#------------------------------------------------------------------------------
#$Date: 2025-07-06 18:31:30 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300768 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/86/7718635.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_7718635
loop_
_publ_author_name
'Kirk, Ryan M.'
'Hill, Anthony F.'
_publ_section_title
;
 Pnictogen-functionalised isocyanide ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8881
_journal_page_last               8887
_journal_paper_doi               10.1039/d5dt00992h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C24 H32 Li2 N6 O10 W2'
_chemical_formula_sum            'C24 H32 Li2 N6 O10 W2'
_chemical_formula_weight         946.13
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                112.5180(10)
_cell_angle_beta                 111.564(2)
_cell_angle_gamma                93.9840(10)
_cell_formula_units_Z            1
_cell_length_a                   8.71120(10)
_cell_length_b                   10.7852(2)
_cell_length_c                   11.3689(2)
_cell_measurement_reflns_used    10165
_cell_measurement_temperature    149(4)
_cell_measurement_theta_max      77.7900
_cell_measurement_theta_min      4.5540
_cell_volume                     889.73(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  58.00   0.50    0.50    --   46.45 -34.00  54.00   84
  2  ω    -28.00   9.00   0.50    0.50    --   46.45 -34.00  54.00   74
  3  ω     33.00 120.00   0.50    0.50    --   46.45  34.00-147.00  174
  4  ω     32.00  61.00   0.50    0.50    --  107.75 -34.00  54.00   58
  5  ω    142.00 168.00   0.50    0.50    --  107.75  34.00-147.00   52
  6  ω     95.00 133.00   0.50    0.50    --  107.75  34.00-147.00   76
  7  ω     -6.00  21.00   0.50    0.50    --  -46.45  34.00-147.00   54
  8  ω    -58.00 -33.00   0.50    0.50    --  -46.45 -38.00 150.00   50
  9  ω    -86.00 -18.00   0.50    0.50    --  -46.45 125.00 -90.00  136
 10  ω   -121.00 -33.00   0.50    0.50    --  -46.45 -34.00  54.00  176
 11  ω   -120.00 -68.00   0.50    0.50    --  -46.45 -38.00 150.00  104
 12  ω     59.00  86.00   0.50    0.50    --   46.45-125.00 -60.00   54
 13  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00-150.00   50
 14  ω     81.00 106.00   0.50    0.50    --  107.75 -95.00-180.00   50
 15  ω     99.00 128.00   0.50    0.50    --  107.75 125.00  90.00   58
 16  ω     44.00  70.00   0.50    0.50    --  107.75 -45.00-180.00   52
 17  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 18  ω     67.00 111.00   0.50    0.50    --  107.75-125.00 150.00   88
 19  ω     51.00  87.00   0.50    0.50    --  107.75 -61.00-120.00   72
 20  ω     64.00 105.00   0.50    0.50    --  107.75 -95.00 -90.00   82
 21  ω     32.00  59.00   0.50    0.50    --  107.75 -30.00-120.00   54
 22  ω     36.00  76.00   0.50    0.50    --  107.75 -95.00-180.00   80
 23  ω     87.00 117.00   0.50    0.50    --  107.75 -77.00-180.00   60
 24  ω     34.00  79.00   0.50    0.50    --  107.75 -77.00-180.00   90
 25  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -30.00   50
 26  ω     36.00  70.00   0.50    0.50    --  107.75 -95.00 -30.00   68
 27  ω     78.00 104.00   0.50    0.50    --  107.75 -95.00 -30.00   52
 28  ω     39.00  73.00   0.50    0.50    --  107.75 -45.00  30.00   68
 29  ω    102.00 139.00   0.50    0.50    --  107.75  30.00 -90.00   74
 30  ω    146.00 171.00   0.50    0.50    --  107.75  30.00 -90.00   50
 31  ω     95.00 138.00   0.50    0.50    --  107.75 125.00 150.00   86
 32  ω    145.00 171.00   0.50    0.50    --  107.75 125.00 150.00   52
 33  ω     39.00  70.00   0.50    0.50    --  107.75 -61.00 120.00   62
 34  ω     52.00 103.00   0.50    0.50    --  107.75 -95.00  60.00  102
 35  ω     78.00 104.00   0.50    0.50    --  107.75 -95.00  30.00   52
 36  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -90.00   50
 37  ω     45.00  71.00   0.50    0.50    --  107.75-100.00 163.50   52
 38  ω     94.00 175.00   0.50    0.50    --  107.75  30.00 150.00  162
 39  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00  60.00   50
 40  ω     32.00  58.00   0.50    0.50    --  107.75 -30.00   0.00   52
 41  ω     79.00 107.00   0.50    0.50    --  107.75-100.00 163.50   56
 42  ω     36.00  65.00   0.50    0.50    --  107.75 -95.00  30.00   58
 43  ω     97.00 140.00   0.50    0.50    --  107.75  45.00 -30.00   86
 44  ω    145.00 176.00   0.50    0.50    --  107.75  45.00 -30.00   62
 45  ω     69.00  95.00   0.50    0.50    --  107.75 -95.00  90.00   52
 46  ω     44.00 106.00   0.50    0.50    --  107.75 -95.00-120.00  124
 47  ω     41.00  66.00   0.50    0.50    --  107.75-125.00 -60.00   50
 48  ω    138.00 173.00   0.50    0.50    --  107.75 125.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1585761000
_diffrn_orient_matrix_UB_12      0.0478289000
_diffrn_orient_matrix_UB_13      0.1404839000
_diffrn_orient_matrix_UB_21      0.1086665000
_diffrn_orient_matrix_UB_22      -0.0506438000
_diffrn_orient_matrix_UB_23      -0.0811456000
_diffrn_orient_matrix_UB_31      0.0388459000
_diffrn_orient_matrix_UB_32      0.1434600000
_diffrn_orient_matrix_UB_33      0.0039522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.051
_diffrn_reflns_theta_min         4.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.236
_exptl_absorpt_correction_T_max  0.27716
_exptl_absorpt_correction_T_min  0.18262
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         1.214
_refine_diff_density_min         -2.720
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0362
_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/[σ²(Fo²)+(0.0570P)²+2.5208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3677
_reflns_number_total             3729
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_325_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718635
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H32Li2N6O10W2
_chemical_oxdiff_usercomment     'THF evap at -30 '
_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_max   0.346
_shelx_estimated_absorpt_t_min   0.079
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C11 \\sim N3-C11'
 with sigma of 0.02
 N3-C12 \\sim N3-C12'
 with sigma of 0.02
 N3-C10 \\sim N3-C10'
 with sigma of 0.02
 C9-C10 \\sim C9-C10'
 with sigma of 0.02
3. Others
 Sof(H9bc)=Sof(H9bd)=Sof(C10')=Sof(H10c)=Sof(H10d)=Sof(C11')=Sof(H11d)=
 Sof(H11e)=Sof(H11f)=Sof(C12')=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(H9aa)=Sof(H9ab)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=Sof(C12)=Sof(H12a)=
 Sof(H12b)=Sof(H12c)=Sof(C10)=Sof(H10a)=Sof(H10b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9aa,H9ab), C9(H9bc,H9bd), C10(H10a,H10b), C10'(H10c,H10d)
4.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C8(H8a,H8b,H8c),
 C11'(H11d,H11e,H11f), C12'(H12d,H12e,H12f)
;
_ins_header
;
TITL RMK_325_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.711187  10.785237  11.368916 112.5179 111.5643  93.9840
ZERR    1.00   0.000149   0.000160   0.000179   0.0014   0.0015   0.0013
LATT  1
SFAC C H Li N O W
UNIT 24.00 32.00 2.00 6.00 10.00 2.00
REM  CrysAlisPro recorded range (K): Min=146.2; max=150.0; aver:148.1
TEMP -125
SIZE 0.11 0.19 0.42
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.489
_oxdiff_exptl_absorpt_empirical_full_min 0.484
loop_
_space_group_symop_operation_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_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
W1 W 0.71211(3) 0.78660(2) 0.32347(2) 0.03180(10) Uani 1 1 d . . . . .
O5 O 0.6950(6) 0.5240(5) 0.0618(5) 0.0493(10) Uani 1 1 d . . . . .
O4 O 1.0749(6) 0.7553(6) 0.4961(5) 0.0589(12) Uani 1 1 d . . . . .
O2 O 0.3316(6) 0.7789(5) 0.1371(5) 0.0615(12) Uani 1 1 d . . . . .
O3 O 0.7255(8) 1.0536(5) 0.5825(5) 0.0632(13) Uani 1 1 d . . . . .
O1 O 0.8764(8) 0.9817(5) 0.2303(5) 0.0658(14) Uani 1 1 d . . . . .
N1 N 0.5632(7) 0.5882(5) 0.4401(5) 0.0454(11) Uani 1 1 d . . . . .
N3 N 0.4171(7) 0.2334(5) 0.2255(5) 0.0466(11) Uani 1 1 d D . . . .
C5 C 0.6994(6) 0.6164(5) 0.1557(5) 0.0348(10) Uani 1 1 d . . . . .
C6 C 0.6126(7) 0.6577(5) 0.3978(5) 0.0368(10) Uani 1 1 d . . . . .
N2 N 0.1485(6) 0.3741(7) 0.2230(6) 0.0569(13) Uani 1 1 d . . . . .
C1 C 0.8138(8) 0.9100(6) 0.2639(6) 0.0437(12) Uani 1 1 d . . . . .
C4 C 0.9468(7) 0.7714(6) 0.4371(6) 0.0424(12) Uani 1 1 d . . . . .
C2 C 0.4654(8) 0.7829(6) 0.2039(6) 0.0412(11) Uani 1 1 d . . . . .
C3 C 0.7222(8) 0.9585(6) 0.4921(6) 0.0417(12) Uani 1 1 d . . . . .
C9 C 0.1343(10) 0.2519(10) 0.0965(9) 0.077(2) Uani 1 1 d D . . . .
H9AA H 0.015751 0.201491 0.040107 0.092 Uiso 0.762(19) 1 calc R U P A 1
H9AB H 0.171150 0.283737 0.039915 0.092 Uiso 0.762(19) 1 calc R U P A 1
H9BC H 0.062933 0.172186 0.086888 0.092 Uiso 0.238(19) 1 calc R U P A 2
H9BD H 0.074764 0.267482 0.014617 0.092 Uiso 0.238(19) 1 calc R U P A 2
C7 C 0.1253(11) 0.4906(11) 0.1870(10) 0.078(2) Uani 1 1 d . . . . .
H7A H 0.212876 0.512154 0.160652 0.116 Uiso 1 1 calc R U . . .
H7B H 0.131980 0.569918 0.267024 0.116 Uiso 1 1 calc R U . . .
H7C H 0.015893 0.465906 0.109634 0.116 Uiso 1 1 calc R U . . .
C11 C 0.4982(17) 0.1414(11) 0.2825(13) 0.065(3) Uani 0.762(19) 1 d D . P A 1
H11A H 0.494907 0.059018 0.206912 0.098 Uiso 0.762(19) 1 calc R U P A 1
H11B H 0.438391 0.117000 0.329572 0.098 Uiso 0.762(19) 1 calc R U P A 1
H11C H 0.614462 0.188009 0.348202 0.098 Uiso 0.762(19) 1 calc R U P A 1
C12 C 0.5021(15) 0.2605(12) 0.1461(12) 0.062(3) Uani 0.762(19) 1 d D . P A 1
H12A H 0.620339 0.304252 0.207315 0.093 Uiso 0.762(19) 1 calc R U P A 1
H12B H 0.450393 0.320379 0.107776 0.093 Uiso 0.762(19) 1 calc R U P A 1
H12C H 0.491828 0.174778 0.070797 0.093 Uiso 0.762(19) 1 calc R U P A 1
C8 C 0.0247(11) 0.3500(13) 0.2733(12) 0.092(3) Uani 1 1 d . . . . .
H8A H -0.087938 0.329342 0.201245 0.138 Uiso 1 1 calc R U . . .
H8B H 0.041358 0.431356 0.355741 0.138 Uiso 1 1 calc R U . . .
H8C H 0.038255 0.273412 0.296264 0.138 Uiso 1 1 calc R U . . .
Li1 Li 0.3952(11) 0.4083(9) 0.3695(9) 0.0366(17) Uani 1 1 d . . . . .
C10 C 0.2348(11) 0.1586(9) 0.1314(9) 0.057(3) Uani 0.762(19) 1 d D . P A 1
H10A H 0.226711 0.084499 0.045544 0.068 Uiso 0.762(19) 1 calc R U P A 1
H10B H 0.189561 0.117584 0.178054 0.068 Uiso 0.762(19) 1 calc R U P A 1
C10' C 0.286(3) 0.217(4) 0.092(2) 0.071(10) Uiso 0.238(19) 1 d D . P A 2
H10C H 0.332925 0.273592 0.058824 0.085 Uiso 0.238(19) 1 calc R U P A 2
H10D H 0.257376 0.121116 0.023342 0.085 Uiso 0.238(19) 1 calc R U P A 2
C11' C 0.421(7) 0.117(4) 0.261(6) 0.085(15) Uiso 0.238(19) 1 d D . P A 2
H11D H 0.489912 0.062169 0.224974 0.128 Uiso 0.238(19) 1 calc R U P A 2
H11E H 0.307301 0.061284 0.219370 0.128 Uiso 0.238(19) 1 calc R U P A 2
H11F H 0.468238 0.151028 0.361259 0.128 Uiso 0.238(19) 1 calc R U P A 2
C12' C 0.577(4) 0.274(4) 0.215(4) 0.065(9) Uiso 0.238(19) 1 d D . P A 2
H12D H 0.673142 0.290587 0.300480 0.097 Uiso 0.238(19) 1 calc R U P A 2
H12E H 0.578052 0.356479 0.201864 0.097 Uiso 0.238(19) 1 calc R U P A 2
H12F H 0.582770 0.200500 0.136836 0.097 Uiso 0.238(19) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 6 0.0980
0 -6 -1 0.1112
1 7 -3 0.1901
-5 1 1 0.0428
1 -1 -6 0.0124
2 1 5 0.0777
4 1 1 0.0803
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
C5 W1 C6 91.0(2) . . ?
C5 W1 C2 88.9(2) . . ?
C5 W1 C3 179.4(2) . . ?
C1 W1 C5 90.5(2) . . ?
C1 W1 C6 177.2(2) . . ?
C1 W1 C4 91.0(3) . . ?
C1 W1 C2 93.4(2) . . ?
C1 W1 C3 89.6(2) . . ?
C4 W1 C5 88.0(2) . . ?
C4 W1 C6 86.7(2) . . ?
C4 W1 C2 174.6(2) . . ?
C4 W1 C3 92.6(2) . . ?
C2 W1 C6 88.9(2) . . ?
C3 W1 C6 88.8(2) . . ?
C3 W1 C2 90.5(2) . . ?
C6 N1 Li1 140.5(5) . . ?
C6 N1 Li1 137.9(5) . 2_666 ?
Li1 N1 Li1 81.6(4) . 2_666 ?
C11 N3 Li1 115.1(6) . . ?
C11 N3 C10 106.8(7) . . ?
C12 N3 C11 108.3(8) . . ?
C12 N3 Li1 113.8(6) . . ?
C12 N3 C10 110.7(7) . . ?
C10 N3 Li1 101.6(5) . . ?
C10' N3 Li1 102.9(12) . . ?
C10' N3 C12' 102.5(19) . . ?
C11' N3 Li1 114(2) . . ?
C11' N3 C10' 119(3) . . ?
C11' N3 C12' 110(3) . . ?
C12' N3 Li1 106.1(15) . . ?
O5 C5 W1 178.2(5) . . ?
N1 C6 W1 178.2(5) . . ?
C9 N2 Li1 102.9(5) . . ?
C7 N2 C9 108.4(7) . . ?
C7 N2 Li1 111.8(6) . . ?
C8 N2 C9 113.2(8) . . ?
C8 N2 C7 108.9(7) . . ?
C8 N2 Li1 111.5(6) . . ?
O1 C1 W1 178.6(6) . . ?
O4 C4 W1 176.3(5) . . ?
O2 C2 W1 178.7(5) . . ?
O3 C3 W1 178.5(6) . . ?
N2 C9 H9AA 109.0 . . ?
N2 C9 H9AB 109.0 . . ?
N2 C9 H9BC 107.8 . . ?
N2 C9 H9BD 107.8 . . ?
H9AA C9 H9AB 107.8 . . ?
H9BC C9 H9BD 107.1 . . ?
C10 C9 N2 113.0(7) . . ?
C10 C9 H9AA 109.0 . . ?
C10 C9 H9AB 109.0 . . ?
C10' C9 N2 118.0(14) . . ?
C10' C9 H9BC 107.8 . . ?
C10' C9 H9BD 107.8 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 Li1 N1 98.4(4) . 2_666 ?
N1 Li1 N3 116.2(4) 2_666 . ?
N1 Li1 N3 117.4(5) . . ?
N1 Li1 N2 120.0(5) 2_666 . ?
N1 Li1 N2 118.2(5) . . ?
N1 Li1 Li1 49.5(3) . 2_666 ?
N1 Li1 Li1 48.9(3) 2_666 2_666 ?
N3 Li1 N2 88.3(4) . . ?
N3 Li1 Li1 133.6(6) . 2_666 ?
N2 Li1 Li1 138.1(6) . 2_666 ?
N3 C10 H10A 109.4 . . ?
N3 C10 H10B 109.4 . . ?
C9 C10 N3 111.0(7) . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N3 C10' H10C 108.4 . . ?
N3 C10' H10D 108.4 . . ?
C9 C10' N3 115.5(16) . . ?
C9 C10' H10C 108.4 . . ?
C9 C10' H10D 108.4 . . ?
H10C C10' H10D 107.5 . . ?
N3 C11' H11D 109.5 . . ?
N3 C11' H11E 109.5 . . ?
N3 C11' H11F 109.5 . . ?
H11D C11' H11E 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
N3 C12' H12D 109.5 . . ?
N3 C12' H12E 109.5 . . ?
N3 C12' H12F 109.5 . . ?
H12D C12' H12E 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 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
W1 C5 2.038(5) . ?
W1 C6 2.161(5) . ?
W1 C1 1.995(6) . ?
W1 C4 2.035(6) . ?
W1 C2 2.066(6) . ?
W1 C3 2.062(5) . ?
O5 C5 1.133(7) . ?
O4 C4 1.136(8) . ?
O2 C2 1.121(8) . ?
O3 C3 1.130(7) . ?
O1 C1 1.167(7) . ?
N1 C6 1.166(7) . ?
N1 Li1 2.025(9) . ?
N1 Li1 2.044(10) 2_666 ?
N3 C11 1.469(9) . ?
N3 C12 1.453(10) . ?
N3 Li1 2.046(10) . ?
N3 C10 1.493(10) . ?
N3 C10' 1.460(19) . ?
N3 C11' 1.46(2) . ?
N3 C12' 1.489(19) . ?
N2 C9 1.488(11) . ?
N2 C7 1.468(10) . ?
N2 C8 1.445(9) . ?
N2 Li1 2.078(10) . ?
C9 H9AA 0.9700 . ?
C9 H9AB 0.9700 . ?
C9 H9BC 0.9700 . ?
C9 H9BD 0.9700 . ?
C9 C10 1.452(12) . ?
C9 C10' 1.41(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
Li1 Li1 2.660(17) 2_666 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C11' H11F 0.9600 . ?
C12' H12D 0.9600 . ?
C12' H12E 0.9600 . ?
C12' H12F 0.9600 . ?
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
N2 C9 C10 N3 -55.3(10) . . . . ?
N2 C9 C10' N3 39(3) . . . . ?
C7 N2 C9 C10 150.4(8) . . . . ?
C7 N2 C9 C10' 102.4(18) . . . . ?
C11 N3 C10 C9 166.3(8) . . . . ?
C12 N3 C10 C9 -75.9(9) . . . . ?
C8 N2 C9 C10 -88.7(9) . . . . ?
C8 N2 C9 C10' -136.6(17) . . . . ?
Li1 N3 C10 C9 45.3(9) . . . . ?
Li1 N3 C10' C9 -37(3) . . . . ?
Li1 N2 C9 C10 31.8(9) . . . . ?
Li1 N2 C9 C10' -16.1(18) . . . . ?
C11' N3 C10' C9 91(4) . . . . ?
C12' N3 C10' C9 -147(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.6969 0.4155 6.2875 0.7926 -0.6070 0.0574
-0.2194 -5.6642 -1.0093 -0.4475 0.3449 -0.8251
0.7585 6.8484 -3.0784 0.0154 -0.0146 0.9998
-5.4856 0.9322 0.9935 -0.6857 -0.7239 -0.0754
0.6736 -0.6085 -6.1837 -0.7910 0.6058 -0.0856
1.7066 0.7953 4.5894 0.9534 -0.2272 0.1985
4.4828 0.6744 1.0285 0.8876 0.3695 0.2750
