Mechanism of H2O Insertion and Chemical Bond Formation in AlPO4-54·xH2O at High Pressure.
Alabarse, Frederico G.; Rouquette, Jérôme; Coasne, Benoît; Haidoux, Abel; Paulmann, Carsten; Cambon, Olivier; Haines, Julien; Journal of the American Chemical Society 137 (2015) 584–587; doi:10.1021/ja511153n

data_4123228
_publ_section_title
;
 Mechanism of H2O Insertion and Chemical Bond Formation in
 AlPO4-54&#x00B7;xH2O at High Pressure.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              584
_journal_page_last               587
_journal_paper_doi               10.1021/ja511153n
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'Al18 O111 P18'
_chemical_formula_weight         2819.10
_chemical_name_common            AlPO4-54.xH2O
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   18.7342(9)
_cell_length_b                   18.7342(9)
_cell_length_c                   7.8979(3)
_cell_measurement_pressure       1200000
_cell_measurement_reflns_used    1357
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      3
_cell_measurement_theta_min      1
_cell_volume                     2400.56(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Absorb7 and Absorb-GUI, Angel and Gonzalez-Platas (2013)
  J. Appl. Cryst. 46:252-254
Average v2.2 (Angel, 2003) www.crystal.vt.edu/crystal 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_pressure         1200000
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.764
_diffrn_measured_fraction_theta_max 0.764
_diffrn_measurement_details
;
  1 phi     60.00  121.00   1.0000  700.0000
omega____ theta____ kappa____ phi______ frames
  57.0000    0.0000 -134.0000     -     61

  2 phi    240.00  301.00   1.0000  700.0000
omega____ theta____ kappa____ phi______ frames
  57.0000    0.0000 -134.0000     -     61

;
_diffrn_measurement_device_type
;
MARCCD 165 
MAR-CrysAlisPro-abstract goniometer: imported MAR images
;
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         'HASYLAB synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.50000
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_av_sigmaI/netI    0.1664
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5103
_diffrn_reflns_reduction_process
; 
data averaged using Blessing (1987) criteria 
;
_diffrn_reflns_theta_full        18.05
_diffrn_reflns_theta_max         18.05
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.633     0.966
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          1.000     1.000

    DAC transmission function via a table of values

    Gasket shadowing corrections were made based upon
    Gasket thickness = 118.1 microns, radius = 250.0 microns
    Gasket absorption coeff =        72.50 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.20

    Non-absorbing pressure medium
;
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
 crystal was described in terms of coordinates of corners
 now back-transformed to potentially non-integer hkl
;
_exptl_crystal_F_000             1392
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2461
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0915P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                1495
_reflns_number_total             2461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja511153n_si_005.cif
_cod_data_source_block           AlPO4-54
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4123227--4123231.cif.
;
_cod_database_code               4123228
_exptl_absorpt_correction_mu     0.310