#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:28:56 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267144 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707508.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_7707508 loop_ _publ_author_name 'Dehmel, Maximilian' 'K\"ohler, Angelina' 'G\"orls, Helmar' 'Kretschmer, Robert' _publ_section_title ; Synthesis, characterization, and reactivity of group 13 hydride complexes based on amido-amine ligands. ; _journal_issue 24 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8434 _journal_page_last 8445 _journal_paper_doi 10.1039/d1dt01454d _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C38 H72 B2 Li2 N4' _chemical_formula_sum 'C38 H72 B2 Li2 N4' _chemical_formula_weight 620.49 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-04-21 deposited with the CCDC. 2021-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.242(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.4274(2) _cell_length_b 13.0691(4) _cell_length_c 18.8840(6) _cell_measurement_reflns_used 11484 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.626 _cell_measurement_theta_min 4.116 _cell_volume 2076.53(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measurement_device_type 'Xcalibur, AtlasS2, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 11484 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.958 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.626 _diffrn_reflns_theta_min 4.116 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_correction_T_min 0.944 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 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 0.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.266 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.146 _refine_diff_density_min -0.148 _refine_diff_density_rms 0.031 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 349 _refine_ls_number_reflns 4024 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0446 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.3258P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1053 _refine_ls_wR_factor_ref 0.1159 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3130 _reflns_number_total 4024 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01454d2.cif _cod_data_source_block FO7178_6a _cod_depositor_comments 'Adding full bibliography for 7707498--7707509.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7707508 _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 0.899 _shelx_estimated_absorpt_t_max 0.984 _shelx_res_file ; TITL rk1844_abs_a.res in P2(1)/n fo7178.res created by SHELXL-2018/3 at 16:51:32 on 20-Apr-2021 CELL 1.54184 8.4274 13.0691 18.8840 90 93.242 90 ZERR 2 0.0002 0.0004 0.0006 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B Li N UNIT 76 144 4 4 8 L.S. 10 0 0 PLAN 20 TEMP -150.16(12) BOND $H SIZE 0.266 0.045 0.040 REM COLOR:colourless fmap 2 acta WGHT 0.050400 0.325800 FVAR 0.41254 0.68010 B1 3 0.322337 0.438777 0.449716 11.00000 0.03213 0.04158 = 0.03629 0.00001 0.00304 -0.00598 H1B1 2 0.431074 0.404015 0.482464 11.00000 0.03772 H2B1 2 0.363448 0.472079 0.396654 11.00000 0.05044 H3B1 2 0.268201 0.500380 0.482781 11.00000 0.06513 H4B1 2 0.235471 0.375278 0.437321 11.00000 0.07236 LI1 4 0.584870 0.500573 0.431148 11.00000 0.03041 0.03573 = 0.03721 0.00039 0.00478 -0.00205 N1 5 0.688356 0.633375 0.383378 11.00000 0.02794 0.02653 = 0.03195 0.00128 0.00063 -0.00091 H1N1 2 0.746475 0.640254 0.424591 11.00000 0.04408 N2 5 0.751248 0.414652 0.375891 11.00000 0.02913 0.02576 = 0.04180 -0.00170 0.00232 -0.00113 C1 1 0.798936 0.591513 0.332784 11.00000 0.03139 0.03399 = 0.04579 0.00477 0.01286 -0.00093 H1A 2 0.737279 0.580943 0.285639 11.00000 0.04520 H1B 2 0.885578 0.640392 0.323741 11.00000 0.04052 C2 1 0.871278 0.492828 0.361193 11.00000 0.02552 0.03352 = 0.05082 -0.00156 0.00755 0.00022 H2A 2 0.947369 0.465491 0.327410 11.00000 0.04694 H2B 2 0.933159 0.506843 0.408495 11.00000 0.04871 C3 1 0.623641 0.732185 0.363743 11.00000 0.03288 0.02599 = 0.03205 0.00313 0.00282 0.00070 C4 1 0.696837 0.822109 0.390350 11.00000 0.05075 0.02949 = 0.03708 -0.00015 -0.00452 -0.00198 C5 1 0.625536 0.915379 0.372664 11.00000 0.07478 0.02733 = 0.05196 -0.00252 -0.00837 0.00372 H5 2 0.676079 0.977398 0.392719 11.00000 0.06546 C6 1 0.490045 0.921020 0.328816 11.00000 0.06882 0.03510 = 0.05919 0.00527 -0.00308 0.01627 H6 2 0.441740 0.989002 0.317024 11.00000 0.06250 C7 1 0.422308 0.832686 0.301342 11.00000 0.04014 0.04662 = 0.04905 0.00864 -0.00444 0.01080 H7 2 0.327049 0.836166 0.269221 11.00000 0.05144 C8 1 0.486350 0.736852 0.318483 11.00000 0.03055 0.03552 = 0.03613 0.00428 0.00339 0.00037 C9 1 0.850031 0.822995 0.437073 11.00000 0.06192 0.03165 = 0.04947 0.00170 -0.01597 -0.01057 H9 2 0.892739 0.754132 0.442068 11.00000 0.05224 C10 1 0.978798 0.885900 0.402903 11.00000 0.06644 0.07219 = 0.07547 0.01271 -0.02132 -0.02524 H10A 2 1.081369 0.879950 0.430477 11.00000 0.07481 H10B 2 0.941480 0.959778 0.401384 11.00000 0.10222 H10C 2 0.994408 0.859593 0.350903 11.00000 0.10262 C11 1 0.821540 0.860977 0.511371 11.00000 0.09332 0.07075 = 0.04904 -0.00493 -0.01990 -0.00573 H11A 2 0.922361 0.858940 0.541189 11.00000 0.08361 H11B 2 0.764553 0.931610 0.508327 11.00000 0.09632 H11C 2 0.736834 0.816118 0.534047 11.00000 0.09910 C12 1 0.402458 0.642034 0.289504 11.00000 0.02865 0.04383 = 0.04063 0.00726 -0.00162 -0.00526 H12 2 0.458867 0.582350 0.309473 11.00000 0.03215 C13 1 0.402069 0.636733 0.208630 11.00000 0.05600 0.06488 = 0.04354 -0.00030 -0.00386 -0.02091 H13A 2 0.345942 0.573297 0.191204 11.00000 0.06525 H13B 2 0.515240 0.635619 0.193526 11.00000 0.06189 H13C 2 0.340696 0.697700 0.186785 11.00000 0.07419 C14 1 0.232922 0.636486 0.314044 11.00000 0.02940 0.06865 = 0.06613 0.01973 -0.00015 -0.00332 H14A 2 0.232390 0.641185 0.368959 11.00000 0.06435 H14B 2 0.168504 0.692532 0.293790 11.00000 0.07817 H14C 2 0.179648 0.571606 0.297973 11.00000 0.07482 C15 1 0.682195 0.371242 0.308722 11.00000 0.04247 0.04891 = 0.04863 -0.01936 0.00618 -0.00349 AFIX 23 PART 1 H15A 2 0.768012 0.338600 0.283030 21.00000 -1.20000 H15B 2 0.637738 0.427638 0.278743 21.00000 -1.20000 PART 2 AFIX 23 H15C 2 0.766929 0.346512 0.278765 -21.00000 -1.20000 H15D 2 0.617913 0.423167 0.281866 -21.00000 -1.20000 AFIX 0 PART 1 C16 1 0.551921 0.292557 0.318966 21.00000 0.03660 0.04273 = 0.06768 -0.02307 -0.00295 -0.01116 AFIX 23 H16A 2 0.508630 0.266948 0.272461 21.00000 -1.20000 H16B 2 0.464138 0.323654 0.344236 21.00000 -1.20000 AFIX 0 C17 1 0.625844 0.207054 0.361645 21.00000 0.05035 0.03734 = 0.07894 -0.01381 0.01052 -0.00962 AFIX 23 H17A 2 0.705477 0.171682 0.333818 21.00000 -1.20000 H17B 2 0.543241 0.156790 0.373115 21.00000 -1.20000 AFIX 0 C18 1 0.706165 0.249449 0.430259 21.00000 0.05914 0.02383 = 0.06405 0.00612 0.00959 0.00817 AFIX 23 H18A 2 0.624366 0.278066 0.460254 21.00000 -1.20000 H18B 2 0.760865 0.193181 0.456898 21.00000 -1.20000 AFIX 0 C19 1 0.821889 0.329571 0.415299 21.00000 0.03405 0.03519 = 0.05467 -0.00980 -0.00235 0.00589 AFIX 23 H19A 2 0.871288 0.355205 0.460696 21.00000 -1.20000 H19B 2 0.907049 0.299450 0.387883 21.00000 -1.20000 AFIX 0 PART 2 C16A 1 0.579423 0.283866 0.330578 -21.00000 0.03715 0.08202 = 0.09288 -0.05965 0.00207 0.00843 AFIX 23 H16C 2 0.482749 0.314333 0.349314 -21.00000 -1.20000 H16D 2 0.544835 0.246596 0.286744 -21.00000 -1.20000 AFIX 0 C17A 1 0.641745 0.202001 0.385539 -21.00000 0.07726 0.02388 = 0.10650 -0.00629 0.04751 0.00376 AFIX 23 H17C 2 0.717289 0.155922 0.362981 -21.00000 -1.20000 H17D 2 0.551459 0.160162 0.400340 -21.00000 -1.20000 AFIX 0 C18A 1 0.723343 0.251169 0.449856 -21.00000 0.05975 0.06364 = 0.10337 0.04815 0.02206 0.01518 AFIX 23 H18C 2 0.643279 0.282569 0.479515 -21.00000 -1.20000 H18D 2 0.782166 0.198708 0.478604 -21.00000 -1.20000 AFIX 0 C19A 1 0.845379 0.338025 0.424883 -21.00000 0.03094 0.02123 = 0.07077 0.02276 0.00143 0.00412 AFIX 23 H19C 2 0.893914 0.374206 0.466775 -21.00000 -1.20000 H19D 2 0.931429 0.306012 0.398991 -21.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM rk1844_abs_a.res in P2(1)/n REM wR2 = 0.1159, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0446 for 3130 Fo > 4sig(Fo) and 0.0599 for all 4024 data REM 349 parameters refined using 0 restraints END WGHT 0.0522 0.3206 REM Highest difference peak 0.146, deepest hole -0.148, 1-sigma level 0.031 Q1 1 0.7084 0.7764 0.3582 11.00000 0.05 0.15 Q2 1 0.7174 0.8868 0.5152 11.00000 0.05 0.14 Q3 1 0.5791 0.7392 0.3214 11.00000 0.05 0.14 Q4 1 0.1954 0.4443 0.4622 11.00000 0.05 0.13 Q5 1 0.4512 0.6949 0.3026 11.00000 0.05 0.13 Q6 1 0.8219 0.9553 0.4949 11.00000 0.05 0.13 Q7 1 0.7601 0.8264 0.4180 11.00000 0.05 0.12 Q8 1 0.3277 0.6474 0.3015 11.00000 0.05 0.12 Q9 1 0.9722 0.4932 0.3702 11.00000 0.05 0.12 Q10 1 1.0351 0.9142 0.4663 11.00000 0.05 0.12 Q11 1 0.5205 0.9054 0.3681 11.00000 0.05 0.12 Q12 1 0.5336 0.7346 0.3538 11.00000 0.05 0.11 Q13 1 0.4190 0.5429 0.1948 11.00000 0.05 0.11 Q14 1 0.5892 0.4754 0.2743 11.00000 0.05 0.10 Q15 1 0.4405 0.4132 0.4490 11.00000 0.05 0.10 Q16 1 0.6346 0.8585 0.3999 11.00000 0.05 0.09 Q17 1 0.4938 0.7722 0.2962 11.00000 0.05 0.09 Q18 1 0.2654 0.4618 0.5017 11.00000 0.05 0.09 Q19 1 0.8265 0.6198 0.2809 11.00000 0.05 0.09 Q20 1 0.9232 0.4653 0.2885 11.00000 0.05 0.09 ; _shelx_res_checksum 50270 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 B1 B 0.32234(18) 0.43878(13) 0.44972(9) 0.0366(4) Uani 1 1 d . . . . . H1B1 H 0.4311(16) 0.4040(10) 0.4825(7) 0.038(4) Uiso 1 1 d . . . . . H2B1 H 0.3634(17) 0.4721(11) 0.3967(8) 0.050(4) Uiso 1 1 d . . . . . H3B1 H 0.268(2) 0.5004(13) 0.4828(9) 0.065(5) Uiso 1 1 d . . . . . H4B1 H 0.235(2) 0.3753(14) 0.4373(9) 0.072(5) Uiso 1 1 d . . . . . Li1 Li 0.5849(2) 0.50057(17) 0.43115(12) 0.0343(5) Uani 1 1 d . . . . . N1 N 0.68836(12) 0.63338(8) 0.38338(6) 0.0288(2) Uani 1 1 d . . . . . H1N1 H 0.7465(18) 0.6403(11) 0.4246(8) 0.044(4) Uiso 1 1 d . . . . . N2 N 0.75125(12) 0.41465(8) 0.37589(6) 0.0322(3) Uani 1 1 d . . . . . C1 C 0.79894(16) 0.59151(11) 0.33278(8) 0.0367(3) Uani 1 1 d . . . . . H1A H 0.7373(17) 0.5809(11) 0.2856(8) 0.045(4) Uiso 1 1 d . . . . . H1B H 0.8856(17) 0.6404(11) 0.3237(7) 0.041(4) Uiso 1 1 d . . . . . C2 C 0.87128(15) 0.49283(10) 0.36119(8) 0.0364(3) Uani 1 1 d . . . . . H2A H 0.9474(18) 0.4655(11) 0.3274(8) 0.047(4) Uiso 1 1 d . . . . . H2B H 0.9332(18) 0.5068(11) 0.4085(8) 0.049(4) Uiso 1 1 d . . . . . C3 C 0.62364(14) 0.73219(9) 0.36374(7) 0.0303(3) Uani 1 1 d . . . . . C4 C 0.69684(17) 0.82211(10) 0.39035(7) 0.0394(3) Uani 1 1 d . . . . . C5 C 0.6255(2) 0.91538(12) 0.37266(9) 0.0518(4) Uani 1 1 d . . . . . H5 H 0.676(2) 0.9774(14) 0.3927(9) 0.065(5) Uiso 1 1 d . . . . . C6 C 0.4900(2) 0.92102(12) 0.32882(9) 0.0546(4) Uani 1 1 d . . . . . H6 H 0.442(2) 0.9890(13) 0.3170(9) 0.062(5) Uiso 1 1 d . . . . . C7 C 0.42231(18) 0.83269(12) 0.30134(8) 0.0455(4) Uani 1 1 d . . . . . H7 H 0.3270(19) 0.8362(12) 0.2692(8) 0.051(4) Uiso 1 1 d . . . . . C8 C 0.48635(15) 0.73685(10) 0.31848(7) 0.0340(3) Uani 1 1 d . . . . . C9 C 0.8500(2) 0.82300(12) 0.43707(8) 0.0484(4) Uani 1 1 d . . . . . H9 H 0.8927(19) 0.7541(13) 0.4421(8) 0.052(4) Uiso 1 1 d . . . . . C10 C 0.9788(3) 0.88590(19) 0.40290(13) 0.0723(6) Uani 1 1 d . . . . . H10A H 1.081(2) 0.8799(14) 0.4305(10) 0.075(6) Uiso 1 1 d . . . . . H10B H 0.941(3) 0.9598(19) 0.4014(12) 0.102(8) Uiso 1 1 d . . . . . H10C H 0.994(3) 0.8596(17) 0.3509(14) 0.103(8) Uiso 1 1 d . . . . . C11 C 0.8215(3) 0.86098(19) 0.51137(11) 0.0719(6) Uani 1 1 d . . . . . H11A H 0.922(3) 0.8589(15) 0.5412(11) 0.084(6) Uiso 1 1 d . . . . . H11B H 0.765(3) 0.9316(18) 0.5083(11) 0.096(7) Uiso 1 1 d . . . . . H11C H 0.737(3) 0.8161(18) 0.5340(12) 0.099(7) Uiso 1 1 d . . . . . C12 C 0.40246(15) 0.64203(11) 0.28950(7) 0.0378(3) Uani 1 1 d . . . . . H12 H 0.4589(15) 0.5824(10) 0.3095(7) 0.032(3) Uiso 1 1 d . . . . . C13 C 0.4021(2) 0.63673(16) 0.20863(9) 0.0551(4) Uani 1 1 d . . . . . H13A H 0.346(2) 0.5733(14) 0.1912(9) 0.065(5) Uiso 1 1 d . . . . . H13B H 0.515(2) 0.6356(12) 0.1935(9) 0.062(5) Uiso 1 1 d . . . . . H13C H 0.341(2) 0.6977(15) 0.1868(10) 0.074(6) Uiso 1 1 d . . . . . C14 C 0.23292(18) 0.63649(16) 0.31404(11) 0.0548(5) Uani 1 1 d . . . . . H14A H 0.232(2) 0.6412(13) 0.3690(10) 0.064(5) Uiso 1 1 d . . . . . H14B H 0.169(2) 0.6925(15) 0.2938(10) 0.078(6) Uiso 1 1 d . . . . . H14C H 0.180(2) 0.5716(15) 0.2980(10) 0.075(6) Uiso 1 1 d . . . . . C15 C 0.68219(18) 0.37124(12) 0.30872(8) 0.0465(4) Uani 1 1 d . . . . . H15A H 0.768012 0.338600 0.283030 0.056 Uiso 0.68(3) 1 calc R U P A 1 H15B H 0.637738 0.427638 0.278743 0.056 Uiso 0.68(3) 1 calc R U P A 1 H15C H 0.766929 0.346512 0.278765 0.056 Uiso 0.32(3) 1 calc R U P A 2 H15D H 0.617913 0.423167 0.281866 0.056 Uiso 0.32(3) 1 calc R U P A 2 C16 C 0.5519(13) 0.2926(7) 0.3190(6) 0.0492(15) Uani 0.68(3) 1 d . . P A 1 H16A H 0.508630 0.266948 0.272461 0.059 Uiso 0.68(3) 1 calc R U P A 1 H16B H 0.464138 0.323654 0.344236 0.059 Uiso 0.68(3) 1 calc R U P A 1 C17 C 0.6258(13) 0.2071(9) 0.3616(6) 0.0553(19) Uani 0.68(3) 1 d . . P A 1 H17A H 0.705477 0.171682 0.333818 0.066 Uiso 0.68(3) 1 calc R U P A 1 H17B H 0.543241 0.156790 0.373115 0.066 Uiso 0.68(3) 1 calc R U P A 1 C18 C 0.7062(14) 0.2494(7) 0.4303(6) 0.0488(16) Uani 0.68(3) 1 d . . P A 1 H18A H 0.624366 0.278066 0.460254 0.059 Uiso 0.68(3) 1 calc R U P A 1 H18B H 0.760865 0.193181 0.456898 0.059 Uiso 0.68(3) 1 calc R U P A 1 C19 C 0.8219(13) 0.3296(7) 0.4153(5) 0.0415(19) Uani 0.68(3) 1 d . . P A 1 H19A H 0.871288 0.355205 0.460696 0.050 Uiso 0.68(3) 1 calc R U P A 1 H19B H 0.907049 0.299450 0.387883 0.050 Uiso 0.68(3) 1 calc R U P A 1 C16A C 0.579(3) 0.2839(18) 0.3306(15) 0.071(7) Uani 0.32(3) 1 d . . P A 2 H16C H 0.482749 0.314333 0.349314 0.085 Uiso 0.32(3) 1 calc R U P A 2 H16D H 0.544835 0.246596 0.286744 0.085 Uiso 0.32(3) 1 calc R U P A 2 C17A C 0.642(3) 0.2020(17) 0.3855(17) 0.068(6) Uani 0.32(3) 1 d . . P A 2 H17C H 0.717289 0.155922 0.362981 0.081 Uiso 0.32(3) 1 calc R U P A 2 H17D H 0.551459 0.160162 0.400340 0.081 Uiso 0.32(3) 1 calc R U P A 2 C18A C 0.723(3) 0.2512(19) 0.4499(18) 0.075(6) Uani 0.32(3) 1 d . . P A 2 H18C H 0.643279 0.282569 0.479515 0.090 Uiso 0.32(3) 1 calc R U P A 2 H18D H 0.782166 0.198708 0.478604 0.090 Uiso 0.32(3) 1 calc R U P A 2 C19A C 0.845(3) 0.3380(13) 0.4249(12) 0.041(3) Uani 0.32(3) 1 d . . P A 2 H19C H 0.893914 0.374206 0.466775 0.049 Uiso 0.32(3) 1 calc R U P A 2 H19D H 0.931429 0.306012 0.398991 0.049 Uiso 0.32(3) 1 calc R U P A 2 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 B1 0.0321(8) 0.0416(9) 0.0363(8) 0.0000(7) 0.0030(6) -0.0060(7) Li1 0.0304(10) 0.0357(12) 0.0372(12) 0.0004(10) 0.0048(9) -0.0020(9) N1 0.0279(5) 0.0265(6) 0.0319(6) 0.0013(5) 0.0006(4) -0.0009(4) N2 0.0291(5) 0.0258(6) 0.0418(6) -0.0017(5) 0.0023(4) -0.0011(4) C1 0.0314(7) 0.0340(7) 0.0458(9) 0.0048(6) 0.0129(6) -0.0009(6) C2 0.0255(6) 0.0335(7) 0.0508(9) -0.0016(6) 0.0076(6) 0.0002(6) C3 0.0329(6) 0.0260(6) 0.0320(7) 0.0031(5) 0.0028(5) 0.0007(5) C4 0.0508(8) 0.0295(7) 0.0371(7) -0.0001(6) -0.0045(6) -0.0020(6) C5 0.0748(11) 0.0273(8) 0.0520(10) -0.0025(7) -0.0084(8) 0.0037(8) C6 0.0688(11) 0.0351(9) 0.0592(11) 0.0053(8) -0.0031(8) 0.0163(8) C7 0.0401(8) 0.0466(9) 0.0490(9) 0.0086(7) -0.0044(7) 0.0108(7) C8 0.0305(6) 0.0355(7) 0.0361(7) 0.0043(6) 0.0034(5) 0.0004(6) C9 0.0619(10) 0.0316(8) 0.0495(9) 0.0017(7) -0.0160(7) -0.0106(7) C10 0.0664(12) 0.0722(15) 0.0755(15) 0.0127(12) -0.0213(11) -0.0252(11) C11 0.0933(16) 0.0708(14) 0.0490(11) -0.0049(10) -0.0199(11) -0.0057(13) C12 0.0287(6) 0.0438(8) 0.0406(8) 0.0073(6) -0.0016(5) -0.0053(6) C13 0.0560(10) 0.0649(12) 0.0435(9) -0.0003(8) -0.0039(8) -0.0209(9) C14 0.0294(7) 0.0687(12) 0.0661(12) 0.0197(10) -0.0001(7) -0.0033(8) C15 0.0425(8) 0.0489(9) 0.0486(9) -0.0194(7) 0.0062(6) -0.0035(7) C16 0.037(3) 0.043(2) 0.068(2) -0.0231(19) -0.003(2) -0.011(2) C17 0.050(2) 0.037(3) 0.079(5) -0.014(3) 0.011(3) -0.0096(19) C18 0.059(3) 0.024(2) 0.064(4) 0.006(2) 0.010(3) 0.0082(17) C19 0.034(3) 0.035(2) 0.055(2) -0.0098(19) -0.002(2) 0.0059(18) C16A 0.037(7) 0.082(10) 0.093(12) -0.060(9) 0.002(7) 0.008(5) C17A 0.077(11) 0.024(4) 0.107(16) -0.006(8) 0.048(10) 0.004(5) C18A 0.060(7) 0.064(8) 0.103(16) 0.048(9) 0.022(9) 0.015(6) C19A 0.031(5) 0.021(4) 0.071(8) 0.023(5) 0.001(5) 0.004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 Li1 B1 Li1 77.18(9) . 3_666 ? Li1 B1 H1B1 60.4(6) . . ? Li1 B1 H1B1 56.2(7) 3_666 . ? Li1 B1 H2B1 55.0(7) . . ? Li1 B1 H2B1 124.8(7) 3_666 . ? H1B1 B1 H2B1 109.8(10) . . ? Li1 B1 H3B1 104.2(8) . . ? Li1 B1 H3B1 52.1(8) 3_666 . ? H1B1 B1 H3B1 108.3(10) . . ? H2B1 B1 H3B1 111.0(11) . . ? Li1 B1 H4B1 144.5(9) . . ? Li1 B1 H4B1 126.6(9) 3_666 . ? H1B1 B1 H4B1 107.8(11) . . ? H2B1 B1 H4B1 108.6(11) . . ? H3B1 B1 H4B1 111.3(12) . . ? N2 Li1 N1 85.76(8) . . ? N2 Li1 B1 122.37(11) . . ? N1 Li1 B1 136.72(11) . . ? N2 Li1 B1 115.77(10) . 3_666 ? N1 Li1 B1 90.46(9) . 3_666 ? B1 Li1 B1 102.82(9) . 3_666 ? N2 Li1 Li1 140.93(14) . 3_666 ? N1 Li1 Li1 125.56(13) . 3_666 ? B1 Li1 Li1 52.45(7) . 3_666 ? B1 Li1 Li1 50.37(7) 3_666 3_666 ? N2 Li1 H1B1 110.7(4) . . ? N1 Li1 H1B1 162.7(4) . . ? B1 Li1 H1B1 29.1(4) . . ? B1 Li1 H1B1 86.8(4) 3_666 . ? Li1 Li1 H1B1 42.7(4) 3_666 . ? N2 Li1 H2B1 112.1(4) . . ? N1 Li1 H2B1 114.2(5) . . ? B1 Li1 H2B1 28.8(4) . . ? B1 Li1 H2B1 127.2(4) 3_666 . ? Li1 Li1 H2B1 78.4(4) 3_666 . ? H1B1 Li1 H2B1 55.9(6) . . ? N2 Li1 H1N1 89.1(4) . . ? N1 Li1 H1N1 23.1(4) . . ? B1 Li1 H1N1 146.5(4) . . ? B1 Li1 H1N1 68.5(4) 3_666 . ? Li1 Li1 H1N1 111.2(4) 3_666 . ? H1B1 Li1 H1N1 153.7(5) . . ? H2B1 Li1 H1N1 133.4(6) . . ? C3 N1 C1 114.12(10) . . ? C3 N1 Li1 132.10(9) . . ? C1 N1 Li1 104.87(9) . . ? C3 N1 H1N1 108.2(9) . . ? C1 N1 H1N1 105.3(10) . . ? Li1 N1 H1N1 86.1(10) . . ? C2 N2 C19 111.2(4) . . ? C2 N2 C15 110.19(11) . . ? C19 N2 C15 106.1(4) . . ? C2 N2 C19A 103.1(9) . . ? C15 N2 C19A 115.3(9) . . ? C2 N2 Li1 101.87(10) . . ? C19 N2 Li1 114.8(4) . . ? C15 N2 Li1 112.76(10) . . ? C19A N2 Li1 112.3(8) . . ? N1 C1 C2 110.06(11) . . ? N1 C1 H1A 107.9(8) . . ? C2 C1 H1A 111.8(8) . . ? N1 C1 H1B 111.7(8) . . ? C2 C1 H1B 108.9(8) . . ? H1A C1 H1B 106.4(12) . . ? N2 C2 C1 112.99(10) . . ? N2 C2 H2A 110.2(8) . . ? C1 C2 H2A 109.9(8) . . ? N2 C2 H2B 106.3(8) . . ? C1 C2 H2B 109.4(8) . . ? H2A C2 H2B 107.9(12) . . ? C8 C3 C4 120.80(12) . . ? C8 C3 N1 118.90(11) . . ? C4 C3 N1 120.29(11) . . ? C5 C4 C3 118.13(13) . . ? C5 C4 C9 118.24(13) . . ? C3 C4 C9 123.63(12) . . ? C6 C5 C4 121.64(15) . . ? C6 C5 H5 121.1(10) . . ? C4 C5 H5 117.3(10) . . ? C5 C6 C7 119.67(15) . . ? C5 C6 H6 119.8(10) . . ? C7 C6 H6 120.5(10) . . ? C6 C7 C8 121.26(14) . . ? C6 C7 H7 120.2(9) . . ? C8 C7 H7 118.6(9) . . ? C7 C8 C3 118.45(12) . . ? C7 C8 C12 118.99(12) . . ? C3 C8 C12 122.54(12) . . ? C11 C9 C4 111.38(16) . . ? C11 C9 C10 111.47(16) . . ? C4 C9 C10 110.95(14) . . ? C11 C9 H9 106.8(9) . . ? C4 C9 H9 110.3(9) . . ? C10 C9 H9 105.7(10) . . ? C9 C10 H10A 110.8(11) . . ? C9 C10 H10B 107.2(13) . . ? H10A C10 H10B 110.5(17) . . ? C9 C10 H10C 110.2(12) . . ? H10A C10 H10C 108.3(17) . . ? H10B C10 H10C 109.8(18) . . ? C9 C11 H11A 109.9(12) . . ? C9 C11 H11B 109.6(12) . . ? H11A C11 H11B 115.6(17) . . ? C9 C11 H11C 110.2(12) . . ? H11A C11 H11C 109.8(17) . . ? H11B C11 H11C 101.4(18) . . ? C8 C12 C13 111.89(12) . . ? C8 C12 C14 110.78(13) . . ? C13 C12 C14 110.58(13) . . ? C8 C12 H12 107.9(8) . . ? C13 C12 H12 108.8(8) . . ? C14 C12 H12 106.7(8) . . ? C12 C13 H13A 109.9(10) . . ? C12 C13 H13B 109.5(10) . . ? H13A C13 H13B 109.3(14) . . ? C12 C13 H13C 109.9(11) . . ? H13A C13 H13C 107.1(15) . . ? H13B C13 H13C 111.1(14) . . ? C12 C14 H14A 110.9(10) . . ? C12 C14 H14B 110.7(11) . . ? H14A C14 H14B 108.2(15) . . ? C12 C14 H14C 111.1(11) . . ? H14A C14 H14C 109.0(15) . . ? H14B C14 H14C 106.7(16) . . ? N2 C15 C16 113.7(4) . . ? N2 C15 C16A 105.1(11) . . ? N2 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N2 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N2 C15 H15C 110.7 . . ? C16A C15 H15C 110.7 . . ? N2 C15 H15D 110.7 . . ? C16A C15 H15D 110.7 . . ? H15C C15 H15D 108.8 . . ? C15 C16 C17 107.0(8) . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16B 110.3 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 109.7(8) . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 111.2(8) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C18 112.8(8) . . ? N2 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? N2 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C17A C16A C15 121.7(18) . . ? C17A C16A H16C 106.9 . . ? C15 C16A H16C 106.9 . . ? C17A C16A H16D 106.9 . . ? C15 C16A H16D 107.0 . . ? H16C C16A H16D 106.7 . . ? C16A C17A C18A 111.4(17) . . ? C16A C17A H17C 109.3 . . ? C18A C17A H17C 109.3 . . ? C16A C17A H17D 109.4 . . ? C18A C17A H17D 109.3 . . ? H17C C17A H17D 108.0 . . ? C19A C18A C17A 109.4(19) . . ? C19A C18A H18C 109.8 . . ? C17A C18A H18C 109.8 . . ? C19A C18A H18D 109.8 . . ? C17A C18A H18D 109.8 . . ? H18C C18A H18D 108.2 . . ? N2 C19A C18A 108.3(17) . . ? N2 C19A H19C 110.0 . . ? C18A C19A H19C 110.1 . . ? N2 C19A H19D 110.0 . . ? C18A C19A H19D 110.0 . . ? H19C C19A H19D 108.4 . . ? 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 B1 Li1 2.400(3) . ? B1 Li1 2.470(3) 3_666 ? B1 H1B1 1.168(14) . ? B1 H2B1 1.163(15) . ? B1 H3B1 1.131(17) . ? B1 H4B1 1.123(18) . ? Li1 N2 2.117(2) . ? Li1 N1 2.162(2) . ? Li1 Li1 3.038(4) 3_666 ? Li1 H1B1 2.086(13) . ? Li1 H2B1 1.977(15) . ? Li1 H1N1 2.285(15) . ? N1 C3 1.4421(15) . ? N1 C1 1.4769(16) . ? N1 H1N1 0.900(16) . ? N2 C2 1.4751(16) . ? N2 C19 1.447(9) . ? N2 C15 1.4785(17) . ? N2 C19A 1.551(19) . ? C1 C2 1.5119(19) . ? C1 H1A 1.015(15) . ? C1 H1B 0.992(15) . ? C2 H2A 0.996(15) . ? C2 H2B 1.025(16) . ? C3 C8 1.4004(17) . ? C3 C4 1.4068(18) . ? C4 C5 1.391(2) . ? C4 C9 1.522(2) . ? C5 C6 1.374(2) . ? C5 H5 0.982(18) . ? C6 C7 1.376(2) . ? C6 H6 0.997(17) . ? C7 C8 1.3946(19) . ? C7 H7 0.979(16) . ? C8 C12 1.5137(19) . ? C9 C11 1.520(3) . ? C9 C10 1.533(3) . ? C9 H9 0.972(17) . ? C10 H10A 0.99(2) . ? C10 H10B 1.02(2) . ? C10 H10C 1.06(2) . ? C11 H11A 0.99(2) . ? C11 H11B 1.04(2) . ? C11 H11C 1.04(2) . ? C12 C13 1.529(2) . ? C12 C14 1.5285(19) . ? C12 H12 0.978(14) . ? C13 H13A 1.001(18) . ? C13 H13B 1.011(18) . ? C13 H13C 1.02(2) . ? C14 H14A 1.039(18) . ? C14 H14B 0.98(2) . ? C14 H14C 1.00(2) . ? C15 C16 1.525(8) . ? C15 C16A 1.50(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 H15C 0.9900 . ? C15 H15D 0.9900 . ? C16 C17 1.493(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.531(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.469(16) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C16A C17A 1.56(3) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C17A C18A 1.51(3) . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C18A C19A 1.62(4) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ?