#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:02:37 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247582 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125681.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_7125681 loop_ _publ_author_name 'Vasilenko, Vladislav' 'Blasius, Clemens K.' 'Wadepohl, Hubert' 'Gade, Lutz H.' _publ_section_title ; Borohydride intermediates pave the way for magnesium-catalysed enantioselective ketone reduction. ; _journal_issue 8 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1203 _journal_page_last 1206 _journal_paper_doi 10.1039/c9cc09111d _journal_volume 56 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C44 H46 F Mg N3 O5' _chemical_formula_sum 'C44 H46 F Mg N3 O5' _chemical_formula_weight 740.15 _chemical_properties_physical 'air-sensitive, moisture-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_block_code ga_vv35 _audit_creation_date 2018-11-09 _audit_creation_method ; Olex2 1.2 (compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-29 deposited with the CCDC. 2019-12-20 downloaded from the CCDC. ; _cell_angle_alpha 65.663(3) _cell_angle_beta 88.065(3) _cell_angle_gamma 84.019(3) _cell_formula_units_Z 1 _cell_length_a 9.5675(4) _cell_length_b 9.7347(4) _cell_length_c 11.4970(3) _cell_measurement_reflns_used 16003 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 70.5300 _cell_measurement_theta_min 4.2080 _cell_volume 970.28(7) _computing_cell_refinement 'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)' _computing_publication_material 'encif (Wadepohl, 2009-18); encifer 1.6.x (CCDC, 2016)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _diffrn_ambient_temperature 120(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9621 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -69.00 21.00 1.00 5.00 -- 0.00 -57.00 -30.00 90 2 \w -21.00 69.00 1.00 5.00 -- 0.00 57.00-120.00 90 3 \w -21.00 69.00 1.00 5.00 -- 0.00 57.00 120.00 90 4 \w -35.00 14.00 1.00 5.00 -- 10.00 106.00 133.46 49 5 \w -39.00 4.00 1.00 5.00 -- 14.00 118.00 -86.04 43 6 \w -37.00 1.00 1.00 5.00 -- 18.00 122.00 14.40 38 7 \w -10.00 17.00 1.00 10.00 -- 34.00 103.00 65.76 27 8 \w -1.00 27.00 1.00 10.00 -- 38.00 93.00-106.78 28 9 \w 6.00 33.00 1.00 10.00 -- 42.00 88.00 88.61 27 10 \w 6.00 33.00 1.00 10.00 -- 42.00 88.00 -77.81 27 11 \w 13.00 40.00 1.00 10.00 -- 46.00 83.00 -42.19 27 12 \w 17.00 45.00 1.00 10.00 -- 50.00 82.00 165.92 28 13 \w 17.00 45.00 1.00 10.00 -- 50.00 82.00 38.45 28 14 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 150.00 100 15 \w -15.00 75.00 1.00 10.00 -- 54.00 -57.00 60.00 90 16 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 90.00 100 17 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 0.00 100 18 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 -90.00 100 19 \w 1.00 96.00 1.00 10.00 -- 54.00 -99.00 -30.00 95 20 \w 23.00 111.00 1.00 10.00 -- 54.00-125.00-120.00 88 21 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 120.00 100 22 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00 -60.00 100 23 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00-120.00 100 24 \w 23.00 111.00 1.00 10.00 -- 54.00-125.00 -60.00 88 25 \w 24.00 124.00 1.00 10.00 -- 54.00 77.00-150.00 100 26 \w 34.00 126.00 1.00 10.00 -- 58.00 67.00 81.54 92 27 \w 29.00 128.00 1.00 10.00 -- 58.00 76.00-173.72 99 28 \w 29.00 128.00 1.00 10.00 -- 58.00 75.00 -21.34 99 29 \w 37.00 134.00 1.00 10.00 -- 62.00 39.00 135.48 97 30 \w 33.00 132.00 1.00 10.00 -- 62.00 76.00 -80.30 99 31 \w 37.00 136.00 1.00 10.00 -- 66.00 76.00-136.16 99 32 \w 38.00 135.00 1.00 10.00 -- 66.00 73.00 53.73 97 33 \w 39.00 135.00 1.00 10.00 -- 66.00 72.00-163.00 96 34 \w 42.00 140.00 1.00 10.00 -- 70.00 74.00 -38.50 98 35 \w 44.00 139.00 1.00 10.00 -- 70.00 70.00 46.23 95 36 \w 49.00 139.00 1.00 10.00 -- 70.00 57.00-142.62 90 37 \w 51.00 145.00 1.00 10.00 -- 74.00 45.00 59.53 94 38 \w 45.00 144.00 1.00 10.00 -- 74.00 76.00 -65.04 99 39 \w 52.00 142.00 1.00 10.00 -- 74.00 61.00 -12.12 90 40 \w 53.00 146.00 1.00 10.00 -- 78.00 69.00 -66.01 93 41 \w 54.00 146.00 1.00 10.00 -- 78.00 67.00 106.32 92 42 \w 50.00 148.00 1.00 10.00 -- 78.00 74.00 140.76 98 43 \w 64.00 156.00 1.00 20.00 -- 86.00 50.00 131.10 92 44 \w 57.00 100.00 1.00 20.00 -- 86.00 76.00-150.13 43 45 \w 133.00 169.00 1.00 20.00 -- 98.00 44.00 147.36 36 46 \w 80.00 127.00 1.00 20.00 -- 98.00 44.00 147.36 47 47 \w 134.00 160.00 1.00 20.00 -- 108.00 64.00 -90.00 26 48 \w 85.00 116.00 1.00 20.00 -- 108.00 64.00 -90.00 31 49 \w 132.00 158.00 1.00 20.00 -- 108.00 77.00 120.00 26 50 \w 78.00 104.00 1.00 20.00 -- 108.00 77.00 120.00 26 51 \w 111.00 178.00 1.00 20.00 -- 108.00 77.00 -60.00 67 52 \w 78.00 104.00 1.00 20.00 -- 108.00 77.00 -60.00 26 53 \w 86.00 177.00 1.00 20.00 -- 108.00 48.00 -15.08 91 54 \w 79.00 176.00 1.00 20.00 -- 108.00 77.00-150.00 97 55 \w 83.00 113.00 1.00 20.00 -- 108.00-111.00 0.00 30 56 \w 146.00 172.00 1.00 20.00 -- 108.00 77.00 0.00 26 57 \w 78.00 113.00 1.00 20.00 -- 108.00 77.00 0.00 35 58 \w 85.00 111.00 1.00 20.00 -- 108.00 64.00 60.00 26 59 \w 86.00 112.00 1.00 20.00 -- 108.00 38.00 -30.00 26 60 \w 82.00 157.00 1.00 20.00 -- 108.00 38.00 -60.00 75 61 \w 84.00 109.00 1.00 20.00 -- 108.00 38.00-180.00 25 62 \w 88.00 170.00 1.00 20.00 -- 108.00 64.00 90.00 82 63 \w 88.00 114.00 1.00 20.00 -- 108.00 64.00 -30.00 26 64 \w 79.00 105.00 1.00 20.00 -- 108.00 77.00 -90.00 26 65 \w 136.00 177.00 1.00 20.00 -- 108.00 77.00 150.00 41 66 \w 88.00 116.00 1.00 20.00 -- 108.00 64.00 150.00 28 67 \w 79.00 105.00 1.00 20.00 -- 108.00 77.00 150.00 26 68 \w 86.00 116.00 1.00 20.00 -- 108.00 64.00 -60.00 30 69 \w 42.00 109.00 1.00 20.00 -- 108.00 -92.00-150.00 67 70 \w 59.00 106.00 1.00 20.00 -- 108.00-111.00 120.00 47 71 \w 37.00 69.00 1.00 20.00 -- 108.00 -92.00 60.00 32 72 \w 86.00 112.00 1.00 20.00 -- 108.00 64.00 0.00 26 73 \w 85.00 142.00 1.00 20.00 -- 108.00 64.00 30.00 57 74 \w 117.00 178.00 1.00 20.00 -- 108.00 77.00-120.00 61 75 \w 81.00 106.00 1.00 20.00 -- 108.00 77.00-120.00 25 76 \w 93.00 124.00 1.00 20.00 -- 108.00 50.00-180.00 31 77 \w 79.00 137.00 1.00 20.00 -- 108.00 -77.00-150.00 58 78 \w 40.00 71.00 1.00 20.00 -- 108.00 -77.00-150.00 31 79 \w 124.00 177.00 1.00 20.00 -- 108.00 77.00 60.00 53 80 \w 79.00 157.00 1.00 20.00 -- 108.00 77.00-180.00 78 81 \w 78.00 104.00 1.00 20.00 -- 108.00 77.00 60.00 26 82 \w 82.00 108.00 1.00 20.00 -- 108.00 77.00 90.00 26 83 \w 122.00 176.00 1.00 20.00 -- 108.00 77.00 30.00 54 84 \w 88.00 115.00 1.00 20.00 -- 108.00 64.00-120.00 27 85 \w 78.00 104.00 1.00 20.00 -- 108.00 77.00 30.00 26 86 \w 83.00 120.00 1.00 20.00 -- 108.00 38.00 90.00 37 87 \w 78.00 104.00 1.00 20.00 -- 108.00 77.00 -30.00 26 88 \w 37.00 108.00 1.00 20.00 -- 108.00 -92.00 0.00 71 89 \w 38.00 108.00 1.00 20.00 -- 108.00 -92.00 150.00 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Agilent SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0613145000 _diffrn_orient_matrix_UB_12 0.1535831000 _diffrn_orient_matrix_UB_13 -0.0444680000 _diffrn_orient_matrix_UB_21 -0.0573888000 _diffrn_orient_matrix_UB_22 0.0452573000 _diffrn_orient_matrix_UB_23 -0.1357860000 _diffrn_orient_matrix_UB_31 -0.1384266000 _diffrn_orient_matrix_UB_32 0.0695083000 _diffrn_orient_matrix_UB_33 0.0348555000 _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.0242 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 23936 _diffrn_reflns_point_group_measured_fraction_full 0.929 _diffrn_reflns_point_group_measured_fraction_max 0.907 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.030 _diffrn_reflns_theta_min 4.221 _diffrn_source 'microfocus X-Ray tube' _diffrn_source_type 'Agilent SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model (Busing & Levy, 1957). Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour bronze _exptl_crystal_density_diffrn 1.267 _exptl_crystal_description irregular _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.116 _exptl_crystal_size_mid 0.084 _exptl_crystal_size_min 0.078 _refine_diff_density_max 0.116 _refine_diff_density_min -0.149 _refine_diff_density_rms 0.028 _refine_ls_abs_structure_details ; Flack x determined using 2912 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.019(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 534 _refine_ls_number_reflns 6787 _refine_ls_number_restraints 121 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0256 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.1299P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.0631 _reflns_Friedel_coverage 0.842 _reflns_Friedel_fraction_full 0.859 _reflns_Friedel_fraction_max 0.829 _reflns_number_gt 6573 _reflns_number_total 6787 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ga_vv35 - #3197 - in P1 - superflip - nova CELL 1.54184 9.5675 9.734667 11.497035 65.6635 88.065 84.0186 ZERR 1 0.000395 0.000399 0.000349 0.0034 0.0029 0.0034 LATT -1 SFAC C H F Mg N O UNIT 44 46 1 1 3 5 SADI 0.01 O5A C51A O5A C54A O5B C51B O5B C54B SADI 0.01 C51A C52A C53A C54A C51B C52B C53B C54B SADI 0.01 C52A C53A C52B C53B SADI C51A C53A C54A C52A C51B C53B C54B C52B SADI O5A C52A O5B C52B O5A C53A O5B C53B SADI Mg O5A Mg O5B Mg O4 SIMU 0.01 0.01 1 $C $O RIGU O5A > C54B L.S. 10 PLAN 25 SIZE 0.1 0.1 0.1 TEMP -153.25 CONF HTAB bond $H fmap 2 acta WGHT 0.032900 0.129900 FVAR 8.43821 0.51761 MG 4 0.506079 0.114912 0.830902 11.00000 0.01723 0.01865 = 0.01783 -0.00691 0.00002 -0.00196 F 3 0.308281 0.967074 0.379019 11.00000 0.08332 0.02744 = 0.07110 -0.00532 -0.02346 -0.00753 O1 6 0.514724 0.363625 1.071994 11.00000 0.03576 0.02540 = 0.03603 -0.01882 -0.00356 0.00005 O2 6 0.659017 -0.281621 0.753872 11.00000 0.03227 0.02049 = 0.02534 -0.01228 -0.00302 -0.00279 O3 6 0.383760 0.255097 0.692320 11.00000 0.02498 0.02722 = 0.02064 -0.00605 -0.00300 0.00207 O4 6 0.685119 0.238325 0.758217 11.00000 0.01818 0.02060 = 0.02892 -0.00957 0.00253 -0.00341 N1 5 0.459271 0.251319 0.944567 11.00000 0.01848 0.02114 = 0.02294 -0.00842 0.00247 -0.00102 N2 5 0.637941 -0.036572 0.998080 11.00000 0.02007 0.01943 = 0.01898 -0.00808 0.00004 -0.00341 N3 5 0.591692 -0.048909 0.748584 11.00000 0.02141 0.02116 = 0.01744 -0.00757 -0.00164 -0.00192 C1 1 0.366686 0.394506 0.901781 11.00000 0.02114 0.01987 = 0.02861 -0.00921 0.00328 -0.00075 AFIX 13 H1 2 0.375339 0.452296 0.807467 11.00000 -1.20000 AFIX 0 C2 1 0.428160 0.479952 0.972002 11.00000 0.02595 0.02341 = 0.04432 -0.01611 -0.00091 -0.00137 AFIX 23 H2A 2 0.485085 0.559403 0.913682 11.00000 -1.20000 H2B 2 0.352492 0.527506 1.008192 11.00000 -1.20000 AFIX 0 C3 1 0.532319 0.242647 1.039676 11.00000 0.02481 0.02222 = 0.02364 -0.01213 0.00455 -0.00510 C4 1 0.630626 0.121443 1.118583 11.00000 0.02689 0.02810 = 0.01976 -0.01126 -0.00237 -0.00473 AFIX 43 H4 2 0.668100 0.129279 1.190838 11.00000 -1.20000 AFIX 0 C5 1 0.674564 -0.003887 1.098312 11.00000 0.02193 0.02323 = 0.01712 -0.00692 0.00032 -0.00717 C6 1 0.771462 -0.128523 1.186308 11.00000 0.02070 0.02482 = 0.01922 -0.00586 0.00101 -0.00684 C7 1 0.842353 -0.147962 1.296840 11.00000 0.02917 0.03168 = 0.02127 -0.00919 -0.00103 -0.00969 AFIX 43 H7 2 0.831615 -0.072653 1.329817 11.00000 -1.20000 AFIX 0 C8 1 0.929040 -0.281058 1.356887 11.00000 0.02731 0.03726 = 0.02039 -0.00389 -0.00663 -0.00827 AFIX 43 H8 2 0.978613 -0.297035 1.432320 11.00000 -1.20000 AFIX 0 C9 1 0.945038 -0.391867 1.309029 11.00000 0.02665 0.02829 = 0.02523 0.00028 -0.00373 -0.00205 AFIX 43 H9 2 1.004593 -0.482349 1.352615 11.00000 -1.20000 AFIX 0 C10 1 0.874996 -0.371865 1.198261 11.00000 0.02543 0.02182 = 0.02421 -0.00276 -0.00014 -0.00309 AFIX 43 H10 2 0.886695 -0.446586 1.164663 11.00000 -1.20000 AFIX 0 C11 1 0.787279 -0.238817 1.138370 11.00000 0.02014 0.02242 = 0.01935 -0.00474 0.00179 -0.00582 C12 1 0.703037 -0.177068 1.019336 11.00000 0.01951 0.01786 = 0.01935 -0.00401 0.00148 -0.00465 C13 1 0.697462 -0.252763 0.942587 11.00000 0.02492 0.01556 = 0.02443 -0.00695 -0.00088 -0.00095 AFIX 43 H13 2 0.731937 -0.356952 0.976641 11.00000 -1.20000 AFIX 0 C14 1 0.643699 -0.186481 0.815426 11.00000 0.01962 0.01964 = 0.02439 -0.01111 0.00127 -0.00368 C15 1 0.586086 -0.198793 0.632972 11.00000 0.03291 0.02551 = 0.02482 -0.01234 -0.00552 -0.00519 AFIX 23 H15A 2 0.489826 -0.229005 0.636625 11.00000 -1.20000 H15B 2 0.637727 -0.215547 0.563116 11.00000 -1.20000 AFIX 0 C16 1 0.582693 -0.032880 0.614460 11.00000 0.02431 0.02510 = 0.01947 -0.01113 -0.00415 0.00124 AFIX 13 H16 2 0.491636 0.024821 0.574148 11.00000 -1.20000 AFIX 0 C17 1 0.214016 0.372117 0.935686 11.00000 0.02087 0.02959 = 0.02907 -0.01951 0.00349 -0.00287 C18 1 0.171672 0.243825 1.034323 11.00000 0.02950 0.03103 = 0.04193 -0.01848 0.00892 -0.00561 AFIX 43 H18 2 0.239071 0.161756 1.080576 11.00000 -1.20000 AFIX 0 C19 1 0.029785 0.235462 1.065557 11.00000 0.04018 0.04545 = 0.04916 -0.02796 0.01827 -0.02069 AFIX 43 H19 2 0.001035 0.146980 1.132912 11.00000 -1.20000 AFIX 0 C20 1 -0.068999 0.353489 1.000217 11.00000 0.02205 0.07035 = 0.05176 -0.04282 0.00682 -0.00523 AFIX 43 H20 2 -0.165257 0.346773 1.022855 11.00000 -1.20000 AFIX 0 C21 1 -0.028162 0.481293 0.902016 11.00000 0.02514 0.06319 = 0.04004 -0.03137 -0.00104 0.00773 AFIX 43 H21 2 -0.096167 0.563025 0.856430 11.00000 -1.20000 AFIX 0 C22 1 0.112084 0.490617 0.869745 11.00000 0.02786 0.04155 = 0.03155 -0.01959 0.00255 0.00349 AFIX 43 H22 2 0.139617 0.579097 0.801576 11.00000 -1.20000 AFIX 0 C23 1 0.705179 0.044092 0.536646 11.00000 0.03434 0.02218 = 0.02198 -0.01401 0.00249 -0.00376 C24 1 0.843283 -0.006999 0.578437 11.00000 0.03420 0.02724 = 0.03209 -0.01654 0.00507 -0.00661 AFIX 43 H24 2 0.861562 -0.090566 0.658410 11.00000 -1.20000 AFIX 0 C25 1 0.955020 0.062410 0.504909 11.00000 0.03606 0.04511 = 0.04999 -0.03363 0.01345 -0.01501 AFIX 43 H25 2 1.048922 0.026040 0.534344 11.00000 -1.20000 AFIX 0 C26 1 0.928800 0.185130 0.388256 11.00000 0.06780 0.04744 = 0.04099 -0.03051 0.02714 -0.03566 AFIX 43 H26 2 1.004688 0.233894 0.338156 11.00000 -1.20000 AFIX 0 C27 1 0.792408 0.235961 0.345384 11.00000 0.07609 0.03341 = 0.02752 -0.01570 0.01166 -0.02412 AFIX 43 H27 2 0.774522 0.319196 0.265148 11.00000 -1.20000 AFIX 0 C28 1 0.680890 0.166186 0.418826 11.00000 0.05274 0.02547 = 0.02278 -0.01361 0.00137 -0.00548 AFIX 43 H28 2 0.587245 0.202100 0.388384 11.00000 -1.20000 AFIX 0 C29 1 0.396840 0.327951 0.561863 11.00000 0.02364 0.03375 = 0.02313 -0.01105 -0.00328 0.00440 AFIX 13 H29 2 0.492824 0.297853 0.537715 11.00000 -1.20000 AFIX 0 C31 1 0.376566 0.500587 0.513129 11.00000 0.02160 0.03375 = 0.02090 -0.00710 -0.00583 0.00165 C32 1 0.268989 0.569599 0.560061 11.00000 0.02482 0.03063 = 0.03096 -0.01107 -0.00412 -0.00133 AFIX 43 H32 2 0.209943 0.508036 0.624407 11.00000 -1.20000 AFIX 0 C33 1 0.244816 0.726441 0.515766 11.00000 0.03091 0.03394 = 0.04382 -0.01715 -0.01220 0.00295 AFIX 43 H33 2 0.170996 0.772204 0.549218 11.00000 -1.20000 AFIX 0 C34 1 0.330684 0.812540 0.422588 11.00000 0.04860 0.02636 = 0.04036 -0.00525 -0.01976 -0.00412 C35 1 0.439047 0.750890 0.373011 11.00000 0.04507 0.04278 = 0.02632 0.00218 -0.00703 -0.01667 AFIX 43 H35 2 0.497612 0.813709 0.308969 11.00000 -1.20000 AFIX 0 C36 1 0.461267 0.593904 0.418771 11.00000 0.03105 0.04820 = 0.02230 -0.00721 -0.00298 -0.00170 AFIX 43 H36 2 0.535761 0.549388 0.384971 11.00000 -1.20000 AFIX 0 C37 1 0.287094 0.282531 0.492627 11.00000 0.03361 0.04100 = 0.03400 -0.01695 -0.01062 0.00668 AFIX 137 H37A 2 0.297813 0.172302 0.520537 11.00000 -1.50000 H37B 2 0.301235 0.331736 0.400242 11.00000 -1.50000 H37C 2 0.192444 0.314671 0.513075 11.00000 -1.50000 AFIX 0 C41 1 0.681343 0.398543 0.722525 11.00000 0.02946 0.01914 = 0.02981 -0.00541 0.00018 -0.00574 AFIX 23 H41A 2 0.689526 0.420404 0.798699 11.00000 -1.20000 H41B 2 0.592828 0.452171 0.676508 11.00000 -1.20000 AFIX 0 C42 1 0.806403 0.445668 0.636579 11.00000 0.03933 0.03983 = 0.03380 -0.00900 0.00979 -0.01857 AFIX 23 H42A 2 0.845406 0.532023 0.644025 11.00000 -1.20000 H42B 2 0.780336 0.474672 0.546319 11.00000 -1.20000 AFIX 0 C43 1 0.912172 0.303935 0.685387 11.00000 0.03020 0.04800 = 0.05887 -0.03650 0.02086 -0.01737 AFIX 23 H43A 2 0.944249 0.275320 0.614893 11.00000 -1.20000 H43B 2 0.994951 0.321045 0.725263 11.00000 -1.20000 AFIX 0 C44 1 0.830552 0.181413 0.783891 11.00000 0.01909 0.03306 = 0.03750 -0.02073 0.00067 -0.00117 AFIX 23 H44A 2 0.849562 0.084701 0.774301 11.00000 -1.20000 H44B 2 0.856990 0.164386 0.871649 11.00000 -1.20000 AFIX 0 PART 1 O5A 6 0.332882 -0.016534 0.916881 21.00000 0.02069 0.02930 = 0.02794 -0.01240 0.00701 -0.00928 C51A 1 0.206705 0.000298 0.845922 21.00000 0.02912 0.05089 = 0.05028 -0.01173 -0.00744 -0.01953 AFIX 23 H51A 2 0.228858 0.011545 0.757899 21.00000 -1.20000 H51B 2 0.143948 0.089698 0.841940 21.00000 -1.20000 AFIX 0 C52A 1 0.138709 -0.146120 0.920625 21.00000 0.02482 0.03255 = 0.08337 -0.02601 -0.00504 -0.00844 AFIX 23 H52A 2 0.035740 -0.131364 0.906348 21.00000 -1.20000 H52B 2 0.179630 -0.229207 0.897669 21.00000 -1.20000 AFIX 0 C53A 1 0.174472 -0.176269 1.054357 21.00000 0.02545 0.06730 = 0.07560 -0.00450 0.01037 -0.02443 AFIX 23 H53A 2 0.173419 -0.285176 1.110836 21.00000 -1.20000 H53B 2 0.107401 -0.116525 1.087246 21.00000 -1.20000 AFIX 0 C54A 1 0.321457 -0.127366 1.046092 21.00000 0.02060 0.02965 = 0.03457 -0.00927 0.00830 0.00199 AFIX 23 H54A 2 0.333796 -0.082355 1.107712 21.00000 -1.20000 H54B 2 0.393235 -0.214726 1.064230 21.00000 -1.20000 AFIX 0 PART 0 PART 2 O5B 6 0.346914 -0.034417 0.911704 -21.00000 0.01915 0.03205 = 0.02344 -0.01225 0.00129 -0.00620 C51B 1 0.229098 -0.048840 0.844994 -21.00000 0.03753 0.04808 = 0.04481 -0.01850 -0.00792 -0.01755 AFIX 23 H51C 2 0.253329 -0.125982 0.810364 -21.00000 -1.20000 H51D 2 0.198340 0.049031 0.773729 -21.00000 -1.20000 AFIX 0 C52B 1 0.114969 -0.097395 0.944551 -21.00000 0.02751 0.05111 = 0.06216 -0.01946 0.00306 -0.01304 AFIX 23 H52C 2 0.059359 -0.008435 0.949641 -21.00000 -1.20000 H52D 2 0.050981 -0.159027 0.925192 -21.00000 -1.20000 AFIX 0 C53B 1 0.195234 -0.188994 1.065212 -21.00000 0.02581 0.05076 = 0.04555 -0.00727 0.01145 -0.00503 AFIX 23 H53C 2 0.194625 -0.298515 1.087101 -21.00000 -1.20000 H53D 2 0.153087 -0.167344 1.136451 -21.00000 -1.20000 AFIX 0 C54B 1 0.343682 -0.144283 1.041758 -21.00000 0.02166 0.02510 = 0.02995 -0.00542 0.01329 -0.00279 AFIX 23 H54C 2 0.368647 -0.099935 1.100897 -21.00000 -1.20000 H54D 2 0.411187 -0.233790 1.054867 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ga_vv35 - #3197 - in P1 - superflip - nova REM wR2 = 0.0631, GooF = S = 1.035, Restrained GooF = 1.031 for all data REM R1 = 0.0256 for 6573 Fo > 4sig(Fo) and 0.0271 for all 6787 data REM 534 parameters refined using 121 restraints END WGHT 0.0329 0.1299 REM Instructions for potential hydrogen bonds EQIV $1 x, y+1, z HTAB C2 O2_$1 REM Highest difference peak 0.116, deepest hole -0.149, 1-sigma level 0.028 Q1 1 0.7975 -0.1804 1.1590 11.00000 0.05 0.12 Q2 1 0.7643 -0.1990 1.1816 11.00000 0.05 0.11 Q3 1 0.4575 0.1829 0.9051 11.00000 0.05 0.11 Q4 1 0.6028 0.1915 1.0590 11.00000 0.05 0.10 Q5 1 0.6461 0.0123 0.5726 11.00000 0.05 0.10 Q6 1 0.0417 -0.0755 1.1819 11.00000 0.05 0.10 Q7 1 0.5547 -0.0379 1.0005 11.00000 0.05 0.10 Q8 1 0.5783 0.4987 0.3606 11.00000 0.05 0.10 Q9 1 0.8346 -0.1193 0.5191 11.00000 0.05 0.10 Q10 1 0.5896 -0.1140 0.6151 11.00000 0.05 0.09 Q11 1 0.4610 0.1978 0.7317 11.00000 0.05 0.09 Q12 1 0.8259 -0.1252 1.2201 11.00000 0.05 0.09 Q13 1 0.3914 0.4394 0.9386 11.00000 0.05 0.09 Q14 1 0.6928 0.1061 0.4929 11.00000 0.05 0.09 Q15 1 0.7833 -0.3254 0.9508 11.00000 0.05 0.09 Q16 1 0.5514 -0.1245 0.7903 11.00000 0.05 0.09 Q17 1 0.5686 0.0148 0.7810 11.00000 0.05 0.09 Q18 1 1.0476 -0.6159 1.3414 11.00000 0.05 0.09 Q19 1 0.6415 -0.2174 0.8944 11.00000 0.05 0.09 Q20 1 0.4214 0.4049 0.3505 11.00000 0.05 0.09 Q21 1 0.2989 0.6382 0.5755 11.00000 0.05 0.09 Q22 1 -0.0430 0.0665 0.9893 11.00000 0.05 0.09 Q23 1 0.1704 -0.0631 1.1226 11.00000 0.05 0.09 Q24 1 0.5139 0.5975 0.6543 11.00000 0.05 0.09 Q25 1 0.1391 -0.4131 1.1997 11.00000 0.05 0.09 ; _cod_data_source_file c9cc09111d2.cif _cod_data_source_block ga_vv35 _cod_depositor_comments 'Adding full bibliography for 7125679--7125681.cif.' _cod_database_code 7125681 _audit_block_refno 3197 _audit_block_usercomment 'VV636, irregular, bronze' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.921 _shelx_estimated_absorpt_t_min 0.921 _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _shelxl_version_number 2018/3 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O5A-C51A \\sim O5A-C54A \\sim O5B-C51B \\sim O5B-C54B with sigma of 0.01 C51A-C52A \\sim C53A-C54A \\sim C51B-C52B \\sim C53B-C54B with sigma of 0.01 C52A-C53A \\sim C52B-C53B with sigma of 0.01 C51A-C53A \\sim C54A-C52A \\sim C51B-C53B \\sim C54B-C52B with sigma of 0.02 O5A-C52A \\sim O5B-C52B \\sim O5A-C53A \\sim O5B-C53B with sigma of 0.02 Mg-O5A \\sim Mg-O5B \\sim Mg-O4 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C51A \\sim C52A \\sim C53A \\sim C54A \\sim C51B \\sim C52B \\sim C53B \\sim C54B \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5A \\sim O5B: within 1A with sigma of 0.01 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains O5A, C51A, C52A, C53A, C54A, O5B, C51B, C52B, C53B, C54B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O5B)=Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)= Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(C54B)=Sof(H54C)=Sof(H54D)=1-FVAR(1) Sof(O5A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)= Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=Sof(H54B)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C1(H1), C16(H16), C29(H29) 6.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C15(H15A,H15B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C51A(H51A,H51B), C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A, H54B), C51B(H51C,H51D), C52B(H52C,H52D), C53B(H53C,H53D), C54B(H54C,H54D) 6.c Aromatic/amide H refined with riding coordinates: C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C35(H35), C36(H36) 6.d Idealised Me refined as rotating group: C37(H37A,H37B,H37C) ; _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.189 _oxdiff_exptl_absorpt_empirical_full_min 0.855 _shelx_res_checksum 47635 _cell_oxdiff_length_a 9.5675(4) _cell_oxdiff_length_b 9.7347(4) _cell_oxdiff_length_c 11.4970(3) _cell_oxdiff_angle_alpha 65.664(3) _cell_oxdiff_angle_beta 88.065(3) _cell_oxdiff_angle_gamma 84.019(3) _cell_oxdiff_volume 970.28(6) _cell_oxdiff_measurement_reflns_used 16003 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.50608(7) 0.11491(7) 0.83090(6) 0.01808(14) Uani 1 1 d D . . . . F F 0.3083(2) 0.96707(17) 0.37902(18) 0.0648(5) Uani 1 1 d . . . . . O1 O 0.51472(17) 0.36362(17) 1.07199(15) 0.0305(3) Uani 1 1 d . U . . . O2 O 0.65902(16) -0.28162(15) 0.75387(13) 0.0250(3) Uani 1 1 d . U . . . O3 O 0.38376(15) 0.25510(16) 0.69232(13) 0.0258(3) Uani 1 1 d . U . . . O4 O 0.68512(14) 0.23832(15) 0.75822(13) 0.0227(3) Uani 1 1 d D U . . . N1 N 0.45927(17) 0.25132(18) 0.94457(15) 0.0212(4) Uani 1 1 d . . . . . N2 N 0.63794(17) -0.03657(18) 0.99808(15) 0.0193(3) Uani 1 1 d . . . . . N3 N 0.59169(18) -0.04891(18) 0.74858(14) 0.0201(3) Uani 1 1 d . . . . . C1 C 0.3667(2) 0.3945(2) 0.9018(2) 0.0236(4) Uani 1 1 d . U . . . H1 H 0.375339 0.452296 0.807467 0.028 Uiso 1 1 calc R . . . . C2 C 0.4282(2) 0.4800(2) 0.9720(2) 0.0305(5) Uani 1 1 d . U . . . H2A H 0.485085 0.559403 0.913682 0.037 Uiso 1 1 calc R . . . . H2B H 0.352492 0.527506 1.008192 0.037 Uiso 1 1 calc R . . . . C3 C 0.5323(2) 0.2426(2) 1.03968(19) 0.0225(4) Uani 1 1 d . U . . . C4 C 0.6306(2) 0.1214(2) 1.11858(18) 0.0242(4) Uani 1 1 d . U . . . H4 H 0.668100 0.129279 1.190838 0.029 Uiso 1 1 calc R . . . . C5 C 0.6746(2) -0.0039(2) 1.09831(17) 0.0208(4) Uani 1 1 d . U . . . C6 C 0.7715(2) -0.1285(2) 1.18631(18) 0.0223(4) Uani 1 1 d . U . . . C7 C 0.8424(2) -0.1480(2) 1.29684(19) 0.0274(5) Uani 1 1 d . U . . . H7 H 0.831615 -0.072653 1.329817 0.033 Uiso 1 1 calc R . . . . C8 C 0.9290(2) -0.2811(3) 1.3569(2) 0.0304(5) Uani 1 1 d . U . . . H8 H 0.978613 -0.297035 1.432320 0.036 Uiso 1 1 calc R . . . . C9 C 0.9450(2) -0.3919(2) 1.3090(2) 0.0304(5) Uani 1 1 d . U . . . H9 H 1.004593 -0.482349 1.352615 0.037 Uiso 1 1 calc R . . . . C10 C 0.8750(2) -0.3719(2) 1.19826(19) 0.0260(4) Uani 1 1 d . U . . . H10 H 0.886695 -0.446586 1.164663 0.031 Uiso 1 1 calc R . . . . C11 C 0.7873(2) -0.2388(2) 1.13837(18) 0.0217(4) Uani 1 1 d . U . . . C12 C 0.7030(2) -0.1771(2) 1.01934(18) 0.0199(4) Uani 1 1 d . U . . . C13 C 0.6975(2) -0.2528(2) 0.94259(19) 0.0221(4) Uani 1 1 d . U . . . H13 H 0.731937 -0.356952 0.976641 0.027 Uiso 1 1 calc R . . . . C14 C 0.6437(2) -0.1865(2) 0.81543(18) 0.0204(4) Uani 1 1 d . U . . . C15 C 0.5861(2) -0.1988(2) 0.6330(2) 0.0268(5) Uani 1 1 d . U . . . H15A H 0.489826 -0.229005 0.636625 0.032 Uiso 1 1 calc R . . . . H15B H 0.637727 -0.215547 0.563116 0.032 Uiso 1 1 calc R . . . . C16 C 0.5827(2) -0.0329(2) 0.61446(18) 0.0225(4) Uani 1 1 d . U . . . H16 H 0.491636 0.024821 0.574148 0.027 Uiso 1 1 calc R . . . . C17 C 0.2140(2) 0.3721(2) 0.9357(2) 0.0241(4) Uani 1 1 d . U . . . C18 C 0.1717(3) 0.2438(3) 1.0343(2) 0.0330(5) Uani 1 1 d . U . . . H18 H 0.239071 0.161756 1.080576 0.040 Uiso 1 1 calc R . . . . C19 C 0.0298(3) 0.2355(3) 1.0656(3) 0.0413(6) Uani 1 1 d . U . . . H19 H 0.001035 0.146980 1.132912 0.050 Uiso 1 1 calc R . . . . C20 C -0.0690(3) 0.3535(3) 1.0002(3) 0.0423(6) Uani 1 1 d . U . . . H20 H -0.165257 0.346773 1.022855 0.051 Uiso 1 1 calc R . . . . C21 C -0.0282(3) 0.4813(3) 0.9020(2) 0.0403(6) Uani 1 1 d . U . . . H21 H -0.096167 0.563025 0.856430 0.048 Uiso 1 1 calc R . . . . C22 C 0.1121(3) 0.4906(3) 0.8697(2) 0.0327(5) Uani 1 1 d . U . . . H22 H 0.139617 0.579097 0.801576 0.039 Uiso 1 1 calc R . . . . C23 C 0.7052(2) 0.0441(2) 0.53665(19) 0.0245(4) Uani 1 1 d . U . . . C24 C 0.8433(3) -0.0070(3) 0.5784(2) 0.0296(5) Uani 1 1 d . U . . . H24 H 0.861562 -0.090566 0.658410 0.035 Uiso 1 1 calc R . . . . C25 C 0.9550(3) 0.0624(3) 0.5049(2) 0.0385(6) Uani 1 1 d . U . . . H25 H 1.048922 0.026040 0.534344 0.046 Uiso 1 1 calc R . . . . C26 C 0.9288(3) 0.1851(3) 0.3883(2) 0.0463(7) Uani 1 1 d . U . . . H26 H 1.004688 0.233894 0.338156 0.056 Uiso 1 1 calc R . . . . C27 C 0.7924(3) 0.2360(3) 0.3454(2) 0.0435(7) Uani 1 1 d . U . . . H27 H 0.774522 0.319196 0.265148 0.052 Uiso 1 1 calc R . . . . C28 C 0.6809(3) 0.1662(2) 0.4188(2) 0.0323(5) Uani 1 1 d . U . . . H28 H 0.587245 0.202100 0.388384 0.039 Uiso 1 1 calc R . . . . C29 C 0.3968(2) 0.3280(2) 0.56186(19) 0.0275(5) Uani 1 1 d . U . . . H29 H 0.492824 0.297853 0.537715 0.033 Uiso 1 1 calc R . . . . C31 C 0.3766(2) 0.5006(2) 0.51313(19) 0.0270(5) Uani 1 1 d . U . . . C32 C 0.2690(2) 0.5696(2) 0.5601(2) 0.0293(5) Uani 1 1 d . U . . . H32 H 0.209943 0.508036 0.624407 0.035 Uiso 1 1 calc R . . . . C33 C 0.2448(3) 0.7264(3) 0.5158(2) 0.0360(5) Uani 1 1 d . U . . . H33 H 0.170996 0.772204 0.549218 0.043 Uiso 1 1 calc R . . . . C34 C 0.3307(3) 0.8125(3) 0.4226(2) 0.0407(6) Uani 1 1 d . U . . . C35 C 0.4390(3) 0.7509(3) 0.3730(2) 0.0424(6) Uani 1 1 d . U . . . H35 H 0.497612 0.813709 0.308969 0.051 Uiso 1 1 calc R . . . . C36 C 0.4613(3) 0.5939(3) 0.4188(2) 0.0364(5) Uani 1 1 d . U . . . H36 H 0.535761 0.549388 0.384971 0.044 Uiso 1 1 calc R . . . . C37 C 0.2871(3) 0.2825(3) 0.4926(2) 0.0362(5) Uani 1 1 d . U . . . H37A H 0.297813 0.172302 0.520537 0.054 Uiso 1 1 calc GR . . . . H37B H 0.301235 0.331736 0.400242 0.054 Uiso 1 1 calc GR . . . . H37C H 0.192444 0.314671 0.513075 0.054 Uiso 1 1 calc GR . . . . C41 C 0.6813(2) 0.3985(2) 0.7225(2) 0.0274(5) Uani 1 1 d . U . . . H41A H 0.689526 0.420404 0.798699 0.033 Uiso 1 1 calc R . . . . H41B H 0.592828 0.452171 0.676508 0.033 Uiso 1 1 calc R . . . . C42 C 0.8064(3) 0.4457(3) 0.6366(2) 0.0388(6) Uani 1 1 d . U . . . H42A H 0.845406 0.532023 0.644025 0.047 Uiso 1 1 calc R . . . . H42B H 0.780336 0.474672 0.546319 0.047 Uiso 1 1 calc R . . . . C43 C 0.9122(3) 0.3039(3) 0.6854(3) 0.0403(6) Uani 1 1 d . U . . . H43A H 0.944249 0.275320 0.614893 0.048 Uiso 1 1 calc R . . . . H43B H 0.994951 0.321045 0.725263 0.048 Uiso 1 1 calc R . . . . C44 C 0.8306(2) 0.1814(3) 0.7839(2) 0.0279(5) Uani 1 1 d . U . . . H44A H 0.849562 0.084701 0.774301 0.034 Uiso 1 1 calc R . . . . H44B H 0.856990 0.164386 0.871649 0.034 Uiso 1 1 calc R . . . . O5A O 0.3329(19) -0.017(3) 0.9169(17) 0.025(3) Uani 0.518(16) 1 d D U P A 1 C51A C 0.2067(13) 0.0003(12) 0.8459(11) 0.045(3) Uani 0.518(16) 1 d D U P A 1 H51A H 0.228858 0.011545 0.757899 0.054 Uiso 0.518(16) 1 calc R . P A 1 H51B H 0.143948 0.089698 0.841940 0.054 Uiso 0.518(16) 1 calc R . P A 1 C52A C 0.1387(9) -0.1461(9) 0.9206(9) 0.046(2) Uani 0.518(16) 1 d D U P A 1 H52A H 0.035740 -0.131364 0.906348 0.055 Uiso 0.518(16) 1 calc R . P A 1 H52B H 0.179630 -0.229207 0.897669 0.055 Uiso 0.518(16) 1 calc R . P A 1 C53A C 0.174(2) -0.176(3) 1.0544(11) 0.063(4) Uani 0.518(16) 1 d D U P A 1 H53A H 0.173419 -0.285176 1.110836 0.076 Uiso 0.518(16) 1 calc R . P A 1 H53B H 0.107401 -0.116525 1.087246 0.076 Uiso 0.518(16) 1 calc R . P A 1 C54A C 0.3215(17) -0.127(3) 1.0461(16) 0.030(3) Uani 0.518(16) 1 d D U P A 1 H54A H 0.333796 -0.082355 1.107712 0.036 Uiso 0.518(16) 1 calc R . P A 1 H54B H 0.393235 -0.214726 1.064230 0.036 Uiso 0.518(16) 1 calc R . P A 1 O5B O 0.347(2) -0.034(3) 0.9117(18) 0.024(3) Uani 0.482(16) 1 d D U P A 2 C51B C 0.2291(13) -0.0488(15) 0.8450(11) 0.042(3) Uani 0.482(16) 1 d D U P A 2 H51C H 0.253329 -0.125982 0.810364 0.051 Uiso 0.482(16) 1 calc R . P A 2 H51D H 0.198340 0.049031 0.773729 0.051 Uiso 0.482(16) 1 calc R . P A 2 C52B C 0.1150(8) -0.0974(14) 0.9446(8) 0.048(2) Uani 0.482(16) 1 d D U P A 2 H52C H 0.059359 -0.008435 0.949641 0.057 Uiso 0.482(16) 1 calc R . P A 2 H52D H 0.050981 -0.159027 0.925192 0.057 Uiso 0.482(16) 1 calc R . P A 2 C53B C 0.1952(17) -0.189(2) 1.0652(9) 0.045(3) Uani 0.482(16) 1 d D U P A 2 H53C H 0.194625 -0.298515 1.087101 0.054 Uiso 0.482(16) 1 calc R . P A 2 H53D H 0.153087 -0.167344 1.136451 0.054 Uiso 0.482(16) 1 calc R . P A 2 C54B C 0.3437(16) -0.144(3) 1.0418(16) 0.028(3) Uani 0.482(16) 1 d D U P A 2 H54C H 0.368647 -0.099935 1.100897 0.033 Uiso 0.482(16) 1 calc R . P A 2 H54D H 0.411187 -0.233790 1.054867 0.033 Uiso 0.482(16) 1 calc R . 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 Mg 0.0172(3) 0.0186(3) 0.0178(3) -0.0069(2) 0.0000(2) -0.0020(2) F 0.0833(13) 0.0274(7) 0.0711(11) -0.0053(7) -0.0235(10) -0.0075(8) O1 0.0358(9) 0.0254(8) 0.0360(8) -0.0188(7) -0.0036(7) 0.0000(6) O2 0.0323(8) 0.0205(7) 0.0253(7) -0.0123(6) -0.0030(6) -0.0028(6) O3 0.0250(8) 0.0272(7) 0.0206(7) -0.0061(6) -0.0030(6) 0.0021(6) O4 0.0182(7) 0.0206(7) 0.0289(7) -0.0096(6) 0.0025(6) -0.0034(6) N1 0.0185(9) 0.0211(8) 0.0229(8) -0.0084(7) 0.0025(7) -0.0010(7) N2 0.0201(9) 0.0194(8) 0.0190(8) -0.0081(6) 0.0000(7) -0.0034(7) N3 0.0214(9) 0.0212(8) 0.0174(8) -0.0076(6) -0.0016(6) -0.0019(7) C1 0.0211(11) 0.0199(10) 0.0286(10) -0.0092(8) 0.0033(8) -0.0008(8) C2 0.0260(12) 0.0234(11) 0.0443(13) -0.0161(10) -0.0009(10) -0.0014(9) C3 0.0248(11) 0.0222(10) 0.0236(10) -0.0121(8) 0.0045(8) -0.0051(8) C4 0.0269(11) 0.0281(10) 0.0198(9) -0.0113(8) -0.0024(8) -0.0047(9) C5 0.0219(11) 0.0232(9) 0.0171(9) -0.0069(7) 0.0003(7) -0.0072(8) C6 0.0207(11) 0.0248(10) 0.0192(9) -0.0059(8) 0.0010(8) -0.0068(8) C7 0.0292(12) 0.0317(11) 0.0213(10) -0.0092(9) -0.0010(8) -0.0097(9) C8 0.0273(12) 0.0373(12) 0.0204(10) -0.0039(9) -0.0066(8) -0.0083(10) C9 0.0267(12) 0.0283(11) 0.0252(10) 0.0003(9) -0.0037(9) -0.0020(9) C10 0.0254(11) 0.0218(10) 0.0242(10) -0.0028(8) -0.0001(8) -0.0031(8) C11 0.0201(10) 0.0224(10) 0.0194(9) -0.0047(8) 0.0018(8) -0.0058(8) C12 0.0195(10) 0.0179(9) 0.0193(9) -0.0040(7) 0.0015(7) -0.0046(8) C13 0.0249(11) 0.0156(9) 0.0244(10) -0.0069(8) -0.0009(8) -0.0010(8) C14 0.0196(10) 0.0196(9) 0.0244(10) -0.0111(8) 0.0013(8) -0.0037(8) C15 0.0329(12) 0.0255(10) 0.0248(10) -0.0123(9) -0.0055(9) -0.0052(9) C16 0.0243(11) 0.0251(10) 0.0195(9) -0.0111(8) -0.0042(8) 0.0012(8) C17 0.0209(11) 0.0296(11) 0.0291(10) -0.0195(9) 0.0035(8) -0.0029(8) C18 0.0295(13) 0.0310(12) 0.0419(13) -0.0185(10) 0.0089(10) -0.0056(10) C19 0.0402(15) 0.0455(14) 0.0492(14) -0.0280(12) 0.0183(12) -0.0207(12) C20 0.0221(12) 0.0704(18) 0.0518(15) -0.0428(15) 0.0068(11) -0.0052(12) C21 0.0251(13) 0.0632(17) 0.0400(13) -0.0314(13) -0.0010(10) 0.0077(12) C22 0.0279(12) 0.0416(13) 0.0316(11) -0.0196(10) 0.0026(9) 0.0035(10) C23 0.0343(12) 0.0222(10) 0.0220(10) -0.0140(8) 0.0025(8) -0.0038(9) C24 0.0342(13) 0.0272(11) 0.0321(11) -0.0165(9) 0.0051(9) -0.0066(9) C25 0.0361(14) 0.0451(14) 0.0500(15) -0.0336(12) 0.0135(11) -0.0150(11) C26 0.068(2) 0.0474(15) 0.0410(14) -0.0305(12) 0.0271(14) -0.0357(15) C27 0.076(2) 0.0334(13) 0.0275(11) -0.0157(10) 0.0117(12) -0.0241(13) C28 0.0527(15) 0.0255(11) 0.0228(10) -0.0136(9) 0.0014(10) -0.0055(10) C29 0.0236(11) 0.0337(11) 0.0231(10) -0.0110(9) -0.0033(8) 0.0044(9) C31 0.0216(11) 0.0338(11) 0.0209(9) -0.0071(8) -0.0058(8) 0.0017(9) C32 0.0248(12) 0.0306(11) 0.0310(11) -0.0111(9) -0.0041(9) -0.0013(9) C33 0.0309(13) 0.0339(12) 0.0438(13) -0.0172(10) -0.0122(10) 0.0030(10) C34 0.0486(16) 0.0264(11) 0.0404(13) -0.0052(10) -0.0198(12) -0.0041(11) C35 0.0451(15) 0.0428(13) 0.0263(11) 0.0022(10) -0.0070(10) -0.0167(12) C36 0.0311(13) 0.0482(14) 0.0223(10) -0.0072(10) -0.0030(9) -0.0017(11) C37 0.0336(13) 0.0410(13) 0.0340(12) -0.0169(10) -0.0106(10) 0.0067(10) C41 0.0295(12) 0.0191(10) 0.0298(10) -0.0054(8) 0.0002(9) -0.0057(9) C42 0.0393(14) 0.0398(14) 0.0338(12) -0.0090(11) 0.0098(11) -0.0186(11) C43 0.0302(14) 0.0480(15) 0.0589(16) -0.0365(13) 0.0209(12) -0.0174(11) C44 0.0191(11) 0.0331(11) 0.0375(12) -0.0207(10) 0.0007(9) -0.0012(9) O5A 0.021(4) 0.029(5) 0.028(3) -0.012(3) 0.007(2) -0.009(4) C51A 0.029(4) 0.051(6) 0.050(3) -0.012(4) -0.007(3) -0.020(4) C52A 0.025(3) 0.033(4) 0.083(5) -0.026(3) -0.005(3) -0.008(3) C53A 0.025(5) 0.067(7) 0.076(6) -0.005(5) 0.010(4) -0.024(5) C54A 0.021(5) 0.030(5) 0.035(4) -0.009(3) 0.008(3) 0.002(4) O5B 0.019(4) 0.032(6) 0.023(3) -0.012(3) 0.001(3) -0.006(4) C51B 0.038(5) 0.048(6) 0.045(3) -0.019(4) -0.008(3) -0.018(5) C52B 0.028(4) 0.051(5) 0.062(4) -0.019(4) 0.003(3) -0.013(3) C53B 0.026(5) 0.051(5) 0.046(4) -0.007(4) 0.011(3) -0.005(4) C54B 0.022(5) 0.025(5) 0.030(3) -0.005(3) 0.013(3) -0.003(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 4 3 -2 0.0233 -4 2 -4 0.0413 1 -1 -7 0.0491 -3 5 2 0.0366 -3 2 6 0.0453 6 0 -3 0.0289 1 0 7 0.0633 -1 -6 -5 0.0575 -3 -6 -1 0.0444 5 -2 2 0.0442 6 1 0 0.0298 0 6 5 0.0428 5 -3 1 0.0472 -5 3 1 0.0330 -2 6 4 0.0384 3 6 2 0.0333 3 3 -3 0.0214 6 0 1 0.0320 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O3 Mg O4 93.51(6) O3 Mg N1 91.81(6) O3 Mg N2 175.64(7) O3 Mg N3 100.69(6) O3 Mg O5A 90.2(5) O3 Mg O5B 92.8(5) O4 Mg N1 87.65(6) O4 Mg N2 87.42(6) O4 Mg N3 88.82(6) O4 Mg O5A 176.0(4) N1 Mg N3 167.20(6) N2 Mg N1 83.98(6) N2 Mg N3 83.58(6) O5A Mg N1 90.8(9) O5A Mg N2 88.8(5) O5A Mg N3 91.9(9) O5B Mg O4 172.4(8) O5B Mg N1 96.5(9) O5B Mg N2 86.7(5) O5B Mg N3 85.8(10) C3 O1 C2 105.75(15) C14 O2 C15 105.16(15) C29 O3 Mg 134.83(14) C41 O4 Mg 122.80(13) C44 O4 Mg 127.27(12) C44 O4 C41 105.27(15) C1 N1 Mg 124.71(12) C3 N1 Mg 125.79(14) C3 N1 C1 107.30(16) C5 N2 Mg 126.08(13) C12 N2 Mg 126.80(12) C12 N2 C5 107.07(16) C14 N3 Mg 124.50(13) C14 N3 C16 106.43(16) C16 N3 Mg 128.53(12) N1 C1 H1 109.7 N1 C1 C2 102.99(16) N1 C1 C17 113.40(16) C2 C1 H1 109.7 C17 C1 H1 109.7 C17 C1 C2 111.01(18) O1 C2 C1 103.99(16) O1 C2 H2A 111.0 O1 C2 H2B 111.0 C1 C2 H2A 111.0 C1 C2 H2B 111.0 H2A C2 H2B 109.0 O1 C3 C4 114.44(17) N1 C3 O1 116.95(19) N1 C3 C4 128.62(18) C3 C4 H4 117.5 C5 C4 C3 125.09(17) C5 C4 H4 117.5 N2 C5 C6 110.00(17) C4 C5 N2 127.37(19) C4 C5 C6 122.63(17) C7 C6 C5 132.5(2) C11 C6 C5 106.42(16) C11 C6 C7 121.1(2) C6 C7 H7 121.2 C8 C7 C6 117.6(2) C8 C7 H7 121.2 C7 C8 H8 119.3 C7 C8 C9 121.42(19) C9 C8 H8 119.3 C8 C9 H9 119.6 C10 C9 C8 120.9(2) C10 C9 H9 119.6 C9 C10 H10 121.1 C11 C10 C9 117.8(2) C11 C10 H10 121.1 C6 C11 C10 121.24(18) C6 C11 C12 105.96(17) C10 C11 C12 132.71(19) N2 C12 C11 110.51(16) C13 C12 N2 126.82(18) C13 C12 C11 122.65(19) C12 C13 H13 117.7 C12 C13 C14 124.61(18) C14 C13 H13 117.7 O2 C14 C13 114.06(17) N3 C14 O2 116.44(16) N3 C14 C13 129.34(17) O2 C15 H15A 111.1 O2 C15 H15B 111.1 O2 C15 C16 103.29(15) H15A C15 H15B 109.1 C16 C15 H15A 111.1 C16 C15 H15B 111.1 N3 C16 C15 101.85(15) N3 C16 H16 110.4 N3 C16 C23 111.20(15) C15 C16 H16 110.4 C23 C16 C15 112.44(17) C23 C16 H16 110.4 C18 C17 C1 123.0(2) C18 C17 C22 118.6(2) C22 C17 C1 118.29(19) C17 C18 H18 120.1 C17 C18 C19 119.8(2) C19 C18 H18 120.1 C18 C19 H19 119.6 C20 C19 C18 120.9(2) C20 C19 H19 119.6 C19 C20 H20 120.1 C19 C20 C21 119.8(2) C21 C20 H20 120.1 C20 C21 H21 120.1 C20 C21 C22 119.8(3) C22 C21 H21 120.1 C17 C22 H22 119.4 C21 C22 C17 121.1(2) C21 C22 H22 119.4 C24 C23 C16 121.46(18) C24 C23 C28 118.5(2) C28 C23 C16 120.0(2) C23 C24 H24 119.5 C25 C24 C23 121.0(2) C25 C24 H24 119.5 C24 C25 H25 120.1 C26 C25 C24 119.7(3) C26 C25 H25 120.1 C25 C26 H26 120.1 C27 C26 C25 119.8(2) C27 C26 H26 120.1 C26 C27 H27 119.8 C26 C27 C28 120.4(2) C28 C27 H27 119.8 C23 C28 H28 119.7 C27 C28 C23 120.6(3) C27 C28 H28 119.7 O3 C29 H29 108.6 O3 C29 C31 112.92(18) O3 C29 C37 110.86(19) C31 C29 H29 108.6 C31 C29 C37 107.08(17) C37 C29 H29 108.6 C32 C31 C29 120.24(19) C32 C31 C36 117.7(2) C36 C31 C29 122.1(2) C31 C32 H32 119.0 C31 C32 C33 122.0(2) C33 C32 H32 119.0 C32 C33 H33 121.1 C34 C33 C32 117.9(2) C34 C33 H33 121.1 C33 C34 F 118.3(3) C33 C34 C35 122.8(2) C35 C34 F 118.9(2) C34 C35 H35 120.8 C34 C35 C36 118.3(2) C36 C35 H35 120.8 C31 C36 H36 119.3 C35 C36 C31 121.4(2) C35 C36 H36 119.3 C29 C37 H37A 109.5 C29 C37 H37B 109.5 C29 C37 H37C 109.5 H37A C37 H37B 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 O4 C41 H41A 110.9 O4 C41 H41B 110.9 O4 C41 C42 104.48(19) H41A C41 H41B 108.9 C42 C41 H41A 110.9 C42 C41 H41B 110.9 C41 C42 H42A 111.0 C41 C42 H42B 111.0 C41 C42 C43 103.91(18) H42A C42 H42B 109.0 C43 C42 H42A 111.0 C43 C42 H42B 111.0 C42 C43 H43A 110.9 C42 C43 H43B 110.9 H43A C43 H43B 108.9 C44 C43 C42 104.37(19) C44 C43 H43A 110.9 C44 C43 H43B 110.9 O4 C44 C43 105.26(19) O4 C44 H44A 110.7 O4 C44 H44B 110.7 C43 C44 H44A 110.7 C43 C44 H44B 110.7 H44A C44 H44B 108.8 C51A O5A Mg 121.5(9) C51A O5A C54A 110.3(7) C54A O5A Mg 128.2(10) O5A C51A H51A 110.9 O5A C51A H51B 110.9 O5A C51A C52A 104.2(8) H51A C51A H51B 108.9 C52A C51A H51A 110.9 C52A C51A H51B 110.9 C51A C52A H52A 111.5 C51A C52A H52B 111.5 H52A C52A H52B 109.3 C53A C52A C51A 101.5(8) C53A C52A H52A 111.5 C53A C52A H52B 111.5 C52A C53A H53A 110.9 C52A C53A H53B 110.9 C52A C53A C54A 104.2(9) H53A C53A H53B 108.9 C54A C53A H53A 110.9 C54A C53A H53B 110.9 O5A C54A C53A 105.0(7) O5A C54A H54A 110.7 O5A C54A H54B 110.7 C53A C54A H54A 110.7 C53A C54A H54B 110.7 H54A C54A H54B 108.8 C51B O5B Mg 126.3(10) C51B O5B C54B 108.1(9) C54B O5B Mg 125.5(10) O5B C51B H51C 110.8 O5B C51B H51D 110.8 O5B C51B C52B 104.9(9) H51C C51B H51D 108.8 C52B C51B H51C 110.8 C52B C51B H51D 110.8 C51B C52B H52C 111.1 C51B C52B H52D 111.1 H52C C52B H52D 109.1 C53B C52B C51B 103.4(8) C53B C52B H52C 111.1 C53B C52B H52D 111.1 C52B C53B H53C 110.4 C52B C53B H53D 110.4 C52B C53B C54B 106.5(7) H53C C53B H53D 108.6 C54B C53B H53C 110.4 C54B C53B H53D 110.4 O5B C54B C53B 106.4(8) O5B C54B H54C 110.5 O5B C54B H54D 110.5 C53B C54B H54C 110.5 C53B C54B H54D 110.5 H54C C54B H54D 108.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mg O3 1.9420(15) Mg O4 2.1402(15) Mg N1 2.2222(18) Mg N2 2.2137(17) Mg N3 2.2426(18) Mg O5A 2.156(9) Mg O5B 2.133(11) F C34 1.371(3) O1 C2 1.444(3) O1 C3 1.367(2) O2 C14 1.373(2) O2 C15 1.447(2) O3 C29 1.377(2) O4 C41 1.437(2) O4 C44 1.436(3) N1 C1 1.475(3) N1 C3 1.286(3) N2 C5 1.380(2) N2 C12 1.369(3) N3 C14 1.292(3) N3 C16 1.489(2) C1 H1 1.0000 C1 C2 1.542(3) C1 C17 1.514(3) C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.430(3) C4 H4 0.9500 C4 C5 1.357(3) C5 C6 1.474(3) C6 C7 1.394(3) C6 C11 1.388(3) C7 H7 0.9500 C7 C8 1.386(3) C8 H8 0.9500 C8 C9 1.392(3) C9 H9 0.9500 C9 C10 1.391(3) C10 H10 0.9500 C10 C11 1.390(3) C11 C12 1.476(3) C12 C13 1.368(3) C13 H13 0.9500 C13 C14 1.422(3) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.537(3) C16 H16 1.0000 C16 C23 1.515(3) C17 C18 1.385(3) C17 C22 1.397(3) C18 H18 0.9500 C18 C19 1.394(3) C19 H19 0.9500 C19 C20 1.374(4) C20 H20 0.9500 C20 C21 1.374(4) C21 H21 0.9500 C21 C22 1.382(3) C22 H22 0.9500 C23 C24 1.390(3) C23 C28 1.392(3) C24 H24 0.9500 C24 C25 1.390(3) C25 H25 0.9500 C25 C26 1.389(4) C26 H26 0.9500 C26 C27 1.378(4) C27 H27 0.9500 C27 C28 1.389(4) C28 H28 0.9500 C29 H29 1.0000 C29 C31 1.529(3) C29 C37 1.541(3) C31 C32 1.385(3) C31 C36 1.393(3) C32 H32 0.9500 C32 C33 1.392(3) C33 H33 0.9500 C33 C34 1.367(4) C34 C35 1.368(4) C35 H35 0.9500 C35 C36 1.391(4) C36 H36 0.9500 C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.510(3) C42 H42A 0.9900 C42 H42B 0.9900 C42 C43 1.534(4) C43 H43A 0.9900 C43 H43B 0.9900 C43 C44 1.528(3) C44 H44A 0.9900 C44 H44B 0.9900 O5A C51A 1.437(8) O5A C54A 1.441(8) C51A H51A 0.9900 C51A H51B 0.9900 C51A C52A 1.529(8) C52A H52A 0.9900 C52A H52B 0.9900 C52A C53A 1.487(11) C53A H53A 0.9900 C53A H53B 0.9900 C53A C54A 1.519(8) C54A H54A 0.9900 C54A H54B 0.9900 O5B C51B 1.435(8) O5B C54B 1.437(8) C51B H51C 0.9900 C51B H51D 0.9900 C51B C52B 1.518(9) C52B H52C 0.9900 C52B H52D 0.9900 C52B C53B 1.490(11) C53B H53C 0.9900 C53B H53D 0.9900 C53B C54B 1.512(8) C54B H54C 0.9900 C54B H54D 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 Mg O3 C29 C31 -120.31(18) Mg O3 C29 C37 119.53(19) Mg O4 C41 C42 -160.72(14) Mg O4 C44 C43 167.03(13) Mg N1 C1 C2 -151.15(14) Mg N1 C1 C17 88.80(19) Mg N1 C3 O1 160.15(13) Mg N1 C3 C4 -20.3(3) Mg N2 C5 C4 4.6(3) Mg N2 C5 C6 -175.95(12) Mg N2 C12 C11 177.07(12) Mg N2 C12 C13 -1.2(3) Mg N3 C14 O2 164.45(12) Mg N3 C14 C13 -20.5(3) Mg N3 C16 C15 -151.20(14) Mg N3 C16 C23 88.82(19) Mg O5A C51A C52A 159.8(18) Mg O5A C54A C53A 177(2) Mg O5B C51B C52B -151(2) Mg O5B C54B C53B 164(2) F C34 C35 C36 179.5(2) O1 C3 C4 C5 -173.87(19) O2 C15 C16 N3 -25.6(2) O2 C15 C16 C23 93.52(19) O3 C29 C31 C32 -43.2(3) O3 C29 C31 C36 138.6(2) O4 C41 C42 C43 -29.5(2) N1 C1 C2 O1 -17.0(2) N1 C1 C17 C18 22.9(3) N1 C1 C17 C22 -161.38(18) N1 C3 C4 C5 6.6(4) N2 C5 C6 C7 176.9(2) N2 C5 C6 C11 -2.2(2) N2 C12 C13 C14 12.2(3) N3 C16 C23 C24 51.7(2) N3 C16 C23 C28 -130.12(19) C1 N1 C3 O1 -3.6(2) C1 N1 C3 C4 175.9(2) C1 C17 C18 C19 175.7(2) C1 C17 C22 C21 -175.6(2) C2 O1 C3 N1 -8.1(2) C2 O1 C3 C4 172.30(18) C2 C1 C17 C18 -92.5(2) C2 C1 C17 C22 83.2(2) C3 O1 C2 C1 15.3(2) C3 N1 C1 C2 12.8(2) C3 N1 C1 C17 -107.25(19) C3 C4 C5 N2 2.3(3) C3 C4 C5 C6 -177.18(19) C4 C5 C6 C7 -3.6(3) C4 C5 C6 C11 177.30(18) C5 N2 C12 C11 -0.5(2) C5 N2 C12 C13 -178.85(19) C5 C6 C7 C8 -179.0(2) C5 C6 C11 C10 178.80(18) C5 C6 C11 C12 1.8(2) C6 C7 C8 C9 -0.1(3) C6 C11 C12 N2 -0.9(2) C6 C11 C12 C13 177.54(18) C7 C6 C11 C10 -0.5(3) C7 C6 C11 C12 -177.49(18) C7 C8 C9 C10 0.5(3) C8 C9 C10 C11 -0.9(3) C9 C10 C11 C6 0.9(3) C9 C10 C11 C12 177.0(2) C10 C11 C12 N2 -177.4(2) C10 C11 C12 C13 1.0(3) C11 C6 C7 C8 0.0(3) C11 C12 C13 C14 -165.89(19) C12 N2 C5 C4 -177.82(19) C12 N2 C5 C6 1.7(2) C12 C13 C14 O2 175.19(18) C12 C13 C14 N3 0.1(3) C14 O2 C15 C16 21.9(2) C14 N3 C16 C15 20.6(2) C14 N3 C16 C23 -99.40(18) C15 O2 C14 N3 -9.8(2) C15 O2 C14 C13 174.44(17) C15 C16 C23 C24 -61.8(2) C15 C16 C23 C28 116.4(2) C16 N3 C14 O2 -7.7(2) C16 N3 C14 C13 167.3(2) C16 C23 C24 C25 178.55(19) C16 C23 C28 C27 -178.76(19) C17 C1 C2 O1 104.71(19) C17 C18 C19 C20 -0.4(4) C18 C17 C22 C21 0.3(3) C18 C19 C20 C21 0.5(4) C19 C20 C21 C22 -0.2(4) C20 C21 C22 C17 -0.2(4) C22 C17 C18 C19 0.0(3) C23 C24 C25 C26 0.4(3) C24 C23 C28 C27 -0.5(3) C24 C25 C26 C27 -0.9(3) C25 C26 C27 C28 0.7(4) C26 C27 C28 C23 0.0(3) C28 C23 C24 C25 0.4(3) C29 C31 C32 C33 -178.29(19) C29 C31 C36 C35 178.2(2) C31 C32 C33 C34 0.4(3) C32 C31 C36 C35 0.0(3) C32 C33 C34 F -179.5(2) C32 C33 C34 C35 -0.8(3) C33 C34 C35 C36 0.7(4) C34 C35 C36 C31 -0.3(3) C36 C31 C32 C33 0.0(3) C37 C29 C31 C32 79.1(2) C37 C29 C31 C36 -99.1(2) C41 O4 C44 C43 -37.0(2) C41 C42 C43 C44 7.2(2) C42 C43 C44 O4 17.4(2) C44 O4 C41 C42 41.9(2) O5A C51A C52A C53A 36(2) C51A O5A C54A C53A -2(3) C51A C52A C53A C54A -37(2) C52A C53A C54A O5A 25(3) C54A O5A C51A C52A -21(3) O5B C51B C52B C53B -32(2) C51B O5B C54B C53B -19(3) C51B C52B C53B C54B 20(2) C52B C53B C54B O5B -1(3) C54B O5B C51B C52B 32(3) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 4.4034 3.4462 -1.9174 0.8845 0.1636 -0.4368 -3.8183 1.6476 -4.0347 0.1983 0.8416 0.5024 0.8425 -1.0359 -7.1404 0.2101 0.8743 -0.4375 -2.6350 5.3874 2.0927 0.5728 0.1109 0.8122 -3.2101 2.1916 6.2407 -0.1377 -0.5640 0.8142 5.5557 0.3215 -2.9301 0.5203 0.0936 -0.8488 1.1892 -0.0636 6.6262 -0.2315 -0.9709 0.0619 -0.8806 -6.0013 -5.0263 -0.7522 0.4614 -0.4704 -3.2677 -5.5629 -1.4206 -0.9916 0.1287 0.0162 5.2493 -1.6212 1.9164 -0.0123 -0.6348 -0.7725 6.1598 1.4356 0.4472 0.5783 -0.3493 -0.7373 -0.0920 5.9368 5.0946 0.6796 -0.4178 0.6030 5.0909 -2.5983 0.5829 -0.1128 -0.4889 -0.8650 -5.2243 2.7711 0.6523 0.0763 0.3367 0.9385 -2.2908 5.5221 3.7379 0.5414 -0.1262 0.8312 3.4108 5.5881 2.1302 0.9726 -0.2321 -0.0095 3.4861 3.3567 -3.0078 0.8630 0.3603 -0.3541 6.0225 -0.4740 0.8445 0.2589 -0.4817 -0.8372