Hydrothermal Synthesis of Vanadium Oxyfluoride Chains Incorporating Covalently Bound Copper Coordination Complexes
Thushitha Mahenthirarajah; Yang Li; Philip Lightfoot; Inorganic Chemistry 47 (2008) 9097–9102; doi:10.1021/ic801106h

data_4306197
_publ_contact_author_address
;
School 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
;
Hydrothermal Synthesis of Vanadium Oxyfluoride Chains Incorporating
Covalently Bound Copper Coordination Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9097
_journal_page_last               9102
_journal_paper_doi               10.1021/ic801106h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H20 Cu F7 N4 O2 V2, C2 H8 N'
_chemical_formula_sum            'C22 H28 Cu F7 N5 O2 V2'
_chemical_formula_weight         692.92
_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                89.15(3)
_cell_angle_beta                 70.64(2)
_cell_angle_gamma                74.19(3)
_cell_formula_units_Z            2
_cell_length_a                   8.981(3)
_cell_length_b                   13.533(6)
_cell_length_c                   13.545(6)
_cell_measurement_reflns_used    10224
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.2
_cell_volume                     1489.2(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, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.760
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.1067
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10224
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.646
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.1236
_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^)+(0.1601P)^2^+14.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3216
_refine_ls_wR_factor_ref         0.3388
_reflns_number_gt                4651
_reflns_number_total             5927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801106h_si_001_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        1489.2(10)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4306197