Powder X-ray studies of <i>meso</i>-hexamethyl propylene amine oxime (<i>meso</i>-HMPAO) in two different phases
Al-Ktaifani, Mahmoud; Rukiah, Mwaffak; Acta Crystallographica, Section C 66 (2010) o479–o483; doi:10.1107/S0108270110032014

data_2017768
_publ_section_title
;
 Powder X-ray studies of <i>meso</i>-hexamethyl propylene amine oxime
 (<i>meso</i>-HMPAO) in two different phases
;
_journal_coeditor_code           SQ3256
_journal_issue                   9
_journal_name_full               'Acta Crystallographica, Section C'
_journal_page_first              o479
_journal_page_last               o483
_journal_paper_doi               10.1107/S0108270110032014
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H28 N4 O2'
_chemical_formula_moiety         'C13 H28 N4 O2'
_chemical_formula_sum            'C13 H28 N4 O2'
_chemical_formula_weight         272.39
_chemical_name_common
;
meso-hexamethyl propylene amine oxime (meso-HMPAO)
;
_chemical_name_systematic
;
<i>meso</i>-3,3'-[2,2-dimethylpropane-1,3-diylbis(azanediyl)]dibutan-2-one
dioxime
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.1652(10)
_cell_angle_beta                 93.4835(10)
_cell_angle_gamma                96.4282(8)
_cell_formula_units_Z            2
_cell_length_a                   15.3159(3)
_cell_length_b                   8.74371(12)
_cell_length_c                   6.21770(9)
_cell_measurement_temperature    298
_cell_volume                     816.80(2)
_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  'Stoe STADI P'
_diffrn_radiation_monochromator  'Ge 111'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.66853
_exptl_absorpt_correction_T_min  0.66015
_exptl_absorpt_process_details
;
GSAS absorption/surface roughness correction (Larson & Von Dreele,
2004):
function number 4. Flat plate in transmission mode, absorption correction
Term (= MU.r/wave) =     0.16000
Correction is not refined.
;
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       needle
_exptl_crystal_F_000             300
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     'needle (visual estimate)'
_pd_instr_dist_mono/spec         230
_pd_instr_dist_spec/detc         220
_pd_instr_dist_src/mono          260
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        79.99
_pd_meas_2theta_range_min        3.0
_pd_meas_number_of_points        7700
_pd_meas_scan_method             step
_pd_phase_name                   'HMPAO Meso Alpha'
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        79.98161
_pd_proc_2theta_range_min        2.99161
_pd_proc_info_datetime           2010-06-21T10:10:05
_pd_proc_ls_background_function
;
GSAS background function number 1 with 20 terms.
Shifted Chebyshev function of 1st kind
      1:    2095.63     2:   -2093.54     3:    1003.99     4:   -224.356
      5:   -35.0151     6:    46.3120     7:    9.05002     8:   -15.5584
      9:   -4.55608    10:    16.8935    11:   -8.33517    12:    3.12503
     13:  -0.184876    14:   -14.2318    15:    26.9383    16:   -17.5033
     17:    5.55156    18:   -2.00997    19:    10.5513    20:   -2.64504
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_profile_function
;
CW Profile function number 4 with 27 terms
Pseudovoigt profile coefficients as parameterized in Thompson <i>et al.</i>
(1987).
Asymmetry correction of (Finger <i>et al.</i>, 1994).
Microstrain broadening (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
Stephens, P. W. (1999). <i>J. Appl. Cryst.</i> <b>32</b>, 281--289.
Thompson, P., Cox, D. E. & Hastings, J. B. (1987). <i>J. Appl.
Cryst.</i>
<b>20</b>, 79--83.
;
_pd_proc_ls_prof_R_factor        0.0169
_pd_proc_ls_prof_wR_expected     0.0191
_pd_proc_ls_prof_wR_factor       0.0225
_pd_proc_number_of_points        7700
_pd_spec_mounting                'drifted powder between two Mylar foils'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              7
_pd_spec_size_equat              7
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.253
_refine_ls_goodness_of_fit_all   1.19
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_restraints     104
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_number_total             998
_cod_data_source_file            sq3256.cif
_cod_data_source_block           Ialpha
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               2017768