#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/48/2004809.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_2004809 loop_ _publ_author_name 'Jones, R. A.' 'Powell, A. K.' 'Whitmore, A. P.' _publ_section_title ; Identification of the N-Alkylation Product of 3-(2-Pyrrolyl)pyridazine ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1002 _journal_page_last 1003 _journal_paper_doi 10.1107/S0108270195015307 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'C10 H12 N3 , B F4' _chemical_formula_sum 'C10 H12 B F4 N3' _chemical_formula_weight 261.0 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source 'SHELXTL-Plus (Sheldrick, 1991)' _cell_angle_alpha 90 _cell_angle_beta 105.85(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.232(2) _cell_length_b 11.599(3) _cell_length_c 12.996(4) _cell_measurement_reflns_used 20 _cell_measurement_temperature 295 _cell_measurement_theta_max 15 _cell_measurement_theta_min 5 _cell_volume 1193.7(6) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2392 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% none _diffrn_standards_interval_count 50 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.452 _exptl_crystal_description prism _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.34 _refine_diff_density_min -0.27 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.17 _refine_ls_hydrogen_treatment 'H atoms located by difference synthesis and refined isotropically' _refine_ls_number_parameters 199 _refine_ls_number_reflns 1615 _refine_ls_R_factor_obs 0.061 _refine_ls_shift/esd_max 0.002 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+0.0070F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.105 _reflns_number_observed 1615 _reflns_number_total 2108 _reflns_observed_criterion F>4.0\s(F) _[local]_cod_data_source_file pt1023.cif _[local]_cod_data_source_block pt1023a _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value ' 1/[\s^2^(F)+0.0070F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)+0.0070F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1193.8 _cod_database_code 2004809 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C(1) .1739(3) .0863(2) .9600(2) .0460(10) C(2) .3011(4) .0208(3) 1.0287(2) .0570(10) C(3) .4164(4) .0746(3) 1.1074(3) .0660(10) C(4) .4056(4) .1915(3) 1.1164(2) .0660(10) C(5) .0467(3) .0346(2) .8742(2) .0490(10) C(6) .0305(4) -.0777(3) .8368(2) .0580(10) C(7) -0.1139(4) -.0826(3) .7517(3) .0680(10) C(8) -0.1823(4) .0247(3) .7374(2) .0660(10) C(9) .2628(5) .3753(3) 1.0589(3) .0700(10) C(10) .1409(7) .4014(3) 1.1183(4) .105(2) N(1) .2828(3) .2488(2) 1.0498(2) .0540(10) N(2) .1647(3) .2003(2) .9710(2) .0490(10) N(3) -.0853(3) .0954(2) .8124(2) .0570(10) B(1) .6048(4) .2063(3) .4014(3) .0540(10) F(1) .5199(3) .1057(2) .3894(2) .1070(10) F(2) .4931(3) .2943(2) .3656(2) .0940(10) F(3) .7145(3) .2028(2) .3405(2) .1080(10) F(4) .6862(4) .2260(3) .5052(2) .1170(10) H(2) .310(5) -.063(4) 1.022(3) .080 H(3A) -0.117(6) .163(4) .817(3) .080 H(3B) .509(5) .031(4) 1.162(3) .080 H(4) .459(5) .241(4) 1.166(3) .080 H(6) .112(5) -0.138(4) .864(3) .080 H(7) -0.155(5) -0.136(4) .716(3) .080 H(8) -0.277(5) .043(4) .687(3) .080 H(9A) .375(5) .413(3) 1.096(3) .080 H(9B) .223(6) .406(3) .979(4) .080 H(10A) .142(5) .480(4) 1.124(3) .080 H(10B) .042(6) .367(4) 1.109(3) .080 H(10C) .204(5) .366(4) 1.196(3) .080 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 C(1) N(2) N(1) 116.8(2) yes N(2) N(1) C(4) 124.1(2) yes N(1) C(4) C(3) 120.1(3) yes C(4) C(3) C(2) 118.5(3) yes C(3) C(2) C(1) 118.9(3) yes C(2) C(1) N(2) 121.6(2) yes N(2) C(1) C(5) 116.5(2) yes C(1) C(5) C(6) 130.2(2) yes C(5) C(6) C(7) 107.3(3) yes C(6) C(7) C(8) 107.8(3) yes C(7) C(8) N(3) 108.4(2) yes C(8) N(3) C(5) 109.3(2) yes N(3) C(5) C(6) 107.2(2) yes N(2) N(1) C(9) 114.0(2) yes N(1) C(9) C(10) 110.8(3) yes F(1) B(1) F(2) 109.1(3) yes F(1) B(1) F(3) 108.4(3) yes F(1) B(1) F(4) 111.2(3) yes F(2) B(1) F(3) 108.5(3) yes F(2) B(1) F(4) 108.4(3) yes F(3) B(1) F(4) 111.1(3) yes C(2) C(1) C(5) 121.9(2) no C(1) C(5) N(3) 122.6(2) no C(4) N(1) C(9) 121.9(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C(1) N(2) 1.335(3) yes N(1) N(2) 1.330(3) yes N(1) C(4) 1.318(4) yes C(4) C(3) 1.366(5) yes C(3) C(2) 1.345(4) yes C(2) C(1) 1.400(4) yes C(1) C(5) 1.435(3) yes C(5) C(6) 1.385(4) yes C(6) C(7) 1.386(5) yes C(7) C(8) 1.358(4) yes C(8) N(3) 1.355(4) yes N(3) C(5) 1.359(3) yes N(1) C(9) 1.484(4) yes C(9) C(10) 1.456(7) yes B(1) F(1) 1.347(4) yes B(1) F(2) 1.368(4) yes B(1) F(3) 1.354(5) yes B(1) F(4) 1.352(4) yes C(5) C(8) 2.213(4) no C(5) C(7) 2.232(4) no C(6) C(8) 2.216(4) no