# Copyright The Royal Society of Chemistry, 1998 data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Cl4 N2 O4 W2' _chemical_formula_weight 803.76 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1433(3) _cell_length_b 10.1298(4) _cell_length_c 14.9460(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.139(1) _cell_angle_gamma 90.00 _cell_volume 1077.15(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6121 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.5 _exptl_crystal_description Blocks _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 11.191 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1098 _exptl_absorpt_correction_T_max 0.4146 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7058 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2475 _reflns_number_gt 2334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART, (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART & SAINT, (Siemens, 1995)' _computing_data_reduction 'Siemens SHELXTL5, (Sheldrick, 1995)' _computing_structure_solution 'SHELXL-97, (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics 'Siemens SHELXTL5' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+1.5572P] 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 SHELXL-97 _refine_ls_extinction_coef 0.0045(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2475 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.480 _refine_ls_restrained_S_all 1.480 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.11329(3) 0.597850(18) 0.600133(11) 0.02202(10) Uani 1 d . . . Cl1 Cl 0.20549(17) 0.45075(12) 0.47722(8) 0.0264(2) Uani 1 d . . . Cl2 Cl 0.0801(2) 0.40471(13) 0.69441(9) 0.0331(3) Uani 1 d . . . N1 N 0.1562(6) 0.7483(4) 0.5472(3) 0.0241(8) Uani 1 d . . . C1 C 0.2011(6) 0.8697(5) 0.5119(3) 0.0225(9) Uani 1 d . . . C2 C 0.2172(7) 0.8791(5) 0.4196(3) 0.0282(10) Uani 1 d . . . H2 H 0.1944 0.8045 0.3817 0.034 Uiso 1 calc R . . C3 C 0.2671(7) 1.0000(6) 0.3843(3) 0.0323(11) Uani 1 d . . . H3 H 0.2810 1.0075 0.3219 0.039 Uiso 1 calc R . . C4 C 0.2967(8) 1.1093(5) 0.4394(4) 0.0306(11) Uani 1 d . . . H4 H 0.3314 1.1911 0.4147 0.037 Uiso 1 calc R . . C5 C 0.2758(8) 1.0997(5) 0.5312(4) 0.0325(12) Uani 1 d . . . H5 H 0.2930 1.1758 0.5682 0.039 Uiso 1 calc R . . C6 C 0.2304(7) 0.9806(5) 0.5687(3) 0.0280(10) Uani 1 d . . . H6 H 0.2191 0.9734 0.6313 0.034 Uiso 1 calc R . . O7 O -0.0383(6) 0.7571(4) 0.7617(3) 0.0417(10) Uani 1 d . . . C7 C 0.0155(7) 0.6982(6) 0.7050(3) 0.0290(10) Uani 1 d . . . O8 O 0.5238(6) 0.6122(5) 0.6988(3) 0.0420(10) Uani 1 d . . . C8 C 0.3772(8) 0.6057(5) 0.6646(3) 0.0276(10) Uani 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 W 0.02786(13) 0.01909(13) 0.01918(12) 0.00050(7) 0.00246(7) -0.00141(7) Cl1 0.0281(5) 0.0260(6) 0.0252(5) -0.0038(4) 0.0035(4) 0.0015(5) Cl2 0.0462(7) 0.0264(6) 0.0267(6) 0.0063(5) 0.0027(5) -0.0039(5) N1 0.0260(19) 0.023(2) 0.0231(18) -0.0022(15) 0.0028(15) 0.0020(16) C1 0.019(2) 0.021(2) 0.027(2) 0.0010(18) 0.0036(17) 0.0007(17) C2 0.031(3) 0.026(2) 0.028(2) -0.0005(19) 0.009(2) -0.002(2) C3 0.035(3) 0.032(3) 0.031(2) 0.007(2) 0.010(2) 0.000(2) C4 0.027(2) 0.023(2) 0.043(3) 0.008(2) 0.007(2) -0.0001(19) C5 0.034(3) 0.022(3) 0.040(3) -0.003(2) -0.003(2) 0.000(2) C6 0.032(2) 0.024(2) 0.026(2) -0.0004(19) -0.0048(18) 0.004(2) O7 0.053(3) 0.041(2) 0.033(2) -0.0068(18) 0.0148(18) -0.002(2) C7 0.034(3) 0.029(3) 0.024(2) 0.000(2) 0.0040(18) -0.004(2) O8 0.037(2) 0.051(3) 0.037(2) -0.0039(18) -0.0020(17) 0.0002(18) C8 0.031(3) 0.027(3) 0.024(2) 0.0008(18) 0.0022(19) 0.002(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 W N1 1.757(4) . ? W C8 2.040(5) . ? W C7 2.043(5) . ? W Cl2 2.4349(12) . ? W Cl1 2.4991(12) . ? W Cl1 2.5085(12) 3_566 ? Cl1 W 2.5085(12) 3_566 ? N1 C1 1.387(6) . ? C1 C2 1.398(7) . ? C1 C6 1.411(7) . ? C2 C3 1.392(7) . ? C2 H2 0.9500 . ? C3 C4 1.385(8) . ? C3 H3 0.9500 . ? C4 C5 1.397(8) . ? C4 H4 0.9500 . ? C5 C6 1.381(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O7 1.131(7) . ? C8 O8 1.125(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W C8 89.30(19) . . ? N1 W C7 90.0(2) . . ? C7 W C8 89.0(2) . . ? N1 W Cl2 170.99(13) . . ? C8 W Cl2 83.79(15) . . ? C7 W Cl2 84.17(15) . . ? N1 W Cl1 96.77(13) . . ? C8 W Cl1 94.43(15) . . ? C7 W Cl1 172.46(15) . . ? Cl2 W Cl1 89.54(4) . . ? N1 W Cl1 98.65(13) . 3_566 ? C8 W Cl1 170.92(14) . 3_566 ? C7 W Cl1 95.31(15) . 3_566 ? Cl2 W Cl1 88.72(4) . 3_566 ? Cl1 W Cl1 80.35(4) . 3_566 ? W Cl1 W 99.65(4) . 3_566 ? C1 N1 W 174.9(3) . . ? N1 C1 C2 118.5(4) . . ? N1 C1 C6 120.3(4) . . ? C2 C1 C6 121.2(5) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.5(5) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 118.6(5) . . ? C5 C6 H6 120.7 . . ? C1 C6 H6 120.7 . . ? O7 C7 W 178.0(5) . . ? O8 C8 W 178.4(5) . . ? _refine_diff_density_max 0.976 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.154 #=END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Br4 N2 O4 W2' _chemical_formula_weight 981.60 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' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1118(1) _cell_length_b 10.492 _cell_length_c 15.7374(1) _cell_angle_alpha 90.00 _cell_angle_beta 95.0790(1) _cell_angle_gamma 90.00 _cell_volume 1169.66(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5919 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.5 _exptl_crystal_description Blocks _exptl_crystal_colour Red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 16.682 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0590 _exptl_absorpt_correction_T_max 0.1457 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7674 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2685 _reflns_number_gt 2423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART, (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART & SAINT, (Siemens, 1995)' _computing_data_reduction 'Siemens SHELXTL5, (Sheldrick, 1995)' _computing_structure_solution 'SHELXL-97, (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics 'Siemens SHELXTL5' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+32.2400P] 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 SHELXL-97 _refine_ls_extinction_coef 0.0014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2685 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.227 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.11476(7) 0.60282(5) 0.60199(3) 0.02821(18) Uani 1 d . . . Br1 Br 0.23283(14) 0.44615(10) 0.47964(7) 0.0237(2) Uani 1 d . . . Br2 Br 0.07232(18) 0.40224(12) 0.70325(7) 0.0313(3) Uani 1 d . . . N1 N 0.1604(13) 0.7473(10) 0.5513(6) 0.028(2) Uani 1 d . . . C1 C 0.2040(15) 0.8606(12) 0.5145(8) 0.030(2) Uani 1 d . . . C2 C 0.2313(19) 0.8652(14) 0.4279(9) 0.039(3) Uani 1 d . . . H2 H 0.2208 0.7899 0.3944 0.047 Uiso 1 calc R . . C3 C 0.2736(19) 0.9794(15) 0.3914(9) 0.043(3) Uani 1 d . . . H3 H 0.2910 0.9832 0.3323 0.052 Uiso 1 calc R . . C4 C 0.2910(17) 1.0903(13) 0.4410(9) 0.038(3) Uani 1 d . . . H4 H 0.3223 1.1690 0.4158 0.045 Uiso 1 calc R . . C5 C 0.2626(19) 1.0851(13) 0.5262(10) 0.041(3) Uani 1 d . . . H5 H 0.2728 1.1611 0.5591 0.050 Uiso 1 calc R . . C6 C 0.2197(19) 0.9720(13) 0.5653(9) 0.037(3) Uani 1 d . . . H6 H 0.2014 0.9692 0.6244 0.045 Uiso 1 calc R . . O7 O -0.0547(15) 0.7540(11) 0.7516(7) 0.053(3) Uani 1 d . . . C7 C 0.0047(19) 0.6977(13) 0.7002(8) 0.037(3) Uani 1 d . . . O8 O 0.5194(16) 0.6105(12) 0.7034(8) 0.059(3) Uani 1 d . . . C8 C 0.3723(19) 0.6063(14) 0.6687(8) 0.037(3) Uani 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 W 0.0285(3) 0.0253(3) 0.0311(3) -0.00102(19) 0.00449(17) -0.00201(19) Br1 0.0243(5) 0.0219(5) 0.0248(5) -0.0060(4) 0.0015(4) 0.0006(4) Br2 0.0425(6) 0.0270(6) 0.0246(5) 0.0051(4) 0.0036(4) -0.0011(5) N1 0.027(5) 0.027(5) 0.031(5) -0.003(4) 0.007(4) -0.003(4) C1 0.021(5) 0.029(6) 0.038(6) 0.001(5) -0.001(4) -0.005(4) C2 0.040(7) 0.035(7) 0.043(7) -0.003(6) 0.015(6) -0.005(6) C3 0.038(7) 0.050(9) 0.043(8) 0.006(7) 0.015(6) -0.009(6) C4 0.029(6) 0.033(7) 0.051(8) 0.014(6) 0.003(5) 0.002(5) C5 0.039(7) 0.025(6) 0.058(9) 0.003(6) -0.008(6) 0.002(5) C6 0.037(6) 0.033(7) 0.042(7) 0.000(6) -0.002(5) 0.000(5) O7 0.053(6) 0.051(6) 0.056(6) -0.016(6) 0.019(5) -0.003(5) C7 0.040(7) 0.039(7) 0.034(6) -0.005(6) 0.011(5) -0.001(6) O8 0.046(6) 0.061(7) 0.065(7) -0.019(6) -0.013(5) -0.002(5) C8 0.036(6) 0.040(7) 0.035(6) -0.008(6) 0.002(5) 0.004(6) _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 W N1 1.757(10) . ? W C8 2.029(13) . ? W C7 2.051(13) . ? W Br2 2.6729(13) . ? W Br1 2.7204(11) . ? W Br1 2.7318(11) 3_566 ? Br1 W 2.7318(11) 3_566 ? N1 C1 1.369(16) . ? C1 C2 1.395(18) . ? C1 C6 1.415(18) . ? C2 C3 1.37(2) . ? C2 H2 0.9500 . ? C3 C4 1.40(2) . ? C3 H3 0.9500 . ? C4 C5 1.38(2) . ? C4 H4 0.9500 . ? C5 C6 1.383(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? O7 C7 1.115(16) . ? O8 C8 1.137(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W C8 91.4(5) . . ? N1 W C7 91.3(5) . . ? C8 W C7 89.3(5) . . ? N1 W Br2 170.2(3) . . ? C8 W Br2 81.4(4) . . ? C7 W Br2 82.1(4) . . ? N1 W Br1 96.8(3) . . ? C8 W Br1 93.2(4) . . ? C7 W Br1 171.5(4) . . ? Br2 W Br1 90.25(4) . . ? N1 W Br1 98.3(3) . 3_566 ? C8 W Br1 169.9(4) . 3_566 ? C7 W Br1 93.2(4) . 3_566 ? Br2 W Br1 89.26(4) . 3_566 ? Br1 W Br1 82.92(3) . 3_566 ? W Br1 W 97.08(3) . 3_566 ? C1 N1 W 177.1(9) . . ? N1 C1 C2 120.0(12) . . ? N1 C1 C6 119.2(11) . . ? C2 C1 C6 120.8(12) . . ? C3 C2 C1 119.6(13) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.2(13) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.8(12) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.7(13) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 117.8(13) . . ? C5 C6 H6 121.1 . . ? C1 C6 H6 121.1 . . ? O7 C7 W 177.0(13) . . ? O8 C8 W 177.3(13) . . ? _refine_diff_density_max 2.674 _refine_diff_density_min -1.898 _refine_diff_density_rms 0.285