#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307620.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_4307620
loop_
_publ_author_name
'Antonio Otero'
'Juan Fernández-Baeza'
'Antonio Antiñolo'
'Juan Tejeda'
'Agustín Lara-Sánchez'
'Luis F. Sánchez-Barba'
'Isabel López-Solera'
'Ana M. Rodríguez'
_publ_contact_author
;                                                                               
     'Fernandez-Baeza, J.'                                     
      Departamento de Quimica Inorganica, Organica y Bioquimica
      Campus Universitario
      Universidad de Castilla-La Mancha
      13071-Ciudad Real
      Spain
;
_publ_contact_author_email       juan.fbaeza@uclm.es
_publ_contact_author_phone       '+34 926295300'
_publ_section_title
;
Lithium, Titanium, and Zirconium Complexes with Novel Amidinate Scorpionate
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1760
_journal_page_last               1770
_journal_paper_doi               10.1021/ic062093c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C42 H68 Li2 N16 O2, C8 H16 O2'
_chemical_formula_sum            'C50 H84 Li2 N16 O4'
_chemical_formula_weight         987.21
_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                 102.064(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.883(6)
_cell_length_b                   11.983(3)
_cell_length_c                   21.052(5)
_cell_measurement_temperature    160(2)
_cell_volume                     5645(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13916
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9609
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4877
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1131P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                2259
_reflns_number_total             4877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062093csi20061102_124645_4.cif
_cod_data_source_block           4
_cod_database_code               4307620
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
N1 N 0.38118(13) 0.1223(2) 0.59896(14) 0.0439(8) Uani 1 1 d . . .
N2 N 0.39916(13) 0.1937(2) 0.55585(14) 0.0459(8) Uani 1 1 d . . .
N3 N 0.33986(12) -0.0371(2) 0.53655(13) 0.0414(8) Uani 1 1 d . . .
N4 N 0.35773(12) -0.0178(2) 0.47861(13) 0.0426(8) Uani 1 1 d . . .
N5 N 0.27452(12) 0.1418(2) 0.64515(13) 0.0462(8) Uani 1 1 d . . .
N6 N 0.22520(13) 0.0214(2) 0.56004(14) 0.0476(8) Uani 1 1 d . . .
N7 N 0.29269(13) 0.2267(2) 0.41804(14) 0.0501(9) Uani 1 1 d . . .
N8 N 0.27896(14) 0.2349(3) 0.30576(15) 0.0599(10) Uani 1 1 d . . .
C1 C 0.44721(17) 0.2460(3) 0.59079(19) 0.0502(10) Uani 1 1 d . . .
C2 C 0.45870(17) 0.2085(3) 0.65482(18) 0.0525(10) Uani 1 1 d . . .
H2 H 0.4899 0.2328 0.6892 0.063 Uiso 1 1 calc R . .
C3 C 0.41629(17) 0.1297(3) 0.65857(18) 0.0471(10) Uani 1 1 d . . .
C4 C 0.40546(17) 0.0627(3) 0.71471(18) 0.0584(11) Uani 1 1 d . . .
H4A H 0.3657 0.0800 0.7225 0.088 Uiso 1 1 calc R . .
H4B H 0.4358 0.0811 0.7535 0.088 Uiso 1 1 calc R . .
H4C H 0.4078 -0.0169 0.7050 0.088 Uiso 1 1 calc R . .
C5 C 0.47871(18) 0.3346(3) 0.55975(19) 0.0664(12) Uani 1 1 d . . .
H5A H 0.5004 0.2996 0.5295 0.100 Uiso 1 1 calc R . .
H5B H 0.5069 0.3746 0.5935 0.100 Uiso 1 1 calc R . .
H5C H 0.4492 0.3872 0.5361 0.100 Uiso 1 1 calc R . .
C6 C 0.36146(16) -0.1190(3) 0.45277(17) 0.0486(10) Uani 1 1 d . . .
C7 C 0.34555(17) -0.2004(3) 0.49322(18) 0.0561(11) Uani 1 1 d . . .
H7 H 0.3446 -0.2786 0.4857 0.067 Uiso 1 1 calc R . .
C8 C 0.33163(17) -0.1479(3) 0.54535(18) 0.0506(10) Uani 1 1 d . . .
C9 C 0.31270(19) -0.1924(3) 0.60424(18) 0.0640(12) Uani 1 1 d . . .
H9A H 0.3349 -0.1541 0.6430 0.096 Uiso 1 1 calc R . .
H9B H 0.3210 -0.2726 0.6081 0.096 Uiso 1 1 calc R . .
H9C H 0.2698 -0.1796 0.6003 0.096 Uiso 1 1 calc R . .
C10 C 0.38103(17) -0.1316(3) 0.39029(17) 0.0606(12) Uani 1 1 d . . .
H10A H 0.3719 -0.0632 0.3647 0.091 Uiso 1 1 calc R . .
H10B H 0.3600 -0.1947 0.3661 0.091 Uiso 1 1 calc R . .
H10C H 0.4242 -0.1453 0.3989 0.091 Uiso 1 1 calc R . .
C11 C 0.33053(16) 0.0537(3) 0.57675(16) 0.0412(9) Uani 1 1 d . . .
C12 C 0.27666(16) 0.0767(3) 0.59295(17) 0.0438(9) Uani 1 1 d . . .
C13 C 0.17419(17) 0.0121(3) 0.59020(19) 0.0623(12) Uani 1 1 d . . .
H13A H 0.1878 0.0103 0.6375 0.093 Uiso 1 1 calc R . .
H13B H 0.1523 -0.0568 0.5756 0.093 Uiso 1 1 calc R . .
H13C H 0.1478 0.0764 0.5779 0.093 Uiso 1 1 calc R . .
C14 C 0.21185(17) 0.0168(4) 0.48971(18) 0.0630(12) Uani 1 1 d . . .
H14A H 0.2449 0.0500 0.4732 0.095 Uiso 1 1 calc R . .
H14B H 0.1750 0.0584 0.4728 0.095 Uiso 1 1 calc R . .
H14C H 0.2066 -0.0611 0.4755 0.095 Uiso 1 1 calc R . .
C15 C 0.26640(16) 0.2750(3) 0.36336(18) 0.0457(10) Uani 1 1 d . . .
C16 C 0.30592(18) 0.1260(3) 0.3029(2) 0.0671(12) Uani 1 1 d . . .
H16A H 0.3480 0.1350 0.3007 0.101 Uiso 1 1 calc R . .
H16B H 0.2848 0.0860 0.2643 0.101 Uiso 1 1 calc R . .
H16C H 0.3032 0.0833 0.3419 0.101 Uiso 1 1 calc R . .
C17 C 0.2635(2) 0.2951(4) 0.24566(19) 0.0752(14) Uani 1 1 d . . .
H17A H 0.2472 0.3683 0.2535 0.113 Uiso 1 1 calc R . .
H17B H 0.2334 0.2530 0.2149 0.113 Uiso 1 1 calc R . .
H17C H 0.2992 0.3051 0.2275 0.113 Uiso 1 1 calc R . .
Li1 Li 0.3666(3) 0.1516(5) 0.4589(3) 0.0524(16) Uani 1 1 d . . .
O1 O 0.43519(11) 0.1779(2) 0.41779(12) 0.0611(8) Uani 1 1 d . . .
C40 C 0.48891(19) 0.1152(4) 0.4298(2) 0.0776(14) Uani 1 1 d . . .
H40A H 0.4810 0.0360 0.4383 0.093 Uiso 1 1 calc R . .
H40B H 0.5177 0.1456 0.4676 0.093 Uiso 1 1 calc R . .
C41 C 0.5122(2) 0.1261(5) 0.3702(3) 0.114(2) Uani 1 1 d . . .
H41A H 0.5564 0.1308 0.3808 0.137 Uiso 1 1 calc R . .
H41B H 0.5003 0.0610 0.3415 0.137 Uiso 1 1 calc R . .
C42 C 0.4872(3) 0.2261(5) 0.3391(3) 0.132(2) Uani 1 1 d . . .
H42A H 0.4682 0.2108 0.2932 0.158 Uiso 1 1 calc R . .
H42B H 0.5189 0.2828 0.3400 0.158 Uiso 1 1 calc R . .
C43 C 0.44228(18) 0.2671(3) 0.37485(19) 0.0621(12) Uani 1 1 d . . .
H43A H 0.4566 0.3355 0.3996 0.074 Uiso 1 1 calc R . .
H43B H 0.4040 0.2837 0.3446 0.074 Uiso 1 1 calc R . .
O2 O 0.4206(6) 0.5628(7) 0.7281(5) 0.092(3) Uani 0.50 1 d PDU A 1
C50 C 0.4193(11) 0.4804(13) 0.7758(8) 0.098(5) Uani 0.50 1 d PDU A 1
H50A H 0.4108 0.5144 0.8158 0.118 Uiso 0.50 1 calc PR A 1
H50B H 0.4580 0.4406 0.7869 0.118 Uiso 0.50 1 calc PR A 1
C51 C 0.3704(14) 0.402(2) 0.7460(15) 0.104(6) Uani 0.50 1 d PDU A 1
H51A H 0.3849 0.3243 0.7502 0.124 Uiso 0.50 1 calc PR A 1
H51B H 0.3363 0.4091 0.7680 0.124 Uiso 0.50 1 calc PR A 1
C52 C 0.3512(11) 0.433(2) 0.6760(12) 0.112(7) Uani 0.50 1 d PDU A 1
H52A H 0.3494 0.3668 0.6477 0.134 Uiso 0.50 1 calc PR A 1
H52B H 0.3118 0.4706 0.6673 0.134 Uiso 0.50 1 calc PR A 1
C53 C 0.3984(9) 0.5093(17) 0.6669(9) 0.072(3) Uani 0.50 1 d PDU A 1
H53A H 0.4309 0.4677 0.6529 0.086 Uiso 0.50 1 calc PR A 1
H53B H 0.3824 0.5656 0.6333 0.086 Uiso 0.50 1 calc PR A 1
O3 O 0.4158(6) 0.4061(14) 0.7780(6) 0.147(5) Uani 0.50 1 d PDU B 2
C60 C 0.3593(10) 0.3713(18) 0.7445(11) 0.079(4) Uani 0.50 1 d PDU B 2
H60A H 0.3280 0.3944 0.7679 0.094 Uiso 0.50 1 calc PR B 2
H60B H 0.3581 0.2891 0.7395 0.094 Uiso 0.50 1 calc PR B 2
C61 C 0.3504(11) 0.4273(13) 0.6794(10) 0.075(5) Uani 0.50 1 d PDU B 2
H61A H 0.3551 0.3728 0.6456 0.090 Uiso 0.50 1 calc PR B 2
H61B H 0.3098 0.4599 0.6677 0.090 Uiso 0.50 1 calc PR B 2
C62 C 0.3960(14) 0.516(2) 0.6847(11) 0.136(9) Uani 0.50 1 d PDU B 2
H62A H 0.3779 0.5886 0.6690 0.163 Uiso 0.50 1 calc PR B 2
H62B H 0.4272 0.4966 0.6603 0.163 Uiso 0.50 1 calc PR B 2
C63 C 0.4203(16) 0.518(2) 0.7552(12) 0.173(11) Uani 0.50 1 d PDU B 2
H63A H 0.4625 0.5427 0.7644 0.207 Uiso 0.50 1 calc PR B 2
H63B H 0.3970 0.5699 0.7769 0.207 Uiso 0.50 1 calc PR B 2
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'
O O 0.0106 0.0060 '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
C3 N1 N2 111.9(3) . . ?
C3 N1 C11 129.3(3) . . ?
N2 N1 C11 118.8(3) . . ?
C1 N2 N1 104.7(3) . . ?
C1 N2 Li1 137.2(3) . . ?
N1 N2 Li1 113.7(3) . . ?
C8 N3 N4 111.0(3) . . ?
C8 N3 C11 128.6(3) . . ?
N4 N3 C11 120.4(3) . . ?
C6 N4 N3 105.2(3) . . ?
C6 N4 Li1 141.4(3) . . ?
N3 N4 Li1 113.3(3) . . ?
C15 N5 C12 117.2(3) 7_556 . ?
C12 N6 C13 119.4(3) . . ?
C12 N6 C14 119.9(3) . . ?
C13 N6 C14 115.4(3) . . ?
C15 N7 Li1 141.7(3) . . ?
C15 N8 C17 122.6(3) . . ?
C15 N8 C16 120.9(3) . . ?
C17 N8 C16 116.4(3) . . ?
N2 C1 C2 110.3(3) . . ?
N2 C1 C5 120.1(3) . . ?
C2 C1 C5 129.5(4) . . ?
C3 C2 C1 106.6(3) . . ?
N1 C3 C2 106.5(3) . . ?
N1 C3 C4 122.6(3) . . ?
C2 C3 C4 130.9(4) . . ?
N4 C6 C7 109.8(3) . . ?
N4 C6 C10 120.6(3) . . ?
C7 C6 C10 129.6(3) . . ?
C8 C7 C6 107.8(3) . . ?
N3 C8 C7 106.2(3) . . ?
N3 C8 C9 122.3(3) . . ?
C7 C8 C9 131.4(3) . . ?
C12 C11 N1 121.0(3) . . ?
C12 C11 N3 123.8(3) . . ?
N1 C11 N3 115.2(3) . . ?
N5 C12 C11 120.2(3) . . ?
N5 C12 N6 120.2(3) . . ?
C11 C12 N6 119.1(3) . . ?
N7 C15 N5 128.0(3) . 7_556 ?
N7 C15 N8 118.1(3) . . ?
N5 C15 N8 113.7(3) 7_556 . ?
N7 Li1 O1 115.5(3) . . ?
N7 Li1 N2 114.8(3) . . ?
O1 Li1 N2 103.7(3) . . ?
N7 Li1 N4 115.1(3) . . ?
O1 Li1 N4 111.2(3) . . ?
N2 Li1 N4 94.0(3) . . ?
C40 O1 C43 107.4(3) . . ?
C40 O1 Li1 125.3(3) . . ?
C43 O1 Li1 127.1(3) . . ?
O1 C40 C41 104.9(4) . . ?
C42 C41 C40 106.6(4) . . ?
C41 C42 C43 107.4(4) . . ?
O1 C43 C42 104.9(3) . . ?
C50 O2 C53 105.7(11) . . ?
O2 C50 C51 105.3(13) . . ?
C52 C51 C50 107.5(15) . . ?
C53 C52 C51 102.2(17) . . ?
O2 C53 C52 107.1(16) . . ?
C60 O3 C63 103.5(15) . . ?
O3 C60 C61 105.2(14) . . ?
C62 C61 C60 107.1(15) . . ?
C61 C62 C63 101.5(17) . . ?
O3 C63 C62 106.5(17) . . ?
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 C3 1.344(4) . ?
N1 N2 1.372(4) . ?
N1 C11 1.418(4) . ?
N2 C1 1.344(4) . ?
N2 Li1 2.083(7) . ?
N3 C8 1.359(4) . ?
N3 N4 1.384(3) . ?
N3 C11 1.421(4) . ?
N4 C6 1.339(4) . ?
N4 Li1 2.090(7) . ?
N5 C15 1.354(4) 7_556 ?
N5 C12 1.356(4) . ?
N6 C12 1.402(4) . ?
N6 C13 1.445(4) . ?
N6 C14 1.449(4) . ?
N7 C15 1.316(4) . ?
N7 Li1 1.950(7) . ?
N8 C15 1.389(4) . ?
N8 C17 1.435(5) . ?
N8 C16 1.450(4) . ?
C1 C2 1.393(5) . ?
C1 C5 1.507(5) . ?
C2 C3 1.368(5) . ?
C3 C4 1.491(5) . ?
C6 C7 1.392(5) . ?
C6 C10 1.483(5) . ?
C7 C8 1.359(5) . ?
C8 C9 1.495(5) . ?
C11 C12 1.374(4) . ?
C15 N5 1.354(4) 7_556 ?
Li1 O1 1.969(7) . ?
O1 C40 1.417(5) . ?
O1 C43 1.431(4) . ?
C40 C41 1.467(6) . ?
C41 C42 1.427(7) . ?
C42 C43 1.481(6) . ?
O2 C50 1.414(14) . ?
O2 C53 1.433(17) . ?
C50 C51 1.49(2) . ?
C51 C52 1.49(3) . ?
C52 C53 1.46(2) . ?
O3 C60 1.401(17) . ?
O3 C63 1.435(19) . ?
C60 C61 1.50(2) . ?
C61 C62 1.48(3) . ?
C62 C63 1.47(2) . ?
