#------------------------------------------------------------------------------
#$Date: 2021-12-21 01:55:10 +0200 (Tue, 21 Dec 2021) $
#$Revision: 271549 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/91/7709116.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_7709116
loop_
_publ_author_name
'Hüttenschmidt, Mareike'
'Lange, Helge'
'Cordero, Miguel A. Argüello'
'Villinger, Alexander'
'Lochbrunner, Stefan'
'Seidel, Wolfram Willy'
_publ_section_title
;
 Development and application of redox-active cyclometallating ligands
 based on W(II) alkyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02393D
_journal_year                    2022
_chemical_formula_moiety
'C34 H41 B I N6 O P W, 0.3(C H2 Cl2), 0.5(C5 H12)'
_chemical_formula_sum            'C36.8 H47.61 B Cl0.61 I N6 O P W'
_chemical_formula_weight         964.06
_chemical_name_systematic
Carbonyl-iodido-tris{hydrido(3,4,5-trimethylpyrazolyl)borato}-(η2-C,C?-2-propinyldiphenylphosphine)-tungsten(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.482(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.299(16)
_cell_length_b                   10.596(4)
_cell_length_c                   16.986(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      2.28
_cell_volume                     7785(5)
_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 0.938
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             3806
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.691
_refine_diff_density_min         -2.094
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.00029(3)
_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   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         14069
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0527
_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)+(0.0369P)²+173.9951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10616
_reflns_number_total             14069
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_hl255b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C36.80 H47.61 B Cl0.61 I N6 O P W'
_cod_database_code               7709116
_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   0.361
_shelx_estimated_absorpt_t_max   0.698
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C35 C 0.2649(7) 0.928(3) -0.054(2) 0.107(9) Uiso 0.5 1 d D U P A -1
H35A H 0.2850 0.9707 -0.0444 0.160 Uiso 0.5 1 calc R U P A -1
H35B H 0.2586 0.9044 -0.1107 0.160 Uiso 0.5 1 calc R U P A -1
H35C H 0.2495 0.9851 -0.0396 0.160 Uiso 0.5 1 calc R U P A -1
C36 C 0.2675(5) 0.807(2) -0.0005(16) 0.064(5) Uiso 0.5 1 d D U P A -1
H36A H 0.2841 0.7547 -0.0145 0.077 Uiso 0.5 1 calc R U P A -1
H36B H 0.2750 0.8348 0.0561 0.077 Uiso 0.5 1 calc R U P A -1
C37 C 0.2401(5) 0.722(2) -0.0019(16) 0.061(4) Uiso 0.5 1 d D U P A -1
H37A H 0.2347 0.6848 -0.0567 0.073 Uiso 0.5 1 calc R U P A -1
H37B H 0.2226 0.7774 0.0031 0.073 Uiso 0.5 1 calc R U P A -1
C38 C 0.2400(4) 0.614(2) 0.0563(13) 0.061(5) Uiso 0.5 1 d D U P A -1
H38A H 0.2428 0.6511 0.1108 0.073 Uiso 0.5 1 calc R U P A -1
H38B H 0.2586 0.5623 0.0559 0.073 Uiso 0.5 1 calc R U P A -1
C39 C 0.2121(5) 0.521(2) 0.0463(15) 0.069(6) Uiso 0.5 1 d D U P A -1
H39A H 0.2163 0.4576 0.0895 0.104 Uiso 0.5 1 calc R U P A -1
H39B H 0.1933 0.5677 0.0492 0.104 Uiso 0.5 1 calc R U P A -1
H39C H 0.2092 0.4783 -0.0061 0.104 Uiso 0.5 1 calc R U P A -1
C40 C 0.5016(9) 0.889(2) 0.7729(18) 0.051(4) Uani 0.303(6) 1 d . U P B -1
H40A H 0.4841 0.8355 0.7796 0.062 Uiso 0.303(6) 1 calc R U P B -1
H40B H 0.5176 0.8331 0.7598 0.062 Uiso 0.303(6) 1 calc R U P B -1
Cl1 Cl 0.51645(19) 0.9597(7) 0.8630(7) 0.053(2) Uani 0.303(6) 1 d . U P B -1
Cl2 Cl 0.4887(2) 0.9882(10) 0.6906(7) 0.069(3) Uani 0.303(6) 1 d . U P B -1
W1 W 0.38771(2) 0.42738(2) 0.38198(2) 0.02061(7) Uani 1 1 d . . . . .
I1 I 0.41792(2) 0.28597(4) 0.28255(3) 0.03002(11) Uani 1 1 d . . . . .
P1 P 0.32087(4) 0.56822(15) 0.23553(9) 0.0224(3) Uani 1 1 d . . . . .
O1 O 0.37555(13) 0.1804(5) 0.4705(3) 0.0393(12) Uani 1 1 d . . . . .
N1 N 0.40670(12) 0.5987(5) 0.3305(3) 0.0225(10) Uani 1 1 d . . . . .
N2 N 0.42015(12) 0.6923(5) 0.3812(3) 0.0235(10) Uani 1 1 d . . . . .
N3 N 0.43296(13) 0.4386(5) 0.4701(3) 0.0276(11) Uani 1 1 d . . . . .
N4 N 0.44311(13) 0.5557(5) 0.5009(3) 0.0273(11) Uani 1 1 d . . . . .
N5 N 0.37605(12) 0.5545(4) 0.4721(3) 0.0217(9) Uani 1 1 d . . . . .
N6 N 0.39262(12) 0.6629(5) 0.4938(3) 0.0231(10) Uani 1 1 d . . . . .
B1 B 0.42465(17) 0.6772(7) 0.4726(4) 0.0258(13) Uani 1 1 d . . . . .
H1 H 0.4357 0.7524 0.5007 0.031 Uiso 1 1 calc R U . . .
C1 C 0.34663(14) 0.4731(6) 0.3068(4) 0.0241(11) Uani 1 1 d . . . . .
C2 C 0.34403(15) 0.3591(6) 0.3386(4) 0.0248(11) Uani 1 1 d . . . . .
C3 C 0.38094(16) 0.2742(6) 0.4387(4) 0.0283(13) Uani 1 1 d . . . . .
C4 C 0.32094(18) 0.2561(7) 0.3316(5) 0.0361(15) Uani 1 1 d . . . . .
H4A H 0.3038 0.2833 0.3557 0.054 Uiso 1 1 calc R U . . .
H4B H 0.3307 0.1811 0.3600 0.054 Uiso 1 1 calc R U . . .
H4C H 0.3130 0.2358 0.2746 0.054 Uiso 1 1 calc R U . . .
C5 C 0.28625(15) 0.5723(6) 0.2796(4) 0.0258(11) Uani 1 1 d . . . . .
C6 C 0.28038(16) 0.6629(7) 0.3331(4) 0.0315(14) Uani 1 1 d . . . . .
H6 H 0.2951 0.7280 0.3502 0.038 Uiso 1 1 calc R U . . .
C7 C 0.25322(18) 0.6604(8) 0.3626(5) 0.0377(16) Uani 1 1 d . . . . .
H7 H 0.2495 0.7234 0.3992 0.045 Uiso 1 1 calc R U . . .
C8 C 0.23170(18) 0.5645(8) 0.3377(6) 0.0410(17) Uani 1 1 d . . . . .
H8 H 0.2133 0.5617 0.3577 0.049 Uiso 1 1 calc R U . . .
C9 C 0.23710(19) 0.4747(9) 0.2847(6) 0.048(2) Uani 1 1 d . . . . .
H9 H 0.2224 0.4093 0.2682 0.058 Uiso 1 1 calc R U . . .
C10 C 0.26396(17) 0.4780(7) 0.2544(5) 0.0363(15) Uani 1 1 d . . . . .
H10 H 0.2672 0.4162 0.2166 0.044 Uiso 1 1 calc R U . . .
C11 C 0.33570(15) 0.7286(6) 0.2498(4) 0.0250(12) Uani 1 1 d . . . . .
C12 C 0.34782(15) 0.7852(6) 0.3230(4) 0.0260(12) Uani 1 1 d . . . . .
H12 H 0.3493 0.7380 0.3712 0.031 Uiso 1 1 calc R U . . .
C13 C 0.35793(16) 0.9096(6) 0.3278(5) 0.0336(14) Uani 1 1 d . . . . .
H13 H 0.3657 0.9479 0.3786 0.040 Uiso 1 1 calc R U . . .
C14 C 0.35647(17) 0.9770(7) 0.2569(5) 0.0371(16) Uani 1 1 d . . . . .
H14 H 0.3640 1.0613 0.2594 0.045 Uiso 1 1 calc R U . . .
C15 C 0.34434(17) 0.9235(7) 0.1832(5) 0.0358(15) Uani 1 1 d . . . . .
H15 H 0.3429 0.9714 0.1353 0.043 Uiso 1 1 calc R U . . .
C16 C 0.33418(16) 0.7999(7) 0.1790(4) 0.0298(13) Uani 1 1 d . . . . .
H16 H 0.3261 0.7627 0.1279 0.036 Uiso 1 1 calc R U . . .
C17 C 0.40681(14) 0.6390(6) 0.2552(4) 0.0238(11) Uani 1 1 d . . . . .
C18 C 0.41986(15) 0.7602(7) 0.2567(5) 0.0315(14) Uani 1 1 d . . . . .
C19 C 0.42798(15) 0.7914(6) 0.3400(4) 0.0286(13) Uani 1 1 d . . . . .
C20 C 0.39400(16) 0.5690(7) 0.1792(4) 0.0300(13) Uani 1 1 d . . . . .
H20A H 0.3813 0.6262 0.1403 0.045 Uiso 1 1 calc R U . . .
H20B H 0.3813 0.4986 0.1907 0.045 Uiso 1 1 calc R U . . .
H20C H 0.4110 0.5364 0.1567 0.045 Uiso 1 1 calc R U . . .
C21 C 0.4241(2) 0.8377(8) 0.1886(5) 0.0428(18) Uani 1 1 d . . . . .
H21A H 0.4065 0.8252 0.1430 0.064 Uiso 1 1 calc R U . . .
H21B H 0.4432 0.8131 0.1727 0.064 Uiso 1 1 calc R U . . .
H21C H 0.4253 0.9269 0.2043 0.064 Uiso 1 1 calc R U . . .
C22 C 0.44156(19) 0.9109(7) 0.3776(5) 0.0381(16) Uani 1 1 d . . . . .
H22A H 0.4422 0.9733 0.3353 0.057 Uiso 1 1 calc R U . . .
H22B H 0.4626 0.8951 0.4084 0.057 Uiso 1 1 calc R U . . .
H22C H 0.4289 0.9433 0.4137 0.057 Uiso 1 1 calc R U . . .
C23 C 0.45303(16) 0.3527(7) 0.5125(4) 0.0304(13) Uani 1 1 d . . . . .
C24 C 0.47539(15) 0.4153(8) 0.5694(4) 0.0347(16) Uani 1 1 d . . . . .
C25 C 0.46839(16) 0.5420(8) 0.5614(4) 0.0327(15) Uani 1 1 d . . . . .
C26 C 0.45143(19) 0.2131(7) 0.4960(5) 0.0391(17) Uani 1 1 d . . . . .
H26A H 0.4724 0.1777 0.5077 0.059 Uiso 1 1 calc R U . . .
H26B H 0.4418 0.1984 0.4391 0.059 Uiso 1 1 calc R U . . .
H26C H 0.4391 0.1722 0.5302 0.059 Uiso 1 1 calc R U . . .
C27 C 0.50186(19) 0.3547(10) 0.6277(5) 0.051(2) Uani 1 1 d . . . . .
H27A H 0.5194 0.4133 0.6394 0.076 Uiso 1 1 calc R U . . .
H27B H 0.5081 0.2773 0.6038 0.076 Uiso 1 1 calc R U . . .
H27C H 0.4954 0.3340 0.6778 0.076 Uiso 1 1 calc R U . . .
C28 C 0.48444(18) 0.6508(10) 0.6083(5) 0.047(2) Uani 1 1 d . . . . .
H28A H 0.5048 0.6238 0.6387 0.070 Uiso 1 1 calc R U . . .
H28B H 0.4721 0.6812 0.6459 0.070 Uiso 1 1 calc R U . . .
H28C H 0.4869 0.7189 0.5713 0.070 Uiso 1 1 calc R U . . .
C29 C 0.35071(15) 0.5628(6) 0.5053(3) 0.0227(11) Uani 1 1 d . . . . .
C30 C 0.35101(15) 0.6764(6) 0.5465(4) 0.0259(12) Uani 1 1 d . . . . .
C31 C 0.37835(15) 0.7364(6) 0.5390(4) 0.0262(12) Uani 1 1 d . . . . .
C32 C 0.32643(16) 0.4630(6) 0.4969(4) 0.0286(13) Uani 1 1 d . . . . .
H32A H 0.3170 0.4649 0.5440 0.043 Uiso 1 1 calc R U . . .
H32B H 0.3358 0.3801 0.4932 0.043 Uiso 1 1 calc R U . . .
H32C H 0.3105 0.4785 0.4480 0.043 Uiso 1 1 calc R U . . .
C33 C 0.32760(19) 0.7242(7) 0.5913(5) 0.0389(17) Uani 1 1 d . . . . .
H33A H 0.3375 0.7355 0.6483 0.058 Uiso 1 1 calc R U . . .
H33B H 0.3107 0.6630 0.5864 0.058 Uiso 1 1 calc R U . . .
H33C H 0.3194 0.8052 0.5684 0.058 Uiso 1 1 calc R U . . .
C34 C 0.39076(18) 0.8619(6) 0.5722(4) 0.0331(14) Uani 1 1 d . . . . .
H34A H 0.3850 0.8768 0.6239 0.050 Uiso 1 1 calc R U . . .
H34B H 0.3821 0.9288 0.5341 0.050 Uiso 1 1 calc R U . . .
H34C H 0.4133 0.8621 0.5801 0.050 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'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 '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
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C35 121.6(14) . . ?
C37 C36 H36A 106.9 . . ?
C35 C36 H36A 106.9 . . ?
C37 C36 H36B 106.9 . . ?
C35 C36 H36B 106.9 . . ?
H36A C36 H36B 106.7 . . ?
C36 C37 C38 124.0(16) . . ?
C36 C37 H37A 106.3 . . ?
C38 C37 H37A 106.3 . . ?
C36 C37 H37B 106.3 . . ?
C38 C37 H37B 106.3 . . ?
H37A C37 H37B 106.4 . . ?
C37 C38 C39 121.4(14) . . ?
C37 C38 H38A 107.0 . . ?
C39 C38 H38A 107.0 . . ?
C37 C38 H38B 107.0 . . ?
C39 C38 H38B 107.0 . . ?
H38A C38 H38B 106.7 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Cl1 C40 Cl2 117.1(16) . . ?
Cl1 C40 H40A 108.0 . . ?
Cl2 C40 H40A 108.0 . . ?
Cl1 C40 H40B 108.0 . . ?
Cl2 C40 H40B 108.0 . . ?
H40A C40 H40B 107.3 . . ?
C3 W1 C1 107.2(3) . . ?
C3 W1 C2 69.4(3) . . ?
C1 W1 C2 38.2(2) . . ?
C3 W1 N5 94.7(2) . . ?
C1 W1 N5 88.8(2) . . ?
C2 W1 N5 97.0(2) . . ?
C3 W1 N3 85.6(3) . . ?
C1 W1 N3 163.1(2) . . ?
C2 W1 N3 154.5(2) . . ?
N5 W1 N3 79.10(19) . . ?
C3 W1 N1 167.1(2) . . ?
C1 W1 N1 85.6(2) . . ?
C2 W1 N1 123.2(2) . . ?
N5 W1 N1 86.56(18) . . ?
N3 W1 N1 82.0(2) . . ?
C3 W1 I1 89.86(19) . . ?
C1 W1 I1 103.10(17) . . ?
C2 W1 I1 97.55(17) . . ?
N5 W1 I1 165.44(14) . . ?
N3 W1 I1 87.49(14) . . ?
N1 W1 I1 85.97(13) . . ?
C1 P1 C11 106.1(3) . . ?
C1 P1 C5 101.8(3) . . ?
C11 P1 C5 103.4(3) . . ?
C17 N1 N2 106.1(5) . . ?
C17 N1 W1 134.5(4) . . ?
N2 N1 W1 119.3(4) . . ?
C19 N2 N1 111.5(5) . . ?
C19 N2 B1 128.0(6) . . ?
N1 N2 B1 120.5(5) . . ?
C23 N3 N4 106.1(5) . . ?
C23 N3 W1 135.0(5) . . ?
N4 N3 W1 118.2(4) . . ?
C25 N4 N3 109.8(6) . . ?
C25 N4 B1 128.4(6) . . ?
N3 N4 B1 121.5(5) . . ?
C29 N5 N6 106.0(5) . . ?
C29 N5 W1 132.1(4) . . ?
N6 N5 W1 120.8(4) . . ?
C31 N6 N5 110.4(5) . . ?
C31 N6 B1 130.2(5) . . ?
N5 N6 B1 119.0(5) . . ?
N2 B1 N6 108.8(5) . . ?
N2 B1 N4 110.3(5) . . ?
N6 B1 N4 107.3(5) . . ?
N2 B1 H1 110.1 . . ?
N6 B1 H1 110.1 . . ?
N4 B1 H1 110.1 . . ?
C2 C1 P1 133.3(5) . . ?
C2 C1 W1 71.1(4) . . ?
P1 C1 W1 155.6(4) . . ?
C1 C2 C4 138.6(6) . . ?
C1 C2 W1 70.7(4) . . ?
C4 C2 W1 150.5(5) . . ?
O1 C3 W1 176.8(7) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 118.3(6) . . ?
C6 C5 P1 124.9(5) . . ?
C10 C5 P1 116.8(5) . . ?
C5 C6 C7 121.3(7) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 119.3(7) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.7(7) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C5 120.4(7) . . ?
C9 C10 H10 119.8 . . ?
C5 C10 H10 119.8 . . ?
C12 C11 C16 118.3(6) . . ?
C12 C11 P1 125.8(5) . . ?
C16 C11 P1 116.0(5) . . ?
C11 C12 C13 121.5(6) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C14 118.9(7) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 120.9(7) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.8(7) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 120.6(7) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
N1 C17 C18 111.0(6) . . ?
N1 C17 C20 125.8(6) . . ?
C18 C17 C20 123.2(6) . . ?
C17 C18 C19 104.2(6) . . ?
C17 C18 C21 128.4(7) . . ?
C19 C18 C21 127.5(7) . . ?
N2 C19 C18 107.2(6) . . ?
N2 C19 C22 124.6(7) . . ?
C18 C19 C22 128.1(6) . . ?
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 . . ?
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 . . ?
N3 C23 C24 109.5(6) . . ?
N3 C23 C26 123.9(7) . . ?
C24 C23 C26 126.5(6) . . ?
C25 C24 C23 106.5(6) . . ?
C25 C24 C27 127.4(8) . . ?
C23 C24 C27 126.1(8) . . ?
N4 C25 C24 108.1(7) . . ?
N4 C25 C28 122.9(7) . . ?
C24 C25 C28 129.0(7) . . ?
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 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 110.2(5) . . ?
N5 C29 C32 123.7(5) . . ?
C30 C29 C32 126.1(6) . . ?
C29 C30 C31 105.2(5) . . ?
C29 C30 C33 127.9(6) . . ?
C31 C30 C33 126.9(6) . . ?
N6 C31 C30 108.2(6) . . ?
N6 C31 C34 123.3(6) . . ?
C30 C31 C34 128.5(6) . . ?
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 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
C35 C36 1.555(15) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.513(15) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.513(15) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.561(15) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 Cl1 1.70(3) . ?
C40 Cl2 1.74(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
W1 C3 1.944(7) . ?
W1 C1 2.043(6) . ?
W1 C2 2.048(6) . ?
W1 N5 2.183(5) . ?
W1 N3 2.231(6) . ?
W1 N1 2.255(5) . ?
W1 I1 2.8045(8) . ?
P1 C1 1.784(6) . ?
P1 C11 1.820(7) . ?
P1 C5 1.847(7) . ?
O1 C3 1.181(8) . ?
N1 C17 1.348(8) . ?
N1 N2 1.363(7) . ?
N2 C19 1.348(8) . ?
N2 B1 1.531(9) . ?
N3 C23 1.364(8) . ?
N3 N4 1.383(8) . ?
N4 C25 1.354(8) . ?
N4 B1 1.545(9) . ?
N5 C29 1.364(8) . ?
N5 N6 1.370(7) . ?
N6 C31 1.343(8) . ?
N6 B1 1.545(9) . ?
B1 H1 1.0000 . ?
C1 C2 1.339(9) . ?
C2 C4 1.483(9) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.386(9) . ?
C5 C10 1.405(9) . ?
C6 C7 1.400(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.395(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.367(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(11) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.380(9) . ?
C11 C16 1.409(9) . ?
C12 C13 1.389(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.373(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(10) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.406(9) . ?
C17 C20 1.491(9) . ?
C18 C19 1.423(10) . ?
C18 C21 1.464(10) . ?
C19 C22 1.485(10) . ?
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 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.393(11) . ?
C23 C26 1.505(11) . ?
C24 C25 1.377(11) . ?
C24 C27 1.505(10) . ?
C25 C28 1.492(12) . ?
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 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.390(8) . ?
C29 C32 1.493(9) . ?
C30 C31 1.398(9) . ?
C30 C33 1.501(9) . ?
C31 C34 1.501(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
C35 C36 C37 C38 -171(4) . . . . ?
C36 C37 C38 C39 -174(2) . . . . ?
C17 N1 N2 C19 1.6(7) . . . . ?
W1 N1 N2 C19 -175.1(4) . . . . ?
C17 N1 N2 B1 -178.5(5) . . . . ?
W1 N1 N2 B1 4.8(7) . . . . ?
C23 N3 N4 C25 -1.0(7) . . . . ?
W1 N3 N4 C25 171.2(4) . . . . ?
C23 N3 N4 B1 -175.1(6) . . . . ?
W1 N3 N4 B1 -2.9(8) . . . . ?
C29 N5 N6 C31 0.1(6) . . . . ?
W1 N5 N6 C31 169.5(4) . . . . ?
C29 N5 N6 B1 174.0(5) . . . . ?
W1 N5 N6 B1 -16.7(7) . . . . ?
C19 N2 B1 N6 118.1(7) . . . . ?
N1 N2 B1 N6 -61.8(7) . . . . ?
C19 N2 B1 N4 -124.5(7) . . . . ?
N1 N2 B1 N4 55.6(7) . . . . ?
C31 N6 B1 N2 -117.8(7) . . . . ?
N5 N6 B1 N2 69.8(7) . . . . ?
C31 N6 B1 N4 122.9(7) . . . . ?
N5 N6 B1 N4 -49.6(7) . . . . ?
C25 N4 B1 N2 129.8(7) . . . . ?
N3 N4 B1 N2 -57.4(8) . . . . ?
C25 N4 B1 N6 -111.8(7) . . . . ?
N3 N4 B1 N6 61.0(7) . . . . ?
C11 P1 C1 C2 160.4(6) . . . . ?
C5 P1 C1 C2 52.5(7) . . . . ?
C11 P1 C1 W1 -24.4(9) . . . . ?
C5 P1 C1 W1 -132.3(9) . . . . ?
P1 C1 C2 C4 2.1(13) . . . . ?
W1 C1 C2 C4 -175.8(9) . . . . ?
P1 C1 C2 W1 177.9(6) . . . . ?
C1 P1 C5 C6 90.9(6) . . . . ?
C11 P1 C5 C6 -19.0(6) . . . . ?
C1 P1 C5 C10 -91.1(6) . . . . ?
C11 P1 C5 C10 158.9(5) . . . . ?
C10 C5 C6 C7 0.9(10) . . . . ?
P1 C5 C6 C7 178.8(6) . . . . ?
C5 C6 C7 C8 0.2(11) . . . . ?
C6 C7 C8 C9 -0.5(13) . . . . ?
C7 C8 C9 C10 -0.4(14) . . . . ?
C8 C9 C10 C5 1.5(14) . . . . ?
C6 C5 C10 C9 -1.7(11) . . . . ?
P1 C5 C10 C9 -179.8(7) . . . . ?
C1 P1 C11 C12 -40.2(6) . . . . ?
C5 P1 C11 C12 66.5(6) . . . . ?
C1 P1 C11 C16 140.4(5) . . . . ?
C5 P1 C11 C16 -113.0(5) . . . . ?
C16 C11 C12 C13 0.9(10) . . . . ?
P1 C11 C12 C13 -178.5(5) . . . . ?
C11 C12 C13 C14 -1.7(10) . . . . ?
C12 C13 C14 C15 2.1(11) . . . . ?
C13 C14 C15 C16 -1.8(11) . . . . ?
C14 C15 C16 C11 1.0(10) . . . . ?
C12 C11 C16 C15 -0.6(10) . . . . ?
P1 C11 C16 C15 178.9(5) . . . . ?
N2 N1 C17 C18 -1.0(7) . . . . ?
W1 N1 C17 C18 174.9(4) . . . . ?
N2 N1 C17 C20 -179.0(6) . . . . ?
W1 N1 C17 C20 -3.0(10) . . . . ?
N1 C17 C18 C19 0.2(7) . . . . ?
C20 C17 C18 C19 178.2(6) . . . . ?
N1 C17 C18 C21 -179.4(7) . . . . ?
C20 C17 C18 C21 -1.4(11) . . . . ?
N1 N2 C19 C18 -1.4(7) . . . . ?
B1 N2 C19 C18 178.7(6) . . . . ?
N1 N2 C19 C22 176.7(6) . . . . ?
B1 N2 C19 C22 -3.2(10) . . . . ?
C17 C18 C19 N2 0.7(7) . . . . ?
C21 C18 C19 N2 -179.6(7) . . . . ?
C17 C18 C19 C22 -177.3(7) . . . . ?
C21 C18 C19 C22 2.3(12) . . . . ?
N4 N3 C23 C24 0.3(7) . . . . ?
W1 N3 C23 C24 -170.0(5) . . . . ?
N4 N3 C23 C26 -177.0(6) . . . . ?
W1 N3 C23 C26 12.7(10) . . . . ?
N3 C23 C24 C25 0.5(8) . . . . ?
C26 C23 C24 C25 177.8(7) . . . . ?
N3 C23 C24 C27 -179.5(7) . . . . ?
C26 C23 C24 C27 -2.2(12) . . . . ?
N3 N4 C25 C24 1.4(8) . . . . ?
B1 N4 C25 C24 174.9(6) . . . . ?
N3 N4 C25 C28 -178.6(6) . . . . ?
B1 N4 C25 C28 -5.0(11) . . . . ?
C23 C24 C25 N4 -1.2(8) . . . . ?
C27 C24 C25 N4 178.8(7) . . . . ?
C23 C24 C25 C28 178.8(7) . . . . ?
C27 C24 C25 C28 -1.2(13) . . . . ?
N6 N5 C29 C30 1.0(7) . . . . ?
W1 N5 C29 C30 -166.6(4) . . . . ?
N6 N5 C29 C32 -179.5(5) . . . . ?
W1 N5 C29 C32 12.9(9) . . . . ?
N5 C29 C30 C31 -1.8(7) . . . . ?
C32 C29 C30 C31 178.8(6) . . . . ?
N5 C29 C30 C33 179.7(7) . . . . ?
C32 C29 C30 C33 0.2(11) . . . . ?
N5 N6 C31 C30 -1.2(7) . . . . ?
B1 N6 C31 C30 -174.2(6) . . . . ?
N5 N6 C31 C34 -179.9(6) . . . . ?
B1 N6 C31 C34 7.1(11) . . . . ?
C29 C30 C31 N6 1.8(7) . . . . ?
C33 C30 C31 N6 -179.6(7) . . . . ?
C29 C30 C31 C34 -179.6(7) . . . . ?
C33 C30 C31 C34 -1.0(12) . . . . ?
