Powder X-ray study of racemic (2<i>RS</i>,3<i>RS</i>)-5-amino-3-[4-(3-methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalen-2-ol
Assaad, Thaer; Rukiah, Mwaffak; Acta Crystallographica Section C 67 (2011) o469–o472; doi:10.1107/S0108270111040844

data_2018270
_publ_section_title
;
 Powder X-ray study of racemic
 (2<i>RS</i>,3<i>RS</i>)-5-amino-3-[4-(3-methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalen-2-ol
;
_journal_coeditor_code           CU3006
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o469
_journal_page_last               o472
_journal_paper_doi               10.1107/S0108270111040844
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H27 N3 O2'
_chemical_formula_moiety         'C21 H27 N3 O2'
_chemical_formula_sum            'C21 H27 N3 O2'
_chemical_formula_weight         353.47
_chemical_name_systematic
;
(2<i>RS</i>,3<i>RS</i>)-5-amino-3-[4-(3-methoxyphenyl)piperazin-1-yl]-
1,2,3,4-tetrahydronaphthalen-2-ol
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 102.8536(11)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.6234(3)
_cell_length_b                   8.90929(16)
_cell_length_c                   17.2752(3)
_cell_measurement_temperature    298
_cell_volume                     1894.18(7)
_computing_cell_refinement       'GSAS (Larson & Von Dreele, 2004)'
_computing_data_collection       'WinXPOW (Stoe & Cie, 1999)'
_computing_data_reduction        'WinXPOW (Stoe & Cie, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'GSAS (Larson & Von Dreele, 2004)'
_computing_structure_solution    'FOX (Favre-Nicolin & \<Cern\'y, 2002)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'transmission Stoe STADI P'
_diffrn_radiation_monochromator  'Ge 111'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.54060
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.50220
_exptl_absorpt_correction_T_min  0.39106
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details   '(GSAS; Larson & Von Dreele, 2004)'
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_F_000             760
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     'fine powder'
_pd_instr_dist_mono/spec         130
_pd_instr_dist_spec/detc         173
_pd_instr_dist_src/mono          260
_pd_instr_location
;
Chemistry Department
Atomic Energy Commission
Damascus
PO Box 6091
Syrian Arab Republic
;
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        84.98
_pd_meas_2theta_range_min        5.0
_pd_meas_number_of_points        4000
_pd_meas_scan_method             step
_pd_phase_name                   (2R,3R)-I
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        84.97774
_pd_proc_2theta_range_min        4.99774
_pd_proc_info_data_reduction     none
_pd_proc_info_datetime           2011-01-23T13:58:47
_pd_proc_info_excluded_regions   ' none'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    2554.25     2:   -2039.65     3:    718.920     4:    109.607
      5:   -289.817     6:    191.958     7:   -40.7231     8:   -116.523
      9:    113.592    10:    19.7866    11:   -99.1759    12:    72.3448
     13:   -3.45975    14:   -24.3312    15:   -3.96068    16:    5.86789
     17:    6.99931    18:   -6.30464    19:   -5.20851    20:    7.35489
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_pref_orient_corr
;
March-Dollase
AXIS  1 Ratio = 1.18166  h = 1.000  k = 0.000  l = 0.000
Preferred orientation correction range: Min = 0.60606, Max = 1.28452
;
_pd_proc_ls_profile_function
;
 CW Profile function number 4 with  21 terms
 Pseudo-voigt profile coefficients as
 parameterized in (Thompson, et al., 1987).
 Asymmetry correction of (Finger et al., 1994).
 Microstrain broadening by (Stephens, 1999).
 Peak tails are ignored  where the intensity is below 0.0010 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0186
_pd_proc_ls_prof_wR_expected     0.0170
_pd_proc_ls_prof_wR_factor       0.0241
_pd_proc_number_of_points        4000
_pd_spec_mounting                'powder loaded between two Mylar foils'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              8
_pd_spec_size_equat              8
_refine_diff_density_max         0.121
_refine_diff_density_min         -0.109
_refine_ls_goodness_of_fit_all   1.65
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_restraints     29
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.00
_reflns_number_total             1335
_cod_data_source_file            cu3006.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018270