#------------------------------------------------------------------------------ #$Date: 2019-12-21 03:45:40 +0200 (Sat, 21 Dec 2019) $ #$Revision: 245465 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125680.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_7125680 loop_ _publ_author_name 'Gade, Lutz H.' 'Vasilenko, Valdislav' 'Blasius, Clemens' 'Wadepohl, Hubert' _publ_section_title ; Borohydride Intermediates Pave the Way for Magnesium-Catalysed Enantioselective Ketone Reduction ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09111D _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C38 H44 B Mg N3 O5' _chemical_formula_sum 'C38 H44 B Mg N3 O5' _chemical_formula_weight 657.88 _chemical_properties_physical 'air-sensitive, moisture-sensitive' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_block_code ga_vv33 _audit_creation_date 2018-09-10 _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 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.60635(16) _cell_length_b 16.6805(3) _cell_length_c 19.3703(2) _cell_measurement_reflns_used 28087 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 29.9810 _cell_measurement_theta_min 2.4930 _cell_volume 3426.98(9) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _diffrn_ambient_environment 'perfluoro polyether oil / N~2~' _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 -4.00 97.00 0.50 15.00 -- 26.43 77.00-120.00 202 2 \w 5.00 95.00 0.50 15.00 -- 26.43 57.00 0.00 180 3 \w -42.00 47.00 0.50 15.00 -- 26.43 -57.00-150.00 178 4 \w 5.00 95.00 0.50 15.00 -- 26.43 57.00-180.00 180 5 \w -42.00 47.00 0.50 15.00 -- 26.43 -57.00 30.00 178 6 \w -20.00 68.00 0.50 15.00 -- 26.43 -99.00 -30.00 176 7 \w -4.00 97.00 0.50 15.00 -- 26.43 77.00 60.00 202 8 \w -20.00 68.00 0.50 15.00 -- 26.43 -99.00 150.00 176 9 \w -71.00 -36.00 0.50 15.00 -- 2.00 150.00 1.66 70 10 \w -4.00 97.00 0.50 15.00 -- 26.43 77.00 -30.00 202 11 \w -20.00 68.00 0.50 15.00 -- 26.43 -99.00 30.00 176 12 \w -20.00 68.00 0.50 15.00 -- 26.43 -99.00-180.00 176 13 \w -46.00 52.00 0.50 15.00 -- 26.43 -38.00 -90.00 196 14 \w -46.00 52.00 0.50 15.00 -- 26.43 -38.00 90.00 196 15 \w -4.00 97.00 0.50 15.00 -- 26.43 77.00-150.00 202 16 \w -4.00 97.00 0.50 15.00 -- 26.43 77.00-120.00 202 17 \w -4.00 97.00 0.50 15.00 -- 26.43 77.00 -90.00 202 18 \w -4.00 85.50 0.50 15.00 -- 26.43 77.00 -60.00 179 ; _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 0.0618536000 _diffrn_orient_matrix_UB_12 0.0147654000 _diffrn_orient_matrix_UB_13 -0.0057455000 _diffrn_orient_matrix_UB_21 0.0240569000 _diffrn_orient_matrix_UB_22 -0.0395804000 _diffrn_orient_matrix_UB_23 0.0023172000 _diffrn_orient_matrix_UB_31 -0.0083560000 _diffrn_orient_matrix_UB_32 -0.0048856000 _diffrn_orient_matrix_UB_33 -0.0360778000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 145176 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.522 _diffrn_reflns_theta_min 2.189 _diffrn_source 'microfocus X-Ray tube' _diffrn_source_type 'Agilent SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (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 yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.275 _exptl_crystal_description irregular _exptl_crystal_F_000 1400 _exptl_crystal_size_max 0.232 _exptl_crystal_size_mid 0.187 _exptl_crystal_size_min 0.126 _refine_diff_density_max 0.320 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 3771 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 473 _refine_ls_number_reflns 12099 _refine_ls_number_restraints 85 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0496 _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^)+(0.0581P)^2^+0.8439P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1127 _refine_ls_wR_factor_ref 0.1207 _reflns_Friedel_coverage 0.799 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.960 _reflns_number_gt 9996 _reflns_number_total 12099 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ga_vv33 - #3166 - in P2(1)2(1)2(1) - superflip - nova CELL 0.71073 10.60635 16.680504 19.370331 90 90 90 ZERR 4 0.000157 0.000256 0.000249 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H B Mg N O UNIT 152 176 4 4 12 20 SADI O5 C35A O5 C35B O5 C38 SADI C35A C36A C35B C36B C38 C37A C38 C37B SADI C36A C37A C36B C37B SIMU 0.01 0.01 1 $C RIGU O5 > C38 L.S. 10 PLAN 25 SIZE 0.1 0.1 0.1 TEMP -153.25 CONF HTAB fmap 2 acta OMIT 0 0 2 OMIT 3 9 3 OMIT -3 9 3 WGHT 0.058100 0.843900 FVAR 2.80129 0.57555 MG 4 0.205315 0.469711 0.353795 11.00000 0.01707 0.01818 = 0.01603 0.00023 -0.00133 -0.00002 O1 6 0.398536 0.243828 0.376942 11.00000 0.04034 0.02210 = 0.02932 -0.00533 -0.00843 0.00922 O2 6 0.164836 0.723960 0.392214 11.00000 0.03342 0.01695 = 0.03166 0.00142 -0.00848 0.00143 O3 6 0.043397 0.412010 0.356808 11.00000 0.02249 0.02411 = 0.01743 0.00356 -0.00066 -0.00726 O4 6 -0.147663 0.361060 0.313750 11.00000 0.02173 0.03725 = 0.02596 0.00541 -0.00508 -0.00546 N1 5 0.306834 0.358442 0.339820 11.00000 0.02165 0.02336 = 0.01981 -0.00336 0.00028 0.00246 N2 5 0.328310 0.491021 0.437467 11.00000 0.01865 0.01897 = 0.01800 0.00012 -0.00223 -0.00019 N3 5 0.140551 0.592322 0.367362 11.00000 0.01816 0.01887 = 0.01921 0.00223 -0.00301 0.00113 C1 1 0.297895 0.301585 0.281384 11.00000 0.02415 0.02624 = 0.02518 -0.00681 -0.00297 0.00452 AFIX 13 H1 2 0.210750 0.301643 0.261679 11.00000 -1.20000 AFIX 0 C2 1 0.326353 0.221035 0.316171 11.00000 0.03846 0.02535 = 0.03258 -0.00727 -0.00788 0.00634 AFIX 23 H2A 2 0.247606 0.193032 0.329265 11.00000 -1.20000 H2B 2 0.376343 0.185879 0.285408 11.00000 -1.20000 AFIX 0 C3 1 0.371410 0.322971 0.387299 11.00000 0.02237 0.02062 = 0.02309 -0.00113 0.00021 0.00340 C4 1 0.424572 0.357385 0.447926 11.00000 0.02396 0.02226 = 0.01998 0.00146 -0.00350 0.00302 AFIX 43 H4 2 0.473306 0.323792 0.477191 11.00000 -1.20000 AFIX 0 C5 1 0.409795 0.435450 0.466470 11.00000 0.01830 0.02337 = 0.01684 0.00284 -0.00008 -0.00028 C6 1 0.484107 0.473893 0.521537 11.00000 0.01890 0.02526 = 0.01696 0.00187 -0.00007 -0.00170 C7 1 0.444514 0.553300 0.524704 11.00000 0.01874 0.02446 = 0.01727 0.00045 -0.00071 -0.00316 C8 1 0.346108 0.563147 0.471251 11.00000 0.01750 0.02181 = 0.01739 0.00068 -0.00086 -0.00374 C9 1 0.288839 0.634369 0.457574 11.00000 0.02231 0.01990 = 0.02354 -0.00207 -0.00397 -0.00121 AFIX 43 H9 2 0.311507 0.679307 0.485029 11.00000 -1.20000 AFIX 0 C10 1 0.196910 0.646033 0.404676 11.00000 0.02235 0.01659 = 0.02438 0.00038 -0.00031 0.00139 C11 1 0.096676 0.722197 0.327051 11.00000 0.03240 0.02073 = 0.02776 0.00614 -0.00500 0.00199 AFIX 23 H11A 2 0.153354 0.734346 0.287814 11.00000 -1.20000 H11B 2 0.026137 0.761066 0.327174 11.00000 -1.20000 AFIX 0 C12 1 0.047855 0.635882 0.323193 11.00000 0.02331 0.02001 = 0.01857 0.00230 -0.00246 0.00255 AFIX 13 H12 2 0.053470 0.615940 0.274605 11.00000 -1.20000 AFIX 0 C13 1 0.582069 0.445775 0.562754 11.00000 0.02442 0.02612 = 0.02129 0.00258 -0.00181 0.00083 AFIX 43 H13 2 0.609961 0.391747 0.560028 11.00000 -1.20000 AFIX 0 C14 1 0.637502 0.500013 0.608119 11.00000 0.02302 0.03719 = 0.02113 0.00162 -0.00492 -0.00091 AFIX 43 H14 2 0.704365 0.482619 0.637112 11.00000 -1.20000 AFIX 0 C15 1 0.597010 0.579060 0.611846 11.00000 0.02433 0.03213 = 0.02141 -0.00069 -0.00483 -0.00645 AFIX 43 H15 2 0.636163 0.614605 0.643607 11.00000 -1.20000 AFIX 0 C16 1 0.500001 0.607166 0.569841 11.00000 0.02463 0.02630 = 0.02331 -0.00092 -0.00287 -0.00402 AFIX 43 H16 2 0.472857 0.661379 0.572078 11.00000 -1.20000 AFIX 0 C17 1 0.393671 0.322431 0.226248 11.00000 0.02364 0.03924 = 0.02391 -0.00857 -0.00138 0.00834 C18 1 0.516211 0.346172 0.243676 11.00000 0.02529 0.05873 = 0.02471 -0.00844 -0.00146 0.00676 AFIX 43 H18 2 0.538640 0.351678 0.290921 11.00000 -1.20000 AFIX 0 C19 1 0.604937 0.361703 0.193309 11.00000 0.02362 0.08905 = 0.03272 -0.00680 0.00396 0.00129 AFIX 43 H19 2 0.687739 0.377652 0.206002 11.00000 -1.20000 AFIX 0 C20 1 0.573277 0.354042 0.124278 11.00000 0.03540 0.11360 = 0.02909 -0.00987 0.01005 0.00078 AFIX 43 H20 2 0.634061 0.364723 0.089450 11.00000 -1.20000 AFIX 0 C21 1 0.452515 0.330726 0.106430 11.00000 0.04224 0.10709 = 0.02281 -0.01443 0.00088 -0.00123 AFIX 43 H21 2 0.430606 0.325677 0.059075 11.00000 -1.20000 AFIX 0 C22 1 0.363260 0.314668 0.156496 11.00000 0.03061 0.06778 = 0.02691 -0.01442 -0.00280 0.00211 AFIX 43 H22 2 0.280889 0.298282 0.143383 11.00000 -1.20000 AFIX 0 C23 1 -0.086165 0.627378 0.349264 11.00000 0.02229 0.02249 = 0.02493 0.00534 -0.00258 0.00482 C24 1 -0.178492 0.596061 0.306158 11.00000 0.02520 0.04061 = 0.02976 0.00398 -0.00642 0.00177 AFIX 43 H24 2 -0.157241 0.579824 0.260612 11.00000 -1.20000 AFIX 0 C25 1 -0.301841 0.588395 0.329418 11.00000 0.02764 0.06302 = 0.04815 0.01672 -0.01021 -0.00396 AFIX 43 H25 2 -0.363986 0.565653 0.300026 11.00000 -1.20000 AFIX 0 C26 1 -0.334758 0.613461 0.394665 11.00000 0.02261 0.07360 = 0.05136 0.02768 0.00856 0.00840 AFIX 43 H26 2 -0.419580 0.608739 0.409885 11.00000 -1.20000 AFIX 0 C27 1 -0.244237 0.645564 0.438122 11.00000 0.03692 0.04980 = 0.03257 0.01358 0.00878 0.01547 AFIX 43 H27 2 -0.266948 0.663213 0.483062 11.00000 -1.20000 AFIX 0 C28 1 -0.120279 0.651898 0.415886 11.00000 0.03060 0.03327 = 0.02555 0.00511 -0.00063 0.00878 AFIX 43 H28 2 -0.058017 0.673035 0.446081 11.00000 -1.20000 AFIX 0 C29 1 -0.028302 0.379846 0.413987 11.00000 0.02357 0.02275 = 0.01933 0.00374 0.00156 -0.00403 C30 1 -0.120944 0.321254 0.376808 11.00000 0.02224 0.02791 = 0.02598 0.00268 -0.00019 -0.00594 C31 1 0.061896 0.339859 0.464964 11.00000 0.03259 0.03791 = 0.02498 0.00853 -0.00473 -0.00631 AFIX 137 H31A 2 0.109104 0.297449 0.441349 11.00000 -1.50000 H31B 2 0.013587 0.316576 0.503147 11.00000 -1.50000 H31C 2 0.120842 0.379908 0.483088 11.00000 -1.50000 AFIX 0 C32 1 -0.095888 0.448889 0.449518 11.00000 0.05202 0.02532 = 0.02972 -0.00013 0.01434 0.00091 AFIX 137 H32A 2 -0.034089 0.489275 0.463840 11.00000 -1.50000 H32B 2 -0.140821 0.428752 0.490182 11.00000 -1.50000 H32C 2 -0.156295 0.473121 0.417422 11.00000 -1.50000 AFIX 0 C33 1 -0.060216 0.240316 0.361207 11.00000 0.04967 0.02411 = 0.03199 0.00121 -0.00122 -0.00531 AFIX 137 H33A 2 -0.116307 0.208892 0.331474 11.00000 -1.50000 H33B 2 -0.045799 0.211303 0.404487 11.00000 -1.50000 H33C 2 0.020457 0.248777 0.337642 11.00000 -1.50000 AFIX 0 C34 1 -0.243480 0.307546 0.415700 11.00000 0.02651 0.05356 = 0.03861 0.00625 0.00520 -0.01293 AFIX 137 H34A 2 -0.289306 0.358350 0.419705 11.00000 -1.50000 H34B 2 -0.224823 0.286790 0.461914 11.00000 -1.50000 H34C 2 -0.295340 0.268658 0.390563 11.00000 -1.50000 AFIX 0 O5 6 0.256099 0.507549 0.254499 11.00000 0.02315 0.03320 = 0.01717 0.00170 -0.00044 -0.00727 PART 1 C35A 1 0.356440 0.567055 0.247669 21.00000 0.03340 0.06063 = 0.02909 -0.00285 0.00310 -0.02227 AFIX 23 H35A 2 0.423193 0.558515 0.282627 21.00000 -1.20000 H35B 2 0.322939 0.622181 0.252374 21.00000 -1.20000 AFIX 0 C36A 1 0.406389 0.552022 0.174581 21.00000 0.03090 0.07365 = 0.02597 0.00300 0.00727 -0.01866 AFIX 23 H36A 2 0.454197 0.598681 0.156906 21.00000 -1.20000 H36B 2 0.460328 0.503635 0.172659 21.00000 -1.20000 AFIX 0 C37A 1 0.283534 0.539998 0.135122 21.00000 0.03492 0.04675 = 0.02162 0.00376 -0.00852 -0.01111 AFIX 23 H37A 2 0.246782 0.592052 0.121058 21.00000 -1.20000 H37B 2 0.296970 0.506607 0.093515 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C35B 1 0.380245 0.543684 0.249927 -21.00000 0.02275 0.03607 = 0.02721 0.00168 -0.00166 -0.01122 AFIX 23 H35C 2 0.446950 0.502321 0.246874 -21.00000 -1.20000 H35D 2 0.397249 0.578734 0.290107 -21.00000 -1.20000 AFIX 0 C36B 1 0.371543 0.591798 0.183866 -21.00000 0.05133 0.06907 = 0.03675 0.01370 -0.00397 -0.03047 AFIX 23 H36C 2 0.327187 0.643275 0.191431 -21.00000 -1.20000 H36D 2 0.456137 0.602611 0.164376 -21.00000 -1.20000 AFIX 0 C37B 1 0.296990 0.537274 0.138103 -21.00000 0.04757 0.07115 = 0.02418 0.01101 0.01520 -0.01828 AFIX 23 H37C 2 0.352117 0.496353 0.116673 -21.00000 -1.20000 H37D 2 0.254330 0.567997 0.101136 -21.00000 -1.20000 AFIX 0 PART 0 C38 1 0.199970 0.497860 0.186407 11.00000 0.02736 0.03920 = 0.01655 0.00185 -0.00211 -0.00528 PART 1 AFIX 23 H38A 2 0.114340 0.521464 0.185641 21.00000 -1.20000 H38B 2 0.193257 0.440244 0.174707 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H38C 2 0.117419 0.525366 0.183593 -21.00000 -1.20000 H38D 2 0.188443 0.440474 0.174997 -21.00000 -1.20000 AFIX 0 PART 0 B13 3 -0.031707 0.398992 0.289842 11.00000 0.02297 0.02500 = 0.01875 0.00053 -0.00252 -0.00389 H13A 2 0.034151 0.359137 0.252959 11.00000 0.03596 H13B 2 -0.043390 0.458466 0.265564 11.00000 0.04335 HKLF 4 REM ga_vv33 - #3166 - in P2(1)2(1)2(1) - superflip - nova REM wR2 = 0.1207, GooF = S = 1.025, Restrained GooF = 1.024 for all data REM R1 = 0.0496 for 9996 Fo > 4sig(Fo) and 0.0670 for all 12099 data REM 473 parameters refined using 85 restraints END WGHT 0.0582 0.8407 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.320, deepest hole -0.254, 1-sigma level 0.051 Q1 1 0.2570 0.6393 0.4254 11.00000 0.05 0.32 Q2 1 -0.1373 0.6196 0.3276 11.00000 0.05 0.31 Q3 1 0.6202 0.5407 0.6025 11.00000 0.05 0.30 Q4 1 0.5920 0.4776 0.5841 11.00000 0.05 0.29 Q5 1 0.3217 0.6013 0.4536 11.00000 0.05 0.28 Q6 1 0.4689 0.5132 0.5316 11.00000 0.05 0.28 Q7 1 0.3969 0.3466 0.4202 11.00000 0.05 0.28 Q8 1 -0.0962 0.3602 0.4054 11.00000 0.05 0.27 Q9 1 0.3905 0.5616 0.4992 11.00000 0.05 0.26 Q10 1 0.0083 0.3580 0.4424 11.00000 0.05 0.26 Q11 1 0.4410 0.5982 0.5400 11.00000 0.05 0.26 Q12 1 0.4624 0.3463 0.2205 11.00000 0.05 0.25 Q13 1 -0.2748 0.6394 0.4099 11.00000 0.05 0.25 Q14 1 0.5356 0.4612 0.5388 11.00000 0.05 0.25 Q15 1 -0.1891 0.2879 0.3866 11.00000 0.05 0.25 Q16 1 0.5773 0.5371 0.6234 11.00000 0.05 0.24 Q17 1 -0.1814 0.6402 0.4270 11.00000 0.05 0.24 Q18 1 -0.1923 0.6645 0.4173 11.00000 0.05 0.24 Q19 1 -0.0243 0.6393 0.3367 11.00000 0.05 0.24 Q20 1 -0.2680 0.5998 0.4301 11.00000 0.05 0.23 Q21 1 0.0837 0.6134 0.3529 11.00000 0.05 0.23 Q22 1 0.4150 0.3396 0.1361 11.00000 0.05 0.23 Q23 1 -0.1070 0.6501 0.3800 11.00000 0.05 0.23 Q24 1 0.5384 0.3622 0.2113 11.00000 0.05 0.23 Q25 1 -0.1776 0.3213 0.4035 11.00000 0.05 0.23 ; _cod_data_source_file c9cc09111d2.cif _cod_data_source_block ga_vv33 _cod_database_code 7125680 _audit_block_refno 3166 _audit_block_usercomment 'VV619 irregular yellow' _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 0.990 _shelx_estimated_absorpt_t_min 0.990 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _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, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O5-C35A \\sim O5-C35B \\sim O5-C38 with sigma of 0.02 C35A-C36A \\sim C35B-C36B \\sim C38-C37A \\sim C38-C37B with sigma of 0.02 C36A-C37A \\sim C36B-C37B 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 C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35A \\sim C36A \\sim C37A \\sim C35B \\sim C36B \\sim C37B \\sim C38: within 1A with sigma of 0.01 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains O5, C35A, C36A, C37A, C35B, C36B, C37B, C38 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)= Sof(H37C)=Sof(H37D)=Sof(H38C)=Sof(H38D)=1-FVAR(1) Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)= Sof(H37A)=Sof(H37B)=Sof(H38A)=Sof(H38B)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C1(H1), C12(H12) 6.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C11(H11A,H11B), C35A(H35A,H35B), C36A(H36A,H36B), C37A(H37A, H37B), C35B(H35C,H35D), C36B(H36C,H36D), C37B(H37C,H37D), C38(H38A,H38B), C38(H38C,H38D) 6.c Aromatic/amide H refined with riding coordinates: C4(H4), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28) 6.d Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B, H34C) ; _olex2_submission_special_instructions 'No special instructions were received' _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 1.112 _oxdiff_exptl_absorpt_empirical_full_min 0.885 _shelx_res_checksum 75399 _cell_oxdiff_length_a 10.6038(3) _cell_oxdiff_length_b 16.6790(3) _cell_oxdiff_length_c 19.3767(5) _cell_oxdiff_angle_alpha 89.9895(18) _cell_oxdiff_angle_beta 90.043(2) _cell_oxdiff_angle_gamma 90.0390(18) _cell_oxdiff_volume 3426.98(14) _cell_oxdiff_measurement_reflns_used 28087 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.20531(7) 0.46971(4) 0.35379(3) 0.01710(14) Uani 1 1 d . . . . . O1 O 0.39854(18) 0.24383(10) 0.37694(9) 0.0306(4) Uani 1 1 d . . . . . O2 O 0.16484(17) 0.72396(9) 0.39221(9) 0.0273(3) Uani 1 1 d . . . . . O3 O 0.04340(14) 0.41201(9) 0.35681(8) 0.0213(3) Uani 1 1 d . . . . . O4 O -0.14766(15) 0.36106(11) 0.31375(8) 0.0283(3) Uani 1 1 d . . . . . N1 N 0.30683(17) 0.35844(11) 0.33982(9) 0.0216(3) Uani 1 1 d . . . . . N2 N 0.32831(16) 0.49102(10) 0.43747(9) 0.0185(3) Uani 1 1 d . . . . . N3 N 0.14055(16) 0.59232(10) 0.36736(9) 0.0187(3) Uani 1 1 d . . . . . C1 C 0.2979(2) 0.30159(13) 0.28138(11) 0.0252(4) Uani 1 1 d . U . . . H1 H 0.210750 0.301643 0.261679 0.030 Uiso 1 1 calc R . . . . C2 C 0.3264(3) 0.22103(14) 0.31617(13) 0.0321(5) Uani 1 1 d . U . . . H2A H 0.247606 0.193032 0.329265 0.039 Uiso 1 1 calc R . . . . H2B H 0.376343 0.185879 0.285408 0.039 Uiso 1 1 calc R . . . . C3 C 0.3714(2) 0.32297(13) 0.38730(11) 0.0220(4) Uani 1 1 d . U . . . C4 C 0.4246(2) 0.35739(13) 0.44793(11) 0.0221(4) Uani 1 1 d . U . . . H4 H 0.473306 0.323792 0.477191 0.026 Uiso 1 1 calc R . . . . C5 C 0.40979(19) 0.43545(12) 0.46647(10) 0.0195(4) Uani 1 1 d . U . . . C6 C 0.48411(19) 0.47389(13) 0.52154(10) 0.0204(4) Uani 1 1 d . U . . . C7 C 0.44451(19) 0.55330(13) 0.52470(10) 0.0202(4) Uani 1 1 d . U . . . C8 C 0.34611(19) 0.56315(12) 0.47125(10) 0.0189(4) Uani 1 1 d . U . . . C9 C 0.2888(2) 0.63437(13) 0.45757(11) 0.0219(4) Uani 1 1 d . U . . . H9 H 0.311507 0.679307 0.485029 0.026 Uiso 1 1 calc R . . . . C10 C 0.1969(2) 0.64603(12) 0.40468(11) 0.0211(4) Uani 1 1 d . U . . . C11 C 0.0967(2) 0.72220(13) 0.32705(12) 0.0270(4) Uani 1 1 d . U . . . H11A H 0.153354 0.734346 0.287814 0.032 Uiso 1 1 calc R . . . . H11B H 0.026137 0.761066 0.327174 0.032 Uiso 1 1 calc R . . . . C12 C 0.0479(2) 0.63588(13) 0.32319(10) 0.0206(4) Uani 1 1 d . U . . . H12 H 0.053470 0.615940 0.274605 0.025 Uiso 1 1 calc R . . . . C13 C 0.5821(2) 0.44578(14) 0.56275(11) 0.0239(4) Uani 1 1 d . U . . . H13 H 0.609961 0.391747 0.560028 0.029 Uiso 1 1 calc R . . . . C14 C 0.6375(2) 0.50001(15) 0.60812(11) 0.0271(4) Uani 1 1 d . U . . . H14 H 0.704365 0.482619 0.637112 0.033 Uiso 1 1 calc R . . . . C15 C 0.5970(2) 0.57906(15) 0.61185(11) 0.0260(4) Uani 1 1 d . U . . . H15 H 0.636163 0.614605 0.643607 0.031 Uiso 1 1 calc R . . . . C16 C 0.5000(2) 0.60717(14) 0.56984(11) 0.0247(4) Uani 1 1 d . U . . . H16 H 0.472857 0.661379 0.572078 0.030 Uiso 1 1 calc R . . . . C17 C 0.3937(2) 0.32243(16) 0.22625(12) 0.0289(5) Uani 1 1 d . U . . . C18 C 0.5162(2) 0.34617(19) 0.24368(13) 0.0362(6) Uani 1 1 d . U . . . H18 H 0.538640 0.351678 0.290921 0.043 Uiso 1 1 calc R . . . . C19 C 0.6049(3) 0.3617(2) 0.19331(15) 0.0485(8) Uani 1 1 d . U . . . H19 H 0.687739 0.377652 0.206002 0.058 Uiso 1 1 calc R . . . . C20 C 0.5733(3) 0.3540(3) 0.12428(16) 0.0594(10) Uani 1 1 d . U . . . H20 H 0.634061 0.364723 0.089450 0.071 Uiso 1 1 calc R . . . . C21 C 0.4525(3) 0.3307(3) 0.10643(15) 0.0574(10) Uani 1 1 d . U . . . H21 H 0.430606 0.325677 0.059075 0.069 Uiso 1 1 calc R . . . . C22 C 0.3633(3) 0.3147(2) 0.15650(13) 0.0418(7) Uani 1 1 d . U . . . H22 H 0.280889 0.298282 0.143383 0.050 Uiso 1 1 calc R . . . . C23 C -0.0862(2) 0.62738(13) 0.34926(11) 0.0232(4) Uani 1 1 d . U . . . C24 C -0.1785(2) 0.59606(16) 0.30616(13) 0.0319(5) Uani 1 1 d . U . . . H24 H -0.157241 0.579824 0.260612 0.038 Uiso 1 1 calc R . . . . C25 C -0.3018(3) 0.5884(2) 0.32942(16) 0.0463(7) Uani 1 1 d . U . . . H25 H -0.363986 0.565653 0.300026 0.056 Uiso 1 1 calc R . . . . C26 C -0.3348(3) 0.6135(2) 0.39466(17) 0.0492(8) Uani 1 1 d . U . . . H26 H -0.419580 0.608739 0.409885 0.059 Uiso 1 1 calc R . . . . C27 C -0.2442(3) 0.64556(19) 0.43812(15) 0.0398(6) Uani 1 1 d . U . . . H27 H -0.266948 0.663213 0.483062 0.048 Uiso 1 1 calc R . . . . C28 C -0.1203(2) 0.65190(16) 0.41589(12) 0.0298(5) Uani 1 1 d . U . . . H28 H -0.058017 0.673035 0.446081 0.036 Uiso 1 1 calc R . . . . C29 C -0.0283(2) 0.37985(13) 0.41399(11) 0.0219(4) Uani 1 1 d . U . . . C30 C -0.1209(2) 0.32125(14) 0.37681(12) 0.0254(4) Uani 1 1 d . U . . . C31 C 0.0619(2) 0.33986(16) 0.46496(12) 0.0318(5) Uani 1 1 d . U . . . H31A H 0.109104 0.297449 0.441349 0.048 Uiso 1 1 calc GR . . . . H31B H 0.013587 0.316576 0.503147 0.048 Uiso 1 1 calc GR . . . . H31C H 0.120842 0.379908 0.483088 0.048 Uiso 1 1 calc GR . . . . C32 C -0.0959(3) 0.44889(15) 0.44952(13) 0.0357(6) Uani 1 1 d . U . . . H32A H -0.034089 0.489275 0.463840 0.054 Uiso 1 1 calc GR . . . . H32B H -0.140821 0.428752 0.490182 0.054 Uiso 1 1 calc GR . . . . H32C H -0.156295 0.473121 0.417422 0.054 Uiso 1 1 calc GR . . . . C33 C -0.0602(3) 0.24032(15) 0.36121(14) 0.0353(6) Uani 1 1 d . U . . . H33A H -0.116307 0.208892 0.331474 0.053 Uiso 1 1 calc GR . . . . H33B H -0.045799 0.211303 0.404487 0.053 Uiso 1 1 calc GR . . . . H33C H 0.020457 0.248777 0.337642 0.053 Uiso 1 1 calc GR . . . . C34 C -0.2435(3) 0.3075(2) 0.41570(15) 0.0396(6) Uani 1 1 d . U . . . H34A H -0.289306 0.358350 0.419705 0.059 Uiso 1 1 calc GR . . . . H34B H -0.224823 0.286790 0.461914 0.059 Uiso 1 1 calc GR . . . . H34C H -0.295340 0.268658 0.390563 0.059 Uiso 1 1 calc GR . . . . O5 O 0.25610(15) 0.50755(10) 0.25450(8) 0.0245(3) Uani 1 1 d D U . . . C35A C 0.3564(10) 0.5671(7) 0.2477(6) 0.041(2) Uani 0.576(15) 1 d D U P A 1 H35A H 0.423193 0.558515 0.282627 0.049 Uiso 0.576(15) 1 calc R . P A 1 H35B H 0.322939 0.622181 0.252374 0.049 Uiso 0.576(15) 1 calc R . P A 1 C36A C 0.4064(6) 0.5520(7) 0.1746(3) 0.0435(19) Uani 0.576(15) 1 d D U P A 1 H36A H 0.454197 0.598681 0.156906 0.052 Uiso 0.576(15) 1 calc R . P A 1 H36B H 0.460328 0.503635 0.172659 0.052 Uiso 0.576(15) 1 calc R . P A 1 C37A C 0.2835(12) 0.5400(9) 0.1351(5) 0.0344(19) Uani 0.576(15) 1 d D U P A 1 H37A H 0.246782 0.592052 0.121058 0.041 Uiso 0.576(15) 1 calc R . P A 1 H37B H 0.296970 0.506607 0.093515 0.041 Uiso 0.576(15) 1 calc R . P A 1 C35B C 0.3802(11) 0.5437(7) 0.2499(7) 0.029(2) Uani 0.424(15) 1 d D U P A 2 H35C H 0.446950 0.502321 0.246874 0.034 Uiso 0.424(15) 1 calc R . P A 2 H35D H 0.397249 0.578734 0.290107 0.034 Uiso 0.424(15) 1 calc R . P A 2 C36B C 0.3715(13) 0.5918(9) 0.1839(5) 0.052(3) Uani 0.424(15) 1 d D U P A 2 H36C H 0.327187 0.643275 0.191431 0.063 Uiso 0.424(15) 1 calc R . P A 2 H36D H 0.456137 0.602611 0.164376 0.063 Uiso 0.424(15) 1 calc R . P A 2 C37B C 0.2970(19) 0.5373(15) 0.1381(8) 0.048(4) Uani 0.424(15) 1 d D U P A 2 H37C H 0.352117 0.496353 0.116673 0.057 Uiso 0.424(15) 1 calc R . P A 2 H37D H 0.254330 0.567997 0.101136 0.057 Uiso 0.424(15) 1 calc R . P A 2 C38 C 0.2000(2) 0.49786(15) 0.18641(10) 0.0277(4) Uani 1 1 d D U . . . H38A H 0.114340 0.521464 0.185641 0.033 Uiso 0.576(15) 1 calc R . P A 1 H38B H 0.193257 0.440244 0.174707 0.033 Uiso 0.576(15) 1 calc R . P A 1 H38C H 0.117419 0.525366 0.183593 0.033 Uiso 0.424(15) 1 calc R . P A 2 H38D H 0.188443 0.440474 0.174997 0.033 Uiso 0.424(15) 1 calc R . P A 2 B13 B -0.0317(2) 0.39899(15) 0.28984(12) 0.0222(4) Uani 1 1 d . . . . . H13A H 0.034(3) 0.3591(18) 0.2530(16) 0.036(8) Uiso 1 1 d . . . . . H13B H -0.043(3) 0.458(2) 0.2656(16) 0.043(9) Uiso 1 1 d . . . . . 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 0.0171(3) 0.0182(3) 0.0160(3) 0.0002(2) -0.0013(2) 0.0000(2) O1 0.0403(10) 0.0221(8) 0.0293(8) -0.0053(6) -0.0084(7) 0.0092(7) O2 0.0334(8) 0.0169(7) 0.0317(8) 0.0014(6) -0.0085(7) 0.0014(6) O3 0.0225(7) 0.0241(7) 0.0174(6) 0.0036(6) -0.0007(6) -0.0073(6) O4 0.0217(7) 0.0373(9) 0.0260(8) 0.0054(7) -0.0051(6) -0.0055(7) N1 0.0217(8) 0.0234(8) 0.0198(8) -0.0034(6) 0.0003(6) 0.0025(7) N2 0.0187(8) 0.0190(8) 0.0180(7) 0.0001(6) -0.0022(6) -0.0002(6) N3 0.0182(8) 0.0189(8) 0.0192(8) 0.0022(6) -0.0030(6) 0.0011(6) C1 0.0242(10) 0.0262(10) 0.0252(10) -0.0068(8) -0.0030(8) 0.0045(9) C2 0.0385(13) 0.0253(11) 0.0326(12) -0.0073(9) -0.0079(10) 0.0063(10) C3 0.0224(10) 0.0206(9) 0.0231(9) -0.0011(8) 0.0002(8) 0.0034(7) C4 0.0240(10) 0.0223(10) 0.0200(9) 0.0015(7) -0.0035(7) 0.0030(8) C5 0.0183(9) 0.0234(9) 0.0168(8) 0.0028(7) -0.0001(7) -0.0003(7) C6 0.0189(9) 0.0253(10) 0.0170(8) 0.0019(7) -0.0001(7) -0.0017(8) C7 0.0187(9) 0.0245(10) 0.0173(8) 0.0005(7) -0.0007(7) -0.0032(7) C8 0.0175(8) 0.0218(9) 0.0174(8) 0.0007(7) -0.0009(7) -0.0037(7) C9 0.0223(9) 0.0199(9) 0.0235(9) -0.0021(7) -0.0040(8) -0.0012(8) C10 0.0223(9) 0.0166(9) 0.0244(9) 0.0004(7) -0.0003(8) 0.0014(7) C11 0.0324(11) 0.0207(10) 0.0278(10) 0.0061(8) -0.0050(9) 0.0020(9) C12 0.0233(9) 0.0200(9) 0.0186(8) 0.0023(7) -0.0025(7) 0.0026(7) C13 0.0244(10) 0.0261(10) 0.0213(9) 0.0026(8) -0.0018(8) 0.0008(8) C14 0.0230(10) 0.0372(12) 0.0211(9) 0.0016(9) -0.0049(8) -0.0009(9) C15 0.0243(10) 0.0321(11) 0.0214(9) -0.0007(8) -0.0048(8) -0.0064(9) C16 0.0246(10) 0.0263(10) 0.0233(10) -0.0009(8) -0.0029(8) -0.0040(8) C17 0.0236(10) 0.0392(13) 0.0239(10) -0.0086(9) -0.0014(8) 0.0083(9) C18 0.0253(11) 0.0587(17) 0.0247(11) -0.0084(11) -0.0015(9) 0.0068(11) C19 0.0236(12) 0.089(2) 0.0327(13) -0.0068(15) 0.0040(10) 0.0013(14) C20 0.0354(15) 0.114(3) 0.0291(13) -0.0099(17) 0.0100(12) 0.0008(18) C21 0.0422(16) 0.107(3) 0.0228(12) -0.0144(16) 0.0009(12) -0.0012(18) C22 0.0306(13) 0.0678(19) 0.0269(12) -0.0144(12) -0.0028(10) 0.0021(12) C23 0.0223(9) 0.0225(9) 0.0249(9) 0.0053(8) -0.0026(8) 0.0048(8) C24 0.0252(11) 0.0406(13) 0.0298(11) 0.0040(10) -0.0064(9) 0.0018(10) C25 0.0276(13) 0.0630(19) 0.0482(16) 0.0167(14) -0.0102(12) -0.0040(13) C26 0.0226(11) 0.074(2) 0.0514(17) 0.0277(16) 0.0086(12) 0.0084(13) C27 0.0369(14) 0.0498(16) 0.0326(12) 0.0136(12) 0.0088(11) 0.0155(12) C28 0.0306(11) 0.0333(12) 0.0255(10) 0.0051(9) -0.0006(9) 0.0088(10) C29 0.0236(10) 0.0228(10) 0.0193(9) 0.0037(7) 0.0016(7) -0.0040(8) C30 0.0222(10) 0.0279(11) 0.0260(10) 0.0027(8) -0.0002(8) -0.0059(8) C31 0.0326(12) 0.0379(13) 0.0250(10) 0.0085(10) -0.0047(9) -0.0063(10) C32 0.0520(16) 0.0253(11) 0.0297(11) -0.0001(9) 0.0143(11) 0.0009(11) C33 0.0497(15) 0.0241(11) 0.0320(12) 0.0012(10) -0.0012(11) -0.0053(10) C34 0.0265(12) 0.0536(17) 0.0386(14) 0.0063(12) 0.0052(10) -0.0129(12) O5 0.0231(7) 0.0332(8) 0.0172(6) 0.0017(6) -0.0004(5) -0.0073(6) C35A 0.033(4) 0.061(6) 0.029(3) -0.003(4) 0.003(3) -0.022(4) C36A 0.031(3) 0.074(5) 0.026(2) 0.003(3) 0.0073(19) -0.019(3) C37A 0.035(3) 0.047(4) 0.022(3) 0.004(3) -0.009(3) -0.011(3) C35B 0.023(4) 0.036(5) 0.027(3) 0.002(3) -0.002(3) -0.011(3) C36B 0.051(6) 0.069(6) 0.037(4) 0.014(4) -0.004(4) -0.030(5) C37B 0.048(7) 0.071(7) 0.024(5) 0.011(5) 0.015(5) -0.018(6) C38 0.0274(10) 0.0392(12) 0.0166(8) 0.0018(8) -0.0021(8) -0.0053(10) B13 0.0230(11) 0.0250(11) 0.0187(10) 0.0005(8) -0.0025(8) -0.0039(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 -13 -9 -7 0.0660 13 -5 12 0.0816 -9 -1 -22 0.1111 12 7 -14 0.0548 -7 -3 24 0.0984 2 3 27 0.0965 3 -23 3 0.1009 3 -18 16 0.1040 0 -12 -23 0.0774 -10 -16 -10 0.0706 4 6 26 0.0903 14 -8 -3 0.0755 -14 4 6 0.0568 14 -4 -10 0.0619 11 12 12 0.0788 10 11 -15 0.0561 -3 23 -1 0.0722 13 9 10 0.0748 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O3 Mg N1 91.06(7) O3 Mg N2 126.76(7) O3 Mg N3 100.41(7) O3 Mg O5 113.49(7) N1 Mg N3 168.53(7) N2 Mg N1 86.15(7) N2 Mg N3 86.79(7) O5 Mg N1 90.90(7) O5 Mg N2 119.70(7) O5 Mg N3 84.77(7) C3 O1 C2 105.10(17) C10 O2 C11 104.95(16) C29 O3 Mg 131.47(13) C29 O3 B13 108.73(15) B13 O3 Mg 119.72(12) C30 O4 B13 107.93(16) C1 N1 Mg 127.87(14) C3 N1 Mg 124.65(14) C3 N1 C1 106.58(18) C5 N2 Mg 125.73(14) C8 N2 Mg 126.47(14) C8 N2 C5 107.75(16) C10 N3 Mg 124.87(14) C10 N3 C12 106.67(17) C12 N3 Mg 126.66(13) N1 C1 C2 102.29(17) N1 C1 C17 110.45(19) C17 C1 C2 112.3(2) O1 C2 C1 103.31(18) O1 C3 C4 115.31(19) N1 C3 O1 116.76(19) N1 C3 C4 127.8(2) C5 C4 C3 123.94(19) N2 C5 C6 109.63(18) C4 C5 N2 127.24(19) C4 C5 C6 123.12(19) C7 C6 C5 106.55(17) C7 C6 C13 121.4(2) C13 C6 C5 131.9(2) C6 C7 C8 106.73(17) C16 C7 C6 121.2(2) C16 C7 C8 132.0(2) N2 C8 C7 109.33(17) C9 C8 N2 127.36(18) C9 C8 C7 123.25(19) C8 C9 C10 124.31(19) O2 C10 C9 115.27(18) N3 C10 O2 116.38(19) N3 C10 C9 128.35(19) O2 C11 C12 103.25(16) N3 C12 C11 101.95(17) N3 C12 C23 112.42(16) C23 C12 C11 112.88(18) C14 C13 C6 117.3(2) C15 C14 C13 121.3(2) C14 C15 C16 121.2(2) C7 C16 C15 117.7(2) C18 C17 C1 121.2(2) C22 C17 C1 120.4(2) C22 C17 C18 118.3(2) C19 C18 C17 121.0(2) C18 C19 C20 120.0(3) C21 C20 C19 119.5(3) C22 C21 C20 120.9(3) C21 C22 C17 120.2(3) C24 C23 C12 119.8(2) C24 C23 C28 118.8(2) C28 C23 C12 121.5(2) C23 C24 C25 120.2(3) C26 C25 C24 120.6(3) C25 C26 C27 120.0(3) C26 C27 C28 119.9(3) C27 C28 C23 120.6(3) O3 C29 C30 102.11(16) O3 C29 C31 109.12(17) O3 C29 C32 108.26(17) C31 C29 C30 114.75(19) C32 C29 C30 112.7(2) C32 C29 C31 109.5(2) O4 C30 C29 103.28(17) O4 C30 C33 109.14(19) O4 C30 C34 109.1(2) C33 C30 C29 112.29(19) C34 C30 C29 113.8(2) C34 C30 C33 109.0(2) C35A O5 Mg 118.4(4) C35B O5 Mg 114.5(5) C35B O5 C38 111.2(6) C38 O5 Mg 133.88(13) C38 O5 C35A 106.9(5) O5 C35A C36A 103.0(7) C37A C36A C35A 100.9(8) C38 C37A C36A 103.5(7) O5 C35B C36B 102.5(8) C37B C36B C35B 102.2(12) C36B C37B C38 104.7(10) O5 C38 C37A 107.8(4) O5 C38 C37B 103.3(7) O4 B13 O3 103.31(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mg O3 1.9695(16) Mg N1 2.1628(19) Mg N2 2.1107(18) Mg N3 2.1734(19) Mg O5 2.0947(16) O1 C2 1.455(3) O1 C3 1.366(3) O2 C10 1.365(2) O2 C11 1.455(3) O3 C29 1.447(2) O3 B13 1.538(3) O4 C30 1.419(3) O4 B13 1.459(3) N1 C1 1.480(3) N1 C3 1.290(3) N2 C5 1.386(3) N2 C8 1.383(3) N3 C10 1.297(3) N3 C12 1.492(3) C1 C2 1.533(3) C1 C17 1.514(3) C3 C4 1.424(3) C4 C5 1.360(3) C5 C6 1.473(3) C6 C7 1.391(3) C6 C13 1.392(3) C7 C8 1.479(3) C7 C16 1.385(3) C8 C9 1.360(3) C9 C10 1.428(3) C11 C12 1.532(3) C12 C23 1.515(3) C13 C14 1.392(3) C14 C15 1.389(3) C15 C16 1.393(3) C17 C18 1.400(3) C17 C22 1.395(3) C18 C19 1.380(4) C19 C20 1.385(4) C20 C21 1.383(5) C21 C22 1.381(4) C23 C24 1.389(3) C23 C28 1.401(3) C24 C25 1.390(4) C25 C26 1.376(5) C26 C27 1.385(5) C27 C28 1.388(4) C29 C30 1.562(3) C29 C31 1.528(3) C29 C32 1.521(3) C30 C33 1.526(4) C30 C34 1.520(3) O5 C35A 1.461(9) O5 C35B 1.451(12) O5 C38 1.456(3) C35A C36A 1.532(11) C36A C37A 1.524(11) C37A C38 1.505(11) C35B C36B 1.513(13) C36B C37B 1.496(16) C37B C38 1.538(13) 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 C30 -163.33(14) Mg O3 C29 C31 -41.5(3) Mg O3 C29 C32 77.6(2) Mg O3 B13 O4 -175.48(13) Mg N1 C1 C2 -149.48(16) Mg N1 C1 C17 90.8(2) Mg N1 C3 O1 161.52(15) Mg N1 C3 C4 -22.4(3) Mg N2 C5 C4 -1.3(3) Mg N2 C5 C6 177.35(13) Mg N2 C8 C7 -177.43(13) Mg N2 C8 C9 -0.1(3) Mg N3 C10 O2 162.08(15) Mg N3 C10 C9 -18.0(3) Mg N3 C12 C11 -147.23(15) Mg N3 C12 C23 91.6(2) Mg O5 C35A C36A 155.7(7) Mg O5 C35B C36B -159.2(10) Mg O5 C38 C37A 179.9(7) Mg O5 C38 C37B -176.0(11) O1 C3 C4 C5 179.0(2) O2 C11 C12 N3 -25.1(2) O2 C11 C12 C23 95.7(2) O3 C29 C30 O4 -35.4(2) O3 C29 C30 C33 82.1(2) O3 C29 C30 C34 -153.5(2) N1 C1 C2 O1 -23.9(2) N1 C1 C17 C18 40.9(3) N1 C1 C17 C22 -142.2(2) N1 C3 C4 C5 2.8(4) N2 C5 C6 C7 0.2(2) N2 C5 C6 C13 -175.6(2) N2 C8 C9 C10 0.7(4) N3 C12 C23 C24 -123.0(2) N3 C12 C23 C28 58.3(3) C1 N1 C3 O1 -8.3(3) C1 N1 C3 C4 167.8(2) C1 C17 C18 C19 177.1(3) C1 C17 C22 C21 -177.4(3) C2 O1 C3 N1 -8.0(3) C2 O1 C3 C4 175.4(2) C2 C1 C17 C18 -72.6(3) C2 C1 C17 C22 104.4(3) C3 O1 C2 C1 19.8(2) C3 N1 C1 C2 19.9(2) C3 N1 C1 C17 -99.8(2) C3 C4 C5 N2 10.5(4) C3 C4 C5 C6 -168.0(2) C4 C5 C6 C7 179.0(2) C4 C5 C6 C13 3.1(4) C5 N2 C8 C7 0.1(2) C5 N2 C8 C9 177.4(2) C5 C6 C7 C8 -0.2(2) C5 C6 C7 C16 -177.39(19) C5 C6 C13 C14 176.4(2) C6 C7 C8 N2 0.0(2) C6 C7 C8 C9 -177.4(2) C6 C7 C16 C15 0.1(3) C6 C13 C14 C15 -0.3(3) C7 C6 C13 C14 1.0(3) C7 C8 C9 C10 177.7(2) C8 N2 C5 C4 -178.9(2) C8 N2 C5 C6 -0.2(2) C8 C7 C16 C15 -176.3(2) C8 C9 C10 O2 -170.5(2) C8 C9 C10 N3 9.6(4) C10 O2 C11 C12 23.7(2) C10 N3 C12 C11 18.0(2) C10 N3 C12 C23 -103.2(2) C11 O2 C10 N3 -13.7(3) C11 O2 C10 C9 166.37(19) C11 C12 C23 C24 122.4(2) C11 C12 C23 C28 -56.4(3) C12 N3 C10 O2 -3.5(3) C12 N3 C10 C9 176.5(2) C12 C23 C24 C25 -179.7(2) C12 C23 C28 C27 178.3(2) C13 C6 C7 C8 176.26(19) C13 C6 C7 C16 -1.0(3) C13 C14 C15 C16 -0.5(4) C14 C15 C16 C7 0.6(3) C16 C7 C8 N2 176.8(2) C16 C7 C8 C9 -0.6(4) C17 C1 C2 O1 94.5(2) C17 C18 C19 C20 0.1(5) C18 C17 C22 C21 -0.4(5) C18 C19 C20 C21 -0.1(6) C19 C20 C21 C22 -0.3(7) C20 C21 C22 C17 0.5(6) C22 C17 C18 C19 0.1(5) C23 C24 C25 C26 1.6(4) C24 C23 C28 C27 -0.5(4) C24 C25 C26 C27 -1.0(5) C25 C26 C27 C28 -0.4(5) C26 C27 C28 C23 1.1(4) C28 C23 C24 C25 -0.9(4) C29 O3 B13 O4 1.7(2) C30 O4 B13 O3 -25.7(2) C31 C29 C30 O4 -153.27(19) C31 C29 C30 C33 -35.8(3) C31 C29 C30 C34 88.6(3) C32 C29 C30 O4 80.5(2) C32 C29 C30 C33 -162.02(19) C32 C29 C30 C34 -37.5(3) O5 C35A C36A C37A 42.2(13) O5 C35B C36B C37B -39.0(18) C35A O5 C38 C37A 10.9(9) C35A C36A C37A C38 -35.1(13) C36A C37A C38 O5 16.0(11) C35B O5 C38 C37B -4.0(12) C35B C36B C37B C38 37(2) C36B C37B C38 O5 -21.1(19) C38 O5 C35A C36A -33.3(10) C38 O5 C35B C36B 27.1(13) B13 O3 C29 C30 19.9(2) B13 O3 C29 C31 141.74(19) B13 O3 C29 C32 -99.2(2) B13 O4 C30 C29 38.3(2) B13 O4 C30 C33 -81.3(2) B13 O4 C30 C34 159.7(2) 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 -12.9995 -9.0048 -6.9944 -0.8968 0.0275 0.4050 13.0011 -4.9972 11.9981 0.6614 0.5384 -0.5171 -9.0008 -1.0056 -21.9987 -0.4452 -0.2277 0.8738 11.9989 7.0001 -14.0065 0.9260 -0.0209 0.3709 -6.9989 -2.9967 24.0048 -0.6151 0.0059 -0.7929 2.0007 3.0062 27.0008 0.0130 -0.0083 -1.0055 3.0024 -23.0040 3.0047 -0.1712 0.9897 -0.0211 3.0024 -18.0004 16.0046 -0.1720 0.8218 -0.5146 0.0003 -12.0071 -22.9990 -0.0451 0.4220 0.8884 -9.9989 -16.0065 -9.9939 -0.7974 0.3698 0.5223 4.0004 6.0069 25.9994 0.1868 -0.0813 -1.0008 14.0008 -8.0007 -3.0027 0.7651 0.6465 0.0304 -14.0003 4.0004 6.0039 -0.8414 -0.4812 -0.1192 14.0002 -4.0012 -10.0042 0.8644 0.4720 0.2635 10.9994 12.0062 11.9947 0.7887 -0.1828 -0.5833 9.9985 11.0005 -15.0069 0.8671 -0.2296 0.4041 -3.0023 23.0044 -1.0046 0.1597 -0.9851 -0.0511 12.9996 9.0054 9.9946 0.8796 -0.0205 -0.5132