#------------------------------------------------------------------------------ #$Date: 2024-10-20 01:10:19 +0300 (Sun, 20 Oct 2024) $ #$Revision: 295550 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572901.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_1572901 loop_ _publ_author_name 'Pedussaut, Lucie' 'Mahieu, Nolwenn' 'Chartier, Camille' 'Rajeshkumar, Thayalan' 'Tricoire, Maxime' 'Douair, Iskander' 'Casaretto, Nicolas' 'Maron, Laurent' 'Danoun, Gr\'egory' 'Nocton, Gr\'egory' _publ_section_title ; The photo-isomerization of the cyclononatetraenyl ligand and related rare earth complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04767B _journal_year 2024 _chemical_formula_moiety '3.204(C5.305 H5.305), Nd' _chemical_formula_sum 'C17 H17 Nd' _chemical_formula_weight 365.54 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2020-07-08 _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _audit_update_record ; 2024-07-13 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0748(18) _cell_length_b 12.8129(19) _cell_length_c 8.8427(14) _cell_measurement_reflns_used 1474 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 21.855 _cell_measurement_theta_min 2.855 _cell_volume 1368.1(4) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1464 _diffrn_reflns_av_unetI/netI 0.0698 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 28912 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.673 _diffrn_reflns_theta_min 2.799 _diffrn_source_current 31.0 _diffrn_source_power 1.705 _diffrn_source_voltage 55.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.773 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.6230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1009 before and 0.0765 after correction. The Ratio of minimum to maximum transmission is 0.8353. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.775 _exptl_crystal_description needle _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.961 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.196 _refine_ls_extinction_coef 0.0039(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 169 _refine_ls_number_reflns 1986 _refine_ls_number_restraints 110 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.8743P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.1087 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1036 _reflns_number_total 1986 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04767b3.cif _cod_data_source_block 2-Nd-cis _cod_database_code 1572901 _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_max 0.928 _shelx_estimated_absorpt_t_min 0.465 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim C5A-C5A_$1 with sigma of 0.02 C1B-C2B \\sim C2B-C3B \\sim C3B-C4B \\sim C4B-C5B \\sim C5B-C5B_$1 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C6A \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C6B \\sim C7B \\sim C8B \\sim C9B \\sim C9B \\sim C10B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A 4. Others Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=1- FVAR(1) Sof(C1B)=Sof(H1B)=0.5*(1-FVAR(2)) Sof(C1A)=Sof(H1A)=0.5*FVAR(2) Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=FVAR(1) Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=1-FVAR(2) Sof(C6B)=Sof(H6B)=Sof(C10B)=Sof(H10B)=0.5*(1-FVAR(3)) Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=FVAR(2) 5.a Aromatic/amide H refined with riding coordinates: C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A) ; _shelx_res_file ; TITL nm023_0m P 1 R = 0.14 New:Pnma nm023_0m_pl.res created by SHELXL-2018/3 at 17:50:25 on 08-Jul-2020 CELL 0.71073 12.0748 12.8129 8.8427 90 90 90 ZERR 4 0.0018 0.0019 0.0014 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM -X,0.5+Y,-Z SFAC C H Nd UNIT 68 68 4 EQIV $1 +X,1.5-Y,+Z SADI C1A C2A C2A C3A C3A C4A C4A C5A C5A C5A_$1 SADI C1B C2B C2B C3B C3B C4B C4B C5B C5B C5B_$1 SIMU 0.004 0.008 2 C1A > C5A SIMU 0.004 0.008 2 C1B > C5B SIMU 0.004 0.008 2 C6A > C9A SIMU 0.004 0.008 2 C6B C7B C8B C9B C9B C10B L.S. 5 PLAN 30 SIZE 0.24 0.03 0.02 TEMP -123 CONF CONN 0 $Nd MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.046000 0.874300 EXTI 0.003933 FVAR 0.10150 0.58946 0.63721 PART 1 C1A 1 0.617549 0.750000 0.318295 20.50000 0.02364 0.04016 = 0.01896 0.00000 -0.00386 0.00000 AFIX 43 H1A 2 0.558211 0.749999 0.388839 20.50000 -1.20000 AFIX 0 C2A 1 0.645549 0.647380 0.285009 21.00000 0.02412 0.04025 = 0.02311 0.00042 -0.00463 0.00446 AFIX 43 H2A 2 0.602528 0.600195 0.343461 21.00000 -1.20000 AFIX 0 C3A 1 0.718651 0.593191 0.190478 21.00000 0.02316 0.04190 = 0.02681 0.00113 -0.00317 0.00482 AFIX 43 H3A 2 0.713220 0.520292 0.208624 21.00000 -1.20000 AFIX 0 C4A 1 0.796977 0.612683 0.077978 21.00000 0.02104 0.04594 = 0.02966 0.00039 -0.00049 0.00745 AFIX 43 H4A 2 0.826691 0.548726 0.041820 21.00000 -1.20000 AFIX 0 C5A 1 0.845273 0.695967 0.002100 21.00000 0.01975 0.05085 = 0.03361 0.00136 -0.00235 0.00756 AFIX 43 H5A 2 0.893803 0.670731 -0.074145 21.00000 -1.20000 AFIX 0 PART 2 C1B 1 0.852068 0.750000 -0.016639 -20.50000 0.02622 0.03319 = 0.03141 0.00000 -0.00214 0.00000 AFIX 43 H1B 2 0.901827 0.750000 -0.099856 -20.50000 -1.20000 AFIX 0 C2B 1 0.826508 0.649346 0.026109 -21.00000 0.02728 0.03372 = 0.03122 0.00640 -0.00270 0.00069 AFIX 43 H2B 2 0.869721 0.601150 -0.030309 -21.00000 -1.20000 AFIX 0 C3B 1 0.758012 0.596295 0.124935 -21.00000 0.02940 0.03862 = 0.03131 0.01178 -0.00560 0.00343 AFIX 43 H3B 2 0.767421 0.523129 0.113221 -21.00000 -1.20000 AFIX 0 C4B 1 0.680153 0.616633 0.235404 -21.00000 0.02956 0.04177 = 0.02902 0.01543 -0.00546 0.00341 AFIX 43 H4B 2 0.654402 0.552211 0.275301 -21.00000 -1.20000 AFIX 0 C5B 1 0.626885 0.696422 0.307870 -21.00000 0.03159 0.04445 = 0.02803 0.01748 -0.00559 0.00162 AFIX 43 H5B 2 0.574783 0.670089 0.378751 -21.00000 -1.20000 AFIX 0 PART 4 C6B 1 0.399941 0.750000 -0.014902 -30.50000 0.02192 0.02210 = 0.02491 0.00000 -0.00264 0.00000 AFIX 43 H6B 2 0.345643 0.750000 0.062844 -30.50000 -1.20000 AFIX 0 C7B 1 0.427556 0.646370 -0.054440 -31.00000 0.02183 0.02130 = 0.02467 -0.00030 -0.00307 -0.00324 AFIX 43 H7B 2 0.385587 0.593936 -0.004589 -31.00000 -1.20000 AFIX 0 C8B 1 0.510130 0.607903 -0.159427 -31.00000 0.02128 0.02112 = 0.02125 -0.00128 -0.00066 -0.00065 AFIX 43 H8B 2 0.512992 0.533814 -0.158092 -31.00000 -1.20000 AFIX 0 C9B 1 0.585170 0.647769 -0.259952 -31.00000 0.02006 0.02273 = 0.01629 -0.00287 0.00193 0.00094 AFIX 43 H9B 2 0.623920 0.594696 -0.313132 -31.00000 -1.20000 AFIX 0 C10B 1 0.619126 0.750000 -0.303990 -30.50000 0.01848 0.02295 = 0.01215 0.00000 0.00475 0.00000 AFIX 43 H10B 2 0.676175 0.750000 -0.377973 -30.50000 -1.20000 AFIX 0 PART 3 C6A 1 0.404624 0.693557 -0.031079 31.00000 0.02556 0.04538 = 0.02612 0.00809 -0.00416 -0.01391 AFIX 43 H6A 2 0.351994 0.664409 0.036695 31.00000 -1.20000 AFIX 0 C7A 1 0.466227 0.617293 -0.110413 31.00000 0.02575 0.03964 = 0.02465 0.00781 -0.00604 -0.01449 AFIX 43 H7A 2 0.442747 0.548473 -0.086532 31.00000 -1.20000 AFIX 0 C8A 1 0.553307 0.617676 -0.215530 31.00000 0.02747 0.03832 = 0.02434 0.00574 -0.00661 -0.01119 AFIX 43 H8A 2 0.575768 0.549038 -0.242168 31.00000 -1.20000 AFIX 0 C9A 1 0.614896 0.693330 -0.290396 31.00000 0.02784 0.04108 = 0.02207 0.00357 -0.00686 -0.00980 AFIX 43 H9A 2 0.669035 0.664499 -0.356209 31.00000 -1.20000 AFIX 0 PART 0 ND1 3 0.615614 0.750000 -0.003081 10.50000 0.02007 0.03289 = 0.02102 0.00000 -0.00075 0.00000 HKLF 4 1 0 1 0 0 0 1 1 0 0 REM nm023_0m P 1 R = 0.14 New:Pnma REM wR2 = 0.1087, GooF = S = 1.022, Restrained GooF = 1.001 for all data REM R1 = 0.0389 for 1036 Fo > 4sig(Fo) and 0.1015 for all 1986 data REM 169 parameters refined using 110 restraints END WGHT 0.0461 0.8815 REM Highest difference peak 1.961, deepest hole -1.071, 1-sigma level 0.196 Q1 1 0.6501 0.7500 -0.5008 10.50000 0.05 1.96 Q2 1 0.5966 0.7022 0.5111 11.00000 0.05 0.77 Q3 1 0.8445 0.7500 -0.1592 10.50000 0.05 0.74 Q4 1 0.5953 0.7500 -0.4303 10.50000 0.05 0.72 Q5 1 0.8816 0.7500 0.0424 10.50000 0.05 0.68 Q6 1 0.3865 0.7500 0.2246 10.50000 0.05 0.67 Q7 1 0.4016 0.6529 -0.0041 11.00000 0.05 0.62 Q8 1 0.6083 0.7239 -0.3259 11.00000 0.05 0.62 Q9 1 0.6588 0.7112 -0.1358 11.00000 0.05 0.61 Q10 1 0.6659 0.6861 0.4300 11.00000 0.05 0.61 Q11 1 0.6437 0.6699 -0.4708 11.00000 0.05 0.61 Q12 1 0.5408 0.6925 0.0404 11.00000 0.05 0.60 Q13 1 0.5432 0.7012 -0.0629 11.00000 0.05 0.60 Q14 1 0.8441 0.7500 0.1610 10.50000 0.05 0.58 Q15 1 0.6348 0.6594 0.0615 11.00000 0.05 0.57 Q16 1 0.6603 0.7500 -0.0439 10.50000 0.05 0.56 Q17 1 0.5874 0.7500 -0.1559 10.50000 0.05 0.55 Q18 1 0.6514 0.6569 -0.0460 11.00000 0.05 0.55 Q19 1 0.8884 0.7108 0.1349 11.00000 0.05 0.55 Q20 1 0.5993 0.7014 0.2370 11.00000 0.05 0.54 Q21 1 0.8884 0.7104 -0.1288 11.00000 0.05 0.54 Q22 1 0.6693 0.7100 0.4061 11.00000 0.05 0.54 Q23 1 0.7016 0.7049 0.0202 11.00000 0.05 0.53 Q24 1 0.7374 0.7500 0.1043 10.50000 0.05 0.53 Q25 1 0.8806 0.7500 -0.0403 10.50000 0.05 0.52 Q26 1 0.6118 0.7232 0.3186 11.00000 0.05 0.52 Q27 1 0.4996 0.5915 -0.2302 11.00000 0.05 0.52 Q28 1 0.5829 0.7500 0.1471 10.50000 0.05 0.52 Q29 1 0.8198 0.6502 -0.0275 11.00000 0.05 0.51 Q30 1 0.8649 0.6289 0.1406 11.00000 0.05 0.51 ; _shelx_res_checksum 76202 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -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 C1A C 0.6175(17) 0.750000 0.318(2) 0.028(3) Uani 0.59(2) 2 d DS TU P A 1 H1A H 0.558211 0.749999 0.388839 0.033 Uiso 0.59(2) 2 calc R U P A 1 C2A C 0.6455(10) 0.6474(9) 0.2850(13) 0.029(3) Uani 0.59(2) 1 d D U P A 1 H2A H 0.602528 0.600195 0.343461 0.035 Uiso 0.59(2) 1 calc R U P A 1 C3A C 0.7187(9) 0.5932(10) 0.1905(12) 0.031(3) Uani 0.59(2) 1 d D U P A 1 H3A H 0.713220 0.520292 0.208624 0.037 Uiso 0.59(2) 1 calc R U P A 1 C4A C 0.7970(9) 0.6127(10) 0.0780(13) 0.032(3) Uani 0.59(2) 1 d D U P A 1 H4A H 0.826691 0.548726 0.041820 0.039 Uiso 0.59(2) 1 calc R U P A 1 C5A C 0.8453(9) 0.6960(5) 0.0021(17) 0.035(3) Uani 0.59(2) 1 d D U P A 1 H5A H 0.893803 0.670731 -0.074145 0.042 Uiso 0.59(2) 1 calc R U P A 1 C1B C 0.852(2) 0.750000 -0.017(3) 0.030(4) Uani 0.41(2) 2 d DS TU P A 2 H1B H 0.901827 0.750000 -0.099856 0.036 Uiso 0.41(2) 2 calc R U P A 2 C2B C 0.8265(13) 0.6493(11) 0.0261(19) 0.031(4) Uani 0.41(2) 1 d D U P A 2 H2B H 0.869721 0.601150 -0.030309 0.037 Uiso 0.41(2) 1 calc R U P A 2 C3B C 0.7580(13) 0.5963(14) 0.1249(18) 0.033(4) Uani 0.41(2) 1 d D U P A 2 H3B H 0.767421 0.523129 0.113221 0.040 Uiso 0.41(2) 1 calc R U P A 2 C4B C 0.6802(14) 0.6166(14) 0.2354(17) 0.033(4) Uani 0.41(2) 1 d D U P A 2 H4B H 0.654402 0.552211 0.275301 0.040 Uiso 0.41(2) 1 calc R U P A 2 C5B C 0.6269(17) 0.6964(6) 0.308(2) 0.035(4) Uani 0.41(2) 1 d D U P A 2 H5B H 0.574783 0.670089 0.378751 0.042 Uiso 0.41(2) 1 calc R U P A 2 C6B C 0.3999(19) 0.750000 -0.015(3) 0.023(4) Uani 0.36(2) 2 d S TU P B 4 H6B H 0.345643 0.750000 0.062844 0.028 Uiso 0.36(2) 2 calc R U P B 4 C7B C 0.4276(17) 0.6464(16) -0.054(2) 0.023(4) Uani 0.36(2) 1 d . U P B 4 H7B H 0.385587 0.593936 -0.004589 0.027 Uiso 0.36(2) 1 calc R U P B 4 C8B C 0.5101(17) 0.6079(14) -0.159(2) 0.021(4) Uani 0.36(2) 1 d . U P B 4 H8B H 0.512992 0.533814 -0.158092 0.025 Uiso 0.36(2) 1 calc R U P B 4 C9B C 0.5852(16) 0.6478(16) -0.260(2) 0.020(4) Uani 0.36(2) 1 d . U P B 4 H9B H 0.623920 0.594696 -0.313132 0.024 Uiso 0.36(2) 1 calc R U P B 4 C10B C 0.619(2) 0.750000 -0.304(3) 0.018(4) Uani 0.36(2) 2 d S TU P B 4 H10B H 0.676175 0.750000 -0.377973 0.021 Uiso 0.36(2) 2 calc R U P B 4 C6A C 0.4046(9) 0.6936(10) -0.0311(12) 0.032(3) Uani 0.64(2) 1 d . U P B 3 H6A H 0.351994 0.664409 0.036695 0.039 Uiso 0.64(2) 1 calc R U P B 3 C7A C 0.4662(10) 0.6173(10) -0.1104(13) 0.030(2) Uani 0.64(2) 1 d . U P B 3 H7A H 0.442747 0.548473 -0.086532 0.036 Uiso 0.64(2) 1 calc R U P B 3 C8A C 0.5533(10) 0.6177(10) -0.2155(14) 0.030(2) Uani 0.64(2) 1 d . U P B 3 H8A H 0.575768 0.549038 -0.242168 0.036 Uiso 0.64(2) 1 calc R U P B 3 C9A C 0.6149(10) 0.6933(10) -0.2904(12) 0.030(3) Uani 0.64(2) 1 d . U P B 3 H9A H 0.669035 0.664499 -0.356209 0.036 Uiso 0.64(2) 1 calc R U P B 3 Nd1 Nd 0.61561(3) 0.750000 -0.00308(6) 0.02466(17) Uani 1 2 d S T P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.024(5) 0.040(6) 0.019(5) 0.000 -0.004(4) 0.000 C2A 0.024(4) 0.040(5) 0.023(4) 0.000(3) -0.005(4) 0.004(3) C3A 0.023(4) 0.042(5) 0.027(4) 0.001(3) -0.003(4) 0.005(3) C4A 0.021(4) 0.046(5) 0.030(4) 0.000(4) 0.000(4) 0.007(4) C5A 0.020(4) 0.051(6) 0.034(4) 0.001(5) -0.002(5) 0.008(4) C1B 0.026(6) 0.033(8) 0.031(8) 0.000 -0.002(6) 0.000 C2B 0.027(6) 0.034(7) 0.031(7) 0.006(3) -0.003(5) 0.001(3) C3B 0.029(6) 0.039(6) 0.031(6) 0.012(4) -0.006(5) 0.003(4) C4B 0.030(6) 0.042(7) 0.029(6) 0.015(5) -0.005(5) 0.003(5) C5B 0.032(7) 0.044(8) 0.028(6) 0.017(6) -0.006(5) 0.002(6) C6B 0.022(7) 0.022(8) 0.025(7) 0.000 -0.003(6) 0.000 C7B 0.022(6) 0.021(7) 0.025(6) 0.000(3) -0.003(5) -0.003(3) C8B 0.021(6) 0.021(6) 0.021(6) -0.001(3) -0.001(5) -0.001(4) C9B 0.020(6) 0.023(7) 0.016(6) -0.003(3) 0.002(5) 0.001(3) C10B 0.018(7) 0.023(8) 0.012(6) 0.000 0.005(5) 0.000 C6A 0.026(4) 0.045(5) 0.026(5) 0.008(4) -0.004(3) -0.014(4) C7A 0.026(4) 0.040(5) 0.025(4) 0.008(3) -0.006(3) -0.014(3) C8A 0.027(4) 0.038(5) 0.024(4) 0.006(3) -0.007(3) -0.011(3) C9A 0.028(5) 0.041(6) 0.022(4) 0.004(4) -0.007(4) -0.010(4) Nd1 0.0201(2) 0.0329(3) 0.0210(2) 0.000 -0.0007(3) 0.000 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' Nd Nd -0.1943 3.0179 '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 C2A C1A H1A 108.8 . . ? C2A C1A H1A 108.8 8_575 . ? C2A C1A C2A 142.4(19) 8_575 . ? C1A C2A H2A 110.7 . . ? C1A C2A C3A 138.5(14) . . ? C3A C2A H2A 110.7 . . ? C2A C3A H3A 110.1 . . ? C4A C3A C2A 139.9(12) . . ? C4A C3A H3A 110.1 . . ? C3A C4A H4A 110.0 . . ? C5A C4A C3A 140.1(12) . . ? C5A C4A H4A 110.0 . . ? C4A C5A H5A 109.9 . . ? C5A C5A C4A 140.2(7) 8_575 . ? C5A C5A H5A 109.9 8_575 . ? C2B C1B H1B 110.7 . . ? C2B C1B H1B 110.7 8_575 . ? C2B C1B C2B 139(3) 8_575 . ? C1B C2B H2B 109.9 . . ? C1B C2B C3B 140.1(19) . . ? C3B C2B H2B 109.9 . . ? C2B C3B H3B 110.2 . . ? C4B C3B C2B 139.7(17) . . ? C4B C3B H3B 110.2 . . ? C3B C4B H4B 108.8 . . ? C5B C4B C3B 142.5(18) . . ? C5B C4B H4B 108.8 . . ? C4B C5B H5B 110.8 . . ? C5B C5B H5B 110.8 8_575 . ? C7B C6B H6B 110.0 8_575 . ? C7B C6B H6B 110.0 . . ? C6B C7B H7B 115.1 . . ? C6B C7B C8B 130(2) . . ? C8B C7B H7B 115.1 . . ? C7B C8B H8B 110.9 . . ? C9B C8B C7B 138.2(17) . . ? C9B C8B H8B 110.9 . . ? C8B C9B H9B 112.4 . . ? C8B C9B C10B 135.3(19) . . ? C10B C9B H9B 112.4 . . ? C9B C10B C9B 133(2) 8_575 . ? C9B C10B H10B 113.3 . . ? C9B C10B H10B 113.3 8_575 . ? C6A C6A H6A 113.1 8_575 . ? C7A C6A H6A 113.1 . . ? C6A C7A H7A 112.0 . . ? C8A C7A C6A 136.1(11) . . ? C8A C7A H7A 112.0 . . ? C7A C8A H8A 112.0 . . ? C9A C8A C7A 136.0(12) . . ? C9A C8A H8A 112.0 . . ? C8A C9A C9A 134.2(8) . 8_575 ? C8A C9A H9A 112.9 . . ? C9A C9A H9A 112.9 8_575 . ? 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 C1A H1A 0.9500 . ? C1A C2A 1.389(11) 8_575 ? C1A C2A 1.389(11) . ? C2A H2A 0.9500 . ? C2A C3A 1.400(11) . ? C3A H3A 0.9500 . ? C3A C4A 1.395(11) . ? C4A H4A 0.9500 . ? C4A C5A 1.389(11) . ? C5A C5A 1.385(14) 8_575 ? C5A H5A 0.9500 . ? C1B H1B 0.9500 . ? C1B C2B 1.379(13) 8_575 ? C1B C2B 1.379(13) . ? C2B H2B 0.9500 . ? C2B C3B 1.382(13) . ? C3B H3B 0.9500 . ? C3B C4B 1.381(13) . ? C4B H4B 0.9500 . ? C4B C5B 1.367(14) . ? C5B C5B 1.373(15) 8_575 ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C6B C7B 1.41(2) 8_575 ? C6B C7B 1.41(2) . ? C7B H7B 0.9500 . ? C7B C8B 1.45(2) . ? C8B H8B 0.9500 . ? C8B C9B 1.37(2) . ? C9B H9B 0.9500 . ? C9B C10B 1.43(2) . ? C10B H10B 0.9500 . ? C6A C6A 1.45(3) 8_575 ? C6A H6A 0.9500 . ? C6A C7A 1.414(16) . ? C7A H7A 0.9500 . ? C7A C8A 1.403(15) . ? C8A H8A 0.9500 . ? C8A C9A 1.390(14) . ? C9A C9A 1.45(2) 8_575 ? C9A H9A 0.9500 . ? 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 C1A C2A C3A C4A -3(3) . . . . ? C2A C1A C2A C3A -3(4) 8_575 . . . ? C2A C3A C4A C5A 2(3) . . . . ? C3A C4A C5A C5A 4(2) . . . 8_575 ? C1B C2B C3B C4B -2(4) . . . . ? C2B C1B C2B C3B 6(6) 8_575 . . . ? C2B C3B C4B C5B 1(4) . . . . ? C3B C4B C5B C5B -2(4) . . . 8_575 ? C6B C7B C8B C9B -4(4) . . . . ? C7B C6B C7B C8B 4(5) 8_575 . . . ? C7B C8B C9B C10B 3(4) . . . . ? C8B C9B C10B C9B -1(5) . . . 8_575 ? C6A C6A C7A C8A 2.7(16) 8_575 . . . ? C6A C7A C8A C9A -2(2) . . . . ? C7A C8A C9A C9A 0.3(17) . . . 8_575 ?