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_2014072
_publ_section_title
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 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
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_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          'C16 H21 N3 O4 S'
_chemical_formula_moiety         'C16 H21 N3 O4 S'
_chemical_formula_sum            'C16 H21 N3 O4 S'
_chemical_formula_weight         351.42
_chemical_name_systematic
;
8-Hydroxymethyl-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                109.2678(18)
_cell_angle_beta                 99.8329(18)
_cell_angle_gamma                101.227(2)
_cell_formula_units_Z            2
_cell_length_a                   6.6682(2)
_cell_length_b                   11.0319(3)
_cell_length_c                   12.3449(4)
_cell_measurement_reflns_used    3737
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.19
_cell_volume                     813.32(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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'
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_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18379
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.15
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_refine_ls_number_reflns         3737
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0660P)^2^+0.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                2502
_reflns_number_total             3737
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1722.cif
_cod_data_source_block           II
_cod_depositor_comments
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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 
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_cod_database_code               2014072
_cod_database_fobs_code          2014072