Direct observation of arylnitrene formation in the photoreaction of arylazide crystals
Takayama, Terufumi; Mitsumori, Takahiro; Kawano, Masaki; Sekine, Akiko; Uekusa, Hidehiro; Ohashi, Yuji; Sugawara, Tadashi; Acta Crystallographica Section B 66 (2010) 639–646; doi:10.1107/S0108768110036608

data_2104837
_publ_section_title
;
 Direct observation of arylnitrene formation in the photoreaction of
 arylazide crystals
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              639
_journal_page_last               646
_journal_paper_doi               10.1107/S0108768110036608
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C7 H5 N3 O2'
_chemical_formula_sum            'C7 H5 N3 O2'
_chemical_formula_weight         163.14
_chemical_melting_point          ?
_chemical_name_common
;
 3-carboxyphenylazide
;
_chemical_name_systematic
;
 3-carboxyphenylazide
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.829(6)
_cell_angle_beta                 83.770(5)
_cell_angle_gamma                86.189(5)
_cell_formula_units_Z            2
_cell_length_a                   3.7639(5)
_cell_length_b                   6.5389(12)
_cell_length_c                   15.141(3)
_cell_measurement_temperature    80(2)
_cell_volume                     365.25(11)
_computing_cell_refinement       'RIGAKU R-AXIS RAPID'
_computing_data_collection       'RIGAKU R-AXIS RAPID'
_computing_data_reduction        'RIGAKU TEXSAN & ABSCOR'
_computing_molecular_graphics    'ORTEP3 for Window (Farrugia,1998)'
_computing_publication_material  SHELXTL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID IP detector system'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2550
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_correction_T_min  0.9560
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Program ABSCOR was used. '
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.278
_refine_ls_extinction_coef       0.19(3)
_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   1.097
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0909P)^2^+0.1356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                1120
_reflns_number_total             1310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5042.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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        365.24(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2104837