#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:21:50 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/02/7700267.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_7700267
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_sum            'B7 F O12 Sn2'
_chemical_formula_weight         524.05
_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-2013
_audit_update_record
;
2018-08-23 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 93.5650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3799(2)
_cell_length_b                   8.5978(2)
_cell_length_c                   23.7071(8)
_cell_measurement_reflns_used    36715
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      3.079
_cell_volume                     2111.63(10)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_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_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36715
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.079
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6858
_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    3.297
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.877
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0349
_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)+(0.0210P)²+27.7161P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2674
_reflns_number_total             3084
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01901d2.cif
_cod_data_source_block           Sn2B7O12F
_cod_depositor_comments
'Adding full bibliography for 7700266--7700267.cif.'
_cod_database_code               7700267
_publcif_datablock.id            {d5944d16-fa9d-4f77-9d91-cf06101c000a}
_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   0.699
_shelx_estimated_absorpt_t_max   0.953
_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, 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
Sn1 Sn 0.40412(3) 0.66830(4) 0.00535(2) 0.01289(8) Uani 1 1 d
Sn2 Sn 0.36537(3) 0.43012(3) 0.16216(2) 0.01347(8) Uani 1 1 d
B1 B 0.2214(4) 0.7372(5) 0.2225(2) 0.0103(8) Uani 1 1 d
B2 B 0.3193(5) 0.9964(6) 0.2214(2) 0.0138(9) Uani 1 1 d
B3 B 0.4306(5) 0.7816(6) 0.1808(2) 0.0126(9) Uani 1 1 d
B4 B 0.5945(4) 0.8328(5) 0.1143(2) 0.0093(8) Uani 1 1 d
B5 B 0.5922(5) 1.1196(6) 0.1409(2) 0.0120(9) Uani 1 1 d
B6 B 0.4294(5) 1.0210(6) 0.0751(2) 0.0109(8) Uani 1 1 d
B7 B 0.7000(4) 0.6274(5) 0.0577(2) 0.0105(9) Uani 1 1 d
O12 O 0.2357(3) 0.8967(3) 0.24407(12) 0.0102(6) Uani 1 1 d
O13 O 0.3492(3) 0.6770(3) 0.20383(13) 0.0104(6) Uani 1 1 d
O15 O 0.1324(3) 0.7398(4) 0.17292(14) 0.0167(7) Uani 1 1 d
O21 O 0.1739(3) 0.6487(4) 0.26764(15) 0.0183(7) Uani 1 1 d
O23 O 0.4070(4) 0.9385(4) 0.18502(17) 0.0267(9) Uani 1 1 d
O34 O 0.5348(3) 0.7312(3) 0.15427(13) 0.0125(6) Uani 1 1 d
O45 O 0.6517(3) 0.9751(3) 0.14311(12) 0.0098(5) Uani 1 1 d
O46 O 0.4940(3) 0.8828(4) 0.07038(13) 0.0117(6) Uani 1 1 d
O47 O 0.7044(3) 0.7539(4) 0.09177(13) 0.0113(6) Uani 1 1 d
O56 O 0.4876(3) 1.1443(4) 0.10247(14) 0.0145(6) Uani 1 1 d
O67 O 0.3078(3) 1.0343(4) 0.04997(14) 0.0165(6) Uani 1 1 d
O7 O 0.5917(3) 0.5800(4) 0.02725(15) 0.0192(7) Uani 1 1 d
F1 F 0.3465(3) 0.5729(4) 0.07924(13) 0.0282(7) 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'
F F 0.0171 0.0103 '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
F1 Sn1 O7 87.70(14) . .
F1 Sn1 O7 85.85(13) . 5_665
O7 Sn1 O7 73.18(13) . 5_665
F1 Sn1 O46 83.57(11) . .
O7 Sn1 O46 79.34(11) . .
O7 Sn1 O46 150.87(11) 5_665 .
O45 Sn2 F1 73.18(11) 3_445 .
O45 Sn2 O13 80.52(10) 3_445 .
F1 Sn2 O13 82.75(11) . .
O45 Sn2 O12 74.99(10) 3_445 4_545
F1 Sn2 O12 141.96(11) . 4_545
O13 Sn2 O12 71.91(10) . 4_545
O21 B1 O15 112.6(4) . .
O21 B1 O12 105.6(3) . .
O15 B1 O12 108.3(4) . .
O21 B1 O13 112.7(4) . .
O15 B1 O13 107.1(3) . .
O12 B1 O13 110.5(3) . .
O21 B2 O12 124.7(4) 4 .
O21 B2 O23 116.4(4) 4 .
O12 B2 O23 118.8(4) . .
O34 B3 O13 120.3(4) . .
O34 B3 O23 119.9(4) . .
O13 B3 O23 119.8(4) . .
O34 B4 O47 109.5(3) . .
O34 B4 O46 108.6(3) . .
O47 B4 O46 114.1(3) . .
O34 B4 O45 111.4(3) . .
O47 B4 O45 104.4(3) . .
O46 B4 O45 108.8(3) . .
O15 B5 O45 123.4(4) 3 .
O15 B5 O56 117.3(4) 3 .
O45 B5 O56 119.3(4) . .
O56 B6 O67 120.8(4) . .
O56 B6 O46 120.5(4) . .
O67 B6 O46 118.7(4) . .
O47 B7 O7 123.6(4) . .
O47 B7 O67 122.8(4) . 3_545
O7 B7 O67 113.6(4) . 3_545
B2 O12 B1 120.4(3) . .
B2 O12 Sn2 125.9(3) . 4
B1 O12 Sn2 112.0(2) . 4
B3 O13 B1 117.7(3) . .
B3 O13 Sn2 111.3(3) . .
B1 O13 Sn2 121.2(2) . .
B5 O15 B1 127.6(4) 3_445 .
B2 O21 B1 130.8(4) 4_545 .
B3 O23 B2 121.6(4) . .
B3 O34 B4 119.6(3) . .
B5 O45 B4 123.3(3) . .
B5 O45 Sn2 126.0(3) . 3
B4 O45 Sn2 107.7(2) . 3
B6 O46 B4 121.1(3) . .
B6 O46 Sn1 121.0(3) . .
B4 O46 Sn1 115.4(2) . .
B7 O47 B4 126.5(3) . .
B6 O56 B5 119.9(4) . .
B6 O67 B7 135.7(4) . 3_455
B7 O7 Sn1 137.5(3) . .
B7 O7 Sn1 115.5(3) . 5_665
Sn1 O7 Sn1 106.82(13) . 5_665
Sn1 F1 Sn2 157.05(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 F1 2.057(3) .
Sn1 O7 2.124(3) .
Sn1 O7 2.272(3) 5_665
Sn1 O46 2.543(3) .
Sn2 O45 2.269(3) 3_445
Sn2 F1 2.315(3) .
Sn2 O13 2.351(3) .
Sn2 O12 2.533(3) 4_545
B1 O21 1.427(6) .
B1 O15 1.448(6) .
B1 O12 1.468(5) .
B1 O13 1.515(5) .
B2 O21 1.336(5) 4
B2 O12 1.355(6) .
B2 O23 1.385(6) .
B3 O34 1.356(6) .
B3 O13 1.371(6) .
B3 O23 1.375(6) .
B4 O34 1.455(6) .
B4 O47 1.457(5) .
B4 O46 1.491(5) .
B4 O45 1.505(5) .
B5 O15 1.334(6) 3
B5 O45 1.387(6) .
B5 O56 1.389(6) .
B6 O56 1.365(6) .
B6 O67 1.366(5) .
B6 O46 1.373(5) .
B7 O47 1.353(5) .
B7 O7 1.361(6) .
B7 O67 1.397(5) 3_545
O12 Sn2 2.533(3) 4
O15 B5 1.334(6) 3_445
O21 B2 1.336(5) 4_545
O45 Sn2 2.269(3) 3
O67 B7 1.398(5) 3_455
O7 Sn1 2.272(3) 5_665
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{d5944d16-fa9d-4f77-9d91-cf06101c000a} 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
{d5944d16-fa9d-4f77-9d91-cf06101c000a} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
EX
