Synthesis and Structure of Alkaline Earth Silicon Nitrides: BaSiN2, SrSiN2, and CaSiN2
Zoltán A. Gál; Phillip M. Mallinson; Heston J. Orchard; Simon J. Clarke; Inorganic Chemistry 43 (2004) 3998–4006; doi:10.1021/ic049901p

data_4311195
_publ_section_title
;
 Synthesis and Structure of Alkaline Earth Silicon Nitrides: BaSiN2,
 SrSiN2, and CaSiN2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3998
_journal_page_last               4006
_journal_paper_doi               10.1021/ic049901p
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Ba1 N2 Si1'
_chemical_formula_sum            'Ba N2 Si'
_chemical_formula_weight         193.45
_chemical_name_common            'Barium Silicon Nitride'
_chemical_name_systematic
;
 Barium Silicon Nitride
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-08-12T17:08:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.60460(10)
_cell_length_b                   11.3605(3)
_cell_length_c                   7.5851(2)
_cell_measurement_reflns_used    6003
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.319
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     482.95(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.120739
_diffrn_orient_matrix_UB_12      0.611E-4
_diffrn_orient_matrix_UB_13      -0.970673E-1
_diffrn_orient_matrix_UB_21      -0.131365
_diffrn_orient_matrix_UB_22      -0.6246E-3
_diffrn_orient_matrix_UB_23      0.892107E-1
_diffrn_orient_matrix_UB_31      -0.8485E-3
_diffrn_orient_matrix_UB_32      0.880221E-1
_diffrn_orient_matrix_UB_33      0.7004E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4121
_diffrn_reflns_theta_full        33.1
_diffrn_reflns_theta_max         33.1
_diffrn_reflns_theta_min         4.48
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    16.563
_exptl_absorpt_correction_T_max  0.6815
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        (see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    5.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       0.00129(13)
_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   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0138
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0282
_refine_ls_wR_factor_ref         0.0286
_reflns_number_gt                473
_reflns_number_total             503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049901psi20040126_125250_1.cif
_cod_data_source_block           BaSiN2
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_formula_sum        'Ba1 N2 Si1'
_cod_database_code               4311195
_exptl_absorpt_correction_t_ave  0.6021