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_4506841
_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             2012-06-07
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.565(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9293(6)
_cell_length_b                   8.3361(2)
_cell_length_c                   15.5173(6)
_cell_measurement_reflns_used    13067
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.3546
_cell_measurement_theta_min      3.2401
_cell_volume                     1696.09(13)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -29.00   -1.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 39

  2 omega    0.00   68.60   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 98

  3 omega   47.00  104.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 82

  4 omega   11.00   66.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000    0.0000 79

  5 omega   27.00  110.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   60.0000 119

  6 omega  -10.00   67.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000   90.0000 110

  7 omega   44.00   83.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -114.0000  -41.0000 57

  8 omega   40.00   71.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -180.0000 45

  9 omega  144.00  171.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000  -90.0000 39

 10 omega   43.00   81.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -30.0000 55

 11 omega   40.00   69.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  150.0000 42

 12 omega  104.00  131.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  121.0000  133.0000 39

 13 omega  147.00  174.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  121.0000  133.0000 39

 14 omega   39.00   66.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000    0.0000 39

 15 omega   49.00   74.20   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  150.0000 36

 16 omega   39.00   70.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -120.0000 45

 17 omega   39.00   70.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   90.0000 45

 18 omega   42.00   67.20   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -180.0000 36

 19 omega   89.00  114.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -114.0000  -41.0000 37

 20 omega   40.00   69.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  120.0000 42

 21 omega   39.00   70.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 45

 22 omega  119.90  178.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000   90.0000 83

 23 omega  136.00  167.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000 -180.0000 45

 24 omega  102.00  131.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000  -90.0000 42

 25 omega   36.00   68.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 47

 26 omega  -26.00   33.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 85

 27 omega  -98.00  -70.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 39

 28 omega  -50.00  -13.60   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 52

 29 omega  -42.00  -12.60   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 42

 30 omega  -42.00  -12.60   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 42

 31 omega  -45.00  -12.80   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 46

 32 omega  -95.00  -67.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 39

 33 omega  -47.00  -12.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 49

 34 omega -113.00  -85.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 39

 35 omega  -46.00  -13.10   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 47

 36 omega   27.00   69.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -90.0000 60

 37 omega   59.00  102.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -120.0000 62

 38 omega  -12.00   78.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000 -150.0000 129

 39 omega  -14.00   85.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000   90.0000 142

 40 omega  -10.00   66.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000 -120.0000 109

 41 omega   77.00  115.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -155.0000   68.0000 55

 42 omega   93.00  118.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 37

 43 omega   26.00  123.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -180.0000 139

 44 omega   26.00   53.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 39

 45 omega  -16.00   11.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000  -30.0000 39

 46 omega   29.00  119.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -30.0000 129

 47 omega   29.00   56.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -120.0000 39

 48 omega   29.00  124.20   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   30.0000 136

 49 omega   75.00  111.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -90.0000 52

 50 omega   43.00   70.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000  -30.0000 39

 51 omega   91.00  146.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  150.0000 79

 52 omega   82.00  107.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   60.0000 37

 53 omega  129.00  168.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 57

 54 omega   90.00  125.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  -60.0000 50

 55 omega   82.00  111.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 42

 56 omega   82.00  107.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 37

 57 omega   82.00  109.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 39

 58 omega   82.00  116.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 49

 59 omega  138.00  173.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 50

 60 omega   82.00  145.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 91

 61 omega   79.00  122.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000 -150.0000 62

 62 omega   82.00  133.10   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 73

 63 omega  136.00  163.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 39

 64 omega   82.00  107.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 37

 65 omega   90.00  142.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000   90.0000 75

 66 omega   82.00  107.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 37

 67 omega  113.00  176.70   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000 -120.0000 91

 68 omega   78.00  132.60   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  -60.0000 78

 69 omega   99.00  137.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -155.0000 -106.0000 55

 70 omega  138.00  165.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 39

 71 omega   78.00  119.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000    0.0000 59

 72 omega   91.00  150.50   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  120.0000 85

 73 omega   51.00   80.40   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   30.0000 42

 74 omega   79.00  107.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  -90.0000 40

 75 omega   65.00   92.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -155.0000 -106.0000 39

 76 omega   42.00   67.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 37

 77 omega   91.00  133.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000    0.0000 60

 78 omega   82.00  107.90   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 37

 79 omega   91.00  177.10   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -150.0000 123

 80 omega   82.00  140.10   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000    0.0000 83

 81 omega   82.00  109.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -60.0000 39

 82 omega  127.00  154.30   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000 -150.0000 39

 83 omega   41.00  104.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -87.0000 -169.0000 90

 84 omega   70.00  105.00   0.7000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   42.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0986859000
_diffrn_orient_matrix_UB_12      0.0336561000
_diffrn_orient_matrix_UB_13      -0.0052246000
_diffrn_orient_matrix_UB_21      -0.0626549000
_diffrn_orient_matrix_UB_22      0.0202653000
_diffrn_orient_matrix_UB_23      -0.1121528000
_diffrn_orient_matrix_UB_31      -0.0113171000
_diffrn_orient_matrix_UB_32      0.1806205000
_diffrn_orient_matrix_UB_33      0.0136348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23656
_diffrn_reflns_theta_full        72.50
_diffrn_reflns_theta_max         72.50
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    3.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40027
_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    1.257
_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         0.239
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      2.262
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.2689
_refine_ls_wR_factor_ref         0.2726
_reflns_number_gt                3076
_reflns_number_total             3318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300943b_si_002.cif
_cod_data_source_block           Form1-THF-CL
_cod_database_code               4506841
_chemical_oxdiff_formula         'c17 h20 n2 s1 cl2'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97