#------------------------------------------------------------------------------
#$Date: 2021-09-04 00:59:46 +0300 (Sat, 04 Sep 2021) $
#$Revision: 268449 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/40/4004025.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_4004025
loop_
_publ_author_name
'Chu, Yu'
'Wang, Peng'
'Zeng, Hao'
'Cheng, Shichao'
'Su, Xin'
'Yang, Zhihua'
'Li, Junjie'
'Pan, Shilie'
_publ_section_title
;
 Hg3P2S8: A New Promising Infrared Nonlinear Optical Material with a Large
 Second-Harmonic Generation and a High Laser-Induced Damage Threshold
;
_journal_issue                   16
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6514
_journal_page_last               6521
_journal_paper_doi               10.1021/acs.chemmater.1c01982
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety         'Hg3 P2 S8'
_chemical_formula_sum            'Hg3 P2 S8'
_chemical_formula_weight         920.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.52(2)
_cell_length_b                   8.223(10)
_cell_length_c                   9.293(11)
_cell_measurement_reflns_used    1382
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.53
_cell_volume                     1262(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3653
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.416
_diffrn_reflns_theta_min         2.466
_exptl_absorpt_coefficient_mu    37.927
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1398 before and 0.0645 after correction. The Ratio of minimum to maximum transmission is 0.3678. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    4.842
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.350
_refine_ls_abs_structure_details
;
 Flack x determined using 451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(17)
_refine_ls_extinction_coef       0.0059(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0309
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                1181
_reflns_number_total             1371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm1c01982_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               4004025
_shelx_shelxl_version_number     2018/3
_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
;
;
_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'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.500000 0.500000 0.29945(14) 0.0268(3) Uani 1 2 d S T P . .
Hg2 Hg 0.25536(4) 0.50015(5) 0.70081(8) 0.0241(2) Uani 1 1 d . . . . .
P1 P 0.3713(2) 0.7641(3) 0.4697(4) 0.0111(7) Uani 1 1 d . . . . .
S1 S 0.4663(2) 0.7815(4) 0.3278(4) 0.0171(7) Uani 1 1 d . . . . .
S2 S 0.38917(19) 0.5624(4) 0.5928(4) 0.0189(7) Uani 1 1 d . . . . .
S3 S 0.25682(19) 0.7570(3) 0.3769(4) 0.0128(8) Uani 1 1 d . . . . .
S4 S 0.3780(2) 0.9851(3) 0.5747(4) 0.0155(7) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
S1 Hg1 S1 167.35(19) 2_665 . ?
S1 Hg1 S4 87.63(11) 2_665 6_664 ?
S1 Hg1 S4 101.53(11) 2_665 5_544 ?
S1 Hg1 S4 87.63(11) . 5_544 ?
S1 Hg1 S4 101.53(11) . 6_664 ?
S4 Hg1 S4 88.05(19) 5_544 6_664 ?
S2 Hg2 S3 98.70(12) . 8_545 ?
S2 Hg2 S3 114.06(11) . 5_545 ?
S2 Hg2 S4 127.28(15) . 4_545 ?
S3 Hg2 S3 102.95(17) 5_545 8_545 ?
S4 Hg2 S3 105.49(12) 4_545 5_545 ?
S4 Hg2 S3 105.03(11) 4_545 8_545 ?
S1 P1 S3 115.5(2) . . ?
S1 P1 S4 101.6(2) . . ?
S2 P1 S1 107.84(19) . . ?
S2 P1 S3 110.04(19) . . ?
S2 P1 S4 116.4(2) . . ?
S4 P1 S3 105.62(19) . . ?
P1 S1 Hg1 100.42(15) . . ?
P1 S2 Hg2 105.42(16) . . ?
Hg2 S3 Hg2 102.87(17) 5_554 8_544 ?
P1 S3 Hg2 110.11(15) . 8_544 ?
P1 S3 Hg2 104.47(16) . 5_554 ?
Hg2 S4 Hg1 105.79(17) 4 5 ?
P1 S4 Hg1 114.44(18) . 5 ?
P1 S4 Hg2 102.57(17) . 4 ?
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
Hg1 S1 2.396(4) 2_665 ?
Hg1 S1 2.396(4) . ?
Hg1 S4 2.905(5) 6_664 ?
Hg1 S4 2.905(5) 5_544 ?
Hg2 S2 2.481(4) . ?
Hg2 S3 2.679(4) 8_545 ?
Hg2 S3 2.584(4) 5_545 ?
Hg2 S4 2.498(5) 4_545 ?
P1 S1 2.055(5) . ?
P1 S2 2.036(5) . ?
P1 S3 2.079(5) . ?
P1 S4 2.066(4) . ?
