#------------------------------------------------------------------------------ #$Date: 2019-11-08 01:12:03 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224439 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/97/7049721.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_7049721 loop_ _publ_author_name 'Davin, Laia' 'Hern\'an-G\'omez, Alberto' 'McLaughlin, Calum' 'Kennedy, Alan R.' 'McLellan, Ross' 'Hevia, Eva' _publ_section_title ; Alkali metal and stoichiometric effects in intermolecular hydroamination catalysed by lithium, sodium and potassium magnesiates. ; _journal_issue 23 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8122 _journal_page_last 8130 _journal_paper_doi 10.1039/c9dt00923j _journal_volume 48 _journal_year 2019 _chemical_formula_moiety 'C46 H92 Mg2 N6 Na2 O4, 2(C4 H8 O)' _chemical_formula_sum 'C54 H108 Mg2 N6 Na2 O6' _chemical_formula_weight 1032.06 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2019-02-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-03-01 deposited with the CCDC. 2019-04-16 downloaded from the CCDC. ; _cell_angle_alpha 100.805(4) _cell_angle_beta 94.008(3) _cell_angle_gamma 106.319(4) _cell_formula_units_Z 2 _cell_length_a 11.6474(5) _cell_length_b 11.7398(7) _cell_length_c 23.4025(8) _cell_measurement_reflns_used 13875 _cell_measurement_temperature 123.0 _cell_measurement_theta_max 73.1413 _cell_measurement_theta_min 3.8761 _cell_measurement_wavelength 1.5418 _cell_volume 2991.0(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 123.0 _diffrn_detector_area_resol_mean 16.0268 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -106.00 -53.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 -77.0000 120.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega -112.00 -21.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 -50.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 3 omega -41.00 -12.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 -77.0000 120.0000 29 #__ type_ start__ end____ width___ exp.time_ 4 omega -95.00 -11.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 125.0000 120.0000 84 #__ type_ start__ end____ width___ exp.time_ 5 omega -13.00 19.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -77.0000 0.0000 32 #__ type_ start__ end____ width___ exp.time_ 6 omega 39.00 88.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -132.0000 -6.0000 49 #__ type_ start__ end____ width___ exp.time_ 7 omega -16.00 25.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 -90.0000 41 #__ type_ start__ end____ width___ exp.time_ 8 omega 34.00 124.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 65.0000 -141.0000 90 #__ type_ start__ end____ width___ exp.time_ 9 omega 20.00 78.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -77.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 10 omega -12.00 15.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 11 omega 24.00 50.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 80.0000 -111.0000 26 #__ type_ start__ end____ width___ exp.time_ 12 omega 29.00 124.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 71.0000 120.0000 95 #__ type_ start__ end____ width___ exp.time_ 13 omega 78.00 150.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 179.0000 -30.0000 72 #__ type_ start__ end____ width___ exp.time_ 14 omega 63.00 144.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 179.0000 -90.0000 81 #__ type_ start__ end____ width___ exp.time_ 15 omega 41.00 105.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -115.0000 24.0000 64 #__ type_ start__ end____ width___ exp.time_ 16 omega 98.00 145.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 77.0000 30.0000 47 #__ type_ start__ end____ width___ exp.time_ 17 omega 90.00 135.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 30.0000 45 #__ type_ start__ end____ width___ exp.time_ 18 omega 88.00 132.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -30.0000 44 #__ type_ start__ end____ width___ exp.time_ 19 omega 94.00 125.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 30.0000 31 #__ type_ start__ end____ width___ exp.time_ 20 omega 82.00 139.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -120.0000 57 #__ type_ start__ end____ width___ exp.time_ 21 omega 93.00 119.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 22 omega 87.00 113.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 23 omega 57.00 131.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 179.0000 -60.0000 74 #__ type_ start__ end____ width___ exp.time_ 24 omega 89.00 128.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -150.0000 39 #__ type_ start__ end____ width___ exp.time_ 25 omega 51.00 127.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -136.0000 -4.0000 76 #__ type_ start__ end____ width___ exp.time_ 26 omega 81.00 126.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -30.0000 45 #__ type_ start__ end____ width___ exp.time_ 27 omega 90.00 172.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 132.0000 -117.0000 82 #__ type_ start__ end____ width___ exp.time_ 28 omega 64.00 91.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -113.0000 46.0000 27 #__ type_ start__ end____ width___ exp.time_ 29 omega 88.00 144.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -180.0000 56 #__ type_ start__ end____ width___ exp.time_ 30 omega 58.00 139.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 179.0000 0.0000 81 #__ type_ start__ end____ width___ exp.time_ 31 omega 88.00 125.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -90.0000 37 #__ type_ start__ end____ width___ exp.time_ 32 omega 41.00 119.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -120.0000 105.0000 78 #__ type_ start__ end____ width___ exp.time_ 33 omega -113.00 -11.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 -79.0000 -141.0000 102 #__ type_ start__ end____ width___ exp.time_ 34 omega -16.00 28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 60.0000 44 #__ type_ start__ end____ width___ exp.time_ 35 omega -16.00 28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 -150.0000 44 #__ type_ start__ end____ width___ exp.time_ 36 omega -16.00 28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 -60.0000 44 #__ type_ start__ end____ width___ exp.time_ 37 omega 24.00 50.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 80.0000 161.0000 26 #__ type_ start__ end____ width___ exp.time_ 38 omega 25.00 127.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 79.0000 -12.0000 102 #__ type_ start__ end____ width___ exp.time_ 39 omega 28.00 125.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 73.0000 80.0000 97 #__ type_ start__ end____ width___ exp.time_ 40 omega 29.00 125.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 71.0000 -72.0000 96 #__ type_ start__ end____ width___ exp.time_ 41 omega -16.00 28.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 0.0000 44 #__ type_ start__ end____ width___ exp.time_ 42 omega 90.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 50.0000 30.0000 88 #__ type_ start__ end____ width___ exp.time_ 43 omega 90.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 50.0000 -180.0000 88 #__ type_ start__ end____ width___ exp.time_ 44 omega 78.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 25.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 45 omega 78.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 25.0000 120.0000 100 #__ type_ start__ end____ width___ exp.time_ 46 omega 82.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 77.0000 -90.0000 96 #__ type_ start__ end____ width___ exp.time_ 47 omega 78.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 25.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 48 omega 90.00 140.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 50.0000 -150.0000 50 #__ type_ start__ end____ width___ exp.time_ 49 omega 40.00 117.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -115.0000 76.0000 77 #__ type_ start__ end____ width___ exp.time_ 50 omega 82.00 178.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 77.0000 120.0000 96 ; _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0806498000 _diffrn_orient_matrix_UB_12 -0.0367070000 _diffrn_orient_matrix_UB_13 -0.0595263000 _diffrn_orient_matrix_UB_21 -0.1113912000 _diffrn_orient_matrix_UB_22 -0.0014841000 _diffrn_orient_matrix_UB_23 0.0320274000 _diffrn_orient_matrix_UB_31 0.0201662000 _diffrn_orient_matrix_UB_32 0.1351658000 _diffrn_orient_matrix_UB_33 -0.0006670000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0270 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 43397 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.680 _diffrn_reflns_theta_max 73.290 _diffrn_reflns_theta_min 5.824 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.486 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 639 _refine_ls_number_reflns 11830 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0578 _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^)+(0.0996P)^2^+0.9844P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1576 _refine_ls_wR_factor_ref 0.1752 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9231 _reflns_number_total 11830 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00923j2.cif _cod_data_source_block calum1b _cod_depositor_comments 'Adding full bibliography for 7049721--7049722.cif.' _cod_database_code 7049721 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 69.95 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A, H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A, H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A, H55B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B) ; _shelx_res_file ; TITL calum1b in P -1 calum1b.res created by SHELXL-2017/1 at 15:55:16 on 28-Feb-2019 CELL 1.5418 11.6474 11.7398 23.4025 100.805 94.008 106.319 ZERR 2 0.0005 0.0007 0.0008 0.004 0.003 0.004 LATT 1 SFAC Mg Na O N C H UNIT 4 4 12 12 108 216 L.S. 8 PLAN 20 TEMP -150 BOND $H CONF fmap 2 ACTA MERG 2 SHEL 8 0.5 OMIT -3 180 OMIT -2 0 3 OMIT -4 -4 3 REM REM REM WGHT 0.099600 0.984400 FVAR 3.48170 MG1 1 0.225622 0.745172 0.187097 11.00000 0.02895 0.02838 = 0.02652 0.00615 0.00603 0.00645 MG2 1 0.259956 0.753297 0.315192 11.00000 0.02819 0.02815 = 0.02680 0.00609 0.00540 0.00647 NA1 2 0.267217 0.674736 0.431699 11.00000 0.03745 0.04107 = 0.03394 0.01410 0.00776 0.01034 NA4 2 0.230551 0.837906 0.074942 11.00000 0.03737 0.03770 = 0.03304 0.01202 0.00757 0.00835 O1 3 0.231610 0.470432 0.437471 11.00000 0.05320 0.04175 = 0.06371 0.01923 -0.00756 0.00767 O2 3 0.286136 0.701630 0.534896 11.00000 0.04691 0.05102 = 0.03664 0.01240 0.00750 0.00284 O3 3 0.220689 0.811104 -0.027620 11.00000 0.05741 0.04728 = 0.03506 0.01000 0.00899 0.00152 O4 3 0.261252 1.043279 0.073520 11.00000 0.04550 0.04077 = 0.06027 0.02057 0.00785 0.00895 N1 4 0.193289 0.611110 0.239539 11.00000 0.03057 0.02732 = 0.03081 0.00634 0.00559 0.00643 N2 4 0.285243 0.887506 0.263183 11.00000 0.03222 0.02671 = 0.03055 0.00684 0.00490 0.00716 N3 4 0.345143 0.732030 0.126768 11.00000 0.03081 0.03252 = 0.03339 0.00707 0.00934 0.00793 N4 4 0.076429 0.745966 0.133251 11.00000 0.02940 0.03543 = 0.03204 0.00720 0.00452 0.00701 N5 4 0.413509 0.755275 0.366666 11.00000 0.02884 0.03420 = 0.03418 0.00736 0.00379 0.00745 N6 4 0.144938 0.768651 0.377991 11.00000 0.02897 0.03430 = 0.03277 0.00334 0.00758 0.00801 C1 5 0.143875 0.357219 0.412964 11.00000 0.04906 0.04304 = 0.04170 0.00822 0.00645 0.00689 AFIX 23 H1A 6 0.095193 0.362577 0.377714 11.00000 -1.20000 H1B 6 0.089200 0.331847 0.441844 11.00000 -1.20000 AFIX 0 C2 5 0.215292 0.267134 0.396741 11.00000 0.12132 0.05919 = 0.04718 0.00530 0.00924 0.04644 AFIX 23 H2A 6 0.212780 0.243309 0.353682 11.00000 -1.20000 H2B 6 0.183959 0.193245 0.412406 11.00000 -1.20000 AFIX 0 C3 5 0.344001 0.340427 0.426378 11.00000 0.07265 0.11994 = 0.08411 0.05238 0.03390 0.05292 AFIX 23 H3A 6 0.381584 0.290300 0.446523 11.00000 -1.20000 H3B 6 0.395660 0.371179 0.397371 11.00000 -1.20000 AFIX 0 C4 5 0.324999 0.442487 0.469302 11.00000 0.05714 0.06452 = 0.09440 0.03043 -0.00829 0.01477 AFIX 23 H4A 6 0.299132 0.416657 0.505480 11.00000 -1.20000 H4B 6 0.399063 0.512807 0.479751 11.00000 -1.20000 AFIX 0 C5 5 0.185025 0.635459 0.560063 11.00000 0.05184 0.09100 = 0.04832 0.02349 0.01024 -0.00390 AFIX 23 H5A 6 0.150037 0.551858 0.536140 11.00000 -1.20000 H5B 6 0.121577 0.676698 0.561440 11.00000 -1.20000 AFIX 0 C6 5 0.231087 0.632142 0.619971 11.00000 0.07382 0.05779 = 0.04145 0.01377 0.00782 -0.00659 AFIX 23 H6A 6 0.241635 0.551768 0.621094 11.00000 -1.20000 H6B 6 0.174945 0.648750 0.648018 11.00000 -1.20000 AFIX 0 C7 5 0.351316 0.730841 0.634682 11.00000 0.06168 0.07729 = 0.04151 0.01636 0.00233 -0.00021 AFIX 23 H7A 6 0.353250 0.789879 0.671270 11.00000 -1.20000 H7B 6 0.418377 0.695628 0.639462 11.00000 -1.20000 AFIX 0 C8 5 0.360120 0.790329 0.583321 11.00000 0.05741 0.04759 = 0.04462 0.00995 0.00990 0.00005 AFIX 23 H8A 6 0.331123 0.862657 0.591140 11.00000 -1.20000 H8B 6 0.444749 0.816179 0.575162 11.00000 -1.20000 AFIX 0 C9 5 0.262407 0.524411 0.226779 11.00000 0.03853 0.03317 = 0.03715 0.00666 0.00983 0.01143 AFIX 23 H9A 6 0.349548 0.569615 0.233800 11.00000 -1.20000 H9B 6 0.242172 0.483409 0.184773 11.00000 -1.20000 AFIX 0 C10 5 0.064545 0.542875 0.229664 11.00000 0.03479 0.03127 = 0.03381 0.00726 0.00454 0.00571 AFIX 23 H10A 6 0.041666 0.503154 0.187571 11.00000 -1.20000 H10B 6 0.017373 0.600603 0.239110 11.00000 -1.20000 AFIX 0 C11 5 0.030554 0.445651 0.266240 11.00000 0.04099 0.03279 = 0.03649 0.00951 0.01054 0.00405 AFIX 23 H11A 6 0.046018 0.485073 0.308470 11.00000 -1.20000 H11B 6 -0.056512 0.400889 0.256384 11.00000 -1.20000 AFIX 0 C12 5 0.104238 0.356946 0.254024 11.00000 0.05393 0.02892 = 0.03846 0.00961 0.01013 0.00912 AFIX 23 H12A 6 0.087346 0.299062 0.280385 11.00000 -1.20000 H12B 6 0.081472 0.309980 0.212993 11.00000 -1.20000 AFIX 0 C13 5 0.237896 0.427508 0.264090 11.00000 0.04830 0.03540 = 0.04079 0.00898 0.00862 0.01637 AFIX 23 H13A 6 0.285861 0.371081 0.253245 11.00000 -1.20000 H13B 6 0.262513 0.467095 0.306122 11.00000 -1.20000 AFIX 0 C14 5 0.410793 0.961695 0.265417 11.00000 0.03465 0.02914 = 0.03338 0.00662 0.00385 0.00381 AFIX 23 H14A 6 0.460420 0.907371 0.253667 11.00000 -1.20000 H14B 6 0.441949 1.006481 0.306324 11.00000 -1.20000 AFIX 0 C15 5 0.424637 1.053002 0.225433 11.00000 0.04767 0.03173 = 0.03865 0.00971 0.01196 0.00792 AFIX 23 H15A 6 0.510382 1.101884 0.229459 11.00000 -1.20000 H15B 6 0.399712 1.008629 0.184051 11.00000 -1.20000 AFIX 0 C16 5 0.347575 1.137131 0.241437 11.00000 0.06446 0.03280 = 0.03791 0.01155 0.01266 0.01661 AFIX 23 H16A 6 0.379247 1.189698 0.280887 11.00000 -1.20000 H16B 6 0.350840 1.189989 0.212849 11.00000 -1.20000 AFIX 0 C17 5 0.217483 1.061120 0.240941 11.00000 0.05532 0.03774 = 0.03657 0.00813 0.00681 0.02281 AFIX 23 H17A 6 0.182510 1.016507 0.200402 11.00000 -1.20000 H17B 6 0.168731 1.114980 0.254976 11.00000 -1.20000 AFIX 0 C18 5 0.214058 0.970524 0.280812 11.00000 0.04009 0.03201 = 0.03155 0.00367 0.00585 0.01049 AFIX 23 H18A 6 0.245166 1.016317 0.321571 11.00000 -1.20000 H18B 6 0.129221 0.922071 0.280308 11.00000 -1.20000 AFIX 0 C19 5 0.322877 0.605973 0.095597 11.00000 0.03408 0.03388 = 0.04105 0.00722 0.01151 0.00753 AFIX 23 H19A 6 0.236036 0.562075 0.093199 11.00000 -1.20000 H19B 6 0.368699 0.566370 0.118460 11.00000 -1.20000 AFIX 0 C20 5 0.358690 0.594316 0.033443 11.00000 0.04543 0.04028 = 0.03656 0.00276 0.00969 0.01284 AFIX 23 H20A 6 0.342620 0.507460 0.014757 11.00000 -1.20000 H20B 6 0.310178 0.629428 0.009368 11.00000 -1.20000 AFIX 0 C21 5 0.492576 0.661416 0.036613 11.00000 0.04745 0.04526 = 0.04417 0.01174 0.02237 0.01518 AFIX 23 H21A 6 0.541235 0.617096 0.054443 11.00000 -1.20000 H21B 6 0.513371 0.664055 -0.003517 11.00000 -1.20000 AFIX 0 C22 5 0.522728 0.790594 0.073034 11.00000 0.03901 0.04053 = 0.05449 0.01273 0.02100 0.00814 AFIX 23 H22A 6 0.486200 0.839443 0.051473 11.00000 -1.20000 H22B 6 0.611280 0.828625 0.079440 11.00000 -1.20000 AFIX 0 C23 5 0.474937 0.790068 0.132425 11.00000 0.03302 0.03663 = 0.04001 0.00443 0.00678 0.00882 AFIX 23 H23A 6 0.516908 0.746874 0.155044 11.00000 -1.20000 H23B 6 0.494056 0.874937 0.154815 11.00000 -1.20000 AFIX 0 C25 5 0.019765 0.645436 0.084036 11.00000 0.03512 0.04277 = 0.04731 0.00271 0.00121 0.00774 AFIX 23 H25A 6 -0.028522 0.576056 0.099027 11.00000 -1.20000 H25B 6 0.083447 0.619534 0.064200 11.00000 -1.20000 AFIX 0 C26 5 -0.062350 0.676085 0.038919 11.00000 0.03630 0.06672 = 0.03726 0.00178 0.00066 0.00901 AFIX 23 H26A 6 -0.013666 0.740780 0.021170 11.00000 -1.20000 H26B 6 -0.100037 0.603236 0.007218 11.00000 -1.20000 AFIX 0 C27 5 -0.160047 0.718587 0.067999 11.00000 0.03254 0.06476 = 0.04209 0.01778 0.00280 0.01192 AFIX 23 H27A 6 -0.205198 0.748865 0.039886 11.00000 -1.20000 H27B 6 -0.217501 0.649414 0.079437 11.00000 -1.20000 AFIX 0 C28 5 -0.104571 0.819004 0.121885 11.00000 0.03800 0.05640 = 0.05287 0.01464 0.00949 0.01803 AFIX 23 H28A 6 -0.169277 0.837536 0.143694 11.00000 -1.20000 H28B 6 -0.059341 0.893573 0.109724 11.00000 -1.20000 AFIX 0 C29 5 -0.019675 0.780724 0.161630 11.00000 0.03263 0.05381 = 0.03831 0.00676 0.00624 0.01124 AFIX 23 H29A 6 0.017089 0.848840 0.195726 11.00000 -1.20000 H29B 6 -0.067559 0.711267 0.176701 11.00000 -1.20000 AFIX 0 C30 5 0.493801 0.683755 0.350149 11.00000 0.03286 0.05084 = 0.05175 0.00093 0.00441 0.01347 AFIX 23 H30A 6 0.544873 0.720209 0.322227 11.00000 -1.20000 H30B 6 0.444950 0.600643 0.329664 11.00000 -1.20000 AFIX 0 C31 5 0.575579 0.675342 0.402471 11.00000 0.04140 0.05365 = 0.07809 0.01616 -0.00214 0.01862 AFIX 23 H31A 6 0.525482 0.633161 0.429153 11.00000 -1.20000 H31B 6 0.629437 0.627251 0.388303 11.00000 -1.20000 AFIX 0 C32 5 0.650432 0.800430 0.435427 11.00000 0.03270 0.05902 = 0.04743 0.01916 -0.00151 0.00947 AFIX 23 H32A 6 0.709967 0.837611 0.410907 11.00000 -1.20000 H32B 6 0.695101 0.794267 0.471729 11.00000 -1.20000 AFIX 0 C33 5 0.569267 0.880072 0.450980 11.00000 0.03537 0.05977 = 0.03940 0.00350 0.00161 0.00664 AFIX 23 H33A 6 0.619090 0.964686 0.468312 11.00000 -1.20000 H33B 6 0.517873 0.849962 0.480207 11.00000 -1.20000 AFIX 0 C34 5 0.489935 0.876636 0.395189 11.00000 0.03463 0.04048 = 0.04678 0.00618 0.00118 0.00986 AFIX 23 H34A 6 0.438202 0.929533 0.405337 11.00000 -1.20000 H34B 6 0.542524 0.910362 0.367143 11.00000 -1.20000 AFIX 0 C35 5 0.014416 0.725003 0.365335 11.00000 0.03378 0.04024 = 0.04246 0.00153 0.00440 0.01235 AFIX 23 H35A 6 -0.009261 0.644823 0.337756 11.00000 -1.20000 H35B 6 -0.013369 0.781771 0.345518 11.00000 -1.20000 AFIX 0 C36 5 -0.049563 0.712446 0.419583 11.00000 0.03708 0.04103 = 0.06880 0.00806 0.02369 0.00630 AFIX 23 H36A 6 -0.137995 0.684192 0.407934 11.00000 -1.20000 H36B 6 -0.027254 0.651174 0.438147 11.00000 -1.20000 AFIX 0 C37 5 -0.014427 0.833744 0.463246 11.00000 0.04374 0.04671 = 0.04500 0.01138 0.02143 0.01657 AFIX 23 H37A 6 -0.047972 0.891447 0.447025 11.00000 -1.20000 H37B 6 -0.048508 0.822633 0.500117 11.00000 -1.20000 AFIX 0 C38 5 0.121912 0.885144 0.475944 11.00000 0.04315 0.05637 = 0.03754 -0.00183 0.00725 0.01917 AFIX 23 H38A 6 0.154558 0.834278 0.497884 11.00000 -1.20000 H38B 6 0.144462 0.968579 0.500394 11.00000 -1.20000 AFIX 0 C39 5 0.175421 0.887395 0.418057 11.00000 0.03571 0.04253 = 0.04827 -0.00411 0.01556 0.00375 C40 5 0.156709 0.713844 -0.075813 11.00000 0.05854 0.04900 = 0.04321 0.00304 0.00753 0.00373 AFIX 23 H40A 6 0.070700 0.683150 -0.070511 11.00000 -1.20000 H40B 6 0.192217 0.645894 -0.079125 11.00000 -1.20000 AFIX 0 C41 5 0.168992 0.766715 -0.129153 11.00000 0.06961 0.08645 = 0.04311 0.01680 -0.00041 -0.00592 AFIX 23 H41A 6 0.097890 0.793197 -0.138964 11.00000 -1.20000 H41B 6 0.176953 0.706368 -0.163172 11.00000 -1.20000 AFIX 0 C42 5 0.280833 0.873065 -0.113499 11.00000 0.08069 0.07182 = 0.04348 0.01541 0.00554 -0.01081 AFIX 23 H42A 6 0.345610 0.856908 -0.135963 11.00000 -1.20000 H42B 6 0.264570 0.947001 -0.121960 11.00000 -1.20000 AFIX 0 C43 5 0.315276 0.888041 -0.051113 11.00000 0.07478 0.10975 = 0.04569 0.02059 0.00758 -0.03234 AFIX 23 H43A 6 0.390693 0.866463 -0.044560 11.00000 -1.20000 H43B 6 0.329951 0.973897 -0.031051 11.00000 -1.20000 AFIX 0 C44 5 0.355734 1.155885 0.084206 11.00000 0.05541 0.03833 = 0.04422 0.00996 0.01481 0.00756 AFIX 23 H44A 6 0.398205 1.162720 0.049229 11.00000 -1.20000 H44B 6 0.414939 1.161054 0.117800 11.00000 -1.20000 AFIX 0 C45 5 0.297526 1.256796 0.097718 11.00000 0.11183 0.05492 = 0.04468 0.01000 0.01153 0.04026 AFIX 23 H45A 6 0.327262 1.306265 0.137950 11.00000 -1.20000 H45B 6 0.313893 1.310545 0.069412 11.00000 -1.20000 AFIX 0 C46 5 0.164564 1.189348 0.091768 11.00000 0.11075 0.12154 = 0.09749 0.06778 0.05738 0.08511 AFIX 23 H46A 6 0.138699 1.180210 0.130494 11.00000 -1.20000 H46B 6 0.115302 1.231948 0.073023 11.00000 -1.20000 AFIX 0 C47 5 0.154195 1.067509 0.053281 11.00000 0.04713 0.08187 = 0.11698 0.05768 0.00700 0.01669 AFIX 23 H47A 6 0.081271 1.004460 0.058552 11.00000 -1.20000 H47B 6 0.151446 1.071784 0.011379 11.00000 -1.20000 AFIX 0 H39A 6 0.261328 0.922478 0.428065 11.00000 0.05652 H39B 6 0.150572 0.951692 0.400188 11.00000 0.06402 O6 3 0.903076 0.138855 0.321782 11.00000 0.08604 0.05255 = 0.05807 0.01785 -0.01195 0.00172 C52 5 0.897452 0.031119 0.342393 11.00000 0.07570 0.06224 = 0.05529 0.02067 0.00457 0.02428 AFIX 23 H52A 6 0.859655 0.032643 0.379016 11.00000 -1.20000 H52B 6 0.979736 0.024954 0.350750 11.00000 -1.20000 AFIX 0 C53 5 0.823847 -0.075348 0.295687 11.00000 0.06254 0.05205 = 0.06064 0.01807 0.02087 0.01813 AFIX 23 H53A 6 0.769772 -0.137719 0.312831 11.00000 -1.20000 H53B 6 0.876004 -0.112860 0.271837 11.00000 -1.20000 AFIX 0 C54 5 0.752766 -0.017692 0.259653 11.00000 0.05005 0.06084 = 0.06275 0.00851 0.00678 0.01347 AFIX 23 H54A 6 0.730586 -0.064080 0.218506 11.00000 -1.20000 H54B 6 0.678663 -0.011417 0.276590 11.00000 -1.20000 AFIX 0 C55 5 0.839983 0.104612 0.263692 11.00000 0.06682 0.06047 = 0.05200 0.02141 -0.00198 0.00932 AFIX 23 H55A 6 0.896647 0.100932 0.234266 11.00000 -1.20000 H55B 6 0.796999 0.163627 0.256977 11.00000 -1.20000 AFIX 0 O5 3 0.594106 0.363996 0.173191 11.00000 0.10780 0.05459 = 0.07680 0.02029 -0.02554 0.00486 C48 5 0.705809 0.525629 0.247790 11.00000 0.07213 0.06959 = 0.07004 0.01423 -0.00641 0.01698 AFIX 23 H48A 6 0.791927 0.535173 0.243932 11.00000 -1.20000 H48B 6 0.699142 0.566273 0.287955 11.00000 -1.20000 AFIX 0 C49 5 0.633583 0.394511 0.234448 11.00000 0.07088 0.07121 = 0.06691 0.03590 0.00178 0.00474 AFIX 23 H49A 6 0.683803 0.343986 0.244690 11.00000 -1.20000 H49B 6 0.563719 0.381713 0.256852 11.00000 -1.20000 AFIX 0 C50 5 0.614659 0.472937 0.152069 11.00000 0.13599 0.07185 = 0.06197 0.02668 0.00581 0.04195 AFIX 23 H50A 6 0.540285 0.472874 0.128817 11.00000 -1.20000 H50B 6 0.679358 0.479238 0.126488 11.00000 -1.20000 AFIX 0 C51 5 0.650251 0.576272 0.202680 11.00000 0.06108 0.05876 = 0.07066 0.02527 0.02112 0.02056 AFIX 23 H51A 6 0.579433 0.599828 0.215609 11.00000 -1.20000 H51B 6 0.709367 0.647507 0.193703 11.00000 -1.20000 AFIX 0 HKLF 4 REM calum1b in P -1 REM R1 = 0.0578 for 9231 Fo > 4sig(Fo) and 0.0723 for all 11830 data REM 639 parameters refined using 0 restraints END WGHT 0.0999 0.9777 REM Highest difference peak 0.486, deepest hole -0.363, 1-sigma level 0.053 Q1 1 0.2335 0.5853 0.5519 11.00000 0.05 0.49 Q2 1 0.3428 0.4198 0.4280 11.00000 0.05 0.45 Q3 1 0.8186 -0.0013 0.2440 11.00000 0.05 0.42 Q4 1 0.3034 0.2789 0.3963 11.00000 0.05 0.41 Q5 1 0.2517 0.9206 -0.0527 11.00000 0.05 0.39 Q6 1 0.2534 0.4490 0.4104 11.00000 0.05 0.33 Q7 1 0.5972 0.6867 0.3690 11.00000 0.05 0.32 Q8 1 0.3244 0.6680 0.5195 11.00000 0.05 0.31 Q9 1 0.1643 0.3804 0.2568 11.00000 0.05 0.31 Q10 1 0.5464 0.8091 0.4615 11.00000 0.05 0.30 Q11 1 0.1686 0.2171 0.3951 11.00000 0.05 0.30 Q12 1 0.2762 1.0887 0.2391 11.00000 0.05 0.30 Q13 1 0.2202 1.2178 0.0998 11.00000 0.05 0.29 Q14 1 0.4201 0.6368 0.0299 11.00000 0.05 0.29 Q15 1 0.3750 0.9414 -0.0265 11.00000 0.05 0.27 Q16 1 0.2552 0.6828 0.5349 11.00000 0.05 0.27 Q17 1 0.0553 0.8593 0.4692 11.00000 0.05 0.27 Q18 1 0.6341 0.3770 0.1737 11.00000 0.05 0.27 Q19 1 0.4755 0.8605 0.4269 11.00000 0.05 0.27 Q20 1 -0.0763 0.8350 0.0940 11.00000 0.05 0.26 ; _shelx_res_checksum 50877 _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 Mg1 Mg 0.22562(5) 0.74517(5) 0.18710(2) 0.02825(15) Uani 1 1 d . Mg2 Mg 0.25996(5) 0.75330(5) 0.31519(2) 0.02802(15) Uani 1 1 d . Na1 Na 0.26722(6) 0.67474(7) 0.43170(3) 0.03682(18) Uani 1 1 d . Na4 Na 0.23055(6) 0.83791(7) 0.07494(3) 0.03590(18) Uani 1 1 d . O1 O 0.23161(14) 0.47043(14) 0.43747(7) 0.0540(4) Uani 1 1 d . O2 O 0.28614(13) 0.70163(14) 0.53490(6) 0.0468(4) Uani 1 1 d . O3 O 0.22069(14) 0.81110(14) -0.02762(6) 0.0493(4) Uani 1 1 d . O4 O 0.26125(13) 1.04328(13) 0.07352(7) 0.0483(4) Uani 1 1 d . N1 N 0.19329(13) 0.61111(13) 0.23954(6) 0.0300(3) Uani 1 1 d . N2 N 0.28524(13) 0.88751(13) 0.26318(6) 0.0301(3) Uani 1 1 d . N3 N 0.34514(13) 0.73203(14) 0.12677(6) 0.0323(3) Uani 1 1 d . N4 N 0.07643(13) 0.74597(14) 0.13325(6) 0.0328(3) Uani 1 1 d . N5 N 0.41351(13) 0.75527(14) 0.36667(6) 0.0329(3) Uani 1 1 d . N6 N 0.14494(13) 0.76865(14) 0.37799(6) 0.0327(3) Uani 1 1 d . C1 C 0.1439(2) 0.35722(19) 0.41296(9) 0.0462(5) Uani 1 1 d . H1A H 0.095193 0.362577 0.377714 0.055 Uiso 1 1 calc R H1B H 0.089200 0.331847 0.441844 0.055 Uiso 1 1 calc R C2 C 0.2153(3) 0.2671(3) 0.39674(11) 0.0728(8) Uani 1 1 d . H2A H 0.212780 0.243309 0.353682 0.087 Uiso 1 1 calc R H2B H 0.183959 0.193245 0.412406 0.087 Uiso 1 1 calc R C3 C 0.3440(3) 0.3404(3) 0.42638(14) 0.0818(10) Uani 1 1 d . H3A H 0.381584 0.290300 0.446523 0.098 Uiso 1 1 calc R H3B H 0.395660 0.371179 0.397371 0.098 Uiso 1 1 calc R C4 C 0.3250(2) 0.4425(3) 0.46930(14) 0.0719(8) Uani 1 1 d . H4A H 0.299132 0.416657 0.505480 0.086 Uiso 1 1 calc R H4B H 0.399063 0.512807 0.479751 0.086 Uiso 1 1 calc R C5 C 0.1850(2) 0.6355(3) 0.56006(11) 0.0677(8) Uani 1 1 d . H5A H 0.150037 0.551858 0.536140 0.081 Uiso 1 1 calc R H5B H 0.121577 0.676698 0.561440 0.081 Uiso 1 1 calc R C6 C 0.2311(2) 0.6321(2) 0.61997(10) 0.0628(7) Uani 1 1 d . H6A H 0.241635 0.551768 0.621094 0.075 Uiso 1 1 calc R H6B H 0.174945 0.648750 0.648018 0.075 Uiso 1 1 calc R C7 C 0.3513(2) 0.7308(3) 0.63468(10) 0.0643(7) Uani 1 1 d . H7A H 0.353250 0.789879 0.671270 0.077 Uiso 1 1 calc R H7B H 0.418377 0.695628 0.639462 0.077 Uiso 1 1 calc R C8 C 0.3601(2) 0.7903(2) 0.58332(9) 0.0530(6) Uani 1 1 d . H8A H 0.331123 0.862657 0.591140 0.064 Uiso 1 1 calc R H8B H 0.444749 0.816179 0.575162 0.064 Uiso 1 1 calc R C9 C 0.26241(17) 0.52441(17) 0.22678(8) 0.0360(4) Uani 1 1 d . H9A H 0.349548 0.569615 0.233800 0.043 Uiso 1 1 calc R H9B H 0.242172 0.483409 0.184773 0.043 Uiso 1 1 calc R C10 C 0.06454(16) 0.54288(17) 0.22966(8) 0.0341(4) Uani 1 1 d . H10A H 0.041666 0.503154 0.187571 0.041 Uiso 1 1 calc R H10B H 0.017373 0.600603 0.239110 0.041 Uiso 1 1 calc R C11 C 0.03055(18) 0.44565(17) 0.26624(8) 0.0377(4) Uani 1 1 d . H11A H 0.046018 0.485073 0.308470 0.045 Uiso 1 1 calc R H11B H -0.056512 0.400889 0.256384 0.045 Uiso 1 1 calc R C12 C 0.10424(19) 0.35695(17) 0.25402(9) 0.0406(4) Uani 1 1 d . H12A H 0.087346 0.299062 0.280385 0.049 Uiso 1 1 calc R H12B H 0.081472 0.309980 0.212993 0.049 Uiso 1 1 calc R C13 C 0.23790(19) 0.42751(18) 0.26409(9) 0.0405(4) Uani 1 1 d . H13A H 0.285861 0.371081 0.253245 0.049 Uiso 1 1 calc R H13B H 0.262513 0.467095 0.306122 0.049 Uiso 1 1 calc R C14 C 0.41079(16) 0.96170(16) 0.26542(8) 0.0337(4) Uani 1 1 d . H14A H 0.460420 0.907371 0.253667 0.040 Uiso 1 1 calc R H14B H 0.441949 1.006481 0.306324 0.040 Uiso 1 1 calc R C15 C 0.42464(19) 1.05300(17) 0.22543(8) 0.0396(4) Uani 1 1 d . H15A H 0.510382 1.101884 0.229459 0.047 Uiso 1 1 calc R H15B H 0.399712 1.008629 0.184051 0.047 Uiso 1 1 calc R C16 C 0.3476(2) 1.13713(18) 0.24144(9) 0.0438(5) Uani 1 1 d . H16A H 0.379247 1.189698 0.280887 0.053 Uiso 1 1 calc R H16B H 0.350840 1.189989 0.212849 0.053 Uiso 1 1 calc R C17 C 0.21748(19) 1.06112(18) 0.24094(8) 0.0413(4) Uani 1 1 d . H17A H 0.182510 1.016507 0.200402 0.050 Uiso 1 1 calc R H17B H 0.168731 1.114980 0.254976 0.050 Uiso 1 1 calc R C18 C 0.21406(17) 0.97052(17) 0.28081(8) 0.0350(4) Uani 1 1 d . H18A H 0.245166 1.016317 0.321571 0.042 Uiso 1 1 calc R H18B H 0.129221 0.922071 0.280308 0.042 Uiso 1 1 calc R C19 C 0.32288(17) 0.60597(17) 0.09560(8) 0.0367(4) Uani 1 1 d . H19A H 0.236036 0.562075 0.093199 0.044 Uiso 1 1 calc R H19B H 0.368699 0.566370 0.118460 0.044 Uiso 1 1 calc R C20 C 0.35869(18) 0.59432(19) 0.03344(8) 0.0413(4) Uani 1 1 d . H20A H 0.342620 0.507460 0.014757 0.050 Uiso 1 1 calc R H20B H 0.310178 0.629428 0.009368 0.050 Uiso 1 1 calc R C21 C 0.49258(19) 0.66142(19) 0.03661(9) 0.0443(5) Uani 1 1 d . H21A H 0.541235 0.617096 0.054443 0.053 Uiso 1 1 calc R H21B H 0.513371 0.664055 -0.003517 0.053 Uiso 1 1 calc R C22 C 0.52273(18) 0.79059(19) 0.07303(9) 0.0444(5) Uani 1 1 d . H22A H 0.486200 0.839443 0.051473 0.053 Uiso 1 1 calc R H22B H 0.611280 0.828625 0.079440 0.053 Uiso 1 1 calc R C23 C 0.47494(16) 0.79007(18) 0.13243(8) 0.0373(4) Uani 1 1 d . H23A H 0.516908 0.746874 0.155044 0.045 Uiso 1 1 calc R H23B H 0.494056 0.874937 0.154815 0.045 Uiso 1 1 calc R C25 C 0.01976(18) 0.64544(19) 0.08404(9) 0.0437(5) Uani 1 1 d . H25A H -0.028522 0.576056 0.099027 0.052 Uiso 1 1 calc R H25B H 0.083447 0.619534 0.064200 0.052 Uiso 1 1 calc R C26 C -0.06235(18) 0.6761(2) 0.03892(9) 0.0496(5) Uani 1 1 d . H26A H -0.013666 0.740780 0.021170 0.060 Uiso 1 1 calc R H26B H -0.100037 0.603236 0.007218 0.060 Uiso 1 1 calc R C27 C -0.16005(18) 0.7186(2) 0.06800(9) 0.0463(5) Uani 1 1 d . H27A H -0.205198 0.748865 0.039886 0.056 Uiso 1 1 calc R H27B H -0.217501 0.649414 0.079437 0.056 Uiso 1 1 calc R C28 C -0.10457(19) 0.8190(2) 0.12188(9) 0.0477(5) Uani 1 1 d . H28A H -0.169277 0.837536 0.143694 0.057 Uiso 1 1 calc R H28B H -0.059341 0.893573 0.109724 0.057 Uiso 1 1 calc R C29 C -0.01967(17) 0.7807(2) 0.16163(9) 0.0423(5) Uani 1 1 d . H29A H 0.017089 0.848840 0.195726 0.051 Uiso 1 1 calc R H29B H -0.067559 0.711267 0.176701 0.051 Uiso 1 1 calc R C30 C 0.49380(18) 0.6838(2) 0.35015(9) 0.0464(5) Uani 1 1 d . H30A H 0.544873 0.720209 0.322227 0.056 Uiso 1 1 calc R H30B H 0.444950 0.600643 0.329664 0.056 Uiso 1 1 calc R C31 C 0.5756(2) 0.6753(2) 0.40247(12) 0.0570(6) Uani 1 1 d . H31A H 0.525482 0.633161 0.429153 0.068 Uiso 1 1 calc R H31B H 0.629437 0.627251 0.388303 0.068 Uiso 1 1 calc R C32 C 0.65043(18) 0.8004(2) 0.43543(9) 0.0466(5) Uani 1 1 d . H32A H 0.709967 0.837611 0.410907 0.056 Uiso 1 1 calc R H32B H 0.695101 0.794267 0.471729 0.056 Uiso 1 1 calc R C33 C 0.56927(18) 0.8801(2) 0.45098(9) 0.0476(5) Uani 1 1 d . H33A H 0.619090 0.964686 0.468312 0.057 Uiso 1 1 calc R H33B H 0.517873 0.849962 0.480207 0.057 Uiso 1 1 calc R C34 C 0.48993(17) 0.87664(18) 0.39519(9) 0.0416(4) Uani 1 1 d . H34A H 0.438202 0.929533 0.405337 0.050 Uiso 1 1 calc R H34B H 0.542524 0.910362 0.367143 0.050 Uiso 1 1 calc R C35 C 0.01442(17) 0.72500(19) 0.36534(9) 0.0396(4) Uani 1 1 d . H35A H -0.009261 0.644823 0.337756 0.048 Uiso 1 1 calc R H35B H -0.013369 0.781771 0.345518 0.048 Uiso 1 1 calc R C36 C -0.04956(19) 0.7124(2) 0.41958(10) 0.0498(5) Uani 1 1 d . H36A H -0.137995 0.684192 0.407934 0.060 Uiso 1 1 calc R H36B H -0.027254 0.651174 0.438147 0.060 Uiso 1 1 calc R C37 C -0.01443(18) 0.8337(2) 0.46325(9) 0.0435(5) Uani 1 1 d . H37A H -0.047972 0.891447 0.447025 0.052 Uiso 1 1 calc R H37B H -0.048508 0.822633 0.500117 0.052 Uiso 1 1 calc R C38 C 0.12191(18) 0.8851(2) 0.47594(9) 0.0463(5) Uani 1 1 d . H38A H 0.154558 0.834278 0.497884 0.056 Uiso 1 1 calc R H38B H 0.144462 0.968579 0.500394 0.056 Uiso 1 1 calc R C39 C 0.17542(19) 0.8874(2) 0.41806(10) 0.0452(5) Uani 1 1 d . C40 C 0.1567(2) 0.7138(2) -0.07581(9) 0.0538(6) Uani 1 1 d . H40A H 0.070700 0.683150 -0.070511 0.065 Uiso 1 1 calc R H40B H 0.192217 0.645894 -0.079125 0.065 Uiso 1 1 calc R C41 C 0.1690(3) 0.7667(3) -0.12915(11) 0.0726(8) Uani 1 1 d . H41A H 0.097890 0.793197 -0.138964 0.087 Uiso 1 1 calc R H41B H 0.176953 0.706368 -0.163172 0.087 Uiso 1 1 calc R C42 C 0.2808(3) 0.8731(3) -0.11350(11) 0.0721(8) Uani 1 1 d . H42A H 0.345610 0.856908 -0.135963 0.087 Uiso 1 1 calc R H42B H 0.264570 0.947001 -0.121960 0.087 Uiso 1 1 calc R C43 C 0.3153(3) 0.8880(3) -0.05111(11) 0.0888(11) Uani 1 1 d . H43A H 0.390693 0.866463 -0.044560 0.107 Uiso 1 1 calc R H43B H 0.329951 0.973897 -0.031051 0.107 Uiso 1 1 calc R C44 C 0.3557(2) 1.15589(19) 0.08421(9) 0.0468(5) Uani 1 1 d . H44A H 0.398205 1.162720 0.049229 0.056 Uiso 1 1 calc R H44B H 0.414939 1.161054 0.117800 0.056 Uiso 1 1 calc R C45 C 0.2975(3) 1.2568(2) 0.09772(11) 0.0673(8) Uani 1 1 d . H45A H 0.327262 1.306265 0.137950 0.081 Uiso 1 1 calc R H45B H 0.313893 1.310545 0.069412 0.081 Uiso 1 1 calc R C46 C 0.1646(3) 1.1893(3) 0.09177(15) 0.0911(12) Uani 1 1 d . H46A H 0.138699 1.180210 0.130494 0.109 Uiso 1 1 calc R H46B H 0.115302 1.231948 0.073023 0.109 Uiso 1 1 calc R C47 C 0.1542(2) 1.0675(3) 0.05328(16) 0.0778(9) Uani 1 1 d . H47A H 0.081271 1.004460 0.058552 0.093 Uiso 1 1 calc R H47B H 0.151446 1.071784 0.011379 0.093 Uiso 1 1 calc R H39A H 0.261(2) 0.922(2) 0.4281(10) 0.057(7) Uiso 1 1 d . H39B H 0.151(2) 0.952(2) 0.4002(11) 0.064(8) Uiso 1 1 d . O6 O 0.90308(18) 0.13886(16) 0.32178(8) 0.0698(5) Uani 1 1 d . C52 C 0.8975(3) 0.0311(2) 0.34239(11) 0.0628(7) Uani 1 1 d . H52A H 0.859655 0.032643 0.379016 0.075 Uiso 1 1 calc R H52B H 0.979736 0.024954 0.350750 0.075 Uiso 1 1 calc R C53 C 0.8238(2) -0.0753(2) 0.29569(11) 0.0568(6) Uani 1 1 d . H53A H 0.769772 -0.137719 0.312831 0.068 Uiso 1 1 calc R H53B H 0.876004 -0.112860 0.271837 0.068 Uiso 1 1 calc R C54 C 0.7528(2) -0.0177(2) 0.25965(12) 0.0592(6) Uani 1 1 d . H54A H 0.730586 -0.064080 0.218506 0.071 Uiso 1 1 calc R H54B H 0.678663 -0.011417 0.276590 0.071 Uiso 1 1 calc R C55 C 0.8400(2) 0.1046(2) 0.26369(11) 0.0610(6) Uani 1 1 d . H55A H 0.896647 0.100932 0.234266 0.073 Uiso 1 1 calc R H55B H 0.796999 0.163627 0.256977 0.073 Uiso 1 1 calc R O5 O 0.5941(2) 0.36400(18) 0.17319(9) 0.0849(7) Uani 1 1 d . C48 C 0.7058(3) 0.5256(3) 0.24779(13) 0.0724(8) Uani 1 1 d . H48A H 0.791927 0.535173 0.243932 0.087 Uiso 1 1 calc R H48B H 0.699142 0.566273 0.287955 0.087 Uiso 1 1 calc R C49 C 0.6336(3) 0.3945(3) 0.23445(12) 0.0706(8) Uani 1 1 d . H49A H 0.683803 0.343986 0.244690 0.085 Uiso 1 1 calc R H49B H 0.563719 0.381713 0.256852 0.085 Uiso 1 1 calc R C50 C 0.6147(4) 0.4729(3) 0.15207(13) 0.0864(10) Uani 1 1 d . H50A H 0.540285 0.472874 0.128817 0.104 Uiso 1 1 calc R H50B H 0.679358 0.479238 0.126488 0.104 Uiso 1 1 calc R C51 C 0.6503(2) 0.5763(2) 0.20268(12) 0.0608(6) Uani 1 1 d . H51A H 0.579433 0.599828 0.215609 0.073 Uiso 1 1 calc R H51B H 0.709367 0.647507 0.193703 0.073 Uiso 1 1 calc R 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 Mg1 0.0289(3) 0.0284(3) 0.0265(3) 0.0061(2) 0.0060(2) 0.0065(2) Mg2 0.0282(3) 0.0281(3) 0.0268(3) 0.0061(2) 0.0054(2) 0.0065(2) Na1 0.0375(4) 0.0411(4) 0.0339(4) 0.0141(3) 0.0078(3) 0.0103(3) Na4 0.0374(4) 0.0377(4) 0.0330(4) 0.0120(3) 0.0076(3) 0.0083(3) O1 0.0532(9) 0.0417(8) 0.0637(10) 0.0192(7) -0.0076(7) 0.0077(7) O2 0.0469(8) 0.0510(9) 0.0366(7) 0.0124(6) 0.0075(6) 0.0028(7) O3 0.0574(9) 0.0473(9) 0.0351(7) 0.0100(6) 0.0090(6) 0.0015(7) O4 0.0455(8) 0.0408(8) 0.0603(9) 0.0206(7) 0.0078(7) 0.0090(7) N1 0.0306(7) 0.0273(7) 0.0308(7) 0.0063(6) 0.0056(6) 0.0064(6) N2 0.0322(7) 0.0267(7) 0.0306(7) 0.0068(6) 0.0049(6) 0.0072(6) N3 0.0308(7) 0.0325(8) 0.0334(7) 0.0071(6) 0.0093(6) 0.0079(6) N4 0.0294(7) 0.0354(8) 0.0320(7) 0.0072(6) 0.0045(6) 0.0070(6) N5 0.0288(7) 0.0342(8) 0.0342(7) 0.0074(6) 0.0038(6) 0.0074(6) N6 0.0290(7) 0.0343(8) 0.0328(7) 0.0033(6) 0.0076(6) 0.0080(6) C1 0.0491(12) 0.0430(12) 0.0417(10) 0.0082(9) 0.0065(9) 0.0069(9) C2 0.121(3) 0.0592(16) 0.0472(13) 0.0053(12) 0.0092(14) 0.0464(17) C3 0.0727(19) 0.120(3) 0.084(2) 0.052(2) 0.0339(16) 0.0529(19) C4 0.0571(15) 0.0645(17) 0.094(2) 0.0304(16) -0.0083(14) 0.0148(13) C5 0.0518(14) 0.091(2) 0.0483(13) 0.0235(13) 0.0102(11) -0.0039(14) C6 0.0738(17) 0.0578(15) 0.0414(12) 0.0138(11) 0.0078(11) -0.0066(13) C7 0.0617(15) 0.0773(18) 0.0415(12) 0.0164(12) 0.0023(10) -0.0002(13) C8 0.0574(13) 0.0476(13) 0.0446(11) 0.0099(10) 0.0099(10) 0.0000(11) C9 0.0385(9) 0.0332(10) 0.0371(9) 0.0067(8) 0.0098(7) 0.0114(8) C10 0.0348(9) 0.0313(9) 0.0338(9) 0.0073(7) 0.0045(7) 0.0057(7) C11 0.0410(10) 0.0328(10) 0.0365(9) 0.0095(8) 0.0105(8) 0.0040(8) C12 0.0539(12) 0.0289(10) 0.0385(10) 0.0096(8) 0.0101(8) 0.0091(9) C13 0.0483(11) 0.0354(10) 0.0408(10) 0.0090(8) 0.0086(8) 0.0164(9) C14 0.0347(9) 0.0291(9) 0.0334(9) 0.0066(7) 0.0038(7) 0.0038(7) C15 0.0477(11) 0.0317(10) 0.0386(10) 0.0097(8) 0.0120(8) 0.0079(8) C16 0.0645(13) 0.0328(10) 0.0379(10) 0.0116(8) 0.0127(9) 0.0166(9) C17 0.0553(12) 0.0377(10) 0.0366(9) 0.0081(8) 0.0068(8) 0.0228(9) C18 0.0401(10) 0.0320(9) 0.0316(9) 0.0037(7) 0.0059(7) 0.0105(8) C19 0.0341(9) 0.0339(10) 0.0411(10) 0.0072(8) 0.0115(8) 0.0075(8) C20 0.0454(11) 0.0403(11) 0.0366(10) 0.0028(8) 0.0097(8) 0.0128(9) C21 0.0475(11) 0.0453(12) 0.0442(10) 0.0117(9) 0.0224(9) 0.0152(9) C22 0.0390(10) 0.0405(11) 0.0545(12) 0.0127(9) 0.0210(9) 0.0081(9) C23 0.0330(9) 0.0366(10) 0.0400(10) 0.0044(8) 0.0068(7) 0.0088(8) C25 0.0351(10) 0.0428(11) 0.0473(11) 0.0027(9) 0.0012(8) 0.0077(9) C26 0.0363(10) 0.0667(15) 0.0373(10) 0.0018(10) 0.0007(8) 0.0090(10) C27 0.0325(9) 0.0648(14) 0.0421(10) 0.0178(10) 0.0028(8) 0.0119(9) C28 0.0380(10) 0.0564(13) 0.0529(12) 0.0146(10) 0.0095(9) 0.0180(10) C29 0.0326(9) 0.0538(12) 0.0383(10) 0.0068(9) 0.0062(8) 0.0112(9) C30 0.0329(10) 0.0508(12) 0.0518(12) 0.0009(10) 0.0044(8) 0.0135(9) C31 0.0414(11) 0.0537(14) 0.0781(16) 0.0162(12) -0.0021(11) 0.0186(10) C32 0.0327(10) 0.0590(14) 0.0474(11) 0.0192(10) -0.0015(8) 0.0095(9) C33 0.0354(10) 0.0598(14) 0.0394(10) 0.0035(10) 0.0016(8) 0.0066(10) C34 0.0346(9) 0.0405(11) 0.0468(11) 0.0062(9) 0.0012(8) 0.0099(8) C35 0.0338(9) 0.0402(11) 0.0425(10) 0.0015(8) 0.0044(8) 0.0123(8) C36 0.0371(10) 0.0410(11) 0.0688(14) 0.0081(10) 0.0237(10) 0.0063(9) C37 0.0437(11) 0.0467(12) 0.0450(11) 0.0114(9) 0.0214(9) 0.0166(9) C38 0.0431(11) 0.0564(13) 0.0375(10) -0.0018(9) 0.0073(8) 0.0192(10) C39 0.0357(10) 0.0425(12) 0.0483(11) -0.0041(9) 0.0156(9) 0.0038(9) C40 0.0585(14) 0.0490(13) 0.0432(11) 0.0030(10) 0.0075(10) 0.0037(11) C41 0.0696(17) 0.086(2) 0.0431(13) 0.0168(13) -0.0004(11) -0.0059(15) C42 0.0807(19) 0.0718(18) 0.0435(13) 0.0154(12) 0.0055(12) -0.0108(15) C43 0.0748(18) 0.110(3) 0.0457(13) 0.0206(15) 0.0076(13) -0.0323(18) C44 0.0554(12) 0.0383(11) 0.0442(11) 0.0100(9) 0.0148(9) 0.0076(10) C45 0.112(2) 0.0549(15) 0.0447(12) 0.0100(11) 0.0115(13) 0.0403(16) C46 0.111(3) 0.122(3) 0.097(2) 0.068(2) 0.057(2) 0.085(2) C47 0.0471(14) 0.082(2) 0.117(3) 0.058(2) 0.0070(15) 0.0167(14) O6 0.0860(13) 0.0525(10) 0.0581(10) 0.0179(8) -0.0120(9) 0.0017(9) C52 0.0757(17) 0.0622(16) 0.0553(14) 0.0207(12) 0.0046(12) 0.0243(14) C53 0.0625(15) 0.0521(14) 0.0606(14) 0.0181(11) 0.0209(11) 0.0181(12) C54 0.0500(13) 0.0608(15) 0.0628(14) 0.0085(12) 0.0068(11) 0.0135(11) C55 0.0668(15) 0.0605(15) 0.0520(13) 0.0214(12) -0.0020(11) 0.0093(13) O5 0.1078(17) 0.0546(11) 0.0768(13) 0.0203(10) -0.0255(12) 0.0049(11) C48 0.0721(18) 0.0696(18) 0.0700(17) 0.0142(14) -0.0064(14) 0.0170(15) C49 0.0709(17) 0.0712(18) 0.0669(16) 0.0359(14) 0.0018(13) 0.0047(14) C50 0.136(3) 0.072(2) 0.0620(17) 0.0267(15) 0.0058(18) 0.042(2) C51 0.0611(15) 0.0588(15) 0.0707(16) 0.0253(13) 0.0211(12) 0.0206(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Mg2 Mg1 Na4 158.48(3) N1 Mg1 Mg2 45.41(4) N1 Mg1 Na4 156.11(5) N2 Mg1 Mg2 45.82(4) N2 Mg1 Na4 112.69(5) N2 Mg1 N1 91.19(6) N3 Mg1 Mg2 128.77(5) N3 Mg1 Na4 54.03(5) N3 Mg1 N1 116.20(6) N3 Mg1 N2 117.72(6) N3 Mg1 N4 100.79(6) N4 Mg1 Mg2 130.43(5) N4 Mg1 Na4 53.92(4) N4 Mg1 N1 115.76(6) N4 Mg1 N2 116.28(6) Mg1 Mg2 Na1 161.77(3) N1 Mg2 Mg1 45.96(4) N1 Mg2 Na1 115.83(5) N1 Mg2 N2 91.39(6) N2 Mg2 Mg1 45.47(4) N2 Mg2 Na1 152.76(5) N5 Mg2 Mg1 128.33(5) N5 Mg2 Na1 53.86(4) N5 Mg2 N1 117.67(6) N5 Mg2 N2 115.65(6) N6 Mg2 Mg1 130.59(5) N6 Mg2 Na1 53.11(5) N6 Mg2 N1 117.33(6) N6 Mg2 N2 114.82(6) N6 Mg2 N5 100.99(6) O1 Na1 Mg2 122.37(5) O1 Na1 O2 81.62(6) O1 Na1 N5 117.61(6) O1 Na1 N6 129.76(6) O1 Na1 C39 150.74(6) O2 Na1 Mg2 155.98(5) O2 Na1 N5 130.77(6) O2 Na1 N6 122.56(6) O2 Na1 C39 99.66(6) N5 Na1 Mg2 42.74(4) N5 Na1 C39 83.83(6) N6 Na1 Mg2 42.71(4) N6 Na1 N5 81.29(5) N6 Na1 C39 28.35(5) C39 Na1 Mg2 59.23(4) O3 Na4 Mg1 152.67(5) O3 Na4 N3 119.46(6) O3 Na4 N4 128.70(6) O3 Na4 C25 100.38(6) O4 Na4 Mg1 122.87(5) O4 Na4 O3 84.46(6) O4 Na4 N3 132.81(6) O4 Na4 N4 117.11(6) O4 Na4 C25 132.50(6) N3 Na4 Mg1 42.75(4) N3 Na4 C25 85.71(6) N4 Na4 Mg1 43.02(4) N4 Na4 N3 80.82(5) N4 Na4 C25 30.17(5) C25 Na4 Mg1 62.84(4) C1 O1 Na1 137.65(13) C1 O1 C4 105.64(18) C4 O1 Na1 116.41(15) C5 O2 Na1 117.48(13) C8 O2 Na1 135.83(12) C8 O2 C5 104.50(17) C40 O3 Na4 133.86(13) C43 O3 Na4 118.22(14) C43 O3 C40 105.82(17) C44 O4 Na4 140.57(13) C47 O4 Na4 112.87(15) C47 O4 C44 106.48(18) Mg2 N1 Mg1 88.63(6) C9 N1 Mg1 113.45(11) C9 N1 Mg2 116.95(11) C10 N1 Mg1 109.21(11) C10 N1 Mg2 118.77(11) C10 N1 C9 108.36(14) Mg1 N2 Mg2 88.71(6) C14 N2 Mg1 112.96(11) C14 N2 Mg2 115.03(11) C14 N2 C18 107.69(14) C18 N2 Mg1 121.20(11) C18 N2 Mg2 110.47(11) Mg1 N3 Na4 83.22(6) C19 N3 Mg1 111.28(11) C19 N3 Na4 111.64(11) C23 N3 Mg1 129.88(12) C23 N3 Na4 111.89(11) C23 N3 C19 106.59(14) Mg1 N4 Na4 83.06(5) C25 N4 Mg1 120.71(12) C25 N4 Na4 91.27(11) C25 N4 C29 107.30(15) C29 N4 Mg1 117.39(11) C29 N4 Na4 135.65(13) Mg2 N5 Na1 83.41(5) C30 N5 Mg2 125.88(12) C30 N5 Na1 115.04(13) C30 N5 C34 106.47(15) C34 N5 Mg2 113.91(12) C34 N5 Na1 110.05(11) Mg2 N6 Na1 84.18(6) C35 N6 Mg2 123.79(12) C35 N6 Na1 124.65(12) C35 N6 C39 106.75(15) C39 N6 Mg2 115.34(12) C39 N6 Na1 99.02(13) O1 C1 H1A 110.6 O1 C1 H1B 110.6 O1 C1 C2 105.5(2) H1A C1 H1B 108.8 C2 C1 H1A 110.6 C2 C1 H1B 110.6 C1 C2 H2A 111.2 C1 C2 H2B 111.2 C1 C2 C3 102.6(2) H2A C2 H2B 109.2 C3 C2 H2A 111.2 C3 C2 H2B 111.2 C2 C3 H3A 111.1 C2 C3 H3B 111.1 H3A C3 H3B 109.0 C4 C3 C2 103.4(2) C4 C3 H3A 111.1 C4 C3 H3B 111.1 O1 C4 C3 102.0(2) O1 C4 H4A 111.4 O1 C4 H4B 111.4 C3 C4 H4A 111.4 C3 C4 H4B 111.4 H4A C4 H4B 109.2 O2 C5 H5A 110.3 O2 C5 H5B 110.3 O2 C5 C6 107.2(2) H5A C5 H5B 108.5 C6 C5 H5A 110.3 C6 C5 H5B 110.3 C5 C6 H6A 110.8 C5 C6 H6B 110.8 C5 C6 C7 105.0(2) H6A C6 H6B 108.8 C7 C6 H6A 110.8 C7 C6 H6B 110.8 C6 C7 H7A 110.9 C6 C7 H7B 110.9 H7A C7 H7B 108.9 C8 C7 C6 104.38(19) C8 C7 H7A 110.9 C8 C7 H7B 110.9 O2 C8 C7 106.23(18) O2 C8 H8A 110.5 O2 C8 H8B 110.5 C7 C8 H8A 110.5 C7 C8 H8B 110.5 H8A C8 H8B 108.7 N1 C9 H9A 108.9 N1 C9 H9B 108.9 N1 C9 C13 113.26(15) H9A C9 H9B 107.7 C13 C9 H9A 108.9 C13 C9 H9B 108.9 N1 C10 H10A 108.8 N1 C10 H10B 108.8 N1 C10 C11 113.66(15) H10A C10 H10B 107.7 C11 C10 H10A 108.8 C11 C10 H10B 108.8 C10 C11 H11A 109.6 C10 C11 H11B 109.6 H11A C11 H11B 108.1 C12 C11 C10 110.26(15) C12 C11 H11A 109.6 C12 C11 H11B 109.6 C11 C12 H12A 109.8 C11 C12 H12B 109.8 H12A C12 H12B 108.3 C13 C12 C11 109.35(16) C13 C12 H12A 109.8 C13 C12 H12B 109.8 C9 C13 H13A 109.7 C9 C13 H13B 109.7 C12 C13 C9 109.81(16) C12 C13 H13A 109.7 C12 C13 H13B 109.7 H13A C13 H13B 108.2 N2 C14 H14A 109.0 N2 C14 H14B 109.0 N2 C14 C15 112.95(15) H14A C14 H14B 107.8 C15 C14 H14A 109.0 C15 C14 H14B 109.0 C14 C15 H15A 109.5 C14 C15 H15B 109.5 H15A C15 H15B 108.1 C16 C15 C14 110.63(16) C16 C15 H15A 109.5 C16 C15 H15B 109.5 C15 C16 H16A 109.8 C15 C16 H16B 109.8 H16A C16 H16B 108.2 C17 C16 C15 109.42(16) C17 C16 H16A 109.8 C17 C16 H16B 109.8 C16 C17 H17A 109.7 C16 C17 H17B 109.7 C16 C17 C18 109.68(16) H17A C17 H17B 108.2 C18 C17 H17A 109.7 C18 C17 H17B 109.7 N2 C18 C17 113.19(15) N2 C18 H18A 108.9 N2 C18 H18B 108.9 C17 C18 H18A 108.9 C17 C18 H18B 108.9 H18A C18 H18B 107.8 N3 C19 H19A 108.9 N3 C19 H19B 108.9 N3 C19 C20 113.41(16) H19A C19 H19B 107.7 C20 C19 H19A 108.9 C20 C19 H19B 108.9 C19 C20 H20A 109.8 C19 C20 H20B 109.8 H20A C20 H20B 108.3 C21 C20 C19 109.35(16) C21 C20 H20A 109.8 C21 C20 H20B 109.8 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 108.1 C22 C21 C20 110.68(16) C22 C21 H21A 109.5 C22 C21 H21B 109.5 C21 C22 H22A 109.5 C21 C22 H22B 109.5 C21 C22 C23 110.60(16) H22A C22 H22B 108.1 C23 C22 H22A 109.5 C23 C22 H22B 109.5 N3 C23 C22 112.94(16) N3 C23 H23A 109.0 N3 C23 H23B 109.0 C22 C23 H23A 109.0 C22 C23 H23B 109.0 H23A C23 H23B 107.8 Na4 C25 H25A 156.9 Na4 C25 H25B 64.1 N4 C25 Na4 58.56(9) N4 C25 H25A 108.8 N4 C25 H25B 108.8 N4 C25 C26 113.61(18) H25A C25 H25B 107.7 C26 C25 Na4 94.18(13) C26 C25 H25A 108.8 C26 C25 H25B 108.8 C25 C26 H26A 109.6 C25 C26 H26B 109.6 H26A C26 H26B 108.1 C27 C26 C25 110.41(17) C27 C26 H26A 109.6 C27 C26 H26B 109.6 C26 C27 H27A 109.6 C26 C27 H27B 109.6 H27A C27 H27B 108.1 C28 C27 C26 110.30(16) C28 C27 H27A 109.6 C28 C27 H27B 109.6 C27 C28 H28A 109.6 C27 C28 H28B 109.6 C27 C28 C29 110.46(18) H28A C28 H28B 108.1 C29 C28 H28A 109.6 C29 C28 H28B 109.6 N4 C29 C28 114.37(16) N4 C29 H29A 108.7 N4 C29 H29B 108.7 C28 C29 H29A 108.7 C28 C29 H29B 108.7 H29A C29 H29B 107.6 N5 C30 H30A 108.9 N5 C30 H30B 108.9 N5 C30 C31 113.40(18) H30A C30 H30B 107.7 C31 C30 H30A 108.9 C31 C30 H30B 108.9 C30 C31 H31A 109.5 C30 C31 H31B 109.5 H31A C31 H31B 108.1 C32 C31 C30 110.56(19) C32 C31 H31A 109.5 C32 C31 H31B 109.5 C31 C32 H32A 109.7 C31 C32 H32B 109.7 C31 C32 C33 109.97(17) H32A C32 H32B 108.2 C33 C32 H32A 109.7 C33 C32 H32B 109.7 C32 C33 H33A 109.9 C32 C33 H33B 109.9 C32 C33 C34 109.04(17) H33A C33 H33B 108.3 C34 C33 H33A 109.9 C34 C33 H33B 109.9 N5 C34 C33 113.62(17) N5 C34 H34A 108.8 N5 C34 H34B 108.8 C33 C34 H34A 108.8 C33 C34 H34B 108.8 H34A C34 H34B 107.7 N6 C35 H35A 108.8 N6 C35 H35B 108.8 N6 C35 C36 113.86(17) H35A C35 H35B 107.7 C36 C35 H35A 108.8 C36 C35 H35B 108.8 C35 C36 H36A 109.6 C35 C36 H36B 109.6 H36A C36 H36B 108.1 C37 C36 C35 110.28(17) C37 C36 H36A 109.6 C37 C36 H36B 109.6 C36 C37 H37A 109.6 C36 C37 H37B 109.6 H37A C37 H37B 108.2 C38 C37 C36 110.07(16) C38 C37 H37A 109.6 C38 C37 H37B 109.6 C37 C38 H38A 109.8 C37 C38 H38B 109.8 C37 C38 C39 109.47(17) H38A C38 H38B 108.2 C39 C38 H38A 109.8 C39 C38 H38B 109.8 Na1 C39 H39A 75.3(14) Na1 C39 H39B 161.8(15) N6 C39 Na1 52.63(10) N6 C39 C38 114.18(18) N6 C39 H39A 111.3(14) N6 C39 H39B 113.7(14) C38 C39 Na1 90.60(14) C38 C39 H39A 106.8(14) C38 C39 H39B 107.0(15) H39A C39 H39B 103(2) O3 C40 H40A 110.6 O3 C40 H40B 110.6 O3 C40 C41 105.69(19) H40A C40 H40B 108.7 C41 C40 H40A 110.6 C41 C40 H40B 110.6 C40 C41 H41A 110.7 C40 C41 H41B 110.7 C40 C41 C42 105.2(2) H41A C41 H41B 108.8 C42 C41 H41A 110.7 C42 C41 H41B 110.7 C41 C42 H42A 110.7 C41 C42 H42B 110.7 H42A C42 H42B 108.8 C43 C42 C41 105.4(2) C43 C42 H42A 110.7 C43 C42 H42B 110.7 O3 C43 C42 109.3(2) O3 C43 H43A 109.8 O3 C43 H43B 109.8 C42 C43 H43A 109.8 C42 C43 H43B 109.8 H43A C43 H43B 108.3 O4 C44 H44A 110.3 O4 C44 H44B 110.3 O4 C44 C45 107.1(2) H44A C44 H44B 108.5 C45 C44 H44A 110.3 C45 C44 H44B 110.3 C44 C45 H45A 111.0 C44 C45 H45B 111.0 H45A C45 H45B 109.0 C46 C45 C44 103.6(2) C46 C45 H45A 111.0 C46 C45 H45B 111.0 C45 C46 H46A 111.1 C45 C46 H46B 111.1 H46A C46 H46B 109.1 C47 C46 C45 103.3(2) C47 C46 H46A 111.1 C47 C46 H46B 111.1 O4 C47 C46 103.0(2) O4 C47 H47A 111.2 O4 C47 H47B 111.2 C46 C47 H47A 111.2 C46 C47 H47B 111.2 H47A C47 H47B 109.1 C52 O6 C55 108.22(19) O6 C52 H52A 110.1 O6 C52 H52B 110.1 O6 C52 C53 108.0(2) H52A C52 H52B 108.4 C53 C52 H52A 110.1 C53 C52 H52B 110.1 C52 C53 H53A 111.3 C52 C53 H53B 111.3 C52 C53 C54 102.4(2) H53A C53 H53B 109.2 C54 C53 H53A 111.3 C54 C53 H53B 111.3 C53 C54 H54A 111.3 C53 C54 H54B 111.3 H54A C54 H54B 109.2 C55 C54 C53 102.1(2) C55 C54 H54A 111.3 C55 C54 H54B 111.3 O6 C55 C54 105.4(2) O6 C55 H55A 110.7 O6 C55 H55B 110.7 C54 C55 H55A 110.7 C54 C55 H55B 110.7 H55A C55 H55B 108.8 C49 O5 C50 108.7(2) H48A C48 H48B 109.0 C49 C48 H48A 111.0 C49 C48 H48B 111.0 C49 C48 C51 103.6(2) C51 C48 H48A 111.0 C51 C48 H48B 111.0 O5 C49 C48 105.7(2) O5 C49 H49A 110.6 O5 C49 H49B 110.6 C48 C49 H49A 110.6 C48 C49 H49B 110.6 H49A C49 H49B 108.7 O5 C50 H50A 110.0 O5 C50 H50B 110.0 O5 C50 C51 108.4(2) H50A C50 H50B 108.4 C51 C50 H50A 110.0 C51 C50 H50B 110.0 C48 C51 H51A 111.4 C48 C51 H51B 111.4 C50 C51 C48 101.9(2) C50 C51 H51A 111.4 C50 C51 H51B 111.4 H51A C51 H51B 109.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mg1 Mg2 2.9764(8) Mg1 Na4 3.0224(9) Mg1 N1 2.1403(15) Mg1 N2 2.1224(15) Mg1 N3 2.0661(15) Mg1 N4 2.0773(16) Mg2 Na1 3.0408(9) Mg2 N1 2.1202(15) Mg2 N2 2.1352(15) Mg2 N5 2.0774(16) Mg2 N6 2.0733(15) Na1 O1 2.3480(17) Na1 O2 2.3625(15) Na1 N5 2.4719(16) Na1 N6 2.4445(17) Na1 C39 3.038(3) Na4 O3 2.3519(15) Na4 O4 2.3429(16) Na4 N3 2.4635(17) Na4 N4 2.4607(16) Na4 C25 2.883(2) O1 C1 1.417(3) O1 C4 1.423(3) O2 C5 1.446(3) O2 C8 1.424(3) O3 C40 1.433(3) O3 C43 1.429(3) O4 C44 1.429(2) O4 C47 1.424(3) N1 C9 1.467(2) N1 C10 1.467(2) N2 C14 1.468(2) N2 C18 1.469(2) N3 C19 1.464(2) N3 C23 1.458(2) N4 C25 1.450(2) N4 C29 1.456(2) N5 C30 1.449(2) N5 C34 1.454(2) N6 C35 1.450(2) N6 C39 1.461(3) C1 H1A 0.9900 C1 H1B 0.9900 C1 C2 1.531(3) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.541(4) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.491(4) C4 H4A 0.9900 C4 H4B 0.9900 C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.477(3) C6 H6A 0.9900 C6 H6B 0.9900 C6 C7 1.514(3) C7 H7A 0.9900 C7 H7B 0.9900 C7 C8 1.495(3) C8 H8A 0.9900 C8 H8B 0.9900 C9 H9A 0.9900 C9 H9B 0.9900 C9 C13 1.537(3) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.534(2) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.526(3) C12 H12A 0.9900 C12 H12B 0.9900 C12 C13 1.522(3) C13 H13A 0.9900 C13 H13B 0.9900 C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.533(2) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.526(3) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.525(3) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.535(3) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19A 0.9900 C19 H19B 0.9900 C19 C20 1.533(3) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.526(3) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.524(3) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.533(3) C23 H23A 0.9900 C23 H23B 0.9900 C25 H25A 0.9900 C25 H25B 0.9900 C25 C26 1.534(3) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.519(3) C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.516(3) C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.524(3) C29 H29A 0.9900 C29 H29B 0.9900 C30 H30A 0.9900 C30 H30B 0.9900 C30 C31 1.533(3) C31 H31A 0.9900 C31 H31B 0.9900 C31 C32 1.508(3) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.522(3) C33 H33A 0.9900 C33 H33B 0.9900 C33 C34 1.533(3) C34 H34A 0.9900 C34 H34B 0.9900 C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.526(3) C36 H36A 0.9900 C36 H36B 0.9900 C36 C37 1.519(3) C37 H37A 0.9900 C37 H37B 0.9900 C37 C38 1.517(3) C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.532(3) C39 H39A 0.96(3) C39 H39B 1.03(3) C40 H40A 0.9900 C40 H40B 0.9900 C40 C41 1.493(3) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.496(4) C42 H42A 0.9900 C42 H42B 0.9900 C42 C43 1.451(3) C43 H43A 0.9900 C43 H43B 0.9900 C44 H44A 0.9900 C44 H44B 0.9900 C44 C45 1.518(3) C45 H45A 0.9900 C45 H45B 0.9900 C45 C46 1.511(5) C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.509(5) C47 H47A 0.9900 C47 H47B 0.9900 O6 C52 1.422(3) O6 C55 1.428(3) C52 H52A 0.9900 C52 H52B 0.9900 C52 C53 1.499(4) C53 H53A 0.9900 C53 H53B 0.9900 C53 C54 1.512(3) C54 H54A 0.9900 C54 H54B 0.9900 C54 C55 1.489(3) C55 H55A 0.9900 C55 H55B 0.9900 O5 C49 1.420(3) O5 C50 1.421(3) C48 H48A 0.9900 C48 H48B 0.9900 C48 C49 1.493(4) C48 C51 1.498(4) C49 H49A 0.9900 C49 H49B 0.9900 C50 H50A 0.9900 C50 H50B 0.9900 C50 C51 1.468(4) C51 H51A 0.9900 C51 H51B 0.9900 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 Mg1 N1 C9 C13 -179.40(12) Mg1 N1 C10 C11 -178.77(12) Mg1 N2 C14 C15 77.82(16) Mg1 N2 C18 C17 -72.51(18) Mg1 N3 C19 C20 151.24(13) Mg1 N3 C23 C22 -161.08(13) Mg1 N4 C25 Na4 -82.68(10) Mg1 N4 C25 C26 -162.67(13) Mg1 N4 C29 C28 161.16(14) Mg2 N1 C9 C13 79.57(17) Mg2 N1 C10 C11 -79.43(17) Mg2 N2 C14 C15 177.65(12) Mg2 N2 C18 C17 -173.93(12) Mg2 N5 C30 C31 -162.73(14) Mg2 N5 C34 C33 155.47(13) Mg2 N6 C35 C36 163.09(14) Mg2 N6 C39 Na1 -87.80(10) Mg2 N6 C39 C38 -158.62(14) Na1 O1 C1 C2 137.01(19) Na1 O1 C4 C3 -127.78(19) Na1 O2 C5 C6 160.83(18) Na1 O2 C8 C7 -162.06(17) Na1 N5 C30 C31 -62.3(2) Na1 N5 C34 C33 63.86(18) Na1 N6 C35 C36 54.8(2) Na1 N6 C39 C38 -70.82(18) Na4 O3 C40 C41 167.36(18) Na4 O3 C43 C42 -169.1(2) Na4 O4 C44 C45 -157.22(16) Na4 O4 C47 C46 142.18(17) Na4 N3 C19 C20 60.20(17) Na4 N3 C23 C22 -61.30(18) Na4 N4 C25 C26 -79.99(16) Na4 N4 C29 C28 51.6(2) Na4 C25 C26 C27 -114.90(17) O1 C1 C2 C3 10.6(2) O2 C5 C6 C7 17.2(3) O3 C40 C41 C42 24.0(3) O4 C44 C45 C46 -1.5(3) N1 C9 C13 C12 58.6(2) N1 C10 C11 C12 -57.0(2) N2 C14 C15 C16 57.7(2) N3 C19 C20 C21 58.8(2) N4 C25 C26 C27 -57.5(2) N5 C30 C31 C32 -57.8(3) N6 C35 C36 C37 58.0(2) C1 O1 C4 C3 47.0(3) C1 C2 C3 C4 16.7(3) C2 C3 C4 O1 -38.3(3) C4 O1 C1 C2 -36.0(2) C5 O2 C8 C7 36.1(3) C5 C6 C7 C8 4.5(3) C6 C7 C8 O2 -25.0(3) C8 O2 C5 C6 -33.3(3) C9 N1 C10 C11 57.20(19) C10 N1 C9 C13 -57.95(19) C10 C11 C12 C13 54.3(2) C11 C12 C13 C9 -55.0(2) C14 N2 C18 C17 59.70(19) C14 C15 C16 C17 -53.8(2) C15 C16 C17 C18 54.0(2) C16 C17 C18 N2 -59.0(2) C18 N2 C14 C15 -58.70(18) C19 N3 C23 C22 61.0(2) C19 C20 C21 C22 -51.2(2) C20 C21 C22 C23 51.0(2) C21 C22 C23 N3 -57.5(2) C23 N3 C19 C20 -62.2(2) C25 N4 C29 C28 -59.0(2) C25 C26 C27 C28 51.4(3) C26 C27 C28 C29 -50.9(2) C27 C28 C29 N4 56.6(2) C29 N4 C25 Na4 139.11(15) C29 N4 C25 C26 59.1(2) C30 N5 C34 C33 -61.4(2) C30 C31 C32 C33 52.3(3) C31 C32 C33 C34 -52.7(2) C32 C33 C34 N5 59.5(2) C34 N5 C30 C31 59.9(2) C35 N6 C39 Na1 130.46(15) C35 N6 C39 C38 59.6(2) C35 C36 C37 C38 -52.6(2) C36 C37 C38 C39 52.3(2) C37 C38 C39 Na1 -106.69(16) C37 C38 C39 N6 -58.0(3) C39 N6 C35 C36 -59.2(2) C40 O3 C43 C42 25.1(4) C40 C41 C42 C43 -8.9(4) C41 C42 C43 O3 -9.6(4) C43 O3 C40 C41 -30.1(3) C44 O4 C47 C46 -40.2(3) C44 C45 C46 C47 -22.0(3) C45 C46 C47 O4 38.2(3) C47 O4 C44 C45 26.3(2) O6 C52 C53 C54 -20.6(3) C52 O6 C55 C54 24.3(3) C52 C53 C54 C55 34.0(3) C53 C54 C55 O6 -36.5(3) C55 O6 C52 C53 -1.9(3) O5 C50 C51 C48 26.9(4) C49 O5 C50 C51 -9.2(4) C49 C48 C51 C50 -33.7(3) C50 O5 C49 C48 -12.9(4) C51 C48 C49 O5 29.3(3)