Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title # Attachment 'ZNCLS10.CIF' ;Bis- and Tris(2-seleno-1-methylimidazolyl)hydroborato Complexes, {[BseMe]ZnX}2 (X = Cl, I), [BseMe]2Zn and [TseMe]Re(CO)3: Structural Evidence that the [BseMe] Ligand is not Merely a "Heavier" Version of the Sulfur Counterpart, [BmMe] ; _publ_contact_author_name 'Prof. G.Parkin' _publ_contact_author_email PARKIN@COLUMBIA.EDU loop_ _publ_author_name 'G. Parkin' 'Daniela Buccella' 'Victoria K. Landry' 'Keliang Pang.' data_zncls10 _database_code_depnum_ccdc_archive 'CCDC 627367' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B2 Cl2 N8 Se4 Zn2' _chemical_formula_weight 867.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5666(6) _cell_length_b 8.5632(7) _cell_length_c 11.8893(10) _cell_angle_alpha 70.0870(10) _cell_angle_beta 76.185(2) _cell_angle_gamma 70.401(2) _cell_volume 675.56(10) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 2239 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 7.384 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5255 _exptl_absorpt_correction_T_max 0.5255 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4858 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3058 _reflns_number_gt 2398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0401P)^2^+0.2759P] 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 3058 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Zn Zn -0.40283(7) 0.08022(6) 0.33256(5) 0.03345(14) Uani 1 1 d . . . Cl Cl -0.45982(17) 0.35793(14) 0.22926(12) 0.0460(3) Uani 1 1 d . . . B B 0.0211(6) -0.0776(6) 0.2524(5) 0.0277(10) Uani 1 1 d . . . H1 H 0.157(5) -0.038(5) 0.215(3) 0.020(10) Uiso 1 1 d . . . H2 H -0.100(6) 0.052(5) 0.253(4) 0.029(11) Uiso 1 1 d . . . Se1 Se -0.26453(5) -0.01540(5) 0.51980(4) 0.02630(12) Uani 1 1 d . . . Se2 Se -0.41266(6) -0.12775(6) 0.23881(4) 0.02991(12) Uani 1 1 d . . . N11 N 0.0422(4) -0.2120(4) 0.3790(3) 0.0252(7) Uani 1 1 d . . . N12 N 0.0311(5) -0.3308(4) 0.5744(3) 0.0264(7) Uani 1 1 d . . . N21 N -0.0088(4) -0.1595(4) 0.1627(3) 0.0276(8) Uani 1 1 d . . . N22 N -0.1371(5) -0.2411(4) 0.0532(3) 0.0301(8) Uani 1 1 d . . . C11 C -0.0543(5) -0.1973(5) 0.4869(4) 0.0245(8) Uani 1 1 d . . . C12 C 0.1930(6) -0.3585(5) 0.3997(4) 0.0307(9) Uani 1 1 d . . . H12A H 0.2848 -0.3998 0.3399 0.037 Uiso 1 1 calc R . . C13 C 0.1871(6) -0.4328(6) 0.5197(4) 0.0357(10) Uani 1 1 d . . . H13A H 0.2727 -0.5346 0.5587 0.043 Uiso 1 1 calc R . . C14 C -0.0248(7) -0.3611(6) 0.7040(4) 0.0359(10) Uani 1 1 d . . . H14A H -0.1388 -0.2719 0.7198 0.054 Uiso 1 1 calc R . . H14B H 0.0763 -0.3582 0.7398 0.054 Uiso 1 1 calc R . . H14C H -0.0491 -0.4734 0.7391 0.054 Uiso 1 1 calc R . . C21 C -0.1705(5) -0.1768(5) 0.1483(4) 0.0250(8) Uani 1 1 d . . . C22 C 0.1315(6) -0.2168(6) 0.0745(4) 0.0362(11) Uani 1 1 d . . . H22A H 0.2597 -0.2203 0.0640 0.043 Uiso 1 1 calc R . . C23 C 0.0532(6) -0.2664(6) 0.0071(4) 0.0384(11) Uani 1 1 d . . . H23A H 0.1158 -0.3100 -0.0589 0.046 Uiso 1 1 calc R . . C24 C -0.2788(7) -0.2724(6) 0.0052(4) 0.0412(11) Uani 1 1 d . . . H24A H -0.4011 -0.2448 0.0541 0.062 Uiso 1 1 calc R . . H24B H -0.2424 -0.3931 0.0070 0.062 Uiso 1 1 calc R . . H24C H -0.2869 -0.2002 -0.0775 0.062 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 Zn 0.0424(3) 0.0225(3) 0.0322(3) -0.0065(2) -0.0103(2) -0.0027(2) Cl 0.0396(6) 0.0228(6) 0.0543(8) -0.0013(5) 0.0071(5) -0.0013(5) B 0.022(2) 0.028(3) 0.029(3) -0.009(2) 0.0000(19) -0.0045(18) Se1 0.0220(2) 0.0283(2) 0.0268(2) -0.00991(18) -0.00034(16) -0.00473(16) Se2 0.0231(2) 0.0345(2) 0.0331(3) -0.0148(2) -0.00052(17) -0.00624(17) N11 0.0223(16) 0.0237(17) 0.029(2) -0.0093(15) -0.0039(14) -0.0037(13) N12 0.0301(17) 0.0245(18) 0.0251(19) -0.0054(15) -0.0050(15) -0.0091(14) N21 0.0233(16) 0.0297(19) 0.0210(18) -0.0033(15) 0.0017(14) -0.0035(14) N22 0.041(2) 0.0261(18) 0.0187(18) -0.0063(15) -0.0016(15) -0.0051(15) C11 0.0240(19) 0.023(2) 0.027(2) -0.0058(17) -0.0066(17) -0.0053(16) C12 0.027(2) 0.026(2) 0.035(3) -0.0124(19) -0.0052(18) 0.0031(17) C13 0.034(2) 0.024(2) 0.045(3) -0.010(2) -0.010(2) 0.0004(18) C14 0.044(3) 0.036(3) 0.024(2) -0.003(2) -0.008(2) -0.011(2) C21 0.029(2) 0.0170(19) 0.022(2) -0.0019(16) -0.0042(17) -0.0010(16) C22 0.029(2) 0.036(3) 0.030(3) -0.008(2) 0.0051(19) 0.0006(19) C23 0.042(3) 0.034(3) 0.023(2) -0.007(2) 0.005(2) 0.002(2) C24 0.056(3) 0.038(3) 0.032(3) -0.015(2) -0.008(2) -0.010(2) _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 Zn Cl 2.2192(12) . ? Zn Se2 2.4291(7) . ? Zn Se1 2.4529(7) . ? Zn Se1 2.8085(7) 2_456 ? B N21 1.553(6) . ? B N11 1.558(6) . ? Se1 C11 1.888(4) . ? Se1 Zn 2.8085(7) 2_456 ? Se2 C21 1.882(4) . ? N11 C11 1.340(5) . ? N11 C12 1.378(5) . ? N12 C11 1.350(5) . ? N12 C13 1.381(5) . ? N12 C14 1.453(5) . ? N21 C21 1.337(5) . ? N21 C22 1.391(5) . ? N22 C21 1.355(5) . ? N22 C23 1.384(6) . ? N22 C24 1.463(6) . ? C12 C13 1.346(6) . ? C22 C23 1.341(7) . ? 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 Cl Zn Se2 119.53(5) . . ? Cl Zn Se1 118.17(4) . . ? Se2 Zn Se1 120.93(2) . . ? Cl Zn Se1 109.75(4) . 2_456 ? Se2 Zn Se1 85.62(2) . 2_456 ? Se1 Zn Se1 86.55(2) . 2_456 ? N21 B N11 110.5(3) . . ? C11 Se1 Zn 99.45(12) . . ? C11 Se1 Zn 121.39(12) . 2_456 ? Zn Se1 Zn 93.45(2) . 2_456 ? C21 Se2 Zn 103.56(12) . . ? C11 N11 C12 107.3(3) . . ? C11 N11 B 128.8(3) . . ? C12 N11 B 123.0(3) . . ? C11 N12 C13 108.1(4) . . ? C11 N12 C14 126.8(4) . . ? C13 N12 C14 125.1(4) . . ? C21 N21 C22 107.3(4) . . ? C21 N21 B 128.0(3) . . ? C22 N21 B 124.5(4) . . ? C21 N22 C23 108.1(4) . . ? C21 N22 C24 125.9(4) . . ? C23 N22 C24 126.0(4) . . ? N11 C11 N12 109.0(3) . . ? N11 C11 Se1 127.9(3) . . ? N12 C11 Se1 123.0(3) . . ? C13 C12 N11 108.8(4) . . ? C12 C13 N12 106.8(4) . . ? N21 C21 N22 108.9(3) . . ? N21 C21 Se2 129.4(3) . . ? N22 C21 Se2 121.7(3) . . ? C23 C22 N21 108.6(4) . . ? C22 C23 N22 107.0(4) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.601 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.112 # Attachment 'BSEZNS10.CIF' data_bsezns10 _database_code_depnum_ccdc_archive 'CCDC 627368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B2 N8 Se4 Zn' _chemical_formula_weight 731.26 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.5572(4) _cell_length_b 14.3524(5) _cell_length_c 18.9224(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.4550(10) _cell_angle_gamma 90.00 _cell_volume 2590.84(18) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 7261 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.35 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 6.588 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5587 _exptl_absorpt_correction_T_max 0.5587 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18394 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.37 _reflns_number_total 6123 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0300P)^2^+0.0000P] 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 6123 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.002 _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 Zn Zn 1.12484(4) 0.25443(2) 0.019095(19) 0.03045(9) Uani 1 1 d . . . Se1 Se 0.94803(3) 0.22379(2) 0.105426(18) 0.03500(9) Uani 1 1 d . . . Se2 Se 1.26376(3) 0.39500(2) 0.042029(18) 0.04128(10) Uani 1 1 d . . . Se3 Se 1.00000(3) 0.28768(2) -0.094684(18) 0.04130(10) Uani 1 1 d . . . Se4 Se 1.25467(3) 0.10849(2) 0.026037(19) 0.04270(10) Uani 1 1 d . . . B1 B 1.2287(4) 0.3113(2) 0.2153(2) 0.0320(8) Uani 1 1 d . . . H1 H 1.150(3) 0.355(2) 0.1859(17) 0.048 Uiso 1 1 d . . . H2 H 1.263(3) 0.327(2) 0.2751(17) 0.048 Uiso 1 1 d . . . B2 B 1.3134(5) 0.1831(3) -0.1468(2) 0.0438(10) Uani 1 1 d . . . H3 H 1.356(4) 0.159(2) -0.199(2) 0.066 Uiso 1 1 d . . . H4 H 1.215(3) 0.143(2) -0.1297(18) 0.066 Uiso 1 1 d . . . N11 N 1.1802(2) 0.20632(15) 0.21083(13) 0.0291(5) Uani 1 1 d . . . N12 N 1.0821(3) 0.07327(16) 0.18159(14) 0.0362(6) Uani 1 1 d . . . N21 N 1.3702(2) 0.32142(15) 0.17792(12) 0.0274(5) Uani 1 1 d . . . N22 N 1.5338(3) 0.34804(17) 0.10472(13) 0.0332(6) Uani 1 1 d . . . N31 N 1.2755(3) 0.28965(17) -0.15262(14) 0.0388(6) Uani 1 1 d . . . N32 N 1.1709(3) 0.42483(18) -0.15635(16) 0.0485(7) Uani 1 1 d . . . N41 N 1.4306(3) 0.16710(17) -0.08629(15) 0.0378(6) Uani 1 1 d . . . N42 N 1.5470(3) 0.12417(17) 0.01159(16) 0.0420(7) Uani 1 1 d . . . C11 C 1.0783(3) 0.16616(18) 0.16908(15) 0.0277(6) Uani 1 1 d . . . C12 C 1.2471(3) 0.1365(2) 0.25001(18) 0.0433(8) Uani 1 1 d . . . H12A H 1.3225 0.1449 0.2836 0.052 Uiso 1 1 calc R . . C13 C 1.1868(3) 0.0546(2) 0.23232(19) 0.0457(9) Uani 1 1 d . . . H13A H 1.2115 -0.0041 0.2511 0.055 Uiso 1 1 calc R . . C14 C 0.9928(4) 0.0031(2) 0.1460(2) 0.0574(10) Uani 1 1 d . . . H14A H 0.9267 0.0332 0.1125 0.086 Uiso 1 1 calc R . . H14B H 0.9420 -0.0306 0.1808 0.086 Uiso 1 1 calc R . . H14C H 1.0504 -0.0402 0.1211 0.086 Uiso 1 1 calc R . . C21 C 1.3940(3) 0.35055(18) 0.11208(16) 0.0279(6) Uani 1 1 d . . . C22 C 1.4988(3) 0.3017(2) 0.21194(17) 0.0344(7) Uani 1 1 d . . . H22A H 1.5133 0.2804 0.2588 0.041 Uiso 1 1 calc R . . C23 C 1.5999(3) 0.3178(2) 0.16698(18) 0.0373(7) Uani 1 1 d . . . H23A H 1.6969 0.3100 0.1764 0.045 Uiso 1 1 calc R . . C24 C 1.6033(4) 0.3759(3) 0.04155(19) 0.0516(9) Uani 1 1 d . . . H24A H 1.5335 0.3948 0.0050 0.077 Uiso 1 1 calc R . . H24B H 1.6567 0.3238 0.0247 0.077 Uiso 1 1 calc R . . H24C H 1.6659 0.4277 0.0529 0.077 Uiso 1 1 calc R . . C31 C 1.1588(3) 0.3353(2) -0.13593(16) 0.0358(7) Uani 1 1 d . . . C32 C 1.3617(4) 0.3542(3) -0.1821(2) 0.0582(11) Uani 1 1 d . . . H32A H 1.4510 0.3416 -0.1981 0.070 Uiso 1 1 calc R . . C33 C 1.2992(4) 0.4367(3) -0.1844(2) 0.0648(12) Uani 1 1 d . . . H33A H 1.3355 0.4925 -0.2019 0.078 Uiso 1 1 calc R . . C34 C 1.0693(4) 0.4992(3) -0.1469(3) 0.0746(13) Uani 1 1 d . . . H34A H 0.9871 0.4736 -0.1262 0.112 Uiso 1 1 calc R . . H34B H 1.0421 0.5268 -0.1924 0.112 Uiso 1 1 calc R . . H34C H 1.1111 0.5465 -0.1157 0.112 Uiso 1 1 calc R . . C41 C 1.4175(3) 0.1375(2) -0.01932(17) 0.0333(7) Uani 1 1 d . . . C42 C 1.5735(4) 0.1725(2) -0.0960(2) 0.0522(10) Uani 1 1 d . . . H42A H 1.6138 0.1917 -0.1377 0.063 Uiso 1 1 calc R . . C43 C 1.6439(4) 0.1461(2) -0.0366(2) 0.0525(10) Uani 1 1 d . . . H43A H 1.7419 0.1430 -0.0290 0.063 Uiso 1 1 calc R . . C44 C 1.5805(4) 0.0911(2) 0.0837(2) 0.0511(9) Uani 1 1 d . . . H44A H 1.4945 0.0801 0.1070 0.077 Uiso 1 1 calc R . . H44B H 1.6361 0.1376 0.1097 0.077 Uiso 1 1 calc R . . H44C H 1.6333 0.0334 0.0821 0.077 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 Zn 0.02706(19) 0.03763(19) 0.0264(2) 0.00243(15) -0.00096(15) 0.00081(14) Se1 0.02114(15) 0.04705(18) 0.0368(2) 0.00583(14) 0.00132(13) 0.00105(13) Se2 0.0442(2) 0.04121(18) 0.0370(2) 0.01488(15) -0.00935(15) -0.01147(14) Se3 0.03395(18) 0.0569(2) 0.0318(2) 0.00503(16) -0.00876(14) 0.00003(15) Se4 0.03971(19) 0.04066(18) 0.0492(2) 0.01180(16) 0.01472(16) 0.00915(14) B1 0.039(2) 0.0270(16) 0.030(2) -0.0013(15) 0.0030(16) -0.0035(15) B2 0.060(3) 0.039(2) 0.032(2) -0.0073(17) 0.005(2) 0.0018(19) N11 0.0285(13) 0.0283(12) 0.0303(14) 0.0030(11) -0.0010(11) -0.0028(10) N12 0.0390(15) 0.0299(12) 0.0395(16) 0.0011(12) 0.0005(13) -0.0076(11) N21 0.0298(13) 0.0252(11) 0.0272(14) -0.0008(10) 0.0010(11) -0.0042(10) N22 0.0330(14) 0.0338(13) 0.0335(15) 0.0019(11) 0.0071(12) -0.0047(11) N31 0.0484(17) 0.0391(14) 0.0295(15) 0.0029(12) 0.0063(13) -0.0007(13) N32 0.0544(19) 0.0371(15) 0.054(2) 0.0022(14) 0.0020(16) 0.0041(13) N41 0.0385(15) 0.0365(14) 0.0393(17) -0.0024(12) 0.0107(13) 0.0007(12) N42 0.0378(16) 0.0367(14) 0.0515(19) -0.0043(13) 0.0032(14) 0.0028(12) C11 0.0260(15) 0.0307(14) 0.0270(16) 0.0008(12) 0.0055(12) -0.0036(12) C12 0.046(2) 0.0375(18) 0.044(2) 0.0112(15) -0.0149(16) -0.0043(15) C13 0.048(2) 0.0349(17) 0.052(2) 0.0145(16) -0.0114(18) -0.0011(15) C14 0.065(3) 0.0389(18) 0.067(3) -0.0013(18) -0.010(2) -0.0235(18) C21 0.0336(16) 0.0220(13) 0.0278(16) -0.0014(12) -0.0002(13) -0.0056(12) C22 0.0359(18) 0.0344(16) 0.0319(18) 0.0011(13) -0.0061(14) 0.0026(13) C23 0.0309(17) 0.0390(16) 0.042(2) 0.0021(15) 0.0012(15) -0.0008(14) C24 0.045(2) 0.062(2) 0.049(2) 0.0087(19) 0.0148(18) -0.0060(18) C31 0.0394(18) 0.0414(17) 0.0261(17) 0.0005(14) -0.0037(14) -0.0014(14) C32 0.066(3) 0.050(2) 0.062(3) 0.0053(19) 0.027(2) -0.0024(19) C33 0.077(3) 0.043(2) 0.076(3) 0.011(2) 0.022(2) -0.008(2) C34 0.071(3) 0.042(2) 0.110(4) 0.005(2) 0.002(3) 0.015(2) C41 0.0323(17) 0.0286(14) 0.0393(19) -0.0054(13) 0.0043(14) 0.0026(12) C42 0.043(2) 0.055(2) 0.061(3) -0.0043(19) 0.0222(19) -0.0010(18) C43 0.0330(19) 0.054(2) 0.071(3) -0.003(2) 0.0124(19) -0.0011(17) C44 0.052(2) 0.048(2) 0.052(2) -0.0027(18) -0.0053(19) 0.0039(17) _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 Zn Se4 2.4340(5) . ? Zn Se2 2.4397(5) . ? Zn Se3 2.4448(5) . ? Zn Se1 2.4597(5) . ? Se1 C11 1.872(3) . ? Se2 C21 1.875(3) . ? Se3 C31 1.877(3) . ? Se4 C41 1.869(3) . ? B1 N21 1.570(4) . ? B1 N11 1.577(4) . ? B2 N41 1.569(5) . ? B2 N31 1.574(5) . ? N11 C11 1.346(3) . ? N11 C12 1.380(4) . ? N12 C11 1.354(3) . ? N12 C13 1.371(4) . ? N12 C14 1.458(4) . ? N21 C21 1.346(4) . ? N21 C22 1.382(3) . ? N22 C21 1.352(4) . ? N22 C23 1.373(4) . ? N22 C24 1.458(4) . ? N31 C31 1.347(4) . ? N31 C32 1.380(4) . ? N32 C31 1.349(4) . ? N32 C33 1.376(4) . ? N32 C34 1.461(4) . ? N41 C41 1.349(4) . ? N41 C42 1.392(4) . ? N42 C41 1.350(4) . ? N42 C43 1.375(4) . ? N42 C44 1.461(4) . ? C12 C13 1.342(4) . ? C22 C23 1.345(4) . ? C32 C33 1.325(5) . ? C42 C43 1.329(5) . ? 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 Se4 Zn Se2 115.583(18) . . ? Se4 Zn Se3 115.827(19) . . ? Se2 Zn Se3 103.103(17) . . ? Se4 Zn Se1 100.295(16) . . ? Se2 Zn Se1 114.708(18) . . ? Se3 Zn Se1 107.542(17) . . ? C11 Se1 Zn 92.83(8) . . ? C21 Se2 Zn 100.10(8) . . ? C31 Se3 Zn 94.20(9) . . ? C41 Se4 Zn 102.68(9) . . ? N21 B1 N11 108.8(2) . . ? N41 B2 N31 110.2(3) . . ? C11 N11 C12 107.4(2) . . ? C11 N11 B1 129.8(2) . . ? C12 N11 B1 122.7(3) . . ? C11 N12 C13 109.0(2) . . ? C11 N12 C14 126.2(3) . . ? C13 N12 C14 124.8(3) . . ? C21 N21 C22 107.5(2) . . ? C21 N21 B1 130.0(3) . . ? C22 N21 B1 122.5(3) . . ? C21 N22 C23 109.1(2) . . ? C21 N22 C24 125.4(3) . . ? C23 N22 C24 125.5(3) . . ? C31 N31 C32 106.9(3) . . ? C31 N31 B2 130.2(3) . . ? C32 N31 B2 122.7(3) . . ? C31 N32 C33 108.8(3) . . ? C31 N32 C34 126.3(3) . . ? C33 N32 C34 124.9(3) . . ? C41 N41 C42 106.8(3) . . ? C41 N41 B2 128.9(3) . . ? C42 N41 B2 124.0(3) . . ? C41 N42 C43 108.5(3) . . ? C41 N42 C44 126.5(3) . . ? C43 N42 C44 125.1(3) . . ? N11 C11 N12 107.9(3) . . ? N11 C11 Se1 128.2(2) . . ? N12 C11 Se1 123.9(2) . . ? C13 C12 N11 108.9(3) . . ? C12 C13 N12 106.7(3) . . ? N21 C21 N22 108.1(2) . . ? N21 C21 Se2 128.2(2) . . ? N22 C21 Se2 123.7(2) . . ? C23 C22 N21 108.8(3) . . ? C22 C23 N22 106.6(3) . . ? N31 C31 N32 108.0(3) . . ? N31 C31 Se3 128.5(2) . . ? N32 C31 Se3 123.4(2) . . ? C33 C32 N31 109.6(3) . . ? C32 C33 N32 106.7(3) . . ? N41 C41 N42 108.5(3) . . ? N41 C41 Se4 128.9(2) . . ? N42 C41 Se4 122.4(2) . . ? C43 C42 N41 108.9(3) . . ? C42 C43 N42 107.4(3) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.440 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.098 # Attachment 'MERESNEW.CIF' data_meresnew _database_code_depnum_ccdc_archive 'CCDC 627369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H16 B N6 O3 Re Se3' _chemical_formula_weight 762.23 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 14.5312(9) _cell_length_b 14.5312(9) _cell_length_c 18.233(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3334.2(5) _cell_formula_units_Z 6 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 2354 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 23.39 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 10.408 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.2300 _exptl_absorpt_correction_T_max 0.6242 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7934 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2361 _reflns_number_gt 1844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0285P)^2^+0.0000P] 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 0.00012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(18) _refine_ls_number_reflns 2361 _refine_ls_number_parameters 178 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _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 Re1 Re 1.3333 0.6667 -0.06199(3) 0.03210(19) Uani 1 3 d S . . Re2 Re 1.3333 0.6667 0.44734(3) 0.0391(2) Uani 1 3 d S . . Se1 Se 1.16310(8) 0.60861(8) 0.01791(6) 0.0390(3) Uani 1 1 d . . . Se2 Se 1.31197(10) 0.80466(9) 0.52924(6) 0.0458(3) Uani 1 1 d . . . B1 B 1.3333 0.6667 0.1760(11) 0.038(6) Uani 1 3 d SD . . H10A H 1.3333 0.6667 0.2383(16) 0.045 Uiso 1 3 d SD . . B2 B 1.3333 0.6667 0.6872(15) 0.036(5) Uani 1 3 d SD . . H20A H 1.3333 0.6667 0.7497(19) 0.043 Uiso 1 3 d SD . . O1 O 1.5313(7) 0.7390(7) -0.1561(4) 0.055(2) Uani 1 1 d . . . O2 O 1.1440(8) 0.6316(9) 0.3531(5) 0.088(3) Uani 1 1 d . . . N11 N 1.2349(7) 0.5590(7) 0.1535(4) 0.0367(19) Uani 1 1 d . . . N12 N 1.0960(6) 0.4228(6) 0.1046(4) 0.037(2) Uani 1 1 d . . . N21 N 1.2361(6) 0.6757(6) 0.6620(4) 0.0330(18) Uani 1 1 d . . . N22 N 1.1152(8) 0.6908(8) 0.6036(5) 0.057(3) Uani 1 1 d . . . C1 C 1.4558(9) 0.7125(9) -0.1196(6) 0.043(3) Uani 1 1 d . . . C11 C 1.1685(7) 0.5275(7) 0.0956(5) 0.030(2) Uani 1 1 d . . . C12 C 1.2024(9) 0.4716(9) 0.1980(6) 0.042(3) Uani 1 1 d . . . H12A H 1.2351 0.4708 0.2423 0.050 Uiso 1 1 calc R . . C13 C 1.1180(8) 0.3885(8) 0.1690(5) 0.038(3) Uani 1 1 d . . . H13A H 1.0805 0.3196 0.1886 0.046 Uiso 1 1 calc R . . C14 C 1.0112(8) 0.3560(8) 0.0529(6) 0.045(3) Uani 1 1 d . . . H14A H 1.0122 0.3989 0.0118 0.068 Uiso 1 1 calc R . . H14B H 0.9430 0.3255 0.0774 0.068 Uiso 1 1 calc R . . H14C H 1.0225 0.2995 0.0351 0.068 Uiso 1 1 calc R . . C2 C 1.2167(11) 0.6441(11) 0.3886(6) 0.061(4) Uani 1 1 d . . . C21 C 1.2174(8) 0.7186(8) 0.6018(5) 0.039(2) Uani 1 1 d . . . C22 C 1.1431(9) 0.6206(9) 0.6994(6) 0.048(3) Uani 1 1 d . . . H22A H 1.1329 0.5811 0.7425 0.057 Uiso 1 1 calc R . . C23 C 1.0686(9) 0.6324(11) 0.6642(7) 0.063(4) Uani 1 1 d . . . H23A H 0.9977 0.6052 0.6788 0.076 Uiso 1 1 calc R . . C24 C 1.0613(13) 0.7192(13) 0.5484(7) 0.085(5) Uani 1 1 d . . . H24A H 1.1116 0.7619 0.5105 0.128 Uiso 1 1 calc R . . H24B H 1.0324 0.7596 0.5711 0.128 Uiso 1 1 calc R . . H24C H 1.0042 0.6551 0.5267 0.128 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 Re1 0.0329(3) 0.0329(3) 0.0305(4) 0.000 0.000 0.01645(13) Re2 0.0452(3) 0.0452(3) 0.0268(4) 0.000 0.000 0.02258(15) Se1 0.0319(6) 0.0449(7) 0.0430(6) 0.0122(5) 0.0033(5) 0.0213(6) Se2 0.0641(8) 0.0434(7) 0.0414(6) 0.0107(5) 0.0092(6) 0.0356(7) B1 0.031(8) 0.031(8) 0.050(16) 0.000 0.000 0.016(4) B2 0.030(7) 0.030(7) 0.047(13) 0.000 0.000 0.015(3) O1 0.048(5) 0.069(6) 0.046(4) 0.007(4) 0.016(4) 0.027(5) O2 0.082(8) 0.136(9) 0.055(5) 0.011(6) -0.016(5) 0.061(7) N11 0.036(5) 0.039(5) 0.038(4) 0.006(4) 0.000(4) 0.021(4) N12 0.032(5) 0.037(5) 0.043(5) 0.013(4) 0.013(4) 0.019(4) N21 0.034(5) 0.038(5) 0.029(4) 0.001(4) 0.011(4) 0.020(4) N22 0.049(6) 0.081(8) 0.054(6) -0.001(5) 0.004(5) 0.043(6) C1 0.053(8) 0.048(7) 0.038(6) -0.014(5) -0.010(6) 0.033(7) C11 0.028(5) 0.035(6) 0.039(5) 0.006(4) 0.008(4) 0.024(5) C12 0.043(7) 0.038(7) 0.043(6) 0.012(5) 0.008(5) 0.020(6) C13 0.036(6) 0.020(5) 0.054(6) 0.013(5) -0.004(5) 0.011(5) C14 0.038(6) 0.034(6) 0.060(7) -0.019(5) -0.016(5) 0.014(5) C2 0.068(9) 0.085(10) 0.037(6) -0.006(6) -0.011(6) 0.045(8) C21 0.040(6) 0.046(7) 0.041(6) -0.007(5) -0.001(5) 0.029(6) C22 0.047(8) 0.043(7) 0.050(6) 0.008(5) 0.020(6) 0.021(6) C23 0.034(7) 0.093(10) 0.069(8) -0.007(8) 0.013(6) 0.037(7) C24 0.107(12) 0.142(14) 0.066(8) -0.024(9) -0.031(8) 0.107(12) _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 Re1 C1 1.878(12) 2_755 ? Re1 C1 1.878(12) 3_775 ? Re1 C1 1.878(12) . ? Re1 Se1 2.6203(11) 3_775 ? Re1 Se1 2.6203(11) . ? Re1 Se1 2.6203(11) 2_755 ? Re2 C2 1.890(13) . ? Re2 C2 1.890(13) 3_775 ? Re2 C2 1.890(13) 2_755 ? Re2 Se2 2.6400(12) . ? Re2 Se2 2.6400(12) 2_755 ? Re2 Se2 2.6400(12) 3_775 ? Se1 C11 1.870(9) . ? Se2 C21 1.867(10) . ? B1 N11 1.557(10) 3_775 ? B1 N11 1.557(10) . ? B1 N11 1.557(10) 2_755 ? B2 N21 1.552(11) . ? B2 N21 1.552(11) 3_775 ? B2 N21 1.552(11) 2_755 ? O1 C1 1.171(12) . ? O2 C2 1.173(14) . ? N11 C11 1.347(12) . ? N11 C12 1.377(13) . ? N12 C11 1.359(11) . ? N12 C13 1.373(11) . ? N12 C14 1.468(12) . ? N21 C21 1.356(11) . ? N21 C22 1.360(13) . ? N22 C21 1.329(13) . ? N22 C23 1.351(15) . ? N22 C24 1.456(14) . ? C12 C13 1.327(14) . ? C22 C23 1.341(16) . ? 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 C1 Re1 C1 91.7(4) 2_755 3_775 ? C1 Re1 C1 91.7(4) 2_755 . ? C1 Re1 C1 91.7(4) 3_775 . ? C1 Re1 Se1 89.4(3) 2_755 3_775 ? C1 Re1 Se1 178.2(3) 3_775 3_775 ? C1 Re1 Se1 86.8(3) . 3_775 ? C1 Re1 Se1 86.8(3) 2_755 . ? C1 Re1 Se1 89.4(3) 3_775 . ? C1 Re1 Se1 178.2(3) . . ? Se1 Re1 Se1 92.09(4) 3_775 . ? C1 Re1 Se1 178.2(4) 2_755 2_755 ? C1 Re1 Se1 86.8(3) 3_775 2_755 ? C1 Re1 Se1 89.4(3) . 2_755 ? Se1 Re1 Se1 92.09(4) 3_775 2_755 ? Se1 Re1 Se1 92.09(4) . 2_755 ? C2 Re2 C2 91.1(5) . 3_775 ? C2 Re2 C2 91.1(5) . 2_755 ? C2 Re2 C2 91.1(5) 3_775 2_755 ? C2 Re2 Se2 90.9(4) . . ? C2 Re2 Se2 86.9(4) 3_775 . ? C2 Re2 Se2 177.2(4) 2_755 . ? C2 Re2 Se2 86.9(4) . 2_755 ? C2 Re2 Se2 177.2(4) 3_775 2_755 ? C2 Re2 Se2 90.9(4) 2_755 2_755 ? Se2 Re2 Se2 91.15(4) . 2_755 ? C2 Re2 Se2 177.2(4) . 3_775 ? C2 Re2 Se2 90.9(4) 3_775 3_775 ? C2 Re2 Se2 86.9(4) 2_755 3_775 ? Se2 Re2 Se2 91.15(4) . 3_775 ? Se2 Re2 Se2 91.15(4) 2_755 3_775 ? C11 Se1 Re1 107.1(3) . . ? C21 Se2 Re2 102.6(3) . . ? N11 B1 N11 113.3(6) 3_775 . ? N11 B1 N11 113.3(6) 3_775 2_755 ? N11 B1 N11 113.3(6) . 2_755 ? N21 B2 N21 111.6(9) . 3_775 ? N21 B2 N21 111.6(9) . 2_755 ? N21 B2 N21 111.6(9) 3_775 2_755 ? C11 N11 C12 106.9(9) . . ? C11 N11 B1 133.6(9) . . ? C12 N11 B1 119.4(9) . . ? C11 N12 C13 108.6(8) . . ? C11 N12 C14 126.0(8) . . ? C13 N12 C14 125.4(8) . . ? C21 N21 C22 107.9(9) . . ? C21 N21 B2 132.8(11) . . ? C22 N21 B2 118.7(10) . . ? C21 N22 C23 110.1(10) . . ? C21 N22 C24 125.0(11) . . ? C23 N22 C24 124.9(11) . . ? O1 C1 Re1 178.7(10) . . ? N11 C11 N12 108.0(8) . . ? N11 C11 Se1 128.9(7) . . ? N12 C11 Se1 122.9(7) . . ? C13 C12 N11 109.8(10) . . ? C12 C13 N12 106.8(9) . . ? O2 C2 Re2 178.6(12) . . ? N22 C21 N21 106.9(9) . . ? N22 C21 Se2 123.9(8) . . ? N21 C21 Se2 129.2(8) . . ? C23 C22 N21 108.2(10) . . ? C22 C23 N22 106.8(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.799 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.165 # Attachment 'SEZNS10.CIF' data_sezns10 _database_code_depnum_ccdc_archive 'CCDC 627370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B2 I2 N8 Se4 Zn2' _chemical_formula_weight 1050.43 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7612(4) _cell_length_b 8.8013(5) _cell_length_c 11.9260(7) _cell_angle_alpha 70.8520(10) _cell_angle_beta 78.2670(10) _cell_angle_gamma 70.8540(10) _cell_volume 722.81(7) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 2338 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.59 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 8.853 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.4714 _exptl_absorpt_correction_T_max 0.4714 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4843 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2922 _reflns_number_gt 2353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0230P)^2^+1.1462P] 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 2922 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 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 Zn Zn 0.09372(8) 0.07088(7) 0.33790(5) 0.03444(16) Uani 1 1 d . . . I I 0.03410(4) 0.37688(4) 0.21436(3) 0.03946(12) Uani 1 1 d . . . B B 0.5067(7) -0.0789(7) 0.2639(5) 0.0292(13) Uani 1 1 d . . . H1 H 0.384(6) 0.039(5) 0.266(4) 0.022(12) Uiso 1 1 d . . . H2 H 0.640(7) -0.038(7) 0.226(5) 0.050(16) Uiso 1 1 d . . . Se1 Se 0.08833(6) -0.13609(6) 0.24594(5) 0.02900(13) Uani 1 1 d . . . Se2 Se 0.23325(6) -0.01464(6) 0.52402(4) 0.02551(12) Uani 1 1 d . . . N11 N 0.4760(5) -0.1574(5) 0.1728(3) 0.0270(9) Uani 1 1 d . . . N12 N 0.3498(5) -0.2285(5) 0.0567(4) 0.0315(10) Uani 1 1 d . . . N21 N 0.5264(5) -0.2082(5) 0.3893(3) 0.0243(8) Uani 1 1 d . . . N22 N 0.5185(5) -0.3246(5) 0.5820(4) 0.0274(9) Uani 1 1 d . . . C11 C 0.3178(6) -0.1731(6) 0.1533(4) 0.0248(10) Uani 1 1 d . . . C12 C 0.6074(6) -0.2055(6) 0.0844(5) 0.0345(12) Uani 1 1 d . . . H12A H 0.7311 -0.2074 0.0757 0.041 Uiso 1 1 calc R . . C13 C 0.5319(7) -0.2487(6) 0.0136(5) 0.0363(12) Uani 1 1 d . . . H13A H 0.5916 -0.2861 -0.0534 0.044 Uiso 1 1 calc R . . C14 C 0.2129(7) -0.2512(7) 0.0005(5) 0.0411(13) Uani 1 1 d . . . H14A H 0.0953 -0.2312 0.0485 0.062 Uiso 1 1 calc R . . H14B H 0.2504 -0.3649 -0.0059 0.062 Uiso 1 1 calc R . . H14C H 0.2021 -0.1727 -0.0786 0.062 Uiso 1 1 calc R . . C21 C 0.4354(5) -0.1943(5) 0.4951(4) 0.0208(9) Uani 1 1 d . . . C22 C 0.6726(6) -0.3520(6) 0.4120(5) 0.0339(12) Uani 1 1 d . . . H22A H 0.7609 -0.3924 0.3539 0.041 Uiso 1 1 calc R . . C23 C 0.6677(7) -0.4240(6) 0.5299(5) 0.0347(12) Uani 1 1 d . . . H23A H 0.7503 -0.5233 0.5695 0.042 Uiso 1 1 calc R . . C24 C 0.4686(7) -0.3524(7) 0.7101(5) 0.0368(13) Uani 1 1 d . . . H24A H 0.3586 -0.2658 0.7247 0.055 Uiso 1 1 calc R . . H24B H 0.5681 -0.3487 0.7461 0.055 Uiso 1 1 calc R . . H24C H 0.4460 -0.4613 0.7449 0.055 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 Zn 0.0468(3) 0.0238(3) 0.0306(4) -0.0072(3) -0.0114(3) -0.0034(3) I 0.02963(17) 0.02449(18) 0.0505(2) -0.00174(16) 0.00222(15) -0.00259(13) B 0.021(2) 0.037(3) 0.028(3) -0.010(3) 0.000(2) -0.006(2) Se1 0.0240(2) 0.0332(3) 0.0315(3) -0.0149(2) 0.0018(2) -0.0076(2) Se2 0.0204(2) 0.0301(3) 0.0247(3) -0.0101(2) 0.00010(19) -0.00455(19) N11 0.027(2) 0.028(2) 0.018(2) -0.0055(17) -0.0014(17) -0.0001(17) N12 0.038(2) 0.031(2) 0.020(2) -0.0078(18) -0.0002(18) -0.0047(19) N21 0.0228(18) 0.025(2) 0.024(2) -0.0088(17) -0.0056(17) -0.0025(16) N22 0.027(2) 0.026(2) 0.026(2) -0.0044(18) -0.0027(17) -0.0070(17) C11 0.026(2) 0.026(3) 0.019(3) -0.004(2) -0.0020(19) -0.0045(19) C12 0.024(2) 0.038(3) 0.032(3) -0.012(2) 0.008(2) -0.001(2) C13 0.039(3) 0.039(3) 0.023(3) -0.014(2) 0.005(2) -0.001(2) C14 0.051(3) 0.049(3) 0.031(3) -0.017(3) 0.001(3) -0.021(3) C21 0.018(2) 0.021(2) 0.025(3) -0.008(2) -0.0036(19) -0.0069(17) C22 0.028(2) 0.031(3) 0.039(3) -0.016(2) -0.006(2) 0.003(2) C23 0.032(3) 0.026(3) 0.041(3) -0.008(2) -0.010(2) 0.001(2) C24 0.030(3) 0.043(3) 0.031(3) -0.001(2) -0.006(2) -0.008(2) _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 Zn Se1 2.4294(8) . ? Zn Se2 2.4522(8) . ? Zn I 2.5485(7) . ? Zn Se2 2.8260(8) 2_556 ? B H2 1.16(5) . ? B H1 1.16(4) . ? B N21 1.554(7) . ? B N11 1.556(7) . ? Se1 C11 1.885(4) . ? Se2 C21 1.895(4) . ? Se2 Zn 2.8260(8) 2_556 ? N11 C11 1.352(6) . ? N11 C12 1.379(6) . ? N12 C11 1.341(6) . ? N12 C13 1.376(6) . ? N12 C14 1.462(7) . ? N21 C21 1.337(6) . ? N21 C22 1.386(6) . ? N22 C21 1.346(6) . ? N22 C23 1.375(6) . ? N22 C24 1.457(6) . ? C12 C13 1.326(7) . ? C22 C23 1.338(7) . ? 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 Se1 Zn Se2 120.92(3) . . ? Se1 Zn I 119.03(3) . . ? Se2 Zn I 118.03(3) . . ? Se1 Zn Se2 86.07(2) . 2_556 ? Se2 Zn Se2 88.51(2) . 2_556 ? I Zn Se2 109.90(2) . 2_556 ? H2 B H1 109(3) . . ? H2 B N21 111(3) . . ? H1 B N21 112(2) . . ? H2 B N11 106(3) . . ? H1 B N11 108(2) . . ? N21 B N11 110.8(4) . . ? C11 Se1 Zn 103.37(14) . . ? C21 Se2 Zn 99.16(14) . . ? C21 Se2 Zn 121.52(13) . 2_556 ? Zn Se2 Zn 91.49(2) . 2_556 ? C11 N11 C12 106.5(4) . . ? C11 N11 B 128.6(4) . . ? C12 N11 B 124.4(4) . . ? C11 N12 C13 108.4(4) . . ? C11 N12 C14 126.2(4) . . ? C13 N12 C14 125.2(4) . . ? C21 N21 C22 106.8(4) . . ? C21 N21 B 129.5(4) . . ? C22 N21 B 122.7(4) . . ? C21 N22 C23 108.4(4) . . ? C21 N22 C24 126.6(4) . . ? C23 N22 C24 124.9(4) . . ? N12 C11 N11 108.7(4) . . ? N12 C11 Se1 123.3(3) . . ? N11 C11 Se1 128.0(3) . . ? C13 C12 N11 109.4(4) . . ? C12 C13 N12 107.1(4) . . ? N21 C21 N22 109.0(4) . . ? N21 C21 Se2 127.0(3) . . ? N22 C21 Se2 123.8(3) . . ? C23 C22 N21 108.9(4) . . ? C22 C23 N22 106.8(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.563 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.125