Gallium and Gallium Dichloride, New Solid-State Reductants in Preparative Transition Metal Chemistry. New, Lower Temperature Syntheses and Convenient Isolation of Hexatantalum Tetradecachloride Octahydrate, Ta6(μ-Cl)12Cl2(OH2)4.4H2O, and Synthesis and Solid-State Structure of a Tetraalkylammonium Derivative, [N(CH2Ph)Bu3]4[Ta6(μ-Cl)12Cl6], of the Reduced [Ta6(μ-Cl)12]2+ Cluster Core1
Daniel N. T. Hay; Dale C. Swenson; Louis Messerle; Inorganic Chemistry 41 (2002) 4700–4707; doi:10.1021/ic0201452

data_4318433
_publ_section_title
;
 Gallium and Gallium Dichloride, New Solid-State Reductants in Preparative
 Transition Metal Chemistry. New, Lower Temperature Syntheses and
 Convenient Isolation of Hexatantalum Tetradecachloride Octahydrate,
 Ta6(\m-Cl)12Cl2(OH2)4.4H2O, and Synthesis and Solid-State Structure of a
 Tetraalkylammonium Derivative, [N(CH2Ph)Bu3]4[Ta6(\m-Cl)12Cl6], of the
 Reduced [Ta6(\m-Cl)12]2+ Cluster Core1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4700
_journal_page_last               4707
_journal_paper_doi               10.1021/ic0201452
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '(Ta6 Cl18)^-4^ ((N1 C19 H34)^+1^)4'
_chemical_formula_sum            'C76 H136 Cl18 N4 Ta6'
_chemical_formula_weight         2829.69
_chemical_name_systematic
;
  ?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.074(3)
_cell_angle_beta                 83.616(3)
_cell_angle_gamma                82.896(3)
_cell_formula_units_Z            1
_cell_length_a                   12.9703(6)
_cell_length_b                   14.0317(8)
_cell_length_c                   14.0542(8)
_cell_measurement_reflns_used    10638
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2364.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowiski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowiski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL v5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v5.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v5.1 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL v5.1 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20677
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    7.462
_exptl_absorpt_correction_T_max  0.2787
_exptl_absorpt_correction_T_min  0.1457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowiski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.140
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00340(7)
_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   1.123
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         10869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+4.0730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0519
_reflns_number_gt                10414
_reflns_number_total             10869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201452_1.cif
_cod_data_source_block           Ta6Cl18-4_solvent_free
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318433