Crystallographic characterisation of arenesulfonyl azides. Structural and kinetic effects induced by ortho- and para-substituents
Besenyei, Gábor; Párkányi, László; Foch, Isabella; Simándi, László I.; Kálmán, Alajos; Journal of the Chemical Society, Perkin Transactions 2  (2000) 1798–; doi:10.1039/b004337k

data_7213389
_publ_section_title
;
 Crystallographic characterisation of arenesulfonyl azides. Structural and
 kinetic effects induced by ortho- and para-substituents
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1798
_journal_paper_doi               10.1039/b004337k
_journal_year                    2000
_chemical_formula_sum            'C10 H9 Fe N3 O2 S'
_chemical_formula_weight         291.11
_chemical_name_systematic
;                                                                               
 ferrocenesulfonyl azide                                                                              
;
_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                 92.29(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   5.984(1)
_cell_length_b                   35.194(1)
_cell_length_c                   10.795(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.99
_cell_measurement_theta_min      15.32
_cell_volume                     2271.6(4)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'MO k\a'
_diffrn_radiation_wavelength     0.710730
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5791
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        41.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   difabs
_exptl_absorpt_process_details   'PLATON (Spek, 1982)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0584P)^2^+0.0959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                3490
_reflns_number_total             5175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004337ksup1.cif
_cod_data_source_block           ferocn3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7213389