4-(3,4-Dichlorophenyl)-9-(4-methylphenylsulfonyl)-4,9-diazatetracyclo[5.3.1.0^2,6^.0^8,10^]undecane-3,5-dione and 4-(4-chlorophenyl)-9-(4-methylphenylsulfonyl)-4,9-diazatetracyclo[5.3.1.0^2,6^.0^8,10^]undecane-3,5-dione
Bortoluzzi, Adailton J.; Andrade, Evilazio S.; Nunes, Ricardo J.; Acta Crystallographica Section C 60 (2004) o614–o616; doi:10.1107/S0108270104015550

data_2014138
_publ_section_title
;4-(3,4-Dichlorophenyl)-9-(4-methylphenylsulfonyl)-4,9-diazatetracyclo[5.3.1.0^2,6^.0^8,10^]undecane-3,5-dione
 and
 4-(4-chlorophenyl)-9-(4-methylphenylsulfonyl)-4,9-diazatetracyclo[5.3.1.0^2,6^.0^8,10^]undecane-3,5-dione
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o614
_journal_page_last               o616
_journal_paper_doi               10.1107/S0108270104015550
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C22 H19 Cl N2 O4 S'
_chemical_formula_moiety         'C22 H19 Cl N2 O4 S'
_chemical_formula_sum            'C22 H19 Cl N2 O4 S'
_chemical_formula_weight         442.90
_chemical_name_systematic
;
4-(4-chlorophenyl)-9-(4-methylphenylsulfonyl)-4,9-
diazatetracyclo[5.3.1.0^2,6^.0^8,10^]undecane-3,5-dione
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                105.06(2)
_cell_angle_beta                 109.89(2)
_cell_angle_gamma                100.97(3)
_cell_formula_units_Z            2
_cell_length_a                   8.975(2)
_cell_length_b                   10.167(5)
_cell_length_c                   12.8760(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.62
_cell_measurement_theta_min      8.63
_cell_volume                     1015.4(6)
_computing_cell_refinement       'SET4 in CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'HELENA (Spek, 1996)'
_computing_molecular_graphics    'ORTEP-3 (Farrgia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3941
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.264
_refine_ls_extinction_coef       0.027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0472P)^2^+0.3187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                3118
_reflns_number_total             3764
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1757.cif
_cod_data_source_block           II
_cod_depositor_comments
;
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_database_code               2014138
_cod_database_fobs_code          2014138