#------------------------------------------------------------------------------ #$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/30/2003016.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_2003016 loop_ _publ_author_name 'Edwards, R. A.' 'Easteal, A. J.' 'Gladkikh, O. P.' 'Robinson, W. T.' 'Turnbull, M. M.' 'Wilkins, C. J.' _publ_section_title ; A Reversible Non-disruptive Phase Transition Shown by the Zinc Iodide Dimethylformamide Complex ZnI~2~(dmf)~2~ ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 663 _journal_page_last 670 _journal_paper_doi 10.1107/S0108768198000536 _journal_volume 54 _journal_year 1998 _chemical_formula_sum 'C6 H14 I2 N2 O2 Zn' _chemical_formula_weight 465.36 _chemical_name_systematic ; ? ; _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 _cell_angle_alpha 90.00 _cell_angle_beta 110.88(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 14.005(8) _cell_length_b 13.697(6) _cell_length_c 15.755(8) _cell_measurement_reflns_used 20 _cell_measurement_temperature 233(2) _cell_measurement_theta_max 12.49 _cell_measurement_theta_min 7.36 _cell_volume 2824(3) _computing_cell_refinement 'XSCANS (Siemens, 1989)' _computing_data_collection 'XSCANS (Siemens, 1989)' _computing_data_reduction 'XPREP (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXL93 (Sheldrick, 1993)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 233(2) _diffrn_measurement_device 'Siemens P4 four-circle' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0094 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 3384 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 'No decay; steady +/-2.5' _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.092 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.189 _exptl_crystal_description irregular _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.40 _refine_diff_density_max 1.994 _refine_diff_density_min -1.359 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.081 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 132 _refine_ls_number_reflns 3236 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.152 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_obs 0.0490 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[s^2^(Fo^2^)+( 0.0436P)^2^+25.8561P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1183 _refine_ls_wR_factor_obs 0.1059 _reflns_number_observed 2310 _reflns_number_total 3236 _reflns_observed_criterion I>2sigma(I) _[local]_cod_data_source_file mu0321.cif _[local]_cod_data_source_block HT _[local]_cod_cif_authors_sg_H-M C2/c _[local]_cod_chemical_formula_sum_orig '[Zn I2 (C3 H7 N O )2 ]' _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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+( 0.0436P)^2^+25.8561P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0436P)^2^+25.8561P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2003016 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_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 I1 0.0605(3) 0.0453(3) 0.0672(4) 0.0066(3) 0.0206(3) 0.0046(3) I2 0.0570(4) 0.0836(5) 0.0629(4) 0.0074(3) 0.0007(3) -0.0174(3) Zn 0.0462(5) 0.0420(5) 0.0494(5) 0.0007(4) 0.0226(4) -0.0022(4) O1 0.038(3) 0.043(3) 0.058(3) 0.003(2) 0.017(2) -0.011(2) O2 0.073(4) 0.051(3) 0.081(4) -0.003(3) 0.049(3) -0.001(3) N1 0.047(3) 0.046(3) 0.046(3) -0.001(3) 0.022(3) -0.003(3) N2 0.080(5) 0.060(5) 0.094(6) 0.012(4) 0.058(5) 0.024(4) C1 0.046(4) 0.043(4) 0.050(4) 0.000(3) 0.019(3) -0.006(3) C2 0.066(6) 0.076(7) 0.109(8) 0.010(5) 0.037(6) -0.033(6) C3 0.065(5) 0.064(6) 0.073(6) -0.019(5) 0.027(5) -0.025(5) C4 0.069(6) 0.053(5) 0.084(6) 0.016(4) 0.043(5) 0.012(5) C6 0.105(8) 0.080(7) 0.088(7) -0.022(6) 0.065(7) -0.017(6) C5 0.16(2) 0.066(10) 0.15(2) -0.003(11) 0.11(2) 0.020(11) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol I1 0.17690(4) 0.03893(4) 0.15652(4) 0.0583(2) Uani d . 1 . I I2 0.43661(5) -0.11479(5) 0.36062(4) 0.0735(2) Uani d . 1 . I Zn 0.25471(7) -0.11222(6) 0.24758(6) 0.0443(2) Uani d . 1 . Zn O1 0.2377(4) -0.2259(4) 0.1629(3) 0.0462(12) Uani d . 1 . O O2 0.1616(5) -0.1526(4) 0.3112(4) 0.062(2) Uani d . 1 . O N1 0.3023(5) -0.3460(4) 0.1020(4) 0.0449(14) Uani d . 1 . N N2 0.0850(6) -0.2627(6) 0.3719(6) 0.070(2) Uani d . 1 . N C1 0.3098(6) -0.2720(5) 0.1565(5) 0.046(2) Uani d . 1 . C H1 0.3758(6) -0.2527(5) 0.1938(5) 0.055 Uiso calc R 1 . H C2 0.3927(7) -0.3996(8) 0.1023(8) 0.082(3) Uani d . 1 . C H2A 0.387(3) -0.413(4) 0.0402(8) 0.098 Uiso calc R 1 . H H2B 0.398(3) -0.461(2) 0.135(4) 0.098 Uiso calc R 1 . H H2C 0.4533(9) -0.361(2) 0.132(4) 0.098 Uiso calc R 1 . H C3 0.2028(7) -0.3831(7) 0.0446(6) 0.067(2) Uani d . 1 . C H3A 0.184(2) -0.437(3) 0.0748(18) 0.080 Uiso calc R 1 . H H3B 0.2063(13) -0.405(4) -0.0127(16) 0.080 Uiso calc R 1 . H H3C 0.1523(11) -0.3315(13) 0.033(3) 0.080 Uiso calc R 1 . H C4 0.1397(7) -0.2361(7) 0.3231(7) 0.064(2) Uani d . 1 . C H4 0.1639(7) -0.2859(7) 0.2950(7) 0.077 Uiso calc R 1 . H C6 0.0454(9) -0.1903(8) 0.4161(7) 0.082(3) Uani d . 1 . C H6A 0.092(3) -0.182(4) 0.4781(15) 0.099 Uiso calc R 1 . H H6B -0.021(2) -0.211(2) 0.416(4) 0.099 Uiso calc R 1 . H H6C 0.038(5) -0.1288(15) 0.384(3) 0.099 Uiso calc R 1 . H C5 0.053(3) -0.3676(12) 0.373(3) 0.109(10) Uani d P 0.81(6) 2 C H51 0.014(3) -0.3738(12) 0.413(3) 0.163 Uiso calc PR 0.81(6) 2 H H52 0.113(3) -0.4085(12) 0.396(3) 0.163 Uiso calc PR 0.81(6) 2 H H53 0.012(3) -0.3879(12) 0.312(3) 0.163 Uiso calc PR 0.81(6) 2 H 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' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 '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' N N .0061 .0033 '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 O2 Zn O1 100.1(2) O2 Zn I1 106.6(2) O1 Zn I1 109.4(2) O2 Zn I2 108.5(2) O1 Zn I2 107.90(14) I1 Zn I2 122.06(4) C1 O1 Zn 123.3(5) C4 O2 Zn 125.9(6) C1 N1 C3 120.9(7) C1 N1 C2 121.3(7) C3 N1 C2 117.5(7) C4 N2 C6 120.0(8) C4 N2 C5 120.7(10) C6 N2 C5 119.0(9) O1 C1 N1 125.3(7) O2 C4 N2 125.6(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 Zn 2.5332(13) I2 Zn 2.535(2) Zn O2 1.986(6) Zn O1 2.009(5) O1 C1 1.224(8) O2 C4 1.215(10) N1 C1 1.307(9) N1 C3 1.456(10) N1 C2 1.463(10) N2 C4 1.316(11) N2 C6 1.432(12) N2 C5 1.51(2) 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 O2 Zn O1 C1 -128.2(6) O1 Zn O2 C4 27.5(9) I1 Zn O1 C1 120.0(6) I2 Zn O1 C1 -14.8(6) I1 Zn O2 C4 141.4(8) I2 Zn O2 C4 -85.4(8) O1 C1 N1 C2 -177.1(8) O1 C1 N1 C3 -2.5(12) O2 C4 N2 C5 173.(2) O2 C4 N2 C6 0.3(16) Zn O1 C1 N1 -179.6(6) Zn O2 C4 N2 173.9(7)