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_4506702
_publ_section_title
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 Crystal Design Approaches for the Synthesis of Paracetamol Co-Crystals
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_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         'C12 H10 N2, 2(C8 H9 N O2), C H4 O'
_chemical_formula_sum            'C29 H32 N4 O5'
_chemical_formula_weight         516.60
_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                82.97(3)
_cell_angle_beta                 89.69(3)
_cell_angle_gamma                73.85(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0546(18)
_cell_length_b                   10.624(2)
_cell_length_c                   14.316(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1312.3(5)
_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 0.956
_diffrn_measured_fraction_theta_max 0.953
_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  0.024
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8780
_diffrn_reflns_theta_full        25.037
_diffrn_reflns_theta_max         26.922
_diffrn_reflns_theta_min         1.434
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.9462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruket SADABS'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.0006435
_refine_ls_shift/su_mean         0.0000489
_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: 
 0.164 0.141 0.483E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0553
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0434
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4904
_reflns_number_total             5422
_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   0.0419
_oxford_refine_ls_scale          0.1641(2)
_oxford_reflns_number_all        5404
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg300689m_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4506702
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  30,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  33,X'S) 
RIDE C   (   8,X'S) H   (   7,X'S) H   (   8,X'S) H   (   6,X'S) 
RIDE C   (  10,X'S) H   (  10,X'S) 
RIDE C   (  11,X'S) H   (  11,X'S) 
RIDE C   (  12,X'S) H   (  12,X'S) 
RIDE C   (  13,X'S) H   (  13,X'S) 
RIDE C   (  16,X'S) H   (  16,X'S) H   (  15,X'S) H   (  14,X'S) 
RIDE C   (  17,X'S) H   (  17,X'S) 
RIDE C   (  18,X'S) H   (  18,X'S) 
RIDE C   (  19,X'S) H   (  19,X'S) 
RIDE C   (  20,X'S) H   (  20,X'S) 
RIDE C   (  22,X'S) H   (  22,X'S) 
RIDE C   (  23,X'S) H   (  23,X'S) 
RIDE C   (  25,X'S) H   (  25,X'S) 
RIDE C   (  26,X'S) H   (  26,X'S) 
RIDE C   (  27,X'S) H   (  27,X'S) 
RIDE C   (  28,X'S) H   (  28,X'S) 
RIDE C   (  29,X'S) H   (  29,X'S) H   (  24,X'S) H   (  21,X'S) 
RIDE O   (   1,X'S) H   (   1,X'S) 
RIDE O   (   3,X'S) H   (   3,X'S) 
RIDE O   (   5,X'S) H   (   5,X'S) 
RIDE N   (   3,X'S) H   (   2,X'S) 
RIDE N   (   4,X'S) H   (   4,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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