#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:28:56 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267144 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707504.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_7707504 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 'C19 H32 B Cl N2' _chemical_formula_sum 'C19 H32 B Cl N2' _chemical_formula_weight 334.72 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.3711(2) _cell_length_b 12.4969(2) _cell_length_c 18.2513(2) _cell_measurement_reflns_used 20700 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 74.331 _cell_measurement_theta_min 4.846 _cell_volume 3962.08(9) _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 0.997 _diffrn_measured_fraction_theta_max 0.980 _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 0.0265 _diffrn_reflns_av_unetI/netI 0.0161 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 20700 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.331 _diffrn_reflns_theta_min 4.846 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_correction_T_min 0.829 _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 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1456 _exptl_crystal_size_max 0.183 _exptl_crystal_size_mid 0.073 _exptl_crystal_size_min 0.043 _refine_diff_density_max 0.257 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.037 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 216 _refine_ls_number_reflns 3963 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0320 _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^)+(0.0430P)^2^+1.3446P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.0869 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3515 _reflns_number_total 3963 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01454d2.cif _cod_data_source_block FO6950_5a _cod_depositor_comments 'Adding full bibliography for 7707498--7707509.cif.' _cod_database_code 7707504 _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 0.748 _shelx_estimated_absorpt_t_max 0.931 _shelx_res_file ; TITL rk1825_abs_a.res in Pbca fo6950.res created by SHELXL-2018/3 at 16:49:47 on 20-Apr-2021 CELL 1.54184 17.3711 12.4969 18.2513 90 90 90 ZERR 8 0.0002 0.0002 0.0002 0.0 0.0 0.0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H B Cl N UNIT 152 256 8 8 16 L.S. 8 PLAN 20 TEMP -150.15(11) BOND $H fmap 2 acta SIZE 0.183 0.073 0.043 REM COLOR:colourless WGHT 0.043000 1.344600 FVAR 0.27765 B1 3 0.732122 0.666326 0.252078 11.00000 0.01847 0.01681 = 0.01971 0.00121 0.00173 0.00134 CL1 4 0.835085 0.628225 0.213159 11.00000 0.02361 0.03184 = 0.02820 0.00182 0.00668 0.00654 N1 5 0.731764 0.684612 0.331164 11.00000 0.02104 0.01384 = 0.01835 -0.00125 -0.00007 -0.00170 N2 5 0.713860 0.786814 0.222867 11.00000 0.02271 0.01655 = 0.02086 0.00077 0.00151 0.00008 C1 1 0.742436 0.796345 0.351997 11.00000 0.03343 0.01640 = 0.02461 -0.00312 -0.00222 -0.00240 AFIX 23 H1A 2 0.787413 0.804717 0.384813 11.00000 -1.20000 H1B 2 0.696103 0.824715 0.376902 11.00000 -1.20000 AFIX 0 C2 1 0.755797 0.852741 0.279145 11.00000 0.03289 0.01756 = 0.02764 -0.00040 -0.00320 -0.00568 AFIX 23 H2A 2 0.735080 0.926511 0.280601 11.00000 -1.20000 H2B 2 0.811459 0.856077 0.267727 11.00000 -1.20000 AFIX 0 C3 1 0.721876 0.607954 0.388090 11.00000 0.01991 0.01500 = 0.01743 -0.00250 0.00121 0.00049 C4 1 0.785288 0.576797 0.431352 11.00000 0.02185 0.01777 = 0.02069 -0.00398 -0.00131 0.00065 C5 1 0.772848 0.508410 0.490790 11.00000 0.02857 0.02153 = 0.02209 -0.00099 -0.00451 0.00456 AFIX 43 H5 2 0.815186 0.487920 0.520601 11.00000 -1.20000 AFIX 0 C6 1 0.700120 0.469920 0.507116 11.00000 0.03520 0.01999 = 0.02108 0.00219 0.00297 0.00213 AFIX 43 H6 2 0.692446 0.424819 0.548375 11.00000 -1.20000 AFIX 0 C7 1 0.638776 0.497744 0.462806 11.00000 0.02375 0.02143 = 0.02543 0.00019 0.00512 -0.00183 AFIX 43 H7 2 0.589189 0.469569 0.473284 11.00000 -1.20000 AFIX 0 C8 1 0.647916 0.566096 0.403165 11.00000 0.02034 0.01804 = 0.02008 -0.00278 0.00183 0.00023 C9 1 0.866471 0.616354 0.415612 11.00000 0.01928 0.02552 = 0.02864 -0.00292 -0.00311 -0.00009 AFIX 13 H9 2 0.864126 0.663702 0.371498 11.00000 -1.20000 AFIX 0 C10 1 0.898001 0.682755 0.479453 11.00000 0.02746 0.03879 = 0.04076 -0.01181 -0.00634 -0.00484 AFIX 137 H10A 2 0.862012 0.740845 0.490757 11.00000 -1.50000 H10B 2 0.948040 0.713020 0.465837 11.00000 -1.50000 H10C 2 0.904122 0.636883 0.522612 11.00000 -1.50000 AFIX 0 C11 1 0.920928 0.523335 0.398139 11.00000 0.02408 0.03533 = 0.04503 -0.00734 0.00087 0.00370 AFIX 137 H11A 2 0.923092 0.474512 0.440107 11.00000 -1.50000 H11B 2 0.972562 0.551314 0.388088 11.00000 -1.50000 H11C 2 0.901959 0.484688 0.355047 11.00000 -1.50000 AFIX 0 C12 1 0.578149 0.596077 0.357549 11.00000 0.01709 0.02544 = 0.02396 -0.00029 0.00184 -0.00129 AFIX 13 H12 2 0.597173 0.633292 0.312550 11.00000 -1.20000 AFIX 0 C13 1 0.526196 0.674309 0.398723 11.00000 0.02901 0.03865 = 0.03757 -0.00648 -0.00213 0.01073 AFIX 137 H13A 2 0.507443 0.640529 0.443773 11.00000 -1.50000 H13B 2 0.482336 0.693735 0.367680 11.00000 -1.50000 H13C 2 0.555490 0.738836 0.411120 11.00000 -1.50000 AFIX 0 C14 1 0.532247 0.498352 0.332791 11.00000 0.02966 0.03443 = 0.05152 -0.00824 -0.01094 -0.00378 AFIX 137 H14A 2 0.566119 0.449460 0.305899 11.00000 -1.50000 H14B 2 0.490024 0.521265 0.300822 11.00000 -1.50000 H14C 2 0.511137 0.461608 0.375762 11.00000 -1.50000 AFIX 0 C15 1 0.628901 0.811497 0.228324 11.00000 0.02439 0.02015 = 0.02594 0.00176 0.00329 0.00600 AFIX 23 H15A 2 0.620957 0.889180 0.220850 11.00000 -1.20000 H15B 2 0.610615 0.793361 0.278176 11.00000 -1.20000 AFIX 0 C16 1 0.581488 0.750125 0.172482 11.00000 0.02346 0.02984 = 0.02866 0.00300 -0.00150 0.00369 AFIX 23 H16A 2 0.526713 0.771034 0.176889 11.00000 -1.20000 H16B 2 0.585421 0.672466 0.182522 11.00000 -1.20000 AFIX 0 C17 1 0.609585 0.772998 0.094856 11.00000 0.03308 0.03803 = 0.02569 0.00440 -0.00471 0.00284 AFIX 23 H17A 2 0.582569 0.725542 0.059852 11.00000 -1.20000 H17B 2 0.597599 0.848025 0.081701 11.00000 -1.20000 AFIX 0 C18 1 0.695998 0.754543 0.089508 11.00000 0.03275 0.03107 = 0.02058 0.00257 0.00340 0.00211 AFIX 23 H18A 2 0.706993 0.677357 0.095802 11.00000 -1.20000 H18B 2 0.714100 0.776017 0.040220 11.00000 -1.20000 AFIX 0 C19 1 0.739531 0.817721 0.147127 11.00000 0.02871 0.02397 = 0.02321 0.00654 0.00471 -0.00127 AFIX 23 H19A 2 0.795406 0.804030 0.142005 11.00000 -1.20000 H19B 2 0.730568 0.895165 0.139533 11.00000 -1.20000 AFIX 0 H1B1 2 0.691077 0.600154 0.225134 11.00000 0.01937 HKLF 4 REM rk1825_abs_a.res in Pbca REM wR2 = 0.0869, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0320 for 3515 Fo > 4sig(Fo) and 0.0372 for all 3963 data REM 216 parameters refined using 0 restraints END WGHT 0.0433 1.3523 REM Highest difference peak 0.257, deepest hole -0.253, 1-sigma level 0.037 Q1 1 0.6128 0.5794 0.3799 11.00000 0.05 0.26 Q2 1 0.7390 0.6658 0.2922 11.00000 0.05 0.25 Q3 1 0.7782 0.5455 0.4570 11.00000 0.05 0.25 Q4 1 0.6813 0.5831 0.3918 11.00000 0.05 0.25 Q5 1 0.6807 0.5641 0.2003 11.00000 0.05 0.25 Q6 1 0.9053 0.7365 0.2516 11.00000 0.05 0.24 Q7 1 0.8233 0.5998 0.4252 11.00000 0.05 0.23 Q8 1 0.7371 0.8201 0.2487 11.00000 0.05 0.23 Q9 1 0.5539 0.6338 0.3765 11.00000 0.05 0.23 Q10 1 0.7563 0.8245 0.3162 11.00000 0.05 0.21 Q11 1 0.6071 0.7807 0.2003 11.00000 0.05 0.21 Q12 1 0.7238 0.7302 0.2320 11.00000 0.05 0.20 Q13 1 0.7065 0.6195 0.2406 11.00000 0.05 0.20 Q14 1 0.7521 0.5953 0.4139 11.00000 0.05 0.20 Q15 1 0.6433 0.5497 0.4351 11.00000 0.05 0.20 Q16 1 0.6521 0.7666 0.0927 11.00000 0.05 0.20 Q17 1 0.7261 0.8016 0.1846 11.00000 0.05 0.19 Q18 1 0.7403 0.7292 0.3395 11.00000 0.05 0.19 Q19 1 0.7375 0.4787 0.4905 11.00000 0.05 0.19 Q20 1 0.7169 0.7803 0.1202 11.00000 0.05 0.19 ; _shelx_res_checksum 15245 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 B1 B 0.73212(7) 0.66633(10) 0.25208(7) 0.0183(3) Uani 1 1 d . . . . . Cl1 Cl 0.83509(2) 0.62823(3) 0.21316(2) 0.02788(10) Uani 1 1 d . . . . . N1 N 0.73176(6) 0.68461(7) 0.33116(5) 0.0177(2) Uani 1 1 d . . . . . N2 N 0.71386(6) 0.78681(8) 0.22287(5) 0.0200(2) Uani 1 1 d . . . . . C1 C 0.74244(8) 0.79634(10) 0.35200(7) 0.0248(3) Uani 1 1 d . . . . . H1A H 0.787413 0.804717 0.384813 0.030 Uiso 1 1 calc R U . . . H1B H 0.696103 0.824715 0.376902 0.030 Uiso 1 1 calc R U . . . C2 C 0.75580(8) 0.85274(10) 0.27915(7) 0.0260(3) Uani 1 1 d . . . . . H2A H 0.735080 0.926511 0.280601 0.031 Uiso 1 1 calc R U . . . H2B H 0.811459 0.856077 0.267727 0.031 Uiso 1 1 calc R U . . . C3 C 0.72188(7) 0.60795(9) 0.38809(6) 0.0174(2) Uani 1 1 d . . . . . C4 C 0.78529(7) 0.57680(9) 0.43135(6) 0.0201(2) Uani 1 1 d . . . . . C5 C 0.77285(7) 0.50841(10) 0.49079(7) 0.0241(3) Uani 1 1 d . . . . . H5 H 0.815186 0.487920 0.520601 0.029 Uiso 1 1 calc R U . . . C6 C 0.70012(8) 0.46992(10) 0.50712(7) 0.0254(3) Uani 1 1 d . . . . . H6 H 0.692446 0.424819 0.548375 0.031 Uiso 1 1 calc R U . . . C7 C 0.63878(7) 0.49774(10) 0.46281(7) 0.0235(3) Uani 1 1 d . . . . . H7 H 0.589189 0.469569 0.473284 0.028 Uiso 1 1 calc R U . . . C8 C 0.64792(7) 0.56610(9) 0.40316(6) 0.0195(2) Uani 1 1 d . . . . . C9 C 0.86647(7) 0.61635(10) 0.41561(7) 0.0245(3) Uani 1 1 d . . . . . H9 H 0.864126 0.663702 0.371498 0.029 Uiso 1 1 calc R U . . . C10 C 0.89800(8) 0.68275(12) 0.47945(8) 0.0357(3) Uani 1 1 d . . . . . H10A H 0.862012 0.740845 0.490757 0.054 Uiso 1 1 calc R U . . . H10B H 0.948040 0.713020 0.465837 0.054 Uiso 1 1 calc R U . . . H10C H 0.904122 0.636883 0.522612 0.054 Uiso 1 1 calc R U . . . C11 C 0.92093(8) 0.52334(12) 0.39814(9) 0.0348(3) Uani 1 1 d . . . . . H11A H 0.923092 0.474512 0.440107 0.052 Uiso 1 1 calc R U . . . H11B H 0.972562 0.551314 0.388088 0.052 Uiso 1 1 calc R U . . . H11C H 0.901959 0.484688 0.355047 0.052 Uiso 1 1 calc R U . . . C12 C 0.57815(7) 0.59608(10) 0.35755(7) 0.0222(3) Uani 1 1 d . . . . . H12 H 0.597173 0.633292 0.312550 0.027 Uiso 1 1 calc R U . . . C13 C 0.52620(8) 0.67431(12) 0.39872(8) 0.0351(3) Uani 1 1 d . . . . . H13A H 0.507443 0.640529 0.443773 0.053 Uiso 1 1 calc R U . . . H13B H 0.482336 0.693735 0.367680 0.053 Uiso 1 1 calc R U . . . H13C H 0.555490 0.738836 0.411120 0.053 Uiso 1 1 calc R U . . . C14 C 0.53225(9) 0.49835(12) 0.33279(9) 0.0385(4) Uani 1 1 d . . . . . H14A H 0.566119 0.449460 0.305899 0.058 Uiso 1 1 calc R U . . . H14B H 0.490024 0.521265 0.300822 0.058 Uiso 1 1 calc R U . . . H14C H 0.511137 0.461608 0.375762 0.058 Uiso 1 1 calc R U . . . C15 C 0.62890(7) 0.81150(10) 0.22832(7) 0.0235(3) Uani 1 1 d . . . . . H15A H 0.620957 0.889180 0.220850 0.028 Uiso 1 1 calc R U . . . H15B H 0.610615 0.793361 0.278176 0.028 Uiso 1 1 calc R U . . . C16 C 0.58149(7) 0.75013(11) 0.17248(7) 0.0273(3) Uani 1 1 d . . . . . H16A H 0.526713 0.771034 0.176889 0.033 Uiso 1 1 calc R U . . . H16B H 0.585421 0.672466 0.182522 0.033 Uiso 1 1 calc R U . . . C17 C 0.60958(8) 0.77300(12) 0.09486(7) 0.0323(3) Uani 1 1 d . . . . . H17A H 0.582569 0.725542 0.059852 0.039 Uiso 1 1 calc R U . . . H17B H 0.597599 0.848025 0.081701 0.039 Uiso 1 1 calc R U . . . C18 C 0.69600(8) 0.75454(11) 0.08951(7) 0.0281(3) Uani 1 1 d . . . . . H18A H 0.706993 0.677357 0.095802 0.034 Uiso 1 1 calc R U . . . H18B H 0.714100 0.776017 0.040220 0.034 Uiso 1 1 calc R U . . . C19 C 0.73953(8) 0.81772(10) 0.14713(7) 0.0253(3) Uani 1 1 d . . . . . H19A H 0.795406 0.804030 0.142005 0.030 Uiso 1 1 calc R U . . . H19B H 0.730568 0.895165 0.139533 0.030 Uiso 1 1 calc R U . . . H1B1 H 0.6911(8) 0.6002(12) 0.2251(8) 0.019(3) Uiso 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 B1 0.0185(6) 0.0168(6) 0.0197(6) 0.0012(5) 0.0017(5) 0.0013(5) Cl1 0.02361(16) 0.03184(17) 0.02820(17) 0.00182(12) 0.00668(11) 0.00654(12) N1 0.0210(5) 0.0138(5) 0.0184(5) -0.0013(4) -0.0001(4) -0.0017(4) N2 0.0227(5) 0.0166(5) 0.0209(5) 0.0008(4) 0.0015(4) 0.0001(4) C1 0.0334(7) 0.0164(6) 0.0246(6) -0.0031(5) -0.0022(5) -0.0024(5) C2 0.0329(7) 0.0176(6) 0.0276(6) -0.0004(5) -0.0032(5) -0.0057(5) C3 0.0199(6) 0.0150(5) 0.0174(5) -0.0025(4) 0.0012(4) 0.0005(4) C4 0.0219(6) 0.0178(6) 0.0207(5) -0.0040(4) -0.0013(4) 0.0007(4) C5 0.0286(7) 0.0215(6) 0.0221(6) -0.0010(5) -0.0045(5) 0.0046(5) C6 0.0352(7) 0.0200(6) 0.0211(6) 0.0022(5) 0.0030(5) 0.0021(5) C7 0.0238(6) 0.0214(6) 0.0254(6) 0.0002(5) 0.0051(5) -0.0018(5) C8 0.0203(6) 0.0180(5) 0.0201(5) -0.0028(4) 0.0018(4) 0.0002(4) C9 0.0193(6) 0.0255(6) 0.0286(6) -0.0029(5) -0.0031(5) -0.0001(5) C10 0.0275(7) 0.0388(8) 0.0408(8) -0.0118(6) -0.0063(6) -0.0048(6) C11 0.0241(7) 0.0353(8) 0.0450(8) -0.0073(6) 0.0009(6) 0.0037(6) C12 0.0171(6) 0.0254(6) 0.0240(6) -0.0003(5) 0.0018(4) -0.0013(5) C13 0.0290(7) 0.0386(8) 0.0376(8) -0.0065(6) -0.0021(6) 0.0107(6) C14 0.0297(7) 0.0344(8) 0.0515(9) -0.0082(7) -0.0109(6) -0.0038(6) C15 0.0244(6) 0.0201(6) 0.0259(6) 0.0018(5) 0.0033(5) 0.0060(5) C16 0.0235(6) 0.0298(7) 0.0287(6) 0.0030(5) -0.0015(5) 0.0037(5) C17 0.0331(7) 0.0380(8) 0.0257(7) 0.0044(6) -0.0047(5) 0.0028(6) C18 0.0328(7) 0.0311(7) 0.0206(6) 0.0026(5) 0.0034(5) 0.0021(5) C19 0.0287(7) 0.0240(6) 0.0232(6) 0.0065(5) 0.0047(5) -0.0013(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Cl Cl 0.3639 0.7018 '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 N1 B1 N2 100.25(9) . . ? N1 B1 Cl1 113.28(8) . . ? N2 B1 Cl1 106.29(8) . . ? N1 B1 H1B1 120.7(7) . . ? N2 B1 H1B1 112.8(7) . . ? Cl1 B1 H1B1 103.0(7) . . ? C3 N1 C1 117.98(9) . . ? C3 N1 B1 128.03(10) . . ? C1 N1 B1 113.99(10) . . ? C19 N2 C2 110.09(9) . . ? C19 N2 C15 107.34(9) . . ? C2 N2 C15 108.43(9) . . ? C19 N2 B1 118.74(9) . . ? C2 N2 B1 100.86(9) . . ? C15 N2 B1 110.94(9) . . ? N1 C1 C2 103.58(10) . . ? N1 C1 H1A 111.0 . . ? C2 C1 H1A 111.0 . . ? N1 C1 H1B 111.0 . . ? C2 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? N2 C2 C1 105.60(10) . . ? N2 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? N2 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? C4 C3 C8 119.91(11) . . ? C4 C3 N1 120.01(10) . . ? C8 C3 N1 120.03(10) . . ? C5 C4 C3 118.86(11) . . ? C5 C4 C9 119.24(11) . . ? C3 C4 C9 121.91(11) . . ? C6 C5 C4 121.37(11) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C5 119.36(11) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 121.58(12) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C3 118.85(11) . . ? C7 C8 C12 119.29(11) . . ? C3 C8 C12 121.84(10) . . ? C4 C9 C10 111.33(11) . . ? C4 C9 C11 111.41(11) . . ? C10 C9 C11 110.40(11) . . ? C4 C9 H9 107.8 . . ? C10 C9 H9 107.8 . . ? C11 C9 H9 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 C14 112.46(11) . . ? C8 C12 C13 111.09(10) . . ? C14 C12 C13 110.42(11) . . ? C8 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 112.49(10) . . ? N2 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N2 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C17 110.81(11) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C16 110.29(11) . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C17 111.62(11) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C18 110.85(10) . . ? N2 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? 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 N1 1.4614(16) . ? B1 N2 1.6285(16) . ? B1 Cl1 1.9825(13) . ? B1 H1B1 1.198(14) . ? N1 C3 1.4236(15) . ? N1 C1 1.4590(15) . ? N2 C19 1.5030(15) . ? N2 C2 1.5048(16) . ? N2 C15 1.5110(16) . ? C1 C2 1.5227(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.4101(17) . ? C3 C8 1.4142(16) . ? C4 C5 1.3978(17) . ? C4 C9 1.5217(17) . ? C5 C6 1.3843(19) . ? C5 H5 0.9500 . ? C6 C7 1.3822(19) . ? C6 H6 0.9500 . ? C7 C8 1.3928(17) . ? C7 H7 0.9500 . ? C8 C12 1.5173(17) . ? C9 C10 1.5317(18) . ? C9 C11 1.5323(18) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.5269(18) . ? C12 C13 1.5281(18) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.5183(18) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.5255(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.522(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.5170(18) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ?