data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Paul Ragogna' _publ_contact_author_address ; Department of Chemistry The University of Western Ontario The University of Western Ontario 1151 Richmond St. London Ontario N6A 5B7 CANADA ; _publ_contact_author_email PRAGOGNA@UWO.CA _publ_section_title ; Synthesis and characterization of cationic selenium-nitrogen heterocycles from tert-butyl-DAB (DAB = 1,4-di-tert-butyl-1,3-diazabutadiene) and SeX4 via the reductive elimination of X2 (X = Cl, Br): A distinct contrast with tellurium. ; loop_ _publ_author_name 'Paul Ragogna' 'Jason L. Dutton' 'Robert Schurko' 'Andre Sutrisno' data_06113 _database_code_depnum_ccdc_archive 'CCDC 625895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Br4 N2 Te' _chemical_formula_sum 'C10 H20 Br4 N2 Te' _chemical_formula_weight 615.52 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.5284(10) _cell_length_b 18.4929(12) _cell_length_c 6.9942(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1749.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11562 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 10.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2937 _exptl_absorpt_correction_T_max 0.4975 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8891 _diffrn_reflns_av_R_equivalents 0.148 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1576 _reflns_number_gt 1046 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1140P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1576 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1919 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Te1 Te -0.00737(9) 0.2500 0.03925(18) 0.0268(4) Uani 1 2 d S . . Br1 Br -0.10421(11) 0.34934(7) -0.1572(2) 0.0370(5) Uani 1 1 d . . . Br2 Br 0.14933(16) 0.2500 -0.1903(3) 0.0408(6) Uani 1 2 d S . . Br3 Br -0.13099(15) 0.2500 0.3358(3) 0.0374(6) Uani 1 2 d S . . N1 N 0.0974(7) 0.3271(5) 0.2434(15) 0.022(2) Uani 1 1 d . . . C1 C 0.1552(9) 0.2890(7) 0.3468(17) 0.029(3) Uani 1 1 d . . . H1A H 0.2007 0.3133 0.4281 0.035 Uiso 1 1 calc R . . C13 C 0.0980(11) 0.4065(7) 0.247(2) 0.042(4) Uani 1 1 d . . . C14 C -0.0069(9) 0.4313(7) 0.296(2) 0.037(4) Uani 1 1 d . . . H14A H -0.0536 0.4106 0.2035 0.055 Uiso 1 1 calc R . . H14B H -0.0103 0.4842 0.2898 0.055 Uiso 1 1 calc R . . H14C H -0.0240 0.4150 0.4248 0.055 Uiso 1 1 calc R . . C15 C 0.1297(10) 0.4302(8) 0.045(2) 0.043(4) Uani 1 1 d . . . H15A H 0.1978 0.4145 0.0218 0.064 Uiso 1 1 calc R . . H15B H 0.1257 0.4830 0.0357 0.064 Uiso 1 1 calc R . . H15C H 0.0857 0.4082 -0.0495 0.064 Uiso 1 1 calc R . . C16 C 0.1703(11) 0.4363(8) 0.395(2) 0.052(5) Uani 1 1 d . . . H16A H 0.1539 0.4168 0.5213 0.078 Uiso 1 1 calc R . . H16B H 0.1656 0.4892 0.3981 0.078 Uiso 1 1 calc R . . H16C H 0.2378 0.4221 0.3606 0.078 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 Te1 0.0252(8) 0.0262(7) 0.0290(7) 0.000 -0.0002(5) 0.000 Br1 0.0414(10) 0.0313(9) 0.0383(9) 0.0023(6) -0.0076(7) 0.0036(6) Br2 0.0383(13) 0.0446(13) 0.0394(12) 0.000 0.0099(10) 0.000 Br3 0.0297(12) 0.0487(13) 0.0337(11) 0.000 0.0044(9) 0.000 N1 0.014(6) 0.023(5) 0.030(6) -0.005(5) 0.000(5) 0.000(4) C1 0.026(8) 0.037(7) 0.026(7) -0.007(6) -0.009(6) -0.014(6) C13 0.046(10) 0.024(8) 0.058(10) 0.002(7) -0.008(8) -0.009(7) C14 0.031(8) 0.030(7) 0.050(9) -0.007(7) -0.014(7) 0.008(6) C15 0.036(9) 0.031(8) 0.062(10) 0.011(8) 0.000(8) -0.004(6) C16 0.045(10) 0.027(8) 0.084(12) -0.004(9) -0.025(10) 0.000(7) _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 Te1 N1 2.466(10) . ? Te1 N1 2.466(10) 7_565 ? Te1 Br1 2.6419(16) . ? Te1 Br1 2.6419(16) 7_565 ? Te1 Br2 2.659(2) . ? Te1 Br3 2.664(2) . ? N1 C1 1.279(15) . ? N1 C13 1.468(17) . ? C1 C1 1.44(3) 7_565 ? C1 H1A 0.9500 . ? C13 C16 1.529(19) . ? C13 C14 1.530(18) . ? C13 C15 1.54(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 Te1 N1 70.7(5) . 7_565 ? N1 Te1 Br1 100.6(2) . . ? N1 Te1 Br1 171.2(2) 7_565 . ? N1 Te1 Br1 171.2(2) . 7_565 ? N1 Te1 Br1 100.6(2) 7_565 7_565 ? Br1 Te1 Br1 88.11(7) . 7_565 ? N1 Te1 Br2 83.8(2) . . ? N1 Te1 Br2 83.8(2) 7_565 . ? Br1 Te1 Br2 94.66(6) . . ? Br1 Te1 Br2 94.66(6) 7_565 . ? N1 Te1 Br3 84.8(2) . . ? N1 Te1 Br3 84.8(2) 7_565 . ? Br1 Te1 Br3 95.37(6) . . ? Br1 Te1 Br3 95.37(6) 7_565 . ? Br2 Te1 Br3 166.02(8) . . ? C1 N1 C13 122.6(11) . . ? C1 N1 Te1 111.1(8) . . ? C13 N1 Te1 126.2(8) . . ? N1 C1 C1 123.5(7) . 7_565 ? N1 C1 H1A 118.3 . . ? C1 C1 H1A 118.3 7_565 . ? N1 C13 C16 112.0(11) . . ? N1 C13 C14 107.3(11) . . ? C16 C13 C14 109.5(13) . . ? N1 C13 C15 105.8(12) . . ? C16 C13 C15 109.9(12) . . ? C14 C13 C15 112.2(13) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 Te1 N1 C1 2.2(9) 7_565 . . . ? Br2 Te1 N1 C1 -83.4(8) . . . . ? Br3 Te1 N1 C1 88.5(8) . . . . ? N1 Te1 N1 C13 -179.5(9) 7_565 . . . ? Br2 Te1 N1 C13 95.0(10) . . . . ? Br3 Te1 N1 C13 -93.2(10) . . . . ? C13 N1 C1 C1 179.5(9) . . . 7_565 ? Te1 N1 C1 C1 -2.2(9) . . . 7_565 ? C1 N1 C13 C16 -3.4(19) . . . . ? Te1 N1 C13 C16 178.4(9) . . . . ? C1 N1 C13 C14 -123.7(13) . . . . ? Te1 N1 C13 C14 58.2(14) . . . . ? C1 N1 C13 C15 116.3(13) . . . . ? Te1 N1 C13 C15 -61.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.879 _refine_diff_density_min -1.606 _refine_diff_density_rms 0.313 data_06095 _database_code_depnum_ccdc_archive 'CCDC 673832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H11 Br N2 Se' _chemical_formula_weight 270.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 '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)/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 9.7366(19) _cell_length_b 9.3214(19) _cell_length_c 10.070(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.47(3) _cell_angle_gamma 90.00 _cell_volume 885.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2112 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 8.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2754 _exptl_absorpt_correction_T_max 0.3556 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3767 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2022 _reflns_number_gt 1600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0721P)^2^+0.4337P] 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 2022 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Br1 Br -0.21127(6) -0.00832(6) 0.36769(6) 0.0238(2) Uani 1 1 d . . . Se1 Se 0.02672(6) 0.03694(7) 0.26732(5) 0.0194(2) Uani 1 1 d . . . N1 N -0.0881(5) 0.1346(5) 0.1284(5) 0.0233(10) Uani 1 1 d . . . C1 C -0.0199(6) 0.1841(6) 0.0434(6) 0.0228(12) Uani 1 1 d . . . H1A H -0.0669 0.2400 -0.0334 0.027 Uiso 1 1 calc R . . C2 C 0.1267(6) 0.1531(6) 0.0674(5) 0.0207(12) Uani 1 1 d . . . H2A H 0.1831 0.1846 0.0085 0.025 Uiso 1 1 calc R . . N2 N 0.1767(5) 0.0783(5) 0.1765(4) 0.0179(10) Uani 1 1 d . . . C3 C 0.3283(6) 0.0367(6) 0.2319(5) 0.0201(12) Uani 1 1 d . . . C6 C 0.3329(6) -0.1135(7) 0.2925(6) 0.0278(13) Uani 1 1 d . . . H6A H 0.2808 -0.1143 0.3641 0.042 Uiso 1 1 calc R . . H6B H 0.4318 -0.1411 0.3322 0.042 Uiso 1 1 calc R . . H6C H 0.2892 -0.1815 0.2201 0.042 Uiso 1 1 calc R . . C5 C 0.3927(6) 0.1446(6) 0.3436(6) 0.0235(12) Uani 1 1 d . . . H5A H 0.3740 0.2421 0.3073 0.035 Uiso 1 1 calc R . . H5B H 0.4953 0.1290 0.3741 0.035 Uiso 1 1 calc R . . H5C H 0.3501 0.1320 0.4214 0.035 Uiso 1 1 calc R . . C4 C 0.4068(6) 0.0387(8) 0.1181(6) 0.0310(15) Uani 1 1 d . . . H4A H 0.3552 -0.0202 0.0411 0.047 Uiso 1 1 calc R . . H4B H 0.5026 0.0000 0.1534 0.047 Uiso 1 1 calc R . . H4C H 0.4129 0.1375 0.0870 0.047 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 Br1 0.0193(3) 0.0239(4) 0.0296(4) 0.0013(2) 0.0090(3) -0.0008(2) Se1 0.0175(3) 0.0213(4) 0.0201(3) 0.0008(2) 0.0060(2) 0.0022(2) N1 0.022(2) 0.021(3) 0.027(3) -0.004(2) 0.007(2) 0.002(2) C1 0.025(3) 0.019(3) 0.022(3) 0.003(2) 0.002(2) 0.003(2) C2 0.025(3) 0.015(3) 0.023(3) -0.002(2) 0.006(2) 0.001(2) N2 0.019(2) 0.017(2) 0.020(2) 0.0014(19) 0.0097(18) -0.0002(19) C3 0.016(3) 0.029(3) 0.016(3) 0.003(2) 0.004(2) 0.003(2) C6 0.028(3) 0.021(3) 0.035(3) 0.003(3) 0.009(3) 0.004(3) C5 0.025(3) 0.018(3) 0.028(3) 0.001(2) 0.008(2) 0.001(2) C4 0.028(3) 0.043(4) 0.025(3) 0.000(3) 0.013(3) 0.000(3) _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 Br1 Se1 2.7820(10) . ? Se1 N1 1.804(5) . ? Se1 N2 1.945(4) . ? N1 C1 1.293(7) . ? C1 C2 1.417(7) . ? C1 H1A 0.9500 . ? C2 N2 1.289(7) . ? C2 H2A 0.9500 . ? N2 C3 1.493(7) . ? C3 C5 1.522(8) . ? C3 C6 1.523(8) . ? C3 C4 1.528(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 Se1 N2 85.9(2) . . ? N1 Se1 Br1 86.97(15) . . ? N2 Se1 Br1 172.76(13) . . ? C1 N1 Se1 111.8(4) . . ? N1 C1 C2 118.5(5) . . ? N1 C1 H1A 120.8 . . ? C2 C1 H1A 120.8 . . ? N2 C2 C1 113.9(5) . . ? N2 C2 H2A 123.0 . . ? C1 C2 H2A 123.0 . . ? C2 N2 C3 125.9(4) . . ? C2 N2 Se1 109.9(4) . . ? C3 N2 Se1 124.1(3) . . ? N2 C3 C5 106.9(4) . . ? N2 C3 C6 108.4(4) . . ? C5 C3 C6 110.2(4) . . ? N2 C3 C4 110.5(4) . . ? C5 C3 C4 110.8(5) . . ? C6 C3 C4 109.9(5) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 Se1 N1 C1 -1.3(4) . . . . ? Br1 Se1 N1 C1 179.8(4) . . . . ? Se1 N1 C1 C2 1.7(7) . . . . ? N1 C1 C2 N2 -1.0(8) . . . . ? C1 C2 N2 C3 -176.3(5) . . . . ? C1 C2 N2 Se1 -0.1(6) . . . . ? N1 Se1 N2 C2 0.8(4) . . . . ? Br1 Se1 N2 C2 9.7(14) . . . . ? N1 Se1 N2 C3 177.0(4) . . . . ? Br1 Se1 N2 C3 -174.1(9) . . . . ? C2 N2 C3 C5 97.4(6) . . . . ? Se1 N2 C3 C5 -78.3(5) . . . . ? C2 N2 C3 C6 -143.8(5) . . . . ? Se1 N2 C3 C6 40.6(6) . . . . ? C2 N2 C3 C4 -23.3(8) . . . . ? Se1 N2 C3 C4 161.1(4) . . . . ? _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 1.146 _refine_diff_density_min -1.235 _refine_diff_density_rms .224 data_7076 _database_code_depnum_ccdc_archive 'CCDC 673833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H11 Cl N2 Se' _chemical_formula_weight 225.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.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)/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 8.2290(16) _cell_length_b 10.646(2) _cell_length_c 10.347(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.74(3) _cell_angle_gamma 90.00 _cell_volume 858.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 4.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6554 _exptl_absorpt_correction_T_max 0.8021 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7234 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.65 _reflns_number_total 1999 _reflns_number_gt 1828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0617P)^2^+0.1815P] 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 1999 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 Se1 Se 0.25521(3) 0.44779(2) 0.83749(2) 0.01786(13) Uani 1 1 d . . . Cl1 Cl 0.29908(8) 0.26009(6) 1.01263(6) 0.02356(17) Uani 1 1 d . . . N2 N 0.0659(3) 0.4827(2) 0.8813(2) 0.0224(5) Uani 1 1 d . . . N1 N 0.1977(3) 0.5927(2) 0.7203(2) 0.0167(4) Uani 1 1 d . . . C4 C 0.4641(4) 0.5638(2) 0.6668(3) 0.0223(6) Uani 1 1 d . . . H4A H 0.4411 0.4736 0.6543 0.033 Uiso 1 1 calc R . . H4B H 0.5290 0.5807 0.7627 0.033 Uiso 1 1 calc R . . H4C H 0.5311 0.5912 0.6089 0.033 Uiso 1 1 calc R . . C3 C 0.2954(3) 0.6351(2) 0.6276(2) 0.0175(5) Uani 1 1 d . . . C2 C 0.0596(3) 0.6460(2) 0.7283(3) 0.0209(5) Uani 1 1 d . . . H2B H 0.0108 0.7193 0.6785 0.025 Uiso 1 1 calc R . . C1 C -0.0118(3) 0.5832(3) 0.8196(3) 0.0235(5) Uani 1 1 d . . . H1A H -0.1127 0.6137 0.8348 0.028 Uiso 1 1 calc R . . C6 C 0.1849(4) 0.6031(3) 0.4826(3) 0.0262(6) Uani 1 1 d . . . H6A H 0.1674 0.5120 0.4742 0.039 Uiso 1 1 calc R . . H6B H 0.2426 0.6313 0.4183 0.039 Uiso 1 1 calc R . . H6C H 0.0736 0.6453 0.4618 0.039 Uiso 1 1 calc R . . C5 C 0.3263(4) 0.7763(2) 0.6459(3) 0.0256(6) Uani 1 1 d . . . H5A H 0.3969 0.7938 0.7402 0.038 Uiso 1 1 calc R . . H5B H 0.2160 0.8198 0.6258 0.038 Uiso 1 1 calc R . . H5C H 0.3858 0.8058 0.5834 0.038 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 Se1 0.01657(19) 0.01911(18) 0.01906(18) 0.00126(8) 0.00734(13) 0.00084(8) Cl1 0.0255(3) 0.0228(3) 0.0222(3) 0.0037(2) 0.0075(3) 0.0023(2) N2 0.0201(11) 0.0278(11) 0.0217(11) -0.0012(10) 0.0102(9) 0.0001(9) N1 0.0157(10) 0.0182(10) 0.0158(10) 0.0005(8) 0.0047(8) -0.0018(8) C4 0.0212(13) 0.0219(12) 0.0263(14) 0.0023(10) 0.0111(11) 0.0007(10) C3 0.0184(12) 0.0185(12) 0.0172(11) 0.0003(9) 0.0077(10) -0.0023(9) C2 0.0187(12) 0.0234(12) 0.0198(12) -0.0028(10) 0.0049(10) 0.0020(10) C1 0.0196(12) 0.0280(13) 0.0247(13) -0.0032(11) 0.0097(11) 0.0025(11) C6 0.0256(14) 0.0325(15) 0.0194(12) 0.0006(11) 0.0055(11) -0.0015(12) C5 0.0255(14) 0.0168(12) 0.0353(15) 0.0009(11) 0.0108(12) -0.0015(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 Se1 N2 1.795(2) . ? Se1 N1 1.924(2) . ? Se1 Cl1 2.6432(8) . ? N2 C1 1.303(4) . ? N1 C2 1.297(3) . ? N1 C3 1.506(3) . ? C4 C3 1.519(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 C6 1.522(4) . ? C3 C5 1.526(3) . ? C2 C1 1.428(4) . ? C2 H2B 0.9500 . ? C1 H1A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 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 N2 Se1 N1 86.29(10) . . ? N2 Se1 Cl1 85.53(8) . . ? N1 Se1 Cl1 171.69(6) . . ? C1 N2 Se1 112.06(18) . . ? C2 N1 C3 124.6(2) . . ? C2 N1 Se1 110.71(17) . . ? C3 N1 Se1 124.66(16) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C3 C4 108.0(2) . . ? N1 C3 C6 106.8(2) . . ? C4 C3 C6 110.9(2) . . ? N1 C3 C5 108.6(2) . . ? C4 C3 C5 110.9(2) . . ? C6 C3 C5 111.5(2) . . ? N1 C2 C1 113.1(2) . . ? N1 C2 H2B 123.4 . . ? C1 C2 H2B 123.4 . . ? N2 C1 C2 117.8(2) . . ? N2 C1 H1A 121.1 . . ? C2 C1 H1A 121.1 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 . . ? 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 Se1 N2 C1 -1.2(2) . . . . ? Cl1 Se1 N2 C1 177.3(2) . . . . ? N2 Se1 N1 C2 0.89(18) . . . . ? Cl1 Se1 N1 C2 -9.4(6) . . . . ? N2 Se1 N1 C3 -176.7(2) . . . . ? Cl1 Se1 N1 C3 173.0(3) . . . . ? C2 N1 C3 C4 170.0(2) . . . . ? Se1 N1 C3 C4 -12.7(3) . . . . ? C2 N1 C3 C6 -70.6(3) . . . . ? Se1 N1 C3 C6 106.6(2) . . . . ? C2 N1 C3 C5 49.7(3) . . . . ? Se1 N1 C3 C5 -133.08(19) . . . . ? C3 N1 C2 C1 177.1(2) . . . . ? Se1 N1 C2 C1 -0.4(3) . . . . ? Se1 N2 C1 C2 1.3(3) . . . . ? N1 C2 C1 N2 -0.6(4) . . . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max 1.118 _refine_diff_density_min -1.353 _refine_diff_density_rms .150 data_7211 _database_code_depnum_ccdc_archive 'CCDC 673834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H11 I N2 Se' _chemical_formula_weight 317.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -.4742 1.8119 '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(2)1/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 10.251(2) _cell_length_b 9.6246(19) _cell_length_c 9.950(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.06(3) _cell_angle_gamma 90.00 _cell_volume 948.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8586 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 7.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3021 _exptl_absorpt_correction_T_max 0.4341 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6589 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.68 _reflns_number_total 2209 _reflns_number_gt 1932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0728P)^2^+1.2656P] 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 2209 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 I1 I 0.29111(4) 0.49034(3) 0.35329(4) 0.02727(15) Uani 1 1 d . . . Se1 Se 0.54054(5) 0.54200(5) 0.26037(5) 0.02173(16) Uani 1 1 d . . . N2 N 0.6857(4) 0.5772(4) 0.1700(4) 0.0212(8) Uani 1 1 d . . . N1 N 0.4324(4) 0.6374(4) 0.1165(4) 0.0252(9) Uani 1 1 d . . . C2 C 0.6384(5) 0.6489(5) 0.0572(5) 0.0245(10) Uani 1 1 d . . . H2A H 0.6925 0.6765 -0.0026 0.029 Uiso 1 1 calc R . . C1 C 0.4994(5) 0.6824(6) 0.0307(5) 0.0268(10) Uani 1 1 d . . . H1B H 0.4560 0.7365 -0.0480 0.032 Uiso 1 1 calc R . . C3 C 0.8299(5) 0.5308(6) 0.2279(5) 0.0227(10) Uani 1 1 d . . . C4 C 0.8948(5) 0.6331(6) 0.3431(5) 0.0285(11) Uani 1 1 d . . . H4A H 0.8480 0.6285 0.4173 0.043 Uiso 1 1 calc R . . H4B H 0.8879 0.7275 0.3050 0.043 Uiso 1 1 calc R . . H4C H 0.9902 0.6090 0.3811 0.043 Uiso 1 1 calc R . . C5 C 0.9009(6) 0.5334(8) 0.1096(6) 0.0402(15) Uani 1 1 d . . . H5A H 0.8572 0.4667 0.0375 0.060 Uiso 1 1 calc R . . H5B H 0.9961 0.5083 0.1464 0.060 Uiso 1 1 calc R . . H5C H 0.8945 0.6269 0.0693 0.060 Uiso 1 1 calc R . . C6 C 0.8283(6) 0.3853(6) 0.2843(6) 0.0357(12) Uani 1 1 d . . . H6A H 0.7870 0.3219 0.2080 0.054 Uiso 1 1 calc R . . H6B H 0.7759 0.3842 0.3538 0.054 Uiso 1 1 calc R . . H6C H 0.9211 0.3554 0.3278 0.054 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 I1 0.0260(2) 0.0259(2) 0.0301(2) 0.00341(12) 0.00764(16) 0.00001(12) Se1 0.0225(3) 0.0235(3) 0.0177(3) -0.00065(17) 0.00249(19) 0.00369(19) N2 0.0198(19) 0.020(2) 0.0209(18) -0.0039(16) 0.0003(15) 0.0005(16) N1 0.027(2) 0.021(2) 0.025(2) -0.0034(16) 0.0005(17) 0.0006(17) C2 0.030(3) 0.024(2) 0.020(2) 0.0026(18) 0.0062(19) -0.001(2) C1 0.030(3) 0.021(2) 0.025(2) 0.001(2) 0.001(2) -0.001(2) C3 0.019(2) 0.030(3) 0.018(2) -0.0033(19) 0.0033(18) 0.004(2) C4 0.024(2) 0.035(3) 0.025(2) -0.001(2) 0.0019(19) -0.004(2) C5 0.029(3) 0.069(4) 0.024(3) 0.003(3) 0.009(2) 0.012(3) C6 0.034(3) 0.027(3) 0.045(3) 0.002(2) 0.007(2) 0.006(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 I1 Se1 2.9781(9) . ? Se1 N1 1.816(4) . ? Se1 N2 1.958(4) . ? N2 C2 1.299(6) . ? N2 C3 1.508(6) . ? N1 C1 1.301(6) . ? C2 C1 1.418(7) . ? C2 H2A 0.9500 . ? C1 H1B 0.9500 . ? C3 C6 1.511(8) . ? C3 C4 1.527(7) . ? C3 C5 1.537(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 Se1 N2 86.07(18) . . ? N1 Se1 I1 86.08(14) . . ? N2 Se1 I1 171.06(11) . . ? C2 N2 C3 126.6(4) . . ? C2 N2 Se1 109.3(3) . . ? C3 N2 Se1 124.0(3) . . ? C1 N1 Se1 111.5(3) . . ? N2 C2 C1 114.4(4) . . ? N2 C2 H2A 122.8 . . ? C1 C2 H2A 122.8 . . ? N1 C1 C2 118.7(4) . . ? N1 C1 H1B 120.7 . . ? C2 C1 H1B 120.7 . . ? N2 C3 C6 108.2(4) . . ? N2 C3 C4 106.8(4) . . ? C6 C3 C4 111.3(4) . . ? N2 C3 C5 108.3(4) . . ? C6 C3 C5 110.7(5) . . ? C4 C3 C5 111.4(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 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 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 Se1 N2 C2 0.5(3) . . . . ? I1 Se1 N2 C2 29.1(10) . . . . ? N1 Se1 N2 C3 178.6(4) . . . . ? I1 Se1 N2 C3 -152.7(6) . . . . ? N2 Se1 N1 C1 -1.3(4) . . . . ? I1 Se1 N1 C1 -177.0(3) . . . . ? C3 N2 C2 C1 -177.7(4) . . . . ? Se1 N2 C2 C1 0.4(5) . . . . ? Se1 N1 C1 C2 1.9(6) . . . . ? N2 C2 C1 N1 -1.6(7) . . . . ? C2 N2 C3 C6 -140.6(5) . . . . ? Se1 N2 C3 C6 41.5(5) . . . . ? C2 N2 C3 C4 99.5(5) . . . . ? Se1 N2 C3 C4 -78.4(5) . . . . ? C2 N2 C3 C5 -20.6(7) . . . . ? Se1 N2 C3 C5 161.6(4) . . . . ? _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 1.187 _refine_diff_density_min -1.646 _refine_diff_density_rms .217 data_06085 _database_code_depnum_ccdc_archive 'CCDC 673835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H25 Br6 N5 Se3' _chemical_formula_weight 979.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 '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)/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 14.7569(8) _cell_length_b 10.7682(5) _cell_length_c 17.0874(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.392(3) _cell_angle_gamma 90.00 _cell_volume 2710.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6268 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description shoebox _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 12.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1020 _exptl_absorpt_correction_T_max 0.3580 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9149 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4788 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1380P)^2^+34.7508P] 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 4788 _refine_ls_number_parameters 253 _refine_ls_number_restraints 164 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2343 _refine_ls_wR_factor_gt 0.2136 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.019 _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 Se1 Se 0.90875(10) 0.63347(13) 0.47959(8) 0.0276(4) Uani 1 1 d U . . N1 N 0.8841(8) 0.5006(11) 0.4195(7) 0.030(3) Uani 1 1 d U . . C1 C 0.9384(10) 0.4955(14) 0.3633(8) 0.031(3) Uani 1 1 d U . . H1B H 0.9356 0.4278 0.3276 0.037 Uiso 1 1 calc R . . C2 C 1.0026(10) 0.5926(14) 0.3551(8) 0.030(3) Uani 1 1 d U . . H2A H 1.0425 0.5982 0.3136 0.036 Uiso 1 1 calc R . . N2 N 0.9995(8) 0.6740(10) 0.4129(6) 0.026(2) Uani 1 1 d U . . C3 C 1.0563(11) 0.7912(14) 0.4214(8) 0.031(3) Uani 1 1 d U . . C6 C 1.0215(12) 0.8824(14) 0.3609(10) 0.044(4) Uani 1 1 d U . . H6A H 1.0575 0.9588 0.3655 0.066 Uiso 1 1 calc R . . H6B H 0.9578 0.9014 0.3690 0.066 Uiso 1 1 calc R . . H6C H 1.0263 0.8468 0.3085 0.066 Uiso 1 1 calc R . . C5 C 1.1542(11) 0.7575(14) 0.4133(11) 0.039(4) Uani 1 1 d U . . H5A H 1.1917 0.8325 0.4186 0.059 Uiso 1 1 calc R . . H5B H 1.1611 0.7201 0.3617 0.059 Uiso 1 1 calc R . . H5C H 1.1736 0.6980 0.4543 0.059 Uiso 1 1 calc R . . C4 C 1.0454(13) 0.8378(16) 0.5034(9) 0.049(4) Uani 1 1 d U . . H4A H 1.0809 0.9140 0.5121 0.074 Uiso 1 1 calc R . . H4B H 1.0669 0.7745 0.5413 0.074 Uiso 1 1 calc R . . H4C H 0.9812 0.8554 0.5103 0.074 Uiso 1 1 calc R . . Se2 Se 0.52529(11) 0.50894(15) 0.62623(10) 0.0381(4) Uani 1 1 d U . . N3 N 0.4115(8) 0.5634(12) 0.6104(7) 0.032(3) Uani 1 1 d U . . C8 C 0.3560(10) 0.4714(15) 0.5929(8) 0.032(3) Uani 1 1 d U . . H8A H 0.2933 0.4856 0.5806 0.038 Uiso 1 1 calc R . . C9 C 0.3930(10) 0.3489(15) 0.5930(9) 0.035(3) Uani 1 1 d U . . H9A H 0.3580 0.2760 0.5829 0.042 Uiso 1 1 calc R . . N4 N 0.4800(8) 0.3487(12) 0.6086(7) 0.032(3) Uani 1 1 d U . . C10 C 0.5411(11) 0.2361(15) 0.6150(10) 0.037(3) Uani 1 1 d U . . C13 C 0.4858(15) 0.1256(19) 0.6248(17) 0.080(7) Uani 1 1 d U . . H13A H 0.4465 0.1122 0.5773 0.120 Uiso 1 1 calc R . . H13B H 0.4483 0.1370 0.6697 0.120 Uiso 1 1 calc R . . H13C H 0.5254 0.0534 0.6339 0.120 Uiso 1 1 calc R . . C12 C 0.6037(14) 0.260(2) 0.6882(12) 0.064(6) Uani 1 1 d U . . H12A H 0.6458 0.1905 0.6964 0.096 Uiso 1 1 calc R . . H12B H 0.5671 0.2689 0.7339 0.096 Uiso 1 1 calc R . . H12C H 0.6381 0.3368 0.6810 0.096 Uiso 1 1 calc R . . C11 C 0.5953(13) 0.2334(15) 0.5440(10) 0.045(4) Uani 1 1 d U . . H11A H 0.5549 0.2180 0.4975 0.067 Uiso 1 1 calc R . . H11B H 0.6408 0.1671 0.5495 0.067 Uiso 1 1 calc R . . H11C H 0.6259 0.3135 0.5385 0.067 Uiso 1 1 calc R . . Se3 Se 0.75464(9) 0.77645(13) 0.66184(8) 0.0250(4) Uani 1 1 d U . . Br1 Br 0.92199(10) 0.77643(15) 0.67382(8) 0.0311(4) Uani 1 1 d U . . Br2 Br 0.57398(11) 0.77459(16) 0.64784(12) 0.0446(5) Uani 1 1 d U . . Br3 Br 0.75999(11) 0.55620(14) 0.58913(9) 0.0364(4) Uani 1 1 d U . . Br4 Br 0.75772(11) 0.88880(14) 0.52474(8) 0.0341(4) Uani 1 1 d U . . Br5 Br 0.74873(11) 0.97978(14) 0.72619(9) 0.0350(4) Uani 1 1 d U . . Br6 Br 0.75256(12) 0.66903(17) 0.79176(10) 0.0456(5) Uani 1 1 d U . . N5 N 1.1520(13) 0.7998(19) 0.7067(11) 0.073(5) Uani 1 1 d U . . C14 C 1.2111(15) 0.8226(17) 0.6726(10) 0.050(4) Uani 1 1 d U . . C15 C 1.2904(15) 0.8512(19) 0.6311(10) 0.060(5) Uani 1 1 d U . . H15A H 1.2721 0.8751 0.5772 0.090 Uiso 1 1 calc R . . H15B H 1.3298 0.7779 0.6306 0.090 Uiso 1 1 calc R . . H15C H 1.3234 0.9199 0.6573 0.090 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 Se1 0.0275(8) 0.0261(8) 0.0296(8) -0.0027(6) 0.0046(6) -0.0038(6) N1 0.029(7) 0.022(6) 0.038(7) -0.002(5) 0.001(5) 0.004(5) C1 0.031(8) 0.033(7) 0.028(7) -0.007(6) -0.004(5) -0.001(6) C2 0.024(7) 0.037(7) 0.028(7) -0.008(5) -0.003(5) 0.005(6) N2 0.032(6) 0.021(5) 0.025(6) 0.003(4) 0.005(5) 0.004(4) C3 0.036(7) 0.033(7) 0.025(6) -0.001(5) 0.006(6) -0.009(5) C6 0.057(10) 0.026(8) 0.048(8) 0.005(6) -0.009(8) -0.015(7) C5 0.036(7) 0.027(8) 0.055(10) -0.009(7) 0.005(7) -0.014(6) C4 0.066(12) 0.044(10) 0.040(7) -0.009(6) 0.021(8) -0.031(9) Se2 0.0242(9) 0.0360(9) 0.0539(10) -0.0027(8) -0.0007(7) -0.0017(7) N3 0.026(6) 0.036(6) 0.032(7) 0.003(6) -0.002(5) 0.000(5) C8 0.021(6) 0.045(7) 0.029(7) 0.006(7) -0.002(6) -0.001(5) C9 0.028(6) 0.032(6) 0.045(9) 0.012(7) 0.000(7) -0.006(5) N4 0.028(6) 0.033(5) 0.037(7) -0.008(5) 0.011(5) -0.002(4) C10 0.024(8) 0.037(6) 0.049(8) -0.001(7) 0.003(6) 0.004(5) C13 0.055(13) 0.046(8) 0.14(2) 0.006(12) 0.027(12) -0.012(8) C12 0.055(12) 0.082(15) 0.053(9) -0.013(10) -0.007(8) 0.025(9) C11 0.055(11) 0.030(9) 0.051(8) 0.003(7) 0.011(7) 0.020(7) Se3 0.0210(8) 0.0254(7) 0.0289(8) 0.0009(6) 0.0044(6) -0.0002(6) Br1 0.0221(8) 0.0410(9) 0.0304(8) -0.0019(6) 0.0028(6) 0.0016(7) Br2 0.0211(9) 0.0375(9) 0.0753(13) -0.0067(8) 0.0027(8) -0.0031(7) Br3 0.0364(9) 0.0237(8) 0.0503(10) -0.0044(7) 0.0135(7) -0.0060(7) Br4 0.0434(10) 0.0275(8) 0.0309(8) 0.0052(6) -0.0022(7) -0.0035(7) Br5 0.0365(9) 0.0274(8) 0.0411(9) -0.0073(6) 0.0015(7) 0.0022(7) Br6 0.0523(11) 0.0456(10) 0.0410(9) 0.0185(8) 0.0197(8) 0.0136(8) N5 0.059(11) 0.088(13) 0.072(12) 0.012(11) -0.010(8) -0.032(11) C14 0.074(13) 0.041(10) 0.036(10) 0.001(8) 0.003(8) 0.002(10) C15 0.086(13) 0.059(12) 0.037(10) 0.007(9) 0.020(9) 0.030(11) _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 Se1 N1 1.786(12) . ? Se1 N2 1.861(12) . ? N1 C1 1.288(19) . ? C1 C2 1.42(2) . ? C1 H1B 0.9500 . ? C2 N2 1.324(18) . ? C2 H2A 0.9500 . ? N2 C3 1.517(19) . ? C3 C5 1.50(2) . ? C3 C6 1.49(2) . ? C3 C4 1.51(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Se2 N3 1.784(12) . ? Se2 N4 1.868(13) . ? N3 C8 1.308(19) . ? C8 C9 1.43(2) . ? C8 H8A 0.9500 . ? C9 N4 1.295(19) . ? C9 H9A 0.9500 . ? N4 C10 1.51(2) . ? C10 C13 1.46(2) . ? C10 C11 1.49(2) . ? C10 C12 1.53(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? Se3 Br5 2.454(2) . ? Se3 Br1 2.4660(19) . ? Se3 Br6 2.505(2) . ? Se3 Br4 2.639(2) . ? Se3 Br2 2.663(2) . ? Se3 Br3 2.681(2) . ? N5 C14 1.11(2) . ? C14 C15 1.44(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 Se1 N2 88.0(5) . . ? C1 N1 Se1 110.4(10) . . ? N1 C1 C2 119.3(13) . . ? N1 C1 H1B 120.4 . . ? C2 C1 H1B 120.4 . . ? N2 C2 C1 111.1(13) . . ? N2 C2 H2A 124.4 . . ? C1 C2 H2A 124.4 . . ? C2 N2 C3 125.3(12) . . ? C2 N2 Se1 111.1(10) . . ? C3 N2 Se1 123.4(9) . . ? C5 C3 C6 112.8(14) . . ? C5 C3 C4 108.8(14) . . ? C6 C3 C4 111.9(15) . . ? C5 C3 N2 108.6(12) . . ? C6 C3 N2 108.4(12) . . ? C4 C3 N2 106.0(12) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 Se2 N4 87.4(6) . . ? C8 N3 Se2 110.9(11) . . ? N3 C8 C9 117.7(13) . . ? N3 C8 H8A 121.1 . . ? C9 C8 H8A 121.1 . . ? N4 C9 C8 112.1(14) . . ? N4 C9 H9A 124.0 . . ? C8 C9 H9A 124.0 . . ? C9 N4 C10 126.5(13) . . ? C9 N4 Se2 111.9(11) . . ? C10 N4 Se2 121.6(10) . . ? C13 C10 C11 114.1(17) . . ? C13 C10 N4 109.1(14) . . ? C11 C10 N4 107.6(13) . . ? C13 C10 C12 111.1(18) . . ? C11 C10 C12 109.9(15) . . ? N4 C10 C12 104.5(13) . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Br5 Se3 Br1 91.42(7) . . ? Br5 Se3 Br6 90.70(7) . . ? Br1 Se3 Br6 89.49(7) . . ? Br5 Se3 Br4 89.52(7) . . ? Br1 Se3 Br4 90.23(7) . . ? Br6 Se3 Br4 179.64(9) . . ? Br5 Se3 Br2 89.14(7) . . ? Br1 Se3 Br2 179.41(8) . . ? Br6 Se3 Br2 90.66(7) . . ? Br4 Se3 Br2 89.63(7) . . ? Br5 Se3 Br3 178.98(8) . . ? Br1 Se3 Br3 88.94(7) . . ? Br6 Se3 Br3 90.25(7) . . ? Br4 Se3 Br3 89.52(6) . . ? Br2 Se3 Br3 90.49(7) . . ? N5 C14 C15 178(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 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 Se1 N1 C1 1.0(10) . . . . ? Se1 N1 C1 C2 -2.9(17) . . . . ? N1 C1 C2 N2 3.8(19) . . . . ? C1 C2 N2 C3 -177.9(13) . . . . ? C1 C2 N2 Se1 -2.6(14) . . . . ? N1 Se1 N2 C2 1.0(10) . . . . ? N1 Se1 N2 C3 176.4(11) . . . . ? C2 N2 C3 C5 -50.7(18) . . . . ? Se1 N2 C3 C5 134.4(11) . . . . ? C2 N2 C3 C6 72.2(18) . . . . ? Se1 N2 C3 C6 -102.6(13) . . . . ? C2 N2 C3 C4 -167.5(14) . . . . ? Se1 N2 C3 C4 17.7(17) . . . . ? N4 Se2 N3 C8 -1.9(10) . . . . ? Se2 N3 C8 C9 2.8(17) . . . . ? N3 C8 C9 N4 -2(2) . . . . ? C8 C9 N4 C10 178.8(13) . . . . ? C8 C9 N4 Se2 0.6(16) . . . . ? N3 Se2 N4 C9 0.7(11) . . . . ? N3 Se2 N4 C10 -177.6(12) . . . . ? C9 N4 C10 C13 -17(2) . . . . ? Se2 N4 C10 C13 160.9(14) . . . . ? C9 N4 C10 C11 107.2(18) . . . . ? Se2 N4 C10 C11 -74.8(15) . . . . ? C9 N4 C10 C12 -136.0(16) . . . . ? Se2 N4 C10 C12 42.0(17) . . . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max 5.495 _refine_diff_density_min -1.222 _refine_diff_density_rms .321 data_07107 _database_code_depnum_ccdc_archive 'CCDC 673836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H11 B F20 N2 Se' _chemical_formula_weight 869.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -.0929 2.2259 '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 9.910(2) _cell_length_b 17.185(3) _cell_length_c 19.626(4) _cell_angle_alpha 68.87(3) _cell_angle_beta 78.32(3) _cell_angle_gamma 81.81(3) _cell_volume 3044.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28373 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5444 _exptl_absorpt_correction_T_max 0.6283 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23198 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.94 _reflns_number_total 14014 _reflns_number_gt 10849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0396P)^2^+2.9074P] 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 14014 _refine_ls_number_parameters 979 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Se1 Se 0.42920(3) 0.101661(15) 0.001959(14) 0.02683(7) Uani 1 1 d . . . F74 F 0.10431(14) 0.34528(9) -0.09688(8) 0.0289(3) Uani 1 1 d . . . F78 F -0.30741(15) 0.44734(9) -0.19771(8) 0.0295(3) Uani 1 1 d . . . F72 F 0.29969(15) 0.34912(9) -0.23157(9) 0.0344(3) Uani 1 1 d . . . F80 F 0.18091(17) 0.28944(9) -0.32014(8) 0.0356(4) Uani 1 1 d . . . F76 F -0.25683(17) 0.48714(10) 0.01826(9) 0.0389(4) Uani 1 1 d . . . F77 F -0.40551(15) 0.50621(9) -0.08874(9) 0.0339(3) Uani 1 1 d . . . F66 F -0.25972(16) 0.26811(9) -0.16348(9) 0.0361(4) Uani 1 1 d . . . F68 F -0.09289(16) 0.52933(9) -0.30243(9) 0.0373(4) Uani 1 1 d . . . F75 F 0.00057(16) 0.40403(10) 0.01330(8) 0.0360(4) Uani 1 1 d . . . F81 F 0.31836(19) 0.13988(10) -0.28948(9) 0.0442(4) Uani 1 1 d . . . F84 F -0.05510(15) 0.21600(9) -0.07381(8) 0.0323(3) Uani 1 1 d . . . F70 F 0.3444(2) 0.63025(11) -0.36098(11) 0.0544(5) Uani 1 1 d . . . F82 F 0.2685(2) 0.02655(10) -0.15161(9) 0.0469(4) Uani 1 1 d . . . N2 N 0.5070(2) 0.19309(12) 0.00306(11) 0.0256(4) Uani 1 1 d . . . F83 F 0.07603(19) 0.06704(9) -0.04734(9) 0.0439(4) Uani 1 1 d . . . F69 F 0.0665(2) 0.65558(9) -0.36385(10) 0.0486(5) Uani 1 1 d . . . F62 F -0.0148(2) 0.42897(11) -0.39093(9) 0.0486(4) Uani 1 1 d . . . F71 F 0.45543(17) 0.47523(11) -0.29479(11) 0.0488(4) Uani 1 1 d . . . N1 N 0.5994(2) 0.05105(13) -0.00499(12) 0.0288(5) Uani 1 1 d . . . F65 F -0.43996(19) 0.24058(13) -0.23402(13) 0.0622(6) Uani 1 1 d . . . C67 C 0.0933(3) 0.43052(15) -0.26580(13) 0.0255(5) Uani 1 1 d . . . C73 C -0.0958(2) 0.38949(14) -0.15260(13) 0.0229(5) Uani 1 1 d . . . C2 C 0.6407(3) 0.17882(16) -0.00120(14) 0.0296(5) Uani 1 1 d . . . H32A H 0.6990 0.2182 -0.0013 0.036 Uiso 1 1 calc R . . C80 C 0.1543(3) 0.23713(15) -0.25035(14) 0.0272(5) Uani 1 1 d . . . C78 C -0.2248(3) 0.43272(14) -0.14684(13) 0.0242(5) Uani 1 1 d . . . C74 C -0.0257(2) 0.38269(14) -0.09629(14) 0.0246(5) Uani 1 1 d . . . C84 C 0.0385(3) 0.20254(15) -0.13058(14) 0.0263(5) Uani 1 1 d . . . F63 F -0.1991(3) 0.40347(17) -0.45975(12) 0.0792(7) Uani 1 1 d . . . C82 C 0.2023(3) 0.10289(15) -0.16711(15) 0.0315(6) Uani 1 1 d . . . B21 B -0.0178(3) 0.35849(17) -0.22315(15) 0.0248(6) Uani 1 1 d . . . C83 C 0.1058(3) 0.12421(15) -0.11435(14) 0.0301(6) Uani 1 1 d . . . C77 C -0.2795(3) 0.46463(15) -0.09038(14) 0.0258(5) Uani 1 1 d . . . C76 C -0.2048(3) 0.45508(15) -0.03599(14) 0.0270(5) Uani 1 1 d . . . C1 C 0.6912(3) 0.09872(15) -0.00568(15) 0.0301(6) Uani 1 1 d . . . H31B H 0.7868 0.0809 -0.0090 0.036 Uiso 1 1 calc R . . C62 C -0.1195(3) 0.38224(19) -0.34838(16) 0.0405(7) Uani 1 1 d . . . C33 C 0.4217(3) 0.27261(15) 0.00709(15) 0.0296(5) Uani 1 1 d . . . C72 C 0.2342(3) 0.42280(15) -0.26556(14) 0.0291(5) Uani 1 1 d . . . C81 C 0.2270(3) 0.16015(16) -0.23629(14) 0.0299(6) Uani 1 1 d . . . C79 C 0.0603(2) 0.26409(14) -0.19877(13) 0.0236(5) Uani 1 1 d . . . C75 C -0.0763(3) 0.41299(15) -0.03851(13) 0.0263(5) Uani 1 1 d . . . C68 C 0.0444(3) 0.51237(16) -0.30039(14) 0.0298(6) Uani 1 1 d . . . C66 C -0.2394(3) 0.30308(17) -0.23798(16) 0.0340(6) Uani 1 1 d . . . C70 C 0.2630(3) 0.56634(17) -0.33138(16) 0.0378(7) Uani 1 1 d . . . C61 C -0.1280(3) 0.35089(16) -0.27266(15) 0.0305(6) Uani 1 1 d . . . C71 C 0.3189(3) 0.48777(17) -0.29772(16) 0.0351(6) Uani 1 1 d . . . C69 C 0.1242(3) 0.57840(16) -0.33250(15) 0.0358(6) Uani 1 1 d . . . C36 C 0.2758(3) 0.24982(18) 0.04361(17) 0.0419(7) Uani 1 1 d . . . H36A H 0.2773 0.2091 0.0936 0.063 Uiso 1 1 calc R . . H36B H 0.2374 0.2254 0.0143 0.063 Uiso 1 1 calc R . . H36C H 0.2183 0.3002 0.0466 0.063 Uiso 1 1 calc R . . F64 F -0.4149(2) 0.30974(18) -0.38365(15) 0.0865(8) Uani 1 1 d . . . C35 C 0.4245(3) 0.33022(17) -0.07250(16) 0.0380(7) Uani 1 1 d . . . H35A H 0.3699 0.3828 -0.0736 0.057 Uiso 1 1 calc R . . H35B H 0.3854 0.3033 -0.0996 0.057 Uiso 1 1 calc R . . H35C H 0.5202 0.3419 -0.0958 0.057 Uiso 1 1 calc R . . C65 C -0.3351(3) 0.2882(2) -0.2732(2) 0.0454(8) Uani 1 1 d . . . C34 C 0.4866(4) 0.30931(19) 0.05183(19) 0.0481(8) Uani 1 1 d . . . H34A H 0.4306 0.3596 0.0562 0.072 Uiso 1 1 calc R . . H34B H 0.5803 0.3240 0.0267 0.072 Uiso 1 1 calc R . . H34C H 0.4907 0.2679 0.1013 0.072 Uiso 1 1 calc R . . C64 C -0.3226(4) 0.3219(2) -0.3478(2) 0.0569(10) Uani 1 1 d . . . C63 C -0.2145(4) 0.3692(2) -0.38550(19) 0.0552(9) Uani 1 1 d . . . Se22 Se 0.26282(3) 0.21121(2) 0.368306(17) 0.04426(9) Uani 1 1 d . . . N22 N 0.2946(2) 0.29584(15) 0.39889(13) 0.0351(5) Uani 1 1 d . . . C22 C 0.3293(3) 0.36049(18) 0.34079(16) 0.0380(6) Uani 1 1 d . . . H22A H 0.3523 0.4112 0.3432 0.046 Uiso 1 1 calc R . . N21 N 0.2978(3) 0.27619(17) 0.27618(14) 0.0427(6) Uani 1 1 d . . . C23 C 0.2701(3) 0.2904(2) 0.47910(16) 0.0442(7) Uani 1 1 d . . . C21 C 0.3293(3) 0.34750(19) 0.27369(17) 0.0417(7) Uani 1 1 d . . . H21A H 0.3522 0.3906 0.2275 0.050 Uiso 1 1 calc R . . C26 C 0.3109(4) 0.2002(2) 0.52229(18) 0.0590(10) Uani 1 1 d . . . H26A H 0.2517 0.1634 0.5156 0.089 Uiso 1 1 calc R . . H26B H 0.2999 0.1929 0.5750 0.089 Uiso 1 1 calc R . . H26C H 0.4076 0.1862 0.5042 0.089 Uiso 1 1 calc R . . C25 C 0.3575(4) 0.3507(2) 0.4891(2) 0.0547(9) Uani 1 1 d . . . H25A H 0.3464 0.3433 0.5418 0.082 Uiso 1 1 calc R . . H25B H 0.3272 0.4084 0.4614 0.082 Uiso 1 1 calc R . . H25C H 0.4549 0.3390 0.4705 0.082 Uiso 1 1 calc R . . C24 C 0.1161(4) 0.3132(3) 0.4992(2) 0.0664(11) Uani 1 1 d . . . H24A H 0.0620 0.2762 0.4893 0.100 Uiso 1 1 calc R . . H24B H 0.0932 0.3714 0.4695 0.100 Uiso 1 1 calc R . . H24C H 0.0944 0.3067 0.5519 0.100 Uiso 1 1 calc R . . F56 F 0.87147(16) 0.95173(9) 0.36268(8) 0.0310(3) Uani 1 1 d . . . F48 F 0.67799(15) 1.13983(9) 0.16329(7) 0.0302(3) Uani 1 1 d . . . F42 F 0.61630(15) 1.20074(9) 0.38108(8) 0.0323(3) Uani 1 1 d . . . F50 F 0.58077(15) 1.25936(9) 0.23102(9) 0.0337(3) Uani 1 1 d . . . F54 F 1.06117(15) 1.20925(9) 0.23756(9) 0.0339(3) Uani 1 1 d . . . F60 F 0.97842(16) 1.15883(9) 0.13093(8) 0.0342(3) Uani 1 1 d . . . F38 F 1.06374(15) 1.05984(9) 0.36503(8) 0.0318(3) Uani 1 1 d . . . F44 F 0.61664(17) 1.02432(10) 0.42337(8) 0.0349(4) Uani 1 1 d . . . F57 F 1.04311(18) 0.84121(9) 0.31251(9) 0.0402(4) Uani 1 1 d . . . F39 F 1.09079(17) 1.07700(10) 0.48934(8) 0.0383(4) Uani 1 1 d . . . F51 F 0.61029(17) 1.42024(9) 0.17206(9) 0.0411(4) Uani 1 1 d . . . F52 F 0.86246(18) 1.47966(9) 0.14121(9) 0.0406(4) Uani 1 1 d . . . F59 F 1.14862(17) 1.04855(11) 0.08382(9) 0.0425(4) Uani 1 1 d . . . F53 F 1.08869(17) 1.37229(10) 0.17186(10) 0.0436(4) Uani 1 1 d . . . F41 F 0.65092(19) 1.22056(11) 0.50486(9) 0.0447(4) Uani 1 1 d . . . F45 F 0.39128(18) 0.96114(11) 0.42245(9) 0.0475(4) Uani 1 1 d . . . F47 F 0.44914(17) 1.07509(11) 0.16450(9) 0.0419(4) Uani 1 1 d . . . F40 F 0.8851(2) 1.15732(11) 0.56224(9) 0.0495(5) Uani 1 1 d . . . F58 F 1.18869(18) 0.89004(11) 0.17276(10) 0.0448(4) Uani 1 1 d . . . F46 F 0.30355(18) 0.98299(12) 0.29348(10) 0.0489(4) Uani 1 1 d . . . C49 C 0.8198(3) 1.22438(14) 0.23709(13) 0.0233(5) Uani 1 1 d . . . C55 C 0.9203(2) 1.06241(15) 0.25181(13) 0.0235(5) Uani 1 1 d . . . C56 C 0.9413(3) 0.97907(15) 0.29341(13) 0.0255(5) Uani 1 1 d . . . C43 C 0.6596(2) 1.08870(14) 0.29304(13) 0.0230(5) Uani 1 1 d . . . C42 C 0.7366(3) 1.16840(15) 0.40587(13) 0.0262(5) Uani 1 1 d . . . C60 C 0.9925(3) 1.08168(15) 0.18043(14) 0.0258(5) Uani 1 1 d . . . C38 C 0.9547(3) 1.09873(14) 0.39738(13) 0.0261(5) Uani 1 1 d . . . C37 C 0.8359(3) 1.12713(14) 0.36629(13) 0.0236(5) Uani 1 1 d . . . C48 C 0.6083(2) 1.09679(15) 0.23005(13) 0.0244(5) Uani 1 1 d . . . C44 C 0.5803(3) 1.04089(15) 0.35700(13) 0.0257(5) Uani 1 1 d . . . B11 B 0.8086(3) 1.12480(16) 0.28682(15) 0.0229(5) Uani 1 1 d . . . C58 C 1.1013(3) 0.94476(17) 0.19859(15) 0.0316(6) Uani 1 1 d . . . C53 C 0.9630(3) 1.34293(16) 0.18767(14) 0.0305(6) Uani 1 1 d . . . C59 C 1.0813(3) 1.02526(17) 0.15437(14) 0.0299(6) Uani 1 1 d . . . C39 C 0.9722(3) 1.10798(16) 0.46217(14) 0.0300(6) Uani 1 1 d . . . C50 C 0.7106(3) 1.28247(15) 0.21778(14) 0.0265(5) Uani 1 1 d . . . C46 C 0.4167(3) 1.01720(17) 0.29388(16) 0.0329(6) Uani 1 1 d . . . C51 C 0.7229(3) 1.36728(15) 0.18622(14) 0.0300(6) Uani 1 1 d . . . C47 C 0.4912(3) 1.06363(16) 0.22887(14) 0.0291(5) Uani 1 1 d . . . C54 C 0.9460(3) 1.25934(15) 0.22040(14) 0.0273(5) Uani 1 1 d . . . C57 C 1.0289(3) 0.92086(15) 0.26894(15) 0.0296(5) Uani 1 1 d . . . C41 C 0.7518(3) 1.17994(16) 0.46980(14) 0.0327(6) Uani 1 1 d . . . C52 C 0.8496(3) 1.39768(15) 0.17081(14) 0.0310(6) Uani 1 1 d . . . C45 C 0.4615(3) 1.00628(16) 0.35821(14) 0.0313(6) Uani 1 1 d . . . C40 C 0.8700(3) 1.14833(16) 0.49938(14) 0.0334(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.02409(13) 0.02626(12) 0.03186(14) -0.01345(10) -0.00334(10) 0.00024(9) F74 0.0221(7) 0.0341(8) 0.0330(8) -0.0152(6) -0.0090(6) 0.0064(6) F78 0.0271(8) 0.0331(8) 0.0322(8) -0.0154(6) -0.0123(6) 0.0071(6) F72 0.0275(8) 0.0294(8) 0.0432(9) -0.0091(7) -0.0101(7) 0.0052(6) F80 0.0469(10) 0.0322(8) 0.0229(7) -0.0083(6) -0.0040(7) 0.0066(7) F76 0.0401(9) 0.0480(9) 0.0353(9) -0.0267(7) -0.0065(7) 0.0098(7) F77 0.0261(8) 0.0365(8) 0.0419(9) -0.0205(7) -0.0080(7) 0.0112(6) F66 0.0307(8) 0.0340(8) 0.0485(10) -0.0200(7) -0.0067(7) -0.0015(6) F68 0.0341(9) 0.0298(8) 0.0400(9) -0.0060(7) -0.0082(7) 0.0098(6) F75 0.0354(9) 0.0468(9) 0.0322(8) -0.0204(7) -0.0137(7) 0.0069(7) F81 0.0527(11) 0.0419(9) 0.0360(9) -0.0205(7) -0.0042(8) 0.0179(8) F84 0.0321(8) 0.0288(7) 0.0304(8) -0.0082(6) 0.0019(6) 0.0008(6) F70 0.0574(12) 0.0349(9) 0.0593(12) -0.0069(8) 0.0085(9) -0.0174(8) F82 0.0624(12) 0.0287(8) 0.0454(10) -0.0133(7) -0.0152(9) 0.0211(8) N2 0.0270(11) 0.0214(10) 0.0270(11) -0.0079(8) -0.0042(9) 0.0011(8) F83 0.0598(11) 0.0269(8) 0.0344(9) -0.0008(7) -0.0055(8) 0.0016(7) F69 0.0614(12) 0.0236(8) 0.0479(10) -0.0005(7) -0.0071(9) 0.0035(7) F62 0.0606(12) 0.0544(11) 0.0287(9) -0.0136(8) -0.0126(8) 0.0084(9) F71 0.0296(9) 0.0452(10) 0.0668(12) -0.0164(9) -0.0004(8) -0.0058(7) N1 0.0285(12) 0.0273(10) 0.0294(11) -0.0109(9) -0.0014(9) 0.0006(9) F65 0.0334(10) 0.0724(13) 0.1053(17) -0.0556(13) -0.0210(11) -0.0003(9) C67 0.0293(13) 0.0249(12) 0.0222(12) -0.0099(9) -0.0041(10) 0.0029(10) C73 0.0242(12) 0.0193(11) 0.0249(12) -0.0076(9) -0.0043(9) -0.0007(9) C2 0.0263(13) 0.0282(13) 0.0328(14) -0.0098(10) -0.0025(11) -0.0021(10) C80 0.0313(14) 0.0259(12) 0.0247(12) -0.0090(10) -0.0085(10) 0.0028(10) C78 0.0248(12) 0.0228(11) 0.0259(12) -0.0079(9) -0.0079(10) -0.0006(9) C74 0.0201(12) 0.0233(11) 0.0298(13) -0.0098(10) -0.0047(10) 0.0031(9) C84 0.0247(13) 0.0278(12) 0.0272(12) -0.0111(10) -0.0037(10) -0.0006(10) F63 0.0881(17) 0.1151(19) 0.0469(12) -0.0388(13) -0.0403(12) 0.0245(14) C82 0.0361(15) 0.0236(12) 0.0382(15) -0.0145(11) -0.0147(12) 0.0096(10) B21 0.0240(14) 0.0250(13) 0.0251(13) -0.0091(11) -0.0065(11) 0.0038(11) C83 0.0377(15) 0.0228(12) 0.0283(13) -0.0053(10) -0.0099(11) -0.0002(10) C77 0.0215(12) 0.0232(11) 0.0318(13) -0.0104(10) -0.0047(10) 0.0044(9) C76 0.0292(13) 0.0280(12) 0.0254(12) -0.0133(10) -0.0025(10) 0.0007(10) C1 0.0253(13) 0.0276(12) 0.0351(14) -0.0101(11) -0.0021(11) -0.0005(10) C62 0.0428(18) 0.0466(17) 0.0370(16) -0.0211(13) -0.0161(13) 0.0131(14) C33 0.0301(14) 0.0211(11) 0.0361(14) -0.0100(10) -0.0066(11) 0.0052(10) C72 0.0307(14) 0.0259(12) 0.0273(13) -0.0079(10) -0.0037(11) 0.0041(10) C81 0.0323(14) 0.0317(13) 0.0293(13) -0.0174(11) -0.0069(11) 0.0075(11) C79 0.0215(12) 0.0249(11) 0.0271(12) -0.0120(10) -0.0057(10) 0.0005(9) C75 0.0269(13) 0.0287(12) 0.0258(12) -0.0107(10) -0.0086(10) -0.0005(10) C68 0.0282(14) 0.0290(13) 0.0286(13) -0.0089(10) -0.0038(10) 0.0053(10) C66 0.0293(14) 0.0362(14) 0.0466(16) -0.0262(13) -0.0149(12) 0.0104(11) C70 0.0416(17) 0.0306(14) 0.0358(15) -0.0089(11) 0.0051(12) -0.0085(12) C61 0.0319(14) 0.0303(13) 0.0342(14) -0.0180(11) -0.0123(11) 0.0103(11) C71 0.0286(14) 0.0373(15) 0.0375(15) -0.0135(12) 0.0006(12) -0.0030(11) C69 0.0461(17) 0.0236(12) 0.0309(14) -0.0055(10) -0.0022(12) 0.0025(11) C36 0.0365(16) 0.0317(14) 0.0478(17) -0.0129(13) 0.0047(13) 0.0097(12) F64 0.0652(15) 0.131(2) 0.106(2) -0.0802(18) -0.0545(14) 0.0187(14) C35 0.0385(16) 0.0286(13) 0.0387(16) -0.0039(11) -0.0071(13) 0.0042(11) C65 0.0325(16) 0.0509(18) 0.071(2) -0.0418(17) -0.0202(15) 0.0110(13) C34 0.060(2) 0.0361(16) 0.059(2) -0.0284(15) -0.0229(17) 0.0130(14) C64 0.044(2) 0.078(2) 0.078(3) -0.056(2) -0.0383(19) 0.0228(18) C63 0.061(2) 0.073(2) 0.0458(19) -0.0359(18) -0.0316(17) 0.0251(19) Se22 0.04615(19) 0.04536(17) 0.04025(17) -0.01401(14) 0.00258(14) -0.01578(14) N22 0.0258(12) 0.0408(13) 0.0357(13) -0.0106(10) -0.0040(10) -0.0006(10) C22 0.0306(15) 0.0356(15) 0.0430(16) -0.0105(12) -0.0050(12) 0.0038(12) N21 0.0284(13) 0.0582(16) 0.0384(14) -0.0163(12) -0.0009(10) -0.0009(11) C23 0.0369(17) 0.065(2) 0.0327(15) -0.0181(14) -0.0025(13) -0.0115(15) C21 0.0316(15) 0.0440(17) 0.0358(16) -0.0038(13) -0.0021(12) 0.0090(12) C26 0.065(2) 0.070(2) 0.0341(17) 0.0037(16) -0.0126(16) -0.0292(19) C25 0.050(2) 0.066(2) 0.054(2) -0.0240(18) -0.0105(16) -0.0123(17) C24 0.0377(19) 0.125(4) 0.048(2) -0.048(2) 0.0026(16) -0.009(2) F56 0.0399(9) 0.0267(7) 0.0224(7) -0.0042(6) -0.0039(6) -0.0024(6) F48 0.0344(8) 0.0338(8) 0.0202(7) -0.0058(6) -0.0037(6) -0.0052(6) F42 0.0288(8) 0.0360(8) 0.0339(8) -0.0165(7) -0.0036(6) 0.0018(6) F50 0.0231(8) 0.0286(7) 0.0450(9) -0.0083(7) -0.0050(7) -0.0001(6) F54 0.0244(8) 0.0326(8) 0.0400(9) -0.0037(7) -0.0094(7) -0.0048(6) F60 0.0384(9) 0.0323(8) 0.0242(7) -0.0044(6) 0.0030(6) -0.0036(6) F38 0.0282(8) 0.0353(8) 0.0320(8) -0.0110(6) -0.0084(6) 0.0014(6) F44 0.0423(9) 0.0414(8) 0.0199(7) -0.0057(6) -0.0023(6) -0.0169(7) F57 0.0581(11) 0.0262(8) 0.0405(9) -0.0136(7) -0.0214(8) 0.0081(7) F39 0.0449(10) 0.0373(8) 0.0322(8) -0.0027(7) -0.0197(7) -0.0071(7) F51 0.0374(9) 0.0276(8) 0.0517(10) -0.0064(7) -0.0120(8) 0.0060(7) F52 0.0565(11) 0.0228(7) 0.0402(9) -0.0021(6) -0.0135(8) -0.0108(7) F59 0.0379(9) 0.0542(10) 0.0332(9) -0.0207(8) 0.0126(7) -0.0076(8) F53 0.0377(9) 0.0382(9) 0.0497(10) -0.0001(7) -0.0126(8) -0.0185(7) F41 0.0529(11) 0.0482(10) 0.0373(9) -0.0260(8) 0.0003(8) 0.0019(8) F45 0.0458(10) 0.0601(11) 0.0335(9) -0.0103(8) 0.0084(8) -0.0309(9) F47 0.0398(10) 0.0568(10) 0.0350(9) -0.0158(8) -0.0163(7) -0.0073(8) F40 0.0714(13) 0.0572(11) 0.0284(9) -0.0191(8) -0.0152(8) -0.0104(9) F58 0.0414(10) 0.0475(10) 0.0531(11) -0.0327(8) -0.0053(8) 0.0105(8) F46 0.0334(9) 0.0667(12) 0.0542(11) -0.0246(9) -0.0048(8) -0.0213(8) C49 0.0271(13) 0.0238(11) 0.0194(11) -0.0077(9) -0.0042(9) -0.0025(9) C55 0.0202(12) 0.0275(12) 0.0237(12) -0.0093(9) -0.0038(9) -0.0024(9) C56 0.0275(13) 0.0296(12) 0.0210(12) -0.0093(10) -0.0053(10) -0.0040(10) C43 0.0233(12) 0.0223(11) 0.0232(12) -0.0081(9) -0.0027(9) -0.0013(9) C42 0.0276(13) 0.0249(12) 0.0254(12) -0.0061(10) -0.0049(10) -0.0053(10) C60 0.0233(12) 0.0269(12) 0.0260(12) -0.0074(10) -0.0040(10) -0.0026(10) C38 0.0296(13) 0.0205(11) 0.0257(12) -0.0042(9) -0.0046(10) -0.0039(9) C37 0.0261(13) 0.0215(11) 0.0219(11) -0.0047(9) -0.0021(9) -0.0077(9) C48 0.0219(12) 0.0248(11) 0.0245(12) -0.0081(9) -0.0019(9) 0.0011(9) C44 0.0274(13) 0.0288(12) 0.0223(12) -0.0104(10) -0.0029(10) -0.0038(10) B11 0.0238(14) 0.0231(12) 0.0207(13) -0.0066(10) -0.0028(10) -0.0017(10) C58 0.0246(13) 0.0376(14) 0.0411(15) -0.0246(12) -0.0076(11) 0.0036(11) C53 0.0297(14) 0.0332(13) 0.0280(13) -0.0059(11) -0.0060(11) -0.0108(11) C59 0.0246(13) 0.0409(15) 0.0280(13) -0.0179(11) -0.0002(10) -0.0039(11) C39 0.0360(15) 0.0274(12) 0.0256(13) -0.0022(10) -0.0118(11) -0.0083(11) C50 0.0239(13) 0.0283(12) 0.0264(12) -0.0075(10) -0.0041(10) -0.0035(10) C46 0.0217(13) 0.0395(14) 0.0424(16) -0.0191(12) -0.0016(11) -0.0099(11) C51 0.0317(14) 0.0257(12) 0.0308(13) -0.0073(10) -0.0089(11) 0.0030(10) C47 0.0288(14) 0.0355(13) 0.0280(13) -0.0155(11) -0.0089(10) 0.0001(11) C54 0.0266(13) 0.0285(12) 0.0255(12) -0.0057(10) -0.0072(10) -0.0027(10) C57 0.0337(14) 0.0246(12) 0.0342(14) -0.0109(10) -0.0153(11) 0.0018(10) C41 0.0422(16) 0.0280(13) 0.0277(13) -0.0116(11) 0.0019(11) -0.0068(11) C52 0.0431(16) 0.0227(12) 0.0271(13) -0.0054(10) -0.0086(11) -0.0069(11) C45 0.0315(14) 0.0344(14) 0.0263(13) -0.0099(11) 0.0032(11) -0.0097(11) C40 0.0480(17) 0.0321(13) 0.0231(13) -0.0089(11) -0.0084(12) -0.0107(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 Se1 N1 1.787(2) . ? Se1 N2 1.854(2) . ? F74 C74 1.355(3) . ? F78 C78 1.349(3) . ? F72 C72 1.342(3) . ? F80 C80 1.337(3) . ? F76 C76 1.350(3) . ? F77 C77 1.348(3) . ? F66 C66 1.349(3) . ? F68 C68 1.356(3) . ? F75 C75 1.344(3) . ? F81 C81 1.349(3) . ? F84 C84 1.364(3) . ? F70 C70 1.341(3) . ? F82 C82 1.338(3) . ? N2 C2 1.304(3) . ? N2 C33 1.520(3) . ? F83 C83 1.333(3) . ? F69 C69 1.343(3) . ? F62 C62 1.350(4) . ? F71 C71 1.349(3) . ? N1 C1 1.304(3) . ? F65 C65 1.344(4) . ? C67 C72 1.384(4) . ? C67 C68 1.388(3) . ? C67 B21 1.647(4) . ? C73 C74 1.383(3) . ? C73 C78 1.389(3) . ? C73 B21 1.667(4) . ? C2 C1 1.423(4) . ? C2 H32A 0.9500 . ? C80 C81 1.375(3) . ? C80 C79 1.393(3) . ? C78 C77 1.390(3) . ? C74 C75 1.389(3) . ? C84 C83 1.371(3) . ? C84 C79 1.373(3) . ? F63 C63 1.346(4) . ? C82 C81 1.357(4) . ? C82 C83 1.376(4) . ? B21 C79 1.641(3) . ? B21 C61 1.648(4) . ? C77 C76 1.369(4) . ? C76 C75 1.373(4) . ? C1 H31B 0.9500 . ? C62 C61 1.375(4) . ? C62 C63 1.387(5) . ? C33 C35 1.515(4) . ? C33 C36 1.515(4) . ? C33 C34 1.525(4) . ? C72 C71 1.376(4) . ? C68 C69 1.360(4) . ? C66 C65 1.380(4) . ? C66 C61 1.381(4) . ? C70 C71 1.363(4) . ? C70 C69 1.365(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? F64 C64 1.340(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C65 C64 1.354(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C64 C63 1.360(6) . ? Se22 N21 1.743(3) . ? Se22 N22 1.847(2) . ? N22 C22 1.300(4) . ? N22 C23 1.514(4) . ? C22 C21 1.413(4) . ? C22 H22A 0.9500 . ? N21 C21 1.289(4) . ? C23 C26 1.516(5) . ? C23 C25 1.527(5) . ? C23 C24 1.528(5) . ? C21 H21A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? F56 C56 1.341(3) . ? F48 C48 1.350(3) . ? F42 C42 1.349(3) . ? F50 C50 1.347(3) . ? F54 C54 1.351(3) . ? F60 C60 1.340(3) . ? F38 C38 1.356(3) . ? F44 C44 1.342(3) . ? F57 C57 1.332(3) . ? F39 C39 1.349(3) . ? F51 C51 1.344(3) . ? F52 C52 1.330(3) . ? F59 C59 1.351(3) . ? F53 C53 1.346(3) . ? F41 C41 1.352(3) . ? F45 C45 1.330(3) . ? F47 C47 1.349(3) . ? F40 C40 1.336(3) . ? F58 C58 1.351(3) . ? F46 C46 1.341(3) . ? C49 C50 1.377(3) . ? C49 C54 1.393(3) . ? C49 B11 1.643(3) . ? C55 C56 1.379(3) . ? C55 C60 1.382(3) . ? C55 B11 1.653(4) . ? C56 C57 1.384(4) . ? C43 C44 1.382(3) . ? C43 C48 1.384(3) . ? C43 B11 1.647(4) . ? C42 C41 1.378(4) . ? C42 C37 1.401(3) . ? C60 C59 1.381(4) . ? C38 C37 1.382(4) . ? C38 C39 1.384(4) . ? C37 B11 1.651(4) . ? C48 C47 1.372(4) . ? C44 C45 1.385(4) . ? C58 C59 1.354(4) . ? C58 C57 1.365(4) . ? C53 C54 1.365(4) . ? C53 C52 1.372(4) . ? C39 C40 1.380(4) . ? C50 C51 1.376(3) . ? C46 C45 1.364(4) . ? C46 C47 1.364(4) . ? C51 C52 1.363(4) . ? C41 C40 1.368(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Se1 N2 88.03(10) . . ? C2 N2 C33 126.8(2) . . ? C2 N2 Se1 110.51(17) . . ? C33 N2 Se1 122.70(16) . . ? C1 N1 Se1 111.20(17) . . ? C72 C67 C68 112.5(2) . . ? C72 C67 B21 127.9(2) . . ? C68 C67 B21 119.2(2) . . ? C74 C73 C78 112.5(2) . . ? C74 C73 B21 120.5(2) . . ? C78 C73 B21 126.5(2) . . ? N2 C2 C1 113.8(2) . . ? N2 C2 H32A 123.1 . . ? C1 C2 H32A 123.1 . . ? F80 C80 C81 115.0(2) . . ? F80 C80 C79 119.1(2) . . ? C81 C80 C79 125.9(2) . . ? F78 C78 C73 121.2(2) . . ? F78 C78 C77 114.6(2) . . ? C73 C78 C77 124.3(2) . . ? F74 C74 C73 118.8(2) . . ? F74 C74 C75 115.8(2) . . ? C73 C74 C75 125.3(2) . . ? F84 C84 C83 115.3(2) . . ? F84 C84 C79 121.1(2) . . ? C83 C84 C79 123.6(2) . . ? F82 C82 C81 120.2(2) . . ? F82 C82 C83 121.1(2) . . ? C81 C82 C83 118.8(2) . . ? C79 B21 C67 111.6(2) . . ? C79 B21 C61 102.22(19) . . ? C67 B21 C61 116.0(2) . . ? C79 B21 C73 114.6(2) . . ? C67 B21 C73 100.65(19) . . ? C61 B21 C73 112.3(2) . . ? F83 C83 C84 120.1(2) . . ? F83 C83 C82 119.1(2) . . ? C84 C83 C82 120.8(2) . . ? F77 C77 C76 119.0(2) . . ? F77 C77 C78 120.8(2) . . ? C76 C77 C78 120.2(2) . . ? F76 C76 C77 120.3(2) . . ? F76 C76 C75 121.3(2) . . ? C77 C76 C75 118.4(2) . . ? N1 C1 C2 116.5(2) . . ? N1 C1 H31B 121.8 . . ? C2 C1 H31B 121.8 . . ? F62 C62 C61 120.1(3) . . ? F62 C62 C63 116.2(3) . . ? C61 C62 C63 123.6(3) . . ? C35 C33 C36 110.8(2) . . ? C35 C33 N2 105.6(2) . . ? C36 C33 N2 107.8(2) . . ? C35 C33 C34 112.3(2) . . ? C36 C33 C34 111.3(3) . . ? N2 C33 C34 108.8(2) . . ? F72 C72 C71 114.0(2) . . ? F72 C72 C67 121.4(2) . . ? C71 C72 C67 124.6(2) . . ? F81 C81 C82 119.8(2) . . ? F81 C81 C80 121.9(2) . . ? C82 C81 C80 118.3(2) . . ? C84 C79 C80 112.5(2) . . ? C84 C79 B21 126.7(2) . . ? C80 C79 B21 120.7(2) . . ? F75 C75 C76 119.8(2) . . ? F75 C75 C74 120.9(2) . . ? C76 C75 C74 119.3(2) . . ? F68 C68 C69 116.5(2) . . ? F68 C68 C67 118.7(2) . . ? C69 C68 C67 124.8(3) . . ? F66 C66 C65 115.9(3) . . ? F66 C66 C61 118.7(2) . . ? C65 C66 C61 125.4(3) . . ? F70 C70 C71 119.5(3) . . ? F70 C70 C69 121.5(3) . . ? C71 C70 C69 119.0(3) . . ? C62 C61 C66 112.5(3) . . ? C62 C61 B21 127.8(3) . . ? C66 C61 B21 119.5(2) . . ? F71 C71 C70 119.6(2) . . ? F71 C71 C72 121.1(2) . . ? C70 C71 C72 119.3(3) . . ? F69 C69 C68 120.2(3) . . ? F69 C69 C70 120.0(3) . . ? C68 C69 C70 119.8(2) . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? F65 C65 C64 120.0(3) . . ? F65 C65 C66 120.6(3) . . ? C64 C65 C66 119.5(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F64 C64 C65 121.0(4) . . ? F64 C64 C63 120.8(4) . . ? C65 C64 C63 118.2(3) . . ? F63 C63 C64 119.6(3) . . ? F63 C63 C62 119.5(4) . . ? C64 C63 C62 120.8(3) . . ? N21 Se22 N22 90.17(12) . . ? C22 N22 C23 127.2(3) . . ? C22 N22 Se22 108.8(2) . . ? C23 N22 Se22 123.77(19) . . ? N22 C22 C21 112.9(3) . . ? N22 C22 H22A 123.5 . . ? C21 C22 H22A 123.5 . . ? C21 N21 Se22 109.2(2) . . ? N22 C23 C26 105.4(3) . . ? N22 C23 C25 110.3(3) . . ? C26 C23 C25 111.5(3) . . ? N22 C23 C24 106.8(3) . . ? C26 C23 C24 111.8(3) . . ? C25 C23 C24 110.9(3) . . ? N21 C21 C22 118.9(3) . . ? N21 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C50 C49 C54 113.6(2) . . ? C50 C49 B11 126.0(2) . . ? C54 C49 B11 119.7(2) . . ? C56 C55 C60 112.4(2) . . ? C56 C55 B11 120.0(2) . . ? C60 C55 B11 127.4(2) . . ? F56 C56 C55 118.0(2) . . ? F56 C56 C57 117.1(2) . . ? C55 C56 C57 124.9(2) . . ? C44 C43 C48 112.3(2) . . ? C44 C43 B11 126.5(2) . . ? C48 C43 B11 120.8(2) . . ? F42 C42 C41 115.5(2) . . ? F42 C42 C37 119.5(2) . . ? C41 C42 C37 124.9(2) . . ? F60 C60 C59 115.3(2) . . ? F60 C60 C55 120.6(2) . . ? C59 C60 C55 124.2(2) . . ? F38 C38 C37 121.2(2) . . ? F38 C38 C39 115.4(2) . . ? C37 C38 C39 123.4(2) . . ? C38 C37 C42 113.1(2) . . ? C38 C37 B11 127.2(2) . . ? C42 C37 B11 119.5(2) . . ? F48 C48 C47 115.7(2) . . ? F48 C48 C43 118.7(2) . . ? C47 C48 C43 125.5(2) . . ? F44 C44 C43 120.6(2) . . ? F44 C44 C45 115.4(2) . . ? C43 C44 C45 124.0(2) . . ? C49 B11 C43 114.6(2) . . ? C49 B11 C37 99.08(18) . . ? C43 B11 C37 113.22(19) . . ? C49 B11 C55 113.19(19) . . ? C43 B11 C55 102.44(19) . . ? C37 B11 C55 114.9(2) . . ? F58 C58 C59 120.4(2) . . ? F58 C58 C57 121.6(2) . . ? C59 C58 C57 118.0(2) . . ? F53 C53 C54 121.2(2) . . ? F53 C53 C52 119.7(2) . . ? C54 C53 C52 119.2(2) . . ? F59 C59 C58 118.3(2) . . ? F59 C59 C60 120.9(2) . . ? C58 C59 C60 120.8(2) . . ? F39 C39 C40 119.6(2) . . ? F39 C39 C38 119.5(2) . . ? C40 C39 C38 121.0(2) . . ? F50 C50 C51 114.8(2) . . ? F50 C50 C49 121.3(2) . . ? C51 C50 C49 123.8(2) . . ? F46 C46 C45 121.6(2) . . ? F46 C46 C47 120.2(3) . . ? C45 C46 C47 118.2(2) . . ? F51 C51 C52 120.0(2) . . ? F51 C51 C50 120.2(2) . . ? C52 C51 C50 119.8(2) . . ? F47 C47 C46 119.3(2) . . ? F47 C47 C48 121.2(2) . . ? C46 C47 C48 119.5(2) . . ? F54 C54 C53 116.1(2) . . ? F54 C54 C49 119.6(2) . . ? C53 C54 C49 124.3(2) . . ? F57 C57 C58 119.0(2) . . ? F57 C57 C56 121.2(2) . . ? C58 C57 C56 119.8(2) . . ? F41 C41 C40 119.1(2) . . ? F41 C41 C42 121.4(3) . . ? C40 C41 C42 119.5(2) . . ? F52 C52 C51 120.3(2) . . ? F52 C52 C53 120.4(2) . . ? C51 C52 C53 119.3(2) . . ? F45 C45 C46 119.6(2) . . ? F45 C45 C44 119.9(2) . . ? C46 C45 C44 120.5(2) . . ? F40 C40 C41 120.3(3) . . ? F40 C40 C39 121.6(3) . . ? C41 C40 C39 118.1(2) . . ? 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 Se1 N2 C2 -0.21(18) . . . . ? N1 Se1 N2 C33 178.81(19) . . . . ? N2 Se1 N1 C1 0.22(19) . . . . ? C33 N2 C2 C1 -178.8(2) . . . . ? Se1 N2 C2 C1 0.1(3) . . . . ? C74 C73 C78 F78 178.5(2) . . . . ? B21 C73 C78 F78 6.4(4) . . . . ? C74 C73 C78 C77 -1.0(3) . . . . ? B21 C73 C78 C77 -173.1(2) . . . . ? C78 C73 C74 F74 -177.0(2) . . . . ? B21 C73 C74 F74 -4.4(3) . . . . ? C78 C73 C74 C75 1.5(3) . . . . ? B21 C73 C74 C75 174.1(2) . . . . ? C72 C67 B21 C79 -17.9(3) . . . . ? C68 C67 B21 C79 170.0(2) . . . . ? C72 C67 B21 C61 -134.4(3) . . . . ? C68 C67 B21 C61 53.4(3) . . . . ? C72 C67 B21 C73 104.1(3) . . . . ? C68 C67 B21 C73 -68.0(3) . . . . ? C74 C73 B21 C79 50.3(3) . . . . ? C78 C73 B21 C79 -138.2(2) . . . . ? C74 C73 B21 C67 -69.7(3) . . . . ? C78 C73 B21 C67 101.9(3) . . . . ? C74 C73 B21 C61 166.3(2) . . . . ? C78 C73 B21 C61 -22.1(3) . . . . ? F84 C84 C83 F83 1.2(4) . . . . ? C79 C84 C83 F83 -178.1(2) . . . . ? F84 C84 C83 C82 179.8(2) . . . . ? C79 C84 C83 C82 0.5(4) . . . . ? F82 C82 C83 F83 -1.5(4) . . . . ? C81 C82 C83 F83 176.8(2) . . . . ? F82 C82 C83 C84 180.0(2) . . . . ? C81 C82 C83 C84 -1.8(4) . . . . ? F78 C78 C77 F77 0.2(3) . . . . ? C73 C78 C77 F77 179.8(2) . . . . ? F78 C78 C77 C76 -179.0(2) . . . . ? C73 C78 C77 C76 0.6(4) . . . . ? F77 C77 C76 F76 -0.2(4) . . . . ? C78 C77 C76 F76 179.0(2) . . . . ? F77 C77 C76 C75 -179.7(2) . . . . ? C78 C77 C76 C75 -0.5(4) . . . . ? Se1 N1 C1 C2 -0.2(3) . . . . ? N2 C2 C1 N1 0.0(4) . . . . ? C2 N2 C33 C35 85.6(3) . . . . ? Se1 N2 C33 C35 -93.3(2) . . . . ? C2 N2 C33 C36 -155.9(3) . . . . ? Se1 N2 C33 C36 25.2(3) . . . . ? C2 N2 C33 C34 -35.1(4) . . . . ? Se1 N2 C33 C34 146.0(2) . . . . ? C68 C67 C72 F72 176.8(2) . . . . ? B21 C67 C72 F72 4.3(4) . . . . ? C68 C67 C72 C71 -1.9(4) . . . . ? B21 C67 C72 C71 -174.5(3) . . . . ? F82 C82 C81 F81 0.1(4) . . . . ? C83 C82 C81 F81 -178.1(2) . . . . ? F82 C82 C81 C80 178.4(2) . . . . ? C83 C82 C81 C80 0.1(4) . . . . ? F80 C80 C81 F81 0.2(4) . . . . ? C79 C80 C81 F81 -178.7(2) . . . . ? F80 C80 C81 C82 -178.1(2) . . . . ? C79 C80 C81 C82 3.1(4) . . . . ? F84 C84 C79 C80 -176.9(2) . . . . ? C83 C84 C79 C80 2.3(4) . . . . ? F84 C84 C79 B21 -0.5(4) . . . . ? C83 C84 C79 B21 178.7(2) . . . . ? F80 C80 C79 C84 177.0(2) . . . . ? C81 C80 C79 C84 -4.2(4) . . . . ? F80 C80 C79 B21 0.4(4) . . . . ? C81 C80 C79 B21 179.2(2) . . . . ? C67 B21 C79 C84 131.8(3) . . . . ? C61 B21 C79 C84 -103.6(3) . . . . ? C73 B21 C79 C84 18.2(4) . . . . ? C67 B21 C79 C80 -52.1(3) . . . . ? C61 B21 C79 C80 72.5(3) . . . . ? C73 B21 C79 C80 -165.7(2) . . . . ? F76 C76 C75 F75 -0.8(4) . . . . ? C77 C76 C75 F75 178.7(2) . . . . ? F76 C76 C75 C74 -178.6(2) . . . . ? C77 C76 C75 C74 0.9(4) . . . . ? F74 C74 C75 F75 -0.7(3) . . . . ? C73 C74 C75 F75 -179.3(2) . . . . ? F74 C74 C75 C76 177.0(2) . . . . ? C73 C74 C75 C76 -1.5(4) . . . . ? C72 C67 C68 F68 -177.9(2) . . . . ? B21 C67 C68 F68 -4.6(3) . . . . ? C72 C67 C68 C69 1.5(4) . . . . ? B21 C67 C68 C69 174.8(2) . . . . ? F62 C62 C61 C66 -178.6(2) . . . . ? C63 C62 C61 C66 1.7(4) . . . . ? F62 C62 C61 B21 -3.6(4) . . . . ? C63 C62 C61 B21 176.8(3) . . . . ? F66 C66 C61 C62 179.7(2) . . . . ? C65 C66 C61 C62 -1.1(4) . . . . ? F66 C66 C61 B21 4.2(3) . . . . ? C65 C66 C61 B21 -176.6(2) . . . . ? C79 B21 C61 C62 -105.0(3) . . . . ? C67 B21 C61 C62 16.7(4) . . . . ? C73 B21 C61 C62 131.7(3) . . . . ? C79 B21 C61 C66 69.8(3) . . . . ? C67 B21 C61 C66 -168.5(2) . . . . ? C73 B21 C61 C66 -53.5(3) . . . . ? F70 C70 C71 F71 -0.2(4) . . . . ? C69 C70 C71 F71 -178.6(3) . . . . ? F70 C70 C71 C72 178.1(3) . . . . ? C69 C70 C71 C72 -0.2(4) . . . . ? F72 C72 C71 F71 0.9(4) . . . . ? C67 C72 C71 F71 179.7(2) . . . . ? F72 C72 C71 C70 -177.4(2) . . . . ? C67 C72 C71 C70 1.4(4) . . . . ? F68 C68 C69 F69 0.2(4) . . . . ? C67 C68 C69 F69 -179.2(2) . . . . ? F68 C68 C69 C70 178.8(2) . . . . ? C67 C68 C69 C70 -0.6(4) . . . . ? F70 C70 C69 F69 0.1(4) . . . . ? C71 C70 C69 F69 178.5(3) . . . . ? F70 C70 C69 C68 -178.5(3) . . . . ? C71 C70 C69 C68 -0.1(4) . . . . ? F66 C66 C65 F65 -0.8(4) . . . . ? C61 C66 C65 F65 -180.0(2) . . . . ? F66 C66 C65 C64 179.3(3) . . . . ? C61 C66 C65 C64 0.1(4) . . . . ? F65 C65 C64 F64 1.1(5) . . . . ? C66 C65 C64 F64 -179.0(3) . . . . ? F65 C65 C64 C63 -179.5(3) . . . . ? C66 C65 C64 C63 0.5(5) . . . . ? F64 C64 C63 F63 -0.7(5) . . . . ? C65 C64 C63 F63 179.9(3) . . . . ? F64 C64 C63 C62 179.6(3) . . . . ? C65 C64 C63 C62 0.1(5) . . . . ? F62 C62 C63 F63 -0.7(4) . . . . ? C61 C62 C63 F63 178.9(3) . . . . ? F62 C62 C63 C64 179.0(3) . . . . ? C61 C62 C63 C64 -1.4(5) . . . . ? N21 Se22 N22 C22 -1.3(2) . . . . ? N21 Se22 N22 C23 173.7(2) . . . . ? C23 N22 C22 C21 -173.5(3) . . . . ? Se22 N22 C22 C21 1.2(3) . . . . ? N22 Se22 N21 C21 0.9(2) . . . . ? C22 N22 C23 C26 -149.5(3) . . . . ? Se22 N22 C23 C26 36.5(3) . . . . ? C22 N22 C23 C25 -29.0(4) . . . . ? Se22 N22 C23 C25 157.0(2) . . . . ? C22 N22 C23 C24 91.5(4) . . . . ? Se22 N22 C23 C24 -82.5(3) . . . . ? Se22 N21 C21 C22 -0.5(3) . . . . ? N22 C22 C21 N21 -0.6(4) . . . . ? C60 C55 C56 F56 -176.8(2) . . . . ? B11 C55 C56 F56 -1.7(3) . . . . ? C60 C55 C56 C57 2.8(4) . . . . ? B11 C55 C56 C57 178.0(2) . . . . ? C56 C55 C60 F60 176.3(2) . . . . ? B11 C55 C60 F60 1.6(4) . . . . ? C56 C55 C60 C59 -3.1(4) . . . . ? B11 C55 C60 C59 -177.9(2) . . . . ? F38 C38 C37 C42 -177.7(2) . . . . ? C39 C38 C37 C42 1.8(3) . . . . ? F38 C38 C37 B11 -3.8(4) . . . . ? C39 C38 C37 B11 175.7(2) . . . . ? F42 C42 C37 C38 178.8(2) . . . . ? C41 C42 C37 C38 -0.6(3) . . . . ? F42 C42 C37 B11 4.4(3) . . . . ? C41 C42 C37 B11 -175.0(2) . . . . ? C44 C43 C48 F48 -178.0(2) . . . . ? B11 C43 C48 F48 -4.4(3) . . . . ? C44 C43 C48 C47 1.2(4) . . . . ? B11 C43 C48 C47 174.8(2) . . . . ? C48 C43 C44 F44 178.1(2) . . . . ? B11 C43 C44 F44 4.9(4) . . . . ? C48 C43 C44 C45 -1.2(4) . . . . ? B11 C43 C44 C45 -174.3(2) . . . . ? C50 C49 B11 C43 17.9(3) . . . . ? C54 C49 B11 C43 -172.2(2) . . . . ? C50 C49 B11 C37 -102.9(3) . . . . ? C54 C49 B11 C37 67.0(3) . . . . ? C50 C49 B11 C55 134.8(2) . . . . ? C54 C49 B11 C55 -55.2(3) . . . . ? C44 C43 B11 C49 -132.2(2) . . . . ? C48 C43 B11 C49 55.2(3) . . . . ? C44 C43 B11 C37 -19.5(3) . . . . ? C48 C43 B11 C37 167.9(2) . . . . ? C44 C43 B11 C55 104.9(3) . . . . ? C48 C43 B11 C55 -67.8(3) . . . . ? C38 C37 B11 C49 -105.5(3) . . . . ? C42 C37 B11 C49 68.1(3) . . . . ? C38 C37 B11 C43 132.7(2) . . . . ? C42 C37 B11 C43 -53.7(3) . . . . ? C38 C37 B11 C55 15.5(3) . . . . ? C42 C37 B11 C55 -171.0(2) . . . . ? C56 C55 B11 C49 168.3(2) . . . . ? C60 C55 B11 C49 -17.4(4) . . . . ? C56 C55 B11 C43 -67.8(3) . . . . ? C60 C55 B11 C43 106.5(3) . . . . ? C56 C55 B11 C37 55.4(3) . . . . ? C60 C55 B11 C37 -130.2(3) . . . . ? F58 C58 C59 F59 1.3(4) . . . . ? C57 C58 C59 F59 -177.6(2) . . . . ? F58 C58 C59 C60 -179.8(2) . . . . ? C57 C58 C59 C60 1.3(4) . . . . ? F60 C60 C59 F59 0.6(4) . . . . ? C55 C60 C59 F59 -179.9(2) . . . . ? F60 C60 C59 C58 -178.3(2) . . . . ? C55 C60 C59 C58 1.2(4) . . . . ? F38 C38 C39 F39 -1.7(3) . . . . ? C37 C38 C39 F39 178.8(2) . . . . ? F38 C38 C39 C40 178.4(2) . . . . ? C37 C38 C39 C40 -1.1(4) . . . . ? C54 C49 C50 F50 -179.0(2) . . . . ? B11 C49 C50 F50 -8.6(4) . . . . ? C54 C49 C50 C51 -1.1(4) . . . . ? B11 C49 C50 C51 169.3(2) . . . . ? F50 C50 C51 F51 1.1(4) . . . . ? C49 C50 C51 F51 -177.0(2) . . . . ? F50 C50 C51 C52 179.6(2) . . . . ? C49 C50 C51 C52 1.6(4) . . . . ? F46 C46 C47 F47 0.5(4) . . . . ? C45 C46 C47 F47 179.8(2) . . . . ? F46 C46 C47 C48 -178.6(2) . . . . ? C45 C46 C47 C48 0.7(4) . . . . ? F48 C48 C47 F47 -0.9(3) . . . . ? C43 C48 C47 F47 179.9(2) . . . . ? F48 C48 C47 C46 178.2(2) . . . . ? C43 C48 C47 C46 -1.1(4) . . . . ? F53 C53 C54 F54 1.9(4) . . . . ? C52 C53 C54 F54 -178.0(2) . . . . ? F53 C53 C54 C49 -178.7(2) . . . . ? C52 C53 C54 C49 1.3(4) . . . . ? C50 C49 C54 F54 179.0(2) . . . . ? B11 C49 C54 F54 7.9(3) . . . . ? C50 C49 C54 C53 -0.4(4) . . . . ? B11 C49 C54 C53 -171.5(2) . . . . ? F58 C58 C57 F57 -1.4(4) . . . . ? C59 C58 C57 F57 177.5(2) . . . . ? F58 C58 C57 C56 179.5(2) . . . . ? C59 C58 C57 C56 -1.6(4) . . . . ? F56 C56 C57 F57 0.0(4) . . . . ? C55 C56 C57 F57 -179.7(2) . . . . ? F56 C56 C57 C58 179.1(2) . . . . ? C55 C56 C57 C58 -0.6(4) . . . . ? F42 C42 C41 F41 0.5(3) . . . . ? C37 C42 C41 F41 180.0(2) . . . . ? F42 C42 C41 C40 179.3(2) . . . . ? C37 C42 C41 C40 -1.3(4) . . . . ? F51 C51 C52 F52 -0.5(4) . . . . ? C50 C51 C52 F52 -179.1(2) . . . . ? F51 C51 C52 C53 178.0(2) . . . . ? C50 C51 C52 C53 -0.5(4) . . . . ? F53 C53 C52 F52 -2.2(4) . . . . ? C54 C53 C52 F52 177.7(2) . . . . ? F53 C53 C52 C51 179.2(2) . . . . ? C54 C53 C52 C51 -0.9(4) . . . . ? F46 C46 C45 F45 -0.5(4) . . . . ? C47 C46 C45 F45 -179.8(2) . . . . ? F46 C46 C45 C44 178.7(2) . . . . ? C47 C46 C45 C44 -0.6(4) . . . . ? F44 C44 C45 F45 0.8(4) . . . . ? C43 C44 C45 F45 -179.9(2) . . . . ? F44 C44 C45 C46 -178.3(2) . . . . ? C43 C44 C45 C46 0.9(4) . . . . ? F41 C41 C40 F40 0.3(4) . . . . ? C42 C41 C40 F40 -178.5(2) . . . . ? F41 C41 C40 C39 -179.3(2) . . . . ? C42 C41 C40 C39 2.0(4) . . . . ? F39 C39 C40 F40 -0.3(4) . . . . ? C38 C39 C40 F40 179.6(2) . . . . ? F39 C39 C40 C41 179.2(2) . . . . ? C38 C39 C40 C41 -0.9(4) . . . . ? _diffrn_measured_fraction_theta_max .959 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full .959 _refine_diff_density_max .396 _refine_diff_density_min -1.043 _refine_diff_density_rms .069