Gallium-Sulfide Supertetrahedral Clusters as Building Blocks of Covalent Organic-Inorganic Networks
Paz Vaqueiro; M. Lucia Romero; Journal of the American Chemical Society 130 (2008) 9630–9631; doi:10.1021/ja801619e

data_4108102
_publ_contact_author_address
; 
 Department of Chemistry, 
 Heriot-Watt University,  
 Edinburgh, EH14 4AS, UK. 
;
_publ_contact_author_email       chepv@hw.ac.uk
_publ_contact_author_fax         '+44 1314512180'
_publ_contact_author_name        'Paz Vaqueiro'
_publ_contact_author_phone       '+44 1314513759'
_publ_section_title
;
 Gallium-Sulfide Supertetrahedral Clusters as Building Blocks of Covalent
 Organic-Inorganic Networks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9630
_journal_page_last               9631
_journal_paper_doi               10.1021/ja801619e
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C25 H24 Ga10 N4 S16'
_chemical_formula_sum            'C25 H24 Ga10 N4 S16'
_chemical_formula_weight         1590.75
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-02-01
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                81.599(6)
_cell_angle_beta                 88.542(5)
_cell_angle_gamma                82.967(5)
_cell_formula_units_Z            2
_cell_length_a                   12.4678(12)
_cell_length_b                   13.6806(13)
_cell_length_c                   20.385(2)
_cell_measurement_reflns_used    20798
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.673
_cell_measurement_theta_min      1.516
_cell_volume                     3413.7(6)
_computing_cell_refinement       'APEX 2 (Bruker, 2005)'
_computing_data_collection       'APEX 2 (Bruker, 2005)'
_computing_data_reduction        'APEX 2 (Bruker, 2005)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type
;
Bruker-Nonius APEX-2 CCD area-detector diffractometer
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89986
_diffrn_reflns_theta_full        29.773
_diffrn_reflns_theta_max         31.673
_diffrn_reflns_theta_min         1.516
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.388
_exptl_absorpt_correction_T_max  0.4956
_exptl_absorpt_correction_T_min  0.1561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.88
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0767
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         11508
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.000826
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.08 0.894 0.503 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1552
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0788
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                11508
_reflns_number_total             20798
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      68.56
_oxford_refine_ls_scale          0.1692(3)
_oxford_structure_analysis_title 'p-1 in P-1'
_cod_data_source_file            ja801619e-file004.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_cell_volume        3413.8(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4108102