Methyl 4-<i>tert</i>-butoxycarbonyl-<i>N</i>-cyanopiperazine-1-carboximidothioate
Bi-Jian Lan; Peng Guo; Zhen-Guang Zou; Yin-Xiang Lu; Acta Crystallographica Section E 61 (2005) o3022–o3024; doi:10.1107/S1600536805026280

data_2206621
_publ_section_title
;
 Methyl
 4-<i>tert</i>-butoxycarbonyl-<i>N</i>-cyanopiperazine-1-carboximidothioate
;
_journal_coeditor_code           BD6009
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3022
_journal_page_last               o3024
_journal_paper_doi               10.1107/S1600536805026280
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C12 H20 N4 O2 S'
_chemical_formula_moiety         'C12 H20 N4 O2 S'
_chemical_formula_sum            'C12 H20 N4 O2 S'
_chemical_formula_weight         284.38
_chemical_name_systematic
;
Methyl 4-tert-butoxycarbonyl-N-cyanopiperazine-1-carboximidothioate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.358(2)
_cell_length_b                   9.382(3)
_cell_length_c                   24.646(8)
_cell_measurement_reflns_used    2619
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.06
_cell_measurement_theta_min      2.32
_cell_volume                     1470.2(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7193
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        2.40
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.9564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       spicula
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.151
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0538P)^2^+0.11P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                2436
_reflns_number_total             2875
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bd6009.cif
_cod_data_source_block           I
_cod_original_cell_volume        1470.1(8)
_cod_database_code               2206621
_cod_database_fobs_code          2206621