#------------------------------------------------------------------------------ #$Date: 2022-08-14 01:46:42 +0300 (Sun, 14 Aug 2022) $ #$Revision: 277242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/09/7710967.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_7710967 loop_ _publ_author_name 'Radius, Udo' 'Philipp, Michael S. M.' 'Bertermann, R\"udiger' _publ_section_title ; N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Adducts of Plumbanes and Plumbylenes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D2DT02462D _journal_year 2022 _chemical_formula_moiety 'C20 H31 I2 N Pb' _chemical_formula_sum 'C20 H31 I2 N Pb' _chemical_formula_weight 746.45 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-07-28 deposited with the CCDC. 2022-08-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.0470(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.1728(2) _cell_length_b 10.33750(10) _cell_length_c 20.4224(3) _cell_measurement_reflns_used 33873 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.8100 _cell_measurement_theta_min 2.0120 _cell_volume 2315.06(6) _computing_cell_refinement 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_unetI/netI 0.0113 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 46993 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.032 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 9.957 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_correction_T_min 0.423 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.142 _exptl_crystal_description block _exptl_crystal_F_000 1384 _exptl_crystal_size_max 0.143 _exptl_crystal_size_mid 0.102 _exptl_crystal_size_min 0.078 _refine_diff_density_max 0.767 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 225 _refine_ls_number_reflns 4725 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0148 _refine_ls_R_factor_gt 0.0138 _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^)+(0.0190P)^2^+1.7778P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0342 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4578 _reflns_number_total 4725 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt02462d2.cif _cod_data_source_block compound_4 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7710967 _shelx_shelxl_version_number 2018/3 _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_min 0.336 _shelx_estimated_absorpt_t_max 0.503 _shelx_res_file ; TITL MiPh031_test2_a.res in P2(1)/c MiPh031_test2_a.res created by SHELXL-2018/3 at 14:38:15 on 29-Jun-2021 REM Old TITL MiPh031_test2 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.054, Rweak 0.004, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C20 N I2 Pb CELL 0.71073 11.1728 10.3375 20.4224 90.000 101.047 90.000 ZERR 4.000 0.0002 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N I PB UNIT 80 124 4 8 4 TEMP -173 SIZE 0.08 0.10 0.14 L.S. 10 BOND $H LIST 4 Acta 52 FMAP 2 PLAN 20 WGHT 0.019000 1.777800 FVAR 0.19161 PB01 5 0.313838 0.537281 0.424389 11.00000 0.01511 0.00966 = 0.01624 -0.00016 0.00238 0.00035 I002 4 0.275545 0.676944 0.297753 11.00000 0.01967 0.01625 = 0.01782 0.00279 0.00388 -0.00072 I003 4 0.120857 0.667937 0.477872 11.00000 0.02229 0.01690 = 0.02551 -0.00334 0.01101 0.00018 N004 3 0.216815 0.242087 0.408665 11.00000 0.01208 0.01092 = 0.01079 0.00030 0.00200 -0.00036 C005 1 0.062776 0.338717 0.333478 11.00000 0.01514 0.01418 = 0.01328 0.00182 0.00045 0.00096 C006 1 0.337626 0.218344 0.449853 11.00000 0.01324 0.00691 = 0.01522 -0.00008 0.00030 -0.00024 C007 1 0.352672 0.218416 0.519679 11.00000 0.01572 0.00877 = 0.01525 0.00008 0.00175 -0.00061 C008 1 0.435286 0.196396 0.416560 11.00000 0.01712 0.00722 = 0.01698 0.00035 0.00391 -0.00109 C009 1 0.127230 0.129873 0.387710 11.00000 0.01486 0.01100 = 0.01684 -0.00120 0.00121 -0.00273 C00A 1 0.468141 0.186979 0.555763 11.00000 0.01992 0.01165 = 0.01346 0.00162 -0.00078 0.00026 AFIX 43 H00A 2 0.480812 0.184061 0.603085 11.00000 -1.20000 AFIX 0 C00B 1 0.564360 0.160031 0.524493 11.00000 0.01340 0.01251 = 0.02496 0.00144 -0.00287 0.00048 AFIX 43 H00B 2 0.641402 0.136520 0.550204 11.00000 -1.20000 AFIX 0 C00C 1 0.255801 0.259935 0.558612 11.00000 0.01900 0.02214 = 0.01302 -0.00124 0.00273 0.00507 AFIX 13 H00C 2 0.178850 0.278942 0.526094 11.00000 -1.20000 AFIX 0 C00D 1 0.093195 0.338667 0.262661 11.00000 0.02089 0.01877 = 0.01357 0.00186 0.00068 0.00133 AFIX 137 H00D 2 0.018544 0.323403 0.229611 11.00000 -1.50000 H00E 2 0.152307 0.270014 0.259494 11.00000 -1.50000 H00F 2 0.127996 0.422552 0.254038 11.00000 -1.50000 AFIX 0 C00E 1 0.101479 0.057565 0.448376 11.00000 0.01854 0.01534 = 0.02198 0.00400 0.00199 -0.00373 AFIX 137 H00G 2 0.041607 -0.010910 0.433863 11.00000 -1.50000 H00H 2 0.069023 0.117921 0.477617 11.00000 -1.50000 H00I 2 0.177214 0.019090 0.472739 11.00000 -1.50000 AFIX 0 C00F 1 -0.028556 0.445967 0.337934 11.00000 0.01822 0.01938 = 0.01922 0.00201 0.00095 0.00495 AFIX 137 H00J 2 0.004718 0.528845 0.326470 11.00000 -1.50000 H00K 2 -0.044291 0.450156 0.383474 11.00000 -1.50000 H00L 2 -0.104929 0.427988 0.306729 11.00000 -1.50000 AFIX 0 C00G 1 0.427663 0.208358 0.341504 11.00000 0.01689 0.01646 = 0.01685 0.00055 0.00533 0.00299 AFIX 13 H00M 2 0.340376 0.223037 0.320279 11.00000 -1.20000 AFIX 0 C00H 1 0.548785 0.167194 0.456009 11.00000 0.01368 0.01257 = 0.02408 -0.00107 0.00572 0.00160 AFIX 43 H00N 2 0.616526 0.151987 0.435153 11.00000 -1.20000 AFIX 0 C00I 1 0.182472 0.353721 0.382784 11.00000 0.01414 0.01318 = 0.01117 -0.00030 0.00443 0.00125 C00J 1 0.228671 0.154813 0.606993 11.00000 0.02546 0.03770 = 0.01664 0.00405 0.00533 0.00222 AFIX 137 H00O 2 0.209845 0.073238 0.582760 11.00000 -1.50000 H00P 2 0.158748 0.181235 0.626387 11.00000 -1.50000 H00Q 2 0.300130 0.142961 0.642671 11.00000 -1.50000 AFIX 0 C00K 1 0.471762 0.085927 0.310699 11.00000 0.02798 0.01978 = 0.02114 -0.00098 0.01167 0.00252 AFIX 137 H00R 2 0.455774 0.094207 0.261997 11.00000 -1.50000 H00S 2 0.428143 0.010479 0.323321 11.00000 -1.50000 H00T 2 0.559507 0.074979 0.327125 11.00000 -1.50000 AFIX 0 C00L 1 0.016024 0.205707 0.351817 11.00000 0.01558 0.01450 = 0.01578 0.00104 0.00082 -0.00030 AFIX 23 H00U 2 -0.043923 0.216519 0.381364 11.00000 -1.20000 H00V 2 -0.023915 0.159238 0.311068 11.00000 -1.20000 AFIX 0 C00M 1 0.502258 0.325528 0.325319 11.00000 0.02970 0.01716 = 0.02890 0.00226 0.01703 0.00260 AFIX 137 H00W 2 0.496348 0.331779 0.276923 11.00000 -1.50000 H00X 2 0.587844 0.314547 0.346937 11.00000 -1.50000 H00Y 2 0.470000 0.404744 0.341809 11.00000 -1.50000 AFIX 0 C00N 1 0.296169 0.383420 0.598181 11.00000 0.03301 0.02561 = 0.01914 -0.00557 0.00149 0.00952 AFIX 137 H00Z 2 0.311383 0.451753 0.567534 11.00000 -1.50000 H010 2 0.371096 0.366229 0.630701 11.00000 -1.50000 H011 2 0.231853 0.411283 0.621625 11.00000 -1.50000 AFIX 0 C00O 1 0.179738 0.034818 0.343464 11.00000 0.02082 0.01328 = 0.02242 -0.00404 0.00258 -0.00100 AFIX 137 H012 2 0.124073 -0.038692 0.332649 11.00000 -1.50000 H013 2 0.259209 0.003799 0.367135 11.00000 -1.50000 H014 2 0.189648 0.078311 0.302198 11.00000 -1.50000 AFIX 0 HKLF 4 REM MiPh031_test2_a.res in P2(1)/c REM wR2 = 0.034207, GooF = S = 1.08710, Restrained GooF = 1.08710 for all data REM R1 = 0.013840 for 4578 Fo > 4sig(Fo) and 0.014826 for all 4725 data REM 225 parameters refined using 0 restraints END WGHT 0.0190 1.7778 REM Highest difference peak 0.767, deepest hole -0.507, 1-sigma level 0.086 Q1 1 0.3314 0.5358 0.3864 11.00000 0.05 0.77 Q2 1 0.3677 0.5287 0.3936 11.00000 0.05 0.75 Q3 1 0.3062 0.5393 0.4667 11.00000 0.05 0.74 Q4 1 0.2663 0.5406 0.4528 11.00000 0.05 0.71 Q5 1 0.3936 0.5441 0.4489 11.00000 0.05 0.70 Q6 1 0.1092 0.6795 0.4340 11.00000 0.05 0.66 Q7 1 0.3619 0.5965 0.4475 11.00000 0.05 0.63 Q8 1 0.3021 0.6738 0.2578 11.00000 0.05 0.57 Q9 1 0.2331 0.6804 0.3320 11.00000 0.05 0.53 Q10 1 0.2675 0.6772 0.2544 11.00000 0.05 0.53 Q11 1 0.0823 0.6716 0.5102 11.00000 0.05 0.48 Q12 1 0.1190 0.3620 0.3570 11.00000 0.05 0.45 Q13 1 0.2230 0.5470 0.4122 11.00000 0.05 0.42 Q14 1 0.3371 0.7147 0.3199 11.00000 0.05 0.42 Q15 1 0.2805 0.2329 0.4306 11.00000 0.05 0.41 Q16 1 0.2018 0.6809 0.5011 11.00000 0.05 0.41 Q17 1 0.3422 0.2323 0.4857 11.00000 0.05 0.41 Q18 1 0.1836 0.6787 0.2735 11.00000 0.05 0.41 Q19 1 0.1795 0.6966 0.5060 11.00000 0.05 0.38 Q20 1 0.0714 0.1729 0.3683 11.00000 0.05 0.37 ; _shelx_res_checksum 79146 loop_ _space_group_symop_operation_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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb01 Pb 0.31384(2) 0.53728(2) 0.42439(2) 0.01375(3) Uani 1 1 d . . . . . I002 I 0.27554(2) 0.67694(2) 0.29775(2) 0.01788(4) Uani 1 1 d . . . . . I003 I 0.12086(2) 0.66794(2) 0.47787(2) 0.02072(4) Uani 1 1 d . . . . . N004 N 0.21682(17) 0.24209(17) 0.40867(9) 0.0113(4) Uani 1 1 d . . . . . C005 C 0.0628(2) 0.3387(2) 0.33348(11) 0.0145(5) Uani 1 1 d . . . . . C006 C 0.3376(2) 0.2183(2) 0.44985(11) 0.0121(4) Uani 1 1 d . . . . . C007 C 0.3527(2) 0.2184(2) 0.51968(11) 0.0134(4) Uani 1 1 d . . . . . C008 C 0.4353(2) 0.1964(2) 0.41656(11) 0.0137(4) Uani 1 1 d . . . . . C009 C 0.1272(2) 0.1299(2) 0.38771(11) 0.0145(5) Uani 1 1 d . . . . . C00A C 0.4681(2) 0.1870(2) 0.55576(11) 0.0155(5) Uani 1 1 d . . . . . H00A H 0.480812 0.184061 0.603085 0.019 Uiso 1 1 calc R U . . . C00B C 0.5644(2) 0.1600(2) 0.52449(12) 0.0178(5) Uani 1 1 d . . . . . H00B H 0.641402 0.136520 0.550204 0.021 Uiso 1 1 calc R U . . . C00C C 0.2558(2) 0.2599(2) 0.55861(11) 0.0181(5) Uani 1 1 d . . . . . H00C H 0.178850 0.278942 0.526094 0.022 Uiso 1 1 calc R U . . . C00D C 0.0932(2) 0.3387(2) 0.26266(11) 0.0181(5) Uani 1 1 d . . . . . H00D H 0.018544 0.323403 0.229611 0.027 Uiso 1 1 calc R U . . . H00E H 0.152307 0.270014 0.259494 0.027 Uiso 1 1 calc R U . . . H00F H 0.127996 0.422552 0.254038 0.027 Uiso 1 1 calc R U . . . C00E C 0.1015(2) 0.0576(2) 0.44838(12) 0.0189(5) Uani 1 1 d . . . . . H00G H 0.041607 -0.010910 0.433863 0.028 Uiso 1 1 calc R U . . . H00H H 0.069023 0.117921 0.477617 0.028 Uiso 1 1 calc R U . . . H00I H 0.177214 0.019090 0.472739 0.028 Uiso 1 1 calc R U . . . C00F C -0.0286(2) 0.4460(2) 0.33793(12) 0.0193(5) Uani 1 1 d . . . . . H00J H 0.004718 0.528845 0.326470 0.029 Uiso 1 1 calc R U . . . H00K H -0.044291 0.450156 0.383474 0.029 Uiso 1 1 calc R U . . . H00L H -0.104929 0.427988 0.306729 0.029 Uiso 1 1 calc R U . . . C00G C 0.4277(2) 0.2084(2) 0.34150(11) 0.0165(5) Uani 1 1 d . . . . . H00M H 0.340376 0.223037 0.320279 0.020 Uiso 1 1 calc R U . . . C00H C 0.5488(2) 0.1672(2) 0.45601(12) 0.0165(5) Uani 1 1 d . . . . . H00N H 0.616526 0.151987 0.435153 0.020 Uiso 1 1 calc R U . . . C00I C 0.1825(2) 0.3537(2) 0.38278(10) 0.0126(4) Uani 1 1 d . . . . . C00J C 0.2287(3) 0.1548(3) 0.60699(12) 0.0264(6) Uani 1 1 d . . . . . H00O H 0.209845 0.073238 0.582760 0.040 Uiso 1 1 calc R U . . . H00P H 0.158748 0.181235 0.626387 0.040 Uiso 1 1 calc R U . . . H00Q H 0.300130 0.142961 0.642671 0.040 Uiso 1 1 calc R U . . . C00K C 0.4718(2) 0.0859(2) 0.31070(12) 0.0220(5) Uani 1 1 d . . . . . H00R H 0.455774 0.094207 0.261997 0.033 Uiso 1 1 calc R U . . . H00S H 0.428143 0.010479 0.323321 0.033 Uiso 1 1 calc R U . . . H00T H 0.559507 0.074979 0.327125 0.033 Uiso 1 1 calc R U . . . C00L C 0.0160(2) 0.2057(2) 0.35182(11) 0.0156(5) Uani 1 1 d . . . . . H00U H -0.043923 0.216519 0.381364 0.019 Uiso 1 1 calc R U . . . H00V H -0.023915 0.159238 0.311068 0.019 Uiso 1 1 calc R U . . . C00M C 0.5023(3) 0.3255(2) 0.32532(13) 0.0237(5) Uani 1 1 d . . . . . H00W H 0.496348 0.331779 0.276923 0.036 Uiso 1 1 calc R U . . . H00X H 0.587844 0.314547 0.346937 0.036 Uiso 1 1 calc R U . . . H00Y H 0.470000 0.404744 0.341809 0.036 Uiso 1 1 calc R U . . . C00N C 0.2962(3) 0.3834(3) 0.59818(13) 0.0264(6) Uani 1 1 d . . . . . H00Z H 0.311383 0.451753 0.567534 0.040 Uiso 1 1 calc R U . . . H010 H 0.371096 0.366229 0.630701 0.040 Uiso 1 1 calc R U . . . H011 H 0.231853 0.411283 0.621625 0.040 Uiso 1 1 calc R U . . . C00O C 0.1797(2) 0.0348(2) 0.34346(12) 0.0190(5) Uani 1 1 d . . . . . H012 H 0.124073 -0.038692 0.332649 0.029 Uiso 1 1 calc R U . . . H013 H 0.259209 0.003799 0.367135 0.029 Uiso 1 1 calc R U . . . H014 H 0.189648 0.078311 0.302198 0.029 Uiso 1 1 calc R U . . . 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 Pb01 0.01511(5) 0.00966(5) 0.01624(5) -0.00016(3) 0.00238(3) 0.00035(3) I002 0.01967(8) 0.01625(8) 0.01782(8) 0.00279(6) 0.00388(6) -0.00072(6) I003 0.02229(9) 0.01690(8) 0.02551(9) -0.00334(6) 0.01101(7) 0.00018(6) N004 0.0121(9) 0.0109(9) 0.0108(8) 0.0003(7) 0.0020(7) -0.0004(7) C005 0.0151(11) 0.0142(11) 0.0133(11) 0.0018(8) 0.0005(9) 0.0010(9) C006 0.0132(11) 0.0069(10) 0.0152(11) -0.0001(8) 0.0003(8) -0.0002(8) C007 0.0157(11) 0.0088(10) 0.0153(11) 0.0001(8) 0.0018(9) -0.0006(9) C008 0.0171(11) 0.0072(10) 0.0170(11) 0.0003(8) 0.0039(9) -0.0011(8) C009 0.0149(11) 0.0110(10) 0.0168(11) -0.0012(9) 0.0012(9) -0.0027(9) C00A 0.0199(12) 0.0116(11) 0.0135(11) 0.0016(8) -0.0008(9) 0.0003(9) C00B 0.0134(12) 0.0125(11) 0.0250(12) 0.0014(9) -0.0029(9) 0.0005(9) C00C 0.0190(12) 0.0221(12) 0.0130(11) -0.0012(9) 0.0027(9) 0.0051(10) C00D 0.0209(13) 0.0188(12) 0.0136(11) 0.0019(9) 0.0007(9) 0.0013(10) C00E 0.0185(12) 0.0153(11) 0.0220(12) 0.0040(9) 0.0020(10) -0.0037(9) C00F 0.0182(12) 0.0194(12) 0.0192(12) 0.0020(9) 0.0010(10) 0.0050(10) C00G 0.0169(12) 0.0165(11) 0.0169(11) 0.0006(9) 0.0053(9) 0.0030(9) C00H 0.0137(11) 0.0126(11) 0.0241(12) -0.0011(9) 0.0057(9) 0.0016(9) C00I 0.0141(11) 0.0132(11) 0.0112(10) -0.0003(8) 0.0044(9) 0.0012(8) C00J 0.0255(14) 0.0377(15) 0.0166(12) 0.0041(11) 0.0053(10) 0.0022(12) C00K 0.0280(14) 0.0198(12) 0.0211(12) -0.0010(10) 0.0117(10) 0.0025(11) C00L 0.0156(12) 0.0145(11) 0.0158(11) 0.0010(9) 0.0008(9) -0.0003(9) C00M 0.0297(14) 0.0172(12) 0.0289(14) 0.0023(10) 0.0170(11) 0.0026(10) C00N 0.0330(15) 0.0256(14) 0.0191(12) -0.0056(10) 0.0015(11) 0.0095(11) C00O 0.0208(13) 0.0133(11) 0.0224(12) -0.0040(9) 0.0026(10) -0.0010(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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 C00I Pb01 I002 95.71(5) . . ? C00I Pb01 I003 92.96(5) . . ? I002 Pb01 I003 96.253(5) . . ? C00I N004 C006 123.39(18) . . ? C00I N004 C009 115.59(18) . . ? C006 N004 C009 120.74(17) . . ? C00I C005 C00F 113.65(19) . . ? C00I C005 C00L 103.06(17) . . ? C00F C005 C00L 111.9(2) . . ? C00I C005 C00D 107.23(19) . . ? C00F C005 C00D 109.03(18) . . ? C00L C005 C00D 111.83(19) . . ? C007 C006 C008 122.5(2) . . ? C007 C006 N004 120.0(2) . . ? C008 C006 N004 117.52(19) . . ? C00A C007 C006 117.1(2) . . ? C00A C007 C00C 117.9(2) . . ? C006 C007 C00C 124.9(2) . . ? C00H C008 C006 117.2(2) . . ? C00H C008 C00G 117.8(2) . . ? C006 C008 C00G 124.9(2) . . ? C00E C009 C00O 108.67(19) . . ? C00E C009 C00L 112.2(2) . . ? C00O C009 C00L 114.50(19) . . ? C00E C009 N004 111.01(18) . . ? C00O C009 N004 110.29(18) . . ? C00L C009 N004 99.91(17) . . ? C00B C00A C007 121.7(2) . . ? C00B C00A H00A 119.1 . . ? C007 C00A H00A 119.1 . . ? C00H C00B C00A 120.1(2) . . ? C00H C00B H00B 120.0 . . ? C00A C00B H00B 120.0 . . ? C007 C00C C00N 110.1(2) . . ? C007 C00C C00J 112.6(2) . . ? C00N C00C C00J 108.9(2) . . ? C007 C00C H00C 108.4 . . ? C00N C00C H00C 108.4 . . ? C00J C00C H00C 108.4 . . ? C005 C00D H00D 109.5 . . ? C005 C00D H00E 109.5 . . ? H00D C00D H00E 109.5 . . ? C005 C00D H00F 109.5 . . ? H00D C00D H00F 109.5 . . ? H00E C00D H00F 109.5 . . ? C009 C00E H00G 109.5 . . ? C009 C00E H00H 109.5 . . ? H00G C00E H00H 109.5 . . ? C009 C00E H00I 109.5 . . ? H00G C00E H00I 109.5 . . ? H00H C00E H00I 109.5 . . ? C005 C00F H00J 109.5 . . ? C005 C00F H00K 109.5 . . ? H00J C00F H00K 109.5 . . ? C005 C00F H00L 109.5 . . ? H00J C00F H00L 109.5 . . ? H00K C00F H00L 109.5 . . ? C008 C00G C00K 112.62(19) . . ? C008 C00G C00M 110.56(19) . . ? C00K C00G C00M 109.3(2) . . ? C008 C00G H00M 108.1 . . ? C00K C00G H00M 108.1 . . ? C00M C00G H00M 108.1 . . ? C00B C00H C008 121.4(2) . . ? C00B C00H H00N 119.3 . . ? C008 C00H H00N 119.3 . . ? N004 C00I C005 109.47(19) . . ? N004 C00I Pb01 115.93(15) . . ? C005 C00I Pb01 134.55(15) . . ? C00C C00J H00O 109.5 . . ? C00C C00J H00P 109.5 . . ? H00O C00J H00P 109.5 . . ? C00C C00J H00Q 109.5 . . ? H00O C00J H00Q 109.5 . . ? H00P C00J H00Q 109.5 . . ? C00G C00K H00R 109.5 . . ? C00G C00K H00S 109.5 . . ? H00R C00K H00S 109.5 . . ? C00G C00K H00T 109.5 . . ? H00R C00K H00T 109.5 . . ? H00S C00K H00T 109.5 . . ? C009 C00L C005 106.92(18) . . ? C009 C00L H00U 110.3 . . ? C005 C00L H00U 110.3 . . ? C009 C00L H00V 110.3 . . ? C005 C00L H00V 110.3 . . ? H00U C00L H00V 108.6 . . ? C00G C00M H00W 109.5 . . ? C00G C00M H00X 109.5 . . ? H00W C00M H00X 109.5 . . ? C00G C00M H00Y 109.5 . . ? H00W C00M H00Y 109.5 . . ? H00X C00M H00Y 109.5 . . ? C00C C00N H00Z 109.5 . . ? C00C C00N H010 109.5 . . ? H00Z C00N H010 109.5 . . ? C00C C00N H011 109.5 . . ? H00Z C00N H011 109.5 . . ? H010 C00N H011 109.5 . . ? C009 C00O H012 109.5 . . ? C009 C00O H013 109.5 . . ? H012 C00O H013 109.5 . . ? C009 C00O H014 109.5 . . ? H012 C00O H014 109.5 . . ? H013 C00O H014 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb01 C00I 2.449(2) . ? Pb01 I002 2.92095(17) . ? Pb01 I003 2.92723(18) . ? N004 C00I 1.296(3) . ? N004 C006 1.468(3) . ? N004 C009 1.538(3) . ? C005 C00I 1.520(3) . ? C005 C00F 1.521(3) . ? C005 C00L 1.542(3) . ? C005 C00D 1.548(3) . ? C006 C007 1.404(3) . ? C006 C008 1.410(3) . ? C007 C00A 1.396(3) . ? C007 C00C 1.522(3) . ? C008 C00H 1.399(3) . ? C008 C00G 1.524(3) . ? C009 C00E 1.521(3) . ? C009 C00O 1.526(3) . ? C009 C00L 1.532(3) . ? C00A C00B 1.380(3) . ? C00A H00A 0.9500 . ? C00B C00H 1.378(3) . ? C00B H00B 0.9500 . ? C00C C00N 1.532(3) . ? C00C C00J 1.537(3) . ? C00C H00C 1.0000 . ? C00D H00D 0.9800 . ? C00D H00E 0.9800 . ? C00D H00F 0.9800 . ? C00E H00G 0.9800 . ? C00E H00H 0.9800 . ? C00E H00I 0.9800 . ? C00F H00J 0.9800 . ? C00F H00K 0.9800 . ? C00F H00L 0.9800 . ? C00G C00K 1.536(3) . ? C00G C00M 1.542(3) . ? C00G H00M 1.0000 . ? C00H H00N 0.9500 . ? C00J H00O 0.9800 . ? C00J H00P 0.9800 . ? C00J H00Q 0.9800 . ? C00K H00R 0.9800 . ? C00K H00S 0.9800 . ? C00K H00T 0.9800 . ? C00L H00U 0.9900 . ? C00L H00V 0.9900 . ? C00M H00W 0.9800 . ? C00M H00X 0.9800 . ? C00M H00Y 0.9800 . ? C00N H00Z 0.9800 . ? C00N H010 0.9800 . ? C00N H011 0.9800 . ? C00O H012 0.9800 . ? C00O H013 0.9800 . ? C00O H014 0.9800 . ?