#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204923.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_2204923 loop_ _publ_author_name 'Zhang, Hui' 'Fang, Liang' _publ_section_title ; Dichlorotetrapyridinenickel(II) 0.76-hydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m180 _journal_page_last m182 _journal_paper_doi 10.1107/S1600536804033586 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Ni Cl2 (C5 H5 N)4] , 0.76H2 O' _chemical_formula_moiety 'C20 H20 Cl2 N4 Ni , 0.76H2 O' _chemical_formula_sum 'C20 H21.52 Cl2 N4 Ni O0.76' _chemical_formula_weight 459.68 _chemical_name_systematic ; Dichlorotetrapyridinenickel(II) 0.76-hydrate ; _space_group_IT_number 142 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4bd 2c' _symmetry_space_group_name_H-M 'I 41/a c d :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 15.815(6) _cell_length_b 15.815(6) _cell_length_c 16.773(9) _cell_measurement_reflns_used 26814 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 28.43 _cell_measurement_theta_min 2.58 _cell_volume 4195(3) _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_molecular_graphics 'PLATON (Spek, 2003) and ATOMS (Dowty, 2002)' _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \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 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26814 _diffrn_reflns_theta_full 28.43 _diffrn_reflns_theta_max 28.43 _diffrn_reflns_theta_min 2.58 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 1900.8 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.189 _refine_diff_density_min -0.251 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 72 _refine_ls_number_reflns 1324 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.831 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0220 _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^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0485 _reflns_number_gt 860 _reflns_number_total 1324 _reflns_threshold_expression I>2\s(I) _cod_data_source_file lh6331.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'I 41/a c d' _cod_original_formula_sum 'C20 H21.52 Cl2 N4 Ni O0.76 ' _cod_database_code 2204923 _cod_database_fobs_code 2204923 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' 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 Ni1 0.5000 0.2500 0.8750 0.01753(9) Uani d S 1 Ni Cl1 0.39171(2) 0.35829(2) 0.8750 0.02491(12) Uani d S 1 Cl O1 0.2500 0.1001(3) 0.5000 0.0339(11) Uani d SP 0.38 O H1 0.280(3) 0.128(3) 0.464(3) 0.076(19) Uiso d P 0.38 H N1 0.43412(7) 0.18264(7) 0.78621(6) 0.0203(2) Uani d . 1 N C2 0.47463(10) 0.14468(10) 0.72598(8) 0.0257(4) Uani d . 1 C H2 0.5345 0.1488 0.7235 0.031 Uiso calc R 1 H C3 0.43294(11) 0.09986(10) 0.66740(9) 0.0322(4) Uani d . 1 C H3 0.4637 0.0739 0.6253 0.039 Uiso calc R 1 H C4 0.34681(11) 0.09319(10) 0.67057(9) 0.0344(4) Uani d . 1 C H4 0.3169 0.0624 0.6309 0.041 Uiso calc R 1 H C5 0.30423(10) 0.13175(10) 0.73208(9) 0.0297(4) Uani d . 1 C H5 0.2444 0.1280 0.7358 0.036 Uiso calc R 1 H C6 0.34981(9) 0.17583(9) 0.78796(9) 0.0235(3) Uani d . 1 C H6 0.3200 0.2029 0.8300 0.028 Uiso calc R 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 0.01897(12) 0.01897(12) 0.01466(16) -0.00102(16) 0.000 0.000 Cl1 0.02456(17) 0.02456(17) 0.0256(3) 0.0045(2) -0.00158(19) -0.00158(19) O1 0.037(3) 0.032(3) 0.033(3) 0.000 0.009(2) 0.000 N1 0.0211(7) 0.0215(7) 0.0184(6) -0.0009(5) 0.0003(5) -0.0006(5) C2 0.0271(8) 0.0281(8) 0.0219(8) -0.0012(7) 0.0050(6) -0.0029(7) C3 0.0410(10) 0.0316(9) 0.0239(9) -0.0045(8) 0.0044(8) -0.0100(7) C4 0.0432(11) 0.0355(11) 0.0245(8) -0.0140(7) -0.0062(8) -0.0055(8) C5 0.0275(9) 0.0334(9) 0.0280(9) -0.0072(8) -0.0043(7) 0.0027(7) C6 0.0232(8) 0.0258(8) 0.0215(8) -0.0012(7) 0.0019(7) 0.0015(7) 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 N1 Ni1 N1 . 16_556 179.10(7) yes N1 Ni1 N1 . 7_546 89.98(7) yes N1 Ni1 N1 16_556 7_546 90.03(7) ? N1 Ni1 N1 . 10_554 90.03(7) yes N1 Ni1 N1 16_556 10_554 89.98(7) ? N1 Ni1 N1 7_546 10_554 179.10(7) ? N1 Ni1 Cl1 . . 90.45(3) yes N1 Ni1 Cl1 16_556 . 90.45(3) ? N1 Ni1 Cl1 7_546 . 89.55(3) yes N1 Ni1 Cl1 10_554 . 89.55(3) ? N1 Ni1 Cl1 . 10_554 89.55(3) ? N1 Ni1 Cl1 16_556 10_554 89.55(3) ? N1 Ni1 Cl1 7_546 10_554 90.45(3) ? N1 Ni1 Cl1 10_554 10_554 90.45(3) ? Cl1 Ni1 Cl1 . 10_554 180.0 yes C6 N1 C2 . . 117.23(12) ? C6 N1 Ni1 . . 121.20(9) ? C2 N1 Ni1 . . 121.58(10) ? N1 C2 C3 . . 122.64(15) ? N1 C2 H2 . . 118.7 ? C3 C2 H2 . . 118.7 ? C4 C3 C2 . . 119.22(15) ? C4 C3 H3 . . 120.4 ? C2 C3 H3 . . 120.4 ? C3 C4 C5 . . 118.87(14) ? C3 C4 H4 . . 120.6 ? C5 C4 H4 . . 120.6 ? C6 C5 C4 . . 118.73(14) ? C6 C5 H5 . . 120.6 ? C4 C5 H5 . . 120.6 ? N1 C6 C5 . . 123.31(14) ? N1 C6 H6 . . 118.3 ? C5 C6 H6 . . 118.3 ? 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 N1 . 2.1067(13) yes Ni1 N1 16_556 2.1067(13) ? Ni1 N1 7_546 2.1067(13) ? Ni1 N1 10_554 2.1067(13) ? Ni1 Cl1 . 2.4219(10) yes Ni1 Cl1 10_554 2.4219(10) ? O1 H1 . 0.89(5) yes N1 C6 . 1.3380(18) ? N1 C2 . 1.3384(18) ? C2 C3 . 1.379(2) ? C2 H2 . 0.9500 ? C3 C4 . 1.367(2) ? C3 H3 . 0.9500 ? C4 C5 . 1.375(2) ? C4 H4 . 0.9500 ? C5 C6 . 1.373(2) ? C5 H5 . 0.9500 ? C6 H6 . 0.9500 ? 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 _geom_hbond_publ_flag O1 H1 Cl1 20_657 0.89(5) 2.32(5) 3.1388(14) 153(4) yes 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_site_symmetry_1 _geom_torsion N1 Ni1 N1 C6 10_554 -129.91(13) Cl1 Ni1 N1 C6 . -40.36(11) Cl1 Ni1 N1 C6 10_554 139.64(11) N1 Ni1 N1 C2 7_546 -130.56(13) N1 Ni1 N1 C2 10_554 50.34(10) Cl1 Ni1 N1 C2 . 139.89(11) Cl1 Ni1 N1 C2 10_554 -40.11(11) C6 N1 C2 C3 . -0.1(2) Ni1 N1 C2 C3 . 179.65(12) N1 C2 C3 C4 . -0.3(3) C2 C3 C4 C5 . 0.2(3) C3 C4 C5 C6 . 0.2(2) C2 N1 C6 C5 . 0.6(2) Ni1 N1 C6 C5 . -179.14(11) C4 C5 C6 N1 . -0.7(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139067329