Triangular Oxalate Clusters [W3(μ3-S)(μ2-S2)3(C2O4)3]2- as Building Blocks for Coordination Polymers and Nanosized Complexes
Maxim N. Sokolov; Artem L. Gushchin; Konstantin A. Kovalenko; Eugenia V. Peresypkina; Alexander V. Virovets; Joaquin Sanchiz; Vladimir P. Fedin; Inorganic Chemistry 46 (2007) 2115–2123; doi:10.1021/ic061540l

data_4307050
_publ_contact_author_address
;
 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         '007 383 3309489'
_publ_contact_author_name        'Dr Eugenia V. Peresypkina'
_publ_section_title
;
Triangular Oxalate Clusters [W3(\m3-S)(\m2-S2)3(C2O4)3]2- as Building Blocks
for Coordination Polymers and Nanosized Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2115
_journal_page_last               2123
_journal_paper_doi               10.1021/ic061540l
_journal_volume                  46
_journal_year                    2007
_chemical_formula_structural
'[Ce (H2 O)6]3 [W3 S7 (C2 O4)3]4 Br * 24.95(H2 O)'
_chemical_formula_sum            'C24 H85.9 Br Ce3 O90.95 S28 W12'
_chemical_formula_weight         5434.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           150
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   25.3218(6)
_cell_length_b                   25.3218(6)
_cell_length_c                   13.2303(5)
_cell_measurement_reflns_used    7363
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.2866
_cell_measurement_theta_min      2.2265
_cell_volume                     7346.7(4)
_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      90(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.017
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.457
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5013
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.303
_refine_diff_density_min         -2.487
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.751
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         11234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.751
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0453P)^2^+179.6040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                9801
_reflns_number_total             11234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061540lsi20060815_124319_3.cif
_cod_data_source_block           compound_Ib
_cod_depositor_comments
;
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_cell_volume        7346.6(4)
_cod_original_formula_sum        'C24 H85.90 Br Ce3 O90.95 S28 W12'
_cod_database_code               4307050