Synthesis and crystal structure of bis-(2-phthal-imido-eth-yl)ammonium chloride dihydrate.
Young, Barry S.; Lee, Jamie L.; Gembicky, Milan; Bailey, Jake; Smith, Gary L. N.; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 575–577; doi:10.1107/S2056989023004565

data_2022773
_publ_section_title
;
 Synthesis and crystal structure of bis-(2-phthal-imido-eth-yl)ammonium
 chloride dihydrate.
;
_journal_coeditor_code           EX2070
_journal_issue                   'Pt 6'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              575
_journal_page_last               577
_journal_paper_doi               10.1107/S2056989023004565
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C20 H18 N3 O4 +, Cl -, 2H2 O'
_chemical_formula_moiety         'C20 H18 N3 O4 +, Cl -, 2(H2 O)'
_chemical_formula_sum            'C20 H22 Cl N3 O6'
_chemical_formula_weight         435.85
_chemical_name_common
;
Bis(2-phthalimidoethyl)ammonium chloride dihydrate
;
_chemical_name_systematic
;
Bis[2-(1,3-dioxoisoindol-2-yl)ethyl]azanium chloride dihydrate
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.7191(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0401(6)
_cell_length_b                   15.4829(7)
_cell_length_c                   11.2543(6)
_cell_measurement_reflns_used    8573
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.56
_cell_volume                     2019.52(17)
_computing_cell_refinement
;
SAINT v8.40B (Bruker, 2019)
;
_computing_data_collection
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APEX4 v2022.1-1 (Bruker, 2022)
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SAINT v8.40B (Bruker, 2019)
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
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SHELXL  (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon III Area Detector'
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0312
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            59713
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  0.7435
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.225
_refine_ls_extinction_coef       0.0027(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/1 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0289P)^2^+1.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                3430
_reflns_number_total             4126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2070sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022773.cif.'
_cod_database_code               2022773
_cod_database_fobs_code          2022773
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.990
_shelx_hkl_checksum              3926
_shelx_res_checksum              89716