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#$Date: 2017-03-04 04:04:19 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192967 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345425.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_4345425
loop_
_publ_author_name
'Schmidt, Anna-Corina'
'Hermsen, Marko'
'Rominger, Frank'
'Dehn, Richard'
'Teles, Joaquim Henrique'
'Schäfer, Ansgar'
'Trapp, Oliver'
'Schaub, Thomas'
_publ_section_title
;
 Synthesis of Mono- and Dinuclear Vanadium Complexes and Their Reactivity
 toward Dehydroperoxidation of Alkyl Hydroperoxides.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1319
_journal_page_last               1332
_journal_paper_doi               10.1021/acs.inorgchem.6b02322
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C13 H16 N O7 V'
_chemical_formula_weight         349.21
_chemical_name_common            '5 H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.1655(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9664(3)
_cell_length_b                   11.2735(4)
_cell_length_c                   8.8911(3)
_cell_measurement_reflns_used    2946
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.44
_cell_volume                     749.56(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4800
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.065
_diffrn_reflns_theta_max         25.065
_diffrn_reflns_theta_min         2.440
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1403
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0356P)²+0.5114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1293
_reflns_number_total             1403
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02322_si_002.cif
_cod_data_source_block           cos4
_cod_original_cell_volume        749.55(5)
_cod_database_code               4345425
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.986
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.73093(6) 0.7500 0.62573(6) 0.03032(18) Uani 1 2 d S T P . .
O1 O 0.9142(3) 0.7500 0.7714(3) 0.0517(7) Uani 1 2 d S T P A .
O2 O 0.4633(3) 0.7500 0.4318(2) 0.0266(4) Uani 1 2 d S T P A .
H2A H 0.452(3) 0.807(2) 0.378(3) 0.044(7) Uiso 1 1 d . . . . .
N1 N 0.5591(3) 0.7500 0.7571(3) 0.0236(5) Uani 1 2 d S T P A .
C2 C 0.5050(3) 0.64696(18) 0.7959(2) 0.0266(4) Uani 1 1 d . . . . .
C3 C 0.3925(3) 0.6435(2) 0.8844(2) 0.0336(5) Uani 1 1 d . . . . .
H3 H 0.3535 0.5700 0.9131 0.040 Uiso 1 1 calc R U . . .
C4 C 0.3384(4) 0.7500 0.9299(3) 0.0360(7) Uani 1 2 d S T P . .
H4 H 0.2634 0.7500 0.9929 0.043 Uiso 1 2 calc R U P . .
C5 C 0.5807(3) 0.5465(2) 0.7292(2) 0.0350(5) Uani 1 1 d . . . . .
O5 O 0.5553(3) 0.44368(14) 0.75758(19) 0.0518(5) Uani 1 1 d . . . . .
O6 O 0.6723(2) 0.58181(14) 0.64193(17) 0.0381(4) Uani 1 1 d . . . . .
O3 O 0.8067(3) 0.7341(15) 0.4634(3) 0.032(3) Uani 0.5 1 d D U P A -1
C11 C 0.9875(5) 0.7283(6) 0.4582(4) 0.0331(18) Uani 0.5 1 d D U P A -1
H11 H 1.0691 0.6901 0.5581 0.040 Uiso 0.5 1 calc R U P A -1
C12 C 1.0484(6) 0.8552(5) 0.4469(6) 0.0459(12) Uani 0.5 1 d D U P A -1
H12A H 1.0355 0.9023 0.5362 0.055 Uiso 0.5 1 calc R U P A -1
H12B H 1.1766 0.8546 0.4587 0.055 Uiso 0.5 1 calc R U P A -1
C13 C 0.9436(8) 0.9133(6) 0.2913(7) 0.0577(15) Uani 0.5 1 d D U P A -1
H13A H 0.9927 0.9934 0.2869 0.069 Uiso 0.5 1 calc R U P A -1
H13B H 0.8175 0.9223 0.2843 0.069 Uiso 0.5 1 calc R U P A -1
C14 C 0.9513(9) 0.8410(6) 0.1517(7) 0.0670(18) Uani 0.5 1 d D U P A -1
H14A H 1.0767 0.8361 0.1551 0.080 Uiso 0.5 1 calc R U P A -1
H14B H 0.8800 0.8805 0.0504 0.080 Uiso 0.5 1 calc R U P A -1
C15 C 0.8800(8) 0.7178(6) 0.1555(6) 0.060(2) Uani 0.5 1 d D U P A -1
H15A H 0.8912 0.6711 0.0651 0.072 Uiso 0.5 1 calc R U P A -1
H15B H 0.7515 0.7224 0.1422 0.072 Uiso 0.5 1 calc R U P A -1
C16 C 0.9818(8) 0.6549(6) 0.3137(7) 0.0478(13) Uani 0.5 1 d D U P A -1
H16A H 0.9234 0.5780 0.3172 0.057 Uiso 0.5 1 calc R U P A -1
H16B H 1.1055 0.6385 0.3183 0.057 Uiso 0.5 1 calc R U P A -1
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'
N N 0.0061 0.0033 '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'
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
O1 V1 O3 101.02(12) . .
O1 V1 O6 96.62(5) . .
O3 V1 O6 96.9(6) . .
O1 V1 O6 96.62(5) . 4_575
O3 V1 O6 108.4(6) . 4_575
O6 V1 O6 148.53(9) . 4_575
O1 V1 N1 98.07(10) . .
O3 V1 N1 160.01(19) . .
O6 V1 N1 74.98(4) . .
O6 V1 N1 74.98(4) 4_575 .
O1 V1 O2 176.28(10) . .
O3 V1 O2 82.67(10) . .
O6 V1 O2 82.48(5) . .
O6 V1 O2 82.48(5) 4_575 .
N1 V1 O2 78.21(8) . .
V1 O2 H2A 110.3(19) . .
C2 N1 C2 122.5(2) 4_575 .
C2 N1 V1 118.75(12) 4_575 .
C2 N1 V1 118.75(12) . .
N1 C2 C3 120.36(19) . .
N1 C2 C5 110.40(18) . .
C3 C2 C5 129.2(2) . .
C2 C3 C4 118.1(2) . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
C3 C4 C3 120.5(3) . 4_575
C3 C4 H4 119.7 . .
C3 C4 H4 119.7 4_575 .
O5 C5 O6 125.7(2) . .
O5 C5 C2 121.3(2) . .
O6 C5 C2 113.02(18) . .
C5 O6 V1 122.37(14) . .
C11 O3 V1 130.8(2) . .
O3 C11 C16 108.1(5) . .
O3 C11 C12 107.4(8) . .
C16 C11 C12 111.9(4) . .
O3 C11 H11 109.8 . .
C16 C11 H11 109.8 . .
C12 C11 H11 109.8 . .
C13 C12 C11 112.5(4) . .
C13 C12 H12A 109.1 . .
C11 C12 H12A 109.1 . .
C13 C12 H12B 109.1 . .
C11 C12 H12B 109.1 . .
H12A C12 H12B 107.8 . .
C12 C13 C14 110.9(5) . .
C12 C13 H13A 109.5 . .
C14 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
C13 C14 C15 111.0(5) . .
C13 C14 H14A 109.4 . .
C15 C14 H14A 109.4 . .
C13 C14 H14B 109.4 . .
C15 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
C14 C15 C16 111.3(5) . .
C14 C15 H15A 109.4 . .
C16 C15 H15A 109.4 . .
C14 C15 H15B 109.4 . .
C16 C15 H15B 109.4 . .
H15A C15 H15B 108.0 . .
C11 C16 C15 112.2(5) . .
C11 C16 H16A 109.2 . .
C15 C16 H16A 109.2 . .
C11 C16 H16B 109.2 . .
C15 C16 H16B 109.2 . .
H16A C16 H16B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.583(2) .
V1 O3 1.755(3) .
V1 O6 1.9699(16) .
V1 O6 1.9699(16) 4_575
V1 N1 2.084(2) .
V1 O2 2.232(2) .
O2 H2A 0.79(2) .
N1 C2 1.325(2) 4_575
N1 C2 1.325(2) .
C2 C3 1.382(3) .
C2 C5 1.498(3) .
C3 C4 1.383(3) .
C3 H3 0.9500 .
C4 C3 1.383(3) 4_575
C4 H4 0.9500 .
C5 O5 1.218(3) .
C5 O6 1.297(3) .
O3 C11 1.458(5) .
C11 C16 1.516(7) .
C11 C12 1.525(8) .
C11 H11 1.0000 .
C12 C13 1.498(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.504(8) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.505(8) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.533(7) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
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_4
C2 N1 C2 C3 -2.1(4) 4_575 .
V1 N1 C2 C3 179.33(15) . .
C2 N1 C2 C5 177.15(17) 4_575 .
V1 N1 C2 C5 -1.4(2) . .
N1 C2 C3 C4 0.3(3) . .
C5 C2 C3 C4 -178.8(2) . .
C2 C3 C4 C3 1.5(4) . 4_575
N1 C2 C5 O5 176.2(2) . .
C3 C2 C5 O5 -4.6(3) . .
N1 C2 C5 O6 -3.7(3) . .
C3 C2 C5 O6 175.46(19) . .
O5 C5 O6 V1 -172.06(18) . .
C2 C5 O6 V1 7.9(2) . .
O1 V1 O3 C11 -2.8(15) . .
O6 V1 O3 C11 -100.9(14) . .
O6 V1 O3 C11 98.1(14) 4_575 .
N1 V1 O3 C11 -165.3(4) . .
O2 V1 O3 C11 177.6(15) . .
V1 O3 C11 C16 151.4(12) . .
V1 O3 C11 C12 -87.6(14) . .
O3 C11 C12 C13 -66.8(5) . .
C16 C11 C12 C13 51.7(6) . .
C11 C12 C13 C14 -55.7(6) . .
C12 C13 C14 C15 58.4(6) . .
C13 C14 C15 C16 -56.8(7) . .
O3 C11 C16 C15 68.4(8) . .
C12 C11 C16 C15 -49.8(6) . .
C14 C15 C16 C11 52.8(7) . .
