Examination of whewellite kidney stones by scanning electron microscopy and powder neutron diffraction techniques
Daudon, Michel; Bazin, Dominique; André, Gilles; Jungers, Paul; Cousson, Alain; Chevallier, Pierre; Véron, Emmanuel; Matzen, Guy; Journal of Applied Crystallography 42 (2009) 109–115; doi:10.1107/S0021889808041277

data_2300210
_publ_section_title
;
 Examination of whewellite kidney stones by scanning electron
 microscopy and powder neutron diffraction techniques
;
_journal_coeditor_code           FE5046
_journal_issue                   1
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              109
_journal_page_last               115
_journal_paper_doi               10.1107/S0021889808041277
_journal_volume                  42
_journal_year                    2009
_chemical_formula_moiety         'C2 H2 Ca O5'
_chemical_formula_sum            'C2 H2 Ca O5'
_chemical_formula_weight         146.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.0(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.316(5)
_cell_length_b                   14.541(3)
_cell_length_c                   10.116(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293
_cell_measurement_theta_max      45
_cell_measurement_theta_min      32
_cell_volume                     878.4(17)
_computing_cell_refinement       'DIF4 STOE MODIFIED VERSION'
_computing_data_collection       'DIF4 STOE MODIFIED VERSION'
_computing_data_reduction        'COLL5 LOCAL MODIFIED VERSION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Echigo et al. 2005'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Huber circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  copper
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           ' neutron '
_diffrn_radiation_wavelength     0.8302
_diffrn_reflns_av_R_equivalents  0.123
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4722
_diffrn_reflns_theta_full        42.549
_diffrn_reflns_theta_max         42.549
_diffrn_reflns_theta_min         2.988
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  450min
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.210
_exptl_crystal_description       'half pyramid'
_exptl_crystal_F_000             328
_exptl_crystal_size_max          6
_exptl_crystal_size_mid          5
_exptl_crystal_size_min          4
_refine_diff_density_max         1.21
_refine_diff_density_min         -4.99
_refine_ls_extinction_coef       112(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          4.249014
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 16.4 -24.1 18.8 -7.69 2.98
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0794
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                1729
_reflns_number_total             3933
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            fe5046.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H4 Ca2 O10'
_cod_original_formula_weight         292.23
_cod_original_formula_moiety         'C4 H4 Ca2 O10'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        878.2(18)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               2300210
_cod_database_fobs_code          2300210