#------------------------------------------------------------------------------
#$Date: 2018-10-29 09:33:49 +0200 (Mon, 29 Oct 2018) $
#$Revision: 211691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/87/7118736.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_7118736
loop_
_publ_author_name
'Ventura, K.'
'Prat, J. R.'
'Aguirre Quintana, L. M.'
'Goos, A.'
'Villagran, D.'
_publ_section_title
;
 Unprecedented W2(0) quadruply bonded complex supported by π-donor
 ligands.
;
_journal_issue                   20
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3974
_journal_page_last               3976
_journal_paper_doi               10.1039/c5cc09972b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C58 H88 K2 N4 O2 W2'
_chemical_formula_weight         1319.22
_chemical_name_systematic        W2(DippF)2K2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-21 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                96.119(6)
_cell_angle_beta                 99.340(6)
_cell_angle_gamma                105.700(6)
_cell_formula_units_Z            2
_cell_length_a                   10.879(2)
_cell_length_b                   13.364(3)
_cell_length_c                   23.272(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3173.4(12)
_computing_cell_refinement       'Apex II Bruker 2015'
_computing_data_collection       'Apex II Bruker 2015'
_computing_data_reduction        'Apex II Bruker 2015'
_computing_molecular_graphics    'Apex II Bruker 2015'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'D8 quest'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_laue_measured_fraction_full 0.966
_diffrn_reflns_laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28893
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        20.841
_diffrn_reflns_theta_max         20.841
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'Mo sealed tube'
_exptl_absorpt_coefficient_mu    3.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SadAbs'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7446
_exptl_transmission_factor_min   0.5817
_refine_diff_density_max         2.715
_refine_diff_density_min         -2.428
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     661
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0740
_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)+(0.1196P)²+135.4914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4600
_reflns_number_total             6451
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc09972b2.cif
_cod_data_source_block           basic_a
_cod_depositor_comments
;
Adding full bibliography for 7118735--7118736.cif.

2018-10-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C116 H176 K4 N8 O4 W4'
_cod_original_formula_weight         2638.44
_cod_original_formula_units_Z            1
_cod_original_cell_volume        3173.6(11)
_cod_database_code               7118736
_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.
;
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
W1 W 0.35480(9) 0.38467(8) 0.21956(4) 0.0215(4) Uani 1 1 d . U
W2 W 0.57733(9) 0.38380(8) 0.24767(4) 0.0216(4) Uani 1 1 d . U
K1 K 1.0120(6) 0.3666(5) 0.2253(2) 0.0388(16) Uani 1 1 d . U
K2 K 0.4494(7) 0.6721(6) 0.2177(3) 0.0605(19) Uani 1 1 d . U
N1 N 0.5619(16) 0.3997(15) 0.3359(7) 0.017(3) Uani 1 1 d . U
C1 C 0.448(2) 0.403(2) 0.3529(10) 0.023(5) Uani 1 1 d . U
H1 H 0.4411 0.4086 0.3932 0.028 Uiso 1 1 calc R U
N2 N 0.3444(17) 0.3995(15) 0.3101(8) 0.019(3) Uani 1 1 d . U
N3 N 0.3706(16) 0.3629(15) 0.1304(7) 0.016(3) Uani 1 1 d . U
C2 C 0.486(2) 0.359(2) 0.1158(10) 0.023(5) Uani 1 1 d . U
H2 H 0.4922 0.3500 0.0754 0.028 Uiso 1 1 calc R U
N4 N 0.5920(17) 0.3681(15) 0.1576(8) 0.020(4) Uani 1 1 d . U
C3 C 0.658(2) 0.385(2) 0.3839(10) 0.0250(18) Uani 1 1 d . U
C4 C 0.674(2) 0.286(2) 0.3775(11) 0.033(5) Uani 1 1 d . U
C5 C 0.601(3) 0.200(2) 0.3230(11) 0.041(5) Uani 1 1 d . U
H5 H 0.5054 0.1909 0.3202 0.050 Uiso 1 1 calc R U
C6 C 0.622(4) 0.095(3) 0.3296(13) 0.063(8) Uani 1 1 d . U
H6A H 0.5716 0.0435 0.2950 0.095 Uiso 1 1 calc R U
H6B H 0.5934 0.0725 0.3651 0.095 Uiso 1 1 calc R U
H6C H 0.7148 0.1016 0.3329 0.095 Uiso 1 1 calc R U
C7 C 0.637(3) 0.243(2) 0.2671(11) 0.041(6) Uani 1 1 d . U
H7A H 0.7320 0.2687 0.2723 0.062 Uiso 1 1 calc R U
H7B H 0.5996 0.3005 0.2603 0.062 Uiso 1 1 calc R U
H7C H 0.6025 0.1862 0.2331 0.062 Uiso 1 1 calc R U
C8 C 0.757(3) 0.268(3) 0.4262(12) 0.051(7) Uani 1 1 d . U
H8 H 0.7690 0.2008 0.4268 0.061 Uiso 1 1 calc R U
C9 C 0.819(3) 0.347(3) 0.4726(12) 0.043(6) Uani 1 1 d . U
H9 H 0.8744 0.3323 0.5044 0.052 Uiso 1 1 calc R U
C10 C 0.808(3) 0.444(3) 0.4758(11) 0.044(6) Uani 1 1 d . U
H10 H 0.8547 0.4958 0.5088 0.053 Uiso 1 1 calc R U
C11 C 0.724(2) 0.468(2) 0.4294(11) 0.038(5) Uani 1 1 d . U
C12 C 0.716(3) 0.578(2) 0.4321(12) 0.042(5) Uani 1 1 d . U
H12 H 0.6467 0.5777 0.3980 0.050 Uiso 1 1 calc R U
C13 C 0.673(3) 0.614(3) 0.4882(13) 0.066(8) Uani 1 1 d . U
H13A H 0.7303 0.6029 0.5227 0.099 Uiso 1 1 calc R U
H13B H 0.5831 0.5725 0.4871 0.099 Uiso 1 1 calc R U
H13C H 0.6789 0.6884 0.4908 0.099 Uiso 1 1 calc R U
C14 C 0.840(3) 0.650(2) 0.4242(13) 0.048(6) Uani 1 1 d . U
H14A H 0.9109 0.6498 0.4561 0.072 Uiso 1 1 calc R U
H14B H 0.8323 0.7215 0.4251 0.072 Uiso 1 1 calc R U
H14C H 0.8593 0.6265 0.3862 0.072 Uiso 1 1 calc R U
C15 C 0.233(2) 0.402(2) 0.3317(10) 0.0250(18) Uani 1 1 d . U
C16 C 0.144(2) 0.312(2) 0.3377(10) 0.027(4) Uani 1 1 d . U
C17 C 0.169(3) 0.204(2) 0.3265(12) 0.043(5) Uani 1 1 d . U
H17 H 0.2375 0.2137 0.3018 0.052 Uiso 1 1 calc R U
C18 C 0.051(3) 0.118(3) 0.2904(15) 0.062(8) Uani 1 1 d . U
H18A H 0.0756 0.0526 0.2827 0.094 Uiso 1 1 calc R U
H18B H 0.0222 0.1392 0.2529 0.094 Uiso 1 1 calc R U
H18C H -0.0192 0.1052 0.3125 0.094 Uiso 1 1 calc R U
C19 C 0.229(3) 0.176(3) 0.3836(13) 0.056(8) Uani 1 1 d . U
H19A H 0.1630 0.1567 0.4075 0.084 Uiso 1 1 calc R U
H19B H 0.3006 0.2370 0.4054 0.084 Uiso 1 1 calc R U
H19C H 0.2636 0.1168 0.3748 0.084 Uiso 1 1 calc R U
C20 C 0.029(2) 0.316(2) 0.3553(10) 0.031(4) Uani 1 1 d . U
H20 H -0.0317 0.2529 0.3608 0.037 Uiso 1 1 calc R U
C21 C 0.004(2) 0.411(2) 0.3647(11) 0.037(6) Uani 1 1 d . U
H21 H -0.0779 0.4130 0.3738 0.044 Uiso 1 1 calc R U
C22 C 0.089(2) 0.499(2) 0.3613(10) 0.031(4) Uani 1 1 d . U
H22 H 0.0684 0.5635 0.3703 0.037 Uiso 1 1 calc R U
C23 C 0.208(2) 0.504(2) 0.3452(10) 0.028(4) Uani 1 1 d . U
C24 C 0.309(2) 0.604(2) 0.3439(12) 0.042(5) Uani 1 1 d . U
H24 H 0.3752 0.5867 0.3226 0.050 Uiso 1 1 calc R U
C25 C 0.251(3) 0.681(3) 0.3117(14) 0.056(6) Uani 1 1 d . U
H25A H 0.3210 0.7454 0.3120 0.084 Uiso 1 1 calc R U
H25B H 0.2109 0.6481 0.2709 0.084 Uiso 1 1 calc R U
H25C H 0.1855 0.6983 0.3318 0.084 Uiso 1 1 calc R U
C26 C 0.378(3) 0.660(3) 0.4067(13) 0.059(7) Uani 1 1 d . U
H26A H 0.3203 0.6921 0.4250 0.088 Uiso 1 1 calc R U
H26B H 0.4577 0.7149 0.4048 0.088 Uiso 1 1 calc R U
H26C H 0.4016 0.6088 0.4302 0.088 Uiso 1 1 calc R U
C27 C 0.273(2) 0.354(2) 0.0772(10) 0.0250(18) Uani 1 1 d . U
C28 C 0.191(3) 0.249(2) 0.0562(12) 0.044(5) Uani 1 1 d . U
C29 C 0.195(3) 0.149(3) 0.0819(14) 0.058(6) Uani 1 1 d . U
H29 H 0.2600 0.1714 0.1201 0.070 Uiso 1 1 calc R U
C30 C 0.065(3) 0.088(3) 0.0960(18) 0.081(10) Uani 1 1 d . U
H30A H 0.0498 0.1268 0.1311 0.121 Uiso 1 1 calc R U
H30B H 0.0679 0.0182 0.1033 0.121 Uiso 1 1 calc R U
H30C H -0.0056 0.0819 0.0625 0.121 Uiso 1 1 calc R U
C31 C 0.247(4) 0.079(3) 0.0416(16) 0.079(9) Uani 1 1 d . U
H31A H 0.1924 0.0626 0.0021 0.119 Uiso 1 1 calc R U
H31B H 0.2461 0.0142 0.0575 0.119 Uiso 1 1 calc R U
H31C H 0.3369 0.1169 0.0395 0.119 Uiso 1 1 calc R U
C32 C 0.098(3) 0.243(3) 0.0033(13) 0.059(7) Uani 1 1 d . U
H32 H 0.0390 0.1765 -0.0148 0.070 Uiso 1 1 calc R U
C33 C 0.094(3) 0.325(3) -0.0203(15) 0.063(7) Uani 1 1 d . U
H33 H 0.0306 0.3168 -0.0549 0.076 Uiso 1 1 calc R U
C34 C 0.171(3) 0.417(3) 0.0000(13) 0.057(6) Uani 1 1 d . U
H34 H 0.1662 0.4743 -0.0201 0.068 Uiso 1 1 calc R U
C35 C 0.260(3) 0.431(3) 0.0515(12) 0.044(5) Uani 1 1 d . U
C36 C 0.342(3) 0.539(3) 0.0749(14) 0.054(5) Uani 1 1 d . U
H36 H 0.3908 0.5355 0.1144 0.065 Uiso 1 1 calc R U
C37 C 0.265(3) 0.617(3) 0.0873(14) 0.060(6) Uani 1 1 d . U
H37A H 0.3253 0.6872 0.1027 0.090 Uiso 1 1 calc R U
H37B H 0.2073 0.6195 0.0507 0.090 Uiso 1 1 calc R U
H37C H 0.2122 0.5938 0.1166 0.090 Uiso 1 1 calc R U
C38 C 0.451(4) 0.591(3) 0.0399(19) 0.088(9) Uani 1 1 d . U
H38A H 0.5174 0.5540 0.0429 0.132 Uiso 1 1 calc R U
H38B H 0.4912 0.6654 0.0570 0.132 Uiso 1 1 calc R U
H38C H 0.4110 0.5855 -0.0017 0.132 Uiso 1 1 calc R U
C39 C 0.707(2) 0.379(2) 0.1391(10) 0.0250(18) Uani 1 1 d . U
C40 C 0.736(2) 0.293(2) 0.1063(10) 0.030(4) Uani 1 1 d . U
C41 C 0.637(3) 0.186(2) 0.0890(12) 0.044(5) Uani 1 1 d . U
H41 H 0.5575 0.1872 0.1051 0.052 Uiso 1 1 calc R U
C42 C 0.694(3) 0.106(3) 0.1161(14) 0.057(7) Uani 1 1 d . U
H42A H 0.7693 0.1005 0.0989 0.086 Uiso 1 1 calc R U
H42B H 0.6283 0.0369 0.1081 0.086 Uiso 1 1 calc R U
H42C H 0.7227 0.1284 0.1588 0.086 Uiso 1 1 calc R U
C43 C 0.598(3) 0.156(3) 0.0218(13) 0.057(7) Uani 1 1 d . U
H43A H 0.5697 0.2118 0.0049 0.085 Uiso 1 1 calc R U
H43B H 0.5263 0.0899 0.0115 0.085 Uiso 1 1 calc R U
H43C H 0.6729 0.1461 0.0060 0.085 Uiso 1 1 calc R U
C44 C 0.855(2) 0.316(2) 0.0882(10) 0.032(5) Uani 1 1 d . U
H44 H 0.8736 0.2615 0.0647 0.038 Uiso 1 1 calc R U
C45 C 0.943(2) 0.409(2) 0.1019(11) 0.032(4) Uani 1 1 d . U
H45 H 1.0215 0.4208 0.0876 0.039 Uiso 1 1 calc R U
C46 C 0.920(2) 0.491(2) 0.1372(10) 0.032(4) Uani 1 1 d . U
H46 H 0.9842 0.5576 0.1480 0.038 Uiso 1 1 calc R U
C47 C 0.803(2) 0.472(2) 0.1564(11) 0.032(4) Uani 1 1 d . U
C48 C 0.780(3) 0.561(2) 0.1962(12) 0.039(4) Uani 1 1 d . U
H48 H 0.6985 0.5729 0.1753 0.047 Uiso 1 1 calc R U
C49 C 0.884(3) 0.668(2) 0.2080(14) 0.055(7) Uani 1 1 d . U
H49A H 0.9612 0.6644 0.2351 0.082 Uiso 1 1 calc R U
H49B H 0.8496 0.7217 0.2257 0.082 Uiso 1 1 calc R U
H49C H 0.9079 0.6860 0.1708 0.082 Uiso 1 1 calc R U
C50 C 0.749(2) 0.525(2) 0.2557(10) 0.027(5) Uani 1 1 d . U
H50A H 0.7347 0.5829 0.2806 0.041 Uiso 1 1 calc R U
H50B H 0.6703 0.4644 0.2473 0.041 Uiso 1 1 calc R U
H50C H 0.8224 0.5047 0.2762 0.041 Uiso 1 1 calc R U
C51 C 0.657(3) 0.813(4) 0.3388(19) 0.091(9) Uani 1 1 d . U
H51A H 0.6894 0.8338 0.3815 0.137 Uiso 1 1 calc R U
H51B H 0.5722 0.8255 0.3280 0.137 Uiso 1 1 calc R U
H51C H 0.6479 0.7381 0.3278 0.137 Uiso 1 1 calc R U
C52 C 0.754(4) 0.879(4) 0.306(2) 0.122(16) Uani 1 1 d . U
H52A H 0.7641 0.9548 0.3142 0.146 Uiso 1 1 calc R U
H52B H 0.8408 0.8662 0.3140 0.146 Uiso 1 1 calc R U
O2 O 0.681(2) 0.831(2) 0.2479(13) 0.090(6) Uani 1 1 d . U
C53 C 0.756(4) 0.889(4) 0.211(2) 0.099(10) Uani 1 1 d . U
H53A H 0.7527 0.9623 0.2168 0.119 Uiso 1 1 calc R U
H53B H 0.8485 0.8900 0.2230 0.119 Uiso 1 1 calc R U
C54 C 0.709(4) 0.843(4) 0.151(2) 0.105(12) Uani 1 1 d . U
H54A H 0.7043 0.7685 0.1465 0.158 Uiso 1 1 calc R U
H54B H 0.7678 0.8794 0.1273 0.158 Uiso 1 1 calc R U
H54C H 0.6218 0.8504 0.1384 0.158 Uiso 1 1 calc R U
O1 O 0.344(2) 0.8320(19) 0.1959(11) 0.079(5) Uani 1 1 d D U
C100 C 0.210(3) 0.809(3) 0.187(2) 0.114(13) Uani 1 1 d D U
H10A H 0.1710 0.7481 0.2057 0.137 Uiso 1 1 calc R U
H10B H 0.1695 0.7951 0.1446 0.137 Uiso 1 1 calc R U
C101 C 0.194(4) 0.908(4) 0.217(3) 0.17(2) Uani 1 1 d D U
H10C H 0.1863 0.9032 0.2583 0.199 Uiso 1 1 calc R U
H10D H 0.1157 0.9233 0.1960 0.199 Uiso 1 1 calc R U
C102 C 0.323(5) 0.995(3) 0.213(3) 0.16(2) Uani 1 1 d D U
H10E H 0.3045 1.0433 0.1856 0.190 Uiso 1 1 calc R U
H10F H 0.3668 1.0369 0.2523 0.190 Uiso 1 1 calc R U
C103 C 0.407(4) 0.933(3) 0.190(2) 0.103(11) Uani 1 1 d D U
H10G H 0.4108 0.9400 0.1487 0.124 Uiso 1 1 calc R U
H10H H 0.4961 0.9572 0.2144 0.124 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'
K K 0.2009 0.2494 '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'
W W -0.8490 6.8722 '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'
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
N3 W1 N2 176.6(6) . .
N3 W1 W2 89.2(4) . .
N2 W1 W2 88.4(5) . .
N3 W1 K1 108.2(5) . 1_455
N2 W1 K1 73.9(5) . 1_455
W2 W1 K1 161.41(10) . 1_455
N3 W1 K2 88.2(5) . .
N2 W1 K2 94.4(5) . .
W2 W1 K2 92.93(11) . .
K1 W1 K2 93.89(15) 1_455 .
N1 W2 N4 179.6(6) . .
N1 W2 C50 97.3(8) . .
N4 W2 C50 82.8(8) . .
N1 W2 W1 89.9(4) . .
N4 W2 W1 89.7(5) . .
C50 W2 W1 123.8(6) . .
C46 K1 C45 26.9(7) . .
C46 K1 C16 161.2(8) . 1_655
C45 K1 C16 164.4(7) . 1_655
C46 K1 C15 138.0(8) . 1_655
C45 K1 C15 144.9(7) . 1_655
C16 K1 C15 25.8(7) 1_655 1_655
C46 K1 C20 147.1(7) . 1_655
C45 K1 C20 169.2(6) . 1_655
C16 K1 C20 25.9(6) 1_655 1_655
C15 K1 C20 45.2(6) 1_655 1_655
C46 K1 C23 115.6(7) . 1_655
C45 K1 C23 134.2(8) . 1_655
C16 K1 C23 45.7(7) 1_655 1_655
C15 K1 C23 26.7(6) 1_655 1_655
C20 K1 C23 51.7(7) 1_655 1_655
C46 K1 C21 123.2(7) . 1_655
C45 K1 C21 149.6(7) . 1_655
C16 K1 C21 44.6(6) 1_655 1_655
C15 K1 C21 51.7(6) 1_655 1_655
C20 K1 C21 24.8(7) 1_655 1_655
C23 K1 C21 42.9(6) 1_655 1_655
C46 K1 C44 43.9(7) . .
C45 K1 C44 23.8(7) . .
C16 K1 C44 154.8(7) 1_655 .
C15 K1 C44 160.1(6) 1_655 .
C20 K1 C44 149.0(7) 1_655 .
C23 K1 C44 157.9(7) 1_655 .
C21 K1 C44 148.1(6) 1_655 .
C46 K1 C47 25.1(6) . .
C45 K1 C47 44.5(6) . .
C16 K1 C47 150.6(6) 1_655 .
C15 K1 C47 144.4(7) 1_655 .
C20 K1 C47 126.2(6) 1_655 .
C23 K1 C47 117.7(7) 1_655 .
C21 K1 C47 106.1(6) 1_655 .
C44 K1 C47 49.1(6) . .
C46 K1 C22 111.7(7) . 1_655
C45 K1 C22 137.5(7) . 1_655
C16 K1 C22 51.1(7) 1_655 1_655
C15 K1 C22 44.6(6) 1_655 1_655
C20 K1 C22 42.4(7) 1_655 1_655
C23 K1 C22 24.6(6) 1_655 1_655
C21 K1 C22 22.9(6) 1_655 1_655
C44 K1 C22 152.3(6) . 1_655
C47 K1 C22 103.2(6) . 1_655
C46 K1 W1 107.7(5) . 1_655
C45 K1 W1 95.3(5) . 1_655
C16 K1 W1 69.8(4) 1_655 1_655
C15 K1 W1 54.2(4) 1_655 1_655
C20 K1 W1 95.5(4) 1_655 1_655
C23 K1 W1 68.8(4) 1_655 1_655
C21 K1 W1 105.7(4) 1_655 1_655
C44 K1 W1 106.1(4) . 1_655
C47 K1 W1 132.7(5) . 1_655
C22 K1 W1 93.2(4) 1_655 1_655
O1 K2 O2 84.1(7) . .
O1 K2 C37 69.4(8) . .
O2 K2 C37 123.3(9) . .
O1 K2 C25 73.2(8) . .
O2 K2 C25 113.5(9) . .
C37 K2 C25 105.6(8) . .
O1 K2 C51 93.5(9) . .
O2 K2 C51 41.1(10) . .
C37 K2 C51 159.8(10) . .
C25 K2 C51 78.3(9) . .
O1 K2 C36 94.1(7) . .
O2 K2 C36 120.3(9) . .
C37 K2 C36 26.2(7) . .
C25 K2 C36 123.0(8) . .
C51 K2 C36 158.8(9) . .
O1 K2 W1 141.5(5) . .
O2 K2 W1 134.3(6) . .
C37 K2 W1 86.5(6) . .
C25 K2 W1 85.7(6) . .
C51 K2 W1 113.7(8) . .
C36 K2 W1 70.5(5) . .
C1 N1 C3 112.9(17) . .
C1 N1 W2 121.8(14) . .
C3 N1 W2 124.1(13) . .
N2 C1 N1 118.0(19) . .
N2 C1 H1 121.0 . .
N1 C1 H1 121.0 . .
C1 N2 C15 113.5(18) . .
C1 N2 W1 121.9(14) . .
C15 N2 W1 124.6(14) . .
C2 N3 C27 110.3(17) . .
C2 N3 W1 120.3(14) . .
C27 N3 W1 129.4(13) . .
N4 C2 N3 121(2) . .
N4 C2 H2 119.4 . .
N3 C2 H2 119.4 . .
C2 N4 C39 116.6(19) . .
C2 N4 W2 119.4(14) . .
C39 N4 W2 123.5(14) . .
C4 C3 C11 126(2) . .
C4 C3 N1 114(2) . .
C11 C3 N1 120(2) . .
C3 C4 C8 114(2) . .
C3 C4 C5 123(2) . .
C8 C4 C5 123(2) . .
C6 C5 C7 114(2) . .
C6 C5 C4 113(2) . .
C7 C5 C4 108(2) . .
C6 C5 H5 107.1 . .
C7 C5 H5 107.1 . .
C4 C5 H5 107.1 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 C4 121(3) . .
C9 C8 H8 119.7 . .
C4 C8 H8 119.7 . .
C10 C9 C8 124(3) . .
C10 C9 H9 118.0 . .
C8 C9 H9 118.0 . .
C9 C10 C11 119(3) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
C3 C11 C10 116(3) . .
C3 C11 C12 125(2) . .
C10 C11 C12 119(2) . .
C11 C12 C14 110(2) . .
C11 C12 C13 112(3) . .
C14 C12 C13 113(3) . .
C11 C12 H12 107.2 . .
C14 C12 H12 107.2 . .
C13 C12 H12 107.2 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 N2 121(2) . .
C16 C15 C23 120(2) . .
N2 C15 C23 119(2) . .
C16 C15 K1 76.1(13) . 1_455
N2 C15 K1 107.2(13) . 1_455
C23 C15 K1 84.0(12) . 1_455
C15 C16 C20 121(2) . .
C15 C16 C17 121(2) . .
C20 C16 C17 118(2) . .
C15 C16 K1 78.1(13) . 1_455
C20 C16 K1 82.1(13) . 1_455
C17 C16 K1 111.4(15) . 1_455
C19 C17 C18 114(3) . .
C19 C17 C16 111(2) . .
C18 C17 C16 114(2) . .
C19 C17 H17 105.9 . .
C18 C17 H17 105.9 . .
C16 C17 H17 105.9 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C21 C20 C16 119(3) . .
C21 C20 K1 81.5(15) . 1_455
C16 C20 K1 71.9(13) . 1_455
C21 C20 H20 120.5 . .
C16 C20 H20 120.5 . .
K1 C20 H20 116.9 1_455 .
C22 C21 C20 122(2) . .
C22 C21 K1 81.3(16) . 1_455
C20 C21 K1 73.7(14) . 1_455
C22 C21 H21 119.1 . .
C20 C21 H21 119.1 . .
K1 C21 H21 116.4 1_455 .
C21 C22 C23 123(3) . .
C21 C22 K1 75.8(16) . 1_455
C23 C22 K1 75.0(14) . 1_455
C21 C22 H22 118.5 . .
C23 C22 H22 118.5 . .
K1 C22 H22 121.9 1_455 .
C22 C23 C15 116(2) . .
C22 C23 C24 124(2) . .
C15 C23 C24 121(2) . .
C22 C23 K1 80.4(14) . 1_455
C15 C23 K1 69.3(12) . 1_455
C24 C23 K1 121.4(16) . 1_455
C23 C24 C26 111(2) . .
C23 C24 C25 112(2) . .
C26 C24 C25 108(2) . .
C23 C24 H24 108.3 . .
C26 C24 H24 108.3 . .
C25 C24 H24 108.3 . .
C24 C25 K2 88.0(16) . .
C24 C25 H25A 109.5 . .
K2 C25 H25A 62.4 . .
C24 C25 H25B 109.5 . .
K2 C25 H25B 62.8 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
K2 C25 H25C 162.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C35 C27 C28 122(2) . .
C35 C27 N3 124(3) . .
C28 C27 N3 114(2) . .
C27 C28 C32 112(3) . .
C27 C28 C29 128(2) . .
C32 C28 C29 120(3) . .
C31 C29 C28 110(3) . .
C31 C29 C30 112(3) . .
C28 C29 C30 113(3) . .
C31 C29 H29 106.9 . .
C28 C29 H29 106.9 . .
C30 C29 H29 106.9 . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C33 C32 C28 122(3) . .
C33 C32 H32 119.2 . .
C28 C32 H32 119.2 . .
C34 C33 C32 124(4) . .
C34 C33 H33 118.0 . .
C32 C33 H33 118.0 . .
C33 C34 C35 119(3) . .
C33 C34 H34 120.7 . .
C35 C34 H34 120.7 . .
C27 C35 C34 122(3) . .
C27 C35 C36 121(3) . .
C34 C35 C36 117(3) . .
C35 C36 C37 114(3) . .
C35 C36 C38 118(3) . .
C37 C36 C38 109(3) . .
C35 C36 K2 130.9(19) . .
C37 C36 K2 69.3(17) . .
C38 C36 K2 105(2) . .
C35 C36 H36 105.0 . .
C37 C36 H36 105.0 . .
C38 C36 H36 105.0 . .
K2 C36 H36 37.7 . .
C36 C37 K2 84.5(17) . .
C36 C37 H37A 109.5 . .
K2 C37 H37A 58.0 . .
C36 C37 H37B 109.5 . .
K2 C37 H37B 164.6 . .
H37A C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
K2 C37 H37C 70.2 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C36 C38 H38A 109.5 . .
C36 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C36 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
C47 C39 N4 119(2) . .
C47 C39 C40 118(2) . .
N4 C39 C40 123(2) . .
C44 C40 C39 117(2) . .
C44 C40 C41 122(2) . .
C39 C40 C41 121(2) . .
C40 C41 C42 109(2) . .
C40 C41 C43 111(2) . .
C42 C41 C43 111(2) . .
C40 C41 H41 108.8 . .
C42 C41 H41 108.8 . .
C43 C41 H41 108.8 . .
C41 C42 H42A 109.5 . .
C41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C45 C44 C40 124(3) . .
C45 C44 K1 66.6(14) . .
C40 C44 K1 90.8(15) . .
C45 C44 H44 118.2 . .
C40 C44 H44 118.2 . .
K1 C44 H44 113.9 . .
C44 C45 C46 120(2) . .
C44 C45 K1 89.6(16) . .
C46 C45 K1 75.8(14) . .
C44 C45 H45 119.8 . .
C46 C45 H45 119.8 . .
K1 C45 H45 104.7 . .
C47 C46 C45 118(3) . .
C47 C46 K1 89.6(15) . .
C45 C46 K1 77.3(14) . .
C47 C46 H46 120.8 . .
C45 C46 H46 120.8 . .
K1 C46 H46 102.8 . .
C39 C47 C46 122(2) . .
C39 C47 C48 120(2) . .
C46 C47 C48 118(2) . .
C39 C47 K1 94.2(15) . .
C46 C47 K1 65.3(13) . .
C48 C47 K1 112.5(15) . .
C47 C48 C49 117(2) . .
C47 C48 C50 111(2) . .
C49 C48 C50 111(2) . .
C47 C48 H48 105.8 . .
C49 C48 H48 105.8 . .
C50 C48 H48 105.8 . .
C48 C49 H49A 109.5 . .
C48 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
C48 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C48 C50 W2 116.1(17) . .
C48 C50 H50A 109.5 . .
W2 C50 H50A 107.7 . .
C48 C50 H50B 109.5 . .
W2 C50 H50B 7.0 . .
H50A C50 H50B 109.5 . .
C48 C50 H50C 109.5 . .
W2 C50 H50C 104.4 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C52 C51 K2 96(3) . .
C52 C51 H51A 109.5 . .
K2 C51 H51A 154.9 . .
C52 C51 H51B 109.5 . .
K2 C51 H51B 60.7 . .
H51A C51 H51B 109.5 . .
C52 C51 H51C 109.5 . .
K2 C51 H51C 59.1 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
O2 C52 C51 96(3) . .
O2 C52 H52A 112.6 . .
C51 C52 H52A 112.6 . .
O2 C52 H52B 112.6 . .
C51 C52 H52B 112.6 . .
H52A C52 H52B 110.1 . .
C52 O2 C53 102(3) . .
C52 O2 K2 128(3) . .
C53 O2 K2 130(3) . .
C54 C53 O2 111(4) . .
C54 C53 H53A 109.5 . .
O2 C53 H53A 109.5 . .
C54 C53 H53B 109.5 . .
O2 C53 H53B 109.5 . .
H53A C53 H53B 108.1 . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C103 O1 C100 114(3) . .
C103 O1 K2 128.5(19) . .
C100 O1 K2 118(2) . .
O1 C100 C101 102(3) . .
O1 C100 H10A 111.4 . .
C101 C100 H10A 111.4 . .
O1 C100 H10B 111.4 . .
C101 C100 H10B 111.4 . .
H10A C100 H10B 109.2 . .
C100 C101 C102 103(2) . .
C100 C101 H10C 111.1 . .
C102 C101 H10C 111.1 . .
C100 C101 H10D 111.1 . .
C102 C101 H10D 111.1 . .
H10C C101 H10D 109.0 . .
C103 C102 C101 104(2) . .
C103 C102 H10E 110.9 . .
C101 C102 H10E 110.9 . .
C103 C102 H10F 110.9 . .
C101 C102 H10F 110.9 . .
H10E C102 H10F 108.9 . .
O1 C103 C102 103(3) . .
O1 C103 H10G 111.1 . .
C102 C103 H10G 111.1 . .
O1 C103 H10H 111.1 . .
C102 C103 H10H 111.1 . .
H10G C103 H10H 109.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N3 2.105(17) .
W1 N2 2.119(17) .
W1 W2 2.4067(13) .
W1 K1 3.697(6) 1_455
W1 K2 3.705(8) .
W2 N1 2.081(17) .
W2 N4 2.121(18) .
W2 C50 2.23(3) .
K1 C46 2.98(2) .
K1 C45 3.00(2) .
K1 C16 3.03(2) 1_655
K1 C15 3.06(2) 1_655
K1 C20 3.16(2) 1_655
K1 C23 3.25(2) 1_655
K1 C21 3.26(3) 1_655
K1 C44 3.27(2) .
K1 C47 3.28(2) .
K1 C22 3.32(2) 1_655
K1 W1 3.697(6) 1_655
K2 O1 2.74(2) .
K2 O2 2.75(3) .
K2 C37 3.24(3) .
K2 C25 3.33(3) .
K2 C51 3.33(4) .
K2 C36 3.45(3) .
N1 C1 1.37(3) .
N1 C3 1.46(3) .
C1 N2 1.36(3) .
C1 H1 0.9500 .
N2 C15 1.39(3) .
N3 C2 1.37(3) .
N3 C27 1.46(3) .
C2 N4 1.35(3) .
C2 H2 0.9500 .
N4 C39 1.36(3) .
C3 C4 1.38(4) .
C3 C11 1.39(4) .
C4 C8 1.41(4) .
C4 C5 1.56(4) .
C5 C6 1.50(4) .
C5 C7 1.54(4) .
C5 H5 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.37(4) .
C8 H8 0.9500 .
C9 C10 1.32(4) .
C9 H9 0.9500 .
C10 C11 1.42(4) .
C10 H10 0.9500 .
C11 C12 1.49(4) .
C12 C14 1.49(4) .
C12 C13 1.53(4) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.36(4) .
C15 C23 1.47(4) .
C15 K1 3.06(2) 1_455
C16 C20 1.40(3) .
C16 C17 1.54(4) .
C16 K1 3.03(2) 1_455
C17 C19 1.51(4) .
C17 C18 1.53(4) .
C17 H17 1.0000 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.38(4) .
C20 K1 3.16(2) 1_455
C20 H20 0.9500 .
C21 C22 1.30(4) .
C21 K1 3.26(3) 1_455
C21 H21 0.9500 .
C22 C23 1.40(3) .
C22 K1 3.32(2) 1_455
C22 H22 0.9500 .
C23 C24 1.49(4) .
C23 K1 3.25(2) 1_455
C24 C26 1.54(4) .
C24 C25 1.54(4) .
C24 H24 1.0000 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 C35 1.28(4) .
C27 C28 1.42(4) .
C28 C32 1.44(4) .
C28 C29 1.53(4) .
C29 C31 1.53(4) .
C29 C30 1.54(5) .
C29 H29 1.0000 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 C33 1.29(5) .
C32 H32 0.9500 .
C33 C34 1.27(5) .
C33 H33 0.9500 .
C34 C35 1.37(4) .
C34 H34 0.9500 .
C35 C36 1.48(4) .
C36 C37 1.53(4) .
C36 C38 1.59(5) .
C36 H36 1.0000 .
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 C47 1.36(4) .
C39 C40 1.45(3) .
C40 C44 1.39(3) .
C40 C41 1.51(4) .
C41 C42 1.52(4) .
C41 C43 1.53(4) .
C41 H41 1.0000 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 C45 1.32(4) .
C44 H44 0.9500 .
C45 C46 1.39(4) .
C45 H45 0.9500 .
C46 C47 1.39(3) .
C46 H46 0.9500 .
C47 C48 1.53(4) .
C48 C49 1.53(4) .
C48 C50 1.57(4) .
C48 H48 1.0000 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C51 C52 1.54(6) .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C52 O2 1.43(5) .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
O2 C53 1.42(5) .
C53 C54 1.42(6) .
C53 H53A 0.9900 .
C53 H53B 0.9900 .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
O1 C103 1.37(3) .
O1 C100 1.39(3) .
C100 C101 1.49(4) .
C100 H10A 0.9900 .
C100 H10B 0.9900 .
C101 C102 1.59(7) .
C101 H10C 0.9900 .
C101 H10D 0.9900 .
C102 C103 1.50(4) .
C102 H10E 0.9900 .
C102 H10F 0.9900 .
C103 H10G 0.9900 .
C103 H10H 0.9900 .
