8,11-Dichloro-N-tosyl-3-aza[5]metacyclophane: A Highly Strained Aromatic System
Daniël S. van Es; Arne Egberts; Stephen Nkrumah; Hans de Nijs; Willem H. de Wolf; Friedrich Bickelhaupt; Nora Veldman; Anthony L. Spek; Journal of the American Chemical Society 119 (1997) 615–616; doi:10.1021/ja9634987

data_4116930
_publ_section_title
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 8,11-Dichloro-N-tosyl-3-aza[5]metacyclophane: A Highly Strained Aromatic
 System
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              615
_journal_page_last               616
_journal_paper_doi               10.1021/ja9634987
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C17 H17 Cl2 N O2 S'
_chemical_formula_weight         1481.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7855(5)
_cell_length_b                   10.5456(4)
_cell_length_c                   23.4215(13)
_cell_measurement_temperature    150(2)
_cell_volume                     1675.98(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            5905
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.520
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             768
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_obs          0.0478
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0260P)^2^+0.5593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_obs         0.0870
_reflns_number_observed          2991
_reflns_number_total             3837
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9634987.cif
_cod_data_source_block           s1131b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0260P)^2^+0.5593P] 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^)+( 0.0260P)^2^+0.5593P] 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        1676.0(2)
_cod_database_code               4116930