Crystal structure of ethyl 2-(diethoxyphosphoryl)-2-(2,3,4-trimethoxyphenyl)acetate
Schubert, Moritz; Schollmeyer, Dieter; Waldvogel, Siegfried R.; Acta Crystallographica Section E 70 (2014) o897–o898; doi:10.1107/S1600536814015803

data_2239855
_publ_section_title
;
 Crystal structure of ethyl
 2-(diethoxyphosphoryl)-2-(2,3,4-trimethoxyphenyl)acetate
;
_journal_coeditor_code           HB7246
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o897
_journal_page_last               o898
_journal_paper_doi               10.1107/S1600536814015803
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C17 H27 O8 P'
_chemical_formula_sum            'C17 H27 O8 P'
_chemical_formula_weight         390.35
_chemical_name_systematic
;
Ethyl 2-(diethoxyphosphoryl)-2-(2,3,4-trimethoxyphenyl)acetate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.117(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6314(14)
_cell_length_b                   23.749(4)
_cell_length_c                   8.8155(14)
_cell_measurement_reflns_used    3917
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.3
_cell_volume                     1955.5(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2008<i>a</i>)'
_computing_structure_solution    'SHELXS2014 (Sheldrick, 2008<i>a</i>)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3859
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2008<i>b</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+2.5572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                3033
_reflns_number_total             3859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7246sup1.cif
_cod_data_source_block           I
_cod_database_code               2239855
_cod_database_fobs_code          2239855
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.989
_shelx_hkl_checksum              65243
_shelx_res_checksum              30363
_shelxl_version_number           2.014