#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/02/2200249.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_2200249 loop_ _publ_author_name 'Vald\'es-Mart\'inez, Jes\'us' 'Alstrum-Acevedo, James H.' 'Toscano, Rub\'en A.' 'Espinosa-P\'erez, Georgina' 'Helfrich, Brian A.' 'West, Douglas X.' _publ_section_title ; Bis(2-pyridiniomethyleneaminoguanidinium) trans-tetraaquadichloronickel(II) dichloride tetrahydrate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m137 _journal_page_last m139 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '(C7 H11 N4)2 [Ni (H2 O)4 Cl2] Cl2, 4H2 O' _chemical_formula_moiety '2C7 H11 N4 1+, 2Cl 1-, Cl2 H8 Ni1 O4, 4H2 O' _chemical_formula_sum 'C14 H38 Cl6 N10 Ni O8' _chemical_formula_weight 745.95 _chemical_name_common ; [2(Fopygu.2HCl)][trans-Ni(H2O)4Cl2]*4H2O ; _chemical_name_systematic ; Bis(2-pyridiniomethyleneaminoguanidinium) trans-tetraaquadichloronickel(II) dichloride tetrahydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.590(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 24.698(4) _cell_length_b 7.1060(10) _cell_length_c 18.538(2) _cell_measurement_reflns_used 33 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 2.5 _cell_volume 3208.0(8) _computing_cell_refinement 'P4 Software' _computing_data_collection 'P4 Software (Siemens, 1995)' _computing_data_reduction 'P4 Software' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .995 _diffrn_measured_fraction_theta_max .995 _diffrn_measurement_device_type 'Siemens P4/PC' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .046 _diffrn_reflns_av_sigmaI/netI .071 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 4547 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.7 _diffrn_standards_decay_% 3 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.16 _exptl_absorpt_correction_T_max .367 _exptl_absorpt_correction_T_min .325 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1544 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .10 _refine_diff_density_max .45 _refine_diff_density_min -.46 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 3656 _refine_ls_number_restraints 14 _refine_ls_restrained_S_all 1.02 _refine_ls_R_factor_all .097 _refine_ls_R_factor_gt .044 _refine_ls_shift/su_max .007 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0678P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .142 _reflns_number_gt 2222 _reflns_number_total 3656 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6010.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2200249 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' '-x+1/2, -y+1/2, -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 .0000 .15359(14) .7500 .02568(18) Uani d S 1 . . Ni Cl1 .06641(4) .1543(2) .85984(5) .0369(3) Uani d . 1 . . Cl Cl2 .01733(5) -.3392(2) .90767(6) .0416(3) Uani d . 1 . . Cl Cl3 .21325(5) .4441(3) .34324(7) .0571(4) Uani d . 1 . . Cl O1 -.04439(13) -.0467(5) .79698(16) .0329(7) Uani d D 1 . . O H1A -.0665(18) -.115(7) .769(2) .040 Uiso d D 1 . . H H1B -.028(2) -.113(7) .831(2) .040 Uiso d D 1 . . H O2 .04223(12) .3594(6) .70079(16) .0348(7) Uani d D 1 . . O H2A .061(2) .431(7) .733(2) .042 Uiso d D 1 . . H H2B .023(2) .439(7) .675(3) .042 Uiso d D 1 . . H O3 .16180(17) .1824(9) .7657(2) .0638(14) Uani d D 1 . . O H3A .137(2) .164(12) .789(4) .077 Uiso d D 1 . . H H3B .187(2) .263(9) .780(4) .077 Uiso d D 1 . . H O4 .09134(14) .3454(7) .28761(19) .0452(8) Uani d D 1 . . O H4A .1262(9) .354(11) .300(3) .054 Uiso d D 1 . . H H4B .078(2) .354(10) .326(2) .054 Uiso d D 1 . . H N1 .20203(16) .5269(7) .5040(2) .0378(9) Uani d D 1 . . N H1 .213(2) .492(9) .4651(19) .045 Uiso d D 1 . . H C2 .23711(18) .5220(7) .5686(2) .0357(10) Uani d . 1 . . C C3 .2159(2) .5567(10) .6320(3) .0503(13) Uani d . 1 . . C H3 .2417 .5589 .6790 .060 Uiso d R 1 . . H C4 .1603(2) .5944(10) .6271(4) .0587(16) Uani d . 1 . . C H4 .1449 .6267 .6714 .070 Uiso d R 1 . . H C5 .1265(2) .5990(9) .5606(4) .0526(14) Uani d . 1 . . C H5 .0925 .6147 .5563 .063 Uiso d R 1 . . H C6 .1485(2) .5638(9) .4985(3) .0475(12) Uani d . 1 . . C H6 .1275 .5750 .4478 .057 Uiso d R 1 . . H C7 .29455(18) .4806(8) .5687(2) .0369(10) Uani d . 1 . . C H7 .3187 .4549 .6124 .044 Uiso d R 1 . . H C8 .38095(18) .3966(7) .4410(2) .0337(10) Uani d . 1 . . C N2 .31041(14) .4551(6) .50681(18) .0331(8) Uani d . 1 . . N N3 .36439(14) .4160(7) .50747(19) .0347(9) Uani d D 1 . . N H3C .3840(19) .438(9) .5469(17) .042 Uiso d D 1 . . H N4 .43360(17) .3601(9) .4416(2) .0472(11) Uani d D 1 . . N H4C .439(3) .338(11) .3988(17) .057 Uiso d D 1 . . H H4D .451(2) .318(9) .481(2) .057 Uiso d D 1 . . H N5 .34519(17) .4116(8) .3810(2) .0442(11) Uani d D 1 . . N H5A .3109(11) .437(10) .379(3) .053 Uiso d D 1 . . H H5B .352(2) .375(9) .3404(19) .053 Uiso d 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 .0262(3) .0259(4) .0236(3) .000 .0003(2) .000 Cl1 .0366(5) .0395(6) .0302(4) -.0008(5) -.0070(4) .0024(5) Cl2 .0472(6) .0406(6) .0347(5) -.0040(6) .0001(4) -.0031(5) Cl3 .0395(6) .0873(11) .0408(6) .0026(7) -.0046(4) .0023(7) O1 .0364(15) .0297(17) .0313(14) -.0070(15) .0014(11) .0011(14) O2 .0368(15) .0319(17) .0336(14) -.0012(16) -.0006(11) .0035(15) O3 .049(2) .102(4) .0419(18) -.005(3) .0096(16) -.006(2) O4 .0436(17) .048(2) .0422(16) -.004(2) .0019(14) -.0055(19) N1 .0360(18) .039(2) .0379(18) -.0005(18) .0032(15) -.0047(18) C2 .035(2) .036(3) .036(2) -.007(2) .0080(16) -.0049(19) C3 .051(3) .061(4) .041(2) -.010(3) .013(2) -.003(3) C4 .054(3) .060(4) .069(4) -.004(3) .031(3) -.006(3) C5 .034(2) .047(3) .079(4) .004(2) .016(2) .000(3) C6 .037(2) .039(3) .064(3) .001(2) .000(2) .008(3) C7 .033(2) .044(3) .0325(19) -.005(2) .0008(16) .000(2) C8 .036(2) .033(2) .0315(18) -.0010(19) .0051(16) .0018(17) N2 .0301(16) .038(2) .0292(16) -.0012(17) .0004(13) -.0035(17) N3 .0280(16) .049(2) .0254(15) -.0001(17) -.0003(12) -.0026(16) N4 .0396(19) .067(3) .0372(18) .009(2) .0120(16) .013(2) N5 .043(2) .061(3) .0263(16) .007(2) -.0020(15) -.0007(19) 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 O1 2_556 2.075(3) no Ni1 O1 . 2.075(3) yes Ni1 O2 . 2.092(4) yes Ni1 O2 2_556 2.092(4) no Ni1 Cl1 . 2.3923(9) yes Ni1 Cl1 2_556 2.3924(9) no N1 C6 . 1.334(6) yes N1 C2 . 1.356(6) yes C2 C3 . 1.386(7) yes C2 C7 . 1.449(6) yes C3 C4 . 1.386(8) yes C4 C5 . 1.369(9) yes C5 C6 . 1.376(8) yes C7 N2 . 1.286(6) yes C8 N3 . 1.368(5) yes C8 N4 . 1.324(6) yes C8 N5 . 1.304(6) yes N2 N3 . 1.360(5) yes 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' O O .0106 .0060 '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' Ni Ni .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 O1 Ni1 O1 2_556 . 93.4(2) ? O1 Ni1 O2 2_556 . 87.70(13) ? O1 Ni1 O2 . . 178.04(13) yes O1 Ni1 O2 2_556 2_556 178.05(13) ? O1 Ni1 O2 . 2_556 87.71(13) ? O2 Ni1 O2 . 2_556 91.3(2) ? O1 Ni1 Cl1 2_556 . 91.35(9) ? O1 Ni1 Cl1 . . 88.83(9) yes O2 Ni1 Cl1 . . 92.79(9) yes O2 Ni1 Cl1 2_556 . 87.03(9) ? O1 Ni1 Cl1 2_556 2_556 88.82(9) ? O1 Ni1 Cl1 . 2_556 91.34(9) ? O2 Ni1 Cl1 . 2_556 87.03(9) ? O2 Ni1 Cl1 2_556 2_556 92.79(9) ? Cl1 Ni1 Cl1 . 2_556 179.75(9) ? C6 N1 C2 . . 123.5(4) no N1 C2 C3 . . 117.9(4) no N1 C2 C7 . . 119.2(4) yes C3 C2 C7 . . 122.9(4) no C2 C3 C4 . . 119.2(5) no C5 C4 C3 . . 120.9(5) no C4 C5 C6 . . 118.7(5) no N1 C6 C5 . . 119.8(5) no N2 C7 C2 . . 118.1(4) yes N5 C8 N4 . . 123.2(4) yes N5 C8 N3 . . 119.9(4) yes N4 C8 N3 . . 116.9(4) yes C7 N2 N3 . . 117.7(4) yes N2 N3 C8 . . 116.9(3) yes 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 O4 5_556 .84 1.99 2.775(5) 156 O1 H1B Cl2 . .84 2.30 3.132(4) 169 O2 H2A O4 6_566 .85 1.97 2.795(6) 163 O2 H2B Cl2 2_566 .84 2.30 3.131(4) 169 O3 H3A Cl1 . .82 2.35 3.163(4) 172 O3 H3B Cl3 6_566 .85 2.42 3.180(6) 147 O4 H4A Cl3 . .86 2.26 3.096(4) 167 O4 H4B Cl2 6 .83 2.31 3.107(4) 161 N1 H1 N2 . .85 2.42 2.717(5) 101 N1 H1 Cl3 . .85 2.29 3.096(4) 160 N3 H3C Cl1 4_556 .82 2.48 3.231(4) 153 N4 H4C O2 7_556 .84 2.43 3.207(6) 155 N4 H4C O1 8 .84 2.49 3.119(5) 132 N4 H4D Cl2 4_556 .84 2.35 3.187(4) 168 N5 H5A N2 . .86 2.37 2.634(5) 98 N5 H5A Cl3 . .86 2.39 3.225(4) 162 N5 H5B O3 7_556 .84 1.98 2.778(6) 157 _journal_paper_doi 10.1107/S1600536801003725