Influence of impurities on the crystallisation of 5-X-aspirin and 5-X-aspirin anhydride polymorphs (X = Cl, Br, Me)
Solanko, Katarzyna A.; Bond., Andrew D.; CrystEngComm 13 (2011) 6991–; doi:10.1039/c1ce06065a

data_7206873
_publ_section_title
;
 Influence of impurities on the crystallisation of 5-X-aspirin and
 5-X-aspirin anhydride polymorphs (X = Cl, Br, Me)
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              6991
_journal_paper_doi               10.1039/c1ce06065a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C20 H18 O7'
_chemical_formula_sum            'C20 H18 O7'
_chemical_formula_weight         370.34
_chemical_name_common            '5-Me-aspirin anhydride (form I)'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.485(7)
_cell_angle_beta                 109.352(7)
_cell_angle_gamma                117.882(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9176(9)
_cell_length_b                   9.9757(10)
_cell_length_c                   11.5419(17)
_cell_measurement_reflns_used    2144
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      2.42
_cell_volume                     908.3(2)
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_collection       'APEX2 v2010.1-2 (Bruker, 2010)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL v.6.12 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Nonius X8APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10529
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                1997
_reflns_number_total             3189
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1ce06065a.txt
_cod_data_source_block           5-Me-AA_I
_cod_original_cell_volume        908.32(18)
_cod_database_code               7206873