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_4506845
_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                 117.588(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8149(13)
_cell_length_b                   8.3237(5)
_cell_length_c                   15.5201(12)
_cell_measurement_reflns_used    2315
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9203
_cell_measurement_theta_min      3.2101
_cell_volume                     1696.3(3)
_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 0.805
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details
;
  1 omega    5.00   33.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  120.0000 28

  2 omega  -19.00   70.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000    0.0000 89

  3 omega   31.00  128.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       56.0000   38.0000  -30.0000 97

  4 omega   36.00   64.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000    0.0000 28

  5 omega  -10.00   21.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000  -30.0000 31

  6 omega   39.00   89.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -113.0000 -136.0000 50

  7 omega   94.00  155.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  120.0000 61

  8 omega  102.00  178.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  112.0000  150.0000 76

  9 omega   45.00   72.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -180.0000 27

 10 omega  153.00  178.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000 -180.0000 25

 11 omega   44.00   74.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000    0.0000 30

 12 omega   58.00   86.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -113.0000 -135.0000 28

 13 omega  106.00  136.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000 -180.0000 30

 14 omega   45.00   70.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -180.0000 25

 15 omega  100.00  178.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  126.0000 -140.0000 78

 16 omega   39.00   69.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 30
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0561699000
_diffrn_orient_matrix_UB_12      0.0137425000
_diffrn_orient_matrix_UB_13      0.1116172000
_diffrn_orient_matrix_UB_21      0.1002539000
_diffrn_orient_matrix_UB_22      0.0351391000
_diffrn_orient_matrix_UB_23      -0.0037302000
_diffrn_orient_matrix_UB_31      -0.0235111000
_diffrn_orient_matrix_UB_32      0.1812680000
_diffrn_orient_matrix_UB_33      -0.0075128000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4413
_diffrn_reflns_theta_full        72.07
_diffrn_reflns_theta_max         72.07
_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    3.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56576
_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          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.001
_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          0.1811
_refine_ls_wR_factor_ref         0.2006
_reflns_number_gt                2097
_reflns_number_total             2687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300943b_si_002.cif
_cod_data_source_block           Form2-THF-CL
_cod_original_cell_volume        1696.3(2)
_cod_database_code               4506845
_chemical_oxdiff_formula         'c17 h20 n2 s1 cl1'
_reflns_odcompleteness_completeness 82.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97