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_1560336
_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 H6 N O6 P2'
_chemical_formula_weight         247.72
_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                   5.2576(2)
_cell_length_b                   5.2576(2)
_cell_length_c                   12.9113(4)
_cell_measurement_reflns_used    2681
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.22
_cell_measurement_theta_min      2.91
_cell_volume                     309.083(19)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4617
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         34.990
_diffrn_reflns_theta_min         4.476
_exptl_absorpt_coefficient_mu    4.943
_exptl_absorpt_correction_T_max  908
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.662
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(10)
_refine_ls_extinction_coef       0.051(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         522
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.1567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.828
_reflns_Friedel_fraction_max     0.768
_reflns_number_gt                479
_reflns_number_total             522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NH4Ga.cif
_cod_data_source_block           2
_cod_original_cell_volume        309.08(3)
_cod_database_code               1560336
_shelxl_version_number           2014/6
_shelx_res_checksum              19889
_shelx_hkl_checksum              76577