[TM(en)3][SnSb4S9] (TM = Ni, Co): 3D Chiral Framework of Mixed Main-Group Metals and [Mn(dien)2]2Sb4S9: 1D Chains with Mixed-Valent Sb Centers
Yue, Cheng-Yang; Lei, Xiao-Wu; Ma, Yun-Xiang; Sheng, Ning; Yang, Ya-Dong; Liu, Guo-Dong; Zhai, Xiu-Rong; Crystal Growth & Design 14 (2014) 101–; doi:10.1021/cg401208p

data_4509990
_publ_section_title
;
 [TM(en)3][SnSb4S9] (TM = Ni, Co): 3D Chiral Framework of Mixed Main-Group
 Metals and [Mn(dien)2]2Sb4S9: 1D Chains with Mixed-Valent Sb Centers
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              101
_journal_paper_doi               10.1021/cg401208p
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C6 H24 N6 Ni S9 Sb4 Sn'
_chemical_formula_weight         1133.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.4328(8)
_cell_length_b                   14.4328(8)
_cell_length_c                   11.3654(13)
_cell_measurement_temperature    296(2)
_cell_volume                     2050.3(3)
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       omega-scan
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23936
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    6.167
_exptl_absorpt_correction_T_max  0.5775
_exptl_absorpt_correction_T_min  0.4581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.389
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       ,
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0156P)^2^+2.2126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                2939
_reflns_number_total             3149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401208p_si_002.cif
_cod_data_source_block           C6N6H24NiSnSb4S9
_cod_original_sg_symbol_H-M      P3221
_cod_database_code               4509990