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_4504047
_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         'K Li8, (Nb12 Si O40), 12.5 O'
_chemical_formula_sum            'K Li8 Nb12 O52.5 Si'
_chemical_formula_weight         2077.63
_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                 105.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.341(4)
_cell_length_b                   10.735(2)
_cell_length_c                   21.438(4)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.91
_cell_measurement_theta_min      0.72
_cell_volume                     4512.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHEXL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'SMART 6000 CCD detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49594
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1095
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6101
_diffrn_reflns_theta_full        15.91
_diffrn_reflns_theta_max         15.91
_diffrn_reflns_theta_min         0.72
_diffrn_source                   synchrotron
_diffrn_source_type              'APS beamline 15-ID'
_exptl_absorpt_coefficient_mu    7.041
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    3.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3876
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.461
_refine_diff_density_min         -1.834
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       0.00130(15)
_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   0.973
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                4068
_reflns_number_total             6101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0606904si20061009_121049.cif
_cod_data_source_block           fb_ord
_cod_original_cell_volume        4512.8(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4504047