data_Compound_2
_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 bis(tetrachloroaurate(III))
;
_chemical_name_common ?
_chemical_formula_moiety 'C12 H18 Au2 Cl8 N2 S2'
_chemical_formula_structural 'C12 H18 Au2 Cl8 N2 S2'
_chemical_formula_analytical ?
_chemical_formula_iupac ?
_chemical_formula_sum 'C12 H18 Au2 Cl8 N2 S2'
_chemical_formula_weight 931.97
_chemical_melting_point 446
_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)'
Au Au '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 monoclinic
_space_group_name_H-M_alt 'P21/c'
_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'x, y, z'
_cell_length_a 11.08294(14)
_cell_length_b 9.58516(16)
_cell_length_c 11.60544(20)
_cell_angle_alpha 90
_cell_angle_beta 75.487(13)
_cell_angle_gamma 90
_cell_volume 1193.550(46)
_cell_formula_units_Z 2
_cell_measurement_temperature 298
_pd_calibration_special_details
?
_cell_special_details
?
_exptl_crystal_density_diffrn 2.5933
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 860
# 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 'light-yellow' # 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.
rigid body 'rigid body of the [AuCl4] ion
prm dAuCl 2.280(4)
point_for_site Au ux 0 uy 0 uz 0
point_for_site Cl1 ux = dAuCl; uy 0 uz 0
point_for_site Cl2 ux 0 uy = dAuCl; uz 0
point_for_site Cl3 ux = -dAuCl; uy 0 uz 0
point_for_site Cl4 ux 0 uy = -dAuCl; uz 0
(RX, RY, RZ) = ( -254.9(2), 48.0(1), -50.0(2) )
(TX, TY, TZ) = ( 0.1645(1), 0.0200(2), 0.5328(2) )
rigid body 'rigid body of the organic dication
z_matrix H
z_matrix C1 H 0.76
z_matrix N1 C1 1.476 H 120
z_matrix C2 N1 1.476 C1 120 H 180
z_matrix C3 C2 1.455 N1 120 C1 180
z_matrix C4 C3 1.39 C2 123 N1 180
z_matrix C5 C4 1.39 C3 112 C2 180
z_matrix C6 C5 1.39 C4 112 C3 0
z_matrix S1 C6 1.707 C5 112 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 126 C6 180
z_matrix H5 C5 0.95 C4 126 C3 180
z_matrix H6 C6 0.95 C5 126 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
Rotate_about_points ( 261 (1), C3, C2, " C4 H4 C5 H5 C6 H6 S1 ")
Rotate_about_points ( -225 (2), C2, N1, " H21 H22 C3 C4 H4 C5 H5 C6 H6 S1 ")
Rotate_about_points ( 340 (2), N1, C1, " H1 H2 C2 H21 H22 C3 C4 H4 C5 H5 C6
H6 S1 ")
Rotate_about_points ( -109 (12), C1, H, " H11 H12 N1 H1 H2 C2 H21 H22 C3 C4
H4 C5 H5 C6 H6 S1 ")
(RX, RY, RZ) = ( -102(1), -192(11), -114(3) )
(TX, TY, TZ) = ( 0.0, 0.0, 0.0 )
;
# 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 0.054
_pd_proc_ls_prof_wR_factor 0.071
_pd_proc_ls_prof_wR_expected 0.010
_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 30
_refine_ls_number_restraints ?
_refine_ls_number_constraints ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all 7.006
_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
Au Au 4 0.16455 0.01998 0.53278 1 3.26(6)
Cl1 Cl 4 0.27854 -0.13188 0.39706 1 3.26(6)
Cl2 Cl 4 0.19496 -0.11697 0.68366 1 3.26(6)
Cl3 Cl 4 0.05056 0.17184 0.66850 1 3.26(6)
Cl4 Cl 4 0.13414 0.15693 0.38190 1 3.26(6)
#H H 4 0.00000 0.00000 0.00000 0 3.26(6)
N1 N 4 0.11421 -0.02647 0.10369 1 3.26(6)
H1 H 4 0.08315 -0.10608 0.15053 1 3.26(6)
H2 H 4 0.08794 0.05565 0.14884 1 3.26(6)
C1 C 4 0.06589 -0.02527 -0.00382 1 3.26(6)
H11 H 4 0.07408 -0.11936 -0.03036 1 3.26(6)
H12 H 4 0.12365 0.03138 -0.05838 1 3.26(6)
C2 C 4 0.24984 -0.03140 0.09207 1 3.26(6)
H21 H 4 0.27997 -0.12268 0.06933 1 3.26(6)
H22 H 4 0.26646 -0.00818 0.16618 1 3.26(6)
C3 C 4 0.33295 0.05897 0.00703 1 3.26(6)
C4 C 4 0.37239 0.02857 -0.11370 1 3.26(6)
H4 H 4 0.34666 -0.05354 -0.14672 1 3.26(6)
C5 C 4 0.45119 0.13093 -0.17605 1 3.26(6)
H5 H 4 0.48876 0.13106 -0.25916 1 3.26(6)
C6 C 4 0.47078 0.23802 -0.10203 1 3.26(6)
H6 H 4 0.52126 0.31816 -0.12601 1 3.26(6)
S1 S 4 0.39203 0.21085 0.04264 1 3.26(6)