Convenient synthesis of fluoride-alkoxides of Nb(V) and Ta(V): a spectroscopic, crystallographic and computational study.
Bortoluzzi, Marco; Guazzelli, Nicola; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 41 (2012) 12898–12906; doi:10.1039/c2dt31453c

data_7029945
_publ_section_title
;
 Convenient synthesis of fluoride-alkoxides of Nb(V) and Ta(V): a
 spectroscopic, crystallographic and computational study.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12898
_journal_page_last               12906
_journal_paper_doi               10.1039/c2dt31453c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C39 H37 F9 Nb3 O6'
_chemical_formula_weight         1051.42
_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                83.930(2)
_cell_angle_beta                 75.313(2)
_cell_angle_gamma                86.150(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5980(18)
_cell_length_b                   11.661(2)
_cell_length_c                   18.367(3)
_cell_measurement_reflns_used    1677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.836
_cell_measurement_theta_min      2.188
_cell_volume                     1975.6(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(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       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_sigmaI/netI    0.1483
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18800
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Data were corrected for Lorentz polarization and absorption
effects (empirical absorption correction SADABS).
R(int) = 0.0859 (selected reflections only, before parameter refinement)
R(int) = 0.0528 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         6969
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                3643
_reflns_number_total             6969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31453c.txt
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029945