‘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_7110566
_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            'C28 H176 Mo6 N14 O155 P4 S8 W34'
_chemical_formula_weight         10396.73
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.419(5)
_cell_length_b                   15.110(3)
_cell_length_c                   56.036(11)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.63
_cell_volume                     18982(7)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.474
_diffrn_measured_fraction_theta_max 0.474
_diffrn_measurement_device_type  'Bruker AXS SMART'
_diffrn_measurement_method       omega-scan
_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  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            50940
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    21.114
_exptl_absorpt_correction_T_max  0.2611
_exptl_absorpt_correction_T_min  0.0868
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            braun
_exptl_crystal_density_diffrn    3.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             18552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.623
_refine_diff_density_min         -5.381
_refine_diff_density_rms         0.692
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.789
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         10571
_refine_ls_number_restraints     378
_refine_ls_restrained_S_all      1.761
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.1225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+5000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2363
_reflns_number_gt                8616
_reflns_number_total             10571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903170gsup1.cif
_cod_data_source_block           long
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+5000.0000P] 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^)+(0.0100P)^2^+5000.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        18983(7)
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               7110566