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#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004679.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_7004679
loop_
_publ_author_name
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 Unusual room temperature activation of 1,2-dialkoxyalkanes by niobium
 and tantalum pentachlorides
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              7026
_journal_page_last               7035
_journal_paper_doi               10.1039/b810210d
_journal_year                    2008
_chemical_formula_sum            'C4 H10 Cl8 Nb2 O3'
_chemical_formula_weight         575.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   7.0287(5)
_cell_length_b                   13.5297(9)
_cell_length_c                   17.5555(12)
_cell_measurement_reflns_used    7726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6855
_cell_measurement_theta_min      2.320
_cell_volume                     1669.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9274
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.6067
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0138
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0129P)²+0.2996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0327
_reflns_number_gt                3496
_reflns_number_total             3564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b810210d.txt
_cod_data_source_block           p212121
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7004679
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
Nb1 Nb 0.62536(3) 0.095614(14) 0.162928(9) 0.01085(4) Uani 1 1 d . . .
Nb2 Nb 0.50147(3) -0.043362(14) -0.023167(9) 0.01226(5) Uani 1 1 d . . .
Cl1 Cl 0.76334(8) 0.02220(4) -0.08677(3) 0.02156(12) Uani 1 1 d . . .
Cl2 Cl 0.40627(8) -0.13701(4) -0.12403(3) 0.02091(12) Uani 1 1 d . . .
Cl3 Cl 0.32875(8) 0.09778(4) -0.05762(3) 0.02228(12) Uani 1 1 d . . .
Cl4 Cl 0.24364(8) -0.08872(4) 0.05269(3) 0.01745(11) Uani 1 1 d . . .
Cl5 Cl 0.69029(8) -0.16421(4) 0.03118(3) 0.02129(12) Uani 1 1 d . . .
Cl6 Cl 0.45264(7) 0.24004(4) 0.13461(3) 0.01709(11) Uani 1 1 d . . .
Cl7 Cl 0.85620(9) -0.01550(4) 0.20671(3) 0.02028(12) Uani 1 1 d . . .
Cl8 Cl 0.38388(8) 0.02300(4) 0.23043(3) 0.01978(12) Uani 1 1 d . . .
O1 O 0.5906(2) 0.04163(11) 0.07292(8) 0.0149(3) Uani 1 1 d . . .
O2 O 0.8701(2) 0.18427(11) 0.13211(8) 0.0131(3) Uani 1 1 d . . .
O3 O 0.7071(2) 0.18824(11) 0.26708(8) 0.0139(3) Uani 1 1 d . . .
C1 C 0.9965(3) 0.15407(17) 0.07020(11) 0.0189(5) Uani 1 1 d . . .
H1A H 1.0671 0.2117 0.0516 0.028 Uiso 1 1 calc R . .
H1B H 0.9209 0.1260 0.0286 0.028 Uiso 1 1 calc R . .
H1C H 1.0862 0.1042 0.0890 0.028 Uiso 1 1 calc R . .
C2 C 0.9736(3) 0.23320(16) 0.19304(11) 0.0147(4) Uani 1 1 d . . .
H2A H 1.0503 0.2884 0.1724 0.018 Uiso 1 1 calc R . .
H2B H 1.0602 0.1860 0.2186 0.018 Uiso 1 1 calc R . .
C3 C 0.8292(3) 0.27122(16) 0.24813(12) 0.0157(5) Uani 1 1 d . . .
H3A H 0.8923 0.2970 0.2945 0.019 Uiso 1 1 calc R . .
H3B H 0.7539 0.3252 0.2248 0.019 Uiso 1 1 calc R . .
C4 C 0.5761(3) 0.21431(18) 0.32779(12) 0.0202(5) Uani 1 1 d . . .
H4A H 0.6480 0.2385 0.3718 0.030 Uiso 1 1 calc R . .
H4B H 0.5024 0.1559 0.3426 0.030 Uiso 1 1 calc R . .
H4C H 0.4895 0.2661 0.3100 0.030 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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 O2 96.67(6) . . ?
O1 Nb1 O3 168.53(6) . . ?
O2 Nb1 O3 72.37(5) . . ?
O1 Nb1 Cl8 100.58(5) . . ?
O2 Nb1 Cl8 162.75(4) . . ?
O3 Nb1 Cl8 90.43(4) . . ?
O1 Nb1 Cl7 97.17(5) . . ?
O2 Nb1 Cl7 83.52(4) . . ?
O3 Nb1 Cl7 85.15(4) . . ?
Cl8 Nb1 Cl7 93.91(2) . . ?
O1 Nb1 Cl6 94.78(5) . . ?
O2 Nb1 Cl6 84.10(4) . . ?
O3 Nb1 Cl6 81.01(4) . . ?
Cl8 Nb1 Cl6 94.77(2) . . ?
Cl7 Nb1 Cl6 163.69(2) . . ?
O1 Nb2 Cl2 178.76(4) . . ?
O1 Nb2 Cl5 83.48(4) . . ?
Cl2 Nb2 Cl5 95.51(2) . . ?
O1 Nb2 Cl1 86.67(4) . . ?
Cl2 Nb2 Cl1 94.09(2) . . ?
Cl5 Nb2 Cl1 90.78(2) . . ?
O1 Nb2 Cl4 85.32(4) . . ?
Cl2 Nb2 Cl4 93.97(2) . . ?
Cl5 Nb2 Cl4 91.39(2) . . ?
Cl1 Nb2 Cl4 171.41(2) . . ?
O1 Nb2 Cl3 85.23(4) . . ?
Cl2 Nb2 Cl3 95.77(2) . . ?
Cl5 Nb2 Cl3 168.71(2) . . ?
Cl1 Nb2 Cl3 88.58(2) . . ?
Cl4 Nb2 Cl3 87.66(2) . . ?
Nb1 O1 Nb2 167.07(9) . . ?
C2 O2 C1 111.77(16) . . ?
C2 O2 Nb1 117.76(11) . . ?
C1 O2 Nb1 120.90(12) . . ?
C3 O3 C4 110.80(16) . . ?
C3 O3 Nb1 112.86(11) . . ?
C4 O3 Nb1 124.07(13) . . ?
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 107.09(17) . . ?
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 C2 106.48(17) . . ?
O3 C3 H3A 110.4 . . ?
C2 C3 H3A 110.4 . . ?
O3 C3 H3B 110.4 . . ?
C2 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
O3 C4 H4A 109.5 . . ?
O3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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
Nb1 O1 1.7579(14) . ?
Nb1 O2 2.1661(15) . ?
Nb1 O3 2.2898(14) . ?
Nb1 Cl8 2.2913(6) . ?
Nb1 Cl7 2.3417(6) . ?
Nb1 Cl6 2.3536(6) . ?
Nb2 O1 2.1353(14) . ?
Nb2 Cl2 2.2778(6) . ?
Nb2 Cl5 2.3120(6) . ?
Nb2 Cl1 2.3284(6) . ?
Nb2 Cl4 2.3311(6) . ?
Nb2 Cl3 2.3423(6) . ?
O2 C2 1.453(2) . ?
O2 C1 1.462(2) . ?
O3 C3 1.452(3) . ?
O3 C4 1.452(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.493(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 Nb1 O1 Nb2 173.0(4) . . . . ?
O3 Nb1 O1 Nb2 -170.2(2) . . . . ?
Cl8 Nb1 O1 Nb2 -6.6(4) . . . . ?
Cl7 Nb1 O1 Nb2 88.7(4) . . . . ?
Cl6 Nb1 O1 Nb2 -102.4(4) . . . . ?
Cl2 Nb2 O1 Nb1 -42(2) . . . . ?
Cl5 Nb2 O1 Nb1 -77.9(4) . . . . ?
Cl1 Nb2 O1 Nb1 -169.1(4) . . . . ?
Cl4 Nb2 O1 Nb1 14.0(4) . . . . ?
Cl3 Nb2 O1 Nb1 102.0(4) . . . . ?
O1 Nb1 O2 C2 -170.44(14) . . . . ?
O3 Nb1 O2 C2 13.01(13) . . . . ?
Cl8 Nb1 O2 C2 8.3(2) . . . . ?
Cl7 Nb1 O2 C2 -73.94(14) . . . . ?
Cl6 Nb1 O2 C2 95.42(14) . . . . ?
O1 Nb1 O2 C1 -26.98(15) . . . . ?
O3 Nb1 O2 C1 156.46(15) . . . . ?
Cl8 Nb1 O2 C1 151.79(13) . . . . ?
Cl7 Nb1 O2 C1 69.51(14) . . . . ?
Cl6 Nb1 O2 C1 -121.12(14) . . . . ?
O1 Nb1 O3 C3 0.0(4) . . . . ?
O2 Nb1 O3 C3 17.53(13) . . . . ?
Cl8 Nb1 O3 C3 -163.85(13) . . . . ?
Cl7 Nb1 O3 C3 102.26(13) . . . . ?
Cl6 Nb1 O3 C3 -69.09(13) . . . . ?
O1 Nb1 O3 C4 138.7(3) . . . . ?
O2 Nb1 O3 C4 156.15(16) . . . . ?
Cl8 Nb1 O3 C4 -25.23(15) . . . . ?
Cl7 Nb1 O3 C4 -119.12(15) . . . . ?
Cl6 Nb1 O3 C4 69.53(15) . . . . ?
C1 O2 C2 C3 173.36(17) . . . . ?
Nb1 O2 C2 C3 -40.0(2) . . . . ?
C4 O3 C3 C2 172.79(16) . . . . ?
Nb1 O3 C3 C2 -43.07(19) . . . . ?
O2 C2 C3 O3 52.1(2) . . . . ?
