 
data_rb51num-sr
# Crystallography Linda JW Shimon
# Angelica Elkin Boris Rybchinski
 
_audit_creation_method            'SHELXL-2016/4'
_shelx_SHELXL_version_number      '2016/4'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C34 H24 N4 O8'
_chemical_formula_sum
 'C34 H24 N4 O8' 
_chemical_formula_weight          616.57

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            9
_space_group_name_H-M_alt         'C c'
_space_group_name_Hall            'C -2yc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'
 
_cell_length_a                    24.7983(2)
_cell_length_b                    10.67570(10)
_cell_length_c                    12.30660(10)
_cell_angle_alpha                 90
_cell_angle_beta                  101.7370(10)
_cell_angle_gamma                 90
_cell_volume                      3189.92(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used   21533
_cell_measurement_theta_min     4.5360
_cell_measurement_theta_max     79.5640
 
_exptl_crystal_description        prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.284          
_exptl_crystal_F_000              1280
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.146
_exptl_crystal_size_mid           0.061
_exptl_crystal_size_min           0.053
_exptl_absorpt_coefficient_mu     0.777
_shelx_estimated_absorpt_T_min    0.895
_shelx_estimated_absorpt_T_max    0.960
_exptl_absorpt_correction_T_min                   0.64697
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min           0.741
_oxdiff_exptl_absorpt_empirical_full_max           1.364
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type   'Rigaku XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             30078
_diffrn_reflns_av_unetI/netI      0.0236
_diffrn_reflns_av_R_equivalents   0.0404
_diffrn_reflns_limit_h_min        -31
_diffrn_reflns_limit_h_max        31
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          4.524
_diffrn_reflns_theta_max          80.016
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.983
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.983
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.983
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              5478
_reflns_number_gt                 5251
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.998
_reflns_Friedel_fraction_max      0.983
_reflns_Friedel_fraction_full     0.993
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXT-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1672P)²+2.5136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.9(5)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          5478
_refine_ls_number_parameters      530
_refine_ls_number_restraints      45
_refine_ls_R_factor_all           0.0835
_refine_ls_R_factor_gt            0.0813
_refine_ls_wR_factor_ref          0.2455
_refine_ls_wR_factor_gt           0.2421
_refine_ls_goodness_of_fit_ref    1.075
_refine_ls_restrained_S_all       1.079
_refine_ls_shift/su_max           0.015
_refine_ls_shift/su_mean          0.003
 
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 0.43743(16) 0.8583(6) -0.0143(4) 0.0817(18) Uani 1 1 d . . . . .
O2 O 0.29059(14) 0.7785(4) 0.1441(3) 0.0504(9) Uani 1 1 d . . . . .
O3 O 0.72043(15) 0.7771(4) 0.8338(3) 0.0560(10) Uani 1 1 d . . . . .
O4 O 0.57512(18) 0.8853(5) 0.9858(4) 0.0666(12) Uani 1 1 d . . . . .
N3 N 0.3685(3) 0.7282(8) 0.5591(7) 0.0534(18) Uani 0.611(5) 1 d . . P A 1
O5 O 0.3881(3) 0.6396(6) 0.6143(6) 0.0566(16) Uani 0.611(5) 1 d . . P A 1
O6 O 0.3276(3) 0.7838(7) 0.5729(6) 0.0610(19) Uani 0.611(5) 1 d . . P A 1
N4 N 0.6068(2) 0.8226(7) 0.2852(6) 0.0424(16) Uani 0.611(5) 1 d . . P A 3
O7 O 0.6317(2) 0.9164(6) 0.3136(5) 0.0480(14) Uani 0.611(5) 1 d . . P A 3
O8 O 0.6278(2) 0.7276(7) 0.2544(6) 0.0533(15) Uani 0.611(5) 1 d . . P A 3
N5 N 0.4056(4) 0.8293(9) 0.6882(7) 0.034(2) Uani 0.389(5) 1 d . . P A 2
O9 O 0.3870(4) 0.7408(9) 0.7282(7) 0.043(2) Uani 0.389(5) 1 d . . P . .
O10 O 0.3821(3) 0.9317(9) 0.6593(8) 0.047(2) Uani 0.389(5) 1 d . . P . .
N6 N 0.6454(3) 0.7220(8) 0.4192(7) 0.0297(19) Uani 0.389(5) 1 d . . P A 4
O11 O 0.6862(4) 0.7752(11) 0.4042(10) 0.057(3) Uani 0.389(5) 1 d . . P A 4
O12 O 0.6251(4) 0.6348(8) 0.3622(9) 0.048(2) Uani 0.389(5) 1 d . . P A 4
N1 N 0.36382(15) 0.8099(4) 0.0616(3) 0.0394(9) Uani 1 1 d . . . . .
N2 N 0.64827(17) 0.8200(5) 0.9155(4) 0.0465(10) Uani 1 1 d . . . . .
C1 C 0.39136(19) 0.7605(5) 0.4617(4) 0.0421(11) Uani 1 1 d . . . . .
C2 C 0.3570(2) 0.7594(5) 0.3558(5) 0.0464(11) Uani 1 1 d . . . . .
H2 H 0.318973 0.740430 0.347821 0.056 Uiso 1 1 calc R U . . .
C3 C 0.37833(19) 0.7857(5) 0.2641(4) 0.0382(10) Uani 1 1 d . . . . .
C4 C 0.45601(18) 0.8208(5) 0.1786(4) 0.0392(10) Uani 1 1 d . . . . .
C5 C 0.5119(2) 0.8335(8) 0.1864(4) 0.0582(15) Uani 1 1 d . . . . .
H5 H 0.526472 0.849295 0.122104 0.070 Uiso 1 1 calc R U . . .
C6 C 0.54725(18) 0.8227(5) 0.2918(4) 0.0447(11) Uani 1 1 d . . . . .
C7 C 0.62043(19) 0.7563(5) 0.5152(4) 0.0390(10) Uani 1 1 d . . . . .
C8 C 0.65531(15) 0.7566(5) 0.6187(4) 0.0392(10) Uani 1 1 d . . . . .
H8 H 0.693142 0.736180 0.625716 0.047 Uiso 1 1 calc R U . . .
C9 C 0.63455(18) 0.7871(5) 0.7123(4) 0.0399(10) Uani 1 1 d . . . . .
C10 C 0.5559(2) 0.8417(5) 0.7949(5) 0.0459(11) Uani 1 1 d . . . . .
C11 C 0.50013(19) 0.8585(6) 0.7845(4) 0.0522(14) Uani 1 1 d . . . . .
H11 H 0.485662 0.880822 0.847590 0.063 Uiso 1 1 calc R U . . .
C12 C 0.46507(19) 0.8431(6) 0.6831(5) 0.0487(12) Uani 1 1 d . . . . .
C13 C 0.34177(19) 0.7901(5) 0.1541(4) 0.0438(11) Uani 1 1 d . . . . .
C14 C 0.4188(2) 0.8319(7) 0.0669(5) 0.0555(15) Uani 1 1 d . . . . .
C15 C 0.3261(3) 0.8185(7) -0.0494(6) 0.0644(11) Uani 1 1 d . . . . .
C16 C 0.3235(8) 0.9507(15) -0.0948(18) 0.037(5) Uani 0.237(18) 1 d . U P B 1
H16A H 0.350820 0.962990 -0.142305 0.045 Uiso 0.237(18) 1 calc R U P B 1
H16B H 0.330341 1.012918 -0.033905 0.045 Uiso 0.237(18) 1 calc R U P B 1
C17 C 0.2565(8) 0.9640(18) -0.1723(17) 0.026(4) Uani 0.237(18) 1 d . U P B 1
H17A H 0.257688 0.981533 -0.249902 0.039 Uiso 0.237(18) 1 calc R U P B 1
H17B H 0.237476 1.032495 -0.142578 0.039 Uiso 0.237(18) 1 calc R U P B 1
H17C H 0.236623 0.885381 -0.167843 0.039 Uiso 0.237(18) 1 calc R U P B 1
C86 C 0.2904(4) 0.9396(8) -0.0543(8) 0.062(2) Uani 0.763(18) 1 d . U P B 2
H86A H 0.312221 1.010583 -0.016476 0.075 Uiso 0.763(18) 1 calc R U P B 2
H86B H 0.257884 0.925878 -0.020675 0.075 Uiso 0.763(18) 1 calc R U P B 2
C87 C 0.2721(6) 0.9638(11) -0.1916(10) 0.066(3) Uani 0.763(18) 1 d . U P B 2
H87A H 0.301022 0.932280 -0.227961 0.099 Uiso 0.763(18) 1 calc R U P B 2
H87B H 0.266899 1.053691 -0.206096 0.099 Uiso 0.763(18) 1 calc R U P B 2
H87C H 0.237543 0.919510 -0.220772 0.099 Uiso 0.763(18) 1 calc R U P B 2
C18 C 0.2947(3) 0.6964(6) -0.0830(6) 0.0644(11) Uani 1 1 d D . . . .
H18A H 0.268584 0.681890 -0.033227 0.077 Uiso 1 1 calc R U . . .
H18B H 0.273000 0.704895 -0.159594 0.077 Uiso 1 1 calc R U . . .
C19 C 0.3328(5) 0.5833(8) -0.0775(8) 0.125(5) Uani 1 1 d D . . . .
H19A H 0.360375 0.599439 -0.122709 0.187 Uiso 1 1 calc R U . . .
H19B H 0.311160 0.509226 -0.106028 0.187 Uiso 1 1 calc R U . . .
H19C H 0.351377 0.568702 -0.000366 0.187 Uiso 1 1 calc R U . . .
C20 C 0.43547(19) 0.8019(5) 0.2759(4) 0.0384(10) Uani 1 1 d . . . . .
C21 C 0.47113(17) 0.8006(4) 0.3806(4) 0.0335(9) Uani 1 1 d . . . . .
C22 C 0.44713(19) 0.7890(4) 0.4787(4) 0.0376(10) Uani 1 1 d . . . . .
C23 C 0.52928(17) 0.8043(4) 0.3887(4) 0.0360(10) Uani 1 1 d . . . . .
C24 C 0.67223(18) 0.7934(5) 0.8233(4) 0.0403(10) Uani 1 1 d . . . . .
C25 C 0.5922(2) 0.8506(5) 0.9054(4) 0.0445(11) Uani 1 1 d . . . . .
C26 C 0.68554(17) 0.8222(4) 1.0276(4) 0.0339(8) Uani 1 1 d . . . . .
C31 C 0.57758(18) 0.8105(4) 0.7010(4) 0.0365(9) Uani 1 1 d . . . . .
C32 C 0.54223(18) 0.8031(4) 0.5950(4) 0.0361(10) Uani 1 1 d . . . . .
C33 C 0.56514(17) 0.7876(4) 0.4980(4) 0.0335(9) Uani 1 1 d . . . . .
C34 C 0.48387(18) 0.8116(5) 0.5861(4) 0.0377(10) Uani 1 1 d . . . . .
C28 C 0.7406(7) 0.9675(15) 1.1704(14) 0.041(4) Uani 0.45(2) 1 d . U P C 5
H28A H 0.721424 0.911263 1.212851 0.062 Uiso 0.45(2) 1 calc R U P C 5
H28B H 0.732470 1.054644 1.186319 0.062 Uiso 0.45(2) 1 calc R U P C 5
H28C H 0.780352 0.953008 1.191372 0.062 Uiso 0.45(2) 1 calc R U P C 5
C27 C 0.7197(4) 0.9402(8) 1.0378(8) 0.034(3) Uani 0.45(2) 1 d . . P C 5
H27A H 0.697256 1.011120 1.001640 0.040 Uiso 0.45(2) 1 calc R U P C 5
H27B H 0.751592 0.928901 1.001876 0.040 Uiso 0.45(2) 1 calc R U P C 5
C98 C 0.7540(8) 0.966(2) 1.1453(16) 0.062(5) Uani 0.55(2) 1 d . . P C 6
H98A H 0.767816 0.881885 1.168948 0.094 Uiso 0.55(2) 1 calc R U P C 6
H98B H 0.754721 1.018348 1.210794 0.094 Uiso 0.55(2) 1 calc R U P C 6
H98C H 0.777467 1.003087 1.098788 0.094 Uiso 0.55(2) 1 calc R U P C 6
C97 C 0.6921(4) 0.9552(9) 1.0757(9) 0.048(3) Uani 0.55(2) 1 d . . P C 6
H97A H 0.665468 0.969814 1.124438 0.057 Uiso 0.55(2) 1 calc R U P C 6
H97B H 0.685421 1.018063 1.015251 0.057 Uiso 0.55(2) 1 calc R U P C 6
C30 C 0.6651(15) 0.597(4) 1.063(4) 0.056(7) Uani 0.318(17) 1 d . U P C 5
H30A H 0.634825 0.639951 1.087200 0.084 Uiso 0.318(17) 1 calc R U P C 5
H30B H 0.679789 0.531036 1.116291 0.084 Uiso 0.318(17) 1 calc R U P C 5
H30C H 0.651491 0.558817 0.989747 0.084 Uiso 0.318(17) 1 calc R U P C 5
C29 C 0.7194(7) 0.7084(12) 1.0533(14) 0.044(4) Uani 0.318(17) 1 d . U P C 5
H29A H 0.746342 0.716143 1.124308 0.053 Uiso 0.318(17) 1 calc R U P C 5
H29B H 0.738808 0.686800 0.993068 0.053 Uiso 0.318(17) 1 calc R U P C 5
C90 C 0.6797(11) 0.5848(19) 1.0419(18) 0.082(6) Uani 0.682(17) 1 d . . P C 6
H90A H 0.654172 0.580212 0.969904 0.124 Uiso 0.682(17) 1 calc R U P C 6
H90B H 0.673021 0.514215 1.088307 0.124 Uiso 0.682(17) 1 calc R U P C 6
H90C H 0.717703 0.580999 1.030576 0.124 Uiso 0.682(17) 1 calc R U P C 6
C99 C 0.6697(4) 0.7245(7) 1.1071(7) 0.055(2) Uani 0.682(17) 1 d . . P C 6
H99A H 0.630841 0.734250 1.114125 0.067 Uiso 0.682(17) 1 calc R U P C 6
H99B H 0.693851 0.730184 1.181648 0.067 Uiso 0.682(17) 1 calc R U P C 6
 
 
_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 C14 1.216(7) . ?
O2 C13 1.256(6) . ?
O3 C24 1.189(6) . ?
O4 C25 1.211(7) . ?
N3a O5 1.208(10) . ?
N3a O6 1.217(10) . ?
N3a C1 1.467(9) . ?
O5a O9 1.775(12) . ?
N4c O7 1.191(9) . ?
N4c O8 1.234(10) . ?
N4c C6 1.495(7) . ?
N5b O9 1.201(13) . ?
N5b O10 1.255(13) . ?
N5b C12 1.496(10) . ?
N6d O11 1.206(14) . ?
N6d O12 1.213(13) . ?
N6d C7 1.487(8) . ?
N1 C14 1.372(6) . ?
N1 C13 1.375(6) . ?
N1 C15 1.494(8) . ?
N2 C25 1.408(6) . ?
N2 C24 1.413(7) . ?
N2 C26 1.496(6) . ?
C1 C22 1.390(7) . ?
C1 C2 1.404(8) . ?
C2 C3 1.369(7) . ?
C2 H2 0.9500 . ?
C3 C20 1.406(6) . ?
C3 C13 1.469(7) . ?
C4 C5 1.376(7) . ?
C4 C20 1.407(6) . ?
C4 C14 1.496(7) . ?
C5 C6 1.414(7) . ?
C5 H5 0.9500 . ?
C6 C23 1.370(6) . ?
C7 C33 1.385(6) . ?
C7 C8 1.387(7) . ?
C8 C9 1.393(6) . ?
C8 H8 0.9500 . ?
C9 C31 1.413(6) . ?
C9 C24 1.492(7) . ?
C10 C11 1.373(6) . ?
C10 C31 1.411(7) . ?
C10 C25 1.474(7) . ?
C11 C12 1.378(7) . ?
C11 H11 0.9500 . ?
C12 C34 1.408(7) . ?
C15 C16 1.514(18) . ?
C15 C18 1.532(10) . ?
C15 C86 1.560(11) . ?
C16a C17 1.74(3) . ?
C16a H16A 0.9900 . ?
C16a H16B 0.9900 . ?
C17a H17A 0.9800 . ?
C17a H17B 0.9800 . ?
C17a H17C 0.9800 . ?
C86b C87 1.678(15) . ?
C86b H86A 0.9900 . ?
C86b H86B 0.9900 . ?
C87b H87A 0.9800 . ?
C87b H87B 0.9800 . ?
C87b H87C 0.9800 . ?
C18 C19 1.526(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.407(6) . ?
C21 C23 1.426(6) . ?
C21 C22 1.457(6) . ?
C22 C34 1.464(7) . ?
C23 C33 1.465(6) . ?
C26 C29 1.474(14) . ?
C26 C27 1.507(10) . ?
C26 C97 1.534(11) . ?
C26 C99 1.536(9) . ?
C31 C32 1.418(7) . ?
C32 C34 1.432(6) . ?
C32 C33 1.432(6) . ?
C28e C27 1.634(18) . ?
C28e H28A 0.9800 . ?
C28e H28B 0.9800 . ?
C28e H28C 0.9800 . ?
C27e H27A 0.9900 . ?
C27e H27B 0.9900 . ?
C98f C97 1.60(2) . ?
C98f H98A 0.9800 . ?
C98f H98B 0.9800 . ?
C98f H98C 0.9800 . ?
C97f H97A 0.9900 . ?
C97f H97B 0.9900 . ?
C30e C29 1.82(4) . ?
C30e H30A 0.9800 . ?
C30e H30B 0.9800 . ?
C30e H30C 0.9800 . ?
C29e H29A 0.9900 . ?
C29e H29B 0.9900 . ?
C90f C99 1.74(2) . ?
C90f H90A 0.9800 . ?
C90f H90B 0.9800 . ?
C90f H90C 0.9800 . ?
C99f H99A 0.9900 . ?
C99f H99B 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
O5a N3a O6 123.7(8) . . ?
O5a N3a C1 117.7(7) . . ?
O6a N3a C1 118.1(7) . . ?
N3a O5a O9 84.2(6) . . ?
O7c N4c O8 123.7(6) . . ?
O7c N4c C6 116.3(6) . . ?
O8c N4c C6 120.0(6) . . ?
O9 N5b O10 127.3(10) . . ?
O9 N5b C12 124.0(9) . . ?
O10 N5b C12 107.9(8) . . ?
O11d N6d O12 122.4(9) . . ?
O11d N6d C7 120.2(8) . . ?
O12d N6d C7 117.3(8) . . ?
C14 N1 C13 123.1(4) . . ?
C14 N1 C15 117.6(5) . . ?
C13 N1 C15 119.1(4) . . ?
C25 N2 C24 123.0(4) . . ?
C25 N2 C26 119.5(4) . . ?
C24 N2 C26 117.5(4) . . ?
C22 C1 C2 122.6(5) . . ?
C22 C1 N3 117.8(5) . . ?
C2 C1 N3 119.6(5) . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C20 119.4(5) . . ?
C2 C3 C13 119.8(4) . . ?
C20 C3 C13 120.7(4) . . ?
C5 C4 C20 119.2(4) . . ?
C5 C4 C14 118.7(4) . . ?
C20 C4 C14 122.0(4) . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C23 C6 C5 124.0(4) . . ?
C23 C6 N4 123.2(5) . . ?
C5 C6 N4 112.7(5) . . ?
C33 C7 C8 123.6(4) . . ?
C33 C7 N6 119.8(5) . . ?
C8 C7 N6 116.6(5) . . ?
C7 C8 C9 119.6(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C31 119.3(4) . . ?
C8 C9 C24 120.0(4) . . ?
C31 C9 C24 120.7(4) . . ?
C11 C10 C31 119.9(5) . . ?
C11 C10 C25 119.5(5) . . ?
C31 C10 C25 120.5(4) . . ?
C10 C11 C12 120.4(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C34 122.7(4) . . ?
C11 C12 N5 114.8(5) . . ?
C34 C12 N5 120.8(6) . . ?
O2 C13 N1 119.9(5) . . ?
O2 C13 C3 120.6(4) . . ?
N1 C13 C3 119.5(4) . . ?
O1 C14 N1 122.7(5) . . ?
O1 C14 C4 120.5(5) . . ?
N1 C14 C4 116.8(4) . . ?
N1 C15 C16 111.5(8) . . ?
N1 C15 C18 112.5(5) . . ?
C16a C15 C18 135.4(9) . . ?
N1 C15 C86 109.3(6) . . ?
C18 C15 C86 116.2(6) . . ?
C15 C16a C17 104.0(13) . . ?
C15 C16a H16A 111.0 . . ?
C17a C16a H16A 111.0 . . ?
C15 C16a H16B 111.0 . . ?
C17a C16a H16B 110.9 . . ?
H16Aa C16a H16B 109.0 . . ?
C16a C17a H17A 109.5 . . ?
C16a C17a H17B 109.5 . . ?
H17Aa C17a H17B 109.5 . . ?
C16a C17a H17C 109.5 . . ?
H17Aa C17a H17C 109.5 . . ?
H17Ba C17a H17C 109.5 . . ?
C15 C86b C87 101.6(7) . . ?
C15 C86b H86A 111.4 . . ?
C87b C86b H86A 111.4 . . ?
C15 C86b H86B 111.4 . . ?
C87b C86b H86B 111.4 . . ?
H86Ab C86b H86B 109.3 . . ?
C86b C87b H87A 109.5 . . ?
C86b C87b H87B 109.5 . . ?
H87Ab C87b H87B 109.5 . . ?
C86b C87b H87C 109.5 . . ?
H87Ab C87b H87C 109.5 . . ?
H87Bb C87b H87C 109.5 . . ?
C19 C18 C15 112.7(7) . . ?
C19 C18 H18A 109.1 . . ?
C15 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C15 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 C21 121.7(4) . . ?
C3 C20 C4 117.5(4) . . ?
C21 C20 C4 120.8(4) . . ?
C20 C21 C23 120.1(4) . . ?
C20 C21 C22 118.3(4) . . ?
C23 C21 C22 121.5(4) . . ?
C1 C22 C21 117.1(4) . . ?
C1 C22 C34 126.2(4) . . ?
C21 C22 C34 116.7(4) . . ?
C6 C23 C21 116.5(4) . . ?
C6 C23 C33 124.9(4) . . ?
C21 C23 C33 118.5(4) . . ?
O3 C24 N2 121.3(5) . . ?
O3 C24 C9 121.4(5) . . ?
N2 C24 C9 117.2(4) . . ?
O4 C25 N2 120.1(5) . . ?
O4 C25 C10 121.6(5) . . ?
N2 C25 C10 118.3(4) . . ?
C29e C26 N2 113.8(7) . . ?
C29e C26 C27 112.7(8) . . ?
N2 C26 C27 108.8(5) . . ?
N2 C26 C97 111.5(5) . . ?
N2 C26 C99 112.7(4) . . ?
C97f C26 C99 113.8(6) . . ?
C10 C31 C9 120.1(5) . . ?
C10 C31 C32 119.9(4) . . ?
C9 C31 C32 120.0(4) . . ?
C31 C32 C34 119.5(4) . . ?
C31 C32 C33 119.8(4) . . ?
C34 C32 C33 120.6(4) . . ?
C7 C33 C32 116.7(4) . . ?
C7 C33 C23 124.5(4) . . ?
C32 C33 C23 118.8(3) . . ?
C12 C34 C32 117.0(4) . . ?
C12 C34 C22 123.5(4) . . ?
C32 C34 C22 119.5(4) . . ?
C27e C28e H28A 109.5 . . ?
C27e C28e H28B 109.5 . . ?
H28Ae C28e H28B 109.5 . . ?
C27e C28e H28C 109.5 . . ?
H28Ae C28e H28C 109.5 . . ?
H28Be C28e H28C 109.5 . . ?
C26 C27e C28 107.0(9) . . ?
C26 C27e H27A 110.3 . . ?
C28e C27e H27A 110.3 . . ?
C26 C27e H27B 110.3 . . ?
C28e C27e H27B 110.3 . . ?
H27Ae C27e H27B 108.6 . . ?
C97f C98f H98A 109.5 . . ?
C97f C98f H98B 109.5 . . ?
H98Af C98f H98B 109.5 . . ?
C97f C98f H98C 109.5 . . ?
H98Af C98f H98C 109.5 . . ?
H98Bf C98f H98C 109.5 . . ?
C26 C97f C98 106.5(10) . . ?
C26 C97f H97A 110.4 . . ?
C98f C97f H97A 110.4 . . ?
C26 C97f H97B 110.4 . . ?
C98f C97f H97B 110.4 . . ?
H97Af C97f H97B 108.6 . . ?
C29e C30e H30A 109.5 . . ?
C29e C30e H30B 109.5 . . ?
H30Ae C30e H30B 109.5 . . ?
C29e C30e H30C 109.5 . . ?
H30Ae C30e H30C 109.5 . . ?
H30Be C30e H30C 109.5 . . ?
C26 C29e C30 99.1(16) . . ?
C26 C29e H29A 112.0 . . ?
C30e C29e H29A 112.0 . . ?
C26 C29e H29B 111.9 . . ?
C30e C29e H29B 111.9 . . ?
H29Ae C29e H29B 109.6 . . ?
C99f C90f H90A 109.5 . . ?
C99f C90f H90B 109.5 . . ?
H90Af C90f H90B 109.5 . . ?
C99f C90f H90C 109.5 . . ?
H90Af C90f H90C 109.5 . . ?
H90Bf C90f H90C 109.5 . . ?
C26 C99f C90 102.1(9) . . ?
C26 C99f H99A 111.4 . . ?
C90f C99f H99A 111.4 . . ?
C26 C99f H99B 111.4 . . ?
C90f C99f H99B 111.3 . . ?
H99Af C99f H99B 109.2 . . ?
 
_refine_diff_density_max    0.424
_refine_diff_density_min   -0.485
_refine_diff_density_rms    0.079



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr                          
  _platon_squeeze_void_average_x                   
  _platon_squeeze_void_average_y                   
  _platon_squeeze_void_average_z                   
  _platon_squeeze_void_volume                      
  _platon_squeeze_void_count_electrons             
  _platon_squeeze_void_content                     
   1  0.006 -0.000  0.003       206        71 ' '
   2  0.506  0.500  0.466       206        71 ' '
_platon_squeeze_details                          
;
;
# start Validation Reply Form
_vrf_PLAT990_rb51num-sr
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note 
RESPONSE: Shelxl-2016/4 was used
;
# end Validation Reply Form
