 
data_CPOC-101-SQ
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C132 H156 N12 O24' 
_chemical_formula_weight          2294.68

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'I 2/a'
_space_group_name_Hall            '-I 2ya'
 
_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+1/2, y, -z'
 'x+1/2, y+1/2, z+1/2'
 '-x+1, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y, z'
 '-x+1/2, -y+1/2, -z+1/2'
 'x, -y+1/2, z+1/2'
 
_cell_length_a                    20.4736(2)
_cell_length_b                    22.3662(3)
_cell_length_c                    30.2829(3)
_cell_angle_alpha                 90
_cell_angle_beta                  93.3220(10)
_cell_angle_gamma                 90
_cell_volume                      13843.7(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used   11573
_cell_measurement_theta_min     3.9330
_cell_measurement_theta_max     72.7080
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.101          
_exptl_crystal_F_000              4896
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.160
_exptl_crystal_size_mid           0.140
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.617
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type     'multi-scan' 
_exptl_absorpt_correction_T_min                   0.75023
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.5594
_diffrn_reflns_number             28415
_diffrn_reflns_av_unetI/netI      0.0250
_diffrn_reflns_av_R_equivalents   0.0200
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        37
_diffrn_reflns_theta_min          3.953
_diffrn_reflns_theta_max          73.425
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.969
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.969
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.969
_diffrn_reflns_point_group_measured_fraction_full  0.995
_reflns_number_total              13492
_reflns_number_gt                 10761
_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.
 
 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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_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)+(0.1599P)²+20.1793P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.00011(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          13492
_refine_ls_number_parameters      602
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0931
_refine_ls_R_factor_gt            0.0801
_refine_ls_wR_factor_ref          0.2627
_refine_ls_wR_factor_gt           0.2440
_refine_ls_goodness_of_fit_ref    1.025
_refine_ls_restrained_S_all       1.040
_refine_ls_shift/su_max           0.021
_refine_ls_shift/su_mean          0.001
 
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
O1 O 0.58443(8) 0.52171(9) 0.76815(5) 0.0427(4) Uani 1 1 d . . . . .
H1O H 0.616411 0.510239 0.751894 0.064 Uiso 1 1 d R U . . .
O2 O 0.44807(9) 0.69309(8) 0.76236(5) 0.0423(4) Uani 1 1 d . . . . .
O3 O 0.43726(10) 0.79012(9) 0.71634(6) 0.0490(5) Uani 1 1 d . . . . .
H3O H 0.454675 0.763630 0.734992 0.073 Uiso 1 1 d R U . . .
O4 O 0.55469(10) 0.85989(9) 0.59621(6) 0.0472(4) Uani 1 1 d . . . . .
O5 O 0.65005(10) 0.82292(9) 0.55003(6) 0.0509(5) Uani 1 1 d . . . . .
H5O H 0.609491 0.835682 0.551025 0.076 Uiso 1 1 d R U . . .
O6 O 0.77739(8) 0.64555(8) 0.55546(5) 0.0408(4) Uani 1 1 d . . . . .
O7 O 0.78855(8) 0.54813(9) 0.60041(5) 0.0402(4) Uani 1 1 d . . . . .
H7O H 0.784800 0.581013 0.584508 0.060 Uiso 1 1 d R U . . .
O8 O 0.67393(8) 0.47653(8) 0.72149(5) 0.0370(4) Uani 1 1 d . . . . .
N1 N 0.51166(10) 0.66026(11) 0.83318(7) 0.0426(5) Uani 1 1 d . . . . .
H1 H 0.485161 0.685257 0.820060 0.051 Uiso 1 1 calc R U . . .
N2 N 0.67074(11) 0.75036(11) 0.94075(6) 0.0424(5) Uani 1 1 d . . . . .
H2 H 0.665611 0.788458 0.942190 0.051 Uiso 1 1 calc R U . . .
N3 N 0.54444(11) 0.92093(10) 0.66722(8) 0.0461(5) Uani 1 1 d . . . . .
N4 N 0.70144(9) 1.01496(10) 0.77551(6) 0.0360(4) Uani 1 1 d . . . . .
H4 H 0.736226 1.025658 0.762984 0.043 Uiso 1 1 calc R U . . .
C1 C 0.54199(10) 0.55678(12) 0.74338(7) 0.0348(5) Uani 1 1 d . . . . .
C2 C 0.51566(11) 0.60669(12) 0.76526(7) 0.0363(5) Uani 1 1 d . . . . .
C3 C 0.47116(11) 0.64662(11) 0.74212(7) 0.0353(5) Uani 1 1 d . . . . .
C4 C 0.45269(11) 0.63404(11) 0.69709(7) 0.0336(5) Uani 1 1 d . . . . .
C5 C 0.47900(10) 0.58426(11) 0.67779(7) 0.0339(5) Uani 1 1 d . . . . .
H5 H 0.467042 0.576762 0.648217 0.041 Uiso 1 1 calc R U . . .
C6 C 0.52272(10) 0.54403(11) 0.69982(7) 0.0322(5) Uani 1 1 d . . . . .
C7 C 0.45747(13) 0.77931(12) 0.67513(8) 0.0414(6) Uani 1 1 d . . . . .
C8 C 0.49464(13) 0.82531(12) 0.65604(8) 0.0414(5) Uani 1 1 d . . . . .
C9 C 0.51892(13) 0.81849(12) 0.61264(8) 0.0404(5) Uani 1 1 d . . . . .
C10 C 0.50298(12) 0.76534(12) 0.58922(8) 0.0388(5) Uani 1 1 d . . . . .
C11 C 0.46710(12) 0.72183(11) 0.60966(7) 0.0363(5) Uani 1 1 d . . . . .
H11 H 0.458308 0.686506 0.594235 0.044 Uiso 1 1 calc R U . . .
C12 C 0.44297(12) 0.72730(11) 0.65216(8) 0.0363(5) Uani 1 1 d . . . . .
C13 C 0.65088(13) 0.76188(12) 0.54907(7) 0.0409(6) Uani 1 1 d . . . . .
C14 C 0.71352(13) 0.73446(12) 0.55181(7) 0.0404(5) Uani 1 1 d . . . . .
C15 C 0.71999(12) 0.67029(12) 0.55177(7) 0.0373(5) Uani 1 1 d . . . . .
C16 C 0.66162(12) 0.63582(12) 0.54702(7) 0.0359(5) Uani 1 1 d . . . . .
C17 C 0.60223(12) 0.66527(12) 0.54438(7) 0.0363(5) Uani 1 1 d . . . . .
H17 H 0.564547 0.642001 0.541965 0.044 Uiso 1 1 calc R U . . .
C18 C 0.59431(12) 0.72776(12) 0.54505(7) 0.0379(5) Uani 1 1 d . . . . .
C19 C 0.72970(11) 0.53438(11) 0.61631(8) 0.0348(5) Uani 1 1 d . . . . .
C20 C 0.73146(11) 0.51093(11) 0.66013(7) 0.0337(5) Uani 1 1 d . . . . .
C21 C 0.67202(11) 0.49563(11) 0.68048(7) 0.0333(5) Uani 1 1 d . . . . .
C22 C 0.61201(11) 0.50326(11) 0.65524(7) 0.0326(5) Uani 1 1 d . . . . .
C23 C 0.61354(11) 0.52618(11) 0.61315(7) 0.0336(5) Uani 1 1 d . . . . .
H23 H 0.573737 0.531922 0.597336 0.040 Uiso 1 1 calc R U . . .
C24 C 0.67077(11) 0.54157(11) 0.59224(7) 0.0335(5) Uani 1 1 d . . . . .
C25 C 0.54881(11) 0.48879(11) 0.67747(7) 0.0339(5) Uani 1 1 d . . . . .
H25 H 0.560734 0.460364 0.701213 0.041 Uiso 1 1 calc R U . . .
C26 C 0.40509(11) 0.67656(11) 0.67261(7) 0.0354(5) Uani 1 1 d . . . . .
H26 H 0.379044 0.694900 0.695140 0.042 Uiso 1 1 calc R U . . .
C27 C 0.52743(13) 0.75745(12) 0.54292(8) 0.0401(5) Uani 1 1 d . . . . .
H27 H 0.533836 0.797831 0.531369 0.048 Uiso 1 1 calc R U . . .
C28 C 0.66817(12) 0.56817(12) 0.54552(7) 0.0358(5) Uani 1 1 d . . . . .
H28 H 0.710927 0.560055 0.533838 0.043 Uiso 1 1 calc R U . . .
C29 C 0.53341(12) 0.61612(13) 0.81039(8) 0.0396(5) Uani 1 1 d . . . . .
H29 H 0.562248 0.589279 0.824598 0.048 Uiso 1 1 calc R U . . .
C30 C 0.50947(13) 0.87715(12) 0.68125(9) 0.0440(6) Uani 1 1 d . . . . .
H30 H 0.493427 0.880107 0.709279 0.053 Uiso 1 1 calc R U . . .
C31 C 0.77000(14) 0.77063(13) 0.55598(8) 0.0442(6) Uani 1 1 d . . . . .
H31 H 0.764497 0.811895 0.556413 0.053 Uiso 1 1 calc R U . . .
C32 C 0.79221(11) 0.50488(11) 0.68401(8) 0.0346(5) Uani 1 1 d . . . . .
H32 H 0.829822 0.515635 0.670132 0.042 Uiso 1 1 calc R U . . .
C33 C 0.35635(12) 0.64411(12) 0.64031(8) 0.0399(5) Uani 1 1 d . . . . .
H33A H 0.377976 0.635547 0.613357 0.048 Uiso 1 1 calc R U . . .
H33B H 0.344964 0.606147 0.653313 0.048 Uiso 1 1 calc R U . . .
C34 C 0.2948(2) 0.67759(18) 0.62848(18) 0.0930(16) Uani 1 1 d D . . . .
H34 H 0.274596 0.671770 0.656719 0.112 Uiso 1 1 calc R U . . .
C35 C 0.2830(4) 0.7331(4) 0.6249(4) 0.230(6) Uani 1 1 d D U . . .
H35A H 0.280850 0.744171 0.594233 0.345 Uiso 1 1 calc R U . . .
H35B H 0.317346 0.755223 0.640457 0.345 Uiso 1 1 calc R U . . .
H35C H 0.242047 0.741892 0.637335 0.345 Uiso 1 1 calc R U . . .
C36 C 0.2468(3) 0.6388(2) 0.6006(3) 0.146(3) Uani 1 1 d . U . . .
H36D H 0.261052 0.635991 0.570993 0.218 Uiso 1 1 calc R U . . .
H36E H 0.204067 0.656594 0.599890 0.218 Uiso 1 1 calc R U . . .
H36F H 0.245145 0.599595 0.613288 0.218 Uiso 1 1 calc R U . . .
C37 C 0.47730(14) 0.72712(14) 0.51068(8) 0.0479(6) Uani 1 1 d . . . . .
H37A H 0.468216 0.687377 0.521581 0.058 Uiso 1 1 calc R U . . .
H37B H 0.496216 0.722746 0.482223 0.058 Uiso 1 1 calc R U . . .
C38 C 0.4113(2) 0.7624(2) 0.50407(16) 0.0891(13) Uani 1 1 d . . . . .
H38 H 0.387545 0.760014 0.531220 0.107 Uiso 1 1 calc R U . . .
C39 C 0.4186(3) 0.8252(3) 0.4916(2) 0.122(2) Uani 1 1 d . . . . .
H39A H 0.448916 0.827374 0.468591 0.183 Uiso 1 1 d R U . . .
H39B H 0.435136 0.848024 0.516631 0.183 Uiso 1 1 d R U . . .
H39C H 0.377106 0.841064 0.480901 0.183 Uiso 1 1 d R U . . .
C40 C 0.3716(4) 0.7299(3) 0.4663(3) 0.190(5) Uani 1 1 d . . . . .
H40A H 0.373036 0.752863 0.439568 0.286 Uiso 1 1 calc R U . . .
H40B H 0.327006 0.725687 0.473984 0.286 Uiso 1 1 calc R U . . .
H40C H 0.390126 0.691121 0.461857 0.286 Uiso 1 1 calc R U . . .
C41 C 0.61720(12) 0.54001(12) 0.51260(7) 0.0389(5) Uani 1 1 d . . . . .
H41A H 0.618196 0.561543 0.484843 0.047 Uiso 1 1 calc R U . . .
H41B H 0.574250 0.546120 0.523780 0.047 Uiso 1 1 calc R U . . .
C42 C 0.62508(12) 0.47287(14) 0.50290(10) 0.0512(7) Uani 1 1 d . . . . .
H42 H 0.606866 0.450793 0.527291 0.061 Uiso 1 1 calc R U . . .
C43 C 0.58250(17) 0.4588(2) 0.46094(14) 0.0824(13) Uani 1 1 d . . . . .
H43A H 0.602375 0.475398 0.435736 0.124 Uiso 1 1 calc R U . . .
H43B H 0.539858 0.475963 0.463275 0.124 Uiso 1 1 calc R U . . .
H43C H 0.578588 0.416275 0.457504 0.124 Uiso 1 1 calc R U . . .
C44 C 0.6945(2) 0.4493(3) 0.49776(19) 0.1005(15) Uani 1 1 d . . . . .
C45 C 0.49721(11) 0.45724(12) 0.64675(8) 0.0387(5) Uani 1 1 d . . . . .
H45A H 0.457282 0.453236 0.662248 0.046 Uiso 1 1 calc R U . . .
H45B H 0.487520 0.482450 0.621142 0.046 Uiso 1 1 calc R U . . .
C46 C 0.51717(14) 0.39545(13) 0.63075(10) 0.0492(6) Uani 1 1 d . . . . .
H46 H 0.557069 0.399990 0.614682 0.059 Uiso 1 1 calc R U . . .
C47 C 0.46358(18) 0.37088(15) 0.59861(11) 0.0617(8) Uani 1 1 d . . . . .
H47A H 0.458652 0.396563 0.573236 0.093 Uiso 1 1 calc R U . . .
H47B H 0.423048 0.369175 0.612990 0.093 Uiso 1 1 calc R U . . .
H47C H 0.475330 0.331445 0.589384 0.093 Uiso 1 1 calc R U . . .
C48 C 0.5310(3) 0.35151(17) 0.66757(15) 0.0860(13) Uani 1 1 d . . . . .
H48A H 0.538378 0.312646 0.655345 0.129 Uiso 1 1 calc R U . . .
H48B H 0.494322 0.349858 0.685873 0.129 Uiso 1 1 calc R U . . .
H48C H 0.569258 0.363908 0.685052 0.129 Uiso 1 1 calc R U . . .
C49 C 0.52998(13) 0.66957(15) 0.88000(8) 0.0477(6) Uani 1 1 d . . . . .
H49A H 0.536897 0.631153 0.894388 0.057 Uiso 1 1 calc R U . . .
H49B H 0.494608 0.689713 0.893939 0.057 Uiso 1 1 calc R U . . .
C50 C 0.59155(13) 0.70657(12) 0.88599(8) 0.0409(5) Uani 1 1 d . . . . .
H50A H 0.583885 0.745794 0.873044 0.049 Uiso 1 1 calc R U . . .
H50B H 0.626310 0.687543 0.870669 0.049 Uiso 1 1 calc R U . . .
C51 C 0.61269(14) 0.71332(14) 0.93482(8) 0.0461(6) Uani 1 1 d . . . . .
H51A H 0.577404 0.731217 0.950299 0.055 Uiso 1 1 calc R U . . .
H51B H 0.621616 0.674158 0.947544 0.055 Uiso 1 1 calc R U . . .
C52 C 0.56018(13) 0.97335(12) 0.69474(10) 0.0473(6) Uani 1 1 d . . . . .
H52A H 0.526615 0.978586 0.715738 0.057 Uiso 1 1 calc R U . . .
H52B H 0.560239 1.008655 0.676133 0.057 Uiso 1 1 calc R U . . .
C53 C 0.62628(13) 0.96746(13) 0.71971(10) 0.0486(6) Uani 1 1 d . . . . .
H53A H 0.627448 0.930822 0.736881 0.058 Uiso 1 1 calc R U . . .
H53B H 0.660372 0.965246 0.698818 0.058 Uiso 1 1 calc R U . . .
C54 C 0.63888(11) 1.02013(11) 0.75014(8) 0.0369(5) Uani 1 1 d . . . . .
H54A H 0.638619 1.056573 0.732761 0.044 Uiso 1 1 calc R U . . .
H54B H 0.603956 1.022909 0.770361 0.044 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
O1 C1 1.363(3) . ?
O2 C3 1.309(3) . ?
O3 C7 1.359(3) . ?
O4 C9 1.298(3) . ?
O5 C13 1.366(3) . ?
O6 C15 1.298(3) . ?
O7 C19 1.358(3) . ?
O8 C21 1.312(3) . ?
N1 C29 1.298(3) . ?
N1 C49 1.461(3) . ?
N2 C31 1.299(4) 7_666 ?
N2 C51 1.451(3) . ?
N3 C30 1.299(4) . ?
N3 C52 1.464(3) . ?
N4 C32 1.303(3) 7_666 ?
N4 C54 1.459(3) . ?
C1 C6 1.384(3) . ?
C1 C2 1.420(4) . ?
C2 C29 1.409(3) . ?
C2 C3 1.430(4) . ?
C3 C4 1.422(3) . ?
C4 C5 1.381(3) . ?
C4 C26 1.523(3) . ?
C5 C6 1.409(3) . ?
C6 C25 1.521(3) . ?
C7 C12 1.379(4) . ?
C7 C8 1.422(4) . ?
C8 C30 1.412(4) . ?
C8 C9 1.440(4) . ?
C9 C10 1.413(4) . ?
C10 C11 1.387(4) . ?
C10 C27 1.526(3) . ?
C11 C12 1.410(3) . ?
C12 C26 1.526(4) . ?
C13 C18 1.386(4) . ?
C13 C14 1.420(4) . ?
C14 C31 1.411(4) . ?
C14 C15 1.441(4) . ?
C15 C16 1.422(3) . ?
C16 C17 1.381(4) . ?
C16 C28 1.520(4) . ?
C17 C18 1.407(4) . ?
C18 C27 1.520(4) . ?
C19 C24 1.382(3) . ?
C19 C20 1.425(3) . ?
C20 C32 1.408(3) . ?
C20 C21 1.437(3) . ?
C21 C22 1.419(3) . ?
C22 C23 1.376(3) . ?
C22 C25 1.528(3) . ?
C23 C24 1.407(3) . ?
C24 C28 1.533(3) . ?
C25 C45 1.538(3) . ?
C26 C33 1.538(3) . ?
C27 C37 1.533(3) . ?
C28 C41 1.536(3) . ?
C33 C34 1.492(4) . ?
C34 C35 1.268(8) . ?
C34 C36 1.528(5) . ?
C37 C38 1.568(5) . ?
C38 C39 1.465(8) . ?
C38 C40 1.545(6) . ?
C41 C42 1.540(4) . ?
C42 C43 1.531(4) . ?
C42 C44 1.532(6) . ?
C45 C46 1.528(4) . ?
C46 C48 1.501(5) . ?
C46 C47 1.526(4) . ?
C49 C50 1.510(4) . ?
C50 C51 1.524(3) . ?
C52 C53 1.517(4) . ?
C53 C54 1.509(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
C29 N1 C49 123.2(2) . . ?
C31 N2 C51 123.9(3) 7_666 . ?
C30 N3 C52 121.7(3) . . ?
C32 N4 C54 124.0(2) 7_666 . ?
O1 C1 C6 122.9(2) . . ?
O1 C1 C2 116.3(2) . . ?
C6 C1 C2 120.8(2) . . ?
C29 C2 C1 119.1(2) . . ?
C29 C2 C3 120.2(2) . . ?
C1 C2 C3 120.7(2) . . ?
O2 C3 C4 121.5(2) . . ?
O2 C3 C2 120.2(2) . . ?
C4 C3 C2 118.2(2) . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 C26 123.5(2) . . ?
C3 C4 C26 118.0(2) . . ?
C4 C5 C6 124.5(2) . . ?
C1 C6 C5 117.2(2) . . ?
C1 C6 C25 120.2(2) . . ?
C5 C6 C25 122.5(2) . . ?
O3 C7 C12 123.0(2) . . ?
O3 C7 C8 116.3(2) . . ?
C12 C7 C8 120.6(2) . . ?
C30 C8 C7 118.5(2) . . ?
C30 C8 C9 120.4(2) . . ?
C7 C8 C9 121.0(2) . . ?
O4 C9 C10 121.8(2) . . ?
O4 C9 C8 120.4(2) . . ?
C10 C9 C8 117.7(2) . . ?
C11 C10 C9 118.6(2) . . ?
C11 C10 C27 122.6(2) . . ?
C9 C10 C27 118.7(2) . . ?
C10 C11 C12 124.7(2) . . ?
C7 C12 C11 117.2(2) . . ?
C7 C12 C26 121.5(2) . . ?
C11 C12 C26 121.3(2) . . ?
O5 C13 C18 122.7(2) . . ?
O5 C13 C14 116.3(2) . . ?
C18 C13 C14 121.0(2) . . ?
C31 C14 C13 119.4(3) . . ?
C31 C14 C15 119.7(2) . . ?
C13 C14 C15 120.9(2) . . ?
O6 C15 C16 121.9(2) . . ?
O6 C15 C14 120.5(2) . . ?
C16 C15 C14 117.6(2) . . ?
C17 C16 C15 118.6(2) . . ?
C17 C16 C28 123.5(2) . . ?
C15 C16 C28 117.9(2) . . ?
C16 C17 C18 125.1(2) . . ?
C13 C18 C17 116.8(2) . . ?
C13 C18 C27 120.6(2) . . ?
C17 C18 C27 122.5(2) . . ?
O7 C19 C24 123.5(2) . . ?
O7 C19 C20 116.0(2) . . ?
C24 C19 C20 120.5(2) . . ?
C32 C20 C19 119.2(2) . . ?
C32 C20 C21 120.1(2) . . ?
C19 C20 C21 120.7(2) . . ?
O8 C21 C22 121.8(2) . . ?
O8 C21 C20 120.3(2) . . ?
C22 C21 C20 117.9(2) . . ?
C23 C22 C21 118.6(2) . . ?
C23 C22 C25 123.5(2) . . ?
C21 C22 C25 117.8(2) . . ?
C22 C23 C24 124.9(2) . . ?
C19 C24 C23 117.3(2) . . ?
C19 C24 C28 121.0(2) . . ?
C23 C24 C28 121.7(2) . . ?
C6 C25 C22 110.63(19) . . ?
C6 C25 C45 113.29(19) . . ?
C22 C25 C45 113.61(18) . . ?
C4 C26 C12 109.63(19) . . ?
C4 C26 C33 112.8(2) . . ?
C12 C26 C33 114.78(19) . . ?
C18 C27 C10 110.74(19) . . ?
C18 C27 C37 113.7(2) . . ?
C10 C27 C37 113.1(2) . . ?
C16 C28 C24 110.93(18) . . ?
C16 C28 C41 111.7(2) . . ?
C24 C28 C41 115.2(2) . . ?
N1 C29 C2 123.5(2) . . ?
N3 C30 C8 123.2(3) . . ?
N2 C31 C14 123.8(3) 7_666 . ?
N4 C32 C20 123.6(2) 7_666 . ?
C34 C33 C26 115.1(2) . . ?
C35 C34 C33 131.7(5) . . ?
C35 C34 C36 113.3(4) . . ?
C33 C34 C36 110.8(3) . . ?
C27 C37 C38 113.5(3) . . ?
C39 C38 C40 108.4(5) . . ?
C39 C38 C37 114.5(4) . . ?
C40 C38 C37 105.7(4) . . ?
C28 C41 C42 116.7(2) . . ?
C43 C42 C44 109.4(3) . . ?
C43 C42 C41 107.3(3) . . ?
C44 C42 C41 117.6(3) . . ?
C46 C45 C25 114.8(2) . . ?
C48 C46 C47 109.6(3) . . ?
C48 C46 C45 113.5(3) . . ?
C47 C46 C45 109.4(2) . . ?
N1 C49 C50 111.1(2) . . ?
C49 C50 C51 111.0(2) . . ?
N2 C51 C50 111.2(2) . . ?
N3 C52 C53 112.0(2) . . ?
C54 C53 C52 110.6(2) . . ?
N4 C54 C53 111.9(2) . . ?
 
_refine_diff_density_max    1.408
_refine_diff_density_min   -0.533
_refine_diff_density_rms    0.069





#===END


 
data_CPOC-102-SQ
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C112 H138 Cl0 N8 O16' 
_chemical_formula_weight          1852.30

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0147   0.0070
 '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'   0.0256   0.0140
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0406   0.0250
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.3293   0.5493
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 2/c'
_space_group_name_Hall            '-C 2yc'
 
_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+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                    16.2614(2)
_cell_length_b                    24.5637(2)
_cell_length_c                    36.5980(5)
_cell_angle_alpha                 90
_cell_angle_beta                  100.3070(10)
_cell_angle_gamma                 90
_cell_volume                      14382.8(3)
_cell_formula_units_Z             4
_cell_measurement_temperature    100(2)
_cell_oxdiff_measurement_reflns_used   24345
_cell_measurement_reflns_used   24345
_cell_measurement_theta_min     2.8740
_cell_measurement_theta_max     59.2650
_exptl_absorpt_correction_T_min                   0.09271
_exptl_absorpt_correction_T_max                   1.00000
 
_exptl_crystal_description        bolck
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.855          
_exptl_crystal_F_000              3976
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min           0.08
_exptl_absorpt_coefficient_mu     0.290
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength      1.3405
_diffrn_radiation_type            GaK\a
_diffrn_source                     'micro-focus metaljet'
_diffrn_measurement_device_type   'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.5594
_diffrn_reflns_number             40886
_diffrn_reflns_av_unetI/netI      0.0356
_diffrn_reflns_av_R_equivalents   0.0383
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -30
_diffrn_reflns_limit_k_max        31
_diffrn_reflns_limit_l_min        -46
_diffrn_reflns_limit_l_max        46
_diffrn_reflns_theta_min          2.866
_diffrn_reflns_theta_max          59.337
_diffrn_reflns_theta_full         53.543
_diffrn_measured_fraction_theta_max   0.973
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.973
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.973
_diffrn_reflns_point_group_measured_fraction_full  0.995
_reflns_number_total              15469
_reflns_number_gt                 13031
_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.
 
 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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_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)+(0.0456P)²+125.8750P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          15469
_refine_ls_number_parameters      620
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1196
_refine_ls_R_factor_gt            0.1044
_refine_ls_wR_factor_ref          0.2538
_refine_ls_wR_factor_gt           0.2477
_refine_ls_goodness_of_fit_ref    1.080
_refine_ls_restrained_S_all       1.080
_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
O1 O 0.57293(17) 0.88068(11) 0.14924(8) 0.0359(6) Uani 1 1 d . . . . .
H1O H 0.529625 0.868053 0.133628 0.054 Uiso 1 1 d R U . . .
O2 O 0.8122(2) 0.80052(12) 0.22173(9) 0.0438(7) Uani 1 1 d . . . . .
O3 O 0.8383(2) 0.69827(12) 0.23749(9) 0.0511(8) Uani 1 1 d . . . . .
H3O H 0.837986 0.732263 0.229875 0.077 Uiso 1 1 d R U . . .
O4 O 0.74565(17) 0.52272(11) 0.19586(8) 0.0335(6) Uani 1 1 d . . . . .
O5 O 0.55586(17) 0.83688(11) 0.39092(8) 0.0346(6) Uani 1 1 d . . . . .
O6 O 0.65793(16) 0.65995(11) 0.42502(8) 0.0319(6) Uani 1 1 d . . . . .
H6O H 0.638106 0.626843 0.426505 0.048 Uiso 1 1 d R U . . .
O7 O 0.60758(17) 0.55813(10) 0.42126(7) 0.0311(6) Uani 1 1 d . . . . .
O8 O 0.36894(18) 0.47287(11) 0.35017(8) 0.0341(6) Uani 1 1 d . . . . .
H8O H 0.331417 0.487604 0.332646 0.051 Uiso 1 1 d R U . . .
N1 N 0.7227(2) 0.86850(14) 0.24839(10) 0.0387(8) Uani 1 1 d . . . . .
H1A H 0.761021 0.843941 0.252036 0.046 Uiso 1 1 calc R U . . .
N2 N 0.6989(2) 0.80466(14) 0.38069(9) 0.0348(7) Uani 1 1 d . . . . .
H2 H 0.659533 0.828498 0.377292 0.042 Uiso 1 1 calc R U . . .
N3 N 0.6202(2) 0.47885(12) 0.37740(9) 0.0309(7) Uani 1 1 d . . . . .
H3 H 0.642964 0.503954 0.392224 0.037 Uiso 1 1 calc R U . . .
N4 N 0.7817(2) 0.54761(14) 0.26446(9) 0.0347(7) Uani 1 1 d . . . . .
H4 H 0.761143 0.524895 0.247359 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6772(3) 0.87237(16) 0.21586(11) 0.0350(9) Uani 1 1 d . . . . .
H1 H 0.631790 0.896005 0.212511 0.042 Uiso 1 1 calc R U . . .
C2 C 0.6937(3) 0.84173(15) 0.18463(11) 0.0331(8) Uani 1 1 d . . . . .
C3 C 0.6387(2) 0.84665(15) 0.14982(11) 0.0295(8) Uani 1 1 d . . . . .
C4 C 0.6542(2) 0.81788(15) 0.11906(11) 0.0299(8) Uani 1 1 d . . . . .
C5 C 0.7238(2) 0.78275(15) 0.12464(11) 0.0286(8) Uani 1 1 d . . . . .
H5 H 0.733568 0.762558 0.104348 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7785(2) 0.77585(15) 0.15746(12) 0.0322(8) Uani 1 1 d . . . . .
C7 C 0.7637(3) 0.80623(16) 0.18922(12) 0.0346(9) Uani 1 1 d . . . . .
C8 C 0.8501(2) 0.73575(16) 0.16271(12) 0.0345(9) Uani 1 1 d . . . . .
H8 H 0.890422 0.748077 0.184309 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8216(2) 0.67881(15) 0.17194(11) 0.0319(8) Uani 1 1 d . . . . .
C10 C 0.7978(2) 0.63913(15) 0.14424(11) 0.0299(8) Uani 1 1 d . . . . .
H10 H 0.799535 0.648741 0.119811 0.036 Uiso 1 1 calc R U . . .
C11 C 0.7722(2) 0.58703(15) 0.15080(11) 0.0294(8) Uani 1 1 d . . . . .
C12 C 0.7689(2) 0.57182(15) 0.18775(11) 0.0297(8) Uani 1 1 d . . . . .
C13 C 0.7922(2) 0.61101(16) 0.21655(12) 0.0337(8) Uani 1 1 d . . . . .
C14 C 0.8170(3) 0.66513(17) 0.20791(13) 0.0390(9) Uani 1 1 d . . . . .
C15 C 0.7979(3) 0.59647(17) 0.25446(12) 0.0358(9) Uani 1 1 d . . . . .
H15 H 0.813758 0.622766 0.272635 0.043 Uiso 1 1 calc R U . . .
C16 C 0.7960(3) 0.52859(17) 0.30289(11) 0.0365(9) Uani 1 1 d . . . . .
H16A H 0.805256 0.559735 0.319413 0.044 Uiso 1 1 calc R U . . .
H16B H 0.846009 0.506302 0.307395 0.044 Uiso 1 1 calc R U . . .
C17 C 0.7229(2) 0.49572(16) 0.31165(11) 0.0311(8) Uani 1 1 d . . . . .
H17A H 0.708546 0.467207 0.293280 0.037 Uiso 1 1 calc R U . . .
H17B H 0.674586 0.519135 0.310819 0.037 Uiso 1 1 calc R U . . .
C18 C 0.7466(2) 0.47070(16) 0.35003(11) 0.0309(8) Uani 1 1 d . . . . .
H18A H 0.792594 0.445630 0.349868 0.037 Uiso 1 1 calc R U . . .
H18B H 0.766290 0.499401 0.367636 0.037 Uiso 1 1 calc R U . . .
C19 C 0.6764(3) 0.44060(15) 0.36340(11) 0.0330(8) Uani 1 1 d . . . . .
H19A H 0.645127 0.419648 0.343090 0.040 Uiso 1 1 calc R U . . .
H19B H 0.699611 0.415476 0.382999 0.040 Uiso 1 1 calc R U . . .
C20 C 0.5387(3) 0.47821(15) 0.36938(11) 0.0312(8) Uani 1 1 d . . . . .
H20 H 0.512650 0.452939 0.352201 0.037 Uiso 1 1 calc R U . . .
C21 C 0.4887(2) 0.51451(14) 0.38583(10) 0.0275(7) Uani 1 1 d . . . . .
C22 C 0.3995(2) 0.51110(14) 0.37533(9) 0.0266(7) Uani 1 1 d . . . . .
C23 C 0.3490(2) 0.54619(14) 0.39064(10) 0.0266(7) Uani 1 1 d . . . . .
C24 C 0.3880(2) 0.58490(14) 0.41633(10) 0.0271(7) Uani 1 1 d . . . . .
H24 H 0.353741 0.609245 0.426005 0.032 Uiso 1 1 calc R U . . .
C25 C 0.4728(2) 0.58968(14) 0.42830(10) 0.0261(7) Uani 1 1 d . . . . .
C26 C 0.5265(2) 0.55433(15) 0.41239(10) 0.0291(8) Uani 1 1 d . . . . .
C27 C 0.5114(2) 0.63127(14) 0.45703(10) 0.0269(7) Uani 1 1 d . . . . .
H27 H 0.566999 0.617548 0.467834 0.032 Uiso 1 1 calc R U . . .
C28 C 0.5245(2) 0.68605(14) 0.43953(10) 0.0267(7) Uani 1 1 d . . . . .
C29 C 0.4636(2) 0.72805(14) 0.43613(10) 0.0270(7) Uani 1 1 d . . . . .
H29 H 0.414207 0.720874 0.444727 0.032 Uiso 1 1 calc R U . . .
C30 C 0.4723(2) 0.77835(15) 0.42110(10) 0.0268(7) Uani 1 1 d . . . . .
C31 C 0.5447(2) 0.79006(15) 0.40598(10) 0.0281(7) Uani 1 1 d . . . . .
C32 C 0.6087(2) 0.74860(15) 0.40928(10) 0.0271(7) Uani 1 1 d . . . . .
C33 C 0.5954(2) 0.69698(15) 0.42492(10) 0.0260(7) Uani 1 1 d . . . . .
C34 C 0.6835(2) 0.75884(16) 0.39579(11) 0.0320(8) Uani 1 1 d . . . . .
H34 H 0.723539 0.731444 0.397836 0.038 Uiso 1 1 calc R U . . .
C35 C 0.7776(3) 0.8193(2) 0.36891(14) 0.0453(11) Uani 1 1 d . . . . .
H35A H 0.816610 0.789312 0.374605 0.054 Uiso 1 1 calc R U . . .
H35B H 0.801433 0.850603 0.383151 0.054 Uiso 1 1 calc R U . . .
C36 C 0.7681(3) 0.8327(2) 0.32750(13) 0.0450(11) Uani 1 1 d . . . . .
H36A H 0.820631 0.846959 0.322626 0.054 Uiso 1 1 calc R U . . .
H36B H 0.756277 0.799296 0.313346 0.054 Uiso 1 1 calc R U . . .
C37 C 0.6988(3) 0.87388(19) 0.31400(12) 0.0405(10) Uani 1 1 d . . . . .
H37A H 0.645558 0.855028 0.308766 0.049 Uiso 1 1 calc R U . . .
H37B H 0.696141 0.900045 0.333608 0.049 Uiso 1 1 calc R U . . .
C38 C 0.7125(3) 0.90392(18) 0.27947(12) 0.0449(11) Uani 1 1 d . . . . .
H38A H 0.665248 0.927857 0.271482 0.054 Uiso 1 1 calc R U . . .
H38B H 0.761903 0.926528 0.285768 0.054 Uiso 1 1 calc R U . . .
C39 C 0.5958(2) 0.82217(15) 0.08191(10) 0.0290(8) Uani 1 1 d . . . . .
H39 H 0.567290 0.857349 0.081805 0.035 Uiso 1 1 calc R U . . .
C40 C 0.6420(3) 0.82303(17) 0.04945(11) 0.0355(9) Uani 1 1 d . . . . .
H40A H 0.674620 0.789880 0.050102 0.043 Uiso 1 1 calc R U . . .
H40B H 0.680857 0.853329 0.052805 0.043 Uiso 1 1 calc R U . . .
C41 C 0.5864(3) 0.82803(19) 0.01038(12) 0.0462(11) Uani 1 1 d . . . . .
H41 H 0.551505 0.795287 0.006200 0.055 Uiso 1 1 calc R U . . .
C42 C 0.6418(4) 0.8294(2) -0.01946(14) 0.0671(17) Uani 1 1 d . . . . .
H42A H 0.607183 0.832076 -0.043567 0.101 Uiso 1 1 calc R U . . .
H42B H 0.674462 0.796705 -0.018064 0.101 Uiso 1 1 calc R U . . .
H42C H 0.678314 0.860379 -0.015393 0.101 Uiso 1 1 calc R U . . .
C43 C 0.5285(4) 0.8769(2) 0.00687(15) 0.0618(14) Uani 1 1 d . . . . .
H43A H 0.499973 0.880214 -0.018366 0.093 Uiso 1 1 calc R U . . .
H43B H 0.560604 0.909283 0.013870 0.093 Uiso 1 1 calc R U . . .
H43C H 0.488301 0.872262 0.022900 0.093 Uiso 1 1 calc R U . . .
C44 C 0.8966(3) 0.73541(16) 0.12911(13) 0.0381(9) Uani 1 1 d . . . . .
H44A H 0.939775 0.707692 0.133310 0.046 Uiso 1 1 calc R U . . .
H44B H 0.857249 0.725194 0.107021 0.046 Uiso 1 1 calc R U . . .
C45 C 0.9369(3) 0.78962(18) 0.12178(15) 0.0467(12) Uani 1 1 d . . . . .
H45 H 0.892305 0.816427 0.114575 0.056 Uiso 1 1 calc R U . . .
C46 C 0.9834(3) 0.7826(2) 0.08944(18) 0.0608(15) Uani 1 1 d . . . . .
H46A H 1.012707 0.815623 0.086018 0.091 Uiso 1 1 calc R U . . .
H46B H 0.944087 0.774621 0.067234 0.091 Uiso 1 1 calc R U . . .
H46C H 1.022604 0.753229 0.094701 0.091 Uiso 1 1 calc R U . . .
C47 C 0.9955(3) 0.8111(2) 0.15548(18) 0.0612(15) Uani 1 1 d . . . . .
H47A H 1.023160 0.843132 0.148775 0.092 Uiso 1 1 calc R U . . .
H47B H 1.036320 0.783797 0.164511 0.092 Uiso 1 1 calc R U . . .
H47C H 0.964129 0.819995 0.174541 0.092 Uiso 1 1 calc R U . . .
C48 C 0.7460(2) 0.54488(15) 0.12088(11) 0.0308(8) Uani 1 1 d . . . . .
H48 H 0.759907 0.509324 0.132500 0.037 Uiso 1 1 calc R U . . .
C49 C 0.7918(3) 0.54823(17) 0.08787(12) 0.0388(9) Uani 1 1 d . . . . .
H49A H 0.772321 0.580055 0.073135 0.047 Uiso 1 1 calc R U . . .
H49B H 0.851108 0.552786 0.097091 0.047 Uiso 1 1 calc R U . . .
C50 C 0.7786(4) 0.4980(2) 0.06317(16) 0.0645(16) Uani 1 1 d . . . . .
H50 H 0.718433 0.491868 0.055502 0.077 Uiso 1 1 calc R U . . .
C51 C 0.8177(6) 0.5063(3) 0.02824(19) 0.090(2) Uani 1 1 d . . . . .
H51A H 0.784854 0.531929 0.011998 0.135 Uiso 1 1 calc R U . . .
H51B H 0.819148 0.472159 0.015601 0.135 Uiso 1 1 calc R U . . .
H51C H 0.873614 0.519991 0.035334 0.135 Uiso 1 1 calc R U . . .
C52 C 0.8174(8) 0.4479(3) 0.0838(2) 0.151(5) Uani 1 1 d . . . . .
H52A H 0.817379 0.418431 0.066636 0.227 Uiso 1 1 calc R U . . .
H52B H 0.785569 0.437853 0.102467 0.227 Uiso 1 1 calc R U . . .
H52C H 0.873859 0.455956 0.095433 0.227 Uiso 1 1 calc R U . . .
C53 C 0.4620(3) 0.63609(15) 0.48943(10) 0.0306(8) Uani 1 1 d . . . . .
H53A H 0.488527 0.663364 0.506794 0.037 Uiso 1 1 calc R U . . .
H53B H 0.405779 0.648537 0.479607 0.037 Uiso 1 1 calc R U . . .
C54 C 0.4568(3) 0.58253(16) 0.51037(11) 0.0353(9) Uani 1 1 d . . . . .
H54 H 0.438230 0.554057 0.491981 0.042 Uiso 1 1 calc R U . . .
C55 C 0.3930(3) 0.5865(2) 0.53582(13) 0.0469(11) Uani 1 1 d . . . . .
H55A H 0.390038 0.552349 0.548281 0.070 Uiso 1 1 calc R U . . .
H55B H 0.339179 0.595008 0.521418 0.070 Uiso 1 1 calc R U . . .
H55C H 0.409291 0.614634 0.553860 0.070 Uiso 1 1 calc R U . . .
C56 C 0.5429(3) 0.5659(2) 0.53223(13) 0.0489(12) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 C3 1.354(5) . ?
O2 C7 1.312(5) . ?
O3 C14 1.349(5) . ?
O4 C12 1.313(4) . ?
O5 C31 1.302(4) . ?
O6 C33 1.364(4) . ?
O7 C26 1.304(5) . ?
O8 C22 1.347(4) . ?
N1 C1 1.288(5) . ?
N1 C38 1.465(5) . ?
N2 C34 1.298(5) . ?
N2 C35 1.467(5) . ?
N3 C20 1.305(5) . ?
N3 C19 1.465(5) . ?
N4 C15 1.296(5) . ?
N4 C16 1.461(5) . ?
C1 C2 1.433(6) . ?
C2 C7 1.420(6) . ?
C2 C3 1.424(6) . ?
C3 C4 1.390(5) . ?
C4 C5 1.409(5) . ?
C4 C39 1.517(5) . ?
C5 C6 1.371(6) . ?
C6 C7 1.437(6) . ?
C6 C8 1.512(5) . ?
C8 C9 1.530(5) . ?
C8 C44 1.555(6) . ?
C9 C14 1.373(6) . ?
C9 C10 1.409(6) . ?
C10 C11 1.380(5) . ?
C11 C12 1.413(5) . ?
C11 C48 1.512(5) . ?
C12 C13 1.428(6) . ?
C13 C15 1.420(6) . ?
C13 C14 1.440(5) . ?
C16 C17 1.517(5) . ?
C17 C18 1.519(5) . ?
C18 C19 1.513(5) . ?
C20 C21 1.412(5) . ?
C21 C22 1.435(5) . ?
C21 C26 1.437(5) . ?
C22 C23 1.378(5) . ?
C23 C24 1.406(5) . ?
C23 C48 1.526(5) 2_655 ?
C24 C25 1.375(5) . ?
C25 C26 1.427(5) . ?
C25 C27 1.519(5) . ?
C27 C28 1.522(5) . ?
C27 C53 1.551(5) . ?
C28 C33 1.380(5) . ?
C28 C29 1.421(5) . ?
C29 C30 1.370(5) . ?
C30 C31 1.418(5) . ?
C30 C39 1.533(5) 2_655 ?
C31 C32 1.445(5) . ?
C32 C34 1.416(5) . ?
C32 C33 1.423(5) . ?
C35 C36 1.531(7) . ?
C36 C37 1.530(6) . ?
C37 C38 1.514(6) . ?
C39 C40 1.516(5) . ?
C40 C41 1.554(6) . ?
C41 C43 1.517(7) . ?
C41 C42 1.535(7) . ?
C44 C45 1.529(6) . ?
C45 C47 1.512(8) . ?
C45 C46 1.524(7) . ?
C48 C49 1.531(5) . ?
C49 C50 1.522(7) . ?
C50 C52 1.521(10) . ?
C50 C51 1.540(7) . ?
C53 C54 1.532(5) . ?
C54 C55 1.517(6) . ?
C54 C56 1.539(7) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 N1 C38 123.2(4) . . ?
C34 N2 C35 125.6(4) . . ?
C20 N3 C19 125.8(3) . . ?
C15 N4 C16 124.3(4) . . ?
N1 C1 C2 122.7(4) . . ?
C7 C2 C3 121.3(4) . . ?
C7 C2 C1 119.2(4) . . ?
C3 C2 C1 119.5(4) . . ?
O1 C3 C4 123.9(4) . . ?
O1 C3 C2 115.7(3) . . ?
C4 C3 C2 120.3(4) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C39 121.0(3) . . ?
C5 C4 C39 122.1(3) . . ?
C6 C5 C4 125.5(4) . . ?
C5 C6 C7 117.9(4) . . ?
C5 C6 C8 123.8(4) . . ?
C7 C6 C8 118.2(4) . . ?
O2 C7 C2 120.8(4) . . ?
O2 C7 C6 121.2(4) . . ?
C2 C7 C6 118.0(4) . . ?
C6 C8 C9 111.5(3) . . ?
C6 C8 C44 112.1(3) . . ?
C9 C8 C44 112.3(3) . . ?
C14 C9 C10 117.7(4) . . ?
C14 C9 C8 120.4(4) . . ?
C10 C9 C8 121.9(4) . . ?
C11 C10 C9 124.6(4) . . ?
C10 C11 C12 118.4(4) . . ?
C10 C11 C48 124.3(4) . . ?
C12 C11 C48 117.2(3) . . ?
O4 C12 C11 121.4(4) . . ?
O4 C12 C13 120.1(3) . . ?
C11 C12 C13 118.5(3) . . ?
C15 C13 C12 120.9(4) . . ?
C15 C13 C14 118.4(4) . . ?
C12 C13 C14 120.5(4) . . ?
O3 C14 C9 124.8(4) . . ?
O3 C14 C13 115.0(4) . . ?
C9 C14 C13 120.1(4) . . ?
N4 C15 C13 121.9(4) . . ?
N4 C16 C17 112.2(3) . . ?
C16 C17 C18 109.4(3) . . ?
C19 C18 C17 114.6(3) . . ?
N3 C19 C18 110.7(3) . . ?
N3 C20 C21 122.4(4) . . ?
C20 C21 C22 118.7(3) . . ?
C20 C21 C26 120.6(4) . . ?
C22 C21 C26 120.6(3) . . ?
O8 C22 C23 122.7(3) . . ?
O8 C22 C21 117.1(3) . . ?
C23 C22 C21 120.2(3) . . ?
C22 C23 C24 117.6(3) . . ?
C22 C23 C48 121.5(3) . 2_655 ?
C24 C23 C48 120.8(3) . 2_655 ?
C25 C24 C23 125.3(3) . . ?
C24 C25 C26 118.0(3) . . ?
C24 C25 C27 123.0(3) . . ?
C26 C25 C27 119.1(3) . . ?
O7 C26 C25 121.3(3) . . ?
O7 C26 C21 120.5(3) . . ?
C25 C26 C21 118.2(3) . . ?
C25 C27 C28 112.0(3) . . ?
C25 C27 C53 112.0(3) . . ?
C28 C27 C53 112.7(3) . . ?
C33 C28 C29 116.3(3) . . ?
C33 C28 C27 121.7(3) . . ?
C29 C28 C27 122.0(3) . . ?
C30 C29 C28 124.7(4) . . ?
C29 C30 C31 119.5(3) . . ?
C29 C30 C39 122.5(3) . 2_655 ?
C31 C30 C39 117.9(3) . 2_655 ?
O5 C31 C30 122.2(3) . . ?
O5 C31 C32 120.3(3) . . ?
C30 C31 C32 117.4(3) . . ?
C34 C32 C33 120.0(3) . . ?
C34 C32 C31 119.8(3) . . ?
C33 C32 C31 120.2(3) . . ?
O6 C33 C28 122.9(3) . . ?
O6 C33 C32 115.4(3) . . ?
C28 C33 C32 121.7(3) . . ?
N2 C34 C32 123.1(4) . . ?
N2 C35 C36 113.8(4) . . ?
C37 C36 C35 113.6(4) . . ?
C38 C37 C36 112.5(4) . . ?
N1 C38 C37 114.4(4) . . ?
C40 C39 C4 112.6(3) . . ?
C40 C39 C30 114.0(3) . 2_655 ?
C4 C39 C30 110.1(3) . 2_655 ?
C39 C40 C41 115.7(4) . . ?
C43 C41 C42 110.9(4) . . ?
C43 C41 C40 113.0(4) . . ?
C42 C41 C40 109.7(4) . . ?
C45 C44 C8 114.7(4) . . ?
C47 C45 C46 110.2(4) . . ?
C47 C45 C44 112.8(4) . . ?
C46 C45 C44 109.0(4) . . ?
C11 C48 C23 109.0(3) . 2_655 ?
C11 C48 C49 114.9(3) . . ?
C23 C48 C49 113.1(3) 2_655 . ?
C50 C49 C48 112.9(4) . . ?
C52 C50 C49 111.0(6) . . ?
C52 C50 C51 108.9(5) . . ?
C49 C50 C51 110.5(5) . . ?
C54 C53 C27 113.5(3) . . ?
C55 C54 C53 110.9(3) . . ?
C55 C54 C56 110.9(4) . . ?
C53 C54 C56 111.2(4) . . ?
 
_refine_diff_density_max    0.543
_refine_diff_density_min   -0.368
_refine_diff_density_rms    0.080





#===END


 
data_CPOC-103-SQ
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C143 H172 Cl17 N8 O18' 
_chemical_formula_weight          2893.53

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.3639   0.7018
 '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                    14.1137(6)
_cell_length_b                    16.1576(7)
_cell_length_c                    16.9639(5)
_cell_angle_alpha                 105.394(3)
_cell_angle_beta                  92.720(3)
_cell_angle_gamma                 93.859(4)
_cell_volume                      3712.7(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   6569
_cell_measurement_theta_min     3.9760
_cell_measurement_theta_max     67.2520
 
_exptl_crystal_description       block 
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.294          
_exptl_crystal_F_000              1519
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.08
_exptl_absorpt_coefficient_mu     3.391
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min                   0.81100
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.5594
_diffrn_reflns_number             25308
_diffrn_reflns_av_unetI/netI      0.0677
_diffrn_reflns_av_R_equivalents   0.0485
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          4.010
_diffrn_reflns_theta_max          67.318
_diffrn_reflns_theta_full         67.318
_diffrn_measured_fraction_theta_max   0.957
_diffrn_measured_fraction_theta_full  0.957
_diffrn_reflns_Laue_measured_fraction_max    0.957
_diffrn_reflns_Laue_measured_fraction_full   0.957
_diffrn_reflns_point_group_measured_fraction_max   0.957
_diffrn_reflns_point_group_measured_fraction_full  0.957
_reflns_number_total              12751
_reflns_number_gt                 7944
_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.
 
 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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_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)+(0.1855P)²+15.2695P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.0125(9)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          12751
_refine_ls_number_parameters      685
_refine_ls_number_restraints      30
_refine_ls_R_factor_all           0.1821
_refine_ls_R_factor_gt            0.1369
_refine_ls_wR_factor_ref          0.4051
_refine_ls_wR_factor_gt           0.3718
_refine_ls_goodness_of_fit_ref    1.054
_refine_ls_restrained_S_all       1.053
_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
O1 O 0.5107(4) 0.6150(4) 0.5578(3) 0.0667(14) Uani 1 1 d . . . . .
H1O H 0.501148 0.571667 0.579586 0.100 Uiso 1 1 d R U . . .
O2 O 0.3263(4) 0.8513(6) 0.5772(4) 0.111(3) Uani 1 1 d . . . . .
O3 O 0.1879(4) 0.9280(4) 0.6561(4) 0.0764(17) Uani 1 1 d . . . . .
H3O H 0.229375 0.903243 0.629062 0.115 Uiso 1 1 d R U . . .
O4 O 0.0006(3) 0.8318(3) 0.8455(3) 0.0494(11) Uani 1 1 d . . . . .
O5 O -0.0087(3) 0.7111(3) 0.9210(3) 0.0537(12) Uani 1 1 d . . . . .
H5O H -0.004127 0.752348 0.896013 0.081 Uiso 1 1 d R U . . .
O6 O 0.1695(3) 0.4683(3) 0.9064(3) 0.0476(11) Uani 1 1 d . . . . .
O7 O 0.3028(3) 0.4075(3) 0.8121(3) 0.0510(11) Uani 1 1 d . . . . .
H7O H 0.265556 0.430531 0.850814 0.077 Uiso 1 1 d R U . . .
O8 O 0.5024(4) 0.4945(3) 0.6266(3) 0.0599(13) Uani 1 1 d . . . . .
N2 N -0.0746(4) 0.8839(4) 0.7271(3) 0.0488(13) Uani 1 1 d . . . . .
H2 H -0.083691 0.860982 0.766695 0.059 Uiso 1 1 calc R U . . .
N3 N 0.0154(4) 0.5443(4) 0.1104(3) 0.0484(13) Uani 1 1 d . . . . .
H3 H -0.036228 0.569821 0.110748 0.058 Uiso 1 1 calc R U . . .
N4 N -0.3814(4) 0.6438(4) 0.4181(3) 0.0527(14) Uani 1 1 d . . . . .
H4 H -0.427372 0.614725 0.432725 0.063 Uiso 1 1 calc R U . . .
C1 C 0.4783(5) 0.6868(6) 0.6063(4) 0.0581(19) Uani 1 1 d . . . . .
C2 C 0.4207(6) 0.7335(8) 0.5671(5) 0.082(3) Uani 1 1 d . . . . .
C3 C 0.3827(6) 0.8102(8) 0.6136(6) 0.083(3) Uani 1 1 d . . . . .
C4 C 0.4075(5) 0.8391(5) 0.6998(5) 0.0559(18) Uani 1 1 d . . . . .
C5 C 0.4633(4) 0.7909(4) 0.7346(4) 0.0480(16) Uani 1 1 d . . . . .
H5 H 0.478491 0.810160 0.790824 0.058 Uiso 1 1 calc R U . . .
C6 C 0.5001(4) 0.7131(5) 0.6909(4) 0.0464(15) Uani 1 1 d . . . . .
C7 C 0.1842(5) 0.9036(5) 0.7274(5) 0.0589(19) Uani 1 1 d . . . . .
C8 C 0.0943(5) 0.8850(4) 0.7538(5) 0.0518(17) Uani 1 1 d . . . . .
C9 C 0.0841(4) 0.8550(4) 0.8257(5) 0.0468(16) Uani 1 1 d . . . . .
C10 C 0.1688(5) 0.8538(4) 0.8744(4) 0.0489(16) Uani 1 1 d . . . . .
C11 C 0.2541(5) 0.8732(4) 0.8463(4) 0.0477(16) Uani 1 1 d . . . . .
H11 H 0.308682 0.870330 0.878033 0.057 Uiso 1 1 calc R U . . .
C12 C 0.2665(5) 0.8974(5) 0.7731(5) 0.0555(19) Uani 1 1 d . . . . .
C13 C 0.0775(4) 0.6802(4) 0.9277(4) 0.0426(14) Uani 1 1 d . . . . .
C14 C 0.0786(4) 0.5905(4) 0.9166(4) 0.0425(14) Uani 1 1 d . . . . .
C15 C 0.1680(4) 0.5522(4) 0.9198(4) 0.0416(14) Uani 1 1 d . . . . .
C16 C 0.2544(4) 0.6078(4) 0.9381(3) 0.0358(13) Uani 1 1 d . . . . .
C17 C 0.2476(4) 0.6932(4) 0.9489(4) 0.0402(14) Uani 1 1 d . . . . .
H17 H 0.304115 0.728467 0.959772 0.048 Uiso 1 1 calc R U . . .
C18 C 0.1615(4) 0.7341(4) 0.9453(4) 0.0439(15) Uani 1 1 d . . . . .
C19 C 0.3649(4) 0.4701(4) 0.7985(4) 0.0397(14) Uani 1 1 d . . . . .
C20 C 0.4010(4) 0.4513(4) 0.7181(4) 0.0424(14) Uani 1 1 d . . . . .
C21 C 0.4680(5) 0.5132(4) 0.6981(4) 0.0465(15) Uani 1 1 d . . . . .
C22 C 0.4922(4) 0.5932(4) 0.7581(4) 0.0419(14) Uani 1 1 d . . . . .
C23 C 0.4515(4) 0.6074(4) 0.8313(4) 0.0406(14) Uani 1 1 d . . . . .
H23 H 0.466273 0.660788 0.868938 0.049 Uiso 1 1 calc R U . . .
C24 C 0.3888(4) 0.5478(4) 0.8547(4) 0.0365(13) Uani 1 1 d . . . . .
C25 C 0.3663(5) 0.9196(5) 0.7492(6) 0.064(2) Uani 1 1 d . . . . .
H25 H 0.357790 0.955786 0.711675 0.077 Uiso 1 1 calc R U . . .
C26 C 0.1604(5) 0.8311(4) 0.9554(4) 0.0463(15) Uani 1 1 d . . . . .
H26 H 0.097587 0.846680 0.973757 0.056 Uiso 1 1 calc R U . . .
C27 C 0.3483(4) 0.5679(4) 0.9385(3) 0.0366(13) Uani 1 1 d . . . . .
H27 H 0.334187 0.512316 0.950181 0.044 Uiso 1 1 calc R U . . .
C28 C 0.5580(5) 0.6606(4) 0.7343(4) 0.0458(15) Uani 1 1 d . . . . .
H28 H 0.599166 0.628675 0.694093 0.055 Uiso 1 1 calc R U . . .
C29 C 0.6237(4) 0.7162(4) 0.8054(3) 0.0364(13) Uani 1 1 d . . . . .
H29A H 0.585164 0.742459 0.849738 0.044 Uiso 1 1 calc R U . . .
H29B H 0.656033 0.762201 0.787562 0.044 Uiso 1 1 calc R U . . .
C30 C 0.6992(5) 0.6669(5) 0.8389(4) 0.0519(17) Uani 1 1 d . . . . .
H30 H 0.668872 0.611902 0.842828 0.062 Uiso 1 1 calc R U . . .
C31 C 0.7776(7) 0.6486(8) 0.7794(6) 0.095(3) Uani 1 1 d . . . . .
H31A H 0.810513 0.701941 0.777507 0.142 Uiso 1 1 calc R U . . .
H31B H 0.749995 0.618703 0.725683 0.142 Uiso 1 1 calc R U . . .
H31C H 0.821718 0.613571 0.797349 0.142 Uiso 1 1 calc R U . . .
C32 C 0.7418(8) 0.7158(8) 0.9214(6) 0.099(3) Uani 1 1 d . . . . .
H32A H 0.792823 0.685924 0.937233 0.148 Uiso 1 1 calc R U . . .
H32B H 0.694061 0.720917 0.960436 0.148 Uiso 1 1 calc R U . . .
H32C H 0.766066 0.772222 0.919617 0.148 Uiso 1 1 calc R U . . .
C33 C 0.4313(5) 0.9745(5) 0.8218(7) 0.081(3) Uani 1 1 d . . . . .
H33A H 0.442977 0.940115 0.859712 0.097 Uiso 1 1 calc R U . . .
H33B H 0.492034 0.987969 0.801641 0.097 Uiso 1 1 calc R U . . .
C34 C 0.3939(6) 1.0591(5) 0.8694(10) 0.114(5) Uani 1 1 d . . . . .
H34 H 0.335284 1.045482 0.893839 0.136 Uiso 1 1 calc R U . . .
C35 C 0.4638(7) 1.1073(6) 0.9357(9) 0.108(4) Uani 1 1 d . . . . .
H35A H 0.521080 1.122320 0.912523 0.162 Uiso 1 1 calc R U . . .
H35B H 0.477852 1.072151 0.971627 0.162 Uiso 1 1 calc R U . . .
H35C H 0.437944 1.158787 0.966015 0.162 Uiso 1 1 calc R U . . .
C36 C 0.3695(8) 1.1130(7) 0.8078(12) 0.160(8) Uani 1 1 d . . . . .
H36A H 0.314450 1.085635 0.772868 0.240 Uiso 1 1 calc R U . . .
H36B H 0.422490 1.116473 0.775014 0.240 Uiso 1 1 calc R U . . .
H36C H 0.356676 1.170018 0.837767 0.240 Uiso 1 1 calc R U . . .
C37 C 0.2334(5) 0.8840(4) 1.0226(5) 0.0549(18) Uani 1 1 d . . . . .
H37A H 0.296748 0.869834 1.006945 0.066 Uiso 1 1 calc R U . . .
H37B H 0.223204 0.868065 1.072950 0.066 Uiso 1 1 calc R U . . .
C38 C 0.2280(6) 0.9814(5) 1.0386(6) 0.068(2) Uani 1 1 d . . . . .
H38 H 0.239346 0.996177 0.987246 0.082 Uiso 1 1 calc R U . . .
C39 C 0.3066(7) 1.0301(6) 1.1023(8) 0.099(4) Uani 1 1 d . . . . .
H39A H 0.367569 1.016455 1.081956 0.148 Uiso 1 1 calc R U . . .
H39B H 0.300204 1.013598 1.152218 0.148 Uiso 1 1 calc R U . . .
H39C H 0.301398 1.090971 1.112648 0.148 Uiso 1 1 calc R U . . .
C40 C 0.1330(7) 1.0113(6) 1.0646(7) 0.088(3) Uani 1 1 d . . . . .
H40A H 0.135069 1.072788 1.075342 0.132 Uiso 1 1 calc R U . . .
H40B H 0.118324 0.994998 1.113395 0.132 Uiso 1 1 calc R U . . .
H40C H 0.084856 0.985091 1.021674 0.132 Uiso 1 1 calc R U . . .
C41 C 0.4202(4) 0.6208(4) 1.0084(4) 0.0390(13) Uani 1 1 d . . . . .
H41A H 0.479839 0.593812 1.003401 0.047 Uiso 1 1 calc R U . . .
H41B H 0.432382 0.677982 1.001062 0.047 Uiso 1 1 calc R U . . .
C42 C 0.3885(4) 0.6295(4) 1.0948(4) 0.0416(14) Uani 1 1 d . . . . .
H42 H 0.328292 0.656801 1.099577 0.050 Uiso 1 1 calc R U . . .
C43 C 0.4631(6) 0.6883(5) 1.1572(5) 0.0620(19) Uani 1 1 d . . . . .
H43A H 0.523862 0.664889 1.150419 0.093 Uiso 1 1 calc R U . . .
H43B H 0.444666 0.692000 1.211737 0.093 Uiso 1 1 calc R U . . .
H43C H 0.467440 0.744759 1.148601 0.093 Uiso 1 1 calc R U . . .
C44 C 0.3728(5) 0.5430(5) 1.1139(4) 0.0525(17) Uani 1 1 d . . . . .
H44A H 0.321644 0.508791 1.078083 0.079 Uiso 1 1 calc R U . . .
H44B H 0.356850 0.552044 1.169776 0.079 Uiso 1 1 calc R U . . .
H44C H 0.429866 0.513596 1.105877 0.079 Uiso 1 1 calc R U . . .
C49 C 0.1268(6) 0.6433(5) 0.2161(5) 0.065(2) Uani 1 1 d . . . . .
C50 C 0.1042(5) 0.5973(5) 0.1251(4) 0.0559(18) Uani 1 1 d . . . . .
H50A H 0.101335 0.639977 0.094372 0.067 Uiso 1 1 calc R U . . .
H50B H 0.155227 0.561571 0.105283 0.067 Uiso 1 1 calc R U . . .
C51 C 0.0125(5) 0.8976(4) 0.7093(4) 0.0513(17) Uani 1 1 d . . . . .
H51 H 0.021527 0.917305 0.663284 0.062 Uiso 1 1 calc R U . . .
C52 C -0.1580(5) 0.9046(5) 0.6848(5) 0.0601(19) Uani 1 1 d . . . . .
H52A H -0.137083 0.931601 0.643159 0.072 Uiso 1 1 calc R U . . .
H52B H -0.190756 0.946372 0.723764 0.072 Uiso 1 1 calc R U . . .
C53 C -0.2276(6) 0.8284(6) 0.6446(5) 0.067(2) Uani 1 1 d . . . . .
H53A H -0.249601 0.801520 0.685867 0.080 Uiso 1 1 calc R U . . .
H53B H -0.282353 0.848281 0.620437 0.080 Uiso 1 1 calc R U . . .
C54 C -0.1848(6) 0.7641(6) 0.5804(6) 0.079(3) Uani 1 1 d . . . . .
H54A H -0.133642 0.740945 0.605896 0.095 Uiso 1 1 calc R U . . .
H54B H -0.157012 0.792872 0.542563 0.095 Uiso 1 1 calc R U . . .
C55 C -0.2556(6) 0.6875(6) 0.5306(5) 0.071(2) Uani 1 1 d . . . . .
H55A H -0.220405 0.645117 0.494652 0.085 Uiso 1 1 calc R U . . .
H55B H -0.286362 0.660156 0.568175 0.085 Uiso 1 1 calc R U . . .
C56 C -0.3282(5) 0.7161(5) 0.4816(5) 0.0580(19) Uani 1 1 d . . . . .
H56A H -0.297851 0.756027 0.454893 0.070 Uiso 1 1 calc R U . . .
H56B H -0.372949 0.746893 0.517836 0.070 Uiso 1 1 calc R U . . .
C57 C -0.0072(5) 0.5396(4) 0.9034(4) 0.0459(15) Uani 1 1 d . . . . .
H57 H -0.062991 0.567333 0.904559 0.055 Uiso 1 1 calc R U . . .
C58 C 0.3617(5) 0.3771(4) 0.6581(4) 0.0516(17) Uani 1 1 d . . . . .
H58 H 0.318268 0.340181 0.674551 0.062 Uiso 1 1 calc R U . . .
C45A C 0.3877(10) 0.6784(9) 0.4787(8) 0.035(3) Uani 0.5 1 d . U P A 1
H45A H 0.408387 0.623982 0.457571 0.042 Uiso 0.5 1 calc R U P A 1
N1A N 0.3297(7) 0.7118(7) 0.4355(6) 0.035(2) Uani 0.5 1 d . U P A 1
H1A H 0.310453 0.761451 0.457872 0.042 Uiso 0.5 1 calc R U P A 1
C46A C 0.2971(9) 0.6693(8) 0.3530(7) 0.040(3) Uani 0.5 1 d . U P A 1
H46A H 0.338063 0.624213 0.330529 0.048 Uiso 0.5 1 calc R U P A 1
H46B H 0.300085 0.710171 0.320275 0.048 Uiso 0.5 1 calc R U P A 1
C47A C 0.1970(9) 0.6309(8) 0.3491(7) 0.042(3) Uani 0.5 1 d . U P A 1
H47A H 0.157252 0.676139 0.373943 0.050 Uiso 0.5 1 calc R U P A 1
H47B H 0.195137 0.589376 0.381196 0.050 Uiso 0.5 1 calc R U P A 1
C48A C 0.1548(8) 0.5857(8) 0.2609(7) 0.036(3) Uani 0.5 1 d . U P A 1
H48A H 0.201768 0.550706 0.231545 0.044 Uiso 0.5 1 calc R U P A 1
H48B H 0.099895 0.547429 0.263986 0.044 Uiso 0.5 1 calc R U P A 1
C45B C 0.3993(13) 0.7290(16) 0.4915(12) 0.072(5) Uani 0.5 1 d . . P A 2
H45B H 0.423295 0.682181 0.455728 0.086 Uiso 0.5 1 calc R U P A 2
N1B N 0.3489(11) 0.7774(15) 0.4514(10) 0.090(5) Uani 0.5 1 d . . P A 2
H1B H 0.326662 0.823078 0.480493 0.108 Uiso 0.5 1 calc R U P A 2
C46B C 0.3319(13) 0.7575(16) 0.3675(10) 0.086(6) Uani 0.5 1 d . . P A 2
H46C H 0.372693 0.713668 0.341506 0.104 Uiso 0.5 1 calc R U P A 2
H46D H 0.346913 0.808346 0.348852 0.104 Uiso 0.5 1 calc R U P A 2
C47B C 0.2275(17) 0.7246(18) 0.3427(13) 0.104(7) Uani 0.5 1 d . . P A 2
H47C H 0.187786 0.771962 0.360498 0.125 Uiso 0.5 1 calc R U P A 2
H47D H 0.209471 0.681224 0.370456 0.125 Uiso 0.5 1 calc R U P A 2
C48B C 0.2084(15) 0.6842(12) 0.2457(12) 0.081(5) Uani 0.5 1 d . . P A 2
H48C H 0.255707 0.689980 0.210755 0.098 Uiso 0.5 1 calc R U P A 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 C1 1.354(10) . ?
O2 C3 1.302(9) . ?
O3 C7 1.370(9) . ?
O4 C9 1.299(8) . ?
O5 C13 1.357(7) . ?
O6 C15 1.316(7) . ?
O7 C19 1.367(7) . ?
O8 C21 1.296(8) . ?
N2 C51 1.298(9) . ?
N2 C52 1.453(9) . ?
N3 C57 1.310(8) 2_566 ?
N3 C50 1.442(9) . ?
N4 C58 1.294(9) 2_566 ?
N4 C56 1.493(9) . ?
C1 C6 1.398(10) . ?
C1 C2 1.404(12) . ?
C2 C45B 1.28(2) . ?
C2 C3 1.435(15) . ?
C2 C45A 1.557(17) . ?
C3 C4 1.430(12) . ?
C4 C5 1.365(9) . ?
C4 C25 1.517(11) . ?
C5 C6 1.425(10) . ?
C6 C28 1.516(9) . ?
C7 C12 1.389(10) . ?
C7 C8 1.406(10) . ?
C8 C51 1.405(10) . ?
C8 C9 1.437(10) . ?
C9 C10 1.425(9) . ?
C10 C11 1.362(10) . ?
C10 C26 1.522(10) . ?
C11 C12 1.413(10) . ?
C12 C25 1.529(10) . ?
C13 C18 1.394(9) . ?
C13 C14 1.413(9) . ?
C14 C57 1.390(9) . ?
C14 C15 1.448(9) . ?
C15 C16 1.434(9) . ?
C16 C17 1.353(8) . ?
C16 C27 1.513(8) . ?
C17 C18 1.427(8) . ?
C18 C26 1.532(9) . ?
C19 C24 1.369(8) . ?
C19 C20 1.442(9) . ?
C20 C58 1.411(9) . ?
C20 C21 1.446(9) . ?
C21 C22 1.427(9) . ?
C22 C23 1.364(9) . ?
C22 C28 1.530(9) . ?
C23 C24 1.411(9) . ?
C24 C27 1.520(8) . ?
C25 C33 1.533(13) . ?
C26 C37 1.531(9) . ?
C27 C41 1.548(8) . ?
C28 C29 1.526(9) . ?
C29 C30 1.546(9) . ?
C30 C32 1.487(12) . ?
C30 C31 1.524(12) . ?
C33 C34 1.533(13) . ?
C34 C35 1.473(16) . ?
C34 C36 1.568(19) . ?
C37 C38 1.532(10) . ?
C38 C40 1.502(12) . ?
C38 C39 1.528(12) . ?
C41 C42 1.527(9) . ?
C42 C44 1.521(9) . ?
C42 C43 1.536(10) . ?
C49 C48B 1.30(2) . ?
C49 C48A 1.413(14) . ?
C49 C50 1.533(10) . ?
C52 C53 1.508(11) . ?
C53 C54 1.475(12) . ?
C54 C55 1.562(12) . ?
C55 C56 1.463(12) . ?
C45A N1A 1.307(18) . ?
N1A C46A 1.424(16) . ?
C46A C47A 1.494(18) . ?
C47A C48A 1.550(16) . ?
C45B N1B 1.38(3) . ?
N1B C46B 1.38(2) . ?
C46B C47B 1.53(3) . ?
C47B C48B 1.60(3) . ?
 
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
C51 N2 C52 124.7(7) . . ?
C57 N3 C50 125.1(6) 2_566 . ?
C58 N4 C56 123.0(6) 2_566 . ?
O1 C1 C6 122.1(7) . . ?
O1 C1 C2 116.4(7) . . ?
C6 C1 C2 121.5(8) . . ?
C45B C2 C1 133.4(14) . . ?
C45B C2 C3 105.8(14) . . ?
C1 C2 C3 120.3(7) . . ?
C1 C2 C45A 110.0(10) . . ?
C3 C2 C45A 127.9(9) . . ?
O2 C3 C4 121.7(10) . . ?
O2 C3 C2 119.9(9) . . ?
C4 C3 C2 118.5(7) . . ?
C5 C4 C3 118.6(8) . . ?
C5 C4 C25 122.8(7) . . ?
C3 C4 C25 118.5(7) . . ?
C4 C5 C6 124.5(7) . . ?
C1 C6 C5 116.5(6) . . ?
C1 C6 C28 121.8(7) . . ?
C5 C6 C28 121.6(6) . . ?
O3 C7 C12 121.6(7) . . ?
O3 C7 C8 118.1(6) . . ?
C12 C7 C8 120.3(7) . . ?
C51 C8 C7 118.9(7) . . ?
C51 C8 C9 119.3(6) . . ?
C7 C8 C9 121.7(6) . . ?
O4 C9 C10 122.2(7) . . ?
O4 C9 C8 120.8(6) . . ?
C10 C9 C8 117.1(6) . . ?
C11 C10 C9 118.5(7) . . ?
C11 C10 C26 122.8(6) . . ?
C9 C10 C26 118.7(6) . . ?
C10 C11 C12 125.5(6) . . ?
C7 C12 C11 116.6(7) . . ?
C7 C12 C25 122.8(7) . . ?
C11 C12 C25 120.5(6) . . ?
O5 C13 C18 122.0(6) . . ?
O5 C13 C14 117.0(6) . . ?
C18 C13 C14 121.1(6) . . ?
C57 C14 C13 119.2(6) . . ?
C57 C14 C15 120.5(6) . . ?
C13 C14 C15 120.3(6) . . ?
O6 C15 C16 121.1(5) . . ?
O6 C15 C14 120.4(6) . . ?
C16 C15 C14 118.5(5) . . ?
C17 C16 C15 117.8(5) . . ?
C17 C16 C27 123.3(5) . . ?
C15 C16 C27 118.7(5) . . ?
C16 C17 C18 126.0(6) . . ?
C13 C18 C17 116.4(6) . . ?
C13 C18 C26 120.9(6) . . ?
C17 C18 C26 122.6(6) . . ?
O7 C19 C24 123.5(6) . . ?
O7 C19 C20 115.5(5) . . ?
C24 C19 C20 120.9(5) . . ?
C58 C20 C19 118.6(6) . . ?
C58 C20 C21 121.4(6) . . ?
C19 C20 C21 119.6(5) . . ?
O8 C21 C22 122.7(6) . . ?
O8 C21 C20 119.2(6) . . ?
C22 C21 C20 118.0(6) . . ?
C23 C22 C21 118.6(6) . . ?
C23 C22 C28 123.7(6) . . ?
C21 C22 C28 117.7(6) . . ?
C22 C23 C24 125.3(6) . . ?
C19 C24 C23 117.4(6) . . ?
C19 C24 C27 120.6(5) . . ?
C23 C24 C27 122.0(5) . . ?
C4 C25 C12 110.4(6) . . ?
C4 C25 C33 115.0(6) . . ?
C12 C25 C33 113.1(8) . . ?
C10 C26 C37 112.7(6) . . ?
C10 C26 C18 112.2(5) . . ?
C37 C26 C18 112.3(5) . . ?
C16 C27 C24 111.9(5) . . ?
C16 C27 C41 112.6(5) . . ?
C24 C27 C41 113.3(5) . . ?
C6 C28 C29 113.0(5) . . ?
C6 C28 C22 109.9(5) . . ?
C29 C28 C22 113.8(5) . . ?
C28 C29 C30 114.5(5) . . ?
C32 C30 C31 109.4(7) . . ?
C32 C30 C29 112.2(7) . . ?
C31 C30 C29 109.2(6) . . ?
C34 C33 C25 115.9(7) . . ?
C35 C34 C33 110.8(8) . . ?
C35 C34 C36 111.7(8) . . ?
C33 C34 C36 108.7(12) . . ?
C26 C37 C38 113.3(6) . . ?
C40 C38 C39 109.9(8) . . ?
C40 C38 C37 113.7(7) . . ?
C39 C38 C37 110.4(7) . . ?
C42 C41 C27 115.0(5) . . ?
C44 C42 C41 112.6(5) . . ?
C44 C42 C43 110.0(5) . . ?
C41 C42 C43 109.3(5) . . ?
C48B C49 C50 123.6(11) . . ?
C48A C49 C50 111.6(8) . . ?
N3 C50 C49 112.4(6) . . ?
N2 C51 C8 125.6(7) . . ?
N2 C52 C53 114.6(7) . . ?
C54 C53 C52 112.1(7) . . ?
C53 C54 C55 114.8(7) . . ?
C56 C55 C54 111.8(8) . . ?
C55 C56 N4 113.3(6) . . ?
N3 C57 C14 124.9(6) 2_566 . ?
N4 C58 C20 125.2(7) 2_566 . ?
N1A C45A C2 117.3(12) . . ?
C45A N1A C46A 122.8(11) . . ?
N1A C46A C47A 110.6(10) . . ?
C46A C47A C48A 113.9(10) . . ?
C49 C48A C47A 113.8(10) . . ?
C2 C45B N1B 135(2) . . ?
C45B N1B C46B 124(2) . . ?
N1B C46B C47B 110.6(16) . . ?
C46B C47B C48B 112.4(16) . . ?
C49 C48B C47B 119.8(17) . . ?
 
_refine_diff_density_max    1.185
_refine_diff_density_min   -0.411
_refine_diff_density_rms    0.109




#===END


 
data_CPOC-104-SQ
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C120 H155 Cl0 N8 O16' 
_chemical_formula_weight          1965.51

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.3639   0.7018
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    20.5854(7)
_cell_length_b                    21.7127(9)
_cell_length_c                    34.6706(11)
_cell_angle_alpha                 90
_cell_angle_beta                  104.350(4)
_cell_angle_gamma                 90
_cell_volume                      15013.0(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used   6310
_cell_measurement_theta_min     4.0330
_cell_measurement_theta_max     58.8410
 
_exptl_crystal_description       block 
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.870          
_exptl_crystal_F_000              4236
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu     0.457
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min                   0.81449
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.5594
_diffrn_reflns_number             53263
_diffrn_reflns_av_unetI/netI      0.0616
_diffrn_reflns_av_R_equivalents   0.0522
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        23
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -42
_diffrn_reflns_limit_l_max        42
_diffrn_reflns_theta_min          3.618
_diffrn_reflns_theta_max          72.412
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.959
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.959
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.959
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              28489
_reflns_number_gt                 13297
_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.
 
 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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_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)+(0.1873P)²+18.8166P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          28489
_refine_ls_number_parameters      1370
_refine_ls_number_restraints      127
_refine_ls_R_factor_all           0.1779
_refine_ls_R_factor_gt            0.1122
_refine_ls_wR_factor_ref          0.3981
_refine_ls_wR_factor_gt           0.3387
_refine_ls_goodness_of_fit_ref    1.026
_refine_ls_restrained_S_all       1.038
_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
O1 O 0.4230(2) 0.8410(2) 0.45639(12) 0.0717(10) Uani 1 1 d . . . . .
H1O H 0.409198 0.803344 0.459341 0.107 Uiso 1 1 d R U . . .
O2 O 0.54735(18) 0.93862(18) 0.37536(11) 0.0637(9) Uani 1 1 d . . . . .
O3 O 0.61919(18) 0.90875(17) 0.32610(11) 0.0654(10) Uani 1 1 d . . . . .
H3O H 0.593548 0.918750 0.342007 0.098 Uiso 1 1 d R U . . .
O4 O 0.68612(19) 0.71512(18) 0.28683(10) 0.0624(9) Uani 1 1 d . . . . .
O5 O 0.66913(19) 0.60280(18) 0.31098(10) 0.0657(10) Uani 1 1 d . . . . .
H5O H 0.669290 0.635795 0.296266 0.099 Uiso 1 1 d R U . . .
O6 O 0.5365(2) 0.50115(19) 0.38534(11) 0.0691(10) Uani 1 1 d . . . . .
O7 O 0.4595(2) 0.5331(2) 0.42958(12) 0.0752(11) Uani 1 1 d . . . . .
H7O H 0.481444 0.520874 0.412171 0.113 Uiso 1 1 d R U . . .
O8 O 0.3927(2) 0.72645(19) 0.46818(12) 0.0723(11) Uani 1 1 d . . . . .
O9 O 0.9310(2) 0.8918(3) 0.65466(18) 0.1135(19) Uani 1 1 d . . . . .
O10 O 1.0703(2) 0.8219(2) 0.57346(14) 0.0836(13) Uani 1 1 d . . . . .
H10 H 1.074466 0.784613 0.564386 0.125 Uiso 1 1 d R U . . .
O11 O 1.0973(2) 0.71330(19) 0.55164(12) 0.0736(11) Uani 1 1 d . . . . .
O12 O 1.02217(19) 0.50996(18) 0.56814(12) 0.0686(10) Uani 1 1 d . . . . .
H12O H 0.992781 0.497253 0.581006 0.103 Uiso 1 1 d R U . . .
O13 O 0.94477(19) 0.4636(2) 0.60854(11) 0.0683(10) Uani 1 1 d . . . . .
O14 O 0.8095(2) 0.5407(3) 0.69018(13) 0.0923(14) Uani 1 1 d . . . . .
H14 H 0.806832 0.573101 0.704957 0.138 Uiso 1 1 d R U . . .
O15 O 0.7886(3) 0.6491(3) 0.71718(15) 0.1065(18) Uani 1 1 d . . . . .
O16 O 0.8545(3) 0.8519(3) 0.69722(16) 0.1105(19) Uani 1 1 d . . . . .
H16 H 0.883026 0.867091 0.684516 0.166 Uiso 1 1 d R U . . .
N1 N 0.5643(2) 0.9641(2) 0.45032(14) 0.0660(12) Uani 1 1 d . . . . .
H1N H 0.574750 0.971755 0.428280 0.079 Uiso 1 1 calc R U . . .
N2 N 0.7701(2) 0.8017(2) 0.31209(13) 0.0643(12) Uani 1 1 d . . . . .
H2N H 0.762987 0.763748 0.305328 0.077 Uiso 1 1 calc R U . . .
N3 N 0.6611(3) 0.4762(2) 0.39236(13) 0.0707(13) Uani 1 1 d . . . . .
H3N H 0.624871 0.472093 0.400252 0.085 Uiso 1 1 calc R U . . .
N4 N 0.4431(3) 0.6424(3) 0.51858(16) 0.0936(18) Uani 1 1 d . . . . .
H4N H 0.431588 0.680295 0.513810 0.112 Uiso 1 1 calc R U . . .
N5 N 0.9243(3) 0.9359(3) 0.5860(2) 0.115(2) Uani 1 1 d . . . . .
H5N H 0.910598 0.933922 0.607421 0.138 Uiso 1 1 calc R U . . .
N6 N 1.0387(2) 0.6477(2) 0.49283(14) 0.0701(13) Uani 1 1 d . . . . .
H6N H 1.060900 0.680329 0.502051 0.084 Uiso 1 1 calc R U . . .
N7 N 0.8231(2) 0.4291(2) 0.60163(13) 0.0690(13) Uani 1 1 d . . . . .
H7N H 0.858191 0.429019 0.592327 0.083 Uiso 1 1 calc R U . . .
N8 N 0.7037(3) 0.7383(5) 0.69672(18) 0.122(3) Uani 1 1 d . . . . .
H8N H 0.711618 0.699795 0.701522 0.147 Uiso 1 1 calc R U . . .
C1 C 0.4337(3) 0.8467(3) 0.41996(17) 0.0638(14) Uani 1 1 d . . . . .
C2 C 0.3998(3) 0.8151(3) 0.38678(17) 0.0619(14) Uani 1 1 d . . . . .
C3 C 0.4168(3) 0.8250(3) 0.35087(17) 0.0600(13) Uani 1 1 d . . . . .
H3 H 0.394534 0.801500 0.329197 0.072 Uiso 1 1 calc R U . . .
C4 C 0.4631(3) 0.8663(3) 0.34455(16) 0.0595(13) Uani 1 1 d . . . . .
C5 C 0.5002(3) 0.8998(3) 0.37819(16) 0.0608(14) Uani 1 1 d . . . . .
C6 C 0.4848(3) 0.8897(3) 0.41615(17) 0.0619(14) Uani 1 1 d . . . . .
C7 C 0.6004(3) 0.8529(3) 0.30955(14) 0.0578(13) Uani 1 1 d . . . . .
C8 C 0.5338(3) 0.8344(2) 0.29885(15) 0.0555(12) Uani 1 1 d . . . . .
C9 C 0.5209(3) 0.7747(2) 0.28301(13) 0.0535(12) Uani 1 1 d . . . . .
H9 H 0.476365 0.762029 0.275718 0.064 Uiso 1 1 calc R U . . .
C10 C 0.5685(3) 0.7336(2) 0.27737(13) 0.0544(12) Uani 1 1 d . . . . .
C11 C 0.6374(3) 0.7523(3) 0.28913(14) 0.0560(12) Uani 1 1 d . . . . .
C12 C 0.6516(3) 0.8142(3) 0.30384(14) 0.0560(13) Uani 1 1 d . . . . .
C13 C 0.6067(3) 0.5947(3) 0.31765(16) 0.0610(13) Uani 1 1 d . . . . .
C14 C 0.5507(3) 0.6242(3) 0.29608(14) 0.0579(13) Uani 1 1 d . . . . .
C15 C 0.4898(3) 0.6127(3) 0.30650(15) 0.0603(14) Uani 1 1 d . . . . .
H15 H 0.451989 0.634197 0.292857 0.072 Uiso 1 1 calc R U . . .
C16 C 0.4826(3) 0.5724(3) 0.33514(15) 0.0600(13) Uani 1 1 d . . . . .
C17 C 0.5389(3) 0.5407(3) 0.35712(15) 0.0626(14) Uani 1 1 d . . . . .
C18 C 0.6021(3) 0.5523(3) 0.34745(15) 0.0599(13) Uani 1 1 d . . . . .
C19 C 0.4297(3) 0.5880(3) 0.41771(18) 0.0680(15) Uani 1 1 d . . . . .
C20 C 0.4071(3) 0.6038(3) 0.37805(16) 0.0630(14) Uani 1 1 d . . . . .
C21 C 0.3785(3) 0.6631(3) 0.37086(16) 0.0645(15) Uani 1 1 d . . . . .
H21 H 0.362513 0.674971 0.344424 0.077 Uiso 1 1 calc R U . . .
C22 C 0.3722(3) 0.7043(3) 0.39907(18) 0.0661(15) Uani 1 1 d . . . . .
C23 C 0.3964(3) 0.6883(3) 0.43967(18) 0.0692(15) Uani 1 1 d . . . . .
C24 C 0.4235(3) 0.6295(3) 0.44920(17) 0.0684(15) Uani 1 1 d . . . . .
C25 C 0.5185(3) 0.9223(3) 0.45009(17) 0.0617(14) Uani 1 1 d . . . . .
H25 H 0.507606 0.913579 0.474000 0.074 Uiso 1 1 calc R U . . .
C26 C 0.7187(3) 0.8356(3) 0.31466(15) 0.0603(13) Uani 1 1 d . . . . .
H26 H 0.726618 0.875720 0.324059 0.072 Uiso 1 1 calc R U . . .
C27 C 0.6611(3) 0.5179(3) 0.36632(15) 0.0640(14) Uani 1 1 d . . . . .
H27 H 0.700899 0.526365 0.359290 0.077 Uiso 1 1 calc R U . . .
C28 C 0.4466(3) 0.6091(3) 0.48876(18) 0.0769(17) Uani 1 1 d . . . . .
H28 H 0.465181 0.569866 0.493378 0.092 Uiso 1 1 calc R U . . .
C29 C 0.4778(3) 0.8765(3) 0.30446(15) 0.0580(13) Uani 1 1 d . . . . .
H29 H 0.495254 0.918583 0.304980 0.070 Uiso 1 1 calc R U . . .
C30 C 0.5546(3) 0.6682(3) 0.26219(14) 0.0588(13) Uani 1 1 d . . . . .
H30 H 0.593805 0.655411 0.252959 0.071 Uiso 1 1 calc R U . . .
C31 C 0.4154(3) 0.5600(3) 0.34553(16) 0.0666(15) Uani 1 1 d . . . . .
H31 H 0.418190 0.518397 0.356790 0.080 Uiso 1 1 calc R U . . .
C32 C 0.3434(3) 0.7694(3) 0.38901(18) 0.0683(15) Uani 1 1 d . . . . .
H32 H 0.326320 0.782492 0.411690 0.082 Uiso 1 1 calc R U . . .
C33 C 0.4150(3) 0.8742(3) 0.26924(17) 0.0713(16) Uani 1 1 d . . . . .
H33A H 0.393579 0.834478 0.269540 0.086 Uiso 1 1 calc R U . . .
H33B H 0.383779 0.905419 0.273445 0.086 Uiso 1 1 calc R U . . .
C34 C 0.4272(4) 0.8838(3) 0.22860(19) 0.083(2) Uani 1 1 d . . . . .
H34 H 0.452239 0.848378 0.222289 0.100 Uiso 1 1 calc R U . . .
C35 C 0.4676(4) 0.9426(3) 0.2265(2) 0.092(2) Uani 1 1 d . . . . .
H35A H 0.469781 0.949479 0.199475 0.137 Uiso 1 1 calc R U . . .
H35B H 0.512171 0.937989 0.243105 0.137 Uiso 1 1 calc R U . . .
H35C H 0.446147 0.977025 0.235520 0.137 Uiso 1 1 calc R U . . .
C36 C 0.3595(5) 0.8873(4) 0.1977(3) 0.143(5) Uani 1 1 d . . . . .
H36A H 0.366858 0.896254 0.171987 0.215 Uiso 1 1 calc R U . . .
H36B H 0.332627 0.919211 0.205030 0.215 Uiso 1 1 calc R U . . .
H36C H 0.336656 0.848530 0.196688 0.215 Uiso 1 1 calc R U . . .
C37 C 0.4942(3) 0.6620(3) 0.22626(15) 0.0653(14) Uani 1 1 d . . . . .
H37A H 0.499362 0.690804 0.205827 0.078 Uiso 1 1 calc R U . . .
H37B H 0.453858 0.673279 0.234297 0.078 Uiso 1 1 calc R U . . .
C38 C 0.4854(3) 0.5966(3) 0.20844(17) 0.0724(16) Uani 1 1 d . . . . .
H38 H 0.478162 0.568909 0.229283 0.087 Uiso 1 1 calc R U . . .
C39 C 0.5486(4) 0.5742(4) 0.1968(2) 0.101(2) Uani 1 1 d . . . . .
H39A H 0.542753 0.532036 0.188325 0.152 Uiso 1 1 calc R U . . .
H39B H 0.586481 0.577516 0.219267 0.152 Uiso 1 1 calc R U . . .
H39C H 0.555983 0.599105 0.175359 0.152 Uiso 1 1 calc R U . . .
C40 C 0.4248(4) 0.5925(4) 0.1745(2) 0.113(3) Uani 1 1 d . . . . .
H40A H 0.427106 0.623446 0.155101 0.169 Uiso 1 1 calc R U . . .
H40B H 0.385329 0.598962 0.184052 0.169 Uiso 1 1 calc R U . . .
H40C H 0.422804 0.552500 0.162489 0.169 Uiso 1 1 calc R U . . .
C41 C 0.3548(3) 0.5603(3) 0.30874(17) 0.0698(16) Uani 1 1 d . . . . .
H41A H 0.314554 0.552642 0.317751 0.084 Uiso 1 1 calc R U . . .
H41B H 0.350821 0.601287 0.297220 0.084 Uiso 1 1 calc R U . . .
C42 C 0.3570(4) 0.5145(3) 0.27628(18) 0.0797(18) Uani 1 1 d . . . . .
H42 H 0.396118 0.524108 0.265988 0.096 Uiso 1 1 calc R U . . .
C43 C 0.2952(5) 0.5186(4) 0.2421(2) 0.111(3) Uani 1 1 d . . . . .
H43A H 0.289108 0.560362 0.232860 0.167 Uiso 1 1 calc R U . . .
H43B H 0.256756 0.505621 0.250967 0.167 Uiso 1 1 calc R U . . .
H43C H 0.300594 0.492388 0.220812 0.167 Uiso 1 1 calc R U . . .
C44 C 0.3652(4) 0.4471(3) 0.2928(2) 0.094(2) Uani 1 1 d . . . . .
H44A H 0.367391 0.419126 0.271715 0.141 Uiso 1 1 calc R U . . .
H44B H 0.327502 0.436725 0.303216 0.141 Uiso 1 1 calc R U . . .
H44C H 0.405679 0.444062 0.313621 0.141 Uiso 1 1 calc R U . . .
C45 C 0.2841(3) 0.7727(3) 0.3525(2) 0.0797(18) Uani 1 1 d . . . . .
H45A H 0.298460 0.756644 0.329838 0.096 Uiso 1 1 calc R U . . .
H45B H 0.249105 0.745733 0.356945 0.096 Uiso 1 1 calc R U . . .
C46 C 0.2544(3) 0.8360(4) 0.3419(2) 0.091(2) Uani 1 1 d . . . . .
H46 H 0.290473 0.862362 0.337418 0.109 Uiso 1 1 calc R U . . .
C47 C 0.2005(4) 0.8345(4) 0.3033(3) 0.120(3) Uani 1 1 d . . . . .
H47A H 0.215341 0.809710 0.284243 0.180 Uiso 1 1 calc R U . . .
H47B H 0.191825 0.875679 0.293221 0.180 Uiso 1 1 calc R U . . .
H47C H 0.160251 0.817316 0.308037 0.180 Uiso 1 1 calc R U . . .
C48 C 0.2301(4) 0.8647(4) 0.3766(2) 0.108(3) Uani 1 1 d . . . . .
H48A H 0.216289 0.906435 0.370165 0.162 Uiso 1 1 calc R U . . .
H48B H 0.266073 0.864103 0.400330 0.162 Uiso 1 1 calc R U . . .
H48C H 0.192995 0.841329 0.380969 0.162 Uiso 1 1 calc R U . . .
C49 C 0.9810(3) 0.8571(4) 0.6507(2) 0.091(2) Uani 1 1 d . . . . .
C50 C 1.0153(3) 0.8189(3) 0.6822(2) 0.086(2) Uani 1 1 d . . . . .
C51 C 1.0656(3) 0.7807(3) 0.6741(2) 0.0791(19) Uani 1 1 d . . . . .
H51 H 1.086847 0.753731 0.694089 0.095 Uiso 1 1 calc R U . . .
C52 C 1.0862(3) 0.7800(3) 0.63878(19) 0.0681(16) Uani 1 1 d . . . . .
C53 C 1.0553(3) 0.8179(3) 0.6094(2) 0.0786(18) Uani 1 1 d . . . . .
C54 C 1.0018(3) 0.8584(3) 0.6141(2) 0.087(2) Uani 1 1 d . . . . .
C55 C 1.0916(3) 0.6684(3) 0.57577(18) 0.0629(14) Uani 1 1 d . . . . .
C56 C 1.1133(3) 0.6746(3) 0.61707(17) 0.0640(14) Uani 1 1 d . . . . .
C57 C 1.1044(3) 0.6261(3) 0.64034(18) 0.0649(15) Uani 1 1 d . . . . .
H57 H 1.118666 0.631148 0.667787 0.078 Uiso 1 1 calc R U . . .
C58 C 1.0753(2) 0.5687(3) 0.62609(17) 0.0650(15) Uani 1 1 d . . . . .
C59 C 1.0525(2) 0.5625(3) 0.58596(17) 0.0634(14) Uani 1 1 d . . . . .
C60 C 1.0607(3) 0.6101(3) 0.55968(17) 0.0627(14) Uani 1 1 d . . . . .
C61 C 0.9405(3) 0.4958(3) 0.63966(15) 0.0640(14) Uani 1 1 d . . . . .
C62 C 0.9967(3) 0.5256(3) 0.66413(17) 0.0705(16) Uani 1 1 d . . . . .
C63 C 0.9892(3) 0.5594(3) 0.69578(17) 0.0766(17) Uani 1 1 d . . . . .
H63 H 1.026910 0.578861 0.711344 0.092 Uiso 1 1 calc R U . . .
C64 C 0.9267(3) 0.5668(4) 0.70668(17) 0.0829(19) Uani 1 1 d . . . . .
C65 C 0.8729(3) 0.5379(3) 0.68316(17) 0.0749(17) Uani 1 1 d . . . . .
C66 C 0.8780(3) 0.5014(3) 0.65013(17) 0.0754(17) Uani 1 1 d . . . . .
C67 C 0.8354(4) 0.6897(5) 0.71889(19) 0.094(2) Uani 1 1 d . . . . .
C68 C 0.9053(4) 0.6713(4) 0.73098(19) 0.092(2) Uani 1 1 d . . . . .
C69 C 0.9533(4) 0.7149(4) 0.73138(18) 0.092(2) Uani 1 1 d . . . . .
H69 H 0.997990 0.702677 0.738965 0.110 Uiso 1 1 calc R U . . .
C70 C 0.9396(4) 0.7764(4) 0.7212(2) 0.096(3) Uani 1 1 d . . . . .
C71 C 0.8735(4) 0.7957(5) 0.7087(2) 0.099(3) Uani 1 1 d . . . . .
C72 C 0.8219(4) 0.7531(5) 0.7094(2) 0.098(3) Uani 1 1 d . . . . .
C73 C 0.9712(4) 0.8981(4) 0.5826(3) 0.103(3) Uani 1 1 d . . . . .
H73 H 0.985036 0.897024 0.559039 0.123 Uiso 1 1 calc R U . . .
C74 C 1.0350(3) 0.6044(3) 0.51934(18) 0.0691(15) Uani 1 1 d . . . . .
H74 H 1.013481 0.567706 0.509880 0.083 Uiso 1 1 calc R U . . .
C75 C 0.8226(3) 0.4671(3) 0.63038(16) 0.0694(16) Uani 1 1 d . . . . .
H75 H 0.782903 0.471650 0.638289 0.083 Uiso 1 1 calc R U . . .
C76 C 0.7529(4) 0.7714(5) 0.6986(2) 0.112(3) Uani 1 1 d . . . . .
H76 H 0.744342 0.812776 0.692437 0.135 Uiso 1 1 calc R U . . .
C77 C 1.1430(3) 0.7368(3) 0.6336(2) 0.0723(17) Uani 1 1 d . . . . .
H77 H 1.162874 0.755421 0.613433 0.087 Uiso 1 1 calc R U . . .
C78 C 1.0657(3) 0.5184(3) 0.65477(18) 0.0726(16) Uani 1 1 d . . . . .
H78 H 1.064772 0.479177 0.640700 0.087 Uiso 1 1 calc R U . . .
C79 C 0.9223(3) 0.6056(4) 0.74223(19) 0.090(2) Uani 1 1 d . . . . .
H79 H 0.884991 0.589082 0.751984 0.107 Uiso 1 1 calc R U . . .
C80 C 0.9966(4) 0.8211(4) 0.7207(2) 0.101(3) Uani 1 1 d . . . . .
H80 H 0.978961 0.862507 0.722843 0.121 Uiso 1 1 calc R U . . .
C81 C 1.1999(3) 0.7290(3) 0.6717(2) 0.0785(18) Uani 1 1 d . . . . .
H81A H 1.181315 0.712767 0.692743 0.094 Uiso 1 1 calc R U . . .
H81B H 1.232066 0.699312 0.666719 0.094 Uiso 1 1 calc R U . . .
C82 C 1.2362(4) 0.7897(4) 0.6857(3) 0.125(4) Uani 1 1 d . . . . .
H82 H 1.204208 0.822393 0.687328 0.150 Uiso 1 1 calc R U . . .
C83 C 1.2774(9) 0.8063(8) 0.6564(5) 0.244(8) Uani 1 1 d . U . . .
H83A H 1.319044 0.784230 0.663072 0.366 Uiso 1 1 calc R U . . .
H83B H 1.286180 0.849812 0.657710 0.366 Uiso 1 1 calc R U . . .
H83C H 1.252926 0.795541 0.629936 0.366 Uiso 1 1 calc R U . . .
C84 C 1.2873(4) 0.7807(5) 0.7257(3) 0.126(3) Uani 1 1 d . . . . .
H84A H 1.316299 0.746809 0.723756 0.189 Uiso 1 1 calc R U . . .
H84B H 1.264208 0.772220 0.745981 0.189 Uiso 1 1 calc R U . . .
H84C H 1.313570 0.817502 0.732410 0.189 Uiso 1 1 calc R U . . .
C85 C 1.1230(4) 0.5140(4) 0.6928(2) 0.096(2) Uani 1 1 d . . . . .
C89 C 0.9870(5) 0.6007(4) 0.7778(2) 0.113(3) Uani 1 1 d . . . . .
H89A H 1.025204 0.614614 0.768432 0.135 Uiso 1 1 calc R U . . .
H89B H 0.982024 0.628874 0.798639 0.135 Uiso 1 1 calc R U . . .
C90 C 1.0020(4) 0.5408(4) 0.7951(2) 0.102(2) Uani 1 1 d . . . . .
H90 H 1.002143 0.510976 0.773859 0.122 Uiso 1 1 calc R U . . .
C91 C 0.9472(7) 0.5204(7) 0.8183(4) 0.194(6) Uani 1 1 d . U . . .
H91A H 0.947013 0.549271 0.839199 0.291 Uiso 1 1 calc R U . . .
H91B H 0.958019 0.480106 0.829493 0.291 Uiso 1 1 calc R U . . .
H91C H 0.903680 0.519454 0.800042 0.291 Uiso 1 1 calc R U . . .
C92 C 1.0710(6) 0.5404(5) 0.8248(3) 0.172(6) Uani 1 1 d . . . . .
H92A H 1.104678 0.552393 0.811491 0.258 Uiso 1 1 calc R U . . .
H92B H 1.080582 0.499681 0.835561 0.258 Uiso 1 1 calc R U . . .
H92C H 1.070853 0.568764 0.846021 0.258 Uiso 1 1 calc R U . . .
C93 C 1.0569(4) 0.8126(5) 0.7575(2) 0.118(3) Uani 1 1 d . . . . .
C97 C 0.5989(3) 0.9989(3) 0.48573(19) 0.0776(17) Uani 1 1 d . . . . .
H97A H 0.584785 0.983596 0.508661 0.093 Uiso 1 1 calc R U . . .
H97B H 0.586102 1.041884 0.482152 0.093 Uiso 1 1 calc R U . . .
C98 C 0.6741(4) 0.9937(4) 0.4936(3) 0.115(3) Uani 1 1 d . . . . .
H98A H 0.687137 0.951223 0.499736 0.138 Uiso 1 1 calc R U . . .
H98B H 0.687666 1.005113 0.469724 0.138 Uiso 1 1 calc R U . . .
C99 C 0.7092(4) 1.0329(5) 0.5265(3) 0.119(3) Uani 1 1 d . . . . .
H99A H 0.699373 1.018294 0.550902 0.142 Uiso 1 1 calc R U . . .
H99B H 0.691738 1.074480 0.521838 0.142 Uiso 1 1 calc R U . . .
C100 C 0.7848(4) 1.0351(5) 0.5325(4) 0.135(4) Uani 1 1 d . . . . .
H10A H 0.795645 1.039460 0.506986 0.161 Uiso 1 1 calc R U . . .
H10B H 0.802954 1.070355 0.548840 0.161 Uiso 1 1 calc R U . . .
C101 C 0.8137(5) 0.9802(5) 0.5514(4) 0.150(5) Uani 1 1 d . . . . .
H10C H 0.794523 0.945001 0.535332 0.181 Uiso 1 1 calc R U . . .
H10D H 0.803477 0.976415 0.577117 0.181 Uiso 1 1 calc R U . . .
C102 C 0.8934(4) 0.9805(4) 0.5572(3) 0.126(3) Uani 1 1 d . . . . .
H10E H 0.903879 0.971543 0.531966 0.151 Uiso 1 1 calc R U . . .
H10F H 0.911008 1.021082 0.565766 0.151 Uiso 1 1 calc R U . . .
C103 C 0.8394(3) 0.8251(3) 0.32012(18) 0.0737(17) Uani 1 1 d . . . . .
H10G H 0.845485 0.858093 0.339560 0.088 Uiso 1 1 calc R U . . .
H10H H 0.847993 0.841432 0.295831 0.088 Uiso 1 1 calc R U . . .
C104 C 0.8874(3) 0.7737(4) 0.3357(2) 0.0830(19) Uani 1 1 d . . . . .
H10I H 0.873540 0.737436 0.319416 0.100 Uiso 1 1 calc R U . . .
H10J H 0.931572 0.785345 0.333088 0.100 Uiso 1 1 calc R U . . .
C105 C 0.8919(3) 0.7577(3) 0.37806(19) 0.0813(18) Uani 1 1 d . . . . .
H10K H 0.848134 0.744600 0.380668 0.098 Uiso 1 1 calc R U . . .
H10L H 0.904594 0.794115 0.394407 0.098 Uiso 1 1 calc R U . . .
C106 C 0.9429(3) 0.7065(3) 0.39329(19) 0.0814(19) Uani 1 1 d . . . . .
H10M H 0.925168 0.668130 0.380593 0.098 Uiso 1 1 calc R U . . .
H10N H 0.983678 0.715736 0.385188 0.098 Uiso 1 1 calc R U . . .
C107 C 0.9602(3) 0.6974(3) 0.43722(17) 0.0725(16) Uani 1 1 d . . . . .
H10O H 0.919577 0.688205 0.445497 0.087 Uiso 1 1 calc R U . . .
H10P H 0.978480 0.735528 0.450072 0.087 Uiso 1 1 calc R U . . .
C108 C 1.0101(3) 0.6465(3) 0.45095(17) 0.0697(15) Uani 1 1 d . . . . .
H10Q H 0.987990 0.607173 0.443792 0.084 Uiso 1 1 calc R U . . .
H10R H 1.045650 0.649966 0.437235 0.084 Uiso 1 1 calc R U . . .
C109 C 0.7162(3) 0.4347(3) 0.41006(17) 0.0757(17) Uani 1 1 d . . . . .
H10S H 0.756110 0.446958 0.401874 0.091 Uiso 1 1 calc R U . . .
H10T H 0.704763 0.393072 0.400674 0.091 Uiso 1 1 calc R U . . .
C110 C 0.7303(3) 0.4362(3) 0.45457(16) 0.0679(15) Uani 1 1 d . . . . .
H11A H 0.688480 0.434044 0.462661 0.082 Uiso 1 1 calc R U . . .
H11B H 0.752548 0.474435 0.464523 0.082 Uiso 1 1 calc R U . . .
C111 C 0.7750(3) 0.3816(3) 0.47200(17) 0.0740(17) Uani 1 1 d . . . . .
H11C H 0.749690 0.343629 0.465611 0.089 Uiso 1 1 calc R U . . .
H11D H 0.812823 0.379678 0.460042 0.089 Uiso 1 1 calc R U . . .
C112 C 0.8005(3) 0.3872(4) 0.51706(19) 0.0835(19) Uani 1 1 d . . . . .
H11E H 0.829992 0.422667 0.523037 0.100 Uiso 1 1 calc R U . . .
H11F H 0.826809 0.350962 0.527085 0.100 Uiso 1 1 calc R U . . .
C113 C 0.7450(3) 0.3941(3) 0.53893(17) 0.0742(17) Uani 1 1 d . . . . .
H11G H 0.725040 0.434648 0.533340 0.089 Uiso 1 1 calc R U . . .
H11H H 0.710376 0.363905 0.528592 0.089 Uiso 1 1 calc R U . . .
C114 C 0.7688(3) 0.3861(3) 0.58351(17) 0.0743(17) Uani 1 1 d . . . . .
H11I H 0.731325 0.392617 0.595380 0.089 Uiso 1 1 calc R U . . .
H11J H 0.784470 0.344226 0.589335 0.089 Uiso 1 1 calc R U . . .
C115 C 0.4564(5) 0.6225(5) 0.5592(2) 0.121(3) Uani 1 1 d D U . . .
H11K H 0.475025 0.581258 0.561482 0.146 Uiso 1 1 calc R U . . .
H11L H 0.414866 0.621328 0.567601 0.146 Uiso 1 1 calc R U . . .
C116 C 0.5027(6) 0.6635(6) 0.5846(3) 0.157(4) Uani 1 1 d D U . . .
H11M H 0.492743 0.705346 0.575247 0.188 Uiso 1 1 calc R U . . .
H11N H 0.547737 0.653862 0.582495 0.188 Uiso 1 1 calc R U . . .
C117 C 0.5010(8) 0.6601(6) 0.6275(3) 0.188(5) Uani 1 1 d D U . . .
H11O H 0.533808 0.631016 0.642020 0.225 Uiso 1 1 calc R U . . .
H11P H 0.456824 0.648425 0.630188 0.225 Uiso 1 1 calc R U . . .
C118 C 0.5190(5) 0.7281(6) 0.6422(4) 0.178(4) Uani 1 1 d D U . . .
H11Q H 0.499754 0.757843 0.621673 0.214 Uiso 1 1 calc R U . . .
H11R H 0.503804 0.737126 0.665958 0.214 Uiso 1 1 calc R U . . .
C119 C 0.5911(4) 0.7274(6) 0.6505(3) 0.135(3) Uani 1 1 d D U . . .
H11S H 0.603388 0.746253 0.627931 0.162 Uiso 1 1 calc R U . . .
H11T H 0.604925 0.684603 0.651139 0.162 Uiso 1 1 calc R U . . .
C120 C 0.6322(4) 0.7573(5) 0.6871(2) 0.119(3) Uani 1 1 d D U . . .
H12A H 0.629594 0.801594 0.683569 0.143 Uiso 1 1 calc R U . . .
H12B H 0.613462 0.747065 0.709311 0.143 Uiso 1 1 calc R U . . .
C86A C 1.1322(5) 0.4635(5) 0.7168(3) 0.060(3) Uani 0.5 1 d . . P A 1
H86A H 1.097052 0.467508 0.731234 0.072 Uiso 0.5 1 calc R U P A 1
C87A C 1.1207(9) 0.4018(8) 0.6991(5) 0.098(5) Uani 0.5 1 d . . P A 1
H87A H 1.151141 0.394788 0.682522 0.147 Uiso 0.5 1 calc R U P A 1
H87B H 1.075423 0.398751 0.683270 0.147 Uiso 0.5 1 calc R U P A 1
H87C H 1.128199 0.371400 0.719838 0.147 Uiso 0.5 1 calc R U P A 1
C88A C 1.1977(7) 0.4643(8) 0.7503(4) 0.081(4) Uani 0.5 1 d . . P A 1
H88A H 1.233863 0.448521 0.740252 0.122 Uiso 0.5 1 calc R U P A 1
H88B H 1.192281 0.439174 0.772056 0.122 Uiso 0.5 1 calc R U P A 1
H88C H 1.207684 0.505845 0.759400 0.122 Uiso 0.5 1 calc R U P A 1
C94A C 1.1065(9) 0.8561(9) 0.7656(5) 0.105(6) Uani 0.5 1 d . . P B 1
C95A C 1.0899(16) 0.9036(15) 0.7624(9) 0.198(12) Uani 0.5 1 d . U P B 1
H95A H 1.044320 0.912575 0.754522 0.238 Uiso 0.5 1 calc R U P B 1
H95B H 1.121145 0.935327 0.767466 0.238 Uiso 0.5 1 calc R U P B 1
C96A C 1.1609(8) 0.8485(9) 0.8042(5) 0.114(6) Uani 0.5 1 d . . P B 1
H96A H 1.190914 0.816108 0.801138 0.171 Uiso 0.5 1 calc R U P B 1
H96B H 1.140552 0.838370 0.825522 0.171 Uiso 0.5 1 calc R U P B 1
H96C H 1.185495 0.886335 0.810367 0.171 Uiso 0.5 1 calc R U P B 1
C86B C 1.1799(6) 0.4877(7) 0.6945(4) 0.076(3) Uani 0.5 1 d . . P A 2
H86B H 1.198507 0.502582 0.672760 0.092 Uiso 0.5 1 calc R U P A 2
C87B C 1.1724(8) 0.4148(8) 0.6923(6) 0.108(6) Uani 0.5 1 d . . P A 2
H87D H 1.126271 0.404169 0.681316 0.162 Uiso 0.5 1 calc R U P A 2
H87E H 1.187217 0.397817 0.718563 0.162 Uiso 0.5 1 calc R U P A 2
H87F H 1.199262 0.398478 0.675655 0.162 Uiso 0.5 1 calc R U P A 2
C88B C 1.2306(8) 0.4959(9) 0.7339(5) 0.110(6) Uani 0.5 1 d . . P A 2
H88D H 1.263739 0.463981 0.737120 0.165 Uiso 0.5 1 calc R U P A 2
H88E H 1.208310 0.493654 0.755091 0.165 Uiso 0.5 1 calc R U P A 2
H88F H 1.251911 0.535343 0.734417 0.165 Uiso 0.5 1 calc R U P A 2
C94B C 1.0388(7) 0.8198(8) 0.7934(4) 0.094(5) Uani 0.5 1 d . . P B 2
H94B H 1.009608 0.785694 0.796815 0.112 Uiso 0.5 1 calc R U P B 2
C95B C 1.0039(9) 0.8813(9) 0.7975(5) 0.126(7) Uani 0.5 1 d . . P B 2
H95C H 1.030407 0.914769 0.791604 0.189 Uiso 0.5 1 calc R U P B 2
H95D H 0.999058 0.885531 0.824194 0.189 Uiso 0.5 1 calc R U P B 2
H95E H 0.960437 0.882040 0.779189 0.189 Uiso 0.5 1 calc R U P B 2
C96B C 1.1033(9) 0.8191(13) 0.8282(5) 0.163(12) Uani 0.5 1 d . . P B 2
H96D H 1.090998 0.815817 0.853121 0.244 Uiso 0.5 1 calc R U P B 2
H96E H 1.127975 0.856556 0.827883 0.244 Uiso 0.5 1 calc R U P B 2
H96F H 1.130711 0.784567 0.825206 0.244 Uiso 0.5 1 calc R U P B 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 C1 1.341(7) . ?
O2 C5 1.307(7) . ?
O3 C7 1.356(6) . ?
O4 C11 1.305(7) . ?
O5 C13 1.372(7) . ?
O6 C17 1.312(6) . ?
O7 C19 1.357(7) . ?
O8 C23 1.305(7) . ?
O9 C49 1.310(8) . ?
O10 C53 1.360(9) . ?
O11 C55 1.309(7) . ?
O12 C59 1.371(7) . ?
O13 C61 1.307(7) . ?
O14 C65 1.387(8) . ?
O15 C67 1.297(10) . ?
O16 C71 1.313(10) . ?
N1 C25 1.308(7) . ?
N1 C97 1.466(7) . ?
N2 C26 1.309(7) . ?
N2 C103 1.474(7) . ?
N3 C27 1.279(7) . ?
N3 C109 1.459(8) . ?
N4 C28 1.280(8) . ?
N4 C115 1.433(9) . ?
N5 C73 1.295(10) . ?
N5 C102 1.422(11) . ?
N6 C74 1.331(8) . ?
N6 C108 1.426(7) . ?
N7 C75 1.296(8) . ?
N7 C114 1.473(8) . ?
N8 C76 1.230(12) . ?
N8 C120 1.484(9) . ?
C1 C2 1.372(8) . ?
C1 C6 1.437(8) . ?
C2 C3 1.391(8) . ?
C2 C32 1.542(8) . ?
C3 C4 1.365(8) . ?
C4 C5 1.426(7) . ?
C4 C29 1.511(8) . ?
C5 C6 1.445(8) . ?
C6 C25 1.401(8) . ?
C7 C8 1.388(7) . ?
C7 C12 1.400(8) . ?
C8 C9 1.407(7) . ?
C8 C29 1.520(8) . ?
C9 C10 1.375(8) . ?
C10 C11 1.436(7) . ?
C10 C30 1.517(7) . ?
C11 C12 1.441(8) . ?
C12 C26 1.417(7) . ?
C13 C14 1.368(8) . ?
C13 C18 1.406(8) . ?
C14 C15 1.410(8) . ?
C14 C30 1.531(7) . ?
C15 C16 1.359(8) . ?
C16 C17 1.400(8) . ?
C16 C31 1.537(8) . ?
C17 C18 1.443(8) . ?
C18 C27 1.437(8) . ?
C19 C20 1.381(8) . ?
C19 C24 1.447(9) . ?
C20 C21 1.413(8) . ?
C20 C31 1.517(8) . ?
C21 C22 1.355(8) . ?
C22 C23 1.415(8) . ?
C22 C32 1.539(9) . ?
C23 C24 1.400(9) . ?
C24 C28 1.408(8) . ?
C29 C33 1.543(7) . ?
C30 C37 1.532(7) . ?
C31 C41 1.548(7) . ?
C32 C45 1.527(8) . ?
C33 C34 1.505(9) . ?
C34 C36 1.535(9) . ?
C34 C35 1.536(9) . ?
C37 C38 1.541(8) . ?
C38 C40 1.491(8) . ?
C38 C39 1.533(10) . ?
C41 C42 1.512(9) . ?
C42 C43 1.511(9) . ?
C42 C44 1.565(10) . ?
C45 C46 1.514(10) . ?
C46 C47 1.510(10) . ?
C46 C48 1.545(11) . ?
C49 C50 1.412(10) . ?
C49 C54 1.435(11) . ?
C50 C51 1.407(9) . ?
C50 C80 1.480(11) . ?
C51 C52 1.393(9) . ?
C52 C53 1.341(9) . ?
C52 C77 1.543(8) . ?
C53 C54 1.450(10) . ?
C54 C73 1.410(10) . ?
C55 C56 1.397(8) . ?
C55 C60 1.464(8) . ?
C56 C57 1.367(9) . ?
C56 C77 1.533(8) . ?
C57 C58 1.417(8) . ?
C58 C59 1.360(8) . ?
C58 C78 1.523(9) . ?
C59 C60 1.415(9) . ?
C60 C74 1.373(8) . ?
C61 C62 1.410(8) . ?
C61 C66 1.427(9) . ?
C62 C63 1.359(9) . ?
C62 C78 1.542(9) . ?
C63 C64 1.437(9) . ?
C64 C65 1.356(9) . ?
C64 C79 1.515(9) . ?
C65 C66 1.418(9) . ?
C66 C75 1.391(9) . ?
C67 C72 1.426(13) . ?
C67 C68 1.451(10) . ?
C68 C69 1.366(12) . ?
C68 C79 1.496(11) . ?
C69 C70 1.393(11) . ?
C70 C71 1.387(9) . ?
C70 C80 1.526(12) . ?
C71 C72 1.411(13) . ?
C72 C76 1.433(10) . ?
C77 C81 1.542(8) . ?
C78 C85 1.538(8) . ?
C79 C89 1.581(9) . ?
C80 C93 1.554(9) . ?
C81 C82 1.532(10) . ?
C82 C83 1.519(19) . ?
C82 C84 1.532(11) . ?
C85 C86B 1.291(15) . ?
C85 C86A 1.362(13) . ?
C89 C90 1.434(12) . ?
C90 C92 1.534(11) . ?
C90 C91 1.603(15) . ?
C93 C94A 1.37(2) . ?
C93 C94B 1.394(17) . ?
C97 C98 1.508(10) . ?
C98 C99 1.463(10) . ?
C99 C100 1.519(12) . ?
C100 C101 1.417(13) . ?
C101 C102 1.604(13) . ?
C103 C104 1.500(9) . ?
C104 C105 1.489(9) . ?
C105 C106 1.531(9) . ?
C106 C107 1.489(8) . ?
C107 C108 1.504(9) . ?
C109 C110 1.498(8) . ?
C110 C111 1.530(8) . ?
C111 C112 1.525(8) . ?
C112 C113 1.527(9) . ?
C113 C114 1.511(8) . ?
C115 C116 1.434(10) . ?
C116 C117 1.498(12) . ?
C117 C118 1.577(12) . ?
C118 C119 1.442(11) . ?
C119 C120 1.487(9) . ?
C86A C87A 1.469(19) . ?
C86A C88A 1.547(16) . ?
C94A C95A 1.08(3) . ?
C94A C96A 1.528(17) . ?
C86B C88B 1.509(17) . ?
C86B C87B 1.59(2) . ?
C94B C95B 1.54(2) . ?
C94B C96B 1.557(19) . ?
 
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
C25 N1 C97 124.2(5) . . ?
C26 N2 C103 123.6(5) . . ?
C27 N3 C109 126.7(6) . . ?
C28 N4 C115 126.0(7) . . ?
C73 N5 C102 125.7(9) . . ?
C74 N6 C108 127.6(5) . . ?
C75 N7 C114 125.5(5) . . ?
C76 N8 C120 127.4(10) . . ?
O1 C1 C2 125.2(5) . . ?
O1 C1 C6 116.2(5) . . ?
C2 C1 C6 118.7(5) . . ?
C1 C2 C3 118.9(5) . . ?
C1 C2 C32 120.8(5) . . ?
C3 C2 C32 120.3(5) . . ?
C4 C3 C2 125.9(5) . . ?
C3 C4 C5 117.2(5) . . ?
C3 C4 C29 123.5(5) . . ?
C5 C4 C29 119.3(5) . . ?
O2 C5 C4 121.6(5) . . ?
O2 C5 C6 120.1(5) . . ?
C4 C5 C6 118.3(5) . . ?
C25 C6 C1 118.2(5) . . ?
C25 C6 C5 120.9(5) . . ?
C1 C6 C5 120.9(5) . . ?
O3 C7 C8 122.0(5) . . ?
O3 C7 C12 116.8(5) . . ?
C8 C7 C12 121.2(5) . . ?
C7 C8 C9 116.6(5) . . ?
C7 C8 C29 121.5(5) . . ?
C9 C8 C29 121.9(5) . . ?
C10 C9 C8 125.6(5) . . ?
C9 C10 C11 117.7(5) . . ?
C9 C10 C30 125.3(5) . . ?
C11 C10 C30 116.9(5) . . ?
O4 C11 C10 121.8(5) . . ?
O4 C11 C12 120.5(5) . . ?
C10 C11 C12 117.6(5) . . ?
C7 C12 C26 119.0(5) . . ?
C7 C12 C11 121.1(5) . . ?
C26 C12 C11 119.9(5) . . ?
C14 C13 O5 123.1(5) . . ?
C14 C13 C18 120.5(5) . . ?
O5 C13 C18 116.4(5) . . ?
C13 C14 C15 117.4(5) . . ?
C13 C14 C30 120.9(5) . . ?
C15 C14 C30 121.7(5) . . ?
C16 C15 C14 124.5(5) . . ?
C15 C16 C17 119.3(5) . . ?
C15 C16 C31 123.4(5) . . ?
C17 C16 C31 117.3(5) . . ?
O6 C17 C16 123.2(5) . . ?
O6 C17 C18 119.4(5) . . ?
C16 C17 C18 117.4(5) . . ?
C13 C18 C27 118.1(5) . . ?
C13 C18 C17 121.0(5) . . ?
C27 C18 C17 120.8(5) . . ?
O7 C19 C20 122.4(6) . . ?
O7 C19 C24 115.9(5) . . ?
C20 C19 C24 121.7(6) . . ?
C19 C20 C21 115.2(6) . . ?
C19 C20 C31 120.8(6) . . ?
C21 C20 C31 124.0(5) . . ?
C22 C21 C20 125.8(5) . . ?
C21 C22 C23 118.9(6) . . ?
C21 C22 C32 122.9(6) . . ?
C23 C22 C32 118.1(6) . . ?
O8 C23 C24 119.6(5) . . ?
O8 C23 C22 121.7(6) . . ?
C24 C23 C22 118.6(6) . . ?
C23 C24 C28 122.5(6) . . ?
C23 C24 C19 119.7(5) . . ?
C28 C24 C19 117.8(6) . . ?
N1 C25 C6 124.2(6) . . ?
N2 C26 C12 123.3(5) . . ?
N3 C27 C18 122.8(6) . . ?
N4 C28 C24 122.3(7) . . ?
C4 C29 C8 111.1(4) . . ?
C4 C29 C33 113.8(5) . . ?
C8 C29 C33 113.1(5) . . ?
C10 C30 C14 111.0(4) . . ?
C10 C30 C37 114.1(5) . . ?
C14 C30 C37 112.6(5) . . ?
C20 C31 C16 109.8(4) . . ?
C20 C31 C41 113.2(5) . . ?
C16 C31 C41 113.2(5) . . ?
C45 C32 C22 114.4(5) . . ?
C45 C32 C2 112.7(5) . . ?
C22 C32 C2 110.5(5) . . ?
C34 C33 C29 115.8(5) . . ?
C33 C34 C36 109.1(7) . . ?
C33 C34 C35 112.2(5) . . ?
C36 C34 C35 109.5(6) . . ?
C30 C37 C38 113.4(5) . . ?
C40 C38 C39 111.8(6) . . ?
C40 C38 C37 111.3(6) . . ?
C39 C38 C37 112.1(5) . . ?
C42 C41 C31 116.3(6) . . ?
C43 C42 C41 111.7(7) . . ?
C43 C42 C44 109.6(6) . . ?
C41 C42 C44 111.3(5) . . ?
C46 C45 C32 115.9(6) . . ?
C47 C46 C45 111.1(7) . . ?
C47 C46 C48 113.0(7) . . ?
C45 C46 C48 111.4(7) . . ?
O9 C49 C50 120.8(8) . . ?
O9 C49 C54 119.7(7) . . ?
C50 C49 C54 119.5(6) . . ?
C51 C50 C49 116.4(7) . . ?
C51 C50 C80 124.5(6) . . ?
C49 C50 C80 119.1(6) . . ?
C52 C51 C50 125.5(6) . . ?
C53 C52 C51 118.0(6) . . ?
C53 C52 C77 121.0(7) . . ?
C51 C52 C77 121.0(5) . . ?
C52 C53 O10 124.2(6) . . ?
C52 C53 C54 121.2(7) . . ?
O10 C53 C54 114.6(6) . . ?
C73 C54 C49 121.5(7) . . ?
C73 C54 C53 119.2(8) . . ?
C49 C54 C53 119.2(6) . . ?
O11 C55 C56 121.7(5) . . ?
O11 C55 C60 120.0(5) . . ?
C56 C55 C60 118.2(5) . . ?
C57 C56 C55 118.3(5) . . ?
C57 C56 C77 123.9(5) . . ?
C55 C56 C77 117.7(6) . . ?
C56 C57 C58 125.4(6) . . ?
C59 C58 C57 117.0(6) . . ?
C59 C58 C78 121.9(6) . . ?
C57 C58 C78 121.0(5) . . ?
C58 C59 O12 123.2(6) . . ?
C58 C59 C60 121.3(6) . . ?
O12 C59 C60 115.5(5) . . ?
C74 C60 C59 120.8(5) . . ?
C74 C60 C55 119.2(6) . . ?
C59 C60 C55 119.7(5) . . ?
O13 C61 C62 122.0(5) . . ?
O13 C61 C66 120.3(5) . . ?
C62 C61 C66 117.7(5) . . ?
C63 C62 C61 119.6(6) . . ?
C63 C62 C78 121.3(5) . . ?
C61 C62 C78 119.2(5) . . ?
C62 C63 C64 124.1(6) . . ?
C65 C64 C63 116.2(6) . . ?
C65 C64 C79 122.8(6) . . ?
C63 C64 C79 121.0(6) . . ?
C64 C65 O14 122.6(6) . . ?
C64 C65 C66 122.1(6) . . ?
O14 C65 C66 115.3(6) . . ?
C75 C66 C65 118.8(6) . . ?
C75 C66 C61 120.7(6) . . ?
C65 C66 C61 120.3(6) . . ?
O15 C67 C72 123.1(7) . . ?
O15 C67 C68 119.9(9) . . ?
C72 C67 C68 117.1(9) . . ?
C69 C68 C67 118.3(8) . . ?
C69 C68 C79 122.4(7) . . ?
C67 C68 C79 119.3(9) . . ?
C68 C69 C70 124.2(7) . . ?
C71 C70 C69 119.3(9) . . ?
C71 C70 C80 120.2(8) . . ?
C69 C70 C80 120.3(6) . . ?
O16 C71 C70 124.7(9) . . ?
O16 C71 C72 116.5(7) . . ?
C70 C71 C72 118.8(9) . . ?
C71 C72 C67 122.1(7) . . ?
C71 C72 C76 121.0(9) . . ?
C67 C72 C76 116.8(10) . . ?
N5 C73 C54 121.2(9) . . ?
N6 C74 C60 124.5(6) . . ?
N7 C75 C66 123.9(6) . . ?
N8 C76 C72 127.0(11) . . ?
C56 C77 C81 111.8(5) . . ?
C56 C77 C52 109.5(4) . . ?
C81 C77 C52 113.8(5) . . ?
C58 C78 C85 114.1(5) . . ?
C58 C78 C62 109.9(5) . . ?
C85 C78 C62 112.2(6) . . ?
C68 C79 C64 112.1(6) . . ?
C68 C79 C89 111.4(7) . . ?
C64 C79 C89 112.8(6) . . ?
C50 C80 C70 111.3(6) . . ?
C50 C80 C93 113.8(7) . . ?
C70 C80 C93 112.0(8) . . ?
C82 C81 C77 112.6(6) . . ?
C83 C82 C81 107.6(10) . . ?
C83 C82 C84 105.2(9) . . ?
C81 C82 C84 110.4(8) . . ?
C86B C85 C78 124.2(9) . . ?
C86A C85 C78 122.4(7) . . ?
C90 C89 C79 116.1(8) . . ?
C89 C90 C92 110.7(8) . . ?
C89 C90 C91 110.8(9) . . ?
C92 C90 C91 108.1(9) . . ?
C94A C93 C80 119.3(10) . . ?
C94B C93 C80 112.6(8) . . ?
N1 C97 C98 112.2(6) . . ?
C99 C98 C97 112.7(7) . . ?
C98 C99 C100 114.6(8) . . ?
C101 C100 C99 109.6(9) . . ?
C100 C101 C102 110.7(9) . . ?
N5 C102 C101 110.5(9) . . ?
N2 C103 C104 109.4(5) . . ?
C105 C104 C103 113.8(6) . . ?
C104 C105 C106 112.3(6) . . ?
C107 C106 C105 114.7(6) . . ?
C106 C107 C108 113.1(6) . . ?
N6 C108 C107 112.7(5) . . ?
N3 C109 C110 110.6(5) . . ?
C109 C110 C111 109.5(5) . . ?
C112 C111 C110 111.3(6) . . ?
C111 C112 C113 114.0(5) . . ?
C114 C113 C112 113.8(5) . . ?
N7 C114 C113 112.5(5) . . ?
N4 C115 C116 110.7(8) . . ?
C115 C116 C117 113.7(10) . . ?
C116 C117 C118 102.4(10) . . ?
C119 C118 C117 101.7(10) . . ?
C118 C119 C120 120.3(9) . . ?
N8 C120 C119 113.2(7) . . ?
C85 C86A C87A 119.7(11) . . ?
C85 C86A C88A 114.4(10) . . ?
C87A C86A C88A 110.2(11) . . ?
C95A C94A C93 116(2) . . ?
C95A C94A C96A 110(2) . . ?
C93 C94A C96A 117.0(16) . . ?
C85 C86B C88B 113.9(12) . . ?
C85 C86B C87B 111.2(11) . . ?
C88B C86B C87B 101.4(13) . . ?
C93 C94B C95B 114.4(14) . . ?
C93 C94B C96B 109.1(13) . . ?
C95B C94B C96B 105.4(14) . . ?
 
_refine_diff_density_max    1.038
_refine_diff_density_min   -0.481
_refine_diff_density_rms    0.064




