Facile Synthesis of Zero-, One-, and Two-Dimensional Vanadyl Pyrophosphates
Diego Solis-Ibarra; Jared S. Silvia; Vojtech Jancik; Christopher C. Cummins; Inorganic Chemistry 50 (2011) 9980–9984; doi:10.1021/ic200510y

data_4326448
_publ_contact_author_address
;
Department of Chemistry, Massachusetts Institute of Technology, 
77 Massachusetts Avenue, Cambridge, Massachusetts 02139
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Facile Synthesis of Zero-, One-, and Two-Dimensional Vanadyl
 Pyrophosphates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9980
_journal_page_last               9984
_journal_paper_doi               10.1021/ic200510y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Na2 O8 P2 V, 8 (H2O)'
_chemical_formula_sum            'H16 Na2 O16 P2 V'
_chemical_formula_weight         430.99
_chemical_name_systematic
; 
 ? 
;
_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                 98.5710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.78520(10)
_cell_length_b                   9.60940(10)
_cell_length_c                   16.7847(3)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.04
_cell_measurement_theta_min      5.32
_cell_volume                     1401.15(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25105
_diffrn_reflns_theta_full        69.74
_diffrn_reflns_theta_max         69.74
_diffrn_reflns_theta_min         5.32
_exptl_absorpt_coefficient_mu    9.539
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.3878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_description       shard
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         2634
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+3.7528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                2618
_reflns_number_total             2634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200510y_si_001_1.cif
_cod_data_source_block           d8_10013
_cod_database_code               4326448