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_4002919
_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         'Br2 C8 N2 O2, C8 H20 N'
_chemical_formula_sum            'C16 H20 Br2 N3 O2'
_chemical_formula_weight         446.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-11
_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                 98.493(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1881(3)
_cell_length_b                   20.1241(10)
_cell_length_c                   12.6012(6)
_cell_measurement_reflns_used    4103
_cell_measurement_temperature    300.3(4)
_cell_measurement_theta_max      62.5010
_cell_measurement_theta_min      4.1500
_cell_volume                     1802.83(15)
_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      300.3(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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      1.00  49.00   0.50    4.00    --   -0.31  57.00   0.00   96
  2  \w     14.00  39.00   0.50    4.00    --   -0.31  26.00-117.00   50
  3  \w     87.00 112.00   0.50   40.00    --   79.64  26.00-117.00   50
  4  \w     71.00 154.00   0.50   40.00    --   79.64  19.00-180.00  166
  5  \w     39.00  89.00   0.50   40.00    --   79.64 -57.00 -90.00  100
  6  \w     26.00 102.00   0.50   40.00    --   79.64 -99.00 -90.00  152
  7  \w     11.00  36.00   0.50   40.00    --   79.64 -26.00  79.00   50
  8  \w     13.00  48.00   0.50   40.00    --   79.64 -37.00 -30.00   70
  9  \w    -25.00  30.00   0.50    4.00    --   -0.31 -99.00-150.00  110
 10  \w    -45.00 -20.00   0.50   40.00    --  -80.26  26.00-117.00   50
 11  \w    -67.00  -9.00   0.50   40.00    --  -80.26  37.00 -60.00  116
 12  \w    -67.00  -7.00   0.50   40.00    --  -80.26  19.00  30.00  120
 13  \w    -64.00 -13.00   0.50   40.00    --  -80.26  37.00 150.00  102
 14  \w    -56.00 -31.00   0.50    4.00    --   -0.31 -26.00  79.00   50
 15  \w    -25.00   1.00   0.50    4.00    --   -0.31 -99.00  90.00   52
 16  \w    -93.00 -68.00   0.50   40.00    --  -80.26 -37.00-120.00   50
 17  \w   -138.00-109.00   0.50   40.00    --  -80.26 -37.00-120.00   58
 18  \w   -131.00-106.00   0.50   40.00    --  -80.26 -26.00  79.00   50
;
_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      0.1836631000
_diffrn_orient_matrix_UB_12      -0.0249819000
_diffrn_orient_matrix_UB_13      0.0665392000
_diffrn_orient_matrix_UB_21      -0.0876913000
_diffrn_orient_matrix_UB_22      0.0084801000
_diffrn_orient_matrix_UB_23      0.1036763000
_diffrn_orient_matrix_UB_31      -0.0741330000
_diffrn_orient_matrix_UB_32      -0.0718494000
_diffrn_orient_matrix_UB_33      -0.0108938000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9253
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        64.039
_diffrn_reflns_theta_max         64.039
_diffrn_reflns_theta_min         4.172
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58885
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_recrystallization_method 'acetonitrile evaporation'
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0474P)^2^+1.0164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2268
_reflns_number_total             2902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00502_si_009.cif
_cod_data_source_block           exp_497
_cod_depositor_comments
'Adding full bibliography for 4002917--4002919.cif.'
_cod_original_cell_volume        1802.81(15)
_cod_database_code               4002919
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C11 H10 N O'
_diffrn_oxdiff_ac3_digest_frames
;
01df5993fcf15bcb05194b937826e7be8b014926f8c
;
_diffrn_oxdiff_ac3_digest_hkl
;
010e3ccf1624b684eaa48ffcffdadb3a3d041f
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C16(H16a,H16b), C14(H14a,H14b), C12(H12a,H12b)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen Mount in 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 1.755
_oxdiff_exptl_absorpt_empirical_full_min 0.575