Methyl 5'-(2-hydroxyphenyl)-4',5',6',7'-tetrahydrospiro[2<i>H</i>-1-benzopyran-2,7'-1,2,4-triazolo[1,5-<i>a</i>]pyrimidine]-3-carboxylate
Kettmann, Viktor; Světlík, Jan; Acta Crystallographica Section E 67 (2011) o92–; doi:10.1107/S160053681005052X

data_2228830
_publ_section_title
;
 Methyl
 5'-(2-hydroxyphenyl)-4',5',6',7'-tetrahydrospiro[2<i>H</i>-1-benzopyran-2,7'-1,2,4-triazolo[1,5-<i>a</i>]pyrimidine]-3-carboxylate
;
_journal_coeditor_code           NK2069
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o92
_journal_paper_doi               10.1107/S160053681005052X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H18 N4 O4'
_chemical_formula_moiety         'C21 H18 N4 O4'
_chemical_formula_sum            'C21 H18 N4 O4'
_chemical_formula_weight         390.39
_chemical_melting_point          511
_chemical_name_systematic
;
Methyl
5'-(2-hydroxyphenyl)-4',5',6',7'-tetrahydrospiro[2<i>H</i>-1-benzopyran-2,7'-
1,2,4-triazolo[1,5-<i>a</i>]pyrimidine]-3-carboxylate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.337(6)
_cell_length_b                   14.824(5)
_cell_length_c                   13.932(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      7
_cell_volume                     3955(2)
_computing_cell_refinement       'XSCANS (Siemens, 1994)'
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'XSCANS (Siemens, 1994)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w/2\q
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            12311
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         10237
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0583P)^2^+0.3383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                5854
_reflns_number_total             10237
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nk2069.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228830
_cod_database_fobs_code          2228830