# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004


data_global
_journal_coden_Cambridge         182

#------------------ SUBMISSION DETAILS --------------------------------------#

_publ_contact_author             
;
Dr Duncan H. Gregory
School of Chemistry
University of Nottingham
University Park
Nottingham  NG7 2RD.
;

_publ_contact_author_email       Duncan.Gregory@nottingham.ac.uk
_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Crystal growth, defect structure and magnetism
of new Li3N-derived lithium nitridocobaltates.
;
loop_
_publ_author_name
_publ_author_address
'Gordon, Alexandra G.'
; School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England
;
'Smith, Ron I.'
; School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England
;
'Wilson, Claire'
; School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England
;
'Gregory, Duncan H.'
; School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_colin1
_database_code_depnum_ccdc_archive 'CCDC 249196'

_audit_creation_date             2004-02-18T17:45:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_name_common            'Lithium Cobalt Nitride'
_chemical_formula_moiety         'Co0.53 Li1.99 N'
_chemical_formula_sum            'Co0.53 Li1.99 N'
_chemical_formula_weight         59.46
_chemical_compound_source        'synthesis as described'
#------------------ UNIT CELL INFORMATION -----------------------------------#

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6/mmm

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z'
'y, -x+y, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z'
'-y, x-y, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, z'

_cell_length_a                   3.7343(13)
_cell_length_b                   3.7343(13)
_cell_length_c                   3.607(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     43.56(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    126
_cell_measurement_theta_min      5.65
_cell_measurement_theta_max      24.15
_cell_measurement_wavelength     0.71073

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            metallic
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             27
_exptl_absorpt_coefficient_mu    4.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_process_details   SADABS

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            205
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         5.65
_diffrn_reflns_theta_max         26.82
_reflns_number_total             35
_reflns_number_gt                35
_reflns_threshold_expression     >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ATOMS 4.1 (Dowty, 1998)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_number_reflns         35
_refine_ls_number_parameters     9
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_restrained_S_all      1.239
_refine_ls_shift/su_max          0

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Co1 Co 0 0 0.5 0.0176(8) Uani 0.53(2) d SP . .
Li1 Li 0 0 0.5 0.0176(8) Uani 0.47(2) d SP . .
N2 N 0 0 0 0.018(2) Uani 1 d S . .
Li2 Li 0.3333 0.6667 0 0.055(8) Uani 0.76(9) d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0211(9) 0.0211(9) 0.0105(10) 0 0 0.0106(4)
Li1 0.0211(9) 0.0211(9) 0.0105(10) 0 0 0.0106(4)
N2 0.017(3) 0.017(3) 0.020(4) 0 0 0.0083(13)
Li2 0.036(7) 0.036(7) 0.091(18) 0 0 0.018(4)

#------------------ MOLECULAR GEOMETRY --------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N2 1.8035(10) 1_556 ?
Co1 N2 1.8035(10) . ?
Co1 Li2 2.8109(9) 13_666 ?
Co1 Li2 2.8109(9) 13 ?
Co1 Li2 2.8109(9) 1_445 ?
Co1 Li2 2.8109(9) 1_556 ?
Co1 Li2 2.8109(9) 13_566 ?
Co1 Li2 2.8109(9) 1_546 ?
Co1 Li2 2.8109(9) 13_565 ?
Co1 Li2 2.8109(9) 1_545 ?
Co1 Li2 2.8109(9) . ?
Co1 Li2 2.8109(9) 13_665 ?
N2 Li1 1.8035(10) 1_554 ?
N2 Co1 1.8035(10) 1_554 ?
N2 Li2 2.1560(8) 13_565 ?
N2 Li2 2.1560(8) 1_545 ?
N2 Li2 2.1560(8) 13_665 ?
N2 Li2 2.1560(8) 1_445 ?
N2 Li2 2.1560(8) 13 ?
N2 Li2 2.1560(8) . ?
Li2 Li2 2.1560(8) 13_675 ?
Li2 Li2 2.1560(7) 13_565 ?
Li2 N2 2.1560(7) 1_565 ?
Li2 N2 2.1560(7) 1_665 ?
Li2 Li2 2.1560(8) 13_665 ?
Li2 Co1 2.8109(9) 1_554 ?
Li2 Li1 2.8109(9) 1_665 ?
Li2 Co1 2.8109(9) 1_665 ?
Li2 Li1 2.8109(9) 1_554 ?
Li2 Co1 2.8109(9) 1_565 ?
Li2 Co1 2.8109(9) 1_564 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Co1 N2 180 1_556 . ?
N2 Co1 Li2 50.087(18) 1_556 13_666 ?
N2 Co1 Li2 129.913(18) . 13_666 ?
N2 Co1 Li2 129.913(18) 1_556 13 ?
N2 Co1 Li2 50.087(18) . 13 ?
Li2 Co1 Li2 134.897(13) 13_666 13 ?
N2 Co1 Li2 129.913(18) 1_556 1_445 ?
N2 Co1 Li2 50.087(18) . 1_445 ?
Li2 Co1 Li2 180 13_666 1_445 ?
Li2 Co1 Li2 45.103(13) 13 1_445 ?
N2 Co1 Li2 50.087(18) 1_556 1_556 ?
N2 Co1 Li2 129.913(18) . 1_556 ?
Li2 Co1 Li2 45.103(13) 13_666 1_556 ?
Li2 Co1 Li2 180 13 1_556 ?
Li2 Co1 Li2 134.897(13) 1_445 1_556 ?
N2 Co1 Li2 50.087(18) 1_556 13_566 ?
N2 Co1 Li2 129.913(19) . 13_566 ?
Li2 Co1 Li2 83.25(3) 13_666 13_566 ?
Li2 Co1 Li2 134.897(13) 13 13_566 ?
Li2 Co1 Li2 96.75(3) 1_445 13_566 ?
Li2 Co1 Li2 45.103(13) 1_556 13_566 ?
N2 Co1 Li2 50.087(18) 1_556 1_546 ?
N2 Co1 Li2 129.913(19) . 1_546 ?
Li2 Co1 Li2 45.103(13) 13_666 1_546 ?
Li2 Co1 Li2 96.75(3) 13 1_546 ?
Li2 Co1 Li2 134.897(13) 1_445 1_546 ?
Li2 Co1 Li2 83.25(3) 1_556 1_546 ?
Li2 Co1 Li2 100.17(4) 13_566 1_546 ?
N2 Co1 Li2 129.913(19) 1_556 13_565 ?
N2 Co1 Li2 50.087(18) . 13_565 ?
Li2 Co1 Li2 134.897(13) 13_666 13_565 ?
Li2 Co1 Li2 83.25(3) 13 13_565 ?
Li2 Co1 Li2 45.103(13) 1_445 13_565 ?
Li2 Co1 Li2 96.75(3) 1_556 13_565 ?
Li2 Co1 Li2 79.83(4) 13_566 13_565 ?
Li2 Co1 Li2 180 1_546 13_565 ?
N2 Co1 Li2 129.913(19) 1_556 1_545 ?
N2 Co1 Li2 50.087(18) . 1_545 ?
Li2 Co1 Li2 96.75(3) 13_666 1_545 ?
Li2 Co1 Li2 45.103(13) 13 1_545 ?
Li2 Co1 Li2 83.25(3) 1_445 1_545 ?
Li2 Co1 Li2 134.897(13) 1_556 1_545 ?
Li2 Co1 Li2 180 13_566 1_545 ?
Li2 Co1 Li2 79.83(4) 1_546 1_545 ?
Li2 Co1 Li2 100.17(4) 13_565 1_545 ?
N2 Co1 Li2 129.913(18) 1_556 . ?
N2 Co1 Li2 50.087(18) . . ?
Li2 Co1 Li2 96.75(3) 13_666 . ?
Li2 Co1 Li2 100.17(4) 13 . ?
Li2 Co1 Li2 83.25(3) 1_445 . ?
Li2 Co1 Li2 79.83(4) 1_556 . ?
Li2 Co1 Li2 96.75(3) 13_566 . ?
Li2 Co1 Li2 134.897(13) 1_546 . ?
Li2 Co1 Li2 45.103(13) 13_565 . ?
Li2 Co1 Li2 83.25(3) 1_545 . ?
N2 Co1 Li2 129.913(18) 1_556 13_665 ?
N2 Co1 Li2 50.087(18) . 13_665 ?
Li2 Co1 Li2 79.83(4) 13_666 13_665 ?
Li2 Co1 Li2 83.25(3) 13 13_665 ?
Li2 Co1 Li2 100.17(4) 1_445 13_665 ?
Li2 Co1 Li2 96.75(3) 1_556 13_665 ?
Li2 Co1 Li2 134.897(13) 13_566 13_665 ?
Li2 Co1 Li2 96.75(3) 1_546 13_665 ?
Li2 Co1 Li2 83.25(3) 13_565 13_665 ?
Li2 Co1 Li2 45.103(13) 1_545 13_665 ?
Li2 Co1 Li2 45.103(13) . 13_665 ?
Co1 N2 Co1 180 . 1_554 ?
Li1 N2 Li2 90 1_554 13_565 ?
Co1 N2 Li2 90 . 13_565 ?
Co1 N2 Li2 90 1_554 13_565 ?
Li1 N2 Li2 90 1_554 1_545 ?
Co1 N2 Li2 90 . 1_545 ?
Co1 N2 Li2 90 1_554 1_545 ?
Li2 N2 Li2 180 13_565 1_545 ?
Li1 N2 Li2 90 1_554 13_665 ?
Co1 N2 Li2 90 . 13_665 ?
Co1 N2 Li2 90 1_554 13_665 ?
Li2 N2 Li2 120 13_565 13_665 ?
Li2 N2 Li2 60 1_545 13_665 ?
Li1 N2 Li2 90 1_554 1_445 ?
Co1 N2 Li2 90 . 1_445 ?
Co1 N2 Li2 90 1_554 1_445 ?
Li2 N2 Li2 60 13_565 1_445 ?
Li2 N2 Li2 120 1_545 1_445 ?
Li2 N2 Li2 180 13_665 1_445 ?
Li1 N2 Li2 90 1_554 13 ?
Co1 N2 Li2 90 . 13 ?
Co1 N2 Li2 90 1_554 13 ?
Li2 N2 Li2 120 13_565 13 ?
Li2 N2 Li2 60 1_545 13 ?
Li2 N2 Li2 120 13_665 13 ?
Li2 N2 Li2 60 1_445 13 ?
Li1 N2 Li2 90 1_554 . ?
Co1 N2 Li2 90 . . ?
Co1 N2 Li2 90 1_554 . ?
Li2 N2 Li2 60 13_565 . ?
Li2 N2 Li2 120 1_545 . ?
Li2 N2 Li2 60 13_665 . ?
Li2 N2 Li2 120 1_445 . ?
Li2 N2 Li2 180 13 . ?
Li2 Li2 Li2 120 13_675 13_565 ?
Li2 Li2 N2 60 13_675 1_565 ?
Li2 Li2 N2 60 13_565 1_565 ?
Li2 Li2 N2 60 13_675 1_665 ?
Li2 Li2 N2 180 13_565 1_665 ?
N2 Li2 N2 120 1_565 1_665 ?
Li2 Li2 N2 180 13_675 . ?
Li2 Li2 N2 60 13_565 . ?
N2 Li2 N2 120 1_565 . ?
N2 Li2 N2 120 1_665 . ?
Li2 Li2 Li2 120 13_675 13_665 ?
Li2 Li2 Li2 120 13_565 13_665 ?
N2 Li2 Li2 180 1_565 13_665 ?
N2 Li2 Li2 60 1_665 13_665 ?
N2 Li2 Li2 60 . 13_665 ?
Li2 Li2 Co1 140.087(18) 13_675 1_554 ?
Li2 Li2 Co1 67.449(6) 13_565 1_554 ?
N2 Li2 Co1 112.551(6) 1_565 1_554 ?
N2 Li2 Co1 112.551(6) 1_665 1_554 ?
N2 Li2 Co1 39.913(18) . 1_554 ?
Li2 Li2 Co1 67.449(6) 13_665 1_554 ?
Li2 Li2 Li1 67.449(6) 13_675 1_665 ?
Li2 Li2 Li1 140.087(18) 13_565 1_665 ?
N2 Li2 Li1 112.551(6) 1_565 1_665 ?
N2 Li2 Li1 39.913(18) 1_665 1_665 ?
N2 Li2 Li1 112.551(6) . 1_665 ?
Li2 Li2 Li1 67.449(6) 13_665 1_665 ?
Co1 Li2 Li1 134.897(13) 1_554 1_665 ?
Li2 Li2 Co1 67.449(6) 13_675 1_665 ?
Li2 Li2 Co1 140.087(18) 13_565 1_665 ?
N2 Li2 Co1 112.551(6) 1_565 1_665 ?
N2 Li2 Co1 39.913(18) 1_665 1_665 ?
N2 Li2 Co1 112.551(6) . 1_665 ?
Li2 Li2 Co1 67.449(6) 13_665 1_665 ?
Co1 Li2 Co1 134.897(13) 1_554 1_665 ?
Li1 Li2 Co1 0 1_665 1_665 ?
Li2 Li2 Li1 140.087(18) 13_675 1_554 ?
Li2 Li2 Li1 67.449(6) 13_565 1_554 ?
N2 Li2 Li1 112.551(6) 1_565 1_554 ?
N2 Li2 Li1 112.551(6) 1_665 1_554 ?
N2 Li2 Li1 39.913(18) . 1_554 ?
Li2 Li2 Li1 67.449(6) 13_665 1_554 ?
Co1 Li2 Li1 0 1_554 1_554 ?
Li1 Li2 Li1 134.897(13) 1_665 1_554 ?
Co1 Li2 Li1 134.897(13) 1_665 1_554 ?
Li2 Li2 Co1 67.449(6) 13_675 1_565 ?
Li2 Li2 Co1 67.449(6) 13_565 1_565 ?
N2 Li2 Co1 39.913(18) 1_565 1_565 ?
N2 Li2 Co1 112.551(6) 1_665 1_565 ?
N2 Li2 Co1 112.551(6) . 1_565 ?
Li2 Li2 Co1 140.087(18) 13_665 1_565 ?
Co1 Li2 Co1 134.897(13) 1_554 1_565 ?
Li1 Li2 Co1 83.25(3) 1_665 1_565 ?
Co1 Li2 Co1 83.25(3) 1_665 1_565 ?
Li1 Li2 Co1 134.897(13) 1_554 1_565 ?
Li2 Li2 Co1 67.449(6) 13_675 1_564 ?
Li2 Li2 Co1 67.449(6) 13_565 1_564 ?
N2 Li2 Co1 39.913(18) 1_565 1_564 ?
N2 Li2 Co1 112.551(6) 1_665 1_564 ?
N2 Li2 Co1 112.551(6) . 1_564 ?
Li2 Li2 Co1 140.087(18) 13_665 1_564 ?
Co1 Li2 Co1 83.25(3) 1_554 1_564 ?
Li1 Li2 Co1 134.897(13) 1_665 1_564 ?
Co1 Li2 Co1 134.897(13) 1_665 1_564 ?
Li1 Li2 Co1 83.25(3) 1_554 1_564 ?
Co1 Li2 Co1 79.83(4) 1_565 1_564 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.82
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.102

#===END