Novel Polyselenidoarsenate and Selenidoarsenate: Solvothermal Synthesis and Characterization of [Co(phen)3][As2Se2(μ-Se3)(μ-Se5)] and [Co(phen)3]2[As8Se14]
Jing Zhao; Jingjing Liang; Jiangfang Chen; Yingli Pan; Yong Zhang; Dingxian Jia; Inorganic Chemistry 50 (2011) 2288–2293; doi:10.1021/ic1024444

data_4324699
_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        'Prof. Dingxian Jia'
_publ_contact_author_phone       86-512-65880089
_publ_section_title
;
 Novel Polyselenidoarsenate and Selenidoarsenate: Solvothermal Synthesis
 and Characterization of [Co(phen)3][As2Se2(\m-Se3)(\m-Se5)] and
 [Co(phen)3]2[As8Se14]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2288
_journal_page_last               2293
_journal_paper_doi               10.1021/ic1024444
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C36 H24 As2 Co N6 Se10'
_chemical_formula_sum            'C36 H24 As2 Co N6 Se10'
_chemical_formula_weight         1538.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 127.736(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.461(6)
_cell_length_b                   11.2937(19)
_cell_length_c                   19.454(5)
_cell_measurement_reflns_used    8353
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.1
_cell_volume                     4250.2(17)
_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      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20984
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    10.550
_exptl_absorpt_correction_T_max  0.4185
_exptl_absorpt_correction_T_min  0.1155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_description       block
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.981
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7627
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0482
_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^)+(0.1385P)^2^+28.2403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                6053
_reflns_number_total             7627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1024444_si_002_1.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        4250.1(16)
_cod_original_sg_symbol_H-M      'C 2 '
_cod_database_code               4324699