#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/00/2210057.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210057
loop_
_publ_author_name
'Feng Li'
'Handong Yin'
'Jun Zhai'
'Daqi Wang'
_publ_section_title
;
 Tris(N,N-diethylcarbamato-κ²S,S')arsenic(III)
;
_journal_coeditor_code           AT2076
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2205
_journal_page_last               m2207
_journal_paper_doi               10.1107/S1600536806031540
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[As (C5 H10 N1 S2)3]'
_chemical_formula_moiety         'C15 H30 As N3 S6'
_chemical_formula_sum            'C15 H30 As N3 S6'
_chemical_formula_weight         519.70
_chemical_name_systematic
;
Tris(N,N-diethylcarbamato-κ²S,S')arsenic(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.990(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.868(5)
_cell_length_b                   8.389(3)
_cell_length_c                   18.548(6)
_cell_measurement_reflns_used    4083
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.454
_cell_measurement_theta_min      2.615
_cell_volume                     2423.8(14)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12134
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.5960
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0397P)²+1.0408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                3141
_reflns_number_total             4257
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2076.cif
_cod_data_source_block           I
_cod_original_cell_volume        2423.9(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2210057
_cod_database_fobs_code          2210057
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
As As1 0.25896(2) 0.80445(4) 0.878817(18) 0.03740(12) Uani d . 1
N N1 0.45510(17) 0.4362(3) 0.89791(15) 0.0455(7) Uani d . 1
N N2 0.03384(17) 0.7385(3) 0.70982(14) 0.0389(7) Uani d . 1
N N3 0.25087(18) 1.0919(3) 1.06807(14) 0.0444(7) Uani d . 1
S S1 0.29442(6) 0.53203(11) 0.88517(5) 0.0472(2) Uani d . 1
S S2 0.44218(7) 0.75214(13) 0.89367(7) 0.0683(3) Uani d . 1
S S3 0.11414(5) 0.73081(11) 0.84921(5) 0.0407(2) Uani d . 1
S S4 0.19631(6) 0.83642(13) 0.72657(5) 0.0538(3) Uani d . 1
S S5 0.25468(6) 0.80706(11) 1.00515(5) 0.0447(2) Uani d . 1
S S6 0.21377(6) 1.10783(11) 0.92238(5) 0.0483(2) Uani d . 1
C C1 0.4053(2) 0.5643(4) 0.89273(18) 0.0423(8) Uani d . 1
C C2 0.5487(2) 0.4508(5) 0.9053(2) 0.0589(11) Uani d . 1
H H2A 0.5761 0.3635 0.9352 0.071 Uiso calc R 1
H H2B 0.5673 0.5494 0.9308 0.071 Uiso calc R 1
C C3 0.5776(3) 0.4496(6) 0.8328(2) 0.0773(14) Uani d . 1
H H3A 0.5539 0.3583 0.8049 0.116 Uiso calc R 1
H H3B 0.6392 0.4445 0.8411 0.116 Uiso calc R 1
H H3C 0.5584 0.5450 0.8062 0.116 Uiso calc R 1
C C4 0.4210(3) 0.2726(5) 0.8998(2) 0.0601(11) Uani d . 1
H H4A 0.4650 0.2054 0.9281 0.072 Uiso calc R 1
H H4B 0.3726 0.2744 0.9247 0.072 Uiso calc R 1
C C5 0.3936(3) 0.2026(6) 0.8271(3) 0.0891(16) Uani d . 1
H H5A 0.3467 0.2634 0.8000 0.134 Uiso calc R 1
H H5B 0.3754 0.0947 0.8320 0.134 Uiso calc R 1
H H5C 0.4406 0.2037 0.8013 0.134 Uiso calc R 1
C C6 0.1087(2) 0.7665(4) 0.75464(17) 0.0371(8) Uani d . 1
C C7 0.0218(2) 0.7745(5) 0.63068(18) 0.0552(10) Uani d . 1
H H7A 0.0609 0.8591 0.6231 0.066 Uiso calc R 1
H H7B -0.0363 0.8123 0.6135 0.066 Uiso calc R 1
C C8 0.0377(3) 0.6305(6) 0.5860(2) 0.0725(13) Uani d . 1
H H8A 0.0934 0.5873 0.6054 0.109 Uiso calc R 1
H H8B 0.0350 0.6615 0.5358 0.109 Uiso calc R 1
H H8C -0.0053 0.5512 0.5884 0.109 Uiso calc R 1
C C9 -0.0411(2) 0.6705(4) 0.73433(19) 0.0425(9) Uani d . 1
H H9A -0.0219 0.6126 0.7798 0.051 Uiso calc R 1
H H9B -0.0689 0.5951 0.6978 0.051 Uiso calc R 1
C C10 -0.1058(3) 0.7959(5) 0.7466(2) 0.0590(11) Uani d . 1
H H10A -0.0799 0.8663 0.7854 0.089 Uiso calc R 1
H H10B -0.1548 0.7448 0.7600 0.089 Uiso calc R 1
H H10C -0.1237 0.8560 0.7023 0.089 Uiso calc R 1
C C11 0.24018(19) 1.0152(4) 1.00431(18) 0.0382(8) Uani d . 1
C C12 0.2768(2) 1.0100(5) 1.13914(19) 0.0536(10) Uani d . 1
H H12A 0.2554 0.9015 1.1346 0.064 Uiso calc R 1
H H12B 0.2508 1.0636 1.1758 0.064 Uiso calc R 1
C C13 0.3729(3) 1.0067(6) 1.1649(2) 0.0739(13) Uani d . 1
H H13A 0.3989 0.9507 1.1296 0.111 Uiso calc R 1
H H13B 0.3865 0.9535 1.2114 0.111 Uiso calc R 1
H H13C 0.3944 1.1139 1.1699 0.111 Uiso calc R 1
C C14 0.2447(3) 1.2667(5) 1.0699(2) 0.0686(13) Uani d . 1
H H14A 0.2694 1.3107 1.0303 0.082 Uiso calc R 1
H H14B 0.2784 1.3050 1.1158 0.082 Uiso calc R 1
C C15 0.1545(3) 1.3265(6) 1.0628(3) 0.0915(17) Uani d . 1
H H15A 0.1225 1.3006 1.0149 0.137 Uiso calc R 1
H H15B 0.1552 1.4401 1.0693 0.137 Uiso calc R 1
H H15C 0.1280 1.2773 1.0996 0.137 Uiso calc R 1
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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_publ_flag
S3 As1 S1 88.29(4) y
S3 As1 S5 91.29(3) y
S1 As1 S5 90.64(3) y
S3 As1 S6 90.78(3) y
S1 As1 S6 159.97(4) y
S5 As1 S6 69.37(3) y
S3 As1 S4 69.37(3) y
S1 As1 S4 100.24(3) y
S5 As1 S4 157.28(4) y
S6 As1 S4 98.13(3) y
S3 As1 S2 154.60(4) y
S1 As1 S2 67.81(3) y
S5 As1 S2 97.20(4) y
S6 As1 S2 114.62(3) y
S4 As1 S2 105.36(4) y
C1 N1 C2 121.1(3) ?
C1 N1 C4 122.6(3) ?
C2 N1 C4 116.3(3) ?
C6 N2 C9 123.6(3) ?
C6 N2 C7 121.0(3) ?
C9 N2 C7 115.4(3) ?
C11 N3 C14 120.4(3) ?
C11 N3 C12 122.5(3) ?
C14 N3 C12 116.9(3) ?
C1 S1 As1 94.63(12) ?
C1 S2 As1 78.48(12) ?
C6 S3 As1 92.77(11) ?
C6 S4 As1 79.12(11) ?
C11 S5 As1 91.65(11) ?
C11 S6 As1 78.95(12) ?
N1 C1 S2 123.9(3) ?
N1 C1 S1 117.0(3) ?
S2 C1 S1 119.1(2) ?
N1 C2 C3 113.1(3) ?
N1 C2 H2A 109.0 ?
C3 C2 H2A 109.0 ?
N1 C2 H2B 109.0 ?
C3 C2 H2B 109.0 ?
H2A C2 H2B 107.8 ?
C2 C3 H3A 109.5 ?
C2 C3 H3B 109.5 ?
H3A C3 H3B 109.5 ?
C2 C3 H3C 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
C5 C4 N1 113.5(4) ?
C5 C4 H4A 108.9 ?
N1 C4 H4A 108.9 ?
C5 C4 H4B 108.9 ?
N1 C4 H4B 108.9 ?
H4A C4 H4B 107.7 ?
C4 C5 H5A 109.5 ?
C4 C5 H5B 109.5 ?
H5A C5 H5B 109.5 ?
C4 C5 H5C 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
N2 C6 S4 124.0(3) ?
N2 C6 S3 117.3(3) ?
S4 C6 S3 118.70(18) ?
N2 C7 C8 112.2(3) ?
N2 C7 H7A 109.2 ?
C8 C7 H7A 109.2 ?
N2 C7 H7B 109.2 ?
C8 C7 H7B 109.2 ?
H7A C7 H7B 107.9 ?
C7 C8 H8A 109.5 ?
C7 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
C7 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
N2 C9 C10 112.9(3) ?
N2 C9 H9A 109.0 ?
C10 C9 H9A 109.0 ?
N2 C9 H9B 109.0 ?
C10 C9 H9B 109.0 ?
H9A C9 H9B 107.8 ?
C9 C10 H10A 109.5 ?
C9 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C9 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
N3 C11 S6 123.2(3) ?
N3 C11 S5 118.5(2) ?
S6 C11 S5 118.32(19) ?
N3 C12 C13 112.6(3) ?
N3 C12 H12A 109.1 ?
C13 C12 H12A 109.1 ?
N3 C12 H12B 109.1 ?
C13 C12 H12B 109.1 ?
H12A C12 H12B 107.8 ?
C12 C13 H13A 109.5 ?
C12 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
C12 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
N3 C14 C15 113.5(4) ?
N3 C14 H14A 108.9 ?
C15 C14 H14A 108.9 ?
N3 C14 H14B 108.9 ?
C15 C14 H14B 108.9 ?
H14A C14 H14B 107.7 ?
C14 C15 H15A 109.5 ?
C14 C15 H15B 109.5 ?
H15A C15 H15B 109.5 ?
C14 C15 H15C 109.5 ?
H15A C15 H15C 109.5 ?
H15B C15 H15C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
As1 S3 2.3417(12) y
As1 S1 2.3513(12) y
As1 S5 2.3573(12) y
As1 S6 2.8047(13) y
As1 S4 2.8221(13) y
As1 S2 2.9009(15) y
N1 C1 1.326(4) ?
N1 C2 1.470(4) ?
N1 C4 1.478(5) ?
N2 C6 1.334(4) ?
N2 C9 1.466(4) ?
N2 C7 1.475(4) ?
N3 C11 1.328(4) ?
N3 C14 1.471(5) ?
N3 C12 1.474(4) ?
S1 C1 1.759(3) y
S2 C1 1.680(4) y
S3 C6 1.765(3) y
S4 C6 1.681(4) y
S5 C11 1.761(3) y
S6 C11 1.687(3) y
C2 C3 1.501(5) ?
C2 H2A 0.9700 ?
C2 H2B 0.9700 ?
C3 H3A 0.9600 ?
C3 H3B 0.9600 ?
C3 H3C 0.9600 ?
C4 C5 1.459(6) ?
C4 H4A 0.9700 ?
C4 H4B 0.9700 ?
C5 H5A 0.9600 ?
C5 H5B 0.9600 ?
C5 H5C 0.9600 ?
C7 C8 1.513(5) ?
C7 H7A 0.9700 ?
C7 H7B 0.9700 ?
C8 H8A 0.9600 ?
C8 H8B 0.9600 ?
C8 H8C 0.9600 ?
C9 C10 1.518(5) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 H10A 0.9600 ?
C10 H10B 0.9600 ?
C10 H10C 0.9600 ?
C12 C13 1.508(5) ?
C12 H12A 0.9700 ?
C12 H12B 0.9700 ?
C13 H13A 0.9600 ?
C13 H13B 0.9600 ?
C13 H13C 0.9600 ?
C14 C15 1.499(6) ?
C14 H14A 0.9700 ?
C14 H14B 0.9700 ?
C15 H15A 0.9600 ?
C15 H15B 0.9600 ?
C15 H15C 0.9600 ?
