Ab Initio Structure Determination of Vaterite by Automated Electron Diffraction
Mugnaioli, E.; Andrusenko, I.; Schüler, T.; Loges, N.; Panthöfer, M.; Dinnebier, R. E.; Tremel, W.; Kolb, U.; Angewandte Chemie International Edition 51 (2012) 7041–7045; doi:10.1002/anie.201200845

data_1508971
_publ_contact_author_address
;
Institut f\"ur Physikalische Chemie
Welderweg 11
Johannes Gutenberg Universit\"at
D-55099 Mainz, Germany
;
_publ_contact_author_email       kolb@uni-mainz.de
_publ_contact_author_name        'Dr. Ute Kolb'
_publ_contact_author_phone       49(6131)3924154
_publ_section_title
;
 Ab Initio Structure Determination of Vaterite by Automated Electron
 Diffraction
;
_journal_issue                   28
_journal_name_full               'Angewandte Chemie International Edition'
_journal_page_first              7041
_journal_page_last               7045
_journal_paper_doi               10.1002/anie.201200845
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C9 Ca9 O27'
_chemical_formula_weight         1334.24
_chemical_name_mineral           Vaterite
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1 (1/2*x+1/2*y,1/2*x-1/2*y,-z)'
_symmetry_space_group_name_H-M   'C -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_type_scat_source
'P.A. Doyle, P.S. Turner, Acta Crystallogr. A 1968, 24, 390-397'
_audit_creation_date             2012-01-04
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.22
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.170
_cell_length_b                   7.120
_cell_length_c                   25.320
_cell_measurement_temperature    295(2)
_cell_volume                     2165.643
_computing_cell_refinement       ADT3D
_computing_data_collection       'ADT module'
_computing_data_reduction        'own developed routines'
_computing_molecular_graphics    'Materials Studio'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir2008
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 '14-bit CCD GATAN 794MSC, 1024x1024 pixels'
_diffrn_measured_fraction_theta_full 0.599
_diffrn_measured_fraction_theta_max 0.599
_diffrn_measurement_device_type  'FEI Tecnai F30 ST'
_diffrn_radiation_monochromator  not
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electrons
_diffrn_radiation_wavelength     0.01970
_diffrn_reflns_av_R_equivalents  0.1633
_diffrn_reflns_av_sigmaI/netI    0.1536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            3001
_diffrn_reflns_theta_full        0.63
_diffrn_reflns_theta_max         0.63
_diffrn_reflns_theta_min         0.07
_exptl_absorpt_coefficient_mu    0.016
_exptl_crystal_density_diffrn    4.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nanocrystal
_exptl_crystal_F_000             1230
_exptl_crystal_size_mid          0.00004
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1876
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      4.857
_refine_ls_R_factor_all          0.4676
_refine_ls_R_factor_gt           0.4558
_refine_ls_shift/su_max          0.438
_refine_ls_shift/su_mean         0.134
_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          0.8028
_refine_ls_wR_factor_ref         0.8102
_reflns_number_gt                1421
_reflns_number_total             1876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CaCO3_vaterite_C_1_DC237.cif
_cod_data_source_block           vaterite3_good_clean_ref_cell
_cod_original_cell_volume        2165.6
_cod_original_sg_symbol_H-M      C-1
_cod_original_formula_sum        'C9 O27 Ca9'
_cod_database_code               1508971