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
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./