Commensurately modulated 1/4 and 1/5 phases of deuterated betaine calcium chloride dihydrate: a neutron structural study
Hernandez, Olivier; Kiat, Jean-Michel; Cousson, Alain; Paulus, Werner; Ezpeleta, Jose Maria; Zuniga, Francisco Javier; Acta Crystallographica Section C 55 (1999) 1463–1466; doi:10.1107/S0108270198017508

data_2008886
_publ_section_title
;
 Commensurately modulated 1/4 and 1/5 phases of deuterated betaine
 calcium chloride dihydrate: a neutron structural study
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1463
_journal_page_last               1466
_journal_paper_doi               10.1107/S0108270198017508
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'Ca Cl2, C5 D11 N O2, 2D2 O'
_chemical_formula_sum            'C5 Ca Cl2 D15 N O4'
_chemical_formula_weight         279.0
_chemical_name_common            D-BCCD
_chemical_name_systematic
;
Deuterated Betaine Calcium Chloride Dihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            20
_cell_length_a                   10.82(3)
_cell_length_b                   9.98(2)
_cell_length_c                   53.93(2)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    68.0
_cell_measurement_theta_max      21.36
_cell_measurement_theta_min      14.77
_cell_volume                     5824(2)
_computing_data_reduction        'COLL5 (Lehmann & Larsen, 1974)'
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1994)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement
'CRYSTALS (Watkin, Prout, Carruthers & Betteridge, 1996)'
_diffrn_measurement_device
'Orph\'ee reactor (Saclay, France), 6T2 four-circle'
_diffrn_measurement_method
;
\w scans between 2\q = 0 and 45\%, \w-\q scans between 2\q = 45 and 80\%
and \w-2\q scans between 2\q = 80 and 120\%
;
_diffrn_radiation_monochromator  pyrolytic_graphite_(0_0_2)
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         Orph\'ee_reactor_Saclay_France
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     1.528
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7098
_diffrn_reflns_theta_max         52.17
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        <1.4
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.0915
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3794.43
_exptl_crystal_size_max          7.5
_exptl_crystal_size_mid          4.5
_exptl_crystal_size_min          3.5
_refine_diff_density_max         1.89
_refine_diff_density_min         -2.00
_refine_ls_extinction_coef       134(7)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.03
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         2336
_refine_ls_R_factor_obs          0.123
_refine_ls_shift/su_max          0.07
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
'Chebyshev weighting scheme: parameters 1.77, 1.38 and 0.331'
_refine_ls_wR_factor_obs         0.154
_reflns_number_observed          2336
_reflns_number_total             2456
_reflns_observed_criterion       F^2^>3\s(F^2^)
_cod_data_source_file            fg1472.cif
_cod_data_source_block           2
_cod_original_cell_volume        582E1(2)
_cod_original_formula_sum        'C5 Ca1 Cl2 D15 N1 O4'
_cod_database_code               2008886
_cod_depositor_comments
;
 Changing the _atom_site_label data item values to match the ones in
 related data items (e. g. _atom_site_aniso_label) and correcting typos
 in the _geom_angle_atom_site_label_* data item values.

 Antanas Vaitkus,
 2017-01-05
;