Distinct Disordered Forms of Promethazine Hydrochloride: A Case of Intergrowth of Polymorphic Domains?
Borodi, Gheorghe; Pop, Mihaela M.; Onija, Oana; Filip, Xenia; Crystal Growth & Design 12 (2012) 5846–; doi:10.1021/cg300943b

data_4506844
_publ_section_title
;
 Distinct Disordered Forms of Promethazine Hydrochloride: A Case of
 Intergrowth of Polymorphic Domains?
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5846
_journal_paper_doi               10.1021/cg300943b
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'Cl, C17 H21 N2 S'
_chemical_formula_sum            'C17 H21 Cl N2 S'
_chemical_formula_weight         320.87
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-02
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.882(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9859(9)
_cell_length_b                   8.3369(3)
_cell_length_c                   15.5132(10)
_cell_measurement_reflns_used    4932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.3365
_cell_measurement_theta_min      3.2508
_cell_volume                     1697.1(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.4335
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
  1 omega   35.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 37

  2 omega  -14.00   19.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 33

  3 omega -100.00  -75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -50.0000  -90.0000 25

  4 omega   41.00   85.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -135.0000   87.0000 44

  5 omega   35.00  108.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   38.0000 -120.0000 73

  6 omega   28.00  123.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -60.0000 95

  7 omega   40.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  150.0000 32

  8 omega   44.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -120.0000 27

  9 omega   45.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   90.0000 36

 10 omega   43.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   90.0000 26

 11 omega   40.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -26.0000 -111.0000 31

 12 omega   39.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  120.0000 33

 13 omega   48.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 28

 14 omega   41.00   68.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000    0.0000 27

 15 omega   41.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -97.0000  -24.0000 59

 16 omega   39.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -180.0000 25

 17 omega   50.00   83.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   30.0000 33

 18 omega  -70.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000    0.0000 100

 19 omega  -64.00   -8.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  135.0000  152.0000 56

 20 omega -113.00  -12.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 101

 21 omega -113.00  -12.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 101

 22 omega  -17.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000    0.0000  150.0000 146

 23 omega   26.00  126.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -120.0000 100

 24 omega  -17.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -26.0000  -51.0000 88

 25 omega   -1.00   97.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -97.0000  155.0000 98

 26 omega   90.00  178.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -180.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0048997000
_diffrn_orient_matrix_UB_12      -0.0550702000
_diffrn_orient_matrix_UB_13      -0.0923810000
_diffrn_orient_matrix_UB_21      0.1157287000
_diffrn_orient_matrix_UB_22      0.0317088000
_diffrn_orient_matrix_UB_23      0.0528834000
_diffrn_orient_matrix_UB_31      0.0196694000
_diffrn_orient_matrix_UB_32      -0.1734908000
_diffrn_orient_matrix_UB_33      0.0389734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9353
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         72.49
_diffrn_reflns_theta_min         5.71
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    3.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         2936
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                2313
_reflns_number_total             2936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300943b_si_002.cif
_cod_data_source_block           Form1-THF-VD
_cod_original_cell_volume        1697.07(17)
_cod_database_code               4506844
_chemical_oxdiff_formula         'c17 h20 n2 s1 cl1'
_reflns_odcompleteness_completeness 90.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97