Crystallization of aluminum polycation sulfates: transformation of tetrahedral crystals into block crystals in aqueous solutions
An, Guangyu; Jiang, Yuqian; Xi, Jinyang; Liu, Libing; Wang, Pin; Xiao, Feng; Wang, Dongsheng; CrystEngComm 21 (2019) 202–; doi:10.1039/C8CE01571F

data_7231864
_publ_section_title
;
 Crystallization of aluminum polycation sulfates: transformation of
 tetrahedral crystals into block crystals in aqueous solutions
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              202
_journal_paper_doi               10.1039/C8CE01571F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'Al13 H53 O67 S3'
_chemical_formula_weight         1572.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-10-31 deposited with the CCDC.
2018-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.030(3)
_cell_length_b                   11.502(2)
_cell_length_c                   17.598(4)
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.7706
_cell_volume                     2775.9(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Rigaku
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_unetI/netI     0.1610
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18655
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.368
_exptl_absorpt_coefficient_mu    0.489
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details
;
 Flack x determined using 1745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         9261
_refine_ls_number_restraints     953
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.1270
_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^)+(0.0812P)^2^+39.9276P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2529
_refine_ls_wR_factor_ref         0.2845
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.875
_reflns_Friedel_fraction_max     0.901
_reflns_number_gt                6959
_reflns_number_total             9261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01571f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7231864--7231865.cif.'
_cod_original_cell_volume        2775.8(10)
_cod_original_formula_sum        'H53 Al13 O67 S3'
_cod_database_code               7231864
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-2
_shelx_res_checksum              38748