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_4318434
_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^ 4(C19 H34)^+1^ 3(C2 H4 Cl2) 0.5(C1 H2 Cl2) 0.5(C7 H8)'
_chemical_formula_sum            'C86 H153 Cl25 N4 Ta6'
_chemical_formula_weight         3215.07
_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                 106.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.259(6)
_cell_length_b                   14.319(3)
_cell_length_c                   30.788(6)
_cell_measurement_reflns_used    51037
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     11537(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & 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 0.796
_diffrn_measured_fraction_theta_max 0.796
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            78473
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    6.287
_exptl_absorpt_correction_T_max  0.6332
_exptl_absorpt_correction_T_min  0.1876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6240
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.368
_refine_diff_density_min         -2.141
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         21153
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+26.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                16260
_reflns_number_total             21153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201452_2.cif
_cod_data_source_block           Ta6Cl18-4_solvated
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        11536(4)
_cod_database_code               4318434