#------------------------------------------------------------------------------ #$Date: 2020-05-16 04:59:56 +0300 (Sat, 16 May 2020) $ #$Revision: 252072 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240538.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_7240538 loop_ _publ_author_name 'Hodorowicz, Maciej' 'Szklarzewicz, Janusz' 'Jurowska, Anna' _publ_section_title ; The versatility of lithium cation coordination modes in salts with [W(CN)6(bpy)]2- anion ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00468E _journal_year 2020 _chemical_formula_sum 'C16 H8 Cl Li3 N8 O2 W' _chemical_formula_weight 584.42 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2019-04-05 deposited with the CCDC. 2020-04-30 downloaded from the CCDC. ; _cell_angle_alpha 94.505(2) _cell_angle_beta 95.182(2) _cell_angle_gamma 95.941(2) _cell_formula_units_Z 2 _cell_length_a 9.2897(2) _cell_length_b 9.4735(2) _cell_length_c 13.3937(3) _cell_measurement_reflns_used 22288 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 27.5990 _cell_measurement_theta_min 3.3070 _cell_volume 1163.00(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 130.10(14) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3756 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 51463 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.706 _diffrn_reflns_theta_min 3.066 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 5.107 _exptl_absorpt_correction_T_max 0.07245 _exptl_absorpt_correction_T_min 0.04730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.669 _exptl_crystal_description prism _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.707 _refine_diff_density_min -2.080 _refine_diff_density_rms 0.174 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 5760 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.117 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0356 _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^)+(0.0488P)^2^+3.8817P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.0929 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5087 _reflns_number_total 5760 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00468e1.cif _cod_data_source_block shelx _cod_database_code 7240538 _shelx_shelxl_version_number 2017/1 _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 0.428 _shelx_estimated_absorpt_t_max 0.629 _exptl_absorpt_special_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL SIR92 run in space group P -1 shelx.res created by SHELXL-2017/1 at 15:00:51 on 17-May-2018 CELL 0.71073 9.2897 9.4735 13.3937 94.505 95.182 95.941 ZERR 2.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N W LI O CL UNIT 32 16 16 2 6 4 2 MERG 2 OMIT 1 -2 1 OMIT 0 2 1 OMIT -1 3 0 OMIT 1 0 2 OMIT -2 2 2 OMIT -2 0 2 OMIT 0 0 3 OMIT -1 1 1 OMIT 1 1 0 OMIT -1 1 0 OMIT 0 -2 1 OMIT -1 -1 1 EQIV $6 -x, -y+1, -z+1 HTAB C5 CL1_$6 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 9 SIZE 0.2 0.15 0.1 TEMP -143.15 WGHT 0.048800 3.881700 FVAR 14.93741 0.20857 W1 4 0.127902 0.297587 0.260185 11.00000 0.02072 0.02210 = 0.01950 0.00342 0.00178 0.00571 N1 3 0.221216 0.447494 0.391452 11.00000 0.04203 0.02529 = 0.03472 -0.00285 -0.01277 0.01569 N16 3 0.036492 -0.041344 0.183695 11.00000 0.05976 0.02862 = 0.02734 0.00631 -0.00521 -0.00659 N17 3 0.076483 0.617090 0.190379 11.00000 0.04860 0.03018 = 0.03737 0.00356 0.00005 0.01196 N12 3 0.013610 0.233623 0.391385 11.00000 0.03229 0.04252 = 0.02352 0.01030 0.00889 0.02055 C18 1 -0.099088 0.306336 0.216548 11.00000 0.02526 0.04761 = 0.03583 0.02050 0.00895 0.01304 C4 1 0.345158 0.610704 0.565498 11.00000 0.10618 0.05260 = 0.07339 -0.03797 -0.06302 0.04814 AFIX 43 H4 2 0.388707 0.666093 0.624805 11.00000 -1.20000 AFIX 0 N13 3 0.363765 0.117233 0.383369 11.00000 0.03121 0.03371 = 0.04996 0.01392 -0.00620 0.00554 C11 1 -0.097170 0.128378 0.386594 11.00000 0.03356 0.05360 = 0.04535 0.02875 0.01584 0.01822 AFIX 43 H11 2 -0.133130 0.081510 0.322537 11.00000 -1.20000 AFIX 0 N18 3 -0.219861 0.312109 0.193417 11.00000 0.02550 0.08761 = 0.05938 0.04162 0.00616 0.01314 C2 1 0.322678 0.557184 0.386869 11.00000 0.05528 0.02521 = 0.05879 -0.00410 -0.02085 0.01273 AFIX 43 H2 2 0.352663 0.578695 0.323295 11.00000 -1.20000 AFIX 0 C16 1 0.067554 0.077667 0.209504 11.00000 0.03019 0.02996 = 0.02050 0.00619 0.00024 0.00147 N14 3 0.447119 0.386086 0.182855 11.00000 0.02389 0.06297 = 0.04835 0.02501 0.00432 0.00329 C5 1 0.240778 0.499275 0.570978 11.00000 0.10001 0.06835 = 0.03698 -0.02143 -0.02720 0.06216 AFIX 43 H5 2 0.211070 0.477202 0.634514 11.00000 -1.20000 AFIX 0 C10 1 -0.160458 0.085666 0.469529 11.00000 0.04383 0.09211 = 0.06668 0.05553 0.03038 0.03659 AFIX 43 H10 2 -0.238854 0.011623 0.462077 11.00000 -1.20000 AFIX 0 C3 1 0.385539 0.640827 0.473507 11.00000 0.07342 0.03527 = 0.08430 -0.01900 -0.04962 0.02261 AFIX 43 H3 2 0.456581 0.718859 0.468261 11.00000 -1.20000 AFIX 0 C17 1 0.095390 0.507939 0.215641 11.00000 0.03243 0.02779 = 0.02814 0.00421 -0.00121 0.01167 C6 1 0.177849 0.417990 0.483591 11.00000 0.06257 0.04261 = 0.02627 -0.00640 -0.00908 0.03749 C13 1 0.282295 0.178610 0.339853 11.00000 0.02629 0.02538 = 0.02536 0.00127 0.00359 0.00201 C7 1 0.062169 0.300141 0.483210 11.00000 0.04832 0.06268 = 0.02211 0.00969 0.00822 0.03737 N15 3 0.100785 0.262737 0.011550 11.00000 0.04207 0.03619 = 0.02514 0.00696 0.00425 0.01017 C15 1 0.109662 0.273263 0.097670 11.00000 0.02578 0.02615 = 0.02638 0.00545 0.00123 0.00624 C14 1 0.335792 0.355590 0.210044 11.00000 0.02317 0.03322 = 0.03180 0.00862 -0.00074 0.00557 C8 1 0.002235 0.259699 0.570206 11.00000 0.07504 0.10885 = 0.02643 0.02091 0.01499 0.07207 AFIX 43 H8 2 0.038039 0.306759 0.634233 11.00000 -1.20000 AFIX 0 C9 1 -0.111168 0.148944 0.561402 11.00000 0.05914 0.13364 = 0.05538 0.06338 0.03714 0.05984 AFIX 43 H9 2 -0.152816 0.118809 0.619472 11.00000 -1.20000 AFIX 0 LI1 5 -0.058980 0.760383 0.140443 11.00000 0.03835 0.03074 = 0.02525 0.00818 -0.00292 0.00462 CL1 7 -0.284901 0.708463 0.209085 11.00000 0.04070 0.08287 = 0.04951 0.02897 0.00792 0.01637 O1 6 -0.350637 0.461360 0.007425 11.00000 0.06945 0.12733 = 0.07611 0.06593 -0.00226 -0.00534 O2 6 -0.419653 0.069413 0.206528 11.00000 0.08396 0.12436 = 0.23906 0.01523 0.01604 0.07093 LI3 5 -0.346736 0.194937 -0.114222 11.00000 0.01468 0.06622 = 0.07045 -0.01520 0.00011 0.01298 LI2 5 -0.355358 0.461325 0.148512 11.00000 0.03056 0.08088 = 0.07650 0.03606 0.00750 0.01043 HKLF 4 REM SIR92 run in space group P -1 REM R1 = 0.0356 for 5087 Fo > 4sig(Fo) and 0.0428 for all 5760 data REM 281 parameters refined using 0 restraints END WGHT 0.0488 3.8861 REM Highest difference peak 2.707, deepest hole -2.080, 1-sigma level 0.174 Q1 1 -0.3810 0.1105 0.2198 11.00000 0.05 2.71 Q2 1 -0.2791 0.7886 0.2402 11.00000 0.05 2.30 Q3 1 -0.3349 0.1581 -0.1970 11.00000 0.05 1.72 Q4 1 -0.3603 0.5471 0.0573 11.00000 0.05 1.60 Q5 1 -0.4751 0.2318 -0.0390 11.00000 0.05 1.48 Q6 1 -0.4377 -0.1148 0.1435 11.00000 0.05 1.34 Q7 1 -0.2893 0.1797 -0.0966 11.00000 0.05 1.27 Q8 1 -0.3616 0.1462 -0.1018 11.00000 0.05 1.26 Q9 1 -0.4222 0.0420 0.1420 11.00000 0.05 1.21 Q10 1 -0.3853 0.3447 0.0842 11.00000 0.05 1.20 Q11 1 -0.4275 0.0189 0.2408 11.00000 0.05 1.19 Q12 1 -0.3381 0.2390 -0.0985 11.00000 0.05 1.07 Q13 1 0.0824 0.2416 0.2222 11.00000 0.05 0.91 Q14 1 0.0730 0.2853 0.3049 11.00000 0.05 0.90 Q15 1 0.1738 0.2800 0.1942 11.00000 0.05 0.88 Q16 1 -0.0761 0.2313 0.5772 11.00000 0.05 0.72 Q17 1 -0.4578 -0.1324 0.2163 11.00000 0.05 0.70 Q18 1 0.1981 0.2539 0.2328 11.00000 0.05 0.69 Q19 1 0.0176 0.2296 0.5729 11.00000 0.05 0.68 Q20 1 0.0263 0.3348 0.5819 11.00000 0.05 0.65 ; _shelx_res_checksum 90556 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 W1 W 0.12790(2) 0.29759(2) 0.26018(2) 0.02047(7) Uani 1 1 d . . . . . N1 N 0.2212(5) 0.4475(5) 0.3915(4) 0.0345(11) Uani 1 1 d . . . . . N16 N 0.0365(6) -0.0413(5) 0.1837(4) 0.0398(12) Uani 1 1 d . . . . . N17 N 0.0765(6) 0.6171(5) 0.1904(4) 0.0384(11) Uani 1 1 d . . . . . N12 N 0.0136(5) 0.2336(5) 0.3914(3) 0.0309(10) Uani 1 1 d . . . . . C18 C -0.0991(6) 0.3063(7) 0.2165(4) 0.0343(12) Uani 1 1 d . . . . . C4 C 0.3452(11) 0.6107(9) 0.5655(7) 0.081(4) Uani 1 1 d . . . . . H4 H 0.388707 0.666093 0.624805 0.098 Uiso 1 1 calc R U . . . N13 N 0.3638(5) 0.1172(5) 0.3834(4) 0.0382(11) Uani 1 1 d . . . . . C11 C -0.0972(6) 0.1284(7) 0.3866(5) 0.0412(14) Uani 1 1 d . . . . . H11 H -0.133130 0.081510 0.322537 0.049 Uiso 1 1 calc R U . . . N18 N -0.2199(6) 0.3121(8) 0.1934(5) 0.0550(17) Uani 1 1 d . . . . . C2 C 0.3227(8) 0.5572(6) 0.3869(6) 0.0479(17) Uani 1 1 d . . . . . H2 H 0.352663 0.578695 0.323295 0.057 Uiso 1 1 calc R U . . . C16 C 0.0676(6) 0.0777(6) 0.2095(4) 0.0269(10) Uani 1 1 d . . . . . N14 N 0.4471(5) 0.3861(7) 0.1829(4) 0.0441(13) Uani 1 1 d . . . . . C5 C 0.2408(11) 0.4993(9) 0.5710(6) 0.068(3) Uani 1 1 d . . . . . H5 H 0.211070 0.477202 0.634514 0.082 Uiso 1 1 calc R U . . . C10 C -0.1605(8) 0.0857(10) 0.4695(6) 0.061(2) Uani 1 1 d . . . . . H10 H -0.238854 0.011623 0.462077 0.074 Uiso 1 1 calc R U . . . C3 C 0.3855(10) 0.6408(8) 0.4735(7) 0.068(3) Uani 1 1 d . . . . . H3 H 0.456581 0.718859 0.468261 0.082 Uiso 1 1 calc R U . . . C17 C 0.0954(6) 0.5079(6) 0.2156(4) 0.0290(11) Uani 1 1 d . . . . . C6 C 0.1778(8) 0.4180(7) 0.4836(4) 0.0429(16) Uani 1 1 d . . . . . C13 C 0.2823(5) 0.1786(5) 0.3399(4) 0.0257(10) Uani 1 1 d . . . . . C7 C 0.0622(7) 0.3001(8) 0.4832(4) 0.0416(15) Uani 1 1 d . . . . . N15 N 0.1008(5) 0.2627(5) 0.0116(3) 0.0338(10) Uani 1 1 d . . . . . C15 C 0.1097(5) 0.2733(5) 0.0977(4) 0.0258(10) Uani 1 1 d . . . . . C14 C 0.3358(6) 0.3556(6) 0.2100(4) 0.0291(11) Uani 1 1 d . . . . . C8 C 0.0022(10) 0.2597(11) 0.5702(5) 0.064(3) Uani 1 1 d . . . . . H8 H 0.038039 0.306759 0.634233 0.077 Uiso 1 1 calc R U . . . C9 C -0.1112(9) 0.1489(12) 0.5614(6) 0.074(3) Uani 1 1 d . . . . . H9 H -0.152816 0.118809 0.619472 0.089 Uiso 1 1 calc R U . . . Li1 Li -0.0590(11) 0.7604(10) 0.1404(7) 0.0315(19) Uani 1 1 d . . . . . Cl1 Cl -0.28490(19) 0.7085(2) 0.20908(14) 0.0556(5) Uani 1 1 d . . . . . O1 O -0.3506(7) 0.4614(9) 0.0074(5) 0.090(2) Uani 1 1 d . . . . . O2 O -0.4197(10) 0.0694(11) 0.2065(10) 0.145(4) Uani 1 1 d . . . . . Li3 Li -0.3467(10) 0.1949(14) -0.1142(10) 0.051(3) Uani 1 1 d . . . . . Li2 Li -0.3554(13) 0.4613(16) 0.1485(11) 0.061(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 W1 0.02072(11) 0.02210(11) 0.01950(10) 0.00342(7) 0.00178(7) 0.00571(7) N1 0.042(3) 0.025(2) 0.035(2) -0.0029(18) -0.013(2) 0.0157(19) N16 0.060(3) 0.029(2) 0.027(2) 0.0063(19) -0.005(2) -0.007(2) N17 0.049(3) 0.030(2) 0.037(3) 0.004(2) 0.000(2) 0.012(2) N12 0.032(2) 0.043(3) 0.024(2) 0.0103(18) 0.0089(17) 0.021(2) C18 0.025(3) 0.048(3) 0.036(3) 0.021(2) 0.009(2) 0.013(2) C4 0.106(7) 0.053(5) 0.073(6) -0.038(4) -0.063(6) 0.048(5) N13 0.031(2) 0.034(2) 0.050(3) 0.014(2) -0.006(2) 0.006(2) C11 0.034(3) 0.054(4) 0.045(3) 0.029(3) 0.016(3) 0.018(3) N18 0.025(3) 0.088(5) 0.059(4) 0.042(3) 0.006(2) 0.013(3) C2 0.055(4) 0.025(3) 0.059(4) -0.004(3) -0.021(3) 0.013(3) C16 0.030(3) 0.030(3) 0.021(2) 0.0062(19) 0.0002(19) 0.001(2) N14 0.024(2) 0.063(4) 0.048(3) 0.025(3) 0.004(2) 0.003(2) C5 0.100(7) 0.068(5) 0.037(4) -0.021(3) -0.027(4) 0.062(5) C10 0.044(4) 0.092(6) 0.067(5) 0.056(5) 0.030(4) 0.037(4) C3 0.073(5) 0.035(3) 0.084(6) -0.019(4) -0.050(5) 0.023(3) C17 0.032(3) 0.028(3) 0.028(2) 0.004(2) -0.001(2) 0.012(2) C6 0.063(4) 0.043(3) 0.026(3) -0.006(2) -0.009(3) 0.037(3) C13 0.026(2) 0.025(2) 0.025(2) 0.0013(19) 0.0036(19) 0.0020(19) C7 0.048(3) 0.063(4) 0.022(2) 0.010(3) 0.008(2) 0.037(3) N15 0.042(3) 0.036(2) 0.025(2) 0.0070(19) 0.0042(19) 0.010(2) C15 0.026(2) 0.026(2) 0.026(2) 0.0055(19) 0.0012(19) 0.0062(19) C14 0.023(2) 0.033(3) 0.032(3) 0.009(2) -0.001(2) 0.006(2) C8 0.075(5) 0.109(7) 0.026(3) 0.021(4) 0.015(3) 0.072(5) C9 0.059(5) 0.134(9) 0.055(5) 0.063(5) 0.037(4) 0.060(6) Li1 0.038(5) 0.031(4) 0.025(4) 0.008(4) -0.003(4) 0.005(4) Cl1 0.0407(8) 0.0829(13) 0.0495(9) 0.0290(9) 0.0079(7) 0.0164(8) O1 0.069(4) 0.127(6) 0.076(4) 0.066(4) -0.002(3) -0.005(4) O2 0.084(6) 0.124(8) 0.239(13) 0.015(8) 0.016(7) 0.071(6) Li3 0.015(4) 0.066(7) 0.070(8) -0.015(6) 0.000(4) 0.013(4) Li2 0.031(6) 0.081(9) 0.077(9) 0.036(7) 0.008(5) 0.010(6) 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 W1 C16 106.8(2) . . ? C14 W1 C18 140.3(2) . . ? C16 W1 C18 81.2(2) . . ? C14 W1 C15 70.8(2) . . ? C16 W1 C15 70.89(19) . . ? C18 W1 C15 75.8(2) . . ? C14 W1 C17 80.7(2) . . ? C16 W1 C17 140.25(19) . . ? C18 W1 C17 70.5(2) . . ? C15 W1 C17 75.40(19) . . ? C14 W1 C13 72.76(19) . . ? C16 W1 C13 73.50(19) . . ? C18 W1 C13 144.1(2) . . ? C15 W1 C13 117.52(19) . . ? C17 W1 C13 143.05(19) . . ? C14 W1 N1 81.7(2) . . ? C16 W1 N1 144.31(18) . . ? C18 W1 N1 114.8(2) . . ? C15 W1 N1 142.03(19) . . ? C17 W1 N1 74.70(18) . . ? C13 W1 N1 76.40(17) . . ? C14 W1 N12 144.37(18) . . ? C16 W1 N12 81.80(19) . . ? C18 W1 N12 74.50(18) . . ? C15 W1 N12 142.13(19) . . ? C17 W1 N12 115.12(19) . . ? C13 W1 N12 77.06(17) . . ? N1 W1 N12 73.10(19) . . ? C2 N1 C6 118.8(6) . . ? C2 N1 W1 124.2(5) . . ? C6 N1 W1 116.8(4) . . ? C16 N16 Li1 168.4(6) . 1_545 ? C17 N17 Li1 151.3(6) . . ? C11 N12 C7 117.4(5) . . ? C11 N12 W1 124.5(4) . . ? C7 N12 W1 118.0(4) . . ? N18 C18 W1 179.5(7) . . ? C3 C4 C5 118.9(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N12 C11 C10 123.3(7) . . ? N12 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C18 N18 Li2 138.8(7) . . ? N1 C2 C3 121.5(8) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? N16 C16 W1 178.8(5) . . ? C14 N14 Li2 172.6(8) . 1_655 ? C4 C5 C6 120.2(9) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C9 C10 C11 119.8(8) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C4 C3 C2 120.1(9) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? N17 C17 W1 178.5(5) . . ? N1 C6 C5 120.5(8) . . ? N1 C6 C7 116.2(5) . . ? C5 C6 C7 123.3(7) . . ? N13 C13 W1 178.9(5) . . ? N12 C7 C8 121.5(7) . . ? N12 C7 C6 115.2(5) . . ? C8 C7 C6 123.3(7) . . ? C15 N15 Li1 173.1(6) . 2_565 ? N15 C15 W1 178.9(5) . . ? N14 C14 W1 179.7(6) . . ? C9 C8 C7 118.9(7) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 119.0(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N16 Li1 N15 109.3(5) 1_565 2_565 ? N16 Li1 N17 108.7(5) 1_565 . ? N15 Li1 N17 111.5(5) 2_565 . ? N16 Li1 Cl1 113.0(5) 1_565 . ? N15 Li1 Cl1 107.2(4) 2_565 . ? N17 Li1 Cl1 107.1(4) . . ? Li1 Cl1 Li2 102.8(4) . . ? O1 Li2 N14 111.1(7) . 1_455 ? O1 Li2 N18 105.8(8) . . ? N14 Li2 N18 104.9(6) 1_455 . ? O1 Li2 Cl1 103.3(6) . . ? N14 Li2 Cl1 113.5(7) 1_455 . ? N18 Li2 Cl1 118.0(6) . . ? 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 W1 C14 2.134(5) . ? W1 C16 2.141(5) . ? W1 C18 2.149(5) . ? W1 C15 2.160(5) . ? W1 C17 2.167(5) . ? W1 C13 2.171(5) . ? W1 N1 2.222(4) . ? W1 N12 2.226(4) . ? N1 C2 1.338(9) . ? N1 C6 1.373(8) . ? N16 C16 1.152(7) . ? N16 Li1 2.010(10) 1_545 ? N17 C17 1.139(7) . ? N17 Li1 2.054(10) . ? N12 C11 1.350(8) . ? N12 C7 1.354(8) . ? C18 N18 1.145(7) . ? C4 C3 1.363(15) . ? C4 C5 1.369(15) . ? C4 H4 0.9500 . ? N13 C13 1.147(7) . ? C11 C10 1.372(8) . ? C11 H11 0.9500 . ? N18 Li2 2.076(14) . ? C2 C3 1.397(9) . ? C2 H2 0.9500 . ? N14 C14 1.144(7) . ? N14 Li2 2.005(13) 1_655 ? C5 C6 1.395(9) . ? C5 H5 0.9500 . ? C10 C9 1.345(14) . ? C10 H10 0.9500 . ? C3 H3 0.9500 . ? C6 C7 1.467(11) . ? C7 C8 1.399(9) . ? N15 C15 1.145(7) . ? N15 Li1 2.028(10) 2_565 ? C8 C9 1.398(14) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? Li1 Cl1 2.387(10) . ? Cl1 Li2 2.420(16) . ? O1 Li2 1.894(16) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C5 H5 Cl1 0.95 2.92 3.685(9) 138.5 2_566 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N12 C11 C10 -0.7(8) . . . . ? W1 N12 C11 C10 176.2(5) . . . . ? C6 N1 C2 C3 0.5(9) . . . . ? W1 N1 C2 C3 -174.8(5) . . . . ? C3 C4 C5 C6 0.3(10) . . . . ? N12 C11 C10 C9 -0.6(10) . . . . ? C5 C4 C3 C2 -1.1(11) . . . . ? N1 C2 C3 C4 0.7(10) . . . . ? C2 N1 C6 C5 -1.3(8) . . . . ? W1 N1 C6 C5 174.3(4) . . . . ? C2 N1 C6 C7 177.6(5) . . . . ? W1 N1 C6 C7 -6.8(6) . . . . ? C4 C5 C6 N1 0.9(9) . . . . ? C4 C5 C6 C7 -177.9(6) . . . . ? C11 N12 C7 C8 1.3(8) . . . . ? W1 N12 C7 C8 -175.8(4) . . . . ? C11 N12 C7 C6 -177.2(5) . . . . ? W1 N12 C7 C6 5.6(6) . . . . ? N1 C6 C7 N12 0.8(7) . . . . ? C5 C6 C7 N12 179.7(5) . . . . ? N1 C6 C7 C8 -177.7(5) . . . . ? C5 C6 C7 C8 1.2(9) . . . . ? N12 C7 C8 C9 -0.6(9) . . . . ? C6 C7 C8 C9 177.8(6) . . . . ? C11 C10 C9 C8 1.4(11) . . . . ? C7 C8 C9 C10 -0.8(10) . . . . ?