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_4003438
_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     iterative
_audit_creation_date             2017-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.838(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7905(4)
_cell_length_b                   9.3048(6)
_cell_length_c                   16.1235(7)
_cell_measurement_reflns_used    1444
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      25.3930
_cell_measurement_theta_min      3.7890
_cell_volume                     1458.38(13)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      143.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -74.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669    0.0000 -120.0000 122

  2 omega  -65.00  -39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  126.0000  -40.0000 26

  3 omega  -75.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000  -30.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0365037000
_diffrn_orient_matrix_UB_12      0.0629674000
_diffrn_orient_matrix_UB_13      -0.0087673000
_diffrn_orient_matrix_UB_21      0.0122987000
_diffrn_orient_matrix_UB_22      0.0152245000
_diffrn_orient_matrix_UB_23      0.0433415000
_diffrn_orient_matrix_UB_31      0.0619921000
_diffrn_orient_matrix_UB_32      -0.0401419000
_diffrn_orient_matrix_UB_33      0.0027580000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5903
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.702
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 700 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4189
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0336P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.335
_reflns_Friedel_fraction_full    0.398
_reflns_Friedel_fraction_max     0.376
_reflns_number_gt                3005
_reflns_number_total             4189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b04495_si_002.cif
_cod_data_source_block           171018_s6_htt
_cod_depositor_comments
'Adding full bibliography for 4003436--4003440.cif.'
_cod_original_cell_volume        1458.38(12)
_cod_database_code               4003438
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.972
_reflns_odcompleteness_completeness 98.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_olex2_submission_special_instructions 'No special instructions were received'