#------------------------------------------------------------------------------ #$Date: 2013-01-20 07:54:01 +0000 (Sun, 20 Jan 2013) $ #$Revision: 71440 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/64/4116439.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_4116439 loop_ _publ_author_name 'Wim T. Klooster' 'Thomas F. Koetzle' 'Per E. M. Siegbahn' 'Thomas B. Richardson' 'Robert H. Crabtree' _publ_contact_author ; Crabtree, R. H. Chemistry Department Yale University New Haven, CT 06511 USA ; _publ_contact_author_email robert.crabtree@yale.edu _publ_contact_author_fax '203 432 6144' _publ_contact_author_phone '203 432 3925' _publ_section_title ; Study of the N-H...H-B Dihydrogen Bond Including the Crystal Structure of BH3NH3 by Neutron Diffraction ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 6337 _journal_page_last 6343 _journal_volume 121 _journal_year 1999 _chemical_formula_sum 'B H6 N' _chemical_formula_weight 30.876 _chemical_name_systematic ; borane ammonia ; _space_group_IT_number 31 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac -2' _symmetry_space_group_name_H-M 'P m n 21' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 5.395(2) _cell_length_b 4.887(2) _cell_length_c 4.986(2) _cell_measurement_reflns_used 32 _cell_measurement_temperature 200 _cell_measurement_theta_max 27 _cell_measurement_theta_min 20 _cell_volume 131.46(9) _computing_cell_refinement local _computing_data_collection local _computing_data_reduction local _computing_structure_refinement UPALS _diffrn_ambient_temperature 200 _diffrn_measurement_device 'beamline H6M, HFBR' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator 'Be (002)' _diffrn_radiation_source reactor _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.0462 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 548 _diffrn_reflns_theta_max 45 _diffrn_reflns_theta_min 3 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 10.369 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_correction_T_min 0.473 _exptl_absorpt_correction_type analytical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.780 _exptl_crystal_density_meas yes _exptl_crystal_density_method calculated _exptl_crystal_description box _exptl_crystal_size_max 1.5 _exptl_crystal_size_mid 0.66 _exptl_crystal_size_min 0.46 _refine_diff_density_max '5 % of maximum' _refine_diff_density_min '5 % of maximum' _refine_ls_abs_structure_details ' ?' _refine_ls_goodness_of_fit_all 1.0467 _refine_ls_goodness_of_fit_obs 1.0158 _refine_ls_hydrogen_treatment ref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 42 _refine_ls_number_reflns 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2833 _refine_ls_R_factor_obs 0.1664 _refine_ls_shift/esd_max .1 _refine_ls_structure_factor_coef F2 _refine_ls_weighting_scheme 1/(s^2(F)) _refine_ls_wR_factor_all 0.1602 _refine_ls_wR_factor_obs 0.1093 _reflns_number_observed 206 _reflns_number_total 548 _reflns_observed_criterion >3sigma _[local]_cod_data_source_file ja9825332.cif _[local]_cod_data_source_block AmmBo _[local]_cod_chemical_formula_sum_orig 'H6 N B' _cod_original_cell_volume 131.5(16) _cod_database_code 4116439 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,-y,1/2+z -x,y,z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N 0.037(5) 0.036(5) 0.026(4) 0.000 0.000 -0.007(5) H1 0.112(22) 0.058(18) 0.129(44) 0.000 0.000 -0.027(30) H2 0.089(15) 0.177(31) 0.017(6) 0.082(22) 0.005(10) 0.004(11) B 0.038(8) 0.032(9) 0.040(8) 0.000 0.000 -0.012(7) H3 0.047(13) 0.094(19) 0.014(11) 0.000 0.000 -0.012(13) H4 0.115(15) 0.117(15) 0.025(8) -0.073(15) 0.023(9) -0.012(12) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type N 0.000 0.235(2) 0.314(4) 0.029(5) Uij H1 0.000 0.453(7) 0.341(15) 0.08(3) Uij H2 0.140(4) 0.148(5) 0.397(6) 0.15(2) Uij B 0.000 0.185(3) 0.000 0.029(7) Uij H3 0.000 -0.043(6) -0.060(6) 0.04(1) Uij H4 0.185(5) 0.264(6) -0.100(5) 0.04(2) Uij loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source H -3.7406 International_Tables_Vol_C B 5.30 International_Tables_Vol_C N 9.36 International_Tables_Vol_C loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 -4 -4 2 0 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_3 _geom_angle_publ_flag B N H1 106.(4) . yes B N H2 111.(2) . yes H1 N H2 113.(3) . yes H2 N H2 104.(3) 4 yes N B H3 114.(2) . yes N B H4 112.(1) . yes H3 B H4 102.(2) . yes H4 B H4 116.(3) 4 yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N B 1.58(2) yes N H1 1.07(4) yes N H2 0.96(3) yes B H3 1.15(3) yes B H4 1.18(3) yes