<i>N</i>-3-Allylation of 2-(<i>N</i>,<i>N</i>-Dimethylaminomethyleneamino)-6-formylpteridin-4-one
Helliwell, Madeleine; Dinsmore, Andrew; Garner, C. David; Joule, John A.; Acta Crystallographica Section C 53 (1997) 1667–1669; doi:10.1107/S0108270197009116

data_2006641
_publ_contact_author
;
John A. Joule
Chemistry Department
The University of Manchester
Manchester M13 9PL
England
;
_publ_section_title
;
 <i>N</i>-3-Allylation of
 2-(<i>N</i>,<i>N</i>-Dimethylaminomethyleneamino)-6-formylpteridin-4-one
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1667
_journal_page_last               1669
_journal_paper_doi               10.1107/S0108270197009116
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C13 H14 N6 O2 '
_chemical_formula_sum            'C13 H14 N6 O2'
_chemical_formula_weight         286.30
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.829(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.056(4)
_cell_length_b                   8.340(2)
_cell_length_c                   15.5461(12)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    296
_cell_measurement_theta_max      18.8
_cell_measurement_theta_min      10.9
_cell_volume                     1385.7(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1995a)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1995b)'
_computing_molecular_graphics    TEXSAN
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2575
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        -1.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of constrained and independent refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_obs          .0500
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.069P)^2^+0.476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1472
_refine_ls_wR_factor_obs         .1276
_reflns_number_observed          1771
_reflns_number_total             2442
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1143.cif
_cod_data_source_block           s561
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
calc w = 1/[\s^2^(Fo^2^)+(0.069P)^2^+0.476P] 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^)+(0.069P)^2^+0.476P] 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        1385.6(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006641