Three hexahydropyridopyrimidine-spiro-cyclohexanetriones: supramolecular structures generated by O—H···O, N—H···O, C—H···O and C—H···π hydrogen bonds, and π–π stacking interactions
Low, John N.; Ferguson, George; Cobo, Justo; Nogueras, Manuel; Cruz, Silvia; Quiroga, Jairo; Glidewell, Christopher; Acta Crystallographica Section C 60 (2004) o438–o443; doi:10.1107/S0108270104009539

data_2014071
_publ_section_title
;
 Three hexahydropyridopyrimidine-spiro-cyclohexanetriones:
 supramolecular structures generated by O---H&#x00B7;&#x00B7;&#x00B7;O,
 N---H&#x00B7;&#x00B7;&#x00B7;O, C---H&#x00B7;&#x00B7;&#x00B7;O and
 C---H&#x00B7;&#x00B7;&#x00B7;\p hydrogen bonds, and \p--\p stacking
 interactions
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o438
_journal_page_last               o443
_journal_paper_doi               10.1107/S0108270104009539
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C15 H19 N3 O3 S'
_chemical_formula_moiety         'C15 H19 N3 O3 S'
_chemical_formula_sum            'C15 H19 N3 O3 S'
_chemical_formula_weight         321.39
_chemical_name_systematic
;
4',4'-Dimethyl-2-methylsulfanyl-3,4,5,6,7,8-hexahydropyrido[2,3-d]pyrimidine-
6-spiro-1'-cyclohexane-2',4,6'-trione
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                74.938(2)
_cell_angle_beta                 84.271(2)
_cell_angle_gamma                81.842(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8990(3)
_cell_length_b                   10.0386(3)
_cell_length_c                   10.0500(3)
_cell_measurement_reflns_used    3462
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.16
_cell_volume                     760.10(4)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15364
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.5301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                2923
_reflns_number_total             3462
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1722.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2014071
_cod_database_fobs_code          2014071