Rational Synthesis and Characterization of the Mixed-Metal Organometallic Polyoxometalates [Cp*Mo~x~W~6-x~O~18~]^-^ (x = 0, 1, 5, 6)
Gülnur Taban-Çalişkan; Daniel Mesquita Fernandes; Jean-Claude Daran; Dominique Agustin; Funda Demirhan; Rinaldo Poli; Inorganic Chemistry 51 (2012) 5931–5940; doi:10.1021/ic300578g

data_4329292
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_name        'Daran, Jean-Claude'
_publ_contact_author_phone       ' (33) 5 61 33 31 18 '
_publ_section_title
;
 Rational Synthesis and Characterization of the Mixed-Metal Organometallic
 Polyoxometalates [Cp*Mo~x~W~6-x~O~18~]^-^ (x = 0, 1, 5, 6)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5931
_journal_page_last               5940
_journal_paper_doi               10.1021/ic300578g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C10 H15 Mo6 O18, C24 H20 P, C3 H6 O'
_chemical_formula_sum            'C37 H41 Mo6 O19 P'
_chemical_formula_weight         1396.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_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                   14.8994(7)
_cell_length_b                   13.8507(7)
_cell_length_c                   21.2967(8)
_cell_measurement_reflns_used    13402
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.89
_cell_volume                     4394.9(3)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       '\w 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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24229
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro (Oxford Diffraction, 2010)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_description       stick
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+9.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3956
_reflns_number_total             4682
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300578g_si_002_3.cif
_cod_data_source_block           1c
_cod_database_code               4329292