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_4002974
_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         '0.5(C28 H24 Se2), Br2 C8 N2 O2'
_chemical_formula_sum            'C22 H12 Br2 N2 O2 Se'
_chemical_formula_weight         575.12
_chemical_name_systematic
'2,3-dibromo-5,6-dicyanobenzioquinone 4,6-dimethyldibenzoselenophene'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-04
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.64274(17)
_cell_length_b                   18.4437(5)
_cell_length_c                   16.9726(4)
_cell_measurement_reflns_used    5411
_cell_measurement_temperature    298.48(10)
_cell_measurement_theta_max      76.6120
_cell_measurement_theta_min      2.6640
_cell_volume                     2079.43(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32e (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32e (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32e (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.48(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    102.00 170.00   0.50    1.40    --  105.75  56.00 139.00  136
  2  \w     88.00 146.00   0.50    1.40    --  105.75 105.00  11.00  116
  3  \w     71.00 118.00   0.50    0.40    --   50.49 125.00   0.00   94
  4  \w     71.00 104.00   0.50    0.40    --   50.49 125.00-150.00   66
  5  \w    -47.00 -14.00   0.50    1.40    --  -84.50  37.00-120.00   66
  6  \w    -66.00 -16.00   0.50    1.40    --  -84.50  37.00 -30.00  100
  7  \w    -54.00 -17.00   0.50    1.40    --  -84.50  37.00 120.00   74
  8  \w   -107.00 -81.00   0.50    0.40    --  -50.49-125.00 -60.00   52
  9  \w     23.00  68.00   0.50    0.40    --   50.49 -70.00 153.00   90
 10  \w    -10.00  20.00   0.50    0.40    --   50.49 -70.00 153.00   60
 11  \w     40.00  65.00   0.50    1.40    --  105.75 -19.00 -60.00   50
 12  \w     35.00  66.00   0.50    1.40    --  105.75 -19.00  30.00   62
 13  \w     36.00  61.00   0.50    1.40    --  105.75 -37.00 -30.00   50
 14  \w     39.00  68.00   0.50    1.40    --  105.75 -37.00-180.00   58
 15  \w     33.00  58.00   0.50    1.40    --  105.75 -37.00   0.00   50
 16  \w     32.00  75.00   0.50    1.40    --  105.75 -19.00-150.00   86
 17  \w     71.00  97.00   0.50    1.40    --  105.75 -70.00 153.00   52
 18  \w     37.00  62.00   0.50    1.40    --  105.75 -70.00 153.00   50
 19  \w   -153.00-121.00   0.50    1.40    --  -84.50 -19.00-180.00   64
 20  \w   -109.00 -83.00   0.50    1.40    --  -84.50 -19.00-180.00   52
;
_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      0.0560842000
_diffrn_orient_matrix_UB_12      -0.0628877000
_diffrn_orient_matrix_UB_13      0.0555507000
_diffrn_orient_matrix_UB_21      0.1448612000
_diffrn_orient_matrix_UB_22      0.0504118000
_diffrn_orient_matrix_UB_23      0.0449738000
_diffrn_orient_matrix_UB_31      -0.1721489000
_diffrn_orient_matrix_UB_32      0.0219627000
_diffrn_orient_matrix_UB_33      0.0559582000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5579
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        66.550
_diffrn_reflns_theta_max         66.550
_diffrn_reflns_theta_min         4.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32e (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_preparation       'solvent evaporation'
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 624 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1676
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0334P)^2^+0.3876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.615
_reflns_Friedel_fraction_full    0.662
_reflns_Friedel_fraction_max     0.662
_reflns_number_gt                1652
_reflns_number_total             1676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00502_si_006.cif
_cod_data_source_block           exp_74
_cod_original_cell_volume        2079.42(9)
_cod_database_code               4002974
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C24 H24 N24 O24 Se24 Br24 '
_diffrn_oxdiff_ac3_digest_frames
;
0190b342717f9b69603d0bc8b0f495417c01428bf7a
;
_diffrn_oxdiff_ac3_digest_hkl
;
01d720a673e49a816b126548779e037ee09d28
;
_reflns_odcompleteness_completeness 100.00
_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. Others
 Fixed Sof: H21A(0.5) H21B(0.5) H21C(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C16(H16), C17(H17), C11(H11), C18(H18)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_exptl_crystal_mounting_method MiTGen
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.587