#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/82/2008212.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_2008212 loop_ _publ_author_name 'De-Liang Long' 'Huai-Ming Hu' 'Jiu-Tong Chen' 'Jin-Shun Huang' _publ_section_title ; [Ni{(CH~3~)~2~SO}~6~]I~4~, a redetermination and reinterpretation ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 339 _journal_page_last 341 _journal_paper_doi 10.1107/S0108270198013055 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Ni (C2 H6 O S)6] I4' _chemical_formula_moiety 'C12 H36 Ni1 O6 S6 2+, I4 2-' _chemical_formula_sum 'C12 H36 I4 Ni O6 S6' _chemical_formula_weight 1035.08 _chemical_name_systematic ; Hexa(dimethylsulfoxide-O)nickel(II) tetraiodide(2-) ; _space_group_IT_number 148 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 11.8241(5) _cell_length_b 11.8241(5) _cell_length_c 19.8441(11) _cell_measurement_reflns_used 3245 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 2.24 _cell_volume 2402.7(2) _computing_cell_refinement 'SMART and SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Siemens, 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method 'area detector' _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 0.019 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 3994 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 2.24 _exptl_absorpt_coefficient_mu 4.874 _exptl_absorpt_correction_T_max 0.614 _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_type 'empirical (SADABS; Sheldrick, 1996)' _exptl_crystal_colour 'deep brown' _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1476 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.32 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.131 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_hydrogen_treatment refiso _refine_ls_matrix_type full _refine_ls_number_parameters 69 _refine_ls_number_reflns 943 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.168 _refine_ls_restrained_S_obs 1.159 _refine_ls_R_factor_all 0.024 _refine_ls_R_factor_obs 0.019 _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^)+(0.0125P)^2^+4.788P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.041 _refine_ls_wR_factor_obs 0.039 _reflns_number_observed 854 _reflns_number_total 944 _reflns_observed_criterion I>2\s(I) _cod_data_source_file bm1277.cif _cod_data_source_block bm1277 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0125P)^2^+4.788P] 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^)+(0.0125P)^2^+4.788P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 2008212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 0.0256(3) 0.0256(3) 0.0371(5) 0.01282(13) 0.000 0.000 I1 0.03985(14) 0.03985(14) 0.0779(3) 0.01993(7) 0.000 0.000 I2 0.0509(2) 0.0509(2) 0.0486(2) 0.02543(8) 0.000 0.000 S 0.0331(4) 0.0341(4) 0.0488(4) 0.0186(3) 0.0063(3) 0.0076(3) O 0.0353(10) 0.0311(10) 0.0463(11) 0.0169(8) 0.0001(8) 0.0033(8) C1 0.054(2) 0.037(2) 0.057(2) 0.022(2) 0.003(2) 0.000(2) C2 0.071(3) 0.058(2) 0.046(2) 0.041(2) 0.007(2) 0.012(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Ni 0.3333 0.6667 -0.3333 0.0294(2) Uani d S 1 . Ni I1 0 0 -0.42824(2) 0.05254(13) Uani d S 1 . I I2 0 0 -0.25984(2) 0.05009(12) Uani d S 1 . I S 0.29182(7) 0.41669(7) -0.25930(4) 0.0378(2) Uani d . 1 . S O 0.3912(2) 0.5581(2) -0.27545(9) 0.0374(4) Uani d . 1 . O C1 0.3264(4) 0.3198(3) -0.3153(2) 0.0496(8) Uani d . 1 . C H11 0.305(3) 0.335(3) -0.357(2) 0.061(11) Uiso d . 1 . H H12 0.405(4) 0.344(4) -0.3083(18) 0.063(12) Uiso d . 1 . H H13 0.275(4) 0.236(4) -0.2999(18) 0.063(11) Uiso d . 1 . H C2 0.3498(4) 0.3834(4) -0.1833(2) 0.0549(9) Uani d . 1 . C H21 0.289(4) 0.294(4) -0.1732(19) 0.070(11) Uiso d . 1 . H H22 0.437(4) 0.399(4) -0.1899(19) 0.071(12) Uiso d . 1 . H H23 0.343(4) 0.435(4) -0.154(2) 0.071(13) Uiso d . 1 . H 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' I I -0.4742 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 O Ni O 3_565 2_665 92.37(7) no O Ni O 3_565 13_564 87.63(7) no O Ni O 2_665 13_564 87.63(7) no O Ni O 3_565 14_454 87.63(7) no O Ni O 2_665 14_454 180.0 no O Ni O 13_564 14_454 92.37(7) no O Ni O 3_565 15_554 180.0 no O Ni O 2_665 15_554 87.63(7) no O Ni O 13_564 15_554 92.37(7) no O Ni O 14_454 15_554 92.37(7) no O Ni O . 3_565 92.37(7) yes O Ni O 2_665 . 92.37(7) no O Ni O 13_564 . 180 yes O Ni O . 14_454 87.63(7) yes O Ni O 15_554 . 87.63(7) no I1 I1 I2 10_554 . 180 yes O S C2 . . 104.5(2) yes O S C1 . . 106.0(2) yes C1 S C2 . . 98.5(2) yes Ni O S . . 118.90(10) yes 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 O 3_565 2.077(2) no Ni O 2_665 2.077(2) no Ni O 13_564 2.077(2) no Ni O 14_454 2.077(2) no Ni O 15_554 2.077(2) no Ni O . 2.077(2) yes I1 I1 10_554 2.8480(10) yes I1 I2 . 3.3420(10) yes S O . 1.521(2) yes S C1 . 1.784(4) yes S C2 . 1.780(4) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168307662