Synthesis and Crystal Structure of a Self-Assembled, Octanuclear Oxo-Tantalum(V) Derivative Containing the First Example of a Transition Metal M8(μ-O)12 Cage
Paola B. Arimondo; Fausto Calderazzo; Ralph Hiemeyer; Cäcilia Maichle-Mössmer; Fabio Marchetti; Guido Pampaloni; Joachim Strähle; Inorganic Chemistry 37 (1998) 5507–5511; doi:10.1021/ic980408l

data_4323095
_publ_contact_author
;
        Guido Pampaloni
        Dipartimento di Chimica e Chimica Industriale
        Universita' di Pisa
        Via Risorgimento, 35
        56126 Pisa
        Italy
;
_publ_contact_author_email       pampa@dcci.unipi.it
_publ_contact_author_fax         '050 20237'
_publ_contact_author_phone       '050 918221'
_publ_section_title
;
 Synthesis and Crystal Structure of a Self-Assembled, Octanuclear
 Oxo-Tantalum(V) Derivative Containing the First Example of a Transition
 Metal M8(\m-O)12 Cage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5507
_journal_page_last               5511
_journal_paper_doi               10.1021/ic980408l
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'Ta8 (*mu*2-O)12 (O2CN(C2H5)2)16'
_chemical_formula_sum            'C80 H160 N16 O44 Ta8'
_chemical_formula_weight         1748.92
_chemical_name_systematic
; 
 Hexadeca-N,N-diethylcarbamate-dodeca*mu*2-oxo-octatantalum(V) 
;
_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                101.53(4)
_cell_angle_beta                 107.51(5)
_cell_angle_gamma                118.80(3)
_cell_formula_units_Z            1
_cell_length_a                   15.440(3)
_cell_length_b                   15.7109(10)
_cell_length_c                   16.090(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      8
_cell_volume                     2971(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius CAD 4'
_diffrn_measurement_method       *omega*-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K*alpha*
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14376
_diffrn_reflns_theta_full        26.92
_diffrn_reflns_theta_max         26.92
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.416
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          '0.3 mm'
_exptl_crystal_size_mid          '0.2 mm'
_exptl_crystal_size_min          '0.2 mm'
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.203
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+13.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                10132
_reflns_number_total             12921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980408l.cif
_cod_data_source_block           tanca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+13.4220P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+13.4220P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2971.4(7)
_cod_database_code               4323095