#------------------------------------------------------------------------------ #$Date: 2026-03-04 22:04:27 +0000 (Wed, 04 Mar 2026) $ #$Revision: 304788 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064329.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_7064329 loop_ _publ_author_name Nafisa, 'Rana, Lata' 'Mahiya, Kuldeep' _publ_section_title ; Catalytic oxidation of tetralin by dioxomolybdenum complexes: design, synthesis, characterization and DFT investigations ; _journal_issue 2 _journal_name_full 'New Journal of Chemistry' _journal_page_first 798 _journal_page_last 809 _journal_paper_doi 10.1039/D5NJ04083C _journal_volume 50 _journal_year 2026 _chemical_formula_moiety 'C18 H19 Cl Mo N2 O7 S' _chemical_formula_sum 'C18 H19 Cl Mo N2 O7 S' _chemical_formula_weight 538.80 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2025-06-27 _audit_creation_method ; Olex2 1.5 (compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254) ; _audit_update_record ; 2025-10-12 deposited with the CCDC. 2025-12-09 downloaded from the CCDC. ; _cell_angle_alpha 65.537(2) _cell_angle_beta 79.809(2) _cell_angle_gamma 83.735(2) _cell_formula_units_Z 2 _cell_length_a 8.4494(2) _cell_length_b 11.4162(3) _cell_length_c 12.3491(3) _cell_measurement_reflns_used 15258 _cell_measurement_temperature 293 _cell_measurement_theta_max 68.0530 _cell_measurement_theta_min 3.9500 _cell_volume 1066.30(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _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 11.00 43.00 0.50 0.20 -- 40.83 87.00 179.92 64 2 \w 8.00 35.00 0.50 0.20 -- 40.83 94.00 121.66 54 3 \w 11.00 43.00 0.50 0.20 -- 40.83 85.00-105.46 64 4 \w 12.00 43.00 0.50 0.20 -- 40.83 84.00-141.81 62 5 \w 79.00 162.00 0.50 0.20 -- 96.04 42.00-120.00 166 6 \w 72.00 164.00 0.50 0.20 -- 96.04 68.00 -90.00 184 7 \w 74.00 163.00 0.50 0.20 -- 96.04 59.00 -60.00 178 8 \w 14.00 110.00 0.50 0.20 -- 40.83 77.00 -30.00 192 9 \w 14.00 110.00 0.50 0.20 -- 40.83 77.00 30.00 192 10 \w 72.00 164.00 0.50 0.20 -- 96.04 68.00 150.00 184 11 \w 74.00 163.00 0.50 0.20 -- 96.04 59.00 120.00 178 12 \w 77.00 163.00 0.50 0.20 -- 96.04 50.00 90.00 172 13 \w 74.00 163.00 0.50 0.20 -- 96.04 59.00 60.00 178 14 \w 77.00 163.00 0.50 0.20 -- 96.04 50.00 30.00 172 15 \w 79.00 162.00 0.50 0.20 -- 96.04 42.00 0.00 166 16 \w 79.00 162.00 0.50 0.20 -- 96.04 42.00-150.00 166 17 \w 105.00 170.00 0.50 0.20 -- 96.04 96.00 -30.00 130 18 \w 99.00 160.00 0.50 0.20 -- 96.04 117.00 -60.00 122 19 \w 81.00 164.00 0.50 0.20 -- 96.04 145.00-180.00 166 20 \w 105.00 170.00 0.50 0.20 -- 96.04 96.00 120.00 130 21 \w 99.00 160.00 0.50 0.20 -- 96.04 117.00 150.00 122 22 \w 81.00 164.00 0.50 0.20 -- 96.04 145.00 150.00 166 23 \w 81.00 164.00 0.50 0.20 -- 96.04 145.00 -60.00 166 24 \w 106.00 169.00 0.50 0.20 -- 96.04 97.00-124.00 126 25 \w 27.00 105.00 0.50 0.20 -- 96.04 -77.00-180.00 156 26 \w 28.00 83.00 0.50 0.20 -- 96.04 -68.00-150.00 110 27 \w 28.00 68.00 0.50 0.20 -- 96.04 -59.00-120.00 80 28 \w 29.00 57.00 0.50 0.20 -- 96.04 -50.00 -30.00 56 29 \w 28.00 83.00 0.50 0.20 -- 96.04 -68.00 30.00 110 30 \w 28.00 68.00 0.50 0.20 -- 96.04 -59.00 120.00 80 31 \w 29.00 57.00 0.50 0.20 -- 96.04 -50.00 120.00 56 32 \w 29.00 57.00 0.50 0.20 -- 96.04 -50.00 90.00 56 33 \w 29.00 57.00 0.50 0.20 -- 96.04 -50.00 30.00 56 34 \w 29.00 57.00 0.50 0.20 -- 96.04 -50.00 -60.00 56 35 \w -35.00 24.00 0.50 0.20 -- 40.83 -11.00 -30.00 118 36 \w -7.00 74.00 0.50 0.20 -- 40.83 -97.00 127.00 162 37 \w 41.00 100.00 0.50 0.20 -- 40.83-138.00 90.00 118 38 \w 41.00 100.00 0.50 0.20 -- 40.83-138.00 60.00 118 39 \w 44.00 127.00 0.50 0.20 -- 96.04-145.00 150.00 166 40 \w 44.00 127.00 0.50 0.20 -- 96.04-145.00 60.00 166 41 \w 23.00 106.00 0.50 0.20 -- 96.04 -97.00 127.00 166 42 \w 44.00 127.00 0.50 0.20 -- 96.04-145.00 0.00 166 43 \w 23.00 106.00 0.50 0.20 -- 96.04 -96.00 -30.00 166 44 \w 32.00 110.00 0.50 0.20 -- 96.04-117.00 -60.00 156 45 \w 32.00 110.00 0.50 0.20 -- 96.04-117.00-120.00 156 46 \w 44.00 127.00 0.50 0.20 -- 96.04-145.00-150.00 166 47 \w -28.00 31.00 0.50 0.20 -- -40.83 21.00-150.00 118 48 \w -28.00 31.00 0.50 0.20 -- -40.83 21.00 -30.00 118 49 \w -28.00 31.00 0.50 0.20 -- -40.83 21.00 30.00 118 50 \w -37.00 27.00 0.50 0.20 -- -40.83 32.00 90.00 128 51 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 150.00 64 52 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 60.00 64 53 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 0.00 64 54 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 -90.00 64 55 \w -81.00 -9.00 0.50 0.20 -- -82.50 97.00-124.00 144 56 \w -74.00 29.00 0.50 0.20 -- -40.83 97.00-124.00 206 57 \w -108.00 -17.00 0.50 0.20 -- -40.83 -65.00 -60.00 182 58 \w -108.00 -17.00 0.50 0.20 -- -40.83 -65.00 -90.00 182 59 \w -108.00 -17.00 0.50 0.20 -- -40.83 -65.00 30.00 182 60 \w -109.00 -14.00 0.50 0.20 -- -40.83 -77.00 0.00 190 61 \w -108.00 -17.00 0.50 0.20 -- -40.83 -65.00 90.00 182 62 \w -107.00 -24.00 0.50 0.20 -- -40.83 -43.00 120.00 166 63 \w -107.00 -24.00 0.50 0.20 -- -40.83 -43.00 150.00 166 64 \w -108.00 -21.00 0.50 0.20 -- -40.83 -54.00 30.00 174 65 \w -108.00 -21.00 0.50 0.20 -- -40.83 -54.00-150.00 174 66 \w -153.00 -68.00 0.50 0.20 -- -82.50 -25.00 90.00 170 67 \w -151.00 -55.00 0.50 0.20 -- -82.50 -77.00 168.97 192 68 \w -151.00 -55.00 0.50 0.20 -- -82.50 -77.00 0.00 192 69 \w -151.00 -55.00 0.50 0.20 -- -82.50 -77.00 -30.00 192 70 \w -151.00 -55.00 0.50 0.20 -- -82.50 -77.00-120.00 192 71 \w -153.00 -78.00 0.50 0.20 -- -82.50 -87.00-150.00 150 72 \w -155.00 -84.00 0.50 0.20 -- -82.50 -97.00 127.00 142 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0330787000 _diffrn_orient_matrix_UB_12 -0.0383088000 _diffrn_orient_matrix_UB_13 0.1293413000 _diffrn_orient_matrix_UB_21 -0.1064098000 _diffrn_orient_matrix_UB_22 0.1158947000 _diffrn_orient_matrix_UB_23 0.0069425000 _diffrn_orient_matrix_UB_31 -0.1481735000 _diffrn_orient_matrix_UB_32 -0.0843522000 _diffrn_orient_matrix_UB_33 0.0491284000 _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 0.0415 _diffrn_reflns_av_unetI/netI 0.0232 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 20146 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.088 _diffrn_reflns_theta_min 3.975 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.487 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.16738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.678 _exptl_crystal_description block _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.756 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.063 _refine_ls_extinction_coef 0.0019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 276 _refine_ls_number_reflns 3872 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0291 _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^)+(0.0504P)^2^+0.3656P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.0793 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3697 _reflns_number_total 3872 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d5nj04083c2.cif _cod_data_source_block dm-cloh_auto _cod_database_code 7064329 _shelx_shelxl_version_number 2019/3 _chemical_oxdiff_formula 'C H N O' _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 0.346 _shelx_estimated_absorpt_t_min 0.198 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14), C16(H16) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C) ; _shelx_res_file ; TITL dm-cloh_auto_a.res in P-1 dm-cloh_auto.res created by SHELXL-2019/3 at 10:06:19 on 27-Jun-2025 REM Old TITL DM-CLOH_auto in P1 REM SHELXT solution in P-1: R1 0.164, Rweak 0.018, Alpha 0.057 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N5 O6 Br CELL 1.54184 8.4494 11.4162 12.3491 65.537 79.809 83.735 ZERR 2 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H Cl Mo N O S UNIT 36 38 2 2 4 14 2 L.S. 10 PLAN 2 SIZE 0.18 0.24 0.32 TEMP 19.85 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.050400 0.365600 EXTI 0.001928 FVAR 0.44966 MO1 4 0.242241 0.261325 0.445100 11.00000 0.04475 0.03086 = 0.04196 -0.01158 -0.00810 -0.00915 CL1 3 -0.194649 0.331027 0.989578 11.00000 0.08561 0.08242 = 0.05182 -0.02039 0.01550 0.00205 S1 7 0.643944 0.246984 0.458919 11.00000 0.04377 0.04058 = 0.05498 -0.01451 0.00350 -0.01079 O1 6 0.381697 0.391921 0.312720 11.00000 0.05876 0.03658 = 0.04233 -0.01476 0.00035 -0.01232 O2 6 0.160677 0.178278 0.613474 11.00000 0.04962 0.03345 = 0.04987 -0.01184 -0.00078 -0.01059 O3 6 0.305010 0.136079 0.405096 11.00000 0.07473 0.04073 = 0.06039 -0.02414 -0.01633 -0.00716 O4 6 0.065374 0.315718 0.390633 11.00000 0.05696 0.04823 = 0.06620 -0.01202 -0.02043 -0.00842 O5 6 0.475311 0.217166 0.526300 11.00000 0.03671 0.05087 = 0.04440 -0.01854 -0.00398 -0.00195 O6 6 0.657576 0.922267 0.081645 11.00000 0.05737 0.04041 = 0.04252 -0.01310 0.00843 -0.01674 O7 6 0.798958 0.843482 -0.080279 11.00000 0.05791 0.05251 = 0.03684 -0.01257 0.01027 -0.01620 N1 5 0.250064 0.430000 0.492756 11.00000 0.03707 0.02942 = 0.04053 -0.00844 -0.00195 -0.00901 N2 5 0.339586 0.533147 0.406519 11.00000 0.04544 0.02980 = 0.04297 -0.00813 0.00298 -0.01188 C1 1 0.567598 0.974800 0.161230 11.00000 0.06910 0.03957 = 0.04723 -0.01457 0.00332 -0.00988 AFIX 137 H1A 2 0.593319 1.063236 0.134372 11.00000 -1.50000 H1B 2 0.594138 0.926874 0.240824 11.00000 -1.50000 H1C 2 0.454677 0.969704 0.162145 11.00000 -1.50000 AFIX 0 C2 1 0.868472 0.805180 -0.175216 11.00000 0.08788 0.07522 = 0.04007 -0.02337 0.01539 -0.02096 AFIX 137 H2A 2 0.925182 0.875441 -0.239122 11.00000 -1.50000 H2B 2 0.784943 0.781516 -0.204964 11.00000 -1.50000 H2C 2 0.942063 0.732810 -0.145443 11.00000 -1.50000 AFIX 0 C3 1 0.627167 0.799027 0.102657 11.00000 0.03982 0.03763 = 0.03680 -0.00924 -0.00405 -0.00647 C4 1 0.704472 0.756934 0.013421 11.00000 0.04293 0.04454 = 0.03259 -0.00909 -0.00087 -0.00790 C5 1 0.531740 0.717213 0.201390 11.00000 0.03999 0.03953 = 0.03534 -0.01161 -0.00040 -0.00617 AFIX 43 H5 2 0.483253 0.744240 0.261315 11.00000 -1.20000 AFIX 0 C6 1 0.679571 0.634835 0.024902 11.00000 0.06817 0.05210 = 0.04563 -0.02081 0.00858 -0.01030 AFIX 43 H6 2 0.729161 0.606979 -0.034230 11.00000 -1.20000 AFIX 0 C7 1 0.581188 0.553197 0.123893 11.00000 0.07064 0.04209 = 0.05117 -0.01985 0.00575 -0.01457 AFIX 43 H7 2 0.565203 0.471006 0.130594 11.00000 -1.20000 AFIX 0 C8 1 0.506856 0.592665 0.212452 11.00000 0.04353 0.03645 = 0.03816 -0.00888 -0.00110 -0.00741 C9 1 0.402449 0.504335 0.316501 11.00000 0.04273 0.03469 = 0.04168 -0.01119 -0.00448 -0.00658 C10 1 0.178914 0.443970 0.587353 11.00000 0.04339 0.03320 = 0.04438 -0.01313 -0.00050 -0.00807 AFIX 43 H10 2 0.187731 0.521930 0.592519 11.00000 -1.20000 AFIX 0 C11 1 0.085489 0.345917 0.686898 11.00000 0.03535 0.03693 = 0.03876 -0.00842 -0.00308 -0.00653 C12 1 0.080552 0.218918 0.696904 11.00000 0.03419 0.03827 = 0.04200 -0.00848 -0.00637 -0.00834 C13 1 -0.007287 0.129452 0.798130 11.00000 0.05261 0.04088 = 0.04956 -0.00552 -0.00272 -0.01747 AFIX 43 H13 2 -0.008319 0.045049 0.805609 11.00000 -1.20000 AFIX 0 C14 1 -0.092550 0.163144 0.887291 11.00000 0.04890 0.05872 = 0.04238 -0.00444 0.00255 -0.01565 AFIX 43 H14 2 -0.152536 0.102806 0.953674 11.00000 -1.20000 AFIX 0 C15 1 -0.087778 0.287844 0.876796 11.00000 0.04297 0.05773 = 0.03890 -0.00987 0.00058 -0.00217 C16 1 0.000333 0.378481 0.779156 11.00000 0.04814 0.04356 = 0.04598 -0.01254 -0.00280 -0.00243 AFIX 43 H16 2 0.003233 0.461641 0.774537 11.00000 -1.20000 AFIX 0 C17 1 0.765642 0.155204 0.570937 11.00000 0.03708 0.06395 = 0.08050 -0.02818 -0.01084 -0.00686 AFIX 137 H17A 2 0.762367 0.195619 0.625774 11.00000 -1.50000 H17B 2 0.874549 0.150275 0.533724 11.00000 -1.50000 H17C 2 0.725976 0.069967 0.614032 11.00000 -1.50000 AFIX 0 C18 1 0.684670 0.157059 0.367602 11.00000 0.06646 0.07756 = 0.06245 -0.03624 0.01161 -0.00343 AFIX 137 H18A 2 0.663598 0.068089 0.416544 11.00000 -1.50000 H18B 2 0.795456 0.164723 0.331328 11.00000 -1.50000 H18C 2 0.616850 0.190018 0.305840 11.00000 -1.50000 AFIX 0 HKLF 4 REM dm-cloh_auto_a.res in P-1 REM wR2 = 0.0793, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0291 for 3697 Fo > 4sig(Fo) and 0.0302 for all 3872 data REM 276 parameters refined using 0 restraints END WGHT 0.0504 0.3656 REM Highest difference peak 0.756, deepest hole -0.654, 1-sigma level 0.063 Q1 1 0.5971 0.1227 0.5168 11.00000 0.05 0.76 Q2 1 0.1383 0.2396 0.4585 11.00000 0.05 0.43 ; _shelx_res_checksum 70874 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 4.413 _oxdiff_exptl_absorpt_empirical_full_min 0.625 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Mo1 Mo 0.24224(2) 0.26132(2) 0.44510(2) 0.03938(10) Uani 1 1 d . . . . . Cl1 Cl -0.19465(12) 0.33103(9) 0.98958(7) 0.0794(3) Uani 1 1 d . . . . . S1 S 0.64394(8) 0.24698(6) 0.45892(6) 0.04873(17) Uani 1 1 d . . . . . O1 O 0.3817(2) 0.39192(17) 0.31272(16) 0.0465(4) Uani 1 1 d . . . . . O2 O 0.1607(2) 0.17828(16) 0.61347(16) 0.0461(4) Uani 1 1 d . . . . . O3 O 0.3050(3) 0.13608(18) 0.40510(18) 0.0561(5) Uani 1 1 d . . . . . O4 O 0.0654(2) 0.3157(2) 0.39063(19) 0.0588(5) Uani 1 1 d . . . . . O5 O 0.4753(2) 0.21717(18) 0.52630(15) 0.0445(4) Uani 1 1 d . . . . . O6 O 0.6576(2) 0.92227(17) 0.08164(16) 0.0489(4) Uani 1 1 d . . . . . O7 O 0.7990(2) 0.84348(19) -0.08028(16) 0.0521(5) Uani 1 1 d . . . . . N1 N 0.2501(2) 0.43000(18) 0.49276(18) 0.0375(4) Uani 1 1 d . . . . . N2 N 0.3396(3) 0.53315(19) 0.40652(18) 0.0420(5) Uani 1 1 d . . . . . C1 C 0.5676(4) 0.9748(3) 0.1612(3) 0.0539(7) Uani 1 1 d . . . . . H1A H 0.593319 1.063236 0.134372 0.081 Uiso 1 1 calc R U . . . H1B H 0.594138 0.926874 0.240824 0.081 Uiso 1 1 calc R U . . . H1C H 0.454677 0.969704 0.162145 0.081 Uiso 1 1 calc R U . . . C2 C 0.8685(5) 0.8052(4) -0.1752(3) 0.0695(9) Uani 1 1 d . . . . . H2A H 0.925182 0.875441 -0.239122 0.104 Uiso 1 1 calc R U . . . H2B H 0.784943 0.781516 -0.204964 0.104 Uiso 1 1 calc R U . . . H2C H 0.942063 0.732810 -0.145443 0.104 Uiso 1 1 calc R U . . . C3 C 0.6272(3) 0.7990(2) 0.1027(2) 0.0398(5) Uani 1 1 d . . . . . C4 C 0.7045(3) 0.7569(3) 0.0134(2) 0.0423(5) Uani 1 1 d . . . . . C5 C 0.5317(3) 0.7172(2) 0.2014(2) 0.0398(5) Uani 1 1 d . . . . . H5 H 0.483253 0.744240 0.261315 0.048 Uiso 1 1 calc R U . . . C6 C 0.6796(4) 0.6348(3) 0.0249(3) 0.0565(7) Uani 1 1 d . . . . . H6 H 0.729161 0.606979 -0.034230 0.068 Uiso 1 1 calc R U . . . C7 C 0.5812(4) 0.5532(3) 0.1239(3) 0.0552(7) Uani 1 1 d . . . . . H7 H 0.565203 0.471006 0.130594 0.066 Uiso 1 1 calc R U . . . C8 C 0.5069(3) 0.5927(2) 0.2125(2) 0.0416(5) Uani 1 1 d . . . . . C9 C 0.4024(3) 0.5043(2) 0.3165(2) 0.0409(5) Uani 1 1 d . . . . . C10 C 0.1789(3) 0.4440(2) 0.5874(2) 0.0414(5) Uani 1 1 d . . . . . H10 H 0.187731 0.521930 0.592519 0.050 Uiso 1 1 calc R U . . . C11 C 0.0855(3) 0.3459(2) 0.6869(2) 0.0392(5) Uani 1 1 d . . . . . C12 C 0.0806(3) 0.2189(2) 0.6969(2) 0.0401(5) Uani 1 1 d . . . . . C13 C -0.0073(3) 0.1295(3) 0.7981(2) 0.0513(6) Uani 1 1 d . . . . . H13 H -0.008319 0.045049 0.805609 0.062 Uiso 1 1 calc R U . . . C14 C -0.0926(3) 0.1631(3) 0.8873(2) 0.0555(7) Uani 1 1 d . . . . . H14 H -0.152536 0.102806 0.953674 0.067 Uiso 1 1 calc R U . . . C15 C -0.0878(3) 0.2878(3) 0.8768(2) 0.0506(6) Uani 1 1 d . . . . . C16 C 0.0003(3) 0.3785(3) 0.7792(2) 0.0482(6) Uani 1 1 d . . . . . H16 H 0.003233 0.461641 0.774537 0.058 Uiso 1 1 calc R U . . . C17 C 0.7656(3) 0.1552(3) 0.5709(3) 0.0601(8) Uani 1 1 d . . . . . H17A H 0.762367 0.195619 0.625774 0.090 Uiso 1 1 calc R U . . . H17B H 0.874549 0.150275 0.533724 0.090 Uiso 1 1 calc R U . . . H17C H 0.725976 0.069967 0.614032 0.090 Uiso 1 1 calc R U . . . C18 C 0.6847(4) 0.1571(4) 0.3676(3) 0.0689(9) Uani 1 1 d . . . . . H18A H 0.663598 0.068089 0.416544 0.103 Uiso 1 1 calc R U . . . H18B H 0.795456 0.164723 0.331328 0.103 Uiso 1 1 calc R U . . . H18C H 0.616850 0.190018 0.305840 0.103 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 0.04475(15) 0.03086(13) 0.04196(14) -0.01158(9) -0.00810(9) -0.00915(9) Cl1 0.0856(6) 0.0824(6) 0.0518(4) -0.0204(4) 0.0155(4) 0.0021(5) S1 0.0438(4) 0.0406(3) 0.0550(4) -0.0145(3) 0.0035(3) -0.0108(3) O1 0.0588(11) 0.0366(9) 0.0423(9) -0.0148(8) 0.0004(8) -0.0123(8) O2 0.0496(10) 0.0335(9) 0.0499(10) -0.0118(8) -0.0008(8) -0.0106(7) O3 0.0747(13) 0.0407(10) 0.0604(12) -0.0241(9) -0.0163(10) -0.0072(9) O4 0.0570(12) 0.0482(11) 0.0662(13) -0.0120(10) -0.0204(10) -0.0084(9) O5 0.0367(9) 0.0509(10) 0.0444(9) -0.0185(8) -0.0040(7) -0.0019(8) O6 0.0574(11) 0.0404(10) 0.0425(9) -0.0131(8) 0.0084(8) -0.0167(8) O7 0.0579(11) 0.0525(11) 0.0368(9) -0.0126(8) 0.0103(8) -0.0162(9) N1 0.0371(10) 0.0294(10) 0.0405(10) -0.0084(8) -0.0019(8) -0.0090(8) N2 0.0454(12) 0.0298(10) 0.0430(11) -0.0081(9) 0.0030(9) -0.0119(8) C1 0.0691(19) 0.0396(14) 0.0472(15) -0.0146(12) 0.0033(13) -0.0099(13) C2 0.088(2) 0.075(2) 0.0401(15) -0.0234(15) 0.0154(15) -0.0210(18) C3 0.0398(13) 0.0376(13) 0.0368(12) -0.0092(10) -0.0041(10) -0.0065(10) C4 0.0429(13) 0.0445(14) 0.0326(12) -0.0091(10) -0.0009(10) -0.0079(11) C5 0.0400(13) 0.0395(13) 0.0353(12) -0.0116(10) -0.0004(10) -0.0062(10) C6 0.0682(19) 0.0521(17) 0.0456(15) -0.0208(13) 0.0086(13) -0.0103(14) C7 0.0706(19) 0.0421(15) 0.0512(15) -0.0198(13) 0.0057(14) -0.0146(13) C8 0.0435(13) 0.0364(13) 0.0382(12) -0.0089(10) -0.0011(10) -0.0074(10) C9 0.0427(13) 0.0347(12) 0.0417(13) -0.0112(10) -0.0045(10) -0.0066(10) C10 0.0434(13) 0.0332(12) 0.0444(13) -0.0131(10) -0.0005(10) -0.0081(10) C11 0.0353(12) 0.0369(13) 0.0388(12) -0.0084(10) -0.0031(10) -0.0065(10) C12 0.0342(12) 0.0383(13) 0.0420(12) -0.0085(10) -0.0064(10) -0.0083(10) C13 0.0526(16) 0.0409(14) 0.0496(15) -0.0055(12) -0.0027(12) -0.0175(12) C14 0.0489(16) 0.0587(18) 0.0424(14) -0.0044(13) 0.0025(12) -0.0156(13) C15 0.0430(14) 0.0577(17) 0.0389(13) -0.0099(12) 0.0006(11) -0.0022(12) C16 0.0481(15) 0.0436(14) 0.0460(14) -0.0125(12) -0.0028(11) -0.0024(11) C17 0.0371(14) 0.0639(19) 0.081(2) -0.0282(16) -0.0108(14) -0.0069(13) C18 0.066(2) 0.078(2) 0.0625(19) -0.0362(17) 0.0116(16) -0.0034(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' Cl Cl 0.3639 0.7018 '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' S S 0.3331 0.5567 '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 O1 Mo1 O5 80.05(7) . . ? O1 Mo1 N1 71.64(7) . . ? O2 Mo1 O1 149.48(8) . . ? O2 Mo1 O5 79.30(7) . . ? O2 Mo1 N1 82.28(7) . . ? O3 Mo1 O1 96.61(9) . . ? O3 Mo1 O2 103.54(9) . . ? O3 Mo1 O5 84.61(8) . . ? O3 Mo1 N1 160.48(9) . . ? O4 Mo1 O1 97.52(9) . . ? O4 Mo1 O2 99.14(9) . . ? O4 Mo1 O3 104.86(10) . . ? O4 Mo1 O5 170.48(9) . . ? O4 Mo1 N1 92.36(9) . . ? N1 Mo1 O5 78.13(7) . . ? O5 S1 C17 102.63(13) . . ? O5 S1 C18 107.05(14) . . ? C17 S1 C18 99.18(17) . . ? C9 O1 Mo1 120.67(16) . . ? C12 O2 Mo1 134.74(15) . . ? S1 O5 Mo1 126.91(10) . . ? C3 O6 C1 116.9(2) . . ? C4 O7 C2 116.4(2) . . ? N2 N1 Mo1 115.66(15) . . ? C10 N1 Mo1 127.58(17) . . ? C10 N1 N2 116.7(2) . . ? C9 N2 N1 109.1(2) . . ? O6 C1 H1A 109.5 . . ? O6 C1 H1B 109.5 . . ? O6 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O7 C2 H2A 109.5 . . ? O7 C2 H2B 109.5 . . ? O7 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O6 C3 C4 114.7(2) . . ? O6 C3 C5 125.4(2) . . ? C5 C3 C4 119.9(2) . . ? O7 C4 C3 116.0(2) . . ? O7 C4 C6 124.6(2) . . ? C6 C4 C3 119.4(2) . . ? C3 C5 H5 119.8 . . ? C3 C5 C8 120.3(2) . . ? C8 C5 H5 119.8 . . ? C4 C6 H6 119.8 . . ? C4 C6 C7 120.5(3) . . ? C7 C6 H6 119.8 . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C5 C8 C9 121.2(2) . . ? C7 C8 C5 119.2(2) . . ? C7 C8 C9 119.6(2) . . ? O1 C9 C8 115.2(2) . . ? N2 C9 O1 122.9(2) . . ? N2 C9 C8 121.9(2) . . ? N1 C10 H10 118.0 . . ? N1 C10 C11 124.1(2) . . ? C11 C10 H10 118.0 . . ? C12 C11 C10 123.2(2) . . ? C16 C11 C10 118.1(2) . . ? C16 C11 C12 118.7(2) . . ? O2 C12 C11 122.9(2) . . ? O2 C12 C13 117.8(2) . . ? C13 C12 C11 119.3(2) . . ? C12 C13 H13 119.3 . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13 119.3 . . ? C13 C14 H14 120.5 . . ? C13 C14 C15 119.0(3) . . ? C15 C14 H14 120.5 . . ? C14 C15 Cl1 119.2(2) . . ? C16 C15 Cl1 119.4(2) . . ? C16 C15 C14 121.3(3) . . ? C11 C16 H16 119.9 . . ? C15 C16 C11 120.2(3) . . ? C15 C16 H16 119.9 . . ? S1 C17 H17A 109.5 . . ? S1 C17 H17B 109.5 . . ? S1 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 C18 H18A 109.5 . . ? S1 C18 H18B 109.5 . . ? S1 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 1.9917(18) . ? Mo1 O2 1.9236(18) . ? Mo1 O3 1.7019(19) . ? Mo1 O4 1.697(2) . ? Mo1 O5 2.2806(17) . ? Mo1 N1 2.245(2) . ? Cl1 C15 1.739(3) . ? S1 O5 1.5133(18) . ? S1 C17 1.771(3) . ? S1 C18 1.786(3) . ? O1 C9 1.335(3) . ? O2 C12 1.347(3) . ? O6 C1 1.424(3) . ? O6 C3 1.366(3) . ? O7 C2 1.427(3) . ? O7 C4 1.360(3) . ? N1 N2 1.401(3) . ? N1 C10 1.279(3) . ? N2 C9 1.297(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.410(3) . ? C3 C5 1.372(3) . ? C4 C6 1.377(4) . ? C5 H5 0.9300 . ? C5 C8 1.407(4) . ? C6 H6 0.9300 . ? C6 C7 1.386(4) . ? C7 H7 0.9300 . ? C7 C8 1.377(4) . ? C8 C9 1.472(3) . ? C10 H10 0.9300 . ? C10 C11 1.448(3) . ? C11 C12 1.408(4) . ? C11 C16 1.399(4) . ? C12 C13 1.392(4) . ? C13 H13 0.9300 . ? C13 C14 1.374(4) . ? C14 H14 0.9300 . ? C14 C15 1.379(4) . ? C15 C16 1.377(4) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 O1 C9 N2 2.6(3) . . . . ? Mo1 O1 C9 C8 -179.34(16) . . . . ? Mo1 O2 C12 C11 -23.6(4) . . . . ? Mo1 O2 C12 C13 157.93(19) . . . . ? Mo1 N1 N2 C9 -1.4(2) . . . . ? Mo1 N1 C10 C11 4.1(4) . . . . ? Cl1 C15 C16 C11 -179.2(2) . . . . ? O2 C12 C13 C14 -179.9(2) . . . . ? O6 C3 C4 O7 0.5(3) . . . . ? O6 C3 C4 C6 -178.9(2) . . . . ? O6 C3 C5 C8 178.9(2) . . . . ? O7 C4 C6 C7 179.9(3) . . . . ? N1 N2 C9 O1 -0.6(3) . . . . ? N1 N2 C9 C8 -178.5(2) . . . . ? N1 C10 C11 C12 8.6(4) . . . . ? N1 C10 C11 C16 -173.5(2) . . . . ? N2 N1 C10 C11 -178.1(2) . . . . ? C1 O6 C3 C4 172.7(2) . . . . ? C1 O6 C3 C5 -8.0(4) . . . . ? C2 O7 C4 C3 -175.7(3) . . . . ? C2 O7 C4 C6 3.6(4) . . . . ? C3 C4 C6 C7 -0.8(4) . . . . ? C3 C5 C8 C7 0.9(4) . . . . ? C3 C5 C8 C9 -178.8(2) . . . . ? C4 C3 C5 C8 -1.8(4) . . . . ? C4 C6 C7 C8 -0.1(5) . . . . ? C5 C3 C4 O7 -178.9(2) . . . . ? C5 C3 C4 C6 1.8(4) . . . . ? C5 C8 C9 O1 176.3(2) . . . . ? C5 C8 C9 N2 -5.6(4) . . . . ? C6 C7 C8 C5 0.1(4) . . . . ? C6 C7 C8 C9 179.8(3) . . . . ? C7 C8 C9 O1 -3.4(4) . . . . ? C7 C8 C9 N2 174.7(3) . . . . ? C10 N1 N2 C9 -179.5(2) . . . . ? C10 C11 C12 O2 -1.0(4) . . . . ? C10 C11 C12 C13 177.4(2) . . . . ? C10 C11 C16 C15 -178.8(2) . . . . ? C11 C12 C13 C14 1.6(4) . . . . ? C12 C11 C16 C15 -0.8(4) . . . . ? C12 C13 C14 C15 -1.3(4) . . . . ? C13 C14 C15 Cl1 -179.7(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C11 1.0(4) . . . . ? C16 C11 C12 O2 -179.0(2) . . . . ? C16 C11 C12 C13 -0.5(4) . . . . ? C17 S1 O5 Mo1 -166.84(14) . . . . ? C18 S1 O5 Mo1 -62.97(18) . . . . ?