Organic-Inorganic Hybrids Based on Polyoxometalates. 6.1 Syntheses, Structure, and Reactivity of the Bis(tert-butylsilyl)decatungstophosphate [(γ-PW10O36)(t-BuSiOH)2]3-
Agnès Mazeaud; Yves Dromzee; René Thouvenot; Inorganic Chemistry 39 (2000) 4735–4740; doi:10.1021/ic0004784

data_4321472
_publ_contact_author
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                             Dr Ren\'e Thouvenot
Laboratoire de Chimie Inorganique et Mat\'eriaux Mol\'eculaires, 
ESA 7071, Universit\'e Pierre et Marie Curie, 
4 place Jussieu , 75252 Paris Cedex 05.
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_publ_contact_author_email       ' rth@ccr.jusieu.fr '
_publ_contact_author_fax         ' (33) 1 44 27 38 41 '
_publ_contact_author_phone       ' (33) 1 44 27 55 53 '
_publ_section_title
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 Organic-Inorganic Hybrids Based on Polyoxometalates. 6.1 Syntheses,
 Structure, and Reactivity of the Bis(tert-butylsilyl)decatungstophosphate
 [(\g-PW10O36)(t-BuSiOH)2]3-
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4735
_journal_page_last               4740
_journal_paper_doi               10.1021/ic0004784
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' (C8 H20 W10 P1 Si2 O38)- (C48 H108 N3)+ '
_chemical_formula_sum            'C56 H128 N3 O38 P Si2 W10'
_chemical_formula_weight         3377.27
_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_primary     direct
_audit_creation_date             00-03-06
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 98.893(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8.00
_cell_length_a                   44.762(10)
_cell_length_b                   19.032(4)
_cell_length_c                   22.079(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      13
_cell_volume                     18583(9)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      295
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17199
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        40.81
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            ' yellowish '
_exptl_crystal_density_diffrn    2.41
_exptl_crystal_description       ' parallelepiped'
_exptl_crystal_F_000             11370.53
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.53
_refine_diff_density_min         -2.32
_refine_ls_extinction_coef       44.2(103)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1420
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         4197
_refine_ls_R_factor_obs          0.0796
_refine_ls_shift/esd_max         0.243969
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0918
_reflns_limit_h_max              52
_reflns_limit_h_min              -53
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_observed          4197
_reflns_number_total             16166
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic0004784.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        18582.44(9)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C56 H128 W10 P1 Si2 O38 N3 '
_cod_database_code               4321472