Fragmentation of oxygen-containing molecules via C‒O bond cleavage promoted by coordination to niobium and tantalum pentahalides
Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton Transactions  (2009) 6759–6772; doi:10.1039/b905023j

data_7001933
_publ_section_title
;
 Fragmentation of oxygen-containing molecules via C--O bond cleavage
 promoted by coordination to niobium and tantalum pentahalides
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              6759
_journal_page_last               6772
_journal_paper_doi               10.1039/b905023j
_journal_year                    2009
_chemical_formula_sum            'C4 H8 Br8 Nb2 O4'
_chemical_formula_weight         945.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6421(18)
_cell_length_b                   9.6914(13)
_cell_length_c                   13.9238(19)
_cell_measurement_reflns_used    3479
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.138
_cell_measurement_theta_min      2.578
_cell_volume                     1840.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11425
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    18.609
_exptl_absorpt_correction_T_max  0.2577
_exptl_absorpt_correction_T_min  0.1667
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.785
_refine_diff_density_min         -3.000
_refine_diff_density_rms         0.379
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0547
_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^)+(0.1043P)^2^+26.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                3184
_reflns_number_total             3580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905023j.txt
_cod_data_source_block           pca21
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7001933