# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Li3P7
_database_code_depnum_ccdc_archive 'CCDC 1423489'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H48 Li3 N6 P7'
_chemical_formula_weight         586.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   11.3403(3)
_cell_length_b                   11.3403(3)
_cell_length_c                   15.1182(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1683.76(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9783
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      29.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.384
_shelx_estimated_absorpt_T_min   0.927
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27833
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.401
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3423
_reflns_number_gt                2824
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component perfect twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0629P)²+0.4867P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3423
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3774(4) 1.1799(3) 0.3032(2) 0.0527(8) Uani 1 1 d . . . . .
H1A H 0.4779 1.2322 0.2980 0.063 Uiso 1 1 calc R U . . .
H1B H 0.3488 1.2364 0.3367 0.063 Uiso 1 1 calc R U . . .
C2 C 0.3174(4) 1.1549(3) 0.2138(2) 0.0520(8) Uani 1 1 d . . . . .
H2A H 0.2181 1.1187 0.2191 0.062 Uiso 1 1 calc R U . . .
H2B H 0.3568 1.2425 0.1815 0.062 Uiso 1 1 calc R U . . .
C3 C 0.4279(5) 1.0802(5) 0.4265(3) 0.0797(14) Uani 1 1 d . . . . .
H3A H 0.5209 1.1155 0.4047 0.119 Uiso 1 1 calc R U . . .
H3B H 0.3990 0.9953 0.4590 0.119 Uiso 1 1 calc R U . . .
H3C H 0.4251 1.1473 0.4660 0.119 Uiso 1 1 calc R U . . .
C4 C 0.1953(4) 0.9959(4) 0.3845(2) 0.0598(9) Uani 1 1 d . . . . .
H4A H 0.1716 0.9168 0.4222 0.090 Uiso 1 1 calc R U . . .
H4B H 0.1338 0.9677 0.3335 0.090 Uiso 1 1 calc R U . . .
H4C H 0.1864 1.0647 0.4185 0.090 Uiso 1 1 calc R U . . .
C5 C 0.4776(4) 1.1308(4) 0.1228(3) 0.0651(10) Uani 1 1 d . . . . .
H5A H 0.4866 1.2057 0.0857 0.098 Uiso 1 1 calc R U . . .
H5B H 0.4908 1.0668 0.0865 0.098 Uiso 1 1 calc R U . . .
H5C H 0.5463 1.1672 0.1698 0.098 Uiso 1 1 calc R U . . .
C6 C 0.2417(5) 0.9966(4) 0.0911(3) 0.0807(14) Uani 1 1 d . . . . .
H6A H 0.1496 0.9484 0.1159 0.121 Uiso 1 1 calc R U . . .
H6B H 0.2598 0.9319 0.0594 0.121 Uiso 1 1 calc R U . . .
H6C H 0.2496 1.0671 0.0502 0.121 Uiso 1 1 calc R U . . .
Li1 Li 0.3373(4) 0.9209(4) 0.2577(3) 0.0298(8) Uani 1 1 d . . . . .
N1 N 0.3380(2) 1.0545(2) 0.35322(14) 0.0349(4) Uani 1 1 d . . . . .
N2 N 0.3405(3) 1.0597(2) 0.16265(15) 0.0368(5) Uani 1 1 d . . . . .
P1 P 0.16172(5) 0.66914(5) 0.27704(5) 0.02912(15) Uani 1 1 d . . . . .
P2 P 0.3333 0.6667 0.34183(7) 0.0247(2) Uani 1 3 d S T P . .
P3 P 0.21897(7) 0.66799(7) 0.14116(5) 0.03807(17) Uani 1 1 d . . . . .


_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
C1 N1 1.468(4) . ?
C1 C2 1.477(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.455(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.434(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.486(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N2 1.475(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.461(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Li1 N1 2.090(4) . ?
Li1 N2 2.118(4) . ?
Li1 P1 2.549(4) 3_565 ?
Li1 P1 2.553(4) . ?
Li1 P3 3.039(4) 3_565 ?
Li1 P3 3.047(4) . ?
P1 P3 2.1565(10) . ?
P1 P2 2.1914(7) . ?
P1 Li1 2.549(4) 2_665 ?
P2 P1 2.1914(7) 3_565 ?
P2 P1 2.1914(7) 2_665 ?
P3 P3 2.2593(12) 3_565 ?
P3 P3 2.2593(12) 2_665 ?
P3 Li1 3.039(4) 2_665 ?

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
N1 C1 C2 113.4(3) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N2 C2 C1 113.1(2) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 Li1 N2 86.43(16) . . ?
N1 Li1 P1 117.27(19) . 3_565 ?
N2 Li1 P1 128.0(2) . 3_565 ?
N1 Li1 P1 116.73(18) . . ?
N2 Li1 P1 128.5(2) . . ?
P1 Li1 P1 83.45(11) 3_565 . ?
N1 Li1 P3 158.0(2) . 3_565 ?
N2 Li1 P3 97.91(16) . 3_565 ?
P1 Li1 P3 44.33(6) 3_565 3_565 ?
P1 Li1 P3 77.18(10) . 3_565 ?
N1 Li1 P3 157.25(19) . . ?
N2 Li1 P3 98.23(16) . . ?
P1 Li1 P3 77.18(10) 3_565 . ?
P1 Li1 P3 44.21(7) . . ?
P3 Li1 P3 43.58(6) 3_565 . ?
C3 N1 C1 111.1(3) . . ?
C3 N1 C4 110.4(3) . . ?
C1 N1 C4 109.5(3) . . ?
C3 N1 Li1 115.2(2) . . ?
C1 N1 Li1 103.60(19) . . ?
C4 N1 Li1 106.7(2) . . ?
C2 N2 C6 112.2(3) . . ?
C2 N2 C5 110.0(3) . . ?
C6 N2 C5 107.8(3) . . ?
C2 N2 Li1 104.4(2) . . ?
C6 N2 Li1 114.5(2) . . ?
C5 N2 Li1 107.8(2) . . ?
P3 P1 P2 98.84(4) . . ?
P3 P1 Li1 80.00(10) . 2_665 ?
P2 P1 Li1 82.32(9) . 2_665 ?
P3 P1 Li1 80.15(10) . . ?
P2 P1 Li1 82.22(9) . . ?
Li1 P1 Li1 152.56(14) 2_665 . ?
P1 P2 P1 101.56(4) . 3_565 ?
P1 P2 P1 101.56(4) . 2_665 ?
P1 P2 P1 101.56(4) 3_565 2_665 ?
P1 P3 P3 105.21(2) . 3_565 ?
P1 P3 P3 105.34(2) . 2_665 ?
P3 P3 P3 60.000(1) 3_565 2_665 ?
P1 P3 Li1 55.67(8) . 2_665 ?
P3 P3 Li1 116.44(8) 3_565 2_665 ?
P3 P3 Li1 68.39(8) 2_665 2_665 ?
P1 P3 Li1 55.64(8) . . ?
P3 P3 Li1 68.03(8) 3_565 . ?
P3 P3 Li1 116.16(8) 2_665 . ?
Li1 P3 Li1 109.04(14) 2_665 . ?

_refine_diff_density_max         0.784
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.070



#===END 

