#------------------------------------------------------------------------------ #$Date: 2026-06-02 23:54:21 +0100 (Tue, 02 Jun 2026) $ #$Revision: 306169 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721068.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_7721068 loop_ _publ_author_name 'Sarjanovi\'c, Josipa' 'Fiser, B\'ela' 'Pisk, Jana' _publ_section_title ; Mechanochemical synthesis, solvent-controlled coordination, and catalytic oxidation activity of furoic acid-based Mo(vi) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00558F _journal_year 2026 _chemical_formula_moiety 'C12 H10 Mo N2 O6' _chemical_formula_sum 'C12 H10 Mo N2 O6' _chemical_formula_weight 374.16 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2025-08-03 _audit_creation_method ; Olex2 1.5 (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) ; _audit_update_record ; 2026-02-04 deposited with the CCDC. 2026-05-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.654(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1957(4) _cell_length_b 10.5996(3) _cell_length_c 12.6277(5) _cell_measurement_reflns_used 5901 _cell_measurement_temperature 169.99(10) _cell_measurement_theta_max 78.4410 _cell_measurement_theta_min 4.8610 _cell_volume 1285.17(9) _computing_cell_refinement 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _computing_data_reduction 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _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_environment N~2~ _diffrn_ambient_temperature 169.99(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 98.00 141.00 0.50 0.05 -- 113.25 77.00 0.00 86 2 \w 150.00 176.00 0.50 0.05 -- 113.25 77.00 0.00 52 3 \w 114.00 178.00 0.50 0.05 -- 113.25 61.00 30.00 128 4 \w 143.00 168.00 0.50 0.05 -- 113.25 30.00 90.00 50 5 \w 102.00 160.00 0.50 0.05 -- 113.25 46.00 111.00 116 6 \w 103.00 128.00 0.50 0.05 -- 113.25 30.00 90.00 50 7 \w 51.00 98.00 0.50 0.05 -- 47.74 46.00 111.00 94 8 \w 101.00 139.00 0.50 0.05 -- 113.25 30.00 -30.00 76 9 \w 151.00 177.00 0.50 0.05 -- 113.25 30.00 -30.00 52 10 \w 140.00 166.00 0.50 0.05 -- 113.25 30.00-120.00 52 11 \w 114.00 156.00 0.50 0.05 -- 113.25 30.00-180.00 84 12 \w 127.00 175.00 0.50 0.05 -- 113.25 15.00-150.00 96 13 \w 103.00 128.00 0.50 0.05 -- 113.25 30.00-120.00 50 14 \w 12.00 39.00 0.50 0.05 -- 47.74 -46.00 -37.00 54 15 \w 46.00 72.00 0.50 0.05 -- 113.25 -77.00-120.00 52 16 \w 80.00 105.00 0.50 0.05 -- 113.25 -77.00-120.00 50 17 \w 42.00 68.00 0.50 0.05 -- 113.25 -61.00-180.00 52 18 \w 43.00 68.00 0.50 0.05 -- 113.25 -61.00 90.00 50 19 \w 51.00 99.00 0.50 0.05 -- 113.25 -77.00 120.00 96 20 \w 62.00 99.00 0.50 0.05 -- 113.25 -77.00 150.00 74 21 \w 43.00 68.00 0.50 0.05 -- 113.25 -61.00 120.00 50 22 \w 42.00 67.00 0.50 0.05 -- 113.25 -61.00 60.00 50 23 \w 46.00 71.00 0.50 0.05 -- 113.25 -61.00 150.00 50 24 \w 42.00 67.00 0.50 0.05 -- 113.25 -61.00 30.00 50 25 \w 42.00 71.00 0.50 0.05 -- 113.25 -61.00 0.00 58 26 \w 43.00 69.00 0.50 0.05 -- 113.25 -61.00 -30.00 52 27 \w 46.00 71.00 0.50 0.05 -- 113.25 -61.00 -60.00 50 28 \w 44.00 88.00 0.50 0.05 -- 113.25 -95.00 0.00 88 29 \w 42.00 73.00 0.50 0.05 -- 113.25 -95.00 -60.00 62 30 \w 51.00 77.00 0.50 0.05 -- 113.25-125.00 -90.00 52 31 \w 78.00 111.00 0.50 0.05 -- 113.25-125.00 -90.00 66 32 \w -22.00 28.00 0.50 0.05 -- -47.74 19.00 -90.00 100 33 \w -86.00 -13.00 0.50 0.05 -- -47.74 125.00-150.00 146 34 \w -16.00 24.00 0.50 0.05 -- -47.74 46.00 111.00 80 35 \w -52.00 -27.00 0.50 0.05 -- -91.75 46.00 111.00 50 36 \w -118.00 -62.00 0.50 0.05 -- -47.74 -46.00 -37.00 112 37 \w -145.00-120.00 0.50 0.05 -- -91.75 -46.00 -37.00 50 38 \w -119.00 -89.00 0.50 0.05 -- -47.74 -77.00-180.00 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0258881000 _diffrn_orient_matrix_UB_12 0.0632935000 _diffrn_orient_matrix_UB_13 0.1010256000 _diffrn_orient_matrix_UB_21 -0.1400189000 _diffrn_orient_matrix_UB_22 0.0515891000 _diffrn_orient_matrix_UB_23 -0.0787187000 _diffrn_orient_matrix_UB_31 -0.0738219000 _diffrn_orient_matrix_UB_32 -0.1202960000 _diffrn_orient_matrix_UB_33 0.0193434000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10190 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.351 _diffrn_reflns_theta_min 4.850 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.670 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.934 _exptl_crystal_description prism _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.2 _refine_diff_density_max 2.098 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 193 _refine_ls_number_reflns 2725 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0443 _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^)+(0.0849P)^2^+0.4325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1225 _refine_ls_wR_factor_ref 0.1253 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2491 _reflns_number_total 2725 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00558f2.cif _cod_data_source_block exp_7265_auto _cod_database_code 7721068 _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 0.276 _shelx_estimated_absorpt_t_min 0.137 _diffrn_oxdiff_digest_hkl ; 01c840d095fa46f69cc0fa0119052d62d6ccd5 ; _olex2_refinement_description ; 1. Restrained distances Mo1-H6A \\sim Mo1-H6B with sigma of 0.02 2.a Free rotating group: O6(H6A,H6B) 2.b Aromatic/amide H refined with riding coordinates: C10(H10), C9(H9), C11(H11), C6(H6), C12(H12), C3(H3), C1(H1), C2(H2) ; _shelx_res_file ; TITL exp_7265_auto_a.res in P2(1)/n exp_7265_auto.res created by SHELXL-2018/3 at 13:00:40 on 22-Jul-2025 REM Old TITL exp_7265_auto in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.068, Rweak 0.002, Alpha 0.031 REM 0.523 for 148 systematic absences, Orientation as input REM Formula found by SHELXT: C1 N1 O5 Br CELL 1.54184 10.1957 10.5996 12.6277 90 109.654 90 ZERR 4 0.0004 0.0003 0.0005 0 0.005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Mo N O UNIT 48 40 4 8 24 SADI Mo1 H6a Mo1 H6b L.S. 4 PLAN 1 SIZE 0.34 0.38 0.2 TEMP -103 CONF MORE -1 BOND $H fmap 2 acta OMIT -12 2 10 OMIT -11 7 3 OMIT -10 5 12 OMIT -9 9 8 OMIT -7 1 1 OMIT -4 0 6 OMIT -4 0 16 OMIT -4 1 16 OMIT -3 13 1 OMIT -3 13 3 OMIT -2 2 2 OMIT -2 11 9 OMIT -2 13 2 OMIT -1 13 1 OMIT 0 2 0 OMIT 0 12 0 OMIT 3 8 5 OMIT 7 8 5 OMIT 11 2 3 OMIT 12 0 0 REM REM REM WGHT 0.084900 0.432500 FVAR 0.29570 MO1 3 0.245953 0.256177 0.443685 11.00000 0.01719 0.01511 = 0.01628 0.00014 0.00737 -0.00103 O2 5 0.193577 0.434583 0.471089 11.00000 0.02070 0.01753 = 0.02285 0.00052 0.01037 -0.00087 O3 5 0.372859 0.136512 0.415569 11.00000 0.02849 0.01787 = 0.02915 0.00299 0.01797 0.00220 O4 5 0.202073 0.181914 0.546354 11.00000 0.02408 0.02223 = 0.02263 0.00394 0.01148 0.00034 O1 5 0.274226 0.756266 0.431581 11.00000 0.02466 0.01994 = 0.02981 0.00034 0.01083 -0.00111 AFIX 6 O6 5 0.437045 0.316516 0.598511 11.00000 0.02123 0.03016 = 0.02053 0.00505 0.00391 -0.00402 H6A 2 0.505998 0.364523 0.597910 11.00000 -1.50000 H6B 2 0.464101 0.283599 0.665531 11.00000 -1.50000 AFIX 0 N2 4 0.371570 0.389244 0.377598 11.00000 0.02036 0.01283 = 0.01898 0.00183 0.00701 -0.00051 O5 5 0.106225 0.237046 0.324168 11.00000 0.02664 0.02788 = 0.02456 -0.00377 0.00480 -0.00265 N1 4 0.350033 0.517704 0.393027 11.00000 0.02182 0.01524 = 0.02109 0.00080 0.00805 0.00042 C5 1 0.255095 0.529918 0.440700 11.00000 0.01655 0.01843 = 0.01662 0.00223 0.00301 -0.00171 C10 1 0.581494 -0.002068 0.264707 11.00000 0.02789 0.02317 = 0.02376 -0.00272 0.00847 0.00537 AFIX 43 H10 2 0.608699 -0.083751 0.249055 11.00000 -1.20000 AFIX 0 C8 1 0.452693 0.129043 0.350496 11.00000 0.01887 0.02396 = 0.01558 -0.00060 0.00613 -0.00028 C7 1 0.499389 0.237158 0.308254 11.00000 0.01838 0.02430 = 0.01517 -0.00034 0.00552 -0.00042 C9 1 0.494121 0.009911 0.327918 11.00000 0.02743 0.02012 = 0.02426 0.00003 0.00905 0.00010 AFIX 43 H9 2 0.462623 -0.063163 0.355749 11.00000 -1.20000 AFIX 0 C4 1 0.215006 0.654651 0.465546 11.00000 0.01866 0.01876 = 0.02128 0.00048 0.00303 -0.00126 C11 1 0.630019 0.103881 0.223779 11.00000 0.02388 0.03463 = 0.02042 -0.00097 0.01059 0.00466 AFIX 43 H11 2 0.690214 0.094641 0.180924 11.00000 -1.20000 AFIX 0 C6 1 0.459838 0.363921 0.328018 11.00000 0.02239 0.02041 = 0.01835 0.00367 0.00731 -0.00054 AFIX 43 H6 2 0.501647 0.432496 0.302823 11.00000 -1.20000 AFIX 0 C12 1 0.589831 0.221588 0.246113 11.00000 0.02762 0.02461 = 0.01693 0.00121 0.00966 0.00175 AFIX 43 H12 2 0.623689 0.293936 0.219125 11.00000 -1.20000 AFIX 0 C3 1 0.126057 0.691559 0.517153 11.00000 0.02111 0.02326 = 0.02688 -0.00254 0.01001 -0.00199 AFIX 43 H3 2 0.072393 0.638883 0.547743 11.00000 -1.20000 AFIX 0 C1 1 0.218617 0.859898 0.465840 11.00000 0.03121 0.01594 = 0.03329 -0.00266 0.00001 0.00050 AFIX 43 H1 2 0.241252 0.944715 0.454815 11.00000 -1.20000 AFIX 0 C2 1 0.128494 0.826038 0.516721 11.00000 0.02134 0.02627 = 0.03660 -0.00915 0.00662 0.00510 AFIX 43 H2 2 0.076188 0.880878 0.546779 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_7265_auto_a.res in P2(1)/n REM wR2 = 0.1253, GooF = S = 1.069, Restrained GooF = 1.069 for all data REM R1 = 0.0443 for 2491 Fo > 4sig(Fo) and 0.0466 for all 2725 data REM 193 parameters refined using 1 restraints END WGHT 0.0849 0.4325 REM Highest difference peak 2.098, deepest hole -1.312, 1-sigma level 0.156 Q1 1 0.1753 0.2596 0.4878 11.00000 0.05 2.10 ; _shelx_res_checksum 56273 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 4.290 _oxdiff_exptl_absorpt_empirical_full_min 0.465 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 0.24595(2) 0.25618(2) 0.44369(2) 0.01576(15) Uani 1 1 d D . . . . O2 O 0.1936(2) 0.43458(19) 0.47109(17) 0.0196(4) Uani 1 1 d . . . . . O3 O 0.3729(2) 0.1365(2) 0.4156(2) 0.0231(5) Uani 1 1 d . . . . . O4 O 0.2021(2) 0.1819(2) 0.54635(17) 0.0221(4) Uani 1 1 d . . . . . O1 O 0.2742(3) 0.75627(18) 0.4316(3) 0.0244(6) Uani 1 1 d . . . . . O6 O 0.4370(2) 0.3165(2) 0.59851(18) 0.0248(5) Uani 1 1 d G . . . . H6A H 0.505998 0.364523 0.597910 0.037 Uiso 1 1 d DG U . . . H6B H 0.464101 0.283599 0.665531 0.037 Uiso 1 1 d DG U . . . N2 N 0.3716(3) 0.3892(2) 0.3776(2) 0.0173(5) Uani 1 1 d . . . . . O5 O 0.1062(3) 0.2370(2) 0.3242(2) 0.0273(6) Uani 1 1 d . . . . . N1 N 0.3500(3) 0.5177(2) 0.3930(2) 0.0192(5) Uani 1 1 d . . . . . C5 C 0.2551(3) 0.5299(3) 0.4407(2) 0.0178(6) Uani 1 1 d . . . . . C10 C 0.5815(3) -0.0021(3) 0.2647(3) 0.0250(7) Uani 1 1 d . . . . . H10 H 0.608699 -0.083751 0.249055 0.030 Uiso 1 1 calc R U . . . C8 C 0.4527(3) 0.1290(3) 0.3505(3) 0.0194(6) Uani 1 1 d . . . . . C7 C 0.4994(3) 0.2372(3) 0.3083(3) 0.0193(9) Uani 1 1 d . . . . . C9 C 0.4941(3) 0.0099(3) 0.3279(3) 0.0238(6) Uani 1 1 d . . . . . H9 H 0.462623 -0.063163 0.355749 0.029 Uiso 1 1 calc R U . . . C4 C 0.2150(3) 0.6547(3) 0.4655(3) 0.0205(6) Uani 1 1 d . . . . . C11 C 0.6300(3) 0.1039(3) 0.2238(3) 0.0255(7) Uani 1 1 d . . . . . H11 H 0.690214 0.094641 0.180924 0.031 Uiso 1 1 calc R U . . . C6 C 0.4598(3) 0.3639(3) 0.3280(3) 0.0203(6) Uani 1 1 d . . . . . H6 H 0.501647 0.432496 0.302823 0.024 Uiso 1 1 calc R U . . . C12 C 0.5898(4) 0.2216(3) 0.2461(3) 0.0225(6) Uani 1 1 d . . . . . H12 H 0.623689 0.293936 0.219125 0.027 Uiso 1 1 calc R U . . . C3 C 0.1261(4) 0.6916(3) 0.5172(3) 0.0233(7) Uani 1 1 d . . . . . H3 H 0.072393 0.638883 0.547743 0.028 Uiso 1 1 calc R U . . . C1 C 0.2186(4) 0.8599(3) 0.4658(3) 0.0296(8) Uani 1 1 d . . . . . H1 H 0.241252 0.944715 0.454815 0.035 Uiso 1 1 calc R U . . . C2 C 0.1285(4) 0.8260(3) 0.5167(3) 0.0289(8) Uani 1 1 d . . . . . H2 H 0.076188 0.880878 0.546779 0.035 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 Mo1 0.0172(2) 0.0151(2) 0.0163(2) 0.00014(6) 0.00737(15) -0.00103(7) O2 0.0207(10) 0.0175(10) 0.0228(10) 0.0005(8) 0.0104(8) -0.0009(8) O3 0.0285(11) 0.0179(10) 0.0292(12) 0.0030(9) 0.0180(10) 0.0022(9) O4 0.0241(11) 0.0222(11) 0.0226(10) 0.0039(8) 0.0115(8) 0.0003(9) O1 0.0247(13) 0.0199(14) 0.0298(15) 0.0003(7) 0.0108(12) -0.0011(7) O6 0.0212(10) 0.0302(12) 0.0205(11) 0.0051(9) 0.0039(8) -0.0040(9) N2 0.0204(12) 0.0128(12) 0.0190(12) 0.0018(9) 0.0070(10) -0.0005(9) O5 0.0266(14) 0.0279(13) 0.0246(14) -0.0038(9) 0.0048(11) -0.0026(9) N1 0.0218(12) 0.0152(12) 0.0211(12) 0.0008(9) 0.0080(10) 0.0004(9) C5 0.0165(14) 0.0184(16) 0.0166(14) 0.0022(10) 0.0030(11) -0.0017(10) C10 0.0279(16) 0.0232(16) 0.0238(15) -0.0027(12) 0.0085(13) 0.0054(12) C8 0.0189(14) 0.0240(15) 0.0156(14) -0.0006(11) 0.0061(11) -0.0003(12) C7 0.018(2) 0.0243(19) 0.0152(19) -0.0003(10) 0.0055(16) -0.0004(10) C9 0.0274(15) 0.0201(15) 0.0243(14) 0.0000(12) 0.0090(12) 0.0001(12) C4 0.0187(14) 0.0188(16) 0.0213(15) 0.0005(12) 0.0030(12) -0.0013(12) C11 0.0239(15) 0.0346(18) 0.0204(15) -0.0010(13) 0.0106(12) 0.0047(13) C6 0.0224(15) 0.0204(15) 0.0184(14) 0.0037(11) 0.0073(12) -0.0005(12) C12 0.0276(17) 0.0246(14) 0.0169(14) 0.0012(13) 0.0097(13) 0.0018(14) C3 0.0211(15) 0.0233(17) 0.0269(16) -0.0025(13) 0.0100(13) -0.0020(13) C1 0.0312(18) 0.0159(16) 0.0333(18) -0.0027(13) 0.0000(15) 0.0005(14) C2 0.0213(15) 0.0263(18) 0.0366(19) -0.0092(15) 0.0066(14) 0.0051(14) 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' Mo Mo -0.0483 2.7339 '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' O O 0.0492 0.0322 '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 O6 78.18(8) . . ? O2 Mo1 N2 72.14(9) . . ? O3 Mo1 O2 151.30(9) . . ? O3 Mo1 O6 84.94(9) . . ? O3 Mo1 N2 80.96(10) . . ? O4 Mo1 O2 98.62(9) . . ? O4 Mo1 O3 101.59(10) . . ? O4 Mo1 O6 81.26(9) . . ? O4 Mo1 N2 154.58(10) . . ? O4 Mo1 O5 105.33(12) . . ? N2 Mo1 O6 73.74(9) . . ? O5 Mo1 O2 94.16(10) . . ? O5 Mo1 O3 99.88(12) . . ? O5 Mo1 O6 170.70(10) . . ? O5 Mo1 N2 99.03(12) . . ? C5 O2 Mo1 119.29(18) . . ? C8 O3 Mo1 137.4(2) . . ? C1 O1 C4 105.0(4) . . ? Mo1 O6 H6A 127.0 . . ? Mo1 O6 H6B 127.3 . . ? H6A O6 H6B 104.5 . . ? N1 N2 Mo1 114.98(18) . . ? C6 N2 Mo1 129.0(2) . . ? C6 N2 N1 116.0(3) . . ? C5 N1 N2 109.6(2) . . ? O2 C5 C4 116.2(3) . . ? N1 C5 O2 124.0(3) . . ? N1 C5 C4 119.8(3) . . ? C9 C10 H10 119.5 . . ? C9 C10 C11 121.1(3) . . ? C11 C10 H10 119.5 . . ? O3 C8 C7 122.4(3) . . ? O3 C8 C9 117.9(3) . . ? C9 C8 C7 119.7(3) . . ? C8 C7 C6 122.6(3) . . ? C12 C7 C8 118.9(3) . . ? C12 C7 C6 118.5(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? O1 C4 C5 117.6(3) . . ? C3 C4 O1 111.3(3) . . ? C3 C4 C5 131.1(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11 120.4 . . ? N2 C6 C7 124.0(3) . . ? N2 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C7 C12 H12 119.4 . . ? C11 C12 C7 121.2(3) . . ? C11 C12 H12 119.4 . . ? C4 C3 H3 127.0 . . ? C4 C3 C2 105.9(3) . . ? C2 C3 H3 127.0 . . ? O1 C1 H1 124.4 . . ? C2 C1 O1 111.2(3) . . ? C2 C1 H1 124.4 . . ? C3 C2 H2 126.7 . . ? C1 C2 C3 106.6(3) . . ? C1 C2 H2 126.7 . . ? 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 O2 2.026(2) . ? Mo1 O3 1.928(2) . ? Mo1 O4 1.700(2) . ? Mo1 O6 2.338(2) . ? Mo1 N2 2.246(3) . ? Mo1 O5 1.704(3) . ? O2 C5 1.313(4) . ? O3 C8 1.339(4) . ? O1 C4 1.372(4) . ? O1 C1 1.371(5) . ? O6 H6A 0.8700 . ? O6 H6B 0.8701 . ? N2 N1 1.403(3) . ? N2 C6 1.286(4) . ? N1 C5 1.307(4) . ? C5 C4 1.449(5) . ? C10 H10 0.9500 . ? C10 C9 1.388(4) . ? C10 C11 1.395(5) . ? C8 C7 1.413(5) . ? C8 C9 1.391(5) . ? C7 C6 1.448(4) . ? C7 C12 1.407(5) . ? C9 H9 0.9500 . ? C4 C3 1.341(5) . ? C11 H11 0.9500 . ? C11 C12 1.372(5) . ? C6 H6 0.9500 . ? C12 H12 0.9500 . ? C3 H3 0.9500 . ? C3 C2 1.426(6) . ? C1 H1 0.9500 . ? C1 C2 1.335(6) . ? C2 H2 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 Mo1 O2 C5 N1 -0.1(4) . . . . ? Mo1 O2 C5 C4 -178.46(19) . . . . ? Mo1 O3 C8 C7 23.2(5) . . . . ? Mo1 O3 C8 C9 -159.1(2) . . . . ? Mo1 N2 N1 C5 -2.1(3) . . . . ? Mo1 N2 C6 C7 -2.2(5) . . . . ? O2 C5 C4 O1 -178.0(3) . . . . ? O2 C5 C4 C3 1.4(5) . . . . ? O3 C8 C7 C6 -2.7(5) . . . . ? O3 C8 C7 C12 176.2(3) . . . . ? O3 C8 C9 C10 -177.4(3) . . . . ? O1 C4 C3 C2 -0.2(4) . . . . ? O1 C1 C2 C3 0.8(4) . . . . ? N2 N1 C5 O2 1.5(4) . . . . ? N2 N1 C5 C4 179.9(2) . . . . ? N1 N2 C6 C7 177.7(3) . . . . ? N1 C5 C4 O1 3.6(4) . . . . ? N1 C5 C4 C3 -177.0(3) . . . . ? C5 C4 C3 C2 -179.6(3) . . . . ? C10 C11 C12 C7 -0.8(5) . . . . ? C8 C7 C6 N2 -5.5(5) . . . . ? C8 C7 C12 C11 1.7(5) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C9 C10 C11 C12 -0.3(5) . . . . ? C9 C8 C7 C6 179.7(3) . . . . ? C9 C8 C7 C12 -1.4(5) . . . . ? C4 O1 C1 C2 -0.9(5) . . . . ? C4 C3 C2 C1 -0.3(3) . . . . ? C11 C10 C9 C8 0.6(5) . . . . ? C6 N2 N1 C5 177.9(3) . . . . ? C6 C7 C12 C11 -179.4(3) . . . . ? C12 C7 C6 N2 175.6(3) . . . . ? C1 O1 C4 C5 -179.8(2) . . . . ? C1 O1 C4 C3 0.6(4) . . . . ?