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
Chunying Tang; Fang Wang; Wenqing Jiang; Yong Zhang; Dingxian Jia; Inorganic Chemistry 52 (2013) 10860–10868; doi:10.1021/ic4007982

data_4336149
_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(\m3-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         'C8 H26 N6 Ni, As6 Ni S6'
_chemical_formula_sum            'C8 H26 As6 N6 Ni2 S6'
_chemical_formula_weight         965.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   11.0037(11)
_cell_length_b                   14.7916(19)
_cell_length_c                   16.6696(17)
_cell_measurement_reflns_used    8989
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.0
_cell_volume                     2713.2(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9558
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    9.123
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0417
_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/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4417
_reflns_number_total             4777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007982_si_002_3.cif
_cod_data_source_block           compound_2
_cod_database_code               4336149