#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/17/7011787.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_7011787
loop_
_publ_author_name
'Cole, Marcus L.'
'Junk, Peter C.'
'Louis, Lance M.'
_publ_section_title
;
 Synthesis and structural characterisation of some novel lithium and
 sodium N,N???-di(para-tolyl)formamidinate complexes
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3906
_journal_paper_doi               10.1039/b204047f
_journal_year                    2002
_chemical_formula_sum            'C36 H46 Li2 N6'
_chemical_formula_weight         576.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.830(6)
_cell_angle_beta                 90.847(6)
_cell_angle_gamma                108.264(6)
_cell_formula_units_Z            1
_cell_length_a                   8.472(3)
_cell_length_b                   10.446(3)
_cell_length_c                   11.821(4)
_cell_measurement_temperature    296(2)
_cell_volume                     888.5(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4135
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.9750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1234P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                1480
_reflns_number_total             2533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204047f.txt
_cod_data_source_block           compound4.CIF
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011787
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.0330(3) 0.1845(3) 0.5456(2) 0.0524(7) Uani 1 1 d . . .
C1 C 0.2935(4) 0.1680(3) 0.3100(3) 0.0544(8) Uani 1 1 d . . .
Li1 Li 0.1535(6) 0.0149(6) 0.4939(5) 0.0619(14) Uani 1 1 d . . .
N2 N 0.1760(3) 0.1204(3) 0.3798(2) 0.0574(7) Uani 1 1 d . . .
C2 C 0.2758(5) 0.0798(4) 0.1814(3) 0.0628(9) Uani 1 1 d . . .
H2 H 0.170(4) -0.008(4) 0.141(3) 0.068(9) Uiso 1 1 d . . .
N3 N 0.3635(4) 0.0709(4) 0.6197(3) 0.0770(9) Uani 1 1 d . . .
C3 C 0.3896(5) 0.1215(4) 0.1109(3) 0.0679(10) Uani 1 1 d . . .
H3 H 0.376(4) 0.056(4) 0.018(3) 0.077(10) Uiso 1 1 d . . .
C4 C 0.5304(5) 0.2528(4) 0.1649(3) 0.0686(10) Uani 1 1 d . . .
C5 C 0.5499(5) 0.3383(4) 0.2929(4) 0.0728(10) Uani 1 1 d . . .
H5 H 0.646(4) 0.431(4) 0.336(3) 0.082(11) Uiso 1 1 d . . .
C6 C 0.4368(5) 0.2987(4) 0.3658(4) 0.0675(10) Uani 1 1 d . . .
H6 H 0.456(4) 0.359(4) 0.455(3) 0.073(10) Uiso 1 1 d . . .
C7 C 0.6518(6) 0.2989(5) 0.0859(4) 0.0995(14) Uani 1 1 d . . .
H7A H 0.6359 0.3813 0.0766 0.149 Uiso 1 1 calc R . .
H7B H 0.6317 0.2152 0.0040 0.149 Uiso 1 1 calc R . .
H7C H 0.7653 0.3297 0.1265 0.149 Uiso 1 1 calc R . .
C8 C -0.0219(4) 0.2937(3) 0.6353(3) 0.0532(8) Uani 1 1 d . . .
C9 C -0.0626(5) 0.4028(4) 0.6153(4) 0.0725(10) Uani 1 1 d . . .
H9 H -0.047(4) 0.400(4) 0.532(3) 0.085(11) Uiso 1 1 d . . .
C10 C -0.1207(5) 0.5024(5) 0.7073(4) 0.0773(11) Uani 1 1 d . . .
H10 H -0.131(5) 0.581(5) 0.698(4) 0.108(14) Uiso 1 1 d . . .
C11 C -0.1434(4) 0.4991(4) 0.8213(3) 0.0672(10) Uani 1 1 d . . .
C12 C -0.1086(4) 0.3881(4) 0.8386(3) 0.0614(9) Uani 1 1 d . . .
H12 H -0.130(4) 0.384(3) 0.918(3) 0.064(9) Uiso 1 1 d . . .
C13 C -0.0495(4) 0.2875(4) 0.7484(3) 0.0530(8) Uani 1 1 d . . .
H13 H -0.022(3) 0.213(3) 0.766(2) 0.053(8) Uiso 1 1 d . . .
C14 C -0.2074(6) 0.6094(5) 0.9214(4) 0.1001(14) Uani 1 1 d . . .
H14A H -0.2174 0.5873 0.9926 0.150 Uiso 1 1 calc R . .
H14B H -0.3157 0.6007 0.8871 0.150 Uiso 1 1 calc R . .
H14C H -0.1296 0.7101 0.9480 0.150 Uiso 1 1 calc R . .
C15 C 0.1279(4) 0.2202(4) 0.4675(3) 0.0540(8) Uani 1 1 d . . .
H15 H 0.165(3) 0.328(3) 0.475(2) 0.050(8) Uiso 1 1 d . . .
C16 C 0.5063(6) 0.0478(8) 0.5594(4) 0.157(3) Uani 1 1 d . . .
H16A H 0.5788 0.1457 0.5692 0.188 Uiso 1 1 calc R . .
H16B H 0.5679 0.0201 0.6098 0.188 Uiso 1 1 calc R . .
C17 C 0.3140(6) -0.0157(6) 0.6909(4) 0.1239(18) Uani 1 1 d . . .
H17A H 0.2793 -0.1213 0.6343 0.186 Uiso 1 1 calc R . .
H17B H 0.2221 0.0054 0.7322 0.186 Uiso 1 1 calc R . .
H17C H 0.4080 0.0115 0.7531 0.186 Uiso 1 1 calc R . .
C18 C 0.4095(6) 0.2303(6) 0.7080(4) 0.1175(17) Uani 1 1 d . . .
H18C H 0.3177 0.2456 0.7522 0.176 Uiso 1 1 calc R . .
H18B H 0.4332 0.2894 0.6621 0.176 Uiso 1 1 calc R . .
H18A H 0.5078 0.2607 0.7678 0.176 Uiso 1 1 calc R . .
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
C15 N1 C8 118.9(3) . . ?
C15 N1 Li1 127.8(3) . 2_556 ?
C8 N1 Li1 104.2(2) . 2_556 ?
C15 N1 Li1 80.5(2) . . ?
C8 N1 Li1 151.6(2) . . ?
Li1 N1 Li1 73.6(2) 2_556 . ?
C2 C1 C6 116.8(3) . . ?
C2 C1 N2 120.1(3) . . ?
C6 C1 N2 122.9(3) . . ?
N1 Li1 N2 123.3(3) 2_556 . ?
N1 Li1 N3 115.5(3) 2_556 . ?
N2 Li1 N3 118.2(3) . . ?
N1 Li1 N1 106.4(2) 2_556 . ?
N2 Li1 N1 65.25(18) . . ?
N3 Li1 N1 115.2(3) . . ?
C15 N2 C1 118.7(3) . . ?
C15 N2 Li1 86.8(2) . . ?
C1 N2 Li1 138.7(2) . . ?
C3 C2 C1 121.7(4) . . ?
C16 N3 C17 111.8(4) . . ?
C16 N3 C18 108.9(4) . . ?
C17 N3 C18 107.9(3) . . ?
C16 N3 Li1 113.3(3) . . ?
C17 N3 Li1 107.5(3) . . ?
C18 N3 Li1 107.1(3) . . ?
C2 C3 C4 122.0(3) . . ?
C5 C4 C3 116.3(3) . . ?
C5 C4 C7 122.4(4) . . ?
C3 C4 C7 121.3(3) . . ?
C4 C5 C6 122.8(4) . . ?
C5 C6 C1 120.4(3) . . ?
C13 C8 C9 116.9(3) . . ?
C13 C8 N1 118.5(3) . . ?
C9 C8 N1 124.5(3) . . ?
C13 C8 Li1 90.7(2) . 2_556 ?
C9 C8 Li1 130.4(3) . 2_556 ?
N1 C8 Li1 46.02(17) . 2_556 ?
C10 C9 C8 120.5(3) . . ?
C9 C10 C11 122.6(4) . . ?
C12 C11 C10 116.6(3) . . ?
C12 C11 C14 121.4(3) . . ?
C10 C11 C14 122.0(3) . . ?
C11 C12 C13 121.9(3) . . ?
C12 C13 C8 121.4(3) . . ?
N2 C15 N1 120.8(3) . . ?
C16 C16 N3 124.0(6) 2_656 . ?
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 C15 1.327(4) . ?
N1 C8 1.405(4) . ?
N1 Li1 2.037(6) 2_556 ?
N1 Li1 2.189(6) . ?
C1 C2 1.383(4) . ?
C1 C6 1.398(5) . ?
C1 N2 1.407(4) . ?
Li1 N1 2.037(6) 2_556 ?
Li1 N2 2.047(6) . ?
Li1 N3 2.064(6) . ?
N2 C15 1.303(4) . ?
C2 C3 1.370(5) . ?
N3 C16 1.448(5) . ?
N3 C17 1.454(5) . ?
N3 C18 1.462(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.371(5) . ?
C4 C7 1.502(5) . ?
C5 C6 1.381(5) . ?
C8 C13 1.385(4) . ?
C8 C9 1.395(4) . ?
C8 Li1 2.745(6) 2_556 ?
C9 C10 1.376(5) . ?
C10 C11 1.377(5) . ?
C11 C12 1.373(5) . ?
C11 C14 1.512(5) . ?
C12 C13 1.377(4) . ?
C16 C16 1.316(8) 2_656 ?
