#------------------------------------------------------------------------------
#$Date: 2021-02-04 23:45:03 +0100 (jue 04 de feb de 2021) $
#$Revision: 261565 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/76/7127638.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_7127638
loop_
_publ_author_name
'Li, Jia-Nuo'
'Yao, Wen-Dong'
'Li, Xiao-Hui'
'Liu, Wenlong'
'Xue, Huai-Guo'
'Guo, Sheng-Ping'
_publ_section_title
;
 A novel promising infrared nonlinear optical selenide
 KAg₃Ga₈Se₁₄ designed from benchmark
 AgGaQ₂ (Q = S, Se).
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1109
_journal_page_last               1112
_journal_paper_doi               10.1039/d0cc07396b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '0.5(Ag6 Ga16 K2 Se28)'
_chemical_formula_sum            'Ag3 Ga8 K Se14'
_chemical_formula_weight         2025.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2020-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.9980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8805(5)
_cell_length_b                   11.6857(4)
_cell_length_c                   9.6600(4)
_cell_measurement_reflns_used    6594
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.30
_cell_measurement_theta_min      2.35
_cell_volume                     1306.87(9)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.346
_exptl_absorpt_coefficient_mu    29.945
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.3408
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1629 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.4562.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.148
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.036(13)
_refine_ls_extinction_coef       0.00136(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0250
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2939
_reflns_number_total             3130
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc07396b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7127638.cif.'
_cod_database_code               7127638
_shelx_shelxl_version_number     2014/7
_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: 0.964(13)
 0.036(13)
;
_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+1/2, z'
'x+1/2, -y+1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K -0.7337(4) -0.5000 -0.2975(5) 0.0567(13) Uani 1 2 d S T P . .
Ag1 Ag -0.31045(10) -0.5000 -0.36985(13) 0.0276(3) Uani 1 2 d S T P . .
Ag2 Ag -0.60302(10) -1.0000 -0.57574(13) 0.0279(3) Uani 1 2 d S T P . .
Ag3 Ag -0.38685(10) -1.0000 -0.82063(13) 0.0262(3) Uani 1 2 d S T P . .
Ga1 Ga -0.19948(8) -0.66594(8) 0.00181(10) 0.0108(2) Uani 1 1 d . . . . .
Ga2 Ga -0.60928(9) -0.66984(7) -0.59502(12) 0.0112(2) Uani 1 1 d . . . . .
Ga3 Ga -0.40289(8) -0.67114(8) -0.79961(10) 0.0110(2) Uani 1 1 d . . . . .
Ga4 Ga -0.50582(9) -0.83511(8) -0.20484(12) 0.0116(2) Uani 1 1 d . . . . .
Se1 Se -0.20019(7) -0.69307(7) -0.24291(10) 0.01251(18) Uani 1 1 d . . . . .
Se2 Se -0.30540(8) -0.82471(8) -0.63471(10) 0.0127(2) Uani 1 1 d . . . . .
Se3 Se -0.53528(10) -0.5000 -0.44412(14) 0.0117(3) Uani 1 2 d S T P . .
Se4 Se -0.40442(7) -0.66288(7) -1.05189(9) 0.01030(19) Uani 1 1 d . . . . .
Se5 Se -0.38923(10) -1.0000 -0.08858(14) 0.0126(3) Uani 1 2 d S T P . .
Se6 Se -0.48677(8) -0.81886(8) -0.43977(10) 0.01165(19) Uani 1 1 d . . . . .
Se7 Se -0.60669(8) -0.66312(7) -0.84952(10) 0.01005(18) Uani 1 1 d . . . . .
Se8 Se -0.32449(11) -0.5000 -0.65792(14) 0.0133(3) Uani 1 2 d S T P . .
Se9 Se -0.60593(11) -1.0000 -0.85578(13) 0.0136(3) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
_geom_angle_publ_flag
Se1 K1 Se1 163.66(15) 3_455 4_435 ?
Se2 K1 Se1 131.32(11) 4_435 3_455 ?
Se2 K1 Se1 62.39(3) 4_435 4_435 ?
Se2 K1 Se1 62.39(3) 3_455 3_455 ?
Se2 K1 Se1 131.32(11) 3_455 4_435 ?
Se2 K1 Se2 69.17(8) 4_435 3_455 ?
Se2 K1 Se6 99.09(11) 4_435 3_455 ?
Se2 K1 Se6 59.54(6) 4_435 4_435 ?
Se2 K1 Se6 99.09(11) 3_455 4_435 ?
Se2 K1 Se6 59.54(6) 3_455 3_455 ?
Se3 K1 Se1 89.84(6) . 3_455 ?
Se3 K1 Se1 89.84(6) . 4_435 ?
Se3 K1 Se2 64.43(6) . 4_435 ?
Se3 K1 Se2 64.43(6) . 3_455 ?
Se3 K1 Se6 123.72(10) . 3_455 ?
Se3 K1 Se6 123.72(10) . 4_435 ?
Se5 K1 Se1 88.70(6) 3_455 4_435 ?
Se5 K1 Se1 88.70(6) 3_455 3_455 ?
Se5 K1 Se2 123.37(10) 3_455 3_455 ?
Se5 K1 Se2 123.37(10) 3_455 4_435 ?
Se5 K1 Se3 169.70(16) 3_455 . ?
Se5 K1 Se6 63.86(6) 3_455 4_435 ?
Se5 K1 Se6 63.86(6) 3_455 3_455 ?
Se6 K1 Se1 131.69(11) 4_435 3_455 ?
Se6 K1 Se1 131.69(11) 3_455 4_435 ?
Se6 K1 Se1 60.38(4) 3_455 3_455 ?
Se6 K1 Se1 60.38(4) 4_435 4_435 ?
Se6 K1 Se6 71.69(8) 4_435 3_455 ?
Se1 Ag1 Se1 115.92(5) 2_545 . ?
Se1 Ag1 Se8 104.79(4) 2_545 . ?
Se1 Ag1 Se8 104.79(4) . . ?
Se3 Ag1 Se1 114.97(3) . 2_545 ?
Se3 Ag1 Se1 114.97(3) . . ?
Se3 Ag1 Se8 98.53(5) . . ?
Se6 Ag2 Se6 109.44(6) 2_535 . ?
Se6 Ag2 Se8 117.81(4) . 3_445 ?
Se6 Ag2 Se8 117.81(4) 2_535 3_445 ?
Se6 Ag2 Se9 105.06(4) 2_535 . ?
Se6 Ag2 Se9 105.06(4) . . ?
Se8 Ag2 Se9 99.38(5) 3_445 . ?
Se2 Ag3 Se2 102.80(6) . 2_535 ?
Se2 Ag3 Se9 99.74(4) 2_535 . ?
Se2 Ag3 Se9 99.74(4) . . ?
Se5 Ag3 Se2 120.90(4) 1_554 2_535 ?
Se5 Ag3 Se2 120.90(4) 1_554 . ?
Se5 Ag3 Se9 108.87(5) 1_554 . ?
Se1 Ga1 Se4 104.83(5) . 1_556 ?
Se1 Ga1 Se7 105.22(5) . 4_536 ?
Se7 Ga1 Se4 109.83(5) 4_536 1_556 ?
Se9 Ga1 Se1 117.61(5) 3_556 . ?
Se9 Ga1 Se4 109.60(6) 3_556 1_556 ?
Se9 Ga1 Se7 109.47(5) 3_556 4_536 ?
Se2 Ga2 Se3 103.33(5) 4_435 . ?
Se2 Ga2 Se6 116.34(5) 4_435 . ?
Se2 Ga2 Se7 108.41(5) 4_435 . ?
Se3 Ga2 Se7 113.75(5) . . ?
Se6 Ga2 Se3 104.16(5) . . ?
Se6 Ga2 Se7 110.75(5) . . ?
Se2 Ga3 Se4 118.33(5) . . ?
Se2 Ga3 Se7 111.60(5) . . ?
Se2 Ga3 Se8 106.50(5) . . ?
Se4 Ga3 Se7 105.29(4) . . ?
Se8 Ga3 Se4 110.96(5) . . ?
Se8 Ga3 Se7 103.19(5) . . ?
Se1 Ga4 Se4 102.76(5) 4_435 1_556 ?
Se1 Ga4 Se5 125.58(5) 4_435 . ?
Se1 Ga4 Se6 112.28(5) 4_435 . ?
Se5 Ga4 Se4 108.20(5) . 1_556 ?
Se6 Ga4 Se4 104.61(5) . 1_556 ?
Se6 Ga4 Se5 101.78(4) . . ?
Ag1 Se1 K1 140.04(8) . 3_545 ?
Ga1 Se1 K1 102.98(7) . 3_545 ?
Ga1 Se1 Ag1 96.52(4) . . ?
Ga1 Se1 Ga4 106.33(5) . 4_535 ?
Ga4 Se1 K1 102.06(7) 4_535 3_545 ?
Ga4 Se1 Ag1 105.41(4) 4_535 . ?
Ag3 Se2 K1 92.41(6) . 3_545 ?
Ga2 Se2 K1 90.34(7) 4_535 3_545 ?
Ga2 Se2 Ag3 99.61(5) 4_535 . ?
Ga3 Se2 K1 152.86(6) . 3_545 ?
Ga3 Se2 Ag3 101.35(4) . . ?
Ga3 Se2 Ga2 109.95(5) . 4_535 ?
Ag1 Se3 K1 144.14(9) . . ?
Ga2 Se3 K1 94.68(6) . . ?
Ga2 Se3 K1 94.68(6) 2_545 . ?
Ga2 Se3 Ag1 105.04(4) . . ?
Ga2 Se3 Ag1 105.04(4) 2_545 . ?
Ga2 Se3 Ga2 111.66(7) . 2_545 ?
Ga1 Se4 Ga4 110.35(5) 1_554 1_554 ?
Ga3 Se4 Ga1 104.59(4) . 1_554 ?
Ga3 Se4 Ga4 109.46(5) . 1_554 ?
Ag3 Se5 K1 147.52(9) 1_556 3_545 ?
Ga4 Se5 K1 97.62(6) 2_535 3_545 ?
Ga4 Se5 K1 97.62(6) . 3_545 ?
Ga4 Se5 Ag3 101.53(4) 2_535 1_556 ?
Ga4 Se5 Ag3 101.53(4) . 1_556 ?
Ga4 Se5 Ga4 106.93(7) 2_535 . ?
Ag2 Se6 K1 86.49(6) . 3_545 ?
Ga2 Se6 K1 154.66(7) . 3_545 ?
Ga2 Se6 Ag2 101.62(5) . . ?
Ga2 Se6 Ga4 109.82(5) . . ?
Ga4 Se6 K1 92.47(7) . 3_545 ?
Ga4 Se6 Ag2 97.99(5) . . ?
Ga1 Se7 Ga2 109.98(5) 4_434 . ?
Ga1 Se7 Ga3 106.84(4) 4_434 . ?
Ga3 Se7 Ga2 106.42(5) . . ?
Ag2 Se8 Ag1 96.66(5) 3 . ?
Ga3 Se8 Ag1 114.25(4) . . ?
Ga3 Se8 Ag1 114.25(4) 2_545 . ?
Ga3 Se8 Ag2 107.87(4) 2_545 3 ?
Ga3 Se8 Ag2 107.87(4) . 3 ?
Ga3 Se8 Ga3 114.08(6) . 2_545 ?
Ag2 Se9 Ag3 108.77(5) . . ?
Ga1 Se9 Ag2 111.23(4) 4_434 . ?
Ga1 Se9 Ag2 111.23(4) 3_444 . ?
Ga1 Se9 Ag3 108.09(5) 3_444 . ?
Ga1 Se9 Ag3 108.09(5) 4_434 . ?
Ga1 Se9 Ga1 109.31(7) 3_444 4_434 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 Se1 3.6235(10) 4_435 ?
K1 Se1 3.6235(10) 3_455 ?
K1 Se2 3.609(4) 4_435 ?
K1 Se2 3.609(4) 3_455 ?
K1 Se3 3.423(4) . ?
K1 Se5 3.410(4) 3_455 ?
K1 Se6 3.615(4) 4_435 ?
K1 Se6 3.615(4) 3_455 ?
Ag1 Se1 2.6616(10) . ?
Ag1 Se1 2.6615(10) 2_545 ?
Ag1 Se3 2.6607(15) . ?
Ag1 Se8 2.7084(16) . ?
Ag2 Se6 2.5930(11) . ?
Ag2 Se6 2.5930(11) 2_535 ?
Ag2 Se8 2.6043(17) 3_445 ?
Ag2 Se9 2.6889(17) . ?
Ag3 Se2 2.6211(12) 2_535 ?
Ag3 Se2 2.6211(12) . ?
Ag3 Se5 2.5751(14) 1_554 ?
Ag3 Se9 2.6904(16) . ?
Ga1 Se1 2.3812(12) . ?
Ga1 Se4 2.4572(12) 1_556 ?
Ga1 Se7 2.4447(13) 4_536 ?
Ga1 Se9 2.3772(11) 3_556 ?
Ga2 Se2 2.3841(14) 4_435 ?
Ga2 Se3 2.3988(12) . ?
Ga2 Se6 2.3868(13) . ?
Ga2 Se7 2.4746(13) . ?
Ga3 Se2 2.3624(13) . ?
Ga3 Se4 2.4304(13) . ?
Ga3 Se7 2.4541(11) . ?
Ga3 Se8 2.3834(12) . ?
Ga4 Se1 2.3884(13) 4_435 ?
Ga4 Se4 2.4995(12) 1_556 ?
Ga4 Se5 2.3981(12) . ?
Ga4 Se6 2.3948(12) . ?
Se1 K1 3.6235(10) 3_545 ?
Se1 Ga4 2.3885(13) 4_535 ?
Se2 K1 3.609(4) 3_545 ?
Se2 Ga2 2.3840(14) 4_535 ?
Se3 Ga2 2.3988(12) 2_545 ?
Se4 Ga1 2.4572(12) 1_554 ?
Se4 Ga4 2.4995(12) 1_554 ?
Se5 K1 3.410(4) 3_545 ?
Se5 Ag3 2.5751(14) 1_556 ?
Se5 Ga4 2.3981(12) 2_535 ?
Se6 K1 3.615(4) 3_545 ?
Se7 Ga1 2.4447(14) 4_434 ?
Se8 Ag2 2.6043(17) 3 ?
Se8 Ga3 2.3834(12) 2_545 ?
Se9 Ga1 2.3772(11) 4_434 ?
Se9 Ga1 2.3772(12) 3_444 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.964(13)
2 0.036(13)
