#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:22:57 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257359 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/70/1557091.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_1557091
loop_
_publ_author_name
'Ryan, Austin J.'
'Ziller, Joseph W.'
'Evans, William J.'
_publ_section_title
;
 The importance of the counter-cation in reductive rare-earth metal
 chemistry: 18-crown-6 instead of 2,2,2-cryptand allows isolation of
 [YII(NR2)3]1− and ynediolate and enediolate complexes from CO
 reactions
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              2006
_journal_page_last               2014
_journal_paper_doi               10.1039/C9SC05794C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C78 H190 K2 N6 O21 Si12 Tm2'
_chemical_formula_weight         2301.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-29 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1418(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.453(3)
_cell_length_b                   18.757(2)
_cell_length_c                   25.744(3)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.26
_cell_volume                     11969(2)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            73762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.125
_diffrn_reflns_theta_min         1.361
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.652
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         15214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0193P)²+19.7209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12794
_reflns_number_total             15214
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc05794c3.cif
_cod_data_source_block           ajr41
_cod_depositor_comments
;Adding full bibliography for 1557089--1557101.cif.

 Adding full bibliography for 1557089--1557101.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1557091
_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   0.710
_shelx_estimated_absorpt_t_max   0.729
_exptl_absorpt_special_details
; 
 Reflections not merged 
   75020 Corrected reflections written to file ajr41s.hkl 
 Estimated minimum and maximum transmission:  0.6513  0.7458 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Tm1 Tm 0.65837(2) 0.16568(2) 0.29756(2) 0.02065(3) Uani 1 1 d . . . . .
K1 K 1.02730(2) 0.20036(2) 0.42669(2) 0.02127(8) Uani 1 1 d . . . . .
Si1 Si 0.62472(3) 0.33931(3) 0.29368(3) 0.03495(15) Uani 1 1 d . . . . .
Si2 Si 0.71921(3) 0.30019(3) 0.38206(3) 0.03671(16) Uani 1 1 d . . . . .
Si3 Si 0.63607(3) 0.09010(3) 0.17668(2) 0.02864(13) Uani 1 1 d . . . . .
Si4 Si 0.73557(2) 0.18185(3) 0.20195(2) 0.02581(12) Uani 1 1 d . . . . .
Si5 Si 0.71891(2) 0.01640(3) 0.36765(2) 0.02727(12) Uani 1 1 d . . . . .
Si6 Si 0.61670(3) 0.07190(3) 0.39142(2) 0.02956(13) Uani 1 1 d . . . . .
N1 N 0.67107(8) 0.27869(9) 0.32662(7) 0.0301(4) Uani 1 1 d . . . . .
N3 N 0.68150(7) 0.14291(9) 0.21970(7) 0.0259(4) Uani 1 1 d . . . . .
N2 N 0.66923(7) 0.07924(8) 0.35988(7) 0.0242(3) Uani 1 1 d . . . . .
O1 O 0.57624(6) 0.16509(7) 0.27258(6) 0.0271(3) Uani 1 1 d . . . . .
O2 O 1.09549(5) 0.09490(7) 0.39376(5) 0.0246(3) Uani 1 1 d . . . . .
O3 O 1.14111(6) 0.20296(8) 0.46398(6) 0.0291(3) Uani 1 1 d . . . . .
O4 O 1.08304(7) 0.33226(8) 0.46276(6) 0.0341(3) Uani 1 1 d . . . . .
O5 O 0.96996(7) 0.33027(7) 0.42789(6) 0.0320(3) Uani 1 1 d . . . . .
O6 O 0.93188(7) 0.22952(8) 0.34877(6) 0.0363(4) Uani 1 1 d . . . . .
O7 O 0.98468(5) 0.09858(7) 0.34790(5) 0.0237(3) Uani 1 1 d . . . . .
O8 O 0.91596(5) -0.03767(7) 0.45508(5) 0.0216(3) Uani 1 1 d . . . . .
O9 O 0.94123(5) 0.15005(7) 0.47368(5) 0.0217(3) Uani 1 1 d . . . . .
O10 O 1.04345(5) 0.18087(7) 0.53589(5) 0.0202(3) Uani 1 1 d . . . . .
C1 C 0.52381(8) 0.16557(10) 0.25714(8) 0.0251(4) Uani 1 1 d . . . . .
C2 C 0.65044(13) 0.43414(12) 0.29661(13) 0.0570(9) Uani 1 1 d . . . . .
H2A H 0.6608 0.4497 0.3339 0.086 Uiso 1 1 calc R U . . .
H2B H 0.6220 0.4654 0.2768 0.086 Uiso 1 1 calc R U . . .
H2C H 0.6819 0.4364 0.2807 0.086 Uiso 1 1 calc R U . . .
C3 C 0.60409(12) 0.31948(13) 0.22042(10) 0.0460(7) Uani 1 1 d . . . . .
H3A H 0.6360 0.3199 0.2052 0.069 Uiso 1 1 calc R U . . .
H3B H 0.5785 0.3558 0.2028 0.069 Uiso 1 1 calc R U . . .
H3C H 0.5870 0.2724 0.2151 0.069 Uiso 1 1 calc R U . . .
C4 C 0.56161(10) 0.34167(11) 0.31990(10) 0.0362(5) Uani 1 1 d . . . . .
H4A H 0.5433 0.2955 0.3136 0.054 Uiso 1 1 calc R U . . .
H4B H 0.5376 0.3791 0.3015 0.054 Uiso 1 1 calc R U . . .
H4C H 0.5710 0.3516 0.3583 0.054 Uiso 1 1 calc R U . . .
C5 C 0.76970(11) 0.36876(13) 0.37172(12) 0.0512(7) Uani 1 1 d . . . . .
H5A H 0.7826 0.3569 0.3397 0.077 Uiso 1 1 calc R U . . .
H5B H 0.8003 0.3693 0.4027 0.077 Uiso 1 1 calc R U . . .
H5C H 0.7526 0.4159 0.3673 0.077 Uiso 1 1 calc R U . . .
C6 C 0.69068(13) 0.33760(16) 0.43780(12) 0.0582(8) Uani 1 1 d . . . . .
H6A H 0.6674 0.3784 0.4246 0.087 Uiso 1 1 calc R U . . .
H6B H 0.7203 0.3530 0.4671 0.087 Uiso 1 1 calc R U . . .
H6C H 0.6695 0.3008 0.4507 0.087 Uiso 1 1 calc R U . . .
C7 C 0.75917(11) 0.21919(14) 0.40897(10) 0.0462(6) Uani 1 1 d . . . . .
H7A H 0.7352 0.1835 0.4189 0.069 Uiso 1 1 calc R U . . .
H7B H 0.7871 0.2323 0.4405 0.069 Uiso 1 1 calc R U . . .
H7C H 0.7762 0.1994 0.3816 0.069 Uiso 1 1 calc R U . . .
C8 C 0.57557(9) 0.14068(12) 0.13961(9) 0.0318(5) Uani 1 1 d . . . . .
H8A H 0.5557 0.1596 0.1650 0.048 Uiso 1 1 calc R U . . .
H8B H 0.5521 0.1087 0.1144 0.048 Uiso 1 1 calc R U . . .
H8C H 0.5873 0.1802 0.1200 0.048 Uiso 1 1 calc R U . . .
C9 C 0.61103(11) 0.01545(12) 0.21344(9) 0.0401(6) Uani 1 1 d . . . . .
H9A H 0.6407 -0.0177 0.2272 0.060 Uiso 1 1 calc R U . . .
H9B H 0.5819 -0.0099 0.1890 0.060 Uiso 1 1 calc R U . . .
H9C H 0.5975 0.0351 0.2432 0.060 Uiso 1 1 calc R U . . .
C10 C 0.66506(11) 0.04515(12) 0.12404(10) 0.0423(6) Uani 1 1 d . . . . .
H10A H 0.6783 0.0814 0.1027 0.063 Uiso 1 1 calc R U . . .
H10B H 0.6370 0.0166 0.1008 0.063 Uiso 1 1 calc R U . . .
H10C H 0.6950 0.0141 0.1412 0.063 Uiso 1 1 calc R U . . .
C11 C 0.79106(10) 0.11810(13) 0.19569(9) 0.0383(6) Uani 1 1 d . . . . .
H11A H 0.8025 0.0910 0.2289 0.057 Uiso 1 1 calc R U . . .
H11B H 0.8218 0.1450 0.1889 0.057 Uiso 1 1 calc R U . . .
H11C H 0.7778 0.0852 0.1661 0.057 Uiso 1 1 calc R U . . .
C12 C 0.71851(9) 0.23267(12) 0.13710(8) 0.0296(5) Uani 1 1 d . . . . .
H12A H 0.7037 0.1998 0.1078 0.044 Uiso 1 1 calc R U . . .
H12B H 0.7512 0.2551 0.1307 0.044 Uiso 1 1 calc R U . . .
H12C H 0.6918 0.2695 0.1391 0.044 Uiso 1 1 calc R U . . .
C13 C 0.76743(9) 0.24997(12) 0.25258(9) 0.0327(5) Uani 1 1 d . . . . .
H13A H 0.7412 0.2875 0.2546 0.049 Uiso 1 1 calc R U . . .
H13B H 0.7987 0.2710 0.2421 0.049 Uiso 1 1 calc R U . . .
H13C H 0.7791 0.2271 0.2875 0.049 Uiso 1 1 calc R U . . .
C14 C 0.76383(9) 0.03448(13) 0.32053(9) 0.0342(5) Uani 1 1 d . . . . .
H14A H 0.7423 0.0343 0.2838 0.051 Uiso 1 1 calc R U . . .
H14B H 0.7916 -0.0026 0.3246 0.051 Uiso 1 1 calc R U . . .
H14C H 0.7811 0.0811 0.3286 0.051 Uiso 1 1 calc R U . . .
C15 C 0.76542(10) 0.01323(14) 0.43607(9) 0.0403(6) Uani 1 1 d . . . . .
H15A H 0.7807 0.0607 0.4456 0.060 Uiso 1 1 calc R U . . .
H15B H 0.7947 -0.0207 0.4360 0.060 Uiso 1 1 calc R U . . .
H15C H 0.7451 -0.0020 0.4622 0.060 Uiso 1 1 calc R U . . .
C16 C 0.69219(11) -0.07692(12) 0.35379(10) 0.0420(6) Uani 1 1 d . . . . .
H16A H 0.6707 -0.0898 0.3795 0.063 Uiso 1 1 calc R U . . .
H16B H 0.7224 -0.1102 0.3570 0.063 Uiso 1 1 calc R U . . .
H16C H 0.6695 -0.0794 0.3176 0.063 Uiso 1 1 calc R U . . .
C17 C 0.63577(12) 0.02955(14) 0.45940(10) 0.0489(7) Uani 1 1 d . . . . .
H17A H 0.6471 -0.0198 0.4559 0.073 Uiso 1 1 calc R U . . .
H17B H 0.6046 0.0301 0.4758 0.073 Uiso 1 1 calc R U . . .
H17C H 0.6655 0.0563 0.4818 0.073 Uiso 1 1 calc R U . . .
C18 C 0.55846(10) 0.01908(12) 0.35234(11) 0.0407(6) Uani 1 1 d . . . . .
H18A H 0.5461 0.0403 0.3169 0.061 Uiso 1 1 calc R U . . .
H18B H 0.5289 0.0195 0.3710 0.061 Uiso 1 1 calc R U . . .
H18C H 0.5699 -0.0302 0.3487 0.061 Uiso 1 1 calc R U . . .
C19 C 0.58988(10) 0.16202(11) 0.40411(10) 0.0350(5) Uani 1 1 d . . . . .
H19A H 0.6194 0.1915 0.4242 0.052 Uiso 1 1 calc R U . . .
H19B H 0.5622 0.1565 0.4248 0.052 Uiso 1 1 calc R U . . .
H19C H 0.5740 0.1851 0.3700 0.052 Uiso 1 1 calc R U . . .
C20 C 1.01984(8) 0.04780(11) 0.33264(8) 0.0270(4) Uani 1 1 d . . . . .
H20A H 1.0350 0.0672 0.3034 0.032 Uiso 1 1 calc R U . . .
H20B H 0.9998 0.0036 0.3199 0.032 Uiso 1 1 calc R U . . .
C21 C 1.06438(8) 0.03192(10) 0.38023(8) 0.0256(4) Uani 1 1 d . . . . .
H21A H 1.0491 0.0167 0.4106 0.031 Uiso 1 1 calc R U . . .
H21B H 1.0874 -0.0070 0.3718 0.031 Uiso 1 1 calc R U . . .
C22 C 1.14274(8) 0.08318(12) 0.43456(9) 0.0292(4) Uani 1 1 d . . . . .
H22A H 1.1653 0.0459 0.4234 0.035 Uiso 1 1 calc R U . . .
H22B H 1.1328 0.0672 0.4677 0.035 Uiso 1 1 calc R U . . .
C23 C 1.17327(9) 0.15206(13) 0.44420(9) 0.0349(5) Uani 1 1 d . . . . .
H23A H 1.2079 0.1448 0.4705 0.042 Uiso 1 1 calc R U . . .
H23B H 1.1813 0.1695 0.4105 0.042 Uiso 1 1 calc R U . . .
C24 C 1.16664(10) 0.27102(13) 0.47346(10) 0.0374(5) Uani 1 1 d . . . . .
H24A H 1.1707 0.2920 0.4393 0.045 Uiso 1 1 calc R U . . .
H24B H 1.2030 0.2657 0.4971 0.045 Uiso 1 1 calc R U . . .
C25 C 1.13288(10) 0.31874(12) 0.49905(10) 0.0386(5) Uani 1 1 d . . . . .
H25A H 1.1263 0.2958 0.5316 0.046 Uiso 1 1 calc R U . . .
H25B H 1.1521 0.3642 0.5095 0.046 Uiso 1 1 calc R U . . .
C26 C 1.04850(11) 0.37314(12) 0.48784(10) 0.0418(6) Uani 1 1 d . . . . .
H26A H 1.0675 0.4165 0.5042 0.050 Uiso 1 1 calc R U . . .
H26B H 1.0381 0.3447 0.5163 0.050 Uiso 1 1 calc R U . . .
C27 C 0.99940(11) 0.39349(12) 0.44655(11) 0.0444(6) Uani 1 1 d . . . . .
H27A H 0.9766 0.4263 0.4621 0.053 Uiso 1 1 calc R U . . .
H27B H 1.0100 0.4182 0.4165 0.053 Uiso 1 1 calc R U . . .
C28 C 0.92546(13) 0.34439(14) 0.38507(11) 0.0592(9) Uani 1 1 d . . . . .
H28A H 0.9381 0.3653 0.3548 0.071 Uiso 1 1 calc R U . . .
H28B H 0.9008 0.3789 0.3964 0.071 Uiso 1 1 calc R U . . .
C29 C 0.89656(11) 0.27620(15) 0.36846(11) 0.0553(8) Uani 1 1 d . . . . .
H29A H 0.8856 0.2540 0.3993 0.066 Uiso 1 1 calc R U . . .
H29B H 0.8637 0.2854 0.3403 0.066 Uiso 1 1 calc R U . . .
C30 C 0.90453(9) 0.16738(13) 0.32487(9) 0.0367(5) Uani 1 1 d . . . . .
H30A H 0.8739 0.1810 0.2954 0.044 Uiso 1 1 calc R U . . .
H30B H 0.8902 0.1403 0.3516 0.044 Uiso 1 1 calc R U . . .
C31 C 0.94378(9) 0.12220(12) 0.30384(8) 0.0321(5) Uani 1 1 d . . . . .
H31A H 0.9249 0.0807 0.2843 0.038 Uiso 1 1 calc R U . . .
H31B H 0.9601 0.1503 0.2790 0.038 Uiso 1 1 calc R U . . .
C32 C 0.90713(8) -0.08332(10) 0.40977(7) 0.0236(4) Uani 1 1 d . . . . .
H32A H 0.9357 -0.0758 0.3899 0.028 Uiso 1 1 calc R U . . .
H32B H 0.8719 -0.0722 0.3856 0.028 Uiso 1 1 calc R U . . .
C33 C 0.91639(8) 0.03523(10) 0.43978(8) 0.0231(4) Uani 1 1 d . . . . .
H33A H 0.8800 0.0499 0.4200 0.028 Uiso 1 1 calc R U . . .
H33B H 0.9419 0.0423 0.4164 0.028 Uiso 1 1 calc R U . . .
C34 C 0.93360(8) 0.07882(10) 0.48978(8) 0.0218(4) Uani 1 1 d . . . . .
H34A H 0.9055 0.0774 0.5108 0.026 Uiso 1 1 calc R U . . .
H34B H 0.9676 0.0598 0.5121 0.026 Uiso 1 1 calc R U . . .
C35 C 0.94889(8) 0.20019(10) 0.51684(8) 0.0234(4) Uani 1 1 d . . . . .
H35A H 0.9168 0.1992 0.5325 0.028 Uiso 1 1 calc R U . . .
H35B H 0.9517 0.2487 0.5026 0.028 Uiso 1 1 calc R U . . .
C36 C 0.99841(8) 0.18550(10) 0.56008(8) 0.0220(4) Uani 1 1 d . . . . .
H36A H 1.0041 0.2244 0.5868 0.026 Uiso 1 1 calc R U . . .
H36B H 0.9941 0.1402 0.5784 0.026 Uiso 1 1 calc R U . . .
C37 C 1.09229(8) 0.15994(10) 0.57201(8) 0.0221(4) Uani 1 1 d . . . . .
H37A H 1.0982 0.1913 0.6037 0.026 Uiso 1 1 calc R U . . .
H37B H 1.1227 0.1673 0.5545 0.026 Uiso 1 1 calc R U . . .
O11 O 1.0000 0.27621(12) 0.2500 0.0462(6) Uani 1 2 d S T P . .
C44 C 1.0287(3) 0.3110(3) 0.2936(3) 0.0586(15) Uiso 0.5 1 d . . P A 1
H44A H 1.0071 0.3137 0.3211 0.070 Uiso 0.5 1 calc R U P A 1
H44B H 1.0363 0.3603 0.2836 0.070 Uiso 0.5 1 calc R U P A 1
C45 C 1.0554(2) 0.3094(3) 0.2707(2) 0.0534(14) Uiso 0.5 1 d . . P A 2
H45A H 1.0768 0.3062 0.2432 0.064 Uiso 0.5 1 calc R U P A 2
H45B H 1.0515 0.3604 0.2791 0.064 Uiso 0.5 1 calc R U P A 2
C46 C 1.08158(14) 0.2729(2) 0.31658(14) 0.0731(9) Uiso 1 1 d . . . . .
H46A H 1.0741 0.2243 0.3269 0.110 Uiso 0.5 1 calc R U P A 1
H46B H 1.1015 0.2988 0.3480 0.110 Uiso 0.5 1 calc R U P A 1
H46C H 1.1032 0.2709 0.2896 0.110 Uiso 0.5 1 calc R U P A 1
H46D H 1.0621 0.2803 0.3449 0.110 Uiso 0.5 1 calc R U P A 2
H46E H 1.1185 0.2908 0.3284 0.110 Uiso 0.5 1 calc R U P A 2
H46F H 1.0825 0.2218 0.3087 0.110 Uiso 0.5 1 calc R U P A 2
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'
Tm Tm -0.3139 5.2483 '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
O1 Tm1 N1 99.76(6) . .
O1 Tm1 N2 99.86(6) . .
N1 Tm1 N2 117.18(6) . .
O1 Tm1 N3 100.05(6) . .
N1 Tm1 N3 115.33(6) . .
N2 Tm1 N3 118.82(6) . .
O1 Tm1 Si3 76.11(4) . .
N1 Tm1 Si3 133.63(5) . .
N2 Tm1 Si3 108.93(4) . .
N3 Tm1 Si3 27.99(5) . .
O1 Tm1 Si6 75.82(4) . .
N1 Tm1 Si6 107.49(4) . .
N2 Tm1 Si6 27.91(4) . .
N3 Tm1 Si6 136.99(4) . .
Si3 Tm1 Si6 115.686(17) . .
O1 Tm1 Si1 76.14(4) . .
N1 Tm1 Si1 27.46(5) . .
N2 Tm1 Si1 135.00(4) . .
N3 Tm1 Si1 105.86(4) . .
Si3 Tm1 Si1 113.211(16) . .
Si6 Tm1 Si1 114.179(14) . .
O10 K1 O7 125.81(4) . .
O10 K1 O6 130.55(4) . .
O7 K1 O6 59.51(4) . .
O10 K1 O3 75.79(4) . .
O7 K1 O3 116.85(4) . .
O6 K1 O3 151.92(5) . .
O10 K1 O5 93.45(4) . .
O7 K1 O5 118.29(4) . .
O6 K1 O5 58.82(4) . .
O3 K1 O5 117.94(5) . .
O10 K1 O2 104.32(4) . .
O7 K1 O2 58.83(4) . .
O6 K1 O2 113.66(4) . .
O3 K1 O2 58.31(4) . .
O5 K1 O2 159.34(4) . .
O10 K1 O9 58.95(4) . .
O7 K1 O9 82.86(4) . .
O6 K1 O9 75.51(5) . .
O3 K1 O9 132.57(4) . .
O5 K1 O9 80.54(4) . .
O2 K1 O9 117.59(4) . .
O10 K1 O4 80.72(4) . .
O7 K1 O4 152.83(4) . .
O6 K1 O4 109.94(5) . .
O3 K1 O4 59.28(5) . .
O5 K1 O4 58.68(5) . .
O2 K1 O4 113.35(4) . .
O9 K1 O4 120.46(4) . .
O10 K1 C35 43.90(4) . .
O7 K1 C35 107.60(5) . .
O6 K1 C35 86.64(5) . .
O3 K1 C35 118.91(5) . .
O5 K1 C35 67.03(4) . .
O2 K1 C35 133.52(4) . .
O9 K1 C35 24.84(4) . .
O4 K1 C35 95.92(4) . .
N1 Si1 C3 111.64(10) . .
N1 Si1 C4 112.70(9) . .
C3 Si1 C4 107.40(12) . .
N1 Si1 C2 114.22(12) . .
C3 Si1 C2 103.99(13) . .
C4 Si1 C2 106.26(10) . .
N1 Si1 Tm1 37.10(6) . .
C3 Si1 Tm1 81.32(7) . .
C4 Si1 Tm1 104.18(7) . .
C2 Si1 Tm1 145.70(9) . .
N1 Si2 C7 110.16(10) . .
N1 Si2 C5 115.32(12) . .
C7 Si2 C5 106.04(13) . .
N1 Si2 C6 113.43(12) . .
C7 Si2 C6 106.95(14) . .
C5 Si2 C6 104.32(12) . .
N3 Si3 C8 112.97(9) . .
N3 Si3 C9 111.08(10) . .
C8 Si3 C9 107.44(11) . .
N3 Si3 C10 113.88(11) . .
C8 Si3 C10 105.74(11) . .
C9 Si3 C10 105.18(11) . .
N3 Si3 Tm1 37.93(5) . .
C8 Si3 Tm1 101.82(7) . .
C9 Si3 Tm1 81.53(8) . .
C10 Si3 Tm1 147.88(9) . .
N3 Si4 C13 110.68(9) . .
N3 Si4 C11 114.60(10) . .
C13 Si4 C11 106.13(11) . .
N3 Si4 C12 114.54(9) . .
C13 Si4 C12 104.32(10) . .
C11 Si4 C12 105.73(10) . .
N2 Si5 C14 110.08(9) . .
N2 Si5 C16 113.19(10) . .
C14 Si5 C16 107.00(11) . .
N2 Si5 C15 114.97(10) . .
C14 Si5 C15 105.30(11) . .
C16 Si5 C15 105.70(11) . .
N2 Si6 C18 113.18(10) . .
N2 Si6 C19 111.23(9) . .
C18 Si6 C19 107.13(11) . .
N2 Si6 C17 114.13(10) . .
C18 Si6 C17 106.34(12) . .
C19 Si6 C17 104.18(11) . .
N2 Si6 Tm1 37.82(5) . .
C18 Si6 Tm1 103.41(8) . .
C19 Si6 Tm1 80.80(7) . .
C17 Si6 Tm1 146.63(9) . .
Si2 N1 Si1 122.63(10) . .
Si2 N1 Tm1 121.57(10) . .
Si1 N1 Tm1 115.44(10) . .
Si4 N3 Si3 122.54(10) . .
Si4 N3 Tm1 123.06(10) . .
Si3 N3 Tm1 114.08(9) . .
Si5 N2 Si6 121.60(9) . .
Si5 N2 Tm1 123.23(8) . .
Si6 N2 Tm1 114.27(8) . .
C1 O1 Tm1 179.09(15) . .
C21 O2 C22 112.53(15) . .
C21 O2 K1 107.65(10) . .
C22 O2 K1 110.69(11) . .
C23 O3 C24 112.58(16) . .
C23 O3 K1 119.53(12) . .
C24 O3 K1 117.59(13) . .
C25 O4 C26 110.44(18) . .
C25 O4 K1 110.99(12) . .
C26 O4 K1 107.25(12) . .
C28 O5 C27 111.91(19) . .
C28 O5 K1 118.29(13) . .
C27 O5 K1 118.97(14) . .
C30 O6 C29 111.72(19) . .
C30 O6 K1 113.87(11) . .
C29 O6 K1 112.02(13) . .
C20 O7 C31 112.35(15) . .
C20 O7 K1 119.30(11) . .
C31 O7 K1 117.04(11) . .
C32 O8 C33 111.16(14) . .
C34 O9 C35 113.12(14) . .
C34 O9 K1 126.45(11) . .
C35 O9 K1 97.33(10) . .
C36 O10 C37 113.55(14) . .
C36 O10 K1 119.10(11) . .
C37 O10 K1 127.11(10) . .
C1 C1 O1 179.5(2) 2_655 .
O7 C20 C21 108.30(15) . .
O2 C21 C20 108.14(16) . .
O2 C22 C23 107.96(18) . .
O3 C23 C22 108.56(16) . .
O3 C24 C25 109.02(18) . .
O4 C25 C24 109.57(19) . .
O4 C26 C27 108.49(19) . .
O5 C27 C26 108.52(18) . .
O5 C28 C29 108.6(2) . .
O6 C29 C28 108.6(2) . .
O6 C30 C31 108.53(19) . .
O7 C31 C30 108.31(16) . .
O8 C32 C37 109.24(15) . 5_756
O8 C33 C34 107.72(15) . .
O9 C34 C33 107.05(15) . .
O9 C35 C36 113.34(15) . .
O9 C35 K1 57.83(8) . .
C36 C35 K1 88.97(11) . .
O10 C36 C35 108.02(15) . .
O10 C37 C32 114.17(15) . 5_756
C44 O11 C44 122.6(6) 2_755 .
C45 O11 C45 131.7(5) . 2_755
O11 C44 C46 111.0(5) . .
C46 C45 O11 108.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 O1 2.0428(14) .
Tm1 N1 2.2465(17) .
Tm1 N2 2.2533(16) .
Tm1 N3 2.2548(16) .
Tm1 Si3 3.3487(7) .
Tm1 Si6 3.3502(6) .
Tm1 Si1 3.3632(7) .
K1 O10 2.7714(13) .
K1 O7 2.8168(14) .
K1 O6 2.8296(15) .
K1 O3 2.8375(15) .
K1 O5 2.8441(15) .
K1 O2 2.8833(14) .
K1 O9 2.8911(14) .
K1 O4 2.8979(15) .
K1 C35 3.388(2) .
Si1 N1 1.717(2) .
Si1 C3 1.876(3) .
Si1 C4 1.879(2) .
Si1 C2 1.891(2) .
Si2 N1 1.705(2) .
Si2 C7 1.871(3) .
Si2 C5 1.879(2) .
Si2 C6 1.885(2) .
Si3 N3 1.721(2) .
Si3 C8 1.875(2) .
Si3 C9 1.881(2) .
Si3 C10 1.883(2) .
Si4 N3 1.7092(18) .
Si4 C13 1.873(2) .
Si4 C11 1.885(2) .
Si4 C12 1.886(2) .
Si5 N2 1.7069(17) .
Si5 C14 1.877(2) .
Si5 C16 1.882(2) .
Si5 C15 1.887(2) .
Si6 N2 1.7203(17) .
Si6 C18 1.874(3) .
Si6 C19 1.879(2) .
Si6 C17 1.882(2) .
O1 C1 1.303(2) .
O2 C21 1.421(2) .
O2 C22 1.422(2) .
O3 C23 1.425(3) .
O3 C24 1.428(3) .
O4 C25 1.417(3) .
O4 C26 1.427(3) .
O5 C28 1.414(3) .
O5 C27 1.426(3) .
O6 C30 1.424(3) .
O6 C29 1.428(3) .
O7 C20 1.422(2) .
O7 C31 1.425(2) .
O8 C32 1.423(2) .
O8 C33 1.424(2) .
O9 C34 1.425(2) .
O9 C35 1.435(2) .
O10 C36 1.426(2) .
O10 C37 1.428(2) .
C1 C1 1.184(4) 2_655
C20 C21 1.498(3) .
C22 C23 1.499(3) .
C24 C25 1.494(3) .
C26 C27 1.494(4) .
C28 C29 1.489(4) .
C30 C31 1.502(3) .
C32 C37 1.511(3) 5_756
C33 C34 1.504(3) .
C35 C36 1.505(3) .
C37 C32 1.511(3) 5_756
O11 C44 1.359(6) 2_755
O11 C44 1.359(6) .
O11 C45 1.523(6) .
O11 C45 1.523(6) 2_755
C44 C46 1.520(7) .
C45 C46 1.396(7) .
