#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/22/2012277.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_2012277 loop_ _publ_author_name 'Bogdanovi\'c, Goran A.' 'Leovac, Vukadin M.' 'Novakovi\'c, Sladjana B.' '\S-methylisothiosemicarbazido-N^1^,N^4^)bis(pyrazole-N^2^)nickel(II) diiodide ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1138 _journal_page_last 1140 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ni (C2 H7 N3 S)2 (C3 H4 N2)2] I2' _chemical_formula_moiety 'C10 H22 N10 Ni S2, 2(I)' _chemical_formula_sum 'C10 H22 I2 N10 Ni S2' _chemical_formula_weight 659.0 _chemical_name_systematic ; bis(S-methylisothiosemicarbazide-N^1^,N^4^)-bis(pyrazole-N^2^)- nickel(II) iodide ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 102.92(3) _cell_angle_beta 92.43(2) _cell_angle_gamma 112.05(2) _cell_formula_units_Z 1 _cell_length_a 7.911(3) _cell_length_b 8.798(3) _cell_length_c 8.819(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(3) _cell_measurement_theta_max 17.58 _cell_measurement_theta_min 13.17 _cell_volume 549.1(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL97 and PARST (Nardelli, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(3) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/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 .0137 _diffrn_reflns_av_sigmaI/netI .0181 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2556 _diffrn_reflns_theta_full 26.97 _diffrn_reflns_theta_max 26.97 _diffrn_reflns_theta_min 2.39 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 3.901 _exptl_absorpt_correction_T_max .4689 _exptl_absorpt_correction_T_min .3612 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(Spek, 1990)' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 318 _exptl_crystal_size_max .36 _exptl_crystal_size_mid .29 _exptl_crystal_size_min .25 _refine_diff_density_max 1.485 _refine_diff_density_min -1.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 2378 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.113 _refine_ls_R_factor_all .0401 _refine_ls_R_factor_gt .0345 _refine_ls_shift/esd_mean .000 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.5270P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .0919 _refine_ls_wR_factor_ref .0953 _reflns_number_gt 2119 _reflns_number_total 2378 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file na1529.cif _[local]_cod_data_source_block III _cod_database_code 2012277 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ni .5000 .0000 .5000 .02522(15) Uani d S 1 . . Ni I .19744(4) -.57364(3) .31790(4) .05072(13) Uani d . 1 . . I S .11687(14) .21452(14) .75518(13) .0437(2) Uani d . 1 . . S N1 .2381(4) -.1630(4) .5372(4) .0326(6) Uani d . 1 . . N N2 .1582(5) -.0600(4) .6254(4) .0410(8) Uani d . 1 . . N N3 .3887(4) .1724(4) .5883(4) .0300(6) Uani d . 1 . . N N4 .3890(4) -.0296(4) .2669(4) .0344(6) Uani d . 1 . . N N5 .3362(5) .0825(5) .2208(4) .0399(7) Uani d . 1 . . N C1 .2385(4) .1088(4) .6454(4) .0287(6) Uani d . 1 . . C C2 .2670(8) .4321(6) .7893(7) .0682(15) Uani d . 1 . . C C3 .2598(7) .0282(6) .0706(5) .0484(10) Uani d . 1 . . C C4 .2619(7) -.1281(7) .0136(5) .0501(10) Uani d . 1 . . C C5 .3420(6) -.1589(5) .1400(5) .0411(8) Uani d . 1 . . C H2A .2122 .5020 .8496 .102 Uiso calc R 1 . . H H2B .2872 .4599 .6906 .102 Uiso calc R 1 . . H H2C .3825 .4517 .8463 .102 Uiso calc R 1 . . H H3 .2138 .0862 .0154 .058 Uiso calc R 1 . . H H4 .2192 -.1985 -.0877 .060 Uiso calc R 1 . . H H5 .3604 -.2580 .1364 .049 Uiso calc R 1 . . H H1N1 .236(6) -.237(6) .586(5) .036(11) Uiso d . 1 . . H H1N2 .065(7) -.096(6) .655(5) .039(12) Uiso d . 1 . . H H1N3 .435(6) .290(6) .613(5) .035(11) Uiso d . 1 . . H H1N5 .343(7) .163(7) .276(6) .040(13) Uiso d . 1 . . H H2N1 .166(10) -.247(9) .453(8) .08(2) 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 Ni .0212(3) .0231(3) .0317(3) .0091(2) .0033(2) .0071(2) I .04079(18) .02786(17) .0788(2) .00839(12) .01312(14) .01298(13) S .0402(5) .0467(6) .0504(6) .0252(4) .0156(4) .0089(4) N1 .0285(14) .0245(14) .0435(17) .0089(12) .0079(12) .0084(13) N2 .0311(16) .0307(16) .060(2) .0085(13) .0211(15) .0122(14) N3 .0262(13) .0247(14) .0390(15) .0102(11) .0067(11) .0073(11) N4 .0342(15) .0356(16) .0369(15) .0168(13) .0029(12) .0110(12) N5 .0457(19) .0383(19) .0419(18) .0215(15) .0043(14) .0144(15) C1 .0261(15) .0340(17) .0281(15) .0150(13) .0016(12) .0070(13) C2 .068(3) .042(3) .086(4) .028(2) .010(3) -.010(2) C3 .050(2) .061(3) .044(2) .026(2) .0041(18) .026(2) C4 .052(2) .064(3) .033(2) .024(2) .0000(17) .0092(18) C5 .046(2) .038(2) .042(2) .0207(17) .0027(16) .0072(15) 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 Ni N1 2_656 2.120(3) no Ni N1 . 2.120(3) yes Ni N3 . 2.053(3) yes Ni N3 2_656 2.053(3) no Ni N4 2_656 2.122(3) no Ni N4 . 2.122(3) yes C1 N2 . 1.343(5) yes C1 S . 1.754(3) yes C2 S . 1.780(6) yes C3 C4 . 1.361(7) no C4 C5 . 1.387(6) no N1 N2 . 1.407(4) no N3 C1 . 1.287(4) yes N4 C5 . 1.328(5) yes N4 N5 . 1.337(4) yes N5 C3 . 1.334(6) yes C2 H2A . .9600 ? C2 H2B . .9600 ? C2 H2C . .9600 ? N3 H1N3 . .92(5) ? N5 H1N5 . .75(5) ? C3 H3 . .9300 ? C5 H5 . .9300 ? C4 H4 . .9300 ? N2 H1N2 . .77(5) ? N1 H1N1 . .85(5) ? N1 H2N1 . .91(7) ? 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' S S .1246 .1234 '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' I I -.4742 1.8119 '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 C1 N3 Ni . . 113.8(2) yes N3 Ni N3 2_656 . 180.0 no N3 Ni N1 2_656 2_656 79.00(12) no N3 Ni N1 . 2_656 101.00(12) no N3 Ni N1 2_656 . 101.00(12) no N3 Ni N1 . . 79.00(12) yes N1 Ni N1 2_656 . 180.0 no N3 Ni N4 2_656 2_656 91.49(12) no N3 Ni N4 . 2_656 88.51(12) no N1 Ni N4 2_656 2_656 89.57(13) no N1 Ni N4 . 2_656 90.43(13) no N3 Ni N4 2_656 . 88.51(12) no N3 Ni N4 . . 91.49(12) no N1 Ni N4 2_656 . 90.43(13) no N1 Ni N4 . . 89.57(13) no N4 Ni N4 2_656 . 180.0 no C3 N5 N4 . . 112.5(4) no C5 N4 N5 . . 104.2(3) no C5 N4 Ni . . 131.0(3) no N5 N4 Ni . . 124.5(3) no N3 C1 N2 . . 119.4(3) yes N3 C1 S . . 128.6(3) no N2 C1 S . . 111.9(3) no C1 S C2 . . 102.8(2) no N5 C3 C4 . . 107.0(4) no N4 C5 C4 . . 111.6(4) no C3 C4 C5 . . 104.6(4) no C1 N2 N1 . . 118.7(3) yes N2 N1 Ni . . 107.4(2) yes S C2 H2A . . 109.5 ? S C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? S C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 N3 H1N3 . . 112(3) ? Ni N3 H1N3 . . 132(3) ? C3 N5 H1N5 . . 125(4) ? N4 N5 H1N5 . . 123(4) ? N5 C3 H3 . . 126.5 ? C4 C3 H3 . . 126.5 ? N4 C5 H5 . . 124.2 ? C4 C5 H5 . . 124.2 ? C3 C4 H4 . . 127.7 ? C5 C4 H4 . . 127.7 ? C1 N2 H1N2 . . 118(4) ? N1 N2 H1N2 . . 123(4) ? N2 N1 H1N1 . . 107(3) ? Ni N1 H1N1 . . 117(3) ? N2 N1 H2N1 . . 118(4) ? Ni N1 H2N1 . . 117(4) ? H1N1 N1 H2N1 . . 90(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 _geom_hbond_publ_flag N2 H1N2 I 2_546 .77(5) 2.94(5) 3.548(4) 138(4) yes N3 H1N3 I 2_656 .92(5) 2.96(5) 3.695(3) 137(3) yes N5 H1N5 I 1_565 .75(5) 2.91(5) 3.536(4) 143(5) yes N1 H2N1 I . .91(7) 2.96(7) 3.585(3) 128(5) yes _cod_database_fobs_code 2012277 _journal_paper_doi 10.1107/S010827010100991X