#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013259.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013259 loop_ _publ_author_name 'Shuvalov, Robert R.' 'Burns, Peter C.' _publ_section_title ; A new polytype of orthoboric acid, H~3~BO~3~-3T ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i47 _journal_page_last i49 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'H3 B O3' _chemical_formula_moiety 'H3 B O3' _chemical_formula_sum 'B H3 O3' _chemical_formula_weight 61.83 _chemical_name_common 'orthoboric acid' _chemical_name_systematic 'boric acid' _space_group_IT_number 145 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'P 32' _symmetry_space_group_name_H-M 'P 32' _audit_creation_method 'SHELXTL and WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 7.0453(4) _cell_length_b 7.0453(4) _cell_length_c 9.5608(7) _cell_measurement_reflns_used 1623 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 33.79 _cell_measurement_theta_min 3.34 _cell_volume 410.98(4) _computing_cell_refinement 'SAINT-Plus (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_molecular_graphics 'ATOMS (Dowty, 2000)' _computing_publication_material 'SHELXTL and WinGX (Farrugia, 1999)' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1998)' _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4615 _diffrn_reflns_theta_full 34.42 _diffrn_reflns_theta_max 34.42 _diffrn_reflns_theta_min 2.13 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_T_max 0.9175 _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(XPREP; Bruker, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'triangular plate' _exptl_crystal_F_000 192 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.284 _refine_diff_density_min -0.253 _refine_ls_extinction_coef 0.051(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXTL (Bruker, 1998)' _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 99 _refine_ls_number_reflns 1143 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_gt 0.0438 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0884 _reflns_number_gt 765 _reflns_number_total 1143 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file fa1014.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2013259 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol B1 0.1837(9) 0.6403(10) 0.2849(7) 0.0485(17) Uani d . 1 . . B B2 0.5180(5) 0.3069(5) 0.2964(5) 0.0277(9) Uani d . 1 . . B O1 0.0621(6) 0.7393(7) 0.2805(3) 0.0514(8) Uani d D 1 . . O O2 0.0864(6) 0.4195(5) 0.2808(3) 0.0467(7) Uani d D 1 . . O O3 0.4090(5) 0.7650(6) 0.2869(3) 0.0441(8) Uani d D 1 . . O O4 0.6437(6) 0.2103(5) 0.2929(2) 0.0413(7) Uani d D 1 . . O O5 0.2950(6) 0.1832(6) 0.2998(3) 0.0506(8) Uani d D 1 . . O O6 0.6136(7) 0.5294(6) 0.2904(3) 0.0464(8) Uani d D 1 . . O H1 0.133(4) 0.877(3) 0.316(3) 0.015(7) Uiso d D 1 . . H H2 -0.057(3) 0.361(5) 0.311(3) 0.013(7) Uiso d D 1 . . H H3 0.483(4) 0.695(4) 0.311(3) 0.022(7) Uiso d D 1 . . H H4 0.565(5) 0.077(4) 0.333(3) 0.048(10) Uiso d D 1 . . H H5 0.243(5) 0.274(4) 0.324(3) 0.027(8) Uiso d D 1 . . H H6 0.755(3) 0.602(4) 0.318(3) 0.027(8) Uiso d D 1 . . H 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 B1 0.045(3) 0.056(3) 0.050(3) 0.029(2) -0.0005(16) -0.002(2) B2 0.0144(12) 0.0177(14) 0.053(3) 0.0093(11) 0.0007(10) 0.0015(11) O1 0.0246(14) 0.0384(18) 0.097(2) 0.0198(14) -0.0021(15) -0.0049(16) O2 0.0263(15) 0.0278(14) 0.0859(19) 0.0133(13) -0.0038(16) -0.0024(14) O3 0.0233(12) 0.0254(14) 0.082(2) 0.0108(12) -0.0006(14) -0.0032(14) O4 0.0279(16) 0.0249(15) 0.072(2) 0.0138(14) -0.0007(13) -0.0025(12) O5 0.0284(14) 0.0379(18) 0.0902(19) 0.0201(13) -0.0026(15) 0.0010(16) O6 0.0307(19) 0.0325(15) 0.0772(18) 0.0167(13) 0.0070(15) 0.0080(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag B1 O1 . 1.349(5) yes B1 O2 . 1.350(6) yes B1 O3 . 1.377(6) yes B2 O4 . 1.361(4) yes B2 O5 . 1.364(4) yes B2 O6 . 1.363(5) yes O1 H1 . 0.91(2) no O2 H2 . 0.93(2) no O3 H3 . 0.91(2) no O4 H4 . 0.90(2) no O5 H5 . 0.91(2) no O6 H6 . 0.91(2) no 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 B1 O2 . 120.4(5) yes O1 B1 O3 . 119.9(5) yes O2 B1 O3 . 119.6(4) yes B1 O1 H1 . 113(2) yes H1 O1 H6 1_455 111(2) no B1 O1 H6 1_455 126.0(10) no B1 O2 H2 . 108(2) yes H2 O2 H5 . 120(2) no B1 O2 H5 . 121.0(10) no B1 O3 H3 . 117(2) yes H3 O3 H4 1_565 114(2) no B1 O3 H4 1_565 123.0(10) no O4 B2 O5 . 120.7(3) yes O4 B2 O6 . 120.2(3) yes O5 B2 O6 . 119.0(2) yes B2 O4 H4 . 107(2) yes H4 O4 H2 1_655 120(2) no B2 O4 H2 1_655 124.0(10) no B2 O5 H5 . 107(2) yes H5 O5 H1 1_545 124(2) no B2 O5 H1 1_545 125.4(8) no B2 O6 H6 . 114(2) yes H6 O6 H3 . 112(2) no B2 O6 H3 . 128.0(10) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O5 1_565 0.91(2) 1.88(2) 2.715(7) 153(2) yes O2 H2 O4 1_455 0.93(2) 1.83(2) 2.705(6) 155(2) yes O3 H3 O6 . 0.91(2) 1.82(2) 2.688(7) 159(3) yes O4 H4 O3 1_545 0.91(2) 1.95(2) 2.719(5) 141(3) yes O5 H5 O2 . 0.91(2) 1.89(2) 2.723(6) 151(2) yes O6 H6 O1 1_655 0.91(2) 1.91(2) 2.740(6) 151(3) yes _cod_database_fobs_code 2013259