Solid state supramolecular structure of diketopyrrolopyrrole chromophores: correlating stacking geometry with visible light absorption
Pop, Flavia; Lewis, William; Amabilino, David B.; CrystEngComm 18 (2016) 8933–; doi:10.1039/C6CE02157C

data_7226994
_publ_section_title
;
 Solid state supramolecular structure of diketopyrrolopyrrole
 chromophores: correlating stacking geometry with visible light absorption
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8933
_journal_paper_doi               10.1039/C6CE02157C
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H16 N2 O4 S2'
_chemical_formula_sum            'C19 H16 N2 O4 S2'
_chemical_formula_weight         400.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-05 deposited with the CCDC.
2016-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8547(5)
_cell_length_b                   6.1380(2)
_cell_length_c                   37.0248(12)
_cell_measurement_reflns_used    4553
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8960
_cell_measurement_theta_min      4.7680
_cell_volume                     3603.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   61.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   30.0000 28

  2 omega   47.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -90.0000 51

  3 omega  116.00  162.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -120.0000 46

  4 omega   32.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   90.0000 55

  5 omega   25.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -60.0000 82

  6 omega   24.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0554  -57.0000  -90.0000 42

  7 omega  -22.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0554  -57.0000  -30.0000 32

  8 omega -100.00  -28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -90.0000 72

  9 omega  -77.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000 -150.0000 75

 10 omega  -16.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   30.0000 26

 11 omega   46.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   30.0000 48

 12 omega   55.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 34

 13 omega   39.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  150.0000 31

 14 omega   51.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000    0.0000 45
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0026794000
_diffrn_orient_matrix_UB_12      0.2484643000
_diffrn_orient_matrix_UB_13      0.0057075000
_diffrn_orient_matrix_UB_21      -0.0971059000
_diffrn_orient_matrix_UB_22      -0.0064709000
_diffrn_orient_matrix_UB_23      -0.0006288000
_diffrn_orient_matrix_UB_31      -0.0010609000
_diffrn_orient_matrix_UB_32      -0.0344681000
_diffrn_orient_matrix_UB_33      0.0412268000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13118
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.903
_diffrn_reflns_theta_min         4.778
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.935
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.3256
_exptl_crystal_size_mid          0.0335
_exptl_crystal_size_min          0.0228
_refine_diff_density_max         1.878
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         4898
_refine_ls_number_restraints     2728
_refine_ls_restrained_S_all      1.433
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.1318
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3771
_refine_ls_wR_factor_ref         0.3826
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4608
_reflns_number_total             4898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02157c2.cif
_cod_data_source_block           2C
_cod_depositor_comments
'Adding full bibliography for 7226989--7226997.cif.'
_cod_database_code               7226994
_nottingham_internal_coll_name   OFFPLH
_nottingham_internal_coll_number 14431
_nottingham_internal_coll_client FFP/DBA
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '20.0000, 5.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   27/02/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 18/03/2015
_nottingham_internal_process_user pczfp
_nottingham_internal_solution_date 18/03/2015
_nottingham_internal_solution_user pczfp
_nottingham_internal_refinement_date 18/03/2015
_nottingham_internal_refinement_user pczfp
_nottingham_internal_self_validation_date 16/08/2016
_nottingham_internal_self_validation_user pczfp/pczwl
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C19 H15 N2 O4 S2'
_chemical_oxdiff_usercomment
'OFFPLH #14431 GVB-451 IN FOMBLIN FIML ON A MICROMOUNT kV=45, mA=18'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(9) 0.45(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1A-C15A \\sim N1B-C15B \\sim N1C-C15C \\sim N1D-C15D
 with sigma of 0.02
 S1A-C1A \\sim S1B-C1B \\sim S1C-C1C \\sim S1D-C1D
 with sigma of 0.02
 S1A-C4A \\sim S1B-C4B \\sim S1C-C4C \\sim S1D-C4D
 with sigma of 0.02
 S2A-C11A \\sim S2B-C11B \\sim S2C-C11C \\sim S2D-C11D
 with sigma of 0.02
 S2A-C14A \\sim S2B-C14B \\sim S2C-C14C \\sim S2D-C14D
 with sigma of 0.02
 O1A-C6A \\sim O1B-C6B \\sim O1C-C6C \\sim O1D-C6D
 with sigma of 0.02
 O2A-C9A \\sim O2B-C9B \\sim O2C-C9C \\sim O2D-C9D
 with sigma of 0.02
 O3A-C15A \\sim O3B-C15B \\sim O3C-C15C \\sim O3D-C15D
 with sigma of 0.02
 O4A-C15A \\sim O4B-C15B \\sim O4C-C15C \\sim O4D-C15D
 with sigma of 0.02
 O4A-C16A \\sim O4B-C16B \\sim O4C-C16C \\sim O4D-C16D
 with sigma of 0.02
 N1A-C5A \\sim N1B-C5B \\sim N1C-C5C \\sim N1D-C5D
 with sigma of 0.02
 N1A-C6A \\sim N1B-C6B \\sim N1C-C6C \\sim N1D-C6D
 with sigma of 0.02
 N2A-C9A \\sim N2B-C9B \\sim N2C-C9C \\sim N2D-C9D
 with sigma of 0.02
 N2A-C10A \\sim N2B-C10B \\sim N2C-C10C \\sim N2D-C10D
 with sigma of 0.02
 C1A-C2A \\sim C1B-C2B \\sim C1C-C2C \\sim C1D-C2D
 with sigma of 0.02
 C3A-C2A \\sim C3B-C2B \\sim C3C-C2C \\sim C3D-C2D
 with sigma of 0.02
 C3A-C4A \\sim C3B-C4B \\sim C3C-C4C \\sim C3D-C4D
 with sigma of 0.02
 C5A-C4A \\sim C5B-C4B \\sim C5C-C4C \\sim C5D-C4D
 with sigma of 0.02
 C5A-C7A \\sim C5B-C7B \\sim C5C-C7C \\sim C5D-C7D
 with sigma of 0.02
 C6A-C8A \\sim C6B-C8B \\sim C6C-C8C \\sim C6D-C8D
 with sigma of 0.02
 C7A-C8A \\sim C7B-C8B \\sim C7C-C8C \\sim C7D-C8D
 with sigma of 0.02
 C7A-C9A \\sim C7B-C9B \\sim C7C-C9C \\sim C7D-C9D
 with sigma of 0.02
 C10A-C8A \\sim C10B-C8B \\sim C10C-C8C \\sim C10D-C8D
 with sigma of 0.02
 C10A-C11A \\sim C10B-C11B \\sim C10C-C11C \\sim C10D-C11D
 with sigma of 0.02
 C12A-C11A \\sim C12B-C11B \\sim C12C-C11C \\sim C12D-C11D
 with sigma of 0.02
 C12A-C13A \\sim C12B-C13B \\sim C12C-C13C \\sim C12D-C13D
 with sigma of 0.02
 C14A-C13A \\sim C14B-C13B \\sim C14C-C13C \\sim C14D-C13D
 with sigma of 0.02
 C16A-C17A \\sim C16A-C18A \\sim C16A-C19A \\sim C16B-C17B \\sim C16B-C18B
\\sim C16B-C19B \\sim C16C-
 C17C \\sim C16C-C18C \\sim C16C-C19C \\sim C16D-C17D \\sim C16D-C18D \\sim
C16D-C19D
 with sigma of 0.02
 C17A-C18A \\sim C18A-C19A \\sim C19A-C17A \\sim C17B-C18B \\sim C18B-C19B
\\sim C19B-C17B \\sim C17C-
 C18C \\sim C18C-C19C \\sim C19C-C17C \\sim C17D-C18D \\sim C18D-C19D \\sim
C19D-C17D
 with sigma of 0.02
 C8C-O1C \\sim C8A-O1A \\sim C8D-O1D \\sim C8B-O1B
 with sigma of 0.02
 N1C-O1C \\sim N1A-O1A \\sim N1B-O1B \\sim N1D-O1D
 with sigma of 0.02
4. Restrained planarity
 O1C, O2C, N1C, N2C, C5C, C6C, C7C, C8C, C9C, C10C, C15C, C4C, C11C
 with sigma of 0.1
 C10C, S2C, C11C, C12C, C13C, C14C
 with sigma of 0.1
 S1C, C2C, C1C, C3C, C4C, C5C
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
6. 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
7. Same fragment restrains
{S1A, S2A, O1A, O2A, O3A, O4A, N1A, N2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A,
C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A} sigma for
1-2: 0.01, 1-3: 0.02
as
{S1B, S2B, O1B, O2B, O3B, O4B, N1B, N2B, C1B, C2B, C3B, C4B, C5B, C6B, C7B,
C8B, C9B, C10B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C19B, C18B}
{S1A, S2A, O1A, O2A, O3A, O4A, N1A, N2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A,
C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A} sigma for
1-2: 0.01, 1-3: 0.02
as
{S1C, S2C, O1C, O2C, O3C, O4C, N1C, N2C, C1C, C2C, C3C, C4C, C5C, C6C, C7C,
C8C, C9C, C10C, C11C, C12C, C13C, C14C, C15C, C16C, C17C, C18C, C19C}
{S1A, S2A, O1A, O2A, O3A, O4A, N1A, N2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A,
C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A} sigma for
1-2: 0.01, 1-3: 0.02
as
{S1D, S2D, O1D, O2D, O3D, O4D, N1D, N2D, C1D, C2D, C3D, C4D, C5D, C6D, C7D,
C8D, C9D, C10D, C11D, C12D, C13D, C14D, C15D, C16D, C17D, C18D, C19D}
8. Others
 Sof(S1C)=Sof(S2C)=Sof(O1C)=Sof(O2C)=Sof(O3C)=Sof(O4C)=Sof(N1C)=Sof(N2C)=
 Sof(H2C)=Sof(C1C)=Sof(H1C)=Sof(C2C)=Sof(H2CA)=Sof(C3C)=Sof(H3C)=Sof(C4C)=
 Sof(C5C)=Sof(C6C)=Sof(C7C)=Sof(C8C)=Sof(C9C)=Sof(C10C)=Sof(C11C)=Sof(C12C)=
 Sof(H12C)=Sof(C13C)=Sof(H13C)=Sof(C14C)=Sof(H14C)=Sof(C15C)=Sof(C16C)=
 Sof(C17C)=Sof(H17G)=Sof(H17H)=Sof(H17I)=Sof(C18C)=Sof(H18G)=Sof(H18H)=
 Sof(H18I)=Sof(C19C)=Sof(H19G)=Sof(H19H)=Sof(H19I)=1-FVAR(1)
 Sof(S1A)=Sof(S2A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(N1A)=Sof(N2A)=
 Sof(H2A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(C5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(C16A)=
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(S1D)=Sof(S2D)=Sof(O1D)=Sof(O2D)=Sof(O3D)=Sof(O4D)=Sof(N1D)=Sof(N2D)=
 Sof(H2D)=Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(H2DA)=Sof(C3D)=Sof(H3D)=Sof(C4D)=
 Sof(C5D)=Sof(C6D)=Sof(C7D)=Sof(C8D)=Sof(C9D)=Sof(C10D)=Sof(C11D)=Sof(C12D)=
 Sof(H12D)=Sof(C13D)=Sof(H13D)=Sof(C14D)=Sof(H14D)=Sof(C15D)=Sof(C16D)=
 Sof(C17D)=Sof(H17J)=Sof(H17K)=Sof(H17L)=Sof(C18D)=Sof(H18J)=Sof(H18K)=
 Sof(H18L)=Sof(C19D)=Sof(H19J)=Sof(H19K)=Sof(H19L)=1-FVAR(2)
 Sof(S1B)=Sof(S2B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(N1B)=Sof(N2B)=
 Sof(H2B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(C3B)=Sof(H3B)=Sof(C4B)=
 Sof(C5B)=Sof(C6B)=Sof(C7B)=Sof(C8B)=Sof(C9B)=Sof(C10B)=Sof(C11B)=Sof(C12B)=
 Sof(H12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(C16B)=
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(2)
 U11(S1C)=U11(S2C)=U11(O1C)=U11(O2C)=U11(O3C)=U11(O4C)=U11(N1C)=U11(N2C)=
 U11(C1C)=U11(C2C)=U11(C3C)=U11(C4C)=U11(C5C)=U11(C6C)=U11(C7C)=U11(C8C)=
 U11(C9C)=U11(C10C)=U11(C11C)=U11(C12C)=U11(C13C)=U11(C14C)=U11(C15C)=U11(C16C)=
 U11(C17C)=U11(C18C)=U11(C19C)=FVAR(3)
 U22(S1C)=U22(S2C)=U22(O1C)=U22(O2C)=U22(O3C)=U22(O4C)=U22(N1C)=U22(N2C)=
 U22(C1C)=U22(C2C)=U22(C3C)=U22(C4C)=U22(C5C)=U22(C6C)=U22(C7C)=U22(C8C)=
 U22(C9C)=U22(C10C)=U22(C11C)=U22(C12C)=U22(C13C)=U22(C14C)=U22(C15C)=U22(C16C)=
 U22(C17C)=U22(C18C)=U22(C19C)=FVAR(4)
 U33(S1C)=U33(S2C)=U33(O1C)=U33(O2C)=U33(O3C)=U33(O4C)=U33(N1C)=U33(N2C)=
 U33(C1C)=U33(C2C)=U33(C3C)=U33(C4C)=U33(C5C)=U33(C6C)=U33(C7C)=U33(C8C)=
 U33(C9C)=U33(C10C)=U33(C11C)=U33(C12C)=U33(C13C)=U33(C14C)=U33(C15C)=U33(C16C)=
 U33(C17C)=U33(C18C)=U33(C19C)=FVAR(5)
 U23(S1C)=U23(S2C)=U23(O1C)=U23(O2C)=U23(O3C)=U23(O4C)=U23(N1C)=U23(N2C)=
 U23(C1C)=U23(C2C)=U23(C3C)=U23(C4C)=U23(C5C)=U23(C6C)=U23(C7C)=U23(C8C)=
 U23(C9C)=U23(C10C)=U23(C11C)=U23(C12C)=U23(C13C)=U23(C14C)=U23(C15C)=U23(C16C)=
 U23(C17C)=U23(C18C)=U23(C19C)=FVAR(6)
 U13(S1C)=U13(S2C)=U13(O1C)=U13(O2C)=U13(O3C)=U13(O4C)=U13(N1C)=U13(N2C)=
 U13(C1C)=U13(C2C)=U13(C3C)=U13(C4C)=U13(C5C)=U13(C6C)=U13(C7C)=U13(C8C)=
 U13(C9C)=U13(C10C)=U13(C11C)=U13(C12C)=U13(C13C)=U13(C14C)=U13(C15C)=U13(C16C)=
 U13(C17C)=U13(C18C)=U13(C19C)=FVAR(7)
 U12(S1C)=U12(S2C)=U12(O1C)=U12(O2C)=U12(O3C)=U12(O4C)=U12(N1C)=U12(N2C)=
 U12(C1C)=U12(C2C)=U12(C3C)=U12(C4C)=U12(C5C)=U12(C6C)=U12(C7C)=U12(C8C)=
 U12(C9C)=U12(C10C)=U12(C11C)=U12(C12C)=U12(C13C)=U12(C14C)=U12(C15C)=U12(C16C)=
 U12(C17C)=U12(C18C)=U12(C19C)=FVAR(8)
 U11(S1D)=U11(S2D)=U11(O1D)=U11(O2D)=U11(O3D)=U11(O4D)=U11(N1D)=U11(N2D)=
 U11(C1D)=U11(C2D)=U11(C3D)=U11(C4D)=U11(C5D)=U11(C6D)=U11(C7D)=U11(C8D)=
 U11(C9D)=U11(C10D)=U11(C11D)=U11(C12D)=U11(C13D)=U11(C14D)=U11(C15D)=U11(C16D)=
 U11(C17D)=U11(C18D)=U11(C19D)=FVAR(9)
 U22(S1D)=U22(S2D)=U22(O1D)=U22(O2D)=U22(O3D)=U22(O4D)=U22(N1D)=U22(N2D)=
 U22(C1D)=U22(C2D)=U22(C3D)=U22(C4D)=U22(C5D)=U22(C6D)=U22(C7D)=U22(C8D)=
 U22(C9D)=U22(C10D)=U22(C11D)=U22(C12D)=U22(C13D)=U22(C14D)=U22(C15D)=U22(C16D)=
 U22(C17D)=U22(C18D)=U22(C19D)=FVAR(10)
 U33(S1D)=U33(S2D)=U33(O1D)=U33(O2D)=U33(O3D)=U33(O4D)=U33(N1D)=U33(N2D)=
 U33(C1D)=U33(C2D)=U33(C3D)=U33(C4D)=U33(C5D)=U33(C6D)=U33(C7D)=U33(C8D)=
 U33(C9D)=U33(C10D)=U33(C11D)=U33(C12D)=U33(C13D)=U33(C14D)=U33(C15D)=U33(C16D)=
 U33(C17D)=U33(C18D)=U33(C19D)=FVAR(11)
 U23(S1D)=U23(S2D)=U23(O1D)=U23(O2D)=U23(O3D)=U23(O4D)=U23(N1D)=U23(N2D)=
 U23(C1D)=U23(C2D)=U23(C3D)=U23(C4D)=U23(C5D)=U23(C6D)=U23(C7D)=U23(C8D)=
 U23(C9D)=U23(C10D)=U23(C11D)=U23(C12D)=U23(C13D)=U23(C14D)=U23(C15D)=U23(C16D)=
 U23(C17D)=U23(C18D)=U23(C19D)=FVAR(12)
 U13(S1D)=U13(S2D)=U13(O1D)=U13(O2D)=U13(O3D)=U13(O4D)=U13(N1D)=U13(N2D)=
 U13(C1D)=U13(C2D)=U13(C3D)=U13(C4D)=U13(C5D)=U13(C6D)=U13(C7D)=U13(C8D)=
 U13(C9D)=U13(C10D)=U13(C11D)=U13(C12D)=U13(C13D)=U13(C14D)=U13(C15D)=U13(C16D)=
 U13(C17D)=U13(C18D)=U13(C19D)=FVAR(13)
 U12(S1D)=U12(S2D)=U12(O1D)=U12(O2D)=U12(O3D)=U12(O4D)=U12(N1D)=U12(N2D)=
 U12(C1D)=U12(C2D)=U12(C3D)=U12(C4D)=U12(C5D)=U12(C6D)=U12(C7D)=U12(C8D)=
 U12(C9D)=U12(C10D)=U12(C11D)=U12(C12D)=U12(C13D)=U12(C14D)=U12(C15D)=U12(C16D)=
 U12(C17D)=U12(C18D)=U12(C19D)=FVAR(14)
9.a Me refined with riding coordinates:
 C17C(H17G,H17H,H17I), C18C(H18G,H18H,H18I), C19C(H19G,H19H,H19I), C17D(H17J,
 H17K,H17L), C18D(H18J,H18K,H18L), C19D(H19J,H19K,H19L)
9.b Aromatic/amide H refined with riding coordinates:
 N2A(H2A), C1A(H1A), C2A(H2AA), C3A(H3A), C12A(H12A), C13A(H13A), C14A(H14A),
 N2B(H2B), C1B(H1B), C2B(H2BA), C3B(H3B), C12B(H12B), C13B(H13B), C14B(H14B),
 N2C(H2C), C1C(H1C), C2C(H2CA), C3C(H3C), C12C(H12C), C13C(H13C), C14C(H14C),
 N2D(H2D), C1D(H1D), C2D(H2DA), C3D(H3D), C12D(H12D), C13D(H13D), C14D(H14D)
9.c Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C17B(H17D,
 H17E,H17F), C19B(H19D,H19E,H19F), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              82218
_olex2_date_sample_data_collection 2015-02-27
_olex2_date_sample_submission    2015-02-04
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'