#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:58:28 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/67/7706794.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_7706794
loop_
_publ_author_name
'Yang, Ya'
'Zhang, Bingbing'
'Wu, Xiaowen'
'Wu, Kui'
_publ_section_title
;
 A series of M₃PS₄ (M = Ag, Cu and Ag/Cu)
 thiophosphates with diamond-like structures exhibiting large second
 harmonic generation responses and moderate ion conductivities.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4129
_journal_page_last               4132
_journal_paper_doi               10.1039/d1dt00366f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'Cu3 P S4'
_chemical_formula_weight         349.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   none
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-01-23 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2789(16)
_cell_length_b                   6.3341(14)
_cell_length_c                   6.0828(14)
_cell_measurement_reflns_used    1333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      4.27
_cell_volume                     280.45(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.966
_diffrn_reflns_theta_max         24.966
_diffrn_reflns_theta_min         3.216
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    12.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.143
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.112
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.5103
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.036(19)
_refine_ls_extinction_coef       0.0335(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         527
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0144
_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          0.0347
_refine_ls_wR_factor_ref         0.0349
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                520
_reflns_number_total             527
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00366f2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7706792--7706794.cif.'
_cod_database_code               7706794
_shelx_shelxl_version_number     2016/6
_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_min   0.5103
_shelx_estimated_absorpt_t_max   0.7455
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, 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
Cu1 Cu 0.500000 0.35265(11) 0.58397(16) 0.0181(3) Uani 1 2 d S T P . .
Cu2 Cu 0.24561(5) -0.17858(7) 0.57297(12) 0.0163(2) Uani 1 1 d . . . . .
S1 S 0.23320(13) 0.16833(16) 0.6968(3) 0.0087(3) Uani 1 1 d . . . . .
S2 S 0.000000 0.3177(3) 0.2447(3) 0.0086(4) Uani 1 2 d S T P . .
S3 S 0.000000 0.6281(3) 0.7040(3) 0.0087(4) Uani 1 2 d S T P . .
P1 P 0.000000 0.3231(2) 0.5853(4) 0.0057(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
Cu Cu 0.3201 1.2651 '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
S2 Cu1 S3 112.07(7) 2_565 2_564 ?
S2 Cu1 S1 108.88(5) 2_565 3_655 ?
S3 Cu1 S1 108.39(5) 2_564 3_655 ?
S2 Cu1 S1 108.88(5) 2_565 . ?
S3 Cu1 S1 108.39(5) 2_564 . ?
S1 Cu1 S1 110.22(7) 3_655 . ?
S1 Cu2 S2 114.17(6) 2_554 2 ?
S1 Cu2 S3 114.29(6) 2_554 1_545 ?
S2 Cu2 S3 105.26(5) 2 1_545 ?
S1 Cu2 S1 107.40(5) 2_554 . ?
S2 Cu2 S1 104.24(6) 2 . ?
S3 Cu2 S1 111.06(6) 1_545 . ?
P1 S1 Cu2 111.57(10) . 2 ?
P1 S1 Cu2 111.88(9) . . ?
Cu2 S1 Cu2 110.32(6) 2 . ?
P1 S1 Cu1 110.10(8) . . ?
Cu2 S1 Cu1 102.71(6) 2 . ?
Cu2 S1 Cu1 109.90(5) . . ?
P1 S2 Cu2 117.40(6) . 4_454 ?
P1 S2 Cu2 117.40(6) . 2_554 ?
Cu2 S2 Cu2 107.14(7) 4_454 2_554 ?
P1 S2 Cu1 114.15(9) . 2_564 ?
Cu2 S2 Cu1 98.87(6) 4_454 2_564 ?
Cu2 S2 Cu1 98.87(6) 2_554 2_564 ?
P1 S3 Cu2 112.08(8) . 1_565 ?
P1 S3 Cu2 112.08(8) . 3_565 ?
Cu2 S3 Cu2 101.48(7) 1_565 3_565 ?
P1 S3 Cu1 113.51(11) . 2_565 ?
Cu2 S3 Cu1 108.47(6) 1_565 2_565 ?
Cu2 S3 Cu1 108.47(6) 3_565 2_565 ?
S3 P1 S2 111.43(13) . . ?
S3 P1 S1 109.16(10) . 3 ?
S2 P1 S1 108.61(10) . 3 ?
S3 P1 S1 109.16(10) . . ?
S2 P1 S1 108.61(10) . . ?
S1 P1 S1 109.86(11) 3 . ?
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
Cu1 S2 2.3059(19) 2_565 ?
Cu1 S3 2.314(2) 2_564 ?
Cu1 S1 2.3675(12) 3_655 ?
Cu1 S1 2.3675(12) . ?
Cu2 S1 2.294(2) 2_554 ?
Cu2 S2 2.3014(11) 2 ?
Cu2 S3 2.3089(11) 1_545 ?
Cu2 S1 2.3246(14) . ?
S1 P1 2.0740(18) . ?
S2 P1 2.072(4) . ?
S3 P1 2.063(3) . ?
