#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:08:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179502 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/99/4339996.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_4339996
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         'H2 O7 Se2, C4 H8 O2'
_chemical_formula_sum            'C4 H10 O9 Se2'
_chemical_formula_weight         360.04
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.176(5)
_cell_angle_beta                 94.356(6)
_cell_angle_gamma                98.012(6)
_cell_formula_units_Z            2
_cell_length_a                   5.9908(5)
_cell_length_b                   7.0818(5)
_cell_length_c                   12.2584(8)
_cell_measurement_reflns_used    6168
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.366
_cell_measurement_theta_min      2.911
_cell_volume                     512.36(7)
_computing_cell_refinement       'Version 1.171.35.19 CrysAlis171'
_computing_data_collection       '1.170.27 CrysAlis170'
_computing_data_reduction        'Version 1.171.35.19 CrysAlis171'
_computing_molecular_graphics    'Gretep and POV-Ray'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'KM4CCD/SAPPHIRE CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5654
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.911
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    7.247
_exptl_absorpt_correction_T_max  0.4312
_exptl_absorpt_correction_T_min  0.3593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2009/1, Sheldrick'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1858
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0190
_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)+(0.0144P)²+0.7556P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1684
_reflns_number_total             1858
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic500137z_si_002.cif
_cod_data_source_block           H2Se2O7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4339987--4339996.cif.
;
_cod_database_code               4339996
#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   0.531
_shelx_estimated_absorpt_t_max   0.713
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.4277(11) 0.0775(14) 0.1564(6) 0.0155(7) Uani 0.54(4) 1 d D U P A 1
O1 O 0.3995(3) 0.0080(3) 0.29412(15) 0.0189(4) Uani 1 1 d D . . . .
O2 O 0.1583(3) 0.0363(3) 0.10649(15) 0.0164(4) Uani 1 1 d D . . . .
H2 H 0.127(5) 0.140(4) 0.082(3) 0.025 Uiso 1 1 d D U . . .
O3 O 0.520(3) 0.3015(16) 0.1708(13) 0.020(2) Uani 0.54(4) 1 d D U P A 1
O4 O 0.583(3) -0.067(3) 0.1095(12) 0.027(2) Uani 0.54(4) 1 d D U P A 1
O3A O 0.555(3) 0.271(2) 0.1557(17) 0.024(3) Uani 0.46(4) 1 d D U P A 2
O4A O 0.539(3) -0.121(3) 0.1099(15) 0.025(3) Uani 0.46(4) 1 d D U P A 2
Se1A Se 0.4308(12) 0.0586(16) 0.1546(6) 0.0141(8) Uani 0.46(4) 1 d D U P A 2
Se2 Se 0.13653(4) -0.00678(4) 0.35236(2) 0.01174(8) Uani 1 1 d D . . . .
O5 O 0.2426(3) -0.0211(3) 0.48265(15) 0.0144(4) Uani 1 1 d D . . . .
H5 H 0.290(5) -0.125(4) 0.485(2) 0.022 Uiso 1 1 d D U . . .
O6 O -0.0110(3) -0.2035(3) 0.30634(16) 0.0214(4) Uani 1 1 d . . . . .
O7 O 0.0444(3) 0.1923(3) 0.34129(16) 0.0209(4) Uani 1 1 d . . . . .
O8 O 0.0351(3) 0.3242(2) 0.03728(15) 0.0149(4) Uani 1 1 d . . . . .
O9 O 0.4039(3) 0.6696(3) 0.49697(15) 0.0173(4) Uani 1 1 d . . . . .
C1 C 0.1266(5) 0.3875(4) -0.0635(2) 0.0154(6) Uani 1 1 d . . . . .
H1A H 0.1353 0.2757 -0.1144 0.018 Uiso 1 1 calc R U . . .
H1B H 0.2810 0.4586 -0.0470 0.018 Uiso 1 1 calc R U . . .
C2 C 0.0269(5) 0.4853(4) 0.1153(2) 0.0148(6) Uani 1 1 d . . . . .
H2A H 0.1805 0.5570 0.1334 0.018 Uiso 1 1 calc R U . . .
H2B H -0.0320 0.4392 0.1839 0.018 Uiso 1 1 calc R U . . .
C3 C 0.4993(5) 0.5944(4) 0.4016(2) 0.0169(6) Uani 1 1 d . . . . .
H3A H 0.5604 0.7007 0.3582 0.020 Uiso 1 1 calc R U . . .
H3B H 0.3802 0.5098 0.3546 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3133(5) 0.5170(4) 0.5619(2) 0.0169(6) Uani 1 1 d . . . . .
H4A H 0.1909 0.4310 0.5178 0.020 Uiso 1 1 calc R U . . .
H4B H 0.2492 0.5709 0.6268 0.020 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
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_3
O4 Se1 O3 119.9(7) .
O4 Se1 O2 114.9(7) .
O3 Se1 O2 111.6(7) .
O4 Se1 O1 102.8(7) .
O3 Se1 O1 104.4(7) .
O2 Se1 O1 100.1(4) .
Se2 O1 Se1A 122.8(3) .
Se2 O1 Se1 121.3(2) .
O3A Se1A O4A 122.7(8) .
O3A Se1A O2 112.6(8) .
O4A Se1A O2 109.6(8) .
O3A Se1A O1 106.8(8) .
O4A Se1A O1 101.9(8) .
O2 Se1A O1 100.1(4) .
O6 Se2 O7 121.70(10) .
O6 Se2 O5 110.85(10) .
O7 Se2 O5 109.45(9) .
O6 Se2 O1 107.53(10) .
O7 Se2 O1 108.26(10) .
O5 Se2 O1 95.90(9) .
C2 O8 C1 111.33(19) .
C4 O9 C3 111.0(2) .
O8 C1 C2 108.3(2) 2_565
O8 C2 C1 107.9(2) 2_565
O9 C3 C4 109.4(2) 2_666
O9 C4 C3 109.2(2) 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 O4 1.588(8) .
Se1 O3 1.601(8) .
Se1 O2 1.662(7) .
Se1 O1 1.797(7) .
O1 Se2 1.7709(19) .
O1 Se1A 1.785(8) .
O2 Se1A 1.676(7) .
O3A Se1A 1.584(9) .
O4A Se1A 1.595(9) .
Se2 O6 1.5921(19) .
Se2 O7 1.5928(18) .
Se2 O5 1.6871(18) .
O8 C2 1.457(3) .
O8 C1 1.458(3) .
O9 C4 1.447(3) .
O9 C3 1.447(3) .
C1 C2 1.505(3) 2_565
C2 C1 1.505(3) 2_565
C3 C4 1.514(3) 2_666
C4 C3 1.514(3) 2_666
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O8 0.85(3) 1.59(3) 2.436(2) 173(3) .
O5 H5 O9 0.83(3) 1.70(3) 2.524(2) 176(3) 1_545
