#------------------------------------------------------------------------------ #$Date: 2021-06-11 01:28:52 +0300 (Fri, 11 Jun 2021) $ #$Revision: 266370 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003954.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_4003954 loop_ _publ_author_name 'Mark, Justin' 'Woo, Katherine E.' 'Zhu, Weidi' 'Ji, Bingheng' 'Lee, Shannon J.' 'Adeyemi, Adedoyin N.' 'Sen, Sabyasachi' 'Kovnir, Kirill' _publ_section_title ; Two-Dimensional and Three-Dimensional Tetrel-Arsenide Frameworks Templated by Li and Cs Cations ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/acs.chemmater.1c01053 _journal_year 2021 _chemical_formula_sum 'As7 Ge4.93 Li1.07' _chemical_formula_weight 889.41 _space_group_crystal_system monoclinic _space_group_IT_number 10 _space_group_name_Hall '-P 2y' _space_group_name_H-M_alt 'P 1 2/m 1' _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 93.929(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.0496(6) _cell_length_b 3.7429(2) _cell_length_c 15.3975(8) _cell_measurement_reflns_used 6035 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.522 _cell_measurement_theta_min 2.501 _cell_volume 577.81(6) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6035 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.522 _diffrn_reflns_theta_min 2.501 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 32.498 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 5.112 _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.079 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.031 _refine_diff_density_max 1.571 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.253 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1526 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0267 _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^)+(0.0282P)^2^+1.0354P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.0616 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1283 _reflns_number_total 1526 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cm1c01053_si_003.cif _cod_data_source_block lige5as7 _cod_original_sg_symbol_H-M 'P 2/m' _cod_database_code 4003954 _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_estimated_absorpt_t_min 0.183 _shelx_estimated_absorpt_t_max 0.432 _shelx_res_file ; lige5as7.res created by SHELXL-2014/7 TITL LiGe5As7 in P2/m CELL 0.71073 10.04960 3.74290 15.39750 90.0000 93.9292 90.0000 ZERR 2.00 0.00060 0.00020 0.00080 0.0000 0.0023 0.0000 LATT 1 SYMM -X, Y, -Z SFAC LI GE AS UNIT 2.15 9.85 14 TEMP -173.150 L.S. 18 list 4 BOND FMAP 2 PLAN -20 size .031 .040 .079 acta eadp Ge5 Li5 exyz Ge5 Li5 WGHT 0.028200 1.035400 FVAR 0.05725 0.92317 AS1 3 -0.028769 1.500000 0.076852 10.50000 0.00626 0.00568 = 0.00797 0.00000 -0.00402 0.00000 AS2 3 0.763262 0.000000 0.505934 10.50000 0.00624 0.00643 = 0.00927 0.00000 -0.00500 0.00000 AS3 3 0.465386 0.500000 0.393812 10.50000 0.00675 0.00568 = 0.00881 0.00000 -0.00462 0.00000 AS4 3 0.173979 1.000000 0.273907 10.50000 0.00585 0.00635 = 0.00757 0.00000 -0.00362 0.00000 GE1 2 0.118272 1.000000 0.118328 10.50000 0.00657 0.00502 = 0.00815 0.00000 -0.00482 0.00000 AS5 3 0.319699 1.000000 0.038239 10.50000 0.00825 0.00621 = 0.01118 0.00000 -0.00351 0.00000 GE2 2 0.328610 0.500000 0.256758 10.50000 0.00689 0.00530 = 0.00973 0.00000 -0.00519 0.00000 AS6 3 0.439801 0.500000 0.116504 10.50000 0.01017 0.00761 = 0.01318 0.00000 -0.00489 0.00000 GE3 2 0.614751 0.000000 0.373533 10.50000 0.00635 0.00555 = 0.01249 0.00000 -0.00681 0.00000 AS7 3 0.751496 0.000000 0.249292 10.50000 0.00905 0.00882 = 0.01202 0.00000 -0.00406 0.00000 GE4 2 0.893885 -0.500000 0.455340 10.50000 0.00696 0.00533 = 0.01355 0.00000 -0.00602 0.00000 GE5 2 0.906741 -0.500000 0.292532 20.50000 0.00920 0.00607 = 0.01456 0.00000 -0.00472 0.00000 LI5 1 0.906741 -0.500000 0.292532 -20.50000 0.00920 0.00607 = 0.01456 0.00000 -0.00472 0.00000 LI1 1 0.708456 0.500000 0.107543 10.50000 0.02199 0.05476 = 0.03642 0.00000 0.01123 0.00000 HKLF 4 REM LiGe5As7 in P2/m REM R1 = 0.0267 for 1283 Fo > 4sig(Fo) and 0.0364 for all 1526 data REM 80 parameters refined using 0 restraints END WGHT 0.0282 1.0354 REM Highest difference peak 1.571, deepest hole -1.137, 1-sigma level 0.253 Q1 1 -0.0770 1.5000 0.1189 10.50000 0.05 1.57 Q2 1 0.3775 0.5000 0.2115 10.50000 0.05 1.26 Q3 1 0.5212 0.5000 0.3472 10.50000 0.05 1.20 Q4 1 0.6648 0.0000 0.3267 10.50000 0.05 1.16 Q5 1 0.6996 0.0000 0.2947 10.50000 0.05 1.15 Q6 1 0.5773 -0.5000 0.5562 10.50000 0.05 1.14 Q7 1 0.8621 0.0000 0.6816 10.50000 0.05 1.12 Q8 1 0.1560 1.0000 0.0734 10.50000 0.05 1.12 Q9 1 0.2637 1.0000 0.0812 10.50000 0.05 1.05 Q10 1 0.7160 0.0000 0.5516 10.50000 0.05 1.03 Q11 1 0.6322 1.0000 0.0092 10.50000 0.05 1.00 Q12 1 0.8824 -0.5000 0.3479 10.50000 0.05 1.00 Q13 1 0.0207 1.5000 0.0323 10.50000 0.05 0.99 Q14 1 0.2735 0.5000 0.3026 10.50000 0.05 0.97 Q15 1 0.8176 0.0000 0.4670 10.50000 0.05 0.95 Q16 1 0.3657 0.5000 0.1584 10.50000 0.05 0.93 Q17 1 0.0585 1.0000 0.1627 10.50000 0.05 0.93 Q18 1 0.7940 0.0000 0.2031 10.50000 0.05 0.92 Q19 1 -0.0358 1.5000 0.2539 10.50000 0.05 0.90 Q20 1 0.9607 -0.5000 0.4077 10.50000 0.05 0.89 ; _shelx_res_checksum 28649 _shelx_hkl_file ; 2 0 0 2.74 0.16 -2 0 0 2.56 0.17 3 0 0 0.91 0.12 -3 0 0 0.89 0.13 -4 0 0 7.44 0.38 -4 0 0 7.54 0.39 4 0 0 8.17 0.40 -5 0 0 21.80 0.89 -5 0 0 20.56 0.91 5 0 0 21.87 0.91 -6 0 0 6.60 0.43 6 0 0 7.29 0.47 -6 0 0 7.49 0.46 7 0 0 0.40 0.29 -7 0 0 -0.04 0.23 -7 0 0 -0.28 0.26 8 0 0 2.02 0.39 -8 0 0 2.41 0.41 -8 0 0 2.15 0.38 -9 0 0 60.86 2.51 -10 0 0 0.75 0.38 -11 0 0 -0.12 0.42 -12 0 0 1.63 0.54 -13 0 0 0.46 0.64 0 -1 0 -1.42 0.08 0 -1 0 -1.36 0.09 0 -1 0 -1.51 0.11 0 1 0 -1.38 0.08 0 1 0 -1.27 0.10 0 1 0 -1.42 0.12 1 -1 0 -0.14 0.08 1 -1 0 0.08 0.10 -1 -1 0 0.01 0.13 -1 -1 0 0.06 0.08 -1 -1 0 0.03 0.10 1 1 0 -0.02 0.10 -1 1 0 0.02 0.13 -1 1 0 0.07 0.09 1 1 0 -0.05 0.13 2 -1 0 297.32 11.69 -2 -1 0 303.74 11.72 2 -1 0 307.18 11.70 -2 -1 0 306.63 11.70 -2 1 0 295.07 11.70 2 1 0 308.81 11.71 3 -1 0 2.11 0.26 3 -1 0 2.30 0.18 -3 -1 0 1.80 0.23 -3 1 0 2.12 0.19 3 1 0 1.71 0.21 -3 1 0 1.58 0.18 4 -1 0 0.10 0.13 -4 -1 0 0.16 0.15 4 -1 0 0.09 0.14 -4 1 0 0.08 0.14 4 1 0 0.38 0.17 -4 1 0 0.28 0.14 4 1 0 0.01 0.18 -5 -1 0 39.59 1.64 5 -1 0 42.38 1.62 -5 1 0 38.96 1.62 -5 1 0 37.30 1.59 5 1 0 42.63 1.65 -6 -1 0 0.31 0.21 6 -1 0 0.32 0.23 6 1 0 0.34 0.25 -6 1 0 0.48 0.23 -7 -1 0 1.14 0.28 7 -1 0 1.81 0.30 -7 1 0 0.79 0.25 7 1 0 1.49 0.34 -8 -1 0 35.03 1.56 8 -1 0 37.00 1.56 -8 1 0 36.07 1.54 9 -1 0 39.54 1.92 -9 -1 0 30.95 1.50 -9 1 0 33.62 1.50 -10 -1 0 0.01 0.37 -10 1 0 1.02 0.37 -11 -1 0 15.34 0.94 -11 -1 0 15.40 1.01 -11 1 0 15.20 1.03 -12 -1 0 4.07 0.70 -12 -1 0 3.82 0.63 -12 1 0 5.63 0.91 0 -2 0 954.75 36.29 0 -2 0 1000.00 36.27 0 -2 0 916.39 36.28 0 2 0 889.97 36.27 -1 -2 0 0.73 0.18 -1 -2 0 0.78 0.21 1 -2 0 0.43 0.18 1 -2 0 0.52 0.22 1 -2 0 0.61 0.17 -1 -2 0 0.20 0.24 -1 2 0 0.34 0.22 1 2 0 0.79 0.24 1 2 0 0.50 0.17 -1 2 0 0.74 0.34 1 2 0 0.76 0.15 -2 -2 0 1.43 0.22 2 -2 0 1.74 0.21 -2 -2 0 1.34 0.30 -2 -2 0 1.52 0.19 -2 -2 0 1.17 0.20 2 -2 0 1.50 0.23 -2 2 0 1.14 0.23 2 2 0 1.18 0.21 -2 2 0 1.50 0.25 -3 -2 0 0.62 0.31 3 -2 0 0.53 0.22 -3 -2 0 0.64 0.19 -3 -2 0 0.41 0.19 3 -2 0 0.37 0.20 -3 2 0 0.43 0.19 -3 2 0 0.31 0.24 3 2 0 0.60 0.19 4 -2 0 5.03 0.42 4 -2 0 4.41 0.39 -4 -2 0 4.36 0.40 -4 -2 0 5.21 0.54 4 2 0 5.04 0.34 -4 2 0 4.22 0.34 -4 2 0 4.39 0.40 5 -2 0 13.56 0.66 5 -2 0 13.99 0.64 -5 -2 0 13.27 0.84 -5 -2 0 12.92 0.69 -5 2 0 13.34 0.65 -6 -2 0 5.38 0.48 6 -2 0 5.07 0.46 6 -2 0 4.12 0.48 6 2 0 6.43 0.49 -6 2 0 4.63 0.40 7 -2 0 0.27 0.32 -7 -2 0 -0.31 0.30 7 -2 0 -1.30 0.38 7 2 0 0.25 0.29 -7 2 0 0.34 0.30 -8 -2 0 1.26 0.37 8 -2 0 1.52 0.41 8 2 0 1.80 0.39 -8 2 0 1.86 0.38 -9 -2 0 43.90 1.93 9 -2 0 42.51 1.92 -9 2 0 44.81 1.89 9 2 0 43.43 1.88 -10 -2 0 -0.01 0.47 -10 2 0 0.65 0.51 10 2 0 0.12 0.49 -11 -2 0 0.67 0.47 -11 -2 0 -0.12 0.54 11 2 0 -0.19 0.53 -11 2 0 0.22 0.61 0 -3 0 -0.02 0.30 0 -3 0 -0.40 0.36 0 -3 0 -0.23 0.41 0 3 0 -0.04 0.32 0 3 0 0.02 0.23 1 -3 0 -0.03 0.30 1 -3 0 0.61 0.38 -1 -3 0 0.67 0.39 1 -3 0 0.27 0.30 -1 -3 0 -0.39 0.35 -1 -3 0 -0.38 0.29 -1 3 0 0.26 0.23 1 3 0 -0.14 0.21 1 3 0 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1.31 -8 0 -1 12.82 0.71 8 0 1 13.72 0.80 -8 0 -1 12.48 0.66 -8 0 -1 12.78 0.78 -9 0 -1 8.36 0.63 -10 0 -1 6.24 0.57 -11 0 -1 0.84 0.46 -12 0 -1 0.40 0.53 -12 -1 1 7.69 0.94 -12 -1 1 8.61 0.80 -12 1 1 8.69 0.99 -11 -1 1 15.30 0.98 -11 1 1 14.06 1.00 -10 -1 1 10.06 0.77 -10 1 1 11.51 0.78 9 -1 -1 0.78 0.47 -9 -1 1 0.13 0.33 -9 1 1 0.77 0.33 8 -1 -1 0.12 0.35 -8 -1 1 0.47 0.30 -8 1 1 0.76 0.29 7 -1 -1 -0.02 0.25 -7 -1 1 0.17 0.24 -7 1 1 -0.05 0.24 -7 1 1 -0.47 0.37 6 -1 -1 7.25 0.44 -6 -1 1 6.64 0.45 -6 1 1 6.19 0.40 5 -1 -1 292.30 10.75 -5 -1 1 272.17 10.77 5 -1 -1 289.62 10.73 5 1 -1 262.22 10.75 -5 1 1 272.89 10.73 -5 1 1 276.93 10.75 4 -1 -1 16.93 0.69 4 -1 -1 17.52 0.69 -4 -1 1 16.56 0.72 4 1 -1 15.44 0.70 -4 1 1 15.72 0.68 -4 1 1 15.76 0.69 3 -1 -1 0.59 0.15 -3 -1 1 0.23 0.14 -3 1 1 0.48 0.12 3 1 -1 0.34 0.12 2 -1 -1 231.92 8.84 -2 -1 1 228.62 8.83 -2 -1 1 227.06 8.85 2 -1 -1 232.94 8.85 -2 -1 1 237.75 8.84 -2 1 1 223.00 8.84 2 1 -1 222.18 8.83 2 1 -1 226.82 8.84 -1 -1 1 0.00 0.10 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-14 0.95 0.56 -2 -3 -14 0.18 0.56 -2 3 -14 0.91 0.61 2 3 14 1.14 0.58 2 3 14 0.08 0.55 -3 -3 -14 22.43 1.29 -3 -3 -14 23.94 1.35 3 3 14 22.69 1.28 -3 3 -14 24.38 1.27 3 3 14 19.80 1.34 -4 -3 -14 3.56 0.66 -4 -3 -14 4.07 0.67 4 3 14 4.35 0.64 4 3 14 3.66 0.70 -4 3 -14 3.80 0.70 9 0 -15 -0.29 0.61 -9 0 15 0.70 0.61 -8 0 15 0.38 0.50 -8 0 15 -0.06 0.47 8 0 -15 0.40 0.54 -7 0 15 10.58 0.84 -7 0 15 10.85 0.77 7 0 -15 8.93 0.88 6 0 -15 39.03 1.74 5 0 -15 0.24 0.47 4 0 -15 2.83 0.47 3 0 -15 54.68 2.29 -2 0 15 18.23 0.91 2 0 -15 20.17 1.01 2 0 -15 19.31 1.08 1 0 -15 1.75 0.44 -1 0 15 1.68 0.32 1 0 -15 2.32 0.44 0 0 15 0.06 0.27 0 0 -15 0.27 0.42 1 0 15 0.47 0.32 -1 0 -15 0.06 0.42 2 0 15 2.14 0.36 -3 0 -15 6.62 0.72 3 0 15 6.24 0.61 4 0 15 7.97 0.70 -4 0 -15 8.11 0.81 -5 0 -15 0.52 0.48 5 0 15 0.21 0.39 -6 0 -15 -0.65 0.52 -7 0 -15 47.33 2.17 8 -1 -15 0.67 0.55 -8 -1 15 0.15 0.57 -8 1 15 -0.18 0.54 7 -1 -15 10.75 0.94 -7 1 15 9.13 0.88 7 1 -15 9.89 0.92 6 -1 -15 4.66 0.78 -6 1 15 4.59 0.71 6 1 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2 15 7.44 0.94 6 -2 -15 30.31 1.65 -6 2 15 32.71 1.59 5 -2 -15 0.29 0.63 -5 2 15 1.14 0.61 -5 2 15 0.00 0.47 4 -2 -15 1.15 0.59 4 -2 -15 1.96 0.61 -4 2 15 1.64 0.48 -4 2 15 1.77 0.59 3 -2 -15 43.08 2.01 3 -2 -15 43.00 2.00 -3 2 15 43.97 1.92 -3 2 15 45.78 2.02 2 -2 -15 14.65 1.01 2 -2 -15 13.57 0.99 -2 2 15 13.30 1.02 -2 2 15 15.32 0.90 1 -2 -15 1.44 0.48 1 -2 -15 1.40 0.50 -1 2 15 0.68 0.41 -1 2 15 1.79 0.56 0 -2 -15 -0.08 0.47 0 -2 -15 -0.53 0.44 0 2 15 -0.33 0.57 0 2 15 0.13 0.43 -1 -2 -15 -0.20 0.46 -1 -2 -15 0.53 0.51 1 2 15 -0.36 0.58 -1 2 -15 0.58 0.46 1 2 15 0.17 0.45 -2 -2 -15 1.90 0.53 -2 -2 -15 1.40 0.51 2 2 15 2.86 0.85 2 2 15 1.29 0.46 -2 2 -15 1.54 0.44 2 2 15 1.04 0.58 -3 -2 -15 5.05 0.74 -3 -2 -15 5.11 0.80 3 2 15 3.86 0.69 3 2 15 3.69 0.66 -3 2 -15 3.66 0.65 -4 -2 -15 4.95 0.76 -4 -2 -15 6.05 0.87 4 2 15 4.48 0.68 4 2 15 6.82 0.79 -4 2 -15 6.42 0.74 -5 -2 -15 0.98 0.54 -5 -2 -15 -0.30 0.52 5 2 15 -0.07 0.61 -5 2 -15 -0.20 0.58 5 2 15 -0.10 0.53 -6 -2 -15 -0.93 0.60 -6 -2 -15 0.15 0.56 -6 -2 -15 0.14 0.55 6 2 15 0.32 0.60 -6 2 -15 -0.10 0.63 3 -3 -15 9.34 1.16 -3 3 15 9.48 0.99 -3 3 15 11.32 1.12 2 -3 -15 6.21 1.03 -2 3 15 6.00 1.02 -2 3 15 5.95 0.91 1 -3 -15 29.40 1.54 1 -3 -15 26.80 1.55 1 3 -15 30.33 1.48 -1 3 15 26.92 1.59 -1 3 15 29.48 1.49 0 -3 -15 17.74 1.24 0 -3 -15 17.51 1.22 0 3 15 18.52 1.26 0 3 15 16.67 1.13 0 3 -15 18.41 1.16 -1 -3 -15 0.57 0.67 -1 -3 -15 0.13 0.62 -1 3 -15 0.14 0.63 1 3 15 -0.04 0.56 1 3 15 1.48 0.68 -2 -3 -15 6.75 1.00 -2 -3 -15 6.95 0.94 2 3 15 5.63 0.96 2 3 15 7.06 0.99 -2 3 -15 7.42 0.90 -8 0 16 6.12 0.82 -8 0 16 6.39 0.88 7 0 -16 1.54 0.56 -7 0 16 1.71 0.49 6 0 -16 11.88 0.90 5 0 -16 -0.21 0.51 4 0 -16 1.32 0.48 3 0 -16 -0.04 0.45 2 0 -16 6.21 0.74 -2 0 16 6.81 0.57 1 0 -16 5.49 0.71 -1 0 16 5.32 0.52 0 0 -16 16.12 1.02 0 0 16 16.51 0.86 1 0 16 0.65 0.32 -1 0 -16 0.13 0.46 -2 0 -16 0.33 0.45 2 0 16 0.51 0.34 3 0 16 4.68 0.61 -3 0 -16 4.77 0.74 -4 0 -16 6.68 0.85 4 0 16 6.28 0.69 -5 0 -16 10.96 0.96 5 0 16 10.26 0.85 6 0 16 13.15 0.95 -6 0 -16 16.16 1.16 -7 0 -16 4.65 0.80 7 0 16 4.43 0.76 -8 -1 16 101.38 4.00 -8 1 16 91.06 3.90 7 -1 -16 0.51 0.58 7 1 -16 1.22 0.59 -7 1 16 0.39 0.57 6 -1 -16 6.31 0.90 6 1 -16 7.75 0.89 -6 1 16 8.91 0.83 5 -1 -16 0.62 0.54 -5 1 16 0.79 0.41 -5 1 16 0.56 0.47 4 -1 -16 1.06 0.54 -4 1 16 0.89 0.48 -4 1 16 0.33 0.43 3 -1 -16 0.42 0.51 3 -1 -16 0.31 0.50 -3 1 16 0.76 0.38 -3 1 16 1.08 0.45 2 -1 -16 1.42 0.50 2 -1 -16 0.85 0.54 -2 1 16 1.43 0.42 -2 1 16 2.29 0.53 1 -1 -16 0.60 0.47 1 -1 -16 -0.58 0.49 -1 1 16 -0.09 0.38 -1 1 16 0.44 0.65 0 -1 16 3.09 0.49 0 -1 -16 3.50 0.51 0 -1 -16 3.02 0.53 0 1 16 3.47 0.55 0 1 16 1.38 0.87 -1 -1 -16 6.74 0.74 -1 -1 -16 6.84 0.78 1 -1 16 7.16 0.61 -1 1 -16 7.12 0.85 1 1 16 7.07 0.64 -2 -1 -16 5.69 0.77 -2 -1 -16 5.94 0.74 2 1 16 6.02 0.67 -2 1 -16 4.81 0.80 -3 -1 -16 9.76 0.80 -3 -1 -16 10.24 0.91 3 1 16 9.54 0.80 -3 1 -16 8.56 0.95 -4 -1 -16 6.73 0.76 -4 -1 -16 5.82 0.86 -4 1 -16 5.67 0.67 -4 1 -16 5.53 0.93 4 1 16 4.96 0.75 -5 -1 -16 0.95 0.58 -5 -1 -16 0.13 0.51 5 1 16 0.09 0.47 -5 1 -16 -0.72 0.62 -6 -1 -16 76.67 3.05 -6 -1 -16 75.81 3.13 -6 1 -16 69.97 3.14 6 1 16 69.15 3.06 6 -2 -16 11.54 1.17 -6 2 16 11.15 1.05 5 -2 -16 0.62 0.67 -5 2 16 -0.01 0.51 -5 2 16 -0.04 0.63 4 -2 -16 1.29 0.66 4 -2 -16 0.98 0.65 -4 2 16 0.70 0.60 -4 2 16 0.48 0.52 3 -2 -16 -0.50 0.58 3 -2 -16 -0.04 0.57 -3 2 16 -0.08 0.63 -3 2 16 0.02 0.49 2 -2 -16 5.46 0.88 2 -2 -16 6.12 0.90 -2 2 16 4.08 0.69 -2 2 16 5.05 0.74 1 -2 -16 3.65 0.62 1 -2 -16 4.27 0.64 -1 2 16 3.43 0.67 -1 2 16 5.20 0.68 0 -2 -16 12.62 0.97 0 -2 -16 12.33 1.00 0 2 16 11.91 1.07 0 2 16 11.93 0.91 -1 -2 -16 0.25 0.51 -1 -2 -16 -1.06 0.51 1 2 16 -0.25 0.61 1 2 16 0.02 0.45 -2 -2 -16 -0.47 0.54 -2 -2 -16 -0.10 0.57 2 2 16 -0.10 0.52 -2 2 -16 0.58 0.50 2 2 16 -0.86 0.59 -3 -2 -16 3.76 0.63 -3 -2 -16 4.04 0.61 -3 2 -16 3.30 0.57 3 2 16 4.47 0.78 3 2 16 1.54 0.62 -4 -2 -16 6.89 0.93 -4 -2 -16 5.06 0.66 4 2 16 3.78 0.72 4 2 16 4.59 0.86 -4 2 -16 5.78 0.75 -5 -2 -16 8.72 1.04 5 2 16 8.81 0.99 7 0 -17 2.16 0.61 -7 0 17 2.33 0.55 6 0 -17 16.70 1.07 5 0 -17 15.26 1.01 4 0 -17 -0.06 0.53 3 0 -17 8.21 0.84 2 0 -17 21.97 1.19 -2 0 17 21.72 1.06 -1 0 17 -0.22 0.35 1 0 -17 0.24 0.51 0 0 17 2.50 0.42 0 0 -17 2.19 0.57 1 0 17 13.94 0.83 -1 0 -17 13.30 1.02 -2 0 -17 1.89 0.59 2 0 17 1.14 0.43 -3 0 -17 4.12 0.64 3 0 17 5.50 0.67 4 0 17 16.74 1.02 -4 0 -17 17.34 1.15 5 0 17 0.24 0.50 -5 0 -17 -1.00 0.61 6 0 17 2.76 0.56 -6 0 -17 3.85 0.72 7 -1 -17 4.20 0.72 -7 1 17 3.43 0.65 7 1 -17 3.94 0.68 6 -1 -17 4.84 0.72 -6 1 17 5.77 0.83 6 1 -17 4.64 0.68 5 -1 -17 3.37 0.67 -5 1 17 6.24 0.71 -5 1 17 5.11 0.79 4 -1 -17 4.53 0.65 -4 1 17 4.28 0.68 -4 1 17 3.15 0.59 3 -1 -17 0.57 0.61 3 -1 -17 1.62 0.58 -3 1 17 2.12 0.44 -3 1 17 1.20 0.49 2 -1 -17 2.30 0.56 2 -1 -17 0.74 0.55 -2 1 17 2.66 0.56 -2 1 17 1.66 0.48 1 -1 -17 9.65 0.88 1 -1 -17 8.59 0.94 -1 1 17 9.13 0.71 0 -1 -17 5.00 0.79 0 -1 17 5.76 0.53 0 -1 -17 6.22 0.86 -1 -1 -17 32.29 1.61 -1 -1 -17 31.99 1.55 1 -1 17 33.43 1.47 -1 1 -17 32.97 1.65 1 1 17 32.75 1.51 2 -1 17 -0.23 0.38 -2 -1 -17 1.37 0.57 -2 -1 -17 0.61 0.51 -2 1 -17 0.30 0.58 2 1 17 0.29 0.44 -3 -1 -17 -0.16 0.53 -3 -1 -17 -1.14 0.51 -3 1 -17 -0.87 0.59 3 1 17 0.18 0.48 -4 -1 -17 3.01 0.58 -4 -1 -17 1.95 0.63 -4 1 -17 2.13 0.70 4 1 17 1.46 0.55 -5 -1 -17 42.81 2.06 -5 -1 -17 44.41 1.96 5 1 17 40.89 1.95 -5 1 -17 42.51 2.09 -5 1 -17 41.63 1.90 5 -2 -17 11.79 1.22 -5 2 17 11.01 1.17 -5 2 17 13.48 1.03 4 -2 -17 -0.14 0.69 -4 2 17 0.54 0.58 -4 2 17 0.17 0.63 3 -2 -17 6.79 1.00 3 -2 -17 6.27 1.01 -3 2 17 5.93 1.02 -3 2 17 5.55 0.84 2 -2 -17 18.08 1.21 2 -2 -17 17.00 1.26 -2 2 17 19.12 1.10 -2 2 17 15.61 1.19 1 -2 -17 0.30 0.61 1 -2 -17 -0.47 0.63 -1 2 17 0.09 0.46 -1 2 17 0.34 0.67 0 -2 -17 1.24 0.59 0 -2 -17 2.01 0.60 0 2 17 1.46 0.54 0 2 17 2.69 0.70 -1 -2 -17 9.60 1.04 -1 -2 -17 11.18 1.01 1 2 17 11.17 0.88 1 2 17 9.46 1.14 -2 -2 -17 -0.16 0.61 -2 -2 -17 1.18 0.62 2 2 17 0.65 0.55 2 2 17 0.73 0.69 -3 -2 -17 3.64 0.66 -3 -2 -17 3.62 0.76 -3 2 -17 3.68 0.65 3 2 17 3.31 0.73 3 2 17 3.41 0.61 -6 0 18 1.36 0.51 6 0 -18 0.58 0.58 5 0 -18 0.11 0.59 4 0 -18 25.67 1.37 3 0 -18 15.53 1.08 2 0 -18 1.54 0.61 -2 0 18 0.33 0.37 -1 0 18 12.62 0.78 1 0 -18 11.46 1.05 0 0 -18 2.84 0.65 0 0 18 2.83 0.45 -1 0 -18 3.62 0.71 1 0 18 5.47 0.66 2 0 18 12.35 0.88 -2 0 -18 13.73 1.10 3 0 18 54.57 2.40 -3 0 -18 58.51 2.53 4 0 18 8.90 0.85 -4 0 -18 10.65 1.07 5 -1 -18 0.01 0.63 -5 1 18 0.91 0.56 -5 1 18 1.54 0.50 4 -1 -18 3.38 0.68 -4 1 18 2.64 0.60 -4 1 18 2.97 0.56 3 -1 -18 19.81 1.29 -3 1 18 21.10 1.12 -3 1 18 20.35 1.18 2 -1 -18 0.41 0.60 2 -1 -18 0.74 0.60 -2 1 18 1.33 0.58 -2 1 18 0.75 0.50 1 -1 -18 20.78 1.24 1 -1 -18 20.38 1.32 -1 1 18 21.08 1.15 0 -1 -18 0.41 0.55 0 -1 18 0.18 0.38 0 -1 -18 -0.78 0.59 0 1 18 0.53 0.49 1 -1 18 10.59 0.77 -1 -1 -18 10.10 1.01 -1 -1 -18 9.69 0.92 1 1 18 9.93 0.82 -2 -1 -18 17.95 1.07 -2 -1 -18 15.42 1.12 2 -1 18 15.13 0.94 2 1 18 14.03 0.99 -2 1 -18 14.85 1.21 -3 -1 -18 13.84 1.04 3 -1 18 9.62 0.88 -3 -1 -18 11.19 1.11 3 1 18 14.64 0.97 -3 1 -18 11.87 1.14 -4 -1 -18 22.01 1.29 -4 -1 -18 21.81 1.42 4 1 18 21.15 1.28 -4 1 -18 20.23 1.42 2 -2 -18 0.13 0.74 2 -2 -18 1.58 0.72 -2 2 18 1.09 0.59 -2 2 18 -0.01 0.69 1 -2 -18 9.23 1.15 1 -2 -18 11.37 1.09 -1 2 18 9.85 0.92 -1 2 18 9.73 1.15 0 -2 -18 2.95 0.70 0 -2 -18 1.96 0.70 0 2 18 3.66 0.78 0 2 18 4.59 0.85 -1 -2 -18 3.00 0.75 -1 -2 -18 3.27 0.70 1 2 18 3.59 0.79 1 2 18 3.59 0.65 4 0 -19 37.71 1.82 3 0 -19 3.81 0.69 1 0 -19 0.44 0.67 -1 0 19 -0.54 0.43 0 0 -19 8.50 0.99 0 0 19 7.67 0.76 1 0 19 25.67 1.31 -1 0 -19 26.17 1.53 -2 0 -19 49.28 2.32 2 0 19 49.52 2.17 3 0 19 0.43 0.52 -3 0 -19 0.86 0.75 3 -1 -19 16.65 1.23 -3 1 19 17.15 1.14 -3 1 19 16.16 1.10 2 -1 -19 43.99 2.12 -2 1 19 47.90 2.10 1 -1 -19 10.27 1.06 1 -1 -19 10.85 1.13 -1 1 19 10.26 0.93 0 -1 -19 8.99 0.98 0 -1 -19 6.77 1.07 0 -1 19 6.99 0.74 0 1 19 7.45 0.83 -1 -1 -19 0.48 0.63 -1 -1 -19 0.16 0.72 1 -1 19 -0.08 0.45 1 1 19 0.41 0.53 2 -1 19 1.01 0.52 -2 -1 -19 0.56 0.62 -2 -1 -19 0.52 0.71 -2 1 -19 1.55 0.73 2 1 19 1.27 0.58 -1 0 20 2.52 0.57 ; _shelx_hkl_checksum 11622 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' '-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 As1 As -0.02877(7) 1.5000 0.07685(5) 0.00684(17) Uani 1 2 d S T P . . As2 As 0.76326(8) 0.0000 0.50593(5) 0.00757(17) Uani 1 2 d S T P . . As3 As 0.46539(8) 0.5000 0.39381(5) 0.00732(16) Uani 1 2 d S T P . . As4 As 0.17398(7) 1.0000 0.27391(5) 0.00678(17) Uani 1 2 d S T P . . Ge1 Ge 0.11827(8) 1.0000 0.11833(5) 0.00683(17) Uani 1 2 d S T P . . As5 As 0.31970(8) 1.0000 0.03824(5) 0.00874(17) Uani 1 2 d S T P . . Ge2 Ge 0.32861(8) 0.5000 0.25676(5) 0.00757(17) Uani 1 2 d S T P . . As6 As 0.43980(8) 0.5000 0.11650(5) 0.01058(18) Uani 1 2 d S T P . . Ge3 Ge 0.61475(8) 0.0000 0.37353(5) 0.00847(18) Uani 1 2 d S T P . . As7 As 0.75150(8) 0.0000 0.24929(5) 0.01018(18) Uani 1 2 d S T P . . Ge4 Ge 0.89388(8) -0.5000 0.45534(5) 0.00892(18) Uani 1 2 d S T P . . Ge5 Ge 0.90674(9) -0.5000 0.29253(5) 0.0102(3) Uani 0.923(4) 2 d S T P . . Li5 Li 0.90674(9) -0.5000 0.29253(5) 0.0102(3) Uani 0.077(4) 2 d S T P . . Li1 Li 0.7085(17) 0.5000 0.1075(11) 0.037(4) Uani 1 2 d S T P . . 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 As1 0.0063(4) 0.0057(4) 0.0080(3) 0.000 -0.0040(3) 0.000 As2 0.0062(4) 0.0064(4) 0.0093(4) 0.000 -0.0050(3) 0.000 As3 0.0068(4) 0.0057(4) 0.0088(3) 0.000 -0.0046(3) 0.000 As4 0.0059(4) 0.0064(4) 0.0076(3) 0.000 -0.0036(3) 0.000 Ge1 0.0066(4) 0.0050(4) 0.0082(4) 0.000 -0.0048(3) 0.000 As5 0.0082(4) 0.0062(4) 0.0112(4) 0.000 -0.0035(3) 0.000 Ge2 0.0069(4) 0.0053(4) 0.0097(4) 0.000 -0.0052(3) 0.000 As6 0.0102(4) 0.0076(4) 0.0132(4) 0.000 -0.0049(3) 0.000 Ge3 0.0063(4) 0.0056(4) 0.0125(4) 0.000 -0.0068(3) 0.000 As7 0.0090(4) 0.0088(4) 0.0120(4) 0.000 -0.0041(3) 0.000 Ge4 0.0070(4) 0.0053(4) 0.0136(4) 0.000 -0.0060(3) 0.000 Ge5 0.0092(5) 0.0061(5) 0.0146(5) 0.000 -0.0047(3) 0.000 Li5 0.0092(5) 0.0061(5) 0.0146(5) 0.000 -0.0047(3) 0.000 Li1 0.022(9) 0.055(12) 0.036(10) 0.000 0.011(8) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 Ge1 As1 Ge1 100.04(4) . 1_565 ? Ge1 As1 As1 94.20(3) . 3_585 ? Ge1 As1 As1 94.20(3) 1_565 3_585 ? Ge1 As1 Li1 122.20(16) . 1_465 ? Ge1 As1 Li1 122.20(16) 1_565 1_465 ? As1 As1 Li1 117.4(4) 3_585 1_465 ? Ge3 As2 Ge4 92.57(3) . 1_565 ? Ge3 As2 Ge4 92.57(3) . . ? Ge4 As2 Ge4 99.95(4) 1_565 . ? Ge3 As3 Ge3 100.59(4) . 1_565 ? Ge3 As3 Ge2 101.84(3) . . ? Ge3 As3 Ge2 101.84(3) 1_565 . ? Ge1 As4 Ge2 89.93(3) . . ? Ge1 As4 Ge2 89.93(3) . 1_565 ? Ge2 As4 Ge2 99.15(4) . 1_565 ? As4 Ge1 As5 110.86(4) . . ? As4 Ge1 As1 110.69(3) . . ? As5 Ge1 As1 112.07(3) . . ? As4 Ge1 As1 110.69(3) . 1_545 ? As5 Ge1 As1 112.07(3) . 1_545 ? As1 Ge1 As1 100.04(4) . 1_545 ? Ge1 As5 As6 98.43(3) . 1_565 ? Ge1 As5 As6 98.43(3) . . ? As6 As5 As6 97.33(3) 1_565 . ? Ge1 As5 Li1 110.4(3) . 3_665 ? As6 As5 Li1 150.5(3) 1_565 3_665 ? As6 As5 Li1 84.8(3) . 3_665 ? Ge1 As5 Li1 110.4(3) . 3_675 ? As6 As5 Li1 84.8(3) 1_565 3_675 ? As6 As5 Li1 150.5(3) . 3_675 ? Li1 As5 Li1 79.7(4) 3_665 3_675 ? As3 Ge2 As4 103.30(3) . 1_545 ? As3 Ge2 As4 103.30(3) . . ? As4 Ge2 As4 99.16(4) 1_545 . ? As3 Ge2 As6 119.28(4) . . ? As4 Ge2 As6 114.60(3) 1_545 . ? As4 Ge2 As6 114.60(3) . . ? As5 As6 As5 97.33(3) 1_545 . ? As5 As6 Ge2 100.80(3) 1_545 . ? As5 As6 Ge2 100.80(3) . . ? As5 As6 Li1 115.2(2) 1_545 . ? As5 As6 Li1 115.2(2) . . ? Ge2 As6 Li1 123.3(4) . . ? As7 Ge3 As3 119.22(3) . . ? As7 Ge3 As3 119.22(3) . 1_545 ? As3 Ge3 As3 100.59(4) . 1_545 ? As7 Ge3 As2 108.11(4) . . ? As3 Ge3 As2 103.89(3) . . ? As3 Ge3 As2 103.89(3) 1_545 . ? Ge3 As7 Li5 99.60(3) . 1_565 ? Ge3 As7 Ge5 99.60(3) . 1_565 ? Li5 As7 Ge5 0.0 1_565 1_565 ? Ge3 As7 Ge5 99.60(3) . . ? Li5 As7 Ge5 97.1 1_565 . ? Ge5 As7 Ge5 97.07(4) 1_565 . ? Ge3 As7 Li1 122.1(3) . 1_545 ? Li5 As7 Li1 138.3(3) 1_565 1_545 ? Ge5 As7 Li1 138.3(3) 1_565 1_545 ? Ge5 As7 Li1 76.9(3) . 1_545 ? Ge3 As7 Li1 122.1(3) . . ? Li5 As7 Li1 76.9(3) 1_565 . ? Ge5 As7 Li1 76.9(3) 1_565 . ? Ge5 As7 Li1 138.3(3) . . ? Li1 As7 Li1 80.9(5) 1_545 . ? As2 Ge4 As2 99.95(4) . 1_545 ? As2 Ge4 Ge4 106.63(3) . 3_746 ? As2 Ge4 Ge4 106.63(3) 1_545 3_746 ? As2 Ge4 Ge5 112.49(3) . . ? As2 Ge4 Ge5 112.49(3) 1_545 . ? Ge4 Ge4 Ge5 117.08(6) 3_746 . ? As7 Ge5 As7 97.07(4) . 1_545 ? As7 Ge5 Ge4 101.05(3) . . ? As7 Ge5 Ge4 101.05(3) 1_545 . ? As6 Li1 As1 172.9(7) . 1_645 ? As6 Li1 As7 93.4(4) . 1_565 ? As1 Li1 As7 92.0(5) 1_645 1_565 ? As6 Li1 As7 93.4(4) . . ? As1 Li1 As7 92.0(5) 1_645 . ? As7 Li1 As7 80.9(5) 1_565 . ? As6 Li1 As5 89.7(5) . 3_665 ? As1 Li1 As5 84.9(4) 1_645 3_665 ? As7 Li1 As5 176.8(7) 1_565 3_665 ? As7 Li1 As5 99.63(3) . 3_665 ? As6 Li1 As5 89.7(5) . 3_675 ? As1 Li1 As5 84.9(4) 1_645 3_675 ? As7 Li1 As5 99.63(3) 1_565 3_675 ? As7 Li1 As5 176.8(7) . 3_675 ? As5 Li1 As5 79.7(4) 3_665 3_675 ? As6 Li1 Li5 119.4(6) . 1_565 ? As1 Li1 Li5 67.7(4) 1_645 1_565 ? As7 Li1 Li5 46.3(3) 1_565 1_565 ? As7 Li1 Li5 46.3(3) . 1_565 ? As5 Li1 Li5 132.2(4) 3_665 1_565 ? As5 Li1 Li5 132.2(4) 3_675 1_565 ? 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 As1 Ge1 2.4422(7) . ? As1 Ge1 2.4422(7) 1_565 ? As1 As1 2.4745(15) 3_585 ? As1 Li1 2.714(17) 1_465 ? As2 Ge3 2.4427(10) . ? As2 Ge4 2.4439(8) 1_565 ? As2 Ge4 2.4439(8) . ? As3 Ge3 2.4325(7) . ? As3 Ge3 2.4325(7) 1_565 ? As3 Ge2 2.4383(10) . ? As4 Ge1 2.4224(10) . ? As4 Ge2 2.4583(7) . ? As4 Ge2 2.4583(7) 1_565 ? Ge1 As5 2.4414(11) . ? Ge1 As1 2.4422(7) 1_545 ? As5 As6 2.4924(7) 1_565 ? As5 As6 2.4924(7) . ? As5 Li1 2.921(13) 3_665 ? As5 Li1 2.921(13) 3_675 ? Ge2 As4 2.4583(7) 1_545 ? Ge2 As6 2.4986(11) . ? As6 As5 2.4924(7) 1_545 ? As6 Li1 2.713(17) . ? Ge3 As7 2.4307(11) . ? Ge3 As3 2.4325(7) 1_545 ? As7 Li5 2.4975(7) 1_565 ? As7 Ge5 2.4975(7) 1_565 ? As7 Ge5 2.4975(7) . ? As7 Li1 2.885(13) 1_545 ? As7 Li1 2.885(13) . ? Ge4 As2 2.4439(8) 1_545 ? Ge4 Ge4 2.4574(15) 3_746 ? Ge4 Ge5 2.5190(12) . ? Ge5 As7 2.4975(7) 1_545 ? Li1 As1 2.714(17) 1_645 ? Li1 As7 2.885(13) 1_565 ? Li1 As5 2.921(13) 3_665 ? Li1 As5 2.921(13) 3_675 ? Li1 Li5 3.362(18) 1_565 ?