#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:10:00 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272569 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/55/1565574.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_1565574
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         'C23 H32 B N6 O3 W +, B F4 -'
_chemical_formula_sum            'C23 H32 B2 F4 N6 O3 W'
_chemical_formula_weight         722.01
_chemical_name_systematic
'[Di(carbonyl)-η2-C,C?-ethinylmethylether-hydridotris(3,4,5-trimethylpyrazolyl)borato-tungsten(II)]-tetrafluoroborate'
_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
_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                98.4140(10)
_cell_angle_beta                 113.0510(10)
_cell_angle_gamma                92.1690(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3289(5)
_cell_length_b                   11.4973(5)
_cell_length_c                   13.0257(6)
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      2.86
_cell_volume                     1400.32(11)
_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 0.991
_diffrn_measured_fraction_theta_max 0.996
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            77362
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.000
_diffrn_reflns_theta_min         2.856
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.187
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_refine_diff_density_max         3.019
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         11395
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0224
_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)+(0.0185P)²+2.2366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10575
_reflns_number_total             11395
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc06149f2.cif
_cod_data_source_block           is_dw012
_cod_depositor_comments
'Adding full bibliography for 1565569--1565576.cif.'
_cod_database_code               1565574
_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   0.376
_shelx_estimated_absorpt_t_max   0.473
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 0.80832(2) 0.25381(2) 0.66319(2) 0.01625(2) Uani 1 1 d . . . . .
O1 O 0.60897(19) 0.05624(15) 0.45977(16) 0.0322(4) Uani 1 1 d . . . . .
O2 O 1.12908(18) 0.22576(17) 0.80568(16) 0.0322(4) Uani 1 1 d . . . . .
O3 O 0.9116(2) 0.40758(17) 0.51852(18) 0.0375(4) Uani 1 1 d . . . . .
N1 N 0.59395(17) 0.31194(15) 0.59415(14) 0.0190(3) Uani 1 1 d . . . . .
N2 N 0.52460(17) 0.33815(15) 0.66427(14) 0.0183(3) Uani 1 1 d . . . . .
N3 N 0.84450(16) 0.41865(14) 0.78723(14) 0.0170(3) Uani 1 1 d . . . . .
N4 N 0.73885(17) 0.44557(14) 0.82338(14) 0.0166(3) Uani 1 1 d . . . . .
N5 N 0.73621(17) 0.17718(14) 0.77693(14) 0.0180(3) Uani 1 1 d . . . . .
N6 N 0.65844(17) 0.23820(14) 0.82684(14) 0.0184(3) Uani 1 1 d . . . . .
C1 C 0.7242(2) 0.11631(18) 0.53608(18) 0.0225(3) Uani 1 1 d . . . . .
C2 C 0.8645(2) 0.11308(18) 0.58251(19) 0.0242(4) Uani 1 1 d . . . . .
H2 H 0.9412 0.0716 0.5795 0.029 Uiso 1 1 calc R U . . .
C3 C 0.6280(3) -0.0512(2) 0.3955(3) 0.0419(6) Uani 1 1 d . . . . .
H3A H 0.5353 -0.0936 0.3458 0.063 Uiso 1 1 calc R U . . .
H3B H 0.6831 -0.1015 0.4478 0.063 Uiso 1 1 calc R U . . .
H3C H 0.6785 -0.0308 0.3496 0.063 Uiso 1 1 calc R U . . .
C4 C 1.0133(2) 0.23630(18) 0.75552(18) 0.0226(3) Uani 1 1 d . . . . .
C5 C 0.8739(2) 0.35368(18) 0.56940(19) 0.0237(4) Uani 1 1 d . . . . .
C6 C 0.5010(2) 0.31829(18) 0.48847(17) 0.0211(3) Uani 1 1 d . . . . .
C7 C 0.3712(2) 0.34572(18) 0.49051(18) 0.0228(4) Uani 1 1 d . . . . .
C8 C 0.3900(2) 0.35837(18) 0.60280(18) 0.0213(3) Uani 1 1 d . . . . .
C9 C 0.5347(3) 0.3018(2) 0.38628(19) 0.0300(4) Uani 1 1 d . . . . .
H9A H 0.4718 0.2357 0.3303 0.045 Uiso 1 1 calc R U . . .
H9B H 0.6332 0.2846 0.4079 0.045 Uiso 1 1 calc R U . . .
H9C H 0.5212 0.3741 0.3534 0.045 Uiso 1 1 calc R U . . .
C10 C 0.2422(3) 0.3599(2) 0.3900(2) 0.0342(5) Uani 1 1 d . . . . .
H10A H 0.2565 0.4338 0.3649 0.051 Uiso 1 1 calc R U . . .
H10B H 0.1606 0.3620 0.4106 0.051 Uiso 1 1 calc R U . . .
H10C H 0.2249 0.2932 0.3284 0.051 Uiso 1 1 calc R U . . .
C11 C 0.2869(2) 0.3872(3) 0.6549(2) 0.0338(5) Uani 1 1 d . . . . .
H11A H 0.1911 0.3782 0.5952 0.051 Uiso 1 1 calc R U . . .
H11B H 0.3104 0.4689 0.6958 0.051 Uiso 1 1 calc R U . . .
H11C H 0.2916 0.3334 0.7078 0.051 Uiso 1 1 calc R U . . .
C12 C 0.94492(19) 0.51258(16) 0.83246(16) 0.0175(3) Uani 1 1 d . . . . .
C13 C 0.9029(2) 0.59920(16) 0.89622(16) 0.0183(3) Uani 1 1 d . . . . .
C14 C 0.7725(2) 0.55411(16) 0.88817(15) 0.0175(3) Uani 1 1 d . . . . .
C15 C 1.0770(2) 0.52301(19) 0.8123(2) 0.0242(4) Uani 1 1 d . . . . .
H15A H 1.0882 0.4468 0.7735 0.036 Uiso 1 1 calc R U . . .
H15B H 1.1584 0.5459 0.8850 0.036 Uiso 1 1 calc R U . . .
H15C H 1.0711 0.5832 0.7651 0.036 Uiso 1 1 calc R U . . .
C16 C 0.9842(2) 0.71617(18) 0.95859(18) 0.0252(4) Uani 1 1 d . . . . .
H16A H 1.0134 0.7552 0.9079 0.038 Uiso 1 1 calc R U . . .
H16B H 1.0681 0.7042 1.0239 0.038 Uiso 1 1 calc R U . . .
H16C H 0.9243 0.7658 0.9848 0.038 Uiso 1 1 calc R U . . .
C17 C 0.6749(2) 0.61076(19) 0.93561(19) 0.0255(4) Uani 1 1 d . . . . .
H17A H 0.5845 0.6167 0.8735 0.038 Uiso 1 1 calc R U . . .
H17B H 0.7176 0.6900 0.9778 0.038 Uiso 1 1 calc R U . . .
H17C H 0.6588 0.5627 0.9865 0.038 Uiso 1 1 calc R U . . .
C18 C 0.7612(2) 0.07609(17) 0.8199(2) 0.0238(4) Uani 1 1 d . . . . .
C19 C 0.7000(3) 0.0730(2) 0.8984(2) 0.0302(5) Uani 1 1 d . . . . .
C20 C 0.6370(2) 0.17733(19) 0.9011(2) 0.0261(4) Uani 1 1 d . . . . .
C21 C 0.8421(3) -0.0146(2) 0.7851(3) 0.0372(6) Uani 1 1 d . . . . .
H21A H 0.7921 -0.0464 0.7041 0.056 Uiso 1 1 calc R U . . .
H21B H 0.8510 -0.0788 0.8286 0.056 Uiso 1 1 calc R U . . .
H21C H 0.9365 0.0216 0.7998 0.056 Uiso 1 1 calc R U . . .
C22 C 0.7034(4) -0.0222(3) 0.9665(3) 0.0539(9) Uani 1 1 d . . . . .
H22A H 0.6375 -0.0906 0.9177 0.081 Uiso 1 1 calc R U . . .
H22B H 0.6756 0.0078 1.0285 0.081 Uiso 1 1 calc R U . . .
H22C H 0.7994 -0.0460 0.9980 0.081 Uiso 1 1 calc R U . . .
C23 C 0.5596(4) 0.2217(3) 0.9738(3) 0.0497(9) Uani 1 1 d . . . . .
H23A H 0.5844 0.3071 1.0000 0.074 Uiso 1 1 calc R U . . .
H23B H 0.5868 0.1814 1.0394 0.074 Uiso 1 1 calc R U . . .
H23C H 0.4574 0.2053 0.9293 0.074 Uiso 1 1 calc R U . . .
B1 B 0.6080(2) 0.35619(19) 0.79263(18) 0.0180(3) Uani 1 1 d . . . . .
H1 H 0.5478 0.3872 0.8326 0.027 Uiso 1 1 calc R U . . .
B2A B 0.8930(5) 0.1416(3) 0.3167(4) 0.0377(8) Uani 0.794(4) 1 d D U P A 1
F1A F 0.8685(3) 0.0186(2) 0.2842(3) 0.0530(7) Uani 0.794(4) 1 d D . P A 1
F2A F 0.7768(3) 0.1828(3) 0.3297(3) 0.0597(8) Uani 0.794(4) 1 d D . P A 1
F3A F 1.0085(3) 0.1668(3) 0.4210(2) 0.0645(8) Uani 0.794(4) 1 d D . P A 1
F4A F 0.9216(3) 0.1894(2) 0.2361(3) 0.0506(7) Uani 0.794(4) 1 d D . P A 1
B2B B 0.8198(14) 0.1439(12) 0.2734(12) 0.062(3) Uiso 0.206(4) 1 d D U P A 2
F1B F 0.9016(17) 0.0729(16) 0.3481(14) 0.109(4) Uiso 0.206(4) 1 d D U P A 2
F2B F 0.6813(11) 0.0998(11) 0.2223(10) 0.075(3) Uiso 0.206(4) 1 d D U P A 2
F3B F 0.8395(19) 0.2541(13) 0.3405(14) 0.112(4) Uiso 0.206(4) 1 d D U P A 2
F4B F 0.8718(16) 0.1508(14) 0.1925(12) 0.080(4) Uiso 0.206(4) 1 d D 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 0.0033 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'
F F 0.0171 0.0103 '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'
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
C1 W1 C4 110.02(9) . . ?
C1 W1 C2 38.84(9) . . ?
C4 W1 C2 71.83(9) . . ?
C1 W1 C5 93.94(8) . . ?
C4 W1 C5 88.60(9) . . ?
C2 W1 C5 86.17(8) . . ?
C1 W1 N5 94.43(7) . . ?
C4 W1 N5 93.02(7) . . ?
C2 W1 N5 103.36(7) . . ?
C5 W1 N5 170.36(7) . . ?
C1 W1 N1 84.04(8) . . ?
C4 W1 N1 165.92(7) . . ?
C2 W1 N1 122.21(8) . . ?
C5 W1 N1 91.31(7) . . ?
N5 W1 N1 84.81(6) . . ?
C1 W1 N3 165.09(8) . . ?
C4 W1 N3 84.84(7) . . ?
C2 W1 N3 155.92(8) . . ?
C5 W1 N3 87.40(7) . . ?
N5 W1 N3 83.29(6) . . ?
N1 W1 N3 81.09(6) . . ?
C1 O1 C3 115.8(2) . . ?
C6 N1 N2 106.52(16) . . ?
C6 N1 W1 133.53(13) . . ?
N2 N1 W1 119.59(12) . . ?
C8 N2 N1 109.91(16) . . ?
C8 N2 B1 130.20(16) . . ?
N1 N2 B1 119.32(15) . . ?
C12 N3 N4 106.44(15) . . ?
C12 N3 W1 135.22(12) . . ?
N4 N3 W1 117.97(11) . . ?
C14 N4 N3 109.66(15) . . ?
C14 N4 B1 128.92(15) . . ?
N3 N4 B1 121.38(15) . . ?
C18 N5 N6 106.85(15) . . ?
C18 N5 W1 132.19(13) . . ?
N6 N5 W1 120.77(12) . . ?
C20 N6 N5 109.83(16) . . ?
C20 N6 B1 130.38(16) . . ?
N5 N6 B1 119.77(15) . . ?
O1 C1 C2 141.5(2) . . ?
O1 C1 W1 146.60(17) . . ?
C2 C1 W1 71.70(13) . . ?
C1 C2 W1 69.46(12) . . ?
C1 C2 H2 145.3 . . ?
W1 C2 H2 145.3 . . ?
O1 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 W1 178.69(19) . . ?
O3 C5 W1 179.0(2) . . ?
N1 C6 C7 109.79(18) . . ?
N1 C6 C9 124.52(19) . . ?
C7 C6 C9 125.67(19) . . ?
C8 C7 C6 105.81(17) . . ?
C8 C7 C10 128.7(2) . . ?
C6 C7 C10 125.5(2) . . ?
N2 C8 C7 107.97(17) . . ?
N2 C8 C11 122.67(19) . . ?
C7 C8 C11 129.36(19) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 109.76(16) . . ?
N3 C12 C15 124.75(17) . . ?
C13 C12 C15 125.44(18) . . ?
C14 C13 C12 105.70(16) . . ?
C14 C13 C16 128.32(18) . . ?
C12 C13 C16 125.98(18) . . ?
N4 C14 C13 108.43(16) . . ?
N4 C14 C17 122.30(18) . . ?
C13 C14 C17 129.23(18) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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 . . ?
N5 C18 C19 109.61(18) . . ?
N5 C18 C21 122.85(19) . . ?
C19 C18 C21 127.5(2) . . ?
C20 C19 C18 105.59(18) . . ?
C20 C19 C22 127.1(2) . . ?
C18 C19 C22 127.3(2) . . ?
N6 C20 C19 108.11(18) . . ?
N6 C20 C23 123.60(19) . . ?
C19 C20 C23 128.3(2) . . ?
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 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
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 . . ?
N2 B1 N6 109.39(16) . . ?
N2 B1 N4 107.69(15) . . ?
N6 B1 N4 108.82(15) . . ?
N2 B1 H1 110.3 . . ?
N6 B1 H1 110.3 . . ?
N4 B1 H1 110.3 . . ?
F2A B2A F4A 112.0(3) . . ?
F2A B2A F3A 108.9(3) . . ?
F4A B2A F3A 110.6(3) . . ?
F2A B2A F1A 108.8(3) . . ?
F4A B2A F1A 108.9(3) . . ?
F3A B2A F1A 107.6(3) . . ?
F2B B2B F4B 109.3(11) . . ?
F2B B2B F3B 112.1(11) . . ?
F4B B2B F3B 110.2(12) . . ?
F2B B2B F1B 111.9(11) . . ?
F4B B2B F1B 108.6(11) . . ?
F3B B2B F1B 104.5(12) . . ?
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 C1 2.000(2) . ?
W1 C4 2.019(2) . ?
W1 C2 2.028(2) . ?
W1 C5 2.066(2) . ?
W1 N5 2.1731(16) . ?
W1 N1 2.2107(16) . ?
W1 N3 2.2179(16) . ?
O1 C1 1.300(3) . ?
O1 C3 1.452(3) . ?
O2 C4 1.138(3) . ?
O3 C5 1.131(3) . ?
N1 C6 1.350(3) . ?
N1 N2 1.373(2) . ?
N2 C8 1.354(2) . ?
N2 B1 1.529(3) . ?
N3 C12 1.356(2) . ?
N3 N4 1.376(2) . ?
N4 C14 1.349(2) . ?
N4 B1 1.548(3) . ?
N5 C18 1.353(2) . ?
N5 N6 1.370(2) . ?
N6 C20 1.353(3) . ?
N6 B1 1.536(3) . ?
C1 C2 1.339(3) . ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C6 C7 1.399(3) . ?
C6 C9 1.491(3) . ?
C7 C8 1.382(3) . ?
C7 C10 1.493(3) . ?
C8 C11 1.493(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 1.394(3) . ?
C12 C15 1.490(3) . ?
C13 C14 1.384(3) . ?
C13 C16 1.495(3) . ?
C14 C17 1.497(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.400(3) . ?
C18 C21 1.489(3) . ?
C19 C20 1.389(3) . ?
C19 C22 1.500(3) . ?
C20 C23 1.509(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
B1 H1 1.0000 . ?
B2A F2A 1.368(4) . ?
B2A F4A 1.376(4) . ?
B2A F3A 1.394(6) . ?
B2A F1A 1.399(4) . ?
B2B F2B 1.359(10) . ?
B2B F4B 1.367(10) . ?
B2B F3B 1.388(10) . ?
B2B F1B 1.403(10) . ?
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
C6 N1 N2 C8 1.1(2) . . . . ?
W1 N1 N2 C8 -172.97(13) . . . . ?
C6 N1 N2 B1 -171.10(17) . . . . ?
W1 N1 N2 B1 14.9(2) . . . . ?
C12 N3 N4 C14 0.7(2) . . . . ?
W1 N3 N4 C14 -173.31(12) . . . . ?
C12 N3 N4 B1 -177.35(16) . . . . ?
W1 N3 N4 B1 8.6(2) . . . . ?
C18 N5 N6 C20 1.0(2) . . . . ?
W1 N5 N6 C20 -174.60(14) . . . . ?
C18 N5 N6 B1 -177.86(18) . . . . ?
W1 N5 N6 B1 6.6(2) . . . . ?
C3 O1 C1 C2 -2.7(4) . . . . ?
C3 O1 C1 W1 -174.2(2) . . . . ?
O1 C1 C2 W1 -175.1(3) . . . . ?
N2 N1 C6 C7 -1.4(2) . . . . ?
W1 N1 C6 C7 171.41(14) . . . . ?
N2 N1 C6 C9 176.9(2) . . . . ?
W1 N1 C6 C9 -10.2(3) . . . . ?
N1 C6 C7 C8 1.3(2) . . . . ?
C9 C6 C7 C8 -177.1(2) . . . . ?
N1 C6 C7 C10 -179.8(2) . . . . ?
C9 C6 C7 C10 1.8(4) . . . . ?
N1 N2 C8 C7 -0.3(2) . . . . ?
B1 N2 C8 C7 170.77(19) . . . . ?
N1 N2 C8 C11 179.0(2) . . . . ?
B1 N2 C8 C11 -10.0(3) . . . . ?
C6 C7 C8 N2 -0.6(2) . . . . ?
C10 C7 C8 N2 -179.5(2) . . . . ?
C6 C7 C8 C11 -179.8(2) . . . . ?
C10 C7 C8 C11 1.3(4) . . . . ?
N4 N3 C12 C13 -0.5(2) . . . . ?
W1 N3 C12 C13 172.05(13) . . . . ?
N4 N3 C12 C15 -177.99(18) . . . . ?
W1 N3 C12 C15 -5.4(3) . . . . ?
N3 C12 C13 C14 0.1(2) . . . . ?
C15 C12 C13 C14 177.55(18) . . . . ?
N3 C12 C13 C16 -179.47(18) . . . . ?
C15 C12 C13 C16 -2.0(3) . . . . ?
N3 N4 C14 C13 -0.7(2) . . . . ?
B1 N4 C14 C13 177.19(17) . . . . ?
N3 N4 C14 C17 177.02(17) . . . . ?
B1 N4 C14 C17 -5.1(3) . . . . ?
C12 C13 C14 N4 0.4(2) . . . . ?
C16 C13 C14 N4 179.92(18) . . . . ?
C12 C13 C14 C17 -177.13(19) . . . . ?
C16 C13 C14 C17 2.4(3) . . . . ?
N6 N5 C18 C19 -0.5(3) . . . . ?
W1 N5 C18 C19 174.35(16) . . . . ?
N6 N5 C18 C21 179.4(2) . . . . ?
W1 N5 C18 C21 -5.7(4) . . . . ?
N5 C18 C19 C20 -0.1(3) . . . . ?
C21 C18 C19 C20 179.9(3) . . . . ?
N5 C18 C19 C22 -179.4(3) . . . . ?
C21 C18 C19 C22 0.7(5) . . . . ?
N5 N6 C20 C19 -1.1(3) . . . . ?
B1 N6 C20 C19 177.6(2) . . . . ?
N5 N6 C20 C23 177.7(3) . . . . ?
B1 N6 C20 C23 -3.6(4) . . . . ?
C18 C19 C20 N6 0.7(3) . . . . ?
C22 C19 C20 N6 180.0(3) . . . . ?
C18 C19 C20 C23 -178.0(3) . . . . ?
C22 C19 C20 C23 1.3(5) . . . . ?
C8 N2 B1 N6 122.0(2) . . . . ?
N1 N2 B1 N6 -67.6(2) . . . . ?
C8 N2 B1 N4 -119.8(2) . . . . ?
N1 N2 B1 N4 50.5(2) . . . . ?
C20 N6 B1 N2 -123.6(2) . . . . ?
N5 N6 B1 N2 55.0(2) . . . . ?
C20 N6 B1 N4 119.0(2) . . . . ?
N5 N6 B1 N4 -62.4(2) . . . . ?
C14 N4 B1 N2 116.8(2) . . . . ?
N3 N4 B1 N2 -65.5(2) . . . . ?
C14 N4 B1 N6 -124.73(19) . . . . ?
N3 N4 B1 N6 53.0(2) . . . . ?
