Structure Analysis of a Transient Triplet Carbene Trapped in a Crystal
Masaki Kawano; Katsuyuki Hirai; Hideo Tomioka; Yuji Ohashi; Journal of the American Chemical Society 123 (2001) 6904–6908; doi:10.1021/ja0106366

data_4115617
_publ_section_title
;
 Structure Analysis of a Transient Triplet Carbene Trapped in a Crystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6904
_journal_page_last               6908
_journal_paper_doi               10.1021/ja0106366
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         (C6H2Cl3)2C=N2+[(C6H2Cl3)2C:]N2
_chemical_formula_sum            'C13 H4 Cl6 N2'
_chemical_formula_weight         400.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.549(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.731(2)
_cell_length_b                   12.813(4)
_cell_length_c                   12.254(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      2.0
_cell_volume                     1527.8(7)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT & SADABS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Siemens SMART CCD area detector system'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26715
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.9361
_exptl_absorpt_correction_T_min  0.6963
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'PROGRAM SADABS was used.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    ride
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                3526
_reflns_number_total             5405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0106366_2.cif
_cod_data_source_block           carbene
_cod_original_cell_volume        1527.9(6)
_cod_database_code               4115617