Manifestation of Polar Reaction Pathways of 2,3-Dichloro-5,6-dicyano-p-benzoquinone
Xingwei Guo; Herbert Mayr; Journal of the American Chemical Society 135 (2013) 12377–12387; doi:10.1021/ja405890d

data_4120330
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus F)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       Herbert.Mayr@cup.uni-muenchen.de
_publ_contact_author_fax         '+49 89 2180 77717'
_publ_contact_author_name        'H. Mayr'
_publ_section_title
;
 Manifestation of Polar Reaction Pathways of
 2,3-Dichloro-5,6-dicyano-p-benzoquinone
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12377
_journal_page_last               12387
_journal_paper_doi               10.1021/ja405890d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C17 H18 Cl2 N2 O4 Si'
_chemical_formula_sum            'C17 H18 Cl2 N2 O4 Si'
_chemical_formula_weight         413.327
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'P. Mayer'
_audit_block_code                C17H18Cl2N2O4Si_qo121_mayr
_audit_creation_date
;
'Tue Jul 17 12:49:13 2012'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             20-Jul-12
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.2550(6)
_cell_length_b                   15.1590(11)
_cell_length_c                   24.5615(14)
_cell_measurement_reflns_used    3630
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.6997
_cell_measurement_theta_min      4.2628
_cell_volume                     3818.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega  -80.00  -47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  126.0000   98.0000 33
  2 omega   34.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  179.0000   90.0000 66
  3 omega   -6.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   38.0000 -150.0000 97
;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0559300000
_diffrn_orient_matrix_UB_12      0.0231083000
_diffrn_orient_matrix_UB_13      -0.0094027000
_diffrn_orient_matrix_UB_21      -0.0335139000
_diffrn_orient_matrix_UB_22      -0.0405002000
_diffrn_orient_matrix_UB_23      -0.0032394000
_diffrn_orient_matrix_UB_31      -0.0232347000
_diffrn_orient_matrix_UB_32      0.0031995000
_diffrn_orient_matrix_UB_33      0.0271233000
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12912
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         4.27
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.43807(15)
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0344P)^2^+2.1970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                3495
_reflns_number_total             4430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405890d_si_002_1.cif
_cod_data_source_block           qo121
_cod_database_code               4120330