#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000093.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000093
_journal_name_full               'Chemistry of Materials'
_journal_year                    2001
_chemical_formula_sum            'H17 Na8 O47.5 Si12 Ti5'
_chemical_formula_weight         1537.64
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   23.2272(4)
_cell_length_b                   7.1751(11)
_cell_length_c                   6.9727(6)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     1162.1(2)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            981
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         4.85
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9008
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             763
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0677
_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/[σ²(Fo²)+(0.0600P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                413
_reflns_number_total             582
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      Cmmm
_cod_original_formula_sum        'H17 Na8 O47.50 Si12 Ti5'
_cod_database_code               4000093
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.2500 0.2500 0.5000 0.0172(8) Uani 1 4 d S . .
Ti2 Ti 0.0000 0.0000 0.4417(14) 0.016(3) Uani 0.25 4 d SP . .
Si1 Si 0.16178(11) 0.5000 0.2304(4) 0.0111(8) Uani 1 2 d S . .
Si2 Si 0.0642(2) 0.4050(8) 0.5000 0.0127(12) Uani 0.50 2 d SP . .
O1 O 0.1537(4) 0.5000 0.0000 0.019(2) Uani 1 4 d S . .
O2 O 0.0955(3) 0.5000 0.3108(11) 0.0236(19) Uani 1 2 d S . .
O3 O 0.1934(2) 0.3122(7) 0.2971(7) 0.0199(13) Uani 1 1 d . . .
O4 O 0.2199(4) 0.0000 0.5000 0.018(2) Uani 1 4 d S . .
O5 O 0.0000 0.5000 0.5000 0.019(3) Uani 1 8 d S . .
O6 O 0.0612(7) 0.179(2) 0.5000 0.026(4) Uani 0.50 2 d SP . .
O7 O 0.0000 0.0000 0.198(9) 0.039(13) Uani 0.25 4 d SP . .
Na1 Na 0.2500 0.2500 0.0000 0.030(3) Uani 0.50 4 d SP . .
Na2 Na 0.1400(4) 0.0000 0.2757(14) 0.063(3) Uani 0.75 2 d SP . .
O1W O 0.2084(10) 0.058(3) 0.0000 0.056(7) Uani 0.50 2 d SP . .
O2W O 0.0812(17) 0.094(7) 0.0000 0.057(13) Uani 0.25 2 d SP . .
O5W O 0.473(2) 0.148(10) 0.0000 0.10(2) Uiso 0.25 2 d SP . .
O6W O 0.5000 0.0000 0.0000 0.08(3) Uiso 0.25 8 d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0173(15) 0.0219(17) 0.0124(14) 0.000 0.000 0.0057(11)
Ti2 0.017(5) 0.014(5) 0.016(7) 0.000 0.000 0.000
Si1 0.0135(14) 0.0147(15) 0.0052(14) 0.000 -0.0008(10) 0.000
Si2 0.010(3) 0.014(3) 0.015(3) 0.000 0.000 0.001(2)
O1 0.023(6) 0.031(6) 0.003(5) 0.000 0.000 0.000
O2 0.013(4) 0.037(5) 0.021(4) 0.000 0.005(3) 0.000
O3 0.024(3) 0.018(3) 0.017(3) 0.001(2) -0.010(2) 0.002(2)
O4 0.009(5) 0.015(5) 0.029(6) 0.000 0.000 0.000
O5 0.018(8) 0.025(9) 0.014(8) 0.000 0.000 0.000
O6 0.037(10) 0.020(9) 0.022(9) 0.000 0.000 -0.014(7)
O7 0.05(3) 0.01(2) 0.06(4) 0.000 0.000 0.000
Na1 0.042(8) 0.030(8) 0.018(6) 0.000 0.000 0.017(6)
Na2 0.089(7) 0.040(5) 0.060(5) 0.000 -0.038(5) 0.000
O1W 0.090(15) 0.037(16) 0.040(11) 0.000 0.000 0.022(10)
O2W 0.04(2) 0.09(3) 0.04(2) 0.000 0.000 0.03(2)
