<i>rac</i>-3-Benzoyl-2-methylpropionic acid and its organic salts: possibilities of Yang photocyclization in crystals
Bakowicz, Julia; Turowska-Tyrk, Ilona; Acta Crystallographica Section C 64 (2008) o437–o440; doi:10.1107/S0108270108021380

data_2016730
_publ_section_title
;
 <i>rac</i>-3-Benzoyl-2-methylpropionic acid and its organic salts:
 possibilities of Yang photocyclization in crystals
;
_journal_coeditor_code           SK3242
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o437
_journal_page_last               o440
_journal_paper_doi               10.1107/S0108270108021380
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C5 H6 N + , H+ , 2C11 H11 O3 -'
_chemical_formula_moiety         'C5 H6 N + , H+ , 2C11 H11 O3 -'
_chemical_formula_sum            'C27 H29 N O6'
_chemical_formula_weight         463.51
_chemical_name_systematic
;
pyridinium [hydrogen bis(<i>rac</i>-3-benzoyl-2-methylpropionate)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.34(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.759(6)
_cell_length_b                   10.172(2)
_cell_length_c                   9.776(2)
_cell_measurement_reflns_used    1115
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      18.93
_cell_measurement_theta_min      2.95
_cell_volume                     2545.8(9)
_computing_cell_refinement       'CrysAlisCCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Kuma KM4 CCD'
_diffrn_measurement_method       \w
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6670
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2199
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1206P)^2^+0.2239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                1454
_reflns_number_total             2199
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3242.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016730
_cod_database_fobs_code          2016730