<i>tert</i>-Butyl 3-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)methylamino]-4-methoxyimino-3-methylpiperidine-1-carboxylate
Wan, Zhilong; Chai, Yun; Liu, Mingliang; Guo, Huiyuan; Acta Crystallographica Section E 65 (2009) o256–; doi:10.1107/S1600536808044255

data_2220897
_publ_section_title
;<i>tert</i>-Butyl
 3-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)methylamino]-4-methoxyimino-3-methylpiperidine-1-carboxylate
;
_journal_coeditor_code           RK2125
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o256
_journal_paper_doi               10.1107/S1600536808044255
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C18 H33 N3 O5'
_chemical_formula_moiety         'C18 H33 N3 O5'
_chemical_formula_sum            'C18 H33 N3 O5'
_chemical_formula_weight         371.47
_chemical_name_systematic
;
<i>tert</i>-Butyl
3-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)methylamino]-4-methoxyimino-3-
methylpiperidine-1-carboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.769(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.867(3)
_cell_length_b                   6.1887(13)
_cell_length_c                   25.379(3)
_cell_measurement_reflns_used    1707
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.101
_cell_measurement_theta_min      2.727
_cell_volume                     4180.6(11)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10032
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_correction_T_min  0.9634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0496
_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^)+(0.058P)^2^+0.3657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                1915
_reflns_number_total             3699
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2125.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2220897
_cod_database_fobs_code          2220897