A New Two-Dimensional Molybdenum(V) Nickel Phosphate Built Up of [H18(Mo16O32)Ni16(PO4)26(OH)6(H2O)8]18- Wheels
Charlotte du Peloux; Anne Dolbecq; Pierre Mialane; Jérôme Marrot; Eric Rivière; Francis Sécheresse; Inorganic Chemistry 41 (2002) 7100–7104; doi:10.1021/ic0204880

data_4319070
_publ_contact_author
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        Pr. F. Secheresse
        Institut Lavoisier, IREM, UMR CNRS C 8637
        Universit\'e de Versailles Saint-Quentin-en-Yvelines
        45 Avenue des Etats Unis
        78035 Versailles cedex
        France
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_publ_contact_author_email       Secheres@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83'
_publ_section_title
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 A New Two-Dimensional Molybdenum(V) Nickel Phosphate Built Up of
 [H18(Mo16O32)Ni16(PO4)26(OH)6(H2O)8]18- Wheels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7100
_journal_page_last               7104
_journal_paper_doi               10.1021/ic0204880
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'H172 Mo16 Na6 Ni22 O216 P26'
_chemical_formula_weight         7399.20
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           66
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_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                   23.999(4)
_cell_length_b                   36.595(6)
_cell_length_c                   20.445(4)
_cell_measurement_reflns_used    24528
_cell_measurement_temperature    296(2)
_cell_volume                     17956(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond Brandenburg'
_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 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61917
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.721
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.5874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             14576
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.447
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.332
_refine_ls_extinction_coef       0.000086(3)
_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   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         12560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+531.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                7601
_reflns_number_total             12560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0204880.cif
_cod_data_source_block           cap5
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4319070