# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sjoerd Harder' _publ_contact_author_email SJOERD.HARDER@UNI-DUE.DE _publ_section_title ; Synthesis and Structure of a Magnesium-Amidoborane Complex and its Role in Catalytic Formation of a New bis-Aminoborane Ligand ; loop_ _publ_author_name 'Sjoerd Harder' 'Michael Bolte' 'Jan Spielmann' # Attachment 'hasj158.cif' data_harder1-hasj158 _database_code_depnum_ccdc_archive 'CCDC 741201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((DIPP-nacnac)MgBH4)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H90 B2 Mg2 N4' _chemical_formula_weight 913.58 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3266(11) _cell_length_b 13.9025(8) _cell_length_c 15.1584(13) _cell_angle_alpha 90.00 _cell_angle_beta 106.287(6) _cell_angle_gamma 90.00 _cell_volume 2898.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17122 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9738 _exptl_absorpt_correction_T_max 0.9768 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 18615 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 25.57 _reflns_number_total 5409 _reflns_number_gt 4369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.4462P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0139(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5409 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.56217(3) 0.57521(4) 0.59724(3) 0.02313(15) Uani 1 1 d . . . B1 B 0.58094(13) 0.40459(14) 0.54449(12) 0.0307(4) Uani 1 1 d . . . H1A H 0.5067(14) 0.3618(15) 0.5171(14) 0.052(6) Uiso 1 1 d . . . H1B H 0.5805(13) 0.4684(14) 0.4932(13) 0.042(5) Uiso 1 1 d . . . H1C H 0.6442(13) 0.3591(14) 0.5545(13) 0.043(5) Uiso 1 1 d . . . H1D H 0.5790(13) 0.4362(14) 0.6134(13) 0.043(5) Uiso 1 1 d . . . N1 N 0.52260(8) 0.60515(9) 0.71313(8) 0.0245(3) Uani 1 1 d . . . N2 N 0.68711(8) 0.65434(9) 0.63319(8) 0.0238(3) Uani 1 1 d . . . C1 C 0.58929(10) 0.63345(12) 0.78986(10) 0.0285(3) Uani 1 1 d . . . C2 C 0.68501(10) 0.66044(13) 0.79287(10) 0.0323(4) Uani 1 1 d . . . H2 H 0.7278 0.6679 0.8529 0.039 Uiso 1 1 calc R . . C3 C 0.72730(10) 0.67811(12) 0.72114(10) 0.0290(3) Uani 1 1 d . . . C4 C 0.56458(12) 0.64109(16) 0.88066(11) 0.0440(5) Uani 1 1 d . . . H4A H 0.5055 0.6040 0.8773 0.066 Uiso 0.50 1 calc PR . . H4B H 0.5537 0.7087 0.8932 0.066 Uiso 0.50 1 calc PR . . H4C H 0.6186 0.6156 0.9301 0.066 Uiso 0.50 1 calc PR . . H4D H 0.6130 0.6815 0.9231 0.066 Uiso 0.50 1 calc PR . . H4E H 0.5648 0.5768 0.9072 0.066 Uiso 0.50 1 calc PR . . H4F H 0.5000 0.6699 0.8703 0.066 Uiso 0.50 1 calc PR . . C5 C 0.82494(12) 0.72906(17) 0.75028(12) 0.0491(5) Uani 1 1 d . . . H5A H 0.8549 0.7277 0.6996 0.074 Uiso 0.50 1 calc PR . . H5B H 0.8675 0.6964 0.8039 0.074 Uiso 0.50 1 calc PR . . H5C H 0.8154 0.7960 0.7662 0.074 Uiso 0.50 1 calc PR . . H5D H 0.8370 0.7523 0.8135 0.074 Uiso 0.50 1 calc PR . . H5E H 0.8243 0.7837 0.7092 0.074 Uiso 0.50 1 calc PR . . H5F H 0.8765 0.6841 0.7469 0.074 Uiso 0.50 1 calc PR . . C11 C 0.42347(10) 0.59299(12) 0.71782(9) 0.0276(3) Uani 1 1 d . . . C12 C 0.39409(10) 0.50651(13) 0.75065(10) 0.0326(4) Uani 1 1 d . . . C13 C 0.29802(11) 0.50067(15) 0.75598(12) 0.0424(4) Uani 1 1 d . . . H13 H 0.2768 0.4434 0.7786 0.051 Uiso 1 1 calc R . . C14 C 0.23365(12) 0.57584(16) 0.72925(12) 0.0471(5) Uani 1 1 d . . . H14 H 0.1696 0.5709 0.7354 0.057 Uiso 1 1 calc R . . C15 C 0.26247(11) 0.65854(15) 0.69352(12) 0.0430(5) Uani 1 1 d . . . H15 H 0.2170 0.7093 0.6737 0.052 Uiso 1 1 calc R . . C16 C 0.35722(10) 0.66921(13) 0.68593(10) 0.0325(4) Uani 1 1 d . . . C17 C 0.46059(11) 0.41929(14) 0.77746(12) 0.0391(4) Uani 1 1 d . . . H17 H 0.5260 0.4373 0.7713 0.047 Uiso 1 1 calc R . . C18 C 0.38812(12) 0.76002(13) 0.64567(12) 0.0385(4) Uani 1 1 d . . . H18 H 0.4394 0.7407 0.6159 0.046 Uiso 1 1 calc R . . C21 C 0.73252(10) 0.68986(11) 0.56560(10) 0.0277(3) Uani 1 1 d . . . C22 C 0.80325(11) 0.63464(14) 0.54007(11) 0.0357(4) Uani 1 1 d . . . C23 C 0.84297(12) 0.67245(18) 0.47234(13) 0.0521(5) Uani 1 1 d . . . H23 H 0.8902 0.6362 0.4535 0.062 Uiso 1 1 calc R . . C24 C 0.81476(14) 0.76108(19) 0.43261(13) 0.0588(6) Uani 1 1 d . . . H24 H 0.8427 0.7852 0.3872 0.071 Uiso 1 1 calc R . . C25 C 0.74674(14) 0.81403(17) 0.45859(14) 0.0534(5) Uani 1 1 d . . . H25 H 0.7281 0.8750 0.4309 0.064 Uiso 1 1 calc R . . C26 C 0.70376(12) 0.78083(13) 0.52498(12) 0.0391(4) Uani 1 1 d . . . C27 C 0.84034(13) 0.53991(15) 0.58575(13) 0.0464(5) Uani 1 1 d . . . H27 H 0.8023 0.5230 0.6297 0.056 Uiso 1 1 calc R . . C28 C 0.62960(15) 0.84322(14) 0.55334(16) 0.0533(5) Uani 1 1 d . . . H28 H 0.6028 0.8047 0.5964 0.064 Uiso 1 1 calc R . . C171 C 0.42176(13) 0.33595(15) 0.71179(15) 0.0485(5) Uani 1 1 d . . . H17A H 0.4648 0.2802 0.7297 0.073 Uiso 1 1 calc R . . H17B H 0.4193 0.3552 0.6490 0.073 Uiso 1 1 calc R . . H17C H 0.3563 0.3189 0.7146 0.073 Uiso 1 1 calc R . . C172 C 0.47353(15) 0.38659(19) 0.87747(14) 0.0603(6) Uani 1 1 d . . . H17D H 0.4980 0.4404 0.9193 0.090 Uiso 1 1 calc R . . H17E H 0.5200 0.3332 0.8922 0.090 Uiso 1 1 calc R . . H17F H 0.4108 0.3654 0.8844 0.090 Uiso 1 1 calc R . . C181 C 0.43401(16) 0.83426(15) 0.71951(15) 0.0583(6) Uani 1 1 d . . . H18A H 0.4532 0.8911 0.6905 0.087 Uiso 1 1 calc R . . H18B H 0.4915 0.8063 0.7631 0.087 Uiso 1 1 calc R . . H18C H 0.3867 0.8530 0.7522 0.087 Uiso 1 1 calc R . . C182 C 0.30556(14) 0.80681(15) 0.57084(13) 0.0497(5) Uani 1 1 d . . . H18D H 0.3301 0.8644 0.5474 0.075 Uiso 1 1 calc R . . H18E H 0.2527 0.8249 0.5969 0.075 Uiso 1 1 calc R . . H18F H 0.2812 0.7611 0.5204 0.075 Uiso 1 1 calc R . . C271 C 0.83047(17) 0.45834(19) 0.51617(19) 0.0694(7) Uani 1 1 d . . . H27A H 0.8551 0.3985 0.5486 0.104 Uiso 1 1 calc R . . H27B H 0.8682 0.4739 0.4732 0.104 Uiso 1 1 calc R . . H27C H 0.7619 0.4503 0.4821 0.104 Uiso 1 1 calc R . . C272 C 0.94963(17) 0.5489(2) 0.6398(2) 0.0798(8) Uani 1 1 d . . . H27D H 0.9730 0.4873 0.6691 0.120 Uiso 1 1 calc R . . H27E H 0.9574 0.5988 0.6870 0.120 Uiso 1 1 calc R . . H27F H 0.9874 0.5664 0.5974 0.120 Uiso 1 1 calc R . . C281 C 0.6768(2) 0.9336(2) 0.6047(2) 0.1005(11) Uani 1 1 d . . . H28A H 0.6275 0.9715 0.6229 0.151 Uiso 1 1 calc R . . H28B H 0.7047 0.9724 0.5644 0.151 Uiso 1 1 calc R . . H28C H 0.7283 0.9149 0.6596 0.151 Uiso 1 1 calc R . . C282 C 0.54437(16) 0.87109(17) 0.47092(19) 0.0674(7) Uani 1 1 d . . . H28D H 0.4979 0.9102 0.4920 0.101 Uiso 1 1 calc R . . H28E H 0.5120 0.8127 0.4410 0.101 Uiso 1 1 calc R . . H28F H 0.5687 0.9082 0.4270 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0223(2) 0.0259(3) 0.0205(2) -0.00307(19) 0.00491(18) -0.00235(18) B1 0.0345(9) 0.0299(10) 0.0245(8) -0.0011(7) 0.0030(7) 0.0048(7) N1 0.0199(5) 0.0317(7) 0.0211(6) -0.0027(5) 0.0043(4) -0.0001(5) N2 0.0214(5) 0.0269(7) 0.0225(6) -0.0012(5) 0.0049(4) -0.0009(5) C1 0.0243(7) 0.0382(9) 0.0214(7) -0.0030(6) 0.0039(5) -0.0001(6) C2 0.0248(7) 0.0480(10) 0.0200(7) -0.0047(7) -0.0003(6) -0.0040(7) C3 0.0209(7) 0.0359(9) 0.0274(8) -0.0044(6) 0.0021(6) -0.0021(6) C4 0.0339(8) 0.0735(14) 0.0238(8) -0.0104(8) 0.0067(6) -0.0081(8) C5 0.0321(8) 0.0775(15) 0.0358(9) -0.0134(9) 0.0063(7) -0.0226(9) C11 0.0208(6) 0.0427(9) 0.0186(7) -0.0077(6) 0.0043(5) -0.0002(6) C12 0.0250(7) 0.0486(10) 0.0234(7) -0.0019(7) 0.0055(6) -0.0032(7) C13 0.0286(8) 0.0660(13) 0.0344(9) -0.0008(8) 0.0117(7) -0.0085(8) C14 0.0242(8) 0.0787(15) 0.0406(10) -0.0115(10) 0.0127(7) -0.0019(8) C15 0.0263(8) 0.0625(13) 0.0382(9) -0.0146(9) 0.0057(7) 0.0103(8) C16 0.0263(7) 0.0440(10) 0.0256(8) -0.0117(7) 0.0044(6) 0.0043(7) C17 0.0270(7) 0.0504(11) 0.0384(9) 0.0114(8) 0.0068(6) -0.0050(7) C18 0.0360(8) 0.0384(10) 0.0381(9) -0.0078(7) 0.0052(7) 0.0108(7) C21 0.0225(7) 0.0340(9) 0.0245(7) -0.0015(6) 0.0030(5) -0.0069(6) C22 0.0257(7) 0.0526(11) 0.0279(8) -0.0039(7) 0.0061(6) -0.0019(7) C23 0.0308(8) 0.0933(17) 0.0339(9) -0.0028(10) 0.0120(7) -0.0035(9) C24 0.0406(10) 0.0988(19) 0.0356(10) 0.0176(11) 0.0083(8) -0.0206(11) C25 0.0478(10) 0.0608(13) 0.0456(11) 0.0198(10) 0.0033(8) -0.0159(9) C26 0.0370(8) 0.0386(10) 0.0369(9) 0.0060(7) 0.0024(7) -0.0099(7) C27 0.0427(9) 0.0500(12) 0.0468(10) -0.0057(9) 0.0131(8) 0.0120(8) C28 0.0588(12) 0.0336(10) 0.0635(13) 0.0088(9) 0.0104(10) 0.0067(9) C171 0.0407(9) 0.0481(12) 0.0577(12) 0.0049(9) 0.0156(8) -0.0018(8) C172 0.0531(11) 0.0755(16) 0.0446(11) 0.0214(11) 0.0009(9) -0.0072(11) C181 0.0630(13) 0.0425(12) 0.0570(13) -0.0121(10) -0.0035(10) 0.0034(9) C182 0.0499(10) 0.0495(12) 0.0446(11) -0.0039(9) 0.0048(8) 0.0186(9) C271 0.0564(12) 0.0709(16) 0.0891(18) -0.0332(14) 0.0338(12) -0.0048(11) C272 0.0603(14) 0.0762(18) 0.0803(17) -0.0004(14) -0.0173(12) 0.0182(12) C281 0.102(2) 0.0647(18) 0.105(2) -0.0306(16) -0.0196(17) 0.0213(15) C282 0.0536(12) 0.0467(13) 0.0886(18) 0.0038(12) -0.0022(11) 0.0069(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N1 2.0345(13) . ? Mg1 N2 2.0406(12) . ? Mg1 B1 2.5352(18) 3_666 ? Mg1 B1 2.5414(19) . ? Mg1 Mg1 3.6457(9) 3_666 ? Mg1 H1B 2.235(19) . ? Mg1 H1D 1.955(19) . ? B1 Mg1 2.5352(17) 3_666 ? B1 H1A 1.19(2) . ? B1 H1B 1.178(19) . ? B1 H1C 1.080(19) . ? B1 H1D 1.141(19) . ? N1 C1 1.3406(18) . ? N1 C11 1.4517(17) . ? N2 C3 1.3371(19) . ? N2 C21 1.4460(19) . ? C1 C2 1.410(2) . ? C1 C4 1.518(2) . ? C2 C3 1.407(2) . ? C2 H2 0.9500 . ? C3 C5 1.519(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C5 H5F 0.9800 . ? C11 C12 1.410(2) . ? C11 C16 1.414(2) . ? C12 C13 1.404(2) . ? C12 C17 1.525(2) . ? C13 C14 1.377(3) . ? C13 H13 0.9500 . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.402(2) . ? C15 H15 0.9500 . ? C16 C18 1.521(3) . ? C17 C171 1.527(3) . ? C17 C172 1.543(3) . ? C17 H17 1.0000 . ? C18 C181 1.529(3) . ? C18 C182 1.535(2) . ? C18 H18 1.0000 . ? C21 C22 1.409(2) . ? C21 C26 1.416(2) . ? C22 C23 1.408(3) . ? C22 C27 1.513(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.365(3) . ? C24 H24 0.9500 . ? C25 C26 1.397(3) . ? C25 H25 0.9500 . ? C26 C28 1.524(3) . ? C27 C271 1.528(3) . ? C27 C272 1.555(3) . ? C27 H27 1.0000 . ? C28 C282 1.532(3) . ? C28 C281 1.532(3) . ? C28 H28 1.0000 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C281 H28A 0.9800 . ? C281 H28B 0.9800 . ? C281 H28C 0.9800 . ? C282 H28D 0.9800 . ? C282 H28E 0.9800 . ? C282 H28F 0.9800 . ? 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 _geom_angle_publ_flag N1 Mg1 N2 95.46(5) . . ? N1 Mg1 B1 110.74(6) . 3_666 ? N2 Mg1 B1 127.37(6) . 3_666 ? N1 Mg1 B1 122.84(6) . . ? N2 Mg1 B1 115.15(6) . . ? B1 Mg1 B1 88.20(6) 3_666 . ? N1 Mg1 Mg1 128.63(4) . 3_666 ? N2 Mg1 Mg1 135.91(4) . 3_666 ? B1 Mg1 Mg1 44.16(4) 3_666 3_666 ? B1 Mg1 Mg1 44.03(4) . 3_666 ? N1 Mg1 H1B 149.5(5) . . ? N2 Mg1 H1B 106.2(5) . . ? B1 Mg1 H1B 72.7(5) 3_666 . ? B1 Mg1 H1B 27.6(5) . . ? Mg1 Mg1 H1B 34.5(4) 3_666 . ? N1 Mg1 H1D 98.5(6) . . ? N2 Mg1 H1D 115.6(5) . . ? B1 Mg1 H1D 104.9(6) 3_666 . ? B1 Mg1 H1D 25.4(6) . . ? Mg1 Mg1 H1D 63.2(6) 3_666 . ? H1B Mg1 H1D 52.9(7) . . ? Mg1 B1 Mg1 91.80(6) 3_666 . ? Mg1 B1 H1A 47.7(10) 3_666 . ? Mg1 B1 H1A 114.5(10) . . ? Mg1 B1 H1B 60.3(9) 3_666 . ? Mg1 B1 H1B 61.5(9) . . ? H1A B1 H1B 107.9(13) . . ? Mg1 B1 H1C 129.1(10) 3_666 . ? Mg1 B1 H1C 131.3(10) . . ? H1A B1 H1C 112.9(14) . . ? H1B B1 H1C 112.5(13) . . ? Mg1 B1 H1D 120.8(9) 3_666 . ? Mg1 B1 H1D 47.2(9) . . ? H1A B1 H1D 105.3(13) . . ? H1B B1 H1D 108.5(13) . . ? H1C B1 H1D 109.3(14) . . ? C1 N1 C11 117.43(12) . . ? C1 N1 Mg1 120.39(9) . . ? C11 N1 Mg1 122.13(9) . . ? C3 N2 C21 117.94(12) . . ? C3 N2 Mg1 119.99(10) . . ? C21 N2 Mg1 122.02(9) . . ? N1 C1 C2 123.79(13) . . ? N1 C1 C4 121.11(13) . . ? C2 C1 C4 115.08(13) . . ? C3 C2 C1 130.33(13) . . ? C3 C2 H2 114.8 . . ? C1 C2 H2 114.8 . . ? N2 C3 C2 124.69(13) . . ? N2 C3 C5 120.61(14) . . ? C2 C3 C5 114.70(13) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4 H4D 109.5 . . ? H4A C4 H4D 141.1 . . ? H4B C4 H4D 56.3 . . ? H4C C4 H4D 56.3 . . ? C1 C4 H4E 109.5 . . ? H4A C4 H4E 56.3 . . ? H4B C4 H4E 141.1 . . ? H4C C4 H4E 56.3 . . ? H4D C4 H4E 109.5 . . ? C1 C4 H4F 109.5 . . ? H4A C4 H4F 56.3 . . ? H4B C4 H4F 56.3 . . ? H4C C4 H4F 141.1 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C5 H5D 109.5 . . ? H5A C5 H5D 141.1 . . ? H5B C5 H5D 56.3 . . ? H5C C5 H5D 56.3 . . ? C3 C5 H5E 109.5 . . ? H5A C5 H5E 56.3 . . ? H5B C5 H5E 141.1 . . ? H5C C5 H5E 56.3 . . ? H5D C5 H5E 109.5 . . ? C3 C5 H5F 109.5 . . ? H5A C5 H5F 56.3 . . ? H5B C5 H5F 56.3 . . ? H5C C5 H5F 141.1 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C12 C11 C16 121.43(13) . . ? C12 C11 N1 120.64(13) . . ? C16 C11 N1 117.91(14) . . ? C13 C12 C11 117.66(16) . . ? C13 C12 C17 119.22(16) . . ? C11 C12 C17 123.09(13) . . ? C14 C13 C12 121.71(18) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.83(15) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 121.51(17) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 117.72(17) . . ? C15 C16 C18 121.21(15) . . ? C11 C16 C18 121.07(13) . . ? C12 C17 C171 110.08(14) . . ? C12 C17 C172 112.96(16) . . ? C171 C17 C172 109.77(16) . . ? C12 C17 H17 108.0 . . ? C171 C17 H17 108.0 . . ? C172 C17 H17 108.0 . . ? C16 C18 C181 112.36(16) . . ? C16 C18 C182 113.42(15) . . ? C181 C18 C182 109.81(15) . . ? C16 C18 H18 106.9 . . ? C181 C18 H18 106.9 . . ? C182 C18 H18 106.9 . . ? C22 C21 C26 120.73(15) . . ? C22 C21 N2 120.64(14) . . ? C26 C21 N2 118.62(14) . . ? C23 C22 C21 117.75(17) . . ? C23 C22 C27 119.79(16) . . ? C21 C22 C27 122.39(15) . . ? C24 C23 C22 121.50(19) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 120.04(18) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.6(2) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 118.34(18) . . ? C25 C26 C28 119.88(18) . . ? C21 C26 C28 121.77(16) . . ? C22 C27 C271 112.17(18) . . ? C22 C27 C272 110.09(18) . . ? C271 C27 C272 107.95(18) . . ? C22 C27 H27 108.9 . . ? C271 C27 H27 108.9 . . ? C272 C27 H27 108.9 . . ? C26 C28 C282 111.92(19) . . ? C26 C28 C281 111.5(2) . . ? C282 C28 C281 110.13(18) . . ? C26 C28 H28 107.7 . . ? C282 C28 H28 107.7 . . ? C281 C28 H28 107.7 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C28 C281 H28A 109.5 . . ? C28 C281 H28B 109.5 . . ? H28A C281 H28B 109.5 . . ? C28 C281 H28C 109.5 . . ? H28A C281 H28C 109.5 . . ? H28B C281 H28C 109.5 . . ? C28 C282 H28D 109.5 . . ? C28 C282 H28E 109.5 . . ? H28D C282 H28E 109.5 . . ? C28 C282 H28F 109.5 . . ? H28D C282 H28F 109.5 . . ? H28E C282 H28F 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mg1 B1 Mg1 113.66(6) . . . 3_666 ? N2 Mg1 B1 Mg1 -131.00(6) . . . 3_666 ? B1 Mg1 B1 Mg1 0.0 3_666 . . 3_666 ? N2 Mg1 N1 C1 -21.97(13) . . . . ? B1 Mg1 N1 C1 -155.45(12) 3_666 . . . ? B1 Mg1 N1 C1 102.76(13) . . . . ? Mg1 Mg1 N1 C1 157.34(10) 3_666 . . . ? N2 Mg1 N1 C11 160.79(12) . . . . ? B1 Mg1 N1 C11 27.31(14) 3_666 . . . ? B1 Mg1 N1 C11 -74.48(13) . . . . ? Mg1 Mg1 N1 C11 -19.90(14) 3_666 . . . ? N1 Mg1 N2 C3 19.52(12) . . . . ? B1 Mg1 N2 C3 140.88(11) 3_666 . . . ? B1 Mg1 N2 C3 -110.77(12) . . . . ? Mg1 Mg1 N2 C3 -159.71(10) 3_666 . . . ? N1 Mg1 N2 C21 -157.76(11) . . . . ? B1 Mg1 N2 C21 -36.40(14) 3_666 . . . ? B1 Mg1 N2 C21 71.94(12) . . . . ? Mg1 Mg1 N2 C21 23.01(14) 3_666 . . . ? C11 N1 C1 C2 -171.29(15) . . . . ? Mg1 N1 C1 C2 11.3(2) . . . . ? C11 N1 C1 C4 7.0(2) . . . . ? Mg1 N1 C1 C4 -170.38(13) . . . . ? N1 C1 C2 C3 10.6(3) . . . . ? C4 C1 C2 C3 -167.72(18) . . . . ? C21 N2 C3 C2 171.02(15) . . . . ? Mg1 N2 C3 C2 -6.4(2) . . . . ? C21 N2 C3 C5 -8.2(2) . . . . ? Mg1 N2 C3 C5 174.41(13) . . . . ? C1 C2 C3 N2 -13.6(3) . . . . ? C1 C2 C3 C5 165.68(18) . . . . ? C1 N1 C11 C12 -83.98(18) . . . . ? Mg1 N1 C11 C12 93.33(15) . . . . ? C1 N1 C11 C16 97.90(16) . . . . ? Mg1 N1 C11 C16 -84.79(15) . . . . ? C16 C11 C12 C13 -3.8(2) . . . . ? N1 C11 C12 C13 178.10(13) . . . . ? C16 C11 C12 C17 174.28(14) . . . . ? N1 C11 C12 C17 -3.8(2) . . . . ? C11 C12 C13 C14 0.8(2) . . . . ? C17 C12 C13 C14 -177.43(16) . . . . ? C12 C13 C14 C15 2.0(3) . . . . ? C13 C14 C15 C16 -1.8(3) . . . . ? C14 C15 C16 C11 -1.2(2) . . . . ? C14 C15 C16 C18 179.40(16) . . . . ? C12 C11 C16 C15 4.1(2) . . . . ? N1 C11 C16 C15 -177.84(13) . . . . ? C12 C11 C16 C18 -176.55(14) . . . . ? N1 C11 C16 C18 1.6(2) . . . . ? C13 C12 C17 C171 64.1(2) . . . . ? C11 C12 C17 C171 -113.97(17) . . . . ? C13 C12 C17 C172 -59.0(2) . . . . ? C11 C12 C17 C172 122.94(17) . . . . ? C15 C16 C18 C181 93.02(19) . . . . ? C11 C16 C18 C181 -86.36(18) . . . . ? C15 C16 C18 C182 -32.3(2) . . . . ? C11 C16 C18 C182 148.36(15) . . . . ? C3 N2 C21 C22 92.10(17) . . . . ? Mg1 N2 C21 C22 -90.56(14) . . . . ? C3 N2 C21 C26 -88.50(17) . . . . ? Mg1 N2 C21 C26 88.84(15) . . . . ? C26 C21 C22 C23 -0.8(2) . . . . ? N2 C21 C22 C23 178.57(14) . . . . ? C26 C21 C22 C27 176.28(15) . . . . ? N2 C21 C22 C27 -4.3(2) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C27 C22 C23 C24 -176.49(17) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C21 0.1(3) . . . . ? C24 C25 C26 C28 178.76(18) . . . . ? C22 C21 C26 C25 0.5(2) . . . . ? N2 C21 C26 C25 -178.94(14) . . . . ? C22 C21 C26 C28 -178.21(15) . . . . ? N2 C21 C26 C28 2.4(2) . . . . ? C23 C22 C27 C271 -57.2(2) . . . . ? C21 C22 C27 C271 125.78(18) . . . . ? C23 C22 C27 C272 63.1(2) . . . . ? C21 C22 C27 C272 -114.0(2) . . . . ? C25 C26 C28 C282 56.4(2) . . . . ? C21 C26 C28 C282 -124.97(19) . . . . ? C25 C26 C28 C281 -67.5(3) . . . . ? C21 C26 C28 C281 111.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.458 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.041 # Attachment 'nacnacMgNHDIPPBH3.cif' data_harder4 _database_code_depnum_ccdc_archive 'CCDC 741202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (DIPP-nacnac)MgNH(DIPP)BH3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H62 B Mg N3' _chemical_formula_weight 632.06 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.295(4) _cell_length_b 11.8119(14) _cell_length_c 18.846(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.004(15) _cell_angle_gamma 90.00 _cell_volume 3968.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5027 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 23.1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9860 _exptl_absorpt_correction_T_max 0.9882 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; Small crystal size and poor diffraction do not allow the determination of a high-accuracy structure. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17455 _diffrn_reflns_av_R_equivalents 0.1089 _diffrn_reflns_av_sigmaI/netI 0.2507 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6903 _reflns_number_gt 2340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6903 _refine_ls_number_parameters 421 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.2345 _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_ref 0.2375 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.75501(11) 0.65029(16) 0.64638(8) 0.0389(5) Uani 1 1 d . . . B1 B 0.8680(4) 0.7319(6) 0.6982(3) 0.0497(19) Uani 1 1 d . . . H1A H 0.8310 0.8032 0.6765 0.060 Uiso 1 1 calc R . . H1B H 0.8790 0.6812 0.6528 0.060 Uiso 1 1 calc R . . H1C H 0.9213 0.7645 0.7310 0.060 Uiso 1 1 calc R . . N1 N 0.6580(3) 0.7002(4) 0.5815(2) 0.0461(13) Uani 1 1 d . . . N2 N 0.7496(3) 0.4901(4) 0.60745(19) 0.0413(12) Uani 1 1 d . . . N3 N 0.8275(3) 0.6532(4) 0.7489(2) 0.0424(12) Uani 1 1 d D . . H3 H 0.841(3) 0.5850(16) 0.743(2) 0.032(16) Uiso 1 1 d D . . C1 C 0.6218(4) 0.6380(6) 0.5237(3) 0.0569(18) Uani 1 1 d . . . C2 C 0.6454(4) 0.5320(6) 0.5066(3) 0.073(2) Uani 1 1 d . . . H2 H 0.6204 0.5045 0.4601 0.087 Uiso 1 1 calc R . . C3 C 0.6997(4) 0.4581(5) 0.5460(3) 0.0557(18) Uani 1 1 d . . . C4 C 0.5497(4) 0.6822(7) 0.4739(3) 0.090(3) Uani 1 1 d . . . H4A H 0.5084 0.6765 0.4991 0.108 Uiso 1 1 calc R . . H4B H 0.5378 0.6369 0.4293 0.108 Uiso 1 1 calc R . . H4C H 0.5565 0.7615 0.4616 0.108 Uiso 1 1 calc R . . C5 C 0.7018(4) 0.3395(6) 0.5155(3) 0.075(2) Uani 1 1 d . . . H5A H 0.7221 0.3424 0.4716 0.091 Uiso 1 1 calc R . . H5B H 0.6508 0.3084 0.5031 0.091 Uiso 1 1 calc R . . H5C H 0.7337 0.2912 0.5520 0.091 Uiso 1 1 calc R . . C11 C 0.6199(3) 0.8029(5) 0.5979(3) 0.0463(16) Uani 1 1 d . . . C12 C 0.5637(4) 0.7925(6) 0.6380(3) 0.0590(18) Uani 1 1 d . . . C13 C 0.5287(4) 0.8928(7) 0.6517(4) 0.073(2) Uani 1 1 d . . . H13 H 0.4899 0.8891 0.6777 0.087 Uiso 1 1 calc R . . C14 C 0.5487(5) 0.9965(7) 0.6289(4) 0.077(2) Uani 1 1 d . . . H14 H 0.5225 1.0625 0.6378 0.092 Uiso 1 1 calc R . . C15 C 0.6061(4) 1.0054(6) 0.5932(3) 0.070(2) Uani 1 1 d . . . H15 H 0.6204 1.0781 0.5796 0.084 Uiso 1 1 calc R . . C16 C 0.6442(4) 0.9088(6) 0.5764(3) 0.0548(17) Uani 1 1 d . A . C17 C 0.5430(4) 0.6769(6) 0.6655(4) 0.073(2) Uani 1 1 d . . . H17 H 0.5588 0.6164 0.6350 0.088 Uiso 1 1 calc R . . C18 C 0.7058(4) 0.9187(6) 0.5359(3) 0.0638(19) Uani 1 1 d D . . H18 H 0.7285 0.8430 0.5306 0.077 Uiso 0.49(2) 1 calc PR A 1 H18' H 0.7407 0.8539 0.5524 0.077 Uiso 0.51(2) 1 calc PR A 2 C21 C 0.7956(3) 0.4039(5) 0.6500(3) 0.0386(14) Uani 1 1 d . . . C22 C 0.7691(3) 0.3482(5) 0.7056(3) 0.0462(15) Uani 1 1 d . . . C23 C 0.8149(4) 0.2668(5) 0.7466(3) 0.0537(17) Uani 1 1 d . . . H23 H 0.7977 0.2274 0.7837 0.064 Uiso 1 1 calc R . . C24 C 0.8844(4) 0.2424(6) 0.7346(3) 0.066(2) Uani 1 1 d . . . H24 H 0.9146 0.1865 0.7635 0.079 Uiso 1 1 calc R . . C25 C 0.9108(4) 0.2974(6) 0.6817(3) 0.0611(18) Uani 1 1 d . . . H25 H 0.9594 0.2803 0.6747 0.073 Uiso 1 1 calc R . . C26 C 0.8665(3) 0.3791(5) 0.6376(3) 0.0453(15) Uani 1 1 d . . . C27 C 0.6936(4) 0.3782(6) 0.7211(3) 0.0601(18) Uani 1 1 d . . . H27 H 0.6794 0.4541 0.6987 0.072 Uiso 1 1 calc R . . C28 C 0.8975(5) 0.4374(6) 0.5786(3) 0.068(2) Uani 1 1 d . . . H28 H 0.8620 0.4990 0.5570 0.082 Uiso 1 1 calc R . . C31 C 0.8358(3) 0.6848(5) 0.8253(2) 0.0408(14) Uani 1 1 d . . . C32 C 0.8052(4) 0.7846(5) 0.8454(3) 0.0497(16) Uani 1 1 d . . . C33 C 0.8198(4) 0.8141(6) 0.9191(3) 0.066(2) Uani 1 1 d . . . H33 H 0.8018 0.8842 0.9332 0.079 Uiso 1 1 calc R . . C34 C 0.8606(4) 0.7421(7) 0.9724(3) 0.070(2) Uani 1 1 d . . . H34 H 0.8699 0.7625 1.0224 0.084 Uiso 1 1 calc R . . C35 C 0.8871(4) 0.6417(6) 0.9518(3) 0.0584(18) Uani 1 1 d . . . H35 H 0.9136 0.5922 0.9884 0.070 Uiso 1 1 calc R . . C36 C 0.8763(3) 0.6094(5) 0.8783(2) 0.0437(15) Uani 1 1 d . . . C37 C 0.7588(4) 0.8666(6) 0.7923(3) 0.066(2) Uani 1 1 d . . . H37 H 0.7421 0.8272 0.7444 0.079 Uiso 1 1 calc R . . C38 C 0.9104(3) 0.4991(5) 0.8589(2) 0.0468(16) Uani 1 1 d . . . H38 H 0.8770 0.4714 0.8126 0.056 Uiso 1 1 calc R . . C171 C 0.4598(5) 0.6639(9) 0.6611(4) 0.113(3) Uani 1 1 d . . . H17A H 0.4320 0.6759 0.6108 0.136 Uiso 1 1 calc R . . H17B H 0.4438 0.7200 0.6929 0.136 Uiso 1 1 calc R . . H17C H 0.4496 0.5876 0.6769 0.136 Uiso 1 1 calc R . . C172 C 0.5840(5) 0.6577(8) 0.7451(4) 0.112(3) Uani 1 1 d . . . H17D H 0.6382 0.6648 0.7496 0.135 Uiso 1 1 calc R . . H17E H 0.5725 0.5817 0.7605 0.135 Uiso 1 1 calc R . . H17F H 0.5675 0.7144 0.7761 0.135 Uiso 1 1 calc R . . C181 C 0.7684(8) 1.0057(13) 0.5793(10) 0.065(5) Uiso 0.49(2) 1 d PD A 1 H18A H 0.8058 1.0200 0.5505 0.078 Uiso 0.49(2) 1 calc PR A 1 H18B H 0.7930 0.9727 0.6263 0.078 Uiso 0.49(2) 1 calc PR A 1 H18C H 0.7442 1.0771 0.5874 0.078 Uiso 0.49(2) 1 calc PR A 1 C182 C 0.6766(10) 0.975(2) 0.4609(7) 0.093(7) Uiso 0.49(2) 1 d PD A 1 H18D H 0.7122 0.9611 0.4300 0.112 Uiso 0.49(2) 1 calc PR A 1 H18E H 0.6714 1.0566 0.4673 0.112 Uiso 0.49(2) 1 calc PR A 1 H18F H 0.6277 0.9426 0.4378 0.112 Uiso 0.49(2) 1 calc PR A 1 C183 C 0.7528(10) 1.0232(12) 0.5478(11) 0.081(5) Uiso 0.51(2) 1 d PD A 2 H18G H 0.7902 1.0198 0.5179 0.122 Uiso 0.51(2) 1 calc PR A 2 H18H H 0.7783 1.0288 0.5993 0.122 Uiso 0.51(2) 1 calc PR A 2 H18I H 0.7208 1.0897 0.5339 0.122 Uiso 0.51(2) 1 calc PR A 2 C184 C 0.6726(7) 0.9009(16) 0.4504(5) 0.053(5) Uiso 0.51(2) 1 d PD A 2 H18J H 0.6414 0.8327 0.4427 0.079 Uiso 0.51(2) 1 calc PR A 2 H18K H 0.7141 0.8924 0.4257 0.079 Uiso 0.51(2) 1 calc PR A 2 H18L H 0.6422 0.9668 0.4306 0.079 Uiso 0.51(2) 1 calc PR A 2 C271 C 0.6314(5) 0.2969(8) 0.6865(4) 0.108(3) Uani 1 1 d . . . H27A H 0.5842 0.3209 0.6983 0.129 Uiso 1 1 calc R . . H27B H 0.6441 0.2204 0.7054 0.129 Uiso 1 1 calc R . . H27C H 0.6257 0.2970 0.6336 0.129 Uiso 1 1 calc R . . C272 C 0.6961(4) 0.3902(7) 0.8028(3) 0.083(2) Uani 1 1 d . . . H27D H 0.6461 0.4102 0.8095 0.099 Uiso 1 1 calc R . . H27E H 0.7319 0.4497 0.8235 0.099 Uiso 1 1 calc R . . H27F H 0.7120 0.3182 0.8274 0.099 Uiso 1 1 calc R . . C281 C 0.9740(5) 0.4902(7) 0.6084(5) 0.099(3) Uani 1 1 d . . . H28A H 0.9913 0.5278 0.5688 0.119 Uiso 1 1 calc R . . H28B H 1.0098 0.4311 0.6296 0.119 Uiso 1 1 calc R . . H28C H 0.9702 0.5459 0.6459 0.119 Uiso 1 1 calc R . . C282 C 0.9026(6) 0.3512(8) 0.5168(4) 0.122(4) Uani 1 1 d . . . H28D H 0.9218 0.3899 0.4787 0.147 Uiso 1 1 calc R . . H28E H 0.8526 0.3206 0.4958 0.147 Uiso 1 1 calc R . . H28F H 0.9366 0.2893 0.5370 0.147 Uiso 1 1 calc R . . C371 C 0.6910(6) 0.9089(9) 0.8150(4) 0.131(4) Uani 1 1 d . . . H37A H 0.6633 0.9603 0.7777 0.157 Uiso 1 1 calc R . . H37B H 0.7062 0.9494 0.8614 0.157 Uiso 1 1 calc R . . H37C H 0.6589 0.8447 0.8209 0.157 Uiso 1 1 calc R . . C372 C 0.8075(6) 0.9715(7) 0.7807(4) 0.120(4) Uani 1 1 d . . . H37D H 0.8524 0.9455 0.7654 0.144 Uiso 1 1 calc R . . H37E H 0.8224 1.0136 0.8265 0.144 Uiso 1 1 calc R . . H37F H 0.7781 1.0209 0.7431 0.144 Uiso 1 1 calc R . . C381 C 0.9878(4) 0.5197(6) 0.8426(3) 0.068(2) Uani 1 1 d . . . H38A H 1.0086 0.4477 0.8304 0.082 Uiso 1 1 calc R . . H38B H 1.0214 0.5526 0.8856 0.082 Uiso 1 1 calc R . . H38C H 0.9828 0.5721 0.8014 0.082 Uiso 1 1 calc R . . C382 C 0.9143(4) 0.4037(6) 0.9151(3) 0.0655(19) Uani 1 1 d . . . H38D H 0.9369 0.3363 0.8986 0.079 Uiso 1 1 calc R . . H38E H 0.8636 0.3855 0.9206 0.079 Uiso 1 1 calc R . . H38F H 0.9450 0.4284 0.9621 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0372(11) 0.0389(11) 0.0349(8) 0.0030(8) -0.0035(7) 0.0079(10) B1 0.039(5) 0.056(5) 0.053(4) 0.008(3) 0.006(3) -0.002(4) N1 0.045(3) 0.049(3) 0.037(2) -0.004(2) -0.005(2) 0.011(3) N2 0.043(3) 0.043(3) 0.034(2) -0.003(2) -0.0018(19) 0.009(2) N3 0.047(3) 0.038(3) 0.036(2) -0.001(2) -0.0040(19) -0.002(3) C1 0.058(5) 0.065(5) 0.039(3) -0.004(3) -0.008(3) 0.021(4) C2 0.083(6) 0.079(5) 0.040(3) -0.021(3) -0.018(3) 0.026(5) C3 0.070(5) 0.050(4) 0.040(3) -0.010(3) -0.002(3) 0.008(4) C4 0.081(6) 0.104(7) 0.063(4) -0.022(4) -0.032(4) 0.044(5) C5 0.098(6) 0.063(5) 0.049(3) -0.023(3) -0.016(3) 0.018(5) C11 0.039(4) 0.051(4) 0.039(3) 0.000(3) -0.011(3) 0.022(3) C12 0.032(4) 0.074(5) 0.071(4) -0.008(4) 0.011(3) 0.003(4) C13 0.049(5) 0.069(6) 0.101(5) -0.014(4) 0.020(4) 0.019(4) C14 0.070(6) 0.057(5) 0.100(5) -0.004(4) 0.011(4) 0.032(5) C15 0.078(6) 0.057(5) 0.076(4) 0.007(4) 0.020(4) 0.021(4) C16 0.055(5) 0.059(5) 0.047(3) 0.007(3) 0.005(3) 0.021(4) C17 0.057(5) 0.059(5) 0.108(5) -0.032(4) 0.028(4) -0.010(4) C18 0.066(5) 0.069(5) 0.058(4) 0.024(3) 0.015(3) 0.017(4) C21 0.033(3) 0.037(3) 0.044(3) -0.004(2) 0.003(2) 0.006(3) C22 0.046(4) 0.047(4) 0.045(3) -0.010(3) 0.009(3) -0.010(3) C23 0.067(5) 0.037(4) 0.056(3) 0.005(3) 0.009(3) -0.002(4) C24 0.068(6) 0.052(5) 0.071(4) 0.019(3) 0.000(4) 0.014(4) C25 0.047(4) 0.053(4) 0.078(4) 0.002(3) 0.005(3) 0.010(4) C26 0.042(4) 0.038(4) 0.053(3) -0.005(3) 0.006(3) 0.002(3) C27 0.053(5) 0.071(5) 0.060(3) -0.001(3) 0.020(3) -0.004(4) C28 0.082(6) 0.062(5) 0.074(4) 0.004(3) 0.044(4) 0.002(4) C31 0.037(4) 0.040(4) 0.038(3) 0.002(2) -0.007(2) -0.006(3) C32 0.052(4) 0.040(4) 0.049(3) -0.006(3) -0.007(3) 0.000(3) C33 0.070(5) 0.063(5) 0.056(3) -0.012(3) -0.002(3) -0.005(4) C34 0.078(6) 0.077(5) 0.050(3) -0.008(4) 0.004(3) -0.001(5) C35 0.053(4) 0.078(5) 0.036(3) 0.008(3) -0.009(3) 0.005(4) C36 0.040(4) 0.046(4) 0.039(3) 0.005(3) -0.004(2) -0.002(3) C37 0.077(6) 0.053(5) 0.058(3) -0.007(3) -0.003(3) 0.018(4) C38 0.048(4) 0.043(4) 0.038(3) 0.014(2) -0.015(2) -0.007(3) C171 0.076(7) 0.134(9) 0.126(6) -0.033(6) 0.016(5) -0.033(6) C172 0.084(7) 0.119(8) 0.127(7) 0.048(6) 0.010(5) -0.011(6) C271 0.069(6) 0.175(10) 0.077(5) -0.043(5) 0.013(4) -0.033(6) C272 0.054(5) 0.117(7) 0.080(4) -0.039(4) 0.020(4) -0.035(5) C281 0.070(6) 0.093(7) 0.150(7) 0.007(5) 0.062(6) -0.009(5) C282 0.154(10) 0.127(8) 0.112(6) -0.022(6) 0.085(6) -0.018(8) C371 0.122(9) 0.143(9) 0.104(6) -0.038(6) -0.025(6) 0.079(8) C372 0.167(11) 0.046(5) 0.114(6) 0.008(5) -0.037(6) -0.009(6) C381 0.052(5) 0.074(5) 0.074(4) 0.006(4) 0.002(3) 0.004(4) C382 0.061(5) 0.066(5) 0.059(3) 0.016(3) -0.009(3) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N1 2.004(5) . ? Mg1 N2 2.024(5) . ? Mg1 N3 2.083(4) . ? Mg1 H3 2.26(4) . ? B1 N3 1.625(8) . ? B1 H1A 1.1000 . ? B1 H1B 1.1000 . ? B1 H1C 1.1000 . ? N1 C1 1.357(7) . ? N1 C11 1.466(7) . ? N2 C3 1.357(7) . ? N2 C21 1.444(7) . ? N3 C31 1.463(6) . ? N3 H3 0.86(3) . ? C1 C2 1.386(8) . ? C1 C4 1.529(8) . ? C2 C3 1.402(9) . ? C2 H2 0.9500 . ? C3 C5 1.518(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C11 C12 1.411(8) . ? C11 C16 1.417(9) . ? C12 C13 1.398(9) . ? C12 C17 1.538(9) . ? C13 C14 1.375(10) . ? C13 H13 0.9500 . ? C14 C15 1.372(10) . ? C14 H14 0.9500 . ? C15 C16 1.410(9) . ? C15 H15 0.9500 . ? C16 C18 1.501(9) . ? C17 C171 1.514(11) . ? C17 C172 1.536(9) . ? C17 H17 1.0000 . ? C18 C183 1.492(12) . ? C18 C182 1.544(11) . ? C18 C184 1.603(10) . ? C18 C181 1.616(12) . ? C18 H18 1.0000 . ? C18 H18' 1.0000 . ? C21 C26 1.400(8) . ? C21 C22 1.412(7) . ? C22 C23 1.390(8) . ? C22 C27 1.518(8) . ? C23 C24 1.371(9) . ? C23 H23 0.9500 . ? C24 C25 1.367(9) . ? C24 H24 0.9500 . ? C25 C26 1.405(8) . ? C25 H25 0.9500 . ? C26 C28 1.522(8) . ? C27 C271 1.518(10) . ? C27 C272 1.536(7) . ? C27 H27 1.0000 . ? C28 C281 1.519(10) . ? C28 C282 1.566(9) . ? C28 H28 1.0000 . ? C31 C32 1.393(8) . ? C31 C36 1.416(7) . ? C32 C33 1.399(7) . ? C32 C37 1.510(8) . ? C33 C34 1.397(9) . ? C33 H33 0.9500 . ? C34 C35 1.369(9) . ? C34 H34 0.9500 . ? C35 C36 1.407(7) . ? C35 H35 0.9500 . ? C36 C38 1.525(8) . ? C37 C371 1.487(11) . ? C37 C372 1.569(11) . ? C37 H37 1.0000 . ? C38 C381 1.535(8) . ? C38 C382 1.538(7) . ? C38 H38 1.0000 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C183 H18G 0.9800 . ? C183 H18H 0.9800 . ? C183 H18I 0.9800 . ? C184 H18J 0.9800 . ? C184 H18K 0.9800 . ? C184 H18L 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C281 H28A 0.9800 . ? C281 H28B 0.9800 . ? C281 H28C 0.9800 . ? C282 H28D 0.9800 . ? C282 H28E 0.9800 . ? C282 H28F 0.9800 . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C381 H38A 0.9800 . ? C381 H38B 0.9800 . ? C381 H38C 0.9800 . ? C382 H38D 0.9800 . ? C382 H38E 0.9800 . ? C382 H38F 0.9800 . ? 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 _geom_angle_publ_flag N1 Mg1 N2 95.11(19) . . ? N1 Mg1 N3 148.5(2) . . ? N2 Mg1 N3 108.7(2) . . ? N1 Mg1 H3 162.6(12) . . ? N2 Mg1 H3 86.6(6) . . ? N3 Mg1 H3 22.3(5) . . ? N3 B1 H1A 109.5 . . ? N3 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? N3 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? C1 N1 C11 116.7(5) . . ? C1 N1 Mg1 122.4(4) . . ? C11 N1 Mg1 120.8(3) . . ? C3 N2 C21 118.3(5) . . ? C3 N2 Mg1 122.6(4) . . ? C21 N2 Mg1 118.9(3) . . ? C31 N3 B1 118.2(5) . . ? C31 N3 Mg1 145.2(4) . . ? B1 N3 Mg1 75.2(3) . . ? C31 N3 H3 113(3) . . ? B1 N3 H3 106(3) . . ? Mg1 N3 H3 91(3) . . ? N1 C1 C2 123.7(5) . . ? N1 C1 C4 120.3(6) . . ? C2 C1 C4 116.0(5) . . ? C1 C2 C3 131.3(5) . . ? C1 C2 H2 114.3 . . ? C3 C2 H2 114.3 . . ? N2 C3 C2 122.6(5) . . ? N2 C3 C5 120.7(5) . . ? C2 C3 C5 116.7(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C11 C16 122.9(6) . . ? C12 C11 N1 118.6(6) . . ? C16 C11 N1 118.4(5) . . ? C13 C12 C11 116.4(7) . . ? C13 C12 C17 122.1(6) . . ? C11 C12 C17 121.5(6) . . ? C14 C13 C12 122.1(7) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 120.5(7) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.3(7) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 116.6(6) . . ? C15 C16 C18 121.1(7) . . ? C11 C16 C18 122.3(6) . . ? C171 C17 C172 107.6(7) . . ? C171 C17 C12 113.1(7) . . ? C172 C17 C12 110.9(6) . . ? C171 C17 H17 108.4 . . ? C172 C17 H17 108.4 . . ? C12 C17 H17 108.4 . . ? C183 C18 C16 117.5(8) . . ? C183 C18 C182 81.4(10) . . ? C16 C18 C182 110.7(8) . . ? C183 C18 C184 109.5(8) . . ? C16 C18 C184 110.0(7) . . ? C182 C18 C184 33.0(7) . . ? C183 C18 C181 23.1(7) . . ? C16 C18 C181 108.7(7) . . ? C182 C18 C181 104.5(10) . . ? C184 C18 C181 131.0(9) . . ? C183 C18 H18 121.1 . . ? C16 C18 H18 110.9 . . ? C182 C18 H18 110.9 . . ? C184 C18 H18 81.5 . . ? C181 C18 H18 110.9 . . ? C183 C18 H18' 106.4 . . ? C16 C18 H18' 106.4 . . ? C182 C18 H18' 132.7 . . ? C184 C18 H18' 106.4 . . ? C181 C18 H18' 90.1 . . ? H18 C18 H18' 25.4 . . ? C26 C21 C22 120.8(5) . . ? C26 C21 N2 120.1(5) . . ? C22 C21 N2 119.1(5) . . ? C23 C22 C21 118.1(6) . . ? C23 C22 C27 121.0(5) . . ? C21 C22 C27 120.9(5) . . ? C24 C23 C22 121.2(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 118.6(5) . . ? C21 C26 C28 122.6(5) . . ? C25 C26 C28 118.8(6) . . ? C271 C27 C22 113.4(6) . . ? C271 C27 C272 109.8(5) . . ? C22 C27 C272 113.0(5) . . ? C271 C27 H27 106.7 . . ? C22 C27 H27 106.7 . . ? C272 C27 H27 106.7 . . ? C281 C28 C26 112.3(6) . . ? C281 C28 C282 109.8(7) . . ? C26 C28 C282 110.2(6) . . ? C281 C28 H28 108.2 . . ? C26 C28 H28 108.2 . . ? C282 C28 H28 108.2 . . ? C32 C31 C36 121.2(5) . . ? C32 C31 N3 121.6(5) . . ? C36 C31 N3 117.1(5) . . ? C31 C32 C33 118.8(5) . . ? C31 C32 C37 124.3(5) . . ? C33 C32 C37 116.9(6) . . ? C34 C33 C32 120.9(6) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 119.3(6) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 122.3(6) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C35 C36 C31 117.3(5) . . ? C35 C36 C38 119.6(5) . . ? C31 C36 C38 123.0(4) . . ? C371 C37 C32 113.9(6) . . ? C371 C37 C372 108.1(7) . . ? C32 C37 C372 110.3(6) . . ? C371 C37 H37 108.1 . . ? C32 C37 H37 108.1 . . ? C372 C37 H37 108.1 . . ? C36 C38 C381 111.0(5) . . ? C36 C38 C382 114.8(5) . . ? C381 C38 C382 110.6(5) . . ? C36 C38 H38 106.7 . . ? C381 C38 H38 106.7 . . ? C382 C38 H38 106.7 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C18 C183 H18G 109.5 . . ? C18 C183 H18H 109.5 . . ? H18G C183 H18H 109.5 . . ? C18 C183 H18I 109.5 . . ? H18G C183 H18I 109.5 . . ? H18H C183 H18I 109.5 . . ? C18 C184 H18J 109.5 . . ? C18 C184 H18K 109.5 . . ? H18J C184 H18K 109.5 . . ? C18 C184 H18L 109.5 . . ? H18J C184 H18L 109.5 . . ? H18K C184 H18L 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C28 C281 H28A 109.5 . . ? C28 C281 H28B 109.5 . . ? H28A C281 H28B 109.5 . . ? C28 C281 H28C 109.5 . . ? H28A C281 H28C 109.5 . . ? H28B C281 H28C 109.5 . . ? C28 C282 H28D 109.5 . . ? C28 C282 H28E 109.5 . . ? H28D C282 H28E 109.5 . . ? C28 C282 H28F 109.5 . . ? H28D C282 H28F 109.5 . . ? H28E C282 H28F 109.5 . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C38 C381 H38A 109.5 . . ? C38 C381 H38B 109.5 . . ? H38A C381 H38B 109.5 . . ? C38 C381 H38C 109.5 . . ? H38A C381 H38C 109.5 . . ? H38B C381 H38C 109.5 . . ? C38 C382 H38D 109.5 . . ? C38 C382 H38E 109.5 . . ? H38D C382 H38E 109.5 . . ? C38 C382 H38F 109.5 . . ? H38D C382 H38F 109.5 . . ? H38E C382 H38F 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mg1 N1 C1 -12.7(5) . . . . ? N3 Mg1 N1 C1 -152.4(5) . . . . ? N2 Mg1 N1 C11 162.9(4) . . . . ? N3 Mg1 N1 C11 23.2(7) . . . . ? N1 Mg1 N2 C3 12.4(5) . . . . ? N3 Mg1 N2 C3 171.4(5) . . . . ? N1 Mg1 N2 C21 -161.9(4) . . . . ? N3 Mg1 N2 C21 -2.8(5) . . . . ? N1 Mg1 N3 C31 11.1(9) . . . . ? N2 Mg1 N3 C31 -126.0(7) . . . . ? N1 Mg1 N3 B1 -107.3(5) . . . . ? N2 Mg1 N3 B1 115.6(3) . . . . ? C11 N1 C1 C2 -171.5(6) . . . . ? Mg1 N1 C1 C2 4.3(9) . . . . ? C11 N1 C1 C4 6.8(9) . . . . ? Mg1 N1 C1 C4 -177.4(5) . . . . ? N1 C1 C2 C3 10.9(13) . . . . ? C4 C1 C2 C3 -167.4(8) . . . . ? C21 N2 C3 C2 170.8(6) . . . . ? Mg1 N2 C3 C2 -3.5(9) . . . . ? C21 N2 C3 C5 -10.7(9) . . . . ? Mg1 N2 C3 C5 175.1(5) . . . . ? C1 C2 C3 N2 -11.3(13) . . . . ? C1 C2 C3 C5 170.1(8) . . . . ? C1 N1 C11 C12 81.7(6) . . . . ? Mg1 N1 C11 C12 -94.2(6) . . . . ? C1 N1 C11 C16 -101.9(6) . . . . ? Mg1 N1 C11 C16 82.3(5) . . . . ? C16 C11 C12 C13 4.2(9) . . . . ? N1 C11 C12 C13 -179.5(5) . . . . ? C16 C11 C12 C17 -175.3(6) . . . . ? N1 C11 C12 C17 1.1(8) . . . . ? C11 C12 C13 C14 -1.2(10) . . . . ? C17 C12 C13 C14 178.2(7) . . . . ? C12 C13 C14 C15 -2.1(11) . . . . ? C13 C14 C15 C16 2.6(11) . . . . ? C14 C15 C16 C11 0.2(10) . . . . ? C14 C15 C16 C18 178.6(6) . . . . ? C12 C11 C16 C15 -3.7(9) . . . . ? N1 C11 C16 C15 180.0(5) . . . . ? C12 C11 C16 C18 177.9(5) . . . . ? N1 C11 C16 C18 1.6(8) . . . . ? C13 C12 C17 C171 38.5(9) . . . . ? C11 C12 C17 C171 -142.2(6) . . . . ? C13 C12 C17 C172 -82.6(9) . . . . ? C11 C12 C17 C172 96.8(8) . . . . ? C15 C16 C18 C183 31.9(13) . . . . ? C11 C16 C18 C183 -149.8(11) . . . . ? C15 C16 C18 C182 -59.1(13) . . . . ? C11 C16 C18 C182 119.2(12) . . . . ? C15 C16 C18 C184 -94.3(9) . . . . ? C11 C16 C18 C184 84.0(9) . . . . ? C15 C16 C18 C181 55.1(10) . . . . ? C11 C16 C18 C181 -126.6(9) . . . . ? C3 N2 C21 C26 92.4(7) . . . . ? Mg1 N2 C21 C26 -93.1(5) . . . . ? C3 N2 C21 C22 -89.8(6) . . . . ? Mg1 N2 C21 C22 84.7(5) . . . . ? C26 C21 C22 C23 -1.1(8) . . . . ? N2 C21 C22 C23 -179.0(5) . . . . ? C26 C21 C22 C27 177.6(5) . . . . ? N2 C21 C22 C27 -0.3(8) . . . . ? C21 C22 C23 C24 1.2(9) . . . . ? C27 C22 C23 C24 -177.5(6) . . . . ? C22 C23 C24 C25 -0.1(10) . . . . ? C23 C24 C25 C26 -1.0(10) . . . . ? C22 C21 C26 C25 0.1(8) . . . . ? N2 C21 C26 C25 177.9(5) . . . . ? C22 C21 C26 C28 -179.7(5) . . . . ? N2 C21 C26 C28 -1.9(8) . . . . ? C24 C25 C26 C21 1.0(9) . . . . ? C24 C25 C26 C28 -179.2(6) . . . . ? C23 C22 C27 C271 -82.5(7) . . . . ? C21 C22 C27 C271 98.9(7) . . . . ? C23 C22 C27 C272 43.3(8) . . . . ? C21 C22 C27 C272 -135.3(6) . . . . ? C21 C26 C28 C281 126.1(7) . . . . ? C25 C26 C28 C281 -53.7(8) . . . . ? C21 C26 C28 C282 -111.3(7) . . . . ? C25 C26 C28 C282 69.0(8) . . . . ? B1 N3 C31 C32 65.7(7) . . . . ? Mg1 N3 C31 C32 -39.5(10) . . . . ? B1 N3 C31 C36 -114.3(6) . . . . ? Mg1 N3 C31 C36 140.4(6) . . . . ? C36 C31 C32 C33 4.8(9) . . . . ? N3 C31 C32 C33 -175.3(5) . . . . ? C36 C31 C32 C37 -177.4(6) . . . . ? N3 C31 C32 C37 2.5(10) . . . . ? C31 C32 C33 C34 -3.7(10) . . . . ? C37 C32 C33 C34 178.3(7) . . . . ? C32 C33 C34 C35 0.6(11) . . . . ? C33 C34 C35 C36 1.6(11) . . . . ? C34 C35 C36 C31 -0.6(10) . . . . ? C34 C35 C36 C38 177.1(6) . . . . ? C32 C31 C36 C35 -2.6(9) . . . . ? N3 C31 C36 C35 177.4(5) . . . . ? C32 C31 C36 C38 179.7(6) . . . . ? N3 C31 C36 C38 -0.2(8) . . . . ? C31 C32 C37 C371 136.3(7) . . . . ? C33 C32 C37 C371 -45.9(9) . . . . ? C31 C32 C37 C372 -101.9(8) . . . . ? C33 C32 C37 C372 75.9(8) . . . . ? C35 C36 C38 C381 -93.2(6) . . . . ? C31 C36 C38 C381 84.4(6) . . . . ? C35 C36 C38 C382 33.1(8) . . . . ? C31 C36 C38 C382 -149.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.342 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.053 # Attachment 'NBNH2-hasj170.cif' data_hasj170 _database_code_depnum_ccdc_archive 'CCDC 741203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HB(NHDIPP)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18.50 B0.50 N' _chemical_formula_weight 182.18 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.2052(9) _cell_length_b 10.3128(9) _cell_length_c 11.5048(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.727(5) _cell_angle_gamma 90.00 _cell_volume 1146.71(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was twinned and reflections from two domains could be well separated and were merged for refinement. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14398 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.12 _reflns_number_total 6317 _reflns_number_gt 5329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.9(19) _refine_ls_number_reflns 6317 _refine_ls_number_parameters 391 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.52242(15) 0.00955(12) 0.40141(13) 0.0200(3) Uani 1 1 d . . . C2 C 0.63471(14) -0.03845(13) 0.36791(13) 0.0221(3) Uani 1 1 d . . . C3 C 0.61953(16) -0.05072(14) 0.24358(14) 0.0262(3) Uani 1 1 d . . . C4 C 0.49616(16) -0.01879(15) 0.15382(14) 0.0277(3) Uani 1 1 d . . . C5 C 0.38539(16) 0.02388(15) 0.18782(14) 0.0267(3) Uani 1 1 d . . . C6 C 0.39494(14) 0.03824(13) 0.31102(13) 0.0224(3) Uani 1 1 d . . . C7 C 0.77069(16) -0.07364(14) 0.46546(15) 0.0273(3) Uani 1 1 d . . . C8 C 0.86458(19) 0.04573(18) 0.5018(2) 0.0425(4) Uani 1 1 d . . . C9 C 0.84709(18) -0.18558(16) 0.42797(17) 0.0322(4) Uani 1 1 d . . . C10 C 0.26704(16) 0.07727(15) 0.34363(15) 0.0274(3) Uani 1 1 d . . . C11 C 0.1672(3) -0.0367(2) 0.3232(3) 0.0622(7) Uani 1 1 d . . . C12 C 0.1942(2) 0.1959(2) 0.26978(19) 0.0419(4) Uani 1 1 d . . . C13 C 0.59084(14) 0.05161(13) 0.79854(13) 0.0209(3) Uani 1 1 d . . . C14 C 0.72647(15) 0.05234(14) 0.88093(13) 0.0250(3) Uani 1 1 d . . . C15 C 0.76917(17) -0.05187(16) 0.96248(15) 0.0306(3) Uani 1 1 d . . . C16 C 0.68226(17) -0.15473(15) 0.96041(15) 0.0302(3) Uani 1 1 d . . . C17 C 0.54825(17) -0.15448(14) 0.87913(14) 0.0278(3) Uani 1 1 d . . . C18 C 0.49945(15) -0.05069(13) 0.79842(13) 0.0232(3) Uani 1 1 d . . . C19 C 0.82431(17) 0.16420(18) 0.88579(17) 0.0342(4) Uani 1 1 d . . . C20 C 0.8369(2) 0.2496(2) 0.9970(2) 0.0468(5) Uani 1 1 d . . . C21 C 0.9660(2) 0.1193(2) 0.8842(3) 0.0514(5) Uani 1 1 d . . . C22 C 0.34775(15) -0.04418(15) 0.72026(14) 0.0261(3) Uani 1 1 d . . . C23 C 0.26797(18) 0.02962(19) 0.79187(17) 0.0367(4) Uani 1 1 d . . . C24 C 0.2828(2) -0.17661(19) 0.6792(2) 0.0489(5) Uani 1 1 d . . . B1 B 0.52576(16) 0.14668(15) 0.58474(15) 0.0226(3) Uani 1 1 d . . . N1 N 0.53837(12) 0.02750(11) 0.52829(10) 0.0213(2) Uani 1 1 d . . . N2 N 0.54515(13) 0.15576(11) 0.71182(11) 0.0227(3) Uani 1 1 d . . . H3 H 0.698(2) -0.0822(19) 0.2177(18) 0.037(5) Uiso 1 1 d . . . H4 H 0.4824(19) -0.028(2) 0.0634(18) 0.034(5) Uiso 1 1 d . . . H5 H 0.293(2) 0.044(2) 0.1253(19) 0.040(5) Uiso 1 1 d . . . H7 H 0.748(2) -0.1071(19) 0.5403(18) 0.035(5) Uiso 1 1 d . . . H8A H 0.821(2) 0.116(2) 0.533(2) 0.048(6) Uiso 1 1 d . . . H8B H 0.953(3) 0.019(2) 0.562(2) 0.059(7) Uiso 1 1 d . . . H8C H 0.889(3) 0.082(2) 0.426(2) 0.065(7) Uiso 1 1 d . . . H9A H 0.931(2) -0.213(2) 0.496(2) 0.045(6) Uiso 1 1 d . . . H9B H 0.787(2) -0.259(2) 0.4020(19) 0.041(5) Uiso 1 1 d . . . H9C H 0.878(2) -0.161(2) 0.3560(19) 0.038(5) Uiso 1 1 d . . . H10 H 0.2955(18) 0.0990(16) 0.4316(17) 0.025(4) Uiso 1 1 d . . . H11A H 0.215(3) -0.091(3) 0.382(2) 0.054(7) Uiso 1 1 d . . . H11B H 0.133(3) -0.067(3) 0.229(3) 0.075 Uiso 1 1 d . . . H11C H 0.089(3) -0.008(3) 0.355(3) 0.093(9) Uiso 1 1 d . . . H12A H 0.117(2) 0.2202(19) 0.3023(17) 0.034(5) Uiso 1 1 d . . . H12B H 0.157(2) 0.176(2) 0.181(2) 0.052(6) Uiso 1 1 d . . . H12C H 0.265(3) 0.278(3) 0.282(3) 0.084(9) Uiso 1 1 d . . . H15 H 0.866(2) -0.054(2) 1.026(2) 0.044(5) Uiso 1 1 d . . . H16 H 0.7162(19) -0.2282(19) 1.0186(16) 0.033(5) Uiso 1 1 d . . . H17 H 0.4873(19) -0.228(2) 0.8815(17) 0.037(5) Uiso 1 1 d . . . H19 H 0.788(2) 0.220(2) 0.819(2) 0.051(6) Uiso 1 1 d . . . H20A H 0.741(3) 0.281(3) 1.000(2) 0.069(8) Uiso 1 1 d . . . H20B H 0.895(3) 0.323(3) 0.994(3) 0.085(9) Uiso 1 1 d . . . H20C H 0.880(2) 0.200(2) 1.074(2) 0.050(6) Uiso 1 1 d . . . H21 H 0.3395(17) 0.0110(16) 0.6455(15) 0.021(4) Uiso 1 1 d . . . H21A H 1.020(3) 0.077(3) 0.968(2) 0.059(7) Uiso 1 1 d . . . H21B H 1.022(3) 0.194(3) 0.876(2) 0.062(7) Uiso 1 1 d . . . H21C H 0.964(2) 0.063(3) 0.812(2) 0.058(6) Uiso 1 1 d . . . H22A H 0.308(2) 0.126(2) 0.817(2) 0.061(7) Uiso 1 1 d . . . H22B H 0.171(2) 0.0367(19) 0.7373(18) 0.037(5) Uiso 1 1 d . . . H22C H 0.275(2) -0.021(2) 0.867(2) 0.049(6) Uiso 1 1 d . . . H23A H 0.191(3) -0.167(2) 0.622(2) 0.067(7) Uiso 1 1 d . . . H23B H 0.341(3) -0.226(3) 0.638(2) 0.070(8) Uiso 1 1 d . . . H24C H 0.277(3) -0.228(3) 0.757(3) 0.088(9) Uiso 1 1 d . . . H101 H 0.538(2) 0.236(2) 0.7455(17) 0.039(5) Uiso 1 1 d . . . H102 H 0.5000(18) 0.2339(18) 0.5282(15) 0.028(4) Uiso 1 1 d . . . H103 H 0.5653(18) -0.0397(19) 0.5730(17) 0.029(4) 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 C1 0.0249(7) 0.0171(6) 0.0196(7) -0.0002(5) 0.0094(5) -0.0013(5) C2 0.0232(7) 0.0206(6) 0.0240(7) -0.0009(5) 0.0094(5) -0.0012(5) C3 0.0285(8) 0.0267(6) 0.0270(8) -0.0007(6) 0.0138(6) -0.0004(6) C4 0.0331(8) 0.0318(7) 0.0204(8) -0.0011(6) 0.0117(6) -0.0006(6) C5 0.0268(7) 0.0303(7) 0.0221(7) 0.0007(6) 0.0068(6) 0.0005(6) C6 0.0231(7) 0.0226(6) 0.0230(7) -0.0012(5) 0.0094(6) -0.0002(5) C7 0.0253(8) 0.0278(7) 0.0285(8) -0.0002(6) 0.0083(6) 0.0047(5) C8 0.0317(9) 0.0326(8) 0.0507(12) -0.0077(8) -0.0042(8) 0.0026(7) C9 0.0282(8) 0.0299(7) 0.0385(10) -0.0016(7) 0.0107(7) 0.0051(6) C10 0.0238(7) 0.0357(8) 0.0230(8) -0.0027(6) 0.0079(6) 0.0022(6) C11 0.0481(13) 0.0467(11) 0.112(2) -0.0107(14) 0.0536(15) -0.0093(10) C12 0.0400(10) 0.0543(11) 0.0321(10) 0.0042(8) 0.0127(8) 0.0200(8) C13 0.0238(7) 0.0235(6) 0.0167(7) -0.0025(5) 0.0084(5) 0.0036(5) C14 0.0250(7) 0.0295(7) 0.0212(7) -0.0052(6) 0.0084(6) 0.0003(6) C15 0.0277(8) 0.0383(8) 0.0238(8) -0.0005(6) 0.0054(6) 0.0085(6) C16 0.0365(9) 0.0302(7) 0.0251(8) 0.0025(6) 0.0113(7) 0.0101(6) C17 0.0339(9) 0.0252(7) 0.0279(8) -0.0001(6) 0.0149(7) 0.0015(6) C18 0.0265(7) 0.0261(6) 0.0194(7) -0.0051(5) 0.0109(6) 0.0015(5) C19 0.0261(8) 0.0408(8) 0.0318(9) -0.0011(7) 0.0039(7) -0.0048(6) C20 0.0425(11) 0.0373(9) 0.0565(13) -0.0156(9) 0.0100(10) -0.0030(8) C21 0.0358(11) 0.0614(13) 0.0632(15) -0.0205(11) 0.0245(11) -0.0134(10) C22 0.0258(7) 0.0286(7) 0.0245(7) -0.0030(6) 0.0090(6) -0.0024(6) C23 0.0277(8) 0.0514(10) 0.0328(9) -0.0006(8) 0.0123(7) 0.0090(7) C24 0.0359(11) 0.0364(9) 0.0661(15) -0.0122(9) 0.0046(10) -0.0090(8) B1 0.0206(8) 0.0224(7) 0.0251(9) -0.0016(6) 0.0078(6) 0.0007(6) N1 0.0257(6) 0.0207(5) 0.0178(6) 0.0012(4) 0.0075(5) 0.0025(4) N2 0.0267(6) 0.0197(5) 0.0212(6) -0.0026(5) 0.0069(5) 0.0010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.4108(19) . ? C1 C6 1.412(2) . ? C1 N1 1.4280(18) . ? C2 C3 1.394(2) . ? C2 C7 1.522(2) . ? C3 C4 1.387(2) . ? C3 H3 0.99(2) . ? C4 C5 1.382(2) . ? C4 H4 1.009(19) . ? C5 C6 1.397(2) . ? C5 H5 1.00(2) . ? C6 C10 1.523(2) . ? C7 C9 1.531(2) . ? C7 C8 1.533(2) . ? C7 H7 1.02(2) . ? C8 H8A 0.98(2) . ? C8 H8B 0.98(2) . ? C8 H8C 1.05(3) . ? C9 H9A 1.00(2) . ? C9 H9B 0.96(2) . ? C9 H9C 1.01(2) . ? C10 C11 1.524(3) . ? C10 C12 1.538(2) . ? C10 H10 0.985(18) . ? C11 H11A 0.89(3) . ? C11 H11B 1.08(3) . ? C11 H11C 1.02(3) . ? C12 H12A 1.00(2) . ? C12 H12B 0.99(2) . ? C12 H12C 1.09(3) . ? C13 C14 1.4043(19) . ? C13 C18 1.4079(19) . ? C13 N2 1.4380(18) . ? C14 C15 1.401(2) . ? C14 C19 1.515(2) . ? C15 C16 1.378(2) . ? C15 H15 1.02(2) . ? C16 C17 1.387(2) . ? C16 H16 0.997(19) . ? C17 C18 1.400(2) . ? C17 H17 0.99(2) . ? C18 C22 1.522(2) . ? C19 C21 1.524(3) . ? C19 C20 1.525(3) . ? C19 H19 0.94(2) . ? C20 H20A 1.04(3) . ? C20 H20B 0.97(3) . ? C20 H20C 0.99(2) . ? C21 H21A 1.04(3) . ? C21 H21B 0.99(3) . ? C21 H21C 1.01(3) . ? C22 C24 1.526(2) . ? C22 C23 1.533(2) . ? C22 H21 1.012(17) . ? C23 H22A 1.08(3) . ? C23 H22B 0.99(2) . ? C23 H22C 0.99(2) . ? C24 H23A 0.96(3) . ? C24 H23B 1.01(3) . ? C24 H24C 1.05(3) . ? B1 N2 1.414(2) . ? B1 N1 1.4151(19) . ? B1 H102 1.092(18) . ? N1 H103 0.85(2) . ? N2 H101 0.93(2) . ? 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 _geom_angle_publ_flag C2 C1 C6 120.64(12) . . ? C2 C1 N1 119.26(12) . . ? C6 C1 N1 120.10(12) . . ? C3 C2 C1 118.66(13) . . ? C3 C2 C7 120.63(13) . . ? C1 C2 C7 120.70(13) . . ? C4 C3 C2 121.16(14) . . ? C4 C3 H3 118.7(11) . . ? C2 C3 H3 120.1(11) . . ? C5 C4 C3 119.62(14) . . ? C5 C4 H4 117.8(11) . . ? C3 C4 H4 122.6(11) . . ? C4 C5 C6 121.61(14) . . ? C4 C5 H5 121.7(11) . . ? C6 C5 H5 116.6(11) . . ? C5 C6 C1 118.21(12) . . ? C5 C6 C10 119.45(13) . . ? C1 C6 C10 122.26(13) . . ? C2 C7 C9 113.47(14) . . ? C2 C7 C8 110.58(13) . . ? C9 C7 C8 110.62(14) . . ? C2 C7 H7 107.6(11) . . ? C9 C7 H7 104.9(11) . . ? C8 C7 H7 109.4(11) . . ? C7 C8 H8A 112.2(13) . . ? C7 C8 H8B 108.5(14) . . ? H8A C8 H8B 111.4(19) . . ? C7 C8 H8C 110.8(14) . . ? H8A C8 H8C 107.2(19) . . ? H8B C8 H8C 106.6(19) . . ? C7 C9 H9A 112.3(12) . . ? C7 C9 H9B 110.9(12) . . ? H9A C9 H9B 108.9(18) . . ? C7 C9 H9C 111.5(12) . . ? H9A C9 H9C 107.1(17) . . ? H9B C9 H9C 105.9(17) . . ? C6 C10 C11 110.00(14) . . ? C6 C10 C12 111.99(14) . . ? C11 C10 C12 110.34(18) . . ? C6 C10 H10 108.7(10) . . ? C11 C10 H10 107.2(10) . . ? C12 C10 H10 108.5(10) . . ? C10 C11 H11A 101.1(17) . . ? C10 C11 H11B 111.7(15) . . ? H11A C11 H11B 120(2) . . ? C10 C11 H11C 106.4(19) . . ? H11A C11 H11C 102(3) . . ? H11B C11 H11C 114(2) . . ? C10 C12 H12A 106.8(11) . . ? C10 C12 H12B 111.1(14) . . ? H12A C12 H12B 110.3(17) . . ? C10 C12 H12C 111.5(15) . . ? H12A C12 H12C 108.8(19) . . ? H12B C12 H12C 108(2) . . ? C14 C13 C18 120.91(12) . . ? C14 C13 N2 119.62(12) . . ? C18 C13 N2 119.47(12) . . ? C15 C14 C13 118.38(13) . . ? C15 C14 C19 119.99(14) . . ? C13 C14 C19 121.61(13) . . ? C16 C15 C14 121.25(15) . . ? C16 C15 H15 117.5(12) . . ? C14 C15 H15 121.2(12) . . ? C15 C16 C17 120.01(14) . . ? C15 C16 H16 119.4(11) . . ? C17 C16 H16 120.6(11) . . ? C16 C17 C18 120.83(14) . . ? C16 C17 H17 118.3(11) . . ? C18 C17 H17 120.8(11) . . ? C17 C18 C13 118.55(13) . . ? C17 C18 C22 120.24(13) . . ? C13 C18 C22 121.02(13) . . ? C14 C19 C21 112.63(16) . . ? C14 C19 C20 110.35(16) . . ? C21 C19 C20 111.16(16) . . ? C14 C19 H19 110.7(14) . . ? C21 C19 H19 107.7(14) . . ? C20 C19 H19 103.9(14) . . ? C19 C20 H20A 112.2(14) . . ? C19 C20 H20B 108.2(18) . . ? H20A C20 H20B 111(2) . . ? C19 C20 H20C 109.9(13) . . ? H20A C20 H20C 106(2) . . ? H20B C20 H20C 109(2) . . ? C19 C21 H21A 109.8(14) . . ? C19 C21 H21B 110.2(15) . . ? H21A C21 H21B 105(2) . . ? C19 C21 H21C 114.7(13) . . ? H21A C21 H21C 113(2) . . ? H21B C21 H21C 104(2) . . ? C18 C22 C24 113.71(14) . . ? C18 C22 C23 108.62(12) . . ? C24 C22 C23 110.97(15) . . ? C18 C22 H21 108.6(9) . . ? C24 C22 H21 109.3(9) . . ? C23 C22 H21 105.3(9) . . ? C22 C23 H22A 112.5(14) . . ? C22 C23 H22B 107.0(12) . . ? H22A C23 H22B 108.4(17) . . ? C22 C23 H22C 107.9(13) . . ? H22A C23 H22C 109.8(18) . . ? H22B C23 H22C 111.3(17) . . ? C22 C24 H23A 110.5(15) . . ? C22 C24 H23B 109.3(16) . . ? H23A C24 H23B 109(2) . . ? C22 C24 H24C 109.0(16) . . ? H23A C24 H24C 109(2) . . ? H23B C24 H24C 110(2) . . ? N2 B1 N1 121.93(13) . . ? N2 B1 H102 119.3(9) . . ? N1 B1 H102 118.8(9) . . ? B1 N1 C1 125.76(12) . . ? B1 N1 H103 119.2(12) . . ? C1 N1 H103 114.8(13) . . ? B1 N2 C13 125.06(12) . . ? B1 N2 H101 119.2(12) . . ? C13 N2 H101 115.4(12) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.12 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.166 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.038