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_7029946
_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            'C48 H40 F2 O8 Ta2'
_chemical_formula_weight         1144.70
_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                68.033(4)
_cell_angle_beta                 86.135(4)
_cell_angle_gamma                68.477(4)
_cell_formula_units_Z            1
_cell_length_a                   9.940(4)
_cell_length_b                   10.003(4)
_cell_length_c                   12.384(5)
_cell_measurement_reflns_used    2919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.8905
_cell_measurement_theta_min      2.210
_cell_volume                     1058.8(7)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9079
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    5.227
_exptl_absorpt_correction_T_max  0.5727
_exptl_absorpt_correction_T_min  0.4885
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Data were corrected for Lorentz polarization and absorption
effects (empirical absorption correction SADABS).
R(int) = 0.0981 (selected reflections only, before parameter refinement)
R(int) = 0.0588 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism irregular'
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.382
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3583
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                2957
_reflns_number_total             3583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31453c.txt
_cod_data_source_block           p1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029946