#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/26/1502676.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_1502676 loop_ _publ_author_name 'Mebs, Stefan' 'Grabowsky, Simon' 'F\"orster, Diana' 'Kickbusch, Rainer' 'Hartl, Monika' 'Daemen, Luke L.' 'Morgenroth, Wolfgang' 'Luger, Peter' 'Paulus, Beate' 'Lentz, Dieter' _publ_contact_author ; Prof. Dr. Dieter Lentz Institut f\"ur Chemie und Biochemie Anorganische Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195, Berlin Germany ; _publ_section_title ; Charge transfer via the dative N-B bond and dihydrogen contacts. Experimental and theoretical electron density studies of small Lewis acid-base adducts. ; _journal_issue 37 _journal_name_full 'The journal of physical chemistry. A' _journal_page_first 10185 _journal_page_last 10196 _journal_paper_doi 10.1021/jp100995n _journal_volume 114 _journal_year 2010 _chemical_absolute_configuration hb _chemical_formula_moiety 'B H7 N2' _chemical_formula_sum 'B H7 N2' _chemical_formula_weight 45.89 _chemical_name_common Hydrazineborane _chemical_name_systematic ; ? ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.974(2) _cell_length_b 5.0702(10) _cell_length_c 9.5069(10) _cell_measurement_temperature 95(2) _cell_volume 625.37(17) _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_collection 'SMART (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_molecular_graphics 'Volkov et al, (2006)' _computing_publication_material 'Volkov et al, (2006)' _computing_structure_refinement 'Volkov et al, (2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 95(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'BRUKER SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 100200 _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 68.10 _diffrn_reflns_theta_max 68.10 _diffrn_reflns_theta_min 3.14 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 208 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.243 _refine_diff_density_min -0.097 _refine_diff_density_rms 0.030 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 4645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.018 _refine_ls_R_Fsqd_factor 0.031 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w2 = 1/[s^2^(Fo^2^)] ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.042 _reflns_number_gt 4645 _reflns_number_total 5759 _reflns_threshold_expression >2sigma(I) _cod_data_source_file jp100995n_si_002.cif _cod_data_source_block hydbor _cod_original_cell_volume 625.36(17) _cod_database_code 1502676 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_local_axes_atom_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 N(1) N(2) X N(1) DUM1 Y N(2) N(1) X N(2) DUM2 Y B(1) N(1) Z B(1) H(1) Y H(1) B(1) Z H(1) H(2) Y H(2) B(1) Z H(2) H(3) Y H(3) B(1) Z H(3) H(1) Y H(4) N(1) Z H(4) H(5) Y H(5) N(1) Z H(5) H(4) Y H(6) N(2) Z H(6) H(7) Y H(7) N(2) Z H(7) H(6) Y loop_ _atom_rho_multipole_atom_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa _atom_rho_multipole_kappa_prime0 _atom_rho_multipole_kappa_prime1 _atom_rho_multipole_kappa_prime2 _atom_rho_multipole_kappa_prime3 _atom_rho_multipole_kappa_prime4 _atom_rho_multipole_radial_slater_n0 _atom_rho_multipole_radial_slater_zeta0 _atom_rho_multipole_radial_slater_n1 _atom_rho_multipole_radial_slater_zeta1 _atom_rho_multipole_radial_slater_n2 _atom_rho_multipole_radial_slater_zeta2 _atom_rho_multipole_radial_slater_n3 _atom_rho_multipole_radial_slater_zeta3 _atom_rho_multipole_radial_slater_n4 _atom_rho_multipole_radial_slater_zeta4 N(1) 4.99(3) 0 -0.061(5) -0.072(5) 0 -0.022(5) 0 0 -0.072(4) 0.020(4) 0 -0.103(5) 0.132(5) 0 0 0.133(4) 0.009(4) 0.013(6) 0 0 -0.060(6) -0.025(6) 0 0 0.023(5) -0.009(6) 1.011931 0.919221 0.919221 0.919221 0.919221 0.919221 2 3.83936 2 3.83936 2 3.83936 3 3.83936 4 3.83936 N(2) 4.92(2) 0 -0.077(4) -0.165(6) 0 -0.035(5) 0 0 -0.112(4) 0.040(4) 0 -0.115(5) 0.061(5) 0 0 0.107(4) 0.005(4) 0.019(6) 0 0 -0.025(6) -0.028(6) 0 0 0.042(5) 0.030(5) 1.009152 0.919545 0.919545 0.919545 0.919545 0.919545 2 3.83936 2 3.83936 2 3.83936 3 3.83936 4 3.83936 B(1) 2.70(4) 0 0 0 -0.015(11) -0.077(10) 0 0 0 0 0.297(11) 0 0 0 0 -0.035(9) -0.185(11) 0.136(12) 0 0 0 0 0.021(11) 0.058(12) 0 0 1.033911 0.949153 0.949153 0.949153 0.949153 0.949153 2 2.5246 2 2.5246 2 2.5246 3 2.5246 4 2.5246 H(1) 1.171(12) 0 0 0 0.157(10) 0.055(13) 0 0 0 0 0.069(15) 0 0 0 0 0 0 0.07(2) 0 0 0 0 0 0 0 0 1.123842 1.055422 1.055422 1.055422 1.055422 1.055422 0 2 1 2 2 2 3 2 4 2 H(2) 1.160(12) 0 0 0 0.148(9) 0.057(12) 0 0 0 0 0.065(15) 0 0 0 0 0 0 0.048(17) 0 0 0 0 0 0 0 0 1.123842 1.055422 1.055422 1.055422 1.055422 1.055422 0 2 1 2 2 2 3 2 4 2 H(3) 1.065(11) 0 0 0 0.170(9) 0.087(12) 0 0 0 0 0.079(14) 0 0 0 0 0 0 0.068(19) 0 0 0 0 0 0 0 0 1.123842 1.055422 1.055422 1.055422 1.055422 1.055422 0 2 1 2 2 2 3 2 4 2 H(4) 0.989(10) 0 0 0 0.225(7) 0.179(11) 0 0 0 0 0.102(14) 0 0 0 0 0 0 -0.012(17) 0 0 0 0 0 0 0 0 1.15693 1.288218 1.288218 1.288218 1.288218 1.288218 0 2 1 2 2 2 3 2 4 2 H(5) 0.998(10) 0 0 0 0.238(8) 0.136(11) 0 0 0 0 0.076(14) 0 0 0 0 0 0 0.032(15) 0 0 0 0 0 0 0 0 1.15693 1.288218 1.288218 1.288218 1.288218 1.288218 0 2 1 2 2 2 3 2 4 2 H(6) 1.058(13) 0 0 0 0.276(9) 0.161(13) 0 0 0 0 0.103(16) 0 0 0 0 0 0 -0.010(17) 0 0 0 0 0 0 0 0 1.14297 1.275013 1.275013 1.275013 1.275013 1.275013 0 2 1 2 2 2 3 2 4 2 H(7) 0.955(11) 0 0 0 0.271(8) 0.192(11) 0 0 0 0 0.126(14) 0 0 0 0 0 0 0.045(14) 0 0 0 0 0 0 0 0 1.14297 1.275013 1.275013 1.275013 1.275013 1.275013 0 2 1 2 2 2 3 2 4 2 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(1) 0.009464(18) 0.010274(18) 0.010281(19) 0.000071(12) 0.000059(11) 0.000513(12) N(2) 0.01134(2) 0.01207(2) 0.01262(2) 0.000935(15) -0.000348(14) -0.001728(14) B(1) 0.01264(3) 0.01587(3) 0.01068(3) -0.00048(2) 0.000231(19) -0.00068(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_U_iso_or_equiv N(1) 0.361634(5) 0.121665(13) 0.560864(6) 1 8 0.010 N(2) 0.343385(6) 0.380910(14) 0.620720(7) 1 8 0.012 B(1) 0.392767(8) 0.13610(2) 0.398674(10) 1 8 0.013 H(1) 0.466562 0.284519 0.390868 1 8 0.044 H(2) 0.417696 -0.086126 0.363116 1 8 0.040 H(3) 0.319034 0.218204 0.332145 1 8 0.034 H(4) 0.294406 0.02022 0.573801 1 8 0.034 H(5) 0.418913 0.027282 0.614412 1 8 0.035 H(6) 0.343698 0.362 0.728063 1 8 0.039 H(7) 0.407236 0.487585 0.592523 1 8 0.033 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) N(1) B(1) 112.243(6) 1_555 1_555 1_555 yes N(2) N(1) H(4) 105.655 1_555 1_555 1_555 yes N(2) N(1) H(5) 110.363 1_555 1_555 1_555 yes B(1) N(1) H(4) 110.861 1_555 1_555 1_555 yes B(1) N(1) H(5) 108.626 1_555 1_555 1_555 yes H(4) N(1) H(5) 109.040 1_555 1_555 1_555 yes N(1) N(2) H(6) 107.753 1_555 1_555 1_555 yes N(1) N(2) H(7) 104.090 1_555 1_555 1_555 yes H(6) N(2) H(7) 107.851 1_555 1_555 1_555 yes N(1) B(1) H(1) 106.602 1_555 1_555 1_555 yes N(1) B(1) H(2) 107.008 1_555 1_555 1_555 yes N(1) B(1) H(3) 108.551 1_555 1_555 1_555 yes H(1) B(1) H(2) 110.167 1_555 1_555 1_555 yes H(1) B(1) H(3) 111.920 1_555 1_555 1_555 yes H(2) B(1) H(3) 112.293 1_555 1_555 1_555 yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N(1) N(2) 1.4518(3) 1_555 1_555 yes N(1) B(1) 1.5956(3) 1_555 1_555 yes N(1) H(4) 1.02001 1_555 1_555 yes N(1) H(5) 1.02000 1_555 1_555 yes N(2) H(6) 1.02500 1_555 1_555 yes N(2) H(7) 1.02500 1_555 1_555 yes B(1) H(1) 1.22000 1_555 1_555 yes B(1) H(2) 1.22000 1_555 1_555 yes B(1) H(3) 1.22000 1_555 1_555 yes #BEGIN Loops that were not found in dictionaries: loop_ _atom_dummy_label _atom_dummy_fract_x _atom_dummy_fract_y _atom_dummy_fract_z DUM0 0 0 0 DUM1 0.356648 0.023753 0.5941 DUM2 0.375383 0.424602 0.660601 #END Loops that were not found in dictionaries