#------------------------------------------------------------------------------ #$Date: 2014-12-24 13:19:24 +0200 (Wed, 24 Dec 2014) $ #$Revision: 129041 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116097.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_7116097 loop_ _publ_author_name 'T. Kruczynski' 'P. Henke' 'T. Augenstein' 'N. Arleth' 'F. Breher' 'H. Schnockel' _publ_section_title ; From MgBr via single-electron transfer (SET) to a paramagnetic Mg(II) compound and back to Mg(I): [MgBr(L^1^)^.^]2 and [K(thf)3]2[Mg2(L^1^)2], L^1^ == RN[double bond, length as m-dash]C(Me)C(Me)[double bond, length as m-dash]NR, R == 2,6-diisopropylphenyl ; _journal_name_full Chem.Commun. _journal_page_first 15677 _journal_paper_doi 10.1039/C4cc07680J _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C56 H80 Br2 Mg2 N4' _chemical_formula_sum 'C56 H80 Br2 Mg2 N4' _chemical_formula_weight 1017.68 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2014-09-19 _audit_creation_method ; Olex2 1.2 (compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874) ; _cell_angle_alpha 90 _cell_angle_beta 108.37(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.183(3) _cell_length_b 14.692(3) _cell_length_c 14.201(3) _cell_measurement_reflns_used 9466 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.88 _cell_measurement_theta_min 2.05 _cell_volume 2808.4(11) _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_collection 'STOE X-AREA' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_unetI/netI 0.0931 _diffrn_reflns_laue_measured_fraction_full 0.959 _diffrn_reflns_laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 21086 _diffrn_reflns_point_group_measured_fraction_full 0.959 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.278 _diffrn_reflns_theta_min 2.051 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _exptl_absorpt_coefficient_mu 1.503 _exptl_absorpt_correction_T_max 0.9098 _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1076 _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.135 _exptl_crystal_size_min 0.099 _refine_diff_density_max 0.616 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 478 _refine_ls_number_reflns 6740 _refine_ls_number_restraints 360 _refine_ls_restrained_S_all 0.954 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0622 _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^)+(0.0521P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.1265 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3743 _reflns_number_total 6740 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c4cc07680j2.cif _[local]_cod_data_source_block y _cod_original_cell_volume 2808.3(11) _cod_database_code 7116097 _shelxl_version_number 2013-2 _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. ; _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. Uiso/Uaniso restraints and constraints Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C13) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(N1) \\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C16) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C15) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C17) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C18) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C19) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C20) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C21) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C22) \\sim Ueq, Uanis(C18A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C26) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C27) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C28) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C23) \\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C25) \\sim Ueq, Uanis(C28A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C24) \\sim Ueq, Uanis(C27A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C1) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C2) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C3) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C5) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C6) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C10) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C12) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C11) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C7) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C8) \\sim Ueq, Uanis(C11A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C9) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(N1A) = Uanis(N1) = Uanis(N2) = Uanis(N2A) Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C17) Uanis(C17A) = Uanis(C14A) = Uanis(C13A) Uanis(C9) = Uanis(C8) 3. Others Sof(C1A)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)= Sof(C2A)=Sof(C7A)=Sof(H7A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C8A)= Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11D)= Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13A)= Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)= Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)= Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)= Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)= Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)= Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(N1A)=Sof(N2A)=1-FVAR(1) Sof(C1)=Sof(C6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(C2)= Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)= Sof(H9C)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)= Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)= Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(C18)=Sof(C19)= Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(C23)=Sof(H23)= Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)= Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)= Sof(H28B)=Sof(H28C)=Sof(N1)=Sof(N2)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C7(H7), C7A(H7A), C10(H10), C10A(H10A), C23(H23), C23A(H23A), C26(H26), C26A(H26A) 4.b Aromatic/amide H refined with riding coordinates: C5(H5), C4(H4), C3(H3), C5A(H5A), C4A(H4A), C3A(H3A), C19(H19), C20(H20), C21(H21), C19A(H19A), C20A(H20A), C21A(H21A) 4.c Fitted hexagon refined as free rotating group: C1(C6,C5,C4,C3,C2), C1A(C6A,C5A,C4A,C3A,C2A), C17(C18,C19,C20,C21,C22) 4.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9A(H9AA,H9AB,H9AC), C9(H9A,H9B,H9C), C8A(H8AA,H8AB,H8AC), C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12A(H12D,H12E, H12F), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F), C25(H25A,H25B, H25C), C25A(H25D,H25E,H25F), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F) ; _shelx_res_file ; TITL p21n in P21/n #14 CELL 0.71073 14.1827 14.692 14.201 90 108.37 90 ZERR 2 0.0028 0.0029 0.0028 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br Mg N UNIT 112 160 4 4 8 ISOR N2 N2A ISOR C14 C14A ISOR C13 C13A ISOR N1 N1A ISOR C16 C16A ISOR C15 C15A ISOR C17 C17A ISOR C18 C22A ISOR C19 C21A ISOR C20 C20A ISOR C21 C19A ISOR C22 C18A ISOR C26 C23A ISOR C27 C24A ISOR C28 C25A ISOR C23 C26A ISOR C25 C28A ISOR C24 C27A ISOR C1 C1A ISOR C2 C6A ISOR C3 C5A ISOR C4 C4A ISOR C5 C3A ISOR C6 C2A ISOR C10 C7A ISOR C12 C8A ISOR C11 C9A ISOR C7 C10A ISOR C8 C11A ISOR C9 C12A EADP N1A N1 N2 N2A EADP C18 C19 C20 C21 C22 C17 EADP C17A C14A C13A EADP C9 C8 L.S. 20 PLAN 5 REM reset to P21/n #14 BOND $H MORE -1 CONF fmap 2 acta SHEL 99.9 0.75 REM C:/Users/me/Desktop/publikacjaMg/struktury/gotowe/TKM107corrected/y.h REM kl WGHT 0.052100 FVAR 0.13053 0.49945 BR1 3 0.613704 0.000025 0.613520 11.00000 0.04644 0.03829 = 0.04556 -0.00948 0.00366 0.00923 PART 1 AFIX 66 C1 1 0.502956 0.287609 0.441674 21.00000 0.05054 0.02573 = 0.02863 -0.00541 0.01421 -0.01282 C6 1 0.424871 0.335096 0.375994 21.00000 0.05384 0.05020 = 0.02819 0.00496 0.01095 -0.01487 C5 1 0.438626 0.379015 0.294615 21.00000 0.06674 0.05945 = 0.03903 0.01536 0.00701 -0.01736 AFIX 43 H5 2 0.386382 0.410787 0.250671 21.00000 -1.20000 AFIX 65 C4 1 0.530466 0.375449 0.278916 21.00000 0.07815 0.08502 = 0.04902 0.00644 0.02699 -0.03260 AFIX 43 H4 2 0.539668 0.404835 0.224468 21.00000 -1.20000 AFIX 65 C3 1 0.608551 0.327964 0.344596 21.00000 0.07918 0.07398 = 0.05086 -0.01481 0.04646 -0.03420 AFIX 43 H3 2 0.669998 0.325578 0.334091 21.00000 -1.20000 AFIX 65 C2 1 0.594797 0.284043 0.425975 21.00000 0.06659 0.03025 = 0.04317 -0.01099 0.02815 -0.01625 AFIX 66 PART 0 PART 2 C1A 1 0.557710 0.287909 0.497509 -21.00000 0.04740 0.02514 = 0.04036 0.01268 0.02280 0.00413 C6A 1 0.623565 0.335035 0.575747 -21.00000 0.03570 0.04592 = 0.05239 0.01755 0.01054 -0.00569 C5A 1 0.705228 0.378866 0.562294 -21.00000 0.04509 0.06407 = 0.06472 0.02013 0.01179 -0.01561 AFIX 43 H5A 2 0.749289 0.410396 0.614641 -21.00000 -1.20000 AFIX 65 C4A 1 0.721037 0.375571 0.470603 -21.00000 0.04692 0.08139 = 0.09333 0.02956 0.04085 -0.00589 AFIX 43 H4A 2 0.775675 0.404897 0.461603 -21.00000 -1.20000 AFIX 65 C3A 1 0.655182 0.328446 0.392365 -21.00000 0.07066 0.05523 = 0.06073 0.02209 0.03792 0.00328 AFIX 43 H3A 2 0.665760 0.326242 0.331018 -21.00000 -1.20000 AFIX 65 C2A 1 0.573519 0.284615 0.405817 -21.00000 0.04375 0.03567 = 0.05757 0.02482 0.02917 0.01368 AFIX 0 PART 0 PART 1 C7 1 0.683436 0.234997 0.497881 21.00000 0.04387 0.03372 = 0.07480 -0.01260 0.03858 -0.00897 AFIX 13 H7 2 0.659450 0.204753 0.547484 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C7A 1 0.501225 0.234666 0.318276 -21.00000 0.07603 0.03696 = 0.04667 0.01057 0.03727 0.01434 AFIX 13 H7A 2 0.451271 0.204374 0.341774 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C8 1 0.726590 0.160681 0.446988 21.00000 0.07599 0.05489 = 0.10347 -0.02057 0.04335 -0.01406 AFIX 137 H8A 2 0.675725 0.117153 0.416225 21.00000 -1.50000 H8B 2 0.780402 0.130590 0.495535 21.00000 -1.50000 H8C 2 0.750564 0.187939 0.397452 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C9A 1 0.447559 0.302897 0.236661 -21.00000 0.08601 0.04862 = 0.05588 0.02099 0.01468 0.00873 AFIX 137 H9AA 2 0.419219 0.350762 0.265106 -21.00000 -1.50000 H9AB 2 0.395772 0.272140 0.186478 -21.00000 -1.50000 H9AC 2 0.494231 0.328323 0.207521 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C9 1 0.765960 0.301488 0.553951 21.00000 0.07599 0.05489 = 0.10347 -0.02057 0.04335 -0.01406 AFIX 137 H9A 2 0.790266 0.333449 0.507327 21.00000 -1.50000 H9B 2 0.819383 0.268107 0.599284 21.00000 -1.50000 H9C 2 0.739684 0.344363 0.590201 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C8A 1 0.553093 0.161675 0.273720 -21.00000 0.12091 0.05220 = 0.08461 0.00763 0.06135 0.02382 AFIX 137 H8AA 2 0.593215 0.190880 0.239329 -21.00000 -1.50000 H8AB 2 0.503865 0.124414 0.228114 -21.00000 -1.50000 H8AC 2 0.594442 0.124358 0.326020 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C10 1 0.320738 0.339008 0.386132 21.00000 0.05049 0.04739 = 0.04127 0.01511 0.00080 -0.00540 AFIX 13 H10 2 0.323618 0.308781 0.448495 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C10A 1 0.614255 0.339692 0.679713 -21.00000 0.03804 0.05168 = 0.04829 0.00243 0.00806 -0.01717 AFIX 13 H10A 2 0.551754 0.309765 0.677195 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C11 1 0.283767 0.436581 0.390815 21.00000 0.05036 0.05755 = 0.06456 0.02025 0.00777 0.00272 AFIX 137 H11A 2 0.326655 0.466643 0.448475 21.00000 -1.50000 H11B 2 0.217371 0.434940 0.394547 21.00000 -1.50000 H11C 2 0.284155 0.469182 0.332352 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C11A 1 0.699453 0.286333 0.754958 -21.00000 0.05489 0.06991 = 0.06124 0.01995 -0.00261 -0.01723 AFIX 137 H11D 2 0.701992 0.225607 0.730916 -21.00000 -1.50000 H11E 2 0.687618 0.283895 0.817849 -21.00000 -1.50000 H11F 2 0.761516 0.316450 0.762710 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C12 1 0.244115 0.286993 0.300914 21.00000 0.06921 0.07266 = 0.05796 0.01696 -0.00753 -0.01970 AFIX 137 H12A 2 0.235485 0.318117 0.239324 21.00000 -1.50000 H12B 2 0.181682 0.284286 0.313827 21.00000 -1.50000 H12C 2 0.267701 0.226347 0.296789 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C12A 1 0.610200 0.436394 0.717117 -21.00000 0.05960 0.05473 = 0.06250 -0.00328 0.00813 -0.01356 AFIX 137 H12D 2 0.671280 0.467215 0.722146 -21.00000 -1.50000 H12E 2 0.600973 0.434397 0.781214 -21.00000 -1.50000 H12F 2 0.555793 0.468475 0.671550 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C13 1 0.466914 0.279401 0.597642 21.00000 0.02072 0.02329 = 0.03344 0.00252 0.00841 -0.00249 PART 0 PART 2 C13A 1 0.401582 0.279927 0.533375 -21.00000 0.02377 0.02151 = 0.02236 -0.00122 0.00574 0.00409 PART 0 PART 1 C14 1 0.420403 0.228562 0.656202 21.00000 0.02030 0.02373 = 0.02362 -0.00409 0.00081 0.00214 PART 0 PART 2 C14A 1 0.343999 0.228954 0.579311 -21.00000 0.02377 0.02151 = 0.02236 -0.00122 0.00574 0.00409 PART 0 PART 1 C15 1 0.493853 0.378831 0.619875 21.00000 0.05147 0.02597 = 0.03448 -0.01114 0.00993 -0.00931 AFIX 137 H15A 2 0.542068 0.384097 0.684566 21.00000 -1.50000 H15B 2 0.435360 0.412622 0.618022 21.00000 -1.50000 H15C 2 0.521169 0.402664 0.571101 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C15A 1 0.379605 0.378814 0.507550 -21.00000 0.02652 0.02706 = 0.05344 0.00982 0.00875 0.00814 AFIX 137 H15D 2 0.427302 0.402457 0.478657 -21.00000 -1.50000 H15E 2 0.383454 0.412453 0.566601 -21.00000 -1.50000 H15F 2 0.314056 0.384534 0.460940 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C16 1 0.392272 0.273043 0.739162 21.00000 0.05582 0.03278 = 0.03251 -0.00794 0.01806 -0.00444 AFIX 137 H16A 2 0.344150 0.236030 0.756004 21.00000 -1.50000 H16B 2 0.364421 0.332027 0.718185 21.00000 -1.50000 H16C 2 0.450323 0.279409 0.796152 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C16A 1 0.260473 0.271707 0.607254 -21.00000 0.03616 0.03000 = 0.05168 0.00445 0.01678 0.00936 AFIX 137 H16D 2 0.205129 0.281940 0.548529 -21.00000 -1.50000 H16E 2 0.282190 0.328709 0.639942 -21.00000 -1.50000 H16F 2 0.240664 0.231825 0.651167 -21.00000 -1.50000 AFIX 66 PART 0 PART 1 C17 1 0.331633 0.090488 0.667761 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 C18 1 0.231594 0.095366 0.612517 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 C19 1 0.161757 0.047004 0.642456 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 AFIX 43 H19 2 0.094825 0.050268 0.605493 21.00000 -1.20000 AFIX 65 C20 1 0.191960 -0.006237 0.727639 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 AFIX 43 H20 2 0.145234 -0.038594 0.747670 21.00000 -1.20000 AFIX 65 C21 1 0.291998 -0.011116 0.782884 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 AFIX 43 H21 2 0.312205 -0.046737 0.839878 21.00000 -1.20000 AFIX 65 C22 1 0.361836 0.037246 0.752946 21.00000 0.03231 0.03210 = 0.03501 0.00140 0.01358 -0.00450 AFIX 0 PART 0 PART 2 C17A 1 0.330394 0.092209 0.668329 -21.00000 0.02377 0.02151 = 0.02236 -0.00122 0.00574 0.00409 C18A 1 0.388393 0.093958 0.768885 -21.00000 0.03366 0.03407 = 0.02673 0.00027 0.01070 0.00634 C19A 1 0.355570 0.045423 0.837143 -21.00000 0.03220 0.04504 = 0.02723 0.00450 0.00963 0.00841 AFIX 43 H19A 2 0.392236 0.047283 0.904157 -21.00000 -1.20000 AFIX 0 C20A 1 0.270349 -0.004691 0.806682 -21.00000 0.04373 0.04322 = 0.03956 0.01025 0.02581 0.00191 AFIX 43 H20A 2 0.247437 -0.034146 0.853216 -21.00000 -1.20000 AFIX 0 C21A 1 0.218892 -0.011663 0.708554 -21.00000 0.04144 0.04176 = 0.05071 0.00099 0.02714 -0.01695 AFIX 43 H21A 2 0.164934 -0.051088 0.688482 -21.00000 -1.20000 AFIX 0 C22A 1 0.244827 0.038959 0.636514 -21.00000 0.03106 0.03669 = 0.02762 -0.00010 0.00718 -0.01047 PART 0 PART 1 C23 1 0.196267 0.149816 0.515334 21.00000 0.03140 0.04593 = 0.03702 0.00914 0.00373 -0.00061 AFIX 13 H23 2 0.255077 0.168724 0.498171 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C23A 1 0.484220 0.149198 0.803999 -21.00000 0.03288 0.04779 = 0.02714 -0.00172 0.00397 -0.00286 AFIX 13 H23A 2 0.500581 0.168181 0.744836 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C24 1 0.141471 0.235493 0.529777 21.00000 0.08634 0.05784 = 0.05880 0.01472 0.00820 0.02681 AFIX 137 H24A 2 0.083864 0.218607 0.547471 21.00000 -1.50000 H24B 2 0.121354 0.269857 0.469202 21.00000 -1.50000 H24C 2 0.184740 0.271887 0.581741 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C24A 1 0.470339 0.235822 0.858401 -21.00000 0.08240 0.04729 = 0.08693 -0.02377 0.01501 -0.01613 AFIX 137 H24D 2 0.415784 0.270433 0.816452 -21.00000 -1.50000 H24E 2 0.529870 0.271721 0.874535 -21.00000 -1.50000 H24F 2 0.456674 0.219547 0.918276 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C25 1 0.130105 0.094337 0.429127 21.00000 0.04966 0.07821 = 0.03079 0.00327 0.00224 -0.00788 AFIX 137 H25A 2 0.163031 0.038534 0.423276 21.00000 -1.50000 H25B 2 0.117020 0.128616 0.368809 21.00000 -1.50000 H25C 2 0.068558 0.080891 0.440955 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C25A 1 0.572016 0.093397 0.868590 -21.00000 0.03201 0.08213 = 0.04613 0.00893 0.00583 -0.00243 AFIX 137 H25D 2 0.561810 0.079706 0.930766 -21.00000 -1.50000 H25E 2 0.632200 0.127772 0.880379 -21.00000 -1.50000 H25F 2 0.577088 0.037725 0.835125 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C26 1 0.470050 0.029429 0.814849 21.00000 0.03686 0.05141 = 0.04743 0.02358 0.00285 -0.00522 AFIX 13 H26 2 0.508931 0.065989 0.782663 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C26A 1 0.183226 0.030438 0.528155 -21.00000 0.05017 0.05099 = 0.03242 -0.00115 0.00685 -0.02950 AFIX 13 H26A 2 0.215441 0.067042 0.489347 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C27 1 0.487113 0.068747 0.919557 21.00000 0.05035 0.08756 = 0.04850 0.02789 -0.00192 -0.01817 AFIX 137 H27A 2 0.471090 0.132418 0.914636 21.00000 -1.50000 H27B 2 0.555473 0.060802 0.958514 21.00000 -1.50000 H27C 2 0.445402 0.037505 0.950725 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C27A 1 0.078964 0.070632 0.512350 -21.00000 0.04771 0.08734 = 0.04207 0.01296 -0.00647 -0.02519 AFIX 137 H27D 2 0.048479 0.040367 0.555240 -21.00000 -1.50000 H27E 2 0.038889 0.062076 0.444521 -21.00000 -1.50000 H27F 2 0.084596 0.134484 0.527448 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C28 1 0.507301 -0.067919 0.820613 21.00000 0.04739 0.06861 = 0.12382 0.04783 0.00871 0.01632 AFIX 137 H28A 2 0.470759 -0.105251 0.852454 21.00000 -1.50000 H28B 2 0.576634 -0.069669 0.858189 21.00000 -1.50000 H28C 2 0.498069 -0.090404 0.754840 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C28A 1 0.180507 -0.068264 0.492849 -21.00000 0.11987 0.06411 = 0.04833 -0.02024 0.01611 -0.03299 AFIX 137 H28D 2 0.247134 -0.089713 0.504359 -21.00000 -1.50000 H28E 2 0.144632 -0.071405 0.423222 -21.00000 -1.50000 H28F 2 0.148049 -0.105570 0.528827 -21.00000 -1.50000 AFIX 0 PART 0 MG1 4 0.467000 0.101976 0.532982 11.00000 0.03450 0.02048 = 0.03356 -0.00226 0.01629 0.00136 PART 1 N1 5 0.474637 0.241886 0.512141 21.00000 0.02318 0.01947 = 0.02358 0.00504 0.00628 0.00495 PART 0 PART 2 N1A 5 0.489629 0.233232 0.523573 -21.00000 0.02318 0.01947 = 0.02358 0.00504 0.00628 0.00495 PART 0 PART 1 N2 5 0.401107 0.139281 0.632225 21.00000 0.02318 0.01947 = 0.02358 0.00504 0.00628 0.00495 PART 0 PART 2 N2A 5 0.367126 0.141160 0.598953 -21.00000 0.02318 0.01947 = 0.02358 0.00504 0.00628 0.00495 HKLF 4 REM p21n in P21/n #14 REM R1 = 0.0622 for 3743 Fo > 4sig(Fo) and 0.1320 for all 6740 data REM 478 parameters refined using 360 restraints END WGHT 0.0521 0.0000 REM Highest difference peak 0.616, deepest hole -0.581, 1-sigma level 0.060 Q1 1 0.5453 -0.0045 0.5562 11.00000 0.05 0.62 Q2 1 0.6673 0.0174 0.6644 11.00000 0.05 0.57 Q3 1 0.4466 0.2555 0.5348 11.00000 0.05 0.29 Q4 1 0.6182 0.0815 0.6368 11.00000 0.05 0.27 Q5 1 0.1617 0.0123 0.6761 11.00000 0.05 0.25 ; _shelx_res_checksum 66683 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Br1 Br 0.61370(3) 0.00002(3) 0.61352(3) 0.04596(12) Uani 1 1 d . . . . . C1 C 0.5030(5) 0.2876(3) 0.4417(3) 0.0346(18) Uani 0.499(2) 1 d . U P A 1 C6 C 0.4249(4) 0.3351(4) 0.3760(4) 0.045(2) Uani 0.499(2) 1 d G U P A 1 C5 C 0.4386(5) 0.3790(4) 0.2946(4) 0.057(3) Uani 0.499(2) 1 d G U P A 1 H5 H 0.3864 0.4108 0.2507 0.069 Uiso 0.499(2) 1 calc R . P A 1 C4 C 0.5305(6) 0.3754(5) 0.2789(4) 0.069(3) Uani 0.499(2) 1 d G U P A 1 H4 H 0.5397 0.4048 0.2245 0.083 Uiso 0.499(2) 1 calc R . P A 1 C3 C 0.6086(4) 0.3280(5) 0.3446(5) 0.062(4) Uani 0.499(2) 1 d G U P A 1 H3 H 0.6700 0.3256 0.3341 0.074 Uiso 0.499(2) 1 calc R . P A 1 C2 C 0.5948(4) 0.2840(5) 0.4260(5) 0.044(4) Uani 0.499(2) 1 d G U P A 1 C1A C 0.5577(4) 0.2879(4) 0.4975(4) 0.0355(18) Uani 0.501(2) 1 d . U P A 2 C6A C 0.6236(4) 0.3350(4) 0.5757(3) 0.045(2) Uani 0.501(2) 1 d G U P A 2 C5A C 0.7052(4) 0.3789(4) 0.5623(4) 0.059(3) Uani 0.501(2) 1 d G U P A 2 H5A H 0.7493 0.4104 0.6146 0.071 Uiso 0.501(2) 1 calc R . P A 2 C4A C 0.7210(4) 0.3756(5) 0.4706(5) 0.070(3) Uani 0.501(2) 1 d G U P A 2 H4A H 0.7757 0.4049 0.4616 0.083 Uiso 0.501(2) 1 calc R . P A 2 C3A C 0.6552(6) 0.3284(5) 0.3924(4) 0.058(3) Uani 0.501(2) 1 d G U P A 2 H3A H 0.6658 0.3262 0.3310 0.070 Uiso 0.501(2) 1 calc R . P A 2 C2A C 0.5735(5) 0.2846(5) 0.4058(4) 0.043(4) Uani 0.501(2) 1 d G U P A 2 C7 C 0.6834(7) 0.2350(5) 0.4979(7) 0.046(2) Uani 0.499(2) 1 d . U P A 1 H7 H 0.6595 0.2048 0.5475 0.055 Uiso 0.499(2) 1 calc R . P A 1 C7A C 0.5012(8) 0.2347(5) 0.3183(6) 0.049(2) Uani 0.501(2) 1 d . U P A 2 H7A H 0.4513 0.2044 0.3418 0.059 Uiso 0.501(2) 1 calc R . P A 2 C8 C 0.7266(10) 0.1607(7) 0.4470(9) 0.075(2) Uani 0.499(2) 1 d . U P A 1 H8A H 0.6757 0.1172 0.4162 0.112 Uiso 0.499(2) 1 calc GR . P A 1 H8B H 0.7804 0.1306 0.4955 0.112 Uiso 0.499(2) 1 calc GR . P A 1 H8C H 0.7506 0.1879 0.3975 0.112 Uiso 0.499(2) 1 calc GR . P A 1 C9A C 0.4476(10) 0.3029(6) 0.2367(7) 0.065(3) Uani 0.501(2) 1 d . U P A 2 H9AA H 0.4192 0.3508 0.2651 0.098 Uiso 0.501(2) 1 calc GR . P A 2 H9AB H 0.3958 0.2721 0.1865 0.098 Uiso 0.501(2) 1 calc GR . P A 2 H9AC H 0.4942 0.3283 0.2075 0.098 Uiso 0.501(2) 1 calc GR . P A 2 C9 C 0.7660(10) 0.3015(7) 0.5540(9) 0.075(2) Uani 0.499(2) 1 d . U P A 1 H9A H 0.7903 0.3334 0.5073 0.112 Uiso 0.499(2) 1 calc GR . P A 1 H9B H 0.8194 0.2681 0.5993 0.112 Uiso 0.499(2) 1 calc GR . P A 1 H9C H 0.7397 0.3444 0.5902 0.112 Uiso 0.499(2) 1 calc GR . P A 1 C8A C 0.5531(11) 0.1617(7) 0.2737(9) 0.079(4) Uani 0.501(2) 1 d . U P A 2 H8AA H 0.5932 0.1909 0.2393 0.119 Uiso 0.501(2) 1 calc GR . P A 2 H8AB H 0.5039 0.1244 0.2281 0.119 Uiso 0.501(2) 1 calc GR . P A 2 H8AC H 0.5944 0.1244 0.3260 0.119 Uiso 0.501(2) 1 calc GR . P A 2 C10 C 0.3207(8) 0.3390(6) 0.3861(6) 0.050(2) Uani 0.499(2) 1 d . U P A 1 H10 H 0.3236 0.3088 0.4485 0.059 Uiso 0.499(2) 1 calc R . P A 1 C10A C 0.6143(7) 0.3397(6) 0.6797(6) 0.047(2) Uani 0.501(2) 1 d . U P A 2 H10A H 0.5518 0.3098 0.6772 0.057 Uiso 0.501(2) 1 calc R . P A 2 C11 C 0.2838(9) 0.4366(6) 0.3908(7) 0.060(3) Uani 0.499(2) 1 d . U P A 1 H11A H 0.3267 0.4666 0.4485 0.090 Uiso 0.499(2) 1 calc GR . P A 1 H11B H 0.2174 0.4349 0.3945 0.090 Uiso 0.499(2) 1 calc GR . P A 1 H11C H 0.2842 0.4692 0.3324 0.090 Uiso 0.499(2) 1 calc GR . P A 1 C11A C 0.6995(9) 0.2863(7) 0.7550(8) 0.067(3) Uani 0.501(2) 1 d . U P A 2 H11D H 0.7020 0.2256 0.7309 0.100 Uiso 0.501(2) 1 calc GR . P A 2 H11E H 0.6876 0.2839 0.8178 0.100 Uiso 0.501(2) 1 calc GR . P A 2 H11F H 0.7615 0.3165 0.7627 0.100 Uiso 0.501(2) 1 calc GR . P A 2 C12 C 0.2441(10) 0.2870(7) 0.3009(7) 0.073(4) Uani 0.499(2) 1 d . U P A 1 H12A H 0.2355 0.3181 0.2393 0.110 Uiso 0.499(2) 1 calc GR . P A 1 H12B H 0.1817 0.2843 0.3138 0.110 Uiso 0.499(2) 1 calc GR . P A 1 H12C H 0.2677 0.2263 0.2968 0.110 Uiso 0.499(2) 1 calc GR . P A 1 C12A C 0.6102(9) 0.4364(6) 0.7171(7) 0.062(3) Uani 0.501(2) 1 d . U P A 2 H12D H 0.6713 0.4672 0.7221 0.092 Uiso 0.501(2) 1 calc GR . P A 2 H12E H 0.6010 0.4344 0.7812 0.092 Uiso 0.501(2) 1 calc GR . P A 2 H12F H 0.5558 0.4685 0.6715 0.092 Uiso 0.501(2) 1 calc GR . P A 2 C13 C 0.4669(6) 0.2794(4) 0.5976(5) 0.0258(15) Uani 0.499(2) 1 d . U P A 1 C13A C 0.4016(6) 0.2799(4) 0.5334(5) 0.0229(8) Uani 0.501(2) 1 d . U P A 2 C14 C 0.4204(5) 0.2286(4) 0.6562(4) 0.0240(14) Uani 0.499(2) 1 d . U P A 1 C14A C 0.3440(5) 0.2290(4) 0.5793(4) 0.0229(8) Uani 0.501(2) 1 d . U P A 2 C15 C 0.4939(7) 0.3788(4) 0.6199(5) 0.0382(19) Uani 0.499(2) 1 d . U P A 1 H15A H 0.5421 0.3841 0.6846 0.057 Uiso 0.499(2) 1 calc GR . P A 1 H15B H 0.4354 0.4126 0.6180 0.057 Uiso 0.499(2) 1 calc GR . P A 1 H15C H 0.5212 0.4027 0.5711 0.057 Uiso 0.499(2) 1 calc GR . P A 1 C15A C 0.3796(6) 0.3788(4) 0.5076(6) 0.0366(17) Uani 0.501(2) 1 d . U P A 2 H15D H 0.4273 0.4025 0.4787 0.055 Uiso 0.501(2) 1 calc GR . P A 2 H15E H 0.3835 0.4125 0.5666 0.055 Uiso 0.501(2) 1 calc GR . P A 2 H15F H 0.3141 0.3845 0.4609 0.055 Uiso 0.501(2) 1 calc GR . P A 2 C16 C 0.3923(7) 0.2730(5) 0.7392(5) 0.0394(19) Uani 0.499(2) 1 d . U P A 1 H16A H 0.3441 0.2360 0.7560 0.059 Uiso 0.499(2) 1 calc GR . P A 1 H16B H 0.3644 0.3320 0.7182 0.059 Uiso 0.499(2) 1 calc GR . P A 1 H16C H 0.4503 0.2794 0.7962 0.059 Uiso 0.499(2) 1 calc GR . P A 1 C16A C 0.2605(7) 0.2717(5) 0.6073(6) 0.0386(18) Uani 0.501(2) 1 d . U P A 2 H16D H 0.2051 0.2819 0.5485 0.058 Uiso 0.501(2) 1 calc GR . P A 2 H16E H 0.2822 0.3287 0.6399 0.058 Uiso 0.501(2) 1 calc GR . P A 2 H16F H 0.2407 0.2318 0.6512 0.058 Uiso 0.501(2) 1 calc GR . P A 2 C17 C 0.3316(4) 0.0905(4) 0.6678(4) 0.0324(8) Uani 0.499(2) 1 d . U P A 1 C18 C 0.2316(4) 0.0954(3) 0.6125(3) 0.0324(8) Uani 0.499(2) 1 d G U P A 1 C19 C 0.1618(3) 0.0470(3) 0.6425(3) 0.0324(8) Uani 0.499(2) 1 d G U P A 1 H19 H 0.0948 0.0503 0.6055 0.039 Uiso 0.499(2) 1 calc R . P A 1 C20 C 0.1920(3) -0.0062(4) 0.7276(4) 0.0324(8) Uani 0.499(2) 1 d G U P A 1 H20 H 0.1452 -0.0386 0.7477 0.039 Uiso 0.499(2) 1 calc R . P A 1 C21 C 0.2920(4) -0.0111(4) 0.7829(3) 0.0324(8) Uani 0.499(2) 1 d G U P A 1 H21 H 0.3122 -0.0467 0.8399 0.039 Uiso 0.499(2) 1 calc R . P A 1 C22 C 0.3618(3) 0.0372(4) 0.7529(4) 0.0324(8) Uani 0.499(2) 1 d G U P A 1 C17A C 0.3304(6) 0.0922(5) 0.6683(6) 0.0229(8) Uani 0.501(2) 1 d . U P A 2 C18A C 0.3884(6) 0.0940(5) 0.7689(5) 0.0312(15) Uani 0.501(2) 1 d . U P A 2 C19A C 0.3556(6) 0.0454(5) 0.8371(5) 0.0348(17) Uani 0.501(2) 1 d . U P A 2 H19A H 0.3922 0.0473 0.9042 0.042 Uiso 0.501(2) 1 calc R . P A 2 C20A C 0.2703(6) -0.0047(6) 0.8067(5) 0.0392(17) Uani 0.501(2) 1 d . U P A 2 H20A H 0.2474 -0.0341 0.8532 0.047 Uiso 0.501(2) 1 calc R . P A 2 C21A C 0.2189(7) -0.0117(6) 0.7086(6) 0.042(2) Uani 0.501(2) 1 d . U P A 2 H21A H 0.1649 -0.0511 0.6885 0.050 Uiso 0.501(2) 1 calc R . P A 2 C22A C 0.2448(6) 0.0390(5) 0.6365(5) 0.0323(16) Uani 0.501(2) 1 d . U P A 2 C23 C 0.1963(7) 0.1498(5) 0.5153(5) 0.0398(18) Uani 0.499(2) 1 d . U P A 1 H23 H 0.2551 0.1687 0.4982 0.048 Uiso 0.499(2) 1 calc R . P A 1 C23A C 0.4842(6) 0.1492(5) 0.8040(5) 0.0372(17) Uani 0.501(2) 1 d . U P A 2 H23A H 0.5006 0.1682 0.7448 0.045 Uiso 0.501(2) 1 calc R . P A 2 C24 C 0.1415(10) 0.2355(7) 0.5298(7) 0.071(3) Uani 0.499(2) 1 d . U P A 1 H24A H 0.0839 0.2186 0.5475 0.107 Uiso 0.499(2) 1 calc GR . P A 1 H24B H 0.1214 0.2699 0.4692 0.107 Uiso 0.499(2) 1 calc GR . P A 1 H24C H 0.1847 0.2719 0.5817 0.107 Uiso 0.499(2) 1 calc GR . P A 1 C24A C 0.4703(10) 0.2358(6) 0.8584(9) 0.075(3) Uani 0.501(2) 1 d . U P A 2 H24D H 0.4158 0.2704 0.8165 0.112 Uiso 0.501(2) 1 calc GR . P A 2 H24E H 0.5299 0.2717 0.8745 0.112 Uiso 0.501(2) 1 calc GR . P A 2 H24F H 0.4567 0.2195 0.9183 0.112 Uiso 0.501(2) 1 calc GR . P A 2 C25 C 0.1301(8) 0.0943(7) 0.4291(6) 0.055(2) Uani 0.499(2) 1 d . U P A 1 H25A H 0.1630 0.0385 0.4233 0.083 Uiso 0.499(2) 1 calc GR . P A 1 H25B H 0.1170 0.1286 0.3688 0.083 Uiso 0.499(2) 1 calc GR . P A 1 H25C H 0.0686 0.0809 0.4410 0.083 Uiso 0.499(2) 1 calc GR . P A 1 C25A C 0.5720(7) 0.0934(7) 0.8686(6) 0.055(2) Uani 0.501(2) 1 d . U P A 2 H25D H 0.5618 0.0797 0.9308 0.082 Uiso 0.501(2) 1 calc GR . P A 2 H25E H 0.6322 0.1278 0.8804 0.082 Uiso 0.501(2) 1 calc GR . P A 2 H25F H 0.5771 0.0377 0.8351 0.082 Uiso 0.501(2) 1 calc GR . P A 2 C26 C 0.4700(7) 0.0294(5) 0.8148(6) 0.048(2) Uani 0.499(2) 1 d . U P A 1 H26 H 0.5089 0.0660 0.7827 0.057 Uiso 0.499(2) 1 calc R . P A 1 C26A C 0.1832(7) 0.0304(5) 0.5282(6) 0.046(2) Uani 0.501(2) 1 d . U P A 2 H26A H 0.2154 0.0670 0.4893 0.055 Uiso 0.501(2) 1 calc R . P A 2 C27 C 0.4871(9) 0.0687(7) 0.9196(7) 0.066(3) Uani 0.499(2) 1 d . U P A 1 H27A H 0.4711 0.1324 0.9146 0.099 Uiso 0.499(2) 1 calc GR . P A 1 H27B H 0.5555 0.0608 0.9585 0.099 Uiso 0.499(2) 1 calc GR . P A 1 H27C H 0.4454 0.0375 0.9507 0.099 Uiso 0.499(2) 1 calc GR . P A 1 C27A C 0.0790(8) 0.0706(7) 0.5124(7) 0.064(3) Uani 0.501(2) 1 d . U P A 2 H27D H 0.0485 0.0404 0.5552 0.096 Uiso 0.501(2) 1 calc GR . P A 2 H27E H 0.0389 0.0621 0.4445 0.096 Uiso 0.501(2) 1 calc GR . P A 2 H27F H 0.0846 0.1345 0.5274 0.096 Uiso 0.501(2) 1 calc GR . P A 2 C28 C 0.5073(9) -0.0679(7) 0.8206(10) 0.084(4) Uani 0.499(2) 1 d . U P A 1 H28A H 0.4708 -0.1053 0.8525 0.126 Uiso 0.499(2) 1 calc GR . P A 1 H28B H 0.5766 -0.0697 0.8582 0.126 Uiso 0.499(2) 1 calc GR . P A 1 H28C H 0.4981 -0.0904 0.7548 0.126 Uiso 0.499(2) 1 calc GR . P A 1 C28A C 0.1805(11) -0.0683(7) 0.4928(7) 0.080(4) Uani 0.501(2) 1 d . U P A 2 H28D H 0.2471 -0.0897 0.5044 0.120 Uiso 0.501(2) 1 calc GR . P A 2 H28E H 0.1446 -0.0714 0.4232 0.120 Uiso 0.501(2) 1 calc GR . P A 2 H28F H 0.1480 -0.1056 0.5288 0.120 Uiso 0.501(2) 1 calc GR . P A 2 Mg1 Mg 0.46700(10) 0.10198(6) 0.53298(8) 0.0282(3) Uani 1 1 d . . . . . N1 N 0.4746(13) 0.2419(8) 0.5121(12) 0.0223(11) Uani 0.499(2) 1 d . U P A 1 N1A N 0.4896(13) 0.2332(8) 0.5236(11) 0.0223(11) Uani 0.501(2) 1 d . U P A 2 N2 N 0.4011(5) 0.1393(4) 0.6322(5) 0.0223(11) Uani 0.499(2) 1 d . U P A 1 N2A N 0.3671(5) 0.1412(4) 0.5990(5) 0.0223(11) Uani 0.501(2) 1 d . 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 Br1 0.0464(2) 0.03829(16) 0.04556(19) -0.0095(2) 0.00366(14) 0.0092(2) C1 0.051(6) 0.026(3) 0.029(4) -0.005(3) 0.014(4) -0.013(3) C6 0.054(6) 0.050(4) 0.028(4) 0.005(3) 0.011(4) -0.015(4) C5 0.067(8) 0.059(5) 0.039(4) 0.015(4) 0.007(5) -0.017(5) C4 0.078(9) 0.085(7) 0.049(5) 0.006(5) 0.027(6) -0.033(6) C3 0.079(10) 0.074(7) 0.051(6) -0.015(6) 0.046(6) -0.034(7) C2 0.067(9) 0.030(6) 0.043(5) -0.011(4) 0.028(6) -0.016(5) C1A 0.047(6) 0.025(3) 0.040(4) 0.013(3) 0.023(4) 0.004(3) C6A 0.036(5) 0.046(4) 0.052(5) 0.018(4) 0.011(4) -0.006(4) C5A 0.045(6) 0.064(5) 0.065(6) 0.020(5) 0.012(5) -0.016(4) C4A 0.047(7) 0.081(7) 0.093(8) 0.030(6) 0.041(6) -0.006(5) C3A 0.071(9) 0.055(6) 0.061(7) 0.022(5) 0.038(6) 0.003(5) C2A 0.044(7) 0.036(6) 0.058(6) 0.025(5) 0.029(6) 0.014(5) C7 0.044(6) 0.034(3) 0.075(6) -0.013(4) 0.039(5) -0.009(3) C7A 0.076(8) 0.037(4) 0.047(4) 0.011(3) 0.037(5) 0.014(4) C8 0.076(7) 0.055(4) 0.103(6) -0.021(4) 0.043(5) -0.014(4) C9A 0.086(9) 0.049(5) 0.056(5) 0.021(4) 0.015(6) 0.009(5) C9 0.076(7) 0.055(4) 0.103(6) -0.021(4) 0.043(5) -0.014(4) C8A 0.121(12) 0.052(5) 0.085(8) 0.008(5) 0.061(8) 0.024(6) C10 0.050(6) 0.047(4) 0.041(4) 0.015(3) 0.001(4) -0.005(4) C10A 0.038(6) 0.052(4) 0.048(5) 0.002(4) 0.008(4) -0.017(4) C11 0.050(7) 0.058(5) 0.065(6) 0.020(4) 0.008(5) 0.003(4) C11A 0.055(7) 0.070(6) 0.061(6) 0.020(5) -0.003(5) -0.017(5) C12 0.069(9) 0.073(6) 0.058(6) 0.017(5) -0.008(6) -0.020(6) C12A 0.060(8) 0.055(5) 0.063(6) -0.003(4) 0.008(5) -0.014(5) C13 0.021(4) 0.023(3) 0.033(4) 0.003(2) 0.008(3) -0.002(2) C13A 0.024(2) 0.0215(16) 0.0224(18) -0.0012(13) 0.0057(16) 0.0041(14) C14 0.020(4) 0.024(3) 0.024(3) -0.004(2) 0.001(3) 0.002(2) C14A 0.024(2) 0.0215(16) 0.0224(18) -0.0012(13) 0.0057(16) 0.0041(14) C15 0.051(6) 0.026(3) 0.034(4) -0.011(3) 0.010(3) -0.009(3) C15A 0.027(4) 0.027(3) 0.053(4) 0.010(3) 0.009(3) 0.008(3) C16 0.056(6) 0.033(3) 0.033(4) -0.008(3) 0.018(4) -0.004(3) C16A 0.036(5) 0.030(3) 0.052(4) 0.004(3) 0.017(4) 0.009(3) C17 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C18 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C19 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C20 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C21 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C22 0.032(2) 0.0321(15) 0.0350(16) 0.0014(13) 0.0136(14) -0.0045(13) C17A 0.024(2) 0.0215(16) 0.0224(18) -0.0012(13) 0.0057(16) 0.0041(14) C18A 0.034(5) 0.034(3) 0.027(3) 0.000(3) 0.011(3) 0.006(3) C19A 0.032(5) 0.045(4) 0.027(3) 0.004(3) 0.010(3) 0.008(3) C20A 0.044(5) 0.043(4) 0.040(4) 0.010(4) 0.026(3) 0.002(4) C21A 0.041(5) 0.042(4) 0.051(5) 0.001(4) 0.027(4) -0.017(4) C22A 0.031(5) 0.037(3) 0.028(3) 0.000(3) 0.007(3) -0.010(3) C23 0.031(5) 0.046(4) 0.037(4) 0.009(3) 0.004(3) -0.001(3) C23A 0.033(5) 0.048(4) 0.027(3) -0.002(3) 0.004(3) -0.003(3) C24 0.086(9) 0.058(5) 0.059(6) 0.015(4) 0.008(6) 0.027(5) C24A 0.082(9) 0.047(5) 0.087(7) -0.024(5) 0.015(7) -0.016(5) C25 0.050(6) 0.078(6) 0.031(4) 0.003(4) 0.002(4) -0.008(5) C25A 0.032(6) 0.082(6) 0.046(5) 0.009(4) 0.006(4) -0.002(5) C26 0.037(5) 0.051(4) 0.047(4) 0.024(3) 0.003(4) -0.005(3) C26A 0.050(6) 0.051(4) 0.032(4) -0.001(3) 0.007(4) -0.029(4) C27 0.050(7) 0.088(7) 0.048(5) 0.028(5) -0.002(5) -0.018(5) C27A 0.048(7) 0.087(7) 0.042(5) 0.013(4) -0.006(4) -0.025(5) C28 0.047(8) 0.069(6) 0.124(10) 0.048(7) 0.009(7) 0.016(5) C28A 0.120(12) 0.064(6) 0.048(6) -0.020(4) 0.016(6) -0.033(6) Mg1 0.0345(7) 0.0205(4) 0.0336(6) -0.0023(4) 0.0163(5) 0.0014(4) N1 0.023(4) 0.0195(13) 0.024(3) 0.0050(15) 0.006(2) 0.0049(15) N1A 0.023(4) 0.0195(13) 0.024(3) 0.0050(15) 0.006(2) 0.0049(15) N2 0.023(4) 0.0195(13) 0.024(3) 0.0050(15) 0.006(2) 0.0049(15) N2A 0.023(4) 0.0195(13) 0.024(3) 0.0050(15) 0.006(2) 0.0049(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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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' 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 Mg1 Br1 Mg1 83.35(4) . 3_656 C6 C1 C2 120.0 . . N1 C1 C6 112.5(7) . . N1 C1 C2 127.3(7) . . C1 C6 C5 120.0 . . C1 C6 C10 123.0(5) . . C5 C6 C10 117.0(5) . . C6 C5 H5 120.0 . . C4 C5 C6 120.0 . . C4 C5 H5 120.0 . . C5 C4 H4 120.0 . . C5 C4 C3 120.0 . . C3 C4 H4 120.0 . . C4 C3 H3 120.0 . . C2 C3 C4 120.0 . . C2 C3 H3 120.0 . . C1 C2 C7 121.7(5) . . C3 C2 C1 120.0 . . C3 C2 C7 118.2(5) . . C6A C1A C2A 120.0 . . C6A C1A N1A 115.0(7) . . C2A C1A N1A 124.0(7) . . C1A C6A C5A 120.0 . . C1A C6A C10A 123.7(5) . . C5A C6A C10A 116.3(5) . . C6A C5A H5A 120.0 . . C6A C5A C4A 120.0 . . C4A C5A H5A 120.0 . . C5A C4A H4A 120.0 . . C3A C4A C5A 120.0 . . C3A C4A H4A 120.0 . . C4A C3A H3A 120.0 . . C4A C3A C2A 120.0 . . C2A C3A H3A 120.0 . . C1A C2A C7A 120.9(5) . . C3A C2A C1A 120.0 . . C3A C2A C7A 119.0(5) . . C2 C7 H7 107.2 . . C2 C7 C8 112.7(8) . . C2 C7 C9 112.2(7) . . C8 C7 H7 107.2 . . C8 C7 C9 110.1(9) . . C9 C7 H7 107.2 . . C2A C7A H7A 108.2 . . C2A C7A C9A 110.2(7) . . C2A C7A C8A 112.5(9) . . C9A C7A H7A 108.2 . . C9A C7A C8A 109.3(7) . . C8A C7A H7A 108.2 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C7A C9A H9AA 109.5 . . C7A C9A H9AB 109.5 . . C7A C9A H9AC 109.5 . . H9AA C9A H9AB 109.5 . . H9AA C9A H9AC 109.5 . . H9AB C9A H9AC 109.5 . . C7 C9 H9A 109.5 . . C7 C9 H9B 109.5 . . C7 C9 H9C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C7A C8A H8AA 109.5 . . C7A C8A H8AB 109.5 . . C7A C8A H8AC 109.5 . . H8AA C8A H8AB 109.5 . . H8AA C8A H8AC 109.5 . . H8AB C8A H8AC 109.5 . . C6 C10 H10 107.6 . . C6 C10 C11 113.1(7) . . C6 C10 C12 111.6(8) . . C11 C10 H10 107.6 . . C11 C10 C12 109.2(8) . . C12 C10 H10 107.6 . . C6A C10A H10A 107.3 . . C6A C10A C11A 111.0(8) . . C11A C10A H10A 107.3 . . C12A C10A C6A 113.8(7) . . C12A C10A H10A 107.3 . . C12A C10A C11A 109.8(8) . . C10 C11 H11A 109.5 . . C10 C11 H11B 109.5 . . C10 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . C10A C11A H11D 109.5 . . C10A C11A H11E 109.5 . . C10A C11A H11F 109.5 . . H11D C11A H11E 109.5 . . H11D C11A H11F 109.5 . . H11E C11A H11F 109.5 . . C10 C12 H12A 109.5 . . C10 C12 H12B 109.5 . . C10 C12 H12C 109.5 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C10A C12A H12D 109.5 . . C10A C12A H12E 109.5 . . C10A C12A H12F 109.5 . . H12D C12A H12E 109.5 . . H12D C12A H12F 109.5 . . H12E C12A H12F 109.5 . . C14 C13 C15 121.0(6) . . C14 C13 Mg1 75.4(3) . . C15 C13 Mg1 161.9(6) . . N1 C13 C14 119.2(9) . . N1 C13 C15 119.1(9) . . C14A C13A C15A 121.3(6) . . C14A C13A Mg1 75.1(3) . . C14A C13A N1A 115.4(7) . . C15A C13A Mg1 162.1(5) . . N1A C13A C15A 123.0(8) . . C13 C14 C16 121.0(6) . . C13 C14 Mg1 74.8(4) . . C16 C14 Mg1 163.5(5) . . N2 C14 C13 116.9(6) . . N2 C14 C16 122.1(6) . . C13A C14A C16A 121.4(5) . . C13A C14A Mg1 75.4(4) . . C16A C14A Mg1 162.4(5) . . N2A C14A C13A 117.9(6) . . N2A C14A C16A 120.7(7) . . C13 C15 H15A 109.5 . . C13 C15 H15B 109.5 . . C13 C15 H15C 109.5 . . H15A C15 H15B 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C13A C15A H15D 109.5 . . C13A C15A H15E 109.5 . . C13A C15A H15F 109.5 . . H15D C15A H15E 109.5 . . H15D C15A H15F 109.5 . . H15E C15A H15F 109.5 . . C14 C16 H16A 109.5 . . C14 C16 H16B 109.5 . . C14 C16 H16C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C14A C16A H16D 109.5 . . C14A C16A H16E 109.5 . . C14A C16A H16F 109.5 . . H16D C16A H16E 109.5 . . H16D C16A H16F 109.5 . . H16E C16A H16F 109.5 . . C18 C17 C22 120.0 . . C18 C17 N2 117.9(4) . . C22 C17 N2 122.0(4) . . C17 C18 C19 120.0 . . C17 C18 C23 121.3(5) . . C19 C18 C23 118.6(5) . . C18 C19 H19 120.0 . . C20 C19 C18 120.0 . . C20 C19 H19 120.0 . . C19 C20 H20 120.0 . . C19 C20 C21 120.0 . . C21 C20 H20 120.0 . . C20 C21 H21 120.0 . . C20 C21 C22 120.0 . . C22 C21 H21 120.0 . . C17 C22 C26 121.7(4) . . C21 C22 C17 120.0 . . C21 C22 C26 118.3(4) . . C18A C17A N2A 117.6(7) . . C22A C17A C18A 120.7(7) . . C22A C17A N2A 121.5(6) . . C17A C18A C23A 121.2(6) . . C19A C18A C17A 118.7(7) . . C19A C18A C23A 120.2(6) . . C18A C19A H19A 119.6 . . C20A C19A C18A 120.8(7) . . C20A C19A H19A 119.6 . . C19A C20A H20A 119.9 . . C21A C20A C19A 120.1(7) . . C21A C20A H20A 119.9 . . C20A C21A H21A 119.1 . . C20A C21A C22A 121.9(7) . . C22A C21A H21A 119.1 . . C17A C22A C21A 117.5(7) . . C17A C22A C26A 122.7(6) . . C21A C22A C26A 119.7(7) . . C18 C23 H23 108.0 . . C24 C23 C18 110.1(7) . . C24 C23 H23 108.0 . . C25 C23 C18 112.8(6) . . C25 C23 H23 108.0 . . C25 C23 C24 109.8(8) . . C18A C23A H23A 107.4 . . C18A C23A C24A 111.3(8) . . C18A C23A C25A 112.6(7) . . C24A C23A H23A 107.4 . . C25A C23A H23A 107.4 . . C25A C23A C24A 110.6(7) . . C23 C24 H24A 109.5 . . C23 C24 H24B 109.5 . . C23 C24 H24C 109.5 . . H24A C24 H24B 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . C23A C24A H24D 109.5 . . C23A C24A H24E 109.5 . . C23A C24A H24F 109.5 . . H24D C24A H24E 109.5 . . H24D C24A H24F 109.5 . . H24E C24A H24F 109.5 . . C23 C25 H25A 109.5 . . C23 C25 H25B 109.5 . . C23 C25 H25C 109.5 . . H25A C25 H25B 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . C23A C25A H25D 109.5 . . C23A C25A H25E 109.5 . . C23A C25A H25F 109.5 . . H25D C25A H25E 109.5 . . H25D C25A H25F 109.5 . . H25E C25A H25F 109.5 . . C22 C26 H26 107.7 . . C22 C26 C27 110.7(8) . . C22 C26 C28 112.0(7) . . C27 C26 H26 107.7 . . C28 C26 H26 107.7 . . C28 C26 C27 110.8(8) . . C22A C26A H26A 107.7 . . C22A C26A C27A 109.6(7) . . C22A C26A C28A 110.9(7) . . C27A C26A H26A 107.7 . . C28A C26A H26A 107.7 . . C28A C26A C27A 113.0(8) . . C26 C27 H27A 109.5 . . C26 C27 H27B 109.5 . . C26 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C26A C27A H27D 109.5 . . C26A C27A H27E 109.5 . . C26A C27A H27F 109.5 . . H27D C27A H27E 109.5 . . H27D C27A H27F 109.5 . . H27E C27A H27F 109.5 . . C26 C28 H28A 109.5 . . C26 C28 H28B 109.5 . . C26 C28 H28C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C26A C28A H28D 109.5 . . C26A C28A H28E 109.5 . . C26A C28A H28F 109.5 . . H28D C28A H28E 109.5 . . H28D C28A H28F 109.5 . . H28E C28A H28F 109.5 . . Br1 Mg1 Br1 96.65(4) . 3_656 Br1 Mg1 C13 141.77(15) 3_656 . Br1 Mg1 C13 119.69(16) . . Br1 Mg1 C13A 119.71(14) 3_656 . Br1 Mg1 C13A 141.81(15) . . Br1 Mg1 C14 115.99(13) . . Br1 Mg1 C14 141.39(15) 3_656 . Br1 Mg1 C14A 116.04(14) 3_656 . Br1 Mg1 C14A 141.44(13) . . Br1 Mg1 Mg1 48.32(3) 3_656 3_656 Br1 Mg1 Mg1 48.33(3) . 3_656 C13 Mg1 C14 29.8(2) . . C13 Mg1 Mg1 164.42(17) . 3_656 C13A Mg1 Mg1 164.52(14) . 3_656 C14 Mg1 Mg1 156.51(14) . 3_656 C14A Mg1 C13A 29.5(2) . . C14A Mg1 Mg1 156.67(15) . 3_656 N1 Mg1 Br1 125.2(4) . . N1 Mg1 Br1 119.9(4) . 3_656 N1 Mg1 C13 28.7(5) . . N1 Mg1 C14 57.4(5) . . N1 Mg1 Mg1 144.0(5) . 3_656 N1A Mg1 Br1 118.9(5) . . N1A Mg1 Br1 124.5(4) . 3_656 N1A Mg1 C13A 30.5(5) . . N1A Mg1 C14A 59.0(5) . . N1A Mg1 Mg1 142.2(5) . 3_656 N1A Mg1 N2A 84.5(6) . . N2 Mg1 Br1 123.5(2) . 3_656 N2 Mg1 Br1 110.18(18) . . N2 Mg1 C13 57.1(2) . . N2 Mg1 C14 27.5(2) . . N2 Mg1 Mg1 132.45(19) . 3_656 N2 Mg1 N1 83.5(6) . . N2A Mg1 Br1 110.50(19) . 3_656 N2A Mg1 Br1 123.98(17) . . N2A Mg1 C13A 56.3(2) . . N2A Mg1 C14A 27.0(2) . . N2A Mg1 Mg1 133.13(19) . 3_656 C1 N1 C13 125.2(11) . . C1 N1 Mg1 129.0(10) . . C13 N1 Mg1 104.4(9) . . C1A N1A C13A 115.9(8) . . C1A N1A Mg1 136.5(10) . . C13A N1A Mg1 106.8(11) . . C14 N2 C17 120.0(7) . . C14 N2 Mg1 109.8(5) . . C17 N2 Mg1 129.6(5) . . C14A N2A C17A 120.3(7) . . C14A N2A Mg1 109.9(5) . . C17A N2A Mg1 129.3(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Br1 Mg1 2.5260(14) . Br1 Mg1 2.5266(13) 3_656 C1 C6 1.3900 . C1 C2 1.3900 . C1 N1 1.366(18) . C6 C5 1.3900 . C6 C10 1.529(12) . C5 H5 0.9300 . C5 C4 1.3900 . C4 H4 0.9300 . C4 C3 1.3900 . C3 H3 0.9300 . C3 C2 1.3900 . C2 C7 1.527(11) . C1A C6A 1.3900 . C1A C2A 1.3900 . C1A N1A 1.393(19) . C6A C5A 1.3900 . C6A C10A 1.525(10) . C5A H5A 0.9300 . C5A C4A 1.3900 . C4A H4A 0.9300 . C4A C3A 1.3900 . C3A H3A 0.9300 . C3A C2A 1.3900 . C2A C7A 1.527(11) . C7 H7 0.9800 . C7 C8 1.539(13) . C7 C9 1.540(14) . C7A H7A 0.9800 . C7A C9A 1.540(11) . C7A C8A 1.544(12) . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C9A H9AA 0.9600 . C9A H9AB 0.9600 . C9A H9AC 0.9600 . C9 H9A 0.9600 . C9 H9B 0.9600 . C9 H9C 0.9600 . C8A H8AA 0.9600 . C8A H8AB 0.9600 . C8A H8AC 0.9600 . C10 H10 0.9800 . C10 C11 1.535(13) . C10 C12 1.549(13) . C10A H10A 0.9800 . C10A C11A 1.550(14) . C10A C12A 1.524(12) . C11 H11A 0.9600 . C11 H11B 0.9600 . C11 H11C 0.9600 . C11A H11D 0.9600 . C11A H11E 0.9600 . C11A H11F 0.9600 . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C12A H12D 0.9600 . C12A H12E 0.9600 . C12A H12F 0.9600 . C13 C14 1.425(10) . C13 C15 1.518(8) . C13 Mg1 2.764(6) . C13 N1 1.369(18) . C13A C14A 1.410(10) . C13A C15A 1.507(8) . C13A Mg1 2.775(6) . C13A N1A 1.469(17) . C14 C16 1.507(10) . C14 Mg1 2.772(6) . C14 N2 1.361(8) . C14A C16A 1.501(10) . C14A Mg1 2.771(6) . C14A N2A 1.338(8) . C15 H15A 0.9600 . C15 H15B 0.9600 . C15 H15C 0.9600 . C15A H15D 0.9600 . C15A H15E 0.9600 . C15A H15F 0.9600 . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C16A H16D 0.9600 . C16A H16E 0.9600 . C16A H16F 0.9600 . C17 C18 1.3900 . C17 C22 1.3900 . C17 N2 1.433(9) . C18 C19 1.3900 . C18 C23 1.536(8) . C19 H19 0.9300 . C19 C20 1.3900 . C20 H20 0.9300 . C20 C21 1.3900 . C21 H21 0.9300 . C21 C22 1.3900 . C22 C26 1.514(10) . C17A C18A 1.406(10) . C17A C22A 1.394(11) . C17A N2A 1.443(10) . C18A C19A 1.396(10) . C18A C23A 1.526(11) . C19A H19A 0.9300 . C19A C20A 1.364(12) . C20A H20A 0.9300 . C20A C21A 1.358(11) . C21A H21A 0.9300 . C21A C22A 1.404(10) . C22A C26A 1.516(10) . C23 H23 0.9800 . C23 C24 1.527(12) . C23 C25 1.523(11) . C23A H23A 0.9800 . C23A C24A 1.533(12) . C23A C25A 1.531(12) . C24 H24A 0.9600 . C24 H24B 0.9600 . C24 H24C 0.9600 . C24A H24D 0.9600 . C24A H24E 0.9600 . C24A H24F 0.9600 . C25 H25A 0.9600 . C25 H25B 0.9600 . C25 H25C 0.9600 . C25A H25D 0.9600 . C25A H25E 0.9600 . C25A H25F 0.9600 . C26 H26 0.9800 . C26 C27 1.542(13) . C26 C28 1.518(13) . C26A H26A 0.9800 . C26A C27A 1.542(15) . C26A C28A 1.531(12) . C27 H27A 0.9600 . C27 H27B 0.9600 . C27 H27C 0.9600 . C27A H27D 0.9600 . C27A H27E 0.9600 . C27A H27F 0.9600 . C28 H28A 0.9600 . C28 H28B 0.9600 . C28 H28C 0.9600 . C28A H28D 0.9600 . C28A H28E 0.9600 . C28A H28F 0.9600 . Mg1 Br1 2.5265(13) 3_656 Mg1 Mg1 3.359(2) 3_656 Mg1 N1 2.084(12) . Mg1 N1A 1.966(13) . Mg1 N2 1.998(8) . Mg1 N2A 2.013(8) . 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 C1 C6 C5 C4 0.0 C1 C6 C10 C11 124.5(6) C1 C6 C10 C12 -111.9(7) C1 C2 C7 C8 123.3(7) C1 C2 C7 C9 -111.8(8) C6 C1 C2 C3 0.0 C6 C1 C2 C7 178.2(7) C6 C1 N1 C13 -82.7(14) C6 C1 N1 Mg1 113.3(10) C6 C5 C4 C3 0.0 C5 C6 C10 C11 -57.9(8) C5 C6 C10 C12 65.8(7) C5 C4 C3 C2 0.0 C4 C3 C2 C1 0.0 C4 C3 C2 C7 -178.3(6) C3 C2 C7 C8 -58.5(8) C3 C2 C7 C9 66.4(8) C2 C1 C6 C5 0.0 C2 C1 C6 C10 177.6(6) C2 C1 N1 C13 103.3(12) C2 C1 N1 Mg1 -60.8(15) C1A C6A C5A C4A 0.0 C1A C6A C10A C11A 111.3(7) C1A C6A C10A C12A -124.3(7) C1A C2A C7A C9A 113.2(8) C1A C2A C7A C8A -124.6(7) C6A C1A C2A C3A 0.0 C6A C1A C2A C7A -178.9(7) C6A C1A N1A C13A 81.8(11) C6A C1A N1A Mg1 -109.7(13) C6A C5A C4A C3A 0.0 C5A C6A C10A C11A -66.7(7) C5A C6A C10A C12A 57.7(9) C5A C4A C3A C2A 0.0 C4A C3A C2A C1A 0.0 C4A C3A C2A C7A 179.0(7) C3A C2A C7A C9A -65.7(9) C3A C2A C7A C8A 56.5(8) C2A C1A C6A C5A 0.0 C2A C1A C6A C10A -177.9(7) C2A C1A N1A C13A -109.9(10) C2A C1A N1A Mg1 58.5(15) C10 C6 C5 C4 -177.7(6) C10A C6A C5A C4A 178.0(6) C13 C14 N2 C17 -162.8(6) C13 C14 N2 Mg1 9.6(7) C13A C14A N2A C17A 163.2(6) C13A C14A N2A Mg1 -10.0(7) C14 C13 N1 C1 169.2(10) C14 C13 N1 Mg1 -23.5(11) C14A C13A N1A C1A -167.3(8) C14A C13A N1A Mg1 21.0(11) C15 C13 C14 C16 2.8(10) C15 C13 C14 Mg1 -171.7(7) C15 C13 C14 N2 -178.5(7) C15 C13 N1 C1 -1.7(18) C15 C13 N1 Mg1 165.6(6) C15A C13A C14A C16A -1.9(10) C15A C13A C14A Mg1 172.2(6) C15A C13A C14A N2A 179.2(6) C15A C13A N1A C1A 5.8(16) C15A C13A N1A Mg1 -165.9(6) C16 C14 N2 C17 15.9(10) C16 C14 N2 Mg1 -171.7(6) C16A C14A N2A C17A -15.7(10) C16A C14A N2A Mg1 171.1(5) C17 C18 C19 C20 0.0 C17 C18 C23 C24 -108.9(8) C17 C18 C23 C25 128.1(7) C17 C22 C26 C27 116.4(6) C17 C22 C26 C28 -119.4(8) C18 C17 C22 C21 0.0 C18 C17 C22 C26 179.5(7) C18 C17 N2 C14 86.0(7) C18 C17 N2 Mg1 -84.8(6) C18 C19 C20 C21 0.0 C19 C18 C23 C24 74.0(8) C19 C18 C23 C25 -49.0(9) C19 C20 C21 C22 0.0 C20 C21 C22 C17 0.0 C20 C21 C22 C26 -179.5(6) C21 C22 C26 C27 -64.0(8) C21 C22 C26 C28 60.2(10) C22 C17 C18 C19 0.0 C22 C17 C18 C23 -177.0(6) C22 C17 N2 C14 -96.0(7) C22 C17 N2 Mg1 93.2(6) C17A C18A C19A C20A 1.7(11) C17A C18A C23A C24A 105.4(9) C17A C18A C23A C25A -129.8(8) C17A C22A C26A C27A -116.0(9) C17A C22A C26A C28A 118.4(10) C18A C17A C22A C21A 0.5(12) C18A C17A C22A C26A -176.3(8) C18A C17A N2A C14A -89.0(9) C18A C17A N2A Mg1 82.7(8) C18A C19A C20A C21A 3.3(12) C19A C18A C23A C24A -73.2(9) C19A C18A C23A C25A 51.6(10) C19A C20A C21A C22A -6.7(13) C20A C21A C22A C17A 4.7(13) C20A C21A C22A C26A -178.4(8) C21A C22A C26A C27A 67.2(10) C21A C22A C26A C28A -58.3(12) C22A C17A C18A C19A -3.6(11) C22A C17A C18A C23A 177.7(7) C22A C17A N2A C14A 96.1(9) C22A C17A N2A Mg1 -92.2(9) C23 C18 C19 C20 177.1(6) C23A C18A C19A C20A -179.6(7) Mg1 C13 C14 C16 174.5(6) Mg1 C13 C14 N2 -6.8(5) Mg1 C13 N1 C1 -167.3(19) Mg1 C13A C14A C16A -174.1(6) Mg1 C13A C14A N2A 7.0(5) Mg1 C13A N1A C1A 171.7(16) Mg1 C14 N2 C17 -172.5(8) Mg1 C14A N2A C17A 173.2(8) N1 C1 C6 C5 -174.5(8) N1 C1 C6 C10 3.1(9) N1 C1 C2 C3 173.6(9) N1 C1 C2 C7 -8.2(10) N1 C13 C14 C16 -168.0(9) N1 C13 C14 Mg1 17.5(8) N1 C13 C14 N2 10.7(12) N1A C1A C6A C5A 168.8(7) N1A C1A C6A C10A -9.1(9) N1A C1A C2A C3A -167.7(7) N1A C1A C2A C7A 13.3(9) N1A C13A C14A C16A 171.4(9) N1A C13A C14A Mg1 -14.6(8) N1A C13A C14A N2A -7.5(11) N2 C17 C18 C19 178.1(6) N2 C17 C18 C23 1.1(6) N2 C17 C22 C21 -178.0(7) N2 C17 C22 C26 1.5(7) N2A C17A C18A C19A -178.6(7) N2A C17A C18A C23A 2.8(11) N2A C17A C22A C21A 175.3(7) N2A C17A C22A C26A -1.5(12)