2-Methoxy-3-methyl-6-[(triphenylphosphoranylidene)amino]pyrimidin-4(3<i>H</i>)-one and 3-Methyl-2-methylthio-6-[(triphenylphosphoranylidene)amino]pyrimidin-4(3<i>H</i>)-one
Low, John N.; Ferguson, George; Cobo, Justo; Nogueras, Manuel; Sanchez, Adolfo; Marchal, Antonio; Acta Crystallographica Section C 54 (1998) 1355–1357; doi:10.1107/S0108270198003795

data_2007642
_publ_section_title
;2-Methoxy-3-methyl-6-[(triphenylphosphoranylidene)amino]pyrimidin-4(3<i>H</i>)-one
 and
 3-Methyl-2-methylthio-6-[(triphenylphosphoranylidene)amino]pyrimidin-4(3<i>H</i>)-one
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1355
_journal_page_last               1357
_journal_paper_doi               10.1107/S0108270198003795
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C24 H22 N3 O P S'
_chemical_formula_sum            'C24 H22 N3 O P S'
_chemical_formula_weight         431.48
_chemical_name_systematic
;
2-methylthio-3-methyl-6-[(triphenylphosphoranylidene)amino]pyrimidin-4(3H)-
one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                79.291(12)
_cell_angle_beta                 75.62(2)
_cell_angle_gamma                70.693(14)
_cell_formula_units_Z            2
_cell_length_a                   8.666(2)
_cell_length_b                   10.985(3)
_cell_length_c                   12.373(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.97
_cell_volume                     1069.8(5)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'MADNES and NRCVAX94'
_computing_molecular_graphics    'NRCVAX94 and PLATON (Spek, 1998)'
_computing_publication_material  'NRCVAX94 and SHELXL93'
_computing_structure_refinement  'NRCVAX94 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    NRCVAX94
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_max 0.735
_diffrn_measurement_device
;
  Enraf-Nonius diffractometer with FAST area detector
;
_diffrn_measurement_method
'MADNES scans (Pflugrath & Messerschmidt, 1980)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4077
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.474
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_obs          .0647
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1641
_refine_ls_wR_factor_obs         .1617
_reflns_number_observed          2507
_reflns_number_total             2788
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ln1053.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1220P)^2^] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1220P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1069.8(4)
_cod_database_code               2007642