#------------------------------------------------------------------------------ #$Date: 2020-04-13 14:26:14 +0300 (Mon, 13 Apr 2020) $ #$Revision: 250679 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557783.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_1557783 loop_ _publ_author_name 'Meng, Miao' 'Tang, Zheng' 'Mallick, Suman' 'Luo, Ming Hui' 'Tan, Zhibing' 'Liu, Junyang' 'Shi, Jia' 'Yang, Yang' 'Liu, Chun Yuan' 'Hong, Wenjing' _publ_section_title ; Enhanced charge transport via d(\d)-p(\p) conjugation in Mo2-integrated single-molecular junctions ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D0NR00195C _journal_year 2020 _chemical_formula_moiety '2(C42 H39.5 Mo2 N6 O8), 2(C H2 Cl2)' _chemical_formula_sum 'C86 H83 Cl4 Mo4 N12 O16' _chemical_formula_weight 2066.20 _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 geom _audit_creation_date 2018-12-04 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155) ; _audit_update_record ; 2018-12-04 deposited with the CCDC. 2020-04-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.726(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.1713(5) _cell_length_b 14.8958(4) _cell_length_c 22.0423(12) _cell_measurement_reflns_used 6170 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 73.1120 _cell_measurement_theta_min 3.0190 _cell_volume 4770.6(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.969 _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 -14.00 21.00 0.50 4.00 -- 0.00 -57.00 150.00 70 2 \w -19.00 88.00 0.50 4.00 -- 0.00 57.00-150.00 214 3 \w -83.00 -50.00 0.50 4.00 -- 0.00 -57.00 0.00 66 4 \w -1.00 26.00 0.50 4.00 -- 0.00 19.00-180.00 54 5 \w -34.00 -7.00 0.50 4.00 -- 0.00 -57.00 0.00 54 6 \w 76.00 116.00 0.50 35.00 -- 95.20 -61.00 30.00 80 7 \w 77.00 159.00 0.50 35.00 -- 95.20 45.00 0.00 164 8 \w 6.00 110.00 0.50 35.00 -- 95.20 -45.00-150.00 208 9 \w 122.00 184.00 0.50 35.00 -- 95.20 45.00 -30.00 124 10 \w 77.00 104.00 0.50 35.00 -- 95.20 45.00 120.00 54 11 \w 33.00 109.00 0.50 35.00 -- 95.20 -45.00 60.00 152 12 \w 76.00 185.00 0.50 35.00 -- 95.20 45.00 90.00 218 13 \w 22.00 102.00 0.50 35.00 -- 95.20 -30.00 90.00 160 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0635353000 _diffrn_orient_matrix_UB_12 -0.0399079000 _diffrn_orient_matrix_UB_13 -0.0615738000 _diffrn_orient_matrix_UB_21 -0.0846174000 _diffrn_orient_matrix_UB_22 0.0358008000 _diffrn_orient_matrix_UB_23 0.0176216000 _diffrn_orient_matrix_UB_31 0.0054716000 _diffrn_orient_matrix_UB_32 0.0884957000 _diffrn_orient_matrix_UB_33 -0.0350434000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_unetI/netI 0.0635 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 26351 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.212 _diffrn_reflns_theta_min 3.041 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.789 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.59107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.438 _exptl_crystal_description plate _exptl_crystal_F_000 1047 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.586 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.177 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 572 _refine_ls_number_reflns 9419 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.1024 _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^)+(0.1154P)^2^+40.0567P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2697 _refine_ls_wR_factor_ref 0.2860 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6841 _reflns_number_total 9419 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0nr00195c2.cif _cod_data_source_block Mo2_INA _cod_database_code 1557783 _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. ; _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Cl1-C1S = Cl2-C1S = Cl3-C2S = Cl4-C2S 1.78 with sigma of 0.02 Cl1-Cl2 = Cl3-Cl4 2.78 with sigma of 0.02 C14-O1 = C14-O1A 1.35 with sigma of 0.02 O1-C17 = O1A-C17A 1.42 with sigma of 0.02 C14-C17 = C14-C17A 2.35 with sigma of 0.02 3. Rigid bond restraints C14, C15 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 Cl4, Cl5 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 4. Uiso/Uaniso restraints and constraints Cl4 \\sim Cl5: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 : with sigma of 0.02 and sigma for terminal atoms of 0.04 5. Same fragment restrains {Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04 as {Cl3, C2S, Cl4} {Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04 as {Cl5, C3S, Cl6} {Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04 as {Cl7, C4S, Cl8} 6. Others Fixed Sof: O1(0.5) C17(0.5) H17D(0.5) H17E(0.5) H17F(0.5) O1A(0.5) C17A(0.5) Cl1(0.25) C1S(0.25) H1SA(0.25) H1SB(0.25) Cl2(0.25) Cl3(0.25) C2S(0.25) H2SA(0.25) H2SB(0.25) Cl4(0.25) Cl5(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25) Cl6(0.25) Cl7(0.25) C4S(0.25) H4SA(0.25) H4SB(0.25) Cl8(0.25) 7.a Secondary CH2 refined with riding coordinates: C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB) 7.b Me refined with riding coordinates: C17(H17D,H17E,H17F), C17A(H17A,H17B,H17C) 7.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C50(H50) 7.d Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C) ; _shelx_res_file ; Mo2_INA.res created by SHELXL-2014/7 TITL mo2_ina_a.res in P2(1)/c REM Old TITL Mo2_INA in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.198, Rweak 0.007, Alpha 0.156, Orientation as input REM Formula found by SHELXT: c40 N11 o7 Mo2 CELL 1.54184 15.171306 14.895819 22.042261 90 106.7261 90 ZERR 2 0.000504 0.000438 0.001151 0 0.0042 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Mo Cl UNIT 86 83 12 16 4 4 delu 0.001 C14 c15 L.S. 50 PLAN 20 BOND $H ACTA FMAP 2 list 4 delu 0.02 cl4 cl5 simu 0.02 Cl4 cl5 isor 0.02 cl4 cl5 REM REM REM DFIX 1.78 0.02 CL1 C1S CL2 C1S CL3 C2S CL4 C2S DFIX 2.78 0.02 CL1 CL2 CL3 CL4 dfix 1.35 0.02 C14 O1 C14 O1A DFIX 1.42 0.02 O1 C17 O1A C17A DFIX 2.35 0.02 c14 c17 c14 c17A WGHT 0.115400 40.056705 FVAR 0.12968 MO1 5 0.204592 0.574348 0.255960 11.00000 0.03263 0.02952 = 0.05862 0.00035 0.01393 -0.00203 MO2 5 0.299286 0.678632 0.252669 11.00000 0.03308 0.02892 = 0.05979 -0.00001 0.01562 -0.00299 N1 3 0.247426 0.575036 0.357490 11.00000 0.05059 0.03485 = 0.06503 -0.00341 0.01586 -0.00979 N2 3 0.352422 0.685553 0.353149 11.00000 0.04203 0.03349 = 0.05752 -0.00821 0.01390 -0.00645 N3 3 0.155654 0.567296 0.154068 11.00000 0.04206 0.04186 = 0.05157 -0.00528 0.00725 -0.00457 N4 3 0.253090 0.682342 0.151591 11.00000 0.04650 0.03402 = 0.06268 0.00324 0.01942 -0.00375 N5 3 0.583478 0.301605 0.252103 11.00000 0.05558 0.05300 = 0.07468 0.00267 0.01974 0.01864 N6 3 -0.084969 0.952068 0.234919 11.00000 0.04469 0.03865 = 0.07482 0.00545 0.01813 0.01151 O5 4 0.303080 0.474565 0.256767 11.00000 0.04112 0.02948 = 0.06178 0.00044 0.01176 -0.00013 O6 4 0.400906 0.583392 0.250163 11.00000 0.04367 0.02783 = 0.05698 0.00229 0.01956 -0.00009 O7 4 0.100460 0.670980 0.253118 11.00000 0.03536 0.03154 = 0.06233 -0.00693 0.01401 0.00309 O8 4 0.201669 0.779955 0.253590 11.00000 0.03919 0.02691 = 0.06286 -0.00084 0.01913 0.00261 C1 1 0.316553 0.630275 0.387651 11.00000 0.06138 0.04689 = 0.04698 0.00128 0.00882 -0.00116 AFIX 43 H1 2 0.338893 0.629968 0.431614 11.00000 -1.20000 AFIX 0 C2 1 0.189138 0.624440 0.120720 11.00000 0.04265 0.04517 = 0.05704 -0.00150 0.01548 -0.00283 AFIX 43 H2 2 0.168543 0.624262 0.076692 11.00000 -1.20000 AFIX 0 C3 1 0.382270 0.500802 0.253215 11.00000 0.03184 0.03867 = 0.05245 -0.00128 0.00759 -0.00467 C4 1 0.450774 0.432429 0.253426 11.00000 0.03889 0.03733 = 0.06416 0.00165 0.01647 0.00760 C5 1 0.438421 0.343262 0.268092 11.00000 0.04244 0.04425 = 0.07773 0.00157 0.02155 0.00514 AFIX 43 H5 2 0.385465 0.325073 0.277864 11.00000 -1.20000 AFIX 0 C6 1 0.507154 0.282589 0.267701 11.00000 0.06466 0.03964 = 0.07959 -0.00221 0.02482 0.01150 AFIX 43 H6 2 0.499414 0.223727 0.279276 11.00000 -1.20000 AFIX 0 C7 1 0.595264 0.388245 0.238982 11.00000 0.04272 0.04018 = 0.10417 -0.00477 0.02531 0.00796 AFIX 43 H7 2 0.649488 0.404364 0.230128 11.00000 -1.20000 AFIX 0 C8 1 0.531675 0.454016 0.237962 11.00000 0.04233 0.03933 = 0.09002 -0.00088 0.02772 0.00179 AFIX 43 H8 2 0.542106 0.512564 0.227089 11.00000 -1.20000 AFIX 0 C9 1 0.121229 0.752516 0.251344 11.00000 0.03474 0.04870 = 0.06208 -0.00189 0.01453 0.01506 C10 1 0.049454 0.822335 0.245925 11.00000 0.04518 0.03953 = 0.05735 -0.00434 0.00925 0.00121 C11 1 0.216613 0.510644 0.395245 11.00000 0.09360 0.08496 = 0.05693 0.00036 0.01337 -0.04461 C12 1 0.131298 0.518010 0.402640 11.00000 0.16581 0.12473 = 0.11050 -0.02627 0.09207 -0.06960 AFIX 43 H12 2 0.096312 0.569090 0.388174 11.00000 -1.20000 AFIX 0 C13 1 0.095743 0.450123 0.431558 11.00000 0.21248 0.20369 = 0.13364 -0.02661 0.09710 -0.13365 AFIX 43 H13 2 0.035172 0.454320 0.432900 11.00000 -1.20000 AFIX 0 C14 1 0.144248 0.381033 0.456766 11.00000 0.33841 0.12533 = 0.11744 0.01052 0.09710 -0.12185 C15 1 0.233283 0.374618 0.454022 11.00000 0.26882 0.15569 = 0.10228 0.05307 -0.00697 -0.12724 AFIX 43 H15 2 0.269606 0.326159 0.472813 11.00000 -1.20000 AFIX 0 C16 1 0.269688 0.441149 0.422865 11.00000 0.12338 0.07810 = 0.10079 0.02722 -0.01330 -0.02786 AFIX 43 H16 2 0.330196 0.437110 0.421365 11.00000 -1.20000 AFIX 0 PART 1 O1 4 0.107070 0.316324 0.487083 10.50000 0.11977 C17 1 0.009800 0.308021 0.465445 10.50000 0.15203 AFIX 33 H17D 2 -0.009716 0.261781 0.489055 10.50000 -1.50000 H17E 2 -0.017986 0.363993 0.471373 10.50000 -1.50000 H17F 2 -0.008676 0.292675 0.421277 10.50000 -1.50000 AFIX 0 PART 2 O1A 4 0.098159 0.323526 0.485118 10.50000 0.40864 C17A 1 0.141333 0.238323 0.498899 10.50000 0.30562 AFIX 33 PART 0 H17A 2 0.106080 0.200882 0.518687 11.00000 -1.50000 H17B 2 0.144820 0.210684 0.460313 11.00000 -1.50000 H17C 2 0.202279 0.245818 0.527012 11.00000 -1.50000 AFIX 0 C20 1 -0.042058 0.799152 0.227922 11.00000 0.04769 0.04334 = 0.08690 -0.00749 0.01240 0.01179 AFIX 43 H20 2 -0.059851 0.739752 0.218807 11.00000 -1.20000 AFIX 0 C21 1 0.419909 0.748084 0.386919 11.00000 0.05546 0.05019 = 0.05890 -0.00530 0.01176 -0.00711 C22 1 0.396906 0.820601 0.417661 11.00000 0.06879 0.05246 = 0.07001 -0.01383 0.02011 -0.02086 AFIX 43 H22 2 0.337313 0.825511 0.420894 11.00000 -1.20000 AFIX 0 C23 1 0.460096 0.885896 0.443677 11.00000 0.09511 0.05161 = 0.08876 -0.02060 0.02896 -0.02175 AFIX 43 H23 2 0.443431 0.933924 0.464994 11.00000 -1.20000 AFIX 0 C24 1 0.548103 0.880650 0.438372 11.00000 0.06697 0.06599 = 0.07252 -0.01508 0.00206 -0.02227 C25 1 0.573517 0.804748 0.410197 11.00000 0.04702 0.05821 = 0.11068 -0.01012 0.00983 -0.01688 AFIX 43 H25 2 0.633882 0.797904 0.408906 11.00000 -1.20000 AFIX 0 C26 1 0.508312 0.739687 0.384174 11.00000 0.04700 0.04899 = 0.09966 -0.00724 0.00933 -0.01290 AFIX 43 H26 2 0.524937 0.689761 0.364626 11.00000 -1.20000 AFIX 0 O2 4 0.607136 0.949927 0.463260 11.00000 0.10090 0.08413 = 0.11238 -0.02285 0.01039 -0.05577 C27 1 0.687804 0.955938 0.445613 11.00000 0.07107 0.12049 = 0.13883 0.01556 -0.00175 -0.04839 AFIX 137 H27A 2 0.672915 0.962733 0.400480 11.00000 -1.50000 H27B 2 0.723465 0.902314 0.458252 11.00000 -1.50000 H27C 2 0.722760 1.006918 0.465916 11.00000 -1.50000 AFIX 0 C30 1 -0.106733 0.864969 0.223608 11.00000 0.04429 0.05558 = 0.08885 -0.01086 0.01781 0.01190 AFIX 43 H30 2 -0.168488 0.848614 0.212340 11.00000 -1.20000 AFIX 0 C31 1 0.082068 0.510153 0.121329 11.00000 0.04801 0.04847 = 0.05837 0.00075 0.00893 -0.01027 C32 1 0.087189 0.418057 0.127038 11.00000 0.04688 0.05010 = 0.08212 -0.00956 0.01025 0.00461 AFIX 43 H32 2 0.142713 0.391308 0.148706 11.00000 -1.20000 AFIX 0 C33 1 0.011137 0.364879 0.101077 11.00000 0.06201 0.05323 = 0.08845 -0.01000 0.01773 -0.01483 AFIX 43 H33 2 0.016457 0.302891 0.105742 11.00000 -1.20000 AFIX 0 C34 1 -0.070310 0.400543 0.069259 11.00000 0.05492 0.05998 = 0.06423 0.00000 0.00412 -0.01767 C35 1 -0.075660 0.495024 0.061373 11.00000 0.06654 0.06920 = 0.11312 0.02069 -0.01026 -0.02183 AFIX 43 H35 2 -0.130835 0.521420 0.038644 11.00000 -1.20000 AFIX 0 C36 1 -0.001013 0.547065 0.086699 11.00000 0.06309 0.05660 = 0.10841 0.02123 -0.00366 -0.01300 AFIX 43 H36 2 -0.005569 0.608889 0.080737 11.00000 -1.20000 AFIX 0 O3 4 -0.149510 0.354299 0.042342 11.00000 0.07400 0.09041 = 0.09716 0.00921 -0.00765 -0.04260 C37 1 -0.151567 0.262713 0.057293 11.00000 0.09276 0.07943 = 0.09915 -0.01159 0.01262 -0.03902 AFIX 137 H37A 2 -0.214034 0.241727 0.044424 11.00000 -1.50000 H37B 2 -0.126154 0.254658 0.102159 11.00000 -1.50000 H37C 2 -0.115917 0.229219 0.035506 11.00000 -1.50000 AFIX 0 C40 1 0.072318 0.910407 0.257417 11.00000 0.04219 0.04744 = 0.09431 0.00625 0.02278 0.00636 AFIX 43 H40 2 0.133747 0.927899 0.268673 11.00000 -1.20000 AFIX 0 C41 1 0.292619 0.743259 0.115908 11.00000 0.05503 0.04259 = 0.05579 0.00376 0.02130 -0.00562 C42 1 0.359546 0.715168 0.088924 11.00000 0.05745 0.05145 = 0.06484 0.00202 0.02618 -0.00460 AFIX 43 H42 2 0.372430 0.654330 0.087267 11.00000 -1.20000 AFIX 0 C43 1 0.407055 0.777295 0.064530 11.00000 0.06467 0.06153 = 0.07012 0.00086 0.03189 -0.00368 AFIX 43 H43 2 0.451395 0.758430 0.045684 11.00000 -1.20000 AFIX 0 C44 1 0.388899 0.868317 0.068001 11.00000 0.06015 0.05984 = 0.07076 0.00573 0.02683 -0.01673 C45 1 0.319194 0.896190 0.090792 11.00000 0.08131 0.04535 = 0.09016 0.01024 0.03950 -0.00958 AFIX 43 H45 2 0.303891 0.956716 0.090080 11.00000 -1.20000 AFIX 0 C46 1 0.271568 0.833598 0.114939 11.00000 0.07975 0.04503 = 0.08681 0.00983 0.03991 0.00151 AFIX 43 H46 2 0.224242 0.852521 0.130931 11.00000 -1.20000 AFIX 0 O4 4 0.443501 0.925107 0.045176 11.00000 0.10370 0.08023 = 0.07793 -0.00870 0.04347 -0.04809 C47 1 0.450592 1.015059 0.066441 11.00000 0.11084 0.06801 = 0.09767 0.00814 0.03129 -0.03269 AFIX 137 H47A 2 0.391173 1.043101 0.052759 11.00000 -1.50000 H47B 2 0.492803 1.046955 0.049150 11.00000 -1.50000 H47C 2 0.472619 1.016220 0.111858 11.00000 -1.50000 AFIX 0 C50 1 0.004595 0.973111 0.252348 11.00000 0.03710 0.03822 = 0.11857 0.00201 0.02557 0.00444 AFIX 43 H50 2 0.021504 1.032737 0.261380 11.00000 -1.20000 AFIX 0 PART 1 CL1 6 -0.307239 0.631879 0.320795 10.25000 0.10668 C1S 1 -0.198748 0.677334 0.357746 10.25000 0.11064 AFIX 23 H1SA 2 -0.195014 0.698197 0.400099 10.25000 -1.20000 H1SB 2 -0.185162 0.726962 0.333389 10.25000 -1.20000 AFIX 0 CL2 6 -0.121563 0.585284 0.360236 10.25000 0.15099 PART 2 SAME 0.02 CL1 > CL2 CL3 6 -0.402982 0.637667 0.127980 10.25000 0.09596 C2S 1 -0.305304 0.571803 0.162681 10.25000 0.13710 AFIX 23 H2SA 2 -0.313639 0.510777 0.146691 10.25000 -1.20000 H2SB 2 -0.292055 0.570561 0.208429 10.25000 -1.20000 AFIX 0 CL4 6 -0.215040 0.627648 0.139295 10.25000 0.20456 PART 3 SAME 0.02 CL1 > CL2 CL5 6 -0.327443 0.715949 0.113663 10.25000 0.19081 C3S 1 -0.361144 0.604830 0.119878 10.25000 0.12141 AFIX 23 H3SA 2 -0.408142 0.586267 0.081942 10.25000 -1.20000 H3SB 2 -0.384273 0.597052 0.156241 10.25000 -1.20000 AFIX 0 CL6 6 -0.255862 0.542834 0.129427 10.25000 0.24257 PART 4 SAME 0.02 CL1 > CL2 CL7 6 -0.294220 0.639029 0.343320 10.25000 0.14178 C4S 1 -0.217880 0.706067 0.318876 10.25000 0.08529 AFIX 23 H4SA 2 -0.203856 0.760404 0.344076 10.25000 -1.20000 H4SB 2 -0.242429 0.722254 0.274579 10.25000 -1.20000 AFIX 0 CL8 6 -0.115848 0.634914 0.331482 10.25000 0.11220 PART 0 HKLF 4 REM mo2_ina_a.res in P2(1)/c REM R1 = 0.1024 for 6841 Fo > 4sig(Fo) and 0.1257 for all 9419 data REM 572 parameters refined using 31 restraints END WGHT 0.1392 38.6108 REM Highest difference peak 2.586, deepest hole -1.490, 1-sigma level 0.177 Q1 1 0.3195 0.6795 0.2996 11.00000 0.05 2.59 Q2 1 0.2468 0.6233 0.2496 11.00000 0.05 2.38 Q3 1 0.1839 0.5802 0.2063 11.00000 0.05 2.31 Q4 1 0.2236 0.5774 0.3028 11.00000 0.05 2.23 Q5 1 0.2734 0.6777 0.2024 11.00000 0.05 1.98 Q6 1 -0.2233 0.6011 0.1825 11.00000 0.05 1.61 Q7 1 0.1525 0.6264 0.2495 11.00000 0.05 1.60 Q8 1 -0.2664 0.6983 0.3193 11.00000 0.05 1.54 Q9 1 0.2556 0.7281 0.2497 11.00000 0.05 1.38 Q10 1 0.3477 0.7288 0.2579 11.00000 0.05 1.29 Q11 1 0.2542 0.5175 0.2619 11.00000 0.05 1.20 Q12 1 -0.1715 0.5422 0.3409 11.00000 0.05 1.18 Q13 1 0.2566 0.6336 0.2885 11.00000 0.05 1.13 Q14 1 0.1529 0.5146 0.2477 11.00000 0.05 1.10 Q15 1 0.1107 0.5796 0.2467 11.00000 0.05 1.09 Q16 1 -0.3713 0.6615 0.1587 11.00000 0.05 1.07 Q17 1 0.3553 0.6187 0.2585 11.00000 0.05 1.06 Q18 1 -0.0946 0.6173 0.3559 11.00000 0.05 1.01 Q19 1 -0.3743 0.6838 0.1302 11.00000 0.05 1.01 Q20 1 0.2955 0.5788 0.2530 11.00000 0.05 0.97 ; _shelx_res_checksum 177 _shelx_shelxl_version_number 2014/7 _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 1.973 _oxdiff_exptl_absorpt_empirical_full_min 0.692 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 0.20459(5) 0.57435(5) 0.25596(4) 0.0401(2) Uani 1 1 d . . . . . Mo2 Mo 0.29929(4) 0.67863(5) 0.25267(4) 0.0401(2) Uani 1 1 d . . . . . N1 N 0.2474(6) 0.5750(5) 0.3575(4) 0.0503(19) Uani 1 1 d . . . . . N2 N 0.3524(5) 0.6856(5) 0.3531(4) 0.0444(17) Uani 1 1 d . . . . . N3 N 0.1557(5) 0.5673(5) 0.1541(4) 0.0465(18) Uani 1 1 d . . . . . N4 N 0.2531(5) 0.6823(5) 0.1516(4) 0.0470(18) Uani 1 1 d . . . . . N5 N 0.5835(6) 0.3016(6) 0.2521(5) 0.061(2) Uani 1 1 d . . . . . N6 N -0.0850(6) 0.9521(5) 0.2349(4) 0.053(2) Uani 1 1 d . . . . . O5 O 0.3031(4) 0.4746(4) 0.2568(3) 0.0448(14) Uani 1 1 d . . . . . O6 O 0.4009(4) 0.5834(4) 0.2502(3) 0.0418(13) Uani 1 1 d . . . . . O7 O 0.1005(4) 0.6710(4) 0.2531(3) 0.0431(14) Uani 1 1 d . . . . . O8 O 0.2017(4) 0.7800(4) 0.2536(3) 0.0421(14) Uani 1 1 d . . . . . C1 C 0.3166(7) 0.6303(7) 0.3877(5) 0.053(2) Uani 1 1 d . . . . . H1 H 0.3389 0.6300 0.4316 0.064 Uiso 1 1 calc R . . . . C2 C 0.1891(6) 0.6244(6) 0.1207(5) 0.048(2) Uani 1 1 d . . . . . H2 H 0.1685 0.6243 0.0767 0.058 Uiso 1 1 calc R . . . . C3 C 0.3823(6) 0.5008(6) 0.2532(4) 0.0419(19) Uani 1 1 d . . . . . C4 C 0.4508(6) 0.4324(6) 0.2534(5) 0.046(2) Uani 1 1 d . . . . . C5 C 0.4384(7) 0.3433(7) 0.2681(5) 0.054(2) Uani 1 1 d . . . . . H5 H 0.3855 0.3251 0.2779 0.065 Uiso 1 1 calc R . . . . C6 C 0.5072(8) 0.2826(7) 0.2677(6) 0.060(3) Uani 1 1 d . . . . . H6 H 0.4994 0.2237 0.2793 0.073 Uiso 1 1 calc R . . . . C7 C 0.5953(7) 0.3882(7) 0.2390(6) 0.061(3) Uani 1 1 d . . . . . H7 H 0.6495 0.4044 0.2301 0.074 Uiso 1 1 calc R . . . . C8 C 0.5317(7) 0.4540(7) 0.2380(6) 0.055(3) Uani 1 1 d . . . . . H8 H 0.5421 0.5126 0.2271 0.066 Uiso 1 1 calc R . . . . C9 C 0.1212(6) 0.7525(7) 0.2513(5) 0.048(2) Uani 1 1 d . . . . . C10 C 0.0495(7) 0.8223(6) 0.2459(5) 0.049(2) Uani 1 1 d . . . . . C11 C 0.2166(10) 0.5106(10) 0.3952(6) 0.080(4) Uani 1 1 d . . . . . C12 C 0.1313(15) 0.5180(13) 0.4026(8) 0.123(7) Uani 1 1 d . . . . . H12 H 0.0963 0.5691 0.3882 0.147 Uiso 1 1 calc R . . . . C13 C 0.096(2) 0.450(2) 0.4316(12) 0.173(13) Uani 1 1 d . . . . . H13 H 0.0352 0.4543 0.4329 0.208 Uiso 1 1 calc R . . . . C14 C 0.144(3) 0.3810(18) 0.4568(12) 0.187(11) Uani 1 1 d D U . . . C15 C 0.233(2) 0.3746(17) 0.4540(10) 0.188(11) Uani 1 1 d . U . . . H15 H 0.2696 0.3262 0.4728 0.226 Uiso 1 1 calc R . . . . C16 C 0.2697(13) 0.4411(11) 0.4229(8) 0.110(6) Uani 1 1 d . . . . . H16 H 0.3302 0.4371 0.4214 0.132 Uiso 1 1 calc R . . . . O1 O 0.1071(18) 0.3163(17) 0.4871(15) 0.120(10) Uiso 0.5 1 d D . P A 1 C17 C 0.0098(19) 0.308(3) 0.465(2) 0.152(17) Uiso 0.5 1 d D . P A 1 H17D H -0.0097 0.2618 0.4891 0.228 Uiso 0.5 1 calc R . P A 1 H17E H -0.0180 0.3640 0.4714 0.228 Uiso 0.5 1 calc R . P A 1 H17F H -0.0087 0.2927 0.4213 0.228 Uiso 0.5 1 calc R . P A 1 O1A O 0.098(5) 0.324(4) 0.485(5) 0.41(6) Uiso 0.5 1 d D . P A 2 C17A C 0.141(5) 0.238(3) 0.499(4) 0.31(4) Uiso 0.5 1 d D . P A 2 H17A H 0.1061 0.2009 0.5187 0.458 Uiso 1 1 calc R . . A . H17B H 0.1448 0.2107 0.4603 0.458 Uiso 1 1 calc R . . A . H17C H 0.2023 0.2458 0.5270 0.458 Uiso 1 1 calc R . . A . C20 C -0.0421(7) 0.7992(7) 0.2279(6) 0.061(3) Uani 1 1 d . . . . . H20 H -0.0599 0.7398 0.2188 0.073 Uiso 1 1 calc R . . . . C21 C 0.4199(7) 0.7481(7) 0.3869(5) 0.056(2) Uani 1 1 d . . . . . C22 C 0.3969(8) 0.8206(7) 0.4177(5) 0.064(3) Uani 1 1 d . . . . . H22 H 0.3373 0.8255 0.4209 0.076 Uiso 1 1 calc R . . . . C23 C 0.4601(10) 0.8859(8) 0.4437(6) 0.078(4) Uani 1 1 d . . . . . H23 H 0.4434 0.9339 0.4650 0.094 Uiso 1 1 calc R . . . . C24 C 0.5481(9) 0.8807(9) 0.4384(6) 0.072(3) Uani 1 1 d . . . . . C25 C 0.5735(8) 0.8047(8) 0.4102(7) 0.075(4) Uani 1 1 d . . . . . H25 H 0.6339 0.7979 0.4089 0.090 Uiso 1 1 calc R . . . . C26 C 0.5083(7) 0.7397(8) 0.3842(6) 0.068(3) Uani 1 1 d . . . . . H26 H 0.5249 0.6898 0.3646 0.081 Uiso 1 1 calc R . . . . O2 O 0.6071(8) 0.9499(7) 0.4633(5) 0.103(3) Uani 1 1 d . . . . . C27 C 0.6878(11) 0.9559(13) 0.4456(9) 0.117(6) Uani 1 1 d . . . . . H27A H 0.6729 0.9627 0.4005 0.175 Uiso 1 1 calc GR . . . . H27B H 0.7235 0.9023 0.4583 0.175 Uiso 1 1 calc GR . . . . H27C H 0.7228 1.0069 0.4659 0.175 Uiso 1 1 calc GR . . . . C30 C -0.1067(7) 0.8650(8) 0.2236(6) 0.063(3) Uani 1 1 d . . . . . H30 H -0.1685 0.8486 0.2123 0.076 Uiso 1 1 calc R . . . . C31 C 0.0821(7) 0.5102(7) 0.1213(5) 0.053(2) Uani 1 1 d . . . . . C32 C 0.0872(7) 0.4181(7) 0.1270(6) 0.061(3) Uani 1 1 d . . . . . H32 H 0.1427 0.3913 0.1487 0.074 Uiso 1 1 calc R . . . . C33 C 0.0111(8) 0.3649(8) 0.1011(6) 0.069(3) Uani 1 1 d . . . . . H33 H 0.0165 0.3029 0.1057 0.082 Uiso 1 1 calc R . . . . C34 C -0.0703(8) 0.4005(8) 0.0693(5) 0.062(3) Uani 1 1 d . . . . . C35 C -0.0757(10) 0.4950(9) 0.0614(7) 0.091(5) Uani 1 1 d . . . . . H35 H -0.1308 0.5214 0.0386 0.109 Uiso 1 1 calc R . . . . C36 C -0.0010(9) 0.5471(9) 0.0867(7) 0.082(4) Uani 1 1 d . . . . . H36 H -0.0056 0.6089 0.0807 0.098 Uiso 1 1 calc R . . . . O3 O -0.1495(6) 0.3543(7) 0.0423(5) 0.094(3) Uani 1 1 d . . . . . C37 C -0.1516(11) 0.2627(10) 0.0573(7) 0.094(5) Uani 1 1 d . . . . . H37A H -0.2140 0.2417 0.0444 0.140 Uiso 1 1 calc GR . . . . H37B H -0.1262 0.2547 0.1022 0.140 Uiso 1 1 calc GR . . . . H37C H -0.1159 0.2292 0.0355 0.140 Uiso 1 1 calc GR . . . . C40 C 0.0723(7) 0.9104(7) 0.2574(6) 0.061(3) Uani 1 1 d . . . . . H40 H 0.1337 0.9279 0.2687 0.073 Uiso 1 1 calc R . . . . C41 C 0.2926(7) 0.7433(7) 0.1159(5) 0.050(2) Uani 1 1 d . . . . . C42 C 0.3595(7) 0.7152(7) 0.0889(5) 0.056(2) Uani 1 1 d . . . . . H42 H 0.3724 0.6543 0.0873 0.067 Uiso 1 1 calc R . . . . C43 C 0.4071(8) 0.7773(8) 0.0645(5) 0.063(3) Uani 1 1 d . . . . . H43 H 0.4514 0.7584 0.0457 0.075 Uiso 1 1 calc R . . . . C44 C 0.3889(8) 0.8683(8) 0.0680(6) 0.062(3) Uani 1 1 d . . . . . C45 C 0.3192(9) 0.8962(8) 0.0908(6) 0.069(3) Uani 1 1 d . . . . . H45 H 0.3039 0.9567 0.0901 0.083 Uiso 1 1 calc R . . . . C46 C 0.2716(9) 0.8336(7) 0.1149(6) 0.067(3) Uani 1 1 d . . . . . H46 H 0.2242 0.8525 0.1309 0.081 Uiso 1 1 calc R . . . . O4 O 0.4435(7) 0.9251(6) 0.0452(4) 0.084(3) Uani 1 1 d . . . . . C47 C 0.4506(11) 1.0151(9) 0.0664(7) 0.092(5) Uani 1 1 d . . . . . H47A H 0.3912 1.0431 0.0528 0.138 Uiso 1 1 calc GR . . . . H47B H 0.4928 1.0470 0.0491 0.138 Uiso 1 1 calc GR . . . . H47C H 0.4726 1.0162 0.1119 0.138 Uiso 1 1 calc GR . . . . C50 C 0.0046(7) 0.9731(7) 0.2523(6) 0.064(3) Uani 1 1 d . . . . . H50 H 0.0215 1.0327 0.2614 0.077 Uiso 1 1 calc R . . . . Cl1 Cl -0.3072(12) 0.6319(16) 0.3208(12) 0.107(7) Uiso 0.25 1 d D . P B 1 C1S C -0.1987(18) 0.677(2) 0.358(3) 0.11(2) Uiso 0.25 1 d D . P B 1 H1SA H -0.1950 0.6982 0.4001 0.133 Uiso 0.25 1 calc R . P B 1 H1SB H -0.1852 0.7270 0.3334 0.133 Uiso 0.25 1 calc R . P B 1 Cl2 Cl -0.1216(14) 0.5853(19) 0.3602(13) 0.151(8) Uiso 0.25 1 d D . P B 1 Cl3 Cl -0.4030(11) 0.6377(12) 0.1280(8) 0.096(4) Uiso 0.25 1 d D . P C 2 C2S C -0.305(2) 0.572(4) 0.163(4) 0.14(3) Uiso 0.25 1 d D . P C 2 H2SA H -0.3136 0.5108 0.1467 0.165 Uiso 0.25 1 calc R . P C 2 H2SB H -0.2921 0.5706 0.2084 0.165 Uiso 0.25 1 calc R . P C 2 Cl4 Cl -0.2150(15) 0.628(3) 0.1393(17) 0.205(13) Uiso 0.25 1 d D U P C 2 Cl5 Cl -0.327(2) 0.716(2) 0.1137(16) 0.191(11) Uiso 0.25 1 d D U P D 3 C3S C -0.361(3) 0.605(3) 0.120(4) 0.12(3) Uiso 0.25 1 d D . P D 3 H3SA H -0.4081 0.5863 0.0819 0.146 Uiso 0.25 1 calc R . P D 3 H3SB H -0.3843 0.5971 0.1562 0.146 Uiso 0.25 1 calc R . P D 3 Cl6 Cl -0.256(3) 0.543(2) 0.129(2) 0.243(17) Uiso 0.25 1 d D . P D 3 Cl7 Cl -0.2942(17) 0.639(2) 0.3433(15) 0.142(11) Uiso 0.25 1 d D . P E 4 C4S C -0.218(2) 0.706(2) 0.319(3) 0.085(16) Uiso 0.25 1 d D . P E 4 H4SA H -0.2039 0.7604 0.3441 0.102 Uiso 0.25 1 calc R . P E 4 H4SB H -0.2424 0.7223 0.2746 0.102 Uiso 0.25 1 calc R . P E 4 Cl8 Cl -0.1158(12) 0.6349(14) 0.3315(9) 0.112(5) Uiso 0.25 1 d D . P E 4 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 0.0326(4) 0.0295(4) 0.0586(5) 0.0003(3) 0.0139(3) -0.0020(3) Mo2 0.0331(4) 0.0289(4) 0.0598(5) 0.0000(3) 0.0156(3) -0.0030(3) N1 0.051(5) 0.035(4) 0.065(5) -0.003(4) 0.016(4) -0.010(3) N2 0.042(4) 0.033(4) 0.058(5) -0.008(3) 0.014(3) -0.006(3) N3 0.042(4) 0.042(4) 0.052(4) -0.005(3) 0.007(3) -0.005(3) N4 0.046(4) 0.034(4) 0.063(5) 0.003(3) 0.019(4) -0.004(3) N5 0.056(5) 0.053(5) 0.075(6) 0.003(4) 0.020(4) 0.019(4) N6 0.045(4) 0.039(4) 0.075(6) 0.005(4) 0.018(4) 0.012(4) O5 0.041(3) 0.029(3) 0.062(4) 0.000(3) 0.012(3) 0.000(2) O6 0.044(3) 0.028(3) 0.057(4) 0.002(3) 0.020(3) 0.000(2) O7 0.035(3) 0.032(3) 0.062(4) -0.007(3) 0.014(3) 0.003(2) O8 0.039(3) 0.027(3) 0.063(4) -0.001(3) 0.019(3) 0.003(2) C1 0.061(6) 0.047(5) 0.047(5) 0.001(4) 0.009(4) -0.001(5) C2 0.043(5) 0.045(5) 0.057(6) -0.001(4) 0.015(4) -0.003(4) C3 0.032(4) 0.039(5) 0.052(5) -0.001(4) 0.008(4) -0.005(4) C4 0.039(5) 0.037(5) 0.064(6) 0.002(4) 0.016(4) 0.008(4) C5 0.042(5) 0.044(5) 0.078(7) 0.002(5) 0.022(5) 0.005(4) C6 0.065(7) 0.040(5) 0.080(7) -0.002(5) 0.025(6) 0.011(5) C7 0.043(5) 0.040(5) 0.104(9) -0.005(5) 0.025(5) 0.008(4) C8 0.042(5) 0.039(5) 0.090(8) -0.001(5) 0.028(5) 0.002(4) C9 0.035(5) 0.049(6) 0.062(6) -0.002(4) 0.015(4) 0.015(4) C10 0.045(5) 0.040(5) 0.057(6) -0.004(4) 0.009(4) 0.001(4) C11 0.094(10) 0.085(9) 0.057(7) 0.000(6) 0.013(6) -0.045(8) C12 0.166(18) 0.125(15) 0.110(13) -0.026(11) 0.092(13) -0.070(13) C13 0.21(3) 0.20(3) 0.134(19) -0.027(18) 0.097(19) -0.13(2) C14 0.34(2) 0.13(2) 0.117(17) 0.011(14) 0.10(2) -0.12(2) C15 0.27(2) 0.16(2) 0.102(14) 0.053(14) -0.007(16) -0.13(2) C16 0.123(14) 0.078(10) 0.101(11) 0.027(9) -0.013(10) -0.028(10) C20 0.048(6) 0.043(6) 0.087(8) -0.007(5) 0.012(5) 0.012(5) C21 0.055(6) 0.050(6) 0.059(6) -0.005(5) 0.012(5) -0.007(5) C22 0.069(7) 0.052(6) 0.070(7) -0.014(5) 0.020(5) -0.021(5) C23 0.095(10) 0.052(7) 0.089(9) -0.021(6) 0.029(7) -0.022(7) C24 0.067(8) 0.066(8) 0.073(8) -0.015(6) 0.002(6) -0.022(6) C25 0.047(6) 0.058(7) 0.111(10) -0.010(7) 0.010(6) -0.017(5) C26 0.047(6) 0.049(6) 0.100(9) -0.007(6) 0.009(6) -0.013(5) O2 0.101(7) 0.084(7) 0.112(8) -0.023(6) 0.010(6) -0.056(6) C27 0.071(10) 0.120(14) 0.139(15) 0.016(11) -0.002(9) -0.048(10) C30 0.044(6) 0.056(6) 0.089(8) -0.011(6) 0.018(5) 0.012(5) C31 0.048(5) 0.048(6) 0.058(6) 0.001(4) 0.009(4) -0.010(4) C32 0.047(6) 0.050(6) 0.082(8) -0.010(5) 0.010(5) 0.005(5) C33 0.062(7) 0.053(6) 0.088(8) -0.010(6) 0.018(6) -0.015(6) C34 0.055(6) 0.060(7) 0.064(7) 0.000(5) 0.004(5) -0.018(5) C35 0.067(8) 0.069(8) 0.113(11) 0.021(8) -0.010(7) -0.022(7) C36 0.063(7) 0.057(7) 0.108(10) 0.021(7) -0.004(7) -0.013(6) O3 0.074(6) 0.090(7) 0.097(7) 0.009(5) -0.008(5) -0.043(5) C37 0.093(10) 0.079(10) 0.099(10) -0.012(8) 0.013(8) -0.039(8) C40 0.042(5) 0.047(6) 0.094(8) 0.006(5) 0.023(5) 0.006(5) C41 0.055(6) 0.043(5) 0.056(6) 0.004(4) 0.021(4) -0.006(4) C42 0.057(6) 0.051(6) 0.065(6) 0.002(5) 0.026(5) -0.005(5) C43 0.065(7) 0.062(7) 0.070(7) 0.001(5) 0.032(6) -0.004(6) C44 0.060(7) 0.060(7) 0.071(7) 0.006(5) 0.027(5) -0.017(5) C45 0.081(8) 0.045(6) 0.090(9) 0.010(6) 0.040(7) -0.010(6) C46 0.080(8) 0.045(6) 0.087(8) 0.010(5) 0.040(7) 0.002(6) O4 0.104(7) 0.080(6) 0.078(6) -0.009(4) 0.043(5) -0.048(5) C47 0.111(12) 0.068(9) 0.098(10) 0.008(7) 0.031(9) -0.033(8) C50 0.037(5) 0.038(5) 0.119(10) 0.002(5) 0.026(6) 0.004(4) 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' 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' Mo Mo -0.0483 2.7339 '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' 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 Mo2 Mo1 N1 91.6(2) . . ? Mo2 Mo1 N3 91.9(2) . . ? N1 Mo1 N3 176.5(3) . . ? O5 Mo1 Mo2 91.79(17) . . ? O5 Mo1 N1 89.6(3) . . ? O5 Mo1 N3 90.3(3) . . ? O5 Mo1 O7 177.4(2) . . ? O7 Mo1 Mo2 90.46(17) . . ? O7 Mo1 N1 91.5(3) . . ? O7 Mo1 N3 88.4(3) . . ? Mo1 Mo2 N4 91.9(2) . . ? N2 Mo2 Mo1 93.3(2) . . ? N2 Mo2 N4 174.8(3) . . ? O6 Mo2 Mo1 90.89(16) . . ? O6 Mo2 N2 89.9(3) . . ? O6 Mo2 N4 90.7(3) . . ? O6 Mo2 O8 176.8(2) . . ? O8 Mo2 Mo1 92.24(16) . . ? O8 Mo2 N2 90.7(3) . . ? O8 Mo2 N4 88.3(3) . . ? C1 N1 Mo1 118.5(7) . . ? C1 N1 C11 117.4(9) . . ? C11 N1 Mo1 123.5(7) . . ? C1 N2 Mo2 117.8(6) . . ? C1 N2 C21 117.0(8) . . ? C21 N2 Mo2 125.1(6) . . ? C2 N3 Mo1 118.5(6) . . ? C2 N3 C31 118.4(8) . . ? C31 N3 Mo1 122.8(6) . . ? C2 N4 Mo2 119.3(6) . . ? C2 N4 C41 119.1(9) . . ? C41 N4 Mo2 121.5(6) . . ? C6 N5 C7 116.1(9) . . ? C50 N6 C30 117.0(9) . . ? C3 O5 Mo1 117.3(6) . . ? C3 O6 Mo2 118.4(6) . . ? C9 O7 Mo1 117.7(5) . . ? C9 O8 Mo2 115.8(6) . . ? N1 C1 H1 120.6 . . ? N2 C1 N1 118.8(9) . . ? N2 C1 H1 120.6 . . ? N3 C2 N4 118.4(9) . . ? N3 C2 H2 120.8 . . ? N4 C2 H2 120.8 . . ? O5 C3 C4 117.8(8) . . ? O6 C3 O5 121.6(8) . . ? O6 C3 C4 120.6(8) . . ? C5 C4 C3 121.7(9) . . ? C5 C4 C8 117.4(9) . . ? C8 C4 C3 120.9(9) . . ? C4 C5 H5 121.0 . . ? C6 C5 C4 118.0(10) . . ? C6 C5 H5 121.0 . . ? N5 C6 C5 125.2(10) . . ? N5 C6 H6 117.4 . . ? C5 C6 H6 117.4 . . ? N5 C7 H7 118.2 . . ? N5 C7 C8 123.5(10) . . ? C8 C7 H7 118.2 . . ? C4 C8 H8 120.2 . . ? C7 C8 C4 119.6(10) . . ? C7 C8 H8 120.2 . . ? O7 C9 O8 123.6(8) . . ? O7 C9 C10 119.6(8) . . ? O8 C9 C10 116.8(9) . . ? C20 C10 C9 120.2(9) . . ? C40 C10 C9 121.2(9) . . ? C40 C10 C20 118.6(9) . . ? C12 C11 N1 119.9(15) . . ? C16 C11 N1 121.7(15) . . ? C16 C11 C12 118.4(16) . . ? C11 C12 H12 119.7 . . ? C11 C12 C13 121(2) . . ? C13 C12 H12 119.7 . . ? C12 C13 H13 119.0 . . ? C14 C13 C12 122(3) . . ? C14 C13 H13 119.0 . . ? C13 C14 C15 118.8(18) . . ? C13 C14 O1 120(3) . . ? C13 C14 O1A 113(4) . . ? C15 C14 O1 121(3) . . ? O1A C14 C15 128(4) . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120(3) . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120(2) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C14 O1 C17 115(2) . . ? O1 C17 H17D 109.5 . . ? O1 C17 H17E 109.5 . . ? O1 C17 H17F 109.5 . . ? H17D C17 H17E 109.5 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C14 O1A C17A 113(2) . . ? O1A C17A H17A 109.5 . . ? O1A C17A H17B 109.5 . . ? O1A C17A H17C 109.5 . . ? H17A C17A H17B 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C10 C20 H20 120.5 . . ? C30 C20 C10 118.9(10) . . ? C30 C20 H20 120.5 . . ? C22 C21 N2 121.7(10) . . ? C26 C21 N2 119.0(10) . . ? C26 C21 C22 119.1(10) . . ? C21 C22 H22 119.4 . . ? C23 C22 C21 121.2(12) . . ? C23 C22 H22 119.4 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.2(12) . . ? C24 C23 H23 119.9 . . ? C23 C24 C25 118.9(11) . . ? O2 C24 C23 117.4(12) . . ? O2 C24 C25 123.7(12) . . ? C24 C25 H25 120.2 . . ? C26 C25 C24 119.6(12) . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 120.7(12) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C24 O2 C27 117.5(13) . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C30 C20 123.0(10) . . ? N6 C30 H30 118.5 . . ? C20 C30 H30 118.5 . . ? C32 C31 N3 122.2(9) . . ? C32 C31 C36 117.6(10) . . ? C36 C31 N3 119.9(10) . . ? C31 C32 H32 119.5 . . ? C31 C32 C33 121.0(11) . . ? C33 C32 H32 119.5 . . ? C32 C33 H33 119.2 . . ? C34 C33 C32 121.6(11) . . ? C34 C33 H33 119.2 . . ? C33 C34 C35 117.9(11) . . ? C33 C34 O3 126.2(11) . . ? O3 C34 C35 115.8(11) . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.4(13) . . ? C36 C35 H35 119.8 . . ? C31 C36 H36 119.3 . . ? C35 C36 C31 121.4(12) . . ? C35 C36 H36 119.3 . . ? C34 O3 C37 117.7(11) . . ? O3 C37 H37A 109.5 . . ? O3 C37 H37B 109.5 . . ? O3 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C10 C40 H40 120.1 . . ? C10 C40 C50 119.8(10) . . ? C50 C40 H40 120.1 . . ? C42 C41 N4 121.2(9) . . ? C46 C41 N4 119.4(9) . . ? C46 C41 C42 118.9(10) . . ? C41 C42 H42 120.1 . . ? C43 C42 C41 119.9(10) . . ? C43 C42 H42 120.1 . . ? C42 C43 H43 120.0 . . ? C42 C43 C44 120.1(10) . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.4(10) . . ? C45 C44 O4 124.1(11) . . ? O4 C44 C43 115.4(10) . . ? C44 C45 H45 120.4 . . ? C44 C45 C46 119.1(11) . . ? C46 C45 H45 120.4 . . ? C41 C46 H46 119.3 . . ? C45 C46 C41 121.4(11) . . ? C45 C46 H46 119.3 . . ? C44 O4 C47 117.2(10) . . ? O4 C47 H47A 109.5 . . ? O4 C47 H47B 109.5 . . ? O4 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N6 C50 C40 122.7(10) . . ? N6 C50 H50 118.7 . . ? C40 C50 H50 118.7 . . ? Cl1 C1S H1SA 111.0 . . ? Cl1 C1S H1SB 111.0 . . ? Cl1 C1S Cl2 103.7(12) . . ? H1SA C1S H1SB 109.0 . . ? Cl2 C1S H1SA 111.0 . . ? Cl2 C1S H1SB 111.0 . . ? Cl3 C2S H2SA 111.1 . . ? Cl3 C2S H2SB 111.1 . . ? Cl3 C2S Cl4 103.5(12) . . ? H2SA C2S H2SB 109.0 . . ? Cl4 C2S H2SA 111.1 . . ? Cl4 C2S H2SB 111.1 . . ? Cl5 C3S H3SA 111.2 . . ? Cl5 C3S H3SB 111.2 . . ? Cl5 C3S Cl6 103.0(19) . . ? H3SA C3S H3SB 109.1 . . ? Cl6 C3S H3SA 111.2 . . ? Cl6 C3S H3SB 111.2 . . ? Cl7 C4S H4SA 111.1 . . ? Cl7 C4S H4SB 111.1 . . ? Cl7 C4S Cl8 103.4(17) . . ? H4SA C4S H4SB 109.1 . . ? Cl8 C4S H4SA 111.1 . . ? Cl8 C4S H4SB 111.1 . . ? 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 Mo2 2.1312(9) . ? Mo1 N1 2.143(9) . ? Mo1 N3 2.156(8) . ? Mo1 O5 2.104(6) . ? Mo1 O7 2.125(6) . ? Mo2 N2 2.130(8) . ? Mo2 N4 2.135(8) . ? Mo2 O6 2.108(6) . ? Mo2 O8 2.119(6) . ? N1 C1 1.348(12) . ? N1 C11 1.434(14) . ? N2 C1 1.338(12) . ? N2 C21 1.425(12) . ? N3 C2 1.318(12) . ? N3 C31 1.424(12) . ? N4 C2 1.330(12) . ? N4 C41 1.440(12) . ? N5 C6 1.330(14) . ? N5 C7 1.346(14) . ? N6 C30 1.344(14) . ? N6 C50 1.339(13) . ? O5 C3 1.287(10) . ? O6 C3 1.268(10) . ? O7 C9 1.258(11) . ? O8 C9 1.274(11) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.454(12) . ? C4 C5 1.392(14) . ? C4 C8 1.402(13) . ? C5 H5 0.9300 . ? C5 C6 1.382(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.371(13) . ? C8 H8 0.9300 . ? C9 C10 1.486(12) . ? C10 C20 1.374(14) . ? C10 C40 1.362(14) . ? C11 C12 1.35(2) . ? C11 C16 1.34(2) . ? C12 H12 0.9300 . ? C12 C13 1.38(2) . ? C13 H13 0.9300 . ? C13 C14 1.29(4) . ? C14 C15 1.37(4) . ? C14 O1 1.382(17) . ? C14 O1A 1.37(2) . ? C15 H15 0.9300 . ? C15 C16 1.41(2) . ? C16 H16 0.9300 . ? O1 C17 1.420(19) . ? C17 H17D 0.9600 . ? C17 H17E 0.9600 . ? C17 H17F 0.9600 . ? O1A C17A 1.42(2) . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C20 H20 0.9300 . ? C20 C30 1.371(14) . ? C21 C22 1.373(15) . ? C21 C26 1.366(15) . ? C22 H22 0.9300 . ? C22 C23 1.370(15) . ? C23 H23 0.9300 . ? C23 C24 1.376(18) . ? C24 C25 1.397(18) . ? C24 O2 1.373(13) . ? C25 H25 0.9300 . ? C25 C26 1.386(14) . ? C26 H26 0.9300 . ? O2 C27 1.390(19) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C30 H30 0.9300 . ? C31 C32 1.378(14) . ? C31 C36 1.386(16) . ? C32 H32 0.9300 . ? C32 C33 1.381(15) . ? C33 H33 0.9300 . ? C33 C34 1.342(16) . ? C34 C35 1.418(18) . ? C34 O3 1.364(12) . ? C35 H35 0.9300 . ? C35 C36 1.353(16) . ? C36 H36 0.9300 . ? O3 C37 1.406(17) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C40 H40 0.9300 . ? C40 C50 1.369(14) . ? C41 C42 1.381(14) . ? C41 C46 1.382(14) . ? C42 H42 0.9300 . ? C42 C43 1.374(14) . ? C43 H43 0.9300 . ? C43 C44 1.390(17) . ? C44 C45 1.360(16) . ? C44 O4 1.377(12) . ? C45 H45 0.9300 . ? C45 C46 1.377(15) . ? C46 H46 0.9300 . ? O4 C47 1.413(16) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C50 H50 0.9300 . ? Cl1 C1S 1.749(16) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? C1S Cl2 1.794(16) . ? Cl3 C2S 1.758(16) . ? C2S H2SA 0.9700 . ? C2S H2SB 0.9700 . ? C2S Cl4 1.800(16) . ? Cl5 C3S 1.75(2) . ? C3S H3SA 0.9700 . ? C3S H3SB 0.9700 . ? C3S Cl6 1.80(2) . ? Cl7 C4S 1.73(2) . ? C4S H4SA 0.9700 . ? C4S H4SB 0.9700 . ? C4S Cl8 1.83(2) . ?