Crystal structures of hydrates of simple inorganic salts. II. Water-rich calcium bromide and iodide hydrates: CaBr2 · 9H2O, CaI2 · 8H2O, CaI2 · 7H2O and CaI2 · 6.5H2O.
Hennings, Erik; Schmidt, Horst; Voigt, Wolfgang; Acta crystallographica. Section C, Structural chemistry 70 (2014) 876–881; doi:10.1107/S2053229614018002

data_2311809
_publ_section_title
;
 Crystal structures of hydrates of simple inorganic salts. II. Water-rich
 calcium bromide and iodide hydrates: CaBr2 &#x00B7; 9H2O, CaI2 &#x00B7;
 8H2O, CaI2 &#x00B7; 7H2O and CaI2 &#x00B7; 6.5H2O.
;
_journal_coeditor_code           QS3039
_journal_issue                   'Pt 9'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              876
_journal_page_last               881
_journal_paper_doi               10.1107/S2053229614018002
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Ca Br2, 9H2 O'
_chemical_formula_moiety         'Ca 2+. 2(Br -), 9(H2 O)'
_chemical_formula_sum            'Br2 Ca H18 O9'
_chemical_formula_weight         362.02
_chemical_name_common            'calcium bromide nonahydrate'
_chemical_name_systematic
;
Calcium bromide nonahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 101.041(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8354(8)
_cell_length_b                   8.7538(5)
_cell_length_c                   18.2615(18)
_cell_measurement_reflns_used    2310
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.25
_cell_volume                     1229.36(19)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2009)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2009)'
_computing_molecular_graphics    'SHELXL2012 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3495
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.247
_diffrn_reflns_theta_min         2.589
_exptl_absorpt_coefficient_mu    7.026
_exptl_absorpt_correction_T_max  0.2967
_exptl_absorpt_correction_T_min  0.0814
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens, 1970)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.267
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.450
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2012 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.2235P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                2968
_reflns_number_total             3495
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3039sup1.cif
_cod_data_source_block           CaBr2_9H2O_100K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2311809
_shelx_hkl_checksum              50533
_shelx_res_checksum              43317
_shelxl_version_number           .000002012