# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2022

####################################################################### 
# 
# 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_cx1883
_database_code_depnum_ccdc_archive 'CCDC 2042985'
loop_
_audit_author_name
_audit_author_address
'Masoud Kazem-Rostami'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-11-07 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_audit_creation_date             2020-05-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
"(5S,11S)-6H,12H-5,11-ethano dibenzo[b,f][1,5]diazocine . (-)-O,O'-Dibenzoyl-L-tartaric acid"
_chemical_formula_moiety         'C18 H13 O8, C16 H17 N2, C3 H6 O'
_chemical_formula_sum            'C37 H36 N2 O9'
_chemical_formula_weight         652.68
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C10H16N2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.31750(10)
_cell_length_b                   11.86530(10)
_cell_length_c                   25.2383(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3389.14(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14679
_cell_measurement_temperature    199.91(17)
_cell_measurement_theta_max      76.2800
_cell_measurement_theta_min      3.4880
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.943
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1376
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0249
-1 0 0 0.0249
0 -1 0 0.0403
0 1 0 0.0374
0 0 1 0.0117
0 0 -1 0.0117

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.023
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0000 -0.0000 -0.0000 0.0029 0.0633 0.1205
-1.0000 0.0000 0.0000 -0.0029 -0.0633 -0.1205
0.0000 -1.0000 -0.0000 -0.0275 -0.1121 0.0595
-0.0000 1.0000 0.0000 0.0275 0.1121 -0.0595
0.0000 0.0000 1.0000 -0.0596 0.0121 -0.0049
-0.0000 -0.0000 -1.0000 0.0596 -0.0121 0.0049

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20030
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.839
_diffrn_reflns_theta_min         3.502
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.91(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  24.00   0.50    1.00    --  -48.95  36.00 -15.00  118
  2  ω   -107.00 -73.00   0.50    1.00    --  -48.95-125.00 129.00   68
  3  ω   -171.00-132.00   0.50    3.00    -- -105.86 -85.00  17.00   78
  4  ω   -177.00-101.00   0.50    3.00    -- -105.86 -36.00-171.00  152
  5  ω     76.00 175.00   0.50    3.00    --  105.86 125.00-152.00  198
  6  ω    -42.00 -12.00   0.50    1.00    --  -48.95  37.00  90.00   60
  7  ω   -122.00 -73.00   0.50    1.00    --  -48.95-125.00 -90.00   98
  8  ω    -19.00  18.00   0.50    1.00    --   48.95 -19.00  90.00   74
  9  ω    -16.00  13.00   0.50    1.00    --   48.95 -19.00  30.00   58
 10  ω     88.00 113.00   0.50    1.00    --   48.95 125.00-152.00   50
 11  ω    -71.00 -45.00   0.50    3.00    -- -105.86  61.00   0.00   52
 12  ω    -74.00 -34.00   0.50    3.00    -- -105.86  61.00 -30.00   80
 13  ω     36.00  62.00   0.50    3.00    --  105.86 -61.00 150.00   52
 14  ω     42.00  71.00   0.50    3.00    --  105.86 -61.00 -30.00   58
 15  ω     38.00 105.00   0.50    3.00    --  105.86 -94.00 120.00  134
 16  ω    149.00 178.00   0.50    3.00    --  105.86  15.00  90.00   58
 17  ω    123.00 175.00   0.50    3.00    --  105.86  15.00 120.00  104
 18  ω     44.00  71.00   0.50    3.00    --  105.86 -61.00-150.00   54
 19  ω     97.00 144.00   0.50    3.00    --  105.86  15.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029013000
_diffrn_orient_matrix_UB_12      0.0274882000
_diffrn_orient_matrix_UB_13      -0.0596272000
_diffrn_orient_matrix_UB_21      0.0632903000
_diffrn_orient_matrix_UB_22      0.1121358000
_diffrn_orient_matrix_UB_23      0.0120544000
_diffrn_orient_matrix_UB_31      0.1204693000
_diffrn_orient_matrix_UB_32      -0.0594707000
_diffrn_orient_matrix_UB_33      -0.0048703000
_diffrn_oxdiff_digest_frames     
;
018dbf239d9c9616b99b772869885c03ff016402a1b
;
_diffrn_oxdiff_digest_hkl        
;
01b8564db76630e86570fa261219eb962f97dc
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                6293
_reflns_number_total             6840
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 
;
 Flack x determined using 2570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_extinction_coef       0.00104(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+0.2847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0818
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O1T)=Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(H1TC)=Sof(C2T)=Sof(C3T)=Sof(H3TA)=
 Sof(H3TB)=Sof(H3TC)=1-FVAR(1)
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(C3S)=Sof(H3SA)=
 Sof(H3SB)=Sof(H3SC)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C27(H27A,H27B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30),
  C31(H31), C32(H32)
3.d Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C1T(H1TA,H1TB,H1TC), C3S(H3SA,H3SB,H3SC), C3T(H3TA,H3TB,
 H3TC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.67404(12) 0.69523(13) 0.64264(5) 0.0411(3) Uani 1 1 d . . . . .
O2 O 0.52102(12) 0.76296(13) 0.59750(5) 0.0429(3) Uani 1 1 d . . . . .
O3 O 0.65041(11) 0.76984(10) 0.50612(5) 0.0315(3) Uani 1 1 d . . . . .
O4 O 0.69148(19) 0.95343(14) 0.51473(8) 0.0679(5) Uani 1 1 d . . . . .
O5 O 0.89777(12) 0.71908(13) 0.48759(6) 0.0442(3) Uani 1 1 d . . . . .
H5 H 0.940(2) 0.719(2) 0.4578(12) 0.058(8) Uiso 1 1 d . . . . .
O6 O 0.83543(18) 0.54783(14) 0.46336(6) 0.0598(4) Uani 1 1 d . . . . .
O7 O 0.67155(11) 0.54876(11) 0.54077(5) 0.0351(3) Uani 1 1 d . . . . .
O8 O 0.77570(16) 0.41657(14) 0.58362(8) 0.0632(5) Uani 1 1 d . . . . .
C1 C 0.62612(16) 0.73461(15) 0.60149(7) 0.0321(4) Uani 1 1 d . . . . .
C2 C 0.71077(15) 0.74257(15) 0.55453(7) 0.0299(3) Uani 1 1 d . . . . .
H2 H 0.773329 0.799973 0.561917 0.036 Uiso 1 1 calc R . . . .
C3 C 0.76698(15) 0.62824(15) 0.54497(7) 0.0308(4) Uani 1 1 d . . . . .
H3 H 0.819384 0.607817 0.575391 0.037 Uiso 1 1 calc R . . . .
C4 C 0.83693(16) 0.62601(16) 0.49345(7) 0.0351(4) Uani 1 1 d . . . . .
C5 C 0.65476(18) 0.87630(17) 0.48862(8) 0.0398(4) Uani 1 1 d . . . . .
C6 C 0.60902(18) 0.88473(19) 0.43320(8) 0.0434(5) Uani 1 1 d . . . . .
C7 C 0.5723(2) 0.7906(2) 0.40518(9) 0.0546(6) Uani 1 1 d . . . . .
H7 H 0.575491 0.718319 0.421295 0.065 Uiso 1 1 calc R . . . .
C8 C 0.5311(3) 0.8015(3) 0.35369(10) 0.0696(7) Uani 1 1 d . . . . .
H8 H 0.504226 0.736957 0.334942 0.084 Uiso 1 1 calc R . . . .
C9 C 0.5289(3) 0.9057(3) 0.32970(11) 0.0704(8) Uani 1 1 d . . . . .
H9 H 0.502525 0.912933 0.294127 0.084 Uiso 1 1 calc R . . . .
C10 C 0.5647(3) 0.9982(3) 0.35719(15) 0.0889(12) Uani 1 1 d . . . . .
H10 H 0.562684 1.069967 0.340568 0.107 Uiso 1 1 calc R . . . .
C11 C 0.6044(3) 0.9895(3) 0.40934(13) 0.0757(9) Uani 1 1 d . . . . .
H11 H 0.628043 1.054910 0.428272 0.091 Uiso 1 1 calc R . . . .
C12 C 0.68778(18) 0.44500(16) 0.56072(8) 0.0374(4) Uani 1 1 d . . . . .
C13 C 0.58323(18) 0.37205(16) 0.55055(7) 0.0360(4) Uani 1 1 d . . . . .
C14 C 0.5961(2) 0.25577(17) 0.55780(9) 0.0453(5) Uani 1 1 d . . . . .
H14 H 0.669213 0.225988 0.569935 0.054 Uiso 1 1 calc R . . . .
C15 C 0.5026(2) 0.18421(18) 0.54731(9) 0.0523(6) Uani 1 1 d . . . . .
H15 H 0.511728 0.105179 0.551717 0.063 Uiso 1 1 calc R . . . .
C16 C 0.3957(2) 0.2277(2) 0.53042(9) 0.0516(5) Uani 1 1 d . . . . .
H16 H 0.331433 0.178423 0.523390 0.062 Uiso 1 1 calc R . . . .
C17 C 0.3819(2) 0.3430(2) 0.52368(9) 0.0477(5) Uani 1 1 d . . . . .
H17 H 0.308060 0.372541 0.512430 0.057 Uiso 1 1 calc R . . . .
C18 C 0.47581(19) 0.41507(17) 0.53336(8) 0.0400(4) Uani 1 1 d . . . . .
H18 H 0.466669 0.493908 0.528221 0.048 Uiso 1 1 calc R . . . .
N1 N 0.52170(15) 0.61126(13) 0.70735(6) 0.0360(3) Uani 1 1 d . . . . .
H1 H 0.585(3) 0.647(3) 0.6800(13) 0.079(10) Uiso 1 1 d . . . . .
N2 N 0.33043(18) 0.57376(15) 0.77746(7) 0.0466(4) Uani 1 1 d . . . . .
C19 C 0.45552(19) 0.71126(17) 0.72819(9) 0.0424(4) Uani 1 1 d . . . . .
H19A H 0.448057 0.768384 0.699795 0.051 Uiso 1 1 calc R . . . .
H19B H 0.500613 0.745432 0.757714 0.051 Uiso 1 1 calc R . . . .
C20 C 0.3335(2) 0.67874(18) 0.74760(10) 0.0498(5) Uani 1 1 d . . . . .
H20A H 0.302651 0.740105 0.770281 0.060 Uiso 1 1 calc R . . . .
H20B H 0.280268 0.671701 0.716660 0.060 Uiso 1 1 calc R . . . .
C21 C 0.31449(19) 0.47295(17) 0.74730(8) 0.0420(4) Uani 1 1 d . . . . .
C22 C 0.2426(2) 0.3898(2) 0.76897(9) 0.0507(5) Uani 1 1 d . . . . .
H22 H 0.207051 0.401695 0.802601 0.061 Uiso 1 1 calc R . . . .
C23 C 0.2223(2) 0.2904(2) 0.74231(11) 0.0555(6) Uani 1 1 d . . . . .
H23 H 0.173530 0.234032 0.757700 0.067 Uiso 1 1 calc R . . . .
C24 C 0.2726(2) 0.27262(19) 0.69341(10) 0.0530(5) Uani 1 1 d . . . . .
H24 H 0.257537 0.204713 0.674654 0.064 Uiso 1 1 calc R . . . .
C25 C 0.3454(2) 0.35417(19) 0.67166(9) 0.0467(5) Uani 1 1 d . . . . .
H25 H 0.380645 0.341240 0.638053 0.056 Uiso 1 1 calc R . . . .
C26 C 0.36778(18) 0.45490(17) 0.69820(8) 0.0400(4) Uani 1 1 d . . . . .
C27 C 0.4480(2) 0.53899(19) 0.67130(8) 0.0416(4) Uani 1 1 d . . . . .
H27A H 0.501810 0.497291 0.647367 0.050 Uiso 1 1 calc R . . . .
H27B H 0.398833 0.589083 0.649007 0.050 Uiso 1 1 calc R . . . .
C28 C 0.58774(19) 0.54719(16) 0.74785(7) 0.0379(4) Uani 1 1 d . . . . .
C29 C 0.6986(2) 0.50936(17) 0.73286(9) 0.0458(5) Uani 1 1 d . . . . .
H29 H 0.725318 0.519781 0.697522 0.055 Uiso 1 1 calc R . . . .
C30 C 0.7702(2) 0.4562(2) 0.76973(11) 0.0583(6) Uani 1 1 d . . . . .
H30 H 0.846425 0.430052 0.759839 0.070 Uiso 1 1 calc R . . . .
C31 C 0.7300(3) 0.4415(2) 0.82100(11) 0.0614(7) Uani 1 1 d . . . . .
H31 H 0.779706 0.407321 0.846723 0.074 Uiso 1 1 calc R . . . .
C32 C 0.6184(3) 0.47631(19) 0.83485(9) 0.0547(6) Uani 1 1 d . . . . .
H32 H 0.591140 0.463289 0.869922 0.066 Uiso 1 1 calc R . . . .
C33 C 0.5441(2) 0.53017(17) 0.79883(8) 0.0441(5) Uani 1 1 d . . . . .
C34 C 0.4218(2) 0.5652(2) 0.81782(8) 0.0522(6) Uani 1 1 d . . . . .
H34A H 0.395251 0.510214 0.844814 0.063 Uiso 1 1 calc R . . . .
H34B H 0.428789 0.639311 0.835586 0.063 Uiso 1 1 calc R . . . .
O1S O 0.4774(7) 0.5175(7) 0.3709(4) 0.164(4) Uani 0.679(6) 1 d . . P A 1
O1T O 0.4896(8) 0.4521(12) 0.3080(4) 0.130(5) Uani 0.321(6) 1 d . . P A 2
C1S C 0.5859(4) 0.3793(7) 0.40943(19) 0.096(2) Uani 0.679(6) 1 d . . P A 1
H1SA H 0.645475 0.345833 0.386047 0.144 Uiso 0.679(6) 1 calc GR . P A 1
H1SB H 0.556718 0.321894 0.434108 0.144 Uiso 0.679(6) 1 calc GR . P A 1
H1SC H 0.621341 0.441449 0.429439 0.144 Uiso 0.679(6) 1 calc GR . P A 1
C1T C 0.431(3) 0.312(3) 0.3509(14) 0.184(18) Uani 0.321(6) 1 d . . P A 2
H1TA H 0.346948 0.308834 0.360459 0.276 Uiso 0.321(6) 1 calc GR . P A 2
H1TB H 0.477622 0.274892 0.378691 0.276 Uiso 0.321(6) 1 calc GR . P A 2
H1TC H 0.443025 0.272305 0.317221 0.276 Uiso 0.321(6) 1 calc GR . P A 2
C2S C 0.4900(6) 0.4209(7) 0.3784(4) 0.092(2) Uani 0.679(6) 1 d . . P A 1
C2T C 0.4607(18) 0.4059(18) 0.3467(7) 0.101(5) Uani 0.321(6) 1 d . . P A 2
C3S C 0.4126(13) 0.3292(13) 0.3536(7) 0.238(12) Uani 0.679(6) 1 d . . P A 1
H3SA H 0.378642 0.357194 0.320363 0.357 Uiso 0.679(6) 1 calc GR . P A 1
H3SB H 0.348741 0.309414 0.378124 0.357 Uiso 0.679(6) 1 calc GR . P A 1
H3SC H 0.460710 0.262294 0.346360 0.357 Uiso 0.679(6) 1 calc GR . P A 1
C3T C 0.415(2) 0.498(3) 0.3894(7) 0.140(9) Uani 0.321(6) 1 d . . P A 2
H3TA H 0.334157 0.478271 0.400576 0.210 Uiso 0.321(6) 1 calc GR . P A 2
H3TB H 0.414653 0.572713 0.373256 0.210 Uiso 0.321(6) 1 calc GR . P A 2
H3TC H 0.467015 0.497414 0.420332 0.210 Uiso 0.321(6) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.261(2) . ?
O2 C1 1.240(2) . ?
O3 C2 1.437(2) . ?
O3 C5 1.339(2) . ?
O4 C5 1.202(3) . ?
O5 H5 0.89(3) . ?
O5 C4 1.310(2) . ?
O6 C4 1.199(2) . ?
O7 C3 1.438(2) . ?
O7 C12 1.343(2) . ?
O8 C12 1.199(3) . ?
C1 C2 1.527(2) . ?
C2 H2 1.0000 . ?
C2 C3 1.518(3) . ?
C3 H3 1.0000 . ?
C3 C4 1.522(2) . ?
C5 C6 1.495(3) . ?
C6 C7 1.386(4) . ?
C6 C11 1.382(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.360(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.488(3) . ?
C13 C14 1.399(3) . ?
C13 C18 1.388(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.387(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(3) . ?
C18 H18 0.9500 . ?
N1 H1 1.08(4) . ?
N1 C19 1.498(3) . ?
N1 C27 1.503(3) . ?
N1 C28 1.477(2) . ?
N2 C20 1.456(3) . ?
N2 C21 1.429(3) . ?
N2 C34 1.455(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.515(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.391(3) . ?
C21 C26 1.395(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.377(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.384(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(3) . ?
C26 C27 1.511(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.385(3) . ?
C28 C33 1.393(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.383(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.374(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.393(3) . ?
C33 C34 1.523(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
O1S C2S 1.170(11) . ?
O1T C2T 1.167(17) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.426(8) . ?
C1T H1TA 0.9800 . ?
C1T H1TB 0.9800 . ?
C1T H1TC 0.9800 . ?
C1T C2T 1.17(4) . ?
C2S C3S 1.532(16) . ?
C2T C3T 1.62(3) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C3T H3TA 0.9800 . ?
C3T H3TB 0.9800 . ?
C3T H3TC 0.9800 . ?

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
C5 O3 C2 118.39(14) . . ?
C4 O5 H5 111.9(19) . . ?
C12 O7 C3 118.10(14) . . ?
O1 C1 C2 113.09(15) . . ?
O2 C1 O1 125.44(17) . . ?
O2 C1 C2 121.46(15) . . ?
O3 C2 C1 112.07(14) . . ?
O3 C2 H2 110.0 . . ?
O3 C2 C3 105.39(13) . . ?
C1 C2 H2 110.0 . . ?
C3 C2 C1 109.34(14) . . ?
C3 C2 H2 110.0 . . ?
O7 C3 C2 106.44(13) . . ?
O7 C3 H3 110.1 . . ?
O7 C3 C4 108.44(14) . . ?
C2 C3 H3 110.1 . . ?
C2 C3 C4 111.68(15) . . ?
C4 C3 H3 110.1 . . ?
O5 C4 C3 110.80(16) . . ?
O6 C4 O5 126.03(18) . . ?
O6 C4 C3 123.16(18) . . ?
O3 C5 C6 111.04(17) . . ?
O4 C5 O3 123.37(18) . . ?
O4 C5 C6 125.59(19) . . ?
C7 C6 C5 121.84(19) . . ?
C11 C6 C5 118.7(2) . . ?
C11 C6 C7 119.4(2) . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.3(2) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.2(3) . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C10 119.3(3) . . ?
C6 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
O7 C12 C13 111.09(16) . . ?
O8 C12 O7 123.52(19) . . ?
O8 C12 C13 125.39(18) . . ?
C14 C13 C12 117.89(18) . . ?
C18 C13 C12 122.43(17) . . ?
C18 C13 C14 119.67(19) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.0(2) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.1(2) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 120.0 . . ?
C17 C18 C13 119.98(19) . . ?
C17 C18 H18 120.0 . . ?
C19 N1 H1 103.9(18) . . ?
C19 N1 C27 112.77(17) . . ?
C27 N1 H1 101.9(18) . . ?
C28 N1 H1 108.2(18) . . ?
C28 N1 C19 114.69(15) . . ?
C28 N1 C27 113.96(15) . . ?
C21 N2 C20 116.32(18) . . ?
C21 N2 C34 113.85(18) . . ?
C34 N2 C20 113.88(19) . . ?
N1 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
N1 C19 C20 111.55(17) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
N2 C20 C19 114.03(19) . . ?
N2 C20 H20A 108.7 . . ?
N2 C20 H20B 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C22 C21 N2 117.28(19) . . ?
C22 C21 C26 119.5(2) . . ?
C26 C21 N2 123.17(19) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.9(2) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.7(2) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.2(2) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C27 123.91(19) . . ?
C25 C26 C21 118.7(2) . . ?
C25 C26 C27 117.39(19) . . ?
N1 C27 C26 116.01(16) . . ?
N1 C27 H27A 108.3 . . ?
N1 C27 H27B 108.3 . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C29 C28 N1 115.86(18) . . ?
C29 C28 C33 121.8(2) . . ?
C33 C28 N1 122.31(19) . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(2) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 120.2 . . ?
C31 C30 C29 119.5(3) . . ?
C31 C30 H30 120.2 . . ?
C30 C31 H31 119.9 . . ?
C32 C31 C30 120.2(2) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 H32 119.1 . . ?
C31 C32 C33 121.8(2) . . ?
C33 C32 H32 119.1 . . ?
C28 C33 C32 117.1(2) . . ?
C28 C33 C34 125.0(2) . . ?
C32 C33 C34 117.9(2) . . ?
N2 C34 C33 116.39(17) . . ?
N2 C34 H34A 108.2 . . ?
N2 C34 H34B 108.2 . . ?
C33 C34 H34A 108.2 . . ?
C33 C34 H34B 108.2 . . ?
H34A C34 H34B 107.3 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1TA C1T H1TB 109.5 . . ?
H1TA C1T H1TC 109.5 . . ?
H1TB C1T H1TC 109.5 . . ?
C2T C1T H1TA 109.5 . . ?
C2T C1T H1TB 109.5 . . ?
C2T C1T H1TC 109.5 . . ?
O1S C2S C1S 121.4(8) . . ?
O1S C2S C3S 124.1(8) . . ?
C1S C2S C3S 114.4(8) . . ?
O1T C2T C1T 127(2) . . ?
O1T C2T C3T 109.4(19) . . ?
C1T C2T C3T 119(2) . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C2T C3T H3TA 109.5 . . ?
C2T C3T H3TB 109.5 . . ?
C2T C3T H3TC 109.5 . . ?
H3TA C3T H3TB 109.5 . . ?
H3TA C3T H3TC 109.5 . . ?
H3TB C3T H3TC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 1.08(4) 1.49(3) 2.575(2) 179(3) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O3 170.46(15) . . . . ?
O1 C1 C2 C3 54.0(2) . . . . ?
O2 C1 C2 O3 -8.3(2) . . . . ?
O2 C1 C2 C3 -124.74(18) . . . . ?
O3 C2 C3 O7 -67.95(16) . . . . ?
O3 C2 C3 C4 50.23(18) . . . . ?
O3 C5 C6 C7 -2.2(3) . . . . ?
O3 C5 C6 C11 178.4(2) . . . . ?
O4 C5 C6 C7 177.5(2) . . . . ?
O4 C5 C6 C11 -1.9(4) . . . . ?
O7 C3 C4 O5 158.89(15) . . . . ?
O7 C3 C4 O6 -21.7(3) . . . . ?
O7 C12 C13 C14 165.68(17) . . . . ?
O7 C12 C13 C18 -13.0(3) . . . . ?
O8 C12 C13 C14 -14.4(3) . . . . ?
O8 C12 C13 C18 166.9(2) . . . . ?
C1 C2 C3 O7 52.69(17) . . . . ?
C1 C2 C3 C4 170.87(14) . . . . ?
C2 O3 C5 O4 -11.1(3) . . . . ?
C2 O3 C5 C6 168.57(15) . . . . ?
C2 C3 C4 O5 41.9(2) . . . . ?
C2 C3 C4 O6 -138.7(2) . . . . ?
C3 O7 C12 O8 3.0(3) . . . . ?
C3 O7 C12 C13 -177.00(15) . . . . ?
C5 O3 C2 C1 101.23(18) . . . . ?
C5 O3 C2 C3 -139.94(16) . . . . ?
C5 C6 C7 C8 -179.6(2) . . . . ?
C5 C6 C11 C10 178.4(3) . . . . ?
C6 C7 C8 C9 1.5(4) . . . . ?
C7 C6 C11 C10 -1.0(5) . . . . ?
C7 C8 C9 C10 -1.6(5) . . . . ?
C8 C9 C10 C11 0.4(5) . . . . ?
C9 C10 C11 C6 1.0(5) . . . . ?
C11 C6 C7 C8 -0.2(4) . . . . ?
C12 O7 C3 C2 -143.95(15) . . . . ?
C12 O7 C3 C4 95.76(18) . . . . ?
C12 C13 C14 C15 -178.05(19) . . . . ?
C12 C13 C18 C17 178.95(19) . . . . ?
C13 C14 C15 C16 -1.0(3) . . . . ?
C14 C13 C18 C17 0.3(3) . . . . ?
C14 C15 C16 C17 0.3(4) . . . . ?
C15 C16 C17 C18 0.7(4) . . . . ?
C16 C17 C18 C13 -0.9(3) . . . . ?
C18 C13 C14 C15 0.7(3) . . . . ?
N1 C19 C20 N2 41.8(3) . . . . ?
N1 C28 C29 C30 175.0(2) . . . . ?
N1 C28 C33 C32 -174.93(18) . . . . ?
N1 C28 C33 C34 5.4(3) . . . . ?
N2 C21 C22 C23 179.7(2) . . . . ?
N2 C21 C26 C25 -179.2(2) . . . . ?
N2 C21 C26 C27 0.0(3) . . . . ?
C19 N1 C27 C26 -82.7(2) . . . . ?
C19 N1 C28 C29 -139.65(18) . . . . ?
C19 N1 C28 C33 37.4(3) . . . . ?
C20 N2 C21 C22 -141.2(2) . . . . ?
C20 N2 C21 C26 39.2(3) . . . . ?
C20 N2 C34 C33 -80.8(2) . . . . ?
C21 N2 C20 C19 -88.3(3) . . . . ?
C21 N2 C34 C33 55.7(2) . . . . ?
C21 C22 C23 C24 -0.5(4) . . . . ?
C21 C26 C27 N1 32.3(3) . . . . ?
C22 C21 C26 C25 1.2(3) . . . . ?
C22 C21 C26 C27 -179.5(2) . . . . ?
C22 C23 C24 C25 1.2(4) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C24 C25 C26 C21 -0.5(3) . . . . ?
C24 C25 C26 C27 -179.9(2) . . . . ?
C25 C26 C27 N1 -148.42(19) . . . . ?
C26 C21 C22 C23 -0.7(3) . . . . ?
C27 N1 C19 C20 45.9(2) . . . . ?
C27 N1 C28 C29 88.3(2) . . . . ?
C27 N1 C28 C33 -94.7(2) . . . . ?
C28 N1 C19 C20 -86.8(2) . . . . ?
C28 N1 C27 C26 50.3(2) . . . . ?
C28 C29 C30 C31 0.1(3) . . . . ?
C28 C33 C34 N2 26.0(3) . . . . ?
C29 C28 C33 C32 2.0(3) . . . . ?
C29 C28 C33 C34 -177.6(2) . . . . ?
C29 C30 C31 C32 2.0(4) . . . . ?
C30 C31 C32 C33 -2.1(4) . . . . ?
C31 C32 C33 C28 0.2(3) . . . . ?
C31 C32 C33 C34 179.8(2) . . . . ?
C32 C33 C34 N2 -153.7(2) . . . . ?
C33 C28 C29 C30 -2.1(3) . . . . ?
C34 N2 C20 C19 47.1(3) . . . . ?
C34 N2 C21 C22 83.3(2) . . . . ?
C34 N2 C21 C26 -96.2(2) . . . . ?

_olex2_date_sample_data_collection 2020-05-25
_olex2_date_sample_submission    2020-05-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a glass fibre with Paratone oil'
_olex2_submission_original_sample_id cx1883
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.934
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive
####################################################################### 
# 
# 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_MR524
_database_code_depnum_ccdc_archive 'CCDC 2123650'
loop_
_audit_author_name
_audit_author_address
'Masoud Kazem-Rostami'
;Northwestern University
United States of America
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_audit_creation_date             2022-07-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
''
''
_chemical_name_common            MR524
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H36 N2 O6'
_chemical_formula_sum            'C34 H36 N2 O6'
_chemical_formula_weight         568.65
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C34H36N2O6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   15.8359(4)
_cell_length_b                   8.6724(2)
_cell_length_c                   20.5944(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.268(2)
_cell_angle_gamma                90
_cell_volume                     2816.40(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17420
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7650
_cell_measurement_theta_min      2.1160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.2603
0 1 0 0.2603
0 0 -1 0.0057
0 0 1 0.0037
-1 0 0 0.0146
1 0 0 0.0010

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.521
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.009
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0076 -0.9990 -0.0010 -0.1530 0.0876 -0.0209
0.0076 0.9990 0.0010 0.1530 -0.0876 0.0209
0.0000 -0.0009 -0.9985 -0.0362 -0.0536 0.0380
-0.0000 0.0009 0.9985 0.0362 0.0536 -0.0380
-1.0003 0.0015 0.0016 -0.0206 -0.0542 -0.0787
1.0003 -0.0015 -0.0016 0.0206 0.0542 0.0787

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40331
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.285
_diffrn_reflns_theta_min         2.802
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -54.00   0.50    7.50    --  -47.44-154.00 -48.00  132
  2  ω    -92.00 -10.00   0.50    7.50    --  -47.44 120.00-167.00  164
  3  ω   -112.00 -29.00   0.50    7.50    --  -47.44 154.00  -9.00  166
  4  ω     33.00 112.00   0.50    7.50    --   47.44-154.00 -48.00  158
  5  ω     59.00 120.00   0.50    7.50    --   47.44 154.00  -9.00  122
  6  ω     29.00  54.00   0.50    7.50    --   47.44-120.00 108.00   50
  7  ω    -97.00 -53.00   0.50   24.00    -- -104.00 154.00  -9.00   88
  8  ω   -151.00-126.00   0.50   24.00    -- -104.00-120.00 108.00   50
  9  ω   -132.00-105.00   0.50   24.00    -- -104.00 154.00  -9.00   54
 10  ω   -101.00 -69.00   0.50   24.00    -- -104.00 120.00-167.00   64
 11  ω     73.00  99.00   0.50   24.00    --  110.25-120.00 108.00   52
 12  ω     39.00  89.00   0.50   24.00    --  110.25-154.00 -48.00  100
 13  ω     82.00 169.00   0.50   24.00    --  110.25 120.00-167.00  174
 14  ω   -120.00 -33.00   0.50    7.50    --  -47.44 -57.00  30.00  174
 15  ω     -7.00  22.00   0.50    7.50    --  -47.44  19.00-180.00   58
 16  ω   -118.00 -74.00   0.50    7.50    --  -47.44-125.00 -90.00   88
 17  ω    -60.00  25.00   0.50    7.50    --  -47.44  57.00 -30.00  170
 18  ω   -120.00 -74.00   0.50    7.50    --  -47.44-125.00-120.00   92
 19  ω   -114.00 -75.00   0.50    7.50    --  -47.44 -77.00  60.00   78
 20  ω    -20.00  39.00   0.50    7.50    --   47.44 -37.00 120.00  118
 21  ω    -57.00 -32.00   0.50   24.00    -- -104.00  61.00  60.00   50
 22  ω   -138.00 -92.00   0.50   24.00    -- -104.00 -48.00  10.01   92
 23  ω   -174.00 -96.00   0.50   24.00    -- -104.00 -50.00 129.84  156
 24  ω    -68.00 -34.00   0.50   24.00    -- -104.00  61.00-150.00   68
 25  ω   -173.00-145.00   0.50   24.00    -- -104.00 -62.00-153.53   56
 26  ω   -174.00-103.00   0.50   24.00    -- -104.00 -54.00  37.50  142
 27  ω   -128.00 -87.00   0.50   24.00    -- -104.00 -62.00-153.53   82
 28  ω    -91.00 -39.00   0.50   24.00    -- -104.00 144.00 173.32  104
 29  ω    -57.00 -31.00   0.50   24.00    -- -104.00 116.00 128.81   52
 30  ω    -68.00 -39.00   0.50   24.00    -- -104.00  61.00 150.00   58
 31  ω   -108.00 -36.00   0.50   24.00    -- -104.00 112.00 -98.01  144
 32  ω   -174.00-144.00   0.50   24.00    -- -104.00 -48.00  10.01   60
 33  ω    -69.00 -32.00   0.50   24.00    -- -104.00  61.00  30.00   74
 34  ω   -107.00 -79.00   0.50   24.00    -- -104.00 108.00  28.12   56
 35  ω    -67.00 -38.00   0.50   24.00    -- -104.00  61.00   0.00   58
 36  ω   -125.00 -99.00   0.50   24.00    -- -104.00 144.00 173.32   52
 37  ω   -109.00 -70.00   0.50   24.00    -- -104.00 116.00 128.81   78
 38  ω     70.00  97.00   0.50   24.00    --  110.25 -94.00 -60.00   54
 39  ω     38.00  66.00   0.50   24.00    --  110.25 -61.00  90.00   56
 40  ω     38.00  65.00   0.50   24.00    --  110.25 -94.00 -60.00   54
 41  ω    108.00 178.00   0.50   24.00    --  110.25  30.00-180.00  140
 42  ω     66.00 101.00   0.50   24.00    --  110.25-125.00 -30.00   70
 43  ω    142.00 178.00   0.50   24.00    --  110.25  61.00 -90.00   72
 44  ω     97.00 130.00   0.50   24.00    --  110.25  61.00 -90.00   66
 45  ω     45.00  70.00   0.50   24.00    --  110.25 -61.00   0.00   50
 46  ω     54.00 110.00   0.50   24.00    --  110.25-125.00-120.00  112
 47  ω     73.00 106.00   0.50   24.00    --  110.25-104.00  99.90   66
 48  ω     83.00 111.00   0.50   24.00    --  110.25-125.00  30.00   56
 49  ω    153.00 178.00   0.50   24.00    --  110.25  45.00   0.00   50
 50  ω     39.00  86.00   0.50   24.00    --  110.25 -94.00 150.00   94
 51  ω    114.00 140.00   0.50   24.00    --  110.25  45.00   0.00   52
 52  ω     47.00  73.00   0.50   24.00    --  110.25 -61.00 150.00   52
 53  ω     87.00 112.00   0.50   24.00    --  110.25 154.00  -9.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0208505000
_diffrn_orient_matrix_UB_12      0.1529818000
_diffrn_orient_matrix_UB_13      0.0360763000
_diffrn_orient_matrix_UB_21      0.0541641000
_diffrn_orient_matrix_UB_22      -0.0881149000
_diffrn_orient_matrix_UB_23      0.0537329000
_diffrn_orient_matrix_UB_31      0.0786177000
_diffrn_orient_matrix_UB_32      0.0203493000
_diffrn_orient_matrix_UB_33      -0.0380385000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                9697
_reflns_number_total             11401
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 
;
 Flack x determined using 3839 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         11401
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0682P)²+0.9971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1355
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C32(H32A,H32B), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,
 H3AB), C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,H12D), C13A(H13C,H13D),
 C22A(H22C,H22D), C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D), C32A(H32C,
 H32D)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C27(H27), C28(H28), C31(H31), C33(H33), C6A(H6A), C7A(H7A), C9A(H9A),
 C15A(H15A), C16A(H16A), C19A(H19A), C20A(H20A), C21A(H21A), C27A(H27A),
 C28A(H28A), C31A(H31A), C33A(H33A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.37373(17) 0.6351(3) 0.47550(13) 0.0298(6) Uani 1 1 d . . . . .
O2 O 0.40351(18) 0.7570(3) 0.34831(14) 0.0356(6) Uani 1 1 d . . . . .
O3 O 0.24063(18) 0.7931(3) 0.28564(15) 0.0357(7) Uani 1 1 d . . . . .
O4 O -0.07367(18) 0.4038(3) 0.25460(14) 0.0358(7) Uani 1 1 d . . . . .
O5 O -0.13472(18) 0.0969(3) 0.21701(13) 0.0344(6) Uani 1 1 d . . . . .
O6 O -0.03370(17) 0.0738(3) 0.34600(13) 0.0286(6) Uani 1 1 d . . . . .
N1 N 0.2267(2) 0.0081(4) 0.54665(15) 0.0268(7) Uani 1 1 d . . . . .
N2 N 0.1540(2) 0.2635(4) 0.60465(15) 0.0265(7) Uani 1 1 d . . . . .
C1 C 0.1881(3) 0.1397(5) 0.64745(19) 0.0307(8) Uani 1 1 d . . . . .
H1A H 0.149609 0.122810 0.682006 0.037 Uiso 1 1 calc R U . . .
H1B H 0.243839 0.172216 0.668856 0.037 Uiso 1 1 calc R U . . .
C2 C 0.1991(3) -0.0120(4) 0.61161(18) 0.0298(8) Uani 1 1 d . . . . .
H2A H 0.241194 -0.076319 0.637758 0.036 Uiso 1 1 calc R U . . .
H2B H 0.144428 -0.068157 0.607983 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3000(2) 0.1094(4) 0.54459(19) 0.0283(8) Uani 1 1 d . . . . .
H3A H 0.328942 0.082694 0.505458 0.034 Uiso 1 1 calc R U . . .
H3B H 0.340111 0.086996 0.583200 0.034 Uiso 1 1 calc R U . . .
C4 C 0.2825(2) 0.2817(4) 0.54313(18) 0.0261(8) Uani 1 1 d . . . . .
C5 C 0.2144(2) 0.3492(4) 0.57155(17) 0.0247(7) Uani 1 1 d . . . . .
C6 C 0.2037(2) 0.5100(5) 0.56805(17) 0.0266(8) Uani 1 1 d . . . . .
H6 H 0.158225 0.556056 0.588082 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2574(2) 0.6023(5) 0.53630(17) 0.0273(8) Uani 1 1 d . . . . .
H7 H 0.248769 0.710643 0.534195 0.033 Uiso 1 1 calc R U . . .
C8 C 0.3246(2) 0.5353(4) 0.50725(18) 0.0270(8) Uani 1 1 d . . . . .
C9 C 0.3370(2) 0.3770(4) 0.51066(18) 0.0258(7) Uani 1 1 d . . . . .
H9 H 0.382932 0.332246 0.490779 0.031 Uiso 1 1 calc R U . . .
C10 C 0.4336(3) 0.5685(5) 0.4361(2) 0.0349(9) Uani 1 1 d . . . . .
H10A H 0.406230 0.486134 0.408332 0.042 Uiso 1 1 calc R U . . .
H10B H 0.481162 0.522351 0.464141 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4664(3) 0.6930(5) 0.3941(2) 0.0375(10) Uani 1 1 d . . . . .
H11A H 0.491108 0.776587 0.422565 0.045 Uiso 1 1 calc R U . . .
H11B H 0.512471 0.649756 0.370177 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3784(3) 0.6639(5) 0.2929(2) 0.0379(10) Uani 1 1 d . . . . .
H12A H 0.355350 0.564334 0.306792 0.045 Uiso 1 1 calc R U . . .
H12B H 0.427746 0.642575 0.267991 0.045 Uiso 1 1 calc R U . . .
C13 C 0.3118(3) 0.7509(5) 0.2512(2) 0.0365(9) Uani 1 1 d . . . . .
H13A H 0.337350 0.845471 0.234557 0.044 Uiso 1 1 calc R U . . .
H13B H 0.291689 0.686475 0.213212 0.044 Uiso 1 1 calc R U . . .
C14 C 0.1867(3) 0.6743(5) 0.3001(2) 0.0318(9) Uani 1 1 d . . . . .
C15 C 0.2023(3) 0.5916(5) 0.3565(2) 0.0329(9) Uani 1 1 d . . . . .
H15 H 0.252350 0.610442 0.384493 0.040 Uiso 1 1 calc R U . . .
C16 C 0.0714(3) 0.4517(4) 0.33318(19) 0.0291(8) Uani 1 1 d . . . . .
H16 H 0.032980 0.374034 0.344404 0.035 Uiso 1 1 calc R U . . .
C17 C 0.0533(3) 0.5391(5) 0.27536(19) 0.0307(8) Uani 1 1 d . . . . .
C18 C -0.0233(3) 0.5183(5) 0.23495(19) 0.0316(8) Uani 1 1 d . . . . .
C19 C -0.0415(3) 0.6086(5) 0.18065(19) 0.0348(9) Uani 1 1 d . . . . .
H19 H -0.093679 0.596051 0.154566 0.042 Uiso 1 1 calc R U . . .
C20 C 0.0177(3) 0.7201(5) 0.16371(19) 0.0359(9) Uani 1 1 d . . . . .
H20 H 0.004976 0.780850 0.125693 0.043 Uiso 1 1 calc R U . . .
C21 C 0.0920(3) 0.7424(5) 0.2003(2) 0.0358(9) Uani 1 1 d . . . . .
H21 H 0.130852 0.818197 0.188007 0.043 Uiso 1 1 calc R U . . .
C22 C -0.1518(3) 0.3700(5) 0.2161(2) 0.0334(9) Uani 1 1 d . . . . .
H22A H -0.142259 0.359911 0.169426 0.040 Uiso 1 1 calc R U . . .
H22B H -0.194008 0.452524 0.220737 0.040 Uiso 1 1 calc R U . . .
C23 C -0.1816(3) 0.2199(5) 0.2424(2) 0.0334(9) Uani 1 1 d . . . . .
H23A H -0.172965 0.220139 0.290586 0.040 Uiso 1 1 calc R U . . .
H23B H -0.242884 0.206016 0.229331 0.040 Uiso 1 1 calc R U . . .
C24 C -0.1245(3) -0.0341(5) 0.25866(19) 0.0300(8) Uani 1 1 d . . . . .
H24A H -0.133609 -0.128954 0.232175 0.036 Uiso 1 1 calc R U . . .
H24B H -0.167984 -0.031328 0.290225 0.036 Uiso 1 1 calc R U . . .
C25 C -0.0381(2) -0.0401(5) 0.29527(18) 0.0281(8) Uani 1 1 d . . . . .
H25A H -0.027789 -0.143898 0.314415 0.034 Uiso 1 1 calc R U . . .
H25B H 0.005901 -0.019440 0.265197 0.034 Uiso 1 1 calc R U . . .
C26 C 0.0341(2) 0.0605(4) 0.39248(17) 0.0248(7) Uani 1 1 d . . . . .
C27 C 0.1047(2) -0.0273(4) 0.38473(18) 0.0266(8) Uani 1 1 d . . . . .
H27 H 0.110386 -0.079031 0.344705 0.032 Uiso 1 1 calc R U . . .
C28 C 0.1679(2) -0.0395(4) 0.43630(18) 0.0270(8) Uani 1 1 d . . . . .
H28 H 0.216806 -0.099920 0.430978 0.032 Uiso 1 1 calc R U . . .
C29 C 0.1606(2) 0.0351(4) 0.49556(18) 0.0255(8) Uani 1 1 d . . . . .
C30 C 0.0901(2) 0.1292(4) 0.50239(18) 0.0248(7) Uani 1 1 d . . . . .
C31 C 0.0275(2) 0.1418(4) 0.45046(18) 0.0249(7) Uani 1 1 d . . . . .
H31 H -0.020193 0.206419 0.454489 0.030 Uiso 1 1 calc R U . . .
C32 C 0.0777(2) 0.2206(4) 0.56404(18) 0.0271(8) Uani 1 1 d . . . . .
H32A H 0.046280 0.316113 0.551115 0.032 Uiso 1 1 calc R U . . .
H32B H 0.041385 0.159098 0.590914 0.032 Uiso 1 1 calc R U . . .
C33 C 0.1444(3) 0.4792(5) 0.3731(2) 0.0344(9) Uani 1 1 d . . . . .
H33 H 0.155716 0.421440 0.412098 0.041 Uiso 1 1 calc R U . . .
C35 C 0.1121(3) 0.6513(5) 0.25776(18) 0.0291(8) Uani 1 1 d . . . . .
O1A O 0.29791(17) 0.9178(3) 0.01757(13) 0.0319(6) Uani 1 1 d . . . . .
O2A O 0.13981(19) 0.8591(4) -0.04513(14) 0.0390(7) Uani 1 1 d . . . . .
O3A O 0.0985(2) 0.5000(4) 0.02965(16) 0.0470(8) Uani 1 1 d . . . . .
O4A O 0.3149(2) 0.2305(4) 0.25561(15) 0.0416(7) Uani 1 1 d . . . . .
O5A O 0.44729(19) 0.2468(3) 0.36430(15) 0.0384(7) Uani 1 1 d . . . . .
O6A O 0.58018(18) 0.4217(3) 0.30801(13) 0.0306(6) Uani 1 1 d . . . . .
N1A N 0.6659(2) 0.7324(4) 0.08470(15) 0.0274(7) Uani 1 1 d . . . . .
N2A N 0.6185(2) 1.0021(4) 0.15021(14) 0.0272(7) Uani 1 1 d . . . . .
C1A C 0.6872(3) 1.0119(5) 0.10795(19) 0.0309(8) Uani 1 1 d . . . . .
H1AA H 0.731569 1.081784 0.128107 0.037 Uiso 1 1 calc R U . . .
H1AB H 0.665063 1.057320 0.065679 0.037 Uiso 1 1 calc R U . . .
C2A C 0.7269(3) 0.8563(5) 0.0956(2) 0.0306(8) Uani 1 1 d . . . . .
H2AA H 0.759632 0.864882 0.057101 0.037 Uiso 1 1 calc R U . . .
H2AB H 0.767180 0.829633 0.133598 0.037 Uiso 1 1 calc R U . . .
C3A C 0.5935(2) 0.7710(4) 0.03841(18) 0.0276(8) Uani 1 1 d . . . . .
H3AA H 0.568087 0.673413 0.021015 0.033 Uiso 1 1 calc R U . . .
H3AB H 0.615093 0.826774 0.001377 0.033 Uiso 1 1 calc R U . . .
C4A C 0.5232(3) 0.8679(4) 0.06388(17) 0.0272(8) Uani 1 1 d . . . . .
C5A C 0.5363(2) 0.9701(4) 0.11727(17) 0.0253(8) Uani 1 1 d . . . . .
C6A C 0.4673(3) 1.0451(4) 0.13935(19) 0.0285(8) Uani 1 1 d . . . . .
H6A H 0.476096 1.110592 0.176316 0.034 Uiso 1 1 calc R U . . .
C7A C 0.3859(3) 1.0279(4) 0.10948(18) 0.0286(8) Uani 1 1 d . . . . .
H7A H 0.339366 1.078479 0.126278 0.034 Uiso 1 1 calc R U . . .
C8A C 0.3737(2) 0.9349(4) 0.05422(17) 0.0272(8) Uani 1 1 d . . . . .
C9A C 0.4420(3) 0.8536(4) 0.03301(18) 0.0271(8) Uani 1 1 d . . . . .
H9A H 0.432708 0.786778 -0.003496 0.032 Uiso 1 1 calc R U . . .
C10A C 0.2304(3) 1.0167(5) 0.0321(2) 0.0344(9) Uani 1 1 d . . . . .
H10C H 0.251386 1.123567 0.038850 0.041 Uiso 1 1 calc R U . . .
H10D H 0.206486 0.981912 0.072367 0.041 Uiso 1 1 calc R U . . .
C11A C 0.1635(3) 1.0106(5) -0.0248(2) 0.0383(9) Uani 1 1 d . . . . .
H11C H 0.112467 1.065712 -0.012757 0.046 Uiso 1 1 calc R U . . .
H11D H 0.184768 1.066096 -0.062021 0.046 Uiso 1 1 calc R U . . .
C12A C 0.0984(3) 0.7742(6) 0.0006(2) 0.0414(10) Uani 1 1 d . . . . .
H12C H 0.040178 0.813940 0.003303 0.050 Uiso 1 1 calc R U . . .
H12D H 0.129788 0.781536 0.044341 0.050 Uiso 1 1 calc R U . . .
C13A C 0.0957(3) 0.6082(5) -0.0230(2) 0.0437(11) Uani 1 1 d . . . . .
H13C H 0.043096 0.591703 -0.052026 0.052 Uiso 1 1 calc R U . . .
H13D H 0.144448 0.589476 -0.048815 0.052 Uiso 1 1 calc R U . . .
C14A C 0.1739(3) 0.4809(5) 0.0672(2) 0.0391(10) Uani 1 1 d . . . . .
C15A C 0.2488(3) 0.5529(5) 0.0567(2) 0.0433(11) Uani 1 1 d . . . . .
H15A H 0.250882 0.623858 0.021702 0.052 Uiso 1 1 calc R U . . .
C16A C 0.3222(3) 0.4204(5) 0.1490(2) 0.0393(10) Uani 1 1 d . . . . .
H16A H 0.373372 0.398450 0.175145 0.047 Uiso 1 1 calc R U . . .
C17A C 0.2448(3) 0.3494(5) 0.1627(2) 0.0353(9) Uani 1 1 d . . . . .
C18A C 0.2398(3) 0.2512(5) 0.2177(2) 0.0361(9) Uani 1 1 d . . . . .
C19A C 0.1640(3) 0.1869(5) 0.2297(2) 0.0408(10) Uani 1 1 d . . . . .
H19A H 0.160502 0.124296 0.267242 0.049 Uiso 1 1 calc R U . . .
C20A C 0.0914(3) 0.2130(5) 0.1870(2) 0.0438(11) Uani 1 1 d . . . . .
H20A H 0.039640 0.164399 0.195112 0.053 Uiso 1 1 calc R U . . .
C21A C 0.0934(3) 0.3071(5) 0.1336(2) 0.0393(10) Uani 1 1 d . . . . .
H21A H 0.043375 0.324499 0.105441 0.047 Uiso 1 1 calc R U . . .
C22A C 0.3118(3) 0.1534(5) 0.3171(2) 0.0386(10) Uani 1 1 d . . . . .
H22C H 0.276875 0.058944 0.311268 0.046 Uiso 1 1 calc R U . . .
H22D H 0.286043 0.221866 0.348292 0.046 Uiso 1 1 calc R U . . .
C23A C 0.4008(3) 0.1124(5) 0.3428(2) 0.0412(10) Uani 1 1 d . . . . .
H23C H 0.399244 0.039399 0.379626 0.049 Uiso 1 1 calc R U . . .
H23D H 0.429694 0.060875 0.308098 0.049 Uiso 1 1 calc R U . . .
C24A C 0.5362(3) 0.2185(5) 0.3730(2) 0.0349(9) Uani 1 1 d . . . . .
H24C H 0.546334 0.108371 0.383649 0.042 Uiso 1 1 calc R U . . .
H24D H 0.561812 0.280896 0.409911 0.042 Uiso 1 1 calc R U . . .
C25A C 0.5779(3) 0.2586(4) 0.31212(19) 0.0307(8) Uani 1 1 d . . . . .
H25C H 0.636087 0.215988 0.314637 0.037 Uiso 1 1 calc R U . . .
H25D H 0.544995 0.215057 0.273187 0.037 Uiso 1 1 calc R U . . .
C26A C 0.6009(2) 0.4894(4) 0.25115(17) 0.0258(8) Uani 1 1 d . . . . .
C27A C 0.6118(2) 0.4111(5) 0.19337(18) 0.0289(8) Uani 1 1 d . . . . .
H27A H 0.604936 0.302434 0.190518 0.035 Uiso 1 1 calc R U . . .
C28A C 0.6330(2) 0.4967(5) 0.13986(18) 0.0267(8) Uani 1 1 d . . . . .
H28A H 0.640745 0.444175 0.100354 0.032 Uiso 1 1 calc R U . . .
C29A C 0.6433(2) 0.6554(4) 0.14217(17) 0.0253(8) Uani 1 1 d . . . . .
C30A C 0.6306(2) 0.7337(5) 0.20023(17) 0.0257(7) Uani 1 1 d . . . . .
C31A C 0.6103(2) 0.6483(4) 0.25381(17) 0.0255(8) Uani 1 1 d . . . . .
H31A H 0.602695 0.700401 0.293427 0.031 Uiso 1 1 calc R U . . .
C32A C 0.6393(2) 0.9071(4) 0.20870(18) 0.0264(8) Uani 1 1 d . . . . .
H32C H 0.602279 0.939850 0.242391 0.032 Uiso 1 1 calc R U . . .
H32D H 0.698492 0.929833 0.225698 0.032 Uiso 1 1 calc R U . . .
C33A C 0.3219(3) 0.5207(5) 0.0978(2) 0.0398(10) Uani 1 1 d . . . . .
H33A H 0.373407 0.570483 0.089783 0.048 Uiso 1 1 calc R U . . .
C35A C 0.1703(3) 0.3778(5) 0.1208(2) 0.0364(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C8 1.370(5) . ?
O1 C10 1.426(5) . ?
O2 C11 1.420(5) . ?
O2 C12 1.425(5) . ?
O3 C13 1.432(5) . ?
O3 C14 1.387(5) . ?
O4 C18 1.358(5) . ?
O4 C22 1.437(5) . ?
O5 C23 1.426(5) . ?
O5 C24 1.424(5) . ?
O6 C25 1.435(4) . ?
O6 C26 1.376(4) . ?
N1 C2 1.455(5) . ?
N1 C3 1.461(5) . ?
N1 C29 1.433(5) . ?
N2 C1 1.461(5) . ?
N2 C5 1.432(5) . ?
N2 C32 1.454(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.526(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.520(5) . ?
C4 C5 1.400(5) . ?
C4 C9 1.408(6) . ?
C5 C6 1.406(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.376(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.394(6) . ?
C8 C9 1.388(5) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.506(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.501(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.368(6) . ?
C14 C35 1.418(6) . ?
C15 H15 0.9500 . ?
C15 C33 1.402(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.418(6) . ?
C16 C33 1.377(6) . ?
C17 C18 1.418(6) . ?
C17 C35 1.417(6) . ?
C18 C19 1.374(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.412(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.352(6) . ?
C21 H21 0.9500 . ?
C21 C35 1.434(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.503(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.501(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.373(5) . ?
C26 C31 1.399(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.395(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(5) . ?
C29 C30 1.400(5) . ?
C30 C31 1.395(5) . ?
C30 C32 1.525(5) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33 0.9500 . ?
O1A C8A 1.366(5) . ?
O1A C10A 1.423(5) . ?
O2A C11A 1.419(6) . ?
O2A C12A 1.405(5) . ?
O3A C13A 1.432(5) . ?
O3A C14A 1.372(6) . ?
O4A C18A 1.373(6) . ?
O4A C22A 1.436(5) . ?
O5A C23A 1.427(5) . ?
O5A C24A 1.424(5) . ?
O6A C25A 1.418(5) . ?
O6A C26A 1.376(5) . ?
N1A C2A 1.448(5) . ?
N1A C3A 1.460(5) . ?
N1A C29A 1.433(5) . ?
N2A C1A 1.456(5) . ?
N2A C5A 1.439(5) . ?
N2A C32A 1.472(5) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C2A 1.520(6) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C4A 1.526(6) . ?
C4A C5A 1.413(5) . ?
C4A C9A 1.387(5) . ?
C5A C6A 1.384(6) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.384(6) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.394(5) . ?
C8A C9A 1.394(6) . ?
C9A H9A 0.9500 . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A C11A 1.506(6) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C13A 1.519(7) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C14A C15A 1.376(7) . ?
C14A C35A 1.425(6) . ?
C15A H15A 0.9500 . ?
C15A C33A 1.398(7) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.423(6) . ?
C16A C33A 1.367(7) . ?
C17A C18A 1.426(6) . ?
C17A C35A 1.417(7) . ?
C18A C19A 1.367(6) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.401(7) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.372(7) . ?
C21A H21A 0.9500 . ?
C21A C35A 1.409(6) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C22A C23A 1.502(7) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A H24C 0.9900 . ?
C24A H24D 0.9900 . ?
C24A C25A 1.509(6) . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C26A C27A 1.395(5) . ?
C26A C31A 1.387(5) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.395(6) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.386(5) . ?
C29A C30A 1.405(5) . ?
C30A C31A 1.391(5) . ?
C30A C32A 1.519(5) . ?
C31A H31A 0.9500 . ?
C32A H32C 0.9900 . ?
C32A H32D 0.9900 . ?
C33A H33A 0.9500 . ?

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
C8 O1 C10 116.9(3) . . ?
C11 O2 C12 115.9(3) . . ?
C14 O3 C13 116.4(3) . . ?
C18 O4 C22 118.9(3) . . ?
C24 O5 C23 114.2(3) . . ?
C26 O6 C25 115.5(3) . . ?
C2 N1 C3 113.9(3) . . ?
C29 N1 C2 115.7(3) . . ?
C29 N1 C3 114.2(3) . . ?
C5 N2 C1 116.3(3) . . ?
C5 N2 C32 114.5(3) . . ?
C32 N2 C1 113.6(3) . . ?
N2 C1 H1A 108.9 . . ?
N2 C1 H1B 108.9 . . ?
N2 C1 C2 113.2(3) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N1 C2 C1 113.5(3) . . ?
N1 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 H3A 108.2 . . ?
N1 C3 H3B 108.2 . . ?
N1 C3 C4 116.5(3) . . ?
H3A C3 H3B 107.3 . . ?
C4 C3 H3A 108.2 . . ?
C4 C3 H3B 108.2 . . ?
C5 C4 C3 123.3(3) . . ?
C5 C4 C9 118.8(3) . . ?
C9 C4 C3 117.9(3) . . ?
C4 C5 N2 123.7(3) . . ?
C4 C5 C6 119.2(3) . . ?
C6 C5 N2 117.1(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 C5 121.6(4) . . ?
C7 C6 H6 119.2 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C8 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
O1 C8 C7 115.5(3) . . ?
O1 C8 C9 124.4(4) . . ?
C9 C8 C7 120.0(4) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 C4 121.0(4) . . ?
C8 C9 H9 119.5 . . ?
O1 C10 H10A 110.0 . . ?
O1 C10 H10B 110.0 . . ?
O1 C10 C11 108.6(3) . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 H10A 110.0 . . ?
C11 C10 H10B 110.0 . . ?
O2 C11 C10 113.8(4) . . ?
O2 C11 H11A 108.8 . . ?
O2 C11 H11B 108.8 . . ?
C10 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
O2 C12 H12A 110.2 . . ?
O2 C12 H12B 110.2 . . ?
O2 C12 C13 107.6(4) . . ?
H12A C12 H12B 108.5 . . ?
C13 C12 H12A 110.2 . . ?
C13 C12 H12B 110.2 . . ?
O3 C13 C12 112.9(3) . . ?
O3 C13 H13A 109.0 . . ?
O3 C13 H13B 109.0 . . ?
C12 C13 H13A 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
O3 C14 C35 117.8(4) . . ?
C15 C14 O3 120.4(4) . . ?
C15 C14 C35 121.6(4) . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C33 120.0(4) . . ?
C33 C15 H15 120.0 . . ?
C17 C16 H16 119.9 . . ?
C33 C16 H16 119.9 . . ?
C33 C16 C17 120.1(4) . . ?
C18 C17 C16 121.3(4) . . ?
C35 C17 C16 119.7(4) . . ?
C35 C17 C18 119.0(4) . . ?
O4 C18 C17 114.3(3) . . ?
O4 C18 C19 125.1(4) . . ?
C19 C18 C17 120.6(4) . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.8(4) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.6(4) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C35 119.8(4) . . ?
C35 C21 H21 120.1 . . ?
O4 C22 H22A 110.7 . . ?
O4 C22 H22B 110.7 . . ?
O4 C22 C23 105.1(3) . . ?
H22A C22 H22B 108.8 . . ?
C23 C22 H22A 110.7 . . ?
C23 C22 H22B 110.7 . . ?
O5 C23 C22 108.9(3) . . ?
O5 C23 H23A 109.9 . . ?
O5 C23 H23B 109.9 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
O5 C24 H24A 109.2 . . ?
O5 C24 H24B 109.2 . . ?
O5 C24 C25 112.2(3) . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
O6 C25 C24 108.8(3) . . ?
O6 C25 H25A 109.9 . . ?
O6 C25 H25B 109.9 . . ?
C24 C25 H25A 109.9 . . ?
C24 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
O6 C26 C31 115.9(3) . . ?
C27 C26 O6 123.9(3) . . ?
C27 C26 C31 120.3(3) . . ?
C26 C27 H27 120.4 . . ?
C26 C27 C28 119.2(3) . . ?
C28 C27 H27 120.4 . . ?
C27 C28 H28 119.3 . . ?
C27 C28 C29 121.3(4) . . ?
C29 C28 H28 119.3 . . ?
C28 C29 N1 117.0(3) . . ?
C28 C29 C30 119.3(3) . . ?
C30 C29 N1 123.8(3) . . ?
C29 C30 C32 123.5(3) . . ?
C31 C30 C29 119.1(3) . . ?
C31 C30 C32 117.4(3) . . ?
C26 C31 H31 119.6 . . ?
C30 C31 C26 120.7(3) . . ?
C30 C31 H31 119.6 . . ?
N2 C32 C30 116.6(3) . . ?
N2 C32 H32A 108.1 . . ?
N2 C32 H32B 108.1 . . ?
C30 C32 H32A 108.1 . . ?
C30 C32 H32B 108.1 . . ?
H32A C32 H32B 107.3 . . ?
C15 C33 H33 119.7 . . ?
C16 C33 C15 120.5(4) . . ?
C16 C33 H33 119.7 . . ?
C14 C35 C21 122.6(4) . . ?
C17 C35 C14 118.0(4) . . ?
C17 C35 C21 119.2(4) . . ?
C8A O1A C10A 117.2(3) . . ?
C12A O2A C11A 114.5(3) . . ?
C14A O3A C13A 118.1(4) . . ?
C18A O4A C22A 117.7(3) . . ?
C24A O5A C23A 112.0(3) . . ?
C26A O6A C25A 119.1(3) . . ?
C2A N1A C3A 113.8(3) . . ?
C29A N1A C2A 115.5(3) . . ?
C29A N1A C3A 113.9(3) . . ?
C1A N2A C32A 113.5(3) . . ?
C5A N2A C1A 115.0(3) . . ?
C5A N2A C32A 113.7(3) . . ?
N2A C1A H1AA 109.0 . . ?
N2A C1A H1AB 109.0 . . ?
N2A C1A C2A 113.0(3) . . ?
H1AA C1A H1AB 107.8 . . ?
C2A C1A H1AA 109.0 . . ?
C2A C1A H1AB 109.0 . . ?
N1A C2A C1A 113.9(3) . . ?
N1A C2A H2AA 108.8 . . ?
N1A C2A H2AB 108.8 . . ?
C1A C2A H2AA 108.8 . . ?
C1A C2A H2AB 108.8 . . ?
H2AA C2A H2AB 107.7 . . ?
N1A C3A H3AA 108.0 . . ?
N1A C3A H3AB 108.0 . . ?
N1A C3A C4A 117.1(3) . . ?
H3AA C3A H3AB 107.3 . . ?
C4A C3A H3AA 108.0 . . ?
C4A C3A H3AB 108.0 . . ?
C5A C4A C3A 123.6(3) . . ?
C9A C4A C3A 117.9(3) . . ?
C9A C4A C5A 118.5(4) . . ?
C4A C5A N2A 123.3(3) . . ?
C6A C5A N2A 117.5(3) . . ?
C6A C5A C4A 119.1(3) . . ?
C5A C6A H6A 118.8 . . ?
C5A C6A C7A 122.3(3) . . ?
C7A C6A H6A 118.8 . . ?
C6A C7A H7A 120.7 . . ?
C6A C7A C8A 118.6(4) . . ?
C8A C7A H7A 120.7 . . ?
O1A C8A C7A 124.2(3) . . ?
O1A C8A C9A 116.1(3) . . ?
C7A C8A C9A 119.7(3) . . ?
C4A C9A C8A 121.6(3) . . ?
C4A C9A H9A 119.2 . . ?
C8A C9A H9A 119.2 . . ?
O1A C10A H10C 110.2 . . ?
O1A C10A H10D 110.2 . . ?
O1A C10A C11A 107.7(3) . . ?
H10C C10A H10D 108.5 . . ?
C11A C10A H10C 110.2 . . ?
C11A C10A H10D 110.2 . . ?
O2A C11A C10A 114.2(4) . . ?
O2A C11A H11C 108.7 . . ?
O2A C11A H11D 108.7 . . ?
C10A C11A H11C 108.7 . . ?
C10A C11A H11D 108.7 . . ?
H11C C11A H11D 107.6 . . ?
O2A C12A H12C 110.4 . . ?
O2A C12A H12D 110.4 . . ?
O2A C12A C13A 106.4(4) . . ?
H12C C12A H12D 108.6 . . ?
C13A C12A H12C 110.4 . . ?
C13A C12A H12D 110.4 . . ?
O3A C13A C12A 112.4(4) . . ?
O3A C13A H13C 109.1 . . ?
O3A C13A H13D 109.1 . . ?
C12A C13A H13C 109.1 . . ?
C12A C13A H13D 109.1 . . ?
H13C C13A H13D 107.9 . . ?
O3A C14A C15A 125.1(4) . . ?
O3A C14A C35A 114.7(4) . . ?
C15A C14A C35A 120.2(4) . . ?
C14A C15A H15A 120.3 . . ?
C14A C15A C33A 119.5(4) . . ?
C33A C15A H15A 120.3 . . ?
C17A C16A H16A 120.5 . . ?
C33A C16A H16A 120.5 . . ?
C33A C16A C17A 119.1(5) . . ?
C16A C17A C18A 121.8(4) . . ?
C35A C17A C16A 119.2(4) . . ?
C35A C17A C18A 118.9(4) . . ?
O4A C18A C17A 114.9(4) . . ?
C19A C18A O4A 125.0(4) . . ?
C19A C18A C17A 120.1(4) . . ?
C18A C19A H19A 119.9 . . ?
C18A C19A C20A 120.3(4) . . ?
C20A C19A H19A 119.9 . . ?
C19A C20A H20A 119.3 . . ?
C21A C20A C19A 121.4(4) . . ?
C21A C20A H20A 119.3 . . ?
C20A C21A H21A 120.2 . . ?
C20A C21A C35A 119.5(4) . . ?
C35A C21A H21A 120.2 . . ?
O4A C22A H22C 110.0 . . ?
O4A C22A H22D 110.0 . . ?
O4A C22A C23A 108.3(4) . . ?
H22C C22A H22D 108.4 . . ?
C23A C22A H22C 110.0 . . ?
C23A C22A H22D 110.0 . . ?
O5A C23A C22A 110.9(4) . . ?
O5A C23A H23C 109.5 . . ?
O5A C23A H23D 109.5 . . ?
C22A C23A H23C 109.5 . . ?
C22A C23A H23D 109.5 . . ?
H23C C23A H23D 108.1 . . ?
O5A C24A H24C 109.4 . . ?
O5A C24A H24D 109.4 . . ?
O5A C24A C25A 111.0(3) . . ?
H24C C24A H24D 108.0 . . ?
C25A C24A H24C 109.4 . . ?
C25A C24A H24D 109.4 . . ?
O6A C25A C24A 107.2(3) . . ?
O6A C25A H25C 110.3 . . ?
O6A C25A H25D 110.3 . . ?
C24A C25A H25C 110.3 . . ?
C24A C25A H25D 110.3 . . ?
H25C C25A H25D 108.5 . . ?
O6A C26A C27A 125.2(3) . . ?
O6A C26A C31A 115.1(3) . . ?
C31A C26A C27A 119.7(4) . . ?
C26A C27A H27A 120.9 . . ?
C26A C27A C28A 118.2(4) . . ?
C28A C27A H27A 120.9 . . ?
C27A C28A H28A 118.8 . . ?
C29A C28A C27A 122.5(3) . . ?
C29A C28A H28A 118.8 . . ?
C28A C29A N1A 118.2(3) . . ?
C28A C29A C30A 118.9(3) . . ?
C30A C29A N1A 122.9(3) . . ?
C29A C30A C32A 123.9(3) . . ?
C31A C30A C29A 118.6(3) . . ?
C31A C30A C32A 117.5(3) . . ?
C26A C31A C30A 122.0(3) . . ?
C26A C31A H31A 119.0 . . ?
C30A C31A H31A 119.0 . . ?
N2A C32A C30A 116.7(3) . . ?
N2A C32A H32C 108.1 . . ?
N2A C32A H32D 108.1 . . ?
C30A C32A H32C 108.1 . . ?
C30A C32A H32D 108.1 . . ?
H32C C32A H32D 107.3 . . ?
C15A C33A H33A 118.7 . . ?
C16A C33A C15A 122.6(4) . . ?
C16A C33A H33A 118.7 . . ?
C17A C35A C14A 119.3(4) . . ?
C21A C35A C14A 120.9(4) . . ?
C21A C35A C17A 119.7(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C10 H10A O5A 0.99 2.38 3.174(5) 136.8 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C8 C9 C4 -178.6(3) . . . . ?
O1 C10 C11 O2 -64.6(5) . . . . ?
O2 C12 C13 O3 -56.5(5) . . . . ?
O3 C14 C15 C33 175.5(4) . . . . ?
O3 C14 C35 C17 -174.6(3) . . . . ?
O3 C14 C35 C21 1.8(6) . . . . ?
O4 C18 C19 C20 -177.4(4) . . . . ?
O4 C22 C23 O5 -78.6(4) . . . . ?
O5 C24 C25 O6 74.2(4) . . . . ?
O6 C26 C27 C28 -176.6(3) . . . . ?
O6 C26 C31 C30 176.1(3) . . . . ?
N1 C3 C4 C5 29.4(5) . . . . ?
N1 C3 C4 C9 -149.6(3) . . . . ?
N1 C29 C30 C31 -177.0(3) . . . . ?
N1 C29 C30 C32 3.3(6) . . . . ?
N2 C1 C2 N1 36.9(5) . . . . ?
N2 C5 C6 C7 -178.8(3) . . . . ?
C1 N2 C5 C4 41.8(5) . . . . ?
C1 N2 C5 C6 -138.2(3) . . . . ?
C1 N2 C32 C30 -81.0(4) . . . . ?
C2 N1 C3 C4 -81.9(4) . . . . ?
C2 N1 C29 C28 -139.1(4) . . . . ?
C2 N1 C29 C30 40.0(5) . . . . ?
C3 N1 C2 C1 49.9(4) . . . . ?
C3 N1 C29 C28 85.7(4) . . . . ?
C3 N1 C29 C30 -95.2(4) . . . . ?
C3 C4 C5 N2 -0.3(5) . . . . ?
C3 C4 C5 C6 179.6(3) . . . . ?
C3 C4 C9 C8 179.8(3) . . . . ?
C4 C5 C6 C7 1.3(5) . . . . ?
C5 N2 C1 C2 -85.3(4) . . . . ?
C5 N2 C32 C30 55.9(4) . . . . ?
C5 C4 C9 C8 0.7(5) . . . . ?
C5 C6 C7 C8 -0.5(5) . . . . ?
C6 C7 C8 O1 178.6(3) . . . . ?
C6 C7 C8 C9 -0.2(5) . . . . ?
C7 C8 C9 C4 0.1(5) . . . . ?
C8 O1 C10 C11 167.2(3) . . . . ?
C9 C4 C5 N2 178.7(3) . . . . ?
C9 C4 C5 C6 -1.4(5) . . . . ?
C10 O1 C8 C7 -169.6(3) . . . . ?
C10 O1 C8 C9 9.1(5) . . . . ?
C11 O2 C12 C13 179.6(3) . . . . ?
C12 O2 C11 C10 -75.4(5) . . . . ?
C13 O3 C14 C15 88.0(5) . . . . ?
C13 O3 C14 C35 -97.3(4) . . . . ?
C14 O3 C13 C12 -72.0(5) . . . . ?
C14 C15 C33 C16 -0.5(6) . . . . ?
C15 C14 C35 C17 -0.1(6) . . . . ?
C15 C14 C35 C21 176.4(4) . . . . ?
C16 C17 C18 O4 -3.5(5) . . . . ?
C16 C17 C18 C19 177.2(4) . . . . ?
C16 C17 C35 C14 -1.5(5) . . . . ?
C16 C17 C35 C21 -178.1(4) . . . . ?
C17 C16 C33 C15 -1.1(6) . . . . ?
C17 C18 C19 C20 1.9(6) . . . . ?
C18 O4 C22 C23 168.2(3) . . . . ?
C18 C17 C35 C14 177.6(4) . . . . ?
C18 C17 C35 C21 1.0(6) . . . . ?
C18 C19 C20 C21 -1.0(6) . . . . ?
C19 C20 C21 C35 0.1(6) . . . . ?
C20 C21 C35 C14 -176.6(4) . . . . ?
C20 C21 C35 C17 -0.1(6) . . . . ?
C22 O4 C18 C17 -178.2(3) . . . . ?
C22 O4 C18 C19 1.1(6) . . . . ?
C23 O5 C24 C25 -101.5(4) . . . . ?
C24 O5 C23 C22 150.8(3) . . . . ?
C25 O6 C26 C27 15.9(5) . . . . ?
C25 O6 C26 C31 -163.4(3) . . . . ?
C26 O6 C25 C24 166.4(3) . . . . ?
C26 C27 C28 C29 0.2(6) . . . . ?
C27 C26 C31 C30 -3.3(5) . . . . ?
C27 C28 C29 N1 176.5(3) . . . . ?
C27 C28 C29 C30 -2.6(6) . . . . ?
C28 C29 C30 C31 2.1(5) . . . . ?
C28 C29 C30 C32 -177.6(3) . . . . ?
C29 N1 C2 C1 -85.4(4) . . . . ?
C29 N1 C3 C4 54.1(4) . . . . ?
C29 C30 C31 C26 0.8(5) . . . . ?
C29 C30 C32 N2 26.3(5) . . . . ?
C31 C26 C27 C28 2.7(5) . . . . ?
C31 C30 C32 N2 -153.5(3) . . . . ?
C32 N2 C1 C2 50.9(4) . . . . ?
C32 N2 C5 C4 -94.0(4) . . . . ?
C32 N2 C5 C6 86.1(4) . . . . ?
C32 C30 C31 C26 -179.5(3) . . . . ?
C33 C16 C17 C18 -177.0(4) . . . . ?
C33 C16 C17 C35 2.1(6) . . . . ?
C35 C14 C15 C33 1.1(6) . . . . ?
C35 C17 C18 O4 177.4(3) . . . . ?
C35 C17 C18 C19 -1.9(6) . . . . ?
O1A C8A C9A C4A 176.4(3) . . . . ?
O1A C10A C11A O2A 49.8(5) . . . . ?
O2A C12A C13A O3A 149.0(4) . . . . ?
O3A C14A C15A C33A -178.5(4) . . . . ?
O3A C14A C35A C17A 179.8(4) . . . . ?
O3A C14A C35A C21A -1.8(6) . . . . ?
O4A C18A C19A C20A -178.6(4) . . . . ?
O4A C22A C23A O5A 71.8(5) . . . . ?
O5A C24A C25A O6A 73.4(4) . . . . ?
O6A C26A C27A C28A -179.8(3) . . . . ?
O6A C26A C31A C30A -179.5(3) . . . . ?
N1A C3A C4A C5A 26.0(5) . . . . ?
N1A C3A C4A C9A -153.6(3) . . . . ?
N1A C29A C30A C31A -178.8(3) . . . . ?
N1A C29A C30A C32A 0.0(6) . . . . ?
N2A C1A C2A N1A 41.3(4) . . . . ?
N2A C5A C6A C7A 177.1(3) . . . . ?
C1A N2A C5A C4A 38.0(5) . . . . ?
C1A N2A C5A C6A -141.6(4) . . . . ?
C1A N2A C32A C30A -81.2(4) . . . . ?
C2A N1A C3A C4A -79.5(4) . . . . ?
C2A N1A C29A C28A -140.4(4) . . . . ?
C2A N1A C29A C30A 40.1(5) . . . . ?
C3A N1A C2A C1A 47.1(4) . . . . ?
C3A N1A C29A C28A 85.1(4) . . . . ?
C3A N1A C29A C30A -94.4(4) . . . . ?
C3A C4A C5A N2A 4.8(6) . . . . ?
C3A C4A C5A C6A -175.7(3) . . . . ?
C3A C4A C9A C8A 178.3(3) . . . . ?
C4A C5A C6A C7A -2.4(6) . . . . ?
C5A N2A C1A C2A -86.9(4) . . . . ?
C5A N2A C32A C30A 52.8(4) . . . . ?
C5A C4A C9A C8A -1.3(5) . . . . ?
C5A C6A C7A C8A -1.7(6) . . . . ?
C6A C7A C8A O1A -174.9(3) . . . . ?
C6A C7A C8A C9A 4.3(6) . . . . ?
C7A C8A C9A C4A -2.9(6) . . . . ?
C8A O1A C10A C11A 163.9(3) . . . . ?
C9A C4A C5A N2A -175.7(3) . . . . ?
C9A C4A C5A C6A 3.8(5) . . . . ?
C10A O1A C8A C7A 8.5(5) . . . . ?
C10A O1A C8A C9A -170.8(3) . . . . ?
C11A O2A C12A C13A -167.9(4) . . . . ?
C12A O2A C11A C10A 66.2(5) . . . . ?
C13A O3A C14A C15A -3.1(6) . . . . ?
C13A O3A C14A C35A 176.6(4) . . . . ?
C14A O3A C13A C12A -72.7(5) . . . . ?
C14A C15A C33A C16A -0.5(7) . . . . ?
C15A C14A C35A C17A -0.5(6) . . . . ?
C15A C14A C35A C21A 177.9(4) . . . . ?
C16A C17A C18A O4A -0.4(6) . . . . ?
C16A C17A C18A C19A 179.1(4) . . . . ?
C16A C17A C35A C14A -2.1(6) . . . . ?
C16A C17A C35A C21A 179.5(4) . . . . ?
C17A C16A C33A C15A -2.1(7) . . . . ?
C17A C18A C19A C20A 2.1(7) . . . . ?
C18A O4A C22A C23A 167.6(4) . . . . ?
C18A C17A C35A C14A 177.4(4) . . . . ?
C18A C17A C35A C21A -1.0(6) . . . . ?
C18A C19A C20A C21A -2.3(7) . . . . ?
C19A C20A C21A C35A 0.8(7) . . . . ?
C20A C21A C35A C14A -177.6(4) . . . . ?
C20A C21A C35A C17A 0.8(6) . . . . ?
C22A O4A C18A C17A 170.4(4) . . . . ?
C22A O4A C18A C19A -9.0(6) . . . . ?
C23A O5A C24A C25A 93.2(4) . . . . ?
C24A O5A C23A C22A -164.8(4) . . . . ?
C25A O6A C26A C27A 7.0(5) . . . . ?
C25A O6A C26A C31A -173.5(3) . . . . ?
C26A O6A C25A C24A -168.3(3) . . . . ?
C26A C27A C28A C29A -0.2(6) . . . . ?
C27A C26A C31A C30A 0.0(6) . . . . ?
C27A C28A C29A N1A 179.4(3) . . . . ?
C27A C28A C29A C30A -1.0(6) . . . . ?
C28A C29A C30A C31A 1.7(5) . . . . ?
C28A C29A C30A C32A -179.6(3) . . . . ?
C29A N1A C2A C1A -87.4(4) . . . . ?
C29A N1A C3A C4A 55.8(4) . . . . ?
C29A C30A C31A C26A -1.2(5) . . . . ?
C29A C30A C32A N2A 30.7(5) . . . . ?
C31A C26A C27A C28A 0.7(5) . . . . ?
C31A C30A C32A N2A -150.5(3) . . . . ?
C32A N2A C1A C2A 46.5(4) . . . . ?
C32A N2A C5A C4A -95.3(4) . . . . ?
C32A N2A C5A C6A 85.2(4) . . . . ?
C32A C30A C31A C26A 180.0(3) . . . . ?
C33A C16A C17A C18A -176.1(4) . . . . ?
C33A C16A C17A C35A 3.4(6) . . . . ?
C35A C14A C15A C33A 1.8(6) . . . . ?
C35A C17A C18A O4A -179.9(4) . . . . ?
C35A C17A C18A C19A -0.5(6) . . . . ?

_olex2_date_sample_data_collection 2021-11-19
_olex2_date_sample_submission    2021-11-11
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in paratone oil'
_olex2_submission_original_sample_id MR524
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.439
_oxdiff_exptl_absorpt_empirical_full_min 0.319
####################################################################### 
# 
# 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_MR530
_database_code_depnum_ccdc_archive 'CCDC 2131821'
loop_
_audit_author_name
_audit_author_address
'Masoud Kazem-Rostami'
;Northwestern University
United States of America
;
_audit_update_record             
;
2021-12-30 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_audit_creation_date             2021-12-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            MR530
_chemical_name_systematic        
'dodecahydro-1H,6H-2,8-(epoxyethanooxyethanooxy[1,5]naphthalenooxyethanooxyethanooxy)-5,11-ethanodibenzo[b,f][1,5]diazocine.1,2,7(4,1),6(1,4)-tetrapyridin-1-iuma-4,9(1,4)-dibenzenacyclodecaphane-11,21,61,71-tetraium.tetrakis hexafluorophosphate'
_chemical_formula_moiety         
'4(F6 P), C34 H36 N2 O6, H2 O, C36 H32 N4, C2 H3 N'
_chemical_formula_sum            'C72 H73 F24 N7 O7 P4'
_chemical_formula_weight         1728.25
_chemical_melting_point          NA
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   13.9868(3)
_cell_length_b                   22.2742(4)
_cell_length_c                   23.3991(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.2222(18)
_cell_angle_gamma                90
_cell_volume                     7270.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18089
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      77.1540
_cell_measurement_theta_min      2.7160
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.904
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black-purple
_exptl_crystal_colour_primary    black-purple
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3544
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/Water'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56425
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.834
_diffrn_reflns_theta_min         2.742
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -121.00 -48.00   0.50   11.42    --  -47.69  -4.00 -41.00  146
  2  ω    -33.00  -8.00   0.50   11.42    --  -47.69   4.00 136.00   50
  3  ω    -14.00  11.00   0.50   11.42    --   47.69  -4.00 -41.00   50
  4  ω    -92.00 -66.00   0.50   45.69    -- -104.00  -4.00 -41.00   52
  5  ω   -154.00 -93.00   0.50   45.69    -- -104.00  -4.00 -41.00  122
  6  ω     62.00 162.00   0.50   45.69    --  110.25   4.00 136.00  200
  7  ω    -37.00  13.00   0.50   11.42    --  -47.69  37.00 -90.00  100
  8  ω     11.00 117.00   0.50   11.42    --   47.69   4.00 136.00  212
  9  ω     44.00  93.00   0.50   11.42    --   47.69-125.00 -60.00   98
 10  ω   -111.00 -85.00   0.50   45.69    -- -104.00 125.00-180.00   52
 11  ω   -112.00 -78.00   0.50   45.69    -- -104.00 125.00-150.00   68
 12  ω   -108.00 -39.00   0.50   45.69    -- -104.00 111.00 171.47  138
 13  ω    -69.00 -34.00   0.50   45.69    -- -104.00  61.00 -90.00   70
 14  ω    -68.00 -41.00   0.50   45.69    -- -104.00  61.00 -60.00   54
 15  ω    -69.00 -43.00   0.50   45.69    -- -104.00  61.00-180.00   52
 16  ω     44.00  73.00   0.50   45.69    --  110.25 -61.00 -90.00   58
 17  ω     38.00  72.00   0.50   45.69    --  110.25 -61.00 120.00   68
 18  ω     96.00 177.00   0.50   45.69    --  110.25  77.00   0.00  162
 19  ω     80.00 106.00   0.50   45.69    --  110.25 -94.00 -90.00   52
 20  ω     79.00 106.00   0.50   45.69    --  110.25 -94.00-120.00   54
 21  ω     39.00 105.00   0.50   45.69    --  110.25 -94.00-180.00  132
 22  ω     44.00  69.00   0.50   45.69    --  110.25 -94.00-120.00   50
 23  ω     48.00  73.00   0.50   45.69    --  110.25 -61.00 -30.00   50
 24  ω     38.00  86.00   0.50   45.69    --  110.25 -77.00  90.00   96
 25  ω     81.00 106.00   0.50   45.69    --  110.25 -94.00   0.00   50
 26  ω     38.00  71.00   0.50   45.69    --  110.25 -94.00 -90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279654000
_diffrn_orient_matrix_UB_12      -0.0027763000
_diffrn_orient_matrix_UB_13      -0.0648718000
_diffrn_orient_matrix_UB_21      -0.1067384000
_diffrn_orient_matrix_UB_22      -0.0026722000
_diffrn_orient_matrix_UB_23      0.0120664000
_diffrn_orient_matrix_UB_31      -0.0053001000
_diffrn_orient_matrix_UB_32      0.0690444000
_diffrn_orient_matrix_UB_33      -0.0019981000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10614
_reflns_number_total             15052
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         15052
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1083P)²+5.1516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1957
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F6-H7B
 2.05 with sigma of 0.02
 H71B-H7A
 2.05 with sigma of 0.02
 H7A-F22
 2.05 with sigma of 0.02
 H71B-H7B
 2.05 with sigma of 0.02
 P4-F19 \\sim P4A-F19A
 with sigma of 0.02
 F23-F22 \\sim F23A-F22A
 with sigma of 0.04
 P4-F21 \\sim P4A-F21A
 with sigma of 0.02
 P4-F20 \\sim P4A-F20A
 with sigma of 0.02
 P4-F24 \\sim P4A-F24A
 with sigma of 0.02
 P4-F23 \\sim P4A-F23A
 with sigma of 0.02
 P4-F22 \\sim P4A-F22A
 with sigma of 0.02
 F21-F20 \\sim F21A-F20A
 with sigma of 0.04
 F21-F23 \\sim F21A-F23A
 with sigma of 0.04
 F20-F23 \\sim F20A-F23A
 with sigma of 0.04
 F24-F22 \\sim F24A-F22A
 with sigma of 0.04
 F21-F24 \\sim F21A-F24A
 with sigma of 0.04
 F21-F22 \\sim F21A-F22A
 with sigma of 0.04
 F20-F24 \\sim F20A-F24A
 with sigma of 0.04
 F20-F22 \\sim F20A-F22A
 with sigma of 0.04
 F24-F23 \\sim F24A-F23A
 with sigma of 0.04
 F19-F21 \\sim F19A-F21A
 with sigma of 0.04
 F19-F20 \\sim F19A-F20A
 with sigma of 0.04
 F19-F24 \\sim F19A-F24A
 with sigma of 0.04
 F19-F23 \\sim F19A-F23A
 with sigma of 0.04
 F19-F22 \\sim F19A-F22A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F19) = Uanis(F19A)
Uanis(F20) = Uanis(F20A)
Uanis(F21) = Uanis(F21A)
Uanis(F22) = Uanis(F22A)
Uanis(F23) = Uanis(F23A)
Uanis(F24) = Uanis(F24A)
Uanis(P4) = Uanis(P4A)
4. Others
 Sof(P4A)=Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(P4)=Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
5.a Free rotating group:
 O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C60(H60A,H60B), C61(H61A,H61B),
 C62(H62A,H62B), C63(H63A,H63B), C70(H70A,H70B), C11(H11A,H11B), C18(H18A,H18B),
  C29(H29A,H29B), C36(H36A,H36B)
5.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C43(H43), C44(H44), C52(H52), C53(H53), C54(H54), C57(H57),
 C58(H58), C59(H59), C65(H65), C66(H66), C69(H69), C1(H1), C2(H2), C4(H4),
 C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C34(H34), C35(H35)
5.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.72102(8) 0.53804(5) 0.27679(4) 0.0431(3) Uani 1 1 d . . . . .
F1 F 0.6760(3) 0.56440(16) 0.33164(12) 0.0839(10) Uani 1 1 d . . . . .
F2 F 0.62316(15) 0.55459(12) 0.23886(10) 0.0492(6) Uani 1 1 d . . . . .
F3 F 0.76438(16) 0.51208(11) 0.22059(11) 0.0487(6) Uani 1 1 d . . . . .
F4 F 0.8201(2) 0.52275(13) 0.31297(14) 0.0773(10) Uani 1 1 d . . . . .
F5 F 0.76138(17) 0.60241(11) 0.26330(10) 0.0473(6) Uani 1 1 d . . . . .
F6 F 0.6786(3) 0.47354(14) 0.28913(14) 0.0775(9) Uani 1 1 d D . . . .
P2 P 0.24715(6) 0.11679(4) 0.42439(3) 0.02717(19) Uani 1 1 d . . . . .
F7 F 0.18375(17) 0.11303(14) 0.36571(9) 0.0569(7) Uani 1 1 d . . . . .
F8 F 0.34112(15) 0.10124(10) 0.39210(9) 0.0402(5) Uani 1 1 d . . . . .
F9 F 0.31175(16) 0.12037(11) 0.48370(9) 0.0448(5) Uani 1 1 d . . . . .
F10 F 0.15454(16) 0.13254(12) 0.45736(9) 0.0474(6) Uani 1 1 d . . . . .
F11 F 0.26458(16) 0.18669(9) 0.41440(10) 0.0427(5) Uani 1 1 d . . . . .
F12 F 0.2322(2) 0.04684(11) 0.43502(11) 0.0569(7) Uani 1 1 d . . . . .
P3 P 0.11012(6) 0.85817(4) 0.39988(4) 0.0336(2) Uani 1 1 d . . . . .
F13 F 0.14347(13) 0.87896(9) 0.33820(9) 0.0342(4) Uani 1 1 d . . . . .
F14 F 0.21790(16) 0.86845(12) 0.42698(9) 0.0495(6) Uani 1 1 d . . . . .
F15 F 0.07852(18) 0.83552(13) 0.46036(9) 0.0565(7) Uani 1 1 d . . . . .
F16 F 0.00410(14) 0.84738(9) 0.37131(10) 0.0391(5) Uani 1 1 d . . . . .
F17 F 0.0844(2) 0.92511(11) 0.41426(14) 0.0695(9) Uani 1 1 d . . . . .
F18 F 0.13785(13) 0.79052(9) 0.38501(8) 0.0325(4) Uani 1 1 d . . . . .
O1 O 0.13708(17) 0.55467(10) 0.41045(10) 0.0310(5) Uani 1 1 d . . . . .
O2 O 0.26481(17) 0.62076(10) 0.33490(9) 0.0299(5) Uani 1 1 d . . . . .
O3 O 0.32680(16) 0.55574(9) 0.23173(9) 0.0267(5) Uani 1 1 d . . . . .
O4 O 0.30805(15) 0.30940(9) 0.13048(9) 0.0249(4) Uani 1 1 d . . . . .
O5 O 0.17887(16) 0.20667(10) 0.14065(9) 0.0278(5) Uani 1 1 d . . . . .
O6 O 0.05604(15) 0.20832(10) 0.24012(9) 0.0251(5) Uani 1 1 d . . . . .
N5 N 0.0300(2) 0.32322(12) 0.47578(11) 0.0277(6) Uani 1 1 d . . . . .
N6 N -0.13471(19) 0.34128(12) 0.40075(12) 0.0283(6) Uani 1 1 d . . . . .
C37 C -0.1451(2) 0.30816(16) 0.45447(14) 0.0313(7) Uani 1 1 d . . . . .
H37A H -0.148586 0.264652 0.445952 0.038 Uiso 1 1 calc R U . . .
H37B H -0.206077 0.320045 0.470201 0.038 Uiso 1 1 calc R U . . .
C38 C -0.0630(3) 0.31942(16) 0.49958(14) 0.0318(7) Uani 1 1 d . . . . .
H38A H -0.075265 0.357357 0.519834 0.038 Uiso 1 1 calc R U . . .
H38B H -0.061411 0.286539 0.528108 0.038 Uiso 1 1 calc R U . . .
C39 C -0.1115(2) 0.40498(15) 0.40845(15) 0.0318(7) Uani 1 1 d . . . . .
H39A H -0.152849 0.421392 0.437273 0.038 Uiso 1 1 calc R U . . .
H39B H -0.129363 0.425734 0.371791 0.038 Uiso 1 1 calc R U . . .
C40 C -0.0088(2) 0.42137(14) 0.42682(13) 0.0272(6) Uani 1 1 d . . . . .
C41 C 0.0216(2) 0.47889(15) 0.41298(14) 0.0291(7) Uani 1 1 d . . . . .
H41 H -0.021557 0.505442 0.392476 0.035 Uiso 1 1 calc R U . . .
C42 C 0.1144(2) 0.49770(14) 0.42888(14) 0.0286(7) Uani 1 1 d . . . . .
C43 C 0.1783(3) 0.45947(16) 0.45926(15) 0.0327(7) Uani 1 1 d . . . . .
H43 H 0.241695 0.472297 0.470400 0.039 Uiso 1 1 calc R U . . .
C44 C 0.1477(2) 0.40194(15) 0.47313(14) 0.0304(7) Uani 1 1 d . . . . .
H44 H 0.191135 0.375707 0.493864 0.036 Uiso 1 1 calc R U . . .
C45 C 0.0550(2) 0.38210(15) 0.45727(13) 0.0281(7) Uani 1 1 d . . . . .
C46 C 0.2302(2) 0.57771(15) 0.42808(14) 0.0305(7) Uani 1 1 d . . . . .
H46A H 0.279833 0.547284 0.421584 0.037 Uiso 1 1 calc R U . . .
H46B H 0.233948 0.587696 0.469409 0.037 Uiso 1 1 calc R U . . .
C47 C 0.2464(3) 0.63355(15) 0.39309(14) 0.0317(7) Uani 1 1 d . . . . .
H47A H 0.189156 0.659621 0.393349 0.038 Uiso 1 1 calc R U . . .
H47B H 0.301527 0.656049 0.411425 0.038 Uiso 1 1 calc R U . . .
C48 C 0.3569(2) 0.59368(15) 0.33007(14) 0.0294(7) Uani 1 1 d . . . . .
H48A H 0.355609 0.551338 0.342861 0.035 Uiso 1 1 calc R U . . .
H48B H 0.406163 0.615265 0.354722 0.035 Uiso 1 1 calc R U . . .
C49 C 0.3813(2) 0.59654(14) 0.26842(14) 0.0298(7) Uani 1 1 d . . . . .
H49A H 0.370097 0.637931 0.254029 0.036 Uiso 1 1 calc R U . . .
H49B H 0.450331 0.587545 0.266565 0.036 Uiso 1 1 calc R U . . .
C50 C 0.3572(2) 0.49715(13) 0.22839(13) 0.0221(6) Uani 1 1 d . . . . .
C51 C 0.3038(2) 0.46282(13) 0.18562(12) 0.0200(6) Uani 1 1 d . . . . .
C52 C 0.2276(2) 0.48811(13) 0.15027(13) 0.0216(6) Uani 1 1 d . . . . .
H52 H 0.209339 0.528676 0.155679 0.026 Uiso 1 1 calc R U . . .
C53 C 0.1805(2) 0.45441(13) 0.10853(13) 0.0235(6) Uani 1 1 d . . . . .
H53 H 0.129993 0.472043 0.084827 0.028 Uiso 1 1 calc R U . . .
C54 C 0.2052(2) 0.39376(13) 0.09982(13) 0.0237(6) Uani 1 1 d . . . . .
H54 H 0.171826 0.371027 0.070350 0.028 Uiso 1 1 calc R U . . .
C55 C 0.2777(2) 0.36780(13) 0.13414(13) 0.0212(6) Uani 1 1 d . . . . .
C56 C 0.3293(2) 0.40169(13) 0.17857(12) 0.0193(6) Uani 1 1 d . . . . .
C57 C 0.4057(2) 0.37631(13) 0.21395(13) 0.0229(6) Uani 1 1 d . . . . .
H57 H 0.422511 0.335320 0.209625 0.027 Uiso 1 1 calc R U . . .
C58 C 0.4549(2) 0.41092(14) 0.25409(14) 0.0271(6) Uani 1 1 d . . . . .
H58 H 0.506114 0.393647 0.277458 0.032 Uiso 1 1 calc R U . . .
C59 C 0.4313(2) 0.47222(15) 0.26180(14) 0.0282(7) Uani 1 1 d . . . . .
H59 H 0.466671 0.495742 0.289882 0.034 Uiso 1 1 calc R U . . .
C60 C 0.2674(2) 0.27260(15) 0.08407(13) 0.0283(7) Uani 1 1 d . . . . .
H60A H 0.311711 0.238872 0.078143 0.034 Uiso 1 1 calc R U . . .
H60B H 0.262488 0.296889 0.048544 0.034 Uiso 1 1 calc R U . . .
C61 C 0.1704(2) 0.24751(14) 0.09358(13) 0.0266(6) Uani 1 1 d . . . . .
H61A H 0.126016 0.280488 0.101871 0.032 Uiso 1 1 calc R U . . .
H61B H 0.144078 0.226416 0.058644 0.032 Uiso 1 1 calc R U . . .
C62 C 0.0926(2) 0.17378(15) 0.14748(14) 0.0285(7) Uani 1 1 d . . . . .
H62A H 0.109075 0.135614 0.167532 0.034 Uiso 1 1 calc R U . . .
H62B H 0.062226 0.163712 0.109122 0.034 Uiso 1 1 calc R U . . .
C63 C 0.0212(2) 0.20765(15) 0.18073(13) 0.0293(7) Uani 1 1 d . . . . .
H63A H 0.014074 0.249236 0.166098 0.035 Uiso 1 1 calc R U . . .
H63B H -0.042166 0.187750 0.176285 0.035 Uiso 1 1 calc R U . . .
C64 C 0.0084(2) 0.24392(13) 0.27709(14) 0.0253(6) Uani 1 1 d . . . . .
C65 C -0.0712(2) 0.27860(15) 0.26093(14) 0.0270(6) Uani 1 1 d . . . . .
H65 H -0.095765 0.280269 0.222023 0.032 Uiso 1 1 calc R U . . .
C66 C -0.1143(2) 0.31097(15) 0.30291(14) 0.0287(7) Uani 1 1 d . . . . .
H66 H -0.169099 0.334715 0.292063 0.034 Uiso 1 1 calc R U . . .
C67 C -0.0799(2) 0.30973(14) 0.36034(14) 0.0261(6) Uani 1 1 d . . . . .
C68 C 0.0028(2) 0.27663(14) 0.37578(13) 0.0248(6) Uani 1 1 d . . . . .
C69 C 0.0455(2) 0.24360(13) 0.33373(13) 0.0239(6) Uani 1 1 d . . . . .
H69 H 0.101129 0.220435 0.344139 0.029 Uiso 1 1 calc R U . . .
C70 C 0.0497(2) 0.27360(15) 0.43707(13) 0.0275(6) Uani 1 1 d . . . . .
H70A H 0.029054 0.235811 0.454712 0.033 Uiso 1 1 calc R U . . .
H70B H 0.120022 0.271069 0.434747 0.033 Uiso 1 1 calc R U . . .
O7 O 0.6762(9) 0.3597(7) 0.3523(5) 0.377(11) Uani 1 1 d G . . . .
H7A H 0.620052 0.349720 0.362859 0.566 Uiso 1 1 d DG U . . .
H7B H 0.667352 0.394476 0.335904 0.566 Uiso 1 1 d DG U . . .
N1 N 0.30658(18) 0.25899(12) 0.30478(11) 0.0247(5) Uani 1 1 d . . . . .
N2 N 0.03795(19) 0.51834(12) 0.24680(12) 0.0270(6) Uani 1 1 d . . . . .
N3 N 0.33146(19) 0.60801(12) 0.06628(11) 0.0273(6) Uani 1 1 d . . . . .
N4 N 0.60648(18) 0.35241(12) 0.13343(12) 0.0261(5) Uani 1 1 d . . . . .
C1 C 0.3076(2) 0.30095(15) 0.34639(13) 0.0291(7) Uani 1 1 d . . . . .
H1 H 0.347633 0.295653 0.380597 0.035 Uiso 1 1 calc R U . . .
C2 C 0.2513(2) 0.35113(15) 0.33972(14) 0.0282(7) Uani 1 1 d . . . . .
H2 H 0.252531 0.380507 0.369196 0.034 Uiso 1 1 calc R U . . .
C3 C 0.1921(2) 0.35915(14) 0.28971(13) 0.0230(6) Uani 1 1 d . . . . .
C4 C 0.1910(2) 0.31393(14) 0.24852(13) 0.0233(6) Uani 1 1 d . . . . .
H4 H 0.150007 0.317485 0.214484 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2485(2) 0.26440(14) 0.25656(13) 0.0237(6) Uani 1 1 d . . . . .
H5 H 0.247394 0.233902 0.228141 0.028 Uiso 1 1 calc R U . . .
C6 C 0.1347(2) 0.41412(14) 0.27839(13) 0.0242(6) Uani 1 1 d . . . . .
C7 C 0.1676(2) 0.46974(14) 0.29884(13) 0.0270(6) Uani 1 1 d . . . . .
H7 H 0.223694 0.472165 0.324237 0.032 Uiso 1 1 calc R U . . .
C8 C 0.1185(2) 0.52122(15) 0.28208(13) 0.0289(7) Uani 1 1 d . . . . .
H8 H 0.141715 0.559139 0.295529 0.035 Uiso 1 1 calc R U . . .
C9 C 0.0022(2) 0.46519(15) 0.22893(16) 0.0316(7) Uani 1 1 d . . . . .
H9 H -0.056266 0.463834 0.205574 0.038 Uiso 1 1 calc R U . . .
C10 C 0.0489(2) 0.41269(15) 0.24391(16) 0.0315(7) Uani 1 1 d . . . . .
H10 H 0.022809 0.375347 0.230816 0.038 Uiso 1 1 calc R U . . .
C11 C -0.0069(2) 0.57549(15) 0.22404(15) 0.0310(7) Uani 1 1 d . . . . .
H11A H -0.013564 0.604136 0.255852 0.037 Uiso 1 1 calc R U . . .
H11B H -0.071581 0.567155 0.205665 0.037 Uiso 1 1 calc R U . . .
C12 C 0.0556(2) 0.60220(14) 0.18095(15) 0.0276(7) Uani 1 1 d . . . . .
C13 C 0.0392(2) 0.58833(15) 0.12309(14) 0.0292(7) Uani 1 1 d . . . . .
H13 H -0.015316 0.565261 0.110240 0.035 Uiso 1 1 calc R U . . .
C14 C 0.1022(2) 0.60804(15) 0.08424(14) 0.0297(7) Uani 1 1 d . . . . .
H14 H 0.091010 0.598040 0.044848 0.036 Uiso 1 1 calc R U . . .
C15 C 0.1820(2) 0.64247(14) 0.10244(14) 0.0273(6) Uani 1 1 d . . . . .
C16 C 0.1945(2) 0.65957(14) 0.15959(14) 0.0266(6) Uani 1 1 d . . . . .
H16 H 0.245969 0.685399 0.171999 0.032 Uiso 1 1 calc R U . . .
C17 C 0.1320(2) 0.63898(14) 0.19861(14) 0.0273(7) Uani 1 1 d . . . . .
H17 H 0.141627 0.650213 0.237773 0.033 Uiso 1 1 calc R U . . .
C18 C 0.2581(2) 0.65725(15) 0.06217(15) 0.0311(7) Uani 1 1 d . . . . .
H18A H 0.229031 0.660402 0.022402 0.037 Uiso 1 1 calc R U . . .
H18B H 0.288575 0.696148 0.072910 0.037 Uiso 1 1 calc R U . . .
C19 C 0.3227(2) 0.56027(15) 0.03086(13) 0.0286(7) Uani 1 1 d . . . . .
H19 H 0.274620 0.560279 -0.000029 0.034 Uiso 1 1 calc R U . . .
C20 C 0.3827(2) 0.51145(15) 0.03903(13) 0.0263(6) Uani 1 1 d . . . . .
H20 H 0.376143 0.478270 0.013528 0.032 Uiso 1 1 calc R U . . .
C21 C 0.4533(2) 0.51049(13) 0.08477(13) 0.0228(6) Uani 1 1 d . . . . .
C22 C 0.4621(2) 0.56181(14) 0.11958(14) 0.0253(6) Uani 1 1 d . . . . .
H22 H 0.510393 0.563553 0.150268 0.030 Uiso 1 1 calc R U . . .
C23 C 0.4012(2) 0.60936(14) 0.10942(15) 0.0280(7) Uani 1 1 d . . . . .
H23 H 0.408093 0.643945 0.133122 0.034 Uiso 1 1 calc R U . . .
C24 C 0.5114(2) 0.45612(13) 0.09866(13) 0.0218(6) Uani 1 1 d . . . . .
C25 C 0.4833(2) 0.40039(14) 0.07599(13) 0.0255(6) Uani 1 1 d . . . . .
H25 H 0.430529 0.397635 0.048157 0.031 Uiso 1 1 calc R U . . .
C26 C 0.5321(2) 0.34960(14) 0.09395(14) 0.0279(7) Uani 1 1 d . . . . .
H26 H 0.512909 0.311807 0.078169 0.034 Uiso 1 1 calc R U . . .
C27 C 0.6375(2) 0.40587(15) 0.15450(15) 0.0294(7) Uani 1 1 d . . . . .
H27 H 0.691690 0.407450 0.181399 0.035 Uiso 1 1 calc R U . . .
C28 C 0.5915(2) 0.45805(15) 0.13751(14) 0.0272(6) Uani 1 1 d . . . . .
H28 H 0.614396 0.495508 0.152319 0.033 Uiso 1 1 calc R U . . .
C29 C 0.6517(2) 0.29457(15) 0.15537(16) 0.0316(7) Uani 1 1 d . . . . .
H29A H 0.660993 0.267322 0.122816 0.038 Uiso 1 1 calc R U . . .
H29B H 0.715243 0.302980 0.175208 0.038 Uiso 1 1 calc R U . . .
C30 C 0.5881(2) 0.26499(14) 0.19621(15) 0.0276(7) Uani 1 1 d . . . . .
C31 C 0.5131(2) 0.22756(14) 0.17622(15) 0.0278(6) Uani 1 1 d . . . . .
H31 H 0.506836 0.216473 0.136921 0.033 Uiso 1 1 calc R U . . .
C32 C 0.4476(2) 0.20631(14) 0.21292(15) 0.0277(7) Uani 1 1 d . . . . .
H32 H 0.396947 0.180691 0.198741 0.033 Uiso 1 1 calc R U . . .
C33 C 0.4557(2) 0.22241(14) 0.27054(15) 0.0286(7) Uani 1 1 d . . . . .
C34 C 0.5332(2) 0.25695(15) 0.29138(15) 0.0305(7) Uani 1 1 d . . . . .
H34 H 0.541391 0.266227 0.331071 0.037 Uiso 1 1 calc R U . . .
C35 C 0.5989(2) 0.27804(15) 0.25424(15) 0.0317(7) Uani 1 1 d . . . . .
H35 H 0.651788 0.301638 0.268838 0.038 Uiso 1 1 calc R U . . .
C36 C 0.3768(2) 0.20787(15) 0.30886(15) 0.0301(7) Uani 1 1 d . . . . .
H36A H 0.344487 0.170037 0.296361 0.036 Uiso 1 1 calc R U . . .
H36B H 0.403515 0.202895 0.348942 0.036 Uiso 1 1 calc R U . . .
N7 N 0.4069(4) 0.4639(2) 0.4112(2) 0.0807(15) Uani 1 1 d . . . . .
C71 C 0.5929(5) 0.4628(4) 0.4285(3) 0.111(3) Uani 1 1 d . . . . .
H71A H 0.619371 0.498670 0.411217 0.166 Uiso 1 1 calc R U . . .
H71B H 0.617786 0.426832 0.410586 0.166 Uiso 1 1 calc DR U . . .
H71C H 0.611546 0.462302 0.469672 0.166 Uiso 1 1 calc R U . . .
C72 C 0.4893(5) 0.4637(3) 0.4195(2) 0.0723(15) Uani 1 1 d . . . . .
P4 P 0.54886(13) 0.28141(8) 0.47915(7) 0.0401(4) Uani 0.805(4) 1 d D . P A 1
F19 F 0.6302(4) 0.2467(3) 0.5169(3) 0.0638(10) Uani 0.805(4) 1 d D . P A 1
F20 F 0.4767(3) 0.2736(2) 0.52688(17) 0.0766(15) Uani 0.805(4) 1 d D . P A 1
F21 F 0.4695(3) 0.31866(18) 0.44167(14) 0.0571(9) Uani 0.805(4) 1 d D . P A 1
F22 F 0.6207(3) 0.2897(2) 0.42953(15) 0.0863(14) Uani 0.805(4) 1 d D . P A 1
F23 F 0.5865(4) 0.34440(19) 0.5060(2) 0.0931(17) Uani 0.805(4) 1 d D . P A 1
F24 F 0.5134(3) 0.2225(2) 0.4487(2) 0.0826(13) Uani 0.805(4) 1 d D . P A 1
P4A P 0.5227(5) 0.2912(4) 0.4876(3) 0.0401(4) Uani 0.195(4) 1 d D . P A 2
F19A F 0.6124(18) 0.2521(14) 0.5158(13) 0.0638(10) Uani 0.195(4) 1 d D . P A 2
F20A F 0.5112(12) 0.3128(8) 0.5498(5) 0.0766(15) Uani 0.195(4) 1 d D . P A 2
F21A F 0.4337(10) 0.3265(7) 0.4604(6) 0.0571(9) Uani 0.195(4) 1 d D . P A 2
F22A F 0.5380(11) 0.2569(9) 0.4283(5) 0.0863(14) Uani 0.195(4) 1 d D . P A 2
F23A F 0.5956(13) 0.3399(8) 0.4733(8) 0.0931(17) Uani 0.195(4) 1 d D . P A 2
F24A F 0.4536(11) 0.2341(7) 0.5001(8) 0.0826(13) Uani 0.195(4) 1 d D . 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
P1 F1 1.584(3) . ?
P1 F2 1.618(2) . ?
P1 F3 1.597(3) . ?
P1 F4 1.606(3) . ?
P1 F5 1.581(3) . ?
P1 F6 1.589(3) . ?
P2 F7 1.581(2) . ?
P2 F8 1.601(2) . ?
P2 F9 1.601(2) . ?
P2 F10 1.595(2) . ?
P2 F11 1.596(2) . ?
P2 F12 1.594(3) . ?
P3 F13 1.617(2) . ?
P3 F14 1.608(2) . ?
P3 F15 1.595(2) . ?
P3 F16 1.599(2) . ?
P3 F17 1.576(3) . ?
P3 F18 1.601(2) . ?
O1 C42 1.385(4) . ?
O1 C46 1.432(4) . ?
O2 C47 1.433(4) . ?
O2 C48 1.434(4) . ?
O3 C49 1.431(4) . ?
O3 C50 1.377(3) . ?
O4 C55 1.373(3) . ?
O4 C60 1.443(4) . ?
O5 C61 1.427(4) . ?
O5 C62 1.430(4) . ?
O6 C63 1.438(4) . ?
O6 C64 1.381(4) . ?
N5 C38 1.456(4) . ?
N5 C45 1.432(4) . ?
N5 C70 1.468(4) . ?
N6 C37 1.474(4) . ?
N6 C39 1.463(4) . ?
N6 C67 1.443(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.522(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.514(4) . ?
C40 C41 1.396(5) . ?
C40 C45 1.406(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.388(5) . ?
C42 C43 1.391(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.397(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.394(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.516(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.508(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.427(4) . ?
C50 C59 1.369(4) . ?
C51 C52 1.416(4) . ?
C51 C56 1.420(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.363(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.413(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.374(4) . ?
C55 C56 1.436(4) . ?
C56 C57 1.420(4) . ?
C57 H57 0.9500 . ?
C57 C58 1.362(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.419(4) . ?
C59 H59 0.9500 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.499(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.512(5) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.384(4) . ?
C64 C69 1.388(4) . ?
C65 H65 0.9500 . ?
C65 C66 1.392(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.394(4) . ?
C67 C68 1.397(4) . ?
C68 C69 1.397(5) . ?
C68 C70 1.534(4) . ?
C69 H69 0.9500 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
O7 H7A 0.8699 . ?
O7 H7B 0.8693 . ?
N1 C1 1.349(4) . ?
N1 C5 1.346(4) . ?
N1 C36 1.502(4) . ?
N2 C8 1.349(4) . ?
N2 C9 1.340(4) . ?
N2 C11 1.499(4) . ?
N3 C18 1.501(4) . ?
N3 C19 1.348(4) . ?
N3 C23 1.351(4) . ?
N4 C26 1.341(4) . ?
N4 C27 1.348(4) . ?
N4 C29 1.508(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.370(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(4) . ?
C3 C4 1.393(4) . ?
C3 C6 1.477(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.370(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(4) . ?
C6 C10 1.397(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.379(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.372(5) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.505(5) . ?
C12 C13 1.391(5) . ?
C12 C17 1.385(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.395(5) . ?
C15 C16 1.389(5) . ?
C15 C18 1.509(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(5) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C19 C20 1.378(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.402(4) . ?
C21 C22 1.404(4) . ?
C21 C24 1.481(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.369(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(4) . ?
C24 C28 1.390(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.371(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.373(5) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.505(5) . ?
C30 C31 1.393(5) . ?
C30 C35 1.386(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.385(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.392(5) . ?
C33 C34 1.388(5) . ?
C33 C36 1.508(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(5) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N7 C72 1.155(8) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C71 C72 1.449(9) . ?
P4 F19 1.589(4) . ?
P4 F20 1.569(4) . ?
P4 F21 1.596(3) . ?
P4 F22 1.601(4) . ?
P4 F23 1.610(4) . ?
P4 F24 1.556(4) . ?
P4A F19A 1.624(14) . ?
P4A F20A 1.552(13) . ?
P4A F21A 1.568(12) . ?
P4A F22A 1.613(13) . ?
P4A F23A 1.543(14) . ?
P4A F24A 1.635(13) . ?

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
F1 P1 F2 89.38(17) . . ?
F1 P1 F3 178.67(18) . . ?
F1 P1 F4 91.8(2) . . ?
F1 P1 F6 90.68(19) . . ?
F3 P1 F2 89.31(13) . . ?
F3 P1 F4 89.55(17) . . ?
F4 P1 F2 178.15(17) . . ?
F5 P1 F1 89.70(16) . . ?
F5 P1 F2 89.07(13) . . ?
F5 P1 F3 90.06(14) . . ?
F5 P1 F4 89.47(14) . . ?
F5 P1 F6 178.64(17) . . ?
F6 P1 F2 89.63(17) . . ?
F6 P1 F3 89.54(17) . . ?
F6 P1 F4 91.82(17) . . ?
F7 P2 F8 90.35(13) . . ?
F7 P2 F9 179.71(16) . . ?
F7 P2 F10 90.47(13) . . ?
F7 P2 F11 90.36(15) . . ?
F7 P2 F12 90.69(15) . . ?
F9 P2 F8 89.39(12) . . ?
F10 P2 F8 179.16(14) . . ?
F10 P2 F9 89.79(12) . . ?
F10 P2 F11 89.68(13) . . ?
F11 P2 F8 90.13(12) . . ?
F11 P2 F9 89.76(13) . . ?
F12 P2 F8 89.09(13) . . ?
F12 P2 F9 89.18(14) . . ?
F12 P2 F10 91.08(14) . . ?
F12 P2 F11 178.69(15) . . ?
F14 P3 F13 89.28(11) . . ?
F15 P3 F13 178.14(15) . . ?
F15 P3 F14 90.47(13) . . ?
F15 P3 F16 90.83(13) . . ?
F15 P3 F18 89.01(14) . . ?
F16 P3 F13 89.39(11) . . ?
F16 P3 F14 178.41(13) . . ?
F16 P3 F18 89.98(11) . . ?
F17 P3 F13 90.28(14) . . ?
F17 P3 F14 90.18(15) . . ?
F17 P3 F15 91.56(16) . . ?
F17 P3 F16 90.70(14) . . ?
F17 P3 F18 179.11(14) . . ?
F18 P3 F13 89.14(11) . . ?
F18 P3 F14 89.12(13) . . ?
C42 O1 C46 117.6(3) . . ?
C47 O2 C48 112.5(3) . . ?
C50 O3 C49 118.9(2) . . ?
C55 O4 C60 118.6(2) . . ?
C61 O5 C62 112.9(2) . . ?
C64 O6 C63 117.8(2) . . ?
C38 N5 C70 114.0(3) . . ?
C45 N5 C38 114.4(3) . . ?
C45 N5 C70 116.2(3) . . ?
C39 N6 C37 114.5(3) . . ?
C67 N6 C37 113.9(3) . . ?
C67 N6 C39 115.4(3) . . ?
N6 C37 H37A 109.0 . . ?
N6 C37 H37B 109.0 . . ?
N6 C37 C38 113.1(3) . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 H37A 109.0 . . ?
C38 C37 H37B 109.0 . . ?
N5 C38 C37 113.2(3) . . ?
N5 C38 H38A 108.9 . . ?
N5 C38 H38B 108.9 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
N6 C39 H39A 107.9 . . ?
N6 C39 H39B 107.9 . . ?
N6 C39 C40 117.8(3) . . ?
H39A C39 H39B 107.2 . . ?
C40 C39 H39A 107.9 . . ?
C40 C39 H39B 107.9 . . ?
C41 C40 C39 117.1(3) . . ?
C41 C40 C45 119.7(3) . . ?
C45 C40 C39 123.2(3) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.7(3) . . ?
C42 C41 H41 119.7 . . ?
O1 C42 C41 115.1(3) . . ?
O1 C42 C43 124.6(3) . . ?
C41 C42 C43 120.3(3) . . ?
C42 C43 H43 120.5 . . ?
C42 C43 C44 119.0(3) . . ?
C44 C43 H43 120.5 . . ?
C43 C44 H44 119.2 . . ?
C45 C44 C43 121.6(3) . . ?
C45 C44 H44 119.2 . . ?
C40 C45 N5 124.3(3) . . ?
C44 C45 N5 116.9(3) . . ?
C44 C45 C40 118.8(3) . . ?
O1 C46 H46A 110.1 . . ?
O1 C46 H46B 110.1 . . ?
O1 C46 C47 107.9(3) . . ?
H46A C46 H46B 108.4 . . ?
C47 C46 H46A 110.1 . . ?
C47 C46 H46B 110.1 . . ?
O2 C47 C46 113.3(3) . . ?
O2 C47 H47A 108.9 . . ?
O2 C47 H47B 108.9 . . ?
C46 C47 H47A 108.9 . . ?
C46 C47 H47B 108.9 . . ?
H47A C47 H47B 107.7 . . ?
O2 C48 H48A 109.9 . . ?
O2 C48 H48B 109.9 . . ?
O2 C48 C49 109.0(3) . . ?
H48A C48 H48B 108.3 . . ?
C49 C48 H48A 109.9 . . ?
C49 C48 H48B 109.9 . . ?
O3 C49 C48 113.5(3) . . ?
O3 C49 H49A 108.9 . . ?
O3 C49 H49B 108.9 . . ?
C48 C49 H49A 108.9 . . ?
C48 C49 H49B 108.9 . . ?
H49A C49 H49B 107.7 . . ?
O3 C50 C51 113.6(3) . . ?
C59 C50 O3 125.2(3) . . ?
C59 C50 C51 121.3(3) . . ?
C52 C51 C50 122.0(3) . . ?
C52 C51 C56 119.9(3) . . ?
C56 C51 C50 118.1(3) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 C51 120.2(3) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 119.4 . . ?
C52 C53 C54 121.3(3) . . ?
C54 C53 H53 119.4 . . ?
C53 C54 H54 120.1 . . ?
C55 C54 C53 119.7(3) . . ?
C55 C54 H54 120.1 . . ?
O4 C55 C54 125.5(3) . . ?
O4 C55 C56 113.7(2) . . ?
C54 C55 C56 120.8(3) . . ?
C51 C56 C55 118.1(3) . . ?
C51 C56 C57 119.9(3) . . ?
C57 C56 C55 122.0(3) . . ?
C56 C57 H57 120.1 . . ?
C58 C57 C56 119.8(3) . . ?
C58 C57 H57 120.1 . . ?
C57 C58 H58 119.3 . . ?
C57 C58 C59 121.5(3) . . ?
C59 C58 H58 119.3 . . ?
C50 C59 C58 119.4(3) . . ?
C50 C59 H59 120.3 . . ?
C58 C59 H59 120.3 . . ?
O4 C60 H60A 108.7 . . ?
O4 C60 H60B 108.7 . . ?
O4 C60 C61 114.2(3) . . ?
H60A C60 H60B 107.6 . . ?
C61 C60 H60A 108.7 . . ?
C61 C60 H60B 108.7 . . ?
O5 C61 C60 109.1(3) . . ?
O5 C61 H61A 109.9 . . ?
O5 C61 H61B 109.9 . . ?
C60 C61 H61A 109.9 . . ?
C60 C61 H61B 109.9 . . ?
H61A C61 H61B 108.3 . . ?
O5 C62 H62A 108.9 . . ?
O5 C62 H62B 108.9 . . ?
O5 C62 C63 113.3(3) . . ?
H62A C62 H62B 107.7 . . ?
C63 C62 H62A 108.9 . . ?
C63 C62 H62B 108.9 . . ?
O6 C63 C62 108.2(3) . . ?
O6 C63 H63A 110.0 . . ?
O6 C63 H63B 110.0 . . ?
C62 C63 H63A 110.0 . . ?
C62 C63 H63B 110.0 . . ?
H63A C63 H63B 108.4 . . ?
O6 C64 C65 124.4(3) . . ?
O6 C64 C69 115.5(3) . . ?
C65 C64 C69 120.1(3) . . ?
C64 C65 H65 120.7 . . ?
C64 C65 C66 118.6(3) . . ?
C66 C65 H65 120.7 . . ?
C65 C66 H66 118.9 . . ?
C65 C66 C67 122.2(3) . . ?
C67 C66 H66 118.9 . . ?
C66 C67 N6 117.4(3) . . ?
C66 C67 C68 118.7(3) . . ?
C68 C67 N6 123.9(3) . . ?
C67 C68 C69 119.0(3) . . ?
C67 C68 C70 123.6(3) . . ?
C69 C68 C70 117.4(3) . . ?
C64 C69 C68 121.4(3) . . ?
C64 C69 H69 119.3 . . ?
C68 C69 H69 119.3 . . ?
N5 C70 C68 117.2(3) . . ?
N5 C70 H70A 108.0 . . ?
N5 C70 H70B 108.0 . . ?
C68 C70 H70A 108.0 . . ?
C68 C70 H70B 108.0 . . ?
H70A C70 H70B 107.2 . . ?
H7A O7 H7B 104.5 . . ?
C1 N1 C36 120.5(3) . . ?
C5 N1 C1 121.1(3) . . ?
C5 N1 C36 118.2(3) . . ?
C8 N2 C11 119.1(3) . . ?
C9 N2 C8 120.6(3) . . ?
C9 N2 C11 120.2(3) . . ?
C19 N3 C18 120.4(3) . . ?
C19 N3 C23 120.3(3) . . ?
C23 N3 C18 119.0(3) . . ?
C26 N4 C27 120.4(3) . . ?
C26 N4 C29 118.6(3) . . ?
C27 N4 C29 121.0(3) . . ?
N1 C1 H1 119.7 . . ?
N1 C1 C2 120.5(3) . . ?
C2 C1 H1 119.7 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C6 122.5(3) . . ?
C4 C3 C2 117.6(3) . . ?
C4 C3 C6 119.8(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 119.9(3) . . ?
N1 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C3 120.9(3) . . ?
C7 C6 C10 117.8(3) . . ?
C10 C6 C3 121.1(3) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
N2 C8 C7 120.7(3) . . ?
N2 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
N2 C9 H9 119.5 . . ?
N2 C9 C10 120.9(3) . . ?
C10 C9 H9 119.5 . . ?
C6 C10 H10 120.0 . . ?
C9 C10 C6 120.1(3) . . ?
C9 C10 H10 120.0 . . ?
N2 C11 H11A 109.9 . . ?
N2 C11 H11B 109.9 . . ?
N2 C11 C12 109.0(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C13 C12 C11 120.2(3) . . ?
C17 C12 C11 120.5(3) . . ?
C17 C12 C13 119.3(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.5(3) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C18 121.0(3) . . ?
C16 C15 C14 119.1(3) . . ?
C16 C15 C18 119.8(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 119.9 . . ?
C12 C17 C16 120.6(3) . . ?
C12 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
N3 C18 C15 108.1(2) . . ?
N3 C18 H18A 110.1 . . ?
N3 C18 H18B 110.1 . . ?
C15 C18 H18A 110.1 . . ?
C15 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
N3 C19 H19 119.7 . . ?
N3 C19 C20 120.7(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.4(3) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C22 117.2(3) . . ?
C20 C21 C24 121.6(3) . . ?
C22 C21 C24 121.0(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
N3 C23 C22 121.2(3) . . ?
N3 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C25 C24 C21 120.6(3) . . ?
C28 C24 C21 121.4(3) . . ?
C28 C24 C25 117.8(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
N4 C26 C25 121.1(3) . . ?
N4 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
N4 C27 H27 119.6 . . ?
N4 C27 C28 120.7(3) . . ?
C28 C27 H27 119.6 . . ?
C24 C28 H28 120.0 . . ?
C27 C28 C24 120.0(3) . . ?
C27 C28 H28 120.0 . . ?
N4 C29 H29A 109.7 . . ?
N4 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 N4 109.7(2) . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
C31 C30 C29 121.0(3) . . ?
C35 C30 C29 120.2(3) . . ?
C35 C30 C31 118.7(3) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.8(3) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.1(3) . . ?
C33 C32 H32 119.9 . . ?
C32 C33 C36 120.6(3) . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 C36 119.8(3) . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.1(3) . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 120.7(3) . . ?
C30 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
N1 C36 C33 107.6(2) . . ?
N1 C36 H36A 110.2 . . ?
N1 C36 H36B 110.2 . . ?
C33 C36 H36A 110.2 . . ?
C33 C36 H36B 110.2 . . ?
H36A C36 H36B 108.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C72 C71 H71A 109.5 . . ?
C72 C71 H71B 109.5 . . ?
C72 C71 H71C 109.5 . . ?
N7 C72 C71 178.4(8) . . ?
F19 P4 F21 177.7(3) . . ?
F19 P4 F22 89.9(3) . . ?
F19 P4 F23 90.4(3) . . ?
F20 P4 F19 91.2(3) . . ?
F20 P4 F21 89.5(2) . . ?
F20 P4 F22 178.9(2) . . ?
F20 P4 F23 91.6(3) . . ?
F21 P4 F22 89.4(2) . . ?
F21 P4 F23 87.5(2) . . ?
F22 P4 F23 88.7(3) . . ?
F24 P4 F19 92.0(3) . . ?
F24 P4 F20 91.9(3) . . ?
F24 P4 F21 90.1(2) . . ?
F24 P4 F22 87.8(3) . . ?
F24 P4 F23 175.8(3) . . ?
F19A P4A F24A 87.8(13) . . ?
F20A P4A F19A 85.3(13) . . ?
F20A P4A F21A 95.2(8) . . ?
F20A P4A F22A 169.6(11) . . ?
F20A P4A F24A 88.3(10) . . ?
F21A P4A F19A 177.7(15) . . ?
F21A P4A F22A 92.2(9) . . ?
F21A P4A F24A 90.0(9) . . ?
F22A P4A F19A 87.0(13) . . ?
F22A P4A F24A 84.4(9) . . ?
F23A P4A F19A 87.8(13) . . ?
F23A P4A F20A 95.8(11) . . ?
F23A P4A F21A 94.4(10) . . ?
F23A P4A F22A 90.8(11) . . ?
F23A P4A F24A 173.7(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C42 C43 C44 -177.1(3) . . . . ?
O1 C46 C47 O2 -73.8(4) . . . . ?
O2 C48 C49 O3 -72.7(3) . . . . ?
O3 C50 C51 C52 0.6(4) . . . . ?
O3 C50 C51 C56 180.0(2) . . . . ?
O3 C50 C59 C58 179.6(3) . . . . ?
O4 C55 C56 C51 179.6(2) . . . . ?
O4 C55 C56 C57 1.3(4) . . . . ?
O4 C60 C61 O5 -65.4(3) . . . . ?
O5 C62 C63 O6 -73.4(3) . . . . ?
O6 C64 C65 C66 177.9(3) . . . . ?
O6 C64 C69 C68 -178.6(3) . . . . ?
N6 C37 C38 N5 -39.0(4) . . . . ?
N6 C39 C40 C41 155.7(3) . . . . ?
N6 C39 C40 C45 -25.3(5) . . . . ?
N6 C67 C68 C69 174.5(3) . . . . ?
N6 C67 C68 C70 -4.7(5) . . . . ?
C37 N6 C39 C40 78.2(4) . . . . ?
C37 N6 C67 C66 137.4(3) . . . . ?
C37 N6 C67 C68 -40.2(4) . . . . ?
C38 N5 C45 C40 -42.4(4) . . . . ?
C38 N5 C45 C44 134.6(3) . . . . ?
C38 N5 C70 C68 78.8(3) . . . . ?
C39 N6 C37 C38 -48.3(4) . . . . ?
C39 N6 C67 C66 -87.1(3) . . . . ?
C39 N6 C67 C68 95.3(4) . . . . ?
C39 C40 C41 C42 179.2(3) . . . . ?
C39 C40 C45 N5 -1.9(5) . . . . ?
C39 C40 C45 C44 -178.8(3) . . . . ?
C40 C41 C42 O1 177.3(3) . . . . ?
C40 C41 C42 C43 -0.4(5) . . . . ?
C41 C40 C45 N5 177.2(3) . . . . ?
C41 C40 C45 C44 0.2(5) . . . . ?
C41 C42 C43 C44 0.4(5) . . . . ?
C42 O1 C46 C47 168.0(3) . . . . ?
C42 C43 C44 C45 0.0(5) . . . . ?
C43 C44 C45 N5 -177.5(3) . . . . ?
C43 C44 C45 C40 -0.3(5) . . . . ?
C45 N5 C38 C37 87.7(3) . . . . ?
C45 N5 C70 C68 -57.6(4) . . . . ?
C45 C40 C41 C42 0.1(5) . . . . ?
C46 O1 C42 C41 176.8(3) . . . . ?
C46 O1 C42 C43 -5.6(5) . . . . ?
C47 O2 C48 C49 -165.4(2) . . . . ?
C48 O2 C47 C46 -70.6(3) . . . . ?
C49 O3 C50 C51 -173.1(3) . . . . ?
C49 O3 C50 C59 6.8(4) . . . . ?
C50 O3 C49 C48 -83.9(3) . . . . ?
C50 C51 C52 C53 177.7(3) . . . . ?
C50 C51 C56 C55 -177.8(3) . . . . ?
C50 C51 C56 C57 0.5(4) . . . . ?
C51 C50 C59 C58 -0.6(5) . . . . ?
C51 C52 C53 C54 0.7(4) . . . . ?
C51 C56 C57 C58 -0.7(4) . . . . ?
C52 C51 C56 C55 1.6(4) . . . . ?
C52 C51 C56 C57 179.9(3) . . . . ?
C52 C53 C54 C55 0.4(5) . . . . ?
C53 C54 C55 O4 179.4(3) . . . . ?
C53 C54 C55 C56 -0.5(4) . . . . ?
C54 C55 C56 C51 -0.5(4) . . . . ?
C54 C55 C56 C57 -178.8(3) . . . . ?
C55 O4 C60 C61 -79.9(3) . . . . ?
C55 C56 C57 C58 177.5(3) . . . . ?
C56 C51 C52 C53 -1.7(4) . . . . ?
C56 C57 C58 C59 0.3(5) . . . . ?
C57 C58 C59 C50 0.4(5) . . . . ?
C59 C50 C51 C52 -179.3(3) . . . . ?
C59 C50 C51 C56 0.1(4) . . . . ?
C60 O4 C55 C54 5.7(4) . . . . ?
C60 O4 C55 C56 -174.4(2) . . . . ?
C61 O5 C62 C63 -83.5(3) . . . . ?
C62 O5 C61 C60 -171.2(3) . . . . ?
C63 O6 C64 C65 0.6(4) . . . . ?
C63 O6 C64 C69 -179.2(3) . . . . ?
C64 O6 C63 C62 171.4(2) . . . . ?
C64 C65 C66 C67 0.3(5) . . . . ?
C65 C64 C69 C68 1.6(4) . . . . ?
C65 C66 C67 N6 -175.3(3) . . . . ?
C65 C66 C67 C68 2.5(5) . . . . ?
C66 C67 C68 C69 -3.1(4) . . . . ?
C66 C67 C68 C70 177.7(3) . . . . ?
C67 N6 C37 C38 87.7(3) . . . . ?
C67 N6 C39 C40 -57.0(4) . . . . ?
C67 C68 C69 C64 1.1(4) . . . . ?
C67 C68 C70 N5 -23.2(4) . . . . ?
C69 C64 C65 C66 -2.3(4) . . . . ?
C69 C68 C70 N5 157.6(3) . . . . ?
C70 N5 C38 C37 -49.5(4) . . . . ?
C70 N5 C45 C40 93.7(4) . . . . ?
C70 N5 C45 C44 -89.3(4) . . . . ?
C70 C68 C69 C64 -179.6(3) . . . . ?
N1 C1 C2 C3 0.2(5) . . . . ?
N2 C9 C10 C6 0.2(5) . . . . ?
N2 C11 C12 C13 92.0(4) . . . . ?
N2 C11 C12 C17 -85.6(4) . . . . ?
N3 C19 C20 C21 0.6(5) . . . . ?
N4 C27 C28 C24 0.7(5) . . . . ?
N4 C29 C30 C31 85.5(4) . . . . ?
N4 C29 C30 C35 -89.8(4) . . . . ?
C1 N1 C5 C4 1.7(4) . . . . ?
C1 N1 C36 C33 -101.1(3) . . . . ?
C1 C2 C3 C4 1.7(4) . . . . ?
C1 C2 C3 C6 -175.8(3) . . . . ?
C2 C3 C4 C5 -1.9(4) . . . . ?
C2 C3 C6 C7 32.3(4) . . . . ?
C2 C3 C6 C10 -151.8(3) . . . . ?
C3 C4 C5 N1 0.2(4) . . . . ?
C3 C6 C7 C8 172.3(3) . . . . ?
C3 C6 C10 C9 -172.9(3) . . . . ?
C4 C3 C6 C7 -145.1(3) . . . . ?
C4 C3 C6 C10 30.8(4) . . . . ?
C5 N1 C1 C2 -1.9(5) . . . . ?
C5 N1 C36 C33 73.6(3) . . . . ?
C6 C3 C4 C5 175.7(3) . . . . ?
C6 C7 C8 N2 1.1(5) . . . . ?
C7 C6 C10 C9 3.1(5) . . . . ?
C8 N2 C9 C10 -3.0(5) . . . . ?
C8 N2 C11 C12 71.1(4) . . . . ?
C9 N2 C8 C7 2.3(5) . . . . ?
C9 N2 C11 C12 -104.1(3) . . . . ?
C10 C6 C7 C8 -3.7(5) . . . . ?
C11 N2 C8 C7 -172.9(3) . . . . ?
C11 N2 C9 C10 172.1(3) . . . . ?
C11 C12 C13 C14 -173.6(3) . . . . ?
C11 C12 C17 C16 174.5(3) . . . . ?
C12 C13 C14 C15 -0.7(5) . . . . ?
C13 C12 C17 C16 -3.1(5) . . . . ?
C13 C14 C15 C16 -3.6(5) . . . . ?
C13 C14 C15 C18 171.8(3) . . . . ?
C14 C15 C16 C17 4.5(4) . . . . ?
C14 C15 C18 N3 -89.0(4) . . . . ?
C15 C16 C17 C12 -1.2(5) . . . . ?
C16 C15 C18 N3 86.3(4) . . . . ?
C17 C12 C13 C14 4.0(5) . . . . ?
C18 N3 C19 C20 -171.7(3) . . . . ?
C18 N3 C23 C22 171.3(3) . . . . ?
C18 C15 C16 C17 -170.9(3) . . . . ?
C19 N3 C18 C15 91.2(4) . . . . ?
C19 N3 C23 C22 -2.4(5) . . . . ?
C19 C20 C21 C22 -2.6(4) . . . . ?
C19 C20 C21 C24 172.9(3) . . . . ?
C20 C21 C22 C23 2.0(4) . . . . ?
C20 C21 C24 C25 -15.3(4) . . . . ?
C20 C21 C24 C28 169.2(3) . . . . ?
C21 C22 C23 N3 0.4(5) . . . . ?
C21 C24 C25 C26 -173.1(3) . . . . ?
C21 C24 C28 C27 172.6(3) . . . . ?
C22 C21 C24 C25 160.0(3) . . . . ?
C22 C21 C24 C28 -15.5(4) . . . . ?
C23 N3 C18 C15 -82.5(4) . . . . ?
C23 N3 C19 C20 1.9(5) . . . . ?
C24 C21 C22 C23 -173.4(3) . . . . ?
C24 C25 C26 N4 0.4(5) . . . . ?
C25 C24 C28 C27 -3.1(5) . . . . ?
C26 N4 C27 C28 2.3(5) . . . . ?
C26 N4 C29 C30 -75.3(4) . . . . ?
C27 N4 C26 C25 -2.9(5) . . . . ?
C27 N4 C29 C30 102.2(3) . . . . ?
C28 C24 C25 C26 2.6(5) . . . . ?
C29 N4 C26 C25 174.6(3) . . . . ?
C29 N4 C27 C28 -175.1(3) . . . . ?
C29 C30 C31 C32 -172.0(3) . . . . ?
C29 C30 C35 C34 171.9(3) . . . . ?
C30 C31 C32 C33 0.3(5) . . . . ?
C31 C30 C35 C34 -3.5(5) . . . . ?
C31 C32 C33 C34 -3.8(5) . . . . ?
C31 C32 C33 C36 170.3(3) . . . . ?
C32 C33 C34 C35 3.6(5) . . . . ?
C32 C33 C36 N1 -88.1(3) . . . . ?
C33 C34 C35 C30 0.0(5) . . . . ?
C34 C33 C36 N1 85.9(3) . . . . ?
C35 C30 C31 C32 3.4(5) . . . . ?
C36 N1 C1 C2 172.5(3) . . . . ?
C36 N1 C5 C4 -172.8(3) . . . . ?
C36 C33 C34 C35 -170.5(3) . . . . ?

_olex2_date_sample_submission    2021-11-23
_olex2_exptl_crystal_mounting_method CryoLoop
_olex2_submission_original_sample_id MR530
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.593
_oxdiff_exptl_absorpt_empirical_full_min 0.497
_vrf_PLAT260_MR530               
;
PROBLEM: Large Average Ueq of Residue Including        O7      0.312 Check 
RESPONSE: O7 is an oxygen atom on the [H2O] solvent molecule.
Structure contains four [PF6]-, one [H2O], and one [MeCN] molecules.
One [PF6]- and the [H2O] molecule were found to be disordered. The [PF6]-
molecule was split and that took care of the extra electron density around
the PF6. Splitting the [H2O] molecule (with and without constrains
on the thermal factors) did not resolve the extra electron density in an
ordered fashion. The water molecule was refined as a single O7 site with
a large thermal factor (especially U22).
;
####################################################################### 
# 
# 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_MR518
_database_code_depnum_ccdc_archive 'CCDC 2087908'
loop_
_audit_author_name
_audit_author_address
'Masoud Kazem-Rostami'
;Northwestern University
United States of America
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_audit_creation_date             2021-06-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            MR518
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H36 N2 O6'
_chemical_formula_sum            'C34 H36 N2 O6'
_chemical_formula_weight         568.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         C34H36N2O6
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   34.8333(8)
_cell_length_b                   9.1764(2)
_cell_length_c                   36.0630(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.626(2)
_cell_angle_gamma                90
_cell_volume                     11471.8(5)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    31163
_cell_measurement_temperature    99.96(17)
_cell_measurement_theta_max      33.6440
_cell_measurement_theta_min      2.2590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4832
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.0849
0 -1 -1 0.0819
0 1 1 0.0789
-1 0 1 0.0724
1 0 1 0.0382
-1 0 -1 0.0382

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeCN / CH2Cl2'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.076
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9993 -0.0003 -0.9998 0.0076 -0.0083 -0.0246
0.0011 -0.9989 -1.0010 0.0104 -0.0776 0.0150
-0.0011 0.9989 1.0010 -0.0104 0.0776 -0.0150
-0.9993 0.0003 0.9998 -0.0076 0.0083 0.0246
1.0436 0.0076 0.9473 0.0279 0.0101 0.0026
-1.0436 -0.0076 -0.9473 -0.0279 -0.0101 -0.0026

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            82245
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.951
_diffrn_reflns_theta_min         2.270
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00   5.00   0.50   15.00    --   13.12 -58.00 152.00   66
  2  ω     22.00  53.00   0.50   15.00    --   13.12  58.00 -67.00   62
  3  ω    -85.00   2.00   0.50   15.00    --  -13.59 -58.00 152.00  174
  4  ω    -57.00 -26.00   0.50   10.00    --   13.12 -58.00 152.00   62
  5  ω    -22.00  11.00   0.50   10.00    --   13.12 -99.00  30.00   66
  6  ω     12.00  38.00   0.50   10.00    --   13.12 -99.00 120.00   52
  7  ω      3.00  28.00   0.50   10.00    --   13.12 -58.00 152.00   50
  8  ω     39.00  64.00   0.50   10.00    --   13.12-178.00   0.00   50
  9  ω    -80.00  -1.00   0.50   10.00    --  -13.59 -57.00  30.00  158
 10  ω    -86.00 -60.00   0.50   10.00    --  -13.59 178.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0176803000
_diffrn_orient_matrix_UB_12      -0.0205284000
_diffrn_orient_matrix_UB_13      0.0101005000
_diffrn_orient_matrix_UB_21      0.0008929000
_diffrn_orient_matrix_UB_22      0.0684573000
_diffrn_orient_matrix_UB_23      0.0091639000
_diffrn_orient_matrix_UB_31      -0.0102717000
_diffrn_orient_matrix_UB_32      -0.0293425000
_diffrn_orient_matrix_UB_33      0.0143193000
_diffrn_oxdiff_digest_frames     
;
012cee533abea897188929c536765d824a0079231b5
;
_diffrn_oxdiff_digest_hkl        
;
01c854fe6600a14f9489e5d3bdb3573ff38668
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14393
_reflns_number_total             19738
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         19738
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0876
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0428P)²+44.7861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2099
_refine_special_details          
'The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied on the disordered atoms. (Acta Cryst. A68 (2012) 448-451)'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Rigid body (RIGU) restrains
 O2A, O3A, O3B, O4A, O4B, O5A, C19A, C20A, C21A, C21B, C22A, C22B, C23A, C23B,
 C24A, C24B, C25A, C25B, C26A, C26B, C27A, C27B, C28A, C28B, C29A, C29B, C30A,
 C30B, C31A, C32A, C33A, C18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(O3B)=Sof(O4B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(C26B)=Sof(C27B)=Sof(H27B)=
 Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=Sof(H27A)=
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10C,H10D), C17(H17C,H17D),
 C18(H18C,H18D), C19(H19C,H19D), C20(H20E,H20F), C31(H31E,H31F), C32(H32C,H32D),
  C33(H33C,H33D), C34(H34C,H34D), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,
 H9AB), C10A(H10A,H10B), C17A(H17A,H17B), C18A(H18A,H18B), C19A(H19A,H19B),
 C20A(H20A,H20B), C20A(H20C,H20D), C31A(H31A,H31B), C31A(H31C,H31D), C32A(H32A,
 H32B), C33A(H33A,H33B), C34A(H34A,H34B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C13(H13), C14(H14), C16(H16), C22(H22), C23(H23),
 C24(H24), C27(H27), C28(H28), C29(H29), C2A(H2A), C3A(H3A), C5A(H5A),
 C13A(H13A), C14A(H14A), C16A(H16A), C22A(H22A), C22B(H22B), C23A(H23A),
 C23B(H23B), C24A(H24A), C24B(H24B), C27A(H27A), C27B(H27B), C28A(H28A),
 C28B(H28B), C29A(H29A), C29B(H29B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.65200(5) 0.73849(19) 0.48121(5) 0.0307(4) Uani 1 1 d . . . . .
O2 O 0.67815(5) 0.90435(18) 0.42289(5) 0.0263(3) Uani 1 1 d . . . . .
O3 O 0.61242(5) 0.7986(2) 0.37834(4) 0.0269(3) Uani 1 1 d . . . . .
O4 O 0.45616(5) 0.54971(19) 0.33872(5) 0.0270(3) Uani 1 1 d . . . . .
O5 O 0.45983(5) 0.24208(18) 0.35827(5) 0.0282(4) Uani 1 1 d . . . . .
O6 O 0.48916(4) 0.06912(19) 0.41615(4) 0.0250(3) Uani 1 1 d . . . . .
N1 N 0.56865(5) 0.3338(2) 0.55681(5) 0.0208(3) Uani 1 1 d . . . . .
N2 N 0.61241(5) 0.1110(2) 0.52777(5) 0.0211(3) Uani 1 1 d . . . . .
C1 C 0.58045(6) 0.1060(2) 0.49927(5) 0.0184(4) Uani 1 1 d . . . . .
C2 C 0.58597(6) 0.0313(2) 0.46661(6) 0.0189(4) Uani 1 1 d . . . . .
H2 H 0.610432 -0.011073 0.463941 0.023 Uiso 1 1 calc R . . . .
C3 C 0.55650(6) 0.0170(2) 0.43768(6) 0.0205(4) Uani 1 1 d . . . . .
H3 H 0.560842 -0.033263 0.415435 0.025 Uiso 1 1 calc R . . . .
C4 C 0.52064(6) 0.0778(2) 0.44210(6) 0.0196(4) Uani 1 1 d . . . . .
C5 C 0.51492(6) 0.1532(2) 0.47457(6) 0.0196(4) Uani 1 1 d . . . . .
H5 H 0.490297 0.194127 0.477263 0.024 Uiso 1 1 calc R . . . .
C6 C 0.54440(6) 0.1702(2) 0.50322(6) 0.0193(4) Uani 1 1 d . . . . .
C7 C 0.53551(6) 0.2602(2) 0.53677(6) 0.0215(4) Uani 1 1 d . . . . .
H7A H 0.516079 0.334855 0.528274 0.026 Uiso 1 1 calc R . . . .
H7B H 0.523703 0.195469 0.554448 0.026 Uiso 1 1 calc R . . . .
C8 C 0.59152(7) 0.2405(3) 0.58318(6) 0.0256(4) Uani 1 1 d . . . . .
H8A H 0.576831 0.221393 0.604820 0.031 Uiso 1 1 calc R . . . .
H8B H 0.615530 0.292196 0.592364 0.031 Uiso 1 1 calc R . . . .
C9 C 0.60200(7) 0.0950(3) 0.56606(6) 0.0260(4) Uani 1 1 d . . . . .
H9A H 0.623966 0.051153 0.581675 0.031 Uiso 1 1 calc R . . . .
H9B H 0.579796 0.027716 0.566060 0.031 Uiso 1 1 calc R . . . .
C10 C 0.63991(6) 0.2279(2) 0.52305(6) 0.0227(4) Uani 1 1 d . . . . .
H10C H 0.652915 0.206475 0.500453 0.027 Uiso 1 1 calc R . . . .
H10D H 0.659891 0.225111 0.544550 0.027 Uiso 1 1 calc R . . . .
C11 C 0.62401(6) 0.3829(2) 0.51960(6) 0.0203(4) Uani 1 1 d . . . . .
C12 C 0.59019(6) 0.4266(2) 0.53453(6) 0.0208(4) Uani 1 1 d . . . . .
C13 C 0.57698(6) 0.5690(3) 0.52861(6) 0.0238(4) Uani 1 1 d . . . . .
H13 H 0.553356 0.597123 0.537630 0.029 Uiso 1 1 calc R . . . .
C14 C 0.59735(7) 0.6704(3) 0.50996(6) 0.0260(4) Uani 1 1 d . . . . .
H14 H 0.587779 0.766716 0.506072 0.031 Uiso 1 1 calc R . . . .
C15 C 0.63232(7) 0.6287(3) 0.49688(6) 0.0246(4) Uani 1 1 d . . . . .
C16 C 0.64500(6) 0.4857(2) 0.50112(6) 0.0229(4) Uani 1 1 d . . . . .
H16 H 0.668213 0.457160 0.491352 0.028 Uiso 1 1 calc R . . . .
C17 C 0.68815(7) 0.7051(3) 0.46777(7) 0.0288(5) Uani 1 1 d . . . . .
H17C H 0.684775 0.630059 0.447998 0.035 Uiso 1 1 calc R . . . .
H17D H 0.706493 0.667659 0.488266 0.035 Uiso 1 1 calc R . . . .
C18 C 0.70313(7) 0.8451(3) 0.45240(7) 0.0303(5) Uani 1 1 d . . . . .
H18C H 0.706856 0.917672 0.472745 0.036 Uiso 1 1 calc R . . . .
H18D H 0.728610 0.826208 0.443373 0.036 Uiso 1 1 calc R . . . .
C19 C 0.67956(6) 0.8266(3) 0.38890(7) 0.0261(4) Uani 1 1 d . . . . .
H19C H 0.680176 0.720480 0.393864 0.031 Uiso 1 1 calc R . . . .
H19D H 0.703240 0.853121 0.377362 0.031 Uiso 1 1 calc R . . . .
C20 C 0.64472(6) 0.8639(3) 0.36301(6) 0.0256(4) Uani 1 1 d . . . . .
H20E H 0.641410 0.970900 0.361228 0.031 Uiso 1 1 calc R . . . .
H20F H 0.647314 0.824892 0.337778 0.031 Uiso 1 1 calc R . . . .
C21 C 0.57896(6) 0.7864(2) 0.35587(6) 0.0228(4) Uani 1 1 d . . . . .
C22 C 0.57097(7) 0.8550(3) 0.32215(6) 0.0264(4) Uani 1 1 d . . . . .
H22 H 0.589304 0.919264 0.313105 0.032 Uiso 1 1 calc R . . . .
C23 C 0.53530(7) 0.8294(3) 0.30103(6) 0.0266(4) Uani 1 1 d . . . . .
H23 H 0.529801 0.877714 0.277822 0.032 Uiso 1 1 calc R . . . .
C24 C 0.50852(7) 0.7367(3) 0.31321(6) 0.0239(4) Uani 1 1 d . . . . .
H24 H 0.484922 0.719648 0.298298 0.029 Uiso 1 1 calc R . . . .
C25 C 0.51604(6) 0.6659(2) 0.34827(6) 0.0198(4) Uani 1 1 d . . . . .
C26 C 0.48918(6) 0.5684(2) 0.36235(6) 0.0210(4) Uani 1 1 d . . . . .
C27 C 0.49705(6) 0.5023(2) 0.39657(6) 0.0217(4) Uani 1 1 d . . . . .
H27 H 0.479218 0.435088 0.405274 0.026 Uiso 1 1 calc R . . . .
C28 C 0.53173(6) 0.5348(2) 0.41860(6) 0.0220(4) Uani 1 1 d . . . . .
H28 H 0.536595 0.491511 0.442521 0.026 Uiso 1 1 calc R . . . .
C29 C 0.55861(6) 0.6280(2) 0.40618(6) 0.0214(4) Uani 1 1 d . . . . .
H29 H 0.581832 0.648623 0.421343 0.026 Uiso 1 1 calc R . . . .
C30 C 0.55131(6) 0.6928(2) 0.37052(6) 0.0195(4) Uani 1 1 d . . . . .
C31 C 0.42522(6) 0.4643(3) 0.35029(7) 0.0262(4) Uani 1 1 d . . . . .
H31E H 0.400405 0.506427 0.339616 0.031 Uiso 1 1 calc R . . . .
H31F H 0.425855 0.468567 0.377771 0.031 Uiso 1 1 calc R . . . .
C32 C 0.42730(7) 0.3078(3) 0.33839(7) 0.0301(5) Uani 1 1 d . . . . .
H32C H 0.403521 0.255850 0.343653 0.036 Uiso 1 1 calc R . . . .
H32D H 0.429574 0.302369 0.311278 0.036 Uiso 1 1 calc R . . . .
C33 C 0.46118(7) 0.0887(3) 0.35431(7) 0.0286(5) Uani 1 1 d . . . . .
H33C H 0.463335 0.062354 0.327975 0.034 Uiso 1 1 calc R . . . .
H33D H 0.437406 0.044024 0.362164 0.034 Uiso 1 1 calc R . . . .
C34 C 0.49601(7) 0.0351(3) 0.37864(6) 0.0280(5) Uani 1 1 d . . . . .
H34C H 0.499171 -0.071376 0.375628 0.034 Uiso 1 1 calc R . . . .
H34D H 0.519651 0.084374 0.371961 0.034 Uiso 1 1 calc R . . . .
O1A O 0.75603(5) 0.9793(2) 0.33528(5) 0.0295(4) Uani 1 1 d . . . . .
O2A O 0.79261(7) 0.9396(4) 0.40754(7) 0.0778(9) Uani 1 1 d . U . . .
O3A O 0.79430(11) 0.6546(4) 0.39531(8) 0.0417(8) Uani 0.613(3) 1 d . U P A 1
O3B O 0.8039(2) 0.5625(11) 0.4004(2) 0.083(2) Uani 0.387(3) 1 d . U P A 2
O4A O 0.65979(12) 0.2419(4) 0.37711(10) 0.0485(9) Uani 0.613(3) 1 d . U P A 1
O4B O 0.6431(2) 0.3274(6) 0.37080(14) 0.0473(11) Uani 0.387(3) 1 d . U P A 2
O5A O 0.58025(9) 0.2270(3) 0.33436(8) 0.0682(7) Uani 1 1 d . U . . .
O6A O 0.59274(5) 0.3650(2) 0.26555(5) 0.0361(4) Uani 1 1 d . . . . .
N1A N 0.63915(6) 0.9807(2) 0.21707(6) 0.0299(4) Uani 1 1 d . . . . .
N2A N 0.68069(6) 0.7496(2) 0.18812(5) 0.0257(4) Uani 1 1 d . . . . .
C1A C 0.65631(6) 0.6603(3) 0.20854(6) 0.0234(4) Uani 1 1 d . . . . .
C2A C 0.66656(6) 0.5134(3) 0.21291(6) 0.0249(4) Uani 1 1 d . . . . .
H2A H 0.688808 0.478787 0.202404 0.030 Uiso 1 1 calc R . . . .
C3A C 0.64520(7) 0.4175(3) 0.23208(6) 0.0281(5) Uani 1 1 d . . . . .
H3A H 0.652696 0.318236 0.234947 0.034 Uiso 1 1 calc R . . . .
C4A C 0.61233(7) 0.4692(3) 0.24719(7) 0.0276(5) Uani 1 1 d . . . . .
C5A C 0.60163(6) 0.6139(3) 0.24319(7) 0.0266(5) Uani 1 1 d . . . . .
H5A H 0.579220 0.647673 0.253574 0.032 Uiso 1 1 calc R . . . .
C6A C 0.62353(6) 0.7113(3) 0.22395(6) 0.0249(4) Uani 1 1 d . . . . .
C7A C 0.60990(7) 0.8689(3) 0.22009(7) 0.0305(5) Uani 1 1 d . . . . .
H7AA H 0.591077 0.875551 0.197729 0.037 Uiso 1 1 calc R . . . .
H7AB H 0.595898 0.892537 0.241925 0.037 Uiso 1 1 calc R . . . .
C8A C 0.65210(9) 0.9975(3) 0.17981(7) 0.0383(6) Uani 1 1 d . . . . .
H8AA H 0.675586 1.058885 0.181591 0.046 Uiso 1 1 calc R . . . .
H8AB H 0.631837 1.048530 0.163550 0.046 Uiso 1 1 calc R . . . .
C9A C 0.66093(8) 0.8515(3) 0.16201(7) 0.0369(6) Uani 1 1 d . . . . .
H9AA H 0.636438 0.807087 0.151244 0.044 Uiso 1 1 calc R . . . .
H9AB H 0.677108 0.869230 0.141374 0.044 Uiso 1 1 calc R . . . .
C10A C 0.71347(6) 0.8107(3) 0.21134(6) 0.0257(4) Uani 1 1 d . . . . .
H10A H 0.728128 0.873663 0.195464 0.031 Uiso 1 1 calc R . . . .
H10B H 0.730662 0.729388 0.220237 0.031 Uiso 1 1 calc R . . . .
C11A C 0.70431(6) 0.8993(3) 0.24508(6) 0.0235(4) Uani 1 1 d . . . . .
C12A C 0.66979(7) 0.9784(3) 0.24676(6) 0.0255(4) Uani 1 1 d . . . . .
C13A C 0.66474(7) 1.0599(3) 0.27855(6) 0.0263(4) Uani 1 1 d . . . . .
H13A H 0.641512 1.113216 0.279685 0.032 Uiso 1 1 calc R . . . .
C14A C 0.69291(7) 1.0649(3) 0.30862(6) 0.0264(4) Uani 1 1 d . . . . .
H14A H 0.689140 1.122105 0.329922 0.032 Uiso 1 1 calc R . . . .
C15A C 0.72665(6) 0.9853(3) 0.30715(6) 0.0243(4) Uani 1 1 d . . . . .
C16A C 0.73199(6) 0.9031(3) 0.27557(6) 0.0236(4) Uani 1 1 d . . . . .
H16A H 0.755075 0.848478 0.274856 0.028 Uiso 1 1 calc R . . . .
C17A C 0.75612(7) 1.0873(3) 0.36408(7) 0.0343(6) Uani 1 1 d . . . . .
H17A H 0.734009 1.072115 0.378926 0.041 Uiso 1 1 calc R . . . .
H17B H 0.754100 1.186184 0.353053 0.041 Uiso 1 1 calc R . . . .
C18A C 0.79283(9) 1.0715(5) 0.38788(8) 0.0554(8) Uani 1 1 d . U . . .
H18A H 0.814670 1.072618 0.372263 0.066 Uiso 1 1 calc R . . . .
H18B H 0.796100 1.153946 0.405609 0.066 Uiso 1 1 calc R . . . .
C19A C 0.82699(11) 0.8614(5) 0.40821(13) 0.0789(12) Uani 1 1 d . U . . .
H19A H 0.847669 0.911304 0.424211 0.095 Uiso 1 1 calc R . . . .
H19B H 0.835116 0.853099 0.382749 0.095 Uiso 1 1 calc R . . . .
C20A C 0.81999(11) 0.7224(6) 0.42257(12) 0.0769(11) Uani 1 1 d . U . . .
H20A H 0.808313 0.730459 0.446435 0.092 Uiso 0.613(3) 1 calc R . P A 1
H20B H 0.844282 0.666207 0.426825 0.092 Uiso 0.613(3) 1 calc R . P A 1
H20C H 0.801556 0.739994 0.441311 0.092 Uiso 0.387(3) 1 calc R . P A 2
H20D H 0.844600 0.695011 0.436959 0.092 Uiso 0.387(3) 1 calc R . P A 2
C21A C 0.77120(14) 0.5498(5) 0.40822(12) 0.0350(7) Uani 0.613(3) 1 d . U P A 1
C21B C 0.6769(3) 0.3393(9) 0.3920(2) 0.0484(12) Uani 0.387(3) 1 d . U P A 2
C22A C 0.77872(15) 0.4824(5) 0.44223(12) 0.0406(9) Uani 0.613(3) 1 d . U P A 1
H22A H 0.800540 0.509279 0.458692 0.049 Uiso 0.613(3) 1 calc R . P A 1
C22B C 0.6872(4) 0.2717(11) 0.4257(2) 0.065(2) Uani 0.387(3) 1 d . U P A 2
H22B H 0.669494 0.207598 0.435760 0.078 Uiso 0.387(3) 1 calc R . P A 2
C23A C 0.75315(17) 0.3718(6) 0.45219(15) 0.0443(10) Uani 0.613(3) 1 d . U P A 1
H23A H 0.758078 0.325649 0.475758 0.053 Uiso 0.613(3) 1 calc R . P A 1
C23B C 0.7230(4) 0.2957(16) 0.4452(3) 0.080(2) Uani 0.387(3) 1 d . U P A 2
H23B H 0.729058 0.248440 0.468500 0.096 Uiso 0.387(3) 1 calc R . P A 2
C24A C 0.72234(18) 0.3301(6) 0.42956(15) 0.0419(10) Uani 0.613(3) 1 d . U P A 1
H24A H 0.706255 0.253950 0.436967 0.050 Uiso 0.613(3) 1 calc R . P A 1
C24B C 0.7501(4) 0.3859(15) 0.4319(3) 0.077(2) Uani 0.387(3) 1 d . U P A 2
H24B H 0.774429 0.400361 0.445763 0.093 Uiso 0.387(3) 1 calc R . P A 2
C25A C 0.71345(15) 0.4006(5) 0.39388(13) 0.0334(7) Uani 0.613(3) 1 d . U P A 1
C25B C 0.7411(3) 0.4577(13) 0.3969(3) 0.0583(15) Uani 0.387(3) 1 d . U P A 2
C26A C 0.68178(14) 0.3605(5) 0.36883(13) 0.0347(8) Uani 0.613(3) 1 d . U P A 1
C26B C 0.7672(3) 0.5533(11) 0.3808(3) 0.0579(15) Uani 0.387(3) 1 d . U P A 2
C27A C 0.67438(13) 0.4281(5) 0.33442(12) 0.0326(8) Uani 0.613(3) 1 d . U P A 1
H27A H 0.652853 0.399725 0.317765 0.039 Uiso 0.613(3) 1 calc R . P A 1
C27B C 0.7581(2) 0.6213(10) 0.3469(3) 0.0515(16) Uani 0.387(3) 1 d . U P A 2
H27B H 0.775616 0.687102 0.337221 0.062 Uiso 0.387(3) 1 calc R . P A 2
C28A C 0.69928(14) 0.5395(5) 0.32460(13) 0.0302(8) Uani 0.613(3) 1 d . U P A 1
H28A H 0.694169 0.586719 0.301194 0.036 Uiso 0.613(3) 1 calc R . P A 1
C28B C 0.7219(2) 0.5902(9) 0.3270(3) 0.0377(13) Uani 0.387(3) 1 d . U P A 2
H28B H 0.715559 0.633972 0.303369 0.045 Uiso 0.387(3) 1 calc R . P A 2
C29A C 0.73042(13) 0.5809(4) 0.34779(12) 0.0277(7) Uani 0.613(3) 1 d . U P A 1
H29A H 0.746808 0.656225 0.340493 0.033 Uiso 0.613(3) 1 calc R . P A 1
C29B C 0.6959(2) 0.4988(8) 0.3410(2) 0.0336(12) Uani 0.387(3) 1 d . U P A 2
H29B H 0.671923 0.478948 0.327006 0.040 Uiso 0.387(3) 1 calc R . P A 2
C30A C 0.73868(14) 0.5108(5) 0.38350(12) 0.0304(7) Uani 0.613(3) 1 d . U P A 1
C30B C 0.7047(3) 0.4336(9) 0.3766(2) 0.0434(12) Uani 0.387(3) 1 d . U P A 2
C31A C 0.62017(14) 0.2676(4) 0.39206(11) 0.0695(8) Uani 1 1 d . U . . .
H31A H 0.612880 0.175558 0.403872 0.083 Uiso 0.613(3) 1 calc R . P A 1
H31B H 0.624084 0.341155 0.412146 0.083 Uiso 0.613(3) 1 calc R . P A 1
H31C H 0.621242 0.312003 0.417152 0.083 Uiso 0.387(3) 1 calc R . P A 2
H31D H 0.623007 0.160372 0.393824 0.083 Uiso 0.387(3) 1 calc R . P A 2
C32A C 0.58668(15) 0.3147(5) 0.36686(14) 0.0853(12) Uani 1 1 d . U . . .
H32A H 0.563375 0.311939 0.380498 0.102 Uiso 1 1 calc R . . . .
H32B H 0.590660 0.416910 0.359304 0.102 Uiso 1 1 calc R . . . .
C33A C 0.55074(12) 0.2814(4) 0.30845(13) 0.0690(9) Uani 1 1 d . U . . .
H33A H 0.528503 0.309006 0.322075 0.083 Uiso 1 1 calc R . . . .
H33B H 0.542119 0.201951 0.291011 0.083 Uiso 1 1 calc R . . . .
C34A C 0.56183(9) 0.4120(3) 0.28583(10) 0.0461(7) Uani 1 1 d . . . . .
H34A H 0.539623 0.444249 0.268528 0.055 Uiso 1 1 calc R . . . .
H34B H 0.570180 0.494202 0.302486 0.055 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.371(3) . ?
O1 C17 1.426(3) . ?
O2 C18 1.416(3) . ?
O2 C19 1.423(3) . ?
O3 C20 1.433(3) . ?
O3 C21 1.357(3) . ?
O4 C26 1.373(3) . ?
O4 C31 1.428(3) . ?
O5 C32 1.415(3) . ?
O5 C33 1.416(3) . ?
O6 C4 1.372(2) . ?
O6 C34 1.431(3) . ?
N1 C7 1.465(3) . ?
N1 C8 1.457(3) . ?
N1 C12 1.433(3) . ?
N2 C1 1.440(3) . ?
N2 C9 1.469(3) . ?
N2 C10 1.459(3) . ?
C1 C2 1.392(3) . ?
C1 C6 1.407(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(3) . ?
C4 C5 1.391(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(3) . ?
C6 C7 1.522(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.529(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 C11 1.527(3) . ?
C11 C12 1.401(3) . ?
C11 C16 1.402(3) . ?
C12 C13 1.394(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.402(3) . ?
C15 C16 1.388(3) . ?
C16 H16 0.9500 . ?
C17 H17C 0.9900 . ?
C17 H17D 0.9900 . ?
C17 C18 1.512(4) . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C19 C20 1.497(3) . ?
C20 H20E 0.9900 . ?
C20 H20F 0.9900 . ?
C21 C22 1.374(3) . ?
C21 C30 1.430(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.412(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.366(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.423(3) . ?
C25 C26 1.424(3) . ?
C25 C30 1.421(3) . ?
C26 C27 1.379(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.411(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.375(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.417(3) . ?
C31 H31E 0.9900 . ?
C31 H31F 0.9900 . ?
C31 C32 1.502(3) . ?
C32 H32C 0.9900 . ?
C32 H32D 0.9900 . ?
C33 H33C 0.9900 . ?
C33 H33D 0.9900 . ?
C33 C34 1.509(3) . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
O1A C15A 1.370(3) . ?
O1A C17A 1.436(3) . ?
O2A C18A 1.404(5) . ?
O2A C19A 1.394(4) . ?
O3A C20A 1.408(5) . ?
O3A C21A 1.365(6) . ?
O3B C20A 1.738(9) . ?
O3B C26B 1.401(11) . ?
O4A C26A 1.380(6) . ?
O4A C31A 1.548(5) . ?
O4B C21B 1.346(12) . ?
O4B C31A 1.284(6) . ?
O5A C32A 1.421(5) . ?
O5A C33A 1.411(5) . ?
O6A C4A 1.381(3) . ?
O6A C34A 1.427(3) . ?
N1A C7A 1.457(3) . ?
N1A C8A 1.467(3) . ?
N1A C12A 1.436(3) . ?
N2A C1A 1.435(3) . ?
N2A C9A 1.452(3) . ?
N2A C10A 1.460(3) . ?
C1A C2A 1.399(3) . ?
C1A C6A 1.399(3) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.381(3) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.399(3) . ?
C4A C5A 1.383(3) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.402(4) . ?
C6A C7A 1.524(3) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A C9A 1.529(4) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10A C11A 1.523(3) . ?
C11A C12A 1.411(3) . ?
C11A C16A 1.390(3) . ?
C12A C13A 1.394(3) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.390(3) . ?
C14A H14A 0.9500 . ?
C14A C15A 1.389(3) . ?
C15A C16A 1.394(3) . ?
C16A H16A 0.9500 . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C17A C18A 1.476(4) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C19A C20A 1.407(7) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C21A C22A 1.376(6) . ?
C21A C30A 1.417(7) . ?
C21B C22B 1.380(12) . ?
C21B C30B 1.449(14) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.420(8) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.388(18) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.339(9) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.38(2) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.446(7) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.432(18) . ?
C25A C26A 1.405(7) . ?
C25A C30A 1.414(7) . ?
C25B C26B 1.425(18) . ?
C25B C30B 1.417(13) . ?
C26A C27A 1.389(6) . ?
C26B C27B 1.382(15) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.408(6) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.417(11) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.357(6) . ?
C28B H28B 0.9500 . ?
C28B C29B 1.367(12) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.443(6) . ?
C29B H29B 0.9500 . ?
C29B C30B 1.422(13) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C31A C32A 1.472(7) . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
C33A H33A 0.9900 . ?
C33A H33B 0.9900 . ?
C33A C34A 1.521(5) . ?
C34A H34A 0.9900 . ?
C34A H34B 0.9900 . ?

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
C15 O1 C17 118.42(19) . . ?
C18 O2 C19 112.60(18) . . ?
C21 O3 C20 117.71(17) . . ?
C26 O4 C31 119.85(18) . . ?
C32 O5 C33 113.93(18) . . ?
C4 O6 C34 117.46(17) . . ?
C8 N1 C7 113.90(18) . . ?
C12 N1 C7 115.33(16) . . ?
C12 N1 C8 115.63(18) . . ?
C1 N2 C9 115.03(17) . . ?
C1 N2 C10 114.26(17) . . ?
C10 N2 C9 114.11(18) . . ?
C2 C1 N2 117.29(18) . . ?
C2 C1 C6 119.36(18) . . ?
C6 C1 N2 123.34(18) . . ?
C1 C2 H2 119.1 . . ?
C1 C2 C3 121.75(19) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.62(19) . . ?
C4 C3 H3 120.7 . . ?
O6 C4 C3 124.38(19) . . ?
O6 C4 C5 115.61(18) . . ?
C5 C4 C3 120.01(19) . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.62(19) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C7 124.13(18) . . ?
C5 C6 C1 118.61(18) . . ?
C5 C6 C7 117.24(18) . . ?
N1 C7 C6 115.48(17) . . ?
N1 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
C6 C7 H7A 108.4 . . ?
C6 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
N1 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
N1 C8 C9 112.72(17) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
N2 C9 C8 112.51(18) . . ?
N2 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 H10C 108.0 . . ?
N2 C10 H10D 108.0 . . ?
N2 C10 C11 117.18(17) . . ?
H10C C10 H10D 107.2 . . ?
C11 C10 H10C 108.0 . . ?
C11 C10 H10D 108.0 . . ?
C12 C11 C10 123.2(2) . . ?
C12 C11 C16 119.2(2) . . ?
C16 C11 C10 117.64(19) . . ?
C11 C12 N1 123.46(19) . . ?
C13 C12 N1 117.39(19) . . ?
C13 C12 C11 119.1(2) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 118.9(2) . . ?
C15 C14 H14 120.5 . . ?
O1 C15 C14 115.1(2) . . ?
O1 C15 C16 125.0(2) . . ?
C16 C15 C14 119.9(2) . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 120.9(2) . . ?
C15 C16 H16 119.5 . . ?
O1 C17 H17C 110.3 . . ?
O1 C17 H17D 110.3 . . ?
O1 C17 C18 106.9(2) . . ?
H17C C17 H17D 108.6 . . ?
C18 C17 H17C 110.3 . . ?
C18 C17 H17D 110.3 . . ?
O2 C18 C17 113.1(2) . . ?
O2 C18 H18C 109.0 . . ?
O2 C18 H18D 109.0 . . ?
C17 C18 H18C 109.0 . . ?
C17 C18 H18D 109.0 . . ?
H18C C18 H18D 107.8 . . ?
O2 C19 H19C 109.8 . . ?
O2 C19 H19D 109.8 . . ?
O2 C19 C20 109.18(18) . . ?
H19C C19 H19D 108.3 . . ?
C20 C19 H19C 109.8 . . ?
C20 C19 H19D 109.8 . . ?
O3 C20 C19 106.43(18) . . ?
O3 C20 H20E 110.4 . . ?
O3 C20 H20F 110.4 . . ?
C19 C20 H20E 110.4 . . ?
C19 C20 H20F 110.4 . . ?
H20E C20 H20F 108.6 . . ?
O3 C21 C22 125.3(2) . . ?
O3 C21 C30 113.53(19) . . ?
C22 C21 C30 121.1(2) . . ?
C21 C22 H22 120.3 . . ?
C21 C22 C23 119.5(2) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.5(2) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.8(2) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 122.3(2) . . ?
C30 C25 C24 119.73(19) . . ?
C30 C25 C26 118.02(19) . . ?
O4 C26 C25 113.40(18) . . ?
O4 C26 C27 125.5(2) . . ?
C27 C26 C25 121.06(19) . . ?
C26 C27 H27 120.2 . . ?
C26 C27 C28 119.7(2) . . ?
C28 C27 H27 120.2 . . ?
C27 C28 H28 119.3 . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 H28 119.3 . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.3(2) . . ?
C30 C29 H29 120.4 . . ?
C25 C30 C21 118.17(19) . . ?
C29 C30 C21 121.33(19) . . ?
C29 C30 C25 120.50(19) . . ?
O4 C31 H31E 109.1 . . ?
O4 C31 H31F 109.1 . . ?
O4 C31 C32 112.5(2) . . ?
H31E C31 H31F 107.8 . . ?
C32 C31 H31E 109.1 . . ?
C32 C31 H31F 109.1 . . ?
O5 C32 C31 108.74(19) . . ?
O5 C32 H32C 109.9 . . ?
O5 C32 H32D 109.9 . . ?
C31 C32 H32C 109.9 . . ?
C31 C32 H32D 109.9 . . ?
H32C C32 H32D 108.3 . . ?
O5 C33 H33C 110.2 . . ?
O5 C33 H33D 110.2 . . ?
O5 C33 C34 107.38(19) . . ?
H33C C33 H33D 108.5 . . ?
C34 C33 H33C 110.2 . . ?
C34 C33 H33D 110.2 . . ?
O6 C34 C33 106.22(19) . . ?
O6 C34 H34C 110.5 . . ?
O6 C34 H34D 110.5 . . ?
C33 C34 H34C 110.5 . . ?
C33 C34 H34D 110.5 . . ?
H34C C34 H34D 108.7 . . ?
C15A O1A C17A 117.2(2) . . ?
C19A O2A C18A 113.9(3) . . ?
C21A O3A C20A 115.4(4) . . ?
C26B O3B C20A 121.3(7) . . ?
C26A O4A C31A 119.2(4) . . ?
C31A O4B C21B 104.8(6) . . ?
C33A O5A C32A 113.1(3) . . ?
C4A O6A C34A 118.0(2) . . ?
C7A N1A C8A 115.0(2) . . ?
C12A N1A C7A 114.08(19) . . ?
C12A N1A C8A 114.3(2) . . ?
C1A N2A C9A 115.7(2) . . ?
C1A N2A C10A 113.19(17) . . ?
C9A N2A C10A 114.8(2) . . ?
C2A C1A N2A 116.8(2) . . ?
C2A C1A C6A 119.2(2) . . ?
C6A C1A N2A 124.0(2) . . ?
C1A C2A H2A 119.1 . . ?
C3A C2A C1A 121.8(2) . . ?
C3A C2A H2A 119.1 . . ?
C2A C3A H3A 120.7 . . ?
C2A C3A C4A 118.7(2) . . ?
C4A C3A H3A 120.7 . . ?
O6A C4A C3A 114.4(2) . . ?
O6A C4A C5A 125.1(2) . . ?
C5A C4A C3A 120.5(2) . . ?
C4A C5A H5A 119.7 . . ?
C4A C5A C6A 120.6(2) . . ?
C6A C5A H5A 119.7 . . ?
C1A C6A C5A 119.2(2) . . ?
C1A C6A C7A 122.7(2) . . ?
C5A C6A C7A 118.1(2) . . ?
N1A C7A C6A 117.43(19) . . ?
N1A C7A H7AA 107.9 . . ?
N1A C7A H7AB 107.9 . . ?
C6A C7A H7AA 107.9 . . ?
C6A C7A H7AB 107.9 . . ?
H7AA C7A H7AB 107.2 . . ?
N1A C8A H8AA 109.1 . . ?
N1A C8A H8AB 109.1 . . ?
N1A C8A C9A 112.6(2) . . ?
H8AA C8A H8AB 107.8 . . ?
C9A C8A H8AA 109.1 . . ?
C9A C8A H8AB 109.1 . . ?
N2A C9A C8A 113.2(2) . . ?
N2A C9A H9AA 108.9 . . ?
N2A C9A H9AB 108.9 . . ?
C8A C9A H9AA 108.9 . . ?
C8A C9A H9AB 108.9 . . ?
H9AA C9A H9AB 107.7 . . ?
N2A C10A H10A 108.1 . . ?
N2A C10A H10B 108.1 . . ?
N2A C10A C11A 116.73(19) . . ?
H10A C10A H10B 107.3 . . ?
C11A C10A H10A 108.1 . . ?
C11A C10A H10B 108.1 . . ?
C12A C11A C10A 123.7(2) . . ?
C16A C11A C10A 117.5(2) . . ?
C16A C11A C12A 118.8(2) . . ?
C11A C12A N1A 123.4(2) . . ?
C13A C12A N1A 117.4(2) . . ?
C13A C12A C11A 119.2(2) . . ?
C12A C13A H13A 119.2 . . ?
C14A C13A C12A 121.5(2) . . ?
C14A C13A H13A 119.2 . . ?
C13A C14A H14A 120.4 . . ?
C15A C14A C13A 119.2(2) . . ?
C15A C14A H14A 120.4 . . ?
O1A C15A C14A 124.5(2) . . ?
O1A C15A C16A 115.7(2) . . ?
C14A C15A C16A 119.8(2) . . ?
C11A C16A C15A 121.5(2) . . ?
C11A C16A H16A 119.3 . . ?
C15A C16A H16A 119.3 . . ?
O1A C17A H17A 110.3 . . ?
O1A C17A H17B 110.3 . . ?
O1A C17A C18A 107.0(2) . . ?
H17A C17A H17B 108.6 . . ?
C18A C17A H17A 110.3 . . ?
C18A C17A H17B 110.3 . . ?
O2A C18A C17A 109.4(3) . . ?
O2A C18A H18A 109.8 . . ?
O2A C18A H18B 109.8 . . ?
C17A C18A H18A 109.8 . . ?
C17A C18A H18B 109.8 . . ?
H18A C18A H18B 108.2 . . ?
O2A C19A H19A 110.3 . . ?
O2A C19A H19B 110.3 . . ?
O2A C19A C20A 107.1(4) . . ?
H19A C19A H19B 108.6 . . ?
C20A C19A H19A 110.3 . . ?
C20A C19A H19B 110.3 . . ?
O3A C20A H20A 110.7 . . ?
O3A C20A H20B 110.7 . . ?
O3B C20A H20C 104.5 . . ?
O3B C20A H20D 104.5 . . ?
C19A C20A O3A 105.4(4) . . ?
C19A C20A O3B 131.0(5) . . ?
C19A C20A H20A 110.7 . . ?
C19A C20A H20B 110.7 . . ?
C19A C20A H20C 104.5 . . ?
C19A C20A H20D 104.5 . . ?
H20A C20A H20B 108.8 . . ?
H20C C20A H20D 105.7 . . ?
O3A C21A C22A 123.6(5) . . ?
O3A C21A C30A 115.2(4) . . ?
C22A C21A C30A 121.2(5) . . ?
O4B C21B C22B 127.0(10) . . ?
O4B C21B C30B 114.3(7) . . ?
C22B C21B C30B 118.7(10) . . ?
C21A C22A H22A 120.7 . . ?
C21A C22A C23A 118.5(5) . . ?
C23A C22A H22A 120.7 . . ?
C21B C22B H22B 119.4 . . ?
C21B C22B C23B 121.2(13) . . ?
C23B C22B H22B 119.4 . . ?
C22A C23A H23A 118.8 . . ?
C24A C23A C22A 122.4(5) . . ?
C24A C23A H23A 118.8 . . ?
C22B C23B H23B 119.0 . . ?
C24B C23B C22B 122.1(13) . . ?
C24B C23B H23B 119.0 . . ?
C23A C24A H24A 119.9 . . ?
C23A C24A C25A 120.2(5) . . ?
C25A C24A H24A 119.9 . . ?
C23B C24B H24B 120.4 . . ?
C23B C24B C25B 119.1(13) . . ?
C25B C24B H24B 120.4 . . ?
C26A C25A C24A 122.8(5) . . ?
C26A C25A C30A 119.1(4) . . ?
C30A C25A C24A 118.1(5) . . ?
C26B C25B C24B 123.2(11) . . ?
C30B C25B C24B 119.3(13) . . ?
C30B C25B C26B 117.4(11) . . ?
O4A C26A C25A 119.0(4) . . ?
O4A C26A C27A 119.2(5) . . ?
C27A C26A C25A 121.5(4) . . ?
O3B C26B C25B 114.8(11) . . ?
C27B C26B O3B 122.4(11) . . ?
C27B C26B C25B 122.5(9) . . ?
C26A C27A H27A 120.5 . . ?
C26A C27A C28A 119.0(4) . . ?
C28A C27A H27A 120.5 . . ?
C26B C27B H27B 120.9 . . ?
C26B C27B C28B 118.2(9) . . ?
C28B C27B H27B 120.9 . . ?
C27A C28A H28A 119.2 . . ?
C29A C28A C27A 121.5(4) . . ?
C29A C28A H28A 119.2 . . ?
C27B C28B H28B 119.1 . . ?
C29B C28B C27B 121.7(9) . . ?
C29B C28B H28B 119.1 . . ?
C28A C29A H29A 119.9 . . ?
C28A C29A C30A 120.2(4) . . ?
C30A C29A H29A 119.9 . . ?
C28B C29B H29B 120.1 . . ?
C28B C29B C30B 119.9(8) . . ?
C30B C29B H29B 120.1 . . ?
C21A C30A C29A 121.7(4) . . ?
C25A C30A C21A 119.6(4) . . ?
C25A C30A C29A 118.7(5) . . ?
C25B C30B C21B 119.5(10) . . ?
C25B C30B C29B 120.2(10) . . ?
C29B C30B C21B 120.3(8) . . ?
O4A C31A H31A 107.2 . . ?
O4A C31A H31B 107.2 . . ?
O4B C31A H31C 113.6 . . ?
O4B C31A H31D 113.6 . . ?
O4B C31A C32A 90.4(4) . . ?
H31A C31A H31B 106.8 . . ?
H31C C31A H31D 110.8 . . ?
C32A C31A O4A 120.6(3) . . ?
C32A C31A H31A 107.2 . . ?
C32A C31A H31B 107.2 . . ?
C32A C31A H31C 113.6 . . ?
C32A C31A H31D 113.6 . . ?
O5A C32A C31A 113.2(3) . . ?
O5A C32A H32A 108.9 . . ?
O5A C32A H32B 108.9 . . ?
C31A C32A H32A 108.9 . . ?
C31A C32A H32B 108.9 . . ?
H32A C32A H32B 107.7 . . ?
O5A C33A H33A 108.5 . . ?
O5A C33A H33B 108.5 . . ?
O5A C33A C34A 115.3(3) . . ?
H33A C33A H33B 107.5 . . ?
C34A C33A H33A 108.5 . . ?
C34A C33A H33B 108.5 . . ?
O6A C34A C33A 106.3(3) . . ?
O6A C34A H34A 110.5 . . ?
O6A C34A H34B 110.5 . . ?
C33A C34A H34A 110.5 . . ?
C33A C34A H34B 110.5 . . ?
H34A C34A H34B 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C15 C16 C11 176.0(2) . . . . ?
O1 C17 C18 O2 -60.0(3) . . . . ?
O2 C19 C20 O3 -70.0(2) . . . . ?
O3 C21 C22 C23 178.2(2) . . . . ?
O3 C21 C30 C25 -176.58(18) . . . . ?
O3 C21 C30 C29 3.3(3) . . . . ?
O4 C26 C27 C28 -178.0(2) . . . . ?
O4 C31 C32 O5 67.8(3) . . . . ?
O5 C33 C34 O6 63.7(3) . . . . ?
O6 C4 C5 C6 179.93(19) . . . . ?
N1 C8 C9 N2 40.2(3) . . . . ?
N1 C12 C13 C14 174.9(2) . . . . ?
N2 C1 C2 C3 178.38(19) . . . . ?
N2 C1 C6 C5 -177.16(19) . . . . ?
N2 C1 C6 C7 4.0(3) . . . . ?
N2 C10 C11 C12 25.7(3) . . . . ?
N2 C10 C11 C16 -155.56(19) . . . . ?
C1 N2 C9 C8 -87.0(2) . . . . ?
C1 N2 C10 C11 55.0(2) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C1 C6 C7 N1 26.9(3) . . . . ?
C2 C1 C6 C5 1.8(3) . . . . ?
C2 C1 C6 C7 -177.1(2) . . . . ?
C2 C3 C4 O6 -178.7(2) . . . . ?
C2 C3 C4 C5 1.1(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 O6 C34 C33 -158.39(19) . . . . ?
C4 C5 C6 C1 -1.6(3) . . . . ?
C4 C5 C6 C7 177.4(2) . . . . ?
C5 C6 C7 N1 -152.02(19) . . . . ?
C6 C1 C2 C3 -0.6(3) . . . . ?
C7 N1 C8 C9 49.3(3) . . . . ?
C7 N1 C12 C11 -97.2(2) . . . . ?
C7 N1 C12 C13 84.8(2) . . . . ?
C8 N1 C7 C6 -81.9(2) . . . . ?
C8 N1 C12 C11 39.2(3) . . . . ?
C8 N1 C12 C13 -138.8(2) . . . . ?
C9 N2 C1 C2 -140.3(2) . . . . ?
C9 N2 C1 C6 38.7(3) . . . . ?
C9 N2 C10 C11 -80.2(2) . . . . ?
C10 N2 C1 C2 84.9(2) . . . . ?
C10 N2 C1 C6 -96.1(2) . . . . ?
C10 N2 C9 C8 47.9(2) . . . . ?
C10 C11 C12 N1 4.7(3) . . . . ?
C10 C11 C12 C13 -177.27(19) . . . . ?
C10 C11 C16 C15 180.0(2) . . . . ?
C11 C12 C13 C14 -3.2(3) . . . . ?
C12 N1 C7 C6 55.2(2) . . . . ?
C12 N1 C8 C9 -87.7(2) . . . . ?
C12 C11 C16 C15 -1.2(3) . . . . ?
C12 C13 C14 C15 -0.4(4) . . . . ?
C13 C14 C15 O1 -175.4(2) . . . . ?
C13 C14 C15 C16 3.2(4) . . . . ?
C14 C15 C16 C11 -2.4(3) . . . . ?
C15 O1 C17 C18 -179.7(2) . . . . ?
C16 C11 C12 N1 -174.05(19) . . . . ?
C16 C11 C12 C13 4.0(3) . . . . ?
C17 O1 C15 C14 179.0(2) . . . . ?
C17 O1 C15 C16 0.6(3) . . . . ?
C18 O2 C19 C20 162.54(18) . . . . ?
C19 O2 C18 C17 -75.1(2) . . . . ?
C20 O3 C21 C22 -13.0(3) . . . . ?
C20 O3 C21 C30 167.11(19) . . . . ?
C21 O3 C20 C19 -164.54(19) . . . . ?
C21 C22 C23 C24 -0.5(4) . . . . ?
C22 C21 C30 C25 3.5(3) . . . . ?
C22 C21 C30 C29 -176.6(2) . . . . ?
C22 C23 C24 C25 1.3(3) . . . . ?
C23 C24 C25 C26 180.0(2) . . . . ?
C23 C24 C25 C30 0.4(3) . . . . ?
C24 C25 C26 O4 0.6(3) . . . . ?
C24 C25 C26 C27 -179.4(2) . . . . ?
C24 C25 C30 C21 -2.7(3) . . . . ?
C24 C25 C30 C29 177.4(2) . . . . ?
C25 C26 C27 C28 2.0(3) . . . . ?
C26 O4 C31 C32 -93.3(2) . . . . ?
C26 C25 C30 C21 177.71(19) . . . . ?
C26 C25 C30 C29 -2.2(3) . . . . ?
C26 C27 C28 C29 -2.1(3) . . . . ?
C27 C28 C29 C30 0.1(3) . . . . ?
C28 C29 C30 C21 -177.8(2) . . . . ?
C28 C29 C30 C25 2.1(3) . . . . ?
C30 C21 C22 C23 -1.9(3) . . . . ?
C30 C25 C26 O4 -179.84(18) . . . . ?
C30 C25 C26 C27 0.2(3) . . . . ?
C31 O4 C26 C25 -175.01(19) . . . . ?
C31 O4 C26 C27 5.0(3) . . . . ?
C32 O5 C33 C34 -176.9(2) . . . . ?
C33 O5 C32 C31 169.6(2) . . . . ?
C34 O6 C4 C3 -19.3(3) . . . . ?
C34 O6 C4 C5 160.9(2) . . . . ?
O1A C15A C16A C11A 179.8(2) . . . . ?
O1A C17A C18A O2A -68.7(3) . . . . ?
O2A C19A C20A O3A 67.8(4) . . . . ?
O2A C19A C20A O3B 89.7(6) . . . . ?
O3A C21A C22A C23A -178.2(4) . . . . ?
O3A C21A C30A C25A 178.4(4) . . . . ?
O3A C21A C30A C29A -1.7(6) . . . . ?
O3B C26B C27B C28B 171.8(7) . . . . ?
O4A C26A C27A C28A -173.7(4) . . . . ?
O4A C31A C32A O5A 50.8(6) . . . . ?
O4B C21B C22B C23B -178.7(8) . . . . ?
O4B C21B C30B C25B 178.5(7) . . . . ?
O4B C21B C30B C29B -3.1(10) . . . . ?
O4B C31A C32A O5A 77.7(5) . . . . ?
O5A C33A C34A O6A 60.7(4) . . . . ?
O6A C4A C5A C6A -179.9(2) . . . . ?
N1A C8A C9A N2A -40.6(3) . . . . ?
N1A C12A C13A C14A -179.6(2) . . . . ?
N2A C1A C2A C3A 179.9(2) . . . . ?
N2A C1A C6A C5A 179.58(19) . . . . ?
N2A C1A C6A C7A 0.9(3) . . . . ?
N2A C10A C11A C12A -29.0(3) . . . . ?
N2A C10A C11A C16A 151.9(2) . . . . ?
C1A N2A C9A C8A 87.3(3) . . . . ?
C1A N2A C10A C11A -55.7(3) . . . . ?
C1A C2A C3A C4A 0.5(3) . . . . ?
C1A C6A C7A N1A -30.0(3) . . . . ?
C2A C1A C6A C5A -0.4(3) . . . . ?
C2A C1A C6A C7A -179.1(2) . . . . ?
C2A C3A C4A O6A 179.5(2) . . . . ?
C2A C3A C4A C5A -0.4(3) . . . . ?
C3A C4A C5A C6A 0.0(3) . . . . ?
C4A O6A C34A C33A -170.0(3) . . . . ?
C4A C5A C6A C1A 0.5(3) . . . . ?
C4A C5A C6A C7A 179.2(2) . . . . ?
C5A C6A C7A N1A 151.3(2) . . . . ?
C6A C1A C2A C3A -0.1(3) . . . . ?
C7A N1A C8A C9A -46.4(3) . . . . ?
C7A N1A C12A C11A 91.6(3) . . . . ?
C7A N1A C12A C13A -88.8(3) . . . . ?
C8A N1A C7A C6A 80.5(3) . . . . ?
C8A N1A C12A C11A -43.6(3) . . . . ?
C8A N1A C12A C13A 136.0(2) . . . . ?
C9A N2A C1A C2A 138.0(2) . . . . ?
C9A N2A C1A C6A -42.0(3) . . . . ?
C9A N2A C10A C11A 80.2(3) . . . . ?
C10A N2A C1A C2A -86.6(2) . . . . ?
C10A N2A C1A C6A 93.5(2) . . . . ?
C10A N2A C9A C8A -47.5(3) . . . . ?
C10A C11A C12A N1A 1.6(4) . . . . ?
C10A C11A C12A C13A -178.0(2) . . . . ?
C10A C11A C16A C15A 177.8(2) . . . . ?
C11A C12A C13A C14A 0.0(4) . . . . ?
C12A N1A C7A C6A -54.4(3) . . . . ?
C12A N1A C8A C9A 88.4(3) . . . . ?
C12A C11A C16A C15A -1.3(3) . . . . ?
C12A C13A C14A C15A -0.9(4) . . . . ?
C13A C14A C15A O1A -178.6(2) . . . . ?
C13A C14A C15A C16A 0.7(3) . . . . ?
C14A C15A C16A C11A 0.4(3) . . . . ?
C15A O1A C17A C18A -172.3(2) . . . . ?
C16A C11A C12A N1A -179.3(2) . . . . ?
C16A C11A C12A C13A 1.1(3) . . . . ?
C17A O1A C15A C14A -15.2(3) . . . . ?
C17A O1A C15A C16A 165.4(2) . . . . ?
C18A O2A C19A C20A -169.3(3) . . . . ?
C19A O2A C18A C17A 136.0(3) . . . . ?
C20A O3A C21A C22A -18.4(6) . . . . ?
C20A O3A C21A C30A 163.2(4) . . . . ?
C20A O3B C26B C25B -113.1(10) . . . . ?
C20A O3B C26B C27B 72.5(10) . . . . ?
C21A O3A C20A C19A -153.6(4) . . . . ?
C21A C22A C23A C24A 0.7(7) . . . . ?
C21B O4B C31A C32A 162.7(5) . . . . ?
C21B C22B C23B C24B -0.8(15) . . . . ?
C22A C21A C30A C25A 0.0(6) . . . . ?
C22A C21A C30A C29A 179.8(4) . . . . ?
C22A C23A C24A C25A -1.6(8) . . . . ?
C22B C21B C30B C25B -1.8(11) . . . . ?
C22B C21B C30B C29B 176.6(7) . . . . ?
C22B C23B C24B C25B 0.1(16) . . . . ?
C23A C24A C25A C26A 179.3(5) . . . . ?
C23A C24A C25A C30A 1.6(7) . . . . ?
C23B C24B C25B C26B 179.8(9) . . . . ?
C23B C24B C25B C30B -0.3(14) . . . . ?
C24A C25A C26A O4A -5.1(6) . . . . ?
C24A C25A C26A C27A -178.7(4) . . . . ?
C24A C25A C30A C21A -0.8(6) . . . . ?
C24A C25A C30A C29A 179.3(4) . . . . ?
C24B C25B C26B O3B 5.5(12) . . . . ?
C24B C25B C26B C27B 179.8(8) . . . . ?
C24B C25B C30B C21B 1.2(11) . . . . ?
C24B C25B C30B C29B -177.3(7) . . . . ?
C25A C26A C27A C28A -0.1(6) . . . . ?
C25B C26B C27B C28B -2.1(11) . . . . ?
C26A O4A C31A C32A 75.3(6) . . . . ?
C26A C25A C30A C21A -178.6(4) . . . . ?
C26A C25A C30A C29A 1.5(6) . . . . ?
C26A C27A C28A C29A 0.6(6) . . . . ?
C26B O3B C20A C19A -63.4(11) . . . . ?
C26B C25B C30B C21B -178.9(7) . . . . ?
C26B C25B C30B C29B 2.6(11) . . . . ?
C26B C27B C28B C29B 1.8(11) . . . . ?
C27A C28A C29A C30A -0.1(6) . . . . ?
C27B C28B C29B C30B 0.7(11) . . . . ?
C28A C29A C30A C21A 179.2(4) . . . . ?
C28A C29A C30A C25A -1.0(6) . . . . ?
C28B C29B C30B C21B 178.6(7) . . . . ?
C28B C29B C30B C25B -3.0(10) . . . . ?
C30A C21A C22A C23A 0.1(7) . . . . ?
C30A C25A C26A O4A 172.6(4) . . . . ?
C30A C25A C26A C27A -1.0(6) . . . . ?
C30B C21B C22B C23B 1.7(12) . . . . ?
C30B C25B C26B O3B -174.4(7) . . . . ?
C30B C25B C26B C27B -0.1(12) . . . . ?
C31A O4A C26A C25A 102.9(5) . . . . ?
C31A O4A C26A C27A -83.3(5) . . . . ?
C31A O4B C21B C22B 13.7(10) . . . . ?
C31A O4B C21B C30B -166.6(5) . . . . ?
C32A O5A C33A C34A 76.2(4) . . . . ?
C33A O5A C32A C31A -173.7(3) . . . . ?
C34A O6A C4A C3A 172.1(2) . . . . ?
C34A O6A C4A C5A -8.0(4) . . . . ?

_olex2_date_sample_data_collection 2021-06-02
_olex2_date_sample_submission    2021-06-02
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder With Paratone oil'
_olex2_submission_original_sample_id MR518
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.869
####################################################################### 
# 
# 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_MR572S
_database_code_depnum_ccdc_archive 'CCDC 2127780'
loop_
_audit_author_name
_audit_author_address
'Masoud Kazem-Rostami'
;Northwestern University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_audit_creation_date             2021-12-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            'SS-TBDR34C6 . BlueBox . 4PF6'
_chemical_name_systematic        
'(2S,4aR,5S,6aS,22S,25aS,26S)-dodecahydro-1H,6H-2,8-(epoxyethanooxyethanooxy[1,5]naphthalenooxyethanooxyethanooxy)-5,11-ethanodibenzo[b,f][1,5]diazocine.1,2,7(4,1),6(1,4)-tetrapyridin-1-iuma-4,9(1,4)-dibenzenacyclodecaphane-11,21,61,71-tetraium.tetrakis hexafluorophosphate'
_chemical_formula_moiety         'C36 H32 N4, C34 H37 N2 O6, 4(F6 P)'
_chemical_formula_sum            'C70 H69 F24 N6 O6 P4'
_chemical_formula_weight         1670.19
_chemical_absolute_configuration syn
_chemical_melting_point          NA
_chemical_oxdiff_formula         C71H12$N6O6P4F24
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.1062(3)
_cell_length_b                   25.2825(7)
_cell_length_c                   24.5285(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.980(3)
_cell_angle_gamma                90
_cell_volume                     8742.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24933
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      75.0340
_cell_measurement_theta_min      3.4800
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.811
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Maroon
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3420
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0615
0 -1 0 0.0635
1 0 0 0.0910
-1 0 0 0.0380
0 0 -1 0.0093
0 0 1 0.0010

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeCN / H2O'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.01
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0005 1.0002 -0.0002 -0.0235 0.0533 -0.0178
0.0005 -1.0002 0.0002 0.0235 -0.0533 0.0178
0.9995 0.0009 -0.0001 0.0201 -0.0260 -0.1042
-0.9995 -0.0009 0.0001 -0.0201 0.0260 0.1042
0.0002 0.0004 -1.0004 -0.0572 -0.0260 -0.0023
-0.0002 -0.0004 1.0004 0.0572 0.0260 0.0023

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103015
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.496
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00   7.00   0.50   15.00    --  -47.48 102.00 165.00  162
  2  ω     15.00  82.00   0.50   15.00    --   47.48-102.00  61.00  134
  3  ω    -14.00  12.00   0.50   15.00    --   47.48-102.00  61.00   52
  4  ω   -121.00 -95.00   0.50   50.00    -- -106.00-102.00  61.00   52
  5  ω   -174.00-134.00   0.50   50.00    -- -106.00-102.00  61.00   80
  6  ω     69.00 105.00   0.50   50.00    --  113.25-102.00  61.00   72
  7  ω    -21.00  12.00   0.50   15.00    --  -47.48  19.00  60.00   66
  8  ω   -117.00 -73.00   0.50   15.00    --  -47.48-125.00-150.00   88
  9  ω   -109.00 -79.00   0.50   15.00    --  -47.48-125.00-120.00   60
 10  ω   -108.00 -77.00   0.50   15.00    --  -47.48-125.00 -60.00   62
 11  ω    -40.00 -14.00   0.50   15.00    --  -47.48  37.00  60.00   52
 12  ω     -4.00  22.00   0.50   15.00    --  -47.48  37.00  60.00   52
 13  ω    -20.00  28.00   0.50   15.00    --  -47.48  19.00-150.00   96
 14  ω    -27.00  14.00   0.50   15.00    --   47.48 -19.00  60.00   82
 15  ω    -19.00  58.00   0.50   15.00    --   47.48 -57.00 120.00  154
 16  ω    -27.00  17.00   0.50   15.00    --   47.48 -19.00 -90.00   88
 17  ω    -71.00 -34.00   0.50   50.00    -- -106.00  61.00 120.00   74
 18  ω    -71.00 -36.00   0.50   50.00    -- -106.00  61.00 -30.00   70
 19  ω    -74.00 -49.00   0.50   50.00    -- -106.00  61.00  30.00   50
 20  ω   -112.00 -38.00   0.50   50.00    -- -106.00 125.00 -30.00  148
 21  ω    -66.00 -40.00   0.50   50.00    -- -106.00  61.00 -60.00   52
 22  ω    -70.00 -35.00   0.50   50.00    -- -106.00 111.00  91.45   70
 23  ω   -105.00 -76.00   0.50   50.00    -- -106.00 102.00 165.00   58
 24  ω   -174.00 -87.00   0.50   50.00    -- -106.00 -77.00 -60.00  174
 25  ω   -176.00-119.00   0.50   50.00    -- -106.00 -45.00   0.00  114
 26  ω   -110.00 -33.00   0.50   50.00    -- -106.00 125.00  90.00  154
 27  ω    -72.00 -47.00   0.50   50.00    -- -106.00  61.00   0.00   50
 28  ω    -73.00 -34.00   0.50   50.00    -- -106.00 125.00 -60.00   78
 29  ω   -112.00 -86.00   0.50   50.00    -- -106.00 125.00 -60.00   52
 30  ω   -175.00-118.00   0.50   50.00    -- -106.00 -45.00 -30.00  114
 31  ω   -108.00 -83.00   0.50   50.00    -- -106.00 111.00  91.45   50
 32  ω     43.00  68.00   0.50   50.00    --  113.25 -61.00 -90.00   50
 33  ω    101.00 178.00   0.50   50.00    --  113.25  61.00   0.00  154
 34  ω     46.00  92.00   0.50   50.00    --  113.25-125.00-150.00   92
 35  ω    101.00 178.00   0.50   50.00    --  113.25  30.00-120.00  154
 36  ω     42.00  67.00   0.50   50.00    --  113.25 -61.00  60.00   50
 37  ω     85.00 111.00   0.50   50.00    --  113.25-125.00 -90.00   52
 38  ω     43.00  70.00   0.50   50.00    --  113.25 -61.00-150.00   54
 39  ω     46.00  71.00   0.50   50.00    --  113.25 -61.00 150.00   50
 40  ω     62.00 106.00   0.50   50.00    --  113.25 -94.00-120.00   88
 41  ω    152.00 177.00   0.50   50.00    --  113.25   0.00 -30.00   50
 42  ω    120.00 178.00   0.50   50.00    --  113.25  15.00 120.00  116
 43  ω     51.00  96.00   0.50   50.00    --  113.25-125.00 120.00   90
 44  ω    122.00 174.00   0.50   50.00    --  113.25   0.00-180.00  104
 45  ω    130.00 171.00   0.50   50.00    --  113.25 102.00 165.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0201810000
_diffrn_orient_matrix_UB_12      -0.0235112000
_diffrn_orient_matrix_UB_13      0.0571676000
_diffrn_orient_matrix_UB_21      -0.0260718000
_diffrn_orient_matrix_UB_22      0.0532886000
_diffrn_orient_matrix_UB_23      0.0260084000
_diffrn_orient_matrix_UB_31      -0.1041996000
_diffrn_orient_matrix_UB_32      -0.0178923000
_diffrn_orient_matrix_UB_33      0.0022268000
_diffrn_oxdiff_digest_frames     
;
01bcb40ea145faa98cb380e7e08a5aea0203846f9c9
;
_diffrn_oxdiff_digest_hkl        
;
0158d5d13e5c947cf2a85aafc853d4494c30f4
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                22932
_reflns_number_total             31872
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 
;
 Flack x determined using 7435 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.21(2)
_refine_ls_extinction_coef       0.0032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1982
_refine_ls_number_reflns         31872
_refine_ls_number_restraints     2600
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.1291
_refine_ls_restrained_S_all      1.255
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3292
_refine_ls_wR_factor_ref         0.3460
_refine_special_details          
;
The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied globally. (Acta Cryst. A68 (2012) 448-451).  Distant restraints were imposed on the disordered PF6 anions and some ring and chain atoms.  
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.Total solvent accessible volume / cell = 2384.2 Ang³[27.3%]
Total electron count / cell = 752.8
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 F37-F41 \\sim F37-F39 \\sim F37-F40 \\sim F37-F42 \\sim F41-F40 \\sim F41-F42
\\sim F41-F38 \\sim F39-F40
 \\sim F39-F42 \\sim F39-F38 \\sim F42-F38
 with sigma of 0.02
 P7-F37 \\sim P7-F41 \\sim P7-F39 \\sim P7-F40 \\sim P7-F42 \\sim P7-F38
 with sigma of 0.01
 F26-F28 \\sim F26-F29 \\sim F26-F30 \\sim F26-F27 \\sim F25-F28 \\sim F25-F29
\\sim F25-F30 \\sim F25-F27
 \\sim F28-F29 \\sim F28-F27 \\sim F29-F30 \\sim F30-F27
 with sigma of 0.02
 P5-F26 \\sim P5-F25 \\sim P5-F28 \\sim P5-F29 \\sim P5-F30 \\sim P5-F27
 with sigma of 0.01
 F36-F32 \\sim F36-F35 \\sim F36-F31 \\sim F36-F33 \\sim F34-F32 \\sim F34-F35
\\sim F34-F31 \\sim F34-F33
 \\sim F32-F35 \\sim F32-F33 \\sim F35-F31
 with sigma of 0.02
 P6-F36 \\sim P6-F34 \\sim P6-F32 \\sim P6-F35 \\sim P6-F31 \\sim P6-F33
 with sigma of 0.01
 N6A-C45A \\sim N5A-C44A \\sim N6-C46 \\sim N6-C45 \\sim N5-C44 \\sim N5-C48
\\sim N5-C43 \\sim N6-C40 ~
 N5A-C48A \\sim N5A-C43A \\sim N6A-C40A \\sim N6A-C46A
 with sigma of 0.01
 C38-C37 \\sim C39-C38 \\sim C40-C39 \\sim C41-C40 \\sim C42-C41 \\sim C42-C37
 with sigma of 0.01
 O2A-C55A \\sim O3A-C56A \\sim O2A-C54A \\sim O1A-C53A \\sim O6A-C37A \\sim
O6A-C70A \\sim O5A-C69A ~
 O5A-C68A \\sim O1-C51 \\sim O1-C53 \\sim O2-C54 \\sim O2-C55 \\sim O3-C56
\\sim O3-C57 \\sim O4-C62 \\sim O4-
 C67 \\sim O5-C68 \\sim O5-C69 \\sim O6-C70 \\sim O6-C37
 with sigma of 0.01
 C70A-C69A \\sim C68A-C67A \\sim C56A-C55A \\sim C54A-C53A \\sim C56-C55 \\sim
C68-C67 \\sim C70-C69 ~
 C54-C53
 with sigma of 0.01
 C6A-C5A \\sim C5A-C4A \\sim C4A-C3A \\sim C3A-C2A \\sim C11A-C10A \\sim
C7A-C11A \\sim C8A-C7A \\sim C9A-
 C8A \\sim C24A-C23A \\sim C23A-C22A \\sim C22A-C21A \\sim C21A-C20A \\sim
C29A-C28A \\sim C29A-C25A ~
 C26A-C25A \\sim C27A-C26A \\sim C50A-C49A \\sim C49A-C48A \\sim C48A-C47A
\\sim C52A-C47A \\sim C52A-
 C51A \\sim C51A-C50A
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 N6(H6), N5A(H5A)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C19(H19A,H19B), C30(H30A,H30B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C53(H53A,H53B), C54(H54A,H54B),
  C55(H55A,H55B), C56(H56A,H56B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,
 H69B), C70(H70A,H70B), C1A(H1AA,H1AB), C12A(H12C,H12D), C19A(H19C,H19D),
 C30A(H30C,H30D), C43A(H43C,H43D), C44A(H44C,H44D), C45A(H45C,H45D), C46A(H46C,
 H46D), C53A(H53C,H53D), C54A(H54C,H54D), C55A(H55C,H55D), C56A(H56C,H56D),
 C67A(H67C,H67D), C68A(H68C,H68D), C69A(H69C,H69D), C70A(H70C,H70D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6A), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
  C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
 C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C35(H35), C36(H36),
  C38(H38), C41(H41), C42(H42), C49(H49), C50(H50), C52(H52), C58(H58),
 C59(H59), C60(H60), C63(H63), C64(H64), C65(H65), C2A(H2A), C3A(H3A),
 C5A(H5AA), C6A(H6AA), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C14A(H14A),
 C15A(H15A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C23A(H23A),
 C24A(H24A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C32A(H32A),
 C33A(H33A), C35A(H35A), C36A(H36A), C38A(H38A), C41A(H41A), C42A(H42A),
 C49A(H49A), C50A(H50A), C52A(H52A), C58A(H58A), C59A(H59A), C60A(H60A),
 C63A(H63A), C64A(H64A), C65A(H65A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.0943(6) 0.5134(4) 0.5190(5) 0.079(2) Uani 1 1 d . U . . .
N2 N 0.6221(7) 0.5672(3) 0.5589(3) 0.0629(19) Uani 1 1 d . U . . .
N3 N 0.4986(7) 0.3402(6) 0.4623(4) 0.085(3) Uani 1 1 d . U . . .
N4 N 0.9785(6) 0.2860(4) 0.4239(5) 0.077(2) Uani 1 1 d . U . . .
C1 C 1.1891(7) 0.4897(5) 0.5031(9) 0.103(5) Uani 1 1 d . U . . .
H1A H 1.214250 0.510614 0.473219 0.124 Uiso 1 1 calc R . . . .
H1B H 1.234132 0.492391 0.534262 0.124 Uiso 1 1 calc R . . . .
C2 C 1.0472(9) 0.5420(6) 0.4820(7) 0.086(3) Uani 1 1 d . U . . .
H2 H 1.076237 0.554060 0.450423 0.103 Uiso 1 1 calc R . . . .
C3 C 0.9531(9) 0.5535(4) 0.4918(6) 0.080(3) Uani 1 1 d . U . . .
H3 H 0.917361 0.571085 0.464252 0.096 Uiso 1 1 calc R . . . .
C4 C 0.9121(6) 0.5419(4) 0.5357(5) 0.064(2) Uani 1 1 d . U . . .
C5 C 0.9647(8) 0.5164(5) 0.5754(5) 0.073(3) Uani 1 1 d . U . . .
H5 H 0.936631 0.509519 0.608884 0.087 Uiso 1 1 calc R . . . .
C6 C 1.0549(11) 0.5007(5) 0.5689(6) 0.088(3) Uani 1 1 d . U . . .
H6A H 1.089363 0.482354 0.596393 0.106 Uiso 1 1 calc R . . . .
C7 C 0.8134(8) 0.5556(5) 0.5437(4) 0.067(3) Uani 1 1 d . U . . .
C8 C 0.7488(7) 0.5725(3) 0.5008(4) 0.056(2) Uani 1 1 d . U . . .
H8 H 0.771937 0.582730 0.466873 0.068 Uiso 1 1 calc R . . . .
C9 C 0.6584(8) 0.5737(5) 0.5087(5) 0.068(2) Uani 1 1 d . U . . .
H9 H 0.616462 0.579193 0.478589 0.081 Uiso 1 1 calc R . . . .
C10 C 0.6739(7) 0.5542(5) 0.6021(4) 0.066(2) Uani 1 1 d . U . . .
H10 H 0.646935 0.548190 0.636094 0.079 Uiso 1 1 calc R . . . .
C11 C 0.7723(6) 0.5498(3) 0.5951(4) 0.0501(18) Uani 1 1 d . U . . .
H11 H 0.812127 0.542800 0.625712 0.060 Uiso 1 1 calc R . . . .
C12 C 0.5086(7) 0.5677(5) 0.5657(6) 0.076(3) Uani 1 1 d . U . . .
H12A H 0.494386 0.568326 0.604562 0.091 Uiso 1 1 calc R . . . .
H12B H 0.481398 0.599553 0.548652 0.091 Uiso 1 1 calc R . . . .
C13 C 0.4644(7) 0.5185(5) 0.5389(5) 0.071(2) Uani 1 1 d . U . . .
C14 C 0.4434(7) 0.5148(4) 0.4881(5) 0.066(2) Uani 1 1 d . U . . .
H14 H 0.443720 0.544753 0.465430 0.079 Uiso 1 1 calc R . . . .
C15 C 0.4193(7) 0.4634(4) 0.4665(4) 0.061(2) Uani 1 1 d . U . . .
H15 H 0.400949 0.459103 0.429570 0.073 Uiso 1 1 calc R . . . .
C16 C 0.4238(11) 0.4216(5) 0.5005(5) 0.081(3) Uani 1 1 d . U . . .
C17 C 0.4446(8) 0.4280(4) 0.5558(5) 0.071(2) Uani 1 1 d . U . . .
H17 H 0.446809 0.398112 0.578511 0.085 Uiso 1 1 calc R . . . .
C18 C 0.4627(9) 0.4794(6) 0.5792(7) 0.094(4) Uani 1 1 d . U . . .
H18 H 0.472288 0.485818 0.616689 0.113 Uiso 1 1 calc R . . . .
C19 C 0.4043(8) 0.3668(4) 0.4783(5) 0.072(3) Uani 1 1 d . U . . .
H19A H 0.361152 0.369080 0.446189 0.086 Uiso 1 1 calc R . . . .
H19B H 0.373670 0.345355 0.505924 0.086 Uiso 1 1 calc R . . . .
C20 C 0.5431(8) 0.3561(5) 0.4197(6) 0.077(3) Uani 1 1 d . U . . .
H20 H 0.509833 0.378439 0.395116 0.092 Uiso 1 1 calc R . . . .
C21 C 0.6306(8) 0.3435(4) 0.4080(5) 0.066(2) Uani 1 1 d . U . . .
H21 H 0.660364 0.357174 0.377310 0.079 Uiso 1 1 calc R . . . .
C22 C 0.6752(9) 0.3094(6) 0.4434(5) 0.078(3) Uani 1 1 d . U . . .
C23 C 0.6369(9) 0.2924(7) 0.4909(6) 0.095(4) Uani 1 1 d . U . . .
H23 H 0.670135 0.270116 0.515587 0.114 Uiso 1 1 calc R . . . .
C24 C 0.5417(8) 0.3110(5) 0.5006(6) 0.076(3) Uani 1 1 d . U . . .
H24 H 0.511417 0.302530 0.533054 0.091 Uiso 1 1 calc R . . . .
C25 C 0.7792(8) 0.2971(5) 0.4353(4) 0.068(2) Uani 1 1 d . U . . .
C26 C 0.8278(8) 0.3004(6) 0.3826(5) 0.077(3) Uani 1 1 d . U . . .
H26 H 0.789360 0.306234 0.351095 0.092 Uiso 1 1 calc R . . . .
C27 C 0.9189(8) 0.2959(6) 0.3759(8) 0.094(4) Uani 1 1 d . U . . .
H27 H 0.944611 0.298981 0.341160 0.113 Uiso 1 1 calc R . . . .
C28 C 0.9400(8) 0.2874(4) 0.4695(6) 0.077(3) Uani 1 1 d . U . . .
H28 H 0.980308 0.284251 0.500631 0.092 Uiso 1 1 calc R . . . .
C29 C 0.8426(9) 0.2931(6) 0.4782(6) 0.083(3) Uani 1 1 d . U . . .
H29 H 0.821058 0.294227 0.513973 0.100 Uiso 1 1 calc R . . . .
C30 C 1.0838(8) 0.2846(7) 0.4179(8) 0.105(5) Uani 1 1 d . U . . .
H30A H 1.098950 0.279414 0.379527 0.127 Uiso 1 1 calc R . . . .
H30B H 1.111744 0.255434 0.439321 0.127 Uiso 1 1 calc R . . . .
C31 C 1.1232(6) 0.3385(4) 0.4389(6) 0.076(3) Uani 1 1 d . U . . .
C32 C 1.1245(12) 0.3822(8) 0.4045(7) 0.105(4) Uani 1 1 d . U . . .
H32 H 1.104870 0.380186 0.367503 0.126 Uiso 1 1 calc R . . . .
C33 C 1.1574(6) 0.4301(5) 0.4286(7) 0.085(3) Uani 1 1 d . U . . .
H33 H 1.162883 0.460115 0.406288 0.103 Uiso 1 1 calc R . . . .
C34 C 1.1829(6) 0.4349(4) 0.4861(7) 0.079(3) Uani 1 1 d . U . . .
C35 C 1.1727(8) 0.3891(5) 0.5195(7) 0.090(4) Uani 1 1 d . U . . .
H35 H 1.181273 0.391938 0.557599 0.107 Uiso 1 1 calc R . . . .
C36 C 1.1498(8) 0.3398(5) 0.4960(7) 0.090(3) Uani 1 1 d . U . . .
H36 H 1.151885 0.308689 0.517008 0.108 Uiso 1 1 calc R . . . .
O1 O 0.6153(7) 0.3246(2) 0.2814(4) 0.082(2) Uani 1 1 d D U . . .
O2 O 0.6273(9) 0.4341(3) 0.3069(4) 0.110(4) Uani 1 1 d D U . . .
O3 O 0.6495(5) 0.4759(4) 0.4197(3) 0.088(2) Uani 1 1 d D U . . .
O4 O 0.9413(6) 0.3753(4) 0.5733(4) 0.098(3) Uani 1 1 d D U . . .
O5 O 1.0359(14) 0.2741(6) 0.5845(5) 0.165(7) Uani 1 1 d D U . . .
O6 O 0.9793(8) 0.1782(5) 0.5239(3) 0.113(4) Uani 1 1 d D U . . .
N5 N 0.8063(5) 0.1305(3) 0.2961(4) 0.069(2) Uani 1 1 d D U . . .
N6 N 0.6860(5) 0.1071(3) 0.3827(4) 0.072(2) Uani 1 1 d D U . . .
H6 H 0.644866 0.090178 0.409504 0.086 Uiso 1 1 calc R . . . .
C37 C 0.9022(6) 0.1609(4) 0.4889(4) 0.070(2) Uani 1 1 d D U . . .
C38 C 0.9258(8) 0.1565(4) 0.4348(4) 0.075(3) Uani 1 1 d D U . . .
H38 H 0.985889 0.166571 0.423053 0.091 Uiso 1 1 calc R . . . .
C39 C 0.8564(5) 0.1363(4) 0.3986(5) 0.067(2) Uani 1 1 d D U . . .
C40 C 0.7643(6) 0.1299(4) 0.4167(4) 0.070(2) Uani 1 1 d D U . . .
C41 C 0.7437(8) 0.1385(4) 0.4717(4) 0.069(2) Uani 1 1 d D U . . .
H41 H 0.681365 0.132913 0.482798 0.083 Uiso 1 1 calc R . . . .
C42 C 0.8128(7) 0.1550(5) 0.5106(5) 0.080(3) Uani 1 1 d D U . . .
H42 H 0.800064 0.161518 0.547404 0.096 Uiso 1 1 calc R . . . .
C43 C 0.8805(8) 0.1280(6) 0.3391(5) 0.080(3) Uani 1 1 d D U . . .
H43A H 0.928574 0.154416 0.330298 0.096 Uiso 1 1 calc R . . . .
H43B H 0.910829 0.093286 0.336539 0.096 Uiso 1 1 calc R . . . .
C44 C 0.7557(11) 0.0793(5) 0.2929(6) 0.086(3) Uani 1 1 d D U . . .
H44A H 0.800408 0.051761 0.282416 0.104 Uiso 1 1 calc R . . . .
H44B H 0.705783 0.081482 0.264246 0.104 Uiso 1 1 calc R . . . .
C45 C 0.7113(8) 0.0631(4) 0.3459(5) 0.072(3) Uani 1 1 d D U . . .
H45A H 0.653737 0.042738 0.337085 0.086 Uiso 1 1 calc R . . . .
H45B H 0.755552 0.039611 0.365837 0.086 Uiso 1 1 calc R . . . .
C46 C 0.6248(6) 0.1473(5) 0.3568(5) 0.073(3) Uani 1 1 d D U . . .
H46A H 0.595114 0.167201 0.385924 0.088 Uiso 1 1 calc R . . . .
H46B H 0.573796 0.128726 0.336500 0.088 Uiso 1 1 calc R . . . .
C47 C 0.6703(8) 0.1903(5) 0.3153(6) 0.077(3) Uani 1 1 d . U . . .
C48 C 0.7561(9) 0.1813(4) 0.2906(6) 0.081(3) Uani 1 1 d D U . . .
C49 C 0.7958(10) 0.2190(6) 0.2615(4) 0.076(3) Uani 1 1 d . U . . .
H49 H 0.853161 0.212588 0.244195 0.091 Uiso 1 1 calc R . . . .
C50 C 0.7490(9) 0.2709(4) 0.2566(7) 0.092(4) Uani 1 1 d . U . . .
H50 H 0.776060 0.299801 0.238774 0.110 Uiso 1 1 calc R . . . .
C51 C 0.6567(7) 0.2736(3) 0.2820(5) 0.066(2) Uani 1 1 d D U . . .
C52 C 0.6137(12) 0.2369(5) 0.3151(6) 0.086(3) Uani 1 1 d . U . . .
H52 H 0.557532 0.241940 0.333976 0.103 Uiso 1 1 calc R . . . .
C53 C 0.6397(8) 0.3662(4) 0.2447(5) 0.072(3) Uani 1 1 d D U . . .
H53A H 0.708054 0.372972 0.247871 0.087 Uiso 1 1 calc R . . . .
H53B H 0.624177 0.355334 0.207085 0.087 Uiso 1 1 calc R . . . .
C54 C 0.5891(11) 0.4135(3) 0.2569(5) 0.090(4) Uani 1 1 d D U . . .
H54A H 0.595822 0.439378 0.227593 0.108 Uiso 1 1 calc R . . . .
H54B H 0.521465 0.405626 0.260238 0.108 Uiso 1 1 calc R . . . .
C55 C 0.5729(9) 0.4769(5) 0.3294(6) 0.091(4) Uani 1 1 d D U . . .
H55A H 0.516632 0.463188 0.346964 0.109 Uiso 1 1 calc R . . . .
H55B H 0.552599 0.501775 0.300662 0.109 Uiso 1 1 calc R . . . .
C56 C 0.6364(13) 0.5026(5) 0.3691(5) 0.100(5) Uani 1 1 d D U . . .
H56A H 0.698515 0.506775 0.352877 0.120 Uiso 1 1 calc R . . . .
H56B H 0.611846 0.538070 0.376210 0.120 Uiso 1 1 calc R . . . .
C57 C 0.7405(6) 0.4541(4) 0.4301(6) 0.070(2) Uani 1 1 d D U . . .
C58 C 0.8065(9) 0.4551(5) 0.3982(6) 0.082(3) Uani 1 1 d . U . . .
H58 H 0.796712 0.468552 0.362694 0.099 Uiso 1 1 calc R . . . .
C59 C 0.8989(8) 0.4353(5) 0.4159(6) 0.080(3) Uani 1 1 d . U . . .
H59 H 0.947013 0.434614 0.390355 0.096 Uiso 1 1 calc R . . . .
C60 C 0.9201(8) 0.4177(5) 0.4675(5) 0.070(3) Uani 1 1 d . U . . .
H60 H 0.981456 0.405950 0.477546 0.085 Uiso 1 1 calc R . . . .
C61 C 0.8469(6) 0.4179(4) 0.5049(5) 0.062(2) Uani 1 1 d . U . . .
C62 C 0.8556(7) 0.4008(5) 0.5571(5) 0.073(3) Uani 1 1 d D U . . .
C63 C 0.7816(12) 0.3980(8) 0.5948(7) 0.108(6) Uani 1 1 d . U . . .
H63 H 0.790597 0.385055 0.630514 0.130 Uiso 1 1 calc R . . . .
C64 C 0.6947(9) 0.4160(7) 0.5739(6) 0.097(5) Uani 1 1 d . U . . .
H64 H 0.643249 0.411874 0.596910 0.117 Uiso 1 1 calc R . . . .
C65 C 0.6738(9) 0.4391(5) 0.5240(6) 0.082(3) Uani 1 1 d . U . . .
H65 H 0.615608 0.455375 0.514499 0.099 Uiso 1 1 calc R . . . .
C66 C 0.7518(7) 0.4352(4) 0.4886(5) 0.063(2) Uani 1 1 d . U . . .
C67 C 0.9517(14) 0.3484(8) 0.6242(6) 0.151(8) Uani 1 1 d D U . . .
H67A H 0.892940 0.329111 0.631007 0.181 Uiso 1 1 calc R . . . .
H67B H 0.960976 0.374547 0.653389 0.181 Uiso 1 1 calc R . . . .
C68 C 1.030(2) 0.3117(10) 0.6266(7) 0.183(13) Uani 1 1 d D U . . .
H68A H 1.088568 0.332310 0.627657 0.220 Uiso 1 1 calc R . . . .
H68B H 1.027313 0.292451 0.661156 0.220 Uiso 1 1 calc R . . . .
C69 C 1.028(2) 0.2225(8) 0.6069(11) 0.181(12) Uani 1 1 d D U . . .
H69A H 1.008654 0.226270 0.644740 0.218 Uiso 1 1 calc R . . . .
H69B H 1.091125 0.206475 0.608027 0.218 Uiso 1 1 calc R . . . .
C70 C 0.9639(12) 0.1862(8) 0.5802(4) 0.116(6) Uani 1 1 d D U . . .
H70A H 0.969055 0.151955 0.598847 0.139 Uiso 1 1 calc R . . . .
H70B H 0.899001 0.199036 0.584121 0.139 Uiso 1 1 calc R . . . .
N1A N 1.1158(9) 0.5262(8) -0.0289(6) 0.117(5) Uani 1 1 d . U . . .
N2A N 0.6484(8) 0.4615(5) -0.0593(5) 0.086(3) Uani 1 1 d . U . . .
N3A N 0.5330(8) 0.6790(5) 0.0491(5) 0.087(3) Uani 1 1 d . U . . .
N4A N 1.0066(6) 0.7460(4) 0.0691(4) 0.066(2) Uani 1 1 d . U . . .
C1A C 1.2162(9) 0.5472(9) -0.0153(9) 0.127(6) Uani 1 1 d . U . . .
H1AA H 1.255402 0.544494 -0.047388 0.153 Uiso 1 1 calc R . . . .
H1AB H 1.246043 0.526239 0.014197 0.153 Uiso 1 1 calc R . . . .
C2A C 1.0785(7) 0.5034(7) 0.0063(9) 0.109(5) Uani 1 1 d D U . . .
H2A H 1.112456 0.498789 0.039585 0.130 Uiso 1 1 calc R . . . .
C3A C 0.9873(7) 0.4828(4) 0.0015(5) 0.090(3) Uani 1 1 d D U . . .
H3A H 0.963027 0.460551 0.028345 0.108 Uiso 1 1 calc R . . . .
C4A C 0.9333(8) 0.4966(5) -0.0453(4) 0.083(3) Uani 1 1 d D U . . .
C5A C 0.9856(8) 0.5201(6) -0.0871(6) 0.099(4) Uani 1 1 d D U . . .
H5AA H 0.956143 0.527100 -0.121321 0.119 Uiso 1 1 calc R . . . .
C6A C 1.0800(10) 0.5328(10) -0.0777(10) 0.140(7) Uani 1 1 d D U . . .
H6AA H 1.117090 0.545701 -0.105837 0.168 Uiso 1 1 calc R . . . .
C7A C 0.8345(7) 0.4783(5) -0.0509(5) 0.085(3) Uani 1 1 d D U . . .
C8A C 0.7881(6) 0.4594(3) -0.0052(6) 0.085(3) Uani 1 1 d D U . . .
H8A H 0.821640 0.454395 0.028211 0.102 Uiso 1 1 calc R . . . .
C9A C 0.6906(7) 0.4480(6) -0.0101(6) 0.084(3) Uani 1 1 d D U . . .
H9A H 0.656951 0.432448 0.018180 0.101 Uiso 1 1 calc R . . . .
C10A C 0.6840(6) 0.4796(8) -0.1038(7) 0.104(5) Uani 1 1 d D U . . .
H10A H 0.647188 0.488422 -0.135150 0.125 Uiso 1 1 calc R . . . .
C11A C 0.7828(6) 0.4845(5) -0.1001(5) 0.087(3) Uani 1 1 d D U . . .
H11A H 0.815528 0.492171 -0.131888 0.105 Uiso 1 1 calc R . . . .
C12A C 0.5366(9) 0.4588(7) -0.0589(4) 0.080(3) Uani 1 1 d . U . . .
H12C H 0.511591 0.455130 -0.096535 0.096 Uiso 1 1 calc R . . . .
H12D H 0.517777 0.427269 -0.038706 0.096 Uiso 1 1 calc R . . . .
C13A C 0.4926(6) 0.5071(5) -0.0335(6) 0.076(3) Uani 1 1 d . U . . .
C14A C 0.4860(7) 0.5072(4) 0.0184(6) 0.071(3) Uani 1 1 d . U . . .
H14A H 0.498627 0.476856 0.039534 0.085 Uiso 1 1 calc R . . . .
C15A C 0.4582(7) 0.5566(4) 0.0426(6) 0.068(3) Uani 1 1 d . U . . .
H15A H 0.445288 0.557523 0.079886 0.081 Uiso 1 1 calc R . . . .
C16A C 0.4495(8) 0.6044(4) 0.0113(6) 0.075(3) Uani 1 1 d . U . . .
C17A C 0.4505(6) 0.5955(6) -0.0405(6) 0.081(3) Uani 1 1 d . U . . .
H17A H 0.426792 0.622334 -0.063630 0.097 Uiso 1 1 calc R . . . .
C18A C 0.4869(10) 0.5449(6) -0.0679(7) 0.096(4) Uani 1 1 d . U . . .
H18A H 0.502573 0.542286 -0.104749 0.116 Uiso 1 1 calc R . . . .
C19A C 0.4331(6) 0.6536(4) 0.0380(6) 0.070(3) Uani 1 1 d . U . . .
H19C H 0.401210 0.647769 0.072326 0.084 Uiso 1 1 calc R . . . .
H19D H 0.393416 0.676689 0.014670 0.084 Uiso 1 1 calc R . . . .
C20A C 0.5849(9) 0.6649(5) 0.0928(7) 0.091(3) Uani 1 1 d D U . . .
H20A H 0.558726 0.643478 0.119719 0.110 Uiso 1 1 calc R . . . .
C21A C 0.6786(8) 0.6823(4) 0.0986(5) 0.078(3) Uani 1 1 d D U . . .
H21A H 0.718586 0.668248 0.126432 0.093 Uiso 1 1 calc R . . . .
C22A C 0.7131(7) 0.7201(4) 0.0633(5) 0.073(3) Uani 1 1 d D U . . .
C23A C 0.6512(7) 0.7359(6) 0.0205(5) 0.093(4) Uani 1 1 d D U . . .
H23A H 0.674171 0.759890 -0.005195 0.111 Uiso 1 1 calc R . . . .
C24A C 0.5582(7) 0.7185(5) 0.0136(6) 0.084(3) Uani 1 1 d D U . . .
H24A H 0.515895 0.732581 -0.013063 0.101 Uiso 1 1 calc R . . . .
C25A C 0.8129(7) 0.7319(4) 0.0670(3) 0.062(2) Uani 1 1 d D U . . .
C26A C 0.8653(8) 0.7376(6) 0.1166(4) 0.088(4) Uani 1 1 d D U . . .
H26A H 0.835501 0.734891 0.150164 0.106 Uiso 1 1 calc R . . . .
C27A C 0.9640(9) 0.7474(8) 0.1146(5) 0.100(5) Uani 1 1 d D U . . .
H27A H 0.998832 0.755144 0.147019 0.120 Uiso 1 1 calc R . . . .
C28A C 0.9579(6) 0.7494(5) 0.0192(4) 0.066(2) Uani 1 1 d D U . . .
H28A H 0.989639 0.756950 -0.012899 0.079 Uiso 1 1 calc R . . . .
C29A C 0.8594(6) 0.7411(4) 0.0184(4) 0.065(2) Uani 1 1 d D U . . .
H29A H 0.824538 0.741673 -0.015009 0.078 Uiso 1 1 calc R . . . .
C30A C 1.1117(6) 0.7547(4) 0.0696(8) 0.098(5) Uani 1 1 d . U . . .
H30C H 1.126864 0.786144 0.048203 0.117 Uiso 1 1 calc R . . . .
H30D H 1.136573 0.759749 0.107069 0.117 Uiso 1 1 calc R . . . .
C31A C 1.1531(7) 0.7069(6) 0.0453(6) 0.083(3) Uani 1 1 d . U . . .
C32A C 1.1712(10) 0.6603(6) 0.0776(8) 0.103(4) Uani 1 1 d . U . . .
H32A H 1.160563 0.663153 0.115107 0.123 Uiso 1 1 calc R . . . .
C33A C 1.2013(9) 0.6137(5) 0.0604(8) 0.097(4) Uani 1 1 d . U . . .
H33A H 1.217447 0.586448 0.085106 0.117 Uiso 1 1 calc R . . . .
C34A C 1.2083(10) 0.6063(10) 0.0027(10) 0.123(5) Uani 1 1 d . U . . .
C35A C 1.1910(11) 0.6506(11) -0.0301(8) 0.120(5) Uani 1 1 d . U . . .
H35A H 1.198481 0.647814 -0.067934 0.144 Uiso 1 1 calc R . . . .
C36A C 1.1655(6) 0.6946(8) -0.0102(7) 0.101(4) Uani 1 1 d . U . . .
H36A H 1.153357 0.722062 -0.035265 0.122 Uiso 1 1 calc R . . . .
O1A O 0.6539(6) 0.7017(3) 0.2215(4) 0.090(3) Uani 1 1 d D U . . .
O2A O 0.681(2) 0.5936(5) 0.1948(5) 0.236(14) Uani 1 1 d D U . . .
O3A O 0.7061(7) 0.5518(4) 0.0846(3) 0.085(2) Uani 1 1 d D U . . .
O4A O 0.9471(6) 0.6626(4) -0.0739(4) 0.094(3) Uani 1 1 d . U . . .
O5A O 1.0146(11) 0.7703(4) -0.0994(5) 0.119(4) Uani 1 1 d D U . . .
O6A O 0.9777(7) 0.8568(6) -0.0234(4) 0.112(4) Uani 1 1 d D U . . .
N5A N 0.8189(6) 0.9036(3) 0.1973(4) 0.068(2) Uani 1 1 d D U . . .
H5A H 0.859266 0.904801 0.231055 0.082 Uiso 1 1 calc R . . . .
N6A N 0.6799(6) 0.9185(3) 0.1123(4) 0.080(2) Uani 1 1 d D U . . .
C37A C 0.8972(6) 0.8704(4) 0.0072(4) 0.062(2) Uani 1 1 d D U . . .
C38A C 0.9249(9) 0.8771(5) 0.0612(4) 0.072(3) Uani 1 1 d . U . . .
H38A H 0.988029 0.872213 0.073685 0.086 Uiso 1 1 calc R . . . .
C39A C 0.8524(8) 0.8917(5) 0.0968(5) 0.071(3) Uani 1 1 d . U . . .
C40A C 0.7611(7) 0.8982(4) 0.0831(5) 0.073(2) Uani 1 1 d D U . . .
C41A C 0.7338(9) 0.8860(7) 0.0294(7) 0.094(4) Uani 1 1 d . U . . .
H41A H 0.668824 0.888322 0.019792 0.112 Uiso 1 1 calc R . . . .
C42A C 0.7964(10) 0.8704(6) -0.0121(7) 0.096(4) Uani 1 1 d . U . . .
H42A H 0.776070 0.861234 -0.047775 0.115 Uiso 1 1 calc R . . . .
C43A C 0.8888(9) 0.9076(5) 0.1549(4) 0.077(3) Uani 1 1 d D U . . .
H43C H 0.943111 0.885147 0.165177 0.093 Uiso 1 1 calc R . . . .
H43D H 0.911615 0.944227 0.153757 0.093 Uiso 1 1 calc R . . . .
C44A C 0.7516(10) 0.9466(5) 0.2061(6) 0.090(3) Uani 1 1 d D U . . .
H44C H 0.784347 0.977013 0.222930 0.108 Uiso 1 1 calc R . . . .
H44D H 0.701851 0.934965 0.230264 0.108 Uiso 1 1 calc R . . . .
C45A C 0.7057(10) 0.9629(4) 0.1469(6) 0.087(3) Uani 1 1 d D U . . .
H45C H 0.649026 0.984397 0.152356 0.104 Uiso 1 1 calc R . . . .
H45D H 0.751352 0.984946 0.127953 0.104 Uiso 1 1 calc R . . . .
C46A C 0.6339(8) 0.8747(5) 0.1403(6) 0.084(3) Uani 1 1 d D U . . .
H46C H 0.582613 0.890246 0.161034 0.101 Uiso 1 1 calc R . . . .
H46D H 0.603606 0.852560 0.111937 0.101 Uiso 1 1 calc R . . . .
C47A C 0.6853(7) 0.8398(3) 0.1768(6) 0.079(3) Uani 1 1 d D U . . .
C48A C 0.7749(7) 0.8511(4) 0.2009(5) 0.079(3) Uani 1 1 d D U . . .
C49A C 0.8265(12) 0.8148(6) 0.2337(10) 0.139(8) Uani 1 1 d D U . . .
H49A H 0.887076 0.823116 0.248403 0.167 Uiso 1 1 calc R . . . .
C50A C 0.7846(8) 0.7663(5) 0.2436(4) 0.085(4) Uani 1 1 d D U . . .
H50A H 0.814880 0.743635 0.269152 0.103 Uiso 1 1 calc R . . . .
C51A C 0.7002(8) 0.7491(4) 0.2180(5) 0.080(3) Uani 1 1 d D U . . .
C52A C 0.6557(7) 0.7864(3) 0.1828(5) 0.071(3) Uani 1 1 d D U . . .
H52A H 0.602641 0.775064 0.161695 0.085 Uiso 1 1 calc R . . . .
C53A C 0.6970(15) 0.6626(5) 0.2566(6) 0.120(6) Uani 1 1 d D U . . .
H53C H 0.689384 0.672679 0.294816 0.144 Uiso 1 1 calc R . . . .
H53D H 0.765047 0.660412 0.250090 0.144 Uiso 1 1 calc R . . . .
C54A C 0.654(2) 0.6119(5) 0.2466(6) 0.169(11) Uani 1 1 d D U . . .
H54C H 0.674038 0.586757 0.275005 0.203 Uiso 1 1 calc R . . . .
H54D H 0.584369 0.615161 0.247033 0.203 Uiso 1 1 calc R . . . .
C55A C 0.664(2) 0.5399(6) 0.1842(8) 0.170(12) Uani 1 1 d D U . . .
H55C H 0.595196 0.533663 0.184224 0.204 Uiso 1 1 calc R . . . .
H55D H 0.693017 0.518846 0.213864 0.204 Uiso 1 1 calc R . . . .
C56A C 0.6990(13) 0.5218(5) 0.1336(5) 0.105(5) Uani 1 1 d D U . . .
H56C H 0.763185 0.508700 0.142093 0.126 Uiso 1 1 calc R . . . .
H56D H 0.660802 0.490743 0.123543 0.126 Uiso 1 1 calc R . . . .
C57A C 0.7856(10) 0.5731(6) 0.0716(6) 0.087(3) Uani 1 1 d . U . . .
C58A C 0.8660(11) 0.5798(6) 0.0985(6) 0.092(4) Uani 1 1 d . U . . .
H58A H 0.868393 0.569419 0.135264 0.110 Uiso 1 1 calc R . . . .
C59A C 0.9523(10) 0.6018(5) 0.0771(6) 0.085(3) Uani 1 1 d . U . . .
H59A H 1.006991 0.606480 0.099539 0.103 Uiso 1 1 calc R . . . .
C60A C 0.9512(6) 0.6146(4) 0.0267(5) 0.066(2) Uani 1 1 d . U . . .
H60A H 1.009335 0.621878 0.010655 0.080 Uiso 1 1 calc R . . . .
C61A C 0.8664(6) 0.6185(5) -0.0066(6) 0.077(3) Uani 1 1 d . U . . .
C62A C 0.8657(7) 0.6378(7) -0.0580(6) 0.090(4) Uani 1 1 d . U . . .
C63A C 0.7846(8) 0.6358(5) -0.0909(7) 0.083(3) Uani 1 1 d . U . . .
H63A H 0.783740 0.646780 -0.127499 0.100 Uiso 1 1 calc R . . . .
C64A C 0.7025(8) 0.6160(7) -0.0658(6) 0.093(4) Uani 1 1 d . U . . .
H64A H 0.643879 0.621363 -0.084392 0.111 Uiso 1 1 calc R . . . .
C65A C 0.7014(7) 0.5898(7) -0.0169(5) 0.088(4) Uani 1 1 d . U . . .
H65A H 0.648214 0.569360 -0.008573 0.105 Uiso 1 1 calc R . . . .
C66A C 0.7785(7) 0.5930(4) 0.0213(5) 0.061(2) Uani 1 1 d . U . . .
C67A C 0.9503(15) 0.6796(7) -0.1261(7) 0.120(6) Uani 1 1 d D U . . .
H67C H 0.884848 0.683227 -0.140353 0.144 Uiso 1 1 calc R . . . .
H67D H 0.980053 0.651673 -0.147411 0.144 Uiso 1 1 calc R . . . .
C68A C 0.9987(17) 0.7280(6) -0.1366(7) 0.126(7) Uani 1 1 d D U . . .
H68C H 1.061523 0.717711 -0.148743 0.151 Uiso 1 1 calc R . . . .
H68D H 0.965419 0.743610 -0.168431 0.151 Uiso 1 1 calc R . . . .
C69A C 0.955(3) 0.8128(9) -0.1140(8) 0.227(19) Uani 1 1 d D U . . .
H69C H 0.889313 0.799839 -0.115254 0.272 Uiso 1 1 calc R . . . .
H69D H 0.969563 0.823790 -0.151083 0.272 Uiso 1 1 calc R . . . .
C70A C 0.959(2) 0.8584(8) -0.0802(5) 0.170(12) Uani 1 1 d D U . . .
H70C H 1.006536 0.881801 -0.095316 0.205 Uiso 1 1 calc R . . . .
H70D H 0.897561 0.876389 -0.085547 0.205 Uiso 1 1 calc R . . . .
P1 P 0.6309(3) 0.31059(13) 0.91963(19) 0.0901(10) Uani 1 1 d . U . . .
F1 F 0.6970(6) 0.2843(4) 0.8783(5) 0.116(3) Uani 1 1 d . U . . .
F2 F 0.5570(9) 0.3353(5) 0.9625(5) 0.136(4) Uani 1 1 d . U . . .
F3 F 0.7150(7) 0.3462(3) 0.9469(7) 0.155(5) Uani 1 1 d . U . . .
F4 F 0.6577(8) 0.2665(3) 0.9619(4) 0.114(3) Uani 1 1 d . U . . .
F5 F 0.5464(6) 0.2707(4) 0.8919(4) 0.115(3) Uani 1 1 d . U . . .
F6 F 0.6095(6) 0.3580(4) 0.8764(5) 0.123(3) Uani 1 1 d . U . . .
P2 P 0.5431(3) 0.5052(3) 0.74815(17) 0.1107(15) Uani 1 1 d . U . . .
F7 F 0.6086(11) 0.4741(8) 0.7090(8) 0.191(6) Uani 1 1 d . U . . .
F8 F 0.4815(14) 0.5383(7) 0.7896(7) 0.180(6) Uani 1 1 d . U . . .
F9 F 0.4483(9) 0.4833(6) 0.7235(6) 0.153(4) Uani 1 1 d . U . . .
F10 F 0.5407(12) 0.4529(6) 0.7881(5) 0.163(5) Uani 1 1 d . U . . .
F11 F 0.6242(10) 0.5336(8) 0.7776(7) 0.207(7) Uani 1 1 d . U . . .
F12 F 0.5385(9) 0.5485(6) 0.7085(4) 0.146(4) Uani 1 1 d . U . . .
P3 P 0.9361(3) 0.5208(2) 0.74707(18) 0.1056(13) Uani 1 1 d . U . . .
F13 F 1.012(2) 0.4989(12) 0.7076(8) 0.256(11) Uani 1 1 d . U . . .
F14 F 0.8681(11) 0.5468(8) 0.7865(7) 0.201(8) Uani 1 1 d . U . . .
F15 F 0.9368(11) 0.4729(5) 0.7893(5) 0.155(5) Uani 1 1 d . U . . .
F16 F 1.0203(10) 0.5394(8) 0.7818(7) 0.192(7) Uani 1 1 d . U . . .
F17 F 0.9332(13) 0.5638(6) 0.7034(5) 0.162(5) Uani 1 1 d . U . . .
F18 F 0.8603(18) 0.5008(10) 0.7137(7) 0.258(11) Uani 1 1 d . U . . .
P4 P 0.6517(2) 0.71941(15) 0.5911(2) 0.0947(11) Uani 1 1 d . U . . .
F19 F 0.7354(10) 0.6820(4) 0.5751(9) 0.177(6) Uani 1 1 d . U . . .
F20 F 0.5701(10) 0.7582(5) 0.6060(8) 0.176(6) Uani 1 1 d . U . . .
F21 F 0.6238(8) 0.6741(4) 0.6313(6) 0.138(4) Uani 1 1 d . U . . .
F22 F 0.7246(12) 0.7406(5) 0.6320(8) 0.194(7) Uani 1 1 d . U . . .
F23 F 0.6810(11) 0.7608(3) 0.5454(6) 0.149(4) Uani 1 1 d . U . . .
F24 F 0.5847(11) 0.6957(7) 0.5484(7) 0.187(6) Uani 1 1 d . U . . .
P5 P 0.4619(6) 0.6544(4) 0.3842(3) 0.177(4) Uani 1 1 d D U . . .
F25 F 0.4504(17) 0.6026(7) 0.3584(10) 0.315(13) Uani 1 1 d D U . . .
F26 F 0.4721(15) 0.7059(7) 0.4098(9) 0.282(11) Uani 1 1 d D U . . .
F27 F 0.4311(16) 0.6317(11) 0.4350(7) 0.379(19) Uani 1 1 d D U . . .
F28 F 0.5595(11) 0.6407(10) 0.3991(7) 0.274(12) Uani 1 1 d D U . . .
F29 F 0.4928(14) 0.6760(10) 0.3328(6) 0.274(11) Uani 1 1 d D U . . .
F30 F 0.3633(9) 0.6667(7) 0.3692(8) 0.225(9) Uani 1 1 d D U . . .
P6 P 0.0933(9) 0.6933(5) 0.2477(3) 0.223(5) Uani 1 1 d D U . . .
F31 F 0.181(2) 0.6582(15) 0.2458(13) 0.49(3) Uani 1 1 d D U . . .
F32 F 0.0057(18) 0.7280(12) 0.2491(7) 0.44(3) Uani 1 1 d D U . . .
F33 F 0.141(2) 0.7257(13) 0.2929(6) 0.45(2) Uani 1 1 d D U . . .
F34 F 0.052(2) 0.6569(10) 0.2902(9) 0.39(2) Uani 1 1 d D U . . .
F35 F 0.046(3) 0.6603(12) 0.2026(10) 0.50(3) Uani 1 1 d D U . . .
F36 F 0.1341(18) 0.7295(11) 0.2050(7) 0.40(2) Uani 1 1 d D U . . .
P7 P 0.9518(9) 0.4101(5) 0.2402(4) 0.253(6) Uani 1 1 d D U . . .
F37 F 1.0430(13) 0.3913(9) 0.2166(9) 0.304(13) Uani 1 1 d D U . . .
F38 F 0.8614(15) 0.4310(12) 0.2629(10) 0.45(2) Uani 1 1 d D U . . .
F39 F 0.8945(14) 0.3760(10) 0.2009(6) 0.336(16) Uani 1 1 d D U . . .
F40 F 0.956(2) 0.3651(9) 0.2806(8) 0.390(19) Uani 1 1 d D U . . .
F41 F 1.0078(16) 0.4442(7) 0.2804(7) 0.244(9) Uani 1 1 d D U . . .
F42 F 0.9510(13) 0.4547(9) 0.1993(8) 0.300(12) Uani 1 1 d D U . . .
P8 P 0.3671(5) 0.2875(3) 0.1284(2) 0.1346(19) Uani 1 1 d . U . . .
F43 F 0.4169(13) 0.2314(9) 0.1110(7) 0.194(7) Uani 1 1 d . U . . .
F44 F 0.310(2) 0.3393(8) 0.1447(8) 0.236(9) Uani 1 1 d . U . . .
F45 F 0.3266(13) 0.2566(8) 0.1759(5) 0.179(6) Uani 1 1 d . U . . .
F46 F 0.4523(18) 0.3078(16) 0.1641(7) 0.311(14) Uani 1 1 d . U . . .
F47 F 0.4165(14) 0.3243(11) 0.0823(8) 0.226(9) Uani 1 1 d . U . . .
F48 F 0.2845(8) 0.2724(6) 0.0911(4) 0.131(3) Uani 1 1 d . 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
N1 C1 1.528(14) . ?
N1 C2 1.32(2) . ?
N1 C6 1.40(2) . ?
N2 C9 1.362(14) . ?
N2 C10 1.308(15) . ?
N2 C12 1.616(13) . ?
N3 C19 1.552(17) . ?
N3 C20 1.302(16) . ?
N3 C24 1.326(18) . ?
N4 C27 1.45(2) . ?
N4 C28 1.260(18) . ?
N4 C30 1.498(13) . ?
C1 C34 1.449(16) . ?
C2 C3 1.388(16) . ?
C3 C4 1.275(17) . ?
C4 C5 1.365(17) . ?
C4 C7 1.454(13) . ?
C5 C6 1.348(19) . ?
C7 C8 1.434(15) . ?
C7 C11 1.412(14) . ?
C8 C9 1.296(15) . ?
C10 C11 1.409(13) . ?
C12 C13 1.531(17) . ?
C13 C14 1.274(17) . ?
C13 C18 1.40(2) . ?
C14 C15 1.440(15) . ?
C15 C16 1.347(17) . ?
C16 C17 1.385(19) . ?
C16 C19 1.511(16) . ?
C17 C18 1.44(2) . ?
C20 C21 1.316(15) . ?
C21 C22 1.362(18) . ?
C22 C23 1.371(19) . ?
C22 C25 1.521(18) . ?
C23 C24 1.450(19) . ?
C25 C26 1.487(17) . ?
C25 C29 1.360(18) . ?
C26 C27 1.305(16) . ?
C28 C29 1.405(17) . ?
C30 C31 1.554(16) . ?
C31 C32 1.39(2) . ?
C31 C36 1.44(2) . ?
C32 C33 1.42(2) . ?
C33 C34 1.45(2) . ?
C34 C35 1.43(2) . ?
C35 C36 1.405(17) . ?
O1 C51 1.416(9) . ?
O1 C53 1.433(9) . ?
O2 C54 1.423(10) . ?
O2 C55 1.445(9) . ?
O3 C56 1.418(9) . ?
O3 C57 1.412(9) . ?
O4 C62 1.417(9) . ?
O4 C67 1.426(10) . ?
O5 C68 1.408(10) . ?
O5 C69 1.423(11) . ?
O6 C37 1.429(9) . ?
O6 C70 1.420(10) . ?
N5 C43 1.461(9) . ?
N5 C44 1.479(9) . ?
N5 C48 1.471(9) . ?
N6 C40 1.477(9) . ?
N6 C45 1.483(9) . ?
N6 C46 1.464(9) . ?
C37 C38 1.384(10) . ?
C37 C42 1.394(10) . ?
C38 C39 1.397(10) . ?
C39 C40 1.397(9) . ?
C39 C43 1.524(17) . ?
C40 C41 1.407(9) . ?
C41 C42 1.405(10) . ?
C44 C45 1.519(18) . ?
C46 C47 1.636(18) . ?
C47 C48 1.390(16) . ?
C47 C52 1.424(17) . ?
C48 C49 1.326(18) . ?
C49 C50 1.473(19) . ?
C50 C51 1.464(16) . ?
C51 C52 1.386(18) . ?
C53 C54 1.429(11) . ?
C55 C56 1.454(11) . ?
C57 C58 1.237(17) . ?
C57 C66 1.517(18) . ?
C58 C59 1.448(19) . ?
C59 C60 1.364(19) . ?
C60 C61 1.406(15) . ?
C61 C62 1.352(17) . ?
C61 C66 1.454(14) . ?
C62 C63 1.419(18) . ?
C63 C64 1.39(2) . ?
C64 C65 1.38(2) . ?
C65 C66 1.429(16) . ?
C67 C68 1.438(13) . ?
C69 C70 1.431(13) . ?
N1A C1A 1.539(19) . ?
N1A C2A 1.18(3) . ?
N1A C6A 1.29(3) . ?
N2A C9A 1.370(19) . ?
N2A C10A 1.30(2) . ?
N2A C12A 1.580(16) . ?
N3A C19A 1.564(13) . ?
N3A C20A 1.33(2) . ?
N3A C24A 1.380(19) . ?
N4A C27A 1.287(15) . ?
N4A C28A 1.384(13) . ?
N4A C30A 1.499(11) . ?
C1A C34A 1.56(3) . ?
C2A C3A 1.389(10) . ?
C3A C4A 1.400(10) . ?
C4A C5A 1.415(10) . ?
C4A C7A 1.470(16) . ?
C5A C6A 1.381(10) . ?
C7A C8A 1.401(10) . ?
C7A C11A 1.399(10) . ?
C8A C9A 1.407(9) . ?
C10A C11A 1.398(8) . ?
C12A C13A 1.514(18) . ?
C13A C14A 1.278(18) . ?
C13A C18A 1.28(2) . ?
C14A C15A 1.444(13) . ?
C15A C16A 1.433(18) . ?
C16A C17A 1.290(19) . ?
C16A C19A 1.428(16) . ?
C17A C18A 1.54(2) . ?
C20A C21A 1.395(10) . ?
C21A C22A 1.389(9) . ?
C22A C23A 1.400(9) . ?
C22A C25A 1.438(14) . ?
C23A C24A 1.388(9) . ?
C25A C26A 1.408(9) . ?
C25A C29A 1.401(9) . ?
C26A C27A 1.417(10) . ?
C28A C29A 1.405(9) . ?
C30A C31A 1.477(17) . ?
C31A C32A 1.44(2) . ?
C31A C36A 1.41(2) . ?
C32A C33A 1.326(18) . ?
C33A C34A 1.43(3) . ?
C34A C35A 1.39(3) . ?
C35A C36A 1.27(3) . ?
O1A C51A 1.369(14) . ?
O1A C53A 1.434(9) . ?
O2A C54A 1.420(10) . ?
O2A C55A 1.404(11) . ?
O3A C56A 1.424(10) . ?
O3A C57A 1.295(15) . ?
O4A C62A 1.376(13) . ?
O4A C67A 1.35(2) . ?
O5A C68A 1.419(10) . ?
O5A C69A 1.407(11) . ?
O6A C37A 1.424(9) . ?
O6A C70A 1.410(10) . ?
N5A C43A 1.461(9) . ?
N5A C44A 1.465(9) . ?
N5A C48A 1.468(9) . ?
N6A C40A 1.466(9) . ?
N6A C45A 1.447(9) . ?
N6A C46A 1.465(9) . ?
C37A C38A 1.378(16) . ?
C37A C42A 1.483(17) . ?
C38A C39A 1.415(17) . ?
C39A C40A 1.330(16) . ?
C39A C43A 1.552(16) . ?
C40A C41A 1.393(19) . ?
C41A C42A 1.43(2) . ?
C44A C45A 1.62(2) . ?
C46A C47A 1.437(15) . ?
C47A C48A 1.406(9) . ?
C47A C52A 1.422(8) . ?
C48A C49A 1.408(10) . ?
C49A C50A 1.385(10) . ?
C50A C51A 1.397(9) . ?
C51A C52A 1.411(9) . ?
C53A C54A 1.437(13) . ?
C55A C56A 1.429(12) . ?
C57A C58A 1.30(2) . ?
C57A C66A 1.334(19) . ?
C58A C59A 1.453(19) . ?
C59A C60A 1.277(19) . ?
C60A C61A 1.429(17) . ?
C61A C62A 1.35(2) . ?
C61A C66A 1.574(14) . ?
C62A C63A 1.38(2) . ?
C63A C64A 1.421(18) . ?
C64A C65A 1.37(2) . ?
C65A C66A 1.413(16) . ?
C67A C68A 1.429(12) . ?
C69A C70A 1.420(13) . ?
P1 F1 1.550(10) . ?
P1 F2 1.630(12) . ?
P1 F3 1.616(10) . ?
P1 F4 1.559(9) . ?
P1 F5 1.686(10) . ?
P1 F6 1.622(9) . ?
P2 F7 1.567(15) . ?
P2 F8 1.597(15) . ?
P2 F9 1.551(12) . ?
P2 F10 1.648(14) . ?
P2 F11 1.513(15) . ?
P2 F12 1.464(13) . ?
P3 F13 1.57(2) . ?
P3 F14 1.532(14) . ?
P3 F15 1.595(11) . ?
P3 F16 1.512(12) . ?
P3 F17 1.525(13) . ?
P3 F18 1.419(15) . ?
P4 F19 1.574(12) . ?
P4 F20 1.565(11) . ?
P4 F21 1.570(9) . ?
P4 F22 1.510(13) . ?
P4 F23 1.598(11) . ?
P4 F24 1.509(13) . ?
P5 F25 1.461(13) . ?
P5 F26 1.452(13) . ?
P5 F27 1.452(12) . ?
P5 F28 1.454(12) . ?
P5 F29 1.455(12) . ?
P5 F30 1.459(11) . ?
P6 F31 1.522(15) . ?
P6 F32 1.515(14) . ?
P6 F33 1.518(14) . ?
P6 F34 1.523(14) . ?
P6 F35 1.524(15) . ?
P6 F36 1.518(14) . ?
P7 F37 1.505(13) . ?
P7 F38 1.504(14) . ?
P7 F39 1.507(13) . ?
P7 F40 1.510(14) . ?
P7 F41 1.511(13) . ?
P7 F42 1.510(13) . ?
P8 F43 1.645(19) . ?
P8 F44 1.60(2) . ?
P8 F45 1.528(16) . ?
P8 F46 1.549(19) . ?
P8 F47 1.639(18) . ?
P8 F48 1.507(13) . ?

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 N1 C1 117.6(13) . . ?
C2 N1 C6 121.3(10) . . ?
C6 N1 C1 120.8(13) . . ?
C9 N2 C12 119.8(9) . . ?
C10 N2 C9 123.2(10) . . ?
C10 N2 C12 116.5(9) . . ?
C20 N3 C19 120.7(12) . . ?
C20 N3 C24 121.2(12) . . ?
C24 N3 C19 116.0(10) . . ?
C27 N4 C30 118.4(13) . . ?
C28 N4 C27 117.5(10) . . ?
C28 N4 C30 123.2(12) . . ?
C34 C1 N1 113.8(8) . . ?
N1 C2 C3 117.3(14) . . ?
C4 C3 C2 124.2(14) . . ?
C3 C4 C5 117.4(10) . . ?
C3 C4 C7 121.5(11) . . ?
C5 C4 C7 121.0(11) . . ?
C6 C5 C4 123.2(13) . . ?
C5 C6 N1 116.2(12) . . ?
C8 C7 C4 124.0(10) . . ?
C11 C7 C4 121.3(10) . . ?
C11 C7 C8 114.5(9) . . ?
C9 C8 C7 120.0(10) . . ?
C8 C9 N2 122.4(11) . . ?
N2 C10 C11 116.4(10) . . ?
C10 C11 C7 122.6(10) . . ?
C13 C12 N2 109.9(8) . . ?
C14 C13 C12 123.8(12) . . ?
C14 C13 C18 129.1(12) . . ?
C18 C13 C12 106.7(12) . . ?
C13 C14 C15 118.0(11) . . ?
C16 C15 C14 118.3(11) . . ?
C15 C16 C17 121.2(11) . . ?
C15 C16 C19 119.4(11) . . ?
C17 C16 C19 119.4(10) . . ?
C16 C17 C18 121.6(12) . . ?
C13 C18 C17 111.3(13) . . ?
C16 C19 N3 109.9(9) . . ?
N3 C20 C21 125.7(14) . . ?
C20 C21 C22 115.4(11) . . ?
C21 C22 C23 123.7(13) . . ?
C21 C22 C25 118.2(10) . . ?
C23 C22 C25 117.2(12) . . ?
C22 C23 C24 115.6(14) . . ?
N3 C24 C23 118.0(12) . . ?
C26 C25 C22 125.4(10) . . ?
C29 C25 C22 121.7(11) . . ?
C29 C25 C26 111.5(11) . . ?
C27 C26 C25 126.2(13) . . ?
C26 C27 N4 117.4(15) . . ?
N4 C28 C29 126.2(13) . . ?
C25 C29 C28 120.7(13) . . ?
N4 C30 C31 106.8(10) . . ?
C32 C31 C30 120.5(15) . . ?
C32 C31 C36 124.3(12) . . ?
C36 C31 C30 115.0(13) . . ?
C31 C32 C33 115.8(15) . . ?
C32 C33 C34 123.0(14) . . ?
C1 C34 C33 111.7(14) . . ?
C35 C34 C1 128.1(15) . . ?
C35 C34 C33 117.7(10) . . ?
C36 C35 C34 120.6(16) . . ?
C35 C36 C31 118.0(14) . . ?
C51 O1 C53 124.6(9) . . ?
C54 O2 C55 114.4(9) . . ?
C57 O3 C56 115.7(11) . . ?
C62 O4 C67 121.6(12) . . ?
C68 O5 C69 109(2) . . ?
C70 O6 C37 119.2(10) . . ?
C43 N5 C44 109.4(10) . . ?
C43 N5 C48 115.7(10) . . ?
C48 N5 C44 121.9(9) . . ?
C40 N6 C45 116.4(7) . . ?
C46 N6 C40 113.2(8) . . ?
C46 N6 C45 114.0(9) . . ?
C38 C37 O6 113.3(8) . . ?
C38 C37 C42 127.5(9) . . ?
C42 C37 O6 118.9(9) . . ?
C37 C38 C39 117.0(10) . . ?
C38 C39 C40 118.6(9) . . ?
C38 C39 C43 119.0(8) . . ?
C40 C39 C43 122.0(8) . . ?
C39 C40 N6 123.4(8) . . ?
C39 C40 C41 120.8(9) . . ?
C41 C40 N6 115.2(8) . . ?
C42 C41 C40 122.4(10) . . ?
C37 C42 C41 112.8(10) . . ?
N5 C43 C39 120.5(10) . . ?
N5 C44 C45 113.8(9) . . ?
N6 C45 C44 115.7(9) . . ?
N6 C46 C47 119.5(8) . . ?
C48 C47 C46 121.9(10) . . ?
C48 C47 C52 129.1(12) . . ?
C52 C47 C46 108.7(10) . . ?
C47 C48 N5 121.9(11) . . ?
C49 C48 N5 117.6(11) . . ?
C49 C48 C47 120.5(11) . . ?
C48 C49 C50 119.1(12) . . ?
C51 C50 C49 114.2(10) . . ?
O1 C51 C50 114.3(9) . . ?
C52 C51 O1 115.3(10) . . ?
C52 C51 C50 129.1(11) . . ?
C51 C52 C47 107.4(12) . . ?
C54 C53 O1 110.4(9) . . ?
O2 C54 C53 108.1(10) . . ?
O2 C55 C56 105.5(11) . . ?
O3 C56 C55 115.6(11) . . ?
O3 C57 C66 111.1(9) . . ?
C58 C57 O3 125.2(12) . . ?
C58 C57 C66 123.2(11) . . ?
C57 C58 C59 119.5(14) . . ?
C60 C59 C58 123.9(12) . . ?
C59 C60 C61 117.5(12) . . ?
C60 C61 C66 120.8(11) . . ?
C62 C61 C60 125.0(10) . . ?
C62 C61 C66 114.1(9) . . ?
O4 C62 C63 115.7(11) . . ?
C61 C62 O4 117.3(10) . . ?
C61 C62 C63 126.0(10) . . ?
C64 C63 C62 113.8(12) . . ?
C65 C64 C63 128.7(12) . . ?
C64 C65 C66 111.3(11) . . ?
C61 C66 C57 114.9(9) . . ?
C65 C66 C57 119.7(10) . . ?
C65 C66 C61 125.2(11) . . ?
O4 C67 C68 113.4(17) . . ?
O5 C68 C67 118.2(18) . . ?
O5 C69 C70 118.0(17) . . ?
O6 C70 C69 115.0(17) . . ?
C2A N1A C1A 116.2(16) . . ?
C2A N1A C6A 124.8(16) . . ?
C6A N1A C1A 118.9(18) . . ?
C9A N2A C12A 112.8(10) . . ?
C10A N2A C9A 131.2(11) . . ?
C10A N2A C12A 115.7(10) . . ?
C20A N3A C19A 120.0(10) . . ?
C20A N3A C24A 123.8(10) . . ?
C24A N3A C19A 116.0(12) . . ?
C27A N4A C28A 122.2(10) . . ?
C27A N4A C30A 118.6(11) . . ?
C28A N4A C30A 117.3(10) . . ?
N1A C1A C34A 108.5(12) . . ?
N1A C2A C3A 123.9(18) . . ?
C2A C3A C4A 116.9(15) . . ?
C3A C4A C5A 114.6(12) . . ?
C3A C4A C7A 119.0(11) . . ?
C5A C4A C7A 125.6(10) . . ?
C6A C5A C4A 120.0(16) . . ?
N1A C6A C5A 118(2) . . ?
C8A C7A C4A 120.0(9) . . ?
C11A C7A C4A 120.6(10) . . ?
C11A C7A C8A 119.0(11) . . ?
C7A C8A C9A 118.9(13) . . ?
N2A C9A C8A 114.7(13) . . ?
N2A C10A C11A 112.9(14) . . ?
C10A C11A C7A 122.3(12) . . ?
C13A C12A N2A 113.0(11) . . ?
C14A C13A C12A 117.2(13) . . ?
C18A C13A C12A 110.4(12) . . ?
C18A C13A C14A 130.7(13) . . ?
C13A C14A C15A 116.2(13) . . ?
C16A C15A C14A 121.9(12) . . ?
C17A C16A C15A 112.1(11) . . ?
C17A C16A C19A 127.7(13) . . ?
C19A C16A C15A 120.0(12) . . ?
C16A C17A C18A 126.2(14) . . ?
C13A C18A C17A 110.3(13) . . ?
C16A C19A N3A 106.1(8) . . ?
N3A C20A C21A 119.5(12) . . ?
C22A C21A C20A 120.3(11) . . ?
C21A C22A C23A 116.2(10) . . ?
C21A C22A C25A 117.8(9) . . ?
C23A C22A C25A 124.8(8) . . ?
C24A C23A C22A 124.3(11) . . ?
N3A C24A C23A 114.5(13) . . ?
C26A C25A C22A 124.0(9) . . ?
C29A C25A C22A 117.8(8) . . ?
C29A C25A C26A 118.1(10) . . ?
C25A C26A C27A 118.4(10) . . ?
N4A C27A C26A 120.9(10) . . ?
N4A C28A C29A 117.7(9) . . ?
C25A C29A C28A 120.2(9) . . ?
C31A C30A N4A 106.3(8) . . ?
C32A C31A C30A 121.0(14) . . ?
C36A C31A C30A 129.3(16) . . ?
C36A C31A C32A 108.8(13) . . ?
C33A C32A C31A 127.3(17) . . ?
C32A C33A C34A 118(2) . . ?
C33A C34A C1A 114(2) . . ?
C35A C34A C1A 128.0(19) . . ?
C35A C34A C33A 116.7(17) . . ?
C36A C35A C34A 121.7(18) . . ?
C35A C36A C31A 128(2) . . ?
C51A O1A C53A 116.6(11) . . ?
C55A O2A C54A 115.4(14) . . ?
C57A O3A C56A 121.1(13) . . ?
C67A O4A C62A 117.9(13) . . ?
C69A O5A C68A 109.4(16) . . ?
C70A O6A C37A 112.7(15) . . ?
C43A N5A C44A 120.6(10) . . ?
C43A N5A C48A 113.8(9) . . ?
C44A N5A C48A 112.6(9) . . ?
C45A N6A C40A 111.9(9) . . ?
C45A N6A C46A 114.7(11) . . ?
C46A N6A C40A 109.4(9) . . ?
O6A C37A C42A 127.2(11) . . ?
C38A C37A O6A 109.4(10) . . ?
C38A C37A C42A 122.9(10) . . ?
C37A C38A C39A 116.0(11) . . ?
C38A C39A C43A 114.3(10) . . ?
C40A C39A C38A 126.2(11) . . ?
C40A C39A C43A 119.1(10) . . ?
C39A C40A N6A 133.4(11) . . ?
C39A C40A C41A 116.5(11) . . ?
C41A C40A N6A 110.1(10) . . ?
C40A C41A C42A 125.3(12) . . ?
C41A C42A C37A 112.5(13) . . ?
N5A C43A C39A 115.2(10) . . ?
N5A C44A C45A 107.3(10) . . ?
N6A C45A C44A 114.4(10) . . ?
C47A C46A N6A 122.3(9) . . ?
C48A C47A C46A 124.3(8) . . ?
C48A C47A C52A 114.4(8) . . ?
C52A C47A C46A 120.3(9) . . ?
C47A C48A N5A 122.3(8) . . ?
C47A C48A C49A 123.1(10) . . ?
C49A C48A N5A 114.4(9) . . ?
C50A C49A C48A 117.6(12) . . ?
C49A C50A C51A 123.9(11) . . ?
O1A C51A C50A 130.2(9) . . ?
O1A C51A C52A 114.8(8) . . ?
C50A C51A C52A 114.9(9) . . ?
C51A C52A C47A 124.9(9) . . ?
O1A C53A C54A 110.0(12) . . ?
O2A C54A C53A 108.4(15) . . ?
O2A C55A C56A 113.9(14) . . ?
O3A C56A C55A 126.9(13) . . ?
O3A C57A C58A 132.5(14) . . ?
O3A C57A C66A 110.4(12) . . ?
C58A C57A C66A 117.1(11) . . ?
C57A C58A C59A 126.4(14) . . ?
C60A C59A C58A 117.6(13) . . ?
C59A C60A C61A 123.6(11) . . ?
C60A C61A C66A 112.3(11) . . ?
C62A C61A C60A 122.5(10) . . ?
C62A C61A C66A 124.9(10) . . ?
O4A C62A C63A 122.3(14) . . ?
C61A C62A O4A 116.7(11) . . ?
C61A C62A C63A 120.8(10) . . ?
C62A C63A C64A 115.6(15) . . ?
C65A C64A C63A 125.6(13) . . ?
C64A C65A C66A 121.4(11) . . ?
C57A C66A C61A 121.5(10) . . ?
C57A C66A C65A 128.6(11) . . ?
C65A C66A C61A 109.6(11) . . ?
O4A C67A C68A 118.3(15) . . ?
O5A C68A C67A 126.6(13) . . ?
O5A C69A C70A 117.4(18) . . ?
O6A C70A C69A 123.8(16) . . ?
F1 P1 F2 176.6(7) . . ?
F1 P1 F3 93.4(6) . . ?
F1 P1 F4 89.4(6) . . ?
F1 P1 F5 85.0(6) . . ?
F1 P1 F6 89.5(6) . . ?
F2 P1 F5 91.7(7) . . ?
F3 P1 F2 89.8(7) . . ?
F3 P1 F5 177.1(6) . . ?
F3 P1 F6 88.7(7) . . ?
F4 P1 F2 89.5(6) . . ?
F4 P1 F3 88.0(7) . . ?
F4 P1 F5 89.6(5) . . ?
F4 P1 F6 176.4(6) . . ?
F6 P1 F2 91.7(5) . . ?
F6 P1 F5 93.7(6) . . ?
F7 P2 F8 176.8(12) . . ?
F7 P2 F10 89.2(9) . . ?
F8 P2 F10 91.1(9) . . ?
F9 P2 F7 95.8(11) . . ?
F9 P2 F8 87.4(10) . . ?
F9 P2 F10 84.8(8) . . ?
F11 P2 F7 94.5(12) . . ?
F11 P2 F8 82.4(12) . . ?
F11 P2 F9 169.6(12) . . ?
F11 P2 F10 97.3(8) . . ?
F12 P2 F7 89.0(8) . . ?
F12 P2 F8 91.2(9) . . ?
F12 P2 F9 89.5(8) . . ?
F12 P2 F10 173.8(9) . . ?
F12 P2 F11 88.7(9) . . ?
F13 P3 F15 98.2(11) . . ?
F14 P3 F13 174.6(16) . . ?
F14 P3 F15 84.6(9) . . ?
F16 P3 F13 85.3(15) . . ?
F16 P3 F14 90.5(12) . . ?
F16 P3 F15 83.2(8) . . ?
F16 P3 F17 100.2(9) . . ?
F17 P3 F13 79.6(11) . . ?
F17 P3 F14 97.8(9) . . ?
F17 P3 F15 175.7(8) . . ?
F18 P3 F13 91.9(18) . . ?
F18 P3 F14 92.4(16) . . ?
F18 P3 F15 95.2(9) . . ?
F18 P3 F16 176.6(17) . . ?
F18 P3 F17 81.2(9) . . ?
F19 P4 F23 90.2(8) . . ?
F20 P4 F19 178.0(8) . . ?
F20 P4 F21 96.3(7) . . ?
F20 P4 F23 87.9(7) . . ?
F21 P4 F19 85.7(7) . . ?
F21 P4 F23 174.0(8) . . ?
F22 P4 F19 83.0(10) . . ?
F22 P4 F20 96.5(10) . . ?
F22 P4 F21 91.2(9) . . ?
F22 P4 F23 92.7(9) . . ?
F24 P4 F19 92.6(12) . . ?
F24 P4 F20 87.9(12) . . ?
F24 P4 F21 88.9(8) . . ?
F24 P4 F22 175.6(12) . . ?
F24 P4 F23 86.9(8) . . ?
F26 P5 F25 179.3(11) . . ?
F26 P5 F28 91.5(9) . . ?
F26 P5 F29 90.6(10) . . ?
F26 P5 F30 89.8(9) . . ?
F27 P5 F25 89.1(10) . . ?
F27 P5 F26 90.6(10) . . ?
F27 P5 F28 89.9(9) . . ?
F27 P5 F29 178.7(12) . . ?
F27 P5 F30 89.4(9) . . ?
F28 P5 F25 89.2(9) . . ?
F28 P5 F29 89.9(9) . . ?
F28 P5 F30 178.5(11) . . ?
F29 P5 F25 89.7(9) . . ?
F29 P5 F30 90.8(9) . . ?
F30 P5 F25 89.5(9) . . ?
F31 P6 F34 89.9(10) . . ?
F31 P6 F35 89.8(11) . . ?
F32 P6 F31 179.4(17) . . ?
F32 P6 F33 90.8(12) . . ?
F32 P6 F34 90.1(9) . . ?
F32 P6 F35 89.6(11) . . ?
F32 P6 F36 89.8(9) . . ?
F33 P6 F31 90(2) . . ?
F33 P6 F34 89.8(9) . . ?
F33 P6 F35 179.3(14) . . ?
F34 P6 F35 89.7(10) . . ?
F36 P6 F31 90.2(9) . . ?
F36 P6 F33 90.6(9) . . ?
F36 P6 F34 179.6(12) . . ?
F36 P6 F35 90.0(9) . . ?
F37 P7 F39 91.1(8) . . ?
F37 P7 F40 89.9(11) . . ?
F37 P7 F41 89.8(9) . . ?
F37 P7 F42 88.1(9) . . ?
F38 P7 F37 177.8(14) . . ?
F38 P7 F39 89.6(9) . . ?
F38 P7 F40 92.1(16) . . ?
F38 P7 F41 89.5(9) . . ?
F38 P7 F42 89.9(11) . . ?
F39 P7 F40 89.8(9) . . ?
F39 P7 F41 179.0(9) . . ?
F39 P7 F42 90.6(9) . . ?
F40 P7 F41 89.7(8) . . ?
F40 P7 F42 178.0(14) . . ?
F42 P7 F41 90.0(9) . . ?
F44 P8 F43 174.8(14) . . ?
F44 P8 F47 86.4(12) . . ?
F45 P8 F43 86.1(11) . . ?
F45 P8 F44 91.3(11) . . ?
F45 P8 F46 92.4(12) . . ?
F45 P8 F47 174.0(12) . . ?
F46 P8 F43 95.9(17) . . ?
F46 P8 F44 88.7(18) . . ?
F46 P8 F47 82.0(14) . . ?
F47 P8 F43 96.6(12) . . ?
F48 P8 F43 87.2(10) . . ?
F48 P8 F44 88.3(12) . . ?
F48 P8 F45 91.9(8) . . ?
F48 P8 F46 174.9(16) . . ?
F48 P8 F47 93.6(10) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.188 0.018 0.750 1192.1 376.4 ?
2 -0.074 0.518 0.250 1192.1 376.4 ?

_olex2_date_sample_data_collection 2021-12-07
_olex2_date_sample_submission    2021-12-06
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id MR572S
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.180
_oxdiff_exptl_absorpt_empirical_full_min 0.545
_vrf_PLAT410_MR572S              
;
PROBLEM: Short Intra H...H Contact  H56A     ..H58      .       1.70 Ang.  
RESPONSE: Hydrogen atoms are refined in riding models. These chains were
somewhat disordered, though modeling the disorder did not help the overall 
structure. This distance should be considered with care.
;
