#------------------------------------------------------------------------------ #$Date: 2023-03-18 03:51:48 +0200 (Sat, 18 Mar 2023) $ #$Revision: 281939 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/64/7246466.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_7246466 loop_ _publ_author_name 'Magott, Micha\/l' 'Wegner, Wojciech' _publ_section_title ; Approaching the free-ion limit in magnetically isotropic gadolinium(III) via borohydride ligands ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/D3CP01047C _journal_year 2023 _chemical_formula_sum 'C16 H52 B4 Gd N' _chemical_formula_weight 459.07 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-09-12 deposited with the CCDC. 2023-03-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 128.2820(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.0900(5) _cell_length_b 19.9970(10) _cell_length_c 14.7492(7) _cell_measurement_reflns_used 9900 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.42 _cell_measurement_theta_min 2.55 _cell_volume 2567.5(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL, Mercury' _computing_publication_material 'Bruker SHELXTL, Mercury' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_unetI/netI 0.0228 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 31968 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.019 _diffrn_reflns_theta_min 2.552 _exptl_absorpt_coefficient_mu 2.580 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.188 _exptl_crystal_description block _exptl_crystal_F_000 956 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.514 _refine_diff_density_min -2.704 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 251 _refine_ls_number_reflns 5054 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.318 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0386 _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^)+(0.0025P)^2^+7.4275P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.0625 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4600 _reflns_number_total 5054 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp01047c2.cif _cod_data_source_block (TBA)Gd(BH4)4_100K _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7246466 _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 0.747 _shelx_estimated_absorpt_t_max 0.861 _shelx_res_file ; CELL 0.71073 11.0900 19.9970 14.7492 90.000 128.282 90.000 ZERR 4.00 0.0005 0.0010 0.0007 0.000 0.001 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N GD B UNIT 64 208 4 4 16 OMIT 1 0 0 LIST 4 TEMP -173.150 SIZE 0.060 0.100 0.120 DFIX 1.15 0.02 B1 H1B DFIX 1.15 0.02 B1 H2B DFIX 1.15 0.02 B1 H3B DFIX 1.15 0.02 B1 H4B DFIX 1.15 0.02 B2 H5B DFIX 1.15 0.02 B2 H6B DFIX 1.15 0.02 B2 H7B DFIX 1.15 0.02 B2 H8B DFIX 1.15 0.02 B3 H9B DFIX 1.15 0.02 B3 H10B DFIX 1.15 0.02 B3 H11B DFIX 1.15 0.02 B3 H12B DFIX 1.15 0.02 B4 H13B DFIX 1.15 0.02 B4 H14B DFIX 1.15 0.02 B4 H15B DFIX 1.15 0.02 B4 H16B ACTA L.S. 10 FMAP 2 PLAN -25 0 0.00 HTAB BOND $H CONF WGHT 0.002500 7.427500 FVAR 0.31615 GD1 4 0.830908 0.688152 0.538955 11.00000 0.01259 0.01424 = 0.01677 0.00124 0.00859 0.00005 N1 3 0.413530 0.622749 0.650068 11.00000 0.01180 0.01219 = 0.01438 -0.00160 0.00818 -0.00017 C1 1 0.387435 0.875679 0.603683 11.00000 0.02624 0.01290 = 0.03585 -0.00072 0.01500 0.00021 AFIX 137 H1 2 0.499640 0.879638 0.656412 11.00000 -1.50000 H11 2 0.342043 0.915513 0.610474 11.00000 -1.50000 H10 2 0.351268 0.871688 0.524146 11.00000 -1.50000 AFIX 0 B1 5 0.709226 0.578957 0.530428 11.00000 0.02060 0.01907 = 0.02795 -0.00282 0.01613 -0.00313 H1B 2 0.734847 0.614977 0.600161 11.00000 -1.50000 H2B 2 0.822830 0.571946 0.546039 11.00000 -1.50000 H3B 2 0.653380 0.530253 0.528115 11.00000 -1.50000 H4B 2 0.632654 0.609789 0.446932 11.00000 -1.50000 C2 1 0.340140 0.814254 0.634576 11.00000 0.02773 0.01598 = 0.03103 0.00173 0.02059 0.00527 AFIX 23 H9 2 0.226669 0.810970 0.582129 11.00000 -1.20000 H12 2 0.375103 0.818910 0.714422 11.00000 -1.20000 AFIX 0 B2 5 0.647015 0.781157 0.495920 11.00000 0.02578 0.02382 = 0.02147 0.00133 0.01265 0.00436 H5B 2 0.687011 0.747313 0.572966 11.00000 -1.50000 H6B 2 0.596691 0.746817 0.417838 11.00000 -1.50000 H7B 2 0.759938 0.799643 0.518285 11.00000 -1.50000 H8B 2 0.564675 0.823454 0.475717 11.00000 -1.50000 C3 1 0.407353 0.750154 0.625662 11.00000 0.01691 0.01398 = 0.01663 0.00004 0.00936 0.00124 AFIX 23 H13 2 0.376877 0.746211 0.547020 11.00000 -1.20000 H8 2 0.520903 0.751836 0.681472 11.00000 -1.20000 AFIX 0 B3 5 0.869734 0.685240 0.386952 11.00000 0.03049 0.04101 = 0.02960 0.00285 0.02119 -0.00022 H9B 2 0.901856 0.733900 0.438375 11.00000 -1.50000 H10B 2 0.746185 0.677431 0.355117 11.00000 -1.50000 H11B 2 0.942406 0.646521 0.459411 11.00000 -1.50000 H12B 2 0.887029 0.682888 0.318588 11.00000 -1.50000 C4 1 0.349475 0.690008 0.651043 11.00000 0.01533 0.01352 = 0.01852 -0.00051 0.01047 0.00307 AFIX 23 H15 2 0.236113 0.688568 0.593252 11.00000 -1.20000 H14 2 0.375162 0.696264 0.727844 11.00000 -1.20000 AFIX 0 B4 5 1.087631 0.701070 0.735854 11.00000 0.02148 0.01916 = 0.02796 -0.00172 0.01220 0.00010 H13B 2 0.985984 0.710897 0.735592 11.00000 -1.50000 H14B 2 1.067086 0.649233 0.694491 11.00000 -1.50000 H15B 2 1.069644 0.737882 0.668172 11.00000 -1.50000 H16B 2 1.208053 0.705591 0.822413 11.00000 -1.50000 C5 1 0.400565 0.615101 0.542111 11.00000 0.01454 0.01376 = 0.01529 -0.00105 0.00986 -0.00029 AFIX 23 H7 2 0.448764 0.572152 0.547094 11.00000 -1.20000 H6 2 0.460590 0.651341 0.541156 11.00000 -1.20000 AFIX 0 C6 1 0.238802 0.616666 0.428437 11.00000 0.01677 0.01691 = 0.01690 -0.00089 0.00905 0.00166 AFIX 23 H34 2 0.183797 0.656687 0.425337 11.00000 -1.20000 H35 2 0.181559 0.576455 0.421563 11.00000 -1.20000 AFIX 0 C7 1 0.247980 0.618538 0.329036 11.00000 0.01870 0.02149 = 0.01652 -0.00010 0.00982 -0.00036 AFIX 23 H4 2 0.287571 0.662647 0.327911 11.00000 -1.20000 H5 2 0.320874 0.583888 0.341838 11.00000 -1.20000 AFIX 0 C8 1 0.091334 0.606458 0.212915 11.00000 0.02602 0.02695 = 0.01597 -0.00092 0.01059 -0.00382 AFIX 137 H36 2 0.057339 0.560803 0.210525 11.00000 -1.50000 H2 2 0.099023 0.612365 0.150693 11.00000 -1.50000 H3 2 0.016918 0.638438 0.202862 11.00000 -1.50000 AFIX 0 C9 1 0.582970 0.619207 0.754402 11.00000 0.00952 0.01524 = 0.01243 -0.00013 0.00423 0.00025 AFIX 23 H24 2 0.638752 0.653971 0.745748 11.00000 -1.20000 H16 2 0.593194 0.630272 0.824310 11.00000 -1.20000 AFIX 0 C10 1 0.660834 0.552209 0.773807 11.00000 0.01478 0.01187 = 0.01883 0.00508 0.00855 0.00259 AFIX 23 H23 2 0.663013 0.542814 0.708932 11.00000 -1.20000 H22 2 0.601759 0.516182 0.776352 11.00000 -1.20000 AFIX 0 C11 1 0.825022 0.553382 0.887402 11.00000 0.01848 0.02149 = 0.01776 0.00389 0.00885 0.00463 AFIX 23 H21 2 0.822755 0.570388 0.949370 11.00000 -1.20000 H20 2 0.864880 0.507033 0.907749 11.00000 -1.20000 AFIX 0 C12 1 0.934598 0.596259 0.883171 11.00000 0.01520 0.02789 = 0.02221 0.00422 0.00535 0.00193 AFIX 137 H18 2 0.934283 0.581064 0.819854 11.00000 -1.50000 H17 2 1.038591 0.592290 0.956483 11.00000 -1.50000 H19 2 0.901578 0.643069 0.870446 11.00000 -1.50000 AFIX 0 C13 1 0.322866 0.566918 0.652733 11.00000 0.01432 0.01285 = 0.01975 -0.00290 0.00962 -0.00197 AFIX 23 H33 2 0.348309 0.524516 0.633362 11.00000 -1.20000 H32 2 0.212240 0.575597 0.591020 11.00000 -1.20000 AFIX 0 C14 1 0.347734 0.556786 0.765548 11.00000 0.01575 0.01744 = 0.01841 0.00176 0.01103 -0.00096 AFIX 23 H31 2 0.456323 0.544874 0.827831 11.00000 -1.20000 H30 2 0.324556 0.598748 0.787638 11.00000 -1.20000 AFIX 0 C15 1 0.243200 0.501153 0.750411 11.00000 0.02179 0.01959 = 0.02741 -0.00012 0.01606 -0.00269 AFIX 23 H25 2 0.259278 0.460914 0.719967 11.00000 -1.20000 H26 2 0.134896 0.515283 0.692736 11.00000 -1.20000 AFIX 0 C16 1 0.271753 0.483182 0.862483 11.00000 0.04046 0.03716 = 0.03612 0.00165 0.02844 -0.01140 AFIX 137 H27 2 0.380010 0.471179 0.921118 11.00000 -1.50000 H29 2 0.206799 0.445157 0.849172 11.00000 -1.50000 H28 2 0.246849 0.521630 0.889372 11.00000 -1.50000 REM ##### REM ##### REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM wR2 = 0.062471, GooF = S = 1.31994, Restrained GooF = 1.31799 for all data REM R1 = 0.038570 for 4600 Fo > 4sig(Fo) and 0.044396 for all 5054 data REM 251 parameters refined using 16 restraints END WGHT 0.0025 7.4275 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.514, deepest hole -2.704, 1-sigma level 0.106 Q1 1 1.1502 0.6885 0.6923 11.00000 0.05 1.51 Q2 1 0.1705 0.5588 0.4601 11.00000 0.05 1.15 Q3 1 0.8069 0.6915 0.5921 11.00000 0.05 0.86 Q4 1 0.8424 0.6856 0.4792 11.00000 0.05 0.80 Q5 1 0.5227 0.7140 0.4173 11.00000 0.05 0.68 Q6 1 0.5175 0.6695 0.3522 11.00000 0.05 0.64 Q7 1 0.7477 0.6905 0.4590 11.00000 0.05 0.61 Q8 1 0.8549 0.5514 1.0870 11.00000 0.05 0.56 Q9 1 0.9290 0.6826 0.6195 11.00000 0.05 0.55 Q10 1 0.5387 0.7136 0.3715 11.00000 0.05 0.54 Q11 1 0.7635 0.5494 1.0177 11.00000 0.05 0.52 Q12 1 0.9098 0.5645 1.0716 11.00000 0.05 0.52 Q13 1 0.4504 0.6680 0.3661 11.00000 0.05 0.49 Q14 1 0.5742 0.6748 0.4307 11.00000 0.05 0.48 Q15 1 0.7776 0.5868 1.0041 11.00000 0.05 0.48 Q16 1 0.8023 0.5650 0.9798 11.00000 0.05 0.42 Q17 1 0.8794 0.7315 0.5688 11.00000 0.05 0.41 Q18 1 0.8668 0.5941 1.0616 11.00000 0.05 0.41 Q19 1 0.4886 0.5609 0.8835 11.00000 0.05 0.41 Q20 1 0.3250 0.6178 0.4900 11.00000 0.05 0.40 Q21 1 0.8471 0.6426 0.5445 11.00000 0.05 0.40 Q22 1 0.8341 0.5320 1.0206 11.00000 0.05 0.39 Q23 1 0.3490 0.7779 0.6179 11.00000 0.05 0.39 Q24 1 0.4505 0.7042 0.3329 11.00000 0.05 0.38 Q25 1 0.3803 0.7229 0.6382 11.00000 0.05 0.37 ; _shelx_res_checksum 72801 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Gd1 Gd 0.83091(2) 0.68815(2) 0.53896(2) 0.01488(6) Uani 1 1 d . . . . . N1 N 0.4135(3) 0.62275(15) 0.6501(3) 0.0127(7) Uani 1 1 d . . . . . C1 C 0.3874(5) 0.8757(2) 0.6037(4) 0.0278(10) Uani 1 1 d . . . . . H1 H 0.499640 0.879638 0.656412 0.042 Uiso 1 1 calc R U . . . H11 H 0.342043 0.915513 0.610474 0.042 Uiso 1 1 calc R U . . . H10 H 0.351268 0.871688 0.524146 0.042 Uiso 1 1 calc R U . . . B1 B 0.7092(6) 0.5790(2) 0.5304(4) 0.0218(10) Uani 1 1 d D . . . . H1B H 0.735(5) 0.6150(19) 0.600(3) 0.033 Uiso 1 1 d D U . . . H2B H 0.823(3) 0.572(2) 0.546(4) 0.033 Uiso 1 1 d D U . . . H3B H 0.653(5) 0.5303(14) 0.528(4) 0.033 Uiso 1 1 d D U . . . H4B H 0.633(4) 0.610(2) 0.447(3) 0.033 Uiso 1 1 d D U . . . C2 C 0.3401(5) 0.8143(2) 0.6346(4) 0.0233(8) Uani 1 1 d . . . . . H9 H 0.226669 0.810970 0.582129 0.028 Uiso 1 1 calc R U . . . H12 H 0.375103 0.818910 0.714422 0.028 Uiso 1 1 calc R U . . . B2 B 0.6470(6) 0.7812(3) 0.4959(4) 0.0250(11) Uani 1 1 d D . . . . H5B H 0.687(5) 0.747(2) 0.573(3) 0.038 Uiso 1 1 d D U . . . H6B H 0.597(5) 0.747(2) 0.418(3) 0.038 Uiso 1 1 d D U . . . H7B H 0.760(3) 0.800(2) 0.518(4) 0.038 Uiso 1 1 d D U . . . H8B H 0.565(4) 0.8235(17) 0.476(4) 0.038 Uiso 1 1 d D U . . . C3 C 0.4074(5) 0.75015(19) 0.6257(3) 0.0165(8) Uani 1 1 d . . . . . H13 H 0.376877 0.746211 0.547020 0.020 Uiso 1 1 calc R U . . . H8 H 0.520903 0.751836 0.681472 0.020 Uiso 1 1 calc R U . . . B3 B 0.8697(6) 0.6852(3) 0.3870(5) 0.0320(11) Uani 1 1 d D . . . . H9B H 0.902(6) 0.7339(16) 0.438(4) 0.048 Uiso 1 1 d D U . . . H10B H 0.746(3) 0.677(3) 0.355(4) 0.048 Uiso 1 1 d D U . . . H11B H 0.942(5) 0.647(2) 0.459(3) 0.048 Uiso 1 1 d D U . . . H12B H 0.887(5) 0.683(3) 0.319(3) 0.048 Uiso 1 1 d D U . . . C4 C 0.3495(4) 0.69001(19) 0.6510(3) 0.0158(7) Uani 1 1 d . . . . . H15 H 0.236113 0.688568 0.593252 0.019 Uiso 1 1 calc R U . . . H14 H 0.375162 0.696264 0.727844 0.019 Uiso 1 1 calc R U . . . B4 B 1.0876(6) 0.7011(2) 0.7359(4) 0.0250(11) Uani 1 1 d D . . . . H13B H 0.986(4) 0.711(2) 0.736(4) 0.037 Uiso 1 1 d D U . . . H14B H 1.067(5) 0.6492(14) 0.694(4) 0.037 Uiso 1 1 d D U . . . H15B H 1.070(5) 0.7379(19) 0.668(3) 0.037 Uiso 1 1 d D U . . . H16B H 1.208(3) 0.706(2) 0.822(2) 0.037 Uiso 1 1 d D U . . . C5 C 0.4006(4) 0.61510(19) 0.5421(3) 0.0141(8) Uani 1 1 d . . . . . H7 H 0.448764 0.572152 0.547094 0.017 Uiso 1 1 calc R U . . . H6 H 0.460590 0.651341 0.541156 0.017 Uiso 1 1 calc R U . . . C6 C 0.2388(4) 0.6167(2) 0.4284(3) 0.0178(8) Uani 1 1 d . . . . . H34 H 0.183797 0.656687 0.425337 0.021 Uiso 1 1 calc R U . . . H35 H 0.181559 0.576455 0.421563 0.021 Uiso 1 1 calc R U . . . C7 C 0.2480(5) 0.6185(2) 0.3290(3) 0.0196(8) Uani 1 1 d . . . . . H4 H 0.287571 0.662647 0.327911 0.024 Uiso 1 1 calc R U . . . H5 H 0.320874 0.583888 0.341838 0.024 Uiso 1 1 calc R U . . . C8 C 0.0913(5) 0.6065(2) 0.2129(3) 0.0246(9) Uani 1 1 d . . . . . H36 H 0.057339 0.560803 0.210525 0.037 Uiso 1 1 calc R U . . . H2 H 0.099023 0.612365 0.150693 0.037 Uiso 1 1 calc R U . . . H3 H 0.016918 0.638438 0.202862 0.037 Uiso 1 1 calc R U . . . C9 C 0.5830(4) 0.61921(19) 0.7544(3) 0.0141(8) Uani 1 1 d . . . . . H24 H 0.638752 0.653971 0.745748 0.017 Uiso 1 1 calc R U . . . H16 H 0.593194 0.630272 0.824310 0.017 Uiso 1 1 calc R U . . . C10 C 0.6608(4) 0.55221(18) 0.7738(3) 0.0164(8) Uani 1 1 d . . . . . H23 H 0.663013 0.542814 0.708932 0.020 Uiso 1 1 calc R U . . . H22 H 0.601759 0.516182 0.776352 0.020 Uiso 1 1 calc R U . . . C11 C 0.8250(4) 0.5534(2) 0.8874(3) 0.0208(9) Uani 1 1 d . . . . . H21 H 0.822755 0.570388 0.949370 0.025 Uiso 1 1 calc R U . . . H20 H 0.864880 0.507033 0.907749 0.025 Uiso 1 1 calc R U . . . C12 C 0.9346(5) 0.5963(2) 0.8832(4) 0.0260(10) Uani 1 1 d . . . . . H18 H 0.934283 0.581064 0.819854 0.039 Uiso 1 1 calc R U . . . H17 H 1.038591 0.592290 0.956483 0.039 Uiso 1 1 calc R U . . . H19 H 0.901578 0.643069 0.870446 0.039 Uiso 1 1 calc R U . . . C13 C 0.3229(4) 0.56692(19) 0.6527(3) 0.0163(8) Uani 1 1 d . . . . . H33 H 0.348309 0.524516 0.633362 0.020 Uiso 1 1 calc R U . . . H32 H 0.212240 0.575597 0.591020 0.020 Uiso 1 1 calc R U . . . C14 C 0.3477(4) 0.5568(2) 0.7655(3) 0.0169(8) Uani 1 1 d . . . . . H31 H 0.456323 0.544874 0.827831 0.020 Uiso 1 1 calc R U . . . H30 H 0.324556 0.598748 0.787638 0.020 Uiso 1 1 calc R U . . . C15 C 0.2432(5) 0.5012(2) 0.7504(4) 0.0224(9) Uani 1 1 d . . . . . H25 H 0.259278 0.460914 0.719967 0.027 Uiso 1 1 calc R U . . . H26 H 0.134896 0.515283 0.692736 0.027 Uiso 1 1 calc R U . . . C16 C 0.2718(6) 0.4832(3) 0.8625(4) 0.0348(11) Uani 1 1 d . . . . . H27 H 0.380010 0.471179 0.921118 0.052 Uiso 1 1 calc R U . . . H29 H 0.206799 0.445157 0.849172 0.052 Uiso 1 1 calc R U . . . H28 H 0.246849 0.521630 0.889372 0.052 Uiso 1 1 calc R U . . . 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 Gd1 0.01259(9) 0.01424(9) 0.01677(9) 0.00124(9) 0.00859(7) 0.00005(9) N1 0.0118(16) 0.0122(16) 0.0144(16) -0.0016(13) 0.0082(14) -0.0002(12) C1 0.026(2) 0.013(2) 0.036(3) -0.0007(19) 0.015(2) 0.0002(17) B1 0.021(2) 0.019(2) 0.028(3) -0.003(2) 0.016(2) -0.0031(19) C2 0.028(2) 0.0160(19) 0.031(2) 0.0017(19) 0.0206(19) 0.0053(19) B2 0.026(3) 0.024(2) 0.021(2) 0.001(2) 0.013(2) 0.004(2) C3 0.017(2) 0.0140(19) 0.0166(19) 0.0000(16) 0.0094(17) 0.0012(16) B3 0.030(3) 0.041(3) 0.030(3) 0.003(3) 0.021(2) 0.000(3) C4 0.0153(18) 0.0135(17) 0.0185(18) -0.0005(17) 0.0105(16) 0.0031(16) B4 0.021(2) 0.019(3) 0.028(3) -0.002(2) 0.012(2) 0.0001(19) C5 0.0145(19) 0.0138(18) 0.0153(19) -0.0011(15) 0.0099(16) -0.0003(15) C6 0.017(2) 0.017(2) 0.017(2) -0.0009(16) 0.0090(17) 0.0017(16) C7 0.019(2) 0.021(2) 0.017(2) -0.0001(17) 0.0098(18) -0.0004(17) C8 0.026(2) 0.027(2) 0.016(2) -0.0009(18) 0.0106(19) -0.0038(18) C9 0.0095(18) 0.0152(19) 0.0124(18) -0.0001(15) 0.0042(16) 0.0003(14) C10 0.0148(19) 0.0119(19) 0.019(2) 0.0051(15) 0.0086(17) 0.0026(15) C11 0.018(2) 0.021(2) 0.018(2) 0.0039(17) 0.0089(17) 0.0046(17) C12 0.015(2) 0.028(2) 0.022(2) 0.0042(18) 0.0053(18) 0.0019(18) C13 0.0143(18) 0.0128(18) 0.0197(19) -0.0029(16) 0.0096(16) -0.0020(15) C14 0.0157(19) 0.0174(19) 0.0184(19) 0.0018(16) 0.0110(17) -0.0010(16) C15 0.022(2) 0.020(2) 0.027(2) -0.0001(18) 0.0161(19) -0.0027(17) C16 0.040(3) 0.037(3) 0.036(3) 0.002(2) 0.028(2) -0.011(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 B4 Gd1 B1 109.43(16) . . ? B4 Gd1 B3 109.39(17) . . ? B1 Gd1 B3 108.32(18) . . ? B4 Gd1 B2 111.87(16) . . ? B1 Gd1 B2 107.43(17) . . ? B3 Gd1 B2 110.31(18) . . ? B4 Gd1 H1B 94.6(10) . . ? B1 Gd1 H1B 26.7(5) . . ? B3 Gd1 H1B 135.0(5) . . ? B2 Gd1 H1B 93.9(10) . . ? B4 Gd1 H2B 95.6(10) . . ? B1 Gd1 H2B 26.7(5) . . ? B3 Gd1 H2B 92.8(9) . . ? B2 Gd1 H2B 134.1(5) . . ? H1B Gd1 H2B 46.2(10) . . ? B4 Gd1 H4B 136.4(5) . . ? B1 Gd1 H4B 27.0(5) . . ? B3 Gd1 H4B 94.9(10) . . ? B2 Gd1 H4B 91.4(9) . . ? H1B Gd1 H4B 45.7(10) . . ? H2B Gd1 H4B 46.1(10) . . ? B4 Gd1 H5B 97.9(10) . . ? B1 Gd1 H5B 92.0(10) . . ? B3 Gd1 H5B 137.2(5) . . ? B2 Gd1 H5B 27.0(5) . . ? H1B Gd1 H5B 71.7(12) . . ? H2B Gd1 H5B 117.2(11) . . ? H4B Gd1 H5B 86.6(16) . . ? B4 Gd1 H6B 138.5(5) . . ? B1 Gd1 H6B 95.1(10) . . ? B3 Gd1 H6B 93.0(9) . . ? B2 Gd1 H6B 26.8(5) . . ? H1B Gd1 H6B 93.0(16) . . ? H2B Gd1 H6B 118.4(12) . . ? H4B Gd1 H6B 72.2(11) . . ? H5B Gd1 H6B 46.8(10) . . ? B4 Gd1 H7B 95.8(9) . . ? B1 Gd1 H7B 134.1(5) . . ? B3 Gd1 H7B 97.8(10) . . ? B2 Gd1 H7B 26.7(5) . . ? H1B Gd1 H7B 117.5(11) . . ? H2B Gd1 H7B 160.8(7) . . ? H4B Gd1 H7B 116.6(10) . . ? H5B Gd1 H7B 45.8(10) . . ? H6B Gd1 H7B 45.4(10) . . ? B4 Gd1 H9B 96.4(12) . . ? B1 Gd1 H9B 135.2(5) . . ? B3 Gd1 H9B 26.9(5) . . ? B2 Gd1 H9B 95.3(11) . . ? H1B Gd1 H9B 161.9(7) . . ? H2B Gd1 H9B 118.2(11) . . ? H4B Gd1 H9B 118.5(12) . . ? H5B Gd1 H9B 120.7(12) . . ? H6B Gd1 H9B 88.2(17) . . ? H7B Gd1 H9B 75.7(12) . . ? B4 Gd1 H10B 136.4(5) . . ? B1 Gd1 H10B 92.6(11) . . ? B3 Gd1 H10B 27.0(5) . . ? B2 Gd1 H10B 95.6(11) . . ? H1B Gd1 H10B 117.4(12) . . ? H2B Gd1 H10B 87.7(17) . . ? H4B Gd1 H10B 72.4(12) . . ? H5B Gd1 H10B 119.0(12) . . ? H6B Gd1 H10B 72.2(12) . . ? H7B Gd1 H10B 94.5(17) . . ? H9B Gd1 H10B 46.1(12) . . ? B4 Gd1 H11B 92.5(10) . . ? B1 Gd1 H11B 95.7(11) . . ? B3 Gd1 H11B 27.0(5) . . ? B2 Gd1 H11B 137.3(5) . . ? H1B Gd1 H11B 119.4(12) . . ? H2B Gd1 H11B 73.3(12) . . ? H4B Gd1 H11B 94.0(17) . . ? H5B Gd1 H11B 164.2(7) . . ? H6B Gd1 H11B 118.5(10) . . ? H7B Gd1 H11B 121.4(12) . . ? H9B Gd1 H11B 45.8(11) . . ? H10B Gd1 H11B 46.9(11) . . ? B4 Gd1 H13B 26.9(5) . . ? B1 Gd1 H13B 101.0(11) . . ? B3 Gd1 H13B 135.2(6) . . ? B2 Gd1 H13B 91.6(8) . . ? H1B Gd1 H13B 78.4(12) . . ? H2B Gd1 H13B 99.1(16) . . ? H4B Gd1 H13B 124.1(12) . . ? H5B Gd1 H13B 72.6(11) . . ? H6B Gd1 H13B 117.7(9) . . ? H7B Gd1 H13B 84.5(15) . . ? H9B Gd1 H13B 116.8(13) . . ? H10B Gd1 H13B 162.0(9) . . ? H11B Gd1 H13B 119.1(11) . . ? B4 Gd1 H14B 27.1(5) . . ? B1 Gd1 H14B 90.0(9) . . ? B3 Gd1 H14B 99.3(11) . . ? B2 Gd1 H14B 137.8(6) . . ? H1B Gd1 H14B 84.9(16) . . ? H2B Gd1 H14B 70.7(11) . . ? H4B Gd1 H14B 115.7(10) . . ? H5B Gd1 H14B 118.5(12) . . ? H6B Gd1 H14B 164.5(9) . . ? H7B Gd1 H14B 122.7(10) . . ? H9B Gd1 H14B 98.5(18) . . ? H10B Gd1 H14B 122.3(13) . . ? H11B Gd1 H14B 75.4(12) . . ? H13B Gd1 H14B 46.8(10) . . ? B4 Gd1 H15B 27.2(5) . . ? B1 Gd1 H15B 135.5(6) . . ? B3 Gd1 H15B 90.2(9) . . ? B2 Gd1 H15B 102.9(11) . . ? H1B Gd1 H15B 121.4(11) . . ? H2B Gd1 H15B 116.5(12) . . ? H4B Gd1 H15B 162.1(9) . . ? H5B Gd1 H15B 101.3(17) . . ? H6B Gd1 H15B 124.7(12) . . ? H7B Gd1 H15B 79.5(12) . . ? H9B Gd1 H15B 71.4(12) . . ? H10B Gd1 H15B 116.1(10) . . ? H11B Gd1 H15B 82.8(17) . . ? H13B Gd1 H15B 46.0(11) . . ? H14B Gd1 H15B 46.4(10) . . ? C5 N1 C13 108.6(3) . . ? C5 N1 C9 108.1(3) . . ? C13 N1 C9 111.2(3) . . ? C5 N1 C4 110.9(3) . . ? C13 N1 C4 109.2(3) . . ? C9 N1 C4 108.8(3) . . ? C2 C1 H1 109.5 . . ? C2 C1 H11 109.5 . . ? H1 C1 H11 109.5 . . ? C2 C1 H10 109.5 . . ? H1 C1 H10 109.5 . . ? H11 C1 H10 109.5 . . ? Gd1 B1 H1B 65(2) . . ? Gd1 B1 H2B 67(2) . . ? H1B B1 H2B 106(3) . . ? Gd1 B1 H3B 178(2) . . ? H1B B1 H3B 113(3) . . ? H2B B1 H3B 114(3) . . ? Gd1 B1 H4B 67(2) . . ? H1B B1 H4B 104(3) . . ? H2B B1 H4B 106(3) . . ? H3B B1 H4B 113(3) . . ? C1 C2 C3 112.1(3) . . ? C1 C2 H9 109.2 . . ? C3 C2 H9 109.2 . . ? C1 C2 H12 109.2 . . ? C3 C2 H12 109.2 . . ? H9 C2 H12 107.9 . . ? Gd1 B2 H5B 64(2) . . ? Gd1 B2 H6B 68(2) . . ? H5B B2 H6B 107(3) . . ? Gd1 B2 H7B 66(2) . . ? H5B B2 H7B 103(3) . . ? H6B B2 H7B 104(3) . . ? Gd1 B2 H8B 179(2) . . ? H5B B2 H8B 117(3) . . ? H6B B2 H8B 112(3) . . ? H7B B2 H8B 113(3) . . ? C4 C3 C2 109.9(3) . . ? C4 C3 H13 109.7 . . ? C2 C3 H13 109.7 . . ? C4 C3 H8 109.7 . . ? C2 C3 H8 109.7 . . ? H13 C3 H8 108.2 . . ? Gd1 B3 H9B 63(3) . . ? Gd1 B3 H10B 63(2) . . ? H9B B3 H10B 101(4) . . ? Gd1 B3 H11B 66(3) . . ? H9B B3 H11B 102(3) . . ? H10B B3 H11B 105(4) . . ? Gd1 B3 H12B 179(3) . . ? H9B B3 H12B 118(4) . . ? H10B B3 H12B 116(3) . . ? H11B B3 H12B 113(4) . . ? C3 C4 N1 115.2(3) . . ? C3 C4 H15 108.5 . . ? N1 C4 H15 108.5 . . ? C3 C4 H14 108.5 . . ? N1 C4 H14 108.5 . . ? H15 C4 H14 107.5 . . ? Gd1 B4 H13B 67(2) . . ? Gd1 B4 H14B 66(2) . . ? H13B B4 H14B 106(3) . . ? Gd1 B4 H15B 67(2) . . ? H13B B4 H15B 104(3) . . ? H14B B4 H15B 104(3) . . ? Gd1 B4 H16B 176(2) . . ? H13B B4 H16B 117(3) . . ? H14B B4 H16B 112(3) . . ? H15B B4 H16B 112(3) . . ? N1 C5 C6 115.9(3) . . ? N1 C5 H7 108.3 . . ? C6 C5 H7 108.3 . . ? N1 C5 H6 108.3 . . ? C6 C5 H6 108.3 . . ? H7 C5 H6 107.4 . . ? C5 C6 C7 108.9(3) . . ? C5 C6 H34 109.9 . . ? C7 C6 H34 109.9 . . ? C5 C6 H35 109.9 . . ? C7 C6 H35 109.9 . . ? H34 C6 H35 108.3 . . ? C8 C7 C6 111.5(3) . . ? C8 C7 H4 109.3 . . ? C6 C7 H4 109.3 . . ? C8 C7 H5 109.3 . . ? C6 C7 H5 109.3 . . ? H4 C7 H5 108.0 . . ? C7 C8 H36 109.5 . . ? C7 C8 H2 109.5 . . ? H36 C8 H2 109.5 . . ? C7 C8 H3 109.5 . . ? H36 C8 H3 109.5 . . ? H2 C8 H3 109.5 . . ? C10 C9 N1 115.6(3) . . ? C10 C9 H24 108.4 . . ? N1 C9 H24 108.4 . . ? C10 C9 H16 108.4 . . ? N1 C9 H16 108.4 . . ? H24 C9 H16 107.4 . . ? C9 C10 C11 110.1(3) . . ? C9 C10 H23 109.6 . . ? C11 C10 H23 109.6 . . ? C9 C10 H22 109.6 . . ? C11 C10 H22 109.6 . . ? H23 C10 H22 108.2 . . ? C12 C11 C10 113.8(3) . . ? C12 C11 H21 108.8 . . ? C10 C11 H21 108.8 . . ? C12 C11 H20 108.8 . . ? C10 C11 H20 108.8 . . ? H21 C11 H20 107.7 . . ? C11 C12 H18 109.5 . . ? C11 C12 H17 109.5 . . ? H18 C12 H17 109.5 . . ? C11 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? N1 C13 C14 116.8(3) . . ? N1 C13 H33 108.1 . . ? C14 C13 H33 108.1 . . ? N1 C13 H32 108.1 . . ? C14 C13 H32 108.1 . . ? H33 C13 H32 107.3 . . ? C15 C14 C13 109.4(3) . . ? C15 C14 H31 109.8 . . ? C13 C14 H31 109.8 . . ? C15 C14 H30 109.8 . . ? C13 C14 H30 109.8 . . ? H31 C14 H30 108.2 . . ? C14 C15 C16 112.8(3) . . ? C14 C15 H25 109.0 . . ? C16 C15 H25 109.0 . . ? C14 C15 H26 109.0 . . ? C16 C15 H26 109.0 . . ? H25 C15 H26 107.8 . . ? C15 C16 H27 109.5 . . ? C15 C16 H29 109.5 . . ? H27 C16 H29 109.5 . . ? C15 C16 H28 109.5 . . ? H27 C16 H28 109.5 . . ? H29 C16 H28 109.5 . . ? 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 Gd1 B4 2.522(5) . ? Gd1 B1 2.529(5) . ? Gd1 B3 2.532(5) . ? Gd1 B2 2.533(5) . ? Gd1 H1B 2.30(5) . ? Gd1 H2B 2.33(4) . ? Gd1 H4B 2.33(4) . ? Gd1 H5B 2.28(5) . ? Gd1 H6B 2.36(5) . ? Gd1 H7B 2.32(5) . ? Gd1 H9B 2.26(5) . ? Gd1 H10B 2.26(5) . ? Gd1 H11B 2.32(5) . ? Gd1 H13B 2.32(5) . ? Gd1 H14B 2.30(5) . ? Gd1 H15B 2.32(5) . ? N1 C5 1.515(5) . ? N1 C13 1.519(5) . ? N1 C9 1.524(5) . ? N1 C4 1.525(5) . ? C1 C2 1.512(6) . ? C1 H1 0.9800 . ? C1 H11 0.9800 . ? C1 H10 0.9800 . ? B1 H1B 1.138(19) . ? B1 H2B 1.140(19) . ? B1 H3B 1.143(19) . ? B1 H4B 1.150(19) . ? C2 C3 1.529(5) . ? C2 H9 0.9900 . ? C2 H12 0.9900 . ? B2 H5B 1.150(19) . ? B2 H6B 1.146(19) . ? B2 H7B 1.141(19) . ? B2 H8B 1.141(19) . ? C3 C4 1.515(5) . ? C3 H13 0.9900 . ? C3 H8 0.9900 . ? B3 H9B 1.146(19) . ? B3 H10B 1.151(19) . ? B3 H11B 1.151(19) . ? B3 H12B 1.138(19) . ? C4 H15 0.9900 . ? C4 H14 0.9900 . ? B4 H13B 1.142(19) . ? B4 H14B 1.152(19) . ? B4 H15B 1.154(19) . ? B4 H16B 1.144(19) . ? C5 C6 1.518(5) . ? C5 H7 0.9900 . ? C5 H6 0.9900 . ? C6 C7 1.532(5) . ? C6 H34 0.9900 . ? C6 H35 0.9900 . ? C7 C8 1.524(5) . ? C7 H4 0.9900 . ? C7 H5 0.9900 . ? C8 H36 0.9800 . ? C8 H2 0.9800 . ? C8 H3 0.9800 . ? C9 C10 1.522(5) . ? C9 H24 0.9900 . ? C9 H16 0.9900 . ? C10 C11 1.531(5) . ? C10 H23 0.9900 . ? C10 H22 0.9900 . ? C11 C12 1.520(6) . ? C11 H21 0.9900 . ? C11 H20 0.9900 . ? C12 H18 0.9800 . ? C12 H17 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.522(5) . ? C13 H33 0.9900 . ? C13 H32 0.9900 . ? C14 C15 1.520(5) . ? C14 H31 0.9900 . ? C14 H30 0.9900 . ? C15 C16 1.521(6) . ? C15 H25 0.9900 . ? C15 H26 0.9900 . ? C16 H27 0.9800 . ? C16 H29 0.9800 . ? C16 H28 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -176.9(3) . . . . ? C2 C3 C4 N1 -177.5(3) . . . . ? C5 N1 C4 C3 -49.1(4) . . . . ? C13 N1 C4 C3 -168.8(3) . . . . ? C9 N1 C4 C3 69.7(4) . . . . ? C13 N1 C5 C6 58.6(4) . . . . ? C9 N1 C5 C6 179.4(3) . . . . ? C4 N1 C5 C6 -61.4(4) . . . . ? N1 C5 C6 C7 171.9(3) . . . . ? C5 C6 C7 C8 168.9(3) . . . . ? C5 N1 C9 C10 -65.7(4) . . . . ? C13 N1 C9 C10 53.5(4) . . . . ? C4 N1 C9 C10 173.7(3) . . . . ? N1 C9 C10 C11 -174.3(3) . . . . ? C9 C10 C11 C12 -71.8(4) . . . . ? C5 N1 C13 C14 167.7(3) . . . . ? C9 N1 C13 C14 48.8(4) . . . . ? C4 N1 C13 C14 -71.2(4) . . . . ? N1 C13 C14 C15 177.6(3) . . . . ? C13 C14 C15 C16 174.5(4) . . . . ?