Crystal Design Approaches for the Synthesis of Paracetamol Co-Crystals
Srirambhatla, Vijay K.; Kraft, Arno; Watt, Stephen; Powell, Anthony V.; Crystal Growth & Design 12 (2012) 4870–; doi:10.1021/cg300689m

data_4506701
_publ_section_title
;
 Crystal Design Approaches for the Synthesis of Paracetamol Co-Crystals
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4870
_journal_paper_doi               10.1021/cg300689m
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C8 H9 N O2, 0.5(C6 H14 N2)'
_chemical_formula_sum            'C11 H16 N2 O2'
_chemical_formula_weight         208.2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                106.205(4)
_cell_angle_beta                 91.404(5)
_cell_angle_gamma                90.153(5)
_cell_formula_units_Z            2
_cell_length_a                   5.0174(5)
_cell_length_b                   8.8907(9)
_cell_length_c                   12.7562(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     546.23(10)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_device       Bruker
_diffrn_measurement_device_type  'Bruker X8 Apex 2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16504
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         39.754
_diffrn_reflns_theta_min         2.386
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.9080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0723
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.0004190
_refine_ls_shift/su_mean         0.0000337
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.205 0.191 0.608E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0655
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0425
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4686
_reflns_number_total             5513
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0375
_oxford_refine_ls_scale          0.3888(5)
_oxford_reflns_number_all        5507
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg300689m_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4506701
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE N   (   1,X'S) H   (  16,X'S) H   (  15,X'S) 
RIDE N   (   2,X'S) H   (   2,X'S) 
RIDE C   (   2,X'S) H   (  14,X'S) 
RIDE C   (   3,X'S) H   (   3,X'S) 
RIDE C   (   4,X'S) H   (   4,X'S) 
RIDE C   (   5,X'S) H   (   5,X'S) 
RIDE C   (   8,X'S) H   (   7,X'S) H   (   8,X'S) H   (   6,X'S) 
RIDE C   (   9,X'S) H   (   9,X'S) 
RIDE C   (  10,X'S) H   (  11,X'S) H   (  10,X'S) 
RIDE C   (  11,X'S) H   (  13,X'S) H   (  12,X'S) 
RIDE O   (   1,X'S) H   (   1,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;