Quaternary Charge-Transfer Solid Solutions: Electronic Tunability through Stoichiometry
Wiscons, Ren A.; Coropceanu, Veaceslav; Matzger, Adam J.; Chemistry of Materials 31 (2019) 6598–; doi:10.1021/acs.chemmater.9b00502

data_4002973
_publ_section_title
;
 Quaternary Charge-Transfer Solid Solutions: Electronic Tunability through
 Stoichiometry
;
_journal_issue                   17
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6598
_journal_paper_doi               10.1021/acs.chemmater.9b00502
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C14 H12 Se'
_chemical_formula_sum            'C14 H12 Se'
_chemical_formula_weight         259.20
_chemical_name_systematic        4,6-dimethyldibenzoselenophene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-02
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7550(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.74881(17)
_cell_length_b                   6.68747(14)
_cell_length_c                   16.9645(3)
_cell_measurement_reflns_used    7224
_cell_measurement_temperature    297.60(10)
_cell_measurement_theta_max      77.4060
_cell_measurement_theta_min      5.2030
_cell_volume                     1105.90(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.60(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -21.00  59.00   0.50    1.00    --   50.24 -43.00 -11.00  160
  2  \w     34.00  60.00   0.50    3.22    --  105.75 -77.00  90.00   52
  3  \w     34.00 123.00   0.50    3.22    --  105.75 -77.00  90.00  178
  4  \w     93.00 123.00   0.50    3.22    --  105.75 -77.00  90.00   60
  5  \w     42.00  68.00   0.50    3.22    --  105.75 -37.00 150.00   52
  6  \w     32.00  72.00   0.50    3.22    --  105.75 -19.00 150.00   80
  7  \w     97.00 178.00   0.50    3.22    --  105.75  43.00 140.00  162
  8  \w     71.00 121.00   0.50    1.00    --   50.24 125.00 -30.00  100
  9  \w     71.00 121.00   0.50    1.00    --   50.24 125.00-150.00  100
 10  \w     37.00  75.00   0.50    3.22    --  105.75 -19.00 -60.00   76
 11  \w     50.00  75.00   0.50    3.22    --  105.75 -19.00-120.00   50
 12  \w     36.00  66.00   0.50    3.22    --  105.75 -37.00-150.00   60
 13  \w     38.00  66.00   0.50    3.22    --  105.75 -37.00-180.00   56
 14  \w     33.00  58.00   0.50    3.22    --  105.75 -37.00-120.00   50
 15  \w     34.00  75.00   0.50    3.22    --  105.75 -43.00 -11.00   82
 16  \w     35.00  61.00   0.50    3.22    --  105.75 -37.00   0.00   52
 17  \w    -59.00  22.00   0.50    1.00    --  -50.24  43.00 140.00  162
 18  \w    -58.00  22.00   0.50    1.00    --  -50.24  37.00-120.00  160
 19  \w    -69.00 -33.00   0.50    3.22    -- -105.75  37.00  60.00   72
 20  \w    -75.00 -34.00   0.50    3.22    -- -105.75  43.00 140.00   82
 21  \w    -76.00 -32.00   0.50    3.22    -- -105.75  19.00 120.00   88
 22  \w    -76.00 -32.00   0.50    3.22    -- -105.75  19.00 150.00   88
 23  \w    -69.00 -33.00   0.50    3.22    -- -105.75  37.00  90.00   72
 24  \w   -106.00 -34.00   0.50    3.22    -- -105.75  57.00   0.00  144
 25  \w   -121.00 -41.00   0.50    1.00    --  -50.24 -43.00 -11.00  160
 26  \w   -121.00 -70.00   0.50    1.00    --  -50.24-125.00 -30.00  102
 27  \w   -177.00 -97.00   0.50    3.22    -- -105.75 -43.00 -11.00  160
 28  \w   -177.00 -93.00   0.50    3.22    -- -105.75 -57.00 -30.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1295754000
_diffrn_orient_matrix_UB_12      0.0546286000
_diffrn_orient_matrix_UB_13      0.0483722000
_diffrn_orient_matrix_UB_21      -0.0893220000
_diffrn_orient_matrix_UB_22      0.1124328000
_diffrn_orient_matrix_UB_23      0.0597570000
_diffrn_orient_matrix_UB_31      -0.0154127000
_diffrn_orient_matrix_UB_32      -0.1933049000
_diffrn_orient_matrix_UB_33      0.0483668000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10191
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.572
_diffrn_reflns_theta_max         66.572
_diffrn_reflns_theta_min         4.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.5a (Rigaku Oxford Diffraction, 2018)
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    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_recrystallization_method sublimation
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0631P)^2^+0.5424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1829
_reflns_number_total             1953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00502_si_003.cif
_cod_data_source_block           exp_754_dmdbs
_cod_original_cell_volume        1105.90(3)
_cod_database_code               4002973
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C56 H48 Se4 '
_diffrn_oxdiff_ac3_digest_frames
;
01ffc993723964e5d5ab97d6126ed5b6e9028283eb8
;
_diffrn_oxdiff_ac3_digest_hkl
;
01298d075568fa750ca9461a4dae4629273349
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C9(H9), C10(H10), C2(H2), C8(H8)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen MicroMount w/ mineral oil'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.714