<i>tert</i>-Butyl 4-(2-diazoacetyl)piperazine-1-carboxylate
Kaupang, Åsmund; Görbitz, Carl Henrik; Hansen, Tore; Acta Crystallographica Section E 66 (2010) o1299–; doi:10.1107/S1600536810016211

data_2226211
_publ_section_title
;
 <i>tert</i>-Butyl 4-(2-diazoacetyl)piperazine-1-carboxylate
;
_journal_coeditor_code           LH5033
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1299
_journal_paper_doi               10.1107/S1600536810016211
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H18 N4 O3'
_chemical_formula_moiety         'C11 H18 N4 O3'
_chemical_formula_sum            'C11 H18 N4 O3'
_chemical_formula_weight         254.29
_chemical_name_systematic
;
<i>tert</i>-Butyl 4-(2-diazoacetyl)piperazine-1-carboxylate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.122(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.654(10)
_cell_length_b                   10.548(7)
_cell_length_c                   8.553(6)
_cell_measurement_reflns_used    2404
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.38
_cell_volume                     1321.8(16)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method
;
Three sets of frames each taken over 0.3\% \w rotation with 20 s
exposure time. Detector set at 2\q = 26\%, crystal-to-detector distance
6.00 cm.
;
_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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7308
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_correction_T_min  0.8703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0463P)^2^+0.1671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                2111
_reflns_number_total             2692
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5033.cif
_cod_data_source_block           I
_cod_original_cell_volume        1321.8(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226211
_cod_database_fobs_code          2226211