Observation of a Solid-State-Induced Thermally Populated Spin-Triplet State in Radical Regioisomers
Hu, Xiaoguang; Chen, Hanjiao; Zhao, Lei; Miao, Maosheng; Zheng, Yonghao; Chemistry of Materials 31 (2019) 10256–; doi:10.1021/acs.chemmater.9b04495

data_4003439
_publ_section_title
;
 Observation of a Solid-State-Induced Thermally Populated Spin-Triplet
 State in Radical Regioisomers
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              10256
_journal_paper_doi               10.1021/acs.chemmater.9b04495
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C39 H28 N3'
_chemical_formula_sum            'C39 H28 N3'
_chemical_formula_weight         538.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.748(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7865(3)
_cell_length_b                   9.3003(3)
_cell_length_c                   16.1043(4)
_cell_measurement_reflns_used    2944
_cell_measurement_temperature    292.5(4)
_cell_measurement_theta_max      72.7740
_cell_measurement_theta_min      4.5520
_cell_volume                     1455.62(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      292.5(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -55.00  33.00   1.00    1.02    --  -36.29  38.00  60.00   88
  2  \w    -53.00  31.00   1.00    1.02    --  -36.29  57.00 -60.00   84
  3  \w      1.00  75.00   1.00    1.02    --   36.29 -99.00  60.00   74
  4  \w     23.00  90.00   1.00    1.02    --   36.29-125.00 -60.00   67
  5  \w    -31.00  53.00   1.00    1.02    --   36.29 -57.00 150.00   84
  6  \w     87.00 178.00   1.00    4.08    --  108.71  30.00 150.00   91
  7  \w     91.00 176.00   1.00    4.08    --  108.71  61.00 -30.00   85
  8  \w     42.00 127.00   1.00    4.08    --  108.71 -61.00-120.00   85
  9  \w     91.00 177.00   1.00    4.08    --  108.71  45.00  30.00   86
 10  \w     39.00 109.00   1.00    4.08    --  108.71 -94.00  90.00   70
 11  \w     39.00 109.00   1.00    4.08    --  108.71 -94.00  30.00   70
 12  \w     42.00 127.00   1.00    4.08    --  108.71 -61.00 150.00   85
 13  \w     39.00 130.00   1.00    4.08    --  108.71 -30.00 -30.00   91
 14  \w   -104.00 -10.00   1.00    1.02    --  -36.29 -77.00 -60.00   94
 15  \w     20.00  70.00   1.00    1.02    --   36.29  57.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0095721000
_diffrn_orient_matrix_UB_12      0.0250097000
_diffrn_orient_matrix_UB_13      0.0950931000
_diffrn_orient_matrix_UB_21      -0.1369567000
_diffrn_orient_matrix_UB_22      -0.0807457000
_diffrn_orient_matrix_UB_23      0.0024168000
_diffrn_orient_matrix_UB_31      0.0792606000
_diffrn_orient_matrix_UB_32      -0.1424060000
_diffrn_orient_matrix_UB_33      0.0152729000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8188
_diffrn_reflns_point_group_measured_fraction_full 0.791
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.753
_diffrn_reflns_theta_min         4.550
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1156 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0977P)^2^+0.0077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.465
_reflns_Friedel_fraction_full    0.553
_reflns_Friedel_fraction_max     0.521
_reflns_number_gt                3980
_reflns_number_total             4438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b04495_si_003.cif
_cod_data_source_block           ch-tpe
_cod_depositor_comments
'Adding full bibliography for 4003436--4003440.cif.'
_cod_database_code               4003439
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C00C(H00C), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016)
;
_shelx_res_checksum              41329
_shelx_hkl_checksum              11830
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2019-01-22
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.833