#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:30:41 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247661.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_7247661 loop_ _publ_author_name 'George, Tanner' 'Brosseau, Christa L.' 'Masuda, Jason D.' _publ_section_title ; Electrochemical and X-ray structural evidence of multiple molybdenum precursor candidates from a reported non-aqueous electrodeposition of molybdenum disulfide ; _journal_issue 46 _journal_name_full 'RSC Advances' _journal_page_first 32199 _journal_page_last 32216 _journal_paper_doi 10.1039/D3RA04605B _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'Mo6 O19, 2(C9 H20 N)' _chemical_formula_sum 'C18 H40 Mo6 N2 O19' _chemical_formula_weight 1164.16 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2023-09-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-10-01 deposited with the CCDC. 2023-10-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.838(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.4347(8) _cell_length_b 16.0288(12) _cell_length_c 10.9136(9) _cell_measurement_reflns_used 9194 _cell_measurement_temperature 125.0 _cell_measurement_theta_max 33.18 _cell_measurement_theta_min 2.29 _cell_volume 1615.3(2) _computing_cell_refinement 'SAINT V8.40B (Bruker AXS Inc., 2016)' _computing_data_collection 'APEX4 (Bruker AXS Inc., 2021)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS Inc., 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 125.00 _diffrn_detector '100 \\times 140 mm^2^ CMOS sensor' _diffrn_detector_area_resol_mean 7.3910 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device '\k--geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 55716 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.259 _diffrn_reflns_theta_min 2.291 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\mS 3.0' _exptl_absorpt_coefficient_mu 2.339 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.5705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0832 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.7642. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.393 _exptl_crystal_description Prism _exptl_crystal_F_000 1132 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.772 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.145 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 6194 _refine_ls_number_restraints 55 _refine_ls_restrained_S_all 1.211 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0332 _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^)+6.6219P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.0731 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5542 _reflns_number_total 6194 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra04605b2.cif _cod_data_source_block mo_2020_09_16_jdm_tg187wash2_0_a _cod_database_code 7247661 _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 0.853 _shelx_estimated_absorpt_t_min 0.665 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N1A-C1A \\sim N1B-C1B with sigma of 0.02 N1A-C2A \\sim N1B-C2B with sigma of 0.02 N1A-C5 \\sim N1B-C5 with sigma of 0.02 N1A-C9 \\sim N1B-C9 with sigma of 0.02 C2A-C3A \\sim C2B-C3B with sigma of 0.02 C3A-C4A \\sim C3B-C4B with sigma of 0.02 N1A-C3A \\sim N1B-C3B with sigma of 0.04 C1A-C2A \\sim C1B-C2B with sigma of 0.04 C1A-C5 \\sim C1B-C5 with sigma of 0.04 C1A-C9 \\sim C1B-C9 with sigma of 0.04 C2A-C4A \\sim C2B-C4B with sigma of 0.04 C2A-C5 \\sim C2B-C5 with sigma of 0.04 C2A-C9 \\sim C2B-C9 with sigma of 0.04 3. Rigid body (RIGU) restrains N1A, C1A, C2A, C3A, C4A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1B, C1B, C2B, C3B, C4B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(H5BC)=Sof(H5BD)=Sof(H9BC)=Sof(H9BD)=Sof(C1B)=Sof(H1AA)=Sof(H1AB)= Sof(H1AC)=Sof(N1B)=Sof(C2B)=Sof(H2AA)=Sof(H2AB)=Sof(C3B)=Sof(H3AA)=Sof(H3AB)= Sof(C4B)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1) Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2A)=Sof(H2A)=Sof(H2B)= Sof(C3A)=Sof(H3A)=Sof(H3B)=Sof(C4A)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(H5AA)= Sof(H5AB)=Sof(H9AA)=Sof(H9AB)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C2A(H2A,H2B), C3A(H3A,H3B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B), C7(H7A, H7B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C2B(H2AA,H2AB), C3B(H3AA,H3AB) 5.b Idealised Me refined as rotating group: C1A(H1A,H1B,H1C), C4A(H4A,H4B,H4C), C1B(H1AA,H1AB,H1AC), C4B(H4AA,H4AB,H4AC) ; _shelx_res_file ; TITL mo_2020_09_16_JDM_TG187wash2_0_a.res in P2(1)/n mo_2020_09_16_jdm_tg187wash2_0_a.res created by SHELXL-2018/3 at 21:13:40 on 10-Sep-2023 REM Old TITL mo_2020_09_16_JDM_TG187wash2_0 in P2(1) REM SHELXT solution in P2(1)/n REM R1 0.068, Rweak 0.004, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C18 Mo6 N2 O19 CELL 0.71073 9.4347 16.0288 10.9136 90 101.838 90 ZERR 2 0.0008 0.0012 0.0009 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Mo N O UNIT 36 80 12 4 38 SADI N1 C1 N1a C1a SADI N1 C2 N1a C2a SADI N1 C5 N1a C5 SADI N1 C9 N1a C9 SADI C2 C3 C2a C3a SADI C3 C4 C3a C4a SADI 0.04 N1 C3 N1a C3a SADI 0.04 C1 C2 C1a C2a SADI 0.04 C1 C5 C1a C5 SADI 0.04 C1 C9 C1a C9 SADI 0.04 C2 C4 C2a C4a SADI 0.04 C2 C5 C2a C5 SADI 0.04 C2 C9 C2a C9 RIGU N1 C1 C2 C3 C4 RIGU N1a C1a C2a C3a C4a L.S. 30 PLAN 34 SIZE 0.07 0.14 0.19 TEMP -148.15 CONF FREE C9 C5 BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.000000 6.621900 FVAR 0.29767 0.83388 MO1 3 0.662196 0.474448 0.372479 11.00000 0.01859 0.02014 = 0.02111 -0.00106 0.00750 0.00058 MO2 3 0.472573 0.636100 0.425875 11.00000 0.02035 0.01552 = 0.02470 0.00182 0.00618 0.00033 MO3 3 0.690152 0.542118 0.658497 11.00000 0.01802 0.02144 = 0.02024 -0.00251 0.00264 -0.00142 O1 5 0.500000 0.500000 0.500000 10.50000 0.01719 0.01669 = 0.01929 0.00005 0.00542 -0.00004 O2 5 0.624566 0.587528 0.344445 11.00000 0.02442 0.02106 = 0.02714 0.00354 0.01009 -0.00058 O3 5 0.636621 0.642292 0.570887 11.00000 0.02187 0.01713 = 0.03018 -0.00340 0.00372 -0.00242 O4 5 0.786599 0.504828 0.533997 11.00000 0.01687 0.02359 = 0.02457 -0.00164 0.00527 -0.00041 O5 5 0.484992 0.443785 0.270179 11.00000 0.02061 0.02984 = 0.01963 -0.00678 0.00527 -0.00115 O6 5 0.337839 0.577311 0.306477 11.00000 0.02218 0.02230 = 0.01974 0.00201 0.00202 0.00100 O7 5 0.349873 0.634526 0.539780 11.00000 0.02235 0.01872 = 0.02799 -0.00107 0.00848 0.00293 O8 5 0.822914 0.570820 0.778681 11.00000 0.02519 0.03331 = 0.02698 -0.00550 -0.00088 -0.00310 O9 5 0.785217 0.450872 0.285330 11.00000 0.02455 0.03019 = 0.02991 -0.00276 0.01255 -0.00074 O10 5 0.461804 0.734136 0.369525 11.00000 0.03100 0.01901 = 0.04168 0.00693 0.00643 0.00062 PART 1 N1 4 0.984051 0.735575 0.405927 21.00000 0.01660 0.02180 = 0.02674 0.00076 0.00375 -0.00076 C1 1 0.984930 0.671075 0.504376 21.00000 0.02892 0.02180 = 0.03340 0.00685 0.01138 0.00291 AFIX 137 H1A 2 0.907070 0.630793 0.475621 21.00000 -1.50000 H1B 2 0.969932 0.697923 0.581387 21.00000 -1.50000 H1C 2 1.078366 0.642080 0.520879 21.00000 -1.50000 AFIX 0 C2 1 1.029541 0.698433 0.291594 21.00000 0.01802 0.02457 = 0.02806 0.00121 0.00905 -0.00026 AFIX 23 H2A 2 1.017003 0.741331 0.224975 21.00000 -1.20000 H2B 2 1.133863 0.684443 0.314029 21.00000 -1.20000 AFIX 0 C3 1 0.946435 0.621034 0.239607 21.00000 0.02490 0.02692 = 0.03157 -0.00278 0.00982 -0.00261 AFIX 23 H3A 2 0.841168 0.630897 0.230217 21.00000 -1.20000 H3B 2 0.973896 0.573732 0.297979 21.00000 -1.20000 AFIX 0 C4 1 0.981419 0.599964 0.111894 21.00000 0.03543 0.03885 = 0.02705 -0.00301 0.01217 0.00778 AFIX 137 H4A 2 0.953370 0.646822 0.054346 21.00000 -1.50000 H4B 2 0.927678 0.549951 0.077862 21.00000 -1.50000 H4C 2 1.085552 0.589662 0.121908 21.00000 -1.50000 AFIX 0 PART 0 C5 1 0.834424 0.774638 0.368925 11.00000 0.01768 0.02466 = 0.03959 -0.00345 0.00398 0.00166 PART 1 AFIX 23 H5AA 2 0.761801 0.729580 0.347463 21.00000 -1.20000 H5AB 2 0.830760 0.808948 0.292911 21.00000 -1.20000 AFIX 23 PART 2 H5BC 2 0.759161 0.731930 0.340115 -21.00000 -1.20000 H5BD 2 0.846426 0.808944 0.296308 -21.00000 -1.20000 AFIX 0 PART 0 C6 1 0.793221 0.828956 0.470411 11.00000 0.02817 0.02996 = 0.03711 0.00244 0.01622 0.00218 AFIX 23 H6A 2 0.785284 0.793945 0.543432 11.00000 -1.20000 H6B 2 0.697724 0.855069 0.438334 11.00000 -1.20000 AFIX 0 C7 1 0.906508 0.896692 0.510931 11.00000 0.04207 0.02733 = 0.02315 -0.00530 0.00901 0.00110 AFIX 23 H7A 2 0.907373 0.935220 0.440188 11.00000 -1.20000 H7B 2 0.881549 0.929280 0.580613 11.00000 -1.20000 AFIX 0 C8 1 1.055339 0.857897 0.552872 11.00000 0.03905 0.03037 = 0.03088 -0.00459 -0.00383 -0.00383 AFIX 23 H8A 2 1.128572 0.902716 0.573369 11.00000 -1.20000 H8B 2 1.057230 0.824697 0.629683 11.00000 -1.20000 AFIX 0 C9 1 1.093936 0.802377 0.452819 11.00000 0.01937 0.02882 = 0.02872 0.00409 0.00363 -0.00504 PART 1 AFIX 23 H9AA 2 1.106061 0.837568 0.381130 21.00000 -1.20000 H9AB 2 1.188260 0.775408 0.486594 21.00000 -1.20000 AFIX 23 PART 2 H9BC 2 1.091555 0.834311 0.374776 -21.00000 -1.20000 H9BD 2 1.192072 0.778610 0.480987 -21.00000 -1.20000 AFIX 0 C1A 1 0.987935 0.687319 0.552517 -21.00000 0.04157 0.02437 = 0.04440 -0.01465 0.01499 -0.00280 AFIX 137 H1AA 2 0.967304 0.726122 0.616021 -21.00000 -1.50000 H1AB 2 1.085243 0.663979 0.580241 -21.00000 -1.50000 H1AC 2 0.916554 0.642077 0.540523 -21.00000 -1.50000 AFIX 0 N1A 4 0.979822 0.732950 0.431110 -21.00000 0.01776 0.03664 = 0.04080 -0.01586 0.01161 0.00212 C2A 1 0.996315 0.663617 0.338173 -21.00000 0.01527 0.01788 = 0.03414 -0.00037 0.00557 -0.00351 AFIX 23 H2AA 2 1.091923 0.636779 0.366577 -21.00000 -1.20000 H2AB 2 0.921307 0.620755 0.340303 -21.00000 -1.20000 AFIX 0 C3A 1 0.984069 0.691773 0.204819 -21.00000 0.04573 0.03035 = 0.03356 0.00136 0.00522 0.00567 AFIX 23 H3AA 2 1.069881 0.725271 0.196872 -21.00000 -1.20000 H3AB 2 0.896484 0.726604 0.178325 -21.00000 -1.20000 AFIX 0 C4A 1 0.974317 0.612959 0.122473 -21.00000 0.01764 0.04138 = 0.04317 -0.01227 0.00106 0.00541 AFIX 137 H4AA 2 0.931536 0.627472 0.035521 -21.00000 -1.50000 H4AB 2 0.913614 0.571215 0.152533 -21.00000 -1.50000 H4AC 2 1.071602 0.590104 0.127036 -21.00000 -1.50000 AFIX 0 HKLF 4 REM mo_2020_09_16_JDM_TG187wash2_0_a.res in P2(1)/n REM wR2 = 0.0731, GooF = S = 1.210, Restrained GooF = 1.211 for all data REM R1 = 0.0332 for 5542 Fo > 4sig(Fo) and 0.0394 for all 6194 data REM 255 parameters refined using 55 restraints END WGHT 0.0000 6.2204 REM Highest difference peak 0.772, deepest hole -1.142, 1-sigma level 0.145 Q1 1 0.6196 0.5012 0.3632 11.00000 0.05 0.77 Q2 1 0.8295 0.7720 0.4304 11.00000 0.05 0.72 Q3 1 0.5821 0.6199 0.4822 11.00000 0.05 0.71 Q4 1 0.7200 0.5250 0.5237 11.00000 0.05 0.69 Q5 1 0.9383 0.9358 0.6393 11.00000 0.05 0.69 Q6 1 1.0043 0.7898 0.2122 11.00000 0.05 0.64 Q7 1 0.7555 0.5494 0.5798 11.00000 0.05 0.55 Q8 1 0.6622 0.6389 0.5194 11.00000 0.05 0.53 Q9 1 0.7915 0.5668 0.7131 11.00000 0.05 0.53 Q10 1 0.5339 0.6418 0.3410 11.00000 0.05 0.52 Q11 1 0.9948 0.6540 0.2698 11.00000 0.05 0.52 Q12 1 0.4773 0.5932 0.3364 11.00000 0.05 0.51 Q13 1 0.5627 0.5977 0.3996 11.00000 0.05 0.51 Q14 1 1.0316 0.8003 0.3045 11.00000 0.05 0.51 Q15 1 0.5371 0.6367 0.5393 11.00000 0.05 0.51 Q16 1 0.5570 0.4648 0.2941 11.00000 0.05 0.51 Q17 1 0.8389 0.6605 0.4594 11.00000 0.05 0.51 Q18 1 0.7238 0.4228 0.3164 11.00000 0.05 0.50 Q19 1 0.6572 0.4757 0.3244 11.00000 0.05 0.50 Q20 1 1.0076 0.7834 0.1203 11.00000 0.05 0.50 Q21 1 0.7877 0.4920 0.4268 11.00000 0.05 0.49 Q22 1 0.3715 0.6023 0.3774 11.00000 0.05 0.48 Q23 1 0.7526 0.4557 0.3299 11.00000 0.05 0.48 Q24 1 0.8049 0.6443 0.3759 11.00000 0.05 0.47 Q25 1 0.3947 0.4728 0.2791 11.00000 0.05 0.46 Q26 1 0.9935 0.8558 0.7459 11.00000 0.05 0.46 Q27 1 1.1070 0.6048 0.4000 11.00000 0.05 0.46 Q28 1 0.3826 0.6293 0.4796 11.00000 0.05 0.46 Q29 1 0.7321 0.4820 0.3043 11.00000 0.05 0.45 Q30 1 1.0960 0.8690 0.5224 11.00000 0.05 0.45 Q31 1 0.8578 0.6139 0.2788 11.00000 0.05 0.45 Q32 1 0.4411 0.7052 0.4359 11.00000 0.05 0.45 Q33 1 0.8358 0.6344 0.4561 11.00000 0.05 0.45 Q34 1 0.8247 0.6157 0.4496 11.00000 0.05 0.44 ; _shelx_res_checksum 10998 _olex2_submission_special_instructions 'No special instructions were received' 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 Mo1 Mo 0.66220(3) 0.47445(2) 0.37248(2) 0.01945(5) Uani 1 1 d . . . . . Mo2 Mo 0.47257(3) 0.63610(2) 0.42587(3) 0.01997(6) Uani 1 1 d . . . . . Mo3 Mo 0.69015(3) 0.54212(2) 0.65850(2) 0.02008(5) Uani 1 1 d . . . . . O1 O 0.500000 0.500000 0.500000 0.0175(5) Uani 1 2 d S . P . . O2 O 0.6246(2) 0.58753(14) 0.3444(2) 0.0235(4) Uani 1 1 d . . . . . O3 O 0.6366(2) 0.64229(13) 0.5709(2) 0.0233(4) Uani 1 1 d . . . . . O4 O 0.7866(2) 0.50483(14) 0.5340(2) 0.0215(4) Uani 1 1 d . . . . . O5 O 0.4850(2) 0.44379(15) 0.2702(2) 0.0232(4) Uani 1 1 d . . . . . O6 O 0.3378(2) 0.57731(14) 0.3065(2) 0.0217(4) Uani 1 1 d . . . . . O7 O 0.3499(2) 0.63453(14) 0.5398(2) 0.0226(4) Uani 1 1 d . . . . . O8 O 0.8229(3) 0.57082(16) 0.7787(2) 0.0294(5) Uani 1 1 d . . . . . O9 O 0.7852(3) 0.45087(16) 0.2853(2) 0.0272(5) Uani 1 1 d . . . . . O10 O 0.4618(3) 0.73414(15) 0.3695(3) 0.0307(5) Uani 1 1 d . . . . . N1 N 0.9841(4) 0.7356(3) 0.4059(5) 0.0218(9) Uani 0.834(8) 1 d D . P A 1 C1 C 0.9849(5) 0.6711(3) 0.5044(5) 0.0273(9) Uani 0.834(8) 1 d D . P A 1 H1A H 0.907070 0.630793 0.475621 0.041 Uiso 0.834(8) 1 calc R U P A 1 H1B H 0.969932 0.697923 0.581387 0.041 Uiso 0.834(8) 1 calc R U P A 1 H1C H 1.078366 0.642080 0.520879 0.041 Uiso 0.834(8) 1 calc R U P A 1 C2 C 1.0295(4) 0.6984(2) 0.2916(4) 0.0229(8) Uani 0.834(8) 1 d D . P A 1 H2A H 1.017003 0.741331 0.224975 0.028 Uiso 0.834(8) 1 calc R U P A 1 H2B H 1.133863 0.684443 0.314029 0.028 Uiso 0.834(8) 1 calc R U P A 1 C3 C 0.9464(4) 0.6210(3) 0.2396(4) 0.0272(9) Uani 0.834(8) 1 d D . P A 1 H3A H 0.841168 0.630897 0.230217 0.033 Uiso 0.834(8) 1 calc R U P A 1 H3B H 0.973896 0.573732 0.297979 0.033 Uiso 0.834(8) 1 calc R U P A 1 C4 C 0.9814(17) 0.6000(6) 0.1119(8) 0.0330(16) Uani 0.834(8) 1 d D . P A 1 H4A H 0.953370 0.646822 0.054346 0.049 Uiso 0.834(8) 1 calc R U P A 1 H4B H 0.927678 0.549951 0.077862 0.049 Uiso 0.834(8) 1 calc R U P A 1 H4C H 1.085552 0.589662 0.121908 0.049 Uiso 0.834(8) 1 calc R U P A 1 C5 C 0.8344(3) 0.7746(2) 0.3689(4) 0.0276(6) Uani 1 1 d D . . . . H5AA H 0.761801 0.729580 0.347463 0.033 Uiso 0.834(8) 1 calc R U P A 1 H5AB H 0.830760 0.808948 0.292911 0.033 Uiso 0.834(8) 1 calc R U P A 1 H5BC H 0.759161 0.731930 0.340115 0.033 Uiso 0.166(8) 1 calc R U P A 2 H5BD H 0.846426 0.808944 0.296308 0.033 Uiso 0.166(8) 1 calc R U P A 2 C6 C 0.7932(4) 0.8290(2) 0.4704(4) 0.0304(7) Uani 1 1 d . . . . . H6A H 0.785284 0.793945 0.543432 0.036 Uiso 1 1 calc R U . . . H6B H 0.697724 0.855069 0.438334 0.036 Uiso 1 1 calc R U . . . C7 C 0.9065(4) 0.8967(2) 0.5109(3) 0.0305(7) Uani 1 1 d . . . . . H7A H 0.907373 0.935220 0.440188 0.037 Uiso 1 1 calc R U . . . H7B H 0.881549 0.929280 0.580613 0.037 Uiso 1 1 calc R U . . . C8 C 1.0553(4) 0.8579(2) 0.5529(4) 0.0350(8) Uani 1 1 d . . . . . H8A H 1.128572 0.902716 0.573369 0.042 Uiso 1 1 calc R U . . . H8B H 1.057230 0.824697 0.629683 0.042 Uiso 1 1 calc R U . . . C9 C 1.0939(3) 0.8024(2) 0.4528(3) 0.0258(6) Uani 1 1 d D . . . . H9AA H 1.106061 0.837568 0.381130 0.031 Uiso 0.834(8) 1 calc R U P A 1 H9AB H 1.188260 0.775408 0.486594 0.031 Uiso 0.834(8) 1 calc R U P A 1 H9BC H 1.091555 0.834311 0.374776 0.031 Uiso 0.166(8) 1 calc R U P A 2 H9BD H 1.192072 0.778610 0.480987 0.031 Uiso 0.166(8) 1 calc R U P A 2 C1A C 0.988(3) 0.6873(14) 0.553(2) 0.036(5) Uani 0.166(8) 1 d D . P A 2 H1AA H 0.967304 0.726122 0.616021 0.054 Uiso 0.166(8) 1 calc R U P A 2 H1AB H 1.085243 0.663979 0.580241 0.054 Uiso 0.166(8) 1 calc R U P A 2 H1AC H 0.916554 0.642077 0.540523 0.054 Uiso 0.166(8) 1 calc R U P A 2 N1A N 0.9798(17) 0.7330(10) 0.4311(18) 0.031(6) Uani 0.166(8) 1 d D . P A 2 C2A C 0.9963(18) 0.6636(10) 0.3382(15) 0.022(4) Uani 0.166(8) 1 d D . P A 2 H2AA H 1.091923 0.636779 0.366577 0.027 Uiso 0.166(8) 1 calc R U P A 2 H2AB H 0.921307 0.620755 0.340303 0.027 Uiso 0.166(8) 1 calc R U P A 2 C3A C 0.984(3) 0.6918(13) 0.2048(17) 0.037(5) Uani 0.166(8) 1 d D . P A 2 H3AA H 1.069881 0.725271 0.196872 0.044 Uiso 0.166(8) 1 calc R U P A 2 H3AB H 0.896484 0.726604 0.178325 0.044 Uiso 0.166(8) 1 calc R U P A 2 C4A C 0.974(8) 0.613(3) 0.122(4) 0.035(9) Uani 0.166(8) 1 d D . P A 2 H4AA H 0.931536 0.627472 0.035521 0.052 Uiso 0.166(8) 1 calc R U P A 2 H4AB H 0.913614 0.571215 0.152533 0.052 Uiso 0.166(8) 1 calc R U P A 2 H4AC H 1.071602 0.590104 0.127036 0.052 Uiso 0.166(8) 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 Mo1 0.01859(11) 0.02014(11) 0.02111(11) -0.00106(8) 0.00750(8) 0.00058(8) Mo2 0.02035(11) 0.01552(10) 0.02470(12) 0.00182(8) 0.00618(9) 0.00033(8) Mo3 0.01802(10) 0.02144(11) 0.02024(11) -0.00251(9) 0.00264(8) -0.00142(8) O1 0.0172(12) 0.0167(12) 0.0193(13) 0.0000(10) 0.0054(10) 0.0000(10) O2 0.0244(10) 0.0211(10) 0.0271(11) 0.0035(8) 0.0101(8) -0.0006(8) O3 0.0219(10) 0.0171(9) 0.0302(11) -0.0034(8) 0.0037(8) -0.0024(8) O4 0.0169(9) 0.0236(10) 0.0246(10) -0.0016(8) 0.0053(8) -0.0004(8) O5 0.0206(10) 0.0298(11) 0.0196(10) -0.0068(8) 0.0053(8) -0.0011(8) O6 0.0222(10) 0.0223(10) 0.0197(10) 0.0020(8) 0.0020(8) 0.0010(8) O7 0.0224(10) 0.0187(9) 0.0280(11) -0.0011(8) 0.0085(8) 0.0029(8) O8 0.0252(11) 0.0333(13) 0.0270(12) -0.0055(10) -0.0009(9) -0.0031(9) O9 0.0246(11) 0.0302(12) 0.0299(12) -0.0028(9) 0.0126(9) -0.0007(9) O10 0.0310(12) 0.0190(10) 0.0417(14) 0.0069(10) 0.0064(10) 0.0006(9) N1 0.017(2) 0.0218(19) 0.0267(18) 0.0008(13) 0.0037(13) -0.0008(14) C1 0.029(2) 0.0218(19) 0.033(2) 0.0068(17) 0.0114(19) 0.0029(16) C2 0.0180(15) 0.0246(17) 0.0281(19) 0.0012(14) 0.0091(13) -0.0003(12) C3 0.0249(17) 0.0269(18) 0.032(2) -0.0028(15) 0.0098(15) -0.0026(14) C4 0.035(4) 0.039(4) 0.027(3) -0.003(2) 0.012(2) 0.008(3) C5 0.0177(12) 0.0247(14) 0.0396(18) -0.0034(13) 0.0040(12) 0.0017(11) C6 0.0282(15) 0.0300(16) 0.0371(18) 0.0024(14) 0.0162(14) 0.0022(13) C7 0.0421(19) 0.0273(16) 0.0232(15) -0.0053(12) 0.0090(13) 0.0011(14) C8 0.0391(19) 0.0304(17) 0.0309(18) -0.0046(14) -0.0038(14) -0.0038(15) C9 0.0194(13) 0.0288(15) 0.0287(15) 0.0041(12) 0.0036(11) -0.0050(11) C1A 0.042(13) 0.024(10) 0.044(11) -0.015(9) 0.015(11) -0.003(9) N1A 0.018(11) 0.037(12) 0.041(10) -0.016(8) 0.012(9) 0.002(9) C2A 0.015(7) 0.018(7) 0.034(7) 0.000(5) 0.006(6) -0.004(6) C3A 0.046(13) 0.030(10) 0.034(8) 0.001(7) 0.005(8) 0.006(9) C4A 0.018(13) 0.041(16) 0.043(14) -0.012(12) 0.001(13) 0.005(12) 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 Mo1 O1 78.37(7) . . ? O2 Mo1 O4 87.99(10) . . ? O2 Mo1 O5 92.33(10) . . ? O2 Mo1 O7 154.05(9) . 3_666 ? O4 Mo1 O1 76.30(6) . . ? O4 Mo1 O7 82.52(9) . 3_666 ? O5 Mo1 O1 77.58(7) . . ? O5 Mo1 O4 153.26(9) . . ? O5 Mo1 O7 85.70(10) . 3_666 ? O7 Mo1 O1 75.94(6) 3_666 . ? O9 Mo1 O1 176.41(9) . . ? O9 Mo1 O2 104.81(11) . . ? O9 Mo1 O4 101.97(11) . . ? O9 Mo1 O5 103.77(11) . . ? O9 Mo1 O7 100.78(11) . 3_666 ? O2 Mo2 O1 75.50(6) . . ? O3 Mo2 O1 75.83(6) . . ? O3 Mo2 O2 81.94(10) . . ? O6 Mo2 O1 77.38(7) . . ? O6 Mo2 O2 86.62(10) . . ? O6 Mo2 O3 152.74(9) . . ? O7 Mo2 O1 78.18(7) . . ? O7 Mo2 O2 153.33(9) . . ? O7 Mo2 O3 87.60(10) . . ? O7 Mo2 O6 91.80(10) . . ? O10 Mo2 O1 176.71(9) . . ? O10 Mo2 O2 101.35(11) . . ? O10 Mo2 O3 102.97(11) . . ? O10 Mo2 O6 103.51(11) . . ? O10 Mo2 O7 104.90(12) . . ? O3 Mo3 O1 77.53(7) . . ? O3 Mo3 O5 86.78(10) . 3_666 ? O3 Mo3 O6 152.79(9) . 3_666 ? O4 Mo3 O1 77.52(7) . . ? O4 Mo3 O3 91.33(10) . . ? O4 Mo3 O5 152.52(9) . 3_666 ? O4 Mo3 O6 86.31(10) . 3_666 ? O5 Mo3 O1 75.31(6) 3_666 . ? O5 Mo3 O6 83.07(10) 3_666 3_666 ? O6 Mo3 O1 75.50(6) 3_666 . ? O8 Mo3 O1 177.03(9) . . ? O8 Mo3 O3 104.00(11) . . ? O8 Mo3 O4 104.90(11) . . ? O8 Mo3 O5 102.15(11) . 3_666 ? O8 Mo3 O6 102.79(11) . 3_666 ? Mo1 O1 Mo1 180.0 . 3_666 ? Mo1 O1 Mo2 89.824(10) . . ? Mo1 O1 Mo2 90.176(10) 3_666 . ? Mo1 O1 Mo2 90.176(10) . 3_666 ? Mo1 O1 Mo2 89.825(10) 3_666 3_666 ? Mo1 O1 Mo3 90.329(11) 3_666 . ? Mo1 O1 Mo3 89.672(11) . . ? Mo1 O1 Mo3 90.328(12) . 3_666 ? Mo1 O1 Mo3 89.671(11) 3_666 3_666 ? Mo2 O1 Mo2 179.999(13) . 3_666 ? Mo3 O1 Mo2 90.012(10) 3_666 3_666 ? Mo3 O1 Mo2 89.987(10) 3_666 . ? Mo3 O1 Mo2 90.014(10) . . ? Mo3 O1 Mo2 89.987(10) . 3_666 ? Mo3 O1 Mo3 180.0 3_666 . ? Mo1 O2 Mo2 115.95(11) . . ? Mo3 O3 Mo2 116.62(11) . . ? Mo3 O4 Mo1 115.95(11) . . ? Mo1 O5 Mo3 116.76(11) . 3_666 ? Mo2 O6 Mo3 116.71(11) . 3_666 ? Mo2 O7 Mo1 115.71(11) . 3_666 ? C1 N1 C2 111.0(4) . . ? C1 N1 C5 110.2(4) . . ? C1 N1 C9 110.3(4) . . ? C5 N1 C2 110.2(3) . . ? C9 N1 C2 105.5(3) . . ? C9 N1 C5 109.5(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C3 C2 N1 114.6(3) . . ? C3 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? C2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C2 C3 C4 109.2(6) . . ? H3A C3 H3B 108.3 . . ? C4 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5AA 108.8 . . ? N1 C5 H5AB 108.8 . . ? N1 C5 C6 113.8(3) . . ? H5AA C5 H5AB 107.7 . . ? H5BC C5 H5BD 108.8 . . ? C6 C5 H5AA 108.8 . . ? C6 C5 H5AB 108.8 . . ? C6 C5 H5BC 110.7 . . ? C6 C5 H5BD 110.7 . . ? N1A C5 H5BC 110.7 . . ? N1A C5 H5BD 110.7 . . ? N1A C5 C6 105.3(7) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 C7 110.5(3) . . ? H6A C6 H6B 108.1 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C8 C7 C6 110.2(3) . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C7 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C9 C8 C7 111.6(3) . . ? C9 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? N1 C9 C8 114.4(3) . . ? N1 C9 H9AA 108.7 . . ? N1 C9 H9AB 108.7 . . ? C8 C9 H9AA 108.7 . . ? C8 C9 H9AB 108.7 . . ? C8 C9 H9BC 110.6 . . ? C8 C9 H9BD 110.6 . . ? H9AA C9 H9AB 107.6 . . ? H9BC C9 H9BD 108.7 . . ? N1A C9 C8 105.9(8) . . ? N1A C9 H9BC 110.6 . . ? N1A C9 H9BD 110.6 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? C5 N1A C2A 102.9(11) . . ? C9 N1A C5 106.6(10) . . ? C9 N1A C2A 117.7(13) . . ? C1A N1A C5 118.4(16) . . ? C1A N1A C9 108.1(14) . . ? C1A N1A C2A 103.7(14) . . ? N1A C2A H2AA 108.5 . . ? N1A C2A H2AB 108.5 . . ? H2AA C2A H2AB 107.5 . . ? C3A C2A N1A 115.1(14) . . ? C3A C2A H2AA 108.5 . . ? C3A C2A H2AB 108.5 . . ? C2A C3A H3AA 110.2 . . ? C2A C3A H3AB 110.2 . . ? C2A C3A C4A 108(2) . . ? H3AA C3A H3AB 108.5 . . ? C4A C3A H3AA 110.2 . . ? C4A C3A H3AB 110.2 . . ? C3A C4A H4AA 109.5 . . ? C3A C4A H4AB 109.5 . . ? C3A C4A H4AC 109.5 . . ? H4AA C4A H4AB 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 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 Mo1 O1 2.3065(3) . ? Mo1 O2 1.860(2) . ? Mo1 O4 1.968(2) . ? Mo1 O5 1.875(2) . ? Mo1 O7 2.006(2) 3_666 ? Mo1 O9 1.687(2) . ? Mo2 O1 2.3226(3) . ? Mo2 O2 1.994(2) . ? Mo2 O3 1.976(2) . ? Mo2 O6 1.877(2) . ? Mo2 O7 1.865(2) . ? Mo2 O10 1.683(2) . ? Mo3 O1 2.3223(3) . ? Mo3 O3 1.884(2) . ? Mo3 O4 1.881(2) . ? Mo3 O5 1.979(2) 3_666 ? Mo3 O6 1.980(2) 3_666 ? Mo3 O8 1.681(2) . ? N1 C1 1.490(6) . ? N1 C2 1.522(6) . ? N1 C5 1.521(5) . ? N1 C9 1.505(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.514(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.534(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5AA 0.9900 . ? C5 H5AB 0.9900 . ? C5 H5BC 0.9900 . ? C5 H5BD 0.9900 . ? C5 C6 1.521(5) . ? C5 N1A 1.551(16) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.524(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.518(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.510(5) . ? C9 H9AA 0.9900 . ? C9 H9AB 0.9900 . ? C9 H9BC 0.9900 . ? C9 H9BD 0.9900 . ? C9 N1A 1.533(16) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1A N1A 1.502(17) . ? N1A C2A 1.534(16) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C2A C3A 1.505(17) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3A C4A 1.54(2) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 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 O1 Mo1 O2 Mo2 -5.31(10) . . . . ? O1 Mo1 O5 Mo3 1.26(10) . . . 3_666 ? O1 Mo2 O6 Mo3 5.84(9) . . . 3_666 ? O1 Mo2 O7 Mo1 -0.58(9) . . . 3_666 ? O1 Mo3 O3 Mo2 0.86(10) . . . . ? O1 Mo3 O4 Mo1 6.57(9) . . . . ? O2 Mo1 O5 Mo3 -76.29(14) . . . 3_666 ? O2 Mo2 O6 Mo3 81.72(13) . . . 3_666 ? O2 Mo2 O7 Mo1 -9.9(3) . . . 3_666 ? O3 Mo2 O6 Mo3 16.6(3) . . . 3_666 ? O3 Mo2 O7 Mo1 -76.61(12) . . . 3_666 ? O3 Mo3 O4 Mo1 -70.34(13) . . . . ? O4 Mo1 O2 Mo2 -81.74(13) . . . . ? O4 Mo1 O5 Mo3 13.9(3) . . . 3_666 ? O4 Mo3 O3 Mo2 77.77(13) . . . . ? O5 Mo1 O2 Mo2 71.51(13) . . . . ? O5 Mo3 O3 Mo2 -74.80(13) 3_666 . . . ? O5 Mo3 O4 Mo1 15.2(3) 3_666 . . . ? O6 Mo2 O7 Mo1 76.12(13) . . . 3_666 ? O6 Mo3 O3 Mo2 -6.8(3) 3_666 . . . ? O6 Mo3 O4 Mo1 82.52(12) 3_666 . . . ? O7 Mo1 O2 Mo2 -13.5(3) 3_666 . . . ? O7 Mo1 O5 Mo3 77.79(13) 3_666 . . 3_666 ? O7 Mo2 O6 Mo3 -71.62(13) . . . 3_666 ? O8 Mo3 O3 Mo2 -176.52(13) . . . . ? O8 Mo3 O4 Mo1 -175.21(13) . . . . ? O9 Mo1 O2 Mo2 176.41(13) . . . . ? O9 Mo1 O5 Mo3 177.85(13) . . . 3_666 ? O10 Mo2 O6 Mo3 -177.41(13) . . . 3_666 ? O10 Mo2 O7 Mo1 -179.39(13) . . . 3_666 ? N1 C2 C3 C4 169.2(6) . . . . ? N1 C5 C6 C7 55.7(4) . . . . ? C1 N1 C2 C3 52.0(5) . . . . ? C1 N1 C5 C6 69.3(4) . . . . ? C1 N1 C9 C8 -70.2(4) . . . . ? C2 N1 C5 C6 -167.8(3) . . . . ? C2 N1 C9 C8 169.8(3) . . . . ? C5 N1 C2 C3 -70.3(4) . . . . ? C5 N1 C9 C8 51.2(5) . . . . ? C5 C6 C7 C8 -55.7(4) . . . . ? C5 N1A C2A C3A 52.9(19) . . . . ? C6 C5 N1A C9 -69.3(11) . . . . ? C6 C5 N1A C1A 52.6(15) . . . . ? C6 C5 N1A C2A 166.2(9) . . . . ? C6 C7 C8 C9 55.1(4) . . . . ? C7 C8 C9 N1 -54.3(4) . . . . ? C7 C8 C9 N1A -61.5(8) . . . . ? C8 C9 N1A C5 68.5(11) . . . . ? C8 C9 N1A C1A -59.8(14) . . . . ? C8 C9 N1A C2A -176.7(11) . . . . ? C9 N1 C2 C3 171.5(3) . . . . ? C9 N1 C5 C6 -52.1(5) . . . . ? C9 N1A C2A C3A -64(2) . . . . ? C1A N1A C2A C3A 176.9(19) . . . . ? N1A C5 C6 C7 62.5(8) . . . . ? N1A C2A C3A C4A -169(3) . . . . ?