#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:12:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179527 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/24/4342456.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_4342456
loop_
_publ_author_name
'Daub, Michael'
'Scherer, Harald'
'Hillebrecht, Harald'
_publ_section_title
;
 Synthesis, Crystal Structure, and Spectroscopy of the Mixed-Valent
 Boroseleniteselenate B2Se3O10.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2325
_journal_paper_doi               10.1021/ic502916j
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'B2 O10 Se3'
_chemical_formula_weight         418.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.922(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.3466(2)
_cell_length_b                   7.9237(4)
_cell_length_c                   22.1460(9)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     759.92(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Crystal impact, 2005)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.007
_diffrn_measured_fraction_theta_max 1.007
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         microsource
_diffrn_radiation_type           Mo_K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.007
_diffrn_reflns_Laue_measured_fraction_max 1.007
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8107
_diffrn_reflns_point_group_measured_fraction_full 1.007
_diffrn_reflns_point_group_measured_fraction_max 1.007
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_min         1.846
_exptl_absorpt_coefficient_mu    14.564
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.658
_exptl_crystal_description       irregular
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.474
_refine_diff_density_min         -2.814
_refine_diff_density_rms         0.669
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0361
_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)+16.0731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2037
_reflns_number_total             2270
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic502916j_si_002.cif
_cod_data_source_block           B2Se3O10
_cod_depositor_comments          'Adding full bibliography for 4342456.cif.'
_cod_database_code               4342456
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Se1 Se 0.07829(14) 0.96721(8) 0.35667(3) 0.00614(15) Uani 1 1 d
Se2 Se 0.48327(14) 1.45600(8) 0.31277(3) 0.00532(15) Uani 1 1 d
Se3 Se -0.20848(14) 0.72282(8) 0.50471(3) 0.00516(15) Uani 1 1 d
O11 O 0.2341(12) 1.1400(6) 0.3400(2) 0.0142(10) Uani 1 1 d
O12 O -0.0277(12) 0.9487(7) 0.4239(2) 0.0142(15) Uani 1 1 d
O13 O 0.3237(10) 0.8039(6) 0.3473(2) 0.0077(8) Uani 1 1 d
O14 O -0.2228(11) 0.9350(6) 0.3038(2) 0.0076(8) Uani 1 1 d
O21 O 0.6417(11) 1.3366(6) 0.25965(19) 0.0076(8) Uani 1 1 d
O22 O 0.7226(10) 1.3797(6) 0.37099(19) 0.0062(8) Uani 1 1 d
O23 O 0.6860(11) 1.6383(6) 0.3007(2) 0.0086(8) Uani 1 1 d
O31 O 0.1748(10) 0.7004(6) 0.5253(2) 0.0066(8) Uani 1 1 d
O32 O -0.2350(11) 0.6011(6) 0.4413(2) 0.0074(8) Uani 1 1 d
O33 O -0.3385(11) 0.5869(6) 0.5572(2) 0.0083(9) Uani 1 1 d
B1 B 0.5383(16) 0.8028(9) 0.2991(3) 0.0053(11) Uani 1 1 d
B2 B -0.3315(16) 0.4240(9) 0.4331(3) 0.0067(12) 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
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
O11 Se1 O12 117.3(3) . .
O11 Se1 O14 106.7(3) . .
O12 Se1 O14 111.2(3) . .
O11 Se1 O13 110.1(2) . .
O12 Se1 O13 106.1(2) . .
O14 Se1 O13 104.8(2) . .
O22 Se2 O21 94.0(2) . .
O22 Se2 O23 97.3(2) . .
O21 Se2 O23 96.7(2) . .
O31 Se3 O32 99.1(2) . .
O31 Se3 O33 97.2(2) . .
O32 Se3 O33 101.6(2) . .
B1 O13 Se1 122.3(4) . .
B1 O14 Se1 130.7(4) 1_455 .
B1 O21 Se2 119.5(4) 2_655 .
B2 O22 Se2 119.5(4) 1_665 .
B1 O23 Se2 121.7(4) 1_565 .
B2 O31 Se3 128.9(4) 3_566 .
B2 O32 Se3 129.9(4) . .
B2 O33 Se3 121.2(4) 3_466 .
O23 B1 O14 109.2(5) 1_545 1_655
O23 B1 O13 107.0(5) 1_545 .
O14 B1 O13 115.5(5) 1_655 .
O23 B1 O21 112.5(5) 1_545 2_645
O14 B1 O21 104.5(5) 1_655 2_645
O13 B1 O21 108.3(5) . 2_645
O22 B2 O33 111.2(5) 1_445 3_466
O22 B2 O32 106.2(5) 1_445 .
O33 B2 O32 108.0(5) 3_466 .
O22 B2 O31 108.9(5) 1_445 3_566
O33 B2 O31 105.9(5) 3_466 3_566
O32 B2 O31 116.7(5) . 3_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 O11 1.585(5) .
Se1 O12 1.602(5) .
Se1 O14 1.699(5) .
Se1 O13 1.702(5) .
Se2 O22 1.697(4) .
Se2 O21 1.701(4) .
Se2 O23 1.725(5) .
Se3 O31 1.699(4) .
Se3 O32 1.699(4) .
Se3 O33 1.715(5) .
O13 B1 1.477(8) .
O14 B1 1.472(8) 1_455
O21 B1 1.483(8) 2_655
O22 B2 1.459(8) 1_665
O23 B1 1.452(8) 1_565
O31 B2 1.475(8) 3_566
O32 B2 1.471(8) .
O33 B2 1.471(8) 3_466
B1 O23 1.452(8) 1_545
B1 O14 1.472(8) 1_655
B1 O21 1.483(8) 2_645
B2 O22 1.458(8) 1_445
B2 O33 1.471(8) 3_466
B2 O31 1.475(8) 3_566
