data_Sn3B4O9

_audit_update_record
;
2018-08-23 # Formatted by publCIF

;
_publcif_datablock.id '{98a6a171-7322-4e9f-9a9e-4d780fab2565}'

_publ_section_exptl_refinement
;
(type here to add)
;

_publ_section_exptl_prep
;
(type here to add)
;

_publ_manuscript_text
;
(type here to add)
;
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'B4 O9 Sn3'
_chemical_formula_sum
 'B4 O9 Sn3' 
_chemical_formula_weight          543.37

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'
 'Sn'  'Sn'  -0.6537   1.4246
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    7.6807(3)
_cell_length_b                    12.0678(4)
_cell_length_c                    9.2496(3)
_cell_angle_alpha                 90
_cell_angle_beta                  101.8470(10)
_cell_angle_gamma                 90
_cell_volume                      839.08(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     13906
_cell_measurement_theta_min       2.813 
_cell_measurement_theta_max       25.242
 
_exptl_crystal_description        rod 
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     4.301          
_exptl_crystal_F_000              968
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.110
_exptl_crystal_size_mid           0.060
_exptl_crystal_size_min           0.030
_exptl_absorpt_coefficient_mu     8.890
_shelx_estimated_absorpt_T_min    0.441
_shelx_estimated_absorpt_T_max    0.776
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.441 
_exptl_absorpt_correction_T_max   0.776
_exptl_absorpt_process_details    
;
'SADABS 2007/2 (Sheldrick, G.M., 2007)'
;  
_exptl_special_details
?
 
_diffrn_ambient_temperature       298(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                      
_diffrn_measurement_device_type   'D8 Venture Bruker'   
_diffrn_measurement_method        'generic phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             13906
_diffrn_reflns_av_unetI/netI      0.0356
_diffrn_reflns_av_R_equivalents   ?
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.813
_diffrn_reflns_theta_max          44.996
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              13906
_reflns_number_gt                 10550
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0237P)²+1.1434P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        ?
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          13906
_refine_ls_number_parameters      147
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0499
_refine_ls_R_factor_gt            0.0319
_refine_ls_wR_factor_ref          0.0738
_refine_ls_wR_factor_gt           0.0704
_refine_ls_goodness_of_fit_ref    1.098
_refine_ls_restrained_S_all       1.098
_refine_ls_shift/su_max           0.022
_refine_ls_shift/su_mean          0.000
 
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
Sn1 Sn 0.34195(2) 0.85438(2) 0.36709(2) 0.00837(3) Uani 1 1 d . . . . .
Sn2 Sn 0.89952(2) 0.83360(2) 0.54859(2) 0.00761(3) Uani 1 1 d . . . . .
Sn3 Sn -0.04378(2) 0.38898(2) 0.65718(2) 0.00807(3) Uani 1 1 d . . . . .
B1 B 0.5714(3) 0.7119(2) 0.6115(2) 0.0066(3) Uani 1 1 d . . . . .
B2 B 0.4126(3) 0.5410(2) 0.6532(3) 0.0074(3) Uani 1 1 d . . . . .
B3 B 0.2458(3) 0.7197(2) 0.6235(2) 0.0065(3) Uani 1 1 d . . . . .
B4 B 0.3478(3) 0.3259(2) 0.6452(2) 0.0060(3) Uani 1 1 d . . . . .
O1 O 0.7408(2) 0.75911(15) 0.69188(17) 0.0080(2) Uani 1 1 d . . . . .
O2 O 0.1646(2) 0.32388(15) 0.56734(18) 0.0081(2) Uani 1 1 d . . . . .
O3 O 0.5457(2) 0.73160(15) 0.45081(17) 0.0078(2) Uani 1 1 d . . . . .
O4 O 0.1670(2) 0.75214(15) 0.46793(17) 0.0084(2) Uani 1 1 d . . . . .
O5 O 0.3804(2) 0.26089(15) 0.78823(16) 0.0072(2) Uani 1 1 d . . . . .
O6 O 0.5691(2) 0.59536(15) 0.6494(2) 0.0100(3) Uani 1 1 d . . . . .
O7 O 0.2551(2) 0.59867(15) 0.6318(2) 0.0103(3) Uani 1 1 d . . . . .
O8 O 0.4244(2) 0.77116(14) 0.66333(17) 0.0065(2) Uani 1 1 d . . . . .
O9 O 0.4238(3) 0.43261(15) 0.6898(2) 0.0132(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
Sn1 O1 2.1421(17) 4_575 ?
Sn1 O4 2.1709(17) . ?
Sn1 O3 2.1787(16) . ?
Sn2 O1 2.1710(16) . ?
Sn2 O2 2.1879(17) 3_666 ?
Sn2 O5 2.2040(15) 2_656 ?
Sn2 O4 2.5244(17) 1_655 ?
Sn3 O2 2.1012(16) . ?
Sn3 O4 2.1645(17) 3_566 ?
Sn3 O8 2.2347(15) 2_546 ?
B1 O6 1.450(3) . ?
B1 O1 1.475(3) . ?
B1 O3 1.478(3) . ?
B1 O8 1.496(3) . ?
B2 O9 1.350(3) . ?
B2 O7 1.374(3) . ?
B2 O6 1.376(3) . ?
B3 O7 1.463(3) . ?
B3 O5 1.476(3) 2_556 ?
B3 O8 1.481(3) . ?
B3 O4 1.495(3) . ?
B4 O9 1.439(3) . ?
B4 O2 1.443(3) . ?
B4 O3 1.496(3) 3_666 ?
B4 O5 1.514(3) . ?
O1 Sn1 2.1421(17) 4_676 ?
O2 Sn2 2.1879(17) 3_666 ?
O3 B4 1.496(3) 3_666 ?
O4 Sn3 2.1645(17) 3_566 ?
O4 Sn2 2.5244(17) 1_455 ?
O5 B3 1.476(3) 2_546 ?
O5 Sn2 2.2040(15) 2_646 ?
O8 Sn3 2.2348(15) 2_556 ?
 
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
O1 Sn1 O4 78.55(6) 4_575 . ?
O1 Sn1 O3 87.51(6) 4_575 . ?
O4 Sn1 O3 85.62(6) . . ?
O1 Sn2 O2 80.88(6) . 3_666 ?
O1 Sn2 O5 82.24(6) . 2_656 ?
O2 Sn2 O5 93.08(6) 3_666 2_656 ?
O1 Sn2 O4 127.74(6) . 1_655 ?
O2 Sn2 O4 68.40(6) 3_666 1_655 ?
O5 Sn2 O4 59.41(5) 2_656 1_655 ?
O2 Sn3 O4 77.25(6) . 3_566 ?
O2 Sn3 O8 79.99(6) . 2_546 ?
O4 Sn3 O8 87.95(6) 3_566 2_546 ?
O6 B1 O1 107.82(17) . . ?
O6 B1 O3 113.15(18) . . ?
O1 B1 O3 111.49(17) . . ?
O6 B1 O8 109.83(17) . . ?
O1 B1 O8 107.46(17) . . ?
O3 B1 O8 106.96(17) . . ?
O9 B2 O7 122.4(2) . . ?
O9 B2 O6 117.2(2) . . ?
O7 B2 O6 120.2(2) . . ?
O7 B3 O5 109.73(18) . 2_556 ?
O7 B3 O8 111.90(17) . . ?
O5 B3 O8 113.64(17) 2_556 . ?
O7 B3 O4 108.53(18) . . ?
O5 B3 O4 105.18(17) 2_556 . ?
O8 B3 O4 107.50(17) . . ?
O9 B4 O2 117.05(19) . . ?
O9 B4 O3 110.28(18) . 3_666 ?
O2 B4 O3 106.96(17) . 3_666 ?
O9 B4 O5 103.22(17) . . ?
O2 B4 O5 113.35(17) . . ?
O3 B4 O5 105.41(16) 3_666 . ?
B1 O1 Sn1 106.24(13) . 4_676 ?
B1 O1 Sn2 113.61(12) . . ?
Sn1 O1 Sn2 124.39(7) 4_676 . ?
B4 O2 Sn3 122.69(13) . . ?
B4 O2 Sn2 110.96(13) . 3_666 ?
Sn3 O2 Sn2 113.92(7) . 3_666 ?
B1 O3 B4 123.11(16) . 3_666 ?
B1 O3 Sn1 113.86(13) . . ?
B4 O3 Sn1 123.02(12) 3_666 . ?
B3 O4 Sn3 110.79(13) . 3_566 ?
B3 O4 Sn1 113.48(12) . . ?
Sn3 O4 Sn1 117.30(7) 3_566 . ?
B3 O4 Sn2 90.63(11) . 1_455 ?
Sn3 O4 Sn2 99.87(6) 3_566 1_455 ?
Sn1 O4 Sn2 121.25(8) . 1_455 ?
B3 O5 B4 130.41(16) 2_546 . ?
B3 O5 Sn2 104.72(12) 2_546 2_646 ?
B4 O5 Sn2 110.98(12) . 2_646 ?
B2 O6 B1 121.46(18) . . ?
B2 O7 B3 122.99(18) . . ?
B3 O8 B1 116.16(16) . . ?
B3 O8 Sn3 132.00(13) . 2_556 ?
B1 O8 Sn3 108.70(12) . 2_556 ?
B2 O9 B4 142.6(2) . . ?
 
_refine_diff_density_max    3.961
_refine_diff_density_min   -3.550
_refine_diff_density_rms    0.706

_shelxl_version_number 2013-4



loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
'{98a6a171-7322-4e9f-9a9e-4d780fab2565}' y y y

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?

_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
"{98a6a171-7322-4e9f-9a9e-4d780fab2565}" "_publcif_info_datablock.publ_exptl"
loop_
_publcif_info_cif.paper_type
 EX



_publcif_funding_html
;
;
