Fine Hierarchy of the V-O Bonds by Advanced Solid State NMR: Novel Pb4(VO2)(PO4)3 Structure as a Textbook Case
Grégory Tricot; Olivier Mentré; Sylvain Cristol; Laurent Delevoye; Inorganic Chemistry 51 (2012) 13108–13113; doi:10.1021/ic300966r

data_4331262
_publ_contact_author_address
;
UCCS, UMR CNRS 8181
Ecole de Chimie de Lille (bat C7)
Villeneuve d'Ascq
France
;
_publ_contact_author_email       olivier@ensc-lille.fr
_publ_contact_author_fax         0033320436814
_publ_contact_author_name        'Dr Olivier Mentre'
_publ_contact_author_phone       0033320337721
_publ_section_title
;
 Fine Hierarchy of the V-O Bonds by Advanced Solid State NMR: Novel
 Pb4(VO2)(PO4)3 Structure as a Textbook Case
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13108
_journal_page_last               13113
_journal_paper_doi               10.1021/ic300966r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'O7 P1.5 Pb2 V0.5'
_chemical_formula_weight         598.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.873(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   13.493(4)
_cell_length_b                   13.798(4)
_cell_length_c                   13.274(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2470.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.1096
_diffrn_reflns_av_sigmaI/netI    0.1307
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18920
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    54.827
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.141156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 Bruker AXS'
_exptl_crystal_colour            yellow-transparent
_exptl_crystal_density_diffrn    6.439
_exptl_crystal_description       block-like
_exptl_crystal_F_000             1019
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         8.104
_refine_diff_density_min         -7.845
_refine_diff_density_rms         0.908
_refine_ls_extinction_coef       0.000106(17)
_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   0.946
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                3850
_reflns_number_total             6093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300966r_si_002.cif
_cod_data_source_block           structure
_cod_original_cell_volume        2470.0(11)
_cod_original_sg_symbol_Hall     '-P 2ycb'
_cod_original_formula_sum        'O7 P1.50 Pb2 V0.50'
_cod_database_code               4331262