#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:10:00 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272569 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/55/1565572.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_1565572
loop_
_publ_author_name
'Timmermann, Christopher'
'Thiem, Paula'
'Wanitschke, Dominik'
'Hüttenschmidt, Mareike'
'Romischke, Johanna'
'Villinger, Alexander'
'Seidel, Wolfram W.'
_publ_section_title
;
 Migratory insertion of isocyanide into a ketenyl-tungsten bond as key
 step in cyclization reactions.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              123
_journal_page_last               132
_journal_paper_doi               10.1039/d1sc06149f
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C33 H44 B N7 O4 W, 0.625(C H2 Cl2)'
_chemical_formula_sum            'C33.62 H45.25 B Cl1.25 N7 O4 W'
_chemical_formula_weight         850.49
_chemical_name_systematic
'[Di(carbonyl)-κ2-C,O-{(E)-3-(2,6-dimethyphenylamino)-1-ethoxyprop-1-en-3-ylidene-1-olate}-hydridotris(3,4,5-trimethylpyrazolyl)borato-tungsten(II)]'
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.658(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8806(4)
_cell_length_b                   22.4324(8)
_cell_length_c                   17.6641(7)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.90
_cell_measurement_theta_min      2.33
_cell_volume                     3769.9(3)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            111517
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.325
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             1713
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The unit cell contains 2.5 dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         2.679
_refine_diff_density_min         -5.315
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         13607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+12.7003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11878
_reflns_number_total             13607
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc06149f2.cif
_cod_data_source_block           is_ct1801
_cod_depositor_comments
'Adding full bibliography for 1565569--1565576.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565572
_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   0.582
_shelx_estimated_absorpt_t_max   0.700
_platon_squeeze_void_probe_radius 1.20
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
B1 B 0.7366(4) 0.24135(15) 0.67553(19) 0.0188(6) Uani 1 1 d . . . . .
H1 H 0.8184 0.2141 0.6799 0.023 Uiso 1 1 calc R U . . .
N1 N 0.2186(3) 0.42885(12) 0.59695(15) 0.0186(5) Uani 1 1 d . . . . .
N2 N 0.4891(3) 0.23556(11) 0.68731(15) 0.0183(5) Uani 1 1 d . . . . .
N3 N 0.6116(3) 0.20645(11) 0.68920(15) 0.0184(5) Uani 1 1 d . . . . .
N4 N 0.6830(3) 0.33635(12) 0.73589(14) 0.0183(4) Uani 1 1 d . . . . .
N5 N 0.7771(3) 0.29177(12) 0.73609(15) 0.0180(5) Uani 1 1 d . . . . .
N6 N 0.5732(3) 0.30461(11) 0.56815(14) 0.0173(5) Uani 1 1 d . . . . .
N7 N 0.6893(3) 0.26848(11) 0.59183(14) 0.0175(5) Uani 1 1 d . . . . .
O1 O 0.4361(2) 0.33037(10) 0.77116(12) 0.0200(4) Uani 1 1 d . . . . .
O2 O 0.3367(3) 0.36728(11) 0.86287(13) 0.0278(5) Uani 1 1 d . . . . .
O3 O 0.5429(3) 0.45633(12) 0.60044(18) 0.0354(6) Uani 1 1 d . . . . .
O4 O 0.1932(3) 0.29390(13) 0.52873(16) 0.0333(6) Uani 1 1 d . . . . .
W1 W 0.46320(2) 0.33293(2) 0.65673(2) 0.01510(4) Uani 1 1 d . . . . .
C1 C 0.2966(3) 0.39669(13) 0.65915(17) 0.0165(5) Uani 1 1 d . . . . .
C2 C 0.2699(3) 0.40376(14) 0.73255(18) 0.0214(6) Uani 1 1 d . . . . .
H2 H 0.2037 0.4314 0.7423 0.026 Uiso 1 1 calc R U . . .
C3 C 0.3490(3) 0.36659(14) 0.78880(17) 0.0200(6) Uani 1 1 d . . . . .
C4 C 0.1126(3) 0.47120(14) 0.60105(17) 0.0187(5) Uani 1 1 d . . . . .
C5 C 0.1400(3) 0.53163(15) 0.59197(19) 0.0235(6) Uani 1 1 d . . . . .
C6 C 0.0368(4) 0.57324(17) 0.5959(2) 0.0332(8) Uani 1 1 d . . . . .
H6 H 0.0520 0.6143 0.5879 0.040 Uiso 1 1 calc R U . . .
C7 C -0.0870(4) 0.55530(19) 0.6111(2) 0.0363(9) Uani 1 1 d . . . . .
H7 H -0.1546 0.5842 0.6159 0.044 Uiso 1 1 calc R U . . .
C8 C -0.1125(4) 0.4958(2) 0.6193(2) 0.0353(8) Uani 1 1 d . . . . .
H8 H -0.1983 0.4841 0.6295 0.042 Uiso 1 1 calc R U . . .
C9 C -0.0148(3) 0.45193(16) 0.6131(2) 0.0253(6) Uani 1 1 d . . . . .
C10 C 0.2765(4) 0.55161(17) 0.5784(3) 0.0349(8) Uani 1 1 d . . . . .
H10A H 0.2900 0.5319 0.5315 0.052 Uiso 1 1 calc R U . . .
H10B H 0.3541 0.5410 0.6241 0.052 Uiso 1 1 calc R U . . .
H10C H 0.2747 0.5949 0.5709 0.052 Uiso 1 1 calc R U . . .
C11 C -0.0498(4) 0.38734(18) 0.6173(3) 0.0382(9) Uani 1 1 d . . . . .
H11A H -0.1520 0.3825 0.6043 0.057 Uiso 1 1 calc R U . . .
H11B H -0.0074 0.3725 0.6706 0.057 Uiso 1 1 calc R U . . .
H11C H -0.0127 0.3648 0.5798 0.057 Uiso 1 1 calc R U . . .
C12 C 0.4240(4) 0.32585(18) 0.91782(19) 0.0318(8) Uani 1 1 d . . . . .
H12A H 0.5245 0.3335 0.9222 0.038 Uiso 1 1 calc R U . . .
H12B H 0.4019 0.2844 0.8995 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3947(5) 0.3346(2) 0.9954(2) 0.0411(10) Uani 1 1 d . . . . .
H13A H 0.2943 0.3286 0.9898 0.062 Uiso 1 1 calc R U . . .
H13B H 0.4212 0.3752 1.0141 0.062 Uiso 1 1 calc R U . . .
H13C H 0.4493 0.3059 1.0332 0.062 Uiso 1 1 calc R U . . .
C14 C 0.5075(3) 0.41121(15) 0.6206(2) 0.0230(6) Uani 1 1 d . . . . .
C15 C 0.2923(3) 0.30985(14) 0.57616(19) 0.0220(6) Uani 1 1 d . . . . .
C16 C 0.3987(3) 0.19426(14) 0.69782(18) 0.0219(6) Uani 1 1 d . . . . .
C17 C 0.4612(4) 0.13794(15) 0.7063(2) 0.0268(7) Uani 1 1 d . . . . .
C18 C 0.5966(4) 0.14742(14) 0.70048(18) 0.0229(6) Uani 1 1 d . . . . .
C19 C 0.2528(4) 0.20910(19) 0.7012(3) 0.0376(9) Uani 1 1 d . . . . .
H19A H 0.2413 0.2525 0.7012 0.056 Uiso 1 1 calc R U . . .
H19B H 0.2367 0.1924 0.7493 0.056 Uiso 1 1 calc R U . . .
H19C H 0.1847 0.1921 0.6553 0.056 Uiso 1 1 calc R U . . .
C20 C 0.3947(5) 0.07992(18) 0.7178(3) 0.0428(10) Uani 1 1 d . . . . .
H20A H 0.3204 0.0702 0.6702 0.064 Uiso 1 1 calc R U . . .
H20B H 0.3542 0.0832 0.7625 0.064 Uiso 1 1 calc R U . . .
H20C H 0.4660 0.0484 0.7281 0.064 Uiso 1 1 calc R U . . .
C21 C 0.7111(5) 0.10349(17) 0.7040(3) 0.0378(9) Uani 1 1 d . . . . .
H21A H 0.7366 0.1039 0.6541 0.057 Uiso 1 1 calc R U . . .
H21B H 0.6786 0.0636 0.7133 0.057 Uiso 1 1 calc R U . . .
H21C H 0.7933 0.1141 0.7470 0.057 Uiso 1 1 calc R U . . .
C22 C 0.7459(3) 0.37506(15) 0.7920(2) 0.0243(6) Uani 1 1 d . . . . .
C23 C 0.8821(3) 0.35564(16) 0.8294(2) 0.0261(6) Uani 1 1 d . . . . .
C24 C 0.8973(3) 0.30256(15) 0.79244(18) 0.0221(6) Uani 1 1 d . . . . .
C25 C 0.6768(5) 0.43043(18) 0.8089(3) 0.0420(10) Uani 1 1 d . . . . .
H25A H 0.7340 0.4650 0.8034 0.063 Uiso 1 1 calc R U . . .
H25B H 0.6672 0.4288 0.8626 0.063 Uiso 1 1 calc R U . . .
H25C H 0.5835 0.4340 0.7717 0.063 Uiso 1 1 calc R U . . .
C26 C 0.9897(4) 0.3866(2) 0.8940(3) 0.0418(10) Uani 1 1 d . . . . .
H26A H 1.0565 0.4079 0.8716 0.063 Uiso 1 1 calc R U . . .
H26B H 1.0401 0.3571 0.9321 0.063 Uiso 1 1 calc R U . . .
H26C H 0.9425 0.4151 0.9204 0.063 Uiso 1 1 calc R U . . .
C27 C 1.0216(4) 0.2617(2) 0.8100(2) 0.0383(9) Uani 1 1 d . . . . .
H27A H 0.9963 0.2237 0.8299 0.057 Uiso 1 1 calc R U . . .
H27B H 1.0993 0.2800 0.8498 0.057 Uiso 1 1 calc R U . . .
H27C H 1.0505 0.2547 0.7619 0.057 Uiso 1 1 calc R U . . .
C28 C 0.5551(3) 0.31549(14) 0.49098(17) 0.0190(5) Uani 1 1 d . . . . .
C29 C 0.6587(3) 0.28593(14) 0.46460(17) 0.0189(5) Uani 1 1 d . . . . .
C30 C 0.7411(3) 0.25670(14) 0.52977(18) 0.0193(5) Uani 1 1 d . . . . .
C31 C 0.4393(4) 0.35331(17) 0.4429(2) 0.0292(7) Uani 1 1 d . . . . .
H31A H 0.4438 0.3536 0.3881 0.044 Uiso 1 1 calc R U . . .
H31B H 0.4495 0.3941 0.4635 0.044 Uiso 1 1 calc R U . . .
H31C H 0.3486 0.3371 0.4454 0.044 Uiso 1 1 calc R U . . .
C32 C 0.6749(4) 0.28314(16) 0.38256(19) 0.0268(7) Uani 1 1 d . . . . .
H32A H 0.6126 0.3126 0.3495 0.040 Uiso 1 1 calc R U . . .
H32B H 0.6500 0.2432 0.3609 0.040 Uiso 1 1 calc R U . . .
H32C H 0.7726 0.2919 0.3837 0.040 Uiso 1 1 calc R U . . .
C33 C 0.8668(4) 0.21848(18) 0.5350(2) 0.0320(8) Uani 1 1 d . . . . .
H33A H 0.8866 0.2170 0.4835 0.048 Uiso 1 1 calc R U . . .
H33B H 0.8484 0.1781 0.5509 0.048 Uiso 1 1 calc R U . . .
H33C H 0.9480 0.2352 0.5739 0.048 Uiso 1 1 calc R U . . .
H1A H 0.241(4) 0.4286(18) 0.555(2) 0.025(10) Uiso 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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 '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'
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
N5 B1 N3 109.6(2) . . ?
N5 B1 N7 109.3(2) . . ?
N3 B1 N7 107.6(2) . . ?
N5 B1 H1 110.1 . . ?
N3 B1 H1 110.1 . . ?
N7 B1 H1 110.1 . . ?
C1 N1 C4 124.9(3) . . ?
C1 N1 H1A 119(3) . . ?
C4 N1 H1A 115(3) . . ?
C16 N2 N3 106.6(2) . . ?
C16 N2 W1 132.2(2) . . ?
N3 N2 W1 120.82(18) . . ?
C18 N3 N2 109.8(3) . . ?
C18 N3 B1 130.3(3) . . ?
N2 N3 B1 119.8(2) . . ?
C22 N4 N5 107.1(2) . . ?
C22 N4 W1 131.4(2) . . ?
N5 N4 W1 121.35(19) . . ?
C24 N5 N4 109.5(2) . . ?
C24 N5 B1 131.2(3) . . ?
N4 N5 B1 119.3(2) . . ?
C28 N6 N7 106.6(2) . . ?
C28 N6 W1 134.6(2) . . ?
N7 N6 W1 118.70(17) . . ?
C30 N7 N6 109.6(2) . . ?
C30 N7 B1 127.8(2) . . ?
N6 N7 B1 122.3(2) . . ?
C3 O1 W1 118.86(18) . . ?
C3 O2 C12 116.7(2) . . ?
C14 W1 C15 102.96(13) . . ?
C14 W1 O1 115.73(12) . . ?
C15 W1 O1 112.39(11) . . ?
C14 W1 C1 69.86(11) . . ?
C15 W1 C1 71.47(12) . . ?
O1 W1 C1 73.07(9) . . ?
C14 W1 N6 80.33(11) . . ?
C15 W1 N6 84.41(11) . . ?
O1 W1 N6 151.42(8) . . ?
C1 W1 N6 135.44(10) . . ?
C14 W1 N4 84.77(11) . . ?
C15 W1 N4 163.68(11) . . ?
O1 W1 N4 75.86(9) . . ?
C1 W1 N4 124.85(10) . . ?
N6 W1 N4 82.75(9) . . ?
C14 W1 N2 158.26(11) . . ?
C15 W1 N2 86.43(12) . . ?
O1 W1 N2 77.24(9) . . ?
C1 W1 N2 131.87(10) . . ?
N6 W1 N2 81.15(9) . . ?
N4 W1 N2 81.68(9) . . ?
N1 C1 C2 118.6(3) . . ?
N1 C1 W1 126.4(2) . . ?
C2 C1 W1 115.0(2) . . ?
C3 C2 C1 112.9(3) . . ?
C3 C2 H2 123.5 . . ?
C1 C2 H2 123.5 . . ?
O1 C3 O2 119.1(3) . . ?
O1 C3 C2 120.0(3) . . ?
O2 C3 C2 120.9(3) . . ?
C5 C4 C9 121.7(3) . . ?
C5 C4 N1 118.1(3) . . ?
C9 C4 N1 120.2(3) . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 C10 120.5(3) . . ?
C4 C5 C10 121.1(3) . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 121.5(3) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 117.5(3) . . ?
C4 C9 C11 122.4(3) . . ?
C8 C9 C11 120.2(3) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 C13 107.6(3) . . ?
O2 C12 H12A 110.2 . . ?
C13 C12 H12A 110.2 . . ?
O2 C12 H12B 110.2 . . ?
C13 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 W1 175.4(3) . . ?
O4 C15 W1 177.3(3) . . ?
N2 C16 C17 110.5(3) . . ?
N2 C16 C19 122.6(3) . . ?
C17 C16 C19 126.8(3) . . ?
C18 C17 C16 105.1(3) . . ?
C18 C17 C20 127.7(3) . . ?
C16 C17 C20 127.2(3) . . ?
N3 C18 C17 107.9(3) . . ?
N3 C18 C21 122.8(3) . . ?
C17 C18 C21 129.3(3) . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 C23 110.1(3) . . ?
N4 C22 C25 123.0(3) . . ?
C23 C22 C25 127.0(3) . . ?
C24 C23 C22 105.0(3) . . ?
C24 C23 C26 127.6(3) . . ?
C22 C23 C26 127.4(3) . . ?
N5 C24 C23 108.4(3) . . ?
N5 C24 C27 123.6(3) . . ?
C23 C24 C27 128.0(3) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C28 C29 110.0(3) . . ?
N6 C28 C31 123.4(3) . . ?
C29 C28 C31 126.6(3) . . ?
C30 C29 C28 105.5(2) . . ?
C30 C29 C32 126.2(3) . . ?
C28 C29 C32 128.2(3) . . ?
N7 C30 C29 108.3(3) . . ?
N7 C30 C33 123.5(3) . . ?
C29 C30 C33 128.1(3) . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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
B1 N5 1.534(4) . ?
B1 N3 1.535(4) . ?
B1 N7 1.550(4) . ?
B1 H1 1.0000 . ?
N1 C1 1.366(4) . ?
N1 C4 1.430(4) . ?
N1 H1A 0.82(4) . ?
N2 C16 1.334(4) . ?
N2 N3 1.368(3) . ?
N2 W1 2.248(2) . ?
N3 C18 1.353(4) . ?
N4 C22 1.338(4) . ?
N4 N5 1.365(3) . ?
N4 W1 2.244(2) . ?
N5 C24 1.350(4) . ?
N6 C28 1.348(4) . ?
N6 N7 1.374(3) . ?
N6 W1 2.225(2) . ?
N7 C30 1.355(4) . ?
O1 C3 1.281(3) . ?
O1 W1 2.110(2) . ?
O2 C3 1.347(4) . ?
O2 C12 1.449(4) . ?
O3 C14 1.158(4) . ?
O4 C15 1.160(4) . ?
W1 C14 1.958(3) . ?
W1 C15 1.962(3) . ?
W1 C1 2.189(3) . ?
C1 C2 1.401(4) . ?
C2 C3 1.369(4) . ?
C2 H2 0.9500 . ?
C4 C5 1.400(4) . ?
C4 C9 1.401(4) . ?
C5 C6 1.397(5) . ?
C5 C10 1.501(5) . ?
C6 C7 1.382(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.373(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.404(5) . ?
C8 H8 0.9500 . ?
C9 C11 1.496(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.487(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C16 C17 1.396(5) . ?
C16 C19 1.497(5) . ?
C17 C18 1.386(5) . ?
C17 C20 1.496(5) . ?
C18 C21 1.489(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.399(5) . ?
C22 C25 1.486(5) . ?
C23 C24 1.385(5) . ?
C23 C26 1.504(5) . ?
C24 C27 1.496(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.400(4) . ?
C28 C31 1.492(4) . ?
C29 C30 1.383(4) . ?
C29 C32 1.502(4) . ?
C30 C33 1.491(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
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
C16 N2 N3 C18 0.3(3) . . . . ?
W1 N2 N3 C18 -173.4(2) . . . . ?
C16 N2 N3 B1 177.6(3) . . . . ?
W1 N2 N3 B1 4.0(3) . . . . ?
N5 B1 N3 C18 -125.8(3) . . . . ?
N7 B1 N3 C18 115.5(3) . . . . ?
N5 B1 N3 N2 57.5(3) . . . . ?
N7 B1 N3 N2 -61.3(3) . . . . ?
C22 N4 N5 C24 0.5(3) . . . . ?
W1 N4 N5 C24 -175.71(19) . . . . ?
C22 N4 N5 B1 -177.8(3) . . . . ?
W1 N4 N5 B1 6.0(3) . . . . ?
N3 B1 N5 C24 118.6(3) . . . . ?
N7 B1 N5 C24 -123.7(3) . . . . ?
N3 B1 N5 N4 -63.5(3) . . . . ?
N7 B1 N5 N4 54.2(3) . . . . ?
C28 N6 N7 C30 -0.7(3) . . . . ?
W1 N6 N7 C30 -179.61(19) . . . . ?
C28 N6 N7 B1 -174.4(3) . . . . ?
W1 N6 N7 B1 6.7(4) . . . . ?
N5 B1 N7 C30 124.4(3) . . . . ?
N3 B1 N7 C30 -116.7(3) . . . . ?
N5 B1 N7 N6 -63.2(3) . . . . ?
N3 B1 N7 N6 55.8(3) . . . . ?
C4 N1 C1 C2 2.0(5) . . . . ?
C4 N1 C1 W1 -178.5(2) . . . . ?
N1 C1 C2 C3 176.4(3) . . . . ?
W1 C1 C2 C3 -3.3(4) . . . . ?
W1 O1 C3 O2 -176.6(2) . . . . ?
W1 O1 C3 C2 3.6(4) . . . . ?
C12 O2 C3 O1 -0.4(5) . . . . ?
C12 O2 C3 C2 179.4(3) . . . . ?
C1 C2 C3 O1 -0.1(5) . . . . ?
C1 C2 C3 O2 -179.9(3) . . . . ?
C1 N1 C4 C5 110.2(3) . . . . ?
C1 N1 C4 C9 -70.4(4) . . . . ?
C9 C4 C5 C6 0.6(5) . . . . ?
N1 C4 C5 C6 180.0(3) . . . . ?
C9 C4 C5 C10 -179.5(3) . . . . ?
N1 C4 C5 C10 -0.1(5) . . . . ?
C4 C5 C6 C7 2.3(5) . . . . ?
C10 C5 C6 C7 -177.7(4) . . . . ?
C5 C6 C7 C8 -2.7(6) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
C5 C4 C9 C8 -2.9(5) . . . . ?
N1 C4 C9 C8 177.8(3) . . . . ?
C5 C4 C9 C11 175.7(3) . . . . ?
N1 C4 C9 C11 -3.7(5) . . . . ?
C7 C8 C9 C4 2.4(5) . . . . ?
C7 C8 C9 C11 -176.2(4) . . . . ?
C3 O2 C12 C13 179.4(3) . . . . ?
N3 N2 C16 C17 -0.2(3) . . . . ?
W1 N2 C16 C17 172.4(2) . . . . ?
N3 N2 C16 C19 178.6(3) . . . . ?
W1 N2 C16 C19 -8.8(5) . . . . ?
N2 C16 C17 C18 0.1(4) . . . . ?
C19 C16 C17 C18 -178.6(3) . . . . ?
N2 C16 C17 C20 -178.9(3) . . . . ?
C19 C16 C17 C20 2.4(6) . . . . ?
N2 N3 C18 C17 -0.2(3) . . . . ?
B1 N3 C18 C17 -177.2(3) . . . . ?
N2 N3 C18 C21 179.0(3) . . . . ?
B1 N3 C18 C21 2.0(5) . . . . ?
C16 C17 C18 N3 0.0(4) . . . . ?
C20 C17 C18 N3 179.0(4) . . . . ?
C16 C17 C18 C21 -179.1(3) . . . . ?
C20 C17 C18 C21 -0.1(6) . . . . ?
N5 N4 C22 C23 -0.1(4) . . . . ?
W1 N4 C22 C23 175.5(2) . . . . ?
N5 N4 C22 C25 179.1(3) . . . . ?
W1 N4 C22 C25 -5.3(5) . . . . ?
N4 C22 C23 C24 -0.2(4) . . . . ?
C25 C22 C23 C24 -179.4(4) . . . . ?
N4 C22 C23 C26 178.2(4) . . . . ?
C25 C22 C23 C26 -0.9(6) . . . . ?
N4 N5 C24 C23 -0.6(3) . . . . ?
B1 N5 C24 C23 177.4(3) . . . . ?
N4 N5 C24 C27 178.5(3) . . . . ?
B1 N5 C24 C27 -3.5(5) . . . . ?
C22 C23 C24 N5 0.5(4) . . . . ?
C26 C23 C24 N5 -178.0(4) . . . . ?
C22 C23 C24 C27 -178.6(4) . . . . ?
C26 C23 C24 C27 3.0(6) . . . . ?
N7 N6 C28 C29 0.6(3) . . . . ?
W1 N6 C28 C29 179.3(2) . . . . ?
N7 N6 C28 C31 -180.0(3) . . . . ?
W1 N6 C28 C31 -1.3(5) . . . . ?
N6 C28 C29 C30 -0.3(3) . . . . ?
C31 C28 C29 C30 -179.7(3) . . . . ?
N6 C28 C29 C32 176.8(3) . . . . ?
C31 C28 C29 C32 -2.6(5) . . . . ?
N6 N7 C30 C29 0.5(3) . . . . ?
B1 N7 C30 C29 173.8(3) . . . . ?
N6 N7 C30 C33 -179.7(3) . . . . ?
B1 N7 C30 C33 -6.5(5) . . . . ?
C28 C29 C30 N7 -0.2(3) . . . . ?
C32 C29 C30 N7 -177.3(3) . . . . ?
C28 C29 C30 C33 -179.9(3) . . . . ?
C32 C29 C30 C33 2.9(5) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.041 0.500 0.000 275 53 ' '
2 0.060 1.000 0.500 275 53 ' '
