Ionothermal synthesis and crystal structures of metal phosphate chains
Wragg, David S.; Le Ouay, Benjamin; Beale, Andrew M.; O-Brien, Matthew G.; Slawin, Alexandra M.Z.; Warren, John E.; Prior, Timothy J.; Morris, Russell E.; Journal of Solid State Chemistry 183 (2010) 1625–1631; doi:10.1016/j.jssc.2010.05.002

data_1563555
_publ_section_title
;
 Ionothermal synthesis and crystal structures of metal phosphate chains
;
_journal_issue                   7
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1625
_journal_page_last               1631
_journal_paper_doi               10.1016/j.jssc.2010.05.002
_journal_volume                  183
_journal_year                    2010
_chemical_formula_moiety         'Al H2 O8 P2, Al H O8 P2, 2(C6 H11 N2)'
_chemical_formula_sum            'C12 H25 Al2 N4 O16 P4'
_chemical_formula_weight         659.20
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                88.510(6)
_cell_angle_beta                 86.240(6)
_cell_angle_gamma                79.848(6)
_cell_formula_units_Z            2
_cell_length_a                   8.079(3)
_cell_length_b                   12.580(5)
_cell_length_c                   12.974(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1295.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'silicon (111)'
_diffrn_radiation_source         'SRS synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69390
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8801
_diffrn_reflns_theta_full        23.22
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.440
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+15.8028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2525
_reflns_number_gt                2584
_reflns_number_total             3968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-1625.cif
_cod_data_source_block           449
_cod_original_cell_volume        1294.9(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563555