‘Adding’ stable functional complementary, nucleophilic and electrophilic clusters: a synthetic route to [{(SiW11O39)Mo3S4(H2O)3(μ-OH)}2]10− and [{(P2W17O61)Mo3S4(H2O)3(μ-OH)}2]14− as examples
Müller, Achim; Fedin, Vladimir P.; Kuhlmann, Christoph; Bögge, Hartmut; Hauptfleisch, Björn; Fenske, Heinz-Dieter; Baum, Gerhard; Chemical Communications (Cambridge, United Kingdom)  (1999) 1189–1190; doi:10.1039/a903170g

data_7110565
_publ_section_title
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 &#x2018;Adding&#x2019; stable functional complementary, nucleophilic and
 electrophilic clusters: a synthetic route to
 [{(SiW11O39)Mo3S4(H2O)3(\m-OH)}2]10&#x2212; and
 [{(P2W17O61)Mo3S4(H2O)3(\m-OH)}2]14&#x2212; as examples
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_journal_coden_ASTM              CHCOFS
_journal_issue                   13
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1189
_journal_page_last               1190
_journal_paper_doi               10.1039/a903170g
_journal_year                    1999
_chemical_formula_sum            'C20 H134 Mo6 N10 O106 S8 Si2 W22'
_chemical_formula_weight         7144.37
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.820(5)
_cell_length_b                   20.980(4)
_cell_length_c                   26.870(5)
_cell_measurement_temperature    293(2)
_cell_volume                     13880(5)
_computing_molecular_graphics
'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.479
_diffrn_measured_fraction_theta_max 0.479
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46509
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    18.905
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             12832
_refine_diff_density_max         3.285
_refine_diff_density_min         -2.695
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         14784
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                9300
_reflns_number_total             14784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903170gsup1.cif
_cod_data_source_block           m17
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.0000P] 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^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7110565