Cycloadditions of 1-aza-2-azoniaallene ions to alkenes
Wirschun, Wolfgang G.; Al-Soud, Yaseen A.; Nusser, Konstanze A.; Orama, Olli; Maier, Gerd-Michael; Jochims, Johannes C.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 4356–; doi:10.1039/b006525k

data_7213431
_publ_section_title
;
 Cycloadditions of 1-aza-2-azoniaallene ions to alkenes
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              4356
_journal_paper_doi               10.1039/b006525k
_journal_year                    2000
_chemical_formula_sum            'C35 H39 Cl18 N9 Sb2'
_chemical_formula_weight         1467.35
_chemical_melting_point          478.15
_chemical_name_common            'NORBORNADIEN EXO'
_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 and geom (H812,H813,H922,H923,H12,H13,H14)'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.85(2)
_cell_angle_beta                 92.16(2)
_cell_angle_gamma                89.99(2)
_cell_formula_units_Z            2
_cell_length_a                   9.537(3)
_cell_length_b                   10.640(4)
_cell_length_c                   27.931(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19.051
_cell_measurement_theta_min      12.010
_cell_volume                     2831.9(18)
_computing_cell_refinement       'Enraf Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'Enraf Nonius MolEN (1990)'
_computing_molecular_graphics    'ORTEP,SCHAKAL 93'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Enraf-Nonius-CAD4 4-circle-diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8824
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        42.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.840
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          1.08
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.885
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.440
_refine_ls_restrained_S_obs      0.990
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_obs          0.0570
_refine_ls_shift/esd_max         -0.049
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+18.3521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3901
_refine_ls_wR_factor_obs         0.1558
_reflns_number_observed          7179
_reflns_number_total             8215
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006525ksup1.cif
_cod_data_source_block           k56
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '205_C' was changed to '478.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

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^)+(0.1099P)^2^+18.3521P] 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^)+(0.1099P)^2^+18.3521P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213431