Nitridogermanate Nitrides Sr7[GeN4]N2 and Ca7[GeN4]N2: Synthesis Employing Sodium Melts, Crystal Structure, and Density-Functional Theory Calculations
Sebastian C. Junggeburth; Oliver Oeckler; Dirk Johrendt; Wolfgang Schnick; Inorganic Chemistry 47 (2008) 12018–12023; doi:10.1021/ic801562c

data_4306749
_publ_contact_author_address
;
  Department Chemie und Biochemie
  Ludwig-Maximilians-Universit\"at
  Butenandtstr. 5-13 (Haus D)
  81377 Muenchen, Germany
;
_publ_contact_author_email       wolfgang.schnick@cup.uni-muenchen.de
_publ_contact_author_fax
;
+49/89/2180-77440
;
_publ_contact_author_name
;
  Prof. Dr. W. Schnick
;
_publ_contact_author_phone
;
+49/89/2180-77421
;
_publ_section_title
;
Nitridogermanate Nitrides Sr7[GeN4]N2 and Ca7[GeN4]N2: Synthesis Employing
Sodium Melts, Crystal Structure, and Density-Functional Theory Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12018
_journal_page_last               12023
_journal_paper_doi               10.1021/ic801562c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'Ca7 Ge N6'
_chemical_formula_weight         437.21
_chemical_name_common
;           
Calcium nitridogermanat nitride
;
_chemical_name_systematic
;
Heptastrontium germanium hexanitride
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-01-14 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.826(2)
_cell_length_b                   6.1940(12)
_cell_length_c                   13.121(3)
_cell_measurement_reflns_used    11075
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     879.8(3)
_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    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_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       'omega scan'
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  'graded multilayer x-ray optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15719
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.63
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_voltage           55.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.514
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'from equivalents'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00166(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0135
_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^)+(0.0000P)^2^+1.2570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0293
_refine_ls_wR_factor_ref         0.0304
_reflns_number_gt                935
_reflns_number_total             1012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801562c_si_001_2.cif
_cod_data_source_block           ca7gen6sad
_cod_database_code               4306749