A new high-pressure polymorph of phosphoric acid
Bull, Craig L.; Funnell, Nicholas P.; Pulham, Colin R.; Marshall, William G.; Allan, David R.; Acta Crystallographica Section B 73 (2017) 1068–1074; doi:10.1107/S205252061701441X

data_2108159
_publ_section_title
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 A new high-pressure polymorph of phosphoric acid
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_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1068
_journal_page_last               1074
_journal_paper_doi               10.1107/S205252061701441X
_journal_volume                  73
_journal_year                    2017
_chemical_compound_source        'Sigma Aldrich'
_chemical_formula_moiety         'H3 O4 P'
_chemical_formula_sum            'H3 O4 P'
_chemical_formula_weight         97.994
_chemical_melting_point          315.5
_chemical_name_common            'Phosphoric acid'
_chemical_name_systematic
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Phosphoric acid
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   4.619(5)
_cell_length_b                   8.479(17)
_cell_length_c                   14.38(3)
_cell_measurement_pressure       1.8
_cell_measurement_reflns_used    19
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.37
_cell_measurement_theta_min      4.84
_cell_volume                     563.2(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.479
_diffrn_measured_fraction_theta_max 0.479
_diffrn_measurement_device_type  'Nonius CAD4'
_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  0.1453
_diffrn_reflns_av_sigmaI/netI    0.1109
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            2503
_diffrn_reflns_theta_full        39.56
_diffrn_reflns_theta_max         39.56
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Diamond anvil cell absorption correction:
Absorb 6.0, R. J. Angel, J. Appl. Cryst., 2004, 37, 486-492
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.305
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1649
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.1219
_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^)+(0.0644P)^2^+10.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2702
_refine_ls_wR_factor_ref         0.3223
_reflns_number_gt                1296
_reflns_number_total             1649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            xk5045sup1.cif
_cod_data_source_block           Phosphoric_acid_II_1.8_GPa_S_Xtal
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '315.5 K' was changed to '315.5' -
the value should be numeric and without a unit designator.

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/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 
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_cod_original_cell_volume        563.0(18)
_cod_database_code               2108159