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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/4/33/61/4336150.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_4336150
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 As4 Co6 N12 S16, 2(C2 H9 N2)'
_chemical_formula_sum            'C16 H66 As4 Co6 N16 S16'
_chemical_formula_weight         1649.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   13.065(2)
_cell_length_b                   13.065(2)
_cell_length_c                   32.007(5)
_cell_measurement_reflns_used    5920
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.1
_cell_volume                     5463.4(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            8544
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    4.832
_exptl_absorpt_correction_T_max  0.4767
_exptl_absorpt_correction_T_min  0.1962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2500
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0451
_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)+(0.0745P)²+65.6282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                2108
_reflns_number_total             2500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007982_si_002_4.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        5463.2(13)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4336150
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
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
As1 As 0.62868(7) 0.47904(7) 0.82874(3) 0.0427(3) Uani 1 1 d .
S1 S 0.47668(17) 0.42275(16) 0.80373(6) 0.0391(5) Uani 1 1 d .
S2 S 0.7400(2) 0.4668(2) 0.77862(7) 0.0577(7) Uani 1 1 d .
S3 S 0.6033(2) 0.63749(19) 0.84343(8) 0.0634(7) Uani 1 1 d .
S4 S 0.36451(17) 0.25227(16) 0.84188(6) 0.0382(5) Uani 1 1 d .
Co1 Co 0.37577(9) 0.41147(9) 0.86340(3) 0.0383(3) Uani 1 1 d .
Co2 Co 0.5000 0.2500 0.79844(4) 0.0344(4) Uani 1 2 d S
N1 N 0.2502(6) 0.4504(6) 0.8291(2) 0.054(2) Uani 1 1 d D
N2 N 0.3762(6) 0.5623(6) 0.8781(2) 0.0512(19) Uani 1 1 d D
N3 N 0.3974(6) 0.2390(5) 0.75053(19) 0.0486(16) Uani 1 1 d .
H3A H 0.3520 0.1878 0.7558 0.050 Uiso 1 1 calc R
H3B H 0.3619 0.2986 0.7480 0.050 Uiso 1 1 calc R
C1A C 0.259(2) 0.5643(13) 0.8268(11) 0.061(6) Uani 0.50 1 d PD
C1B C 0.215(2) 0.5583(14) 0.8298(13) 0.062(6) Uani 0.50 1 d PD
C2A C 0.280(3) 0.619(3) 0.8675(10) 0.058(6) Uani 0.50 1 d PD
C2B C 0.295(3) 0.614(3) 0.8544(11) 0.063(6) Uani 0.50 1 d PD
C3 C 0.4534(8) 0.2173(8) 0.7112(2) 0.064(2) Uani 1 1 d .
H3C H 0.4103 0.2334 0.6870 0.064 Uiso 1 1 calc R
H3D H 0.4725 0.1448 0.7098 0.064 Uiso 1 1 calc R
N4 N 0.0000 0.7500 0.7429(12) 0.094(10) Uiso 1 2 d SD
C4 C 0.038(3) 0.842(3) 0.7643(17) 0.094(10) Uiso 0.50 1 d PD
C5 C 0.104(4) 0.808(5) 0.7999(12) 0.094(10) Uiso 0.50 1 d PD
N5 N 0.183(3) 0.786(4) 0.7678(15) 0.094(10) Uiso 0.50 1 d PD
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
C C 0.0033 0.0016 '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'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
S3 As1 S2 109.63(11) . .
S3 As1 S1 104.78(11) . .
S2 As1 S1 107.59(9) . .
S3 As1 Co1 114.74(9) . 10_667
S2 As1 Co1 114.75(9) . 10_667
S1 As1 Co1 104.48(7) . 10_667
As1 S1 Co2 103.31(9) . .
As1 S1 Co1 103.14(8) . .
Co2 S1 Co1 94.24(8) . .
Co1 S4 Co1 120.98(9) . 16_657
Co1 S4 Co2 98.84(9) . .
Co1 S4 Co2 120.68(10) 16_657 .
N2 Co1 N1 83.4(3) . .
N2 Co1 S4 173.9(2) . .
N1 Co1 S4 90.8(2) . .
N2 Co1 S4 89.8(2) . 10_667
N1 Co1 S4 171.0(2) . 10_667
S4 Co1 S4 96.19(12) . 10_667
N2 Co1 S1 97.3(2) . .
N1 Co1 S1 89.9(2) . .
S4 Co1 S1 80.81(8) . .
S4 Co1 S1 96.75(9) 10_667 .
N2 Co1 As1 89.8(2) . 16_657
N1 Co1 As1 90.0(2) . 16_657
S4 Co1 As1 92.04(7) . 16_657
S4 Co1 As1 84.10(6) 10_667 16_657
S1 Co1 As1 172.86(8) . 16_657
N3 Co2 N3 82.6(4) . 7_554
N3 Co2 S4 168.3(2) . 7_554
N3 Co2 S4 87.1(2) 7_554 7_554
N3 Co2 S4 87.1(2) . .
N3 Co2 S4 168.3(2) 7_554 .
S4 Co2 S4 103.71(12) 7_554 .
N3 Co2 S1 92.2(2) . .
N3 Co2 S1 94.2(2) 7_554 .
S4 Co2 S1 94.14(8) 7_554 .
S4 Co2 S1 80.58(8) . .
N3 Co2 S1 94.2(2) . 7_554
N3 Co2 S1 92.2(2) 7_554 7_554
S4 Co2 S1 80.58(8) 7_554 7_554
S4 Co2 S1 94.14(8) . 7_554
S1 Co2 S1 171.50(12) . 7_554
C1B N1 C1A 22.8(17) . .
C1B N1 Co1 118.8(11) . .
C1A N1 Co1 102.6(11) . .
C2B N2 C2A 18(2) . .
C2B N2 Co1 108.9(14) . .
C2A N2 Co1 115.2(16) . .
C3 N3 Co2 109.1(6) . .
C3 N3 H3A 109.9 . .
Co2 N3 H3A 109.9 . .
C3 N3 H3B 109.9 . .
Co2 N3 H3B 109.9 . .
H3A N3 H3B 108.3 . .
N1 C1A C2A 116(3) . .
N1 C1B C2B 104.4(19) . .
N2 C2A C1A 97.0(17) . .
N2 C2B C1B 124(3) . .
N3 C3 C3 107.1(6) . 7_554
N3 C3 H3C 110.3 . .
C3 C3 H3C 110.3 7_554 .
N3 C3 H3D 110.3 . .
C3 C3 H3D 110.3 7_554 .
H3C C3 H3D 108.5 . .
C4 N4 C4 124(6) 7_464 .
N4 C4 C5 108(4) . .
N5 C5 C4 85.9(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 S3 2.149(3) .
As1 S2 2.171(3) .
As1 S1 2.264(2) .
As1 Co1 2.3425(14) 10_667
S1 Co2 2.284(2) .
S1 Co1 2.326(2) .
S4 Co1 2.196(2) .
S4 Co1 2.213(2) 16_657
S4 Co2 2.251(2) .
Co1 N2 2.025(8) .
Co1 N1 2.037(7) .
Co1 S4 2.213(2) 10_667
Co1 As1 2.3425(14) 16_657
Co2 N3 2.042(7) .
Co2 N3 2.042(7) 7_554
Co2 S4 2.251(2) 7_554
Co2 S1 2.284(2) 7_554
N1 C1B 1.486(17) .
N1 C1A 1.494(17) .
N2 C2B 1.471(17) .
N2 C2A 1.492(18) .
N3 C3 1.485(11) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
C1A C2A 1.512(19) .
C1B C2B 1.497(19) .
C3 C3 1.487(19) 7_554
C3 H3C 0.9800 .
C3 H3D 0.9800 .
N4 C4 1.47(2) 7_464
N4 C4 1.47(2) .
C4 C5 1.49(2) .
C5 N5 1.48(2) .
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
N3 H3A S2 0.91 2.46 3.355(7) 167.7 7_554
N3 H3B S2 0.91 2.85 3.737(8) 166.6 11_557
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 As1 S1 Co2 -171.37(10) . .
S2 As1 S1 Co2 72.01(11) . .
Co1 As1 S1 Co2 -50.36(9) 10_667 .
S3 As1 S1 Co1 -73.71(11) . .
S2 As1 S1 Co1 169.67(10) . .
Co1 As1 S1 Co1 47.29(9) 10_667 .
Co1 S4 Co1 N2 -135(2) 16_657 .
Co2 S4 Co1 N2 91(2) . .
Co1 S4 Co1 N1 -118.1(3) 16_657 .
Co2 S4 Co1 N1 107.8(2) . .
Co1 S4 Co1 S4 56.21(12) 16_657 10_667
Co2 S4 Co1 S4 -77.87(8) . 10_667
Co1 S4 Co1 S1 152.08(13) 16_657 .
Co2 S4 Co1 S1 18.00(8) . .
Co1 S4 Co1 As1 -28.07(12) 16_657 16_657
Co2 S4 Co1 As1 -162.16(7) . 16_657
As1 S1 Co1 N2 63.6(2) . .
Co2 S1 Co1 N2 168.3(2) . .
As1 S1 Co1 N1 146.9(2) . .
Co2 S1 Co1 N1 -108.4(2) . .
As1 S1 Co1 S4 -122.30(10) . .
Co2 S1 Co1 S4 -17.57(8) . .
As1 S1 Co1 S4 -27.09(10) . 10_667
Co2 S1 Co1 S4 77.64(9) . 10_667
As1 S1 Co1 As1 -123.5(6) . 16_657
Co2 S1 Co1 As1 -18.8(6) . 16_657
Co1 S4 Co2 N3 -111.0(2) . .
Co1 S4 Co2 N3 114.7(2) 16_657 .
Co1 S4 Co2 N3 -82.7(10) . 7_554
Co1 S4 Co2 N3 143.1(10) 16_657 7_554
Co1 S4 Co2 S4 73.64(7) . 7_554
Co1 S4 Co2 S4 -60.63(9) 16_657 7_554
Co1 S4 Co2 S1 -18.35(8) . .
Co1 S4 Co2 S1 -152.62(12) 16_657 .
Co1 S4 Co2 S1 154.94(9) . 7_554
Co1 S4 Co2 S1 20.67(12) 16_657 7_554
As1 S1 Co2 N3 -151.6(2) . .
Co1 S1 Co2 N3 103.8(2) . .
As1 S1 Co2 N3 -68.9(2) . 7_554
Co1 S1 Co2 N3 -173.4(2) . 7_554
As1 S1 Co2 S4 18.49(9) . 7_554
Co1 S1 Co2 S4 -86.10(9) . 7_554
As1 S1 Co2 S4 121.72(9) . .
Co1 S1 Co2 S4 17.13(8) . .
As1 S1 Co2 S1 69.71(6) . 7_554
Co1 S1 Co2 S1 -34.88(6) . 7_554
N2 Co1 N1 C1B -1.2(19) . .
S4 Co1 N1 C1B -179.4(19) . .
S4 Co1 N1 C1B 40(3) 10_667 .
S1 Co1 N1 C1B -98.6(19) . .
As1 Co1 N1 C1B 88.5(19) 16_657 .
N2 Co1 N1 C1A 15.9(15) . .
S4 Co1 N1 C1A -162.3(15) . .
S4 Co1 N1 C1A 57(2) 10_667 .
S1 Co1 N1 C1A -81.5(15) . .
As1 Co1 N1 C1A 105.7(15) 16_657 .
N1 Co1 N2 C2B -4(2) . .
S4 Co1 N2 C2B 13(3) . .
S4 Co1 N2 C2B -178(2) 10_667 .
S1 Co1 N2 C2B 85(2) . .
As1 Co1 N2 C2B -94(2) 16_657 .
N1 Co1 N2 C2A 14.1(18) . .
S4 Co1 N2 C2A 31(3) . .
S4 Co1 N2 C2A -160.1(18) 10_667 .
S1 Co1 N2 C2A 103.1(18) . .
As1 Co1 N2 C2A -76.0(18) 16_657 .
N3 Co2 N3 C3 14.9(4) 7_554 .
S4 Co2 N3 C3 -13.8(14) 7_554 .
S4 Co2 N3 C3 -170.7(6) . .
S1 Co2 N3 C3 108.8(6) . .
S1 Co2 N3 C3 -76.8(6) 7_554 .
C1B N1 C1A C2A 91(8) . .
Co1 N1 C1A C2A -47(3) . .
C1A N1 C1B C2B -42(5) . .
Co1 N1 C1B C2B 6(4) . .
C2B N2 C2A C1A 35(8) . .
Co1 N2 C2A C1A -38(3) . .
N1 C1A C2A N2 56(4) . .
C2A N2 C2B C1B -104(13) . .
Co1 N2 C2B C1B 10(5) . .
N1 C1B C2B N2 -10(5) . .
Co2 N3 C3 C3 -41.7(11) . 7_554
C4 N4 C4 C5 43(3) 7_464 .
N4 C4 C5 N5 76(5) . .
