Azulene revisited: solid-state structure, invariom modeling and lattice-energy minimization of a classical example of disorder
Dittrich, B.; Fabbiani, F. P. A.; Henn, J.; Schmidt, M. U.; Macchi, P.; Meindl, K.; Spackman, M. A.; Acta Crystallographica Section B 74 (2018) –; doi:10.1107/S2052520618010120

data_2108280
_publ_contact_author
;
Dittrich, Birger, Institute of inorganic chemistry,
Georg-August-University Goettingen, Tammannstr. 4,
D-37077 Goettingen, Germany.
;
_publ_section_title
;
 Azulene revisited: solid-state structure, invariom modeling and
 lattice-energy minimization of a classical example of disorder
;
_journal_coeditor_code           WF5141SUP1
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520618010120
_journal_volume                  74
_journal_year                    2018
_chemical_compound_source        ' Sigma Aldrich '
_chemical_formula_moiety         'C10 H8'
_chemical_formula_sum            'C10 H8'
_chemical_formula_weight         128.16
_chemical_name_systematic        azulene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2011-12-12T12:21:38-00:00
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 100.411(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7154(2)
_cell_length_b                   5.9019(1)
_cell_length_c                   7.6969(2)
_cell_measurement_reflns_used    15500
_cell_measurement_temperature    100
_cell_measurement_theta_max      52.154
_cell_measurement_theta_min      3.4314
_cell_volume                     344.712(14)
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'Koritsanszky et al, (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 97.6
_diffrn_measurement_details
;
  1 omega   23.00   66.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -2.9400   45.0000  240.0000    0.0000    0.0000 43

  2 omega  -70.00  -23.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -2.9400  -75.0000    0.0000    0.0000    0.0000 47

  3 omega  -21.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -45.0000  120.0000    0.0000    0.0000 43

  4 omega  -64.00  -21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -45.0000  120.0000    0.0000    0.0000 43

  5 omega   30.00   73.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440   45.0000    0.0000    0.0000    0.0000 43

  6 omega  -21.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -45.0000    0.0000    0.0000    0.0000 43

  7 omega  -21.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -45.0000  240.0000    0.0000    0.0000 43

  8 omega  -16.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -75.0000  120.0000    0.0000    0.0000 46

  9 omega  -64.00  -21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -45.0000  240.0000    0.0000    0.0000 43

 10 omega  -16.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440  -75.0000  240.0000    0.0000    0.0000 46

 11 omega   11.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -75.0000  240.0000    0.0000    0.0000 47

 12 omega  105.00  147.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   50.0000  250.0000    0.0000    0.0000 42

 13 omega    9.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -111.0000   82.0000    0.0000    0.0000 54

 14 omega  105.00  147.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   52.0000  118.0000    0.0000    0.0000 42

 15 omega   53.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -45.0000  240.0000    0.0000    0.0000 43

 16 omega   53.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -45.0000    0.0000    0.0000    0.0000 43

 17 omega   63.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -111.0000   82.0000    0.0000    0.0000 53

 18 omega   64.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -118.0000   31.0000    0.0000    0.0000 54

 19 omega   61.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   61.0000  -76.0000    0.0000    0.0000 43

 20 omega   53.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -45.0000  120.0000    0.0000    0.0000 43

 21 omega   11.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -75.0000    0.0000    0.0000    0.0000 47

 22 omega  104.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   61.0000  163.0000    0.0000    0.0000 42

 23 omega   61.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   61.0000  163.0000    0.0000    0.0000 43

 24 omega  104.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   59.0000  224.0000    0.0000    0.0000 42

 25 omega   11.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -75.0000  120.0000    0.0000    0.0000 47

 26 omega   58.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -75.0000  240.0000    0.0000    0.0000 47

 27 omega   62.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -110.0000  181.0000    0.0000    0.0000 53

 28 omega   59.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -79.0000  139.0000    0.0000    0.0000 48

 29 omega  105.00  147.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   52.0000    8.0000    0.0000    0.0000 42

 30 omega   58.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488  -75.0000    0.0000    0.0000    0.0000 47

 31 omega   62.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   52.0000  127.0000    0.0000    0.0000 43

 32 omega    9.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -110.0000  181.0000    0.0000    0.0000 53

 33 omega   62.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   55.0000  184.0000    0.0000    0.0000 42

 34 omega  101.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   21.0000   -5.0000    0.0000    0.0000 49

 35 phi    120.00  180.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 36 omega   51.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   21.0000   -5.0000    0.0000    0.0000 50

 37 omega -125.00  -64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -54.5448  -10.0000  123.0000    0.0000    0.0000 61

 38 omega  -28.00   40.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440   86.0000   42.0000    0.0000    0.0000 68

 39 omega   -9.00   54.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        4.2440 -118.0000  172.0000    0.0000    0.0000 63

 40 phi   -180.00 -120.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    4.2440    0.0000     -        0.0000    0.0000 60

 41 phi      0.00   60.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    4.2440    0.0000     -        0.0000    0.0000 60

 42 phi   -120.00  -60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 43 phi     60.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 44 phi    -60.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 45 phi      0.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 46 phi   -180.00 -120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   78.8488    0.0000     -        0.0000    0.0000 60

 47 omega    9.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -118.0000   31.0000    0.0000    0.0000 55

 48 omega    9.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -110.0000  130.0000    0.0000    0.0000 53

 49 omega   62.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488 -110.0000  130.0000    0.0000    0.0000 53

 50 omega   51.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   21.0000   -2.0000    0.0000    0.0000 50

 51 omega  100.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   20.0000   16.0000    0.0000    0.0000 50

 52 omega   50.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   20.0000  255.0000    0.0000    0.0000 50

 53 omega  100.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       78.8488   20.0000  244.0000    0.0000    0.0000 50
;
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_orient_matrix_UB_11      -0.0022886673
_diffrn_orient_matrix_UB_12      -0.1198874111
_diffrn_orient_matrix_UB_13      -0.0042037416
_diffrn_orient_matrix_UB_21      0.0759616618
_diffrn_orient_matrix_UB_22      0.0004366111
_diffrn_orient_matrix_UB_23      -0.0397834910
_diffrn_orient_matrix_UB_31      0.0545228896
_diffrn_orient_matrix_UB_32      -0.0058481764
_diffrn_orient_matrix_UB_33      0.0843906242
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35883
_diffrn_reflns_theta_full        51.420
_diffrn_reflns_theta_max         51.420
_diffrn_reflns_theta_min         3.4314
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.2348
_exptl_crystal_description       triangular
_exptl_crystal_F_000             136.0
_exptl_crystal_size_max          0.8793
_exptl_crystal_size_mid          0.8061
_exptl_crystal_size_min          0.1298
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.0429
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         3356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
     calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0275
_reflns_number_gt                3356
_reflns_number_total             3834
_reflns_threshold_expression     F>2(\s)F
_cod_data_source_file            wf5141sup1.cif
_cod_data_source_block           I
_cod_database_code               2108280
_cod_database_fobs_code          2108280