data_Compound_1
_audit_update_record
;
2014-04-11 # Formatted by publCIF
;
# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents
section
;
Introduction
;
;
;
section
;
Experimental
;
;
;
subsection
;
Synthesis and crystallization
;
;
;
subsection
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;
section
;
Results and discussion
;
;
;
# publcif _publ_body_element loop end
#==============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name 'Alexandre Cuin'
_publ_contact_author_address
;
LQBin - Laboratorio de Quimica Bioinorganica
Departamento de Quimica - Instituto de Ciencias Exatas,
Universidade Federal de Juiz de Fora,
Campus Universitario, 36036-900 Juiz de Fora-MG, Brazil
;
_publ_contact_author_email 'alexandre_cuin@yahoo.com'
_publ_contact_author_fax '+ 55 32 3229-3330'
_publ_contact_author_phone '+ 55 32 3229-3310'
_publ_requested_journal 'Powder Diffraction'
_publ_requested_category ?
_publ_contact_letter
;
;
#==============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
?
_journal_techeditor_code ?
_journal_paper_category ?
_iucr_compatibility_tag ?
_journal_techeditor_notes
?
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#==============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Crystal Structures of
N,N'-bis(thiophen-2-ylmethyl)ethane-1,2-diaminium Hydrochloride
and of its Au(III) Salt solved by Powder Diffraction.
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
'Silva, Silvioney A.'
; LQBin - Laboratorio de Quimica Bioinorganica
Departamento de Quimica - Instituto de Ciencias Exatas,
Universidade Federal de Juiz de Fora - UFJF
Campus Universitario, 36036-900 Juiz de Fora-MG, Brazil
;
'Masciocchi, Norberto'
; Dipartimento di Scienza e Alta Tecnologia,
Universita' dell'Insubria,
Via Valleggio 11, 22100 Como, Italy
;
'Cuin, Alexandre'
; LQBin - Laboratorio de Quimica Bioinorganica
Departamento de Quimica - Instituto de Ciencias Exatas,
Universidade Federal de Juiz de Fora - UFJF
Campus Universitario, 36036-900 Juiz de Fora-MG, Brazil
;
#==============================================================================
#data_Compound3
_chemical_name_systematic
;
N,N'-bis(thiophen-2-ylmethyl)ethane-1,2-diaminium hydrochloride
;
_chemical_name_common ?
_chemical_formula_moiety 'C12 H18 Cl2 N2 S2'
_chemical_formula_structural 'C12 H18 Cl2 N2 S2'
_chemical_formula_analytical ?
_chemical_formula_iupac ?
_chemical_formula_sum 'C12 H18 Cl2 N2 S2'
_chemical_formula_weight 325.32
_chemical_melting_point 257
_chemical_compound_source ?
loop_
_atom_type_symbol
_atom_type_description
# _atom_type_scat_dispersion_real
# _atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 'International Tables for Crystallography (Vol. IV)'
H H 'International Tables for Crystallography (Vol. IV)'
Cl Cl 'International Tables for Crystallography (Vol. IV)'
N N 'International Tables for Crystallography (Vol. IV)'
S s 'International Tables for Crystallography (Vol. IV)'
#==============================================================================
# 4. POWDER SPECIMEN AND CRYSTAL DATA
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'Iba2'
_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, z'
'-x, y, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x, -y, z+1/2'
'x, y, z'
'x+1/2, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
_cell_length_a 29.8565(1)
_cell_length_b 5.1372(2)
_cell_length_c 10.1635(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1558.9(1)
_cell_formula_units_Z 4
_cell_measurement_temperature 298
_pd_calibration_special_details
?
_cell_special_details
?
_exptl_crystal_density_diffrn 1.3862
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 680
# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.
_pd_spec_size_axial 10 # perpendicular to
# equatorial plane
_pd_spec_size_equat 25 # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick 0.08 # parallel to
# scattering vector
# in reflection
# The next five fields are character fields that describe the specimen.
_pd_spec_mounting
;
packed powder flat plate
;
_pd_spec_mount_mode reflection # options are 'reflection'
# or 'transmission'
_pd_spec_shape flat_sheet # options are 'cylinder',
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology ?
_pd_char_colour 'colorless' # use ICDD colour descriptions
# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu ?
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
#==============================================================================
# 5. EXPERIMENTAL DATA
_exptl_special_details
?
# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.
_pd_instr_location
?
_diffrn_ambient_temperature 298
_diffrn_source_target ?
_diffrn_source_type 'X-ray tube'
_diffrn_measurement_device_type 'Bruker D8 diffractometer'
_diffrn_detector_type 'Lynxeye linear PSD'
_pd_meas_scan_method step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details
?
# The following six items are used for angular dispersive measurements only.
loop_
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
# ' 1.540596 and 1.544493 '
_diffrn_radiation_monochromator 'Ni filter'
# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.
_pd_meas_number_of_points 5001
_pd_meas_2theta_range_min 5
_pd_meas_2theta_range_max 105
_pd_meas_2theta_range_inc 0.02
# The following three items are used for time-of-flight measurements only.
_pd_instr_dist_src/spec ?
_pd_instr_dist_spec/detc ?
_pd_meas_2theta_fixed ?
# The following fields are used to identify the programs used.
_computing_data_collection ?
_computing_cell_refinement 'TOPAS, Bruker AXS 2005, Karlsruhe, Germany'
_computing_data_reduction ?
_computing_structure_solution 'TOPAS, Bruker AXS 2005, Karlsruhe, Germany'
_computing_structure_refinement 'TOPAS, Bruker AXS 2005, Karlsruhe, Germany'
_computing_molecular_graphics 'SCHAKAL, E.Keller, Chemie uns. Zeit 1980,14,56'
_computing_publication_material 'TOPAS, Bruker AXS 2005, Karlsruhe, Germany'
#==============================================================================
# 6. REFINEMENT DATA
# Use the next field to give any special details about the fitting of the
# powder pattern.
_pd_proc_ls_special_details
; The use of a rigid body description for the crystallographically
independent portion of the molecule does not allow the derivation
of statistically meaningful s.u.'s for their atoms.
S.u.'s are available only for the position of the center of mass (X, Y, Z)
and for the rotational angles (RX, RY, RZ)
and torsion angles of the rigid body.
site Cl x -0.06707(3), y 0.0245(2), z -0.674
rigid body 'rigid body of the organic dication
prm ang1 240(1)
prm ang2 175(3)
z_matrix H
z_matrix C1 H 0.76
z_matrix N1 C1 1.476 H 109.3
z_matrix C2 N1 1.45 C1 117.75 H 180
z_matrix C3 C2 1.455 N1 121.4 C1 180
z_matrix C4 C3 1.360 C2 127.2 N1 180
z_matrix C5 C4 1.404 C3 112.5 C2 180
z_matrix C6 C5 1.325 C4 112.5 C3 0
z_matrix S1 C6 1.707 C5 112.5 C4 0
z_matrix H21 C2 0.95 N1 109.5 C1 60
z_matrix H22 C2 0.95 N1 109.5 C1 300
z_matrix H4 C4 0.95 C5 120 C6 180
z_matrix H5 C5 0.95 C4 120 C3 180
z_matrix H6 C6 0.95 C5 120 C4 180
z_matrix H11 C1 0.95 H 109.5 N1 120
z_matrix H12 C1 0.95 H 109.5 N1 240
z_matrix H1 N1 0.95 C1 109.5 H 60
z_matrix H2 N1 0.95 C1 109.5 H 300
z_matrix C4a C3 1.360 C2 127.2 N1 180
z_matrix C5a C4a 1.404 C3 112.5 C2 180
z_matrix C6a C5a 1.325 C4a 112.5 C3 0
z_matrix S1a C6a 1.707 C5a 112.5 C4a 0
z_matrix H4a C4a 0.95 C5a 120 C6a 180
z_matrix H5a C5a 0.95 C4a 120 C3 180
z_matrix H6a C6a 0.95 C5a 120 C4a 180
Rotate_about_points (=ang1;, C3, C2, " C4 H4 C5 H5 C6 H6 S1 ")
Rotate_about_points (=ang1-ang2;, C3, C2, " C4a H4a C5a H5a C6a H6a S1a ")
Rotate_about_points (-350(1), C2, N1,
" H21 H22 C3 C4 H4 C5 H5 C6 H6 S1 C4a H4a C5a H5a C6a H6a S1a ")
Rotate_about_points ( 51(3) , N1, C1,
" H1 H2 C2 H21 H22 C3 C4 H4 C5 H5 C6 H6 S1 C4a H4a C5a H5a C6a H6a S1a")
Rotate_about_points (-41(2), C1, H, " H11 H12 N1
H1 H2 C2 H21 H22 C3 C4 H4 C5 H5 C6 H6 S1 C4a H4a C5a H5a C6a H6a S1a")
(RX, RY, RZ) = ( -101, -248, -139 )
# esd's not available because of Rx,Ry correlation for the symmetry
# location of the molecule
(TX, TY, TZ) = ( 0.0, 0.5, 0.0892 )
;
# The next three items are given as text
_pd_proc_ls_profile_function 'fundamental parameters approach'
_pd_proc_ls_background_function 'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr ?
_pd_proc_ls_prof_R_factor 0.090
_pd_proc_ls_prof_wR_factor 0.130
_pd_proc_ls_prof_wR_expected 0.008
_refine_special_details
?
_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type fullcycle
_refine_ls_weighting_scheme sigma
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_parameters 55
_refine_ls_number_restraints ?
_refine_ls_number_constraints ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all 20.65
_refine_ls_restrained_S_all ?
_refine_ls_restrained_S_obs ?
_refine_ls_shift/su_max .01
_refine_ls_shift/su_mean ?
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min 5
_pd_proc_2theta_range_max 105
_pd_proc_2theta_range_inc 0.02
loop_
_pd_proc_wavelength 1.5418 # '1.540596 / 1.544493'
_pd_block_diffractogram_id ? # The id used for the block
# containing the powder
# pattern profile (section 11).
# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions ?
_pd_proc_info_data_reduction ?
#==============================================================================
# 7. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Cl Cl 8 -0.06707 0.02455 -0.67400 1 15
#H H 4 0.00000 0.50000 0.08924 0 15 dummy
N1 N 8 0.05958 0.52802 0.03422 1 15
H1 H 8 0.05340 0.70527 0.01470 1 15
H2 H 8 0.06698 0.43851 -0.04463 1 15
C1 C 8 0.01972 0.40700 0.09451 1 15
H11 H 8 0.02556 0.37063 0.18453 1 15
H12 H 8 0.01283 0.24959 0.04982 1 15
C2 C 8 0.10062 0.53219 0.11049 1 15
H21 H 8 0.10646 0.36298 0.14406 1 15
H22 H 8 0.09753 0.65103 0.18153 1 15
C3 C 8 0.14313 0.60675 0.05155 1 15
C4 C 8 0.16421 0.49022 -0.05143 0.84 15
H4 H 8 0.15438 0.34317 -0.10020 0.84 15
C5 C 8 0.20486 0.61200 -0.08353 0.84 15
H5 H 8 0.22255 0.54734 -0.15403 0.84 15
C6 C 8 0.21370 0.81349 -0.00639 0.84 15
H6 H 8 0.24038 0.91113 -0.01894 0.84 15
S1 S 8 0.17298 0.86410 0.10870 0.84 15
C4a C 8 0.16844 0.81896 0.08114 0.16 15
H4a H 8 0.16219 0.94998 0.14450 0.16 15
C5a C 8 0.20770 0.83262 0.00544 0.16 15
H5a H 8 0.22802 0.97288 0.01758 0.16 15
C6a C 8 0.21141 0.63574 -0.07807 0.16 15
H6a H 8 0.23669 0.62446 -0.13454 0.16 15
S1a S 8 0.16733 0.42500 -0.06838 0.16 15
# for the large isotropic B value, see text of the paper