#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:26:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179790 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/86/7008672.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_7008672
loop_
_publ_author_name
'Rosenthal, Esther C. E.'
'Cui, Huiling'
'Koch, Juliane'
'Escarpa Gaede, Petra'
'Hummert, Markus'
'Dechert, Sebastian'
_publ_section_title
;
 Chloride-bridged oxovanadium(V) complexes with alkoxyalkoxide ligands.
 Synthesis, structure, electrochemistry and reactivities.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3108
_journal_page_last               3117
_journal_paper_doi               10.1039/b505750g
_journal_year                    2005
_chemical_formula_sum            'C9 H19 Cl2 O4 V'
_chemical_formula_weight         313.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7037(4)
_cell_length_b                   17.0284(9)
_cell_length_c                   10.6692(5)
_cell_measurement_reflns_used    2622
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.32
_cell_volume                     1341.39(12)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       ω
_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  0.1031
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9092
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0639P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                1779
_reflns_number_total             2626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b505750g.txt
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P2(1)/n '
_cod_database_code               7008672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
C1 C 0.0411(5) 0.2289(2) 0.9072(4) 0.0190(8) Uani 1 1 d . . .
C2 C 0.2278(5) 0.2143(2) 1.0016(4) 0.0198(8) Uani 1 1 d . . .
H2A H 0.3092 0.2592 1.0013 0.024 Uiso 1 1 calc R . .
H2B H 0.2194 0.2067 1.0917 0.024 Uiso 1 1 calc R . .
C3 C 0.4685(5) 0.1226(3) 1.0406(4) 0.0294(10) Uani 1 1 d . . .
H3A H 0.5545 0.1656 1.0446 0.044 Uiso 1 1 calc R . .
H3B H 0.5118 0.0753 1.0068 0.044 Uiso 1 1 calc R . .
H3C H 0.4579 0.1122 1.1285 0.044 Uiso 1 1 calc R . .
C4 C -0.1014(5) 0.1724(3) 0.9268(4) 0.0286(10) Uani 1 1 d . . .
H4A H -0.2146 0.1800 0.8570 0.043 Uiso 1 1 calc R . .
H4B H -0.1225 0.1825 1.0117 0.043 Uiso 1 1 calc R . .
H4C H -0.0593 0.1183 0.9243 0.043 Uiso 1 1 calc R . .
C5 C -0.0148(6) 0.3144(3) 0.9168(4) 0.0311(10) Uani 1 1 d . . .
H5A H 0.0728 0.3493 0.8941 0.047 Uiso 1 1 calc R . .
H5B H -0.0178 0.3255 1.0063 0.047 Uiso 1 1 calc R . .
H5C H -0.1353 0.3232 0.8561 0.047 Uiso 1 1 calc R . .
C6 C -0.1259(5) 0.0626(3) 0.6259(4) 0.0250(9) Uani 1 1 d . . .
H6A H -0.1196 0.0745 0.5365 0.030 Uiso 1 1 calc R . .
H6B H -0.2049 0.1019 0.6507 0.030 Uiso 1 1 calc R . .
C7 C -0.1968(6) -0.0191(2) 0.6327(4) 0.0310(10) Uani 1 1 d . . .
H7A H -0.1621 -0.0547 0.5705 0.037 Uiso 1 1 calc R . .
H7B H -0.3302 -0.0193 0.6143 0.037 Uiso 1 1 calc R . .
C8 C -0.1043(6) -0.0424(3) 0.7735(4) 0.0323(10) Uani 1 1 d . . .
H8A H -0.1661 -0.0190 0.8342 0.039 Uiso 1 1 calc R . .
H8B H -0.1004 -0.1002 0.7843 0.039 Uiso 1 1 calc R . .
C9 C 0.0834(6) -0.0087(2) 0.7951(4) 0.0295(10) Uani 1 1 d . . .
H9A H 0.1403 0.0026 0.8890 0.035 Uiso 1 1 calc R . .
H9B H 0.1617 -0.0455 0.7642 0.035 Uiso 1 1 calc R . .
O1 O 0.1484(4) 0.17422(16) 0.5751(3) 0.0247(6) Uani 1 1 d . . .
O2 O 0.0566(3) 0.21767(15) 0.7761(2) 0.0184(6) Uani 1 1 d . . .
O3 O 0.2941(3) 0.14435(16) 0.9554(2) 0.0197(6) Uani 1 1 d . . .
O4 O 0.0550(3) 0.06317(16) 0.7189(3) 0.0229(6) Uani 1 1 d . . .
Cl2 Cl 0.44143(13) 0.06787(6) 0.73824(10) 0.0289(3) Uani 1 1 d . . .
Cl1 Cl 0.43569(13) 0.25878(6) 0.77267(10) 0.0281(3) Uani 1 1 d . . .
V1 V 0.22187(8) 0.16196(4) 0.72803(6) 0.01715(19) Uani 1 1 d . . .
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'
V V 0.3005 0.5294 '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
O2 C1 C4 108.1(3) . . ?
O2 C1 C2 107.1(3) . . ?
C4 C1 C2 113.0(3) . . ?
O2 C1 C5 107.0(3) . . ?
C4 C1 C5 111.4(3) . . ?
C2 C1 C5 110.0(3) . . ?
O3 C2 C1 105.6(3) . . ?
O4 C6 C7 105.2(3) . . ?
C6 C7 C8 102.4(3) . . ?
C9 C8 C7 102.1(3) . . ?
O4 C9 C8 104.5(3) . . ?
C1 O2 V1 127.7(2) . . ?
C2 O3 C3 110.8(3) . . ?
C2 O3 V1 104.2(2) . . ?
C3 O3 V1 126.1(2) . . ?
C9 O4 C6 109.7(3) . . ?
C9 O4 V1 131.0(2) . . ?
C6 O4 V1 119.2(2) . . ?
O1 V1 O2 98.77(13) . . ?
O1 V1 O4 91.37(13) . . ?
O2 V1 O4 87.78(11) . . ?
O1 V1 Cl1 98.31(11) . . ?
O2 V1 Cl1 95.05(9) . . ?
O4 V1 Cl1 169.37(8) . . ?
O1 V1 Cl2 100.49(11) . . ?
O2 V1 Cl2 158.78(9) . . ?
O4 V1 Cl2 82.94(8) . . ?
Cl1 V1 Cl2 90.92(4) . . ?
O1 V1 O3 173.03(12) . . ?
O2 V1 O3 75.39(10) . . ?
O4 V1 O3 84.67(10) . . ?
Cl1 V1 O3 86.13(7) . . ?
Cl2 V1 O3 84.74(7) . . ?
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
C1 O2 1.449(4) . ?
C1 C4 1.518(5) . ?
C1 C2 1.522(5) . ?
C1 C5 1.531(5) . ?
C2 O3 1.437(4) . ?
C3 O3 1.439(5) . ?
C6 O4 1.462(5) . ?
C6 C7 1.505(6) . ?
C7 C8 1.520(6) . ?
C8 C9 1.511(6) . ?
C9 O4 1.451(5) . ?
O1 V1 1.581(3) . ?
O2 V1 1.777(2) . ?
O3 V1 2.348(3) . ?
O4 V1 2.103(3) . ?
Cl2 V1 2.3096(12) . ?
Cl1 V1 2.2827(12) . ?
