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_4003440
_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           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.700(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6751(3)
_cell_length_b                   19.2046(7)
_cell_length_c                   15.8341(5)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    296.3(9)
_cell_measurement_theta_max      72.2700
_cell_measurement_theta_min      5.3620
_cell_volume                     2938.81(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      296.3(9)
_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 0.982
_diffrn_measurement_details
;
  1 omega   17.00  105.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921   38.0000 -150.0000 88

  2 omega  -31.00   53.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -57.0000  120.0000 84

  3 omega    1.00   75.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -99.0000   60.0000 74

  4 omega  -31.00   53.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -57.0000   30.0000 84

  5 omega   20.00  104.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000  150.0000 84

  6 omega   23.00   90.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000 -150.0000 67

  7 omega   90.00  175.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000    0.0000 85

  8 omega   40.00   98.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

  9 omega   57.00  150.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -90.0000 93

 10 omega   38.00   91.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 11 omega   87.00  178.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

 12 omega   38.00  116.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 78

 13 omega   38.00  116.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 78

 14 omega   40.00   98.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 15 omega   38.00   91.00   1.0000   15.9400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 16 omega   20.00  104.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000   60.0000 84

 17 omega    1.00   27.00   1.0000    3.9800
omega____ theta____ kappa____ phi______ frames
    -       36.2921   93.0000   23.5844 26
;
_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_UB_11      -0.1111969000
_diffrn_orient_matrix_UB_12      -0.0265180000
_diffrn_orient_matrix_UB_13      0.0587009000
_diffrn_orient_matrix_UB_21      -0.0292044000
_diffrn_orient_matrix_UB_22      0.0754226000
_diffrn_orient_matrix_UB_23      0.0269978000
_diffrn_orient_matrix_UB_31      -0.1103487000
_diffrn_orient_matrix_UB_32      0.0067590000
_diffrn_orient_matrix_UB_33      -0.0729020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16571
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.786
_diffrn_reflns_theta_min         4.605
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull greenish green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0950P)^2^+0.2973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4698
_reflns_number_total             5748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b04495_si_004.cif
_cod_data_source_block           ch-tpe-br-r-2
_cod_depositor_comments
'Adding full bibliography for 4003436--4003440.cif.'
_cod_database_code               4003440
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.87
_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:
 C007(H007), C00F(H00F), C00H(H00H), 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)
;
_olex2_date_sample_data_collection 2017-09-20
_olex2_submission_special_instructions 'No special instructions were received'