#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:30:46 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224274 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049221.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_7049221
loop_
_publ_author_name
'Netzsch, Philip'
'Hämmer, Matthias'
'Gross, Peter'
'Bariss, Harijs'
'Block, Theresa'
'Heletta, Lukas'
'Pöttgen, Rainer'
'Bruns, Jörn'
'Huppertz, Hubert'
'Höppe, Henning A'
_publ_section_title
;
 RE₂[B₂(SO₄)₆] (RE = Y, La-Nd,
 Sm, Eu, Tb-Lu): a silicate-analogous host structure with weak
 coordination behaviour.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4387
_journal_page_last               4397
_journal_paper_doi               10.1039/c9dt00445a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'B2 O24 Pr2 S6'
_chemical_formula_weight         879.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.638(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7141(11)
_cell_length_b                   11.5305(9)
_cell_length_c                   11.2643(9)
_cell_measurement_reflns_used    2565
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      30.555
_cell_measurement_theta_min      2.310
_cell_volume                     1777.6(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega scan'
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.310
_exptl_absorpt_coefficient_mu    6.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 multi-scan absorption correction using SADABS 
(G. M. Sheldrick, (1996). SADABS. Program for Empirical 
Absorption Correction. University of Göttingen, Germany.)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.287
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6174
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00090(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0162P)²+3.7272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2565
_reflns_number_total             2719
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00445a10.cif
_cod_data_source_block           mo_pn38_2_0m
_cod_depositor_comments
'Adding full bibliography for 7049219--7049233.cif.'
_cod_database_code               7049221
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pr01 Pr 0.31256(2) 0.45204(2) 0.34302(2) 0.00552(4) Uani 1 1 d
S1 S 0.63584(3) 0.70243(4) 0.36238(4) 0.00535(8) Uani 1 1 d
S2 S 0.62690(3) 0.98672(4) 0.57578(4) 0.00614(8) Uani 1 1 d
S3 S 0.42194(3) 0.65239(4) 0.57949(4) 0.00650(8) Uani 1 1 d
O11 O 0.61843(10) 0.61129(12) 0.27541(13) 0.0132(3) Uani 1 1 d
O12 O 0.69251(10) 0.79722(12) 0.31739(13) 0.0139(3) Uani 1 1 d
O13 O 0.67807(10) 0.65908(12) 0.47522(12) 0.0111(3) Uani 1 1 d
O14 O 0.53353(9) 0.75083(11) 0.38327(12) 0.0093(2) Uani 1 1 d
O21 O 0.68530(10) 0.98015(12) 0.68547(13) 0.0130(3) Uani 1 1 d
O22 O 0.67560(10) 1.01881(12) 0.47151(13) 0.0139(3) Uani 1 1 d
O23 O 0.58034(10) 0.86820(11) 0.55876(12) 0.0107(3) Uani 1 1 d
O24 O 0.45805(9) 0.93196(11) 0.40466(12) 0.0080(2) Uani 1 1 d
O31 O 0.51888(10) 0.61873(14) 0.62233(14) 0.0179(3) Uani 1 1 d
O32 O 0.38654(13) 0.58525(14) 0.47799(14) 0.0225(3) Uani 1 1 d
O33 O 0.35265(10) 0.65378(13) 0.67128(13) 0.0149(3) Uani 1 1 d
O34 O 0.42461(10) 0.77906(11) 0.53887(13) 0.0122(3) Uani 1 1 d
B1 B 0.49995(14) 0.83078(17) 0.47162(18) 0.0067(3) 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
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Pr Pr -0.2180 2.8214 '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
O32 Pr01 O33 138.54(5) . 6_565
O32 Pr01 O13 78.47(5) . 5_666
O33 Pr01 O13 114.51(5) 6_565 5_666
O32 Pr01 O12 144.96(5) . 3_445
O33 Pr01 O12 73.56(5) 6_565 3_445
O13 Pr01 O12 73.15(5) 5_666 3_445
O32 Pr01 O31 75.58(6) . 5_666
O33 Pr01 O31 72.28(5) 6_565 5_666
O13 Pr01 O31 71.95(5) 5_666 5_666
O12 Pr01 O31 113.43(5) 3_445 5_666
O32 Pr01 O11 72.61(5) . 2_655
O33 Pr01 O11 80.07(5) 6_565 2_655
O13 Pr01 O11 147.62(5) 5_666 2_655
O12 Pr01 O11 138.97(5) 3_445 2_655
O31 Pr01 O11 86.81(5) 5_666 2_655
O32 Pr01 O21 120.16(5) . 8_465
O33 Pr01 O21 76.89(5) 6_565 8_465
O13 Pr01 O21 139.12(5) 5_666 8_465
O12 Pr01 O21 73.28(5) 3_445 8_465
O31 Pr01 O21 144.36(5) 5_666 8_465
O11 Pr01 O21 70.46(5) 2_655 8_465
O32 Pr01 O22 74.90(5) . 3_445
O33 Pr01 O22 145.95(5) 6_565 3_445
O13 Pr01 O22 71.43(5) 5_666 3_445
O12 Pr01 O22 76.86(5) 3_445 3_445
O31 Pr01 O22 136.53(5) 5_666 3_445
O11 Pr01 O22 113.46(5) 2_655 3_445
O21 Pr01 O22 78.80(5) 8_465 3_445
O11 S1 O12 112.32(9) . .
O11 S1 O13 112.49(8) . .
O12 S1 O13 111.86(8) . .
O11 S1 O14 104.69(8) . .
O12 S1 O14 107.06(8) . .
O13 S1 O14 107.90(8) . .
O21 S2 O22 117.13(9) . .
O21 S2 O23 105.65(8) . .
O22 S2 O23 110.06(8) . .
O21 S2 O24 107.41(8) . 5_676
O22 S2 O24 111.07(8) . 5_676
O23 S2 O24 104.68(8) . 5_676
O31 S3 O32 112.29(10) . .
O31 S3 O33 113.44(9) . .
O32 S3 O33 111.69(10) . .
O31 S3 O34 108.56(9) . .
O32 S3 O34 106.78(9) . .
O33 S3 O34 103.41(8) . .
S1 O11 Pr01 147.81(8) . 2_655
S1 O12 Pr01 152.20(9) . 3
S1 O13 Pr01 157.37(9) . 5_666
B1 O14 S1 131.70(12) . .
S2 O21 Pr01 155.74(9) . 8_566
S2 O22 Pr01 141.31(8) . 3
B1 O23 S2 129.17(12) . .
B1 O24 S2 133.27(12) . 5_676
S3 O31 Pr01 169.16(10) . 5_666
S3 O32 Pr01 167.70(11) . .
S3 O33 Pr01 140.38(9) . 6_566
B1 O34 S3 125.49(12) . .
O34 B1 O14 111.39(15) . .
O34 B1 O24 108.87(14) . .
O14 B1 O24 106.25(14) . .
O34 B1 O23 107.27(15) . .
O14 B1 O23 112.39(15) . .
O24 B1 O23 110.66(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr01 O32 2.3461(15) .
Pr01 O33 2.3808(14) 6_565
Pr01 O13 2.4118(13) 5_666
Pr01 O12 2.4332(14) 3_445
Pr01 O31 2.4592(14) 5_666
Pr01 O11 2.4915(13) 2_655
Pr01 O21 2.5326(14) 8_465
Pr01 O22 2.5614(13) 3_445
S1 O11 1.4462(14) .
S1 O12 1.4510(14) .
S1 O13 1.4516(14) .
S1 O14 1.5419(13) .
S2 O21 1.4311(15) .
S2 O22 1.4360(14) .
S2 O23 1.5154(13) .
S2 O24 1.5224(13) 5_676
S3 O31 1.4386(15) .
S3 O32 1.4394(16) .
S3 O33 1.4480(14) .
S3 O34 1.5317(13) .
O11 Pr01 2.4914(13) 2_655
O12 Pr01 2.4332(14) 3
O13 Pr01 2.4118(13) 5_666
O14 B1 1.453(2) .
O21 Pr01 2.5325(14) 8_566
O22 Pr01 2.5615(13) 3
O23 B1 1.493(2) .
O24 B1 1.485(2) .
O24 S2 1.5224(13) 5_676
O31 Pr01 2.4592(14) 5_666
O33 Pr01 2.3809(14) 6_566
O34 B1 1.448(2) .
