Polyphosphate Ions Encapsulated in Oxothiomolybdate Rings: Synthesis, Structure, and Behavior in Solution
Emmanuel Cadot; Marie-José Pouet; Chantal Robert-Labarre; Charlotte du Peloux; Jérôme Marrot; Francis Sécheresse; Journal of the American Chemical Society 126 (2004) 9127–9134; doi:10.1021/ja048746a

data_4112784
_publ_contact_author
; 
      Pr E. Cadot
      Institut Lavoisier, IREM, UMR CNRS 8637
      Universit\'e de Versailles Saint-Quentin-en-Yvelines
      45 Avenue des Etats Unis
      78035 Versailles cedex
      France
;
_publ_contact_author_email       cadot@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 82'
_publ_section_title
;
 Polyphosphate Ions Encapsulated in Oxothiomolybdate Rings: Synthesis,
 Structure, and Behavior in Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9127
_journal_page_last               9134
_journal_paper_doi               10.1021/ja048746a
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'Cl H64 K5 Mo12 O57 P2 S12'
_chemical_formula_weight         2805.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.4100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3478(2)
_cell_length_b                   15.9535(3)
_cell_length_c                   24.4659(4)
_cell_measurement_reflns_used    12555
_cell_measurement_temperature    296(2)
_cell_volume                     3645.38(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24423
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  0.8500
_exptl_absorpt_correction_T_min  0.6327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.556
_exptl_crystal_description       needle
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.690
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00062(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+14.8969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                6062
_reflns_number_total             9304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048746asi20040304_114327_1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'H64 Cl K5 Mo12 O57 P2 S12'
_cod_database_code               4112784