[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_4509992
_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            'C16 H52 Mn2 N12 S9 Sb4'
_chemical_formula_weight         1298.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 95.5660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6991(7)
_cell_length_b                   11.1853(7)
_cell_length_c                   32.2459(19)
_cell_measurement_temperature    296(2)
_cell_volume                     4199.7(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            48110
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_T_max  0.8407
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         9665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+11.3935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                7025
_reflns_number_total             9665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401208p_si_002.cif
_cod_data_source_block           C16N12H52Mn2Sb4S9
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4509992