#------------------------------------------------------------------------------ #$Date: 2019-10-11 03:39:08 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219264 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234529.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_7234529 loop_ _publ_author_name 'Nayak, Biswajit' 'Halder, Senjuti' 'De, Sagnik' 'Das, Gopal' _publ_section_title ; Binding Consistency of Anion by Effect of Aromatic Meta-Substitution of Bis-urea Receptors: Entrapment of Hexafluorosilicate Clusters ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE01485C _journal_year 2019 _chemical_formula_moiety '2(C22 H16 N6 O2), 2(C16 H36 N), F6 Si' _chemical_formula_sum 'C76 H104 F6 N14 O4 Si' _chemical_formula_weight 1419.82 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-09-13 deposited with the CCDC. 2019-10-10 downloaded from the CCDC. ; _cell_angle_alpha 96.1210(10) _cell_angle_beta 96.470(2) _cell_angle_gamma 114.2000(10) _cell_formula_units_Z 1 _cell_length_a 11.3980(3) _cell_length_b 11.8157(3) _cell_length_c 16.3102(4) _cell_measurement_reflns_used 6774 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 18.1650 _cell_measurement_theta_min 3.0760 _cell_volume 1962.28(9) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 29413 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.049 _diffrn_reflns_theta_max 25.049 _diffrn_reflns_theta_min 1.275 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.202 _exptl_crystal_description needle _exptl_crystal_F_000 758.0 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_transmission_factor_max 0.983 _exptl_transmission_factor_min 0.972 _refine_diff_density_max 0.203 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 468 _refine_ls_number_reflns 6836 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.876 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0478 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0311P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1333 _refine_ls_wR_factor_ref 0.1476 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4399 _reflns_number_total 6836 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01485c2.cif _cod_data_source_block L3-SiF6 _cod_database_code 7234529 _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 ; 1.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 11.3980 11.8157 16.3102 96.121 96.470 114.200 ZERR 1.00 0.0003 0.0003 0.0004 0.001 0.002 0.001 LATT 1 SFAC C H N O F Si UNIT 76 96 14 4 6 1 OMIT -3 50.1 L.S. 10 ACTA BOND FMAP 2 PLAN 5 EADP F4 F3 EADP F6 F1 DFIX 1.67 0.001 SI1 F6 SI1 F4 TEMP 23.000 WGHT 0.100000 0.031063 FVAR 0.28417 0.90465 MOLE 1 SI1 6 0.500000 0.500000 0.500000 10.50000 0.06149 0.04586 = 0.04478 0.00255 0.01631 0.02783 F2 5 0.439766 0.458715 0.397827 11.00000 0.11753 0.09606 = 0.04895 0.00035 0.00721 0.04578 PART 1 F1 5 0.625381 0.471387 0.477837 21.00000 0.08830 0.08889 = 0.08887 0.02646 0.04217 0.05902 F3 5 0.579745 0.649984 0.487130 21.00000 0.10630 0.05101 = 0.08786 0.01278 0.05045 0.03533 PART 2 F4 5 0.523374 0.645302 0.486337 -21.00000 0.10630 0.05101 = 0.08786 0.01278 0.05045 0.03533 F6 5 0.657566 0.535874 0.499107 -21.00000 0.08830 0.08889 = 0.08887 0.02646 0.04217 0.05902 PART 0 C9 1 0.531029 0.925656 0.551015 11.00000 0.07721 0.04280 = 0.04047 0.00063 0.00374 0.03043 C8 1 0.582863 0.863719 0.683760 11.00000 0.08148 0.04765 = 0.04768 0.00540 0.00692 0.03322 C10 1 0.580828 0.946375 0.478058 11.00000 0.08564 0.06456 = 0.04731 0.00547 0.01465 0.04738 AFIX 43 H10 2 0.635443 0.910153 0.462615 11.00000 -1.20000 AFIX 0 C11 1 0.449913 0.979367 0.572250 11.00000 0.08695 0.06456 = 0.04163 0.00735 0.01576 0.04227 AFIX 43 H11 2 0.415213 0.965573 0.621144 11.00000 -1.20000 AFIX 0 C6 1 0.607711 0.753116 0.800214 11.00000 0.06799 0.05806 = 0.04899 0.00977 0.00388 0.03337 C5 1 0.590359 0.635829 0.817230 11.00000 0.08511 0.06739 = 0.06122 0.01326 0.01065 0.04981 AFIX 43 H5 2 0.572819 0.570949 0.773353 11.00000 -1.20000 AFIX 0 C7 1 0.629721 0.846708 0.865738 11.00000 0.12985 0.05624 = 0.05147 0.00607 0.00029 0.03886 AFIX 43 H7 2 0.640330 0.926009 0.855566 11.00000 -1.20000 AFIX 0 C4 1 0.598721 0.613868 0.898338 11.00000 0.11545 0.07686 = 0.07033 0.02558 0.01570 0.05983 AFIX 43 H4 2 0.588193 0.534666 0.908693 11.00000 -1.20000 AFIX 0 C2 1 0.636045 0.822623 0.946822 11.00000 0.13020 0.07379 = 0.05155 0.00907 0.00261 0.04503 C3 1 0.622113 0.706190 0.963373 11.00000 0.11543 0.08519 = 0.05698 0.01874 0.00365 0.05198 AFIX 43 H3 2 0.628646 0.691257 1.018171 11.00000 -1.20000 AFIX 0 C1 1 0.653286 0.919103 1.013735 11.00000 0.28977 0.08704 = 0.05084 0.00715 0.00521 0.08352 N1 3 0.666166 0.995597 1.067019 11.00000 0.50377 0.11936 = 0.06122 0.00504 0.02600 0.14931 N3 3 0.559119 0.844070 0.598890 11.00000 0.09603 0.05291 = 0.04198 0.00307 0.00765 0.04339 AFIX 43 H3N 2 0.561276 0.778045 0.572621 11.00000 -1.20000 AFIX 0 N2 3 0.598819 0.767730 0.715895 11.00000 0.09073 0.05533 = 0.04712 0.00562 0.00756 0.04225 AFIX 43 H2N 2 0.603902 0.710710 0.680953 11.00000 -1.20000 AFIX 0 O1 4 0.587980 0.956688 0.726597 11.00000 0.13777 0.05740 = 0.04649 0.00069 0.00402 0.05570 C17 1 0.738641 0.476115 0.270042 11.00000 0.05199 0.06648 = 0.05029 0.00118 0.00365 0.02543 C18 1 0.756980 0.505253 0.191219 11.00000 0.06794 0.07220 = 0.04999 0.00273 0.00282 0.03702 AFIX 43 H18 2 0.776831 0.586571 0.181174 11.00000 -1.20000 AFIX 0 C13 1 0.745545 0.412461 0.127518 11.00000 0.07341 0.08788 = 0.04948 -0.00479 -0.00343 0.04671 C12 1 0.766260 0.444636 0.046422 11.00000 0.12423 0.11011 = 0.05193 -0.00837 -0.00083 0.07752 C16 1 0.709162 0.354843 0.283020 11.00000 0.07353 0.07299 = 0.06848 0.01472 0.00911 0.03242 AFIX 43 H16 2 0.697453 0.334324 0.335915 11.00000 -1.20000 AFIX 0 C14 1 0.715018 0.291078 0.140585 11.00000 0.08880 0.08242 = 0.07484 -0.01131 0.00343 0.04478 AFIX 43 H14 2 0.706964 0.229101 0.097213 11.00000 -1.20000 AFIX 0 C15 1 0.696950 0.264070 0.218400 11.00000 0.09865 0.07124 = 0.09785 0.01098 0.01492 0.04288 AFIX 43 H15 2 0.675874 0.182394 0.228074 11.00000 -1.20000 AFIX 0 N4 3 0.782634 0.470251 -0.018491 11.00000 0.20968 0.16445 = 0.05293 0.00545 0.01826 0.12460 C19 1 0.831299 0.688601 0.349740 11.00000 0.05425 0.07113 = 0.04359 0.00748 0.00824 0.02843 O2 4 0.908868 0.732988 0.303455 11.00000 0.06972 0.07668 = 0.05274 0.00296 0.02301 0.02538 C21 1 0.913670 0.879852 0.457522 11.00000 0.05548 0.06470 = 0.04344 0.00591 0.01007 0.02829 C20 1 0.906780 0.921293 0.538296 11.00000 0.06274 0.07267 = 0.04639 0.01054 0.02110 0.02527 AFIX 43 H20 2 0.842956 0.868155 0.564817 11.00000 -1.20000 AFIX 0 C22 1 1.008274 0.960855 0.419168 11.00000 0.06978 0.07455 = 0.04188 0.00447 0.01778 0.02605 AFIX 43 H22 2 1.014668 0.935786 0.364472 11.00000 -1.20000 AFIX 0 N6 3 0.823617 0.756878 0.420131 11.00000 0.05966 0.06885 = 0.04796 0.00344 0.01859 0.02006 AFIX 43 H6N 2 0.757345 0.721402 0.444016 11.00000 -1.20000 AFIX 0 N5 3 0.745002 0.565099 0.336754 11.00000 0.06697 0.06840 = 0.04813 0.00165 0.01573 0.01976 AFIX 43 H5N 2 0.691544 0.540263 0.371240 11.00000 -1.20000 AFIX 0 C31 1 0.248093 0.659005 0.365580 11.00000 0.07381 0.08211 = 0.04962 0.00178 0.00583 0.04125 AFIX 23 H31A 2 0.272729 0.594321 0.382339 11.00000 -1.20000 H31B 2 0.323032 0.739466 0.384493 11.00000 -1.20000 AFIX 0 C27 1 0.338146 0.643272 0.236806 11.00000 0.07145 0.07266 = 0.06032 -0.00245 0.01431 0.03997 AFIX 23 H27A 2 0.360521 0.579124 0.257007 11.00000 -1.20000 H27B 2 0.315683 0.621336 0.176295 11.00000 -1.20000 AFIX 0 C28 1 0.456855 0.765473 0.258204 11.00000 0.07968 0.06894 = 0.07439 0.00388 0.02269 0.03817 AFIX 23 H28A 2 0.480693 0.789120 0.318596 11.00000 -1.20000 H28B 2 0.437290 0.830254 0.236498 11.00000 -1.20000 AFIX 0 C35 1 0.108135 0.508991 0.236014 11.00000 0.06341 0.08212 = 0.06320 0.00085 0.00451 0.03232 AFIX 23 H35A 2 0.027730 0.508798 0.250316 11.00000 -1.20000 H35B 2 0.098567 0.497075 0.175452 11.00000 -1.20000 AFIX 0 C23 1 0.177461 0.737610 0.244852 11.00000 0.08651 0.08831 = 0.06158 0.01558 0.02162 0.05645 AFIX 23 H23A 2 0.100016 0.728811 0.268007 11.00000 -1.20000 H23B 2 0.246425 0.819140 0.270618 11.00000 -1.20000 AFIX 0 C29 1 0.569566 0.758403 0.222976 11.00000 0.07999 0.08153 = 0.10260 0.00979 0.02994 0.03772 AFIX 23 H29A 2 0.546180 0.737984 0.162453 11.00000 -1.20000 H29B 2 0.585384 0.690341 0.242478 11.00000 -1.20000 AFIX 0 C32 1 0.137622 0.658156 0.409883 11.00000 0.08292 0.12087 = 0.05686 0.02020 0.02179 0.05260 AFIX 23 H32A 2 0.115860 0.726009 0.396412 11.00000 -1.20000 H32B 2 0.060948 0.579381 0.389817 11.00000 -1.20000 AFIX 0 C33 1 0.172956 0.673201 0.501837 11.00000 0.09145 0.11512 = 0.06456 0.00159 0.01616 0.05211 AFIX 23 H33A 2 0.260151 0.740334 0.519679 11.00000 -1.20000 H33B 2 0.175252 0.596194 0.515617 11.00000 -1.20000 AFIX 0 C30 1 0.693266 0.876999 0.245942 11.00000 0.08104 0.09639 = 0.10470 0.02908 0.02326 0.03539 AFIX 137 H30A 2 0.678909 0.945026 0.226686 11.00000 -1.50000 H30B 2 0.760486 0.866094 0.220212 11.00000 -1.50000 H30C 2 0.719729 0.895928 0.305656 11.00000 -1.50000 AFIX 0 C34 1 0.081803 0.702359 0.549760 11.00000 0.11721 0.15741 = 0.06661 0.02510 0.03189 0.08391 AFIX 137 H34A 2 0.093263 0.786865 0.546721 11.00000 -1.50000 H34B 2 0.100115 0.694324 0.607206 11.00000 -1.50000 H34C 2 -0.006594 0.644641 0.526173 11.00000 -1.50000 AFIX 0 C24 1 0.149321 0.738112 0.152355 11.00000 0.13013 0.11367 = 0.06959 0.02351 0.02409 0.07632 AFIX 23 H24A 2 0.229992 0.764879 0.129956 11.00000 -1.20000 H24B 2 0.091299 0.653676 0.123723 11.00000 -1.20000 AFIX 0 C36 1 0.122094 0.397273 0.264714 11.00000 0.06863 0.08033 = 0.08798 0.01468 0.01071 0.02697 AFIX 23 H36A 2 0.211616 0.408801 0.265963 11.00000 -1.20000 H36B 2 0.103829 0.393328 0.321270 11.00000 -1.20000 AFIX 0 C25 1 0.086843 0.826095 0.137348 11.00000 0.14164 0.13586 = 0.09653 0.05003 0.02427 0.07396 AFIX 23 H25A 2 0.008757 0.800979 0.162538 11.00000 -1.20000 H25B 2 0.146673 0.910522 0.165033 11.00000 -1.20000 AFIX 0 C37 1 0.033931 0.277195 0.210187 11.00000 0.09757 0.08543 = 0.12548 0.00657 -0.00802 0.03141 AFIX 23 H37A 2 -0.054544 0.269666 0.206860 11.00000 -1.20000 H37B 2 0.055182 0.281843 0.154338 11.00000 -1.20000 AFIX 0 C26 1 0.051114 0.828431 0.047003 11.00000 0.23549 0.21603 = 0.12482 0.07914 0.00380 0.11601 AFIX 137 H26A 2 0.128790 0.859997 0.022607 11.00000 -1.50000 H26B 2 0.007270 0.882097 0.041532 11.00000 -1.50000 H26C 2 -0.005734 0.744704 0.018669 11.00000 -1.50000 AFIX 0 C38 1 0.035242 0.161447 0.234320 11.00000 0.10540 0.09247 = 0.18948 0.02717 0.01568 0.02681 AFIX 137 H38A 2 0.116949 0.159372 0.227526 11.00000 -1.50000 H38B 2 -0.034951 0.089656 0.199425 11.00000 -1.50000 H38C 2 0.024585 0.159636 0.291789 11.00000 -1.50000 AFIX 0 N7 3 0.217303 0.637454 0.270586 11.00000 0.06713 0.07204 = 0.05027 0.00148 0.01083 0.03945 HKLF 4 REM 1 in P-1 REM R1 = 0.0478 for 4399 Fo > 4sig(Fo) and 0.0724 for all 6836 data REM 468 parameters refined using 2 restraints END WGHT 0.0885 0.0000 REM Highest difference peak 0.203, deepest hole -0.247, 1-sigma level 0.043 Q1 1 -0.0367 0.2820 0.1618 11.00000 0.05 0.20 Q2 1 -0.0238 0.8002 0.1065 11.00000 0.05 0.19 Q3 1 0.1767 0.7605 0.4718 11.00000 0.05 0.19 Q4 1 0.6909 0.3982 -0.0215 11.00000 0.05 0.16 Q5 1 0.2021 0.4179 0.2996 11.00000 0.05 0.15 ; _shelx_res_checksum 80074 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 Si1 Si 0.5000 0.5000 0.5000 0.0488(2) Uani 1 2 d DS . P . . F2 F 0.43977(14) 0.45871(13) 0.39783(7) 0.0890(4) Uani 1 1 d . . . . . F1 F 0.6254(2) 0.4714(3) 0.47784(14) 0.0783(7) Uani 0.905(7) 1 d . . P A 1 F3 F 0.5797(3) 0.64998(12) 0.48713(11) 0.0782(7) Uani 0.905(7) 1 d . . P A 1 F4 F 0.523(3) 0.6453(9) 0.4863(13) 0.0782(7) Uani 0.095(7) 1 d D . P A 2 F6 F 0.6576(7) 0.536(2) 0.4991(13) 0.0783(7) Uani 0.095(7) 1 d D . P A 2 C9 C 0.53103(19) 0.92566(16) 0.55102(11) 0.0529(5) Uani 1 1 d . . . . . C8 C 0.5829(2) 0.86372(18) 0.68376(12) 0.0576(5) Uani 1 1 d . . . . . C10 C 0.5808(2) 0.94638(19) 0.47806(11) 0.0607(5) Uani 1 1 d . . . . . H10 H 0.6354 0.9102 0.4626 0.073 Uiso 1 1 calc R U . . . C11 C 0.4499(2) 0.97937(19) 0.57225(11) 0.0608(5) Uani 1 1 d . . . . . H11 H 0.4152 0.9656 0.6211 0.073 Uiso 1 1 calc R U . . . C6 C 0.60771(19) 0.75312(18) 0.80021(11) 0.0566(5) Uani 1 1 d . . . . . C5 C 0.5904(2) 0.6358(2) 0.81723(13) 0.0654(6) Uani 1 1 d . . . . . H5 H 0.5728 0.5709 0.7734 0.078 Uiso 1 1 calc R U . . . C7 C 0.6297(3) 0.8467(2) 0.86574(13) 0.0810(7) Uani 1 1 d . . . . . H7 H 0.6403 0.9260 0.8556 0.097 Uiso 1 1 calc R U . . . C4 C 0.5987(3) 0.6139(2) 0.89834(14) 0.0802(7) Uani 1 1 d . . . . . H4 H 0.5882 0.5347 0.9087 0.096 Uiso 1 1 calc R U . . . C2 C 0.6360(3) 0.8226(2) 0.94682(13) 0.0859(7) Uani 1 1 d . . . . . C3 C 0.6221(3) 0.7062(2) 0.96337(14) 0.0832(7) Uani 1 1 d . . . . . H3 H 0.6286 0.6913 1.0182 0.100 Uiso 1 1 calc R U . . . C1 C 0.6533(5) 0.9191(3) 1.01374(18) 0.1439(16) Uani 1 1 d . . . . . N1 N 0.6662(6) 0.9956(3) 1.06702(17) 0.225(3) Uani 1 1 d . . . . . N3 N 0.55912(17) 0.84407(14) 0.59889(9) 0.0605(4) Uani 1 1 d . . . . . H3N H 0.5613 0.7780 0.5726 0.073 Uiso 1 1 calc R U . . . N2 N 0.59882(17) 0.76773(15) 0.71589(9) 0.0613(4) Uani 1 1 d . . . . . H2N H 0.6039 0.7107 0.6810 0.074 Uiso 1 1 calc R U . . . O1 O 0.58798(17) 0.95669(13) 0.72660(8) 0.0775(5) Uani 1 1 d . . . . . C17 C 0.73864(18) 0.47611(19) 0.27004(12) 0.0573(5) Uani 1 1 d . . . . . C18 C 0.75698(19) 0.5053(2) 0.19122(12) 0.0622(5) Uani 1 1 d . . . . . H18 H 0.7768 0.5866 0.1812 0.075 Uiso 1 1 calc R U . . . C13 C 0.7455(2) 0.4125(2) 0.12752(12) 0.0686(6) Uani 1 1 d . . . . . C12 C 0.7663(3) 0.4446(3) 0.04642(15) 0.0893(8) Uani 1 1 d . . . . . C16 C 0.7092(2) 0.3548(2) 0.28302(14) 0.0713(6) Uani 1 1 d . . . . . H16 H 0.6975 0.3343 0.3359 0.086 Uiso 1 1 calc R U . . . C14 C 0.7150(2) 0.2911(2) 0.14058(16) 0.0821(7) Uani 1 1 d . . . . . H14 H 0.7070 0.2291 0.0972 0.099 Uiso 1 1 calc R U . . . C15 C 0.6969(3) 0.2641(2) 0.21840(18) 0.0875(7) Uani 1 1 d . . . . . H15 H 0.6759 0.1824 0.2281 0.105 Uiso 1 1 calc R U . . . N4 N 0.7826(3) 0.4703(3) -0.01849(14) 0.1286(10) Uani 1 1 d . . . . . C19 C 0.83130(19) 0.6886(2) 0.34974(11) 0.0560(5) Uani 1 1 d . . . . . O2 O 0.90887(14) 0.73299(13) 0.30346(8) 0.0679(4) Uani 1 1 d . . . . . C21 C 0.91367(18) 0.87985(18) 0.45752(11) 0.0538(5) Uani 1 1 d . . . . . C20 C 0.90678(19) 0.92129(19) 0.53830(11) 0.0608(5) Uani 1 1 d . . . . . H20 H 0.8430 0.8682 0.5648 0.073 Uiso 1 1 calc R U . . . C22 C 1.0083(2) 0.9609(2) 0.41917(12) 0.0634(6) Uani 1 1 d . . . . . H22 H 1.0147 0.9358 0.3645 0.076 Uiso 1 1 calc R U . . . N6 N 0.82362(16) 0.75688(15) 0.42013(9) 0.0610(4) Uani 1 1 d . . . . . H6N H 0.7573 0.7214 0.4440 0.073 Uiso 1 1 calc R U . . . N5 N 0.74500(16) 0.56510(16) 0.33675(9) 0.0644(5) Uani 1 1 d . . . . . H5N H 0.6915 0.5403 0.3712 0.077 Uiso 1 1 calc R U . . . C31 C 0.2481(2) 0.6590(2) 0.36558(12) 0.0670(6) Uani 1 1 d . . . . . H31A H 0.2727 0.5943 0.3823 0.080 Uiso 1 1 calc R U . . . H31B H 0.3230 0.7395 0.3845 0.080 Uiso 1 1 calc R U . . . C27 C 0.3381(2) 0.6433(2) 0.23681(13) 0.0659(6) Uani 1 1 d . . . . . H27A H 0.3605 0.5791 0.2570 0.079 Uiso 1 1 calc R U . . . H27B H 0.3157 0.6213 0.1763 0.079 Uiso 1 1 calc R U . . . C28 C 0.4569(2) 0.7655(2) 0.25820(14) 0.0720(6) Uani 1 1 d . . . . . H28A H 0.4807 0.7891 0.3186 0.086 Uiso 1 1 calc R U . . . H28B H 0.4373 0.8303 0.2365 0.086 Uiso 1 1 calc R U . . . C35 C 0.1081(2) 0.5090(2) 0.23601(13) 0.0706(6) Uani 1 1 d . . . . . H35A H 0.0277 0.5088 0.2503 0.085 Uiso 1 1 calc R U . . . H35B H 0.0986 0.4971 0.1755 0.085 Uiso 1 1 calc R U . . . C23 C 0.1775(2) 0.7376(2) 0.24485(13) 0.0713(6) Uani 1 1 d . . . . . H23A H 0.1000 0.7288 0.2680 0.086 Uiso 1 1 calc R U . . . H23B H 0.2464 0.8191 0.2706 0.086 Uiso 1 1 calc R U . . . C29 C 0.5696(2) 0.7584(2) 0.22298(17) 0.0862(7) Uani 1 1 d . . . . . H29A H 0.5462 0.7380 0.1625 0.103 Uiso 1 1 calc R U . . . H29B H 0.5854 0.6903 0.2425 0.103 Uiso 1 1 calc R U . . . C32 C 0.1376(2) 0.6582(3) 0.40988(13) 0.0826(7) Uani 1 1 d . . . . . H32A H 0.1159 0.7260 0.3964 0.099 Uiso 1 1 calc R U . . . H32B H 0.0609 0.5794 0.3898 0.099 Uiso 1 1 calc R U . . . C33 C 0.1730(3) 0.6732(3) 0.50184(14) 0.0885(7) Uani 1 1 d . . . . . H33A H 0.2602 0.7403 0.5197 0.106 Uiso 1 1 calc R U . . . H33B H 0.1753 0.5962 0.5156 0.106 Uiso 1 1 calc R U . . . C30 C 0.6933(2) 0.8770(2) 0.24594(17) 0.0933(8) Uani 1 1 d . . . . . H30A H 0.6789 0.9450 0.2267 0.140 Uiso 1 1 calc R U . . . H30B H 0.7605 0.8661 0.2202 0.140 Uiso 1 1 calc R U . . . H30C H 0.7197 0.8959 0.3057 0.140 Uiso 1 1 calc R U . . . C34 C 0.0818(3) 0.7024(3) 0.54976(15) 0.1033(9) Uani 1 1 d . . . . . H34A H 0.0933 0.7869 0.5467 0.155 Uiso 1 1 calc R U . . . H34B H 0.1001 0.6943 0.6072 0.155 Uiso 1 1 calc R U . . . H34C H -0.0066 0.6446 0.5262 0.155 Uiso 1 1 calc R U . . . C24 C 0.1493(3) 0.7381(3) 0.15236(15) 0.0950(8) Uani 1 1 d . . . . . H24A H 0.2300 0.7649 0.1300 0.114 Uiso 1 1 calc R U . . . H24B H 0.0913 0.6537 0.1237 0.114 Uiso 1 1 calc R U . . . C36 C 0.1221(2) 0.3973(2) 0.26471(15) 0.0808(7) Uani 1 1 d . . . . . H36A H 0.2116 0.4088 0.2660 0.097 Uiso 1 1 calc R U . . . H36B H 0.1038 0.3933 0.3213 0.097 Uiso 1 1 calc R U . . . C25 C 0.0868(3) 0.8261(3) 0.13735(19) 0.1169(10) Uani 1 1 d . . . . . H25A H 0.0088 0.8010 0.1625 0.140 Uiso 1 1 calc R U . . . H25B H 0.1467 0.9105 0.1650 0.140 Uiso 1 1 calc R U . . . C37 C 0.0339(3) 0.2772(3) 0.2102(2) 0.1086(9) Uani 1 1 d . . . . . H37A H -0.0545 0.2697 0.2069 0.130 Uiso 1 1 calc R U . . . H37B H 0.0552 0.2818 0.1543 0.130 Uiso 1 1 calc R U . . . C26 C 0.0511(5) 0.8284(5) 0.0470(3) 0.1837(19) Uani 1 1 d . . . . . H26A H 0.1288 0.8600 0.0226 0.276 Uiso 1 1 calc R U . . . H26B H 0.0073 0.8821 0.0415 0.276 Uiso 1 1 calc R U . . . H26C H -0.0057 0.7447 0.0187 0.276 Uiso 1 1 calc R U . . . C38 C 0.0352(3) 0.1614(3) 0.2343(3) 0.1349(12) Uani 1 1 d . . . . . H38A H 0.1169 0.1594 0.2275 0.202 Uiso 1 1 calc R U . . . H38B H -0.0350 0.0897 0.1994 0.202 Uiso 1 1 calc R U . . . H38C H 0.0246 0.1596 0.2918 0.202 Uiso 1 1 calc R U . . . N7 N 0.21730(16) 0.63745(16) 0.27059(10) 0.0605(4) 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 Si1 0.0615(4) 0.0459(4) 0.0448(4) 0.0026(3) 0.0163(3) 0.0278(3) F2 0.1175(10) 0.0961(10) 0.0490(7) 0.0003(6) 0.0072(6) 0.0458(8) F1 0.0883(10) 0.0889(19) 0.0889(12) 0.0265(12) 0.0422(9) 0.0590(12) F3 0.1063(17) 0.0510(7) 0.0879(9) 0.0128(6) 0.0504(11) 0.0353(8) F4 0.1063(17) 0.0510(7) 0.0879(9) 0.0128(6) 0.0504(11) 0.0353(8) F6 0.0883(10) 0.0889(19) 0.0889(12) 0.0265(12) 0.0422(9) 0.0590(12) C9 0.0772(13) 0.0428(10) 0.0405(10) 0.0006(8) 0.0037(9) 0.0304(9) C8 0.0815(14) 0.0476(11) 0.0477(11) 0.0054(9) 0.0069(9) 0.0332(10) C10 0.0856(14) 0.0646(12) 0.0473(11) 0.0055(9) 0.0146(10) 0.0474(11) C11 0.0870(14) 0.0646(12) 0.0416(10) 0.0073(9) 0.0158(9) 0.0423(11) C6 0.0680(12) 0.0581(12) 0.0490(11) 0.0098(9) 0.0039(9) 0.0334(10) C5 0.0851(15) 0.0674(13) 0.0612(13) 0.0133(10) 0.0107(10) 0.0498(12) C7 0.130(2) 0.0562(13) 0.0515(12) 0.0061(10) 0.0003(12) 0.0389(13) C4 0.1154(19) 0.0769(16) 0.0703(15) 0.0256(13) 0.0157(13) 0.0598(15) C2 0.130(2) 0.0738(16) 0.0516(13) 0.0091(12) 0.0026(12) 0.0450(15) C3 0.1154(19) 0.0852(17) 0.0570(13) 0.0187(13) 0.0036(12) 0.0520(15) C1 0.290(5) 0.087(2) 0.0508(15) 0.0071(15) 0.005(2) 0.084(3) N1 0.504(8) 0.119(3) 0.0612(16) 0.0050(16) 0.026(3) 0.149(4) N3 0.0960(12) 0.0529(10) 0.0420(9) 0.0031(7) 0.0076(8) 0.0434(9) N2 0.0907(12) 0.0553(10) 0.0471(9) 0.0056(7) 0.0076(8) 0.0422(9) O1 0.1378(14) 0.0574(9) 0.0465(8) 0.0007(7) 0.0040(8) 0.0557(9) C17 0.0520(11) 0.0665(13) 0.0503(11) 0.0012(10) 0.0036(8) 0.0254(9) C18 0.0679(12) 0.0722(13) 0.0500(11) 0.0027(10) 0.0028(9) 0.0370(11) C13 0.0734(14) 0.0879(17) 0.0495(12) -0.0048(11) -0.0034(10) 0.0467(12) C12 0.124(2) 0.110(2) 0.0519(15) -0.0084(13) -0.0008(13) 0.0775(17) C16 0.0735(14) 0.0730(15) 0.0685(14) 0.0147(12) 0.0091(10) 0.0324(12) C14 0.0888(16) 0.0824(18) 0.0748(16) -0.0113(13) 0.0034(12) 0.0448(14) C15 0.0987(18) 0.0712(16) 0.098(2) 0.0110(15) 0.0149(15) 0.0429(14) N4 0.210(3) 0.164(3) 0.0529(13) 0.0055(14) 0.0183(15) 0.125(2) C19 0.0542(11) 0.0711(14) 0.0436(10) 0.0075(10) 0.0082(9) 0.0284(10) O2 0.0697(9) 0.0767(10) 0.0527(8) 0.0030(7) 0.0230(7) 0.0254(7) C21 0.0555(11) 0.0647(12) 0.0434(10) 0.0059(9) 0.0101(8) 0.0283(10) C20 0.0627(12) 0.0727(14) 0.0464(11) 0.0105(10) 0.0211(9) 0.0253(10) C22 0.0698(13) 0.0746(14) 0.0419(10) 0.0045(10) 0.0178(9) 0.0260(11) N6 0.0597(9) 0.0688(11) 0.0480(9) 0.0034(8) 0.0186(7) 0.0201(8) N5 0.0670(10) 0.0684(11) 0.0481(9) 0.0017(8) 0.0157(7) 0.0198(9) C31 0.0738(13) 0.0821(15) 0.0496(11) 0.0018(10) 0.0058(9) 0.0413(12) C27 0.0715(13) 0.0727(14) 0.0603(12) -0.0024(10) 0.0143(10) 0.0400(11) C28 0.0797(14) 0.0689(14) 0.0744(14) 0.0039(11) 0.0227(11) 0.0382(12) C35 0.0634(13) 0.0821(15) 0.0632(13) 0.0009(11) 0.0045(10) 0.0323(12) C23 0.0865(15) 0.0883(16) 0.0616(13) 0.0156(11) 0.0216(11) 0.0564(13) C29 0.0800(16) 0.0815(17) 0.1026(19) 0.0098(14) 0.0299(13) 0.0377(13) C32 0.0829(15) 0.121(2) 0.0569(13) 0.0202(13) 0.0218(11) 0.0526(15) C33 0.0915(17) 0.115(2) 0.0646(14) 0.0016(13) 0.0162(12) 0.0521(15) C30 0.0810(17) 0.0964(19) 0.105(2) 0.0291(15) 0.0233(14) 0.0354(15) C34 0.117(2) 0.157(3) 0.0666(15) 0.0251(16) 0.0319(14) 0.084(2) C24 0.130(2) 0.114(2) 0.0696(15) 0.0235(14) 0.0241(14) 0.0763(19) C36 0.0686(14) 0.0803(16) 0.0880(16) 0.0147(13) 0.0107(12) 0.0270(12) C25 0.142(3) 0.136(3) 0.097(2) 0.0500(19) 0.0243(18) 0.074(2) C37 0.098(2) 0.085(2) 0.125(2) 0.0066(17) -0.0080(17) 0.0314(16) C26 0.235(5) 0.216(5) 0.125(3) 0.079(3) 0.004(3) 0.116(4) C38 0.105(2) 0.092(2) 0.189(4) 0.027(2) 0.016(2) 0.0268(18) N7 0.0671(10) 0.0720(11) 0.0503(9) 0.0015(8) 0.0108(7) 0.0394(9) 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' 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' F F 0.0171 0.0103 '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' 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 F1 Si1 F1 180.0 2_666 . F1 Si1 F2 92.85(10) 2_666 . F1 Si1 F2 87.15(10) . . F1 Si1 F2 87.14(10) 2_666 2_666 F1 Si1 F2 92.86(10) . 2_666 F2 Si1 F2 180.0 . 2_666 F2 Si1 F4 85.6(8) . . F2 Si1 F4 94.4(8) 2_666 . F2 Si1 F4 94.4(8) . 2_666 F2 Si1 F4 85.6(8) 2_666 2_666 F4 Si1 F4 180.0 . 2_666 F2 Si1 F6 100.9(7) . . F2 Si1 F6 79.1(7) 2_666 . F4 Si1 F6 90.9(9) . . F4 Si1 F6 89.1(9) 2_666 . F2 Si1 F6 79.1(7) . 2_666 F2 Si1 F6 100.9(7) 2_666 2_666 F4 Si1 F6 89.1(9) . 2_666 F4 Si1 F6 90.9(9) 2_666 2_666 F6 Si1 F6 180.0 . 2_666 F1 Si1 F3 90.10(7) 2_666 2_666 F1 Si1 F3 89.90(7) . 2_666 F2 Si1 F3 90.00(9) . 2_666 F2 Si1 F3 90.00(9) 2_666 2_666 F1 Si1 F3 89.90(7) 2_666 . F1 Si1 F3 90.10(7) . . F2 Si1 F3 90.00(9) . . F2 Si1 F3 90.00(9) 2_666 . F3 Si1 F3 180.0 2_666 . C11 C9 C10 118.80(17) . . C11 C9 N3 122.21(17) . . C10 C9 N3 118.88(17) . . O1 C8 N3 123.18(18) . . O1 C8 N2 123.62(17) . . N3 C8 N2 113.19(16) . . C9 C10 C11 120.36(18) . 2_676 C9 C11 C10 120.84(18) . 2_676 C7 C6 C5 118.74(18) . . C7 C6 N2 124.19(18) . . C5 C6 N2 117.05(17) . . C4 C5 C6 120.7(2) . . C6 C7 C2 119.8(2) . . C3 C4 C5 120.8(2) . . C3 C2 C7 121.0(2) . . C3 C2 C1 119.9(2) . . C7 C2 C1 119.0(2) . . C4 C3 C2 118.8(2) . . N1 C1 C2 179.6(6) . . C8 N3 C9 123.91(15) . . C8 N2 C6 126.39(16) . . C16 C17 C18 119.01(19) . . C16 C17 N5 118.79(18) . . C18 C17 N5 122.2(2) . . C13 C18 C17 119.4(2) . . C14 C13 C18 121.4(2) . . C14 C13 C12 119.9(2) . . C18 C13 C12 118.6(2) . . N4 C12 C13 179.9(5) . . C15 C16 C17 120.4(2) . . C15 C14 C13 118.4(2) . . C14 C15 C16 121.4(2) . . O2 C19 N5 123.03(18) . . O2 C19 N6 123.48(19) . . N5 C19 N6 113.48(17) . . C20 C21 C22 118.02(17) . . C20 C21 N6 117.36(17) . . C22 C21 N6 124.61(16) . . C22 C20 C21 121.85(18) 2_776 . C20 C22 C21 120.13(17) 2_776 . C19 N6 C21 126.34(16) . . C19 N5 C17 123.46(17) . . C32 C31 N7 115.18(17) . . C28 C27 N7 117.04(16) . . C27 C28 C29 111.93(17) . . C36 C35 N7 117.16(17) . . C24 C23 N7 117.16(18) . . C28 C29 C30 114.2(2) . . C33 C32 C31 111.8(2) . . C32 C33 C34 114.2(2) . . C25 C24 C23 110.1(2) . . C37 C36 C35 112.8(2) . . C26 C25 C24 113.5(3) . . C38 C37 C36 117.4(3) . . C35 N7 C23 109.38(16) . . C35 N7 C27 107.51(15) . . C23 N7 C27 111.96(16) . . C35 N7 C31 111.55(16) . . C23 N7 C31 108.25(15) . . C27 N7 C31 108.22(15) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 F1 1.6655(13) 2_666 Si1 F1 1.6655(13) . Si1 F2 1.6675(11) . Si1 F2 1.6675(11) 2_666 Si1 F4 1.6698(11) . Si1 F4 1.6698(10) 2_666 Si1 F6 1.6698(11) . Si1 F6 1.6699(10) 2_666 Si1 F3 1.6770(13) 2_666 Si1 F3 1.6771(13) . C9 C11 1.373(3) . C9 C10 1.378(3) . C9 N3 1.414(2) . C8 O1 1.214(2) . C8 N3 1.356(2) . C8 N2 1.367(2) . C10 C11 1.381(3) 2_676 C11 C10 1.381(3) 2_676 C6 C7 1.374(3) . C6 C5 1.381(3) . C6 N2 1.402(2) . C5 C4 1.375(3) . C7 C2 1.382(3) . C4 C3 1.355(3) . C2 C3 1.379(3) . C2 C1 1.425(4) . C1 N1 1.135(4) . C17 C16 1.377(3) . C17 C18 1.382(3) . C17 N5 1.404(2) . C18 C13 1.381(3) . C13 C14 1.377(3) . C13 C12 1.433(3) . C12 N4 1.146(3) . C16 C15 1.373(3) . C14 C15 1.359(3) . C19 O2 1.217(2) . C19 N5 1.361(2) . C19 N6 1.364(2) . C21 C20 1.378(2) . C21 C22 1.380(3) . C21 N6 1.409(2) . C20 C22 1.377(3) 2_776 C22 C20 1.377(3) 2_776 C31 C32 1.518(3) . C31 N7 1.519(2) . C27 C28 1.491(3) . C27 N7 1.519(2) . C28 C29 1.494(3) . C35 C36 1.508(3) . C35 N7 1.510(3) . C23 C24 1.508(3) . C23 N7 1.512(3) . C29 C30 1.497(3) . C32 C33 1.480(3) . C33 C34 1.493(3) . C24 C25 1.507(4) . C36 C37 1.475(3) . C25 C26 1.490(4) . C37 C38 1.468(4) .