# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

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

data_fos016_4m

_database_code_depnum_ccdc_archive 'CCDC 2078130'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H20 Na O6 P'
_chemical_formula_weight         434.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   19.211(2)
_cell_length_b                   8.5749(9)
_cell_length_c                   12.3647(13)
_cell_angle_alpha                90
_cell_angle_beta                 97.328(7)
_cell_angle_gamma                90
_cell_volume                     2020.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    4107
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      31.79

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.076
_exptl_absorpt_coefficient_mu    0.195
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   
;
Crystal faces:

     H       K       L      d(mm)

  -2.000   0.000  -1.000   0.08200
   2.000   1.000   0.000   0.03400
   0.000   0.000  -1.000   0.00100
   0.000   0.000   1.000   0.03800
   2.000   0.000   1.000   0.03700
  -1.000   1.000   0.000   0.11900
  -2.000   0.000   1.000   0.09400
  -1.000  -1.000   0.000   0.11000
   0.000   5.000  -1.000   0.08400
;
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_measurement_device_type  
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            20004
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.605
_diffrn_reflns_theta_max         33.235
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6780
_reflns_number_gt                4096
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom. The hydrogen 
 atoms of the OH groups were refined freely.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0614P)²+0.4489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6780
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1114
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.38700(3) 0.43543(5) 0.17971(4) 0.01498(12) Uani 1 1 d . . . . .
Na1 Na 0.54196(4) 0.27755(9) 0.20585(6) 0.02087(19) Uani 1 1 d . . . . .
O1 O 0.33257(7) 0.40816(14) 0.07087(10) 0.0152(3) Uani 1 1 d . . . . .
O2 O 0.33497(7) 0.47679(15) 0.26859(10) 0.0158(3) Uani 1 1 d . . . . .
O3 O 0.43014(7) 0.57738(15) 0.17187(11) 0.0190(3) Uani 1 1 d . . . . .
O4 O 0.42277(7) 0.28375(15) 0.20384(12) 0.0209(3) Uani 1 1 d . . . . .
O98 O 0.53277(10) 0.2709(2) 0.01865(14) 0.0370(4) Uani 1 1 d . . . . .
H98 H 0.5464(17) 0.327(4) -0.029(3) 0.058(10) Uiso 1 1 d . . . . .
O99 O 0.61261(8) 0.47927(17) 0.27077(12) 0.0244(3) Uani 1 1 d . . . . .
H99 H 0.6031(15) 0.572(3) 0.268(2) 0.041(8) Uiso 1 1 d . . . . .
C1 C 0.28484(10) 0.5278(2) 0.04019(14) 0.0136(4) Uani 1 1 d . . . . .
C2 C 0.29522(10) 0.6143(2) -0.05312(15) 0.0166(4) Uani 1 1 d . . . . .
H2 H 0.3331 0.5905 -0.0928 0.020 Uiso 1 1 calc R U . . .
C3 C 0.25003(11) 0.7332(2) -0.08565(15) 0.0180(4) Uani 1 1 d . . . . .
H3 H 0.2550 0.7886 -0.1507 0.022 Uiso 1 1 calc R U . . .
C4 C 0.19589(10) 0.7748(2) -0.02374(15) 0.0152(4) Uani 1 1 d . . . . .
C5 C 0.15295(11) 0.9069(2) -0.04986(16) 0.0193(4) Uani 1 1 d . . . . .
H5 H 0.1585 0.9654 -0.1135 0.023 Uiso 1 1 calc R U . . .
C6 C 0.10371(11) 0.9523(2) 0.01414(16) 0.0199(4) Uani 1 1 d . . . . .
H6 H 0.0757 1.0419 -0.0049 0.024 Uiso 1 1 calc R U . . .
C7 C 0.09445(11) 0.8663(2) 0.10844(16) 0.0183(4) Uani 1 1 d . . . . .
H7 H 0.0605 0.8988 0.1533 0.022 Uiso 1 1 calc R U . . .
C8 C 0.13421(10) 0.7359(2) 0.13575(15) 0.0155(4) Uani 1 1 d . . . . .
H8 H 0.1274 0.6789 0.1995 0.019 Uiso 1 1 calc R U . . .
C9 C 0.18539(10) 0.68479(19) 0.07017(14) 0.0136(4) Uani 1 1 d . . . . .
C10 C 0.22922(10) 0.55176(19) 0.09838(14) 0.0127(3) Uani 1 1 d . . . . .
C11 C 0.27070(10) 0.4015(2) 0.26620(15) 0.0146(4) Uani 1 1 d . . . . .
C12 C 0.26269(11) 0.2947(2) 0.35009(15) 0.0186(4) Uani 1 1 d . . . . .
H12 H 0.3014 0.2696 0.4029 0.022 Uiso 1 1 calc R U . . .
C13 C 0.19912(11) 0.2276(2) 0.35491(16) 0.0187(4) Uani 1 1 d . . . . .
H13 H 0.1933 0.1583 0.4131 0.022 Uiso 1 1 calc R U . . .
C14 C 0.14136(11) 0.2590(2) 0.27475(15) 0.0159(4) Uani 1 1 d . . . . .
C15 C 0.07473(11) 0.1899(2) 0.27911(16) 0.0191(4) Uani 1 1 d . . . . .
H15 H 0.0682 0.1230 0.3382 0.023 Uiso 1 1 calc R U . . .
C16 C 0.01976(11) 0.2176(2) 0.20015(16) 0.0209(4) Uani 1 1 d . . . . .
H16 H -0.0246 0.1708 0.2048 0.025 Uiso 1 1 calc R U . . .
C17 C 0.02890(11) 0.3157(2) 0.11168(16) 0.0188(4) Uani 1 1 d . . . . .
H17 H -0.0092 0.3331 0.0560 0.023 Uiso 1 1 calc R U . . .
C18 C 0.09200(10) 0.3861(2) 0.10527(15) 0.0153(4) Uani 1 1 d . . . . .
H18 H 0.0972 0.4513 0.0447 0.018 Uiso 1 1 calc R U . . .
C19 C 0.15015(10) 0.36394(19) 0.18739(14) 0.0138(4) Uani 1 1 d . . . . .
C20 C 0.21661(10) 0.43962(19) 0.18598(14) 0.0130(3) Uani 1 1 d . . . . .
C98 C 0.47367(18) 0.1935(4) -0.0351(2) 0.0651(10) Uani 1 1 d . . . . .
H98A H 0.4473 0.1451 0.0190 0.098 Uiso 1 1 calc R U . . .
H98B H 0.4889 0.1127 -0.0830 0.098 Uiso 1 1 calc R U . . .
H98C H 0.4436 0.2686 -0.0787 0.098 Uiso 1 1 calc R U . . .
C99 C 0.67470(13) 0.4598(3) 0.34602(19) 0.0318(5) Uani 1 1 d . . . . .
H99A H 0.6665 0.4992 0.4178 0.048 Uiso 1 1 calc R U . . .
H99B H 0.7133 0.5181 0.3203 0.048 Uiso 1 1 calc R U . . .
H99C H 0.6869 0.3489 0.3517 0.048 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
P1 O3 1.4826(14) . ?
P1 O4 1.4834(14) . ?
P1 O1 1.6125(14) . ?
P1 O2 1.6165(14) . ?
P1 Na1 3.2485(10) . ?
Na1 O99 2.2805(17) . ?
Na1 O4 2.2872(16) . ?
Na1 O98 2.2996(19) . ?
Na1 O3 2.3050(15) 2_645 ?
O1 C1 1.396(2) . ?
O2 C11 1.390(2) . ?
O3 Na1 2.3049(15) 2_655 ?
O98 C98 1.407(3) . ?
O99 C99 1.426(3) . ?
C1 C10 1.378(3) . ?
C1 C2 1.407(3) . ?
C2 C3 1.366(3) . ?
C3 C4 1.414(3) . ?
C4 C5 1.414(3) . ?
C4 C9 1.430(2) . ?
C5 C6 1.365(3) . ?
C6 C7 1.410(3) . ?
C7 C8 1.372(3) . ?
C8 C9 1.421(3) . ?
C9 C10 1.434(2) . ?
C10 C20 1.491(2) . ?
C11 C20 1.381(3) . ?
C11 C12 1.407(3) . ?
C12 C13 1.358(3) . ?
C13 C14 1.416(3) . ?
C14 C15 1.418(3) . ?
C14 C19 1.432(2) . ?
C15 C16 1.365(3) . ?
C16 C17 1.409(3) . ?
C17 C18 1.365(3) . ?
C18 C19 1.423(3) . ?
C19 C20 1.434(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
O3 P1 O4 118.98(8) . . ?
O3 P1 O1 111.89(7) . . ?
O4 P1 O1 105.97(7) . . ?
O3 P1 O2 105.28(7) . . ?
O4 P1 O2 111.49(8) . . ?
O1 P1 O2 101.99(7) . . ?
O3 P1 Na1 80.56(6) . . ?
O4 P1 Na1 38.70(6) . . ?
O1 P1 Na1 120.74(5) . . ?
O2 P1 Na1 131.46(5) . . ?
O99 Na1 O4 122.43(6) . . ?
O99 Na1 O98 109.81(7) . . ?
O4 Na1 O98 92.37(7) . . ?
O99 Na1 O3 104.82(6) . 2_645 ?
O4 Na1 O3 99.97(6) . 2_645 ?
O98 Na1 O3 128.56(7) . 2_645 ?
O99 Na1 P1 102.45(5) . . ?
O4 Na1 P1 23.92(3) . . ?
O98 Na1 P1 87.62(6) . . ?
O3 Na1 P1 120.61(5) 2_645 . ?
C1 O1 P1 116.99(11) . . ?
C11 O2 P1 120.55(11) . . ?
P1 O3 Na1 130.82(8) . 2_655 ?
P1 O4 Na1 117.38(8) . . ?
C98 O98 Na1 116.15(16) . . ?
C99 O99 Na1 123.50(13) . . ?
C10 C1 O1 119.62(15) . . ?
C10 C1 C2 123.36(17) . . ?
O1 C1 C2 116.97(16) . . ?
C3 C2 C1 118.94(18) . . ?
C2 C3 C4 120.86(17) . . ?
C3 C4 C5 121.78(17) . . ?
C3 C4 C9 119.54(17) . . ?
C5 C4 C9 118.64(17) . . ?
C6 C5 C4 121.55(18) . . ?
C5 C6 C7 119.99(18) . . ?
C8 C7 C6 120.32(19) . . ?
C7 C8 C9 121.00(17) . . ?
C8 C9 C4 118.44(16) . . ?
C8 C9 C10 122.28(16) . . ?
C4 C9 C10 119.19(17) . . ?
C1 C10 C9 117.52(16) . . ?
C1 C10 C20 119.46(16) . . ?
C9 C10 C20 123.01(16) . . ?
C20 C11 O2 119.36(16) . . ?
C20 C11 C12 122.72(18) . . ?
O2 C11 C12 117.84(17) . . ?
C13 C12 C11 119.44(18) . . ?
C12 C13 C14 121.15(17) . . ?
C13 C14 C15 121.62(17) . . ?
C13 C14 C19 119.36(18) . . ?
C15 C14 C19 119.02(18) . . ?
C16 C15 C14 121.33(18) . . ?
C15 C16 C17 119.86(19) . . ?
C18 C17 C16 120.57(19) . . ?
C17 C18 C19 121.42(17) . . ?
C18 C19 C14 117.70(17) . . ?
C18 C19 C20 123.34(16) . . ?
C14 C19 C20 118.96(17) . . ?
C11 C20 C19 118.27(16) . . ?
C11 C20 C10 119.81(16) . . ?
C19 C20 C10 121.87(16) . . ?

_refine_diff_density_max         0.454
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.079


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

data_st010_4m

_database_code_depnum_ccdc_archive 'CCDC 2078135'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H20 Br N3'
_chemical_formula_weight         418.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8577(2)
_cell_length_b                   8.9307(2)
_cell_length_c                   18.7699(4)
_cell_angle_alpha                91.7000(10)
_cell_angle_beta                 93.9750(10)
_cell_angle_gamma                108.2000(10)
_cell_volume                     1405.06(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9984
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      16.7

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.989
_exptl_crystal_F_000             428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_exptl_absorpt_coefficient_mu    1.471
_shelx_estimated_absorpt_T_min   0.785
_shelx_estimated_absorpt_T_max   0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_measurement_device_type  
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            38397
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.404
_diffrn_reflns_theta_max         32.575
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9887
_reflns_number_gt                7853
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom. NH hydrogen atoms were 
 refined freely with its NH bond length restraint to 0.87Å and its 
 displacement parameter constrained to 1.2 times the Ueq of the connecting N atom.
 SQUEEZE:
 The structure contained to molecules of chloroform which were disordered
 other at least two positions. These two positions could be refined quite well
 however the difference fourier synthesis show several more electron peaks in 
 the vicinity (approx 3.5 electrons high) which coulds not be attributed to 
 further orientations. Thus the final refinement was performed using solvent
 free data from a PLATON/SQUEEZE run. The solvent molecule are not atributed
 for in the sum formula.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.002 0.000 0.012 561 281 ' '
_platon_squeeze_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)+(0.0678P)²+0.3442P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9887
_refine_ls_number_parameters     260
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1161
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_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
Br1 Br 0.77511(2) 0.59338(2) 0.41095(2) 0.01943(6) Uani 1 1 d . . . . .
N1 N 0.31117(18) 0.7072(2) 0.35722(9) 0.0190(3) Uani 1 1 d . . . . .
N2 N 0.4281(2) 0.6444(3) 0.46192(10) 0.0331(5) Uani 1 1 d D . . . .
H2A H 0.407(4) 0.611(3) 0.5025(11) 0.040 Uiso 1 1 d D U . . .
H2B H 0.509(3) 0.636(3) 0.4410(15) 0.040 Uiso 1 1 d D U . . .
N3 N 0.1753(3) 0.6569(3) 0.45993(11) 0.0369(5) Uani 1 1 d D . . . .
H3A H 0.093(3) 0.664(4) 0.4395(15) 0.044 Uiso 1 1 d D U . . .
H3B H 0.173(4) 0.611(3) 0.4953(12) 0.044 Uiso 1 1 d D U . . .
C1 C 0.3990(2) 0.9319(2) 0.23179(9) 0.0152(3) Uani 1 1 d . . . . .
C2 C 0.4881(2) 0.9176(2) 0.29354(10) 0.0180(3) Uani 1 1 d . . . . .
C3 C 0.5978(2) 1.0518(2) 0.33071(11) 0.0225(4) Uani 1 1 d . . . . .
H3 H 0.6585 1.0399 0.3726 0.027 Uiso 1 1 calc R U . . .
C4 C 0.6167(2) 1.1993(2) 0.30636(12) 0.0249(4) Uani 1 1 d . . . . .
H4 H 0.6935 1.2887 0.3305 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5232(2) 1.2195(2) 0.24579(11) 0.0203(4) Uani 1 1 d . . . . .
C6 C 0.5349(3) 1.3734(2) 0.22265(12) 0.0265(4) Uani 1 1 d . . . . .
H6 H 0.6103 1.4633 0.2472 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4407(3) 1.3929(2) 0.16654(13) 0.0282(4) Uani 1 1 d . . . . .
H7 H 0.4498 1.4963 0.1522 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3281(3) 1.2606(2) 0.12877(12) 0.0250(4) Uani 1 1 d . . . . .
H8 H 0.2614 1.2755 0.0895 0.030 Uiso 1 1 calc R U . . .
C9 C 0.3155(2) 1.1112(2) 0.14894(10) 0.0192(3) Uani 1 1 d . . . . .
H9 H 0.2403 1.0232 0.1231 0.023 Uiso 1 1 calc R U . . .
C10 C 0.4127(2) 1.0857(2) 0.20769(10) 0.0164(3) Uani 1 1 d . . . . .
C11 C 0.2857(2) 0.7849(2) 0.19625(10) 0.0158(3) Uani 1 1 d . . . . .
C12 C 0.1749(2) 0.6848(2) 0.23638(10) 0.0176(3) Uani 1 1 d . . . . .
C13 C 0.0673(2) 0.5422(2) 0.20534(11) 0.0225(4) Uani 1 1 d . . . . .
H13 H -0.0090 0.4759 0.2334 0.027 Uiso 1 1 calc R U . . .
C14 C 0.0717(2) 0.4984(2) 0.13529(11) 0.0236(4) Uani 1 1 d . . . . .
H14 H -0.0032 0.4033 0.1149 0.028 Uiso 1 1 calc R U . . .
C15 C 0.1866(2) 0.5932(2) 0.09276(11) 0.0208(4) Uani 1 1 d . . . . .
C16 C 0.2009(3) 0.5436(3) 0.02213(11) 0.0260(4) Uani 1 1 d . . . . .
H16 H 0.1275 0.4478 0.0015 0.031 Uiso 1 1 calc R U . . .
C17 C 0.3187(3) 0.6312(3) -0.01736(12) 0.0305(5) Uani 1 1 d . . . . .
H17 H 0.3267 0.5962 -0.0648 0.037 Uiso 1 1 calc R U . . .
C18 C 0.4280(3) 0.7738(3) 0.01303(11) 0.0291(4) Uani 1 1 d . . . . .
H18 H 0.5096 0.8346 -0.0143 0.035 Uiso 1 1 calc R U . . .
C19 C 0.4179(2) 0.8255(2) 0.08157(11) 0.0226(4) Uani 1 1 d . . . . .
H19 H 0.4932 0.9211 0.1013 0.027 Uiso 1 1 calc R U . . .
C20 C 0.2961(2) 0.7380(2) 0.12339(10) 0.0174(3) Uani 1 1 d . . . . .
C21 C 0.4638(2) 0.7573(2) 0.32342(10) 0.0196(4) Uani 1 1 d . . . . .
H21A H 0.4624 0.6795 0.2845 0.024 Uiso 1 1 calc R U . . .
H21B H 0.5530 0.7624 0.3593 0.024 Uiso 1 1 calc R U . . .
C22 C 0.1715(2) 0.7261(2) 0.31508(10) 0.0193(3) Uani 1 1 d . . . . .
H22A H 0.1716 0.8366 0.3213 0.023 Uiso 1 1 calc R U . . .
H22B H 0.0724 0.6566 0.3329 0.023 Uiso 1 1 calc R U . . .
C23 C 0.3043(2) 0.6688(3) 0.42506(11) 0.0234(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C23 1.329(2) . ?
N1 C22 1.479(2) . ?
N1 C21 1.480(2) . ?
N2 C23 1.335(3) . ?
N3 C23 1.333(3) . ?
C1 C2 1.388(2) . ?
C1 C10 1.430(2) . ?
C1 C11 1.486(3) . ?
C2 C3 1.413(3) . ?
C2 C21 1.511(3) . ?
C3 C4 1.371(3) . ?
C4 C5 1.409(3) . ?
C5 C10 1.421(3) . ?
C5 C6 1.429(3) . ?
C6 C7 1.348(3) . ?
C7 C8 1.418(3) . ?
C8 C9 1.371(3) . ?
C9 C10 1.420(3) . ?
C11 C12 1.387(2) . ?
C11 C20 1.436(3) . ?
C12 C13 1.411(3) . ?
C12 C22 1.517(3) . ?
C13 C14 1.367(3) . ?
C14 C15 1.416(3) . ?
C15 C16 1.412(3) . ?
C15 C20 1.428(3) . ?
C16 C17 1.372(3) . ?
C17 C18 1.412(3) . ?
C18 C19 1.372(3) . ?
C19 C20 1.420(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
C23 N1 C22 121.53(15) . . ?
C23 N1 C21 121.78(16) . . ?
C22 N1 C21 116.04(14) . . ?
C2 C1 C10 119.27(17) . . ?
C2 C1 C11 117.57(16) . . ?
C10 C1 C11 123.05(16) . . ?
C1 C2 C3 121.03(17) . . ?
C1 C2 C21 119.88(17) . . ?
C3 C2 C21 119.05(17) . . ?
C4 C3 C2 120.11(18) . . ?
C3 C4 C5 120.59(19) . . ?
C4 C5 C10 119.95(17) . . ?
C4 C5 C6 121.01(19) . . ?
C10 C5 C6 119.03(18) . . ?
C7 C6 C5 121.0(2) . . ?
C6 C7 C8 120.61(19) . . ?
C9 C8 C7 119.9(2) . . ?
C8 C9 C10 121.24(19) . . ?
C9 C10 C5 118.26(16) . . ?
C9 C10 C1 122.77(17) . . ?
C5 C10 C1 118.92(17) . . ?
C12 C11 C20 119.28(17) . . ?
C12 C11 C1 118.76(16) . . ?
C20 C11 C1 121.77(15) . . ?
C11 C12 C13 120.78(17) . . ?
C11 C12 C22 119.95(17) . . ?
C13 C12 C22 119.25(16) . . ?
C14 C13 C12 120.66(18) . . ?
C13 C14 C15 120.82(18) . . ?
C16 C15 C14 121.47(19) . . ?
C16 C15 C20 119.31(18) . . ?
C14 C15 C20 119.14(18) . . ?
C17 C16 C15 121.3(2) . . ?
C16 C17 C18 119.5(2) . . ?
C19 C18 C17 120.8(2) . . ?
C18 C19 C20 120.84(19) . . ?
C19 C20 C15 118.24(17) . . ?
C19 C20 C11 122.43(17) . . ?
C15 C20 C11 119.22(16) . . ?
N1 C21 C2 109.54(15) . . ?
N1 C22 C12 110.86(15) . . ?
N1 C23 N3 121.64(18) . . ?
N1 C23 N2 121.38(18) . . ?
N3 C23 N2 116.96(18) . . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.101



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

data_mt_230_23_mom

_database_code_depnum_ccdc_archive 'CCDC 2078132'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H24 I N O2'
_chemical_formula_weight         521.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   10.158(5)
_cell_length_b                   9.420(4)
_cell_length_c                   12.633(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.94(2)
_cell_angle_gamma                90
_cell_volume                     1143.4(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7665
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      39.60

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.192
_exptl_absorpt_coefficient_mu    1.424
_shelx_estimated_absorpt_T_min   0.615
_shelx_estimated_absorpt_T_max   0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 2/COSMO'
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            40148
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.704
_diffrn_reflns_theta_max         33.140
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8111
_reflns_number_gt                7744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER APEX2(v2009.5-1)'
_computing_cell_refinement       'BRUKER APEX2(v2009.5-1)'
_computing_data_reduction        'BRUKER APEX2(v2009.5-1)'
_computing_structure_solution    'BRUKER APEX2(v2009.5-1)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 Twinning:
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0630P)²+2.2600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(3)
_chemical_absolute_configuration .
_refine_ls_number_reflns         8111
_refine_ls_number_parameters     284
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1386
_refine_ls_wR_factor_gt          0.1375
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_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
I1 I 0.98963(4) 1.00202(6) 0.99109(3) 0.04360(13) Uani 1 1 d . . . . .
O1 O 1.3228(4) 1.0226(5) 0.7335(3) 0.0326(7) Uani 1 1 d . . . . .
O2 O 1.3338(4) 0.9843(4) 0.9143(3) 0.0322(8) Uani 1 1 d . . . . .
N1 N 1.2045(4) 0.8405(4) 0.7795(3) 0.0245(7) Uani 1 1 d . . . . .
C1 C 0.9156(5) 0.6964(5) 0.7162(4) 0.0215(7) Uani 1 1 d . . . . .
C2 C 0.9828(5) 0.7805(5) 0.8077(4) 0.0216(8) Uani 1 1 d . . . . .
C3 C 0.9011(5) 0.8736(5) 0.8494(4) 0.0245(8) Uani 1 1 d . . . . .
C4 C 0.7595(5) 0.8854(5) 0.7994(4) 0.0273(9) Uani 1 1 d . . . . .
H4 H 0.706983 0.945081 0.831263 0.033 Uiso 1 1 calc R U . . .
C5 C 0.6924(5) 0.8091(5) 0.7009(4) 0.0251(8) Uani 1 1 d . . . . .
C6 C 0.5477(5) 0.8298(6) 0.6421(5) 0.0329(11) Uani 1 1 d . . . . .
H6 H 0.494852 0.891110 0.672378 0.039 Uiso 1 1 calc R U . . .
C7 C 0.4850(6) 0.7628(7) 0.5434(6) 0.0376(13) Uani 1 1 d . . . . .
H7 H 0.388767 0.777765 0.504950 0.045 Uiso 1 1 calc R U . . .
C8 C 0.5630(6) 0.6704(6) 0.4977(5) 0.0335(11) Uani 1 1 d . . . . .
H8 H 0.518957 0.625677 0.427658 0.040 Uiso 1 1 calc R U . . .
C9 C 0.7009(5) 0.6449(5) 0.5534(4) 0.0266(9) Uani 1 1 d . . . . .
H9 H 0.750804 0.580833 0.522412 0.032 Uiso 1 1 calc R U . . .
C10 C 0.7705(5) 0.7130(5) 0.6567(4) 0.0213(8) Uani 1 1 d . . . . .
C11 C 1.0008(5) 0.5910(5) 0.6782(4) 0.0208(8) Uani 1 1 d . . . . .
C12 C 1.1168(5) 0.6390(5) 0.6535(4) 0.0238(8) Uani 1 1 d . . . . .
C13 C 1.2018(6) 0.5415(6) 0.6205(4) 0.0298(10) Uani 1 1 d . . . . .
H13 H 1.281650 0.574666 0.604556 0.036 Uiso 1 1 calc R U . . .
C14 C 1.1702(7) 0.3997(6) 0.6113(5) 0.0335(11) Uani 1 1 d . . . . .
H14 H 1.227015 0.336014 0.586932 0.040 Uiso 1 1 calc R U . . .
C15 C 1.0550(6) 0.3469(6) 0.6374(4) 0.0271(9) Uani 1 1 d . . . . .
C16 C 1.0228(7) 0.1990(6) 0.6307(5) 0.0351(12) Uani 1 1 d . . . . .
H16 H 1.078154 0.135127 0.604911 0.042 Uiso 1 1 calc R U . . .
C17 C 0.9141(8) 0.1475(6) 0.6605(5) 0.0391(12) Uani 1 1 d . . . . .
H17 H 0.892874 0.049069 0.653639 0.047 Uiso 1 1 calc R U . . .
C18 C 0.8337(7) 0.2411(7) 0.7014(5) 0.0348(10) Uani 1 1 d . . . . .
H18 H 0.761197 0.204528 0.725765 0.042 Uiso 1 1 calc R U . . .
C19 C 0.8590(6) 0.3853(6) 0.7065(4) 0.0283(9) Uani 1 1 d . . . . .
H19 H 0.802428 0.447089 0.732793 0.034 Uiso 1 1 calc R U . . .
C20 C 0.9689(5) 0.4425(5) 0.6728(4) 0.0232(8) Uani 1 1 d . . . . .
C21 C 1.1406(5) 0.7738(4) 0.8564(4) 0.0220(9) Uani 1 1 d . . . . .
H21A H 1.171925 0.823499 0.929353 0.026 Uiso 1 1 calc R U . . .
H21B H 1.170753 0.673490 0.869133 0.026 Uiso 1 1 calc R U . . .
C22 C 1.1519(5) 0.7941(5) 0.6614(4) 0.0252(9) Uani 1 1 d . . . . .
H22A H 1.223441 0.812433 0.625393 0.030 Uiso 1 1 calc R U . . .
H22B H 1.067824 0.849565 0.621033 0.030 Uiso 1 1 calc R U . . .
C23 C 1.2887(5) 0.9572(5) 0.8036(4) 0.0257(9) Uani 1 1 d . . . . .
C24 C 1.4012(6) 1.1219(6) 0.9567(5) 0.0353(12) Uani 1 1 d . . . . .
C25 C 1.5368(7) 1.1394(8) 0.9326(7) 0.0493(17) Uani 1 1 d . . . . .
H25A H 1.592365 1.052627 0.954033 0.074 Uiso 1 1 calc R U . . .
H25B H 1.588713 1.219784 0.975526 0.074 Uiso 1 1 calc R U . . .
H25C H 1.517212 1.157044 0.852452 0.074 Uiso 1 1 calc R U . . .
C26 C 1.2991(8) 1.2410(8) 0.9081(7) 0.0492(16) Uani 1 1 d . . . . .
H26A H 1.338741 1.331253 0.942497 0.074 Uiso 1 1 calc R U . . .
H26B H 1.211900 1.222710 0.923192 0.074 Uiso 1 1 calc R U . . .
H26C H 1.280598 1.246061 0.827037 0.074 Uiso 1 1 calc R U . . .
C27 C 1.4280(9) 1.1059(9) 1.0817(6) 0.0544(19) Uani 1 1 d . . . . .
H27A H 1.473785 1.191578 1.120489 0.082 Uiso 1 1 calc R U . . .
H27B H 1.488121 1.023457 1.109634 0.082 Uiso 1 1 calc R U . . .
H27C H 1.339335 1.092230 1.095555 0.082 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
I1 C3 2.105(5) . ?
O1 C23 1.217(6) . ?
O2 C23 1.347(6) . ?
O2 C24 1.483(6) . ?
N1 C23 1.366(6) . ?
N1 C21 1.473(6) . ?
N1 C22 1.478(7) . ?
C1 C2 1.385(7) . ?
C1 C10 1.429(6) . ?
C1 C11 1.495(6) . ?
C2 C3 1.422(7) . ?
C2 C21 1.520(6) . ?
C3 C4 1.375(7) . ?
C4 C5 1.406(7) . ?
C5 C6 1.429(7) . ?
C5 C10 1.430(7) . ?
C6 C7 1.357(10) . ?
C7 C8 1.420(9) . ?
C8 C9 1.370(7) . ?
C9 C10 1.420(7) . ?
C11 C12 1.389(7) . ?
C11 C20 1.432(6) . ?
C12 C13 1.412(7) . ?
C12 C22 1.500(7) . ?
C13 C14 1.371(9) . ?
C14 C15 1.405(9) . ?
C15 C20 1.424(7) . ?
C15 C16 1.427(8) . ?
C16 C17 1.366(10) . ?
C17 C18 1.410(10) . ?
C18 C19 1.380(8) . ?
C19 C20 1.424(8) . ?
C24 C25 1.514(10) . ?
C24 C26 1.516(9) . ?
C24 C27 1.520(10) . ?

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
C23 O2 C24 120.2(4) . . ?
C23 N1 C21 125.1(4) . . ?
C23 N1 C22 117.3(4) . . ?
C21 N1 C22 116.5(4) . . ?
C2 C1 C10 121.4(4) . . ?
C2 C1 C11 117.9(4) . . ?
C10 C1 C11 120.7(4) . . ?
C1 C2 C3 118.3(4) . . ?
C1 C2 C21 118.9(4) . . ?
C3 C2 C21 122.8(4) . . ?
C4 C3 C2 121.9(4) . . ?
C4 C3 I1 116.1(4) . . ?
C2 C3 I1 122.0(4) . . ?
C3 C4 C5 120.0(4) . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 C10 119.8(4) . . ?
C6 C5 C10 119.4(5) . . ?
C7 C6 C5 120.8(5) . . ?
C6 C7 C8 120.0(5) . . ?
C9 C8 C7 120.7(6) . . ?
C8 C9 C10 120.9(5) . . ?
C9 C10 C1 123.6(4) . . ?
C9 C10 C5 118.1(4) . . ?
C1 C10 C5 118.2(4) . . ?
C12 C11 C20 120.1(4) . . ?
C12 C11 C1 118.5(4) . . ?
C20 C11 C1 121.3(4) . . ?
C11 C12 C13 120.0(5) . . ?
C11 C12 C22 120.2(4) . . ?
C13 C12 C22 119.9(4) . . ?
C14 C13 C12 120.7(5) . . ?
C13 C14 C15 121.0(5) . . ?
C14 C15 C20 119.5(5) . . ?
C14 C15 C16 121.5(5) . . ?
C20 C15 C16 118.9(5) . . ?
C17 C16 C15 121.3(5) . . ?
C16 C17 C18 119.7(5) . . ?
C19 C18 C17 120.7(6) . . ?
C18 C19 C20 120.7(5) . . ?
C19 C20 C15 118.4(5) . . ?
C19 C20 C11 122.8(5) . . ?
C15 C20 C11 118.7(5) . . ?
N1 C21 C2 110.4(4) . . ?
N1 C22 C12 110.9(4) . . ?
O1 C23 O2 125.3(5) . . ?
O1 C23 N1 123.4(5) . . ?
O2 C23 N1 111.2(4) . . ?
O2 C24 C25 111.4(5) . . ?
O2 C24 C26 109.0(5) . . ?
C25 C24 C26 112.7(6) . . ?
O2 C24 C27 101.2(5) . . ?
C25 C24 C27 110.6(6) . . ?
C26 C24 C27 111.3(6) . . ?

_refine_diff_density_max         2.000
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.140


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

data_fos016_27m

_database_code_depnum_ccdc_archive 'CCDC 2078131'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44.92 H38.29 N3 O5.43 P'
_chemical_formula_weight         738.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   18.1178(12)
_cell_length_b                   19.5762(12)
_cell_length_c                   22.3911(12)
_cell_angle_alpha                80.708(3)
_cell_angle_beta                 72.212(2)
_cell_angle_gamma                86.459(3)
_cell_volume                     7462.1(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9774
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      33.06

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_F_000             3098
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.201
_exptl_absorpt_coefficient_mu    0.127
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_measurement_device_type  
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            153929
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         33.203
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             50065
_reflns_number_gt                33644
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom. The hydrogen atoms of NH
 groups were refined freely. Those of the methanol molecule were
 refined using AFIX 147 i.e. rotating refinment with a bond angle
 fixed to the tetrahedral angle. In case of the disordered molecules 
 they were restraint to point towards the most reasonable H bond
 acceptor employing a FLAT restraint. This was not possible for
 H95K. Since its position did not converge properly the refinment
 was damped to settle its position.

 The atoms of the disorderd solvent molecules could only be 
 refined isotropically. The phenyl ring of the toluene molecule was
 constraint to a regular hexagon. Despite the use of distance restraints
 (SADI, DFIX) in some cases the bond length are not very realistic and 
 should be ignored. The residual electron density suggests further disorder
 components of methanol 95 which could not be modelled properly.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0780P)²+3.0116P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         50065
_refine_ls_number_parameters     2038
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1584
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.012
_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
P2 P 0.06283(2) 0.10098(2) 0.68577(2) 0.01400(6) Uani 1 1 d . . . . .
P4 P 0.42151(2) 0.17745(2) 0.48171(2) 0.01396(6) Uani 1 1 d . . . . .
P6 P 0.62981(2) 0.32416(2) 0.99834(2) 0.01572(6) Uani 1 1 d . . . . .
P8 P 0.97561(2) 0.39975(2) 0.78545(2) 0.01763(6) Uani 1 1 d . . . . .
O201 O 0.00030(4) 0.04031(4) 0.70784(3) 0.01531(16) Uani 1 1 d . . . . .
O202 O 0.04377(4) 0.14498(4) 0.62462(3) 0.01625(17) Uani 1 1 d . . . . .
O203 O 0.04236(4) 0.14141(4) 0.73983(3) 0.01773(17) Uani 1 1 d . . . . .
O204 O 0.14389(4) 0.07672(4) 0.66164(4) 0.01983(18) Uani 1 1 d . . . . .
O401 O 0.46735(4) 0.24920(4) 0.45908(3) 0.01663(17) Uani 1 1 d . . . . .
O402 O 0.35661(4) 0.18741(4) 0.44492(3) 0.01639(16) Uani 1 1 d . . . . .
O403 O 0.47083(4) 0.11721(4) 0.46062(4) 0.01890(18) Uani 1 1 d . . . . .
O404 O 0.38273(4) 0.17484(4) 0.55156(3) 0.01658(17) Uani 1 1 d . . . . .
O601 O 0.57757(4) 0.25696(4) 1.00966(3) 0.01598(16) Uani 1 1 d . . . . .
O602 O 0.68070(4) 0.30302(4) 1.04640(4) 0.01976(18) Uani 1 1 d . . . . .
O603 O 0.67918(4) 0.33050(4) 0.93106(4) 0.01856(18) Uani 1 1 d . . . . .
O604 O 0.58209(5) 0.38537(4) 1.01956(4) 0.02135(19) Uani 1 1 d . . . . .
O801 O 0.97822(4) 0.36397(4) 0.85501(4) 0.01993(18) Uani 1 1 d . . . . .
O802 O 1.04146(4) 0.45756(4) 0.76556(4) 0.01838(17) Uani 1 1 d . . . . .
O803 O 1.00211(4) 0.35071(4) 0.73881(4) 0.02150(18) Uani 1 1 d . . . . .
O804 O 0.89609(4) 0.42978(4) 0.79629(4) 0.02414(19) Uani 1 1 d . . . . .
N101 N 0.24719(5) 0.42112(5) 0.11952(5) 0.0202(2) Uani 1 1 d . . . . .
N102 N 0.34821(6) 0.48842(5) 0.05027(5) 0.0254(3) Uani 1 1 d . . . . .
H11 H 0.3738(9) 0.4520(8) 0.0356(7) 0.037(4) Uiso 1 1 d . . . . .
H12 H 0.3681(9) 0.5296(8) 0.0301(7) 0.039(4) Uiso 1 1 d . . . . .
N103 N 0.24302(6) 0.54097(5) 0.11265(5) 0.0242(2) Uani 1 1 d . . . . .
H13 H 0.2678(8) 0.5800(8) 0.0980(7) 0.033(4) Uiso 1 1 d . . . . .
H14 H 0.1940(9) 0.5415(8) 0.1378(7) 0.034(4) Uiso 1 1 d . . . . .
N301 N 0.23814(5) 0.32796(5) 0.63867(4) 0.01563(19) Uani 1 1 d . . . . .
N302 N 0.23577(5) 0.20837(5) 0.63990(4) 0.0174(2) Uani 1 1 d . . . . .
H31 H 0.2811(8) 0.2084(7) 0.6120(6) 0.027(4) Uiso 1 1 d . . . . .
H32 H 0.2063(8) 0.1708(8) 0.6496(7) 0.031(4) Uiso 1 1 d . . . . .
N303 N 0.13356(5) 0.26247(5) 0.70395(5) 0.0204(2) Uani 1 1 d . . . . .
H33 H 0.1091(9) 0.2198(8) 0.7159(7) 0.035(4) Uiso 1 1 d . . . . .
H34 H 0.1052(9) 0.2996(8) 0.7128(7) 0.037(4) Uiso 1 1 d . . . . .
N501 N 0.70070(5) 0.07156(5) 0.39252(4) 0.0173(2) Uani 1 1 d . . . . .
N502 N 0.59429(5) 0.01014(5) 0.45955(5) 0.0227(2) Uani 1 1 d . . . . .
H51 H 0.5609(9) 0.0452(8) 0.4559(7) 0.041(4) Uiso 1 1 d . . . . .
H52 H 0.5741(8) -0.0298(7) 0.4836(6) 0.027(4) Uiso 1 1 d . . . . .
N503 N 0.70774(5) -0.04780(5) 0.41596(5) 0.0197(2) Uani 1 1 d . . . . .
H53 H 0.6800(9) -0.0869(8) 0.4247(7) 0.038(4) Uiso 1 1 d . . . . .
H54 H 0.7599(8) -0.0490(8) 0.3911(7) 0.033(4) Uiso 1 1 d . . . . .
N701 N 0.80104(5) 0.16563(5) 0.85515(4) 0.0165(2) Uani 1 1 d . . . . .
N702 N 0.90968(6) 0.22456(5) 0.78722(5) 0.0217(2) Uani 1 1 d . . . . .
H71 H 0.9312(9) 0.1871(8) 0.7779(7) 0.036(4) Uiso 1 1 d . . . . .
H72 H 0.9356(9) 0.2639(8) 0.7717(7) 0.034(4) Uiso 1 1 d . . . . .
N703 N 0.81327(6) 0.28460(5) 0.84996(5) 0.0235(2) Uani 1 1 d . . . . .
H73 H 0.8442(8) 0.3197(8) 0.8363(7) 0.033(4) Uiso 1 1 d . . . . .
H74 H 0.7677(8) 0.2886(7) 0.8774(7) 0.031(4) Uiso 1 1 d . . . . .
C101 C 0.21463(6) 0.31677(5) 0.08641(5) 0.0189(2) Uani 1 1 d . . . . .
C102 C 0.20299(7) 0.31880(6) 0.02654(5) 0.0237(3) Uani 1 1 d . . . . .
H102 H 0.2372 0.3447 -0.0099 0.028 Uiso 1 1 calc R U . . .
C103 C 0.14343(7) 0.28418(6) 0.02026(5) 0.0243(3) Uani 1 1 d . . . . .
H103 H 0.1369 0.2859 -0.0205 0.029 Uiso 1 1 calc R U . . .
C104 C 0.09134(6) 0.24573(6) 0.07372(5) 0.0198(2) Uani 1 1 d . . . . .
C105 C 0.02869(7) 0.21022(7) 0.06761(6) 0.0258(3) Uani 1 1 d . . . . .
H105 H 0.0227 0.2110 0.0268 0.031 Uiso 1 1 calc R U . . .
C106 C -0.02292(7) 0.17501(7) 0.11936(6) 0.0293(3) Uani 1 1 d . . . . .
H106 H -0.0644 0.1512 0.1146 0.035 Uiso 1 1 calc R U . . .
C107 C -0.01468(7) 0.17404(7) 0.18020(6) 0.0265(3) Uani 1 1 d . . . . .
H107 H -0.0516 0.1503 0.2163 0.032 Uiso 1 1 calc R U . . .
C108 C 0.04569(6) 0.20675(6) 0.18793(5) 0.0195(2) Uani 1 1 d . . . . .
H108 H 0.0505 0.2051 0.2292 0.023 Uiso 1 1 calc R U . . .
C109 C 0.10127(6) 0.24319(5) 0.13489(5) 0.0163(2) Uani 1 1 d . . . . .
C110 C 0.16521(6) 0.27921(5) 0.14025(5) 0.0158(2) Uani 1 1 d . . . . .
C111 C 0.17862(6) 0.34833(6) 0.21928(5) 0.0177(2) Uani 1 1 d . . . . .
C112 C 0.18587(6) 0.35528(6) 0.27918(5) 0.0215(3) Uani 1 1 d . . . . .
H112 H 0.1846 0.4001 0.2907 0.026 Uiso 1 1 calc R U . . .
C113 C 0.19470(6) 0.29814(6) 0.32059(5) 0.0214(3) Uani 1 1 d . . . . .
H113 H 0.1972 0.3035 0.3613 0.026 Uiso 1 1 calc R U . . .
C114 C 0.20011(6) 0.23107(6) 0.30335(5) 0.0190(2) Uani 1 1 d . . . . .
C115 C 0.21696(7) 0.17175(6) 0.34275(5) 0.0226(3) Uani 1 1 d . . . . .
H115 H 0.2217 0.1765 0.3830 0.027 Uiso 1 1 calc R U . . .
C116 C 0.22647(7) 0.10806(6) 0.32405(6) 0.0237(3) Uani 1 1 d . . . . .
H116 H 0.2380 0.0690 0.3511 0.028 Uiso 1 1 calc R U . . .
C117 C 0.21924(7) 0.10002(6) 0.26432(5) 0.0216(3) Uani 1 1 d . . . . .
H117 H 0.2264 0.0556 0.2513 0.026 Uiso 1 1 calc R U . . .
C118 C 0.20192(6) 0.15610(6) 0.22523(5) 0.0184(2) Uani 1 1 d . . . . .
H118 H 0.1967 0.1500 0.1855 0.022 Uiso 1 1 calc R U . . .
C119 C 0.19167(6) 0.22299(6) 0.24343(5) 0.0161(2) Uani 1 1 d . . . . .
C120 C 0.17693(6) 0.28323(6) 0.20271(5) 0.0157(2) Uani 1 1 d . . . . .
C121 C 0.27888(7) 0.35760(6) 0.09256(6) 0.0220(3) Uani 1 1 d . . . . .
H12A H 0.3058 0.3290 0.1204 0.026 Uiso 1 1 calc R U . . .
H12B H 0.3171 0.3701 0.0503 0.026 Uiso 1 1 calc R U . . .
C122 C 0.17428(6) 0.41294(6) 0.17302(5) 0.0205(3) Uani 1 1 d . . . . .
H12C H 0.1300 0.4097 0.1565 0.025 Uiso 1 1 calc R U . . .
H12D H 0.1657 0.4540 0.1951 0.025 Uiso 1 1 calc R U . . .
C123 C 0.27936(6) 0.48320(6) 0.09412(5) 0.0187(2) Uani 1 1 d . . . . .
C201 C -0.02073(6) 0.01008(5) 0.66298(5) 0.0143(2) Uani 1 1 d . . . . .
C202 C 0.00299(6) -0.05909(6) 0.65746(5) 0.0168(2) Uani 1 1 d . . . . .
H202 H 0.0321 -0.0831 0.6833 0.020 Uiso 1 1 calc R U . . .
C203 C -0.01622(6) -0.09127(6) 0.61463(5) 0.0182(2) Uani 1 1 d . . . . .
H203 H -0.0006 -0.1380 0.6109 0.022 Uiso 1 1 calc R U . . .
C204 C -0.05931(6) -0.05542(6) 0.57564(5) 0.0163(2) Uani 1 1 d . . . . .
C205 C -0.07881(6) -0.08796(6) 0.53035(5) 0.0198(2) Uani 1 1 d . . . . .
H205 H -0.0619 -0.1342 0.5256 0.024 Uiso 1 1 calc R U . . .
C206 C -0.12132(7) -0.05414(6) 0.49343(5) 0.0219(3) Uani 1 1 d . . . . .
H206 H -0.1352 -0.0771 0.4642 0.026 Uiso 1 1 calc R U . . .
C207 C -0.14439(6) 0.01539(6) 0.49910(5) 0.0211(3) Uani 1 1 d . . . . .
H207 H -0.1734 0.0393 0.4731 0.025 Uiso 1 1 calc R U . . .
C208 C -0.12548(6) 0.04878(6) 0.54160(5) 0.0178(2) Uani 1 1 d . . . . .
H208 H -0.1404 0.0959 0.5438 0.021 Uiso 1 1 calc R U . . .
C209 C -0.08411(6) 0.01420(5) 0.58235(5) 0.0151(2) Uani 1 1 d . . . . .
C210 C -0.06527(6) 0.04735(5) 0.62866(5) 0.0138(2) Uani 1 1 d . . . . .
C211 C -0.03277(6) 0.16758(6) 0.63266(5) 0.0160(2) Uani 1 1 d . . . . .
C212 C -0.04816(7) 0.23883(6) 0.63532(5) 0.0198(2) Uani 1 1 d . . . . .
H212 H -0.0072 0.2696 0.6296 0.024 Uiso 1 1 calc R U . . .
C213 C -0.12275(7) 0.26294(6) 0.64623(5) 0.0227(3) Uani 1 1 d . . . . .
H213 H -0.1335 0.3110 0.6469 0.027 Uiso 1 1 calc R U . . .
C214 C -0.18388(6) 0.21697(6) 0.65645(5) 0.0197(2) Uani 1 1 d . . . . .
C215 C -0.26240(7) 0.24037(7) 0.67206(6) 0.0271(3) Uani 1 1 d . . . . .
H215 H -0.2738 0.2881 0.6743 0.033 Uiso 1 1 calc R U . . .
C216 C -0.32152(7) 0.19565(7) 0.68385(6) 0.0302(3) Uani 1 1 d . . . . .
H216 H -0.3736 0.2124 0.6941 0.036 Uiso 1 1 calc R U . . .
C217 C -0.30585(7) 0.12466(7) 0.68088(5) 0.0257(3) Uani 1 1 d . . . . .
H217 H -0.3474 0.0937 0.6895 0.031 Uiso 1 1 calc R U . . .
C218 C -0.23092(6) 0.09998(6) 0.66561(5) 0.0191(2) Uani 1 1 d . . . . .
H218 H -0.2213 0.0520 0.6639 0.023 Uiso 1 1 calc R U . . .
C219 C -0.16743(6) 0.14517(6) 0.65223(5) 0.0163(2) Uani 1 1 d . . . . .
C220 C -0.08838(6) 0.12058(5) 0.63732(5) 0.0146(2) Uani 1 1 d . . . . .
C301 C 0.37522(6) 0.34579(5) 0.62452(5) 0.0149(2) Uani 1 1 d . . . . .
C302 C 0.42296(6) 0.28992(6) 0.63933(5) 0.0194(2) Uani 1 1 d . . . . .
H302 H 0.4195 0.2464 0.6268 0.023 Uiso 1 1 calc R U . . .
C303 C 0.47418(7) 0.29819(6) 0.67158(6) 0.0228(3) Uani 1 1 d . . . . .
H303 H 0.5066 0.2604 0.6807 0.027 Uiso 1 1 calc R U . . .
C304 C 0.47957(6) 0.36239(6) 0.69163(5) 0.0195(2) Uani 1 1 d . . . . .
C305 C 0.53094(7) 0.37087(6) 0.72664(6) 0.0245(3) Uani 1 1 d . . . . .
H305 H 0.5641 0.3336 0.7353 0.029 Uiso 1 1 calc R U . . .
C306 C 0.53336(7) 0.43207(7) 0.74811(6) 0.0263(3) Uani 1 1 d . . . . .
H306 H 0.5680 0.4371 0.7715 0.032 Uiso 1 1 calc R U . . .
C307 C 0.48412(7) 0.48773(6) 0.73541(5) 0.0237(3) Uani 1 1 d . . . . .
H307 H 0.4856 0.5300 0.7507 0.028 Uiso 1 1 calc R U . . .
C308 C 0.43436(7) 0.48155(6) 0.70141(5) 0.0192(2) Uani 1 1 d . . . . .
H308 H 0.4016 0.5195 0.6935 0.023 Uiso 1 1 calc R U . . .
C309 C 0.43089(6) 0.41899(5) 0.67767(5) 0.0159(2) Uani 1 1 d . . . . .
C310 C 0.37929(6) 0.41003(5) 0.64216(5) 0.0147(2) Uani 1 1 d . . . . .
C311 C 0.24758(6) 0.45332(5) 0.64252(5) 0.0162(2) Uani 1 1 d . . . . .
C312 C 0.19555(7) 0.50493(6) 0.62645(6) 0.0218(3) Uani 1 1 d . . . . .
H312 H 0.1415 0.4960 0.6400 0.026 Uiso 1 1 calc R U . . .
C313 C 0.22213(7) 0.56712(6) 0.59183(6) 0.0236(3) Uani 1 1 d . . . . .
H313 H 0.1864 0.6016 0.5825 0.028 Uiso 1 1 calc R U . . .
C314 C 0.30241(7) 0.58082(6) 0.56966(5) 0.0198(2) Uani 1 1 d . . . . .
C315 C 0.33158(8) 0.64361(6) 0.53012(6) 0.0266(3) Uani 1 1 d . . . . .
H315 H 0.2963 0.6779 0.5196 0.032 Uiso 1 1 calc R U . . .
C316 C 0.40916(8) 0.65556(6) 0.50706(6) 0.0275(3) Uani 1 1 d . . . . .
H316 H 0.4275 0.6980 0.4809 0.033 Uiso 1 1 calc R U . . .
C317 C 0.46253(7) 0.60485(6) 0.52202(6) 0.0246(3) Uani 1 1 d . . . . .
H317 H 0.5166 0.6132 0.5054 0.030 Uiso 1 1 calc R U . . .
C318 C 0.43654(7) 0.54372(6) 0.56036(5) 0.0193(2) Uani 1 1 d . . . . .
H318 H 0.4729 0.5100 0.5700 0.023 Uiso 1 1 calc R U . . .
C319 C 0.35606(6) 0.53006(5) 0.58587(5) 0.0165(2) Uani 1 1 d . . . . .
C320 C 0.32644(6) 0.46623(5) 0.62497(5) 0.0150(2) Uani 1 1 d . . . . .
C321 C 0.31619(6) 0.33516(5) 0.59187(5) 0.0151(2) Uani 1 1 d . . . . .
H32A H 0.3164 0.3751 0.5585 0.018 Uiso 1 1 calc R U . . .
H32B H 0.3297 0.2930 0.5714 0.018 Uiso 1 1 calc R U . . .
C322 C 0.21508(6) 0.38444(5) 0.67865(5) 0.0190(2) Uani 1 1 d . . . . .
H32C H 0.2339 0.3726 0.7162 0.023 Uiso 1 1 calc R U . . .
H32D H 0.1578 0.3881 0.6938 0.023 Uiso 1 1 calc R U . . .
C323 C 0.20296(6) 0.26666(5) 0.66026(5) 0.0143(2) Uani 1 1 d . . . . .
C401 C 0.48517(6) 0.27905(5) 0.39514(5) 0.0152(2) Uani 1 1 d . . . . .
C402 C 0.56332(6) 0.28018(6) 0.35776(5) 0.0189(2) Uani 1 1 d . . . . .
H402 H 0.6031 0.2647 0.3764 0.023 Uiso 1 1 calc R U . . .
C403 C 0.58112(6) 0.30383(6) 0.29439(5) 0.0200(3) Uani 1 1 d . . . . .
H403 H 0.6337 0.3037 0.2687 0.024 Uiso 1 1 calc R U . . .
C404 C 0.52241(6) 0.32869(5) 0.26605(5) 0.0174(2) Uani 1 1 d . . . . .
C405 C 0.53992(7) 0.35064(6) 0.19974(5) 0.0213(3) Uani 1 1 d . . . . .
H405 H 0.5917 0.3469 0.1732 0.026 Uiso 1 1 calc R U . . .
C406 C 0.48342(7) 0.37714(6) 0.17342(5) 0.0228(3) Uani 1 1 d . . . . .
H406 H 0.4960 0.3919 0.1290 0.027 Uiso 1 1 calc R U . . .
C407 C 0.40636(7) 0.38256(6) 0.21248(5) 0.0223(3) Uani 1 1 d . . . . .
H407 H 0.3673 0.4013 0.1941 0.027 Uiso 1 1 calc R U . . .
C408 C 0.38720(6) 0.36113(6) 0.27654(5) 0.0187(2) Uani 1 1 d . . . . .
H408 H 0.3349 0.3648 0.3020 0.022 Uiso 1 1 calc R U . . .
C409 C 0.44440(6) 0.33347(5) 0.30560(5) 0.0151(2) Uani 1 1 d . . . . .
C410 C 0.42638(6) 0.30836(5) 0.37210(5) 0.0147(2) Uani 1 1 d . . . . .
C411 C 0.31249(6) 0.24884(6) 0.44971(5) 0.0160(2) Uani 1 1 d . . . . .
C412 C 0.23486(6) 0.24551(7) 0.48921(5) 0.0205(2) Uani 1 1 d . . . . .
H412 H 0.2122 0.2022 0.5101 0.025 Uiso 1 1 calc R U . . .
C413 C 0.19277(6) 0.30581(7) 0.49682(5) 0.0246(3) Uani 1 1 d . . . . .
H413 H 0.1399 0.3040 0.5219 0.030 Uiso 1 1 calc R U . . .
C414 C 0.22677(7) 0.37085(7) 0.46795(5) 0.0236(3) Uani 1 1 d . . . . .
C415 C 0.18663(8) 0.43445(7) 0.48038(6) 0.0350(3) Uani 1 1 d . . . . .
H415 H 0.1340 0.4337 0.5060 0.042 Uiso 1 1 calc R U . . .
C416 C 0.22243(9) 0.49609(8) 0.45612(7) 0.0419(4) Uani 1 1 d . . . . .
H416 H 0.1947 0.5379 0.4650 0.050 Uiso 1 1 calc R U . . .
C417 C 0.30051(9) 0.49856(7) 0.41783(7) 0.0364(4) Uani 1 1 d . . . . .
H417 H 0.3255 0.5419 0.4022 0.044 Uiso 1 1 calc R U . . .
C418 C 0.34064(8) 0.43864(6) 0.40307(6) 0.0255(3) Uani 1 1 d . . . . .
H418 H 0.3928 0.4409 0.3764 0.031 Uiso 1 1 calc R U . . .
C419 C 0.30474(6) 0.37327(6) 0.42742(5) 0.0183(2) Uani 1 1 d . . . . .
C420 C 0.34624(6) 0.30966(6) 0.41601(5) 0.0153(2) Uani 1 1 d . . . . .
C501 C 0.73083(6) 0.17567(5) 0.42698(5) 0.0162(2) Uani 1 1 d . . . . .
C502 C 0.73016(7) 0.17665(6) 0.49019(5) 0.0208(3) Uani 1 1 d . . . . .
H502 H 0.6885 0.1560 0.5244 0.025 Uiso 1 1 calc R U . . .
C503 C 0.78856(7) 0.20683(6) 0.50262(5) 0.0220(3) Uani 1 1 d . . . . .
H503 H 0.7862 0.2085 0.5453 0.026 Uiso 1 1 calc R U . . .
C504 C 0.85290(6) 0.23584(6) 0.45247(5) 0.0199(2) Uani 1 1 d . . . . .
C505 C 0.91722(7) 0.26236(7) 0.46444(6) 0.0289(3) Uani 1 1 d . . . . .
H505 H 0.9168 0.2625 0.5070 0.035 Uiso 1 1 calc R U . . .
C506 C 0.97986(7) 0.28777(8) 0.41558(6) 0.0319(3) Uani 1 1 d . . . . .
H506 H 1.0226 0.3053 0.4243 0.038 Uiso 1 1 calc R U . . .
C507 C 0.98132(7) 0.28813(7) 0.35235(6) 0.0257(3) Uani 1 1 d . . . . .
H507 H 1.0252 0.3056 0.3187 0.031 Uiso 1 1 calc R U . . .
C508 C 0.91995(6) 0.26345(6) 0.33892(5) 0.0188(2) Uani 1 1 d . . . . .
H508 H 0.9215 0.2645 0.2960 0.023 Uiso 1 1 calc R U . . .
C509 C 0.85396(6) 0.23634(5) 0.38848(5) 0.0157(2) Uani 1 1 d . . . . .
C510 C 0.79044(6) 0.20680(5) 0.37665(5) 0.0141(2) Uani 1 1 d . . . . .
C511 C 0.78233(6) 0.13932(5) 0.29482(5) 0.0144(2) Uani 1 1 d . . . . .
C512 C 0.77944(6) 0.13356(6) 0.23342(5) 0.0175(2) Uani 1 1 d . . . . .
H512 H 0.7772 0.0891 0.2222 0.021 Uiso 1 1 calc R U . . .
C513 C 0.77991(6) 0.19158(6) 0.19009(5) 0.0181(2) Uani 1 1 d . . . . .
H513 H 0.7805 0.1870 0.1484 0.022 Uiso 1 1 calc R U . . .
C514 C 0.77947(6) 0.25837(6) 0.20665(5) 0.0159(2) Uani 1 1 d . . . . .
C515 C 0.76999(6) 0.31902(6) 0.16520(5) 0.0185(2) Uani 1 1 d . . . . .
H515 H 0.7683 0.3152 0.1239 0.022 Uiso 1 1 calc R U . . .
C516 C 0.76330(6) 0.38289(6) 0.18380(5) 0.0191(2) Uani 1 1 d . . . . .
H516 H 0.7557 0.4227 0.1558 0.023 Uiso 1 1 calc R U . . .
C517 C 0.76759(6) 0.38992(6) 0.24446(5) 0.0192(2) Uani 1 1 d . . . . .
H517 H 0.7632 0.4345 0.2570 0.023 Uiso 1 1 calc R U . . .
C518 C 0.77805(6) 0.33232(6) 0.28537(5) 0.0166(2) Uani 1 1 d . . . . .
H518 H 0.7814 0.3376 0.3259 0.020 Uiso 1 1 calc R U . . .
C519 C 0.78385(6) 0.26523(5) 0.26796(5) 0.0142(2) Uani 1 1 d . . . . .
C520 C 0.78801(6) 0.20356(5) 0.31125(5) 0.0140(2) Uani 1 1 d . . . . .
C521 C 0.66869(6) 0.13773(5) 0.41398(5) 0.0185(2) Uani 1 1 d . . . . .
H52A H 0.6243 0.1287 0.4530 0.022 Uiso 1 1 calc R U . . .
H52B H 0.6498 0.1665 0.3809 0.022 Uiso 1 1 calc R U . . .
C522 C 0.77695(6) 0.07424(5) 0.34266(5) 0.0159(2) Uani 1 1 d . . . . .
H52C H 0.7835 0.0331 0.3209 0.019 Uiso 1 1 calc R U . . .
H52D H 0.8190 0.0735 0.3624 0.019 Uiso 1 1 calc R U . . .
C523 C 0.66786(6) 0.01151(6) 0.42206(5) 0.0167(2) Uani 1 1 d . . . . .
C601 C 0.54091(6) 0.22848(5) 1.07289(5) 0.0162(2) Uani 1 1 d . . . . .
C602 C 0.46056(6) 0.23935(6) 1.09699(5) 0.0200(2) Uani 1 1 d . . . . .
H602 H 0.4319 0.2625 1.0704 0.024 Uiso 1 1 calc R U . . .
C603 C 0.42446(7) 0.21575(6) 1.15974(6) 0.0227(3) Uani 1 1 d . . . . .
H603 H 0.3700 0.2219 1.1766 0.027 Uiso 1 1 calc R U . . .
C604 C 0.46747(7) 0.18238(6) 1.19956(5) 0.0205(3) Uani 1 1 d . . . . .
C605 C 0.43236(7) 0.16384(6) 1.26599(6) 0.0261(3) Uani 1 1 d . . . . .
H605 H 0.3787 0.1731 1.2839 0.031 Uiso 1 1 calc R U . . .
C606 C 0.47427(8) 0.13308(7) 1.30440(5) 0.0278(3) Uani 1 1 d . . . . .
H606 H 0.4499 0.1217 1.3487 0.033 Uiso 1 1 calc R U . . .
C607 C 0.55367(7) 0.11818(7) 1.27843(5) 0.0260(3) Uani 1 1 d . . . . .
H607 H 0.5825 0.0962 1.3054 0.031 Uiso 1 1 calc R U . . .
C608 C 0.58974(7) 0.13503(6) 1.21472(5) 0.0214(2) Uani 1 1 d . . . . .
H608 H 0.6432 0.1243 1.1979 0.026 Uiso 1 1 calc R U . . .
C609 C 0.54813(6) 0.16842(6) 1.17350(5) 0.0174(2) Uani 1 1 d . . . . .
C610 C 0.58510(6) 0.19119(5) 1.10729(5) 0.0163(2) Uani 1 1 d . . . . .
C611 C 0.71490(6) 0.23696(6) 1.04641(5) 0.0187(2) Uani 1 1 d . . . . .
C612 C 0.79539(6) 0.23196(7) 1.01605(5) 0.0224(3) Uani 1 1 d . . . . .
H612 H 0.8251 0.2725 0.9974 0.027 Uiso 1 1 calc R U . . .
C613 C 0.82998(7) 0.16787(7) 1.01391(5) 0.0263(3) Uani 1 1 d . . . . .
H613 H 0.8844 0.1641 0.9948 0.032 Uiso 1 1 calc R U . . .
C614 C 0.78552(7) 0.10706(7) 1.03983(5) 0.0231(3) Uani 1 1 d . . . . .
C615 C 0.81959(7) 0.04040(7) 1.03262(6) 0.0303(3) Uani 1 1 d . . . . .
H615 H 0.8738 0.0360 1.0132 0.036 Uiso 1 1 calc R U . . .
C616 C 0.77506(8) -0.01742(7) 1.05338(6) 0.0326(3) Uani 1 1 d . . . . .
H616 H 0.7985 -0.0618 1.0485 0.039 Uiso 1 1 calc R U . . .
C617 C 0.69452(8) -0.01165(7) 1.08196(6) 0.0288(3) Uani 1 1 d . . . . .
H617 H 0.6638 -0.0521 1.0950 0.035 Uiso 1 1 calc R U . . .
C618 C 0.65993(7) 0.05181(6) 1.09111(5) 0.0228(3) Uani 1 1 d . . . . .
H618 H 0.6057 0.0547 1.1113 0.027 Uiso 1 1 calc R U . . .
C619 C 0.70417(6) 0.11301(6) 1.07072(5) 0.0194(2) Uani 1 1 d . . . . .
C620 C 0.66937(6) 0.18039(6) 1.07586(5) 0.0169(2) Uani 1 1 d . . . . .
C701 C 0.78308(6) 0.03996(6) 0.85854(5) 0.0181(2) Uani 1 1 d . . . . .
C702 C 0.83523(7) -0.01292(6) 0.87172(6) 0.0238(3) Uani 1 1 d . . . . .
H702 H 0.8895 -0.0057 0.8547 0.029 Uiso 1 1 calc R U . . .
C703 C 0.80855(7) -0.07413(6) 0.90848(6) 0.0266(3) Uani 1 1 d . . . . .
H703 H 0.8444 -0.1097 0.9155 0.032 Uiso 1 1 calc R U . . .
C704 C 0.72807(7) -0.08531(6) 0.93626(5) 0.0222(3) Uani 1 1 d . . . . .
C705 C 0.69927(8) -0.14718(6) 0.97797(6) 0.0299(3) Uani 1 1 d . . . . .
H705 H 0.7347 -0.1827 0.9859 0.036 Uiso 1 1 calc R U . . .
C706 C 0.62202(9) -0.15632(7) 1.00666(6) 0.0319(3) Uani 1 1 d . . . . .
H706 H 0.6039 -0.1982 1.0339 0.038 Uiso 1 1 calc R U . . .
C707 C 0.56867(8) -0.10345(6) 0.99592(6) 0.0274(3) Uani 1 1 d . . . . .
H707 H 0.5148 -0.1096 1.0168 0.033 Uiso 1 1 calc R U . . .
C708 C 0.59401(7) -0.04353(6) 0.95573(5) 0.0211(3) Uani 1 1 d . . . . .
H708 H 0.5574 -0.0086 0.9489 0.025 Uiso 1 1 calc R U . . .
C709 C 0.67438(6) -0.03262(6) 0.92394(5) 0.0175(2) Uani 1 1 d . . . . .
C710 C 0.70352(6) 0.02979(5) 0.88221(5) 0.0153(2) Uani 1 1 d . . . . .
C711 C 0.66006(6) 0.15215(5) 0.87996(5) 0.0139(2) Uani 1 1 d . . . . .
C712 C 0.61029(6) 0.20811(6) 0.86843(5) 0.0171(2) Uani 1 1 d . . . . .
H712 H 0.6179 0.2526 0.8773 0.021 Uiso 1 1 calc R U . . .
C713 C 0.55142(6) 0.19821(6) 0.84459(5) 0.0197(2) Uani 1 1 d . . . . .
H713 H 0.5170 0.2355 0.8387 0.024 Uiso 1 1 calc R U . . .
C714 C 0.54090(6) 0.13310(6) 0.82852(5) 0.0182(2) Uani 1 1 d . . . . .
C715 C 0.48228(7) 0.12327(7) 0.80066(6) 0.0250(3) Uani 1 1 d . . . . .
H715 H 0.4476 0.1603 0.7945 0.030 Uiso 1 1 calc R U . . .
C716 C 0.47538(7) 0.06128(7) 0.78267(6) 0.0286(3) Uani 1 1 d . . . . .
H716 H 0.4355 0.0552 0.7647 0.034 Uiso 1 1 calc R U . . .
C717 C 0.52710(7) 0.00612(7) 0.79066(6) 0.0259(3) Uani 1 1 d . . . . .
H717 H 0.5228 -0.0364 0.7768 0.031 Uiso 1 1 calc R U . . .
C718 C 0.58356(7) 0.01341(6) 0.81821(5) 0.0202(2) Uani 1 1 d . . . . .
H718 H 0.6177 -0.0243 0.8236 0.024 Uiso 1 1 calc R U . . .
C719 C 0.59150(6) 0.07683(6) 0.83873(5) 0.0162(2) Uani 1 1 d . . . . .
C720 C 0.65036(6) 0.08687(5) 0.86730(5) 0.0143(2) Uani 1 1 d . . . . .
C721 C 0.81640(7) 0.10684(6) 0.81803(5) 0.0200(2) Uani 1 1 d . . . . .
H72A H 0.8731 0.1009 0.7995 0.024 Uiso 1 1 calc R U . . .
H72B H 0.7935 0.1178 0.7827 0.024 Uiso 1 1 calc R U . . .
C722 C 0.72567(6) 0.16331(6) 0.90552(5) 0.0154(2) Uani 1 1 d . . . . .
H72C H 0.7169 0.2073 0.9232 0.018 Uiso 1 1 calc R U . . .
H72D H 0.7268 0.1253 0.9402 0.018 Uiso 1 1 calc R U . . .
C723 C 0.84086(6) 0.22432(6) 0.83088(5) 0.0168(2) Uani 1 1 d . . . . .
C801 C 1.05104(6) 0.33968(6) 0.85879(5) 0.0184(2) Uani 1 1 d . . . . .
C802 C 1.06529(8) 0.26773(6) 0.86313(5) 0.0241(3) Uani 1 1 d . . . . .
H802 H 1.0251 0.2370 0.8665 0.029 Uiso 1 1 calc R U . . .
C803 C 1.13747(8) 0.24272(6) 0.86251(6) 0.0265(3) Uani 1 1 d . . . . .
H803 H 1.1472 0.1942 0.8664 0.032 Uiso 1 1 calc R U . . .
C804 C 1.19808(7) 0.28845(6) 0.85616(5) 0.0233(3) Uani 1 1 d . . . . .
C805 C 1.27448(8) 0.26372(7) 0.85180(6) 0.0323(3) Uani 1 1 d . . . . .
H805 H 1.2851 0.2154 0.8547 0.039 Uiso 1 1 calc R U . . .
C806 C 1.33284(8) 0.30807(8) 0.84359(6) 0.0359(4) Uani 1 1 d . . . . .
H806 H 1.3837 0.2905 0.8406 0.043 Uiso 1 1 calc R U . . .
C807 C 1.31821(7) 0.37983(8) 0.83945(6) 0.0303(3) Uani 1 1 d . . . . .
H807 H 1.3595 0.4105 0.8329 0.036 Uiso 1 1 calc R U . . .
C808 C 1.24449(6) 0.40584(7) 0.84485(5) 0.0228(3) Uani 1 1 d . . . . .
H808 H 1.2353 0.4544 0.8424 0.027 Uiso 1 1 calc R U . . .
C809 C 1.18221(6) 0.36113(6) 0.85404(5) 0.0192(2) Uani 1 1 d . . . . .
C810 C 1.10511(6) 0.38676(6) 0.85776(5) 0.0167(2) Uani 1 1 d . . . . .
C811 C 1.05089(6) 0.49450(6) 0.81119(5) 0.0175(2) Uani 1 1 d . . . . .
C812 C 1.02977(6) 0.56502(6) 0.80625(6) 0.0224(3) Uani 1 1 d . . . . .
H812 H 1.0105 0.5862 0.7726 0.027 Uiso 1 1 calc R U . . .
C813 C 1.03723(6) 0.60288(6) 0.85030(6) 0.0241(3) Uani 1 1 d . . . . .
H813 H 1.0239 0.6508 0.8467 0.029 Uiso 1 1 calc R U . . .
C814 C 1.06456(6) 0.57138(6) 0.90116(6) 0.0213(3) Uani 1 1 d . . . . .
C815 C 1.06973(7) 0.60929(6) 0.94898(6) 0.0277(3) Uani 1 1 d . . . . .
H815 H 1.0552 0.6569 0.9464 0.033 Uiso 1 1 calc R U . . .
C816 C 1.09500(8) 0.57858(7) 0.99823(6) 0.0300(3) Uani 1 1 d . . . . .
H816 H 1.0984 0.6048 1.0295 0.036 Uiso 1 1 calc R U . . .
C817 C 1.11614(7) 0.50766(7) 1.00292(6) 0.0285(3) Uani 1 1 d . . . . .
H817 H 1.1332 0.4861 1.0377 0.034 Uiso 1 1 calc R U . . .
C818 C 1.11221(7) 0.46970(6) 0.95757(5) 0.0224(3) Uani 1 1 d . . . . .
H818 H 1.1265 0.4220 0.9615 0.027 Uiso 1 1 calc R U . . .
C819 C 1.08734(6) 0.50008(6) 0.90500(5) 0.0183(2) Uani 1 1 d . . . . .
C820 C 1.08248(6) 0.46141(5) 0.85714(5) 0.0164(2) Uani 1 1 d . . . . .
O91 O 0.43590(6) 0.09531(6) 0.64259(5) 0.0388(3) Uani 1 1 d D . . . .
H91 H 0.4227 0.1217 0.6140 0.058 Uiso 1 1 calc R U . . .
C91 C 0.51548(9) 0.07867(11) 0.62015(8) 0.0512(5) Uani 1 1 d D . . . .
H91A H 0.5462 0.1194 0.6169 0.077 Uiso 1 1 calc R U . . .
H91B H 0.5270 0.0643 0.5783 0.077 Uiso 1 1 calc R U . . .
H91C H 0.5286 0.0408 0.6497 0.077 Uiso 1 1 calc R U . . .
O92 O 0.44981(5) 0.39107(5) 0.98753(4) 0.0301(2) Uani 1 1 d D . . . .
H92 H 0.4884 0.3861 1.0012 0.045 Uiso 1 1 calc R U . . .
C92 C 0.47483(11) 0.41026(14) 0.92097(8) 0.0715(7) Uani 1 1 d D . . . .
H92A H 0.4320 0.4330 0.9069 0.107 Uiso 1 1 calc R U . . .
H92B H 0.4916 0.3689 0.9007 0.107 Uiso 1 1 calc R U . . .
H92C H 0.5182 0.4423 0.9091 0.107 Uiso 1 1 calc R U . . .
O93 O 0.30668(8) 0.02631(7) 0.73115(6) 0.0626(4) Uani 1 1 d D . . . .
H93 H 0.3441 0.0441 0.7013 0.094 Uiso 1 1 calc R U . . .
C93 C 0.26610(11) 0.07785(12) 0.76566(8) 0.0625(6) Uani 1 1 d D . . . .
H93A H 0.2593 0.0630 0.8109 0.094 Uiso 1 1 calc R U . . .
H93B H 0.2152 0.0856 0.7588 0.094 Uiso 1 1 calc R U . . .
H93C H 0.2954 0.1209 0.7514 0.094 Uiso 1 1 calc R U . . .
O94 O 0.8217(2) 0.45732(19) 0.70535(16) 0.0681(10) Uiso 0.412(2) 1 d D . P A 1
H94 H 0.8410 0.4504 0.7355 0.102 Uiso 0.412(2) 1 calc R U P A 1
C94 C 0.7461(2) 0.4423(2) 0.7273(2) 0.0437(9) Uiso 0.412(2) 1 d D . P A 1
H94E H 0.7399 0.3934 0.7461 0.066 Uiso 0.412(2) 1 calc R U P A 1
H94F H 0.7233 0.4512 0.6923 0.066 Uiso 0.412(2) 1 calc R U P A 1
H94G H 0.7199 0.4712 0.7597 0.066 Uiso 0.412(2) 1 calc R U P A 1
O94A O 0.81722(12) 0.41454(11) 0.70612(10) 0.0515(5) Uiso 0.588(2) 1 d D . P A
2
H94D H 0.8441 0.4160 0.7305 0.077 Uiso 0.588(2) 1 calc R U P A 2
C94A C 0.73745(17) 0.42394(16) 0.73937(14) 0.0464(7) Uiso 0.588(2) 1 d D . P A
2
H94A H 0.7225 0.3891 0.7775 0.070 Uiso 0.588(2) 1 calc R U P A 2
H94B H 0.7058 0.4188 0.7119 0.070 Uiso 0.588(2) 1 calc R U P A 2
H94C H 0.7292 0.4703 0.7516 0.070 Uiso 0.588(2) 1 calc R U P A 2
C95 C 1.0392(2) 0.02957(19) 0.87711(18) 0.0688(10) Uiso 0.58584(9) 1 d D . P B
3
H95A H 1.0958 0.0327 0.8645 0.103 Uiso 0.58584(9) 1 calc R U P B 3
H95B H 1.0245 0.0019 0.8499 0.103 Uiso 0.58584(9) 1 calc R U P B 3
H95C H 1.0200 0.0076 0.9214 0.103 Uiso 0.58584(9) 1 calc R U P B 3
O95 O 1.00514(13) 0.09932(11) 0.87033(10) 0.0570(6) Uiso 0.58584(9) 1 d D . P B
3
H95 H 0.9802 0.1090 0.9063 0.086 Uiso 0.58584(9) 1 calc R U P B 3
O95A O 1.0614(3) 0.0813(3) 0.8519(3) 0.0619(14) Uiso 0.24232(9) 1 d D . P C 4
H95G H 1.0588 0.0814 0.8899 0.093 Uiso 0.24232(9) 1 calc R U P C 4
C95A C 1.0900(6) 0.0103(4) 0.8333(5) 0.080(3) Uiso 0.24232(9) 1 d D . P C 4
H95D H 1.0472 -0.0141 0.8281 0.120 Uiso 0.24232(9) 1 calc R U P C 4
H95E H 1.1089 -0.0168 0.8666 0.120 Uiso 0.24232(9) 1 calc R U P C 4
H95F H 1.1322 0.0162 0.7932 0.120 Uiso 0.24232(9) 1 calc R U P C 4
O95B O 1.0228(7) 0.0863(6) 0.9699(5) 0.113(4) Uiso 0.17187(9) 1 d D . P D 5
H95K H 1.0023 0.1259 0.9673 0.170 Uiso 0.17187(9) 1 calc R U P D 5
C95B C 1.0349(4) 0.0551(4) 0.9036(3) 0.0257(14) Uiso 0.17187(9) 1 d D . P D 5
H95H H 1.0840 0.0290 0.8933 0.039 Uiso 0.17187(9) 1 calc R U P D 5
H94I H 1.0361 0.0934 0.8692 0.039 Uiso 0.17187(9) 1 calc R U P D 5
H95J H 0.9920 0.0244 0.9088 0.039 Uiso 0.17187(9) 1 calc R U P D 5
O96 O -0.0249(3) 0.5951(2) 0.3910(2) 0.1897(18) Uiso 0.7125(13) 1 d . . P E 6
H96 H -0.0178 0.6103 0.3524 0.284 Uiso 0.7125(13) 1 calc R U P E 6
C96 C 0.0203(4) 0.5214(3) 0.3979(3) 0.169(2) Uiso 0.7125(13) 1 d . . P E 6
H96A H 0.0751 0.5295 0.3920 0.253 Uiso 0.7125(13) 1 calc R U P E 6
H96B H 0.0160 0.4947 0.3657 0.253 Uiso 0.7125(13) 1 calc R U P E 6
H96C H -0.0030 0.4954 0.4402 0.253 Uiso 0.7125(13) 1 calc R U P E 6
C991 C -0.0036(3) 0.5173(2) 0.56601(15) 0.0542(6) Uiso 0.2875(13) 1 d DG U P E
-7
C992 C 0.0300(3) 0.5602(2) 0.50936(16) 0.0542(6) Uiso 0.2875(13) 1 d G U P E -7
H992 H 0.0498 0.6038 0.5099 0.065 Uiso 0.2875(13) 1 calc R U P E -7
C993 C 0.0345(3) 0.5394(3) 0.45188(15) 0.0542(6) Uiso 0.2875(13) 1 d G U P E -7
H993 H 0.0574 0.5687 0.4132 0.065 Uiso 0.2875(13) 1 calc R U P E -7
C994 C 0.0054(4) 0.4756(3) 0.45105(17) 0.0542(6) Uiso 0.2875(13) 1 d G U P E -7
H994 H 0.0084 0.4613 0.4118 0.065 Uiso 0.2875(13) 1 calc R U P E -7
C995 C -0.0282(3) 0.4327(3) 0.5077(2) 0.0542(6) Uiso 0.2875(13) 1 d G U P E -7
H995 H -0.0481 0.3891 0.5071 0.065 Uiso 0.2875(13) 1 calc R U P E -7
C996 C -0.0327(3) 0.4535(2) 0.56518(17) 0.0542(6) Uiso 0.2875(13) 1 d G U P E
-7
H996 H -0.0556 0.4242 0.6039 0.065 Uiso 0.2875(13) 1 calc R U P E -7
C997 C -0.0113(4) 0.5381(3) 0.6210(3) 0.0563(16) Uiso 0.2875(13) 1 d D . P E -7
H99A H 0.0261 0.5746 0.6149 0.084 Uiso 0.2875(13) 1 calc R U P E -7
H99B H -0.0017 0.4989 0.6511 0.084 Uiso 0.2875(13) 1 calc R U P E -7
H99C H -0.0640 0.5562 0.6378 0.084 Uiso 0.2875(13) 1 calc R U P E -7


_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
P2 O204 1.4785(8) . ?
P2 O203 1.4925(8) . ?
P2 O201 1.6040(8) . ?
P2 O202 1.6147(8) . ?
P4 O403 1.4846(8) . ?
P4 O404 1.4998(7) . ?
P4 O401 1.6052(8) . ?
P4 O402 1.6159(9) . ?
P6 O604 1.4879(8) . ?
P6 O603 1.4881(8) . ?
P6 O601 1.6093(8) . ?
P6 O602 1.6108(9) . ?
P8 O803 1.4844(9) . ?
P8 O804 1.4860(8) . ?
P8 O802 1.6068(8) . ?
P8 O801 1.6147(9) . ?
O201 C201 1.3994(14) . ?
O202 C211 1.3959(13) . ?
O401 C401 1.4022(12) . ?
O402 C411 1.4025(13) . ?
O601 C601 1.4045(12) . ?
O602 C611 1.3990(14) . ?
O801 C801 1.3971(14) . ?
O802 C811 1.3986(14) . ?
N101 C123 1.3423(14) . ?
N101 C121 1.4774(14) . ?
N101 C122 1.4843(13) . ?
N102 C123 1.3288(14) . ?
N103 C123 1.3331(14) . ?
N301 C323 1.3410(13) . ?
N301 C321 1.4797(12) . ?
N301 C322 1.4942(14) . ?
N302 C323 1.3349(14) . ?
N303 C323 1.3341(13) . ?
N501 C523 1.3297(13) . ?
N501 C521 1.4776(13) . ?
N501 C522 1.4849(12) . ?
N502 C523 1.3400(13) . ?
N503 C523 1.3328(14) . ?
N701 C723 1.3405(14) . ?
N701 C722 1.4795(12) . ?
N701 C721 1.4901(14) . ?
N702 C723 1.3286(13) . ?
N703 C723 1.3358(14) . ?
C101 C110 1.3897(14) . ?
C101 C102 1.4134(17) . ?
C101 C121 1.5037(17) . ?
C102 C103 1.3629(19) . ?
C103 C104 1.4132(15) . ?
C104 C105 1.4190(18) . ?
C104 C109 1.4276(16) . ?
C105 C106 1.3606(17) . ?
C106 C107 1.4121(18) . ?
C107 C108 1.3690(18) . ?
C108 C109 1.4206(14) . ?
C109 C110 1.4376(16) . ?
C110 C120 1.4921(16) . ?
C111 C120 1.3883(16) . ?
C111 C112 1.4155(17) . ?
C111 C122 1.5144(15) . ?
C112 C113 1.3674(17) . ?
C113 C114 1.4168(17) . ?
C114 C115 1.4179(16) . ?
C114 C119 1.4300(16) . ?
C115 C116 1.3628(18) . ?
C116 C117 1.4171(18) . ?
C117 C118 1.3729(16) . ?
C118 C119 1.4182(16) . ?
C119 C120 1.4338(15) . ?
C201 C210 1.3779(15) . ?
C201 C202 1.4084(15) . ?
C202 C203 1.3654(17) . ?
C203 C204 1.4194(16) . ?
C204 C205 1.4193(17) . ?
C204 C209 1.4252(15) . ?
C205 C206 1.3653(17) . ?
C206 C207 1.4131(17) . ?
C207 C208 1.3706(17) . ?
C208 C209 1.4172(16) . ?
C209 C210 1.4401(16) . ?
C210 C220 1.4946(15) . ?
C211 C220 1.3754(16) . ?
C211 C212 1.4127(15) . ?
C212 C213 1.3657(16) . ?
C213 C214 1.4109(17) . ?
C214 C215 1.4224(16) . ?
C214 C219 1.4309(16) . ?
C215 C216 1.3607(19) . ?
C216 C217 1.409(2) . ?
C217 C218 1.3719(16) . ?
C218 C219 1.4230(16) . ?
C219 C220 1.4384(14) . ?
C301 C310 1.3900(15) . ?
C301 C302 1.4127(15) . ?
C301 C321 1.5085(16) . ?
C302 C303 1.3692(18) . ?
C303 C304 1.4193(17) . ?
C304 C305 1.4194(18) . ?
C304 C309 1.4281(15) . ?
C305 C306 1.3689(19) . ?
C306 C307 1.4139(18) . ?
C307 C308 1.3673(18) . ?
C308 C309 1.4235(16) . ?
C309 C310 1.4341(16) . ?
C310 C320 1.4946(15) . ?
C311 C320 1.3888(15) . ?
C311 C312 1.4181(16) . ?
C311 C322 1.5080(14) . ?
C312 C313 1.3619(16) . ?
C313 C314 1.4135(17) . ?
C314 C315 1.4201(16) . ?
C314 C319 1.4297(16) . ?
C315 C316 1.3620(19) . ?
C316 C317 1.4158(18) . ?
C317 C318 1.3716(15) . ?
C318 C319 1.4190(15) . ?
C319 C320 1.4347(14) . ?
C401 C410 1.3764(15) . ?
C401 C402 1.4069(14) . ?
C402 C403 1.3634(16) . ?
C403 C404 1.4210(17) . ?
C404 C405 1.4188(15) . ?
C404 C409 1.4269(14) . ?
C405 C406 1.3670(18) . ?
C406 C407 1.4111(16) . ?
C407 C408 1.3686(15) . ?
C408 C409 1.4212(16) . ?
C409 C410 1.4324(14) . ?
C410 C420 1.4855(13) . ?
C411 C420 1.3708(15) . ?
C411 C412 1.4133(14) . ?
C412 C413 1.3705(17) . ?
C413 C414 1.4164(18) . ?
C414 C419 1.4257(15) . ?
C414 C415 1.4258(18) . ?
C415 C416 1.357(2) . ?
C416 C417 1.412(2) . ?
C417 C418 1.3735(18) . ?
C418 C419 1.4208(16) . ?
C419 C420 1.4320(15) . ?
C501 C510 1.3870(13) . ?
C501 C502 1.4149(16) . ?
C501 C521 1.5091(16) . ?
C502 C503 1.3625(18) . ?
C503 C504 1.4208(15) . ?
C504 C505 1.4177(18) . ?
C504 C509 1.4255(16) . ?
C505 C506 1.3667(17) . ?
C506 C507 1.4069(18) . ?
C507 C508 1.3703(17) . ?
C508 C509 1.4214(14) . ?
C509 C510 1.4307(16) . ?
C510 C520 1.4898(15) . ?
C511 C520 1.3842(15) . ?
C511 C512 1.4144(16) . ?
C511 C522 1.5136(14) . ?
C512 C513 1.3683(15) . ?
C513 C514 1.4143(16) . ?
C514 C515 1.4202(15) . ?
C514 C519 1.4269(15) . ?
C515 C516 1.3675(17) . ?
C516 C517 1.4129(17) . ?
C517 C518 1.3758(15) . ?
C518 C519 1.4182(15) . ?
C519 C520 1.4347(14) . ?
C601 C610 1.3749(16) . ?
C601 C602 1.4051(15) . ?
C602 C603 1.3718(16) . ?
C603 C604 1.4151(18) . ?
C604 C605 1.4230(16) . ?
C604 C609 1.4253(15) . ?
C605 C606 1.3615(19) . ?
C606 C607 1.4088(18) . ?
C607 C608 1.3698(15) . ?
C608 C609 1.4201(17) . ?
C609 C610 1.4360(14) . ?
C610 C620 1.4908(14) . ?
C611 C620 1.3734(15) . ?
C611 C612 1.4131(15) . ?
C612 C613 1.3686(18) . ?
C613 C614 1.4187(18) . ?
C614 C615 1.4204(18) . ?
C614 C619 1.4303(15) . ?
C615 C616 1.365(2) . ?
C616 C617 1.4086(19) . ?
C617 C618 1.3731(17) . ?
C618 C619 1.4160(17) . ?
C619 C620 1.4327(16) . ?
C701 C710 1.3902(15) . ?
C701 C702 1.4151(16) . ?
C701 C721 1.5103(15) . ?
C702 C703 1.3628(17) . ?
C703 C704 1.4150(17) . ?
C704 C705 1.4237(16) . ?
C704 C709 1.4262(16) . ?
C705 C706 1.359(2) . ?
C706 C707 1.4148(19) . ?
C707 C708 1.3675(16) . ?
C708 C709 1.4243(16) . ?
C709 C710 1.4332(14) . ?
C710 C720 1.4937(15) . ?
C711 C720 1.3855(15) . ?
C711 C712 1.4171(15) . ?
C711 C722 1.5088(16) . ?
C712 C713 1.3665(17) . ?
C713 C714 1.4180(17) . ?
C714 C715 1.4223(17) . ?
C714 C719 1.4241(15) . ?
C715 C716 1.3631(19) . ?
C716 C717 1.4110(18) . ?
C717 C718 1.3709(18) . ?
C718 C719 1.4211(16) . ?
C719 C720 1.4382(16) . ?
C801 C810 1.3785(16) . ?
C801 C802 1.4093(16) . ?
C802 C803 1.3645(19) . ?
C803 C804 1.4187(19) . ?
C804 C805 1.4176(18) . ?
C804 C809 1.4301(16) . ?
C805 C806 1.360(2) . ?
C806 C807 1.407(2) . ?
C807 C808 1.3766(17) . ?
C808 C809 1.4155(17) . ?
C809 C810 1.4371(16) . ?
C810 C820 1.4923(15) . ?
C811 C820 1.3801(16) . ?
C811 C812 1.4056(16) . ?
C812 C813 1.3676(19) . ?
C813 C814 1.4152(18) . ?
C814 C815 1.4256(19) . ?
C814 C819 1.4275(16) . ?
C815 C816 1.359(2) . ?
C816 C817 1.4132(19) . ?
C817 C818 1.3720(18) . ?
C818 C819 1.4169(17) . ?
C819 C820 1.4341(17) . ?
O91 C91 1.4106(18) . ?
O92 C92 1.4126(19) . ?
O93 C93 1.403(2) . ?
O94 C94 1.339(5) . ?
O94A C94A 1.425(3) . ?
C95 O95 1.468(4) . ?
O95A C95A 1.530(10) . ?
O95B C95B 1.642(11) . ?
O96 C96 1.624(7) . ?
C991 C997 1.324(7) . ?
C991 C992 1.3900 . ?
C991 C996 1.3900 . ?
C992 C993 1.3900 . ?
C993 C994 1.3900 . ?
C994 C995 1.3900 . ?
C995 C996 1.3900 . ?

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
O204 P2 O203 118.39(5) . . ?
O204 P2 O201 114.07(4) . . ?
O203 P2 O201 104.36(4) . . ?
O204 P2 O202 104.95(4) . . ?
O203 P2 O202 110.98(4) . . ?
O201 P2 O202 103.17(4) . . ?
O403 P4 O404 117.37(4) . . ?
O403 P4 O401 112.88(4) . . ?
O404 P4 O401 105.59(4) . . ?
O403 P4 O402 107.18(5) . . ?
O404 P4 O402 109.42(4) . . ?
O401 P4 O402 103.54(4) . . ?
O604 P6 O603 117.87(5) . . ?
O604 P6 O601 111.91(4) . . ?
O603 P6 O601 105.55(4) . . ?
O604 P6 O602 106.11(5) . . ?
O603 P6 O602 111.31(5) . . ?
O601 P6 O602 103.19(4) . . ?
O803 P8 O804 118.37(5) . . ?
O803 P8 O802 105.90(4) . . ?
O804 P8 O802 112.98(5) . . ?
O803 P8 O801 111.16(5) . . ?
O804 P8 O801 104.47(5) . . ?
O802 P8 O801 102.97(4) . . ?
C201 O201 P2 120.61(6) . . ?
C211 O202 P2 116.87(6) . . ?
C401 O401 P4 118.87(7) . . ?
C411 O402 P4 116.05(7) . . ?
C601 O601 P6 116.92(7) . . ?
C611 O602 P6 116.24(7) . . ?
C801 O801 P8 115.42(6) . . ?
C811 O802 P8 119.78(6) . . ?
C123 N101 C121 121.85(9) . . ?
C123 N101 C122 122.07(9) . . ?
C121 N101 C122 115.90(8) . . ?
C323 N301 C321 122.31(9) . . ?
C323 N301 C322 118.74(8) . . ?
C321 N301 C322 114.76(8) . . ?
C523 N501 C521 121.37(8) . . ?
C523 N501 C522 121.26(9) . . ?
C521 N501 C522 116.82(8) . . ?
C723 N701 C722 122.32(9) . . ?
C723 N701 C721 119.51(8) . . ?
C722 N701 C721 114.94(8) . . ?
C110 C101 C102 120.37(11) . . ?
C110 C101 C121 119.56(11) . . ?
C102 C101 C121 120.02(10) . . ?
C103 C102 C101 121.00(10) . . ?
C102 C103 C104 120.65(11) . . ?
C103 C104 C105 120.93(11) . . ?
C103 C104 C109 119.60(11) . . ?
C105 C104 C109 119.46(10) . . ?
C106 C105 C104 120.95(12) . . ?
C105 C106 C107 119.81(12) . . ?
C108 C107 C106 120.97(11) . . ?
C107 C108 C109 120.75(11) . . ?
C108 C109 C104 118.02(10) . . ?
C108 C109 C110 123.16(10) . . ?
C104 C109 C110 118.79(9) . . ?
C101 C110 C109 119.57(10) . . ?
C101 C110 C120 117.86(10) . . ?
C109 C110 C120 122.35(9) . . ?
C120 C111 C112 120.49(10) . . ?
C120 C111 C122 120.45(10) . . ?
C112 C111 C122 119.05(10) . . ?
C113 C112 C111 120.60(11) . . ?
C112 C113 C114 120.69(11) . . ?
C113 C114 C115 121.78(11) . . ?
C113 C114 C119 119.39(10) . . ?
C115 C114 C119 118.77(11) . . ?
C116 C115 C114 121.28(11) . . ?
C115 C116 C117 120.09(11) . . ?
C118 C117 C116 120.30(11) . . ?
C117 C118 C119 120.86(11) . . ?
C118 C119 C114 118.67(10) . . ?
C118 C119 C120 122.42(10) . . ?
C114 C119 C120 118.83(10) . . ?
C111 C120 C119 119.56(10) . . ?
C111 C120 C110 117.99(9) . . ?
C119 C120 C110 122.31(10) . . ?
N101 C121 C101 110.16(9) . . ?
N101 C122 C111 110.33(9) . . ?
N102 C123 N103 118.57(10) . . ?
N102 C123 N101 120.79(10) . . ?
N103 C123 N101 120.64(9) . . ?
C210 C201 O201 119.59(9) . . ?
C210 C201 C202 123.46(10) . . ?
O201 C201 C202 116.90(9) . . ?
C203 C202 C201 119.39(10) . . ?
C202 C203 C204 120.52(10) . . ?
C205 C204 C203 121.09(10) . . ?
C205 C204 C209 119.29(10) . . ?
C203 C204 C209 119.62(10) . . ?
C206 C205 C204 121.38(11) . . ?
C205 C206 C207 119.30(11) . . ?
C208 C207 C206 120.87(11) . . ?
C207 C208 C209 121.13(11) . . ?
C208 C209 C204 117.96(10) . . ?
C208 C209 C210 122.39(10) . . ?
C204 C209 C210 119.64(10) . . ?
C201 C210 C209 117.29(9) . . ?
C201 C210 C220 120.33(10) . . ?
C209 C210 C220 122.28(9) . . ?
C220 C211 O202 119.36(9) . . ?
C220 C211 C212 123.76(10) . . ?
O202 C211 C212 116.88(10) . . ?
C213 C212 C211 119.13(11) . . ?
C212 C213 C214 120.42(11) . . ?
C213 C214 C215 121.20(11) . . ?
C213 C214 C219 119.93(10) . . ?
C215 C214 C219 118.86(11) . . ?
C216 C215 C214 121.20(12) . . ?
C215 C216 C217 120.26(11) . . ?
C218 C217 C216 120.44(12) . . ?
C217 C218 C219 121.04(11) . . ?
C218 C219 C214 118.19(10) . . ?
C218 C219 C220 122.27(10) . . ?
C214 C219 C220 119.49(10) . . ?
C211 C220 C219 116.95(10) . . ?
C211 C220 C210 119.74(9) . . ?
C219 C220 C210 123.29(10) . . ?
C310 C301 C302 120.92(11) . . ?
C310 C301 C321 119.12(9) . . ?
C302 C301 C321 119.90(10) . . ?
C303 C302 C301 120.34(11) . . ?
C302 C303 C304 120.92(11) . . ?
C303 C304 C305 121.31(11) . . ?
C303 C304 C309 119.26(11) . . ?
C305 C304 C309 119.41(11) . . ?
C306 C305 C304 120.90(11) . . ?
C305 C306 C307 119.78(12) . . ?
C308 C307 C306 120.88(12) . . ?
C307 C308 C309 120.93(11) . . ?
C308 C309 C304 118.08(11) . . ?
C308 C309 C310 122.84(10) . . ?
C304 C309 C310 119.05(10) . . ?
C301 C310 C309 119.46(10) . . ?
C301 C310 C320 117.50(10) . . ?
C309 C310 C320 122.99(9) . . ?
C320 C311 C312 120.46(10) . . ?
C320 C311 C322 121.23(10) . . ?
C312 C311 C322 118.31(10) . . ?
C313 C312 C311 120.74(10) . . ?
C312 C313 C314 120.62(11) . . ?
C313 C314 C315 121.43(11) . . ?
C313 C314 C319 119.77(10) . . ?
C315 C314 C319 118.79(11) . . ?
C316 C315 C314 121.22(12) . . ?
C315 C316 C317 120.14(11) . . ?
C318 C317 C316 120.33(11) . . ?
C317 C318 C319 120.93(11) . . ?
C318 C319 C314 118.57(9) . . ?
C318 C319 C320 122.76(10) . . ?
C314 C319 C320 118.62(10) . . ?
C311 C320 C319 119.58(10) . . ?
C311 C320 C310 118.65(9) . . ?
C319 C320 C310 121.49(9) . . ?
N301 C321 C301 109.85(8) . . ?
N301 C322 C311 111.92(8) . . ?
N303 C323 N302 117.98(9) . . ?
N303 C323 N301 120.10(9) . . ?
N302 C323 N301 121.92(9) . . ?
C410 C401 O401 119.03(8) . . ?
C410 C401 C402 122.67(10) . . ?
O401 C401 C402 118.25(10) . . ?
C403 C402 C401 119.05(11) . . ?
C402 C403 C404 121.13(9) . . ?
C405 C404 C403 121.56(10) . . ?
C405 C404 C409 119.37(10) . . ?
C403 C404 C409 119.05(10) . . ?
C406 C405 C404 120.97(10) . . ?
C405 C406 C407 119.79(10) . . ?
C408 C407 C406 120.82(11) . . ?
C407 C408 C409 120.97(10) . . ?
C408 C409 C404 118.07(9) . . ?
C408 C409 C410 122.73(9) . . ?
C404 C409 C410 119.16(10) . . ?
C401 C410 C409 118.33(9) . . ?
C401 C410 C420 119.24(9) . . ?
C409 C410 C420 122.36(9) . . ?
C420 C411 O402 118.83(8) . . ?
C420 C411 C412 122.59(10) . . ?
O402 C411 C412 118.57(9) . . ?
C413 C412 C411 118.84(11) . . ?
C412 C413 C414 121.10(10) . . ?
C413 C414 C419 119.32(11) . . ?
C413 C414 C415 122.02(10) . . ?
C419 C414 C415 118.60(11) . . ?
C416 C415 C414 120.99(12) . . ?
C415 C416 C417 120.53(13) . . ?
C418 C417 C416 120.40(13) . . ?
C417 C418 C419 120.47(11) . . ?
C418 C419 C414 118.95(10) . . ?
C418 C419 C420 121.89(10) . . ?
C414 C419 C420 119.02(10) . . ?
C411 C420 C419 118.62(9) . . ?
C411 C420 C410 119.44(9) . . ?
C419 C420 C410 121.81(9) . . ?
C510 C501 C502 120.26(11) . . ?
C510 C501 C521 119.61(10) . . ?
C502 C501 C521 120.06(9) . . ?
C503 C502 C501 120.74(10) . . ?
C502 C503 C504 120.78(11) . . ?
C505 C504 C503 121.64(11) . . ?
C505 C504 C509 119.13(10) . . ?
C503 C504 C509 119.21(11) . . ?
C506 C505 C504 120.83(12) . . ?
C505 C506 C507 120.27(12) . . ?
C508 C507 C506 120.56(11) . . ?
C507 C508 C509 120.78(11) . . ?
C508 C509 C504 118.44(10) . . ?
C508 C509 C510 122.58(10) . . ?
C504 C509 C510 118.92(9) . . ?
C501 C510 C509 119.94(10) . . ?
C501 C510 C520 117.62(10) . . ?
C509 C510 C520 122.30(8) . . ?
C520 C511 C512 120.48(9) . . ?
C520 C511 C522 120.69(10) . . ?
C512 C511 C522 118.82(10) . . ?
C513 C512 C511 120.39(10) . . ?
C512 C513 C514 120.83(10) . . ?
C513 C514 C515 121.62(10) . . ?
C513 C514 C519 119.50(10) . . ?
C515 C514 C519 118.77(10) . . ?
C516 C515 C514 121.05(11) . . ?
C515 C516 C517 120.36(10) . . ?
C518 C517 C516 120.05(11) . . ?
C517 C518 C519 120.99(11) . . ?
C518 C519 C514 118.77(9) . . ?
C518 C519 C520 122.52(10) . . ?
C514 C519 C520 118.54(10) . . ?
C511 C520 C519 119.95(10) . . ?
C511 C520 C510 118.33(9) . . ?
C519 C520 C510 121.44(9) . . ?
N501 C521 C501 109.51(9) . . ?
N501 C522 C511 110.38(8) . . ?
N501 C523 N503 120.80(9) . . ?
N501 C523 N502 120.10(9) . . ?
N503 C523 N502 119.08(9) . . ?
C610 C601 O601 118.51(9) . . ?
C610 C601 C602 123.87(9) . . ?
O601 C601 C602 117.62(10) . . ?
C603 C602 C601 118.53(11) . . ?
C602 C603 C604 120.68(10) . . ?
C603 C604 C605 121.34(11) . . ?
C603 C604 C609 119.93(10) . . ?
C605 C604 C609 118.71(11) . . ?
C606 C605 C604 121.22(11) . . ?
C605 C606 C607 120.03(11) . . ?
C608 C607 C606 120.66(12) . . ?
C607 C608 C609 120.77(11) . . ?
C608 C609 C604 118.59(9) . . ?
C608 C609 C610 122.33(10) . . ?
C604 C609 C610 119.03(10) . . ?
C601 C610 C609 117.58(9) . . ?
C601 C610 C620 119.17(9) . . ?
C609 C610 C620 123.12(10) . . ?
C620 C611 O602 119.01(9) . . ?
C620 C611 C612 123.15(11) . . ?
O602 C611 C612 117.84(10) . . ?
C613 C612 C611 119.07(11) . . ?
C612 C613 C614 120.72(10) . . ?
C613 C614 C615 121.06(11) . . ?
C613 C614 C619 119.49(11) . . ?
C615 C614 C619 119.35(11) . . ?
C616 C615 C614 120.54(12) . . ?
C615 C616 C617 120.31(12) . . ?
C618 C617 C616 120.71(12) . . ?
C617 C618 C619 120.72(11) . . ?
C618 C619 C614 118.32(11) . . ?
C618 C619 C620 122.24(10) . . ?
C614 C619 C620 119.29(10) . . ?
C611 C620 C619 118.04(9) . . ?
C611 C620 C610 119.07(10) . . ?
C619 C620 C610 122.72(10) . . ?
C710 C701 C702 120.35(10) . . ?
C710 C701 C721 121.50(10) . . ?
C702 C701 C721 118.14(10) . . ?
C703 C702 C701 120.78(11) . . ?
C702 C703 C704 120.74(11) . . ?
C703 C704 C705 121.51(11) . . ?
C703 C704 C709 119.47(10) . . ?
C705 C704 C709 118.99(11) . . ?
C706 C705 C704 121.21(12) . . ?
C705 C706 C707 120.01(12) . . ?
C708 C707 C706 120.51(12) . . ?
C707 C708 C709 121.07(11) . . ?
C708 C709 C704 118.18(10) . . ?
C708 C709 C710 122.89(10) . . ?
C704 C709 C710 118.89(10) . . ?
C701 C710 C709 119.57(10) . . ?
C701 C710 C720 118.75(9) . . ?
C709 C710 C720 121.51(9) . . ?
C720 C711 C712 121.09(10) . . ?
C720 C711 C722 118.84(9) . . ?
C712 C711 C722 120.06(10) . . ?
C713 C712 C711 120.09(10) . . ?
C712 C713 C714 121.00(10) . . ?
C713 C714 C715 121.39(11) . . ?
C713 C714 C719 119.39(11) . . ?
C715 C714 C719 119.20(11) . . ?
C716 C715 C714 120.63(11) . . ?
C715 C716 C717 120.37(12) . . ?
C718 C717 C716 120.57(12) . . ?
C717 C718 C719 120.62(11) . . ?
C718 C719 C714 118.55(11) . . ?
C718 C719 C720 122.41(10) . . ?
C714 C719 C720 119.00(10) . . ?
C711 C720 C719 119.26(10) . . ?
C711 C720 C710 118.29(10) . . ?
C719 C720 C710 122.42(10) . . ?
N701 C721 C701 112.00(8) . . ?
N701 C722 C711 111.09(8) . . ?
N702 C723 N703 117.46(10) . . ?
N702 C723 N701 121.13(10) . . ?
N703 C723 N701 121.41(9) . . ?
C810 C801 O801 118.85(10) . . ?
C810 C801 C802 123.45(11) . . ?
O801 C801 C802 117.70(11) . . ?
C803 C802 C801 119.18(12) . . ?
C802 C803 C804 120.64(11) . . ?
C805 C804 C803 121.41(12) . . ?
C805 C804 C809 118.98(12) . . ?
C803 C804 C809 119.60(11) . . ?
C806 C805 C804 121.08(13) . . ?
C805 C806 C807 120.27(12) . . ?
C808 C807 C806 120.45(13) . . ?
C807 C808 C809 120.79(12) . . ?
C808 C809 C804 118.36(10) . . ?
C808 C809 C810 122.17(10) . . ?
C804 C809 C810 119.38(11) . . ?
C801 C810 C809 117.40(10) . . ?
C801 C810 C820 119.14(10) . . ?
C809 C810 C820 123.38(10) . . ?
C820 C811 O802 119.31(10) . . ?
C820 C811 C812 123.18(11) . . ?
O802 C811 C812 117.47(10) . . ?
C813 C812 C811 119.38(11) . . ?
C812 C813 C814 120.59(11) . . ?
C813 C814 C815 121.42(11) . . ?
C813 C814 C819 119.54(11) . . ?
C815 C814 C819 119.04(11) . . ?
C816 C815 C814 121.22(12) . . ?
C815 C816 C817 119.94(13) . . ?
C818 C817 C816 120.37(13) . . ?
C817 C818 C819 121.39(12) . . ?
C818 C819 C814 118.01(11) . . ?
C818 C819 C820 122.41(10) . . ?
C814 C819 C820 119.56(11) . . ?
C811 C820 C819 117.53(10) . . ?
C811 C820 C810 119.51(10) . . ?
C819 C820 C810 122.84(10) . . ?
C997 C991 C992 120.4(4) . . ?
C997 C991 C996 119.5(4) . . ?
C992 C991 C996 120.0 . . ?
C991 C992 C993 120.0 . . ?
C994 C993 C992 120.0 . . ?
C995 C994 C993 120.0 . . ?
C994 C995 C996 120.0 . . ?
C995 C996 C991 120.0 . . ?

_refine_diff_density_max         1.466
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.072


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

data_mt_317_2m

_database_code_depnum_ccdc_archive 'CCDC 2078133'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H27 I2 N O3'
_chemical_formula_weight         679.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
I I -0.3257 6.8362 '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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   11.8508(16)
_cell_length_b                   9.1039(12)
_cell_length_c                   13.2298(17)
_cell_angle_alpha                90
_cell_angle_beta                 115.219(6)
_cell_angle_gamma                90
_cell_volume                     1291.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9394
_cell_measurement_theta_min      3.69
_cell_measurement_theta_max      80.12

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.011
_exptl_absorpt_coefficient_mu    19.363
_shelx_estimated_absorpt_T_min   0.081
_shelx_estimated_absorpt_T_max   0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture (Photon II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/Queen'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            49382
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.693
_diffrn_reflns_theta_max         81.331
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5431
_reflns_number_gt                5111
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3(v2017.3-0)'
_computing_cell_refinement       'Bruker APEX3(v2017.3-0)'
_computing_data_reduction        'Bruker APEX3(v2017.3-0)'
_computing_structure_solution    'Bruker APEX3(v2017.3-0)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom. The OH hydrogen atoms was refined freely.
 Twinning:
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0522P)²+4.0856P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.163(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5431
_refine_ls_number_parameters     316
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_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
I1 I -0.35079(5) 0.11928(6) 0.38220(5) 0.03625(16) Uani 1 1 d . . . . .
I2 I 0.01191(6) -0.26932(8) 0.01592(5) 0.04436(19) Uani 1 1 d . . . . .
O1 O -0.2976(7) -0.2648(10) 0.0477(5) 0.0408(15) Uani 1 1 d . . . . .
O2 O -0.3217(6) -0.2878(8) 0.2089(6) 0.0381(15) Uani 1 1 d . . . . .
N1 N -0.1956(7) -0.1140(8) 0.1914(6) 0.0289(15) Uani 1 1 d . . . . .
C1 C -0.0214(8) 0.1455(10) 0.3124(6) 0.0271(17) Uani 1 1 d . . . . .
C2 C -0.1241(8) 0.0931(9) 0.3260(7) 0.0277(17) Uani 1 1 d . . . . .
C3 C -0.1962(8) 0.1909(10) 0.3558(7) 0.0294(18) Uani 1 1 d . . . . .
C4 C -0.1670(8) 0.3370(11) 0.3736(7) 0.0293(17) Uani 1 1 d . . . . .
H4 H -0.214683 0.398979 0.398347 0.035 Uiso 1 1 calc R U . . .
C5 C -0.0371(10) 0.5464(10) 0.3687(7) 0.0337(19) Uani 1 1 d . . . . .
H5 H -0.084263 0.610212 0.392735 0.040 Uiso 1 1 calc R U . . .
C6 C 0.0576(9) 0.6027(11) 0.3478(7) 0.0353(18) Uani 1 1 d . . . . .
H6 H 0.077222 0.704397 0.358720 0.042 Uiso 1 1 calc R U . . .
C7 C 0.1259(9) 0.5092(11) 0.3102(8) 0.0350(19) Uani 1 1 d . . . . .
H7 H 0.189773 0.549216 0.293143 0.042 Uiso 1 1 calc R U . . .
C8 C 0.1024(9) 0.3619(9) 0.2975(7) 0.0300(19) Uani 1 1 d . . . . .
H8 H 0.149982 0.300730 0.272159 0.036 Uiso 1 1 calc R U . . .
C9 C 0.0066(8) 0.2998(10) 0.3221(7) 0.0276(17) Uani 1 1 d . . . . .
C10 C -0.0660(9) 0.3974(11) 0.3555(7) 0.0306(18) Uani 1 1 d . . . . .
C11 C 0.0593(8) 0.0417(9) 0.2859(7) 0.0269(16) Uani 1 1 d . . . . .
C12 C 0.0041(8) -0.0460(9) 0.1910(7) 0.0267(16) Uani 1 1 d . . . . .
C13 C 0.0821(10) -0.1395(9) 0.1621(7) 0.0309(19) Uani 1 1 d . . . . .
C14 C 0.2077(9) -0.1508(10) 0.2273(8) 0.0311(18) Uani 1 1 d . . . . .
H14 H 0.257423 -0.213859 0.205597 0.037 Uiso 1 1 calc R U . . .
C15 C 0.3928(9) -0.0835(12) 0.3987(8) 0.038(2) Uani 1 1 d . . . . .
H15 H 0.442901 -0.147141 0.377992 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4443(8) -0.0073(13) 0.4965(8) 0.043(2) Uani 1 1 d . . . . .
H16 H 0.530184 -0.020214 0.544474 0.051 Uiso 1 1 calc R U . . .
C17 C 0.3724(9) 0.0903(12) 0.5276(8) 0.040(2) Uani 1 1 d . . . . .
H17 H 0.410039 0.145160 0.594912 0.048 Uiso 1 1 calc R U . . .
C18 C 0.2485(8) 0.1053(11) 0.4602(7) 0.0322(17) Uani 1 1 d . . . . .
H18 H 0.200553 0.169533 0.483057 0.039 Uiso 1 1 calc R U . . .
C19 C 0.1886(8) 0.0301(9) 0.3586(7) 0.0280(16) Uani 1 1 d . . . . .
C20 C 0.2632(9) -0.0675(10) 0.3276(8) 0.0303(18) Uani 1 1 d . . . . .
C21 C -0.1507(9) -0.0689(10) 0.3095(7) 0.0294(17) Uani 1 1 d . . . . .
H21A H -0.073740 -0.124036 0.355116 0.035 Uiso 1 1 calc R U . . .
H21B H -0.214454 -0.094758 0.336314 0.035 Uiso 1 1 calc R U . . .
C22 C -0.1364(9) -0.0426(11) 0.1264(7) 0.0329(19) Uani 1 1 d . . . . .
H22A H -0.165110 0.060521 0.110473 0.040 Uiso 1 1 calc R U . . .
H22B H -0.160958 -0.094163 0.054214 0.040 Uiso 1 1 calc R U . . .
C23 C -0.2764(9) -0.2284(10) 0.1530(8) 0.034(2) Uani 1 1 d . . . . .
C24 C -0.3605(10) -0.4011(14) -0.0055(9) 0.047(2) Uani 1 1 d . . . . .
C25 C -0.4991(10) -0.387(2) -0.0391(10) 0.060(3) Uani 1 1 d . . . . .
H25A H -0.532068 -0.303181 -0.089321 0.090 Uiso 1 1 calc R U . . .
H25B H -0.513693 -0.372702 0.027792 0.090 Uiso 1 1 calc R U . . .
H25C H -0.541247 -0.477196 -0.077399 0.090 Uiso 1 1 calc R U . . .
C26 C -0.2977(18) -0.5321(16) 0.0702(13) 0.079(5) Uani 1 1 d . . . . .
H26A H -0.341796 -0.622622 0.035257 0.119 Uiso 1 1 calc R U . . .
H26B H -0.300401 -0.518710 0.142675 0.119 Uiso 1 1 calc R U . . .
H26C H -0.210663 -0.538851 0.081260 0.119 Uiso 1 1 calc R U . . .
C27 C -0.3392(10) -0.4093(17) -0.1098(9) 0.054(3) Uani 1 1 d . . . . .
H27A H -0.384152 -0.494006 -0.154591 0.081 Uiso 1 1 calc R U . . .
H27B H -0.249818 -0.420162 -0.089206 0.081 Uiso 1 1 calc R U . . .
H27C H -0.369846 -0.319141 -0.153419 0.081 Uiso 1 1 calc R U . . .
O1_1 O -0.5634(8) -0.3379(10) 0.2005(7) 0.056(2) Uani 1 1 d D . . . .
H1_1 H -0.492(7) -0.319(17) 0.200(13) 0.07(5) Uiso 1 1 d D . . . .
C1_1 C -0.5928(14) -0.4862(16) 0.1864(11) 0.060(3) Uani 1 1 d . . . . .
H1A_1 H -0.678795 -0.500344 0.176603 0.090 Uiso 1 1 calc R U . . .
H1B_1 H -0.535866 -0.540438 0.252485 0.090 Uiso 1 1 calc R U . . .
H1C_1 H -0.584339 -0.522529 0.120242 0.090 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
I1 C3 2.109(9) . ?
I2 C13 2.112(8) . ?
O1 C23 1.347(11) . ?
O1 C24 1.464(13) . ?
O2 C23 1.210(12) . ?
N1 C23 1.358(12) . ?
N1 C22 1.474(11) . ?
N1 C21 1.478(11) . ?
C1 C2 1.388(12) . ?
C1 C9 1.436(12) . ?
C1 C11 1.490(12) . ?
C2 C3 1.402(12) . ?
C2 C21 1.504(12) . ?
C3 C4 1.369(14) . ?
C4 C10 1.428(13) . ?
C5 C6 1.365(14) . ?
C5 C10 1.391(13) . ?
C6 C7 1.404(13) . ?
C7 C8 1.365(13) . ?
C8 C9 1.424(13) . ?
C9 C10 1.432(12) . ?
C11 C12 1.393(12) . ?
C11 C19 1.423(12) . ?
C12 C13 1.422(12) . ?
C12 C22 1.513(13) . ?
C13 C14 1.370(14) . ?
C14 C20 1.423(13) . ?
C15 C16 1.362(16) . ?
C15 C20 1.425(13) . ?
C16 C17 1.409(16) . ?
C17 C18 1.362(13) . ?
C18 C19 1.403(12) . ?
C19 C20 1.431(12) . ?
C24 C27 1.507(15) . ?
C24 C25 1.513(15) . ?
C24 C26 1.531(19) . ?
O1_1 C1_1 1.386(17) . ?

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
C23 O1 C24 122.5(8) . . ?
C23 N1 C22 123.7(7) . . ?
C23 N1 C21 119.2(8) . . ?
C22 N1 C21 116.6(7) . . ?
C2 C1 C9 120.5(8) . . ?
C2 C1 C11 119.9(8) . . ?
C9 C1 C11 119.6(8) . . ?
C1 C2 C3 119.4(8) . . ?
C1 C2 C21 117.4(8) . . ?
C3 C2 C21 123.2(8) . . ?
C4 C3 C2 121.7(8) . . ?
C4 C3 I1 116.4(6) . . ?
C2 C3 I1 121.8(7) . . ?
C3 C4 C10 120.9(8) . . ?
C6 C5 C10 121.4(9) . . ?
C5 C6 C7 119.4(9) . . ?
C8 C7 C6 121.4(9) . . ?
C7 C8 C9 120.2(9) . . ?
C8 C9 C10 117.8(8) . . ?
C8 C9 C1 123.0(8) . . ?
C10 C9 C1 119.2(8) . . ?
C5 C10 C4 122.3(9) . . ?
C5 C10 C9 119.7(9) . . ?
C4 C10 C9 118.0(9) . . ?
C12 C11 C19 121.5(8) . . ?
C12 C11 C1 118.3(8) . . ?
C19 C11 C1 120.1(7) . . ?
C11 C12 C13 118.4(8) . . ?
C11 C12 C22 118.6(7) . . ?
C13 C12 C22 123.0(8) . . ?
C14 C13 C12 122.2(8) . . ?
C14 C13 I2 115.6(7) . . ?
C12 C13 I2 122.2(7) . . ?
C13 C14 C20 119.5(8) . . ?
C16 C15 C20 119.7(10) . . ?
C15 C16 C17 121.1(9) . . ?
C18 C17 C16 119.3(9) . . ?
C17 C18 C19 122.9(9) . . ?
C18 C19 C11 124.8(8) . . ?
C18 C19 C20 117.1(8) . . ?
C11 C19 C20 118.1(8) . . ?
C14 C20 C15 120.1(9) . . ?
C14 C20 C19 120.1(8) . . ?
C15 C20 C19 119.8(9) . . ?
N1 C21 C2 112.6(7) . . ?
N1 C22 C12 110.2(7) . . ?
O2 C23 O1 125.9(9) . . ?
O2 C23 N1 122.6(8) . . ?
O1 C23 N1 111.5(8) . . ?
O1 C24 C27 103.5(9) . . ?
O1 C24 C25 109.7(10) . . ?
C27 C24 C25 108.6(9) . . ?
O1 C24 C26 109.9(8) . . ?
C27 C24 C26 109.6(12) . . ?
C25 C24 C26 114.9(13) . . ?

_refine_diff_density_max         2.152
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.144


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

data_mt_383m_sq

_database_code_depnum_ccdc_archive 'CCDC 2078134'
loop_
_audit_author_name
_audit_author_address
'Christoph Wolper'
;Universitaet Duisburg Essen
Germany
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H52 N2 O4'
_chemical_formula_weight         913.07

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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_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'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   10.0422(3)
_cell_length_b                   10.0422(3)
_cell_length_c                   53.3248(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5377.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    104(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      79.53

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_F_000             1928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    0.547
_shelx_estimated_absorpt_T_min   0.947
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      104(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture (Photon II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/Queen'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            84164
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_theta_min         3.315
_diffrn_reflns_theta_max         79.876
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5790
_reflns_number_gt                5496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_max     0.980
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX3(v2017.3-0)'
_computing_cell_refinement       'Bruker APEX3(v2017.3-0)'
_computing_data_reduction        'Bruker APEX3(v2017.3-0)'
_computing_structure_solution    'Bruker APEX3(v2017.3-0)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 Disorder:
 The central phenyl ring is diordered over the two-fold axis. Two alternate
 positions were used in the refinement and the local symmetry was ignored in the 
 refinement (negative PART). The bond lengths were restrained to be equal to
 1.39\,Å{} (DFIX, $σ=0.001$) and the angle were restrained to be equal
 (SADI, $σ=0.001$). The ring was restrained to planarity (FLAT, 
 $σ=0.001$). All atoms of both positions were refined with common
 displacement parameters (EADP) and the connecting atoms (C30, C30' and C36,
 C36') were constrained to equal positions (EXYZ).
 SQUEEZE:
 The structure contains highly disordered solvent - possibly methanol. 
 The final refinement  was done with a solvent free dataset from a
 PLATON/SQUEEZE run. (For details see: A.~L.~Spek, Acta Cryst. A46 
 (1990),194--201). Since the nature and amount of the solvent is
 not clear it was not included in the sum formula.
 Possible twinning by inversion:
 The Flack parameter suggest twinning by inversion, however refining so yields
 a very high standard uncertainty for the BASF rendering it meaningless. Thus,
 the twinning model was discarded. The chosen chirality resembles chemical
 expectation but should not be considered reliable.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0670P)²+2.3338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2131 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.24(5)
_chemical_absolute_configuration syn #rmad?
_refine_ls_number_reflns         5790
_refine_ls_number_parameters     328
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_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
C1 C 0.5281(2) 1.0118(2) 0.63931(4) 0.0241(4) Uani 1 1 d . . . . .
O1 O 0.78287(17) 1.11809(17) 0.56051(3) 0.0318(4) Uani 1 1 d . . . . .
N1 N 0.6676(2) 0.9945(2) 0.58777(4) 0.0303(4) Uani 1 1 d . . . . .
C2 C 0.6141(2) 1.1004(2) 0.62754(4) 0.0271(5) Uani 1 1 d . . . . .
O2 O 0.81107(17) 0.89271(17) 0.56107(3) 0.0329(4) Uani 1 1 d . . . . .
C3 C 0.7112(2) 1.1706(2) 0.64150(5) 0.0308(5) Uani 1 1 d . . . . .
H3 H 0.766094 1.234190 0.633326 0.037 Uiso 1 1 calc R U . . .
C4 C 0.7270(2) 1.1480(3) 0.66657(5) 0.0333(5) Uani 1 1 d . . . . .
H4 H 0.791625 1.197078 0.675727 0.040 Uiso 1 1 calc R U . . .
C5 C 0.6476(3) 1.0519(3) 0.67901(4) 0.0304(5) Uani 1 1 d . . . . .
C6 C 0.6686(3) 1.0214(3) 0.70466(5) 0.0389(6) Uani 1 1 d . . . . .
H6 H 0.735459 1.067414 0.713820 0.047 Uiso 1 1 calc R U . . .
C7 C 0.5938(3) 0.9270(3) 0.71624(5) 0.0441(7) Uani 1 1 d . . . . .
H7 H 0.609027 0.907507 0.733435 0.053 Uiso 1 1 calc R U . . .
C8 C 0.4941(3) 0.8575(3) 0.70310(4) 0.0379(6) Uani 1 1 d . . . . .
H8 H 0.443058 0.791138 0.711395 0.046 Uiso 1 1 calc R U . . .
C9 C 0.4705(2) 0.8855(2) 0.67835(4) 0.0288(5) Uani 1 1 d . . . . .
H9 H 0.402753 0.838425 0.669645 0.035 Uiso 1 1 calc R U . . .
C10 C 0.5456(2) 0.9835(2) 0.66555(4) 0.0263(4) Uani 1 1 d . . . . .
C11 C 0.4278(2) 0.9419(2) 0.62346(4) 0.0241(4) Uani 1 1 d . . . . .
C12 C 0.4758(2) 0.8728(2) 0.60275(4) 0.0243(4) Uani 1 1 d . . . . .
C13 C 0.3852(3) 0.8156(2) 0.58509(4) 0.0265(5) Uani 1 1 d . . . . .
C14 C 0.2504(3) 0.8269(2) 0.58859(4) 0.0276(5) Uani 1 1 d . . . . .
H14 H 0.191231 0.788150 0.576753 0.033 Uiso 1 1 calc R U . . .
C15 C 0.1981(2) 0.8956(2) 0.60963(4) 0.0252(4) Uani 1 1 d . . . . .
C16 C 0.0585(3) 0.9080(2) 0.61310(4) 0.0301(5) Uani 1 1 d . . . . .
H16 H -0.000721 0.871393 0.601043 0.036 Uiso 1 1 calc R U . . .
C17 C 0.0086(2) 0.9723(2) 0.63366(5) 0.0314(5) Uani 1 1 d . . . . .
H17 H -0.084989 0.977910 0.636090 0.038 Uiso 1 1 calc R U . . .
C18 C 0.0959(2) 1.0302(2) 0.65123(4) 0.0303(5) Uani 1 1 d . . . . .
H18 H 0.060515 1.074469 0.665502 0.036 Uiso 1 1 calc R U . . .
C19 C 0.2308(2) 1.0236(2) 0.64801(4) 0.0280(5) Uani 1 1 d . . . . .
H19 H 0.287833 1.066041 0.659762 0.034 Uiso 1 1 calc R U . . .
C20 C 0.2868(2) 0.9540(2) 0.62731(4) 0.0244(4) Uani 1 1 d . . . . .
C21 C 0.6120(3) 1.1157(2) 0.59934(4) 0.0298(5) Uani 1 1 d . . . . .
H21A H 0.519497 1.129635 0.593506 0.036 Uiso 1 1 calc R U . . .
H21B H 0.665607 1.194194 0.594374 0.036 Uiso 1 1 calc R U . . .
C22 C 0.6238(2) 0.8664(2) 0.59811(4) 0.0271(5) Uani 1 1 d . . . . .
H22A H 0.671184 0.848023 0.614011 0.033 Uiso 1 1 calc R U . . .
H22B H 0.644194 0.793852 0.586148 0.033 Uiso 1 1 calc R U . . .
C23 C 0.7590(2) 0.9933(2) 0.56902(4) 0.0259(4) Uani 1 1 d . . . . .
C24 C 0.8797(3) 1.1396(3) 0.54037(4) 0.0323(5) Uani 1 1 d . . . . .
C25 C 0.8343(5) 1.0668(4) 0.51689(5) 0.0617(10) Uani 1 1 d . . . . .
H25A H 0.891450 1.091991 0.502769 0.093 Uiso 1 1 calc R U . . .
H25B H 0.741883 1.091080 0.513126 0.093 Uiso 1 1 calc R U . . .
H25C H 0.840219 0.970531 0.519632 0.093 Uiso 1 1 calc R U . . .
C26 C 1.0175(3) 1.0981(3) 0.54859(7) 0.0512(7) Uani 1 1 d . . . . .
H26A H 1.021978 1.000774 0.549622 0.077 Uiso 1 1 calc R U . . .
H26B H 1.036859 1.136536 0.565087 0.077 Uiso 1 1 calc R U . . .
H26C H 1.083160 1.130081 0.536396 0.077 Uiso 1 1 calc R U . . .
C27 C 0.8731(3) 1.2895(3) 0.53662(5) 0.0429(6) Uani 1 1 d . . . . .
H27A H 0.936048 1.315888 0.523491 0.064 Uiso 1 1 calc R U . . .
H27B H 0.896225 1.334477 0.552338 0.064 Uiso 1 1 calc R U . . .
H27C H 0.782641 1.314842 0.531615 0.064 Uiso 1 1 calc R U . . .
C28 C 0.4367(3) 0.7505(2) 0.56309(4) 0.0301(5) Uani 1 1 d . . . . .
C29 C 0.4813(3) 0.7012(2) 0.54436(4) 0.0335(5) Uani 1 1 d . . . . .
C30 C 0.5281(4) 0.6498(5) 0.52086(8) 0.0293(5) Uani 0.25 1 d D . P A -1
C36 C 0.6407(5) 0.5452(4) 0.47746(9) 0.0293(5) Uani 0.25 1 d D . P A -1
C31 C 0.5622(4) 0.7337(4) 0.50113(9) 0.0293(5) Uani 0.25 1 d D . P A -1
H31 H 0.547054 0.826774 0.502466 0.035 Uiso 0.25 1 calc R U P A -1
C32 C 0.6185(4) 0.6812(4) 0.47944(9) 0.0293(5) Uani 0.25 1 d D . P A -1
H32 H 0.641880 0.738596 0.465974 0.035 Uiso 0.25 1 calc R U P A -1
C33 C 0.6066(7) 0.4611(3) 0.49721(12) 0.0293(5) Uani 0.25 1 d D . P A -1
H33 H 0.621850 0.367970 0.495869 0.035 Uiso 0.25 1 calc R U P A -1
C34 C 0.5504(6) 0.5135(4) 0.51889(11) 0.0293(5) Uani 0.25 1 d D . P A -1
H34 H 0.527173 0.456141 0.532374 0.035 Uiso 0.25 1 calc R U P A -1
C30' C 0.5281(4) 0.6498(5) 0.52086(8) 0.0293(5) Uani 0.25 1 d D . P A -2
C31' C 0.6649(4) 0.6565(4) 0.51721(9) 0.0293(5) Uani 0.25 1 d D . P A -2
H31' H 0.720014 0.696763 0.529550 0.035 Uiso 0.25 1 calc R U P A -2
C32' C 0.7212(3) 0.6042(5) 0.49552(9) 0.0293(5) Uani 0.25 1 d D . P A -2
H32' H 0.814806 0.608921 0.493031 0.035 Uiso 0.25 1 calc R U P A -2
C36' C 0.6407(5) 0.5452(4) 0.47746(9) 0.0293(5) Uani 0.25 1 d D . P A -2
C33' C 0.5036(5) 0.5387(6) 0.48109(12) 0.0293(5) Uani 0.25 1 d D . P A -2
H33' H 0.448516 0.498567 0.468737 0.035 Uiso 0.25 1 calc R U P A -2
C34' C 0.4473(4) 0.5909(7) 0.50278(12) 0.0293(5) Uani 0.25 1 d D . P A -2
H34' H 0.353747 0.586376 0.505262 0.035 Uiso 0.25 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
C1 C2 1.390(3) . ?
C1 C10 1.438(3) . ?
C1 C11 1.490(3) . ?
O1 C23 1.354(3) . ?
O1 C24 1.465(3) . ?
N1 C23 1.358(3) . ?
N1 C22 1.466(3) . ?
N1 C21 1.475(3) . ?
C2 C3 1.415(3) . ?
C2 C21 1.512(3) . ?
O2 C23 1.214(3) . ?
C3 C4 1.365(4) . ?
C4 C5 1.417(4) . ?
C5 C6 1.417(3) . ?
C5 C10 1.427(3) . ?
C6 C7 1.359(4) . ?
C7 C8 1.407(4) . ?
C8 C9 1.370(3) . ?
C9 C10 1.415(3) . ?
C11 C12 1.390(3) . ?
C11 C20 1.436(3) . ?
C12 C13 1.430(3) . ?
C12 C22 1.508(3) . ?
C13 C14 1.372(3) . ?
C13 C28 1.439(3) . ?
C14 C15 1.418(3) . ?
C15 C16 1.419(3) . ?
C15 C20 1.424(3) . ?
C16 C17 1.367(3) . ?
C17 C18 1.409(3) . ?
C18 C19 1.367(3) . ?
C19 C20 1.423(3) . ?
C24 C26 1.511(4) . ?
C24 C25 1.520(4) . ?
C24 C27 1.520(4) . ?
C28 C29 1.201(3) . ?
C29 C30' 1.434(5) . ?
C29 C30 1.434(5) . ?
C30 C31 1.3900(11) . ?
C30 C34 1.3918(11) . ?
C36 C32 1.3885(11) . ?
C36 C33 1.3925(11) . ?
C31 C32 1.3909(11) . ?
C33 C34 1.3901(11) . ?
C30' C31' 1.3892(11) . ?
C30' C34' 1.3920(11) . ?
C31' C32' 1.3906(11) . ?
C32' C36' 1.3904(11) . ?
C36' C33' 1.3914(11) . ?
C33' C34' 1.3902(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 119.3(2) . . ?
C2 C1 C11 117.73(19) . . ?
C10 C1 C11 122.8(2) . . ?
C23 O1 C24 119.99(18) . . ?
C23 N1 C22 118.16(19) . . ?
C23 N1 C21 124.8(2) . . ?
C22 N1 C21 116.97(17) . . ?
C1 C2 C3 120.6(2) . . ?
C1 C2 C21 120.4(2) . . ?
C3 C2 C21 118.8(2) . . ?
C4 C3 C2 120.9(2) . . ?
C3 C4 C5 120.4(2) . . ?
C4 C5 C6 121.0(2) . . ?
C4 C5 C10 119.8(2) . . ?
C6 C5 C10 119.2(2) . . ?
C7 C6 C5 120.5(2) . . ?
C6 C7 C8 120.9(2) . . ?
C9 C8 C7 120.0(3) . . ?
C8 C9 C10 121.0(2) . . ?
C9 C10 C5 118.3(2) . . ?
C9 C10 C1 122.8(2) . . ?
C5 C10 C1 118.8(2) . . ?
C12 C11 C20 119.8(2) . . ?
C12 C11 C1 116.8(2) . . ?
C20 C11 C1 123.06(19) . . ?
C11 C12 C13 120.2(2) . . ?
C11 C12 C22 119.5(2) . . ?
C13 C12 C22 120.10(19) . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 C28 120.2(2) . . ?
C12 C13 C28 119.4(2) . . ?
C13 C14 C15 120.9(2) . . ?
C14 C15 C16 120.8(2) . . ?
C14 C15 C20 119.5(2) . . ?
C16 C15 C20 119.7(2) . . ?
C17 C16 C15 120.6(2) . . ?
C16 C17 C18 120.0(2) . . ?
C19 C18 C17 120.9(2) . . ?
C18 C19 C20 120.9(2) . . ?
C19 C20 C15 117.9(2) . . ?
C19 C20 C11 122.9(2) . . ?
C15 C20 C11 119.21(19) . . ?
N1 C21 C2 109.06(19) . . ?
N1 C22 C12 108.67(18) . . ?
O2 C23 O1 125.2(2) . . ?
O2 C23 N1 123.8(2) . . ?
O1 C23 N1 111.01(19) . . ?
O1 C24 C26 110.8(2) . . ?
O1 C24 C25 109.5(2) . . ?
C26 C24 C25 112.4(3) . . ?
O1 C24 C27 102.3(2) . . ?
C26 C24 C27 110.6(2) . . ?
C25 C24 C27 110.8(2) . . ?
C29 C28 C13 177.3(3) . . ?
C28 C29 C30' 175.4(3) . . ?
C28 C29 C30 175.4(3) . . ?
C31 C30 C34 119.96(7) . . ?
C31 C30 C29 121.6(3) . . ?
C34 C30 C29 118.2(3) . . ?
C32 C36 C33 120.01(7) . . ?
C30 C31 C32 120.02(8) . . ?
C36 C32 C31 120.05(8) . . ?
C34 C33 C36 119.94(8) . . ?
C33 C34 C30 120.03(8) . . ?
C31' C30' C34' 120.00(7) . . ?
C31' C30' C29 115.4(3) . . ?
C34' C30' C29 124.5(3) . . ?
C30' C31' C32' 120.04(8) . . ?
C36' C32' C31' 120.02(8) . . ?
C32' C36' C33' 119.96(7) . . ?
C34' C33' C36' 120.02(8) . . ?
C33' C34' C30' 119.97(8) . . ?

_refine_diff_density_max         0.521
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.044



