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#$Date: 2016-03-23 15:29:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179330 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/27/4322776.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_4322776
loop_
_publ_author_name
'Donna M. Smith'
'Michael A. Pell'
'James A. Ibers'
_publ_section_title
;
 Se22-, Se52-, and Se72- Ligands in [NEt4]2[As2Se6],
 [enH][AsSe6].2.2.2-cryptand, [NEt4][AsSe8], and [(en)2In(SeAs(Se)Se2)].en
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2340
_journal_page_last               2343
_journal_paper_doi               10.1021/ic971181h
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C8 H20 As N Se3'
_chemical_formula_weight         442.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.46(3)
_cell_angle_beta                 96.61(4)
_cell_angle_gamma                114.67(5)
_cell_formula_units_Z            2
_cell_length_a                   7.465(5)
_cell_length_b                   8.418(4)
_cell_length_c                   12.873(4)
_cell_measurement_temperature    113(2)
_cell_volume                     709.7(7)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_monochromator  'beta filtered'
_diffrn_radiation_source         ' normal focus sealed tube'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2811
_diffrn_reflns_theta_max         64.82
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    11.750
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.178
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             420
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.665
_refine_diff_density_rms         0.259
_refine_ls_extinction_coef       0.0043(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   2.518
_refine_ls_goodness_of_fit_obs   2.582
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.518
_refine_ls_restrained_S_obs      2.582
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_obs          0.0581
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0400P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1428
_refine_ls_wR_factor_obs         0.1421
_reflns_number_observed          1935
_reflns_number_total             2050
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971181h_1.cif
_cod_data_source_block           C8H20AsNSe3
_cod_original_cell_volume        709.7(6)
_cod_database_code               4322776
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N -0.2231(8) 0.6328(7) 0.2989(4) 0.0214(11) Uani 1 d . .
As1 As 0.10441(11) 0.23391(10) 0.12986(5) 0.0239(3) Uani 1 d . .
Se1 Se -0.25017(10) 0.04824(10) 0.05616(5) 0.0257(3) Uani 1 d . .
Se2 Se 0.22862(11) 0.01061(9) 0.12581(5) 0.0251(3) Uani 1 d . .
Se3 Se 0.09481(11) 0.27141(10) 0.30929(5) 0.0274(3) Uani 1 d . .
C1 C -0.3158(11) 0.4763(9) 0.1997(5) 0.0294(15) Uani 1 d . .
H1A H -0.2753 0.3824 0.2133 0.035 Uiso 1 calc R .
H1B H -0.4642 0.4239 0.1901 0.035 Uiso 1 calc R .
C2 C 0.0015(10) 0.6967(9) 0.3226(5) 0.0266(14) Uani 1 d . .
H2A H 0.0544 0.7364 0.2595 0.032 Uiso 1 calc R .
H2B H 0.0281 0.5933 0.3310 0.032 Uiso 1 calc R .
C3 C -0.3199(10) 0.5649(9) 0.3920(5) 0.0262(14) Uani 1 d . .
H3A H -0.2600 0.6651 0.4571 0.031 Uiso 1 calc R .
H3B H -0.4654 0.5321 0.3738 0.031 Uiso 1 calc R .
C4 C -0.2646(10) 0.7881(8) 0.2802(5) 0.0274(14) Uani 1 d . .
H4A H -0.1870 0.8419 0.2273 0.033 Uiso 1 calc R .
H4B H -0.2142 0.8811 0.3486 0.033 Uiso 1 calc R .
C5 C -0.2584(13) 0.5235(11) 0.0956(5) 0.0379(18) Uani 1 d . .
H5A H -0.3242 0.4150 0.0368 0.057 Uiso 1 calc R .
H5B H -0.1120 0.5727 0.1031 0.057 Uiso 1 calc R .
H5C H -0.3021 0.6132 0.0795 0.057 Uiso 1 calc R .
C6 C 0.1182(11) 0.8487(9) 0.4217(6) 0.0336(16) Uani 1 d . .
H6A H 0.2620 0.8800 0.4302 0.050 Uiso 1 calc R .
H6B H 0.0706 0.8105 0.4854 0.050 Uiso 1 calc R .
H6C H 0.0976 0.9540 0.4136 0.050 Uiso 1 calc R .
C7 C -0.2974(11) 0.4077(9) 0.4186(5) 0.0309(16) Uani 1 d . .
H7A H -0.3647 0.3737 0.4780 0.046 Uiso 1 calc R .
H7B H -0.1541 0.4396 0.4398 0.046 Uiso 1 calc R .
H7C H -0.3587 0.3063 0.3553 0.046 Uiso 1 calc R .
C8 C -0.4848(11) 0.7398(11) 0.2401(6) 0.0357(17) Uani 1 d . .
H8A H -0.4970 0.8477 0.2292 0.054 Uiso 1 calc R .
H8B H -0.5628 0.6916 0.2934 0.054 Uiso 1 calc R .
H8C H -0.5365 0.6491 0.1718 0.054 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 '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
C2 N1 C4 108.5(5) . . ?
C2 N1 C1 108.6(5) . . ?
C4 N1 C1 111.3(5) . . ?
C2 N1 C3 112.2(5) . . ?
C4 N1 C3 108.8(4) . . ?
C1 N1 C3 107.6(5) . . ?
Se3 As1 Se2 95.07(4) . . ?
Se3 As1 Se1 98.88(6) . . ?
Se2 As1 Se1 101.48(6) . . ?
Se2 Se1 As1 97.62(6) 2 . ?
Se1 Se2 As1 100.59(4) 2 . ?
C5 C1 N1 115.4(5) . . ?
N1 C2 C6 115.8(5) . . ?
C7 C3 N1 115.5(5) . . ?
N1 C4 C8 115.2(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
N1 C2 1.506(8) . ?
N1 C4 1.512(7) . ?
N1 C1 1.526(8) . ?
N1 C3 1.539(7) . ?
As1 Se3 2.2929(11) . ?
As1 Se2 2.4145(15) . ?
As1 Se1 2.415(2) . ?
Se1 Se2 2.3517(11) 2 ?
Se2 Se1 2.3517(11) 2 ?
C1 C5 1.518(9) . ?
C2 C6 1.517(9) . ?
C3 C7 1.489(8) . ?
C4 C8 1.520(9) . ?
