Experimental and theoretical evidence of a supercritical-like transition in an organic semiconductor presenting colossal uniaxial negative thermal expansion.
van der Lee, Arie; Roche, Gilles H.; Wantz, Guillaume; Moreau, Joël J E; Dautel, Olivier J.; Filhol, Jean-Sébastien; Chemical science 9 (2018) 3948–3956; doi:10.1039/c8sc00159f

data_1549102
_publ_section_title
;
 Experimental and theoretical evidence of a supercritical-like transition
 in an organic semiconductor presenting colossal uniaxial negative thermal
 expansion.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              3948
_journal_page_last               3956
_journal_paper_doi               10.1039/c8sc00159f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C26 H32 O2 S2'
_chemical_formula_sum            'C26 H32 O2 S2'
_chemical_formula_weight         440.66
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.762(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8186(5)
_cell_length_b                   5.8811(3)
_cell_length_c                   49.458(3)
_cell_measurement_reflns_used    3004
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.5810
_cell_measurement_theta_min      2.6460
_cell_volume                     2262.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_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    -54.00  32.00   1.00   33.52    --   13.31 -57.00   0.00   86
  2  \w     -4.00  23.00   1.00   33.52    --  -14.02-100.00   0.00   27
  3  \w    -18.00  23.00   1.00   33.52    --  -14.02-100.00 -90.00   41
  4  \w    -50.00  41.00   1.00   33.52    --   13.31 -77.00 120.00   91
  5  \w     20.00  47.00   1.00   33.52    --  -14.02  38.00 150.00   27
  6  \w    -15.00  83.00   1.00   33.52    --   13.31  77.00-120.00   98
;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0265752932
_diffrn_orient_matrix_UB_12      -0.0075768346
_diffrn_orient_matrix_UB_13      0.0132626291
_diffrn_orient_matrix_UB_21      0.0844333356
_diffrn_orient_matrix_UB_22      0.0279127961
_diffrn_orient_matrix_UB_23      0.0056139645
_diffrn_orient_matrix_UB_31      -0.0219046335
_diffrn_orient_matrix_UB_32      0.1171198698
_diffrn_orient_matrix_UB_33      -0.0004845929
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            7900
_diffrn_reflns_theta_full        25.226
_diffrn_reflns_theta_max         27.721
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.0014681
_refine_ls_shift/su_mean         0.0000924
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are: 
 0.130E+04 0.210E+04 0.124E+04 475. 77.1 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0651
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0639
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              63
_reflns_limit_l_min              0
_reflns_number_gt                2140
_reflns_number_total             2324
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0319
_oxford_refine_ls_scale          3.84(3)
_oxford_reflns_number_all        2324
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c8sc00159f2.cif
_cod_data_source_block           115K
_cod_depositor_comments
'Adding full bibliography for 1549094--1549104.cif.'
_cod_original_cell_volume        2262.64(14)
_cod_original_sg_symbol_H-M      'I 1 2/a 1 '
_cod_database_code               1549102
_cell_oxdiff_length_a            7.8182(5)
_cell_oxdiff_length_b            5.8796(3)
_cell_oxdiff_length_c            49.474(2)
_cell_oxdiff_angle_alpha         89.986(4)
_cell_oxdiff_angle_beta          95.773(4)
_cell_oxdiff_angle_gamma         89.963(4)
_cell_oxdiff_volume              2262.6(2)
_oxdiff_exptl_absorpt_empirical_full_min 0.892
_oxdiff_exptl_absorpt_empirical_full_max 1.604
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_montpellier_reflns_maxres       0.76
_montpellier_reflns_completeness_maxres 87.29
_montpellier_reflns_redundancy_maxres 3.28