<i>rac</i>-Diethyl 9-hydroxy-9-methyl-7-phenyl-1,4-diazaspiro[4.5]decane-6,8-dicarboxylate
Maharramov, Abel M.; Ismiyev, Arif I.; Rashidov, Bahruz A.; Rahimova, Gunel M.; Allahverdiyev, Mirza A.; Acta Crystallographica Section E 67 (2011) o291–; doi:10.1107/S1600536810054498

data_2229215
_publ_section_title
;
 <i>rac</i>-Diethyl
 9-hydroxy-9-methyl-7-phenyl-1,4-diazaspiro[4.5]decane-6,8-dicarboxylate
;
_journal_coeditor_code           SI2321
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o291
_journal_paper_doi               10.1107/S1600536810054498
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H30 N2 O5'
_chemical_formula_moiety         'C21 H30 N2 O5'
_chemical_formula_sum            'C21 H30 N2 O5'
_chemical_formula_weight         390.47
_chemical_name_systematic
;
<i>rac</i>-Diethyl
9-hydroxy-9-methyl-7-phenyl-1,4-diazaspiro[4.5]decane-6,8-dicarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.000(4)
_cell_angle_beta                 97.413(4)
_cell_angle_gamma                97.736(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4140(17)
_cell_length_b                   10.7606(19)
_cell_length_c                   10.7874(19)
_cell_measurement_reflns_used    1499
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.266
_cell_measurement_theta_min      2.406
_cell_volume                     1040.6(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1083
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8475
_diffrn_reflns_theta_full        26.54
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4252
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                2225
_reflns_number_total             4252
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2321.cif
_cod_data_source_block           I
_cod_database_code               2229215
_cod_database_fobs_code          2229215