#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:10:00 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272569 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/55/1565570.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_1565570
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         'C31 H40 B N7 O4 W, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C32.5 H43 B Cl3 N7 O4 W'
_chemical_formula_weight         896.75
_chemical_name_systematic
'[Di(carbonyl)-κ2-C,O-{3-(2,6-dimethylphenylamino)propan-3-ylidene-1-oate}-hydridotris(3,4,5-trimethylpyrazolyl)borato-tungsten(II)]'
_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   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                98.146(2)
_cell_angle_beta                 97.680(2)
_cell_angle_gamma                105.730(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9415(5)
_cell_length_b                   11.0539(6)
_cell_length_c                   17.5643(9)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.27
_cell_volume                     1808.92(16)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0467
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86328
_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         31.998
_diffrn_reflns_theta_min         2.274
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       needle
_exptl_crystal_F_000             898
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
The unit cell contains three dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. These were removed from the model, but included 
in the empirical formula.
;
_refine_diff_density_max         2.039
_refine_diff_density_min         -1.687
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         12545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0269P)²+1.6791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10776
_reflns_number_total             12545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc06149f2.cif
_cod_data_source_block           is_ct1734
_cod_depositor_comments
'Adding full bibliography for 1565569--1565576.cif.'
_cod_original_formula_sum        'C32.50 H43 B Cl3 N7 O4 W'
_cod_database_code               1565570
_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   0.377
_shelx_estimated_absorpt_t_max   0.819
_platon_squeeze_void_probe_radius 1.20
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
H1A H 0.780(4) 0.518(3) 0.3989(19) 0.031(9) Uiso 1 1 d . . . . .
W1 W 0.60113(2) 0.63920(2) 0.27633(2) 0.01563(3) Uani 1 1 d . . . . .
O1 O 0.72018(19) 0.82424(18) 0.27020(11) 0.0219(4) Uani 1 1 d . . . . .
O2 O 0.9157(2) 0.9902(2) 0.30572(13) 0.0297(5) Uani 1 1 d . . . . .
O3 O 0.7553(2) 0.4424(2) 0.21849(12) 0.0313(5) Uani 1 1 d . . . . .
O4 O 0.5286(2) 0.5708(2) 0.43484(13) 0.0364(5) Uani 1 1 d . . . . .
N1 N 0.8393(2) 0.6000(2) 0.39949(12) 0.0175(4) Uani 1 1 d . . . . .
N2 N 0.4473(2) 0.7507(2) 0.29139(12) 0.0176(4) Uani 1 1 d . . . . .
N3 N 0.3265(2) 0.7262(2) 0.23733(12) 0.0169(4) Uani 1 1 d . . . . .
N4 N 0.4051(2) 0.4747(2) 0.23993(13) 0.0192(4) Uani 1 1 d . . . . .
N5 N 0.2879(2) 0.4907(2) 0.19577(12) 0.0174(4) Uani 1 1 d . . . . .
N7 N 0.4093(2) 0.6437(2) 0.11781(12) 0.0165(4) Uani 1 1 d . . . . .
N6 N 0.5459(2) 0.6551(2) 0.15048(12) 0.0179(4) Uani 1 1 d . . . . .
B1 B 0.2915(3) 0.6167(3) 0.16647(16) 0.0170(5) Uani 1 1 d . . . . .
H1 H 0.1979 0.6087 0.1340 0.020 Uiso 1 1 calc R U . . .
C1 C 0.7925(3) 0.6761(2) 0.35636(14) 0.0168(5) Uani 1 1 d . . . . .
C2 C 0.8977(3) 0.8059(3) 0.36503(16) 0.0205(5) Uani 1 1 d . . . . .
H2A H 0.9894 0.7960 0.3537 0.025 Uiso 1 1 calc R U . . .
H2B H 0.9140 0.8517 0.4197 0.025 Uiso 1 1 calc R U . . .
C3 C 0.8452(3) 0.8840(3) 0.31049(15) 0.0196(5) Uani 1 1 d . . . . .
C4 C 0.6979(3) 0.5153(3) 0.24076(15) 0.0200(5) Uani 1 1 d . . . . .
C5 C 0.5592(3) 0.5934(3) 0.37680(16) 0.0227(5) Uani 1 1 d . . . . .
C6 C 0.9734(3) 0.6383(3) 0.45322(15) 0.0192(5) Uani 1 1 d . . . . .
C7 C 1.0912(3) 0.6112(3) 0.42745(16) 0.0212(5) Uani 1 1 d . . . . .
C8 C 1.2203(3) 0.6527(3) 0.47976(19) 0.0286(6) Uani 1 1 d . . . . .
H8 H 1.3019 0.6352 0.4640 0.034 Uiso 1 1 calc R U . . .
C9 C 1.2307(3) 0.7193(3) 0.55442(19) 0.0314(7) Uani 1 1 d . . . . .
H9 H 1.3196 0.7478 0.5891 0.038 Uiso 1 1 calc R U . . .
C10 C 1.1128(3) 0.7445(3) 0.57898(17) 0.0293(6) Uani 1 1 d . . . . .
H10 H 1.1215 0.7906 0.6302 0.035 Uiso 1 1 calc R U . . .
C11 C 0.9811(3) 0.7028(3) 0.52886(16) 0.0224(5) Uani 1 1 d . . . . .
C12 C 1.0803(3) 0.5405(3) 0.34625(17) 0.0288(6) Uani 1 1 d . . . . .
H12A H 1.0459 0.5869 0.3081 0.043 Uiso 1 1 calc R U . . .
H12B H 1.0138 0.4545 0.3391 0.043 Uiso 1 1 calc R U . . .
H12C H 1.1741 0.5340 0.3385 0.043 Uiso 1 1 calc R U . . .
C13 C 0.8532(3) 0.7274(3) 0.55668(17) 0.0321(7) Uani 1 1 d . . . . .
H13A H 0.8067 0.7678 0.5192 0.048 Uiso 1 1 calc R U . . .
H13B H 0.8826 0.7843 0.6079 0.048 Uiso 1 1 calc R U . . .
H13C H 0.7867 0.6462 0.5611 0.048 Uiso 1 1 calc R U . . .
C14 C 0.4464(3) 0.8462(3) 0.34714(15) 0.0188(5) Uani 1 1 d . . . . .
C15 C 0.3243(3) 0.8845(2) 0.32941(15) 0.0189(5) Uani 1 1 d . . . . .
C16 C 0.2517(3) 0.8065(2) 0.25894(15) 0.0178(5) Uani 1 1 d . . . . .
C17 C 0.5614(3) 0.8997(3) 0.41683(17) 0.0292(6) Uani 1 1 d . . . . .
H17A H 0.6235 0.8444 0.4194 0.044 Uiso 1 1 calc R U . . .
H17B H 0.5195 0.9040 0.4642 0.044 Uiso 1 1 calc R U . . .
H17C H 0.6171 0.9857 0.4128 0.044 Uiso 1 1 calc R U . . .
C18 C 0.2818(3) 0.9848(3) 0.37866(17) 0.0257(6) Uani 1 1 d . . . . .
H18A H 0.3597 1.0650 0.3907 0.039 Uiso 1 1 calc R U . . .
H18B H 0.2609 0.9569 0.4274 0.039 Uiso 1 1 calc R U . . .
H18C H 0.1971 0.9984 0.3501 0.039 Uiso 1 1 calc R U . . .
C19 C 0.1157(3) 0.8035(3) 0.21032(16) 0.0235(6) Uani 1 1 d . . . . .
H19A H 0.1322 0.8188 0.1582 0.035 Uiso 1 1 calc R U . . .
H19B H 0.0794 0.8703 0.2352 0.035 Uiso 1 1 calc R U . . .
H19C H 0.0459 0.7197 0.2055 0.035 Uiso 1 1 calc R U . . .
C20 C 0.3675(3) 0.3530(3) 0.25114(16) 0.0235(6) Uani 1 1 d . . . . .
C21 C 0.2278(3) 0.2900(3) 0.21339(16) 0.0241(6) Uani 1 1 d . . . . .
C22 C 0.1816(3) 0.3798(3) 0.17917(15) 0.0202(5) Uani 1 1 d . . . . .
C23 C 0.4632(3) 0.2974(3) 0.2990(2) 0.0354(7) Uani 1 1 d . . . . .
H23A H 0.4288 0.2039 0.2853 0.053 Uiso 1 1 calc R U . . .
H23B H 0.4636 0.3246 0.3546 0.053 Uiso 1 1 calc R U . . .
H23C H 0.5599 0.3275 0.2884 0.053 Uiso 1 1 calc R U . . .
C24 C 0.1467(3) 0.1518(3) 0.2083(2) 0.0354(7) Uani 1 1 d . . . . .
H24A H 0.0982 0.1147 0.1543 0.053 Uiso 1 1 calc R U . . .
H24B H 0.0762 0.1459 0.2428 0.053 Uiso 1 1 calc R U . . .
H24C H 0.2127 0.1047 0.2245 0.053 Uiso 1 1 calc R U . . .
C25 C 0.0407(3) 0.3647(3) 0.13070(18) 0.0293(6) Uani 1 1 d . . . . .
H25A H 0.0539 0.3818 0.0785 0.044 Uiso 1 1 calc R U . . .
H25B H -0.0034 0.4253 0.1557 0.044 Uiso 1 1 calc R U . . .
H25C H -0.0208 0.2772 0.1261 0.044 Uiso 1 1 calc R U . . .
C26 C 0.6241(3) 0.6750(3) 0.09382(15) 0.0185(5) Uani 1 1 d . . . . .
C27 C 0.5371(3) 0.6758(3) 0.02440(15) 0.0201(5) Uani 1 1 d . . . . .
C28 C 0.4022(3) 0.6555(2) 0.04197(14) 0.0177(5) Uani 1 1 d . . . . .
C29 C 0.7801(3) 0.6964(3) 0.10773(17) 0.0277(6) Uani 1 1 d . . . . .
H29A H 0.8132 0.6924 0.0576 0.042 Uiso 1 1 calc R U . . .
H29B H 0.8024 0.6301 0.1343 0.042 Uiso 1 1 calc R U . . .
H29C H 0.8276 0.7807 0.1405 0.042 Uiso 1 1 calc R U . . .
C30 C 0.5801(3) 0.6911(3) -0.05305(17) 0.0315(7) Uani 1 1 d . . . . .
H30A H 0.5823 0.6085 -0.0808 0.047 Uiso 1 1 calc R U . . .
H30B H 0.6747 0.7531 -0.0448 0.047 Uiso 1 1 calc R U . . .
H30C H 0.5114 0.7219 -0.0842 0.047 Uiso 1 1 calc R U . . .
C31 C 0.2675(3) 0.6501(3) -0.00915(16) 0.0283(6) Uani 1 1 d . . . . .
H31A H 0.2860 0.6618 -0.0615 0.042 Uiso 1 1 calc R U . . .
H31B H 0.2305 0.7182 0.0132 0.042 Uiso 1 1 calc R U . . .
H31C H 0.1974 0.5668 -0.0128 0.042 Uiso 1 1 calc R U . . .
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
C4 W1 C5 101.94(11) . . ?
C4 W1 O1 110.25(9) . . ?
C5 W1 O1 121.11(10) . . ?
C4 W1 C1 71.94(10) . . ?
C5 W1 C1 70.11(10) . . ?
O1 W1 C1 74.89(9) . . ?
C4 W1 N4 84.70(10) . . ?
C5 W1 N4 77.26(10) . . ?
O1 W1 N4 150.96(7) . . ?
C1 W1 N4 134.14(9) . . ?
C4 W1 N2 165.31(9) . . ?
C5 W1 N2 83.52(9) . . ?
O1 W1 N2 77.44(8) . . ?
C1 W1 N2 122.69(9) . . ?
N4 W1 N2 83.22(8) . . ?
C4 W1 N6 87.57(9) . . ?
C5 W1 N6 154.95(9) . . ?
O1 W1 N6 75.46(7) . . ?
C1 W1 N6 134.87(8) . . ?
N4 W1 N6 80.67(8) . . ?
N2 W1 N6 82.25(8) . . ?
C3 O1 W1 125.12(17) . . ?
C1 N1 C6 124.7(2) . . ?
C1 N1 H1A 119(2) . . ?
C6 N1 H1A 116(2) . . ?
C14 N2 N3 106.8(2) . . ?
C14 N2 W1 132.25(16) . . ?
N3 N2 W1 120.95(15) . . ?
C16 N3 N2 109.9(2) . . ?
C16 N3 B1 130.0(2) . . ?
N2 N3 B1 120.1(2) . . ?
C20 N4 N5 106.4(2) . . ?
C20 N4 W1 134.73(17) . . ?
N5 N4 W1 118.89(16) . . ?
C22 N5 N4 109.5(2) . . ?
C22 N5 B1 128.2(2) . . ?
N4 N5 B1 122.1(2) . . ?
C28 N7 N6 110.0(2) . . ?
C28 N7 B1 130.1(2) . . ?
N6 N7 B1 119.94(19) . . ?
C26 N6 N7 106.6(2) . . ?
C26 N6 W1 132.71(16) . . ?
N7 N6 W1 120.72(15) . . ?
N7 B1 N3 109.1(2) . . ?
N7 B1 N5 108.0(2) . . ?
N3 B1 N5 109.1(2) . . ?
N7 B1 H1 110.2 . . ?
N3 B1 H1 110.2 . . ?
N5 B1 H1 110.2 . . ?
N1 C1 C2 113.4(2) . . ?
N1 C1 W1 130.33(19) . . ?
C2 C1 W1 116.21(17) . . ?
C1 C2 C3 111.4(2) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 O1 125.2(2) . . ?
O2 C3 C2 122.5(2) . . ?
O1 C3 C2 112.4(2) . . ?
O3 C4 W1 178.9(2) . . ?
O4 C5 W1 175.7(2) . . ?
C11 C6 C7 122.3(2) . . ?
C11 C6 N1 118.7(2) . . ?
C7 C6 N1 119.0(2) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 120.7(2) . . ?
C6 C7 C12 121.5(2) . . ?
C9 C8 C7 120.7(3) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.4(3) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C6 118.1(3) . . ?
C10 C11 C13 120.1(3) . . ?
C6 C11 C13 121.9(2) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 C15 110.2(2) . . ?
N2 C14 C17 122.7(2) . . ?
C15 C14 C17 127.1(2) . . ?
C16 C15 C14 104.9(2) . . ?
C16 C15 C18 128.5(2) . . ?
C14 C15 C18 126.5(2) . . ?
N3 C16 C15 108.2(2) . . ?
N3 C16 C19 122.0(2) . . ?
C15 C16 C19 129.9(2) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 . . ?
N4 C20 C21 110.0(2) . . ?
N4 C20 C23 123.6(2) . . ?
C21 C20 C23 126.3(3) . . ?
C22 C21 C20 105.5(2) . . ?
C22 C21 C24 127.2(3) . . ?
C20 C21 C24 127.3(3) . . ?
N5 C22 C21 108.5(2) . . ?
N5 C22 C25 122.8(2) . . ?
C21 C22 C25 128.7(3) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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 . . ?
N6 C26 C27 109.9(2) . . ?
N6 C26 C29 122.6(2) . . ?
C27 C26 C29 127.4(2) . . ?
C28 C27 C26 105.3(2) . . ?
C28 C27 C30 127.3(2) . . ?
C26 C27 C30 127.4(2) . . ?
N7 C28 C27 108.3(2) . . ?
N7 C28 C31 122.7(2) . . ?
C27 C28 C31 129.0(2) . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
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 . . ?
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 C4 1.955(3) . ?
W1 C5 1.970(3) . ?
W1 O1 2.0929(19) . ?
W1 C1 2.113(2) . ?
W1 N4 2.220(2) . ?
W1 N2 2.229(2) . ?
W1 N6 2.249(2) . ?
O1 C3 1.292(3) . ?
O2 C3 1.214(3) . ?
O3 C4 1.161(3) . ?
O4 C5 1.144(3) . ?
N1 C1 1.340(3) . ?
N1 C6 1.446(3) . ?
N1 H1A 0.94(3) . ?
N2 C14 1.336(3) . ?
N2 N3 1.365(3) . ?
N3 C16 1.350(3) . ?
N3 B1 1.538(4) . ?
N4 C20 1.345(4) . ?
N4 N5 1.379(3) . ?
N5 C22 1.348(3) . ?
N5 B1 1.545(4) . ?
N7 C28 1.351(3) . ?
N7 N6 1.366(3) . ?
N7 B1 1.530(3) . ?
N6 C26 1.349(3) . ?
B1 H1 1.0000 . ?
C1 C2 1.502(4) . ?
C2 C3 1.510(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C6 C11 1.398(4) . ?
C6 C7 1.400(4) . ?
C7 C8 1.396(4) . ?
C7 C12 1.501(4) . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(4) . ?
C10 H10 0.9500 . ?
C11 C13 1.499(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.402(3) . ?
C14 C17 1.486(4) . ?
C15 C16 1.385(4) . ?
C15 C18 1.495(4) . ?
C16 C19 1.490(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.397(4) . ?
C20 C23 1.496(4) . ?
C21 C22 1.378(4) . ?
C21 C24 1.506(4) . ?
C22 C25 1.493(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.400(4) . ?
C26 C29 1.485(4) . ?
C27 C28 1.383(4) . ?
C27 C30 1.498(4) . ?
C28 C31 1.491(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
C14 N2 N3 C16 0.5(3) . . . . ?
W1 N2 N3 C16 -179.47(16) . . . . ?
C14 N2 N3 B1 -177.5(2) . . . . ?
W1 N2 N3 B1 2.6(3) . . . . ?
C20 N4 N5 C22 -1.1(3) . . . . ?
W1 N4 N5 C22 179.24(16) . . . . ?
C20 N4 N5 B1 -176.4(2) . . . . ?
W1 N4 N5 B1 3.9(3) . . . . ?
C28 N7 N6 C26 0.4(3) . . . . ?
B1 N7 N6 C26 178.4(2) . . . . ?
C28 N7 N6 W1 -179.47(16) . . . . ?
B1 N7 N6 W1 -1.5(3) . . . . ?
C28 N7 B1 N3 -122.1(3) . . . . ?
N6 N7 B1 N3 60.4(3) . . . . ?
C28 N7 B1 N5 119.6(3) . . . . ?
N6 N7 B1 N5 -58.0(3) . . . . ?
C16 N3 B1 N7 121.0(3) . . . . ?
N2 N3 B1 N7 -61.4(3) . . . . ?
C16 N3 B1 N5 -121.3(3) . . . . ?
N2 N3 B1 N5 56.2(3) . . . . ?
C22 N5 B1 N7 -116.9(3) . . . . ?
N4 N5 B1 N7 57.5(3) . . . . ?
C22 N5 B1 N3 124.7(3) . . . . ?
N4 N5 B1 N3 -60.9(3) . . . . ?
C6 N1 C1 C2 3.5(3) . . . . ?
C6 N1 C1 W1 -179.28(18) . . . . ?
N1 C1 C2 C3 175.3(2) . . . . ?
W1 C1 C2 C3 -2.3(3) . . . . ?
W1 O1 C3 O2 178.3(2) . . . . ?
W1 O1 C3 C2 -1.0(3) . . . . ?
C1 C2 C3 O2 -177.2(2) . . . . ?
C1 C2 C3 O1 2.1(3) . . . . ?
C1 N1 C6 C11 83.6(3) . . . . ?
C1 N1 C6 C7 -95.4(3) . . . . ?
C11 C6 C7 C8 -1.0(4) . . . . ?
N1 C6 C7 C8 178.0(2) . . . . ?
C11 C6 C7 C12 179.3(3) . . . . ?
N1 C6 C7 C12 -1.6(4) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C12 C7 C8 C9 179.2(3) . . . . ?
C7 C8 C9 C10 0.8(5) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C10 C11 C6 -1.6(4) . . . . ?
C9 C10 C11 C13 178.3(3) . . . . ?
C7 C6 C11 C10 2.0(4) . . . . ?
N1 C6 C11 C10 -177.0(2) . . . . ?
C7 C6 C11 C13 -177.9(3) . . . . ?
N1 C6 C11 C13 3.1(4) . . . . ?
N3 N2 C14 C15 -0.1(3) . . . . ?
W1 N2 C14 C15 179.90(18) . . . . ?
N3 N2 C14 C17 179.7(3) . . . . ?
W1 N2 C14 C17 -0.3(4) . . . . ?
N2 C14 C15 C16 -0.4(3) . . . . ?
C17 C14 C15 C16 179.9(3) . . . . ?
N2 C14 C15 C18 177.5(3) . . . . ?
C17 C14 C15 C18 -2.2(5) . . . . ?
N2 N3 C16 C15 -0.7(3) . . . . ?
B1 N3 C16 C15 177.0(2) . . . . ?
N2 N3 C16 C19 178.9(2) . . . . ?
B1 N3 C16 C19 -3.4(4) . . . . ?
C14 C15 C16 N3 0.7(3) . . . . ?
C18 C15 C16 N3 -177.2(3) . . . . ?
C14 C15 C16 C19 -178.9(3) . . . . ?
C18 C15 C16 C19 3.2(5) . . . . ?
N5 N4 C20 C21 1.0(3) . . . . ?
W1 N4 C20 C21 -179.45(19) . . . . ?
N5 N4 C20 C23 -177.7(3) . . . . ?
W1 N4 C20 C23 1.8(4) . . . . ?
N4 C20 C21 C22 -0.5(3) . . . . ?
C23 C20 C21 C22 178.1(3) . . . . ?
N4 C20 C21 C24 177.2(3) . . . . ?
C23 C20 C21 C24 -4.2(5) . . . . ?
N4 N5 C22 C21 0.8(3) . . . . ?
B1 N5 C22 C21 175.8(2) . . . . ?
N4 N5 C22 C25 -178.7(2) . . . . ?
B1 N5 C22 C25 -3.8(4) . . . . ?
C20 C21 C22 N5 -0.2(3) . . . . ?
C24 C21 C22 N5 -177.9(3) . . . . ?
C20 C21 C22 C25 179.3(3) . . . . ?
C24 C21 C22 C25 1.6(5) . . . . ?
N7 N6 C26 C27 -0.3(3) . . . . ?
W1 N6 C26 C27 179.53(18) . . . . ?
N7 N6 C26 C29 178.0(2) . . . . ?
W1 N6 C26 C29 -2.2(4) . . . . ?
N6 C26 C27 C28 0.1(3) . . . . ?
C29 C26 C27 C28 -178.1(3) . . . . ?
N6 C26 C27 C30 -178.2(3) . . . . ?
C29 C26 C27 C30 3.7(5) . . . . ?
N6 N7 C28 C27 -0.3(3) . . . . ?
B1 N7 C28 C27 -178.1(2) . . . . ?
N6 N7 C28 C31 -178.7(2) . . . . ?
B1 N7 C28 C31 3.5(4) . . . . ?
C26 C27 C28 N7 0.1(3) . . . . ?
C30 C27 C28 N7 178.4(3) . . . . ?
C26 C27 C28 C31 178.4(3) . . . . ?
C30 C27 C28 C31 -3.3(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 -0.034 0.000 0.000 316 117 ' '
