Hydrothermal synthesis, structural and thermal characterizations of three open-framework gallium phosphites
Hamchaoui, Farida; Alonzo, Véronique; Marlart, Isabelle; Auguste, Sandy; Galven, Cyrille; Rebbah, Houria; Le Fur, Eric; Journal of Solid State Chemistry 255 (2017) 8–12; doi:10.1016/j.jssc.2017.07.030

data_1560335
_publ_section_title
;
 Hydrothermal synthesis, structural and thermal characterizations of three
 open-framework gallium phosphites
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              8
_journal_page_last               12
_journal_paper_doi               10.1016/j.jssc.2017.07.030
_journal_volume                  255
_journal_year                    2017
_chemical_formula_sum            'Ga H2 K O6 P2'
_chemical_formula_weight         268.78
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   5.2567(2)
_cell_length_b                   5.2567(2)
_cell_length_c                   12.2582(3)
_cell_measurement_reflns_used    7302
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.11
_cell_measurement_theta_min      2.91
_cell_volume                     293.348(17)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6120
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         41.878
_diffrn_reflns_theta_min         4.477
_exptl_absorpt_coefficient_mu    5.908
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.043
_exptl_crystal_description       block
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 256 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.800
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         745
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0241P)^2^+0.6653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.778
_reflns_number_gt                644
_reflns_number_total             745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            KGa.cif
_cod_data_source_block           1
_cod_original_cell_volume        293.35(2)
_cod_database_code               1560335
_shelxl_version_number           2014/6
_shelx_res_checksum              949
_shelx_hkl_checksum              73304