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_2017769
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 94.7097(13)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.4453(4)
_cell_length_b                   15.9587(3)
_cell_length_c                   6.20073(11)
_cell_measurement_temperature    298
_cell_volume                     1621.86(6)
_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    0.613
_exptl_absorpt_correction_T_max  0.89354
_exptl_absorpt_correction_T_min  0.89289
_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) = 0.0434000
Correction is not refined
;
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_F_000             600
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     'fine powder (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        69.99
_pd_meas_2theta_range_min        6.0
_pd_meas_scan_method             step
_pd_phase_name                   'HMPAO Meso Beta'
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        69.95945
_pd_proc_2theta_range_min        5.96945
_pd_proc_info_datetime           2010-06-22T20:12:20
_pd_proc_ls_background_function
;
GSAS background function number 1 with 20 terms.
Shifted Chebyshev function of 1st kind
      1:    1694.08     2:   -1888.90     3:    780.704     4:   -143.263
      5:   -45.4949     6:    51.0746     7:    7.48171     8:   -51.4972
      9:    12.7024    10:    17.5629    11:   -17.3374    12:    2.64363
     13:    3.91414    14:   -2.81271    15:    4.80400    16:    5.62048
     17:   -5.95626    18:    1.07944    19:    1.90253    20:   -5.42175
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_profile_function
;
CW Profile function number 4 with 21 terms
Pseudovoigt profile coefficients as parameterized in Thompson <i>et al.</i>
(1987).
Asymmetry correction of (Finger <i>et al.</i>, 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
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        0.0203
_pd_proc_ls_prof_wR_expected     0.0235
_pd_proc_ls_prof_wR_factor       0.0271
_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         0.110
_refine_diff_density_min         -0.107
_refine_ls_goodness_of_fit_all   1.16
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_restraints     104
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_number_total             699
_cod_data_source_file            sq3256.cif
_cod_data_source_block           Ibeta
_cod_original_cell_volume        1621.86(7)
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017769