Cycloadditions of 1-aza-2-azoniaallene cations to isothiocyanates
El-Gazzar, Abdel-Rahman B.A.; Scholten, Kirsten; Guo, Yiping; Weißenbach, Kerstin; Hitzler, Martin G.; Roth, Gerhard; Fischer, Helmut; Jochims, Johannes C.; Journal of the Chemical Society, Perkin Transactions 1  (1999) 1999–; doi:10.1039/a902505g

data_7213069
_publ_section_title
;
 Cycloadditions of 1-aza-2-azoniaallene cations to isothiocyanates
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1999
_journal_paper_doi               10.1039/a902505g
_journal_year                    1999
_chemical_formula_moiety         'C18 H17 Cl3 N3 S +, Sb Cl6 -'
_chemical_formula_sum            'C18 H17 Cl9 N3 S Sb'
_chemical_formula_weight         748.21
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.42(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.114(11)
_cell_length_b                   26.501(11)
_cell_length_c                   13.450(6)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    248
_cell_measurement_theta_max      12.95
_cell_measurement_theta_min      7.11
_cell_volume                     2835(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6621
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_obs          0.0380
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+5.6604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0973
_refine_ls_wR_factor_obs         0.0904
_reflns_number_observed          5218
_reflns_number_total             6194
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902505gsup1.cif
_cod_data_source_block           sand
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+5.6604P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+5.6604P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2835.0(43)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7213069