Diisopropyl 1-(methylsulfonyl)hydrazine-1,2-dicarboxylate
Banwell, Martin G.; Dauge, Delphine; Willis, Anthony C.; Acta Crystallographica Section E 63 (2007) o2009–o2011; doi:10.1107/S1600536807011737

data_2212919
_publ_section_title
;
 Diisopropyl 1-(methylsulfonyl)hydrazine-1,2-dicarboxylate
;
_journal_coeditor_code           HG2206
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2009
_journal_page_last               o2011
_journal_paper_doi               10.1107/S1600536807011737
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C9 H18 N2 O6 S'
_chemical_formula_moiety         'C9 H18 N2 O6 S'
_chemical_formula_sum            'C9 H18 N2 O6 S'
_chemical_formula_weight         282.32
_chemical_melting_point          375
_chemical_name_systematic
;
Diisopropyl 1-(methylsulfonyl)hydrazine-1,2-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 110.9720(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0845(2)
_cell_length_b                   17.1465(4)
_cell_length_c                   9.9094(2)
_cell_measurement_reflns_used    18147
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     1441.31(6)
_computing_cell_refinement       'DENZO and SCALEPACK'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation,
1997)
;
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28645
_diffrn_reflns_theta_full        26.931
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.679
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
[Gaussian method (Coppens, 1970) implemented in MAXUS (Mackay <i>et
al.</i>,  1999)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9441
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = [1-(F~o~-F~c~)^2^/36\s^2^(F)]^2^/
[28.0T~0~(x) + 45.0T~1~(x) + 26.4T~2~(x) + 10.7T~3~(x) + 2.11T~4~(x)],
where T~i~ are the Chebychev polynomials and
x = F~c~/F~max~ (Carruthers & Watkin, 1979; Prince, 1982)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0887
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                2459
_reflns_number_total             3285
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2206.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212919
_cod_database_fobs_code          2212919