Salts of Amoxapine with Improved Solubility for Enhanced Pharmaceutical Applicability.
Joshi, Mayank; Roy Choudhury, Angshuman; ACS omega 3 (2018) 2406–2416; doi:10.1021/acsomega.7b02023

data_4516034
_publ_section_title
;
 Salts of Amoxapine with Improved Solubility for Enhanced Pharmaceutical
 Applicability.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              2406
_journal_page_last               2416
_journal_paper_doi               10.1021/acsomega.7b02023
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         '(C4 H3 O4)-, (C17 H17 Cl N3 O)+'
_chemical_formula_sum            'C21 H20 Cl N3 O5'
_chemical_formula_weight         429.85
_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_date             2017-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.143(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5724(6)
_cell_length_b                   9.8586(3)
_cell_length_c                   9.7866(3)
_cell_measurement_reflns_used    7223
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.0830
_cell_measurement_theta_min      2.8570
_cell_volume                     1969.47(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -69.00 119.00   0.40   10.00    --   29.89  54.00  90.00  470
  2  \w    -69.00 119.00   0.40   10.00    --   29.89  54.00-120.00  470
  3  \w    -69.00 119.00   0.40   10.00    --   29.89  54.00-150.00  470
  4  \w    -69.00  60.20   0.40   10.00    --   29.89  54.00 -90.00  323
  5  \w    -69.00 119.00   0.40   10.00    --   29.89  54.00   0.00  470
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0226990000
_diffrn_orient_matrix_UB_12      0.0477663000
_diffrn_orient_matrix_UB_13      0.0322958000
_diffrn_orient_matrix_UB_21      0.0256280000
_diffrn_orient_matrix_UB_22      -0.0478773000
_diffrn_orient_matrix_UB_23      -0.0012696000
_diffrn_orient_matrix_UB_31      0.0059086000
_diffrn_orient_matrix_UB_32      0.0244877000
_diffrn_orient_matrix_UB_33      -0.0655332000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.839
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         7218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1016P)^2^+1.0838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4998
_reflns_number_total             7218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b02023_si_004.cif
_cod_data_source_block           amx-f13-et-100k
_cod_original_cell_volume        1969.46(10)
_cod_database_code               4516034
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C17(H17A,H17B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C19(H19), C20(H20), C9(H9), C10(H10), C11(H11),
 C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.923