#------------------------------------------------------------------------------
#$Date: 2015-10-09 09:05:47 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161121 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/62/7036217.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_7036217
loop_
_publ_author_name
'Gorczyński, Adam'
'Kubicki, Maciej'
'Pinkowicz, Dawid'
'Pełka, Robert'
'Patroniak, Violetta'
'Podgajny, Robert'
_publ_section_title
;
 The first example of erbium triple-stranded helicates displaying SMM
 behaviour.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16833
_journal_page_last               16839
_journal_paper_doi               10.1039/c5dt02554k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C84 H87 N24 O3 Tm2, 3(N O3)'
_chemical_formula_sum            'C84 H87 N27 O12 Tm2'
_chemical_formula_weight         2004.66
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   26.1210(5)
_cell_length_b                   26.1210(5)
_cell_length_c                   47.7029(13)
_cell_measurement_reflns_used    14499
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.2040
_cell_measurement_theta_min      3.1890
_cell_volume                     28187.4(11)
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            32539
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.931
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       prism
_exptl_crystal_F_000             12168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.713
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0426
_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)+(0.0964P)²+3.9341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3653
_reflns_number_total             5515
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02554k3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7036214--7036219.cif.'
_cod_original_cell_volume        28187.4(13)
_cod_database_code               7036217
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Tm1 Tm 0.3333 0.6667 0.07417(2) 0.02834(17) Uani 1 3 d S T P
Tm2 Tm 0.3333 0.6667 0.00095(2) 0.02733(16) Uani 1 3 d S T P
N1 N 0.2460(2) 0.60996(18) 0.10383(10) 0.0404(11) Uani 1 1 d . . .
C2 C 0.1973(2) 0.6110(2) 0.09779(12) 0.0363(13) Uani 1 1 d . . .
N3 N 0.1476(2) 0.56370(19) 0.10736(11) 0.0437(12) Uani 1 1 d . . .
H3 H 0.1120 0.5566 0.1050 0.052 Uiso 1 1 calc R U .
C4 C 0.1647(2) 0.5289(2) 0.12158(12) 0.0446(14) Uani 1 1 d . . .
C5 C 0.1320(3) 0.4756(3) 0.13594(13) 0.0598(17) Uani 1 1 d . . .
H5 H 0.0909 0.4563 0.1364 0.072 Uiso 1 1 calc R U .
C6 C 0.1624(3) 0.4529(3) 0.14934(15) 0.071(2) Uani 1 1 d . . .
H6 H 0.1419 0.4172 0.1589 0.085 Uiso 1 1 calc R U .
C7 C 0.2246(4) 0.4832(3) 0.14874(15) 0.070(2) Uani 1 1 d . . .
H7 H 0.2445 0.4673 0.1583 0.083 Uiso 1 1 calc R U .
C8 C 0.2572(3) 0.5360(3) 0.13447(13) 0.0521(17) Uani 1 1 d . . .
H8 H 0.2983 0.5558 0.1344 0.063 Uiso 1 1 calc R U .
C9 C 0.2257(2) 0.5584(2) 0.12003(12) 0.0390(13) Uani 1 1 d . . .
N10 N 0.19575(18) 0.65450(18) 0.08281(10) 0.0424(11) Uani 1 1 d . . .
C10A C 0.1445(2) 0.6613(3) 0.08177(17) 0.079(2) Uani 1 1 d . . .
H10A H 0.1094 0.6232 0.0828 0.119 Uiso 1 1 calc R U .
H10B H 0.1444 0.6802 0.0645 0.119 Uiso 1 1 calc R U .
H10C H 0.1453 0.6852 0.0973 0.119 Uiso 1 1 calc R U .
N11 N 0.25071(17) 0.69709(18) 0.07236(9) 0.0352(10) Uani 1 1 d . . .
C12 C 0.2552(2) 0.7458(2) 0.06426(13) 0.0386(14) Uani 1 1 d . . .
H12 H 0.2229 0.7511 0.0668 0.046 Uiso 1 1 calc R U .
C13 C 0.3077(2) 0.7935(2) 0.05128(11) 0.0335(12) Uani 1 1 d . . .
C14 C 0.3493(2) 0.7818(2) 0.03764(11) 0.0311(11) Uani 1 1 d . . .
O14 O 0.34178(14) 0.72754(14) 0.03738(7) 0.0341(8) Uani 1 1 d . . .
C15 C 0.3980(2) 0.8283(2) 0.02401(12) 0.0344(12) Uani 1 1 d . . .
C16 C 0.4050(2) 0.8847(2) 0.02465(11) 0.0398(13) Uani 1 1 d . . .
H16 H 0.4383 0.9154 0.0162 0.048 Uiso 1 1 calc R U .
C17 C 0.3649(2) 0.8972(2) 0.03719(13) 0.0449(14) Uani 1 1 d . U .
C17A C 0.3735(3) 0.9598(2) 0.03763(15) 0.0636(16) Uani 1 1 d . U .
C17B C 0.4008(3) 0.9871(3) 0.06654(18) 0.098(2) Uani 1 1 d . U .
H17A H 0.4042 1.0254 0.0682 0.147 Uiso 1 1 calc R U .
H17B H 0.4392 0.9910 0.0681 0.147 Uiso 1 1 calc R U .
H17C H 0.3757 0.9619 0.0812 0.147 Uiso 1 1 calc R U .
C17C C 0.3177(3) 0.9602(3) 0.03441(19) 0.098(2) Uani 1 1 d . U .
H17D H 0.3255 1.0002 0.0347 0.148 Uiso 1 1 calc R U .
H17E H 0.2914 0.9384 0.0495 0.148 Uiso 1 1 calc R U .
H17F H 0.2996 0.9421 0.0169 0.148 Uiso 1 1 calc R U .
C17D C 0.4193(4) 1.0001(3) 0.0165(2) 0.128(3) Uani 1 1 d . U .
H17G H 0.4066 0.9845 -0.0020 0.192 Uiso 1 1 calc R U .
H17H H 0.4564 1.0024 0.0205 0.192 Uiso 1 1 calc R U .
H17I H 0.4239 1.0388 0.0176 0.192 Uiso 1 1 calc R U .
C18 C 0.3161(2) 0.8501(2) 0.05020(12) 0.0415(13) Uani 1 1 d . . .
H18 H 0.2880 0.8571 0.0585 0.050 Uiso 1 1 calc R U .
C19 C 0.4438(2) 0.8204(2) 0.01131(11) 0.0384(13) Uani 1 1 d . . .
H19 H 0.4811 0.8535 0.0090 0.046 Uiso 1 1 calc R U .
N20 N 0.43577(16) 0.76947(17) 0.00286(9) 0.0343(10) Uani 1 1 d . . .
N21 N 0.48460(17) 0.76793(19) -0.00703(10) 0.0434(12) Uani 1 1 d . . .
C21A C 0.5440(2) 0.8183(2) -0.00597(17) 0.074(2) Uani 1 1 d . . .
H21A H 0.5720 0.8052 -0.0089 0.111 Uiso 1 1 calc R U .
H21B H 0.5507 0.8370 0.0120 0.111 Uiso 1 1 calc R U .
H21C H 0.5486 0.8459 -0.0204 0.111 Uiso 1 1 calc R U .
N22 N 0.41656(18) 0.67616(18) -0.02839(9) 0.0406(11) Uani 1 1 d . . .
C23 C 0.4714(2) 0.7183(2) -0.02123(12) 0.0384(13) Uani 1 1 d . . .
N24 N 0.51386(18) 0.70704(18) -0.02983(10) 0.0448(12) Uani 1 1 d . . .
H24 H 0.5513 0.7290 -0.0272 0.054 Uiso 1 1 calc R U .
C25 C 0.4859(2) 0.6534(2) -0.04376(12) 0.0460(14) Uani 1 1 d . . .
C26 C 0.5090(3) 0.6210(3) -0.05664(14) 0.0574(17) Uani 1 1 d . . .
H26 H 0.5493 0.6339 -0.0567 0.069 Uiso 1 1 calc R U .
C27 C 0.4680(3) 0.5684(3) -0.06938(14) 0.0632(18) Uani 1 1 d . . .
H27 H 0.4807 0.5446 -0.0778 0.076 Uiso 1 1 calc R U .
C28 C 0.4088(3) 0.5511(3) -0.06976(14) 0.0619(18) Uani 1 1 d . . .
H28 H 0.3828 0.5161 -0.0789 0.074 Uiso 1 1 calc R U .
C29 C 0.3860(3) 0.5834(3) -0.05711(13) 0.0533(16) Uani 1 1 d . . .
H29 H 0.3458 0.5708 -0.0577 0.064 Uiso 1 1 calc R U .
C30 C 0.4260(2) 0.6355(2) -0.04344(12) 0.0410(13) Uani 1 1 d . . .
N1A N 0.4699(4) 0.4740(4) 0.12867(15) 0.081(2) Uani 1 1 d . . .
O1A O 0.5115(5) 0.5200(4) 0.1364(2) 0.181(4) Uani 1 1 d . . .
O2A O 0.4611(3) 0.4298(3) 0.14039(16) 0.129(3) Uani 1 1 d . . .
O3A O 0.4438(4) 0.4787(3) 0.10970(16) 0.146(3) 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 0.0033 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'
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
O14 Tm1 O14 68.25(12) . 2_665
O14 Tm1 O14 68.25(12) . 3_565
O14 Tm1 O14 68.25(12) 2_665 3_565
O14 Tm1 N1 126.53(13) . .
O14 Tm1 N1 85.60(13) 2_665 .
O14 Tm1 N1 143.06(12) 3_565 .
O14 Tm1 N1 85.60(13) . 3_565
O14 Tm1 N1 143.06(12) 2_665 3_565
O14 Tm1 N1 126.53(13) 3_565 3_565
N1 Tm1 N1 90.07(16) . 3_565
O14 Tm1 N1 143.06(12) . 2_665
O14 Tm1 N1 126.53(13) 2_665 2_665
O14 Tm1 N1 85.61(13) 3_565 2_665
N1 Tm1 N1 90.07(16) . 2_665
N1 Tm1 N1 90.07(16) 3_565 2_665
O14 Tm1 N11 65.11(12) . .
O14 Tm1 N11 74.32(12) 2_665 .
O14 Tm1 N11 128.08(12) 3_565 .
N1 Tm1 N11 63.17(14) . .
N1 Tm1 N11 71.07(13) 3_565 .
N1 Tm1 N11 146.31(15) 2_665 .
O14 Tm1 N11 74.32(12) . 3_565
O14 Tm1 N11 128.08(12) 2_665 3_565
O14 Tm1 N11 65.11(12) 3_565 3_565
N1 Tm1 N11 146.31(15) . 3_565
N1 Tm1 N11 63.17(14) 3_565 3_565
N1 Tm1 N11 71.07(13) 2_665 3_565
N11 Tm1 N11 119.896(11) . 3_565
O14 Tm1 N11 128.08(12) . 2_665
O14 Tm1 N11 65.11(12) 2_665 2_665
O14 Tm1 N11 74.32(12) 3_565 2_665
N1 Tm1 N11 71.07(13) . 2_665
N1 Tm1 N11 146.31(15) 3_565 2_665
N1 Tm1 N11 63.17(14) 2_665 2_665
N11 Tm1 N11 119.894(11) . 2_665
N11 Tm1 N11 119.895(11) 3_565 2_665
O14 Tm1 Tm2 40.37(8) . .
O14 Tm1 Tm2 40.37(8) 2_665 .
O14 Tm1 Tm2 40.37(8) 3_565 .
N1 Tm1 Tm2 125.21(11) . .
N1 Tm1 Tm2 125.21(11) 3_565 .
N1 Tm1 Tm2 125.21(11) 2_665 .
N11 Tm1 Tm2 88.14(9) . .
N11 Tm1 Tm2 88.14(9) 3_565 .
N11 Tm1 Tm2 88.14(9) 2_665 .
O14 Tm2 O14 68.69(13) 2_665 3_565
O14 Tm2 O14 68.69(13) 2_665 .
O14 Tm2 O14 68.69(13) 3_565 .
O14 Tm2 N22 125.50(13) 2_665 2_665
O14 Tm2 N22 142.75(12) 3_565 2_665
O14 Tm2 N22 84.36(13) . 2_665
O14 Tm2 N22 142.75(12) 2_665 .
O14 Tm2 N22 84.36(13) 3_565 .
O14 Tm2 N22 125.50(13) . .
N22 Tm2 N22 91.53(14) 2_665 .
O14 Tm2 N22 84.36(13) 2_665 3_565
O14 Tm2 N22 125.50(13) 3_565 3_565
O14 Tm2 N22 142.76(12) . 3_565
N22 Tm2 N22 91.53(14) 2_665 3_565
N22 Tm2 N22 91.53(14) . 3_565
O14 Tm2 N20 65.01(11) 2_665 2_665
O14 Tm2 N20 128.29(12) 3_565 2_665
O14 Tm2 N20 74.06(12) . 2_665
N22 Tm2 N20 62.32(13) 2_665 2_665
N22 Tm2 N20 147.32(14) . 2_665
N22 Tm2 N20 71.35(12) 3_565 2_665
O14 Tm2 N20 74.06(12) 2_665 3_565
O14 Tm2 N20 65.01(11) 3_565 3_565
O14 Tm2 N20 128.29(12) . 3_565
N22 Tm2 N20 147.32(14) 2_665 3_565
N22 Tm2 N20 71.35(12) . 3_565
N22 Tm2 N20 62.31(13) 3_565 3_565
N20 Tm2 N20 119.885(11) 2_665 3_565
O14 Tm2 N20 128.29(12) 2_665 .
O14 Tm2 N20 74.06(12) 3_565 .
O14 Tm2 N20 65.01(11) . .
N22 Tm2 N20 71.35(12) 2_665 .
N22 Tm2 N20 62.32(13) . .
N22 Tm2 N20 147.32(14) 3_565 .
N20 Tm2 N20 119.884(11) 2_665 .
N20 Tm2 N20 119.886(11) 3_565 .
O14 Tm2 Tm1 40.65(8) 2_665 .
O14 Tm2 Tm1 40.65(8) 3_565 .
O14 Tm2 Tm1 40.65(8) . .
N22 Tm2 Tm1 124.18(10) 2_665 .
N22 Tm2 Tm1 124.18(10) . .
N22 Tm2 Tm1 124.17(10) 3_565 .
N20 Tm2 Tm1 88.05(9) 2_665 .
N20 Tm2 Tm1 88.05(9) 3_565 .
N20 Tm2 Tm1 88.05(9) . .
C2 N1 C9 103.6(4) . .
C2 N1 Tm1 118.5(4) . .
C9 N1 Tm1 133.3(3) . .
N1 C2 N3 113.8(5) . .
N1 C2 N10 124.4(5) . .
N3 C2 N10 121.8(5) . .
C2 N3 C4 106.9(5) . .
C2 N3 H3 126.6 . .
C4 N3 H3 126.6 . .
N3 C4 C5 131.4(5) . .
N3 C4 C9 105.7(4) . .
C5 C4 C9 122.9(5) . .
C6 C5 C4 117.7(6) . .
C6 C5 H5 121.2 . .
C4 C5 H5 121.2 . .
C5 C6 C7 120.3(6) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C8 C7 C6 122.3(6) . .
C8 C7 H7 118.9 . .
C6 C7 H7 118.9 . .
C7 C8 C9 117.2(6) . .
C7 C8 H8 121.4 . .
C9 C8 H8 121.4 . .
C4 C9 C8 119.6(5) . .
C4 C9 N1 110.0(5) . .
C8 C9 N1 130.4(5) . .
C2 N10 N11 113.9(4) . .
C2 N10 C10A 122.7(4) . .
N11 N10 C10A 122.6(4) . .
N10 C10A H10A 109.5 . .
N10 C10A H10B 109.5 . .
H10A C10A H10B 109.5 . .
N10 C10A H10C 109.5 . .
H10A C10A H10C 109.5 . .
H10B C10A H10C 109.5 . .
C12 N11 N10 116.6(4) . .
C12 N11 Tm1 128.7(3) . .
N10 N11 Tm1 114.6(3) . .
N11 C12 C13 124.1(5) . .
N11 C12 H12 117.9 . .
C13 C12 H12 117.9 . .
C18 C13 C14 118.9(4) . .
C18 C13 C12 120.7(5) . .
C14 C13 C12 120.3(4) . .
O14 C14 C15 120.3(4) . .
O14 C14 C13 120.7(4) . .
C15 C14 C13 119.0(4) . .
C14 O14 Tm2 131.2(3) . .
C14 O14 Tm1 129.8(3) . .
Tm2 O14 Tm1 98.98(12) . .
C16 C15 C14 119.2(5) . .
C16 C15 C19 118.7(5) . .
C14 C15 C19 121.9(4) . .
C17 C16 C15 123.2(5) . .
C17 C16 H16 118.4 . .
C15 C16 H16 118.4 . .
C16 C17 C18 116.7(4) . .
C16 C17 C17A 122.2(5) . .
C18 C17 C17A 121.1(5) . .
C17C C17A C17D 111.5(6) . .
C17C C17A C17 112.7(5) . .
C17D C17A C17 112.1(5) . .
C17C C17A C17B 108.5(6) . .
C17D C17A C17B 104.5(6) . .
C17 C17A C17B 107.0(5) . .
C17A C17B H17A 109.5 . .
C17A C17B H17B 109.5 . .
H17A C17B H17B 109.5 . .
C17A C17B H17C 109.5 . .
H17A C17B H17C 109.5 . .
H17B C17B H17C 109.5 . .
C17A C17C H17D 109.5 . .
C17A C17C H17E 109.5 . .
H17D C17C H17E 109.5 . .
C17A C17C H17F 109.5 . .
H17D C17C H17F 109.5 . .
H17E C17C H17F 109.5 . .
C17A C17D H17G 109.5 . .
C17A C17D H17H 109.5 . .
H17G C17D H17H 109.5 . .
C17A C17D H17I 109.5 . .
H17G C17D H17I 109.5 . .
H17H C17D H17I 109.5 . .
C13 C18 C17 123.0(5) . .
C13 C18 H18 118.5 . .
C17 C18 H18 118.5 . .
N20 C19 C15 123.6(4) . .
N20 C19 H19 118.2 . .
C15 C19 H19 118.2 . .
C19 N20 N21 117.1(4) . .
C19 N20 Tm2 127.1(3) . .
N21 N20 Tm2 115.7(3) . .
C23 N21 N20 113.8(4) . .
C23 N21 C21A 122.3(4) . .
N20 N21 C21A 123.2(4) . .
N21 C21A H21A 109.5 . .
N21 C21A H21B 109.5 . .
H21A C21A H21B 109.5 . .
N21 C21A H21C 109.5 . .
H21A C21A H21C 109.5 . .
H21B C21A H21C 109.5 . .
C23 N22 C30 103.4(4) . .
C23 N22 Tm2 117.3(3) . .
C30 N22 Tm2 133.5(3) . .
N22 C23 N21 125.0(5) . .
N22 C23 N24 113.6(5) . .
N21 C23 N24 121.4(5) . .
C23 N24 C25 107.0(4) . .
C23 N24 H24 126.5 . .
C25 N24 H24 126.5 . .
N24 C25 C30 105.7(4) . .
N24 C25 C26 130.7(5) . .
C30 C25 C26 123.6(5) . .
C27 C26 C25 115.8(5) . .
C27 C26 H26 122.1 . .
C25 C26 H26 122.1 . .
C26 C27 C28 121.0(6) . .
C26 C27 H27 119.5 . .
C28 C27 H27 119.5 . .
C27 C28 C29 123.1(6) . .
C27 C28 H28 118.4 . .
C29 C28 H28 118.4 . .
C30 C29 C28 117.0(6) . .
C30 C29 H29 121.5 . .
C28 C29 H29 121.5 . .
C25 C30 C29 119.4(5) . .
C25 C30 N22 110.2(5) . .
C29 C30 N22 130.3(5) . .
O3A N1A O2A 128.2(10) . .
O3A N1A O1A 114.3(9) . .
O2A N1A O1A 117.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 O14 2.304(3) .
Tm1 O14 2.304(3) 2_665
Tm1 O14 2.304(3) 3_565
Tm1 N1 2.454(4) .
Tm1 N1 2.454(4) 3_565
Tm1 N1 2.454(4) 2_665
Tm1 N11 2.648(4) .
Tm1 N11 2.648(4) 3_565
Tm1 N11 2.648(4) 2_665
Tm1 Tm2 3.4927(5) .
Tm2 O14 2.290(3) 2_665
Tm2 O14 2.290(3) 3_565
Tm2 O14 2.290(3) .
Tm2 N22 2.491(4) 2_665
Tm2 N22 2.491(4) .
Tm2 N22 2.491(4) 3_565
Tm2 N20 2.682(4) 2_665
Tm2 N20 2.682(4) 3_565
Tm2 N20 2.682(4) .
N1 C2 1.319(7) .
N1 C9 1.407(6) .
C2 N3 1.348(7) .
C2 N10 1.359(7) .
N3 C4 1.378(7) .
N3 H3 0.8600 .
C4 C5 1.395(7) .
C4 C9 1.381(7) .
C5 C6 1.364(8) .
C5 H5 0.9300 .
C6 C7 1.408(9) .
C6 H6 0.9300 .
C7 C8 1.383(9) .
C7 H7 0.9300 .
C8 C9 1.407(8) .
C8 H8 0.9300 .
N10 N11 1.396(5) .
N10 C10A 1.438(6) .
C10A H10A 0.9600 .
C10A H10B 0.9600 .
C10A H10C 0.9600 .
N11 C12 1.278(7) .
C12 C13 1.452(7) .
C12 H12 0.9300 .
C13 C18 1.383(6) .
C13 C14 1.425(7) .
C14 O14 1.330(5) .
C14 C15 1.403(7) .
C15 C16 1.392(7) .
C15 C19 1.445(7) .
C16 C17 1.381(7) .
C16 H16 0.9300 .
C17 C18 1.398(7) .
C17 C17A 1.535(7) .
C17A C17C 1.473(9) .
C17A C17D 1.515(10) .
C17A C17B 1.552(9) .
C17B H17A 0.9600 .
C17B H17B 0.9600 .
C17B H17C 0.9600 .
C17C H17D 0.9600 .
C17C H17E 0.9600 .
C17C H17F 0.9600 .
C17D H17G 0.9600 .
C17D H17H 0.9600 .
C17D H17I 0.9600 .
C18 H18 0.9300 .
C19 N20 1.302(6) .
C19 H19 0.9300 .
N20 N21 1.379(5) .
N21 C23 1.345(7) .
N21 C21A 1.448(6) .
C21A H21A 0.9600 .
C21A H21B 0.9600 .
C21A H21C 0.9600 .
N22 C23 1.343(7) .
N22 C30 1.403(6) .
C23 N24 1.348(6) .
N24 C25 1.384(6) .
N24 H24 0.8600 .
C25 C30 1.389(7) .
C25 C26 1.404(7) .
C26 C27 1.390(9) .
C26 H26 0.9300 .
C27 C28 1.378(9) .
C27 H27 0.9300 .
C28 C29 1.390(8) .
C28 H28 0.9300 .
C29 C30 1.397(8) .
C29 H29 0.9300 .
N1A O3A 1.175(8) .
N1A O2A 1.199(8) .
N1A O1A 1.206(12) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O3A 0.86 2.02 2.853(8) 162.7 3_565
C10A H10A O3A 0.96 2.26 3.106(9) 147.2 3_565
C21A H21A O1A 0.96 2.55 3.286(9) 133.5 29
C21A H21A O2A 0.96 2.54 3.485(8) 168.1 29
N24 H24 O2A 0.86 1.91 2.755(7) 166.1 29
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
C9 N1 C2 N3 -3.1(6)
Tm1 N1 C2 N3 156.0(4)
C9 N1 C2 N10 178.3(5)
Tm1 N1 C2 N10 -22.6(7)
N1 C2 N3 C4 1.6(7)
N10 C2 N3 C4 -179.8(5)
C2 N3 C4 C5 178.9(6)
C2 N3 C4 C9 0.7(6)
N3 C4 C5 C6 -176.7(6)
C9 C4 C5 C6 1.2(10)
C4 C5 C6 C7 0.8(11)
C5 C6 C7 C8 -1.0(12)
C6 C7 C8 C9 -0.8(11)
N3 C4 C9 C8 175.3(5)
C5 C4 C9 C8 -3.0(9)
N3 C4 C9 N1 -2.6(6)
C5 C4 C9 N1 179.0(5)
C7 C8 C9 C4 2.7(9)
C7 C8 C9 N1 -179.8(6)
C2 N1 C9 C4 3.5(6)
Tm1 N1 C9 C4 -151.0(4)
C2 N1 C9 C8 -174.2(6)
Tm1 N1 C9 C8 31.3(9)
N1 C2 N10 N11 4.3(8)
N3 C2 N10 N11 -174.2(5)
N1 C2 N10 C10A -166.0(6)
N3 C2 N10 C10A 15.5(9)
C2 N10 N11 C12 -163.3(5)
C10A N10 N11 C12 6.9(8)
C2 N10 N11 Tm1 14.2(5)
C10A N10 N11 Tm1 -175.6(5)
N10 N11 C12 C13 -176.1(5)
Tm1 N11 C12 C13 6.8(8)
N11 C12 C13 C18 -161.8(6)
N11 C12 C13 C14 22.9(9)
C18 C13 C14 O14 -177.7(5)
C12 C13 C14 O14 -2.2(8)
C18 C13 C14 C15 1.2(8)
C12 C13 C14 C15 176.7(5)
C15 C14 O14 Tm2 -57.2(6)
C13 C14 O14 Tm2 121.7(5)
C15 C14 O14 Tm1 122.8(5)
C13 C14 O14 Tm1 -58.3(6)
O14 C14 C15 C16 -179.9(5)
C13 C14 C15 C16 1.2(8)
O14 C14 C15 C19 -5.1(8)
C13 C14 C15 C19 176.0(5)
C14 C15 C16 C17 -2.7(9)
C19 C15 C16 C17 -177.6(5)
C15 C16 C17 C18 1.4(9)
C15 C16 C17 C17A 180.0(6)
C16 C17 C17A C17C 142.9(7)
C18 C17 C17A C17C -38.6(9)
C16 C17 C17A C17D 16.1(10)
C18 C17 C17A C17D -165.4(7)
C16 C17 C17A C17B -97.9(7)
C18 C17 C17A C17B 80.6(7)
C14 C13 C18 C17 -2.5(8)
C12 C13 C18 C17 -177.9(5)
C16 C17 C18 C13 1.2(9)
C17A C17 C18 C13 -177.3(5)
C16 C15 C19 N20 -161.1(5)
C14 C15 C19 N20 24.1(9)
C15 C19 N20 N21 -175.4(5)
C15 C19 N20 Tm2 6.7(8)
C19 N20 N21 C23 -165.4(5)
Tm2 N20 N21 C23 12.8(6)
C19 N20 N21 C21A 5.9(8)
Tm2 N20 N21 C21A -176.0(5)
C30 N22 C23 N21 178.1(5)
Tm2 N22 C23 N21 -25.2(7)
C30 N22 C23 N24 -1.5(6)
Tm2 N22 C23 N24 155.2(4)
N20 N21 C23 N22 7.2(8)
C21A N21 C23 N22 -164.1(6)
N20 N21 C23 N24 -173.1(5)
C21A N21 C23 N24 15.5(9)
N22 C23 N24 C25 -0.1(6)
N21 C23 N24 C25 -179.7(5)
C23 N24 C25 C30 1.7(6)
C23 N24 C25 C26 -179.5(6)
N24 C25 C26 C27 -178.9(6)
C30 C25 C26 C27 -0.3(9)
C25 C26 C27 C28 1.9(10)
C26 C27 C28 C29 -1.7(11)
C27 C28 C29 C30 -0.2(11)
N24 C25 C30 C29 177.3(5)
C26 C25 C30 C29 -1.6(9)
N24 C25 C30 N22 -2.7(6)
C26 C25 C30 N22 178.4(5)
C28 C29 C30 C25 1.8(9)
C28 C29 C30 N22 -178.2(6)
C23 N22 C30 C25 2.6(6)
Tm2 N22 C30 C25 -148.5(4)
C23 N22 C30 C29 -177.4(6)
Tm2 N22 C30 C29 31.6(9)
