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_4307051
_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 O38 Pr2 S14 W6, Br, (H2 O)14.7'
_chemical_formula_structural
'K[(W3 S7 (C2 O4)3)Pr(H2 O)5)2(C2 O4)]Br * 14.7(H2 O)'
_chemical_formula_sum            'C14 H49.4 Br K O52.7 Pr2 S14 W6'
_chemical_formula_weight         3013.91
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0999(6)
_cell_length_b                   18.6732(5)
_cell_length_c                   16.4904(6)
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      27.9875
_cell_measurement_theta_min      2.5143
_cell_volume                     6685.9(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.973
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0763
_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       -15
_diffrn_reflns_number            19706
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.912
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities, SADABS (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.994
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5644
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.704
_refine_diff_density_min         -2.348
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7485
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0376P)^2^+125.3853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                5373
_reflns_number_total             7485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061540lsi20060815_124319_4.cif
_cod_data_source_block           compound_IIa
_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_formula_sum        'C14 H49.40 Br K O52.70 Pr2 S14 W6'
_cod_database_code               4307051