Drug solid solutions ‒ a method for tuning phase transformations
Delori, Amit; Maclure, Pauline; Bhardwaj, Rajni M.; Johnston, Andrea; Florence, Alastair J.; Sutcliffe, Oliver B.; Oswald, Iain D. H.; CrystEngComm 16 (2014) 5827–; doi:10.1039/c4ce00211c

data_7216525
_publ_section_title
;
 Drug solid solutions -- a method for tuning phase transformations
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_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5827
_journal_paper_doi               10.1039/c4ce00211c
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C11 H16 N O,  0.4(Br),  0.6(Cl)'
_chemical_formula_sum            'C11 H16 Br0.4 Cl0.6 N O'
_chemical_formula_weight         231.63
_chemical_melting_point          494
_chemical_name_systematic
'60:40 (+-)-4'-methylmethcathinone hydrochloride hydrobromide salt solution'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90.359(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1409(11)
_cell_length_b                   22.488(3)
_cell_length_c                   10.4979(11)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    123
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     2394.0(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15233
_diffrn_reflns_theta_full        25.088
_diffrn_reflns_theta_max         25.864
_diffrn_reflns_theta_min         1.811
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             970.105
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         4.08
_refine_diff_density_min         -4.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.5578
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4333
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.1186
_refine_ls_shift/su_max          0.0051076
_refine_ls_shift/su_mean         0.0000928
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4127
_refine_ls_wR_factor_gt          0.3897
_refine_ls_wR_factor_ref         0.4127
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2731
_reflns_number_total             4353
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.03
_oxford_diffrn_Wilson_scale      229.13
_oxford_refine_ls_r_factor_ref   0.1608
_oxford_refine_ls_scale          0.0942(2)
_oxford_reflns_number_all        4333
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_123k_0m in P2(1)/c'
_cod_data_source_file            c4ce00211c2.cif
_cod_data_source_block           1c_6040
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '494 K' was changed to '494' - the
value should be numeric and without a unit
designator.

'_atom_sites_solution_primary' value 'Other' changed to
'other' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7216513--7216526.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C11 H16 Br0.40 Cl0.60 N O'
_cod_database_code               7216525
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV CL(10, X'S) BR(11, X'S) 
EQUIV CL(20, X'S) BR(21, X'S) 
EQUIV CL(10, OCC) BR(11, OCC) 
WEIGHT -1 BR(11, OCC) 
EQUIV CL(20, OCC) BR(21, OCC) 
WEIGHT -1 BR(21, OCC) 
RIDE C   (   1,X'S) H   (  13,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 113,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE N   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 133,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) H   ( 143,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) H   ( 243,X'S) 
RIDE N   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 263,X'S) H   ( 261,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
VIBRATION 0.0, 0.020000 = CL(20) TO BR(21) 
U(IJ)'S  0.0, 0.010000 = CL(20) TO BR(21) 
VIBRATION 0.0, 0.020000 = CL(10) TO BR(11) 
U(IJ)'S  0.0, 0.010000 = CL(10) TO BR(11) 
END                                                                             
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