Synthesis, characterization and properties of a glycol-coordinated ε-Keggin-type Al13 chloride
Gu, Bin; Sun, Chenlin; Fettinger, James C.; Casey, William H.; Dikhtiarenko, Alla; Gascon, Jorge; Koichumanova, Kamila; Babu, Karthick; Heeres, Erik; He, Songbo; Chemical Communications  (2018) –; doi:10.1039/C8CC01363B

data_7121464
_publ_section_title
;
 Synthesis, characterization and properties of a glycol-coordinated
 \e-Keggin-type Al13 chloride
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC01363B
_journal_year                    2018
_chemical_formula_moiety         'C24 H72 Al13 O40, 7(Cl), H2O, [+ solvent]'
_chemical_formula_sum            'C24 H74 Al13 Cl7 O41'
_chemical_formula_weight         1617.72
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6762(11)
_cell_length_b                   24.6762(11)
_cell_length_c                   24.6762(11)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.33
_cell_volume                     15025.7(12)
_computing_cell_refinement       'SAINT (8.37a) (Bruker, 2016)'
_computing_data_collection       'Apex3 (2017.3) (Bruker, 2017)'
_computing_data_reduction        'SAINT (8.37a) (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0059
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.334
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.9148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       Cube
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00028(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         874
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0569
_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^)+(0.1014P)^2^+100.6762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                822
_reflns_number_total             874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01363b2.cif
_cod_data_source_block           JF2690FMI_SQ
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        15026(2)
_cod_database_code               7121464
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              24157
_shelx_fab_checksum              55770