Crystal Engineering of Pharmaceutical Co-crystals: Application of Methyl Paraben as Molecular Hook
Mujeeb Khan; Volker Enkelmann; Gunther Brunklaus; Journal of the American Chemical Society 132 (2010) 5254–5263; doi:10.1021/ja100146f

data_4102233
_publ_contact_author_address
; Max-Planck-Institute for Polymer Research 
 Ackermannweg 10 
 D-55128 Mainz
 Germany 
;
_publ_contact_author_email       brunklaus@mpip-mainz.mpg.de
_publ_contact_author_fax         '+49 379100'
_publ_contact_author_name        'Gunther Brunklaus'
_publ_contact_author_phone       '+49 379240'
_publ_section_title
;
 Crystal Engineering of Pharmaceutical Co-crystals: Application of Methyl
 Paraben as Molecular Hook
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5254
_journal_page_last               5263
_journal_paper_doi               10.1021/ja100146f
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H32 N2 O5'
_chemical_formula_sum            'C28 H32 N2 O5'
_chemical_formula_weight         476.57
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-05-26
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9621(2)
_cell_length_b                   11.4794(3)
_cell_length_c                   21.7107(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2482.81(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.069
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22363
_diffrn_reflns_theta_full        29.537
_diffrn_reflns_theta_max         29.537
_diffrn_reflns_theta_min         1.876
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.30
_refine_ls_abs_structure_details 'Flack (1983), 3003 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.1(09)
_refine_ls_goodness_of_fit_ref   1.1090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000176
_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: 

 1.23 0.547 0.917 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0567
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0416
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                4239
_reflns_number_total             6881
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            ja100146f_si_002.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4102233