#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/05/2200520.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_2200520 loop_ _publ_author_name 'Thadani, Avinash N.' 'Batey, Robert A.' 'Lough, Alan J.' _publ_section_title ; 4,5,7,8-Tetrahydro-2-(2-propenyl)-6H-[1,3,6,2]dioxazaborocine ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o762 _journal_page_last o763 _journal_paper_doi 10.1107/S1600536801011679 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C7 H14 B N O2' _chemical_formula_moiety 'C7 H14 B N O2' _chemical_formula_sum 'C7 H14 B N O2' _chemical_formula_weight 155.00 _chemical_name_systematic ; 4,5,7,8-Tetrahydro-2-(2-Propenyl)-6H-[1,3,6,2]-dioxazaborocine ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 100.524(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 21.1480(17) _cell_length_b 8.5399(11) _cell_length_c 9.4229(10) _cell_measurement_reflns_used 6734 _cell_measurement_temperature 100.0(10) _cell_measurement_theta_max 26.19 _cell_measurement_theta_min 4.10 _cell_volume 1673.2(3) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1999)' _diffrn_ambient_temperature 100.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full .990 _diffrn_measured_fraction_theta_max .990 _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .138 _diffrn_reflns_av_sigmaI/netI .1017 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 6735 _diffrn_reflns_theta_full 26.19 _diffrn_reflns_theta_max 26.19 _diffrn_reflns_theta_min 4.10 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .086 _exptl_absorpt_correction_T_max .994 _exptl_absorpt_correction_T_min .966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 672 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .07 _refine_diff_density_max .281 _refine_diff_density_min -.327 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .987 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1668 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .987 _refine_ls_R_factor_all .1201 _refine_ls_R_factor_gt .0630 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0903P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1760 _reflns_number_gt 978 _reflns_number_total 1668 _reflns_threshold_expression I>2\s(I) _cod_data_source_file om6035.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 'Monoclinic' changed to 'monoclinic' 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_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2200520 _cod_database_fobs_code 2200520 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 O1 .41836(8) .0141(2) .5642(2) .0274(5) Uani d . 1 . . O O2 .30289(9) .0089(3) .4862(2) .0316(6) Uani d . 1 . . O N1 .37166(10) -.0895(3) .3277(2) .0260(6) Uani d . 1 . . N H1C .3760 -.0462 .2395 .031 Uiso calc R 1 . . H C1 .36857(13) .2228(3) .3826(3) .0303(7) Uani d . 1 . . C H1A .4116 .2389 .3575 .036 Uiso calc R 1 . . H H1B .3361 .2331 .2930 .036 Uiso calc R 1 . . H C2 .35697(13) .3458(4) .4873(3) .0310(7) Uani d . 1 . . C H2A .3134 .3649 .4947 .037 Uiso calc R 1 . . H C3 .40050(15) .4301(4) .5700(4) .0393(8) Uani d . 1 . . C H3A .4448 .4156 .5668 .047 Uiso calc R 1 . . H H3B .3879 .5058 .6332 .047 Uiso calc R 1 . . H C4 .43536(13) -.1462(4) .5535(3) .0299(7) Uani d . 1 . . C H4A .4052 -.2148 .5935 .036 Uiso calc R 1 . . H H4B .4795 -.1657 .6065 .036 Uiso calc R 1 . . H C5 .43104(12) -.1760(4) .3935(3) .0273(7) Uani d . 1 . . C H5A .4692 -.1344 .3591 .033 Uiso calc R 1 . . H H5B .4269 -.2893 .3713 .033 Uiso calc R 1 . . H C6 .26518(13) -.0741(4) .3716(3) .0336(8) Uani d . 1 . . C H6A .2446 -.0010 .2955 .040 Uiso calc R 1 . . H H6B .2312 -.1346 .4067 .040 Uiso calc R 1 . . H C7 .31068(12) -.1828(4) .3135(3) .0283(7) Uani d . 1 . . C H7A .3176 -.2803 .3710 .034 Uiso calc R 1 . . H H7B .2940 -.2099 .2114 .034 Uiso calc R 1 . . H B1 .36479(14) .0496(4) .4468(4) .0271(8) Uani d . 1 . . B 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 O1 .0306(10) .0247(12) .0270(11) .0029(8) .0056(8) -.0009(9) O2 .0298(11) .0362(13) .0306(12) -.0033(8) .0099(8) -.0060(10) N1 .0287(12) .0253(15) .0251(14) .0000(10) .0078(9) -.0003(10) C1 .0314(15) .0296(18) .0311(17) .0050(12) .0092(12) .0019(14) C2 .0350(15) .0248(17) .0345(17) .0033(13) .0100(12) .0026(14) C3 .0457(18) .0278(19) .046(2) .0017(14) .0117(15) .0001(15) C4 .0326(15) .0269(18) .0299(17) .0027(12) .0052(12) -.0012(13) C5 .0242(14) .0276(17) .0308(16) .0028(12) .0071(11) -.0015(13) C6 .0314(15) .0363(19) .0336(18) -.0003(13) .0073(12) -.0041(14) C7 .0316(14) .0257(17) .0284(16) -.0032(12) .0079(11) -.0021(12) B1 .0271(17) .028(2) .0261(18) .0007(13) .0046(13) -.0061(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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_publ_flag C4 O1 B1 108.4(2) ? C6 O2 B1 109.3(2) ? C5 N1 C7 114.8(2) ? C5 N1 B1 104.16(19) ? C7 N1 B1 105.11(19) ? C5 N1 H1C 110.8 ? C7 N1 H1C 110.8 ? B1 N1 H1C 110.8 ? C2 C1 B1 112.0(2) ? C2 C1 H1A 109.2 ? B1 C1 H1A 109.2 ? C2 C1 H1B 109.2 ? B1 C1 H1B 109.2 ? H1A C1 H1B 107.9 ? C3 C2 C1 126.8(3) ? C3 C2 H2A 116.6 ? C1 C2 H2A 116.6 ? C2 C3 H3A 120.0 ? C2 C3 H3B 120.0 ? H3A C3 H3B 120.0 ? O1 C4 C5 105.2(2) ? O1 C4 H4A 110.7 ? C5 C4 H4A 110.7 ? O1 C4 H4B 110.7 ? C5 C4 H4B 110.7 ? H4A C4 H4B 108.8 ? N1 C5 C4 102.9(2) ? N1 C5 H5A 111.2 ? C4 C5 H5A 111.2 ? N1 C5 H5B 111.2 ? C4 C5 H5B 111.2 ? H5A C5 H5B 109.1 ? O2 C6 C7 106.1(2) ? O2 C6 H6A 110.5 ? C7 C6 H6A 110.5 ? O2 C6 H6B 110.5 ? C7 C6 H6B 110.5 ? H6A C6 H6B 108.7 ? N1 C7 C6 103.6(2) ? N1 C7 H7A 111.0 ? C6 C7 H7A 111.0 ? N1 C7 H7B 111.0 ? C6 C7 H7B 111.0 ? H7A C7 H7B 109.0 ? O1 B1 O2 111.3(2) y O1 B1 C1 113.0(2) ? O2 B1 C1 115.0(2) ? O1 B1 N1 102.2(2) y O2 B1 N1 101.2(2) y C1 B1 N1 112.8(2) y 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 O1 C4 . 1.424(4) ? O1 B1 . 1.463(4) y O2 C6 . 1.411(3) ? O2 B1 . 1.466(4) y N1 C5 . 1.491(3) ? N1 C7 . 1.501(3) ? N1 B1 . 1.659(4) y N1 H1C . .9300 ? C1 C2 . 1.492(4) ? C1 B1 . 1.606(4) y C1 H1A . .9900 ? C1 H1B . .9900 ? C2 C3 . 1.308(4) ? C2 H2A . .9500 ? C3 H3A . .9500 ? C3 H3B . .9500 ? C4 C5 . 1.515(4) ? C4 H4A . .9900 ? C4 H4B . .9900 ? C5 H5A . .9900 ? C5 H5B . .9900 ? C6 C7 . 1.510(4) ? C6 H6A . .9900 ? C6 H6B . .9900 ? C7 H7A . .9900 ? C7 H7B . .9900 ? 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 N1 H1C O1 6 .93 2.04 2.907(3) 155.4