#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:21:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179106 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/68/4306894.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_4306894
loop_
_publ_author_name
'Luca Maretti'
'Marilena Ferbinteanu'
'Fanica Cimpoesu'
'Saiful S. M. Islam'
'Yasunori Ohba'
'Takashi Kajiwara'
'Masahiro Yamashita'
'Seigo Yamauchi'
_publ_contact_author_address
; Department of Chemistry, Graduate School of Science,
  Tohoku University, Sendai 980-8578, JAPAN
;
_publ_contact_author_email       marilena@agnus.chem.tohoku.ac.jp
_publ_contact_author_fax         81-22-795-6547
_publ_contact_author_name        'Marilena Ferbinteanu'
_publ_contact_author_phone       81-22-795-6546
_publ_section_title
;
Spin Coupling in the Supramolecular Structure of a New
Tetra(Quinoline-TEMPO)Yttrium(III) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              660
_journal_page_last               669
_journal_paper_doi               10.1021/ic0610841
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C86 H107 K N11 O16.25 Y'
_chemical_formula_weight         1682.84
_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                111.181(3)
_cell_angle_beta                 106.205(4)
_cell_angle_gamma                92.444(3)
_cell_formula_units_Z            2
_cell_length_a                   15.3236(16)
_cell_length_b                   15.4411(17)
_cell_length_c                   21.331(3)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.43
_cell_volume                     4460.8(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.1900
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44485
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.92805
_exptl_absorpt_correction_T_min  0.74570
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         20332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          26.360
_refine_ls_shift/su_mean         0.287
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                8735
_reflns_number_total             20332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0610841si20060615_094115.cif
_cod_data_source_block           qt4yk
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4460.9(9)
_cod_database_code               4306894
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
Y Y 0.74352(3) 0.00447(3) 0.24918(2) 0.02529(12) Uani 1 1 d . . .
K K 0.19593(7) -0.43041(6) 0.23374(5) 0.0389(3) Uani 1 1 d . . .
O1 O 0.72101(18) 0.01867(19) 0.14565(14) 0.0336(7) Uani 1 1 d . . .
O2 O 0.59062(18) -0.06549(18) 0.17227(14) 0.0306(6) Uani 1 1 d . . .
O3 O 0.46313(19) -0.1385(2) 0.08433(14) 0.0380(7) Uani 1 1 d . . .
O4 O 0.2538(2) -0.2980(2) 0.19538(18) 0.0501(9) Uani 1 1 d . . .
N1 N 0.6538(2) -0.0204(2) -0.03626(17) 0.0331(8) Uani 1 1 d . . .
N2 N 0.3041(2) -0.2601(2) 0.17037(19) 0.0359(9) Uani 1 1 d . . .
C1 C 0.7832(3) 0.0824(3) 0.0607(2) 0.0421(12) Uani 1 1 d . . .
H1 H 0.7926 0.1000 0.0230 0.063 Uiso 1 1 calc R . .
H2 H 0.8360 0.0552 0.0794 0.063 Uiso 1 1 calc R . .
H3 H 0.7771 0.1384 0.0989 0.063 Uiso 1 1 calc R . .
C2 C 0.6975(3) 0.0116(3) 0.0315(2) 0.0293(9) Uani 1 1 d . . .
C3 C 0.5733(3) -0.0840(3) -0.0630(2) 0.0317(10) Uani 1 1 d . . .
C4 C 0.5315(3) -0.1181(3) -0.1361(2) 0.0409(11) Uani 1 1 d . . .
H4 H 0.5592 -0.0971 -0.1639 0.049 Uiso 1 1 calc R . .
C5 C 0.4512(3) -0.1813(3) -0.1688(2) 0.0481(13) Uani 1 1 d . . .
H5 H 0.4237 -0.2046 -0.2188 0.058 Uiso 1 1 calc R . .
C6 C 0.4114(3) -0.2102(3) -0.1281(2) 0.0440(12) Uani 1 1 d . . .
H6 H 0.3556 -0.2538 -0.1505 0.053 Uiso 1 1 calc R . .
C7 C 0.4503(3) -0.1778(3) -0.0556(2) 0.0387(11) Uani 1 1 d . . .
H7 H 0.4206 -0.1992 -0.0290 0.046 Uiso 1 1 calc R . .
C8 C 0.5337(3) -0.1129(3) -0.0197(2) 0.0275(9) Uani 1 1 d . . .
C9 C 0.5825(3) -0.0760(3) 0.0561(2) 0.0264(9) Uani 1 1 d . . .
C10 C 0.6677(3) -0.0155(3) 0.0817(2) 0.0284(9) Uani 1 1 d . . .
C11 C 0.5486(3) -0.0918(3) 0.1089(2) 0.0252(9) Uani 1 1 d . . .
C12 C 0.1663(3) -0.2202(3) 0.1036(3) 0.0586(15) Uani 1 1 d . . .
H8 H 0.1611 -0.2802 0.0645 0.088 Uiso 1 1 calc R . .
H9 H 0.1418 -0.1741 0.0845 0.088 Uiso 1 1 calc R . .
H10 H 0.1311 -0.2292 0.1333 0.088 Uiso 1 1 calc R . .
C13 C 0.2747(4) -0.0970(3) 0.2141(3) 0.0621(15) Uani 1 1 d . . .
H11 H 0.2510 -0.1154 0.2464 0.093 Uiso 1 1 calc R . .
H12 H 0.2384 -0.0524 0.2002 0.093 Uiso 1 1 calc R . .
H13 H 0.3392 -0.0673 0.2380 0.093 Uiso 1 1 calc R . .
C14 C 0.2674(3) -0.1843(3) 0.1481(3) 0.0407(11) Uani 1 1 d . . .
C15 C 0.3207(3) -0.1639(3) 0.1027(2) 0.0410(11) Uani 1 1 d . . .
H14 H 0.3004 -0.2155 0.0551 0.049 Uiso 1 1 calc R . .
H15 H 0.3059 -0.1050 0.0967 0.049 Uiso 1 1 calc R . .
C16 C 0.4234(3) -0.1544(3) 0.1342(2) 0.0343(10) Uani 1 1 d . . .
H16 H 0.4461 -0.1000 0.1811 0.041 Uiso 1 1 calc R . .
C17 C 0.4475(3) -0.2446(3) 0.1424(2) 0.0381(11) Uani 1 1 d . . .
H17 H 0.5152 -0.2380 0.1618 0.046 Uiso 1 1 calc R . .
H18 H 0.4273 -0.2966 0.0950 0.046 Uiso 1 1 calc R . .
C18 C 0.4039(3) -0.2701(3) 0.1903(2) 0.0350(10) Uani 1 1 d . . .
C19 C 0.4502(3) -0.2088(4) 0.2683(2) 0.0538(14) Uani 1 1 d . . .
H19 H 0.4589 -0.1426 0.2744 0.081 Uiso 1 1 calc R . .
H20 H 0.5102 -0.2269 0.2849 0.081 Uiso 1 1 calc R . .
H21 H 0.4114 -0.2173 0.2958 0.081 Uiso 1 1 calc R . .
C20 C 0.4085(3) -0.3737(3) 0.1780(3) 0.0577(15) Uani 1 1 d . . .
H22 H 0.3820 -0.3902 0.2098 0.087 Uiso 1 1 calc R . .
H23 H 0.4728 -0.3837 0.1876 0.087 Uiso 1 1 calc R . .
H24 H 0.3735 -0.4134 0.1287 0.087 Uiso 1 1 calc R . .
O5 O 0.7333(2) -0.08580(18) 0.30932(14) 0.0364(7) Uani 1 1 d . . .
O6 O 0.73759(19) -0.16324(18) 0.17650(14) 0.0339(7) Uani 1 1 d . . .
O7 O 0.7465(2) -0.31600(18) 0.13822(14) 0.0406(8) Uani 1 1 d . . .
O8 O 0.7717(2) -0.4314(2) -0.12866(15) 0.0501(9) Uani 1 1 d . . .
N3 N 0.6821(3) -0.2668(3) 0.36519(19) 0.0418(9) Uani 1 1 d . . .
N4 N 0.7672(2) -0.4000(2) -0.06533(18) 0.0337(8) Uani 1 1 d . . .
C21 C 0.7187(4) -0.0985(3) 0.4303(2) 0.0531(14) Uani 1 1 d . . .
H25 H 0.6738 -0.0577 0.4209 0.080 Uiso 1 1 calc R . .
H26 H 0.7811 -0.0646 0.4451 0.080 Uiso 1 1 calc R . .
H27 H 0.7109 -0.1169 0.4681 0.080 Uiso 1 1 calc R . .
C22 C 0.7035(3) -0.1849(3) 0.3642(2) 0.0358(10) Uani 1 1 d . . .
C23 C 0.6666(3) -0.3463(3) 0.3038(2) 0.0362(10) Uani 1 1 d . . .
C24 C 0.6387(3) -0.4324(3) 0.3065(3) 0.0486(13) Uani 1 1 d . . .
H28 H 0.6354 -0.4335 0.3501 0.058 Uiso 1 1 calc R . .
C25 C 0.6163(3) -0.5145(3) 0.2482(3) 0.0512(13) Uani 1 1 d . . .
H29 H 0.5963 -0.5719 0.2506 0.061 Uiso 1 1 calc R . .
C26 C 0.6232(3) -0.5129(3) 0.1855(3) 0.0431(12) Uani 1 1 d . . .
H30 H 0.6076 -0.5698 0.1446 0.052 Uiso 1 1 calc R . .
C27 C 0.6521(3) -0.4302(3) 0.1815(2) 0.0358(10) Uani 1 1 d . . .
H31 H 0.6562 -0.4312 0.1376 0.043 Uiso 1 1 calc R . .
C28 C 0.6762(3) -0.3432(3) 0.2411(2) 0.0309(10) Uani 1 1 d . . .
C29 C 0.7045(3) -0.2525(3) 0.2414(2) 0.0303(10) Uani 1 1 d . . .
C30 C 0.7139(3) -0.1708(3) 0.3027(2) 0.0292(9) Uani 1 1 d . . .
C31 C 0.7283(3) -0.2375(3) 0.1840(2) 0.0292(10) Uani 1 1 d . . .
C32 C 0.8679(3) -0.5092(3) -0.0391(2) 0.0524(14) Uani 1 1 d . . .
H32 H 0.8109 -0.5541 -0.0568 0.079 Uiso 1 1 calc R . .
H33 H 0.9126 -0.5205 -0.0010 0.079 Uiso 1 1 calc R . .
H34 H 0.8935 -0.5172 -0.0777 0.079 Uiso 1 1 calc R . .
C33 C 0.9315(3) -0.3377(3) 0.0050(3) 0.0603(15) Uani 1 1 d . . .
H35 H 0.9403 -0.3423 -0.0398 0.090 Uiso 1 1 calc R . .
H36 H 0.9862 -0.3518 0.0342 0.090 Uiso 1 1 calc R . .
H37 H 0.9217 -0.2738 0.0304 0.090 Uiso 1 1 calc R . .
C34 C 0.8471(3) -0.4085(3) -0.0103(2) 0.0360(10) Uani 1 1 d . . .
C35 C 0.8197(3) -0.3942(3) 0.0559(2) 0.0406(11) Uani 1 1 d . . .
H38 H 0.7782 -0.4514 0.0468 0.049 Uiso 1 1 calc R . .
H39 H 0.8757 -0.3874 0.0953 0.049 Uiso 1 1 calc R . .
C36 C 0.7720(3) -0.3098(3) 0.0792(2) 0.0347(10) Uani 1 1 d . . .
H40 H 0.8143 -0.2497 0.0943 0.042 Uiso 1 1 calc R . .
C37 C 0.6863(3) -0.3197(3) 0.0185(2) 0.0358(10) Uani 1 1 d . . .
H41 H 0.6435 -0.3766 0.0082 0.043 Uiso 1 1 calc R . .
H42 H 0.6549 -0.2647 0.0337 0.043 Uiso 1 1 calc R . .
C38 C 0.7057(3) -0.3270(3) -0.0486(2) 0.0350(10) Uani 1 1 d . . .
C39 C 0.7530(3) -0.2331(3) -0.0427(2) 0.0483(13) Uani 1 1 d . . .
H43 H 0.8054 -0.2069 0.0010 0.072 Uiso 1 1 calc R . .
H44 H 0.7090 -0.1888 -0.0417 0.072 Uiso 1 1 calc R . .
H45 H 0.7747 -0.2439 -0.0835 0.072 Uiso 1 1 calc R . .
C40 C 0.6160(3) -0.3608(3) -0.1105(2) 0.0521(13) Uani 1 1 d . . .
H46 H 0.6286 -0.3632 -0.1536 0.078 Uiso 1 1 calc R . .
H47 H 0.5725 -0.3171 -0.1001 0.078 Uiso 1 1 calc R . .
H48 H 0.5894 -0.4237 -0.1175 0.078 Uiso 1 1 calc R . .
O9 O 0.88391(19) -0.01327(19) 0.24264(14) 0.0343(7) Uani 1 1 d . . .
O10 O 0.8641(2) 0.08272(19) 0.36676(13) 0.0348(7) Uani 1 1 d . . .
O11 O 0.99464(19) 0.1319(2) 0.45760(14) 0.0366(7) Uani 1 1 d . . .
O12 O 0.8827(2) 0.2961(2) 0.68983(14) 0.0446(8) Uani 1 1 d . . .
N5 N 1.1106(2) 0.0449(2) 0.24664(18) 0.0356(9) Uani 1 1 d . . .
N6 N 0.9082(2) 0.2577(2) 0.63493(17) 0.0333(8) Uani 1 1 d . . .
C41 C 0.9815(3) -0.0630(3) 0.1512(2) 0.0473(12) Uani 1 1 d . . .
H49 H 1.0252 -0.0675 0.1246 0.071 Uiso 1 1 calc R . .
H50 H 0.9260 -0.0426 0.1284 0.071 Uiso 1 1 calc R . .
H51 H 0.9650 -0.1247 0.1517 0.071 Uiso 1 1 calc R . .
C42 C 1.0251(3) 0.0074(3) 0.2260(2) 0.0308(10) Uani 1 1 d . . .
C43 C 1.1501(3) 0.1081(3) 0.3159(2) 0.0321(10) Uani 1 1 d . . .
C44 C 1.2430(3) 0.1486(3) 0.3353(2) 0.0416(11) Uani 1 1 d . . .
H52 H 1.2738 0.1312 0.3007 0.050 Uiso 1 1 calc R . .
C45 C 1.2897(3) 0.2114(3) 0.4016(2) 0.0433(12) Uani 1 1 d . . .
H53 H 1.3521 0.2381 0.4134 0.052 Uiso 1 1 calc R . .
C46 C 1.2432(3) 0.2358(3) 0.4524(2) 0.0415(11) Uani 1 1 d . . .
H54 H 1.2750 0.2789 0.4994 0.050 Uiso 1 1 calc R . .
C47 C 1.1530(3) 0.1986(3) 0.4352(2) 0.0367(11) Uani 1 1 d . . .
H55 H 1.1235 0.2172 0.4706 0.044 Uiso 1 1 calc R . .
C48 C 1.1022(3) 0.1334(3) 0.3664(2) 0.0293(10) Uani 1 1 d . . .
C49 C 1.0065(3) 0.0908(3) 0.3422(2) 0.0279(9) Uani 1 1 d . . .
C50 C 0.9665(3) 0.0290(3) 0.2712(2) 0.0285(9) Uani 1 1 d . . .
C51 C 0.9484(3) 0.1016(3) 0.3874(2) 0.0297(10) Uani 1 1 d . . .
C52 C 1.0285(3) 0.1986(3) 0.7042(2) 0.0462(12) Uani 1 1 d . . .
H56 H 1.0713 0.2544 0.7141 0.069 Uiso 1 1 calc R . .
H57 H 1.0623 0.1458 0.7031 0.069 Uiso 1 1 calc R . .
H58 H 0.9993 0.2119 0.7414 0.069 Uiso 1 1 calc R . .
C53 C 0.8830(3) 0.0916(3) 0.6189(2) 0.0477(12) Uani 1 1 d . . .
H59 H 0.8524 0.1104 0.6554 0.072 Uiso 1 1 calc R . .
H60 H 0.9132 0.0374 0.6205 0.072 Uiso 1 1 calc R . .
H61 H 0.8372 0.0744 0.5721 0.072 Uiso 1 1 calc R . .
C54 C 0.9546(3) 0.1731(3) 0.6324(2) 0.0367(11) Uani 1 1 d . . .
C55 C 1.0019(3) 0.1519(3) 0.5752(2) 0.0385(11) Uani 1 1 d . . .
H62 H 1.0572 0.2001 0.5926 0.046 Uiso 1 1 calc R . .
H63 H 1.0226 0.0900 0.5670 0.046 Uiso 1 1 calc R . .
C56 C 0.9395(3) 0.1505(3) 0.5051(2) 0.0332(10) Uani 1 1 d . . .
H64 H 0.8844 0.1004 0.4852 0.040 Uiso 1 1 calc R . .
C57 C 0.9107(3) 0.2461(3) 0.5173(2) 0.0383(11) Uani 1 1 d . . .
H65 H 0.8720 0.2460 0.4715 0.046 Uiso 1 1 calc R . .
H66 H 0.9663 0.2939 0.5349 0.046 Uiso 1 1 calc R . .
C58 C 0.8574(3) 0.2736(3) 0.5700(2) 0.0376(11) Uani 1 1 d . . .
C59 C 0.8532(4) 0.3797(3) 0.5938(2) 0.0533(14) Uani 1 1 d . . .
H67 H 0.8135 0.3965 0.6238 0.080 Uiso 1 1 calc R . .
H68 H 0.8282 0.3947 0.5520 0.080 Uiso 1 1 calc R . .
H69 H 0.9153 0.4154 0.6206 0.080 Uiso 1 1 calc R . .
C60 C 0.7597(3) 0.2185(3) 0.5393(2) 0.0506(13) Uani 1 1 d . . .
H70 H 0.7606 0.1528 0.5107 0.076 Uiso 1 1 calc R . .
H71 H 0.7200 0.2461 0.5094 0.076 Uiso 1 1 calc R . .
H72 H 0.7360 0.2212 0.5780 0.076 Uiso 1 1 calc R . .
O13 O 0.65444(18) 0.09055(18) 0.30575(14) 0.0334(7) Uani 1 1 d . . .
O14 O 0.78701(18) 0.17106(18) 0.27698(14) 0.0317(7) Uani 1 1 d . . .
O15 O 0.8016(2) 0.32663(18) 0.31119(16) 0.0424(8) Uani 1 1 d . . .
O16 O 1.0674(2) 0.4403(2) 0.21928(19) 0.0584(10) Uani 1 1 d . . .
N7 N 0.5627(2) 0.2673(3) 0.41505(18) 0.0418(9) Uani 1 1 d . . .
H73 H 0.5157 0.2712 0.4315 0.050 Uiso 1 1 calc R . .
N8 N 1.0055(3) 0.4108(2) 0.2399(2) 0.0418(9) Uani 1 1 d . . .
C61 C 0.5080(3) 0.0996(3) 0.3551(3) 0.0530(13) Uani 1 1 d . . .
H74 H 0.5393 0.0590 0.3772 0.079 Uiso 1 1 calc R . .
H75 H 0.4856 0.0656 0.3035 0.079 Uiso 1 1 calc R . .
H76 H 0.4558 0.1176 0.3723 0.079 Uiso 1 1 calc R . .
C62 C 0.5742(3) 0.1865(3) 0.3739(2) 0.0353(10) Uani 1 1 d . . .
C63 C 0.6230(3) 0.3468(3) 0.4332(2) 0.0388(11) Uani 1 1 d . . .
C64 C 0.6101(4) 0.4300(3) 0.4828(2) 0.0546(14) Uani 1 1 d . . .
H77 H 0.5606 0.4290 0.5013 0.066 Uiso 1 1 calc R . .
C65 C 0.6686(4) 0.5133(3) 0.5049(3) 0.0606(15) Uani 1 1 d . . .
H78 H 0.6598 0.5695 0.5386 0.073 Uiso 1 1 calc R . .
C66 C 0.7406(4) 0.5137(3) 0.4770(3) 0.0562(14) Uani 1 1 d . . .
H79 H 0.7806 0.5710 0.4918 0.067 Uiso 1 1 calc R . .
C67 C 0.7550(3) 0.4330(3) 0.4284(2) 0.0451(12) Uani 1 1 d . . .
H80 H 0.8054 0.4351 0.4109 0.054 Uiso 1 1 calc R . .
C68 C 0.6950(3) 0.3461(3) 0.4040(2) 0.0334(10) Uani 1 1 d . . .
C69 C 0.7065(3) 0.2569(3) 0.3553(2) 0.0297(9) Uani 1 1 d . . .
C70 C 0.6491(3) 0.1748(3) 0.3437(2) 0.0283(9) Uani 1 1 d . . .
C71 C 0.7682(3) 0.2453(3) 0.3121(2) 0.0289(9) Uani 1 1 d . . .
C72 C 0.9176(3) 0.5326(3) 0.2196(3) 0.0563(14) Uani 1 1 d . . .
H81 H 0.9490 0.5733 0.2694 0.084 Uiso 1 1 calc R . .
H82 H 0.8558 0.5480 0.2046 0.084 Uiso 1 1 calc R . .
H83 H 0.9529 0.5425 0.1902 0.084 Uiso 1 1 calc R . .
C73 C 0.8698(4) 0.3652(4) 0.1323(2) 0.0640(16) Uani 1 1 d . . .
H84 H 0.9122 0.3735 0.1072 0.096 Uiso 1 1 calc R . .
H85 H 0.8103 0.3817 0.1121 0.096 Uiso 1 1 calc R . .
H86 H 0.8611 0.2995 0.1271 0.096 Uiso 1 1 calc R . .
C74 C 0.9101(3) 0.4294(3) 0.2113(2) 0.0425(12) Uani 1 1 d . . .
C75 C 0.8517(3) 0.4135(3) 0.2541(3) 0.0431(12) Uani 1 1 d . . .
H87 H 0.8695 0.4675 0.3004 0.052 Uiso 1 1 calc R . .
H88 H 0.7864 0.4124 0.2290 0.052 Uiso 1 1 calc R . .
C76 C 0.8598(3) 0.3237(3) 0.2672(2) 0.0366(11) Uani 1 1 d . . .
H89 H 0.8374 0.2673 0.2216 0.044 Uiso 1 1 calc R . .
C77 C 0.9582(3) 0.3252(3) 0.3063(2) 0.0419(12) Uani 1 1 d . . .
H90 H 0.9629 0.2666 0.3151 0.050 Uiso 1 1 calc R . .
H91 H 0.9765 0.3787 0.3530 0.050 Uiso 1 1 calc R . .
C78 C 1.0246(3) 0.3341(3) 0.2675(3) 0.0430(12) Uani 1 1 d . . .
C79 C 1.0178(3) 0.2414(3) 0.2037(3) 0.0575(14) Uani 1 1 d . . .
H92 H 0.9533 0.2190 0.1741 0.086 Uiso 1 1 calc R . .
H93 H 1.0414 0.1936 0.2212 0.086 Uiso 1 1 calc R . .
H94 H 1.0543 0.2530 0.1757 0.086 Uiso 1 1 calc R . .
C80 C 1.1231(3) 0.3610(3) 0.3180(3) 0.0612(15) Uani 1 1 d . . .
H95 H 1.1659 0.3636 0.2918 0.092 Uiso 1 1 calc R . .
H96 H 1.1367 0.3140 0.3387 0.092 Uiso 1 1 calc R . .
H97 H 1.1300 0.4229 0.3558 0.092 Uiso 1 1 calc R . .
N9 N 0.3613(6) -0.3921(6) 0.3404(5) 0.167(3) Uiso 1 1 d . . .
C81 C 0.4227(7) -0.3250(7) 0.3864(5) 0.134(3) Uiso 1 1 d . . .
C82 C 0.5019(6) -0.2472(6) 0.4432(5) 0.146(3) Uiso 1 1 d . . .
H98 H 0.5130 -0.2530 0.4889 0.219 Uiso 1 1 calc R . .
H99 H 0.4850 -0.1854 0.4472 0.219 Uiso 1 1 calc R . .
H100 H 0.5579 -0.2539 0.4294 0.219 Uiso 1 1 calc R . .
N10 N 1.0132(5) -0.8713(5) 0.0275(3) 0.125(2) Uiso 1 1 d . . .
C83 C 1.0744(5) -0.9020(5) 0.0579(4) 0.099(2) Uiso 1 1 d . . .
C84 C 1.1511(4) -0.9294(4) 0.0998(3) 0.093(2) Uiso 1 1 d . . .
H101 H 1.1747 -0.8803 0.1477 0.140 Uiso 1 1 calc R . .
H102 H 1.2000 -0.9378 0.0777 0.140 Uiso 1 1 calc R . .
H103 H 1.1306 -0.9887 0.1024 0.140 Uiso 1 1 calc R . .
C86 C 0.3270(9) 0.2420(9) 0.2371(7) 0.243(6) Uiso 1 1 d . . .
H104 H 0.2945 0.2540 0.1952 0.365 Uiso 1 1 calc R . .
H105 H 0.2827 0.2289 0.2592 0.365 Uiso 1 1 calc R . .
H106 H 0.3584 0.1876 0.2229 0.365 Uiso 1 1 calc R . .
C85 C 0.3916(10) 0.3208(12) 0.2853(8) 0.224(6) Uiso 1 1 d . . .
N12 N 0.4149(8) 0.4122(9) 0.3167(6) 0.244(5) Uiso 1 1 d . . .
O17 O 0.5000 0.0000 0.5000 0.164(7) Uiso 0.50 2 d SP . .
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'
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Y O1 83.18(10) . . ?
O9 Y O5 98.44(10) . . ?
O1 Y O5 149.36(10) . . ?
O9 Y O13 147.88(10) . . ?
O1 Y O13 109.08(10) . . ?
O5 Y O13 85.76(10) . . ?
O9 Y O2 135.35(9) . . ?
O1 Y O2 69.49(9) . . ?
O5 Y O2 89.33(10) . . ?
O13 Y O2 76.19(9) . . ?
O9 Y O14 87.06(9) . . ?
O1 Y O14 73.66(9) . . ?
O5 Y O14 136.89(9) . . ?
O13 Y O14 69.25(9) . . ?
O2 Y O14 116.25(9) . . ?
O9 Y O6 72.92(9) . . ?
O1 Y O6 82.70(9) . . ?
O5 Y O6 68.84(9) . . ?
O13 Y O6 136.63(9) . . ?
O2 Y O6 69.23(9) . . ?
O14 Y O6 150.69(9) . . ?
O9 Y O10 67.86(9) . . ?
O1 Y O10 132.69(9) . . ?
O5 Y O10 74.23(10) . . ?
O13 Y O10 83.01(9) . . ?
O2 Y O10 154.39(9) . . ?
O14 Y O10 68.47(9) . . ?
O6 Y O10 120.12(9) . . ?
O16 K O8 83.47(11) 1_445 2_645 ?
O16 K O4 150.52(11) 1_445 . ?
O8 K O4 92.88(10) 2_645 . ?
O16 K O12 90.00(10) 1_445 2_656 ?
O8 K O12 163.30(10) 2_645 2_656 ?
O4 K O12 85.25(10) . 2_656 ?
O16 K N9 118.37(19) 1_445 . ?
O8 K N9 100.86(19) 2_645 . ?
O4 K N9 91.07(19) . . ?
O12 K N9 95.77(19) 2_656 . ?
C10 O1 Y 141.6(3) . . ?
C11 O2 Y 137.2(3) . . ?
C11 O3 C16 118.3(3) . . ?
N2 O4 K 155.6(3) . . ?
C2 N1 C3 118.7(4) . . ?
O4 N2 C14 115.7(3) . . ?
O4 N2 C18 116.1(3) . . ?
C14 N2 C18 124.3(3) . . ?
N1 C2 C10 124.3(4) . . ?
N1 C2 C1 118.7(4) . . ?
C10 C2 C1 117.0(4) . . ?
N1 C3 C4 115.9(4) . . ?
N1 C3 C8 123.0(4) . . ?
C4 C3 C8 121.1(4) . . ?
C5 C4 C3 121.3(4) . . ?
C4 C5 C6 118.9(4) . . ?
C5 C6 C7 121.7(4) . . ?
C6 C7 C8 121.3(4) . . ?
C7 C8 C3 115.8(4) . . ?
C7 C8 C9 126.3(4) . . ?
C3 C8 C9 117.9(4) . . ?
C10 C9 C11 116.6(3) . . ?
C10 C9 C8 118.0(4) . . ?
C11 C9 C8 125.3(4) . . ?
O1 C10 C9 125.8(4) . . ?
O1 C10 C2 116.3(4) . . ?
C9 C10 C2 117.9(4) . . ?
O2 C11 O3 118.7(4) . . ?
O2 C11 C9 126.2(4) . . ?
O3 C11 C9 115.1(3) . . ?
N2 C14 C12 107.6(3) . . ?
N2 C14 C13 109.1(4) . . ?
C12 C14 C13 109.5(4) . . ?
N2 C14 C15 109.3(3) . . ?
C12 C14 C15 109.2(4) . . ?
C13 C14 C15 112.0(4) . . ?
C16 C15 C14 113.0(4) . . ?
O3 C16 C15 106.2(3) . . ?
O3 C16 C17 109.7(3) . . ?
C15 C16 C17 109.7(3) . . ?
C16 C17 C18 113.5(4) . . ?
N2 C18 C17 109.1(3) . . ?
N2 C18 C19 109.0(4) . . ?
C17 C18 C19 112.6(4) . . ?
N2 C18 C20 107.2(3) . . ?
C17 C18 C20 109.0(4) . . ?
C19 C18 C20 109.7(4) . . ?
C30 O5 Y 143.6(3) . . ?
C31 O6 Y 135.7(3) . . ?
C31 O7 C36 118.3(3) . . ?
N4 O8 K 148.5(3) . 2_645 ?
C22 N3 C23 118.7(4) . . ?
O8 N4 C34 115.8(3) . . ?
O8 N4 C38 116.6(3) . . ?
C34 N4 C38 122.9(3) . . ?
N3 C22 C30 124.3(4) . . ?
N3 C22 C21 118.8(4) . . ?
C30 C22 C21 116.9(4) . . ?
N3 C23 C28 123.1(4) . . ?
N3 C23 C24 116.4(4) . . ?
C28 C23 C24 120.5(4) . . ?
C25 C24 C23 121.6(4) . . ?
C24 C25 C26 119.0(4) . . ?
C27 C26 C25 120.9(4) . . ?
C26 C27 C28 121.9(4) . . ?
C23 C28 C27 116.2(4) . . ?
C23 C28 C29 118.0(4) . . ?
C27 C28 C29 125.8(4) . . ?
C30 C29 C28 118.6(4) . . ?
C30 C29 C31 116.2(4) . . ?
C28 C29 C31 125.1(4) . . ?
O5 C30 C29 125.7(4) . . ?
O5 C30 C22 117.2(4) . . ?
C29 C30 C22 117.1(4) . . ?
O6 C31 O7 119.5(4) . . ?
O6 C31 C29 127.2(4) . . ?
O7 C31 C29 113.1(3) . . ?
N4 C34 C35 108.7(3) . . ?
N4 C34 C32 107.6(3) . . ?
C35 C34 C32 108.1(4) . . ?
N4 C34 C33 110.2(4) . . ?
C35 C34 C33 112.3(4) . . ?
C32 C34 C33 109.8(4) . . ?
C36 C35 C34 114.7(4) . . ?
O7 C36 C35 104.2(3) . . ?
O7 C36 C37 110.3(3) . . ?
C35 C36 C37 108.7(3) . . ?
C38 C37 C36 113.8(3) . . ?
C37 C38 N4 109.1(3) . . ?
C37 C38 C40 109.7(4) . . ?
N4 C38 C40 107.0(3) . . ?
C37 C38 C39 112.6(3) . . ?
N4 C38 C39 108.7(3) . . ?
C40 C38 C39 109.6(4) . . ?
C50 O9 Y 141.2(2) . . ?
C51 O10 Y 135.2(3) . . ?
C51 O11 C56 116.8(3) . . ?
N6 O12 K 150.6(2) . 2_656 ?
C42 N5 C43 118.7(4) . . ?
O12 N6 C58 116.3(3) . . ?
O12 N6 C54 115.3(3) . . ?
C58 N6 C54 123.3(3) . . ?
N5 C42 C50 123.9(4) . . ?
N5 C42 C41 119.4(4) . . ?
C50 C42 C41 116.7(4) . . ?
N5 C43 C44 116.5(4) . . ?
N5 C43 C48 123.5(4) . . ?
C44 C43 C48 120.0(4) . . ?
C45 C44 C43 122.3(4) . . ?
C44 C45 C46 118.1(4) . . ?
C47 C46 C45 121.1(4) . . ?
C46 C47 C48 122.3(4) . . ?
C47 C48 C43 116.2(4) . . ?
C47 C48 C49 126.8(4) . . ?
C43 C48 C49 116.9(3) . . ?
C50 C49 C48 119.0(4) . . ?
C50 C49 C51 115.9(4) . . ?
C48 C49 C51 124.9(4) . . ?
O9 C50 C49 126.0(4) . . ?
O9 C50 C42 116.1(3) . . ?
C49 C50 C42 117.9(4) . . ?
O10 C51 O11 119.5(4) . . ?
O10 C51 C49 125.5(4) . . ?
O11 C51 C49 114.9(4) . . ?
N6 C54 C53 108.8(4) . . ?
N6 C54 C52 107.8(3) . . ?
C53 C54 C52 110.2(4) . . ?
N6 C54 C55 108.4(3) . . ?
C53 C54 C55 113.0(4) . . ?
C52 C54 C55 108.5(4) . . ?
C56 C55 C54 113.1(3) . . ?
O11 C56 C57 109.6(3) . . ?
O11 C56 C55 106.3(3) . . ?
C57 C56 C55 108.9(3) . . ?
C56 C57 C58 113.0(3) . . ?
N6 C58 C57 109.3(3) . . ?
N6 C58 C60 109.4(4) . . ?
C57 C58 C60 112.5(4) . . ?
N6 C58 C59 106.7(3) . . ?
C57 C58 C59 109.2(4) . . ?
C60 C58 C59 109.5(4) . . ?
C70 O13 Y 142.7(2) . . ?
C71 O14 Y 136.8(3) . . ?
C71 O15 C76 118.6(3) . . ?
N8 O16 K 151.7(3) . 1_665 ?
C62 N7 C63 120.5(4) . . ?
O16 N8 C74 115.9(3) . . ?
O16 N8 C78 117.3(4) . . ?
C74 N8 C78 123.2(3) . . ?
N7 C62 C70 122.9(4) . . ?
N7 C62 C61 119.9(4) . . ?
C70 C62 C61 117.2(4) . . ?
N7 C63 C64 116.7(4) . . ?
N7 C63 C68 122.2(4) . . ?
C64 C63 C68 121.1(4) . . ?
C65 C64 C63 120.6(5) . . ?
C64 C65 C66 119.1(5) . . ?
C67 C66 C65 121.5(5) . . ?
C66 C67 C68 120.6(5) . . ?
C63 C68 C67 117.1(4) . . ?
C63 C68 C69 118.0(4) . . ?
C67 C68 C69 124.7(4) . . ?
C70 C69 C68 118.0(4) . . ?
C70 C69 C71 116.7(3) . . ?
C68 C69 C71 125.1(4) . . ?
O13 C70 C69 125.6(4) . . ?
O13 C70 C62 116.6(4) . . ?
C69 C70 C62 117.8(4) . . ?
O14 C71 O15 120.3(4) . . ?
O14 C71 C69 126.2(4) . . ?
O15 C71 C69 113.4(3) . . ?
N8 C74 C75 109.1(4) . . ?
N8 C74 C72 107.8(3) . . ?
C75 C74 C72 109.3(4) . . ?
N8 C74 C73 109.1(4) . . ?
C75 C74 C73 112.0(4) . . ?
C72 C74 C73 109.5(4) . . ?
C76 C75 C74 114.6(4) . . ?
O15 C76 C77 110.7(4) . . ?
O15 C76 C75 104.2(3) . . ?
C77 C76 C75 109.2(3) . . ?
C76 C77 C78 113.8(4) . . ?
N8 C78 C77 110.2(4) . . ?
N8 C78 C80 107.5(3) . . ?
C77 C78 C80 110.1(4) . . ?
N8 C78 C79 108.1(4) . . ?
C77 C78 C79 112.2(4) . . ?
C80 C78 C79 108.7(4) . . ?
C81 N9 K 142.0(7) . . ?
N9 C81 C82 176.6(10) . . ?
N10 C83 C84 174.3(8) . . ?
N12 C85 C86 149.8(16) . . ?
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
Y O9 2.216(3) . ?
Y O1 2.231(3) . ?
Y O5 2.236(3) . ?
Y O13 2.236(3) . ?
Y O2 2.389(3) . ?
Y O14 2.438(3) . ?
Y O6 2.474(3) . ?
Y O10 2.489(3) . ?
K O16 2.615(3) 1_445 ?
K O8 2.661(3) 2_645 ?
K O4 2.664(3) . ?
K O12 2.697(3) 2_656 ?
K N9 2.762(9) . ?
O1 C10 1.276(4) . ?
O2 C11 1.226(4) . ?
O3 C11 1.331(4) . ?
O3 C16 1.449(5) . ?
O4 N2 1.279(4) . ?
N1 C2 1.303(5) . ?
N1 C3 1.382(5) . ?
N2 C14 1.491(5) . ?
N2 C18 1.500(5) . ?
C1 C2 1.495(5) . ?
C2 C10 1.454(5) . ?
C3 C4 1.393(5) . ?
C3 C8 1.418(5) . ?
C4 C5 1.371(6) . ?
C5 C6 1.371(6) . ?
C6 C7 1.379(6) . ?
C7 C8 1.420(6) . ?
C8 C9 1.456(5) . ?
C9 C10 1.415(5) . ?
C9 C11 1.453(5) . ?
C12 C14 1.528(6) . ?
C13 C14 1.530(6) . ?
C14 C15 1.531(6) . ?
C15 C16 1.505(5) . ?
C16 C17 1.514(5) . ?
C17 C18 1.515(6) . ?
C18 C19 1.521(6) . ?
C18 C20 1.533(6) . ?
O5 C30 1.280(4) . ?
O6 C31 1.222(4) . ?
O7 C31 1.351(4) . ?
O7 C36 1.450(5) . ?
O8 N4 1.283(4) . ?
O8 K 2.661(3) 2_645 ?
N3 C22 1.302(5) . ?
N3 C23 1.384(5) . ?
N4 C34 1.489(5) . ?
N4 C38 1.508(5) . ?
C21 C22 1.500(6) . ?
C22 C30 1.454(5) . ?
C23 C28 1.403(6) . ?
C23 C24 1.406(6) . ?
C24 C25 1.363(6) . ?
C25 C26 1.377(6) . ?
C26 C27 1.375(6) . ?
C27 C28 1.421(5) . ?
C28 C29 1.446(5) . ?
C29 C30 1.418(5) . ?
C29 C31 1.459(5) . ?
C32 C34 1.537(5) . ?
C33 C34 1.536(6) . ?
C34 C35 1.527(6) . ?
C35 C36 1.515(5) . ?
C36 C37 1.523(6) . ?
C37 C38 1.508(5) . ?
C38 C40 1.527(6) . ?
C38 C39 1.539(6) . ?
O9 C50 1.269(4) . ?
O10 C51 1.227(5) . ?
O11 C51 1.354(5) . ?
O11 C56 1.452(5) . ?
O12 N6 1.284(4) . ?
O12 K 2.697(3) 2_656 ?
N5 C42 1.294(5) . ?
N5 C43 1.382(5) . ?
N6 C58 1.498(5) . ?
N6 C54 1.505(5) . ?
C41 C42 1.505(5) . ?
C42 C50 1.456(5) . ?
C43 C44 1.414(6) . ?
C43 C48 1.419(5) . ?
C44 C45 1.355(6) . ?
C45 C46 1.410(6) . ?
C46 C47 1.367(6) . ?
C47 C48 1.415(5) . ?
C48 C49 1.449(5) . ?
C49 C50 1.402(5) . ?
C49 C51 1.459(5) . ?
C52 C54 1.530(6) . ?
C53 C54 1.521(6) . ?
C54 C55 1.532(6) . ?
C55 C56 1.526(5) . ?
C56 C57 1.512(5) . ?
C57 C58 1.520(6) . ?
C58 C60 1.528(6) . ?
C58 C59 1.539(5) . ?
O13 C70 1.280(4) . ?
O14 C71 1.220(4) . ?
O15 C71 1.344(4) . ?
O15 C76 1.455(5) . ?
O16 N8 1.281(4) . ?
O16 K 2.615(3) 1_665 ?
N7 C62 1.293(5) . ?
N7 C63 1.368(5) . ?
N8 C74 1.504(5) . ?
N8 C78 1.508(5) . ?
C61 C62 1.503(6) . ?
C62 C70 1.454(5) . ?
C63 C64 1.402(6) . ?
C63 C68 1.408(6) . ?
C64 C65 1.381(7) . ?
C65 C66 1.393(7) . ?
C66 C67 1.376(6) . ?
C67 C68 1.429(6) . ?
C68 C69 1.448(5) . ?
C69 C70 1.414(5) . ?
C69 C71 1.467(5) . ?
C72 C74 1.534(6) . ?
C73 C74 1.537(6) . ?
C74 C75 1.515(6) . ?
C75 C76 1.514(5) . ?
C76 C77 1.500(6) . ?
C77 C78 1.510(6) . ?
C78 C80 1.524(6) . ?
C78 C79 1.553(6) . ?
N9 C81 1.260(10) . ?
C81 C82 1.545(11) . ?
N10 C83 1.202(8) . ?
C83 C84 1.445(9) . ?
C86 C85 1.394(15) . ?
C85 N12 1.307(16) . ?
