(1<i>R</i>,3<i>S</i>,6<i>S</i>)-6-<i>tert</i>-Butyl-1-hydroxymethyl-5-methoxy-6-methyl-7-oxa-4-azaspiro[2.5]oct-4-en-8-one and dimethyl [(1<i>S</i>,1'<i>R</i>,3'<i>S</i>,6'<i>S</i>)-(6'-<i>tert</i>-butyl-5'-methoxy-6'-methyl-8'-oxo-7'-oxa-4'-azaspiro[2.5]oct-4'-en-1'-yl)hydroxymethyl]phosphonate
Małecka, Magdalena; Wanner, Klaus Th.; Budzisz, Elżbieta; Acta Crystallographica Section C 59 (2003) o317–o320; doi:10.1107/S0108270103008564

data_2013332
_publ_section_title
;(1<i>R</i>,3<i>S</i>,6<i>S</i>)-6-<i>tert</i>-Butyl-1-hydroxymethyl-5-methoxy-6-methyl-7-oxa-4-azaspiro[2.5]oct-4-en-8-one
 and dimethyl
 [(1<i>S</i>,1'<i>R</i>,3'<i>S</i>,6'<i>S</i>)-(6'-<i>tert</i>-butyl-5'-methoxy-6'-methyl-8'-oxo-7'-oxa-4'-azaspiro[2.5]oct-4'-en-1'-yl)hydroxymethyl]phosphonate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o317
_journal_page_last               o320
_journal_paper_doi               10.1107/S0108270103008564
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C13 H21 N O4'
_chemical_formula_sum            'C13 H21 N O4'
_chemical_formula_weight         255.31
_chemical_name_systematic
;
(1R,3S,6S)-[6-tert-butyl-1-hydroxymethyl-5-methyoxy-6-methyl-7-oxa-8-oxo
-4-aza-spiro[2.5]oct-4-en-8-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
_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                   8.134(3)
_cell_length_b                   22.802(2)
_cell_length_c                   7.744(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.37
_cell_measurement_theta_min      23.46
_cell_volume                     1436.3(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular  Structure Corporation, 1989a)
;
_computing_data_reduction
'TEXSAN (Molecular  Structure Corporation, 1989b)'
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_publication_material  'PARST97 (Nardelli, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'AFC5S Rigaku'
_diffrn_measurement_method       '\w scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1480
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.88
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(De Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.164
_refine_ls_extinction_coef       0.017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0524
_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^)+(0.1207P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                1195
_reflns_number_total             1480
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1611.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Removing the _chemical_melting_point data item since it contained the
 _chemical_formula_sum data item value and not the melting temperature.

 Antanas Vaitkus,
 2017-09-27
;
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               2013332
_cod_database_fobs_code          2013332