Synthesis, Characterization, and Crystal Structure of 1,3,7,9-Tetramethylpyrido-[2,3-d:6,5-d']-dipyrimidine-2,4,6,8-tetrone
Carmen Enrique; Miguel Quirós; M. Angustias Romero; Juan M. Salas; M. Purificación Sánchez; Francisco Hueso-Ureña; Miguel N. Moreno-Carretero; J. Daniel Martín; Journal of Chemical Crystallography 24 (1994) 465–468; doi:10.1007/BF01666096

data_1511768
_publ_contact_author
;    Miguel Quir\'os
     Departamento de Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-243322
_publ_contact_author_phone       34-58-243325
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structure of
 1,3,7,9-Tetramethylpyrido-[2,3-d:6,5-d']-dipyrimidine-2,4,6,8-tetrone
;
_journal_name_full               'Journal of Chemical Crystallography'
_journal_page_first              465
_journal_page_last               468
_journal_paper_doi               10.1007/BF01666096
_journal_volume                  24
_journal_year                    1994
_chemical_formula_sum            'C13 H13 N5 O4'
_chemical_formula_weight         303.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_type_scat_source           ' SHELXTL PLUS package (Sheldrick, NICOLET)'
_audit_creation_date             94-02-25
_audit_creation_method           'Programa PASACIF'
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.06(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.720(5)
_cell_length_b                   13.688(7)
_cell_length_c                   8.079(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      12.5
_cell_volume                     1344.8(10)
_computing_cell_refinement       ' DIF4 Control program vers. 7 (STOE & CIE)'
_computing_data_collection       ' DIF4 Control program vers. 7 (STOE & CIE)'
_computing_data_reduction        ' REDU4 program (STOE & CIE)'
_computing_molecular_graphics
' Program XP, SHELXTL PLUS package (Sheldrick, NICOLET)'
_computing_publication_material
; Program PASACIF, PASCAL program from SHELXTL data to
CIF format file. Unpublished.
;
_computing_structure_refinement
' Program XLS, SHELXTL PLUS package (Sheldrick, NICOLET)'
_computing_structure_solution
' Program XS, SHELXTL PLUS package (Sheldrick, NICOLET)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'Siemens R3m/V Kristalloflex'
_diffrn_measurement_method       'omega/2_theta (Learn profile method)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6266
_diffrn_reflns_theta_max         62.19
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.50
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.47
_refine_ls_goodness_of_fit_obs   0.45
_refine_ls_hydrogen_treatment
;
   Fixed C-H (0.95 \%A) and geminal H-H (1.54 \%A) distances.
   Common fixed isotropic U refined.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         1616
_refine_ls_R_factor_obs          0.059
_refine_ls_shift/esd_max         0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w^-1^ = \s^2^(F) + 0.05000 F^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.084
_reflns_number_observed          1616
_reflns_number_total             2107
_reflns_observed_criterion       'F > 6.00 \s(F)'
_cod_data_source_file            fdue.cif
_cod_data_source_block           triciclo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w^-1^ = \s^2^(F) + 0.05000 F^2^'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w^-1^ = \s^2^(F) +
0.05000 F^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1344.7(9)
_cod_original_formula_sum        'C13 H13 N5 O4 '
_cod_database_code               1511768