#------------------------------------------------------------------------------
#$Date: 2020-04-03 23:14:44 +0200 (vie 03 de abr de 2020) $
#$Revision: 250000 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/75/4517545.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_4517545
loop_
_publ_author_name
'Chi, Yang'
'Sun, Zong-Dong'
'Xu, Qian-Ting'
'Xue, Huai-Guo'
'Guo, Sheng-Ping'
_publ_section_title
;
 Hexagonal In₂Se₃: A Defect Wurtzite-Type Infrared
 Nonlinear Optical Material with Moderate Birefringence Contributed by
 Unique InSe₅ Unit.
;
_journal_name_full               'ACS applied materials & interfaces'
_journal_paper_doi               10.1021/acsami.9b23085
_journal_year                    2020
_chemical_formula_moiety         'In2 Se3'
_chemical_formula_sum            'In2 Se3'
_chemical_formula_weight         466.52
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-31
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.03.09 svn.r3491 for OlexSys, GUI svn.r5480)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   7.1231(3)
_cell_length_b                   7.1231(3)
_cell_length_c                   19.3925(16)
_cell_measurement_reflns_used    3001
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      3.30
_cell_volume                     852.12(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4124
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         1.050
_exptl_absorpt_coefficient_mu    27.172
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.455
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.833
_refine_diff_density_min         -2.669
_refine_diff_density_rms         0.545
_refine_ls_abs_structure_details
;
 Flack x determined using 581 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1290
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0188P)²+35.3993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1267
_reflns_number_total             1290
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am9b23085_si_002.cif
_cod_data_source_block           p65
_cod_original_cell_volume        852.12(10)
_cod_database_code               4517545
_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.
;
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.613
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.097(6)
 0.903(6)
;
_shelx_res_file
;
    p65.res created by SHELXL-2014/7

TITL a_a.res in P6(1)
CELL 0.71073 7.1231 7.1231 19.3925 90 90 120
ZERR 6 0.0003 0.0003 0.0016 0 0 0
LATT -1
SYMM -Y+X,+X,0.833+Z
SYMM -Y,+X-Y,0.667+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,0.333+Z
SYMM +Y,-X+Y,0.167+Z
SFAC In Se
UNIT 12 18

L.S. 10
PLAN  5
SIZE 0.02 0.02 0.015
list 4
fmap 2
acta NOHKL
TWIN 0 1 0 1 0 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\p65.hkl">
REM </olex2.extras>

WGHT    0.018800   35.399300
BASF   0.90269
FVAR       0.17952
IN1   1   -0.010961   -0.313099    0.000108    11.00000    0.01512    0.01072 =
         0.02778   -0.00120    0.00840    0.00601
IN2   1   -0.015149   -0.673036   -0.138407    11.00000    0.01471    0.01200 =
         0.01969   -0.00446   -0.00073    0.00721
SE1   2   -0.073633   -0.345556   -0.147123    11.00000    0.01367    0.01457 =
         0.01350    0.00118   -0.00226    0.00939
SE2   2   -0.042196   -0.695314   -0.003549    11.00000    0.01049    0.00935 =
         0.01228   -0.00225   -0.00011    0.00442
SE3   2    0.367139    0.025582   -0.014571    11.00000    0.01333    0.01191 =
         0.01999   -0.00315    0.00397    0.00364
HKLF 4

REM  a_a.res in P6(1)
REM R1 =  0.0424 for    1267 Fo > 4sig(Fo)  and  0.0434 for all    1290 data
REM     47 parameters refined using      1 restraints

END

WGHT      0.0188     35.3995

REM Highest difference peak  3.833,  deepest hole -2.669,  1-sigma level  0.545
Q1    1  -0.3591 -0.3747 -0.1480  11.00000  0.05    3.83
Q2    1   0.0208 -0.3430 -0.1759  11.00000  0.05    2.95
Q3    1   0.5949 -0.0435 -0.0331  11.00000  0.05    2.10
Q4    1  -0.2465 -0.2725 -0.1690  11.00000  0.05    1.99
Q5    1  -0.0033 -0.6629 -0.1790  11.00000  0.05    1.92
;
_shelx_res_checksum              31581
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+5/6'
'-y, x-y, z+2/3'
'-x, -y, z+1/2'
'-x+y, -x, z+1/3'
'y, -x+y, z+1/6'
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
In1 In -0.0110(3) -0.3131(3) 0.00011(10) 0.0181(5) Uani 1 1 d . . . . .
In2 In -0.0151(3) -0.6730(3) -0.13841(9) 0.0152(4) Uani 1 1 d . . . . .
Se1 Se -0.0736(4) -0.3456(4) -0.14712(15) 0.0129(5) Uani 1 1 d . . . . .
Se2 Se -0.0422(4) -0.6953(4) -0.00355(13) 0.0109(5) Uani 1 1 d . . . . .
Se3 Se 0.3671(4) 0.0256(4) -0.01457(14) 0.0163(6) Uani 1 1 d . . . . .
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
In1 0.0151(9) 0.0107(8) 0.0278(11) -0.0012(8) 0.0084(8) 0.0060(8)
In2 0.0147(9) 0.0120(8) 0.0197(10) -0.0045(7) -0.0007(7) 0.0072(7)
Se1 0.0137(12) 0.0146(12) 0.0135(11) 0.0012(10) -0.0023(10) 0.0094(10)
Se2 0.0105(12) 0.0094(10) 0.0123(12) -0.0022(10) -0.0001(10) 0.0044(9)
Se3 0.0133(12) 0.0119(12) 0.0200(12) -0.0032(11) 0.0040(11) 0.0036(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
In In -0.7276 1.3100 '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 In1 Se1 92.24(9) 6 . ?
Se1 In1 Se2 121.39(11) 6 . ?
Se1 In1 Se3 88.87(10) 6 6 ?
Se1 In1 Se3 120.23(10) 6 . ?
Se1 In1 Se3 172.62(10) . 6 ?
Se2 In1 Se1 87.74(10) . . ?
Se2 In1 Se3 85.46(10) . 6 ?
Se3 In1 Se1 90.75(10) . . ?
Se3 In1 Se2 118.38(11) . . ?
Se3 In1 Se3 94.99(10) . 6 ?
Se1 In2 Se2 94.60(11) . . ?
Se1 In2 Se2 115.29(12) . 2_444 ?
Se2 In2 Se2 100.06(10) 2_444 . ?
Se3 In2 Se1 118.75(12) 2_544 . ?
Se3 In2 Se2 111.76(10) 2_544 . ?
Se3 In2 Se2 112.94(10) 2_544 2_444 ?
In1 Se1 In1 91.33(10) 2_554 . ?
In1 Se1 In2 106.55(11) 2_554 . ?
In2 Se1 In1 85.34(10) . . ?
In1 Se2 In2 89.92(10) . . ?
In2 Se2 In1 109.48(11) 6_655 . ?
In2 Se2 In2 101.06(10) 6_655 . ?
In1 Se3 In1 89.05(10) . 2_554 ?
In2 Se3 In1 108.59(11) 6_665 2_554 ?
In2 Se3 In1 105.35(11) 6_665 . ?
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
In1 Se1 2.571(3) 6 ?
In1 Se1 2.881(3) . ?
In1 Se2 2.619(3) . ?
In1 Se3 2.580(3) . ?
In1 Se3 2.975(3) 6 ?
In2 Se1 2.572(3) . ?
In2 Se2 2.582(3) 2_444 ?
In2 Se2 2.621(3) . ?
In2 Se3 2.550(3) 2_544 ?
Se1 In1 2.570(3) 2_554 ?
Se2 In2 2.582(3) 6_655 ?
Se3 In1 2.975(3) 2_554 ?
Se3 In2 2.550(3) 6_665 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.097(6)
2 0.903(6)
