#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/25/8102530.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_8102530 loop_ _publ_author_name 'Zheng-Jing Jiang' 'Guo-Dong Tang' 'Yu Zhang' 'Jian-Ying Zhao' 'Gang Wang' _publ_section_title ; Crystal structure of [3-(2-(N-1H-methylpyrrolidinyl))pyridine]zinc(II) trichloride, Zn(C10H15N2)Cl3 ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 577 _journal_volume 224 _journal_year 2009 _chemical_absolute_configuration trans _chemical_formula_moiety 'C10 H15 Cl3 N2 Zn' _chemical_formula_sum 'C10 H15 Cl3 N2 Zn' _chemical_formula_weight 334.96 _chemical_name_systematic ; trichlorido-3-(2-(N-1H-methylpyrrolidinyl)) pyridine-zinc(II), [ZnCl~3~[H-(Nicotine)]] ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.9228(9) _cell_length_b 11.6108(11) _cell_length_c 13.8766(14) _cell_measurement_reflns_used 2566 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.42 _cell_measurement_theta_min 2.13 _cell_volume 1437.6(2) _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXL97 _computing_publication_material 'SHELXL97 and PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker Smart Aepex II CCD ' _diffrn_measurement_method 'phi and omega scans' _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 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10323 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 2.29 _exptl_absorpt_coefficient_mu 2.242 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 680 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.237 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 156 _refine_ls_number_reflns 2747 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0253 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.0681 _reflns_number_gt 2566 _reflns_number_total 2747 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file 1267-2738.cff _[local]_cod_data_source_block 1 _cod_database_code 8102530 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5489(3) 0.4894(2) 0.34858(18) 0.0369(6) Uani 1 1 d . . . H1 H 0.5786 0.4149 0.3330 0.044 Uiso 1 1 calc R . . C2 C 0.4195(3) 0.5319(2) 0.30684(19) 0.0366(6) Uani 1 1 d . . . C3 C 0.3791(3) 0.6436(3) 0.3284(2) 0.0448(7) Uani 1 1 d . . . H3 H 0.2942 0.6762 0.3006 0.054 Uiso 1 1 calc R . . C4 C 0.4656(4) 0.7065(2) 0.3916(2) 0.0474(7) Uani 1 1 d . . . H4 H 0.4393 0.7817 0.4073 0.057 Uiso 1 1 calc R . . C5 C 0.5906(3) 0.6572(3) 0.4310(2) 0.0450(7) Uani 1 1 d . . . H5 H 0.6481 0.6999 0.4739 0.054 Uiso 1 1 calc R . . C6 C 0.3326(3) 0.4561(2) 0.23788(19) 0.0413(6) Uani 1 1 d . B . H6 H 0.3989 0.3935 0.2173 0.050 Uiso 1 1 calc R . . C7 C 0.0910(4) 0.3763(4) 0.2046(3) 0.0767(12) Uani 1 1 d . . . H7A H 0.0878 0.2938 0.1936 0.092 Uiso 1 1 calc R A 1 H7B H -0.0091 0.4020 0.2212 0.092 Uiso 1 1 calc R A 1 C8 C 0.1065(16) 0.489(2) 0.1429(13) 0.069(4) Uani 0.45(3) 1 d P B 2 H8A H 0.0741 0.4763 0.0770 0.083 Uiso 0.45(3) 1 calc PR B 2 H8B H 0.0485 0.5515 0.1705 0.083 Uiso 0.45(3) 1 calc PR B 2 C9 C 0.2697(4) 0.5141(4) 0.1472(2) 0.0655(10) Uani 1 1 d . . . H9A H 0.3442 0.5177 0.0963 0.079 Uiso 1 1 calc R B 1 H9B H 0.2339 0.5913 0.1609 0.079 Uiso 1 1 calc R B 1 C10 C 0.2335(5) 0.3050(4) 0.3488(4) 0.0938(16) Uani 1 1 d . . . H10A H 0.2857 0.2471 0.3126 0.141 Uiso 1 1 calc R B . H10B H 0.1427 0.2729 0.3745 0.141 Uiso 1 1 calc R . . H10C H 0.2959 0.3312 0.4007 0.141 Uiso 1 1 calc R . . C8' C 0.1400(12) 0.4330(16) 0.1202(7) 0.068(3) Uani 0.55(3) 1 d P B 1 H8'1 H 0.0582 0.4768 0.0924 0.081 Uiso 0.55(3) 1 calc PR B 1 H8'2 H 0.1736 0.3770 0.0731 0.081 Uiso 0.55(3) 1 calc PR B 1 Cl1 Cl 0.79696(9) 0.50752(8) 0.62768(5) 0.0556(2) Uani 1 1 d . . . Cl2 Cl 0.83532(11) 0.29986(7) 0.41448(7) 0.0641(2) Uani 1 1 d . . . Cl3 Cl 1.01623(9) 0.58968(6) 0.40956(6) 0.0510(2) Uani 1 1 d . . . N1 N 0.6333(3) 0.54912(18) 0.40975(16) 0.0370(5) Uani 1 1 d . . . N2 N 0.1968(3) 0.4027(2) 0.28519(18) 0.0420(5) Uani 1 1 d . B . H2 H 0.1533 0.4580 0.3223 0.050 Uiso 1 1 calc R . . Zn1 Zn 0.82536(3) 0.47919(3) 0.46971(2) 0.03941(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0390(14) 0.0373(14) 0.0345(14) -0.0034(12) 0.0035(10) 0.0031(11) C2 0.0360(14) 0.0393(14) 0.0344(14) 0.0000(13) 0.0015(11) -0.0004(12) C3 0.0367(15) 0.0419(15) 0.0558(19) 0.0060(15) 0.0047(13) 0.0030(12) C4 0.0506(19) 0.0313(13) 0.0603(19) -0.0047(13) 0.0106(15) 0.0016(13) C5 0.0470(18) 0.0428(16) 0.0453(17) -0.0064(14) 0.0043(13) -0.0082(14) C6 0.0355(15) 0.0466(16) 0.0419(15) -0.0020(12) -0.0012(12) 0.0060(14) C7 0.061(2) 0.095(3) 0.074(3) -0.027(3) -0.010(2) -0.025(2) C8 0.057(6) 0.097(11) 0.052(7) -0.008(7) -0.015(5) -0.003(6) C9 0.064(2) 0.084(3) 0.0483(18) 0.016(2) -0.0154(16) -0.001(2) C10 0.079(3) 0.064(2) 0.138(4) 0.054(3) 0.019(3) 0.006(2) C8' 0.047(5) 0.105(8) 0.051(5) -0.028(5) -0.018(3) 0.011(5) Cl1 0.0583(5) 0.0719(5) 0.0367(4) 0.0005(4) -0.0029(3) -0.0126(4) Cl2 0.0722(6) 0.0387(4) 0.0814(6) -0.0075(4) 0.0022(5) -0.0033(4) Cl3 0.0504(5) 0.0415(4) 0.0612(5) -0.0083(4) 0.0185(4) -0.0077(3) N1 0.0378(13) 0.0386(12) 0.0345(12) -0.0030(10) 0.0001(9) -0.0011(9) N2 0.0353(13) 0.0374(11) 0.0534(15) -0.0035(11) -0.0026(10) 0.0014(11) Zn1 0.03892(17) 0.04010(17) 0.03921(18) -0.00203(14) -0.00252(14) -0.00387(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.7(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C6 123.4(3) . . ? C1 C2 C6 119.0(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 122.3(3) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N2 C6 C2 112.0(2) . . ? N2 C6 C9 104.1(2) . . ? C2 C6 C9 116.8(3) . . ? N2 C6 H6 107.9 . . ? C2 C6 H6 107.9 . . ? C9 C6 H6 107.9 . . ? C8' C7 N2 109.2(4) . . ? C8' C7 C8 29.8(4) . . ? N2 C7 C8 100.4(6) . . ? C8' C7 H7A 109.8 . . ? N2 C7 H7A 109.8 . . ? C8 C7 H7A 137.7 . . ? C8' C7 H7B 109.8 . . ? N2 C7 H7B 109.8 . . ? C8 C7 H7B 87.4 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C7 103.2(9) . . ? C9 C8 H8A 111.1 . . ? C7 C8 H8A 111.1 . . ? C9 C8 H8B 111.1 . . ? C7 C8 H8B 111.1 . . ? H8A C8 H8B 109.1 . . ? C8 C9 C6 107.8(5) . . ? C8 C9 C8' 29.9(6) . . ? C6 C9 C8' 101.9(5) . . ? C8 C9 H9A 130.6 . . ? C6 C9 H9A 111.4 . . ? C8' C9 H9A 111.4 . . ? C8 C9 H9B 82.3 . . ? C6 C9 H9B 111.4 . . ? C8' C9 H9B 111.4 . . ? H9A C9 H9B 109.3 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8' C9 108.5(6) . . ? C7 C8' H8'1 110.0 . . ? C9 C8' H8'1 110.0 . . ? C7 C8' H8'2 110.0 . . ? C9 C8' H8'2 110.0 . . ? H8'1 C8' H8'2 108.4 . . ? C1 N1 C5 117.8(2) . . ? C1 N1 Zn1 121.38(17) . . ? C5 N1 Zn1 120.8(2) . . ? C10 N2 C7 115.5(3) . . ? C10 N2 C6 113.4(3) . . ? C7 N2 C6 105.4(2) . . ? C10 N2 H2 107.4 . . ? C7 N2 H2 107.4 . . ? C6 N2 H2 107.4 . . ? N1 Zn1 Cl2 105.19(7) . . ? N1 Zn1 Cl1 104.06(7) . . ? Cl2 Zn1 Cl1 118.81(4) . . ? N1 Zn1 Cl3 104.44(7) . . ? Cl2 Zn1 Cl3 111.70(3) . . ? Cl1 Zn1 Cl3 111.11(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.329(3) . ? C1 C2 1.383(4) . ? C1 H1 0.9300 . ? C2 C3 1.379(4) . ? C2 C6 1.514(4) . ? C3 C4 1.378(4) . ? C3 H3 0.9300 . ? C4 C5 1.368(4) . ? C4 H4 0.9300 . ? C5 N1 1.344(4) . ? C5 H5 0.9300 . ? C6 N2 1.511(4) . ? C6 C9 1.534(4) . ? C6 H6 0.9800 . ? C7 C8' 1.412(10) . ? C7 N2 1.496(4) . ? C7 C8 1.570(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.486(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C8' 1.538(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.475(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? Cl1 Zn1 2.2310(8) . ? Cl2 Zn1 2.2206(8) . ? Cl3 Zn1 2.2898(8) . ? N1 Zn1 2.071(2) . ? N2 H2 0.9100 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 Cl1 0.93 2.80 3.655(3) 153.4 4_466 C9 H9B Cl2 0.97 2.71 3.552(4) 145.5 3_655