data_tbe226_1
_audit_creation_date               2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C30 H31 N3 O3'
_chemical_formula_sum              'C30 H31 N3 O3'
_chemical_formula_weight           481.58
_chemical_absolute_configuration   'syn'
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             19
_space_group_name_H-M_alt          'P 21 21 21'
_space_group_name_Hall             'P 2ac 2ab'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'

_cell_length_a                     12.8492(7)
_cell_length_b                     23.7824(12)
_cell_length_c                     8.4063(4)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       2568.8(2)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      9953
_cell_measurement_temperature      299(2)
_cell_measurement_theta_max        70.64
_cell_measurement_theta_min        3.91
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.646
_exptl_absorpt_correction_T_max    0.7535
_exptl_absorpt_correction_T_min    0.6637
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1126 before and 0.0719 after correction.
The Ratio of minimum to maximum transmission is 0.8808.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'colorless'
_exptl_crystal_density_diffrn      1.245
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'prism'
_exptl_crystal_F_000               1024
_exptl_crystal_size_max            0.41
_exptl_crystal_size_mid            0.27
_exptl_crystal_size_min            0.12
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0461
_diffrn_reflns_av_unetI/netI       0.0322
_diffrn_reflns_Laue_measured_fraction_full  0.989
_diffrn_reflns_Laue_measured_fraction_max  0.978
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -15
_diffrn_reflns_limit_k_max         29
_diffrn_reflns_limit_k_min         -28
_diffrn_reflns_limit_l_max         9
_diffrn_reflns_limit_l_min         -10
_diffrn_reflns_number              34823
_diffrn_reflns_point_group_measured_fraction_full  0.992
_diffrn_reflns_point_group_measured_fraction_max  0.975
_diffrn_reflns_theta_full          67.679
_diffrn_reflns_theta_max           71.529
_diffrn_reflns_theta_min           3.910
_diffrn_ambient_temperature        299.15
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.989
_diffrn_measured_fraction_theta_max  0.978
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.749
_reflns_Friedel_fraction_full      0.995
_reflns_Friedel_fraction_max       0.971
_reflns_number_gt                  4422
_reflns_number_total               4896
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max           0.480
_refine_diff_density_min           -0.155
_refine_diff_density_rms           0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 1710 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     0.25(8)
_refine_ls_extinction_coef         0.0029(17)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.070
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       333
_refine_ls_number_reflns           4896
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0564
_refine_ls_R_factor_gt             0.0510
_refine_ls_restrained_S_all        1.070
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0766P)²+0.4488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1398
_refine_ls_wR_factor_ref           0.1439
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 O10 O 0.31416(15) 0.20057(10) 0.3368(3) 0.0705(7) Uani 1 1 d . . . . .
 O11 O 0.6433(2) 0.09081(11) 0.5820(3) 0.0767(7) Uani 1 1 d . . . . .
 O12 O 0.6651(2) 0.22152(12) 0.6331(3) 0.0783(7) Uani 1 1 d . . . . .
 H12 H 0.726(4) 0.2530(19) 0.631(6) 0.094(13) Uiso 1 1 d . . . . .
 N3 N 0.55120(19) 0.26108(11) 0.1969(3) 0.0592(6) Uani 1 1 d . . . . .
 N6 N 0.51831(18) 0.14538(10) 0.4694(3) 0.0533(6) Uani 1 1 d . . . . .
 N9 N 0.68247(18) 0.21202(12) 0.3479(3) 0.0562(6) Uani 1 1 d . . . . .
 C1 C 0.4063(2) 0.21494(12) 0.3136(4) 0.0542(7) Uani 1 1 d . . . . .
 C2 C 0.4368(2) 0.26037(14) 0.1979(5) 0.0665(8) Uani 1 1 d . . . . .
 H2A H 0.409996 0.252079 0.092588 0.080 Uiso 1 1 calc R . . . .
 H2B H 0.409598 0.296481 0.231864 0.080 Uiso 1 1 calc R . . . .
 C4 C 0.5816(2) 0.22208(12) 0.3056(3) 0.0492(6) Uani 1 1 d . . . . .
 C5 C 0.5002(2) 0.19279(11) 0.3735(3) 0.0487(6) Uani 1 1 d . . . . .
 C7 C 0.6166(2) 0.13460(14) 0.5188(4) 0.0576(7) Uani 1 1 d . . . . .
 C8 C 0.6921(2) 0.18352(16) 0.4996(4) 0.0652(8) Uani 1 1 d . . . . .
 H8 H 0.763636 0.169968 0.512859 0.078 Uiso 1 1 calc R . . . .
 C13 C 0.6049(3) 0.31581(14) 0.1721(4) 0.0641(8) Uani 1 1 d . . . . .
 H13 H 0.679232 0.309074 0.190307 0.077 Uiso 1 1 calc R . . . .
 C14 C 0.5932(4) 0.3320(2) -0.0041(5) 0.0933(13) Uani 1 1 d . . . . .
 H14A H 0.622123 0.302849 -0.069602 0.140 Uiso 1 1 calc GR . . . .
 H14B H 0.629460 0.366626 -0.023811 0.140 Uiso 1 1 calc GR . . . .
 H14C H 0.520830 0.336674 -0.028993 0.140 Uiso 1 1 calc GR . . . .
 C15 C 0.5718(3) 0.36005(13) 0.2898(5) 0.0681(9) Uani 1 1 d . . . . .
 C16 C 0.4958(4) 0.39978(18) 0.2546(7) 0.0988(14) Uani 1 1 d . . . . .
 H16 H 0.463020 0.399008 0.155967 0.119 Uiso 1 1 calc R . . . .
 C17 C 0.4686(6) 0.4399(2) 0.3631(10) 0.129(2) Uani 1 1 d . . . . .
 H17 H 0.417085 0.465854 0.337778 0.155 Uiso 1 1 calc R . . . .
 C18 C 0.5150(7) 0.4425(3) 0.5052(11) 0.141(3) Uani 1 1 d . . . . .
 H18 H 0.497304 0.470825 0.576448 0.170 Uiso 1 1 calc R . . . .
 C19 C 0.5900(6) 0.4027(3) 0.5468(7) 0.126(2) Uani 1 1 d . . . . .
 H19 H 0.621186 0.403811 0.646524 0.152 Uiso 1 1 calc R . . . .
 C20 C 0.6175(4) 0.36136(19) 0.4380(5) 0.0855(11) Uani 1 1 d . . . . .
 H20 H 0.667021 0.334502 0.465225 0.103 Uiso 1 1 calc R . . . .
 C21 C 0.4348(3) 0.10359(13) 0.4933(5) 0.0666(9) Uani 1 1 d . . . . .
 H21 H 0.372554 0.118814 0.441506 0.080 Uiso 1 1 calc R . . . .
 C22 C 0.4615(5) 0.0486(2) 0.4059(7) 0.1080(16) Uani 1 1 d . . . . .
 H22A H 0.488617 0.057245 0.302271 0.162 Uiso 1 1 calc GR . . . .
 H22B H 0.399879 0.026156 0.395243 0.162 Uiso 1 1 calc GR . . . .
 H22C H 0.512811 0.028220 0.465571 0.162 Uiso 1 1 calc GR . . . .
 C23 C 0.4074(2) 0.09619(14) 0.6688(5) 0.0656(9) Uani 1 1 d . . . . .
 C24 C 0.4502(3) 0.12681(17) 0.7895(5) 0.0766(10) Uani 1 1 d . . . . .
 H24 H 0.501323 0.153301 0.766613 0.092 Uiso 1 1 calc R . . . .
 C25 C 0.4185(5) 0.1190(3) 0.9469(6) 0.1068(16) Uani 1 1 d . . . . .
 H25 H 0.450029 0.139724 1.027414 0.128 Uiso 1 1 calc R . . . .
 C26 C 0.3441(5) 0.0824(3) 0.9835(8) 0.130(3) Uani 1 1 d . . . . .
 H26 H 0.324590 0.076568 1.088726 0.156 Uiso 1 1 calc R . . . .
 C27 C 0.2976(5) 0.0542(4) 0.8649(10) 0.154(3) Uani 1 1 d . . . . .
 H27 H 0.242522 0.030230 0.888623 0.184 Uiso 1 1 calc R . . . .
 C28 C 0.3290(4) 0.0595(3) 0.7106(8) 0.118(2) Uani 1 1 d . . . . .
 H28 H 0.296847 0.038082 0.632187 0.142 Uiso 1 1 calc R . . . .
 C29 C 0.7671(2) 0.20775(13) 0.2255(4) 0.0547(7) Uani 1 1 d . . . . .
 H29 H 0.748668 0.233390 0.138673 0.066 Uiso 1 1 calc R . . . .
 C30 C 0.8696(2) 0.22873(17) 0.2960(5) 0.0721(10) Uani 1 1 d . . . . .
 H30A H 0.859079 0.265010 0.343430 0.108 Uiso 1 1 calc GR . . . .
 H30B H 0.920825 0.231605 0.213282 0.108 Uiso 1 1 calc GR . . . .
 H30C H 0.893263 0.202762 0.375592 0.108 Uiso 1 1 calc GR . . . .
 C31 C 0.7707(2) 0.14918(13) 0.1561(4) 0.0537(7) Uani 1 1 d . . . . .
 C32 C 0.8252(4) 0.10604(17) 0.2234(5) 0.0827(11) Uani 1 1 d . . . . .
 H32 H 0.863956 0.112691 0.314945 0.099 Uiso 1 1 calc R . . . .
 C33 C 0.8240(4) 0.05246(17) 0.1580(5) 0.0889(12) Uani 1 1 d . . . . .
 H33 H 0.861751 0.023803 0.206444 0.107 Uiso 1 1 calc R . . . .
 C34 C 0.7691(4) 0.04149(16) 0.0258(5) 0.0817(11) Uani 1 1 d . . . . .
 H34 H 0.767094 0.005343 -0.016259 0.098 Uiso 1 1 calc R . . . .
 C35 C 0.7165(4) 0.0842(2) -0.0453(6) 0.1018(15) Uani 1 1 d . . . . .
 H35 H 0.678960 0.077320 -0.137904 0.122 Uiso 1 1 calc R . . . .
 C36 C 0.7181(3) 0.13759(16) 0.0181(5) 0.0797(11) Uani 1 1 d . . . . .
 H36 H 0.682802 0.166370 -0.033737 0.096 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 O10 C1 1.248(4) . ?
 O11 C7 1.218(4) . ?
 O12 C8 1.482(5) . ?
 N3 C2 1.470(4) . ?
 N3 C4 1.360(4) . ?
 N3 C13 1.488(4) . ?
 N6 C5 1.406(4) . ?
 N6 C7 1.354(4) . ?
 N6 C21 1.476(4) . ?
 N9 C4 1.365(4) . ?
 N9 C8 1.450(4) . ?
 N9 C29 1.500(4) . ?
 C1 C2 1.506(5) . ?
 C1 C5 1.409(4) . ?
 C4 C5 1.380(4) . ?
 C7 C8 1.523(5) . ?
 C13 C14 1.538(5) . ?
 C13 C15 1.506(5) . ?
 C15 C16 1.391(6) . ?
 C15 C20 1.378(6) . ?
 C16 C17 1.366(8) . ?
 C17 C18 1.336(11) . ?
 C18 C19 1.395(11) . ?
 C19 C20 1.388(7) . ?
 C21 C22 1.538(6) . ?
 C21 C23 1.526(5) . ?
 C23 C24 1.365(6) . ?
 C23 C28 1.378(6) . ?
 C24 C25 1.397(6) . ?
 C25 C26 1.329(9) . ?
 C26 C27 1.342(10) . ?
 C27 C28 1.365(9) . ?
 C29 C30 1.528(4) . ?
 C29 C31 1.511(4) . ?
 C31 C32 1.365(5) . ?
 C31 C36 1.370(5) . ?
 C32 C33 1.388(6) . ?
 C33 C34 1.342(6) . ?
 C34 C35 1.359(6) . ?
 C35 C36 1.377(6) . ?

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
 C2 N3 C13 118.4(3) . . ?
 C4 N3 C2 106.0(3) . . ?
 C4 N3 C13 123.9(3) . . ?
 C5 N6 C21 119.8(2) . . ?
 C7 N6 C5 118.8(2) . . ?
 C7 N6 C21 120.6(3) . . ?
 C4 N9 C8 113.1(2) . . ?
 C4 N9 C29 121.4(2) . . ?
 C8 N9 C29 120.6(2) . . ?
 O10 C1 C2 123.0(3) . . ?
 O10 C1 C5 130.9(3) . . ?
 C5 C1 C2 106.0(2) . . ?
 N3 C2 C1 105.8(3) . . ?
 N3 C4 N9 124.6(3) . . ?
 N3 C4 C5 113.8(2) . . ?
 N9 C4 C5 121.6(3) . . ?
 N6 C5 C1 130.3(3) . . ?
 C4 C5 N6 121.1(2) . . ?
 C4 C5 C1 108.2(3) . . ?
 O11 C7 N6 123.9(3) . . ?
 O11 C7 C8 121.3(3) . . ?
 N6 C7 C8 114.7(3) . . ?
 O12 C8 C7 103.7(3) . . ?
 N9 C8 O12 111.1(3) . . ?
 N9 C8 C7 113.3(3) . . ?
 N3 C13 C14 108.0(3) . . ?
 N3 C13 C15 112.8(3) . . ?
 C15 C13 C14 115.5(3) . . ?
 C16 C15 C13 122.2(4) . . ?
 C20 C15 C13 119.3(3) . . ?
 C20 C15 C16 118.5(4) . . ?
 C17 C16 C15 120.8(6) . . ?
 C18 C17 C16 121.0(6) . . ?
 C17 C18 C19 120.1(6) . . ?
 C20 C19 C18 119.4(6) . . ?
 C15 C20 C19 120.2(5) . . ?
 N6 C21 C22 110.2(3) . . ?
 N6 C21 C23 112.1(3) . . ?
 C23 C21 C22 114.5(3) . . ?
 C24 C23 C21 124.4(3) . . ?
 C24 C23 C28 116.3(4) . . ?
 C28 C23 C21 119.2(4) . . ?
 C23 C24 C25 121.1(4) . . ?
 C26 C25 C24 121.1(6) . . ?
 C25 C26 C27 118.4(5) . . ?
 C26 C27 C28 121.9(5) . . ?
 C27 C28 C23 121.2(6) . . ?
 N9 C29 C30 109.7(2) . . ?
 N9 C29 C31 110.5(2) . . ?
 C31 C29 C30 115.1(3) . . ?
 C32 C31 C29 123.3(3) . . ?
 C32 C31 C36 116.9(3) . . ?
 C36 C31 C29 119.8(3) . . ?
 C31 C32 C33 121.4(4) . . ?
 C34 C33 C32 120.8(4) . . ?
 C33 C34 C35 118.7(4) . . ?
 C34 C35 C36 120.7(4) . . ?
 C31 C36 C35 121.4(4) . . ?

_olex2_submission_special_instructions  'No special instructions were received'

#===END


data_tbe242_1_1
_audit_creation_date               2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C37 H38 N4 O4'
_chemical_formula_sum              'C37 H38 N4 O4'
_chemical_formula_weight           602.71
_chemical_absolute_configuration   'syn'
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             4
_space_group_name_H-M_alt          'P 1 21 1'
_space_group_name_Hall             'P 2yb'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'

_cell_length_a                     8.8020(5)
_cell_length_b                     11.2590(6)
_cell_length_c                     15.7919(8)
_cell_angle_alpha                  90
_cell_angle_beta                   95.669(2)
_cell_angle_gamma                  90
_cell_volume                       1557.35(14)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      8134
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        74.01
_cell_measurement_theta_min        2.81
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.675
_exptl_absorpt_correction_T_max    0.7538
_exptl_absorpt_correction_T_min    0.6903
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1671 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.9158.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'colorless'
_exptl_crystal_density_diffrn      1.285
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'prism'
_exptl_crystal_F_000               640
_exptl_crystal_size_max            0.22
_exptl_crystal_size_mid            0.19
_exptl_crystal_size_min            0.15
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0789
_diffrn_reflns_av_unetI/netI       0.0530
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.968
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         14
_diffrn_reflns_limit_k_min         -13
_diffrn_reflns_limit_l_max         19
_diffrn_reflns_limit_l_min         -19
_diffrn_reflns_number              30976
_diffrn_reflns_point_group_measured_fraction_full  0.997
_diffrn_reflns_point_group_measured_fraction_max  0.954
_diffrn_reflns_theta_full          67.679
_diffrn_reflns_theta_max           74.280
_diffrn_reflns_theta_min           2.812
_diffrn_ambient_temperature        293(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.968
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.873
_reflns_Friedel_fraction_full      0.995
_reflns_Friedel_fraction_max       0.939
_reflns_number_gt                  4405
_reflns_number_total               6045
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max           0.155
_refine_diff_density_min           -0.144
_refine_diff_density_rms           0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1627 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     0.0(2)
_refine_ls_extinction_coef         0.0046(8)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.030
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       408
_refine_ls_number_reflns           6045
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0720
_refine_ls_R_factor_gt             0.0449
_refine_ls_restrained_S_all        1.030
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0530P)²+0.1647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1039
_refine_ls_wR_factor_ref           0.1164
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C13(H13A,H13B), C20(H20A,H20B), C22(H22A,H22B),
 C29(H29A,H29B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 C1 C 0.9116(4) 0.4518(3) 0.8519(2) 0.0352(9) Uani 1 1 d . . . . .
 H1A H 0.930698 0.451191 0.913489 0.042 Uiso 1 1 calc R . . . .
 H1B H 0.920109 0.370665 0.832308 0.042 Uiso 1 1 calc R . . . .
 C2 C 0.7485(4) 0.4950(4) 0.8276(2) 0.0339(9) Uani 1 1 d . . . . .
 C3 C 1.0925(5) 0.6305(4) 0.8635(2) 0.0452(10) Uani 1 1 d . . . . .
 H3 H 1.203539 0.627254 0.862544 0.054 Uiso 1 1 calc R . . . .
 C4 C 1.0384(6) 0.7425(4) 0.8163(3) 0.0739(13) Uani 1 1 d . . . . .
 H4A H 1.068302 0.740118 0.759543 0.111 Uiso 1 1 calc GR . . . .
 H4B H 1.083343 0.810606 0.845574 0.111 Uiso 1 1 calc GR . . . .
 H4C H 0.929162 0.747678 0.814090 0.111 Uiso 1 1 calc GR . . . .
 C5 C 1.0615(5) 0.6285(4) 0.9558(3) 0.0445(11) Uani 1 1 d . . . . .
 C6 C 1.1510(5) 0.5576(5) 1.0132(3) 0.0593(13) Uani 1 1 d . . . . .
 H6 H 1.230461 0.513284 0.994567 0.071 Uiso 1 1 calc R . . . .
 C7 C 1.1225(7) 0.5526(5) 1.0980(3) 0.0744(16) Uani 1 1 d . . . . .
 H7 H 1.182078 0.504914 1.136202 0.089 Uiso 1 1 calc R . . . .
 C8 C 1.0051(7) 0.6188(6) 1.1248(3) 0.080(2) Uani 1 1 d . . . . .
 H8 H 0.985121 0.615065 1.181499 0.096 Uiso 1 1 calc R . . . .
 C9 C 0.9181(6) 0.6893(5) 1.0701(3) 0.0690(16) Uani 1 1 d . . . . .
 H9 H 0.839531 0.733888 1.089417 0.083 Uiso 1 1 calc R . . . .
 C10 C 0.9461(5) 0.6949(4) 0.9856(3) 0.0545(13) Uani 1 1 d . . . . .
 H10 H 0.886566 0.744053 0.948424 0.065 Uiso 1 1 calc R . . . .
 C11 C 0.4771(4) 0.4428(4) 0.8164(2) 0.0423(10) Uani 1 1 d . . . . .
 H11A H 0.470540 0.514706 0.782387 0.051 Uiso 1 1 calc R . . . .
 H11B H 0.416607 0.454381 0.863887 0.051 Uiso 1 1 calc R . . . .
 C12 C 0.4121(4) 0.3382(4) 0.7621(2) 0.0410(10) Uani 1 1 d . . . . .
 C13 C 0.6590(4) 0.3208(4) 0.9077(2) 0.0414(10) Uani 1 1 d . . . . .
 H13A H 0.766052 0.298831 0.913621 0.050 Uiso 1 1 calc R . . . .
 H13B H 0.600917 0.253191 0.884148 0.050 Uiso 1 1 calc R . . . .
 C14 C 0.6097(4) 0.3496(4) 0.9951(2) 0.0429(10) Uani 1 1 d . . . . .
 C15 C 0.6541(5) 0.4522(4) 1.0365(3) 0.0564(12) Uani 1 1 d . . . . .
 H15 H 0.713944 0.506020 1.009911 0.068 Uiso 1 1 calc R . . . .
 C16 C 0.6129(6) 0.4791(5) 1.1170(3) 0.0673(13) Uani 1 1 d . . . . .
 H16 H 0.644073 0.549761 1.143875 0.081 Uiso 1 1 calc R . . . .
 C17 C 0.5249(6) 0.3989(5) 1.1560(3) 0.0729(15) Uani 1 1 d . . . . .
 H17 H 0.496188 0.415366 1.209859 0.087 Uiso 1 1 calc R . . . .
 C18 C 0.4789(6) 0.2947(6) 1.1161(3) 0.0746(16) Uani 1 1 d . . . . .
 H18 H 0.420668 0.240254 1.143220 0.090 Uiso 1 1 calc R . . . .
 C19 C 0.5204(5) 0.2709(5) 1.0345(3) 0.0593(12) Uani 1 1 d . . . . .
 H19 H 0.487141 0.201417 1.006778 0.071 Uiso 1 1 calc R . . . .
 C20 C 0.5817(4) 0.3935(4) 0.6541(2) 0.0374(9) Uani 1 1 d . . . . .
 H20A H 0.574471 0.473101 0.676820 0.045 Uiso 1 1 calc R . . . .
 H20B H 0.563129 0.398559 0.592593 0.045 Uiso 1 1 calc R . . . .
 C21 C 0.7425(4) 0.3461(4) 0.6777(2) 0.0366(9) Uani 1 1 d . . . . .
 C22 C 0.4138(6) 0.2103(4) 0.6395(3) 0.0576(13) Uani 1 1 d . . . . .
 H22A H 0.306435 0.197438 0.645651 0.069 Uiso 1 1 calc R . . . .
 H22B H 0.470095 0.143041 0.664914 0.069 Uiso 1 1 calc R . . . .
 C23 C 0.4358(5) 0.2154(4) 0.5463(3) 0.0479(12) Uani 1 1 d . . . . .
 C24 C 0.3476(6) 0.2881(5) 0.4920(3) 0.0652(14) Uani 1 1 d . . . . .
 H24 H 0.269925 0.332970 0.512012 0.078 Uiso 1 1 calc R . . . .
 C25 C 0.3746(8) 0.2948(7) 0.4061(4) 0.093(2) Uani 1 1 d . . . . .
 H25 H 0.314290 0.343620 0.369073 0.112 Uiso 1 1 calc R . . . .
 C26 C 0.4906(9) 0.2289(7) 0.3762(4) 0.096(3) Uani 1 1 d . . . . .
 H26 H 0.509608 0.234382 0.319460 0.116 Uiso 1 1 calc R . . . .
 C27 C 0.5756(7) 0.1571(6) 0.4296(4) 0.087(2) Uani 1 1 d . . . . .
 H27 H 0.652169 0.111530 0.409183 0.104 Uiso 1 1 calc R . . . .
 C28 C 0.5511(5) 0.1499(5) 0.5144(3) 0.0651(15) Uani 1 1 d . . . . .
 H28 H 0.612382 0.100608 0.550625 0.078 Uiso 1 1 calc R . . . .
 C29 C 1.0165(4) 0.3919(4) 0.6898(2) 0.0425(10) Uani 1 1 d . . . . .
 H29A H 1.075351 0.378119 0.641973 0.051 Uiso 1 1 calc R . . . .
 H29B H 1.019360 0.319917 0.723730 0.051 Uiso 1 1 calc R . . . .
 C30 C 1.0875(4) 0.4937(4) 0.7437(2) 0.0408(10) Uani 1 1 d . . . . .
 C31 C 0.8391(4) 0.5251(4) 0.6057(2) 0.0418(10) Uani 1 1 d . . . . .
 H31A H 0.898411 0.589396 0.633290 0.050 Uiso 1 1 calc R . . . .
 H31B H 0.732553 0.548487 0.600855 0.050 Uiso 1 1 calc R . . . .
 C32 C 0.8882(4) 0.5065(4) 0.5177(2) 0.0430(10) Uani 1 1 d . . . . .
 C33 C 0.8273(6) 0.4154(6) 0.4676(3) 0.0787(17) Uani 1 1 d . . . . .
 H33 H 0.759005 0.363259 0.489324 0.094 Uiso 1 1 calc R . . . .
 C34 C 0.8651(8) 0.3995(6) 0.3854(3) 0.102(2) Uani 1 1 d . . . . .
 H34 H 0.821925 0.337613 0.352187 0.123 Uiso 1 1 calc R . . . .
 C35 C 0.9658(7) 0.4748(7) 0.3535(3) 0.093(2) Uani 1 1 d . . . . .
 H35 H 0.992552 0.463959 0.298493 0.112 Uiso 1 1 calc R . . . .
 C36 C 1.0274(6) 0.5660(6) 0.4017(4) 0.0840(18) Uani 1 1 d . . . . .
 H36 H 1.096031 0.617281 0.379448 0.101 Uiso 1 1 calc R . . . .
 C37 C 0.9887(6) 0.5832(5) 0.4842(3) 0.0649(13) Uani 1 1 d . . . . .
 H37 H 1.030440 0.646366 0.516617 0.078 Uiso 1 1 calc R . . . .
 N1 N 1.0288(3) 0.5230(3) 0.81750(18) 0.0375(8) Uani 1 1 d . . . . .
 N2 N 0.6361(3) 0.4216(3) 0.84869(18) 0.0380(8) Uani 1 1 d . . . . .
 N3 N 0.4649(4) 0.3196(3) 0.6860(2) 0.0425(8) Uani 1 1 d . . . . .
 N4 N 0.8588(3) 0.4189(3) 0.65855(17) 0.0357(8) Uani 1 1 d . . . . .
 O1 O 0.7226(3) 0.5879(2) 0.78805(16) 0.0420(7) Uani 1 1 d . . . . .
 O2 O 0.3157(3) 0.2747(3) 0.78894(17) 0.0571(8) Uani 1 1 d . . . . .
 O3 O 0.7649(3) 0.2516(3) 0.71474(16) 0.0472(7) Uani 1 1 d . . . . .
 O4 O 1.1942(3) 0.5503(3) 0.71838(17) 0.0539(8) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 C1 C2 1.528(5) . ?
 C1 N1 1.453(5) . ?
 C2 N2 1.356(5) . ?
 C2 O1 1.227(5) . ?
 C3 C4 1.516(7) . ?
 C3 C5 1.510(5) . ?
 C3 N1 1.492(6) . ?
 C5 C6 1.393(7) . ?
 C5 C10 1.381(6) . ?
 C6 C7 1.388(6) . ?
 C7 C8 1.375(8) . ?
 C8 C9 1.353(8) . ?
 C9 C10 1.383(6) . ?
 C11 C12 1.535(6) . ?
 C11 N2 1.461(5) . ?
 C12 N3 1.347(4) . ?
 C12 O2 1.217(5) . ?
 C13 C14 1.521(5) . ?
 C13 N2 1.470(5) . ?
 C14 C15 1.366(6) . ?
 C14 C19 1.373(6) . ?
 C15 C16 1.389(6) . ?
 C16 C17 1.374(7) . ?
 C17 C18 1.373(8) . ?
 C18 C19 1.400(6) . ?
 C20 C21 1.524(5) . ?
 C20 N3 1.452(5) . ?
 C21 N4 1.368(5) . ?
 C21 O3 1.222(5) . ?
 C22 C23 1.504(6) . ?
 C22 N3 1.480(6) . ?
 C23 C24 1.370(7) . ?
 C23 C28 1.389(6) . ?
 C24 C25 1.402(7) . ?
 C25 C26 1.381(10) . ?
 C26 C27 1.342(10) . ?
 C27 C28 1.380(7) . ?
 C29 C30 1.524(6) . ?
 C29 N4 1.459(5) . ?
 C30 N1 1.362(4) . ?
 C30 O4 1.234(4) . ?
 C31 C32 1.510(5) . ?
 C31 N4 1.459(5) . ?
 C32 C33 1.371(7) . ?
 C32 C37 1.379(6) . ?
 C33 C34 1.383(6) . ?
 C34 C35 1.359(8) . ?
 C35 C36 1.359(9) . ?
 C36 C37 1.392(7) . ?

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
 N1 C1 C2 114.4(3) . . ?
 N2 C2 C1 115.7(3) . . ?
 O1 C2 C1 121.5(3) . . ?
 O1 C2 N2 122.7(4) . . ?
 C5 C3 C4 114.1(4) . . ?
 N1 C3 C4 110.6(3) . . ?
 N1 C3 C5 111.3(3) . . ?
 C6 C5 C3 119.5(4) . . ?
 C10 C5 C3 122.0(4) . . ?
 C10 C5 C6 118.5(4) . . ?
 C7 C6 C5 120.4(5) . . ?
 C8 C7 C6 119.3(5) . . ?
 C9 C8 C7 121.1(5) . . ?
 C8 C9 C10 120.0(5) . . ?
 C5 C10 C9 120.8(5) . . ?
 N2 C11 C12 111.1(3) . . ?
 N3 C12 C11 118.4(3) . . ?
 O2 C12 C11 119.4(3) . . ?
 O2 C12 N3 122.2(4) . . ?
 N2 C13 C14 112.2(3) . . ?
 C15 C14 C13 121.4(4) . . ?
 C15 C14 C19 118.5(4) . . ?
 C19 C14 C13 120.1(4) . . ?
 C14 C15 C16 122.3(4) . . ?
 C17 C16 C15 118.4(5) . . ?
 C18 C17 C16 120.7(4) . . ?
 C17 C18 C19 119.6(4) . . ?
 C14 C19 C18 120.5(5) . . ?
 N3 C20 C21 112.8(3) . . ?
 N4 C21 C20 115.7(3) . . ?
 O3 C21 C20 121.6(4) . . ?
 O3 C21 N4 122.6(4) . . ?
 N3 C22 C23 113.0(4) . . ?
 C24 C23 C22 121.0(4) . . ?
 C24 C23 C28 118.7(5) . . ?
 C28 C23 C22 120.2(5) . . ?
 C23 C24 C25 119.8(5) . . ?
 C26 C25 C24 120.2(7) . . ?
 C27 C26 C25 119.6(6) . . ?
 C26 C27 C28 121.0(6) . . ?
 C27 C28 C23 120.7(6) . . ?
 N4 C29 C30 110.9(3) . . ?
 N1 C30 C29 119.4(3) . . ?
 O4 C30 C29 119.4(3) . . ?
 O4 C30 N1 121.2(4) . . ?
 N4 C31 C32 112.6(3) . . ?
 C33 C32 C31 120.3(4) . . ?
 C33 C32 C37 118.4(4) . . ?
 C37 C32 C31 121.2(4) . . ?
 C32 C33 C34 121.5(5) . . ?
 C35 C34 C33 119.5(6) . . ?
 C36 C35 C34 120.1(5) . . ?
 C35 C36 C37 120.6(5) . . ?
 C32 C37 C36 119.8(5) . . ?
 C1 N1 C3 120.8(3) . . ?
 C30 N1 C1 122.0(3) . . ?
 C30 N1 C3 117.2(3) . . ?
 C2 N2 C11 120.8(3) . . ?
 C2 N2 C13 124.7(3) . . ?
 C11 N2 C13 114.5(3) . . ?
 C12 N3 C20 122.7(4) . . ?
 C12 N3 C22 117.2(3) . . ?
 C20 N3 C22 119.7(3) . . ?
 C21 N4 C29 120.5(3) . . ?
 C21 N4 C31 124.6(3) . . ?
 C29 N4 C31 114.8(3) . . ?

_olex2_submission_special_instructions  'No special instructions were received'
#===END
data_tbe243_1_a
_audit_creation_date               2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C38 H40 N4 O4'
_chemical_formula_sum              'C38 H40 N4 O4'
_chemical_formula_weight           616.74
_chemical_absolute_configuration   'syn'
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             4
_space_group_name_H-M_alt          'P 1 21 1'
_space_group_name_Hall             'P 2yb'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'

_cell_length_a                     8.9528(11)
_cell_length_b                     11.419(3)
_cell_length_c                     15.863(2)
_cell_angle_alpha                  90
_cell_angle_beta                   93.945(12)
_cell_angle_gamma                  90
_cell_volume                       1617.8(5)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      9904
_cell_measurement_temperature      296(2)
_cell_measurement_theta_max        73.72
_cell_measurement_theta_min        2.80
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.661
_exptl_absorpt_correction_T_max    0.7538
_exptl_absorpt_correction_T_min    0.6994
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1401 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9278.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'colorless'
_exptl_crystal_density_diffrn      1.266
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'prism'
_exptl_crystal_F_000               656
_exptl_crystal_size_max            0.46
_exptl_crystal_size_mid            0.12
_exptl_crystal_size_min            0.06
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0406
_diffrn_reflns_av_unetI/netI       0.0253
_diffrn_reflns_Laue_measured_fraction_full  0.982
_diffrn_reflns_Laue_measured_fraction_max  0.951
_diffrn_reflns_limit_h_max         9
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         14
_diffrn_reflns_limit_k_min         -14
_diffrn_reflns_limit_l_max         19
_diffrn_reflns_limit_l_min         -19
_diffrn_reflns_number              34032
_diffrn_reflns_point_group_measured_fraction_full  0.982
_diffrn_reflns_point_group_measured_fraction_max  0.934
_diffrn_reflns_theta_full          67.679
_diffrn_reflns_theta_max           74.970
_diffrn_reflns_theta_min           2.792
_diffrn_ambient_temperature        296.15
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.982
_diffrn_measured_fraction_theta_max  0.951
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.865
_reflns_Friedel_fraction_full      0.981
_reflns_Friedel_fraction_max       0.914
_reflns_number_gt                  5364
_reflns_number_total               6225
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max           0.174
_refine_diff_density_min           -0.163
_refine_diff_density_rms           0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 2189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     -0.02(8)
_refine_ls_extinction_coef         0.0121(15)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.015
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       470
_refine_ls_number_reflns           6225
_refine_ls_number_restraints       97
_refine_ls_R_factor_all            0.0513
_refine_ls_R_factor_gt             0.0420
_refine_ls_restrained_S_all        1.013
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0554P)²+0.2517P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1052
_refine_ls_wR_factor_ref           0.1116
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C9B, C7B, C8B, C10B, C6B, C5B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6A, C5A, C10A, C7A, C8A, C9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C9B \\sim C7B \\sim C8B \\sim C10B \\sim C6B \\sim C5B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C6A \\sim C5A \\sim C10A \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=Sof(C9B)=Sof(H9B)=Sof(C7B)=Sof(H7B)=
 Sof(C8B)=Sof(H8B)=Sof(C10B)=Sof(H10B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=
 Sof(H8A)=Sof(C7A)=Sof(H7A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C32(H32A,H32B), C11(H11A,H11B), C20(H20A,H20B), C13(H13A,H13B),
 C30(H30A,H30B)
5.c Me refined with riding coordinates:
 C4B(H4BA,H4BB,H4BC)
5.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C6A(H6A), C10A(H10A), C9A(H9A), C8A(H8A), C7A(H7A), C26(H26),
 C29(H29), C38(H38), C25(H25), C28(H28), C18(H18), C36(H36), C35(H35), C34(H34),
  C16(H16), C19(H19), C27(H27), C17(H17), C37(H37), C9B(H9B), C7B(H7B),
 C8B(H8B), C10B(H10B), C6B(H6B)
5.e Fitted hexagon refined as free rotating group:
 C6A(C5A,C10A,C9A,C8A,C7A)
5.f Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C4A(H4AA,H4AB,H4AC)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 O3 O 0.7630(2) 0.64524(16) 0.71120(12) 0.0484(5) Uani 1 1 d . . . . .
 O2 O 0.2932(3) 0.6154(3) 0.77292(15) 0.0808(8) Uani 1 1 d . . . . .
 O1 O 0.7039(3) 0.31545(19) 0.77805(13) 0.0660(6) Uani 1 1 d . . . . .
 N4 N 0.8503(2) 0.4796(2) 0.65369(13) 0.0439(5) Uani 1 1 d . . . . .
 N3 N 0.4635(2) 0.5857(2) 0.67635(14) 0.0472(5) Uani 1 1 d . . . . .
 C21 C 0.7393(3) 0.5544(2) 0.67184(14) 0.0387(5) Uani 1 1 d . . . . .
 C12 C 0.3991(3) 0.5581(3) 0.74914(18) 0.0573(8) Uani 1 1 d . . . . .
 N2 N 0.6155(3) 0.4793(2) 0.83599(13) 0.0536(6) Uani 1 1 d . . . . .
 N1 N 1.0005(4) 0.3704(3) 0.81418(17) 0.0686(8) Uani 1 1 d . . . . .
 C33 C 0.8891(3) 0.4023(3) 0.51101(18) 0.0521(7) Uani 1 1 d . . . . .
 C1 C 0.8849(4) 0.4460(3) 0.84481(17) 0.0576(8) Uani 1 1 d . . . . .
 H1A H 0.899069 0.524890 0.824060 0.069 Uiso 1 1 calc R . . . .
 H1B H 0.896115 0.448591 0.906039 0.069 Uiso 1 1 calc R . . . .
 C2 C 0.7276(4) 0.4060(3) 0.81761(16) 0.0531(7) Uani 1 1 d . . . . .
 C32 C 0.8309(3) 0.3793(3) 0.59661(18) 0.0506(7) Uani 1 1 d . . . . .
 H32A H 0.725315 0.359820 0.589315 0.061 Uiso 1 1 calc R . . . .
 H32B H 0.882989 0.312252 0.622119 0.061 Uiso 1 1 calc R . . . .
 C11 C 0.4623(4) 0.4571(3) 0.80307(19) 0.0632(8) Uani 1 1 d . . . . .
 H11A H 0.399848 0.444715 0.849884 0.076 Uiso 1 1 calc R . . . .
 H11B H 0.459699 0.386161 0.769348 0.076 Uiso 1 1 calc R . . . .
 C20 C 0.5800(3) 0.5142(2) 0.64436(15) 0.0413(6) Uani 1 1 d . . . . .
 H20A H 0.568204 0.514181 0.583113 0.050 Uiso 1 1 calc R . . . .
 H20B H 0.567361 0.434265 0.663277 0.050 Uiso 1 1 calc R . . . .
 C15 C 0.6404(5) 0.4529(3) 1.0244(2) 0.0764(11) Uani 1 1 d . . . . .
 H15 H 0.699787 0.399814 0.997402 0.092 Uiso 1 1 calc R . . . .
 C6A C 1.1129(15) 0.3376(12) 0.9979(7) 0.088(4) Uani 0.531(15) 1 d . U P A 1
 H6A H 1.183133 0.386015 0.975001 0.106 Uiso 0.531(15) 1 calc R . P A 1
 C5A C 1.0242(14) 0.2640(12) 0.9457(4) 0.057(4) Uani 0.531(15) 1 d G U P A 1
 C10A C 0.9192(10) 0.1917(8) 0.9800(6) 0.077(2) Uani 0.531(15) 1 d G U P A 1
 H10A H 0.859925 0.142420 0.945020 0.092 Uiso 0.531(15) 1 calc R . P A 1
 C9A C 0.9029(13) 0.1929(10) 1.0665(7) 0.107(4) Uani 0.531(15) 1 d G U P A 1
 H9A H 0.832626 0.144494 1.089397 0.128 Uiso 0.531(15) 1 calc R . P A 1
 C8A C 0.9915(18) 0.2665(12) 1.1187(4) 0.125(6) Uani 0.531(15) 1 d G U P A 1
 H8A H 0.980580 0.267328 1.176578 0.150 Uiso 0.531(15) 1 calc R . P A 1
 C7A C 1.0965(16) 0.3388(10) 1.0844(6) 0.117(4) Uani 0.531(15) 1 d G U P A 1
 H7A H 1.155834 0.388089 1.119382 0.141 Uiso 0.531(15) 1 calc R . P A 1
 O4 O 1.1604(3) 0.3356(3) 0.7143(2) 0.1069(11) Uani 1 1 d . . . . .
 C13 C 0.6332(4) 0.5796(3) 0.89354(17) 0.0547(7) Uani 1 1 d . . . . .
 H13A H 0.572852 0.644099 0.870519 0.066 Uiso 1 1 calc R . . . .
 H13B H 0.737069 0.604505 0.896874 0.066 Uiso 1 1 calc R . . . .
 C26 C 0.3854(7) 0.6084(5) 0.3974(3) 0.0994(16) Uani 1 1 d . . . . .
 H26 H 0.327633 0.560922 0.360385 0.119 Uiso 1 1 calc R . . . .
 C29 C 0.5562(4) 0.7462(3) 0.5064(2) 0.0720(9) Uani 1 1 d . . . . .
 H29 H 0.615507 0.793427 0.542819 0.086 Uiso 1 1 calc R . . . .
 C38 C 0.9742(4) 0.3201(4) 0.4725(2) 0.0762(10) Uani 1 1 d . . . . .
 H38 H 1.000340 0.250679 0.500404 0.091 Uiso 1 1 calc R . . . .
 C25 C 0.3524(4) 0.6157(3) 0.4816(2) 0.0733(10) Uani 1 1 d . . . . .
 H25 H 0.272025 0.574071 0.500587 0.088 Uiso 1 1 calc R . . . .
 C24 C 0.4396(3) 0.6854(3) 0.53713(19) 0.0558(7) Uani 1 1 d . . . . .
 C22 C 0.4047(3) 0.6906(3) 0.62892(18) 0.0577(7) Uani 1 1 d . . . . .
 H22 H 0.295384 0.688124 0.629881 0.069 Uiso 1 1 calc R . . . .
 C30 C 1.0037(3) 0.4992(3) 0.68807(18) 0.0524(7) Uani 1 1 d . . . . .
 H30A H 1.007370 0.568980 0.722982 0.063 Uiso 1 1 calc R . . . .
 H30B H 1.067946 0.511706 0.642082 0.063 Uiso 1 1 calc R . . . .
 C23 C 0.4558(6) 0.8019(4) 0.6742(3) 0.0873(12) Uani 1 1 d . . . . .
 H23A H 0.420698 0.802226 0.730028 0.131 Uiso 1 1 calc GR . . . .
 H23B H 0.415911 0.868514 0.643340 0.131 Uiso 1 1 calc GR . . . .
 H23C H 0.563177 0.805464 0.677892 0.131 Uiso 1 1 calc GR . . . .
 C14 C 0.5882(4) 0.5527(3) 0.98159(18) 0.0582(7) Uani 1 1 d . . . . .
 C31 C 1.0614(3) 0.3943(3) 0.7410(2) 0.0616(8) Uani 1 1 d . . . . .
 C28 C 0.5875(6) 0.7388(4) 0.4227(3) 0.0928(14) Uani 1 1 d . . . . .
 H28 H 0.667136 0.780706 0.403102 0.111 Uiso 1 1 calc R . . . .
 C18 C 0.4682(7) 0.6083(5) 1.1064(3) 0.1110(18) Uani 1 1 d . . . . .
 H18 H 0.411453 0.662034 1.134503 0.133 Uiso 1 1 calc R . . . .
 C36 C 0.9839(6) 0.4408(5) 0.3503(3) 0.1011(15) Uani 1 1 d . . . . .
 H36 H 1.014738 0.453073 0.296168 0.121 Uiso 1 1 calc R . . . .
 C35 C 0.9012(6) 0.5239(5) 0.3877(3) 0.0970(14) Uani 1 1 d . . . . .
 H35 H 0.876687 0.593597 0.359758 0.116 Uiso 1 1 calc R . . . .
 C34 C 0.8544(4) 0.5033(4) 0.4672(2) 0.0749(10) Uani 1 1 d . . . . .
 H34 H 0.797129 0.559976 0.492137 0.090 Uiso 1 1 calc R . . . .
 C16 C 0.6056(6) 0.4312(4) 1.1064(2) 0.0940(14) Uani 1 1 d . . . . .
 H16 H 0.642119 0.364657 1.134580 0.113 Uiso 1 1 calc R . . . .
 C19 C 0.5037(5) 0.6301(4) 1.0233(2) 0.0857(12) Uani 1 1 d . . . . .
 H19 H 0.469393 0.698183 0.996186 0.103 Uiso 1 1 calc R . . . .
 C27 C 0.5012(8) 0.6699(5) 0.3688(3) 0.1072(19) Uani 1 1 d . . . . .
 H27 H 0.521843 0.665067 0.312285 0.129 Uiso 1 1 calc R . . . .
 C17 C 0.5169(7) 0.5085(5) 1.1458(3) 0.1157(19) Uani 1 1 d . . . . .
 H17 H 0.489711 0.492529 1.200189 0.139 Uiso 1 1 calc R . . . .
 C3 C 1.0190(6) 0.2559(4) 0.8596(3) 0.1041(17) Uani 1 1 d . . . . .
 H3 H 0.941764 0.200154 0.838929 0.125 Uiso 1 1 calc R . . A 1
 C37 C 1.0212(5) 0.3404(5) 0.3921(3) 0.0994(15) Uani 1 1 d . . . . .
 H37 H 1.078814 0.284432 0.366785 0.119 Uiso 1 1 calc R . . . .
 C4A C 1.1956(17) 0.2034(13) 0.8425(6) 0.112(5) Uani 0.531(15) 1 d . . P A 1
 H4AA H 1.202881 0.190127 0.783145 0.168 Uiso 0.531(15) 1 calc GR . P A 1
 H4AB H 1.212364 0.131104 0.872581 0.168 Uiso 0.531(15) 1 calc GR . P A 1
 H4AC H 1.269522 0.259722 0.862211 0.168 Uiso 0.531(15) 1 calc GR . P A 1
 C4B C 1.077(2) 0.1560(11) 0.8363(6) 0.106(5) Uani 0.469(15) 1 d . . P A 2
 H4BA H 1.071412 0.099563 0.880885 0.159 Uiso 0.469(15) 1 calc R . P A 2
 H4BB H 1.021964 0.127726 0.786333 0.159 Uiso 0.469(15) 1 calc R . P A 2
 H4BC H 1.179749 0.167735 0.824779 0.159 Uiso 0.469(15) 1 calc R . P A 2
 C9B C 0.987(3) 0.253(3) 1.1057(13) 0.137(7) Uani 0.469(15) 1 d . U P A 2
 H9B H 0.930440 0.218928 1.146233 0.164 Uiso 0.469(15) 1 calc R . P A 2
 C7B C 1.202(2) 0.3711(14) 1.0682(9) 0.120(5) Uani 0.469(15) 1 d . U P A 2
 H7B H 1.286868 0.415508 1.081982 0.144 Uiso 0.469(15) 1 calc R . P A 2
 C8B C 1.116(3) 0.3272(17) 1.1286(8) 0.136(7) Uani 0.469(15) 1 d . U P A 2
 H8B H 1.140404 0.344649 1.185132 0.163 Uiso 0.469(15) 1 calc R . P A 2
 C10B C 0.9542(14) 0.2376(14) 1.0242(10) 0.100(5) Uani 0.469(15) 1 d . U P A 2
 H10B H 0.869974 0.192765 1.008896 0.120 Uiso 0.469(15) 1 calc R . P A 2
 C5B C 1.0323(18) 0.2811(16) 0.9596(9) 0.052(3) Uani 0.469(15) 1 d . U P A 2
 C6B C 1.155(2) 0.3461(17) 0.9855(10) 0.081(3) Uani 0.469(15) 1 d . U P A 2
 H6B H 1.211886 0.376217 0.943684 0.098 Uiso 0.469(15) 1 calc R . P A 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 O3 C21 1.222(3) . ?
 O2 C12 1.232(4) . ?
 O1 C2 1.220(4) . ?
 N4 C21 1.356(3) . ?
 N4 C32 1.463(4) . ?
 N4 C30 1.460(3) . ?
 N3 C12 1.362(4) . ?
 N3 C20 1.444(3) . ?
 N3 C22 1.492(4) . ?
 C21 C20 1.533(3) . ?
 C12 C11 1.522(5) . ?
 N2 C2 1.354(4) . ?
 N2 C11 1.456(4) . ?
 N2 C13 1.467(4) . ?
 N1 C1 1.457(4) . ?
 N1 C31 1.344(5) . ?
 N1 C3 1.497(5) . ?
 C33 C32 1.511(4) . ?
 C33 C38 1.378(4) . ?
 C33 C34 1.372(5) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.514(5) . ?
 C32 H32A 0.9700 . ?
 C32 H32B 0.9700 . ?
 C11 H11A 0.9700 . ?
 C11 H11B 0.9700 . ?
 C20 H20A 0.9700 . ?
 C20 H20B 0.9700 . ?
 C15 H15 0.9300 . ?
 C15 C14 1.391(5) . ?
 C15 C16 1.380(5) . ?
 C6A H6A 0.9300 . ?
 C6A C5A 1.3900 . ?
 C6A C7A 1.3900 . ?
 C5A C10A 1.3900 . ?
 C5A C3 1.366(9) . ?
 C10A H10A 0.9300 . ?
 C10A C9A 1.3900 . ?
 C9A H9A 0.9300 . ?
 C9A C8A 1.3900 . ?
 C8A H8A 0.9300 . ?
 C8A C7A 1.3900 . ?
 C7A H7A 0.9300 . ?
 O4 C31 1.211(4) . ?
 C13 H13A 0.9700 . ?
 C13 H13B 0.9700 . ?
 C13 C14 1.512(4) . ?
 C26 H26 0.9300 . ?
 C26 C25 1.389(6) . ?
 C26 C27 1.356(8) . ?
 C29 H29 0.9300 . ?
 C29 C24 1.371(5) . ?
 C29 C28 1.378(6) . ?
 C38 H38 0.9300 . ?
 C38 C37 1.388(6) . ?
 C25 H25 0.9300 . ?
 C25 C24 1.387(5) . ?
 C24 C22 1.511(4) . ?
 C22 H22 0.9800 . ?
 C22 C23 1.514(5) . ?
 C30 H30A 0.9700 . ?
 C30 H30B 0.9700 . ?
 C30 C31 1.532(5) . ?
 C23 H23A 0.9600 . ?
 C23 H23B 0.9600 . ?
 C23 H23C 0.9600 . ?
 C14 C19 1.364(5) . ?
 C28 H28 0.9300 . ?
 C28 C27 1.361(8) . ?
 C18 H18 0.9300 . ?
 C18 C19 1.400(6) . ?
 C18 C17 1.358(7) . ?
 C36 H36 0.9300 . ?
 C36 C35 1.364(7) . ?
 C36 C37 1.355(8) . ?
 C35 H35 0.9300 . ?
 C35 C34 1.377(5) . ?
 C34 H34 0.9300 . ?
 C16 H16 0.9300 . ?
 C16 C17 1.366(6) . ?
 C19 H19 0.9300 . ?
 C27 H27 0.9300 . ?
 C17 H17 0.9300 . ?
 C3 H3 0.9800 . ?
 C3 C4A 1.730(12) . ?
 C3 C4B 1.317(13) . ?
 C3 C5B 1.608(16) . ?
 C37 H37 0.9300 . ?
 C4A H4AA 0.9600 . ?
 C4A H4AB 0.9600 . ?
 C4A H4AC 0.9600 . ?
 C4B H4BA 0.9600 . ?
 C4B H4BB 0.9600 . ?
 C4B H4BC 0.9600 . ?
 C9B H9B 0.9300 . ?
 C9B C8B 1.46(3) . ?
 C9B C10B 1.32(2) . ?
 C7B H7B 0.9300 . ?
 C7B C8B 1.36(2) . ?
 C7B C6B 1.379(16) . ?
 C8B H8B 0.9300 . ?
 C10B H10B 0.9300 . ?
 C10B C5B 1.373(12) . ?
 C5B C6B 1.364(17) . ?
 C6B H6B 0.9300 . ?

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
 C21 N4 C32 124.5(2) . . ?
 C21 N4 C30 120.6(2) . . ?
 C30 N4 C32 114.8(2) . . ?
 C12 N3 C20 121.7(2) . . ?
 C12 N3 C22 117.2(2) . . ?
 C20 N3 C22 121.0(2) . . ?
 O3 C21 N4 122.6(2) . . ?
 O3 C21 C20 121.7(2) . . ?
 N4 C21 C20 115.6(2) . . ?
 O2 C12 N3 121.1(3) . . ?
 O2 C12 C11 119.6(3) . . ?
 N3 C12 C11 119.2(3) . . ?
 C2 N2 C11 120.6(3) . . ?
 C2 N2 C13 124.5(2) . . ?
 C11 N2 C13 114.7(3) . . ?
 C1 N1 C3 114.5(3) . . ?
 C31 N1 C1 120.5(3) . . ?
 C31 N1 C3 123.7(4) . . ?
 C38 C33 C32 121.0(3) . . ?
 C34 C33 C32 121.4(3) . . ?
 C34 C33 C38 117.5(3) . . ?
 N1 C1 H1A 108.9 . . ?
 N1 C1 H1B 108.9 . . ?
 N1 C1 C2 113.2(3) . . ?
 H1A C1 H1B 107.8 . . ?
 C2 C1 H1A 108.9 . . ?
 C2 C1 H1B 108.9 . . ?
 O1 C2 N2 121.9(3) . . ?
 O1 C2 C1 121.9(3) . . ?
 N2 C2 C1 116.1(3) . . ?
 N4 C32 C33 112.7(2) . . ?
 N4 C32 H32A 109.0 . . ?
 N4 C32 H32B 109.0 . . ?
 C33 C32 H32A 109.0 . . ?
 C33 C32 H32B 109.0 . . ?
 H32A C32 H32B 107.8 . . ?
 C12 C11 H11A 109.2 . . ?
 C12 C11 H11B 109.2 . . ?
 N2 C11 C12 112.0(2) . . ?
 N2 C11 H11A 109.2 . . ?
 N2 C11 H11B 109.2 . . ?
 H11A C11 H11B 107.9 . . ?
 N3 C20 C21 114.3(2) . . ?
 N3 C20 H20A 108.7 . . ?
 N3 C20 H20B 108.7 . . ?
 C21 C20 H20A 108.7 . . ?
 C21 C20 H20B 108.7 . . ?
 H20A C20 H20B 107.6 . . ?
 C14 C15 H15 119.4 . . ?
 C16 C15 H15 119.4 . . ?
 C16 C15 C14 121.1(4) . . ?
 C5A C6A H6A 120.0 . . ?
 C5A C6A C7A 120.0 . . ?
 C7A C6A H6A 120.0 . . ?
 C10A C5A C6A 120.0 . . ?
 C3 C5A C6A 128.0(7) . . ?
 C3 C5A C10A 111.9(6) . . ?
 C5A C10A H10A 120.0 . . ?
 C5A C10A C9A 120.0 . . ?
 C9A C10A H10A 120.0 . . ?
 C10A C9A H9A 120.0 . . ?
 C10A C9A C8A 120.0 . . ?
 C8A C9A H9A 120.0 . . ?
 C9A C8A H8A 120.0 . . ?
 C7A C8A C9A 120.0 . . ?
 C7A C8A H8A 120.0 . . ?
 C6A C7A H7A 120.0 . . ?
 C8A C7A C6A 120.0 . . ?
 C8A C7A H7A 120.0 . . ?
 N2 C13 H13A 109.0 . . ?
 N2 C13 H13B 109.0 . . ?
 N2 C13 C14 113.1(2) . . ?
 H13A C13 H13B 107.8 . . ?
 C14 C13 H13A 109.0 . . ?
 C14 C13 H13B 109.0 . . ?
 C25 C26 H26 119.7 . . ?
 C27 C26 H26 119.7 . . ?
 C27 C26 C25 120.5(5) . . ?
 C24 C29 H29 119.3 . . ?
 C24 C29 C28 121.5(4) . . ?
 C28 C29 H29 119.3 . . ?
 C33 C38 H38 119.8 . . ?
 C33 C38 C37 120.3(4) . . ?
 C37 C38 H38 119.8 . . ?
 C26 C25 H25 120.1 . . ?
 C24 C25 C26 119.8(4) . . ?
 C24 C25 H25 120.1 . . ?
 C29 C24 C25 118.3(4) . . ?
 C29 C24 C22 122.4(3) . . ?
 C25 C24 C22 119.3(3) . . ?
 N3 C22 C24 111.4(2) . . ?
 N3 C22 H22 106.7 . . ?
 N3 C22 C23 110.5(3) . . ?
 C24 C22 H22 106.7 . . ?
 C24 C22 C23 114.5(3) . . ?
 C23 C22 H22 106.7 . . ?
 N4 C30 H30A 109.4 . . ?
 N4 C30 H30B 109.4 . . ?
 N4 C30 C31 111.0(2) . . ?
 H30A C30 H30B 108.0 . . ?
 C31 C30 H30A 109.4 . . ?
 C31 C30 H30B 109.4 . . ?
 C22 C23 H23A 109.5 . . ?
 C22 C23 H23B 109.5 . . ?
 C22 C23 H23C 109.5 . . ?
 H23A C23 H23B 109.5 . . ?
 H23A C23 H23C 109.5 . . ?
 H23B C23 H23C 109.5 . . ?
 C15 C14 C13 121.1(3) . . ?
 C19 C14 C15 118.2(3) . . ?
 C19 C14 C13 120.5(3) . . ?
 N1 C31 C30 119.4(3) . . ?
 O4 C31 N1 122.7(3) . . ?
 O4 C31 C30 117.9(3) . . ?
 C29 C28 H28 120.1 . . ?
 C27 C28 C29 119.7(5) . . ?
 C27 C28 H28 120.1 . . ?
 C19 C18 H18 120.1 . . ?
 C17 C18 H18 120.1 . . ?
 C17 C18 C19 119.8(4) . . ?
 C35 C36 H36 120.1 . . ?
 C37 C36 H36 120.1 . . ?
 C37 C36 C35 119.9(4) . . ?
 C36 C35 H35 120.4 . . ?
 C36 C35 C34 119.3(5) . . ?
 C34 C35 H35 120.4 . . ?
 C33 C34 C35 122.3(4) . . ?
 C33 C34 H34 118.8 . . ?
 C35 C34 H34 118.8 . . ?
 C15 C16 H16 120.3 . . ?
 C17 C16 C15 119.5(4) . . ?
 C17 C16 H16 120.3 . . ?
 C14 C19 C18 120.7(4) . . ?
 C14 C19 H19 119.6 . . ?
 C18 C19 H19 119.6 . . ?
 C26 C27 C28 120.2(4) . . ?
 C26 C27 H27 119.9 . . ?
 C28 C27 H27 119.9 . . ?
 C18 C17 C16 120.6(4) . . ?
 C18 C17 H17 119.7 . . ?
 C16 C17 H17 119.7 . . ?
 N1 C3 H3 110.7 . . ?
 N1 C3 C4A 107.4(6) . . ?
 N1 C3 C5B 108.5(7) . . ?
 C5A C3 N1 114.7(7) . . ?
 C5A C3 H3 110.7 . . ?
 C5A C3 C4A 102.2(8) . . ?
 C4A C3 H3 110.7 . . ?
 C4B C3 N1 130.9(7) . . ?
 C4B C3 C5B 115.3(9) . . ?
 C38 C37 H37 119.6 . . ?
 C36 C37 C38 120.7(4) . . ?
 C36 C37 H37 119.6 . . ?
 C3 C4A H4AA 109.5 . . ?
 C3 C4A H4AB 109.5 . . ?
 C3 C4A H4AC 109.5 . . ?
 H4AA C4A H4AB 109.5 . . ?
 H4AA C4A H4AC 109.5 . . ?
 H4AB C4A H4AC 109.5 . . ?
 C3 C4B H4BA 109.5 . . ?
 C3 C4B H4BB 109.5 . . ?
 C3 C4B H4BC 109.5 . . ?
 H4BA C4B H4BB 109.5 . . ?
 H4BA C4B H4BC 109.5 . . ?
 H4BB C4B H4BC 109.5 . . ?
 C8B C9B H9B 121.9 . . ?
 C10B C9B H9B 121.9 . . ?
 C10B C9B C8B 116.1(15) . . ?
 C8B C7B H7B 121.8 . . ?
 C8B C7B C6B 116.4(16) . . ?
 C6B C7B H7B 121.8 . . ?
 C9B C8B H8B 119.6 . . ?
 C7B C8B C9B 120.8(15) . . ?
 C7B C8B H8B 119.6 . . ?
 C9B C10B H10B 116.8 . . ?
 C9B C10B C5B 126.5(15) . . ?
 C5B C10B H10B 116.8 . . ?
 C10B C5B C3 131.6(13) . . ?
 C6B C5B C3 113.4(10) . . ?
 C6B C5B C10B 114.4(14) . . ?
 C7B C6B H6B 117.1 . . ?
 C5B C6B C7B 125.7(16) . . ?
 C5B C6B H6B 117.1 . . ?

_olex2_submission_special_instructions  'No special instructions were received'


#===END
data_tbe267_1_0m_a
_audit_creation_date               2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C60 H66 N6 O6'
_chemical_formula_sum              'C60 H66 N6 O6'
_chemical_formula_weight           967.18
_chemical_absolute_configuration   'ad'
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             4
_space_group_name_H-M_alt          'P 1 21 1'
_space_group_name_Hall             'P 2yb'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'

_cell_length_a                     10.962(4)
_cell_length_b                     19.047(5)
_cell_length_c                     12.850(4)
_cell_angle_alpha                  90
_cell_angle_beta                   97.523(17)
_cell_angle_gamma                  90
_cell_volume                       2659.9(16)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      8332
_cell_measurement_temperature      296(2)
_cell_measurement_theta_max        72.28
_cell_measurement_theta_min        3.45
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.624
_exptl_absorpt_correction_T_max    0.7536
_exptl_absorpt_correction_T_min    0.6835
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1342 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.9070.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'colorless'
_exptl_crystal_density_diffrn      1.208
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'prism'
_exptl_crystal_F_000               1032
_exptl_crystal_size_max            0.37
_exptl_crystal_size_mid            0.25
_exptl_crystal_size_min            0.21
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0322
_diffrn_reflns_av_unetI/netI       0.0345
_diffrn_reflns_Laue_measured_fraction_full  0.980
_diffrn_reflns_Laue_measured_fraction_max  0.965
_diffrn_reflns_limit_h_max         11
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         23
_diffrn_reflns_limit_k_min         -23
_diffrn_reflns_limit_l_max         15
_diffrn_reflns_limit_l_min         -15
_diffrn_reflns_number              34865
_diffrn_reflns_point_group_measured_fraction_full  0.972
_diffrn_reflns_point_group_measured_fraction_max  0.947
_diffrn_reflns_theta_full          67.679
_diffrn_reflns_theta_max           72.585
_diffrn_reflns_theta_min           3.469
_diffrn_ambient_temperature        296.15
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.980
_diffrn_measured_fraction_theta_max  0.965
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.902
_reflns_Friedel_fraction_full      0.962
_reflns_Friedel_fraction_max       0.927
_reflns_number_gt                  9465
_reflns_number_total               10023
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max           0.149
_refine_diff_density_min           -0.118
_refine_diff_density_rms           0.022
_refine_ls_abs_structure_details
;
 Flack x determined using 4236 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     0.04(7)
_refine_ls_extinction_coef         0.0117(11)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.024
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       656
_refine_ls_number_reflns           10023
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0371
_refine_ls_R_factor_gt             0.0347
_refine_ls_restrained_S_all        1.024
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0479P)²+0.2361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0900
_refine_ls_wR_factor_ref           0.0919
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C13(H13), C23(H23), C33(H33), C43(H43), C53(H53)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C21(H21A,H21B), C31(H31A,H31B), C41(H41A,H41B),
 C51(H51A,H51B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C34(H34A,H34B,
 H34C), C44(H44A,H44B,H44C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 C1 C 0.49022(19) 0.50642(11) 0.37198(16) 0.0438(4) Uani 1 1 d . . . . .
 H1A H 0.438012 0.541227 0.333188 0.053 Uiso 1 1 calc R . . . .
 H1B H 0.439224 0.477976 0.411686 0.053 Uiso 1 1 calc R . . . .
 C2 C 0.54875(18) 0.45966(10) 0.29494(16) 0.0405(4) Uani 1 1 d . . . . .
 C3 C 0.6281(2) 0.50295(12) 0.54176(16) 0.0502(5) Uani 1 1 d . . . . .
 H3 H 0.597585 0.454870 0.530046 0.060 Uiso 1 1 calc R . . . .
 C4 C 0.7671(3) 0.49634(18) 0.5648(2) 0.0713(8) Uani 1 1 d . . . . .
 H4A H 0.799840 0.483129 0.501874 0.107 Uiso 1 1 calc GR . . . .
 H4B H 0.787770 0.461141 0.617645 0.107 Uiso 1 1 calc GR . . . .
 H4C H 0.801631 0.540567 0.589438 0.107 Uiso 1 1 calc GR . . . .
 C5 C 0.5707(2) 0.52963(12) 0.63495(16) 0.0475(5) Uani 1 1 d . . . . .
 C6 C 0.5619(2) 0.60049(13) 0.65720(19) 0.0565(5) Uani 1 1 d . . . . .
 H6 H 0.590372 0.633574 0.612944 0.068 Uiso 1 1 calc R . . . .
 C7 C 0.5110(3) 0.62243(17) 0.7446(2) 0.0705(7) Uani 1 1 d . . . . .
 H7 H 0.505245 0.670137 0.758559 0.085 Uiso 1 1 calc R . . . .
 C8 C 0.4694(3) 0.5747(2) 0.8103(2) 0.0800(9) Uani 1 1 d . . . . .
 H8 H 0.435855 0.589719 0.869353 0.096 Uiso 1 1 calc R . . . .
 C9 C 0.4771(3) 0.5049(2) 0.7895(2) 0.0794(8) Uani 1 1 d . . . . .
 H9 H 0.447910 0.472315 0.834152 0.095 Uiso 1 1 calc R . . . .
 C10 C 0.5280(2) 0.48175(15) 0.7019(2) 0.0623(6) Uani 1 1 d . . . . .
 H10 H 0.533255 0.433925 0.688669 0.075 Uiso 1 1 calc R . . . .
 C11 C 0.54889(19) 0.40175(12) 0.13169(17) 0.0454(4) Uani 1 1 d . . . . .
 H11A H 0.616499 0.430478 0.114447 0.055 Uiso 1 1 calc R . . . .
 H11B H 0.494651 0.392506 0.067267 0.055 Uiso 1 1 calc R . . . .
 C12 C 0.59906(19) 0.33273(11) 0.17858(18) 0.0473(5) Uani 1 1 d . . . . .
 C13 C 0.35177(19) 0.46005(13) 0.16897(18) 0.0495(5) Uani 1 1 d . . . . .
 H13 H 0.321550 0.484517 0.227626 0.059 Uiso 1 1 calc R . . . .
 C14 C 0.3457(3) 0.51195(17) 0.0791(2) 0.0750(8) Uani 1 1 d . . . . .
 H14A H 0.392200 0.553138 0.101800 0.113 Uiso 1 1 calc GR . . . .
 H14B H 0.261513 0.524738 0.057266 0.113 Uiso 1 1 calc GR . . . .
 H14C H 0.379472 0.490857 0.021354 0.113 Uiso 1 1 calc GR . . . .
 C15 C 0.27390(19) 0.39485(14) 0.14769(19) 0.0556(6) Uani 1 1 d . . . . .
 C16 C 0.2463(3) 0.3565(2) 0.2327(3) 0.0862(10) Uani 1 1 d . . . . .
 H16 H 0.272027 0.373206 0.299994 0.103 Uiso 1 1 calc R . . . .
 C17 C 0.1824(4) 0.2950(3) 0.2210(5) 0.1238(17) Uani 1 1 d . . . . .
 H17 H 0.164333 0.270383 0.279585 0.149 Uiso 1 1 calc R . . . .
 C18 C 0.1452(4) 0.2699(3) 0.1227(7) 0.133(2) Uani 1 1 d . . . . .
 H18 H 0.104896 0.226875 0.114300 0.160 Uiso 1 1 calc R . . . .
 C19 C 0.1668(4) 0.3078(3) 0.0355(5) 0.1198(18) Uani 1 1 d . . . . .
 H19 H 0.138575 0.291470 -0.031528 0.144 Uiso 1 1 calc R . . . .
 C20 C 0.2314(3) 0.3707(2) 0.0491(3) 0.0823(9) Uani 1 1 d . . . . .
 H20 H 0.245839 0.396609 -0.009355 0.099 Uiso 1 1 calc R . . . .
 C21 C 0.80328(19) 0.36490(11) 0.13382(16) 0.0442(4) Uani 1 1 d . . . . .
 H21A H 0.885210 0.345042 0.148508 0.053 Uiso 1 1 calc R . . . .
 H21B H 0.800694 0.406399 0.177220 0.053 Uiso 1 1 calc R . . . .
 C22 C 0.78167(18) 0.38702(11) 0.01901(17) 0.0452(4) Uani 1 1 d . . . . .
 C23 C 0.7603(2) 0.24429(12) 0.1969(2) 0.0568(6) Uani 1 1 d . . . . .
 H23 H 0.689349 0.218547 0.216525 0.068 Uiso 1 1 calc R . . . .
 C24 C 0.8012(3) 0.20510(18) 0.1037(3) 0.0841(9) Uani 1 1 d . . . . .
 H24A H 0.737883 0.208096 0.044745 0.126 Uiso 1 1 calc GR . . . .
 H24B H 0.816098 0.156722 0.122103 0.126 Uiso 1 1 calc GR . . . .
 H24C H 0.875467 0.225867 0.085630 0.126 Uiso 1 1 calc GR . . . .
 C25 C 0.8546(2) 0.24704(13) 0.2948(2) 0.0575(6) Uani 1 1 d . . . . .
 C26 C 0.8608(3) 0.30323(16) 0.3632(2) 0.0667(7) Uani 1 1 d . . . . .
 H26 H 0.808828 0.341399 0.347252 0.080 Uiso 1 1 calc R . . . .
 C27 C 0.9427(3) 0.3041(2) 0.4549(3) 0.0840(9) Uani 1 1 d . . . . .
 H27 H 0.945153 0.342546 0.499809 0.101 Uiso 1 1 calc R . . . .
 C28 C 1.0205(3) 0.2479(3) 0.4797(3) 0.0943(11) Uani 1 1 d . . . . .
 H28 H 1.076312 0.248565 0.540798 0.113 Uiso 1 1 calc R . . . .
 C29 C 1.0150(4) 0.1920(2) 0.4149(4) 0.0994(12) Uani 1 1 d . . . . .
 H29 H 1.066370 0.153756 0.432300 0.119 Uiso 1 1 calc R . . . .
 C30 C 0.9335(3) 0.19095(17) 0.3224(3) 0.0812(9) Uani 1 1 d . . . . .
 H30 H 0.931716 0.152137 0.278325 0.097 Uiso 1 1 calc R . . . .
 C31 C 0.93140(17) 0.48112(11) 0.06978(15) 0.0410(4) Uani 1 1 d . . . . .
 H31A H 0.988141 0.507797 0.033323 0.049 Uiso 1 1 calc R . . . .
 H31B H 0.978985 0.447535 0.115111 0.049 Uiso 1 1 calc R . . . .
 C32 C 0.86476(17) 0.53136(10) 0.13741(15) 0.0394(4) Uani 1 1 d . . . . .
 C33 C 0.8296(2) 0.47204(13) -0.11451(17) 0.0527(5) Uani 1 1 d . . . . .
 H33 H 0.760386 0.446663 -0.153531 0.063 Uiso 1 1 calc R . . . .
 C34 C 0.7945(3) 0.54912(15) -0.1157(2) 0.0712(7) Uani 1 1 d . . . . .
 H34A H 0.720530 0.554870 -0.083928 0.107 Uiso 1 1 calc GR . . . .
 H34B H 0.780910 0.565614 -0.186830 0.107 Uiso 1 1 calc GR . . . .
 H34C H 0.859748 0.575644 -0.076947 0.107 Uiso 1 1 calc GR . . . .
 C35 C 0.9427(2) 0.45528(13) -0.16632(17) 0.0556(5) Uani 1 1 d . . . . .
 C36 C 0.9618(4) 0.38776(17) -0.1974(3) 0.0812(9) Uani 1 1 d . . . . .
 H36 H 0.904924 0.352897 -0.187963 0.097 Uiso 1 1 calc R . . . .
 C37 C 1.0674(5) 0.3714(2) -0.2436(3) 0.1074(14) Uani 1 1 d . . . . .
 H37 H 1.079232 0.325727 -0.266041 0.129 Uiso 1 1 calc R . . . .
 C38 C 1.1527(5) 0.4217(3) -0.2559(3) 0.1106(15) Uani 1 1 d . . . . .
 H38 H 1.222446 0.410339 -0.286457 0.133 Uiso 1 1 calc R . . . .
 C39 C 1.1360(4) 0.4880(3) -0.2238(3) 0.1060(13) Uani 1 1 d . . . . .
 H39 H 1.194977 0.522138 -0.230934 0.127 Uiso 1 1 calc R . . . .
 C40 C 1.0316(3) 0.50490(18) -0.1806(3) 0.0818(9) Uani 1 1 d . . . . .
 H40 H 1.020178 0.551041 -0.160242 0.098 Uiso 1 1 calc R . . . .
 C41 C 0.86654(19) 0.60497(11) 0.28643(16) 0.0453(4) Uani 1 1 d . . . . .
 H41A H 0.924171 0.619027 0.346614 0.054 Uiso 1 1 calc R . . . .
 H41B H 0.809418 0.571753 0.310719 0.054 Uiso 1 1 calc R . . . .
 C42 C 0.7952(2) 0.66933(11) 0.24244(19) 0.0498(5) Uani 1 1 d . . . . .
 C43 C 1.06902(19) 0.57820(12) 0.21540(17) 0.0479(5) Uani 1 1 d . . . . .
 H43 H 1.097681 0.539204 0.175155 0.057 Uiso 1 1 calc R . . . .
 C44 C 1.1013(3) 0.64539(18) 0.1610(3) 0.0754(8) Uani 1 1 d . . . . .
 H44A H 1.059296 0.646159 0.090662 0.113 Uiso 1 1 calc GR . . . .
 H44B H 1.188564 0.647167 0.159227 0.113 Uiso 1 1 calc GR . . . .
 H44C H 1.076568 0.685222 0.198973 0.113 Uiso 1 1 calc GR . . . .
 C45 C 1.13127(19) 0.56991(13) 0.32711(17) 0.0496(5) Uani 1 1 d . . . . .
 C46 C 1.2047(3) 0.62154(18) 0.3789(2) 0.0709(7) Uani 1 1 d . . . . .
 H46 H 1.215745 0.663796 0.345072 0.085 Uiso 1 1 calc R . . . .
 C47 C 1.2614(3) 0.6112(3) 0.4795(3) 0.0917(11) Uani 1 1 d . . . . .
 H47 H 1.310389 0.646475 0.513034 0.110 Uiso 1 1 calc R . . . .
 C48 C 1.2470(3) 0.5510(3) 0.5295(3) 0.0995(14) Uani 1 1 d . . . . .
 H48 H 1.285574 0.544599 0.597702 0.119 Uiso 1 1 calc R . . . .
 C49 C 1.1757(4) 0.4987(3) 0.4810(3) 0.1022(12) Uani 1 1 d . . . . .
 H49 H 1.165534 0.456930 0.516162 0.123 Uiso 1 1 calc R . . . .
 C50 C 1.1182(3) 0.50810(18) 0.3785(2) 0.0748(8) Uani 1 1 d . . . . .
 H50 H 1.070800 0.472154 0.344989 0.090 Uiso 1 1 calc R . . . .
 C51 C 0.60633(18) 0.62083(11) 0.29769(16) 0.0427(4) Uani 1 1 d . . . . .
 H51A H 0.614415 0.580632 0.252765 0.051 Uiso 1 1 calc R . . . .
 H51B H 0.520393 0.634592 0.288451 0.051 Uiso 1 1 calc R . . . .
 C52 C 0.64322(18) 0.59880(11) 0.41209(16) 0.0414(4) Uani 1 1 d . . . . .
 C53 C 0.6125(3) 0.74368(13) 0.2293(2) 0.0616(6) Uani 1 1 d . . . . .
 H53 H 0.674821 0.779884 0.223853 0.074 Uiso 1 1 calc R . . . .
 C54 C 0.5414(4) 0.7342(2) 0.1200(3) 0.0949(11) Uani 1 1 d . . . . .
 H54A H 0.596905 0.719768 0.072171 0.142 Uiso 1 1 calc GR . . . .
 H54B H 0.503342 0.777801 0.096687 0.142 Uiso 1 1 calc GR . . . .
 H54C H 0.479144 0.698956 0.122371 0.142 Uiso 1 1 calc GR . . . .
 C55 C 0.5361(2) 0.76751(12) 0.3131(2) 0.0609(6) Uani 1 1 d . . . . .
 C56 C 0.5918(3) 0.77619(17) 0.4148(3) 0.0807(9) Uani 1 1 d . . . . .
 H56 H 0.676237 0.769250 0.429960 0.097 Uiso 1 1 calc R . . . .
 C57 C 0.5250(5) 0.7951(2) 0.4959(3) 0.0988(12) Uani 1 1 d . . . . .
 H57 H 0.564352 0.799577 0.564174 0.119 Uiso 1 1 calc R . . . .
 C58 C 0.4025(5) 0.8069(2) 0.4743(4) 0.1040(13) Uani 1 1 d . . . . .
 H58 H 0.357335 0.819393 0.527871 0.125 Uiso 1 1 calc R . . . .
 C59 C 0.3455(4) 0.80030(19) 0.3740(4) 0.0989(13) Uani 1 1 d . . . . .
 H59 H 0.261551 0.809095 0.359490 0.119 Uiso 1 1 calc R . . . .
 C60 C 0.4110(3) 0.78063(15) 0.2929(3) 0.0760(8) Uani 1 1 d . . . . .
 H60 H 0.370574 0.776285 0.224875 0.091 Uiso 1 1 calc R . . . .
 N1 N 0.58444(16) 0.54150(9) 0.44368(13) 0.0426(4) Uani 1 1 d . . . . .
 N2 N 0.48114(15) 0.44012(9) 0.20463(13) 0.0437(4) Uani 1 1 d . . . . .
 N3 N 0.71535(16) 0.31420(9) 0.16383(15) 0.0461(4) Uani 1 1 d . . . . .
 N4 N 0.84650(16) 0.44367(9) -0.00628(13) 0.0439(4) Uani 1 1 d . . . . .
 N5 N 0.93426(15) 0.56999(9) 0.21060(13) 0.0418(4) Uani 1 1 d . . . . .
 N6 N 0.67880(17) 0.67813(9) 0.26423(15) 0.0473(4) Uani 1 1 d . . . . .
 O1 O 0.65692(13) 0.44202(8) 0.31574(12) 0.0492(4) Uani 1 1 d . . . . .
 O2 O 0.53292(17) 0.29461(9) 0.22280(19) 0.0742(6) Uani 1 1 d . . . . .
 O3 O 0.71099(17) 0.35509(10) -0.04559(14) 0.0662(5) Uani 1 1 d . . . . .
 O4 O 0.75246(13) 0.53303(8) 0.12885(12) 0.0495(3) Uani 1 1 d . . . . .
 O5 O 0.8466(2) 0.71325(10) 0.1943(2) 0.0794(6) Uani 1 1 d . . . . .
 O6 O 0.72172(15) 0.63091(9) 0.46868(12) 0.0544(4) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.533(3) . ?
 C1 N1 1.454(3) . ?
 C2 N2 1.345(3) . ?
 C2 O1 1.228(3) . ?
 C3 H3 0.9800 . ?
 C3 C4 1.519(4) . ?
 C3 C5 1.512(3) . ?
 C3 N1 1.483(3) . ?
 C4 H4A 0.9600 . ?
 C4 H4B 0.9600 . ?
 C4 H4C 0.9600 . ?
 C5 C6 1.386(3) . ?
 C5 C10 1.377(4) . ?
 C6 H6 0.9300 . ?
 C6 C7 1.382(4) . ?
 C7 H7 0.9300 . ?
 C7 C8 1.359(5) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.362(5) . ?
 C9 H9 0.9300 . ?
 C9 C10 1.391(4) . ?
 C10 H10 0.9300 . ?
 C11 H11A 0.9700 . ?
 C11 H11B 0.9700 . ?
 C11 C12 1.519(3) . ?
 C11 N2 1.465(3) . ?
 C12 N3 1.360(3) . ?
 C12 O2 1.218(3) . ?
 C13 H13 0.9800 . ?
 C13 C14 1.515(4) . ?
 C13 C15 1.511(3) . ?
 C13 N2 1.481(3) . ?
 C14 H14A 0.9600 . ?
 C14 H14B 0.9600 . ?
 C14 H14C 0.9600 . ?
 C15 C16 1.379(4) . ?
 C15 C20 1.371(4) . ?
 C16 H16 0.9300 . ?
 C16 C17 1.364(6) . ?
 C17 H17 0.9300 . ?
 C17 C18 1.362(8) . ?
 C18 H18 0.9300 . ?
 C18 C19 1.379(8) . ?
 C19 H19 0.9300 . ?
 C19 C20 1.391(7) . ?
 C20 H20 0.9300 . ?
 C21 H21A 0.9700 . ?
 C21 H21B 0.9700 . ?
 C21 C22 1.523(3) . ?
 C21 N3 1.452(3) . ?
 C22 N4 1.355(3) . ?
 C22 O3 1.221(3) . ?
 C23 H23 0.9800 . ?
 C23 C24 1.528(4) . ?
 C23 C25 1.521(4) . ?
 C23 N3 1.464(3) . ?
 C24 H24A 0.9600 . ?
 C24 H24B 0.9600 . ?
 C24 H24C 0.9600 . ?
 C25 C26 1.381(4) . ?
 C25 C30 1.391(4) . ?
 C26 H26 0.9300 . ?
 C26 C27 1.385(4) . ?
 C27 H27 0.9300 . ?
 C27 C28 1.380(5) . ?
 C28 H28 0.9300 . ?
 C28 C29 1.348(7) . ?
 C29 H29 0.9300 . ?
 C29 C30 1.391(6) . ?
 C30 H30 0.9300 . ?
 C31 H31A 0.9700 . ?
 C31 H31B 0.9700 . ?
 C31 C32 1.540(3) . ?
 C31 N4 1.446(2) . ?
 C32 N5 1.349(3) . ?
 C32 O4 1.222(2) . ?
 C33 H33 0.9800 . ?
 C33 C34 1.517(4) . ?
 C33 C35 1.516(4) . ?
 C33 N4 1.481(3) . ?
 C34 H34A 0.9600 . ?
 C34 H34B 0.9600 . ?
 C34 H34C 0.9600 . ?
 C35 C36 1.371(4) . ?
 C35 C40 1.387(4) . ?
 C36 H36 0.9300 . ?
 C36 C37 1.403(5) . ?
 C37 H37 0.9300 . ?
 C37 C38 1.363(7) . ?
 C38 H38 0.9300 . ?
 C38 C39 1.347(7) . ?
 C39 H39 0.9300 . ?
 C39 C40 1.375(5) . ?
 C40 H40 0.9300 . ?
 C41 H41A 0.9700 . ?
 C41 H41B 0.9700 . ?
 C41 C42 1.522(3) . ?
 C41 N5 1.461(3) . ?
 C42 N6 1.352(3) . ?
 C42 O5 1.221(3) . ?
 C43 H43 0.9800 . ?
 C43 C44 1.522(4) . ?
 C43 C45 1.515(3) . ?
 C43 N5 1.479(3) . ?
 C44 H44A 0.9600 . ?
 C44 H44B 0.9600 . ?
 C44 H44C 0.9600 . ?
 C45 C46 1.385(4) . ?
 C45 C50 1.366(4) . ?
 C46 H46 0.9300 . ?
 C46 C47 1.373(5) . ?
 C47 H47 0.9300 . ?
 C47 C48 1.334(7) . ?
 C48 H48 0.9300 . ?
 C48 C49 1.364(7) . ?
 C49 H49 0.9300 . ?
 C49 C50 1.395(5) . ?
 C50 H50 0.9300 . ?
 C51 H51A 0.9700 . ?
 C51 H51B 0.9700 . ?
 C51 C52 1.531(3) . ?
 C51 N6 1.448(3) . ?
 C52 N1 1.356(3) . ?
 C52 O6 1.216(3) . ?
 C53 H53 0.9800 . ?
 C53 C54 1.525(5) . ?
 C53 C55 1.517(4) . ?
 C53 N6 1.485(3) . ?
 C54 H54A 0.9600 . ?
 C54 H54B 0.9600 . ?
 C54 H54C 0.9600 . ?
 C55 C56 1.378(5) . ?
 C55 C60 1.385(4) . ?
 C56 H56 0.9300 . ?
 C56 C57 1.396(5) . ?
 C57 H57 0.9300 . ?
 C57 C58 1.353(7) . ?
 C58 H58 0.9300 . ?
 C58 C59 1.363(7) . ?
 C59 H59 0.9300 . ?
 C59 C60 1.392(5) . ?
 C60 H60 0.9300 . ?

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
 H1A C1 H1B 108.1 . . ?
 C2 C1 H1A 109.5 . . ?
 C2 C1 H1B 109.5 . . ?
 N1 C1 H1A 109.5 . . ?
 N1 C1 H1B 109.5 . . ?
 N1 C1 C2 110.71(16) . . ?
 N2 C2 C1 119.20(17) . . ?
 O1 C2 C1 119.49(18) . . ?
 O1 C2 N2 121.30(18) . . ?
 C4 C3 H3 105.4 . . ?
 C5 C3 H3 105.4 . . ?
 C5 C3 C4 112.62(19) . . ?
 N1 C3 H3 105.4 . . ?
 N1 C3 C4 114.3(2) . . ?
 N1 C3 C5 112.65(17) . . ?
 C3 C4 H4A 109.5 . . ?
 C3 C4 H4B 109.5 . . ?
 C3 C4 H4C 109.5 . . ?
 H4A C4 H4B 109.5 . . ?
 H4A C4 H4C 109.5 . . ?
 H4B C4 H4C 109.5 . . ?
 C6 C5 C3 122.6(2) . . ?
 C10 C5 C3 118.9(2) . . ?
 C10 C5 C6 118.5(2) . . ?
 C5 C6 H6 119.7 . . ?
 C7 C6 C5 120.6(3) . . ?
 C7 C6 H6 119.7 . . ?
 C6 C7 H7 119.8 . . ?
 C8 C7 C6 120.4(3) . . ?
 C8 C7 H7 119.8 . . ?
 C7 C8 H8 120.1 . . ?
 C7 C8 C9 119.7(3) . . ?
 C9 C8 H8 120.1 . . ?
 C8 C9 H9 119.7 . . ?
 C8 C9 C10 120.7(3) . . ?
 C10 C9 H9 119.7 . . ?
 C5 C10 C9 120.1(3) . . ?
 C5 C10 H10 120.0 . . ?
 C9 C10 H10 120.0 . . ?
 H11A C11 H11B 108.0 . . ?
 C12 C11 H11A 109.3 . . ?
 C12 C11 H11B 109.3 . . ?
 N2 C11 H11A 109.3 . . ?
 N2 C11 H11B 109.3 . . ?
 N2 C11 C12 111.45(18) . . ?
 N3 C12 C11 117.83(18) . . ?
 O2 C12 C11 119.62(19) . . ?
 O2 C12 N3 122.4(2) . . ?
 C14 C13 H13 106.9 . . ?
 C15 C13 H13 106.9 . . ?
 C15 C13 C14 115.5(2) . . ?
 N2 C13 H13 106.9 . . ?
 N2 C13 C14 110.3(2) . . ?
 N2 C13 C15 109.91(18) . . ?
 C13 C14 H14A 109.5 . . ?
 C13 C14 H14B 109.5 . . ?
 C13 C14 H14C 109.5 . . ?
 H14A C14 H14B 109.5 . . ?
 H14A C14 H14C 109.5 . . ?
 H14B C14 H14C 109.5 . . ?
 C16 C15 C13 117.9(2) . . ?
 C20 C15 C13 124.0(3) . . ?
 C20 C15 C16 118.1(3) . . ?
 C15 C16 H16 119.0 . . ?
 C17 C16 C15 122.0(4) . . ?
 C17 C16 H16 119.0 . . ?
 C16 C17 H17 120.3 . . ?
 C18 C17 C16 119.4(5) . . ?
 C18 C17 H17 120.3 . . ?
 C17 C18 H18 119.8 . . ?
 C17 C18 C19 120.5(4) . . ?
 C19 C18 H18 119.8 . . ?
 C18 C19 H19 120.4 . . ?
 C18 C19 C20 119.2(4) . . ?
 C20 C19 H19 120.4 . . ?
 C15 C20 C19 120.7(4) . . ?
 C15 C20 H20 119.6 . . ?
 C19 C20 H20 119.6 . . ?
 H21A C21 H21B 107.6 . . ?
 C22 C21 H21A 108.6 . . ?
 C22 C21 H21B 108.6 . . ?
 N3 C21 H21A 108.6 . . ?
 N3 C21 H21B 108.6 . . ?
 N3 C21 C22 114.65(17) . . ?
 N4 C22 C21 115.65(17) . . ?
 O3 C22 C21 121.7(2) . . ?
 O3 C22 N4 122.7(2) . . ?
 C24 C23 H23 106.3 . . ?
 C25 C23 H23 106.3 . . ?
 C25 C23 C24 115.3(2) . . ?
 N3 C23 H23 106.3 . . ?
 N3 C23 C24 109.8(2) . . ?
 N3 C23 C25 112.1(2) . . ?
 C23 C24 H24A 109.5 . . ?
 C23 C24 H24B 109.5 . . ?
 C23 C24 H24C 109.5 . . ?
 H24A C24 H24B 109.5 . . ?
 H24A C24 H24C 109.5 . . ?
 H24B C24 H24C 109.5 . . ?
 C26 C25 C23 121.6(2) . . ?
 C26 C25 C30 117.1(3) . . ?
 C30 C25 C23 121.1(3) . . ?
 C25 C26 H26 119.2 . . ?
 C25 C26 C27 121.6(3) . . ?
 C27 C26 H26 119.2 . . ?
 C26 C27 H27 120.0 . . ?
 C28 C27 C26 119.9(4) . . ?
 C28 C27 H27 120.0 . . ?
 C27 C28 H28 120.2 . . ?
 C29 C28 C27 119.6(3) . . ?
 C29 C28 H28 120.2 . . ?
 C28 C29 H29 119.6 . . ?
 C28 C29 C30 120.7(3) . . ?
 C30 C29 H29 119.6 . . ?
 C25 C30 H30 119.5 . . ?
 C29 C30 C25 121.0(4) . . ?
 C29 C30 H30 119.5 . . ?
 H31A C31 H31B 107.9 . . ?
 C32 C31 H31A 109.2 . . ?
 C32 C31 H31B 109.2 . . ?
 N4 C31 H31A 109.2 . . ?
 N4 C31 H31B 109.2 . . ?
 N4 C31 C32 112.15(15) . . ?
 N5 C32 C31 117.79(16) . . ?
 O4 C32 C31 120.80(17) . . ?
 O4 C32 N5 121.28(18) . . ?
 C34 C33 H33 107.1 . . ?
 C35 C33 H33 107.1 . . ?
 C35 C33 C34 114.9(2) . . ?
 N4 C33 H33 107.1 . . ?
 N4 C33 C34 111.3(2) . . ?
 N4 C33 C35 109.05(18) . . ?
 C33 C34 H34A 109.5 . . ?
 C33 C34 H34B 109.5 . . ?
 C33 C34 H34C 109.5 . . ?
 H34A C34 H34B 109.5 . . ?
 H34A C34 H34C 109.5 . . ?
 H34B C34 H34C 109.5 . . ?
 C36 C35 C33 119.4(3) . . ?
 C36 C35 C40 117.6(3) . . ?
 C40 C35 C33 122.9(2) . . ?
 C35 C36 H36 120.0 . . ?
 C35 C36 C37 119.9(4) . . ?
 C37 C36 H36 120.0 . . ?
 C36 C37 H37 119.7 . . ?
 C38 C37 C36 120.5(4) . . ?
 C38 C37 H37 119.7 . . ?
 C37 C38 H38 120.0 . . ?
 C39 C38 C37 120.1(4) . . ?
 C39 C38 H38 120.0 . . ?
 C38 C39 H39 120.1 . . ?
 C38 C39 C40 119.8(4) . . ?
 C40 C39 H39 120.1 . . ?
 C35 C40 H40 119.0 . . ?
 C39 C40 C35 122.0(4) . . ?
 C39 C40 H40 119.0 . . ?
 H41A C41 H41B 107.7 . . ?
 C42 C41 H41A 108.8 . . ?
 C42 C41 H41B 108.8 . . ?
 N5 C41 H41A 108.8 . . ?
 N5 C41 H41B 108.8 . . ?
 N5 C41 C42 113.62(18) . . ?
 N6 C42 C41 118.40(19) . . ?
 O5 C42 C41 119.4(2) . . ?
 O5 C42 N6 122.0(2) . . ?
 C44 C43 H43 106.6 . . ?
 C45 C43 H43 106.6 . . ?
 C45 C43 C44 114.8(2) . . ?
 N5 C43 H43 106.6 . . ?
 N5 C43 C44 111.2(2) . . ?
 N5 C43 C45 110.61(17) . . ?
 C43 C44 H44A 109.5 . . ?
 C43 C44 H44B 109.5 . . ?
 C43 C44 H44C 109.5 . . ?
 H44A C44 H44B 109.5 . . ?
 H44A C44 H44C 109.5 . . ?
 H44B C44 H44C 109.5 . . ?
 C46 C45 C43 122.9(2) . . ?
 C50 C45 C43 119.0(2) . . ?
 C50 C45 C46 118.1(2) . . ?
 C45 C46 H46 119.6 . . ?
 C47 C46 C45 120.9(3) . . ?
 C47 C46 H46 119.6 . . ?
 C46 C47 H47 119.7 . . ?
 C48 C47 C46 120.6(3) . . ?
 C48 C47 H47 119.7 . . ?
 C47 C48 H48 119.9 . . ?
 C47 C48 C49 120.2(3) . . ?
 C49 C48 H48 119.9 . . ?
 C48 C49 H49 120.0 . . ?
 C48 C49 C50 120.0(4) . . ?
 C50 C49 H49 120.0 . . ?
 C45 C50 C49 120.2(3) . . ?
 C45 C50 H50 119.9 . . ?
 C49 C50 H50 119.9 . . ?
 H51A C51 H51B 107.7 . . ?
 C52 C51 H51A 108.8 . . ?
 C52 C51 H51B 108.8 . . ?
 N6 C51 H51A 108.8 . . ?
 N6 C51 H51B 108.8 . . ?
 N6 C51 C52 113.92(17) . . ?
 N1 C52 C51 115.58(17) . . ?
 O6 C52 C51 120.89(19) . . ?
 O6 C52 N1 123.52(19) . . ?
 C54 C53 H53 107.1 . . ?
 C55 C53 H53 107.1 . . ?
 C55 C53 C54 115.3(2) . . ?
 N6 C53 H53 107.1 . . ?
 N6 C53 C54 110.5(2) . . ?
 N6 C53 C55 109.3(2) . . ?
 C53 C54 H54A 109.5 . . ?
 C53 C54 H54B 109.5 . . ?
 C53 C54 H54C 109.5 . . ?
 H54A C54 H54B 109.5 . . ?
 H54A C54 H54C 109.5 . . ?
 H54B C54 H54C 109.5 . . ?
 C56 C55 C53 119.5(3) . . ?
 C56 C55 C60 117.4(3) . . ?
 C60 C55 C53 123.0(3) . . ?
 C55 C56 H56 119.1 . . ?
 C55 C56 C57 121.9(3) . . ?
 C57 C56 H56 119.1 . . ?
 C56 C57 H57 120.2 . . ?
 C58 C57 C56 119.6(4) . . ?
 C58 C57 H57 120.2 . . ?
 C57 C58 H58 120.1 . . ?
 C57 C58 C59 119.9(4) . . ?
 C59 C58 H58 120.1 . . ?
 C58 C59 H59 119.5 . . ?
 C58 C59 C60 121.0(4) . . ?
 C60 C59 H59 119.5 . . ?
 C55 C60 C59 120.2(4) . . ?
 C55 C60 H60 119.9 . . ?
 C59 C60 H60 119.9 . . ?
 C1 N1 C3 115.77(17) . . ?
 C52 N1 C1 120.41(17) . . ?
 C52 N1 C3 122.65(17) . . ?
 C2 N2 C11 114.94(16) . . ?
 C2 N2 C13 126.37(17) . . ?
 C11 N2 C13 118.35(16) . . ?
 C12 N3 C21 122.11(17) . . ?
 C12 N3 C23 118.81(18) . . ?
 C21 N3 C23 118.18(17) . . ?
 C22 N4 C31 122.82(17) . . ?
 C22 N4 C33 120.70(17) . . ?
 C31 N4 C33 116.44(17) . . ?
 C32 N5 C41 115.09(16) . . ?
 C32 N5 C43 123.84(17) . . ?
 C41 N5 C43 121.07(16) . . ?
 C42 N6 C51 122.51(17) . . ?
 C42 N6 C53 118.68(19) . . ?
 C51 N6 C53 117.23(18) . . ?

_olex2_submission_special_instructions  'No special instructions were received'
#===END
 
data_fifi2
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
;
2(C80 H90 F6 N8 Na O9 P), 0.25(C2 H3 N), 0.25(C2 H3 N)
;
_chemical_formula_sum
 'C161 H181.5 F12 N16.50 Na2 O18 P2'
_chemical_formula_weight          2966.10

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'F'  'F'   0.0727   0.0534
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.1353   0.1239
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            75
_space_group_name_H-M_alt         'P 4'
_space_group_name_Hall            'P 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, z'
 '-y, x, z'
 'y, -x, z'
 
_cell_length_a                    20.141(3)
_cell_length_b                    20.141(3)
_cell_length_c                    10.316(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      4184.8(17)
_cell_formula_units_Z             1
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     9500
_cell_measurement_theta_min       4.91
_cell_measurement_theta_max       70.96
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.179          
_exptl_crystal_F_000              1564
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.550
_exptl_crystal_size_mid           0.310
_exptl_crystal_size_min           0.280
_exptl_absorpt_coefficient_mu     0.931
_shelx_estimated_absorpt_T_min    0.628
_shelx_estimated_absorpt_T_max    0.780
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.5872
_exptl_absorpt_correction_T_max   0.7535
_exptl_absorpt_process_details    
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1380 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7793.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             67493
_diffrn_reflns_av_unetI/netI      0.0228
_diffrn_reflns_av_R_equivalents   0.0361
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        24
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.194
_diffrn_reflns_theta_max          71.549
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.976
_diffrn_measured_fraction_theta_full  0.984
_diffrn_reflns_Laue_measured_fraction_max    0.976
_diffrn_reflns_Laue_measured_fraction_full   0.984
_diffrn_reflns_point_group_measured_fraction_max   0.967
_diffrn_reflns_point_group_measured_fraction_full  0.981
_reflns_number_total              7930
_reflns_number_gt                 7536
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.872
_reflns_Friedel_fraction_max      0.957
_reflns_Friedel_fraction_full     0.977
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1211P)²+0.5898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.015(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 3339 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.063(7)
_chemical_absolute_configuration  syn
_refine_ls_number_reflns          7930
_refine_ls_number_parameters      489
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0577
_refine_ls_R_factor_gt            0.0556
_refine_ls_wR_factor_ref          0.1707
_refine_ls_wR_factor_gt           0.1679
_refine_ls_goodness_of_fit_ref    1.052
_refine_ls_restrained_S_all       1.052
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.000000 1.000000 0.9608(2) 0.0669(5) Uiso 1 4 d GS U P . .
F1 F -0.0370(4) 0.9661(3) 0.8304(6) 0.145(7) Uiso 0.25 1 d G U P . .
F2 F 0.0317(4) 1.0319(3) 1.0900(6) 0.129(5) Uiso 0.25 1 d G U P . .
F3 F 0.0614(2) 1.0227(4) 0.8727(7) 0.102(4) Uiso 0.25 1 d G U P . .
F4 F 0.0346(2) 0.92801(12) 0.9911(7) 0.082(3) Uiso 0.25 1 d G U P . .
F5 F -0.0400(2) 1.06995(13) 0.9293(7) 0.065(2) Uiso 0.25 1 d G U P . .
F6 F -0.0667(2) 0.9753(4) 1.0478(8) 0.116(5) Uiso 0.25 1 d G U P . .
Na1 Na 0.000000 1.000000 0.5889(4) 0.0690(8) Uani 1 4 d S T P . .
O1 O 0.09114(12) 0.92985(11) 0.5945(3) 0.0551(6) Uani 1 1 d . . . . .
O2 O 0.22445(16) 0.97838(13) 0.4712(3) 0.0706(7) Uani 1 1 d . . . . .
O5 O 0.000000 1.000000 0.3526(12) 0.155(5) Uani 1 4 d S T P . .
N1 N 0.08390(13) 0.79705(13) 0.5339(3) 0.0498(6) Uani 1 1 d . . . . .
N2 N 0.18839(13) 0.92187(13) 0.7000(3) 0.0503(6) Uani 1 1 d . . . . .
C1 C 0.13537(15) 0.89530(15) 0.6402(3) 0.0460(6) Uani 1 1 d . . . . .
C2 C 0.13049(15) 0.81974(15) 0.6316(3) 0.0472(7) Uani 1 1 d . . . . .
H2A H 0.174071 0.801836 0.612082 0.057 Uiso 1 1 calc R U . . .
H2B H 0.116996 0.802449 0.715285 0.057 Uiso 1 1 calc R U . . .
C3 C 0.10775(19) 0.78910(19) 0.3977(4) 0.0591(8) Uani 1 1 d . . . . .
H3 H 0.077100 0.758002 0.355751 0.071 Uiso 1 1 calc R U . . .
C4 C 0.1019(3) 0.8540(3) 0.3241(5) 0.0873(14) Uani 1 1 d . . . . .
H4A H 0.056747 0.869283 0.327375 0.131 Uiso 1 1 calc R U . . .
H4B H 0.114696 0.847240 0.235502 0.131 Uiso 1 1 calc R U . . .
H4C H 0.130412 0.886561 0.363011 0.131 Uiso 1 1 calc R U . . .
C5 C 0.17496(19) 0.75582(19) 0.3977(4) 0.0604(8) Uani 1 1 d . . . . .
C6 C 0.2323(3) 0.7890(3) 0.3623(6) 0.0892(14) Uani 1 1 d . . . . .
H1AA H 0.230231 0.832305 0.331509 0.107 Uiso 1 1 calc R U . . .
C7 C 0.2941(3) 0.7562(5) 0.3734(8) 0.116(2) Uani 1 1 d . . . . .
H7 H 0.332831 0.778465 0.350646 0.139 Uiso 1 1 calc R U . . .
C8 C 0.2976(3) 0.6931(5) 0.4167(7) 0.113(2) Uani 1 1 d . . . . .
H8 H 0.338600 0.672312 0.425264 0.136 Uiso 1 1 calc R U . . .
C9 C 0.2412(4) 0.6601(3) 0.4475(6) 0.0992(18) Uani 1 1 d . . . . .
H9 H 0.243589 0.616139 0.474690 0.119 Uiso 1 1 calc R U . . .
C10 C 0.1801(2) 0.6910(2) 0.4391(5) 0.0750(11) Uani 1 1 d . . . . .
H10 H 0.141898 0.667708 0.461615 0.090 Uiso 1 1 calc R U . . .
C11 C 0.20785(16) 1.01755(16) 0.5556(4) 0.0528(7) Uani 1 1 d . . . . .
C12 C 0.19338(17) 0.99406(15) 0.6936(4) 0.0508(7) Uani 1 1 d . . . . .
H12A H 0.228559 1.008987 0.750782 0.061 Uiso 1 1 calc R U . . .
H12B H 0.152070 1.013622 0.723209 0.061 Uiso 1 1 calc R U . . .
C13 C 0.24180(17) 0.88342(18) 0.7638(4) 0.0554(8) Uani 1 1 d . . . . .
H13 H 0.226603 0.837283 0.769248 0.067 Uiso 1 1 calc R U . . .
C14 C 0.3046(2) 0.8838(3) 0.6791(5) 0.0919(16) Uani 1 1 d . . . . .
H14A H 0.323220 0.927702 0.677905 0.138 Uiso 1 1 calc R U . . .
H14B H 0.293365 0.870696 0.592418 0.138 Uiso 1 1 calc R U . . .
H14C H 0.336531 0.853305 0.714230 0.138 Uiso 1 1 calc R U . . .
C15 C 0.25285(18) 0.90735(16) 0.9009(4) 0.0558(8) Uani 1 1 d . . . . .
C16 C 0.2000(2) 0.9300(2) 0.9756(4) 0.0658(9) Uani 1 1 d . . . . .
H16 H 0.157858 0.931682 0.938992 0.079 Uiso 1 1 calc R U . . .
C17 C 0.2082(3) 0.9500(3) 1.1011(5) 0.0846(14) Uani 1 1 d . . . . .
H17 H 0.171832 0.965256 1.148004 0.102 Uiso 1 1 calc R U . . .
C18 C 0.2690(3) 0.9476(3) 1.1582(5) 0.0906(16) Uani 1 1 d . . . . .
H18 H 0.274474 0.961374 1.243573 0.109 Uiso 1 1 calc R U . . .
C19 C 0.3211(4) 0.9252(3) 1.0894(7) 0.106(2) Uani 1 1 d . . . . .
H19 H 0.362415 0.922384 1.129057 0.128 Uiso 1 1 calc R U . . .
C20 C 0.3146(2) 0.9060(3) 0.9593(5) 0.0822(13) Uani 1 1 d . . . . .
H20 H 0.351671 0.892473 0.912526 0.099 Uiso 1 1 calc R U . . .
P2 P 0.500000 0.500000 0.3950(2) 0.0706(5) Uiso 1 4 d GS U P . .
F7 F 0.5353(4) 0.4806(3) 0.2583(5) 0.128(6) Uiso 0.25 1 d G U P . .
F8 F 0.4611(4) 0.5169(4) 0.5336(5) 0.131(6) Uiso 0.25 1 d G U P . .
F9 F 0.4480(3) 0.5496(2) 0.3186(7) 0.093(3) Uiso 0.25 1 d G U P . .
F10 F 0.55090(18) 0.56001(15) 0.4193(9) 0.099(4) Uiso 0.25 1 d G U P . .
F11 F 0.5484(3) 0.4479(2) 0.4733(7) 0.121(5) Uiso 0.25 1 d G U P . .
F12 F 0.44548(19) 0.43738(16) 0.3727(10) 0.072(2) Uiso 0.25 1 d G U P . .
Na2 Na 0.500000 0.500000 0.0101(3) 0.0604(7) Uani 1 4 d S T P . .
O3 O 0.53343(12) 0.61242(11) 0.0298(3) 0.0570(6) Uani 1 1 d . . . . .
O4 O 0.43116(15) 0.71953(18) -0.0834(3) 0.0781(9) Uani 1 1 d . . . . .
O7 O 0.475(3) 0.494(7) -0.2084(13) 0.106(13) Uani 0.25 1 d . . P . .
N3 N 0.34161(14) 0.66183(14) -0.0146(3) 0.0524(6) Uani 1 1 d . . . . .
N4 N 0.50213(13) 0.70296(14) 0.1414(3) 0.0513(6) Uani 1 1 d . . . . .
C21 C 0.54808(15) 0.66490(15) 0.0805(3) 0.0467(7) Uani 1 1 d . . . . .
C22 C 0.62004(16) 0.68987(15) 0.0813(3) 0.0509(7) Uani 1 1 d . . . . .
H22A H 0.620023 0.737404 0.066104 0.061 Uiso 1 1 calc R U . . .
H22B H 0.638887 0.682198 0.166502 0.061 Uiso 1 1 calc R U . . .
C23 C 0.3099(2) 0.6680(2) -0.1439(4) 0.0660(9) Uani 1 1 d . . . . .
H23 H 0.328603 0.707593 -0.185229 0.079 Uiso 1 1 calc R U . . .
C24 C 0.3283(3) 0.6094(4) -0.2278(5) 0.1007(18) Uani 1 1 d . . . . .
H24A H 0.375703 0.605347 -0.231404 0.151 Uiso 1 1 calc R U . . .
H24B H 0.311135 0.616044 -0.313659 0.151 Uiso 1 1 calc R U . . .
H24C H 0.309586 0.569686 -0.191625 0.151 Uiso 1 1 calc R U . . .
C25 C 0.23585(19) 0.68045(19) -0.1262(4) 0.0618(9) Uani 1 1 d . . . . .
C26 C 0.1880(3) 0.6427(3) -0.1829(6) 0.0932(15) Uani 1 1 d . . . . .
H26 H 0.200312 0.608576 -0.238698 0.112 Uiso 1 1 calc R U . . .
C27 C 0.1209(3) 0.6541(5) -0.1589(9) 0.118(3) Uani 1 1 d . . . . .
H27 H 0.089061 0.627923 -0.199447 0.142 Uiso 1 1 calc R U . . .
C28 C 0.1018(3) 0.7025(5) -0.0779(8) 0.117(3) Uani 1 1 d . . . . .
H28 H 0.057064 0.708723 -0.059579 0.141 Uiso 1 1 calc R U . . .
C29 C 0.1487(4) 0.7429(4) -0.0222(7) 0.106(2) Uani 1 1 d . . . . .
H29 H 0.135542 0.777483 0.031827 0.127 Uiso 1 1 calc R U . . .
C30 C 0.2149(3) 0.7325(2) -0.0462(5) 0.0789(12) Uani 1 1 d . . . . .
H30 H 0.246314 0.760336 -0.008719 0.095 Uiso 1 1 calc R U . . .
C31 C 0.40326(17) 0.68800(18) 0.0014(4) 0.0549(8) Uani 1 1 d . . . . .
C32 C 0.43414(16) 0.67896(18) 0.1350(3) 0.0529(7) Uani 1 1 d . . . . .
H32A H 0.407554 0.702570 0.198413 0.063 Uiso 1 1 calc R U . . .
H32B H 0.433401 0.632208 0.157498 0.063 Uiso 1 1 calc R U . . .
C33 C 0.51543(18) 0.76729(17) 0.2030(4) 0.0579(8) Uani 1 1 d . . . . .
H33 H 0.563784 0.772639 0.203908 0.069 Uiso 1 1 calc R U . . .
C34 C 0.4881(4) 0.8240(2) 0.1217(6) 0.102(2) Uani 1 1 d . . . . .
H34A H 0.496156 0.815220 0.031633 0.153 Uiso 1 1 calc R U . . .
H34B H 0.509652 0.864673 0.145987 0.153 Uiso 1 1 calc R U . . .
H34C H 0.441171 0.828015 0.136249 0.153 Uiso 1 1 calc R U . . .
C35 C 0.49293(17) 0.76788(19) 0.3452(4) 0.0573(8) Uani 1 1 d . . . . .
C36 C 0.4798(3) 0.8272(3) 0.4071(5) 0.0860(14) Uani 1 1 d . . . . .
H36 H 0.481415 0.866821 0.360964 0.103 Uiso 1 1 calc R U . . .
C37 C 0.4641(4) 0.8278(4) 0.5378(7) 0.114(2) Uani 1 1 d . . . . .
H37 H 0.455237 0.867936 0.578785 0.137 Uiso 1 1 calc R U . . .
C38 C 0.4614(3) 0.7700(4) 0.6076(5) 0.1019(18) Uani 1 1 d . . . . .
H38 H 0.451568 0.770840 0.695632 0.122 Uiso 1 1 calc R U . . .
C39 C 0.4733(2) 0.7118(3) 0.5469(5) 0.0806(12) Uani 1 1 d . . . . .
H39 H 0.470511 0.672244 0.593014 0.097 Uiso 1 1 calc R U . . .
C40 C 0.4899(2) 0.7105(2) 0.4150(4) 0.0653(9) Uani 1 1 d . . . . .
H40 H 0.498965 0.670129 0.374841 0.078 Uiso 1 1 calc R U . . .
N5 N 0.500000 1.000000 -0.284(8) 0.107(8) Uiso 0.125 2 d S U P . .
C51 C 0.500000 1.000000 -0.184(9) 0.107(8) Uiso 0.125 2 d S U P . .
C52 C 0.500000 1.000000 -0.051(9) 0.107(8) Uiso 0.125 2 d S U P . .
N6 N 0.500000 1.000000 0.275(7) 0.107(8) Uiso 0.125 2 d S U P . .
C61 C 0.605(6) 1.000(6) 0.440(12) 0.107(8) Uiso 0.0625 1 d . U P . .
C62 C 0.549(6) 0.995(6) 0.352(12) 0.107(8) Uiso 0.0625 1 d . U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
P1 F3 1.6018 . ?
P1 F3 1.602(8) 2_575 ?
P1 F3 1.602(8) 4_465 ?
P1 F3 1.602(5) 3_665 ?
P1 F2 1.6111 . ?
P1 F2 1.611(5) 4_465 ?
P1 F2 1.611(6) 3_665 ?
P1 F2 1.611(9) 2_575 ?
P1 F4 1.6388 . ?
P1 F4 1.639(5) 3_665 ?
P1 F4 1.639(5) 4_465 ?
P1 F4 1.639(3) 2_575 ?
F1 F3 0.695(8) 2_575 ?
F1 F5 1.2228(19) 3_665 ?
F1 F3 1.395(5) 4_465 ?
F1 F1 1.430(11) 4_465 ?
F1 F1 1.431(14) 3_665 ?
F1 Na1 2.689(10) . ?
F2 F6 0.841(9) 2_575 ?
F2 F2 1.281(14) 3_665 ?
F2 F2 1.281(11) 4_465 ?
F2 F4 1.304(2) 3_665 ?
F2 F6 1.405(6) 4_465 ?
F3 F5 0.7015(13) 4_465 ?
F3 F4 1.2622(17) 3_665 ?
F4 F6 0.627(3) 3_665 ?
F4 F5 0.647(2) 2_575 ?
F5 F6 1.2621(13) 4_465 ?
Na1 O1 2.317(2) . ?
Na1 O1 2.317(2) 3_665 ?
Na1 O1 2.317(2) 4_465 ?
Na1 O1 2.317(2) 2_575 ?
Na1 O5 2.438(13) . ?
O1 C1 1.225(4) . ?
O2 C11 1.221(5) . ?
N1 C11 1.359(4) 4_465 ?
N1 C2 1.451(4) . ?
N1 C3 1.494(5) . ?
N2 C1 1.345(4) . ?
N2 C12 1.459(4) . ?
N2 C13 1.480(4) . ?
C1 C2 1.528(4) . ?
C3 C5 1.510(5) . ?
C3 C4 1.516(6) . ?
C5 C10 1.378(6) . ?
C5 C1AA 1.383(7) . ?
C1AA C7 1.413(9) . ?
C7 C8 1.349(12) . ?
C8 C9 1.354(12) . ?
C9 C10 1.382(7) . ?
C11 C12 1.528(5) . ?
C13 C15 1.511(5) . ?
C13 C14 1.537(6) . ?
C15 C20 1.382(6) . ?
C15 C16 1.391(6) . ?
C16 C17 1.365(7) . ?
C17 C18 1.359(9) . ?
C18 C19 1.344(10) . ?
C19 C20 1.403(8) . ?
P2 F10 1.6045 . ?
P2 F10 1.604(3) 2_665 ?
P2 F10 1.604(5) 4_565 ?
P2 F10 1.604(5) 3_655 ?
P2 F7 1.627(6) 4_565 ?
P2 F7 1.627(7) 2_665 ?
P2 F7 1.627(5) 3_655 ?
P2 F7 1.6275 . ?
P2 F11 1.6443 . ?
P2 F11 1.644(5) 3_655 ?
P2 F11 1.644(7) 4_565 ?
P2 F11 1.644(7) 2_665 ?
F7 F9 0.932(6) 2_665 ?
F7 F7 1.148(12) 3_655 ?
F7 F7 1.148(10) 4_565 ?
F7 F12 1.481(3) 3_655 ?
F7 F9 1.593(6) 4_565 ?
F7 F7 1.624(15) 2_665 ?
F7 Na2 2.686(7) . ?
F8 F11 0.962(7) 2_665 ?
F8 F8 1.208(11) 4_565 ?
F8 F8 1.208(12) 3_655 ?
F8 F10 1.4279(19) 3_655 ?
F8 F11 1.479(6) 4_565 ?
F8 F8 1.709(15) 2_665 ?
F9 F12 0.6053(14) 4_565 ?
F9 F10 1.0512(11) 3_655 ?
F9 F11 1.5980 2_665 ?
F10 F12 0.4894 2_665 ?
F10 F11 0.605(3) 3_655 ?
F11 F12 1.0781(19) 3_655 ?
Na2 O7 2.314(16) . ?
Na2 O7 2.314(16) 3_655 ?
Na2 O7 2.314(16) 4_565 ?
Na2 O7 2.314(16) 2_665 ?
Na2 O3 2.371(2) . ?
Na2 O3 2.371(2) 2_665 ?
Na2 O3 2.371(2) 4_565 ?
Na2 O3 2.371(2) 3_655 ?
O3 C21 1.215(4) . ?
O4 C31 1.218(4) . ?
O7 O7 0.74(4) 4_565 ?
O7 O7 0.74(4) 3_655 ?
O7 O7 1.05(5) 2_665 ?
N3 C31 1.359(5) . ?
N3 C22 1.446(4) 3_655 ?
N3 C23 1.484(5) . ?
N4 C21 1.356(4) . ?
N4 C32 1.454(4) . ?
N4 C33 1.468(5) . ?
C21 C22 1.534(4) . ?
C23 C24 1.508(7) . ?
C23 C25 1.524(6) . ?
C25 C26 1.360(7) . ?
C25 C30 1.398(7) . ?
C26 C27 1.393(10) . ?
C27 C28 1.340(13) . ?
C28 C29 1.372(12) . ?
C29 C30 1.373(8) . ?
C31 C32 1.523(5) . ?
C33 C34 1.520(7) . ?
C33 C35 1.536(5) . ?
C35 C40 1.364(6) . ?
C35 C36 1.380(6) . ?
C36 C37 1.385(8) . ?
C37 C38 1.369(11) . ?
C38 C39 1.351(9) . ?
C39 C40 1.401(7) . ?
N5 C51 1.03(10) . ?
C51 C52 1.38(12) . ?
N6 C62 1.26(12) . ?
N6 C62 1.26(12) 2_675 ?
C61 C62 1.45(17) . ?
C62 C62 2.0(2) 2_675 ?
 
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
F3 P1 F3 110.9(2) . 2_575 ?
F3 P1 F3 71.2(3) . 4_465 ?
F3 P1 F3 71.22(18) 2_575 4_465 ?
F3 P1 F3 71.2(3) . 3_665 ?
F3 P1 F3 71.22(18) 2_575 3_665 ?
F3 P1 F3 110.9(2) 4_465 3_665 ?
F3 P1 F2 92.8 . . ?
F3 P1 F2 152.8(3) 2_575 . ?
F3 P1 F2 131.58(14) 4_465 . ?
F3 P1 F2 105.95(15) 3_665 . ?
F3 P1 F2 106.0(2) . 4_465 ?
F3 P1 F2 131.6(3) 2_575 4_465 ?
F3 P1 F2 92.8(2) 4_465 4_465 ?
F3 P1 F2 152.8(3) 3_665 4_465 ?
F2 P1 F2 46.9(3) . 4_465 ?
F3 P1 F2 131.6(4) . 3_665 ?
F3 P1 F2 106.0(4) 2_575 3_665 ?
F3 P1 F2 152.8(3) 4_465 3_665 ?
F3 P1 F2 92.8(2) 3_665 3_665 ?
F2 P1 F2 46.9(5) . 3_665 ?
F2 P1 F2 68.4(5) 4_465 3_665 ?
F3 P1 F2 152.8(4) . 2_575 ?
F3 P1 F2 92.8(2) 2_575 2_575 ?
F3 P1 F2 106.0(4) 4_465 2_575 ?
F3 P1 F2 131.6(4) 3_665 2_575 ?
F2 P1 F2 68.4(5) . 2_575 ?
F2 P1 F2 46.9(2) 4_465 2_575 ?
F2 P1 F2 46.9(3) 3_665 2_575 ?
F3 P1 F4 91.8 . . ?
F3 P1 F4 100.6(4) 2_575 . ?
F3 P1 F4 45.82(19) 4_465 . ?
F3 P1 F4 155.89(14) 3_665 . ?
F2 P1 F4 91.5 . . ?
F2 P1 F4 47.3(3) 4_465 . ?
F2 P1 F4 111.3(2) 3_665 . ?
F2 P1 F4 70.1(4) 2_575 . ?
F3 P1 F4 45.8 . 3_665 ?
F3 P1 F4 155.9(2) 2_575 3_665 ?
F3 P1 F4 100.62(12) 4_465 3_665 ?
F3 P1 F4 91.8(3) 3_665 3_665 ?
F2 P1 F4 47.3 . 3_665 ?
F2 P1 F4 70.1(3) 4_465 3_665 ?
F2 P1 F4 91.5(4) 3_665 3_665 ?
F2 P1 F4 111.3(4) 2_575 3_665 ?
F4 P1 F4 87.9(2) . 3_665 ?
F3 P1 F4 155.9 . 4_465 ?
F3 P1 F4 45.8(2) 2_575 4_465 ?
F3 P1 F4 91.81(18) 4_465 4_465 ?
F3 P1 F4 100.6(4) 3_665 4_465 ?
F2 P1 F4 111.3 . 4_465 ?
F2 P1 F4 91.5(3) 4_465 4_465 ?
F2 P1 F4 70.1(3) 3_665 4_465 ?
F2 P1 F4 47.3(4) 2_575 4_465 ?
F4 P1 F4 87.9(2) . 4_465 ?
F4 P1 F4 158.1 3_665 4_465 ?
F3 P1 F4 100.6(4) . 2_575 ?
F3 P1 F4 91.8(3) 2_575 2_575 ?
F3 P1 F4 155.9(2) 4_465 2_575 ?
F3 P1 F4 45.82(12) 3_665 2_575 ?
F2 P1 F4 70.1(2) . 2_575 ?
F2 P1 F4 111.3(3) 4_465 2_575 ?
F2 P1 F4 47.3(3) 3_665 2_575 ?
F2 P1 F4 91.5(4) 2_575 2_575 ?
F4 P1 F4 158.1 . 2_575 ?
F4 P1 F4 87.9(2) 3_665 2_575 ?
F4 P1 F4 87.9(2) 4_465 2_575 ?
F3 F1 F5 29.0(6) 2_575 3_665 ?
F3 F1 F3 122.9(5) 2_575 4_465 ?
F5 F1 F3 99.59(7) 3_665 4_465 ?
F3 F1 F1 72.9(10) 2_575 4_465 ?
F5 F1 F1 97.1(4) 3_665 4_465 ?
F3 F1 F1 111.0(5) 4_465 4_465 ?
F3 F1 F1 136.1(6) 2_575 3_665 ?
F5 F1 F1 122.48(11) 3_665 3_665 ?
F3 F1 F1 28.4(4) 4_465 3_665 ?
F1 F1 F1 90.0 4_465 3_665 ?
F3 F1 P1 71.3(7) 2_575 . ?
F5 F1 P1 67.3(2) 3_665 . ?
F3 F1 P1 61.9(3) 4_465 . ?
F1 F1 P1 64.85(13) 4_465 . ?
F1 F1 P1 64.85(13) 3_665 . ?
F3 F1 Na1 134.0(9) 2_575 . ?
F5 F1 Na1 161.6(4) 3_665 . ?
F3 F1 Na1 98.7(4) 4_465 . ?
F1 F1 Na1 74.6(4) 4_465 . ?
F1 F1 Na1 74.6(3) 3_665 . ?
P1 F1 Na1 121.0(5) . . ?
F6 F2 F2 146.9(4) 2_575 3_665 ?
F6 F2 F2 80.0(9) 2_575 4_465 ?
F2 F2 F2 90.0 3_665 4_465 ?
F6 F2 F4 23.3(4) 2_575 3_665 ?
F2 F2 F4 128.42(10) 3_665 3_665 ?
F2 F2 F4 92.4(4) 4_465 3_665 ?
F6 F2 F6 127.1(3) 2_575 4_465 ?
F2 F2 F6 36.1(5) 3_665 4_465 ?
F2 F2 F6 120.1(6) 4_465 4_465 ?
F4 F2 F6 103.82(6) 3_665 4_465 ?
F6 F2 P1 80.6(5) 2_575 . ?
F2 F2 P1 66.57(13) 3_665 . ?
F2 F2 P1 66.57(13) 4_465 . ?
F4 F2 P1 67.5(2) 3_665 . ?
F6 F2 P1 67.8(3) 4_465 . ?
F1 F3 F5 122.2(16) 2_575 4_465 ?
F1 F3 F4 131.6(8) 2_575 3_665 ?
F5 F3 F4 19.8(3) 4_465 3_665 ?
F1 F3 F1 78.7(17) 2_575 3_665 ?
F5 F3 F1 141.9(2) 4_465 3_665 ?
F4 F3 F1 122.3(3) 3_665 3_665 ?
F1 F3 P1 84.4(9) 2_575 . ?
F5 F3 P1 81.9(4) 4_465 . ?
F4 F3 P1 68.6(2) 3_665 . ?
F1 F3 P1 67.9(4) 3_665 . ?
F6 F4 F5 163.8(6) 3_665 2_575 ?
F6 F4 F3 144.4(7) 3_665 4_465 ?
F5 F4 F3 21.5(7) 2_575 4_465 ?
F6 F4 F2 32.0(5) 3_665 4_465 ?
F5 F4 F2 137.5(7) 2_575 4_465 ?
F3 F4 F2 130.1(3) 4_465 4_465 ?
F6 F4 P1 83.8(5) 3_665 . ?
F5 F4 P1 80.1(2) 2_575 . ?
F3 F4 P1 65.5(4) 4_465 . ?
F2 F4 P1 65.2(4) 4_465 . ?
F4 F5 F3 138.7(10) 2_575 3_665 ?
F4 F5 F1 147.0(3) 2_575 4_465 ?
F3 F5 F1 28.7(6) 3_665 4_465 ?
F4 F5 F6 8.0(5) 2_575 4_465 ?
F3 F5 F6 132.2(6) 3_665 4_465 ?
F1 F5 F6 139.1(3) 4_465 4_465 ?
F4 F5 P1 77.2(2) 2_575 . ?
F3 F5 P1 73.3(4) 3_665 . ?
F1 F5 P1 69.7(4) 4_465 . ?
F6 F5 P1 69.3(4) 4_465 . ?
F4 F6 F2 124.7(12) 4_465 2_575 ?
F4 F6 F5 8.2(6) 4_465 3_665 ?
F2 F6 F5 120.1(5) 2_575 3_665 ?
F4 F6 F2 129.1(3) 4_465 3_665 ?
F2 F6 F2 63.9(14) 2_575 3_665 ?
F5 F6 F2 121.6(4) 3_665 3_665 ?
F4 F6 P1 74.5(5) 4_465 . ?
F2 F6 P1 70.1(7) 2_575 . ?
F5 F6 P1 66.4(2) 3_665 . ?
F2 F6 P1 61.9(4) 3_665 . ?
O1 Na1 O1 89.966(7) . 3_665 ?
O1 Na1 O1 89.964(7) . 4_465 ?
O1 Na1 O1 177.2(2) 3_665 4_465 ?
O1 Na1 O1 177.2(2) . 2_575 ?
O1 Na1 O1 89.965(7) 3_665 2_575 ?
O1 Na1 O1 89.965(7) 4_465 2_575 ?
O1 Na1 O5 91.42(12) . . ?
O1 Na1 O5 91.42(13) 3_665 . ?
O1 Na1 O5 91.42(12) 4_465 . ?
O1 Na1 O5 91.42(12) 2_575 . ?
O1 Na1 F1 92.40(18) . . ?
O1 Na1 F1 110.33(19) 3_665 . ?
O1 Na1 F1 66.84(15) 4_465 . ?
O1 Na1 F1 84.96(17) 2_575 . ?
O5 Na1 F1 157.90(12) . . ?
O1 Na1 F1 84.97(16) . 2_575 ?
O1 Na1 F1 66.8(2) 3_665 2_575 ?
O1 Na1 F1 110.3(3) 4_465 2_575 ?
O1 Na1 F1 92.40(17) 2_575 2_575 ?
O5 Na1 F1 157.9(2) . 2_575 ?
F1 Na1 F1 44.2(3) . 2_575 ?
O1 Na1 F1 66.8(2) . 3_665 ?
O1 Na1 F1 92.40(17) 3_665 3_665 ?
O1 Na1 F1 84.97(16) 4_465 3_665 ?
O1 Na1 F1 110.3(2) 2_575 3_665 ?
O5 Na1 F1 157.9(2) . 3_665 ?
F1 Na1 F1 30.9(2) . 3_665 ?
F1 Na1 F1 30.9(3) 2_575 3_665 ?
O1 Na1 F1 110.3(2) . 4_465 ?
O1 Na1 F1 84.97(15) 3_665 4_465 ?
O1 Na1 F1 92.40(16) 4_465 4_465 ?
O1 Na1 F1 66.84(19) 2_575 4_465 ?
O5 Na1 F1 157.90(16) . 4_465 ?
F1 Na1 F1 30.85(19) . 4_465 ?
F1 Na1 F1 30.9(2) 2_575 4_465 ?
F1 Na1 F1 44.2(3) 3_665 4_465 ?
C1 O1 Na1 158.8(3) . . ?
C11 N1 C2 123.0(3) 4_465 . ?
C11 N1 C3 117.6(3) 4_465 . ?
C2 N1 C3 118.6(3) . . ?
C1 N2 C12 115.5(3) . . ?
C1 N2 C13 125.0(3) . . ?
C12 N2 C13 119.5(3) . . ?
O1 C1 N2 121.9(3) . . ?
O1 C1 C2 119.8(3) . . ?
N2 C1 C2 118.3(3) . . ?
N1 C2 C1 113.3(3) . . ?
N1 C3 C5 109.6(3) . . ?
N1 C3 C4 110.7(3) . . ?
C5 C3 C4 116.9(4) . . ?
C10 C5 C1AA 118.5(4) . . ?
C10 C5 C3 119.2(4) . . ?
C1AA C5 C3 122.3(4) . . ?
C5 C1AA C7 119.3(6) . . ?
C8 C7 C1AA 120.8(6) . . ?
C7 C8 C9 119.7(6) . . ?
C8 C9 C10 120.8(6) . . ?
C5 C10 C9 120.8(5) . . ?
O2 C11 N1 122.5(3) . 3_665 ?
O2 C11 C12 121.1(3) . . ?
N1 C11 C12 116.4(3) 3_665 . ?
N2 C12 C11 111.3(3) . . ?
N2 C13 C15 110.9(3) . . ?
N2 C13 C14 110.1(3) . . ?
C15 C13 C14 114.1(3) . . ?
C20 C15 C16 116.9(4) . . ?
C20 C15 C13 122.3(4) . . ?
C16 C15 C13 120.7(3) . . ?
C17 C16 C15 122.0(4) . . ?
C18 C17 C16 120.6(5) . . ?
C19 C18 C17 119.1(5) . . ?
C18 C19 C20 121.7(5) . . ?
C15 C20 C19 119.7(5) . . ?
F10 P2 F10 162.1 . 2_665 ?
F10 P2 F10 88.6(2) . 4_565 ?
F10 P2 F10 88.61(19) 2_665 4_565 ?
F10 P2 F10 88.61(19) . 3_655 ?
F10 P2 F10 88.61(19) 2_665 3_655 ?
F10 P2 F10 162.1 4_565 3_655 ?
F10 P2 F7 128.2(4) . 4_565 ?
F10 P2 F7 69.6(4) 2_665 4_565 ?
F10 P2 F7 92.1(3) 4_565 4_565 ?
F10 P2 F7 103.5(3) 3_655 4_565 ?
F10 P2 F7 103.5(6) . 2_665 ?
F10 P2 F7 92.1(5) 2_665 2_665 ?
F10 P2 F7 128.2(4) 4_565 2_665 ?
F10 P2 F7 69.6(4) 3_655 2_665 ?
F7 P2 F7 41.3(2) 4_565 2_665 ?
F10 P2 F7 69.6(3) . 3_655 ?
F10 P2 F7 128.2(3) 2_665 3_655 ?
F10 P2 F7 103.5(4) 4_565 3_655 ?
F10 P2 F7 92.1(4) 3_655 3_655 ?
F7 P2 F7 59.9(4) 4_565 3_655 ?
F7 P2 F7 41.3(3) 2_665 3_655 ?
F10 P2 F7 92.1 . . ?
F10 P2 F7 103.50(18) 2_665 . ?
F10 P2 F7 69.6 4_565 . ?
F10 P2 F7 128.2 3_655 . ?
F7 P2 F7 41.3(3) 4_565 . ?
F7 P2 F7 59.9(4) 2_665 . ?
F7 P2 F7 41.3(4) 3_655 . ?
F10 P2 F11 91.5 . . ?
F10 P2 F11 79.7(3) 2_665 . ?
F10 P2 F11 21.4 4_565 . ?
F10 P2 F11 141.1 3_655 . ?
F7 P2 F11 106.8(3) 4_565 . ?
F7 P2 F11 146.9(4) 2_665 . ?
F7 P2 F11 124.2(4) 3_655 . ?
F7 P2 F11 90.7 . . ?
F10 P2 F11 21.41(14) . 3_655 ?
F10 P2 F11 141.07(10) 2_665 3_655 ?
F10 P2 F11 79.7(3) 4_565 3_655 ?
F10 P2 F11 91.5(2) 3_655 3_655 ?
F7 P2 F11 146.9(3) 4_565 3_655 ?
F7 P2 F11 124.2(6) 2_665 3_655 ?
F7 P2 F11 90.7(3) 3_655 3_655 ?
F7 P2 F11 106.79(15) . 3_655 ?
F11 P2 F11 76.1(2) . 3_655 ?
F10 P2 F11 141.07(14) . 4_565 ?
F10 P2 F11 21.41(19) 2_665 4_565 ?
F10 P2 F11 91.5(2) 4_565 4_565 ?
F10 P2 F11 79.71(14) 3_655 4_565 ?
F7 P2 F11 90.7(3) 4_565 4_565 ?
F7 P2 F11 106.8(6) 2_665 4_565 ?
F7 P2 F11 146.9(4) 3_655 4_565 ?
F7 P2 F11 124.20(16) . 4_565 ?
F11 P2 F11 76.1(3) . 4_565 ?
F11 P2 F11 121.19(13) 3_655 4_565 ?
F10 P2 F11 79.7(4) . 2_665 ?
F10 P2 F11 91.5(3) 2_665 2_665 ?
F10 P2 F11 141.07(16) 4_565 2_665 ?
F10 P2 F11 21.41(17) 3_655 2_665 ?
F7 P2 F11 124.2(4) 4_565 2_665 ?
F7 P2 F11 90.7(3) 2_665 2_665 ?
F7 P2 F11 106.8(5) 3_655 2_665 ?
F7 P2 F11 146.94(17) . 2_665 ?
F11 P2 F11 121.19(13) . 2_665 ?
F11 P2 F11 76.1(2) 3_655 2_665 ?
F11 P2 F11 76.1(2) 4_565 2_665 ?
F9 F7 F7 136.6(5) 2_665 3_655 ?
F9 F7 F7 99.4(11) 2_665 4_565 ?
F7 F7 F7 90.0 3_655 4_565 ?
F9 F7 F12 12.4(5) 2_665 3_655 ?
F7 F7 F12 124.19(15) 3_655 3_655 ?
F7 F7 F12 102.9(5) 4_565 3_655 ?
F9 F7 F9 105.2(4) 2_665 4_565 ?
F7 F7 F9 35.2(5) 3_655 4_565 ?
F7 F7 F9 115.1(6) 4_565 4_565 ?
F12 F7 F9 93.05(8) 3_655 4_565 ?
F9 F7 F7 129.0(7) 2_665 2_665 ?
F7 F7 F7 45.00(17) 3_655 2_665 ?
F7 F7 F7 45.00(17) 4_565 2_665 ?
F12 F7 F7 123.7(3) 3_655 2_665 ?
F9 F7 F7 73.9(6) 4_565 2_665 ?
F9 F7 P2 74.7(3) 2_665 . ?
F7 F7 P2 69.3(2) 3_655 . ?
F7 F7 P2 69.3(2) 4_565 . ?
F12 F7 P2 65.59(17) 3_655 . ?
F9 F7 P2 61.5(2) 4_565 . ?
F7 F7 P2 60.1 2_665 . ?
F9 F7 Na2 145.8(7) 2_665 . ?
F7 F7 Na2 77.7(3) 3_655 . ?
F7 F7 Na2 77.7(4) 4_565 . ?
F12 F7 Na2 158.0(4) 3_655 . ?
F9 F7 Na2 106.8(5) 4_565 . ?
F7 F7 Na2 72.4(4) 2_665 . ?
P2 F7 Na2 132.5(4) . . ?
F11 F8 F8 85.1(10) 2_665 4_565 ?
F11 F8 F8 139.3(3) 2_665 3_655 ?
F8 F8 F8 90.0 4_565 3_655 ?
F11 F8 F10 18.9(5) 2_665 3_655 ?
F8 F8 F10 95.8(4) 4_565 3_655 ?
F8 F8 F10 123.71(8) 3_655 3_655 ?
F11 F8 F11 110.4(4) 2_665 4_565 ?
F8 F8 F11 119.6(6) 4_565 4_565 ?
F8 F8 F11 40.4(6) 3_655 4_565 ?
F10 F8 F11 91.47(10) 3_655 4_565 ?
F11 F8 P2 71.9(3) 2_665 . ?
F8 F8 P2 68.72(19) 4_565 . ?
F8 F8 P2 68.72(19) 3_655 . ?
F10 F8 P2 61.94(18) 3_655 . ?
F11 F8 P2 62.7(2) 4_565 . ?
F11 F8 F8 118.4(8) 2_665 2_665 ?
F8 F8 F8 45.00(17) 4_565 2_665 ?
F8 F8 F8 45.00(17) 3_655 2_665 ?
F10 F8 F8 117.7(3) 3_655 2_665 ?
F11 F8 F8 79.1(6) 4_565 2_665 ?
P2 F8 F8 59.1 . 2_665 ?
F12 F9 F7 148.2(11) 4_565 2_665 ?
F12 F9 F10 14.5(7) 4_565 3_655 ?
F7 F9 F10 137.0(5) 2_665 3_655 ?
F12 F9 F7 135.1(2) 4_565 3_655 ?
F7 F9 F7 45.3(11) 2_665 3_655 ?
F10 F9 F7 121.9(4) 3_655 3_655 ?
F12 F9 F11 24.7(5) 4_565 2_665 ?
F7 F9 F11 132.2(3) 2_665 2_665 ?
F10 F9 F11 11.4(3) 3_655 2_665 ?
F7 F9 F11 110.8(3) 3_655 2_665 ?
F12 F9 P2 83.3(4) 4_565 . ?
F7 F9 P2 72.3(6) 2_665 . ?
F10 F9 P2 68.9(3) 3_655 . ?
F7 F9 P2 60.3(3) 3_655 . ?
F11 F9 P2 60.9(3) 2_665 . ?
F12 F10 F11 160.3(16) 2_665 3_655 ?
F12 F10 F9 18.1(4) 2_665 4_565 ?
F11 F10 F9 148.4(8) 3_655 4_565 ?
F12 F10 F8 156.2(5) 2_665 4_565 ?
F11 F10 F8 31.1(7) 3_655 4_565 ?
F9 F10 F8 139.3(4) 4_565 4_565 ?
F12 F10 P2 91.3(3) 2_665 . ?
F11 F10 P2 83.0(6) 3_655 . ?
F9 F10 P2 73.4(4) 4_565 . ?
F8 F10 P2 66.3(4) 4_565 . ?
F10 F11 F8 130.0(12) 4_565 2_665 ?
F10 F11 F12 8.8(2) 4_565 3_655 ?
F8 F11 F12 135.1(6) 2_665 3_655 ?
F10 F11 F8 136.4(3) 4_565 3_655 ?
F8 F11 F8 54.5(12) 2_665 3_655 ?
F12 F11 F8 130.5(4) 3_655 3_655 ?
F10 F11 F9 20.2(5) 4_565 2_665 ?
F8 F11 F9 129.1(4) 2_665 2_665 ?
F12 F11 F9 13.6(3) 3_655 2_665 ?
F8 F11 F9 117.0(2) 3_655 2_665 ?
F10 F11 P2 75.6(4) 4_565 . ?
F8 F11 P2 74.3(6) 2_665 . ?
F12 F11 P2 73.4(3) 3_655 . ?
F8 F11 P2 64.2(3) 3_655 . ?
F9 F11 P2 61.1(3) 2_665 . ?
F10 F12 F9 147.4(6) 2_665 3_655 ?
F10 F12 F11 10.9(9) 2_665 4_565 ?
F9 F12 F11 141.8(6) 3_655 4_565 ?
F10 F12 F7 132.2(3) 2_665 4_565 ?
F9 F12 F7 19.4(6) 3_655 4_565 ?
F11 F12 F7 130.3(3) 4_565 4_565 ?
F10 F12 P2 71.8(3) 2_665 . ?
F9 F12 P2 75.8(5) 3_655 . ?
F11 F12 P2 68.9(4) 4_565 . ?
F7 F12 P2 61.4(4) 4_565 . ?
O7 Na2 O7 18.4(9) . 3_655 ?
O7 Na2 O7 18.4(9) . 4_565 ?
O7 Na2 O7 26.1(13) 3_655 4_565 ?
O7 Na2 O7 26.1(13) . 2_665 ?
O7 Na2 O7 18.4(9) 3_655 2_665 ?
O7 Na2 O7 18.4(9) 4_565 2_665 ?
O7 Na2 O3 101(3) . . ?
O7 Na2 O3 106(2) 3_655 . ?
O7 Na2 O3 84(2) 4_565 . ?
O7 Na2 O3 88(3) 2_665 . ?
O7 Na2 O3 88(3) . 2_665 ?
O7 Na2 O3 84(2) 3_655 2_665 ?
O7 Na2 O3 106(2) 4_565 2_665 ?
O7 Na2 O3 101(3) 2_665 2_665 ?
O3 Na2 O3 170.2(2) . 2_665 ?
O7 Na2 O3 106(2) . 4_565 ?
O7 Na2 O3 88(3) 3_655 4_565 ?
O7 Na2 O3 101(3) 4_565 4_565 ?
O7 Na2 O3 84(2) 2_665 4_565 ?
O3 Na2 O3 89.578(18) . 4_565 ?
O3 Na2 O3 89.580(18) 2_665 4_565 ?
O7 Na2 O3 84(2) . 3_655 ?
O7 Na2 O3 101(3) 3_655 3_655 ?
O7 Na2 O3 88(3) 4_565 3_655 ?
O7 Na2 O3 106(2) 2_665 3_655 ?
O3 Na2 O3 89.581(18) . 3_655 ?
O3 Na2 O3 89.580(18) 2_665 3_655 ?
O3 Na2 O3 170.2(2) 4_565 3_655 ?
O7 Na2 F7 168(4) . . ?
O7 Na2 F7 151.9(14) 3_655 . ?
O7 Na2 F7 167(4) 4_565 . ?
O7 Na2 F7 151(2) 2_665 . ?
O3 Na2 F7 88.98(19) . . ?
O3 Na2 F7 81.64(19) 2_665 . ?
O3 Na2 F7 67.92(16) 4_565 . ?
O3 Na2 F7 102.28(18) 3_655 . ?
O7 Na2 F7 167(4) . 3_655 ?
O7 Na2 F7 168(4) 3_655 3_655 ?
O7 Na2 F7 151(2) 4_565 3_655 ?
O7 Na2 F7 151.9(14) 2_665 3_655 ?
O3 Na2 F7 67.92(19) . 3_655 ?
O3 Na2 F7 102.3(2) 2_665 3_655 ?
O3 Na2 F7 81.64(18) 4_565 3_655 ?
O3 Na2 F7 88.98(19) 3_655 3_655 ?
F7 Na2 F7 24.7(2) . 3_655 ?
O7 Na2 F7 151(2) . 2_665 ?
O7 Na2 F7 167(4) 3_655 2_665 ?
O7 Na2 F7 151.9(14) 4_565 2_665 ?
O7 Na2 F7 168(4) 2_665 2_665 ?
O3 Na2 F7 81.64(18) . 2_665 ?
O3 Na2 F7 88.98(19) 2_665 2_665 ?
O3 Na2 F7 102.3(2) 4_565 2_665 ?
O3 Na2 F7 67.9(2) 3_655 2_665 ?
F7 Na2 F7 35.2(3) . 2_665 ?
F7 Na2 F7 24.7(2) 3_655 2_665 ?
O7 Na2 F7 151.9(14) . 4_565 ?
O7 Na2 F7 151(2) 3_655 4_565 ?
O7 Na2 F7 168(4) 4_565 4_565 ?
O7 Na2 F7 167(4) 2_665 4_565 ?
O3 Na2 F7 102.3(2) . 4_565 ?
O3 Na2 F7 67.9(2) 2_665 4_565 ?
O3 Na2 F7 88.98(18) 4_565 4_565 ?
O3 Na2 F7 81.64(17) 3_655 4_565 ?
F7 Na2 F7 24.7(2) . 4_565 ?
F7 Na2 F7 35.2(3) 3_655 4_565 ?
F7 Na2 F7 24.7(2) 2_665 4_565 ?
C21 O3 Na2 159.4(3) . . ?
O7 O7 O7 90.00(8) 4_565 3_655 ?
O7 O7 O7 45.00(3) 4_565 2_665 ?
O7 O7 O7 45.00(5) 3_655 2_665 ?
O7 O7 Na2 80.8(5) 4_565 . ?
O7 O7 Na2 80.8(5) 3_655 . ?
O7 O7 Na2 76.9(7) 2_665 . ?
C31 N3 C22 122.9(3) . 3_655 ?
C31 N3 C23 118.0(3) . . ?
C22 N3 C23 118.4(3) 3_655 . ?
C21 N4 C32 115.7(3) . . ?
C21 N4 C33 125.1(3) . . ?
C32 N4 C33 119.0(3) . . ?
O3 C21 N4 121.7(3) . . ?
O3 C21 C22 121.1(3) . . ?
N4 C21 C22 117.2(3) . . ?
N3 C22 C21 113.7(3) 4_565 . ?
N3 C23 C24 110.2(4) . . ?
N3 C23 C25 109.1(3) . . ?
C24 C23 C25 116.0(4) . . ?
C26 C25 C30 117.3(5) . . ?
C26 C25 C23 123.3(5) . . ?
C30 C25 C23 119.3(4) . . ?
C25 C26 C27 121.2(7) . . ?
C28 C27 C26 120.6(7) . . ?
C27 C28 C29 119.7(6) . . ?
C30 C29 C28 120.1(7) . . ?
C29 C30 C25 121.0(6) . . ?
O4 C31 N3 122.4(3) . . ?
O4 C31 C32 121.6(3) . . ?
N3 C31 C32 115.9(3) . . ?
N4 C32 C31 112.7(3) . . ?
N4 C33 C34 111.0(4) . . ?
N4 C33 C35 111.5(3) . . ?
C34 C33 C35 114.5(3) . . ?
C40 C35 C36 118.7(4) . . ?
C40 C35 C33 120.7(3) . . ?
C36 C35 C33 120.4(4) . . ?
C35 C36 C37 120.1(5) . . ?
C38 C37 C36 120.9(6) . . ?
C39 C38 C37 119.1(5) . . ?
C38 C39 C40 120.6(5) . . ?
C35 C40 C39 120.5(4) . . ?
N5 C51 C52 180.00(6) . . ?
C62 N6 C62 102(10) . 2_675 ?
N6 C62 C61 172(10) . . ?
N6 C62 C62 39(6) . 2_675 ?
C61 C62 C62 140(7) . 2_675 ?
 
_refine_diff_density_max    0.528
_refine_diff_density_min   -0.516
_refine_diff_density_rms    0.045



#===END
