#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:03:17 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179823 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/19/7011989.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_7011989
loop_
_publ_author_name
'Stéphane Daniele'
'Peter B. Hitchcock'
'Michael F. Lappert'
'Terence A. Nile'
'Colette M. Zdanski'
_publ_section_title
;
 Synthesis and structures of dinuclear low-coordinate lithium and
 zirconium(IV) complexes derived from the diamido ligands
 1,3-(CH2C6H3R12)2C6H4(R1= Me or Pri)
;
_journal_issue                   21
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3980
_journal_page_last               3984
_journal_paper_doi               10.1039/b206508h
_journal_year                    2002
_chemical_formula_sum            'C64 H84 Li4 N4'
_chemical_formula_weight         937.11
_chemical_name_common            '[C6H4{CH2N(Li)C6H3iPr2}2]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 115.79(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.045(6)
_cell_length_b                   15.874(3)
_cell_length_c                   18.651(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     5610(2)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.748
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta 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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3778
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0442P)²+3.3811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                2564
_reflns_number_total             3688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206508h.txt
_cod_data_source_block           jan1798-(MFL-3)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011989
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, 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
Li1 Li 0.0625(2) 0.0402(3) 0.2714(2) 0.0333(12) Uani 1 1 d . . .
Li2 Li 0.0133(2) 0.3368(3) 0.1953(2) 0.0359(12) Uani 1 1 d . . .
N1 N -0.00738(10) 0.03031(13) 0.16381(10) 0.0229(6) Uani 1 1 d . . .
N2 N 0.08134(9) 0.34515(13) 0.30586(10) 0.0228(5) Uani 1 1 d . . .
C1 C -0.00154(12) 0.08710(17) 0.10490(13) 0.0276(7) Uani 1 1 d . . .
H1A H -0.0447 0.1220 0.0803 0.033 Uiso 1 1 calc R . .
H1B H 0.0023 0.0534 0.0623 0.033 Uiso 1 1 calc R . .
C2 C 0.06205(11) 0.14365(16) 0.14283(12) 0.0220(6) Uani 1 1 d . . .
C3 C 0.07535(12) 0.18781(16) 0.21275(12) 0.0245(7) Uani 1 1 d . . .
H3 H 0.0437 0.1810 0.2362 0.029 Uiso 1 1 calc R . .
C4 C 0.13277(12) 0.24127(17) 0.24948(13) 0.0246(7) Uani 1 1 d . . .
C5 C 0.14287(12) 0.29089(17) 0.32307(13) 0.0302(7) Uani 1 1 d . . .
H5A H 0.1490 0.2516 0.3669 0.036 Uiso 1 1 calc R . .
H5B H 0.1859 0.3259 0.3404 0.036 Uiso 1 1 calc R . .
C6 C 0.17857(12) 0.25076(18) 0.21426(14) 0.0352(7) Uani 1 1 d . . .
H6 H 0.2182 0.2872 0.2376 0.042 Uiso 1 1 calc R . .
C7 C 0.16658(13) 0.20720(19) 0.14530(15) 0.0391(8) Uani 1 1 d . . .
H7 H 0.1983 0.2139 0.1218 0.047 Uiso 1 1 calc R . .
C8 C 0.10919(12) 0.15418(18) 0.11008(14) 0.0319(7) Uani 1 1 d . . .
H8 H 0.1020 0.1246 0.0629 0.038 Uiso 1 1 calc R . .
C9 C -0.04921(13) -0.0414(2) 0.12908(12) 0.0244(7) Uani 1 1 d . . .
C10 C -0.12417(13) -0.03547(19) 0.08980(13) 0.0272(7) Uani 1 1 d . . .
C11 C -0.16454(15) -0.1077(2) 0.05925(14) 0.0375(9) Uani 1 1 d . . .
H11 H -0.2145 -0.1031 0.0323 0.045 Uiso 1 1 calc R . .
C12 C -0.13348(16) -0.1854(2) 0.06741(15) 0.0432(9) Uani 1 1 d . . .
H12 H -0.1616 -0.2340 0.0456 0.052 Uiso 1 1 calc R . .
C13 C -0.06089(16) -0.1922(2) 0.10764(15) 0.0401(8) Uani 1 1 d . . .
H13 H -0.0398 -0.2462 0.1139 0.048 Uiso 1 1 calc R . .
C14 C -0.01798(14) -0.1224(2) 0.13908(13) 0.0293(8) Uani 1 1 d . . .
C15 C -0.16120(12) 0.04761(18) 0.08524(13) 0.0292(7) Uani 1 1 d . . .
H15 H -0.1238 0.0910 0.1119 0.035 Uiso 1 1 calc R . .
C16 C -0.20707(13) 0.0439(2) 0.13082(15) 0.0423(8) Uani 1 1 d . . .
H16A H -0.2302 0.0984 0.1268 0.063 Uiso 1 1 calc R . .
H16B H -0.1772 0.0309 0.1869 0.063 Uiso 1 1 calc R . .
H16C H -0.2430 -0.0001 0.1077 0.063 Uiso 1 1 calc R . .
C17 C -0.20555(13) 0.0771(2) -0.00071(14) 0.0436(8) Uani 1 1 d . . .
H17A H -0.2282 0.1309 -0.0002 0.065 Uiso 1 1 calc R . .
H17B H -0.2418 0.0349 -0.0292 0.065 Uiso 1 1 calc R . .
H17C H -0.1749 0.0843 -0.0276 0.065 Uiso 1 1 calc R . .
C18 C 0.06193(14) -0.13224(19) 0.18467(15) 0.0347(8) Uani 1 1 d . . .
H18 H 0.0771 -0.0972 0.2339 0.042 Uiso 1 1 calc R . .
C19 C 0.10015(14) -0.0974(2) 0.13751(16) 0.0464(8) Uani 1 1 d . . .
H19A H 0.0840 -0.0398 0.1201 0.070 Uiso 1 1 calc R . .
H19B H 0.0898 -0.1330 0.0908 0.070 Uiso 1 1 calc R . .
H19C H 0.1511 -0.0970 0.1714 0.070 Uiso 1 1 calc R . .
C20 C 0.08683(17) -0.2211(2) 0.21156(17) 0.0516(9) Uani 1 1 d . . .
H20A H 0.1384 -0.2218 0.2402 0.077 Uiso 1 1 calc R . .
H20B H 0.0716 -0.2582 0.1650 0.077 Uiso 1 1 calc R . .
H20C H 0.0666 -0.2409 0.2469 0.077 Uiso 1 1 calc R . .
C21 C 0.09903(11) 0.41643(18) 0.35707(12) 0.0225(7) Uani 1 1 d . . .
C22 C 0.09200(12) 0.41382(18) 0.42939(13) 0.0253(7) Uani 1 1 d . . .
C23 C 0.10207(12) 0.4872(2) 0.47391(13) 0.0299(7) Uani 1 1 d . . .
H23 H 0.0968 0.4854 0.5219 0.036 Uiso 1 1 calc R . .
C24 C 0.11946(13) 0.56217(19) 0.45016(14) 0.0324(7) Uani 1 1 d . . .
H24 H 0.1247 0.6120 0.4805 0.039 Uiso 1 1 calc R . .
C25 C 0.12926(12) 0.56415(19) 0.38128(14) 0.0313(7) Uani 1 1 d . . .
H25 H 0.1423 0.6156 0.3653 0.038 Uiso 1 1 calc R . .
C26 C 0.12036(12) 0.49259(19) 0.33533(13) 0.0256(7) Uani 1 1 d . . .
C27 C 0.07458(13) 0.33244(18) 0.45948(13) 0.0304(7) Uani 1 1 d . . .
H27 H 0.0673 0.2880 0.4187 0.036 Uiso 1 1 calc R . .
C28 C 0.13585(14) 0.30405(19) 0.53744(14) 0.0444(8) Uani 1 1 d . . .
H28A H 0.1231 0.2514 0.5555 0.067 Uiso 1 1 calc R . .
H28B H 0.1456 0.3476 0.5781 0.067 Uiso 1 1 calc R . .
H28C H 0.1780 0.2949 0.5286 0.067 Uiso 1 1 calc R . .
C29 C 0.00643(14) 0.33846(19) 0.47018(15) 0.0428(8) Uani 1 1 d . . .
H29A H -0.0024 0.2845 0.4897 0.064 Uiso 1 1 calc R . .
H29B H -0.0332 0.3519 0.4189 0.064 Uiso 1 1 calc R . .
H29C H 0.0114 0.3829 0.5088 0.064 Uiso 1 1 calc R . .
C30 C 0.13227(13) 0.49722(19) 0.26068(14) 0.0326(7) Uani 1 1 d . . .
H30 H 0.1345 0.4382 0.2431 0.039 Uiso 1 1 calc R . .
C31 C 0.20125(15) 0.5412(2) 0.27456(17) 0.0649(11) Uani 1 1 d . . .
H31A H 0.2062 0.5424 0.2247 0.097 Uiso 1 1 calc R . .
H31B H 0.2410 0.5104 0.3151 0.097 Uiso 1 1 calc R . .
H31C H 0.2007 0.5990 0.2928 0.097 Uiso 1 1 calc R . .
C32 C 0.07045(15) 0.5413(2) 0.19377(15) 0.0477(9) Uani 1 1 d . . .
H32A H 0.0789 0.5437 0.1461 0.072 Uiso 1 1 calc R . .
H32B H 0.0658 0.5986 0.2104 0.072 Uiso 1 1 calc R . .
H32C H 0.0269 0.5098 0.1817 0.072 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'
N N 0.0061 0.0033 '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'
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 Li1 N1 104.10(19) . 6_556 ?
N2 Li2 N2 106.25(19) . 6_556 ?
C9 N1 C1 112.99(17) . . ?
C9 N1 Li1 126.1(2) . . ?
C1 N1 Li1 117.35(19) . . ?
C9 N1 Li1 86.06(18) . 6_556 ?
C1 N1 Li1 131.3(2) . 6_556 ?
Li1 N1 Li1 75.14(19) . 6_556 ?
C21 N2 C5 111.79(17) . . ?
C21 N2 Li2 128.7(2) . . ?
C5 N2 Li2 111.42(19) . . ?
C21 N2 Li2 91.63(18) . 6_556 ?
C5 N2 Li2 138.4(2) . 6_556 ?
Li2 N2 Li2 73.21(19) . 6_556 ?
N1 C1 C2 111.15(18) . . ?
C8 C2 C3 117.4(2) . . ?
C8 C2 C1 121.7(2) . . ?
C3 C2 C1 120.88(19) . . ?
C4 C3 C2 123.0(2) . . ?
C3 C4 C6 117.8(2) . . ?
C3 C4 C5 120.9(2) . . ?
C6 C4 C5 121.2(2) . . ?
N2 C5 C4 110.11(18) . . ?
C7 C6 C4 120.1(2) . . ?
C8 C7 C6 121.0(2) . . ?
C2 C8 C7 120.7(2) . . ?
N1 C9 C14 120.6(2) . . ?
N1 C9 C10 120.8(3) . . ?
C14 C9 C10 118.3(2) . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 C15 119.1(2) . . ?
C9 C10 C15 121.0(2) . . ?
C12 C11 C10 121.2(3) . . ?
C11 C12 C13 119.4(3) . . ?
C12 C13 C14 121.9(3) . . ?
C13 C14 C9 119.3(3) . . ?
C13 C14 C18 120.7(3) . . ?
C9 C14 C18 120.1(3) . . ?
C10 C15 C17 112.8(2) . . ?
C10 C15 C16 111.5(2) . . ?
C17 C15 C16 110.2(2) . . ?
C20 C18 C14 114.8(3) . . ?
C20 C18 C19 109.6(2) . . ?
C14 C18 C19 111.7(2) . . ?
C26 C21 C22 118.4(2) . . ?
C26 C21 N2 120.8(2) . . ?
C22 C21 N2 120.6(2) . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 C27 119.4(2) . . ?
C21 C22 C27 121.2(2) . . ?
C24 C23 C22 121.7(2) . . ?
C23 C24 C25 119.1(3) . . ?
C26 C25 C24 121.3(3) . . ?
C25 C26 C21 120.0(2) . . ?
C25 C26 C30 119.7(2) . . ?
C21 C26 C30 120.3(2) . . ?
C22 C27 C29 112.7(2) . . ?
C22 C27 C28 111.3(2) . . ?
C29 C27 C28 110.1(2) . . ?
C26 C30 C32 110.5(2) . . ?
C26 C30 C31 113.0(2) . . ?
C32 C30 C31 109.8(2) . . ?
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
Li1 N1 1.909(4) . ?
Li1 N1 2.013(4) 6_556 ?
Li2 N2 1.937(4) . ?
Li2 N2 1.988(4) 6_556 ?
N1 C9 1.413(3) . ?
N1 C1 1.467(3) . ?
N1 Li1 2.013(4) 6_556 ?
N2 C21 1.422(3) . ?
N2 C5 1.470(3) . ?
N2 Li2 1.988(4) 6_556 ?
C1 C2 1.508(3) . ?
C2 C8 1.383(3) . ?
C2 C3 1.397(3) . ?
C3 C4 1.389(3) . ?
C4 C6 1.391(3) . ?
C4 C5 1.515(3) . ?
C6 C7 1.383(3) . ?
C7 C8 1.381(4) . ?
C9 C14 1.418(4) . ?
C9 C10 1.424(3) . ?
C10 C11 1.392(4) . ?
C10 C15 1.515(4) . ?
C11 C12 1.373(4) . ?
C12 C13 1.382(4) . ?
C13 C14 1.388(4) . ?
C14 C18 1.527(4) . ?
C15 C17 1.536(3) . ?
C15 C16 1.540(3) . ?
C18 C20 1.512(4) . ?
C18 C19 1.531(3) . ?
C21 C26 1.409(3) . ?
C21 C22 1.420(3) . ?
C22 C23 1.392(3) . ?
C22 C27 1.516(4) . ?
C23 C24 1.374(4) . ?
C24 C25 1.387(3) . ?
C25 C26 1.386(4) . ?
C26 C30 1.520(3) . ?
C27 C29 1.535(3) . ?
C27 C28 1.533(3) . ?
C30 C32 1.525(4) . ?
C30 C31 1.528(4) . ?
