#------------------------------------------------------------------------------ #$Date: 2020-08-15 04:54:03 +0300 (Sat, 15 Aug 2020) $ #$Revision: 255334 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705163.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_7705163 loop_ _publ_author_name 'He, Zhiyuan' 'Xue, Xiaolian' 'Liu, Yilan' 'Yu, Na' 'Krogman, Jeremy P.' _publ_section_title ; Aminolysis of Bis[bis(trimethylsilyl)amido]-Manganese, -Iron, and -Cobalt for the Synthesis of Mono- and Bis-Silylene Complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT00570C _journal_year 2020 _chemical_formula_moiety 'C30 H46 Br0.84 Cl3.16 Mn N4 Si2' _chemical_formula_sum 'C30 H46 Br0.84 Cl3.16 Mn N4 Si2' _chemical_formula_weight 752.97 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-12-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-02-14 deposited with the CCDC. 2020-08-05 downloaded from the CCDC. ; _cell_angle_alpha 77.080(4) _cell_angle_beta 79.212(4) _cell_angle_gamma 73.855(4) _cell_formula_units_Z 2 _cell_length_a 10.5954(9) _cell_length_b 10.9184(8) _cell_length_c 17.2222(14) _cell_measurement_reflns_used 6237 _cell_measurement_temperature 150.03 _cell_measurement_theta_max 26.433 _cell_measurement_theta_min 2.449 _cell_volume 1848.6(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 0.0814 _diffrn_reflns_av_unetI/netI 0.0600 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 35332 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.020 _diffrn_reflns_theta_min 2.443 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.583 _exptl_absorpt_correction_T_max 0.0277 _exptl_absorpt_correction_T_min 0.0104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0768 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.3755. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.353 _exptl_crystal_description block _exptl_crystal_F_000 780 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Diethyl Ether' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.187 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.519 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 433 _refine_ls_number_reflns 7211 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0461 _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^)+(0.0372P)^2^+1.5811P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.1096 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4630 _reflns_number_total 7211 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 4 _cod_database_code 7705163 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.845 _shelx_estimated_absorpt_t_min 0.623 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C11-C28 \\sim C11-C33 with sigma of 0.02 C11-C29 \\sim C11-C32 with sigma of 0.02 C11-C30 \\sim C11-C31 with sigma of 0.02 3. Others Sof(Br1)=1-FVAR(1) Sof(Cl1)=FVAR(1) Sof(Br2)=1-FVAR(2) Sof(Cl2)=FVAR(2) Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)= Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(3) Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)= Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3) 4.a Aromatic/amide H refined with riding coordinates: C3(H3), C12(H12), C13(H13), C15(H15), C17(H17), C18(H18), C21(H21), C24(H24), C25(H25), C26(H26) 4.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B, H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A, H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C) ; _shelx_res_file ; mo_hzy241_0m.res created by SHELXL-2014/7 TITL mo_hzy241_0m_a.res in P-1 REM Old TITL mo_hzy241_0m_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.198, Rweak 0.023, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C30 Br Cl2 Mn N4 Si2 CELL 0.71073 10.5954 10.9184 17.2222 77.08 79.212 73.855 ZERR 2 0.0009 0.0008 0.0014 0.004 0.004 0.004 LATT 1 SFAC C H Br Cl Mn N Si UNIT 60 92 1.68 6.32 2 8 4 SADI C11 C28 C11 C33 SADI C11 C29 C11 C32 SADI C11 C30 C11 C31 L.S. 10 PLAN 10 SIZE 0.11 0.187 0.33 TEMP -123.12 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.037200 1.581100 FVAR 0.48596 0.45347 0.70724 0.38039 MN01 5 0.400937 0.324595 0.271516 11.00000 0.03620 0.03745 = 0.03521 -0.00851 -0.00811 -0.00806 CL3 4 0.590863 -0.018587 0.194986 11.00000 0.05068 0.04139 = 0.04703 -0.01226 -0.01697 -0.00148 CL4 4 0.778147 0.257910 0.190551 11.00000 0.04344 0.09228 = 0.03843 -0.01382 -0.00449 -0.01930 SI1 7 0.432993 0.145975 0.184478 11.00000 0.03846 0.03558 = 0.03326 -0.00774 -0.00808 -0.00952 SI2 7 0.644707 0.310953 0.289734 11.00000 0.04032 0.04337 = 0.03323 -0.00228 -0.01217 -0.01512 N1 6 0.724072 0.220089 0.378295 11.00000 0.03290 0.03697 = 0.03095 -0.00509 -0.00747 -0.01023 N2 6 0.714156 0.418956 0.326885 11.00000 0.04721 0.03668 = 0.03967 0.00349 -0.02040 -0.01698 N3 6 0.409747 0.187648 0.078400 11.00000 0.03968 0.03860 = 0.02926 -0.00301 -0.00808 -0.01191 N4 6 0.291267 0.090496 0.172839 11.00000 0.04171 0.04001 = 0.03108 -0.00313 -0.00913 -0.01339 C1 1 0.747839 0.327640 0.390788 11.00000 0.02706 0.04311 = 0.03403 -0.00487 -0.00630 -0.00854 C2 1 0.793105 0.344639 0.463585 11.00000 0.04352 0.02905 = 0.03473 -0.00507 -0.01122 -0.01159 C3 1 0.926350 0.320158 0.469347 11.00000 0.04125 0.04273 = 0.04165 -0.01030 -0.01033 -0.01161 AFIX 43 H3 2 0.990999 0.292187 0.426487 11.00000 -1.20000 AFIX 0 C4 1 0.716601 0.095690 0.434484 11.00000 0.03790 0.03462 = 0.03720 -0.00004 -0.01179 -0.01212 C5 1 0.293173 0.154047 0.096885 11.00000 0.03755 0.03618 = 0.03724 -0.01002 -0.00639 -0.00701 C6 1 0.603854 0.116796 0.502380 11.00000 0.04311 0.04475 = 0.03729 -0.00339 -0.00680 -0.01891 AFIX 137 H6A 2 0.621686 0.170330 0.535769 11.00000 -1.50000 H6B 2 0.595984 0.032859 0.535271 11.00000 -1.50000 H6C 2 0.520907 0.160862 0.480049 11.00000 -1.50000 AFIX 0 C7 1 0.187280 0.188485 0.043973 11.00000 0.03913 0.04010 = 0.03757 -0.00410 -0.00965 -0.00914 C8 1 0.500366 0.188011 -0.064065 11.00000 0.04399 0.04423 = 0.03932 -0.01261 -0.00651 -0.00850 AFIX 137 H8A 2 0.551227 0.099210 -0.046635 11.00000 -1.50000 H8B 2 0.552353 0.231148 -0.109740 11.00000 -1.50000 H8C 2 0.417252 0.185835 -0.080259 11.00000 -1.50000 AFIX 0 C9 1 0.379757 0.396241 -0.017684 11.00000 0.06137 0.03891 = 0.03718 -0.00767 -0.00598 -0.00894 AFIX 137 H9A 2 0.299609 0.388016 -0.034575 11.00000 -1.50000 H9B 2 0.426527 0.447359 -0.061951 11.00000 -1.50000 H9C 2 0.355102 0.439753 0.028894 11.00000 -1.50000 AFIX 0 C10 1 0.469733 0.262277 0.004920 11.00000 0.04244 0.03697 = 0.03403 -0.00360 -0.00598 -0.01282 C11 1 0.736958 0.550730 0.299166 11.00000 0.05868 0.03875 = 0.03989 0.00718 -0.01970 -0.02165 C12 1 0.698700 0.386412 0.526198 11.00000 0.04831 0.03949 = 0.04273 -0.00733 -0.00697 -0.01150 AFIX 43 H12 2 0.606964 0.405191 0.521772 11.00000 -1.20000 AFIX 0 C13 1 0.083450 0.296933 0.050850 11.00000 0.04495 0.05747 = 0.04614 -0.00793 -0.00714 -0.00396 AFIX 43 H13 2 0.080378 0.349705 0.088510 11.00000 -1.20000 AFIX 0 C14 1 0.692600 0.009231 0.382936 11.00000 0.06523 0.04062 = 0.04257 -0.00870 -0.01147 -0.01812 AFIX 137 H14A 2 0.606317 0.047479 0.363607 11.00000 -1.50000 H14B 2 0.693461 -0.077085 0.415237 11.00000 -1.50000 H14C 2 0.762633 0.001870 0.336915 11.00000 -1.50000 AFIX 0 C15 1 0.965225 0.336621 0.537994 11.00000 0.05471 0.05172 = 0.05413 -0.01010 -0.02406 -0.01858 AFIX 43 H15 2 1.056772 0.320673 0.542112 11.00000 -1.20000 AFIX 0 C16 1 0.848190 0.032399 0.467137 11.00000 0.04494 0.04153 = 0.05196 0.00624 -0.01491 -0.01018 AFIX 137 H16A 2 0.919869 0.021109 0.422248 11.00000 -1.50000 H16B 2 0.844622 -0.052391 0.500364 11.00000 -1.50000 H16C 2 0.864714 0.087769 0.499800 11.00000 -1.50000 AFIX 0 C17 1 0.738705 0.400462 0.594672 11.00000 0.06794 0.05082 = 0.04273 -0.01743 -0.00096 -0.01921 AFIX 43 H17 2 0.674619 0.427042 0.638119 11.00000 -1.20000 AFIX 0 C18 1 0.871708 0.375901 0.599975 11.00000 0.08372 0.04711 = 0.03755 -0.00934 -0.01887 -0.02445 AFIX 43 H18 2 0.898990 0.386286 0.647106 11.00000 -1.20000 AFIX 0 C19 1 0.598978 0.273811 0.026042 11.00000 0.05351 0.05670 = 0.04365 -0.00333 -0.00731 -0.02678 AFIX 137 H19A 2 0.579489 0.320917 0.070814 11.00000 -1.50000 H19B 2 0.645024 0.320963 -0.020795 11.00000 -1.50000 H19C 2 0.655464 0.186963 0.041679 11.00000 -1.50000 AFIX 0 C20 1 0.185206 0.041049 0.230585 11.00000 0.04711 0.05958 = 0.03866 -0.00183 -0.00760 -0.02566 C21 1 0.190952 0.113189 -0.011399 11.00000 0.04743 0.05358 = 0.05102 -0.01137 -0.01739 -0.00911 AFIX 43 H21 2 0.261871 0.038654 -0.016656 11.00000 -1.20000 AFIX 0 C22 1 0.256447 -0.054561 0.296508 11.00000 0.06486 0.07179 = 0.04955 0.01325 -0.01182 -0.03213 AFIX 137 H22A 2 0.321505 -0.124707 0.273381 11.00000 -1.50000 H22B 2 0.191908 -0.090801 0.337081 11.00000 -1.50000 H22C 2 0.301953 -0.009943 0.321650 11.00000 -1.50000 AFIX 0 C23 1 0.114858 -0.027546 0.190437 11.00000 0.06862 0.07736 = 0.05338 -0.01120 -0.00513 -0.04230 AFIX 137 H23A 2 0.065785 0.035621 0.149636 11.00000 -1.50000 H23B 2 0.053049 -0.067684 0.231000 11.00000 -1.50000 H23C 2 0.180571 -0.094620 0.164896 11.00000 -1.50000 AFIX 0 C24 1 -0.016314 0.328264 0.002387 11.00000 0.03832 0.07025 = 0.06179 0.00361 -0.00917 0.00493 AFIX 43 H24 2 -0.088337 0.402029 0.007262 11.00000 -1.20000 AFIX 0 C25 1 0.090422 0.147003 -0.059358 11.00000 0.06014 0.08072 = 0.05784 -0.01135 -0.02419 -0.02372 AFIX 43 H25 2 0.093036 0.095071 -0.097415 11.00000 -1.20000 AFIX 0 C26 1 -0.010556 0.252198 -0.052692 11.00000 0.04033 0.09538 = 0.05288 0.00383 -0.01986 -0.01482 AFIX 43 H26 2 -0.078314 0.274181 -0.086162 11.00000 -1.20000 AFIX 0 C27 1 0.087487 0.153742 0.264905 11.00000 0.04243 0.08247 = 0.05010 -0.01293 -0.00080 -0.02068 AFIX 137 H27A 2 0.133989 0.192723 0.293191 11.00000 -1.50000 H27B 2 0.017018 0.121958 0.302542 11.00000 -1.50000 H27C 2 0.048620 0.219007 0.221049 11.00000 -1.50000 AFIX 0 PART 1 CL1 4 0.287139 0.525342 0.193732 21.00000 0.05290 0.04758 = 0.02017 0.00137 -0.01603 0.02052 CL2 4 0.287246 0.259117 0.399038 31.00000 0.06043 0.06715 = 0.03878 0.00901 -0.01920 -0.01391 C28 1 0.690205 0.603419 0.217483 41.00000 0.11454 0.10612 = 0.04217 0.04534 -0.05089 -0.07956 AFIX 137 H28A 2 0.750625 0.555973 0.177585 41.00000 -1.50000 H28B 2 0.689104 0.695680 0.202061 41.00000 -1.50000 H28C 2 0.600647 0.592682 0.219971 41.00000 -1.50000 AFIX 0 C29 1 0.879762 0.560473 0.291814 41.00000 0.07058 0.04318 = 0.13260 0.01517 -0.05222 -0.02952 AFIX 137 H29A 2 0.907866 0.538413 0.345351 41.00000 -1.50000 H29B 2 0.885463 0.649174 0.267236 41.00000 -1.50000 H29C 2 0.937670 0.500090 0.258133 41.00000 -1.50000 AFIX 0 C30 1 0.644882 0.642915 0.352147 41.00000 0.13748 0.04829 = 0.04456 0.01179 0.02115 0.01328 AFIX 137 H30A 2 0.552519 0.649783 0.346941 41.00000 -1.50000 H30B 2 0.663411 0.728741 0.335207 41.00000 -1.50000 H30C 2 0.659587 0.609421 0.408319 41.00000 -1.50000 AFIX 0 PART 0 PART 2 BR1 3 0.298385 0.528654 0.192459 -21.00000 0.06728 0.04605 = 0.04368 -0.00478 -0.00526 -0.00572 BR2 3 0.285298 0.260897 0.399983 -31.00000 0.03424 0.03547 = 0.04394 -0.01010 0.00981 -0.01350 C31 1 0.694209 0.629606 0.366367 -41.00000 0.11669 0.02683 = 0.07102 -0.00287 -0.01763 -0.02014 AFIX 137 H31A 2 0.602602 0.628890 0.389695 -41.00000 -1.50000 H31B 2 0.699951 0.719132 0.344594 -41.00000 -1.50000 H31C 2 0.752563 0.591558 0.408060 -41.00000 -1.50000 AFIX 0 C32 1 0.885576 0.529423 0.274525 -41.00000 0.07822 0.05159 = 0.09020 0.00620 -0.00202 -0.04527 AFIX 137 H32A 2 0.931254 0.489153 0.321831 -41.00000 -1.50000 H32B 2 0.906841 0.612956 0.251223 -41.00000 -1.50000 H32C 2 0.914585 0.472405 0.234612 -41.00000 -1.50000 AFIX 0 C33 1 0.661096 0.608098 0.229002 -41.00000 0.16256 0.03263 = 0.10747 0.02563 -0.08330 -0.04372 AFIX 137 H33A 2 0.686834 0.548770 0.190477 -41.00000 -1.50000 H33B 2 0.680946 0.691315 0.202858 -41.00000 -1.50000 H33C 2 0.565875 0.621742 0.247766 -41.00000 -1.50000 AFIX 0 HKLF 4 REM mo_hzy241_0m_a.res in P-1 REM R1 = 0.0461 for 4630 Fo > 4sig(Fo) and 0.0916 for all 7211 data REM 433 parameters refined using 3 restraints END WGHT 0.0372 1.5812 REM Highest difference peak 0.519, deepest hole -0.301, 1-sigma level 0.070 Q1 1 0.4944 0.3622 0.2759 11.00000 0.05 0.52 Q2 1 0.0964 -0.1411 0.2749 11.00000 0.05 0.30 Q3 1 1.0015 0.3810 0.6573 11.00000 0.05 0.29 Q4 1 0.7221 0.3559 0.2978 11.00000 0.05 0.28 Q5 1 0.6661 0.1033 0.4671 11.00000 0.05 0.26 Q6 1 0.3190 0.5412 -0.1165 11.00000 0.05 0.26 Q7 1 0.8871 -0.0807 0.4778 11.00000 0.05 0.25 Q8 1 0.2480 0.4681 0.1815 11.00000 0.05 0.25 Q9 1 0.2398 0.2969 -0.0248 11.00000 0.05 0.25 Q10 1 0.8128 0.4239 0.5781 11.00000 0.05 0.25 ; _shelx_res_checksum 33126 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn01 Mn 0.40094(6) 0.32460(6) 0.27152(3) 0.03573(17) Uani 1 1 d . . . . . Cl3 Cl 0.59086(11) -0.01859(10) 0.19499(6) 0.0463(3) Uani 1 1 d . . . . . Cl4 Cl 0.77815(11) 0.25791(13) 0.19055(6) 0.0573(3) Uani 1 1 d . . . . . Si1 Si 0.43299(11) 0.14597(10) 0.18448(6) 0.0350(3) Uani 1 1 d . . . . . Si2 Si 0.64471(11) 0.31095(11) 0.28973(6) 0.0378(3) Uani 1 1 d . . . . . N1 N 0.7241(3) 0.2201(3) 0.37830(17) 0.0330(7) Uani 1 1 d . . . . . N2 N 0.7142(3) 0.4190(3) 0.32688(19) 0.0395(8) Uani 1 1 d . . . . . N3 N 0.4097(3) 0.1876(3) 0.07840(18) 0.0354(7) Uani 1 1 d . . . . . N4 N 0.2913(3) 0.0905(3) 0.17284(18) 0.0369(7) Uani 1 1 d . . . . . C1 C 0.7478(4) 0.3276(4) 0.3908(2) 0.0348(9) Uani 1 1 d . . . . . C2 C 0.7931(4) 0.3446(3) 0.4636(2) 0.0345(9) Uani 1 1 d . . . . . C3 C 0.9264(4) 0.3202(4) 0.4693(2) 0.0405(9) Uani 1 1 d . . . . . H3 H 0.9910 0.2922 0.4265 0.049 Uiso 1 1 calc R . . . . C4 C 0.7166(4) 0.0957(4) 0.4345(2) 0.0361(9) Uani 1 1 d . . . . . C5 C 0.2932(4) 0.1540(4) 0.0969(2) 0.0367(9) Uani 1 1 d . . . . . C6 C 0.6039(4) 0.1168(4) 0.5024(2) 0.0405(9) Uani 1 1 d . . . . . H6A H 0.6217 0.1703 0.5358 0.061 Uiso 1 1 calc GR . . . . H6B H 0.5960 0.0329 0.5353 0.061 Uiso 1 1 calc GR . . . . H6C H 0.5209 0.1609 0.4800 0.061 Uiso 1 1 calc GR . . . . C7 C 0.1873(4) 0.1885(4) 0.0440(2) 0.0389(9) Uani 1 1 d . . . . . C8 C 0.5004(4) 0.1880(4) -0.0641(2) 0.0421(10) Uani 1 1 d . . . . . H8A H 0.5512 0.0992 -0.0466 0.063 Uiso 1 1 calc GR . . . . H8B H 0.5524 0.2311 -0.1097 0.063 Uiso 1 1 calc GR . . . . H8C H 0.4173 0.1858 -0.0803 0.063 Uiso 1 1 calc GR . . . . C9 C 0.3798(4) 0.3962(4) -0.0177(2) 0.0465(10) Uani 1 1 d . . . . . H9A H 0.2996 0.3880 -0.0346 0.070 Uiso 1 1 calc GR . . . . H9B H 0.4265 0.4474 -0.0620 0.070 Uiso 1 1 calc GR . . . . H9C H 0.3551 0.4398 0.0289 0.070 Uiso 1 1 calc GR . . . . C10 C 0.4697(4) 0.2623(4) 0.0049(2) 0.0375(9) Uani 1 1 d . . . . . C11 C 0.7370(4) 0.5507(4) 0.2992(2) 0.0443(10) Uani 1 1 d D . . . . C12 C 0.6987(4) 0.3864(4) 0.5262(2) 0.0433(10) Uani 1 1 d . . . . . H12 H 0.6070 0.4052 0.5218 0.052 Uiso 1 1 calc R . . . . C13 C 0.0834(4) 0.2969(4) 0.0508(3) 0.0514(11) Uani 1 1 d . . . . . H13 H 0.0804 0.3497 0.0885 0.062 Uiso 1 1 calc R . . . . C14 C 0.6926(5) 0.0092(4) 0.3829(2) 0.0477(11) Uani 1 1 d . . . . . H14A H 0.6063 0.0475 0.3636 0.071 Uiso 1 1 calc GR . . . . H14B H 0.6935 -0.0771 0.4152 0.071 Uiso 1 1 calc GR . . . . H14C H 0.7626 0.0019 0.3369 0.071 Uiso 1 1 calc GR . . . . C15 C 0.9652(5) 0.3366(4) 0.5380(3) 0.0500(11) Uani 1 1 d . . . . . H15 H 1.0568 0.3207 0.5421 0.060 Uiso 1 1 calc R . . . . C16 C 0.8482(4) 0.0324(4) 0.4671(3) 0.0475(11) Uani 1 1 d . . . . . H16A H 0.9199 0.0211 0.4222 0.071 Uiso 1 1 calc GR . . . . H16B H 0.8446 -0.0524 0.5004 0.071 Uiso 1 1 calc GR . . . . H16C H 0.8647 0.0878 0.4998 0.071 Uiso 1 1 calc GR . . . . C17 C 0.7387(5) 0.4005(4) 0.5947(3) 0.0523(11) Uani 1 1 d . . . . . H17 H 0.6746 0.4270 0.6381 0.063 Uiso 1 1 calc R . . . . C18 C 0.8717(5) 0.3759(4) 0.6000(3) 0.0527(12) Uani 1 1 d . . . . . H18 H 0.8990 0.3863 0.6471 0.063 Uiso 1 1 calc R . . . . C19 C 0.5990(4) 0.2738(4) 0.0260(3) 0.0494(11) Uani 1 1 d . . . . . H19A H 0.5795 0.3209 0.0708 0.074 Uiso 1 1 calc GR . . . . H19B H 0.6450 0.3210 -0.0208 0.074 Uiso 1 1 calc GR . . . . H19C H 0.6555 0.1870 0.0417 0.074 Uiso 1 1 calc GR . . . . C20 C 0.1852(4) 0.0410(4) 0.2306(2) 0.0468(11) Uani 1 1 d . . . . . C21 C 0.1910(4) 0.1132(4) -0.0114(3) 0.0496(11) Uani 1 1 d . . . . . H21 H 0.2619 0.0387 -0.0167 0.060 Uiso 1 1 calc R . . . . C22 C 0.2564(5) -0.0546(5) 0.2965(3) 0.0623(13) Uani 1 1 d . . . . . H22A H 0.3215 -0.1247 0.2734 0.093 Uiso 1 1 calc GR . . . . H22B H 0.1919 -0.0908 0.3371 0.093 Uiso 1 1 calc GR . . . . H22C H 0.3020 -0.0099 0.3217 0.093 Uiso 1 1 calc GR . . . . C23 C 0.1149(5) -0.0275(5) 0.1904(3) 0.0620(13) Uani 1 1 d . . . . . H23A H 0.0658 0.0356 0.1496 0.093 Uiso 1 1 calc GR . . . . H23B H 0.0530 -0.0677 0.2310 0.093 Uiso 1 1 calc GR . . . . H23C H 0.1806 -0.0946 0.1649 0.093 Uiso 1 1 calc GR . . . . C24 C -0.0163(5) 0.3283(5) 0.0024(3) 0.0628(14) Uani 1 1 d . . . . . H24 H -0.0883 0.4020 0.0073 0.075 Uiso 1 1 calc R . . . . C25 C 0.0904(5) 0.1470(5) -0.0594(3) 0.0629(13) Uani 1 1 d . . . . . H25 H 0.0930 0.0951 -0.0974 0.075 Uiso 1 1 calc R . . . . C26 C -0.0106(5) 0.2522(5) -0.0527(3) 0.0642(14) Uani 1 1 d . . . . . H26 H -0.0783 0.2742 -0.0862 0.077 Uiso 1 1 calc R . . . . C27 C 0.0875(4) 0.1537(5) 0.2649(3) 0.0578(12) Uani 1 1 d . . . . . H27A H 0.1340 0.1927 0.2932 0.087 Uiso 1 1 calc GR . . . . H27B H 0.0170 0.1220 0.3025 0.087 Uiso 1 1 calc GR . . . . H27C H 0.0486 0.2190 0.2210 0.087 Uiso 1 1 calc GR . . . . Cl1 Cl 0.2871(15) 0.5253(13) 0.1937(6) 0.047(3) Uani 0.453(4) 1 d . . P A 1 Cl2 Cl 0.2872(6) 0.2591(6) 0.3990(4) 0.057(3) Uani 0.707(4) 1 d . . P A 1 C28 C 0.690(5) 0.603(4) 0.2175(19) 0.081(11) Uani 0.38(6) 1 d D . P B 1 H28A H 0.7506 0.5560 0.1776 0.121 Uiso 0.38(6) 1 calc GR . P B 1 H28B H 0.6891 0.6957 0.2021 0.121 Uiso 0.38(6) 1 calc GR . P B 1 H28C H 0.6006 0.5927 0.2200 0.121 Uiso 0.38(6) 1 calc GR . P B 1 C29 C 0.8798(19) 0.560(4) 0.292(3) 0.079(11) Uani 0.38(6) 1 d D . P B 1 H29A H 0.9079 0.5384 0.3454 0.118 Uiso 0.38(6) 1 calc GR . P B 1 H29B H 0.8855 0.6492 0.2672 0.118 Uiso 0.38(6) 1 calc GR . P B 1 H29C H 0.9377 0.5001 0.2581 0.118 Uiso 0.38(6) 1 calc GR . P B 1 C30 C 0.645(6) 0.643(3) 0.352(2) 0.092(13) Uani 0.38(6) 1 d D . P B 1 H30A H 0.5525 0.6498 0.3469 0.138 Uiso 0.38(6) 1 calc GR . P B 1 H30B H 0.6634 0.7287 0.3352 0.138 Uiso 0.38(6) 1 calc GR . P B 1 H30C H 0.6596 0.6094 0.4083 0.138 Uiso 0.38(6) 1 calc GR . P B 1 Br1 Br 0.2984(6) 0.5287(5) 0.1925(3) 0.0549(11) Uani 0.547(4) 1 d . . P A 2 Br2 Br 0.2853(5) 0.2609(5) 0.4000(3) 0.0384(19) Uani 0.293(4) 1 d . . P A 2 C31 C 0.694(3) 0.6296(18) 0.3664(10) 0.071(5) Uani 0.62(6) 1 d D . P B 2 H31A H 0.6026 0.6289 0.3897 0.107 Uiso 0.62(6) 1 calc GR . P B 2 H31B H 0.7000 0.7191 0.3446 0.107 Uiso 0.62(6) 1 calc GR . P B 2 H31C H 0.7526 0.5916 0.4081 0.107 Uiso 0.62(6) 1 calc GR . P B 2 C32 C 0.8856(12) 0.529(3) 0.2745(17) 0.072(5) Uani 0.62(6) 1 d D . P B 2 H32A H 0.9313 0.4892 0.3218 0.108 Uiso 0.62(6) 1 calc GR . P B 2 H32B H 0.9068 0.6130 0.2512 0.108 Uiso 0.62(6) 1 calc GR . P B 2 H32C H 0.9146 0.4724 0.2346 0.108 Uiso 0.62(6) 1 calc GR . P B 2 C33 C 0.661(4) 0.6081(19) 0.2290(15) 0.094(9) Uani 0.62(6) 1 d D . P B 2 H33A H 0.6868 0.5488 0.1905 0.141 Uiso 0.62(6) 1 calc GR . P B 2 H33B H 0.6809 0.6913 0.2029 0.141 Uiso 0.62(6) 1 calc GR . P B 2 H33C H 0.5659 0.6217 0.2478 0.141 Uiso 0.62(6) 1 calc GR . P B 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 Mn01 0.0362(4) 0.0375(3) 0.0352(3) -0.0085(3) -0.0081(3) -0.0081(3) Cl3 0.0507(6) 0.0414(6) 0.0470(6) -0.0123(5) -0.0170(5) -0.0015(5) Cl4 0.0434(6) 0.0923(9) 0.0384(6) -0.0138(6) -0.0045(5) -0.0193(6) Si1 0.0385(6) 0.0356(6) 0.0333(6) -0.0077(5) -0.0081(5) -0.0095(5) Si2 0.0403(6) 0.0434(6) 0.0332(6) -0.0023(5) -0.0122(5) -0.0151(5) N1 0.0329(18) 0.0370(17) 0.0310(17) -0.0051(14) -0.0075(14) -0.0102(14) N2 0.047(2) 0.0367(18) 0.0397(19) 0.0035(15) -0.0204(16) -0.0170(15) N3 0.0397(19) 0.0386(18) 0.0293(17) -0.0030(14) -0.0081(14) -0.0119(15) N4 0.042(2) 0.0400(18) 0.0311(17) -0.0031(14) -0.0091(15) -0.0134(15) C1 0.027(2) 0.043(2) 0.034(2) -0.0049(17) -0.0063(16) -0.0085(17) C2 0.044(2) 0.0290(19) 0.035(2) -0.0051(16) -0.0112(18) -0.0116(17) C3 0.041(2) 0.043(2) 0.042(2) -0.0103(18) -0.0103(19) -0.0116(19) C4 0.038(2) 0.035(2) 0.037(2) 0.0000(17) -0.0118(18) -0.0121(17) C5 0.038(2) 0.036(2) 0.037(2) -0.0100(17) -0.0064(18) -0.0070(17) C6 0.043(2) 0.045(2) 0.037(2) -0.0034(18) -0.0068(19) -0.0189(19) C7 0.039(2) 0.040(2) 0.038(2) -0.0041(18) -0.0097(18) -0.0091(18) C8 0.044(2) 0.044(2) 0.039(2) -0.0126(19) -0.0065(19) -0.0085(19) C9 0.061(3) 0.039(2) 0.037(2) -0.0077(18) -0.006(2) -0.009(2) C10 0.042(2) 0.037(2) 0.034(2) -0.0036(17) -0.0060(18) -0.0128(18) C11 0.059(3) 0.039(2) 0.040(2) 0.0072(18) -0.020(2) -0.022(2) C12 0.048(3) 0.039(2) 0.043(2) -0.0073(19) -0.007(2) -0.0115(19) C13 0.045(3) 0.057(3) 0.046(3) -0.008(2) -0.007(2) -0.004(2) C14 0.065(3) 0.041(2) 0.043(2) -0.0087(19) -0.011(2) -0.018(2) C15 0.055(3) 0.052(3) 0.054(3) -0.010(2) -0.024(2) -0.019(2) C16 0.045(3) 0.042(2) 0.052(3) 0.006(2) -0.015(2) -0.0102(19) C17 0.068(3) 0.051(3) 0.043(3) -0.017(2) -0.001(2) -0.019(2) C18 0.084(4) 0.047(3) 0.038(2) -0.009(2) -0.019(2) -0.024(2) C19 0.054(3) 0.057(3) 0.044(2) -0.003(2) -0.007(2) -0.027(2) C20 0.047(3) 0.060(3) 0.039(2) -0.002(2) -0.008(2) -0.026(2) C21 0.047(3) 0.054(3) 0.051(3) -0.011(2) -0.017(2) -0.009(2) C22 0.065(3) 0.072(3) 0.050(3) 0.013(2) -0.012(2) -0.032(3) C23 0.069(3) 0.077(3) 0.053(3) -0.011(3) -0.005(2) -0.042(3) C24 0.038(3) 0.070(3) 0.062(3) 0.004(3) -0.009(2) 0.005(2) C25 0.060(3) 0.081(4) 0.058(3) -0.011(3) -0.024(3) -0.024(3) C26 0.040(3) 0.095(4) 0.053(3) 0.004(3) -0.020(2) -0.015(3) C27 0.042(3) 0.082(4) 0.050(3) -0.013(3) -0.001(2) -0.021(2) Cl1 0.053(4) 0.048(6) 0.020(3) 0.001(3) -0.016(3) 0.021(4) Cl2 0.060(4) 0.067(4) 0.039(4) 0.009(2) -0.019(3) -0.014(3) C28 0.11(2) 0.11(2) 0.042(12) 0.045(12) -0.051(12) -0.080(18) C29 0.071(13) 0.043(15) 0.13(3) 0.015(15) -0.052(15) -0.030(9) C30 0.14(3) 0.048(11) 0.045(13) 0.012(9) 0.021(16) 0.013(14) Br1 0.0673(19) 0.0461(18) 0.0437(17) -0.0048(12) -0.0053(11) -0.0057(14) Br2 0.034(3) 0.035(3) 0.044(3) -0.010(2) 0.010(2) -0.0135(19) C31 0.117(13) 0.027(7) 0.071(9) -0.003(6) -0.018(7) -0.020(7) C32 0.078(9) 0.052(10) 0.090(11) 0.006(7) -0.002(8) -0.045(6) C33 0.16(2) 0.033(8) 0.107(16) 0.026(8) -0.083(15) -0.044(9) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' Si Si 0.0817 0.0704 '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 Si2 Mn01 Si1 102.66(4) . . ? Cl1 Mn01 Si1 105.6(3) . . ? Cl1 Mn01 Si2 115.7(4) . . ? Cl2 Mn01 Si1 108.42(16) . . ? Cl2 Mn01 Si2 108.01(15) . . ? Cl2 Mn01 Cl1 115.4(4) . . ? Br1 Mn01 Si1 106.52(13) . . ? Br1 Mn01 Si2 112.66(16) . . ? Br2 Mn01 Si1 108.90(12) . . ? Br2 Mn01 Si2 108.16(14) . . ? Br2 Mn01 Br1 116.92(19) . . ? Cl3 Si1 Mn01 120.55(5) . . ? Cl3 Si1 C5 115.44(11) . . ? N3 Si1 Mn01 121.93(11) . . ? N3 Si1 Cl3 106.03(11) . . ? N4 Si1 Mn01 120.37(11) . . ? N4 Si1 Cl3 105.97(11) . . ? N4 Si1 N3 71.45(14) . . ? C5 Si1 Mn01 123.98(10) . . ? Cl4 Si2 Mn01 111.53(5) . . ? Cl4 Si2 C1 112.51(11) . . ? N1 Si2 Mn01 124.49(11) . . ? N1 Si2 Cl4 105.99(11) . . ? N2 Si2 Mn01 131.27(12) . . ? N2 Si2 Cl4 105.08(12) . . ? N2 Si2 N1 71.39(14) . . ? C1 Si2 Mn01 135.76(11) . . ? C1 N1 Si2 90.9(2) . . ? C1 N1 C4 130.5(3) . . ? C4 N1 Si2 134.3(2) . . ? C1 N2 Si2 91.1(2) . . ? C1 N2 C11 131.7(3) . . ? C11 N2 Si2 137.1(2) . . ? C5 N3 Si1 90.3(2) . . ? C5 N3 C10 132.2(3) . . ? C10 N3 Si1 135.5(2) . . ? C5 N4 Si1 90.7(2) . . ? C5 N4 C20 131.8(3) . . ? C20 N4 Si1 133.7(3) . . ? N1 C1 Si2 53.30(18) . . ? N1 C1 N2 105.9(3) . . ? N1 C1 C2 126.9(3) . . ? N2 C1 Si2 53.08(18) . . ? N2 C1 C2 127.1(3) . . ? C2 C1 Si2 170.8(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 C12 120.1(3) . . ? C12 C2 C1 118.9(3) . . ? C2 C3 H3 120.2 . . ? C2 C3 C15 119.6(4) . . ? C15 C3 H3 120.2 . . ? N1 C4 C6 111.3(3) . . ? N1 C4 C14 105.0(3) . . ? N1 C4 C16 110.2(3) . . ? C6 C4 C14 110.3(3) . . ? C6 C4 C16 110.8(3) . . ? C16 C4 C14 109.0(3) . . ? N3 C5 Si1 53.39(18) . . ? N3 C5 C7 126.3(3) . . ? N4 C5 Si1 53.33(19) . . ? N4 C5 N3 105.3(3) . . ? N4 C5 C7 128.3(4) . . ? C7 C5 Si1 167.2(3) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C13 C7 C5 119.6(4) . . ? C21 C7 C5 120.9(4) . . ? C21 C7 C13 119.5(4) . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C8 H8A 109.5 . . ? C10 C8 H8B 109.5 . . ? C10 C8 H8C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? N3 C10 C8 110.1(3) . . ? N3 C10 C9 111.2(3) . . ? N3 C10 C19 105.3(3) . . ? C8 C10 C19 109.4(3) . . ? C9 C10 C8 110.7(3) . . ? C9 C10 C19 110.1(3) . . ? N2 C11 C28 107.8(15) . . ? N2 C11 C29 116.2(15) . . ? N2 C11 C30 109.9(16) . . ? N2 C11 C31 111.5(8) . . ? N2 C11 C32 105.2(10) . . ? N2 C11 C33 104.8(8) . . ? C28 C11 C29 108(3) . . ? C28 C11 C30 104(3) . . ? C29 C11 C30 110(2) . . ? C32 C11 C31 109.3(12) . . ? C33 C11 C31 113.5(14) . . ? C33 C11 C32 112.3(18) . . ? C2 C12 H12 120.1 . . ? C17 C12 C2 119.8(4) . . ? C17 C12 H12 120.1 . . ? C7 C13 H13 120.2 . . ? C7 C13 C24 119.7(4) . . ? C24 C13 H13 120.2 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C15 H15 120.0 . . ? C18 C15 C3 120.0(4) . . ? C18 C15 H15 120.0 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17 120.1 . . ? C18 C17 C12 119.8(4) . . ? C18 C17 H17 120.1 . . ? C15 C18 C17 120.7(4) . . ? C15 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 C22 105.1(3) . . ? N4 C20 C23 111.2(3) . . ? N4 C20 C27 109.1(3) . . ? C22 C20 C23 110.0(4) . . ? C22 C20 C27 110.2(4) . . ? C27 C20 C23 111.0(4) . . ? C7 C21 H21 120.2 . . ? C7 C21 C25 119.6(4) . . ? C25 C21 H21 120.2 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C13 C24 H24 120.1 . . ? C26 C24 C13 119.9(4) . . ? C26 C24 H24 120.1 . . ? C21 C25 H25 119.5 . . ? C26 C25 C21 120.9(5) . . ? C26 C25 H25 119.5 . . ? C24 C26 H26 119.8 . . ? C25 C26 C24 120.4(4) . . ? C25 C26 H26 119.8 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C11 C28 H28A 109.5 . . ? C11 C28 H28B 109.5 . . ? C11 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C11 C29 H29A 109.5 . . ? C11 C29 H29B 109.5 . . ? C11 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C11 C30 H30A 109.5 . . ? C11 C30 H30B 109.5 . . ? C11 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 C31 H31A 109.5 . . ? C11 C31 H31B 109.5 . . ? C11 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C11 C32 H32A 109.5 . . ? C11 C32 H32B 109.5 . . ? C11 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C11 C33 H33A 109.5 . . ? C11 C33 H33B 109.5 . . ? C11 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 Mn01 Si1 2.6295(12) . ? Mn01 Si2 2.6192(12) . ? Mn01 Cl1 2.424(10) . ? Mn01 Cl2 2.360(6) . ? Mn01 Br1 2.419(4) . ? Mn01 Br2 2.377(5) . ? Cl3 Si1 2.0870(15) . ? Cl4 Si2 2.0821(16) . ? Si1 N3 1.827(3) . ? Si1 N4 1.826(3) . ? Si1 C5 2.277(4) . ? Si2 N1 1.832(3) . ? Si2 N2 1.827(3) . ? Si2 C1 2.285(4) . ? N1 C1 1.337(4) . ? N1 C4 1.494(5) . ? N2 C1 1.338(5) . ? N2 C11 1.483(5) . ? N3 C5 1.347(5) . ? N3 C10 1.482(5) . ? N4 C5 1.336(5) . ? N4 C20 1.491(5) . ? C1 C2 1.488(5) . ? C2 C3 1.380(5) . ? C2 C12 1.391(5) . ? C3 H3 0.9500 . ? C3 C15 1.385(5) . ? C4 C6 1.514(5) . ? C4 C14 1.529(5) . ? C4 C16 1.524(5) . ? C5 C7 1.492(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C13 1.384(5) . ? C7 C21 1.380(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 C10 1.521(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9 C10 1.519(5) . ? C10 C19 1.525(5) . ? C11 C28 1.515(14) . ? C11 C29 1.526(15) . ? C11 C30 1.526(15) . ? C11 C31 1.523(11) . ? C11 C32 1.518(11) . ? C11 C33 1.498(11) . ? C12 H12 0.9500 . ? C12 C17 1.378(6) . ? C13 H13 0.9500 . ? C13 C24 1.390(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 0.9500 . ? C15 C18 1.370(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17 0.9500 . ? C17 C18 1.376(6) . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.517(6) . ? C20 C23 1.526(6) . ? C20 C27 1.524(6) . ? C21 H21 0.9500 . ? C21 C25 1.388(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24 0.9500 . ? C24 C26 1.377(7) . ? C25 H25 0.9500 . ? C25 C26 1.344(7) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ?