A Novel Zirconium Polyoxometalate Complex That Contains Both a Coordinated Saturated Anion, [PMo12O40]3-, and a Coordinated Unsaturated Anion, [PMo11O39]7-
Andrew J. Gaunt; Iain May; David Collison; O. Danny Fox; Inorganic Chemistry 42 (2003) 5049–5051; doi:10.1021/ic034273h

data_4314063
_publ_section_title
;
 A Novel Zirconium Polyoxometalate Complex That Contains Both a
 Coordinated Saturated Anion, [PMo12O40]3-, and a Coordinated Unsaturated
 Anion, [PMo11O39]7-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5049
_journal_page_last               5051
_journal_paper_doi               10.1021/ic034273h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'H76 Mo23 N6 O105 P2 Zr'
_chemical_formula_weight         4200.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 93.726(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.743(3)
_cell_length_b                   19.827(4)
_cell_length_c                   18.791(4)
_cell_measurement_reflns_used    7218
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2865
_cell_measurement_theta_min      2.403
_cell_volume                     4737.6(18)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'XSHELL, Bruker'
_computing_publication_material  'XP, Bruker; Diamond 2.1e, Crystal Impact'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART platform CCD, Bruker'
_diffrn_measurement_method       '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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35245
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    3.203
_exptl_absorpt_correction_T_max  0.9387
_exptl_absorpt_correction_T_min  0.5392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3988
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.580
_refine_diff_density_min         -5.875
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0686
_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^)+(0.1070P)^2^+177.5144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                7696
_reflns_number_total             8621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034273hsi20030313_055933.cif
_cod_data_source_block           ajg28z
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_database_code               4314063