Synthesis and characterization of two layered aluminophosphates [R-C8H12N]8[H2O]2·[Al8P12O48H4] and [S-C8H12N]8[H2O]2·[Al8P12O48H4] with mirror symmetric feature and their proton conductivity
Yu, Yue; Zhu, Jingran; liu, jiancong; Yan, Yan; Song, Xiaowei; Dalton Trans.  (2017) –; doi:10.1039/C7DT01643C

data_7043311
_publ_section_title
;
 Synthesis and characterization of two layered aluminophosphates
 [R-C8H12N]8[H2O]2&#x00B7;[Al8P12O48H4] and
 [S-C8H12N]8[H2O]2&#x00B7;[Al8P12O48H4] with mirror symmetric feature and
 their proton conductivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01643C
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_compound_source
'Aluminum triisopropoxide, Orthophosphoric acid, Water, (R)-\a-Methylbenzylamine'
_chemical_formula_moiety         '8(C8 H12 N1 1+), 2(H2O1), Al8 P12 O48 H4 8-'
_chemical_formula_sum            'C64 H104 Al8 N8 O50 P12'
_chemical_formula_weight         2373.03
_chemical_name_systematic        R-AlPO-CJ72
_chemical_temperature_decomposition 190
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-15 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.2040(10)
_cell_angle_beta                 90.9300(10)
_cell_angle_gamma                105.3390(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8831(5)
_cell_length_b                   15.9285(9)
_cell_length_c                   16.7042(9)
_cell_measurement_reflns_used    4015
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.42
_cell_volume                     2523.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.1203
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18675
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_correction_T_min  0.9264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1228
_exptl_crystal_recrystallization_method 'Solvothermal Synthesis'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         12391
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                8811
_reflns_number_total             12391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01643c2.cif
_cod_data_source_block           y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '190
decomposition'. The value '190 decomposition' was changed to '190'.

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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.

'_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_sg_symbol_H-M      P1
_cod_database_code               7043311