<i>tert</i>-Butyl (7<i>R</i>)-7-[(4<i>S</i>)-2,2-dimethyl-[1,3]dioxolan-4-yl]-1,4-dioxa-8-azaspiro[4.5]decane-8-carboxylate
Badorrey, Ramon; Cativiela, Carlos; Díaz-de-Villegas, Maria D.; Gálvez, Jose A.; Acta Crystallographica Section E 58 (2002) o750–o752; doi:10.1107/S160053680200898X

data_2201648
_publ_section_title
;<i>tert</i>-Butyl
 (7<i>R</i>)-7-[(4<i>S</i>)-2,2-dimethyl-[1,3]dioxolan-4-yl]-1,4-dioxa-8-azaspiro[4.5]decane-8-carboxylate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o750
_journal_page_last               o752
_journal_paper_doi               10.1107/S160053680200898X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C17 H29 N O6'
_chemical_formula_moiety         'C17 H29 N O6'
_chemical_formula_sum            'C17 H29 N O6'
_chemical_formula_weight         343.41
_chemical_name_systematic
;
tert-Butyl (7R)-7-[(4S)-2,2-dimethyl-[1,3]dioxolan-4-yl]-1,4-dioxa-8-
azaspiro[4.5]decane-8-carboxylate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.770(10)
_cell_angle_beta                 69.720(10)
_cell_angle_gamma                69.590(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6410(10)
_cell_length_b                   9.9970(10)
_cell_length_c                   11.0420(10)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      7.19
_cell_volume                     935.06(18)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1993)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1989)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3913
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3277
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.1664P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                2068
_reflns_number_total             3277
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6098.cif
_cod_data_source_block           I
_cod_original_cell_volume        935.1(2)
_cod_database_code               2201648
_cod_database_fobs_code          2201648