#------------------------------------------------------------------------------ #$Date: 2017-06-19 10:02:37 +0100 (Mon, 19 Jun 2017) $ #$Revision: 197922 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202311.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_2202311 loop_ _publ_author_name 'Shiu, Kom-Bei' 'Yen, Chia-Hung' 'Liao, Fen-Ling' 'Wang, Sue-Lein' _publ_section_title ; trans-Diaquatetrakis(imidazole)nickel(II) dichloride ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1189 _journal_page_last m1191 _journal_paper_doi 10.1107/S1600536803026886 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Ni (C3 H4 N2)4 (H2 O)2] Cl2' _chemical_formula_moiety 'C12 H20 N8 Ni O2 2+, 2Cl 1-' _chemical_formula_sum 'C12 H20 Cl2 N8 Ni O2' _chemical_formula_weight 437.97 _chemical_name_systematic ; trans-Diaquatetrakis(imidazole)nickel(II) dichloride ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 107.323(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.4020(12) _cell_length_b 10.9759(11) _cell_length_c 14.2847(14) _cell_measurement_reflns_used 2924 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2.5 _cell_volume 1856.3(3) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5720 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_min 2.53 _exptl_absorpt_coefficient_mu 1.357 _exptl_absorpt_correction_T_max 0.81731 _exptl_absorpt_correction_T_min 0.77428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1995)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.567 _exptl_crystal_description Equant _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.311 _refine_diff_density_min -0.209 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 2231 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0267 _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^)+(0.032P)^2^+0.0266P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.0626 _reflns_number_gt 1833 _reflns_number_total 2231 _reflns_threshold_expression I>2\s(I) _cod_data_source_file br6126.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 A spurious symmop was removed from the symmop list miguel ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2202311 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' '1/2-x, 1/2-y, -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 Ni1 0.2500 0.7500 0.0000 0.02385(9) Uani d S 1 . . Ni Cl1 0.09150(4) 0.34790(4) -0.07166(3) 0.04217(13) Uani d . 1 . . Cl O1 0.11950(10) 0.62207(10) -0.00434(9) 0.0373(3) Uani d . 1 . . O N1 0.25806(11) 0.79631(12) 0.14688(9) 0.0286(3) Uani d . 1 . . N N2 0.23508(14) 0.78228(15) 0.29349(11) 0.0426(4) Uani d . 1 . . N N3 0.37191(11) 0.61853(12) 0.05610(9) 0.0288(3) Uani d . 1 . . N N4 0.45838(13) 0.44308(13) 0.09409(11) 0.0407(4) Uani d . 1 . . N C1 0.32034(15) 0.88534(16) 0.20717(12) 0.0365(4) Uani d . 1 . . C C2 0.30663(16) 0.87751(17) 0.29753(12) 0.0425(4) Uani d . 1 . . C C3 0.20776(16) 0.73593(16) 0.20240(13) 0.0384(4) Uani d . 1 . . C C4 0.47786(15) 0.63682(16) 0.12175(13) 0.0381(4) Uani d . 1 . . C C5 0.53151(15) 0.52949(18) 0.14486(13) 0.0446(5) Uani d . 1 . . C C6 0.36447(15) 0.50011(16) 0.04152(13) 0.0368(4) Uani d . 1 . . C H1A 0.1152 0.5484 -0.0213 0.050 Uiso d . 1 . . H H1B 0.0568 0.6360 0.0090 0.050 Uiso d . 1 . . H H1C 0.3663 0.9390 0.1844 0.050 Uiso d . 1 . . H H2A 0.2082 0.7522 0.3394 0.050 Uiso d . 1 . . H H2B 0.3374 0.9243 0.3558 0.050 Uiso d . 1 . . H H3A 0.1544 0.6723 0.1810 0.050 Uiso d . 1 . . H H4A 0.4691 0.3600 0.0980 0.050 Uiso d . 1 . . H H4B 0.5013 0.7203 0.1446 0.050 Uiso d . 1 . . H H5A 0.5994 0.5079 0.1931 0.050 Uiso d . 1 . . H H6A 0.3006 0.4574 -0.0046 0.050 Uiso 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 Ni1 0.02701(15) 0.02001(14) 0.02788(15) 0.00003(11) 0.01330(11) -0.00110(11) Cl1 0.0441(3) 0.0316(2) 0.0606(3) -0.00807(19) 0.0306(2) -0.0128(2) O1 0.0367(6) 0.0265(6) 0.0578(7) -0.0064(5) 0.0282(5) -0.0092(6) N1 0.0333(7) 0.0258(7) 0.0298(7) 0.0019(6) 0.0141(6) -0.0009(6) N2 0.0547(10) 0.0481(9) 0.0319(8) 0.0031(8) 0.0232(7) 0.0063(7) N3 0.0318(7) 0.0237(7) 0.0334(7) 0.0015(5) 0.0135(6) -0.0016(6) N4 0.0460(9) 0.0246(8) 0.0564(9) 0.0097(7) 0.0227(7) 0.0054(7) C1 0.0409(10) 0.0363(9) 0.0343(9) -0.0051(8) 0.0145(7) -0.0011(8) C2 0.0528(11) 0.0453(11) 0.0279(9) 0.0007(9) 0.0098(8) -0.0052(8) C3 0.0452(10) 0.0373(10) 0.0377(9) -0.0052(8) 0.0198(8) -0.0008(7) C4 0.0382(9) 0.0342(10) 0.0390(9) 0.0016(8) 0.0071(7) -0.0046(8) C5 0.0412(10) 0.0462(12) 0.0431(10) 0.0123(9) 0.0072(8) 0.0027(9) C6 0.0347(9) 0.0279(9) 0.0503(10) -0.0015(7) 0.0163(8) -0.0052(8) 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 '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_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 Ni1 N3 7_565 . 180.0 ? N3 Ni1 O1 7_565 . 89.27(5) ? N3 Ni1 O1 . . 90.73(5) yes N3 Ni1 O1 7_565 7_565 90.73(5) ? N3 Ni1 O1 . 7_565 89.27(5) ? O1 Ni1 O1 . 7_565 180.0 ? N3 Ni1 N1 7_565 . 91.70(5) ? N3 Ni1 N1 . . 88.30(5) yes O1 Ni1 N1 . . 89.91(5) yes O1 Ni1 N1 7_565 . 90.09(5) ? N3 Ni1 N1 7_565 7_565 88.30(5) ? N3 Ni1 N1 . 7_565 91.70(5) ? O1 Ni1 N1 . 7_565 90.09(5) ? O1 Ni1 N1 7_565 7_565 89.91(5) ? N1 Ni1 N1 . 7_565 180.0 ? Ni1 O1 H1A . . 128.7 ? Ni1 O1 H1B . . 126.9 ? H1A O1 H1B . . 104.4 ? C3 N1 C1 . . 104.90(13) ? C3 N1 Ni1 . . 125.30(11) ? C1 N1 Ni1 . . 129.62(10) ? C3 N2 C2 . . 107.76(14) ? C3 N2 H2A . . 122.4 ? C2 N2 H2A . . 129.9 ? C6 N3 C4 . . 104.98(14) ? C6 N3 Ni1 . . 128.21(12) ? C4 N3 Ni1 . . 126.73(11) ? C6 N4 C5 . . 107.65(14) ? C6 N4 H4A . . 125.7 ? C5 N4 H4A . . 126.6 ? C2 C1 N1 . . 110.17(15) ? C2 C1 H1C . . 129.0 ? N1 C1 H1C . . 120.8 ? C1 C2 N2 . . 105.88(15) ? C1 C2 H2B . . 131.7 ? N2 C2 H2B . . 122.4 ? N1 C3 N2 . . 111.27(15) ? N1 C3 H3A . . 125.7 ? N2 C3 H3A . . 122.8 ? C5 C4 N3 . . 109.88(15) ? C5 C4 H4B . . 131.0 ? N3 C4 H4B . . 119.1 ? C4 C5 N4 . . 106.07(15) ? C4 C5 H5A . . 131.8 ? N4 C5 H5A . . 121.4 ? N3 C6 N4 . . 111.41(15) ? N3 C6 H6A . . 125.5 ? N4 C6 H6A . . 123.0 ? 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 Ni1 N3 7_565 2.0709(13) ? Ni1 N3 . 2.0709(13) yes Ni1 O1 . 2.1296(11) yes Ni1 O1 7_565 2.1296(11) ? Ni1 N1 . 2.1321(12) yes Ni1 N1 7_565 2.1321(12) ? O1 H1A . 0.8413 ? O1 H1B . 0.8675 ? N1 C3 . 1.324(2) ? N1 C1 . 1.377(2) ? N2 C3 . 1.343(2) ? N2 C2 . 1.361(2) ? N2 H2A . 0.8834 ? N3 C6 . 1.315(2) ? N3 C4 . 1.383(2) ? N4 C6 . 1.338(2) ? N4 C5 . 1.363(2) ? N4 H4A . 0.9208 ? C1 C2 . 1.354(2) ? C1 H1C . 0.9424 ? C2 H2B . 0.9556 ? C3 H3A . 0.9480 ? C4 C5 . 1.345(2) ? C4 H4B . 0.9870 ? C5 H5A . 0.9458 ? C6 H6A . 0.9851 ? 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 O1 H1A Cl1 . 0.84 2.31 3.1470(10) 176 O1 H1B Cl1 5_565 0.87 2.28 3.135(2) 169 C1 H1C Cl1 7_565 0.94 2.97 3.844(2) 154 N2 H2A Cl1 6_566 0.88 2.45 3.311(3) 165 C3 H3A Cl1 5_565 0.95 2.99 3.739(4) 136 N4 H4A Cl1 7 0.92 2.40 3.251(2) 154 C6 H6A Cl1 . 0.99 2.76 3.689(3) 158