A crystalline AlPO4-5 intermediate: designed synthesis, structure and phase transformation
Lin, Cong; Li, Jian; Pan, Fengjuan; Zhao, Yifang; Xu, Le; Yang, Yanquan; Du, Xin; Lin, Xiaohuan; Liao, Fuhui; Lin, Jianhua; Yang, Tao; Sun, Junliang; Dalton Trans.  (2017) –; doi:10.1039/C7DT02772A

data_7043997
_publ_section_title
;
 A crystalline AlPO4-5 intermediate: designed synthesis, structure and
 phase transformation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02772A
_journal_year                    2017
_chemical_formula_moiety         'Al3 O16 P4, 2(C7 H11 N2), H3 O'
_chemical_formula_sum            'C14 H25 Al3 N4 O17 P4'
_chemical_formula_weight         726.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-29 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.108(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9973(7)
_cell_length_b                   14.6074(11)
_cell_length_c                   21.2615(15)
_cell_measurement_reflns_used    2019
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      24.9830
_cell_measurement_theta_min      3.7760
_cell_volume                     2787.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3714
_diffrn_measured_fraction_theta_full 0.9874
_diffrn_measured_fraction_theta_max 0.9874
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.9874
_diffrn_reflns_Laue_measured_fraction_max 0.9874
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9162
_diffrn_reflns_point_group_measured_fraction_full 0.9874
_diffrn_reflns_point_group_measured_fraction_max 0.9874
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.0214
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+2.7715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3001
_reflns_number_total             4279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02772a2.cif
_cod_data_source_block           22
_cod_database_code               7043997
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              59847