High-Pressure Synthesis, Electron Energy-Loss Spectroscopy Investigations, and Single Crystal Structure Determination of a Spinel-Type Gallium Oxonitride Ga2.79◻0.21(O3.05N0.76◻0.19)
Huppertz, Hubert; Hering, Stefanie A.; Zvoriste, Carmen E.; Lauterbach, Stefan; Oeckler, Oliver; Riedel, Ralf; Kinski, Isabel; Chemistry of Materials 21 (2009) 2101–; doi:10.1021/cm803371k

data_4001005
_publ_section_title
;
 High-Pressure Synthesis, Electron Energy-Loss Spectroscopy
 Investigations, and Single Crystal Structure Determination of a
 Spinel-Type Gallium Oxonitride Ga2.79&#x25FB;0.21(O3.05N0.76&#x25FB;0.19)
;
_journal_issue                   10
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2101
_journal_paper_doi               10.1021/cm803371k
_journal_volume                  21
_journal_year                    2009
_chemical_formula_sum            'Ga2.79 N0.76 O3.05'
_chemical_formula_weight         254.00
_chemical_name_common            Spinel-gallium-oxonitride
_chemical_name_systematic
; 
 Gallium-oxonitride 
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'July 08, 2008'
_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                   8.2783(10)
_cell_length_b                   8.2783(10)
_cell_length_c                   8.2783(10)
_cell_measurement_reflns_used    719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      3.134
_cell_volume                     567.31(12)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0012425
_diffrn_orient_matrix_UB_12      0.1177348
_diffrn_orient_matrix_UB_13      0.0270014
_diffrn_orient_matrix_UB_21      -0.0792122
_diffrn_orient_matrix_UB_22      -0.0211801
_diffrn_orient_matrix_UB_23      0.0887070
_diffrn_orient_matrix_UB_31      0.0911920
_diffrn_orient_matrix_UB_32      -0.0167935
_diffrn_orient_matrix_UB_33      0.0774215
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  'vertically mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            171
_diffrn_reflns_theta_full        32.31
_diffrn_reflns_theta_max         32.31
_diffrn_reflns_theta_min         4.26
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    26.127
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10
_refine_ls_number_reflns         69
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                62
_reflns_number_total             69
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm803371k_si_001.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      FD-3M
_cod_database_code               4001005
_kl_diffrn_measurement_scan_angle omega-scan
_kl_diffrn_measurement_scan_step_degree 2.0
_kl_diffrn_measurement_scan_time_per_degree 110
_kl_diffrn_measurement_detector_distance 40