Solid-State Structural Characterization of a Rigid Framework of Lacunary Heteropolyniobates
Nyman, May; Celestian, Aaron J.; Parise, John B.; Holland, Gregory P.; Alam, Todd M.; Inorganic Chemistry 45 (2006) 1043–1052; doi:10.1021/ic051155g

data_4331589
_publ_section_title
;
 Solid-State Structural Characterization of a Rigid Framework of Lacunary
 Heteropolyniobates
;
_journal_issue                   3
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1043
_journal_page_last               1052
_journal_paper_doi               10.1021/ic051155g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '15(Na+), Nb9 O40 P4, 22(H2 O)'
_chemical_formula_sum            'Na15 Nb9 O62 P4'
_chemical_formula_weight         2296.92
_chemical_melting_point          ?
_chemical_name_common            'A-type trivacant alpha-Keggin ion'
_chemical_name_systematic
; 
 Lacunary Keggin Ion 
;
_space_group_IT_number           2
_symmetry_cell_setting           1
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.12(3)
_cell_angle_beta                 99.78(3)
_cell_angle_gamma                119.84(3)
_cell_formula_units_Z            2
_cell_length_a                   12.242(2)
_cell_length_b                   12.291(3)
_cell_length_c                   22.056(4)
_cell_measurement_reflns_used    7522
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.19
_cell_measurement_theta_min      2.61
_cell_volume                     2799.1(14)
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  MAR345
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.92200
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7522
_diffrn_reflns_theta_full        31.19
_diffrn_reflns_theta_max         31.19
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.725
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.0015
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         7522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0724P)^2^+37.0798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                7418
_reflns_number_total             7522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051155gsup1.cif
_cod_data_source_block           NaNbPO_Lacunary
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1148.46
_cod_original_formula_moiety         'Na7.50 Nb4.50 O31 P2'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        2799.2(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'Na7.50 Nb4.50 O31 P2'
_cod_database_code               4331589