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_4319658
_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[Nb6O19{Re(CO)3}2].29H2O
_chemical_formula_sum            'C6 H58 K6 Nb6 O54 Re2'
_chemical_formula_weight         2158.98
_chemical_melting_point          'decomposes before melting'
_chemical_name_common            'Potassium dirheniumhexacarbonylhexaniobate'
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8666(19)
_cell_length_b                   10.3085(9)
_cell_length_c                   26.780(2)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      56.617
_cell_measurement_theta_min      4.414
_cell_volume                     5714.9(8)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  SMART-CCD
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62719
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    5.931
_exptl_absorpt_correction_T_max  0.212023
_exptl_absorpt_correction_T_min  0.097660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         4.536
_refine_diff_density_min         -2.542
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         13991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+103.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                12172
_reflns_number_total             13991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001031y_5.cif
_cod_data_source_block           cre2nb6
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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        5714.8(9)
_cod_database_code               4319658