Mixed-Valent Selenidoantimonates(III,V) with Transition-Metal Complexes as Counterions: Solvothermal Syntheses and Characterization of [M(dien)2]2Sb4Se9(M = Mn, Fe), [Co(dien)2]2Sb2Se6, and [Ni(dien)2]2Sb2Se5
Jia, Dingxian; Zhang, Yong; Zhao, Qianxin; Deng, Jie; Inorganic Chemistry 45 (2006) 9812–9817; doi:10.1021/ic061520j

data_4333147
_publ_section_title
;
 Mixed-Valent Selenidoantimonates(III,V) with Transition-Metal Complexes
 as Counterions:&#x00A0; Solvothermal Syntheses and Characterization of
 [M(dien)2]2Sb4Se9(M = Mn, Fe), [Co(dien)2]2Sb2Se6, and [Ni(dien)2]2Sb2Se5
;
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9812
_journal_page_last               9817
_journal_paper_doi               10.1021/ic061520j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '2(C8 H26 Mn N6), Sb4 Se9'
_chemical_formula_sum            'C16 H52 Mn2 N12 Sb4 Se9'
_chemical_formula_weight         1720.22
_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                   11.8398(10)
_cell_length_b                   11.8284(7)
_cell_length_c                   31.099(3)
_cell_measurement_reflns_used    17761
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     4355.3(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42888
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    10.558
_exptl_absorpt_correction_T_max  0.5152
_exptl_absorpt_correction_T_min  0.1148
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.112(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0411P)^2^+6.1187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                7513
_reflns_number_total             7962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061520jsup1.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4355.2(6)
_cod_original_sg_symbol_Hall     'p 2ac 2ab'
_cod_original_sg_symbol_H-M      'p 21 21 21'
_cod_database_code               4333147