Quantification of the ambident electrophilicities of halogen-substituted quinones.
Guo, Xingwei; Mayr, Herbert; Journal of the American Chemical Society 136 (2014) 11499–11512; doi:10.1021/ja505613b

data_4122542
_publ_section_title
;
 Quantification of the ambident electrophilicities of halogen-substituted
 quinones.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11499
_journal_page_last               11512
_journal_paper_doi               10.1021/ja505613b
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C23 H24 Cl8 O6 Si2'
_chemical_formula_sum            'C23 H24 Cl8 O6 Si2'
_chemical_formula_weight         736.226
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                C23H24Cl8O6Si2_so015_mayr
_audit_creation_date
;
'Tue Apr 08 15:17:03 2014'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             08-Apr-14
_cell_angle_alpha                79.908(5)
_cell_angle_beta                 81.840(5)
_cell_angle_gamma                83.374(5)
_cell_formula_units_Z            2
_cell_length_a                   8.8302(5)
_cell_length_b                   11.9810(7)
_cell_length_c                   15.2909(8)
_cell_measurement_reflns_used    3026
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.6600
_cell_measurement_theta_min      4.4490
_cell_volume                     1569.73(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   -2.00   90.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       21.5431   57.0000   90.0000 92

  2 omega  -24.00   25.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -99.0000 -150.0000 49

  3 omega  -49.00   45.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       21.5431  -57.0000  -60.0000 94

  4 omega  -50.00   48.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931   77.0000 -180.0000 98

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0553983000
_diffrn_orient_matrix_UB_12      -0.0477769000
_diffrn_orient_matrix_UB_13      0.0047385000
_diffrn_orient_matrix_UB_21      -0.0589396000
_diffrn_orient_matrix_UB_22      -0.0353130000
_diffrn_orient_matrix_UB_23      0.0198802000
_diffrn_orient_matrix_UB_31      -0.0099753000
_diffrn_orient_matrix_UB_32      -0.0108506000
_diffrn_orient_matrix_UB_33      -0.0428624000
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9306
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.28
_diffrn_source_current           45_mA
_diffrn_source_power             2.48_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.55767(16)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.3493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5074
_reflns_number_total             6317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja505613b_si_002.cif
_cod_data_source_block           so015
_cod_original_cell_volume        1569.72(16)
_cod_database_code               4122542