#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:21:50 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/02/7700266.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_7700266
loop_
_publ_author_name
'Schäfer, Martin J'
'Jantz, Stephan G.'
'Pielnhofer, Florian'
'Höppe, Henning A'
_publ_section_title
;
 The very first normal-pressure tin borate
 Sn₃B₄O₉, and the intermediate
 Sn₂[B₇O₁₂]F.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10398
_journal_page_last               10402
_journal_paper_doi               10.1039/c9dt01901d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'B4 O9 Sn3'
_chemical_formula_sum            'B4 O9 Sn3'
_chemical_formula_weight         543.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-08-23 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 101.8470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6807(3)
_cell_length_b                   12.0678(4)
_cell_length_c                   9.2496(3)
_cell_measurement_reflns_used    13906
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.813
_cell_volume                     839.08(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Venture Bruker'
_diffrn_measurement_method       'generic phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.996
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.890
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS 2007/2 (Sheldrick, G.M., 2007)'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.301
_exptl_crystal_description       rod
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.961
_refine_diff_density_min         -3.550
_refine_diff_density_rms         0.706
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         13906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0237P)²+1.1434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10550
_reflns_number_total             13906
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01901d3.cif
_cod_data_source_block           Sn3B4O9
_cod_depositor_comments
'Adding full bibliography for 7700266--7700267.cif.'
_cod_database_code               7700266
_publcif_datablock.id            {98a6a171-7322-4e9f-9a9e-4d780fab2565}
_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.
;
_shelx_estimated_absorpt_t_min   0.441
_shelx_estimated_absorpt_t_max   0.776
_shelxl_version_number           2013-4
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;
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'
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
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
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_
_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_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
