A fluorophosphate-based inverse Keggin structure.
Fielden, John; Quasdorf, Kyle; Cronin, Leroy; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9876–9878; doi:10.1039/c2dt30501a

data_7019777
_publ_section_title
;
 A fluorophosphate-based inverse Keggin structure.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9876
_journal_page_last               9878
_journal_paper_doi               10.1039/c2dt30501a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
;
3 (H), C8 H12 Cu N4, F4 Mo12 O46 P4, 4(C2 H3 N), 32 (H2 O)
;
_chemical_formula_sum            'C16 H91 Cu F4 Mo12 N8 O78 P4'
_chemical_formula_weight         3058.67
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m 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                   30.162(5)
_cell_length_b                   17.875(3)
_cell_length_c                   20.715(3)
_cell_measurement_reflns_used    996
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.37
_cell_volume                     11168(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41216
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.7903
_exptl_absorpt_correction_T_min  0.6380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The void space is occupied by disordered solvent (assumed to be water on IR
spectral evidence) which does not refine successfully.
;
_refine_diff_density_max         2.149
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5187
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                3518
_reflns_number_total             5187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30501a.txt
_cod_data_source_block           kq136ags3
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               7019777
_platon_squeeze_results
;
Note: Data are Listed for all Voids in the P1 Unit Cell i.e. Centre of Gravity,
Solvent Accessible Volume, Recovered number of Electrons in the Void and
Details about the Squeezed Material
;