#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:17:43 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258848 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705448.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_7705448
loop_
_publ_author_name
'Li, Jikun'
'Wei, Chuanping'
'Guo, Daigaojie'
'Wang, Congcong'
'Han, Yinfeng'
'He, Guofang'
'Zhang, Jianping'
'Huang, Xianqiang'
'Hu, Changwen'
_publ_section_title
;
Inorganic-organic hybrid polyoxovanadates based on
[V4O12]4- or
[VO3]22- clusters: controllable
synthesis, crystal structures and catalytic properties in selective
oxidation of sulfides.
;
_journal_issue 40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 14148
_journal_page_last 14157
_journal_paper_doi 10.1039/d0dt03015e
_journal_volume 49
_journal_year 2020
_chemical_formula_moiety 'C5 H8 Co N2 O7 V2'
_chemical_formula_sum 'C5 H8 Co N2 O7 V2'
_chemical_formula_weight 368.94
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2014/7
_audit_update_record
;
2020-08-06 deposited with the CCDC. 2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 98.297(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.057(3)
_cell_length_b 5.8528(14)
_cell_length_c 15.556(4)
_cell_measurement_reflns_used 3854
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.36
_cell_measurement_theta_min 2.65
_cell_volume 1086.3(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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature 298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0212
_diffrn_reflns_av_unetI/netI 0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 6077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.497
_diffrn_reflns_theta_min 1.707
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 3.218
_exptl_absorpt_correction_T_max 0.702
_exptl_absorpt_correction_T_min 0.566
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details sadabs
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.256
_exptl_crystal_description block
_exptl_crystal_F_000 724
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.331
_refine_diff_density_min -0.260
_refine_diff_density_rms 0.069
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.306
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 154
_refine_ls_number_reflns 2020
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.306
_refine_ls_R_factor_all 0.0231
_refine_ls_R_factor_gt 0.0200
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0568
_refine_ls_wR_factor_ref 0.0586
_reflns_Friedel_coverage 0.000
_reflns_number_gt 1850
_reflns_number_total 2020
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0dt03015e2.cif
_cod_data_source_block 1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705447--7705449.cif.'
_cod_original_cell_volume 1086.2(4)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 7705448
_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 0.595
_shelx_estimated_absorpt_t_max 0.718
_shelx_res_file
;
1.res created by SHELXL-2014/7
TITL 1 in P2(1)/c
CELL 0.71073 12.0567 5.8528 15.5557 90.000 98.297 90.000
ZERR 4.00 0.0028 0.0014 0.0036 0.000 0.004 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H N O V Co
UNIT 20 32 8 28 8 4
OMIT -3 51
L.S. 8
ACTA
BOND $h
FMAP 2
PLAN 20
HTAB C5 O3_$4
HTAB C3 O7
HTAB C2 O3_$4
HTAB C1 O4_$3
HTAB O7 O6_$2
HTAB O7 O6_$1
HTAB C5 O3_$4
HTAB C3 O7
HTAB C2 O3_$4
HTAB C1 O4_$3
HTAB O7 O6_$2
HTAB O7 O6_$1
HTAB C5 O3_$4
HTAB C3 O7
HTAB C2 O3_$4
HTAB C1 O4_$3
HTAB O7 O6_$2
HTAB O7 O6_$1
HTAB C5 O3_$4
HTAB C3 O7
HTAB C2 O3_$4
HTAB C1 O4_$3
HTAB O7 O6_$2
HTAB O7 O6_$1
HTAB C5 O3_$4
HTAB C3 O7
HTAB C2 O3_$4
EQIV $4 x+1, y+1, z
HTAB C1 O4_$3
EQIV $3 -x, y+1/2, -z+1/2
HTAB O7 O6_$2
EQIV $2 x, y+1, z
HTAB O7 O6_$1
EQIV $1 -x, -y+2, -z+1
size 0.18 0.15 0.11
htab
conf
HTAB O7 O6_$1
HTAB O7 O6_$2
HTAB C1 O4_$3
HTAB C2 O3_$4
HTAB C3 O7
HTAB C5 O3_$4
HTAB O7 O6_$1
HTAB O7 O6_$2
HTAB C1 O4_$3
HTAB C2 O3_$4
HTAB C3 O7
HTAB C5 O3_$4
HTAB O7 O6_$1
HTAB O7 O6_$2
HTAB C1 O4_$3
HTAB C2 O3_$4
HTAB C3 O7
HTAB C5 O3_$4
HTAB O7 O6_$1
HTAB O7 O6_$2
HTAB C1 O4_$3
HTAB C2 O3_$4
HTAB C3 O7
HTAB C5 O3_$4
TEMP 0.000
WGHT 0.027400 0.001000
FVAR 0.43409
MOLE 1
CO1 6 0.078344 1.014816 0.425670 11.00000 0.01176 0.01404 =
0.01025 0.00065 0.00198 0.00042
V1 5 -0.186097 0.145283 0.359551 11.00000 0.01202 0.00886 =
0.01317 0.00125 -0.00047 0.00019
V2 5 -0.093927 0.663452 0.290493 11.00000 0.01505 0.00918 =
0.00926 -0.00003 0.00093 -0.00003
O1 4 -0.172630 0.418701 0.307931 11.00000 0.01969 0.01215 =
0.02175 0.00416 0.00070 -0.00128
O2 4 -0.086775 0.100290 0.447865 11.00000 0.01382 0.01513 =
0.01361 0.00071 0.00260 0.00209
O3 4 -0.305867 0.143445 0.391598 11.00000 0.01592 0.02696 =
0.02832 0.00519 0.00389 0.00104
O4 4 -0.184022 -0.094777 0.286977 11.00000 0.02115 0.01186 =
0.01691 -0.00166 -0.00419 0.00170
O5 4 -0.041346 0.646997 0.198387 11.00000 0.02400 0.02113 =
0.01396 -0.00301 0.00460 -0.00300
O6 4 0.007990 0.696090 0.374780 11.00000 0.01987 0.01273 =
0.01551 -0.00205 -0.00085 0.00079
O7 4 0.123756 1.351141 0.473752 11.00000 0.02628 0.01660 =
0.02234 -0.00043 0.00225 0.00335
AFIX 3
H7A 2 0.099582 1.369653 0.521970 11.00000 -1.20000
H7B 2 0.090952 1.455657 0.441694 11.00000 -1.20000
AFIX 0
N1 3 0.240053 0.943560 0.409603 11.00000 0.01415 0.02248 =
0.01714 0.00083 0.00167 0.00112
N2 3 0.388466 0.781771 0.367814 11.00000 0.01568 0.02394 =
0.02898 0.00101 0.00677 0.00368
C1 1 0.278815 0.759721 0.375839 11.00000 0.01640 0.02403 =
0.02153 0.00097 0.00349 -0.00190
AFIX 43
H1 2 0.236147 0.630361 0.359469 11.00000 -1.20000
AFIX 0
C2 1 0.420895 0.995791 0.398553 11.00000 0.01808 0.02838 =
0.04056 -0.00324 0.00856 -0.00518
AFIX 43
H2 2 0.491759 1.060481 0.401181 11.00000 -1.20000
AFIX 0
C3 1 0.330096 1.092587 0.423965 11.00000 0.02178 0.02308 =
0.03672 -0.00775 0.00638 -0.00336
AFIX 43
H3 2 0.327933 1.238089 0.447693 11.00000 -1.20000
AFIX 0
C4 1 0.453602 0.611756 0.333310 11.00000 0.03102 0.02373 =
0.04447 -0.00155 0.01247 0.00671
AFIX 43
H4 2 0.417178 0.481597 0.309346 11.00000 -1.20000
AFIX 0
C5 1 0.561552 0.627404 0.333250 11.00000 0.03002 0.04124 =
0.06780 -0.00321 0.01990 0.01224
AFIX 93
H5A 2 0.600237 0.755577 0.356768 11.00000 -1.20000
H5B 2 0.599804 0.510383 0.309688 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1 in P2(1)/c
REM R1 = 0.0200 for 1850 Fo > 4sig(Fo) and 0.0231 for all 2020 data
REM 154 parameters refined using 0 restraints
END
WGHT 0.0279 0.7922
REM Instructions for potential hydrogen bonds
HTAB O7 O6_$1
HTAB O7 O6_$2
HTAB C1 O4_$3
HTAB C2 O3_$4
HTAB C3 O7
HTAB C5 O3_$4
REM Highest difference peak 0.331, deepest hole -0.260, 1-sigma level 0.069
Q1 1 -0.0399 0.6191 0.3577 11.00000 0.05 0.33
Q2 1 0.1826 0.9821 0.4191 11.00000 0.05 0.32
Q3 1 0.2732 1.0180 0.4199 11.00000 0.05 0.32
Q4 1 -0.1643 0.3765 0.3444 11.00000 0.05 0.30
Q5 1 -0.1000 -0.0029 0.4126 11.00000 0.05 0.29
Q6 1 -0.2931 0.1508 0.3449 11.00000 0.05 0.27
Q7 1 -0.0209 0.7746 0.3374 11.00000 0.05 0.26
Q8 1 -0.1265 -0.1318 0.3015 11.00000 0.05 0.26
Q9 1 -0.1404 0.1636 0.4263 11.00000 0.05 0.26
Q10 1 -0.1884 -0.0445 0.2640 11.00000 0.05 0.25
Q11 1 -0.1168 0.4705 0.3015 11.00000 0.05 0.24
Q12 1 0.0439 0.6702 0.3619 11.00000 0.05 0.23
Q13 1 0.3307 0.7712 0.3610 11.00000 0.05 0.23
Q14 1 -0.2030 0.3918 0.2989 11.00000 0.05 0.23
Q15 1 0.3790 1.0196 0.4280 11.00000 0.05 0.23
Q16 1 0.4028 0.8914 0.3838 11.00000 0.05 0.23
Q17 1 0.0061 0.8174 0.3791 11.00000 0.05 0.23
Q18 1 0.4102 0.8655 0.4025 11.00000 0.05 0.22
Q19 1 -0.1026 0.6592 0.2196 11.00000 0.05 0.22
Q20 1 0.2434 0.9275 0.3737 11.00000 0.05 0.22
;
_shelx_res_checksum 88309
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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
Co1 Co 0.07834(2) 1.01482(5) 0.42567(2) 0.01198(10) Uani 1 1 d . . . . .
V1 V -0.18610(3) 0.14528(6) 0.35955(2) 0.01158(11) Uani 1 1 d . . . . .
V2 V -0.09393(3) 0.66345(6) 0.29049(2) 0.01125(11) Uani 1 1 d . . . . .
O1 O -0.17263(13) 0.4187(3) 0.30793(10) 0.0181(3) Uani 1 1 d . . . . .
O2 O -0.08677(12) 0.1003(3) 0.44786(9) 0.0141(3) Uani 1 1 d . . . . .
O3 O -0.30587(13) 0.1434(3) 0.39160(11) 0.0237(4) Uani 1 1 d . . . . .
O4 O -0.18402(13) -0.0948(3) 0.28698(10) 0.0173(3) Uani 1 1 d . . . . .
O5 O -0.04135(14) 0.6470(3) 0.19839(10) 0.0195(4) Uani 1 1 d . . . . .
O6 O 0.00799(13) 0.6961(2) 0.37478(10) 0.0164(3) Uani 1 1 d . . . . .
O7 O 0.12376(14) 1.3511(3) 0.47375(11) 0.0219(4) Uani 1 1 d . . . . .
H7A H 0.0996 1.3697 0.5220 0.026 Uiso 1 1 d R U . . .
H7B H 0.0910 1.4557 0.4417 0.026 Uiso 1 1 d R U . . .
N1 N 0.24005(16) 0.9436(3) 0.40960(12) 0.0180(4) Uani 1 1 d . . . . .
N2 N 0.38847(17) 0.7818(4) 0.36781(13) 0.0225(5) Uani 1 1 d . . . . .
C1 C 0.2788(2) 0.7597(4) 0.37584(15) 0.0206(5) Uani 1 1 d . . . . .
H1 H 0.2361 0.6304 0.3595 0.025 Uiso 1 1 calc R U . . .
C2 C 0.4209(2) 0.9958(4) 0.39855(18) 0.0286(6) Uani 1 1 d . . . . .
H2 H 0.4918 1.0605 0.4012 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3301(2) 1.0926(5) 0.42397(17) 0.0270(6) Uani 1 1 d . . . . .
H3 H 0.3279 1.2381 0.4477 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4536(2) 0.6118(5) 0.33331(19) 0.0324(7) Uani 1 1 d . . . . .
H4 H 0.4172 0.4816 0.3093 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5616(3) 0.6274(5) 0.3332(2) 0.0451(8) Uani 1 1 d . . . . .
H5A H 0.6002 0.7556 0.3568 0.054 Uiso 1 1 calc R U . . .
H5B H 0.5998 0.5104 0.3097 0.054 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01176(17) 0.01404(18) 0.01025(17) 0.00065(11) 0.00198(12) 0.00042(12)
V1 0.0120(2) 0.0089(2) 0.0132(2) 0.00125(13) -0.00047(15) 0.00019(14)
V2 0.0151(2) 0.0092(2) 0.0093(2) -0.00003(13) 0.00093(15) -0.00003(15)
O1 0.0197(8) 0.0122(8) 0.0218(9) 0.0042(7) 0.0007(7) -0.0013(7)
O2 0.0138(8) 0.0151(8) 0.0136(8) 0.0007(6) 0.0026(6) 0.0021(7)
O3 0.0159(9) 0.0270(10) 0.0283(10) 0.0052(7) 0.0039(7) 0.0010(7)
O4 0.0212(8) 0.0119(8) 0.0169(8) -0.0017(6) -0.0042(7) 0.0017(7)
O5 0.0240(9) 0.0211(9) 0.0140(8) -0.0030(6) 0.0046(7) -0.0030(7)
O6 0.0199(8) 0.0127(8) 0.0155(8) -0.0020(6) -0.0008(7) 0.0008(7)
O7 0.0263(9) 0.0166(9) 0.0223(9) -0.0004(7) 0.0023(7) 0.0034(7)
N1 0.0142(10) 0.0225(11) 0.0171(10) 0.0008(8) 0.0017(8) 0.0011(9)
N2 0.0157(10) 0.0239(11) 0.0290(12) 0.0010(9) 0.0068(9) 0.0037(9)
C1 0.0164(12) 0.0240(13) 0.0215(12) 0.0010(10) 0.0035(10) -0.0019(10)
C2 0.0181(13) 0.0284(15) 0.0406(17) -0.0032(12) 0.0086(12) -0.0052(11)
C3 0.0218(13) 0.0231(13) 0.0367(15) -0.0078(12) 0.0064(12) -0.0034(11)
C4 0.0310(15) 0.0237(14) 0.0445(17) -0.0016(12) 0.0125(13) 0.0067(12)
C5 0.0300(16) 0.0412(19) 0.068(2) -0.0032(16) 0.0199(16) 0.0122(14)
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'
Co Co 0.3494 0.9721 '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
N1 Co1 O5 92.49(7) . 2 ?
N1 Co1 O2 97.64(7) . 3_566 ?
O5 Co1 O2 169.85(6) 2 3_566 ?
N1 Co1 O2 177.03(7) . 1_565 ?
O5 Co1 O2 89.00(6) 2 1_565 ?
O2 Co1 O2 80.85(6) 3_566 1_565 ?
N1 Co1 O7 91.71(7) . . ?
O5 Co1 O7 89.54(6) 2 . ?
O2 Co1 O7 89.55(6) 3_566 . ?
O2 Co1 O7 85.73(6) 1_565 . ?
N1 Co1 O6 96.34(7) . . ?
O5 Co1 O6 87.74(6) 2 . ?
O2 Co1 O6 91.73(6) 3_566 . ?
O2 Co1 O6 86.28(6) 1_565 . ?
O7 Co1 O6 171.60(6) . . ?
O3 V1 O2 108.00(8) . . ?
O3 V1 O4 106.58(8) . . ?
O2 V1 O4 108.17(7) . . ?
O3 V1 O1 106.75(8) . . ?
O2 V1 O1 113.34(8) . . ?
O4 V1 O1 113.64(8) . . ?
O5 V2 O6 110.86(8) . . ?
O5 V2 O1 111.66(8) . . ?
O6 V2 O1 108.86(7) . . ?
O5 V2 O4 109.19(8) . 1_565 ?
O6 V2 O4 108.01(7) . 1_565 ?
O1 V2 O4 108.15(8) . 1_565 ?
V2 O1 V1 150.85(10) . . ?
V1 O2 Co1 138.42(8) . 3_566 ?
V1 O2 Co1 118.00(8) . 1_545 ?
Co1 O2 Co1 99.15(6) 3_566 1_545 ?
V2 O4 V1 131.54(9) 1_545 . ?
V2 O5 Co1 140.69(10) . 2_545 ?
V2 O6 Co1 126.37(8) . . ?
Co1 O7 H7A 108.7 . . ?
Co1 O7 H7B 112.4 . . ?
H7A O7 H7B 103.7 . . ?
C1 N1 C3 105.3(2) . . ?
C1 N1 Co1 128.11(17) . . ?
C3 N1 Co1 126.22(17) . . ?
C1 N2 C2 106.7(2) . . ?
C1 N2 C4 124.7(2) . . ?
C2 N2 C4 128.6(2) . . ?
N1 C1 N2 111.6(2) . . ?
N1 C1 H1 124.2 . . ?
N2 C1 H1 124.2 . . ?
C3 C2 N2 106.5(2) . . ?
C3 C2 H2 126.8 . . ?
N2 C2 H2 126.8 . . ?
C2 C3 N1 109.9(2) . . ?
C2 C3 H3 125.1 . . ?
N1 C3 H3 125.1 . . ?
C5 C4 N2 123.9(3) . . ?
C5 C4 H4 118.1 . . ?
N2 C4 H4 118.1 . . ?
C4 C5 H5A 120.0 . . ?
C4 C5 H5B 120.0 . . ?
H5A C5 H5B 120.0 . . ?
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
Co1 N1 2.0441(19) . ?
Co1 O5 2.0672(16) 2 ?
Co1 O2 2.0679(15) 3_566 ?
Co1 O2 2.1287(15) 1_565 ?
Co1 O7 2.1484(16) . ?
Co1 O6 2.1523(16) . ?
V1 O3 1.5942(17) . ?
V1 O2 1.7076(15) . ?
V1 O4 1.8048(16) . ?
V1 O1 1.8082(16) . ?
V2 O5 1.6511(16) . ?
V2 O6 1.6735(16) . ?
V2 O1 1.7608(16) . ?
V2 O4 1.7799(16) 1_565 ?
O2 Co1 2.0680(16) 3_566 ?
O2 Co1 2.1287(15) 1_545 ?
O4 V2 1.7799(16) 1_545 ?
O5 Co1 2.0671(16) 2_545 ?
O7 H7A 0.8499 . ?
O7 H7B 0.8499 . ?
N1 C1 1.313(3) . ?
N1 C3 1.385(3) . ?
N2 C1 1.352(3) . ?
N2 C2 1.377(3) . ?
N2 C4 1.420(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.342(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.305(4) . ?
C4 H4 0.9300 . ?
C5 H5A 0.9300 . ?
C5 H5B 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
O7 H7A O6 0.85 2.24 3.038(2) 156.8 3_576
O7 H7B O6 0.85 1.94 2.788(2) 175.6 1_565
C1 H1 O4 0.93 2.63 3.345(3) 134.4 2
C2 H2 O3 0.93 2.51 3.423(3) 165.8 1_665
C3 H3 O7 0.93 2.64 3.104(3) 111.8 .
C5 H5A O3 0.93 2.56 3.476(4) 168.5 1_665
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
O5 V2 O1 V1 100.4(2) . . . . ?
O6 V2 O1 V1 -22.3(2) . . . . ?
O4 V2 O1 V1 -139.45(19) 1_565 . . . ?
O3 V1 O1 V2 135.8(2) . . . . ?
O2 V1 O1 V2 17.0(2) . . . . ?
O4 V1 O1 V2 -107.0(2) . . . . ?
O3 V1 O2 Co1 15.40(16) . . . 3_566 ?
O4 V1 O2 Co1 -99.59(13) . . . 3_566 ?
O1 V1 O2 Co1 133.46(12) . . . 3_566 ?
O3 V1 O2 Co1 165.94(9) . . . 1_545 ?
O4 V1 O2 Co1 50.95(10) . . . 1_545 ?
O1 V1 O2 Co1 -76.00(10) . . . 1_545 ?
O3 V1 O4 V2 -121.25(13) . . . 1_545 ?
O2 V1 O4 V2 -5.33(14) . . . 1_545 ?
O1 V1 O4 V2 121.46(12) . . . 1_545 ?
O6 V2 O5 Co1 154.38(13) . . . 2_545 ?
O1 V2 O5 Co1 32.81(17) . . . 2_545 ?
O4 V2 O5 Co1 -86.74(15) 1_565 . . 2_545 ?
O5 V2 O6 Co1 88.35(11) . . . . ?
O1 V2 O6 Co1 -148.45(9) . . . . ?
O4 V2 O6 Co1 -31.25(12) 1_565 . . . ?
C3 N1 C1 N2 0.1(3) . . . . ?
Co1 N1 C1 N2 173.82(15) . . . . ?
C2 N2 C1 N1 -0.2(3) . . . . ?
C4 N2 C1 N1 -179.9(2) . . . . ?
C1 N2 C2 C3 0.3(3) . . . . ?
C4 N2 C2 C3 179.9(3) . . . . ?
N2 C2 C3 N1 -0.2(3) . . . . ?
C1 N1 C3 C2 0.1(3) . . . . ?
Co1 N1 C3 C2 -173.81(19) . . . . ?
C1 N2 C4 C5 -173.5(3) . . . . ?
C2 N2 C4 C5 6.9(5) . . . . ?