Dipole-Induced Polymorphs of trans-2-Hydroxycycloheptanecarboxylic Acid with Virtually the Same Unit Cell
Alajos Kálmán; László Fábián; Gyula Argay; Gábor Bernáth; Zsuzsanna Gyarmati; Journal of the American Chemical Society 125 (2003) 34–35; doi:10.1021/ja0289447

data_4113383
_publ_contact_author_address
;
       Institute of Chemistry, Chemical Research Center
    Hungarian Academy of Sciences
    PO Box 17
    H-1525 Budapest
    Hungary
;
_publ_contact_author_email       akalman@cric.chemres.hu
_publ_contact_author_fax         '036 1 325-7554'
_publ_contact_author_name        'Prof. Alajos K\'alm\'an'
_publ_contact_author_phone       '036 1 325-7547'
_publ_section_title
;
 Dipole-Induced Polymorphs of trans-2-Hydroxycycloheptanecarboxylic Acid
 with Virtually the Same Unit Cell
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              34
_journal_page_last               35
_journal_paper_doi               10.1021/ja0289447
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C8 H14 O3'
_chemical_formula_sum            'C8 H14 O3'
_chemical_formula_weight         158.19
_chemical_name_common
'trans (1R*,2R*)-2-hydroxy-1-cycloheptanecarboxylic acid form A'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   21.184(3)
_cell_length_b                   6.824(1)
_cell_length_c                   5.892(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.55
_cell_measurement_theta_min      25.07
_cell_volume                     851.7(3)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'CU k\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1343
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7374
_diffrn_reflns_theta_full        74.67
_diffrn_reflns_theta_max         74.67
_diffrn_reflns_theta_min         4.17
_diffrn_standards_decay_%        19
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'North A.C., Philips, D.C. & Mathews, F. (1968) Acta Cryst. A24, 350-359'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.02
_exptl_crystal_thermal_history
;
  First dipole-induced polymorph
;
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(6)
_refine_ls_extinction_coef       0.010(4)
_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   2.072
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1712
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      2.016
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.1112
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2984
_refine_ls_wR_factor_ref         0.3028
_reflns_number_gt                1554
_reflns_number_total             1712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0289447_s1_1.cif
_cod_data_source_block           bg0133o
_cod_depositor_comments
'Adding a tag to indicate that is the first of two polymorphs'
_cod_database_code               4113383