(+)-<i>N</i>,<i>N</i>'-Bis[(7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methylsulfonyl]piperazine
Małgorzata Ullrich; Anna Kozakiewicz; Mirosław Wełniak; Andrzej Wojtczak; Acta Crystallographica Section E 62 (2006) o3750–o3751; doi:10.1107/S1600536806028595

data_2210224
_publ_section_title
(+)-<i>N</i>,<i>N</i>'-Bis[(7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methylsulfonyl]piperazine
_journal_coeditor_code           FL2038
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3750
_journal_page_last               o3751
_journal_paper_doi               10.1107/S1600536806028595
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C24 H38 N2 O6 S2'
_chemical_formula_sum            'C24 H38 N2 O6 S2'
_chemical_formula_weight         514.68
_chemical_name_common            (+)-N,N'-dicamphorsulfonylpiperazine
_chemical_name_systematic
;
(+)-N,N'-Bis[(7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-
yl)methylsulfonyl]piperazine
;
_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           SHELX-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.4677(3)
_cell_length_b                   11.1826(4)
_cell_length_c                   27.0427(10)
_cell_measurement_reflns_used    7818
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      31.25
_cell_measurement_theta_min      2.36
_cell_volume                     2560.70(16)
_computing_cell_refinement       'CrysAlis CCD'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2000)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2000)'
_computing_molecular_graphics    'PLEASE SUPPLY'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Oxford Sapphire CCD'
_diffrn_measurement_method       \q/2\q
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            25421
_diffrn_reflns_theta_full        31.25
_diffrn_reflns_theta_max         31.25
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.9204
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.284
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         7818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0664P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                6202
_reflns_number_total             7818
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2038.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_database_code               2210224