#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:16:00 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224213 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551209.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_1551209 loop_ _publ_author_name 'Li, Nan' 'Zhao, Zifeng' 'Yu, Chao' 'Wu, Botao' 'Bian, Zuqiang' 'Zhang, Wen-Xiong' 'Xi, Zhenfeng' _publ_section_title ; Alkaline-earth metallacyclic complexes bearing a diborane-bridged tetraamide ligand: synthesis, structure and fluorescence property. ; _journal_issue 25 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 9067 _journal_page_last 9071 _journal_paper_doi 10.1039/c9dt02118c _journal_volume 48 _journal_year 2019 _chemical_formula_moiety 'C44 H60 B2 Mg2 N4 O6' _chemical_formula_sum 'C44 H60 B2 Mg2 N4 O6' _chemical_formula_weight 811.20 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-04-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-04-16 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.484(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.0637(3) _cell_length_b 14.0668(6) _cell_length_c 16.2694(6) _cell_measurement_reflns_used 4777 _cell_measurement_temperature 119.99(10) _cell_measurement_theta_max 29.6310 _cell_measurement_theta_min 3.7800 _cell_volume 2070.47(14) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 119.99(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.982 _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 -10.00 27.00 0.50 24.00 -- -1.70 -82.00 120.00 74 2 \w -29.00 -2.00 0.50 24.00 -- -1.70 -82.00 -60.00 54 3 \w -4.00 30.00 0.50 24.00 -- -1.70 -82.00 30.00 68 4 \w -89.00 43.00 0.50 24.00 -- -1.70 0.00-150.00 264 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0001591000 _diffrn_orient_matrix_UB_12 0.0400993000 _diffrn_orient_matrix_UB_13 0.0263944000 _diffrn_orient_matrix_UB_21 0.0430963000 _diffrn_orient_matrix_UB_22 -0.0254513000 _diffrn_orient_matrix_UB_23 0.0304754000 _diffrn_orient_matrix_UB_31 0.0655092000 _diffrn_orient_matrix_UB_32 0.0168820000 _diffrn_orient_matrix_UB_33 -0.0168246000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 17412 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 3.575 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.301 _exptl_crystal_description block _exptl_crystal_F_000 868 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.770 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 4662 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0646 _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^)+(0.1055P)^2^+1.9235P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1752 _refine_ls_wR_factor_ref 0.1885 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3627 _reflns_number_total 4662 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_2102_a.res in P2(1)/c exp_2102.res created by SHELXL-2017/1 at 20:16:31 on 16-Apr-2019 REM Old TITL exp_2102 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.139, Rweak 0.007, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C20 O3 O4 Mg CELL 0.71073 9.0637 14.0668 16.2694 90 93.484 90 ZERR 2 0.0003 0.0006 0.0006 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B Mg N O UNIT 88 120 4 4 8 12 L.S. 4 PLAN 1 SIZE 0.1 0.1 0.1 BOND $H LIST 6 MORE -1 CONF fmap 2 acta SHEL 999 0.77 OMIT 2 1 3 OMIT 2 0 4 OMIT 0 1 3 OMIT 3 1 5 OMIT 2 3 5 OMIT -1 4 5 OMIT 3 2 1 OMIT -1 3 7 OMIT 3 1 1 OMIT -3 0 8 OMIT -1 4 1 OMIT -2 6 2 OMIT 6 1 0 OMIT 0 3 4 OMIT 0 8 3 OMIT -1 2 8 OMIT -2 6 1 OMIT 0 3 1 OMIT -1 6 2 OMIT -3 3 6 OMIT -1 1 9 OMIT -2 4 2 REM REM REM WGHT 0.105500 1.923500 FVAR 0.77459 MG1 4 0.461901 0.443631 0.647966 11.00000 0.02061 0.02239 = 0.01662 0.00121 0.00161 0.00050 O1 6 0.645267 0.514089 0.706076 11.00000 0.02298 0.02319 = 0.02657 -0.00165 -0.00393 -0.00114 O2 6 0.423500 0.407324 0.770798 11.00000 0.02208 0.04007 = 0.02136 0.00539 0.00314 -0.00109 O3 6 0.266498 0.353209 0.620819 11.00000 0.02226 0.03113 = 0.02073 -0.00349 0.00080 -0.00272 N2 5 0.618421 0.438384 0.413553 11.00000 0.01199 0.01570 = 0.01016 0.00060 0.00006 -0.00041 N1 5 0.585406 0.385074 0.558980 11.00000 0.01514 0.01464 = 0.00959 0.00005 0.00043 -0.00078 C1 1 0.836717 0.215876 0.457069 11.00000 0.01215 0.01553 = 0.01486 -0.00170 -0.00232 -0.00033 C2 1 0.897955 0.203682 0.379262 11.00000 0.01292 0.01769 = 0.02036 -0.00441 0.00004 0.00191 AFIX 43 H2 2 0.960845 0.152823 0.370861 11.00000 -1.20000 AFIX 0 C3 1 0.864240 0.267083 0.316364 11.00000 0.01529 0.02329 = 0.01401 -0.00499 0.00342 -0.00200 AFIX 43 H3 2 0.904725 0.258197 0.265756 11.00000 -1.20000 AFIX 0 C4 1 0.770639 0.344379 0.326918 11.00000 0.01731 0.01798 = 0.01053 0.00105 0.00122 -0.00068 AFIX 43 H4 2 0.749191 0.385377 0.282963 11.00000 -1.20000 AFIX 0 C5 1 0.708004 0.361671 0.402547 11.00000 0.01047 0.01584 = 0.01043 -0.00029 -0.00086 -0.00371 C6 1 0.741306 0.295311 0.468788 11.00000 0.01207 0.01296 = 0.01008 -0.00079 -0.00224 -0.00259 C7 1 0.867424 0.151566 0.523209 11.00000 0.02318 0.01861 = 0.02084 0.00038 -0.00209 0.00567 AFIX 43 H7 2 0.929998 0.100084 0.516639 11.00000 -1.20000 AFIX 0 C8 1 0.804305 0.165683 0.597006 11.00000 0.03065 0.01870 = 0.01657 0.00552 -0.00449 0.00334 AFIX 43 H8 2 0.825626 0.123336 0.639993 11.00000 -1.20000 AFIX 0 C9 1 0.708723 0.242093 0.609304 11.00000 0.02525 0.01845 = 0.01186 0.00183 0.00133 0.00134 AFIX 43 H9 2 0.666188 0.248510 0.659607 11.00000 -1.20000 AFIX 0 C10 1 0.676315 0.309020 0.546813 11.00000 0.01378 0.01531 = 0.01076 -0.00013 -0.00283 -0.00264 C11 1 0.275604 0.277734 0.560236 11.00000 0.03141 0.03136 = 0.02475 -0.00792 0.00448 -0.00949 AFIX 23 H11A 2 0.214380 0.224031 0.573644 11.00000 -1.20000 H11B 2 0.376739 0.256265 0.556780 11.00000 -1.20000 AFIX 0 C12 1 0.218119 0.324722 0.479861 11.00000 0.04133 0.06478 = 0.02288 -0.00217 -0.00480 -0.03074 AFIX 23 H12A 2 0.298952 0.351387 0.450932 11.00000 -1.20000 H12B 2 0.165731 0.279057 0.444219 11.00000 -1.20000 AFIX 0 C13 1 0.114953 0.402128 0.505586 11.00000 0.03329 0.05277 = 0.05042 0.01383 -0.01921 -0.01932 AFIX 23 H13A 2 0.145965 0.463685 0.486030 11.00000 -1.20000 H13B 2 0.014542 0.389947 0.484127 11.00000 -1.20000 AFIX 0 C14 1 0.125544 0.398579 0.598164 11.00000 0.01890 0.03660 = 0.05477 -0.00044 0.00220 -0.00425 AFIX 23 H14A 2 0.122538 0.462180 0.621038 11.00000 -1.20000 H14B 2 0.044568 0.361924 0.618284 11.00000 -1.20000 AFIX 0 C15 1 0.282232 0.405859 0.807605 11.00000 0.02484 0.03284 = 0.03055 0.00303 0.00726 0.00362 AFIX 23 H15A 2 0.230590 0.346775 0.794888 11.00000 -1.20000 H15B 2 0.220931 0.458384 0.787354 11.00000 -1.20000 AFIX 0 C16 1 0.316830 0.414882 0.898885 11.00000 0.04393 0.05120 = 0.02634 0.00449 0.00643 0.01170 AFIX 23 H16A 2 0.239143 0.387774 0.930006 11.00000 -1.20000 H16B 2 0.332541 0.480629 0.915129 11.00000 -1.20000 AFIX 0 C17 1 0.460195 0.356738 0.909528 11.00000 0.04148 0.05071 = 0.02749 0.01027 0.00609 0.01263 AFIX 23 H17A 2 0.517714 0.374924 0.959271 11.00000 -1.20000 H17B 2 0.439514 0.289141 0.911380 11.00000 -1.20000 AFIX 0 C18 1 0.539006 0.382213 0.833966 11.00000 0.02694 0.04187 = 0.02678 0.00687 0.00082 0.00204 AFIX 23 H18A 2 0.605014 0.435573 0.845081 11.00000 -1.20000 H18B 2 0.596438 0.328681 0.816098 11.00000 -1.20000 AFIX 0 C19 1 0.796602 0.481252 0.706101 11.00000 0.02362 0.02870 = 0.03255 -0.00062 -0.00292 -0.00009 AFIX 23 H19A 2 0.831982 0.483773 0.651060 11.00000 -1.20000 H19B 2 0.804963 0.416460 0.726254 11.00000 -1.20000 AFIX 0 C20 1 0.883364 0.548670 0.763137 11.00000 0.02968 0.03706 = 0.03668 0.00011 -0.00915 -0.00480 AFIX 23 H20A 2 0.985151 0.554035 0.748431 11.00000 -1.20000 H20B 2 0.881616 0.528480 0.820078 11.00000 -1.20000 AFIX 0 C21 1 0.800016 0.641923 0.748514 11.00000 0.03430 0.02935 = 0.02829 -0.00524 0.00014 -0.00814 AFIX 23 H21A 2 0.817285 0.685140 0.794554 11.00000 -1.20000 H21B 2 0.828084 0.672810 0.698495 11.00000 -1.20000 AFIX 0 C22 1 0.640311 0.609152 0.740709 11.00000 0.02985 0.02780 = 0.02834 -0.00555 0.00165 -0.00041 AFIX 23 H22A 2 0.598424 0.607894 0.794164 11.00000 -1.20000 H22B 2 0.581313 0.651097 0.704607 11.00000 -1.20000 AFIX 0 B1 3 0.556398 0.451312 0.492541 11.00000 0.01050 0.01505 = 0.00975 0.00044 -0.00030 -0.00077 HKLF 4 REM exp_2102_a.res in P2(1)/c REM R1 = 0.0646 for 3627 Fo > 4sig(Fo) and 0.0849 for all 4662 data REM 262 parameters refined using 0 restraints END WGHT 0.1055 1.9235 REM Highest difference peak 0.770, deepest hole -0.462, 1-sigma level 0.088 Q1 1 0.5017 0.4450 0.7366 11.00000 0.05 0.77 REM The information below was added by Olex2. REM REM R1 = 0.0646 for 3627 Fo > 4sig(Fo) and 0.0849 for all 18939 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.77, deepest hole -0.46 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0849 REM R1_gt = 0.0646 REM wR_ref = 0.1885 REM GOOF = 1.056 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 18939 REM Reflections_gt = 3627 REM Parameters = n/a REM Hole = -0.46 REM Peak = 0.77 REM Flack = n/a ; _cod_data_source_file c9dt02118c2.cif _cod_data_source_block 2b _cod_depositor_comments 'Adding full bibliography for 1551209--1551214.cif.' _cod_database_code 1551209 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'C H O N Mg B' _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 0.989 _shelx_estimated_absorpt_t_min 0.989 _reflns_odcompleteness_completeness 98.32 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: 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) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9) ; _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.458 _oxdiff_exptl_absorpt_empirical_full_min 0.795 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 Mg1 Mg 0.46190(9) 0.44363(6) 0.64797(5) 0.0199(2) Uani 1 1 d . O1 O 0.64527(18) 0.51409(12) 0.70608(11) 0.0245(4) Uani 1 1 d . O2 O 0.42350(19) 0.40732(14) 0.77080(11) 0.0278(4) Uani 1 1 d . O3 O 0.26650(18) 0.35321(13) 0.62082(11) 0.0247(4) Uani 1 1 d . N2 N 0.61842(19) 0.43838(12) 0.41355(10) 0.0126(4) Uani 1 1 d . N1 N 0.58541(19) 0.38507(13) 0.55898(10) 0.0131(4) Uani 1 1 d . C1 C 0.8367(2) 0.21588(15) 0.45707(13) 0.0143(4) Uani 1 1 d . C2 C 0.8980(2) 0.20368(16) 0.37926(14) 0.0170(4) Uani 1 1 d . H2 H 0.960845 0.152823 0.370861 0.020 Uiso 1 1 calc R C3 C 0.8642(2) 0.26708(17) 0.31636(13) 0.0174(4) Uani 1 1 d . H3 H 0.904725 0.258197 0.265756 0.021 Uiso 1 1 calc R C4 C 0.7706(2) 0.34438(16) 0.32692(13) 0.0153(4) Uani 1 1 d . H4 H 0.749191 0.385377 0.282963 0.018 Uiso 1 1 calc R C5 C 0.7080(2) 0.36167(15) 0.40255(12) 0.0123(4) Uani 1 1 d . C6 C 0.7413(2) 0.29531(14) 0.46879(12) 0.0118(4) Uani 1 1 d . C7 C 0.8674(3) 0.15157(17) 0.52321(15) 0.0210(5) Uani 1 1 d . H7 H 0.929998 0.100084 0.516639 0.025 Uiso 1 1 calc R C8 C 0.8043(3) 0.16568(17) 0.59701(14) 0.0222(5) Uani 1 1 d . H8 H 0.825626 0.123336 0.639993 0.027 Uiso 1 1 calc R C9 C 0.7087(3) 0.24209(16) 0.60930(13) 0.0185(5) Uani 1 1 d . H9 H 0.666188 0.248510 0.659607 0.022 Uiso 1 1 calc R C10 C 0.6763(2) 0.30902(15) 0.54681(12) 0.0134(4) Uani 1 1 d . C11 C 0.2756(3) 0.2777(2) 0.56024(16) 0.0291(6) Uani 1 1 d . H11A H 0.214380 0.224031 0.573644 0.035 Uiso 1 1 calc R H11B H 0.376739 0.256265 0.556780 0.035 Uiso 1 1 calc R C12 C 0.2181(4) 0.3247(3) 0.47986(18) 0.0433(8) Uani 1 1 d . H12A H 0.298952 0.351387 0.450932 0.052 Uiso 1 1 calc R H12B H 0.165731 0.279057 0.444219 0.052 Uiso 1 1 calc R C13 C 0.1150(3) 0.4021(3) 0.5056(2) 0.0464(8) Uani 1 1 d . H13A H 0.145965 0.463685 0.486030 0.056 Uiso 1 1 calc R H13B H 0.014542 0.389947 0.484127 0.056 Uiso 1 1 calc R C14 C 0.1255(3) 0.3986(2) 0.5982(2) 0.0368(7) Uani 1 1 d . H14A H 0.122538 0.462180 0.621038 0.044 Uiso 1 1 calc R H14B H 0.044568 0.361924 0.618284 0.044 Uiso 1 1 calc R C15 C 0.2822(3) 0.4059(2) 0.80760(17) 0.0292(6) Uani 1 1 d . H15A H 0.230590 0.346775 0.794888 0.035 Uiso 1 1 calc R H15B H 0.220931 0.458384 0.787354 0.035 Uiso 1 1 calc R C16 C 0.3168(4) 0.4149(3) 0.89888(18) 0.0403(7) Uani 1 1 d . H16A H 0.239143 0.387774 0.930006 0.048 Uiso 1 1 calc R H16B H 0.332541 0.480629 0.915129 0.048 Uiso 1 1 calc R C17 C 0.4602(3) 0.3567(2) 0.90953(18) 0.0397(7) Uani 1 1 d . H17A H 0.517714 0.374924 0.959271 0.048 Uiso 1 1 calc R H17B H 0.439514 0.289141 0.911380 0.048 Uiso 1 1 calc R C18 C 0.5390(3) 0.3822(2) 0.83397(17) 0.0319(6) Uani 1 1 d . H18A H 0.605014 0.435573 0.845081 0.038 Uiso 1 1 calc R H18B H 0.596438 0.328681 0.816098 0.038 Uiso 1 1 calc R C19 C 0.7966(3) 0.48125(19) 0.70610(17) 0.0285(6) Uani 1 1 d . H19A H 0.831982 0.483773 0.651060 0.034 Uiso 1 1 calc R H19B H 0.804963 0.416460 0.726254 0.034 Uiso 1 1 calc R C20 C 0.8834(3) 0.5487(2) 0.76314(19) 0.0349(6) Uani 1 1 d . H20A H 0.985151 0.554035 0.748431 0.042 Uiso 1 1 calc R H20B H 0.881616 0.528480 0.820078 0.042 Uiso 1 1 calc R C21 C 0.8000(3) 0.6419(2) 0.74851(17) 0.0307(6) Uani 1 1 d . H21A H 0.817285 0.685140 0.794554 0.037 Uiso 1 1 calc R H21B H 0.828084 0.672810 0.698495 0.037 Uiso 1 1 calc R C22 C 0.6403(3) 0.60915(19) 0.74071(17) 0.0287(6) Uani 1 1 d . H22A H 0.598424 0.607894 0.794164 0.034 Uiso 1 1 calc R H22B H 0.581313 0.651097 0.704607 0.034 Uiso 1 1 calc R B1 B 0.5564(2) 0.45131(17) 0.49254(14) 0.0118(4) Uani 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 Mg1 0.0206(4) 0.0224(4) 0.0166(4) 0.0012(3) 0.0016(3) 0.0005(3) O1 0.0230(8) 0.0232(9) 0.0266(9) -0.0017(7) -0.0039(7) -0.0011(7) O2 0.0221(8) 0.0401(11) 0.0214(9) 0.0054(8) 0.0031(7) -0.0011(8) O3 0.0223(8) 0.0311(9) 0.0207(8) -0.0035(7) 0.0008(7) -0.0027(7) N2 0.0120(8) 0.0157(9) 0.0102(8) 0.0006(7) 0.0001(6) -0.0004(6) N1 0.0151(8) 0.0146(8) 0.0096(8) 0.0000(7) 0.0004(6) -0.0008(7) C1 0.0121(9) 0.0155(10) 0.0149(10) -0.0017(8) -0.0023(7) -0.0003(8) C2 0.0129(9) 0.0177(10) 0.0204(11) -0.0044(8) 0.0000(8) 0.0019(8) C3 0.0153(10) 0.0233(11) 0.0140(10) -0.0050(8) 0.0034(8) -0.0020(8) C4 0.0173(10) 0.0180(10) 0.0105(10) 0.0011(8) 0.0012(8) -0.0007(8) C5 0.0105(9) 0.0158(10) 0.0104(9) -0.0003(8) -0.0009(7) -0.0037(7) C6 0.0121(9) 0.0130(9) 0.0101(9) -0.0008(7) -0.0022(7) -0.0026(7) C7 0.0232(11) 0.0186(11) 0.0208(11) 0.0004(9) -0.0021(9) 0.0057(9) C8 0.0307(12) 0.0187(11) 0.0166(11) 0.0055(9) -0.0045(9) 0.0033(9) C9 0.0252(11) 0.0185(11) 0.0119(10) 0.0018(8) 0.0013(8) 0.0013(9) C10 0.0138(9) 0.0153(10) 0.0108(9) -0.0001(8) -0.0028(7) -0.0026(8) C11 0.0314(13) 0.0314(14) 0.0247(13) -0.0079(11) 0.0045(10) -0.0095(11) C12 0.0413(16) 0.065(2) 0.0229(14) -0.0022(14) -0.0048(12) -0.0307(15) C13 0.0333(15) 0.0528(19) 0.0504(19) 0.0138(16) -0.0192(14) -0.0193(14) C14 0.0189(12) 0.0366(15) 0.0548(19) -0.0004(14) 0.0022(12) -0.0043(11) C15 0.0248(12) 0.0328(14) 0.0305(14) 0.0030(11) 0.0073(10) 0.0036(10) C16 0.0439(17) 0.0512(18) 0.0263(14) 0.0045(13) 0.0064(12) 0.0117(14) C17 0.0415(16) 0.0507(18) 0.0275(14) 0.0103(13) 0.0061(12) 0.0126(14) C18 0.0269(12) 0.0419(16) 0.0268(13) 0.0069(11) 0.0008(10) 0.0020(11) C19 0.0236(12) 0.0287(13) 0.0325(14) -0.0006(11) -0.0029(10) -0.0001(10) C20 0.0297(14) 0.0371(15) 0.0367(15) 0.0001(12) -0.0091(11) -0.0048(11) C21 0.0343(14) 0.0294(14) 0.0283(13) -0.0052(11) 0.0001(11) -0.0081(11) C22 0.0298(13) 0.0278(13) 0.0283(13) -0.0056(11) 0.0017(10) -0.0004(10) B1 0.0105(10) 0.0150(11) 0.0097(10) 0.0004(8) -0.0003(8) -0.0008(8) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Mg1 O2 81.96(7) . . O1 Mg1 O3 164.40(8) . . O1 Mg1 B1 96.54(7) . . O1 Mg1 B1 97.33(7) . 3_666 O2 Mg1 O3 82.73(7) . . O2 Mg1 B1 157.22(8) . 3_666 O2 Mg1 B1 165.54(8) . . O3 Mg1 B1 97.54(7) . . O3 Mg1 B1 97.93(7) . 3_666 N2 Mg1 O1 94.89(7) 3_666 . N2 Mg1 O2 125.74(8) 3_666 . N2 Mg1 O3 96.45(8) 3_666 . N2 Mg1 N1 99.97(8) 3_666 . N2 Mg1 B1 31.48(7) 3_666 3_666 N2 Mg1 B1 68.68(7) 3_666 . N1 Mg1 O1 93.21(7) . . N1 Mg1 O2 134.25(8) . . N1 Mg1 O3 95.34(7) . . N1 Mg1 B1 31.31(7) . . N1 Mg1 B1 68.51(7) . 3_666 B1 Mg1 B1 37.20(9) 3_666 . C19 O1 Mg1 124.83(15) . . C19 O1 C22 110.20(18) . . C22 O1 Mg1 124.36(15) . . C15 O2 Mg1 126.60(15) . . C15 O2 C18 108.60(19) . . C18 O2 Mg1 124.77(15) . . C11 O3 Mg1 118.63(14) . . C11 O3 C14 103.5(2) . . C14 O3 Mg1 118.70(16) . . C5 N2 Mg1 140.42(14) . 3_666 C5 N2 B1 118.78(17) . . B1 N2 Mg1 100.76(13) . 3_666 C10 N1 Mg1 140.50(15) . . C10 N1 B1 118.71(17) . . B1 N1 Mg1 100.78(13) . . C2 C1 C6 118.92(19) . . C7 C1 C2 121.87(19) . . C7 C1 C6 119.21(19) . . C1 C2 H2 119.9 . . C3 C2 C1 120.12(19) . . C3 C2 H2 119.9 . . C2 C3 H3 119.3 . . C2 C3 C4 121.5(2) . . C4 C3 H3 119.3 . . C3 C4 H4 119.2 . . C3 C4 C5 121.5(2) . . C5 C4 H4 119.2 . . N2 C5 C4 121.65(19) . . N2 C5 C6 120.72(18) . . C4 C5 C6 117.63(18) . . C1 C6 C5 120.36(18) . . C1 C6 C10 120.18(18) . . C5 C6 C10 119.46(18) . . C1 C7 H7 120.1 . . C8 C7 C1 119.8(2) . . C8 C7 H7 120.1 . . C7 C8 H8 119.0 . . C7 C8 C9 121.9(2) . . C9 C8 H8 119.0 . . C8 C9 H9 119.5 . . C8 C9 C10 121.0(2) . . C10 C9 H9 119.5 . . N1 C10 C6 120.76(18) . . N1 C10 C9 121.31(19) . . C9 C10 C6 117.93(19) . . O3 C11 H11A 111.1 . . O3 C11 H11B 111.1 . . O3 C11 C12 103.5(2) . . H11A C11 H11B 109.0 . . C12 C11 H11A 111.1 . . C12 C11 H11B 111.1 . . C11 C12 H12A 110.7 . . C11 C12 H12B 110.7 . . H12A C12 H12B 108.8 . . C13 C12 C11 105.0(2) . . C13 C12 H12A 110.7 . . C13 C12 H12B 110.7 . . C12 C13 H13A 110.8 . . C12 C13 H13B 110.8 . . H13A C13 H13B 108.9 . . C14 C13 C12 104.5(3) . . C14 C13 H13A 110.8 . . C14 C13 H13B 110.8 . . O3 C14 C13 105.7(2) . . O3 C14 H14A 110.6 . . O3 C14 H14B 110.6 . . C13 C14 H14A 110.6 . . C13 C14 H14B 110.6 . . H14A C14 H14B 108.7 . . O2 C15 H15A 110.6 . . O2 C15 H15B 110.6 . . O2 C15 C16 105.7(2) . . H15A C15 H15B 108.7 . . C16 C15 H15A 110.6 . . C16 C15 H15B 110.6 . . C15 C16 H16A 111.6 . . C15 C16 H16B 111.6 . . C15 C16 C17 101.0(2) . . H16A C16 H16B 109.4 . . C17 C16 H16A 111.6 . . C17 C16 H16B 111.6 . . C16 C17 H17A 111.2 . . C16 C17 H17B 111.2 . . H17A C17 H17B 109.1 . . C18 C17 C16 102.8(2) . . C18 C17 H17A 111.2 . . C18 C17 H17B 111.2 . . O2 C18 C17 106.1(2) . . O2 C18 H18A 110.5 . . O2 C18 H18B 110.5 . . C17 C18 H18A 110.5 . . C17 C18 H18B 110.5 . . H18A C18 H18B 108.7 . . O1 C19 H19A 110.8 . . O1 C19 H19B 110.8 . . O1 C19 C20 104.9(2) . . H19A C19 H19B 108.8 . . C20 C19 H19A 110.8 . . C20 C19 H19B 110.8 . . C19 C20 H20A 111.4 . . C19 C20 H20B 111.4 . . C19 C20 C21 102.1(2) . . H20A C20 H20B 109.2 . . C21 C20 H20A 111.4 . . C21 C20 H20B 111.4 . . C20 C21 H21A 111.3 . . C20 C21 H21B 111.3 . . H21A C21 H21B 109.2 . . C22 C21 C20 102.3(2) . . C22 C21 H21A 111.3 . . C22 C21 H21B 111.3 . . O1 C22 C21 105.1(2) . . O1 C22 H22A 110.7 . . O1 C22 H22B 110.7 . . C21 C22 H22A 110.7 . . C21 C22 H22B 110.7 . . H22A C22 H22B 108.8 . . Mg1 B1 Mg1 142.80(9) 3_666 . N2 B1 Mg1 169.39(16) . . N2 B1 Mg1 47.76(10) . 3_666 N2 B1 B1 119.2(2) . 3_666 N1 B1 Mg1 169.27(15) . 3_666 N1 B1 Mg1 47.91(10) . . N1 B1 N2 121.55(18) . . N1 B1 B1 119.2(2) . 3_666 B1 B1 Mg1 71.33(14) 3_666 . B1 B1 Mg1 71.47(14) 3_666 3_666 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mg1 O1 2.1089(18) . Mg1 O2 2.1119(19) . Mg1 O3 2.2033(19) . Mg1 N2 2.0489(19) 3_666 Mg1 N1 2.0554(19) . Mg1 B1 2.719(2) 3_666 Mg1 B1 2.721(2) . O1 C19 1.447(3) . O1 C22 1.453(3) . O2 C15 1.446(3) . O2 C18 1.465(3) . O3 C11 1.454(3) . O3 C14 1.455(3) . N2 C5 1.369(3) . N2 B1 1.445(3) . N1 C10 1.372(3) . N1 B1 1.439(3) . C1 C2 1.423(3) . C1 C6 1.433(3) . C1 C7 1.420(3) . C2 H2 0.9300 . C2 C3 1.378(3) . C3 H3 0.9300 . C3 C4 1.396(3) . C4 H4 0.9300 . C4 C5 1.407(3) . C5 C6 1.444(3) . C6 C10 1.444(3) . C7 H7 0.9300 . C7 C8 1.375(3) . C8 H8 0.9300 . C8 C9 1.402(3) . C9 H9 0.9300 . C9 C10 1.404(3) . C11 H11A 0.9700 . C11 H11B 0.9700 . C11 C12 1.528(4) . C12 H12A 0.9700 . C12 H12B 0.9700 . C12 C13 1.511(5) . C13 H13A 0.9700 . C13 H13B 0.9700 . C13 C14 1.504(5) . C14 H14A 0.9700 . C14 H14B 0.9700 . C15 H15A 0.9700 . C15 H15B 0.9700 . C15 C16 1.504(4) . C16 H16A 0.9700 . C16 H16B 0.9700 . C16 C17 1.536(4) . C17 H17A 0.9700 . C17 H17B 0.9700 . C17 C18 1.502(4) . C18 H18A 0.9700 . C18 H18B 0.9700 . C19 H19A 0.9700 . C19 H19B 0.9700 . C19 C20 1.513(4) . C20 H20A 0.9700 . C20 H20B 0.9700 . C20 C21 1.525(4) . C21 H21A 0.9700 . C21 H21B 0.9700 . C21 C22 1.517(4) . C22 H22A 0.9700 . C22 H22B 0.9700 . B1 B1 1.735(5) 3_666 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Mg1 O1 C19 C20 -173.73(17) . . Mg1 O1 C22 C21 -161.38(16) . . Mg1 O2 C15 C16 -157.84(19) . . Mg1 O2 C18 C17 -176.90(19) . . Mg1 O3 C11 C12 -92.5(2) . . Mg1 O3 C14 C13 93.6(2) . . Mg1 N2 C5 C4 -3.7(3) 3_666 . Mg1 N2 C5 C6 176.36(16) 3_666 . Mg1 N2 B1 Mg1 175.3(8) 3_666 . Mg1 N2 B1 N1 -178.75(17) 3_666 . Mg1 N2 B1 B1 1.6(3) 3_666 3_666 Mg1 N1 C10 C6 179.24(16) . . Mg1 N1 C10 C9 -0.5(3) . . Mg1 N1 B1 Mg1 176.5(8) . 3_666 Mg1 N1 B1 N2 -178.52(17) . . Mg1 N1 B1 B1 1.2(3) . 3_666 O1 C19 C20 C21 -33.4(3) . . O2 C15 C16 C17 -36.3(3) . . O3 C11 C12 C13 -27.1(3) . . N2 C5 C6 C1 -179.19(18) . . N2 C5 C6 C10 1.5(3) . . C1 C2 C3 C4 0.2(3) . . C1 C6 C10 N1 179.65(18) . . C1 C6 C10 C9 -0.6(3) . . C1 C7 C8 C9 0.4(4) . . C2 C1 C6 C5 0.1(3) . . C2 C1 C6 C10 179.38(18) . . C2 C1 C7 C8 -179.3(2) . . C2 C3 C4 C5 0.8(3) . . C3 C4 C5 N2 178.76(19) . . C3 C4 C5 C6 -1.3(3) . . C4 C5 C6 C1 0.9(3) . . C4 C5 C6 C10 -178.44(18) . . C5 N2 B1 Mg1 -6.7(9) . . C5 N2 B1 Mg1 178.0(2) . 3_666 C5 N2 B1 N1 -0.7(3) . . C5 N2 B1 B1 179.6(2) . 3_666 C5 C6 C10 N1 -1.0(3) . . C5 C6 C10 C9 178.75(18) . . C6 C1 C2 C3 -0.6(3) . . C6 C1 C7 C8 0.7(3) . . C7 C1 C2 C3 179.3(2) . . C7 C1 C6 C5 -179.88(19) . . C7 C1 C6 C10 -0.6(3) . . C7 C8 C9 C10 -1.6(4) . . C8 C9 C10 N1 -178.6(2) . . C8 C9 C10 C6 1.6(3) . . C10 N1 B1 Mg1 179.7(2) . . C10 N1 B1 Mg1 -3.8(9) . 3_666 C10 N1 B1 N2 1.1(3) . . C10 N1 B1 B1 -179.2(2) . 3_666 C11 O3 C14 C13 -40.3(3) . . C11 C12 C13 C14 3.0(3) . . C12 C13 C14 O3 22.4(3) . . C14 O3 C11 C12 41.4(2) . . C15 O2 C18 C17 4.9(3) . . C15 C16 C17 C18 38.5(3) . . C16 C17 C18 O2 -27.4(3) . . C18 O2 C15 C16 20.3(3) . . C19 O1 C22 C21 10.0(3) . . C19 C20 C21 C22 38.9(3) . . C20 C21 C22 O1 -30.5(3) . . C22 O1 C19 C20 14.9(3) . . B1 N2 C5 C4 179.30(18) . . B1 N2 C5 C6 -0.6(3) . . B1 N1 C10 C6 -0.3(3) . . B1 N1 C10 C9 179.97(19) . .