#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:19:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178945 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/74/4117408.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_4117408
loop_
_publ_author_name
'Hua-Jun Zhao'
'Yong-Fan Zhang'
'Ling Chen'
_publ_section_title
;
 Strong Kleinman-Forbidden Second Harmonic Generation in Chiral Sulfide:
 La4InSbS9
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1993
_journal_page_last               1995
_journal_paper_doi               10.1021/ja2109008
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'In Nd4 S9 Sb'
_chemical_formula_weight         1102.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.07210(10)
_cell_length_b                   10.07210(10)
_cell_length_c                   27.8292(10)
_cell_measurement_reflns_used    6505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4642
_cell_measurement_theta_min      2.0219
_cell_volume                     2823.19(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22430
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    19.857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8509
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    5.343
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.0500
_exptl_crystal_size_mid          0.0400
_exptl_crystal_size_min          0.0300
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.322
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.000215(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+53.8496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                3017
_reflns_number_total             3243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2109008_si_001_3.cif
_cod_data_source_block           Nd4InSbS9
_cod_database_code               4117408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nd1 Nd 0.55967(7) 0.77561(6) 0.08828(2) 0.01257(14) Uani 1 1 d .
Nd2 Nd 0.51027(7) 0.84942(6) -0.05276(2) 0.01339(13) Uani 1 1 d .
Nd3 Nd 0.23302(6) 0.99840(7) 0.05068(2) 0.01422(13) Uani 1 1 d .
Nd4 Nd 0.55620(7) 1.22772(6) 0.09243(2) 0.01280(14) Uani 1 1 d .
In1 In 0.79569(8) 0.98705(9) 0.20315(3) 0.01518(17) Uani 1 1 d .
Sb1 Sb -0.14136(8) 1.00922(10) 0.05544(3) 0.02143(19) Uani 1 1 d .
S1 S 0.0099(3) 0.8229(3) 0.03876(10) 0.0167(6) Uani 1 1 d .
S2 S 0.5200(3) 1.3120(3) 0.20030(10) 0.0134(6) Uani 1 1 d .
S3 S 0.4904(3) 0.5047(3) 0.10105(9) 0.0166(5) Uani 1 1 d .
S4 S 0.6021(2) 0.9964(3) 0.15099(10) 0.0123(5) Uani 1 1 d .
S5 S 0.8070(4) 1.1930(4) 0.2500 0.0416(17) Uani 1 2 d S
S6 S 0.7066(3) 1.3025(3) 0.00572(12) 0.0167(7) Uani 1 1 d .
S7 S 0.5033(3) 1.0010(3) 0.03145(9) 0.0126(5) Uani 1 1 d .
S8 S 0.7985(3) 1.3234(3) 0.12641(11) 0.0125(6) Uani 1 1 d .
S9 S 0.7981(3) 0.6899(3) 0.12796(11) 0.0120(6) Uani 1 1 d .
S10 S 0.6835(3) 0.6835(3) 0.0000 0.0153(9) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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
S9 Nd1 S9 135.50(3) . 6_465
S9 Nd1 S7 130.21(9) . .
S9 Nd1 S7 84.24(8) 6_465 .
S9 Nd1 S3 82.18(9) . .
S9 Nd1 S3 81.21(9) 6_465 .
S7 Nd1 S3 142.50(8) . .
S9 Nd1 S4 82.53(8) . .
S9 Nd1 S4 80.82(8) 6_465 .
S7 Nd1 S4 75.32(8) . .
S3 Nd1 S4 135.08(8) . .
S9 Nd1 S10 82.30(7) . .
S9 Nd1 S10 136.22(10) 6_465 .
S7 Nd1 S10 82.49(7) . .
S3 Nd1 S10 84.52(10) . .
S4 Nd1 S10 134.41(11) . .
S9 Nd1 Nd2 123.46(7) . .
S9 Nd1 Nd2 100.75(6) 6_465 .
S7 Nd1 Nd2 44.00(5) . .
S3 Nd1 Nd2 105.62(6) . .
S4 Nd1 Nd2 118.02(6) . .
S10 Nd1 Nd2 44.603(13) . .
S9 Nd1 Nd2 43.52(6) . 7
S9 Nd1 Nd2 146.14(7) 6_465 7
S7 Nd1 Nd2 122.32(6) . 7
S3 Nd1 Nd2 64.94(6) . 7
S4 Nd1 Nd2 123.41(6) . 7
S10 Nd1 Nd2 43.874(12) . 7
Nd2 Nd1 Nd2 88.458(19) . 7
S9 Nd1 Nd3 163.79(7) . .
S9 Nd1 Nd3 43.16(6) 6_465 .
S7 Nd1 Nd3 42.20(6) . .
S3 Nd1 Nd3 111.06(6) . .
S4 Nd1 Nd3 81.41(6) . .
S10 Nd1 Nd3 107.57(2) . .
Nd2 Nd1 Nd3 63.439(16) . .
Nd2 Nd1 Nd3 150.13(2) 7 .
S7 Nd2 S9 137.67(9) . 7
S7 Nd2 S10 84.43(7) . .
S9 Nd2 S10 83.16(7) 7 .
S7 Nd2 S8 133.56(9) . 7_455
S9 Nd2 S8 81.69(8) 7 7_455
S10 Nd2 S8 132.81(10) . 7_455
S7 Nd2 S4 83.71(8) . 3_654
S9 Nd2 S4 81.01(9) 7 3_654
S10 Nd2 S4 140.92(12) . 3_654
S8 Nd2 S4 79.58(9) 7_455 3_654
S7 Nd2 S6 82.68(9) . 7_455
S9 Nd2 S6 135.97(9) 7 7_455
S10 Nd2 S6 85.21(11) . 7_455
S8 Nd2 S6 75.73(9) 7_455 7_455
S4 Nd2 S6 129.69(10) 3_654 7_455
S7 Nd2 Nd1 44.54(6) . .
S9 Nd2 Nd1 127.72(6) 7 .
S10 Nd2 Nd1 46.230(15) . .
S8 Nd2 Nd1 139.03(7) 7_455 .
S4 Nd2 Nd1 127.41(6) 3_654 .
S6 Nd2 Nd1 63.30(7) 7_455 .
S7 Nd2 Nd1 127.58(6) . 7
S9 Nd2 Nd1 42.87(6) 7 7
S10 Nd2 Nd1 45.458(15) . 7
S8 Nd2 Nd1 97.50(6) 7_455 7
S4 Nd2 Nd1 122.99(6) 3_654 7
S6 Nd2 Nd1 103.34(7) 7_455 7
Nd1 Nd2 Nd1 91.331(18) . 7
S7 Nd3 S8 84.39(9) . 6_475
S7 Nd3 S9 85.09(8) . 6_465
S8 Nd3 S9 82.27(8) 6_475 6_465
S7 Nd3 S2 88.06(8) . 3_654
S8 Nd3 S2 134.81(9) 6_475 3_654
S9 Nd3 S2 141.34(9) 6_465 3_654
S7 Nd3 S2 136.45(9) . 6_475
S8 Nd3 S2 75.86(9) 6_475 6_475
S9 Nd3 S2 128.80(8) 6_465 6_475
S2 Nd3 S2 79.65(9) 3_654 6_475
S7 Nd3 S1 138.56(9) . .
S8 Nd3 S1 131.59(9) 6_475 .
S9 Nd3 S1 81.37(9) 6_465 .
S2 Nd3 S1 78.98(8) 3_654 .
S2 Nd3 S1 79.86(8) 6_475 .
S7 Nd3 Nd1 43.13(6) . .
S8 Nd3 Nd1 88.67(6) 6_475 .
S9 Nd3 Nd1 43.09(6) 6_465 .
S2 Nd3 Nd1 114.80(6) 3_654 .
S2 Nd3 Nd1 164.06(6) 6_475 .
S1 Nd3 Nd1 108.58(6) . .
S8 Nd4 S8 140.71(3) 6_475 .
S8 Nd4 S3 86.49(9) 6_475 1_565
S8 Nd4 S3 80.68(9) . 1_565
S8 Nd4 S4 79.86(8) 6_475 .
S8 Nd4 S4 86.97(8) . .
S3 Nd4 S4 140.71(8) 1_565 .
S8 Nd4 S7 82.25(9) 6_475 .
S8 Nd4 S7 129.23(9) . .
S3 Nd4 S7 140.48(8) 1_565 .
S4 Nd4 S7 73.93(8) . .
S8 Nd4 S6 141.39(9) 6_475 .
S8 Nd4 S6 74.90(9) . .
S3 Nd4 S6 86.49(9) 1_565 .
S4 Nd4 S6 125.98(9) . .
S7 Nd4 S6 79.41(8) . .
S8 Nd4 S2 69.15(8) 6_475 .
S8 Nd4 S2 71.59(8) . .
S3 Nd4 S2 68.38(7) 1_565 .
S4 Nd4 S2 72.33(8) . .
S7 Nd4 S2 138.78(8) . .
S6 Nd4 S2 140.64(8) . .
S4 In1 S6 114.32(11) . 4_465
S4 In1 S5 108.76(14) . .
S6 In1 S5 110.87(9) 4_465 .
S4 In1 S3 105.66(10) . 6_565
S6 In1 S3 111.71(11) 4_465 6_565
S5 In1 S3 104.99(9) . 6_565
S2 Sb1 S1 97.97(9) 6_475 .
S2 Sb1 S1 91.37(10) 6_475 7_465
S1 Sb1 S1 84.21(11) . 7_465
S2 Sb1 S3 77.91(9) 6_475 6_465
S1 Sb1 S3 81.40(9) . 6_465
S1 Sb1 S3 160.62(9) 7_465 6_465
Sb1 S1 Sb1 94.69(10) . 7_465
Sb1 S1 Nd3 89.62(9) . .
Sb1 S1 Nd3 91.87(9) 7_465 .
Sb1 S2 Nd3 97.57(10) 6_575 4_465
Sb1 S2 Nd3 90.36(9) 6_575 6_575
Nd3 S2 Nd3 99.95(9) 4_465 6_575
Sb1 S2 Nd4 102.42(10) 6_575 .
Nd3 S2 Nd4 155.01(10) 4_465 .
Nd3 S2 Nd4 94.81(8) 6_575 .
In1 S3 Nd1 94.93(9) 6_465 .
In1 S3 Nd4 99.45(10) 6_465 1_545
Nd1 S3 Nd4 149.87(12) . 1_545
In1 S3 Sb1 100.62(10) 6_465 6_565
Nd1 S3 Sb1 105.60(9) . 6_565
Nd4 S3 Sb1 97.61(9) 1_545 6_565
In1 S4 Nd2 116.41(10) . 4_465
In1 S4 Nd1 116.99(11) . .
Nd2 S4 Nd1 97.09(9) 4_465 .
In1 S4 Nd4 119.86(11) . .
Nd2 S4 Nd4 97.54(9) 4_465 .
Nd1 S4 Nd4 105.06(9) . .
In1 S5 In1 111.2(2) . 8_775
In1 S6 Nd2 134.29(14) 3_654 7_565
In1 S6 Nd4 94.17(11) 3_654 .
Nd2 S6 Nd4 94.07(10) 7_565 .
Nd3 S7 Nd2 100.43(9) . .
Nd3 S7 Nd1 94.67(9) . .
Nd2 S7 Nd1 91.46(9) . .
Nd3 S7 Nd4 94.29(8) . .
Nd2 S7 Nd4 156.50(11) . .
Nd1 S7 Nd4 105.59(8) . .
Nd4 S8 Nd3 96.48(9) 6_575 6_575
Nd4 S8 Nd4 149.00(12) 6_575 .
Nd3 S8 Nd4 105.21(10) 6_575 .
Nd4 S8 Nd2 100.35(10) 6_575 7_565
Nd3 S8 Nd2 98.16(9) 6_575 7_565
Nd4 S8 Nd2 98.22(9) . 7_565
Nd1 S9 Nd2 93.61(9) . 7
Nd1 S9 Nd1 154.32(12) . 6_565
Nd2 S9 Nd1 98.93(10) 7 6_565
Nd1 S9 Nd3 106.72(10) . 6_565
Nd2 S9 Nd3 97.71(10) 7 6_565
Nd1 S9 Nd3 93.75(9) 6_565 6_565
Nd2 S10 Nd2 177.88(19) . 7
Nd2 S10 Nd1 90.67(2) . 7
Nd2 S10 Nd1 89.17(2) 7 7
Nd2 S10 Nd1 89.17(2) . .
Nd2 S10 Nd1 90.67(2) 7 .
Nd1 S10 Nd1 171.08(19) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd1 S9 2.780(3) .
Nd1 S9 2.819(3) 6_465
Nd1 S7 2.824(3) .
Nd1 S3 2.839(3) .
Nd1 S4 2.859(3) .
Nd1 S10 2.9073(7) .
Nd2 S7 2.798(3) .
Nd2 S9 2.814(3) 7
Nd2 S10 2.827(3) .
Nd2 S8 2.829(3) 7_455
Nd2 S4 2.853(3) 3_654
Nd2 S6 2.857(3) 7_455
Nd3 S7 2.775(3) .
Nd3 S8 2.788(3) 6_475
Nd3 S9 2.823(3) 6_465
Nd3 S2 2.839(3) 3_654
Nd3 S2 2.872(3) 6_475
Nd3 S1 2.879(3) .
Nd4 S8 2.785(3) 6_475
Nd4 S8 2.789(3) .
Nd4 S3 2.877(3) 1_565
Nd4 S4 2.880(3) .
Nd4 S7 2.895(3) .
Nd4 S6 2.947(3) .
Nd4 S2 3.141(3) .
In1 S4 2.433(3) .
In1 S6 2.439(3) 4_465
In1 S5 2.453(3) .
In1 S3 2.476(3) 6_565
Sb1 S2 2.431(3) 6_475
Sb1 S1 2.461(3) .
Sb1 S1 2.646(3) 7_465
Sb1 S3 2.924(3) 6_465
S1 Sb1 2.646(3) 7_465
S2 Sb1 2.431(3) 6_575
S2 Nd3 2.839(3) 4_465
S2 Nd3 2.872(3) 6_575
S3 In1 2.476(3) 6_465
S3 Nd4 2.877(3) 1_545
S3 Sb1 2.925(3) 6_565
S4 Nd2 2.853(3) 4_465
S5 In1 2.453(3) 8_775
S6 In1 2.439(3) 3_654
S6 Nd2 2.857(3) 7_565
S8 Nd4 2.785(3) 6_575
S8 Nd3 2.788(3) 6_575
S8 Nd2 2.829(3) 7_565
S9 Nd2 2.814(3) 7
S9 Nd1 2.819(3) 6_565
S9 Nd3 2.823(3) 6_565
S10 Nd2 2.827(3) 7
S10 Nd1 2.9073(7) 7
