#------------------------------------------------------------------------------ #$Date: 2026-06-02 23:54:21 +0100 (Tue, 02 Jun 2026) $ #$Revision: 306169 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721067.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_7721067 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 'C13 H12 Mo N2 O6' _chemical_formula_sum 'C13 H12 Mo N2 O6' _chemical_formula_weight 388.19 _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_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 101.188(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.4144(2) _cell_length_b 9.9662(2) _cell_length_c 18.8356(4) _cell_measurement_reflns_used 2232 _cell_measurement_temperature 169.97(10) _cell_measurement_theta_max 78.0580 _cell_measurement_theta_min 4.7510 _cell_volume 1365.38(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _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 169.97(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.984 _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 44.00 111.00 0.50 0.40 -- 113.25-125.00 60.00 134 2 \w 42.00 88.00 0.50 0.10 -- 47.74-125.00 -60.00 92 3 \w 85.00 110.00 0.50 0.40 -- 113.25-125.00-150.00 50 4 \w 79.00 105.00 0.50 0.40 -- 113.25-125.00-180.00 52 5 \w 45.00 77.00 0.50 0.40 -- 113.25-125.00-180.00 64 6 \w 58.00 83.00 0.50 0.40 -- 113.25-125.00-120.00 50 7 \w 45.00 71.00 0.50 0.40 -- 113.25-125.00 -60.00 52 8 \w 86.00 111.00 0.50 0.40 -- 113.25-125.00 -60.00 50 9 \w 86.00 111.00 0.50 0.40 -- 113.25-125.00 0.00 50 10 \w 55.00 80.00 0.50 0.40 -- 113.25-125.00 150.00 50 11 \w 86.00 111.00 0.50 0.40 -- 113.25-125.00 150.00 50 12 \w 69.00 100.00 0.50 0.40 -- 113.25 -95.00 30.00 62 13 \w 53.00 79.00 0.50 0.40 -- 113.25-125.00 0.00 52 14 \w 55.00 98.00 0.50 0.40 -- 113.25 -95.00 -60.00 86 15 \w 58.00 86.00 0.50 0.40 -- 113.25 -95.00-120.00 56 16 \w 69.00 105.00 0.50 0.40 -- 113.25 -95.00-150.00 72 17 \w 43.00 69.00 0.50 0.40 -- 113.25 -95.00 0.00 52 18 \w 44.00 70.00 0.50 0.40 -- 113.25 -95.00 120.00 52 19 \w 45.00 70.00 0.50 0.40 -- 113.25 -95.00 150.00 50 20 \w 81.00 106.00 0.50 0.40 -- 113.25 -95.00 150.00 50 21 \w 44.00 99.00 0.50 0.40 -- 113.25 -95.00 -90.00 110 22 \w 43.00 69.00 0.50 0.40 -- 113.25 -95.00-180.00 52 23 \w 77.00 103.00 0.50 0.40 -- 113.25 -95.00-180.00 52 24 \w 73.00 105.00 0.50 0.40 -- 113.25 -95.00 60.00 64 25 \w 44.00 82.00 0.50 0.40 -- 113.25 -77.00 60.00 76 26 \w 66.00 91.00 0.50 0.40 -- 113.25 -77.00 120.00 50 27 \w 47.00 73.00 0.50 0.40 -- 113.25 -77.00 30.00 52 28 \w 45.00 70.00 0.50 0.40 -- 113.25 -61.00 0.00 50 29 \w 58.00 84.00 0.50 0.40 -- 113.25 -77.00 -30.00 52 30 \w 58.00 84.00 0.50 0.40 -- 113.25 -77.00-180.00 52 31 \w 45.00 70.00 0.50 0.40 -- 113.25 -61.00-120.00 50 32 \w 45.00 105.00 0.50 0.40 -- 113.25 -77.00 -60.00 120 33 \w 44.00 69.00 0.50 0.40 -- 113.25 -61.00 60.00 50 34 \w 44.00 70.00 0.50 0.40 -- 113.25 -61.00 120.00 52 35 \w 42.00 70.00 0.50 0.40 -- 113.25 -61.00 150.00 56 36 \w 112.00 176.00 0.50 0.40 -- 113.25 61.00 -90.00 128 37 \w 103.00 178.00 0.50 0.40 -- 113.25 39.00-110.00 150 38 \w 97.00 124.00 0.50 0.40 -- 113.25 61.00-150.00 54 39 \w 104.00 175.00 0.50 0.40 -- 113.25 45.00 -60.00 142 40 \w 113.00 157.00 0.50 0.40 -- 113.25 45.00 -30.00 88 41 \w 107.00 150.00 0.50 0.40 -- 113.25 45.00 60.00 86 42 \w 102.00 175.00 0.50 0.40 -- 113.25 30.00 30.00 146 43 \w 49.00 119.00 0.50 0.10 -- 47.74 39.00-110.00 140 44 \w 112.00 138.00 0.50 0.40 -- 113.25 30.00-150.00 52 45 \w 144.00 178.00 0.50 0.40 -- 113.25 30.00-150.00 68 46 \w 128.00 168.00 0.50 0.40 -- 113.25 15.00-180.00 80 47 \w 126.00 152.00 0.50 0.40 -- 113.25 125.00-150.00 52 48 \w -15.00 10.00 0.50 0.10 -- 47.74 -39.00 95.00 50 49 \w -20.00 66.00 0.50 0.10 -- 47.74 -77.00 120.00 172 50 \w -27.00 23.00 0.50 0.10 -- 47.74 -19.00 -30.00 100 51 \w -101.00 -34.00 0.50 0.10 -- -47.74 -39.00 95.00 134 52 \w -113.00 -82.00 0.50 0.40 -- -91.75 -39.00 95.00 62 53 \w -51.00 -21.00 0.50 0.40 -- -91.75 45.00 60.00 60 54 \w -59.00 -28.00 0.50 0.40 -- -91.75 125.00 -30.00 62 55 \w -44.00 -18.00 0.50 0.10 -- -47.74 39.00-110.00 52 56 \w -17.00 9.00 0.50 0.10 -- -47.74 39.00-110.00 52 ; _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 -0.1704858000 _diffrn_orient_matrix_UB_12 -0.0755758000 _diffrn_orient_matrix_UB_13 0.0287935000 _diffrn_orient_matrix_UB_21 -0.0875118000 _diffrn_orient_matrix_UB_22 0.0089345000 _diffrn_orient_matrix_UB_23 -0.1620022000 _diffrn_orient_matrix_UB_31 0.0899522000 _diffrn_orient_matrix_UB_32 -0.1346894000 _diffrn_orient_matrix_UB_33 -0.0268497000 _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 0.0537 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 17679 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.055 _diffrn_reflns_theta_min 4.787 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.187 _exptl_absorpt_correction_T_max 0.537 _exptl_absorpt_correction_T_min 0.038 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orangish orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier orangish _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.888 _exptl_crystal_description plate _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.164 _exptl_crystal_size_mid 0.057 _exptl_crystal_size_min 0.025 _refine_diff_density_max 1.349 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 2936 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0446 _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^)+(0.0504P)^2^+3.4152P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1155 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2552 _reflns_number_total 2936 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00558f2.cif _cod_data_source_block exp_7221 _cod_database_code 7721067 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C13 H12 N2 O6 Mo' _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 0.821 _shelx_estimated_absorpt_t_min 0.347 _diffrn_oxdiff_digest_hkl ; 01fd8c943e2133d9dc825d9e12d6af5f9f206c ; _olex2_refinement_description ; 1. Restrained distances H6-O6 0.82 with sigma of 0.02 2.a Aromatic/amide H refined with riding coordinates: C6(H6A), C12(H12), C9(H9), C3(H3), C11(H11), C10(H10), C2(H2), C1(H1) 2.b Idealised Me refined as rotating group: C13(H13A,H13B,H13C) ; _shelx_res_file ; TITL exp_7221_a.res in P2(1)/c exp_7221.res created by SHELXL-2018/3 at 13:05:00 on 22-Jul-2025 REM Old TITL exp_7221 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.096, Rweak 0.004, Alpha 0.043 REM 0.439 for 173 systematic absences, Orientation as input REM Formula found by SHELXT: C12 N1 O4 Mo CELL 1.54184 7.4144 9.9662 18.8356 90 101.188 90 ZERR 4 0.0002 0.0002 0.0004 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Mo N O UNIT 52 48 4 8 24 DFIX 0.82 H6 O6 L.S. 30 PLAN 5 SIZE 0.025 0.057 0.164 TEMP -103 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.050400 3.415200 FVAR 0.39677 MO1 3 0.789073 0.754163 0.581934 11.00000 0.02933 0.01810 = 0.03242 -0.00387 0.00874 -0.00240 O2 5 0.707366 0.604751 0.641279 11.00000 0.03934 0.01858 = 0.03285 -0.00223 0.01233 -0.00228 O3 5 0.802157 0.834419 0.490233 11.00000 0.04612 0.01967 = 0.03703 -0.00130 0.01726 -0.00289 O6 5 0.477271 0.749820 0.537179 11.00000 0.03129 0.02486 = 0.04055 -0.00770 0.00503 0.00376 O1 5 0.617206 0.252519 0.633379 11.00000 0.03829 0.02282 = 0.03850 0.00009 0.01258 -0.00343 O4 5 0.732710 0.885566 0.630859 11.00000 0.04108 0.02438 = 0.03814 -0.00565 0.01013 -0.00316 N1 4 0.694911 0.454606 0.547000 11.00000 0.02620 0.01764 = 0.03426 -0.00009 0.00839 -0.00243 O5 5 1.017556 0.726145 0.612891 11.00000 0.03452 0.02938 = 0.05271 -0.00514 0.00964 -0.00247 N2 4 0.748714 0.568569 0.513320 11.00000 0.02513 0.01568 = 0.03223 -0.00158 0.00621 -0.00112 C4 1 0.636043 0.379803 0.660658 11.00000 0.02643 0.02185 = 0.03540 -0.00051 0.00785 -0.00051 C6 1 0.778475 0.551954 0.449072 11.00000 0.02769 0.01794 = 0.03445 -0.00422 0.00929 0.00121 AFIX 43 H6A 2 0.761349 0.464672 0.428599 11.00000 -1.20000 AFIX 0 C5 1 0.682107 0.483668 0.613163 11.00000 0.02320 0.01955 = 0.03402 -0.00108 0.00926 0.00005 C8 1 0.848575 0.792997 0.428332 11.00000 0.02805 0.02405 = 0.03529 -0.00048 0.00962 -0.00078 C7 1 0.836142 0.656935 0.405947 11.00000 0.02388 0.02308 = 0.03629 0.00230 0.00894 -0.00133 C12 1 0.879084 0.625382 0.338509 11.00000 0.02787 0.03517 = 0.03410 -0.00069 0.00850 0.00437 AFIX 43 H12 2 0.867099 0.535161 0.321987 11.00000 -1.20000 AFIX 0 C9 1 0.910147 0.890346 0.384490 11.00000 0.03314 0.02774 = 0.04251 0.00618 0.01143 -0.00233 AFIX 43 H9 2 0.921930 0.981261 0.399850 11.00000 -1.20000 AFIX 0 C3 1 0.615285 0.382034 0.730159 11.00000 0.03588 0.02343 = 0.03970 -0.00256 0.01491 -0.00007 AFIX 43 H3 2 0.622462 0.458223 0.760890 11.00000 -1.20000 AFIX 0 C11 1 0.937721 0.720780 0.295848 11.00000 0.03332 0.03915 = 0.03712 0.00504 0.01106 0.00491 AFIX 43 H11 2 0.967448 0.696482 0.250718 11.00000 -1.20000 AFIX 0 C10 1 0.953494 0.853676 0.319057 11.00000 0.03028 0.03939 = 0.04158 0.00937 0.01300 -0.00049 AFIX 43 H10 2 0.994535 0.919904 0.289562 11.00000 -1.20000 AFIX 0 C2 1 0.580211 0.246225 0.748273 11.00000 0.04113 0.03500 = 0.03909 0.00663 0.01553 0.00065 AFIX 43 H2 2 0.558513 0.213862 0.793310 11.00000 -1.20000 AFIX 0 C1 1 0.584345 0.174242 0.688506 11.00000 0.04125 0.02182 = 0.05106 0.00753 0.01512 -0.00334 AFIX 43 H1 2 0.566457 0.079895 0.685117 11.00000 -1.20000 AFIX 0 C13 1 0.355201 0.861374 0.530907 11.00000 0.03453 0.02538 = 0.05910 -0.00605 0.01223 0.00262 AFIX 137 H13A 2 0.343442 0.901130 0.482639 11.00000 -1.50000 H13B 2 0.403923 0.928526 0.567652 11.00000 -1.50000 H13C 2 0.234226 0.831239 0.538113 11.00000 -1.50000 AFIX 0 H6 2 0.433971 0.688469 0.510287 11.00000 -1.20000 HKLF 4 REM exp_7221_a.res in P2(1)/c REM wR2 = 0.1155, GooF = S = 1.094, Restrained GooF = 1.094 for all data REM R1 = 0.0446 for 2552 Fo > 4sig(Fo) and 0.0502 for all 2936 data REM 203 parameters refined using 1 restraints END WGHT 0.0504 3.4152 REM Highest difference peak 1.349, deepest hole -1.135, 1-sigma level 0.117 Q1 1 0.8250 0.7289 0.6281 11.00000 0.05 1.35 Q2 1 0.6909 0.7563 0.5379 11.00000 0.05 1.01 Q3 1 0.7792 0.7593 0.5191 11.00000 0.05 0.79 Q4 1 0.5032 0.7544 0.5962 11.00000 0.05 0.62 Q5 1 0.7156 0.8846 0.5781 11.00000 0.05 0.45 ; _shelx_res_checksum 76782 _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 2.226 _oxdiff_exptl_absorpt_empirical_full_min 0.615 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 Mo1 Mo 0.78907(4) 0.75416(3) 0.58193(2) 0.02624(14) Uani 1 1 d . . . . . O2 O 0.7074(4) 0.6048(3) 0.64128(16) 0.0295(6) Uani 1 1 d . . . . . O3 O 0.8022(4) 0.8344(3) 0.49023(17) 0.0330(6) Uani 1 1 d . . . . . O6 O 0.4773(4) 0.7498(3) 0.53718(18) 0.0325(7) Uani 1 1 d D . . . . O1 O 0.6172(5) 0.2525(3) 0.63338(18) 0.0325(6) Uani 1 1 d . . . . . O4 O 0.7327(4) 0.8856(3) 0.63086(17) 0.0342(6) Uani 1 1 d . . . . . N1 N 0.6949(4) 0.4546(3) 0.54700(18) 0.0257(6) Uani 1 1 d . . . . . O5 O 1.0176(5) 0.7261(3) 0.6129(2) 0.0387(7) Uani 1 1 d . . . . . N2 N 0.7487(4) 0.5686(3) 0.51332(18) 0.0243(6) Uani 1 1 d . . . . . C4 C 0.6360(5) 0.3798(4) 0.6607(2) 0.0276(8) Uani 1 1 d . . . . . C6 C 0.7785(5) 0.5520(4) 0.4491(2) 0.0263(8) Uani 1 1 d . . . . . H6A H 0.761349 0.464672 0.428599 0.032 Uiso 1 1 calc R U . . . C5 C 0.6821(5) 0.4837(4) 0.6132(2) 0.0251(7) Uani 1 1 d . . . . . C8 C 0.8486(6) 0.7930(4) 0.4283(2) 0.0287(8) Uani 1 1 d . . . . . C7 C 0.8361(5) 0.6569(4) 0.4059(2) 0.0273(8) Uani 1 1 d . . . . . C12 C 0.8791(6) 0.6254(5) 0.3385(2) 0.0320(9) Uani 1 1 d . . . . . H12 H 0.867099 0.535161 0.321987 0.038 Uiso 1 1 calc R U . . . C9 C 0.9101(6) 0.8903(4) 0.3845(3) 0.0339(9) Uani 1 1 d . . . . . H9 H 0.921930 0.981261 0.399850 0.041 Uiso 1 1 calc R U . . . C3 C 0.6153(6) 0.3820(4) 0.7302(2) 0.0320(9) Uani 1 1 d . . . . . H3 H 0.622462 0.458223 0.760890 0.038 Uiso 1 1 calc R U . . . C11 C 0.9377(6) 0.7208(5) 0.2958(3) 0.0360(9) Uani 1 1 d . . . . . H11 H 0.967448 0.696482 0.250718 0.043 Uiso 1 1 calc R U . . . C10 C 0.9535(6) 0.8537(5) 0.3191(3) 0.0363(9) Uani 1 1 d . . . . . H10 H 0.994535 0.919904 0.289562 0.044 Uiso 1 1 calc R U . . . C2 C 0.5802(7) 0.2462(4) 0.7483(3) 0.0374(10) Uani 1 1 d . . . . . H2 H 0.558513 0.213862 0.793310 0.045 Uiso 1 1 calc R U . . . C1 C 0.5843(6) 0.1742(4) 0.6885(3) 0.0372(10) Uani 1 1 d . . . . . H1 H 0.566457 0.079895 0.685117 0.045 Uiso 1 1 calc R U . . . C13 C 0.3552(6) 0.8614(4) 0.5309(3) 0.0392(10) Uani 1 1 d . . . . . H13A H 0.343442 0.901130 0.482639 0.059 Uiso 1 1 calc R U . . . H13B H 0.403923 0.928526 0.567652 0.059 Uiso 1 1 calc R U . . . H13C H 0.234226 0.831239 0.538113 0.059 Uiso 1 1 calc R U . . . H6 H 0.434(8) 0.688(4) 0.510(3) 0.047 Uiso 1 1 d D 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 0.0293(2) 0.01810(19) 0.0324(2) -0.00387(11) 0.00874(13) -0.00240(10) O2 0.0393(16) 0.0186(12) 0.0328(14) -0.0022(11) 0.0123(12) -0.0023(11) O3 0.0461(17) 0.0197(13) 0.0370(15) -0.0013(11) 0.0173(13) -0.0029(12) O6 0.0313(15) 0.0249(15) 0.0406(17) -0.0077(11) 0.0050(13) 0.0038(11) O1 0.0383(16) 0.0228(14) 0.0385(16) 0.0001(11) 0.0126(13) -0.0034(11) O4 0.0411(16) 0.0244(14) 0.0381(16) -0.0057(12) 0.0101(13) -0.0032(12) N1 0.0262(15) 0.0176(14) 0.0343(17) -0.0001(12) 0.0084(13) -0.0024(12) O5 0.0345(16) 0.0294(14) 0.053(2) -0.0051(14) 0.0096(14) -0.0025(12) N2 0.0251(15) 0.0157(14) 0.0322(16) -0.0016(12) 0.0062(13) -0.0011(11) C4 0.0264(18) 0.0218(18) 0.035(2) -0.0005(15) 0.0079(16) -0.0005(14) C6 0.0277(18) 0.0179(16) 0.034(2) -0.0042(14) 0.0093(15) 0.0012(14) C5 0.0232(17) 0.0196(17) 0.034(2) -0.0011(14) 0.0093(15) 0.0001(13) C8 0.0281(19) 0.0241(18) 0.035(2) -0.0005(16) 0.0096(16) -0.0008(15) C7 0.0239(17) 0.0231(18) 0.036(2) 0.0023(16) 0.0089(15) -0.0013(14) C12 0.0279(19) 0.035(2) 0.034(2) -0.0007(17) 0.0085(16) 0.0044(16) C9 0.033(2) 0.028(2) 0.043(2) 0.0062(17) 0.0114(18) -0.0023(16) C3 0.036(2) 0.0234(19) 0.040(2) -0.0026(16) 0.0149(18) -0.0001(15) C11 0.033(2) 0.039(2) 0.037(2) 0.0050(19) 0.0111(18) 0.0049(18) C10 0.030(2) 0.039(2) 0.042(2) 0.0094(19) 0.0130(18) -0.0005(17) C2 0.041(2) 0.035(2) 0.039(2) 0.0066(18) 0.0155(19) 0.0006(17) C1 0.041(2) 0.0218(19) 0.051(3) 0.0075(18) 0.015(2) -0.0033(16) C13 0.035(2) 0.025(2) 0.059(3) -0.006(2) 0.012(2) 0.0026(17) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0438 0 1 0 0.0132 2 0 -1 0.0549 2 -2 -1 0.0583 -2 -1 0 0.0945 0 0 -1 0.0231 0 0 1 0.0019 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 78.55(12) . . ? O2 Mo1 N2 71.99(11) . . ? O3 Mo1 O2 151.02(12) . . ? O3 Mo1 O6 84.32(13) . . ? O3 Mo1 N2 81.36(12) . . ? O4 Mo1 O2 97.82(14) . . ? O4 Mo1 O3 103.13(13) . . ? O4 Mo1 O6 82.99(13) . . ? O4 Mo1 O5 105.87(16) . . ? O4 Mo1 N2 158.21(14) . . ? O5 Mo1 O2 94.28(15) . . ? O5 Mo1 O3 98.94(16) . . ? O5 Mo1 O6 169.43(13) . . ? O5 Mo1 N2 94.28(14) . . ? N2 Mo1 O6 76.19(11) . . ? C5 O2 Mo1 119.1(2) . . ? C8 O3 Mo1 135.9(3) . . ? Mo1 O6 H6 119(4) . . ? C13 O6 Mo1 126.3(3) . . ? C13 O6 H6 111(4) . . ? C1 O1 C4 105.4(3) . . ? C5 N1 N2 109.5(3) . . ? N1 N2 Mo1 115.3(2) . . ? C6 N2 Mo1 128.5(3) . . ? C6 N2 N1 116.1(3) . . ? O1 C4 C5 116.7(4) . . ? C3 C4 O1 111.0(4) . . ? C3 C4 C5 132.2(4) . . ? N2 C6 H6A 117.9 . . ? N2 C6 C7 124.3(4) . . ? C7 C6 H6A 117.9 . . ? O2 C5 C4 116.0(3) . . ? N1 C5 O2 123.9(3) . . ? N1 C5 C4 120.1(3) . . ? O3 C8 C7 122.6(4) . . ? O3 C8 C9 117.7(4) . . ? C9 C8 C7 119.7(4) . . ? C8 C7 C6 122.5(4) . . ? C12 C7 C6 119.5(4) . . ? C12 C7 C8 118.1(4) . . ? C7 C12 H12 119.0 . . ? C11 C12 C7 121.9(4) . . ? C11 C12 H12 119.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C4 C3 H3 127.0 . . ? C4 C3 C2 106.0(4) . . ? C2 C3 H3 127.0 . . ? C12 C11 H11 120.2 . . ? C12 C11 C10 119.5(4) . . ? C10 C11 H11 120.2 . . ? C9 C10 C11 120.8(4) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C3 C2 H2 127.1 . . ? C1 C2 C3 105.7(4) . . ? C1 C2 H2 127.1 . . ? O1 C1 H1 124.1 . . ? C2 C1 O1 111.8(4) . . ? C2 C1 H1 124.1 . . ? O6 C13 H13A 109.5 . . ? O6 C13 H13B 109.5 . . ? O6 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 O2 2.024(3) . ? Mo1 O3 1.923(3) . ? Mo1 O6 2.302(3) . ? Mo1 O4 1.700(3) . ? Mo1 O5 1.704(3) . ? Mo1 N2 2.243(3) . ? O2 C5 1.317(5) . ? O3 C8 1.343(5) . ? O6 C13 1.424(5) . ? O6 H6 0.82(2) . ? O1 C4 1.366(5) . ? O1 C1 1.358(5) . ? N1 N2 1.396(4) . ? N1 C5 1.301(5) . ? N2 C6 1.282(5) . ? C4 C5 1.452(5) . ? C4 C3 1.348(6) . ? C6 H6A 0.9500 . ? C6 C7 1.439(5) . ? C8 C7 1.418(6) . ? C8 C9 1.406(6) . ? C7 C12 1.404(6) . ? C12 H12 0.9500 . ? C12 C11 1.369(6) . ? C9 H9 0.9500 . ? C9 C10 1.382(7) . ? C3 H3 0.9500 . ? C3 C2 1.432(6) . ? C11 H11 0.9500 . ? C11 C10 1.393(7) . ? C10 H10 0.9500 . ? C2 H2 0.9500 . ? C2 C1 1.340(7) . ? C1 H1 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 Mo1 O2 C5 N1 -4.6(5) . . . . ? Mo1 O2 C5 C4 175.9(3) . . . . ? Mo1 O3 C8 C7 25.4(6) . . . . ? Mo1 O3 C8 C9 -155.2(3) . . . . ? Mo1 N2 C6 C7 -3.9(6) . . . . ? O3 C8 C7 C6 -2.1(6) . . . . ? O3 C8 C7 C12 176.8(4) . . . . ? O3 C8 C9 C10 -177.8(4) . . . . ? O1 C4 C5 O2 -177.3(3) . . . . ? O1 C4 C5 N1 3.2(6) . . . . ? O1 C4 C3 C2 -0.2(5) . . . . ? N1 N2 C6 C7 -179.5(4) . . . . ? N2 N1 C5 O2 3.3(5) . . . . ? N2 N1 C5 C4 -177.2(3) . . . . ? N2 C6 C7 C8 -6.2(6) . . . . ? N2 C6 C7 C12 174.9(4) . . . . ? C4 O1 C1 C2 0.5(5) . . . . ? C4 C3 C2 C1 0.5(5) . . . . ? C6 C7 C12 C11 -178.8(4) . . . . ? C5 N1 N2 Mo1 -0.7(4) . . . . ? C5 N1 N2 C6 175.6(4) . . . . ? C5 C4 C3 C2 -176.7(4) . . . . ? C8 C7 C12 C11 2.3(6) . . . . ? C8 C9 C10 C11 -0.3(7) . . . . ? C7 C8 C9 C10 1.7(6) . . . . ? C7 C12 C11 C10 -0.8(7) . . . . ? C12 C11 C10 C9 -0.2(7) . . . . ? C9 C8 C7 C6 178.5(4) . . . . ? C9 C8 C7 C12 -2.7(6) . . . . ? C3 C4 C5 O2 -0.9(7) . . . . ? C3 C4 C5 N1 179.6(4) . . . . ? C3 C2 C1 O1 -0.6(6) . . . . ? C1 O1 C4 C5 176.9(4) . . . . ? C1 O1 C4 C3 -0.2(5) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0001 -1.0001 0.0009 0.0756 -0.0091 0.1347 0.0001 1.0001 -0.0009 -0.0756 0.0091 -0.1347 1.9999 0.0016 -1.0035 -0.3700 -0.0124 0.2066 1.9997 -1.9986 -1.0017 -0.2187 -0.0306 0.4760 -2.0017 -1.0011 0.0050 0.4171 0.1654 -0.0453 -0.0016 0.0007 -0.9994 -0.0285 0.1621 0.0266 0.0016 -0.0007 0.9994 0.0285 -0.1621 -0.0266