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_4002972
_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 H14 Se'
_chemical_formula_sum            'C14 H14 Se'
_chemical_formula_weight         261.21
_chemical_name_systematic        'di(ortho-methylphenyl) selane'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-07
_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                   7.13182(14)
_cell_length_b                   7.33176(14)
_cell_length_c                   22.8392(4)
_cell_measurement_reflns_used    9157
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      77.1050
_cell_measurement_theta_min      1.9350
_cell_volume                     1194.23(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_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     98.00 178.00   0.50    0.80    --  105.75  13.00-157.00  160
  2  \w     71.00 122.00   0.50    0.29    --   50.49 124.00 -86.00  102
  3  \w     71.00 122.00   0.50    0.29    --   50.49 125.00-120.00  102
  4  \w     43.00 122.00   0.50    0.29    --   50.49  37.00-180.00  158
  5  \w   -144.00 -30.00   0.50    0.80    --  -84.50 165.00 156.00  228
  6  \w     34.00 110.00   0.50    0.80    --  105.75 -99.00 -30.00  152
  7  \w    -21.00  58.00   0.50    0.29    --   50.49 -37.00 -90.00  158
  8  \w    -22.00  58.00   0.50    0.29    --   50.49 -19.00-180.00  160
  9  \w     32.00  76.00   0.50    0.80    --  105.75 -19.00-120.00   88
 10  \w     33.00  69.00   0.50    0.80    --  105.75 -37.00-180.00   72
 11  \w     32.00  76.00   0.50    0.80    --  105.75 -19.00 -60.00   88
 12  \w     32.00  76.00   0.50    0.80    --  105.75 -19.00 -30.00   88
 13  \w     33.00  69.00   0.50    0.80    --  105.75 -37.00 -60.00   72
 14  \w     33.00  69.00   0.50    0.80    --  105.75 -37.00-150.00   72
 15  \w     32.00  76.00   0.50    0.80    --  105.75 -19.00-150.00   88
 16  \w     34.00 127.00   0.50    0.80    --  105.75 -77.00-180.00  186
 17  \w   -121.00 -30.00   0.50    0.29    --  -50.49 -77.00   0.00  182
 18  \w   -156.00 -71.00   0.50    0.80    --  -84.50-124.00-165.00  170
 19  \w   -156.00 -76.00   0.50    0.80    --  -84.50-116.00 -79.00  160
;
_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      0.0173987000
_diffrn_orient_matrix_UB_12      0.1692262000
_diffrn_orient_matrix_UB_13      0.0396039000
_diffrn_orient_matrix_UB_21      -0.0343914000
_diffrn_orient_matrix_UB_22      -0.1200106000
_diffrn_orient_matrix_UB_23      0.0543092000
_diffrn_orient_matrix_UB_31      0.2125864000
_diffrn_orient_matrix_UB_32      -0.0332181000
_diffrn_orient_matrix_UB_33      0.0055683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10891
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56841
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method sublimation
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 833 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0546P)^2^+1.0770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2084
_reflns_number_total             2117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00502_si_002.cif
_cod_data_source_block           exp_198
_cod_original_cell_volume        1194.24(4)
_cod_database_code               4002972
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C56 H56 Se4 '
_diffrn_oxdiff_ac3_digest_frames
;
01f4b7d0307764b7c63229ff9d1c621b4c024868546
;
_diffrn_oxdiff_ac3_digest_hkl
;
01962c05876a6525ed0e93b72e3b30926b63f7
;
_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: Se1(0.75) Se2(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C11(H11), C13(H13), C10(H10), C12(H12)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_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 1.703
_oxdiff_exptl_absorpt_empirical_full_min 0.636