The First Observation of Heteronuclear Two-Bond J-Coupling in the Solid State: Crystal Structure and Solid-State NMR Spectroscopy of Rb4(NbO)2(Si8O21)
Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 41 (2002) 5644–5646; doi:10.1021/ic0204373

data_4318781
_publ_section_title
;
 The First Observation of Heteronuclear Two-Bond J-Coupling in the Solid
 State: Crystal Structure and Solid-State NMR Spectroscopy of
 Rb4(NbO)2(Si8O21)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5644
_journal_page_last               5646
_journal_paper_doi               10.1021/ic0204373
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_structural     Rb4(NbO)2(Si8O21)
_chemical_formula_sum            'Nb2 O23 Rb4 Si8'
_chemical_formula_weight         1120.42
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.4900(10)
_cell_angle_beta                 89.2970(10)
_cell_angle_gamma                71.8310(10)
_cell_formula_units_Z            1
_cell_length_a                   6.8977(5)
_cell_length_b                   7.7585(5)
_cell_length_c                   11.0133(7)
_cell_measurement_temperature    294(2)
_cell_volume                     543.33(6)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Siemens Smart CCD diffractometer'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5369
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    10.507
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.424
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0153(7)
_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_all   1.060
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_obs          0.0209
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.1439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0562
_refine_ls_wR_factor_obs         0.0553
_reflns_number_observed          2225
_reflns_number_total             2400
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0204373.cif
_cod_data_source_block           nv42m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.1439P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.1439P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318781