Guest-Directed Assembly of Caffeine and Succinic Acid into Topologically Different Heteromolecular Host Networks upon Grinding
Friščić, Tomislav; Trask, Andrew V.; Motherwell, W. D. S.; Jones, W.; Crystal Growth & Design 8 (2008) 1605–; doi:10.1021/cg700929e

data_4503272
_publ_section_title
;
 Guest-Directed Assembly of Caffeine and Succinic Acid into Topologically
 Different Heteromolecular Host Networks upon Grinding
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1605
_journal_paper_doi               10.1021/cg700929e
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         '4(C8 H10 N4 O2), (C4 H6 O4), 2(C1 H1 Cl3)'
_chemical_formula_sum            'C38 H48 Cl6 N16 O12'
_chemical_formula_weight         1133.1
_chemical_name_common            2.(CHCl3)2
_chemical_name_systematic
;
 caffeine-succinic acid-chloroform 4/1/2
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.64390(10)
_cell_length_b                   23.2514(4)
_cell_length_c                   33.5615(7)
_cell_measurement_reflns_used    14947
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     5184.58(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            14049
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.0107(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1545P)^2^+10.5169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2459
_refine_ls_wR_factor_ref         0.2849
_reflns_number_gt                2077
_reflns_number_total             3152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg700929e-file003.cif
_cod_data_source_block           2.(CHCl3)2
_cod_original_sg_symbol_H-M      Cmca
_cod_database_code               4503272