Persistent, highly localized, and tunable [4]helicene radicals
Shaikh, Aslam C.; Moutet, Jules; Veleta, José M.; Hossain, Md Mubarak; Bloch, Jan; Astashkin, Andrei V.; Gianetti, Thomas L.; Chemical Science  (2020) –; doi:10.1039/D0SC04850J

data_1559175
_publ_section_title
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 Persistent, highly localized, and tunable [4]helicene radicals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04850J
_journal_year                    2020
_chemical_formula_moiety         'C1 H2 Cl2, B F4, C31 H39 N4 O2'
_chemical_formula_sum            'C32 H41 B Cl2 F4 N4 O2'
_chemical_formula_weight         671.43
_chemical_name_systematic        2-Hcation
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-20 deposited with the CCDC.	2020-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.1060(18)
_cell_angle_beta                 78.778(2)
_cell_angle_gamma                64.945(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5110(3)
_cell_length_b                   12.4254(3)
_cell_length_c                   13.1831(3)
_cell_measurement_reflns_used    12735
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.3260
_cell_measurement_theta_min      3.1460
_cell_volume                     1675.47(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_details
;
  1 omega  -46.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   38.0000  -60.0000 81

  2 omega  -24.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -60.0000 26

  3 omega   14.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   38.0000  -90.0000 26

  4 omega  -19.00   20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  150.0000 39

  5 omega  -21.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -90.0000 34

  6 omega  -49.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -38.0000 -150.0000 40

  7 omega   -3.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   71.0000  133.0000 93

  8 omega  -44.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -71.0000    2.0000 93

  9 omega  -98.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904 -179.0000   30.0000 64

 10 omega    1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   57.0000   30.0000 90

 11 omega   -3.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   38.0000 -150.0000 98

 12 omega  -25.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -99.0000 -120.0000 89

 13 omega  -25.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -99.0000   90.0000 63

 14 omega    1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   57.0000  -60.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35035
_diffrn_reflns_theta_full        26.3714
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.3308
_exptl_crystal_description       block
_exptl_crystal_F_000             704.9552
_exptl_crystal_recrystallization_method DCM/Hexane
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.3598
_refine_diff_density_min         -0.2530
_refine_diff_density_rms         0.0538
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             6.4655
_refine_ls_goodness_of_fit_ref   1.0699
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    67
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0699
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.2295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                6350
_reflns_number_total             6857
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc04850j2.cif
_cod_data_source_block           2-Hcation
_cod_original_cell_volume        1675.45(8)
_cod_database_code               1559175
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl2A)=Sof(C19A)=Sof(H19c)=Sof(H19d)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl1)=Sof(C19)=Sof(H19a)=Sof(H19b)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00U(H00a,H00b), C00V(H00c,H00d), C00W(H00e,H00f), C00Z(H00g,H00i), C012(H01g,
 H01h), C013(H01i,H01j), C19(H19a,H19b), C19A(H19c,H19d)
3.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00N(H00N), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00T(H00T), C00X(H00X), C00Y(H00Y)
3.c Idealised Me refined as rotating group:
 C010(H01a,H01b,H01c), C011(H01d,H01e,H01f), C014(H01k,H01l,H01m), C015(H01n,
 H01o,H01p), C016(H01q,H01r,H01s), C018(H01t,H01u,H01v)
;
_olex2_submission_original_sample_id tlg4xr1
_olex2_submission_special_instructions 'No special instructions were received'