#------------------------------------------------------------------------------ #$Date: 2019-12-17 21:39:28 +0000 (Tue, 17 Dec 2019) $ #$Revision: 245269 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500086.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500086 loop_ _publ_author_name 'Thierry Maris' _journal_name_full 'Personal communication to COD' _journal_year 2019 _chemical_formula_moiety 'Br, C4 H12 N' _chemical_formula_sum 'C4 H12 Br N' _chemical_formula_weight 154.06 _space_group_crystal_system tetragonal _space_group_IT_number 129 _space_group_name_Hall '-P 4a 2a' _space_group_name_H-M_alt 'P 4/n m m :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2013-03-28 _audit_creation_method ; Olex2 1.2 (compiled Mar 21 2013 11:16:32, GUI svn.r4446) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.6590(3) _cell_length_b 7.6590(3) _cell_length_c 5.4566(2) _cell_measurement_reflns_used 4465 _cell_measurement_temperature 150 _cell_measurement_theta_max 69.203 _cell_measurement_theta_min 5.777 _cell_volume 320.09(2) _computing_cell_refinement 'SAINT v8.27A (Bruker, 2012)' _computing_data_collection 'APEX2 (Bruker, 2012)' _computing_data_reduction 'SAINT v8.27A (Bruker, 2012)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XLMP, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 150 _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Microstar X8' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'Helios Mirror Optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_unetI/netI 0.0172 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 5415 _diffrn_reflns_theta_full 69.19 _diffrn_reflns_theta_max 69.19 _diffrn_reflns_theta_min 8.12 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 7.711 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_correction_T_min 0.6252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0877 before and 0.0707 after correction. The Ratio of minimum to maximum transmission is 0.8301. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 156 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _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. ; _refine_diff_density_max 0.352 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 19 _refine_ls_number_reflns 195 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0199 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.1180P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0496 _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. ; _reflns_number_gt 191 _reflns_number_total 195 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c1nbr.cif _cod_data_source_block c1nbr _cod_original_sg_symbol_H-M 'P 4/n m m' _cod_database_code 3500086 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y+1/2, x, z' 3 '-x+1/2, -y+1/2, z' 4 'y, -x+1/2, z' 5 'x+1/2, -y, -z' 6 '-x, y+1/2, -z' 7 'y+1/2, x+1/2, -z' 8 '-y, -x, -z' 9 '-x, -y, -z' 10 'y-1/2, -x, -z' 11 'x-1/2, y-1/2, -z' 12 '-y, x-1/2, -z' 13 '-x-1/2, y, z' 14 'x, -y-1/2, z' 15 '-y-1/2, -x-1/2, z' 16 'y, x, z' 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 0.2500 0.2500 0.12377(7) 0.0215(2) Uani 1 8 d S . . N1 N 0.7500 0.2500 0.5000 0.0176(8) Uani 1 8 d S . . C1 C 0.5912(3) 0.2500 0.6605(4) 0.0269(6) Uani 1 2 d S . . H1A H 0.492(4) 0.2500 0.560(5) 0.025(7) Uiso 1 2 d S . . H1B H 0.594(3) 0.359(2) 0.763(2) 0.033(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0219(3) 0.0219(3) 0.0206(3) 0.000 0.000 0.000 N1 0.0175(11) 0.0175(11) 0.0178(17) 0.000 0.000 0.000 C1 0.0169(13) 0.0379(15) 0.0259(11) 0.000 0.0035(10) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 N1 C1 109.97(10) . 10_666 C1 N1 C1 108.5(2) 12_656 10_666 C1 N1 C1 109.97(10) 3_655 10_666 C1 N1 C1 109.97(10) . 12_656 C1 N1 C1 108.5(2) . 3_655 C1 N1 C1 109.97(10) 12_656 3_655 N1 C1 H1A 108.4(18) . . N1 C1 H1B 107.9(11) . . H1A C1 H1B 110.2(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N1 C1 1.499(3) 3_655 N1 C1 1.499(3) 10_666 N1 C1 1.499(3) 12_656 N1 C1 1.499(3) . C1 H1A 0.94(3) . C1 H1B 1.003(17) . _cod_database_fobs_code 3500086