Robust, Alkali-Stable, Triscarbonyl Metal Derivatives of Hexametalate Anions, [M6O19{M'(CO)3}n](8-n)- (M = Nb, Ta; M' = Mn, Re; n= 1, 2)
Alexei V. Besserguenev; Michael H. Dickman; Michael T. Pope; Inorganic Chemistry 40 (2001) 2582–2586; doi:10.1021/ic001031y

data_4319654
_publ_section_title
;
 Robust, Alkali-Stable, Triscarbonyl Metal Derivatives of Hexametalate
 Anions, [M6O19{M'(CO)3}n](8-n)- (M = Nb, Ta; M' = Mn, Re; n= 1, 2)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2582
_journal_page_last               2586
_journal_paper_doi               10.1021/ic001031y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         K6[Ta6O19{Re(CO)3}2].10H2O
_chemical_formula_sum            'C6 H20 K4 Na2 O35 Re2 Ta6'
_chemical_formula_weight         2312.70
_chemical_melting_point          'decomposes before melting'
_chemical_name_common
'Potassium sodium Dirheniumhexacarbonylhexatantalate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.531(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.648(3)
_cell_length_b                   10.0561(14)
_cell_length_c                   13.1714(19)
_cell_measurement_reflns_used    4996
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      56.57
_cell_measurement_theta_min      4.76
_cell_volume                     2159.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      171(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12287
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    21.217
_exptl_absorpt_correction_T_max  0.314
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.859
_refine_diff_density_min         -3.461
_refine_diff_density_rms         0.631
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+148.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                2272
_reflns_number_total             2793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001031y_1.cif
_cod_data_source_block           tre2ta6
_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        2159.1(5)
_cod_database_code               4319654