#------------------------------------------------------------------------------
#$Date: 2015-10-09 09:05:47 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161121 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/62/7036216.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_7036216
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 Ho2 N24 O3, 3(N O3)'
_chemical_formula_sum            'C84 H87 Ho2 N27 O12'
_chemical_formula_weight         1996.66
_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                   26.1368(10)
_cell_length_b                   26.1368(10)
_cell_length_c                   48.150(2)
_cell_measurement_reflns_used    2769
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.4380
_cell_measurement_theta_min      3.1740
_cell_volume                     28486.0(19)
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0684
_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       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            18209
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.921
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             12120
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0408
_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)+(0.0419P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2877
_reflns_number_total             5577
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02554k3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7036214--7036219.cif.'
_cod_original_cell_volume        28486(2)
_cod_database_code               7036216
_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
Ho1 Ho 0.3333 0.6667 0.07324(2) 0.03784(13) Uani 1 3 d S T P
Ho2 Ho 0.3333 0.6667 0.00017(2) 0.03486(13) Uani 1 3 d S T P
N1 N 0.2452(2) 0.6108(2) 0.10315(9) 0.0490(13) Uani 1 1 d . . .
C2 C 0.1967(3) 0.6129(3) 0.09699(12) 0.0480(17) Uani 1 1 d . . .
N3 N 0.1470(2) 0.5662(2) 0.10669(9) 0.0522(13) Uani 1 1 d . . .
H3 H 0.1116 0.5594 0.1043 0.063 Uiso 1 1 calc R U .
C4 C 0.1635(3) 0.5318(3) 0.12117(13) 0.0561(17) Uani 1 1 d . . .
C5 C 0.1301(3) 0.4796(3) 0.13538(13) 0.0686(19) Uani 1 1 d . . .
H5 H 0.0891 0.4603 0.1357 0.082 Uiso 1 1 calc R U .
C6 C 0.1617(4) 0.4576(3) 0.14909(15) 0.086(2) Uani 1 1 d . . .
H6 H 0.1411 0.4227 0.1591 0.104 Uiso 1 1 calc R U .
C7 C 0.2232(4) 0.4857(3) 0.14850(14) 0.081(2) Uani 1 1 d . . .
H7 H 0.2428 0.4697 0.1581 0.097 Uiso 1 1 calc R U .
C8 C 0.2550(3) 0.5376(3) 0.13364(13) 0.066(2) Uani 1 1 d . . .
H8 H 0.2961 0.5569 0.1332 0.079 Uiso 1 1 calc R U .
C9 C 0.2248(3) 0.5601(3) 0.11957(12) 0.0529(17) Uani 1 1 d . . .
N10 N 0.1962(2) 0.6561(2) 0.08168(10) 0.0516(13) Uani 1 1 d . . .
C10A C 0.1441(3) 0.6621(3) 0.07926(16) 0.097(3) Uani 1 1 d . . .
H10A H 0.1093 0.6241 0.0818 0.146 Uiso 1 1 calc R U .
H10B H 0.1432 0.6771 0.0612 0.146 Uiso 1 1 calc R U .
H10C H 0.1452 0.6889 0.0932 0.146 Uiso 1 1 calc R U .
N11 N 0.25101(19) 0.6979(2) 0.07150(9) 0.0443(12) Uani 1 1 d . . .
C12 C 0.2560(3) 0.7469(3) 0.06341(11) 0.0495(14) Uani 1 1 d . . .
H12 H 0.2241 0.7529 0.0659 0.059 Uiso 1 1 calc R U .
C13 C 0.3096(2) 0.7940(2) 0.05043(11) 0.0407(14) Uani 1 1 d . . .
C14 C 0.3502(2) 0.7821(2) 0.03695(11) 0.0389(14) Uani 1 1 d . . .
O14 O 0.34194(14) 0.72771(15) 0.03653(6) 0.0382(9) Uani 1 1 d . . .
C15 C 0.3986(2) 0.8284(2) 0.02355(11) 0.0391(14) Uani 1 1 d . . .
C16 C 0.4071(3) 0.8854(2) 0.02440(11) 0.0483(15) Uani 1 1 d . . .
H16 H 0.4407 0.9160 0.0161 0.058 Uiso 1 1 calc R U .
C17 C 0.3673(3) 0.8981(3) 0.03716(12) 0.0528(16) Uani 1 1 d . U .
C17A C 0.3770(3) 0.9612(3) 0.03836(16) 0.076(2) Uani 1 1 d . U .
C17B C 0.3985(4) 0.9851(3) 0.06762(18) 0.117(3) Uani 1 1 d . U .
H17A H 0.4049 1.0245 0.0690 0.175 Uiso 1 1 calc R U .
H17B H 0.4349 0.9857 0.0713 0.175 Uiso 1 1 calc R U .
H17C H 0.3694 0.9602 0.0810 0.175 Uiso 1 1 calc R U .
C17C C 0.3221(3) 0.9629(3) 0.03346(18) 0.118(3) Uani 1 1 d . U .
H17D H 0.3288 1.0018 0.0376 0.178 Uiso 1 1 calc R U .
H17E H 0.2914 0.9346 0.0453 0.178 Uiso 1 1 calc R U .
H17F H 0.3105 0.9536 0.0144 0.178 Uiso 1 1 calc R U .
C17D C 0.4241(4) 1.0026(3) 0.01840(18) 0.126(3) Uani 1 1 d . U .
H17G H 0.4144 0.9865 0.0000 0.189 Uiso 1 1 calc R U .
H17H H 0.4616 1.0073 0.0238 0.189 Uiso 1 1 calc R U .
H17I H 0.4262 1.0403 0.0188 0.189 Uiso 1 1 calc R U .
C18 C 0.3183(3) 0.8511(2) 0.04980(11) 0.0517(16) Uani 1 1 d . . .
H18 H 0.2904 0.8582 0.0582 0.062 Uiso 1 1 calc R U .
C19 C 0.4437(2) 0.8197(2) 0.01054(11) 0.0447(15) Uani 1 1 d . . .
H19 H 0.4809 0.8527 0.0079 0.054 Uiso 1 1 calc R U .
N20 N 0.43580(18) 0.76928(19) 0.00240(9) 0.0401(11) Uani 1 1 d . . .
N21 N 0.4844(2) 0.7680(2) -0.00806(10) 0.0511(14) Uani 1 1 d . . .
C21A C 0.5434(3) 0.8194(3) -0.00773(16) 0.094(3) Uani 1 1 d . . .
H21A H 0.5718 0.8075 -0.0121 0.141 Uiso 1 1 calc R U .
H21B H 0.5516 0.8371 0.0104 0.141 Uiso 1 1 calc R U .
H21C H 0.5458 0.8475 -0.0212 0.141 Uiso 1 1 calc R U .
N22 N 0.4164(2) 0.6761(2) -0.02933(9) 0.0471(12) Uani 1 1 d . . .
C23 C 0.4713(3) 0.7180(3) -0.02201(12) 0.0445(15) Uani 1 1 d . . .
N24 N 0.5139(2) 0.7062(2) -0.03038(9) 0.0519(13) Uani 1 1 d . . .
H24 H 0.5513 0.7280 -0.0276 0.062 Uiso 1 1 calc R U .
C25 C 0.4862(3) 0.6528(3) -0.04412(12) 0.0500(16) Uani 1 1 d . . .
C26 C 0.5090(3) 0.6209(3) -0.05625(13) 0.0621(18) Uani 1 1 d . . .
H26 H 0.5491 0.6333 -0.0556 0.074 Uiso 1 1 calc R U .
C27 C 0.4695(3) 0.5699(3) -0.06927(13) 0.070(2) Uani 1 1 d . . .
H27 H 0.4829 0.5469 -0.0778 0.084 Uiso 1 1 calc R U .
C28 C 0.4096(4) 0.5517(3) -0.06999(13) 0.072(2) Uani 1 1 d . . .
H28 H 0.3840 0.5169 -0.0792 0.087 Uiso 1 1 calc R U .
C29 C 0.3866(3) 0.5838(3) -0.05729(12) 0.0576(18) Uani 1 1 d . . .
H29 H 0.3465 0.5714 -0.0579 0.069 Uiso 1 1 calc R U .
C30 C 0.4266(3) 0.6353(3) -0.04373(11) 0.0417(14) Uani 1 1 d . . .
N1A N 0.4648(4) 0.4687(4) 0.12781(17) 0.094(2) Uani 1 1 d . . .
O1A O 0.5072(4) 0.5144(4) 0.13353(19) 0.182(4) Uani 1 1 d . . .
O2A O 0.4582(3) 0.4267(3) 0.14010(14) 0.135(3) Uani 1 1 d . . .
O3A O 0.4351(4) 0.4734(3) 0.11115(16) 0.171(4) 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'
Ho Ho -0.2175 4.6783 '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 Ho1 O14 68.03(13) . 2_665
O14 Ho1 O14 68.03(13) . 3_565
O14 Ho1 O14 68.03(13) 2_665 3_565
O14 Ho1 N1 86.14(14) . 3_565
O14 Ho1 N1 143.79(13) 2_665 3_565
O14 Ho1 N1 126.21(13) 3_565 3_565
O14 Ho1 N1 126.21(13) . .
O14 Ho1 N1 86.14(14) 2_665 .
O14 Ho1 N1 143.79(13) 3_565 .
N1 Ho1 N1 89.65(15) 3_565 .
O14 Ho1 N1 143.79(13) . 2_665
O14 Ho1 N1 126.21(13) 2_665 2_665
O14 Ho1 N1 86.14(14) 3_565 2_665
N1 Ho1 N1 89.65(15) 3_565 2_665
N1 Ho1 N1 89.65(15) . 2_665
O14 Ho1 N11 65.10(13) . .
O14 Ho1 N11 74.54(13) 2_665 .
O14 Ho1 N11 127.98(13) 3_565 .
N1 Ho1 N11 71.62(14) 3_565 .
N1 Ho1 N11 62.78(14) . .
N1 Ho1 N11 145.87(15) 2_665 .
O14 Ho1 N11 74.54(13) . 3_565
O14 Ho1 N11 127.98(13) 2_665 3_565
O14 Ho1 N11 65.10(13) 3_565 3_565
N1 Ho1 N11 62.78(14) 3_565 3_565
N1 Ho1 N11 145.87(15) . 3_565
N1 Ho1 N11 71.62(14) 2_665 3_565
N11 Ho1 N11 119.900(11) . 3_565
O14 Ho1 N11 127.98(13) . 2_665
O14 Ho1 N11 65.10(13) 2_665 2_665
O14 Ho1 N11 74.54(13) 3_565 2_665
N1 Ho1 N11 145.87(15) 3_565 2_665
N1 Ho1 N11 71.62(14) . 2_665
N1 Ho1 N11 62.78(14) 2_665 2_665
N11 Ho1 N11 119.903(11) . 2_665
N11 Ho1 N11 119.901(11) 3_565 2_665
O14 Ho1 Ho2 40.24(8) . .
O14 Ho1 Ho2 40.24(8) 2_665 .
O14 Ho1 Ho2 40.24(8) 3_565 .
N1 Ho1 Ho2 125.51(11) 3_565 .
N1 Ho1 Ho2 125.51(11) . .
N1 Ho1 Ho2 125.51(11) 2_665 .
N11 Ho1 Ho2 88.19(10) . .
N11 Ho1 Ho2 88.19(10) 3_565 .
N11 Ho1 Ho2 88.19(10) 2_665 .
O14 Ho2 O14 68.47(13) 2_665 3_565
O14 Ho2 O14 68.47(13) 2_665 .
O14 Ho2 O14 68.47(13) 3_565 .
O14 Ho2 N22 143.05(13) 2_665 .
O14 Ho2 N22 84.93(14) 3_565 .
O14 Ho2 N22 125.76(13) . .
O14 Ho2 N22 125.76(13) 2_665 2_665
O14 Ho2 N22 143.05(13) 3_565 2_665
O14 Ho2 N22 84.93(14) . 2_665
N22 Ho2 N22 90.94(15) . 2_665
O14 Ho2 N22 84.93(14) 2_665 3_565
O14 Ho2 N22 125.76(13) 3_565 3_565
O14 Ho2 N22 143.05(13) . 3_565
N22 Ho2 N22 90.94(15) . 3_565
N22 Ho2 N22 90.94(15) 2_665 3_565
O14 Ho2 N20 64.78(12) 2_665 2_665
O14 Ho2 N20 127.80(12) 3_565 2_665
O14 Ho2 N20 73.84(12) . 2_665
N22 Ho2 N20 147.25(14) . 2_665
N22 Ho2 N20 62.68(14) 2_665 2_665
N22 Ho2 N20 71.72(14) 3_565 2_665
O14 Ho2 N20 127.80(12) 2_665 .
O14 Ho2 N20 73.84(12) 3_565 .
O14 Ho2 N20 64.78(12) . .
N22 Ho2 N20 62.68(14) . .
N22 Ho2 N20 71.72(14) 2_665 .
N22 Ho2 N20 147.24(14) 3_565 .
N20 Ho2 N20 119.841(13) 2_665 .
O14 Ho2 N20 73.84(12) 2_665 3_565
O14 Ho2 N20 64.78(12) 3_565 3_565
O14 Ho2 N20 127.80(12) . 3_565
N22 Ho2 N20 71.72(14) . 3_565
N22 Ho2 N20 147.24(14) 2_665 3_565
N22 Ho2 N20 62.68(14) 3_565 3_565
N20 Ho2 N20 119.840(13) 2_665 3_565
N20 Ho2 N20 119.840(13) . 3_565
O14 Ho2 Ho1 40.51(8) 2_665 .
O14 Ho2 Ho1 40.51(8) 3_565 .
O14 Ho2 Ho1 40.51(8) . .
N22 Ho2 Ho1 124.60(10) . .
N22 Ho2 Ho1 124.60(10) 2_665 .
N22 Ho2 Ho1 124.60(10) 3_565 .
N20 Ho2 Ho1 87.70(9) 2_665 .
N20 Ho2 Ho1 87.70(9) . .
N20 Ho2 Ho1 87.70(9) 3_565 .
C2 N1 C9 104.3(5) . .
C2 N1 Ho1 118.0(4) . .
C9 N1 Ho1 133.4(4) . .
N1 C2 N3 113.2(5) . .
N1 C2 N10 124.3(5) . .
N3 C2 N10 122.5(6) . .
C2 N3 C4 107.1(5) . .
C2 N3 H3 126.4 . .
C4 N3 H3 126.4 . .
N3 C4 C5 130.7(6) . .
N3 C4 C9 106.2(6) . .
C5 C4 C9 123.1(7) . .
C4 C5 C6 115.6(7) . .
C4 C5 H5 122.2 . .
C6 C5 H5 122.2 . .
C5 C6 C7 122.7(7) . .
C5 C6 H6 118.6 . .
C7 C6 H6 118.6 . .
C8 C7 C6 119.9(7) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C9 C8 C7 118.8(7) . .
C9 C8 H8 120.6 . .
C7 C8 H8 120.6 . .
C8 C9 C4 119.9(6) . .
C8 C9 N1 131.0(6) . .
C4 C9 N1 109.1(6) . .
C2 N10 N11 114.3(5) . .
C2 N10 C10A 122.3(5) . .
N11 N10 C10A 123.0(5) . .
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 116.3(5) . .
C12 N11 Ho1 128.5(4) . .
N10 N11 Ho1 115.1(3) . .
N11 C12 C13 123.2(5) . .
N11 C12 H12 118.4 . .
C13 C12 H12 118.4 . .
C18 C13 C14 119.3(5) . .
C18 C13 C12 119.1(5) . .
C14 C13 C12 121.4(5) . .
O14 C14 C15 120.8(5) . .
O14 C14 C13 120.5(5) . .
C15 C14 C13 118.6(5) . .
C14 O14 Ho2 131.4(3) . .
C14 O14 Ho1 129.4(3) . .
Ho2 O14 Ho1 99.25(13) . .
C16 C15 C14 120.2(5) . .
C16 C15 C19 118.2(5) . .
C14 C15 C19 121.3(5) . .
C17 C16 C15 122.1(5) . .
C17 C16 H16 118.9 . .
C15 C16 H16 118.9 . .
C16 C17 C18 116.9(5) . .
C16 C17 C17A 122.1(5) . .
C18 C17 C17A 121.0(5) . .
C17C C17A C17D 109.4(7) . .
C17C C17A C17B 107.4(6) . .
C17D C17A C17B 106.9(7) . .
C17C C17A C17 112.6(6) . .
C17D C17A C17 112.5(6) . .
C17B C17A C17 107.6(6) . .
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 122.7(5) . .
C13 C18 H18 118.6 . .
C17 C18 H18 118.6 . .
N20 C19 C15 124.3(5) . .
N20 C19 H19 117.8 . .
C15 C19 H19 117.8 . .
C19 N20 N21 117.1(5) . .
C19 N20 Ho2 127.2(4) . .
N21 N20 Ho2 115.5(3) . .
C23 N21 N20 114.3(5) . .
C23 N21 C21A 122.6(5) . .
N20 N21 C21A 122.4(5) . .
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 102.5(5) . .
C23 N22 Ho2 116.8(3) . .
C30 N22 Ho2 133.7(4) . .
N22 C23 N21 124.7(5) . .
N22 C23 N24 113.6(5) . .
N21 C23 N24 121.7(6) . .
C23 N24 C25 107.3(5) . .
C23 N24 H24 126.3 . .
C25 N24 H24 126.3 . .
N24 C25 C26 130.7(6) . .
N24 C25 C30 105.2(5) . .
C26 C25 C30 124.1(6) . .
C27 C26 C25 116.3(6) . .
C27 C26 H26 121.8 . .
C25 C26 H26 121.8 . .
C26 C27 C28 121.2(6) . .
C26 C27 H27 119.4 . .
C28 C27 H27 119.4 . .
C27 C28 C29 122.3(6) . .
C27 C28 H28 118.9 . .
C29 C28 H28 118.9 . .
C30 C29 C28 116.5(6) . .
C30 C29 H29 121.8 . .
C28 C29 H29 121.8 . .
C29 C30 C25 119.5(5) . .
C29 C30 N22 129.1(6) . .
C25 C30 N22 111.4(5) . .
O3A N1A O2A 130.4(11) . .
O3A N1A O1A 113.0(10) . .
O2A N1A O1A 116.6(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O14 2.315(3) .
Ho1 O14 2.316(3) 2_665
Ho1 O14 2.316(3) 3_565
Ho1 N1 2.480(4) 3_565
Ho1 N1 2.480(4) .
Ho1 N1 2.480(4) 2_665
Ho1 N11 2.656(5) .
Ho1 N11 2.656(5) 3_565
Ho1 N11 2.656(5) 2_665
Ho1 Ho2 3.5182(5) .
Ho2 O14 2.303(3) 2_665
Ho2 O14 2.303(3) 3_565
Ho2 O14 2.303(3) .
Ho2 N22 2.501(4) .
Ho2 N22 2.501(4) 2_665
Ho2 N22 2.501(4) 3_565
Ho2 N20 2.682(4) 2_665
Ho2 N20 2.682(4) .
Ho2 N20 2.682(4) 3_565
N1 C2 1.328(7) .
N1 C9 1.399(7) .
C2 N3 1.345(7) .
C2 N10 1.355(7) .
N3 C4 1.368(7) .
N3 H3 0.8600 .
C4 C5 1.379(8) .
C4 C9 1.391(8) .
C5 C6 1.386(9) .
C5 H5 0.9300 .
C6 C7 1.393(9) .
C6 H6 0.9300 .
C7 C8 1.384(8) .
C7 H7 0.9300 .
C8 C9 1.376(8) .
C8 H8 0.9300 .
N10 N11 1.386(6) .
N10 C10A 1.451(7) .
C10A H10A 0.9600 .
C10A H10B 0.9600 .
C10A H10C 0.9600 .
N11 C12 1.283(7) .
C12 C13 1.463(7) .
C12 H12 0.9300 .
C13 C18 1.393(7) .
C13 C14 1.407(7) .
C14 O14 1.327(6) .
C14 C15 1.396(7) .
C15 C16 1.394(7) .
C15 C19 1.450(7) .
C16 C17 1.385(7) .
C16 H16 0.9300 .
C17 C18 1.393(7) .
C17 C17A 1.539(8) .
C17A C17C 1.477(8) .
C17A C17D 1.509(9) .
C17A C17B 1.530(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 1.288(6) .
C19 H19 0.9300 .
N20 N21 1.383(5) .
N21 C23 1.352(7) .
N21 C21A 1.453(7) .
C21A H21A 0.9600 .
C21A H21B 0.9600 .
C21A H21C 0.9600 .
N22 C23 1.345(7) .
N22 C30 1.405(6) .
C23 N24 1.357(6) .
N24 C25 1.377(7) .
N24 H24 0.8600 .
C25 C26 1.375(7) .
C25 C30 1.387(7) .
C26 C27 1.363(8) .
C26 H26 0.9300 .
C27 C28 1.390(8) .
C27 H27 0.9300 .
C28 C29 1.396(8) .
C28 H28 0.9300 .
C29 C30 1.387(7) .
C29 H29 0.9300 .
N1A O3A 1.164(8) .
N1A O2A 1.182(8) .
N1A O1A 1.187(10) .
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 2.834(8) 157.7 3_565
C10A H10A O3A 0.96 2.23 3.071(9) 145.7 3_565
C21A H21A O1A 0.96 2.54 3.338(10) 141.0 29
N24 H24 O2A 0.86 1.92 2.757(7) 164.8 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 -3.6(6)
Ho1 N1 C2 N3 156.2(4)
C9 N1 C2 N10 178.6(5)
Ho1 N1 C2 N10 -21.6(7)
N1 C2 N3 C4 2.3(7)
N10 C2 N3 C4 -179.8(5)
C2 N3 C4 C5 179.3(6)
C2 N3 C4 C9 0.1(6)
N3 C4 C5 C6 -176.9(6)
C9 C4 C5 C6 2.3(10)
C4 C5 C6 C7 -0.6(11)
C5 C6 C7 C8 -0.4(12)
C6 C7 C8 C9 -0.3(11)
C7 C8 C9 C4 2.0(10)
C7 C8 C9 N1 -179.9(6)
N3 C4 C9 C8 176.3(6)
C5 C4 C9 C8 -3.1(10)
N3 C4 C9 N1 -2.2(7)
C5 C4 C9 N1 178.4(6)
C2 N1 C9 C8 -174.8(7)
Ho1 N1 C9 C8 30.0(10)
C2 N1 C9 C4 3.5(6)
Ho1 N1 C9 C4 -151.7(4)
N1 C2 N10 N11 3.0(8)
N3 C2 N10 N11 -174.7(5)
N1 C2 N10 C10A -169.6(6)
N3 C2 N10 C10A 12.7(9)
C2 N10 N11 C12 -162.2(5)
C10A N10 N11 C12 10.3(8)
C2 N10 N11 Ho1 15.4(6)
C10A N10 N11 Ho1 -172.0(5)
N10 N11 C12 C13 -175.8(5)
Ho1 N11 C12 C13 6.9(8)
N11 C12 C13 C18 -161.1(5)
N11 C12 C13 C14 23.3(8)
C18 C13 C14 O14 -178.0(5)
C12 C13 C14 O14 -2.4(8)
C18 C13 C14 C15 0.7(8)
C12 C13 C14 C15 176.3(5)
C15 C14 O14 Ho2 -56.3(6)
C13 C14 O14 Ho2 122.3(5)
C15 C14 O14 Ho1 122.6(5)
C13 C14 O14 Ho1 -58.7(6)
O14 C14 C15 C16 -179.3(5)
C13 C14 C15 C16 2.0(8)
O14 C14 C15 C19 -4.6(8)
C13 C14 C15 C19 176.7(5)
C14 C15 C16 C17 -3.1(9)
C19 C15 C16 C17 -178.0(5)
C15 C16 C17 C18 1.4(9)
C15 C16 C17 C17A 179.3(6)
C16 C17 C17A C17C 139.1(7)
C18 C17 C17A C17C -43.0(9)
C16 C17 C17A C17D 14.8(10)
C18 C17 C17A C17D -167.3(7)
C16 C17 C17A C17B -102.8(7)
C18 C17 C17A C17B 75.1(8)
C14 C13 C18 C17 -2.5(9)
C12 C13 C18 C17 -178.2(5)
C16 C17 C18 C13 1.4(9)
C17A C17 C18 C13 -176.6(6)
C16 C15 C19 N20 -162.6(5)
C14 C15 C19 N20 22.6(8)
C15 C19 N20 N21 -176.1(5)
C15 C19 N20 Ho2 8.4(8)
C19 N20 N21 C23 -165.5(5)
Ho2 N20 N21 C23 10.6(6)
C19 N20 N21 C21A 5.6(8)
Ho2 N20 N21 C21A -178.4(5)
C30 N22 C23 N21 178.4(5)
Ho2 N22 C23 N21 -26.8(7)
C30 N22 C23 N24 -0.6(6)
Ho2 N22 C23 N24 154.2(4)
N20 N21 C23 N22 9.9(8)
C21A N21 C23 N22 -161.1(6)
N20 N21 C23 N24 -171.1(5)
C21A N21 C23 N24 17.8(9)
N22 C23 N24 C25 -0.3(7)
N21 C23 N24 C25 -179.3(5)
C23 N24 C25 C26 -179.0(6)
C23 N24 C25 C30 1.1(6)
N24 C25 C26 C27 -177.7(6)
C30 C25 C26 C27 2.1(10)
C25 C26 C27 C28 -0.2(10)
C26 C27 C28 C29 -0.7(11)
C27 C28 C29 C30 -0.1(9)
C28 C29 C30 C25 1.9(8)
C28 C29 C30 N22 179.9(5)
N24 C25 C30 C29 176.8(5)
C26 C25 C30 C29 -3.1(9)
N24 C25 C30 N22 -1.5(6)
C26 C25 C30 N22 178.6(5)
C23 N22 C30 C29 -176.8(6)
Ho2 N22 C30 C29 34.8(9)
C23 N22 C30 C25 1.3(6)
Ho2 N22 C30 C25 -147.0(4)
