data_publication

# 1. SUBMISSION DETAILS

_publ_contact_author
;
	'Univ.-Prof. Dr. Hubert Huppertz
	Institute of General, Inorganic and Theoretical Chemistry
	University of Innsbruck
	Innrain 80-82
	A-6020 Innsbruck
	AUSTRIA, Europe'
;

_publ_contact_author_phone       '+43 (0)512 507 57000'
_publ_contact_author_fax         '+43 (0)512 507 57099'
_publ_contact_author_email       'hubert.huppertz@uibk.ac.at'
_publ_requested_journal          'Z. Kristallogr. NCS'


#===================================================================== 


# 2. TITLE AND AUTHOR LIST

_publ_section_title
;
Serendipitous formation and crystal structure of Sm[B(SO4)3]
;

loop_
 _publ_author_name
 _publ_author_address

	'Joern Bruns'
;	Institute of General, Inorganic and Theoretical Chemistry
	University of Innsbruck
	Innrain 80-82
	6020 Innsbruck
	Austria
;
	'Hubert Huppertz'
;	Institute of General, Inorganic and Theoretical Chemistry
	University of Innsbruck
	Innrain 80-82
	6020 Innsbruck
	Austria
;

#=====================================================================

# 3. CHEMICAL DATA

data_SmBS3O12

_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;

_shelxl_version_number            2013-4
_chemical_name_systematic         'samarium-trissulfatoborate'
_chemical_name_common             'Samariumborosulfate'
_chemical_formula_moiety          'Sm B O12 S3'
_chemical_formula_sum             'B O12 S3 Sm '
_chemical_formula_weight           449.34

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'
 'Sm' 'Sm' -0.1638 3.4418
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system       'monoclinic'
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 1 2/c 1'
_space_group_name_Hall            '-C 2yc'
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'

_cell_length_a                    13.6077(6)
_cell_length_b                    11.4725(4)
_cell_length_c                    11.1229(4)
_cell_angle_alpha                 90
_cell_angle_beta                  93.5718(12)
_cell_angle_gamma                 90
_cell_volume                      1733.07(12)
_cell_formula_units_Z             8
_cell_measurement_reflns_used     4853
_cell_measurement_temperature     173(2)
_cell_measurement_theta_max       37.84
_cell_measurement_theta_min       2.32
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     7.567
_exptl_absorpt_correction_T_max   0.7474
_exptl_absorpt_correction_T_min   0.5636
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details    'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour             colorless
_exptl_crystal_density_diffrn     3.444
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              1688
_exptl_crystal_size_max           0.11
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.06
_exptl_transmission_factor_max    0.7474
_exptl_transmission_factor_min    0.5636
_diffrn_reflns_av_R_equivalents   0.0333
_diffrn_reflns_av_unetI/netI      0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max        23
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_number             31611
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          37.844
_diffrn_reflns_theta_min          2.324
_diffrn_ambient_temperature       173.0
_diffrn_detector_area_resol_mean  10.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type   'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'Incoatec Microfocus'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 4351
_reflns_number_total              4675
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection        'Bruker Apex II'
_computing_data_reduction         'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2008)'
_computing_structure_solution     'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max          0.755
_refine_diff_density_min          -2.225
_refine_diff_density_rms          0.200
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.098
_refine_ls_hydrogen_treatment     undef
_refine_ls_matrix_type            full
_refine_ls_number_parameters      154
_refine_ls_number_reflns          4675
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0228
_refine_ls_R_factor_gt            0.0197
_refine_ls_restrained_S_all       1.098
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0222P)²+3.8755P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0448
_refine_ls_wR_factor_ref          0.0458
_refine_special_details
;
 ?
;
_olex2_refinement_description
;
;
_atom_sites_solution_hydrogens    .
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
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
 Sm1 Sm 0.18794(2) 0.04858(2) 0.15578(2) 0.00360(2) Uani 1 1 d . . . . .
 S1 S 0.36291(3) 0.29843(3) 0.13879(3) 0.00380(6) Uani 1 1 d . . . . .
 S3 S -0.12768(3) 0.51353(3) -0.07719(3) 0.00435(6) Uani 1 1 d . . . . .
 S2 S -0.07792(3) 0.15037(3) 0.08028(3) 0.00431(6) Uani 1 1 d . . . . .
 O13 O 0.32019(9) 0.34201(10) 0.02450(11) 0.00722(19) Uani 1 1 d . . . . .
 O11 O 0.30617(9) 0.20207(11) 0.18362(11) 0.0091(2) Uani 1 1 d . . . . .
 O12 O 0.37991(9) 0.38992(10) 0.22730(11) 0.0087(2) Uani 1 1 d . . . . .
 O14 O 0.46646(9) 0.25101(10) 0.11758(11) 0.00638(18) Uani 1 1 d . . . . .
 O33 O -0.08089(9) 0.63303(10) -0.06009(11) 0.00742(19) Uani 1 1 d . . . . .
 O34 O -0.04155(9) 0.43194(10) -0.09630(11) 0.00593(18) Uani 1 1 d . . . . .
 O24 O -0.07657(9) 0.27824(10) 0.03928(12) 0.0084(2) Uani 1 1 d . . . . .
 O21 O 0.02058(10) 0.11814(12) 0.12361(12) 0.0119(2) Uani 1 1 d . . . . .
 O31 O -0.17686(10) 0.48117(11) 0.02887(12) 0.0090(2) Uani 1 1 d . . . . .
 O32 O -0.18626(9) 0.51974(11) -0.18858(12) 0.0086(2) Uani 1 1 d . . . . .
 O22 O -0.14829(10) 0.15082(11) 0.17291(12) 0.0096(2) Uani 1 1 d . . . . .
 O23 O -0.11274(11) 0.08230(12) -0.02284(12) 0.0143(2) Uani 1 1 d . . . . .
 B1 B -0.00024(13) 0.32987(14) -0.02847(16) 0.0058(3) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Sm1 O13 2.3624(12) 7 ?
 Sm1 O11 2.3922(12) . ?
 Sm1 O12 2.4509(12) 4_545 ?
 Sm1 O21 2.4187(13) . ?
 Sm1 O31 2.5098(13) 3_545 ?
 Sm1 O32 2.4843(12) 8_556 ?
 Sm1 O22 2.3293(12) 2 ?
 Sm1 O23 2.3021(13) 5 ?
 S1 O13 1.4532(12) . ?
 S1 O11 1.4542(13) . ?
 S1 O12 1.4478(12) . ?
 S1 O14 1.5422(12) . ?
 S3 O33 1.5185(12) . ?
 S3 O34 1.5252(12) . ?
 S3 O31 1.4407(13) . ?
 S3 O32 1.4327(13) . ?
 S2 O24 1.5366(12) . ?
 S2 O21 1.4440(13) . ?
 S2 O22 1.4497(13) . ?
 S2 O23 1.4430(13) . ?
 O13 Sm1 2.3624(12) 7 ?
 O12 Sm1 2.4509(12) 4 ?
 O14 B1 1.453(2) 7 ?
 O33 B1 1.495(2) 5_565 ?
 O34 B1 1.485(2) . ?
 O24 B1 1.447(2) . ?
 O31 Sm1 2.5098(13) 3_455 ?
 O32 Sm1 2.4844(12) 8_455 ?
 O22 Sm1 2.3293(12) 2 ?
 O23 Sm1 2.3021(13) 5 ?
 B1 O14 1.453(2) 7 ?
 B1 O33 1.495(2) 5_565 ?

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
 O13 Sm1 O11 73.40(4) 7 . ?
 O13 Sm1 O12 147.75(4) 7 4_545 ?
 O13 Sm1 O21 72.85(4) 7 . ?
 O13 Sm1 O31 71.55(4) 7 3_545 ?
 O13 Sm1 O32 138.84(4) 7 8_556 ?
 O11 Sm1 O12 138.64(4) . 4_545 ?
 O11 Sm1 O21 113.31(5) . . ?
 O11 Sm1 O31 77.82(4) . 3_545 ?
 O11 Sm1 O32 73.35(4) . 8_556 ?
 O12 Sm1 O31 112.53(4) 4_545 3_545 ?
 O12 Sm1 O32 70.24(4) 4_545 8_556 ?
 O21 Sm1 O12 86.63(4) . 4_545 ?
 O21 Sm1 O31 137.30(4) . 3_545 ?
 O21 Sm1 O32 143.97(4) . 8_556 ?
 O32 Sm1 O31 78.31(4) 8_556 3_545 ?
 O22 Sm1 O13 115.20(5) 2 7 ?
 O22 Sm1 O11 73.24(4) 2 . ?
 O22 Sm1 O12 79.97(4) 2 4_545 ?
 O22 Sm1 O21 71.99(5) 2 . ?
 O22 Sm1 O31 146.16(4) 2 3_545 ?
 O22 Sm1 O32 76.91(5) 2 8_556 ?
 O23 Sm1 O13 78.81(5) 5 7 ?
 O23 Sm1 O11 146.27(5) 5 . ?
 O23 Sm1 O12 71.90(5) 5 4_545 ?
 O23 Sm1 O21 75.13(5) 5 . ?
 O23 Sm1 O31 75.51(5) 5 3_545 ?
 O23 Sm1 O32 120.08(5) 5 8_556 ?
 O23 Sm1 O22 137.52(5) 5 2 ?
 O13 S1 O11 111.69(7) . . ?
 O13 S1 O14 107.88(7) . . ?
 O11 S1 O14 107.10(7) . . ?
 O12 S1 O13 112.56(7) . . ?
 O12 S1 O11 112.56(8) . . ?
 O12 S1 O14 104.53(7) . . ?
 O33 S3 O34 104.58(7) . . ?
 O31 S3 O33 110.04(8) . . ?
 O31 S3 O34 110.87(7) . . ?
 O32 S3 O33 105.65(7) . . ?
 O32 S3 O34 107.52(7) . . ?
 O32 S3 O31 117.33(8) . . ?
 O21 S2 O24 108.39(8) . . ?
 O21 S2 O22 113.84(8) . . ?
 O22 S2 O24 103.19(7) . . ?
 O23 S2 O24 106.87(8) . . ?
 O23 S2 O21 112.26(9) . . ?
 O23 S2 O22 111.60(8) . . ?
 S1 O13 Sm1 156.98(8) . 7 ?
 S1 O11 Sm1 151.92(8) . . ?
 S1 O12 Sm1 148.18(8) . 4 ?
 B1 O14 S1 131.33(11) 7 . ?
 B1 O33 S3 128.78(10) 5_565 . ?
 B1 O34 S3 133.10(11) . . ?
 B1 O24 S2 124.57(11) . . ?
 S2 O21 Sm1 168.45(9) . . ?
 S3 O31 Sm1 140.83(7) . 3_455 ?
 S3 O32 Sm1 155.37(8) . 8_455 ?
 S2 O22 Sm1 140.95(8) . 2 ?
 S2 O23 Sm1 167.00(9) . 5 ?
 O14 B1 O33 112.29(13) 7 5_565 ?
 O14 B1 O34 106.43(13) 7 . ?
 O34 B1 O33 110.54(12) . 5_565 ?
 O24 B1 O14 111.20(13) . 7 ?
 O24 B1 O33 107.33(13) . 5_565 ?
 O24 B1 O34 109.03(13) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
