Hydrothermal Syntheses and Characterizations of Thioarsenates [Fe(phen)~3~][As~3~S~6~]·dien·7H~2~O and [Mn~2~(phen)~4~(As~2~S~5~)]·phen·2H~2~O: A New Coordination Mode of the As~2~S~5~^4-^ Anion
Pan, Yingli; Jin, Qinyan; Chen, Jiangfang; Zhang, Yong; Jia, Dingxian; Inorganic chemistry 48 (2009) 5412–5417; doi:10.1021/ic9003615

data_4338565
_publ_section_title
;
 Hydrothermal Syntheses and Characterizations of Thioarsenates
 [Fe(phen)~3~][As~3~S~6~]&#x00B7;dien&#x00B7;7H~2~O and
 [Mn~2~(phen)~4~(As~2~S~5~)]&#x00B7;phen&#x00B7;2H~2~O:
 A New Coordination Mode of the As~2~S~5~^4-^ Anion
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5412
_journal_page_last               5417
_journal_paper_doi               10.1021/ic9003615
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C48 H32 As2 Mn2 N8 S5,(C12 H8 N2), 2(H2 O)'
_chemical_formula_sum            'C60 H44 As2 Mn2 N10 O2 S5'
_chemical_formula_weight         1357.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.173(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.959(2)
_cell_length_b                   20.696(3)
_cell_length_c                   21.970(4)
_cell_measurement_reflns_used    19035
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      3.0
_cell_volume                     5817.0(16)
_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      193(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  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53274
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.6148
_exptl_absorpt_correction_T_min  0.5562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         9661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0455P)^2^+26.7615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                7802
_reflns_number_total             9661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003615_si_001.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        5817.1(16)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4338565