#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:11:00 +0300 (Fri, 05 May 2023) $
#$Revision: 283291 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/19/7711902.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_7711902
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 Cl1 N6 O P2 W, 0.893(C5 H12), 0.107(C H2 Cl2)'
_chemical_formula_sum            'C49.57 H58.93 B Cl1.22 N6 O P2 W'
_chemical_formula_weight         1054.46
_chemical_name_systematic
η2-{bis(diphenylphosphanyl)ethyne}-carbonyl-chlorido-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.355(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1334(6)
_cell_length_b                   19.3491(8)
_cell_length_c                   19.7000(8)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      35.01
_cell_measurement_theta_min      2.92
_cell_volume                     4939.6(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.998
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            129485
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         2.627
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.511
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         17834
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0226P)²+7.4289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15411
_reflns_number_total             17834
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           is_sl363
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711902
_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   0.314
_shelx_estimated_absorpt_t_max   0.736
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C46A C 0.9155(6) 0.3200(4) -0.0028(4) 0.118(3) Uiso 0.893(4) 1 d . U P A 1
H46A H 0.8796 0.2877 0.0235 0.177 Uiso 0.893(4) 1 calc R U P A 1
H46B H 0.9237 0.2988 -0.0468 0.177 Uiso 0.893(4) 1 calc R U P A 1
H46C H 0.8751 0.3626 -0.0114 0.177 Uiso 0.893(4) 1 calc R U P A 1
C47A C 1.0183(5) 0.3363(3) 0.0367(3) 0.0857(16) Uiso 0.893(4) 1 d . U P A 1
H47A H 1.0094 0.3448 0.0850 0.103 Uiso 0.893(4) 1 calc R U P A 1
H47B H 1.0616 0.2945 0.0368 0.103 Uiso 0.893(4) 1 calc R U P A 1
C48A C 1.0775(4) 0.3951(3) 0.0150(3) 0.0707(13) Uiso 0.893(4) 1 d . U P A 1
H48A H 1.0363 0.4376 0.0172 0.085 Uiso 0.893(4) 1 calc R U P A 1
H48B H 1.0846 0.3879 -0.0338 0.085 Uiso 0.893(4) 1 calc R U P A 1
C49A C 1.1826(5) 0.4071(4) 0.0552(4) 0.0898(17) Uiso 0.893(4) 1 d . U P A 1
H49A H 1.1736 0.4020 0.1038 0.108 Uiso 0.893(4) 1 calc R U P A 1
H49B H 1.2233 0.3664 0.0450 0.108 Uiso 0.893(4) 1 calc R U P A 1
C50A C 1.2532(10) 0.4658(6) 0.0551(7) 0.179(5) Uiso 0.893(4) 1 d . U P A 1
H50A H 1.3131 0.4516 0.0346 0.268 Uiso 0.893(4) 1 calc R U P A 1
H50B H 1.2763 0.4812 0.1025 0.268 Uiso 0.893(4) 1 calc R U P A 1
H50C H 1.2174 0.5037 0.0282 0.268 Uiso 0.893(4) 1 calc R U P A 1
C46B C 1.127(5) 0.431(2) 0.027(3) 0.100(17) Uiso 0.107(4) 1 d D . P A 2
H46D H 1.1123 0.4071 -0.0183 0.120 Uiso 0.107(4) 1 calc R U P A 2
H46E H 1.0676 0.4617 0.0297 0.120 Uiso 0.107(4) 1 calc R U P A 2
Cl2 Cl 1.2288(10) 0.4796(6) 0.0265(7) 0.072(3) Uiso 0.107(4) 1 d D . P A 2
Cl3 Cl 1.1303(12) 0.3718(8) 0.0871(8) 0.099(5) Uiso 0.107(4) 1 d D . P A 2
B1 B 1.03807(16) 0.32236(11) 0.37709(11) 0.0154(3) Uani 1 1 d . . . . .
H1 H 1.1147 0.3218 0.3797 0.019 Uiso 1 1 calc R U . . .
N1 N 0.89206(12) 0.23717(8) 0.36745(8) 0.0147(3) Uani 1 1 d . . . . .
N2 N 0.99485(12) 0.24881(8) 0.36761(8) 0.0155(3) Uani 1 1 d . . . . .
N3 N 0.90787(12) 0.36238(8) 0.45033(8) 0.0147(3) Uani 1 1 d . . . . .
N4 N 1.00911(12) 0.35402(8) 0.44316(8) 0.0150(3) Uani 1 1 d . . . . .
N5 N 0.88402(12) 0.38206(8) 0.30848(8) 0.0140(3) Uani 1 1 d . . . . .
N6 N 0.98785(12) 0.36813(8) 0.31675(8) 0.0150(3) Uani 1 1 d . . . . .
O1 O 0.68373(12) 0.46728(8) 0.39430(8) 0.0229(3) Uani 1 1 d . . . . .
P1 P 0.69161(4) 0.21810(3) 0.21238(3) 0.01770(9) Uani 1 1 d . . . . .
P2 P 0.52221(4) 0.36645(3) 0.26690(3) 0.01829(9) Uani 1 1 d . . . . .
W1 W 0.78386(2) 0.32596(2) 0.36722(2) 0.01124(2) Uani 1 1 d . . . . .
Cl1 Cl 0.72120(4) 0.26288(3) 0.45859(3) 0.02043(9) Uani 1 1 d . . . . .
C1 C 0.70714(14) 0.28159(9) 0.27966(9) 0.0144(3) Uani 1 1 d . . . . .
C2 C 0.64663(13) 0.33009(9) 0.29978(9) 0.0136(3) Uani 1 1 d . . . . .
C3 C 0.71704(14) 0.41319(10) 0.38578(10) 0.0161(3) Uani 1 1 d . . . . .
C4 C 0.47456(14) 0.39806(11) 0.34334(11) 0.0195(4) Uani 1 1 d . . . . .
C5 C 0.49010(17) 0.36377(13) 0.40652(12) 0.0260(4) Uani 1 1 d . . . . .
H5 H 0.5257 0.3209 0.4110 0.031 Uiso 1 1 calc R U . . .
C6 C 0.45383(18) 0.39192(14) 0.46272(13) 0.0309(5) Uani 1 1 d . . . . .
H6 H 0.4648 0.3683 0.5056 0.037 Uiso 1 1 calc R U . . .
C7 C 0.40160(18) 0.45441(14) 0.45653(14) 0.0323(5) Uani 1 1 d . . . . .
H7 H 0.3780 0.4740 0.4954 0.039 Uiso 1 1 calc R U . . .
C8 C 0.38385(18) 0.48808(12) 0.39425(15) 0.0312(5) Uani 1 1 d . . . . .
H8 H 0.3466 0.5304 0.3899 0.037 Uiso 1 1 calc R U . . .
C9 C 0.42036(16) 0.46024(11) 0.33739(13) 0.0242(4) Uani 1 1 d . . . . .
H9 H 0.4082 0.4838 0.2945 0.029 Uiso 1 1 calc R U . . .
C10 C 0.44344(15) 0.28835(12) 0.24904(11) 0.0228(4) Uani 1 1 d . . . . .
C11 C 0.35898(18) 0.29240(16) 0.19589(13) 0.0338(5) Uani 1 1 d . . . . .
H11 H 0.3456 0.3341 0.1705 0.041 Uiso 1 1 calc R U . . .
C12 C 0.2944(2) 0.23555(19) 0.17995(16) 0.0452(8) Uani 1 1 d . . . . .
H12 H 0.2372 0.2387 0.1438 0.054 Uiso 1 1 calc R U . . .
C13 C 0.3127(2) 0.17543(17) 0.21593(19) 0.0471(8) Uani 1 1 d . . . . .
H13 H 0.2685 0.1368 0.2045 0.057 Uiso 1 1 calc R U . . .
C14 C 0.3957(2) 0.17038(15) 0.26929(19) 0.0424(7) Uani 1 1 d . . . . .
H14 H 0.4078 0.1286 0.2946 0.051 Uiso 1 1 calc R U . . .
C15 C 0.46135(18) 0.22691(13) 0.28564(14) 0.0302(5) Uani 1 1 d . . . . .
H15 H 0.5184 0.2233 0.3219 0.036 Uiso 1 1 calc R U . . .
C16 C 0.6897(2) 0.32684(16) 0.11456(14) 0.0386(6) Uani 1 1 d . . . . .
H16 H 0.7583 0.3371 0.1356 0.046 Uiso 1 1 calc R U . . .
C17 C 0.6411(3) 0.3677(2) 0.06062(16) 0.0563(9) Uani 1 1 d . . . . .
H17 H 0.6762 0.4061 0.0453 0.068 Uiso 1 1 calc R U . . .
C18 C 0.5413(3) 0.3522(2) 0.02934(15) 0.0590(10) Uani 1 1 d . . . . .
H18 H 0.5076 0.3808 -0.0066 0.071 Uiso 1 1 calc R U . . .
C19 C 0.4910(2) 0.2956(2) 0.05014(15) 0.0522(9) Uani 1 1 d . . . . .
H19 H 0.4237 0.2842 0.0274 0.063 Uiso 1 1 calc R U . . .
C20 C 0.53885(18) 0.25514(15) 0.10449(13) 0.0350(6) Uani 1 1 d . . . . .
H20 H 0.5037 0.2163 0.1191 0.042 Uiso 1 1 calc R U . . .
C21 C 0.63802(17) 0.27115(12) 0.13768(11) 0.0247(4) Uani 1 1 d . . . . .
C22 C 0.82194(14) 0.19985(10) 0.19614(10) 0.0163(3) Uani 1 1 d . . . . .
C23 C 0.83838(15) 0.13305(10) 0.17260(10) 0.0186(3) Uani 1 1 d . . . . .
H23 H 0.7843 0.1000 0.1689 0.022 Uiso 1 1 calc R U . . .
C24 C 0.93260(16) 0.11456(11) 0.15463(11) 0.0235(4) Uani 1 1 d . . . . .
H24 H 0.9422 0.0695 0.1376 0.028 Uiso 1 1 calc R U . . .
C25 C 1.01283(17) 0.16224(12) 0.16169(12) 0.0266(4) Uani 1 1 d . . . . .
H25 H 1.0776 0.1497 0.1498 0.032 Uiso 1 1 calc R U . . .
C26 C 0.99824(16) 0.22825(12) 0.18608(12) 0.0241(4) Uani 1 1 d . . . . .
H26 H 1.0534 0.2606 0.1914 0.029 Uiso 1 1 calc R U . . .
C27 C 0.90319(15) 0.24717(10) 0.20270(10) 0.0194(4) Uani 1 1 d . . . . .
H27 H 0.8935 0.2926 0.2186 0.023 Uiso 1 1 calc R U . . .
C28 C 0.87781(16) 0.16829(10) 0.36005(10) 0.0180(3) Uani 1 1 d . . . . .
C29 C 0.97179(17) 0.13610(10) 0.35442(11) 0.0211(4) Uani 1 1 d . . . . .
C30 C 1.04402(16) 0.18841(11) 0.35994(11) 0.0205(4) Uani 1 1 d . . . . .
C31 C 0.77733(18) 0.13248(11) 0.35909(13) 0.0267(4) Uani 1 1 d . . . . .
H31A H 0.7839 0.0984 0.3964 0.040 Uiso 1 1 calc R U . . .
H31B H 0.7575 0.1090 0.3148 0.040 Uiso 1 1 calc R U . . .
H31C H 0.7243 0.1664 0.3655 0.040 Uiso 1 1 calc R U . . .
C32 C 0.9876(2) 0.06004(12) 0.34497(14) 0.0328(5) Uani 1 1 d . . . . .
H32A H 1.0613 0.0506 0.3467 0.049 Uiso 1 1 calc R U . . .
H32B H 0.9496 0.0454 0.3003 0.049 Uiso 1 1 calc R U . . .
H32C H 0.9623 0.0344 0.3818 0.049 Uiso 1 1 calc R U . . .
C33 C 1.15723(18) 0.18466(14) 0.35946(15) 0.0339(5) Uani 1 1 d . . . . .
H33A H 1.1775 0.1364 0.3547 0.051 Uiso 1 1 calc R U . . .
H33B H 1.1944 0.2035 0.4027 0.051 Uiso 1 1 calc R U . . .
H33C H 1.1743 0.2116 0.3207 0.051 Uiso 1 1 calc R U . . .
C34 C 0.90780(15) 0.39743(9) 0.50979(9) 0.0157(3) Uani 1 1 d . . . . .
C35 C 1.00907(16) 0.41250(10) 0.54015(10) 0.0172(3) Uani 1 1 d . . . . .
C36 C 1.07115(15) 0.38373(10) 0.49694(10) 0.0165(3) Uani 1 1 d . . . . .
C37 C 0.81346(17) 0.41568(12) 0.53878(11) 0.0241(4) Uani 1 1 d . . . . .
H37A H 0.8264 0.4087 0.5887 0.036 Uiso 1 1 calc R U . . .
H37B H 0.7561 0.3861 0.5181 0.036 Uiso 1 1 calc R U . . .
H37C H 0.7958 0.4642 0.5286 0.036 Uiso 1 1 calc R U . . .
C38 C 1.04213(19) 0.45102(11) 0.60603(11) 0.0252(4) Uani 1 1 d . . . . .
H38A H 1.1133 0.4672 0.6080 0.038 Uiso 1 1 calc R U . . .
H38B H 1.0382 0.4203 0.6451 0.038 Uiso 1 1 calc R U . . .
H38C H 0.9965 0.4908 0.6081 0.038 Uiso 1 1 calc R U . . .
C39 C 1.18575(16) 0.38090(13) 0.50486(12) 0.0267(4) Uani 1 1 d . . . . .
H39A H 1.2158 0.4131 0.5411 0.040 Uiso 1 1 calc R U . . .
H39B H 1.2076 0.3939 0.4613 0.040 Uiso 1 1 calc R U . . .
H39C H 1.2093 0.3339 0.5174 0.040 Uiso 1 1 calc R U . . .
C40 C 0.86448(16) 0.42901(10) 0.25715(10) 0.0183(3) Uani 1 1 d . . . . .
C41 C 0.95549(17) 0.44438(11) 0.23177(11) 0.0228(4) Uani 1 1 d . . . . .
C42 C 1.03201(16) 0.40577(11) 0.27143(10) 0.0202(4) Uani 1 1 d . . . . .
C43 C 0.76097(18) 0.45993(12) 0.23331(12) 0.0266(4) Uani 1 1 d . . . . .
H43A H 0.7647 0.4909 0.1944 0.040 Uiso 1 1 calc R U . . .
H43B H 0.7391 0.4862 0.2710 0.040 Uiso 1 1 calc R U . . .
H43C H 0.7110 0.4231 0.2188 0.040 Uiso 1 1 calc R U . . .
C44 C 0.9655(2) 0.49335(15) 0.17440(15) 0.0399(6) Uani 1 1 d . . . . .
H44A H 1.0374 0.4942 0.1667 0.060 Uiso 1 1 calc R U . . .
H44B H 0.9449 0.5398 0.1866 0.060 Uiso 1 1 calc R U . . .
H44C H 0.9209 0.4781 0.1323 0.060 Uiso 1 1 calc R U . . .
C45 C 1.14559(18) 0.40372(15) 0.27015(13) 0.0322(5) Uani 1 1 d . . . . .
H45A H 1.1616 0.4333 0.2329 0.048 Uiso 1 1 calc R U . . .
H45B H 1.1666 0.3561 0.2625 0.048 Uiso 1 1 calc R U . . .
H45C H 1.1830 0.4205 0.3142 0.048 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'
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
C47A C46A H46A 109.5 . . ?
C47A C46A H46B 109.5 . . ?
H46A C46A H46B 109.5 . . ?
C47A C46A H46C 109.5 . . ?
H46A C46A H46C 109.5 . . ?
H46B C46A H46C 109.5 . . ?
C48A C47A C46A 119.3(6) . . ?
C48A C47A H47A 107.5 . . ?
C46A C47A H47A 107.5 . . ?
C48A C47A H47B 107.5 . . ?
C46A C47A H47B 107.5 . . ?
H47A C47A H47B 107.0 . . ?
C47A C48A C49A 116.7(5) . . ?
C47A C48A H48A 108.1 . . ?
C49A C48A H48A 108.1 . . ?
C47A C48A H48B 108.1 . . ?
C49A C48A H48B 108.1 . . ?
H48A C48A H48B 107.3 . . ?
C50A C49A C48A 130.6(8) . . ?
C50A C49A H49A 104.6 . . ?
C48A C49A H49A 104.6 . . ?
C50A C49A H49B 104.6 . . ?
C48A C49A H49B 104.6 . . ?
H49A C49A H49B 105.7 . . ?
C49A C50A H50A 109.5 . . ?
C49A C50A H50B 109.5 . . ?
H50A C50A H50B 109.5 . . ?
C49A C50A H50C 109.5 . . ?
H50A C50A H50C 109.5 . . ?
H50B C50A H50C 109.5 . . ?
Cl2 C46B Cl3 118(4) . . ?
Cl2 C46B H46D 107.7 . . ?
Cl3 C46B H46D 107.7 . . ?
Cl2 C46B H46E 107.7 . . ?
Cl3 C46B H46E 107.7 . . ?
H46D C46B H46E 107.1 . . ?
N2 B1 N4 109.56(15) . . ?
N2 B1 N6 109.63(15) . . ?
N4 B1 N6 106.82(15) . . ?
N2 B1 H1 110.3 . . ?
N4 B1 H1 110.3 . . ?
N6 B1 H1 110.3 . . ?
C28 N1 N2 106.39(15) . . ?
C28 N1 W1 133.10(13) . . ?
N2 N1 W1 120.10(11) . . ?
C30 N2 N1 110.21(16) . . ?
C30 N2 B1 129.84(17) . . ?
N1 N2 B1 119.94(15) . . ?
C34 N3 N4 106.61(15) . . ?
C34 N3 W1 133.72(13) . . ?
N4 N3 W1 119.53(11) . . ?
C36 N4 N3 109.86(15) . . ?
C36 N4 B1 129.01(16) . . ?
N3 N4 B1 120.74(15) . . ?
C40 N5 N6 106.53(15) . . ?
C40 N5 W1 132.42(13) . . ?
N6 N5 W1 120.85(12) . . ?
C42 N6 N5 109.85(16) . . ?
C42 N6 B1 129.95(16) . . ?
N5 N6 B1 119.75(15) . . ?
C1 P1 C22 105.34(8) . . ?
C1 P1 C21 101.07(9) . . ?
C22 P1 C21 102.44(10) . . ?
C2 P2 C4 104.29(9) . . ?
C2 P2 C10 101.41(9) . . ?
C4 P2 C10 100.13(9) . . ?
C3 W1 C1 110.17(7) . . ?
C3 W1 C2 73.50(7) . . ?
C1 W1 C2 37.89(7) . . ?
C3 W1 N5 89.84(7) . . ?
C1 W1 N5 91.06(7) . . ?
C2 W1 N5 100.29(7) . . ?
C3 W1 N3 83.50(7) . . ?
C1 W1 N3 162.95(6) . . ?
C2 W1 N3 156.99(6) . . ?
N5 W1 N3 78.48(6) . . ?
C3 W1 N1 165.02(7) . . ?
C1 W1 N1 84.52(6) . . ?
C2 W1 N1 121.46(6) . . ?
N5 W1 N1 86.87(6) . . ?
N3 W1 N1 81.53(6) . . ?
C3 W1 Cl1 94.50(6) . . ?
C1 W1 Cl1 103.59(5) . . ?
C2 W1 Cl1 97.55(5) . . ?
N5 W1 Cl1 162.15(4) . . ?
N3 W1 Cl1 84.81(4) . . ?
N1 W1 Cl1 84.48(4) . . ?
C2 C1 P1 134.50(15) . . ?
C2 C1 W1 71.84(11) . . ?
P1 C1 W1 153.36(11) . . ?
C1 C2 P2 136.01(15) . . ?
C1 C2 W1 70.27(11) . . ?
P2 C2 W1 153.55(10) . . ?
O1 C3 W1 174.45(17) . . ?
C9 C4 C5 118.95(19) . . ?
C9 C4 P2 117.29(17) . . ?
C5 C4 P2 123.76(16) . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C6 120.1(2) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.2(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C4 C9 C8 120.2(2) . . ?
C4 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C15 C10 C11 118.9(2) . . ?
C15 C10 P2 124.25(16) . . ?
C11 C10 P2 116.9(2) . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C10 C15 C14 120.2(2) . . ?
C10 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C21 C16 C17 120.2(3) . . ?
C21 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 119.9(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C21 120.4(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C16 C21 C20 119.2(2) . . ?
C16 C21 P1 123.50(18) . . ?
C20 C21 P1 117.3(2) . . ?
C27 C22 C23 118.61(17) . . ?
C27 C22 P1 125.53(14) . . ?
C23 C22 P1 115.81(14) . . ?
C24 C23 C22 120.90(19) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 119.74(19) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 120.2(2) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C22 120.51(18) . . ?
C26 C27 H27 119.7 . . ?
C22 C27 H27 119.7 . . ?
N1 C28 C29 109.78(18) . . ?
N1 C28 C31 124.61(18) . . ?
C29 C28 C31 125.60(18) . . ?
C30 C29 C28 105.70(17) . . ?
C30 C29 C32 128.4(2) . . ?
C28 C29 C32 125.9(2) . . ?
N2 C30 C29 107.91(17) . . ?
N2 C30 C33 122.4(2) . . ?
C29 C30 C33 129.64(19) . . ?
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 109.90(17) . . ?
N3 C34 C37 124.65(17) . . ?
C35 C34 C37 125.44(17) . . ?
C36 C35 C34 105.49(16) . . ?
C36 C35 C38 127.92(19) . . ?
C34 C35 C38 126.59(19) . . ?
N4 C36 C35 108.14(16) . . ?
N4 C36 C39 122.37(18) . . ?
C35 C36 C39 129.45(18) . . ?
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 109.90(18) . . ?
N5 C40 C43 123.91(18) . . ?
C41 C40 C43 126.18(19) . . ?
C42 C41 C40 105.47(18) . . ?
C42 C41 C44 128.4(2) . . ?
C40 C41 C44 126.1(2) . . ?
N6 C42 C41 108.22(18) . . ?
N6 C42 C45 122.1(2) . . ?
C41 C42 C45 129.6(2) . . ?
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 . . ?
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
C46A C47A 1.479(9) . ?
C46A H46A 0.9800 . ?
C46A H46B 0.9800 . ?
C46A H46C 0.9800 . ?
C47A C48A 1.479(8) . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C48A C49A 1.494(8) . ?
C48A H48A 0.9900 . ?
C48A H48B 0.9900 . ?
C49A C50A 1.466(12) . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C50A H50A 0.9800 . ?
C50A H50B 0.9800 . ?
C50A H50C 0.9800 . ?
C46B Cl2 1.64(4) . ?
C46B Cl3 1.65(4) . ?
C46B H46D 0.9900 . ?
C46B H46E 0.9900 . ?
B1 N2 1.532(3) . ?
B1 N4 1.541(3) . ?
B1 N6 1.542(3) . ?
B1 H1 1.0000 . ?
N1 C28 1.350(2) . ?
N1 N2 1.368(2) . ?
N1 W1 2.2291(15) . ?
N2 C30 1.356(2) . ?
N3 C34 1.354(2) . ?
N3 N4 1.369(2) . ?
N3 W1 2.2278(16) . ?
N4 C36 1.355(2) . ?
N5 C40 1.352(2) . ?
N5 N6 1.374(2) . ?
N5 W1 2.1778(16) . ?
N6 C42 1.354(2) . ?
O1 C3 1.157(2) . ?
P1 C1 1.7943(18) . ?
P1 C22 1.8262(19) . ?
P1 C21 1.838(2) . ?
P2 C2 1.8001(18) . ?
P2 C4 1.827(2) . ?
P2 C10 1.833(2) . ?
W1 C3 1.9641(19) . ?
W1 C1 2.0402(18) . ?
W1 C2 2.0595(18) . ?
W1 Cl1 2.4265(5) . ?
C1 C2 1.331(2) . ?
C4 C9 1.393(3) . ?
C4 C5 1.396(3) . ?
C5 C6 1.386(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.375(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.396(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.390(4) . ?
C10 C11 1.398(3) . ?
C11 C12 1.394(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.363(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.398(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.389(4) . ?
C16 C17 1.393(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.375(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(3) . ?
C20 H20 0.9500 . ?
C22 C27 1.396(3) . ?
C22 C23 1.402(3) . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.390(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.403(3) . ?
C28 C31 1.488(3) . ?
C29 C30 1.379(3) . ?
C29 C32 1.502(3) . ?
C30 C33 1.490(3) . ?
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 1.398(3) . ?
C34 C37 1.489(3) . ?
C35 C36 1.387(3) . ?
C35 C38 1.498(3) . ?
C36 C39 1.489(3) . ?
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 1.400(3) . ?
C40 C43 1.490(3) . ?
C41 C42 1.387(3) . ?
C41 C44 1.497(3) . ?
C42 C45 1.497(3) . ?
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 . ?
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
C46A C47A C48A C49A -177.4(6) . . . . ?
C47A C48A C49A C50A -168.6(9) . . . . ?
C28 N1 N2 C30 0.5(2) . . . . ?
W1 N1 N2 C30 -173.16(13) . . . . ?
C28 N1 N2 B1 -178.44(16) . . . . ?
W1 N1 N2 B1 7.9(2) . . . . ?
N4 B1 N2 C30 -124.5(2) . . . . ?
N6 B1 N2 C30 118.6(2) . . . . ?
N4 B1 N2 N1 54.1(2) . . . . ?
N6 B1 N2 N1 -62.8(2) . . . . ?
C34 N3 N4 C36 -0.4(2) . . . . ?
W1 N3 N4 C36 175.87(12) . . . . ?
C34 N3 N4 B1 -173.86(16) . . . . ?
W1 N3 N4 B1 2.4(2) . . . . ?
N2 B1 N4 C36 127.17(19) . . . . ?
N6 B1 N4 C36 -114.2(2) . . . . ?
N2 B1 N4 N3 -60.8(2) . . . . ?
N6 B1 N4 N3 57.9(2) . . . . ?
C40 N5 N6 C42 0.1(2) . . . . ?
W1 N5 N6 C42 175.60(12) . . . . ?
C40 N5 N6 B1 173.15(16) . . . . ?
W1 N5 N6 B1 -11.3(2) . . . . ?
N2 B1 N6 C42 -123.0(2) . . . . ?
N4 B1 N6 C42 118.3(2) . . . . ?
N2 B1 N6 N5 65.4(2) . . . . ?
N4 B1 N6 N5 -53.2(2) . . . . ?
C22 P1 C1 C2 155.3(2) . . . . ?
C21 P1 C1 C2 49.0(2) . . . . ?
C22 P1 C1 W1 -34.8(3) . . . . ?
C21 P1 C1 W1 -141.1(2) . . . . ?
P1 C1 C2 P2 -8.4(3) . . . . ?
W1 C1 C2 P2 176.3(2) . . . . ?
P1 C1 C2 W1 175.2(2) . . . . ?
C4 P2 C2 C1 154.0(2) . . . . ?
C10 P2 C2 C1 50.3(2) . . . . ?
C4 P2 C2 W1 -33.9(3) . . . . ?
C10 P2 C2 W1 -137.5(2) . . . . ?
C2 P2 C4 C9 141.73(16) . . . . ?
C10 P2 C4 C9 -113.61(17) . . . . ?
C2 P2 C4 C5 -37.8(2) . . . . ?
C10 P2 C4 C5 66.8(2) . . . . ?
C9 C4 C5 C6 -1.2(3) . . . . ?
P2 C4 C5 C6 178.33(18) . . . . ?
C4 C5 C6 C7 0.1(4) . . . . ?
C5 C6 C7 C8 1.2(4) . . . . ?
C6 C7 C8 C9 -1.4(3) . . . . ?
C5 C4 C9 C8 1.0(3) . . . . ?
P2 C4 C9 C8 -178.56(17) . . . . ?
C7 C8 C9 C4 0.3(3) . . . . ?
C2 P2 C10 C15 30.3(2) . . . . ?
C4 P2 C10 C15 -76.6(2) . . . . ?
C2 P2 C10 C11 -151.03(17) . . . . ?
C4 P2 C10 C11 102.00(18) . . . . ?
C15 C10 C11 C12 -0.2(4) . . . . ?
P2 C10 C11 C12 -178.9(2) . . . . ?
C10 C11 C12 C13 0.0(4) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C11 C10 C15 C14 0.0(4) . . . . ?
P2 C10 C15 C14 178.6(2) . . . . ?
C13 C14 C15 C10 0.5(4) . . . . ?
C21 C16 C17 C18 -0.8(5) . . . . ?
C16 C17 C18 C19 -1.7(5) . . . . ?
C17 C18 C19 C20 2.4(5) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
C17 C16 C21 C20 2.5(4) . . . . ?
C17 C16 C21 P1 -175.4(2) . . . . ?
C19 C20 C21 C16 -1.8(3) . . . . ?
C19 C20 C21 P1 176.19(19) . . . . ?
C1 P1 C21 C16 60.9(2) . . . . ?
C22 P1 C21 C16 -47.7(2) . . . . ?
C1 P1 C21 C20 -117.00(17) . . . . ?
C22 P1 C21 C20 134.39(17) . . . . ?
C1 P1 C22 C27 -32.1(2) . . . . ?
C21 P1 C22 C27 73.19(19) . . . . ?
C1 P1 C22 C23 150.46(15) . . . . ?
C21 P1 C22 C23 -104.21(16) . . . . ?
C27 C22 C23 C24 -1.5(3) . . . . ?
P1 C22 C23 C24 176.12(16) . . . . ?
C22 C23 C24 C25 1.7(3) . . . . ?
C23 C24 C25 C26 -0.6(4) . . . . ?
C24 C25 C26 C27 -0.8(4) . . . . ?
C25 C26 C27 C22 1.0(3) . . . . ?
C23 C22 C27 C26 0.1(3) . . . . ?
P1 C22 C27 C26 -177.23(17) . . . . ?
N2 N1 C28 C29 -0.9(2) . . . . ?
W1 N1 C28 C29 171.52(14) . . . . ?
N2 N1 C28 C31 178.30(19) . . . . ?
W1 N1 C28 C31 -9.3(3) . . . . ?
N1 C28 C29 C30 1.0(2) . . . . ?
C31 C28 C29 C30 -178.2(2) . . . . ?
N1 C28 C29 C32 -179.5(2) . . . . ?
C31 C28 C29 C32 1.3(4) . . . . ?
N1 N2 C30 C29 0.2(2) . . . . ?
B1 N2 C30 C29 178.92(18) . . . . ?
N1 N2 C30 C33 -178.9(2) . . . . ?
B1 N2 C30 C33 -0.1(3) . . . . ?
C28 C29 C30 N2 -0.7(2) . . . . ?
C32 C29 C30 N2 179.8(2) . . . . ?
C28 C29 C30 C33 178.2(2) . . . . ?
C32 C29 C30 C33 -1.3(4) . . . . ?
N4 N3 C34 C35 1.0(2) . . . . ?
W1 N3 C34 C35 -174.57(13) . . . . ?
N4 N3 C34 C37 -177.89(18) . . . . ?
W1 N3 C34 C37 6.6(3) . . . . ?
N3 C34 C35 C36 -1.1(2) . . . . ?
C37 C34 C35 C36 177.72(19) . . . . ?
N3 C34 C35 C38 179.51(19) . . . . ?
C37 C34 C35 C38 -1.6(3) . . . . ?
N3 N4 C36 C35 -0.3(2) . . . . ?
B1 N4 C36 C35 172.47(18) . . . . ?
N3 N4 C36 C39 177.74(18) . . . . ?
B1 N4 C36 C39 -9.5(3) . . . . ?
C34 C35 C36 N4 0.8(2) . . . . ?
C38 C35 C36 N4 -179.80(19) . . . . ?
C34 C35 C36 C39 -177.0(2) . . . . ?
C38 C35 C36 C39 2.4(4) . . . . ?
N6 N5 C40 C41 0.9(2) . . . . ?
W1 N5 C40 C41 -173.89(13) . . . . ?
N6 N5 C40 C43 -177.92(19) . . . . ?
W1 N5 C40 C43 7.3(3) . . . . ?
N5 C40 C41 C42 -1.5(2) . . . . ?
C43 C40 C41 C42 177.3(2) . . . . ?
N5 C40 C41 C44 179.3(2) . . . . ?
C43 C40 C41 C44 -1.9(4) . . . . ?
N5 N6 C42 C41 -1.0(2) . . . . ?
B1 N6 C42 C41 -173.18(18) . . . . ?
N5 N6 C42 C45 177.41(19) . . . . ?
B1 N6 C42 C45 5.2(3) . . . . ?
C40 C41 C42 N6 1.5(2) . . . . ?
C44 C41 C42 N6 -179.3(2) . . . . ?
C40 C41 C42 C45 -176.8(2) . . . . ?
C44 C41 C42 C45 2.4(4) . . . . ?
