#------------------------------------------------------------------------------ #$Date: 2026-05-11 23:54:08 +0100 (Mon, 11 May 2026) $ #$Revision: 305926 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721018.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_7721018 loop_ _publ_author_name 'Mandal, Souvik' 'Song, Ethan Y.' 'Emge, Thomas J.' 'Hasanayn, Faraj' 'Goldman, Alan S.' _publ_section_title ; A metal-metal quadruply bonded dimer of two pincer-ligated metal centers ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00920D _journal_year 2026 _chemical_formula_sum 'C28 H40 I Mo N O2 P2' _chemical_formula_weight 707.39 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc2njv02 _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2026-04-17 deposited with the CCDC. 2026-05-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.857(7) _cell_length_b 10.099(4) _cell_length_c 17.473(5) _cell_measurement_reflns_used 959 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 18.10 _cell_measurement_theta_min 2.28 _cell_volume 3151(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_unetI/netI 0.0748 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 23700 _diffrn_reflns_point_group_measured_fraction_full 0.915 _diffrn_reflns_point_group_measured_fraction_max 0.915 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 2.016 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type none _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.491 _exptl_crystal_description irregular _exptl_crystal_F_000 1424 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _refine_diff_density_max 2.200 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.167 _refine_ls_abs_structure_details ; Flack x determined using 1176 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 5274 _refine_ls_number_restraints 584 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0888 _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^)+(0.1100P)^2^+7.7000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2044 _refine_ls_wR_factor_ref 0.2325 _reflns_Friedel_coverage 0.774 _reflns_Friedel_fraction_full 0.828 _reflns_Friedel_fraction_max 0.829 _reflns_number_gt 3807 _reflns_number_total 5274 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00920d2.cif _cod_data_source_block sm_120_final _cod_database_code 7721018 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.804 _shelx_estimated_absorpt_t_max 0.901 _shelx_res_file ; TITL sm_120_B_ONLY_a.res in Pca2(1) sm_120_final.res created by SHELXL-2019/3 at 07:40:11 on 17-Apr-2026 REM Old TITL sm_120_B_ONLY in Pca2(1) REM SHELXT solution in Pca2(1): R1 0.173, Rweak 0.048, Alpha 0.009 REM 1.279 for 282 systematic absences, Orientation as input REM Flack x = -0.025 ( 0.062 ) from 1301 Parsons' quotients REM Formula found by SHELXT: C28 Mo2 O3 P2 CELL 0.71073 17.8572 10.0995 17.4732 90.000 90.000 90.000 ZERR 4.000 0.0073 0.0037 0.0052 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, -Y, Z SYMM 1/2-X, Y, 1/2+Z SFAC C H I MO N O P UNIT 112 160 4 4 4 8 8 TEMP -153. SIZE 0.15 0.10 0.07 L.S. 22 SHEL .83 11. BOND $H LIST 4 ACTA CONF REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, z+1/2 HTAB C18 I1A_$1 HTAB C20 I1A HTAB C21 I1A HTAB C24 O1 HTAB C27 I1A HTAB C28 I1B OMIT 0 0 2 OMIT 2 0 -2 OMIT 2 0 2 OMIT 4 0 -4 OMIT 2 0 -1 FMAP -2 PLAN 20 EADP I1B O2A EADP I1B C2A ISOR .02 SIMU .02 DELU .02 REM DFIX 2.80 .01 I2B MO1 REM DFIX 2.03 .003 C2A MO1 C2B MO1 REM DFIX 1.15 .003 C2A O2A C2B O2B REM DFIX 3.18 .003 O2A MO1 O2B MO1 EADP I1A O2B EADP I1A C2B WGHT 0.110000 7.700000 FVAR 0.05323 0.90848 MO1 4 0.627482 0.173121 0.537781 11.00000 0.05710 0.05590 = 0.04948 0.00114 0.00539 0.00466 SAME .001 I1B > C2B PART 1 I1A 3 0.556181 -0.042756 0.468170 21.00000 0.08897 0.07377 = 0.09302 -0.02731 0.01917 -0.01855 O2A 6 0.730124 -0.055968 0.602476 21.00000 0.11015 0.09704 = 0.11078 0.03128 0.00690 0.03871 C2A 1 0.690568 0.034458 0.573750 21.00000 0.11015 0.09704 = 0.11078 0.03128 0.00690 0.03871 PART 2 REM AFIX 1 I1B 3 0.683218 -0.024653 0.592823 -21.00000 0.11015 0.09704 = 0.11078 0.03128 0.00690 0.03871 O2B 6 0.535925 -0.103634 0.457694 -21.00000 0.08897 0.07377 = 0.09302 -0.02731 0.01917 -0.01855 C2B 1 0.555303 0.013379 0.472699 -21.00000 0.08897 0.07377 = 0.09302 -0.02731 0.01917 -0.01855 PART 0 P1 7 0.740180 0.220039 0.455903 11.00000 0.04651 0.06156 = 0.04674 -0.00204 -0.00593 0.00989 P2 7 0.500367 0.228234 0.588721 11.00000 0.06072 0.05506 = 0.04963 0.00243 0.01063 -0.00227 REM SAME .001 O2B C2B O1 6 0.673910 0.253866 0.702538 11.00000 0.10582 0.16478 = 0.06284 -0.00953 -0.02098 0.01531 C1 1 0.656482 0.223077 0.641284 11.00000 0.08065 0.09665 = 0.05586 0.00844 -0.01936 0.00438 N1 5 0.616858 0.375053 0.513956 11.00000 0.04552 0.04707 = 0.04800 0.00182 0.00143 0.00607 C3 1 0.580213 0.456501 0.570501 11.00000 0.04651 0.05047 = 0.04098 0.00171 -0.00370 0.00880 C4 1 0.520937 0.398629 0.611268 11.00000 0.05457 0.05790 = 0.03805 0.00227 -0.00225 0.00219 C5 1 0.482361 0.473633 0.668630 11.00000 0.05652 0.07166 = 0.04522 -0.00258 0.00526 0.00446 AFIX 43 H5 2 0.439952 0.436629 0.693531 11.00000 -1.20000 AFIX 0 C6 1 0.506764 0.601708 0.688413 11.00000 0.06666 0.06321 = 0.03950 -0.00560 -0.01485 0.01752 C7 1 0.566749 0.654926 0.646185 11.00000 0.07140 0.06305 = 0.04762 -0.01267 -0.02001 0.01062 AFIX 43 H7 2 0.583372 0.742203 0.657256 11.00000 -1.20000 AFIX 0 C8 1 0.601680 0.584926 0.589888 11.00000 0.06053 0.05727 = 0.05602 0.00344 -0.00096 -0.00111 AFIX 43 H8 2 0.641981 0.624934 0.562964 11.00000 -1.20000 AFIX 0 C9 1 0.466769 0.675789 0.751240 11.00000 0.10522 0.09492 = 0.05691 -0.02467 0.01236 0.01098 AFIX 33 H9A 2 0.427100 0.619832 0.772595 11.00000 -1.50000 H9B 2 0.502535 0.698774 0.791652 11.00000 -1.50000 H9C 2 0.444686 0.756894 0.730295 11.00000 -1.50000 AFIX 0 C10 1 0.651793 0.439197 0.452037 11.00000 0.04543 0.05366 = 0.04088 -0.00681 -0.00031 -0.00323 C11 1 0.711934 0.380419 0.417057 11.00000 0.04867 0.05866 = 0.04029 0.00237 -0.00697 0.00628 C12 1 0.745217 0.440606 0.353035 11.00000 0.05841 0.07429 = 0.05364 0.00044 0.01330 -0.00372 AFIX 43 H12 2 0.787114 0.398410 0.330062 11.00000 -1.20000 AFIX 0 C13 1 0.719723 0.559443 0.321510 11.00000 0.07665 0.06767 = 0.05769 0.00699 0.01261 -0.00536 C14 1 0.659592 0.617416 0.358575 11.00000 0.07882 0.05987 = 0.05586 0.01008 0.00783 0.00215 AFIX 43 H14 2 0.643013 0.701891 0.341697 11.00000 -1.20000 AFIX 0 C15 1 0.621677 0.556848 0.420371 11.00000 0.06377 0.06804 = 0.05211 0.01147 0.00690 0.00159 AFIX 43 H15 2 0.576917 0.594274 0.440260 11.00000 -1.20000 AFIX 0 C16 1 0.757300 0.619570 0.253470 11.00000 0.09447 0.11720 = 0.09308 0.03320 0.03750 -0.00664 AFIX 33 H16A 2 0.798284 0.561999 0.236618 11.00000 -1.50000 H16B 2 0.720891 0.629479 0.211898 11.00000 -1.50000 H16C 2 0.777373 0.706669 0.267267 11.00000 -1.50000 AFIX 0 C17 1 0.458544 0.154153 0.677185 11.00000 0.09220 0.08551 = 0.06663 0.00714 0.03271 -0.01031 AFIX 13 H17 2 0.414023 0.208573 0.691873 11.00000 -1.20000 AFIX 0 C18 1 0.510919 0.152104 0.743138 11.00000 0.13283 0.13597 = 0.06253 0.03246 0.02178 0.00431 AFIX 33 H18A 2 0.526849 0.242686 0.754945 11.00000 -1.50000 H18B 2 0.485658 0.113930 0.787773 11.00000 -1.50000 H18C 2 0.554829 0.098345 0.730241 11.00000 -1.50000 AFIX 0 C19 1 0.429933 0.011472 0.654169 11.00000 0.12302 0.09068 = 0.12716 0.02315 0.03856 -0.02769 AFIX 33 H19A 2 0.395690 0.018524 0.610531 11.00000 -1.50000 H19B 2 0.472772 -0.044070 0.640089 11.00000 -1.50000 H19C 2 0.403601 -0.028485 0.697621 11.00000 -1.50000 AFIX 0 C20 1 0.421187 0.232752 0.518641 11.00000 0.05922 0.07686 = 0.06896 -0.00478 -0.00060 -0.01289 AFIX 13 H20 2 0.407854 0.139030 0.506185 11.00000 -1.20000 AFIX 0 C21 1 0.443194 0.298263 0.446082 11.00000 0.08413 0.10269 = 0.06104 0.01011 -0.02201 0.00383 AFIX 33 H21A 2 0.487823 0.254803 0.425241 11.00000 -1.50000 H21B 2 0.402074 0.291494 0.409145 11.00000 -1.50000 H21C 2 0.454227 0.391782 0.455916 11.00000 -1.50000 AFIX 0 C22 1 0.352070 0.297456 0.552784 11.00000 0.06198 0.09883 = 0.11072 -0.01421 -0.00226 -0.00171 AFIX 33 H22A 2 0.338697 0.252491 0.600569 11.00000 -1.50000 H22B 2 0.362531 0.390960 0.563294 11.00000 -1.50000 H22C 2 0.310379 0.290672 0.516523 11.00000 -1.50000 AFIX 0 C23 1 0.830425 0.245845 0.505456 11.00000 0.04961 0.07559 = 0.08323 0.01117 -0.02209 -0.00184 AFIX 13 H23 2 0.849198 0.155869 0.519691 11.00000 -1.20000 AFIX 0 C24 1 0.820303 0.321873 0.580806 11.00000 0.10591 0.14830 = 0.09455 -0.02216 -0.02456 -0.02213 AFIX 33 H24A 2 0.781112 0.279366 0.611430 11.00000 -1.50000 H24B 2 0.867509 0.321326 0.609408 11.00000 -1.50000 H24C 2 0.805824 0.413473 0.569691 11.00000 -1.50000 AFIX 0 C25 1 0.890278 0.307702 0.456312 11.00000 0.06239 0.11968 = 0.12633 -0.00174 0.00469 -0.00646 AFIX 33 H25A 2 0.895410 0.257081 0.408751 11.00000 -1.50000 H25B 2 0.876335 0.399204 0.444251 11.00000 -1.50000 H25C 2 0.938021 0.307057 0.483968 11.00000 -1.50000 AFIX 0 C26 1 0.764480 0.119533 0.371123 11.00000 0.05776 0.07334 = 0.04681 -0.00862 0.00828 0.01212 AFIX 13 H26 2 0.808120 0.162091 0.345024 11.00000 -1.20000 AFIX 0 C27 1 0.700149 0.107315 0.312625 11.00000 0.06362 0.11177 = 0.05106 -0.00514 0.00983 0.00250 AFIX 33 H27A 2 0.684371 0.195886 0.296352 11.00000 -1.50000 H27B 2 0.717453 0.057001 0.268047 11.00000 -1.50000 H27C 2 0.657756 0.061296 0.336312 11.00000 -1.50000 AFIX 0 C28 1 0.787745 -0.022020 0.395347 11.00000 0.12179 0.10443 = 0.09423 -0.01615 -0.00847 0.05651 AFIX 33 H28A 2 0.828661 -0.016927 0.432609 11.00000 -1.50000 H28B 2 0.744805 -0.067233 0.418518 11.00000 -1.50000 H28C 2 0.804501 -0.071528 0.350252 11.00000 -1.50000 REM REM sm_120_final.hkl REM AFIX 0 HKLF 4 REM sm_120_B_ONLY_a.res in Pca2(1) REM wR2 = 0.2325, GooF = S = 1.153, Restrained GooF = 1.110 for all data REM R1 = 0.0888 for 3807 Fo > 4sig(Fo) and 0.1232 for all 5274 data REM 320 parameters refined using 584 restraints END WGHT 0.1148 9.1450 REM Highest difference peak 2.200, deepest hole -0.899, 1-sigma level 0.167 Q1 1 0.6231 0.2788 0.5371 11.00000 0.05 2.20 Q2 1 0.6148 0.0735 0.5400 11.00000 0.05 1.98 Q3 1 0.5602 0.0548 0.4702 11.00000 0.05 1.88 Q4 1 0.5952 0.1638 0.4946 11.00000 0.05 1.57 Q5 1 0.5465 -0.1392 0.4631 11.00000 0.05 1.35 Q6 1 0.5651 -0.1536 0.4747 11.00000 0.05 1.28 Q7 1 0.5979 -0.0565 0.5079 11.00000 0.05 0.93 Q8 1 0.5156 0.3196 0.5990 11.00000 0.05 0.91 Q9 1 0.6328 0.1739 0.5989 11.00000 0.05 -0.90 Q10 1 0.6847 0.1683 0.5404 11.00000 0.05 -0.86 Q11 1 0.5007 -0.0310 0.4682 11.00000 0.05 -0.81 Q12 1 0.5721 0.1776 0.5401 11.00000 0.05 -0.79 Q13 1 0.7407 0.3125 0.4566 11.00000 0.05 0.75 Q14 1 0.5307 -0.0620 0.5006 11.00000 0.05 0.71 Q15 1 0.6189 0.3751 0.5440 11.00000 0.05 0.67 Q16 1 0.6664 0.1179 0.5812 11.00000 0.05 0.66 Q17 1 0.5528 -0.0377 0.3997 11.00000 0.05 -0.65 Q18 1 0.6547 -0.0297 0.5573 11.00000 0.05 0.63 Q19 1 0.7213 0.1325 0.4577 11.00000 0.05 0.61 Q20 1 0.6415 0.1542 0.4676 11.00000 0.05 -0.59 ; _shelx_res_checksum 95804 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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 0.62748(9) 0.17312(14) 0.5378(6) 0.0542(5) Uani 1 1 d . U . . . I1A I 0.55618(10) -0.04276(16) 0.4682(6) 0.0853(7) Uani 0.908(5) 1 d D U P A 1 O2A O 0.7301(13) -0.0560(19) 0.6025(14) 0.106(4) Uani 0.908(5) 1 d D U P A 1 C2A C 0.6906(19) 0.034(3) 0.574(2) 0.106(4) Uani 0.908(5) 1 d D U P A 1 I1B I 0.6832(17) -0.025(2) 0.5928(15) 0.106(4) Uani 0.092(5) 1 d D U P A 2 O2B O 0.536(7) -0.104(5) 0.458(9) 0.0853(7) Uani 0.092(5) 1 d D U P A 2 C2B C 0.555(5) 0.013(5) 0.473(5) 0.0853(7) Uani 0.092(5) 1 d D U P A 2 P1 P 0.7402(2) 0.2200(5) 0.4559(7) 0.0516(12) Uani 1 1 d . U . . . P2 P 0.5004(3) 0.2282(5) 0.5887(7) 0.0551(12) Uani 1 1 d . U . . . O1 O 0.6739(12) 0.254(2) 0.7025(13) 0.111(6) Uani 1 1 d . U . . . C1 C 0.6565(14) 0.223(2) 0.6413(16) 0.078(5) Uani 1 1 d . U . . . N1 N 0.6169(8) 0.3751(14) 0.5140(10) 0.047(3) Uani 1 1 d . U . . . C3 C 0.5802(10) 0.4565(16) 0.5705(12) 0.046(3) Uani 1 1 d . U . . . C4 C 0.5209(10) 0.3986(18) 0.6113(12) 0.050(4) Uani 1 1 d . U . . . C5 C 0.4824(11) 0.4736(19) 0.6686(13) 0.058(4) Uani 1 1 d . U . . . H5 H 0.439952 0.436629 0.693531 0.069 Uiso 1 1 calc R U . . . C6 C 0.5068(12) 0.6017(19) 0.6884(13) 0.056(4) Uani 1 1 d . U . . . C7 C 0.5667(12) 0.655(2) 0.6462(14) 0.061(4) Uani 1 1 d . U . . . H7 H 0.583372 0.742203 0.657256 0.073 Uiso 1 1 calc R U . . . C8 C 0.6017(12) 0.5849(19) 0.5899(14) 0.058(4) Uani 1 1 d . U . . . H8 H 0.641981 0.624934 0.562964 0.070 Uiso 1 1 calc R U . . . C9 C 0.4668(16) 0.676(2) 0.7512(17) 0.086(7) Uani 1 1 d . U . . . H9A H 0.427100 0.619832 0.772595 0.129 Uiso 1 1 calc R U . . . H9B H 0.502535 0.698774 0.791652 0.129 Uiso 1 1 calc R U . . . H9C H 0.444686 0.756894 0.730295 0.129 Uiso 1 1 calc R U . . . C10 C 0.6518(9) 0.4392(16) 0.4520(12) 0.047(4) Uani 1 1 d . U . . . C11 C 0.7119(10) 0.3804(18) 0.4171(13) 0.049(4) Uani 1 1 d . U . . . C12 C 0.7452(12) 0.4406(19) 0.3530(15) 0.062(4) Uani 1 1 d . U . . . H12 H 0.787114 0.398410 0.330062 0.075 Uiso 1 1 calc R U . . . C13 C 0.7197(13) 0.559(2) 0.3215(15) 0.067(5) Uani 1 1 d . U . . . C14 C 0.6596(12) 0.617(2) 0.3586(14) 0.065(5) Uani 1 1 d . U . . . H14 H 0.643013 0.701891 0.341697 0.078 Uiso 1 1 calc R U . . . C15 C 0.6217(12) 0.557(2) 0.4204(14) 0.061(5) Uani 1 1 d . U . . . H15 H 0.576917 0.594274 0.440260 0.074 Uiso 1 1 calc R U . . . C16 C 0.7573(16) 0.620(3) 0.2535(18) 0.102(9) Uani 1 1 d . U . . . H16A H 0.798284 0.561999 0.236618 0.152 Uiso 1 1 calc R U . . . H16B H 0.720891 0.629479 0.211898 0.152 Uiso 1 1 calc R U . . . H16C H 0.777373 0.706669 0.267267 0.152 Uiso 1 1 calc R U . . . C17 C 0.4585(15) 0.154(2) 0.6772(17) 0.081(6) Uani 1 1 d . U . . . H17 H 0.414023 0.208573 0.691873 0.098 Uiso 1 1 calc R U . . . C18 C 0.5109(18) 0.152(3) 0.7431(18) 0.110(9) Uani 1 1 d . U . . . H18A H 0.526849 0.242686 0.754945 0.166 Uiso 1 1 calc R U . . . H18B H 0.485658 0.113930 0.787773 0.166 Uiso 1 1 calc R U . . . H18C H 0.554829 0.098345 0.730241 0.166 Uiso 1 1 calc R U . . . C19 C 0.4299(18) 0.011(3) 0.654(2) 0.114(9) Uani 1 1 d . U . . . H19A H 0.395690 0.018524 0.610531 0.170 Uiso 1 1 calc R U . . . H19B H 0.472772 -0.044070 0.640089 0.170 Uiso 1 1 calc R U . . . H19C H 0.403601 -0.028485 0.697621 0.170 Uiso 1 1 calc R U . . . C20 C 0.4212(12) 0.233(2) 0.5186(15) 0.068(5) Uani 1 1 d . U . . . H20 H 0.407854 0.139030 0.506185 0.082 Uiso 1 1 calc R U . . . C21 C 0.4432(13) 0.298(3) 0.4461(16) 0.083(6) Uani 1 1 d . U . . . H21A H 0.487823 0.254803 0.425241 0.124 Uiso 1 1 calc R U . . . H21B H 0.402074 0.291494 0.409145 0.124 Uiso 1 1 calc R U . . . H21C H 0.454227 0.391782 0.455916 0.124 Uiso 1 1 calc R U . . . C22 C 0.3521(12) 0.297(3) 0.553(2) 0.091(7) Uani 1 1 d . U . . . H22A H 0.338697 0.252491 0.600569 0.136 Uiso 1 1 calc R U . . . H22B H 0.362531 0.390960 0.563294 0.136 Uiso 1 1 calc R U . . . H22C H 0.310379 0.290672 0.516523 0.136 Uiso 1 1 calc R U . . . C23 C 0.8304(11) 0.246(2) 0.5055(15) 0.069(5) Uani 1 1 d . U . . . H23 H 0.849198 0.155869 0.519691 0.083 Uiso 1 1 calc R U . . . C24 C 0.8203(18) 0.322(3) 0.581(2) 0.116(10) Uani 1 1 d . U . . . H24A H 0.781112 0.279366 0.611430 0.174 Uiso 1 1 calc R U . . . H24B H 0.867509 0.321326 0.609408 0.174 Uiso 1 1 calc R U . . . H24C H 0.805824 0.413473 0.569691 0.174 Uiso 1 1 calc R U . . . C25 C 0.8903(14) 0.308(3) 0.456(2) 0.103(8) Uani 1 1 d . U . . . H25A H 0.895410 0.257081 0.408751 0.154 Uiso 1 1 calc R U . . . H25B H 0.876335 0.399204 0.444251 0.154 Uiso 1 1 calc R U . . . H25C H 0.938021 0.307057 0.483968 0.154 Uiso 1 1 calc R U . . . C26 C 0.7645(11) 0.120(2) 0.3711(13) 0.059(4) Uani 1 1 d . U . . . H26 H 0.808120 0.162091 0.345024 0.071 Uiso 1 1 calc R U . . . C27 C 0.7001(12) 0.107(3) 0.3126(15) 0.075(6) Uani 1 1 d . U . . . H27A H 0.684371 0.195886 0.296352 0.113 Uiso 1 1 calc R U . . . H27B H 0.717453 0.057001 0.268047 0.113 Uiso 1 1 calc R U . . . H27C H 0.657756 0.061296 0.336312 0.113 Uiso 1 1 calc R U . . . C28 C 0.7877(18) -0.022(3) 0.395(2) 0.107(9) Uani 1 1 d . U . . . H28A H 0.828661 -0.016927 0.432609 0.160 Uiso 1 1 calc R U . . . H28B H 0.744805 -0.067233 0.418518 0.160 Uiso 1 1 calc R U . . . H28C H 0.804501 -0.071528 0.350252 0.160 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 0.0571(9) 0.0559(8) 0.0495(10) 0.0011(8) 0.0054(9) 0.0047(7) I1A 0.0890(12) 0.0738(10) 0.0930(15) -0.0273(10) 0.0192(11) -0.0186(8) O2A 0.110(9) 0.097(8) 0.111(9) 0.031(7) 0.007(8) 0.039(7) C2A 0.110(9) 0.097(8) 0.111(9) 0.031(7) 0.007(8) 0.039(7) I1B 0.110(9) 0.097(8) 0.111(9) 0.031(7) 0.007(8) 0.039(7) O2B 0.0890(12) 0.0738(10) 0.0930(15) -0.0273(10) 0.0192(11) -0.0186(8) C2B 0.0890(12) 0.0738(10) 0.0930(15) -0.0273(10) 0.0192(11) -0.0186(8) P1 0.047(2) 0.062(3) 0.047(3) -0.002(2) -0.006(2) 0.0099(19) P2 0.061(3) 0.055(3) 0.050(3) 0.002(2) 0.011(2) -0.002(2) O1 0.106(14) 0.165(17) 0.063(11) -0.010(11) -0.021(10) 0.015(12) C1 0.081(11) 0.097(11) 0.056(10) 0.008(9) -0.019(9) 0.004(10) N1 0.046(7) 0.047(6) 0.048(8) 0.002(5) 0.001(5) 0.006(6) C3 0.047(8) 0.050(7) 0.041(8) 0.002(6) -0.004(6) 0.009(6) C4 0.055(8) 0.058(8) 0.038(9) 0.002(7) -0.002(7) 0.002(7) C5 0.057(9) 0.072(9) 0.045(10) -0.003(8) 0.005(8) 0.004(8) C6 0.067(9) 0.063(9) 0.040(9) -0.006(7) -0.015(7) 0.018(8) C7 0.071(10) 0.063(9) 0.048(10) -0.013(8) -0.020(8) 0.011(8) C8 0.061(9) 0.057(8) 0.056(10) 0.003(7) -0.001(8) -0.001(7) C9 0.105(16) 0.095(15) 0.057(14) -0.025(11) 0.012(12) 0.011(13) C10 0.045(7) 0.054(7) 0.041(9) -0.007(7) 0.000(6) -0.003(6) C11 0.049(8) 0.059(8) 0.040(9) 0.002(7) -0.007(6) 0.006(7) C12 0.058(9) 0.074(9) 0.054(10) 0.000(8) 0.013(8) -0.004(8) C13 0.077(10) 0.068(10) 0.058(11) 0.007(8) 0.013(9) -0.005(8) C14 0.079(11) 0.060(9) 0.056(11) 0.010(8) 0.008(8) 0.002(8) C15 0.064(10) 0.068(9) 0.052(10) 0.011(8) 0.007(8) 0.002(8) C16 0.094(17) 0.117(18) 0.093(19) 0.033(14) 0.037(14) -0.007(15) C17 0.092(12) 0.086(11) 0.067(11) 0.007(10) 0.033(9) -0.010(10) C18 0.13(2) 0.14(2) 0.063(15) 0.032(15) 0.022(13) 0.004(16) C19 0.12(2) 0.091(15) 0.13(2) 0.023(15) 0.039(17) -0.028(14) C20 0.059(9) 0.077(11) 0.069(11) -0.005(8) -0.001(8) -0.013(8) C21 0.084(15) 0.103(15) 0.061(14) 0.010(12) -0.022(11) 0.004(12) C22 0.062(11) 0.099(15) 0.11(2) -0.014(15) -0.002(12) -0.002(10) C23 0.050(9) 0.076(11) 0.083(12) 0.011(9) -0.022(8) -0.002(8) C24 0.106(19) 0.15(2) 0.095(18) -0.022(17) -0.025(14) -0.022(17) C25 0.062(12) 0.120(19) 0.13(2) -0.002(18) 0.005(14) -0.006(12) C26 0.058(9) 0.073(9) 0.047(10) -0.009(8) 0.008(8) 0.012(8) C27 0.064(12) 0.112(16) 0.051(12) -0.005(11) 0.010(9) 0.003(11) C28 0.122(19) 0.104(16) 0.094(19) -0.016(14) -0.008(16) 0.057(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 C2A Mo1 C1 74.1(13) . . ? C2A Mo1 N1 146.8(12) . . ? C1 Mo1 N1 87.5(8) . . ? C1 Mo1 C2B 140(3) . . ? N1 Mo1 C2B 121.5(12) . . ? C1 Mo1 I1B 74.7(10) . . ? N1 Mo1 I1B 156.6(8) . . ? C2B Mo1 I1B 81.5(10) . . ? C2A Mo1 P2 125.7(12) . . ? C1 Mo1 P2 81.6(8) . . ? N1 Mo1 P2 76.8(4) . . ? C2B Mo1 P2 80(3) . . ? I1B Mo1 P2 114.4(7) . . ? C2A Mo1 P1 81.5(12) . . ? C1 Mo1 P1 105.5(8) . . ? N1 Mo1 P1 77.0(4) . . ? C2B Mo1 P1 107(3) . . ? I1B Mo1 P1 93.0(7) . . ? P2 Mo1 P1 152.51(17) . . ? C2A Mo1 I1A 80.8(11) . . ? C1 Mo1 I1A 136.5(8) . . ? N1 Mo1 I1A 129.2(4) . . ? P2 Mo1 I1A 85.14(14) . . ? P1 Mo1 I1A 105.27(13) . . ? O2A C2A Mo1 176(3) . . ? O2B C2B Mo1 153(7) . . ? C11 P1 C26 104.7(9) . . ? C11 P1 C23 106.8(9) . . ? C26 P1 C23 104.4(10) . . ? C11 P1 Mo1 99.1(6) . . ? C26 P1 Mo1 122.7(7) . . ? C23 P1 Mo1 117.3(8) . . ? C4 P2 C20 105.9(9) . . ? C4 P2 C17 106.4(10) . . ? C20 P2 C17 104.4(12) . . ? C4 P2 Mo1 96.0(6) . . ? C20 P2 Mo1 117.3(8) . . ? C17 P2 Mo1 124.5(9) . . ? O1 C1 Mo1 179(3) . . ? C10 N1 C3 117.7(13) . . ? C10 N1 Mo1 124.2(11) . . ? C3 N1 Mo1 117.5(11) . . ? C8 C3 C4 118.1(17) . . ? C8 C3 N1 124.9(17) . . ? C4 C3 N1 116.9(15) . . ? C3 C4 C5 119.8(17) . . ? C3 C4 P2 116.1(14) . . ? C5 C4 P2 124.0(15) . . ? C6 C5 C4 120.6(18) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 117.2(18) . . ? C7 C6 C9 123.5(19) . . ? C5 C6 C9 119(2) . . ? C8 C7 C6 121.9(19) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C3 122(2) . . ? C7 C8 H8 118.9 . . ? C3 C8 H8 118.9 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N1 119.4(15) . . ? C11 C10 C15 119.1(17) . . ? N1 C10 C15 121.2(15) . . ? C10 C11 C12 119.9(17) . . ? C10 C11 P1 115.8(14) . . ? C12 C11 P1 124.2(14) . . ? C13 C12 C11 123.2(19) . . ? C13 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C14 C13 C12 115.6(19) . . ? C14 C13 C16 123(2) . . ? C12 C13 C16 121(2) . . ? C13 C14 C15 123.1(19) . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C14 C15 C10 118.6(19) . . ? C14 C15 H15 120.7 . . ? C10 C15 H15 120.7 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 113(2) . . ? C18 C17 P2 113.3(19) . . ? C19 C17 P2 106.4(19) . . ? C18 C17 H17 108.0 . . ? C19 C17 H17 108.0 . . ? P2 C17 H17 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111(2) . . ? C21 C20 P2 111.7(15) . . ? C22 C20 P2 111.6(18) . . ? C21 C20 H20 107.4 . . ? C22 C20 H20 107.4 . . ? P2 C20 H20 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 111(2) . . ? C25 C23 P1 114.2(19) . . ? C24 C23 P1 111.7(18) . . ? C25 C23 H23 106.3 . . ? C24 C23 H23 106.3 . . ? P1 C23 H23 106.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 108(2) . . ? C27 C26 P1 113.6(14) . . ? C28 C26 P1 110.6(17) . . ? C27 C26 H26 108.2 . . ? C28 C26 H26 108.2 . . ? P1 C26 H26 108.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C2A 1.90(3) . ? Mo1 C1 1.95(3) . ? Mo1 N1 2.090(14) . ? Mo1 C2B 2.36(5) . ? Mo1 I1B 2.43(2) . ? Mo1 P2 2.501(5) . ? Mo1 P1 2.514(5) . ? Mo1 I1A 2.803(2) . ? O2A C2A 1.26(4) . ? O2B C2B 1.26(4) . ? P1 C11 1.827(18) . ? P1 C26 1.85(2) . ? P1 C23 1.85(2) . ? P2 C4 1.803(19) . ? P2 C20 1.87(2) . ? P2 C17 1.87(2) . ? O1 C1 1.16(3) . ? N1 C10 1.41(2) . ? N1 C3 1.44(2) . ? C3 C8 1.39(3) . ? C3 C4 1.40(3) . ? C4 C5 1.43(3) . ? C5 C6 1.41(3) . ? C5 H5 0.9500 . ? C6 C7 1.41(3) . ? C6 C9 1.51(3) . ? C7 C8 1.36(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.37(2) . ? C10 C15 1.42(3) . ? C11 C12 1.41(3) . ? C12 C13 1.40(3) . ? C12 H12 0.9500 . ? C13 C14 1.38(3) . ? C13 C16 1.49(3) . ? C14 C15 1.41(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.48(4) . ? C17 C19 1.58(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.48(3) . ? C20 C22 1.52(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.51(4) . ? C23 C24 1.53(4) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.54(3) . ? C26 C28 1.55(3) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C18 H18B I1A^a 0.98 3.32 4.26(3) 160.9 2_655 yes C20 H20 I1A^a 1.00 3.29 3.79(2) 112.4 . yes C21 H21A I1A^a 0.98 3.33 4.01(2) 128.2 . yes C24 H24A O1 0.98 2.50 3.44(4) 159.8 . yes C27 H27C I1A^a 0.98 3.11 4.04(2) 157.3 . yes C28 H28B I1B^b 0.98 3.27 3.92(4) 126.0 . yes 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 C10 N1 C3 C8 -30(2) . . . . ? Mo1 N1 C3 C8 141.6(15) . . . . ? C10 N1 C3 C4 153.4(16) . . . . ? Mo1 N1 C3 C4 -35(2) . . . . ? C8 C3 C4 C5 3(3) . . . . ? N1 C3 C4 C5 179.6(16) . . . . ? C8 C3 C4 P2 -175.4(14) . . . . ? N1 C3 C4 P2 2(2) . . . . ? C20 P2 C4 C3 -97.1(15) . . . . ? C17 P2 C4 C3 152.2(16) . . . . ? Mo1 P2 C4 C3 23.5(14) . . . . ? C20 P2 C4 C5 84.9(18) . . . . ? C17 P2 C4 C5 -26(2) . . . . ? Mo1 P2 C4 C5 -154.5(16) . . . . ? C3 C4 C5 C6 -5(3) . . . . ? P2 C4 C5 C6 173.4(15) . . . . ? C4 C5 C6 C7 4(3) . . . . ? C4 C5 C6 C9 -178(2) . . . . ? C5 C6 C7 C8 -2(3) . . . . ? C9 C6 C7 C8 180(2) . . . . ? C6 C7 C8 C3 0(3) . . . . ? C4 C3 C8 C7 0(3) . . . . ? N1 C3 C8 C7 -177.1(17) . . . . ? C3 N1 C10 C11 151.7(16) . . . . ? Mo1 N1 C10 C11 -19(2) . . . . ? C3 N1 C10 C15 -34(2) . . . . ? Mo1 N1 C10 C15 154.7(14) . . . . ? N1 C10 C11 C12 177.2(17) . . . . ? C15 C10 C11 C12 3(3) . . . . ? N1 C10 C11 P1 0(2) . . . . ? C15 C10 C11 P1 -173.6(14) . . . . ? C26 P1 C11 C10 140.2(14) . . . . ? C23 P1 C11 C10 -109.5(15) . . . . ? Mo1 P1 C11 C10 12.7(14) . . . . ? C26 P1 C11 C12 -36.5(19) . . . . ? C23 P1 C11 C12 73.9(19) . . . . ? Mo1 P1 C11 C12 -163.9(16) . . . . ? C10 C11 C12 C13 -1(3) . . . . ? P1 C11 C12 C13 176.0(17) . . . . ? C11 C12 C13 C14 1(3) . . . . ? C11 C12 C13 C16 180(2) . . . . ? C12 C13 C14 C15 -5(3) . . . . ? C16 C13 C14 C15 177(2) . . . . ? C13 C14 C15 C10 8(3) . . . . ? C11 C10 C15 C14 -7(3) . . . . ? N1 C10 C15 C14 179.5(18) . . . . ? C4 P2 C17 C18 -63(2) . . . . ? C20 P2 C17 C18 -175(2) . . . . ? Mo1 P2 C17 C18 46(2) . . . . ? C4 P2 C17 C19 172.1(19) . . . . ? C20 P2 C17 C19 60(2) . . . . ? Mo1 P2 C17 C19 -78(2) . . . . ? C4 P2 C20 C21 63.8(19) . . . . ? C17 P2 C20 C21 175.9(17) . . . . ? Mo1 P2 C20 C21 -41.8(19) . . . . ? C4 P2 C20 C22 -61.2(18) . . . . ? C17 P2 C20 C22 50.9(19) . . . . ? Mo1 P2 C20 C22 -166.8(14) . . . . ? C11 P1 C23 C25 -55(2) . . . . ? C26 P1 C23 C25 56(2) . . . . ? Mo1 P1 C23 C25 -164.8(16) . . . . ? C11 P1 C23 C24 73(2) . . . . ? C26 P1 C23 C24 -176.7(19) . . . . ? Mo1 P1 C23 C24 -37(2) . . . . ? C11 P1 C26 C27 -57.0(18) . . . . ? C23 P1 C26 C27 -169.1(16) . . . . ? Mo1 P1 C26 C27 54.2(18) . . . . ? C11 P1 C26 C28 -178.5(17) . . . . ? C23 P1 C26 C28 69.4(19) . . . . ? Mo1 P1 C26 C28 -67.2(18) . . . . ?