The role of temperature in the solvothermal synthesis of hybrid vanadium oxyfluorides
Aldous, David W.; Stephens, Nicholas F.; Lightfoot, Philip; Dalton Transactions  (2007) 4207–; doi:10.1039/b708889b

data_7006088
_publ_section_title
;
 The role of temperature in the solvothermal synthesis of hybrid
 vanadium oxyfluorides
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              4207
_journal_paper_doi               10.1039/b708889b
_journal_year                    2007
_chemical_formula_moiety         'C4 H12 N2, F4 H2 O2 V'
_chemical_formula_sum            'C4 H14 F4 N2 O2 V'
_chemical_formula_weight         249.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                97.444(3)
_cell_angle_beta                 101.073(3)
_cell_angle_gamma                104.340(3)
_cell_formula_units_Z            2
_cell_length_a                   5.7184(8)
_cell_length_b                   8.2456(12)
_cell_length_c                   9.8105(14)
_cell_measurement_temperature    125(2)
_cell_volume                     432.13(11)
_computing_cell_refinement       'Crystalclear (Rigaku Corp., 2004)'
_computing_data_collection       'Crystalclear (Rigaku Corp., 2004)'
_computing_data_reduction        'Crystalclear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Confocal Optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4505
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1970
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                1790
_reflns_number_total             1970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708889b.txt
_cod_data_source_block           IV
_cod_database_code               7006088