# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ce10_merge_a
_database_code_depnum_ccdc_archive 'CCDC 1881082'
_audit_update_record             
;
2018-11-25 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(H2 O4 P), C140 H127 N11 O2, 2(C16 H36 N)'
_chemical_formula_sum            'C172 H203 N13 O10 P2'
_chemical_formula_weight         2674.40
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.469(4)
_cell_length_b                   29.096(6)
_cell_length_c                   28.543(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.17(3)
_cell_angle_gamma                90
_cell_volume                     17757(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    394308
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5744
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.1684
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            45276
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         1.317
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   'PLSII 2D bending magnet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8173
_reflns_number_total             22866
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         22866
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.0712
_refine_ls_restrained_S_all      0.842
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0792P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1857
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C62-C65 \\sim C62-C164
 with sigma of 0.02
 C62-C64 \\sim C62-C163
 with sigma of 0.02
 C62-C63 \\sim C62-C165
 with sigma of 0.02
 C66-C69 \\sim C66-C169
 with sigma of 0.02
 C66-C67 \\sim C66-C167
 with sigma of 0.02
 C66-C68 \\sim C66-C168
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C164) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C163) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.01
4. Others
 Sof(C163)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C164)=Sof(H16G)=Sof(H16H)=
 Sof(H16I)=Sof(C165)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C63)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C64)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=
 Sof(C65)=Sof(H02U)=Sof(H02S)=Sof(H02T)=FVAR(1)
 Sof(C167)=Sof(H16P)=Sof(H16Q)=Sof(H16R)=Sof(C168)=Sof(H16J)=Sof(H16K)=
 Sof(H16L)=Sof(C169)=Sof(H16M)=Sof(H16N)=Sof(H16O)=1-FVAR(2)
 Sof(C67)=Sof(H02Y)=Sof(HK)=Sof(HL)=Sof(C68)=Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=
 Sof(C69)=Sof(H02V)=Sof(H02W)=Sof(H02X)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,
 H89B), C90(H90A,H90B), C92(H92B,H92A), C93(H93A,H93B), C94(H94A,H94B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N23(H23), N26(H26), N48(H48), C9(H9), C11(H11), C14(H14),
 C15(H15), C18(H18), C20(H20), C29(H29), C31(H31), C34(H34), C35(H35), C38(H38),
  C40(H40), C44(H44), C45(H45), C46(H46), C49(H49)
5.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C71(H71A,H71B,H71C), C72(H72A,H72B,
 H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,
 H77B,H77C), C163(H16A,H16B,H16C), C164(H16G,H16H,H16I), C165(H16D,H16E,H16F),
 C167(H16P,H16Q,H16R), C168(H16J,H16K,H16L), C169(H16M,H16N,H16O), C87(H87A,
 H87B,H87C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C), C99(H99A,H99B,H99C),
 C63(H3AA,H3AB,H3AC), C64(H2AD,H2AE,H2AF), C65(H02U,H02S,H02T), C67(H02Y,HK,HL),
  C68(H1AB,H1AC,H1AD), C69(H02V,H02W,H02X)
5.d Idealised tetrahedral OH refined as rotating group:
 O80(H80), O81(H81), O59(H59)
;
_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
P78 P 0.51355(4) 0.53362(2) 0.32142(3) 0.0388(2) Uani 1 1 d . . . . .
O79 O 0.52982(10) 0.56040(6) 0.36516(7) 0.0465(5) Uani 1 1 d . . . . .
O80 O 0.45779(10) 0.55973(6) 0.29271(7) 0.0427(5) Uani 1 1 d . . . . .
H80 H 0.448325 0.546173 0.267897 0.064 Uiso 1 1 calc GR . . . .
O81 O 0.48228(10) 0.48622(6) 0.33267(8) 0.0479(5) Uani 1 1 d . . . . .
H81 H 0.509491 0.466563 0.337451 0.072 Uiso 1 1 calc GR . . . .
O82 O 0.56659(9) 0.52569(6) 0.29048(6) 0.0418(5) Uani 1 1 d . . . . .
O59 O 0.35296(11) 0.56443(6) 0.34626(8) 0.0492(6) Uani 1 1 d . . . . .
H59 H 0.384845 0.564318 0.332459 0.074 Uiso 1 1 calc GR . . . .
N3 N 0.53805(12) 0.64974(7) 0.40280(8) 0.0427(6) Uani 1 1 d . . . . .
H3 H 0.519452 0.625526 0.391303 0.051 Uiso 1 1 calc R . . . .
N6 N 0.63578(12) 0.56972(8) 0.42299(8) 0.0427(6) Uani 1 1 d . . . . .
H6 H 0.603796 0.556435 0.408554 0.051 Uiso 1 1 calc R . . . .
N23 N 0.33392(12) 0.45460(7) 0.21724(8) 0.0413(6) Uani 1 1 d . . . . .
H23 H 0.368248 0.468104 0.227120 0.050 Uiso 1 1 calc R . . . .
N26 N 0.30819(12) 0.55944(7) 0.18413(8) 0.0396(6) Uani 1 1 d . . . . .
H26 H 0.346273 0.560138 0.196373 0.047 Uiso 1 1 calc R . . . .
N42 N 0.55041(13) 0.40815(7) 0.34535(8) 0.0392(6) Uani 1 1 d . . . . .
N48 N 0.500000 0.66247(11) 0.250000 0.0461(9) Uani 1 2 d S T P . .
H48 H 0.500001 0.632914 0.249999 0.055 Uiso 1 2 calc RS T P . .
C1 C 0.45318(17) 0.70765(10) 0.38685(11) 0.0487(8) Uani 1 1 d . . . . .
C2 C 0.51289(16) 0.69346(9) 0.40270(10) 0.0438(8) Uani 1 1 d . . . . .
C4 C 0.59738(15) 0.65153(9) 0.42422(10) 0.0398(7) Uani 1 1 d . . . . .
C5 C 0.64108(15) 0.61646(9) 0.43393(10) 0.0399(7) Uani 1 1 d . . . . .
C7 C 0.69067(15) 0.54888(10) 0.43938(10) 0.0409(7) Uani 1 1 d . . . . .
C8 C 0.70780(15) 0.50252(10) 0.43771(10) 0.0427(7) Uani 1 1 d . . . . .
C9 C 0.76589(16) 0.49079(11) 0.46019(10) 0.0474(8) Uani 1 1 d . . . . .
H9 H 0.777862 0.460089 0.459761 0.057 Uiso 1 1 calc R . . . .
C10 C 0.80750(16) 0.52213(11) 0.48341(10) 0.0493(8) Uani 1 1 d . . . . .
C11 C 0.78896(15) 0.56829(11) 0.48301(10) 0.0460(8) Uani 1 1 d . . . . .
H11 H 0.815794 0.590241 0.497363 0.055 Uiso 1 1 calc R . . . .
C12 C 0.73153(15) 0.58185(10) 0.46170(10) 0.0442(8) Uani 1 1 d . . . . .
C13 C 0.69866(15) 0.62558(10) 0.45748(10) 0.0440(8) Uani 1 1 d . . . . .
C14 C 0.71385(16) 0.67110(10) 0.47287(10) 0.0463(8) Uani 1 1 d . . . . .
H14 H 0.752351 0.677442 0.489192 0.056 Uiso 1 1 calc R . . . .
C15 C 0.67076(16) 0.70553(10) 0.46322(10) 0.0491(8) Uani 1 1 d . . . . .
H15 H 0.680556 0.735375 0.472957 0.059 Uiso 1 1 calc R . . . .
C16 C 0.61233(16) 0.69652(10) 0.43899(10) 0.0450(8) Uani 1 1 d . . . . .
C17 C 0.55691(16) 0.72367(10) 0.42448(10) 0.0468(8) Uani 1 1 d . . . . .
C18 C 0.54049(18) 0.76994(10) 0.43067(11) 0.0561(9) Uani 1 1 d . . . . .
H18 H 0.569367 0.790149 0.445628 0.067 Uiso 1 1 calc R . . . .
C19 C 0.48160(19) 0.78544(10) 0.41459(12) 0.0624(10) Uani 1 1 d . . . . .
C20 C 0.43889(18) 0.75395(10) 0.39308(11) 0.0574(9) Uani 1 1 d . . . . .
H20 H 0.399135 0.764316 0.382434 0.069 Uiso 1 1 calc R . . . .
C21 C 0.35457(16) 0.37330(9) 0.24700(10) 0.0442(8) Uani 1 1 d . . . . .
C22 C 0.31994(16) 0.40843(9) 0.22287(10) 0.0427(8) Uani 1 1 d . . . . .
C24 C 0.28213(15) 0.47502(9) 0.19267(10) 0.0411(7) Uani 1 1 d . . . . .
C25 C 0.27030(15) 0.52104(9) 0.17892(10) 0.0398(7) Uani 1 1 d . . . . .
C27 C 0.27372(15) 0.59642(9) 0.16607(10) 0.0388(7) Uani 1 1 d . . . . .
C28 C 0.29146(15) 0.64279(9) 0.16369(10) 0.0391(7) Uani 1 1 d . . . . .
C29 C 0.24604(16) 0.67286(10) 0.14364(10) 0.0450(8) Uani 1 1 d . . . . .
H29 H 0.256806 0.703685 0.141329 0.054 Uiso 1 1 calc R . . . .
C30 C 0.18586(15) 0.65998(10) 0.12690(10) 0.0427(7) Uani 1 1 d . . . . .
C31 C 0.16992(16) 0.61379(10) 0.13096(10) 0.0471(8) Uani 1 1 d . . . . .
H31 H 0.129615 0.604078 0.121004 0.057 Uiso 1 1 calc R . . . .
C32 C 0.21415(15) 0.58190(9) 0.14992(10) 0.0411(7) Uani 1 1 d . . . . .
C33 C 0.21144(15) 0.53256(10) 0.15832(10) 0.0420(7) Uani 1 1 d . . . . .
C34 C 0.16427(16) 0.49985(10) 0.14865(11) 0.0490(8) Uani 1 1 d . . . . .
H34 H 0.125458 0.508549 0.134285 0.059 Uiso 1 1 calc R . . . .
C35 C 0.17594(16) 0.45475(10) 0.16060(10) 0.0486(8) Uani 1 1 d . . . . .
H35 H 0.145172 0.432538 0.154313 0.058 Uiso 1 1 calc R . . . .
C36 C 0.23481(16) 0.44258(10) 0.18240(10) 0.0456(8) Uani 1 1 d . . . . .
C37 C 0.26008(16) 0.39925(9) 0.20113(10) 0.0452(8) Uani 1 1 d . . . . .
C38 C 0.23596(18) 0.35487(10) 0.19971(11) 0.0560(9) Uani 1 1 d . . . . .
H38 H 0.196687 0.349282 0.184251 0.067 Uiso 1 1 calc R . . . .
C39 C 0.26990(19) 0.31889(10) 0.22114(11) 0.0551(9) Uani 1 1 d . . . . .
C40 C 0.32759(18) 0.32910(10) 0.24469(11) 0.0530(9) Uani 1 1 d . . . . .
H40 H 0.349937 0.305222 0.259947 0.064 Uiso 1 1 calc R . . . .
C41 C 0.60459(16) 0.40093(9) 0.37140(10) 0.0417(7) Uani 1 1 d . . . . .
C43 C 0.52141(17) 0.37151(9) 0.32399(10) 0.0457(8) Uani 1 1 d . . . . .
C44 C 0.54582(19) 0.32668(10) 0.32984(11) 0.0571(10) Uani 1 1 d . . . . .
H44 H 0.524799 0.301879 0.315209 0.068 Uiso 1 1 calc R . . . .
C45 C 0.60052(18) 0.32001(10) 0.35715(11) 0.0556(9) Uani 1 1 d . . . . .
H45 H 0.617299 0.290676 0.361326 0.067 Uiso 1 1 calc R . . . .
C46 C 0.63049(17) 0.35733(10) 0.37842(11) 0.0525(9) Uani 1 1 d . . . . .
H46 H 0.667726 0.353475 0.397315 0.063 Uiso 1 1 calc R . . . .
C47 C 0.45451(15) 0.68878(9) 0.22757(11) 0.0444(8) Uani 1 1 d . . . . .
C49 C 0.47209(18) 0.73348(11) 0.23570(15) 0.0823(13) Uani 1 1 d . . . . .
H49 H 0.450424 0.759345 0.224085 0.099 Uiso 1 1 calc R . . . .
C50 C 0.37097(15) 0.64494(9) 0.35650(10) 0.0433(8) Uani 1 1 d . . . . .
C51 C 0.40665(16) 0.67494(9) 0.36834(10) 0.0458(8) Uani 1 1 d . . . . .
C52 C 0.66769(15) 0.46871(10) 0.41437(10) 0.0439(7) Uani 1 1 d . . . . .
C53 C 0.63602(15) 0.43937(10) 0.39466(10) 0.0431(7) Uani 1 1 d . . . . .
C54 C 0.46303(18) 0.37842(9) 0.29656(11) 0.0430(8) Uani 1 1 d . . . . .
C55 C 0.41414(17) 0.37890(9) 0.27293(11) 0.0414(8) Uani 1 1 d . . . . .
C56 C 0.35093(16) 0.65831(9) 0.18306(10) 0.0386(7) Uani 1 1 d . . . . .
C57 C 0.39956(16) 0.67089(9) 0.20265(10) 0.0413(7) Uani 1 1 d . . . . .
C58 C 0.32451(15) 0.60914(9) 0.34232(11) 0.0439(8) Uani 1 1 d . . . . .
C60 C 0.29708(18) 0.61717(10) 0.29228(11) 0.0584(10) Uani 1 1 d . . . . .
H60A H 0.329811 0.616007 0.271502 0.088 Uiso 1 1 calc GR . . . .
H60B H 0.277370 0.646804 0.290032 0.088 Uiso 1 1 calc GR . . . .
H60C H 0.266661 0.593803 0.283545 0.088 Uiso 1 1 calc GR . . . .
C61 C 0.27407(17) 0.60863(11) 0.37654(12) 0.0606(10) Uani 1 1 d . . . . .
H61A H 0.242619 0.586459 0.366329 0.091 Uiso 1 1 calc GR . . . .
H61B H 0.255356 0.638547 0.377499 0.091 Uiso 1 1 calc GR . . . .
H61C H 0.292419 0.600579 0.407358 0.091 Uiso 1 1 calc GR . . . .
C62 C 0.4633(2) 0.83604(11) 0.42127(17) 0.0899(15) Uani 1 1 d D . . . .
C66 C 0.86970(16) 0.50652(13) 0.50701(12) 0.0592(10) Uani 1 1 d D . . . .
C70 C 0.2447(2) 0.26962(11) 0.21656(13) 0.0712(12) Uani 1 1 d . . . . .
C71 C 0.2472(2) 0.25346(11) 0.16565(12) 0.0712(11) Uani 1 1 d . . . . .
H71A H 0.225539 0.275119 0.144677 0.107 Uiso 1 1 calc GR . . . .
H71B H 0.227636 0.223878 0.161721 0.107 Uiso 1 1 calc GR . . . .
H71C H 0.290018 0.251276 0.158683 0.107 Uiso 1 1 calc GR . . . .
C72 C 0.1761(2) 0.26740(12) 0.22784(13) 0.0894(15) Uani 1 1 d . . . . .
H72A H 0.172846 0.278652 0.259138 0.134 Uiso 1 1 calc GR . . . .
H72B H 0.161838 0.236147 0.225662 0.134 Uiso 1 1 calc GR . . . .
H72C H 0.150913 0.286006 0.205781 0.134 Uiso 1 1 calc GR . . . .
C73 C 0.2826(3) 0.23706(12) 0.24992(16) 0.120(2) Uani 1 1 d . . . . .
H73A H 0.321985 0.230647 0.237776 0.180 Uiso 1 1 calc GR . . . .
H73B H 0.259914 0.208912 0.252637 0.180 Uiso 1 1 calc GR . . . .
H73C H 0.289885 0.251148 0.280338 0.180 Uiso 1 1 calc GR . . . .
C74 C 0.13676(16) 0.69465(11) 0.10674(12) 0.0535(9) Uani 1 1 d . . . . .
C75 C 0.10668(19) 0.67847(12) 0.05886(12) 0.0679(11) Uani 1 1 d . . . . .
H75A H 0.138671 0.673244 0.038042 0.102 Uiso 1 1 calc GR . . . .
H75B H 0.078357 0.701603 0.045761 0.102 Uiso 1 1 calc GR . . . .
H75C H 0.084168 0.650431 0.062787 0.102 Uiso 1 1 calc GR . . . .
C76 C 0.16522(18) 0.74222(11) 0.09909(14) 0.0688(11) Uani 1 1 d . . . . .
H76A H 0.180020 0.755237 0.128946 0.103 Uiso 1 1 calc GR . . . .
H76B H 0.133935 0.761957 0.083657 0.103 Uiso 1 1 calc GR . . . .
H76C H 0.199481 0.739195 0.079901 0.103 Uiso 1 1 calc GR . . . .
C77 C 0.08631(19) 0.70015(14) 0.14067(13) 0.0762(12) Uani 1 1 d . . . . .
H77A H 0.067185 0.670891 0.145392 0.114 Uiso 1 1 calc GR . . . .
H77B H 0.055160 0.721408 0.127737 0.114 Uiso 1 1 calc GR . . . .
H77C H 0.104835 0.711618 0.170250 0.114 Uiso 1 1 calc GR . . . .
C163 C 0.5030(7) 0.8684(3) 0.4035(5) 0.117(4) Uani 0.475(8) 1 d D U . A 2
H16A H 0.543832 0.865919 0.420024 0.176 Uiso 0.475(8) 1 calc GR . . A 2
H16B H 0.486713 0.898678 0.407746 0.176 Uiso 0.475(8) 1 calc GR . . A 2
H16C H 0.505690 0.862758 0.370643 0.176 Uiso 0.475(8) 1 calc GR . . A 2
C164 C 0.4626(6) 0.8447(4) 0.4789(3) 0.105(4) Uani 0.475(8) 1 d D U . A 2
H16G H 0.431205 0.825623 0.490858 0.158 Uiso 0.475(8) 1 calc GR . . A 2
H16H H 0.453306 0.876420 0.484540 0.158 Uiso 0.475(8) 1 calc GR . . A 2
H16I H 0.502796 0.837181 0.494392 0.158 Uiso 0.475(8) 1 calc GR . . A 2
C165 C 0.3963(6) 0.8461(5) 0.4037(5) 0.090(4) Uani 0.475(8) 1 d D U . A 2
H16D H 0.389991 0.839596 0.370666 0.134 Uiso 0.475(8) 1 calc GR . . A 2
H16E H 0.387239 0.877843 0.409109 0.134 Uiso 0.475(8) 1 calc GR . . A 2
H16F H 0.368902 0.827117 0.420277 0.134 Uiso 0.475(8) 1 calc GR . . A 2
C167 C 0.9018(4) 0.5372(3) 0.5397(3) 0.059(3) Uani 0.460(6) 1 d D . . B 2
H16P H 0.873768 0.547462 0.561935 0.088 Uiso 0.460(6) 1 calc GR . . B 2
H16Q H 0.916610 0.563153 0.523237 0.088 Uiso 0.460(6) 1 calc GR . . B 2
H16R H 0.936647 0.521571 0.556132 0.088 Uiso 0.460(6) 1 calc GR . . B 2
C168 C 0.9110(4) 0.4837(3) 0.4733(3) 0.059(2) Uani 0.460(6) 1 d D . . B 2
H16J H 0.887148 0.461117 0.454865 0.089 Uiso 0.460(6) 1 calc GR . . B 2
H16K H 0.945686 0.468963 0.490923 0.089 Uiso 0.460(6) 1 calc GR . . B 2
H16L H 0.926324 0.506434 0.452906 0.089 Uiso 0.460(6) 1 calc GR . . B 2
C169 C 0.8561(4) 0.4591(2) 0.5403(3) 0.061(3) Uani 0.460(6) 1 d D . . B 2
H16M H 0.826266 0.466702 0.562158 0.092 Uiso 0.460(6) 1 calc GR . . B 2
H16N H 0.894530 0.449450 0.557178 0.092 Uiso 0.460(6) 1 calc GR . . B 2
H16O H 0.839889 0.434730 0.520066 0.092 Uiso 0.460(6) 1 calc GR . . B 2
N83 N 0.33266(13) 0.42523(7) 0.40305(8) 0.0436(6) Uani 1 1 d . . . . .
C84 C 0.39029(15) 0.39640(9) 0.39899(10) 0.0453(8) Uani 1 1 d . . . . .
H84A H 0.423446 0.416458 0.390280 0.054 Uiso 1 1 calc R . . . .
H84B H 0.381358 0.374761 0.373408 0.054 Uiso 1 1 calc R . . . .
C85 C 0.41469(16) 0.36960(10) 0.44237(11) 0.0504(9) Uani 1 1 d . . . . .
H85A H 0.382371 0.349171 0.451803 0.060 Uiso 1 1 calc R . . . .
H85B H 0.426015 0.390626 0.468109 0.060 Uiso 1 1 calc R . . . .
C86 C 0.47201(17) 0.34159(10) 0.43147(11) 0.0544(9) Uani 1 1 d . . . . .
H86A H 0.461134 0.323010 0.403716 0.065 Uiso 1 1 calc R . . . .
H86B H 0.504995 0.362539 0.424298 0.065 Uiso 1 1 calc R . . . .
C87 C 0.49673(19) 0.31023(11) 0.47175(12) 0.0654(10) Uani 1 1 d . . . . .
H87A H 0.534062 0.295155 0.463657 0.098 Uiso 1 1 calc GR . . . .
H87B H 0.465655 0.287609 0.477226 0.098 Uiso 1 1 calc GR . . . .
H87C H 0.506027 0.328196 0.499718 0.098 Uiso 1 1 calc GR . . . .
C88 C 0.27815(16) 0.39565(10) 0.41599(10) 0.0486(8) Uani 1 1 d . . . . .
H88A H 0.291104 0.379429 0.444929 0.058 Uiso 1 1 calc R . . . .
H88B H 0.243973 0.415852 0.422364 0.058 Uiso 1 1 calc R . . . .
C89 C 0.25372(17) 0.36082(10) 0.37963(11) 0.0517(9) Uani 1 1 d . . . . .
H89A H 0.287248 0.340183 0.372867 0.062 Uiso 1 1 calc R . . . .
H89B H 0.239146 0.376513 0.350716 0.062 Uiso 1 1 calc R . . . .
C90 C 0.2006(2) 0.33337(13) 0.39714(12) 0.0725(12) Uani 1 1 d . . . . .
H90A H 0.216180 0.316245 0.424903 0.087 Uiso 1 1 calc R . . . .
H90B H 0.168758 0.354423 0.406254 0.087 Uiso 1 1 calc R . . . .
C91 C 0.17107(19) 0.30026(11) 0.36086(12) 0.0672(11) Uani 1 1 d . . . . .
H91A H 0.151650 0.317188 0.334611 0.101 Uiso 1 1 calc GR . . . .
H91B H 0.140112 0.282108 0.374610 0.101 Uiso 1 1 calc GR . . . .
H91C H 0.202715 0.280438 0.350316 0.101 Uiso 1 1 calc GR . . . .
C92 C 0.31694(16) 0.44842(9) 0.35578(10) 0.0451(8) Uani 1 1 d . . . . .
H92B H 0.314786 0.425022 0.331476 0.054 Uiso 1 1 calc R . . . .
H92A H 0.350908 0.469038 0.349979 0.054 Uiso 1 1 calc R . . . .
C93 C 0.25615(16) 0.47556(9) 0.35107(10) 0.0473(8) Uani 1 1 d . . . . .
H93A H 0.222932 0.457125 0.362325 0.057 Uiso 1 1 calc R . . . .
H93B H 0.260819 0.503055 0.370292 0.057 Uiso 1 1 calc R . . . .
C94 C 0.23892(16) 0.48881(10) 0.30062(10) 0.0491(8) Uani 1 1 d . . . . .
H94A H 0.236512 0.461176 0.281535 0.059 Uiso 1 1 calc R . . . .
H94B H 0.271954 0.507889 0.290035 0.059 Uiso 1 1 calc R . . . .
C95 C 0.17739(17) 0.51452(11) 0.29249(12) 0.0605(10) Uani 1 1 d . . . . .
H95A H 0.169304 0.521595 0.259652 0.091 Uiso 1 1 calc GR . . . .
H95B H 0.179753 0.542509 0.310368 0.091 Uiso 1 1 calc GR . . . .
H95C H 0.144199 0.495717 0.302300 0.091 Uiso 1 1 calc GR . . . .
C96 C 0.34458(16) 0.46084(9) 0.44180(10) 0.0470(8) Uani 1 1 d . . . . .
H96A H 0.306971 0.479159 0.442799 0.056 Uiso 1 1 calc R . . . .
H96B H 0.351240 0.444732 0.471580 0.056 Uiso 1 1 calc R . . . .
C97 C 0.39892(16) 0.49319(9) 0.43800(10) 0.0464(8) Uani 1 1 d . . . . .
H97A H 0.393490 0.509516 0.408286 0.056 Uiso 1 1 calc R . . . .
H97B H 0.437480 0.475721 0.438754 0.056 Uiso 1 1 calc R . . . .
C98 C 0.40310(17) 0.52753(10) 0.47841(11) 0.0517(9) Uani 1 1 d . . . . .
H98A H 0.363531 0.543595 0.478595 0.062 Uiso 1 1 calc R . . . .
H98B H 0.410455 0.511081 0.507951 0.062 Uiso 1 1 calc R . . . .
C99 C 0.45504(18) 0.56233(11) 0.47460(12) 0.0615(10) Uani 1 1 d . . . . .
H99A H 0.447309 0.579322 0.445835 0.092 Uiso 1 1 calc GR . . . .
H99B H 0.494368 0.546607 0.474748 0.092 Uiso 1 1 calc GR . . . .
H99C H 0.456311 0.583089 0.500817 0.092 Uiso 1 1 calc GR . . . .
C63 C 0.4708(5) 0.8575(3) 0.3668(4) 0.102(4) Uani 0.525(8) 1 d D U . A 1
H3AA H 0.512155 0.851182 0.358111 0.152 Uiso 0.525(8) 1 calc GR . . A 1
H3AB H 0.464028 0.890075 0.366890 0.152 Uiso 0.525(8) 1 calc GR . . A 1
H3AC H 0.440571 0.843266 0.344539 0.152 Uiso 0.525(8) 1 calc GR . . A 1
C64 C 0.5113(5) 0.8617(2) 0.4490(4) 0.097(4) Uani 0.525(8) 1 d D U . A 1
H2AD H 0.519554 0.847485 0.479273 0.145 Uiso 0.525(8) 1 calc GR . . A 1
H2AE H 0.497268 0.892696 0.452986 0.145 Uiso 0.525(8) 1 calc GR . . A 1
H2AF H 0.548868 0.862020 0.433149 0.145 Uiso 0.525(8) 1 calc GR . . A 1
C65 C 0.3955(5) 0.8419(4) 0.4267(4) 0.076(3) Uani 0.525(8) 1 d D U . A 1
H02U H 0.385532 0.827342 0.455234 0.114 Uiso 0.525(8) 1 calc GR . . A 1
H02S H 0.371482 0.828073 0.400381 0.114 Uiso 0.525(8) 1 calc GR . . A 1
H02T H 0.385821 0.874056 0.427887 0.114 Uiso 0.525(8) 1 calc GR . . A 1
C67 C 0.9213(3) 0.53859(19) 0.4830(2) 0.055(2) Uani 0.540(6) 1 d D . . B 1
H02Y H 0.921137 0.531104 0.450265 0.083 Uiso 0.540(6) 1 calc GR . . B 1
HK H 0.962143 0.532983 0.498535 0.083 Uiso 0.540(6) 1 calc GR . . B 1
HL H 0.910729 0.570423 0.486292 0.083 Uiso 0.540(6) 1 calc GR . . B 1
C68 C 0.8854(3) 0.46062(19) 0.5005(3) 0.059(2) Uani 0.540(6) 1 d D . . B 1
H1AB H 0.854185 0.441187 0.512292 0.089 Uiso 0.540(6) 1 calc GR . . B 1
H1AC H 0.925303 0.454290 0.517185 0.089 Uiso 0.540(6) 1 calc GR . . B 1
H1AD H 0.887432 0.454757 0.467590 0.089 Uiso 0.540(6) 1 calc GR . . B 1
C69 C 0.8761(4) 0.5240(3) 0.5591(3) 0.061(2) Uani 0.540(6) 1 d D . . B 1
H02V H 0.864718 0.555894 0.559846 0.091 Uiso 0.540(6) 1 calc GR . . B 1
H02W H 0.918543 0.520337 0.572272 0.091 Uiso 0.540(6) 1 calc GR . . B 1
H02X H 0.848871 0.506504 0.577231 0.091 Uiso 0.540(6) 1 calc GR . . B 1


_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
P78 O79 1.486(2) . ?
P78 O80 1.583(2) . ?
P78 O81 1.5796(19) . ?
P78 O82 1.520(2) . ?
O59 C58 1.437(3) . ?
N3 C2 1.382(4) . ?
N3 C4 1.363(4) . ?
N6 C5 1.398(3) . ?
N6 C7 1.370(4) . ?
N23 C22 1.389(3) . ?
N23 C24 1.393(4) . ?
N26 C25 1.382(3) . ?
N26 C27 1.379(3) . ?
N42 C41 1.339(4) . ?
N42 C43 1.352(4) . ?
N48 C47 1.355(3) . ?
N48 C47 1.355(3) 2_655 ?
C1 C2 1.384(4) . ?
C1 C20 1.396(4) . ?
C1 C51 1.445(4) . ?
C2 C17 1.395(4) . ?
C4 C5 1.397(4) . ?
C4 C16 1.403(4) . ?
C5 C13 1.379(4) . ?
C7 C8 1.400(4) . ?
C7 C12 1.412(4) . ?
C8 C9 1.392(4) . ?
C8 C52 1.432(4) . ?
C9 C10 1.401(4) . ?
C10 C11 1.401(4) . ?
C10 C66 1.510(5) . ?
C11 C12 1.382(4) . ?
C12 C13 1.455(4) . ?
C13 C14 1.424(4) . ?
C14 C15 1.375(4) . ?
C15 C16 1.401(4) . ?
C16 C17 1.457(4) . ?
C17 C18 1.407(4) . ?
C18 C19 1.381(5) . ?
C19 C20 1.398(4) . ?
C19 C62 1.540(5) . ?
C21 C22 1.407(4) . ?
C21 C40 1.409(4) . ?
C21 C55 1.428(5) . ?
C22 C37 1.401(4) . ?
C24 C25 1.412(4) . ?
C24 C36 1.398(4) . ?
C25 C33 1.386(4) . ?
C27 C28 1.405(4) . ?
C27 C32 1.386(4) . ?
C28 C29 1.394(4) . ?
C28 C56 1.419(4) . ?
C29 C30 1.388(4) . ?
C30 C31 1.394(4) . ?
C30 C74 1.533(4) . ?
C31 C32 1.401(4) . ?
C32 C33 1.457(4) . ?
C33 C34 1.399(4) . ?
C34 C35 1.373(4) . ?
C35 C36 1.403(4) . ?
C36 C37 1.455(4) . ?
C37 C38 1.391(4) . ?
C38 C39 1.386(5) . ?
C39 C40 1.387(5) . ?
C39 C70 1.534(4) . ?
C41 C46 1.392(4) . ?
C41 C53 1.438(4) . ?
C43 C44 1.410(4) . ?
C43 C54 1.431(5) . ?
C44 C45 1.363(5) . ?
C45 C46 1.375(4) . ?
C47 C49 1.368(4) . ?
C47 C57 1.420(4) . ?
C49 C49 1.388(7) 2_655 ?
C50 C51 1.190(4) . ?
C50 C58 1.473(4) . ?
C52 C53 1.199(4) . ?
C54 C55 1.195(4) . ?
C56 C57 1.196(4) . ?
C58 C60 1.513(4) . ?
C58 C61 1.522(4) . ?
C62 C163 1.395(10) . ?
C62 C164 1.664(9) . ?
C62 C165 1.509(13) . ?
C62 C63 1.697(9) . ?
C62 C64 1.450(8) . ?
C62 C65 1.486(12) . ?
C66 C167 1.424(9) . ?
C66 C168 1.519(7) . ?
C66 C169 1.713(8) . ?
C66 C67 1.644(7) . ?
C66 C68 1.394(6) . ?
C66 C69 1.567(8) . ?
C70 C71 1.533(5) . ?
C70 C72 1.535(6) . ?
C70 C73 1.526(5) . ?
C74 C75 1.532(4) . ?
C74 C76 1.536(5) . ?
C74 C77 1.525(5) . ?
N83 C84 1.508(4) . ?
N83 C88 1.525(4) . ?
N83 C92 1.519(3) . ?
N83 C96 1.520(3) . ?
C84 C85 1.516(4) . ?
C85 C86 1.531(4) . ?
C86 C87 1.525(4) . ?
C88 C89 1.511(4) . ?
C89 C90 1.514(4) . ?
C90 C91 1.511(4) . ?
C92 C93 1.521(4) . ?
C93 C94 1.504(4) . ?
C94 C95 1.518(5) . ?
C96 C97 1.510(4) . ?
C97 C98 1.523(4) . ?
C98 C99 1.517(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O79 P78 O80 107.03(11) . . ?
O79 P78 O81 111.04(12) . . ?
O79 P78 O82 115.85(12) . . ?
O81 P78 O80 102.06(12) . . ?
O82 P78 O80 110.07(11) . . ?
O82 P78 O81 109.86(11) . . ?
C4 N3 C2 108.3(2) . . ?
C7 N6 C5 107.7(2) . . ?
C22 N23 C24 107.4(2) . . ?
C27 N26 C25 107.4(2) . . ?
C41 N42 C43 117.9(2) . . ?
C47 N48 C47 111.2(3) . 2_655 ?
C2 C1 C20 117.0(3) . . ?
C2 C1 C51 120.8(3) . . ?
C20 C1 C51 122.0(3) . . ?
N3 C2 C1 128.7(3) . . ?
N3 C2 C17 109.3(3) . . ?
C1 C2 C17 121.9(3) . . ?
N3 C4 C5 130.1(3) . . ?
N3 C4 C16 110.5(3) . . ?
C5 C4 C16 119.4(3) . . ?
C4 C5 N6 128.8(3) . . ?
C13 C5 N6 110.3(3) . . ?
C13 C5 C4 120.8(3) . . ?
N6 C7 C8 129.5(3) . . ?
N6 C7 C12 109.5(3) . . ?
C8 C7 C12 121.0(3) . . ?
C7 C8 C52 121.9(3) . . ?
C9 C8 C7 116.6(3) . . ?
C9 C8 C52 121.5(3) . . ?
C8 C9 C10 124.4(3) . . ?
C9 C10 C66 121.0(3) . . ?
C11 C10 C9 116.9(3) . . ?
C11 C10 C66 122.1(3) . . ?
C12 C11 C10 121.3(3) . . ?
C7 C12 C13 106.2(3) . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 C13 133.9(3) . . ?
C5 C13 C12 106.2(3) . . ?
C5 C13 C14 120.0(3) . . ?
C14 C13 C12 133.8(3) . . ?
C15 C14 C13 119.0(3) . . ?
C14 C15 C16 121.2(3) . . ?
C4 C16 C17 105.2(3) . . ?
C15 C16 C4 119.6(3) . . ?
C15 C16 C17 135.3(3) . . ?
C2 C17 C16 106.7(3) . . ?
C2 C17 C18 119.4(3) . . ?
C18 C17 C16 133.7(3) . . ?
C19 C18 C17 120.2(3) . . ?
C18 C19 C20 118.4(3) . . ?
C18 C19 C62 120.5(3) . . ?
C20 C19 C62 121.1(3) . . ?
C1 C20 C19 123.0(3) . . ?
C22 C21 C40 116.3(3) . . ?
C22 C21 C55 125.4(3) . . ?
C40 C21 C55 118.3(3) . . ?
N23 C22 C21 130.5(3) . . ?
N23 C22 C37 109.4(3) . . ?
C37 C22 C21 120.1(3) . . ?
N23 C24 C25 131.3(3) . . ?
N23 C24 C36 110.4(2) . . ?
C36 C24 C25 118.2(3) . . ?
N26 C25 C24 130.3(3) . . ?
N26 C25 C33 110.8(2) . . ?
C33 C25 C24 118.8(3) . . ?
N26 C27 C28 128.9(3) . . ?
N26 C27 C32 109.5(2) . . ?
C32 C27 C28 121.5(3) . . ?
C27 C28 C56 121.7(3) . . ?
C29 C28 C27 116.1(3) . . ?
C29 C28 C56 122.1(3) . . ?
C30 C29 C28 124.5(3) . . ?
C29 C30 C31 117.4(3) . . ?
C29 C30 C74 122.6(3) . . ?
C31 C30 C74 120.0(3) . . ?
C30 C31 C32 120.5(3) . . ?
C27 C32 C31 120.0(3) . . ?
C27 C32 C33 107.2(3) . . ?
C31 C32 C33 132.8(3) . . ?
C25 C33 C32 105.0(3) . . ?
C25 C33 C34 122.4(3) . . ?
C34 C33 C32 132.6(3) . . ?
C35 C34 C33 119.2(3) . . ?
C34 C35 C36 119.2(3) . . ?
C24 C36 C35 122.1(3) . . ?
C24 C36 C37 105.5(3) . . ?
C35 C36 C37 132.3(3) . . ?
C22 C37 C36 107.1(3) . . ?
C38 C37 C22 120.9(3) . . ?
C38 C37 C36 131.9(3) . . ?
C39 C38 C37 120.6(3) . . ?
C38 C39 C40 117.6(3) . . ?
C38 C39 C70 120.1(3) . . ?
C40 C39 C70 122.3(3) . . ?
C39 C40 C21 124.3(3) . . ?
N42 C41 C46 122.6(3) . . ?
N42 C41 C53 118.8(3) . . ?
C46 C41 C53 118.5(3) . . ?
N42 C43 C44 121.7(3) . . ?
N42 C43 C54 118.8(3) . . ?
C44 C43 C54 119.5(3) . . ?
C45 C44 C43 119.4(3) . . ?
C44 C45 C46 119.0(3) . . ?
C45 C46 C41 119.4(3) . . ?
N48 C47 C49 106.3(3) . . ?
N48 C47 C57 124.1(3) . . ?
C49 C47 C57 129.6(3) . . ?
C47 C49 C49 108.1(2) . 2_655 ?
C51 C50 C58 177.5(3) . . ?
C50 C51 C1 173.3(3) . . ?
C53 C52 C8 177.5(3) . . ?
C52 C53 C41 173.3(3) . . ?
C55 C54 C43 172.5(3) . . ?
C54 C55 C21 172.2(3) . . ?
C57 C56 C28 175.1(3) . . ?
C56 C57 C47 175.3(3) . . ?
O59 C58 C50 110.2(3) . . ?
O59 C58 C60 109.9(2) . . ?
O59 C58 C61 105.2(2) . . ?
C50 C58 C60 110.3(2) . . ?
C50 C58 C61 109.5(2) . . ?
C60 C58 C61 111.6(3) . . ?
C19 C62 C164 107.0(4) . . ?
C19 C62 C63 101.0(4) . . ?
C163 C62 C19 115.4(6) . . ?
C163 C62 C164 108.4(7) . . ?
C163 C62 C165 110.2(8) . . ?
C165 C62 C19 113.0(6) . . ?
C165 C62 C164 101.8(7) . . ?
C64 C62 C19 112.6(4) . . ?
C64 C62 C63 100.9(7) . . ?
C64 C62 C65 122.6(7) . . ?
C65 C62 C19 112.7(5) . . ?
C65 C62 C63 103.2(6) . . ?
C10 C66 C168 113.1(4) . . ?
C10 C66 C169 107.5(4) . . ?
C10 C66 C67 104.2(3) . . ?
C10 C66 C69 108.9(4) . . ?
C167 C66 C10 117.4(5) . . ?
C167 C66 C168 114.5(6) . . ?
C167 C66 C169 103.7(5) . . ?
C168 C66 C169 97.9(5) . . ?
C68 C66 C10 116.3(4) . . ?
C68 C66 C67 108.0(4) . . ?
C68 C66 C69 115.9(5) . . ?
C69 C66 C67 101.9(5) . . ?
C39 C70 C72 111.0(3) . . ?
C71 C70 C39 109.0(3) . . ?
C71 C70 C72 107.6(3) . . ?
C73 C70 C39 111.2(3) . . ?
C73 C70 C71 109.8(4) . . ?
C73 C70 C72 108.1(4) . . ?
C30 C74 C76 112.2(3) . . ?
C75 C74 C30 110.7(3) . . ?
C75 C74 C76 106.9(3) . . ?
C77 C74 C30 109.5(3) . . ?
C77 C74 C75 109.4(3) . . ?
C77 C74 C76 108.1(3) . . ?
C84 N83 C88 111.0(2) . . ?
C84 N83 C92 107.3(2) . . ?
C84 N83 C96 110.5(2) . . ?
C92 N83 C88 110.6(2) . . ?
C92 N83 C96 110.7(2) . . ?
C96 N83 C88 106.9(2) . . ?
N83 C84 C85 116.7(2) . . ?
C84 C85 C86 109.4(3) . . ?
C87 C86 C85 113.4(3) . . ?
C89 C88 N83 116.0(2) . . ?
C88 C89 C90 110.6(3) . . ?
C91 C90 C89 113.1(3) . . ?
N83 C92 C93 115.4(2) . . ?
C94 C93 C92 110.6(2) . . ?
C93 C94 C95 114.1(3) . . ?
C97 C96 N83 116.9(2) . . ?
C96 C97 C98 110.4(3) . . ?
C99 C98 C97 112.2(3) . . ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hm7merge_a
_database_code_depnum_ccdc_archive 'CCDC 1881086'
_audit_update_record             
;
2018-11-25 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;
_audit_creation_date             2018-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        Inverted_pyridine_heptamer
_chemical_formula_moiety         '2(H2 O4 P), C141 H127 N11 O2, 2(C16 H36 N)'
_chemical_formula_sum            'C173 H203 N13 O10 P2'
_chemical_formula_weight         2686.41
_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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.505(4)
_cell_length_b                   29.114(6)
_cell_length_c                   28.751(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.83(3)
_cell_angle_gamma                90
_cell_volume                     17937(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    400159
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5768
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            94417
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.397
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13239
_reflns_number_total             24407
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.00064(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         24407
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0904
_refine_ls_restrained_S_all      1.027
_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)+(0.1712P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2576
_refine_ls_wR_factor_ref         0.2822
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C65-C63
 1.6 with sigma of 0.002
 C66-C63 \\sim C65-C63 \\sim C64-C63
 with sigma of 0.002
 C168-C67 \\sim C68-C67 \\sim C69-C67 \\sim C169-C67 \\sim C170-C67 \\sim
C70-C67
 with sigma of 0.002
 C64-C63 \\sim C165-C63 \\sim C65-C63 \\sim C166-C63 \\sim C66-C63 \\sim
C164-C63
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C169) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C164) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C166) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C165)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C166) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5) H65A(0.5)
 H65B(0.5) H65C(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C68(0.75)
 H68A(0.75) H68B(0.75) H68C(0.75) C69(0.75) H69A(0.75) H69B(0.75) H69C(0.75)
 C70(0.75) H70A(0.75) H70B(0.75) H70C(0.75) C164(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C165(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C166(0.5) H16G(0.5)
 H16H(0.5) H16I(0.5) C168(0.25) H16J(0.25) H16K(0.25) H16L(0.25) C169(0.25)
 H16M(0.25) H16N(0.25) H16O(0.25) C170(0.25) H17A(0.25) H17B(0.25) H17C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C89(H89A,H89B), C90(H90A,
 H90B), C91(H91A,H91B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N23(H23), N26(H26), C9(H9), C11(H11), C14(H14), C15(H15),
 C18(H18), C20(H20), C29(H29), C31(H31), C34(H34), C35(H35), C38(H38), C40(H40),
  C44(H44), C45(H45), C46(H46), C48(H48), C50(H50)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C164(H16A,H16B,
 H16C), C165(H16D,H16E,H16F), C166(H16G,H16H,H16I), C168(H16J,H16K,H16L),
 C169(H16M,H16N,H16O), C170(H17A,H17B,H17C), C88(H88A,H88B,H88C), C92(H92A,H92B,
 H92C), C96(H96A,H96B,H96C), C100(H10A,H10B,H10C)
5.d Idealised tetrahedral OH refined as rotating group:
 O80(H80), O83(H83), O52(H52)
;
_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
P79 P 0.51270(3) 0.46725(2) 0.32152(2) 0.04061(16) Uani 1 1 d . . . . .
O80 O 0.45648(8) 0.44175(6) 0.29321(6) 0.0443(4) Uani 1 1 d . . . . .
H80 H 0.448901 0.454508 0.267148 0.066 Uiso 1 1 calc GR . . . .
O81 O 0.52868(9) 0.44054(6) 0.36521(6) 0.0489(4) Uani 1 1 d . . . . .
O82 O 0.56581(8) 0.47419(6) 0.29037(6) 0.0439(4) Uani 1 1 d . . . . .
O83 O 0.48275(9) 0.51487(6) 0.33277(7) 0.0483(4) Uani 1 1 d . . . . .
H83 H 0.510732 0.535053 0.335533 0.072 Uiso 1 1 calc GR . . . .
O52 O 0.35030(9) 0.43538(6) 0.34371(7) 0.0497(4) Uani 1 1 d . . . . .
H52 H 0.382373 0.437088 0.329021 0.074 Uiso 1 1 calc GR . . . .
N3 N 0.53617(10) 0.35286(7) 0.40337(7) 0.0452(5) Uani 1 1 d . . . . .
H3 H 0.516867 0.377553 0.391929 0.054 Uiso 1 1 calc R . . . .
N6 N 0.63367(10) 0.43289(7) 0.42363(7) 0.0442(5) Uani 1 1 d . . . . .
H6 H 0.601168 0.446783 0.409261 0.053 Uiso 1 1 calc R . . . .
N23 N 0.33451(10) 0.54339(7) 0.21650(7) 0.0439(5) Uani 1 1 d . . . . .
H23 H 0.369593 0.529732 0.226576 0.053 Uiso 1 1 calc R . . . .
N26 N 0.31083(10) 0.43881(6) 0.18226(7) 0.0409(4) Uani 1 1 d . . . . .
H26 H 0.349909 0.438298 0.194102 0.049 Uiso 1 1 calc R . . . .
N42 N 0.54993(10) 0.59314(7) 0.34450(7) 0.0431(5) Uani 1 1 d . . . . .
N49 N 0.500000 0.23023(12) 0.250000 0.0838(14) Uani 1 2 d S T P . .
C1 C 0.45291(14) 0.29406(9) 0.38664(10) 0.0510(6) Uani 1 1 d . . . . .
C2 C 0.51223(13) 0.30905(8) 0.40281(9) 0.0474(6) Uani 1 1 d . . . . .
C4 C 0.59581(12) 0.35120(8) 0.42503(9) 0.0448(6) Uani 1 1 d . . . . .
C5 C 0.63809(12) 0.38674(8) 0.43396(9) 0.0430(5) Uani 1 1 d . . . . .
C7 C 0.68912(12) 0.45353(9) 0.43975(9) 0.0449(6) Uani 1 1 d . . . . .
C8 C 0.70630(13) 0.49999(9) 0.43736(9) 0.0478(6) Uani 1 1 d . . . . .
C9 C 0.76490(13) 0.51202(10) 0.45870(10) 0.0525(6) Uani 1 1 d . . . . .
H9 H 0.777494 0.543261 0.457818 0.063 Uiso 1 1 calc R . . . .
C10 C 0.80597(14) 0.48011(10) 0.48137(10) 0.0541(7) Uani 1 1 d . . . . .
C11 C 0.78724(13) 0.43422(10) 0.48209(9) 0.0503(6) Uani 1 1 d . . . . .
H11 H 0.814610 0.411995 0.496815 0.060 Uiso 1 1 calc R . . . .
C12 C 0.72939(12) 0.42037(9) 0.46171(9) 0.0431(5) Uani 1 1 d . . . . .
C13 C 0.69623(12) 0.37733(9) 0.45791(9) 0.0455(6) Uani 1 1 d . . . . .
C14 C 0.71180(13) 0.33192(9) 0.47318(10) 0.0484(6) Uani 1 1 d . . . . .
H14 H 0.751176 0.325781 0.489498 0.058 Uiso 1 1 calc R . . . .
C15 C 0.66950(13) 0.29711(9) 0.46414(10) 0.0506(6) Uani 1 1 d . . . . .
H15 H 0.679628 0.266769 0.474295 0.061 Uiso 1 1 calc R . . . .
C16 C 0.61111(14) 0.30616(8) 0.43986(9) 0.0482(6) Uani 1 1 d . . . . .
C17 C 0.55636(13) 0.27881(9) 0.42524(10) 0.0502(6) Uani 1 1 d . . . . .
C18 C 0.54039(16) 0.23273(9) 0.43163(11) 0.0604(8) Uani 1 1 d . . . . .
H18 H 0.569678 0.212397 0.447307 0.072 Uiso 1 1 calc R . . . .
C19 C 0.48217(18) 0.21678(9) 0.41519(13) 0.0697(9) Uani 1 1 d . . . . .
C20 C 0.43970(16) 0.24748(10) 0.39288(12) 0.0648(8) Uani 1 1 d . . . . .
H20 H 0.399875 0.236236 0.381359 0.078 Uiso 1 1 calc R . . . .
C21 C 0.35388(13) 0.62441(8) 0.24601(9) 0.0460(6) Uani 1 1 d . . . . .
C22 C 0.32027(13) 0.58924(8) 0.22223(9) 0.0462(6) Uani 1 1 d . . . . .
C24 C 0.28339(12) 0.52267(8) 0.19190(9) 0.0446(6) Uani 1 1 d . . . . .
C25 C 0.27241(12) 0.47690(8) 0.17818(9) 0.0429(5) Uani 1 1 d . . . . .
C27 C 0.27660(12) 0.40160(8) 0.16431(9) 0.0426(5) Uani 1 1 d . . . . .
C28 C 0.29407(12) 0.35531(8) 0.16141(9) 0.0435(5) Uani 1 1 d . . . . .
C29 C 0.24858(13) 0.32488(8) 0.14168(9) 0.0475(6) Uani 1 1 d . . . . .
H29 H 0.259579 0.293445 0.139018 0.057 Uiso 1 1 calc R . . . .
C30 C 0.18843(13) 0.33806(9) 0.12581(10) 0.0496(6) Uani 1 1 d . . . . .
C31 C 0.17299(13) 0.38411(9) 0.12991(10) 0.0487(6) Uani 1 1 d . . . . .
H31 H 0.132095 0.394058 0.119514 0.058 Uiso 1 1 calc R . . . .
C32 C 0.21578(12) 0.41574(9) 0.14875(9) 0.0452(6) Uani 1 1 d . . . . .
C33 C 0.21367(12) 0.46487(8) 0.15683(9) 0.0445(5) Uani 1 1 d . . . . .
C34 C 0.16616(14) 0.49781(9) 0.14822(10) 0.0521(6) Uani 1 1 d . . . . .
H34 H 0.126389 0.489052 0.134127 0.063 Uiso 1 1 calc R . . . .
C35 C 0.17799(14) 0.54264(10) 0.16042(10) 0.0552(7) Uani 1 1 d . . . . .
H35 H 0.146533 0.565217 0.154042 0.066 Uiso 1 1 calc R . . . .
C36 C 0.23613(13) 0.55546(9) 0.18222(9) 0.0471(6) Uani 1 1 d . . . . .
C37 C 0.25999(13) 0.59825(9) 0.20065(9) 0.0485(6) Uani 1 1 d . . . . .
C38 C 0.23599(15) 0.64277(9) 0.19948(10) 0.0553(7) Uani 1 1 d . . . . .
H38 H 0.195937 0.648428 0.184011 0.066 Uiso 1 1 calc R . . . .
C39 C 0.26972(17) 0.67902(9) 0.22060(10) 0.0603(8) Uani 1 1 d . . . . .
C40 C 0.32731(15) 0.66897(9) 0.24419(10) 0.0542(7) Uani 1 1 d . . . . .
H40 H 0.349957 0.693242 0.259859 0.065 Uiso 1 1 calc R . . . .
C41 C 0.60384(13) 0.60128(8) 0.37068(9) 0.0462(6) Uani 1 1 d . . . . .
C43 C 0.51999(13) 0.62908(8) 0.32285(9) 0.0460(6) Uani 1 1 d . . . . .
C44 C 0.54288(15) 0.67389(9) 0.32745(10) 0.0547(7) Uani 1 1 d . . . . .
H44 H 0.520939 0.698630 0.312034 0.066 Uiso 1 1 calc R . . . .
C45 C 0.59736(16) 0.68168(9) 0.35446(10) 0.0581(7) Uani 1 1 d . . . . .
H45 H 0.613445 0.711960 0.358288 0.070 Uiso 1 1 calc R . . . .
C46 C 0.62865(15) 0.64511(10) 0.37607(10) 0.0549(7) Uani 1 1 d . . . . .
H46 H 0.666875 0.649905 0.394491 0.066 Uiso 1 1 calc R . . . .
C47 C 0.45400(12) 0.30222(8) 0.22371(10) 0.0467(6) Uani 1 1 d . . . . .
C48 C 0.500000 0.32670(11) 0.250000 0.0436(8) Uani 1 2 d S T P . .
H48 H 0.500000 0.359328 0.249999 0.052 Uiso 1 2 calc RS T P . .
C50 C 0.45751(15) 0.25416(10) 0.22395(13) 0.0688(9) Uani 1 1 d . . . . .
H50 H 0.427655 0.237656 0.204261 0.083 Uiso 1 1 calc R . . . .
C51 C 0.32419(13) 0.39057(8) 0.33840(10) 0.0471(6) Uani 1 1 d . . . . .
C53 C 0.27017(15) 0.38947(11) 0.36957(12) 0.0630(8) Uani 1 1 d . . . . .
H53A H 0.286021 0.395437 0.401969 0.094 Uiso 1 1 calc GR . . . .
H53B H 0.250241 0.359184 0.367477 0.094 Uiso 1 1 calc GR . . . .
H53C H 0.239560 0.413079 0.359295 0.094 Uiso 1 1 calc GR . . . .
C54 C 0.30213(16) 0.38231(10) 0.28739(10) 0.0597(8) Uani 1 1 d . . . . .
H54A H 0.270083 0.404964 0.277301 0.090 Uiso 1 1 calc GR . . . .
H54B H 0.284578 0.351323 0.283792 0.090 Uiso 1 1 calc GR . . . .
H54C H 0.337511 0.385321 0.268241 0.090 Uiso 1 1 calc GR . . . .
C55 C 0.37011(13) 0.35524(9) 0.35426(10) 0.0487(6) Uani 1 1 d . . . . .
C56 C 0.40711(13) 0.32598(8) 0.36757(10) 0.0497(6) Uani 1 1 d . . . . .
C57 C 0.66676(12) 0.53383(9) 0.41408(9) 0.0466(6) Uani 1 1 d . . . . .
C58 C 0.63527(12) 0.56323(9) 0.39395(9) 0.0454(6) Uani 1 1 d . . . . .
C59 C 0.46215(13) 0.62077(8) 0.29583(9) 0.0454(6) Uani 1 1 d . . . . .
C60 C 0.41386(14) 0.61959(8) 0.27217(9) 0.0472(6) Uani 1 1 d . . . . .
C61 C 0.35382(12) 0.33884(8) 0.18010(9) 0.0437(5) Uani 1 1 d . . . . .
C62 C 0.40132(13) 0.32393(8) 0.19833(10) 0.0461(6) Uani 1 1 d . . . . .
C63 C 0.46209(18) 0.16780(11) 0.42373(17) 0.1089(18) Uani 1 1 d D . . . .
C67 C 0.86969(15) 0.49352(10) 0.50365(11) 0.0695(9) Uani 1 1 d D . . . .
C71 C 0.24438(18) 0.72799(10) 0.21661(12) 0.0723(10) Uani 1 1 d . . . . .
C72 C 0.2833(3) 0.76101(13) 0.2485(2) 0.145(3) Uani 1 1 d . . . . .
H72A H 0.285769 0.749471 0.280652 0.217 Uiso 1 1 calc GR . . . .
H72B H 0.263720 0.791415 0.247262 0.217 Uiso 1 1 calc GR . . . .
H72C H 0.325460 0.763289 0.238124 0.217 Uiso 1 1 calc GR . . . .
C73 C 0.1771(2) 0.72984(14) 0.22874(14) 0.0936(14) Uani 1 1 d . . . . .
H73A H 0.150458 0.713472 0.204833 0.140 Uiso 1 1 calc GR . . . .
H73B H 0.163579 0.761936 0.230036 0.140 Uiso 1 1 calc GR . . . .
H73C H 0.173680 0.715304 0.259165 0.140 Uiso 1 1 calc GR . . . .
C74 C 0.24573(18) 0.74396(11) 0.16585(13) 0.0740(10) Uani 1 1 d . . . . .
H74A H 0.289081 0.745749 0.157867 0.111 Uiso 1 1 calc GR . . . .
H74B H 0.226253 0.774320 0.162185 0.111 Uiso 1 1 calc GR . . . .
H74C H 0.222724 0.722011 0.145066 0.111 Uiso 1 1 calc GR . . . .
C75 C 0.13980(14) 0.30307(10) 0.10525(11) 0.0562(7) Uani 1 1 d . . . . .
C76 C 0.10906(17) 0.32066(12) 0.05823(13) 0.0711(9) Uani 1 1 d . . . . .
H76A H 0.086726 0.349342 0.063246 0.107 Uiso 1 1 calc GR . . . .
H76B H 0.079608 0.297596 0.044787 0.107 Uiso 1 1 calc GR . . . .
H76C H 0.141317 0.326235 0.036762 0.107 Uiso 1 1 calc GR . . . .
C77 C 0.08918(18) 0.29766(14) 0.13945(14) 0.0803(10) Uani 1 1 d . . . . .
H77A H 0.108608 0.288750 0.170183 0.120 Uiso 1 1 calc GR . . . .
H77B H 0.059496 0.273885 0.127954 0.120 Uiso 1 1 calc GR . . . .
H77C H 0.067138 0.326886 0.142047 0.120 Uiso 1 1 calc GR . . . .
C78 C 0.16864(17) 0.25633(11) 0.09751(13) 0.0724(9) Uani 1 1 d . . . . .
H78A H 0.204993 0.260009 0.079454 0.109 Uiso 1 1 calc GR . . . .
H78B H 0.137816 0.236531 0.080341 0.109 Uiso 1 1 calc GR . . . .
H78C H 0.181719 0.242311 0.127750 0.109 Uiso 1 1 calc GR . . . .
C64 C 0.4441(5) 0.1657(3) 0.4759(2) 0.121(4) Uani 0.5 1 d D U . A 1
H64A H 0.479725 0.175785 0.496955 0.181 Uiso 0.5 1 calc GR . . A 1
H64B H 0.433147 0.134068 0.483606 0.181 Uiso 0.5 1 calc GR . . A 1
H64C H 0.408392 0.185869 0.479529 0.181 Uiso 0.5 1 calc GR . . A 1
C65 C 0.5203(4) 0.1348(4) 0.4211(4) 0.130(6) Uani 0.5 1 d D U . A 1
H65A H 0.533048 0.134517 0.389198 0.195 Uiso 0.5 1 calc GR . . A 1
H65B H 0.508859 0.103589 0.430013 0.195 Uiso 0.5 1 calc GR . . A 1
H65C H 0.554936 0.145787 0.442555 0.195 Uiso 0.5 1 calc GR . . A 1
C66 C 0.3981(3) 0.1520(3) 0.3980(4) 0.097(3) Uani 0.5 1 d D U . A 1
H66A H 0.364573 0.172121 0.406945 0.146 Uiso 0.5 1 calc GR . . A 1
H66B H 0.389254 0.120267 0.406846 0.146 Uiso 0.5 1 calc GR . . A 1
H66C H 0.400520 0.153655 0.364143 0.146 Uiso 0.5 1 calc GR . . A 1
C68 C 0.8765(3) 0.4792(2) 0.55428(15) 0.0880(17) Uani 0.75 1 d D . . B 1
H68A H 0.847327 0.496818 0.571681 0.132 Uiso 0.75 1 calc GR . . B 1
H68B H 0.919348 0.485201 0.567354 0.132 Uiso 0.75 1 calc GR . . B 1
H68C H 0.867428 0.446371 0.556692 0.132 Uiso 0.75 1 calc GR . . B 1
C69 C 0.8861(3) 0.54257(13) 0.4936(2) 0.0834(16) Uani 0.75 1 d D . . B 1
H69A H 0.892891 0.545762 0.460464 0.125 Uiso 0.75 1 calc GR . . B 1
H69B H 0.924267 0.551150 0.512654 0.125 Uiso 0.75 1 calc GR . . B 1
H69C H 0.851869 0.562737 0.501102 0.125 Uiso 0.75 1 calc GR . . B 1
C70 C 0.9177(2) 0.46397(16) 0.4821(2) 0.0849(15) Uani 0.75 1 d D . . B 1
H70A H 0.905462 0.431620 0.483553 0.127 Uiso 0.75 1 calc GR . . B 1
H70B H 0.958560 0.468225 0.499468 0.127 Uiso 0.75 1 calc GR . . B 1
H70C H 0.920260 0.472976 0.449516 0.127 Uiso 0.75 1 calc GR . . B 1
C164 C 0.3907(3) 0.1630(4) 0.4319(5) 0.138(5) Uani 0.5 1 d D U . A 2
H16A H 0.383738 0.174219 0.463149 0.207 Uiso 0.5 1 calc GR . . A 2
H16B H 0.378375 0.130673 0.429080 0.207 Uiso 0.5 1 calc GR . . A 2
H16C H 0.365802 0.181191 0.408451 0.207 Uiso 0.5 1 calc GR . . A 2
C165 C 0.5149(4) 0.1351(3) 0.4459(4) 0.078(3) Uani 0.5 1 d D U . A 2
H16D H 0.553879 0.141232 0.431711 0.116 Uiso 0.5 1 calc GR . . A 2
H16E H 0.502578 0.103035 0.440322 0.116 Uiso 0.5 1 calc GR . . A 2
H16F H 0.521046 0.140681 0.479635 0.116 Uiso 0.5 1 calc GR . . A 2
C166 C 0.4538(7) 0.1476(3) 0.3725(2) 0.175(6) Uani 0.5 1 d D U . A 2
H16G H 0.429309 0.169050 0.352114 0.262 Uiso 0.5 1 calc GR . . A 2
H16H H 0.432108 0.118026 0.372889 0.262 Uiso 0.5 1 calc GR . . A 2
H16I H 0.494932 0.143209 0.360859 0.262 Uiso 0.5 1 calc GR . . A 2
C168 C 0.9063(5) 0.4615(3) 0.5369(4) 0.047(3) Uani 0.25 1 d D . . B 2
H16J H 0.879719 0.451160 0.560929 0.071 Uiso 0.25 1 calc GR . . B 2
H16K H 0.942672 0.477715 0.551711 0.071 Uiso 0.25 1 calc GR . . B 2
H16L H 0.920172 0.434899 0.519679 0.071 Uiso 0.25 1 calc GR . . B 2
C169 C 0.8573(6) 0.5326(3) 0.5362(4) 0.083(4) Uani 0.25 1 d D U . B 2
H16M H 0.839979 0.558794 0.518001 0.124 Uiso 0.25 1 calc GR . . B 2
H16N H 0.896464 0.541804 0.553647 0.124 Uiso 0.25 1 calc GR . . B 2
H16O H 0.827462 0.522658 0.558106 0.124 Uiso 0.25 1 calc GR . . B 2
C170 C 0.9092(4) 0.5194(3) 0.4715(3) 0.040(2) Uani 0.25 1 d D . . B 2
H17A H 0.883839 0.543097 0.454709 0.060 Uiso 0.25 1 calc GR . . B 2
H17B H 0.925207 0.498076 0.448993 0.060 Uiso 0.25 1 calc GR . . B 2
H17C H 0.944310 0.533995 0.489852 0.060 Uiso 0.25 1 calc GR . . B 2
N84 N 0.33072(11) 0.57209(7) 0.40176(8) 0.0480(5) Uani 1 1 d . . . . .
C85 C 0.27692(14) 0.60117(10) 0.41541(10) 0.0529(6) Uani 1 1 d . . . . .
H85A H 0.242270 0.580422 0.422017 0.064 Uiso 1 1 calc R . . . .
H85B H 0.290416 0.617385 0.444806 0.064 Uiso 1 1 calc R . . . .
C86 C 0.25192(16) 0.63643(10) 0.38005(11) 0.0593(7) Uani 1 1 d . . . . .
H86A H 0.285749 0.657877 0.373336 0.071 Uiso 1 1 calc R . . . .
H86B H 0.237202 0.620805 0.350571 0.071 Uiso 1 1 calc R . . . .
C87 C 0.19895(19) 0.66294(13) 0.39805(13) 0.0781(10) Uani 1 1 d . . . . .
H87A H 0.167031 0.641024 0.407303 0.094 Uiso 1 1 calc R . . . .
H87B H 0.214789 0.680175 0.426280 0.094 Uiso 1 1 calc R . . . .
C88 C 0.16891(19) 0.69593(12) 0.36314(13) 0.0781(10) Uani 1 1 d . . . . .
H88A H 0.143198 0.678931 0.339197 0.117 Uiso 1 1 calc GR . . . .
H88B H 0.201275 0.713044 0.348447 0.117 Uiso 1 1 calc GR . . . .
H88C H 0.142591 0.717421 0.378895 0.117 Uiso 1 1 calc GR . . . .
C89 C 0.38816(13) 0.60127(8) 0.39738(9) 0.0488(6) Uani 1 1 d . . . . .
H89A H 0.378980 0.623221 0.371413 0.059 Uiso 1 1 calc R . . . .
H89B H 0.422226 0.580976 0.388632 0.059 Uiso 1 1 calc R . . . .
C90 C 0.41174(14) 0.62824(9) 0.44040(10) 0.0516(6) Uani 1 1 d . . . . .
H90A H 0.423343 0.606873 0.466479 0.062 Uiso 1 1 calc R . . . .
H90B H 0.378381 0.648786 0.449915 0.062 Uiso 1 1 calc R . . . .
C91 C 0.46853(15) 0.65669(10) 0.42971(11) 0.0567(7) Uani 1 1 d . . . . .
H91A H 0.502677 0.635636 0.422735 0.068 Uiso 1 1 calc R . . . .
H91B H 0.457556 0.675429 0.401476 0.068 Uiso 1 1 calc R . . . .
C92 C 0.49177(16) 0.68823(10) 0.46942(11) 0.0632(8) Uani 1 1 d . . . . .
H92A H 0.528679 0.704938 0.460828 0.095 Uiso 1 1 calc GR . . . .
H92B H 0.502759 0.669952 0.497536 0.095 Uiso 1 1 calc GR . . . .
H92C H 0.458904 0.710192 0.475553 0.095 Uiso 1 1 calc GR . . . .
C93 C 0.34301(14) 0.53645(9) 0.44056(10) 0.0500(6) Uani 1 1 d . . . . .
H93A H 0.348900 0.552899 0.470741 0.060 Uiso 1 1 calc R . . . .
H93B H 0.305274 0.517092 0.441413 0.060 Uiso 1 1 calc R . . . .
C94 C 0.39871(14) 0.50504(9) 0.43667(10) 0.0510(6) Uani 1 1 d . . . . .
H94A H 0.393770 0.487923 0.406830 0.061 Uiso 1 1 calc R . . . .
H94B H 0.437400 0.523517 0.437103 0.061 Uiso 1 1 calc R . . . .
C95 C 0.40331(15) 0.47154(9) 0.47733(11) 0.0566(7) Uani 1 1 d . . . . .
H95A H 0.363625 0.454307 0.477412 0.068 Uiso 1 1 calc R . . . .
H95B H 0.409199 0.488999 0.506918 0.068 Uiso 1 1 calc R . . . .
C96 C 0.45691(18) 0.43760(11) 0.47508(12) 0.0691(9) Uani 1 1 d . . . . .
H96A H 0.450644 0.419515 0.446319 0.104 Uiso 1 1 calc GR . . . .
H96B H 0.458159 0.417010 0.502113 0.104 Uiso 1 1 calc GR . . . .
H96C H 0.496397 0.454437 0.475370 0.104 Uiso 1 1 calc GR . . . .
C97 C 0.31494(14) 0.54916(9) 0.35488(9) 0.0502(6) Uani 1 1 d . . . . .
H97A H 0.313546 0.573077 0.330344 0.060 Uiso 1 1 calc R . . . .
H97B H 0.349189 0.527755 0.349006 0.060 Uiso 1 1 calc R . . . .
C98 C 0.25417(14) 0.52286(9) 0.34990(10) 0.0514(6) Uani 1 1 d . . . . .
H98A H 0.220438 0.541853 0.361329 0.062 Uiso 1 1 calc R . . . .
H98B H 0.258074 0.494515 0.368951 0.062 Uiso 1 1 calc R . . . .
C99 C 0.23788(14) 0.51039(10) 0.29852(10) 0.0553(7) Uani 1 1 d . . . . .
H99A H 0.237395 0.538771 0.279532 0.066 Uiso 1 1 calc R . . . .
H99B H 0.270820 0.490054 0.287996 0.066 Uiso 1 1 calc R . . . .
C100 C 0.17476(16) 0.48634(12) 0.28990(12) 0.0673(8) Uani 1 1 d . . . . .
H10A H 0.166577 0.479662 0.256539 0.101 Uiso 1 1 calc GR . . . .
H10B H 0.141826 0.506360 0.300004 0.101 Uiso 1 1 calc GR . . . .
H10C H 0.175415 0.457569 0.307635 0.101 Uiso 1 1 calc GR . . . .


_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
P79 O80 1.5843(18) . ?
P79 O81 1.4929(18) . ?
P79 O82 1.523(2) . ?
P79 O83 1.5736(18) . ?
O52 C51 1.423(3) . ?
N3 C2 1.375(3) . ?
N3 C4 1.379(3) . ?
N6 C5 1.377(3) . ?
N6 C7 1.380(3) . ?
N23 C22 1.383(3) . ?
N23 C24 1.393(3) . ?
N26 C25 1.382(3) . ?
N26 C27 1.385(3) . ?
N42 C41 1.349(3) . ?
N42 C43 1.352(3) . ?
N49 C50 1.329(3) . ?
N49 C50 1.329(3) 2_655 ?
C1 C2 1.391(4) . ?
C1 C20 1.400(4) . ?
C1 C56 1.430(4) . ?
C2 C17 1.410(4) . ?
C4 C5 1.387(4) . ?
C4 C16 1.409(3) . ?
C5 C13 1.403(4) . ?
C7 C8 1.405(4) . ?
C7 C12 1.410(3) . ?
C8 C9 1.399(4) . ?
C8 C57 1.430(4) . ?
C9 C10 1.404(4) . ?
C10 C11 1.396(4) . ?
C10 C67 1.514(4) . ?
C11 C12 1.390(4) . ?
C12 C13 1.441(4) . ?
C13 C14 1.424(4) . ?
C14 C15 1.372(4) . ?
C15 C16 1.409(4) . ?
C16 C17 1.454(4) . ?
C17 C18 1.401(4) . ?
C18 C19 1.381(5) . ?
C19 C20 1.395(4) . ?
C19 C63 1.516(4) . ?
C21 C22 1.398(4) . ?
C21 C40 1.417(3) . ?
C21 C60 1.444(4) . ?
C22 C37 1.414(4) . ?
C24 C25 1.404(3) . ?
C24 C36 1.405(3) . ?
C25 C33 1.402(4) . ?
C27 C28 1.404(3) . ?
C27 C32 1.408(4) . ?
C28 C29 1.403(3) . ?
C28 C61 1.433(4) . ?
C29 C30 1.389(4) . ?
C30 C31 1.389(4) . ?
C30 C75 1.542(4) . ?
C31 C32 1.380(4) . ?
C32 C33 1.451(3) . ?
C33 C34 1.408(4) . ?
C34 C35 1.370(4) . ?
C35 C36 1.401(4) . ?
C36 C37 1.432(4) . ?
C37 C38 1.394(4) . ?
C38 C39 1.391(4) . ?
C39 C40 1.392(4) . ?
C39 C71 1.527(4) . ?
C41 C46 1.387(4) . ?
C41 C58 1.434(4) . ?
C43 C44 1.397(3) . ?
C43 C59 1.431(4) . ?
C44 C45 1.369(4) . ?
C45 C46 1.379(4) . ?
C47 C48 1.390(3) . ?
C47 C50 1.401(4) . ?
C47 C62 1.441(4) . ?
C51 C53 1.526(4) . ?
C51 C54 1.522(4) . ?
C51 C55 1.471(4) . ?
C55 C56 1.206(4) . ?
C57 C58 1.208(4) . ?
C59 C60 1.193(4) . ?
C61 C62 1.190(4) . ?
C63 C64 1.582(3) . ?
C63 C65 1.5850(18) . ?
C63 C66 1.577(3) . ?
C63 C164 1.578(3) . ?
C63 C165 1.575(3) . ?
C63 C166 1.581(3) . ?
C67 C68 1.509(3) . ?
C67 C69 1.505(3) . ?
C67 C70 1.516(3) . ?
C67 C168 1.508(3) . ?
C67 C169 1.512(3) . ?
C67 C170 1.510(3) . ?
C71 C72 1.529(5) . ?
C71 C73 1.518(6) . ?
C71 C74 1.534(5) . ?
C75 C76 1.542(4) . ?
C75 C77 1.535(5) . ?
C75 C78 1.520(4) . ?
N84 C85 1.512(3) . ?
N84 C89 1.513(4) . ?
N84 C93 1.530(3) . ?
N84 C97 1.517(3) . ?
C85 C86 1.511(4) . ?
C86 C87 1.503(5) . ?
C87 C88 1.496(4) . ?
C89 C90 1.516(4) . ?
C90 C91 1.528(4) . ?
C91 C92 1.517(4) . ?
C93 C94 1.519(4) . ?
C94 C95 1.519(4) . ?
C95 C96 1.524(4) . ?
C97 C98 1.511(4) . ?
C98 C99 1.533(4) . ?
C99 C100 1.529(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O81 P79 O80 107.44(10) . . ?
O81 P79 O82 115.66(11) . . ?
O81 P79 O83 110.80(11) . . ?
O82 P79 O80 109.74(10) . . ?
O82 P79 O83 110.14(10) . . ?
O83 P79 O80 102.16(10) . . ?
C2 N3 C4 107.8(2) . . ?
C5 N6 C7 108.1(2) . . ?
C22 N23 C24 107.8(2) . . ?
C25 N26 C27 107.5(2) . . ?
C41 N42 C43 118.3(2) . . ?
C50 N49 C50 116.8(3) . 2_655 ?
C2 C1 C20 116.8(3) . . ?
C2 C1 C56 120.5(2) . . ?
C20 C1 C56 122.6(3) . . ?
N3 C2 C1 128.8(2) . . ?
N3 C2 C17 109.7(2) . . ?
C1 C2 C17 121.3(2) . . ?
N3 C4 C5 128.9(2) . . ?
N3 C4 C16 110.7(2) . . ?
C5 C4 C16 120.4(2) . . ?
N6 C5 C4 131.0(2) . . ?
N6 C5 C13 109.8(2) . . ?
C4 C5 C13 119.2(2) . . ?
N6 C7 C8 128.8(2) . . ?
N6 C7 C12 109.4(2) . . ?
C8 C7 C12 121.8(2) . . ?
C7 C8 C57 122.5(2) . . ?
C9 C8 C7 116.8(2) . . ?
C9 C8 C57 120.7(2) . . ?
C8 C9 C10 123.1(3) . . ?
C9 C10 C67 122.5(3) . . ?
C11 C10 C9 118.0(3) . . ?
C11 C10 C67 119.5(3) . . ?
C12 C11 C10 121.4(3) . . ?
C7 C12 C13 106.3(2) . . ?
C11 C12 C7 119.0(2) . . ?
C11 C12 C13 134.7(2) . . ?
C5 C13 C12 106.4(2) . . ?
C5 C13 C14 120.6(2) . . ?
C14 C13 C12 133.0(2) . . ?
C15 C14 C13 119.5(2) . . ?
C14 C15 C16 120.3(2) . . ?
C4 C16 C15 119.9(2) . . ?
C4 C16 C17 105.0(2) . . ?
C15 C16 C17 135.0(2) . . ?
C2 C17 C16 106.7(2) . . ?
C18 C17 C2 119.7(3) . . ?
C18 C17 C16 133.5(3) . . ?
C19 C18 C17 120.1(3) . . ?
C18 C19 C20 118.8(3) . . ?
C18 C19 C63 121.5(3) . . ?
C20 C19 C63 119.5(3) . . ?
C19 C20 C1 123.2(3) . . ?
C22 C21 C40 117.5(2) . . ?
C22 C21 C60 125.9(2) . . ?
C40 C21 C60 116.6(2) . . ?
N23 C22 C21 130.9(2) . . ?
N23 C22 C37 109.3(2) . . ?
C21 C22 C37 119.7(2) . . ?
N23 C24 C25 131.3(2) . . ?
N23 C24 C36 109.5(2) . . ?
C25 C24 C36 119.2(2) . . ?
N26 C25 C24 130.7(2) . . ?
N26 C25 C33 110.3(2) . . ?
C33 C25 C24 119.0(2) . . ?
N26 C27 C28 129.6(2) . . ?
N26 C27 C32 109.9(2) . . ?
C28 C27 C32 120.5(2) . . ?
C27 C28 C61 122.3(2) . . ?
C29 C28 C27 116.7(2) . . ?
C29 C28 C61 120.9(2) . . ?
C30 C29 C28 123.8(2) . . ?
C29 C30 C75 121.8(2) . . ?
C31 C30 C29 117.5(2) . . ?
C31 C30 C75 120.7(3) . . ?
C32 C31 C30 121.4(3) . . ?
C27 C32 C33 106.2(2) . . ?
C31 C32 C27 120.0(2) . . ?
C31 C32 C33 133.8(2) . . ?
C25 C33 C32 106.1(2) . . ?
C25 C33 C34 121.4(2) . . ?
C34 C33 C32 132.5(2) . . ?
C35 C34 C33 119.2(3) . . ?
C34 C35 C36 120.5(3) . . ?
C24 C36 C37 106.7(2) . . ?
C35 C36 C24 120.7(2) . . ?
C35 C36 C37 132.5(2) . . ?
C22 C37 C36 106.7(2) . . ?
C38 C37 C22 120.4(3) . . ?
C38 C37 C36 132.8(3) . . ?
C39 C38 C37 121.1(3) . . ?
C38 C39 C40 117.6(2) . . ?
C38 C39 C71 120.4(3) . . ?
C40 C39 C71 122.0(3) . . ?
C39 C40 C21 123.4(3) . . ?
N42 C41 C46 121.9(2) . . ?
N42 C41 C58 118.3(2) . . ?
C46 C41 C58 119.8(2) . . ?
N42 C43 C44 121.9(3) . . ?
N42 C43 C59 118.5(2) . . ?
C44 C43 C59 119.5(2) . . ?
C45 C44 C43 119.1(3) . . ?
C44 C45 C46 119.3(3) . . ?
C45 C46 C41 119.4(3) . . ?
C48 C47 C50 118.3(2) . . ?
C48 C47 C62 122.9(2) . . ?
C50 C47 C62 118.7(2) . . ?
C47 C48 C47 118.3(3) . 2_655 ?
N49 C50 C47 124.1(3) . . ?
O52 C51 C53 105.6(2) . . ?
O52 C51 C54 109.7(2) . . ?
O52 C51 C55 111.0(2) . . ?
C54 C51 C53 111.8(3) . . ?
C55 C51 C53 109.1(2) . . ?
C55 C51 C54 109.6(2) . . ?
C56 C55 C51 179.1(3) . . ?
C55 C56 C1 174.9(3) . . ?
C58 C57 C8 177.6(3) . . ?
C57 C58 C41 173.7(3) . . ?
C60 C59 C43 171.8(3) . . ?
C59 C60 C21 172.1(3) . . ?
C62 C61 C28 175.2(3) . . ?
C61 C62 C47 172.8(3) . . ?
C19 C63 C64 106.6(4) . . ?
C19 C63 C65 109.0(5) . . ?
C19 C63 C66 116.6(4) . . ?
C19 C63 C164 113.6(5) . . ?
C19 C63 C165 115.4(5) . . ?
C19 C63 C166 102.1(4) . . ?
C64 C63 C65 106.1(6) . . ?
C66 C63 C64 99.2(6) . . ?
C66 C63 C65 117.5(7) . . ?
C164 C63 C166 94.1(7) . . ?
C165 C63 C164 124.3(6) . . ?
C165 C63 C166 100.0(6) . . ?
C10 C67 C70 107.7(3) . . ?
C68 C67 C10 110.4(3) . . ?
C68 C67 C70 102.8(4) . . ?
C69 C67 C10 112.5(3) . . ?
C69 C67 C68 116.2(4) . . ?
C69 C67 C70 106.3(4) . . ?
C168 C67 C10 120.9(5) . . ?
C168 C67 C169 100.5(7) . . ?
C168 C67 C170 114.0(6) . . ?
C169 C67 C10 104.8(5) . . ?
C170 C67 C10 113.9(4) . . ?
C170 C67 C169 98.1(7) . . ?
C39 C71 C72 111.6(3) . . ?
C39 C71 C74 108.6(3) . . ?
C72 C71 C74 109.1(4) . . ?
C73 C71 C39 110.9(3) . . ?
C73 C71 C72 108.9(4) . . ?
C73 C71 C74 107.6(3) . . ?
C76 C75 C30 110.1(2) . . ?
C77 C75 C30 108.5(3) . . ?
C77 C75 C76 108.7(3) . . ?
C78 C75 C30 112.1(2) . . ?
C78 C75 C76 108.6(3) . . ?
C78 C75 C77 108.8(3) . . ?
C85 N84 C89 110.8(2) . . ?
C85 N84 C93 106.2(2) . . ?
C85 N84 C97 111.0(2) . . ?
C89 N84 C93 110.4(2) . . ?
C89 N84 C97 107.2(2) . . ?
C97 N84 C93 111.18(19) . . ?
C86 C85 N84 116.3(2) . . ?
C87 C86 C85 110.7(3) . . ?
C88 C87 C86 113.3(3) . . ?
N84 C89 C90 116.3(2) . . ?
C89 C90 C91 109.6(2) . . ?
C92 C91 C90 113.3(3) . . ?
C94 C93 N84 116.3(2) . . ?
C95 C94 C93 109.3(2) . . ?
C94 C95 C96 112.6(3) . . ?
C98 C97 N84 115.7(2) . . ?
C97 C98 C99 109.7(2) . . ?
C100 C99 C98 113.1(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.809 0.250 -0.559 2188.2 405.5 ?
2 -0.211 0.750 -0.461 2188.2 405.5 ?

_olex2_submission_special_instructions 'No special instructions were received'
