#------------------------------------------------------------------------------
#$Date: 2019-11-16 04:01:12 +0100 (Sat 16 de Nov de 2019) $
#$Revision: 227928 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/19/7701945.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_7701945
loop_
_publ_author_name
'Xing, Wen-Hao'
'Wang, Naizheng'
'Guo, Yangwu'
'Li, Zhuang'
'Tang, Jian'
'Kang, Kaijin'
'Yin, Wenlong'
'Lin, Zheshuai'
'Yao, Jiyong'
'Bin, Kang'
_publ_section_title
;
 Two rare-earth-based quaternary chalcogenides EuCdGeQ4 (Q = S, Se) with
 strong second-harmonic generation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03755A
_journal_year                    2019
_chemical_formula_moiety         '0.25(Cd4 Eu4 Ge4 Se16)'
_chemical_formula_sum            'Cd Eu Ge Se4'
_chemical_formula_weight         652.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_audit_creation_date             2019-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-16 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7525(8)
_cell_length_b                   10.6275(8)
_cell_length_c                   6.6740(5)
_cell_measurement_reflns_used    2298
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      3.60
_cell_volume                     762.65(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.173
_diffrn_reflns_theta_min         3.605
_exptl_absorpt_coefficient_mu    33.777
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.497108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.1358 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.4971.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    5.685
_exptl_crystal_description       IRREGULAR
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.552
_refine_diff_density_min         -1.769
_refine_diff_density_rms         0.335
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0333P)²+1.3666P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                1359
_reflns_number_total             1514
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03755a2.cif
_cod_data_source_block           ama2_CCDC1
_cod_database_code               7701945
_shelxl_version_number           2013-2
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(3)
;
_shelx_res_file
;
TITL Ama2 in Ama2
REM OMIT 4.00 180.00
CELL 0.71073 10.7525 10.6275 6.674 90 90 90
ZERR 4 0.0008 0.0008 0.0005 0 0 0
LATT -5
SYMM -X,-Y,+Z
SYMM 0.5+X,-Y,+Z
SYMM 0.5-X,+Y,+Z
SFAC Cd Eu Ge Se
UNIT 4 4 4 16

L.S. 4
PLAN  20
TEMP 23
fmap 2
acta
MERG 2
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\Ama2.hkl">
REM </olex2.extras>

WGHT    0.033300    1.366600
EXTI    0.002333
BASF   0.06072
FVAR       0.21288
EU    2    0.500000    0.000000    0.641948    10.50000    0.01589    0.01580 =
         0.02001    0.00000    0.00000    0.00146
GE    3    0.750000    0.220219    0.155221    10.50000    0.01337    0.01393 =
         0.01152    0.00021    0.00000    0.00000
SE1   4    0.750000    0.063479    0.398872    10.50000    0.01869    0.01655 =
         0.01710    0.00635    0.00000    0.00000
SE2   4    0.574912    0.230368    0.941182    11.00000    0.01500    0.01692 =
         0.01824   -0.00319   -0.00286    0.00006
SE3   4    0.250000    0.088462    0.840313    10.50000    0.01703    0.01455 =
         0.01147   -0.00068    0.00000    0.00000
CD    1    0.750000   -0.168221    0.202678    10.50000    0.03520    0.03720 =
         0.01555    0.00971    0.00000    0.00000
HKLF 4

REM  Ama2 in Ama2
REM R1 =  0.0316 for    1359 Fo > 4sig(Fo)  and  0.0386 for all    1514 data
REM     41 parameters refined using      1 restraints

END

WGHT      0.0333      1.3667

REM Highest difference peak  2.552,  deepest hole -1.769,  1-sigma level  0.335
Q1    1   0.7500 -0.2188  0.1348  10.50000  0.05    2.55
Q2    1   0.2500  0.1741  0.7234  10.50000  0.05    1.76
Q3    1   0.2500 -0.0747  0.8710  10.50000  0.05    1.73
Q4    1   0.7500 -0.0706  0.4132  10.50000  0.05    1.66
Q5    1   0.7500  0.1600  0.1974  10.50000  0.05    1.65
Q6    1   0.4285  0.2355  0.9464  11.00000  0.05    1.32
Q7    1   0.5775  0.3404  0.9304  11.00000  0.05    1.28
Q8    1   0.4904  0.0541  0.7314  11.00000  0.05    1.28
Q9    1   0.2500  0.0791  1.0274  10.50000  0.05    1.20
Q10   1   0.5802  0.0918  0.7189  11.00000  0.05    1.18
Q11   1   0.6703  0.0726  0.3747  11.00000  0.05    1.18
Q12   1   0.4947  0.0476  1.1504  11.00000  0.05    1.17
Q13   1   0.6807 -0.0048  0.4328  11.00000  0.05    1.15
Q14   1   0.7500  0.1581  0.0555  10.50000  0.05    1.13
Q15   1   0.5927  0.1579  0.8032  11.00000  0.05    1.09
Q16   1   0.7500  0.0502  0.5862  10.50000  0.05    1.07
Q17   1   0.5774  0.1025  0.5836  11.00000  0.05    1.07
Q18   1   0.4384  0.1046  0.6228  11.00000  0.05    1.05
Q19   1   0.5075  0.1569  0.8820  11.00000  0.05    1.04
Q20   1   0.5137  0.1019  0.8240  11.00000  0.05    1.03
;
_shelx_res_checksum              31543
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Eu Eu 0.5000 0.0000 0.64195(11) 0.01723(17) Uani 1 2 d S T P
Ge Ge 0.7500 0.22022(13) 0.1552(2) 0.0129(3) Uani 1 2 d S T P
Se1 Se 0.7500 0.06348(13) 0.3989(2) 0.0174(3) Uani 1 2 d S T P
Se2 Se 0.57491(9) 0.23037(9) 0.94118(16) 0.0167(2) Uani 1 1 d . . .
Se3 Se 0.2500 0.08846(14) 0.84031(19) 0.0144(3) Uani 1 2 d S T P
Cd Cd 0.7500 -0.16822(13) 0.20268(17) 0.0293(3) Uani 1 2 d S T P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Eu 0.0159(3) 0.0158(3) 0.0200(3) 0.000 0.000 0.0015(2)
Ge 0.0134(6) 0.0139(6) 0.0115(6) 0.0002(6) 0.000 0.000
Se1 0.0187(7) 0.0166(7) 0.0171(7) 0.0063(5) 0.000 0.000
Se2 0.0150(4) 0.0169(5) 0.0182(4) -0.0032(4) -0.0029(4) 0.0001(3)
Se3 0.0170(6) 0.0146(6) 0.0115(5) -0.0007(5) 0.000 0.000
Cd 0.0352(7) 0.0372(7) 0.0155(5) 0.0097(5) 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'
Se Se -0.0929 2.2259 '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 Eu Se1 119.31(5) 2_655 .
Se1 Eu Se2 86.84(3) . .
Se1 Eu Se2 76.73(3) 2_655 6_654
Se1 Eu Se2 86.84(3) 2_655 2_655
Se1 Eu Se2 79.33(3) 2_655 5_544
Se1 Eu Se2 132.37(3) . 2_655
Se1 Eu Se2 79.33(3) . 6_654
Se1 Eu Se2 132.37(3) 2_655 .
Se1 Eu Se2 76.73(3) . 5_544
Se2 Eu Se2 131.53(4) 5_544 6_654
Se2 Eu Se2 148.17(3) . 5_544
Se2 Eu Se2 69.711(14) . 6_654
Se2 Eu Se2 69.711(14) 2_655 5_544
Se2 Eu Se2 148.17(3) 2_655 6_654
Se2 Eu Se2 104.46(4) 2_655 .
Se3 Eu Se1 150.06(4) . .
Se3 Eu Se1 150.06(4) 2_655 2_655
Se3 Eu Se1 63.85(3) 2_655 .
Se3 Eu Se1 63.85(3) . 2_655
Se3 Eu Se2 130.32(3) . 5_544
Se3 Eu Se2 75.83(3) 2_655 .
Se3 Eu Se2 74.24(3) . .
Se3 Eu Se2 72.48(3) 2_655 5_544
Se3 Eu Se2 74.25(3) 2_655 2_655
Se3 Eu Se2 75.82(3) . 2_655
Se3 Eu Se2 130.32(3) 2_655 6_654
Se3 Eu Se2 72.48(3) . 6_654
Se3 Eu Se3 130.13(5) . 2_655
Se1 Ge Se2 117.03(5) . 4_654
Se1 Ge Se2 117.03(5) . 1_554
Se1 Ge Se3 104.41(8) . 6_654
Se2 Ge Se2 105.46(7) 1_554 4_654
Se2 Ge Se3 105.94(5) 4_654 6_654
Se2 Ge Se3 105.94(5) 1_554 6_654
Eu Se1 Eu 113.66(5) . 3
Ge Se1 Eu 120.21(3) . 3
Ge Se1 Eu 120.21(3) . .
Ge Se1 Cd 107.69(7) . .
Cd Se1 Eu 92.96(3) . .
Cd Se1 Eu 92.96(3) . 3
Eu Se2 Eu 148.17(3) . 5
Ge Se2 Eu 122.16(5) 1_556 .
Ge Se2 Eu 89.34(5) 1_556 5
Ge Se2 Cd 79.55(4) 1_556 5
Cd Se2 Eu 96.39(4) 5 .
Cd Se2 Eu 93.66(4) 5 5
Eu Se3 Eu 117.73(5) 3_455 .
Ge Se3 Eu 92.12(4) 6_655 .
Ge Se3 Eu 92.12(4) 6_655 3_455
Ge Se3 Cd 101.97(8) 6_655 2_656
Cd Se3 Eu 119.79(2) 2_656 3_455
Cd Se3 Eu 119.79(2) 2_656 .
Se2 Cd Se1 94.35(4) 5_544 .
Se2 Cd Se1 94.35(4) 8_644 .
Se2 Cd Se2 88.80(5) 8_644 5_544
Se3 Cd Se1 98.69(6) 2_654 .
Se3 Cd Se2 133.69(3) 2_654 8_644
Se3 Cd Se2 133.69(3) 2_654 5_544
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu Se1 3.2114(8) 2_655
Eu Se1 3.2114(8) .
Eu Se2 3.2643(11) 6_654
Eu Se2 3.2643(11) 5_544
Eu Se2 3.2605(11) 2_655
Eu Se2 3.2605(11) .
Eu Se3 3.1405(8) 2_655
Eu Se3 3.1405(8) .
Ge Se1 2.328(2) .
Ge Se2 2.3657(13) 1_554
Ge Se2 2.3657(13) 4_654
Ge Se3 2.379(2) 6_654
Se1 Eu 3.2114(8) 3
Se1 Cd 2.789(2) .
Se2 Eu 3.2643(11) 5
Se2 Ge 2.3657(13) 1_556
Se2 Cd 2.6906(13) 5
Se3 Eu 3.1405(8) 3_455
Se3 Ge 2.379(2) 6_655
Se3 Cd 2.5627(17) 2_656
Cd Se2 2.6906(13) 8_644
Cd Se2 2.6906(13) 5_544
Cd Se3 2.5627(17) 2_654
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.94(3)
2 0.06(3)
