Coordination-Induced Condensation of [Ta6O19](8-): Synthesis and Structure of [{(C6H6)Ru}2Ta6O19](4-) and [{(C6H6)RuTa6O18}2(μ-O)](10-)
Abramov, P. A.; Sokolov, M. N.; Floquet, S.; Haouas, M.; Taulelle, F.; Cadot, E.; Peresypkina, E. V.; Virovets, A. V.; Vicent, C.; Kompankov, N. B.; Zhdanov, A. A.; Shuvaeva, O. V.; Fedin, V. P.; Inorganic chemistry  (2014) 141203085652001–; doi:10.1021/ic501622t

data_4341840
_publ_section_title
;
 Coordination-Induced Condensation of [Ta6O19](8-): Synthesis and
 Structure of [{(C6H6)Ru}2Ta6O19](4-) and [{(C6H6)RuTa6O18}2(\m-O)](10-)
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141203085652001
_journal_paper_doi               10.1021/ic501622t
_journal_year                    2014
_chemical_formula_structural     'Na10 [(Ta6 O19)2 O (Ru (C6 H6))2]*39.4H2O'
_chemical_formula_sum            'C12 H90.8 Na10 O76.4 Ru2 Ta12'
_chemical_formula_weight         4061.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8487(9)
_cell_length_b                   17.7022(9)
_cell_length_c                   27.7928(13)
_cell_measurement_reflns_used    4882
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.353
_cell_measurement_theta_min      2.301
_cell_volume                     9765.4(8)
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8Apex CCD detector'
_diffrn_measurement_method       'combined omega- and phi-scans'
_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  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            28289
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.825
_exptl_absorpt_correction_T_max  0.7326
_exptl_absorpt_correction_T_min  0.1667
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.763
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.045
_refine_diff_density_min         -3.689
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         7637
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0174P)^2^+804.2580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                5738
_reflns_number_total             7637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501622t_si_001.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      Cmca
_cod_original_formula_sum        'C12 H90.80 Na10 O76.40 Ru2 Ta12'
_cod_database_code               4341840