#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314292.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_4314292
loop_
_publ_author_name
'F. Albert Cotton'
'Elizabeth A. Hillard'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_section_title
;
 New Chemistry of the Triply Bonded Divanadium (V24+) Unit and Reduction
 to an Unprecedented V23+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6063
_journal_page_last               6070
_journal_paper_doi               10.1021/ic034646e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C55 H53 Cl12 Li N6 O4 V1'
_chemical_formula_sum            'C55 H53 Cl12 Li N6 O4 V'
_chemical_formula_weight         1345.31
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(THF)lithium-tris-3,5-dichlorophenylformamdinate vanadium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.4680(10)
_cell_angle_beta                 96.0810(10)
_cell_angle_gamma                105.7370(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0014(7)
_cell_length_b                   15.9750(10)
_cell_length_c                   18.9046(12)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.289
_cell_measurement_theta_min      2.204
_cell_volume                     3125.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELTXL v5.05 (Siemens, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART area detector'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14877
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         'none(area detector data)'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.8294
_exptl_absorpt_correction_T_min  0.7193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0544
_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)+(0.0860P)²+0.5518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                5424
_reflns_number_total             8151
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic034646esi20030610_035606_8.cif
_cod_data_source_block           footnote_compound
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C55 H53 Cl12 Li N6 O4 V1'
_cod_database_code               4314292
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
V1 V 0.64604(7) 0.23926(5) 0.21879(4) 0.0437(3) Uani 1 1 d . . .
N1 N 0.8279(3) 0.3101(2) 0.22589(17) 0.0409(9) Uani 1 1 d . . .
N2 N 0.7082(3) 0.3271(2) 0.31160(18) 0.0441(10) Uani 1 1 d . . .
N3 N 0.5407(3) 0.2904(2) 0.14675(18) 0.0440(10) Uani 1 1 d . . .
N4 N 0.4389(3) 0.2033(2) 0.21508(19) 0.0418(9) Uani 1 1 d . . .
N5 N 0.6498(3) 0.1279(2) 0.13627(18) 0.0431(10) Uani 1 1 d . . .
N6 N 0.6632(3) 0.1234(2) 0.25318(17) 0.0408(9) Uani 1 1 d . . .
C1 C 0.9336(4) 0.3245(3) 0.1912(2) 0.0369(11) Uani 1 1 d . . .
C2 C 1.0565(4) 0.3715(3) 0.2259(2) 0.0482(12) Uani 1 1 d . . .
H2A H 1.0708 0.3948 0.2757 0.058 Uiso 1 1 calc R . .
C3 C 1.1582(5) 0.3841(3) 0.1867(3) 0.0590(14) Uani 1 1 d . . .
C4 C 1.1417(5) 0.3519(3) 0.1136(3) 0.0606(15) Uani 1 1 d . . .
H4A H 1.2107 0.3617 0.0874 0.073 Uiso 1 1 calc R . .
C5 C 1.0203(5) 0.3050(3) 0.0807(3) 0.0569(15) Uani 1 1 d . . .
C6 C 0.9160(5) 0.2900(3) 0.1171(2) 0.0465(12) Uani 1 1 d . . .
H6A H 0.8344 0.2571 0.0923 0.056 Uiso 1 1 calc R . .
C7 C 0.8398(4) 0.3537(3) 0.2997(2) 0.0492(13) Uani 1 1 d . . .
H7A H 0.9131 0.3897 0.3314 0.059 Uiso 1 1 calc R . .
C8 C 0.6787(4) 0.3589(3) 0.3779(2) 0.0418(12) Uani 1 1 d . . .
C9 C 0.7711(5) 0.4113(3) 0.4351(2) 0.0504(13) Uani 1 1 d . . .
H9A H 0.8579 0.4277 0.4299 0.060 Uiso 1 1 calc R . .
C10 C 0.7327(5) 0.4388(3) 0.4998(3) 0.0623(15) Uani 1 1 d . . .
C11 C 0.6082(6) 0.4175(4) 0.5107(3) 0.0764(19) Uani 1 1 d . . .
H11A H 0.5848 0.4378 0.5550 0.092 Uiso 1 1 calc R . .
C12 C 0.5191(5) 0.3654(4) 0.4543(3) 0.0707(17) Uani 1 1 d . . .
C13 C 0.5508(5) 0.3359(3) 0.3879(2) 0.0539(14) Uani 1 1 d . . .
H13A H 0.4867 0.3008 0.3501 0.065 Uiso 1 1 calc R . .
C14 C 0.5536(5) 0.3338(3) 0.0880(2) 0.0414(12) Uani 1 1 d . . .
C15 C 0.4550(5) 0.3236(3) 0.0319(2) 0.0500(13) Uani 1 1 d . . .
H15A H 0.3726 0.2870 0.0328 0.060 Uiso 1 1 calc R . .
C16 C 0.4787(5) 0.3676(3) -0.0253(2) 0.0550(14) Uani 1 1 d . . .
C17 C 0.5984(6) 0.4220(3) -0.0286(3) 0.0612(15) Uani 1 1 d . . .
H17A H 0.6134 0.4519 -0.0675 0.073 Uiso 1 1 calc R . .
C18 C 0.6953(5) 0.4310(3) 0.0273(3) 0.0513(13) Uani 1 1 d . . .
C19 C 0.6752(5) 0.3884(3) 0.0847(2) 0.0469(12) Uani 1 1 d . . .
H19A H 0.7432 0.3958 0.1218 0.056 Uiso 1 1 calc R . .
C20 C 0.4269(4) 0.2502(3) 0.1644(2) 0.0438(12) Uani 1 1 d . . .
H20A H 0.3484 0.2550 0.1431 0.053 Uiso 1 1 calc R . .
C21 C 0.3339(4) 0.1594(3) 0.2456(2) 0.0399(11) Uani 1 1 d . . .
C22 C 0.2189(4) 0.1793(3) 0.2431(2) 0.0445(12) Uani 1 1 d . . .
H22A H 0.2055 0.2241 0.2187 0.053 Uiso 1 1 calc R . .
C23 C 0.1233(4) 0.1325(3) 0.2770(3) 0.0490(13) Uani 1 1 d . . .
C24 C 0.1400(5) 0.0671(3) 0.3142(2) 0.0497(13) Uani 1 1 d . . .
H24A H 0.0749 0.0367 0.3374 0.060 Uiso 1 1 calc R . .
C25 C 0.2542(5) 0.0480(3) 0.3161(2) 0.0506(13) Uani 1 1 d . . .
C26 C 0.3502(4) 0.0930(3) 0.2815(2) 0.0470(12) Uani 1 1 d . . .
H26A H 0.4273 0.0781 0.2826 0.056 Uiso 1 1 calc R . .
C27 C 0.6589(4) 0.0962(3) 0.0642(2) 0.0458(13) Uani 1 1 d . . .
C28 C 0.7269(5) 0.0360(3) 0.0456(2) 0.0549(14) Uani 1 1 d . . .
H28A H 0.7695 0.0149 0.0817 0.066 Uiso 1 1 calc R . .
C29 C 0.7303(5) 0.0078(3) -0.0268(3) 0.0624(16) Uani 1 1 d . . .
C30 C 0.6732(5) 0.0388(4) -0.0811(3) 0.0670(17) Uani 1 1 d . . .
H30A H 0.6766 0.0186 -0.1299 0.080 Uiso 1 1 calc R . .
C31 C 0.6105(5) 0.1006(3) -0.0618(2) 0.0587(15) Uani 1 1 d . . .
C32 C 0.6018(5) 0.1291(3) 0.0102(3) 0.0546(14) Uani 1 1 d . . .
H32A H 0.5573 0.1705 0.0221 0.066 Uiso 1 1 calc R . .
C33 C 0.6617(4) 0.0809(3) 0.1861(2) 0.0459(12) Uani 1 1 d . . .
H33A H 0.6685 0.0231 0.1761 0.055 Uiso 1 1 calc R . .
C34 C 0.6591(4) 0.0825(3) 0.3135(2) 0.0423(12) Uani 1 1 d . . .
C35 C 0.6527(5) -0.0049(3) 0.3130(3) 0.0560(14) Uani 1 1 d . . .
H35A H 0.6558 -0.0413 0.2698 0.067 Uiso 1 1 calc R . .
C36 C 0.6416(5) -0.0395(3) 0.3761(3) 0.0611(15) Uani 1 1 d . . .
C37 C 0.6369(5) 0.0111(4) 0.4408(3) 0.0594(14) Uani 1 1 d . . .
H37A H 0.6299 -0.0127 0.4833 0.071 Uiso 1 1 calc R . .
C38 C 0.6427(5) 0.0979(3) 0.4403(2) 0.0500(13) Uani 1 1 d . . .
C39 C 0.6564(4) 0.1348(3) 0.3796(2) 0.0466(12) Uani 1 1 d . . .
H39A H 0.6640 0.1952 0.3822 0.056 Uiso 1 1 calc R . .
Cl1 Cl 1.31115(14) 0.43923(12) 0.23126(10) 0.1008(6) Uani 1 1 d . . .
Cl2 Cl 0.99426(18) 0.26309(11) -0.01183(8) 0.1025(7) Uani 1 1 d . . .
Cl3 Cl 0.85110(16) 0.50430(12) 0.57110(8) 0.1005(6) Uani 1 1 d . . .
Cl4 Cl 0.35859(16) 0.33434(13) 0.46521(10) 0.1199(8) Uani 1 1 d . . .
Cl5 Cl 0.35547(17) 0.35227(12) -0.09616(8) 0.0938(5) Uani 1 1 d . . .
Cl6 Cl 0.84762(15) 0.49721(10) 0.02352(8) 0.0851(5) Uani 1 1 d . . .
Cl7 Cl -0.02327(13) 0.15464(9) 0.27199(9) 0.0759(5) Uani 1 1 d . . .
Cl8 Cl 0.27971(14) -0.03462(11) 0.36052(8) 0.0792(5) Uani 1 1 d . . .
Cl9 Cl 0.54143(18) 0.14463(11) -0.12842(7) 0.0926(6) Uani 1 1 d . . .
Cl10 Cl 0.81422(17) -0.06937(11) -0.04801(8) 0.0924(6) Uani 1 1 d . . .
Cl11 Cl 0.6287(2) -0.15126(11) 0.37259(9) 0.1076(7) Uani 1 1 d . . .
Cl12 Cl 0.63056(18) 0.16378(9) 0.51948(7) 0.0871(6) Uani 1 1 d . . .
O1S O 2.0960(4) 0.6730(3) 0.2673(2) 0.0821(12) Uani 1 1 d . A .
C1S C 2.0842(6) 0.6177(4) 0.1979(3) 0.090(2) Uani 1 1 d . . .
H1SA H 2.0207 0.6281 0.1625 0.109 Uiso 1 1 calc R . .
H1SB H 2.0584 0.5550 0.2018 0.109 Uiso 1 1 calc R . .
C2S C 2.2147(8) 0.6437(5) 0.1760(4) 0.118(3) Uani 1 1 d . . .
H2SA H 2.2359 0.5916 0.1525 0.142 Uiso 1 1 calc R . .
H2SB H 2.2194 0.6856 0.1426 0.142 Uiso 1 1 calc R . .
C3S C 2.3030(8) 0.6858(7) 0.2451(5) 0.146(3) Uani 1 1 d . . .
H3SA H 2.3584 0.6493 0.2565 0.175 Uiso 1 1 calc R . .
H3SB H 2.3568 0.7444 0.2413 0.175 Uiso 1 1 calc R . .
C4S C 2.2233(8) 0.6933(6) 0.3013(4) 0.126(3) Uani 1 1 d . . .
H4SA H 2.2306 0.6522 0.3341 0.151 Uiso 1 1 calc R . .
H4SB H 2.2511 0.7536 0.3296 0.151 Uiso 1 1 calc R . .
O2S O 1.8065(4) 0.6404(2) 0.2864(3) 0.1068(17) Uani 0.601(14) 1 d P A 1
C5S C 1.7694(5) 0.5586(3) 0.2418(3) 0.0664(15) Uani 0.601(14) 1 d P A 1
H5SA H 1.8247 0.5231 0.2560 0.080 Uiso 0.601(14) 1 calc PR A 1
H5SB H 1.7755 0.5652 0.1915 0.080 Uiso 0.601(14) 1 calc PR A 1
C6S C 1.6344(6) 0.5144(4) 0.2493(3) 0.0760(18) Uani 0.601(14) 1 d P A 1
H6SA H 1.6229 0.4529 0.2549 0.091 Uiso 0.601(14) 1 calc PR A 1
H6SB H 1.5752 0.5156 0.2071 0.091 Uiso 0.601(14) 1 calc PR A 1
C7S C 1.6140(6) 0.5691(4) 0.3169(3) 0.093(2) Uani 0.601(14) 1 d P A 1
H7SA H 1.5238 0.5661 0.3165 0.112 Uiso 0.601(14) 1 calc PR A 1
H7SB H 1.6459 0.5509 0.3607 0.112 Uiso 0.601(14) 1 calc PR A 1
C8S C 1.6882(10) 0.6541(6) 0.3105(6) 0.069(4) Uiso 0.601(14) 1 d P A 1
H8SA H 1.7080 0.6947 0.3572 0.083 Uiso 0.601(14) 1 calc PR A 1
H8SB H 1.6430 0.6783 0.2749 0.083 Uiso 0.601(14) 1 calc PR A 1
O2T O 1.8065(4) 0.6404(2) 0.2864(3) 0.1068(17) Uani 0.399(14) 1 d P A 2
C5T C 1.7694(5) 0.5586(3) 0.2418(3) 0.0664(15) Uani 0.399(14) 1 d P A 2
H5TA H 1.8247 0.5231 0.2560 0.080 Uiso 0.399(14) 1 calc PR A 2
H5TB H 1.7755 0.5652 0.1915 0.080 Uiso 0.399(14) 1 calc PR A 2
C6T C 1.6344(6) 0.5144(4) 0.2493(3) 0.0760(18) Uani 0.399(14) 1 d P A 2
H6TA H 1.6229 0.4529 0.2549 0.091 Uiso 0.399(14) 1 calc PR A 2
H6TB H 1.5752 0.5156 0.2071 0.091 Uiso 0.399(14) 1 calc PR A 2
C7T C 1.6140(6) 0.5691(4) 0.3169(3) 0.093(2) Uani 0.399(14) 1 d P A 2
H7TA H 1.5573 0.6042 0.3040 0.112 Uiso 0.399(14) 1 calc PR A 2
H7TB H 1.5742 0.5302 0.3488 0.112 Uiso 0.399(14) 1 calc PR A 2
C8T C 1.7372(13) 0.6273(8) 0.3536(8) 0.056(5) Uiso 0.399(14) 1 d P A 2
H8TA H 1.7795 0.5988 0.3871 0.067 Uiso 0.399(14) 1 calc PR A 2
H8TB H 1.7301 0.6832 0.3795 0.067 Uiso 0.399(14) 1 calc PR A 2
O3S O 2.0025(4) 0.7672(3) 0.4050(2) 0.0869(13) Uani 1 1 d . A .
C9S C 2.0066(11) 0.7072(6) 0.4549(5) 0.159(4) Uani 1 1 d . . .
H9SA H 1.9357 0.6527 0.4392 0.191 Uiso 1 1 calc R . .
H9SB H 2.0870 0.6918 0.4564 0.191 Uiso 1 1 calc R . .
C10S C 1.9964(8) 0.7507(7) 0.5256(4) 0.127(3) Uani 1 1 d . . .
H10A H 2.0754 0.7607 0.5592 0.152 Uiso 1 1 calc R . .
H10B H 1.9253 0.7142 0.5449 0.152 Uiso 1 1 calc R . .
C11S C 1.9744(9) 0.8348(6) 0.5171(4) 0.132(3) Uani 1 1 d . . .
H11B H 2.0305 0.8827 0.5547 0.159 Uiso 1 1 calc R . .
H11C H 1.8855 0.8323 0.5211 0.159 Uiso 1 1 calc R . .
C12S C 2.0033(7) 0.8505(4) 0.4431(3) 0.092(2) Uani 1 1 d . . .
H12A H 1.9380 0.8722 0.4187 0.111 Uiso 1 1 calc R . .
H12B H 2.0870 0.8940 0.4468 0.111 Uiso 1 1 calc R . .
O4S O 1.9621(4) 0.8180(3) 0.24606(19) 0.0801(12) Uani 1 1 d . A .
C13S C 1.8534(7) 0.8502(5) 0.2371(4) 0.112(3) Uani 1 1 d . . .
H13B H 1.8556 0.8944 0.2794 0.134 Uiso 1 1 calc R . .
H13C H 1.7746 0.8014 0.2318 0.134 Uiso 1 1 calc R . .
C14S C 1.8569(9) 0.8903(6) 0.1714(6) 0.154(4) Uani 1 1 d . . .
H14A H 1.8393 0.9476 0.1807 0.185 Uiso 1 1 calc R . .
H14B H 1.7934 0.8515 0.1315 0.185 Uiso 1 1 calc R . .
C15S C 1.9881(9) 0.9018(5) 0.1538(4) 0.111(3) Uani 1 1 d . . .
H15B H 1.9863 0.8876 0.1014 0.133 Uiso 1 1 calc R . .
H15C H 2.0419 0.9628 0.1716 0.133 Uiso 1 1 calc R . .
C16S C 2.0353(7) 0.8407(5) 0.1900(3) 0.093(2) Uani 1 1 d . . .
H16A H 2.0286 0.7872 0.1551 0.111 Uiso 1 1 calc R . .
H16B H 2.1255 0.8679 0.2107 0.111 Uiso 1 1 calc R . .
Li1 Li 1.9718(10) 0.7269(6) 0.3011(5) 0.077(3) 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'
Li Li -0.0003 0.0001 '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'
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
N1 V1 N2 67.65(13) . . ?
N1 V1 N3 106.01(14) . . ?
N2 V1 N3 108.97(15) . . ?
N1 V1 N6 102.35(15) . . ?
N2 V1 N6 100.89(14) . . ?
N3 V1 N6 144.74(14) . . ?
N1 V1 N4 161.89(14) . . ?
N2 V1 N4 102.18(13) . . ?
N3 V1 N4 61.97(14) . . ?
N6 V1 N4 94.16(14) . . ?
N1 V1 N5 97.37(13) . . ?
N2 V1 N5 155.29(16) . . ?
N3 V1 N5 93.74(14) . . ?
N6 V1 N5 61.91(13) . . ?
N4 V1 N5 96.95(13) . . ?
N1 V1 C7 33.93(12) . . ?
N2 V1 C7 34.11(12) . . ?
N3 V1 C7 115.11(15) . . ?
N6 V1 C7 100.12(15) . . ?
N4 V1 C7 135.77(13) . . ?
N5 V1 C7 126.71(14) . . ?
N1 V1 C33 101.25(14) . . ?
N2 V1 C33 130.09(16) . . ?
N3 V1 C33 120.68(14) . . ?
N6 V1 C33 31.40(13) . . ?
N4 V1 C33 96.71(14) . . ?
N5 V1 C33 30.51(12) . . ?
C7 V1 C33 116.81(16) . . ?
C1 N1 C7 119.4(3) . . ?
C1 N1 V1 144.9(3) . . ?
C7 N1 V1 95.5(2) . . ?
C8 N2 C7 118.6(4) . . ?
C8 N2 V1 145.8(3) . . ?
C7 N2 V1 94.9(2) . . ?
C20 N3 C14 123.2(4) . . ?
C20 N3 V1 94.9(3) . . ?
C14 N3 V1 140.8(3) . . ?
C20 N4 C21 122.2(4) . . ?
C20 N4 V1 91.5(3) . . ?
C21 N4 V1 146.2(3) . . ?
C33 N5 C27 120.3(4) . . ?
C33 N5 V1 90.6(2) . . ?
C27 N5 V1 148.4(3) . . ?
C33 N6 C34 123.2(4) . . ?
C33 N6 V1 94.1(3) . . ?
C34 N6 V1 142.0(3) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 C6 118.1(4) . . ?
C2 C1 C6 118.5(4) . . ?
C3 C2 C1 119.9(4) . . ?
C4 C3 C2 122.1(5) . . ?
C4 C3 Cl1 118.5(4) . . ?
C2 C3 Cl1 119.3(4) . . ?
C5 C4 C3 117.0(4) . . ?
C4 C5 C6 123.4(4) . . ?
C4 C5 Cl2 118.8(4) . . ?
C6 C5 Cl2 117.9(4) . . ?
C5 C6 C1 119.1(4) . . ?
N1 C7 N2 100.8(3) . . ?
N1 C7 V1 50.53(19) . . ?
N2 C7 V1 51.00(19) . . ?
N2 C8 C9 123.0(4) . . ?
N2 C8 C13 118.3(4) . . ?
C9 C8 C13 118.7(4) . . ?
C10 C9 C8 118.9(5) . . ?
C11 C10 C9 123.4(5) . . ?
C11 C10 Cl3 118.7(4) . . ?
C9 C10 Cl3 117.9(4) . . ?
C10 C11 C12 117.0(4) . . ?
C11 C12 C13 122.6(5) . . ?
C11 C12 Cl4 119.3(4) . . ?
C13 C12 Cl4 118.1(4) . . ?
C12 C13 C8 119.4(5) . . ?
N3 C14 C15 124.2(4) . . ?
N3 C14 C19 117.1(4) . . ?
C15 C14 C19 118.6(4) . . ?
C16 C15 C14 119.8(5) . . ?
C17 C16 C15 121.8(5) . . ?
C17 C16 Cl5 118.9(4) . . ?
C15 C16 Cl5 119.3(4) . . ?
C18 C17 C16 117.7(4) . . ?
C19 C18 C17 122.0(5) . . ?
C19 C18 Cl6 119.3(4) . . ?
C17 C18 Cl6 118.6(4) . . ?
C18 C19 C14 120.1(5) . . ?
N4 C20 N3 111.7(4) . . ?
C26 C21 C22 118.9(4) . . ?
C26 C21 N4 116.3(4) . . ?
C22 C21 N4 124.7(4) . . ?
C21 C22 C23 119.3(4) . . ?
C24 C23 C22 122.0(4) . . ?
C24 C23 Cl7 118.2(3) . . ?
C22 C23 Cl7 119.7(4) . . ?
C25 C24 C23 118.1(4) . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 Cl8 120.2(4) . . ?
C26 C25 Cl8 119.0(4) . . ?
C21 C26 C25 120.9(5) . . ?
C32 C27 C28 119.2(4) . . ?
C32 C27 N5 118.0(5) . . ?
C28 C27 N5 122.7(5) . . ?
C29 C28 C27 118.9(5) . . ?
C30 C29 C28 122.6(5) . . ?
C30 C29 Cl10 119.8(4) . . ?
C28 C29 Cl10 117.6(5) . . ?
C29 C30 C31 117.8(4) . . ?
C30 C31 C32 121.5(5) . . ?
C30 C31 Cl9 119.5(4) . . ?
C32 C31 Cl9 119.0(5) . . ?
C27 C32 C31 119.9(5) . . ?
N5 C33 N6 113.3(4) . . ?
N5 C33 V1 58.8(2) . . ?
N6 C33 V1 54.5(2) . . ?
C35 C34 N6 125.6(4) . . ?
C35 C34 C39 117.8(4) . . ?
N6 C34 C39 116.6(4) . . ?
C34 C35 C36 120.3(4) . . ?
C37 C36 C35 122.1(5) . . ?
C37 C36 Cl11 119.0(4) . . ?
C35 C36 Cl11 118.9(4) . . ?
C38 C37 C36 116.9(4) . . ?
C39 C38 C37 122.6(4) . . ?
C39 C38 Cl12 118.4(4) . . ?
C37 C38 Cl12 118.9(3) . . ?
C38 C39 C34 120.2(4) . . ?
C4S O1S C1S 107.6(5) . . ?
C4S O1S Li1 124.9(5) . . ?
C1S O1S Li1 126.6(5) . . ?
O1S C1S C2S 105.2(5) . . ?
C3S C2S C1S 104.6(6) . . ?
C4S C3S C2S 106.9(7) . . ?
O1S C4S C3S 108.0(7) . . ?
C5S O2S C8S 105.8(5) . . ?
C5S O2S Li1 126.7(4) . . ?
C8S O2S Li1 126.7(5) . . ?
O2S C5S C6S 107.5(4) . . ?
C5S C6S C7S 103.4(4) . . ?
C8S C7S C6S 100.4(6) . . ?
C7S C8S O2S 104.8(7) . . ?
C12S O3S C9S 109.9(5) . . ?
C12S O3S Li1 127.5(5) . . ?
C9S O3S Li1 121.8(5) . . ?
C10S C9S O3S 108.1(7) . . ?
C9S C10S C11S 107.1(7) . . ?
C10S C11S C12S 106.9(6) . . ?
O3S C12S C11S 105.2(6) . . ?
C13S O4S C16S 107.8(5) . . ?
C13S O4S Li1 123.5(5) . . ?
C16S O4S Li1 125.4(5) . . ?
O4S C13S C14S 107.9(6) . . ?
C13S C14S C15S 105.7(7) . . ?
C16S C15S C14S 104.7(7) . . ?
O4S C16S C15S 109.5(6) . . ?
O1S Li1 O4S 108.1(4) . . ?
O1S Li1 O2S 110.2(5) . . ?
O4S Li1 O2S 108.9(6) . . ?
O1S Li1 O3S 113.1(6) . . ?
O4S Li1 O3S 114.0(5) . . ?
O2S Li1 O3S 102.2(4) . . ?
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
V1 N1 1.992(3) . ?
V1 N2 2.004(3) . ?
V1 N3 2.091(4) . ?
V1 N6 2.098(4) . ?
V1 N4 2.185(4) . ?
V1 N5 2.200(3) . ?
V1 C7 2.569(5) . ?
V1 C33 2.570(5) . ?
N1 C1 1.377(5) . ?
N1 C7 1.441(5) . ?
N2 C8 1.386(5) . ?
N2 C7 1.446(5) . ?
N3 C20 1.344(5) . ?
N3 C14 1.393(5) . ?
N4 C20 1.318(5) . ?
N4 C21 1.407(5) . ?
N5 C33 1.305(6) . ?
N5 C27 1.405(5) . ?
N6 C33 1.343(5) . ?
N6 C34 1.394(5) . ?
C1 C2 1.392(6) . ?
C1 C6 1.401(6) . ?
C2 C3 1.392(6) . ?
C3 C4 1.376(7) . ?
C3 Cl1 1.731(5) . ?
C4 C5 1.370(7) . ?
C5 C6 1.382(6) . ?
C5 Cl2 1.743(5) . ?
C8 C9 1.394(6) . ?
C8 C13 1.396(6) . ?
C9 C10 1.384(6) . ?
C10 C11 1.365(7) . ?
C10 Cl3 1.755(5) . ?
C11 C12 1.365(7) . ?
C12 C13 1.389(6) . ?
C12 Cl4 1.743(5) . ?
C14 C15 1.393(6) . ?
C14 C19 1.397(6) . ?
C15 C16 1.384(6) . ?
C16 C17 1.380(7) . ?
C16 Cl5 1.741(5) . ?
C17 C18 1.381(7) . ?
C18 C19 1.370(6) . ?
C18 Cl6 1.737(5) . ?
C21 C26 1.381(6) . ?
C21 C22 1.384(6) . ?
C22 C23 1.391(6) . ?
C23 C24 1.383(6) . ?
C23 Cl7 1.738(5) . ?
C24 C25 1.369(6) . ?
C25 C26 1.391(6) . ?
C25 Cl8 1.732(5) . ?
C27 C32 1.383(7) . ?
C27 C28 1.399(7) . ?
C28 C29 1.384(6) . ?
C29 C30 1.370(7) . ?
C29 Cl10 1.756(6) . ?
C30 C31 1.379(7) . ?
C31 C32 1.391(6) . ?
C31 Cl9 1.734(6) . ?
C34 C35 1.378(6) . ?
C34 C39 1.405(6) . ?
C35 C36 1.390(6) . ?
C36 C37 1.377(6) . ?
C36 Cl11 1.743(5) . ?
C37 C38 1.372(6) . ?
C38 C39 1.368(6) . ?
C38 Cl12 1.738(4) . ?
O1S C4S 1.408(8) . ?
O1S C1S 1.442(6) . ?
O1S Li1 1.918(10) . ?
C1S C2S 1.504(9) . ?
C2S C3S 1.491(10) . ?
C3S C4S 1.458(10) . ?
O2S C5S 1.377(6) . ?
O2S C8S 1.483(10) . ?
O2S Li1 1.927(10) . ?
C5S C6S 1.492(7) . ?
C6S C7S 1.512(7) . ?
C7S C8S 1.410(10) . ?
O3S C12S 1.415(6) . ?
O3S C9S 1.446(8) . ?
O3S Li1 1.938(10) . ?
C9S C10S 1.443(10) . ?
C10S C11S 1.456(10) . ?
C11S C12S 1.509(9) . ?
O4S C13S 1.427(8) . ?
O4S C16S 1.428(6) . ?
O4S Li1 1.928(11) . ?
C13S C14S 1.478(10) . ?
C14S C15S 1.485(11) . ?
C15S C16S 1.445(9) . ?
