Crystal structure of (4-methoxyphenyl)[(4-methoxyphenyl)phosphonato]dioxidophosphate(1{-}) 2-amino-6-benzyl-3-ethoxycarbonyl-4,5,6,7-tetrahydrothieno[2,3-<i>c</i>]pyridin-6-ium
Mague, Joel T.; Mohamed, Shaaban K.; Akkurt, Mehmet; Younes, Sabry H. H.; Ahmed, Essam K.; Albayati, Mustafa R.; Acta Crystallographica Section E 71 (2015) o997–o998; doi:10.1107/S2056989015022331

data_2241376
_publ_section_title
;
 Crystal structure of
 (4-methoxyphenyl)[(4-methoxyphenyl)phosphonato]dioxidophosphate(1{-})
 2-amino-6-benzyl-3-ethoxycarbonyl-4,5,6,7-tetrahydrothieno[2,3-<i>c</i>]pyridin-6-ium
;
_journal_coeditor_code           HB7549
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o997
_journal_page_last               o998
_journal_paper_doi               10.1107/S2056989015022331
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C17 H21 N2 O2 S +, C14 H15 O7 P2 -'
_chemical_formula_moiety         'C17 H21 N2 O2 S, C14 H15 O7 P2'
_chemical_formula_sum            'C31 H36 N2 O9 P2 S'
_chemical_formula_weight         674.62
_chemical_name_systematic
;(4-Methoxyphenyl)[(4-methoxyphenyl)phosphonato]dioxidophosphate(1-)
2-amino-6-benzyl-3-ethoxycarbonyl-4,5,6,7-tetrahydrothieno[2,3-<i>c</i>]pyridin-6-ium
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                107.099(2)
_cell_angle_beta                 90.376(2)
_cell_angle_gamma                96.899(2)
_cell_formula_units_Z            4
_cell_length_a                   12.443(2)
_cell_length_b                   15.194(3)
_cell_length_c                   17.856(3)
_cell_measurement_reflns_used    4184
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      23.1193
_cell_measurement_theta_min      2.1735
_cell_volume                     3200.1(10)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2015)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2015)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27878
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.862
_diffrn_reflns_theta_min         1.194
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2015)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13602
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                6997
_reflns_number_total             13602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7549sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3200.4(10)
_cod_database_code               2241376
_cod_database_fobs_code          2241376
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              12556
_shelx_res_checksum              52585