Behavior of Tri(n-butyl)ammonium Bis[citrato(3-)-O1,O3,O6]silicate in Aqueous Solution: Analysis of a Sol-Gel Process by Small-Angle Neutron Scattering
Oliver Seiler; Christian Burschka; Dietmar Schwahn; Reinhold Tacke; Inorganic Chemistry 44 (2005) 2318–2325; doi:10.1021/ic048748w

data_4309003
_publ_contact_author_name        'Reinhold Tacke'
_publ_section_title
;
Behavior of Tri(n-butyl)ammonium Bis[citrato(3-)-O1,O3,O6]silicate in
Aqueous Solution: Analysis of a Sol-Gel Process by Small-Angle Neutron
Scattering
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2318
_journal_page_last               2325
_journal_paper_doi               10.1021/ic048748w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H66 Ge N2 O14'
_chemical_formula_sum            'C36 H66 Ge N2 O14'
_chemical_formula_weight         823.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.796(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7426(9)
_cell_length_b                   15.6919(8)
_cell_length_c                   25.024(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      4.3
_cell_volume                     4188.7(5)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Bruker-SHELXTL
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Stoe-IPDS
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39608
_diffrn_reflns_theta_full        26.95
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8886
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                7478
_reflns_number_total             8886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048748wsi20040921_030108.cif
_cod_data_source_block           sei25e
_cod_database_code               4309003