[M(dap)3]InSb3S7 (M = Co, Ni): Two Novel Open-Framework Thioindate-Thioantimonates with 8-, 12-, and 16-Ring Intersecting Channels
Jian Zhou; Litao An; Feng Zhang; Inorganic Chemistry 50 (2011) 415–417; doi:10.1021/ic101912s

data_4324247
_publ_section_title
;
 [M(dap)3]InSb3S7 (M = Co, Ni): Two Novel Open-Framework
 Thioindate-Thioantimonates with 8-, 12-, and 16-Ring Intersecting
 Channels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              415
_journal_page_last               417
_journal_paper_doi               10.1021/ic101912s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'In S7 Sb3, C9 H30 N6 Ni '
_chemical_formula_sum            'C9 H30 In N6 Ni S7 Sb3'
_chemical_formula_weight         985.67
_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                 117.05(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.668(2)
_cell_length_b                   16.207(3)
_cell_length_c                   18.247(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.14
_cell_volume                     2809.7(13)
_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      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1064
_diffrn_reflns_av_sigmaI/netI    0.2276
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15162
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.844
_exptl_absorpt_correction_T_max  0.7938
_exptl_absorpt_correction_T_min  0.6179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.0033(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   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                2426
_reflns_number_total             4975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101912s_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C9 H30 In N6 Ni S7 Sb3 '
_cod_database_code               4324247