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_4302370
_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         'C36 H24 As3 Fe N6 S6, C4 N3 H13, 7(H2 O)'
_chemical_formula_sum            'C40 H51 As3 Fe N9 O7 S6'
_chemical_formula_weight         1242.87
_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                104.361(3)
_cell_angle_beta                 106.783(4)
_cell_angle_gamma                93.384(4)
_cell_formula_units_Z            2
_cell_length_a                   11.947(2)
_cell_length_b                   13.444(3)
_cell_length_c                   16.825(3)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      3.1
_cell_volume                     2481.4(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23172
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  0.7811
_exptl_absorpt_correction_T_min  0.5628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         8241
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0679P)^2^+14.5075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1939
_reflns_number_gt                5887
_reflns_number_total             8241
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338564
_cod_data_source_file            ic9003615_si_001_2.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        2481.5(8)
_cod_database_code               4302370