Crystal structure of diethyl {2,2,2-trichloro-1-[2-(1,3-dioxo-2,3-dihydro-1<i>H</i>-isoindol-2-yl)-4-methylpentanamido]ethyl}phosphonate
Brovarets, V. S.; Golovchenko, O. V.; Rusanov, E. B.; Rusanova, J. A.; Acta Crystallographica Section E 74 (2018) 915–917; doi:10.1107/S2056989018008277

data_2242528
_publ_section_title
;
 Crystal structure of diethyl
 {2,2,2-trichloro-1-[2-(1,3-dioxo-2,3-dihydro-1<i>H</i>-isoindol-2-yl)-4-methylpentanamido]ethyl}phosphonate
;
_journal_coeditor_code           LH5875
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              915
_journal_page_last               917
_journal_paper_doi               10.1107/S2056989018008277
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C20 H26 Cl3 N2 O6 P'
_chemical_formula_moiety         'C20 H26 Cl3 N2 O6 P'
_chemical_formula_sum            'C20 H26 Cl3 N2 O6 P'
_chemical_formula_weight         527.75
_chemical_name_systematic
'Diethyl {2,2,2-trichloro-1-[2-(1,3-dioxo-2,3-dihydro-1<i>H</i>-isoindol-2-yl)-4-methylpentanamido]ethyl}phosphonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                78.188(2)
_cell_angle_beta                 88.644(2)
_cell_angle_gamma                75.442(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4601(2)
_cell_length_b                   10.9425(3)
_cell_length_c                   13.5321(4)
_cell_measurement_reflns_used    2780
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      45.8
_cell_measurement_theta_min      3.4
_cell_volume                     1186.32(6)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16619
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.233
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.444
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                3306
_reflns_number_total             4423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5875sup1.cif
_cod_data_source_block           I
_cod_database_code               2242528
_cod_database_fobs_code          2242528
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.962
_shelx_hkl_checksum              2319
_shelx_res_checksum              4000