4-(4-Bromo-3-methyl-1<i>H</i>-pyrazol-1-yl)-6-(but-3-ynyloxy)pyrimidine
Heng, Lin-Sen; Li, Yong-Hong; Mei, Xiang-Dong; Ning, Jun; Acta Crystallographica Section E 65 (2009) o3031–; doi:10.1107/S1600536809046194

data_2224234
_publ_section_title
;
 4-(4-Bromo-3-methyl-1<i>H</i>-pyrazol-1-yl)-6-(but-3-ynyloxy)pyrimidine
;
_journal_coeditor_code           HB5193
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3031
_journal_paper_doi               10.1107/S1600536809046194
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C12 H11 Br N4 O'
_chemical_formula_moiety         'C12 H11 Br N4 O'
_chemical_formula_sum            'C12 H11 Br N4 O'
_chemical_formula_weight         307.16
_chemical_name_systematic
;
4-(4-Bromo-3-methyl-1<i>H</i>-pyrazol-1-yl)-6-(but-3-ynyloxy)pyrimidine
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.34(3)
_cell_angle_beta                 77.98(3)
_cell_angle_gamma                80.78(3)
_cell_formula_units_Z            4
_cell_length_a                   7.9053(16)
_cell_length_b                   10.045(2)
_cell_length_c                   16.807(3)
_cell_measurement_reflns_used    536
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.17
_cell_volume                     1254.7(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15373
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0360P)^2^+1.1156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                4988
_reflns_number_total             5693
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5193.cif
_cod_data_source_block           I
_cod_original_cell_volume        1254.7(4)
_cod_database_code               2224234
_cod_database_fobs_code          2224234