 0.06612 0.04218 0.01517 -0.02591 F6 8 0.297866 0.060923 0.182008 11.00000 0.12094 0.05467 = 0.06493 0.00589 0.03119 -0.02341 CL1 9 0.940505 0.426405 0.628702 11.00000 0.09621 0.03166 = 0.11531 0.01005 0.05651 0.00509 CL2 9 0.820460 0.568663 0.644131 11.00000 0.04304 0.04619 = 0.04917 0.00663 0.01216 0.00800 HKLF 4 REM ATP092_a.res in P2(1)/c REM R1 = 0.0302 for 12480 Fo > 4sig(Fo) and 0.0392 for all 14574 data REM 434 parameters refined using 0 restraints END WGHT 0.0390 6.5331 REM Highest difference peak 3.222, deepest hole -1.849, 1-sigma level 0.121 Q1 1 0.3289 0.1819 0.1427 11.00000 0.05 3.22 Q2 1 0.4844 0.2244 0.4165 11.00000 0.05 3.09 Q3 1 0.4767 0.1773 0.4632 11.00000 0.05 2.52 Q4 1 0.2974 0.1261 0.1386 11.00000 0.05 1.76 Q5 1 0.4861 0.2564 0.4603 11.00000 0.05 1.04 Q6 1 0.4193 0.2195 0.4444 11.00000 0.05 0.90 Q7 1 0.9022 0.1259 0.6892 11.00000 0.05 0.86 Q8 1 0.6364 0.1345 0.6088 11.00000 0.05 0.79 Q9 1 0.8700 0.1301 0.6069 11.00000 0.05 0.79 Q10 1 0.8136 0.2457 0.7004 11.00000 0.05 0.79 Q11 1 0.9257 0.2042 0.7222 11.00000 0.05 0.76 Q12 1 0.2727 0.1911 0.4221 11.00000 0.05 0.73 Q13 1 0.8751 0.4256 0.6289 11.00000 0.05 0.72 Q14 1 0.7817 0.5398 0.6164 11.00000 0.05 0.72 Q15 1 0.7973 0.0850 0.7142 11.00000 0.05 0.68 Q16 1 0.5501 0.2174 0.4564 11.00000 0.05 0.67 Q17 1 0.4822 0.3516 0.4506 11.00000 0.05 0.67 Q18 1 0.9847 0.4424 0.6582 11.00000 0.05 0.66 Q19 1 0.6785 0.1359 0.6929 11.00000 0.05 0.61 Q20 1 0.7111 0.4823 0.6233 11.00000 0.05 0.59 ; _shelx_res_checksum 1870 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '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 C1 C 0.7738(2) 0.27242(13) 0.45842(12) 0.0197(4) Uani 1 1 d . . C2 C 0.9062(2) 0.27549(15) 0.46906(15) 0.0267(5) Uani 1 1 d . . H2 H 0.9557 0.2325 0.4873 0.032 Uiso 1 1 calc R U C3 C 0.9660(3) 0.33968(18) 0.45358(17) 0.0346(6) Uani 1 1 d . . H3 H 1.0556 0.3406 0.4612 0.041 Uiso 1 1 calc R U C4 C 0.8943(3) 0.40233(18) 0.42691(19) 0.0385(7) Uani 1 1 d . . H4 H 0.9346 0.4465 0.4161 0.046 Uiso 1 1 calc R U C5 C 0.7643(3) 0.40075(16) 0.41596(16) 0.0313(5) Uani 1 1 d . . H5 H 0.7161 0.4442 0.3977 0.038 Uiso 1 1 calc R U C6 C 0.7024(2) 0.33663(13) 0.43122(12) 0.0214(4) Uani 1 1 d . . C7 C 0.5284(3) 0.39571(17) 0.46573(18) 0.0339(6) Uani 1 1 d . . H7A H 0.5728 0.3859 0.5153 0.051 Uiso 1 1 calc R U H7B H 0.4367 0.393 0.4601 0.051 Uiso 1 1 calc R U H7C H 0.5509 0.446 0.4522 0.051 Uiso 1 1 calc R U C8 C 0.5027(3) 0.35309(19) 0.34440(15) 0.0338(6) Uani 1 1 d . . H8A H 0.5324 0.4011 0.3299 0.051 Uiso 1 1 calc R U H8B H 0.4108 0.3553 0.3381 0.051 Uiso 1 1 calc R U H8C H 0.523 0.3124 0.3152 0.051 Uiso 1 1 calc R U C9 C 0.7564(2) 0.17852(12) 0.58047(11) 0.0178(4) Uani 1 1 d . . C10 C 0.7146(4) 0.25129(17) 0.61056(15) 0.0377(7) Uani 1 1 d . . H10A H 0.757 0.295 0.5952 0.045 Uiso 1 1 calc R U H10B H 0.6218 0.2579 0.5921 0.045 Uiso 1 1 calc R U C11 C 0.7490(4) 0.2477(2) 0.69199(17) 0.0485(10) Uani 1 1 d . . H11 H 0.7205 0.2952 0.7108 0.058 Uiso 1 1 calc R U C12 C 0.6924(3) 0.11089(19) 0.60553(15) 0.0363(7) Uani 1 1 d . . H12A H 0.721 0.0638 0.5874 0.044 Uiso 1 1 calc R U H12B H 0.5992 0.1146 0.5866 0.044 Uiso 1 1 calc R U C13 C 0.9339(3) 0.1676(2) 0.69199(15) 0.0384(7) Uani 1 1 d . . H13 H 1.0279 0.1626 0.7108 0.046 Uiso 1 1 calc R U C14 C 0.8697(4) 0.10041(19) 0.71546(16) 0.0396(7) Uani 1 1 d . . H14A H 0.8928 0.0974 0.7679 0.048 Uiso 1 1 calc R U H14B H 0.898 0.0535 0.6968 0.048 Uiso 1 1 calc R U C15 C 0.7264(3) 0.1091(2) 0.68742(15) 0.0403(7) Uani 1 1 d . . H15 H 0.6831 0.0654 0.7035 0.048 Uiso 1 1 calc R U C16 C 0.6840(3) 0.1818(3) 0.71577(17) 0.0505(10) Uani 1 1 d . . H16A H 0.591 0.1874 0.698 0.061 Uiso 1 1 calc R U H16B H 0.7054 0.1802 0.7682 0.061 Uiso 1 1 calc R U C17 C 0.9007(3) 0.1716(2) 0.61002(15) 0.0364(7) Uani 1 1 d . . H17A H 0.943 0.2156 0.5951 0.044 Uiso 1 1 calc R U H17B H 0.9313 0.1257 0.591 0.044 Uiso 1 1 calc R U C18 C 0.8904(4) 0.2399(2) 0.72065(17) 0.0488(9) Uani 1 1 d . . H18A H 0.9125 0.2383 0.7731 0.059 Uiso 1 1 calc R U H18B H 0.9337 0.2837 0.706 0.059 Uiso 1 1 calc R U C19 C 0.7313(2) 0.10876(13) 0.42697(11) 0.0175(4) Uani 1 1 d . . C20 C 0.6205(3) 0.00318(18) 0.30965(17) 0.0362(6) Uani 1 1 d . . H20A H 0.629 -0.0378 0.2768 0.043 Uiso 1 1 calc R U H20B H 0.53 0.0176 0.2994 0.043 Uiso 1 1 calc R U C21 C 0.8840(3) 0.02075(17) 0.39022(16) 0.0316(5) Uani 1 1 d . . H21 H 0.9752 0.0058 0.4 0.038 Uiso 1 1 calc R U C22 C 0.8389(3) 0.04804(19) 0.31385(17) 0.0375(7) Uani 1 1 d . . H22A H 0.849 0.0074 0.281 0.045 Uiso 1 1 calc R U H22B H 0.8905 0.0916 0.3064 0.045 Uiso 1 1 calc R U C23 C 0.6996(3) 0.07089(17) 0.29869(13) 0.0331(6) Uani 1 1 d . . H23 H 0.6697 0.0886 0.2485 0.04 Uiso 1 1 calc R U C24 C 0.8705(2) 0.08442(17) 0.44145(15) 0.0285(5) Uani 1 1 d . . H24A H 0.9009 0.0667 0.491 0.034 Uiso 1 1 calc R U H24B H 0.9232 0.1279 0.4351 0.034 Uiso 1 1 calc R U C25 C 0.6667(3) -0.02400(15) 0.38650(15) 0.0293(5) Uani 1 1 d . . H25 H 0.615 -0.0684 0.3937 0.035 Uiso 1 1 calc R U C26 C 0.6515(3) 0.03956(14) 0.43721(15) 0.0261(5) Uani 1 1 d . . H26A H 0.6798 0.0217 0.4869 0.031 Uiso 1 1 calc R U H26B H 0.5611 0.054 0.4277 0.031 Uiso 1 1 calc R U C27 C 0.6852(3) 0.13495(15) 0.34900(12) 0.0268(5) Uani 1 1 d . . H27A H 0.5952 0.1504 0.3388 0.032 Uiso 1 1 calc R U H27B H 0.7356 0.179 0.3412 0.032 Uiso 1 1 calc R U C28 C 0.8060(3) -0.04709(16) 0.40191(16) 0.0339(6) Uani 1 1 d . . H28A H 0.836 -0.0648 0.4515 0.041 Uiso 1 1 calc R U H28B H 0.8159 -0.0887 0.37 0.041 Uiso 1 1 calc R U C29 C 0.2769(2) 0.23325(19) 0.42147(17) 0.0305(5) Uani 1 1 d . . H29 H 0.270(5) 0.271(3) 0.447(3) 0.049(13) Uiso 1 1 d . . C30 C 0.2939(3) 0.1641(2) 0.45530(19) 0.0406(7) Uani 1 1 d . . H30 H 0.306(4) 0.163(2) 0.509(2) 0.043(11) Uiso 1 1 d . . C31 C 0.2584(5) 0.1003(2) 0.3473(3) 0.0627(12) Uani 1 1 d . . H31A H 0.2299 0.0509 0.3254 0.075 Uiso 1 1 calc R U H31B H 0.3414 0.1121 0.3381 0.075 Uiso 1 1 calc R U C32 C 0.1642(4) 0.1595(2) 0.3147(2) 0.0503(9) Uani 1 1 d . . H32A H 0.0827 0.1499 0.3267 0.06 Uiso 1 1 calc R U H32B H 0.1487 0.1584 0.2625 0.06 Uiso 1 1 calc R U C33 C 0.2162(3) 0.2366(2) 0.3432(2) 0.0437(8) Uani 1 1 d . . H33A H 0.2794 0.2535 0.3181 0.052 Uiso 1 1 calc R U H33B H 0.1461 0.2737 0.3338 0.052 Uiso 1 1 calc R U C34 C 0.8012(5) 0.4794(3) 0.6049(3) 0.0644(12) Uani 1 1 d . . H34A H 0.7329 0.4522 0.6195 0.077 Uiso 1 1 calc R U H34B H 0.775 0.485 0.5526 0.077 Uiso 1 1 calc R U Au1 Au 0.48274(2) 0.21549(2) 0.45092(2) 0.02131(3) Uani 1 1 d . . N1 N 0.5661(2) 0.33871(12) 0.41973(11) 0.0225(4) Uani 1 1 d . . O1 O 0.2719(3) 0.09644(17) 0.42250(18) 0.0645(9) Uani 1 1 d . . P1 P 0.69639(5) 0.18854(3) 0.48187(3) 0.01594(9) Uani 1 1 d . . Sb1 Sb 0.33855(2) 0.14493(2) 0.13608(2) 0.04078(6) Uani 1 1 d . . F1 F 0.4928(3) 0.1011(3) 0.13423(15) 0.0887(11) Uani 1 1 d . . F2 F 0.4151(3) 0.18821(18) 0.22401(13) 0.0670(7) Uani 1 1 d . . F3 F 0.1848(3) 0.1895(2) 0.13664(18) 0.0743(8) Uani 1 1 d . . F4 F 0.2653(3) 0.1010(2) 0.04777(14) 0.0754(9) Uani 1 1 d . . F5 F 0.3811(4) 0.2284(2) 0.08943(18) 0.0873(11) Uani 1 1 d . . F6 F 0.2979(4) 0.06092(17) 0.18201(17) 0.0788(9) Uani 1 1 d . . Cl1 Cl 0.94050(15) 0.42641(6) 0.62870(9) 0.0757(4) Uani 1 1 d . . Cl2 Cl 0.82046(9) 0.56866(5) 0.64413(5) 0.04608(18) 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 C1 0.0183(9) 0.0208(10) 0.0195(9) 0.0013(7) 0.0037(7) -0.0018(7) C2 0.0190(10) 0.0289(12) 0.0325(12) 0.0031(9) 0.0070(9) -0.0022(8) C3 0.0253(12) 0.0360(14) 0.0448(17) 0.0036(12) 0.0133(11) -0.0090(10) C4 0.0388(15) 0.0315(14) 0.0486(18) 0.0066(12) 0.0176(13) -0.0100(12) C5 0.0352(13) 0.0226(11) 0.0381(14) 0.0091(10) 0.0131(11) -0.0026(10) C6 0.0250(10) 0.0205(10) 0.0187(9) 0.0029(7) 0.0059(8) -0.0003(8) C7 0.0362(14) 0.0280(13) 0.0401(15) -0.0011(11) 0.0147(12) 0.0070(11) C8 0.0309(13) 0.0435(16) 0.0253(12) 0.0111(11) 0.0042(10) 0.0061(11) C9 0.0170(9) 0.0189(9) 0.0164(9) 0.0002(7) 0.0024(7) 0.0009(7) C10 0.060(2) 0.0302(14) 0.0201(11) -0.0008(10) 0.0063(12) 0.0189(13) C11 0.081(3) 0.0409(18) 0.0220(13) -0.0067(12) 0.0096(15) 0.0224(18) C12 0.0435(16) 0.0410(15) 0.0201(11) 0.0076(10) 0.0007(10) -0.0184(13) C13 0.0228(12) 0.065(2) 0.0225(12) 0.0019(12) -0.0022(9) 0.0031(12) C14 0.0536(19) 0.0373(15) 0.0223(12) 0.0037(11) -0.0005(12) 0.0139(14) C15 0.0465(17) 0.0516(19) 0.0199(11) 0.0093(12) 0.0034(11) -0.0182(14) C16 0.0352(16) 0.096(3) 0.0233(13) 0.0098(16) 0.0128(12) 0.0202(18) C17 0.0199(11) 0.067(2) 0.0209(11) 0.0038(12) 0.0022(9) 0.0045(12) C18 0.068(2) 0.0483(19) 0.0221(13) -0.0054(13) -0.0033(14) -0.0158(18) C19 0.0175(8) 0.0209(9) 0.0131(8) 0.0005(7) 0.0021(7) 0.0015(7) C20 0.0351(14) 0.0343(14) 0.0329(14) -0.0118(11) -0.0030(11) -0.0008(11) C21 0.0256(12) 0.0362(14) 0.0330(13) -0.0086(11) 0.0077(10) 0.0053(10) C22 0.0472(17) 0.0391(15) 0.0330(14) -0.0083(12) 0.0227(13) -0.0044(13) C23 0.0484(16) 0.0335(13) 0.0142(10) -0.0008(9) 0.0021(10) 0.0027(12) C24 0.0187(10) 0.0361(13) 0.0287(12) -0.0090(10) 0.0024(9) 0.0045(9) C25 0.0365(13) 0.0197(10) 0.0327(13) -0.0044(9) 0.0107(11) -0.0018(9) C26 0.0310(12) 0.0204(10) 0.0296(12) 0.0000(9) 0.0129(10) -0.0020(9) C27 0.0371(13) 0.0262(11) 0.0136(9) 0.0028(8) 0.0001(9) 0.0028(10) C28 0.0425(15) 0.0264(12) 0.0316(13) -0.0020(10) 0.0070(11) 0.0116(11) C29 0.0172(10) 0.0375(14) 0.0343(14) -0.0019(11) 0.0022(9) 0.0009(9) C30 0.0325(14) 0.0512(19) 0.0358(15) 0.0097(13) 0.0047(12) -0.0134(13) C31 0.074(3) 0.0384(19) 0.060(3) -0.0074(18) -0.012(2) -0.0074(19) C32 0.0368(17) 0.055(2) 0.048(2) -0.0033(16) -0.0096(15) -0.0087(15) C33 0.0304(14) 0.0464(18) 0.0449(18) 0.0098(15) -0.0076(13) 0.0042(13) C34 0.057(3) 0.068(3) 0.063(3) -0.021(2) 0.007(2) -0.021(2) Au1 0.01453(4) 0.02720(5) 0.02079(4) -0.00017(3) 0.00196(3) 0.00155(3) N1 0.0237(9) 0.0219(9) 0.0214(9) 0.0052(7) 0.0049(7) 0.0044(7) O1 0.074(2) 0.0408(14) 0.0649(19) 0.0154(13) -0.0068(16) -0.0254(14) P1 0.0137(2) 0.0173(2) 0.0159(2) 0.00240(18) 0.00233(17) 0.00045(17) Sb1 0.03743(11) 0.05587(14) 0.02585(9) 0.00538(8) 0.00234(8) -0.00804(9) F1 0.0563(17) 0.158(4) 0.0467(15) 0.0047(18) 0.0045(12) 0.033(2) F2 0.0749(18) 0.0747(18) 0.0405(13) -0.0073(12) -0.0048(12) -0.0183(15) F3 0.0488(15) 0.093(2) 0.079(2) -0.0055(18) 0.0120(14) 0.0062(15) F4 0.0641(17) 0.115(3) 0.0375(12) -0.0193(14) -0.0053(11) 0.0006(17) F5 0.084(2) 0.110(3) 0.0661(19) 0.0422(18) 0.0152(16) -0.0259(19) F6 0.121(3) 0.0547(16) 0.0649(18) 0.0059(13) 0.0312(18) -0.0234(17) Cl1 0.0962(9) 0.0317(4) 0.1153(11) 0.0101(5) 0.0565(9) 0.0051(5) Cl2 0.0430(4) 0.0462(4) 0.0492(5) 0.0066(4) 0.0122(4) 0.0080(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.006 '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' Sb Sb -0.5866 1.5461 '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' Cl Cl 0.1484 0.1585 '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 C6 C1 C2 118.2(2) C6 C1 P1 120.57(18) C2 C1 P1 121.18(18) C3 C2 C1 121.6(3) C3 C2 H2 119.2 C1 C2 H2 119.2 C4 C3 C2 119.5(3) C4 C3 H3 120.3 C2 C3 H3 120.3 C5 C4 C3 120.1(3) C5 C4 H4 119.9 C3 C4 H4 119.9 C4 C5 C6 121.3(3) C4 C5 H5 119.4 C6 C5 H5 119.4 C5 C6 C1 119.4(2) C5 C6 N1 118.8(2) C1 C6 N1 121.8(2) N1 C7 H7A 109.5 N1 C7 H7B 109.5 H7A C7 H7B 109.5 N1 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 N1 C8 H8A 109.5 N1 C8 H8B 109.5 H8A C8 H8B 109.5 N1 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C12 C9 C17 109.0(2) C12 C9 C10 109.5(2) C17 C9 C10 107.5(2) C12 C9 P1 109.54(16) C17 C9 P1 116.53(17) C10 C9 P1 104.63(16) C11 C10 C9 110.0(2) C11 C10 H10A 109.7 C9 C10 H10A 109.7 C11 C10 H10B 109.7 C9 C10 H10B 109.7 H10A C10 H10B 108.2 C16 C11 C18 109.5(3) C16 C11 C10 110.0(3) C18 C11 C10 110.0(3) C16 C11 H11 109.1 C18 C11 H11 109.1 C10 C11 H11 109.1 C9 C12 C15 109.8(2) C9 C12 H12A 109.7 C15 C12 H12A 109.7 C9 C12 H12B 109.7 C15 C12 H12B 109.7 H12A C12 H12B 108.2 C14 C13 C18 110.0(3) C14 C13 C17 110.2(3) C18 C13 C17 109.2(3) C14 C13 H13 109.2 C18 C13 H13 109.2 C17 C13 H13 109.2 C13 C14 C15 108.9(2) C13 C14 H14A 109.9 C15 C14 H14A 109.9 C13 C14 H14B 109.9 C15 C14 H14B 109.9 H14A C14 H14B 108.3 C16 C15 C14 109.5(3) C16 C15 C12 110.1(3) C14 C15 C12 108.9(3) C16 C15 H15 109.4 C14 C15 H15 109.4 C12 C15 H15 109.4 C11 C16 C15 109.7(3) C11 C16 H16A 109.7 C15 C16 H16A 109.7 C11 C16 H16B 109.7 C15 C16 H16B 109.7 H16A C16 H16B 108.2 C9 C17 C13 109.7(2) C9 C17 H17A 109.7 C13 C17 H17A 109.7 C9 C17 H17B 109.7 C13 C17 H17B 109.7 H17A C17 H17B 108.2 C11 C18 C13 109.1(3) C11 C18 H18A 109.9 C13 C18 H18A 109.9 C11 C18 H18B 109.9 C13 C18 H18B 109.9 H18A C18 H18B 108.3 C24 C19 C27 108.8(2) C24 C19 C26 108.4(2) C27 C19 C26 108.3(2) C24 C19 P1 116.45(16) C27 C19 P1 105.80(16) C26 C19 P1 108.82(15) C23 C20 C25 109.2(2) C23 C20 H20A 109.8 C25 C20 H20A 109.8 C23 C20 H20B 109.8 C25 C20 H20B 109.8 H20A C20 H20B 108.3 C22 C21 C28 110.2(2) C22 C21 C24 109.9(3) C28 C21 C24 109.4(2) C22 C21 H21 109.1 C28 C21 H21 109.1 C24 C21 H21 109.1 C21 C22 C23 109.2(2) C21 C22 H22A 109.8 C23 C22 H22A 109.8 C21 C22 H22B 109.8 C23 C22 H22B 109.8 H22A C22 H22B 108.3 C22 C23 C20 109.5(3) C22 C23 C27 109.5(2) C20 C23 C27 109.9(3) C22 C23 H23 109.3 C20 C23 H23 109.3 C27 C23 H23 109.3 C19 C24 C21 110.0(2) C19 C24 H24A 109.7 C21 C24 H24A 109.7 C19 C24 H24B 109.7 C21 C24 H24B 109.7 H24A C24 H24B 108.2 C28 C25 C20 109.7(2) C28 C25 C26 109.7(2) C20 C25 C26 109.6(2) C28 C25 H25 109.3 C20 C25 H25 109.3 C26 C25 H25 109.3 C25 C26 C19 110.0(2) C25 C26 H26A 109.7 C19 C26 H26A 109.7 C25 C26 H26B 109.7 C19 C26 H26B 109.7 H26A C26 H26B 108.2 C23 C27 C19 110.2(2) C23 C27 H27A 109.6 C19 C27 H27A 109.6 C23 C27 H27B 109.6 C19 C27 H27B 109.6 H27A C27 H27B 108.1 C21 C28 C25 108.9(2) C21 C28 H28A 109.9 C25 C28 H28A 109.9 C21 C28 H28B 109.9 C25 C28 H28B 109.9 H28A C28 H28B 108.3 C30 C29 C33 119.3(3) C30 C29 Au1 75.23(18) C33 C29 Au1 115.3(2) C30 C29 H29 117(3) C33 C29 H29 118(3) Au1 C29 H29 102(3) O1 C30 C29 125.2(3) O1 C30 Au1 113.0(3) C29 C30 Au1 68.73(17) O1 C30 H30 116(2) C29 C30 H30 118(2) Au1 C30 H30 100(2) O1 C31 C32 110.2(4) O1 C31 H31A 109.6 C32 C31 H31A 109.6 O1 C31 H31B 109.6 C32 C31 H31B 109.6 H31A C31 H31B 108.1 C31 C32 C33 109.0(3) C31 C32 H32A 109.9 C33 C32 H32A 109.9 C31 C32 H32B 109.9 C33 C32 H32B 109.9 H32A C32 H32B 108.3 C29 C33 C32 111.0(3) C29 C33 H33A 109.4 C32 C33 H33A 109.4 C29 C33 H33B 109.4 C32 C33 H33B 109.4 H33A C33 H33B 108 Cl1 C34 Cl2 111.9(2) Cl1 C34 H34A 109.2 Cl2 C34 H34A 109.2 Cl1 C34 H34B 109.2 Cl2 C34 H34B 109.2 H34A C34 H34B 107.9 C29 Au1 C30 36.05(13) C29 Au1 P1 176.27(9) C30 Au1 P1 140.53(10) C29 Au1 N1 102.82(10) C30 Au1 N1 138.49(11) P1 Au1 N1 80.74(5) C6 N1 C8 111.0(2) C6 N1 C7 111.0(2) C8 N1 C7 110.7(2) C6 N1 Au1 111.29(14) C8 N1 Au1 106.66(17) C7 N1 Au1 106.03(16) C30 O1 C31 113.6(3) C1 P1 C19 107.36(10) C1 P1 C9 105.80(10) C19 P1 C9 116.49(10) C1 P1 Au1 105.46(8) C19 P1 Au1 110.39(7) C9 P1 Au1 110.60(7) F6 Sb1 F3 90.64(17) F6 Sb1 F5 179.13(18) F3 Sb1 F5 90.16(17) F6 Sb1 F1 90.15(18) F3 Sb1 F1 179.10(16) F5 Sb1 F1 89.05(18) F6 Sb1 F2 89.64(14) F3 Sb1 F2 90.62(15) F5 Sb1 F2 90.70(15) F1 Sb1 F2 89.82(15) F6 Sb1 F4 90.58(15) F3 Sb1 F4 90.62(14) F5 Sb1 F4 89.06(17) F1 Sb1 F4 88.94(14) F2 Sb1 F4 178.74(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C6 1.406(3) C1 C2 1.407(3) C1 P1 1.828(2) C2 C3 1.385(4) C2 H2 0.95 C3 C4 1.383(5) C3 H3 0.95 C4 C5 1.379(4) C4 H4 0.95 C5 C6 1.395(3) C5 H5 0.95 C6 N1 1.446(3) C7 N1 1.480(4) C7 H7A 0.98 C7 H7B 0.98 C7 H7C 0.98 C8 N1 1.477(3) C8 H8A 0.98 C8 H8B 0.98 C8 H8C 0.98 C9 C12 1.532(4) C9 C17 1.536(4) C9 C10 1.537(4) C9 P1 1.874(2) C10 C11 1.537(4) C10 H10A 0.99 C10 H10B 0.99 C11 C16 1.502(6) C11 C18 1.506(6) C11 H11 1 C12 C15 1.545(4) C12 H12A 0.99 C12 H12B 0.99 C13 C14 1.514(5) C13 C18 1.523(6) C13 C17 1.548(4) C13 H13 1 C14 C15 1.526(5) C14 H14A 0.99 C14 H14B 0.99 C15 C16 1.524(6) C15 H15 1 C16 H16A 0.99 C16 H16B 0.99 C17 H17A 0.99 C17 H17B 0.99 C18 H18A 0.99 C18 H18B 0.99 C19 C24 1.534(3) C19 C27 1.546(3) C19 C26 1.549(3) C19 P1 1.874(2) C20 C23 1.527(5) C20 C25 1.532(4) C20 H20A 0.99 C20 H20B 0.99 C21 C22 1.523(5) C21 C28 1.526(5) C21 C24 1.541(4) C21 H21 1 C22 C23 1.527(5) C22 H22A 0.99 C22 H22B 0.99 C23 C27 1.537(4) C23 H23 1 C24 H24A 0.99 C24 H24B 0.99 C25 C28 1.527(4) C25 C26 1.538(4) C25 H25 1 C26 H26A 0.99 C26 H26B 0.99 C27 H27A 0.99 C27 H27B 0.99 C28 H28A 0.99 C28 H28B 0.99 C29 C30 1.385(5) C29 C33 1.502(5) C29 Au1 2.193(3) C29 H29 0.86(5) C30 O1 1.353(5) C30 Au1 2.276(3) C30 H30 1.03(4) C31 O1 1.438(6) C31 C32 1.493(6) C31 H31A 0.99 C31 H31B 0.99 C32 C33 1.531(5) C32 H32A 0.99 C32 H32B 0.99 C33 H33A 0.99 C33 H33B 0.99 C34 Cl1 1.746(6) C34 Cl2 1.750(5) C34 H34A 0.99 C34 H34B 0.99 Au1 P1 2.3032(6) Au1 N1 2.505(2) Sb1 F6 1.853(3) Sb1 F3 1.857(3) Sb1 F5 1.860(3) Sb1 F1 1.864(3) Sb1 F2 1.869(2) Sb1 F4 1.873(3)