Synthesis and Characterization of the First Carbene Derivative of a Polyoxometalate
Vincent Artero; Anna Proust; Patrick Herson; Françoise Villain; Christophe Cartier dit Moulin; Pierre Gouzerh; Journal of the American Chemical Society 125 (2003) 11156–11157; doi:10.1021/ja036257p

data_4114157
_publ_contact_author
;
' Pr A. Proust                         
  Laboratoire de Chimie Inorganiques et Materiaux Moleculaires,
  Universite Pierre et Marie Curie, 4, place Jussieu, Case 42,
  75252 Paris cedex 05, France'
;
_publ_contact_author_email       'proust@ccr.jussieu.fr '
_publ_contact_author_fax         '33 1 44 27 38 41 '
_publ_contact_author_phone       '33 1 44 27 30 34 '
_publ_section_title
;
 Synthesis and Characterization of the First Carbene Derivative of a
 Polyoxometalate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11156
_journal_page_last               11157
_journal_paper_doi               10.1021/ja036257p
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source
;
?
;
_chemical_formula_moiety
' (C10 H20 O70 P2 RU1 W19)13-, (K9 Na4)13+, 15(H2 O1) '
_chemical_formula_sum            'C10 H50 K9 N4 Na4 O85 P2 Ru W19'
_chemical_formula_weight         5686.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-02-05
_audit_creation_method           CRYSTALS
_cell_angle_alpha                99.03(3)
_cell_angle_beta                 106.56(2)
_cell_angle_gamma                108.06(2)
_cell_formula_units_Z            2
_cell_length_a                   14.820(3)
_cell_length_b                   17.064(5)
_cell_length_c                   25.011(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      14
_cell_volume                     5551(3)
_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      298
_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  0.05
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20342
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        7.17
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    20.63
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan'
_exptl_crystal_colour            ' brown '
_exptl_crystal_density_diffrn    3.40
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             4872.34
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         4.51
_refine_diff_density_min         -3.32
_refine_ls_extinction_coef       35.506
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0738
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         8956
_refine_ls_R_factor_obs          0.0670
_refine_ls_shift/esd_max         0.041304
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0792
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_observed          8956
_reflns_number_total             19511
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ja036257psi20030728_042611.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'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C10 H50 W19 Ru1 P2 N4 O85 K9 Na4 '
_cod_database_code               4114157