##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_global
_audit_creation_method     'form.cif (version 2.0)'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2019-06-21
_journal_date_accepted     2019-07-26
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2019
_journal_volume     75
_journal_issue      9
_journal_page_first     1291
_journal_page_last     1296
_journal_paper_category     GI
_journal_paper_doi     10.1107/S2056989019010636
_journal_coeditor_code     VN2150
_publ_contact_author_name     'Brian J. Riley'
_publ_contact_author_address
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
_publ_contact_author_email     'brian.riley@pnnl.gov'
_publ_contact_author_fax     ?
_publ_contact_author_phone     ?
_publ_section_title
;
Crystal structure and chemistry of tricadmium digermanium tetraarsenide,
Cd₃Ge₂As₄
;
_publ_section_title_footnote     .
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Thompson, Michael R.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Riley, Brian J.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Bowden, Mark E.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Olszta, Matthew J.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Edwards, Danny J.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Crum, Jarrod V.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Johnson, Bradley R.' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
    'Chong, Saehwa' .
;
Pacific Northwest National Laboratory, Richland, WA 99354, USA
;
_publ_section_synopsis
;
A cadmium germanium arsenide compound, Cd₃Ge₂As₄, was synthesized using a
double-containment fused quartz ampoule method within a rocking furnace and a
melt-quench technique. The crystal structure was determined from
single-crystal X-ray diffraction, scanning and transmission electron
microscopies, and selected area diffraction and confirmed with electron
backscatter diffraction. The chemistry was verified with electron energy loss
spectroscopy.
;
data_I
_chemical_name_systematic
;
Tricadmium digermanium tetraarsenide
;
_chemical_name_common     ?
_chemical_formula_moiety     ?
_chemical_formula_sum     'Cd3 Ge2 As4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac     'Cd3 Ge2 As4'
_chemical_formula_weight     782.06
_chemical_melting_point     ?
_symmetry_cell_setting     trigonal
_symmetry_space_group_name_H-M     'R -3'
_symmetry_space_group_name_Hall     '-R 3'
loop_
    _space_group_symop_operation_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'
_cell_length_a     7.3748(13)
_cell_length_b     7.3748(13)
_cell_length_c     27.415(5)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     120
_cell_volume     1291.3(5)
_cell_formula_units_Z     6
_cell_measurement_reflns_used     20756
_cell_measurement_theta_min     2.229
_cell_measurement_theta_max     42.350
_cell_measurement_temperature     150
_exptl_crystal_description     'triangular prism'
_exptl_crystal_colour     'black'
_exptl_crystal_size_max     0.070
_exptl_crystal_size_mid     0.070
_exptl_crystal_size_min     0.030
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     6.034
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     2040
_exptl_absorpt_coefficient_mu     29.357
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_absorpt_correction_T_min     0.147
_exptl_absorpt_correction_T_max     0.414
_exptl_special_details     ?
_diffrn_ambient_temperature     150
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     ?
_diffrn_radiation_monochromator     ?
_diffrn_measurement_device_type     'Bruker APEXII CCD area detector'
_diffrn_measurement_method     'ω and φ scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     20756
_diffrn_reflns_av_R_equivalents     0.0618
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_theta_min     2.229
_diffrn_reflns_theta_max     42.350
_diffrn_reflns_theta_full     25.242
_diffrn_measured_fraction_theta_max     0.986
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     13
_diffrn_reflns_limit_k_min     -13
_diffrn_reflns_limit_k_max     13
_diffrn_reflns_limit_l_min     -51
_diffrn_reflns_limit_l_max     51
_diffrn_reflns_reduction_process     ?
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    ? ? ?
_refine_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_number_total     2026
_reflns_number_gt     1702
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0362
_refine_ls_R_factor_gt     0.0253
_refine_ls_wR_factor_all     ?
_refine_ls_wR_factor_ref     0.0491
_refine_ls_goodness_of_fit_all     1.032
_refine_ls_goodness_of_fit_ref     1.032
_refine_ls_restrained_S_all     1.032
_refine_ls_restrained_S_obs     ?
_refine_ls_number_reflns     2026
_refine_ls_number_parameters     29
_refine_ls_number_restraints     0
_refine_ls_number_constraints     ?
_refine_ls_hydrogen_treatment     ?
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
             'w=1/[σ²(Fo²)+(0.0102P)²+16.7635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.996
_refine_diff_density_min     -2.180
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_extinction_coef     0.00068(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details     ?
_refine_ls_abs_structure_Flack     ?
_refine_ls_abs_structure_Rogers     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'As' 'As' 0.0499 2.0058
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Cd' 'Cd' -0.8075 1.2024
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ge' 'Ge' 0.1547 1.8001
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_cell_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_molecular_graphics
;
VESTA (Momma & Izumi, 2011)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Cd Cd1 0.63686(3) 0.64317(3) 0.05011(2) 0.01073(5) Uani d 1 . .
    As As1 0.49777(4) 0.50674(4) 0.14283(2) 0.00577(5) Uani d 1 . .
    As As2 1.000000 1.000000 0.15184(2) 0.00553(7) Uani d 1 . .
    Ge Ge1 1.000000 1.000000 0.06367(2) 0.00604(8) Uani d 1 . .
    Ge Ge2 0.666667 0.333333 0.00242(2) 0.00535(7) Uani d 1 . .
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
    Cd1 Ge1 . 2.6810(5) ?
    Cd1 Ge2 . 2.7352(5) ?
    Cd1 As1 . 2.7374(5) ?
    Cd1 Ge2 10_665 2.7390(5) ?
    Cd1 Cd1 10_665 3.4379(6) ?
    As1 As2 13_665 2.4296(5) ?
    As1 As1 14_455 2.4496(5) ?
    As1 As1 15 2.4496(5) ?
    As2 Ge1 . 2.4172(8) ?
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
    Ge1 Cd1 Ge2 . . 115.352(9) ?
    Ge1 Cd1 As1 . . 103.815(15) ?
    Ge2 Cd1 As1 . . 107.978(14) ?
    Ge1 Cd1 Ge2 . 10_665 117.239(9) ?
    Ge2 Cd1 Ge2 . 10_665 102.189(11) ?
    As1 Cd1 Ge2 . 10_665 110.095(15) ?
    Ge1 Cd1 Cd1 . 10_665 134.854(15) ?
    Ge2 Cd1 Cd1 . 10_665 51.144(9) ?
    As1 Cd1 Cd1 . 10_665 121.283(16) ?
    Ge2 Cd1 Cd1 10_665 10_665 51.045(9) ?
    As2 As1 As1 13_665 14_455 97.897(17) ?
    As2 As1 As1 13_665 15 99.093(17) ?
    As1 As1 As1 14_455 15 94.181(17) ?
    As2 As1 Cd1 13_665 . 113.706(15) ?
    As1 As1 Cd1 14_455 . 140.455(14) ?
    As1 As1 Cd1 15 . 103.154(16) ?
    Ge1 As2 As1 . 13_665 115.864(13) ?
    Ge1 As2 As1 . 14_565 115.864(13) ?
    As1 As2 As1 13_665 14_565 102.389(15) ?
    Ge1 As2 As1 . 15 115.864(13) ?
    As1 As2 As1 13_665 15 102.389(15) ?
    As1 As2 As1 14_565 15 102.388(15) ?
    As2 Ge1 Cd1 . . 97.973(11) ?
    As2 Ge1 Cd1 . 2_765 97.973(11) ?
    Cd1 Ge1 Cd1 . 2_765 118.108(5) ?
    As2 Ge1 Cd1 . 3_675 97.973(11) ?
    Cd1 Ge1 Cd1 . 3_675 118.109(5) ?
    Cd1 Ge1 Cd1 2_765 3_675 118.108(5) ?
    Cd1 Ge2 Cd1 3_665 2_655 99.051(15) ?
    Cd1 Ge2 Cd1 3_665 . 99.050(14) ?
    Cd1 Ge2 Cd1 2_655 . 99.050(14) ?
    Cd1 Ge2 Cd1 3_665 11 88.526(12) ?
    Cd1 Ge2 Cd1 2_655 11 77.810(11) ?
    Cd1 Ge2 Cd1 . 11 172.207(10) ?
    Cd1 Ge2 Cd1 3_665 12_655 77.810(11) ?
    Cd1 Ge2 Cd1 2_655 12_655 172.207(10) ?
    Cd1 Ge2 Cd1 . 12_655 88.526(11) ?
    Cd1 Ge2 Cd1 11 12_655 94.898(15) ?
    Cd1 Ge2 Cd1 3_665 10_665 172.207(10) ?
    Cd1 Ge2 Cd1 2_655 10_665 88.526(11) ?
    Cd1 Ge2 Cd1 . 10_665 77.810(11) ?
    Cd1 Ge2 Cd1 11 10_665 94.898(15) ?
    Cd1 Ge2 Cd1 12_655 10_665 94.898(15) ?
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_T_min     0.233
_shelx_estimated_absorpt_T_max     0.473
