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_7006087
_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         'F20 O3 V5, 4(C4 H12 N2), 2(H2O)'
_chemical_formula_sum            'C16 H52 F20 N8 O5 V5'
_chemical_formula_weight         1071.31
_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                86.675(2)
_cell_angle_beta                 84.838(2)
_cell_angle_gamma                67.417(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7781(17)
_cell_length_b                   12.5240(18)
_cell_length_c                   13.3317(19)
_cell_measurement_temperature    150(2)
_cell_volume                     1807.8(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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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     0.84600
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13387
_diffrn_reflns_theta_full        33.11
_diffrn_reflns_theta_max         33.11
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    2.463
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1070.0
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.063
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+7.2189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                5955
_reflns_number_total             7374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708889b.txt
_cod_data_source_block           III
_cod_database_code               7006087