#------------------------------------------------------------------------------ #$Date: 2026-06-05 20:05:34 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306407 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721020.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_7721020 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_issue 20 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7816 _journal_page_last 7820 _journal_paper_doi 10.1039/d6dt00920d _journal_volume 55 _journal_year 2026 _chemical_formula_sum 'C26 H40 Br Mo N O P2' _chemical_formula_weight 620.38 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc2qfw9c _audit_creation_method SHELXL-2013 _audit_update_record ; 2025-12-14 deposited with the CCDC. 2026-05-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.018(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.4244(3) _cell_length_b 9.5870(3) _cell_length_c 12.5215(3) _cell_measurement_reflns_used 8033 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 77.8200 _cell_measurement_theta_min 3.5690 _cell_volume 1361.15(6) _computing_cell_refinement 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _computing_data_reduction 'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 12854 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.074 _diffrn_reflns_theta_min 4.612 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.906 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.514 _exptl_crystal_description plate _exptl_crystal_F_000 636 _exptl_crystal_size_max 0.242 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.021 _refine_diff_density_max 0.816 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.103 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 2580 _refine_ls_number_restraints 350 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0512 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+4.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1475 _refine_ls_wR_factor_ref 0.1497 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2405 _reflns_number_total 2580 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00920d2.cif _cod_data_source_block SM-882a_faces _cod_depositor_comments 'Adding full bibliography for 7721018--7721021.cif.' _cod_original_sg_symbol_H-M 'P 2/n' _cod_database_code 7721020 _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. ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL SM-882a_faces in P3/n CELL 1.54184 11.42441 9.58703 12.52148 90.0000 97.018 90.0000 ZERR 2.00 0.00028 0.00027 0.00028 0.0000 0.002 0.0000 LATT 1 SYMM 1/2-X, Y, 1/2-Z SFAC C H N O P BR MO UNIT 52 80 2 2 4 2 2 TEMP -153 L.S. 11 SHEL .82 11. ISOR .015 SIMU .015 DELU .015 BOND ACTA CONF REM Instructions for potential hydrogen bonds HTAB C9 Br1 EQIV $1 -x+3/2, y, -z+3/2 HTAB C9 O1_$1 HTAB C12 O1 HTAB C12B O1 LIST 4 FMAP -2 PLAN 10 REM EXTI 0.000091 WGHT 0.073000 4.200000 FVAR 5.16430 MO1 7 0.748653 0.862521 0.707548 10.50000 0.02159 0.02935 = 0.03834 0.00437 0.00694 0.00055 BR1 6 0.752949 1.056777 0.847695 10.50000 0.03047 0.04300 = 0.09447 -0.02903 0.00590 0.00113 O1 4 0.758099 0.916988 0.578459 10.50000 0.02121 0.04518 = 0.05373 0.01825 0.00478 -0.00147 N1 3 0.750000 0.646890 0.750000 10.50000 0.01939 0.02285 = 0.11196 0.00000 0.00591 0.00000 P1 5 0.539860 0.809850 0.706777 11.00000 0.01987 0.02536 = 0.03954 -0.00231 0.01229 -0.00059 C1 1 0.650977 0.572568 0.779236 11.00000 0.02177 0.02572 = 0.06286 -0.00619 -0.00051 -0.00198 C2 1 0.540177 0.638307 0.765677 11.00000 0.02292 0.02691 = 0.03530 -0.00397 0.00284 -0.00157 C3 1 0.442963 0.572871 0.802138 11.00000 0.02598 0.03332 = 0.03468 -0.00290 0.00818 -0.00167 AFIX 43 H3 2 0.368760 0.618863 0.792804 11.00000 -1.20000 AFIX 0 C4 1 0.451367 0.443539 0.851277 11.00000 0.04077 0.03202 = 0.03334 -0.00208 0.01035 -0.00590 C5 1 0.561704 0.378533 0.863068 11.00000 0.04749 0.02854 = 0.04316 -0.00020 -0.00218 0.00008 AFIX 43 H5 2 0.570141 0.289427 0.896309 11.00000 -1.20000 AFIX 0 C6 1 0.658943 0.441167 0.827364 11.00000 0.02989 0.02815 = 0.06939 -0.00157 -0.00817 0.00210 AFIX 43 H6 2 0.732508 0.393744 0.835803 11.00000 -1.20000 AFIX 0 C7 1 0.347484 0.377279 0.895677 11.00000 0.05743 0.03795 = 0.04618 -0.00096 0.02463 -0.01074 AFIX 137 H7A 2 0.351683 0.275696 0.888278 11.00000 -1.50000 H7B 2 0.274016 0.411522 0.855676 11.00000 -1.50000 H7C 2 0.349367 0.401636 0.971879 11.00000 -1.50000 AFIX 0 C8 1 0.422253 0.910431 0.757524 11.00000 0.02004 0.03146 = 0.02765 -0.00405 0.00843 0.00051 AFIX 13 H8 2 0.346519 0.858259 0.740185 11.00000 -1.20000 AFIX 0 C9 1 0.444984 0.929111 0.878797 11.00000 0.04624 0.04473 = 0.02795 -0.00376 0.01138 -0.00008 AFIX 137 H9A 2 0.377857 0.977223 0.904078 11.00000 -1.50000 H9B 2 0.516654 0.984638 0.897079 11.00000 -1.50000 H9C 2 0.455100 0.837519 0.913447 11.00000 -1.50000 AFIX 0 C10 1 0.410253 1.051166 0.699827 11.00000 0.03610 0.03542 = 0.03880 0.00212 0.01263 0.01136 AFIX 137 H10A 2 0.351898 1.108455 0.730860 11.00000 -1.50000 H10B 2 0.384535 1.036260 0.623117 11.00000 -1.50000 H10C 2 0.486634 1.099002 0.708518 11.00000 -1.50000 AFIX 0 EADP c11 c11b EADP c12 c12b EADP c13 c13b SAME .01 c11b c12b c13b PART 1 C11 1 0.469106 0.781631 0.555660 10.50000 0.03201 0.03817 = 0.02782 -0.00541 0.01026 0.00446 AFIX 13 H11 2 0.471225 0.873563 0.518214 10.50000 -1.20000 AFIX 0 C12 1 0.547378 0.679615 0.499855 10.50000 0.04629 0.03442 = 0.03515 -0.00486 0.01959 0.00524 AFIX 137 H12A 2 0.509818 0.659605 0.426865 10.50000 -1.50000 H12B 2 0.557010 0.592645 0.541121 10.50000 -1.50000 H12C 2 0.624849 0.722023 0.496258 10.50000 -1.50000 AFIX 0 C13 1 0.342440 0.735865 0.545717 10.50000 0.03165 0.09607 = 0.04348 -0.03473 -0.00079 -0.00025 AFIX 137 H13A 2 0.308607 0.738946 0.469965 10.50000 -1.50000 H13B 2 0.298031 0.798425 0.587820 10.50000 -1.50000 H13C 2 0.338075 0.640376 0.572884 10.50000 -1.50000 AFIX 0 PART 2 C11B 1 0.508292 0.786402 0.568509 10.50000 0.03201 0.03817 = 0.02782 -0.00541 0.01026 0.00446 AFIX 13 H11B 2 0.507270 0.880747 0.534346 10.50000 -1.20000 AFIX 0 C12B 1 0.608038 0.701377 0.525806 10.50000 0.04629 0.03442 = 0.03515 -0.00486 0.01959 0.00524 AFIX 137 H12D 2 0.590145 0.689369 0.447796 10.50000 -1.50000 H12E 2 0.614106 0.609698 0.560662 10.50000 -1.50000 H12F 2 0.682991 0.751253 0.541937 10.50000 -1.50000 AFIX 0 C13B 1 0.388628 0.721708 0.537514 10.50000 0.03165 0.09607 = 0.04348 -0.03473 -0.00079 -0.00025 AFIX 137 H13D 2 0.378773 0.699689 0.460510 10.50000 -1.50000 H13E 2 0.327188 0.787461 0.552925 10.50000 -1.50000 H13F 2 0.382168 0.635936 0.578967 10.50000 -1.50000 PART 0 REM REM SM-882a_faces.hkl REM AFIX 0 HKLF 4 REM SM-882a_faces in P3/n REM R1 = 0.0512 for 2405 Fo > 4sig(Fo) and 0.0540 for all 2580 data REM 175 parameters refined using 350 restraints END WGHT 0.0728 4.0556 REM Highest difference peak 0.816, deepest hole -0.650, 1-sigma level 0.103 Q1 1 0.7500 0.7394 0.7500 10.50000 0.05 0.82 Q2 1 0.7585 1.0511 0.8967 11.00000 0.05 -0.65 Q3 1 0.7449 0.6459 0.7066 11.00000 0.05 0.61 Q4 1 0.5331 0.7979 0.6797 11.00000 0.05 0.60 Q5 1 0.6458 0.8994 0.7137 11.00000 0.05 0.59 Q6 1 0.5424 0.7628 0.7192 11.00000 0.05 0.58 Q7 1 0.5078 0.8242 0.7177 11.00000 0.05 0.54 Q8 1 0.7756 0.8369 0.7202 11.00000 0.05 -0.51 Q9 1 0.7802 0.8829 0.7079 11.00000 0.05 -0.49 Q10 1 0.7100 0.8642 0.7013 11.00000 0.05 -0.49 ; _shelx_res_checksum 11667 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -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 0.74865(5) 0.86252(6) 0.70755(5) 0.0295(2) Uani 0.5 1 d . U P A . Br1 Br 0.75295(8) 1.05678(11) 0.84769(10) 0.0561(3) Uani 0.5 1 d . U P . . O1 O 0.7581(5) 0.9170(7) 0.5785(5) 0.0400(13) Uani 0.5 1 d . U P . . N1 N 0.7500 0.6469(5) 0.7500 0.0516(15) Uani 1 2 d S TU P . . P1 P 0.53986(8) 0.80985(10) 0.70678(8) 0.0275(3) Uani 1 1 d . U . . . C1 C 0.6510(3) 0.5726(4) 0.7792(4) 0.0373(9) Uani 1 1 d . U . . . C2 C 0.5402(3) 0.6383(4) 0.7657(3) 0.0284(8) Uani 1 1 d . U . . . C3 C 0.4430(3) 0.5729(4) 0.8021(3) 0.0310(8) Uani 1 1 d . U . . . H3 H 0.3688 0.6189 0.7928 0.037 Uiso 1 1 calc R U . . . C4 C 0.4514(4) 0.4435(4) 0.8513(3) 0.0349(9) Uani 1 1 d . U . . . C5 C 0.5617(4) 0.3785(5) 0.8631(3) 0.0404(10) Uani 1 1 d . U . . . H5 H 0.5701 0.2894 0.8963 0.048 Uiso 1 1 calc R U . . . C6 C 0.6589(4) 0.4412(4) 0.8274(4) 0.0437(10) Uani 1 1 d . U . . . H6 H 0.7325 0.3937 0.8358 0.052 Uiso 1 1 calc R U . . . C7 C 0.3475(5) 0.3773(5) 0.8957(4) 0.0457(11) Uani 1 1 d . U . . . H7A H 0.3517 0.2757 0.8883 0.069 Uiso 1 1 calc R U . . . H7B H 0.2740 0.4115 0.8557 0.069 Uiso 1 1 calc R U . . . H7C H 0.3494 0.4016 0.9719 0.069 Uiso 1 1 calc R U . . . C8 C 0.4223(3) 0.9104(4) 0.7575(3) 0.0259(7) Uani 1 1 d . U . . . H8 H 0.3465 0.8583 0.7402 0.031 Uiso 1 1 calc R U . . . C9 C 0.4450(4) 0.9291(5) 0.8788(3) 0.0391(9) Uani 1 1 d . U . . . H9A H 0.3779 0.9772 0.9041 0.059 Uiso 1 1 calc R U . . . H9B H 0.5167 0.9846 0.8971 0.059 Uiso 1 1 calc R U . . . H9C H 0.4551 0.8375 0.9134 0.059 Uiso 1 1 calc R U . . . C10 C 0.4103(4) 1.0512(4) 0.6998(3) 0.0361(9) Uani 1 1 d . U . . . H10A H 0.3519 1.1085 0.7309 0.054 Uiso 1 1 calc R U . . . H10B H 0.3845 1.0363 0.6231 0.054 Uiso 1 1 calc R U . . . H10C H 0.4866 1.0990 0.7085 0.054 Uiso 1 1 calc R U . . . C11 C 0.4691(8) 0.7816(14) 0.5557(11) 0.0321(16) Uani 0.5 1 d D U P A 1 H11 H 0.4712 0.8736 0.5182 0.039 Uiso 0.5 1 calc R U P A 1 C12 C 0.5474(9) 0.6796(10) 0.4999(7) 0.0374(16) Uani 0.5 1 d D U P A 1 H12A H 0.5098 0.6596 0.4269 0.056 Uiso 0.5 1 calc R U P A 1 H12B H 0.5570 0.5926 0.5411 0.056 Uiso 0.5 1 calc R U P A 1 H12C H 0.6248 0.7220 0.4963 0.056 Uiso 0.5 1 calc R U P A 1 C13 C 0.3424(9) 0.7359(18) 0.5457(12) 0.058(2) Uani 0.5 1 d D U P A 1 H13A H 0.3086 0.7389 0.4700 0.086 Uiso 0.5 1 calc R U P A 1 H13B H 0.2980 0.7984 0.5878 0.086 Uiso 0.5 1 calc R U P A 1 H13C H 0.3381 0.6404 0.5729 0.086 Uiso 0.5 1 calc R U P A 1 C11B C 0.5083(8) 0.7864(14) 0.5685(11) 0.0321(16) Uani 0.5 1 d D U P A 2 H11B H 0.5073 0.8807 0.5343 0.039 Uiso 0.5 1 calc R U P A 2 C12B C 0.6080(9) 0.7014(10) 0.5258(8) 0.0374(16) Uani 0.5 1 d D U P A 2 H12D H 0.5901 0.6894 0.4478 0.056 Uiso 0.5 1 calc R U P A 2 H12E H 0.6141 0.6097 0.5607 0.056 Uiso 0.5 1 calc R U P A 2 H12F H 0.6830 0.7513 0.5419 0.056 Uiso 0.5 1 calc R U P A 2 C13B C 0.3886(9) 0.7217(18) 0.5375(12) 0.058(2) Uani 0.5 1 d D U P A 2 H13D H 0.3788 0.6997 0.4605 0.086 Uiso 0.5 1 calc R U P A 2 H13E H 0.3272 0.7875 0.5529 0.086 Uiso 0.5 1 calc R U P A 2 H13F H 0.3822 0.6359 0.5790 0.086 Uiso 0.5 1 calc R U P A 2 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 0.0216(3) 0.0293(4) 0.0383(3) 0.0044(2) 0.0069(3) 0.0005(2) Br1 0.0305(5) 0.0430(6) 0.0945(8) -0.0290(5) 0.0059(5) 0.0011(4) O1 0.021(2) 0.045(3) 0.054(3) 0.018(3) 0.005(2) -0.001(2) N1 0.019(2) 0.023(2) 0.112(5) 0.000 0.006(3) 0.000 P1 0.0199(5) 0.0254(5) 0.0395(5) -0.0023(4) 0.0123(4) -0.0006(3) C1 0.0218(18) 0.0257(19) 0.063(3) -0.0062(17) -0.0005(17) -0.0020(15) C2 0.0229(18) 0.0269(18) 0.0353(19) -0.0040(14) 0.0028(14) -0.0016(14) C3 0.0260(18) 0.033(2) 0.0347(19) -0.0029(15) 0.0082(14) -0.0017(15) C4 0.041(2) 0.032(2) 0.0333(19) -0.0021(16) 0.0104(16) -0.0059(17) C5 0.047(2) 0.029(2) 0.043(2) -0.0002(17) -0.0022(18) 0.0001(18) C6 0.030(2) 0.028(2) 0.069(3) -0.0016(19) -0.0082(19) 0.0021(16) C7 0.057(3) 0.038(2) 0.046(2) -0.0010(19) 0.025(2) -0.011(2) C8 0.0200(16) 0.0315(19) 0.0276(17) -0.0040(14) 0.0084(13) 0.0005(14) C9 0.046(2) 0.045(2) 0.0279(19) -0.0038(17) 0.0114(17) -0.0001(19) C10 0.036(2) 0.035(2) 0.039(2) 0.0021(17) 0.0126(16) 0.0114(17) C11 0.032(4) 0.038(2) 0.028(3) -0.005(2) 0.010(4) 0.004(4) C12 0.046(4) 0.034(3) 0.035(4) -0.005(3) 0.020(3) 0.005(4) C13 0.032(5) 0.096(5) 0.043(3) -0.035(3) -0.001(5) 0.000(6) C11B 0.032(4) 0.038(2) 0.028(3) -0.005(2) 0.010(4) 0.004(4) C12B 0.046(4) 0.034(3) 0.035(4) -0.005(3) 0.020(3) 0.005(4) C13B 0.032(5) 0.096(5) 0.043(3) -0.035(3) -0.001(5) 0.000(6) 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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' 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 Mo1 Mo1 O1 161.5(2) 2_656 . ? Mo1 Mo1 Br1 110.32(4) 2_656 2_656 ? O1 Mo1 Br1 52.0(2) . 2_656 ? Mo1 Mo1 N1 75.62(4) 2_656 . ? O1 Mo1 N1 122.0(2) . . ? Br1 Mo1 N1 174.05(6) 2_656 . ? Mo1 Mo1 P1 84.98(6) 2_656 . ? O1 Mo1 P1 103.51(18) . . ? Br1 Mo1 P1 103.04(4) 2_656 . ? N1 Mo1 P1 77.15(3) . . ? Mo1 Mo1 Br1 46.79(3) 2_656 . ? O1 Mo1 Br1 115.3(2) . . ? Br1 Mo1 Br1 63.53(7) 2_656 . ? N1 Mo1 Br1 122.41(5) . . ? P1 Mo1 Br1 95.19(4) . . ? Mo1 Mo1 P1 70.78(6) 2_656 2_656 ? O1 Mo1 P1 106.80(18) . 2_656 ? Br1 Mo1 P1 107.32(4) 2_656 2_656 ? N1 Mo1 P1 74.22(3) . 2_656 ? P1 Mo1 P1 146.14(4) . 2_656 ? Br1 Mo1 P1 85.32(4) . 2_656 ? O1 Br1 Mo1 55.4(2) 2_656 2_656 ? O1 Br1 Br1 124.8(2) 2_656 2_656 ? Mo1 Br1 Br1 69.68(4) 2_656 2_656 ? O1 Br1 Mo1 78.2(2) 2_656 . ? Mo1 Br1 Mo1 22.89(3) 2_656 . ? Br1 Br1 Mo1 46.79(3) 2_656 . ? Br1 O1 Mo1 72.5(3) 2_656 . ? C1 N1 C1 119.9(5) 2_656 . ? C1 N1 Mo1 124.6(2) 2_656 2_656 ? C1 N1 Mo1 113.8(2) . 2_656 ? C1 N1 Mo1 113.8(2) 2_656 . ? C1 N1 Mo1 124.6(2) . . ? Mo1 N1 Mo1 28.75(7) 2_656 . ? C11B P1 C2 106.2(5) . . ? C11B P1 C8 110.0(3) . . ? C2 P1 C8 107.68(17) . . ? C2 P1 C11 104.3(4) . . ? C8 P1 C11 99.9(3) . . ? C11B P1 Mo1 96.6(3) . . ? C2 P1 Mo1 103.56(12) . . ? C8 P1 Mo1 130.49(13) . . ? C11 P1 Mo1 108.5(3) . . ? C11B P1 Mo1 120.7(3) . 2_656 ? C2 P1 Mo1 93.08(12) . 2_656 ? C8 P1 Mo1 116.37(12) . 2_656 ? C11 P1 Mo1 132.7(3) . 2_656 ? Mo1 P1 Mo1 24.24(3) . 2_656 ? C6 C1 C2 117.9(4) . . ? C6 C1 N1 123.5(4) . . ? C2 C1 N1 118.5(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 P1 125.5(3) . . ? C1 C2 P1 114.5(3) . . ? C4 C3 C2 122.2(4) . . ? C3 C4 C5 117.4(4) . . ? C3 C4 C7 121.7(4) . . ? C5 C4 C7 120.8(4) . . ? C6 C5 C4 121.4(4) . . ? C5 C6 C1 121.3(4) . . ? C9 C8 C10 111.3(3) . . ? C9 C8 P1 111.5(3) . . ? C10 C8 P1 109.2(2) . . ? C13 C11 C12 112.4(8) . . ? C13 C11 P1 113.3(9) . . ? C12 C11 P1 109.0(7) . . ? C13B C11B C12B 112.1(8) . . ? C13B C11B P1 112.4(10) . . ? C12B C11B P1 109.9(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo1 1.0598(12) 2_656 ? Mo1 O1 1.715(6) . ? Mo1 Br1 1.9860(11) 2_656 ? Mo1 N1 2.134(5) . ? Mo1 P1 2.4371(10) . ? Mo1 Br1 2.5552(12) . ? Mo1 P1 2.5710(11) 2_656 ? Br1 O1 1.642(7) 2_656 ? Br1 Mo1 1.9860(11) 2_656 ? Br1 Br1 2.439(3) 2_656 ? O1 Br1 1.642(7) 2_656 ? N1 C1 1.422(5) 2_656 ? N1 C1 1.422(5) . ? N1 Mo1 2.134(5) 2_656 ? P1 C11B 1.739(12) . ? P1 C2 1.802(4) . ? P1 C8 1.830(4) . ? P1 C11 1.983(12) . ? P1 Mo1 2.5710(11) 2_656 ? C1 C6 1.395(6) . ? C1 C2 1.406(5) . ? C2 C3 1.400(5) . ? C3 C4 1.382(6) . ? C4 C5 1.398(6) . ? C4 C7 1.511(6) . ? C5 C6 1.384(7) . ? C8 C9 1.520(5) . ? C8 C10 1.529(5) . ? C11 C13 1.503(11) . ? C11 C12 1.548(9) . ? C11B C13B 1.508(11) . ? C11B C12B 1.548(8) . ? 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 C9 H9B Br1 0.98 2.93 3.790(5) 147.7 . C9 H9B O1 0.98 2.64 3.371(7) 132.0 2_656 C12 H12C O1 0.98 2.55 3.371(12) 141.7 . C12B H12F O1 0.98 1.84 2.715(12) 147.5 . 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 Mo1 O1 Br1 -19.6(7) 2_656 . . 2_656 ? N1 Mo1 O1 Br1 179.27(6) . . . 2_656 ? P1 Mo1 O1 Br1 96.13(15) . . . 2_656 ? Br1 Mo1 O1 Br1 -6.4(2) . . . 2_656 ? P1 Mo1 O1 Br1 -99.14(15) 2_656 . . 2_656 ? C1 N1 C1 C6 29.7(3) 2_656 . . . ? Mo1 N1 C1 C6 -135.8(4) 2_656 . . . ? Mo1 N1 C1 C6 -166.5(3) . . . . ? C1 N1 C1 C2 -154.7(4) 2_656 . . . ? Mo1 N1 C1 C2 39.8(4) 2_656 . . . ? Mo1 N1 C1 C2 9.2(5) . . . . ? C6 C1 C2 C3 1.3(6) . . . . ? N1 C1 C2 C3 -174.5(3) . . . . ? C6 C1 C2 P1 178.1(3) . . . . ? N1 C1 C2 P1 2.2(5) . . . . ? C11B P1 C2 C3 -92.1(4) . . . . ? C8 P1 C2 C3 25.7(4) . . . . ? C11 P1 C2 C3 -79.8(4) . . . . ? Mo1 P1 C2 C3 166.8(3) . . . . ? Mo1 P1 C2 C3 144.7(3) 2_656 . . . ? C11B P1 C2 C1 91.3(4) . . . . ? C8 P1 C2 C1 -150.8(3) . . . . ? C11 P1 C2 C1 103.6(4) . . . . ? Mo1 P1 C2 C1 -9.8(3) . . . . ? Mo1 P1 C2 C1 -31.9(3) 2_656 . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? P1 C2 C3 C4 -176.8(3) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C2 C3 C4 C7 176.7(4) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C7 C4 C5 C6 -176.9(4) . . . . ? C4 C5 C6 C1 0.7(7) . . . . ? C2 C1 C6 C5 -1.5(7) . . . . ? N1 C1 C6 C5 174.1(4) . . . . ? C11B P1 C8 C9 178.2(6) . . . . ? C2 P1 C8 C9 62.9(3) . . . . ? C11 P1 C8 C9 171.4(5) . . . . ? Mo1 P1 C8 C9 -63.7(3) . . . . ? Mo1 P1 C8 C9 -39.9(3) 2_656 . . . ? C11B P1 C8 C10 -58.5(6) . . . . ? C2 P1 C8 C10 -173.8(3) . . . . ? C11 P1 C8 C10 -65.2(5) . . . . ? Mo1 P1 C8 C10 59.6(3) . . . . ? Mo1 P1 C8 C10 83.5(3) 2_656 . . . ? C2 P1 C11B C13B 61.8(9) . . . . ? C8 P1 C11B C13B -54.5(9) . . . . ? C11 P1 C11B C13B -20(4) . . . . ? Mo1 P1 C11B C13B 168.0(8) . . . . ? Mo1 P1 C11B C13B 165.5(7) 2_656 . . . ? C2 P1 C11B C12B -63.8(9) . . . . ? C8 P1 C11B C12B 179.9(7) . . . . ? C11 P1 C11B C12B -146(4) . . . . ? Mo1 P1 C11B C12B 42.4(9) . . . . ? Mo1 P1 C11B C12B 40.0(10) 2_656 . . . ?