Solvothermal Synthesis and Characterization of Polyselenidoarsenate Salts of Transition Metal Complex Cations
Dingxian Jia; Jing Zhao; Yingli Pan; Weiwei Tang; Bing Wu; Yong Zhang; Inorganic Chemistry 50 (2011) 7195–7201; doi:10.1021/ic2007809

data_4325810
_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
;
 Solvothermal Synthesis and Characterization of Polyselenidoarsenate Salts
 of Transition Metal Complex Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7195
_journal_page_last               7201
_journal_paper_doi               10.1021/ic2007809
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '2(C48 H32 As Mn2 N8 Se4), As2 Se6, H2 O'
_chemical_formula_sum            'C96 H66 As4 Mn4 N16 O Se14'
_chemical_formula_weight         3084.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.302(12)
_cell_angle_beta                 89.540(11)
_cell_angle_gamma                74.714(9)
_cell_formula_units_Z            1
_cell_length_a                   11.394(4)
_cell_length_b                   12.975(4)
_cell_length_c                   17.797(6)
_cell_measurement_reflns_used    7858
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.0
_cell_volume                     2499.9(14)
_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 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17674
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    6.961
_exptl_absorpt_correction_T_max  0.6802
_exptl_absorpt_correction_T_min  0.2461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_description       block
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9093
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0425
_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/[\s^2^(Fo^2^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                6035
_reflns_number_total             9093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2007809_si_002_4.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        2499.7(13)
_cod_database_code               4325810