#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:14:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179717 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/19/7001933.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7001933
loop_
_publ_author_name
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_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/[σ²(Fo²)+(0.1043P)²+26.5580P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.12179(14) 0.8388(2) 0.86634(14) 0.0263(4) Uani 1 1 d . . .
Br2 Br 0.91471(15) 1.03905(19) 0.91199(13) 0.0249(4) Uani 1 1 d . . .
Br3 Br 0.81300(15) 0.9215(2) 0.69488(17) 0.0316(5) Uani 1 1 d U . .
Br4 Br 1.02782(17) 0.7354(2) 0.65345(18) 0.0381(5) Uani 1 1 d U . .
Br5 Br 1.04629(15) 1.0929(2) 0.68955(16) 0.0293(5) Uani 1 1 d U . .
Br6 Br 0.96301(15) 0.4087(2) 0.81834(17) 0.0296(5) Uani 1 1 d U . .
Br7 Br 0.94512(16) 0.6057(2) 1.04079(15) 0.0323(5) Uani 1 1 d U . .
Br8 Br 0.72252(14) 0.5414(2) 0.77502(16) 0.0323(5) Uani 1 1 d U . .
Nb1 Nb 0.97496(10) 0.90190(14) 0.77307(10) 0.0079(3) Uani 1 1 d U . .
Nb2 Nb 0.85824(10) 0.57770(13) 0.88912(10) 0.0077(3) Uani 1 1 d U . .
C1 C 0.6904(13) 0.8082(16) 0.9326(12) 0.015(3) Uani 1 1 d U . .
H1A H 0.7358 0.8585 0.8932 0.022 Uiso 1 1 calc R . .
H1B H 0.6704 0.8648 0.9857 0.022 Uiso 1 1 calc R . .
H1C H 0.6340 0.7833 0.8951 0.022 Uiso 1 1 calc R . .
C2 C 0.6714(12) 0.6060(17) 1.0280(12) 0.011(2) Uani 1 1 d U . .
H2A H 0.6061 0.6046 1.0004 0.013 Uiso 1 1 calc R . .
H2B H 0.6676 0.6462 1.0917 0.013 Uiso 1 1 calc R . .
C3 C 0.7128(12) 0.4601(17) 1.0335(11) 0.012(2) Uani 1 1 d U . .
C4 C 0.7000(11) 0.2464(16) 1.1110(12) 0.012(3) Uani 1 1 d U . .
H4A H 0.6617 0.2047 1.1611 0.017 Uiso 1 1 calc R . .
H4B H 0.7680 0.2450 1.1288 0.017 Uiso 1 1 calc R . .
H4C H 0.6911 0.1957 1.0524 0.017 Uiso 1 1 calc R . .
O1 O 0.9024(8) 0.7308(11) 0.8390(8) 0.0138(17) Uani 1 1 d U . .
O2 O 0.7370(8) 0.6854(11) 0.9682(8) 0.0126(17) Uani 1 1 d U . .
O3 O 0.7767(9) 0.4247(11) 0.9772(9) 0.0187(18) Uani 1 1 d U . .
O4 O 0.6683(8) 0.3887(11) 1.0972(8) 0.012(2) Uani 1 1 d U . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 Br5 175.4(3) . . ?
O1 Nb1 Br4 85.2(3) . . ?
Br5 Nb1 Br4 93.44(9) . . ?
O1 Nb1 Br1 87.6(3) . . ?
Br5 Nb1 Br1 96.75(8) . . ?
Br4 Nb1 Br1 87.42(9) . . ?
O1 Nb1 Br3 80.5(3) . . ?
Br5 Nb1 Br3 95.16(9) . . ?
Br4 Nb1 Br3 90.83(9) . . ?
Br1 Nb1 Br3 168.04(9) . . ?
O1 Nb1 Br2 85.9(3) . . ?
Br5 Nb1 Br2 95.68(8) . . ?
Br4 Nb1 Br2 170.66(10) . . ?
Br1 Nb1 Br2 89.51(8) . . ?
Br3 Nb1 Br2 90.34(9) . . ?
O1 Nb2 O3 163.7(5) . . ?
O1 Nb2 O2 93.2(5) . . ?
O3 Nb2 O2 70.8(4) . . ?
O1 Nb2 Br6 102.2(4) . . ?
O3 Nb2 Br6 94.0(3) . . ?
O2 Nb2 Br6 164.3(3) . . ?
O1 Nb2 Br7 94.8(4) . . ?
O3 Nb2 Br7 80.8(4) . . ?
O2 Nb2 Br7 83.2(3) . . ?
Br6 Nb2 Br7 98.22(9) . . ?
O1 Nb2 Br8 97.1(4) . . ?
O3 Nb2 Br8 83.4(4) . . ?
O2 Nb2 Br8 80.1(3) . . ?
Br6 Nb2 Br8 94.92(9) . . ?
Br7 Nb2 Br8 160.02(10) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C3 107.1(12) . . ?
O2 C2 H2A 110.3 . . ?
C3 C2 H2A 110.3 . . ?
O2 C2 H2B 110.3 . . ?
C3 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
O3 C3 O4 129.1(15) . . ?
O3 C3 C2 119.6(14) . . ?
O4 C3 C2 111.2(14) . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Nb2 O1 Nb1 171.8(7) . . ?
C1 O2 C2 111.5(12) . . ?
C1 O2 Nb2 122.8(9) . . ?
C2 O2 Nb2 119.5(9) . . ?
C3 O3 Nb2 121.6(10) . . ?
C3 O4 C4 117.7(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Nb1 2.464(2) . ?
Br2 Nb1 2.487(2) . ?
Br3 Nb1 2.470(2) . ?
Br4 Nb1 2.429(3) . ?
Br5 Nb1 2.392(2) . ?
Br6 Nb2 2.387(2) . ?
Br7 Nb2 2.437(3) . ?
Br8 Nb2 2.465(2) . ?
Nb1 O1 2.138(11) . ?
Nb2 O1 1.747(11) . ?
Nb2 O3 2.222(12) . ?
Nb2 O2 2.244(11) . ?
C1 O2 1.437(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O2 1.444(19) . ?
C2 C3 1.52(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O3 1.22(2) . ?
C3 O4 1.28(2) . ?
C4 O4 1.458(19) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C2 C3 O3 -14(2) . . . . ?
O2 C2 C3 O4 169.5(13) . . . . ?
O3 Nb2 O1 Nb1 154(4) . . . . ?
O2 Nb2 O1 Nb1 164(5) . . . . ?
Br6 Nb2 O1 Nb1 -19(5) . . . . ?
Br7 Nb2 O1 Nb1 81(5) . . . . ?
Br8 Nb2 O1 Nb1 -115(5) . . . . ?
Br5 Nb1 O1 Nb2 115(5) . . . . ?
Br4 Nb1 O1 Nb2 42(5) . . . . ?
Br1 Nb1 O1 Nb2 -46(5) . . . . ?
Br3 Nb1 O1 Nb2 134(5) . . . . ?
Br2 Nb1 O1 Nb2 -135(5) . . . . ?
C3 C2 O2 C1 161.1(13) . . . . ?
C3 C2 O2 Nb2 8.1(16) . . . . ?
O1 Nb2 O2 C1 31.1(12) . . . . ?
O3 Nb2 O2 C1 -151.9(13) . . . . ?
Br6 Nb2 O2 C1 -138.2(11) . . . . ?
Br7 Nb2 O2 C1 125.6(12) . . . . ?
Br8 Nb2 O2 C1 -65.5(11) . . . . ?
O1 Nb2 O2 C2 -179.1(11) . . . . ?
O3 Nb2 O2 C2 -2.0(10) . . . . ?
Br6 Nb2 O2 C2 11.7(19) . . . . ?
Br7 Nb2 O2 C2 -84.6(10) . . . . ?
Br8 Nb2 O2 C2 84.3(10) . . . . ?
O4 C3 O3 Nb2 -170.2(13) . . . . ?
C2 C3 O3 Nb2 14(2) . . . . ?
O1 Nb2 O3 C3 4(3) . . . . ?
O2 Nb2 O3 C3 -6.7(13) . . . . ?
Br6 Nb2 O3 C3 177.0(13) . . . . ?
Br7 Nb2 O3 C3 79.3(13) . . . . ?
Br8 Nb2 O3 C3 -88.5(14) . . . . ?
O3 C3 O4 C4 4(3) . . . . ?
C2 C3 O4 C4 -179.9(13) . . . . ?
