#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:18:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178808 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/62/4106295.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4106295
loop_
_publ_author_name
'Tao Wu'
'Xianhui Bu'
'Xiang Zhao'
'Ripsime Khazhakyan'
'Pingyun Feng'
_publ_section_title
;
 Phase Selection and Site-Selective Distribution by Tin and Sulfur in
 Supertetrahedral Zinc Gallium Selenides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9616
_journal_page_last               9625
_journal_paper_doi               10.1021/ja203143q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'Ga16 N2 S16.11 Se16.89 Zn4'
_chemical_formula_weight         3255.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.8934(12)
_cell_length_b                   22.8934(12)
_cell_length_c                   41.516(4)
_cell_measurement_reflns_used    185
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      4.4
_cell_volume                     21759(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            43681
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    10.718
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_meas      ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             11696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       0.000057(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3128
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1379P)²+1062.1071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2793
_reflns_number_gt                1881
_reflns_number_total             3128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203143q_si_002_03.cif
_cod_data_source_block           OCF-5-ZnGaSeS-AEP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4106295
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ga1 Ga 0.68936(9) 0.10114(9) 0.03050(5) 0.0409(7) Uani 1 1 d .
Ga2 Ga 0.67886(9) 0.21256(9) 0.09284(5) 0.0379(7) Uani 1 1 d .
Ga3 Ga 0.57790(9) 0.08451(9) 0.09297(5) 0.0381(7) Uani 1 1 d .
Ga4 Ga 0.56467(9) 0.19953(9) 0.02927(5) 0.0383(7) Uani 1 1 d .
Zn5 Zn 0.56455(11) 0.19872(11) 0.15707(6) 0.0555(9) Uani 1 1 d .
Se1 Se 0.7500 0.03940(16) 0.0000 0.0512(17) Uani 0.654(17) 2 d SP
Se2 Se 0.74836(12) 0.16406(13) 0.06154(7) 0.0488(13) Uani 0.545(13) 1 d P
Se3 Se 0.64127(13) 0.02830(12) 0.06149(7) 0.0519(13) Uani 0.584(13) 1 d P
Se4 Se 0.62762(13) 0.15118(13) -0.00560(7) 0.0523(14) Uani 0.517(13) 1 d P
Se5 Se 0.63206(14) 0.14567(14) 0.12674(8) 0.0457(15) Uani 0.366(12) 1 d P
Se6 Se 0.52746(11) 0.01599(11) 0.12509(6) 0.0518(11) Uani 0.758(13) 1 d P
Se7 Se 0.61835(14) 0.26817(13) 0.05909(7) 0.0451(14) Uani 0.412(13) 1 d P
Se8 Se 0.51074(14) 0.13210(14) 0.05948(8) 0.0443(15) Uani 0.349(12) 1 d P
Se9 Se 0.5000 0.2500 -0.00514(8) 0.0511(15) Uani 0.727(16) 2 d SP
Se10 Se 0.5000 0.2500 0.1250 0.036(4) Uani 0.00(2) 4 d SP
S1 S 0.7500 0.03940(16) 0.0000 0.0512(17) Uani 0.346(17) 2 d SP
S2 S 0.74836(12) 0.16406(13) 0.06154(7) 0.0488(13) Uani 0.455(13) 1 d P
S3 S 0.64127(13) 0.02830(12) 0.06149(7) 0.0519(13) Uani 0.416(14) 1 d P
S4 S 0.62762(13) 0.15118(13) -0.00560(7) 0.0523(14) Uani 0.483(13) 1 d P
S5 S 0.63206(14) 0.14567(14) 0.12674(8) 0.0457(15) Uani 0.634(13) 1 d P
S6 S 0.52746(11) 0.01599(11) 0.12509(6) 0.0518(11) Uani 0.242(13) 1 d P
S7 S 0.61835(14) 0.26817(13) 0.05909(7) 0.0451(14) Uani 0.588(13) 1 d P
S8 S 0.51074(14) 0.13210(14) 0.05948(8) 0.0443(15) Uani 0.651(12) 1 d P
S9 S 0.5000 0.2500 -0.00514(8) 0.0511(15) Uani 0.273(16) 2 d SP
S10 S 0.5000 0.2500 0.1250 0.036(4) Uani 1.00(2) 4 d SP
N1 N 0.7500 0.270(3) 0.0000 0.21(2) Uiso 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
Se1 Ga1 Se4 107.68(11) . .
Se1 Ga1 Se2 108.86(11) . .
Se4 Ga1 Se2 113.21(14) . .
Se1 Ga1 Se3 98.24(12) . .
Se4 Ga1 Se3 114.04(14) . .
Se2 Ga1 Se3 113.46(13) . .
Se2 Ga2 Se5 109.60(13) . .
Se2 Ga2 Se7 109.16(13) . .
Se5 Ga2 Se7 116.36(14) . .
Se2 Ga2 S6 104.40(12) . 20_656
Se5 Ga2 S6 108.51(13) . 20_656
Se7 Ga2 S6 108.13(13) . 20_656
Se2 Ga2 Se6 104.40(12) . 20_656
Se5 Ga2 Se6 108.51(13) . 20_656
Se7 Ga2 Se6 108.13(13) . 20_656
S6 Ga2 Se6 0.00(13) 20_656 20_656
Se5 Ga3 Se3 109.62(14) . .
Se5 Ga3 Se8 115.19(15) . .
Se3 Ga3 Se8 109.37(14) . .
Se5 Ga3 Se6 108.58(13) . .
Se3 Ga3 Se6 104.69(12) . .
Se8 Ga3 Se6 108.87(13) . .
Se4 Ga4 Se8 110.29(14) . .
Se4 Ga4 Se7 108.83(14) . .
Se8 Ga4 Se7 115.78(14) . .
Se4 Ga4 Se9 104.20(13) . .
Se8 Ga4 Se9 108.44(12) . .
Se7 Ga4 Se9 108.65(11) . .
Se10 Zn5 S8 111.65(13) . 20_656
Se10 Zn5 Se8 111.65(13) . 20_656
S8 Zn5 Se8 0.00(18) 20_656 20_656
Se10 Zn5 Se5 112.15(13) . .
S8 Zn5 Se5 106.94(15) 20_656 .
Se8 Zn5 Se5 106.94(15) 20_656 .
Se10 Zn5 Se7 112.94(13) . 27_565
S8 Zn5 Se7 106.27(15) 20_656 27_565
Se8 Zn5 Se7 106.27(15) 20_656 27_565
Se5 Zn5 Se7 106.46(15) . 27_565
Se10 Zn5 S7 112.94(13) . 27_565
S8 Zn5 S7 106.27(15) 20_656 27_565
Se8 Zn5 S7 106.27(15) 20_656 27_565
Se5 Zn5 S7 106.46(15) . 27_565
Se7 Zn5 S7 0.0(2) 27_565 27_565
Ga1 Se1 Ga1 106.10(17) . 5_655
Ga2 Se2 Ga1 101.78(13) . .
Ga3 Se3 Ga1 101.76(13) . .
Ga4 Se4 Ga1 101.97(14) . .
Zn5 Se5 Ga3 106.50(15) . .
Zn5 Se5 Ga2 106.69(15) . .
Ga3 Se5 Ga2 105.91(15) . .
Ga3 Se6 Ga2 105.74(12) . 27_565
Zn5 Se7 Ga2 106.00(14) 20_656 .
Zn5 Se7 Ga4 106.10(15) 20_656 .
Ga2 Se7 Ga4 105.12(14) . .
Zn5 Se8 Ga4 107.15(15) 27_565 .
Zn5 Se8 Ga3 106.86(15) 27_565 .
Ga4 Se8 Ga3 106.18(15) . .
Ga4 Se9 Ga4 105.48(16) . 10_554
Zn5 Se10 Zn5 109.41(6) 27_565 .
Zn5 Se10 Zn5 109.41(6) 27_565 10_554
Zn5 Se10 Zn5 109.59(12) . 10_554
Zn5 Se10 Zn5 109.59(12) 27_565 20_656
Zn5 Se10 Zn5 109.41(6) . 20_656
Zn5 Se10 Zn5 109.41(6) 10_554 20_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 Se1 2.351(3) .
Ga1 Se4 2.357(4) .
Ga1 Se2 2.358(4) .
Ga1 Se3 2.376(4) .
Ga2 Se2 2.335(3) .
Ga2 Se5 2.340(4) .
Ga2 Se7 2.346(4) .
Ga2 S6 2.361(3) 20_656
Ga2 Se6 2.361(3) 20_656
Ga3 Se5 2.337(4) .
Ga3 Se3 2.338(3) .
Ga3 Se8 2.342(4) .
Ga3 Se6 2.361(3) .
Ga4 Se4 2.323(4) .
Ga4 Se8 2.341(4) .
Ga4 Se7 2.348(4) .
Ga4 Se9 2.360(3) .
Zn5 Se10 2.310(3) .
Zn5 S8 2.331(4) 20_656
Zn5 Se8 2.331(4) 20_656
Zn5 Se5 2.335(4) .
Zn5 Se7 2.336(4) 27_565
Zn5 S7 2.336(4) 27_565
Se1 Ga1 2.351(3) 5_655
Se6 Ga2 2.361(3) 27_565
Se7 Zn5 2.336(4) 20_656
Se8 Zn5 2.331(4) 27_565
Se9 Ga4 2.360(3) 10_554
Se10 Zn5 2.310(3) 27_565
Se10 Zn5 2.310(3) 10_554
Se10 Zn5 2.310(3) 20_656
