Unprecedented radical-radical reaction of a [2.2]paracyclophane derivative containing an imidazolyl radical moiety.
Hatano, Sayaka; Sakai, Ken; Abe, Jiro; Organic letters 12 (2010) 4152–4155; doi:10.1021/ol1017933

data_1503204
_publ_section_title
;
 Unprecedented radical-radical reaction of a [2.2]paracyclophane
 derivative containing an imidazolyl radical moiety.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4152
_journal_page_last               4155
_journal_paper_doi               10.1021/ol1017933
_journal_volume                  12
_journal_year                    2010
_chemical_formula_analytical     'C93 H72 N8, C H2 Cl2, H0.44 O0.22'
_chemical_formula_iupac          'C94 H74.44 Cl2 N8 O0.22'
_chemical_formula_moiety         'C93 H72 N8, C H2 Cl2, H0.44 O0.22'
_chemical_formula_structural     'C93 H72 N8, C H2 Cl2, H0.44 O0.22'
_chemical_formula_sum            'C94 H74.44 Cl2 N8 O0.22'
_chemical_formula_weight         1390.48
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.406(2)
_cell_angle_beta                 74.527(2)
_cell_angle_gamma                74.304(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6760(18)
_cell_length_b                   18.951(3)
_cell_length_c                   19.394(3)
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_cell_measurement_temperature    97(2)
_cell_measurement_theta_max      27.43
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_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'KENX (Sakai, 2004)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), 
KENX, and ORTEP (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      97(2)
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_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device
'Bruker SMART APEXII CCD-detector diffractometer'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0192
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_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_l_max       22
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_diffrn_reflns_number            15840
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_diffrn_reflns_theta_max         25.03
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_diffrn_standards_decay_%        0
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_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.7456
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_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(XPREP in SAINT; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
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_exptl_crystal_description       plate
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_exptl_crystal_size_rad          0.29
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.479
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         12206
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_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+3.1402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                9272
_reflns_number_total             12206
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol1017933_si_002.cif
_cod_data_source_block           hatano
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3640.4(10)
_cod_database_code               1503204