#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:11:00 +0300 (Fri, 05 May 2023) $
#$Revision: 283291 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/19/7711907.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_7711907
loop_
_publ_author_name
'Ludwig, Stephan'
'Hamann, Friederike M.'
'Helmdach, Kai'
'Villinger, Alexander'
'Seidel, Wolfram W.'
_publ_section_title
;
 Tuning the potential of redox-active diphosphine ligands based on the
 alkyne complexes
 [Tp*W(CO)L{η²-C₂(PPh₂)₂}].
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              326
_journal_page_last               337
_journal_paper_doi               10.1039/d2dt02794a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C45 H48 B Br I2 N6 O P2 Pd W, 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H52 B Br Cl4 I2 N6 O P2 Pd W'
_chemical_formula_weight         1555.45
_chemical_name_systematic
Carbonyl-bromido-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II){\m-\h2-\k1-\k1-bis(diphenylphosphanylethyne)}]-diiodidopalladium(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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-11-02 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.596(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7620(7)
_cell_length_b                   15.7369(10)
_cell_length_c                   27.1915(16)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      33.66
_cell_measurement_theta_min      2.31
_cell_volume                     5367.9(6)
_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_detector_area_resol_mean 10.4167
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            119210
_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         30.999
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.671
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.163
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         17111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0331
_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)+(0.0273P)²+15.6170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13826
_reflns_number_total             17111
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           is_fh052
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7711907
_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   0.284
_shelx_estimated_absorpt_t_max   0.736
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 0.4122(3) 0.1584(2) 0.24097(14) 0.0174(7) Uani 1 1 d . . . . .
H1 H 0.3335 0.1631 0.2289 0.026 Uiso 1 1 calc R U . . .
Br1 Br 0.76981(3) 0.02123(2) 0.25299(2) 0.02178(7) Uani 1 1 d . . . . .
N1 N 0.5437(2) 0.05376(17) 0.28692(10) 0.0149(5) Uani 1 1 d . . . . .
N2 N 0.4394(2) 0.07431(17) 0.26821(10) 0.0155(5) Uani 1 1 d . . . . .
N3 N 0.5808(2) 0.15453(17) 0.20373(10) 0.0158(5) Uani 1 1 d . . . . .
N4 N 0.4713(2) 0.16118(18) 0.19649(10) 0.0161(5) Uani 1 1 d . . . . .
N5 N 0.5597(2) 0.24739(17) 0.28893(10) 0.0140(5) Uani 1 1 d . . . . .
N6 N 0.4523(2) 0.23237(17) 0.27628(10) 0.0149(5) Uani 1 1 d . . . . .
O1 O 0.8280(2) 0.27353(17) 0.24254(10) 0.0256(5) Uani 1 1 d . . . . .
P1 P 0.89817(7) 0.22504(5) 0.38626(3) 0.01624(16) Uani 1 1 d . . . . .
P2 P 0.70160(7) 0.13991(5) 0.42266(3) 0.01466(15) Uani 1 1 d . . . . .
Pd1 Pd 0.84217(2) 0.21870(2) 0.46132(2) 0.01667(5) Uani 1 1 d . . . . .
W1 W 0.67229(2) 0.14747(2) 0.28145(2) 0.01214(3) Uani 1 1 d . . . . .
I1 I 1.01010(2) 0.30594(2) 0.50849(2) 0.02811(6) Uani 1 1 d . . . . .
I2 I 0.76900(2) 0.19060(2) 0.54425(2) 0.02795(6) Uani 1 1 d . . . . .
C1 C 0.7842(2) 0.1859(2) 0.34140(11) 0.0142(6) Uani 1 1 d . . . . .
C2 C 0.7112(2) 0.1391(2) 0.35733(11) 0.0144(6) Uani 1 1 d . . . . .
C3 C 0.7716(3) 0.2269(2) 0.25695(12) 0.0186(6) Uani 1 1 d . . . . .
C4 C 0.9492(3) 0.3226(2) 0.36391(14) 0.0219(7) Uani 1 1 d . . . . .
C5 C 0.9245(3) 0.4004(2) 0.38391(15) 0.0253(8) Uani 1 1 d . . . . .
H5 H 0.8838 0.4017 0.4099 0.030 Uiso 1 1 calc R U . . .
C6 C 0.9594(3) 0.4755(3) 0.36586(17) 0.0331(9) Uani 1 1 d . . . . .
H6 H 0.9437 0.5283 0.3798 0.040 Uiso 1 1 calc R U . . .
C7 C 1.0180(3) 0.4733(3) 0.32704(19) 0.0362(10) Uani 1 1 d . . . . .
H7 H 1.0417 0.5248 0.3145 0.043 Uiso 1 1 calc R U . . .
C8 C 1.0409(3) 0.3973(3) 0.30731(17) 0.0327(9) Uani 1 1 d . . . . .
H8 H 1.0794 0.3963 0.2806 0.039 Uiso 1 1 calc R U . . .
C9 C 1.0087(3) 0.3215(3) 0.32583(15) 0.0254(8) Uani 1 1 d . . . . .
H9 H 1.0273 0.2689 0.3126 0.031 Uiso 1 1 calc R U . . .
C10 C 0.9932(3) 0.1415(2) 0.38029(13) 0.0177(6) Uani 1 1 d . . . . .
C11 C 0.9930(3) 0.1030(2) 0.33390(13) 0.0215(7) Uani 1 1 d . . . . .
H11 H 0.9464 0.1233 0.3050 0.026 Uiso 1 1 calc R U . . .
C12 C 1.0599(3) 0.0359(2) 0.33001(14) 0.0238(7) Uani 1 1 d . . . . .
H12 H 1.0586 0.0093 0.2985 0.029 Uiso 1 1 calc R U . . .
C13 C 1.1294(3) 0.0068(2) 0.37200(15) 0.0270(8) Uani 1 1 d . . . . .
H13 H 1.1758 -0.0394 0.3693 0.032 Uiso 1 1 calc R U . . .
C14 C 1.1310(3) 0.0453(3) 0.41781(15) 0.0297(8) Uani 1 1 d . . . . .
H14 H 1.1790 0.0256 0.4465 0.036 Uiso 1 1 calc R U . . .
C15 C 1.0631(3) 0.1123(2) 0.42225(14) 0.0255(8) Uani 1 1 d . . . . .
H15 H 1.0643 0.1384 0.4539 0.031 Uiso 1 1 calc R U . . .
C16 C 0.7053(3) 0.0298(2) 0.44282(12) 0.0181(6) Uani 1 1 d . . . . .
C17 C 0.7971(3) -0.0164(2) 0.43914(13) 0.0216(7) Uani 1 1 d . . . . .
H17 H 0.8544 0.0104 0.4273 0.026 Uiso 1 1 calc R U . . .
C18 C 0.8046(3) -0.1016(2) 0.45281(13) 0.0259(8) Uani 1 1 d . . . . .
H18 H 0.8662 -0.1335 0.4495 0.031 Uiso 1 1 calc R U . . .
C19 C 0.7220(4) -0.1402(2) 0.47133(14) 0.0302(9) Uani 1 1 d . . . . .
H19 H 0.7275 -0.1983 0.4809 0.036 Uiso 1 1 calc R U . . .
C20 C 0.6321(3) -0.0946(2) 0.47598(15) 0.0293(8) Uani 1 1 d . . . . .
H20 H 0.5758 -0.1215 0.4885 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6235(3) -0.0087(2) 0.46226(14) 0.0248(7) Uani 1 1 d . . . . .
H21 H 0.5622 0.0230 0.4662 0.030 Uiso 1 1 calc R U . . .
C22 C 0.5675(3) 0.1801(2) 0.42058(12) 0.0167(6) Uani 1 1 d . . . . .
C23 C 0.5509(3) 0.2573(2) 0.44297(12) 0.0203(7) Uani 1 1 d . . . . .
H23 H 0.6095 0.2891 0.4602 0.024 Uiso 1 1 calc R U . . .
C24 C 0.4469(3) 0.2873(2) 0.43985(13) 0.0260(8) Uani 1 1 d . . . . .
H24 H 0.4348 0.3398 0.4551 0.031 Uiso 1 1 calc R U . . .
C25 C 0.3619(3) 0.2414(3) 0.41499(14) 0.0272(8) Uani 1 1 d . . . . .
H25 H 0.2914 0.2619 0.4135 0.033 Uiso 1 1 calc R U . . .
C26 C 0.3785(3) 0.1655(3) 0.39209(13) 0.0246(8) Uani 1 1 d . . . . .
H26 H 0.3193 0.1342 0.3748 0.030 Uiso 1 1 calc R U . . .
C27 C 0.4810(3) 0.1345(2) 0.39418(13) 0.0197(7) Uani 1 1 d . . . . .
H27 H 0.4923 0.0828 0.3778 0.024 Uiso 1 1 calc R U . . .
C28 C 0.5419(3) -0.0237(2) 0.30840(12) 0.0168(6) Uani 1 1 d . . . . .
C29 C 0.4362(3) -0.0515(2) 0.30434(13) 0.0195(7) Uani 1 1 d . . . . .
C30 C 0.3744(3) 0.0110(2) 0.27783(12) 0.0179(6) Uani 1 1 d . . . . .
C31 C 0.6374(3) -0.0727(2) 0.33223(12) 0.0204(7) Uani 1 1 d . . . . .
H31A H 0.6509 -0.1185 0.3098 0.031 Uiso 1 1 calc R U . . .
H31B H 0.6250 -0.0971 0.3638 0.031 Uiso 1 1 calc R U . . .
H31C H 0.6994 -0.0348 0.3388 0.031 Uiso 1 1 calc R U . . .
C32 C 0.4028(3) -0.1328(2) 0.32458(16) 0.0277(8) Uani 1 1 d . . . . .
H32A H 0.3249 -0.1340 0.3209 0.042 Uiso 1 1 calc R U . . .
H32B H 0.4350 -0.1376 0.3601 0.042 Uiso 1 1 calc R U . . .
H32C H 0.4263 -0.1805 0.3061 0.042 Uiso 1 1 calc R U . . .
C33 C 0.2566(3) 0.0149(2) 0.26040(15) 0.0260(8) Uani 1 1 d . . . . .
H33A H 0.2409 0.0232 0.2241 0.039 Uiso 1 1 calc R U . . .
H33B H 0.2273 0.0624 0.2768 0.039 Uiso 1 1 calc R U . . .
H33C H 0.2243 -0.0384 0.2688 0.039 Uiso 1 1 calc R U . . .
C34 C 0.6071(3) 0.1540(2) 0.15788(12) 0.0191(6) Uani 1 1 d . . . . .
C35 C 0.5150(3) 0.1592(2) 0.12131(13) 0.0214(7) Uani 1 1 d . . . . .
C36 C 0.4310(3) 0.1636(2) 0.14681(12) 0.0207(7) Uani 1 1 d . . . . .
C37 C 0.7183(3) 0.1493(3) 0.14834(14) 0.0262(8) Uani 1 1 d . . . . .
H37A H 0.7201 0.1130 0.1193 0.039 Uiso 1 1 calc R U . . .
H37B H 0.7651 0.1255 0.1777 0.039 Uiso 1 1 calc R U . . .
H37C H 0.7429 0.2065 0.1418 0.039 Uiso 1 1 calc R U . . .
C38 C 0.5085(4) 0.1599(3) 0.06552(14) 0.0349(10) Uani 1 1 d . . . . .
H38A H 0.4342 0.1523 0.0489 0.052 Uiso 1 1 calc R U . . .
H38B H 0.5520 0.1136 0.0560 0.052 Uiso 1 1 calc R U . . .
H38C H 0.5351 0.2144 0.0554 0.052 Uiso 1 1 calc R U . . .
C39 C 0.3140(3) 0.1704(3) 0.12678(14) 0.0297(8) Uani 1 1 d . . . . .
H39A H 0.3014 0.1679 0.0902 0.045 Uiso 1 1 calc R U . . .
H39B H 0.2873 0.2245 0.1374 0.045 Uiso 1 1 calc R U . . .
H39C H 0.2767 0.1233 0.1397 0.045 Uiso 1 1 calc R U . . .
C40 C 0.5704(3) 0.3233(2) 0.31271(12) 0.0155(6) Uani 1 1 d . . . . .
C41 C 0.4704(3) 0.3554(2) 0.31643(12) 0.0178(6) Uani 1 1 d . . . . .
C42 C 0.3982(3) 0.2969(2) 0.29290(12) 0.0163(6) Uani 1 1 d . . . . .
C43 C 0.6748(3) 0.3636(2) 0.33352(14) 0.0218(7) Uani 1 1 d . . . . .
H43A H 0.7246 0.3543 0.3106 0.033 Uiso 1 1 calc R U . . .
H43B H 0.7038 0.3384 0.3661 0.033 Uiso 1 1 calc R U . . .
H43C H 0.6646 0.4248 0.3375 0.033 Uiso 1 1 calc R U . . .
C44 C 0.4506(3) 0.4375(2) 0.34120(14) 0.0236(7) Uani 1 1 d . . . . .
H44A H 0.4679 0.4852 0.3209 0.035 Uiso 1 1 calc R U . . .
H44B H 0.4956 0.4402 0.3745 0.035 Uiso 1 1 calc R U . . .
H44C H 0.3754 0.4408 0.3443 0.035 Uiso 1 1 calc R U . . .
C45 C 0.2793(3) 0.2971(2) 0.28586(15) 0.0245(7) Uani 1 1 d . . . . .
H45A H 0.2491 0.3112 0.2510 0.037 Uiso 1 1 calc R U . . .
H45B H 0.2564 0.3394 0.3081 0.037 Uiso 1 1 calc R U . . .
H45C H 0.2543 0.2407 0.2938 0.037 Uiso 1 1 calc R U . . .
C46 C 0.1921(4) 0.5126(4) 0.4772(2) 0.0517(13) Uani 1 1 d . . . . .
H46A H 0.1284 0.4814 0.4834 0.062 Uiso 1 1 calc R U . . .
H46B H 0.1681 0.5682 0.4622 0.062 Uiso 1 1 calc R U . . .
Cl1 Cl 0.25273(13) 0.45522(10) 0.43552(6) 0.0647(4) Uani 1 1 d . . . . .
Cl2 Cl 0.28041(14) 0.52924(11) 0.53474(6) 0.0682(4) Uani 1 1 d . . . . .
C47 C 0.9947(4) 0.7660(3) 0.34266(17) 0.0426(11) Uani 1 1 d . . . . .
H47A H 1.0059 0.7408 0.3766 0.051 Uiso 1 1 calc R U . . .
H47B H 1.0644 0.7871 0.3368 0.051 Uiso 1 1 calc R U . . .
Cl3 Cl 0.94909(10) 0.68745(7) 0.29889(6) 0.0504(3) Uani 1 1 d . . . . .
Cl4 Cl 0.90772(10) 0.85091(8) 0.34031(5) 0.0478(3) Uani 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'
Br Br -0.2901 2.4595 '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'
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'
Pd Pd -0.9988 1.0072 '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'
I I -0.4742 1.8119 '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
N2 B1 N6 109.5(3) . . ?
N2 B1 N4 107.8(3) . . ?
N6 B1 N4 108.4(3) . . ?
N2 B1 H1 110.4 . . ?
N6 B1 H1 110.4 . . ?
N4 B1 H1 110.4 . . ?
C28 N1 N2 106.2(3) . . ?
C28 N1 W1 134.1(2) . . ?
N2 N1 W1 119.6(2) . . ?
C30 N2 N1 110.0(3) . . ?
C30 N2 B1 129.8(3) . . ?
N1 N2 B1 120.2(3) . . ?
C34 N3 N4 106.7(3) . . ?
C34 N3 W1 134.6(2) . . ?
N4 N3 W1 118.79(19) . . ?
C36 N4 N3 109.5(3) . . ?
C36 N4 B1 129.3(3) . . ?
N3 N4 B1 121.0(3) . . ?
C40 N5 N6 106.3(2) . . ?
C40 N5 W1 132.5(2) . . ?
N6 N5 W1 120.1(2) . . ?
C42 N6 N5 109.6(3) . . ?
C42 N6 B1 130.3(3) . . ?
N5 N6 B1 119.3(3) . . ?
C4 P1 C10 107.20(16) . . ?
C4 P1 C1 110.65(15) . . ?
C10 P1 C1 99.16(15) . . ?
C4 P1 Pd1 121.75(13) . . ?
C10 P1 Pd1 111.83(11) . . ?
C1 P1 Pd1 103.92(10) . . ?
C2 P2 C22 101.89(14) . . ?
C2 P2 C16 106.75(15) . . ?
C22 P2 C16 108.28(16) . . ?
C2 P2 Pd1 105.59(11) . . ?
C22 P2 Pd1 118.92(12) . . ?
C16 P2 Pd1 114.00(12) . . ?
P2 Pd1 P1 87.74(3) . . ?
P2 Pd1 I2 86.01(2) . . ?
P1 Pd1 I2 172.31(3) . . ?
P2 Pd1 I1 177.86(2) . . ?
P1 Pd1 I1 92.95(2) . . ?
I2 Pd1 I1 93.139(12) . . ?
C3 W1 C2 109.26(13) . . ?
C3 W1 C1 71.72(13) . . ?
C2 W1 C1 37.73(12) . . ?
C3 W1 N5 92.86(12) . . ?
C2 W1 N5 89.67(11) . . ?
C1 W1 N5 95.09(11) . . ?
C3 W1 N3 84.57(12) . . ?
C2 W1 N3 162.74(11) . . ?
C1 W1 N3 155.35(11) . . ?
N5 W1 N3 79.10(10) . . ?
C3 W1 N1 164.44(12) . . ?
C2 W1 N1 86.27(11) . . ?
C1 W1 N1 123.71(11) . . ?
N5 W1 N1 87.98(10) . . ?
N3 W1 N1 80.33(10) . . ?
C3 W1 Br1 90.66(10) . . ?
C2 W1 Br1 102.50(9) . . ?
C1 W1 Br1 99.44(9) . . ?
N5 W1 Br1 165.43(7) . . ?
N3 W1 Br1 87.17(7) . . ?
N1 W1 Br1 84.89(7) . . ?
C2 C1 P1 119.5(2) . . ?
C2 C1 W1 70.51(19) . . ?
P1 C1 W1 169.64(18) . . ?
C1 C2 P2 119.9(3) . . ?
C1 C2 W1 71.76(19) . . ?
P2 C2 W1 161.82(18) . . ?
O1 C3 W1 179.1(3) . . ?
C9 C4 C5 119.5(3) . . ?
C9 C4 P1 121.1(3) . . ?
C5 C4 P1 119.3(3) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C8 C7 C6 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C4 119.9(4) . . ?
C8 C9 H9 120.0 . . ?
C4 C9 H9 120.0 . . ?
C15 C10 C11 119.4(3) . . ?
C15 C10 P1 120.3(3) . . ?
C11 C10 P1 120.2(3) . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.5(4) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C10 119.8(4) . . ?
C14 C15 H15 120.1 . . ?
C10 C15 H15 120.1 . . ?
C21 C16 C17 119.8(3) . . ?
C21 C16 P2 123.4(3) . . ?
C17 C16 P2 116.8(3) . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.3(4) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C16 C21 C20 119.5(4) . . ?
C16 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C23 C22 C27 120.1(3) . . ?
C23 C22 P2 120.6(3) . . ?
C27 C22 P2 119.2(2) . . ?
C22 C23 C24 119.2(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C25 C24 C23 120.5(3) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 120.5(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C22 119.4(3) . . ?
C26 C27 H27 120.3 . . ?
C22 C27 H27 120.3 . . ?
N1 C28 C29 109.9(3) . . ?
N1 C28 C31 125.2(3) . . ?
C29 C28 C31 124.9(3) . . ?
C30 C29 C28 105.6(3) . . ?
C30 C29 C32 129.2(3) . . ?
C28 C29 C32 125.2(3) . . ?
N2 C30 C29 108.3(3) . . ?
N2 C30 C33 121.7(3) . . ?
C29 C30 C33 129.9(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 . . ?
N3 C34 C35 109.7(3) . . ?
N3 C34 C37 124.6(3) . . ?
C35 C34 C37 125.7(3) . . ?
C36 C35 C34 106.0(3) . . ?
C36 C35 C38 127.0(3) . . ?
C34 C35 C38 127.0(3) . . ?
N4 C36 C35 108.2(3) . . ?
N4 C36 C39 122.4(3) . . ?
C35 C36 C39 129.5(3) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N5 C40 C41 110.0(3) . . ?
N5 C40 C43 124.2(3) . . ?
C41 C40 C43 125.8(3) . . ?
C42 C41 C40 105.5(3) . . ?
C42 C41 C44 129.2(3) . . ?
C40 C41 C44 125.3(3) . . ?
N6 C42 C41 108.7(3) . . ?
N6 C42 C45 121.8(3) . . ?
C41 C42 C45 129.5(3) . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Cl1 C46 Cl2 111.4(3) . . ?
Cl1 C46 H46A 109.3 . . ?
Cl2 C46 H46A 109.3 . . ?
Cl1 C46 H46B 109.3 . . ?
Cl2 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
Cl4 C47 Cl3 113.1(3) . . ?
Cl4 C47 H47A 109.0 . . ?
Cl3 C47 H47A 109.0 . . ?
Cl4 C47 H47B 109.0 . . ?
Cl3 C47 H47B 109.0 . . ?
H47A C47 H47B 107.8 . . ?
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 N2 1.525(5) . ?
B1 N6 1.535(5) . ?
B1 N4 1.539(5) . ?
B1 H1 1.0000 . ?
Br1 W1 2.5395(4) . ?
N1 C28 1.354(4) . ?
N1 N2 1.374(4) . ?
N1 W1 2.231(3) . ?
N2 C30 1.352(4) . ?
N3 C34 1.350(4) . ?
N3 N4 1.379(4) . ?
N3 W1 2.222(3) . ?
N4 C36 1.355(4) . ?
N5 C40 1.353(4) . ?
N5 N6 1.371(4) . ?
N5 W1 2.165(3) . ?
N6 C42 1.351(4) . ?
O1 C3 1.146(4) . ?
P1 C4 1.816(4) . ?
P1 C10 1.816(3) . ?
P1 C1 1.825(3) . ?
P1 Pd1 2.2853(9) . ?
P2 C2 1.803(3) . ?
P2 C22 1.815(3) . ?
P2 C16 1.816(3) . ?
P2 Pd1 2.2732(9) . ?
Pd1 I2 2.6319(4) . ?
Pd1 I1 2.6669(4) . ?
W1 C3 1.980(4) . ?
W1 C2 2.036(3) . ?
W1 C1 2.051(3) . ?
C1 C2 1.321(4) . ?
C4 C9 1.392(5) . ?
C4 C5 1.399(5) . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.401(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.365(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.391(5) . ?
C10 C11 1.399(5) . ?
C11 C12 1.375(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.392(5) . ?
C16 C17 1.399(5) . ?
C17 C18 1.390(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.401(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.393(5) . ?
C22 C27 1.399(5) . ?
C23 C24 1.397(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.373(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(5) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.403(5) . ?
C28 C31 1.487(5) . ?
C29 C30 1.378(5) . ?
C29 C32 1.486(5) . ?
C30 C33 1.492(5) . ?
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 . ?
C34 C35 1.396(5) . ?
C34 C37 1.491(5) . ?
C35 C36 1.381(5) . ?
C35 C38 1.504(5) . ?
C36 C39 1.496(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.394(4) . ?
C40 C43 1.491(5) . ?
C41 C42 1.374(5) . ?
C41 C44 1.500(5) . ?
C42 C45 1.495(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 Cl1 1.738(5) . ?
C46 Cl2 1.772(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 Cl4 1.731(5) . ?
C47 Cl3 1.740(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
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
C28 N1 N2 C30 -0.1(3) . . . . ?
W1 N1 N2 C30 -176.6(2) . . . . ?
C28 N1 N2 B1 -179.7(3) . . . . ?
W1 N1 N2 B1 3.8(4) . . . . ?
N6 B1 N2 C30 120.6(3) . . . . ?
N4 B1 N2 C30 -121.6(3) . . . . ?
N6 B1 N2 N1 -59.8(4) . . . . ?
N4 B1 N2 N1 57.9(4) . . . . ?
C34 N3 N4 C36 0.8(4) . . . . ?
W1 N3 N4 C36 -179.3(2) . . . . ?
C34 N3 N4 B1 176.4(3) . . . . ?
W1 N3 N4 B1 -3.6(4) . . . . ?
N2 B1 N4 C36 116.2(4) . . . . ?
N6 B1 N4 C36 -125.3(3) . . . . ?
N2 B1 N4 N3 -58.5(4) . . . . ?
N6 B1 N4 N3 60.0(4) . . . . ?
C40 N5 N6 C42 -1.2(3) . . . . ?
W1 N5 N6 C42 168.2(2) . . . . ?
C40 N5 N6 B1 169.7(3) . . . . ?
W1 N5 N6 B1 -20.8(4) . . . . ?
N2 B1 N6 C42 -119.9(3) . . . . ?
N4 B1 N6 C42 122.8(3) . . . . ?
N2 B1 N6 N5 71.3(3) . . . . ?
N4 B1 N6 N5 -46.1(4) . . . . ?
C4 P1 C1 C2 -152.9(3) . . . . ?
C10 P1 C1 C2 94.7(3) . . . . ?
Pd1 P1 C1 C2 -20.6(3) . . . . ?
C4 P1 C1 W1 42.8(11) . . . . ?
C10 P1 C1 W1 -69.6(10) . . . . ?
Pd1 P1 C1 W1 175.1(10) . . . . ?
P1 C1 C2 P2 18.3(4) . . . . ?
W1 C1 C2 P2 -164.7(2) . . . . ?
P1 C1 C2 W1 -177.0(2) . . . . ?
C22 P2 C2 C1 118.9(3) . . . . ?
C16 P2 C2 C1 -127.6(3) . . . . ?
Pd1 P2 C2 C1 -5.9(3) . . . . ?
C22 P2 C2 W1 -7.5(6) . . . . ?
C16 P2 C2 W1 105.9(6) . . . . ?
Pd1 P2 C2 W1 -132.4(6) . . . . ?
C10 P1 C4 C9 32.1(3) . . . . ?
C1 P1 C4 C9 -75.1(3) . . . . ?
Pd1 P1 C4 C9 162.6(3) . . . . ?
C10 P1 C4 C5 -150.6(3) . . . . ?
C1 P1 C4 C5 102.3(3) . . . . ?
Pd1 P1 C4 C5 -20.1(3) . . . . ?
C9 C4 C5 C6 -0.1(5) . . . . ?
P1 C4 C5 C6 -177.5(3) . . . . ?
C4 C5 C6 C7 1.0(6) . . . . ?
C5 C6 C7 C8 -0.4(6) . . . . ?
C6 C7 C8 C9 -1.2(7) . . . . ?
C7 C8 C9 C4 2.2(6) . . . . ?
C5 C4 C9 C8 -1.5(5) . . . . ?
P1 C4 C9 C8 175.9(3) . . . . ?
C4 P1 C10 C15 103.2(3) . . . . ?
C1 P1 C10 C15 -141.7(3) . . . . ?
Pd1 P1 C10 C15 -32.6(3) . . . . ?
C4 P1 C10 C11 -80.0(3) . . . . ?
C1 P1 C10 C11 35.1(3) . . . . ?
Pd1 P1 C10 C11 144.1(3) . . . . ?
C15 C10 C11 C12 1.2(5) . . . . ?
P1 C10 C11 C12 -175.5(3) . . . . ?
C10 C11 C12 C13 -1.1(5) . . . . ?
C11 C12 C13 C14 0.2(6) . . . . ?
C12 C13 C14 C15 0.5(6) . . . . ?
C13 C14 C15 C10 -0.3(6) . . . . ?
C11 C10 C15 C14 -0.5(6) . . . . ?
P1 C10 C15 C14 176.2(3) . . . . ?
C2 P2 C16 C21 -120.3(3) . . . . ?
C22 P2 C16 C21 -11.3(3) . . . . ?
Pd1 P2 C16 C21 123.5(3) . . . . ?
C2 P2 C16 C17 61.1(3) . . . . ?
C22 P2 C16 C17 170.1(3) . . . . ?
Pd1 P2 C16 C17 -55.1(3) . . . . ?
C21 C16 C17 C18 2.8(5) . . . . ?
P2 C16 C17 C18 -178.5(3) . . . . ?
C16 C17 C18 C19 -1.7(5) . . . . ?
C17 C18 C19 C20 0.4(6) . . . . ?
C18 C19 C20 C21 -0.3(6) . . . . ?
C17 C16 C21 C20 -2.7(5) . . . . ?
P2 C16 C21 C20 178.8(3) . . . . ?
C19 C20 C21 C16 1.5(6) . . . . ?
C2 P2 C22 C23 -116.5(3) . . . . ?
C16 P2 C22 C23 131.2(3) . . . . ?
Pd1 P2 C22 C23 -1.0(3) . . . . ?
C2 P2 C22 C27 60.6(3) . . . . ?
C16 P2 C22 C27 -51.7(3) . . . . ?
Pd1 P2 C22 C27 176.1(2) . . . . ?
C27 C22 C23 C24 1.7(5) . . . . ?
P2 C22 C23 C24 178.7(3) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C23 C24 C25 C26 -0.9(5) . . . . ?
C24 C25 C26 C27 0.3(5) . . . . ?
C25 C26 C27 C22 1.3(5) . . . . ?
C23 C22 C27 C26 -2.3(5) . . . . ?
P2 C22 C27 C26 -179.3(3) . . . . ?
N2 N1 C28 C29 -1.3(3) . . . . ?
W1 N1 C28 C29 174.4(2) . . . . ?
N2 N1 C28 C31 177.9(3) . . . . ?
W1 N1 C28 C31 -6.3(5) . . . . ?
N1 C28 C29 C30 2.2(4) . . . . ?
C31 C28 C29 C30 -177.1(3) . . . . ?
N1 C28 C29 C32 -178.6(3) . . . . ?
C31 C28 C29 C32 2.1(5) . . . . ?
N1 N2 C30 C29 1.5(4) . . . . ?
B1 N2 C30 C29 -178.9(3) . . . . ?
N1 N2 C30 C33 -178.1(3) . . . . ?
B1 N2 C30 C33 1.5(5) . . . . ?
C28 C29 C30 N2 -2.2(4) . . . . ?
C32 C29 C30 N2 178.7(3) . . . . ?
C28 C29 C30 C33 177.3(3) . . . . ?
C32 C29 C30 C33 -1.8(6) . . . . ?
N4 N3 C34 C35 -0.8(4) . . . . ?
W1 N3 C34 C35 179.3(2) . . . . ?
N4 N3 C34 C37 178.8(3) . . . . ?
W1 N3 C34 C37 -1.1(5) . . . . ?
N3 C34 C35 C36 0.4(4) . . . . ?
C37 C34 C35 C36 -179.1(3) . . . . ?
N3 C34 C35 C38 -179.6(4) . . . . ?
C37 C34 C35 C38 0.9(6) . . . . ?
N3 N4 C36 C35 -0.6(4) . . . . ?
B1 N4 C36 C35 -175.7(3) . . . . ?
N3 N4 C36 C39 179.8(3) . . . . ?
B1 N4 C36 C39 4.7(6) . . . . ?
C34 C35 C36 N4 0.1(4) . . . . ?
C38 C35 C36 N4 -179.9(4) . . . . ?
C34 C35 C36 C39 179.6(4) . . . . ?
C38 C35 C36 C39 -0.4(7) . . . . ?
N6 N5 C40 C41 1.6(3) . . . . ?
W1 N5 C40 C41 -165.9(2) . . . . ?
N6 N5 C40 C43 179.2(3) . . . . ?
W1 N5 C40 C43 11.6(5) . . . . ?
N5 C40 C41 C42 -1.4(4) . . . . ?
C43 C40 C41 C42 -178.9(3) . . . . ?
N5 C40 C41 C44 178.9(3) . . . . ?
C43 C40 C41 C44 1.4(5) . . . . ?
N5 N6 C42 C41 0.4(4) . . . . ?
B1 N6 C42 C41 -169.3(3) . . . . ?
N5 N6 C42 C45 -178.3(3) . . . . ?
B1 N6 C42 C45 12.0(5) . . . . ?
C40 C41 C42 N6 0.6(4) . . . . ?
C44 C41 C42 N6 -179.8(3) . . . . ?
C40 C41 C42 C45 179.1(3) . . . . ?
C44 C41 C42 C45 -1.2(6) . . . . ?
