High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal Structure, and Solid State NMR Spectroscopy of a New Vanadium(IV) Silicate: Rb2(VO)(Si4O10).xH2O
Chun-Yi Li; Chan-Yen Hsieh; Hsiu-Mei Lin; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 41 (2002) 4206–4210; doi:10.1021/ic020187q

data_4318319
_publ_section_title
;
 High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal
 Structure, and Solid State NMR Spectroscopy of a New Vanadium(IV)
 Silicate: Rb2(VO)(Si4O10).xH2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4206
_journal_page_last               4210
_journal_paper_doi               10.1021/ic020187q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Rb2(VO)(Si4O10).xH2O
_chemical_formula_sum            'O11 Rb2 Si4 V'
_chemical_formula_weight         510.24
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           109
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2'
_symmetry_space_group_name_H-M   'I 41 m d'
_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                   12.2225(7)
_cell_length_b                   12.2225(7)
_cell_length_c                   7.7948(6)
_cell_measurement_temperature    295(2)
_cell_volume                     1164.46(13)
_computing_molecular_graphics    'XP, Diamond'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens Smart CCD'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3629
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    9.617
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.910
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       dipyramidal
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.043(11)
_refine_ls_extinction_coef       0.0032(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   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         686
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0469P)^2^+1.8995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                669
_reflns_number_total             686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020187q.cif
_cod_data_source_block           au07sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4318319