#------------------------------------------------------------------------------ #$Date: 2024-05-18 04:52:03 +0300 (Sat, 18 May 2024) $ #$Revision: 291952 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023132.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023132 loop_ _publ_author_name 'Carneiro Neto, Jos\'e Severiano' 'Iwaya, Eduardo Mariano' 'Santana, Francielli Sousa' 'Soares, Ja\'isa Fernandes' _publ_section_title ; Crystal structure of a three-coordinate lithium complex with monodentate phenyloxazoline and hexamethyldisilylamide ligands ; _journal_coeditor_code EJ2003 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024004237 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Li (C6 H18 N Si2) (C11 H13 N O)2]' _chemical_formula_moiety 'C28 H44 Li N3 O2 Si2' _chemical_formula_structural '[Li(N(Si(CH3)3)2)(NC7H5OC4H8)2]' _chemical_formula_sum 'C28 H44 Li N3 O2 Si2' _chemical_formula_weight 517.78 _chemical_name_systematic Bis(4,4-dimethyl-2-phenyl-2-oxazoline-\kN)(hexamethyldisilylamido-\kN)lithium _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 116.243(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.612(2) _cell_length_b 12.7649(17) _cell_length_c 17.180(4) _cell_measurement_reflns_used 9967 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.66 _cell_measurement_theta_min 2.85 _cell_volume 3070.8(9) _computing_cell_refinement ; APEX3 and SAINT (Bruker, 2015) ; _computing_data_collection ; APEX3 and SAINT (Bruker, 2015) ; _computing_data_reduction ; APEX3 and SAINT (Bruker, 2015) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 1999, v. 4.6.4) and Mercury (Macrae et al., 2020, v. 2023.3.1) ; _computing_publication_material ; WINGX (Farrugia, 2012) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS2008 (Sheldrick 2008) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture/Photon 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_unetI/netI 0.0294 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 44358 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 2.848 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.120 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.497 _exptl_crystal_size_mid 0.436 _exptl_crystal_size_min 0.284 _refine_diff_density_max 0.294 _refine_diff_density_min -0.235 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 252 _refine_ls_number_reflns 3522 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0352 _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^)+(0.0461P)^2^+1.6645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.0915 _reflns_number_gt 2888 _reflns_number_total 3522 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ej2003.cif _cod_data_source_block I _cod_original_cell_volume 3070.9(9) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2023132 _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_hkl_file ; 4 0 -4 763.72 38.77 4 0 -4 811.24 38.89 4 0 -4 777.24 38.77 -4 0 4 774.96 38.76 -4 0 4 827.92 38.90 -4 0 4 777.97 38.76 6 0 -6 1.15 0.53 6 0 -6 1.15 0.52 -6 0 6 1.17 0.48 -6 0 6 1.01 0.53 8 0 -8 54.56 3.13 8 0 -8 55.00 3.09 8 0 -8 55.16 3.48 -8 0 8 51.96 3.42 -8 0 8 54.39 3.04 -8 0 8 59.38 3.10 10 0 -10 109.32 6.36 10 0 -10 102.94 5.96 10 0 -10 113.82 6.01 -10 0 10 117.12 5.95 -10 0 10 121.19 5.94 12 0 -12 1.20 1.04 12 0 -12 0.09 0.91 12 0 -12 1.14 1.58 -12 0 12 0.57 0.90 -12 0 12 1.33 0.86 -12 0 12 -1.48 1.24 14 0 -14 2.31 1.29 14 0 -14 1.59 1.94 14 0 -14 3.15 1.27 -14 0 14 4.71 1.21 -14 0 14 3.95 1.15 -14 0 14 5.29 1.57 16 0 -16 3.15 1.56 16 0 -16 4.34 1.57 -16 0 16 3.55 1.79 -16 0 16 2.62 1.38 -16 0 16 2.56 0.78 18 0 -18 16.35 2.23 18 0 -18 11.80 2.24 18 0 -18 13.76 2.74 -18 0 18 11.51 1.81 -18 0 18 11.58 1.95 -18 0 18 16.21 2.87 -17 1 17 1.06 1.59 -17 1 17 -0.89 0.80 -17 1 17 2.23 1.85 -17 1 17 0.44 1.48 17 -1 -17 0.68 1.72 17 -1 -17 -3.77 1.55 -15 1 15 -0.25 1.18 -15 1 15 0.35 1.47 15 -1 -15 0.78 1.34 15 -1 -15 1.84 1.40 -13 1 13 12.09 1.46 -13 1 13 13.71 1.80 -13 1 13 14.92 1.57 13 -1 -13 12.11 2.10 13 -1 -13 10.25 1.55 13 -1 -13 18.16 2.08 -11 1 11 0.17 0.81 -11 1 11 -0.93 0.87 11 -1 -11 -0.31 0.85 11 -1 -11 1.61 1.38 11 -1 -11 0.13 0.89 -9 1 9 236.68 12.12 -9 1 9 241.84 12.11 9 -1 -9 236.77 12.33 9 -1 -9 236.24 12.15 9 -1 -9 249.83 12.16 -7 1 7 19.03 1.38 -7 1 7 17.79 1.42 7 -1 -7 16.40 1.38 7 -1 -7 14.38 1.71 7 -1 -7 18.43 1.42 -5 1 5 67.71 3.68 -5 1 5 67.57 3.57 -5 1 5 62.87 3.56 5 -1 -5 70.53 3.69 5 -1 -5 67.44 3.59 5 -1 -5 71.52 3.60 -3 1 3 10.23 0.88 -3 1 3 11.12 0.90 -3 1 3 9.93 0.62 3 -1 -3 10.95 0.94 3 -1 -3 9.28 0.93 3 -1 -3 9.06 0.93 3 1 -3 10.50 1.32 3 1 -3 9.29 0.78 3 1 -3 9.41 0.79 -3 -1 3 11.71 0.72 -3 -1 3 9.24 0.76 -3 -1 3 9.09 0.74 -3 -1 3 8.34 1.30 5 1 -5 78.31 4.11 5 1 -5 70.10 3.77 5 1 -5 67.33 3.75 -5 -1 5 69.66 3.73 -5 -1 5 69.45 3.74 -5 -1 5 83.08 4.14 7 1 -7 17.22 1.31 7 1 -7 16.79 2.01 7 1 -7 15.00 1.32 -7 -1 7 15.99 1.26 -7 -1 7 17.50 1.23 -7 -1 7 15.94 1.82 9 1 -9 245.69 12.50 9 1 -9 233.50 12.11 9 1 -9 246.13 12.13 -9 -1 9 243.23 12.05 -9 -1 9 234.31 12.48 -9 -1 9 239.10 12.06 11 1 -11 -0.26 0.87 11 1 -11 0.66 0.88 11 1 -11 -2.68 1.41 -11 -1 11 -0.75 0.72 -11 -1 11 0.39 1.20 -11 -1 11 0.23 0.70 -11 -1 11 -0.20 0.54 13 1 -13 11.66 1.49 13 1 -13 10.83 2.21 13 1 -13 10.26 1.44 -13 -1 13 10.63 1.25 -13 -1 13 12.29 1.86 -13 -1 13 11.86 1.22 -13 -1 13 11.70 1.31 15 1 -15 1.50 1.35 15 1 -15 -4.24 1.84 15 1 -15 -1.39 1.20 -15 -1 15 -1.16 1.50 -15 -1 15 -1.52 1.07 -15 -1 15 -0.35 0.99 -15 -1 15 0.29 0.61 17 1 -17 -0.63 2.07 17 1 -17 -1.82 1.59 17 1 -17 0.41 1.65 -17 -1 17 2.52 2.18 -17 -1 17 -1.07 1.31 -18 2 18 12.91 2.66 -16 2 16 -0.60 1.38 -16 2 16 -0.02 1.64 -16 2 16 1.92 1.43 16 -2 -16 4.48 1.72 16 -2 -16 2.19 1.56 -14 2 14 24.17 2.78 -14 2 14 34.17 2.58 14 -2 -14 27.31 2.64 14 -2 -14 25.09 2.50 -12 2 12 7.43 1.26 -12 2 12 7.46 1.20 12 -2 -12 9.01 1.39 12 -2 -12 6.57 1.27 12 -2 -12 9.84 1.69 -10 2 10 32.00 2.25 -10 2 10 33.28 2.27 10 -2 -10 31.73 2.31 10 -2 -10 33.42 2.29 10 -2 -10 33.37 2.56 -8 2 8 2.94 0.75 -8 2 8 2.88 0.79 8 -2 -8 2.66 0.76 8 -2 -8 2.51 0.91 8 -2 -8 3.02 0.77 -6 2 6 42.75 2.45 -6 2 6 40.06 2.41 6 -2 -6 40.67 2.46 6 -2 -6 51.10 2.52 6 -2 -6 39.52 2.52 -4 2 4 481.18 24.51 -4 2 4 506.12 24.43 -4 2 4 502.57 24.52 4 -2 -4 508.94 24.52 4 -2 -4 501.42 24.48 4 -2 -4 481.85 24.51 -2 2 2 197.64 9.61 -2 2 2 196.55 9.61 2 -2 -2 186.24 9.60 2 -2 -2 194.52 9.61 0 2 0 583.08 30.17 0 -2 0 634.13 30.18 0 -2 0 625.75 30.19 2 2 -2 194.80 9.70 2 2 -2 185.68 9.70 2 2 -2 188.06 9.77 2 2 -2 205.19 9.93 2 2 -2 197.72 9.84 -2 -2 2 180.00 9.83 -2 -2 2 202.06 9.95 -2 -2 2 212.76 9.98 -2 -2 2 210.76 9.79 -2 -2 2 194.90 9.83 4 2 -4 476.36 24.28 4 2 -4 509.56 24.56 4 2 -4 478.75 24.43 4 2 -4 470.24 24.29 4 2 -4 508.22 24.30 -4 -2 4 480.21 24.27 -4 -2 4 534.86 24.58 -4 -2 4 495.75 24.27 -4 -2 4 490.63 24.29 6 2 -6 36.18 3.02 6 2 -6 43.10 2.44 6 2 -6 44.17 2.47 -6 -2 6 45.15 2.40 -6 -2 6 51.69 3.08 -6 -2 6 44.64 2.40 -6 -2 6 47.30 2.39 8 2 -8 1.81 0.62 8 2 -8 2.74 0.67 8 2 -8 0.95 1.19 -8 -2 8 2.12 0.47 -8 -2 8 2.17 1.24 -8 -2 8 1.39 0.50 -8 -2 8 2.49 0.98 -8 -2 8 2.26 0.56 10 2 -10 32.45 2.28 10 2 -10 33.58 3.15 10 2 -10 33.98 1.79 10 2 -10 32.21 2.22 -10 -2 10 34.97 2.12 -10 -2 10 34.75 1.97 -10 -2 10 30.27 2.65 -10 -2 10 34.35 2.94 -10 -2 10 35.01 2.09 12 2 -12 6.01 1.22 12 2 -12 7.37 1.20 12 2 -12 6.10 1.94 -12 -2 12 6.54 0.76 -12 -2 12 7.39 1.02 -12 -2 12 6.33 0.93 -12 -2 12 7.18 1.52 14 2 -14 21.60 2.85 14 2 -14 35.91 2.64 14 2 -14 25.45 3.47 14 2 -14 34.61 2.64 -14 -2 14 32.10 3.08 -14 -2 14 26.07 2.19 -14 -2 14 31.11 2.29 16 2 -16 1.07 1.47 16 2 -16 -3.11 2.52 16 2 -16 3.69 1.50 16 2 -16 3.42 2.02 -16 -2 16 1.49 1.06 -16 -2 16 0.22 1.87 -16 -2 16 1.59 1.16 18 2 -18 21.11 3.18 -18 -2 18 12.28 2.84 -17 3 17 3.47 1.76 -17 3 17 0.85 1.85 -17 3 17 2.51 1.79 17 -3 -17 4.98 1.92 17 -3 -17 2.69 1.89 -15 3 15 -0.70 1.46 -15 3 15 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105.00 5.61 -3 -3 3 110.25 5.70 -3 -3 3 111.40 5.39 -3 -3 3 101.72 5.43 -3 -3 3 105.90 5.49 5 3 -5 -0.96 0.99 5 3 -5 0.34 0.39 5 3 -5 0.21 0.37 5 3 -5 0.87 0.37 -5 -3 5 1.55 1.30 -5 -3 5 -0.59 0.98 -5 -3 5 -0.06 0.71 -5 -3 5 1.20 0.26 -5 -3 5 0.88 0.28 7 3 -7 111.24 6.46 7 3 -7 117.46 6.23 7 3 -7 114.23 5.96 7 3 -7 121.34 5.97 -7 -3 7 122.57 6.22 -7 -3 7 115.11 5.88 -7 -3 7 114.11 5.88 -7 -3 7 117.17 6.47 9 3 -9 25.28 1.89 9 3 -9 29.52 2.91 9 3 -9 25.08 2.28 9 3 -9 30.32 1.94 -9 -3 9 36.25 2.81 -9 -3 9 28.29 1.75 -9 -3 9 28.15 1.74 -9 -3 9 29.12 2.29 11 3 -11 5.80 1.09 11 3 -11 7.78 0.84 11 3 -11 10.78 2.17 11 3 -11 7.11 1.10 11 3 -11 9.76 1.70 -11 -3 11 8.76 0.93 -11 -3 11 8.95 0.93 -11 -3 11 9.01 1.55 -11 -3 11 12.42 2.11 13 3 -13 4.78 1.64 13 3 -13 6.80 1.25 13 3 -13 6.30 2.15 13 3 -13 4.65 1.26 -13 -3 13 7.81 0.97 -13 -3 13 5.23 1.63 -13 -3 13 5.66 0.95 15 3 -15 -2.65 1.24 15 3 -15 -1.48 1.17 15 3 -15 0.10 2.53 15 3 -15 0.20 1.75 -15 -3 15 0.39 1.76 -15 -3 15 -0.44 0.84 -15 -3 15 -0.81 0.90 -15 -3 15 -4.04 3.36 17 3 -17 8.99 2.44 17 3 -17 2.40 1.70 17 3 -17 3.79 1.72 -17 -3 17 3.43 1.10 -17 -3 17 4.63 2.55 -17 -3 17 3.73 1.18 -17 -3 17 -2.72 4.46 -17 -3 17 8.92 2.52 -16 4 16 2.24 1.78 -16 4 16 4.17 1.63 -16 4 16 1.62 1.58 16 -4 -16 3.66 1.69 16 -4 -16 -1.39 1.63 -14 4 14 98.99 5.87 -14 4 14 95.85 5.77 -14 4 14 105.64 5.88 14 -4 -14 94.53 5.90 14 -4 -14 110.82 5.94 -12 4 12 0.04 1.04 -12 4 12 0.91 1.00 12 -4 -12 1.64 1.10 -10 4 10 104.15 5.81 -10 4 10 107.59 5.77 10 -4 -10 103.65 5.77 10 -4 -10 108.98 5.70 10 -4 -10 108.26 5.78 -8 4 8 58.76 3.10 -8 4 8 47.95 2.99 -8 4 8 49.02 2.69 8 -4 -8 55.14 3.02 8 -4 -8 48.17 2.97 8 -4 -8 48.34 2.84 -6 4 6 6.34 0.84 -6 4 6 6.43 0.88 6 -4 -6 5.77 0.87 6 -4 -6 6.19 0.85 -4 4 4 1.30 0.53 -4 4 4 0.94 0.50 4 -4 -4 1.54 0.52 -2 4 2 41.35 2.23 -2 4 2 41.43 2.24 2 -4 -2 41.13 2.20 2 -4 -2 42.03 2.17 2 -4 -2 39.57 2.20 0 4 0 111.65 5.52 0 4 0 108.15 5.46 0 4 0 109.89 5.46 0 4 0 104.33 5.58 0 -4 0 105.00 5.41 0 -4 0 107.28 5.41 0 -4 0 114.45 5.61 0 -4 0 115.89 5.65 0 -4 0 109.17 5.64 2 4 -2 36.96 2.43 2 4 -2 39.53 2.01 2 4 -2 40.43 2.26 2 4 -2 37.84 2.35 2 4 -2 38.24 2.20 2 4 -2 38.72 2.23 2 4 -2 36.19 2.38 2 4 -2 42.04 2.59 2 4 -2 39.23 2.01 -2 -4 2 41.19 2.27 -2 -4 2 41.31 2.54 -2 -4 2 41.24 2.55 -2 -4 2 40.69 2.34 -2 -4 2 38.25 2.35 4 4 -4 2.07 0.34 4 4 -4 1.07 0.71 4 4 -4 0.67 0.75 4 4 -4 1.87 0.56 4 4 -4 1.77 0.33 -4 -4 4 1.02 1.05 -4 -4 4 2.01 1.17 -4 -4 4 2.44 0.62 6 4 -6 5.23 1.09 6 4 -6 4.46 0.58 6 4 -6 4.78 1.55 6 4 -6 4.24 0.65 6 4 -6 3.84 0.56 -6 -4 6 3.19 1.46 -6 -4 6 5.67 0.44 -6 -4 6 4.34 1.03 -6 -4 6 4.41 0.44 -6 -4 6 7.05 1.78 8 4 -8 48.76 2.71 8 4 -8 52.13 2.73 8 4 -8 44.39 3.15 8 4 -8 47.55 3.47 -8 -4 8 47.12 3.14 -8 -4 8 48.12 3.58 -8 -4 8 48.87 2.98 -8 -4 8 45.47 3.83 -8 -4 8 49.74 2.53 -8 -4 8 46.48 2.53 10 4 -10 110.47 5.73 10 4 -10 109.17 6.56 10 4 -10 109.78 5.75 -10 -4 10 107.80 6.98 -10 -4 10 123.55 6.19 -10 -4 10 104.11 5.52 -10 -4 10 104.84 5.53 -10 -4 10 106.21 6.51 -10 -4 10 103.40 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26.23 1.54 6 8 -10 25.80 2.22 6 8 -10 20.43 2.73 -6 -8 10 23.03 3.62 8 8 -12 5.99 0.76 8 8 -12 4.36 1.16 8 8 -12 5.26 0.79 -8 -8 12 4.60 1.66 -8 -8 12 1.61 2.64 -8 -8 12 3.88 1.56 10 8 -14 37.18 2.70 10 8 -14 30.70 3.66 10 8 -14 32.13 4.46 10 8 -14 36.59 2.39 10 8 -14 35.95 2.41 10 8 -14 35.87 3.31 -10 -8 14 34.59 3.38 -10 -8 14 32.19 5.08 -10 -8 14 35.57 3.37 12 8 -16 43.40 3.03 12 8 -16 42.33 3.03 12 8 -16 41.47 5.08 12 8 -16 40.07 3.98 12 8 -16 44.65 3.00 12 8 -16 40.43 4.19 -12 -8 16 47.79 4.37 -12 -8 16 40.71 4.05 -12 -8 16 40.37 6.00 -15 9 11 52.52 3.87 -15 9 11 52.17 3.98 15 -9 -11 52.21 3.94 15 -9 -11 46.62 3.89 -13 9 9 6.39 1.53 -13 9 9 9.60 1.77 13 -9 -9 11.18 1.63 13 -9 -9 10.43 2.53 -11 9 7 35.15 2.91 -11 9 7 42.77 3.10 -11 9 7 40.86 2.87 11 -9 -7 37.63 2.81 11 -9 -7 42.07 2.81 -9 9 5 9.38 1.28 -9 9 5 11.62 1.45 -9 9 5 10.94 1.37 9 -9 -5 10.84 1.19 9 -9 -5 7.98 1.12 9 -9 -5 11.86 1.29 -7 9 3 1.08 0.95 -7 9 3 1.28 0.85 -7 9 3 0.67 0.81 7 -9 -3 1.32 1.19 7 -9 -3 0.66 0.60 7 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-5.57 1.86 6 -2 15 -0.21 0.90 6 -2 15 0.48 0.98 -4 2 -17 2.40 1.51 -4 2 -17 4.10 3.57 -4 2 -17 2.36 1.74 4 -2 17 1.84 0.77 4 -2 17 7.02 2.33 4 -2 17 3.95 2.30 4 -2 17 3.79 0.84 -13 3 -8 3.26 1.93 -13 3 -8 5.70 1.72 -13 3 -8 1.91 1.92 13 -3 8 4.93 2.24 13 -3 8 1.50 1.41 13 -3 8 6.54 1.48 13 -3 8 3.11 1.42 -11 3 -10 3.42 1.68 -11 3 -10 5.88 1.81 -11 3 -10 6.19 2.09 11 -3 10 5.71 1.31 11 -3 10 3.76 1.22 11 -3 10 0.48 1.97 11 -3 10 3.07 1.29 11 -3 10 3.11 2.03 -9 3 -12 2.90 3.36 -9 3 -12 0.15 1.89 -9 3 -12 0.08 1.44 -9 3 -12 1.33 1.48 9 -3 12 -1.13 2.04 9 -3 12 0.07 1.99 9 -3 12 0.18 0.95 9 -3 12 -1.13 1.03 -7 3 -14 7.94 3.64 -7 3 -14 6.35 1.68 -7 3 -14 7.49 1.78 7 -3 14 7.34 1.00 7 -3 14 8.63 1.06 7 -3 14 4.14 2.20 7 -3 14 7.23 2.29 -5 3 -16 4.41 0.90 -5 3 -16 2.64 1.64 -5 3 -16 6.27 1.71 -5 3 -16 7.27 3.62 5 -3 16 4.93 0.53 5 -3 16 -0.95 2.22 5 -3 16 5.92 2.13 5 -3 16 6.17 0.62 -3 3 -18 3.95 1.63 -3 3 -18 2.61 2.37 -3 3 -18 1.15 3.61 -3 3 -18 1.44 1.24 -3 3 -18 0.73 1.68 3 -3 18 2.03 2.09 -14 4 -7 2.30 2.14 -14 4 -7 -2.70 1.67 14 -4 7 1.01 1.60 14 -4 7 3.05 1.49 14 -4 7 3.14 1.95 14 -4 7 1.87 1.44 -12 4 -9 2.97 0.56 -12 4 -9 4.04 2.14 -12 4 -9 2.77 1.77 -12 4 -9 3.52 0.61 -12 4 -9 1.81 1.86 12 -4 9 4.85 1.99 12 -4 9 3.60 1.47 12 -4 9 2.56 1.23 12 -4 9 3.99 1.19 -10 4 -11 -3.16 1.93 -10 4 -11 -1.85 1.56 10 -4 11 0.72 0.95 10 -4 11 0.68 0.91 10 -4 11 1.67 1.98 10 -4 11 -0.92 1.92 10 -4 11 0.73 1.18 -8 4 -13 -0.98 2.15 -8 4 -13 2.57 1.54 -8 4 -13 -2.75 1.39 -8 4 -13 6.85 3.45 8 -4 13 0.74 0.68 8 -4 13 -3.80 2.03 8 -4 13 -1.26 1.95 8 -4 13 -0.30 0.60 -6 4 -15 1.07 1.52 -6 4 -15 3.16 3.64 -6 4 -15 0.02 1.41 6 -4 15 -1.18 1.99 6 -4 15 1.46 2.29 -4 4 -17 11.04 1.34 -4 4 -17 10.46 1.87 -4 4 -17 13.51 4.03 -4 4 -17 10.75 1.92 4 -4 17 9.11 2.50 4 -4 17 10.28 2.67 -13 5 -8 8.54 2.48 -13 5 -8 8.47 2.05 13 -5 8 5.03 1.17 -11 5 -10 16.65 2.22 -11 5 -10 15.98 2.24 -11 5 -10 15.02 2.66 -11 5 -10 14.29 1.45 11 -5 10 17.26 1.57 11 -5 10 15.17 1.38 11 -5 10 13.98 1.86 11 -5 10 14.03 2.29 -9 5 -12 1.19 3.68 -9 5 -12 2.70 2.25 -9 5 -12 5.20 1.64 9 -5 12 3.15 2.35 9 -5 12 -0.63 1.94 -7 5 -14 -1.39 1.45 -7 5 -14 0.25 2.25 -7 5 -14 -2.03 1.48 -7 5 -14 3.98 3.89 7 -5 14 3.21 2.39 7 -5 14 -4.76 1.84 -5 5 -16 6.19 3.87 -5 5 -16 5.35 1.76 -5 5 -16 7.18 1.70 5 -5 16 3.47 2.06 5 -5 16 3.37 2.22 -10 6 -11 7.84 1.73 -10 6 -11 1.66 2.34 -10 6 -11 3.53 1.71 -10 6 -11 5.00 1.18 10 -6 11 2.11 1.50 -8 6 -13 7.45 3.94 -8 6 -13 4.29 1.69 -8 6 -13 4.56 1.76 -8 6 -13 3.59 2.49 -8 6 -13 1.88 1.48 8 -6 13 4.43 1.96 8 -6 13 1.70 2.43 -10 -4 -12 5.55 2.24 10 4 12 2.35 1.76 10 4 12 3.80 2.12 8 4 14 16.56 2.79 -11 -3 -11 4.61 2.44 -11 -3 -11 1.09 2.20 11 3 11 -0.64 2.01 11 3 11 2.97 1.90 11 3 11 2.68 1.79 -9 -3 -13 9.28 1.99 -9 -3 -13 2.37 1.86 -9 -3 -13 11.50 2.70 9 3 13 8.17 1.86 9 3 13 7.96 2.43 9 3 13 12.12 2.04 -7 -3 -15 6.83 1.13 -7 -3 -15 10.00 2.79 -7 -3 -15 6.13 1.86 7 3 15 6.46 2.53 7 3 15 6.18 1.78 7 3 15 10.24 2.04 -12 -2 -10 4.60 2.48 12 2 10 14.39 2.15 12 2 10 13.75 2.36 12 2 10 15.61 2.14 -10 -2 -12 4.52 1.72 -10 -2 -12 0.50 1.82 10 2 12 2.19 2.05 10 2 12 3.59 1.73 10 2 12 4.58 1.66 -8 -2 -14 14.33 2.14 -8 -2 -14 12.46 2.18 8 2 14 14.12 2.02 8 2 14 13.56 2.03 8 2 14 13.05 2.70 -6 -2 -16 1.10 1.79 -6 -2 -16 -0.67 1.74 -6 -2 -16 0.15 0.93 6 2 16 1.71 1.57 6 2 16 3.16 1.53 6 2 16 0.37 2.31 -13 -1 -9 1.62 1.63 -13 -1 -9 2.32 2.36 13 1 9 3.32 2.00 13 1 9 2.63 0.91 13 1 9 2.51 1.76 13 1 9 6.46 1.90 -11 -1 -11 15.33 3.35 -11 -1 -11 11.08 2.12 11 1 11 13.62 2.01 11 1 11 10.72 2.00 11 1 11 18.90 2.55 -9 -1 -13 10.10 3.13 -9 -1 -13 10.36 2.05 -9 -1 -13 6.33 1.98 9 1 13 8.01 1.69 9 1 13 8.95 1.79 9 1 13 4.81 2.22 -7 -1 -15 0.66 1.76 -7 -1 -15 5.90 2.94 -7 -1 -15 -1.32 1.73 7 1 15 6.24 2.40 7 1 15 2.51 1.42 7 1 15 2.13 1.52 -5 -1 -17 6.01 2.02 -5 -1 -17 2.89 3.14 -5 -1 -17 3.63 1.88 5 1 17 3.11 1.49 5 1 17 8.13 1.64 5 1 17 4.67 2.14 -12 0 -10 6.63 1.88 -12 0 -10 2.74 1.83 12 0 10 7.09 1.83 12 0 10 5.24 0.96 12 0 10 7.27 1.73 12 0 10 5.81 2.07 -10 0 -12 9.17 3.22 -10 0 -12 0.85 1.71 -10 0 -12 1.96 1.74 10 0 12 1.92 1.49 10 0 12 0.51 1.34 10 0 12 -1.81 2.04 -8 0 -14 108.14 6.52 -8 0 -14 104.75 7.84 -8 0 -14 115.19 6.61 8 0 14 108.21 6.12 8 0 14 97.93 6.94 -6 0 -16 60.22 6.27 -6 0 -16 60.13 4.53 -6 0 -16 66.14 4.55 6 0 16 60.67 4.03 -13 1 -9 3.60 1.97 -13 1 -9 3.52 1.78 -13 1 -9 4.36 2.19 -13 1 -9 2.40 1.21 13 -1 9 1.33 1.63 13 -1 9 0.91 1.71 13 -1 9 2.41 2.11 13 -1 9 3.66 1.17 -11 1 -11 13.92 2.19 11 -1 11 14.78 1.49 11 -1 11 11.75 2.39 11 -1 11 15.72 1.91 11 -1 11 13.78 1.88 -9 1 -13 12.73 3.51 -9 1 -13 5.72 1.79 -9 1 -13 5.02 1.84 9 -1 13 7.54 1.55 9 -1 13 5.61 2.28 -7 1 -15 2.33 1.75 -7 1 -15 4.91 1.85 -7 1 -15 11.67 3.36 7 -1 15 1.19 1.23 7 -1 15 1.73 2.37 7 -1 15 2.37 1.22 -5 1 -17 6.37 1.93 -5 1 -17 8.74 2.07 -5 1 -17 7.16 3.50 5 -1 17 7.14 1.22 5 -1 17 5.05 2.30 5 -1 17 6.47 2.50 5 -1 17 7.60 1.27 -12 2 -10 13.34 2.43 -12 2 -10 14.57 2.28 -12 2 -10 12.54 2.28 12 -2 10 14.18 1.81 12 -2 10 14.72 1.57 12 -2 10 14.43 2.51 12 -2 10 14.39 1.93 12 -2 10 17.93 2.63 -10 2 -12 4.62 3.47 -10 2 -12 8.14 1.89 -10 2 -12 3.50 1.81 10 -2 12 4.92 1.67 10 -2 12 3.20 1.34 10 -2 12 -0.78 2.04 10 -2 12 2.49 2.17 -8 2 -14 11.63 2.19 -8 2 -14 17.30 4.17 -8 2 -14 13.03 2.14 8 -2 14 12.14 2.60 8 -2 14 11.95 2.61 8 -2 14 14.62 1.58 8 -2 14 18.69 2.03 -6 2 -16 0.83 1.77 -6 2 -16 3.00 3.40 -6 2 -16 -1.89 1.63 6 -2 16 1.67 2.26 6 -2 16 -0.42 0.94 6 -2 16 1.69 0.85 6 -2 16 3.02 2.24 -11 3 -11 0.85 1.82 -11 3 -11 7.11 1.89 -11 3 -11 1.51 2.05 11 -3 11 2.17 1.10 11 -3 11 0.93 1.20 11 -3 11 1.47 1.89 11 -3 11 2.96 2.30 11 -3 11 1.69 1.21 -9 3 -13 11.87 3.86 -9 3 -13 11.25 2.05 -9 3 -13 12.41 2.03 -9 3 -13 8.02 2.59 9 -3 13 10.44 1.28 9 -3 13 10.28 2.66 9 -3 13 11.62 1.33 9 -3 13 7.47 2.32 -7 3 -15 12.70 3.88 -7 3 -15 10.80 1.99 -7 3 -15 5.23 1.92 7 -3 15 9.39 1.04 7 -3 15 9.51 2.19 7 -3 15 1.29 2.37 7 -3 15 10.93 1.16 -10 4 -12 11.08 3.87 -10 4 -12 2.70 1.75 -10 4 -12 0.60 2.21 10 -4 12 3.62 0.92 10 -4 12 2.97 2.38 -8 4 -14 14.61 3.06 8 -4 14 19.98 2.94 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 12964 _shelx_res_file ; TITL mo_10set21a_JC1_186ca in C2/c shelx.res created by SHELXL-2018/3 at 15:02:10 on 04-Mar-2024 CELL 0.71073 15.6124 12.7649 17.1797 90.000 116.243 90.000 ZERR 8.00 0.0024 0.0017 0.0035 0.000 0.005 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H LI N O SI UNIT 112 176 4 12 8 8 MERG 2 OMIT 0.00 55.00 OMIT 0 0 2 OMIT -2 2 6 OMIT 0 6 2 DFIX 0.950 0.020 C1 H1A DFIX 0.950 0.020 C6 H6A DFIX 0.950 0.020 C6 H6B DFIX 0.950 0.020 C7 H7B DFIX 0.950 0.020 C11 H11 DFIX 0.950 0.020 C15 H15 DFIX 0.950 0.020 C14 H14 MPLA 5 N2 C4 C7 O8 C9 FREE SI LI FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 TEMP -173.15 WGHT 0.046100 1.664500 FVAR 0.14744 LI 3 0.500000 0.452375 0.250000 10.50000 0.01694 0.01934 = 0.01972 0.00000 0.00327 0.00000 SI 6 0.570498 0.242463 0.212031 11.00000 0.01801 0.01873 = 0.01628 -0.00047 0.00498 0.00254 N1 4 0.500000 0.300275 0.250000 10.50000 0.01875 0.01686 = 0.01714 0.00000 0.00614 0.00000 N2 4 0.379954 0.540705 0.163852 11.00000 0.01580 0.02108 = 0.01619 0.00247 0.00282 -0.00055 O8 5 0.284900 0.677525 0.094336 11.00000 0.02832 0.03001 = 0.01900 0.00558 0.00348 0.01245 C1 1 0.505258 0.152883 0.116382 11.00000 0.03222 0.02608 = 0.02210 -0.00476 0.00792 0.00300 C2 1 0.669914 0.158622 0.292663 11.00000 0.02603 0.02961 = 0.03020 0.00166 0.00401 0.00920 C3 1 0.629475 0.342860 0.171465 11.00000 0.02429 0.03254 = 0.02844 -0.00008 0.01458 0.00028 C4 1 0.316612 0.501690 0.074056 11.00000 0.02070 0.02360 = 0.01705 0.00298 -0.00069 -0.00130 C5 1 0.373817 0.447807 0.034103 11.00000 0.03798 0.03907 = 0.02424 -0.00973 -0.00069 0.01017 C6 1 0.242479 0.429998 0.080626 11.00000 0.04192 0.05971 = 0.03164 0.01093 -0.00638 -0.03065 C7 1 0.270669 0.603314 0.025890 11.00000 0.03224 0.03140 = 0.01964 0.00330 0.00339 0.00883 C9 1 0.353501 0.634263 0.167904 11.00000 0.01434 0.02381 = 0.01830 0.00611 0.00573 0.00299 C10 1 0.389160 0.703705 0.243995 11.00000 0.01675 0.02340 = 0.02078 0.00284 0.00965 0.00432 C11 1 0.382589 0.812221 0.232587 11.00000 0.02706 0.02503 = 0.02464 0.00621 0.01160 0.00716 C12 1 0.418666 0.878067 0.303689 11.00000 0.03884 0.02204 = 0.03454 0.00100 0.01764 0.00562 C13 1 0.461393 0.836967 0.386670 11.00000 0.03514 0.03250 = 0.02766 -0.00654 0.01590 0.00268 C14 1 0.466644 0.728874 0.398807 11.00000 0.03221 0.03356 = 0.02040 0.00238 0.01370 0.00696 C15 1 0.430345 0.662441 0.327822 11.00000 0.02344 0.02403 = 0.02193 0.00451 0.01162 0.00615 H1A 2 0.456393 0.190148 0.068089 11.00000 0.04025 H1B 2 0.549744 0.122294 0.095227 11.00000 0.04859 H1C 2 0.475040 0.093157 0.131247 11.00000 0.04130 H2A 2 0.646673 0.098871 0.314689 11.00000 0.04635 H2B 2 0.713372 0.198494 0.341032 11.00000 0.06438 H2C 2 0.705203 0.123336 0.266603 11.00000 0.05353 H3A 2 0.670567 0.308296 0.148918 11.00000 0.05089 H3B 2 0.582624 0.387325 0.123219 11.00000 0.04764 H3C 2 0.670229 0.394312 0.217579 11.00000 0.05153 H5A 2 0.423971 0.494831 0.033430 11.00000 0.04915 H5B 2 0.331405 0.428653 -0.025360 11.00000 0.05429 H5C 2 0.404990 0.385475 0.068215 11.00000 0.05764 H6A 2 0.202045 0.403990 0.022331 11.00000 0.06444 H6B 2 0.273626 0.369572 0.112190 11.00000 0.05976 H6C 2 0.204248 0.464976 0.110304 11.00000 0.10082 H7A 2 0.302117 0.631933 -0.011267 11.00000 0.04150 H7B 2 0.203311 0.596955 -0.009036 11.00000 0.04145 H11 2 0.355186 0.839876 0.175738 11.00000 0.03258 H12 2 0.413130 0.951730 0.295438 11.00000 0.03779 H13 2 0.489109 0.882143 0.436920 11.00000 0.03999 H14 2 0.494924 0.700375 0.456643 11.00000 0.02993 H15 2 0.432078 0.588583 0.336009 11.00000 0.02570 HKLF 4 REM mo_10set21a_JC1_186ca in C2/c REM wR2 = 0.0915, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0352 for 2888 Fo > 4sig(Fo) and 0.0492 for all 3522 data REM 252 parameters refined using 7 restraints END WGHT 0.0461 1.6647 REM Highest difference peak 0.294, deepest hole -0.235, 1-sigma level 0.043 Q1 1 0.6034 0.2978 0.1938 11.00000 0.05 0.29 Q2 1 0.3750 0.6691 0.2098 11.00000 0.05 0.27 Q3 1 0.6304 0.1966 0.2603 11.00000 0.05 0.26 Q4 1 0.4119 0.6843 0.2834 11.00000 0.05 0.26 Q5 1 0.3735 0.7549 0.2365 11.00000 0.05 0.25 Q6 1 0.2967 0.5482 0.0450 11.00000 0.05 0.24 Q7 1 0.2741 0.3755 0.0724 11.00000 0.05 0.23 Q8 1 0.5372 0.1879 0.1642 11.00000 0.05 0.22 Q9 1 0.3568 0.5178 0.1256 11.00000 0.05 0.21 Q10 1 0.4120 0.5038 0.2009 11.00000 0.05 0.21 Q11 1 0.3887 0.8352 0.2743 11.00000 0.05 0.20 Q12 1 0.4559 0.8495 0.3385 11.00000 0.05 0.19 Q13 1 0.5000 0.3516 0.2500 10.50000 0.05 0.19 Q14 1 0.4435 0.7855 0.3869 11.00000 0.05 0.18 Q15 1 0.5239 0.2599 0.2389 11.00000 0.05 0.18 Q16 1 0.3532 0.5741 0.1685 11.00000 0.05 0.18 Q17 1 0.2836 0.4713 0.0785 11.00000 0.05 0.17 Q18 1 0.4412 0.6973 0.3596 11.00000 0.05 0.16 Q19 1 0.3477 0.4727 0.0559 11.00000 0.05 0.16 Q20 1 0.6816 0.1559 0.3557 11.00000 0.05 0.15 ; _shelx_res_checksum 9287 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Li Li 0.500000 0.4524(2) 0.250000 0.0204(6) Uani d 1 . . Si Si 0.57050(2) 0.24246(3) 0.21203(2) 0.01863(10) Uani d 1 . . N N1 0.500000 0.30027(11) 0.250000 0.0182(3) Uani d 1 . . N N2 0.37995(7) 0.54071(8) 0.16385(7) 0.0192(2) Uani d 1 . . O O8 0.28490(7) 0.67752(8) 0.09434(6) 0.0283(2) Uani d 1 . . C C1 0.50526(11) 0.15288(11) 0.11638(9) 0.0283(3) Uani d 1 . . C C2 0.66991(11) 0.15862(12) 0.29266(10) 0.0317(3) Uani d 1 . . C C3 0.62947(10) 0.34286(12) 0.17146(10) 0.0274(3) Uani d 1 . . C C4 0.31661(9) 0.50169(10) 0.07406(8) 0.0238(3) Uani d 1 . . C C5 0.37382(13) 0.44781(14) 0.03410(10) 0.0391(4) Uani d 1 . . C C6 0.24248(14) 0.43000(18) 0.08063(12) 0.0527(6) Uani d 1 . . C C7 0.27067(11) 0.60331(12) 0.02589(9) 0.0307(3) Uani d 1 . . C C9 0.35350(8) 0.63426(10) 0.16790(8) 0.0194(3) Uani d 1 . . C C10 0.38916(9) 0.70370(10) 0.24400(8) 0.0198(3) Uani d 1 . . C C11 0.38259(10) 0.81222(10) 0.23259(9) 0.0255(3) Uani d 1 . . C C12 0.41867(11) 0.87807(11) 0.30369(10) 0.0313(3) Uani d 1 . . C C13 0.46139(11) 0.83697(12) 0.38667(10) 0.0310(3) Uani d 1 . . C C14 0.46664(10) 0.72887(11) 0.39881(9) 0.0280(3) Uani d 1 . . C C15 0.43035(9) 0.66244(11) 0.32782(8) 0.0226(3) Uani d 1 . . H H1A 0.4564(12) 0.1901(13) 0.0681(10) 0.040(5) Uiso d 1 . . H H1B 0.5497(14) 0.1223(15) 0.0952(12) 0.049(5) Uiso d 1 . . H H1C 0.4750(13) 0.0932(15) 0.1312(12) 0.041(5) Uiso d 1 . . H H2A 0.6467(14) 0.0989(15) 0.3147(12) 0.046(5) Uiso d 1 . . H H2B 0.7134(16) 0.1985(18) 0.3410(15) 0.064(6) Uiso d 1 . . H H2C 0.7052(15) 0.1233(16) 0.2666(13) 0.054(6) Uiso d 1 . . H H3A 0.6706(14) 0.3083(15) 0.1489(12) 0.051(5) Uiso d 1 . . H H3B 0.5826(14) 0.3873(15) 0.1232(13) 0.048(5) Uiso d 1 . . H H3C 0.6702(15) 0.3943(16) 0.2176(13) 0.052(5) Uiso d 1 . . H H5A 0.4240(14) 0.4948(15) 0.0334(12) 0.049(5) Uiso d 1 . . H H5B 0.3314(14) 0.4287(16) -0.0254(14) 0.054(6) Uiso d 1 . . H H5C 0.4050(15) 0.3855(17) 0.0682(14) 0.058(6) Uiso d 1 . . H H6A 0.2020(15) 0.4040(16) 0.0223(11) 0.064(6) Uiso d 1 . . H H6B 0.2736(14) 0.3696(14) 0.1122(13) 0.060(6) Uiso d 1 . . H H6C 0.204(2) 0.465(2) 0.110(2) 0.101(10) Uiso d 1 . . H H7A 0.3021(13) 0.6319(14) -0.0113(12) 0.041(5) Uiso d 1 . . H H7B 0.2033(10) 0.5970(14) -0.0090(11) 0.041(5) Uiso d 1 . . H H11 0.3552(12) 0.8399(12) 0.1757(9) 0.033(4) Uiso d 1 . . H H12 0.4131(12) 0.9517(14) 0.2954(11) 0.038(5) Uiso d 1 . . H H13 0.4891(13) 0.8821(14) 0.4369(12) 0.040(5) Uiso d 1 . . H H14 0.4949(11) 0.7004(12) 0.4566(9) 0.030(4) Uiso d 1 . . H H15 0.4321(11) 0.5886(10) 0.3360(10) 0.026(4) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Li 0.0169(14) 0.0193(14) 0.0197(14) 0.000 0.0033(11) 0.000 Si 0.01801(18) 0.01873(17) 0.01628(17) 0.00254(12) 0.00498(13) -0.00047(12) N1 0.0188(7) 0.0169(7) 0.0171(7) 0.000 0.0061(6) 0.000 N2 0.0158(5) 0.0211(5) 0.0162(5) -0.0006(4) 0.0028(4) 0.0025(4) O8 0.0283(5) 0.0300(5) 0.0190(4) 0.0125(4) 0.0035(4) 0.0056(4) C1 0.0322(8) 0.0261(7) 0.0221(7) 0.0030(6) 0.0079(6) -0.0048(5) C2 0.0260(7) 0.0296(7) 0.0302(8) 0.0092(6) 0.0040(6) 0.0017(6) C3 0.0243(7) 0.0325(7) 0.0284(7) 0.0003(6) 0.0146(6) -0.0001(6) C4 0.0207(6) 0.0236(6) 0.0170(6) -0.0013(5) -0.0007(5) 0.0030(5) C5 0.0380(9) 0.0391(9) 0.0242(7) 0.0102(7) -0.0007(7) -0.0097(6) C6 0.0419(10) 0.0597(12) 0.0316(9) -0.0306(9) -0.0064(8) 0.0109(8) C7 0.0322(8) 0.0314(7) 0.0196(6) 0.0088(6) 0.0034(6) 0.0033(5) C9 0.0143(6) 0.0238(6) 0.0183(6) 0.0030(5) 0.0057(5) 0.0061(5) C10 0.0168(6) 0.0234(6) 0.0208(6) 0.0043(5) 0.0096(5) 0.0028(5) C11 0.0271(7) 0.0250(7) 0.0246(7) 0.0072(5) 0.0116(6) 0.0062(5) C12 0.0388(8) 0.0220(7) 0.0345(8) 0.0056(6) 0.0176(7) 0.0010(6) C13 0.0351(8) 0.0325(7) 0.0277(7) 0.0027(6) 0.0159(6) -0.0065(6) C14 0.0322(7) 0.0336(7) 0.0204(6) 0.0070(6) 0.0137(6) 0.0024(5) C15 0.0234(6) 0.0240(6) 0.0219(6) 0.0061(5) 0.0116(5) 0.0045(5) 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' Li Li -0.0003 0.0001 '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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Li N2 . . 122.02(7) ? N1 Li N2 . 2_655 122.02(7) ? N2 Li N2 . 2_655 115.95(14) ? N1 Li Si . 2_655 29.36(3) ? N2 Li Si . 2_655 108.77(5) ? N2 Li Si 2_655 2_655 127.05(6) ? N1 Si C3 . . 110.90(7) ? N1 Si C1 . . 114.23(6) ? C3 Si C1 . . 104.72(7) ? N1 Si C2 . . 115.55(6) ? C3 Si C2 . . 106.22(7) ? C1 Si C2 . . 104.31(7) ? Si N1 Si . 2_655 127.83(9) ? Si N1 Li . . 116.09(4) ? Si N1 Li 2_655 . 116.09(4) ? C9 N2 C4 . . 106.52(10) ? C9 N2 Li . . 131.72(11) ? C4 N2 Li . . 121.09(9) ? C9 O8 C7 . . 105.29(10) ? Si C1 H1A . . 111.5(11) ? Si C1 H1B . . 111.1(11) ? H1A C1 H1B . . 107.0(15) ? Si C1 H1C . . 112.2(10) ? H1A C1 H1C . . 108.4(15) ? H1B C1 H1C . . 106.4(15) ? Si C2 H2A . . 113.3(11) ? Si C2 H2B . . 111.9(13) ? H2A C2 H2B . . 108.5(17) ? Si C2 H2C . . 112.2(12) ? H2A C2 H2C . . 101.5(16) ? H2B C2 H2C . . 108.8(18) ? Si C3 H3A . . 110.5(11) ? Si C3 H3B . . 113.2(11) ? H3A C3 H3B . . 106.9(15) ? Si C3 H3C . . 113.2(11) ? H3A C3 H3C . . 107.8(16) ? H3B C3 H3C . . 104.9(15) ? N2 C4 C5 . . 111.37(11) ? N2 C4 C6 . . 107.51(12) ? C5 C4 C6 . . 112.48(16) ? N2 C4 C7 . . 102.23(10) ? C5 C4 C7 . . 111.64(12) ? C6 C4 C7 . . 111.07(14) ? C4 C5 H5A . . 111.0(11) ? C4 C5 H5B . . 109.1(12) ? H5A C5 H5B . . 108.4(16) ? C4 C5 H5C . . 109.6(12) ? H5A C5 H5C . . 108.2(16) ? H5B C5 H5C . . 110.6(16) ? C4 C6 H6A . . 107.3(13) ? C4 C6 H6B . . 108.6(13) ? H6A C6 H6B . . 104.3(17) ? C4 C6 H6C . . 113.5(16) ? H6A C6 H6C . . 113(2) ? H6B C6 H6C . . 109(2) ? O8 C7 C4 . . 104.34(10) ? O8 C7 H7A . . 109.1(10) ? C4 C7 H7A . . 113.4(10) ? O8 C7 H7B . . 107.2(11) ? C4 C7 H7B . . 112.9(11) ? H7A C7 H7B . . 109.6(15) ? N2 C9 O8 . . 118.04(11) ? N2 C9 C10 . . 127.49(11) ? O8 C9 C10 . . 114.47(11) ? C15 C10 C11 . . 119.42(12) ? C15 C10 C9 . . 120.72(11) ? C11 C10 C9 . . 119.86(11) ? C12 C11 C10 . . 120.24(13) ? C12 C11 H11 . . 120.5(10) ? C10 C11 H11 . . 119.2(10) ? C11 C12 C13 . . 120.21(13) ? C11 C12 H12 . . 119.8(11) ? C13 C12 H12 . . 120.0(11) ? C12 C13 C14 . . 120.00(14) ? C12 C13 H13 . . 121.0(11) ? C14 C13 H13 . . 118.9(11) ? C15 C14 C13 . . 120.07(13) ? C15 C14 H14 . . 120.0(10) ? C13 C14 H14 . . 119.9(10) ? C14 C15 C10 . . 120.03(12) ? C14 C15 H15 . . 120.2(9) ? C10 C15 H15 . . 119.8(9) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Li N1 . 1.942(3) ? Li N2 . 2.1263(18) ? Li N2 2_655 2.1264(18) ? Li Si 2_655 3.074(3) ? Si N1 . 1.6782(7) ? Si C3 . 1.8824(15) ? Si C1 . 1.8881(14) ? Si C2 . 1.8900(14) ? N2 C9 . 1.2756(16) ? N2 C4 . 1.5022(16) ? O8 C9 . 1.3610(15) ? O8 C7 . 1.4486(17) ? C1 H1A . 0.968(14) ? C1 H1B . 1.00(2) ? C1 H1C . 0.988(19) ? C2 H2A . 0.99(2) ? C2 H2B . 0.95(2) ? C2 H2C . 0.96(2) ? C3 H3A . 0.99(2) ? C3 H3B . 1.00(2) ? C3 H3C . 1.01(2) ? C4 C5 . 1.511(2) ? C4 C6 . 1.518(2) ? C4 C7 . 1.5353(18) ? C5 H5A . 0.99(2) ? C5 H5B . 0.97(2) ? C5 H5C . 0.98(2) ? C6 H6A . 0.976(15) ? C6 H6B . 0.945(15) ? C6 H6C . 1.04(3) ? C7 H7A . 1.029(19) ? C7 H7B . 0.956(14) ? C9 C10 . 1.4700(18) ? C10 C15 . 1.3950(18) ? C10 C11 . 1.3964(18) ? C11 C12 . 1.381(2) ? C11 H11 . 0.944(13) ? C12 C13 . 1.383(2) ? C12 H12 . 0.949(18) ? C13 C14 . 1.392(2) ? C13 H13 . 0.967(18) ? C14 C15 . 1.3843(19) ? C14 H14 . 0.963(13) ? C15 H15 . 0.952(13) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C3 Si N1 Si . . . 2_655 176.77(5) ? C1 Si N1 Si . . . 2_655 58.73(6) ? C2 Si N1 Si . . . 2_655 -62.30(6) ? C3 Si N1 Li . . . . -3.23(5) ? C1 Si N1 Li . . . . -121.27(6) ? C2 Si N1 Li . . . . 117.70(6) ? C9 N2 C4 C5 . . . . 133.79(13) ? Li N2 C4 C5 . . . . -37.89(15) ? C9 N2 C4 C6 . . . . -102.56(15) ? Li N2 C4 C6 . . . . 85.76(15) ? C9 N2 C4 C7 . . . . 14.45(14) ? Li N2 C4 C7 . . . . -157.23(10) ? C9 O8 C7 C4 . . . . 16.31(14) ? N2 C4 C7 O8 . . . . -18.50(14) ? C5 C4 C7 O8 . . . . -137.66(13) ? C6 C4 C7 O8 . . . . 95.91(15) ? C4 N2 C9 O8 . . . . -4.81(15) ? Li N2 C9 O8 . . . . 165.63(9) ? C4 N2 C9 C10 . . . . 175.66(12) ? Li N2 C9 C10 . . . . -13.9(2) ? C7 O8 C9 N2 . . . . -7.87(16) ? C7 O8 C9 C10 . . . . 171.71(11) ? N2 C9 C10 C15 . . . . -24.5(2) ? O8 C9 C10 C15 . . . . 155.95(12) ? N2 C9 C10 C11 . . . . 154.97(13) ? O8 C9 C10 C11 . . . . -24.56(17) ? C15 C10 C11 C12 . . . . 1.6(2) ? C9 C10 C11 C12 . . . . -177.93(13) ? C10 C11 C12 C13 . . . . -0.1(2) ? C11 C12 C13 C14 . . . . -1.1(2) ? C12 C13 C14 C15 . . . . 0.9(2) ? C13 C14 C15 C10 . . . . 0.5(2) ? C11 C10 C15 C14 . . . . -1.77(19) ? C9 C10 C15 C14 . . . . 177.72(12) ?