#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:08:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179502 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/99/4339992.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_4339992
loop_
_publ_author_name
'Richtera, Lukas'
'Jancik, Vojtech'
'Martínez-Otero, Diego'
'Pokluda, Ales'
'Zak, Zdirad'
'Taraba, Jan'
'Touzin, Jiri'
_publ_section_title
;
 Taming the Oxidative Power of SeO3 in 1,4-Dioxane, Isolation of Two New
 Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic
 Esters of Selenic Acid.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6569
_journal_page_last               6577
_journal_paper_doi               10.1021/ic500137z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'O9 Se3'
_chemical_formula_sum            'O9 Se3'
_chemical_formula_weight         380.88
_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'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.008(2)
_cell_length_b                   20.213(6)
_cell_length_c                   5.462(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.7
_cell_volume                     728.7(4)
_computing_cell_refinement       'KM-4 software'
_computing_data_collection       'KM-4 software'
_computing_data_reduction        'KM-4 software'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'KUMA KM-4 point detector'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1764
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.015
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'after every 150 reflections'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.163
_exptl_absorpt_correction_T_max  0.0924
_exptl_absorpt_correction_T_min  0.0645
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
Bruker SHELXTL V5.1, XEMP program
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.472
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.823
_refine_diff_density_min         -2.263
_refine_diff_density_rms         0.347
_refine_ls_extinction_coef       0.0121(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0512
_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)+(0.1036P)²+0.1258P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1225
_reflns_number_total             1596
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic500137z_si_002.cif
_cod_data_source_block           (SEO3)3
_cod_depositor_comments
'Adding full bibliography for 4339987--4339996.cif.'
_cod_database_code               4339992
#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.
;
_shelx_estimated_absorpt_t_min   0.065
_shelx_estimated_absorpt_t_max   0.092
_shelxl_version_number           2013-2
#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 0.26333(11) 0.54795(4) 0.09150(15) 0.0207(3) Uani 1 1 d
Se2 Se 0.50869(11) 0.65770(3) 0.47005(16) 0.0197(3) Uani 1 1 d
Se3 Se 0.03904(11) 0.66420(4) 0.25938(15) 0.0196(3) Uani 1 1 d
O1 O 0.4860(8) 0.5791(3) 0.3267(12) 0.0286(13) Uani 1 1 d
O2 O 0.2731(8) 0.6596(3) 0.5208(12) 0.0260(13) Uani 1 1 d
O3 O 0.1196(8) 0.6224(3) 0.0212(11) 0.0242(11) Uani 1 1 d
O4 O 0.3090(9) 0.5338(3) -0.1666(13) 0.0354(15) Uani 1 1 d
O5 O 0.1726(9) 0.4965(3) 0.2401(13) 0.0328(14) Uani 1 1 d
O6 O 0.6678(9) 0.6491(3) 0.7492(13) 0.0330(15) Uani 1 1 d
O7 O 0.5065(9) 0.7111(3) 0.2575(12) 0.0331(15) Uani 1 1 d
O8 O -0.1089(9) 0.6196(3) 0.3489(12) 0.0300(13) Uani 1 1 d
O9 O -0.0040(9) 0.7368(3) 0.1529(11) 0.0276(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'
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
O4 Se1 O5 125.4(4)
O4 Se1 O1 108.7(3)
O5 Se1 O1 105.7(3)
O4 Se1 O3 103.4(3)
O5 Se1 O3 111.8(3)
O1 Se1 O3 98.8(2)
O6 Se2 O7 128.2(4)
O6 Se2 O1 105.1(3)
O7 Se2 O1 108.3(3)
O6 Se2 O2 104.3(3)
O7 Se2 O2 108.8(3)
O1 Se2 O2 98.1(3)
O9 Se3 O8 126.0(3)
O9 Se3 O2 110.9(3)
O8 Se3 O2 104.3(3)
O9 Se3 O3 103.8(3)
O8 Se3 O3 110.9(3)
O2 Se3 O3 97.3(3)
Se2 O1 Se1 124.8(3)
Se2 O2 Se3 122.3(4)
Se1 O3 Se3 122.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 O4 1.573(7)
Se1 O5 1.578(6)
Se1 O1 1.770(5)
Se1 O3 1.780(6)
Se2 O6 1.567(6)
Se2 O7 1.582(6)
Se2 O1 1.755(5)
Se2 O2 1.764(6)
Se3 O9 1.569(5)
Se3 O8 1.571(6)
Se3 O2 1.779(6)
Se3 O3 1.794(6)
