Water channel structure of bassanite at high air humidity: crystal structure of CaSO~4~·0.625H~2~O
Schmidt, Horst; Paschke, Iris; Freyer, Daniela; Voigt, Wolfgang; Acta Crystallographica Section B 67 (2011) 467–475; doi:10.1107/S0108768111041759

data_2105042
_publ_section_title
;
 Water channel structure of bassanite at high air humidity: crystal
 structure of CaSO~4~&#x00B7;0.625H~2~O
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              467
_journal_page_last               475
_journal_paper_doi               10.1107/S0108768111041759
_journal_volume                  67
_journal_year                    2011
_chemical_compound_source        Synthetic
_chemical_formula_sum            'Ca H O4.5 S'
_chemical_formula_weight         145.16
_chemical_name_mineral           Bassanite
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.655(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   17.5180(8)
_cell_length_b                   6.92910(10)
_cell_length_c                   12.0344(2)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1
_cell_volume                     1056.89(9)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    'Diamond 3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_database_code_amcsd             0019833
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker X8 Kappa. Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15532
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.254
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.489
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.00034(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         15543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                12774
_reflns_number_total             15543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn5106.cif
_cod_data_source_block           caso4_05
_cod_original_cell_volume        1056.88(4)
_cod_original_formula_sum        'Ca O4.5 S H'
_cod_database_code               2105042