Size-Matched Radical Multivalency.
Lipke, Mark C.; Cheng, Tao; Wu, Yilei; Arslan, Hasan; Xiao, Hai; Wasielewski, Michael R.; Goddard, William A.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.6b09892

data_4125851
_publ_section_title
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 Size-Matched Radical Multivalency.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.6b09892
_journal_year                    2017
_chemical_formula_moiety         '2(F6 P), C36 H32 N4'
_chemical_formula_sum            'C36 H32 F12 N4 P2'
_chemical_formula_weight         810.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 126.9238(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6496(9)
_cell_length_b                   8.7129(3)
_cell_length_c                   20.6646(12)
_cell_measurement_reflns_used    7162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.056
_cell_measurement_theta_min      3.447
_cell_volume                     3691.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13001
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.231
_diffrn_reflns_theta_min         3.447
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0718 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.8139.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0772P)^2^+3.8858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3074
_reflns_number_total             3584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09892_si_003.cif
_cod_data_source_block           ml3_0ma
_cod_database_code               4125851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H17A(0.5) H17B(0.5) H24A(0.5) H24B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C3(H3), C10(H10), C9(H9), C4(H4), C21(H21), C12(H12),
 C19(H19), C16(H16), C22(H22), C11(H11), C15(H15), C23(H23)
;
_shelx_res_checksum              93836
_shelx_hkl_checksum              43694
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'