#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2010679.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_2010679 loop_ _publ_author_name 'Hensen, Karl' 'Spangenberg, Bj\"orn' 'Bolte, Michael' _publ_section_title ; Two phenanthroline hydrochlorides ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 208 _journal_page_last 210 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C12 H9 N2+ , Cl- ' _chemical_formula_sum 'C12 H9 Cl N2' _chemical_formula_weight 216.66 _chemical_name_systematic ; ? ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 96.91(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.8770(10) _cell_length_b 9.7870(10) _cell_length_c 15.547(2) _cell_measurement_reflns_used 1982 _cell_measurement_temperature 173 _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 1.00 _cell_volume 1038.8(2) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'XP (Siemens, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173 _diffrn_measured_fraction_theta_full .920 _diffrn_measured_fraction_theta_max .920 _diffrn_measurement_device 'Siemens CCD three circle diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'highly oriented graphite crystal' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0834 _diffrn_reflns_av_sigmaI/netI .0851 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 7686 _diffrn_reflns_theta_full 26.03 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_min 2.46 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 720 _diffrn_standards_number 53 _exptl_absorpt_coefficient_mu .331 _exptl_absorpt_correction_T_max .9676 _exptl_absorpt_correction_T_min .9217 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_meas N/A _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 448 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _refine_diff_density_max .564 _refine_diff_density_min -.306 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 140 _refine_ls_number_reflns 1884 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all .1377 _refine_ls_R_factor_gt .0679 _refine_ls_R_factor_obs .0679 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.6383P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .1498 _refine_ls_wR_factor_obs .1247 _refine_ls_wR_factor_ref .1498 _reflns_number_gt 1093 _reflns_number_total 1884 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1328.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _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. '_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical' 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 2010679 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_type_symbol Cl1 .31541(18) .05264(11) .37599(6) .0564(4) Uani d . 1 Cl N1 .2924(4) .2822(3) .5009(2) .0342(8) Uani d . 1 N H1 .275(6) .239(4) .446(3) .066(14) Uiso d . 1 H C2 .3453(6) .2038(5) .5697(2) .0453(11) Uani d . 1 C H2 .3623 .1082 .5630 .054 Uiso calc R 1 H C3 .3757(6) .2635(5) .6517(3) .0505(13) Uani d . 1 C H3 .4105 .2082 .7014 .061 Uiso calc R 1 H C4 .3556(6) .4011(6) .6606(3) .0519(13) Uani d . 1 C H4 .3772 .4416 .7164 .062 Uiso calc R 1 H C5 .3034(5) .4829(5) .5880(3) .0418(11) Uani d . 1 C C6 .2845(6) .6278(5) .5927(3) .0550(13) Uani d . 1 C H6 .3078 .6723 .6473 .066 Uiso calc R 1 H C7 .2336(6) .7028(5) .5202(3) .0538(13) Uani d . 1 C H7 .2233 .7992 .5249 .065 Uiso calc R 1 H C8 .1953(5) .6404(4) .4376(3) .0406(11) Uani d . 1 C C9 .1382(6) .7142(4) .3612(3) .0499(12) Uani d . 1 C H9 .1261 .8108 .3631 .060 Uiso calc R 1 H C10 .1003(6) .6471(4) .2845(3) .0467(12) Uani d . 1 C H10 .0577 .6955 .2328 .056 Uiso calc R 1 H C11 .1253(5) .5058(4) .2833(3) .0407(11) Uani d . 1 C H11 .1008 .4606 .2290 .049 Uiso calc R 1 H N12 .1805(4) .4303(3) .35232(19) .0358(8) Uani d . 1 N C13 .2125(5) .4983(4) .4292(2) .0320(9) Uani d . 1 C C14 .2694(5) .4212(4) .5061(2) .0340(10) Uani d . 1 C 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 Cl1 .0929(10) .0341(6) .0378(6) .0029(6) -.0099(5) -.0012(6) N1 .032(2) .039(2) .0319(19) -.0022(16) .0022(15) -.0001(17) C2 .041(3) .056(3) .039(2) -.006(2) .0047(19) .010(2) C3 .033(3) .084(4) .034(2) -.010(3) .0010(18) .010(3) C4 .035(3) .084(4) .036(2) -.011(2) .0046(19) -.017(2) C5 .024(2) .061(3) .040(3) -.010(2) .0049(18) -.018(2) C6 .035(3) .067(4) .064(3) -.010(3) .011(2) -.035(3) C7 .037(3) .040(3) .084(4) -.004(2) .010(3) -.031(3) C8 .026(2) .033(3) .064(3) -.0056(19) .010(2) -.012(2) C9 .031(3) .031(3) .088(4) -.004(2) .006(2) -.001(3) C10 .035(3) .037(3) .067(3) -.001(2) .002(2) .020(2) C11 .036(2) .036(3) .049(3) -.0033(19) .001(2) .001(2) N12 .0335(19) .037(2) .0369(18) -.0010(16) .0038(15) .0051(17) C13 .023(2) .033(2) .040(2) -.0038(17) .0029(17) -.0046(18) C14 .019(2) .039(3) .045(2) -.0046(18) .0085(17) -.009(2) 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' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 '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 C2 N1 C14 123.1(4) y N1 C2 C3 119.3(4) ? C4 C3 C2 120.0(4) ? C3 C4 C5 120.3(4) ? C4 C5 C14 119.0(4) ? C4 C5 C6 123.1(4) ? C14 C5 C6 117.9(4) ? C7 C6 C5 120.8(4) ? C6 C7 C8 121.4(4) ? C13 C8 C9 116.6(4) ? C13 C8 C7 120.2(4) ? C9 C8 C7 123.2(4) ? C10 C9 C8 119.9(4) ? C9 C10 C11 118.8(4) ? N12 C11 C10 124.6(4) ? C11 N12 C13 116.1(3) y N12 C13 C8 124.0(4) ? N12 C13 C14 118.4(3) ? C8 C13 C14 117.6(4) ? N1 C14 C5 118.2(4) ? N1 C14 C13 119.7(3) ? C5 C14 C13 122.1(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.331(5) y N1 C14 1.373(5) y C2 C3 1.395(6) ? C3 C4 1.363(6) ? C4 C5 1.394(6) ? C5 C14 1.404(5) ? C5 C6 1.427(6) ? C6 C7 1.355(6) ? C7 C8 1.418(5) ? C8 C13 1.404(5) ? C8 C9 1.405(6) ? C9 C10 1.358(6) ? C10 C11 1.394(6) ? C11 N12 1.321(5) y N12 C13 1.362(5) y C13 C14 1.428(5) ? 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 H1 Cl1 . .95(4) 2.16(4) 2.986(4) 145(4) C2 H2 Cl1 3_656 .95 2.79 3.462(4) 128.4 C4 H4 Cl1 4_566 .95 2.57 3.424(4) 150.1 C9 H9 Cl1 1_565 .95 2.70 3.527(4) 146.4 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C14 N1 C2 C3 1.3(6) N1 C2 C3 C4 -1.5(6) C2 C3 C4 C5 .4(6) C3 C4 C5 C14 .9(6) C3 C4 C5 C6 -178.5(4) C4 C5 C6 C7 179.9(4) C14 C5 C6 C7 .5(6) C5 C6 C7 C8 .7(6) C6 C7 C8 C13 -.9(6) C6 C7 C8 C9 178.6(4) C13 C8 C9 C10 .9(6) C7 C8 C9 C10 -178.7(4) C8 C9 C10 C11 -2.0(6) C9 C10 C11 N12 1.3(6) C10 C11 N12 C13 .6(5) C11 N12 C13 C8 -1.8(5) C11 N12 C13 C14 179.0(3) C9 C8 C13 N12 1.1(6) C7 C8 C13 N12 -179.3(3) C9 C8 C13 C14 -179.7(3) C7 C8 C13 C14 -.1(5) C2 N1 C14 C5 .0(5) C2 N1 C14 C13 179.9(3) C4 C5 C14 N1 -1.1(5) C6 C5 C14 N1 178.3(3) C4 C5 C14 C13 179.0(4) C6 C5 C14 C13 -1.6(5) N12 C13 C14 N1 .7(5) C8 C13 C14 N1 -178.6(3) N12 C13 C14 C5 -179.4(3) C8 C13 C14 C5 1.4(5)