#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:47 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310713.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_4310713
loop_
_publ_author_name
'Tiina Maaninen'
'Heikki M. Tuononen'
'Gabriele Schatte'
'Reijo Suontamo'
'Jussi Valkonen'
'Risto Laitinen'
'Tristram Chivers'
_publ_contact_author_address
; Department of Chemistry
  University of Calgary
  Calgary Alberta T2N 1N4
  Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Experimental and Theoretical Investigations of Structural Trends for
 Selenium(IV) Imides and Oxides: X-ray Structure of Se3(NAd)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2097
_journal_page_last               2104
_journal_paper_doi               10.1021/ic034944b
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'O2 Se'
_chemical_formula_sum            'O2 Se'
_chemical_formula_weight         110.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           135
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2ab'
_symmetry_space_group_name_H-M   'P 42/m b c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.3350(2)
_cell_length_b                   8.3350(2)
_cell_length_c                   5.06000(10)
_cell_measurement_reflns_used    1026
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     351.529(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
' HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
' Cameron (WinGX v1.64-03a), Ortep (SHELXTL-NT v5.1, Bruker)'
_computing_publication_material  'WinGX v1.64-03a (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    ' SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5584
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    20.880
_exptl_absorpt_correction_T_max  0.1027
_exptl_absorpt_correction_T_min  0.0778
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;SADABS, V 5.0, Software for Area-Detector Absorption
 Corrections; Bruker AXS Inc., Madison, WI, 1998.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.066(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0272P)²+2.2806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                269
_reflns_number_total             271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034944bsi20040123_111158_1.cif
_cod_data_source_block           3
_cod_database_code               4310713
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x, z+1/2'
'-y, x, z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z'
'x-1/2, -y-1/2, z'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x, -z-1/2'
'y, -x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.13389(5) 0.20950(5) 0.0000 0.0074(3) Uani 1 2 d S . .
O1 O -0.0585(4) 0.1736(5) 0.0000 0.0130(7) Uani 1 2 d S . .
O2 O 0.1340 0.3660 0.2500 0.0113(7) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Se1 0.0066(3) 0.0075(3) 0.0082(3) 0.000 0.000 0.00026(13)
O1 0.0062(15) 0.0166(16) 0.0163(17) 0.000 0.000 -0.0036(12)
O2 0.0128(10) 0.0128(10) 0.0083(14) -0.0024(9) -0.0024(9) 0.0024(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Se Se -0.0929 2.2259 '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'
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
_geom_angle_publ_flag
O1 Se1 O1 0.0(3) 10 . ?
O1 Se1 O2 97.60(10) 10 . ?
O1 Se1 O2 97.60(10) . . ?
O1 Se1 O2 97.60(10) 10 10 ?
O1 Se1 O2 97.60(10) . 10 ?
O2 Se1 O2 88.242(19) . 10 ?
O1 O1 Se1 0(3) 10 . ?
Se1 O2 Se1 119.04(2) . 5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 O1 1.631(3) 10 ?
Se1 O1 1.631(3) . ?
Se1 O2 1.8171(3) . ?
Se1 O2 1.8171(3) 10 ?
O1 O1 0.000(10) 10 ?
O2 Se1 1.8171(3) 5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Se1 O1 O1 0.000(13) . . . 10 ?
O2 Se1 O1 O1 0.000(13) 10 . . 10 ?
O1 Se1 O2 Se1 137.76(10) 10 . . 5 ?
O1 Se1 O2 Se1 137.76(10) . . . 5 ?
O2 Se1 O2 Se1 -124.806(18) 10 . . 5 ?
