Supramolecular architecture in azaheterocyclic phosphonates. III. Structures of an ethyl phosphonamidate and an ethyl phosphonate
Pietrzak, Anna; Modranka, Jakub; Wojciechowski, Jakub; Janecki, Tomasz; Wolf, Wojciech M.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618009609

data_2021181
_publ_section_title
;
 Supramolecular architecture in azaheterocyclic phosphonates. III.
 Structures of an ethyl phosphonamidate and an ethyl phosphonate
;
_journal_coeditor_code           YF3147
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618009609
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C18 H25 N2 O4 P S'
_chemical_formula_moiety         'C18 H25 N2 O4 P S'
_chemical_formula_sum            'C18 H25 N2 O4 P S'
_chemical_formula_weight         396.43
_chemical_name_systematic
;Diethyl
(4-isopropyl-2-oxo-3,4-dihydro-2<i>H</i>-benzo[4,5]thiazolo[3,2-<i>a</i>]pyrimidin-3-yl)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   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                65.779(5)
_cell_angle_beta                 67.462(5)
_cell_angle_gamma                74.329(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6275(4)
_cell_length_b                   10.0903(5)
_cell_length_c                   11.8585(6)
_cell_measurement_reflns_used    10170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.9830
_cell_measurement_theta_min      4.2560
_cell_volume                     961.59(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.980
_diffrn_reflns_theta_min         4.300
_exptl_absorpt_coefficient_mu    2.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.557
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3490
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0554
_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^)+(0.1232P)^2^+0.4140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1647
_reflns_number_gt                3290
_reflns_number_total             3490
_reflns_threshold_expression     'I > 2\s(I)'
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