#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:23:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178948 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/77/4117774.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_4117774
loop_
_publ_author_name
'Ming Fang'
'Joy H. Farnaby'
'Joseph W. Ziller'
'Jefferson E. Bates'
'Filipp Furche'
'William J. Evans'
_publ_section_title
;
 Isolation of (CO)1- and (CO2)1-Radical Complexes of Rare Earths via
 Ln(NR2)3/K Reduction and [K2(18-crown-6)2]2+ Oligomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6064
_journal_page_last               6067
_journal_paper_doi               10.1021/ja211220r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C78 H188 K2 N6 O18 Si12 Y2'
_chemical_formula_weight         2091.44
_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           SHELXTL
_cell_angle_alpha                94.6026(6)
_cell_angle_beta                 114.8876(6)
_cell_angle_gamma                108.3425(6)
_cell_formula_units_Z            1
_cell_length_a                   14.9104(7)
_cell_length_b                   15.1022(7)
_cell_length_c                   15.5953(8)
_cell_measurement_reflns_used    8457
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.33
_cell_volume                     2930.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31853
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.7959
_exptl_absorpt_correction_T_min  0.6522
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1126
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.817
_refine_diff_density_min         -2.778
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         11922
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0687
_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)+(0.1261P)²+9.0664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2120
_reflns_number_gt                9608
_reflns_number_total             11922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211220r_si_004.cif
_cod_data_source_block           mf68
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4117774
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
Y1 Y -0.29055(3) 0.88229(3) -0.38447(3) 0.01750(14) Uani 1 1 d . . .
Si1 Si -0.50168(11) 0.69468(9) -0.56895(9) 0.0250(3) Uani 1 1 d . . .
Si2 Si -0.28150(12) 0.70700(10) -0.53144(10) 0.0259(3) Uani 1 1 d . . .
Si3 Si -0.02642(10) 1.05350(9) -0.26992(9) 0.0232(3) Uani 1 1 d . . .
Si4 Si -0.17957(10) 1.07438(9) -0.45730(9) 0.0232(3) Uani 1 1 d . . .
Si5 Si -0.28104(10) 0.77095(9) -0.19543(9) 0.0216(3) Uani 1 1 d . . .
Si6 Si -0.34612(12) 0.93990(9) -0.20278(10) 0.0252(3) Uani 1 1 d . . .
O1 O -0.4087(3) 0.9348(2) -0.4435(2) 0.0238(7) Uani 1 1 d . . .
N1 N -0.3645(3) 0.7439(3) -0.5034(3) 0.0220(8) Uani 1 1 d . . .
N2 N -0.1490(3) 1.0102(3) -0.3706(3) 0.0206(8) Uani 1 1 d . . .
N3 N -0.3005(3) 0.8639(3) -0.2444(3) 0.0214(8) Uani 1 1 d . . .
C1 C -0.4728(4) 0.9784(3) -0.4823(3) 0.0222(9) Uani 1 1 d . . .
C2 C -0.5639(4) 0.6924(4) -0.4866(4) 0.0341(12) Uani 1 1 d . . .
H2A H -0.5417 0.7582 -0.4506 0.051 Uiso 1 1 calc R . .
H2B H -0.5404 0.6540 -0.4404 0.051 Uiso 1 1 calc R . .
H2C H -0.6421 0.6637 -0.5256 0.051 Uiso 1 1 calc R . .
C3 C -0.5559(5) 0.7617(4) -0.6604(4) 0.0367(13) Uani 1 1 d . . .
H3A H -0.5346 0.8283 -0.6268 0.055 Uiso 1 1 calc R . .
H3B H -0.6343 0.7307 -0.6957 0.055 Uiso 1 1 calc R . .
H3C H -0.5274 0.7614 -0.7067 0.055 Uiso 1 1 calc R . .
C4 C -0.5577(5) 0.5656(4) -0.6395(4) 0.0385(13) Uani 1 1 d . . .
H4A H -0.5322 0.5623 -0.6878 0.058 Uiso 1 1 calc R . .
H4B H -0.6361 0.5411 -0.6729 0.058 Uiso 1 1 calc R . .
H4C H -0.5337 0.5263 -0.5945 0.058 Uiso 1 1 calc R . .
C5 C -0.2949(5) 0.5800(4) -0.5263(4) 0.0344(12) Uani 1 1 d . . .
H5A H -0.2898 0.5704 -0.4633 0.052 Uiso 1 1 calc R . .
H5B H -0.2375 0.5681 -0.5341 0.052 Uiso 1 1 calc R . .
H5C H -0.3645 0.5353 -0.5790 0.052 Uiso 1 1 calc R . .
C6 C -0.2973(6) 0.7163(4) -0.6561(4) 0.0435(15) Uani 1 1 d . . .
H6A H -0.2879 0.7824 -0.6619 0.065 Uiso 1 1 calc R . .
H6B H -0.3689 0.6720 -0.7058 0.065 Uiso 1 1 calc R . .
H6C H -0.2432 0.6995 -0.6656 0.065 Uiso 1 1 calc R . .
C7 C -0.1385(4) 0.7839(4) -0.4425(4) 0.0357(12) Uani 1 1 d . . .
H7A H -0.1255 0.7791 -0.3763 0.053 Uiso 1 1 calc R . .
H7B H -0.1244 0.8511 -0.4461 0.053 Uiso 1 1 calc R . .
H7C H -0.0910 0.7618 -0.4585 0.053 Uiso 1 1 calc R . .
C8 C -0.0293(4) 0.9828(4) -0.1764(4) 0.0283(11) Uani 1 1 d . . .
H8A H -0.0781 0.9929 -0.1534 0.042 Uiso 1 1 calc R . .
H8B H 0.0429 1.0046 -0.1211 0.042 Uiso 1 1 calc R . .
H8C H -0.0543 0.9142 -0.2058 0.042 Uiso 1 1 calc R . .
C9 C 0.0850(4) 1.0457(4) -0.2937(4) 0.0371(13) Uani 1 1 d . . .
H9A H 0.0951 1.0868 -0.3371 0.056 Uiso 1 1 calc R . .
H9B H 0.0665 0.9789 -0.3245 0.056 Uiso 1 1 calc R . .
H9C H 0.1515 1.0673 -0.2318 0.056 Uiso 1 1 calc R . .
C10 C 0.0180(5) 1.1824(3) -0.2075(4) 0.0331(12) Uani 1 1 d . . .
H10A H -0.0398 1.1912 -0.1979 0.050 Uiso 1 1 calc R . .
H10B H 0.0355 1.2241 -0.2478 0.050 Uiso 1 1 calc R . .
H10C H 0.0815 1.1992 -0.1440 0.050 Uiso 1 1 calc R . .
C11 C -0.2820(4) 0.9913(4) -0.5805(4) 0.0338(12) Uani 1 1 d . . .
H11A H -0.3435 0.9481 -0.5757 0.051 Uiso 1 1 calc R . .
H11B H -0.2501 0.9532 -0.6029 0.051 Uiso 1 1 calc R . .
H11C H -0.3059 1.0293 -0.6270 0.051 Uiso 1 1 calc R . .
C12 C -0.2334(4) 1.1633(4) -0.4300(4) 0.0295(11) Uani 1 1 d . . .
H12A H -0.3042 1.1289 -0.4357 0.044 Uiso 1 1 calc R . .
H12B H -0.2396 1.2039 -0.4765 0.044 Uiso 1 1 calc R . .
H12C H -0.1847 1.2037 -0.3635 0.044 Uiso 1 1 calc R . .
C13 C -0.0614(4) 1.1437(4) -0.4740(4) 0.0346(12) Uani 1 1 d . . .
H13A H -0.0031 1.1869 -0.4115 0.052 Uiso 1 1 calc R . .
H13B H -0.0824 1.1817 -0.5215 0.052 Uiso 1 1 calc R . .
H13C H -0.0371 1.0987 -0.4979 0.052 Uiso 1 1 calc R . .
C14 C -0.2403(4) 0.6989(3) -0.2657(4) 0.0272(10) Uani 1 1 d . . .
H14A H -0.1692 0.7381 -0.2567 0.041 Uiso 1 1 calc R . .
H14B H -0.2924 0.6801 -0.3352 0.041 Uiso 1 1 calc R . .
H14C H -0.2382 0.6411 -0.2419 0.041 Uiso 1 1 calc R . .
C15 C -0.1727(5) 0.8071(4) -0.0654(4) 0.0335(12) Uani 1 1 d . . .
H15A H -0.1083 0.8583 -0.0583 0.050 Uiso 1 1 calc R . .
H15B H -0.1559 0.7513 -0.0477 0.050 Uiso 1 1 calc R . .
H15C H -0.1973 0.8305 -0.0224 0.050 Uiso 1 1 calc R . .
C16 C -0.4052(4) 0.6842(4) -0.1981(4) 0.0287(11) Uani 1 1 d . . .
H16A H -0.4643 0.6622 -0.2649 0.043 Uiso 1 1 calc R . .
H16B H -0.4243 0.7165 -0.1553 0.043 Uiso 1 1 calc R . .
H16C H -0.3916 0.6288 -0.1754 0.043 Uiso 1 1 calc R . .
C17 C -0.2854(5) 1.0651(4) -0.2122(4) 0.0336(12) Uani 1 1 d . . .
H17A H -0.3067 1.0652 -0.2808 0.050 Uiso 1 1 calc R . .
H17B H -0.2072 1.0884 -0.1752 0.050 Uiso 1 1 calc R . .
H17C H -0.3105 1.1074 -0.1854 0.050 Uiso 1 1 calc R . .
C18 C -0.4959(5) 0.9005(4) -0.2696(4) 0.0350(12) Uani 1 1 d . . .
H18A H -0.5184 0.9065 -0.3369 0.053 Uiso 1 1 calc R . .
H18B H -0.5177 0.9411 -0.2368 0.053 Uiso 1 1 calc R . .
H18C H -0.5295 0.8332 -0.2699 0.053 Uiso 1 1 calc R . .
C19 C -0.3104(6) 0.9507(4) -0.0696(4) 0.0446(15) Uani 1 1 d . . .
H19A H -0.2325 0.9727 -0.0302 0.067 Uiso 1 1 calc R . .
H19B H -0.3451 0.8879 -0.0608 0.067 Uiso 1 1 calc R . .
H19C H -0.3351 0.9973 -0.0489 0.067 Uiso 1 1 calc R . .
K1 K 0.20608(9) 0.62888(7) -0.10990(7) 0.0263(2) Uani 1 1 d . A .
O2 O 0.1049(7) 0.7643(6) -0.1430(6) 0.0310(16) Uani 0.50 1 d P A 1
O3 O 0.2198(6) 0.7374(6) -0.2397(5) 0.0336(17) Uani 0.50 1 d P A 1
O4 O 0.2634(6) 0.5667(5) -0.2417(5) 0.0310(16) Uani 0.50 1 d P A 1
O5 O 0.2907(6) 0.4889(5) -0.0766(5) 0.0311(16) Uani 0.50 1 d P A 1
O6 O 0.1842(6) 0.5165(5) 0.0292(6) 0.0311(16) Uani 0.50 1 d P A 1
O7 O 0.1296(7) 0.6814(5) 0.0188(6) 0.0283(15) Uani 0.50 1 d P A 1
C20 C 0.154(4) 0.836(3) -0.179(3) 0.040(7) Uani 0.50 1 d P A 1
H20A H 0.2285 0.8750 -0.1279 0.047 Uiso 0.50 1 calc PR A 1
H20B H 0.1146 0.8787 -0.1964 0.047 Uiso 0.50 1 calc PR A 1
C21 C 0.1559(13) 0.7909(10) -0.2664(10) 0.038(3) Uani 0.50 1 d P A 1
H21A H 0.0821 0.7485 -0.3161 0.045 Uiso 0.50 1 calc PR A 1
H21B H 0.1847 0.8416 -0.2951 0.045 Uiso 0.50 1 calc PR A 1
C22 C 0.225(2) 0.6907(15) -0.318(2) 0.032(4) Uani 0.50 1 d P A 1
H22A H 0.2482 0.7379 -0.3525 0.038 Uiso 0.50 1 calc PR A 1
H22B H 0.1527 0.6421 -0.3653 0.038 Uiso 0.50 1 calc PR A 1
C23 C 0.3017(12) 0.6431(13) -0.2796(12) 0.034(3) Uani 0.50 1 d P A 1
H23A H 0.3141 0.6181 -0.3325 0.040 Uiso 0.50 1 calc PR A 1
H23B H 0.3711 0.6910 -0.2276 0.040 Uiso 0.50 1 calc PR A 1
C24 C 0.3364(13) 0.5223(11) -0.2015(11) 0.033(3) Uani 0.50 1 d P A 1
H24A H 0.4058 0.5708 -0.1501 0.040 Uiso 0.50 1 calc PR A 1
H24B H 0.3488 0.4939 -0.2529 0.040 Uiso 0.50 1 calc PR A 1
C25 C 0.2926(13) 0.4455(10) -0.1591(11) 0.038(3) Uani 0.50 1 d P A 1
H25A H 0.2191 0.4015 -0.2081 0.046 Uiso 0.50 1 calc PR A 1
H25B H 0.3379 0.4074 -0.1399 0.046 Uiso 0.50 1 calc PR A 1
C26 C 0.2597(11) 0.4239(9) -0.0251(10) 0.037(3) Uani 0.50 1 d P A 1
H26A H 0.3090 0.3896 -0.0036 0.044 Uiso 0.50 1 calc PR A 1
H26B H 0.1865 0.3755 -0.0685 0.044 Uiso 0.50 1 calc PR A 1
C27 C 0.2618(12) 0.4758(14) 0.0613(15) 0.030(4) Uani 0.50 1 d P A 1
H27A H 0.2464 0.4306 0.1005 0.035 Uiso 0.50 1 calc PR A 1
H27B H 0.3336 0.5271 0.1028 0.035 Uiso 0.50 1 calc PR A 1
C28 C 0.1828(12) 0.5709(10) 0.1066(10) 0.037(3) Uani 0.50 1 d P A 1
H28A H 0.2537 0.6240 0.1466 0.044 Uiso 0.50 1 calc PR A 1
H28B H 0.1683 0.5293 0.1490 0.044 Uiso 0.50 1 calc PR A 1
C29 C 0.0991(12) 0.6110(11) 0.0676(11) 0.035(3) Uani 0.50 1 d P A 1
H29A H 0.0295 0.5590 0.0214 0.042 Uiso 0.50 1 calc PR A 1
H29B H 0.0913 0.6409 0.1215 0.042 Uiso 0.50 1 calc PR A 1
C30 C 0.0527(15) 0.7220(12) -0.0215(12) 0.028(3) Uani 0.50 1 d P A 1
H30A H 0.0371 0.7469 0.0291 0.034 Uiso 0.50 1 calc PR A 1
H30B H -0.0148 0.6727 -0.0746 0.034 Uiso 0.50 1 calc PR A 1
C31 C 0.0981(13) 0.8036(11) -0.0611(11) 0.032(3) Uani 0.50 1 d P A 1
H31A H 0.0512 0.8402 -0.0807 0.038 Uiso 0.50 1 calc PR A 1
H31B H 0.1702 0.8481 -0.0101 0.038 Uiso 0.50 1 calc PR A 1
O2A O 0.1352(5) 0.7456(5) -0.0408(5) 0.0239(14) Uani 0.50 1 d P A 2
O3A O 0.1573(6) 0.7662(5) -0.2116(5) 0.0268(15) Uani 0.50 1 d P A 2
O4A O 0.2749(7) 0.6743(5) -0.2531(5) 0.0262(15) Uani 0.50 1 d P A 2
O5A O 0.2896(7) 0.5074(6) -0.1819(6) 0.0246(16) Uani 0.50 1 d P A 2
O6A O 0.2766(6) 0.4976(5) -0.0059(5) 0.0243(14) Uani 0.50 1 d P A 2
O7A O 0.1511(5) 0.5837(5) 0.0313(5) 0.0229(14) Uani 0.50 1 d P A 2
C20A C 0.0830(12) 0.7942(11) -0.1081(13) 0.032(3) Uani 0.50 1 d P A 2
H20C H 0.0722 0.8446 -0.0735 0.039 Uiso 0.50 1 calc PR A 2
H20D H 0.0118 0.7478 -0.1590 0.039 Uiso 0.50 1 calc PR A 2
C21A C 0.150(4) 0.839(3) -0.155(3) 0.041(7) Uani 0.50 1 d P A 2
H21C H 0.1180 0.8783 -0.1966 0.050 Uiso 0.50 1 calc PR A 2
H21D H 0.2231 0.8826 -0.1036 0.050 Uiso 0.50 1 calc PR A 2
C22A C 0.2221(12) 0.8059(8) -0.2582(8) 0.033(2) Uani 0.50 1 d P A 2
H22C H 0.2958 0.8478 -0.2079 0.039 Uiso 0.50 1 calc PR A 2
H22D H 0.1912 0.8455 -0.3003 0.039 Uiso 0.50 1 calc PR A 2
C23A C 0.225(3) 0.7244(15) -0.319(2) 0.039(5) Uani 0.50 1 d P A 2
H23C H 0.1510 0.6808 -0.3678 0.047 Uiso 0.50 1 calc PR A 2
H23D H 0.2658 0.7500 -0.3536 0.047 Uiso 0.50 1 calc PR A 2
C24A C 0.2877(12) 0.5992(11) -0.3023(10) 0.027(3) Uani 0.50 1 d P A 2
H24C H 0.3262 0.6254 -0.3389 0.033 Uiso 0.50 1 calc PR A 2
H24D H 0.2167 0.5494 -0.3492 0.033 Uiso 0.50 1 calc PR A 2
C25A C 0.3509(12) 0.5560(11) -0.2270(10) 0.033(3) Uani 0.50 1 d P A 2
H25C H 0.3692 0.5097 -0.2584 0.040 Uiso 0.50 1 calc PR A 2
H25D H 0.4185 0.6074 -0.1766 0.040 Uiso 0.50 1 calc PR A 2
C26A C 0.3488(12) 0.4697(10) -0.1092(11) 0.034(3) Uani 0.50 1 d P A 2
H26C H 0.4171 0.5218 -0.0608 0.041 Uiso 0.50 1 calc PR A 2
H26D H 0.3657 0.4209 -0.1388 0.041 Uiso 0.50 1 calc PR A 2
C27A C 0.2863(10) 0.4248(9) -0.0598(9) 0.030(2) Uani 0.50 1 d P A 2
H27C H 0.2143 0.3782 -0.1090 0.036 Uiso 0.50 1 calc PR A 2
H27D H 0.3231 0.3897 -0.0157 0.036 Uiso 0.50 1 calc PR A 2
C28A C 0.2170(12) 0.4598(13) 0.0435(15) 0.027(4) Uani 0.50 1 d P A 2
H28C H 0.2525 0.4247 0.0886 0.033 Uiso 0.50 1 calc PR A 2
H28D H 0.1440 0.4140 -0.0045 0.033 Uiso 0.50 1 calc PR A 2
C29A C 0.2101(11) 0.5407(10) 0.0996(9) 0.031(3) Uani 0.50 1 d P A 2
H29C H 0.1738 0.5157 0.1382 0.038 Uiso 0.50 1 calc PR A 2
H29D H 0.2829 0.5887 0.1450 0.038 Uiso 0.50 1 calc PR A 2
C30A C 0.1333(12) 0.6563(11) 0.0785(10) 0.030(3) Uani 0.50 1 d P A 2
H30C H 0.2026 0.7061 0.1285 0.036 Uiso 0.50 1 calc PR A 2
H30D H 0.0907 0.6278 0.1109 0.036 Uiso 0.50 1 calc PR A 2
C31A C 0.0733(14) 0.7008(13) 0.0012(14) 0.031(4) Uani 0.50 1 d P A 2
H31C H 0.0055 0.6500 -0.0499 0.037 Uiso 0.50 1 calc PR A 2
H31D H 0.0554 0.7484 0.0311 0.037 Uiso 0.50 1 calc PR A 2
O8 O 0.4130(5) 0.7432(4) 0.0050(4) 0.0856(8) Uiso 1 1 d D A .
C32 C 0.4506(7) 0.8405(5) -0.0068(6) 0.0856(8) Uiso 1 1 d D . .
H32A H 0.3940 0.8664 -0.0208 0.103 Uiso 1 1 calc R A .
H32B H 0.4655 0.8388 -0.0630 0.103 Uiso 1 1 calc R . .
C33 C 0.5502(7) 0.9051(7) 0.0831(6) 0.0856(8) Uiso 1 1 d D A .
H33A H 0.6159 0.9068 0.0805 0.103 Uiso 1 1 calc R . .
H33B H 0.5528 0.9715 0.0955 0.103 Uiso 1 1 calc R . .
C34 C 0.5332(7) 0.8542(6) 0.1558(6) 0.0856(8) Uiso 1 1 d D . .
H34A H 0.5225 0.8956 0.2001 0.103 Uiso 1 1 calc R A .
H34B H 0.5977 0.8414 0.1956 0.103 Uiso 1 1 calc R . .
C35 C 0.4375(7) 0.7608(6) 0.1066(5) 0.0856(8) Uiso 1 1 d D A .
H35A H 0.4544 0.7081 0.1349 0.103 Uiso 1 1 calc R . .
H35B H 0.3763 0.7661 0.1136 0.103 Uiso 1 1 calc R . .
O9 O -0.0083(5) 0.5144(5) -0.2315(5) 0.0856(8) Uiso 1 1 d D A .
C36 C -0.0145(9) 0.4193(5) -0.2666(6) 0.0856(8) Uiso 1 1 d D . .
H36A H -0.0794 0.3686 -0.2724 0.103 Uiso 1 1 calc R A .
H36B H 0.0493 0.4085 -0.2216 0.103 Uiso 1 1 calc R . .
C37 C -0.0192(8) 0.4185(7) -0.3648(6) 0.0856(8) Uiso 1 1 d D A .
H37A H -0.0555 0.3522 -0.4067 0.103 Uiso 1 1 calc R . .
H37B H 0.0536 0.4471 -0.3583 0.103 Uiso 1 1 calc R . .
C38 C -0.0828(8) 0.4789(7) -0.4060(6) 0.0856(8) Uiso 1 1 d D . .
H38A H -0.0494 0.5239 -0.4368 0.103 Uiso 1 1 calc R A .
H38B H -0.1572 0.4377 -0.4553 0.103 Uiso 1 1 calc R . .
C39 C -0.0807(8) 0.5329(7) -0.3196(5) 0.0856(8) Uiso 1 1 d D A .
H39A H -0.0555 0.6027 -0.3160 0.103 Uiso 1 1 calc R . .
H39B H -0.1536 0.5112 -0.3259 0.103 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'
Si Si 0.0817 0.0704 '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'
Y Y -2.7962 3.5667 '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
O1 Y1 N2 99.02(13) .
O1 Y1 N3 98.38(14) .
N2 Y1 N3 116.94(14) .
O1 Y1 N1 98.91(13) .
N2 Y1 N1 120.32(14) .
N3 Y1 N1 115.87(14) .
N1 Si1 C3 112.8(2) .
N1 Si1 C2 111.0(2) .
C3 Si1 C2 107.6(3) .
N1 Si1 C4 113.7(2) .
C3 Si1 C4 106.0(3) .
C2 Si1 C4 105.2(3) .
N1 Si1 Y1 36.79(13) .
C3 Si1 Y1 99.96(18) .
C2 Si1 Y1 83.93(17) .
C4 Si1 Y1 148.02(19) .
N1 Si2 C7 109.8(2) .
N1 Si2 C5 115.2(2) .
C7 Si2 C5 105.4(3) .
N1 Si2 C6 113.5(3) .
C7 Si2 C6 106.4(3) .
C5 Si2 C6 105.9(3) .
N1 Si2 Y1 35.92(13) .
C7 Si2 Y1 74.16(17) .
C5 Si2 Y1 131.25(18) .
C6 Si2 Y1 121.2(2) .
N2 Si3 C10 113.5(2) .
N2 Si3 C8 110.1(2) .
C10 Si3 C8 105.9(2) .
N2 Si3 C9 114.4(2) .
C10 Si3 C9 106.4(3) .
C8 Si3 C9 106.0(2) .
N2 Si4 C12 113.2(2) .
N2 Si4 C11 110.7(2) .
C12 Si4 C11 107.7(2) .
N2 Si4 C13 113.0(2) .
C12 Si4 C13 106.7(2) .
C11 Si4 C13 105.0(3) .
N2 Si4 Y1 37.39(13) .
C12 Si4 Y1 103.28(16) .
C11 Si4 Y1 81.03(17) .
C13 Si4 Y1 145.68(19) .
N3 Si5 C15 114.9(2) .
N3 Si5 C14 110.5(2) .
C15 Si5 C14 105.3(2) .
N3 Si5 C16 112.9(2) .
C15 Si5 C16 106.1(2) .
C14 Si5 C16 106.4(2) .
N3 Si6 C17 111.3(2) .
N3 Si6 C18 113.3(2) .
C17 Si6 C18 108.0(3) .
N3 Si6 C19 112.9(2) .
C17 Si6 C19 105.5(3) .
C18 Si6 C19 105.3(3) .
N3 Si6 Y1 37.52(13) .
C17 Si6 Y1 82.53(17) .
C18 Si6 Y1 102.17(18) .
C19 Si6 Y1 147.1(2) .
C1 O1 Y1 171.3(3) .
Si2 N1 Si1 124.6(2) .
Si2 N1 Y1 118.2(2) .
Si1 N1 Y1 116.5(2) .
Si3 N2 Si4 120.8(2) .
Si3 N2 Y1 122.7(2) .
Si4 N2 Y1 115.47(19) .
Si5 N3 Si6 122.8(2) .
Si5 N3 Y1 121.4(2) .
Si6 N3 Y1 115.26(19) .
C1 C1 O1 176.8(7) 2_474
O8 K1 O2A 93.4(2) .
O8 K1 O7A 98.68(19) .
O2A K1 O7A 62.59(19) .
O8 K1 O3 84.9(2) .
O2A K1 O3 89.4(2) .
O7A K1 O3 151.9(2) .
O8 K1 O4 88.3(2) .
O2A K1 O4 151.8(2) .
O7A K1 O4 144.8(2) .
O3 K1 O4 62.7(2) .
O8 K1 O5 81.1(2) .
O2A K1 O5 145.8(2) .
O7A K1 O5 84.7(2) .
O3 K1 O5 123.3(2) .
O4 K1 O5 62.2(2) .
O8 K1 O9 178.46(19) .
O2A K1 O9 86.11(19) .
O7A K1 O9 82.4(2) .
O3 K1 O9 93.6(2) .
O4 K1 O9 91.5(2) .
O5 K1 O9 100.1(2) .
O8 K1 O3A 94.5(2) .
O2A K1 O3A 62.5(2) .
O7A K1 O3A 124.0(2) .
O3 K1 O3A 28.2(2) .
O4 K1 O3A 89.4(2) .
O5 K1 O3A 151.2(2) .
O9 K1 O3A 84.0(2) .
O8 K1 O6A 80.62(19) .
O2A K1 O6A 120.92(19) .
O7A K1 O6A 60.53(19) .
O3 K1 O6A 146.9(2) .
O4 K1 O6A 87.1(2) .
O5 K1 O6A 24.9(2) .
O9 K1 O6A 100.89(19) .
O3A K1 O6A 174.1(2) .
O8 K1 O2 102.2(2) .
O2A K1 O2 32.0(2) .
O7A K1 O2 91.9(2) .
O3 K1 O2 60.2(2) .
O4 K1 O2 120.4(2) .
O5 K1 O2 175.6(2) .
O9 K1 O2 76.6(2) .
O3A K1 O2 32.1(2) .
O6A K1 O2 152.3(2) .
O8 K1 O7 96.3(2) .
O2A K1 O7 29.1(2) .
O7A K1 O7 33.5(2) .
O3 K1 O7 118.5(2) .
O4 K1 O7 175.4(2) .
O5 K1 O7 117.5(2) .
O9 K1 O7 84.0(2) .
O3A K1 O7 91.2(2) .
O6A K1 O7 92.7(2) .
O2 K1 O7 59.6(2) .
O8 K1 O4A 79.1(2) .
O2A K1 O4A 119.7(2) .
O7A K1 O4A 176.7(2) .
O3 K1 O4A 30.8(2) .
O4 K1 O4A 33.3(2) .
O5 K1 O4A 92.5(2) .
O9 K1 O4A 99.9(2) .
O3A K1 O4A 58.8(2) .
O6A K1 O4A 116.5(2) .
O2 K1 O4A 90.9(2) .
O7 K1 O4A 148.7(2) .
O8 K1 O5A 84.8(2) .
O2A K1 O5A 178.1(2) .
O7A K1 O5A 118.1(2) .
O3 K1 O5A 89.9(2) .
O4 K1 O5A 27.8(2) .
O5 K1 O5A 34.4(2) .
O9 K1 O5A 95.7(2) .
O3A K1 O5A 117.2(2) .
O6A K1 O5A 59.3(2) .
O2 K1 O5A 148.0(2) .
O7 K1 O5A 151.5(3) .
O4A K1 O5A 59.5(2) .
O8 K1 O6 96.2(2) .
O2A K1 O6 88.1(2) .
O7A K1 O6 25.6(2) .
O3 K1 O6 177.3(2) .
O4 K1 O6 119.7(2) .
O5 K1 O6 59.3(2) .
O9 K1 O6 85.2(2) .
O3A K1 O6 149.2(2) .
O6A K1 O6 35.8(2) .
O2 K1 O6 117.2(2) .
O7 K1 O6 59.0(2) .
O4A K1 O6 151.8(2) .
O5A K1 O6 92.6(2) .
C20 O2 C31 112.4(16) .
C20 O2 K1 109.9(19) .
C31 O2 K1 114.1(7) .
C21 O3 C22 113.5(12) .
C21 O3 K1 118.5(8) .
C22 O3 K1 114.0(8) .
C24 O4 C23 112.7(12) .
C24 O4 K1 111.7(8) .
C23 O4 K1 110.2(9) .
C26 O5 C25 114.0(10) .
C26 O5 K1 118.3(8) .
C25 O5 K1 112.9(8) .
C27 O6 C28 113.2(12) .
C27 O6 K1 111.4(10) .
C28 O6 K1 111.4(7) .
C30 O7 C29 111.9(10) .
C30 O7 K1 114.1(9) .
C29 O7 K1 116.3(8) .
O2 C20 C21 110(3) .
O3 C21 C20 109(2) .
O3 C22 C23 108.4(18) .
O4 C23 C22 111.4(13) .
O4 C23 K1 47.5(6) .
C22 C23 K1 80.1(12) .
O4 C24 C25 109.6(15) .
O4 C24 K1 46.4(6) .
C25 C24 K1 79.5(9) .
O5 C25 C24 108.9(11) .
O5 C26 C27 110.4(12) .
O6 C27 C26 109.0(14) .
O6 C28 C29 110.2(11) .
O7 C29 C28 108.7(12) .
O7 C30 C31 107.8(14) .
O2 C31 C30 109.0(12) .
C31A O2A C20A 110.9(10) .
C31A O2A K1 112.9(8) .
C20A O2A K1 115.2(8) .
C21A O3A C22A 111.8(18) .
C21A O3A K1 111.8(16) .
C22A O3A K1 116.5(6) .
C23A O4A C24A 111.2(14) .
C23A O4A K1 117.6(14) .
C24A O4A K1 116.2(7) .
C26A O5A C25A 111.0(10) .
C26A O5A K1 112.2(7) .
C25A O5A K1 112.3(7) .
C27A O6A C28A 112.2(11) .
C27A O6A K1 115.2(6) .
C28A O6A K1 112.3(8) .
C29A O7A C30A 111.2(10) .
C29A O7A K1 118.0(7) .
C30A O7A K1 115.3(7) .
O2A C20A C21A 109.6(19) .
O2A C20A K1 43.4(6) .
C21A C20A K1 79.3(17) .
O3A C21A C20A 109(3) .
O3A C22A C23A 109.2(13) .
O4A C23A C22A 107(2) .
O4A C24A C25A 108.2(11) .
O5A C25A C24A 110.3(11) .
O5A C26A C27A 110.0(10) .
O6A C27A C26A 109.0(10) .
O6A C28A C29A 109.6(13) .
O7A C29A C28A 107.7(11) .
O7A C30A C31A 107.8(11) .
O2A C31A C30A 110.4(13) .
O2A C31A K1 45.5(6) .
C30A C31A K1 81.3(8) .
C35 O8 C32 102.1(7) .
C35 O8 K1 110.8(5) .
C32 O8 K1 118.0(5) .
O8 C32 C33 111.1(7) .
C34 C33 C32 98.8(7) .
C33 C34 C35 111.0(7) .
O8 C35 C34 105.1(7) .
O8 C35 K1 46.3(4) .
C34 C35 K1 144.7(6) .
C36 O9 C39 103.0(7) .
C36 O9 K1 107.6(5) .
C39 O9 K1 126.5(6) .
O9 C36 C37 105.3(7) .
O9 C36 K1 49.1(4) .
C37 C36 K1 104.8(6) .
C36 C37 C38 103.7(7) .
C39 C38 C37 104.6(7) .
O9 C39 C38 108.4(7) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O1 2.052(3) .
Y1 N2 2.284(4) .
Y1 N3 2.285(4) .
Y1 N1 2.286(4) .
Si1 N1 1.715(4) .
Si1 C3 1.868(6) .
Si1 C2 1.871(6) .
Si1 C4 1.889(5) .
Si2 N1 1.699(4) .
Si2 C7 1.874(6) .
Si2 C5 1.876(5) .
Si2 C6 1.880(6) .
Si3 N2 1.703(4) .
Si3 C10 1.876(5) .
Si3 C8 1.883(5) .
Si3 C9 1.883(6) .
Si4 N2 1.716(4) .
Si4 C12 1.873(5) .
Si4 C11 1.880(5) .
Si4 C13 1.881(5) .
Si5 N3 1.697(4) .
Si5 C15 1.879(5) .
Si5 C14 1.881(5) .
Si5 C16 1.883(5) .
Si6 N3 1.715(4) .
Si6 C17 1.869(5) .
Si6 C18 1.879(6) .
Si6 C19 1.893(6) .
O1 C1 1.299(6) .
C1 C1 1.183(9) 2_474
K1 O8 2.685(7) .
K1 O2A 2.686(6) .
K1 O7A 2.720(7) .
K1 O3 2.738(8) .
K1 O4 2.740(7) .
K1 O5 2.763(7) .
K1 O9 2.774(7) .
K1 O3A 2.802(7) .
K1 O6A 2.839(7) .
K1 O2 2.860(9) .
K1 O7 2.864(8) .
K1 O4A 2.871(8) .
K1 O5A 2.909(8) .
K1 O6 2.920(8) .
O2 C20 1.40(4) .
O2 C31 1.420(15) .
O3 C21 1.392(14) .
O3 C22 1.40(3) .
O4 C24 1.407(15) .
O4 C23 1.409(16) .
O5 C26 1.406(14) .
O5 C25 1.410(14) .
O6 C27 1.405(18) .
O6 C28 1.417(15) .
O7 C30 1.409(14) .
O7 C29 1.424(15) .
C20 C21 1.49(3) .
C22 C23 1.49(3) .
C24 C25 1.49(2) .
C26 C27 1.49(3) .
C28 C29 1.48(2) .
C30 C31 1.52(2) .
O2A C31A 1.388(19) .
O2A C20A 1.429(15) .
O3A C21A 1.42(4) .
O3A C22A 1.455(14) .
O4A C23A 1.42(2) .
O4A C24A 1.425(13) .
O5A C26A 1.403(14) .
O5A C25A 1.437(13) .
O6A C27A 1.410(14) .
O6A C28A 1.43(2) .
O7A C29A 1.419(14) .
O7A C30A 1.425(14) .
C20A C21A 1.51(4) .
C22A C23A 1.51(3) .
C24A C25A 1.51(2) .
C26A C27A 1.488(19) .
C28A C29A 1.50(3) .
C30A C31A 1.52(2) .
O8 C35 1.448(4) .
O8 C32 1.455(4) .
C32 C33 1.497(4) .
C33 C34 1.484(4) .
C34 C35 1.500(4) .
O9 C36 1.455(4) .
O9 C39 1.460(4) .
C36 C37 1.502(4) .
C37 C38 1.505(4) .
C38 C39 1.502(4) .
