#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:24:06 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042743.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_7042743 loop_ _publ_author_name 'Parvin, Nasrina' 'Dasgupta, Rajarshi' 'Pal, Shiv' 'Sen, Sakya Singha' 'Khan, Shabana' _publ_section_title ; “Strikingly diverse reactivity of structurally identical silylene and stannylene" ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01055A _journal_year 2017 _chemical_formula_sum 'C42 H79.5 Ag F6 N6 Sb Si4 Sn2' _chemical_formula_weight 1361.97 _chemical_properties_physical ', Air-sensitive,Moisture-sensitive,Oxygen-sensitive' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-03-03 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90.00(3) _cell_angle_beta 107.03(3) _cell_angle_gamma 90.00(3) _cell_formula_units_Z 4 _cell_length_a 15.748(3) _cell_length_b 19.935(4) _cell_length_c 20.701(4) _cell_measurement_reflns_used 9942 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 22.32 _cell_measurement_theta_min 2.30 _cell_volume 6214(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1741 _diffrn_reflns_av_unetI/netI 0.0618 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 95896 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.249 _diffrn_reflns_theta_min 2.288 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sheldrick,G.M(2012)SADABS.BrukerAXS Inc.,Madison,Wisconsin,USA.' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description block _exptl_crystal_F_000 2726 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max 0.7074 _exptl_transmission_factor_min 0.5589 _refine_diff_density_max 1.020 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 5635 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0519 _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^)+(0.0573P)^2^+48.2216P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1157 _refine_ls_wR_factor_ref 0.1479 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3519 _reflns_number_total 5635 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01055a2.cif _cod_data_source_block mo_NP_170_0m_a _cod_original_formula_sum 'C42 H79.50 Ag F6 N6 Sb Si4 Sn2' _cod_database_code 7042743 _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_res_file ; mo_NP_170_0m_a.res created by SHELXL-2014/7 TITL mo_NP_170_0m_a.res in C2/c CELL 0.71073 15.7476 19.9351 20.7014 90.000 107.030 90.000 ZERR 4.000 0.0030 0.0040 0.0040 0.030 0.030 0.030 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H Ag F Sb Sn Si N UNIT 168 318 4 24 4 8 16 24 OMIT -3 50.5 L.S. 5 ACTA BOND $H FMAP 2 PLAN 10 ISOR 0.001 C21A C21 ISOR 0.001 C18A C20A C15A C12A C17 C12 TEMP 23.000 WGHT 0.057300 48.221600 FVAR 0.15731 0.60433 PART 1 C1 1 0.778645 0.625315 0.334235 11.00000 0.04339 0.04780 = 0.07635 0.00733 0.02085 0.00861 C2 1 0.697323 0.513380 0.320911 11.00000 0.05917 0.03804 = 0.07906 0.01591 0.02843 0.00656 C3 1 0.842267 0.615029 0.402519 11.00000 0.05040 0.05622 = 0.08998 0.00800 0.00216 0.00419 C4 1 0.926492 0.589059 0.408784 11.00000 0.04726 0.07953 = 0.10609 0.02783 0.01661 0.01050 AFIX 43 H4 2 0.942495 0.577639 0.370375 11.00000 -1.20000 AFIX 0 C5 1 0.815388 0.748406 0.318471 11.00000 0.06877 0.06153 = 0.14284 0.03876 -0.00453 -0.01509 C6 1 0.638058 0.481070 0.256554 11.00000 0.11797 0.05441 = 0.11997 0.01391 -0.00308 -0.02557 AFIX 137 H6A 2 0.672005 0.473262 0.225589 11.00000 -1.50000 H6B 2 0.589320 0.510459 0.236060 11.00000 -1.50000 H6C 2 0.615598 0.439178 0.267559 11.00000 -1.50000 AFIX 0 C7 1 0.820104 0.631906 0.460335 11.00000 0.08922 0.09555 = 0.08156 -0.02216 0.00465 0.01556 AFIX 43 H7 2 0.764675 0.650484 0.456517 11.00000 -1.20000 AFIX 0 C8 1 0.774829 0.468196 0.349416 11.00000 0.09309 0.05927 = 0.17199 0.04435 0.03325 0.01037 AFIX 137 H8A 2 0.808776 0.484471 0.392968 11.00000 -1.50000 H8B 2 0.811555 0.467374 0.319699 11.00000 -1.50000 H8C 2 0.754012 0.423679 0.353917 11.00000 -1.50000 AFIX 0 C9 1 0.986238 0.580279 0.472107 11.00000 0.05530 0.10309 = 0.13088 0.03635 0.00653 0.01508 AFIX 43 H9 2 1.042593 0.563365 0.476131 11.00000 -1.20000 AFIX 0 C10 1 0.642380 0.521007 0.369358 11.00000 0.13282 0.09209 = 0.11651 0.01959 0.07601 -0.01481 AFIX 137 H10A 2 0.592655 0.549803 0.349710 11.00000 -1.50000 H10B 2 0.678262 0.540274 0.410895 11.00000 -1.50000 H10C 2 0.621337 0.477785 0.378231 11.00000 -1.50000 AFIX 0 C11 1 0.963065 0.596223 0.528460 11.00000 0.09400 0.12187 = 0.10722 0.00588 -0.00952 -0.00221 AFIX 43 H11 2 1.004055 0.590050 0.570668 11.00000 -1.20000 PART 1 21.00 AFIX 0 C12 1 0.847463 0.578811 0.190746 21.00000 0.09456 0.09584 = 0.09597 -0.00103 0.02877 0.00194 AFIX 137 H12A 2 0.879454 0.614573 0.218442 21.00000 -1.50000 H12B 2 0.887989 0.551719 0.175259 21.00000 -1.50000 H12C 2 0.819102 0.551656 0.216695 21.00000 -1.50000 PART 0 AFIX 0 C16 1 0.786541 0.782360 0.371838 11.00000 0.16042 0.05082 = 0.25822 -0.04887 0.00153 0.00804 AFIX 137 H16A 2 0.818731 0.764408 0.415113 11.00000 -1.50000 H16B 2 0.724093 0.775166 0.364210 11.00000 -1.50000 H16C 2 0.798036 0.829587 0.370898 11.00000 -1.50000 AFIX 0 C17 1 0.786373 0.789295 0.255052 11.00000 0.13595 0.13349 = 0.13875 0.00387 0.03713 -0.00274 AFIX 137 H17A 2 0.722680 0.790872 0.239431 11.00000 -1.50000 H17B 2 0.808429 0.769199 0.220996 11.00000 -1.50000 H17C 2 0.809421 0.834011 0.264098 11.00000 -1.50000 PART 1 21.00 AFIX 0 C19 1 0.756807 0.527468 0.078486 21.00000 0.14319 0.18142 = 0.11891 -0.07032 0.02526 0.08031 AFIX 137 H19A 2 0.811965 0.504487 0.083617 21.00000 -1.50000 H19B 2 0.730309 0.538529 0.031770 21.00000 -1.50000 H19C 2 0.717330 0.499001 0.093660 21.00000 -1.50000 PART 0 AFIX 0 SN1 6 0.648001 0.652786 0.226402 11.00000 0.04469 0.04698 = 0.06395 0.01007 0.02517 0.00863 AG1 3 0.500000 0.689505 0.250000 10.50000 0.04146 0.05757 = 0.07351 0.00000 0.02565 0.00000 SB1 5 0.500000 0.886065 0.250000 10.50000 0.10616 0.05413 = 0.08591 0.00000 -0.00413 0.00000 PART 1 21.00 SI2 7 0.778312 0.607759 0.130988 21.00000 0.06669 0.10186 = 0.07004 0.00655 0.04013 0.02469 PART 0 C13 1 0.879691 0.621489 0.524464 11.00000 0.12971 0.10289 = 0.09467 -0.01898 0.01234 -0.00155 AFIX 43 H13 2 0.863815 0.631240 0.563315 11.00000 -1.20000 PART 1 21.00 AFIX 0 SI1 7 0.595104 0.676133 0.068828 21.00000 0.10177 0.08344 = 0.06254 0.02552 0.04380 0.03986 PART 0 N1 8 0.721154 0.579276 0.299366 11.00000 0.04953 0.04219 = 0.05923 0.00539 0.01806 0.00535 N3 8 0.668560 0.634929 0.135317 11.00000 0.09547 0.07502 = 0.07109 0.02487 0.04590 0.02922 F3 4 0.486630 0.951604 0.309752 11.00000 0.21121 0.11909 = 0.13067 -0.00137 0.08533 0.02012 F2 4 0.618134 0.896506 0.293841 11.00000 0.14165 0.31178 = 0.24152 -0.02141 -0.02880 0.05620 PART 1 21.00 C21 1 0.830091 0.671887 0.087286 21.00000 0.13104 0.13219 = 0.13156 0.00138 0.03975 0.00003 AFIX 137 H21A 2 0.845322 0.711191 0.115077 21.00000 -1.50000 H21B 2 0.788604 0.683700 0.044718 21.00000 -1.50000 H21C 2 0.882729 0.653447 0.079795 21.00000 -1.50000 PART 0 AFIX 0 N2 8 0.771077 0.681944 0.298728 11.00000 0.04239 0.04455 = 0.10289 0.01968 0.01749 0.00450 PART 1 21.00 C15 1 0.488085 0.678573 0.073879 21.00000 0.08521 0.34639 = 0.07518 0.03070 0.02808 0.04383 AFIX 137 H15A 2 0.469992 0.634245 0.082304 21.00000 -1.50000 H15B 2 0.449158 0.695037 0.032078 21.00000 -1.50000 H15C 2 0.485357 0.707798 0.110075 21.00000 -1.50000 AFIX 0 C18 1 0.620013 0.768522 0.067714 21.00000 0.17753 0.09727 = 0.14182 0.06299 0.05709 0.06120 AFIX 137 H18A 2 0.601685 0.790791 0.102527 21.00000 -1.50000 H18B 2 0.588392 0.787001 0.024546 21.00000 -1.50000 H18C 2 0.682649 0.774834 0.075501 21.00000 -1.50000 AFIX 0 C20 1 0.602971 0.645424 -0.013180 21.00000 0.18861 0.16467 = 0.06917 0.00284 0.02205 0.07727 AFIX 137 H20A 2 0.657465 0.660831 -0.019997 21.00000 -1.50000 H20B 2 0.553651 0.662166 -0.048738 21.00000 -1.50000 H20C 2 0.601897 0.597274 -0.013529 21.00000 -1.50000 PART 0 AFIX 0 C14 1 0.918128 0.740551 0.336287 11.00000 0.05941 0.10135 = 0.29877 0.04676 -0.00380 -0.02832 AFIX 137 H14A 2 0.933046 0.720486 0.298874 11.00000 -1.50000 H14B 2 0.938990 0.712456 0.375406 11.00000 -1.50000 H14C 2 0.945637 0.783872 0.345555 11.00000 -1.50000 PART 1 21.00 AFIX 0 F1 4 0.530810 0.814476 0.306273 21.00000 0.31180 0.05605 = 0.08953 0.01673 0.06272 -0.00471 PART 2 -21.00 C21A 1 0.769854 0.608350 0.036662 -21.00000 0.14384 0.14423 = 0.14380 0.00043 0.04283 0.00034 AFIX 137 H21D 2 0.779012 0.570603 0.010687 -21.00000 -1.50000 H21E 2 0.823999 0.633514 0.052234 -21.00000 -1.50000 H21F 2 0.724047 0.636490 0.008961 -21.00000 -1.50000 AFIX 0 C19A 1 0.694888 0.491012 0.092600 -21.00000 0.18916 0.10182 = 0.18143 -0.00752 0.08187 0.07854 AFIX 137 H19D 2 0.677721 0.473604 0.130171 -21.00000 -1.50000 H19E 2 0.741208 0.463597 0.085074 -21.00000 -1.50000 H19F 2 0.644570 0.490698 0.052912 -21.00000 -1.50000 AFIX 0 C12A 1 0.868876 0.592780 0.219056 -21.00000 0.06370 0.06558 = 0.06506 -0.00099 0.01901 0.00134 SI2A 7 0.735641 0.577927 0.111169 -21.00000 0.08753 0.09849 = 0.08906 0.01462 0.05000 0.02782 SI1A 7 0.571991 0.648250 0.060355 -21.00000 0.12866 0.14233 = 0.08124 -0.02016 0.04410 -0.04165 C20A 1 0.519630 0.592894 -0.004210 -21.00000 0.15671 0.15686 = 0.15700 -0.00062 0.04596 0.00040 AFIX 137 H20D 2 0.555006 0.587896 -0.034608 -21.00000 -1.50000 H20E 2 0.462271 0.610256 -0.028408 -21.00000 -1.50000 H20F 2 0.512778 0.550043 0.014828 -21.00000 -1.50000 AFIX 0 C15A 1 0.468426 0.686329 0.082974 -21.00000 0.07132 0.07125 = 0.07152 -0.00017 0.02030 0.00064 AFIX 137 H15D 2 0.424748 0.700384 0.042291 -21.00000 -1.50000 H15E 2 0.486979 0.724206 0.112366 -21.00000 -1.50000 H15F 2 0.443223 0.652901 0.105257 -21.00000 -1.50000 AFIX 0 C18A 1 0.609279 0.724453 0.014058 -21.00000 0.16332 0.16343 = 0.16325 0.00041 0.04790 -0.00003 AFIX 137 H18D 2 0.598096 0.714029 -0.032971 -21.00000 -1.50000 H18E 2 0.671562 0.732612 0.033984 -21.00000 -1.50000 H18F 2 0.576305 0.763758 0.018656 -21.00000 -1.50000 AFIX 0 F1A 4 0.443552 0.834448 0.307593 -21.00000 0.28306 0.09983 = 0.08350 0.00048 0.05904 -0.08919 PART HKLF 4 REM mo_NP_170_0m_a.res in C2/c REM R1 = 0.0519 for 3519 Fo > 4sig(Fo) and 0.1040 for all 5635 data REM 380 parameters refined using 48 restraints END WGHT 0.0573 48.2208 REM Highest difference peak 1.020, deepest hole -0.729, 1-sigma level 0.107 Q1 1 0.5000 0.6190 0.2500 10.50000 0.05 1.02 Q2 1 0.8008 0.6897 0.2066 11.00000 0.05 0.86 Q3 1 0.7766 0.7993 0.2798 11.00000 0.05 0.73 Q4 1 0.4194 0.9104 0.2838 11.00000 0.05 0.73 Q5 1 0.5422 0.8659 0.2488 11.00000 0.05 0.68 Q6 1 0.5000 0.9062 0.2500 10.50000 0.05 0.67 Q7 1 0.5348 0.5492 0.0482 11.00000 0.05 0.57 Q8 1 0.5000 0.8027 0.2500 10.50000 0.05 0.54 Q9 1 0.5000 1.0098 0.2500 10.50000 0.05 0.49 Q10 1 0.5608 0.9311 0.3087 11.00000 0.05 0.46 ; _shelx_res_checksum 86996 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 C1 C 0.7786(5) 0.6253(4) 0.3342(4) 0.055(2) Uani 1 1 d . . . A 1 C2 C 0.6973(5) 0.5134(4) 0.3209(4) 0.057(2) Uani 1 1 d . . . B 1 C3 C 0.8423(5) 0.6150(4) 0.4025(5) 0.069(2) Uani 1 1 d . . . A 1 C4 C 0.9265(5) 0.5891(5) 0.4088(5) 0.079(3) Uani 1 1 d . . . A 1 H4 H 0.9425 0.5776 0.3704 0.095 Uiso 1 1 calc R U . A 1 C5 C 0.8154(6) 0.7484(5) 0.3185(7) 0.099(4) Uani 1 1 d . . . C 1 C6 C 0.6381(7) 0.4811(5) 0.2566(6) 0.106(4) Uani 1 1 d . . . B 1 H6A H 0.6720 0.4733 0.2256 0.158 Uiso 1 1 calc R U . B 1 H6B H 0.5893 0.5105 0.2361 0.158 Uiso 1 1 calc R U . B 1 H6C H 0.6156 0.4392 0.2676 0.158 Uiso 1 1 calc R U . B 1 C7 C 0.8201(7) 0.6319(5) 0.4603(6) 0.093(3) Uani 1 1 d . . . A 1 H7 H 0.7647 0.6505 0.4565 0.112 Uiso 1 1 calc R U . A 1 C8 C 0.7748(7) 0.4682(5) 0.3494(6) 0.109(4) Uani 1 1 d . . . B 1 H8A H 0.8088 0.4845 0.3930 0.164 Uiso 1 1 calc R U . B 1 H8B H 0.8116 0.4674 0.3197 0.164 Uiso 1 1 calc R U . B 1 H8C H 0.7540 0.4237 0.3539 0.164 Uiso 1 1 calc R U . B 1 C9 C 0.9862(7) 0.5803(6) 0.4721(7) 0.101(4) Uani 1 1 d . . . A 1 H9 H 1.0426 0.5634 0.4761 0.121 Uiso 1 1 calc R U . A 1 C10 C 0.6424(8) 0.5210(5) 0.3694(6) 0.105(4) Uani 1 1 d . . . B 1 H10A H 0.5927 0.5498 0.3497 0.158 Uiso 1 1 calc R U . B 1 H10B H 0.6783 0.5403 0.4109 0.158 Uiso 1 1 calc R U . B 1 H10C H 0.6213 0.4778 0.3782 0.158 Uiso 1 1 calc R U . B 1 C11 C 0.9631(9) 0.5962(7) 0.5285(7) 0.116(4) Uani 1 1 d . . . A 1 H11 H 1.0041 0.5901 0.5707 0.139 Uiso 1 1 calc R U . A 1 C12 C 0.8475(13) 0.5788(10) 0.1907(10) 0.095(6) Uani 0.604(12) 1 d . U P D 1 H12A H 0.8795 0.6146 0.2184 0.143 Uiso 0.604(12) 1 calc R U P D 1 H12B H 0.8880 0.5517 0.1753 0.143 Uiso 0.604(12) 1 calc R U P D 1 H12C H 0.8191 0.5517 0.2167 0.143 Uiso 0.604(12) 1 calc R U P D 1 C16 C 0.7865(10) 0.7824(5) 0.3718(9) 0.169(8) Uani 1 1 d . . . . . H16A H 0.8187 0.7644 0.4151 0.254 Uiso 1 1 calc R U . C 1 H16B H 0.7241 0.7752 0.3642 0.254 Uiso 1 1 calc R U . C 1 H16C H 0.7980 0.8296 0.3709 0.254 Uiso 1 1 calc R U . C 1 C17 C 0.7864(9) 0.7893(7) 0.2551(7) 0.137(5) Uani 1 1 d . U . . . H17A H 0.7227 0.7909 0.2394 0.205 Uiso 1 1 calc R U . C 1 H17B H 0.8084 0.7692 0.2210 0.205 Uiso 1 1 calc R U . C 1 H17C H 0.8094 0.8340 0.2641 0.205 Uiso 1 1 calc R U . C 1 C19 C 0.7568(18) 0.5275(15) 0.0785(13) 0.151(13) Uani 0.604(12) 1 d . . P D 1 H19A H 0.8120 0.5045 0.0836 0.226 Uiso 0.604(12) 1 calc R U P D 1 H19B H 0.7303 0.5385 0.0318 0.226 Uiso 0.604(12) 1 calc R U P D 1 H19C H 0.7173 0.4990 0.0937 0.226 Uiso 0.604(12) 1 calc R U P D 1 Sn1 Sn 0.64800(3) 0.65279(3) 0.22640(3) 0.04990(19) Uani 1 1 d . . . . . Ag1 Ag 0.5000 0.68950(4) 0.2500 0.0556(3) Uani 1 2 d S T P A . Sb1 Sb 0.5000 0.88606(4) 0.2500 0.0890(3) Uani 1 2 d S T P . . Si2 Si 0.7783(5) 0.6078(4) 0.1310(3) 0.075(2) Uani 0.604(12) 1 d . . P D 1 C13 C 0.8797(10) 0.6215(6) 0.5245(6) 0.113(4) Uani 1 1 d . . . . . H13 H 0.8638 0.6312 0.5633 0.136 Uiso 1 1 calc R U . A 1 Si1 Si 0.5951(6) 0.6761(4) 0.0688(5) 0.078(3) Uani 0.604(12) 1 d . . P D 1 N1 N 0.7212(4) 0.5793(3) 0.2994(3) 0.0499(15) Uani 1 1 d . . . . . N3 N 0.6686(5) 0.6349(4) 0.1353(4) 0.076(2) Uani 1 1 d . . . . . F3 F 0.4866(6) 0.9516(4) 0.3098(4) 0.146(3) Uani 1 1 d . . . . . F2 F 0.6181(7) 0.8965(7) 0.2938(6) 0.250(6) Uani 1 1 d . . . . . C21 C 0.8301(15) 0.6719(11) 0.0873(12) 0.131(8) Uani 0.604(12) 1 d . U P D 1 H21A H 0.8453 0.7112 0.1151 0.197 Uiso 0.604(12) 1 calc R U P D 1 H21B H 0.7886 0.6837 0.0447 0.197 Uiso 0.604(12) 1 calc R U P D 1 H21C H 0.8827 0.6534 0.0798 0.197 Uiso 0.604(12) 1 calc R U P D 1 N2 N 0.7711(4) 0.6819(3) 0.2987(4) 0.0641(19) Uani 1 1 d . . . . . C15 C 0.4881(19) 0.679(2) 0.0739(16) 0.168(17) Uani 0.604(12) 1 d . . P D 1 H15A H 0.4700 0.6342 0.0823 0.252 Uiso 0.604(12) 1 calc R U P D 1 H15B H 0.4492 0.6950 0.0321 0.252 Uiso 0.604(12) 1 calc R U P D 1 H15C H 0.4854 0.7078 0.1101 0.252 Uiso 0.604(12) 1 calc R U P D 1 C18 C 0.6200(17) 0.7685(10) 0.0677(12) 0.137(10) Uani 0.604(12) 1 d . . P D 1 H18A H 0.6017 0.7908 0.1025 0.205 Uiso 0.604(12) 1 calc R U P D 1 H18B H 0.5884 0.7870 0.0245 0.205 Uiso 0.604(12) 1 calc R U P D 1 H18C H 0.6826 0.7748 0.0755 0.205 Uiso 0.604(12) 1 calc R U P D 1 C20 C 0.6030(18) 0.6454(13) -0.0132(9) 0.144(11) Uani 0.604(12) 1 d . . P D 1 H20A H 0.6575 0.6608 -0.0200 0.216 Uiso 0.604(12) 1 calc R U P D 1 H20B H 0.5537 0.6622 -0.0487 0.216 Uiso 0.604(12) 1 calc R U P D 1 H20C H 0.6019 0.5973 -0.0135 0.216 Uiso 0.604(12) 1 calc R U P D 1 C14 C 0.9181(7) 0.7406(7) 0.3363(9) 0.165(7) Uani 1 1 d . . . . . H14A H 0.9330 0.7205 0.2989 0.248 Uiso 1 1 calc R U . C 1 H14B H 0.9390 0.7125 0.3754 0.248 Uiso 1 1 calc R U . C 1 H14C H 0.9456 0.7839 0.3456 0.248 Uiso 1 1 calc R U . C 1 F1 F 0.5308(15) 0.8145(5) 0.3063(6) 0.152(7) Uani 0.604(12) 1 d . . P D 1 C21A C 0.770(2) 0.608(2) 0.0367(18) 0.144(14) Uani 0.396(12) 1 d . U P D 2 H21D H 0.7790 0.5706 0.0107 0.216 Uiso 0.396(12) 1 calc R U P D 2 H21E H 0.8240 0.6335 0.0522 0.216 Uiso 0.396(12) 1 calc R U P D 2 H21F H 0.7240 0.6365 0.0090 0.216 Uiso 0.396(12) 1 calc R U P D 2 C19A C 0.695(3) 0.4910(18) 0.093(3) 0.152(18) Uani 0.396(12) 1 d . . P D 2 H19D H 0.6777 0.4736 0.1302 0.227 Uiso 0.396(12) 1 calc R U P D 2 H19E H 0.7412 0.4636 0.0851 0.227 Uiso 0.396(12) 1 calc R U P D 2 H19F H 0.6446 0.4907 0.0529 0.227 Uiso 0.396(12) 1 calc R U P D 2 C12A C 0.8689(17) 0.5928(13) 0.2191(13) 0.065(7) Uani 0.396(12) 1 d . U P D 2 Si2A Si 0.7356(10) 0.5779(7) 0.1112(6) 0.087(3) Uani 0.396(12) 1 d . . P D 2 Si1A Si 0.5720(12) 0.6483(9) 0.0604(10) 0.115(6) Uani 0.396(12) 1 d . . P D 2 C20A C 0.520(3) 0.593(2) -0.004(2) 0.157(15) Uani 0.396(12) 1 d . U P D 2 H20D H 0.5550 0.5879 -0.0346 0.235 Uiso 0.396(12) 1 calc R U P D 2 H20E H 0.4623 0.6103 -0.0284 0.235 Uiso 0.396(12) 1 calc R U P D 2 H20F H 0.5128 0.5500 0.0148 0.235 Uiso 0.396(12) 1 calc R U P D 2 C15A C 0.468(3) 0.6863(18) 0.083(2) 0.071(9) Uani 0.396(12) 1 d . U P D 2 H15D H 0.4247 0.7004 0.0423 0.107 Uiso 0.396(12) 1 calc R U P D 2 H15E H 0.4870 0.7242 0.1124 0.107 Uiso 0.396(12) 1 calc R U P D 2 H15F H 0.4432 0.6529 0.1053 0.107 Uiso 0.396(12) 1 calc R U P D 2 C18A C 0.609(3) 0.724(2) 0.014(2) 0.163(16) Uani 0.396(12) 1 d . U P D 2 H18D H 0.5981 0.7140 -0.0330 0.245 Uiso 0.396(12) 1 calc R U P D 2 H18E H 0.6716 0.7326 0.0340 0.245 Uiso 0.396(12) 1 calc R U P D 2 H18F H 0.5763 0.7638 0.0187 0.245 Uiso 0.396(12) 1 calc R U P D 2 F1A F 0.444(2) 0.8344(11) 0.3076(10) 0.154(11) Uani 0.396(12) 1 d . . P D 2 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 0.043(4) 0.048(4) 0.076(6) 0.007(4) 0.021(4) 0.009(4) C2 0.059(5) 0.038(4) 0.079(6) 0.016(4) 0.028(4) 0.007(4) C3 0.050(5) 0.056(5) 0.090(7) 0.008(5) 0.002(5) 0.004(4) C4 0.047(5) 0.080(6) 0.106(8) 0.028(6) 0.017(5) 0.010(5) C5 0.069(7) 0.062(6) 0.143(10) 0.039(7) -0.005(7) -0.015(5) C6 0.118(9) 0.054(6) 0.120(9) 0.014(6) -0.003(7) -0.026(6) C7 0.089(7) 0.096(8) 0.082(7) -0.022(6) 0.005(6) 0.016(6) C8 0.093(8) 0.059(6) 0.172(12) 0.044(7) 0.033(8) 0.010(6) C9 0.055(6) 0.103(9) 0.131(10) 0.036(8) 0.007(7) 0.015(6) C10 0.133(9) 0.092(8) 0.117(9) 0.020(7) 0.076(8) -0.015(7) C11 0.094(10) 0.122(10) 0.107(10) 0.006(8) -0.010(8) -0.002(8) C12 0.095(7) 0.096(7) 0.096(7) -0.001(2) 0.029(3) 0.002(2) C16 0.160(14) 0.051(7) 0.26(2) -0.049(10) 0.002(13) 0.008(8) C17 0.136(5) 0.133(5) 0.139(5) 0.004(2) 0.037(2) -0.003(2) C19 0.14(2) 0.18(3) 0.12(2) -0.07(2) 0.025(17) 0.08(2) Sn1 0.0447(3) 0.0470(3) 0.0639(4) 0.0101(3) 0.0252(2) 0.0086(2) Ag1 0.0415(5) 0.0576(5) 0.0735(6) 0.000 0.0257(4) 0.000 Sb1 0.1062(8) 0.0541(5) 0.0859(7) 0.000 -0.0041(6) 0.000 Si2 0.067(4) 0.102(5) 0.070(4) 0.007(3) 0.040(3) 0.025(3) C13 0.130(11) 0.103(9) 0.095(9) -0.019(7) 0.012(8) -0.002(8) Si1 0.102(6) 0.083(5) 0.063(4) 0.026(4) 0.044(4) 0.040(4) N1 0.050(4) 0.042(3) 0.059(4) 0.005(3) 0.018(3) 0.005(3) N3 0.095(6) 0.075(5) 0.071(5) 0.025(4) 0.046(4) 0.029(4) F3 0.211(8) 0.119(6) 0.131(6) -0.001(5) 0.085(6) 0.020(5) F2 0.142(8) 0.312(16) 0.242(12) -0.021(11) -0.029(8) 0.056(9) C21 0.131(8) 0.132(8) 0.132(8) 0.001(2) 0.040(3) 0.000(2) N2 0.042(4) 0.045(4) 0.103(5) 0.020(4) 0.017(4) 0.004(3) C15 0.09(2) 0.35(5) 0.075(17) 0.03(2) 0.028(14) 0.04(2) C18 0.18(2) 0.097(15) 0.14(2) 0.063(15) 0.057(17) 0.061(15) C20 0.19(3) 0.16(2) 0.069(13) 0.003(13) 0.022(14) 0.08(2) C14 0.059(7) 0.101(9) 0.30(2) 0.047(11) -0.004(10) -0.028(7) F1 0.31(2) 0.056(6) 0.090(8) 0.017(6) 0.063(12) -0.005(10) C21A 0.144(14) 0.144(14) 0.144(14) 0.000(2) 0.043(5) 0.000(2) C19A 0.19(5) 0.10(3) 0.18(4) -0.01(3) 0.08(4) 0.08(3) C12A 0.064(7) 0.066(7) 0.065(7) -0.001(2) 0.019(3) 0.001(2) Si2A 0.088(8) 0.098(8) 0.089(7) 0.015(6) 0.050(6) 0.028(6) Si1A 0.129(10) 0.142(14) 0.081(7) -0.020(9) 0.044(6) -0.042(9) C20A 0.157(15) 0.157(15) 0.157(15) -0.001(2) 0.046(5) 0.000(2) C15A 0.071(9) 0.071(9) 0.072(9) 0.000(2) 0.020(3) 0.001(2) C18A 0.163(16) 0.163(16) 0.163(16) 0.000(2) 0.048(5) 0.000(2) F1A 0.28(3) 0.100(15) 0.084(12) 0.000(11) 0.059(17) -0.089(19) 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' F F 0.0171 0.0103 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 C1 N1 110.2(7) . . N2 C1 C3 124.5(7) . . N1 C1 C3 125.3(7) . . N2 C1 Sn1 55.3(4) . . N1 C1 Sn1 56.3(4) . . C3 C1 Sn1 169.5(6) . . N1 C2 C8 114.0(7) . . N1 C2 C10 111.0(7) . . C8 C2 C10 111.0(8) . . N1 C2 C6 104.9(6) . . C8 C2 C6 108.1(8) . . C10 C2 C6 107.4(8) . . C7 C3 C4 119.0(9) . . C7 C3 C1 121.2(8) . . C4 C3 C1 119.8(9) . . C9 C4 C3 120.0(10) . . C9 C4 H4 120.0 . . C3 C4 H4 120.0 . . C16 C5 N2 112.9(9) . . C16 C5 C17 108.9(11) . . N2 C5 C17 104.1(10) . . C16 C5 C14 113.2(12) . . N2 C5 C14 110.1(9) . . C17 C5 C14 106.9(11) . . C2 C6 H6A 109.5 . . C2 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C2 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C3 C7 C13 121.1(10) . . C3 C7 H7 119.5 . . C13 C7 H7 119.5 . . C2 C8 H8A 109.5 . . C2 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C2 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C11 C9 C4 120.4(11) . . C11 C9 H9 119.8 . . C4 C9 H9 119.8 . . C2 C10 H10A 109.5 . . C2 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C2 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C9 C11 C13 121.5(12) . . C9 C11 H11 119.3 . . C13 C11 H11 119.3 . . Si2 C12 H12A 109.5 . . Si2 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . Si2 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C5 C16 H16A 109.5 . . C5 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . C5 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C5 C17 H17A 109.5 . . C5 C17 H17B 109.5 . . H17A C17 H17B 109.5 . . C5 C17 H17C 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . Si2 C19 H19A 109.5 . . Si2 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . Si2 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . N3 Sn1 N2 109.7(3) . . N3 Sn1 N1 109.2(2) . . N2 Sn1 N1 60.9(2) . . N3 Sn1 C1 117.1(3) . . N2 Sn1 C1 30.6(2) . . N1 Sn1 C1 30.9(2) . . N3 Sn1 Ag1 127.8(2) . . N2 Sn1 Ag1 117.60(19) . . N1 Sn1 Ag1 112.17(15) . . C1 Sn1 Ag1 114.83(17) . . Sn1 Ag1 Sn1 147.57(4) . 2_655 F1 Sb1 F1 76.4(8) . 2_655 F1 Sb1 F2 74.3(8) . . F1 Sb1 F2 116.7(9) 2_655 . F1 Sb1 F2 116.7(9) . 2_655 F1 Sb1 F2 74.3(8) 2_655 2_655 F2 Sb1 F2 166.9(9) . 2_655 F1 Sb1 F3 157.1(8) . 2_655 F1 Sb1 F3 100.8(5) 2_655 2_655 F2 Sb1 F3 87.3(5) . 2_655 F2 Sb1 F3 83.5(5) 2_655 2_655 F1 Sb1 F3 100.8(5) . . F1 Sb1 F3 157.1(8) 2_655 . F2 Sb1 F3 83.5(5) . . F2 Sb1 F3 87.3(5) 2_655 . F3 Sb1 F3 90.3(5) 2_655 . F2 Sb1 F1A 109.4(10) . . F2 Sb1 F1A 77.7(10) 2_655 . F3 Sb1 F1A 158.5(11) 2_655 . F3 Sb1 F1A 78.8(8) . . F2 Sb1 F1A 77.7(10) . 2_655 F2 Sb1 F1A 109.4(10) 2_655 2_655 F3 Sb1 F1A 78.7(8) 2_655 2_655 F3 Sb1 F1A 158.5(11) . 2_655 F1A Sb1 F1A 117.1(17) . 2_655 C12 Si2 N3 122.5(9) . . C12 Si2 C21 110.2(12) . . N3 Si2 C21 111.6(8) . . C12 Si2 C19 96.4(12) . . N3 Si2 C19 105.2(9) . . C21 Si2 C19 109.0(13) . . C11 C13 C7 118.1(12) . . C11 C13 H13 120.9 . . C7 C13 H13 120.9 . . C15 Si1 N3 113.9(13) . . C15 Si1 C20 113.4(15) . . N3 Si1 C20 111.5(8) . . C15 Si1 C18 100.6(16) . . N3 Si1 C18 112.4(10) . . C20 Si1 C18 104.1(12) . . C1 N1 C2 129.8(7) . . C1 N1 Sn1 92.8(4) . . C2 N1 Sn1 133.0(5) . . Si1 N3 Si2 121.5(5) . . Si2A N3 Si1A 106.0(10) . . Si2A N3 Sn1 131.4(5) . . Si1 N3 Sn1 113.9(4) . . Si2 N3 Sn1 120.2(4) . . Si1A N3 Sn1 116.0(7) . . Si2 C21 H21A 109.5 . . Si2 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . Si2 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C1 N2 C5 129.7(8) . . C1 N2 Sn1 94.1(5) . . C5 N2 Sn1 132.9(5) . . Si1 C15 H15A 109.5 . . Si1 C15 H15B 109.5 . . H15A C15 H15B 109.5 . . Si1 C15 H15C 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . Si1 C18 H18A 109.5 . . Si1 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . Si1 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . Si1 C20 H20A 109.5 . . Si1 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . Si1 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C5 C14 H14A 109.5 . . C5 C14 H14B 109.5 . . H14A C14 H14B 109.5 . . C5 C14 H14C 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . Si2A C21A H21D 109.5 . . Si2A C21A H21E 109.5 . . H21D C21A H21E 109.5 . . Si2A C21A H21F 109.5 . . H21D C21A H21F 109.5 . . H21E C21A H21F 109.5 . . Si2A C19A H19D 109.5 . . Si2A C19A H19E 109.5 . . H19D C19A H19E 109.5 . . Si2A C19A H19F 109.5 . . H19D C19A H19F 109.5 . . H19E C19A H19F 109.5 . . N3 Si2A C19A 118.3(14) . . N3 Si2A C21A 111.9(14) . . C19A Si2A C21A 107(2) . . C20A Si1A N3 129.9(18) . . C20A Si1A C18A 105(2) . . N3 Si1A C18A 103.3(15) . . C20A Si1A C15A 101(2) . . N3 Si1A C15A 113.0(16) . . C18A Si1A C15A 102(2) . . Si1A C20A H20D 109.5 . . Si1A C20A H20E 109.5 . . H20D C20A H20E 109.5 . . Si1A C20A H20F 109.5 . . H20D C20A H20F 109.5 . . H20E C20A H20F 109.5 . . Si1A C15A H15D 109.5 . . Si1A C15A H15E 109.5 . . H15D C15A H15E 109.5 . . Si1A C15A H15F 109.5 . . H15D C15A H15F 109.5 . . H15E C15A H15F 109.5 . . Si1A C18A H18D 109.5 . . Si1A C18A H18E 109.5 . . H18D C18A H18E 109.5 . . Si1A C18A H18F 109.5 . . H18D C18A H18F 109.5 . . H18E C18A H18F 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N2 1.333(9) . C1 N1 1.342(9) . C1 C3 1.488(12) . C1 Sn1 2.613(8) . C2 N1 1.471(9) . C2 C8 1.492(11) . C2 C10 1.512(12) . C2 C6 1.527(12) . C3 C7 1.383(13) . C3 C4 1.394(11) . C4 C9 1.383(14) . C4 H4 0.9300 . C5 C16 1.476(18) . C5 N2 1.497(12) . C5 C17 1.498(15) . C5 C14 1.558(14) . C6 H6A 0.9600 . C6 H6B 0.9600 . C6 H6C 0.9600 . C7 C13 1.399(15) . C7 H7 0.9300 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C9 C11 1.358(16) . C9 H9 0.9300 . C10 H10A 0.9600 . C10 H10B 0.9600 . C10 H10C 0.9600 . C11 C13 1.386(17) . C11 H11 0.9300 . C12 Si2 1.50(2) . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C17 H17A 0.9600 . C17 H17B 0.9600 . C17 H17C 0.9600 . C19 Si2 1.91(2) . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . Sn1 N3 2.036(7) . Sn1 N2 2.153(7) . Sn1 N1 2.176(6) . Sn1 Ag1 2.6217(8) . Ag1 Sn1 2.6217(8) 2_655 Sb1 F1 1.816(11) . Sb1 F1 1.816(11) 2_655 Sb1 F2 1.827(10) . Sb1 F2 1.827(10) 2_655 Sb1 F3 1.853(7) 2_655 Sb1 F3 1.853(7) . Sb1 F1A 1.973(19) . Sb1 F1A 1.973(19) 2_655 Si2 N3 1.838(9) . Si2 C21 1.88(2) . C13 H13 0.9300 . Si1 C15 1.72(3) . Si1 N3 1.725(11) . Si1 C20 1.84(2) . Si1 C18 1.88(2) . N3 Si2A 1.722(12) . N3 Si1A 1.85(2) . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . C15 H15A 0.9600 . C15 H15B 0.9600 . C15 H15C 0.9600 . C18 H18A 0.9600 . C18 H18B 0.9600 . C18 H18C 0.9600 . C20 H20A 0.9600 . C20 H20B 0.9600 . C20 H20C 0.9600 . C14 H14A 0.9600 . C14 H14B 0.9600 . C14 H14C 0.9600 . C21A Si2A 1.88(4) . C21A H21D 0.9600 . C21A H21E 0.9600 . C21A H21F 0.9600 . C19A Si2A 1.85(4) . C19A H19D 0.9600 . C19A H19E 0.9600 . C19A H19F 0.9600 . Si1A C20A 1.74(4) . Si1A C18A 1.98(4) . Si1A C15A 1.98(4) . C20A H20D 0.9600 . C20A H20E 0.9600 . C20A H20F 0.9600 . C15A H15D 0.9600 . C15A H15E 0.9600 . C15A H15F 0.9600 . C18A H18D 0.9600 . C18A H18E 0.9600 . C18A H18F 0.9600 .