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_4506842
_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             2012-06-08
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.696(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8123(8)
_cell_length_b                   8.3170(2)
_cell_length_c                   15.5334(8)
_cell_measurement_reflns_used    7752
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7132
_cell_measurement_theta_min      3.2106
_cell_volume                     1694.37(17)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   40.00   77.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 37

  2 omega  -64.00  -14.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   90.0000 50

  3 omega  -23.00    4.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 27

  4 omega  -29.00   50.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -120.0000 79

  5 omega  -12.00   37.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   90.0000 49

  6 omega  -76.00   17.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -56.8839   45.0000   60.0000 93

  7 omega   25.00   73.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -       56.8839  -45.0000  -30.0000 48

  8 omega   21.00  130.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -       56.8839   77.0000 -120.0000 109

  9 omega    3.00   91.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -       56.8839  -77.0000   90.0000 88

 10 omega  -18.00    9.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -       56.8839  -45.0000  -30.0000 27

 11 omega  -25.00    8.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  112.0000  -90.0000 33

 12 omega  -87.00  -59.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  112.0000  -90.0000 28

 13 omega  -71.00    8.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   25.0000 -150.0000 79

 14 omega  -89.00  -64.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  112.0000   30.0000 25

 15 omega  -40.00   -2.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -25.0000 -180.0000 38

 16 omega -118.00  -47.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -25.0000 -180.0000 71

 17 omega  -74.00  -28.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   50.0000  -90.0000 46

 18 omega  -92.00  -29.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   62.0000   14.0000 63

 19 omega  -51.00  -24.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   77.0000  120.0000 27

 20 omega  -86.00  -56.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  112.0000  150.0000 30

 21 omega  -21.00    5.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  112.0000   30.0000 26

 22 omega  -27.00   -2.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   62.0000   14.0000 25

 23 omega  -97.00  -53.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   77.0000  120.0000 44

 24 omega   52.00   79.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000 -120.0000 27

 25 omega  136.00  176.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   77.0000  150.0000 40

 26 omega   35.00  107.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -89.0000    6.0000 72

 27 omega   42.00   81.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000  150.0000 39

 28 omega   52.00   82.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000  -90.0000 30

 29 omega  148.00  178.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   50.0000 -120.0000 30

 30 omega   62.00  174.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   25.0000   90.0000 112

 31 omega   92.00  148.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -92.0000  131.0000 56

 32 omega   83.00  108.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -97.0000 -109.0000 25

 33 omega   89.00  126.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   50.0000 -120.0000 37

 34 omega  109.00  175.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000  -60.0000 66

 35 omega   61.00   90.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -92.0000  131.0000 29

 36 omega  113.00  176.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000   60.0000 63

 37 omega   50.00   80.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000   60.0000 30

 38 omega  127.00  173.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -25.0000  -30.0000 46

 39 omega   46.00   82.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000    0.0000 36

 40 omega  113.00  171.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000   30.0000 58

 41 omega   91.00  164.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   50.0000    0.0000 73

 42 omega   85.00  173.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677   50.0000  -30.0000 88

 43 omega   40.00  114.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677 -106.0000  112.0000 74

 44 omega   58.00  121.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677 -125.0000  -86.0000 63

 45 omega   41.00   66.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  -50.0000   30.0000 25

 46 omega  101.00  127.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000 -180.0000 26

 47 omega  139.00  164.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000 -180.0000 25

 48 omega  114.00  163.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677  112.0000  -90.0000 49

 49 omega   64.00  113.00   1.0000    5.7200
omega____ theta____ kappa____ phi______ frames
    -      113.7677 -104.0000   -7.0000 49
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0565353000
_diffrn_orient_matrix_UB_12      0.0343635000
_diffrn_orient_matrix_UB_13      0.0599426000
_diffrn_orient_matrix_UB_21      0.0992263000
_diffrn_orient_matrix_UB_22      -0.0303551000
_diffrn_orient_matrix_UB_23      0.0946821000
_diffrn_orient_matrix_UB_31      0.0275949000
_diffrn_orient_matrix_UB_32      0.1792423000
_diffrn_orient_matrix_UB_33      0.0045376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11904
_diffrn_reflns_theta_full        70.85
_diffrn_reflns_theta_max         70.85
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.478
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.478
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0566
_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          0.1816
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                2851
_reflns_number_total             3234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300943b_si_002.cif
_cod_data_source_block           Form2-ACN-CL
_cod_database_code               4506842
_chemical_oxdiff_formula         'C17 H21 N2 S1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97