Mechanical-Bond-Protected, Air-Stable Radicals.
Sun, Junling; Liu, Zhichang; Liu, Wei-Guang; Wu, Yilei; Wang, Yuping; Barnes, Jonathan C.; Hermann, Keith R.; Goddard, 3rd, William A; Wasielewski, Michael R.; Stoddart, J. Fraser; Journal of the American Chemical Society 139 (2017) 12704–12709; doi:10.1021/jacs.7b06857

data_4131572
_publ_section_title
;
 Mechanical-Bond-Protected, Air-Stable Radicals.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12704
_journal_page_last               12709
_journal_paper_doi               10.1021/jacs.7b06857
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C40 H32 N4, C26 H24 Br2 N2, 4(F6 P), C4 H6 N2'
_chemical_formula_sum            'C70 H62 Br2 F24 N8 P4'
_chemical_formula_weight         1754.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.398(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0874(5)
_cell_length_b                   17.3630(7)
_cell_length_c                   18.0711(8)
_cell_measurement_reflns_used    6973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.778
_cell_measurement_theta_min      2.466
_cell_volume                     3449.9(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6312
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.789
_diffrn_reflns_theta_min         3.544
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0770 before and 0.0576 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1385 before and 0.0659 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 77107 reflections, Rint = 0.0519
 (29915 with I > 3sig(I), Rint = 0.0429)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         6312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+5.4426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5351
_reflns_number_total             6312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06857_si_002.cif
_cod_data_source_block           cx0314
_cod_database_code               4131572
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.827(2) 0.173(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Sof(H38C)=Sof(H38D)=Sof(Br2A)=0.5*(1-FVAR(2))
 Sof(Br2)=Sof(H38A)=Sof(H38B)=0.5*FVAR(2)
 Fixed Sof: H21A(0.5) H21B(0.5) H26A(0.5) H26B(0.5) H33A(0.5) H33B(0.5)
 H40A(0.5) H40B(0.5) H40C(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C21(H21A,H21B), C26(H26A,H26B), C33(H33A,H33B),
 C38(H38A,H38B), C38(H38C,H38D)
4.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C27(H27), C28(H28), C31(H31),
  C32(H32), C35(H35), C36(H36)
;
_shelx_res_checksum              43756
_shelx_hkl_checksum              14508
_olex2_date_sample_data_collection 2015-03-09
_olex2_date_sample_submission    2015-03-04
_olex2_submission_original_sample_id cx0314
_olex2_submission_special_instructions 'No special instructions were received'