<i>rac</i>-(1<i>S</i>,2<i>R</i>)-Diethyl 6-hydroxy-1-(4-methoxyphenyl)-3-oxo-2,3-dihydro-1<i>H</i>-benzo[<i>f</i>]chromen-2-yl]phosphonate
Wojciechowski, Jakub; Krawczyk, Henryk; Albrecht, Łukasz; Wolf, Wojciech M.; Acta Crystallographica Section E 64 (2008) o1240–o1241; doi:10.1107/S1600536808015857

data_2218773
_publ_section_title
;<i>rac</i>-(1<i>S</i>,2<i>R</i>)-Diethyl
 6-hydroxy-1-(4-methoxyphenyl)-3-oxo-2,3-dihydro-1<i>H</i>-benzo[<i>f</i>]chromen-2-yl]phosphonate
;
_journal_coeditor_code           NG2458
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1240
_journal_page_last               o1241
_journal_paper_doi               10.1107/S1600536808015857
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C24 H25 O7 P'
_chemical_formula_moiety         'C24 H25 O7 P'
_chemical_formula_sum            'C24 H25 O7 P'
_chemical_formula_weight         456.41
_chemical_melting_point_gt       396
_chemical_melting_point_lt       398
_chemical_name_systematic
;
rac-(1S,2R)-Diethyl
6-hydroxy-1-(4-methoxyphenyl)-3-oxo-2,3-dihydro-1H-
benzo[f]chromen-2-yl]phosphonate
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.8060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.6231(17)
_cell_length_b                   10.0018(8)
_cell_length_c                   22.4011(17)
_cell_measurement_reflns_used    8721
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.274
_cell_measurement_theta_min      2.236
_cell_volume                     4498.0(6)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37601
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0691P)^2^+2.0425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                3585
_reflns_number_total             5076
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2458.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2218773
_cod_database_fobs_code          2218773