Lithium Polyniobates. A Lindqvist-Supported Lithium−Water Adamantane Cluster and Conversion of Hexaniobate to a Discrete Keggin Complex
Anderson, Travis M.; Thoma, Steven G.; Bonhomme, François; Rodriguez, Mark A.; Park, Hyunsoo; Parise, John B.; Alam, Todd M.; Larentzos, James P.; Nyman, May; Crystal Growth & Design 7 (2007) 719–; doi:10.1021/cg0606904

data_4504046
_publ_section_title
;
 Lithium Polyniobates. A Lindqvist-Supported Lithium&#x2212;Water
 Adamantane Cluster and Conversion of Hexaniobate to a Discrete Keggin
 Complex
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              719
_journal_paper_doi               10.1021/cg0606904
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'Nb6O19 15(H2O) 7(Li) 1(K)'
_chemical_formula_sum            'H30 K Li7 Nb6 O34'
_chemical_formula_weight         1219.34
_chemical_name_common            'hexaniobate salt'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.609(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.859(10)
_cell_length_b                   17.500(17)
_cell_length_c                   17.384(17)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.0
_cell_volume                     2998(5)
_computing_cell_refinement       'SMART 5.054 (Bruker, 1998)'
_computing_data_collection       'SMART 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT 6.02 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1  (Bruker, 1998)'
_computing_publication_material  'SHELXTL 5.1  (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL 5.1  (Bruker, 1998)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_method       '\w and \f 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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20141
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.475
_exptl_absorpt_correction_T_max  0.7555
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.519
_refine_diff_density_min         -2.514
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+39.7348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                4640
_reflns_number_total             5343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0606904si20061009_121029.cif
_cod_data_source_block           kli7nb6-mn
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'H30 K Li7 Nb6 O34 '
_cod_database_code               4504046