Searching for novel crystal forms by in situ high-pressure crystallisation: the example of gabapentin heptahydrate
Fabbiani, Francesca P. A.; Levendis, Demetrius C.; Buth, Gernot; Kuhs, Werner F.; Shankland, Norman; Sowa, Heidrun; CrystEngComm 12 (2010) 2354–; doi:10.1039/b924573a

data_7212308
_publ_section_title
;
 Searching for novel crystal forms by in situ high-pressure
 crystallisation: the example of gabapentin heptahydrate
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2354
_journal_paper_doi               10.1039/b924573a
_journal_volume                  12
_journal_year                    2010
_chemical_compound_source
;
The compound was used as received from Sigma-Aldrich
;
_chemical_formula_moiety         'C9 H17 N O2, 7(H2 O) '
_chemical_formula_sum            'C9 H31 N O9'
_chemical_formula_weight         297.35
_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                86.297(6)
_cell_angle_beta                 78.924(11)
_cell_angle_gamma                72.713(6)
_cell_formula_units_Z            2
_cell_length_a                   6.7906(12)
_cell_length_b                   7.3159(4)
_cell_length_c                   15.8428(14)
_cell_measurement_reflns_used    1722
_cell_measurement_temperature    293
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     737.49(16)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    MERCURY
_computing_publication_material
'CRYSTALS (Betteridge et al., 2003), PLATON, XCIF, ENCIFER'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.573
_diffrn_measured_fraction_theta_max 0.516
_diffrn_measurement_device       'Bruker AXS SMART APEX'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72000
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6429
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         26.573
_diffrn_reflns_theta_min         2.654
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'based on symmetry-related measuraments'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_preparation
;
High-pressure crystallisation of aqueous solution at 0.8 GPa.
Single-crystal data collected at 0.9 GPa
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9522
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1523
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.000126
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 0.27P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1310
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1310
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1294
_reflns_number_total             1533
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.59
_oxford_diffrn_Wilson_scale      0.49
_oxford_refine_ls_r_factor_ref   0.0528
_oxford_refine_ls_scale          4.99(18)
_oxford_reflns_number_all        1523
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            b924573a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C9 H31 N1 O9'
_cod_database_code               7212308