#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:11:00 +0300 (Fri, 05 May 2023) $
#$Revision: 283291 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/18/7711897.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_7711897
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
'C46 H48 B Cl2 N7 O P2 Pd W, (C2 H3 N), (C H2 Cl2)'
_chemical_formula_sum            'C48.8 H52.6 B Cl2.6 N8 O P2 Pd W'
_chemical_formula_weight         1222.36
_chemical_name_systematic
'Carbonyl-cyanido-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II) {\m-\h2-\k2-bis(diphenylphosphanylethyne)}-palladiumdichloride'
_chemical_properties_physical    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
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.352(4)
_cell_angle_beta                 92.815(4)
_cell_angle_gamma                119.240(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5408(11)
_cell_length_b                   13.7166(11)
_cell_length_c                   16.4682(12)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.48
_cell_volume                     2658.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    2.805
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile / dichloromethane'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The unit cell contains 2 CH2Cl2 molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.418
_refine_diff_density_min         -2.066
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         19133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0379
_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)+(0.0404P)²+8.4770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15229
_reflns_number_total             19133
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           kh_sl141
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_formula_sum        'C48.80 H52.60 B Cl2.60 N8 O P2 Pd W'
_cod_database_code               7711897
_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   0.767
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014-3
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
N8 N 0.3978(11) 0.6285(10) 0.6056(11) 0.205(7) Uani 1 1 d . . . . .
C47 C 0.3385(9) 0.6217(8) 0.5471(12) 0.146(6) Uani 1 1 d . . . . .
C48 C 0.2691(11) 0.6195(8) 0.4782(9) 0.164(6) Uani 1 1 d . . . . .
H48A H 0.1896 0.5831 0.4912 0.246 Uiso 1 1 calc R U . . .
H48B H 0.2770 0.5775 0.4318 0.246 Uiso 1 1 calc R U . . .
H48C H 0.2931 0.6963 0.4644 0.246 Uiso 1 1 calc R U . . .
W1 W 0.68116(2) 0.84945(2) 0.14953(2) 0.01854(4) Uani 1 1 d . . . . .
Pd1 Pd 0.89752(2) 1.17156(2) 0.36520(2) 0.02391(6) Uani 1 1 d . . . . .
Cl1 Cl 0.85383(9) 1.19319(9) 0.49817(7) 0.0442(2) Uani 1 1 d . . . . .
Cl2 Cl 1.05934(8) 1.34968(8) 0.37399(7) 0.0415(2) Uani 1 1 d . . . . .
P1 P 0.74439(7) 1.00139(7) 0.35871(5) 0.02069(15) Uani 1 1 d . . . . .
P2 P 0.93500(7) 1.12943(7) 0.24068(5) 0.02057(15) Uani 1 1 d . . . . .
O1 O 0.8324(2) 0.9817(2) 0.01069(17) 0.0358(6) Uani 1 1 d . . . . .
N1 N 0.5748(2) 0.7276(2) 0.04685(17) 0.0214(5) Uani 1 1 d . . . . .
N2 N 0.4585(2) 0.6810(2) 0.04575(17) 0.0219(5) Uani 1 1 d . . . . .
N5 N 0.5574(2) 0.9056(2) 0.12784(17) 0.0209(5) Uani 1 1 d . . . . .
N6 N 0.4431(2) 0.8325(2) 0.12296(17) 0.0217(5) Uani 1 1 d . . . . .
N3 N 0.5522(2) 0.7129(2) 0.21606(17) 0.0208(5) Uani 1 1 d . . . . .
N4 N 0.4383(2) 0.6724(2) 0.19456(18) 0.0236(5) Uani 1 1 d . . . . .
N7 N 0.8241(3) 0.7133(3) 0.1550(2) 0.0337(7) Uani 1 1 d . . . . .
B1 B 0.4017(3) 0.7062(3) 0.1170(2) 0.0225(7) Uani 1 1 d . . . . .
H1 H 0.3172 0.6630 0.1065 0.027 Uiso 1 1 calc R U . . .
C1 C 0.7380(3) 0.9372(3) 0.2592(2) 0.0206(6) Uani 1 1 d . . . . .
C2 C 0.8119(2) 0.9954(2) 0.20598(19) 0.0192(6) Uani 1 1 d . . . . .
C3 C 0.7769(3) 0.9344(3) 0.0612(2) 0.0246(6) Uani 1 1 d . . . . .
C4 C 0.7719(3) 0.7579(3) 0.1528(2) 0.0246(6) Uani 1 1 d . . . . .
C5 C 0.7115(3) 0.7136(4) -0.0444(2) 0.0326(8) Uani 1 1 d . . . . .
H5A H 0.7080 0.6483 -0.0738 0.049 Uiso 1 1 calc R U . . .
H5B H 0.7631 0.7348 0.0050 0.049 Uiso 1 1 calc R U . . .
H5C H 0.7393 0.7763 -0.0794 0.049 Uiso 1 1 calc R U . . .
C6 C 0.5960(3) 0.6853(3) -0.0214(2) 0.0245(6) Uani 1 1 d . . . . .
C7 C 0.4940(3) 0.6117(3) -0.0666(2) 0.0275(7) Uani 1 1 d . . . . .
C8 C 0.4102(3) 0.6126(3) -0.0224(2) 0.0262(7) Uani 1 1 d . . . . .
C9 C 0.2837(3) 0.5505(4) -0.0432(3) 0.0400(9) Uani 1 1 d . . . . .
H9A H 0.2663 0.5056 -0.0951 0.060 Uiso 1 1 calc R U . . .
H9B H 0.2461 0.5012 -0.0001 0.060 Uiso 1 1 calc R U . . .
H9C H 0.2563 0.6045 -0.0480 0.060 Uiso 1 1 calc R U . . .
C10 C 0.4799(4) 0.5468(4) -0.1457(3) 0.0425(10) Uani 1 1 d . . . . .
H10A H 0.5547 0.5631 -0.1623 0.064 Uiso 1 1 calc R U . . .
H10B H 0.4341 0.4664 -0.1389 0.064 Uiso 1 1 calc R U . . .
H10C H 0.4417 0.5681 -0.1876 0.064 Uiso 1 1 calc R U . . .
C17 C 0.6802(3) 1.1133(3) 0.1229(3) 0.0308(8) Uani 1 1 d . . . . .
H17A H 0.6681 1.1773 0.1158 0.046 Uiso 1 1 calc R U . . .
H17B H 0.7221 1.1237 0.1758 0.046 Uiso 1 1 calc R U . . .
H17C H 0.7241 1.1076 0.0792 0.046 Uiso 1 1 calc R U . . .
C18 C 0.5689(3) 1.0090(3) 0.1199(2) 0.0214(6) Uani 1 1 d . . . . .
C19 C 0.4621(3) 1.0009(3) 0.1103(2) 0.0241(6) Uani 1 1 d . . . . .
C20 C 0.3848(3) 0.8874(3) 0.1116(2) 0.0233(6) Uani 1 1 d . . . . .
C21 C 0.2578(3) 0.8291(3) 0.1032(3) 0.0334(8) Uani 1 1 d . . . . .
H21A H 0.2325 0.8841 0.0955 0.050 Uiso 1 1 calc R U . . .
H21B H 0.2294 0.7740 0.0561 0.050 Uiso 1 1 calc R U . . .
H21C H 0.2282 0.7909 0.1527 0.050 Uiso 1 1 calc R U . . .
C22 C 0.4401(3) 1.0964(3) 0.0994(3) 0.0327(8) Uani 1 1 d . . . . .
H22A H 0.4765 1.1519 0.1461 0.049 Uiso 1 1 calc R U . . .
H22B H 0.3581 1.0686 0.0959 0.049 Uiso 1 1 calc R U . . .
H22C H 0.4712 1.1312 0.0492 0.049 Uiso 1 1 calc R U . . .
C11 C 0.6657(3) 0.6689(3) 0.3186(2) 0.0275(7) Uani 1 1 d . . . . .
H11A H 0.6596 0.6623 0.3774 0.041 Uiso 1 1 calc R U . . .
H11B H 0.7290 0.7425 0.3089 0.041 Uiso 1 1 calc R U . . .
H11C H 0.6793 0.6101 0.2952 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5586(3) 0.6565(3) 0.2796(2) 0.0231(6) Uani 1 1 d . . . . .
C13 C 0.4482(3) 0.5803(3) 0.2993(2) 0.0292(7) Uani 1 1 d . . . . .
C14 C 0.3754(3) 0.5920(3) 0.2441(2) 0.0283(7) Uani 1 1 d . . . . .
C15 C 0.2486(3) 0.5288(3) 0.2328(3) 0.0385(9) Uani 1 1 d . . . . .
H15A H 0.2187 0.4746 0.2744 0.058 Uiso 1 1 calc R U . . .
H15B H 0.2193 0.5813 0.2381 0.058 Uiso 1 1 calc R U . . .
H15C H 0.2246 0.4890 0.1785 0.058 Uiso 1 1 calc R U . . .
C16 C 0.4198(4) 0.4999(4) 0.3653(3) 0.0424(10) Uani 1 1 d . . . . .
H16A H 0.4545 0.5420 0.4180 0.064 Uiso 1 1 calc R U . . .
H16B H 0.4494 0.4488 0.3535 0.064 Uiso 1 1 calc R U . . .
H16C H 0.3373 0.4567 0.3672 0.064 Uiso 1 1 calc R U . . .
C23 C 0.6067(3) 0.9917(3) 0.3615(2) 0.0244(6) Uani 1 1 d . . . . .
C24 C 0.5095(3) 0.8888(3) 0.3437(3) 0.0381(9) Uani 1 1 d . . . . .
H24 H 0.5158 0.8246 0.3285 0.046 Uiso 1 1 calc R U . . .
C25 C 0.4028(3) 0.8793(4) 0.3481(3) 0.0462(11) Uani 1 1 d . . . . .
H25 H 0.3364 0.8088 0.3355 0.055 Uiso 1 1 calc R U . . .
C26 C 0.3934(4) 0.9714(4) 0.3705(3) 0.0441(10) Uani 1 1 d . . . . .
H26 H 0.3209 0.9639 0.3778 0.053 Uiso 1 1 calc R U . . .
C27 C 0.4896(4) 1.0749(4) 0.3825(3) 0.0498(12) Uani 1 1 d . . . . .
H27 H 0.4827 1.1398 0.3932 0.060 Uiso 1 1 calc R U . . .
C28 C 0.5968(4) 1.0854(4) 0.3791(3) 0.0389(9) Uani 1 1 d . . . . .
H28 H 0.6628 1.1568 0.3889 0.047 Uiso 1 1 calc R U . . .
C29 C 0.7572(3) 0.9134(3) 0.4321(2) 0.0260(7) Uani 1 1 d . . . . .
C30 C 0.6700(4) 0.8478(4) 0.4803(3) 0.0393(9) Uani 1 1 d . . . . .
H30 H 0.6011 0.8505 0.4769 0.047 Uiso 1 1 calc R U . . .
C31 C 0.6843(4) 0.7788(4) 0.5332(3) 0.0500(12) Uani 1 1 d . . . . .
H31 H 0.6251 0.7342 0.5661 0.060 Uiso 1 1 calc R U . . .
C32 C 0.7835(4) 0.7744(4) 0.5383(3) 0.0436(10) Uani 1 1 d . . . . .
H32 H 0.7924 0.7264 0.5743 0.052 Uiso 1 1 calc R U . . .
C33 C 0.8710(4) 0.8401(3) 0.4907(3) 0.0372(9) Uani 1 1 d . . . . .
H33 H 0.9396 0.8369 0.4942 0.045 Uiso 1 1 calc R U . . .
C34 C 0.8582(3) 0.9103(3) 0.4384(2) 0.0293(7) Uani 1 1 d . . . . .
H34 H 0.9185 0.9564 0.4068 0.035 Uiso 1 1 calc R U . . .
C35 C 1.0517(3) 1.1004(3) 0.2428(2) 0.0251(7) Uani 1 1 d . . . . .
C36 C 1.0356(3) 0.9923(4) 0.2418(3) 0.0457(11) Uani 1 1 d . . . . .
H36 H 0.9609 0.9302 0.2393 0.055 Uiso 1 1 calc R U . . .
C37 C 1.1284(4) 0.9749(4) 0.2445(4) 0.0564(14) Uani 1 1 d . . . . .
H37 H 1.1169 0.9008 0.2439 0.068 Uiso 1 1 calc R U . . .
C38 C 1.2360(4) 1.0635(5) 0.2479(3) 0.0472(11) Uani 1 1 d . . . . .
H38 H 1.2989 1.0507 0.2487 0.057 Uiso 1 1 calc R U . . .
C39 C 1.2541(3) 1.1717(4) 0.2502(3) 0.0427(10) Uani 1 1 d . . . . .
H39 H 1.3294 1.2329 0.2532 0.051 Uiso 1 1 calc R U . . .
C40 C 1.1628(3) 1.1915(3) 0.2482(2) 0.0339(8) Uani 1 1 d . . . . .
H40 H 1.1754 1.2661 0.2505 0.041 Uiso 1 1 calc R U . . .
C41 C 0.9652(3) 1.2277(3) 0.1629(2) 0.0241(6) Uani 1 1 d . . . . .
C42 C 1.0047(3) 1.2105(3) 0.0895(2) 0.0284(7) Uani 1 1 d . . . . .
H42 H 1.0204 1.1505 0.0821 0.034 Uiso 1 1 calc R U . . .
C43 C 1.0209(3) 1.2817(4) 0.0275(2) 0.0353(9) Uani 1 1 d . . . . .
H43 H 1.0460 1.2695 -0.0229 0.042 Uiso 1 1 calc R U . . .
C44 C 1.0001(3) 1.3705(4) 0.0398(3) 0.0416(10) Uani 1 1 d . . . . .
H44 H 1.0109 1.4190 -0.0026 0.050 Uiso 1 1 calc R U . . .
C45 C 0.9638(3) 1.3895(3) 0.1129(3) 0.0372(9) Uani 1 1 d . . . . .
H45 H 0.9512 1.4515 0.1209 0.045 Uiso 1 1 calc R U . . .
C46 C 0.9459(3) 1.3178(3) 0.1747(2) 0.0287(7) Uani 1 1 d . . . . .
H46 H 0.9204 1.3303 0.2247 0.034 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'
P P 0.1023 0.0942 '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'
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'
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
N8 C47 C48 177.1(12) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C3 W1 C1 111.79(13) . . ?
C3 W1 C2 73.88(13) . . ?
C1 W1 C2 38.06(12) . . ?
C3 W1 C4 87.94(13) . . ?
C1 W1 C4 99.81(13) . . ?
C2 W1 C4 95.50(13) . . ?
C3 W1 N5 94.25(12) . . ?
C1 W1 N5 92.47(12) . . ?
C2 W1 N5 98.66(11) . . ?
C4 W1 N5 165.73(12) . . ?
C3 W1 N1 83.40(12) . . ?
C1 W1 N1 163.95(11) . . ?
C2 W1 N1 157.20(11) . . ?
C4 W1 N1 85.40(12) . . ?
N5 W1 N1 80.86(10) . . ?
C3 W1 N3 161.94(13) . . ?
C1 W1 N3 86.05(11) . . ?
C2 W1 N3 123.68(11) . . ?
C4 W1 N3 86.18(11) . . ?
N5 W1 N3 87.47(10) . . ?
N1 W1 N3 79.12(10) . . ?
P1 Pd1 P2 88.82(3) . . ?
P1 Pd1 Cl1 86.08(4) . . ?
P2 Pd1 Cl1 172.96(4) . . ?
P1 Pd1 Cl2 179.08(4) . . ?
P2 Pd1 Cl2 91.71(4) . . ?
Cl1 Pd1 Cl2 93.33(4) . . ?
C29 P1 C23 109.28(16) . . ?
C29 P1 C1 106.53(16) . . ?
C23 P1 C1 103.50(16) . . ?
C29 P1 Pd1 112.48(12) . . ?
C23 P1 Pd1 118.27(12) . . ?
C1 P1 Pd1 105.68(10) . . ?
C35 P2 C41 104.52(15) . . ?
C35 P2 C2 103.84(15) . . ?
C41 P2 C2 109.89(15) . . ?
C35 P2 Pd1 113.58(12) . . ?
C41 P2 Pd1 119.19(13) . . ?
C2 P2 Pd1 104.84(11) . . ?
C6 N1 N2 106.7(3) . . ?
C6 N1 W1 134.9(2) . . ?
N2 N1 W1 118.4(2) . . ?
C8 N2 N1 109.1(3) . . ?
C8 N2 B1 129.4(3) . . ?
N1 N2 B1 121.5(3) . . ?
C18 N5 N6 106.0(3) . . ?
C18 N5 W1 132.3(2) . . ?
N6 N5 W1 121.6(2) . . ?
C20 N6 N5 110.4(3) . . ?
C20 N6 B1 130.0(3) . . ?
N5 N6 B1 118.7(3) . . ?
C12 N3 N4 106.8(2) . . ?
C12 N3 W1 133.5(2) . . ?
N4 N3 W1 119.59(19) . . ?
C14 N4 N3 109.5(3) . . ?
C14 N4 B1 129.7(3) . . ?
N3 N4 B1 120.0(2) . . ?
N4 B1 N6 110.5(3) . . ?
N4 B1 N2 107.9(3) . . ?
N6 B1 N2 107.8(3) . . ?
N4 B1 H1 110.2 . . ?
N6 B1 H1 110.2 . . ?
N2 B1 H1 110.2 . . ?
C2 C1 P1 120.2(2) . . ?
C2 C1 W1 72.5(2) . . ?
P1 C1 W1 162.89(18) . . ?
C1 C2 P2 119.1(3) . . ?
C1 C2 W1 69.46(19) . . ?
P2 C2 W1 171.38(19) . . ?
O1 C3 W1 178.8(3) . . ?
N7 C4 W1 177.2(3) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 110.0(3) . . ?
N1 C6 C5 124.5(3) . . ?
C7 C6 C5 125.5(3) . . ?
C8 C7 C6 105.0(3) . . ?
C8 C7 C10 128.0(3) . . ?
C6 C7 C10 127.0(4) . . ?
N2 C8 C7 109.2(3) . . ?
N2 C8 C9 122.5(3) . . ?
C7 C8 C9 128.3(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 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 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 C19 110.0(3) . . ?
N5 C18 C17 123.5(3) . . ?
C19 C18 C17 126.5(3) . . ?
C20 C19 C18 105.2(3) . . ?
C20 C19 C22 129.1(3) . . ?
C18 C19 C22 125.7(3) . . ?
N6 C20 C19 108.3(3) . . ?
N6 C20 C21 122.5(3) . . ?
C19 C20 C21 129.1(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 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 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 109.3(3) . . ?
N3 C12 C11 124.7(3) . . ?
C13 C12 C11 125.9(3) . . ?
C14 C13 C12 105.9(3) . . ?
C14 C13 C16 128.8(3) . . ?
C12 C13 C16 125.3(4) . . ?
N4 C14 C13 108.4(3) . . ?
N4 C14 C15 121.6(3) . . ?
C13 C14 C15 129.9(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 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 . . ?
C28 C23 C24 119.5(3) . . ?
C28 C23 P1 121.0(3) . . ?
C24 C23 P1 119.5(3) . . ?
C23 C24 C25 120.2(4) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 120.1(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 119.7(4) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C28 120.6(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C23 C28 C27 119.7(4) . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C34 C29 C30 119.7(3) . . ?
C34 C29 P1 117.3(3) . . ?
C30 C29 P1 122.9(3) . . ?
C31 C30 C29 119.7(4) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 C30 120.5(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 120.1(4) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.0(4) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 120.0(3) . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
C36 C35 C40 119.2(3) . . ?
C36 C35 P2 122.6(3) . . ?
C40 C35 P2 118.2(3) . . ?
C35 C36 C37 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C38 C37 C36 120.4(5) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.5(4) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C40 120.3(4) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C39 C40 C35 119.5(4) . . ?
C39 C40 H40 120.3 . . ?
C35 C40 H40 120.3 . . ?
C46 C41 C42 120.0(3) . . ?
C46 C41 P2 120.3(3) . . ?
C42 C41 P2 119.7(3) . . ?
C43 C42 C41 119.8(4) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C44 C43 C42 119.5(4) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C45 C44 C43 120.9(3) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C44 C45 C46 119.9(4) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C45 C46 C41 119.9(4) . . ?
C45 C46 H46 120.0 . . ?
C41 C46 H46 120.0 . . ?
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
N8 C47 1.193(19) . ?
C47 C48 1.427(18) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
W1 C3 2.000(3) . ?
W1 C1 2.020(3) . ?
W1 C2 2.057(3) . ?
W1 C4 2.143(3) . ?
W1 N5 2.180(3) . ?
W1 N1 2.215(3) . ?
W1 N3 2.218(2) . ?
Pd1 P1 2.2335(8) . ?
Pd1 P2 2.2556(9) . ?
Pd1 Cl1 2.3407(11) . ?
Pd1 Cl2 2.3454(9) . ?
P1 C29 1.803(3) . ?
P1 C23 1.807(3) . ?
P1 C1 1.807(3) . ?
P2 C35 1.808(3) . ?
P2 C41 1.810(3) . ?
P2 C2 1.819(3) . ?
O1 C3 1.144(4) . ?
N1 C6 1.350(5) . ?
N1 N2 1.379(4) . ?
N2 C8 1.346(4) . ?
N2 B1 1.550(5) . ?
N5 C18 1.362(4) . ?
N5 N6 1.369(4) . ?
N6 C20 1.343(4) . ?
N6 B1 1.535(4) . ?
N3 C12 1.351(4) . ?
N3 N4 1.380(4) . ?
N4 C14 1.354(4) . ?
N4 B1 1.518(5) . ?
N7 C4 1.140(5) . ?
B1 H1 1.0000 . ?
C1 C2 1.330(4) . ?
C5 C6 1.488(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.399(5) . ?
C7 C8 1.382(5) . ?
C7 C10 1.497(5) . ?
C8 C9 1.507(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C17 C18 1.483(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.395(4) . ?
C19 C20 1.390(4) . ?
C19 C22 1.494(5) . ?
C20 C21 1.498(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C11 C12 1.485(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.408(5) . ?
C13 C14 1.379(5) . ?
C13 C16 1.506(5) . ?
C14 C15 1.496(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C23 C28 1.377(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.392(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.367(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.378(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.388(5) . ?
C29 C30 1.395(5) . ?
C30 C31 1.388(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.372(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.388(6) . ?
C35 C40 1.405(5) . ?
C36 C37 1.388(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.364(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.379(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.388(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C46 1.391(5) . ?
C41 C42 1.403(5) . ?
C42 C43 1.393(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
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 -0.6(3) . . . . ?
W1 N1 N2 C8 178.0(2) . . . . ?
C6 N1 N2 B1 177.3(3) . . . . ?
W1 N1 N2 B1 -4.1(4) . . . . ?
C18 N5 N6 C20 0.5(4) . . . . ?
W1 N5 N6 C20 178.3(2) . . . . ?
C18 N5 N6 B1 170.9(3) . . . . ?
W1 N5 N6 B1 -11.3(4) . . . . ?
C12 N3 N4 C14 0.0(4) . . . . ?
W1 N3 N4 C14 -178.5(2) . . . . ?
C12 N3 N4 B1 -170.9(3) . . . . ?
W1 N3 N4 B1 10.7(4) . . . . ?
C14 N4 B1 N6 126.5(4) . . . . ?
N3 N4 B1 N6 -64.8(4) . . . . ?
C14 N4 B1 N2 -115.9(4) . . . . ?
N3 N4 B1 N2 52.8(4) . . . . ?
C20 N6 B1 N4 -126.5(4) . . . . ?
N5 N6 B1 N4 65.3(4) . . . . ?
C20 N6 B1 N2 115.8(4) . . . . ?
N5 N6 B1 N2 -52.4(4) . . . . ?
C8 N2 B1 N4 120.0(3) . . . . ?
N1 N2 B1 N4 -57.5(3) . . . . ?
C8 N2 B1 N6 -120.6(3) . . . . ?
N1 N2 B1 N6 61.9(4) . . . . ?
C29 P1 C1 C2 -124.3(3) . . . . ?
C23 P1 C1 C2 120.5(3) . . . . ?
Pd1 P1 C1 C2 -4.4(3) . . . . ?
C29 P1 C1 W1 100.8(6) . . . . ?
C23 P1 C1 W1 -14.4(6) . . . . ?
Pd1 P1 C1 W1 -139.4(6) . . . . ?
P1 C1 C2 P2 11.9(4) . . . . ?
W1 C1 C2 P2 179.2(2) . . . . ?
P1 C1 C2 W1 -167.4(2) . . . . ?
C35 P2 C2 C1 106.5(3) . . . . ?
C41 P2 C2 C1 -142.1(3) . . . . ?
Pd1 P2 C2 C1 -12.9(3) . . . . ?
N2 N1 C6 C7 0.0(4) . . . . ?
W1 N1 C6 C7 -178.3(2) . . . . ?
N2 N1 C6 C5 -179.9(3) . . . . ?
W1 N1 C6 C5 1.8(5) . . . . ?
N1 C6 C7 C8 0.5(4) . . . . ?
C5 C6 C7 C8 -179.5(3) . . . . ?
N1 C6 C7 C10 -179.5(4) . . . . ?
C5 C6 C7 C10 0.4(6) . . . . ?
N1 N2 C8 C7 0.9(4) . . . . ?
B1 N2 C8 C7 -176.7(3) . . . . ?
N1 N2 C8 C9 -178.5(3) . . . . ?
B1 N2 C8 C9 3.8(5) . . . . ?
C6 C7 C8 N2 -0.9(4) . . . . ?
C10 C7 C8 N2 179.1(4) . . . . ?
C6 C7 C8 C9 178.5(4) . . . . ?
C10 C7 C8 C9 -1.5(6) . . . . ?
N6 N5 C18 C19 0.2(4) . . . . ?
W1 N5 C18 C19 -177.2(2) . . . . ?
N6 N5 C18 C17 179.1(3) . . . . ?
W1 N5 C18 C17 1.7(5) . . . . ?
N5 C18 C19 C20 -0.9(4) . . . . ?
C17 C18 C19 C20 -179.7(3) . . . . ?
N5 C18 C19 C22 -179.7(3) . . . . ?
C17 C18 C19 C22 1.5(6) . . . . ?
N5 N6 C20 C19 -1.1(4) . . . . ?
B1 N6 C20 C19 -170.1(3) . . . . ?
N5 N6 C20 C21 179.4(3) . . . . ?
B1 N6 C20 C21 10.5(6) . . . . ?
C18 C19 C20 N6 1.2(4) . . . . ?
C22 C19 C20 N6 180.0(4) . . . . ?
C18 C19 C20 C21 -179.4(4) . . . . ?
C22 C19 C20 C21 -0.7(6) . . . . ?
N4 N3 C12 C13 -0.6(4) . . . . ?
W1 N3 C12 C13 177.5(2) . . . . ?
N4 N3 C12 C11 176.0(3) . . . . ?
W1 N3 C12 C11 -5.9(5) . . . . ?
N3 C12 C13 C14 1.0(4) . . . . ?
C11 C12 C13 C14 -175.5(3) . . . . ?
N3 C12 C13 C16 178.3(4) . . . . ?
C11 C12 C13 C16 1.7(6) . . . . ?
N3 N4 C14 C13 0.7(4) . . . . ?
B1 N4 C14 C13 170.3(3) . . . . ?
N3 N4 C14 C15 -177.1(3) . . . . ?
B1 N4 C14 C15 -7.4(6) . . . . ?
C12 C13 C14 N4 -1.0(4) . . . . ?
C16 C13 C14 N4 -178.1(4) . . . . ?
C12 C13 C14 C15 176.5(4) . . . . ?
C16 C13 C14 C15 -0.6(7) . . . . ?
C29 P1 C23 C28 121.0(3) . . . . ?
C1 P1 C23 C28 -125.8(3) . . . . ?
Pd1 P1 C23 C28 -9.4(4) . . . . ?
C29 P1 C23 C24 -60.5(4) . . . . ?
C1 P1 C23 C24 52.7(3) . . . . ?
Pd1 P1 C23 C24 169.1(3) . . . . ?
C28 C23 C24 C25 -3.5(7) . . . . ?
P1 C23 C24 C25 178.0(4) . . . . ?
C23 C24 C25 C26 -0.5(7) . . . . ?
C24 C25 C26 C27 5.1(8) . . . . ?
C25 C26 C27 C28 -5.7(8) . . . . ?
C24 C23 C28 C27 2.9(7) . . . . ?
P1 C23 C28 C27 -178.6(4) . . . . ?
C26 C27 C28 C23 1.7(8) . . . . ?
C23 P1 C29 C34 180.0(3) . . . . ?
C1 P1 C29 C34 68.7(3) . . . . ?
Pd1 P1 C29 C34 -46.6(3) . . . . ?
C23 P1 C29 C30 1.4(4) . . . . ?
C1 P1 C29 C30 -109.8(4) . . . . ?
Pd1 P1 C29 C30 134.8(3) . . . . ?
C34 C29 C30 C31 -1.0(7) . . . . ?
P1 C29 C30 C31 177.5(4) . . . . ?
C29 C30 C31 C32 -0.1(8) . . . . ?
C30 C31 C32 C33 0.5(8) . . . . ?
C31 C32 C33 C34 0.2(7) . . . . ?
C32 C33 C34 C29 -1.3(6) . . . . ?
C30 C29 C34 C33 1.8(6) . . . . ?
P1 C29 C34 C33 -176.9(3) . . . . ?
C41 P2 C35 C36 -132.2(4) . . . . ?
C2 P2 C35 C36 -17.0(4) . . . . ?
Pd1 P2 C35 C36 96.3(4) . . . . ?
C41 P2 C35 C40 49.8(3) . . . . ?
C2 P2 C35 C40 165.0(3) . . . . ?
Pd1 P2 C35 C40 -81.7(3) . . . . ?
C40 C35 C36 C37 -1.3(7) . . . . ?
P2 C35 C36 C37 -179.3(4) . . . . ?
C35 C36 C37 C38 -0.1(9) . . . . ?
C36 C37 C38 C39 1.1(9) . . . . ?
C37 C38 C39 C40 -0.7(7) . . . . ?
C38 C39 C40 C35 -0.8(6) . . . . ?
C36 C35 C40 C39 1.7(6) . . . . ?
P2 C35 C40 C39 179.8(3) . . . . ?
C35 P2 C41 C46 -139.5(3) . . . . ?
C2 P2 C41 C46 109.6(3) . . . . ?
Pd1 P2 C41 C46 -11.4(3) . . . . ?
C35 P2 C41 C42 42.5(3) . . . . ?
C2 P2 C41 C42 -68.4(3) . . . . ?
Pd1 P2 C41 C42 170.7(2) . . . . ?
C46 C41 C42 C43 -2.2(5) . . . . ?
P2 C41 C42 C43 175.8(3) . . . . ?
C41 C42 C43 C44 1.5(5) . . . . ?
C42 C43 C44 C45 0.2(6) . . . . ?
C43 C44 C45 C46 -1.2(6) . . . . ?
C44 C45 C46 C41 0.5(5) . . . . ?
C42 C41 C46 C45 1.2(5) . . . . ?
P2 C41 C46 C45 -176.7(3) . . . . ?
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 0.089 0.448 0.691 171 43 ' '
2 -0.091 0.553 0.305 168 43 ' '
