Diastereoselective T-Reaction of 1-Alkyl-5-(5-nitro-2-N-morpholino-benzylidene)barbituric Acids in the Solid State: Synthesis of 1-Alkyl-2,4,6-trioxoperhydropyrimidino-5-spiro-10′-(7′-nitro-1′,3′,4′,9′,10′,10a′-hexahydro-2′-oxa)-4a′-azaphenanthrenes and Their 2′-Thia Analogues
Krasnov, Konstantin A.; Khrustalev, Victor N.; Crystal Growth & Design 14 (2014) 3975–; doi:10.1021/cg500570u

data_4511715
_publ_section_title
;
 Diastereoselective T-Reaction of
 1-Alkyl-5-(5-nitro-2-N-morpholino-benzylidene)barbituric Acids in the
 Solid State: Synthesis of
 1-Alkyl-2,4,6-trioxoperhydropyrimidino-5-spiro-10&#x2032;-(7&#x2032;-nitro-1&#x2032;,3&#x2032;,4&#x2032;,9&#x2032;,10&#x2032;,10a&#x2032;-hexahydro-2&#x2032;-oxa)-4a&#x2032;-azaphenanthrenes
 and Their 2&#x2032;-Thia Analogues
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3975
_journal_paper_doi               10.1021/cg500570u
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C19 H22 N4 O6'
_chemical_formula_sum            'C19 H22 N4 O6'
_chemical_formula_weight         402.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.538(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.065(5)
_cell_length_b                   11.414(5)
_cell_length_c                   13.752(5)
_cell_measurement_reflns_used    2418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.32
_cell_volume                     1891.9(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20614
_diffrn_reflns_theta_full        28.13
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                2758
_reflns_number_total             4579
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg500570u_si_001.cif
_cod_data_source_block           5f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511715--4511716.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4511715