#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:25:53 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180078 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/24/7052464.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7052464
loop_
_publ_author_name
'Cole, Marcus L.'
'Davies, Aaron J.'
'Jones, Cameron'
'Junk, Peter C.'
_publ_section_title
;
 Bulky formamidinate complexes of lithium: the first examples of
 η2:η1-CN,N′ metal amidinate coordination
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1404
_journal_paper_doi               10.1039/b511519a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C34 H58 Li N5'
_chemical_formula_sum            'C34 H58 Li N5'
_chemical_formula_weight         543.79
_chemical_melting_point          422
_chemical_name_common
'[Li{N(2,6-iPr2C6H3)C(H)N(2,6-iPr2C6H3)}(PMDETA)]'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7197(2)
_cell_length_b                   16.5509(2)
_cell_length_c                   17.5383(3)
_cell_measurement_temperature    123(2)
_cell_volume                     3401.93(9)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31582
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9756
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.5(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0545P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                5411
_reflns_number_total             8298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b511519a.txt
_cod_data_source_block           Compound_3
_cod_database_code               7052464
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.12005(12) 0.84804(7) 0.15494(8) 0.0214(3) Uani 1 1 d . . .
N2 N 0.11255(12) 0.98347(7) 0.12369(8) 0.0235(3) Uani 1 1 d . . .
N3 N 0.07352(13) 0.97066(8) 0.32945(8) 0.0273(4) Uani 1 1 d . . .
N4 N -0.05666(13) 0.82240(8) 0.32366(9) 0.0300(4) Uani 1 1 d . . .
N5 N -0.17213(13) 0.90744(8) 0.20208(8) 0.0281(4) Uani 1 1 d . . .
C1 C 0.15477(14) 0.77009(9) 0.13031(9) 0.0204(4) Uani 1 1 d . . .
C2 C 0.23306(14) 0.72576(9) 0.17544(9) 0.0210(4) Uani 1 1 d . . .
C3 C 0.26659(15) 0.64911(10) 0.15171(10) 0.0232(4) Uani 1 1 d . . .
H3 H 0.3200 0.6196 0.1815 0.028 Uiso 1 1 calc R . .
C4 C 0.22368(15) 0.61516(9) 0.08566(10) 0.0244(4) Uani 1 1 d . . .
H4 H 0.2484 0.5632 0.0697 0.029 Uiso 1 1 calc R . .
C5 C 0.14489(15) 0.65723(10) 0.04318(10) 0.0244(4) Uani 1 1 d . . .
H5 H 0.1138 0.6330 -0.0013 0.029 Uiso 1 1 calc R . .
C6 C 0.10962(14) 0.73442(9) 0.06376(10) 0.0209(4) Uani 1 1 d . . .
C7 C 0.28393(15) 0.76395(9) 0.24603(10) 0.0255(4) Uani 1 1 d . . .
H7 H 0.2256 0.8019 0.2671 0.031 Uiso 1 1 calc R . .
C8 C 0.31279(18) 0.70336(11) 0.30898(10) 0.0332(5) Uani 1 1 d . . .
H8A H 0.3744 0.6678 0.2917 0.050 Uiso 1 1 calc R . .
H8B H 0.2451 0.6709 0.3208 0.050 Uiso 1 1 calc R . .
H8C H 0.3373 0.7325 0.3548 0.050 Uiso 1 1 calc R . .
C9 C 0.38916(18) 0.81415(11) 0.22564(12) 0.0378(5) Uani 1 1 d . . .
H9A H 0.3699 0.8520 0.1846 0.057 Uiso 1 1 calc R . .
H9B H 0.4505 0.7782 0.2086 0.057 Uiso 1 1 calc R . .
H9C H 0.4144 0.8444 0.2706 0.057 Uiso 1 1 calc R . .
C10 C 0.02303(15) 0.77686(10) 0.01344(10) 0.0256(4) Uani 1 1 d . . .
H10 H -0.0006 0.8276 0.0401 0.031 Uiso 1 1 calc R . .
C11 C -0.08458(16) 0.72548(10) 0.00159(12) 0.0329(5) Uani 1 1 d . . .
H11A H -0.1158 0.7098 0.0513 0.049 Uiso 1 1 calc R . .
H11B H -0.0650 0.6769 -0.0275 0.049 Uiso 1 1 calc R . .
H11C H -0.1416 0.7570 -0.0265 0.049 Uiso 1 1 calc R . .
C12 C 0.07441(19) 0.80113(12) -0.06354(11) 0.0385(5) Uani 1 1 d . . .
H12A H 0.0995 0.7526 -0.0908 0.058 Uiso 1 1 calc R . .
H12B H 0.1399 0.8369 -0.0551 0.058 Uiso 1 1 calc R . .
H12C H 0.0167 0.8294 -0.0939 0.058 Uiso 1 1 calc R . .
C13 C 0.15869(15) 1.04804(9) 0.08087(10) 0.0229(4) Uani 1 1 d . . .
C14 C 0.09363(15) 1.08306(9) 0.02124(10) 0.0246(4) Uani 1 1 d . . .
C15 C 0.13229(16) 1.15265(10) -0.01450(11) 0.0282(4) Uani 1 1 d . . .
H15 H 0.0871 1.1767 -0.0533 0.034 Uiso 1 1 calc R . .
C16 C 0.23541(17) 1.18792(10) 0.00524(11) 0.0301(5) Uani 1 1 d . . .
H16 H 0.2603 1.2360 -0.0193 0.036 Uiso 1 1 calc R . .
C17 C 0.30100(16) 1.15237(10) 0.06071(10) 0.0292(4) Uani 1 1 d . . .
H17 H 0.3728 1.1755 0.0731 0.035 Uiso 1 1 calc R . .
C18 C 0.26527(15) 1.08319(9) 0.09953(10) 0.0253(4) Uani 1 1 d . . .
C19 C -0.01785(15) 1.04548(10) -0.00565(11) 0.0285(4) Uani 1 1 d . . .
H19 H -0.0264 0.9920 0.0202 0.034 Uiso 1 1 calc R . .
C20 C -0.11906(18) 1.09745(12) 0.01673(15) 0.0500(6) Uani 1 1 d . . .
H20A H -0.1141 1.1497 -0.0094 0.075 Uiso 1 1 calc R . .
H20B H -0.1185 1.1061 0.0720 0.075 Uiso 1 1 calc R . .
H20C H -0.1899 1.0702 0.0020 0.075 Uiso 1 1 calc R . .
C21 C -0.01765(19) 1.03076(14) -0.09166(13) 0.0523(6) Uani 1 1 d . . .
H21A H 0.0478 0.9969 -0.1053 0.078 Uiso 1 1 calc R . .
H21B H -0.0122 1.0826 -0.1184 0.078 Uiso 1 1 calc R . .
H21C H -0.0884 1.0034 -0.1064 0.078 Uiso 1 1 calc R . .
C22 C 0.34142(16) 1.04861(11) 0.16159(11) 0.0322(4) Uani 1 1 d . . .
H22 H 0.3002 1.0018 0.1849 0.039 Uiso 1 1 calc R . .
C23 C 0.3639(2) 1.10987(12) 0.22504(12) 0.0436(5) Uani 1 1 d . . .
H23A H 0.2912 1.1277 0.2469 0.065 Uiso 1 1 calc R . .
H23B H 0.4046 1.1566 0.2040 0.065 Uiso 1 1 calc R . .
H23C H 0.4105 1.0847 0.2649 0.065 Uiso 1 1 calc R . .
C24 C 0.45346(18) 1.01652(12) 0.12860(13) 0.0441(6) Uani 1 1 d . . .
H24A H 0.4960 1.0611 0.1053 0.066 Uiso 1 1 calc R . .
H24B H 0.4369 0.9755 0.0899 0.066 Uiso 1 1 calc R . .
H24C H 0.4991 0.9924 0.1695 0.066 Uiso 1 1 calc R . .
C25 C 0.15132(14) 0.91013(9) 0.11183(10) 0.0219(4) Uani 1 1 d . . .
H25 H 0.2034 0.9012 0.0712 0.026 Uiso 1 1 calc R . .
C26 C 0.19585(16) 0.95638(11) 0.34271(12) 0.0345(5) Uani 1 1 d . . .
H26A H 0.2227 0.9916 0.3839 0.052 Uiso 1 1 calc R . .
H26B H 0.2386 0.9682 0.2960 0.052 Uiso 1 1 calc R . .
H26C H 0.2078 0.8998 0.3571 0.052 Uiso 1 1 calc R . .
C27 C 0.05684(19) 1.05748(10) 0.31645(12) 0.0384(5) Uani 1 1 d . . .
H27A H 0.0936 1.0731 0.2685 0.058 Uiso 1 1 calc R . .
H27B H 0.0908 1.0880 0.3586 0.058 Uiso 1 1 calc R . .
H27C H -0.0250 1.0693 0.3135 0.058 Uiso 1 1 calc R . .
C28 C 0.00782(17) 0.94247(11) 0.39574(11) 0.0342(5) Uani 1 1 d . . .
H28A H -0.0688 0.9677 0.3951 0.041 Uiso 1 1 calc R . .
H28B H 0.0469 0.9595 0.4432 0.041 Uiso 1 1 calc R . .
C29 C -0.00484(18) 0.85086(11) 0.39533(11) 0.0349(5) Uani 1 1 d . . .
H29A H 0.0711 0.8256 0.4017 0.042 Uiso 1 1 calc R . .
H29B H -0.0531 0.8340 0.4388 0.042 Uiso 1 1 calc R . .
C30 C -0.03040(19) 0.73649(10) 0.30996(13) 0.0416(5) Uani 1 1 d . . .
H30A H -0.0623 0.7037 0.3513 0.062 Uiso 1 1 calc R . .
H30B H 0.0525 0.7291 0.3081 0.062 Uiso 1 1 calc R . .
H30C H -0.0640 0.7196 0.2613 0.062 Uiso 1 1 calc R . .
C31 C -0.18185(16) 0.83425(12) 0.32470(11) 0.0358(5) Uani 1 1 d . . .
H31A H -0.2004 0.8836 0.3541 0.043 Uiso 1 1 calc R . .
H31B H -0.2186 0.7877 0.3503 0.043 Uiso 1 1 calc R . .
C32 C -0.22781(18) 0.84215(11) 0.24500(11) 0.0373(5) Uani 1 1 d . . .
H32A H -0.2165 0.7905 0.2176 0.045 Uiso 1 1 calc R . .
H32B H -0.3109 0.8528 0.2474 0.045 Uiso 1 1 calc R . .
C33 C -0.20152(19) 0.89934(12) 0.12220(11) 0.0415(5) Uani 1 1 d . . .
H33A H -0.1612 0.9406 0.0926 0.062 Uiso 1 1 calc R . .
H33B H -0.2840 0.9063 0.1159 0.062 Uiso 1 1 calc R . .
H33C H -0.1792 0.8456 0.1041 0.062 Uiso 1 1 calc R . .
C34 C -0.21000(19) 0.98628(11) 0.22842(13) 0.0459(6) Uani 1 1 d . . .
H34A H -0.2924 0.9914 0.2205 0.069 Uiso 1 1 calc R . .
H34B H -0.1703 1.0286 0.1997 0.069 Uiso 1 1 calc R . .
H34C H -0.1928 0.9920 0.2828 0.069 Uiso 1 1 calc R . .
Li1 Li 0.0123(3) 0.89925(16) 0.23148(17) 0.0279(7) Uani 1 1 d . . .
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'
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'
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
C25 N1 C1 116.81(14) . . ?
C25 N1 Li1 103.02(13) . . ?
C1 N1 Li1 139.40(13) . . ?
C25 N2 C13 118.84(14) . . ?
C25 N2 Li1 77.18(11) . . ?
C13 N2 Li1 162.70(12) . . ?
C27 N3 C28 111.33(15) . . ?
C27 N3 C26 108.15(14) . . ?
C28 N3 C26 109.52(15) . . ?
C27 N3 Li1 111.11(14) . . ?
C28 N3 Li1 105.99(13) . . ?
C26 N3 Li1 110.74(13) . . ?
C29 N4 C30 111.18(15) . . ?
C29 N4 C31 110.84(16) . . ?
C30 N4 C31 109.66(15) . . ?
C29 N4 Li1 106.82(13) . . ?
C30 N4 Li1 111.06(14) . . ?
C31 N4 Li1 107.16(14) . . ?
C33 N5 C34 108.52(16) . . ?
C33 N5 C32 108.76(15) . . ?
C34 N5 C32 111.21(16) . . ?
C33 N5 Li1 116.68(14) . . ?
C34 N5 Li1 106.11(14) . . ?
C32 N5 Li1 105.53(14) . . ?
C6 C1 C2 119.23(14) . . ?
C6 C1 N1 121.62(15) . . ?
C2 C1 N1 119.09(14) . . ?
C3 C2 C1 119.20(15) . . ?
C3 C2 C7 120.96(15) . . ?
C1 C2 C7 119.75(14) . . ?
C4 C3 C2 121.23(16) . . ?
C5 C4 C3 119.49(15) . . ?
C4 C5 C6 121.60(16) . . ?
C5 C6 C1 119.19(16) . . ?
C5 C6 C10 118.25(15) . . ?
C1 C6 C10 122.56(14) . . ?
C2 C7 C8 113.83(13) . . ?
C2 C7 C9 110.69(15) . . ?
C8 C7 C9 110.29(15) . . ?
C6 C10 C12 111.78(15) . . ?
C6 C10 C11 111.82(13) . . ?
C12 C10 C11 110.42(16) . . ?
N2 C13 C18 121.68(16) . . ?
N2 C13 C14 119.67(15) . . ?
C18 C13 C14 118.47(15) . . ?
C15 C14 C13 119.79(16) . . ?
C15 C14 C19 118.66(16) . . ?
C13 C14 C19 121.54(15) . . ?
C16 C15 C14 121.44(17) . . ?
C17 C16 C15 119.01(16) . . ?
C16 C17 C18 121.95(17) . . ?
C17 C18 C13 119.25(16) . . ?
C17 C18 C22 118.81(16) . . ?
C13 C18 C22 121.93(15) . . ?
C20 C19 C14 111.06(15) . . ?
C20 C19 C21 110.31(18) . . ?
C14 C19 C21 111.70(15) . . ?
C18 C22 C23 111.91(15) . . ?
C18 C22 C24 111.34(16) . . ?
C23 C22 C24 110.94(16) . . ?
N2 C25 N1 122.01(15) . . ?
N2 C25 Li1 74.09(11) . . ?
N1 C25 Li1 47.92(10) . . ?
N3 C28 C29 111.29(15) . . ?
N4 C29 C28 111.25(15) . . ?
N4 C31 C32 110.80(16) . . ?
N5 C32 C31 112.39(16) . . ?
N1 Li1 N3 122.47(15) . . ?
N1 Li1 N4 118.11(13) . . ?
N3 Li1 N4 81.80(12) . . ?
N1 Li1 N5 118.47(15) . . ?
N3 Li1 N5 117.63(14) . . ?
N4 Li1 N5 81.35(12) . . ?
N1 Li1 N2 57.79(9) . . ?
N3 Li1 N2 97.51(11) . . ?
N4 Li1 N2 174.61(15) . . ?
N5 Li1 N2 103.62(12) . . ?
N1 Li1 C25 29.06(7) . . ?
N3 Li1 C25 112.24(13) . . ?
N4 Li1 C25 147.05(13) . . ?
N5 Li1 C25 114.05(13) . . ?
N2 Li1 C25 28.73(5) . . ?
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
N1 C25 1.327(2) . ?
N1 C1 1.420(2) . ?
N1 Li1 2.029(3) . ?
N2 C25 1.313(2) . ?
N2 C13 1.414(2) . ?
N2 Li1 2.626(3) . ?
N3 C27 1.468(2) . ?
N3 C28 1.471(2) . ?
N3 C26 1.472(2) . ?
N3 Li1 2.206(3) . ?
N4 C29 1.473(2) . ?
N4 C30 1.475(2) . ?
N4 C31 1.480(2) . ?
N4 Li1 2.210(3) . ?
N5 C33 1.449(2) . ?
N5 C34 1.454(2) . ?
N5 C32 1.470(2) . ?
N5 Li1 2.226(3) . ?
C1 C6 1.411(2) . ?
C1 C2 1.417(2) . ?
C2 C3 1.392(2) . ?
C2 C7 1.513(2) . ?
C3 C4 1.382(2) . ?
C4 C5 1.376(2) . ?
C5 C6 1.390(2) . ?
C6 C10 1.517(2) . ?
C7 C8 1.529(2) . ?
C7 C9 1.529(3) . ?
C10 C12 1.532(3) . ?
C10 C11 1.535(2) . ?
C13 C18 1.416(2) . ?
C13 C14 1.418(2) . ?
C14 C15 1.387(2) . ?
C14 C19 1.522(2) . ?
C15 C16 1.386(3) . ?
C16 C17 1.372(3) . ?
C17 C18 1.396(2) . ?
C18 C22 1.519(3) . ?
C19 C20 1.517(3) . ?
C19 C21 1.528(3) . ?
C22 C23 1.528(3) . ?
C22 C24 1.530(3) . ?
C25 Li1 2.663(4) . ?
C28 C29 1.523(3) . ?
C31 C32 1.504(3) . ?
