Flux Synthesis, Crystal Structures, and Solid-State NMR Spectroscopy of Two Indium Silicates Containing Varied In-O Coordination Geometries
Ling-I Hung; Sue-Lein Wang; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 46 (2007) 3301–3305; doi:10.1021/ic0700349

data_4308062
_publ_section_title
;
Flux Synthesis, Crystal Structures, and Solid-State NMR Spectroscopy of Two
Indium Silicates Containing Varied In-O Coordination Geometries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3301
_journal_page_last               3305
_journal_paper_doi               10.1021/ic0700349
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         K5In3Si7O21
_chemical_formula_sum            'In3 K5 O21 Si7'
_chemical_formula_weight         1072.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   12.4914(3)
_cell_length_b                   16.8849(3)
_cell_length_c                   10.2275(2)
_cell_measurement_reflns_used    5070
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.03
_cell_volume                     2157.14(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scan'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13326
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.303
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(14)
_refine_ls_extinction_coef       0.00046(5)
_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   0.702
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.702
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+8.1366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                4772
_reflns_number_total             4921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0700349si20070213_103121_1.cif
_cod_data_source_block           1
_cod_database_code               4308062