#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321494.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_4321494
loop_
_publ_author_name
'Carl Redshaw'
'Mark R. J. Elsegood'
_publ_section_title
;
 Group 6 Metallocalixarenes Bearing "Hydrazido(2-)" Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5164
_journal_page_last               5168
_journal_paper_doi               10.1021/ic000098i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C62 H71 N5 O4 W'
_chemical_formula_weight         1134.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.057(2)
_cell_angle_beta                 91.513(2)
_cell_angle_gamma                108.029(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7852(6)
_cell_length_b                   14.7376(8)
_cell_length_c                   18.2479(9)
_cell_measurement_reflns_used    14244
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.23
_cell_volume                     2747.6(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16884
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00080(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11800
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0284P)²+2.6383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                11128
_reflns_number_total             11800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000098i_1.cif
_cod_data_source_block           1
_cod_database_code               4321494
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.634646(8) 0.759268(6) 0.644937(5) 0.01750(4) Uani 1 1 d . . .
N1 N 0.69085(18) 0.68579(14) 0.58341(11) 0.0217(4) Uani 1 1 d . . .
N2 N 0.72744(19) 0.61903(14) 0.54475(11) 0.0229(4) Uani 1 1 d . . .
C1 C 0.8490(2) 0.64935(17) 0.51008(12) 0.0224(4) Uani 1 1 d . . .
C2 C 0.9151(2) 0.74665(18) 0.50825(14) 0.0270(5) Uani 1 1 d . . .
H2 H 0.8809 0.7932 0.5310 0.032 Uiso 1 1 calc R . .
C3 C 1.0318(3) 0.7748(2) 0.47278(15) 0.0334(6) Uani 1 1 d . . .
H3 H 1.0767 0.8411 0.4710 0.040 Uiso 1 1 calc R . .
C4 C 1.0832(3) 0.7084(2) 0.44019(16) 0.0371(6) Uani 1 1 d . . .
H4 H 1.1638 0.7287 0.4169 0.045 Uiso 1 1 calc R . .
C5 C 1.0168(3) 0.6116(2) 0.44156(16) 0.0372(6) Uani 1 1 d . . .
H5 H 1.0514 0.5656 0.4183 0.045 Uiso 1 1 calc R . .
C6 C 0.9000(3) 0.58147(19) 0.47672(14) 0.0307(5) Uani 1 1 d . . .
H6 H 0.8552 0.5151 0.4780 0.037 Uiso 1 1 calc R . .
C7 C 0.6857(2) 0.52680(16) 0.57552(13) 0.0227(4) Uani 1 1 d . . .
C8 C 0.6180(2) 0.44508(17) 0.53134(14) 0.0273(5) Uani 1 1 d . . .
H8 H 0.5976 0.4489 0.4809 0.033 Uiso 1 1 calc R . .
C9 C 0.5805(3) 0.35729(18) 0.56198(15) 0.0320(5) Uani 1 1 d . . .
H9 H 0.5351 0.3006 0.5322 0.038 Uiso 1 1 calc R . .
C10 C 0.6090(3) 0.35252(18) 0.63540(15) 0.0330(6) Uani 1 1 d . . .
H10 H 0.5838 0.2923 0.6558 0.040 Uiso 1 1 calc R . .
C11 C 0.6745(3) 0.43537(19) 0.67990(15) 0.0326(5) Uani 1 1 d . . .
H11 H 0.6922 0.4318 0.7307 0.039 Uiso 1 1 calc R . .
C12 C 0.7139(2) 0.52312(17) 0.64962(14) 0.0288(5) Uani 1 1 d . . .
H12 H 0.7596 0.5799 0.6793 0.035 Uiso 1 1 calc R . .
O1 O 0.72157(15) 0.72845(11) 0.73213(9) 0.0212(3) Uani 1 1 d . . .
O2 O 0.77618(15) 0.87744(11) 0.64179(8) 0.0202(3) Uani 1 1 d . . .
O3 O 0.53233(15) 0.80609(11) 0.57458(8) 0.0193(3) Uani 1 1 d . . .
O4 O 0.47585(15) 0.66344(11) 0.66845(9) 0.0213(3) Uani 1 1 d . . .
C13 C 0.7164(2) 0.76245(16) 0.80321(12) 0.0197(4) Uani 1 1 d . . .
C14 C 0.6171(2) 0.71277(16) 0.84718(12) 0.0201(4) Uani 1 1 d . . .
C15 C 0.6120(2) 0.75167(17) 0.91881(13) 0.0227(4) Uani 1 1 d . . .
H15 H 0.5440 0.7189 0.9485 0.027 Uiso 1 1 calc R . .
C16 C 0.7036(2) 0.83711(17) 0.94819(13) 0.0237(5) Uani 1 1 d . . .
C17 C 0.8023(2) 0.88255(16) 0.90324(13) 0.0228(4) Uani 1 1 d . . .
H17 H 0.8672 0.9396 0.9226 0.027 Uiso 1 1 calc R . .
C18 C 0.8099(2) 0.84790(16) 0.83113(12) 0.0198(4) Uani 1 1 d . . .
C19 C 0.7009(3) 0.8809(2) 1.02697(15) 0.0351(6) Uani 1 1 d . . .
C20 C 0.7121(5) 0.9867(3) 1.0258(2) 0.0712(13) Uani 1 1 d . . .
H20A H 0.7927 1.0204 1.0028 0.107 Uiso 1 1 calc R . .
H20B H 0.7137 1.0148 1.0763 0.107 Uiso 1 1 calc R . .
H20C H 0.6369 0.9928 0.9975 0.107 Uiso 1 1 calc R . .
C21 C 0.8193(4) 0.8739(3) 1.07207(18) 0.0638(11) Uani 1 1 d . . .
H21A H 0.8995 0.9057 1.0479 0.096 Uiso 1 1 calc R . .
H21B H 0.8119 0.8064 1.0755 0.096 Uiso 1 1 calc R . .
H21C H 0.8220 0.9052 1.1216 0.096 Uiso 1 1 calc R . .
C22 C 0.5778(3) 0.8304(3) 1.06464(18) 0.0502(8) Uani 1 1 d . . .
H22A H 0.5717 0.7630 1.0676 0.075 Uiso 1 1 calc R . .
H22B H 0.5015 0.8344 1.0363 0.075 Uiso 1 1 calc R . .
H22C H 0.5807 0.8612 1.1143 0.075 Uiso 1 1 calc R . .
C23 C 0.9116(2) 0.90654(16) 0.78251(13) 0.0214(4) Uani 1 1 d . . .
H23A H 0.9294 0.8637 0.7427 0.026 Uiso 1 1 calc R . .
H23B H 0.9941 0.9377 0.8121 0.026 Uiso 1 1 calc R . .
C24 C 0.7961(2) 0.96409(15) 0.68100(12) 0.0180(4) Uani 1 1 d . . .
C25 C 0.8648(2) 0.98261(16) 0.74894(12) 0.0199(4) Uani 1 1 d . . .
C26 C 0.8817(2) 1.07053(16) 0.78860(12) 0.0226(4) Uani 1 1 d . . .
H26 H 0.9295 1.0838 0.8347 0.027 Uiso 1 1 calc R . .
C27 C 0.8314(2) 1.13952(17) 0.76318(13) 0.0235(4) Uani 1 1 d . A .
C28 C 0.7633(2) 1.11773(16) 0.69439(12) 0.0211(4) Uani 1 1 d . . .
H28 H 0.7286 1.1638 0.6756 0.025 Uiso 1 1 calc R . .
C29 C 0.7446(2) 1.03148(16) 0.65244(12) 0.0185(4) Uani 1 1 d . . .
C30 C 0.8489(3) 1.23507(19) 0.80764(15) 0.0340(6) Uani 1 1 d D . .
C31 C 0.9227(8) 1.2469(4) 0.8804(3) 0.060(2) Uani 0.714(9) 1 d PD A 1
H31A H 0.9297 1.3096 0.9053 0.090 Uiso 0.714(9) 1 calc PR A 1
H31B H 1.0103 1.2427 0.8724 0.090 Uiso 0.714(9) 1 calc PR A 1
H31C H 0.8762 1.1963 0.9109 0.090 Uiso 0.714(9) 1 calc PR A 1
C32 C 0.9183(5) 1.3196(3) 0.7622(3) 0.0474(14) Uani 0.714(9) 1 d PD A 1
H32A H 0.8709 1.3125 0.7145 0.071 Uiso 0.714(9) 1 calc PR A 1
H32B H 1.0079 1.3196 0.7544 0.071 Uiso 0.714(9) 1 calc PR A 1
H32C H 0.9201 1.3801 0.7889 0.071 Uiso 0.714(9) 1 calc PR A 1
C33 C 0.7118(5) 1.2440(4) 0.8228(3) 0.0518(14) Uani 0.714(9) 1 d PD A 1
H33A H 0.6612 1.2365 0.7761 0.078 Uiso 0.714(9) 1 calc PR A 1
H33B H 0.7216 1.3070 0.8479 0.078 Uiso 0.714(9) 1 calc PR A 1
H33C H 0.6661 1.1940 0.8541 0.078 Uiso 0.714(9) 1 calc PR A 1
C31A C 0.840(2) 1.2180(12) 0.8902(6) 0.060(5) Uani 0.286(9) 1 d PD A 2
H31D H 0.9013 1.1839 0.9037 0.090 Uiso 0.286(9) 1 calc PR A 2
H31E H 0.7512 1.1797 0.8998 0.090 Uiso 0.286(9) 1 calc PR A 2
H31F H 0.8631 1.2798 0.9196 0.090 Uiso 0.286(9) 1 calc PR A 2
C32A C 0.9978(13) 1.2915(9) 0.7987(10) 0.081(6) Uani 0.286(9) 1 d PD A 2
H32D H 1.0519 1.2533 0.8148 0.122 Uiso 0.286(9) 1 calc PR A 2
H32E H 1.0218 1.3527 0.8288 0.122 Uiso 0.286(9) 1 calc PR A 2
H32F H 1.0120 1.3034 0.7470 0.122 Uiso 0.286(9) 1 calc PR A 2
C33A C 0.760(2) 1.2841(12) 0.7860(11) 0.089(9) Uani 0.286(9) 1 d PD A 2
H33D H 0.7771 1.3442 0.8170 0.133 Uiso 0.286(9) 1 calc PR A 2
H33E H 0.6698 1.2436 0.7918 0.133 Uiso 0.286(9) 1 calc PR A 2
H33F H 0.7707 1.2979 0.7344 0.133 Uiso 0.286(9) 1 calc PR A 2
C34 C 0.6645(2) 1.00844(15) 0.57966(12) 0.0187(4) Uani 1 1 d . . .
H34A H 0.6943 0.9628 0.5479 0.022 Uiso 1 1 calc R . .
H34B H 0.6796 1.0678 0.5543 0.022 Uiso 1 1 calc R . .
C35 C 0.4601(2) 0.86611(15) 0.59027(11) 0.0176(4) Uani 1 1 d . . .
C36 C 0.5189(2) 0.96534(16) 0.59026(11) 0.0180(4) Uani 1 1 d . . .
C37 C 0.4426(2) 1.02513(15) 0.60364(11) 0.0182(4) Uani 1 1 d . . .
H37 H 0.4817 1.0923 0.6023 0.022 Uiso 1 1 calc R . .
C38 C 0.3112(2) 0.99018(16) 0.61885(11) 0.0186(4) Uani 1 1 d . . .
C39 C 0.2577(2) 0.89105(16) 0.62134(12) 0.0195(4) Uani 1 1 d . . .
H39 H 0.1690 0.8658 0.6332 0.023 Uiso 1 1 calc R . .
C40 C 0.3285(2) 0.82804(15) 0.60726(11) 0.0184(4) Uani 1 1 d . . .
C41 C 0.2284(2) 1.05655(16) 0.63522(13) 0.0219(4) Uani 1 1 d . . .
C42 C 0.2124(3) 1.0647(2) 0.71859(15) 0.0349(6) Uani 1 1 d . . .
H42A H 0.1558 1.1041 0.7298 0.052 Uiso 1 1 calc R . .
H42B H 0.2981 1.0945 0.7440 0.052 Uiso 1 1 calc R . .
H42C H 0.1730 1.0007 0.7351 0.052 Uiso 1 1 calc R . .
C43 C 0.2919(2) 1.15712(17) 0.61116(16) 0.0310(5) Uani 1 1 d . . .
H43A H 0.2309 1.1942 0.6166 0.046 Uiso 1 1 calc R . .
H43B H 0.3139 1.1526 0.5595 0.046 Uiso 1 1 calc R . .
H43C H 0.3715 1.1889 0.6419 0.046 Uiso 1 1 calc R . .
C44 C 0.0937(2) 1.01608(18) 0.59465(15) 0.0300(5) Uani 1 1 d . . .
H44A H 0.0419 1.0591 0.6059 0.045 Uiso 1 1 calc R . .
H44B H 0.0486 0.9526 0.6107 0.045 Uiso 1 1 calc R . .
H44C H 0.1044 1.0107 0.5415 0.045 Uiso 1 1 calc R . .
C45 C 0.2647(2) 0.72079(15) 0.61233(12) 0.0202(4) Uani 1 1 d . . .
H45A H 0.1720 0.7031 0.5948 0.024 Uiso 1 1 calc R . .
H45B H 0.3081 0.6854 0.5792 0.024 Uiso 1 1 calc R . .
C46 C 0.3793(2) 0.66480(15) 0.71538(12) 0.0193(4) Uani 1 1 d . . .
C47 C 0.2713(2) 0.68953(15) 0.68996(12) 0.0190(4) Uani 1 1 d . . .
C48 C 0.1712(2) 0.68540(16) 0.73787(13) 0.0215(4) Uani 1 1 d . . .
H48 H 0.0972 0.7016 0.7211 0.026 Uiso 1 1 calc R . .
C49 C 0.1758(2) 0.65847(15) 0.80928(13) 0.0212(4) Uani 1 1 d . . .
C50 C 0.2877(2) 0.63786(15) 0.83295(12) 0.0212(4) Uani 1 1 d . . .
H50 H 0.2942 0.6213 0.8820 0.025 Uiso 1 1 calc R . .
C51 C 0.3898(2) 0.64069(15) 0.78739(12) 0.0202(4) Uani 1 1 d . . .
C52 C 0.0645(2) 0.65604(18) 0.86097(13) 0.0258(5) Uani 1 1 d . . .
C53 C 0.0869(3) 0.7579(2) 0.89705(18) 0.0447(7) Uani 1 1 d . . .
H53A H 0.0146 0.7580 0.9284 0.067 Uiso 1 1 calc R . .
H53B H 0.0912 0.8019 0.8587 0.067 Uiso 1 1 calc R . .
H53C H 0.1691 0.7784 0.9270 0.067 Uiso 1 1 calc R . .
C54 C 0.0607(3) 0.5887(2) 0.92175(17) 0.0427(7) Uani 1 1 d . . .
H54A H -0.0148 0.5853 0.9514 0.064 Uiso 1 1 calc R . .
H54B H 0.1410 0.6131 0.9532 0.064 Uiso 1 1 calc R . .
H54C H 0.0534 0.5246 0.8995 0.064 Uiso 1 1 calc R . .
C55 C -0.0683(3) 0.6221(2) 0.81844(17) 0.0402(7) Uani 1 1 d . . .
H55A H -0.1379 0.6163 0.8530 0.060 Uiso 1 1 calc R . .
H55B H -0.0799 0.5596 0.7918 0.060 Uiso 1 1 calc R . .
H55C H -0.0721 0.6685 0.7833 0.060 Uiso 1 1 calc R . .
C56 C 0.5124(2) 0.62148(16) 0.81648(13) 0.0212(4) Uani 1 1 d . . .
H56A H 0.4889 0.5769 0.8557 0.025 Uiso 1 1 calc R . .
H56B H 0.5481 0.5901 0.7762 0.025 Uiso 1 1 calc R . .
N3 N 0.56256(17) 0.84887(13) 0.72898(10) 0.0186(4) Uani 1 1 d . . .
C57 C 0.5193(3) 0.8895(2) 0.76828(15) 0.0358(6) Uani 1 1 d . . .
C58 C 0.4591(7) 0.9413(5) 0.8194(3) 0.104(2) Uani 1 1 d D . .
H58A H 0.531(5) 0.991(3) 0.848(3) 0.156 Uiso 1 1 d D . .
H58B H 0.406(4) 0.897(4) 0.853(3) 0.156 Uiso 1 1 d D . .
H58C H 0.405(4) 0.971(4) 0.792(3) 0.156 Uiso 1 1 d D . .
N4 N 0.3375(7) 0.3412(4) 0.7953(3) 0.125(2) Uani 1 1 d . . .
C59 C 0.3245(5) 0.3739(3) 0.7429(2) 0.0670(11) Uani 1 1 d . . .
C60 C 0.3094(5) 0.4160(3) 0.6766(2) 0.0636(10) Uani 1 1 d . . .
H60A H 0.3890 0.4685 0.6696 0.095 Uiso 1 1 calc R . .
H60B H 0.2351 0.4409 0.6796 0.095 Uiso 1 1 calc R . .
H60C H 0.2936 0.3674 0.6349 0.095 Uiso 1 1 calc R . .
N5 N 0.6273(5) 0.4237(3) 0.9650(3) 0.1051(15) Uani 1 1 d . . .
C61 C 0.6681(4) 0.4977(3) 0.9924(2) 0.0574(9) Uani 1 1 d . . .
C62 C 0.7204(4) 0.5918(3) 1.0286(3) 0.0691(11) Uani 1 1 d . . .
H62A H 0.7308 0.6393 0.9924 0.104 Uiso 1 1 calc R . .
H62B H 0.8055 0.5987 1.0527 0.104 Uiso 1 1 calc R . .
H62C H 0.6606 0.6018 1.0656 0.104 Uiso 1 1 calc R . .
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'
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'
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
N1 W1 O4 97.40(8) . . ?
N1 W1 O2 99.02(8) . . ?
O4 W1 O2 163.57(6) . . ?
N1 W1 O3 98.85(8) . . ?
O4 W1 O3 89.20(6) . . ?
O2 W1 O3 88.93(6) . . ?
N1 W1 O1 93.95(8) . . ?
O4 W1 O1 88.18(7) . . ?
O2 W1 O1 90.04(7) . . ?
O3 W1 O1 167.16(6) . . ?
N1 W1 N3 176.98(8) . . ?
O4 W1 N3 81.11(7) . . ?
O2 W1 N3 82.46(6) . . ?
O3 W1 N3 83.79(6) . . ?
O1 W1 N3 83.39(6) . . ?
N2 N1 W1 170.43(17) . . ?
N1 N2 C1 117.46(19) . . ?
N1 N2 C7 112.78(18) . . ?
C1 N2 C7 120.24(18) . . ?
C2 C1 C6 120.1(2) . . ?
C2 C1 N2 120.0(2) . . ?
C6 C1 N2 119.9(2) . . ?
C3 C2 C1 119.2(2) . . ?
C4 C3 C2 121.2(3) . . ?
C3 C4 C5 119.6(2) . . ?
C4 C5 C6 120.4(2) . . ?
C5 C6 C1 119.6(2) . . ?
C8 C7 C12 121.4(2) . . ?
C8 C7 N2 120.1(2) . . ?
C12 C7 N2 118.5(2) . . ?
C7 C8 C9 119.0(2) . . ?
C10 C9 C8 120.2(2) . . ?
C9 C10 C11 120.5(2) . . ?
C12 C11 C10 119.7(2) . . ?
C7 C12 C11 119.2(2) . . ?
C13 O1 W1 125.98(13) . . ?
C24 O2 W1 129.29(13) . . ?
C35 O3 W1 127.00(13) . . ?
C46 O4 W1 133.22(14) . . ?
O1 C13 C18 119.2(2) . . ?
O1 C13 C14 120.2(2) . . ?
C18 C13 C14 120.6(2) . . ?
C15 C14 C13 118.6(2) . . ?
C15 C14 C56 120.4(2) . . ?
C13 C14 C56 120.9(2) . . ?
C16 C15 C14 122.2(2) . . ?
C17 C16 C15 117.2(2) . . ?
C17 C16 C19 119.6(2) . . ?
C15 C16 C19 123.2(2) . . ?
C18 C17 C16 122.7(2) . . ?
C17 C18 C13 118.7(2) . . ?
C17 C18 C23 120.0(2) . . ?
C13 C18 C23 121.2(2) . . ?
C22 C19 C20 108.8(3) . . ?
C22 C19 C21 108.7(3) . . ?
C20 C19 C21 108.1(3) . . ?
C22 C19 C16 112.7(2) . . ?
C20 C19 C16 109.9(2) . . ?
C21 C19 C16 108.5(2) . . ?
C18 C23 C25 110.92(17) . . ?
O2 C24 C25 119.36(19) . . ?
O2 C24 C29 119.26(19) . . ?
C25 C24 C29 121.4(2) . . ?
C24 C25 C26 118.4(2) . . ?
C24 C25 C23 121.3(2) . . ?
C26 C25 C23 120.1(2) . . ?
C27 C26 C25 122.5(2) . . ?
C26 C27 C28 116.9(2) . . ?
C26 C27 C30 122.1(2) . . ?
C28 C27 C30 121.0(2) . . ?
C29 C28 C27 122.8(2) . . ?
C28 C29 C24 117.9(2) . . ?
C28 C29 C34 121.26(19) . . ?
C24 C29 C34 120.72(19) . . ?
C33A C30 C31 127.6(7) . . ?
C33A C30 C27 114.6(6) . . ?
C31 C30 C27 114.4(3) . . ?
C33A C30 C31A 110.9(10) . . ?
C31 C30 C31A 33.8(7) . . ?
C27 C30 C31A 108.9(6) . . ?
C33A C30 C32 69.6(11) . . ?
C31 C30 C32 108.8(4) . . ?
C27 C30 C32 110.3(3) . . ?
C31A C30 C32 135.8(7) . . ?
C33A C30 C33 37.9(10) . . ?
C31 C30 C33 107.7(4) . . ?
C27 C30 C33 108.7(3) . . ?
C31A C30 C33 79.0(7) . . ?
C32 C30 C33 106.6(4) . . ?
C33A C30 C32A 114.7(11) . . ?
C31 C30 C32A 70.6(7) . . ?
C27 C30 C32A 102.6(6) . . ?
C31A C30 C32A 104.4(9) . . ?
C32 C30 C32A 47.3(7) . . ?
C33 C30 C32A 145.6(6) . . ?
C29 C34 C36 112.11(17) . . ?
O3 C35 C36 119.47(19) . . ?
O3 C35 C40 119.90(19) . . ?
C36 C35 C40 120.6(2) . . ?
C37 C36 C35 118.66(19) . . ?
C37 C36 C34 119.92(19) . . ?
C35 C36 C34 121.35(19) . . ?
C38 C37 C36 122.5(2) . . ?
C37 C38 C39 117.1(2) . . ?
C37 C38 C41 122.24(19) . . ?
C39 C38 C41 120.66(19) . . ?
C40 C39 C38 122.9(2) . . ?
C39 C40 C35 118.22(19) . . ?
C39 C40 C45 120.13(19) . . ?
C35 C40 C45 121.63(19) . . ?
C43 C41 C38 112.36(18) . . ?
C43 C41 C42 108.4(2) . . ?
C38 C41 C42 108.31(19) . . ?
C43 C41 C44 107.5(2) . . ?
C38 C41 C44 110.50(19) . . ?
C42 C41 C44 109.8(2) . . ?
C47 C45 C40 113.61(18) . . ?
O4 C46 C51 119.38(19) . . ?
O4 C46 C47 119.33(19) . . ?
C51 C46 C47 121.3(2) . . ?
C48 C47 C46 118.0(2) . . ?
C48 C47 C45 121.39(19) . . ?
C46 C47 C45 120.6(2) . . ?
C49 C48 C47 122.5(2) . . ?
C48 C49 C50 117.3(2) . . ?
C48 C49 C52 121.1(2) . . ?
C50 C49 C52 121.5(2) . . ?
C51 C50 C49 122.4(2) . . ?
C50 C51 C46 118.4(2) . . ?
C50 C51 C56 120.6(2) . . ?
C46 C51 C56 121.0(2) . . ?
C55 C52 C54 108.0(2) . . ?
C55 C52 C49 111.0(2) . . ?
C54 C52 C49 111.6(2) . . ?
C55 C52 C53 109.0(2) . . ?
C54 C52 C53 108.6(2) . . ?
C49 C52 C53 108.6(2) . . ?
C14 C56 C51 112.35(17) . . ?
C57 N3 W1 175.4(2) . . ?
N3 C57 C58 178.5(4) . . ?
N4 C59 C60 179.4(7) . . ?
N5 C61 C62 179.0(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
W1 N1 1.7523(19) . ?
W1 O4 1.9336(16) . ?
W1 O2 1.9338(15) . ?
W1 O3 1.9657(15) . ?
W1 O1 1.9758(15) . ?
W1 N3 2.2610(18) . ?
N1 N2 1.333(3) . ?
N2 C1 1.429(3) . ?
N2 C7 1.452(3) . ?
C1 C2 1.393(3) . ?
C1 C6 1.395(3) . ?
C2 C3 1.390(4) . ?
C3 C4 1.375(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.390(4) . ?
C7 C8 1.386(3) . ?
C7 C12 1.387(3) . ?
C8 C9 1.393(4) . ?
C9 C10 1.378(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.390(4) . ?
O1 C13 1.366(3) . ?
O2 C24 1.372(3) . ?
O3 C35 1.369(3) . ?
O4 C46 1.370(3) . ?
C13 C18 1.400(3) . ?
C13 C14 1.403(3) . ?
C14 C15 1.399(3) . ?
C14 C56 1.523(3) . ?
C15 C16 1.398(3) . ?
C16 C17 1.392(3) . ?
C16 C19 1.538(3) . ?
C17 C18 1.391(3) . ?
C18 C23 1.520(3) . ?
C19 C22 1.515(4) . ?
C19 C20 1.528(5) . ?
C19 C21 1.535(4) . ?
C23 C25 1.523(3) . ?
C24 C25 1.393(3) . ?
C24 C29 1.402(3) . ?
C25 C26 1.396(3) . ?
C26 C27 1.393(3) . ?
C27 C28 1.402(3) . ?
C27 C30 1.530(3) . ?
C28 C29 1.392(3) . ?
C29 C34 1.523(3) . ?
C30 C33A 1.434(11) . ?
C30 C31 1.500(5) . ?
C30 C31A 1.546(12) . ?
C30 C32 1.550(5) . ?
C30 C33 1.555(6) . ?
C30 C32A 1.582(13) . ?
C34 C36 1.525(3) . ?
C35 C36 1.402(3) . ?
C35 C40 1.407(3) . ?
C36 C37 1.393(3) . ?
C37 C38 1.393(3) . ?
C38 C39 1.399(3) . ?
C38 C41 1.535(3) . ?
C39 C40 1.389(3) . ?
C40 C45 1.527(3) . ?
C41 C43 1.529(3) . ?
C41 C42 1.536(3) . ?
C41 C44 1.536(3) . ?
C45 C47 1.527(3) . ?
C46 C51 1.396(3) . ?
C46 C47 1.401(3) . ?
C47 C48 1.396(3) . ?
C48 C49 1.393(3) . ?
C49 C50 1.398(3) . ?
C49 C52 1.539(3) . ?
C50 C51 1.389(3) . ?
C51 C56 1.526(3) . ?
C52 C55 1.532(4) . ?
C52 C54 1.533(4) . ?
C52 C53 1.540(4) . ?
N3 C57 1.105(3) . ?
C57 C58 1.453(5) . ?
N4 C59 1.126(6) . ?
C59 C60 1.427(6) . ?
N5 C61 1.117(6) . ?
C61 C62 1.429(6) . ?
