Unusually Short (C-H...π) Hydrogen Bonds for Effective Supramolecular (Aromatic/Aromatic) Organization in Edge-to-Face Motifs
S. V. Lindeman; D. Kosynkin; J. K. Kochi; Journal of the American Chemical Society 120 (1998) 13268–13269; doi:10.1021/ja982945a

data_4116916
_publ_section_title
;
 Unusually Short (C-H...\p) Hydrogen Bonds for Effective Supramolecular
 (Aromatic/Aromatic) Organization in Edge-to-Face Motifs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13268
_journal_page_last               13269
_journal_paper_doi               10.1021/ja982945a
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety
;
(C6 H5 N2)^+^, (C24 H20 B)^-^, 0.4(C H2 I2)
;
_chemical_formula_sum            'C60.8 H51.6 B2 I1.6 N4'
_chemical_formula_weight         1062.92
_chemical_name_systematic
; 
 Phenyldiazonium tetraphenylborate diiodomethane hemisolvate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                83.8590(10)
_cell_angle_beta                 81.9320(10)
_cell_angle_gamma                83.2040(10)
_cell_formula_units_Z            4
_cell_length_a                   9.97400(10)
_cell_length_b                   21.2237(3)
_cell_length_c                   26.01470(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      0.8
_cell_volume                     5391.19(10)
_computing_cell_refinement       'SAINT V4.050 (Siemens, 1989-95)'
_computing_data_collection       'SMART V4.050 (Siemens, 1989-95)'
_computing_data_reduction        'SAINT & SADABS (Sheldrick, 1996)'
_computing_molecular_graphics    'XP V5.06 (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 & XCIF V5.05 (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method
;
\w-scan, scan range 0.3 deg, hemisphere
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            34733
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         0.79
_diffrn_standards_decay_%        0.2
_diffrn_standards_number         946
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   'empirical (SADABS procedure)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2157
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_hydrogen_treatment
;
riding model wit Uiso = 1.2Ueq/iso of an adjacent atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         22387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_obs          0.0779
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+21.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1960
_refine_ls_wR_factor_obs         0.1660
_reflns_number_observed          16625
_reflns_number_total             22946
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982945a_2.cif
_cod_data_source_block           dimcs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+21.9981P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+21.9981P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C60.80 H51.60 B2 I1.60 N4'
_cod_database_code               4116916