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.
Richtera, Lukas; Jancik, Vojtech; Martínez-Otero, Diego; Pokluda, Ales; Zak, Zdirad; Taraba, Jan; Touzin, Jiri; Inorganic chemistry 53 (2014) 6569–6577; doi:10.1021/ic500137z

data_4339993
_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         'O12 Se4'
_chemical_formula_sum            'O12 Se4'
_chemical_formula_weight         507.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.527(3)
_cell_length_b                   9.527(3)
_cell_length_c                   5.1710(10)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      3.76
_cell_volume                     469.3(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM-4 point detector'
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_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1459
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
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_diffrn_reflns_theta_max         30.029
_diffrn_reflns_theta_min         3.024
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'after every 150 reflections'
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_exptl_absorpt_correction_T_min  0.0618
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;
Bruker SHELXTL V5.1, XEMP program
;
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_refine_diff_density_min         -0.672
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_refine_ls_abs_structure_details
;
 Flack x determined using 188 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
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_refine_ls_number_parameters     38
_refine_ls_number_reflns         684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+0.9120P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                542
_reflns_number_total             684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500137z_si_002.cif
_cod_data_source_block           (SeO3)4
_cod_depositor_comments
'Adding full bibliography for 4339987--4339996.cif.'
_cod_original_cell_volume        469.3(3)
_cod_database_code               4339993
_shelx_estimated_absorpt_t_min   0.062
_shelx_estimated_absorpt_t_max   0.088
_shelxl_version_number           2013-2
_shelx_res_checksum              82877
_shelx_hkl_checksum              26768