Synthesis and Characterization of a Novel Tantalum Chalcogen-Rich Molecular Cluster with Square Planar Metal Core
Maxim N. Sokolov; Artyom L. Gushchin; Alexandr V. Virovets; Eugenia V. Peresypkina; Svetlana G. Kozlova; Vladimir P. Fedin; Inorganic Chemistry 43 (2004) 7966–7968; doi:10.1021/ic0489239

data_4312159
_publ_contact_author_address
;
Nikolaev Institute of Inorganic Chemistry SD RAS  Ak.Lavrentiev prosp. 3  
Novosibirsk 630090  Russia 
;
_publ_contact_author_email       peresyp@che.nsk.su
_publ_contact_author_fax         '007 3832 344489'
_publ_contact_author_name        'Dr Eugenia V Peresypkina'
_publ_contact_author_phone       '007 3832 344466'
_publ_section_title
;
 Synthesis and Characterization of a Novel Tantalum Chalcogen-Rich
 Molecular Cluster with Square Planar Metal Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7966
_journal_page_last               7968
_journal_paper_doi               10.1021/ic0489239
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'I8 Se9 Ta4'
_chemical_formula_sum            'I8 Se9 Ta4'
_chemical_formula_weight         2449.64
_chemical_name_systematic
;
 mu4-seleno-tetrakis(mu2,hapta2-diseleno)-octaiodo-tetratantalum(IV,V)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   14.3251(4)
_cell_length_b                   14.8440(5)
_cell_length_c                   13.0603(4)
_cell_measurement_reflns_used    6222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.7
_cell_measurement_theta_min      3.1
_cell_volume                     2777.17(15)
_computing_cell_refinement       'APEX2 v.1.0-8 (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-8 (Bruker, 2003)'
_computing_data_reduction        'APEX2 v.1.0-8 (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL v.6.22 (Bruker, 1990-2003)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXTL v.6.22 (Bruker, 1990-2003)'
_computing_structure_solution    'SHELXTL v.6.22 (Bruker, 1990-2003)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23515
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    36.387
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 1990-2003)'
_exptl_crystal_colour            'metallic black'
_exptl_crystal_density_diffrn    5.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         6221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0168
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                5880
_reflns_number_total             6221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0489239rom20040805_114347.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
'__diffrn_standards_decay_%' tag replaced with
'_diffrn_standards_decay_%'.

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 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4312159