Synthesis, chemistry and structures of complexes of the dioxovanadium(v) halides VO2F and VO2Cl
Davis, Martin F.; Jura, Marek; Leung, Alethea; Levason, William; Littlefield, Benjamin; Reid, Gillian; Webster, Michael; Dalton Transactions  (2008) 6265–6273; doi:10.1039/b811422f

data_7004738
_publ_section_title
;
 Synthesis, chemistry and structures of complexes of the
 dioxovanadium(v) halides VO2F and VO2Cl
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6265
_journal_page_last               6273
_journal_paper_doi               10.1039/b811422f
_journal_year                    2008
_chemical_formula_moiety         'C54 H45 O5 P3 V 1+, Cl2 O2 V 1-'
_chemical_formula_structural     '((C18 H15 O P)3 O2 V) (Cl2 O2 V)'
_chemical_formula_sum            'C54 H45 Cl2 O7 P3 V2'
_chemical_formula_weight         1071.59
_chemical_name_common
;Dioxotris(triphenylphosphine oxide-O)vanadium(V)
dichlorodioxovanadate
;
_chemical_name_systematic
;
Dioxotris(triphenylphosphine oxide-O)vanadium(V) dichlorodioxovanadate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2008-04-29
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                94.45(2)
_cell_angle_beta                 94.367(15)
_cell_angle_gamma                97.27(2)
_cell_formula_units_Z            2
_cell_length_a                   12.431(4)
_cell_length_b                   14.080(4)
_cell_length_c                   14.558(4)
_cell_measurement_reflns_used    80284
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2510.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29767
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         4.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+5.7632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                8449
_reflns_number_total             11001
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b811422f.txt
_cod_data_source_block           08mj25
_cod_original_cell_volume        2510.5(12)
_cod_database_code               7004738