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_4108101
_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         'C24 H26 Ga10 N4 S16'
_chemical_formula_sum            'C24 H26 Ga10 N4 S16'
_chemical_formula_weight         1580.75
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-01-30
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.4329(14)
_cell_length_b                   19.7762(8)
_cell_length_c                   18.5622(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     13741.2(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.051
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            156171
_diffrn_reflns_theta_full        29.850
_diffrn_reflns_theta_max         30.459
_diffrn_reflns_theta_min         1.030
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.360
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0998
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6921
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000609
_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: 
 0.410 0.365 0.327 0.119 0.796E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1155
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0448
_reflns_limit_h_max              53
_reflns_limit_h_min              0
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6921
_reflns_number_total             20783
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   2.05
_oxford_diffrn_Wilson_scale      3073.99
_oxford_refine_ls_scale          0.02558(3)
_oxford_structure_analysis_title 'Orth2 in Pcca'
_cod_data_source_file            ja801619e-file003.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P c c a '
_cod_database_code               4108101