Accurate single crystal and gas-phase molecular structures of acenaphthene: a starting point in the search for the longest C-C bond.
Vishnevskiy, Yury V.; Otlyotov, Arseniy A.; Lamm, Jan-Hendrik; Stammler, Hans-Georg; Girichev, Georgiy V.; Mitzel, Norbert W.; Physical chemistry chemical physics : PCCP 25 (2023) 11464–11476; doi:10.1039/d2cp05613e

data_7246442
_publ_section_title
;
 Accurate single crystal and gas-phase molecular structures of
 acenaphthene: a starting point in the search for the longest C-C bond.
;
_journal_issue                   16
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              11464
_journal_page_last               11476
_journal_paper_doi               10.1039/d2cp05613e
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C12 H10'
_chemical_formula_sum            'C12 H10'
_chemical_formula_weight         154.213
_chemical_name_common            Acenaphthene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_symmetry_Int_Tables_number      26
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-10-05 deposited with the CCDC.	2023-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8073(7)
_cell_length_b                   8.2291(7)
_cell_length_c                   7.0858(4)
_cell_measurement_reflns_used    30530
_cell_measurement_temperature    95.0(2)
_cell_measurement_theta_max      62.5550
_cell_measurement_theta_min      3.7800
_cell_volume                     805.10(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      95.0(2)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9831
_diffrn_measured_fraction_theta_max 0.9963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  21.00   1.00   12.50    --    0.00 -38.00 -90.00   92
  2  \w    -77.00  33.00   1.00   12.50    --    0.00 -19.00  90.00  110
  3  \w    -20.00  39.00   1.00   12.50    --    0.00 -99.00 -90.00   59
  4  \w    -77.00  33.00   1.00   12.50    --    0.00 -19.00-180.00  110
  5  \w    -71.00  30.00   1.00   12.50    --    0.00 -77.00-120.00  101
  6  \w    -77.00  33.00   1.00   12.50    --    0.00 -19.00   0.00  110
  7  \w    -20.00  39.00   1.00   12.50    --    0.00 -99.00   0.00   59
  8  \w     63.00 156.00   1.00   50.00    --   87.07  52.00-123.03   93
  9  \w     60.00 156.00   1.00   50.00    --   87.07  65.00-170.50   96
 10  \w     60.00 156.00   1.00   50.00    --   87.07  64.00 124.69   96
 11  \w     58.00 157.00   1.00   50.00    --   87.07  73.00 138.09   99
 12  \w     59.00 140.00   1.00   50.00    --   87.07  69.00 -76.78   81
 13  \w     61.00 100.00   1.00   50.00    --   87.07  60.00 -94.19   39
 14  \w     60.00  89.00   1.00   50.00    --   87.07  63.00-108.78   29
 15  \w     57.00  82.00   1.00   50.00    --   87.07  75.00  19.33   25
 16  \w     73.00 147.00   1.00   50.00    --   87.07 125.00  90.00   74
 17  \w     65.00 157.00   1.00   50.00    --   87.07  44.00  94.79   92
 18  \w     62.00 128.00   1.00   50.00    --   87.07  58.00 -45.22   66
 19  \w     57.00  83.00   1.00   50.00    --   87.07  77.00-120.00   26
 20  \w     62.00 131.00   1.00   50.00    --   87.07  57.00  60.00   69
 21  \w     62.00  88.00   1.00   50.00    --   87.07  57.00 -30.00   26
 22  \w     57.00  82.00   1.00   50.00    --   87.07  77.00-150.00   25
 23  \w     57.00  82.00   1.00   50.00    --   87.07  77.00  60.00   25
 24  \w     62.00  88.00   1.00   50.00    --   87.07  57.00-150.00   26
 25  \w     57.00  87.00   1.00   50.00    --   87.07  77.00   0.00   30
 26  \w     57.00  82.00   1.00   50.00    --   87.07  77.00 120.00   25
 27  \w     57.00  82.00   1.00   50.00    --   87.07  77.00 -60.00   25
 28  \w      8.00 102.00   1.00   50.00    --   87.07 -92.00  84.62   94
 29  \w      7.00 109.00   1.00   50.00    --   87.07 -92.00 174.61  102
 30  \w     64.00  89.00   1.00   50.00    --   87.07  49.00 -62.77   25
 31  \w     57.00  92.00   1.00   50.00    --   87.07  77.00 150.00   35
 32  \w     57.00  83.00   1.00   50.00    --   87.07  77.00 -30.00   26
 33  \w     99.00 127.00   1.00   50.00    --   87.07  77.00 150.00   28
 34  \w      9.00  54.00   1.00   50.00    --   87.07 -99.00 150.00   45
 35  \w     56.00 109.00   1.00   50.00    --   87.07 -92.00 -95.40   53
 36  \w     57.00  83.00   1.00   50.00    --   87.07  77.00-180.00   26
 37  \w     96.00 157.00   1.00   50.00    --   87.07  77.00-180.00   61
 38  \w     87.00 122.00   1.00   50.00    --   87.07  77.00  30.00   35
 39  \w     57.00  82.00   1.00   50.00    --   87.07  77.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.9831
_diffrn_reflns_Laue_measured_fraction_max 0.9963
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            106572
_diffrn_reflns_point_group_measured_fraction_full 0.9868
_diffrn_reflns_point_group_measured_fraction_max 0.9727
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             328.165
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.1865
_refine_diff_density_min         -0.1884
_refine_diff_density_rms         0.0411
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -3(3)
_refine_ls_d_res_high            0.4100
_refine_ls_d_res_low             7.0689
_refine_ls_extinction_coef       0.0060
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.1889
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     206
_refine_ls_number_reflns         12162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.1889
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+0.0115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0475
_reflns_Friedel_coverage         0.947
_reflns_limit_h_max              33
_reflns_limit_h_min              -33
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                10765
_reflns_number_total             12162
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cp05613e3.cif
_cod_data_source_block           ACE_95K
_cod_depositor_comments
'Adding full bibliography for 7246440--7246442.cif.'
_cod_original_sg_symbol_Hall     ' P 2c -2'
_cod_database_code               7246442
_olex2_refinement_description
;
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
( F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021)
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         PBE0
   BASIS SET:      def2-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2022-09-30_11-20-35
;
_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
- Detector area scaling
;