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_4125850
_publ_section_title
;
 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
'8(F3 P0.5), 2(C18 H16 N2), 2(C24 H20 N2), 4(C2 H3 N)'
_chemical_formula_sum            'C92 H84 F24 N12 P4'
_chemical_formula_weight         1937.59
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                80.501(6)
_cell_angle_beta                 70.268(5)
_cell_angle_gamma                63.067(5)
_cell_formula_units_Z            2
_cell_length_a                   16.436(2)
_cell_length_b                   17.359(2)
_cell_length_c                   18.633(2)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.95
_cell_measurement_theta_min      2.86
_cell_volume                     4460.8(9)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.966
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43499
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.198
_diffrn_reflns_theta_min         2.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  0.7339
_exptl_absorpt_correction_T_min  0.6562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0686 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.8941.
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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         15775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0971P)^2^+6.5721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14117
_reflns_number_total             15775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09892_si_002.cif
_cod_data_source_block           boxinboxaug26_0m
_cod_database_code               4125850
_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(P6A)=1-FVAR(1)
 Sof(P6)=FVAR(1)
 Sof(F21A)=Sof(F20A)=Sof(F24A)=Sof(F23A)=1-FVAR(2)
 Sof(F20)=Sof(F21)=Sof(F24)=Sof(F23)=FVAR(2)
 Sof(F22A)=1-FVAR(3)
 Sof(F22)=FVAR(3)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C72(H72A,H72B), C61(H61A,H61B), C60(H60A,H60B),
 C49(H49A,H49B), C36(H36A,H36B), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C8(H8), C11(H11), C2(H2), C9(H9), C10(H10), C3(H3), C6(H6),
 C16(H16), C14(H14), C15(H15), C70(H70), C63(H63), C65(H65), C69(H69), C71(H71),
  C66(H66), C68(H68), C73(H73), C79(H79), C82(H82), C81(H81), C62(H62),
 C80(H80), C77(H77), C74(H74), C76(H76), C56(H56), C58(H58), C57(H57), C59(H59),
  C51(H51), C44(H44), C48(H48), C50(H50), C47(H47), C54(H54), C53(H53),
 C45(H45), C41(H41), C39(H39), C42(H42), C38(H38), C29(H29), C23(H23), C35(H35),
  C34(H34), C32(H32), C27(H27), C33(H33), C28(H28), C26(H26), C21(H21),
 C20(H20), C19(H19)
3.c Idealised Me refined as rotating group:
 C87(H87A,H87B,H87C), C91(H91A,H91B,H91C), C89(H89A,H89B,H89C), C94(H94A,H94B,
 H94C)
;
_shelx_res_checksum              87691
_shelx_hkl_checksum              91348
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'