Selective transformation pathways between crystalline forms of an organic material established from powder X-ray diffraction analysis
Fujii, Kotaro; Ashida, Yasunari; Uekusa, Hidehiro; Guo, Fang; Harris, Kenneth D. M.; Chemical Communications 46 (2010) 4264–4266; doi:10.1039/c0cc00233j

data_7111673
_publ_section_title
;
 Selective transformation pathways between crystalline forms of an organic
 material established from powder X-ray diffraction analysis
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              4264
_journal_page_last               4266
_journal_paper_doi               10.1039/c0cc00233j
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C10 H6 O8 . 2(C H4 O)'
_chemical_formula_sum            'C12 H14 O10'
_chemical_formula_weight         318.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.827(2)
_cell_angle_beta                 88.318(2)
_cell_angle_gamma                89.997(2)
_cell_formula_units_Z            2
_cell_length_a                   3.8860(3)
_cell_length_b                   11.0240(9)
_cell_length_c                   15.9140(13)
_cell_measurement_reflns_used    9230
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.28
_cell_volume                     681.45(9)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004(Burla et al.,2004)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9230
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_type              'Rigaku Ultrax18'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.808366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.9256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                2918
_reflns_number_total             3119
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           pam
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