6-Hydroxy-2,5,7,8-tetramethyl-3,4-dihydro-2<i>H</i>-1-benzopyran-2-carbonitrile, from synchrotron data
Brzezinski, Krzysztof; Baj, Aneta; Wałejko, Piotr; Witkowski, Stanisław; Dauter, Zbigniew; Acta Crystallographica Section E 67 (2011) o1901–; doi:10.1107/S1600536811025517

data_2231191
_publ_section_title
;
 6-Hydroxy-2,5,7,8-tetramethyl-3,4-dihydro-2<i>H</i>-1-benzopyran-2-carbonitrile,
 from synchrotron data
;
_journal_coeditor_code           KP2339
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1901
_journal_paper_doi               10.1107/S1600536811025517
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H17 N O2'
_chemical_formula_moiety         'C14 H17 N O2'
_chemical_formula_sum            'C14 H17 N O2'
_chemical_formula_weight         231.29
_chemical_name_systematic
;
6-Hydroxy-2,5,7,8-tetramethyl-3,4-dihydro-2<i>H</i>-1-benzopyran-2-carbonitrile
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.890(5)
_cell_length_b                   10.300(10)
_cell_length_c                   19.710(19)
_cell_measurement_reflns_used    1841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.94
_cell_measurement_theta_min      2.18
_cell_volume                     1195.7(19)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'SER-CAT APS beamline software'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PyMOL (DeLano, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'MAR 300 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si111 double crystal'
_diffrn_radiation_source         'SER-CAT 22-ID synchrotron beamline APS, USA'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75000
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15411
_diffrn_reflns_theta_full        30.94
_diffrn_reflns_theta_max         30.94
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski <i>et al.</i>, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.2970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                1815
_reflns_number_total             1818
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kp2339.cif
_cod_data_source_block           I
_cod_database_code               2231191
_cod_database_fobs_code          2231191