#------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000673.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_4000673
loop_
_publ_author_name
'Yvonne Klawitter'
'Wolfgang Bensch'
'Claudia Wickleder'
_publ_section_title
;
 Synthesis, Crystal Structure, and Vibrational and Optical Spectroscopy
 of the First Quaternary Alkaline-Earth Rare Earth Thiophosphates
 Ba3Ln2[P4S16] (Ln = Gd-Er)
;
_journal_name_full               'Chem. Mater.'
_journal_page_first              187
_journal_page_last               197
_journal_paper_doi               10.1021/cm051860n
_journal_volume                  18
_journal_year                    2006
_chemical_formula_sum            'Ba3 Ho2 P4 S16'
_chemical_formula_weight         1378.72
_chemical_name_systematic        '  ?'
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   19.088(3)
_cell_length_b                   10.2481(13)
_cell_length_c                   12.565(2)
_cell_measurement_reflns_used    122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37
_cell_measurement_theta_min      22
_cell_volume                     2457.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Philips PW 1100'
_diffrn_measurement_method       'omega theta 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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7992
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'every 120 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.710
_exptl_absorpt_correction_T_max  0.3695
_exptl_absorpt_correction_T_min  0.2631
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       0.00061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0333P)²+5.5169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                2815
_reflns_number_total             3591
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4000673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ho1 Ho 0.573300(11) 0.12804(2) 0.113142(17) 0.00957(7) Uani 1 1 d .
Ba1 Ba 0.727533(15) -0.28946(3) -0.11140(3) 0.01495(8) Uani 1 1 d .
Ba2 Ba 0.5000 -0.38058(4) 0.2500 0.01702(10) Uani 1 2 d S
S1 S 0.65017(8) -0.38270(14) 0.10579(11) 0.0195(3) Uani 1 1 d .
S2 S 0.64694(7) -0.56968(14) -0.11305(10) 0.0149(2) Uani 1 1 d .
S3 S 0.48430(7) -0.11314(13) 0.09881(10) 0.0136(2) Uani 1 1 d .
S4 S 0.69213(7) 0.29220(13) 0.11471(11) 0.0138(2) Uani 1 1 d .
S5 S 0.43086(6) 0.18059(13) 0.16906(11) 0.0142(2) Uani 1 1 d .
S6 S 0.53152(7) 0.38064(13) 0.08548(12) 0.0154(3) Uani 1 1 d .
S7 S 0.66769(6) -0.00598(14) -0.01367(10) 0.0154(2) Uani 1 1 d .
S8 S 0.65220(7) -0.06718(15) 0.23021(10) 0.0188(3) Uani 1 1 d .
P1 P 0.39767(7) -0.00507(13) 0.13963(10) 0.0107(2) Uani 1 1 d .
P2 P 0.63097(7) -0.56208(13) 0.04847(11) 0.0111(2) 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
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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
S6 Ho1 S7 125.93(4) . .
S6 Ho1 S5 86.19(4) . 3_655
S7 Ho1 S5 132.72(4) . 3_655
S6 Ho1 S4 70.78(4) . .
S7 Ho1 S4 77.11(4) . .
S5 Ho1 S4 84.32(4) 3_655 .
S6 Ho1 S5 64.85(4) . .
S7 Ho1 S5 148.57(4) . .
S5 Ho1 S5 72.28(4) 3_655 .
S4 Ho1 S5 130.53(4) . .
S6 Ho1 S3 79.71(4) . 5_655
S7 Ho1 S3 71.98(4) . 5_655
S5 Ho1 S3 154.78(4) 3_655 5_655
S4 Ho1 S3 110.12(4) . 5_655
S5 Ho1 S3 82.78(4) . 5_655
S6 Ho1 S8 150.33(4) . .
S7 Ho1 S8 67.20(4) . .
S5 Ho1 S8 69.57(4) 3_655 .
S4 Ho1 S8 89.44(4) . .
S5 Ho1 S8 119.89(4) . .
S3 Ho1 S8 128.95(4) 5_655 .
S6 Ho1 S3 127.37(4) . .
S7 Ho1 S3 85.72(4) . .
S5 Ho1 S3 101.62(4) 3_655 .
S4 Ho1 S3 160.84(4) . .
S5 Ho1 S3 68.41(4) . .
S3 Ho1 S3 71.68(4) 5_655 .
S8 Ho1 S3 75.93(4) . .
S7 Ba1 S1 76.11(4) 8_755 .
S7 Ba1 S2 71.90(3) 8_755 .
S1 Ba1 S2 62.04(3) . .
S7 Ba1 S2 91.25(3) 8_755 8_765
S1 Ba1 S2 122.57(3) . 8_765
S2 Ba1 S2 161.39(3) . 8_765
S7 Ba1 S5 151.91(3) 8_755 5_655
S1 Ba1 S5 82.38(4) . 5_655
S2 Ba1 S5 82.19(3) . 5_655
S2 Ba1 S5 115.73(4) 8_765 5_655
S7 Ba1 S4 64.14(3) 8_755 8_755
S1 Ba1 S4 64.34(4) . 8_755
S2 Ba1 S4 116.34(3) . 8_755
S2 Ba1 S4 59.90(3) 8_765 8_755
S5 Ba1 S4 121.53(3) 5_655 8_755
S7 Ba1 S7 131.81(4) 8_755 .
S1 Ba1 S7 78.01(4) . .
S2 Ba1 S7 127.22(3) . .
S2 Ba1 S7 69.96(3) 8_765 .
S5 Ba1 S7 58.40(3) 5_655 .
S4 Ba1 S7 68.13(3) 8_755 .
S7 Ba1 S8 60.26(3) 8_755 2_644
S1 Ba1 S8 132.60(4) . 2_644
S2 Ba1 S8 86.20(4) . 2_644
S2 Ba1 S8 78.39(4) 8_765 2_644
S5 Ba1 S8 129.82(3) 5_655 2_644
S4 Ba1 S8 107.39(3) 8_755 2_644
S7 Ba1 S8 145.54(4) . 2_644
S7 Ba1 S4 119.13(3) 8_755 7
S1 Ba1 S4 137.29(4) . 7
S2 Ba1 S4 84.01(3) . 7
S2 Ba1 S4 98.03(3) 8_765 7
S5 Ba1 S4 67.12(3) 5_655 7
S4 Ba1 S4 157.889(18) 8_755 7
S7 Ba1 S4 107.49(3) . 7
S8 Ba1 S4 63.19(3) 2_644 7
S6 Ba2 S6 82.68(5) 1_545 3_645
S6 Ba2 S2 93.29(3) 1_545 7_546
S6 Ba2 S2 73.31(3) 3_645 7_546
S6 Ba2 S2 73.31(3) 1_545 5_645
S6 Ba2 S2 93.29(3) 3_645 5_645
S2 Ba2 S2 162.39(5) 7_546 5_645
S6 Ba2 S3 163.32(3) 1_545 3_655
S6 Ba2 S3 105.74(4) 3_645 3_655
S2 Ba2 S3 75.92(3) 7_546 3_655
S2 Ba2 S3 119.60(3) 5_645 3_655
S6 Ba2 S3 105.74(4) 1_545 .
S6 Ba2 S3 163.32(3) 3_645 .
S2 Ba2 S3 119.60(3) 7_546 .
S2 Ba2 S3 75.92(3) 5_645 .
S3 Ba2 S3 70.11(5) 3_655 .
S6 Ba2 S1 60.02(3) 1_545 .
S6 Ba2 S1 119.35(4) 3_645 .
S2 Ba2 S1 64.10(4) 7_546 .
S2 Ba2 S1 115.78(4) 5_645 .
S3 Ba2 S1 103.46(3) 3_655 .
S3 Ba2 S1 77.16(3) . .
S6 Ba2 S1 119.35(4) 1_545 3_655
S6 Ba2 S1 60.02(3) 3_645 3_655
S2 Ba2 S1 115.78(4) 7_546 3_655
S2 Ba2 S1 64.10(4) 5_645 3_655
S3 Ba2 S1 77.16(3) 3_655 3_655
S3 Ba2 S1 103.46(3) . 3_655
S1 Ba2 S1 179.26(5) . 3_655
P2 S1 Ba1 92.92(6) . .
P2 S1 Ba2 92.48(6) . .
Ba1 S1 Ba2 146.27(5) . .
P2 S2 Ba1 91.74(6) . .
P2 S2 Ba1 97.35(6) . 8_755
Ba1 S2 Ba1 105.05(4) . 8_755
P2 S2 Ba2 113.04(6) . 5_645
Ba1 S2 Ba2 122.41(4) . 5_645
Ba1 S2 Ba2 120.81(4) 8_755 5_645
P1 S3 Ho1 87.26(6) . 5_655
P1 S3 Ho1 89.81(6) . .
Ho1 S3 Ho1 108.32(4) 5_655 .
P1 S3 Ba2 111.81(6) . .
Ho1 S3 Ba2 120.96(4) 5_655 .
Ho1 S3 Ba2 126.07(4) . .
P2 S4 Ho1 88.50(6) 1_565 .
P2 S4 Ba1 95.61(6) 1_565 8_765
Ho1 S4 Ba1 102.35(4) . 8_765
P2 S4 Ba1 120.59(6) 1_565 7_556
Ho1 S4 Ba1 99.02(4) . 7_556
Ba1 S4 Ba1 138.18(4) 8_765 7_556
P1 S5 Ho1 89.37(6) . 3_655
P1 S5 Ho1 94.31(6) . .
Ho1 S5 Ho1 103.40(4) 3_655 .
P1 S5 Ba1 89.49(6) . 5_655
Ho1 S5 Ba1 104.73(4) 3_655 5_655
Ho1 S5 Ba1 151.65(5) . 5_655
P2 S6 Ho1 91.72(6) 1_565 .
P2 S6 Ba2 95.76(6) 1_565 1_565
Ho1 S6 Ba2 133.22(5) . 1_565
P1 S7 Ho1 91.21(6) 5_655 .
P1 S7 Ba1 92.64(6) 5_655 8_765
Ho1 S7 Ba1 106.31(4) . 8_765
P1 S7 Ba1 88.40(6) 5_655 .
Ho1 S7 Ba1 149.49(5) . .
Ba1 S7 Ba1 104.18(4) 8_765 .
P1 S8 Ho1 87.02(6) 3_655 .
P1 S8 Ba1 88.86(6) 3_655 2_645
Ho1 S8 Ba1 162.05(6) . 2_645
S8 P1 S7 111.43(8) 3_655 5_655
S8 P1 S5 107.28(8) 3_655 .
S7 P1 S5 106.37(8) 5_655 .
S8 P1 S3 114.60(9) 3_655 .
S7 P1 S3 109.38(8) 5_655 .
S5 P1 S3 107.34(8) . .
S1 P2 S6 110.57(8) . 1_545
S1 P2 S2 111.23(8) . .
S6 P2 S2 110.64(8) 1_545 .
S1 P2 S4 114.40(9) . 1_545
S6 P2 S4 103.03(8) 1_545 1_545
S2 P2 S4 106.63(8) . 1_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 S6 2.7310(14) .
Ho1 S7 2.7697(13) .
Ho1 S5 2.7902(14) 3_655
Ho1 S4 2.8242(13) .
Ho1 S5 2.8595(13) .
Ho1 S3 2.8852(13) 5_655
Ho1 S8 2.9042(14) .
Ho1 S3 3.0046(14) .
Ba1 S7 3.2298(14) 8_755
Ba1 S1 3.2467(15) .
Ba1 S2 3.2579(14) .
Ba1 S2 3.2886(14) 8_765
Ba1 S5 3.3031(14) 5_655
Ba1 S4 3.3351(14) 8_755
Ba1 S7 3.3544(14) .
Ba1 S8 3.3749(14) 2_644
Ba1 S4 3.5072(15) 7
Ba2 S6 3.2593(15) 1_545
Ba2 S6 3.2593(15) 3_645
Ba2 S2 3.3298(13) 7_546
Ba2 S2 3.3298(13) 5_645
Ba2 S3 3.3482(14) 3_655
Ba2 S3 3.3482(14) .
Ba2 S1 3.3912(15) .
Ba2 S1 3.3912(15) 3_655
S1 P2 2.0081(19) .
S2 P2 2.0537(19) .
S2 Ba1 3.2886(14) 8_755
S2 Ba2 3.3298(13) 5_645
S3 P1 2.0552(18) .
S3 Ho1 2.8852(13) 5_655
S4 P2 2.0703(19) 1_565
S4 Ba1 3.3351(14) 8_765
S4 Ba1 3.5072(15) 7_556
S5 P1 2.0391(18) .
S5 Ho1 2.7902(14) 3_655
S5 Ba1 3.3031(14) 5_655
S6 P2 2.0407(18) 1_565
S6 Ba2 3.2593(15) 1_565
S7 P1 2.0185(18) 5_655
S7 Ba1 3.2298(14) 8_765
S8 P1 1.9965(18) 3_655
S8 Ba1 3.3749(14) 2_645
P1 S8 1.9965(18) 3_655
P1 S7 2.0185(18) 5_655
P2 S6 2.0407(18) 1_545
P2 S4 2.0703(19) 1_545
