Using a Ni2+ complex as a structure-directing molecule: solvothermal synthesis and properties of [Ni(en)(tren)]4Sb14S25 featuring an unprecedented three-dimensional network architecture
Seidlhofer, Beatrix; Näther, Christian; Bensch, Wolfgang; CrystEngComm 14 (2012) 5441–; doi:10.1039/c2ce25141h

data_7208197
_publ_section_title
;
 Using a Ni2+ complex as a structure-directing molecule: solvothermal
 synthesis and properties of [Ni(en)(tren)]4Sb14S25 featuring an
 unprecedented three-dimensional network architecture
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5441
_journal_paper_doi               10.1039/c2ce25141h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'S25 Sb14, 4(C8 H26 N6 Ni)'
_chemical_formula_sum            'C32 H104 N24 Ni4 S25 Sb14'
_chemical_formula_weight         3566.23
_chemical_name_common            '[Ni(en)(tren)]4Sb14S25'
_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                 98.8810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5428(3)
_cell_length_b                   25.8974(4)
_cell_length_c                   22.5225(4)
_cell_measurement_reflns_used    15953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      1.25
_cell_volume                     9533.3(3)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63078
_diffrn_reflns_theta_full        24.63
_diffrn_reflns_theta_max         24.63
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.252
_exptl_absorpt_correction_T_max  0.5230
_exptl_absorpt_correction_T_min  0.4033
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedrons
_exptl_crystal_F_000             6760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         15953
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+18.6590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                13509
_reflns_number_total             15953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25141h.txt
_cod_data_source_block           chris
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7208197