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#$Date: 2016-03-23 22:02:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179464 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/61/4336147.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_4336147
loop_
_publ_author_name
'Chunying Tang'
'Fang Wang'
'Wenqing Jiang'
'Yong Zhang'
'Dingxian Jia'
_publ_contact_author_address
;Soochow University
      College of Chemistry, Chemical Engineering and Materials Science
      P.O. Box 174, Renai Road 199, Suzhou 215123
      P.R.China.
;
_publ_contact_author_email       jiadingxian@suda.edu.cn
_publ_contact_author_fax         86-512-65880089
_publ_contact_author_name        'Dr. Dingxian Jia'
_publ_contact_author_phone       86-512-65880089
_publ_section_title
;
 Clusters [Co(As3S3)2]2-, [Ni(As3S3)2]2-, and [{Co(en)}6(μ3-S)4(AsS3)4]2-
 with Co-As or Ni-As Bonds: Solvothermal Syntheses and Characterizations
 of Thioarsenates Containing Transition-Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10860
_journal_page_last               10868
_journal_paper_doi               10.1021/ic4007982
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C12 H48 As2 Co2 N12 S5'
_chemical_formula_sum            'C12 H48 As2 Co2 N12 S5'
_chemical_formula_weight         788.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4084(17)
_cell_length_b                   11.2176(13)
_cell_length_c                   17.3415(18)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.2
_cell_volume                     2997.4(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9252
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    3.673
_exptl_absorpt_correction_T_max  0.3213
_exptl_absorpt_correction_T_min  0.3213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+2.2771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                2535
_reflns_number_total             2721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007982_si_002_1.cif
_cod_data_source_block           compound_5
_cod_database_code               4336147
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'x-1/2, y, -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
As1A As 0.42907(5) 0.09843(6) 0.44356(4) 0.02062(18) Uani 0.50 1 d P
As1B As 0.48571(5) 0.08352(6) 0.41018(4) 0.02096(18) Uani 0.50 1 d P
S1 S 0.55460(11) -0.00966(16) 0.46999(9) 0.0230(4) Uani 0.50 1 d P
S2 S 0.38513(6) 0.01587(8) 0.33221(5) 0.0264(2) Uani 1 1 d .
S3 S 0.46620(9) 0.27462(9) 0.41070(6) 0.0468(3) Uani 1 1 d .
Co1 Co 0.60133(3) 0.13517(4) 0.14221(2) 0.01691(14) Uani 1 1 d .
N1 N 0.48939(19) 0.0748(3) 0.08445(16) 0.0279(7) Uani 1 1 d .
H1A H 0.4873 0.1063 0.0361 0.033 Uiso 1 1 calc R
H1B H 0.4905 -0.0060 0.0804 0.033 Uiso 1 1 calc R
N2 N 0.50944(19) 0.2458(3) 0.19877(16) 0.0288(7) Uani 1 1 d .
H2A H 0.5019 0.2210 0.2483 0.035 Uiso 1 1 calc R
H2B H 0.5287 0.3225 0.1996 0.035 Uiso 1 1 calc R
N3 N 0.70277(19) 0.2002(3) 0.21323(16) 0.0307(7) Uani 1 1 d .
H3A H 0.7553 0.1778 0.1942 0.037 Uiso 1 1 calc R
H3B H 0.7010 0.2811 0.2159 0.037 Uiso 1 1 calc R
N4 N 0.5932(2) 0.0031(3) 0.22915(17) 0.0318(7) Uani 1 1 d .
H4A H 0.5435 0.0127 0.2569 0.038 Uiso 1 1 calc R
H4B H 0.5925 -0.0707 0.2075 0.038 Uiso 1 1 calc R
N5 N 0.6296(2) 0.2623(3) 0.05657(16) 0.0319(7) Uani 1 1 d .
H5A H 0.5849 0.2673 0.0225 0.038 Uiso 1 1 calc R
H5B H 0.6374 0.3353 0.0785 0.038 Uiso 1 1 calc R
N6 N 0.6857(2) 0.0289(3) 0.07270(17) 0.0335(7) Uani 1 1 d .
H6A H 0.7368 0.0164 0.0978 0.040 Uiso 1 1 calc R
H6B H 0.6608 -0.0431 0.0630 0.040 Uiso 1 1 calc R
C1 C 0.4128(2) 0.1125(4) 0.1288(2) 0.0332(9) Uani 1 1 d .
H1C H 0.4043 0.0593 0.1730 0.040 Uiso 1 1 calc R
H1D H 0.3609 0.1087 0.0963 0.040 Uiso 1 1 calc R
C2 C 0.4268(3) 0.2384(3) 0.1564(2) 0.0340(9) Uani 1 1 d .
H2C H 0.4281 0.2928 0.1122 0.041 Uiso 1 1 calc R
H2D H 0.3789 0.2623 0.1902 0.041 Uiso 1 1 calc R
C3 C 0.6883(2) 0.1470(4) 0.29028(19) 0.0338(9) Uani 1 1 d .
H3C H 0.6391 0.1861 0.3157 0.041 Uiso 1 1 calc R
H3D H 0.7399 0.1577 0.3225 0.041 Uiso 1 1 calc R
C4 C 0.6695(2) 0.0158(4) 0.2799(2) 0.0334(9) Uani 1 1 d .
H4C H 0.7198 -0.0240 0.2567 0.040 Uiso 1 1 calc R
H4D H 0.6579 -0.0212 0.3300 0.040 Uiso 1 1 calc R
C5 C 0.7090(2) 0.2254(4) 0.0166(2) 0.0368(9) Uani 1 1 d .
H5C H 0.7598 0.2408 0.0491 0.044 Uiso 1 1 calc R
H5D H 0.7156 0.2703 -0.0315 0.044 Uiso 1 1 calc R
C6 C 0.7015(2) 0.0930(4) -0.0004(2) 0.0364(9) Uani 1 1 d .
H6C H 0.6535 0.0787 -0.0363 0.044 Uiso 1 1 calc R
H6D H 0.7552 0.0641 -0.0243 0.044 Uiso 1 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 0.0033 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'
Co Co 0.3494 0.9721 '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
S1 As1A S3 133.66(7) 5_656 .
S1 As1A S2 121.67(7) 5_656 .
S3 As1A S2 103.47(4) . .
S1 As1A S1 55.75(9) 5_656 .
S3 As1A S1 108.18(6) . .
S2 As1A S1 101.82(6) . .
S1 As1B S3 130.47(7) . .
S1 As1B S2 124.50(7) . .
S3 As1B S2 104.31(5) . .
S1 As1B S1 55.91(9) . 5_656
S3 As1B S1 108.21(6) . 5_656
S2 As1B S1 103.85(6) . 5_656
As1B S1 As1A 150.21(11) . 5_656
As1B S1 S1 75.04(10) . 5_656
As1A S1 S1 75.24(9) 5_656 5_656
As1B S1 As1B 124.09(9) . 5_656
As1A S1 As1B 26.25(4) 5_656 5_656
S1 S1 As1B 49.05(7) 5_656 5_656
As1B S1 As1A 26.09(4) . .
As1A S1 As1A 124.25(9) 5_656 .
S1 S1 As1A 49.00(8) 5_656 .
As1B S1 As1A 98.04(7) 5_656 .
As1B S2 As1A 27.61(3) . .
As1A S3 As1B 28.55(3) . .
N5 Co1 N1 92.98(12) . .
N5 Co1 N4 171.42(12) . .
N1 Co1 N4 93.74(12) . .
N5 Co1 N3 91.38(12) . .
N1 Co1 N3 172.25(11) . .
N4 Co1 N3 82.56(12) . .
N5 Co1 N2 93.91(12) . .
N1 Co1 N2 82.04(11) . .
N4 Co1 N2 92.31(12) . .
N3 Co1 N2 91.28(11) . .
N5 Co1 N6 81.60(12) . .
N1 Co1 N6 92.90(12) . .
N4 Co1 N6 92.73(12) . .
N3 Co1 N6 94.08(12) . .
N2 Co1 N6 173.08(11) . .
C1 N1 Co1 108.4(2) . .
C1 N1 H1A 110.0 . .
Co1 N1 H1A 110.0 . .
C1 N1 H1B 110.0 . .
Co1 N1 H1B 110.0 . .
H1A N1 H1B 108.4 . .
C2 N2 Co1 108.3(2) . .
C2 N2 H2A 110.0 . .
Co1 N2 H2A 110.0 . .
C2 N2 H2B 110.0 . .
Co1 N2 H2B 110.0 . .
H2A N2 H2B 108.4 . .
C3 N3 Co1 105.9(2) . .
C3 N3 H3A 110.5 . .
Co1 N3 H3A 110.5 . .
C3 N3 H3B 110.5 . .
Co1 N3 H3B 110.5 . .
H3A N3 H3B 108.7 . .
C4 N4 Co1 108.0(2) . .
C4 N4 H4A 110.1 . .
Co1 N4 H4A 110.1 . .
C4 N4 H4B 110.1 . .
Co1 N4 H4B 110.1 . .
H4A N4 H4B 108.4 . .
C5 N5 Co1 108.4(2) . .
C5 N5 H5A 110.0 . .
Co1 N5 H5A 110.0 . .
C5 N5 H5B 110.0 . .
Co1 N5 H5B 110.0 . .
H5A N5 H5B 108.4 . .
C6 N6 Co1 108.2(2) . .
C6 N6 H6A 110.0 . .
Co1 N6 H6A 110.0 . .
C6 N6 H6B 110.0 . .
Co1 N6 H6B 110.0 . .
H6A N6 H6B 108.4 . .
N1 C1 C2 108.7(3) . .
N1 C1 H1C 110.0 . .
C2 C1 H1C 110.0 . .
N1 C1 H1D 110.0 . .
C2 C1 H1D 110.0 . .
H1C C1 H1D 108.3 . .
N2 C2 C1 109.6(3) . .
N2 C2 H2C 109.8 . .
C1 C2 H2C 109.8 . .
N2 C2 H2D 109.8 . .
C1 C2 H2D 109.8 . .
H2C C2 H2D 108.2 . .
N3 C3 C4 108.3(3) . .
N3 C3 H3C 110.0 . .
C4 C3 H3C 110.0 . .
N3 C3 H3D 110.0 . .
C4 C3 H3D 110.0 . .
H3C C3 H3D 108.4 . .
N4 C4 C3 108.5(3) . .
N4 C4 H4C 110.0 . .
C3 C4 H4C 110.0 . .
N4 C4 H4D 110.0 . .
C3 C4 H4D 110.0 . .
H4C C4 H4D 108.4 . .
N5 C5 C6 107.8(3) . .
N5 C5 H5C 110.1 . .
C6 C5 H5C 110.1 . .
N5 C5 H5D 110.1 . .
C6 C5 H5D 110.1 . .
H5C C5 H5D 108.5 . .
N6 C6 C5 108.7(3) . .
N6 C6 H6C 109.9 . .
C5 C6 H6C 109.9 . .
N6 C6 H6D 109.9 . .
C5 C6 H6D 109.9 . .
H6C C6 H6D 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1A S1 1.8173(17) 5_656
As1A S3 2.1350(13) .
As1A S2 2.2460(11) .
As1A S1 2.3283(19) .
As1B S1 1.8152(18) .
As1B S3 2.1647(13) .
As1B S2 2.1922(11) .
As1B S1 2.3218(17) 5_656
S1 As1A 1.8173(17) 5_656
S1 S1 1.990(3) 5_656
S1 As1B 2.3218(17) 5_656
Co1 N5 2.105(3) .
Co1 N1 2.106(3) .
Co1 N4 2.117(3) .
Co1 N3 2.119(3) .
Co1 N2 2.123(3) .
Co1 N6 2.136(3) .
N1 C1 1.471(4) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N2 C2 1.472(5) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N3 C3 1.480(4) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N4 C4 1.476(5) .
N4 H4A 0.9100 .
N4 H4B 0.9100 .
N5 C5 1.465(5) .
N5 H5A 0.9100 .
N5 H5B 0.9100 .
N6 C6 1.478(5) .
N6 H6A 0.9100 .
N6 H6B 0.9100 .
C1 C2 1.507(5) .
C1 H1C 0.9800 .
C1 H1D 0.9800 .
C2 H2C 0.9800 .
C2 H2D 0.9800 .
C3 C4 1.510(5) .
C3 H3C 0.9800 .
C3 H3D 0.9800 .
C4 H4C 0.9800 .
C4 H4D 0.9800 .
C5 C6 1.519(6) .
C5 H5C 0.9800 .
C5 H5D 0.9800 .
C6 H6C 0.9800 .
C6 H6D 0.9800 .
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
N1 H1A S3 0.91 2.57 3.473(3) 169.8 3_554
N1 H1B S3 0.91 2.55 3.437(3) 163.8 7_656
N2 H2A S3 0.91 2.93 3.749(3) 150.2 .
N2 H2B S2 0.91 2.60 3.480(3) 161.9 7_666
N3 H3A S2 0.91 2.74 3.576(3) 153.2 8_656
N4 H4A S2 0.91 2.77 3.673(3) 172.7 .
N4 H4B S3 0.91 2.83 3.645(3) 149.4 7_656
N5 H5A S3 0.91 2.71 3.593(3) 165.2 3_554
N5 H5B S2 0.91 2.57 3.444(3) 160.3 7_666
N6 H6A S2 0.91 2.59 3.491(3) 171.2 8_656
N6 H6B S3 0.91 2.87 3.701(4) 153.1 7_656
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_4
S3 As1B S1 As1A 89.3(2) . 5_656
S2 As1B S1 As1A -79.5(2) . 5_656
S1 As1B S1 As1A 3.93(13) 5_656 5_656
S3 As1B S1 S1 85.33(12) . 5_656
S2 As1B S1 S1 -83.43(11) . 5_656
S3 As1B S1 As1B 85.33(12) . 5_656
S2 As1B S1 As1B -83.43(11) . 5_656
S1 As1B S1 As1B 0.0 5_656 5_656
S3 As1B S1 As1A 81.87(9) . .
S2 As1B S1 As1A -86.89(8) . .
S1 As1B S1 As1A -3.47(12) 5_656 .
S1 As1A S1 As1B 175.56(15) 5_656 .
S3 As1A S1 As1B -53.48(8) . .
S2 As1A S1 As1B 55.14(8) . .
S1 As1A S1 As1A 0.0 5_656 5_656
S3 As1A S1 As1A 130.96(10) . 5_656
S2 As1A S1 As1A -120.42(10) . 5_656
S3 As1A S1 S1 130.96(10) . 5_656
S2 As1A S1 S1 -120.42(10) . 5_656
S1 As1A S1 As1B -1.54(5) 5_656 5_656
S3 As1A S1 As1B 129.42(6) . 5_656
S2 As1A S1 As1B -121.96(6) . 5_656
S1 As1B S2 As1A 100.85(9) . .
S3 As1B S2 As1A -70.35(6) . .
S1 As1B S2 As1A 42.92(6) 5_656 .
S1 As1A S2 As1B -97.02(9) 5_656 .
S3 As1A S2 As1B 72.07(7) . .
S1 As1A S2 As1B -40.14(6) . .
S1 As1A S3 As1B 97.98(11) 5_656 .
S2 As1A S3 As1B -69.15(5) . .
S1 As1A S3 As1B 38.33(6) . .
S1 As1B S3 As1A -96.52(10) . .
S2 As1B S3 As1A 73.94(6) . .
S1 As1B S3 As1A -36.18(6) 5_656 .
N5 Co1 N1 C1 -110.0(2) . .
N4 Co1 N1 C1 75.3(3) . .
N3 Co1 N1 C1 14.2(10) . .
N2 Co1 N1 C1 -16.5(2) . .
N6 Co1 N1 C1 168.3(2) . .
N5 Co1 N2 C2 80.5(2) . .
N1 Co1 N2 C2 -12.0(2) . .
N4 Co1 N2 C2 -105.4(2) . .
N3 Co1 N2 C2 172.0(2) . .
N6 Co1 N2 C2 31.3(11) . .
N5 Co1 N3 C3 166.5(2) . .
N1 Co1 N3 C3 42.2(10) . .
N4 Co1 N3 C3 -19.6(2) . .
N2 Co1 N3 C3 72.5(2) . .
N6 Co1 N3 C3 -111.8(2) . .
N5 Co1 N4 C4 35.0(9) . .
N1 Co1 N4 C4 176.4(2) . .
N3 Co1 N4 C4 -10.4(2) . .
N2 Co1 N4 C4 -101.4(2) . .
N6 Co1 N4 C4 83.4(2) . .
N1 Co1 N5 C5 -111.7(2) . .
N4 Co1 N5 C5 29.8(9) . .
N3 Co1 N5 C5 74.7(2) . .
N2 Co1 N5 C5 166.1(2) . .
N6 Co1 N5 C5 -19.2(2) . .
N5 Co1 N6 C6 -10.6(2) . .
N1 Co1 N6 C6 82.0(2) . .
N4 Co1 N6 C6 175.8(2) . .
N3 Co1 N6 C6 -101.4(2) . .
N2 Co1 N6 C6 39.2(11) . .
Co1 N1 C1 C2 41.7(3) . .
Co1 N2 C2 C1 38.1(4) . .
N1 C1 C2 N2 -54.1(4) . .
Co1 N3 C3 C4 46.2(3) . .
Co1 N4 C4 C3 38.5(3) . .
N3 C3 C4 N4 -57.9(4) . .
Co1 N5 C5 C6 45.1(3) . .
Co1 N6 C6 C5 37.9(3) . .
N5 C5 C6 N6 -56.0(4) . .
