Novel Vanadium(IV) Oxyfluorides with 'Spin-Ladder'-Like Structures, and Their Relationship to (VO)2P2O7
David W. Aldous; Richard J. Goff; J. Paul Attfield; Philip Lightfoot; Inorganic Chemistry 46 (2007) 1277–1282; doi:10.1021/ic0617386

data_4307199
_publ_contact_author_address
;
Department of Chemistry
University of St Andrews
St Andrews
Fife
KY16 9ST
UNITED KINGDOM
;
_publ_contact_author_email       PL@ST-ANDREWS.AC.UK
_publ_contact_author_name        'Dr Philip Lightfoot'
_publ_section_title
;
Novel Vanadium(IV) Oxyfluorides with 'Spin-Ladder'-Like Structures, and
Their Relationship to (VO)2P2O7
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1277
_journal_page_last               1282
_journal_paper_doi               10.1021/ic0617386
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C6 H5 N, F3 O V'
_chemical_formula_sum            'C48 H48 F24 N8 O8 V8'
_chemical_formula_weight         215.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.010(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.972(2)
_cell_length_b                   15.663(3)
_cell_length_c                   7.5810(16)
_cell_measurement_temperature    150(2)
_cell_volume                     1416.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART 1K CCD Diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'SRS Daresbury Laboratories'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.84620
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5136
_diffrn_reflns_theta_full        33.02
_diffrn_reflns_theta_max         33.02
_diffrn_reflns_theta_min         3.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.485
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                989
_reflns_number_total             1506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0617386si20060914_110505_1.cif
_cod_data_source_block           bpe-VOF3
_cod_database_code               4307199