data_fapbbr3_2ndcrystal_rt _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H5 Br3 N2 Pb' _chemical_formula_weight 491.99 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 6.0134(3) _cell_length_b 6.0134(3) _cell_length_c 6.0134(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 217.450(19) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 212 _exptl_absorpt_coefficient_mu 33.090 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0828 _exptl_absorpt_correction_T_max 0.1547 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 775 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 30.33 _reflns_number_total 91 _reflns_number_gt 87 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 91 _refine_ls_number_parameters 9 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.176 _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 Pb1 Pb 0.0000 0.0000 0.0000 0.0465(4) Uani 1 48 d S . . Br1 Br 0.5000 0.0000 0.0000 0.0922(9) Uani 1 16 d S . . C1 C 0.5000 0.573(12) 0.5000 0.07(3) Uiso 0.17 8 d SPD . . N1 N 0.657(8) 0.425(10) 0.5000 0.08(3) Uiso 0.08 2 d SPD . . 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 Pb1 0.0465(4) 0.0465(4) 0.0465(4) 0.000 0.000 0.000 Br1 0.0430(11) 0.1168(14) 0.1168(14) 0.000 0.000 0.000 _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 Pb1 Br1 3.00670(15) 9 ? Pb1 Br1 3.00670(15) . ? Pb1 Br1 3.00670(15) 1_455 ? Pb1 Br1 3.00670(15) 5_545 ? Pb1 Br1 3.00670(15) 5 ? Pb1 Br1 3.00670(15) 9_554 ? Br1 Pb1 3.00670(15) 1_655 ? C1 C1 0.62(10) 33_666 ? C1 C1 0.62(10) 29_666 ? C1 C1 0.62(10) 9 ? C1 C1 0.62(10) 5 ? C1 N1 0.68(10) 39_656 ? C1 N1 0.68(10) 31_556 ? C1 N1 0.68(10) 13_556 ? C1 N1 0.68(10) 5 ? C1 C1 0.88(14) 25_666 ? C1 N1 0.94(5) 27_565 ? C1 N1 0.94(5) 47_566 ? C1 N1 0.94(5) 45_665 ? N1 N1 0.64(9) 17_556 ? N1 N1 0.64(9) 43 ? N1 C1 0.68(10) 9 ? N1 N1 0.69(12) 37_665 ? N1 N1 0.91(12) 27_565 ? N1 C1 0.94(5) 25_666 ? N1 C1 1.13(2) 29_666 ? N1 C1 1.13(2) 5 ? N1 N1 1.15(6) 7_665 ? N1 N1 1.15(6) 33_666 ? N1 N1 1.15(6) 29_666 ? N1 N1 1.15(6) 35_655 ? 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 Br1 Pb1 Br1 90.0 9 . ? Br1 Pb1 Br1 90.0 9 1_455 ? Br1 Pb1 Br1 180.0 . 1_455 ? Br1 Pb1 Br1 90.0 9 5_545 ? Br1 Pb1 Br1 90.0 . 5_545 ? Br1 Pb1 Br1 90.0 1_455 5_545 ? Br1 Pb1 Br1 90.0 9 5 ? Br1 Pb1 Br1 90.0 . 5 ? Br1 Pb1 Br1 90.0 1_455 5 ? Br1 Pb1 Br1 180.0 5_545 5 ? Br1 Pb1 Br1 180.0 9 9_554 ? Br1 Pb1 Br1 90.0 . 9_554 ? Br1 Pb1 Br1 90.0 1_455 9_554 ? Br1 Pb1 Br1 90.0 5_545 9_554 ? Br1 Pb1 Br1 90.0 5 9_554 ? Pb1 Br1 Pb1 180.0 1_655 . ? C1 C1 C1 60.000(15) 33_666 29_666 ? C1 C1 C1 90.000(7) 33_666 9 ? C1 C1 C1 60.000(13) 29_666 9 ? C1 C1 C1 60.000(18) 33_666 5 ? C1 C1 C1 90.000(7) 29_666 5 ? C1 C1 C1 60.000(7) 9 5 ? C1 C1 N1 177(6) 33_666 39_656 ? C1 C1 N1 122(3) 29_666 39_656 ? C1 C1 N1 93(6) 9 39_656 ? C1 C1 N1 122(3) 5 39_656 ? C1 C1 N1 122(3) 33_666 31_556 ? C1 C1 N1 177(6) 29_666 31_556 ? C1 C1 N1 122(3) 9 31_556 ? C1 C1 N1 93(6) 5 31_556 ? N1 C1 N1 57(7) 39_656 31_556 ? C1 C1 N1 93(6) 33_666 13_556 ? C1 C1 N1 122(3) 29_666 13_556 ? C1 C1 N1 177(6) 9 13_556 ? C1 C1 N1 122(3) 5 13_556 ? N1 C1 N1 84(10) 39_656 13_556 ? N1 C1 N1 57(7) 31_556 13_556 ? C1 C1 N1 122(3) 33_666 5 ? C1 C1 N1 93(6) 29_666 5 ? C1 C1 N1 122(3) 9 5 ? C1 C1 N1 177(6) 5 5 ? N1 C1 N1 57(7) 39_656 5 ? N1 C1 N1 84(10) 31_556 5 ? N1 C1 N1 57(7) 13_556 5 ? C1 C1 C1 45.000(2) 33_666 25_666 ? C1 C1 C1 45.000(15) 29_666 25_666 ? C1 C1 C1 45.0 9 25_666 ? C1 C1 C1 45.000(15) 5 25_666 ? N1 C1 C1 138(6) 39_656 25_666 ? N1 C1 C1 138(6) 31_556 25_666 ? N1 C1 C1 138(6) 13_556 25_666 ? N1 C1 C1 138(6) 5 25_666 ? C1 C1 N1 136(7) 33_666 27_565 ? C1 C1 N1 91(5) 29_666 27_565 ? C1 C1 N1 46(7) 9 27_565 ? C1 C1 N1 91(5) 5 27_565 ? N1 C1 N1 47(9) 39_656 27_565 ? N1 C1 N1 89(5) 31_556 27_565 ? N1 C1 N1 131(10) 13_556 27_565 ? N1 C1 N1 89(5) 5 27_565 ? C1 C1 N1 91(7) 25_666 27_565 ? C1 C1 N1 91(5) 33_666 47_566 ? C1 C1 N1 46(7) 29_666 47_566 ? C1 C1 N1 91(5) 9 47_566 ? C1 C1 N1 136(7) 5 47_566 ? N1 C1 N1 89(5) 39_656 47_566 ? N1 C1 N1 131(10) 31_556 47_566 ? N1 C1 N1 89(5) 13_556 47_566 ? N1 C1 N1 47(9) 5 47_566 ? C1 C1 N1 91(7) 25_666 47_566 ? N1 C1 N1 90.0(2) 27_565 47_566 ? C1 C1 N1 91(5) 33_666 45_665 ? C1 C1 N1 136(7) 29_666 45_665 ? C1 C1 N1 91(5) 9 45_665 ? C1 C1 N1 46(7) 5 45_665 ? N1 C1 N1 89(5) 39_656 45_665 ? N1 C1 N1 47(9) 31_556 45_665 ? N1 C1 N1 89(5) 13_556 45_665 ? N1 C1 N1 131(10) 5 45_665 ? C1 C1 N1 91(7) 25_666 45_665 ? N1 C1 N1 90.0(2) 27_565 45_665 ? N1 C1 N1 178(10) 47_566 45_665 ? N1 N1 N1 90.00(4) 17_556 43 ? N1 N1 C1 62(4) 17_556 9 ? N1 N1 C1 62(4) 43 9 ? N1 N1 N1 120.00(2) 17_556 37_665 ? N1 N1 N1 120.00(2) 43 37_665 ? C1 N1 N1 87(6) 9 37_665 ? N1 N1 N1 45.000(5) 17_556 27_565 ? N1 N1 N1 45.000(6) 43 27_565 ? C1 N1 N1 48(6) 9 27_565 ? N1 N1 N1 135.000(19) 37_665 27_565 ? N1 N1 C1 89(5) 17_556 25_666 ? N1 N1 C1 89(5) 43 25_666 ? C1 N1 C1 41(10) 9 25_666 ? N1 N1 C1 46(7) 37_665 25_666 ? N1 N1 C1 89(7) 27_565 25_666 ? N1 N1 C1 89(4) 17_556 29_666 ? N1 N1 C1 56(3) 43 29_666 ? C1 N1 C1 28(6) 9 29_666 ? N1 N1 C1 72(3) 37_665 29_666 ? N1 N1 C1 66(3) 27_565 29_666 ? C1 N1 C1 33(6) 25_666 29_666 ? N1 N1 C1 56(3) 17_556 5 ? N1 N1 C1 89(4) 43 5 ? C1 N1 C1 28(6) 9 5 ? N1 N1 C1 72(3) 37_665 5 ? N1 N1 C1 66(3) 27_565 5 ? C1 N1 C1 33(6) 25_666 5 ? C1 N1 C1 46(8) 29_666 5 ? N1 N1 N1 125.26(6) 17_556 7_665 ? N1 N1 N1 91(5) 43 7_665 ? C1 N1 N1 71(4) 9 7_665 ? N1 N1 N1 29(5) 37_665 7_665 ? N1 N1 N1 115(4) 27_565 7_665 ? C1 N1 N1 36(5) 25_666 7_665 ? C1 N1 N1 48.6(9) 29_666 7_665 ? C1 N1 N1 69(3) 5 7_665 ? N1 N1 N1 107(3) 17_556 33_666 ? N1 N1 N1 31(5) 43 33_666 ? C1 N1 N1 54.7(2) 9 33_666 ? N1 N1 N1 89(5) 37_665 33_666 ? N1 N1 N1 67(4) 27_565 33_666 ? C1 N1 N1 65(3) 25_666 33_666 ? C1 N1 N1 34(5) 29_666 33_666 ? C1 N1 N1 79(4) 5 33_666 ? N1 N1 N1 60.000(11) 7_665 33_666 ? N1 N1 N1 91(5) 17_556 29_666 ? N1 N1 N1 125.26(6) 43 29_666 ? C1 N1 N1 71(4) 9 29_666 ? N1 N1 N1 29(5) 37_665 29_666 ? N1 N1 N1 115(4) 27_565 29_666 ? C1 N1 N1 36(5) 25_666 29_666 ? C1 N1 N1 69(3) 29_666 29_666 ? C1 N1 N1 48.6(9) 5 29_666 ? N1 N1 N1 46(8) 7_665 29_666 ? N1 N1 N1 98(6) 33_666 29_666 ? N1 N1 N1 31(5) 17_556 35_655 ? N1 N1 N1 107(3) 43 35_655 ? C1 N1 N1 54.7(2) 9 35_655 ? N1 N1 N1 89(5) 37_665 35_655 ? N1 N1 N1 67(4) 27_565 35_655 ? C1 N1 N1 65(3) 25_666 35_655 ? C1 N1 N1 79(4) 29_666 35_655 ? C1 N1 N1 34(5) 5 35_655 ? N1 N1 N1 98(6) 7_665 35_655 ? N1 N1 N1 109.4(3) 33_666 35_655 ? N1 N1 N1 60.000(11) 29_666 35_655 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.758 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.150