data_global #============================================================================= # start Validation Reply Form #Alert level C _vrf_SHFSU01 ; PROBLEM: The absolute value of parameter shift to su ratio > 0.05 Absolute value of the parameter shift to su ratio given 0.100 Additional refinement cycles may be required. RESPONSE: The quality of refinement for powder diffraction data is worse compare to single crystal. ; _vrf_PLAT080 ; PROBLEM: Maximum Shift/Error ............................ 0.10 RESPONSE: The quality of refinement for powder diffraction data is worse compare to single crystal. ; _vrf_PLAT420 ; PROBLEM: Without Acceptor N7 - H7C RESPONSE: Positions of hydrogen atoms were not directly defined. Hydrogens were attached according to ideal tetrahedral coordination of the nitrogen. This is the reasons why H7C has a distance with nearest chlorine higher that limit for hydrogen bond N-H...Cl. ; _vrf_PLAT790 ; PROBLEM: Centre of Gravity not Within Unit Cell: Resd. #1 Note Cl4 Cu RESPONSE: The choice was done to present Cu coordination sphere in integrity. ; # end Validation Reply Form #==================================================================== _publ_requested_journal 'xxx' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Kirik, Sergei D.' # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; Siberian Federal Univ, 660041, Krasnoyarsk, Russia ; _publ_contact_author_email kirik@icct.ru _publ_contact_author_phone '+7 (391) 29070636:25 31/10/2014' _publ_contact_author_fax ? loop_ _publ_author_name _publ_author_address 'Golovnev, N. N.' ; Siberian Federal Univ, 660041, Krasnoyarsk, Russia ; 'Kirik, Sergei D.' ; Siberian Federal Univ, 660041, Krasnoyarsk, Russia ; 'Leshok, Darya Y.' ; Siberian Federal Univ, 660041, Krasnoyarsk, Russia ; _publ_contact_letter ; ? ; _publ_requested_coeditor_name ? _publ_requested_category ? #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) # ============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Cystamindi-ium tetrachloridocuprate [NH3(CH2)2SS(CH2)2NH3][CuCl4]: synthesis, crystal structure and thermal decomposition. ; _publ_section_title_footnote . loop_ _publ_author_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis . _publ_section_abstract ; (type here to add abstract) ; _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; (type here to add preparation details) ; _publ_section_exptl_refinement ; (type here to add refinement details) ; _publ_section_references ; ? ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; #============================================================================= data_gn1178 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common '' _chemical_formula_moiety 'Cl4 Cu, C4 H14 N2 S2' _chemical_formula_structural '[CuCl4](SC2H4NH3)2' _chemical_formula_analytical ? _chemical_formula_sum 'C4 H14 Cl4 Cu N2 S2' _chemical_formula_weight 359.64 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source cu 13.33800 3.58280 7.16760 0.24700 5.61580 11.39660 1.67350 64.81260 1.19100 -2.01900 0.58900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 cl 11.46040 0.01040 7.19640 1.16620 6.25560 18.51940 1.64550 47.77840 -9.55740 0.34800 0.70200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 s 6.90530 1.46790 5.20340 22.21510 1.43790 0.25360 1.58630 56.17200 0.86690 0.31900 0.55700 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 'x,y,z' '-x,y+1/2,-z' _cell_length_a 7.184(1) _cell_length_b 7.503(1) _cell_length_c 12.011(10) _cell_angle_alpha 90.00000 _cell_angle_beta 101.181(9) _cell_angle_gamma 90.00000 _cell_volume 635.12(13) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Final cell parameters are obtained from the Rietveld refinement ; _exptl_absorpt_coefficient_mu 12.936 _exptl_crystal_density_diffrn 1.880 _exptl_crystal_F_000 362.0 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour 'pale yellow' # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_temperature 295 #============================================================================= # 7. EXPERIMENTAL DATA _pd_instr_location ; ? Structure And Spectroscopic Investigations Lab. Institute of Chem.& Chem. Tech., 660049,Krasnoyarsk, Russia ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_ambient_temperature 295 _diffrn_measurement_device 'PANalytical X'Pert PRO' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector ? _diffrn_detector_type PIXcel # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 2997 _pd_meas_2theta_range_min 3.03900 _pd_meas_2theta_range_max 80.93500 _pd_meas_2theta_range_inc 0.026000 #============================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; # The next two items are given as text _pd_proc_ls_profile_function 'Pearson VII' _pd_proc_ls_background_function 'linear interpolation between 30 points with refined heights' _pd_proc_ls_pref_orient_corr 'March-Dollase correction' _pd_proc_2theta_range_min 3.03900 _pd_proc_2theta_range_max 89.93500 _pd_proc_2theta_range_inc 0.026000 _pd_proc_ls_prof_R_factor 3.67 _pd_proc_ls_prof_wR_factor 4.85 _pd_proc_ls_prof_wR_expected 4.00 _refine_special_details ; ? ; _refine_ls_matrix_type userblock _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 104 _refine_ls_number_restraints 28 _refine_ls_number_constraints ? _refine_ls_R_I_factor 3.73 _refine_ls_goodness_of_fit_all 1.46 _refine_ls_shift/su_max 0.10 _refine_ls_shift/su_mean 0.10 _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction none _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _computing_data_collection '' _computing_cell_refinement 'DICVOL04 (Boultif, Louer, 2004)' _computing_structure_solution 'FOX (Favre-Nicolin, Cerny, 2002)' _computing_structure_refinement 'FULLPROF (Rodriguez-Carvajal, )' _computing_molecular_graphics '' _computing_publication_material '' #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Cu1 0.7368(1) 0.0980(1) 0.000(1) . 1.00000 Uani Cu Cl2 0.6769(1) 0.0627(1) -0.1945(1) . 1.00000 Uani Cl Cl3 0.9555(1) 0.3131(21) -0.0134(1) . 1.00000 Uani Cl Cl4 0.7966(1) 0.1332(1) 0.1945(2) . 1.00000 Uani Cl Cl5 0.5181(1) -0.1170(1) 0.0134(10) . 1.00000 Uani Cl S1 0.7963(1) 0.4615(1) 0.5587(1) . 1.00000 Uani S S2 0.8428(1) 0.7101(1) 0.4983(1) . 1.00000 Uani S C3 0.5509(1) 0.5090(1) 0.5723(1) 0.02533 1.00000 Uiso C H3A 0.5025(11) 0.3986(13) 0.5954(10) 0.03800 1.00000 Uiso H H3B 0.4720(11) 0.5432(13) 0.5016(10) 0.03800 1.00000 Uiso H C4 0.5143(1) 0.6534(1) 0.6575(1) 0.02533 1.00000 Uiso C H4A 0.3845(10) 0.6437(10) 0.6658(13) 0.03800 1.00000 Uiso H H4B 0.5557(10) 0.7599(10) 0.6252(13) 0.03800 1.00000 Uiso H C5 0.7597(1) 0.6664(1) 0.3442(1) 0.02533 1.00000 Uiso C H5A 0.7796(10) 0.7741(12) 0.3048(10) 0.03800 1.00000 Uiso H H5B 0.6280(10) 0.6344(12) 0.3257(10) 0.03800 1.00000 Uiso H C6 0.8871(1) 0.5146(1) 0.3167(1) 0.02533 1.00000 Uiso C H6A 0.8394(10) 0.4017(11) 0.3361(13) 0.03800 1.00000 Uiso H H6B 1.0140(10) 0.5291(11) 0.3591(13) 0.03800 1.00000 Uiso H N7 0.6357(1) 0.6303(21) 0.7728(1) 0.02533 1.00000 Uiso N H7A 0.6123(11) 0.7269(10) 0.8209(11) 0.03800 1.00000 Uiso H H7B 0.6038(11) 0.5195(10) 0.8049(11) 0.03800 1.00000 Uiso H H7C 0.7669(11) 0.6295(10) 0.7865(11) 0.03800 1.00000 Uiso H N8 0.8863(1) 0.5225(1) 0.1935(1) 0.02533 1.00000 Uiso N H8A 0.9649(11) 0.4290(10) 0.1734(11) 0.03800 1.00000 Uiso H H8B 0.7589(11) 0.5077(10) 0.1520(11) 0.03800 1.00000 Uiso H H8C 0.9345(11) 0.6358(10) 0.1751(11) 0.03800 1.00000 Uiso 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 _atom_site_aniso_type_symbol Cu1 0.042(21) 0.021(45) 0.076(34) 0.00000 0.040(51) 0.00000 Cu Cl2 0.025(30) 0.037(13) 0.052(12) 0.00000 0.015(12) 0.00000 Cl Cl3 0.030(44) 0.050(11) 0.073(13) 0.00000 0.024(13) 0.00000 Cl Cl4 0.031(23) 0.041(65) 0.051(41) 0.00000 0.027(11) 0.00000 Cl Cl5 0.049(61) 0.017(19) 0.082(16) 0.00000 0.018(10) 0.00000 Cl S1 0.048(13) 0.051(30) 0.050(12) 0.00000 0.013(16) 0.00000 S S2 0.023(23) 0.064(20) 0.065(14) 0.00000 0.020(19) 0.00000 S # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ; CuCl4(NSC2H7)2 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cl2 2.307(4) . . ? Cu1 Cl3 2.279(8) . . ? Cu1 Cl4 2.307(4) . . ? Cu1 Cl5 2.279(8) . . ? S1 S2 2.052(2) . . ? S1 C3 1.8367(19) . . ? S2 C5 1.860(2) . . ? C3 H3A 0.960(10) . . ? C3 H3B 0.960(11) . . ? C3 C4 1.5474(19) . . ? C4 H4A 0.960(8) . . ? C4 H4B 0.960(9) . . ? C4 N7 1.496(3) . . ? C5 H5A 0.961(10) . . ? C5 H5B 0.960(8) . . ? C5 C6 1.5367(11) . . ? C6 H6A 0.959(9) . . ? C6 H6B 0.960(11) . . ? C6 N8 1.479(4) . . ? N7 H7A 0.961(15) . . ? N7 H7B 0.958(16) . . ? N7 H7C 0.925(9) . . ? N8 H8A 0.960(8) . . ? N8 H8B 0.960(10) . . ? N8 H8C 0.960(8) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Cu1 Cl3 90.3(3) . . . ? Cl2 Cu1 Cl4 180.00(1) . . . ? Cl2 Cu1 Cl5 89.7(3) . . . ? Cl3 Cu1 Cl4 89.7(3) . . . ? Cl3 Cu1 Cl5 180.0(4) . . . ? Cl4 Cu1 Cl5 90.3(3) . . . ? S2 S1 C3 94.59(5) . . . ? S1 S2 C5 98.55(6) . . . ? S1 C3 H3A 105.4(5) . . . ? S1 C3 H3B 112.7(6) . . . ? S1 C3 C4 118.93(7) . . . ? H3A C3 H3B 107.6(9) . . . ? H3A C3 C4 107.2(6) . . . ? H3B C3 C4 104.5(6) . . . ? C3 C4 H4A 108.0(7) . . . ? C3 C4 H4B 102.1(8) . . . ? C3 C4 N7 112.7(5) . . . ? H4A C4 H4B 119.2(7) . . . ? H4A C4 N7 107.4(9) . . . ? H4B C4 N7 107.5(9) . . . ? S2 C5 H5A 107.0(7) . . . ? S2 C5 H5B 112.7(7) . . . ? S2 C5 C6 104.77(7) . . . ? H5A C5 H5B 109.3(8) . . . ? H5A C5 C6 111.5(5) . . . ? H5B C5 C6 111.5(6) . . . ? C5 C6 H6A 110.3(5) . . . ? C5 C6 H6B 110.2(6) . . . ? C5 C6 N8 107.35(8) . . . ? H6A C6 H6B 108.6(9) . . . ? H6A C6 N8 110.2(9) . . . ? H6B C6 N8 110.2(8) . . . ? C4 N7 H7A 109.4(8) . . . ? C4 N7 H7B 109.6(7) . . . ? C4 N7 H7C 123.8(8) . . . ? H7A N7 H7B 109.5(9) . . . ? H7A N7 H7C 100.8(12) . . . ? H7B N7 H7C 103.9(13) . . . ? C6 N8 H8A 109.5(8) . . . ? C6 N8 H8B 109.5(7) . . . ? C6 N8 H8C 109.5(8) . . . ? H8A N8 H8B 109.4(8) . . . ? H8A N8 H8C 109.5(7) . . . ? H8B N8 H8C 109.5(8) . . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Cu1 Cl5 Cu1 28.09(1) . . . . ? Cl4 Cu1 Cl5 Cu1 -151.91(1) . . . . ? Cl5 Cu1 Cl5 Cu1 120.25(1) . . . . ? C3 S1 S2 C5 -88.98(6) . . . . ? S2 S1 C3 H3A 175.7(7) . . . . ? S2 S1 C3 H3B 58.7(6) . . . . ? S2 S1 C3 C4 -64.10(9) . . . . ? S1 S2 C5 H5A -177.5(5) . . . . ? S1 S2 C5 H5B 62.3(6) . . . . ? S1 S2 C5 C6 -59.10(6) . . . . ? S1 C3 C4 H4A -167.9(8) . . . . ? S1 C3 C4 H4B 65.6(7) . . . . ? S1 C3 C4 N7 -49.5(4) . . . . ? H3A C3 C4 H4A -48.6(10) . . . . ? H3A C3 C4 H4B -175.6(6) . . . . ? H3A C3 C4 N7 69.8(7) . . . . ? H3B C3 C4 H4A 65.8(8) . . . . ? H3B C3 C4 H4B -61.2(9) . . . . ? H3B C3 C4 N7 -176.7(4) . . . . ? C3 C4 N7 H7A 176.8(7) . . . . ? C3 C4 N7 H7B -63.9(7) . . . . ? C3 C4 N7 H7C 60.2(13) . . . . ? H4A C4 N7 H7A -64.8(9) . . . . ? H4A C4 N7 H7B 55.2(9) . . . . ? H4A C4 N7 H7C 177.5(15) . . . . ? H4B C4 N7 H7A 64.7(8) . . . . ? H4B C4 N7 H7B -175.3(7) . . . . ? H4B C4 N7 H7C -53.0(18) . . . . ? S2 C5 C6 H6A 82.8(9) . . . . ? S2 C5 C6 H6B -37.1(8) . . . . ? S2 C5 C6 N8 -157.07(6) . . . . ? H5A C5 C6 H6A -161.9(11) . . . . ? H5A C5 C6 H6B 78.3(10) . . . . ? H5A C5 C6 N8 -41.7(7) . . . . ? H5B C5 C6 H6A -39.4(12) . . . . ? H5B C5 C6 H6B -159.3(11) . . . . ? H5B C5 C6 N8 80.7(7) . . . . ? C5 C6 N8 H8A -180.00(1) . . . . ? C5 C6 N8 H8B -60.0(5) . . . . ? C5 C6 N8 H8C 60.0(5) . . . . ? H6A C6 N8 H8A -59.9(5) . . . . ? H6A C6 N8 H8B 60.1(5) . . . . ? H6A C6 N8 H8C -179.9(5) . . . . ? H6B C6 N8 H8A 60.0(5) . . . . ? H6B C6 N8 H8B 179.9(5) . . . . ? H6B C6 N8 H8C -60.1(5) . . . . ? #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./