Phase Selection and Energetics in Chiral Alkaline Earth Tartrates and Their Racemic and Meso Analogues: Synthetic, Structural, Computational, and Calorimetric Studies
Leah N. Appelhans; Monica Kosa; A. V. Radha; Petra Simoncic; Alexandra Navrotsky; Michele Parrinello; Anthony K. Cheetham; Journal of the American Chemical Society 131 (2009) 15375–15386; doi:10.1021/ja905690t

data_4105178
_publ_contact_author_address
;
Department of Materials Science and Metallurgy
University of Cambridge
Cambridge CB2 3QZ, UK
;
_publ_contact_author_email       akc30@cam.ac.uk
_publ_contact_author_name        'Anthony K. Cheetham'
_publ_contact_author_phone       '+44 01223-767061'
_publ_section_title
;
 Phase Selection and Energetics in Chiral Alkaline Earth Tartrates and
 Their Racemic and Meso Analogues: Synthetic, Structural, Computational,
 and Calorimetric Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15375
_journal_page_last               15386
_journal_paper_doi               10.1021/ja905690t
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C4 H4 Ca O6'
_chemical_formula_weight         188.15
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 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                   7.6418(10)
_cell_length_b                   9.9656(13)
_cell_length_c                   7.2395(9)
_cell_measurement_temperature    298(2)
_cell_volume                     551.33(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2301
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 232 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         605
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0908P)^2^+0.2925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                584
_reflns_number_total             605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905690t_si_002_05.cif
_cod_data_source_block           catartm
_cod_database_code               4105178