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_2311812
_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 I2, 6.5H2 O'
_chemical_formula_moiety         'Ca 2+, 2(I -), 6.5(H2 O)'
_chemical_formula_sum            'Ca H13 I2 O6.5'
_chemical_formula_weight         200.99
_chemical_name_common            'calcium iodide 6.5 hydrate'
_chemical_name_systematic
;
Calcium iodide 6.5-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 111.045(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.466(3)
_cell_length_b                   8.2919(11)
_cell_length_c                   17.947(3)
_cell_measurement_reflns_used    4977
_cell_measurement_temperature    153.0(10)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.80
_cell_volume                     2286.9(7)
_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      153.0(10)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2626
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.432
_exptl_absorpt_coefficient_mu    5.930
_exptl_absorpt_correction_T_max  0.6980
_exptl_absorpt_correction_T_min  0.1360
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens, 1970)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.5395
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.0605
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.178
_refine_ls_extinction_coef       0.00069(7)
_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   1.111
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0397P)^2^+14.5175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                2329
_reflns_number_total             2603
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3039sup1.cif
_cod_data_source_block           CaI2_6H2O_153K
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'Ca1 H13 I2 O6.5'
_cod_database_code               2311812
_shelx_hkl_checksum              38813
_shelx_res_checksum              4597
_shelxl_version_number           2.013