High-Pressure Synthesis and Characterization of Li2Ca3[N2]3 - An Uncommon Metallic Diazenide with [N2]2- Ions
Sebastian B. Schneider; Markus Seibald; Volker L. Deringer; Ralf P. Stoffel; Rainer Frankovsky; Gina M. Friederichs; Henryk Laqua; Viola Duppel; Gunnar Jeschke; Richard Dronskowski; Wolfgang Schnick; Journal of the American Chemical Society 135 (2013) 16668–16679; doi:10.1021/ja408816t

data_4121091
_publ_contact_author
;
 Prof. Dr. Wolfgang Schnick
 Department Chemie
 Ludwig-Maximilians-Universit\"at M\"unchen
 Butenandtstr. 5-13 (D)
 D-81377 Munich, Germany
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_publ_contact_author_email       wolfgang.schnick@uni-muenchen.de
_publ_contact_author_fax         +49/89/2180-77440
_publ_contact_author_phone       +49/89/2180-77436
_publ_section_title
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 High-Pressure Synthesis and Characterization of Li2Ca3[N2]3 - An Uncommon
 Metallic Diazenide with [N2]2- Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16668
_journal_page_last               16679
_journal_paper_doi               10.1021/ja408816t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '(Ca 2+)3 (N2 2-)3 (Li +)2'
_chemical_formula_sum            'Ca3 Li2 N6'
_chemical_formula_weight         218.16
_chemical_name_common            'Lithium calcium diazenide'
_chemical_name_systematic
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Lithium pernitride 
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      51
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_audit_creation_method           'TOPAS ACADEMIC 4.1 + PLATON'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   4.77472(7)
_cell_length_b                   13.9792(4)
_cell_length_c                   8.0718(4)
_cell_measurement_temperature    298
_cell_volume                     538.77(3)
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  'TOPAS ACADEMIC 4.1'
_computing_structure_refinement  'TOPAS ACADEMIC 4.1'
_computing_structure_solution    'TOPAS ACADEMIC 4.1'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device_type  'STOE Stadi P'
_diffrn_radiation_monochromator  Ge-111
_diffrn_radiation_polarisn_ratio 0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a1'
_diffrn_radiation_wavelength     1.540596
_exptl_absorpt_coefficient_mu    26.09
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   '(A. Cohelo, TOPAS_Academic, Version 4.1)'
_exptl_crystal_density_diffrn    2.690(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_F_000             432
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  gold
_pd_char_particle_morphology     powder
_pd_meas_number_of_points        9000
_pd_proc_ls_prof_R_factor        0.06168
_pd_proc_ls_prof_wR_factor       0.08109
_pd_proc_number_of_points        9000
_refine_ls_goodness_of_fit_all   1.644
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     65
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.03787
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        8.07183
_reflns_d_resolution_low         1.00329
_reflns_limit_h_max              4
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_total             345
_cod_data_source_file            ja408816t_si_002.cif
_cod_data_source_block           Li2Ca3N6
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4121091
_solution_special_details
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A structure solution was performed with the TOPAS package 
using the charge-flipping algorithm and difference fourier
syntheses. A first indexing resulted in a hexagonal unit-cell metrics 
with a = 8.06 and c = 4.76 \%A. With the use of electron diffraction 
methods, symmetry-reduction as well as density-functional theory, 
an orthorhombic unit cell in space group Pmma (no. 51)
was derived with a = 4.76, b = 13.96 and c = 8.06 \%A. Subsequently, 
the powder x-ray pattern was refined with as-obtained parameters
and supported the theoretical model. Further elemental analysis in
accordance with the Roetveld refinment and theoretical stability 
calculations finally resulted in Li2Ca3(N2)3.
;
_pd_proc_ls_prof_r_expected      0.04932