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_4307052
_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_moiety         'K, C14 H36 Nd2 O38 S14 W6, Br, 14(H2 O)'
_chemical_formula_structural
'K [(W3 S7 (C2 O4)3 Nd(H2 O)5)2 C2 O4] Br * 14H2 O'
_chemical_formula_sum            'C14 H48 Br K Nd2 O52 S14 W6'
_chemical_formula_weight         3007.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.2490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9015(4)
_cell_length_b                   18.8307(4)
_cell_length_c                   16.3162(3)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      28.2524
_cell_measurement_theta_min      2.5058
_cell_volume                     6641.7(2)
_computing_cell_refinement       'APEX2 v.1.0-27 (Bruker, 2004)'
_computing_data_collection       'APEX2 v.1.0-27 (Bruker, 2004)'
_computing_data_reduction        'APEX2 v.1.0-27 (Bruker, 2004)'
_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      90.0(5)
_diffrn_detector_area_resol_mean 25.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8APEX CCD diffractometer'
_diffrn_measurement_method       'phi & omega 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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31045
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.092
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on untensities, SADABS (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.024
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             5624
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.977
_refine_diff_density_min         -5.754
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7599
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0318P)^2^+293.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                6119
_reflns_number_total             7599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061540lsi20060815_124319_5.cif
_cod_data_source_block           compound_IIb
_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_database_code               4307052