Crystal structure of (5S,8S)-8-hydroxymethyl-1-methyl-2,7-dioxa-1- aza-spiro[4,4]nonan-6-one, C~8~H~13~NO~4~
W. Frey; M. Imerhasan; Y. Bathich; V. Jäger; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 151–152; doi:

data_8101673
_publ_section_title
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Crystal structure of (5S,8S)-8-hydroxymethyl-1-methyl-2,7-dioxa-1-
aza-spiro[4,4]nonan-6-one, C~8~H~13~NO~4~
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              151
_journal_page_last               152
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C8 H13 N O4'
_chemical_formula_weight         187.19
_chemical_melting_point          383.5(5)
_chemical_name_systematic
; 
(5S,8S)-8-hydroxymethyl-1-methyl-2,7-dioxa-1-aza-spiro[4,4]nonan-6-one 
;
_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                   8.8739(5)
_cell_length_b                   9.5664(5)
_cell_length_c                   10.7489(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      31.5
_cell_volume                     912.49(9)
_computing_cell_refinement       'Bruker XSCans V. 2.31'
_computing_data_collection       'Bruker XScans V. 2.31'
_computing_data_reduction        'Bruker XScans V. 2.31'
_computing_molecular_graphics    'SHELXTL - XP'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1640
_diffrn_reflns_theta_full        67.98
_diffrn_reflns_theta_max         67.98
_diffrn_reflns_theta_min         6.19
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(4)
_refine_ls_extinction_coef       0.048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    free
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         1389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0842P)^2^+0.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                1304
_reflns_number_total             1389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1301.cff
_cod_data_source_block           wf998yb
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '383-384 K' was changed to '383.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               8101673