#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:33:00 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242069 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/20/4132027.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_4132027
loop_
_publ_author_name
'Cai, Li-Xuan'
'Li, Shao-Chuan'
'Yan, Dan-Ni'
'Zhou, Li-Peng'
'Guo, Fang'
'Sun, Qing-Fu'
_publ_section_title
;
 Water-Soluble Redox-Active Cage Hosting Polyoxometalates for Selective
 Desulfurization Catalysis.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4869
_journal_page_last               4876
_journal_paper_doi               10.1021/jacs.8b00394
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C72 H160 Mo8 N4 O28'
_chemical_formula_weight         2297.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 94.276(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0401(15)
_cell_length_b                   22.3150(19)
_cell_length_c                   16.9829(16)
_cell_measurement_reflns_used    51042
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.740
_cell_measurement_theta_min      1.884
_cell_volume                     4928.1(8)
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7388
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51042
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        26.313
_diffrn_reflns_theta_max         28.740
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'SSRF BL17B Beamline'
_exptl_absorpt_coefficient_mu    1.157
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10575
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1027P)²+9.9275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8431
_reflns_number_total             10575
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b00394_si_004.cif
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132027
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
MO1 Mo 0.56201(3) 0.04245(2) 0.08178(3) 0.03773(14) Uani 1 1 d . .
O1 O 0.6387(4) 0.0454(2) -0.0005(3) 0.0573(11) Uani 1 1 d . .
MO2 Mo 0.62160(4) -0.12647(2) 0.06169(3) 0.04657(16) Uani 1 1 d . .
O2 O 0.4418(3) 0.07869(19) 0.0591(3) 0.0511(10) Uani 1 1 d . .
MO3 Mo 0.72925(4) -0.03507(2) -0.06788(3) 0.04700(16) Uani 1 1 d . .
O3 O 0.6537(3) 0.0107(2) -0.1442(2) 0.0535(10) Uani 1 1 d . .
MO4 Mo 0.39493(4) -0.09020(2) 0.12732(3) 0.05232(17) Uani 1 1 d . .
O5 O 0.5450(3) -0.0344(2) 0.1072(3) 0.0586(11) Uani 1 1 d . .
O6 O 0.4799(3) -0.13981(19) 0.0684(3) 0.0558(11) Uani 1 1 d . .
O7 O 0.6695(4) -0.1383(2) 0.1561(3) 0.0683(13) Uani 1 1 d . .
O8 O 0.6554(4) -0.1885(2) 0.0125(3) 0.0678(13) Uani 1 1 d . .
O9 O 0.7648(4) -0.0933(2) -0.1241(3) 0.0695(13) Uani 1 1 d . .
O10 O 0.8385(4) 0.0060(2) -0.0503(3) 0.0641(12) Uani 1 1 d . .
N13 N 1.0620(4) 0.0208(3) -0.1992(3) 0.0515(12) Uani 1 1 d . .
C14 C 1.1705(5) 0.0329(3) -0.2232(4) 0.0530(15) Uani 1 1 d . .
H14A H 1.176973 0.075465 -0.233195 0.064 Uiso 1 1 calc R U
H14B H 1.218881 0.022902 -0.179040 0.064 Uiso 1 1 calc R U
C15 C 0.9869(5) 0.0468(4) -0.2636(4) 0.0584(16) Uani 1 1 d . .
H15A H 1.006270 0.088007 -0.272805 0.070 Uiso 1 1 calc R U
H15B H 0.994383 0.024718 -0.312019 0.070 Uiso 1 1 calc R U
C16 C 1.0422(5) -0.0458(3) -0.1913(4) 0.0581(16) Uani 1 1 d . .
H16A H 1.042537 -0.063864 -0.243225 0.070 Uiso 1 1 calc R U
H16B H 0.973948 -0.051190 -0.173345 0.070 Uiso 1 1 calc R U
C17 C 1.0505(5) 0.0510(3) -0.1207(4) 0.0503(14) Uani 1 1 d . .
H17A H 0.984031 0.040039 -0.102897 0.060 Uiso 1 1 calc R U
H17B H 1.102593 0.034890 -0.082654 0.060 Uiso 1 1 calc R U
C18 C 0.8746(5) 0.0455(4) -0.2460(5) 0.0634(18) Uani 1 1 d . .
H18A H 0.851137 0.004288 -0.244620 0.076 Uiso 1 1 calc R U
H18B H 0.866995 0.063226 -0.194662 0.076 Uiso 1 1 calc R U
O19 O 0.6251(3) 0.0773(2) 0.1602(3) 0.0622(12) Uani 1 1 d . .
C20 C 1.1186(5) -0.0793(3) -0.1354(5) 0.0621(17) Uani 1 1 d . .
H20A H 1.188018 -0.070921 -0.149138 0.075 Uiso 1 1 calc R U
H20B H 1.112285 -0.065636 -0.081756 0.075 Uiso 1 1 calc R U
C21 C 1.0987(8) -0.1455(4) -0.1404(6) 0.083(2) Uani 1 1 d . .
H21A H 1.099996 -0.158297 -0.194915 0.100 Uiso 1 1 calc R U
H21B H 1.030686 -0.153786 -0.123557 0.100 Uiso 1 1 calc R U
C22 C 1.1780(9) -0.1816(5) -0.0894(8) 0.109(4) Uani 1 1 d . .
H22A H 1.168186 -0.223560 -0.099834 0.164 Uiso 1 1 calc R U
H22B H 1.169698 -0.173790 -0.034610 0.164 Uiso 1 1 calc R U
H22C H 1.245981 -0.170100 -0.101557 0.164 Uiso 1 1 calc R U
C23 C 1.2006(6) -0.0003(4) -0.2939(5) 0.0695(19) Uani 1 1 d . .
H23A H 1.149242 0.005810 -0.337515 0.083 Uiso 1 1 calc R U
H23B H 1.204459 -0.042817 -0.282462 0.083 Uiso 1 1 calc R U
C24 C 1.3059(7) 0.0223(6) -0.3171(6) 0.100(3) Uani 1 1 d . .
H24A H 1.303138 0.065359 -0.324854 0.120 Uiso 1 1 calc R U
H24B H 1.357882 0.013848 -0.274681 0.120 Uiso 1 1 calc R U
C25 C 1.0588(6) 0.1172(3) -0.1193(4) 0.0610(17) Uani 1 1 d . .
H25A H 1.011026 0.134270 -0.159729 0.073 Uiso 1 1 calc R U
H25B H 1.127851 0.129125 -0.130277 0.073 Uiso 1 1 calc R U
C26 C 1.0344(6) 0.1406(4) -0.0381(4) 0.0684(19) Uani 1 1 d . .
H26A H 1.075303 0.118865 0.002544 0.082 Uiso 1 1 calc R U
H26B H 0.962448 0.133328 -0.030543 0.082 Uiso 1 1 calc R U
C27 C 0.8105(5) 0.0793(4) -0.3077(5) 0.073(2) Uani 1 1 d . .
H27A H 0.824935 0.063984 -0.359175 0.088 Uiso 1 1 calc R U
H27B H 0.738609 0.071386 -0.300683 0.088 Uiso 1 1 calc R U
O28 O 0.2813(4) -0.1273(2) 0.1140(4) 0.0821(17) Uani 1 1 d . .
O29 O 0.4402(5) -0.1072(3) 0.2214(3) 0.0796(16) Uani 1 1 d . .
C30 C 1.0568(9) 0.2077(4) -0.0297(6) 0.100(3) Uani 1 1 d . .
H30A H 1.019199 0.229064 -0.071506 0.150 Uiso 1 1 calc R U
H30B H 1.129148 0.214555 -0.032500 0.150 Uiso 1 1 calc R U
H30C H 1.036263 0.221515 0.020311 0.150 Uiso 1 1 calc R U
C31 C 1.3338(13) -0.0069(12) -0.3898(11) 0.211(10) Uani 1 1 d . .
H31A H 1.280520 -0.000263 -0.430997 0.316 Uiso 1 1 calc R U
H31B H 1.341815 -0.049198 -0.380756 0.316 Uiso 1 1 calc R U
H31C H 1.397275 0.009518 -0.405247 0.316 Uiso 1 1 calc R U
C32 C 0.8266(8) 0.1453(5) -0.3072(8) 0.110(4) Uani 1 1 d . .
H32A H 0.895633 0.153965 -0.319811 0.165 Uiso 1 1 calc R U
H32B H 0.815861 0.160841 -0.255760 0.165 Uiso 1 1 calc R U
H32C H 0.778869 0.163602 -0.345659 0.165 Uiso 1 1 calc R U
C33 C 0.5930(9) -0.1257(4) -0.3218(7) 0.096(3) Uani 1 1 d . .
H33A H 0.539435 -0.137035 -0.361784 0.115 Uiso 1 1 calc R U
H33B H 0.656494 -0.144787 -0.334619 0.115 Uiso 1 1 calc R U
C34 C 0.6065(10) -0.0573(5) -0.3217(6) 0.103(3) Uani 1 1 d D .
H34A H 0.546149 -0.038933 -0.301846 0.123 Uiso 1 1 calc R U
H34B H 0.665289 -0.046887 -0.285937 0.123 Uiso 1 1 calc R U
C35 C 0.6217(12) -0.0326(6) -0.4004(7) 0.133(5) Uani 1 1 d D .
H35A H 0.691097 -0.039987 -0.413143 0.199 Uiso 1 1 calc R U
H35B H 0.609131 0.009779 -0.400344 0.199 Uiso 1 1 calc R U
H35C H 0.574849 -0.051509 -0.439004 0.199 Uiso 1 1 calc R U
N36 N 0.5451(5) -0.2129(3) -0.2352(4) 0.0718(17) Uani 1 1 d . .
C37 C 0.5646(6) -0.1468(3) -0.2422(5) 0.0661(19) Uani 1 1 d . .
H37A H 0.619640 -0.135791 -0.203228 0.079 Uiso 1 1 calc R U
H37B H 0.503341 -0.125474 -0.229048 0.079 Uiso 1 1 calc R U
C38 C 0.5109(7) -0.2228(3) -0.1540(5) 0.072(2) Uani 1 1 d . .
H38A H 0.449202 -0.199320 -0.148577 0.086 Uiso 1 1 calc R U
H38B H 0.563742 -0.207446 -0.116067 0.086 Uiso 1 1 calc R U
C39 C 0.4639(7) -0.2340(4) -0.2964(5) 0.076(2) Uani 1 1 d . .
H39A H 0.489022 -0.227940 -0.348186 0.091 Uiso 1 1 calc R U
H39B H 0.454290 -0.276710 -0.289621 0.091 Uiso 1 1 calc R U
C40 C 0.3617(8) -0.2040(4) -0.2950(6) 0.091(3) Uani 1 1 d . .
H40A H 0.370614 -0.160962 -0.298432 0.110 Uiso 1 1 calc R U
H40B H 0.332569 -0.212818 -0.245376 0.110 Uiso 1 1 calc R U
C41 C 0.6430(8) -0.2491(4) -0.2438(7) 0.097(3) Uani 1 1 d . .
H41A H 0.625673 -0.291335 -0.241375 0.116 Uiso 1 1 calc R U
H41B H 0.665799 -0.241547 -0.295990 0.116 Uiso 1 1 calc R U
C42 C 0.7301(9) -0.2377(7) -0.1856(10) 0.153(7) Uani 1 1 d . .
H42A H 0.708527 -0.246926 -0.133525 0.183 Uiso 1 1 calc R U
H42B H 0.746166 -0.195304 -0.186577 0.183 Uiso 1 1 calc R U
C43 C 0.4885(10) -0.2880(4) -0.1326(6) 0.105(3) Uani 1 1 d . .
H43A H 0.438064 -0.304421 -0.171618 0.126 Uiso 1 1 calc R U
H43B H 0.551045 -0.311361 -0.134217 0.126 Uiso 1 1 calc R U
C44 C 0.4493(10) -0.2937(5) -0.0532(6) 0.103(3) Uani 1 1 d D .
H44A H 0.499260 -0.276917 -0.014095 0.124 Uiso 1 1 calc R U
H44B H 0.386114 -0.270995 -0.051675 0.124 Uiso 1 1 calc R U
C45 C 0.4296(13) -0.3568(6) -0.0330(7) 0.137(5) Uani 1 1 d D .
H45A H 0.377494 -0.372924 -0.069940 0.205 Uiso 1 1 calc R U
H45B H 0.406801 -0.358896 0.019361 0.205 Uiso 1 1 calc R U
H45C H 0.491783 -0.379564 -0.035349 0.205 Uiso 1 1 calc R U
C46 C 0.2886(9) -0.2250(5) -0.3628(7) 0.105(3) Uani 1 1 d D .
H46A H 0.318019 -0.215607 -0.412087 0.126 Uiso 1 1 calc R U
H46B H 0.281905 -0.268244 -0.359778 0.126 Uiso 1 1 calc R U
C47 C 0.1869(11) -0.1984(9) -0.3636(12) 0.199(9) Uani 1 1 d D .
H47A H 0.142852 -0.216212 -0.405015 0.298 Uiso 1 1 calc R U
H47B H 0.191740 -0.156038 -0.372749 0.298 Uiso 1 1 calc R U
H47C H 0.158821 -0.205234 -0.313749 0.298 Uiso 1 1 calc R U
C48 C 0.8268(12) -0.2724(7) -0.1974(12) 0.153(6) Uani 1 1 d D .
H48A H 0.870419 -0.274707 -0.148662 0.184 Uiso 1 1 calc R U
H48B H 0.810798 -0.312736 -0.215799 0.184 Uiso 1 1 calc R U
C49 C 0.8756(17) -0.2391(10) -0.2556(11) 0.201(9) Uani 1 1 d D .
H49A H 0.853764 -0.254177 -0.307156 0.301 Uiso 1 1 calc R U
H49B H 0.948827 -0.243157 -0.246824 0.301 Uiso 1 1 calc R U
H49C H 0.856995 -0.197643 -0.252229 0.301 Uiso 1 1 calc R U
C50 C -0.0960(19) -0.1032(14) -0.4021(13) 0.230(13) Uani 1 1 d D .
H50A H -0.077282 -0.134264 -0.363796 0.276 Uiso 1 1 calc R U
H50B H -0.150874 -0.079713 -0.381871 0.276 Uiso 1 1 calc R U
C52 C 0.023(3) -0.0797(12) -0.4812(17) 0.261(15) Uani 1 1 d D .
H52A H 0.029688 -0.042646 -0.510257 0.313 Uiso 1 1 calc R U
H52B H 0.091550 -0.097091 -0.472642 0.313 Uiso 1 1 calc R U
C53 C -0.038(3) -0.1178(11) -0.5247(16) 0.244(14) Uani 1 1 d D .
H53A H -0.001932 -0.154865 -0.534530 0.292 Uiso 1 1 calc R U
H53B H -0.061645 -0.099915 -0.574772 0.292 Uiso 1 1 calc R U
C54 C -0.1314(19) -0.1291(9) -0.4700(18) 0.240(15) Uani 1 1 d D .
H54A H -0.194027 -0.109996 -0.491793 0.288 Uiso 1 1 calc R U
H54B H -0.143872 -0.171500 -0.462965 0.288 Uiso 1 1 calc R U
O55 O -0.0136(16) -0.0671(8) -0.4092(9) 0.219(7) Uani 1 1 d . .
O4 O 0.7208(3) -0.06884(19) 0.0337(2) 0.0470(9) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0038 0.0019 '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 0.0074 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.4769 0.7523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0125 0.0068 '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
O19 MO1 O1 109.3(2) . .
O19 MO1 O2 109.2(2) . .
O1 MO1 O2 110.5(2) . .
O19 MO1 O5 108.1(3) . .
O1 MO1 O5 108.2(2) . .
O2 MO1 O5 111.4(2) . .
MO1 O1 MO4 130.5(2) . 3_655
MO1 O1 MO3 130.6(2) . .
MO4 O1 MO3 87.03(16) 3_655 .
O8 MO2 O7 104.4(3) . .
O8 MO2 O6 101.2(2) . .
O7 MO2 O6 102.2(2) . .
O8 MO2 O4 102.8(2) . .
O7 MO2 O4 97.6(2) . .
O6 MO2 O4 143.87(18) . .
O8 MO2 O2 91.5(2) . 3_655
O7 MO2 O2 162.6(2) . 3_655
O6 MO2 O2 81.11(18) . 3_655
O4 MO2 O2 71.64(15) . 3_655
O8 MO2 O5 167.1(2) . .
O7 MO2 O5 87.8(2) . .
O6 MO2 O5 71.76(17) . .
O4 MO2 O5 79.17(17) . .
O2 MO2 O5 76.91(16) 3_655 .
MO1 O2 MO2 128.8(2) . 3_655
MO1 O2 MO3 126.7(2) . 3_655
MO2 O2 MO3 88.37(13) 3_655 3_655
O9 MO3 O10 104.5(3) . .
O9 MO3 O3 100.4(2) . .
O10 MO3 O3 102.6(2) . .
O9 MO3 O4 104.2(2) . .
O10 MO3 O4 99.14(19) . .
O3 MO3 O4 141.69(18) . .
O9 MO3 O2 91.1(2) . 3_655
O10 MO3 O2 163.3(2) . 3_655
O3 MO3 O2 79.88(17) . 3_655
O4 MO3 O2 70.81(15) . 3_655
O9 MO3 O1 167.2(2) . .
O10 MO3 O1 87.1(2) . .
O3 MO3 O1 71.29(17) . .
O4 MO3 O1 78.78(17) . .
O2 MO3 O1 78.01(15) 3_655 .
MO3 O3 MO4 124.5(2) . 3_655
O28 MO4 O29 104.7(3) . .
O28 MO4 O6 100.6(3) . .
O29 MO4 O6 100.9(2) . .
O28 MO4 O3 100.1(2) . 3_655
O29 MO4 O3 99.3(2) . 3_655
O6 MO4 O3 146.19(19) . 3_655
O28 MO4 O5 163.8(3) . .
O29 MO4 O5 91.2(2) . .
O6 MO4 O5 73.11(17) . .
O3 MO4 O5 79.67(17) 3_655 .
O28 MO4 O1 89.1(3) . 3_655
O29 MO4 O1 165.3(3) . 3_655
O6 MO4 O1 81.00(18) . 3_655
O3 MO4 O1 72.91(17) 3_655 3_655
O5 MO4 O1 75.36(17) . 3_655
MO1 O5 MO4 131.2(2) . .
MO1 O5 MO2 132.3(2) . .
MO4 O5 MO2 87.99(15) . .
MO2 O6 MO4 123.5(2) . .
C17 N13 C16 109.3(5) . .
C17 N13 C14 108.2(5) . .
C16 N13 C14 111.3(5) . .
C17 N13 C15 111.3(5) . .
C16 N13 C15 109.3(5) . .
C14 N13 C15 107.4(5) . .
C23 C14 N13 115.8(6) . .
C23 C14 H14A 108.3 . .
N13 C14 H14A 108.3 . .
C23 C14 H14B 108.3 . .
N13 C14 H14B 108.3 . .
H14A C14 H14B 107.4 . .
C18 C15 N13 115.4(6) . .
C18 C15 H15A 108.4 . .
N13 C15 H15A 108.4 . .
C18 C15 H15B 108.4 . .
N13 C15 H15B 108.4 . .
H15A C15 H15B 107.5 . .
N13 C16 C20 115.4(5) . .
N13 C16 H16A 108.4 . .
C20 C16 H16A 108.4 . .
N13 C16 H16B 108.4 . .
C20 C16 H16B 108.4 . .
H16A C16 H16B 107.5 . .
C25 C17 N13 116.5(5) . .
C25 C17 H17A 108.2 . .
N13 C17 H17A 108.2 . .
C25 C17 H17B 108.2 . .
N13 C17 H17B 108.2 . .
H17A C17 H17B 107.3 . .
C27 C18 C15 110.6(6) . .
C27 C18 H18A 109.5 . .
C15 C18 H18A 109.5 . .
C27 C18 H18B 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 108.1 . .
C21 C20 C16 110.3(7) . .
C21 C20 H20A 109.6 . .
C16 C20 H20A 109.6 . .
C21 C20 H20B 109.6 . .
C16 C20 H20B 109.6 . .
H20A C20 H20B 108.1 . .
C20 C21 C22 112.3(8) . .
C20 C21 H21A 109.1 . .
C22 C21 H21A 109.1 . .
C20 C21 H21B 109.1 . .
C22 C21 H21B 109.1 . .
H21A C21 H21B 107.9 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C14 C23 C24 109.7(7) . .
C14 C23 H23A 109.7 . .
C24 C23 H23A 109.7 . .
C14 C23 H23B 109.7 . .
C24 C23 H23B 109.7 . .
H23A C23 H23B 108.2 . .
C31 C24 C23 110.6(12) . .
C31 C24 H24A 109.5 . .
C23 C24 H24A 109.5 . .
C31 C24 H24B 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 108.1 . .
C17 C25 C26 109.5(6) . .
C17 C25 H25A 109.8 . .
C26 C25 H25A 109.8 . .
C17 C25 H25B 109.8 . .
C26 C25 H25B 109.8 . .
H25A C25 H25B 108.2 . .
C25 C26 C30 111.5(7) . .
C25 C26 H26A 109.3 . .
C30 C26 H26A 109.3 . .
C25 C26 H26B 109.3 . .
C30 C26 H26B 109.3 . .
H26A C26 H26B 108.0 . .
C32 C27 C18 115.1(7) . .
C32 C27 H27A 108.5 . .
C18 C27 H27A 108.5 . .
C32 C27 H27B 108.5 . .
C18 C27 H27B 108.5 . .
H27A C27 H27B 107.5 . .
C26 C30 H30A 109.5 . .
C26 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C26 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C24 C31 H31A 109.5 . .
C24 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C24 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C27 C32 H32A 109.5 . .
C27 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C27 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C37 C33 C34 110.2(8) . .
C37 C33 H33A 109.6 . .
C34 C33 H33A 109.6 . .
C37 C33 H33B 109.6 . .
C34 C33 H33B 109.6 . .
H33A C33 H33B 108.1 . .
C35 C34 C33 113.2(10) . .
C35 C34 H34A 108.9 . .
C33 C34 H34A 108.9 . .
C35 C34 H34B 108.9 . .
C33 C34 H34B 108.9 . .
H34A C34 H34B 107.8 . .
C34 C35 H35A 109.5 . .
C34 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C34 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C38 N36 C37 106.3(5) . .
C38 N36 C39 110.4(7) . .
C37 N36 C39 111.5(7) . .
C38 N36 C41 108.6(7) . .
C37 N36 C41 111.3(7) . .
C39 N36 C41 108.6(6) . .
N36 C37 C33 115.6(6) . .
N36 C37 H37A 108.4 . .
C33 C37 H37A 108.4 . .
N36 C37 H37B 108.4 . .
C33 C37 H37B 108.4 . .
H37A C37 H37B 107.4 . .
N36 C38 C43 115.7(7) . .
N36 C38 H38A 108.4 . .
C43 C38 H38A 108.4 . .
N36 C38 H38B 108.4 . .
C43 C38 H38B 108.4 . .
H38A C38 H38B 107.4 . .
C40 C39 N36 115.6(6) . .
C40 C39 H39A 108.4 . .
N36 C39 H39A 108.4 . .
C40 C39 H39B 108.4 . .
N36 C39 H39B 108.4 . .
H39A C39 H39B 107.4 . .
C39 C40 C46 111.2(8) . .
C39 C40 H40A 109.4 . .
C46 C40 H40A 109.4 . .
C39 C40 H40B 109.4 . .
C46 C40 H40B 109.4 . .
H40A C40 H40B 108.0 . .
C42 C41 N36 116.9(7) . .
C42 C41 H41A 108.1 . .
N36 C41 H41A 108.1 . .
C42 C41 H41B 108.1 . .
N36 C41 H41B 108.1 . .
H41A C41 H41B 107.3 . .
C41 C42 C48 115.7(11) . .
C41 C42 H42A 108.4 . .
C48 C42 H42A 108.4 . .
C41 C42 H42B 108.4 . .
C48 C42 H42B 108.4 . .
H42A C42 H42B 107.4 . .
C44 C43 C38 112.5(8) . .
C44 C43 H43A 109.1 . .
C38 C43 H43A 109.1 . .
C44 C43 H43B 109.1 . .
C38 C43 H43B 109.1 . .
H43A C43 H43B 107.8 . .
C45 C44 C43 111.8(10) . .
C45 C44 H44A 109.3 . .
C43 C44 H44A 109.3 . .
C45 C44 H44B 109.3 . .
C43 C44 H44B 109.3 . .
H44A C44 H44B 107.9 . .
C44 C45 H45A 109.5 . .
C44 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C44 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C47 C46 C40 113.8(10) . .
C47 C46 H46A 108.8 . .
C40 C46 H46A 108.8 . .
C47 C46 H46B 108.8 . .
C40 C46 H46B 108.8 . .
H46A C46 H46B 107.7 . .
C46 C47 H47A 109.5 . .
C46 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C46 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C49 C48 C42 104.2(16) . .
C49 C48 H48A 110.9 . .
C42 C48 H48A 110.9 . .
C49 C48 H48B 110.9 . .
C42 C48 H48B 110.9 . .
H48A C48 H48B 108.9 . .
C48 C49 H49A 109.5 . .
C48 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
C48 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C54 C50 O55 114(2) . .
C54 C50 H50A 108.8 . .
O55 C50 H50A 108.8 . .
C54 C50 H50B 108.8 . .
O55 C50 H50B 108.8 . .
H50A C50 H50B 107.7 . .
C53 C52 O55 113(3) . .
C53 C52 H52A 109.1 . .
O55 C52 H52A 109.1 . .
C53 C52 H52B 109.1 . .
O55 C52 H52B 109.1 . .
H52A C52 H52B 107.8 . .
C52 C53 C54 103(2) . .
C52 C53 H53A 111.2 . .
C54 C53 H53A 111.2 . .
C52 C53 H53B 111.2 . .
C54 C53 H53B 111.2 . .
H53A C53 H53B 109.1 . .
C50 C54 C53 102(2) . .
C50 C54 H54A 111.4 . .
C53 C54 H54A 111.4 . .
C50 C54 H54B 111.4 . .
C53 C54 H54B 111.4 . .
H54A C54 H54B 109.3 . .
C50 O55 C52 106.9(18) . .
MO3 O4 MO2 125.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
MO1 O19 1.701(4) .
MO1 O1 1.779(5) .
MO1 O2 1.781(4) .
MO1 O5 1.786(4) .
O1 MO4 2.385(5) 3_655
O1 MO3 2.477(5) .
MO2 O8 1.693(5) .
MO2 O7 1.698(5) .
MO2 O6 1.883(5) .
MO2 O4 1.909(4) .
MO2 O2 2.403(4) 3_655
MO2 O5 2.435(5) .
O2 MO2 2.403(4) 3_655
O2 MO3 2.448(4) 3_655
MO3 O9 1.696(5) .
MO3 O10 1.702(5) .
MO3 O3 1.872(4) .
MO3 O4 1.894(4) .
MO3 O2 2.448(4) 3_655
O3 MO4 1.912(5) 3_655
MO4 O28 1.697(5) .
MO4 O29 1.705(5) .
MO4 O6 1.903(5) .
MO4 O3 1.912(5) 3_655
MO4 O5 2.366(4) .
MO4 O1 2.385(5) 3_655
N13 C17 1.511(8) .
N13 C16 1.515(9) .
N13 C14 1.526(8) .
N13 C15 1.526(8) .
C14 C23 1.487(10) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C18 1.516(9) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C20 1.520(10) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 C25 1.482(10) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 C27 1.495(10) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C20 C21 1.502(11) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C22 1.528(14) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 C24 1.540(11) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 C31 1.47(2) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 C26 1.530(10) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 C30 1.530(12) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C27 C32 1.487(13) .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C33 C37 1.504(13) .
C33 C34 1.537(14) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 C35 1.473(13) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
N36 C38 1.496(11) .
N36 C37 1.503(10) .
N36 C39 1.504(10) .
N36 C41 1.528(11) .
C37 H37A 0.9700 .
C37 H37B 0.9700 .
C38 C43 1.535(12) .
C38 H38A 0.9700 .
C38 H38B 0.9700 .
C39 C40 1.492(13) .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C40 C46 1.514(12) .
C40 H40A 0.9700 .
C40 H40B 0.9700 .
C41 C42 1.471(15) .
C41 H41A 0.9700 .
C41 H41B 0.9700 .
C42 C48 1.506(17) .
C42 H42A 0.9700 .
C42 H42B 0.9700 .
C43 C44 1.483(16) .
C43 H43A 0.9700 .
C43 H43B 0.9700 .
C44 C45 1.475(12) .
C44 H44A 0.9700 .
C44 H44B 0.9700 .
C45 H45A 0.9600 .
C45 H45B 0.9600 .
C45 H45C 0.9600 .
C46 C47 1.453(14) .
C46 H46A 0.9700 .
C46 H46B 0.9700 .
C47 H47A 0.9600 .
C47 H47B 0.9600 .
C47 H47C 0.9600 .
C48 C49 1.424(15) .
C48 H48A 0.9700 .
C48 H48B 0.9700 .
C49 H49A 0.9600 .
C49 H49B 0.9600 .
C49 H49C 0.9600 .
C50 C54 1.34(2) .
C50 O55 1.36(2) .
C50 H50A 0.9700 .
C50 H50B 0.9700 .
C52 C53 1.35(2) .
C52 O55 1.38(3) .
C52 H52A 0.9700 .
C52 H52B 0.9700 .
C53 C54 1.61(4) .
C53 H53A 0.9700 .
C53 H53B 0.9700 .
C54 H54A 0.9700 .
C54 H54B 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O19 MO1 O1 MO4 -118.9(3) . 3_655
O2 MO1 O1 MO4 1.3(4) . 3_655
O5 MO1 O1 MO4 123.6(3) . 3_655
O19 MO1 O1 MO3 111.2(3) . .
O2 MO1 O1 MO3 -128.6(3) . .
O5 MO1 O1 MO3 -6.4(4) . .
O19 MO1 O2 MO2 120.7(3) . 3_655
O1 MO1 O2 MO2 0.4(3) . 3_655
O5 MO1 O2 MO2 -120.0(3) . 3_655
O19 MO1 O2 MO3 -115.6(3) . 3_655
O1 MO1 O2 MO3 124.1(3) . 3_655
O5 MO1 O2 MO3 3.7(4) . 3_655
O9 MO3 O3 MO4 -170.5(3) . 3_655
O10 MO3 O3 MO4 -62.9(3) . 3_655
O4 MO3 O3 MO4 60.2(4) . 3_655
O2 MO3 O3 MO4 100.3(3) 3_655 3_655
O1 MO3 O3 MO4 19.7(2) . 3_655
O19 MO1 O5 MO4 113.0(3) . .
O1 MO1 O5 MO4 -128.7(3) . .
O2 MO1 O5 MO4 -7.0(4) . .
O19 MO1 O5 MO2 -109.9(4) . .
O1 MO1 O5 MO2 8.4(4) . .
O2 MO1 O5 MO2 130.1(3) . .
O8 MO2 O6 MO4 173.2(3) . .
O7 MO2 O6 MO4 65.7(3) . .
O4 MO2 O6 MO4 -56.0(5) . .
O2 MO2 O6 MO4 -96.9(3) 3_655 .
O5 MO2 O6 MO4 -17.9(2) . .
C17 N13 C14 C23 172.0(6) . .
C16 N13 C14 C23 51.9(8) . .
C15 N13 C14 C23 -67.8(8) . .
C17 N13 C15 C18 -55.2(8) . .
C16 N13 C15 C18 65.7(8) . .
C14 N13 C15 C18 -173.4(6) . .
C17 N13 C16 C20 -64.2(7) . .
C14 N13 C16 C20 55.3(8) . .
C15 N13 C16 C20 173.7(6) . .
C16 N13 C17 C25 -175.1(5) . .
C14 N13 C17 C25 63.5(7) . .
C15 N13 C17 C25 -54.2(7) . .
N13 C15 C18 C27 172.3(7) . .
N13 C16 C20 C21 -173.0(6) . .
C16 C20 C21 C22 176.2(8) . .
N13 C14 C23 C24 172.9(7) . .
C14 C23 C24 C31 -176.2(12) . .
N13 C17 C25 C26 174.2(5) . .
C17 C25 C26 C30 171.8(7) . .
C15 C18 C27 C32 -68.9(10) . .
C37 C33 C34 C35 -172.9(10) . .
C38 N36 C37 C33 -175.9(8) . .
C39 N36 C37 C33 -55.5(10) . .
C41 N36 C37 C33 66.0(10) . .
C34 C33 C37 N36 177.7(8) . .
C37 N36 C38 C43 -178.7(8) . .
C39 N36 C38 C43 60.1(10) . .
C41 N36 C38 C43 -58.8(10) . .
C38 N36 C39 C40 59.6(10) . .
C37 N36 C39 C40 -58.4(10) . .
C41 N36 C39 C40 178.6(8) . .
N36 C39 C40 C46 175.6(9) . .
C38 N36 C41 C42 -56.2(14) . .
C37 N36 C41 C42 60.5(14) . .
C39 N36 C41 C42 -176.3(12) . .
N36 C41 C42 C48 -177.8(13) . .
N36 C38 C43 C44 -176.7(9) . .
C38 C43 C44 C45 -179.2(10) . .
C39 C40 C46 C47 178.8(13) . .
C41 C42 C48 C49 82.0(19) . .
O55 C52 C53 C54 2(4) . .
O55 C50 C54 C53 15(3) . .
C52 C53 C54 C50 -10(3) . .
C54 C50 O55 C52 -14(3) . .
C53 C52 O55 C50 7(4) . .
O9 MO3 O4 MO2 -67.7(3) . .
O10 MO3 O4 MO2 -175.3(3) . .
O3 MO3 O4 MO2 60.6(4) . .
O2 MO3 O4 MO2 18.4(2) 3_655 .
O1 MO3 O4 MO2 99.5(3) . .
