 
data_Anth26pdc
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C71 H66 N10 O17' 
_chemical_formula_weight          1331.33

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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'
 
_cell_length_a                    8.9684(14)
_cell_length_b                    14.022(2)
_cell_length_c                    26.653(4)
_cell_angle_alpha                 101.059(5)
_cell_angle_beta                  94.792(5)
_cell_angle_gamma                 95.101(5)
_cell_volume                      3259.2(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used      9822
_cell_measurement_theta_min        2.29
_cell_measurement_theta_max       20.32
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.357          
_exptl_crystal_F_000              1396
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.26
_exptl_crystal_size_min           0.22
_exptl_absorpt_coefficient_mu     0.099
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type   'none'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details   'none'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\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             134264
_diffrn_reflns_av_unetI/netI      0.0472
_diffrn_reflns_av_R_equivalents   0.1049
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          0.783
_diffrn_reflns_theta_max          25.048
_diffrn_reflns_theta_full         25.048
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              11550
_reflns_number_gt                 7298
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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       '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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.1000P)²+0.2310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          11550
_refine_ls_number_parameters      905
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.1119
_refine_ls_R_factor_gt            0.0659
_refine_ls_wR_factor_ref          0.2174
_refine_ls_wR_factor_gt           0.1769
_refine_ls_goodness_of_fit_ref    1.258
_refine_ls_restrained_S_all       6.499
_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
O8 O 1.2304(2) 0.24815(16) 0.87149(8) 0.0551(6) Uani 1 1 d . . . . .
O7 O 0.9848(2) 0.20281(17) 0.86149(8) 0.0562(6) Uani 1 1 d . . . . .
O15 O 0.0543(2) 0.17394(18) -0.05229(8) 0.0571(6) Uani 1 1 d D . . . .
O2 O 0.4712(2) 0.20914(16) 0.58702(8) 0.0544(6) Uani 1 1 d . . . . .
O3 O 0.0650(2) 0.16987(17) 0.46339(8) 0.0558(6) Uani 1 1 d . . . . .
O10 O 0.9896(2) 0.18052(19) 0.37398(8) 0.0621(6) Uani 1 1 d D . . . .
O13 O 0.4599(2) 0.19199(17) 0.07083(9) 0.0591(6) Uani 1 1 d . . . . .
N3 N 0.3616(2) 0.26072(15) 0.97697(8) 0.0366(5) Uani 1 1 d . . . . .
H3N' H 0.3280 0.2365 1.0029 0.044 Uiso 1 1 calc R U . . .
H3N H 0.2829 0.2625 0.9546 0.044 Uiso 1 1 calc R U . . .
O9 O 1.2300(2) 0.23617(17) 0.37850(9) 0.0630(6) Uani 1 1 d . . . . .
N4 N 0.1729(2) 0.16528(16) 0.55949(9) 0.0399(6) Uani 1 1 d . . . . .
N10 N 0.1594(2) 0.15896(16) 0.04167(9) 0.0400(6) Uani 1 1 d . . . . .
O14 O 0.4166(3) 0.19702(19) 0.15255(9) 0.0670(7) Uani 1 1 d D . . . .
N8 N 0.3694(2) 0.26343(15) 0.49350(9) 0.0403(6) Uani 1 1 d D . . . .
H8N' H 0.3452 0.2432 0.5217 0.048 Uiso 1 1 calc R U . . .
H8N H 0.2850 0.2619 0.4732 0.048 Uiso 1 1 calc R U . . .
N2 N 0.5349(3) 0.08130(17) 0.85188(9) 0.0429(6) Uani 1 1 d . . . . .
N9 N 0.9330(3) 0.22338(17) 0.28098(9) 0.0431(6) Uani 1 1 d . . . . .
O11 O 0.7064(3) 0.12647(19) 0.20848(9) 0.0710(7) Uani 1 1 d . . . . .
O16 O -0.1736(2) 0.1091(2) -0.04357(9) 0.0724(7) Uani 1 1 d . . . . .
N5 N 0.9551(3) 0.26618(19) 0.77196(9) 0.0486(6) Uani 1 1 d . . . . .
N7 N 0.5357(3) 0.05903(18) 0.37296(10) 0.0475(6) Uani 1 1 d . . . . .
O4 O -0.1615(3) 0.1047(2) 0.47457(9) 0.0774(8) Uani 1 1 d . . . . .
O12 O 0.6799(3) 0.26769(19) 0.18454(10) 0.0818(8) Uani 1 1 d . . . . .
O1 O 0.4410(3) 0.1959(2) 0.66751(9) 0.0856(8) Uani 1 1 d . . . . .
N1 N 0.6729(3) 0.1551(2) 0.80598(11) 0.0555(7) Uani 1 1 d . . . . .
N6 N 0.6740(3) 0.1162(2) 0.32120(11) 0.0578(7) Uani 1 1 d . . . . .
O5 O 0.7087(3) 0.2206(3) 0.70264(11) 0.1010(11) Uani 1 1 d . . . . .
H5O H 0.6273 0.2197 0.6860 0.151 Uiso 1 1 calc R U . . .
C6 C 0.4682(3) 0.19621(19) 0.95147(11) 0.0393(7) Uani 1 1 d . . . . .
H6B H 0.5506 0.1913 0.9765 0.047 Uiso 1 1 calc R U . . .
H6A H 0.5099 0.2252 0.9248 0.047 Uiso 1 1 calc R U . . .
C44 C 0.3485(3) 0.4435(2) 0.52988(12) 0.0430(7) Uani 1 1 d . . . . .
C35 C 1.1056(3) 0.2398(2) 0.84752(11) 0.0434(7) Uani 1 1 d . . . . .
C8 C 0.3396(3) 0.4372(2) 1.01981(12) 0.0428(7) Uani 1 1 d . . . . .
C42 C 0.4700(3) 0.19662(19) 0.46653(11) 0.0422(7) Uani 1 1 d . . . . .
H42A H 0.5592 0.1953 0.4895 0.051 Uiso 1 1 calc R U . . .
H42B H 0.5016 0.2212 0.4370 0.051 Uiso 1 1 calc R U . . .
C41 C 0.3925(3) 0.09401(19) 0.44878(12) 0.0441(7) Uani 1 1 d . . . . .
H41A H 0.3009 0.0958 0.4271 0.053 Uiso 1 1 calc R U . . .
H41B H 0.3648 0.0685 0.4784 0.053 Uiso 1 1 calc R U . . .
C66 C 0.2106(3) 0.1552(2) 0.08993(11) 0.0444(7) Uani 1 1 d . . . . .
C70 C 0.0135(3) 0.1329(2) 0.02711(11) 0.0437(7) Uani 1 1 d . . . . .
C45 C 0.3638(3) 0.4815(2) 0.58366(12) 0.0466(7) Uani 1 1 d . . . . .
C57 C 0.2576(3) 0.4865(2) 0.49639(12) 0.0459(7) Uani 1 1 d . . . . .
C5 C 0.3921(3) 0.0950(2) 0.92806(11) 0.0437(7) Uani 1 1 d . . . . .
H5B H 0.3665 0.0616 0.9554 0.052 Uiso 1 1 calc R U . . .
H5A H 0.2994 0.1005 0.9079 0.052 Uiso 1 1 calc DR U . . .
C21 C 0.2551(3) 0.4866(2) 0.98785(12) 0.0459(7) Uani 1 1 d . . . . .
C7 C 0.4372(3) 0.3619(2) 0.99666(11) 0.0440(7) Uani 1 1 d . . . . .
H7A H 0.4818 0.3844 0.9685 0.053 Uiso 1 1 calc R U . . .
H7B H 0.5187 0.3589 1.0224 0.053 Uiso 1 1 calc R U . . .
C22 C 0.3936(4) 0.1934(2) 0.62115(12) 0.0505(8) Uani 1 1 d . . . . .
C4 C 0.4908(3) 0.0347(2) 0.89416(11) 0.0446(7) Uani 1 1 d . . . . .
H4A H 0.5806 0.0255 0.9148 0.054 Uiso 1 1 calc R U . . .
H4B H 0.4371 -0.0292 0.8800 0.054 Uiso 1 1 calc R U . . .
C23 C 0.2266(3) 0.1639(2) 0.60761(11) 0.0455(7) Uani 1 1 d . . . . .
C43 C 0.4441(3) 0.36603(19) 0.50790(12) 0.0438(7) Uani 1 1 d . . . . .
H43A H 0.4825 0.3834 0.4775 0.053 Uiso 1 1 calc R U . . .
H43B H 0.5299 0.3674 0.5328 0.053 Uiso 1 1 calc R U . . .
C27 C 0.0269(3) 0.1376(2) 0.54525(11) 0.0455(7) Uani 1 1 d . . . . .
C28 C -0.0315(3) 0.1360(2) 0.49028(12) 0.0485(8) Uani 1 1 d . . . . .
C71 C -0.0440(3) 0.1373(2) -0.02700(11) 0.0450(7) Uani 1 1 d . . . . .
C34 C 1.0906(3) 0.2788(2) 0.79877(11) 0.0455(7) Uani 1 1 d . . . . .
C59 C 1.0670(3) 0.2548(2) 0.30716(11) 0.0455(7) Uani 1 1 d . . . . .
C9 C 0.3456(3) 0.4670(2) 1.07399(12) 0.0476(8) Uani 1 1 d . . . . .
C65 C 0.3761(4) 0.1833(2) 0.10341(12) 0.0502(8) Uani 1 1 d . . . . .
C58 C 1.1021(3) 0.2212(2) 0.35714(12) 0.0466(7) Uani 1 1 d . . . . .
C64 C 0.7477(4) 0.2129(3) 0.20845(11) 0.0526(8) Uani 1 1 d . . . . .
C1 C 0.6737(3) 0.1154(2) 0.84722(12) 0.0514(8) Uani 1 1 d . . . . .
H1 H 0.7583 0.1121 0.8693 0.062 Uiso 1 1 calc R U . . .
C52 C 0.1804(3) 0.5687(2) 0.51677(14) 0.0529(8) Uani 1 1 d . . . . .
C63 C 0.8969(4) 0.2561(2) 0.23776(11) 0.0511(8) Uani 1 1 d . . . . .
C16 C 0.1741(3) 0.5656(2) 1.01013(14) 0.0535(8) Uani 1 1 d . . . . .
C40 C 0.4920(3) 0.0261(2) 0.41915(12) 0.0526(8) Uani 1 1 d . . . . .
H40A H 0.5819 0.0225 0.4413 0.063 Uiso 1 1 calc R U . . .
H40B H 0.4387 -0.0390 0.4093 0.063 Uiso 1 1 calc R U . . .
C3 C 0.4413(3) 0.1014(3) 0.81271(12) 0.0552(8) Uani 1 1 d . . . . .
H3 H 0.3374 0.0863 0.8071 0.066 Uiso 1 1 calc R U . . .
C46 C 0.4585(4) 0.4466(2) 0.62012(13) 0.0566(9) Uani 1 1 d . . . . .
H46 H 0.5110 0.3934 0.6090 0.068 Uiso 1 1 calc R U . . .
C50 C 0.2851(4) 0.5635(2) 0.60301(13) 0.0539(8) Uani 1 1 d . . . . .
C37 C 0.6731(3) 0.0931(2) 0.36677(13) 0.0547(8) Uani 1 1 d . . . . .
H37 H 0.7565 0.0998 0.3908 0.066 Uiso 1 1 calc R U . . .
C56 C 0.2435(4) 0.4563(2) 0.44171(13) 0.0580(9) Uani 1 1 d . . . . .
H56 H 0.2902 0.4027 0.4270 0.070 Uiso 1 1 calc R U . . .
C2 C 0.5288(4) 0.1470(3) 0.78408(13) 0.0593(9) Uani 1 1 d . . . . .
H2 H 0.4967 0.1690 0.7546 0.071 Uiso 1 1 calc R U . . .
C20 C 0.2488(4) 0.4651(2) 0.93301(13) 0.0592(9) Uani 1 1 d . . . . .
H20 H 0.2988 0.4143 0.9169 0.071 Uiso 1 1 calc R U . . .
C14 C 0.2642(4) 0.5458(2) 1.09529(13) 0.0564(9) Uani 1 1 d . . . . .
C10 C 0.4338(4) 0.4245(2) 1.10956(14) 0.0619(9) Uani 1 1 d . . . . .
H10 H 0.4878 0.3729 1.0972 0.074 Uiso 1 1 calc R U . . .
C15 C 0.1821(4) 0.5926(2) 1.06262(15) 0.0600(9) Uani 1 1 d . . . . .
H15 H 0.1306 0.6442 1.0769 0.072 Uiso 1 1 calc R U . . .
C51 C 0.1968(4) 0.6036(2) 0.56914(15) 0.0609(9) Uani 1 1 d . . . . .
H51 H 0.1461 0.6564 0.5823 0.073 Uiso 1 1 calc R U . . .
C69 C -0.0857(4) 0.1030(3) 0.05949(13) 0.0625(9) Uani 1 1 d . . . . .
H69 H -0.1873 0.0862 0.0482 0.075 Uiso 1 1 calc R U . . .
C67 C 0.1172(4) 0.1255(3) 0.12412(12) 0.0612(9) Uani 1 1 d . . . . .
H67 H 0.1559 0.1240 0.1574 0.073 Uiso 1 1 calc R U . . .
C30 C 0.9410(4) 0.3091(3) 0.73082(13) 0.0619(9) Uani 1 1 d . . . . .
C26 C -0.0701(4) 0.1089(3) 0.57827(13) 0.0707(11) Uani 1 1 d . . . . .
H26 H -0.1716 0.0905 0.5674 0.085 Uiso 1 1 calc R U . . .
C24 C 0.1358(4) 0.1342(3) 0.64258(13) 0.0710(11) Uani 1 1 d . . . . .
H24 H 0.1759 0.1322 0.6756 0.085 Uiso 1 1 calc R U . . .
C53 C 0.0950(4) 0.6146(3) 0.48257(18) 0.0713(11) Uani 1 1 d . . . . .
H53 H 0.0433 0.6668 0.4958 0.086 Uiso 1 1 calc R U . . .
C68 C -0.0314(4) 0.0985(3) 0.10873(14) 0.0726(11) Uani 1 1 d . . . . .
H68 H -0.0953 0.0774 0.1311 0.087 Uiso 1 1 calc R U . . .
C17 C 0.0922(4) 0.6162(3) 0.97723(18) 0.0707(11) Uani 1 1 d . . . . .
H17 H 0.0381 0.6663 0.9917 0.085 Uiso 1 1 calc R U . . .
O6 O 0.7560(4) 0.3618(3) 0.67847(16) 0.1508(16) Uani 1 1 d . . . . .
C47 C 0.4742(4) 0.4893(3) 0.67111(14) 0.0712(10) Uani 1 1 d . . . . .
H47 H 0.5384 0.4655 0.6939 0.085 Uiso 1 1 calc R U . . .
C39 C 0.4454(4) 0.0610(3) 0.32935(14) 0.0752(11) Uani 1 1 d . . . . .
H39 H 0.3426 0.0413 0.3230 0.090 Uiso 1 1 calc R U . . .
C55 C 0.1638(4) 0.5037(3) 0.41110(15) 0.0738(11) Uani 1 1 d . . . . .
H55 H 0.1587 0.4832 0.3756 0.089 Uiso 1 1 calc R U . . .
C33 C 1.2140(4) 0.3281(3) 0.78470(14) 0.0700(10) Uani 1 1 d . . . . .
H33 H 1.3073 0.3327 0.8035 0.084 Uiso 1 1 calc R U . . .
C19 C 0.1711(5) 0.5177(3) 0.90406(16) 0.0758(11) Uani 1 1 d . . . . .
H19 H 0.1709 0.5028 0.8685 0.091 Uiso 1 1 calc R U . . .
C49 C 0.3043(5) 0.6039(3) 0.65691(15) 0.0758(11) Uani 1 1 d . . . . .
H49 H 0.2521 0.6562 0.6696 0.091 Uiso 1 1 calc R U . . .
C38 C 0.5331(4) 0.0968(3) 0.29726(14) 0.0760(11) Uani 1 1 d . . . . .
H38 H 0.5021 0.1065 0.2646 0.091 Uiso 1 1 calc R U . . .
C60 C 1.1723(4) 0.3168(3) 0.29123(14) 0.0768(11) Uani 1 1 d . . . . .
H60 H 1.2669 0.3344 0.3094 0.092 Uiso 1 1 calc R U . . .
C29 C 0.7909(5) 0.2999(4) 0.70192(15) 0.0829(12) Uani 1 1 d . . . . .
C13 C 0.2727(5) 0.5773(3) 1.14962(16) 0.0782(12) Uani 1 1 d . . . . .
H13 H 0.2178 0.6275 1.1635 0.094 Uiso 1 1 calc R U . . .
C62 C 0.9929(5) 0.3231(3) 0.22141(14) 0.0820(12) Uani 1 1 d . . . . .
H62 H 0.9629 0.3486 0.1929 0.098 Uiso 1 1 calc R U . . .
C11 C 0.4400(5) 0.4584(3) 1.16107(15) 0.0806(12) Uani 1 1 d . . . . .
H11 H 0.4988 0.4299 1.1833 0.097 Uiso 1 1 calc R U . . .
C54 C 0.0880(5) 0.5837(3) 0.43162(19) 0.0827(12) Uani 1 1 d . . . . .
H54 H 0.0331 0.6151 0.4098 0.099 Uiso 1 1 calc R U . . .
C48 C 0.3950(5) 0.5685(3) 0.68969(15) 0.0794(12) Uani 1 1 d . . . . .
H48 H 0.4056 0.5963 0.7246 0.095 Uiso 1 1 calc R U . . .
C18 C 0.0914(5) 0.5936(3) 0.92623(18) 0.0835(12) Uani 1 1 d . . . . .
H18 H 0.0381 0.6280 0.9055 0.100 Uiso 1 1 calc R U . . .
C12 C 0.3591(6) 0.5356(3) 1.18118(16) 0.0889(13) Uani 1 1 d . . . . .
H12 H 0.3652 0.5580 1.2165 0.107 Uiso 1 1 calc R U . . .
C25 C -0.0139(5) 0.1080(3) 0.62746(15) 0.0896(14) Uani 1 1 d . . . . .
H25 H -0.0775 0.0895 0.6506 0.108 Uiso 1 1 calc R U . . .
C31 C 1.0594(5) 0.3636(3) 0.71639(16) 0.0875(13) Uani 1 1 d . . . . .
H31 H 1.0445 0.3954 0.6891 0.105 Uiso 1 1 calc R U . . .
C32 C 1.1985(5) 0.3707(3) 0.74242(17) 0.0940(14) Uani 1 1 d . . . . .
H32 H 1.2811 0.4035 0.7318 0.113 Uiso 1 1 calc R U . . .
C61 C 1.1340(5) 0.3524(3) 0.24748(17) 0.1017(16) Uani 1 1 d . . . . .
H61 H 1.2019 0.3952 0.2359 0.122 Uiso 1 1 calc R U . . .
H6N H 0.764(5) 0.151(3) 0.3095(15) 0.100(13) Uiso 1 1 d . . . . .
H1N H 0.758(4) 0.185(3) 0.7949(13) 0.072(11) Uiso 1 1 d . . . . .
H14O H 0.517(3) 0.224(3) 0.1583(17) 0.116(17) Uiso 1 1 d D . . . .
H15O H 0.019(4) 0.178(3) -0.0860(9) 0.102(14) Uiso 1 1 d D . . . .
H10O H 1.015(5) 0.168(3) 0.4070(10) 0.125(17) Uiso 1 1 d D . . . .
C36 C 0.9619(5) 0.0034(3) 0.75219(18) 0.0989(15) Uani 1 1 d . . . . .
H36C H 0.9010 -0.0295 0.7730 0.148 Uiso 1 1 calc R U . . .
H36A H 0.9514 -0.0341 0.7177 0.148 Uiso 1 1 calc R U . . .
H36B H 0.9298 0.0668 0.7520 0.148 Uiso 1 1 calc R U . . .
O17 O 1.1028(4) 0.0128(3) 0.7712(2) 0.173(2) Uani 1 1 d . . . . .
H17O H 1.1270 -0.0406 0.7749 0.260 Uiso 1 1 calc R U . . .
 
 
_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
O8 C35 1.226(3) . ?
O7 C35 1.274(3) . ?
O15 C71 1.283(3) . ?
O15 H15O 0.942(19) . ?
O2 C22 1.231(4) . ?
O3 C28 1.284(3) . ?
O10 C58 1.271(4) . ?
O10 H10O 0.942(19) . ?
O13 C65 1.212(4) . ?
N3 C6 1.491(3) . ?
N3 C7 1.494(3) . ?
N3 H3N' 0.8900 . ?
N3 H3N 0.8900 . ?
O9 C58 1.220(3) . ?
N4 C27 1.334(3) . ?
N4 C23 1.336(4) . ?
N10 C70 1.331(3) . ?
N10 C66 1.342(3) . ?
O14 C65 1.302(4) . ?
O14 H14O 0.933(19) . ?
N8 C42 1.486(3) . ?
N8 C43 1.496(3) . ?
N8 H8N' 0.8900 . ?
N8 H8N 0.8900 . ?
N2 C1 1.318(4) . ?
N2 C3 1.372(4) . ?
N2 C4 1.471(4) . ?
N9 C59 1.332(3) . ?
N9 C63 1.345(4) . ?
O11 C64 1.235(4) . ?
O16 C71 1.211(3) . ?
N5 C34 1.337(4) . ?
N5 C30 1.351(4) . ?
N7 C37 1.316(4) . ?
N7 C39 1.367(4) . ?
N7 C40 1.466(4) . ?
O4 C28 1.219(3) . ?
O12 C64 1.254(4) . ?
O1 C22 1.266(4) . ?
N1 C1 1.324(4) . ?
N1 C2 1.358(4) . ?
N1 H1N 0.93(4) . ?
N6 C37 1.316(4) . ?
N6 C38 1.348(4) . ?
N6 H6N 1.01(4) . ?
O5 C29 1.282(5) . ?
O5 H5O 0.8200 . ?
C6 C5 1.513(4) . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C44 C57 1.413(4) . ?
C44 C45 1.421(4) . ?
C44 C43 1.505(4) . ?
C35 C34 1.504(4) . ?
C8 C21 1.411(4) . ?
C8 C9 1.419(4) . ?
C8 C7 1.505(4) . ?
C42 C41 1.511(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C41 C40 1.518(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C66 C67 1.385(4) . ?
C66 C65 1.496(4) . ?
C70 C69 1.383(4) . ?
C70 C71 1.505(4) . ?
C45 C46 1.423(4) . ?
C45 C50 1.437(4) . ?
C57 C56 1.429(4) . ?
C57 C52 1.439(4) . ?
C5 C4 1.512(4) . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C21 C20 1.430(4) . ?
C21 C16 1.439(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C22 C23 1.512(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C23 C24 1.386(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C27 C26 1.376(4) . ?
C27 C28 1.510(4) . ?
C34 C33 1.369(4) . ?
C59 C60 1.375(4) . ?
C59 C58 1.513(4) . ?
C9 C14 1.431(4) . ?
C9 C10 1.434(5) . ?
C64 C63 1.506(4) . ?
C1 H1 0.9300 . ?
C52 C51 1.379(5) . ?
C52 C53 1.424(5) . ?
C63 C62 1.376(5) . ?
C16 C15 1.372(5) . ?
C16 C17 1.427(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C3 C2 1.344(4) . ?
C3 H3 0.9300 . ?
C46 C47 1.366(5) . ?
C46 H46 0.9300 . ?
C50 C51 1.383(5) . ?
C50 C49 1.430(5) . ?
C37 H37 0.9300 . ?
C56 C55 1.348(5) . ?
C56 H56 0.9300 . ?
C2 H2 0.9300 . ?
C20 C19 1.358(5) . ?
C20 H20 0.9300 . ?
C14 C15 1.389(5) . ?
C14 C13 1.424(5) . ?
C10 C11 1.359(5) . ?
C10 H10 0.9300 . ?
C15 H15 0.9300 . ?
C51 H51 0.9300 . ?
C69 C68 1.376(5) . ?
C69 H69 0.9300 . ?
C67 C68 1.359(5) . ?
C67 H67 0.9300 . ?
C30 C31 1.377(5) . ?
C30 C29 1.476(5) . ?
C26 C25 1.367(5) . ?
C26 H26 0.9300 . ?
C24 C25 1.366(5) . ?
C24 H24 0.9300 . ?
C53 C54 1.338(5) . ?
C53 H53 0.9300 . ?
C68 H68 0.9300 . ?
C17 C18 1.334(5) . ?
C17 H17 0.9300 . ?
O6 C29 1.211(5) . ?
C47 C48 1.405(5) . ?
C47 H47 0.9300 . ?
C39 C38 1.345(5) . ?
C39 H39 0.9300 . ?
C55 C54 1.407(5) . ?
C55 H55 0.9300 . ?
C33 C32 1.376(5) . ?
C33 H33 0.9300 . ?
C19 C18 1.399(5) . ?
C19 H19 0.9300 . ?
C49 C48 1.338(5) . ?
C49 H49 0.9300 . ?
C38 H38 0.9300 . ?
C60 C61 1.383(5) . ?
C60 H60 0.9300 . ?
C13 C12 1.346(6) . ?
C13 H13 0.9300 . ?
C62 C61 1.379(5) . ?
C62 H62 0.9300 . ?
C11 C12 1.403(6) . ?
C11 H11 0.9300 . ?
C54 H54 0.9300 . ?
C48 H48 0.9300 . ?
C18 H18 0.9300 . ?
C12 H12 0.9300 . ?
C25 H25 0.9300 . ?
C31 C32 1.362(6) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C61 H61 0.9300 . ?
C36 O17 1.306(5) . ?
C36 H36C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
O17 H17O 0.8200 . ?
 
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
C71 O15 H15O 115(3) . . ?
C58 O10 H10O 111(3) . . ?
C6 N3 C7 110.6(2) . . ?
C6 N3 H3N' 109.5 . . ?
C7 N3 H3N' 109.5 . . ?
C6 N3 H3N 109.5 . . ?
C7 N3 H3N 109.5 . . ?
H3N' N3 H3N 108.1 . . ?
C27 N4 C23 118.3(2) . . ?
C70 N10 C66 117.7(2) . . ?
C65 O14 H14O 108(3) . . ?
C42 N8 C43 111.1(2) . . ?
C42 N8 H8N' 109.4 . . ?
C43 N8 H8N' 109.4 . . ?
C42 N8 H8N 109.4 . . ?
C43 N8 H8N 109.4 . . ?
H8N' N8 H8N 108.0 . . ?
C1 N2 C3 108.5(3) . . ?
C1 N2 C4 124.4(3) . . ?
C3 N2 C4 127.0(2) . . ?
C59 N9 C63 118.6(3) . . ?
C34 N5 C30 117.0(3) . . ?
C37 N7 C39 107.7(3) . . ?
C37 N7 C40 124.7(3) . . ?
C39 N7 C40 127.6(3) . . ?
C1 N1 C2 108.5(3) . . ?
C1 N1 H1N 125(2) . . ?
C2 N1 H1N 126(2) . . ?
C37 N6 C38 108.5(3) . . ?
C37 N6 H6N 124(2) . . ?
C38 N6 H6N 127(2) . . ?
C29 O5 H5O 109.5 . . ?
N3 C6 C5 111.9(2) . . ?
N3 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
N3 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
H6B C6 H6A 107.9 . . ?
C57 C44 C45 120.1(3) . . ?
C57 C44 C43 119.6(3) . . ?
C45 C44 C43 119.9(3) . . ?
O8 C35 O7 124.9(3) . . ?
O8 C35 C34 118.5(3) . . ?
O7 C35 C34 116.6(3) . . ?
C21 C8 C9 119.5(3) . . ?
C21 C8 C7 120.0(3) . . ?
C9 C8 C7 120.2(3) . . ?
N8 C42 C41 111.7(2) . . ?
N8 C42 H42A 109.3 . . ?
C41 C42 H42A 109.3 . . ?
N8 C42 H42B 109.3 . . ?
C41 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C42 C41 C40 112.1(2) . . ?
C42 C41 H41A 109.2 . . ?
C40 C41 H41A 109.2 . . ?
C42 C41 H41B 109.2 . . ?
C40 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
N10 C66 C67 122.2(3) . . ?
N10 C66 C65 115.0(3) . . ?
C67 C66 C65 122.9(3) . . ?
N10 C70 C69 122.9(3) . . ?
N10 C70 C71 117.7(2) . . ?
C69 C70 C71 119.4(3) . . ?
C44 C45 C46 124.2(3) . . ?
C44 C45 C50 118.8(3) . . ?
C46 C45 C50 116.9(3) . . ?
C44 C57 C56 123.4(3) . . ?
C44 C57 C52 120.0(3) . . ?
C56 C57 C52 116.5(3) . . ?
C4 C5 C6 112.3(2) . . ?
C4 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
C4 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
H5B C5 H5A 107.9 . . ?
C8 C21 C20 123.4(3) . . ?
C8 C21 C16 120.1(3) . . ?
C20 C21 C16 116.4(3) . . ?
N3 C7 C8 116.5(2) . . ?
N3 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N3 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
O2 C22 O1 126.1(3) . . ?
O2 C22 C23 118.9(3) . . ?
O1 C22 C23 115.0(3) . . ?
N2 C4 C5 112.2(2) . . ?
N2 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N4 C23 C24 122.1(3) . . ?
N4 C23 C22 116.0(3) . . ?
C24 C23 C22 121.9(3) . . ?
N8 C43 C44 116.7(2) . . ?
N8 C43 H43A 108.1 . . ?
C44 C43 H43A 108.1 . . ?
N8 C43 H43B 108.1 . . ?
C44 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
N4 C27 C26 122.6(3) . . ?
N4 C27 C28 117.9(2) . . ?
C26 C27 C28 119.5(3) . . ?
O4 C28 O3 124.9(3) . . ?
O4 C28 C27 120.2(3) . . ?
O3 C28 C27 114.9(3) . . ?
O16 C71 O15 124.8(3) . . ?
O16 C71 C70 120.9(3) . . ?
O15 C71 C70 114.3(2) . . ?
N5 C34 C33 123.0(3) . . ?
N5 C34 C35 118.0(3) . . ?
C33 C34 C35 119.0(3) . . ?
N9 C59 C60 123.0(3) . . ?
N9 C59 C58 117.7(3) . . ?
C60 C59 C58 119.3(3) . . ?
C8 C9 C14 119.4(3) . . ?
C8 C9 C10 123.6(3) . . ?
C14 C9 C10 116.9(3) . . ?
O13 C65 O14 125.3(3) . . ?
O13 C65 C66 121.7(3) . . ?
O14 C65 C66 113.0(3) . . ?
O9 C58 O10 125.3(3) . . ?
O9 C58 C59 119.8(3) . . ?
O10 C58 C59 114.9(3) . . ?
O11 C64 O12 126.2(3) . . ?
O11 C64 C63 117.5(3) . . ?
O12 C64 C63 116.2(3) . . ?
N2 C1 N1 108.7(3) . . ?
N2 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
C51 C52 C53 121.7(3) . . ?
C51 C52 C57 118.6(3) . . ?
C53 C52 C57 119.6(3) . . ?
N9 C63 C62 121.4(3) . . ?
N9 C63 C64 115.7(3) . . ?
C62 C63 C64 122.9(3) . . ?
C15 C16 C17 121.6(3) . . ?
C15 C16 C21 119.0(3) . . ?
C17 C16 C21 119.4(3) . . ?
N7 C40 C41 112.2(2) . . ?
N7 C40 H40A 109.2 . . ?
C41 C40 H40A 109.2 . . ?
N7 C40 H40B 109.2 . . ?
C41 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C2 C3 N2 106.7(3) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
C47 C46 C45 121.5(3) . . ?
C47 C46 H46 119.2 . . ?
C45 C46 H46 119.2 . . ?
C51 C50 C49 121.5(3) . . ?
C51 C50 C45 119.6(3) . . ?
C49 C50 C45 118.9(3) . . ?
N7 C37 N6 109.4(3) . . ?
N7 C37 H37 125.3 . . ?
N6 C37 H37 125.3 . . ?
C55 C56 C57 121.4(3) . . ?
C55 C56 H56 119.3 . . ?
C57 C56 H56 119.3 . . ?
C3 C2 N1 107.5(3) . . ?
C3 C2 H2 126.2 . . ?
N1 C2 H2 126.2 . . ?
C19 C20 C21 121.1(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C15 C14 C13 120.9(3) . . ?
C15 C14 C9 119.5(3) . . ?
C13 C14 C9 119.6(4) . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C16 C15 C14 122.5(3) . . ?
C16 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
C52 C51 C50 122.9(3) . . ?
C52 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
C68 C69 C70 118.8(3) . . ?
C68 C69 H69 120.6 . . ?
C70 C69 H69 120.6 . . ?
C68 C67 C66 119.6(3) . . ?
C68 C67 H67 120.2 . . ?
C66 C67 H67 120.2 . . ?
N5 C30 C31 122.4(3) . . ?
N5 C30 C29 118.1(3) . . ?
C31 C30 C29 119.4(3) . . ?
C25 C26 C27 118.6(3) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C54 C53 C52 121.0(4) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C67 C68 C69 118.8(3) . . ?
C67 C68 H68 120.6 . . ?
C69 C68 H68 120.6 . . ?
C18 C17 C16 121.6(4) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C46 C47 C48 121.1(4) . . ?
C46 C47 H47 119.5 . . ?
C48 C47 H47 119.5 . . ?
C38 C39 N7 107.1(3) . . ?
C38 C39 H39 126.5 . . ?
N7 C39 H39 126.5 . . ?
C56 C55 C54 121.4(4) . . ?
C56 C55 H55 119.3 . . ?
C54 C55 H55 119.3 . . ?
C34 C33 C32 119.3(4) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C20 C19 C18 121.8(4) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C48 C49 C50 122.0(4) . . ?
C48 C49 H49 119.0 . . ?
C50 C49 H49 119.0 . . ?
C39 C38 N6 107.3(3) . . ?
C39 C38 H38 126.3 . . ?
N6 C38 H38 126.3 . . ?
C59 C60 C61 118.4(3) . . ?
C59 C60 H60 120.8 . . ?
C61 C60 H60 120.8 . . ?
O6 C29 O5 125.2(4) . . ?
O6 C29 C30 120.7(4) . . ?
O5 C29 C30 114.0(4) . . ?
C12 C13 C14 120.9(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C63 C62 C61 119.7(3) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C53 C54 C55 120.0(4) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C49 C48 C47 119.6(4) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C32 C31 C30 119.5(4) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 118.5(4) . . ?
C31 C32 H32 120.7 . . ?
C33 C32 H32 120.7 . . ?
C62 C61 C60 118.7(3) . . ?
C62 C61 H61 120.7 . . ?
C60 C61 H61 120.7 . . ?
O17 C36 H36C 109.5 . . ?
O17 C36 H36A 109.5 . . ?
H36C C36 H36A 109.5 . . ?
O17 C36 H36B 109.5 . . ?
H36C C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C36 O17 H17O 109.5 . . ?
 
_refine_diff_density_max    0.540
_refine_diff_density_min   -0.353
_refine_diff_density_rms    0.048



