Geometric changes around an N atom due to a urethane-type bis(<i>tert</i>-butoxycarbonyl) substituent
Wojewska, Dominika; Kluczyk, Alicja; Ślepokura, Katarzyna; Acta Crystallographica Section C 69 (2013) 82–86; doi:10.1107/S0108270112048846

data_2018757
_publ_section_title
;
 Geometric changes around an N atom due to a urethane-type
 bis(<i>tert</i>-butoxycarbonyl) substituent
;
_journal_coeditor_code           QS3019
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              82
_journal_page_last               86
_journal_paper_doi               10.1107/S0108270112048846
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C11 H19 N O6'
_chemical_formula_moiety         'C11 H19 N O6'
_chemical_formula_sum            'C11 H19 N O6'
_chemical_formula_weight         261.27
_chemical_melting_point          335.7
_chemical_name_systematic
;
Dimethyl (2<i>S</i>)-2-[(<i>tert</i>-butoxycarbonyl)amino]butanedioate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.219(3)
_cell_length_b                   5.815(2)
_cell_length_c                   12.263(4)
_cell_measurement_reflns_used    5074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.57
_cell_measurement_theta_min      4.97
_cell_volume                     647.9(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type
'Oxford Xcalibur PX \k-geometry diffractometer with Onyx CCD camera'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7321
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         32.99
_diffrn_reflns_theta_min         4.87
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.179
_refine_ls_abs_structure_details 'known absolute configuration'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2219
_reflns_number_total             2437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3019.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018757
_cod_database_fobs_code          2018757